data_cubothioplumbite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'cubothioplumbite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H1.33 O4.33 Pb1.67 S2' _chemical_formula_weight 480.11 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 cubic _space_group_IT_number 205 _space_group_name_H-M_alt 'P a -3' _space_group_name_Hall '-P 2ac 2ab 3' _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' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z, -x-1/2, y-1/2' 'z-1/2, x, -y-1/2' '-y, -z, -x' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' 'y-1/2, z, -x-1/2' _cell_length_a 14.9179(13) _cell_length_b 14.9179(13) _cell_length_c 14.9179(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3319.9(9) _cell_formula_units_Z 24 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7206 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'equant' _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 5.763 _exptl_crystal_F_000 4912 _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.130 _exptl_absorpt_coefficient_mu 51.355 _shelx_estimated_absorpt_T_min 0.042 _shelx_estimated_absorpt_T_max 0.057 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.486 _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 10556 _diffrn_reflns_av_unetI/netI 0.0544 _diffrn_reflns_av_R_equivalents 0.1160 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.345 _diffrn_reflns_theta_max 27.432 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 1274 _reflns_number_gt 1090 _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^)+(0.0308P)^2^+15.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_extinction_coef 0.00035(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1274 _refine_ls_number_parameters 79 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _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_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 0.58314(3) 0.22600(3) 0.75169(3) 0.01548(17) Uani 1 1 d . . . . . Pb2 Pb 0.82483(3) 0.17517(3) 0.67517(3) 0.0151(2) Uani 1 3 d S T P . . Pb3 Pb 0.500000 0.500000 0.500000 0.0204(3) Uani 1 6 d S T P . . Pb4 Pb 0.500000 0.500000 0.000000 0.0344(3) Uani 1 6 d S T P . . S1 S 0.49888(16) 0.49387(17) 0.73490(17) 0.0118(6) Uani 1 1 d . . . . . S2 S 0.59473(18) 0.53880(18) 0.81950(19) 0.0170(6) Uani 1 1 d . . . . . O1 O 0.5247(6) 0.4077(5) 0.6975(5) 0.0226(17) Uani 1 1 d . . . . . O2 O 0.4166(5) 0.4887(6) 0.7875(6) 0.0269(19) Uani 1 1 d . . . . . O3 O 0.4923(5) 0.5612(5) 0.6630(5) 0.0237(19) Uani 1 1 d . . . . . OH4 O 0.7178(5) 0.1545(5) 0.7978(5) 0.0132(15) Uani 1 1 d D . . . . H4 H 0.715(7) 0.093(3) 0.817(7) 0.020 Uiso 1 1 d D U . . . OH5 O 0.6692(4) 0.3308(4) 0.8308(4) 0.009(3) Uani 1 3 d DS T P . . H5 H 0.6315(13) 0.3685(13) 0.8685(13) 0.013 Uiso 1 3 d DS U P . . 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 0.0094(2) 0.0190(3) 0.0181(3) -0.00083(16) -0.00061(15) -0.00393(15) Pb2 0.0151(2) 0.0151(2) 0.0151(2) -0.00244(15) 0.00244(15) 0.00244(15) Pb3 0.0204(3) 0.0204(3) 0.0204(3) -0.0052(2) -0.0052(2) -0.0052(2) Pb4 0.0344(3) 0.0344(3) 0.0344(3) -0.0053(3) 0.0053(3) 0.0053(3) S1 0.0139(14) 0.0117(13) 0.0100(13) -0.0011(9) 0.0012(10) 0.0008(10) S2 0.0144(13) 0.0169(13) 0.0197(14) -0.0021(11) -0.0050(11) -0.0037(11) O1 0.035(5) 0.012(4) 0.021(4) -0.002(3) 0.005(4) 0.004(3) O2 0.011(4) 0.042(5) 0.028(5) -0.005(4) 0.006(4) -0.003(4) O3 0.032(5) 0.019(4) 0.020(4) 0.005(3) -0.005(4) 0.011(3) OH4 0.014(4) 0.008(3) 0.018(4) 0.004(3) 0.005(3) 0.002(3) OH5 0.009(3) 