data_wiklundite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H108 As12 Cl36 Fe12 Mg Mn126 O288 Pb12 Si36' _chemical_formula_weight 18006.57 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 8.257(2) _cell_length_b 8.257(2) _cell_length_c 126.59(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7474(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4059 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description thin plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.030 mm _exptl_crystal_size_mid 0.020 mm _exptl_crystal_size_min 0.003 mm _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 4.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8382 _exptl_absorpt_coefficient_mu 14.302 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX II 4K CCD _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 15497 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -150 _diffrn_reflns_limit_l_max 150 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1480 _reflns_number_gt 1290 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0335P)^2^+120.9879P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1480 _refine_ls_number_parameters 151 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.169 _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 Pb Pb 0.0000 0.0000 0.337719(4) 0.03190(19) Uani 1 3 d S . . As As 0.0000 0.0000 0.306006(9) 0.0232(3) Uani 1 3 d S . . T Mn 0.0000 0.73465(18) 0.2500 0.0256(6) Uani 1.018(7) 2 d SP . . M1 Fe 0.6667 0.3333 0.287697(14) 0.0233(7) Uani 0.965(8) 3 d SP . . M2 Mn 0.55471(15) 0.62502(15) 0.267891(8) 0.0244(4) Uani 0.991(6) 1 d P . . M3 Mn 0.98277(14) 0.75908(14) 0.287118(8) 0.0242(4) Uani 1.002(5) 1 d P . . M4 Mn 0.08962(14) 0.44920(14) 0.305811(8) 0.0246(4) Uani 1.000(5) 1 d . . . M5 Mn 0.6667 0.3333 0.3333 0.0259(9) Uani 1.048(12) 6 d SP . . As1 As 0.6667 0.3333 0.25468(2) 0.0219(11) Uani 0.110(10) 3 d SP . . Si1 Si 0.6667 0.3333 0.25468(2) 0.0219(11) Uani 0.890(10) 3 d SP . . Si2 Si 0.0000 0.0000 0.26590(2) 0.0204(7) Uani 1 3 d S . . Si3 Si 0.3333 0.6667 0.28417(2) 0.0198(7) Uani 1 3 d S . . O1 O 0.6667 0.3333 0.24164(6) 0.0259(18) Uani 1 3 d S . . O2 O 0.8721(6) 0.4931(6) 0.25923(4) 0.0239(10) Uani 1 1 d . . . O3 O 0.0000 0.0000 0.27871(6) 0.0238(18) Uani 1 3 d S . . O4 O 0.0596(6) 0.2064(6) 0.26114(4) 0.0247(11) Uani 1 1 d . . . O5 O 0.3333 0.6667 0.29700(6) 