data_omp4p11 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common omphacite _chemical_formula_moiety ? _chemical_formula_sum 'Al Ca Cr Fe Fe Mg Mn Na O O Si Si Si Ti' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 7340000 _chemical_formula_weight 497.14 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 0.0060 '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-2 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si+4 0.0720 0.0710 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si+2 0.0720 0.0710 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al+3 0.0560 0.0520 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe+2 0.3010 0.8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe+3 0.3010 0.8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg+2 0.0420 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca+2 0.2030 0.3060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na+1 0.0300 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn+2 0.2950 0.7290 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti+4 0.2480 0.4460 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr+3 0.2840 0.6240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_int_tables_number 13 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 9.3992(6) _cell_length_b 8.5857(7) _cell_length_c 5.1593(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.216(5) _cell_angle_gamma 90.00 _cell_volume 399.78(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 211 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1433 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 29.85 _reflns_number_total 497 _reflns_number_gt 285 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.023(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 497 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1698 _refine_ls_R_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.2856 _refine_ls_wR_factor_gt 0.2433 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 O11 O 0.3608(10) 0.3393(8) 0.1201(14) 0.0036(19) Uiso 1 1 d . . . O12 O 0.3620(11) 0.1754(10) 0.6527(16) 0.016(2) Uiso 1 1 d . . . O21 O 0.6166(10) 0.5167(10) 0.3154(15) 0.012(2) Uiso 1 1 d . . . O22 O 0.6070(10) 0.9926(9) 0.8135(15) 0.012(2) Uiso 1 1 d . . . O31 O 0.6057(10) 0.2719(10) -0.0034(15) 0.011(2) Uiso 1 1 d . . . O32 O 0.5999(11) 0.2353(10) 0.4909(15) 0.013(2) Uiso 1 1 d . . . Si1A Si 0.5392(5) 0.3495(4) 0.2253(6) 0.0098(11) Uiso 0.50 1 d P . . Si1B Si+4 0.5392(5) 0.3495(4) 0.2253(6) 0.0098(11) Uiso 0.50 1 d P . . Si2A Si+2 0.5378(5) 0.1608(4) 0.7293(6) 0.0102(11) Uiso 0.96 1 d P . . SI2B Al+3 0.5378(5) 0.1608(4) 0.7293(6) 0.0102(11) Uiso 0.04 1 d P . . M1A Mg+2 0.2500 0.1599(6) 0.2500 0.0100(15) Uiso 0.84 2 d SP . . M1B