The crystal structure of munakataite, Pb2Cu2(Se4+O3)(SO4)(OH)4, from Otto Mountain, San Bernardino County, California, USA A. R. KAMPF1,*, S. J. MILLS2 AND R. M. HOUSLEY3 data_mun _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Cu3.79 O22 Pb3.87 S2.30 Se1.70' _chemical_formula_weight 1610.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.802(3) _cell_length_b 5.6751(14) _cell_length_c 9.281(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.443(6) _cell_angle_gamma 90.00 _cell_volume 504.2(2) _cell_formula_units_Z 1 _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 0.11 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 39.514 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0978 _exptl_absorpt_correction_T_max 0.8269 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _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 8377 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 20.79 _reflns_number_total 590 _reflns_number_gt 544 _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^)+(0.0000P)^2^+22.0107P] 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 590 _refine_ls_number_parameters 106 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.536 _refine_ls_shift/su_mean 0.005 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 Pb1 Pb 0.31694(9) 0.2500 0.41854(10) 0.0219(4) Uani 0.976(14) 2 d SP . . Pb2 Pb 0.33579(10) 0.2500 0.97549(12) 0.0329(5) Uani 0.958(14) 2 d SP . . Cu Cu 0.9886(2) -0.0002(3) 0.24421(19) 0.0148(9) Uani 0.947(14) 1 d P . . Se1 Se 0.3597(2) 0.7500 0.2215(3) 0.0174(12) Uani 0.85(3) 2 d SP . . S1 S 0.3597(2) 0.7500 0.2215(3) 0.0174(12) Uani 0.15(3) 2 d SP . . S2 S 0.3349(6) 0.7500 0.6883(6) 0.0172(18) Uani 1 2 d S . . O11 O 0.376(2) 0.7500 0.0476(18) 0.045(5) Uani 1 2 d S . . O12 O 0.2514(10) 0.5148(18) 0.2152(11) 0.023(3) Uani 1 1 d . . . O21 O 0.4828(15) 0.7500 0.7514(16) 0.028(4) Uani 1 2 d S . . O22 O 0.3154(17) 0.7500 0.5248(15) 0.035(5) Uani 1 2 d S . . O23 O 0.2690(11) 0.963(2) 0.7326(11) 0.031(3) Uani 1 1 d . . . OH1 O 0.0260(15) 0.7500 0.3883(16) 0.018(4) Uani 1 2 d SD . . H1 H 0.119(5) 0.7500 0.40(3) 0.050 Uiso 1 2 d SD . . OH2 O 0.0775(15) 0.2500 0.3780(14) 0.016(4) Uani 1 2 d SD . . H2 H 0.06(3) 0.2500 0.470(11) 0.050 Uiso 1 2 d SD . . OH3 O 0.0529(14) 0.7500 0.8975(16) 0.019(4) Uani 1 2 d SD . . H3 H 0.141(10) 0.7500 0.95(2) 0.050 Uiso 1 2 d SD . . OH4 O 0.0881(15) 0.2500 0.8924(14) 0.019(4) Uani 1 2 d SD . . H4 H 0.07(3) 0.2500 0.984(12) 0.050 Uiso 1 2 d SD . . 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 Pb1 0.0208(7) 0.0198(6) 0.0232(7) 0.000 0.0008(4) 0.000 Pb2 0.0195(7) 0.0331(8) 0.0436(8) 0.000 0.0010(5) 0.000 Cu 0.0221(14) 0.0079(13) 0.0137(12) 0.0001(9) 0.0024(9) -0.0011(9) Se1 0.0190(18) 0.0146(17) 0.0191(17) 0.000 0.0054(11) 0.000 S1 0.0190(18) 0.0146(17) 0.0191(17) 0.000 0.0054(11) 0.000 S2 0.016(4) 0.010(3) 0.026(4) 0.000 0.006(3) 0.000 O11 0.064(13) 0.049(13) 0.026(10) 0.000 0.020(9) 0.000 O12 0.019(6) 0.021(7) 