data_global _journal_name_full 'Journal of Geophysical Research, Solid Earth' _journal_year 2016 _journal_volume . _journal_page_first . _journal_paper_doi . loop_ _publ_author_name _publ_author_address _publ_author_email 'J. Michael Brown' ; Department of Earth and Space Sciences Box 35-1310 University of Washington Seattle, WA 98195 ; brown@ess.washington.edu 'Angel R.J.' ;Virginia Tech Crystallography Laboratory Department of Geosciences Virginia Tech Blacksburg VA 24060-0420 USA ; rossjohnangel@gmail.com 'Ross, N.L.' ;Virginia Tech Crystallography Laboratory Department of Geosciences Virginia Tech Blacksburg VA 24060-0420 USA ; nross@vt.edu _publ_contact_author 'Ross, N.L.' _publ_contact_author_email nross@vt.edu _audit_contact_author_name 'Angel, Ross J.' _audit_contact_author_address ; Department of Geosciences, University of Padova Via Gradenigo 6, 35131 Padova, Italy ; _audit_contact_author_email rossjohnangel@gmail.com loop_ _audit_link_block_code _audit_link_block_description . ; This Cif contains seven structure refinements publlished for the first time in the paper listed in publ_ items. The data bloacks are named by nominal composition. The original sample numbers are given in this loop structure. ; An27plagioclase 'data collected as rja1002_x2' An37plagioclase 'data collected as rja1003_x1' An48plagioclase 'data collected as rja6_010x1abs' An60plagioclase 'data collected as rja6_011' An78plagioclase 'data collected as rja907x1' An98plagioclase 'data collected as rja6_006x2i' data_An27plagioclase _audit_creation_date 2010-07-02T11:38:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_mineral "plagioclase, low" _chemical_formula_moiety 'Al1.26 Ca0.26 Na0.74 O8 Si2.74' _chemical_formula_sum 'Al1.26 Ca0.26 Na0.74 O8 Si2.74' _chemical_formula_weight 266.379 _chemical_compound_source ; Natural mineral An26 low plagioclase supplied by J M Brown (university of Washington) His sample id plg1. Locality unknown ; #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_space_group_name_Hall '-C 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 8.1605(15) _cell_length_b 12.8391(5) _cell_length_c 7.1288(3) _cell_angle_alpha 93.833(13) _cell_angle_beta 116.440(5) _cell_angle_gamma 89.124(4) _cell_volume 667.20(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_pressure 100(1) _cell_measurement_reflns_used 1869 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 30 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.235 _exptl_crystal_size_mid 0.155 _exptl_crystal_size_min 0.055 _exptl_crystal_density_diffrn 2.64 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.09 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'CrysAlisPro (Oxford Diffraction, 2009)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.92 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'fine-focus sealed tube' _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_unetI/netI 0.0374 _diffrn_reflns_number 2941 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 1941 _reflns_number_gt 1537 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' _computing_publication_material 'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_number_reflns 1941 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.503 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.2675(3) -0.01542(18) 0.1576(3) 0.0371(5) Uani 0.74 1 d P . . Ca Ca 0.2749(4) 0.0281(2) 0.1017(4) 0.0253(5) Uani 0.26 1 d P . . T1O Si 0.00782(9) 0.16611(5) 0.21185(9) 0.01040(14) Uani 0.32 1 d P . . T1M Si 0.00345(8) 0.81794(5) 0.23343(9) 0.01023(13) Uani 0.83 1 d P . . T2O Si 0.68869(8) 0.10954(4) 0.31657(9) 0.00973(13) Uani 0.79 1 d P . . T2M Si 0.68207(8) 0.87999(4) 0.35776(9) 0.00961(13) Uani 0.8 1 d P . . T1OA Al 0.00782(9) 0.16611(5) 0.21185(9) 0.01040(14) Uani 0.68 1 d P . . T1MA Al 0.00345(8) 0.81794(5) 0.23343(9) 0.01023(13) Uani 0.17 1 d P . . T2OA Al 0.68869(8) 0.10954(4) 0.31657(9) 0.00973(13) Uani 0.21 1 d P . . T2MA Al 0.68207(8) 0.87999(4) 0.35776(9) 0.00961(13) Uani 0.2 1 d P . . OA1 O 0.0052(2) 0.13104(13) 0.9755(2) 0.0192(4) Uani 1 1 d . . . OA2 O 0.5873(2) 0.99416(11) 0.2793(2) 0.0140(3) Uani 1 1 d . . . OBO O 0.8136(2) 0.10810(13) 0.1903(3) 0.0185(3) Uani 1 1 d . . . OBM O 0.8179(2) 0.85138(14) 0.2507(3) 0.0236(4) Uani 1 1 d . . . OCO O 0.0142(2) 0.29586(13) 0.2757(3) 0.0184(3) Uani 1 1 d . . . OCM O 0.0187(2) 0.69041(13) 0.2210(3) 0.0186(3) Uani 1 1 d . . . ODO O 0.2012(2) 0.10907(12) 0.3862(2) 0.0170(3) Uani 1 1 d . . . ODM O 0.1870(2) 0.86713(13) 0.4317(3) 0.0197(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na 0.0131(7) 0.0592(15) 0.0339(11) -0.0289(10) 0.0098(8) -0.0112(9) Ca 0.0159(10) 0.0303(13) 0.0252(13) -0.0057(10) 0.0063(9) 0.0024(10) T1O 0.0115(3) 0.0115(3) 0.0081(3) 0.0008(2) 0.0041(2) -0.0032(2) T1M 0.0114(3) 0.0119(3) 0.0076(3) 0.0008(2) 0.0045(2) 0.0015(2) T2O 0.0102(3) 0.0079(3) 0.0102(3) 0.0001(2) 0.0038(2) -0.0013(2) T2M 0.0099(3) 0.0089(3) 0.0097(3) 0.0014(2) 0.0039(2) -0.0005(2) T1OA 0.0115(3) 0.0115(3) 0.0081(3) 0.0008(2) 0.0041(2) -0.0032(2) T1MA 0.0114(3) 0.0119(3) 0.0076(3) 0.0008(2) 0.0045(2) 0.0015(2) T2OA 0.0102(3) 0.0079(3) 0.0102(3) 0.0001(2) 0.0038(2) -0.0013(2) T2MA 0.0099(3) 0.0089(3) 0.0097(3) 0.0014(2) 0.0039(2) -0.0005(2) OA1 0.0262(9) 0.0217(8) 0.0133(8) 0.0036(6) 0.0117(7) 0.0001(7) OA2 0.0137(7) 0.0115(7) 0.0153(7) 0.0026(6) 0.0049(6) -0.0022(6) OBO 0.0212(9) 0.0170(8) 0.0209(8) -0.0012(6) 0.0129(7) -0.0049(7) OBM 0.0213(9) 0.0254(9) 0.0300(10) -0.0012(8) 0.0172(8) 0.0025(7) OCO 0.0176(8) 0.0178(8) 0.0187(8) -0.0001(6) 0.0071(7) -0.0048(7) OCM 0.0176(8) 0.0174(8) 0.0170(8) -0.0013(6) 0.0047(7) 0.0033(6) ODO 0.0174(8) 0.0180(8) 0.0112(7) 0.0012(6) 0.0023(6) 0.0003(7) ODM 0.0187(8) 0.0189(8) 0.0137(8) -0.0025(6) 0.0005(6) -0.0023(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na OA2 2.358(2) 1_545 ? Na ODO 2.431(2) . ? Na OA1 2.467(2) 3_556 ? Na OBO 2.485(2) 3_655 ? Na OA1 2.744(3) 1_554 ? Na ODM 2.844(3) 1_545 ? Ca OA2 2.337(3) 1_545 ? Ca OA1 2.389(3) 1_554 ? Ca OBO 2.475(3) 3_655 ? Ca ODO 2.518(3) . ? Ca OCM 2.721(3) 2_545 ? Ca OBM 2.840(3) 3_665 ? Ca OA1 2.929(3) 3_556 ? T1O OCO 1.6926(18) . ? T1O OBO 1.7010(17) 1_455 ? T1O OA1 1.7057(17) 1_554 ? T1O ODO 1.7063(18) . ? T1M OBM 1.6220(19) 1_455 ? T1M ODM 1.6323(17) . ? T1M OCM 1.6397(18) . ? T1M OA1 1.6392(16) 3_566 ? T2O ODM 1.6294(17) 3_666 ? T2O OBO 1.6324(18) . ? T2O OCM 1.6359(18) 2_545 ? T2O OA2 1.6547(15) 1_545 ? T2M OCO 1.6225(17) 2 ? T2M OBM 1.6279(19) . ? T2M ODO 1.6372(16) 3_666 ? T2M OA2 1.6580(16) . ? OA1 T1M 1.6392(16) 3_566 ? OA1 T1O 1.7058(17) 1_556 ? OA1 Ca 2.389(3) 1_556 ? OA1 Na 2.467(2) 3_556 ? OA1 Na 2.744(3) 1_556 ? OA1 Ca 2.929(3) 3_556 ? OA2 T2O 1.6547(15) 1_565 ? OA2 Ca 2.337(3) 1_565 ? OA2 Na 2.358(2) 1_565 ? OBO T1O 1.7010(17) 1_655 ? OBO Ca 2.475(3) 3_655 ? OBO Na 2.485(2) 3_655 ? OBM T1M 1.6220(19) 1_655 ? OBM Ca 2.840(3) 3_665 ? OCO T2M 1.6225(17) 2_445 ? OCM T2O 1.6359(18) 2_455 ? OCM Ca 2.721(3) 2_455 ? ODO T2M 1.6372(16) 3_666 ? ODM T2O 1.6294(17) 3_666 ? ODM Na 2.844(3) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OA2 Na ODO 105.47(8) 1_545 . ? OA2 Na OA1 145.96(12) 1_545 3_556 ? ODO Na OA1 100.66(9) . 3_556 ? OA2 Na OBO 98.31(9) 1_545 3_655 ? ODO Na OBO 151.60(11) . 3_655 ? OA1 Na OBO 65.01(7) 3_556 3_655 ? OA2 Na OA1 130.16(11) 1_545 1_554 ? ODO Na OA1 61.80(7) . 1_554 ? OA1 Na OA1 81.62(8) 3_556 1_554 ? OBO Na OA1 90.99(9) 3_655 1_554 ? OA2 Na ODM 109.26(10) 1_545 1_545 ? ODO Na ODM 72.95(7) . 1_545 ? OA1 Na ODM 58.48(7) 3_556 1_545 ? OBO Na ODM 113.64(9) 3_655 1_545 ? OA1 Na ODM 111.26(8) 1_554 1_545 ? OA2 Ca OA1 156.98(14) 1_545 1_554 ? OA2 Ca OBO 99.16(11) 1_545 3_655 ? OA1 Ca OBO 100.27(11) 1_554 3_655 ? OA2 Ca ODO 103.42(11) 1_545 . ? OA1 Ca ODO 65.92(9) 1_554 . ? OBO Ca ODO 145.29(13) 3_655 . ? OA2 Ca OCM 61.13(8) 1_545 2_545 ? OA1 Ca OCM 96.54(11) 1_554 2_545 ? OBO Ca OCM 131.03(13) 3_655 2_545 ? ODO Ca OCM 83.32(9) . 2_545 ? OA2 Ca OBM 113.50(12) 1_545 3_665 ? OA1 Ca OBM 59.40(8) 1_554 3_665 ? OBO Ca OBM 77.80(9) 3_655 3_665 ? ODO Ca OBM 115.53(11) . 3_665 ? OCM Ca OBM 72.09(9) 2_545 3_665 ? OA2 Ca OA1 122.01(12) 1_545 3_556 ? OA1 Ca OA1 79.14(10) 1_554 3_556 ? OBO Ca OA1 58.29(8) 3_655 3_556 ? ODO Ca OA1 87.29(10) . 3_556 ? OCM Ca OA1 170.60(12) 2_545 3_556 ? OBM Ca OA1 111.94(10) 3_665 3_556 ? OCO T1O OBO 111.82(9) . 1_455 ? OCO T1O OA1 116.18(9) . 1_554 ? OBO T1O OA1 102.73(9) 1_455 1_554 ? OCO T1O ODO 110.20(8) . . ? OBO T1O ODO 112.43(9) 1_455 . ? OA1 T1O ODO 103.07(9) 1_554 . ? OBM T1M ODM 112.23(10) 1_455 . ? OBM T1M OCM 110.09(9) 1_455 . ? ODM T1M OCM 108.98(9) . . ? OBM T1M OA1 106.93(10) 1_455 3_566 ? ODM T1M OA1 106.16(9) . 3_566 ? OCM T1M OA1 112.44(9) . 3_566 ? ODM T2O OBO 111.37(9) 3_666 . ? ODM T2O OCM 112.13(9) 3_666 2_545 ? OBO T2O OCM 111.75(9) . 2_545 ? ODM T2O OA2 107.76(9) 3_666 1_545 ? OBO T2O OA2 109.46(9) . 1_545 ? OCM T2O OA2 104.01(9) 2_545 1_545 ? OCO T2M OBM 110.66(10) 2 . ? OCO T2M ODO 113.15(9) 2 3_666 ? OBM T2M ODO 110.13(10) . 3_666 ? OCO T2M OA2 105.99(9) 2 . ? OBM T2M OA2 108.69(9) . . ? ODO T2M OA2 108.02(8) 3_666 . ? T1M OA1 T1O 141.17(11) 3_566 1_556 ? T1M OA1 Ca 105.10(11) 3_566 1_556 ? T1O OA1 Ca 97.82(10) 1_556 1_556 ? T1M OA1 Na 104.82(10) 3_566 3_556 ? T1O OA1 Na 96.23(9) 1_556 3_556 ? Ca OA1 Na 109.50(9) 1_556 3_556 ? T1M OA1 Na 117.50(10) 3_566 1_556 ? T1O OA1 Na 90.53(8) 1_556 1_556 ? Ca OA1 Na 14.21(6) 1_556 1_556 ? Na OA1 Na 98.38(8) 3_556 1_556 ? T1M OA1 Ca 115.83(10) 3_566 3_556 ? T1O OA1 Ca 89.38(9) 1_556 3_556 ? Ca OA1 Ca 100.86(10) 1_556 3_556 ? Na OA1 Ca 11.99(8) 3_556 3_556 ? Na OA1 Ca 88.65(7) 1_556 3_556 ? T2O OA2 T2M 128.59(10) 1_565 . ? T2O OA2 Ca 104.46(10) 1_565 1_565 ? T2M OA2 Ca 126.89(10) . 1_565 ? T2O OA2 Na 119.41(10) 1_565 1_565 ? T2M OA2 Na 110.94(9) . 1_565 ? Ca OA2 Na 17.80(7) 1_565 1_565 ? T2O OBO T1O 138.67(11) . 1_655 ? T2O OBO Ca 114.72(10) . 3_655 ? T1O OBO Ca 106.25(10) 1_655 3_655 ? T2O OBO Na 125.36(9) . 3_655 ? T1O OBO Na 95.72(9) 1_655 3_655 ? Ca OBO Na 16.84(6) 3_655 3_655 ? T1M OBM T2M 159.00(13) 1_655 . ? T1M OBM Ca 88.35(9) 1_655 3_665 ? T2M OBM Ca 109.45(10) . 3_665 ? T2M OCO T1O 130.51(12) 2_445 . ? T2O OCM T1M 133.92(11) 2_455 . ? T2O OCM Ca 90.31(9) 2_455 2_455 ? T1M OCM Ca 134.89(11) . 2_455 ? T2M ODO T1O 133.68(11) 3_666 . ? T2M ODO Na 124.31(10) 3_666 . ? T1O ODO Na 101.87(9) . . ? T2M ODO Ca 132.26(11) 3_666 . ? T1O ODO Ca 93.17(9) . . ? Na ODO Ca 16.76(6) . . ? T2O ODM T1M 150.85(12) 3_666 . ? T2O ODM Na 117.57(9) 3_666 1_565 ? T1M ODM Na 90.54(8) . 1_565 ? data_An37plagioclase _audit_creation_date 2010-07-24T10:17:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_mineral "plagioclase, low" _chemical_formula_moiety 'Al1.37 Ca0.37 Na0.63 O8 Si2.63' _chemical_formula_sum 'Al1.37 Ca0.37 Na0.63 O8 Si2.63' _chemical_formula_weight 268.15 _chemical_compound_source ; Natural mineral An37 low plagioclase supplied by George Rossman (CalTech) His sample id GRR1550 Locality unknown ; #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_space_group_name_Hall '-C 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 8.16577(9) _cell_length_b 12.85623(11) _cell_length_c 7.11418(9) _cell_angle_alpha 93.622(1) _cell_angle_beta 116.278(1) _cell_angle_gamma 89.679(1) _cell_volume 668.123(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15.1 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour none _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.052 _exptl_crystal_density_diffrn 2.