0.009(3) 0.009(3) -0.001(3) 0.001(3) 0.001(3) _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 OH5 2.342(4) . ? Pb1 OH4 2.375(7) . ? Pb1 OH4 2.441(7) 8_665 ? Pb1 O2 2.737(8) 21_666 ? Pb1 O1 2.959(7) . ? Pb1 O3 2.988(8) 3_646 ? Pb1 S2 3.241(3) 11_646 ? Pb1 O1 3.366(8) 11_646 ? Pb1 O2 3.589(9) 3_646 ? Pb1 S1 3.678(3) 3_646 ? Pb1 OH4 3.738(7) 22_655 ? Pb1 Pb1 3.7847(8) 11_646 ? Pb1 Pb1 3.7847(8) 8_665 ? Pb1 Pb2 3.8570(8) . ? Pb1 S1 3.897(2) 11_646 ? Pb2 OH4 2.448(7) . ? Pb2 OH4 2.448(7) 11_646 ? Pb2 OH4 2.448(7) 8_665 ? Pb2 S2 3.196(3) 18_755 ? Pb2 S2 3.196(3) 22_755 ? Pb2 S2 3.196(3) 14_755 ? Pb2 O3 3.219(9) 18_755 ? Pb2 O3 3.219(9) 22_755 ? Pb2 O3 3.219(9) 14_755 ? Pb2 S1 3.876(3) 18_755 ? Pb2 S1 3.876(3) 22_755 ? Pb2 S1 3.876(3) 14_755 ? Pb3 O3 2.600(8) 13_666 ? Pb3 O3 2.600(8) 21_666 ? Pb3 O3 2.600(8) 9 ? Pb3 O3 2.600(8) 17_666 ? Pb3 O3 2.600(8) 5 ? Pb3 O3 2.600(8) . ? Pb3 O1 3.273(8) . ? Pb3 O1 3.273(8) 21_666 ? Pb3 O1 3.273(8) 9 ? Pb3 O1 3.273(8) 17_666 ? Pb3 O1 3.273(8) 5 ? Pb3 O1 3.273(8) 13_666 ? Pb3 S1 3.505(3) 17_666 ? Pb3 S1 3.505(3) 5 ? Pb3 S1 3.505(3) 13_666 ? Pb4 S2 3.096(3) 23_575 ? Pb4 S2 3.096(3) 11_645 ? Pb4 S2 3.096(3) 20_556 ? Pb4 S2 3.096(3) 8_664 ? Pb4 S2 3.096(3) 13_666 ? Pb4 S2 3.096(3) 1_554 ? Pb4 O2 3.410(9) 13_666 ? Pb4 O2 3.410(9) 1_554 ? Pb4 O2 3.410(9) 20_556 ? Pb4 O2 3.410(9) 8_664 ? Pb4 O2 3.410(9) 23_575 ? Pb4 O2 3.410(9) 11_645 ? Pb4 S1 3.956(3) 13_666 ? Pb4 S1 3.956(3) 1_554 ? Pb4 S1 3.956(3) 20_556 ? S1 O1 1.454(8) . ? S1 O2 1.458(8) . ? S1 O3 1.473(8) . ? S1 S2 2.021(4) . ? OH4 H4 0.96(3) . ? OH5 H5 0.97(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 OH5 Pb1 OH4 72.0(3) . . ? OH5 Pb1 OH4 70.8(3) . 8_665 ? OH4 Pb1 OH4 73.2(3) . 8_665 ? OH5 Pb1 O2 136.53(18) . 21_666 ? OH4 Pb1 O2 124.3(3) . 21_666 ? OH4 Pb1 O2 76.4(2) 8_665 21_666 ? OH5 Pb1 O1 71.8(2) . . ? OH4 Pb1 O1 137.7(2) . . ? OH4 Pb1 O1 74.8(2) 8_665 . ? O2 Pb1 O1 72.6(2) 21_666 . ? OH5 Pb1 O3 122.76(16) . 3_646 ? OH4 Pb1 O3 80.0(2) . 3_646 ? OH4 Pb1 O3 144.1(2) 8_665 3_646 ? O2 Pb1 O3 100.5(2) 21_666 3_646 ? O1 Pb1 O3 139.3(2) . 3_646 ? OH5 Pb1 S2 70.4(3) . 11_646 ? OH4 Pb1 S2 117.57(18) . 11_646 ? OH4 Pb1 S2 132.86(17) 8_665 11_646 ? O2 Pb1 S2 117.41(19) 21_666 11_646 ? O1 Pb1 S2 68.51(16) . 11_646 ? O3 Pb1 S2 80.88(16) 3_646 11_646 ? OH5 Pb1 O1 64.06(16) . 11_646 ? OH4 Pb1 O1 67.8(2) . 11_646 ? OH4 Pb1 O1 127.0(2) 8_665 11_646 ? O2 Pb1 O1 156.3(2) 21_666 11_646 ? O1 Pb1 O1 113.5(3) . 11_646 ? O3 Pb1 O1 59.29(19) 3_646 11_646 ? S2 Pb1 O1 51.44(13) 11_646 11_646 ? OH5 Pb1 O2 137.7(2) . 3_646 ? OH4 Pb1 O2 66.6(2) . 3_646 ? OH4 Pb1 O2 104.0(2) 8_665 3_646 ? O2 Pb1 O2 77.2(3) 21_666 3_646 ? O1 Pb1 O2 149.2(2) . 3_646 ? O3 Pb1 O2 42.1(2) 3_646 3_646 ? S2 Pb1 O2 122.70(13) 11_646 3_646 ? O1 Pb1 O2 92.09(19) 11_646 3_646 ? OH5 Pb1 S1 141.58(4) . 3_646 ? OH4 Pb1 S1 80.96(17) . 3_646 ? OH4 Pb1 S1 126.72(17) 8_665 3_646 ? O2 Pb1 S1 81.41(18) 21_666 3_646 ? O1 Pb1 S1 141.16(17) . 3_646 ? O3 Pb1 S1 22.64(14) 3_646 3_646 ? S2 Pb1 S1 100.37(6) 11_646 3_646 ? O1 Pb1 S1 80.83(13) 11_646 3_646 ? O2 Pb1 S1 23.11(12) 3_646 3_646 ? OH5 Pb1 OH4 113.4(3) . 22_655 ? OH4 Pb1 OH4 165.84(8) . 22_655 ? OH4 Pb1 OH4 120.7(3) 8_665 22_655 ? O2 Pb1 OH4 61.7(2) 21_666 22_655 ? O1 Pb1 OH4 54.63(19) . 22_655 ? O3 Pb1 OH4 86.3(2) 3_646 22_655 ? S2 Pb1 OH4 55.95(12) 11_646 22_655 ? O1 Pb1 OH4 102.07(16) 11_646 22_655 ? O2 Pb1 OH4 105.17(17) 3_646 22_655 ? S1 Pb1 OH4 87.80(12) 3_646 22_655 ? OH5 Pb1 Pb1 36.10(13) . 11_646 ? OH4 Pb1 Pb1 38.83(18) . 