data_publication_text _publ_requested_journal Am.Miner. _publ_contact_author_name 'Pandolfo Francesco' _publ_contact_author_email francesco.pandolfo@unipv.it loop_ _publ_author_name _publ_author_address 'Pandolfo , Francesco' 'via Ferrata 1, Pavia (PV) I-27100' data_omp4p0 _publ_requested_journal Am.Miner. loop_ _publ_author_name _publ_author_address 'Pandolfo, F.' '' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al Ca Cr Fe Fe Mg Mn Na O O Si Si Si Ti' _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 ? _symmetry_space_group_name_H-M ? 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 9.5685(11) _cell_length_b 8.7608(15) _cell_length_c 5.2561(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.995(10) _cell_angle_gamma 90.00 _cell_volume 421.37(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 211 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_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 1569 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 29.36 _reflns_number_total 534 _reflns_number_gt 315 _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^)+(0.0871P)^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 0.002(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 534 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2147 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.000 _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 0.3626(8) 0.3358(8) 0.1183(11) 0.0108(18) Uiso 1 1 d . . . O12 O 0.3623(8) 0.1769(8) 0.6493(11) 0.0104(17) Uiso 1 1 d . . . O21 O 0.6168(9) 0.5109(8) 0.3098(11) 0.0131(18) Uiso 1 1 d . . . O22 O 0.6050(9) 0.9984(8) 0.8043(11) 0.0108(17) Uiso 1 1 d . . . O31 O 0.6069(8) 0.2662(8) 0.0041(10) 0.0089(16) Uiso 1 1 d . . . O32 O 0.5970(8) 0.2387(8) 0.4976(10) 0.0111(17) Uiso 1 1 d . . . Si1A Si 0.5390(4) 0.3485(3) 0.2261(5) 0.0099(8) Uiso 0.50 1 d P . . Si1B Si+4 0.5390(4) 0.3485(3) 0.2261(5) 0.0099(8) Uiso 0.50 1 d P . . Si2A Si+2 0.5369(3) 0.1632(3) 0.7307(5) 0.0086(8) Uiso 0.96 1 d P . . SI2B Al+3 0.5369(3) 0.1632(3) 0.7307(5) 0.0086(8) Uiso 0.04 1 d P . . M1A Mg+2 0.2500 0.1592(5) 0.2500 0.0121(12) Uiso 0.84 2 d SP . . M1B Fe+2 0.2500 0.1592(5) 0.2500 0.0121(12) Uiso 0.09 2 d SP . . M1C Al+3 0.2500 0.1592(5) 0.2500 0.0121(12) Uiso 0.07 2 d SP . . M1D Mn+2 0.2500 0.1592(5) 0.2500 0.0121(12) Uiso 0.00 2 d SP . . M11A Mg+2 0.2500 0.3481(5) 0.7500 0.0075(10) Uiso 0.02 2 d SP . . M11B Fe+2 0.2500 0.3481(5) 0.7500 0.0075(10) Uiso 0.02 2 d SP . . M11C Al+3 0.2500 0.3481(5) 0.7500 0.0075(10) Uiso 0.96 2 d SP . . M11D Ti+4 0.2500 0.3481(5) 0.7500 0.0075(10) Uiso 0.01 2 d SP . . M11E Cr+3 0.2500 