0.0245(18) Uani 1 3 d S . . O6 O 0.1722(6) 0.7028(7) 0.27903(4) 0.0245(10) Uani 1 1 d . . . O7 O 0.0272(6) 0.1956(6) 0.29844(4) 0.0233(10) Uani 1 1 d . . . OH1 O 0.1538(7) 0.6884(7) 0.31599(4) 0.0281(11) Uani 1 1 d D . . OH2 O 0.6123(6) 0.1100(7) 0.29748(4) 0.0265(11) Uani 1 1 d D . . OH3 O 0.8239(6) 0.2626(6) 0.27845(4) 0.0250(11) Uani 1 1 d D . . Cl Cl 0.5834(3) 0.0507(3) 0.344833(15) 0.0352(5) Uani 1 1 d . . . H1 H 0.035(7) 0.679(13) 0.3182(8) 0.078(19) Uiso 1 1 d D . . H2 H 0.699(11) 0.163(14) 0.3034(5) 0.078(19) Uiso 1 1 d D . . H3 H 0.751(12) 0.206(14) 0.2720(5) 0.078(19) Uiso 1 1 d 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 Pb 0.0362(2) 0.0362(2) 0.0233(3) 0.000 0.000 0.01811(11) As 0.0246(4) 0.0246(4) 0.0203(6) 0.000 0.000 0.0123(2) T 0.0287(9) 0.0256(7) 0.0236(9) -0.0017(3) -0.0033(6) 0.0144(5) M1 0.0236(8) 0.0236(8) 0.0227(11) 0.000 0.000 0.0118(4) M2 0.0243(7) 0.0237(6) 0.0244(7) 0.0003(4) 0.0020(4) 0.0115(5) M3 0.0240(6) 0.0242(6) 0.0250(7) -0.0014(4) -0.0004(4) 0.0126(5) M4 0.0253(7) 0.0236(6) 0.0247(7) -0.0012(4) -0.0011(4) 0.0119(5) M5 0.0271(11) 0.0271(11) 0.0235(15) 0.000 0.000 0.0135(6) As1 0.0233(12) 0.0233(12) 0.0189(17) 0.000 0.000 0.0117(6) Si1 0.0233(12) 0.0233(12) 0.0189(17) 0.000 0.000 0.0117(6) Si2 0.0227(10) 0.0227(10) 0.0160(16) 0.000 0.000 0.0113(5) Si3 0.0210(10) 0.0210(10) 0.0174(16) 0.000 0.000 0.0105(5) O1 0.029(3) 0.029(3) 0.019(4) 0.000 0.000 0.0147(14) O2 0.024(2) 0.021(2) 0.024(3) 0.0013(19) -0.002(2) 0.009(2) O3 0.029(3) 0.029(3) 0.013(4) 0.000 0.000 0.0146(14) O4 0.028(3) 0.021(2) 0.027(3) 0.001(2) 0.002(2) 0.013(2) O5 0.027(3) 0.027(3) 0.018(4) 0.000 0.000 0.0137(14) O6 0.022(2) 0.031(3) 0.023(3) 0.000(2) 0.0005(19) 0.015(2) O7 0.029(3) 0.020(2) 0.023(3) 0.001(2) 0.000(2) 0.013(2) OH1 0.026(3) 0.026(3) 0.032(3) -0.001(2) 0.001(2) 0.013(2) OH2 0.023(3) 0.027(3) 0.027(3) 0.001(2) 0.001(2) 0.011(2) OH3 0.026(3) 0.022(2) 0.026(3) 0.002(2) 0.001(2) 0.012(2) Cl 0.0318(10) 0.0358(10) 0.0379(11) 0.0079(8) -0.0001(8) 0.0169(8) _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 Pb OH1 2.277(5) 32_445 ? Pb OH1 2.277(5) 33_545 ? Pb OH1 2.277(5) 31 ? Pb Cl 3.437(2) 33_445 ? Pb Cl 3.437(2) 31_545 ? Pb Cl 3.437(2) 32 ? Pb M4 3.4978(14) 32_445 ? Pb M4 3.4978(14) 31 ? Pb M4 3.4978(14) 33_545 ? Pb Cl 3.776(2) 3_665 ? Pb Cl 3.776(2) 2_545 ? Pb Cl 3.776(2) 1_455 ? As O7 1.793(5) . ? As O7 1.793(5) 2 ? As O7 