11_646 ? OH4 Pb1 Pb1 78.73(16) 8_665 11_646 ? O2 Pb1 Pb1 154.03(18) 21_666 11_646 ? O1 Pb1 Pb1 107.87(16) . 11_646 ? O3 Pb1 Pb1 95.14(15) 3_646 11_646 ? S2 Pb1 Pb1 85.32(5) 11_646 11_646 ? O1 Pb1 Pb1 48.46(12) 11_646 11_646 ? O2 Pb1 Pb1 101.83(13) 3_646 11_646 ? S1 Pb1 Pb1 108.07(4) 3_646 11_646 ? OH4 Pb1 Pb1 140.59(11) 22_655 11_646 ? OH5 Pb1 Pb1 36.10(13) . 8_665 ? OH4 Pb1 Pb1 79.44(16) . 8_665 ? OH4 Pb1 Pb1 37.60(16) 8_665 8_665 ? O2 Pb1 Pb1 102.54(17) 21_666 8_665 ? O1 Pb1 Pb1 58.35(16) . 8_665 ? O3 Pb1 Pb1 155.13(15) 3_646 8_665 ? S2 Pb1 Pb1 96.50(5) 11_646 8_665 ? O1 Pb1 Pb1 99.73(13) 11_646 8_665 ? O2 Pb1 Pb1 136.48(12) 3_646 8_665 ? S1 Pb1 Pb1 158.49(4) 3_646 8_665 ? OH4 Pb1 Pb1 112.84(11) 22_655 8_665 ? Pb1 Pb1 Pb1 60.0 11_646 8_665 ? OH5 Pb1 Pb2 76.6(3) . . ? OH4 Pb1 Pb2 37.56(17) . . ? OH4 Pb1 Pb2 37.99(16) 8_665 . ? O2 Pb1 Pb2 94.58(18) 21_666 . ? O1 Pb1 Pb2 112.00(16) . . ? O3 Pb1 Pb2 108.46(16) 3_646 . ? S2 Pb1 Pb2 144.93(5) 11_646 . ? O1 Pb1 Pb2 103.32(12) 11_646 . ? O2 Pb1 Pb2 75.93(12) 3_646 . ? S1 Pb1 Pb2 98.16(4) 3_646 . ? OH4 Pb1 Pb2 154.53(11) 22_655 . ? Pb1 Pb1 Pb2 60.618(7) 11_646 . ? Pb1 Pb1 Pb2 60.618(7) 8_665 . ? OH5 Pb1 S1 69.98(18) . 11_646 ? OH4 Pb1 S1 89.31(18) . 11_646 ? OH4 Pb1 S1 140.34(16) 8_665 11_646 ? O2 Pb1 S1 139.74(18) 21_666 11_646 ? O1 Pb1 S1 98.22(15) . 11_646 ? O3 Pb1 S1 60.68(15) 3_646 11_646 ? S2 Pb1 S1 31.21(6) 11_646 11_646 ? O1 Pb1 S1 21.54(13) 11_646 11_646 ? O2 Pb1 S1 100.91(14) 3_646 11_646 ? S1 Pb1 S1 83.23(8) 3_646 11_646 ? OH4 Pb1 S1 80.79(11) 22_655 11_646 ? Pb1 Pb1 S1 66.21(4) 11_646 11_646 ? Pb1 Pb1 S1 105.25(4) 8_665 11_646 ? Pb2 Pb1 S1 124.40(4) . 11_646 ? OH4 Pb2 OH4 71.9(3) . 11_646 ? OH4 Pb2 OH4 71.9(3) . 8_665 ? OH4 Pb2 OH4 71.9(3) 11_646 8_665 ? OH4 Pb2 S2 89.37(18) . 18_755 ? OH4 Pb2 S2 141.32(17) 11_646 18_755 ? OH4 Pb2 S2 70.21(17) 8_665 18_755 ? OH4 Pb2 S2 141.33(17) . 22_755 ? OH4 Pb2 S2 70.21(17) 11_646 22_755 ? OH4 Pb2 S2 89.37(18) 8_665 22_755 ? S2 Pb2 S2 116.28(3) 18_755 22_755 ? OH4 Pb2 S2 70.21(17) . 14_755 ? OH4 Pb2 S2 89.37(18) 11_646 14_755 ? OH4 Pb2 S2 141.32(17) 8_665 14_755 ? S2 Pb2 S2 116.28(3) 18_755 14_755 ? S2 Pb2 S2 116.28(3) 22_755 14_755 ? OH4 Pb2 O3 108.9(2) . 18_755 ? OH4 Pb2 O3 166.1(2) 11_646 18_755 ? OH4 Pb2 O3 121.9(2) 8_665 18_755 ? S2 Pb2 O3 51.95(14) 18_755 18_755 ? S2 Pb2 O3 109.67(15) 22_755 18_755 ? S2 Pb2 O3 78.18(14) 14_755 18_755 ? OH4 Pb2 O3 166.1(2) . 22_755 ? OH4 Pb2 O3 121.9(2) 11_646 22_755 ? OH4 Pb2 O3 108.9(2) 8_665 22_755 ? S2 Pb2 O3 78.18(14) 18_755 22_755 ? S2 Pb2 O3 51.95(14) 22_755 22_755 ? S2 Pb2 O3 109.67(15) 14_755 22_755 ? O3 Pb2 O3 58.3(2) 18_755 22_755 ? OH4 Pb2 O3 121.9(2) . 14_755 ? OH4 Pb2 O3 108.9(2) 11_646 14_755 ? OH4 Pb2 O3 166.1(2) 8_665 14_755 ? S2 Pb2 O3 109.67(15) 18_755 14_755 ? S2 Pb2 O3 78.18(14) 22_755 14_755 ? S2 Pb2 O3 51.95(14) 14_755 14_755 ? O3 Pb2 O3 58.3(2) 18_755 14_755 ? O3 Pb2 O3 58.3(2) 22_755 14_755 ? OH4 Pb2 Pb1 37.86(17) . 11_646 ? OH4 Pb2 Pb1 36.26(16) 11_646 11_646 ? OH4 Pb2 Pb1 77.15(16) 8_665 11_646 ? S2 Pb2 Pb1 125.01(5) 18_755 11_646 ? S2 Pb2 Pb1 106.07(5) 22_755 11_646 ? S2 Pb2 Pb1 68.44(5) 14_755 11_646 ? O3 Pb2 Pb1 139.06(14) 18_755 11_646 ? O3 Pb2 Pb1 155.86(13) 22_755 11_646 ? O3 Pb2 Pb1 112.06(13) 14_755 11_646 ? OH4 Pb2 Pb1 77.15(16) . 