data_boojumite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'boojumite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H2 O15 Pb8 S6' _chemical_formula_weight 2091.90 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' 'Pb' 'Pb' -3.3944 10.1111 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_H-M_alt 'P n m a' _space_group_name_Hall '-P 2ac 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 14.0103(8) _cell_length_b 20.5529(10) _cell_length_c 7.2668(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2092.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6747 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_density_diffrn 6.640 _exptl_crystal_F_000 3496 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.025 _exptl_absorpt_coefficient_mu 64.780 _shelx_estimated_absorpt_T_min 0.093 _shelx_estimated_absorpt_T_max 0.294 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.240 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 9087 _diffrn_reflns_av_unetI/netI 0.1164 _diffrn_reflns_av_R_equivalents 0.2031 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.072 _diffrn_reflns_theta_max 25.023 _diffrn_reflns_theta_full 25.023 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_point_group_measured_fraction_full 0.984 _reflns_number_total 1878 _reflns_number_gt 1538 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_extinction_coef 0.00003(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1878 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.27081(9) 0.750000 0.07748(17) 0.0169(4) Uani 1 2 d S T P . . Pb2 Pb 0.40233(7) 0.55989(4) 0.49933(13) 0.0192(3) Uani 1 1 d . . . . . Pb3 Pb 0.50454(10) 0.750000 0.38327(17) 0.0192(4) Uani 1 2 d S T P . . Pb4 Pb 0.61938(7) 0.62592(4) 0.68977(12) 0.0200(3) Uani 1 1 d . . . . . Pb5 Pb 0.63260(7) 0.59774(5) 0.21233(13) 0.0203(3) Uani 1 1 d . . . . . S1 S 0.3859(5) 0.5829(3) 0.9994(9) 0.0222(14) Uani 1 1 d . . . . . S1A S 0.2990(5) 0.5204(3) 0.1289(9) 0.0295(16) Uani 1 1 d . . . . . S2 S 0.7373(7) 0.750000 0.9729(11) 0.023(2) Uani 1 2 d S T P . . S2A S 0.5961(8) 0.750000 0.9719(14) 0.035(2) Uani 1 2 d S T P . . O1 O 0.4466(13) 0.6119(9) 0.140(2) 0.030(4) Uani 1 1 d . . . . . O2 O 0.3278(15) 0.6316(9) 0.902(3) 0.040(5) Uani 1 1 d . . . . . O3 O 0.4410(15) 0.5445(8) 0.864(3) 0.036(5) Uani 1 1 d . . . . . O4 O 0.768(2) 0.750000 0.782(3) 0.030(6) Uani 1 2 d S T P . . O5 O 0.7701(13) 0.6918(8) 0.071(3) 0.031(4) Uani 1 1 d . . . . . O6 O 0.5605(13) 0.5534(6) 0.472(2) 0.020(4) Uani 1 1 d . . . . . O7 O 0.6440(12) 0.6808(7) 0.429(2) 0.018(4) Uiso 1 1 d . . . . . OH8 O 0.4743(14) 0.6701(7) 0.616(2) 0.027(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0130(8) 0.0210(6) 0.0166(7) 0.000 -0.0001(5) 0.000 Pb2 0.0156(6) 0.0201(5) 0.0219(6) 0.0009(4) -0.0002(4) -0.0002(4) Pb3 0.0181(8) 0.0180(6) 0.0215(7) 0.000 -0.0032(6) 0.000 Pb4 0.0240(6) 0.0198(5) 0.0162(6) 0.0021(4) -0.0035(4) -0.0008(4) Pb5 0.0218(6) 0.0218(6) 0.0173(5) -0.0014(4) 0.0029(4) -0.0007(4) S1 0.024(4) 0.021(3) 0.022(3) 0.003(3) 0.001(3) 0.008(3) S1A 0.026(4) 0.033(3) 0.029(4) -0.004(3) 0.005(3) -0.005(3) S2 0.030(6) 0.027(4) 0.011(4) 0.000 -0.007(4) 0.000 S2A 0.027(7) 0.040(5) 0.037(6) 0.000 -0.003(5) 0.000 O1 0.020(11) 0.048(10) 0.022(9) 0.008(9) 0.000(8) -0.020(9) O2 0.032(13) 0.045(11) 0.045(12) 0.010(10) 0.009(10) 0.030(10) O3 0.045(14) 0.034(9) 0.029(11) -0.001(9) 0.008(10) 0.028(9) O4 0.05(2) 0.031(14) 0.007(11) 0.000 0.000(12) 0.000 O5 0.009(10) 0.044(11) 0.039(11) 0.017(9) 0.000(8) 0.005(8) O6 0.017(10) 0.009(7) 0.035(10) 0.001(7) 0.004(8) -0.001(6) OH8 0.042(13) 0.013(8) 0.027(10) 0.002(8) 0.000(9) 0.001(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 Pb1 O7 2.277(16) 8_556 ? Pb1 O7 2.277(16) 2_465 ? Pb1 O4 2.62(2) 2_465 ? Pb1 O5 