1.793(5) 3 ? As M3 3.0677(15) 1_445 ? As M3 3.0677(15) 3_565 ? As M3 3.0677(16) 2_655 ? T O4 2.070(5) 3_565 ? T O4 2.070(5) 5_565 ? T O2 2.086(5) 1_455 ? T O2 2.086(5) 6_665 ? T O4 2.742(5) 2_565 ? T O4 2.742(5) 4_565 ? T Si2 2.975(2) 1_565 ? T Si2 2.975(2) 4_565 ? T As1 3.1282(13) 4 ? T Si1 3.1282(13) 4 ? T Si1 3.1283(13) 1_455 ? T As1 3.1283(13) 1_455 ? M1 OH3 2.038(5) 3_665 ? M1 OH3 2.038(5) 2_655 ? M1 OH3 2.039(5) . ? M1 OH2 2.075(5) 2_655 ? M1 OH2 2.075(5) 3_665 ? M1 OH2 2.076(5) . ? M2 O4 2.110(5) 2_665 ? M2 O2 2.164(5) 2_655 ? M2 OH3 2.266(5) 2_655 ? M2 O6 2.272(5) 3_565 ? M2 O6 2.329(5) 2_665 ? M2 O1 2.355(4) 4 ? M2 Si3 2.887(3) . ? M2 T 3.5102(13) 3_565 ? M2 T 3.5441(17) 2_665 ? M3 O6 2.107(5) 1_655 ? M3 OH3 2.160(5) 2_655 ? M3 O7 2.193(5) 3_665 ? M3 O3 2.197(4) 1_665 ? M3 OH2 2.275(5) 2_655 ? M3 O7 2.337(5) 2_665 ? M3 As 3.0674(15) 1_665 ? M4 O7 2.108(5) . ? M4 OH2 2.178(5) 2 ? M4 OH1 2.189(5) 2_665 ? M4 OH1 2.190(5) . ? M4 O5 2.215(4) . ? M4 Cl 2.682(2) 33_445 ? M4 Pb 3.4981(14) 31 ? M5 Cl 2.5364(19) 31_655 ? M5 Cl 2.536(2) 32 ? M5 Cl 2.5364(19) 33_545 ? M5 Cl 2.5364(19) . ? M5 Cl 2.537(2) 2_655 ? M5 Cl 2.5366(19) 3_665 ? As1 O2 1.647(5) 2_655 ? As1 O2 1.647(5) 3_665 ? As1 O2 1.647(5) . ? As1 O1 1.650(8) . ? As1 T 3.1282(13) 3 ? As1 T 3.1282(13) 1_655 ? As1 T 3.1282(13) 2_665 ? Si2 O3 1.622(8) . ? Si2 O4 1.634(5) . ? Si2 O4 1.634(5) 2 ? Si2 O4 1.634(5) 3 ? Si2 T 2.975(2) 1_545 ? Si2 T 2.975(2) 3_455 ? Si2 T 2.975(2) 2_665 ? Si3 O5 1.624(8) . ? Si3 O6 1.637(5) . ? Si3 O6 1.637(5) 3_565 ? Si3 O6 1.637(5) 2_665 ? Si3 M2 2.887(3) 3_565 ? Si3 M2 2.887(3) 2_665 ? O1 M2 2.354(4) 6_655 ? O1 M2 2.354(4) 5_665 ? O1 M2 2.354(4) 4 ? O2 T 2.086(5) 1_655 ? O2 M2 2.164(5) 3_665 ? O3 M3 2.197(4) 2_655 ? O3 M3 2.197(4) 1_445 ? O3 M3 2.197(4) 3_565 ? O4 T 2.070(5) 2_665 ? O4 M2 2.111(5) 3_565 ? O4 T 2.742(5) 3_455 ? O5 M4 2.215(4) 3_565 ? O5 M4 2.215(4) 2_665 ? O6 M3 2.107(5) 1_455 ? O6 M2 2.272(5) 2_665 ? O6 M2 2.329(5) 3_565 ? O7 M3 2.193(5) 2_655 ? O7 M3 2.337(5) 3_565 ? OH1 M4 2.189(5) 3_565 ? OH1 Pb 2.277(5) 31 ? OH2 M4 2.178(5) 3 ? OH2 M3 2.275(5) 3_665 ? OH3 M3 2.160(5) 3_665 ? OH3 M2 2.265(5) 3_665 ? Cl M4 2.681(2) 32_545 ? Cl Pb 3.437(2) 31_545 ? Cl Pb 3.776(2) 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 OH1 Pb OH1 73.9(2) 32_445 33_545 ? OH1 Pb OH1 73.9(2) 32_445 31 ? OH1 Pb OH1 73.9(2) 33_545 31 ? OH1 Pb Cl 85.10(13) 