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.16 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'CrysAlisPro (Oxford Diffraction, 2009)' _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.944 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'fine-focus sealed tube' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_number 3010 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 30.09 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 1951 _reflns_number_gt 1632 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.3965P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0055(11) _refine_ls_number_reflns 1951 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.591 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.2678(2) -0.02232(19) 0.1663(3) 0.0336(5) Uani 0.63 1 d P . . Ca Ca 0.27103(17) 0.02926(12) 0.1017(2) 0.0198(3) Uani 0.37 1 d P . . T1O Si 0.00663(8) 0.16485(5) 0.21338(9) 0.01347(15) Uani 0.41 1 d P . . T1M Si 0.00328(8) 0.81779(5) 0.23223(8) 0.01325(14) Uani 0.75 1 d P . . T2O Si 0.68630(7) 0.10933(4) 0.31661(8) 0.01147(14) Uani 0.75 1 d P . . T2M Si 0.68166(7) 0.87963(4) 0.35717(8) 0.01162(14) Uani 0.72 1 d P . . T1OA Al 0.00663(8) 0.16485(5) 0.21338(9) 0.01347(15) Uani 0.59 1 d P . . T1MA Al 0.00328(8) 0.81779(5) 0.23223(8) 0.01325(14) Uani 0.25 1 d P . . T2OA Al 0.68630(7) 0.10933(4) 0.31661(8) 0.01147(14) Uani 0.25 1 d P . . T2MA Al 0.68166(7) 0.87963(4) 0.35717(8) 0.01162(14) Uani 0.28 1 d P . . OA1 O 0.0036(2) 0.12947(14) 0.9779(2) 0.0243(4) Uani 1 1 d . . . OA2 O 0.58259(19) 0.99346(11) 0.2783(2) 0.0158(3) Uani 1 1 d . . . OBO O 0.8126(2) 0.10613(13) 0.1897(3) 0.0206(3) Uani 1 1 d . . . OBM O 0.8166(2) 0.85312(14) 0.2462(3) 0.0273(4) Uani 1 1 d . . . OCO O 0.0141(2) 0.29325(14) 0.2777(3) 0.0225(3) Uani 1 1 d . . . OCM O 0.0159(2) 0.68939(14) 0.2175(3) 0.0261(4) Uani 1 1 d . . . ODO O 0.1991(2) 0.10810(13) 0.3841(2) 0.0207(3) Uani 1 1 d . . . ODM O 0.1890(2) 0.86717(13) 0.4308(3) 0.0235(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na 0.0067(7) 0.0638(14) 0.0258(9) -0.0297(9) 0.0072(6) -0.0118(8) Ca 0.0112(5) 0.0229(7) 0.0196(6) -0.0051(5) 0.0024(5) 0.0029(5) T1O 0.0113(3) 0.0195(3) 0.0086(3) 0.0018(2) 0.0033(2) -0.0047(2) T1M 0.0116(3) 0.0189(3) 0.0078(2) 0.0000(2) 0.0032(2) 0.0050(2) T2O 0.0098(2) 0.0123(3) 0.0104(3) -0.00063(19) 0.0030(2) 0.00048(18) T2M 0.0099(2) 0.0141(3) 0.0100(3) 0.00189(19) 0.0034(2) -0.00090(19) T1OA 0.0113(3) 0.0195(3) 0.0086(3) 0.0018(2) 0.0033(2) -0.0047(2) T1MA 0.0116(3) 0.0189(3) 0.0078(2) 0.0000(2) 0.0032(2) 0.0050(2) T2OA 0.0098(2) 0.0123(3) 0.0104(3) -0.00063(19) 0.0030(2) 0.00048(18) T2MA 0.0099(2) 0.0141(3) 0.0100(3) 0.00189(19) 0.0034(2) -0.00090(19) OA1 0.0273(8) 0.0363(10) 0.0122(7) 0.0054(7) 0.0107(7) 0.0010(7) OA2 0.0130(6) 0.0169(7) 0.0158(7) 0.0024(5) 0.0046(6) -0.0017(5) OBO 0.0200(8) 0.0202(8) 0.0232(8) -0.0015(6) 0.0116(7) -0.0042(6) OBM 0.0226(8) 0.0263(9) 0.0386(10) -0.0030(7) 0.0194(8) 0.0019(7) OCO 0.0202(8) 0.0259(8) 0.0204(8) 0.0026(6) 0.0079(7) -0.0058(6) OCM 0.0204(8) 0.0300(9) 0.0178(8) -0.0060(7) 0.0005(7) 0.0112(7) ODO 0.0182(7) 0.0256(8) 0.0131(7) 0.0011(6) 0.0023(6) -0.0012(6) ODM 0.0186(7) 0.0264(9) 0.0160(7) -0.0040(6) -0.0002(6) 0.0000(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na OA2 2.335(2) 1_545 ? Na OA1 2.389(2) 3_556 ? Na ODO 2.441(2) . ? Na OBO 2.490(2) 3_655 ? Na ODM 2.719(3) 1_545 ? Na OA1 2.825(3) 1_554 ? Ca OA2 2.3437(19) 1_545 ? Ca OA1 2.369(2) 1_554 ? Ca OBO 2.469(2) 3_655 ? Ca ODO 2.488(2) . ? Ca OCM 2.699(2) 2_545 ? Ca OBM 2.796(3) 3_665 ? Ca OA1 2.880(2) 3_556 ? T1O OCO 1.6790(19) . ? T1O OBO 1.6941(16) 1_455 ? T1O OA1 1.6976(16) 1_554 ? T1O ODO 1.6989(17) . ? T1M OBM 1.6316(18) 1_455 ? T1M ODM 1.6430(17) . ? T1M OCM 1.6529(19) . ? T1M OA1 1.6584(16) 3_566 ? T2O ODM 1.6344(16) 3_666 ? T2O OBO 1.6430(17) . ? T2O OCM 1.6434(17) 2_545 ? T2O OA2 1.6640(15) 1_545 ? T2M OCO 1.6367(16) 2 ? T2M OBM 1.6384(18) . ? T2M ODO 1.6550(16) 3_666 ? T2M OA2 1.6731(16) . ? OA1 T1M 1.6584(16) 3_566 ? OA1 T1O 1.6976(16) 1_556 ? OA1 Ca 2.369(2) 1_556 ? OA1 Na 2.389(2) 3_556 ? OA1 Na 2.825(3) 1_556 ? OA1 Ca 2.880(2) 3_556 ? OA2 T2O 1.6640(15) 1_565 ? OA2 Na 2.335(2) 1_565 ? OA2 Ca 2.3437(19) 1_565 ? OBO T1O 1.6941(16) 1_655 ? OBO Ca 2.469(2) 3_655 ? OBO Na 2.490(2) 3_655 ? OBM T1M 1.6316(18) 1_655 ? OBM Ca 2.796(3) 3_665 ? OCO T2M 1.6367(16) 2_445 ? OCO Na 3.011(3) 2_455 ? OCM T2O 1.6434(17) 2_455 ? OCM Ca 2.699(2) 2_455 ? ODO T2M 1.6550(16) 3_666 ? ODM T2O 1.6344(16) 3_666 ? ODM Na 2.719(3) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OA2 Na OA1 149.06(12) 1_545 3_556 ? OA2 Na ODO 105.40(8) 1_545 . ? OA1 Na ODO 101.50(8) 3_556 . ? OA2 Na OBO 97.32(8) 1_545 3_655 ? OA1 Na OBO 65.32(6) 3_556 3_655 ? ODO Na OBO 148.30(11) . 3_655 ? OA2 Na ODM 111.54(10) 1_545 1_545 ? OA1 Na ODM 61.47(7) 3_556 1_545 ? ODO Na ODM 74.78(7) . 1_545 ? OBO Na ODM 117.04(9) 3_655 1_545 ? OA2 Na OA1 127.17(11) 1_545 1_554 ? OA1 Na OA1 79.96(8) 3_556 1_554 ? ODO Na OA1 59.72(7) . 1_554 ? OBO Na OA1 88.96(8) 3_655 1_554 ? ODM Na OA1 111.64(7) 1_545 1_554 ? OA2 Ca OA1 158.11(9) 1_545 1_554 ? OA2 Ca OBO 97.67(7) 1_545 3_655 ? OA1 Ca OBO 100.92(7) 1_554 3_655 ? OA2 Ca ODO 103.67(7) 1_545 . ? OA1 Ca ODO 65.88(6) 1_554 . ? OBO Ca ODO 146.18(8) 3_655 . ? OA2 Ca OCM 61.50(6) 1_545 2_545 ? OA1 Ca OCM 97.42(8) 1_554 2_545 ? OBO Ca OCM 129.50(8) 3_655 2_545 ? ODO Ca OCM 84.07(7) . 2_545 ? OA2 Ca OBM 113.47(8) 1_545 3_665 ? OA1 Ca OBM 60.32(6) 1_554 3_665 ? OBO Ca OBM 77.38(7) 3_655 3_665 ? ODO Ca OBM 116.19(7) . 3_665 ? OCM Ca OBM 71.88(7) 2_545 3_665 ? OA2 Ca OA1 120.93(8) 1_545 3_556 ? OA1 Ca OA1 79.13(7) 1_554 3_556 ? OBO Ca OA1 58.39(6) 3_655 3_556 ? ODO Ca OA1 88.01(7) . 3_556 ? OCM Ca OA1 172.07(8) 2_545 3_556 ? OBM Ca OA1 111.83(6) 3_665 3_556 ? OCO T1O OBO 112.07(9) . 1_455 ? OCO T1O OA1 116.73(9) . 1_554 ? OBO T1O OA1 101.91(8) 1_455 1_554 ? OCO T1O ODO 110.42(8) . . ? OBO T1O ODO 113.00(8) 1_455 . ? OA1 T1O ODO 102.19(9) 1_554 . ? OBM T1M ODM 112.89(10) 1_455 . ? OBM T1M OCM 110.96(10) 1_455 . ? ODM T1M OCM 109.27(9) . . ? OBM T1M OA1 105.63(10) 1_455 3_566 ? ODM T1M OA1 105.39(9) . 3_566 ? OCM T1M OA1 112.59(9) . 3_566 ? ODM T2O OBO 111.28(9) 3_666 . ? ODM T2O OCM 112.97(9) 3_666 2_545 ? OBO T2O OCM 112.01(9) . 2_545 ? ODM T2O OA2 108.02(9) 3_666 1_545 ? OBO T2O OA2 108.65(8) . 1_545 ? OCM T2O OA2 103.47(9) 2_545 1_545 ? OCO T2M OBM 110.92(9) 2 . ? OCO T2M ODO 113.07(8) 2 3_666 ? OBM T2M ODO 110.39(9) . 3_666 ? OCO T2M OA2 105.61(8) 2 . ? OBM T2M OA2 108.83(9) . . ? ODO T2M OA2 107.79(8) 3_666 . ? T1M OA1 T1O 140.37(12) 3_566 1_556 ? T1M OA1 Ca 104.69(9) 3_566 1_556 ? T1O OA1 Ca 98.14(8) 1_556 1_556 ? T1M OA1 Na 102.58(9) 3_566 3_556 ? T1O OA1 Na 98.15(9) 1_556 3_556 ? Ca OA1 Na 112.01(9) 1_556 3_556 ? T1M OA1 Na 118.28(10) 3_566 1_556 ? T1O OA1 Na 90.36(8) 1_556 1_556 ? Ca OA1 Na 15.60(4) 1_556 1_556 ? Na OA1 Na 100.04(8) 3_556 1_556 ? T1M OA1 Ca 115.90(8) 3_566 3_556 ? T1O OA1 Ca 90.41(7) 1_556 3_556 ? Ca OA1 Ca 100.87(7) 1_556 3_556 ? Na OA1 Ca 14.85(6) 3_556 3_556 ? Na OA1 Ca 87.47(6) 1_556 3_556 ? T2O OA2 T2M 127.06(9) 1_565 . ? T2O OA2 Na 121.51(10) 1_565 1_565 ? T2M OA2 Na 110.24(10) . 1_565 ? T2O OA2 Ca 103.98(8) 1_565 1_565 ? T2M OA2 Ca 128.93(9) . 1_565 ? Na OA2 Ca 20.62(6) 1_565 1_565 ? T2O OBO T1O 137.59(10) . 1_655 ? T2O OBO Ca 116.30(8) . 3_655 ? T1O OBO Ca 105.83(9) 1_655 3_655 ? T2O OBO Na 127.21(9) . 3_655 ? T1O OBO Na 94.55(8) 1_655 3_655 ? Ca OBO Na 19.44(5) 3_655 3_655 ? T1M OBM T2M 157.18(13) 1_655 . ? T1M OBM Ca 89.23(8) 1_655 3_665 ? T2M OBM Ca 110.98(9) . 3_665 ? T2M OCO T1O 131.04(11) 2_445 . ? T2M OCO Na 85.42(8) 2_445 2_455 ? T1O OCO Na 139.68(9) . 2_455 ? T2O OCM T1M 133.04(11) 2_455 . ? T2O OCM Ca 91.02(9) 2_455 2_455 ? T1M OCM Ca 134.76(9) . 2_455 ? T2M ODO T1O 132.98(11) 3_666 . ? T2M ODO Na 122.27(10) 3_666 . ? T1O ODO Na 104.52(9) . . ? T2M ODO Ca 132.19(9) 3_666 . ? T1O ODO Ca 93.77(8) . . ? Na ODO Ca 19.53(6) . . ? T2O ODM T1M 150.56(13) 3_666 . ? T2O ODM Na 117.85(9) 3_666 1_565 ? T1M ODM Na 90.55(8) . 1_565 ? data_An48plagioclase _audit_creation_date 2010-06-21T16:08:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_mineral "plagioclase, low" _chemical_formula_moiety 'Al1.5 Ca0.5 Na0.5 O8 Si2.5' _chemical_formula_sum 'Al1.5 Ca0.5 Na0.5 O8 Si2.5' _chemical_formula_weight 270 _chemical_compound_source 'R050104 from RT Downs, locality unknown' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_space_group_name_Hall '-C 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 8.1744(2) _cell_length_b 12.8638(3) _cell_length_c 7.1102(2) _cell_angle_alpha 93.525(2) _cell_angle_beta 116.2360(10) _cell_angle_gamma 89.915(2) _cell_volume 669.10(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_pressure 100(1) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 5.6 _cell_measurement_theta_max 9.6 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour none _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.68 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.28 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction)' _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.953 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'fine-focus sealed tube' _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_unetI/netI 0.0484 _diffrn_reflns_number 3499 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 1931 _reflns_number_gt 1505 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Crysalis (Oxford Diffraction)' _computing_cell_refinement 'Crysalis (Oxford Diffraction)' _computing_data_reduction 'Crysalis (Oxford Diffraction)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. This sample is a coherent Boggild intergrowth from which the diffraction maxima of the two phases cannot be distinguished. The refined model therefore represents some average structure of the (semi?)-coherently diffracting phases refined in C-1. The M site is modelled as a split site with free Na and Ca occupancies, following Johnson (MS thesis VT). The total M site occupancy corresponds to an electron number equal to that for Ca0.5Na0.5 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.3913P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_number_reflns 1931 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.531 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.151 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.2687(3) -0.0218(4) 0.1688(5) 0.0323(13) Uani 0.615(11) 1 d P . . Ca1 Ca 0.2705(2) 0.0285(2) 0.1017(4) 0.0243(7) Uani 0.437(6) 1 d P . . T1O Si 0.00644(9) 0.16455(6) 0.21388(11) 0.01655(16) Uani 1 1 d . . . T1M Si 0.00330(9) 0.81738(5) 0.23141(10) 0.01507(16) Uani 1 1 d . . . T2O Si 0.68614(9) 0.10928(5) 0.31736(11) 0.01359(15) Uani 1 1 d . . . T2M Si 0.68215(9) 0.87941(5) 0.35698(10) 0.01404(15) Uani 1 1 d . . . OA1 O 0.0030(3) 0.12955(16) 0.9793(3) 0.0246(4) Uani 1 1 d . . . OA2 O 0.5827(2) -0.00717(13) 0.2782(3) 0.0168(4) Uani 1 1 d . . . OBO O 0.8127(3) 0.10623(15) 0.1905(3) 0.0224(4) Uani 1 1 d . . . OBM O 0.8171(3) 0.85313(16) 0.2447(4) 0.0288(5) Uani 1 1 d . . . OCO O 0.0146(3) 0.29238(16) 0.2791(3) 0.0233(4) Uani 1 1 d . . . OCM O 0.0151(3) 0.68854(16) 0.2167(3) 0.0266(4) Uani 1 1 d . . . ODO O 0.1979(3) 0.10808(15) 0.3830(3) 0.0220(4) Uani 1 1 d . . . ODM O 0.1895(3) 0.86683(16) 0.4302(3) 0.0251(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na 0.0087(9) 0.062(3) 0.0226(14) -0.0231(16) 0.0067(8) -0.0089(10) Ca1 0.0137(6) 0.0282(11) 0.0238(9) -0.0068(7) 0.0029(5) 0.0040(5) T1O 0.0146(3) 0.0219(3) 0.0120(3) 0.0015(2) 0.0047(2) -0.0043(3) T1M 0.0138(3) 0.0201(3) 0.0101(3) 0.0002(2) 0.0043(2) 0.0057(2) T2O 0.0118(3) 0.0140(3) 0.0130(3) -0.0003(2) 0.0038(2) 0.0009(2) T2M 0.0125(3) 0.0155(3) 0.0127(3) 0.0021(2) 0.0042(2) -0.0007(2) OA1 0.0290(10) 0.0354(11) 0.0121(9) 0.0036(8) 0.0112(8) 0.0014(8) OA2 0.0162(8) 0.0162(8) 0.0161(8) 0.0028(6) 0.0052(7) -0.0016(6) OBO 0.0215(9) 0.0214(9) 0.0262(10) 0.0000(8) 0.0124(8) -0.0037(7) OBM 0.0233(10) 0.0256(10) 0.0422(13) -0.0031(9) 0.0195(10) 0.0024(8) OCO 0.0212(9) 0.0266(10) 0.0205(9) 0.0034(8) 0.0075(8) -0.0055(8) OCM 0.0227(10) 0.0284(11) 0.0197(9) -0.0048(8) 0.0020(8) 0.0111(8) ODO 0.0198(9) 0.0257(10) 0.0136(9) 0.0014(7) 0.0013(7) -0.0017(7) ODM 0.0204(9) 0.0271(10) 0.0171(9) -0.0040(7) -0.0007(7) 0.0012(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na Ca1 0.830(4) . ? Na OA2 2.334(3) . ? Na OA1 2.392(4) 3_556 ? Na ODO 2.431(3) . ? Na OBO 2.511(3) 3_655 ? Na ODM 2.706(6) 1_545 ? Na OA1 2.836(5) 1_554 ? Na T1O 3.134(2) 3 ? Na T1M 3.188(5) 1_545 ? Na T1O 3.308(4) . ? Na T2M 3.321(3) 1_545 ? Na T2O 3.495(3) . ? Ca1 OA2 2.353(2) . ? Ca1 OA1 2.383(3) 1_554 ? Ca1 OBO 2.468(2) 3_655 ? Ca1 ODO 2.489(3) . ? Ca1 OCM 2.696(3) 2_545 ? Ca1 OBM 2.793(4) 3_665 ? Ca1 OA1 2.862(3) 3_556 ? Ca1 T1O 3.1142(16) . ? Ca1 T2O 3.192(2) . ? Ca1 T1M 3.229(3) 3_565 ? Ca1 T1O 3.3411(19) 3 ? T1O OCO 1.674(2) . ? T1O OA1 1.688(2) 1_554 ? T1O OBO 1.6896(19) 1_455 ? T1O ODO 1.6921(19) . ? T1O Na 3.134(2) 3 ? T1O Ca1 3.3411(19) 3 ? T1M OBM 1.630(2) 1_455 ? T1M ODM 1.646(2) . ? T1M OCM 1.660(2) . ? T1M OA1 1.6647(19) 3_566 ? T1M Na 3.188(5) 1_565 ? T1M Ca1 3.229(3) 3_565 ? T2O ODM 1.633(2) 3_666 ? T2O OBO 1.645(2) . ? T2O OCM 1.646(2) 2_545 ? T2O OA2 1.6677(18) . ? T2O Ca1 3.5250(19) 3_655 ? T2M OCO 1.641(2) 2 ? T2M OBM 1.647(2) . ? T2M ODO 1.6635(19) 3_666 ? T2M OA2 1.6726(18) 1_565 ? T2M Na 3.321(3) 1_565 ? OA1 T1M 1.6647(19) 3_566 ? OA1 T1O 1.688(2) 1_556 ? OA1 Ca1 2.383(3) 1_556 ? OA1 Na 2.392(4) 3_556 ? OA1 Na 2.836(5) 1_556 ? OA1 Ca1 2.862(3) 3_556 ? OA2 T2M 1.6726(18) 1_545 ? OBO T1O 1.6896(19) 1_655 ? OBO Ca1 2.468(2) 3_655 ? OBO Na 2.511(3) 3_655 ? OBM T1M 1.630(2) 1_655 ? OBM Ca1 2.793(4) 3_665 ? OCO T2M 1.641(2) 2_445 ? OCM T2O 1.646(2) 2_455 ? OCM Ca1 2.696(3) 2_455 ? ODO T2M 1.6635(19) 3_666 ? ODM T2O 1.633(2) 3_666 ? ODM Na 2.706(6) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ca1 Na OA2 81.06(19) . . ? Ca1 Na OA1 116.6(3) . 