0.3481(5) 0.7500 0.0075(10) Uiso 0.00 2 d SP . . M2A Ca+2 0.2500 0.5521(6) 0.2500 0.0157(12) Uiso 0.25 2 d SP . . M2B Na+1 0.2500 0.5521(6) 0.2500 0.0157(12) Uiso 0.74 2 d SP . . M2C Fe+2 0.2500 0.5521(6) 0.2500 0.0157(12) Uiso 0.01 2 d SP . . M21A Ca+2 0.2500 0.9502(4) 0.7500 0.0131(10) Uiso 0.71 2 d SP . . M21B Na+1 0.2500 0.9502(4) 0.7500 0.0131(10) Uiso 0.23 2 d SP . . M21C Mg+2 0.2500 0.9502(4) 0.7500 0.0131(10) 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 1.620(8) . ? O11 M11E 1.924(6) 1_554 ? O11 M11D 1.924(6) 1_554 ? O11 M11B 1.924(6) 1_554 ? O11 M11A 1.924(6) 1_554 ? O11 M1A 2.114(7) . ? O11 M2A 2.380(7) . ? O12 Si2A 1.603(7) . ? O12 M11A 2.004(8) . ? O12 M1A 2.065(6) . ? O12 M21C 2.390(7) 1_545 ? O12 M21A 2.390(7) 1_545 ? O21 Si1A 1.607(7) . ? O21 M11E 1.866(7) 3_666 ? O21 M11A 1.866(7) 3_666 ? O21 M11B 1.866(7) 3_666 ? O21 M11D 1.866(7) 3_666 ? O21 M2C 2.358(7) 3_666 ? O21 M2A 2.358(7) 3_666 ? O21 O22 5.018(10) . ? O22 SI2B 1.585(7) 1_565 ? O22 Si2A 1.585(7) 1_565 ? O22 M1D 2.036(7) 3_666 ? O22 M1A 2.036(7) 3_666 ? O22 M21C 2.391(7) 3_677 ? O22 M21A 2.391(7) 3_677 ? O22 O21 5.014(10) 1_556 ? O31 Si1A 1.657(6) . ? O31 SI2B 1.663(6) 1_554 ? O31 Si2A 1.663(6) 1_554 ? O31 M21C 2.471(7) 3_666 ? O31 M21A 2.471(7) 3_666 ? O31 O32 2.634(7) . ? O31 M2A 2.694(7) 3_665 ? O32 O32 0.026(11) ? ? O32 Si2A 1.638(6) . ? O32 Si1A 1.675(6) . ? O32 M2A 2.475(8) 3_666 ? O32 O31 2.605(8) ? ? O32 M21A 2.773(7) 3_666 ? Si1A O32 1.694(6) ? ? Si1A M2A 3.028(3) 3_666 ? Si1A M11E 3.141(3) 1_554 ? Si1A M11D 3.141(3) 1_554 ? Si1A M11A 3.141(3) 1_554 ? Si1A M1A 3.258(4) . ? Si1A M21A 3.285(5) 3_666 ? Si2A O22 1.585(7) 1_545 ? Si2A O32 1.616(8) ? ? Si2A O31 1.631(6) ? ? Si2A M21C 3.057(3) 3_667 ? Si2A M21A 3.057(3) 3_667 ? Si2A M1A 3.141(3) . ? Si2A M2A 3.204(5) 3_666 ? Si2A M11A 3.214(4) . ? M1A O22 2.036(7) 2_464 ? M1A O22 2.036(7) 3_666 ? M1A O12 2.065(6) 4_656 ? M1A O11 2.114(7) 4_656 ? M1A M11A 3.105(3) . ? M1A M11E 3.105(3) 1_554 ? M1A M11D 3.105(3) 1_554 ? M11A O21 1.866(7) 3_666 ? M11A O21 1.866(7) 2_465 ? M11A O11 1.924(6) 4_656 ? M11A O11 1.924(6) 1_556 ? M11A O12 2.004(8) 4_657 ? M11A M1D 3.105(3) 1_556 ? M11A M1A 3.105(3) 1_556 ? M11A Si1B 3.141(3) 1_556 ? M11A Si1A 3.141(3) 1_556 ? M2A O21 2.358(7) 2_464 ? M2A O21 2.358(7) 3_666 ? M2A O11 2.380(7) 4_656 ? M2A O32 2.475(8) 3_666 ? M2A O32 2.475(8) 2_464 ? M2A O31 2.694(7) 3_665 ? M2A O31 2.694(7) 2_465 ? M2A Si1B 3.028(3) 3_666 ? M2A Si1A 3.028(3) 3_666 ? M2A Si1B 3.028(3) 2_464 ? M2A Si1A 3.028(3) 2_464 ? M21A O12 2.390(7) 1_565 ? M21A O12 2.390(7) 4_667 ? M21A O22 2.391(7) 3_677 ? M21A O22 2.391(7) 2_474 ? M21A O31 2.471(7) 2_465 ? M21A O31 2.471(7) 3_666 ? M21A O32 2.773(7) 2_465 ? M21A O32 2.773(7) 3_666 ? M21A SI2B 3.057(3) 2_464 ? M21A Si2A 3.057(3) 2_464 ? M21A SI2B 3.057(3) 3_667 ? M21A Si2A 3.057(3) 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 124.6(3) . 