32_445 33_445 ? OH1 Pb Cl 117.59(13) 33_545 33_445 ? OH1 Pb Cl 152.42(13) 31 33_445 ? OH1 Pb Cl 152.42(13) 32_445 31_545 ? OH1 Pb Cl 85.10(13) 33_545 31_545 ? OH1 Pb Cl 117.59(13) 31 31_545 ? Cl Pb Cl 89.23(5) 33_445 31_545 ? OH1 Pb Cl 117.59(13) 32_445 32 ? OH1 Pb Cl 152.42(12) 33_545 32 ? OH1 Pb Cl 85.10(13) 31 32 ? Cl Pb Cl 89.23(5) 33_445 32 ? Cl Pb Cl 89.23(5) 31_545 32 ? OH1 Pb M4 37.57(13) 32_445 32_445 ? OH1 Pb M4 37.56(13) 33_545 32_445 ? OH1 Pb M4 77.09(13) 31 32_445 ? Cl Pb M4 97.08(4) 33_445 32_445 ? Cl Pb M4 117.18(4) 31_545 32_445 ? Cl Pb M4 152.79(4) 32 32_445 ? OH1 Pb M4 37.56(12) 32_445 31 ? OH1 Pb M4 77.09(13) 33_545 31 ? OH1 Pb M4 37.57(12) 31 31 ? Cl Pb M4 117.18(4) 33_445 31 ? Cl Pb M4 152.79(4) 31_545 31 ? Cl Pb M4 97.07(4) 32 31 ? M4 Pb M4 56.55(3) 32_445 31 ? OH1 Pb M4 77.09(13) 32_445 33_545 ? OH1 Pb M4 37.57(12) 33_545 33_545 ? OH1 Pb M4 37.56(13) 31 33_545 ? Cl Pb M4 152.79(4) 33_445 33_545 ? Cl Pb M4 97.07(4) 31_545 33_545 ? Cl Pb M4 117.18(4) 32 33_545 ? M4 Pb M4 56.55(3) 32_445 33_545 ? M4 Pb M4 56.55(3) 31 33_545 ? OH1 Pb Cl 59.45(13) 32_445 3_665 ? OH1 Pb Cl 120.13(13) 33_545 3_665 ? OH1 Pb Cl 59.40(13) 31 3_665 ? Cl Pb Cl 94.68(5) 33_445 3_665 ? Cl Pb Cl 148.08(3) 31_545 3_665 ? Cl Pb Cl 59.23(6) 32 3_665 ? M4 Pb Cl 93.80(4) 32_445 3_665 ? M4 Pb Cl 43.04(4) 31 3_665 ? M4 Pb Cl 93.75(4) 33_545 3_665 ? OH1 Pb Cl 120.12(13) 32_445 2_545 ? OH1 Pb Cl 59.40(13) 33_545 2_545 ? OH1 Pb Cl 59.45(13) 31 2_545 ? Cl Pb Cl 148.08(4) 33_445 2_545 ? Cl Pb Cl 59.23(6) 31_545 2_545 ? Cl Pb Cl 94.68(4) 32 2_545 ? M4 Pb Cl 93.75(4) 32_445 2_545 ? M4 Pb Cl 93.79(4) 31 2_545 ? M4 Pb Cl 43.04(3) 33_545 2_545 ? Cl Pb Cl 114.49(2) 3_665 2_545 ? OH1 Pb Cl 59.40(13) 32_445 1_455 ? OH1 Pb Cl 59.45(12) 33_545 1_455 ? OH1 Pb Cl 120.13(13) 31 1_455 ? Cl Pb Cl 59.23(6) 33_445 1_455 ? Cl Pb Cl 94.68(4) 31_545 1_455 ? Cl Pb Cl 148.08(3) 32 1_455 ? M4 Pb Cl 43.04(3) 32_445 1_455 ? M4 Pb Cl 93.76(4) 31 1_455 ? M4 Pb Cl 93.80(4) 33_545 1_455 ? Cl Pb Cl 114.49(2) 3_665 1_455 ? Cl Pb Cl 114.49(2) 2_545 1_455 ? O7 As O7 94.1(2) . 2 ? O7 As O7 94.1(2) . 3 ? O7 As O7 94.1(2) 2 3 ? O7 As M3 96.42(16) . 1_445 ? O7 As M3 49.37(15) 2 1_445 ? O7 As M3 44.72(15) 3 1_445 ? O7 As M3 49.37(16) . 3_565 ? O7 As M3 44.72(15) 2 3_565 ? O7 As M3 96.41(16) 3 3_565 ? M3 As M3 65.72(4) 1_445 3_565 ? O7 As M3 44.73(15) . 