3_556 ? OA2 Na OA1 148.3(2) . 3_556 ? Ca1 Na ODO 84.3(3) . . ? OA2 Na ODO 106.44(11) . . ? OA1 Na ODO 101.67(10) 3_556 . ? Ca1 Na OBO 77.5(2) . 3_655 ? OA2 Na OBO 96.80(9) . 3_655 ? OA1 Na OBO 64.66(8) 3_556 3_655 ? ODO Na OBO 147.8(2) . 3_655 ? Ca1 Na ODM 158.3(3) . 1_545 ? OA2 Na ODM 111.6(2) . 1_545 ? OA1 Na ODM 61.78(13) 3_556 1_545 ? ODO Na ODM 75.33(11) . 1_545 ? OBO Na ODM 116.62(19) 3_655 1_545 ? Ca1 Na OA1 49.5(3) . 1_554 ? OA2 Na OA1 127.7(2) . 1_554 ? OA1 Na OA1 79.66(10) 3_556 1_554 ? ODO Na OA1 59.26(11) . 1_554 ? OBO Na OA1 88.88(14) 3_655 1_554 ? ODM Na OA1 111.62(9) 1_545 1_554 ? Ca1 Na T1O 97.2(2) . 3 ? OA2 Na T1O 125.65(9) . 3 ? OA1 Na T1O 32.16(5) 3_556 3 ? ODO Na T1O 127.58(8) . 3 ? OBO Na T1O 32.52(5) 3_655 3 ? ODM Na T1O 89.50(13) 1_545 3 ? OA1 Na T1O 82.27(8) 1_554 3 ? Ca1 Na T1M 143.3(3) . 1_545 ? OA2 Na T1M 135.2(2) . 1_545 ? OA1 Na T1M 30.70(8) 3_556 1_545 ? ODO Na T1M 88.55(10) . 1_545 ? OBO Na T1M 90.40(11) 3_655 1_545 ? ODM Na T1M 31.09(7) 1_545 1_545 ? OA1 Na T1M 96.38(7) 1_554 1_545 ? T1O Na T1M 59.86(7) 3 1_545 ? Ca1 Na T1O 69.4(3) . . ? OA2 Na T1O 126.01(16) . . ? OA1 Na T1O 85.69(8) 3_556 . ? ODO Na T1O 29.57(6) . . ? OBO Na T1O 118.20(15) 3_655 . ? ODM Na T1O 88.99(7) 1_545 . ? OA1 Na T1O 30.70(5) 1_554 . ? T1O Na T1O 102.70(7) 3 . ? T1M Na T1O 87.08(5) 1_545 . ? Ca1 Na T2M 106.72(18) . 1_545 ? OA2 Na T2M 28.07(7) . 1_545 ? OA1 Na T2M 122.2(2) 3_556 1_545 ? ODO Na T2M 119.57(9) . 1_545 ? OBO Na T2M 91.30(8) 3_655 1_545 ? ODM Na T2M 90.10(16) 1_545 1_545 ? OA1 Na T2M 155.52(19) 1_554 1_545 ? T1O Na T2M 110.11(11) 3 1_545 ? T1M Na T2M 108.10(18) 1_545 1_545 ? T1O Na T2M 147.17(7) . 1_545 ? Ca1 Na T2O 62.08(17) . . ? OA2 Na T2O 24.20(7) . . ? OA1 Na T2O 169.27(9) 3_556 . ? ODO Na T2O 88.89(10) . . ? OBO Na T2O 105.24(11) 3_655 . ? ODM Na T2O 123.87(12) 1_545 . ? OA1 Na T2O 104.54(17) 1_554 . ? T1O Na T2O 137.72(9) 3 . ? T1M Na T2O 153.90(17) 1_545 . ? T1O Na T2O 103.00(12) . . ? T2M Na T2O 51.95(3) 1_545 . ? Na Ca1 OA2 78.53(18) . . ? Na Ca1 OA1 115.1(3) . 1_554 ? OA2 Ca1 OA1 157.86(12) . 1_554 ? Na Ca1 OBO 83.35(19) . 3_655 ? OA2 Ca1 OBO 97.50(8) . 3_655 ? OA1 Ca1 OBO 101.29(8) 1_554 3_655 ? Na Ca1 ODO 76.3(3) . . ? OA2 Ca1 ODO 104.01(9) . . ? OA1 Ca1 ODO 65.24(7) 1_554 . ? OBO Ca1 ODO 146.55(14) 3_655 . ? Na Ca1 OCM 129.2(2) . 2_545 ? OA2 Ca1 OCM 61.52(7) . 2_545 ? OA1 Ca1 OCM 97.19(11) 1_554 2_545 ? OBO Ca1 OCM 129.15(13) 3_655 2_545 ? ODO Ca1 OCM 83.99(8) . 2_545 ? Na Ca1 OBM 158.4(2) . 3_665 ? OA2 Ca1 OBM 113.51(13) . 3_665 ? OA1 Ca1 OBM 60.23(9) 1_554 3_665 ? OBO Ca1 OBM 77.44(9) 3_655 3_665 ? ODO Ca1 OBM 115.47(10) . 3_665 ? OCM Ca1 OBM 71.69(11) 2_545 3_665 ? Na Ca1 OA1 48.39(19) . 3_556 ? OA2 Ca1 OA1 121.03(13) . 3_556 ? OA1 Ca1 OA1 79.28(9) 1_554 3_556 ? OBO Ca1 OA1 58.43(7) 3_655 3_556 ? ODO Ca1 OA1 88.38(11) . 3_556 ? OCM Ca1 OA1 172.37(10) 2_545 3_556 ? OBM Ca1 OA1 111.67(8) 3_665 3_556 ? Na Ca1 T1O 96.1(3) . . ? OA2 Ca1 T1O 134.29(8) . . ? OA1 Ca1 T1O 32.44(5) 1_554 . ? OBO Ca1 T1O 127.26(7) 3_655 . ? ODO Ca1 T1O 32.80(5) . . ? OCM Ca1 T1O 91.18(7) 2_545 . ? OBM Ca1 T1O 87.82(7) 3_665 . ? OA1 Ca1 T1O 82.21(7) 3_556 . ? Na Ca1 T2O 104.63(18) . . ? OA2 Ca1 T2O 30.50(5) . . ? OA1 Ca1 T2O 128.04(11) 1_554 . ? OBO Ca1 T2O 115.80(8) 3_655 . ? ODO Ca1 T2O 95.10(6) . . ? OCM Ca1 T2O 31.03(5) 2_545 . ? OBM Ca1 T2O 92.70(10) 3_665 . ? OA1 Ca1 T2O 151.10(11) 3_556 . ? T1O Ca1 T2O 115.23(5) . . ? Na Ca1 T1M 140.6(2) . 3_565 ? OA2 Ca1 T1M 140.84(15) . 3_565 ? OA1 Ca1 T1M 29.95(6) 1_554 3_565 ? OBO Ca1 T1M 88.25(8) 3_655 3_565 ? ODO Ca1 T1M 90.86(6) . 3_565 ? OCM Ca1 T1M 84.90(10) 2_545 3_565 ? OBM Ca1 T1M 30.33(5) 3_665 3_565 ? OA1 Ca1 T1M 94.97(6) 3_556 3_565 ? T1O Ca1 T1M 59.61(4) . 3_565 ? T2O Ca1 T1M 113.62(10) . 3_565 ? Na Ca1 T1O 68.52(18) . 3 ? OA2 Ca1 T1O 116.83(8) . 3 ? OA1 Ca1 T1O 85.08(7) 1_554 3 ? OBO Ca1 T1O 29.18(5) 3_655 3 ? ODO Ca1 T1O 117.42(11) . 3 ? OCM Ca1 T1O 156.78(12) 2_545 3 ? OBM Ca1 T1O 89.87(7) 3_665 3 ? OA1 Ca1 T1O 30.35(4) 3_556 3 ? T1O Ca1 T1O 102.37(5) . 3 ? T2O Ca1 T1O 142.39(5) . 3 ? T1M Ca1 T1O 85.86(4) 3_565 3 ? OCO T1O OA1 116.90(10) . 1_554 ? OCO T1O OBO 111.85(10) . 1_455 ? OA1 T1O OBO 101.95(10) 1_554 1_455 ? OCO T1O ODO 110.37(10) . . ? OA1 T1O ODO 102.03(10) 1_554 . ? OBO T1O ODO 113.27(10) 1_455 . ? OCO T1O Ca1 130.52(9) . . ? OA1 T1O Ca1 49.20(8) 1_554 . ? OBO T1O Ca1 117.45(9) 1_455 . ? ODO T1O Ca1 52.84(8) . . ? OCO T1O Na 132.86(12) . 3 ? OA1 T1O Na 48.96(10) 1_554 3 ? OBO T1O Na 53.03(9) 1_455 3 ? ODO T1O Na 116.51(12) . 3 ? Ca1 T1O Na 78.46(5) . 3 ? OCO T1O Na 140.47(10) . . ? OA1 T1O Na 59.03(10) 1_554 . ? OBO T1O Na 107.14(10) 1_455 . ? ODO T1O Na 45.14(8) . . ? Ca1 T1O Na 14.45(5) . . ? Na T1O Na 77.30(7) 3 . ? OCO T1O Ca1 142.74(8) . 3 ? OA1 T1O Ca1 58.93(9) 1_554 3 ? OBO T1O Ca1 45.41(8) 1_455 3 ? ODO T1O Ca1 106.45(8) . 3 ? Ca1 T1O Ca1 77.63(5) . 3 ? Na T1O Ca1 14.28(7) 3 3 ? Na T1O Ca1 72.93(5) . 3 ? OBM T1M ODM 112.97(11) 1_455 . ? OBM T1M OCM 111.15(11) 1_455 . ? ODM T1M OCM 109.26(10) . . ? OBM T1M OA1 105.37(11) 1_455 3_566 ? ODM T1M OA1 105.25(11) . 3_566 ? OCM T1M OA1 112.71(11) . 3_566 ? OBM T1M Na 122.41(11) 1_455 1_565 ? ODM T1M Na 58.06(10) . 1_565 ? OCM T1M Na 125.76(10) . 1_565 ? OA1 T1M Na 47.20(10) 3_566 1_565 ? OBM T1M Ca1 59.86(10) 1_455 3_565 ? ODM T1M Ca1 119.01(9) . 3_565 ? OCM T1M Ca1 130.49(8) . 3_565 ? OA1 T1M Ca1 45.61(9) 3_566 3_565 ? Na T1M Ca1 76.01(5) 1_565 3_565 ? ODM T2O OBO 111.24(11) 3_666 . ? ODM T2O OCM 113.21(10) 3_666 2_545 ? OBO T2O OCM 112.02(11) . 2_545 ? ODM T2O OA2 108.30(10) 3_666 . ? OBO T2O OA2 108.30(10) . . ? OCM T2O OA2 103.31(10) 2_545 . ? ODM T2O Ca1 125.12(10) 3_666 . ? OBO T2O Ca1 122.32(9) . . ? OCM T2O Ca1 57.60(9) 2_545 . ? OA2 T2O Ca1 45.72(8) . . ? ODM T2O Na 115.95(10) 3_666 . ? OBO T2O Na 127.34(8) . . ? OCM T2O Na 68.93(12) 2_545 . ? OA2 T2O Na 35.00(10) . . ? Ca1 T2O Na 13.29(5) . . ? ODM T2O Ca1 137.19(8) 3_666 3_655 ? OBO T2O Ca1 38.78(8) . 3_655 ? OCM T2O Ca1 107.94(8) 2_545 3_655 ? OA2 T2O Ca1 72.07(8) . 3_655 ? Ca1 T2O Ca1 86.83(6) . 3_655 ? Na T2O Ca1 89.17(5) . 3_655 ? OCO T2M OBM 111.04(11) 2 . ? OCO T2M ODO 112.78(10) 2 3_666 ? OBM T2M ODO 110.48(11) . 3_666 ? OCO T2M OA2 105.60(10) 2 1_565 ? OBM T2M OA2 108.95(10) . 1_565 ? ODO T2M OA2 107.76(10) 3_666 1_565 ? OCO T2M Na 65.46(11) 2 1_565 ? OBM T2M Na 131.05(11) . 1_565 ? ODO T2M Na 115.42(9) 3_666 1_565 ? OA2 T2M Na 41.04(11) 1_565 1_565 ? T1M OA1 T1O 140.38(14) 3_566 1_556 ? T1M OA1 Ca1 104.45(12) 3_566 1_556 ? T1O OA1 Ca1 98.36(10) 1_556 1_556 ? T1M OA1 Na 102.10(15) 3_566 3_556 ? T1O OA1 Na 98.87(11) 1_556 3_556 ? Ca1 OA1 Na 111.69(12) 1_556 3_556 ? T1M OA1 Na 118.09(12) 3_566 1_556 ? T1O OA1 Na 90.27(9) 1_556 1_556 ? Ca1 OA1 Na 15.38(5) 1_556 1_556 ? Na OA1 Na 100.34(10) 3_556 1_556 ? T1M OA1 Ca1 115.73(11) 3_566 3_556 ? T1O OA1 Ca1 90.72(9) 1_556 3_556 ? Ca1 OA1 Ca1 100.72(9) 1_556 3_556 ? Na OA1 Ca1 15.04(10) 3_556 3_556 ? Na OA1 Ca1 87.81(8) 1_556 3_556 ? T2O OA2 T2M 126.98(11) . 1_545 ? T2O OA2 Na 120.80(17) . . ? T2M OA2 Na 110.89(17) 1_545 . ? T2O OA2 Ca1 103.79(11) . . ? T2M OA2 Ca1 129.19(12) 1_545 . ? Na OA2 Ca1 20.41(9) . . ? T2O OBO T1O 137.76(13) . 1_655 ? T2O OBO Ca1 116.55(12) . 3_655 ? T1O OBO Ca1 105.41(11) 1_655 3_655 ? T2O OBO Na 127.14(12) . 3_655 ? T1O OBO Na 94.45(12) 1_655 3_655 ? Ca1 OBO Na 19.17(8) 3_655 3_655 ? T1M OBM T2M 156.78(16) 1_655 . ? T1M OBM Ca1 89.82(10) 1_655 3_665 ? T2M OBM Ca1 110.85(10) . 3_665 ? T2M OCO T1O 131.15(13) 2_445 . ? T2O OCM T1M 132.54(14) 2_455 . ? T2O OCM Ca1 91.37(10) 2_455 2_455 ? T1M OCM Ca1 134.88(11) . 2_455 ? T2M ODO T1O 132.73(13) 3_666 . ? T2M ODO Na 121.76(14) 3_666 . ? T1O ODO Na 105.30(13) . . ? T2M ODO Ca1 131.89(11) 3_666 . ? T1O ODO Ca1 94.35(9) . . ? Na ODO Ca1 19.39(9) . . ? T2O ODM T1M 150.54(15) 3_666 . ? T2O ODM Na 117.45(11) 3_666 1_565 ? T1M ODM Na 90.86(10) . 1_565 ? data_An60plagioclase _audit_creation_date 2010-06-21T14:24:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_mineral "plagioclase, low" _chemical_formula_moiety 'Al1.6 Ca0.6 Na0.4 O8 Si2.4' _chemical_formula_sum 'Al1.6 Ca0.6 Na0.4 O8 Si2.4' _chemical_formula_weight 271.8 _chemical_compound_source ; Smithsonian Institution, Washington Sample #166853 ; #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'I -1' _symmetry_space_group_name_Hall '-I 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z+1/2' '-x, -y, -z' '-x+1/2, -y+1/2, -z+1/2' _cell_length_a 8.1717(2) _cell_length_b 12.8752(2) _cell_length_c 14.2074(3) _cell_angle_alpha 93.4530(10) _cell_angle_beta 116.0780(10) _cell_angle_gamma 91.4250(10) _cell_volume 1337.98(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_pressure 100(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 6.1 _cell_measurement_theta_max 9.8 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.217 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.133 _exptl_crystal_density_diffrn 2.68 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1077 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.44 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'CrysAlis (Oxford Diffraction)' _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.863 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'fine-focus sealed tube' _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_number 6606 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 30.36 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.946 _reflns_number_total 3822 _reflns_number_gt 1720 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Crysalis (Oxford Diffraction, 2006)' _computing_cell_refinement 'Crysalis (Oxford Diffraction, 2006)' _computing_data_reduction 'Crysalis (Oxford Diffraction, 2006)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure model is the "I-1 split-Ca model" of Angel et al (1990), with Al and Si disordered over the T sites, but full occupancies allocated for simplicity. The M sites are split in two, and assigned Ca scattering factors and their occupancies refined independently. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0195(7) _refine_ls_number_reflns 3822 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.089 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 0.524 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.133 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group MOO Ca 0.2671(4) 0.9783(7) 0.0852(4) 0.0395(17) Uani 0.316(8) 1 d P . . MZO Ca 0.2735(4) 1.0321(3) 0.5461(3) 0.0169(8) Uani 0.393(10) 1 d P . . MOI Ca 0.7714(3) 0.5277(3) 0.5511(2) 0.0294(10) Uani 0.519(8) 1 d P . . MZI Ca 0.7670(3) 0.4909(7) 0.0794(5) 0.051(2) Uani 0.441(10) 1 d P . . T1OO Si 0.00590(13) 0.16331(7) 0.10756(8) 0.0147(2) Uani 1 1 d . . . T1OZ Al 0.00694(12) 0.16339(7) 0.60757(7) 0.0087(2) Uani 1 1 d . . . T1MO Al 0.00334(12) 0.81645(7) 0.11584(8) 0.0083(2) Uani 1 1 d . . . T1MZ Si 0.00227(13) 0.81591(7) 0.61519(8) 0.0141(2) Uani 1 1 d . . . T2OO Al 0.68541(12) 0.10885(6) 0.15913(8) 0.0080(2) Uani 1 1 d . . . T2OZ Si 0.68504(12) 0.10892(7) 0.65897(8) 0.0140(2) Uani 1 1 d . . . T2MO Si 0.68119(12) 0.87882(6) 0.17848(8) 0.0129(2) Uani 1 1 d . . . T2MZ Al 0.68141(12) 0.87870(6) 0.67849(8) 0.0080(2) Uani 1 1 d . . . OA1O O 0.0037(3) 0.12858(17) -0.01012(17) 0.0232(6) Uani 1 1 d . . . OA1Z O 0.0044(3) 0.13004(17) 0.49098(17) 0.0216(6) Uani 1 1 d . . . OA2O O 0.5799(3) 0.99270(14) 0.13914(17) 0.0167(5) Uani 1 1 d . . . OA2Z O 0.5811(3) 0.99006(14) 0.63950(17) 0.0163(5) Uani 1 1 d . . . OBOO O 0.8126(3) 0.10339(16) 0.09536(19) 0.0225(6) Uani 1 1 d . . . OBOZ O 0.8138(3) 0.10475(16) 0.59434(19) 0.0227(6) Uani 1 1 d . . . OBMO O 0.8172(3) 0.85265(16) 0.1213(2) 0.0276(6) Uani 1 1 d . . . OBMZ O 0.8137(3) 0.85321(17) 0.6226(2) 0.0293(7) Uani 1 1 d . . . OCOO O 0.0144(3) 0.29010(17) 0.14084(19) 0.0242(6) Uani 1 1 d . . . OCOZ O 0.0149(3) 0.28941(15) 0.64143(18) 0.0199(5) Uani 1 1 d . . . OCMO O 0.0114(3) 0.68713(16) 0.10671(18) 0.0204(5) Uani 1 1 d . . . OCMZ O 0.0134(3) 0.68699(16) 0.6064(2) 0.0236(6) Uani 1 1 d . . . ODOO O 0.1974(3) 0.10777(15) 0.19193(18) 0.0214(6) Uani 1 1 d . . . ODOZ O 0.1975(3) 0.10678(16) 0.69088(18) 0.0207(6) Uani 1 1 d . . . ODMO O 0.1902(3) 0.86650(16) 0.21388(19) 0.0242(6) Uani 1 1 d . . . ODMZ O 0.1902(3) 0.86598(17) 0.7158(2) 0.0281(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 