2.82(2) 2_465 ? Pb1 O5 2.82(2) 8_556 ? Pb1 O2 2.862(18) 1_554 ? Pb1 O2 2.862(18) 7_574 ? Pb1 S2 3.301(8) 2_466 ? Pb1 Pb3 3.7414(19) 2_465 ? Pb1 O1 3.785(19) . ? Pb1 O1 3.785(19) 7_575 ? Pb1 S1 3.836(6) 7_574 ? Pb2 O6 2.230(19) . ? Pb2 O6 2.395(13) 5_666 ? Pb2 OH8 2.620(16) . ? Pb2 O3 2.723(19) . ? Pb2 O1 2.890(17) . ? Pb2 S1A 3.162(7) . ? Pb2 O5 3.324(17) 8_556 ? Pb2 S1A 3.401(7) 4_565 ? Pb2 O2 3.436(19) . ? Pb2 Pb4 3.6060(14) . ? Pb2 S1 3.671(6) 1_554 ? Pb2 S1 3.672(6) . ? Pb3 OH8 2.394(15) 7_575 ? Pb3 OH8 2.394(16) . ? Pb3 O7 2.439(16) 7_575 ? Pb3 O7 2.439(16) . ? Pb3 S2A 3.252(11) 1_554 ? Pb3 O1 3.442(17) . ? Pb3 O1 3.442(17) 7_575 ? Pb3 O5 3.511(18) 8_556 ? Pb3 O5 3.511(18) 2_465 ? Pb3 Pb4 3.7487(13) 7_575 ? Pb3 Pb4 3.7487(13) . ? Pb4 O7 2.231(16) . ? Pb4 OH8 2.290(18) . ? Pb4 O6 2.327(16) . ? Pb4 O2 3.00(2) 8_657 ? Pb4 O3 3.26(2) . ? Pb4 S2A 3.289(7) . ? Pb4 O4 3.360(18) . ? Pb4 S1A 3.476(7) 5_666 ? Pb4 Pb5 3.5223(13) . ? Pb4 S2 3.669(6) . ? Pb4 O5 3.739(19) 1_556 ? Pb5 O6 2.324(16) . ? Pb5 O7 2.329(15) . ? Pb5 O1 2.675(19) . ? Pb5 O5 2.915(18) . ? Pb5 S1A 3.049(7) 8_656 ? Pb5 O3 3.149(19) 5_666 ? Pb5 S1A 3.600(6) 5_665 ? Pb5 S2A 3.620(5) 1_554 ? Pb5 S1 3.799(7) 1_554 ? S1 O1 1.455(18) 1_556 ? S1 O2 1.474(18) . ? S1 O3 1.479(18) . ? S1 S1A 2.005(9) 1_556 ? S2 O4 1.45(2) . ? S2 O5 1.467(17) 7_576 ? S2 O5 1.467(17) 1_556 ? S2 S2A 1.978(15) . ? O2 OH8 3.02(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 O7 Pb1 O7 77.3(8) 8_556 2_465 ? O7 Pb1 O4 88.1(6) 8_556 2_465 ? O7 Pb1 O4 88.1(6) 2_465 2_465 ? O7 Pb1 O5 106.3(5) 8_556 2_465 ? O7 Pb1 O5 75.6(5) 2_465 2_465 ? O4 Pb1 O5 154.9(3) 2_465 2_465 ? O7 Pb1 O5 75.6(5) 8_556 8_556 ? O7 Pb1 O5 106.3(5) 2_465 8_556 ? O4 Pb1 O5 154.9(3) 2_465 8_556 ? O5 Pb1 O5 50.2(7) 2_465 8_556 ? O7 Pb1 O2 71.2(6) 8_556 1_554 ? O7 Pb1 O2 137.7(6) 2_465 1_554 ? O4 Pb1 O2 63.7(4) 2_465 1_554 ? O5 Pb1 O2 140.0(5) 2_465 1_554 ? O5 Pb1 O2 92.6(5) 8_556 1_554 ? O7 Pb1 O2 137.7(6) 8_556 7_574 ? O7 Pb1 O2 71.2(6) 2_465 7_574 ? O4 Pb1 O2 63.7(4) 2_465 7_574 ? O5 Pb1 O2 92.6(5) 2_465 7_574 ? O5 Pb1 O2 140.0(5) 8_556 7_574 ? O2 Pb1 O2 116.4(8) 1_554 7_574 ? O7 Pb1 S2 84.8(4) 8_556 2_466 ? O7 Pb1 S2 84.8(4) 2_465 2_466 ? O4 Pb1 S2 170.9(7) 2_465 2_466 ? O5 Pb1 S2 26.3(3) 2_465 2_466 ? O5 Pb1 S2 26.3(3) 8_556 2_466 ? O2 Pb1 S2 118.8(4) 1_554 2_466 ? O2 Pb1 S2 118.8(4) 7_574 2_466 ? O7 Pb1 Pb3 39.0(4) 8_556 2_465 ? O7 Pb1 Pb3 39.0(4) 2_465 2_465 ? O4 Pb1 Pb3 93.5(6) 2_465 2_465 ? O5 Pb1 Pb3 85.8(4) 2_465 2_465 ? O5 Pb1 Pb3 85.8(4) 8_556 2_465 ? O2 Pb1 Pb3 108.2(4) 1_554 2_465 ? O2 Pb1 Pb3 108.2(4) 7_574 2_465 ? S2 Pb1 Pb3 77.44(18) 2_466 2_465 ? O7 Pb1 O1 92.4(5) 8_556 . ? O7 Pb1 O1 168.2(5) 2_465 . ? O4 Pb1 O1 97.4(5) 2_465 . ? O5 Pb1 O1 102.3(4) 2_465 . ? O5 Pb1 O1 64.9(4) 8_556 . ? O2 Pb1 O1 40.1(5) 1_554 . ? O2 Pb1 O1 120.6(5) 7_574 . ? S2 Pb1 O1 88.5(3) 2_466 . ? Pb3 Pb1 O1 129.8(2) 2_465 . ? O7 Pb1 O1 168.2(5) 8_556 7_575 ? O7 Pb1 O1 92.4(5) 2_465 7_575 ? O4 Pb1 O1 97.4(5) 2_465 7_575 ? O5 Pb1 O1 64.9(4) 2_465 7_575 ? O5 Pb1 O1 102.3(4) 8_556 7_575 ? O2 Pb1 O1 120.6(5) 1_554 7_575 ? O2 Pb1 O1 40.1(5) 7_574 7_575 ? S2 Pb1 O1 88.5(3) 2_466 7_575 ? Pb3 Pb1 O1 129.8(2) 2_465 7_575 ? O1 Pb1 O1 97.2(5) . 7_575 ? O7 Pb1 S1 152.2(4) 8_556 7_574 ? O7 Pb1 S1 76.5(4) 2_465 7_574 ? O4 Pb1 S1 81.9(3) 2_465 7_574 ? O5 Pb1 S1 75.9(3) 2_465 7_574 ? O5 Pb1 S1 121.0(4) 8_556 7_574 ? O2 Pb1 S1 125.3(4) 1_554 7_574 ? O2 Pb1 S1 19.2(4) 7_574 7_574 ? S2 Pb1 S1 101.90(12) 2_466 7_574 ? Pb3 Pb1 S1 115.49(11) 2_465 7_574 ? O1 Pb1 S1 114.6(3) . 7_574 ? O1 Pb1 S1 22.0(3) 7_575 7_574 ? O6 Pb2 O6 74.6(6) . 