2_655 ? O7 As M3 96.41(16) 2 2_655 ? O7 As M3 49.37(15) 3 2_655 ? M3 As M3 65.72(4) 1_445 2_655 ? M3 As M3 65.72(4) 3_565 2_655 ? O7 As Pb 122.31(15) . . ? O7 As Pb 122.32(15) 2 . ? O7 As Pb 122.32(15) 3 . ? M3 As Pb 141.20(3) 1_445 . ? M3 As Pb 141.20(3) 3_565 . ? M3 As Pb 141.20(3) 2_655 . ? O4 T O4 116.3(3) 3_565 5_565 ? O4 T O2 102.24(18) 3_565 1_455 ? O4 T O2 122.02(19) 5_565 1_455 ? O4 T O2 122.02(19) 3_565 6_665 ? O4 T O2 102.23(18) 5_565 6_665 ? O2 T O2 90.7(3) 1_455 6_665 ? O4 T O4 64.5(2) 3_565 2_565 ? O4 T O4 74.05(19) 5_565 2_565 ? O2 T O4 86.87(16) 1_455 2_565 ? O2 T O4 173.40(17) 6_665 2_565 ? O4 T O4 74.04(19) 3_565 4_565 ? O4 T O4 64.5(2) 5_565 4_565 ? O2 T O4 173.40(16) 1_455 4_565 ? O2 T O4 86.86(17) 6_665 4_565 ? O4 T O4 96.2(2) 2_565 4_565 ? O4 T Si2 31.82(13) 3_565 1_565 ? O4 T Si2 94.13(14) 5_565 1_565 ? O2 T Si2 97.99(14) 1_455 1_565 ? O2 T Si2 153.70(13) 6_665 1_565 ? O4 T Si2 32.89(10) 2_565 1_565 ? O4 T Si2 81.73(11) 4_565 1_565 ? O4 T Si2 94.13(14) 3_565 4_565 ? O4 T Si2 31.82(13) 5_565 4_565 ? O2 T Si2 153.70(13) 1_455 4_565 ? O2 T Si2 97.98(14) 6_665 4_565 ? O4 T Si2 81.73(11) 2_565 4_565 ? O4 T Si2 32.89(10) 4_565 4_565 ? Si2 T Si2 85.13(10) 1_565 4_565 ? O4 T As1 93.98(13) 3_565 4 ? O4 T As1 125.76(14) 5_565 4 ? O2 T As1 90.27(14) 1_455 4 ? O2 T As1 28.90(13) 6_665 4 ? O4 T As1 157.06(11) 2_565 4 ? O4 T As1 84.62(10) 4_565 4 ? Si2 T As1 125.74(4) 1_565 4 ? Si2 T As1 109.16(5) 4_565 4 ? O4 T Si1 93.98(13) 3_565 4 ? O4 T Si1 125.76(14) 5_565 4 ? O2 T Si1 90.27(14) 1_455 4 ? O2 T Si1 28.90(13) 6_665 4 ? O4 T Si1 157.06(11) 2_565 4 ? O4 T Si1 84.62(10) 4_565 4 ? Si2 T Si1 125.74(4) 1_565 4 ? Si2 T Si1 109.16(5) 4_565 4 ? As1 T Si1 0.00(10) 4 4 ? O4 T Si1 125.75(14) 3_565 1_455 ? O4 T Si1 93.99(13) 5_565 1_455 ? O2 T Si1 28.89(13) 1_455 1_455 ? O2 T Si1 90.27(14) 6_665 1_455 ? O4 T Si1 84.61(10) 2_565 1_455 ? O4 T Si1 157.07(11) 4_565 1_455 ? Si2 T Si1 109.15(5) 1_565 1_455 ? Si2 T Si1 125.75(4) 4_565 1_455 ? As1 T Si1 103.46(5) 4 1_455 ? Si1 T Si1 103.46(5) 4 1_455 ? O4 T As1 125.75(14) 3_565 1_455 ? O4 T As1 93.99(13) 5_565 1_455 ? O2 T As1 28.89(13) 1_455 1_455 ? O2 T As1 90.27(14) 6_665 1_455 ? O4 T As1 84.61(10) 2_565 1_455 ? O4 T As1 157.07(11) 4_565 1_455 ? Si2 T As1 109.15(5) 1_565 1_455 ? Si2 T As1 125.75(4) 4_565 1_455 ? As1 T As1 103.46(5) 4 1_455 ? Si1 T As1 103.46(5) 4 1_455 ? Si1 T As1 0.00(10) 1_455 1_455 ? OH3 M1 OH3 90.3(2) 3_665 2_655 ? OH3 M1 OH3 90.3(2) 3_665 . ? OH3 M1 OH3 90.3(2) 2_655 . ? OH3 M1 OH2 176.28(19) 3_665 2_655 ? OH3 M1 OH2 88.47(19) 2_655 2_655 ? OH3 M1 OH2 93.20(19) . 