MOO 0.0218(15) 0.067(4) 0.028(2) -0.023(2) 0.0139(14) -0.0211(15) MZO 0.0134(10) 0.0231(15) 0.0092(10) -0.0008(9) 0.0004(7) 0.0059(8) MOI 0.0115(8) 0.0338(15) 0.0356(14) -0.0157(11) 0.0058(8) 0.0042(7) MZI 0.0140(11) 0.089(4) 0.042(3) -0.035(3) 0.0106(12) -0.0063(13) T1OO 0.0137(5) 0.0164(5) 0.0129(5) 0.0012(4) 0.0051(4) -0.0014(4) T1OZ 0.0089(5) 0.0099(5) 0.0070(5) 0.0003(4) 0.0036(4) -0.0036(4) T1MO 0.0073(5) 0.0118(5) 0.0066(5) 0.0007(4) 0.0034(4) 0.0053(4) T1MZ 0.0147(5) 0.0160(5) 0.0100(5) 0.0007(4) 0.0040(4) 0.0021(4) T2OO 0.0064(5) 0.0070(5) 0.0093(5) 0.0002(4) 0.0023(4) 0.0000(4) T2OZ 0.0131(5) 0.0135(5) 0.0141(5) 0.0005(4) 0.0047(4) 0.0012(4) T2MO 0.0130(5) 0.0114(5) 0.0140(5) 0.0012(4) 0.0056(4) 0.0002(4) T2MZ 0.0062(5) 0.0085(5) 0.0083(5) 0.0019(4) 0.0022(4) 0.0007(4) OA1O 0.0336(17) 0.0261(13) 0.0140(14) 0.0021(11) 0.0143(13) 0.0029(11) OA1Z 0.0280(16) 0.0270(13) 0.0123(14) 0.0059(11) 0.0105(12) 0.0039(10) OA2O 0.0159(13) 0.0130(12) 0.0194(14) 0.0061(10) 0.0055(11) 0.0047(10) OA2Z 0.0143(13) 0.0151(12) 0.0176(14) 0.0004(10) 0.0058(11) -0.0040(10) OBOO 0.0234(15) 0.0185(12) 0.0290(16) -0.0015(11) 0.0152(13) -0.0038(10) OBOZ 0.0238(15) 0.0192(13) 0.0283(16) -0.0007(11) 0.0150(13) -0.0012(11) OBMO 0.0225(15) 0.0252(14) 0.0377(17) -0.0056(12) 0.0166(13) 0.0007(11) OBMZ 0.0227(15) 0.0296(15) 0.0415(18) 0.0000(13) 0.0198(14) 0.0031(12) OCOO 0.0228(14) 0.0230(14) 0.0237(16) 0.0031(12) 0.0075(12) -0.0012(11) OCOZ 0.0195(13) 0.0183(12) 0.0242(15) 0.0010(11) 0.0123(12) -0.0059(10) OCMO 0.0173(13) 0.0218(13) 0.0153(13) -0.0026(10) 0.0013(10) 0.0058(10) OCMZ 0.0236(15) 0.0227(14) 0.0212(15) -0.0008(11) 0.0070(12) 0.0060(11) ODOO 0.0223(15) 0.0167(12) 0.0173(15) 0.0010(11) 0.0015(12) 0.0023(10) ODOZ 0.0198(14) 0.0243(13) 0.0134(14) 0.0025(11) 0.0032(11) 0.0004(10) ODMO 0.0206(14) 0.0240(13) 0.0173(14) -0.0054(11) -0.0004(12) 0.0029(10) ODMZ 0.0227(15) 0.0255(14) 0.0248(17) 0.0000(12) 0.0005(13) 0.0011(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag MOO MOI 0.831(5) 2_454 ? MOO OA2O 2.323(3) . ? MOO OA1O 2.350(5) 3_565 ? MOO ODOO 2.430(4) 1_565 ? MOO OBOO 2.506(4) 3_665 ? MOO ODMO 2.663(8) . ? MOO OA1O 2.858(8) 1_565 ? MOO T1OO 3.102(3) 3_565 ? MOO OCOZ 3.116(8) 2_554 ? MOO T1MO 3.145(7) . ? MOO T1OO 3.330(6) 1_565 ? MOO T2MO 3.365(6) . ? MZO MZI 0.747(7) 2_455 ? MZO OA2Z 2.365(3) . ? MZO OA1Z 2.405(3) 1_565 ? MZO OBOZ 2.421(3) 3_666 ? MZO ODOZ 2.540(4) 1_565 ? MZO OCMO 2.575(5) 2 ? MZO OBMZ 2.722(5) 3_676 ? MZO OA1Z 2.894(5) 3_566 ? MZO T2OZ 3.124(4) 1_565 ? MZO T1OZ 3.169(3) 1_565 ? MZO T1MZ 3.221(3) 3_576 ? MZO T1OZ 3.318(3) 3_566 ? MOI MOO 0.831(5) 2_545 ? MOI OA2O 2.340(3) 2_545 ? MOI OA1O 2.415(3) 2 ? MOI OBOO 2.432(3) 4_655 ? MOI ODOO 2.505(3) 2 ? MOI OCMZ 2.641(4) 1_655 ? MOI OBMO 2.801(5) 4_665 ? MOI OA1O 2.815(4) 4 ? MOI T1OO 3.154(2) 2 ? MOI T2OO 3.156(3) 2 ? MOI T1MO 3.288(4) 4_565 ? MOI T1OO 3.291(3) 4 ? MZI MZO 0.747(7) 2_544 ? MZI OA2Z 2.322(3) 2_544 ? MZI ODOZ 2.367(3) 2_554 ? MZI OA1Z 2.457(6) 4 ? MZI OBOZ 2.491(4) 4_655 ? MZI OA1Z 2.736(8) 2_554 ? MZI ODMZ 2.852(11) 2_544 ? MZI OCMO 3.077(8) 1_655 ? MZI T1OZ 3.151(3) 4 ? MZI T1OZ 3.238(5) 2_554 ? MZI T1MZ 3.298(9) 2_544 ? MZI T2OZ 3.376(4) 2_554 ? T1OO OCOO 1.663(2) . ? T1OO OBOO 1.674(2) 1_455 ? T1OO OA1O 1.697(2) . ? T1OO ODOO 1.705(2) . ? T1OZ OCOZ 1.656(2) . ? T1OZ OBOZ 1.661(2) 1_455 ? T1OZ OA1Z 1.677(2) . ? T1OZ ODOZ 1.702(2) . ? T1MO ODMO 1.631(2) . ? T1MO OBMO 1.634(2) 1_455 ? T1MO OCMO 1.667(2) . ? T1MO OA1O 1.678(2) 3_565 ? T1MZ ODMZ 1.651(3) . ? T1MZ OCMZ 1.665(2) . ? T1MZ OBMZ 1.671(2) 1_455 ? T1MZ OA1Z 1.679(2) 3_566 ? T2OO ODMZ 1.619(3) 3_666 ? T2OO OA2O 1.652(2) 1_545 ? T2OO OBOO 1.652(2) . ? T2OO OCMZ 1.669(2) 2_544 ? T2OZ ODMO 1.643(2) 3_666 ? T2OZ OBOZ 1.673(2) . ? T2OZ OCMO 1.678(2) 2_545 ? T2OZ OA2Z 1.679(2) 1_545 ? T2MO OCOZ 1.634(2) 2_554 ? T2MO OBMO 1.670(2) . ? T2MO ODOZ 1.671(2) 3_666 ? T2MO OA2O 1.7028(19) . ? T2MZ OBMZ 1.627(2) . ? T2MZ OCOO 1.630(2) 2 ? T2MZ ODOO 1.658(2) 3_666 ? T2MZ OA2Z 1.670(2) . ? OA1O T1MO 1.678(2) 3_565 ? OA1O MOO 2.350(5) 3_565 ? OA1O MOI 2.415(3) 2_444 ? OA1O MOI 2.815(4) 4 ? OA1O MOO 2.858(8) 1_545 ? OA1Z T1MZ 1.679(2) 3_566 ? OA1Z MZO 2.405(3) 1_545 ? OA1Z MZI 2.457(6) 4 ? OA1Z MZI 2.736(8) 2_445 ? OA1Z MZO 2.894(5) 3_566 ? OA2O T2OO 1.652(2) 1_565 ? OA2O MOI 2.340(3) 2_454 ? OA2Z T2OZ 1.679(2) 1_565 ? OA2Z MZI 2.322(3) 2_455 ? OBOO T1OO 1.674(2) 1_655 ? OBOO MOI 2.432(3) 4_655 ? OBOO MOO 2.506(4) 3_665 ? OBOZ T1OZ 1.661(2) 1_655 ? OBOZ MZO 2.421(3) 3_666 ? OBOZ MZI 2.491(4) 4_655 ? OBMO T1MO 1.634(2) 1_655 ? OBMO MOI 2.801(5) 4_665 ? OBMZ T1MZ 1.671(2) 1_655 ? OBMZ MZO 2.722(5) 3_676 ? OCOO T2MZ 1.630(2) 2_444 ? OCOZ T2MO 1.634(2) 2_445 ? OCOZ MOO 3.116(8) 2_445 ? OCMO T2OZ 1.678(2) 2_454 ? OCMO MZO 2.575(5) 2_444 ? OCMO MZI 3.077(8) 1_455 ? OCMZ T2OO 1.669(2) 2_455 ? OCMZ MOI 2.641(4) 1_455 ? ODOO T2MZ 1.658(2) 3_666 ? ODOO MOO 2.430(4) 1_545 ? ODOO MOI 2.505(3) 2_444 ? ODOZ T2MO 1.671(2) 3_666 ? ODOZ MZI 2.367(3) 2_445 ? ODOZ MZO 2.540(4) 1_545 ? ODMO T2OZ 1.643(2) 3_666 ? ODMZ T2OO 1.619(3) 3_666 ? ODMZ MZI 2.852(11) 2_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MOI MOO OA2O 80.9(2) 2_454 . ? MOI MOO OA1O 115.9(4) 2_454 3_565 ? OA2O MOO OA1O 147.7(3) . 3_565 ? MOI MOO ODOO 85.4(5) 2_454 1_565 ? OA2O MOO ODOO 107.45(15) . 1_565 ? OA1O MOO ODOO 101.49(13) 3_565 1_565 ? MOI MOO OBOO 75.3(3) 2_454 3_665 ? OA2O MOO OBOO 95.70(13) . 3_665 ? OA1O MOO OBOO 65.29(10) 3_565 3_665 ? ODOO MOO OBOO 147.1(3) 1_565 3_665 ? MOI MOO ODMO 160.4(5) 2_454 . ? OA2O MOO ODMO 110.6(3) . . ? OA1O MOO ODMO 62.78(19) 3_565 . ? ODOO MOO ODMO 76.04(15) 1_565 . ? OBOO MOO ODMO 117.7(3) 3_665 . ? MOI MOO OA1O 50.4(4) 2_454 1_565 ? OA2O MOO OA1O 128.4(4) . 1_565 ? OA1O MOO OA1O 79.17(16) 3_565 1_565 ? ODOO MOO OA1O 59.07(17) 1_565 1_565 ? OBOO MOO OA1O 88.3(2) 3_665 1_565 ? ODMO MOO OA1O 112.64(12) . 1_565 ? MOI MOO T1OO 95.7(3) 2_454 3_565 ? OA2O MOO T1OO 124.40(14) . 3_565 ? OA1O MOO T1OO 32.72(7) 3_565 3_565 ? ODOO MOO T1OO 127.72(14) 1_565 3_565 ? OBOO MOO T1OO 32.58(6) 3_665 3_565 ? ODMO MOO T1OO 90.63(19) . 3_565 ? OA1O MOO T1OO 81.95(14) 1_565 3_565 ? MOI MOO OCOZ 127.5(3) 2_454 2_554 ? OA2O MOO OCOZ 56.39(15) . 2_554 ? OA1O MOO OCOZ 93.2(3) 3_565 2_554 ? ODOO MOO OCOZ 132.6(3) 1_565 2_554 ? OBOO MOO OCOZ 79.76(16) 3_665 2_554 ? ODMO MOO OCOZ 71.3(2) . 2_554 ? OA1O MOO OCOZ 167.75(13) 1_565 2_554 ? T1OO MOO OCOZ 86.49(17) 3_565 2_554 ? MOI MOO T1MO 144.2(4) 2_454 . ? OA2O MOO T1MO 134.2(4) . . ? OA1O MOO T1MO 31.54(11) 3_565 . ? ODOO MOO T1MO 88.75(14) 1_565 . ? OBOO MOO T1MO 91.55(16) 3_665 . ? ODMO MOO T1MO 31.24(9) . . ? OA1O MOO T1MO 96.92(10) 1_565 . ? T1OO MOO T1MO 60.95(10) 3_565 . ? OCOZ MOO T1MO 80.8(2) 2_554 . ? MOI MOO T1OO 70.7(5) 2_454 1_565 ? OA2O MOO T1OO 127.1(2) . 1_565 ? OA1O MOO T1OO 85.22(12) 3_565 1_565 ? ODOO MOO T1OO 29.49(10) 1_565 1_565 ? OBOO MOO T1OO 117.7(2) 3_665 1_565 ? ODMO MOO T1OO 89.85(9) . 1_565 ? OA1O MOO T1OO 30.63(8) 1_565 1_565 ? T1OO MOO T1OO 102.56(13) 3_565 1_565 ? OCOZ MOO T1OO 159.4(2) 2_554 1_565 ? T1MO MOO T1OO 87.37(7) . 1_565 ? MOI MOO T2MO 106.2(3) 2_454 . ? OA2O MOO T2MO 27.86(11) . . ? OA1O MOO T2MO 122.0(3) 3_565 . ? ODOO MOO T2MO 120.49(14) 1_565 . ? OBOO MOO T2MO 90.74(13) 3_665 . ? ODMO MOO T2MO 89.1(2) . . ? OA1O MOO T2MO 155.9(3) 1_565 . ? T1OO MOO T2MO 109.32(17) 3_565 . ? OCOZ MOO T2MO 28.88(7) 2_554 . ? T1MO MOO T2MO 107.2(3) . . ? T1OO MOO T2MO 148.11(11) 1_565 . ? MZI MZO OA2Z 77.6(3) 2_455 . ? MZI MZO OA1Z 108.5(5) 2_455 1_565 ? OA2Z MZO OA1Z 159.79(15) . 1_565 ? MZI MZO OBOZ 86.6(3) 2_455 3_666 ? OA2Z MZO OBOZ 96.91(11) . 3_666 ? OA1Z MZO OBOZ 102.60(11) 1_565 3_666 ? MZI MZO ODOZ 68.2(4) 2_455 1_565 ? OA2Z MZO ODOZ 102.90(13) . 1_565 ? OA1Z MZO ODOZ 63.75(10) 1_565 1_565 ? OBOZ MZO ODOZ 143.3(2) 3_666 1_565 ? MZI MZO OCMO 126.3(3) 2_455 2 ? OA2Z MZO OCMO 64.40(11) . 2 ? OA1Z MZO OCMO 97.94(13) 1_565 2 ? OBOZ MZO OCMO 132.3(2) 3_666 2 ? ODOZ MZO OCMO 84.33(10) 1_565 2 ? MZI MZO OBMZ 160.0(4) 2_455 3_676 ? OA2Z MZO OBMZ 117.8(2) . 3_676 ? OA1Z MZO OBMZ 61.76(10) 1_565 3_676 ? OBOZ MZO OBMZ 79.23(13) 3_666 3_676 ? ODOZ MZO OBMZ 116.48(12) 1_565 3_676 ? OCMO MZO OBMZ 73.50(15) 2 3_676 ? MZI MZO OA1Z 47.9(4) 2_455 3_566 ? OA2Z MZO OA1Z 117.12(15) . 3_566 ? OA1Z MZO OA1Z 78.54(13) 1_565 3_566 ? OBOZ MZO OA1Z 57.62(10) 3_666 3_566 ? ODOZ MZO OA1Z 85.79(16) 1_565 3_566 ? OCMO MZO OA1Z 170.06(17) 2 3_566 ? OBMZ MZO OA1Z 112.13(10) 3_676 3_566 ? MZI MZO T2OZ 103.3(3) 2_455 1_565 ? OA2Z MZO T2OZ 31.97(7) . 1_565 ? OA1Z MZO T2OZ 129.96(15) 1_565 1_565 ? OBOZ MZO T2OZ 117.01(13) 3_666 1_565 ? ODOZ MZO T2OZ 95.23(9) 1_565 1_565 ? OCMO MZO T2OZ 32.46(6) 2 1_565 ? OBMZ MZO T2OZ 95.67(16) 3_676 1_565 ? OA1Z MZO T2OZ 148.43(13) 3_566 1_565 ? MZI MZO T1OZ 88.6(5) 2_455 1_565 ? OA2Z MZO T1OZ 133.60(12) . 1_565 ? OA1Z MZO T1OZ 31.37(7) 1_565 1_565 ? OBOZ MZO T1OZ 126.60(12) 3_666 1_565 ? ODOZ MZO T1OZ 32.37(6) 1_565 1_565 ? OCMO MZO T1OZ 91.39(9) 2 1_565 ? OBMZ MZO T1OZ 88.62(8) 3_676 1_565 ? OA1Z MZO T1OZ 80.77(11) 3_566 1_565 ? T2OZ MZO T1OZ 115.83(8) 1_565 1_565 ? MZI MZO T1MZ 136.4(5) 2_455 3_576 ? OA2Z MZO T1MZ 145.8(2) . 3_576 ? OA1Z MZO T1MZ 30.56(7) 1_565 3_576 ? OBOZ MZO T1MZ 90.26(10) 3_666 3_576 ? ODOZ MZO T1MZ 90.33(8) 1_565 3_576 ? OCMO MZO T1MZ 86.18(12) 2 3_576 ? OBMZ MZO T1MZ 31.23(6) 3_676 3_576 ? OA1Z MZO T1MZ 94.93(8) 3_566 3_576 ? T2OZ MZO T1MZ 116.59(15) 1_565 3_576 ? T1OZ MZO T1MZ 59.27(5) 1_565 3_576 ? MZI MZO T1OZ 70.7(3) 2_455 3_566 ? OA2Z MZO T1OZ 114.77(11) . 3_566 ? OA1Z MZO T1OZ 85.26(10) 1_565 3_566 ? OBOZ MZO T1OZ 28.56(7) 3_666 3_566 ? ODOZ MZO T1OZ 114.96(17) 1_565 3_566 ? OCMO MZO T1OZ 159.39(19) 2 3_566 ? OBMZ MZO T1OZ 90.49(9) 3_676 3_566 ? OA1Z MZO T1OZ 30.35(6) 3_566 3_566 ? T2OZ MZO T1OZ 142.41(9) 1_565 3_566 ? T1OZ MZO T1OZ 101.32(10) 1_565 3_566 ? T1MZ MZO T1OZ 86.50(6) 3_576 3_566 ? MOO MOI OA2O 78.5(3) 2_545 2_545 ? MOO MOI OA1O 114.2(4) 2_545 2 ? OA2O MOI OA1O 158.25(16) 2_545 2 ? MOO MOI OBOO 85.4(3) 2_545 4_655 ? OA2O MOI OBOO 97.27(9) 2_545 4_655 ? OA1O MOI OBOO 101.18(10) 2 4_655 ? MOO MOI ODOO 75.2(4) 2_545 2 ? OA2O MOI ODOO 104.49(12) 2_545 2 ? OA1O MOI ODOO 64.69(8) 2 2 ? OBOO MOI ODOO 147.05(18) 4_655 2 ? MOO MOI OCMZ 129.6(3) 2_545 1_655 ? OA2O MOI OCMZ 62.57(9) 2_545 1_655 ? OA1O MOI OCMZ 96.67(14) 2 1_655 ? OBOO MOI OCMZ 127.99(18) 4_655 1_655 ? ODOO MOI OCMZ 84.42(9) 2 1_655 ? MOO MOI OBMO 158.9(3) 2_545 4_665 ? OA2O MOI OBMO 114.88(18) 2_545 4_665 ? OA1O MOI OBMO 59.22(11) 2 4_665 ? OBOO MOI OBMO 77.00(12) 4_655 4_665 ? ODOO MOI OBMO 114.24(12) 2 4_665 ? OCMZ MOI OBMO 71.28(14) 1_655 4_665 ? MOO MOI OA1O 48.7(3) 2_545 4 ? OA2O MOI OA1O 120.78(17) 2_545 4 ? OA1O MOI OA1O 79.02(10) 2 4 ? OBOO MOI OA1O 59.45(9) 4_655 4 ? ODOO MOI OA1O 87.99(14) 2 4 ? OCMZ MOI OA1O 172.33(12) 1_655 4 ? OBMO MOI OA1O 111.14(9) 4_665 4 ? MOO MOI T1OO 94.9(4) 2_545 2 ? OA2O MOI T1OO 134.72(10) 2_545 2 ? OA1O MOI T1OO 32.13(6) 2 2 ? OBOO MOI T1OO 127.13(9) 4_655 2 ? ODOO MOI T1OO 32.58(5) 2 2 ? OCMZ MOI T1OO 91.28(8) 1_655 2 ? OBMO MOI T1OO 86.68(9) 4_665 2 ? OA1O MOI T1OO 81.70(9) 4 2 ? MOO MOI T2OO 104.4(3) 2_545 2 ? OA2O MOI T2OO 30.66(6) 2_545 2 ? OA1O MOI T2OO 128.33(15) 2 2 ? OBOO MOI T2OO 115.26(10) 4_655 2 ? ODOO MOI T2OO 95.50(8) 2 2 ? OCMZ MOI T2OO 31.91(6) 1_655 2 ? OBMO MOI T2OO 93.68(14) 4_665 2 ? OA1O MOI T2OO 150.98(14) 4 2 ? T1OO MOI T2OO 115.71(7) 2 2 ? MOO MOI T1MO 139.8(4) 2_545 4_565 ? OA2O MOI T1MO 141.7(2) 2_545 4_565 ? OA1O MOI T1MO 29.46(7) 2 4_565 ? OBOO MOI T1MO 88.05(10) 4_655 4_565 ? ODOO MOI T1MO 89.88(8) 2 4_565 ? OCMZ MOI T1MO 84.30(13) 1_655 4_565 ? OBMO MOI T1MO 29.80(6) 4_665 4_565 ? OA1O MOI T1MO 94.62(7) 4 4_565 ? T1OO MOI T1MO 58.88(4) 2 4_565 ? T2OO MOI T1MO 114.15(14) 2 4_565 ? MOO MOI T1OO 69.7(3) 2_545 4 ? OA2O MOI T1OO 116.42(10) 2_545 4 ? OA1O MOI T1OO 85.12(8) 2 4 ? OBOO MOI T1OO 29.42(6) 4_655 4 ? ODOO MOI T1OO 117.64(14) 2 4 ? OCMZ MOI T1OO 155.74(17) 1_655 4 ? OBMO MOI T1OO 89.34(8) 4_665 4 ? OA1O MOI T1OO 31.04(5) 4 4 ? T1OO MOI T1OO 102.32(7) 2 4 ? T2OO MOI T1OO 141.96(6) 2 4 ? T1MO MOI T1OO 85.71(5) 4_565 4 ? MZO MZI OA2Z 84.1(3) 2_544 2_544 ? MZO MZI ODOZ 94.7(6) 2_544 2_554 ? OA2Z MZI ODOZ 109.85(12) 2_544 2_554 ? MZO MZI OA1Z 119.0(5) 2_544 4 ? OA2Z MZI OA1Z 140.3(4) 2_544 4 ? ODOZ MZI OA1Z 100.45(16) 2_554 4 ? MZO MZI OBOZ 75.9(4) 2_544 4_655 ? OA2Z MZI OBOZ 96.10(12) 2_544 4_655 ? ODOZ MZI OBOZ 151.5(3) 2_554 4_655 ? OA1Z MZI OBOZ 63.25(9) 4 4_655 ? MZO MZI OA1Z 56.5(5) 2_544 2_554 ? OA2Z MZI OA1Z 136.2(4) 2_544 2_554 ? ODOZ MZI OA1Z 61.12(15) 2_554 2_554 ? OA1Z MZI OA1Z 80.89(12) 4 2_554 ? OBOZ MZI OA1Z 92.1(2) 