1_554 ? Si1A O11 M11D 124.6(3) . 1_554 ? M11E O11 M11D 0.0(3) 1_554 1_554 ? Si1A O11 M11B 124.6(3) . 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 124.6(3) . 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 120.9(4) . . ? M11E O11 M1A 100.4(3) 1_554 . ? M11D O11 M1A 100.4(3) 1_554 . ? M11B O11 M1A 100.4(3) 1_554 . ? M11A O11 M1A 100.4(3) 1_554 . ? Si1A O11 M2A 111.0(4) . . ? M11E O11 M2A 94.6(3) 1_554 . ? M11D O11 M2A 94.6(3) 1_554 . ? M11B O11 M2A 94.6(3) 1_554 . ? M11A O11 M2A 94.6(3) 1_554 . ? M1A O11 M2A 99.8(3) . . ? Si2A O12 M11A 125.7(4) . . ? Si2A O12 M1A 117.2(3) . . ? M11A O12 M1A 99.5(3) . . ? Si2A O12 M21C 112.3(4) . 1_545 ? M11A O12 M21C 104.6(3) . 1_545 ? M1A O12 M21C 91.6(3) . 1_545 ? Si2A O12 M21A 112.3(4) . 1_545 ? M11A O12 M21A 104.6(3) . 1_545 ? M1A O12 M21A 91.6(3) . 1_545 ? M21C O12 M21A 0.00(10) 1_545 1_545 ? Si1A O21 M11E 145.6(4) . 3_666 ? Si1A O21 M11A 145.6(4) . 3_666 ? M11E O21 M11A 0.00(19) 3_666 3_666 ? Si1A O21 M11B 145.6(4) . 3_666 ? M11E O21 M11B 0.00(19) 3_666 3_666 ? M11A O21 M11B 0.00(19) 3_666 3_666 ? Si1A O21 M11D 145.6(4) . 3_666 ? M11E O21 M11D 0.00(19) 3_666 3_666 ? M11A O21 M11D 0.00(19) 3_666 3_666 ? M11B O21 M11D 0.00(19) 3_666 3_666 ? Si1A O21 M2C 97.8(3) . 3_666 ? M11E O21 M2C 96.9(3) 3_666 3_666 ? M11A O21 M2C 96.9(3) 3_666 3_666 ? M11B O21 M2C 96.9(3) 3_666 3_666 ? M11D O21 M2C 96.9(3) 3_666 3_666 ? Si1A O21 M2A 97.8(3) . 3_666 ? M11E O21 M2A 96.9(3) 3_666 3_666 ? M11A O21 M2A 96.9(3) 3_666 3_666 ? M11B O21 M2A 96.9(3) 3_666 3_666 ? M11D O21 M2A 96.9(3) 3_666 3_666 ? M2C O21 M2A 0.0(2) 3_666 3_666 ? Si1A O21 O22 144.8(3) . . ? M11E O21 O22 69.1(2) 3_666 . ? M11A O21 O22 69.1(2) 3_666 . ? M11B O21 O22 69.1(2) 3_666 . ? M11D O21 O22 69.1(2) 3_666 . ? M2C O21 O22 77.2(2) 3_666 . ? M2A O21 O22 77.2(2) 3_666 . ? SI2B O22 Si2A 0.0(2) 1_565 1_565 ? SI2B O22 M1D 146.4(4) 1_565 3_666 ? Si2A O22 M1D 146.4(4) 1_565 3_666 ? SI2B O22 M1A 146.4(4) 1_565 3_666 ? Si2A O22 M1A 146.4(4) 1_565 3_666 ? M1D O22 M1A 0.00(18) 3_666 3_666 ? SI2B O22 M21C 98.5(3) 1_565 3_677 ? Si2A O22 M21C 98.5(3) 1_565 3_677 ? M1D O22 M21C 92.4(3) 3_666 3_677 ? M1A O22 M21C 92.4(3) 3_666 3_677 ? SI2B O22 M21A 98.5(3) 1_565 3_677 ? Si2A O22 M21A 98.5(3) 1_565 3_677 ? M1D O22 M21A 92.4(3) 3_666 3_677 ? M1A O22 M21A 92.4(3) 3_666 3_677 ? M21C O22 M21A 0.0 3_677 3_677 ? SI2B O22 