0.027(6) 0.003(5) 0.003(5) -0.002(5) O21 0.019(10) 0.039(11) 0.027(9) 0.000 0.009(7) 0.000 O22 0.041(11) 0.062(13) 0.000(8) 0.000 0.001(7) 0.000 O23 0.036(7) 0.026(7) 0.031(7) 0.006(6) 0.006(6) 0.008(6) OH1 0.017(8) 0.014(9) 0.019(8) 0.000 -0.004(7) 0.000 OH2 0.023(9) 0.016(9) 0.008(8) 0.000 0.000(7) 0.000 OH3 0.007(8) 0.021(9) 0.023(9) 0.000 -0.009(7) 0.000 OH4 0.029(9) 0.024(9) 0.002(8) 0.000 -0.004(7) 0.000 _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 Pb1 OH2 2.296(14) . ? Pb1 O12 2.389(10) 4_565 ? Pb1 O12 2.389(10) . ? Pb1 O21 2.771(15) 3_666 ? Pb1 O22 3.005(5) 1_545 ? Pb1 O22 3.005(5) . ? Pb1 S1 3.4502(16) 1_545 ? Pb1 Se1 3.4502(16) 1_545 ? Pb1 Se1 3.4502(16) . ? Pb1 O23 3.458(11) 1_545 ? Pb1 O23 3.458(11) 4_575 ? Pb1 O22 3.528(16) 3_666 ? Pb1 Cu 3.570(2) 1_455 ? Pb1 Cu 3.570(2) 4_465 ? Pb1 S2 3.754(6) 3_666 ? Pb2 OH4 2.384(15) . ? Pb2 O23 2.743(11) 1_545 ? Pb2 O23 2.743(11) 4_575 ? Pb2 O21 2.764(15) 3_667 ? Pb2 O11 2.875(19) 3_666 ? Pb2 O11 2.923(4) 1_546 ? Pb2 O11 2.923(4) 1_556 ? Pb2 O12 2.947(10) 1_556 ? Pb2 O12 2.947(10) 4_566 ? Pb2 S1 3.6176(18) 1_546 ? Pb2 Se1 3.6176(18) 1_546 ? Pb2 S1 3.6176(18) 1_556 ? Pb2 Se1 3.6176(18) 1_556 ? Pb2 Cu 3.672(2) 3_656 ? Pb2 Cu 3.672(2) 2_656 ? Pb2 S1 3.821(3) 3_666 ? Cu OH3 1.919(10) 3_666 ? Cu OH1 1.929(10) 1_645 ? Cu OH4 1.942(9) 3_656 ? Cu OH2 1.962(9) 1_655 ? Cu O23 2.589(11) 3_666 ? Cu O12 2.648(10) 4_665 ? Cu Cu 2.835(4) 4 ? Cu Cu 2.840(4) 4_565 ? Cu Pb1 3.570(2) 1_655 ? Cu S2 3.650(5) 3_666 ? Se1 O11 1.656(16) . ? Se1 O12 1.699(10) . ? Se1 O12 1.699(10) 4_575 ? Se1 Pb1 3.4502(16) 1_565 ? Se1 Pb2 3.6176(18) 1_554 ? Se1 Pb2 3.6176(18) 1_564 ? Se1 Pb2 3.821(3) 3_666 ? Se1 Cu 3.952(3) 1_465 ? Se1 Cu 3.952(3) 4_465 ? Se1 Pb1 4.080(3) 3_666 ? S2 O21 1.442(16) . ? S2 O23 1.471(12) 4_575 ? S2 O23 1.471(12) . ? S2 O22 1.488(15) . ? S2 Cu 3.650(5) 3_666 ? S2 Cu 3.650(5) 2_656 ? S2 Pb1 3.754(6) 3_666 ? S2 Pb1 3.763(4) 1_565 ? S2 Pb2 3.892(4) 1_565 ? S2 Pb2 3.977(6) 3_667 ? O11 Pb2 2.875(18) 3_666 ? O11 Pb2 2.923(4) 1_554 ? O11 Pb2 2.923(4) 1_564 ? O12 Cu 2.648(10) 4_465 ? O12 Pb2 2.947(10) 1_554 ? O12 Cu 3.818(10) 1_465 ? O12 Cu 3.943(10) 1_455 ? O21 Pb2 2.764(15) 3_667 ? O21 Pb1 2.771(15) 3_666 ? O21 Pb2 3.968(10) 1_565 ? O22 Pb1 3.005(5) 1_565 ? O22 Pb1 3.528(16) 3_666 ? O22 Cu 3.931(14) 4_465 ? O22 Cu 3.931(14) 1_465 ? O23 Cu 2.589(11) 3_666 ? O23 Pb2 2.743(11) 1_565 ? O23 Pb1 3.458(11) 1_565 ? O23 Cu 3.684(12) 2_656 ? O23 Cu 3.992(11) 2_666 ? OH1 Cu 1.929(10) 1_465 ? OH1 Cu 1.929(10) 4_465 ? OH1 Cu 3.725(14) 3_666 ? OH1 Cu 3.725(14) 2_656 ? OH1 Pb1 3.990(10) 1_565 ? OH1 Pb1 4.136(15) 3_566 ? OH1 H1 0.90(3) . ? OH2 Cu 1.962(9) 4_465 ? OH2 Cu 1.962(9) 1_455 ? OH2 Cu 3.963(13) 2_656 ? OH2 Cu 3.963(13) 3_656 ? OH2 H2 0.90(3) . ? OH3 Cu 1.919(10) 3_666 ? OH3 Cu 1.919(10) 2_656 ? OH3 Cu 3.692(14) 1_466 ? OH3 Cu 3.692(14) 4_466 ? OH3 Pb2 3.924(9) 1_565 ? OH3 Pb1 4.143(13) 3_566 ? OH3 H3 0.90(3) . ? OH4 Cu 1.942(9) 2_656 ? OH4 Cu 1.942(9) 3_656 ? OH4 Cu 3.873(13) 4_466 ? OH4 Cu 3.873(13) 1_456 ? OH4 H4 0.90(3) . ? 