4_655 2_554 ? MZO MZI ODMZ 166.9(5) 2_544 2_544 ? OA2Z MZI ODMZ 104.9(3) 2_544 2_544 ? ODOZ MZI ODMZ 73.4(2) 2_554 2_544 ? OA1Z MZI ODMZ 59.6(2) 4 2_544 ? OBOZ MZI ODMZ 111.9(3) 4_655 2_544 ? OA1Z MZI ODMZ 111.62(13) 2_554 2_544 ? MZO MZI OCMO 42.4(3) 2_544 1_655 ? OA2Z MZI OCMO 56.44(15) 2_544 1_655 ? ODOZ MZI OCMO 76.98(18) 2_554 1_655 ? OA1Z MZI OCMO 159.7(4) 4 1_655 ? OBOZ MZI OCMO 109.8(3) 4_655 1_655 ? OA1Z MZI OCMO 80.3(3) 2_554 1_655 ? ODMZ MZI OCMO 135.86(16) 2_544 1_655 ? MZO MZI T1OZ 96.3(4) 2_544 4 ? OA2Z MZI T1OZ 122.46(12) 2_544 4 ? ODOZ MZI T1OZ 127.30(10) 2_554 4 ? OA1Z MZI T1OZ 31.84(6) 4 4 ? OBOZ MZI T1OZ 31.58(6) 4_655 4 ? OA1Z MZI T1OZ 83.54(13) 2_554 4 ? ODMZ MZI T1OZ 86.9(2) 2_544 4 ? OCMO MZI T1OZ 137.2(3) 1_655 4 ? MZO MZI T1OZ 78.1(5) 2_544 2_554 ? OA2Z MZI T1OZ 132.2(2) 2_544 2_554 ? ODOZ MZI T1OZ 30.64(9) 2_554 2_554 ? OA1Z MZI T1OZ 86.24(8) 4 2_554 ? OBOZ MZI T1OZ 121.2(2) 4_655 2_554 ? OA1Z MZI T1OZ 31.19(7) 2_554 2_554 ? ODMZ MZI T1OZ 88.83(12) 2_544 2_554 ? OCMO MZI T1OZ 81.68(19) 1_655 2_554 ? T1OZ MZI T1OZ 103.51(10) 4 2_554 ? MZO MZI T1MZ 146.7(5) 2_544 2_544 ? OA2Z MZI T1MZ 126.9(4) 2_544 2_544 ? ODOZ MZI T1MZ 86.2(2) 2_554 2_544 ? OA1Z MZI T1MZ 29.56(13) 4 2_544 ? OBOZ MZI T1MZ 87.57(17) 4_655 2_544 ? OA1Z MZI T1MZ 96.34(9) 2_554 2_544 ? ODMZ MZI T1MZ 30.04(10) 2_544 2_544 ? OCMO MZI T1MZ 162.30(14) 1_655 2_544 ? T1OZ MZI T1MZ 58.62(11) 4 2_544 ? T1OZ MZI T1MZ 86.57(9) 2_554 2_544 ? MZO MZI T2OZ 64.2(3) 2_544 2_554 ? OA2Z MZI T2OZ 26.99(10) 2_544 2_554 ? ODOZ MZI T2OZ 92.37(13) 2_554 2_554 ? OA1Z MZI T2OZ 166.25(18) 4 2_554 ? OBOZ MZI T2OZ 106.89(18) 4_655 2_554 ? OA1Z MZI T2OZ 110.0(3) 2_554 2_554 ? ODMZ MZI T2OZ 120.6(2) 2_544 2_554 ? OCMO MZI T2OZ 29.68(6) 1_655 2_554 ? T1OZ MZI T2OZ 138.25(14) 4 2_554 ? T1OZ MZI T2OZ 107.44(19) 2_554 2_554 ? T1MZ MZI T2OZ 149.0(3) 2_544 2_554 ? OCOO T1OO OBOO 111.33(12) . 1_455 ? OCOO T1OO OA1O 117.17(12) . . ? OBOO T1OO OA1O 102.19(12) 1_455 . ? OCOO T1OO ODOO 110.95(12) . . ? OBOO T1OO ODOO 113.25(12) 1_455 . ? OA1O T1OO ODOO 101.47(12) . . ? OCOZ T1OZ OBOZ 110.72(11) . 1_455 ? OCOZ T1OZ OA1Z 117.16(11) . . ? OBOZ T1OZ OA1Z 102.01(12) 1_455 . ? OCOZ T1OZ ODOZ 111.47(12) . . ? OBOZ T1OZ ODOZ 113.65(12) 1_455 . ? OA1Z T1OZ ODOZ 101.34(12) . . ? ODMO T1MO OBMO 113.68(13) . 1_455 ? ODMO T1MO OCMO 109.32(11) . . ? OBMO T1MO OCMO 112.14(12) 1_455 . ? ODMO T1MO OA1O 104.98(12) . 3_565 ? OBMO T1MO OA1O 103.39(12) 1_455 3_565 ? OCMO T1MO OA1O 113.07(12) . 3_565 ? ODMZ T1MZ OCMZ 108.49(12) . . ? ODMZ T1MZ OBMZ 112.33(14) . 1_455 ? OCMZ T1MZ OBMZ 113.08(13) . 1_455 ? ODMZ T1MZ OA1Z 106.04(12) . 3_566 ? OCMZ T1MZ OA1Z 112.37(12) . 3_566 ? OBMZ T1MZ OA1Z 104.33(12) 1_455 3_566 ? ODMZ T2OO OA2O 108.64(11) 3_666 1_545 ? ODMZ T2OO OBOO 111.12(13) 3_666 . ? OA2O T2OO OBOO 106.88(11) 1_545 . ? ODMZ T2OO OCMZ 114.22(13) 3_666 2_544 ? OA2O T2OO OCMZ 103.02(12) 1_545 2_544 ? OBOO T2OO OCMZ 112.32(12) . 2_544 ? ODMO T2OZ OBOZ 111.59(12) 3_666 . ? ODMO T2OZ OCMO 113.96(12) 3_666 2_545 ? OBOZ T2OZ OCMO 112.41(12) . 2_545 ? ODMO T2OZ OA2Z 107.61(11) 3_666 1_545 ? OBOZ T2OZ OA2Z 106.95(11) . 1_545 ? OCMO T2OZ OA2Z 103.65(11) 2_545 1_545 ? OCOZ T2MO OBMO 110.83(12) 2_554 . ? OCOZ T2MO ODOZ 112.16(12) 2_554 3_666 ? OBMO T2MO ODOZ 110.38(12) . 3_666 ? OCOZ T2MO OA2O 105.87(12) 2_554 . ? OBMO T2MO OA2O 109.92(11) . . ? ODOZ T2MO OA2O 107.52(11) 3_666 . ? OBMZ T2MZ OCOO 110.86(13) . 2 ? OBMZ T2MZ ODOO 110.16(13) . 3_666 ? OCOO T2MZ ODOO 112.42(12) 2 3_666 ? OBMZ T2MZ OA2Z 109.95(11) . . ? OCOO T2MZ OA2Z 105.16(12) 2 . ? ODOO T2MZ OA2Z 108.13(11) 3_666 . ? T1MO OA1O T1OO 139.75(15) 3_565 . ? T1MO OA1O MOO 101.3(2) 3_565 3_565 ? T1OO OA1O MOO 98.80(14) . 3_565 ? T1MO OA1O MOI 105.47(15) 3_565 2_444 ? T1OO OA1O MOI 98.67(13) . 2_444 ? MOO OA1O MOI 111.90(16) 3_565 2_444 ? T1MO OA1O MOI 115.58(14) 3_565 4 ? T1OO OA1O MOI 90.15(11) . 4 ? MOO OA1O MOI 15.40(17) 3_565 4 ? MOI OA1O MOI 100.98(10) 2_444 4 ? T1MO OA1O MOO 119.28(15) 3_565 1_545 ? T1OO OA1O MOO 90.24(12) . 1_545 ? MOO OA1O MOO 100.83(16) 3_565 1_545 ? MOI OA1O MOO 15.39(6) 2_444 1_545 ? MOI OA1O MOO 88.21(10) 4 1_545 ? T1OZ OA1Z T1MZ 140.66(15) . 3_566 ? T1OZ OA1Z MZO 100.34(13) . 1_545 ? T1MZ OA1Z MZO 102.71(16) 3_566 1_545 ? T1OZ OA1Z MZI 97.56(17) . 4 ? T1MZ OA1Z MZI 104.2(2) 3_566 4 ? MZO OA1Z MZI 109.32(14) 1_545 4 ? T1OZ OA1Z MZI 91.17(14) . 2_445 ? T1MZ OA1Z MZI 116.6(2) 3_566 2_445 ? MZO OA1Z MZI 15.01(8) 1_545 2_445 ? MZI OA1Z MZI 99.11(12) 4 2_445 ? T1OZ OA1Z MZO 88.96(11) . 3_566 ? T1MZ OA1Z MZO 116.72(14) 3_566 3_566 ? MZO OA1Z MZO 101.46(13) 1_545 3_566 ? MZI OA1Z MZO 13.05(19) 4 3_566 ? MZI OA1Z MZO 89.52(14) 2_445 3_566 ? T2OO OA2O T2MO 126.18(13) 1_565 . ? T2OO OA2O MOO 120.0(2) 1_565 . ? T2MO OA2O MOO 112.5(2) . . ? T2OO OA2O MOI 103.10(13) 1_565 2_454 ? T2MO OA2O MOI 130.70(15) . 2_454 ? MOO OA2O MOI 20.54(13) . 2_454 ? T2MZ OA2Z T2OZ 126.80(13) . 1_565 ? T2MZ OA2Z MZI 118.1(3) . 2_455 ? T2OZ OA2Z MZI 114.1(2) 1_565 2_455 ? T2MZ OA2Z MZO 133.42(15) . . ? T2OZ OA2Z MZO 99.78(13) 1_565 . ? MZI OA2Z MZO 18.32(17) 2_455 . ? T2OO OBOO T1OO 136.49(16) . 1_655 ? T2OO OBOO MOI 118.37(14) . 4_655 ? T1OO OBOO MOI 105.04(14) 1_655 4_655 ? T2OO OBOO MOO 128.73(14) . 3_665 ? T1OO OBOO MOO 93.69(15) 1_655 3_665 ? MOI OBOO MOO 19.31(12) 4_655 3_665 ? T1OZ OBOZ T2OZ 136.69(16) 1_655 . ? T1OZ OBOZ MZO 107.29(16) 1_655 3_666 ? T2OZ OBOZ MZO 115.65(16) . 3_666 ? T1OZ OBOZ MZI 96.68(17) 1_655 4_655 ? T2OZ OBOZ MZI 126.32(16) . 4_655 ? MZO OBOZ MZI 17.43(15) 3_666 4_655 ? T1MO OBMO T2MO 155.98(18) 1_655 . ? T1MO OBMO MOI 91.81(11) 1_655 4_665 ? T2MO OBMO MOI 109.76(11) . 4_665 ? T2MZ OBMZ T1MZ 156.66(19) . 1_655 ? T2MZ OBMZ MZO 110.03(13) . 3_676 ? T1MZ OBMZ MZO 91.12(13) 1_655 3_676 ? T2MZ OCOO T1OO 130.67(15) 2_444 . ? T2MO OCOZ T1OZ 130.72(14) 2_445 . ? T2MO OCOZ MOO 84.06(12) 2_445 2_445 ? T1OZ OCOZ MOO 140.25(13) . 2_445 ? T1MO OCMO T2OZ 131.67(15) . 2_454 ? T1MO OCMO MZO 135.12(13) . 2_444 ? T2OZ OCMO MZO 92.09(10) 2_454 2_444 ? T1MO OCMO MZI 139.23(14) . 1_455 ? T2OZ OCMO MZI 85.07(15) 2_454 1_455 ? MZO OCMO MZI 11.29(10) 2_444 1_455 ? T1MZ OCMZ T2OO 132.58(16) . 2_455 ? T1MZ OCMZ MOI 134.36(13) . 1_455 ? T2OO OCMZ MOI 91.31(11) 2_455 1_455 ? T2MZ ODOO T1OO 132.79(15) 3_666 . ? T2MZ ODOO MOO 121.1(2) 3_666 1_545 ? T1OO ODOO MOO 105.95(19) . 1_545 ? T2MZ ODOO MOI 130.98(13) 3_666 2_444 ? T1OO ODOO MOI 95.14(12) . 2_444 ? MOO ODOO MOI 19.32(13) 1_545 2_444 ? T2MO ODOZ T1OZ 131.84(15) 3_666 . ? T2MO ODOZ MZI 123.9(2) 3_666 2_445 ? T1OZ ODOZ MZI 104.2(2) . 2_445 ? T2MO ODOZ MZO 131.97(13) 3_666 1_545 ? T1OZ ODOZ MZO 94.58(11) . 1_545 ? MZI ODOZ MZO 17.05(19) 2_445 1_545 ? T1MO ODMO T2OZ 149.76(16) . 3_666 ? T1MO ODMO MOO 90.90(12) . . ? T2OZ ODMO MOO 117.95(13) 3_666 . ? T2OO ODMZ T1MZ 151.34(17) 3_666 . ? T2OO ODMZ MZI 116.88(12) 3_666 2_455 ? T1MZ ODMZ MZI 90.11(12) . 2_455 ? data_An78plagioclase _audit_creation_date 2010-06-25T16:45:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FI #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_mineral "plagioclase, low" _chemical_formula_moiety 'Al1.8 Ca0.8 Na0.2 O8 Si2.2' _chemical_formula_sum 'Al1.8 Ca0.8 Na0.2 O8 Si2.2' _chemical_formula_weight 275 _chemical_compound_source ; Harker Collection, University of Cambridge, no 103685 Sample from Beaver River Anorthosite. ; #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'I -1' _symmetry_space_group_name_Hall '-I 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z+1/2' '-x, -y, -z' '-x+1/2, -y+1/2, -z+1/2' _cell_length_a 8.1798(3) _cell_length_b 12.8761(3) _cell_length_c 14.1974(6) _cell_angle_alpha 93.423(2) _cell_angle_beta 116.054(2) _cell_angle_gamma 90.705(2) _cell_volume 1339.74(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_pressure 100 _cell_measurement_reflns_used 39 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 12.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour none _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.73 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.48 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_detector_area_resol_mean 16.0122 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_number 6468 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.5 _diffrn_reflns_theta_max 30.06 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 3915 _reflns_number_gt 2735 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Crysalis Pro (Oxford Diffraction)' _computing_cell_refinement 'Crysalis Pro (Oxford Diffraction)' _computing_data_reduction 'Crysalis Pro (Oxford Diffraction)' _computing_structure_solution 'known structure type' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure model is the "I-1 split-Ca model" of Angel et al (1990), with Al and Si disordered over the T sites, but full occupancies allocated for simplicity. The M sites are split in two, and assigned Ca scattering factors and their occupancies refined independently. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_number_reflns 3915 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.425 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group CaOO Ca 0.26759(15) 0.98396(16) 0.08625(12) 0.0316(6) Uani 0.455(3) 1 d P . . CaZO Ca 0.26836(18) 0.02977(13) 0.5465(2) 0.0139(5) Uani 0.612(14) 1 d P . . CaOI Ca 0.77497(15) 0.53406(12) 0.54589(11) 0.0173(4) Uani 0.410(3) 1 d P . . CaZI Ca 0.7647(4) 0.4999(11) 0.0762(8) 0.038(2) Uani 0.301(14) 1 d P . . T1OO Si 0.00757(7) 0.15954(4) 0.10453(4) 0.00948(12) Uani 1 1 d . . . T1OZ Al 0.00342(8) 0.16487(5) 0.61094(4) 0.00855(13) Uani 1 1 d . . . T1MO Al 0.00016(8) 0.81544(5) 0.11862(4) 0.00826(13) Uani 1 1 d . . . T1MZ Si 0.00528(7) 0.81730(4) 0.61283(4) 0.00948(12) Uani 1 1 d . . . T2OO Al 0.68794(8) 0.11160(5) 0.15799(4) 0.00839(12) Uani 1 1 d . . . T2OZ Si 0.67904(8) 0.10622(4) 0.65870(4) 0.01025(12) Uani 1 1 d . . . T2MO Si 0.67771(7) 0.88147(4) 0.18128(4) 0.00984(12) Uani 1 1 d . . . T2MZ Al 0.68340(8) 0.87570(4) 0.67666(4) 0.00808(12) Uani 1 1 d . . . OA1O O 0.0083(2) 0.12733(12) -0.00857(10) 0.0173(3) Uani 1 1 d . . . OA1Z O -0.0045(2) 0.12686(12) 0.48860(10) 0.0189(3) Uani 1 1 d . . . OA2O O 0.57858(19) 0.99082(11) 0.14001(10) 0.0130(3) Uani 1 1 d . . . OA2Z O 0.57536(19) 0.99139(11) 0.63802(10) 0.0124(3) Uani 1 1 d . . . OBOO O 0.8198(2) 0.10183(12) 0.09157(11) 0.0178(3) Uani 1 1 d . . . OBOZ O 0.8028(2) 0.10228(12) 0.59525(11) 0.0188(3) Uani 1 1 d . . . OBMO O 0.8105(2) 0.85457(13) 0.12785(13) 0.0260(4) Uani 1 1 d . . . OBMZ O 0.8202(2) 0.85452(13) 0.61502(13) 0.0234(4) Uani 1 1 d . . . OCOO O 0.0129(2) 0.28183(11) 0.13636(10) 0.0165(3) Uani 1 1 d . . . OCOZ O 0.0147(2) 0.29490(11) 0.64730(11) 0.0156(3) Uani 1 1 d . . . OCMO O 0.0098(2) 0.68164(11) 0.10869(10) 0.0155(3) Uani 1 1 d . . . OCMZ O 0.0097(2) 0.69127(12) 0.60134(10) 0.0173(3) Uani 1 1 d . . . ODOO O 0.1911(2) 0.10734(12) 0.18855(10) 0.0177(3) Uani 1 1 d . . . ODOZ O 0.2030(2) 0.10438(12) 0.69146(10) 0.0186(3) Uani 1 1 d . . . ODMO O 0.1968(2) 0.86841(12) 0.21809(11) 0.0228(4) Uani 1 1 d . . . ODMZ O 0.1843(2) 0.86246(13) 0.71261(11) 0.0260(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 CaOO 0.0131(6) 0.0547(12) 0.0244(7) -0.0209(7) 0.0090(5) -0.0084(5) CaZO 0.0089(4) 0.0187(7) 0.0108(7) -0.0029(4) 0.0016(4) 0.0041(3) CaOI 0.0107(6) 0.0213(8) 0.0158(6) -0.0053(5) 0.0028(4) 0.0040(5) CaZI 0.0122(10) 0.073(4) 0.024(2) -0.024(3) 0.0059(10) 0.0012(13) T1OO 0.0096(3) 0.0110(3) 0.0077(2) 0.00027(18) 0.0037(2) -0.0014(2) T1OZ 0.0087(3) 0.0093(3) 0.0074(3) 0.0006(2) 0.0033(2) -0.0009(2) T1MO 0.0092(3) 0.0094(3) 0.0060(2) 0.0004(2) 0.0032(2) 0.0024(2) T1MZ 0.0102(3) 0.0114(3) 0.0065(2) 0.00071(19) 0.0032(2) 0.0034(2) T2OO 0.0074(3) 0.0071(3) 0.0095(3) 0.0007(2) 0.0026(2) 0.0001(2) T2OZ 0.0090(3) 0.0083(3) 0.0122(2) -0.00078(19) 0.0037(2) 0.0001(2) T2MO 0.0090(3) 0.0084(3) 0.0106(2) 0.00152(19) 0.0028(2) 0.0014(2) T2MZ 0.0074(3) 0.0075(3) 0.0090(3) 0.0015(2) 0.0032(2) 0.0004(2) OA1O 0.0262(9) 0.0192(8) 0.0090(6) 0.0010(5) 0.0100(6) 0.0006(6) OA1Z 0.0280(9) 0.0213(8) 0.0110(7) 0.0040(6) 0.0117(7) 0.0048(7) OA2O 0.0111(7) 0.0117(7) 0.0143(6) 0.0035(5) 0.0035(6) 0.0021(6) OA2Z 0.0109(7) 0.0088(7) 0.0147(6) 0.0009(5) 0.0030(6) -0.0015(5) OBOO 0.0154(8) 0.0143(8) 0.0270(8) -0.0029(6) 0.0130(7) -0.0052(6) OBOZ 0.0175(8) 0.0155(8) 0.0289(8) -0.0011(6) 0.0157(7) -0.0013(6) OBMO 0.0207(9) 0.0211(9) 0.0429(10) -0.0045(7) 0.0211(8) 0.0012(7) OBMZ 0.0190(9) 0.0219(9) 0.0366(9) -0.0008(7) 0.0191(7) 0.0031(7) OCOO 0.0172(8) 0.0130(8) 0.0200(7) -0.0015(6) 0.0091(6) -0.0021(6) OCOZ 0.0146(8) 0.0127(8) 0.0180(7) -0.0017(5) 