5_666 ? O6 Pb2 OH8 72.5(5) . . ? O6 Pb2 OH8 136.8(6) 5_666 . ? O6 Pb2 O3 83.3(6) . . ? O6 Pb2 O3 76.0(5) 5_666 . ? OH8 Pb2 O3 73.1(5) . . ? O6 Pb2 O1 74.2(6) . . ? O6 Pb2 O1 113.1(6) 5_666 . ? OH8 Pb2 O1 83.7(5) . . ? O3 Pb2 O1 151.6(6) . . ? O6 Pb2 S1A 111.3(5) . . ? O6 Pb2 S1A 85.7(4) 5_666 . ? OH8 Pb2 S1A 132.3(4) . . ? O3 Pb2 S1A 152.8(5) . . ? O1 Pb2 S1A 54.8(4) . . ? O6 Pb2 O5 126.1(5) . 8_556 ? O6 Pb2 O5 158.1(5) 5_666 8_556 ? OH8 Pb2 O5 63.8(5) . 8_556 ? O3 Pb2 O5 110.9(5) . 8_556 ? O1 Pb2 O5 71.2(5) . 8_556 ? S1A Pb2 O5 79.8(3) . 8_556 ? O6 Pb2 S1A 145.1(4) . 4_565 ? O6 Pb2 S1A 71.6(4) 5_666 4_565 ? OH8 Pb2 S1A 130.5(4) . 4_565 ? O3 Pb2 S1A 80.8(5) . 4_565 ? O1 Pb2 S1A 127.4(4) . 4_565 ? S1A Pb2 S1A 74.42(9) . 4_565 ? O5 Pb2 S1A 88.6(3) 8_556 4_565 ? O6 Pb2 O2 113.9(6) . . ? O6 Pb2 O2 114.1(5) 5_666 . ? OH8 Pb2 O2 58.1(5) . . ? O3 Pb2 O2 44.2(4) . . ? O1 Pb2 O2 132.5(5) . . ? S1A Pb2 O2 134.0(4) . . ? O5 Pb2 O2 67.2(4) 8_556 . ? S1A Pb2 O2 73.8(4) 4_565 . ? O6 Pb2 Pb4 38.6(4) . . ? O6 Pb2 Pb4 98.6(4) 5_666 . ? OH8 Pb2 Pb4 39.3(4) . . ? O3 Pb2 Pb4 60.2(5) . . ? O1 Pb2 Pb4 91.5(3) . . ? S1A Pb2 Pb4 144.02(13) . . ? O5 Pb2 Pb4 102.8(3) 8_556 . ? S1A Pb2 Pb4 140.87(12) 4_565 . ? O2 Pb2 Pb4 76.6(4) . . ? O6 Pb2 S1 88.9(4) . 1_554 ? O6 Pb2 S1 103.1(4) 5_666 1_554 ? OH8 Pb2 S1 103.4(4) . 1_554 ? O3 Pb2 S1 172.1(5) . 1_554 ? O1 Pb2 S1 21.7(3) . 1_554 ? S1A Pb2 S1 33.07(16) . 1_554 ? O5 Pb2 S1 73.0(3) 8_556 1_554 ? S1A Pb2 S1 106.53(16) 4_565 1_554 ? O2 Pb2 S1 140.1(3) . 1_554 ? Pb4 Pb2 S1 112.59(11) . 1_554 ? O6 Pb2 S1 99.2(4) . . ? O6 Pb2 S1 93.0(4) 5_666 . ? OH8 Pb2 S1 66.0(4) . . ? O3 Pb2 S1 20.7(4) . . ? O1 Pb2 S1 149.4(4) . . ? S1A Pb2 S1 147.87(17) . . ? O5 Pb2 S1 90.7(4) 8_556 . ? S1A Pb2 S1 74.72(16) 4_565 . ? O2 Pb2 S1 23.6(3) . . ? Pb4 Pb2 S1 67.95(11) . . ? S1 Pb2 S1 163.52(19) 1_554 . ? OH8 Pb3 OH8 86.6(7) 7_575 . ? OH8 Pb3 O7 69.2(6) 7_575 7_575 ? OH8 Pb3 O7 116.4(6) . 7_575 ? OH8 Pb3 O7 116.4(6) 7_575 . ? OH8 Pb3 O7 69.2(6) . . ? O7 Pb3 O7 71.3(7) 7_575 . ? OH8 Pb3 S2A 135.9(4) 7_575 1_554 ? OH8 Pb3 S2A 135.9(4) . 1_554 ? O7 Pb3 S2A 79.0(4) 7_575 1_554 ? O7 Pb3 S2A 79.0(4) . 1_554 ? OH8 Pb3 O1 152.5(5) 7_575 . ? OH8 Pb3 O1 75.9(5) . . ? O7 Pb3 O1 137.7(5) 7_575 . ? O7 Pb3 O1 77.2(5) . . ? S2A Pb3 O1 67.7(3) 1_554 . ? OH8 Pb3 O1 75.9(5) 7_575 7_575 ? OH8 Pb3 O1 152.5(5) . 7_575 ? O7 Pb3 O1 77.2(5) 7_575 7_575 ? O7 Pb3 O1 137.7(5) . 7_575 ? S2A Pb3 O1 67.7(3) 1_554 7_575 ? O1 Pb3 O1 111.1(6) . 7_575 ? OH8 Pb3 O5 90.1(5) 7_575 8_556 ? OH8 Pb3 O5 62.3(6) . 8_556 ? O7 Pb3 O5 159.2(5) 7_575 8_556 ? O7 Pb3 O5 122.5(4) . 8_556 ? S2A Pb3 O5 117.1(4) 1_554 8_556 ? O1 Pb3 O5 63.1(4) . 8_556 ? O1 Pb3 O5 96.2(4) 7_575 8_556 ? OH8 Pb3 O5 62.3(6) 7_575 2_465 ? OH8 Pb3 O5 90.1(5) . 2_465 ? O7 Pb3 O5 122.5(4) 7_575 2_465 ? O7 Pb3 O5 159.2(5) . 2_465 ? S2A Pb3 O5 117.1(4) 1_554 2_465 ? O1 Pb3 O5 96.2(4) . 2_465 ? O1 Pb3 O5 63.1(4) 7_575 2_465 ? O5 Pb3 O5 39.8(5) 8_556 2_465 ? OH8 Pb3 Pb1 97.0(5) 7_575 2_565 ? OH8 Pb3 Pb1 97.0(5) . 2_565 ? O7 Pb3 Pb1 36.0(4) 7_575 2_565 ? O7 Pb3 Pb1 36.0(4) . 2_565 ? S2A Pb3 Pb1 71.2(2) 1_554 2_565 ? O1 Pb3 Pb1 105.9(3) . 2_565 ? O1 Pb3 Pb1 105.9(3) 7_575 2_565 ? O5 Pb3 Pb1 157.8(3) 8_556 2_565 ? O5 Pb3 Pb1 157.8(3) 2_465 2_565 ? OH8 Pb3 Pb4 35.9(5) 7_575 7_575 ? OH8 Pb3 Pb4 97.1(4) . 7_575 ? O7 Pb3 Pb4 34.8(4) 7_575 7_575 ? O7 Pb3 Pb4 88.4(4) . 7_575 ? S2A Pb3 Pb4 112.14(13) 1_554 7_575 ? O1 Pb3 Pb4 165.4(3) . 7_575 ? O1 Pb3 Pb4 81.1(3) 7_575 7_575 ? O5 Pb3 Pb4 125.3(3) 8_556 7_575 ? O5 Pb3 Pb4 96.6(3) 2_465 7_575 ? Pb1 Pb3 Pb4 61.76(3) 2_565 7_575 ? OH8 Pb3 Pb4 97.1(4) 7_575 . ? OH8 Pb3 Pb4 35.9(5) . . ? O7 Pb3 Pb4 88.4(4) 7_575 . ? O7 Pb3 Pb4 34.8(4) . . ? S2A Pb3 Pb4 112.14(13) 1_554 . ? O1 Pb3 Pb4 81.1(3) . . ? O1 Pb3 Pb4 165.4(3) 7_575 . ? O5 Pb3 Pb4 96.6(3) 8_556 . ? O5 Pb3 Pb4 125.3(3) 2_465 . ? Pb1 Pb3 Pb4 61.76(3) 2_565 . ? Pb4 Pb3 Pb4 85.73(4) 7_575 . ? O7 Pb4 OH8 74.8(6) . . ? O7 Pb4 O6 78.5(5) . . ? OH8 Pb4 O6 77.3(6) . . ? O7 Pb4 O2 69.0(6) . 