O21 148.1(3) 1_565 1_556 ? Si2A O22 O21 148.1(3) 1_565 1_556 ? M1D O22 O21 65.5(2) 3_666 1_556 ? M1A O22 O21 65.5(2) 3_666 1_556 ? M21C O22 O21 73.99(18) 3_677 1_556 ? M21A O22 O21 73.99(18) 3_677 1_556 ? SI2B O22 O21 136.0(3) 1_565 . ? Si2A O22 O21 136.0(3) 1_565 . ? M1D O22 O21 39.70(18) 3_666 . ? M1A O22 O21 39.70(18) 3_666 . ? M21C O22 O21 125.0(3) 3_677 . ? M21A O22 O21 125.0(3) 3_677 . ? O21 O22 O21 63.19(13) 1_556 . ? Si1A O31 SI2B 134.6(5) . 1_554 ? Si1A O31 Si2A 134.6(5) . 1_554 ? SI2B O31 Si2A 0.0(3) 1_554 1_554 ? Si1A O31 M21C 103.7(3) . 3_666 ? SI2B O31 M21C 93.3(3) 1_554 3_666 ? Si2A O31 M21C 93.3(3) 1_554 3_666 ? Si1A O31 M21A 103.7(3) . 3_666 ? SI2B O31 M21A 93.3(3) 1_554 3_666 ? Si2A O31 M21A 93.3(3) 1_554 3_666 ? M21C O31 M21A 0.00(11) 3_666 3_666 ? Si1A O31 O32 38.0(2) . . ? SI2B O31 O32 132.8(4) 1_554 . ? Si2A O31 O32 132.8(4) 1_554 . ? M21C O31 O32 65.7(2) 3_666 . ? M21A O31 O32 65.7(2) 3_666 . ? Si1A O31 M2A 116.9(3) . 3_665 ? SI2B O31 M2A 91.5(2) 1_554 3_665 ? Si2A O31 M2A 91.5(2) 1_554 3_665 ? M21C O31 M2A 115.4(3) 3_666 3_665 ? M21A O31 M2A 115.4(3) 3_666 3_665 ? O32 O31 M2A 135.4(3) . 3_665 ? O32 O32 Si2A 31.7(4) ? . ? O32 O32 Si1A 139.0(2) ? . ? Si2A O32 Si1A 140.1(5) . . ? O32 O32 M2A 68.70(12) ? 3_666 ? Si2A O32 M2A 100.4(3) . 3_666 ? Si1A O32 M2A 91.6(3) . 3_666 ? O32 O32 O31 5.7(3) ? ? ? Si2A O32 O31 37.1(2) . ? ? Si1A O32 O31 135.1(4) . ? ? M2A O32 O31 63.3(2) 3_666 ? ? O32 O32 O31 174.4(2) ? . ? Si2A O32 O31 153.5(4) . . ? Si1A O32 O31 37.5(2) . . ? M2A O32 O31 105.9(3) 3_666 . ? O31 O32 O31 168.7(4) ? . ? O32 O32 M21A 128.58(12) ? 3_666 ? Si2A O32 M21A 117.3(4) . 3_666 ? Si1A O32 M21A 91.8(2) . 3_666 ? M2A O32 M21A 112.5(3) 3_666 3_666 ? O31 O32 M21A 131.2(3) ? 3_666 ? O31 O32 M21A 54.32(19) . 3_666 ? O21 Si1A O11 120.6(4) . . ? O21 Si1A O31 109.4(4) . . ? O11 Si1A O31 107.9(4) . . ? O21 Si1A O32 105.3(4) . . ? O11 Si1A O32 108.1(4) . . ? O31 Si1A O32 104.5(3) . . ? O21 Si1A O32 105.0(4) . ? ? O11 Si1A O32 108.0(4) . ? ? O31 Si1A O32 105.0(4) . ? ? O32 Si1A O32 0.6(2) . ? ? O21 Si1A M2A 50.5(3) . 3_666 ? O11 Si1A M2A 133.4(2) . 3_666 ? O31 Si1A M2A 118.1(3) . 3_666 ? O32 Si1A M2A 54.8(3) . 3_666 ? O32 Si1A M2A 54.5(2) ? 3_666 ? O21 Si1A M11E 116.7(3) . 1_554 ? O11 Si1A M11E 30.3(2) . 1_554 ? O31 Si1A M11E 82.7(3) . 1_554 ? O32 Si1A M11E 132.4(3) . 1_554 ? O32 Si1A M11E 132.4(3) ? 1_554 ? M2A Si1A M11E 157.34(14) 3_666 1_554 ? O21 Si1A M11D 116.7(3) . 1_554 ? O11 Si1A M11D 30.3(2) . 1_554 ? O31 Si1A M11D 82.7(3) . 1_554 ? O32 Si1A M11D 132.4(3) . 1_554 ? O32 Si1A M11D 132.4(3) ? 