8_665 ? OH4 Pb2 Pb1 37.85(17) 11_646 8_665 ? OH4 Pb2 Pb1 36.26(16) 8_665 8_665 ? S2 Pb2 Pb1 106.07(5) 18_755 8_665 ? S2 Pb2 Pb1 68.44(5) 22_755 8_665 ? S2 Pb2 Pb1 125.01(5) 14_755 8_665 ? O3 Pb2 Pb1 155.86(13) 18_755 8_665 ? O3 Pb2 Pb1 112.06(13) 22_755 8_665 ? O3 Pb2 Pb1 139.06(14) 14_755 8_665 ? Pb1 Pb2 Pb1 58.765(13) 11_646 8_665 ? OH4 Pb2 Pb1 36.26(16) . . ? OH4 Pb2 Pb1 77.15(16) 11_646 . ? OH4 Pb2 Pb1 37.85(17) 8_665 . ? S2 Pb2 Pb1 68.44(5) 18_755 . ? S2 Pb2 Pb1 125.01(5) 22_755 . ? S2 Pb2 Pb1 106.07(5) 14_755 . ? O3 Pb2 Pb1 112.06(13) 18_755 . ? O3 Pb2 Pb1 139.06(14) 22_755 . ? O3 Pb2 Pb1 155.86(13) 14_755 . ? Pb1 Pb2 Pb1 58.764(13) 11_646 . ? Pb1 Pb2 Pb1 58.764(13) 8_665 . ? OH4 Pb2 S1 106.62(17) . 18_755 ? OH4 Pb2 S1 172.39(17) 11_646 18_755 ? OH4 Pb2 S1 100.55(16) 8_665 18_755 ? S2 Pb2 S1 31.38(6) 18_755 18_755 ? S2 Pb2 S1 109.96(6) 22_755 18_755 ? S2 Pb2 S1 97.15(6) 14_755 18_755 ? O3 Pb2 S1 21.51(13) 18_755 18_755 ? O3 Pb2 S1 59.46(14) 22_755 18_755 ? O3 Pb2 S1 78.30(14) 14_755 18_755 ? Pb1 Pb2 S1 143.88(4) 11_646 18_755 ? Pb1 Pb2 S1 134.70(4) 8_665 18_755 ? Pb1 Pb2 S1 97.18(4) . 18_755 ? OH4 Pb2 S1 172.39(17) . 22_755 ? OH4 Pb2 S1 100.55(16) 11_646 22_755 ? OH4 Pb2 S1 106.62(17) 8_665 22_755 ? S2 Pb2 S1 97.15(6) 18_755 22_755 ? S2 Pb2 S1 31.38(6) 22_755 22_755 ? S2 Pb2 S1 109.96(6) 14_755 22_755 ? O3 Pb2 S1 78.30(14) 18_755 22_755 ? O3 Pb2 S1 21.51(13) 22_755 22_755 ? O3 Pb2 S1 59.46(14) 14_755 22_755 ? Pb1 Pb2 S1 134.70(4) 11_646 22_755 ? Pb1 Pb2 S1 97.18(4) 8_665 22_755 ? Pb1 Pb2 S1 143.88(4) . 22_755 ? S1 Pb2 S1 80.96(6) 18_755 22_755 ? OH4 Pb2 S1 100.55(16) . 14_755 ? OH4 Pb2 S1 106.62(17) 11_646 14_755 ? OH4 Pb2 S1 172.39(17) 8_665 14_755 ? S2 Pb2 S1 109.96(6) 18_755 14_755 ? S2 Pb2 S1 97.15(6) 22_755 14_755 ? S2 Pb2 S1 31.38(6) 14_755 14_755 ? O3 Pb2 S1 59.46(14) 18_755 14_755 ? O3 Pb2 S1 78.30(14) 22_755 14_755 ? O3 Pb2 S1 21.51(13) 14_755 14_755 ? Pb1 Pb2 S1 97.18(4) 11_646 14_755 ? Pb1 Pb2 S1 143.88(4) 8_665 14_755 ? Pb1 Pb2 S1 134.70(4) . 14_755 ? S1 Pb2 S1 80.96(6) 18_755 14_755 ? S1 Pb2 S1 80.96(6) 22_755 14_755 ? O3 Pb3 O3 74.2(3) 13_666 21_666 ? O3 Pb3 O3 105.8(3) 13_666 9 ? O3 Pb3 O3 180.0 21_666 9 ? O3 Pb3 O3 74.2(3) 13_666 17_666 ? O3 Pb3 O3 74.2(3) 21_666 17_666 ? O3 Pb3 O3 105.8(3) 9 17_666 ? O3 Pb3 O3 105.8(3) 13_666 5 ? O3 Pb3 O3 105.8(3) 21_666 5 ? O3 Pb3 O3 74.2(3) 9 5 ? O3 Pb3 O3 180.0 17_666 5 ? O3 Pb3 O3 180.0 13_666 . ? O3 Pb3 O3 105.8(3) 21_666 . ? O3 Pb3 O3 74.2(3) 9 . ? O3 Pb3 O3 105.8(3) 17_666 . ? O3 Pb3 O3 74.2(3) 5 . ? O3 Pb3 O1 133.5(2) 13_666 . ? O3 Pb3 O1 66.8(2) 21_666 . ? O3 Pb3 O1 113.2(2) 9 . ? O3 Pb3 O1 116.1(2) 17_666 . ? O3 Pb3 O1 63.9(2) 5 . ? O3 Pb3 O1 46.5(2) . . ? O3 Pb3 O1 63.9(2) 13_666 21_666 ? O3 Pb3 O1 46.5(2) 21_666 21_666 ? O3 Pb3 O1 133.5(2) 9 21_666 ? O3 Pb3 O1 113.2(2) 17_666 21_666 ? O3 Pb3 O1 66.8(2) 5 21_666 ? O3 Pb3 O1 116.1(2) . 21_666 ? O1 Pb3 O1 71.04(14) . 21_666 ? O3 Pb3 O1 116.1(2) 13_666 9 ? O3 Pb3 O1 133.5(2) 21_666 9 ? O3 Pb3 O1 46.5(2) 9 9 ? O3 Pb3 O1 66.8(2) 17_666 9 ? O3 Pb3 O1 113.2(2) 5 9 ? O3 Pb3 O1 63.9(2) . 9 ? O1 Pb3 O1 108.96(14) . 9 ? O1 Pb3 O1 180.0 21_666 9 ? O3 Pb3 O1 113.2(2) 13_666 17_666 ? O3 Pb3 O1 63.9(2) 21_666 17_666 ? O3 Pb3 O1 116.1(2) 9 17_666 ? O3 Pb3 O1 46.5(2) 17_666 17_666 ? O3 Pb3 O1 133.5(2) 5 17_666 ? O3 Pb3 O1 66.8(2) . 17_666 ? O1 Pb3 O1 71.04(14) . 17_666 ? O1 Pb3 O1 108.96(14) 21_666 17_666 ? O1 Pb3 O1 71.04(14) 9 17_666 ? O3 Pb3 O1 66.8(2) 13_666 5 ? O3 Pb3 O1 116.1(2) 21_666 5 ? O3 Pb3 O1 63.9(2) 9 5 ? O3 Pb3 O1 133.5(2) 17_666 5 ? O3 Pb3 O1 46.5(2) 5 5 ? O3 Pb3 O1 113.2(2) . 5 ? O1 Pb3 O1 108.96(14) . 5 ? O1 Pb3 O1 71.04(14) 21_666 5 ? O1 Pb3 O1 108.96(14) 9 5 ? O1 Pb3 O1 180.0 17_666 5 ? O3 Pb3 O1 46.5(2) 13_666 13_666 ? O3 Pb3 O1 113.2(2) 21_666 13_666 ? O3 Pb3 O1 66.8(2) 9 13_666 ? O3 Pb3 O1 63.9(2) 17_666 13_666 ? O3 Pb3 O1 116.1(2) 5 13_666 ? O3 Pb3 O1 133.5(2) . 