0.0063(6) -0.0040(6) OCMO 0.0137(8) 0.0152(8) 0.0141(7) -0.0008(5) 0.0029(6) 0.0045(6) OCMZ 0.0191(8) 0.0134(8) 0.0147(7) -0.0013(5) 0.0033(6) 0.0046(6) ODOO 0.0153(8) 0.0178(8) 0.0129(7) 0.0017(5) -0.0004(6) 0.0023(6) ODOZ 0.0173(8) 0.0151(8) 0.0140(7) 0.0006(5) -0.0017(6) 0.0017(6) ODMO 0.0167(8) 0.0204(9) 0.0179(7) -0.0055(6) -0.0039(6) 0.0012(7) ODMZ 0.0197(9) 0.0240(9) 0.0186(7) -0.0053(6) -0.0051(7) 0.0021(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag CaOO CaOI 0.9065(17) 2_454 ? CaOO OA2O 2.3113(17) . ? CaOO ODOO 2.3606(18) 1_565 ? CaOO OA1O 2.430(2) 3_565 ? CaOO OBOO 2.4833(18) 3_665 ? CaOO ODMO 2.705(3) . ? CaOO OA1O 2.758(2) 1_565 ? CaZO CaZI 0.597(14) 2_445 ? CaZO OA2Z 2.3409(18) 1_545 ? CaZO OA1Z 2.4080(18) . ? CaZO OBOZ 2.412(3) 3_656 ? CaZO ODOZ 2.487(3) . ? CaZO OCMO 2.583(2) 2_545 ? CaZO OBMZ 2.642(4) 3_666 ? CaOI CaOO 0.9065(17) 2_545 ? CaOI OA2O 2.3390(17) 2_545 ? CaOI OA1O 2.3438(18) 2 ? CaOI OBOO 2.3876(18) 4_655 ? CaOI ODOO 2.5441(19) 2 ? CaOI OCMZ 2.606(2) 1_655 ? CaOI OBMO 2.750(2) 4_665 ? CaZI CaZO 0.597(14) 2_554 ? CaZI ODOZ 2.285(3) 2_554 ? CaZI OA2Z 2.302(3) 2_544 ? CaZI OA1Z 2.461(10) 4 ? CaZI OBOZ 2.526(4) 4_655 ? CaZI OA1Z 2.644(11) 2_554 ? CaZI OCMO 2.941(13) 1_655 ? T1OO OCOO 1.6067(16) . ? T1OO OBOO 1.6283(16) 1_455 ? T1OO ODOO 1.6356(14) . ? T1OO OA1O 1.6368(13) . ? T1OZ OCOZ 1.7114(16) . ? T1OZ OBOZ 1.7367(16) 1_455 ? T1OZ OA1Z 1.7493(14) . ? T1OZ ODOZ 1.7543(15) . ? T1MO OBMO 1.6935(16) 1_455 ? T1MO ODMO 1.7058(17) . ? T1MO OCMO 1.7259(16) . ? T1MO OA1O 1.7416(13) 3_565 ? T1MZ ODMZ 1.5963(17) . ? T1MZ OBMZ 1.6062(16) 1_455 ? T1MZ OCMZ 1.6237(16) . ? T1MZ OA1Z 1.6450(13) 3_566 ? T2OO ODMZ 1.6764(15) 3_666 ? T2OO OCMZ 1.7117(15) 2_544 ? T2OO OBOO 1.7182(15) . ? T2OO OA2O 1.7326(16) 1_545 ? T2OZ ODMO 1.6003(15) 3_666 ? T2OZ OCMO 1.6172(14) 2_545 ? T2OZ OBOZ 1.6237(15) . ? T2OZ OA2Z 1.6402(15) 1_545 ? T2MO OBMO 1.6052(16) . ? T2MO OCOZ 1.6083(16) 2_554 ? T2MO ODOZ 1.6301(14) 3_666 ? T2MO OA2O 1.6409(14) . ? T2MZ OCOO 1.7053(17) 2 ? T2MZ OBMZ 1.7122(16) . ? T2MZ ODOO 1.7271(14) 3_666 ? T2MZ OA2Z 1.7335(14) . ? OA1O T1MO 1.7416(13) 3_565 ? OA1O CaOI 2.3438(18) 2_444 ? OA1O CaOO 2.430(2) 3_565 ? OA1O CaOO 2.758(2) 1_545 ? OA1O CaOI 2.939(2) 4 ? OA1Z T1MZ 1.6450(13) 3_566 ? OA1Z CaZI 2.461(10) 4 ? OA1Z CaZI 2.644(11) 2_445 ? OA1Z CaZO 2.793(3) 3_556 ? OA2O T2OO 1.7326(16) 1_565 ? OA2O CaOI 2.3390(17) 2_454 ? OA2Z T2OZ 1.6402(15) 1_565 ? OA2Z CaZI 2.302(3) 2_455 ? OA2Z CaZO 2.3409(18) 1_565 ? OBOO T1OO 1.6283(16) 1_655 ? OBOO CaOI 2.3876(18) 4_655 ? OBOO CaOO 2.4833(18) 3_665 ? OBOZ T1OZ 1.7367(16) 1_655 ? OBOZ CaZO 2.412(3) 3_656 ? OBOZ CaZI 2.526(4) 4_655 ? OBMO T1MO 1.6935(16) 1_655 ? OBMO CaOI 2.750(2) 4_665 ? OBMZ T1MZ 1.6062(15) 1_655 ? OBMZ CaZO 2.642(4) 3_666 ? OCOO T2MZ 1.7053(16) 2_444 ? OCOZ T2MO 1.6083(16) 2_445 ? OCOZ CaOO 3.098(2) 2_445 ? OCMO T2OZ 1.6172(14) 2_454 ? OCMO CaZO 2.583(2) 2_454 ? OCMO CaZI 2.941(13) 1_455 ? OCMZ T2OO 1.7117(15) 2_455 ? OCMZ CaOI 2.606(2) 1_455 ? ODOO T2MZ 1.7271(14) 3_666 ? ODOO CaOO 2.3606(18) 1_545 ? ODOO CaOI 2.5441(19) 2_444 ? ODOZ T2MO 1.6301(14) 3_666 ? ODOZ CaZI 2.285(3) 2_445 ? ODMO T2OZ 1.6003(15) 3_666 ? ODMZ T2OO 1.6764(15) 3_666 ? ODMZ CaZI 2.969(17) 2_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CaOI CaOO OA2O 80.48(11) 2_454 . ? CaOI CaOO ODOO 91.05(14) 2_454 1_565 ? OA2O CaOO ODOO 110.22(7) . 1_565 ? CaOI CaOO OA1O 115.68(13) 2_454 3_565 ? OA2O CaOO OA1O 144.99(9) . 3_565 ? ODOO CaOO OA1O 100.72(7) 1_565 3_565 ? CaOI CaOO OBOO 73.38(11) 2_454 3_665 ? OA2O CaOO OBOO 96.85(6) . 3_665 ? ODOO CaOO OBOO 146.19(9) 1_565 3_665 ? OA1O CaOO OBOO 62.35(5) 3_565 3_665 ? CaOI CaOO ODMO 166.10(14) 2_454 . ? OA2O CaOO ODMO 108.34(9) . . ? ODOO CaOO ODMO 75.93(7) 1_565 . ? OA1O CaOO ODMO 63.25(6) 3_565 . ? OBOO CaOO ODMO 115.05(8) 3_665 . ? CaOI CaOO OA1O 54.08(12) 2_454 1_565 ? OA2O CaOO OA1O 130.96(10) . 1_565 ? ODOO CaOO OA1O 59.42(5) 1_565 1_565 ? OA1O CaOO OA1O 78.95(6) 3_565 1_565 ? OBOO CaOO OA1O 87.67(7) 3_665 1_565 ? ODMO CaOO OA1O 113.62(6) . 1_565 ? CaZI CaZO OA2Z 79.0(4) 2_445 1_545 ? CaZI CaZO OA1Z 106.9(6) 2_445 . ? OA2Z CaZO OA1Z 159.59(8) 1_545 . ? CaZI CaZO OBOZ 94.1(5) 2_445 3_656 ? OA2Z CaZO OBOZ 95.73(8) 1_545 3_656 ? OA1Z CaZO OBOZ 103.19(8) . 3_656 ? CaZI CaZO ODOZ 63.5(7) 2_445 . ? OA2Z CaZO ODOZ 101.43(11) 1_545 . ? OA1Z CaZO ODOZ 65.81(7) . . ? OBOZ CaZO ODOZ 148.04(13) 3_656 . ? CaZI CaZO OCMO 121.8(5) 2_445 2_545 ? OA2Z CaZO OCMO 61.71(6) 1_545 2_545 ? OA1Z CaZO OCMO 99.78(8) . 2_545 ? OBOZ CaZO OCMO 128.77(16) 3_656 2_545 ? ODOZ CaZO OCMO 83.20(7) . 2_545 ? CaZI CaZO OBMZ 162.8(4) 2_445 3_666 ? OA2Z CaZO OBMZ 117.20(14) 1_545 3_666 ? OA1Z CaZO OBMZ 60.30(7) . 3_666 ? OBOZ CaZO OBMZ 78.98(11) 3_656 3_666 ? ODOZ CaZO OBMZ 115.39(6) . 3_666 ? OCMO CaZO OBMZ 73.84(10) 2_545 3_666 ? CaOO CaOI OA2O 77.05(11) 2_545 2_545 ? CaOO CaOI OA1O 107.66(14) 2_545 2 ? OA2O CaOI OA1O 160.55(8) 2_545 2 ? CaOO CaOI OBOO 85.28(12) 2_545 4_655 ? OA2O CaOI OBOO 98.78(6) 2_545 4_655 ? OA1O CaOI OBOO 100.40(7) 2 4_655 ? CaOO CaOI ODOO 68.08(12) 2_545 2 ? OA2O CaOI ODOO 103.32(7) 2_545 2 ? OA1O CaOI ODOO 63.01(5) 2 2 ? OBOO CaOI ODOO 140.01(9) 4_655 2 ? CaOO CaOI OCMZ 128.03(13) 2_545 1_655 ? OA2O CaOI OCMZ 65.54(6) 2_545 1_655 ? OA1O CaOI OCMZ 98.45(7) 2 1_655 ? OBOO CaOI OCMZ 133.40(8) 4_655 1_655 ? ODOO CaOI OCMZ 86.36(6) 2 1_655 ? CaOO CaOI OBMO 159.47(13) 2_545 4_665 ? OA2O CaOI OBMO 117.55(8) 2_545 4_665 ? OA1O CaOI OBMO 63.80(6) 2 4_665 ? OBOO CaOI OBMO 78.44(6) 4_655 4_665 ? ODOO CaOI OBMO 118.14(6) 2 4_665 ? OCMZ CaOI OBMO 72.50(7) 1_655 4_665 ? CaZO CaZI ODOZ 102.9(10) 2_554 2_554 ? CaZO CaZI OA2Z 86.3(4) 2_554 2_544 ? ODOZ CaZI OA2Z 109.17(13) 2_554 2_544 ? CaZO CaZI OA1Z 118.2(5) 2_554 4 ? ODOZ CaZI OA1Z 100.7(3) 2_554 4 ? OA2Z CaZI OA1Z 135.8(6) 2_544 4 ? CaZO CaZI OBOZ 72.3(4) 2_554 4_655 ? ODOZ CaZI OBOZ 156.5(3) 2_554 4_655 ? OA2Z CaZI OBOZ 93.67(12) 2_544 4_655 ? OA1Z CaZI OBOZ 64.17(13) 4 4_655 ? CaZO CaZI OA1Z 60.7(7) 2_554 2_554 ? ODOZ CaZI OA1Z 64.9(2) 2_554 2_554 ? OA2Z CaZI OA1Z 141.7(7) 2_544 2_554 ? OA1Z CaZI OA1Z 80.48(11) 4 2_554 ? OBOZ CaZI OA1Z 93.9(3) 4_655 2_554 ? CaZO CaZI OCMO 48.3(6) 2_554 1_655 ? ODOZ CaZI OCMO 79.1(3) 2_554 1_655 ? OA2Z CaZI OCMO 56.2(2) 2_544 1_655 ? OA1Z CaZI OCMO 165.1(6) 4 1_655 ? OBOZ CaZI OCMO 110.7(5) 4_655 1_655 ? OA1Z CaZI OCMO 86.1(5) 2_554 1_655 ? OCOO T1OO OBOO 111.17(8) . 1_455 ? OCOO T1OO ODOO 109.97(8) . . ? OBOO T1OO ODOO 113.28(8) 1_455 . ? OCOO T1OO OA1O 116.81(7) . . ? OBOO T1OO OA1O 102.37(8) 1_455 . ? ODOO T1OO OA1O 102.95(8) . . ? OCOZ T1OZ OBOZ 112.83(7) . 1_455 ? OCOZ T1OZ OA1Z 118.89(7) . . ? OBOZ T1OZ OA1Z 98.93(8) 1_455 . ? OCOZ T1OZ ODOZ 111.54(8) . . ? OBOZ T1OZ ODOZ 114.79(8) 1_455 . ? OA1Z T1OZ ODOZ 98.80(7) . . ? OBMO T1MO ODMO 113.29(9) 1_455 . ? OBMO T1MO OCMO 112.64(9) 1_455 . ? ODMO T1MO OCMO 110.11(7) . . ? OBMO T1MO OA1O 104.37(8) 1_455 3_565 ? ODMO T1MO OA1O 103.24(8) . 3_565 ? OCMO T1MO OA1O 112.73(7) . 3_565 ? ODMZ T1MZ OBMZ 113.25(9) . 1_455 ? ODMZ T1MZ OCMZ 109.55(8) . . ? OBMZ T1MZ OCMZ 111.82(9) 1_455 . ? ODMZ T1MZ OA1Z 106.03(9) . 3_566 ? OBMZ T1MZ OA1Z 102.99(8) 1_455 3_566 ? OCMZ T1MZ OA1Z 112.98(8) . 3_566 ? ODMZ T2OO OCMZ 115.08(8) 3_666 2_544 ? ODMZ T2OO OBOO 111.49(9) 3_666 . ? OCMZ T2OO OBOO 112.61(7) 2_544 . ? ODMZ T2OO OA2O 107.73(8) 3_666 1_545 ? OCMZ T2OO OA2O 102.48(8) 2_544 1_545 ? OBOO T2OO OA2O 106.56(7) . 1_545 ? ODMO T2OZ OCMO 113.80(8) 3_666 2_545 ? ODMO T2OZ OBOZ 110.76(9) 3_666 . ? OCMO T2OZ OBOZ 112.53(7) 2_545 . ? ODMO T2OZ OA2Z 109.89(8) 3_666 1_545 ? OCMO T2OZ OA2Z 102.12(8) 2_545 1_545 ? OBOZ T2OZ OA2Z 107.19(8) . 1_545 ? OBMO T2MO OCOZ 111.85(9) . 2_554 ? OBMO T2MO ODOZ 109.28(9) . 3_666 ? OCOZ T2MO ODOZ 111.68(8) 2_554 3_666 ? OBMO T2MO OA2O 109.64(8) . . ? OCOZ T2MO OA2O 105.55(8) 2_554 . ? ODOZ T2MO OA2O 108.74(7) 3_666 . ? OCOO T2MZ OBMZ 110.98(8) 2 . ? OCOO T2MZ ODOO 113.96(7) 2 3_666 ? OBMZ T2MZ ODOO 111.59(8) . 3_666 ? OCOO T2MZ OA2Z 105.47(7) 2 . ? OBMZ T2MZ OA2Z 108.46(7) . . ? ODOO T2MZ OA2Z 105.92(7) 3_666 . ? T1OO OA1O T1MO 140.19(10) . 3_565 ? T1OO OA1O CaOI 100.83(7) . 2_444 ? T1MO OA1O CaOI 102.58(8) 3_565 2_444 ? T1OO OA1O CaOO 98.50(8) . 3_565 ? T1MO OA1O CaOO 101.24(8) 3_565 3_565 ? CaOI OA1O CaOO 113.15(7) 2_444 3_565 ? T1OO OA1O CaOO 89.69(6) . 1_545 ? T1MO OA1O CaOO 119.51(8) 3_565 1_545 ? CaOI OA1O CaOO 18.25(4) 2_444 1_545 ? CaOO OA1O CaOO 101.05(6) 3_565 1_545 ? T1OO OA1O CaOI 88.13(7) . 4 ? T1MO OA1O CaOI 116.72(7) 3_565 4 ? CaOI OA1O CaOI 103.38(6) 2_444 4 ? CaOO OA1O CaOI 16.14(4) 3_565 4 ? CaOO OA1O CaOI 88.71(5) 1_545 4 ? T1MZ OA1Z T1OZ 137.95(10) 3_566 . ? T1MZ OA1Z CaZO 102.34(12) 3_566 . ? T1OZ OA1Z CaZO 99.20(10) . . ? T1MZ OA1Z CaZI 108.2(3) 3_566 4 ? T1OZ OA1Z CaZI 99.0(2) . 4 ? CaZO OA1Z CaZI 107.4(2) . 4 ? T1MZ OA1Z CaZI 114.4(3) 3_566 2_445 ? T1OZ OA1Z CaZI 91.14(17) . 2_445 ? CaZO OA1Z CaZI 12.5(2) . 2_445 ? CaZI OA1Z CaZI 99.52(11) 4 2_445 ? T1MZ OA1Z CaZO 118.86(10) 3_566 3_556 ? T1OZ OA1Z CaZO 91.08(9) . 3_556 ? CaZO OA1Z CaZO 101.61(7) . 3_556 ? CaZI OA1Z CaZO 10.8(3) 4 3_556 ? CaZI OA1Z CaZO 92.3(3) 2_445 3_556 ? T2MO OA2O T2OO 125.95(9) . 1_565 ? T2MO OA2O CaOO 114.34(9) . . ? T2OO OA2O CaOO 118.34(8) 1_565 . ? T2MO OA2O CaOI 133.59(9) . 2_454 ? T2OO OA2O CaOI 100.47(7) 1_565 2_454 ? CaOO OA2O CaOI 22.47(4) . 2_454 ? T2OZ OA2Z T2MZ 125.05(9) 1_565 . ? T2OZ OA2Z CaZI 113.0(4) 1_565 2_455 ? T2MZ OA2Z CaZI 121.2(4) . 2_455 ? T2OZ OA2Z CaZO 102.43(8) 1_565 1_565 ? T2MZ OA2Z CaZO 132.51(9) . 1_565 ? CaZI OA2Z CaZO 14.7(4) 2_455 1_565 ? T1OO OBOO T2OO 134.88(10) 1_655 . ? T1OO OBOO CaOI 109.93(8) 1_655 4_655 ? T2OO OBOO CaOI 115.04(9) . 4_655 ? T1OO OBOO CaOO 96.70(7) 1_655 3_665 ? T2OO OBOO CaOO 127.21(8) . 3_665 ? CaOI OBOO CaOO 21.33(4) 4_655 3_665 ? T2OZ OBOZ T1OZ 135.31(10) . 1_655 ? T2OZ OBOZ CaZO 118.98(11) . 3_656 ? T1OZ OBOZ CaZO 105.33(10) 1_655 3_656 ? T2OZ OBOZ CaZI 127.6(2) . 4_655 ? T1OZ OBOZ CaZI 97.0(2) 1_655 4_655 ? CaZO OBOZ CaZI 13.6(3) 3_656 4_655 ? T2MO OBMO T1MO 158.33(12) . 1_655 ? T2MO OBMO CaOI 110.57(8) . 4_665 ? T1MO OBMO CaOI 89.24(7) 1_655 4_665 ? T1MZ OBMZ T2MZ 152.31(11) 1_655 . ? T1MZ OBMZ CaZO 94.32(8) 1_655 3_666 ? T2MZ OBMZ CaZO 111.47(9) . 3_666 ? T1OO OCOO T2MZ 131.65(10) . 2_444 ? T2MO OCOZ T1OZ 131.00(9) 2_445 . ? T2MO OCOZ CaOO 84.10(7) 2_445 2_445 ? T1OZ OCOZ CaOO 138.73(8) . 2_445 ? T2OZ OCMO T1MO 131.20(10) 2_454 . ? T2OZ OCMO CaZO 93.68(7) 2_454 2_454 ? T1MO OCMO CaZO 134.04(8) . 2_454 ? T2OZ OCMO CaZI 88.0(2) 2_454 1_455 ? T1MO OCMO CaZI 137.16(15) . 1_455 ? CaZO OCMO CaZI 9.94(17) 2_454 1_455 ? T1MZ OCMZ T2OO 129.70(10) . 2_455 ? T1MZ OCMZ CaOI 136.82(9) . 1_455 ? T2OO OCMZ CaOI 91.45(7) 2_455 1_455 ? T1OO ODOO T2MZ 133.46(10) . 3_666 ? T1OO ODOO CaOO 104.92(8) . 1_545 ? T2MZ ODOO CaOO 121.59(8) 3_666 1_545 ? T1OO ODOO CaOI 93.21(6) . 2_444 ? T2MZ ODOO CaOI 131.24(8) 3_666 2_444 ? CaOO ODOO CaOI 20.87(4) 1_545 2_444 ? T2MO ODOZ T1OZ 129.21(9) 3_666 . ? T2MO ODOZ CaZI 126.8(3) 3_666 2_445 ? T1OZ ODOZ CaZI 104.0(3) . 2_445 ? T2MO ODOZ CaZO 133.25(9) 3_666 . ? T1OZ ODOZ CaZO 96.19(7) . . ? CaZI ODOZ CaZO 13.5(4) 2_445 . ? T2OZ ODMO T1MO 149.30(12) 3_666 . ? T2OZ ODMO CaOO 116.78(9) 3_666 . ? T1MO ODMO CaOO 92.26(7) . . ? T1MZ ODMZ T2OO 153.25(13) . 3_666 ? T1MZ ODMZ CaZI 89.59(9) . 2_455 ? T2OO ODMZ CaZI 115.00(10) 3_666 2_455 ? data_An98plagioclase _audit_creation_date 2006-03-27T20:47:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'Al2 Ca1 O8 Si2' _chemical_formula_sum 'Al2 Ca O8 Si2' _chemical_formula_weight 278.22 _chemical_compound_source 'natural sample from Miyake, Japan' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'I -1' _symmetry_space_group_name_Hall '-I 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z+1/2' '-x, -y, -z' '-x+1/2, -y+1/2, -z+1/2' _cell_length_a 8.1789(3) _cell_length_b 12.8717(6) _cell_length_c 14.1765(7) _cell_angle_alpha 93.194(4) _cell_angle_beta 115.893(3) _cell_angle_gamma 91.195(3) _cell_volume 1338.84(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.85 _cell_measurement_theta_max 9.75 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 2.