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 OH2 Pb1 O12 77.2(3) . 4_565 ? OH2 Pb1 O12 77.2(3) . . ? O12 Pb1 O12 77.9(5) 4_565 . ? OH2 Pb1 O21 137.0(5) . 3_666 ? O12 Pb1 O21 69.7(3) 4_565 3_666 ? O12 Pb1 O21 69.7(3) . 3_666 ? OH2 Pb1 O22 88.7(3) . 1_545 ? O12 Pb1 O22 69.3(3) 4_565 1_545 ? O12 Pb1 O22 146.5(4) . 1_545 ? O21 Pb1 O22 104.0(3) 3_666 1_545 ? OH2 Pb1 O22 88.7(3) . . ? O12 Pb1 O22 146.5(4) 4_565 . ? O12 Pb1 O22 69.3(3) . . ? O21 Pb1 O22 103.9(3) 3_666 . ? O22 Pb1 O22 141.6(5) 1_545 . ? OH2 Pb1 S1 98.62(19) . 1_545 ? O12 Pb1 S1 26.7(2) 4_565 1_545 ? O12 Pb1 S1 98.1(2) . 1_545 ? O21 Pb1 S1 61.06(11) 3_666 1_545 ? O22 Pb1 S1 53.6(3) 1_545 1_545 ? O22 Pb1 S1 163.8(3) . 1_545 ? OH2 Pb1 Se1 98.62(19) . 1_545 ? O12 Pb1 Se1 26.7(2) 4_565 1_545 ? O12 Pb1 Se1 98.1(2) . 1_545 ? O21 Pb1 Se1 61.06(11) 3_666 1_545 ? O22 Pb1 Se1 53.6(3) 1_545 1_545 ? O22 Pb1 Se1 163.8(3) . 1_545 ? S1 Pb1 Se1 0.00(11) 1_545 1_545 ? OH2 Pb1 Se1 98.62(19) . . ? O12 Pb1 Se1 98.1(2) 4_565 . ? O12 Pb1 Se1 26.7(2) . . ? O21 Pb1 Se1 61.06(11) 3_666 . ? O22 Pb1 Se1 163.8(3) 1_545 . ? O22 Pb1 Se1 53.6(3) . . ? S1 Pb1 Se1 110.66(7) 1_545 . ? Se1 Pb1 Se1 110.66(7) 1_545 . ? OH2 Pb1 O23 79.5(3) . 1_545 ? O12 Pb1 O23 107.9(3) 4_565 1_545 ? O12 Pb1 O23 154.1(3) . 1_545 ? O21 Pb1 O23 136.2(3) 3_666 1_545 ? O22 Pb1 O23 42.9(3) 1_545 1_545 ? O22 Pb1 O23 99.0(3) . 1_545 ? S1 Pb1 O23 96.53(19) 1_545 1_545 ? Se1 Pb1 O23 96.53(19) 1_545 1_545 ? Se1 Pb1 O23 152.65(19) . 1_545 ? OH2 Pb1 O23 79.5(3) . 4_575 ? O12 Pb1 O23 154.1(3) 4_565 4_575 ? O12 Pb1 O23 107.9(3) . 4_575 ? O21 Pb1 O23 136.2(3) 3_666 4_575 ? O22 Pb1 O23 99.0(3) 1_545 4_575 ? O22 Pb1 O23 42.9(3) . 4_575 ? S1 Pb1 O23 152.65(19) 1_545 4_575 ? Se1 Pb1 O23 152.65(19) 1_545 4_575 ? Se1 Pb1 O23 96.53(19) . 4_575 ? O23 Pb1 O23 56.2(4) 1_545 4_575 ? OH2 Pb1 O22 179.2(4) . 3_666 ? O12 Pb1 O22 102.1(3) 4_565 3_666 ? O12 Pb1 O22 102.1(3) . 3_666 ? O21 Pb1 O22 42.2(4) 3_666 3_666 ? O22 Pb1 O22 91.6(3) 1_545 3_666 ? O22 Pb1 O22 91.6(3) . 3_666 ? S1 Pb1 O22 80.92(13) 1_545 3_666 ? Se1 Pb1 O22 80.92(13) 1_545 3_666 ? Se1 Pb1 O22 80.92(13) . 3_666 ? O23 Pb1 O22 101.2(3) 1_545 3_666 ? O23 Pb1 O22 101.2(3) 4_575 3_666 ? OH2 Pb1 Cu 30.2(2) . 1_455 ? O12 Pb1 Cu 47.9(2) 4_565 1_455 ? O12 Pb1 Cu 80.2(2) . 1_455 ? O21 Pb1 Cu 115.0(3) 3_666 1_455 ? O22 Pb1 Cu 72.9(3) 1_545 1_455 ? O22 Pb1 Cu 117.2(3) . 1_455 ? S1 Pb1 Cu 68.48(5) 1_545 1_455 ? Se1 Pb1 Cu 68.48(5) 1_545 1_455 ? Se1 Pb1 Cu 106.71(5) . 1_455 ? O23 Pb1 Cu 85.51(19) 1_545 1_455 ? O23 Pb1 Cu 107.24(18) 4_575 1_455 ? O22 Pb1 Cu 149.27(14) 3_666 1_455 ? OH2 Pb1 Cu 30.2(2) . 4_465 ? O12 Pb1 Cu 80.2(2) 4_565 4_465 ? O12 Pb1 Cu 47.9(2) . 4_465 ? O21 Pb1 Cu 115.0(3) 3_666 4_465 ? O22 Pb1 Cu 117.2(3) 1_545 4_465 ? O22 Pb1 Cu 72.9(3) . 4_465 ? S1 Pb1 Cu 106.71(5) 1_545 4_465 ? Se1 Pb1 Cu 106.71(5) 1_545 4_465 ? Se1 Pb1 Cu 68.48(5) . 