13_666 ? O1 Pb3 O1 180.0 . 13_666 ? O1 Pb3 O1 108.96(14) 21_666 13_666 ? O1 Pb3 O1 71.04(14) 9 13_666 ? O1 Pb3 O1 108.96(14) 17_666 13_666 ? O1 Pb3 O1 71.04(14) 5 13_666 ? O3 Pb3 S1 94.01(19) 13_666 17_666 ? O3 Pb3 S1 69.64(17) 21_666 17_666 ? O3 Pb3 S1 110.36(17) 9 17_666 ? O3 Pb3 S1 22.19(17) 17_666 17_666 ? O3 Pb3 S1 157.81(17) 5 17_666 ? O3 Pb3 S1 85.99(19) . 17_666 ? O1 Pb3 S1 95.22(15) . 17_666 ? O1 Pb3 S1 115.34(13) 21_666 17_666 ? O1 Pb3 S1 64.66(13) 9 17_666 ? O1 Pb3 S1 24.47(13) 17_666 17_666 ? O1 Pb3 S1 155.53(13) 5 17_666 ? O1 Pb3 S1 84.78(15) 13_666 17_666 ? O3 Pb3 S1 85.99(19) 13_666 5 ? O3 Pb3 S1 110.36(17) 21_666 5 ? O3 Pb3 S1 69.64(17) 9 5 ? O3 Pb3 S1 157.81(17) 17_666 5 ? O3 Pb3 S1 22.19(17) 5 5 ? O3 Pb3 S1 94.01(19) . 5 ? O1 Pb3 S1 84.78(15) . 5 ? O1 Pb3 S1 64.66(13) 21_666 5 ? O1 Pb3 S1 115.34(13) 9 5 ? O1 Pb3 S1 155.53(13) 17_666 5 ? O1 Pb3 S1 24.47(13) 5 5 ? O1 Pb3 S1 95.22(15) 13_666 5 ? S1 Pb3 S1 180.0 17_666 5 ? O3 Pb3 S1 22.19(17) 13_666 13_666 ? O3 Pb3 S1 94.01(19) 21_666 13_666 ? O3 Pb3 S1 85.99(19) 9 13_666 ? O3 Pb3 S1 69.64(17) 17_666 13_666 ? O3 Pb3 S1 110.36(17) 5 13_666 ? O3 Pb3 S1 157.81(17) . 13_666 ? O1 Pb3 S1 155.53(13) . 13_666 ? O1 Pb3 S1 84.78(15) 21_666 13_666 ? O1 Pb3 S1 95.22(15) 9 13_666 ? O1 Pb3 S1 115.34(13) 17_666 13_666 ? O1 Pb3 S1 64.66(13) 5 13_666 ? O1 Pb3 S1 24.47(13) 13_666 13_666 ? S1 Pb3 S1 91.76(6) 17_666 13_666 ? S1 Pb3 S1 88.24(6) 5 13_666 ? S2 Pb4 S2 180.00(9) 23_575 11_645 ? S2 Pb4 S2 81.42(8) 23_575 20_556 ? S2 Pb4 S2 98.58(8) 11_645 20_556 ? S2 Pb4 S2 98.58(8) 23_575 8_664 ? S2 Pb4 S2 81.42(8) 11_645 8_664 ? S2 Pb4 S2 180.0 20_556 8_664 ? S2 Pb4 S2 81.42(8) 23_575 13_666 ? S2 Pb4 S2 98.58(8) 11_645 13_666 ? S2 Pb4 S2 81.42(8) 20_556 13_666 ? S2 Pb4 S2 98.58(8) 8_664 13_666 ? S2 Pb4 S2 98.58(8) 23_575 1_554 ? S2 Pb4 S2 81.42(8) 11_645 1_554 ? S2 Pb4 S2 98.58(8) 20_556 1_554 ? S2 Pb4 S2 81.42(8) 8_664 1_554 ? S2 Pb4 S2 180.00(10) 13_666 1_554 ? S2 Pb4 O2 57.60(15) 23_575 13_666 ? S2 Pb4 O2 122.40(15) 11_645 13_666 ? S2 Pb4 O2 117.94(14) 20_556 13_666 ? S2 Pb4 O2 62.06(14) 8_664 13_666 ? S2 Pb4 O2 50.73(13) 13_666 13_666 ? S2 Pb4 O2 129.27(13) 1_554 13_666 ? S2 Pb4 O2 122.40(15) 23_575 1_554 ? S2 Pb4 O2 57.60(15) 11_645 1_554 ? S2 Pb4 O2 62.06(14) 20_556 1_554 ? S2 Pb4 O2 117.94(14) 8_664 1_554 ? S2 Pb4 O2 129.27(13) 13_666 1_554 ? S2 Pb4 O2 50.73(13) 1_554 1_554 ? O2 Pb4 O2 180.0 13_666 1_554 ? S2 Pb4 O2 117.94(14) 23_575 20_556 ? S2 Pb4 O2 62.06(14) 11_645 20_556 ? S2 Pb4 O2 50.73(13) 20_556 20_556 ? S2 Pb4 O2 129.27(13) 8_664 20_556 ? S2 Pb4 O2 57.60(15) 13_666 20_556 ? S2 Pb4 O2 122.40(15) 1_554 20_556 ? O2 Pb4 O2 108.13(14) 13_666 20_556 ? O2 Pb4 O2 71.87(14) 1_554 20_556 ? S2 Pb4 O2 62.06(14) 23_575 8_664 ? S2 Pb4 O2 117.94(14) 11_645 8_664 ? S2 Pb4 O2 129.27(13) 20_556 8_664 ? S2 Pb4 O2 50.73(13) 8_664 8_664 ? S2 Pb4 O2 122.40(15) 13_666 8_664 ? S2 Pb4 O2 57.60(15) 1_554 8_664 ? O2 Pb4 O2 71.87(14) 13_666 8_664 ? O2 Pb4 O2 108.13(14) 1_554 8_664 ? O2 Pb4 O2 180.0 20_556 8_664 ? S2 Pb4 O2 50.73(13) 23_575 23_575 ? S2 Pb4 O2 129.27(13) 11_645 23_575 ? S2 Pb4 O2 57.60(15) 20_556 23_575 ? S2 Pb4 O2 122.40(15) 8_664 23_575 ? S2 Pb4 O2 117.94(14) 13_666 23_575 ? S2 Pb4 O2 62.06(14) 1_554 23_575 ? O2 Pb4 O2 108.13(14) 13_666 23_575 ? O2 Pb4 O2 71.87(14) 1_554 23_575 ? O2 Pb4 O2 108.13(14) 20_556 23_575 ? O2 Pb4 O2 71.87(14) 8_664 23_575 ? S2 Pb4 O2 129.27(13) 23_575 11_645 ? S2 Pb4 O2 50.73(13) 11_645 11_645 ? S2 Pb4 O2 122.40(15) 20_556 11_645 ? S2 Pb4 O2 57.60(15) 8_664 11_645 ? S2 Pb4 O2 62.06(14) 13_666 11_645 ? S2 Pb4 O2 117.94(14) 1_554 11_645 ? O2 Pb4 O2 71.87(14) 13_666 11_645 ? O2 Pb4 O2 108.13(14) 1_554 11_645 ? O2 Pb4 O2 71.87(14) 20_556 11_645 ? O2 Pb4 O2 108.13(14) 8_664 11_645 ? O2 Pb4 O2 180.0(2) 23_575 11_645 ? S2 Pb4 S1 61.49(6) 23_575 13_666 ? S2 Pb4 S1 118.51(6) 11_645 13_666 ? S2 Pb4 S1 100.37(6) 20_556 13_666 ? S2 Pb4 S1 79.63(6) 8_664 13_666 ? S2 Pb4 S1 30.30(6) 13_666 13_666 ? S2 Pb4 S1 149.70(6) 1_554 13_666 ? O2 Pb4 S1 21.22(13) 13_666 13_666 ? O2 Pb4 S1 158.78(13) 1_554 13_666 ? O2 Pb4 S1 87.86(15) 20_556 13_666 ? O2 Pb4 S1 92.14(15) 8_664 13_666 ? O2 Pb4 S1 110.09(13) 23_575 13_666 ? O2 Pb4 S1 69.91(13) 11_645 13_666 ? S2 Pb4 S1 118.51(6) 23_575 1_554 ? S2 Pb4 S1 61.49(6) 11_645 1_554 ? S2 Pb4 S1 79.63(6) 20_556 1_554 ? S2 Pb4 S1 100.37(6) 8_664 1_554 ? S2 Pb4 S1 149.70(6) 13_666 1_554 ? S2 Pb4 S1 30.30(6) 1_554 1_554 ? O2 Pb4 S1 158.78(13) 13_666 1_554 ? O2 Pb4 S1 21.22(13) 1_554 1_554 ? O2 Pb4 S1 92.14(15) 20_556 1_554 ? O2 Pb4 S1 87.86(15) 8_664 1_554 ? O2 Pb4 S1 69.91(13) 23_575 1_554 ? O2 Pb4 S1 110.09(13) 11_645 1_554 ? S1 Pb4 S1 180.0 13_666 1_554 ? S2 Pb4 S1 100.37(6) 23_575 20_556 ? S2 Pb4 S1 79.63(6) 11_645 20_556 ? S2 Pb4 S1 30.30(6) 20_556 20_556 ? S2 Pb4 S1 149.70(6) 8_664 20_556 ? S2 Pb4 S1 61.49(6) 13_666 20_556 ? S2 Pb4 S1 118.51(6) 1_554 20_556 ? O2 Pb4 S1 110.09(13) 13_666 20_556 ? O2 Pb4 S1 69.91(13) 1_554 20_556 ? O2 Pb4 S1 21.22(13) 20_556 20_556 ? O2 Pb4 S1 158.78(13) 8_664 20_556 ? O2 Pb4 S1 87.86(15) 23_575 20_556 ? O2 Pb4 S1 92.14(15) 11_645 20_556 ? S1 Pb4 S1 88.92(5) 13_666 20_556 ? S1 Pb4 S1 91.08(5) 1_554 20_556 ? O1 S1 O2 112.5(5) . . ? O1 S1 O3 110.0(4) . . ? O2 S1 O3 111.8(5) . . ? O1 S1 S2 110.2(4) . . ? O2 S1 S2 106.1(4) . . ? O3 S1 S2 106.0(4) . . ? O1 S1 Pb3 68.8(3) . . ? O2 S1 Pb3 122.9(4) . . ? O3 S1 Pb3 41.8(3) . . ? S2 S1 Pb3 127.74(13) . . ? O1 S1 Pb1 160.3(3) . 3_656 ? O2 S1 Pb1 75.0(4) . 3_656 ? O3 S1 Pb1 51.3(3) . 3_656 ? S2 S1 Pb1 83.64(11) . 3_656 ? Pb3 S1 Pb1 91.80(6) . 3_656 ? O1 S1 Pb2 110.4(3) . 14_765 ? O2 S1 Pb2 137.0(4) . 14_765 ? O3 S1 Pb2 53.2(3) . 14_765 ? S2 S1 Pb2 55.41(10) . 14_765 ? Pb3 S1 Pb2 75.45(5) . 14_765 ? Pb1 S1 Pb2 65.25(4) 3_656 14_765 ? O1 S1 Pb1 58.2(3) . 8_665 ? O2 S1 Pb1 143.7(4) . 8_665 ? O3 S1 Pb1 103.9(3) . 8_665 ? S2 S1 Pb1 56.19(10) . 8_665 ? Pb3 S1 Pb1 88.23(5) . 8_665 ? Pb1 S1 Pb1 126.67(7) 3_656 8_665 ? Pb2 S1 Pb1 63.26(4) 14_765 8_665 ? O1 S1 Pb1 92.9(4) . 17_666 ? O2 S1 Pb1 27.1(3) . 17_666 ? O3 S1 Pb1 104.1(3) . 17_666 ? S2 S1 Pb1 132.30(13) . 17_666 ? Pb3 S1 Pb1 99.18(6) . 17_666 ? Pb1 S1 Pb1 87.19(5) 3_656 17_666 ? Pb2 S1 Pb1 151.41(7) 14_765 17_666 ? Pb1 S1 Pb1 145.30(7) 8_665 17_666 ? O1 S1 Pb4 113.8(3) . 1_556 ? O2 S1 Pb4 57.8(3) . 1_556 ? O3 S1 Pb4 135.4(3) . 1_556 ? S2 S1 Pb4 50.60(10) . 1_556 ? Pb3 S1 Pb4 177.13(8) . 1_556 ? Pb1 S1 Pb4 85.71(5) 3_656 1_556 ? Pb2 S1 Pb4 102.17(6) 14_765 1_556 ? Pb1 S1 Pb4 92.11(5) 8_665 1_556 ? Pb1 S1 Pb4 82.14(5) 17_666 1_556 ? O1 S1 Pb1 26.0(3) . . ? O2 S1 Pb1 99.7(4) . . ? O3 S1 Pb1 135.5(3) . . ? S2 S1 Pb1 93.82(11) . . ? Pb3 S1 Pb1 94.76(6) . . ? Pb1 S1 Pb1 173.16(7) 3_656 . ? Pb2 S1 Pb1 118.35(6) 14_765 . ? Pb1 S1 Pb1 55.61(3) 8_665 . ? Pb1 S1 Pb1 89.87(5) 17_666 . ? Pb4 S1 Pb1 87.77(5) 1_556 . ? S1 S2 Pb4 99.10(12) . 1_556 ? S1 S2 Pb2 93.21(12) . 14_765 ? Pb4 S2 Pb2 151.21(10) 1_556 14_765 ? S1 S2 Pb1 92.60(12) . 