8_657 ? OH8 Pb4 O2 142.9(6) . 8_657 ? O6 Pb4 O2 102.7(6) . 8_657 ? O7 Pb4 O3 135.0(5) . . ? OH8 Pb4 O3 67.3(5) . . ? O6 Pb4 O3 70.4(5) . . ? O2 Pb4 O3 148.5(5) 8_657 . ? O7 Pb4 S2A 98.8(4) . . ? OH8 Pb4 S2A 75.5(4) . . ? O6 Pb4 S2A 152.4(5) . . ? O2 Pb4 S2A 101.8(4) 8_657 . ? O3 Pb4 S2A 94.6(3) . . ? O7 Pb4 O4 72.0(5) . . ? OH8 Pb4 O4 107.2(5) . . ? O6 Pb4 O4 147.4(6) . . ? O2 Pb4 O4 53.9(5) 8_657 . ? O3 Pb4 O4 141.8(5) . . ? S2A Pb4 O4 49.3(4) . . ? O7 Pb4 S1A 135.1(4) . 5_666 ? OH8 Pb4 S1A 136.4(4) . 5_666 ? O6 Pb4 S1A 79.7(4) . 5_666 ? O2 Pb4 S1A 78.3(4) 8_657 5_666 ? O3 Pb4 S1A 70.2(3) . 5_666 ? S2A Pb4 S1A 117.85(19) . 5_666 ? O4 Pb4 S1A 112.1(4) . 5_666 ? O7 Pb4 Pb5 40.4(4) . . ? OH8 Pb4 Pb5 83.2(4) . . ? O6 Pb4 Pb5 40.7(4) . . ? O2 Pb4 Pb5 74.8(4) 8_657 . ? O3 Pb4 Pb5 109.8(3) . . ? S2A Pb4 Pb5 138.32(15) . . ? O4 Pb4 Pb5 106.8(4) . . ? S1A Pb4 Pb5 102.34(11) 5_666 . ? O7 Pb4 Pb2 89.7(4) . . ? OH8 Pb4 Pb2 46.4(4) . . ? O6 Pb4 Pb2 36.7(4) . . ? O2 Pb4 Pb2 138.7(4) 8_657 . ? O3 Pb4 Pb2 46.4(3) . . ? S2A Pb4 Pb2 116.6(2) . . ? O4 Pb4 Pb2 152.2(4) . . ? S1A Pb4 Pb2 95.58(12) 5_666 . ? Pb5 Pb4 Pb2 66.70(3) . . ? O7 Pb4 S2 93.2(4) . . ? OH8 Pb4 S2 104.8(4) . . ? O6 Pb4 S2 170.6(4) . . ? O2 Pb4 S2 70.0(4) 8_657 . ? O3 Pb4 S2 118.9(4) . . ? S2A Pb4 S2 32.5(2) . . ? O4 Pb4 S2 23.3(4) . . ? S1A Pb4 S2 103.93(15) 5_666 . ? Pb5 Pb4 S2 130.01(14) . . ? Pb2 Pb4 S2 148.90(15) . . ? O7 Pb4 O5 111.0(5) . 1_556 ? OH8 Pb4 O5 122.1(5) . 1_556 ? O6 Pb4 O5 159.6(5) . 1_556 ? O2 Pb4 O5 66.4(5) 8_657 1_556 ? O3 Pb4 O5 109.3(4) . 1_556 ? S2A Pb4 O5 46.6(3) . 1_556 ? O4 Pb4 O5 39.3(4) . 1_556 ? S1A Pb4 O5 81.2(3) 5_666 1_556 ? Pb5 Pb4 O5 139.5(3) . 1_556 ? Pb2 Pb4 O5 153.8(3) . 1_556 ? S2 Pb4 O5 22.8(3) . 1_556 ? O6 Pb5 O7 76.6(5) . . ? O6 Pb5 O1 77.2(6) . . ? O7 Pb5 O1 96.9(6) . . ? O6 Pb5 O5 146.3(6) . . ? O7 Pb5 O5 72.9(5) . . ? O1 Pb5 O5 120.1(5) . . ? O6 Pb5 S1A 79.7(5) . 8_656 ? O7 Pb5 S1A 94.3(4) . 8_656 ? O1 Pb5 S1A 151.2(4) . 8_656 ? O5 Pb5 S1A 88.5(3) . 8_656 ? O6 Pb5 O3 68.7(5) . 5_666 ? O7 Pb5 O3 145.3(5) . 5_666 ? O1 Pb5 O3 75.4(5) . 5_666 ? O5 Pb5 O3 140.4(5) . 5_666 ? S1A Pb5 O3 80.4(4) 8_656 5_666 ? O6 Pb5 Pb4 40.8(4) . . ? O7 Pb5 Pb4 38.4(4) . . ? O1 Pb5 Pb4 97.2(4) . . ? O5 Pb5 Pb4 105.8(4) . . ? S1A Pb5 Pb4 75.72(13) 8_656 . ? O3 Pb5 Pb4 108.0(3) 5_666 . ? O6 Pb5 S1A 114.2(4) . 5_665 ? O7 Pb5 S1A 160.4(4) . 5_665 ? O1 Pb5 S1A 101.3(4) . 5_665 ? O5 Pb5 S1A 91.7(4) . 5_665 ? S1A Pb5 S1A 72.87(9) 8_656 5_665 ? O3 Pb5 S1A 48.7(3) 5_666 5_665 ? Pb4 Pb5 S1A 143.46(12) . 5_665 ? O6 Pb5 S2A 132.0(4) . 1_554 ? O7 Pb5 S2A 72.7(4) . 1_554 ? O1 Pb5 S2A 70.9(4) . 1_554 ? O5 Pb5 S2A 49.5(4) . 1_554 ? S1A Pb5 S2A 137.9(2) 8_656 1_554 ? O3 Pb5 S2A 132.2(4) 5_666 1_554 ? Pb4 Pb5 S2A 109.01(15) . 1_554 ? S1A Pb5 S2A 106.74(19) 5_665 1_554 ? O6 Pb5 S1 84.5(5) . 1_554 ? O7 Pb5 S1 113.4(4) . 1_554 ? O1 Pb5 S1 16.7(4) . 1_554 ? O5 Pb5 S1 120.7(4) . 1_554 ? S1A Pb5 S1 143.91(15) 8_656 1_554 ? O3 Pb5 S1 63.6(4) 5_666 1_554 ? Pb4 Pb5 S1 111.50(10) . 1_554 ? S1A Pb5 S1 84.69(15) 5_665 1_554 ? S2A Pb5 S1 75.17(19) 1_554 1_554 ? O6 Pb5 Pb3 81.6(4) . . ? O7 Pb5 Pb3 37.9(4) . . ? O1 Pb5 Pb3 61.1(4) . . ? O5 Pb5 Pb3 83.2(3) . . ? S1A Pb5 Pb3 131.63(13) 8_656 . ? O3 Pb5 Pb3 131.7(3) 5_666 . ? Pb4 Pb5 Pb3 61.29(3) . . ? S1A Pb5 Pb3 154.49(12) 5_665 . ? S2A Pb5 Pb3 51.80(16) 1_554 . ? S1 Pb5 Pb3 76.73(10) 1_554 . ? O6 Pb5 Pb4 147.0(4) . 1_554 ? O7 Pb5 Pb4 124.1(4) . 1_554 ? O1 Pb5 Pb4 75.0(4) . 1_554 ? O5 Pb5 Pb4 65.5(4) . 1_554 ? S1A Pb5 Pb4 119.27(13) 8_656 1_554 ? O3 Pb5 Pb4 87.1(3) 5_666 1_554 ? Pb4 Pb5 Pb4 160.96(4) . 1_554 ? S1A Pb5 Pb4 55.54(11) 5_665 1_554 ? S2A Pb5 Pb4 52.16(15) 1_554 1_554 ? S1 Pb5 Pb4 64.29(10) 1_554 1_554 ? Pb3 Pb5 Pb4 100.09(3) . 