2_655 ? OH3 M1 OH2 88.47(19) 3_665 3_665 ? OH3 M1 OH2 93.20(19) 2_655 3_665 ? OH3 M1 OH2 176.29(19) . 3_665 ? OH2 M1 OH2 88.1(2) 2_655 3_665 ? OH3 M1 OH2 93.20(19) 3_665 . ? OH3 M1 OH2 176.3(2) 2_655 . ? OH3 M1 OH2 88.48(19) . . ? OH2 M1 OH2 88.1(2) 2_655 . ? OH2 M1 OH2 88.1(2) 3_665 . ? O4 M2 O2 106.45(18) 2_665 2_655 ? O4 M2 OH3 90.72(18) 2_665 2_655 ? O2 M2 OH3 84.91(17) 2_655 2_655 ? O4 M2 O6 88.88(18) 2_665 3_565 ? O2 M2 O6 164.57(18) 2_655 3_565 ? OH3 M2 O6 96.83(17) 2_655 3_565 ? O4 M2 O6 157.70(18) 2_665 2_665 ? O2 M2 O6 95.81(18) 2_655 2_665 ? OH3 M2 O6 92.57(17) 2_655 2_665 ? O6 M2 O6 68.8(2) 3_565 2_665 ? O4 M2 O1 96.29(16) 2_665 4 ? O2 M2 O1 94.98(17) 2_655 4 ? OH3 M2 O1 172.72(19) 2_655 4 ? O6 M2 O1 81.36(19) 3_565 4 ? O6 M2 O1 80.19(18) 2_665 4 ? O4 M2 Si3 123.19(14) 2_665 . ? O2 M2 Si3 130.12(13) 2_655 . ? OH3 M2 Si3 98.11(14) 2_655 . ? O6 M2 Si3 34.46(12) 3_565 . ? O6 M2 Si3 34.52(11) 2_665 . ? O1 M2 Si3 76.38(18) 4 . ? O4 M2 T 32.54(13) 2_665 3_565 ? O2 M2 T 107.41(13) 2_655 3_565 ? OH3 M2 T 123.24(13) 2_655 3_565 ? O6 M2 T 84.53(12) 3_565 3_565 ? O6 M2 T 138.07(12) 2_665 3_565 ? O1 M2 T 63.75(10) 4 3_565 ? Si3 M2 T 111.68(5) . 3_565 ? O4 M2 T 115.28(14) 2_665 2_665 ? O2 M2 T 32.81(12) 2_655 2_665 ? OH3 M2 T 115.51(13) 2_655 2_665 ? O6 M2 T 137.99(13) 3_565 2_665 ? O6 M2 T 82.96(12) 2_665 2_665 ? O1 M2 T 63.10(9) 4 2_665 ? Si3 M2 T 110.74(4) . 2_665 ? T M2 T 97.91(4) 3_565 2_665 ? O6 M3 OH3 96.05(18) 1_655 2_655 ? O6 M3 O7 101.42(18) 1_655 3_665 ? OH3 M3 O7 162.52(18) 2_655 3_665 ? O6 M3 O3 104.18(18) 1_655 1_665 ? OH3 M3 O3 92.86(17) 2_655 1_665 ? O7 M3 O3 83.41(19) 3_665 1_665 ? O6 M3 OH2 90.90(18) 1_655 2_655 ? OH3 M3 OH2 80.61(18) 2_655 2_655 ? O7 M3 OH2 98.49(18) 3_665 2_655 ? O3 M3 OH2 164.18(16) 1_665 2_655 ? O6 M3 O7 170.77(18) 1_655 2_665 ? OH3 M3 O7 91.83(18) 2_655 2_665 ? O7 M3 O7 70.7(2) 3_665 2_665 ? O3 M3 O7 80.14(18) 1_665 2_665 ? OH2 M3 O7 85.65(17) 2_655 2_665 ? O6 M3 As 136.32(14) 1_655 1_665 ? OH3 M3 As 127.43(13) 2_655 1_665 ? O7 M3 As 35.12(12) 3_665 1_665 ? O3 M3 As 80.19(18) 1_665 1_665 ? OH2 M3 As 92.30(13) 2_655 1_665 ? O7 M3 As 35.60(12) 2_665 1_665 ? O7 M4 OH2 98.74(18) . 2 ? O7 M4 OH1 95.90(18) . 