1_554 ? M2A Si1A M11D 157.34(14) 3_666 1_554 ? M11E Si1A M11D 0.0 1_554 1_554 ? O21 Si1A M11A 116.7(3) . 1_554 ? O11 Si1A M11A 30.3(2) . 1_554 ? O31 Si1A M11A 82.7(3) . 1_554 ? O32 Si1A M11A 132.4(3) . 1_554 ? O32 Si1A M11A 132.4(3) ? 1_554 ? M2A Si1A M11A 157.34(14) 3_666 1_554 ? M11E Si1A M11A 0.0 1_554 1_554 ? M11D Si1A M11A 0.0 1_554 1_554 ? O21 Si1A M1A 140.4(3) . . ? O11 Si1A M1A 33.8(2) . . ? O31 Si1A M1A 108.5(3) . . ? O32 Si1A M1A 75.5(3) . . ? O32 Si1A M1A 75.4(3) ? . ? M2A Si1A M1A 117.34(9) 3_666 . ? M11E Si1A M1A 58.04(8) 1_554 . ? M11D Si1A M1A 58.04(8) 1_554 . ? M11A Si1A M1A 58.04(8) 1_554 . ? O21 Si1A M21A 117.7(3) . 3_666 ? O11 Si1A M21A 121.7(3) . 3_666 ? O31 Si1A M21A 47.0(2) . 3_666 ? O32 Si1A M21A 57.5(2) . 3_666 ? O32 Si1A M21A 58.1(3) ? 3_666 ? M2A Si1A M21A 87.43(11) 3_666 3_666 ? M11E Si1A M21A 114.69(12) 1_554 3_666 ? M11D Si1A M21A 114.69(12) 1_554 3_666 ? M11A Si1A M21A 114.69(12) 1_554 3_666 ? M1A Si1A M21A 96.45(11) . 3_666 ? O22 Si2A O12 117.1(4) 1_545 . ? O22 Si2A O32 110.1(4) 1_545 ? ? O12 Si2A O32 109.9(3) . ? ? O22 Si2A O31 105.0(4) 1_545 ? ? O12 Si2A O31 108.8(4) . ? ? O32 Si2A O31 105.2(4) ? ? ? O22 Si2A O32 109.9(4) 1_545 . ? O12 Si2A O32 109.7(4) . . ? O32 Si2A O32 0.5(2) ? . ? O31 Si2A O32 105.6(4) ? . ? O22 Si2A M21C 50.7(3) 1_545 3_667 ? O12 Si2A M21C 129.3(2) . 3_667 ? O32 Si2A M21C 120.4(3) ? 3_667 ? O31 Si2A M21C 54.3(2) ? 3_667 ? O32 Si2A M21C 120.7(3) . 3_667 ? O22 Si2A M21A 50.7(3) 1_545 3_667 ? O12 Si2A M21A 129.3(2) . 3_667 ? O32 Si2A M21A 120.4(3) ? 3_667 ? O31 Si2A M21A 54.3(2) ? 3_667 ? O32 Si2A M21A 120.7(3) . 3_667 ? M21C Si2A M21A 0.00(13) 3_667 3_667 ? O22 Si2A M1A 112.8(3) 1_545 . ? O12 Si2A M1A 35.8(2) . . ? O32 Si2A M1A 79.9(2) ? . ? O31 Si2A M1A 137.5(3) ? . ? O32 Si2A M1A 79.5(3) . . ? M21C Si2A M1A 155.90(14) 3_667 . ? M21A Si2A M1A 155.90(14) 3_667 . ? O22 Si2A M2A 119.2(3) 1_545 3_666 ? O12 Si2A M2A 123.6(3) . 3_666 ? O32 Si2A M2A 49.0(2) ? 3_666 ? O31 Si2A M2A 56.2(3) ? 3_666 ? O32 Si2A M2A 49.4(2) . 3_666 ? M21C Si2A M2A 88.42(10) 3_667 3_666 ? M21A Si2A M2A 88.42(10) 3_667 3_666 ? M1A Si2A M2A 115.63(12) . 3_666 ? O22 Si2A M11A 138.2(3) 1_545 . ? O12 Si2A M11A 30.4(3) . . ? O32 Si2A M11A 108.1(3) ? . ? O31 Si2A M11A 80.5(3) ? . ? O32 Si2A M11A 108.1(3) . . ? M21C Si2A M11A 119.25(8) 3_667 . ? M21A Si2A M11A 119.25(8) 3_667 . ? M1A Si2A M11A 58.49(8) . . ? M2A Si2A M11A 98.53(12) 3_666 . ? O22 M1A O22 94.6(4) 2_464 3_666 ? O22 M1A O12 91.1(3) 2_464 4_656 ? O22 M1A O12 94.7(3) 3_666 4_656 ? O22 M1A O12 94.7(3) 2_464 . ? O22 M1A O12 91.1(3) 3_666 . ? O12 M1A O12 171.4(5) 4_656 . ? O22 M1A O11 167.3(3) 2_464 . ? O22 M1A O11 91.0(3) 3_666 . ? O12 M1A O11 77.0(3) 4_656 . ? O12 M1A O11 96.6(3) . . ? O22 M1A O11 91.0(3) 2_464 4_656 ? O22 M1A O11 167.3(3) 3_666 4_656 ? O12 M1A O11 96.6(3) 4_656 4_656 ? O12 M1A O11 77.0(3) . 