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.57 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'fine-focus sealed tube' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector CCD _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_number 14034 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 30.12 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 3929 _reflns_number_gt 2542 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Crysalis (Oxford Diffraction 2005)' _computing_cell_refinement 'Single (Angel et al. 2000)' _computing_data_reduction 'Crysalis (Oxford Diffraction 2005)' _computing_structure_solution none _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure refinement with end-member composition. True composition is An98Ab2 Structure model is the "I-1 split-Ca model" of Angel et al (1990), with Al and Si disordered over the T sites, but full occupancies allocated for simplicity. The M sites are split in two, and assigned Ca scattering factors and their occupancies refined independently. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_number_reflns 3929 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.565 _refine_diff_density_min -0.75 _refine_diff_density_rms 0.106 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.26578(14) 0.98608(10) 0.08636(9) 0.0265(3) Uani 0.5 1 d P . . Ca2 Ca 0.2687(2) 1.03172(13) 0.54332(11) 0.0101(3) Uani 0.5 1 d P . . Ca3 Ca 0.27420(12) 1.03603(8) 0.04196(7) 0.01081(18) Uani 0.5 1 d P . . Ca4 Ca 0.7354(2) 0.99359(15) 0.42672(13) 0.0265(4) Uani 0.5 1 d P . . Si11 Si 0.00768(8) 1.15772(5) 0.10418(5) 0.00804(13) Uani 1 1 d . . . Al13 Al 0.50272(9) 0.66352(5) 0.11201(5) 0.00781(14) Uani 1 1 d . . . Al15 Al -0.00038(9) 0.81483(5) 0.11941(5) 0.00833(14) Uani 1 1 d . . . Si17 Si -0.00504(8) 1.18224(5) 0.38812(5) 0.00828(13) Uani 1 1 d . . . Al21 Al 0.68774(9) 1.11225(5) 0.15931(5) 0.01040(15) Uani 1 1 d . . . Si23 Si 0.32336(8) 0.89467(5) 0.34263(5) 0.01084(14) Uani 1 1 d . . . Si25 Si 0.67552(8) 0.88136(5) 0.18075(5) 0.01057(13) Uani 1 1 d . . . Al27 Al 0.31664(9) 1.12505(5) 0.32273(5) 0.00864(14) Uani 1 1 d . . . OA11 O 0.0070(2) 1.12487(12) -0.00909(12) 0.0173(4) Uani 1 1 d . . . OA13 O -0.0017(2) 1.12522(12) 0.48977(12) 0.0172(4) Uani 1 1 d . . . OA21 O 0.5744(2) 0.98970(11) 0.13912(12) 0.0109(3) Uani 1 1 d . . . OA23 O 0.4279(2) 1.00902(11) 0.36193(12) 0.0103(3) Uani 1 1 d . . . OBO1 O 0.1776(2) 0.90096(12) -0.09196(15) 0.0200(4) Uani 1 1 d . . . OBO3 O 0.2989(2) 0.60040(12) 0.09278(16) 0.0226(4) Uani 1 1 d . . . OBM1 O 0.1932(3) 1.14444(14) -0.12589(18) 0.0298(5) Uani 1 1 d . . . OBM3 O 0.1769(3) 1.14471(14) 0.38379(17) 0.0267(4) Uani 1 1 d . . . OCO1 O 0.0126(2) 1.27875(12) 0.13601(13) 0.0130(3) Uani 1 1 d . . . OCO3 O 0.5148(2) 0.79367(12) 0.14919(13) 0.0144(3) Uani 1 1 d . . . OCM1 O 0.0077(2) 0.67987(12) 0.10747(12) 0.0126(3) Uani 1 1 d . . . OCM3 O 0.5066(2) 1.19195(12) 0.09915(12) 0.0133(3) Uani 1 1 d . . . ODO1 O 0.1917(2) 1.10647(12) 0.18562(13) 0.0183(4) Uani 1 1 d . . . ODO3 O 0.7974(2) 0.89685(12) 0.30781(14) 0.0223(4) Uani 1 1 d . . . ODM1 O 0.1971(2) 0.86819(13) 0.22062(15) 0.0283(5) Uani 1 1 d . . . ODM3 O 0.8135(3) 1.13731(15) 0.29112(16) 0.0350(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0127(5) 0.0417(7) 0.0218(6) -0.0141(6) 0.0067(5) -0.0027(5) Ca2 0.0096(5) 0.0126(6) 0.0082(6) 0.0011(4) 0.0038(5) 0.0027(4) Ca3 0.0078(4) 0.0134(5) 0.0093(4) -0.0003(4) 0.0020(4) 0.0032(3) Ca4 0.0084(6) 0.0385(12) 0.0249(10) -0.0186(7) 0.0025(7) 0.0023(7) Si11 0.0081(3) 0.0092(3) 0.0068(3) 0.0001(2) 0.0034(2) -0.0009(2) Al13 0.0083(3) 0.0080(3) 0.0070(3) 0.0004(3) 0.0033(3) -0.0010(2) Al15 0.0103(3) 0.0082(3) 0.0066(3) 0.0001(3) 0.0038(3) 0.0013(3) Si17 0.0084(3) 0.0095(3) 0.0067(3) 0.0002(2) 0.0031(2) 0.0022(2) Al21 0.0075(3) 0.0076(3) 0.0153(3) -0.0004(3) 0.0043(3) 0.0002(3) Si23 0.0086(3) 0.0079(3) 0.0163(3) -0.0015(2) 0.0060(3) -0.0004(2) Si25 0.0074(3) 0.0078(3) 0.0143(3) 0.0024(2) 0.0025(3) 0.0007(2) Al27 0.0072(3) 0.0082(3) 0.0103(3) 0.0022(3) 0.0035(3) 0.0012(3) OA11 0.0306(10) 0.0147(8) 0.0090(8) 0.0010(7) 0.0108(8) 0.0020(7) OA13 0.0322(11) 0.0127(8) 0.0133(8) 0.0012(7) 0.0162(8) 0.0017(7) OA21 0.0088(8) 0.0086(7) 0.0132(8) 0.0026(6) 0.0025(7) 0.0008(6) OA23 0.0092(8) 0.0075(7) 0.0136(8) 0.0015(6) 0.0045(7) 0.0000(6) OBO1 0.0163(9) 0.0123(8) 0.0360(11) -0.0069(8) 0.0169(8) -0.0047(7) OBO3 0.0201(9) 0.0133(9) 0.0437(12) -0.0085(8) 0.0243(9) -0.0060(7) OBM1 0.0179(9) 0.0164(9) 0.0623(15) -0.0038(9) 0.0248(10) 0.0013(7) OBM3 0.0243(10) 0.0186(9) 0.0520(13) 0.0055(9) 0.0298(10) 0.0060(8) OCO1 0.0143(8) 0.0085(8) 0.0162(8) -0.0022(6) 0.0072(7) -0.0022(6) OCO3 0.0140(8) 0.0117(8) 0.0162(8) -0.0008(7) 0.0059(7) -0.0033(6) OCM1 0.0120(8) 0.0109(8) 0.0131(8) -0.0002(6) 0.0039(7) 0.0020(6) OCM3 0.0134(8) 0.0105(8) 0.0126(8) -0.0013(6) 0.0027(7) 0.0022(6) ODO1 0.0151(9) 0.0155(9) 0.0140(8) 0.0002(7) -0.0032(7) 0.0033(7) ODO3 0.0190(9) 0.0118(8) 0.0194(9) 0.0004(7) -0.0070(8) 0.0015(7) ODM1 0.0155(9) 0.0194(10) 0.0300(10) -0.0112(8) -0.0072(8) 0.0036(7) ODM3 0.0209(11) 0.0251(11) 0.0284(11) -0.0133(9) -0.0158(9) 0.0064(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 Ca3 0.9463(14) . ? Ca1 OA21 2.2966(18) . ? Ca1 ODO1 2.2998(19) . ? Ca1 OA11 2.403(2) 3_575 ? Ca1 OBO1 2.485(2) . ? Ca1 ODM1 2.731(3) . ? Ca1 OA11 2.725(2) . ? Ca1 Si11 3.1174(12) 3_575 ? Ca1 Si11 3.1621(13) . ? Ca1 Al15 3.2593(15) . ? Ca1 Si25 3.3631(13) . ? Ca1 Al21 3.4755(13) . ? Ca2 Ca4 0.5614(18) 3_676 ? Ca2 OA23 2.336(2) 3_676 ? Ca2 OBO3 2.363(2) 4_565 ? Ca2 OA13 2.380(2) . ? Ca2 ODO3 2.528(2) 3_676 ? Ca2 OCM1 2.526(2) 2 ? Ca2 OBM3 2.593(2) . ? Ca2 OA13 2.808(2) 3_576 ? Ca2 Si23 3.1032(18) 3_676 ? Ca2 Si17 3.1562(17) . ? Ca2 Al13 3.2216(18) 2_455 ? Ca2 Al13 3.3127(19) 4_565 ? Ca3 OA11 2.3285(19) . ? Ca3 OA21 2.3408(17) . ? Ca3 OBO1 2.3486(18) . ? Ca3 ODO1 2.5386(19) . ? Ca3 OCM3 2.5713(19) . ? Ca3 OBM1 2.661(2) . ? Ca3 OA11 2.925(2) 3_575 ? Ca3 Si11 3.1065(10) . ? Ca3 Al21 3.1520(12) . ? Ca3 Al15 3.1825(12) 3_575 ? Ca3 Si11 3.2924(11) 3_575 ? Ca4 Ca2 0.5614(18) 3_676 ? Ca4 ODO3 2.278(2) . ? Ca4 OA23 2.287(2) . ? Ca4 OA13 2.509(3) 1_655 ? Ca4 OBO3 2.499(2) 2 ? Ca4 OA13 2.564(3) 3_676 ? Ca4 OCM1 2.833(2) 4_565 ? Ca4 ODM3 2.991(3) . ? Ca4 Al13 3.1719(19) 4_665 ? Ca4 Al13 3.2570(19) 2 ? Ca4 Si23 3.2472(18) . ? Ca4 Si17 3.413(2) 1_655 ? Si11 OCO1 1.5924(17) . ? Si11 OBO1 1.6140(17) 3_575 ? Si11 ODO1 1.6255(17) . ? Si11 OA11 1.6351(16) . ? Si11 Ca1 3.1174(12) 3_575 ? Si11 Ca3 3.2924(11) 3_575 ? Al13 OCO3 1.7157(17) . ? Al13 OBO3 1.7422(18) . ? Al13 OA13 1.7598(16) 2_544 ? Al13 ODO3 1.7599(18) 4_665 ? Al13 Ca4 3.1719(19) 4_665 ? Al13 Ca2 3.2216(18) 2_544 ? Al13 Ca4 3.2570(19) 2_444 ? Al13 Ca2 3.3127(19) 4_565 ? Al15 OBM1 1.7107(18) 3_575 ? Al15 ODM1 1.7204(19) . ? Al15 OCM1 1.7414(17) . ? Al15 OA11 1.7648(16) 3_575 ? Al15 Ca3 3.1825(12) 3_575 ? Si17 ODM3 1.588(2) 1_455 ? Si17 OBM3 1.5991(18) . ? Si17 OCM3 1.6202(17) 4_575 ? Si17 OA13 1.6433(16) . ? Si17 Ca4 3.413(2) 1_455 ? Si17 Ca4 3.5623(19) 3_676 ? Al21 ODM3 1.701(2) . ? Al21 OCM3 1.7413(17) . ? Al21 OBO1 1.7499(18) 3_675 ? Al21 OA21 1.7570(16) . ? Al21 Ca3 3.4749(11) 3_675 ? Si23 ODM1 1.592(2) . ? Si23 OCM1 1.6148(17) 4_565 ? Si23 OBO3 1.6243(17) 4_565 ? Si23 OA23 1.6343(16) . ? Si23 Ca2 3.1032(18) 3_676 ? Si25 OCO3 1.6031(17) . ? Si25 OBM1 1.6072(19) 3_675 ? Si25 ODO3 1.6314(19) . ? Si25 OA21 1.6403(16) . ? Si25 Ca3 3.5718(12) 3_675 ? Al27 OCO1 1.7205(17) 4_575 ? Al27 OBM3 1.7239(18) . ? Al27 OA23 1.7536(16) . ? Al27 ODO1 1.7559(18) . ? OA11 Al15 1.7648(16) 3_575 ? OA11 Ca1 2.403(2) 3_575 ? OA11 Ca3 2.925(2) 3_575 ? OA13 Al13 1.7598(16) 2_455 ? OA13 Ca4 2.509(3) 1_455 ? OA13 Ca4 2.564(3) 3_676 ? OA13 Ca2 2.808(2) 3_576 ? OA23 Ca2 2.336(2) 3_676 ? OBO1 Si11 1.6140(17) 3_575 ? OBO1 Al21 1.7499(18) 3_675 ? OBO3 Si23 1.6243(17) 4_565 ? OBO3 Ca2 2.363(2) 4_565 ? OBO3 Ca4 2.499(2) 2_444 ? OBM1 Si25 1.6072(19) 3_675 ? OBM1 Al15 1.7107(18) 3_575 ? OCO1 Al27 1.7205(17) 4_575 ? OCM1 Si23 1.6148(17) 4_565 ? OCM1 Ca2 2.526(2) 2_444 ? OCM1 Ca4 2.833(2) 4_565 ? OCM3 Si17 1.6202(17) 4_575 ? ODO3 Al13 1.7599(18) 4_665 ? ODO3 Ca2 2.528(2) 3_676 ? ODM3 Si17 1.5880(19) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ca3 Ca1 OA21 80.86(9) . . ? Ca3 Ca1 ODO1 93.43(10) . . ? OA21 Ca1 ODO1 111.16(7) . . ? Ca3 Ca1 OA11 114.45(11) . 3_575 ? OA21 Ca1 OA11 143.58(8) . 3_575 ? ODO1 Ca1 OA11 101.07(7) . 3_575 ? Ca3 Ca1 OBO1 70.68(9) . . ? OA21 Ca1 OBO1 96.34(6) . . ? ODO1 Ca1 OBO1 145.84(8) . . ? OA11 Ca1 OBO1 62.10(6) 3_575 . ? Ca3 Ca1 ODM1 168.83(11) . . ? OA21 Ca1 ODM1 107.06(7) . . ? ODO1 Ca1 ODM1 76.48(7) . . ? OA11 Ca1 ODM1 63.86(6) 3_575 . ? OBO1 Ca1 ODM1 115.27(7) . . ? Ca3 Ca1 OA11 55.77(9) . . ? OA21 Ca1 OA11 132.78(8) . . ? ODO1 Ca1 OA11 59.76(6) . . ? OA11 Ca1 OA11 78.16(6) 3_575 . ? OBO1 Ca1 OA11 86.83(6) . . ? ODM1 Ca1 OA11 113.94(6) . . ? Ca3 Ca1 Si11 92.19(9) . 3_575 ? OA21 Ca1 Si11 122.63(6) . 3_575 ? ODO1 Ca1 Si11 126.13(6) . 3_575 ? OA11 Ca1 Si11 31.17(4) 3_575 3_575 ? OBO1 Ca1 Si11 30.94(4) . 3_575 ? ODM1 Ca1 Si11 90.03(5) . 3_575 ? OA11 Ca1 Si11 80.55(5) . 3_575 ? Ca3 Ca1 Si11 78.00(9) . . ? OA21 Ca1 Si11 131.71(6) . . ? ODO1 Ca1 Si11 29.60(4) . . ? OA11 Ca1 Si11 84.64(5) 3_575 . ? OBO1 Ca1 Si11 116.24(6) . . ? ODM1 Ca1 Si11 90.82(5) . . ? OA11 Ca1 Si11 31.13(3) . . ? Si11 Ca1 Si11 101.19(3) 3_575 . ? Ca3 Ca1 Al15 145.32(10) . . ? OA21 Ca1 Al15 130.32(7) . . ? ODO1 Ca1 Al15 88.48(6) . . ? OA11 Ca1 Al15 32.01(4) 3_575 . ? OBO1 Ca1 Al15 88.72(5) . . ? ODM1 Ca1 Al15 31.85(4) . . ? OA11 Ca1 Al15 96.77(5) . . ? Si11 Ca1 Al15 59.85(3) 3_575 . ? Si11 Ca1 Al15 87.26(3) . . ? Ca3 Ca1 Si25 103.36(9) . . ? OA21 Ca1 Si25 25.91(4) . . ? ODO1 Ca1 Si25 121.81(6) . . ? OA11 Ca1 Si25 120.07(6) 3_575 . ? OBO1 Ca1 Si25 91.74(5) . . ? ODM1 Ca1 Si25 86.26(5) . . ? OA11 Ca1 Si25 158.25(6) . . ? Si11 Ca1 Si25 108.65(4) 3_575 . ? Si11 Ca1 Si25 150.00(4) . . ? Al15 Ca1 Si25 104.90(4) . . ? Ca3 Ca1 Al21 62.48(8) . . ? OA21 Ca1 Al21 26.66(4) . . ? ODO1 Ca1 Al21 91.96(5) . . ? OA11 Ca1 Al21 166.86(6) 3_575 . ? OBO1 Ca1 Al21 105.80(5) . . ? ODM1 Ca1 Al21 121.82(6) . . ? OA11 Ca1 Al21 107.48(6) . . ? Si11 Ca1 Al21 136.64(4) 3_575 . ? Si11 Ca1 Al21 106.39(4) . . ? Al15 Ca1 Al21 152.13(5) . . ? Si25 Ca1 Al21 52.16(2) . . ? Ca4 Ca2 OA23 78.1(3) 3_676 3_676 ? Ca4 Ca2 OBO3 97.5(4) 3_676 4_565 ? OA23 Ca2 OBO3 95.24(8) 3_676 4_565 ? Ca4 Ca2 OA13 102.9(3) 3_676 . ? OA23 Ca2 OA13 159.80(10) 3_676 . ? OBO3 Ca2 OA13 104.55(9) 4_565 . ? Ca4 Ca2 ODO3 57.6(3) 3_676 3_676 ? OA23 Ca2 ODO3 99.93(8) 3_676 3_676 ? OBO3 Ca2 ODO3 146.68(9) 4_565 3_676 ? OA13 Ca2 ODO3 65.32(7) . 3_676 ? Ca4 Ca2 OCM1 117.9(4) 3_676 2 ? OA23 Ca2 OCM1 62.27(7) 3_676 2 ? OBO3 Ca2 OCM1 129.90(8) 4_565 2 ? OA13 Ca2 OCM1 100.87(8) . 2 ? ODO3 Ca2 OCM1 83.33(7) 3_676 2 ? Ca4 Ca2 OBM3 161.8(4) 3_676 . ? OA23 Ca2 OBM3 120.03(8) 3_676 . ? OBO3 Ca2 OBM3 80.05(7) 4_565 . ? OA13 Ca2 OBM3 60.97(6) . . ? ODO3 Ca2 OBM3 116.22(8) 3_676 . ? OCM1 Ca2 OBM3 75.73(7) 2 . ? Ca4 Ca2 OA13 52.8(3) 3_676 3_576 ? OA23 Ca2 OA13 117.04(8) 3_676 3_576 ? OBO3 Ca2 OA13 60.85(6) 4_565 3_576 ? OA13 Ca2 OA13 77.16(7) . 3_576 ? ODO3 Ca2 OA13 85.83(6) 3_676 3_576 ? OCM1 Ca2 OA13 168.76(7) 2 3_576 ? OBM3 Ca2 OA13 112.01(8) . 3_576 ? Ca4 Ca2 Si23 99.9(3) 3_676 3_676 ? OA23 Ca2 Si23 31.09(4) 3_676 3_676 ? OBO3 Ca2 Si23 114.06(7) 4_565 3_676 ? OA13 Ca2 Si23 131.64(8) . 3_676 ? ODO3 Ca2 Si23 93.37(7) 3_676 3_676 ? OCM1 Ca2 Si23 31.25(4) 2 3_676 ? OBM3 Ca2 Si23 97.55(6) . 3_676 ? OA13 Ca2 Si23 147.42(7) 3_576 3_676 ? Ca4 Ca2 Si17 132.9(3) 3_676 . ? OA23 Ca2 Si17 146.71(7) 3_676 . ? OBO3 Ca2 Si17 92.20(7) 4_565 . ? OA13 Ca2 Si17 30.64(4) . . ? ODO3 Ca2 Si17 91.14(6) 3_676 . ? OCM1 Ca2 Si17 88.34(6) 2 . ? OBM3 Ca2 Si17 30.33(4) . . ? OA13 Ca2 Si17 94.87(6) 3_576 . ? Si23 Ca2 Si17 117.71(5) 3_676 . ? Ca4 Ca2 Al13 79.9(3) 3_676 2_455 ? OA23 Ca2 Al13 131.31(7) 3_676 2_455 ? OBO3 Ca2 Al13 130.48(8) 4_565 2_455 ? OA13 Ca2 Al13 32.41(4) . 2_455 ? ODO3 Ca2 Al13 32.93(5) 3_676 2_455 ? OCM1 Ca2 Al13 91.91(6) 2 2_455 ? OBM3 Ca2 Al13 87.96(6) . 2_455 ? OA13 Ca2 Al13 80.52(5) 3_576 2_455 ? Si23 Ca2 Al13 115.09(6) 3_676 2_455 ? Si17 Ca2 Al13 59.59(3) . 2_455 ? Ca4 Ca2 Al13 79.5(3) 3_676 4_565 ? OA23 Ca2 Al13 114.67(7) 3_676 4_565 ? OBO3 Ca2 Al13 30.26(5) 4_565 4_565 ? OA13 Ca2 Al13 85.09(6) . 4_565 ? ODO3 Ca2 Al13 117.05(6) 3_676 4_565 ? OCM1 Ca2 Al13 159.14(6) 2 4_565 ? OBM3 Ca2 Al13 90.21(6) . 4_565 ? OA13 Ca2 Al13 32.09(4) 3_576 4_565 ? Si23 Ca2 Al13 141.20(6) 3_676 4_565 ? Si17 Ca2 Al13 86.91(4) . 4_565 ? Al13 Ca2 Al13 103.09(5) 2_455 4_565 ? Ca1 Ca3 OA11 104.59(10) . . ? Ca1 Ca3 OA21 75.61(9) . . ? OA11 Ca3 OA21 160.92(7) . . ? Ca1 Ca3 OBO1 86.98(10) . . ? OA11 Ca3 OBO1 100.09(7) . . ? OA21 Ca3 OBO1 98.98(6) . . ? Ca1 Ca3 ODO1 64.73(9) . . ? OA11 Ca3 ODO1 62.47(6) . . ? OA21 Ca3 ODO1 101.91(6) . . ? OBO1 Ca3 ODO1 138.75(7) . . ? Ca1 Ca3 OCM3 125.76(10) . . ? OA11 Ca3 OCM3 99.57(6) . . ? OA21 Ca3 OCM3 66.84(6) . . ? OBO1 Ca3 OCM3 135.16(7) . . ? ODO1 Ca3 OCM3 85.96(6) . . ? Ca1 Ca3 OBM1 160.94(11) . . ? OA11 Ca3 OBM1 65.47(6) . . ? OA21 Ca3 OBM1 119.34(7) . . ? OBO1 Ca3 OBM1 79.29(7) . . ? ODO1 Ca3 OBM1 118.78(6) . . ? OCM3 Ca3 OBM1 73.03(6) . . ? Ca1 Ca3 OA11 48.42(9) . 