1_554 ? O1 S1 O2 112.5(12) 1_556 . ? O1 S1 O3 112.3(12) 1_556 . ? O2 S1 O3 109.3(11) . . ? O1 S1 S1A 106.7(8) 1_556 1_556 ? O2 S1 S1A 109.1(9) . 1_556 ? O3 S1 S1A 106.7(9) . 1_556 ? O1 S1 Pb2 47.4(7) 1_556 1_556 ? O2 S1 Pb2 126.9(8) . 1_556 ? O3 S1 Pb2 123.8(8) . 1_556 ? S1A S1 Pb2 59.4(2) 1_556 1_556 ? O1 S1 Pb2 135.2(8) 1_556 . ? O2 S1 Pb2 69.2(8) . . ? O3 S1 Pb2 40.5(7) . . ? S1A S1 Pb2 114.8(3) 1_556 . ? Pb2 S1 Pb2 163.52(19) 1_556 . ? O1 S1 Pb5 31.8(8) 1_556 1_556 ? O2 S1 Pb5 130.2(9) . 1_556 ? O3 S1 Pb5 80.7(9) . 1_556 ? S1A S1 Pb5 114.4(3) 1_556 1_556 ? Pb2 S1 Pb5 63.27(11) 1_556 1_556 ? Pb2 S1 Pb5 110.87(17) . 1_556 ? O1 S1 Pb1 77.0(8) 1_556 1_556 ? O2 S1 Pb1 39.7(8) . 1_556 ? O3 S1 Pb1 142.7(8) . 1_556 ? S1A S1 Pb1 104.4(3) 1_556 1_556 ? Pb2 S1 Pb1 89.74(14) 1_556 1_556 ? Pb2 S1 Pb1 106.74(15) . 1_556 ? Pb5 S1 Pb1 104.50(16) 1_556 1_556 ? O1 S1 Pb5 133.1(8) 1_556 5_666 ? O2 S1 Pb5 114.0(9) . 5_666 ? O3 S1 Pb5 44.6(8) . 5_666 ? S1A S1 Pb5 63.2(2) 1_556 5_666 ? Pb2 S1 Pb5 105.27(15) 1_556 5_666 ? Pb2 S1 Pb5 60.47(10) . 5_666 ? Pb5 S1 Pb5 106.74(15) 1_556 5_666 ? Pb1 S1 Pb5 148.73(19) 1_556 5_666 ? O1 S1 Pb4 80.1(7) 1_556 . ? O2 S1 Pb4 91.7(8) . . ? O3 S1 Pb4 47.8(8) . . ? S1A S1 Pb4 152.5(3) 1_556 . ? Pb2 S1 Pb4 121.67(18) 1_556 . ? Pb2 S1 Pb4 55.25(9) . . ? Pb5 S1 Pb4 58.41(10) 1_556 . ? Pb1 S1 Pb4 103.02(15) 1_556 . ? Pb5 S1 Pb4 92.33(13) 5_666 . ? O1 S1 Pb4 133.1(8) 1_556 8_557 ? O2 S1 Pb4 35.3(9) . 8_557 ? O3 S1 Pb4 111.7(9) . 8_557 ? S1A S1 Pb4 75.0(3) 1_556 8_557 ? Pb2 S1 Pb4 114.78(17) 1_556 8_557 ? Pb2 S1 Pb4 75.62(12) . 8_557 ? Pb5 S1 Pb4 162.44(18) 1_556 8_557 ? Pb1 S1 Pb4 58.04(9) 1_556 8_557 ? Pb5 S1 Pb4 90.69(14) 5_666 8_557 ? Pb4 S1 Pb4 120.20(15) . 8_557 ? O1 S1 Pb5 96.7(8) 1_556 8_557 ? O2 S1 Pb5 73.7(8) . 8_557 ? O3 S1 Pb5 145.6(9) . 8_557 ? S1A S1 Pb5 44.6(2) 1_556 8_557 ? Pb2 S1 Pb5 64.00(10) 1_556 8_557 ? Pb2 S1 Pb5 124.41(18) . 8_557 ? Pb5 S1 Pb5 124.68(16) 1_556 8_557 ? Pb1 S1 Pb5 59.87(9) 1_556 8_557 ? Pb5 S1 Pb5 101.91(15) 5_666 8_557 ? Pb4 S1 Pb5 162.77(17) . 8_557 ? Pb4 S1 Pb5 50.82(8) 8_557 8_557 ? S1 S1A Pb5 107.9(3) 1_554 8_556 ? S1 S1A Pb2 87.5(3) 1_554 . ? Pb5 S1A Pb2 83.92(16) 8_556 . ? S1 S1A Pb2 133.2(3) 1_554 4_564 ? Pb5 S1A Pb2 73.94(16) 8_556 4_564 ? Pb2 S1A Pb2 137.7(2) . 4_564 ? S1 S1A Pb4 122.2(3) 1_554 5_666 ? Pb5 S1A Pb4 124.0(2) 8_556 5_666 ? Pb2 S1A Pb4 75.47(15) . 5_666 ? Pb2 S1A Pb4 87.60(15) 4_564 5_666 ? S1 S1A Pb5 87.0(3) 1_554 5_665 ? Pb5 S1A Pb5 144.7(2) 8_556 5_665 ? Pb2 S1A Pb5 129.6(2) . 5_665 ? Pb2 S1A Pb5 72.71(13) 4_564 5_665 ? Pb4 S1A Pb5 65.82(12) 5_666 5_665 ? S1 S1A Pb4 76.4(3) 1_554 8_556 ? Pb5 S1A Pb4 57.43(12) 8_556 8_556 ? Pb2 S1A Pb4 129.31(19) . 8_556 ? Pb2 S1A Pb4 65.54(12) 4_564 8_556 ? Pb4 S1A Pb4 152.2(2) 5_666 8_556 ? Pb5 S1A Pb4 97.62(15) 5_665 8_556 ? O4 S2 O5 111.9(10) . 7_576 ? O4 S2 O5 111.9(10) . 1_556 ? O5 S2 O5 109.1(16) 7_576 1_556 ? O4 S2 S2A 107.1(12) . . ? O5 S2 S2A 108.4(8) 7_576 . ? O5 S2 S2A 108.4(8) 1_556 . ? O4 S2 Pb1 154.5(13) . 2_566 ? O5 S2 Pb1 58.2(8) 7_576 2_566 ? O5 S2 Pb1 58.2(8) 1_556 2_566 ? S2A S2 Pb1 98.4(4) . 2_566 ? O4 S2 Pb4 66.3(8) . 7_575 ? O5 S2 Pb4 81.3(8) 7_576 7_575 ? O5 S2 Pb4 168.8(8) 1_556 7_575 ? S2A S2 Pb4 63.1(3) . 7_575 ? Pb1 S2 Pb4 128.25(17) 2_566 7_575 ? O4 S2 Pb4 66.3(8) . . ? O5 S2 Pb4 168.8(8) 7_576 . ? O5 S2 Pb4 81.3(8) 1_556 . ? S2A S2 Pb4 63.1(3) . . ? Pb1 S2 Pb4 128.25(17) 2_566 . ? Pb4 S2 Pb4 88.06(19) 7_575 . ? O4 S2 Pb5 122.8(3) . 7_576 ? O5 S2 Pb5 40.6(7) 7_576 7_576 ? O5 S2 Pb5 124.0(9) 1_556 7_576 ? S2A S2 Pb5 67.8(2) . 7_576 ? Pb1 S2 Pb5 66.97(13) 2_566 7_576 ? Pb4 S2 Pb5 61.28(8) 7_575 7_576 ? Pb4 S2 Pb5 130.1(3) . 7_576 ? O4 S2 Pb5 122.8(3) . 1_556 ? O5 S2 Pb5 124.0(9) 7_576 1_556 ? O5 S2 Pb5 40.6(7) 1_556 1_556 ? S2A S2 Pb5 67.8(2) . 