Fe+2 0.2500 0.1599(6) 0.2500 0.0100(15) Uiso 0.09 2 d SP . . M1C Al+3 0.2500 0.1599(6) 0.2500 0.0100(15) Uiso 0.07 2 d SP . . M1D Mn+2 0.2500 0.1599(6) 0.2500 0.0100(15) Uiso 0.00 2 d SP . . M11A Mg+2 0.2500 0.3451(6) 0.7500 0.0124(15) Uiso 0.02 2 d SP . . M11B Fe+2 0.2500 0.3451(6) 0.7500 0.0124(15) Uiso 0.02 2 d SP . . M11C Al+3 0.2500 0.3451(6) 0.7500 0.0124(15) Uiso 0.96 2 d SP . . M11D Ti+4 0.2500 0.3451(6) 0.7500 0.0124(15) Uiso 0.01 2 d SP . . M11E Cr+3 0.2500 0.3451(6) 0.7500 0.0124(15) Uiso 0.00 2 d SP . . M2A Ca+2 0.2500 0.5553(6) 0.2500 0.0128(15) Uiso 0.25 2 d SP . . M2B Na+1 0.2500 0.5553(6) 0.2500 0.0128(15) Uiso 0.74 2 d SP . . M2C Fe+2 0.2500 0.5553(6) 0.2500 0.0128(15) Uiso 0.01 2 d SP . . M21A Ca+2 0.2500 0.9470(5) 0.7500 0.0128(13) Uiso 0.71 2 d SP . . M21B Na+1 0.2500 0.9470(5) 0.7500 0.0128(13) Uiso 0.23 2 d SP . . M21C Mg+2 0.2500 0.9470(5) 0.7500 0.0128(13) Uiso 0.06 2 d SP . . O000 Si 0.0000 0.0000 0.0000 0.050 Uiso 0.00 2 d SP . . O010 Si 0.0000 1.0000 0.0000 0.050 Uiso 0.00 2 d SP . . O001 Si 0.0000 0.0000 1.0000 0.050 Uiso 0.00 2 d SP . . _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 O11 Si1A 1.614(10) . ? O11 M11E 1.903(8) 1_554 ? O11 M11D 1.903(8) 1_554 ? O11 M11B 1.903(8) 1_554 ? O11 M11A 1.903(8) 1_554 ? O11 M1A 2.072(8) . ? O11 M2A 2.316(8) . ? O12 Si2A 1.593(10) . ? O12 M11A 1.944(9) . ? O12 M1A 2.054(9) . ? O12 M21C 2.345(9) 1_545 ? O12 M21A 2.345(9) 1_545 ? O21 Si1A 1.618(9) . ? O21 M11E 1.825(9) 3_666 ? O21 M11A 1.825(9) 3_666 ? O21 M11B 1.825(9) 3_666 ? O21 M11D 1.825(9) 3_666 ? O21 M2C 2.327(8) 3_666 ? O21 M2A 2.327(8) 3_666 ? O21 O22 4.841(11) . ? O22 SI2B 1.593(9) 1_565 ? O22 Si2A 1.593(9) 1_565 ? O22 M1D 1.968(9) 3_666 ? O22 M1A 1.968(9) 3_666 ? O22 M21C 2.336(8) 3_677 ? O22 M21A 2.336(8) 3_677 ? O22 O21 4.824(11) 1_556 ? O31 Si1A 1.625(8) . ? O31 SI2B 1.652(9) 1_554 ? O31 Si2A 1.652(9) 1_554 ? O31 M21C 2.468(9) 3_666 ? O31 M21A 2.468(9) 3_666 ? O31 M2A 2.573(8) 3_665 ? O31 O32 2.585(8) . ? O32 O32 0.094(16) ? ? O32 Si2A 1.633(8) . ? O32 Si1A 1.651(9) . ? O32 M2A 2.440(10) 3_666 ? O32 M21A 2.639(8) 3_666 ? O32 M21C 2.639(8) 3_666 ? O32 O31 2.648(13) ? ? Si1A O32 1.722(8) ? ? Si1A M2A 2.988(4) 3_666 ? Si1A M11E 3.111(4) 1_554 ? Si1A M11D 3.111(4) 1_554 ? Si1A M11A 3.111(4) 1_554 ? Si1A M1A 3.201(5) . ? Si1A M21C 3.207(5) 3_666 ? Si2A O32 1.553(12) ? ? Si2A O22 1.593(9) 1_545 ? Si2A O31 1.677(8) ? ? Si2A M21C 3.009(4) 3_667 ? Si2A M21A 3.009(4) 3_667 ? Si2A M1A 3.114(4) . ? Si2A M2A 3.132(6) 3_666 ? Si2A M11A 3.162(5) . ? M1A O22 1.968(9) 2_464 ? M1A O22 1.968(9) 3_666 ? M1A O12 2.054(9) 4_656 ? M1A O11 2.072(8) 4_656 ? M1A M11A 3.031(4) . ? M1A M11E 3.031(4) 1_554 ? M1A M11D 3.031(4) 1_554 ? M11A O21 1.825(9) 3_666 ? M11A O21 1.825(9) 2_465 ? M11A O11 1.903(8) 4_656 ? M11A O11 1.903(8) 1_556 ? M11A O12 1.944(9) 4_657 ? M11A M1D 3.031(4) 1_556 ? M11A M1A 3.031(4) 1_556 ? M11A Si1B 3.111(4) 4_656 ? M11A Si1A 3.111(4) 4_656 ? M2A O11 2.316(8) 4_656 ? M2A O21 2.327(8) 2_464 ? M2A O21 2.327(8) 3_666 ? M2A O32 2.440(10) 3_666 ? M2A O32 2.440(10) 2_464 ? M2A O31 2.573(8) 3_665 ? M2A O31 2.573(8) 2_465 ? M2A Si1B 2.988(4) 3_666 ? M2A Si1A 2.988(4) 3_666 ? M2A Si1B 2.988(4) 2_464 ? M2A Si1A 2.988(4) 2_464 ? M21A O22 2.336(8) 3_677 ? M21A O22 2.336(8) 2_474 ? M21A O12 2.345(9) 1_565 ? M21A O12 2.345(9) 4_667 ? M21A O31 2.468(9) 2_465 ? M21A O31 2.468(9) 3_666 ? M21A O32 2.639(8) 2_465 ? M21A O32 2.639(8) 3_666 ? M21A SI2B 3.009(4) 2_464 ? M21A Si2A 3.009(4) 2_464 ? M21A SI2B 3.009(4) 3_667 ? M21A Si2A 3.009(4) 3_667 ? 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 Si1A O11 M11E 124.2(4) . 1_554 ? Si1A O11 M11D 124.2(4) . 1_554 ? M11E O11 M11D 0.0(3) 1_554 1_554 ? Si1A O11 M11B 124.2(4) . 1_554 ? M11E O11 M11B 0.0(3) 1_554 1_554 ? M11D O11 M11B 0.0(3) 1_554 1_554 ? Si1A O11 M11A 124.2(4) . 1_554 ? M11E O11 M11A 0.0(3) 1_554 1_554 ? M11D O11 M11A 0.0(3) 1_554 1_554 ? M11B O11 M11A 0.0(3) 1_554 1_554 ? Si1A O11 M1A 120.0(4) . . ? M11E O11 M1A 99.2(4) 1_554 . ? M11D O11 M1A 99.2(4) 1_554 . ? M11B O11 M1A 99.2(4) 1_554 . ? M11A O11 M1A 99.2(4) 1_554 . ? Si1A O11 M2A 111.6(4) . . ? M11E O11 M2A 96.0(4) 1_554 . ? M11D O11 M2A 96.0(4) 1_554 . ? M11B O11 M2A 96.0(4) 1_554 . ? M11A O11 M2A 96.0(4) 1_554 . ? M1A O11 M2A 101.2(3) . . ? Si2A O12 M11A 126.4(6) . . ? Si2A O12 M1A 116.7(4) . . ? M11A O12 M1A 98.5(4) . . ? Si2A O12 M21C 112.2(5) . 1_545 ? M11A O12 M21C 105.3(4) . 1_545 ? M1A O12 M21C 91.6(4) . 1_545 ? Si2A O12 M21A 112.2(5) . 1_545 ? M11A O12 M21A 105.3(4) . 1_545 ? M1A O12 M21A 91.6(4) . 1_545 ? M21C O12 M21A 0.00(11) 1_545 1_545 ? Si1A O21 M11E 143.2(5) . 3_666 ? Si1A O21 M11A 143.2(5) . 3_666 ? M11E O21 M11A 0.0(2) 3_666 3_666 ? Si1A O21 M11B 143.2(5) . 3_666 ? M11E O21 M11B 0.0(2) 3_666 3_666 ? M11A O21 M11B 0.0(2) 3_666 3_666 ? Si1A O21 M11D 143.2(5) . 3_666 ? M11E O21 M11D 0.0(2) 3_666 3_666 ? M11A O21 M11D 0.0(2) 3_666 3_666 ? M11B O21 M11D 0.0(2) 3_666 3_666 ? Si1A O21 M2C 96.8(4) . 3_666 ? M11E O21 M2C 97.9(4) 3_666 3_666 ? M11A O21 M2C 97.9(4) 3_666 3_666 ? M11B O21 M2C 97.9(4) 3_666 3_666 ? M11D O21 M2C 97.9(4) 3_666 3_666 ? Si1A O21 M2A 96.8(4) . 