4_465 ? O23 Pb1 Cu 107.24(18) 1_545 4_465 ? O23 Pb1 Cu 85.51(18) 4_575 4_465 ? O22 Pb1 Cu 149.27(14) 3_666 4_465 ? Cu Pb1 Cu 46.88(6) 1_455 4_465 ? OH2 Pb1 S2 155.8(3) . 3_666 ? O12 Pb1 S2 84.1(2) 4_565 3_666 ? O12 Pb1 S2 84.1(2) . 3_666 ? O21 Pb1 S2 18.8(3) 3_666 3_666 ? O22 Pb1 S2 99.0(3) 1_545 3_666 ? O22 Pb1 S2 99.0(3) . 3_666 ? S1 Pb1 S2 68.82(6) 1_545 3_666 ? Se1 Pb1 S2 68.82(6) 1_545 3_666 ? Se1 Pb1 S2 68.82(6) . 3_666 ? O23 Pb1 S2 121.3(2) 1_545 3_666 ? O23 Pb1 S2 121.3(2) 4_575 3_666 ? O22 Pb1 S2 23.3(2) 3_666 3_666 ? Cu Pb1 S2 131.48(8) 1_455 3_666 ? Cu Pb1 S2 131.48(8) 4_465 3_666 ? OH4 Pb2 O23 71.8(3) . 1_545 ? OH4 Pb2 O23 71.8(3) . 4_575 ? O23 Pb2 O23 72.8(5) 1_545 4_575 ? OH4 Pb2 O21 134.9(4) . 3_667 ? O23 Pb2 O21 138.2(3) 1_545 3_667 ? O23 Pb2 O21 138.2(3) 4_575 3_667 ? OH4 Pb2 O11 157.4(5) . 3_666 ? O23 Pb2 O11 90.2(3) 1_545 3_666 ? O23 Pb2 O11 90.2(4) 4_575 3_666 ? O21 Pb2 O11 67.7(4) 3_667 3_666 ? OH4 Pb2 O11 98.8(4) . 1_546 ? O23 Pb2 O11 67.0(4) 1_545 1_546 ? O23 Pb2 O11 139.6(4) 4_575 1_546 ? O21 Pb2 O11 76.2(3) 3_667 1_546 ? O11 Pb2 O11 86.0(4) 3_666 1_546 ? OH4 Pb2 O11 98.8(4) . 1_556 ? O23 Pb2 O11 139.6(4) 1_545 1_556 ? O23 Pb2 O11 67.0(4) 4_575 1_556 ? O21 Pb2 O11 76.2(3) 3_667 1_556 ? O11 Pb2 O11 86.0(4) 3_666 1_556 ? O11 Pb2 O11 152.2(6) 1_546 1_556 ? OH4 Pb2 O12 79.2(3) . 1_556 ? O23 Pb2 O12 150.1(3) 1_545 1_556 ? O23 Pb2 O12 105.2(3) 4_575 1_556 ? O21 Pb2 O12 62.5(3) 3_667 1_556 ? O11 Pb2 O12 119.7(3) 3_666 1_556 ? O11 Pb2 O12 111.6(4) 1_546 1_556 ? O11 Pb2 O12 51.6(4) 1_556 1_556 ? OH4 Pb2 O12 79.2(3) . 4_566 ? O23 Pb2 O12 105.2(3) 1_545 4_566 ? O23 Pb2 O12 150.1(3) 4_575 4_566 ? O21 Pb2 O12 62.5(3) 3_667 4_566 ? O11 Pb2 O12 119.7(3) 3_666 4_566 ? O11 Pb2 O12 51.6(4) 1_546 4_566 ? O11 Pb2 O12 111.6(4) 1_556 4_566 ? O12 Pb2 O12 61.3(4) 1_556 4_566 ? OH4 Pb2 S1 97.3(2) . 1_546 ? O23 Pb2 S1 91.4(2) 1_545 1_546 ? O23 Pb2 S1 162.9(2) 4_575 1_546 ? O21 Pb2 S1 58.67(13) 3_667 1_546 ? O11 Pb2 S1 96.7(2) 3_666 1_546 ? O11 Pb2 S1 26.7(3) 1_546 1_546 ? O11 Pb2 S1 129.0(3) 1_556 1_546 ? O12 Pb2 S1 85.1(2) 1_556 1_546 ? O12 Pb2 S1 27.7(2) 4_566 1_546 ? OH4 Pb2 Se1 97.3(2) . 1_546 ? O23 Pb2 Se1 91.4(2) 1_545 1_546 ? O23 Pb2 Se1 162.9(2) 4_575 1_546 ? O21 Pb2 Se1 58.67(13) 3_667 1_546 ? O11 Pb2 Se1 96.7(2) 3_666 1_546 ? O11 Pb2 Se1 26.7(3) 1_546 1_546 ? O11 Pb2 Se1 129.0(3) 1_556 1_546 ? O12 Pb2 Se1 85.1(2) 1_556 1_546 ? O12 Pb2 Se1 27.7(2) 4_566 1_546 ? S1 Pb2 Se1 0.00(8) 1_546 1_546 ? OH4 Pb2 S1 97.3(2) . 1_556 ? O23 Pb2 S1 162.9(2) 1_545 1_556 ? O23 Pb2 S1 91.4(2) 4_575 1_556 ? O21 Pb2 S1 58.67(13) 3_667 1_556 ? O11 Pb2 S1 96.7(2) 3_666 1_556 ? O11 Pb2 S1 129.0(3) 1_546 1_556 ? O11 Pb2 S1 26.7(3) 1_556 1_556 ? O12 Pb2 S1 27.7(2) 1_556 1_556 ? O12 Pb2 S1 85.1(2) 4_566 1_556 ? S1 Pb2 S1 103.33(7) 1_546 1_556 ? Se1 Pb2 S1 103.33(7) 1_546 1_556 ? OH4 Pb2 Se1 97.3(2) . 