1_556 ? Pb1 S2 Pb5 66.97(13) 2_566 1_556 ? Pb4 S2 Pb5 130.1(3) 7_575 1_556 ? Pb4 S2 Pb5 61.28(8) . 1_556 ? Pb5 S2 Pb5 108.0(2) 7_576 1_556 ? O4 S2 Pb3 88.3(12) . 2_566 ? O5 S2 Pb3 64.3(8) 7_576 2_566 ? O5 S2 Pb3 64.3(8) 1_556 2_566 ? S2A S2 Pb3 164.6(5) . 2_566 ? Pb1 S2 Pb3 66.21(16) 2_566 2_566 ? Pb4 S2 Pb3 125.75(18) 7_575 2_566 ? Pb4 S2 Pb3 125.75(18) . 2_566 ? Pb5 S2 Pb3 104.13(15) 7_576 2_566 ? Pb5 S2 Pb3 104.13(15) 1_556 2_566 ? O4 S2 Pb1 10.6(12) . 2_565 ? O5 S2 Pb1 116.6(8) 7_576 2_565 ? O5 S2 Pb1 116.6(8) 1_556 2_565 ? S2A S2 Pb1 96.5(4) . 2_565 ? Pb1 S2 Pb1 165.1(3) 2_566 2_565 ? Pb4 S2 Pb1 59.71(11) 7_575 2_565 ? Pb4 S2 Pb1 59.71(11) . 2_565 ? Pb5 S2 Pb1 119.40(13) 7_576 2_565 ? Pb5 S2 Pb1 119.40(13) 1_556 2_565 ? Pb3 S2 Pb1 98.9(2) 2_566 2_565 ? O4 S2 Pb3 149.7(12) . 1_556 ? O5 S2 Pb3 84.4(8) 7_576 1_556 ? O5 S2 Pb3 84.4(8) 1_556 1_556 ? S2A S2 Pb3 42.6(4) . 1_556 ? Pb1 S2 Pb3 55.74(14) 2_566 1_556 ? Pb4 S2 Pb3 92.65(19) 7_575 1_556 ? Pb4 S2 Pb3 92.65(19) . 1_556 ? Pb5 S2 Pb3 54.33(12) 7_576 1_556 ? Pb5 S2 Pb3 54.33(12) 1_556 1_556 ? Pb3 S2 Pb3 121.96(19) 2_566 1_556 ? Pb1 S2 Pb3 139.2(2) 2_565 1_556 ? S2 S2A Pb3 113.0(5) . 1_556 ? S2 S2A Pb4 84.4(3) . 7_575 ? Pb3 S2A Pb4 127.75(16) 1_556 7_575 ? S2 S2A Pb4 84.4(3) . . ? Pb3 S2A Pb4 127.75(16) 1_556 . ? Pb4 S2A Pb4 101.7(3) 7_575 . ? S2 S2A Pb5 81.8(2) . 7_576 ? Pb3 S2A Pb5 67.19(16) 1_556 7_576 ? Pb4 S2A Pb5 67.45(4) 7_575 7_576 ? Pb4 S2A Pb5 163.2(3) . 7_576 ? S2 S2A Pb5 81.8(2) . 1_556 ? Pb3 S2A Pb5 67.19(16) 1_556 1_556 ? Pb4 S2A Pb5 163.2(3) 7_575 1_556 ? Pb4 S2A Pb5 67.45(4) . 1_556 ? Pb5 S2A Pb5 119.6(3) 7_576 1_556 ? S2 S2A Pb1 53.0(3) . 2_566 ? Pb3 S2A Pb1 60.00(17) 1_556 2_566 ? Pb4 S2A Pb1 116.1(2) 7_575 2_566 ? Pb4 S2A Pb1 116.1(2) . 2_566 ? Pb5 S2A Pb1 61.89(15) 7_576 2_566 ? Pb5 S2A Pb1 61.89(15) 1_556 2_566 ? S2 S2A Pb3 106.9(4) . . ? Pb3 S2A Pb3 140.1(3) 1_556 . ? Pb4 S2A Pb3 55.34(15) 7_575 . ? Pb4 S2A Pb3 55.34(15) . . ? Pb5 S2A Pb3 120.19(14) 7_576 . ? Pb5 S2A Pb3 120.19(14) 1_556 . ? Pb1 S2A Pb3 159.9(3) 2_566 . ? S1 O1 Pb5 131.5(11) 1_554 . ? S1 O1 Pb2 110.9(8) 1_554 . ? Pb5 O1 Pb2 89.5(5) . . ? S1 O1 Pb3 146.7(11) 1_554 . ? Pb5 O1 Pb3 76.0(4) . . ? Pb2 O1 Pb3 83.7(4) . . ? S1 O1 Pb1 81.0(8) 1_554 . ? Pb5 O1 Pb1 137.7(6) . . ? Pb2 O1 Pb1 104.2(5) . . ? Pb3 O1 Pb1 66.2(3) . . ? S1 O1 Pb4 79.3(7) 1_554 1_554 ? Pb5 O1 Pb4 65.6(4) . 1_554 ? Pb2 O1 Pb4 151.4(6) . 1_554 ? Pb3 O1 Pb4 102.4(4) . 1_554 ? Pb1 O1 Pb4 103.7(4) . 1_554 ? S1 O2 Pb1 121.1(11) . 1_556 ? S1 O2 Pb4 128.2(11) . 8_557 ? Pb1 O2 Pb4 82.0(5) 1_556 8_557 ? S1 O2 OH8 97.7(10) . . ? Pb1 O2 OH8 105.9(7) 1_556 . ? Pb4 O2 OH8 121.3(7) 8_557 . ? S1 O2 Pb2 87.2(8) . . ? Pb1 O2 Pb2 146.1(6) 1_556 . ? Pb4 O2 Pb2 95.2(6) 8_557 . ? OH8 O2 Pb2 47.3(4) . . ? S1 O2 Pb5 85.4(8) . 8_557 ? Pb1 O2 Pb5 69.0(4) 1_556 8_557 ? Pb4 O2 Pb5 58.7(3) 8_557 8_557 ? OH8 O2 Pb5 174.9(7) . 8_557 ? Pb2 O2 Pb5 137.2(6) . 8_557 ? S1 O3 Pb2 118.8(10) . . ? S1 O3 Pb5 116.2(11) . 5_666 ? Pb2 O3 Pb5 82.6(5) . 5_666 ? S1 O3 Pb4 112.6(10) . . ? Pb2 O3 Pb4 73.5(4) . . ? Pb5 O3 Pb4 131.2(5) 5_666 . ? S1 O3 Pb5 77.0(8) . 1_556 ? Pb2 O3 Pb5 138.2(7) . 1_556 ? Pb5 O3 Pb5 127.5(5) 5_666 1_556 ? Pb4 O3 Pb5 64.9(4) . 1_556 ? S1 O3 Pb2 178.6(12) . 5_666 ? Pb2 O3 Pb2 62.3(3) . 5_666 ? Pb5 O3 Pb2 64.6(3) 5_666 5_666 ? Pb4 O3 Pb2 66.7(3) . 5_666 ? Pb5 O3 Pb2 101.6(4) 1_556 5_666 ? S2 O4 Pb1 163.6(18) . 2_565 ? S2 O4 Pb4 90.4(9) . 7_575 ? Pb1 O4 Pb4 79.0(5) 2_565 7_575 ? S2 O4 Pb4 90.4(9) . . ? Pb1 O4 Pb4 79.0(5) 2_565 . ? Pb4 O4 Pb4 98.7(7) 7_575 . ? S2 O4 Pb3 71.0(11) . 2_566 ? Pb1 O4 Pb3 125.4(9) 2_565 2_566 ? Pb4 O4 Pb3 128.2(3) 7_575 2_566 ? Pb4 O4 Pb3 128.2(3) . 2_566 ? S2 O5 Pb1 95.6(9) 1_554 2_565 ? S2 O5 Pb5 120.3(10) 1_554 . ? Pb1 O5 Pb5 88.0(5) 2_565 . ? S2 O5 Pb2 139.8(11) 1_554 8_656 ? Pb1 O5 Pb2 118.9(6) 2_565 8_656 ? Pb5 O5 Pb2 83.2(4) . 