3_666 ? M11E O21 M2A 97.9(4) 3_666 3_666 ? M11A O21 M2A 97.9(4) 3_666 3_666 ? M11B O21 M2A 97.9(4) 3_666 3_666 ? M11D O21 M2A 97.9(4) 3_666 3_666 ? M2C O21 M2A 0.0(3) 3_666 3_666 ? Si1A O21 O22 145.9(4) . . ? M11E O21 O22 70.4(3) 3_666 . ? M11A O21 O22 70.4(3) 3_666 . ? M11B O21 O22 70.4(3) 3_666 . ? M11D O21 O22 70.4(3) 3_666 . ? M2C O21 O22 78.3(2) 3_666 . ? M2A O21 O22 78.3(2) 3_666 . ? SI2B O22 Si2A 0.0(3) 1_565 1_565 ? SI2B O22 M1D 143.4(5) 1_565 3_666 ? Si2A O22 M1D 143.4(5) 1_565 3_666 ? SI2B O22 M1A 143.4(5) 1_565 3_666 ? Si2A O22 M1A 143.4(5) 1_565 3_666 ? M1D O22 M1A 0.0(2) 3_666 3_666 ? SI2B O22 M21C 98.2(4) 1_565 3_677 ? Si2A O22 M21C 98.2(4) 1_565 3_677 ? M1D O22 M21C 94.1(4) 3_666 3_677 ? M1A O22 M21C 94.1(4) 3_666 3_677 ? SI2B O22 M21A 98.2(4) 1_565 3_677 ? Si2A O22 M21A 98.2(4) 1_565 3_677 ? M1D O22 M21A 94.1(4) 3_666 3_677 ? M1A O22 M21A 94.1(4) 3_666 3_677 ? M21C O22 M21A 0.0 3_677 3_677 ? SI2B O22 O21 149.2(4) 1_565 1_556 ? Si2A O22 O21 149.2(4) 1_565 1_556 ? M1D O22 O21 67.3(3) 3_666 1_556 ? M1A O22 O21 67.3(3) 3_666 1_556 ? M21C O22 O21 75.6(2) 3_677 1_556 ? M21A O22 O21 75.6(2) 3_677 1_556 ? SI2B O22 O21 133.4(4) 1_565 . ? Si2A O22 O21 133.4(4) 1_565 . ? M1D O22 O21 40.1(2) 3_666 . ? M1A O22 O21 40.1(2) 3_666 . ? M21C O22 O21 127.5(3) 3_677 . ? M21A O22 O21 127.5(3) 3_677 . ? O21 O22 O21 64.52(15) 1_556 . ? Si1A O31 SI2B 134.9(7) . 1_554 ? Si1A O31 Si2A 134.9(7) . 1_554 ? SI2B O31 Si2A 0.0(4) 1_554 1_554 ? Si1A O31 M21C 101.2(4) . 3_666 ? SI2B O31 M21C 91.7(4) 1_554 3_666 ? Si2A O31 M21C 91.7(4) 1_554 3_666 ? Si1A O31 M21A 101.2(4) . 3_666 ? SI2B O31 M21A 91.7(4) 1_554 3_666 ? Si2A O31 M21A 91.7(4) 1_554 3_666 ? M21C O31 M21A 0.00(13) 3_666 3_666 ? Si1A O31 M2A 119.1(4) . 3_665 ? SI2B O31 M2A 93.1(3) 1_554 3_665 ? Si2A O31 M2A 93.1(3) 1_554 3_665 ? M21C O31 M2A 114.4(3) 3_666 3_665 ? M21A O31 M2A 114.4(3) 3_666 3_665 ? Si1A O31 O32 38.3(3) . . ? SI2B O31 O32 130.1(5) 1_554 . ? Si2A O31 O32 130.1(5) 1_554 . ? M21C O31 O32 62.9(3) 3_666 . ? M21A O31 O32 62.9(3) 3_666 . ? M2A O31 O32 135.8(4) 3_665 . ? O32 O32 Si2A 31.4(4) ? . ? O32 O32 Si1A 137.1(3) ? . ? Si2A O32 Si1A 138.1(7) . . ? O32 O32 M2A 67.26(16) ? 3_666 ? Si2A O32 M2A 98.6(4) . 3_666 ? Si1A O32 M2A 91.7(4) . 3_666 ? O32 O32 O31 172.9(3) ? . ? Si2A O32 O31 154.3(6) . . ? Si1A O32 O31 37.5(3) . . ? M2A O32 O31 106.4(4) 3_666 . ? O32 O32 M21A 128.33(19) ? 3_666 ? Si2A O32 M21A 118.2(4) . 3_666 ? Si1A O32 M21A 93.9(3) . 3_666 ? M2A O32 M21A 113.1(3) 3_666 3_666 ? O31 O32 M21A 56.4(2) . 3_666 ? O32 O32 M21C 128.33(19) ? 3_666 ? Si2A O32 M21C 118.2(4) . 3_666 ? Si1A O32 M21C 93.9(3) . 3_666 ? M2A O32 M21C 113.1(3) 3_666 3_666 ? O31 O32 M21C 56.4(2) . 3_666 ? M21A O32 M21C 0.00(15) 3_666 3_666 ? O32 O32 O31 6.9(3) ? ? ? Si2A O32 O31 37.4(3) . ? ? Si1A O32 O31 131.6(5) . ? ? M2A O32 O31 61.2(3) 3_666 ? ? O31 O32 O31 166.0(5) . ? ? M21A O32 O31 132.5(4) 3_666 ? ? M21C O32 O31 132.5(4) 3_666 ? ? O11 Si1A O21 119.1(4) . . ? O11 Si1A O31 107.9(5) . . ? O21 Si1A O31 109.8(4) . . ? O11 Si1A O32 109.4(5) . . ? O21 Si1A O32 105.4(5) . . ? O31 Si1A O32 104.2(4) . . ? O11 Si1A O32 108.8(5) . ? ? O21 Si1A O32 104.2(4) . ? ? O31 Si1A O32 106.3(5) . ? ? O32 Si1A O32 2.1(4) . ? ? O11 Si1A M2A 133.1(3) . 