1_556 ? O23 Pb2 Se1 162.9(2) 1_545 1_556 ? O23 Pb2 Se1 91.4(2) 4_575 1_556 ? O21 Pb2 Se1 58.67(13) 3_667 1_556 ? O11 Pb2 Se1 96.7(2) 3_666 1_556 ? O11 Pb2 Se1 129.0(3) 1_546 1_556 ? O11 Pb2 Se1 26.7(3) 1_556 1_556 ? O12 Pb2 Se1 27.7(2) 1_556 1_556 ? O12 Pb2 Se1 85.1(2) 4_566 1_556 ? S1 Pb2 Se1 103.33(7) 1_546 1_556 ? Se1 Pb2 Se1 103.33(7) 1_546 1_556 ? S1 Pb2 Se1 0.00(9) 1_556 1_556 ? OH4 Pb2 Cu 28.44(19) . 3_656 ? O23 Pb2 Cu 44.7(2) 1_545 3_656 ? O23 Pb2 Cu 75.4(2) 4_575 3_656 ? O21 Pb2 Cu 144.9(2) 3_667 3_656 ? O11 Pb2 Cu 134.8(3) 3_666 3_656 ? O11 Pb2 Cu 79.1(4) 1_546 3_656 ? O11 Pb2 Cu 124.1(4) 1_556 3_656 ? O12 Pb2 Cu 105.4(2) 1_556 3_656 ? O12 Pb2 Cu 82.65(19) 4_566 3_656 ? S1 Pb2 Cu 88.75(5) 1_546 3_656 ? Se1 Pb2 Cu 88.75(5) 1_546 3_656 ? S1 Pb2 Cu 125.72(5) 1_556 3_656 ? Se1 Pb2 Cu 125.72(5) 1_556 3_656 ? OH4 Pb2 Cu 28.44(19) . 2_656 ? O23 Pb2 Cu 75.4(2) 1_545 2_656 ? O23 Pb2 Cu 44.7(2) 4_575 2_656 ? O21 Pb2 Cu 144.9(2) 3_667 2_656 ? O11 Pb2 Cu 134.8(3) 3_666 2_656 ? O11 Pb2 Cu 124.1(4) 1_546 2_656 ? O11 Pb2 Cu 79.1(4) 1_556 2_656 ? O12 Pb2 Cu 82.65(19) 1_556 2_656 ? O12 Pb2 Cu 105.40(19) 4_566 2_656 ? S1 Pb2 Cu 125.72(5) 1_546 2_656 ? Se1 Pb2 Cu 125.72(5) 1_546 2_656 ? S1 Pb2 Cu 88.75(5) 1_556 2_656 ? Se1 Pb2 Cu 88.75(5) 1_556 2_656 ? Cu Pb2 Cu 45.41(6) 3_656 2_656 ? OH4 Pb2 S1 133.7(3) . 3_666 ? O23 Pb2 S1 71.3(2) 1_545 3_666 ? O23 Pb2 S1 71.3(2) 4_575 3_666 ? O21 Pb2 S1 91.4(3) 3_667 3_666 ? O11 Pb2 S1 23.7(3) 3_666 3_666 ? O11 Pb2 S1 91.6(3) 1_546 3_666 ? O11 Pb2 S1 91.6(3) 1_556 3_666 ? O12 Pb2 S1 137.4(2) 1_556 3_666 ? O12 Pb2 S1 137.4(2) 4_566 3_666 ? S1 Pb2 S1 110.53(4) 1_546 3_666 ? Se1 Pb2 S1 110.53(4) 1_546 3_666 ? S1 Pb2 S1 110.53(4) 1_556 3_666 ? Se1 Pb2 S1 110.53(4) 1_556 3_666 ? Cu Pb2 S1 113.99(5) 3_656 3_666 ? Cu Pb2 S1 113.99(5) 2_656 3_666 ? OH3 Cu OH1 178.5(6) 3_666 1_645 ? OH3 Cu OH4 95.6(4) 3_666 3_656 ? OH1 Cu OH4 84.6(4) 1_645 3_656 ? OH3 Cu OH2 84.1(4) 3_666 1_655 ? OH1 Cu OH2 95.8(4) 1_645 1_655 ? OH4 Cu OH2 176.3(6) 3_656 1_655 ? OH3 Cu O23 86.0(5) 3_666 3_666 ? OH1 Cu O23 92.6(5) 1_645 3_666 ? OH4 Cu O23 82.3(5) 3_656 3_666 ? OH2 Cu O23 101.3(5) 1_655 3_666 ? OH3 Cu O12 91.2(5) 3_666 4_665 ? OH1 Cu O12 90.2(5) 1_645 4_665 ? OH4 Cu O12 99.2(5) 3_656 4_665 ? OH2 Cu O12 77.2(5) 1_655 4_665 ? O23 Cu O12 176.9(4) 3_666 4_665 ? OH3 Cu Cu 137.7(3) 3_666 4 ? OH1 Cu Cu 42.7(3) 1_645 4 ? OH4 Cu Cu 43.1(3) 3_656 4 ? OH2 Cu Cu 136.4(3) 1_655 4 ? O23 Cu Cu 94.7(3) 3_666 4 ? O12 Cu Cu 88.2(2) 4_665 4 ? OH3 Cu Cu 42.3(3) 3_666 4_565 ? OH1 Cu Cu 137.3(3) 1_645 4_565 ? OH4 Cu Cu 136.9(3) 3_656 4_565 ? OH2 Cu Cu 43.6(3) 1_655 4_565 ? O23 Cu Cu 85.3(3) 3_666 4_565 ? O12 Cu Cu 91.8(2) 4_665 4_565 ? Cu Cu Cu 179.999(1) 4 4_565 ? OH3 Cu Pb1 93.1(4) 3_666 1_655 ? OH1 Cu Pb1 87.7(4) 1_645 1_655 ? OH4 Cu Pb1 140.4(4) 3_656 1_655 ? OH2 Cu Pb1 36.1(4) 1_655 1_655 ? O23 Cu Pb1 136.9(3) 3_666 1_655 ? O12 Cu Pb1 42.0(2) 4_665 1_655 ? Cu Cu Pb1 113.44(3) 4 1_655 ? Cu Cu Pb1 66.56(3) 4_565 1_655 ? OH3 Cu S2 76.5(4) 3_666 3_666 ? OH1 Cu S2 102.1(4) 1_645 3_666 ? OH4 Cu S2 99.6(4) 3_656 3_666 ? OH2 Cu S2 83.9(4) 1_655 3_666 ? O23 Cu S2 19.1(3) 3_666 3_666 ? O12 Cu S2 158.4(2) 4_665 3_666 ? Cu Cu S2 112.90(5) 4 3_666 ? Cu Cu S2 67.10(4) 4_565 3_666 ? Pb1 Cu S2 119.94(8) 1_655 3_666 ? O11 Se1 O12 99.2(5) . . ? O11 Se1 O12 99.2(5) . 