4_656 ? O11 M1A O11 85.9(4) . 4_656 ? O22 M1A M11A 94.26(16) 2_464 . ? O22 M1A M11A 130.43(18) 3_666 . ? O12 M1A M11A 133.7(2) 4_656 . ? O12 M1A M11A 39.5(2) . . ? O11 M1A M11A 90.8(2) . . ? O11 M1A M11A 37.53(18) 4_656 . ? O22 M1A M11E 130.43(18) 2_464 1_554 ? O22 M1A M11E 94.26(16) 3_666 1_554 ? O12 M1A M11E 39.5(2) 4_656 1_554 ? O12 M1A M11E 133.7(2) . 1_554 ? O11 M1A M11E 37.53(18) . 1_554 ? O11 M1A M11E 90.8(2) 4_656 1_554 ? M11A M1A M11E 115.61(18) . 1_554 ? O22 M1A M11D 130.43(18) 2_464 1_554 ? O22 M1A M11D 94.26(16) 3_666 1_554 ? O12 M1A M11D 39.5(2) 4_656 1_554 ? O12 M1A M11D 133.7(2) . 1_554 ? O11 M1A M11D 37.53(18) . 1_554 ? O11 M1A M11D 90.8(2) 4_656 1_554 ? M11A M1A M11D 115.61(18) . 1_554 ? M11E M1A M11D 0.00(13) 1_554 1_554 ? O21 M11A O21 97.1(5) 3_666 2_465 ? O21 M11A O11 94.4(3) 3_666 4_656 ? O21 M11A O11 89.9(3) 2_465 4_656 ? O21 M11A O11 89.9(3) 3_666 1_556 ? O21 M11A O11 94.4(3) 2_465 1_556 ? O11 M11A O11 173.6(5) 4_656 1_556 ? O21 M11A O12 170.1(3) 3_666 4_657 ? O21 M11A O12 90.3(3) 2_465 4_657 ? O11 M11A O12 92.2(3) 4_656 4_657 ? O11 M11A O12 83.0(3) 1_556 4_657 ? O21 M11A O12 90.3(3) 3_666 . ? O21 M11A O12 170.1(3) 2_465 . ? O11 M11A O12 83.0(3) 4_656 . ? O11 M11A O12 92.2(3) 1_556 . ? O12 M11A O12 83.1(4) 4_657 . ? O21 M11A M1A 92.36(19) 3_666 . ? O21 M11A M1A 131.6(2) 2_465 . ? O11 M11A M1A 42.0(2) 4_656 . ? O11 M11A M1A 133.1(3) 1_556 . ? O12 M11A M1A 87.6(2) 4_657 . ? O12 M11A M1A 40.99(18) . . ? O21 M11A M1D 131.6(2) 3_666 1_556 ? O21 M11A M1D 92.36(19) 2_465 1_556 ? O11 M11A M1D 133.1(3) 4_656 1_556 ? O11 M11A M1D 42.0(2) 1_556 1_556 ? O12 M11A M1D 40.99(18) 4_657 1_556 ? O12 M11A M1D 87.6(2) . 1_556 ? M1A M11A M1D 115.61(18) . 1_556 ? O21 M11A M1A 131.6(2) 3_666 1_556 ? O21 M11A M1A 92.36(19) 2_465 1_556 ? O11 M11A M1A 133.1(3) 4_656 1_556 ? O11 M11A M1A 42.0(2) 1_556 1_556 ? O12 M11A M1A 40.99(18) 4_657 1_556 ? O12 M11A M1A 87.6(2) . 1_556 ? M1A M11A M1A 115.61(18) . 1_556 ? M1D M11A M1A 0.00(14) 1_556 1_556 ? O21 M11A Si1B 69.4(2) 3_666 1_556 ? O21 M11A Si1B 110.5(2) 2_465 1_556 ? O11 M11A Si1B 154.9(2) 4_656 1_556 ? O11 M11A Si1B 25.1(2) 1_556 1_556 ? O12 M11A Si1B 101.9(2) 4_657 1_556 ? O12 M11A Si1B 78.2(2) . 1_556 ? M1A M11A Si1B 117.20(9) . 1_556 ? M1D M11A Si1B 62.87(6) 1_556 1_556 ? M1A M11A Si1B 62.87(6) 1_556 1_556 ? O21 M11A Si1A 69.4(2) 3_666 1_556 ? O21 M11A Si1A 110.5(2) 2_465 1_556 ? O11 M11A Si1A 154.9(2) 4_656 1_556 ? O11 M11A Si1A 25.1(2) 1_556 1_556 ? O12 M11A Si1A 101.9(2) 4_657 1_556 ? O12 M11A Si1A 78.2(2) . 