8_665 ? Pb4 S2 Pb1 126.31(9) 1_556 8_665 ? Pb2 S2 Pb1 78.58(6) 14_765 8_665 ? S1 S2 Pb1 66.18(10) . 3_656 ? Pb4 S2 Pb1 93.36(7) 1_556 3_656 ? Pb2 S2 Pb1 68.00(5) 14_765 3_656 ? Pb1 S2 Pb1 138.36(8) 8_665 3_656 ? S1 S2 Pb1 146.66(13) . 24_657 ? Pb4 S2 Pb1 93.21(6) 1_556 24_657 ? Pb2 S2 Pb1 63.63(5) 14_765 24_657 ? Pb1 S2 Pb1 104.81(7) 8_665 24_657 ? Pb1 S2 Pb1 82.35(5) 3_656 24_657 ? S1 O1 Pb1 141.5(4) . . ? S1 O1 Pb3 86.8(3) . . ? Pb1 O1 Pb3 131.7(2) . . ? S1 O1 Pb1 100.2(4) . 8_665 ? Pb1 O1 Pb1 73.19(17) . 8_665 ? Pb3 O1 Pb1 102.0(2) . 8_665 ? S1 O2 Pb1 138.9(5) . 17_666 ? S1 O2 Pb4 101.0(4) . 1_556 ? Pb1 O2 Pb4 115.0(3) 17_666 1_556 ? S1 O2 Pb1 81.9(4) . 3_656 ? Pb1 O2 Pb1 112.0(3) 17_666 3_656 ? Pb4 O2 Pb1 95.9(2) 1_556 3_656 ? S1 O3 Pb3 116.0(4) . . ? S1 O3 Pb1 106.0(4) . 3_656 ? Pb3 O3 Pb1 134.7(3) . 3_656 ? S1 O3 Pb2 105.3(4) . 14_765 ? Pb3 O3 Pb2 101.6(2) . 14_765 ? Pb1 O3 Pb2 82.0(2) 3_656 14_765 ? Pb1 OH4 Pb1 103.6(3) . 11_646 ? Pb1 OH4 Pb2 106.2(3) . . ? Pb1 OH4 Pb2 104.2(3) 11_646 . ? Pb1 OH4 Pb1 117.2(2) . 19_566 ? Pb1 OH4 Pb1 136.5(2) 11_646 19_566 ? Pb2 OH4 Pb1 79.45(18) . 19_566 ? Pb1 OH4 Pb1 65.68(15) . 8_665 ? Pb1 OH4 Pb1 65.38(15) 11_646 8_665 ? Pb2 OH4 Pb1 67.07(15) . 8_665 ? Pb1 OH4 Pb1 145.0(2) 19_566 8_665 ? Pb1 OH4 H4 118(7) . . ? Pb1 OH4 H4 111(6) 11_646 . ? Pb2 OH4 H4 112(7) . . ? Pb1 OH4 H4 35(7) 19_566 . ? Pb1 OH4 H4 176(7) 8_665 . ? Pb1 OH5 Pb1 107.8(3) . 11_646 ? Pb1 OH5 Pb1 107.8(3) . 8_665 ? Pb1 OH5 Pb1 107.8(3) 11_646 8_665 ? Pb1 OH5 Pb2 68.9(3) . . ? Pb1 OH5 Pb2 68.9(3) 11_646 . ? Pb1 OH5 Pb2 68.9(3) 8_665 . ? Pb1 OH5 H5 111.1(3) . . ? Pb1 OH5 H5 111.1(3) 11_646 . ? Pb1 OH5 H5 111.1(3) 8_665 . ? Pb2 OH5 H5 180.0(12) . . ? 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 OH4 H4 O1 0.96(3) 2.23(5) 3.150(11) 159(9) 19_566 OH5 H5 S2 0.97(3) 2.700(17) 3.300(8) 120.3(6) . OH5 H5 S2 0.97(3) 2.700(17) 3.300(8) 120.3(6) 8_665 OH5 H5 S2 0.97(3) 2.700(17) 3.300(8) 120.3(6) 11_646 _refine_diff_density_max 2.025 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.408 _shelx_res_file ; TITL Redmond5 Redmond5.res created by SHELXL-2016/6 at 09:32:36 on 12-Sep-2021 CELL 0.71075 14.91790 14.91790 14.91790 90.00000 90.00000 90.00000 ZERR 24 0.00131 0.00131 0.00131 0.00000 0.00000 0.00000 LATT 1 SYMM .50+X, .50-Y, -Z SYMM -X, .50+Y, .50-Z SYMM .50-X, -Y, .50+Z SYMM +Z, +X, +Y SYMM .50+Z, .50-X, -Y SYMM -Z, .50+X, .50-Y SYMM .50-Z, -X, .50+Y SYMM +Y, +Z, +X SYMM .50+Y, .50-Z, -X SYMM -Y, .50+Z, .50-X SYMM .50-Y, -Z, .50+X SFAC O PB S H UNIT 104 40 48 32 L.S. 20 omit 7 10 15 omit 2 1 3 omit 1 0 2 CONN 15 3.0 PB1 CONN 15 3.0 PB2 CONN 15 3.0 PB3 CONN 15 3.0 PB4 FMAP 2 PLAN 20 ACTA BOND $H EQIV $12 z, -x+1/2, y+1/2 HTAB OH4 O1_$12 HTAB OH5 S2 EQIV $2 -z+3/2, -x+1, y+1/2 HTAB OH5 S2_$2 EQIV $3 -y+1, z-1/2, -x+3/2 HTAB OH5 S2_$3 DFIX 0.97 0.03 OH4 H4 OH5 H5 SIZE 0.170 0.170 0.130 WGHT 0.030800 15.500000 EXTI 0.000349 FVAR 0.06355 PB1 2 0.583145 0.226000 0.751689 11.00000 0.00935 0.01903 = 0.01806 -0.00083 -0.00061 -0.00393 PB2 2 0.824826 0.175174 0.675174 10.33333 0.01511 0.01511 = 0.01511 -0.00244 0.00244 0.00244 PB3 2 0.500000 0.500000 0.500000 10.16667 0.02039 0.02039 = 0.02039 -0.00519 -0.00519 -0.00519 PB4 2 0.500000 0.500000 0.000000 10.16667 0.03440 0.03440 = 0.03440 -0.00528 0.00528 0.00528 S1 3 0.498881 0.493872 0.734904 11.00000 0.01391 0.01166 = 0.00997 -0.00114 0.00123 0.00082 S2 3 0.594734 0.538796 0.819496 11.00000 0.01443 0.01687 = 0.01975 -0.00212 -0.00498 -0.00370 O1 1 0.524690 