3_666 ? O21 Si1A M2A 50.6(3) . 3_666 ? O31 Si1A M2A 118.5(4) . 3_666 ? O32 Si1A M2A 54.7(3) . 3_666 ? O32 Si1A M2A 53.6(3) ? 3_666 ? O11 Si1A M11E 30.4(2) . 1_554 ? O21 Si1A M11E 117.4(4) . 1_554 ? O31 Si1A M11E 81.4(4) . 1_554 ? O32 Si1A M11E 132.1(4) . 1_554 ? O32 Si1A M11E 132.3(4) ? 1_554 ? M2A Si1A M11E 158.41(17) 3_666 1_554 ? O11 Si1A M11D 30.4(2) . 1_554 ? O21 Si1A M11D 117.4(4) . 1_554 ? O31 Si1A M11D 81.4(4) . 1_554 ? O32 Si1A M11D 132.1(4) . 1_554 ? O32 Si1A M11D 132.3(4) ? 1_554 ? M2A Si1A M11D 158.41(17) 3_666 1_554 ? M11E Si1A M11D 0.00(19) 1_554 1_554 ? O11 Si1A M11A 30.4(2) . 1_554 ? O21 Si1A M11A 117.4(4) . 1_554 ? O31 Si1A M11A 81.4(4) . 1_554 ? O32 Si1A M11A 132.1(4) . 1_554 ? O32 Si1A M11A 132.3(4) ? 1_554 ? M2A Si1A M11A 158.41(17) 3_666 1_554 ? M11E Si1A M11A 0.00(19) 1_554 1_554 ? M11D Si1A M11A 0.00(19) 1_554 1_554 ? O11 Si1A M1A 34.1(3) . . ? O21 Si1A M1A 139.3(3) . . ? O31 Si1A M1A 108.9(4) . . ? O32 Si1A M1A 76.5(4) . . ? O32 Si1A M1A 76.1(4) ? . ? M2A Si1A M1A 117.31(11) 3_666 . ? M11E Si1A M1A 57.36(10) 1_554 . ? M11D Si1A M1A 57.36(10) 1_554 . ? M11A Si1A M1A 57.36(10) 1_554 . ? O11 Si1A M21C 122.9(3) . 3_666 ? O21 Si1A M21C 118.0(4) . 3_666 ? O31 Si1A M21C 49.0(3) . 3_666 ? O32 Si1A M21C 55.2(3) . 3_666 ? O32 Si1A M21C 57.3(4) ? 3_666 ? M2A Si1A M21C 86.27(14) 3_666 3_666 ? M11E Si1A M21C 114.58(14) 1_554 3_666 ? M11D Si1A M21C 114.58(14) 1_554 3_666 ? M11A Si1A M21C 114.58(14) 1_554 3_666 ? M1A Si1A M21C 96.71(13) . 3_666 ? O32 Si2A O22 111.4(5) ? 1_545 ? O32 Si2A O12 111.2(4) ? . ? O22 Si2A O12 117.1(5) 1_545 . ? O32 Si2A O32 1.8(3) ? . ? O22 Si2A O32 110.9(4) 1_545 . ? O12 Si2A O32 110.3(5) . . ? O32 Si2A O31 104.5(5) ? ? ? O22 Si2A O31 104.8(4) 1_545 ? ? O12 Si2A O31 106.8(5) . ? ? O32 Si2A O31 106.3(6) . ? ? O32 Si2A M21C 119.3(4) ? 3_667 ? O22 Si2A M21C 50.2(3) 1_545 3_667 ? O12 Si2A M21C 129.0(3) . 3_667 ? O32 Si2A M21C 120.4(4) . 3_667 ? O31 Si2A M21C 54.6(3) ? 3_667 ? O32 Si2A M21A 119.3(4) ? 3_667 ? O22 Si2A M21A 50.2(3) 1_545 3_667 ? O12 Si2A M21A 129.0(3) . 3_667 ? O32 Si2A M21A 120.4(4) . 3_667 ? O31 Si2A M21A 54.6(3) ? 3_667 ? M21C Si2A M21A 0.00(15) 3_667 3_667 ? O32 Si2A M1A 80.8(3) ? . ? O22 Si2A M1A 114.3(4) 1_545 . ? O12 Si2A M1A 36.1(3) . . ? O32 Si2A M1A 79.4(4) . . ? O31 Si2A M1A 135.4(4) ? . ? M21C Si2A M1A 156.97(16) 3_667 . ? M21A Si2A M1A 156.97(16) 3_667 . ? O32 Si2A M2A 48.6(3) ? 3_666 ? O22 Si2A M2A 119.2(4) 1_545 3_666 ? O12 Si2A M2A 123.6(4) . 3_666 ? O32 Si2A M2A 50.4(3) . 3_666 ? O31 Si2A M2A 55.9(4) ? 3_666 ? M21C Si2A M2A 87.24(13) 3_667 3_666 ? M21A Si2A M2A 87.24(13) 3_667 3_666 ? M1A Si2A M2A 115.63(13) . 