8_656 ? S2 O5 Pb3 93.5(8) 1_554 2_565 ? Pb1 O5 Pb3 76.5(4) 2_565 2_565 ? Pb5 O5 Pb3 144.2(6) . 2_565 ? Pb2 O5 Pb3 76.7(4) 8_656 2_565 ? S2 O5 Pb4 75.9(8) 1_554 1_554 ? Pb1 O5 Pb4 145.8(6) 2_565 1_554 ? Pb5 O5 Pb4 69.3(4) . 1_554 ? Pb2 O5 Pb4 84.5(4) 8_656 1_554 ? Pb3 O5 Pb4 136.2(6) 2_565 1_554 ? Pb2 O6 Pb5 118.8(7) . . ? Pb2 O6 Pb4 104.6(6) . . ? Pb5 O6 Pb4 98.5(6) . . ? Pb2 O6 Pb2 105.4(6) . 5_666 ? Pb5 O6 Pb2 111.0(7) . 5_666 ? Pb4 O6 Pb2 119.1(7) . 5_666 ? Pb4 O7 Pb1 117.0(7) . 2_565 ? Pb4 O7 Pb5 101.1(6) . . ? Pb1 O7 Pb5 119.8(7) 2_565 . ? Pb4 O7 Pb3 106.7(6) . . ? Pb1 O7 Pb3 105.0(6) 2_565 . ? Pb5 O7 Pb3 106.3(6) . . ? Pb4 OH8 Pb3 106.3(7) . . ? Pb4 OH8 Pb2 94.3(5) . . ? Pb3 OH8 Pb2 115.6(6) . . ? Pb4 OH8 O2 109.7(7) . . ? Pb3 OH8 O2 141.6(8) . . ? Pb2 OH8 O2 74.6(6) . . ? Pb4 OH8 Pb5 61.9(4) . . ? Pb3 OH8 Pb5 68.7(4) . . ? Pb2 OH8 Pb5 69.6(3) . . ? O2 OH8 Pb5 142.1(6) . . ? _refine_diff_density_max 5.904 _refine_diff_density_min -3.945 _refine_diff_density_rms 0.830 _shelx_res_file ; TITL User-defined R21-84.res created by SHELXL-2016/6 at 21:45:07 on 11-Mar-2022 CELL 0.71075 14.01030 20.55290 7.26680 90.00000 90.00000 90.00000 ZERR 4 0.00080 0.00100 0.00050 0.00000 0.00000 0.00000 LATT 1 SYMM .50+X, .50-Y, .50-Z SYMM -X, .50+Y, -Z SYMM .50-X, -Y, .50+Z SFAC O PB S H UNIT 60 32 24 8 L.S. 20 omit 0 24 0 CONN 12 3.0 PB1 CONN 12 3.0 PB2 CONN 12 3.0 PB3 CONN 12 3.0 PB4 CONN 12 3.0 PB5 BIND OH8 O2 FMAP 2 PLAN 20 ACTA SIZE 0.070 0.060 0.025 WGHT 0.067600 EXTI 0.000032 FVAR 0.05931 PB1 2 0.270811 0.750000 0.077475 10.50000 0.01300 0.02096 = 0.01661 0.00000 -0.00014 0.00000 PB2 2 0.402332 0.559894 0.499333 11.00000 0.01559 0.02015 = 0.02190 0.00085 -0.00024 -0.00023 PB3 2 0.504540 0.750000 0.383266 10.50000 0.01809 0.01798 = 0.02146 0.00000 -0.00317 0.00000 PB4 2 0.619376 0.625920 0.689768 11.00000 0.02400 0.01976 = 0.01625 0.00210 -0.00347 -0.00077 PB5 2 0.632604 0.597737 0.212334 11.00000 0.02180 0.02184 = 0.01733 -0.00139 0.00294 -0.00065 S1 3 0.385897 0.582917 0.999418 11.00000 0.02420 0.02068 = 0.02171 0.00305 0.00113 0.00788 S1A 3 0.299041 0.520377 0.128946 11.00000 0.02633 0.03347 = 0.02867 -0.00391 0.00473 -0.00468 S2 3 0.737252 0.750000 0.972890 10.50000 0.03020 0.02674 = 0.01083 0.00000 -0.00693 0.00000 S2A 3 0.596051 0.750000 0.971936 10.50000 0.02681 0.04042 = 0.03724 0.00000 -0.00254 0.00000 O1 1 0.446590 0.611902 0.139776 11.00000 0.02040 0.04781 = 0.02230 0.00840 -0.00020 -0.01983 O2 1 0.327758 0.631634 0.901505 11.00000 0.03156 0.04491 = 0.04467 0.01019 0.00929 0.02954 O3 1 0.441033 0.544509 0.863973 11.00000 0.04530 0.03360 = 0.02894 -0.00110 0.00808 0.02806 O4 1 0.767995 0.750000 0.782395 10.50000 0.05150 0.03088 = 0.00713 0.00000 0.00007 0.00000 O5 1 0.770067 0.691831 0.071349 11.00000 0.00926 0.04357 = 0.03908 0.01656 0.00018 0.00540 O6 1 0.560529 0.553395 0.471610 11.00000 0.01681 0.00892 = 0.03537 0.00136 0.00391 -0.00113 O7 1 0.643952 0.680809 0.429151 11.00000 0.01848 OH8 1 0.474290 0.670132 0.615852 11.00000 0.04181 0.01270 = 0.02734 0.00156 0.00047 0.00124 HKLF 4 REM User-defined REM R1 = 0.0570 for 1538 Fo > 4sig(Fo) and 0.0684 for all 1878 data REM 135 parameters refined using 0 restraints END WGHT 0.0675 0.0000 REM Highest difference peak 5.904, deepest hole -3.945, 1-sigma level 0.830 Q1 1 0.5768 0.7500 0.3739 10.50000 0.05 5.90 Q2 1 0.4732 0.5611 0.4924 11.00000 0.05 5.60 Q3 1 0.4365 0.7500 0.3797 10.50000 0.05 5.08 Q4 1 0.2007 0.7500 0.0770 10.50000 0.05 4.95 Q5 1 0.5462 0.6250 0.6936 11.00000 0.05 4.90 Q6 1 0.3411 0.7500 0.0844 10.50000 0.05 4.84 Q7 1 0.3316 0.5603 0.5004 11.00000 0.05 4.82 Q8 1 0.5581 0.5997 0.2116 11.00000 0.05 4.67 Q9 1 0.7011 0.5979 0.2059 11.00000 0.05 4.45 Q10 1 0.6926 0.6249 0.6825 11.00000 0.05 4.26 Q11 1 0.6365 