0.407655 0.697471 11.00000 0.03487 0.01191 = 0.02101 -0.00238 0.00484 0.00369 O2 1 0.416609 0.488656 0.787459 11.00000 0.01058 0.04192 = 0.02822 -0.00542 0.00625 -0.00329 O3 1 0.492347 0.561239 0.663018 11.00000 0.03215 0.01868 = 0.02029 0.00506 -0.00513 0.01102 OH4 1 0.717751 0.154518 0.797817 11.00000 0.01393 0.00770 = 0.01800 0.00400 0.00486 0.00207 H4 4 0.714901 0.092957 0.816914 11.00000 -1.50000 OH5 1 0.669191 0.330809 0.830809 10.33333 0.00869 0.00869 = 0.00869 -0.00078 0.00078 0.00078 H5 4 0.631497 0.368503 0.868503 10.33333 -1.50000 HKLF 4 REM Redmond5 REM R1 = 0.0353 for 1090 Fo > 4sig(Fo) and 0.0438 for all 1274 data REM 79 parameters refined using 2 restraints END WGHT 0.0307 15.7556 REM Highest difference peak 2.025, deepest hole -1.599, 1-sigma level 0.408 Q1 1 0.7526 0.0831 0.7303 11.00000 0.05 1.92 Q2 1 0.5842 0.4219 0.7435 11.00000 0.05 1.74 Q3 1 0.5895 0.2988 0.7043 11.00000 0.05 1.55 Q4 1 0.7755 0.1672 0.7479 11.00000 0.05 1.51 Q5 1 0.7385 0.0968 0.7206 11.00000 0.05 1.49 Q6 1 0.5125 0.3406 0.6529 11.00000 0.05 1.46 Q7 1 0.4774 0.6706 0.6591 11.00000 0.05 1.45 Q8 1 0.5839 0.4161 0.9161 10.33333 0.05 1.43 Q9 1 0.6498 0.2741 0.7453 11.00000 0.05 1.40 Q10 1 0.3545 0.5116 0.8295 11.00000 0.05 1.38 Q11 1 0.4211 0.5397 0.7479 11.00000 0.05 1.36 Q12 1 0.5805 0.1541 0.7073 11.00000 0.05 1.34 Q13 1 0.5782 0.5607 0.5929 11.00000 0.05 1.33 Q14 1 0.6991 0.3009 0.8009 10.33333 0.05 1.25 Q15 1 0.6254 0.2283 0.6771 11.00000 0.05 1.23 Q16 1 0.5009 0.4993 0.8417 11.00000 0.05 1.22 Q17 1 0.6745 0.4792 0.8421 11.00000 0.05 1.16 Q18 1 0.7369 0.1192 0.7191 11.00000 0.05 1.15 Q19 1 0.5900 0.2918 0.8001 11.00000 0.05 1.15 Q20 1 0.6849 0.2822 0.7965 11.00000 0.05 1.12 ; _shelx_res_checksum 99586 _shelx_hkl_file ; 0 -2 -1 28.63 1.74 -1 0 -2 29.34 1.39 0 2 1 32.72 1.78 1 0 2 26.11 1.41 1 0 -2 38.48 2.95 -1 2 0 20.80 1.06 1 -2 0 22.89 1.08 0 -1 -2 14.92 1.79 0 1 2 23.43 1.90 2 -1 -1 75.23 3.79 1 -2 -1 87.10 2.93 -1 2 1 85.45 4.29 1 -1 -2 67.09 3.92 -1 -1 -2 83.03 2.78 -1 1 2 63.84 4.19 1 1 2 83.04 3.86 -1 1 -2 62.25 2.06 0 2 2 1507.21 53.55 0 -2 -2 1489.05 48.81 -2 0 -2 1556.83 40.68 2 -2 0 1389.11 39.44 2 0 2 1577.22 41.47 -2 2 0 1120.39 34.62 0 0 3 6.55 2.14 0 0 -3 -0.06 2.13 -1 -2 -2 400.76 10.84 -1 2 2 347.96 11.12 -2 2 -1 370.39 6.36 2 -1 -2 336.81 13.70 2 1 2 417.29 9.53 1 -2 -2 357.44 11.22 1 2 2 411.98 10.94 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13.12 -1 7 18 20.39 25.01 18 -1 -7 1.50 18.59 1 7 18 2.23 23.94 -7 18 -1 -8.88 10.42 -1 7 -18 -3.59 12.02 9 2 17 55.38 22.49 9 2 -17 35.31 32.89 9 -2 -17 47.81 31.33 7 6 17 -4.72 21.89 7 6 -17 35.71 25.73 -6 17 7 20.10 31.75 17 -7 -6 2.02 18.39 10 7 15 0.02 41.86 10 7 -15 77.69 46.81 15 -10 -7 78.27 21.83 -7 15 10 103.57 40.29 19 -2 -3 0.13 34.67 2 3 -19 261.47 42.32 -2 3 -19 143.47 45.86 -3 19 -2 195.63 29.40 19 -3 -2 -0.39 11.71 3 2 -19 0.29 14.76 3 -2 -19 -0.63 14.85 13 6 -13 17.49 26.60 -6 13 13 12.95 26.90 13 6 13 0.22 13.10 13 -6 -13 11.86 20.16 13 3 -14 29.99 48.11 -3 14 13 76.36 32.71 13 3 14 30.13 21.69 14 -13 -3 1.46 7.49 13 -3 -14 77.75 25.76 6 7 -17 -20.93 22.46 -7 17 6 2.98 19.26 17 -6 -7 -7.26 14.03 6 7 17 7.99 21.00 7 -1 -18 1.37 21.76 7 1 -18 23.58 23.39 15 7 10 -0.01 10.57 -10 15 7 -1.16 17.86 5 5 18 -2.93 37.68 5 5 -18 15.03 23.50 18 -5 -5 18.12 14.93 -9 17 2 93.19 25.85 2 9 -17 92.52 50.26 17 -2 -9 73.48 36.45 17 2 -9 59.52 41.49 2 9 17 81.06 43.67 -2 9 17 34.68 48.03 -2 9 -17 45.55 19.77 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1218