1_556 ? M1A M11A Si1A 117.20(9) . 1_556 ? M1D M11A Si1A 62.87(6) 1_556 1_556 ? M1A M11A Si1A 62.87(6) 1_556 1_556 ? Si1B M11A Si1A 0.0 1_556 1_556 ? O21 M2A O21 152.9(4) 2_464 3_666 ? O21 M2A O11 86.5(3) 2_464 4_656 ? O21 M2A O11 71.9(2) 3_666 4_656 ? O21 M2A O11 71.9(2) 2_464 . ? O21 M2A O11 86.5(3) 3_666 . ? O11 M2A O11 74.5(3) 4_656 . ? O21 M2A O32 139.9(3) 2_464 3_666 ? O21 M2A O32 65.3(2) 3_666 3_666 ? O11 M2A O32 132.88(19) 4_656 3_666 ? O11 M2A O32 119.9(2) . 3_666 ? O21 M2A O32 65.3(2) 2_464 2_464 ? O21 M2A O32 139.9(3) 3_666 2_464 ? O11 M2A O32 119.9(2) 4_656 2_464 ? O11 M2A O32 132.88(19) . 2_464 ? O32 M2A O32 84.5(4) 3_666 2_464 ? O21 M2A O31 81.9(2) 2_464 3_665 ? O21 M2A O31 114.7(2) 3_666 3_665 ? O11 M2A O31 162.4(2) 4_656 3_665 ? O11 M2A O31 89.3(2) . 3_665 ? O32 M2A O31 61.44(19) 3_666 3_665 ? O32 M2A O31 66.7(2) 2_464 3_665 ? O21 M2A O31 114.7(2) 2_464 2_465 ? O21 M2A O31 81.9(2) 3_666 2_465 ? O11 M2A O31 89.3(2) 4_656 2_465 ? O11 M2A O31 162.4(2) . 2_465 ? O32 M2A O31 66.7(2) 3_666 2_465 ? O32 M2A O31 61.44(19) 2_464 2_465 ? O31 M2A O31 107.6(3) 3_665 2_465 ? O21 M2A Si1B 170.2(2) 2_464 3_666 ? O21 M2A Si1B 31.72(17) 3_666 3_666 ? O11 M2A Si1B 101.69(17) 4_656 3_666 ? O11 M2A Si1B 104.78(18) . 3_666 ? O32 M2A Si1B 33.57(15) 3_666 3_666 ? O32 M2A Si1B 114.0(2) 2_464 3_666 ? O31 M2A Si1B 88.88(16) 3_665 3_666 ? O31 M2A Si1B 71.33(16) 2_465 3_666 ? O21 M2A Si1A 170.2(2) 2_464 3_666 ? O21 M2A Si1A 31.72(17) 3_666 3_666 ? O11 M2A Si1A 101.69(17) 4_656 3_666 ? O11 M2A Si1A 104.78(18) . 3_666 ? O32 M2A Si1A 33.57(15) 3_666 3_666 ? O32 M2A Si1A 114.0(2) 2_464 3_666 ? O31 M2A Si1A 88.88(16) 3_665 3_666 ? O31 M2A Si1A 71.33(16) 2_465 3_666 ? Si1B M2A Si1A 0.00(7) 3_666 3_666 ? O21 M2A Si1B 31.72(17) 2_464 2_464 ? O21 M2A Si1B 170.2(2) 3_666 2_464 ? O11 M2A Si1B 104.78(18) 4_656 2_464 ? O11 M2A Si1B 101.69(17) . 2_464 ? O32 M2A Si1B 114.0(2) 3_666 2_464 ? O32 M2A Si1B 33.57(15) 2_464 2_464 ? O31 M2A Si1B 71.33(16) 3_665 2_464 ? O31 M2A Si1B 88.88(16) 2_465 2_464 ? Si1B M2A Si1B 146.6(2) 3_666 2_464 ? Si1A M2A Si1B 146.6(2) 3_666 2_464 ? O21 M2A Si1A 31.72(17) 2_464 2_464 ? O21 M2A Si1A 170.2(2) 3_666 2_464 ? O11 M2A Si1A 104.78(18) 4_656 2_464 ? O11 M2A Si1A 101.69(17) . 