0.7500 0.3755 10.50000 0.05 4.08 Q12 1 0.8623 0.7500 0.1301 10.50000 0.05 3.65 Q13 1 0.3921 0.7500 0.1291 10.50000 0.05 3.35 Q14 1 0.5428 0.5912 0.5872 11.00000 0.05 2.88 Q15 1 0.6112 0.7500 0.7933 10.50000 0.05 2.79 Q16 1 0.6365 0.5930 0.4067 11.00000 0.05 2.70 Q17 1 0.2677 0.7500 -0.0608 10.50000 0.05 2.58 Q18 1 0.4871 0.5871 0.2116 11.00000 0.05 2.47 Q19 1 0.7240 0.7500 0.6379 10.50000 0.05 2.43 Q20 1 0.6168 0.5279 0.1946 11.00000 0.05 2.43 ; _shelx_res_checksum 94122 _shelx_hkl_file ; -2 1 0 901.31 38.94 2 -1 0 735.87 30.27 2 1 0 658.48 30.19 -2 -1 0 709.16 31.57 -1 0 -1 1871.59 73.87 1 0 1 2136.68 81.50 1 -1 1 116.75 2.63 -1 -1 1 121.07 3.55 -1 1 -1 111.71 2.41 -1 -3 0 -0.40 1.21 1 3 0 0.69 1.40 0 -2 1 9.51 0.83 0 2 1 7.53 1.44 -2 2 0 174.36 6.78 2 2 0 162.47 8.06 -2 -2 0 155.83 9.99 2 -2 0 173.92 6.55 1 -2 1 20.76 1.58 -1 -2 -1 33.98 2.18 -1 -2 1 27.39 3.38 1 2 1 33.10 2.27 0 -4 0 412.65 9.89 0 4 0 406.43 10.06 -2 0 1 13.93 3.66 -2 0 -1 1.35 1.69 2 0 1 4.52 1.95 2 0 -1 -1.24 2.02 0 -3 1 43.66 0.81 0 3 1 55.96 2.62 -2 -1 -1 4.51 1.76 2 1 -1 0.47 2.14 -2 1 1 1.25 2.12 2 -1 1 3.47 1.83 -2 -1 1 0.52 2.44 2 1 1 0.68 2.00 -2 1 -1 1.81 1.53 -2 -3 0 284.46 14.55 -2 3 0 332.05 10.37 2 3 0 265.28 11.47 1 4 0 2.23 1.71 -1 -4 0 1.28 1.43 -1 -3 -1 417.09 12.87 1 3 1 454.20 13.96 1 3 -1 264.52 13.32 -1 -3 1 250.88 9.27 3 0 0 -3.10 3.82 -3 0 0 6.40 3.26 3 -1 0 -1.64 2.93 -3 1 0 0.34 3.39 3 1 0 4.92 3.20 -2 -2 -1 120.13 5.46 2 2 -1 92.56 6.02 2 2 1 160.66 6.59 2 -2 1 79.23 5.00 -2 -2 1 108.89 10.36 -2 2 -1 95.74 4.38 -3 -2 0 -0.29 3.01 3 2 0 2.16 3.16 3 -2 0 -0.78 2.42 -3 2 0 1.09 2.80 0 -4 1 2.76 0.52 0 4 1 3.24 2.86 0 4 -1 4.91 1.05 2 4 0 54.69 4.34 -2 -4 0 53.28 3.93 0 5 0 1.89 1.38 0 -5 0 2.67 1.33 -2 3 -1 72.95 5.17 -2 -3 -1 91.04 5.01 -2 -3 1 58.85 4.92 2 -3 1 65.60 3.06 2 3 1 105.79 5.64 2 3 -1 62.63 6.18 -1 4 -1 59.85 1.37 -1 -4 1 54.10 2.49 1 4 1 79.86 4.22 -1 -4 -1 70.76 3.83 1 5 0 3.12 1.64 -1 -5 0 -1.32 1.63 -3 0 -1 204.15 9.66 3 0 -1 225.51 10.75 3 0 1 195.89 10.89 -3 0 1 268.89 12.57 3 -1 -1 174.12 8.75 -3 1 1 202.12 10.04 3 1 -1 154.41 9.34 -3 -1 -1 163.38 11.20 3 1 1 169.41 9.44 3 -1 1 123.15 8.01 -3 -1 1 193.10 10.81 -3 1 -1 144.79 10.72 -3 -3 0 3.99 2.94 -3 3 0 2.14 2.70 3 3 0 5.87 3.39 3 -3 0 1.77 2.36 3 2 1 316.07 14.60 -3 2 -1 228.90 11.26 3 -2 1 254.37 18.46 -3 2 1 351.95 14.29 3 2 -1 218.95 18.94 -3 -2 -1 263.73 12.41 -3 -2 1 295.76 16.39 2 4 -1 9.16 3.26 -2 -4 1 9.91 4.09 2 4 1 10.72 3.07 -2 -4 -1 8.80 4.07 -2 4 -1 11.32 2.73 0 1 2 4.77 1.69 0 -5 1 1815.98 65.25 0 5 1 2537.92 103.63 0 5 -1 1680.78 63.55 2 5 0 2752.13 161.34 -2 -5 0 2883.81 164.99 1 0 2 72.15 2.69 -1 0 -2 46.65 2.43 4 0 0 2378.93 226.51 -4 0 0 3402.63 253.08 -1 -1 -2 12.00 1.89 1 1 2 10.64 1.95 1 -1 2 14.13 1.47 -1 1 -2 12.59 1.35 -1 -5 1 114.91 5.32 1 5 1 155.69 6.81 1 5 -1 91.66 4.48 -3 4 0 0.21 2.50 -3 -4 0 -5.14 2.81 3 4 0 2.45 3.43 -4 1 0 21.02 8.06 -4 -1 0 9.42 4.41 4 -1 0 8.87 4.52 4 1 0 8.55 5.42 0 2 2 0.57 1.81 0 6 0 9346.48 821.16 0 -6 0 9999.00 866.20 3 3 -1 38.09 6.87 3 3 1 60.84 5.58 3 -3 1 46.31 4.27 -3 -3 1 40.99 5.47 -3 3 -1 49.20 4.54 -3 -3 -1 49.59 4.79 -1 -2 2 233.15 7.41 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35.22 14.94 11 7 6 57.22 27.99 -11 7 6 90.11 28.43 -7 10 7 324.44 46.22 -7 10 7 257.45 35.39 7 10 7 409.23 46.63 -7 -10 7 147.84 30.93 -7 -22 -1 64.41 24.41 -7 22 1 63.04 14.46 -7 22 -1 92.31 18.48 -7 22 -1 51.32 11.75 7 22 -1 92.41 26.48 -7 22 1 87.68 20.69 7 22 1 84.53 28.48 -7 -22 1 72.72 14.67 -5 16 6 4.84 14.66 5 16 6 58.61 19.04 -14 -12 2 20.98 20.45 -14 -12 -2 41.55 18.66 14 12 -2 18.34 26.76 -12 0 -6 -1.15 8.23 -12 16 2 55.02 36.54 -12 -16 -2 15.65 17.05 -12 -16 2 33.97 16.00 -6 3 8 166.42 23.02 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 58349