4_575 ? O12 Se1 O12 103.6(7) . 4_575 ? O11 Se1 Pb1 124.42(6) . . ? O12 Se1 Pb1 39.2(3) . . ? O12 Se1 Pb1 121.2(4) 4_575 . ? O11 Se1 Pb1 124.42(6) . 1_565 ? O12 Se1 Pb1 121.2(4) . 1_565 ? O12 Se1 Pb1 39.2(3) 4_575 1_565 ? Pb1 Se1 Pb1 110.66(7) . 1_565 ? O11 Se1 Pb2 52.55(11) . 1_554 ? O12 Se1 Pb2 53.6(3) . 1_554 ? O12 Se1 Pb2 129.8(3) 4_575 1_554 ? Pb1 Se1 Pb2 71.98(3) . 1_554 ? Pb1 Se1 Pb2 168.78(8) 1_565 1_554 ? O11 Se1 Pb2 52.55(11) . 1_564 ? O12 Se1 Pb2 129.8(3) . 1_564 ? O12 Se1 Pb2 53.6(3) 4_575 1_564 ? Pb1 Se1 Pb2 168.78(8) . 1_564 ? Pb1 Se1 Pb2 71.98(3) 1_565 1_564 ? Pb2 Se1 Pb2 103.32(7) 1_554 1_564 ? O11 Se1 Pb2 44.2(7) . 3_666 ? O12 Se1 Pb2 122.0(3) . 3_666 ? O12 Se1 Pb2 122.0(4) 4_575 3_666 ? Pb1 Se1 Pb2 116.76(4) . 3_666 ? Pb1 Se1 Pb2 116.76(4) 1_565 3_666 ? Pb2 Se1 Pb2 69.47(4) 1_554 3_666 ? Pb2 Se1 Pb2 69.47(4) 1_564 3_666 ? O11 Se1 Cu 109.7(6) . 1_465 ? O12 Se1 Cu 73.0(3) . 1_465 ? O12 Se1 Cu 31.2(3) 4_575 1_465 ? Pb1 Se1 Cu 92.77(6) . 1_465 ? Pb1 Se1 Cu 57.20(4) 1_565 1_465 ? Pb2 Se1 Cu 112.32(6) 1_554 1_465 ? Pb2 Se1 Cu 79.46(5) 1_564 1_465 ? Pb2 Se1 Cu 148.04(6) 3_666 1_465 ? O11 Se1 Cu 109.7(6) . 4_465 ? O12 Se1 Cu 31.2(3) . 4_465 ? O12 Se1 Cu 73.0(3) 4_575 4_465 ? Pb1 Se1 Cu 57.20(4) . 4_465 ? Pb1 Se1 Cu 92.77(6) 1_565 4_465 ? Pb2 Se1 Cu 79.46(5) 1_554 4_465 ? Pb2 Se1 Cu 112.32(6) 1_564 4_465 ? Pb2 Se1 Cu 148.04(6) 3_666 4_465 ? Cu Se1 Cu 42.04(6) 1_465 4_465 ? O11 Se1 Pb1 125.1(7) . 3_666 ? O12 Se1 Pb1 113.4(3) . 3_666 ? O12 Se1 Pb1 113.4(3) 4_575 3_666 ? Pb1 Se1 Pb1 74.19(4) . 3_666 ? Pb1 Se1 Pb1 74.19(4) 1_565 3_666 ? Pb2 Se1 Pb1 116.75(5) 1_554 3_666 ? Pb2 Se1 Pb1 116.75(5) 1_564 3_666 ? Pb2 Se1 Pb1 80.95(5) 3_666 3_666 ? Cu Se1 Pb1 121.19(6) 1_465 3_666 ? Cu Se1 Pb1 121.19(6) 4_465 3_666 ? O21 S2 O23 110.5(6) . 4_575 ? O21 S2 O23 110.5(6) . . ? O23 S2 O23 110.6(9) 4_575 . ? O21 S2 O22 108.1(9) . . ? O23 S2 O22 108.5(6) 4_575 . ? O23 S2 O22 108.5(6) . . ? O21 S2 Cu 139.9(5) . 3_666 ? O23 S2 Cu 79.7(5) 4_575 3_666 ? O23 S2 Cu 35.1(5) . 3_666 ? O22 S2 Cu 104.5(6) . 3_666 ? O21 S2 Cu 139.9(5) . 2_656 ? O23 S2 Cu 35.1(5) 4_575 2_656 ? O23 S2 Cu 79.7(5) . 2_656 ? O22 S2 Cu 104.5(6) . 2_656 ? Cu S2 Cu 45.79(9) 3_666 2_656 ? O21 S2 Pb1 38.3(6) . 3_666 ? O23 S2 Pb1 123.6(5) 4_575 3_666 ? O23 S2 Pb1 123.6(5) . 3_666 ? O22 S2 Pb1 69.8(7) . 3_666 ? Cu S2 Pb1 156.70(6) 3_666 3_666 ? Cu S2 Pb1 156.70(6) 2_656 3_666 ? O21 S2 Pb1 99.7(4) . . ? O23 S2 Pb1 66.8(4) 4_575 . ? O23 S2 Pb1 147.7(5) . . ? O22 S2 Pb1 49.02(8) . . ? Cu S2 Pb1 119.33(14) 3_666 . ? Cu S2 Pb1 84.44(8) 2_656 . ? Pb1 S2 Pb1 74.88(9) 3_666 . ? O21 S2 Pb1 99.7(4) . 1_565 ? O23 S2 Pb1 147.7(5) 4_575 1_565 ? O23 S2 Pb1 66.8(4) . 1_565 ? O22 S2 Pb1 49.02(7) . 1_565 ? Cu S2 Pb1 84.44(8) 3_666 1_565 ? Cu S2 Pb1 119.33(14) 2_656 1_565 ? Pb1 S2 Pb1 74.88(9) 3_666 1_565 ? Pb1 S2 Pb1 97.89(13) . 