2_665 ? OH2 M4 OH1 165.34(19) 2 2_665 ? O7 M4 OH1 170.16(19) . . ? OH2 M4 OH1 88.27(19) 2 . ? OH1 M4 OH1 77.3(3) 2_665 . ? O7 M4 O5 104.71(18) . . ? OH2 M4 O5 93.72(18) 2 . ? OH1 M4 O5 81.57(19) 2_665 . ? OH1 M4 O5 81.56(19) . . ? O7 M4 Cl 88.54(14) . 33_445 ? OH2 M4 Cl 97.57(15) 2 33_445 ? OH1 M4 Cl 83.75(15) 2_665 33_445 ? OH1 M4 Cl 83.67(15) . 33_445 ? O5 M4 Cl 161.10(19) . 33_445 ? O7 M4 Pb 132.28(13) . 31 ? OH2 M4 Pb 126.95(13) 2 31 ? OH1 M4 Pb 39.35(13) 2_665 31 ? OH1 M4 Pb 39.34(13) . 31 ? O5 M4 Pb 87.09(18) . 31 ? Cl M4 Pb 74.01(5) 33_445 31 ? Cl M5 Cl 90.34(7) 31_655 32 ? Cl M5 Cl 90.34(7) 31_655 33_545 ? Cl M5 Cl 90.34(7) 32 33_545 ? Cl M5 Cl 180.00(7) 31_655 . ? Cl M5 Cl 89.66(7) 32 . ? Cl M5 Cl 89.66(7) 33_545 . ? Cl M5 Cl 89.67(7) 31_655 2_655 ? Cl M5 Cl 179.993(1) 32 2_655 ? Cl M5 Cl 89.67(7) 33_545 2_655 ? Cl M5 Cl 90.33(7) . 2_655 ? Cl M5 Cl 89.67(7) 31_655 3_665 ? Cl M5 Cl 89.67(7) 32 3_665 ? Cl M5 Cl 179.992(2) 33_545 3_665 ? Cl M5 Cl 90.33(7) . 3_665 ? Cl M5 Cl 90.33(7) 2_655 3_665 ? O2 As1 O2 108.44(19) 2_655 3_665 ? O2 As1 O2 108.44(19) 2_655 . ? O2 As1 O2 108.44(19) 3_665 . ? O2 As1 O1 110.48(18) 2_655 . ? O2 As1 O1 110.48(18) 3_665 . ? O2 As1 O1 110.48(18) . . ? O2 As1 T 141.66(17) 2_655 3 ? O2 As1 T 37.75(16) 3_665 3 ? O2 As1 T 101.82(16) . 3 ? O1 As1 T 79.10(5) . 3 ? O2 As1 T 101.82(17) 2_655 1_655 ? O2 As1 T 141.66(17) 3_665 1_655 ? O2 As1 T 37.75(16) . 1_655 ? O1 As1 T 79.10(5) . 1_655 ? T As1 T 116.51(3) 3 1_655 ? O2 As1 T 37.75(16) 2_655 2_665 ? O2 As1 T 101.82(16) 3_665 2_665 ? O2 As1 T 141.66(16) . 2_665 ? O1 As1 T 79.10(5) . 2_665 ? T As1 T 116.51(3) 3 2_665 ? T As1 T 116.51(3) 1_655 2_665 ? O3 Si2 O4 111.61(19) . . ? O3 Si2 O4 111.6(2) . 2 ? O4 Si2 O4 107.2(2) . 2 ? O3 Si2 O4 111.61(19) . 3 ? O4 Si2 O4 107.2(2) . 3 ? O4 Si2 O4 107.2(2) 2 3 ? O3 Si2 T 132.56(5) . 1_545 ? O4 Si2 T 114.1(2) . 1_545 ? O4 Si2 T 65.70(18) 2 1_545 ? O4 Si2 T 41.92(17) 3 1_545 ? O3 Si2 T 132.56(5) . 3_455 ? O4 Si2 T 65.71(18) . 3_455 ? O4 Si2 T 41.92(17) 2 3_455 ? O4 Si2 T 114.1(2) 3 3_455 ? T Si2 T 79.27(8) 1_545 3_455 ? O3 Si2 T 132.56(5) . 2_665 ? O4 Si2 T 41.92(17) . 2_665 ? O4 Si2 T 114.1(2) 2 2_665 ? O4 Si2 T 65.70(18) 3 2_665 ? T Si2 T 79.27(8) 1_545 2_665 ? T Si2 T 79.27(8) 3_455 2_665 ? O5 Si3 O6 113.43(19) . . ? O5 Si3 O6 113.4(2) . 3_565 ? O6 Si3 O6 105.2(2) . 3_565 ? O5 Si3 O6 113.45(19) . 2_665 ? O6 Si3 O6 105.2(2) . 2_665 ? O6 Si3 O6 105.2(2) 3_565 2_665 ? O5 Si3 M2 135.54(5) . 