3_666 ? O32 Si2A M11A 108.6(4) ? . ? O22 Si2A M11A 137.1(3) 1_545 . ? O12 Si2A M11A 29.6(3) . . ? O32 Si2A M11A 108.6(4) . . ? O31 Si2A M11A 79.3(4) ? . ? M21C Si2A M11A 118.93(10) 3_667 . ? M21A Si2A M11A 118.93(10) 3_667 . ? M1A Si2A M11A 57.74(10) . . ? M2A Si2A M11A 98.74(14) 3_666 . ? O22 M1A O22 96.6(5) 2_464 3_666 ? O22 M1A O12 91.7(3) 2_464 4_656 ? O22 M1A O12 93.2(3) 3_666 4_656 ? O22 M1A O12 93.2(3) 2_464 . ? O22 M1A O12 91.7(3) 3_666 . ? O12 M1A O12 172.6(5) 4_656 . ? O22 M1A O11 167.5(4) 2_464 . ? O22 M1A O11 90.7(3) 3_666 . ? O12 M1A O11 77.7(3) 4_656 . ? O12 M1A O11 96.7(3) . . ? O22 M1A O11 90.7(3) 2_464 4_656 ? O22 M1A O11 167.5(4) 3_666 4_656 ? O12 M1A O11 96.7(3) 4_656 4_656 ? O12 M1A O11 77.7(3) . 4_656 ? O11 M1A O11 84.0(4) . 4_656 ? O22 M1A M11A 92.6(2) 2_464 . ? O22 M1A M11A 130.8(2) 3_666 . ? O12 M1A M11A 134.8(3) 4_656 . ? O12 M1A M11A 39.4(2) . . ? O11 M1A M11A 90.3(2) . . ? O11 M1A M11A 38.3(2) 4_656 . ? O22 M1A M11E 130.8(2) 2_464 1_554 ? O22 M1A M11E 92.6(2) 3_666 1_554 ? O12 M1A M11E 39.4(2) 4_656 1_554 ? O12 M1A M11E 134.8(3) . 1_554 ? O11 M1A M11E 38.3(2) . 1_554 ? O11 M1A M11E 90.3(2) 4_656 1_554 ? M11A M1A M11E 116.7(2) . 1_554 ? O22 M1A M11D 130.8(2) 2_464 1_554 ? O22 M1A M11D 92.6(2) 3_666 1_554 ? O12 M1A M11D 39.4(2) 4_656 1_554 ? O12 M1A M11D 134.8(3) . 1_554 ? O11 M1A M11D 38.3(2) . 1_554 ? O11 M1A M11D 90.3(2) 4_656 1_554 ? M11A M1A M11D 116.7(2) . 1_554 ? M11E M1A M11D 0.00(16) 1_554 1_554 ? O21 M11A O21 98.9(6) 3_666 2_465 ? O21 M11A O11 92.5(3) 3_666 4_656 ? O21 M11A O11 89.5(3) 2_465 4_656 ? O21 M11A O11 89.5(3) 3_666 1_556 ? O21 M11A O11 92.5(3) 2_465 1_556 ? O11 M11A O11 177.0(5) 4_656 1_556 ? O21 M11A O12 170.0(4) 3_666 4_657 ? O21 M11A O12 89.4(4) 2_465 4_657 ? O11 M11A O12 93.2(4) 4_656 4_657 ? O11 M11A O12 84.5(4) 1_556 4_657 ? O21 M11A O12 89.4(4) 3_666 . ? O21 M11A O12 170.0(4) 2_465 . ? O11 M11A O12 84.5(4) 4_656 . ? O11 M11A O12 93.2(4) 1_556 . ? O12 M11A O12 82.9(5) 4_657 . ? O21 M11A M1A 91.2(2) 3_666 . ? O21 M11A M1A 131.4(3) 2_465 . ? O11 M11A M1A 42.4(2) 4_656 . ? O11 M11A M1A 135.2(3) 1_556 . ? O12 M11A M1A 87.4(3) 4_657 . ? O12 M11A M1A 42.1(3) . . ? O21 M11A M1D 131.4(3) 3_666 1_556 ? O21 M11A M1D 91.2(2) 2_465 1_556 ? O11 M11A M1D 135.2(3) 4_656 1_556 ? O11 M11A M1D 42.4(2) 1_556 1_556 ? O12 M11A M1D 42.1(3) 4_657 1_556 ? O12 M11A M1D 87.4(3) . 1_556 ? M1A M11A M1D 116.7(2) . 1_556 ? O21 M11A M1A 131.4(3) 3_666 1_556 ? O21 M11A M1A 91.2(2) 2_465 1_556 ? O11 M11A M1A 135.2(3) 4_656 1_556 ? O11 M11A M1A 42.4(2) 1_556 1_556 ? O12 M11A M1A 42.1(3) 4_657 1_556 ? O12 M11A M1A 87.4(3) . 1_556 ? M1A M11A M1A 116.7(2) . 1_556 ? M1D M11A M1A 0.00(16) 1_556 1_556 ? O21 M11A Si1B 109.9(3) 3_666 4_656 ? O21 M11A Si1B 69.1(3) 2_465 4_656 ? O11 M11A Si1B 25.4(2) 4_656 4_656 ? O11 M11A Si1B 154.7(2) 1_556 4_656 ? O12 M11A Si1B 78.2(3) 4_657 4_656 ? O12 M11A Si1B 102.8(3) . 