1_565 ? O21 S2 Pb2 82.4(4) . 1_565 ? O23 S2 Pb2 110.1(5) 4_575 1_565 ? O23 S2 Pb2 31.3(4) . 1_565 ? O22 S2 Pb2 132.79(10) . 1_565 ? Cu S2 Pb2 58.17(7) 3_666 1_565 ? Cu S2 Pb2 92.29(12) 2_656 1_565 ? Pb1 S2 Pb2 108.23(11) 3_666 1_565 ? Pb1 S2 Pb2 176.68(15) . 1_565 ? Pb1 S2 Pb2 84.19(3) 1_565 1_565 ? O21 S2 Pb2 82.4(4) . . ? O23 S2 Pb2 31.3(4) 4_575 . ? O23 S2 Pb2 110.1(5) . . ? O22 S2 Pb2 132.79(10) . . ? Cu S2 Pb2 92.29(12) 3_666 . ? Cu S2 Pb2 58.17(7) 2_656 . ? Pb1 S2 Pb2 108.23(11) 3_666 . ? Pb1 S2 Pb2 84.19(3) . . ? Pb1 S2 Pb2 176.68(15) 1_565 . ? Pb2 S2 Pb2 93.62(12) 1_565 . ? O21 S2 Pb2 26.6(6) . 3_667 ? O23 S2 Pb2 96.4(5) 4_575 3_667 ? O23 S2 Pb2 96.4(5) . 3_667 ? O22 S2 Pb2 134.8(7) . 3_667 ? Cu S2 Pb2 116.98(14) 3_666 3_667 ? Cu S2 Pb2 116.98(14) 2_656 3_667 ? Pb1 S2 Pb2 64.96(9) 3_666 3_667 ? Pb1 S2 Pb2 115.83(10) . 3_667 ? Pb1 S2 Pb2 115.83(10) 1_565 3_667 ? Pb2 S2 Pb2 65.22(8) 1_565 3_667 ? Pb2 S2 Pb2 65.22(8) . 3_667 ? Se1 O11 Pb2 112.2(8) . 3_666 ? Se1 O11 Pb2 100.7(3) . 1_554 ? Pb2 O11 Pb2 94.0(4) 3_666 1_554 ? Se1 O11 Pb2 100.7(3) . 1_564 ? Pb2 O11 Pb2 94.0(4) 3_666 1_564 ? Pb2 O11 Pb2 152.2(6) 1_554 1_564 ? Se1 O12 Pb1 114.1(5) . . ? Se1 O12 Cu 129.5(5) . 4_465 ? Pb1 O12 Cu 90.1(3) . 4_465 ? Se1 O12 Pb2 98.7(4) . 1_554 ? Pb1 O12 Pb2 101.8(4) . 1_554 ? Cu O12 Pb2 119.9(4) 4_465 1_554 ? Se1 O12 Cu 81.8(4) . 1_465 ? Pb1 O12 Cu 117.9(3) . 1_465 ? Cu O12 Cu 47.91(18) 4_465 1_465 ? Pb2 O12 Cu 136.4(3) 1_554 1_465 ? Se1 O12 Cu 173.1(5) . 1_455 ? Pb1 O12 Cu 63.2(2) . 1_455 ? Cu O12 Cu 46.05(17) 4_465 1_455 ? Pb2 O12 Cu 88.1(2) 1_554 1_455 ? Cu O12 Cu 94.0(2) 1_465 1_455 ? S2 O21 Pb2 139.9(9) . 3_667 ? S2 O21 Pb1 122.8(8) . 3_666 ? Pb2 O21 Pb1 97.3(5) 3_667 3_666 ? S2 O21 Pb2 76.5(4) . 1_565 ? Pb2 O21 Pb2 75.8(3) 3_667 1_565 ? Pb1 O21 Pb2 132.87(18) 3_666 1_565 ? S2 O21 Pb2 76.5(4) . . ? Pb2 O21 Pb2 75.8(3) 3_667 . ? Pb1 O21 Pb2 132.87(18) 3_666 . ? Pb2 O21 Pb2 91.3(3) 1_565 . ? S2 O22 Pb1 109.0(2) . . ? S2 O22 Pb1 109.0(2) . 1_565 ? Pb1 O22 Pb1 141.6(5) . 1_565 ? S2 O22 Pb1 86.9(7) . 3_666 ? Pb1 O22 Pb1 88.4(3) . 3_666 ? Pb1 O22 Pb1 88.4(3) 1_565 3_666 ? S2 O22 Cu 125.6(7) . 4_465 ? Pb1 O22 Cu 60.2(2) . 4_465 ? Pb1 O22 Cu 100.6(3) 1_565 4_465 ? Pb1 O22 Cu 139.4(4) 3_666 4_465 ? S2 O22 Cu 125.6(7) . 1_465 ? Pb1 O22 Cu 100.6(3) . 1_465 ? Pb1 O22 Cu 60.2(2) 1_565 1_465 ? Pb1 O22 Cu 139.4(4) 3_666 1_465 ? Cu O22 Cu 42.27(17) 4_465 1_465 ? S2 O23 Cu 125.8(7) . 3_666 ? S2 O23 Pb2 132.6(6) . 1_565 ? Cu O23 Pb2 87.0(3) 3_666 1_565 ? S2 O23 Pb1 90.2(5) . 1_565 ? Cu O23 Pb1 110.1(3) 3_666 1_565 ? Pb2 O23 Pb1 111.2(4) 1_565 1_565 ? S2 O23 Cu 77.1(5) . 2_656 ? Cu O23 Cu 50.2(2) 3_666 2_656 ? Pb2 O23 Cu 114.9(3) 1_565 2_656 ? Pb1 O23 Cu 127.2(3) 1_565 2_656 ? S2 O23 Cu 164.5(6) . 