3_575 ? OA11 Ca3 OA11 75.28(6) . 3_575 ? OA21 Ca3 OA11 115.52(6) . 3_575 ? OBO1 Ca3 OA11 55.87(5) . 3_575 ? ODO1 Ca3 OA11 82.99(6) . 3_575 ? OCM3 Ca3 OA11 168.95(6) . 3_575 ? OBM1 Ca3 OA11 112.53(6) . 3_575 ? Ca1 Ca3 Si11 84.66(9) . . ? OA11 Ca3 Si11 31.01(4) . . ? OA21 Ca3 Si11 132.40(5) . . ? OBO1 Ca3 Si11 123.06(5) . . ? ODO1 Ca3 Si11 31.47(4) . . ? OCM3 Ca3 Si11 92.77(5) . . ? OBM1 Ca3 Si11 91.77(5) . . ? OA11 Ca3 Si11 77.77(4) 3_575 . ? Ca1 Ca3 Al21 102.08(9) . . ? OA11 Ca3 Al21 132.09(6) . . ? OA21 Ca3 Al21 33.34(4) . . ? OBO1 Ca3 Al21 120.48(5) . . ? ODO1 Ca3 Al21 95.51(5) . . ? OCM3 Ca3 Al21 33.51(4) . . ? OBM1 Ca3 Al21 96.29(5) . . ? OA11 Ca3 Al21 147.98(5) 3_575 . ? Si11 Ca3 Al21 116.36(3) . . ? Ca1 Ca3 Al15 135.55(10) . 3_575 ? OA11 Ca3 Al15 32.96(4) . 3_575 ? OA21 Ca3 Al15 148.38(6) . 3_575 ? OBO1 Ca3 Al15 89.53(5) . 3_575 ? ODO1 Ca3 Al15 90.87(5) . 3_575 ? OCM3 Ca3 Al15 85.66(5) . 3_575 ? OBM1 Ca3 Al15 32.51(4) . 3_575 ? OA11 Ca3 Al15 94.50(4) 3_575 3_575 ? Si11 Ca3 Al15 60.81(2) . 3_575 ? Al21 Ca3 Al15 117.51(4) . 3_575 ? Ca1 Ca3 Si11 71.12(9) . 3_575 ? OA11 Ca3 Si11 82.86(5) . 3_575 ? OA21 Ca3 Si11 114.51(5) . 3_575 ? OBO1 Ca3 Si11 27.23(4) . 3_575 ? ODO1 Ca3 Si11 111.69(5) . 3_575 ? OCM3 Ca3 Si11 160.73(5) . 3_575 ? OBM1 Ca3 Si11 91.01(5) . 3_575 ? OA11 Ca3 Si11 29.75(3) 3_575 3_575 ? Si11 Ca3 Si11 98.58(3) . 3_575 ? Al21 Ca3 Si11 143.93(3) . 3_575 ? Al15 Ca3 Si11 86.36(3) 3_575 3_575 ? Ca2 Ca4 ODO3 110.4(4) 3_676 . ? Ca2 Ca4 OA23 88.0(3) 3_676 . ? ODO3 Ca4 OA23 109.44(9) . . ? Ca2 Ca4 OA13 117.0(3) 3_676 1_655 ? ODO3 Ca4 OA13 98.89(8) . 1_655 ? OA23 Ca4 OA13 132.70(10) . 1_655 ? Ca2 Ca4 OBO3 69.7(3) 3_676 2 ? ODO3 Ca4 OBO3 157.68(10) . 2 ? OA23 Ca4 OBO3 92.88(8) . 2 ? OA13 Ca4 OBO3 63.81(7) 1_655 2 ? Ca2 Ca4 OA13 64.8(3) 3_676 3_676 ? ODO3 Ca4 OA13 66.11(7) . 3_676 ? OA23 Ca4 OA13 146.24(10) . 3_676 ? OA13 Ca4 OA13 79.76(7) 1_655 3_676 ? OBO3 Ca4 OA13 95.63(8) 2 3_676 ? Ca2 Ca4 OCM1 52.0(3) 3_676 4_565 ? ODO3 Ca4 OCM1 81.43(8) . 4_565 ? OA23 Ca4 OCM1 57.78(6) . 4_565 ? OA13 Ca4 OCM1 167.28(9) 1_655 4_565 ? OBO3 Ca4 OCM1 112.22(8) 2 4_565 ? OA13 Ca4 OCM1 88.87(8) 3_676 4_565 ? Ca2 Ca4 ODM3 171.5(4) 3_676 . ? ODO3 Ca4 ODM3 71.22(7) . . ? OA23 Ca4 ODM3 99.40(8) . . ? OA13 Ca4 ODM3 54.77(6) 1_655 . ? OBO3 Ca4 ODM3 105.56(8) 2 . ? OA13 Ca4 ODM3 109.56(8) 3_676 . ? OCM1 Ca4 ODM3 135.90(8) 4_565 . ? Ca2 Ca4 Al13 90.0(3) 3_676 4_665 ? ODO3 Ca4 Al13 32.75(5) . 4_665 ? OA23 Ca4 Al13 136.24(8) . 4_665 ? OA13 Ca4 Al13 86.15(6) 1_655 4_665 ? OBO3 Ca4 Al13 127.00(8) 2 4_665 ? OA13 Ca4 Al13 33.66(4) 3_676 4_665 ? OCM1 Ca4 Al13 87.50(6) 4_565 4_665 ? ODM3 Ca4 Al13 87.49(6) . 4_665 ? Ca2 Ca4 Al13 90.8(3) 3_676 2 ? ODO3 Ca4 Al13 128.27(8) . 2 ? OA23 Ca4 Al13 118.25(8) . 2 ? OA13 Ca4 Al13 32.35(4) 1_655 2 ? OBO3 Ca4 Al13 31.91(4) 2 2 ? OA13 Ca4 Al13 83.49(6) 3_676 2 ? OCM1 Ca4 Al13 141.10(7) 4_565 2 ? ODM3 Ca4 Al13 82.06(6) . 2 ? Al13 Ca4 Al13 105.49(5) 4_665 2 ? Ca2 Ca4 Si23 70.3(3) 3_676 . ? ODO3 Ca4 Si23 94.70(7) . . ? OA23 Ca4 Si23 28.09(4) . . ? OA13 Ca4 Si23 160.58(8) 1_655 . ? OBO3 Ca4 Si23 105.75(7) 2 . ? OA13 Ca4 Si23 118.68(8) 3_676 . ? OCM1 Ca4 Si23 29.82(4) 4_565 . ? ODM3 Ca4 Si23 118.13(7) . . ? Al13 Ca4 Si23 112.49(6) 4_665 . ? Al13 Ca4 Si23 137.01(6) 2 . ? Ca2 Ca4 Si17 143.9(4) 3_676 1_655 ? ODO3 Ca4 Si17 83.52(7) . 1_655 ? OA23 Ca4 Si17 119.58(8) . 1_655 ? OA13 Ca4 Si17 27.12(4) 1_655 1_655 ? OBO3 Ca4 Si17 85.09(6) 2 1_655 ? OA13 Ca4 Si17 93.71(6) 3_676 1_655 ? OCM1 Ca4 Si17 162.19(7) 4_565 1_655 ? ODM3 Ca4 Si17 27.72(4) . 1_655 ? Al13 Ca4 Si17 84.96(4) 4_665 1_655 ? Al13 Ca4 Si17 56.69(3) 2 1_655 ? Si23 Ca4 Si17 143.81(6) . 1_655 ? OCO1 Si11 OBO1 111.21(9) . 3_575 ? OCO1 Si11 ODO1 110.24(9) . . ? OBO1 Si11 ODO1 113.82(10) 3_575 . ? OCO1 Si11 OA11 117.54(9) . . ? OBO1 Si11 OA11 101.86(9) 3_575 . ? ODO1 Si11 OA11 101.80(9) . . ? OCO1 Si11 Ca3 129.08(7) . . ? OBO1 Si11 Ca3 119.29(7) 3_575 . ? ODO1 Si11 Ca3 54.62(6) . . ? OA11 Si11 Ca3 47.20(6) . . ? OCO1 Si11 Ca1 132.42(7) . 3_575 ? OBO1 Si11 Ca1 52.35(7) 3_575 3_575 ? ODO1 Si11 Ca1 117.17(7) . 3_575 ? OA11 Si11 Ca1 49.53(7) . 3_575 ? Ca3 Si11 Ca1 79.29(3) . 3_575 ? OCO1 Si11 Ca1 140.27(7) . . ? OBO1 Si11 Ca1 107.82(7) 3_575 . ? ODO1 Si11 Ca1 44.34(6) . . ? OA11 Si11 Ca1 59.52(7) . . ? Ca3 Si11 Ca1 17.34(3) . . ? Ca1 Si11 Ca1 78.81(3) 3_575 . ? OCO1 Si11 Ca3 141.49(7) . 3_575 ? OBO1 Si11 Ca3 41.75(6) 3_575 3_575 ? ODO1 Si11 Ca3 106.97(7) . 3_575 ? OA11 Si11 Ca3 62.57(7) . 3_575 ? Ca3 Si11 Ca3 81.42(3) . 3_575 ? Ca1 Si11 Ca3 16.69(3) 3_575 3_575 ? Ca1 Si11 Ca3 75.91(3) . 3_575 ? OCO3 Al13 OBO3 112.94(8) . . ? OCO3 Al13 OA13 119.37(8) . 2_544 ? OBO3 Al13 OA13 98.19(9) . 2_544 ? OCO3 Al13 ODO3 111.47(9) . 4_665 ? OBO3 Al13 ODO3 115.95(9) . 4_665 ? OA13 Al13 ODO3 97.76(9) 2_544 4_665 ? OCO3 Al13 Ca4 135.70(7) . 4_665 ? OBO3 Al13 Ca4 111.35(7) . 4_665 ? OA13 Al13 Ca4 53.84(7) 2_544 4_665 ? ODO3 Al13 Ca4 44.44(7) 4_665 4_665 ? OCO3 Al13 Ca2 129.70(7) . 2_544 ? OBO3 Al13 Ca2 116.73(7) . 2_544 ? OA13 Al13 Ca2 46.44(6) 2_544 2_544 ? ODO3 Al13 Ca2 51.34(7) 4_665 2_544 ? Ca4 Al13 Ca2 10.04(3) 4_665 2_544 ? OCO3 Al13 Ca4 139.64(7) . 2_444 ? OBO3 Al13 Ca4 49.31(7) . 2_444 ? OA13 Al13 Ca4 49.72(7) 2_544 2_444 ? ODO3 Al13 Ca4 108.68(7) 4_665 2_444 ? Ca4 Al13 Ca4 74.51(5) 4_665 2_444 ? Ca2 Al13 Ca4 74.90(4) 2_544 2_444 ? OCO3 Al13 Ca2 144.42(7) . 4_565 ? OBO3 Al13 Ca2 43.12(6) . 4_565 ? OA13 Al13 Ca2 57.97(6) 2_544 4_565 ? ODO3 Al13 Ca2 103.82(7) 4_665 4_565 ? Ca4 Al13 Ca2 74.79(4) 4_665 4_565 ? Ca2 Al13 Ca2 76.91(5) 2_544 4_565 ? Ca4 Al13 Ca2 9.76(3) 2_444 4_565 ? OBM1 Al15 ODM1 113.49(10) 3_575 . ? OBM1 Al15 OCM1 113.62(9) 3_575 . ? ODM1 Al15 OCM1 110.48(9) . . ? OBM1 Al15 OA11 102.59(10) 3_575 3_575 ? ODM1 Al15 OA11 103.11(10) . 3_575 ? OCM1 Al15 OA11 112.85(8) . 3_575 ? OBM1 Al15 Ca3 56.72(8) 3_575 3_575 ? ODM1 Al15 Ca3 119.11(7) . 3_575 ? OCM1 Al15 Ca3 128.93(7) . 3_575 ? OA11 Al15 Ca3 45.87(6) 3_575 3_575 ? OBM1 Al15 Ca1 118.72(7) 3_575 . ? ODM1 Al15 Ca1 56.91(8) . . ? OCM1 Al15 Ca1 126.56(6) . . ? OA11 Al15 Ca1 46.20(6) 3_575 . ? Ca3 Al15 Ca1 76.10(3) 3_575 . ? ODM3 Si17 OBM3 113.86(11) 1_455 . ? ODM3 Si17 OCM3 109.92(10) 1_455 4_575 ? OBM3 Si17 OCM3 111.99(9) . 4_575 ? ODM3 Si17 OA13 105.09(11) 1_455 . ? OBM3 Si17 OA13 102.51(10) . . ? OCM3 Si17 OA13 113.14(8) 4_575 . ? ODM3 Si17 Ca2 120.83(8) 1_455 . ? OBM3 Si17 Ca2 54.96(8) . . ? OCM3 Si17 Ca2 128.57(7) 4_575 . ? OA13 Si17 Ca2 47.56(6) . . ? ODM3 Si17 Ca4 61.17(9) 1_455 1_455 ? OBM3 Si17 Ca4 115.74(8) . 1_455 ? OCM3 Si17 Ca4 130.48(7) 4_575 1_455 ? OA13 Si17 Ca4 44.10(7) . 1_455 ? Ca2 Si17 Ca4 73.58(3) . 1_455 ? ODM3 Si17 Ca4 118.29(8) 1_455 3_676 ? OBM3 Si17 Ca4 61.45(8) . 3_676 ? OCM3 Si17 Ca4 129.45(7) 4_575 3_676 ? OA13 Si17 Ca4 41.13(7) . 3_676 ? Ca2 Si17 Ca4 6.63(4) . 3_676 ? Ca4 Si17 Ca4 67.80(5) 1_455 3_676 ? ODM3 Al21 OCM3 115.98(9) . . ? ODM3 Al21 OBO1 112.63(11) . 3_675 ? OCM3 Al21 OBO1 112.82(9) . 3_675 ? ODM3 Al21 OA21 107.58(9) . . ? OCM3 Al21 OA21 101.66(8) . . ? OBO1 Al21 OA21 104.74(8) 3_675 . ? ODM3 Al21 Ca3 126.91(9) . . ? OCM3 Al21 Ca3 54.62(6) . . ? OBO1 Al21 Ca3 118.57(7) 3_675 . ? OA21 Al21 Ca3 47.08(5) . . ? ODM3 Al21 Ca3 136.83(7) . 3_675 ? OCM3 Al21 Ca3 106.41(6) . 3_675 ? OBO1 Al21 Ca3 37.71(6) 3_675 3_675 ? OA21 Al21 Ca3 69.73(6) . 3_675 ? Ca3 Al21 Ca3 84.15(3) . 3_675 ? ODM3 Al21 Ca1 114.79(9) . . ? OCM3 Al21 Ca1 66.84(6) . . ? OBO1 Al21 Ca1 125.72(7) 3_675 . ? OA21 Al21 Ca1 35.91(5) . . ? Ca3 Al21 Ca1 15.44(2) . . ? Ca3 Al21 Ca1 88.47(3) 3_675 . ? ODM1 Si23 OCM1 114.11(9) . 4_565 ? ODM1 Si23 OBO3 110.32(11) . 4_565 ? OCM1 Si23 OBO3 112.74(9) 4_565 4_565 ? ODM1 Si23 OA23 110.32(10) . . ? OCM1 Si23 OA23 101.70(8) 4_565 . ? OBO3 Si23 OA23 107.09(8) 4_565 . ? ODM1 Si23 Ca2 129.60(8) . 3_676 ? OCM1 Si23 Ca2 54.26(7) 4_565 3_676 ? OBO3 Si23 Ca2 119.25(8) 4_565 3_676 ? OA23 Si23 Ca2 47.57(6) . 3_676 ? ODM1 Si23 Ca4 121.43(9) . . ? OCM1 Si23 Ca4 60.74(7) 4_565 . ? OBO3 Si23 Ca4 125.62(8) 4_565 . ? OA23 Si23 Ca4 41.23(7) . . ? Ca2 Si23 Ca4 9.81(3) 3_676 . ? ODM1 Si23 Ca2 134.41(8) . . ? OCM1 Si23 Ca2 109.36(7) 4_565 . ? OBO3 Si23 Ca2 36.48(7) 4_565 . ? OA23 Si23 Ca2 72.46(6) . . ? Ca2 Si23 Ca2 87.19(4) 3_676 . ? Ca4 Si23 Ca2 91.30(5) . . ? OCO3 Si25 OBM1 112.02(9) . 3_675 ? OCO3 Si25 ODO3 111.66(9) . . ? OBM1 Si25 ODO3 109.12(11) 3_675 . ? OCO3 Si25 OA21 105.59(9) . . ? OBM1 Si25 OA21 109.59(9) 3_675 . ? ODO3 Si25 OA21 108.77(8) . . ? OCO3 Si25 Ca1 68.61(7) . . ? OBM1 Si25 Ca1 130.85(9) 3_675 . ? ODO3 Si25 Ca1 115.91(7) . . ? OA21 Si25 Ca1 37.72(6) . . ? OCO3 Si25 Ca4 104.68(7) . . ? OBM1 Si25 Ca4 135.48(9) 3_675 . ? ODO3 Si25 Ca4 30.73(7) . . ? OA21 Si25 Ca4 82.80(7) . . ? Ca1 Si25 Ca4 85.34(4) . . ? OCO3 Si25 Ca3 112.52(7) . 3_675 ? OBM1 Si25 Ca3 43.99(8) 3_675 3_675 ? ODO3 Si25 Ca3 134.86(7) . 3_675 ? OA21 Si25 Ca3 67.33(6) . 3_675 ? Ca1 Si25 Ca3 88.67(3) . 3_675 ? Ca4 Si25 Ca3 136.99(4) . 3_675 ? OCO1 Al27 OBM3 110.92(9) 4_575 . ? OCO1 Al27 OA23 105.26(8) 4_575 . ? OBM3 Al27 OA23 108.92(9) . . ? OCO1 Al27 ODO1 114.20(9) 4_575 . ? OBM3 Al27 ODO1 111.72(10) . . ? OA23 Al27 ODO1 105.33(8) . . ? OCO1 Al27 Ca1 111.57(6) 4_575 . ? OBM3 Al27 Ca1 134.45(8) . . ? OA23 Al27 Ca1 74.57(6) . . ? ODO1 Al27 Ca1 33.09(6) . . ? OCO1 Al27 Ca4 74.10(7) 4_575 . ? OBM3 Al27 Ca4 125.86(8) . . ? OA23 Al27 Ca4 31.59(6) . . ? ODO1 Al27 Ca4 114.15(7) . . ? Ca1 Al27 Ca4 81.51(4) . . ? OCO1 Al27 Ca2 110.35(7) 4_575 . ? OBM3 Al27 Ca2 42.61(7) . . ? OA23 Al27 Ca2 68.19(6) . . ? ODO1 Al27 Ca2 134.92(7) . . ? Ca1 Al27 Ca2 129.44(4) . . ? Ca4 Al27 Ca2 84.02(4) . . ? Si11 OA11 Al15 138.88(10) . 3_575 ? Si11 OA11 Ca3 101.78(8) . . ? Al15 OA11 Ca3 101.17(8) 3_575 . ? Si11 OA11 Ca1 99.29(8) . 3_575 ? Al15 OA11 Ca1 101.79(8) 3_575 3_575 ? Ca3 OA11 Ca1 114.10(7) . 3_575 ? Si11 OA11 Ca1 89.34(7) . . ? Al15 OA11 Ca1 119.81(8) 3_575 . ? Ca3 OA11 Ca1 19.63(3) . . ? Ca1 OA11 Ca1 101.84(6) 3_575 . ? Si11 OA11 Ca3 87.68(7) . 3_575 ? Al15 OA11 Ca3 118.48(8) 3_575 3_575 ? Ca3 OA11 Ca3 104.72(6) . 3_575 ? Ca1 OA11 Ca3 17.13(4) 3_575 3_575 ? Ca1 OA11 Ca3 89.23(5) . 3_575 ? Si17 OA13 Al13 137.29(10) . 2_455 ? Si17 OA13 Ca2 101.80(8) . . ? Al13 OA13 Ca2 101.15(9) 2_455 . ? Si17 OA13 Ca4 108.79(9) . 1_455 ? Al13 OA13 Ca4 97.93(8) 2_455 1_455 ? Ca2 OA13 Ca4 107.37(8) . 1_455 ? Si17 OA13 Ca4 113.94(9) . 3_676 ? Al13 OA13 Ca4 92.49(8) 2_455 3_676 ? Ca2 OA13 Ca4 12.33(4) . 3_676 ? Ca4 OA13 Ca4 100.24(7) 1_455 3_676 ? Si17 OA13 Ca2 119.00(9) . 3_576 ? Al13 OA13 Ca2 89.95(7) 2_455 3_576 ? Ca2 OA13 Ca2 102.84(7) . 3_576 ? Ca4 OA13 Ca2 10.26(5) 1_455 3_576 ? Ca4 OA13 Ca2 94.23(7) 3_676 3_576 ? Si25 OA21 Al21 124.59(10) . . ? Si25 OA21 Ca1 116.36(9) . . ? Al21 OA21 Ca1 117.43(8) . . ? Si25 OA21 Ca3 135.82(9) . . ? Al21 OA21 Ca3 99.58(7) . . ? Ca1 OA21 Ca3 23.52(4) . . ? Si23 OA23 Al27 124.14(10) . . ? Si23 OA23 Ca4 110.68(9) . . ? Al27 OA23 Ca4 124.73(9) . . ? Si23 OA23 Ca2 101.33(8) . 3_676 ? Al27 OA23 Ca2 134.42(9) . 3_676 ? Ca4 OA23 Ca2 13.90(5) . 3_676 ? Si11 OBO1 Al21 133.76(11) 3_575 3_675 ? Si11 OBO1 Ca3 111.01(9) 3_575 . ? Al21 OBO1 Ca3 115.18(8) 3_675 . ? Si11 OBO1 Ca1 96.70(8) 3_575 . ? Al21 OBO1 Ca1 127.72(9) 3_675 . ? Ca3 OBO1 Ca1 22.35(4) . . ? Si23 OBO3 Al13 133.31(12) 4_565 . ? Si23 OBO3 Ca2 119.40(9) 4_565 4_565 ? Al13 OBO3 Ca2 106.62(9) . 4_565 ? Si23 OBO3 Ca4 127.91(10) 4_565 2_444 ? Al13 OBO3 Ca4 98.78(8) . 2_444 ? Ca2 OBO3 Ca4 12.87(5) 4_565 2_444 ? Si25 OBM1 Al15 156.21(16) 3_675 3_575 ? Si25 OBM1 Ca3 111.21(10) 3_675 . ? Al15 OBM1 Ca3 90.77(9) 3_575 . ? Si17 OBM3 Al27 153.37(15) . . ? Si17 OBM3 Ca2 94.71(9) . . ? Al27 OBM3 Ca2 110.64(9) . . ? Si11 OCO1 Al27 132.05(10) . 4_575 ? Si25 OCO3 Al13 131.21(10) . . ? Si23 OCM1 Al15 130.62(10) 4_565 . ? Si23 OCM1 Ca2 94.49(8) 4_565 2_444 ? Al15 OCM1 Ca2 133.80(9) . 2_444 ? Si23 OCM1 Ca4 89.44(8) 4_565 4_565 ? Al15 OCM1 Ca4 136.17(9) . 4_565 ? Ca2 OCM1 Ca4 10.08(4) 2_444 4_565 ? Si17 OCM3 Al21 128.47(10) 4_575 . ? Si17 OCM3 Ca3 137.46(9) 4_575 . ? Al21 OCM3 Ca3 91.87(7) . . ? Si11 ODO1 Al27 131.58(11) . . ? Si11 ODO1 Ca1 106.06(9) . . ? Al27 ODO1 Ca1 122.28(9) . . ? Si11 ODO1 Ca3 93.92(8) . . ? Al27 ODO1 Ca3 132.45(9) . . ? Ca1 ODO1 Ca3 21.85(4) . . ? Si25 ODO3 Al13 129.23(11) . 4_665 ? Si25 ODO3 Ca4 127.80(11) . . ? Al13 ODO3 Ca4 102.81(9) 4_665 . ? Si25 ODO3 Ca2 133.14(11) . 3_676 ? Al13 ODO3 Ca2 95.74(9) 4_665 3_676 ? Ca4 ODO3 Ca2 12.02(6) . 3_676 ? Si23 ODM1 Al15 151.07(15) . . ? Si23 ODM1 Ca1 116.03(10) . . ? Al15 ODM1 Ca1 91.24(9) . . ? Si17 ODM3 Al21 150.29(16) 1_655 . ? Si17 ODM3 Ca4 91.11(10) 1_655 . ? Al21 ODM3 Ca4 115.61(10) . . ?