4_656 ? M1A M11A Si1B 62.81(8) . 4_656 ? M1D M11A Si1B 118.01(10) 1_556 4_656 ? M1A M11A Si1B 118.01(10) 1_556 4_656 ? O21 M11A Si1A 109.9(3) 3_666 4_656 ? O21 M11A Si1A 69.1(3) 2_465 4_656 ? O11 M11A Si1A 25.4(2) 4_656 4_656 ? O11 M11A Si1A 154.7(2) 1_556 4_656 ? O12 M11A Si1A 78.2(3) 4_657 4_656 ? O12 M11A Si1A 102.8(3) . 4_656 ? M1A M11A Si1A 62.81(8) . 4_656 ? M1D M11A Si1A 118.01(10) 1_556 4_656 ? M1A M11A Si1A 118.01(10) 1_556 4_656 ? Si1B M11A Si1A 0.00(12) 4_656 4_656 ? O11 M2A O11 73.5(4) 4_656 . ? O11 M2A O21 84.3(3) 4_656 2_464 ? O11 M2A O21 70.9(3) . 2_464 ? O11 M2A O21 70.9(3) 4_656 3_666 ? O11 M2A O21 84.3(3) . 3_666 ? O21 M2A O21 149.2(5) 2_464 3_666 ? O11 M2A O32 132.0(3) 4_656 3_666 ? O11 M2A O32 120.7(3) . 3_666 ? O21 M2A O32 142.9(3) 2_464 3_666 ? O21 M2A O32 66.1(3) 3_666 3_666 ? O11 M2A O32 120.7(3) 4_656 2_464 ? O11 M2A O32 132.0(3) . 2_464 ? O21 M2A O32 66.1(3) 2_464 2_464 ? O21 M2A O32 142.9(3) 3_666 2_464 ? O32 M2A O32 85.1(4) 3_666 2_464 ? O11 M2A O31 161.1(3) 4_656 3_665 ? O11 M2A O31 88.7(2) . 3_665 ? O21 M2A O31 83.9(3) 2_464 3_665 ? O21 M2A O31 114.4(3) 3_666 3_665 ? O32 M2A O31 62.8(2) 3_666 3_665 ? O32 M2A O31 66.9(3) 2_464 3_665 ? O11 M2A O31 88.7(2) 4_656 2_465 ? O11 M2A O31 161.1(3) . 2_465 ? O21 M2A O31 114.4(3) 2_464 2_465 ? O21 M2A O31 83.9(3) 3_666 2_465 ? O32 M2A O31 66.9(3) 3_666 2_465 ? O32 M2A O31 62.8(2) 2_464 2_465 ? O31 M2A O31 109.6(4) 3_665 2_465 ? O11 M2A Si1B 101.2(2) 4_656 3_666 ? O11 M2A Si1B 104.1(2) . 3_666 ? O21 M2A Si1B 171.3(2) 2_464 3_666 ? O21 M2A Si1B 32.5(2) 3_666 3_666 ? O32 M2A Si1B 33.5(2) 3_666 3_666 ? O32 M2A Si1B 115.5(3) 2_464 3_666 ? O31 M2A Si1B 89.0(2) 3_665 3_666 ? O31 M2A Si1B 72.7(2) 2_465 3_666 ? O11 M2A Si1A 101.2(2) 4_656 3_666 ? O11 M2A Si1A 104.1(2) . 3_666 ? O21 M2A Si1A 171.3(2) 2_464 3_666 ? O21 M2A Si1A 32.5(2) 3_666 3_666 ? O32 M2A Si1A 33.5(2) 3_666 3_666 ? O32 M2A Si1A 115.5(3) 2_464 3_666 ? O31 M2A Si1A 89.0(2) 3_665 3_666 ? O31 M2A Si1A 72.7(2) 2_465 3_666 ? Si1B M2A Si1A 0.00(9) 3_666 3_666 ? O11 M2A Si1B 104.1(2) 4_656 2_464 ? O11 M2A Si1B 101.2(2) . 2_464 ? O21 M2A Si1B 32.5(2) 2_464 2_464 ? O21 M2A Si1B 171.3(2) 3_666 2_464 ? O32 M2A Si1B 115.5(3) 3_666 2_464 ? O32 M2A Si1B 33.5(2) 2_464 2_464 ? O31 M2A Si1B 72.7(2) 3_665 2_464 ? O31 M2A Si1B 89.0(2) 2_465 2_464 ? Si1B M2A Si1B 148.3(3) 3_666 2_464 ? Si1A M2A Si1B 148.3(3) 3_666 2_464 ? O11 M2A Si1A 104.1(2) 4_656 2_464 ? O11 M2A Si1A 101.2(2) . 