2_666 ? Cu O23 Cu 45.06(19) 3_666 2_666 ? Pb2 O23 Cu 62.9(2) 1_565 2_666 ? Pb1 O23 Cu 83.6(2) 1_565 2_666 ? Cu O23 Cu 95.3(2) 2_656 2_666 ? Cu OH1 Cu 94.6(6) 1_465 4_465 ? Cu OH1 Cu 108.4(3) 1_465 3_666 ? Cu OH1 Cu 151.2(5) 4_465 3_666 ? Cu OH1 Cu 151.2(5) 1_465 2_656 ? Cu OH1 Cu 108.4(3) 4_465 2_656 ? Cu OH1 Cu 44.81(18) 3_666 2_656 ? Cu OH1 Pb1 126.7(6) 1_465 . ? Cu OH1 Pb1 63.4(3) 4_465 . ? Cu OH1 Pb1 112.0(3) 3_666 . ? Cu OH1 Pb1 80.36(18) 2_656 . ? Cu OH1 Pb1 63.4(3) 1_465 1_565 ? Cu OH1 Pb1 126.7(6) 4_465 1_565 ? Cu OH1 Pb1 80.36(18) 3_666 1_565 ? Cu OH1 Pb1 112.0(3) 2_656 1_565 ? Pb1 OH1 Pb1 90.7(3) . 1_565 ? Cu OH1 Pb1 104.5(5) 1_465 3_566 ? Cu OH1 Pb1 104.5(5) 4_465 3_566 ? Cu OH1 Pb1 53.7(2) 3_666 3_566 ? Cu OH1 Pb1 53.7(2) 2_656 3_566 ? Pb1 OH1 Pb1 127.2(2) . 3_566 ? Pb1 OH1 Pb1 127.2(2) 1_565 3_566 ? Cu OH1 H1 95(10) 1_465 . ? Cu OH1 H1 95(10) 4_465 . ? Cu OH1 H1 99(10) 3_666 . ? Cu OH1 H1 99(10) 2_656 . ? Pb1 OH1 H1 45.3(4) . . ? Pb1 OH1 H1 45.3(3) 1_565 . ? Pb1 OH1 H1 150(10) 3_566 . ? Cu OH2 Cu 92.7(6) 4_465 1_455 ? Cu OH2 Pb1 113.7(5) 4_465 . ? Cu OH2 Pb1 113.7(5) 1_455 . ? Cu OH2 Cu 99.6(3) 4_465 2_656 ? Cu OH2 Cu 133.1(5) 1_455 2_656 ? Pb1 OH2 Cu 102.2(4) . 2_656 ? Cu OH2 Cu 133.1(5) 4_465 3_656 ? Cu OH2 Cu 99.6(3) 1_455 3_656 ? Pb1 OH2 Cu 102.2(4) . 3_656 ? Cu OH2 Cu 41.92(15) 2_656 3_656 ? Cu OH2 H2 117(10) 4_465 . ? Cu OH2 H2 117(10) 1_455 . ? Pb1 OH2 H2 103(10) . . ? Cu OH2 H2 20.96(9) 2_656 . ? Cu OH2 H2 20.96(12) 3_656 . ? Cu OH3 Cu 95.5(6) 3_666 2_656 ? Cu OH3 Cu 105.2(3) 3_666 1_466 ? Cu OH3 Cu 146.2(5) 2_656 1_466 ? Cu OH3 Cu 146.2(5) 3_666 4_466 ? Cu OH3 Cu 105.2(3) 2_656 4_466 ? Cu OH3 Cu 45.15(19) 1_466 4_466 ? Cu OH3 Pb2 134.3(6) 3_666 . ? Cu OH3 Pb2 68.2(2) 2_656 . ? Cu OH3 Pb2 111.3(3) 1_466 . ? Cu OH3 Pb2 78.94(18) 4_466 . ? Cu OH3 Pb2 68.2(2) 3_666 1_565 ? Cu OH3 Pb2 134.3(6) 2_656 1_565 ? Cu OH3 Pb2 78.94(18) 1_466 1_565 ? Cu OH3 Pb2 111.3(3) 4_466 1_565 ? Pb2 OH3 Pb2 92.6(3) . 1_565 ? Cu OH3 Pb1 59.4(3) 3_666 3_566 ? Cu OH3 Pb1 59.4(3) 2_656 3_566 ? Cu OH3 Pb1 109.2(3) 1_466 3_566 ? Cu OH3 Pb1 109.2(3) 4_466 3_566 ? Pb2 OH3 Pb1 127.3(2) . 3_566 ? Pb2 OH3 Pb1 127.3(2) 1_565 3_566 ? Cu OH3 H3 115(10) 3_666 . ? Cu OH3 H3 115(10) 2_656 . ? Cu OH3 H3 81(10) 1_466 . ? Cu OH3 H3 81(10) 4_466 . ? Pb2 OH3 H3 49(5) . . ? Pb2 OH3 H3 49(5) 1_565 . ? Pb1 OH3 H3 169(10) 3_566 . ? Cu OH4 Cu 93.7(6) 2_656 3_656 ? Cu OH4 Pb2 115.8(5) 2_656 . ? Cu OH4 Pb2 115.8(5) 3_656 . ? Cu OH4 Cu 98.7(3) 2_656 4_466 ? Cu OH4 Cu 133.3(6) 3_656 4_466 ? Pb2 OH4 Cu 98.7(4) . 4_466 ? Cu OH4 Cu 133.3(6) 2_656 1_456 ? Cu OH4 Cu 98.7(3) 3_656 1_456 ? Pb2 OH4 Cu 98.7(4) . 1_456 ? Cu OH4 Cu 43.03(16) 4_466 1_456 ? Cu OH4 H4 119(9) 2_656 . ? Cu OH4 H4 119(9) 3_656 . ? Pb2 OH4 H4 95(10) . . ? Cu OH4 H4 22(3) 4_466 . ? Cu OH4 H4 22(3) 1_456 . ? 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 O22 0.90(3) 2.04(14) 2.85(2) 150(23) . OH2 H2 OH1 0.90(3) 1.72(9) 2.58(2) 161(24) 3_566 OH3 H3 O11 0.90(3) 2.29(6) 3.18(2) 170(23) 1_556 OH4 H4 OH3 0.90(3) 1.80(13) 2.62(2) 150(23) 3_567 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 20.79 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.038 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.241