2_464 ? O32 M2A Si1A 114.0(2) 3_666 2_464 ? O32 M2A Si1A 33.57(15) 2_464 2_464 ? O31 M2A Si1A 71.33(16) 3_665 2_464 ? O31 M2A Si1A 88.88(16) 2_465 2_464 ? Si1B M2A Si1A 146.6(2) 3_666 2_464 ? Si1A M2A Si1A 146.6(2) 3_666 2_464 ? Si1B M2A Si1A 0.00(16) 2_464 2_464 ? O12 M21A O12 67.6(3) 1_565 4_667 ? O12 M21A O22 83.7(2) 1_565 3_677 ? O12 M21A O22 78.2(2) 4_667 3_677 ? O12 M21A O22 78.2(2) 1_565 2_474 ? O12 M21A O22 83.7(2) 4_667 2_474 ? O22 M21A O22 158.3(4) 3_677 2_474 ? O12 M21A O31 137.57(19) 1_565 2_465 ? O12 M21A O31 122.5(2) 4_667 2_465 ? O22 M21A O31 137.0(2) 3_677 2_465 ? O22 M21A O31 63.8(2) 2_474 2_465 ? O12 M21A O31 122.5(2) 1_565 3_666 ? O12 M21A O31 137.57(19) 4_667 3_666 ? O22 M21A O31 63.8(2) 3_677 3_666 ? O22 M21A O31 137.0(2) 2_474 3_666 ? O31 M21A O31 79.8(3) 2_465 3_666 ? O12 M21A O32 158.9(2) 1_565 2_465 ? O12 M21A O32 93.4(2) 4_667 2_465 ? O22 M21A O32 83.5(2) 3_677 2_465 ? O22 M21A O32 109.7(2) 2_474 2_465 ? O31 M21A O32 59.97(18) 2_465 2_465 ? O31 M21A O32 65.4(2) 3_666 2_465 ? O12 M21A O32 93.4(2) 1_565 3_666 ? O12 M21A O32 158.9(2) 4_667 3_666 ? O22 M21A O32 109.7(2) 3_677 3_666 ? O22 M21A O32 83.5(2) 2_474 3_666 ? O31 M21A O32 65.4(2) 2_465 3_666 ? O31 M21A O32 59.97(18) 3_666 3_666 ? O32 M21A O32 106.7(3) 2_465 3_666 ? O12 M21A SI2B 107.35(15) 1_565 2_464 ? O12 M21A SI2B 104.01(17) 4_667 2_464 ? O22 M21A SI2B 168.8(2) 3_677 2_464 ? O22 M21A SI2B 30.86(16) 2_474 2_464 ? O31 M21A SI2B 32.90(15) 2_465 2_464 ? O31 M21A SI2B 109.9(2) 3_666 2_464 ? O32 M21A SI2B 85.36(15) 2_465 2_464 ? O32 M21A SI2B 72.11(15) 3_666 2_464 ? O12 M21A Si2A 107.35(15) 1_565 2_464 ? O12 M21A Si2A 104.01(17) 4_667 2_464 ? O22 M21A Si2A 168.8(2) 3_677 2_464 ? O22 M21A Si2A 30.86(16) 2_474 2_464 ? O31 M21A Si2A 32.90(15) 2_465 2_464 ? O31 M21A Si2A 109.9(2) 3_666 2_464 ? O32 M21A Si2A 85.36(15) 2_465 2_464 ? O32 M21A Si2A 72.11(15) 3_666 2_464 ? SI2B M21A Si2A 0.00(15) 2_464 2_464 ? O12 M21A SI2B 104.01(17) 1_565 3_667 ? O12 M21A SI2B 107.35(15) 4_667 3_667 ? O22 M21A SI2B 30.86(16) 3_677 3_667 ? O22 M21A SI2B 168.8(2) 2_474 3_667 ? O31 M21A SI2B 109.9(2) 2_465 3_667 ? O31 M21A SI2B 32.90(15) 3_666 3_667 ? O32 M21A SI2B 72.11(15) 2_465 3_667 ? O32 M21A SI2B 85.36(15) 3_666 3_667 ? SI2B M21A SI2B 142.05(18) 2_464 3_667 ? Si2A M21A SI2B 142.05(18) 2_464 3_667 ? O12 M21A Si2A 104.01(17) 1_565 3_667 ? O12 M21A Si2A 107.35(15) 4_667 3_667 ? O22 M21A Si2A 30.86(16) 3_677 3_667 ? O22 M21A Si2A 168.8(2) 2_474 3_667 ? O31 M21A Si2A 109.9(2) 2_465 3_667 ? O31 M21A Si2A 32.90(15) 3_666 3_667 ? O32 M21A Si2A 72.11(15) 2_465 3_667 ? O32 M21A Si2A 85.36(15) 3_666 3_667 ? SI2B M21A Si2A 142.05(18) 2_464 3_667 ? Si2A M21A Si2A 142.05(18) 2_464 3_667 ? SI2B M21A Si2A 0.00(12) 3_667 3_667 ? _diffrn_measured_fraction_theta_max 0.460 _diffrn_reflns_theta_full 29.36 _diffrn_measured_fraction_theta_full 0.460 _refine_diff_density_max 0.726 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.156