3_565 ? O6 Si3 M2 53.75(18) . 3_565 ? O6 Si3 M2 111.0(2) 3_565 3_565 ? O6 Si3 M2 51.76(17) 2_665 3_565 ? O5 Si3 M2 135.54(5) . 2_665 ? O6 Si3 M2 51.76(18) . 2_665 ? O6 Si3 M2 53.75(18) 3_565 2_665 ? O6 Si3 M2 111.0(2) 2_665 2_665 ? M2 Si3 M2 74.68(8) 3_565 2_665 ? O5 Si3 M2 135.55(5) . . ? O6 Si3 M2 111.0(2) . . ? O6 Si3 M2 51.76(17) 3_565 . ? O6 Si3 M2 53.75(18) 2_665 . ? M2 Si3 M2 74.68(8) 3_565 . ? M2 Si3 M2 74.68(8) 2_665 . ? As1 O1 M2 120.82(17) . 6_655 ? As1 O1 M2 120.82(17) . 5_665 ? M2 O1 M2 96.1(2) 6_655 5_665 ? As1 O1 M2 120.82(17) . 4 ? M2 O1 M2 96.1(2) 6_655 4 ? M2 O1 M2 96.1(2) 5_665 4 ? As1 O2 T 113.4(2) . 1_655 ? As1 O2 M2 127.0(2) . 3_665 ? T O2 M2 113.0(2) 1_655 3_665 ? Si2 O3 M3 118.99(17) . 2_655 ? Si2 O3 M3 118.99(17) . 1_445 ? M3 O3 M3 98.5(2) 2_655 1_445 ? Si2 O3 M3 118.99(17) . 3_565 ? M3 O3 M3 98.5(2) 2_655 3_565 ? M3 O3 M3 98.5(2) 1_445 3_565 ? Si2 O4 T 106.3(2) . 2_665 ? Si2 O4 M2 132.5(3) . 3_565 ? T O4 M2 114.2(2) 2_665 3_565 ? Si2 O4 T 81.40(19) . 3_455 ? T O4 T 103.23(19) 2_665 3_455 ? M2 O4 T 111.09(18) 3_565 3_455 ? Si3 O5 M4 120.25(18) . . ? Si3 O5 M4 120.25(18) . 3_565 ? M4 O5 M4 96.9(2) . 3_565 ? Si3 O5 M4 120.25(18) . 2_665 ? M4 O5 M4 96.9(2) . 2_665 ? M4 O5 M4 96.8(2) 3_565 2_665 ? Si3 O6 M3 127.4(3) . 1_455 ? Si3 O6 M2 93.8(2) . 2_665 ? M3 O6 M2 116.2(2) 1_455 2_665 ? Si3 O6 M2 91.7(2) . 3_565 ? M3 O6 M2 121.8(2) 1_455 3_565 ? M2 O6 M2 99.10(19) 2_665 3_565 ? As O7 M4 121.1(2) . . ? As O7 M3 100.2(2) . 2_655 ? M4 O7 M3 113.6(2) . 2_655 ? As O7 M3 95.03(19) . 3_565 ? M4 O7 M3 126.6(2) . 3_565 ? M3 O7 M3 94.54(18) 2_655 3_565 ? M4 OH1 M4 98.3(2) 3_565 . ? M4 OH1 Pb 103.10(19) 3_565 31 ? M4 OH1 Pb 103.08(19) . 31 ? M1 OH2 M4 131.4(2) . 3 ? M1 OH2 M3 93.14(19) . 3_665 ? M4 OH2 M3 122.1(2) 3 3_665 ? M1 OH3 M3 97.7(2) . 3_665 ? M1 OH3 M2 129.5(2) . 3_665 ? M3 OH3 M2 127.3(2) 3_665 3_665 ? M5 Cl M4 127.52(8) . 32_545 ? M5 Cl Pb 105.93(7) . 31_545 ? M4 Cl Pb 118.76(7) 32_545 31_545 ? M5 Cl Pb 97.02(5) . 1_655 ? M4 Cl Pb 62.94(5) 32_545 1_655 ? Pb Cl Pb 85.32(4) 31_545 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OH1 H1 Cl 0.9800(18) 2.195(15) 3.167(5) 171(9) 31 OH2 H2 Cl 0.980(3) 2.62(2) 3.579(5) 167(8) 33_545 OH3 H3 O2 0.980(3) 1.871(14) 2.847(7) 173(10) 3_665 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.143 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.171