2_464 ? O21 M2A Si1A 32.5(2) 2_464 2_464 ? O21 M2A Si1A 171.3(2) 3_666 2_464 ? O32 M2A Si1A 115.5(3) 3_666 2_464 ? O32 M2A Si1A 33.5(2) 2_464 2_464 ? O31 M2A Si1A 72.7(2) 3_665 2_464 ? O31 M2A Si1A 89.0(2) 2_465 2_464 ? Si1B M2A Si1A 148.3(3) 3_666 2_464 ? Si1A M2A Si1A 148.3(3) 3_666 2_464 ? Si1B M2A Si1A 0.0(2) 2_464 2_464 ? O22 M21A O22 154.3(5) 3_677 2_474 ? O22 M21A O12 81.3(3) 3_677 1_565 ? O22 M21A O12 77.3(3) 2_474 1_565 ? O22 M21A O12 77.3(3) 3_677 4_667 ? O22 M21A O12 81.3(3) 2_474 4_667 ? O12 M21A O12 66.5(4) 1_565 4_667 ? O22 M21A O31 139.7(3) 3_677 2_465 ? O22 M21A O31 64.9(3) 2_474 2_465 ? O12 M21A O31 137.4(3) 1_565 2_465 ? O12 M21A O31 122.5(3) 4_667 2_465 ? O22 M21A O31 64.9(3) 3_677 3_666 ? O22 M21A O31 139.7(3) 2_474 3_666 ? O12 M21A O31 122.5(3) 1_565 3_666 ? O12 M21A O31 137.4(3) 4_667 3_666 ? O31 M21A O31 80.8(4) 2_465 3_666 ? O22 M21A O32 85.2(3) 3_677 2_465 ? O22 M21A O32 110.3(3) 2_474 2_465 ? O12 M21A O32 158.1(3) 1_565 2_465 ? O12 M21A O32 93.7(3) 4_667 2_465 ? O31 M21A O32 60.7(2) 2_465 2_465 ? O31 M21A O32 65.5(3) 3_666 2_465 ? O22 M21A O32 110.3(3) 3_677 3_666 ? O22 M21A O32 85.2(3) 2_474 3_666 ? O12 M21A O32 93.7(3) 1_565 3_666 ? O12 M21A O32 158.1(3) 4_667 3_666 ? O31 M21A O32 65.5(3) 2_465 3_666 ? O31 M21A O32 60.7(2) 3_666 3_666 ? O32 M21A O32 107.2(4) 2_465 3_666 ? O22 M21A SI2B 171.2(2) 3_677 2_464 ? O22 M21A SI2B 31.6(2) 2_474 2_464 ? O12 M21A SI2B 106.9(2) 1_565 2_464 ? O12 M21A SI2B 102.9(2) 4_667 2_464 ? O31 M21A SI2B 33.3(2) 2_465 2_464 ? O31 M21A SI2B 111.6(2) 3_666 2_464 ? O32 M21A SI2B 86.0(2) 2_465 2_464 ? O32 M21A SI2B 72.9(2) 3_666 2_464 ? O22 M21A Si2A 171.2(2) 3_677 2_464 ? O22 M21A Si2A 31.6(2) 2_474 2_464 ? O12 M21A Si2A 106.9(2) 1_565 2_464 ? O12 M21A Si2A 102.9(2) 4_667 2_464 ? O31 M21A Si2A 33.3(2) 2_465 2_464 ? O31 M21A Si2A 111.6(2) 3_666 2_464 ? O32 M21A Si2A 86.0(2) 2_465 2_464 ? O32 M21A Si2A 72.9(2) 3_666 2_464 ? SI2B M21A Si2A 0.0(2) 2_464 2_464 ? O22 M21A SI2B 31.6(2) 3_677 3_667 ? O22 M21A SI2B 171.2(2) 2_474 3_667 ? O12 M21A SI2B 102.9(2) 1_565 3_667 ? O12 M21A SI2B 106.9(2) 4_667 3_667 ? O31 M21A SI2B 111.6(2) 2_465 3_667 ? O31 M21A SI2B 33.3(2) 3_666 3_667 ? O32 M21A SI2B 72.9(2) 2_465 3_667 ? O32 M21A SI2B 86.0(2) 3_666 3_667 ? SI2B M21A SI2B 144.2(2) 2_464 3_667 ? Si2A M21A SI2B 144.2(2) 2_464 3_667 ? O22 M21A Si2A 31.6(2) 3_677 3_667 ? O22 M21A Si2A 171.2(2) 2_474 3_667 ? O12 M21A Si2A 102.9(2) 1_565 3_667 ? O12 M21A Si2A 106.9(2) 4_667 3_667 ? O31 M21A Si2A 111.6(2) 2_465 3_667 ? O31 M21A Si2A 33.3(2) 3_666 3_667 ? O32 M21A Si2A 72.9(2) 2_465 3_667 ? O32 M21A Si2A 86.0(2) 3_666 3_667 ? SI2B M21A Si2A 144.2(2) 2_464 3_667 ? Si2A M21A Si2A 144.2(2) 2_464 3_667 ? SI2B M21A Si2A 0.00(16) 3_667 3_667 ? _diffrn_measured_fraction_theta_max 0.431 _diffrn_reflns_theta_full 29.85 _diffrn_measured_fraction_theta_full 0.431 _refine_diff_density_max 0.968 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.211