data_zincochenite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'zincochenite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H6 O14 Pb4 S2 Zn' _chemical_formula_weight 1188.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 5.883(4) _cell_length_b 7.938(5) _cell_length_c 7.948(5) _cell_angle_alpha 110.511(12) _cell_angle_beta 98.497(10) _cell_angle_gamma 100.152(8) _cell_volume 333.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 560 _cell_measurement_theta_min 7.9 _cell_measurement_theta_max 24.9 _exptl_crystal_description 'tablet' _exptl_crystal_colour 'blue' _exptl_crystal_density_diffrn 5.922 _exptl_crystal_F_000 508 _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 52.514 _shelx_estimated_absorpt_T_min 0.145 _shelx_estimated_absorpt_T_max 0.420 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.470 _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 4558 _diffrn_reflns_av_unetI/netI 0.0962 _diffrn_reflns_av_R_equivalents 0.1446 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.122 _diffrn_reflns_theta_max 24.961 _diffrn_reflns_theta_full 24.961 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.991 _reflns_number_total 1152 _reflns_number_gt 936 _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^)+(0.1829P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1152 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2558 _refine_ls_wR_factor_gt 0.2321 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.36858(18) 0.25660(15) 0.48590(14) 0.0253(6) Uani 1 1 d . . . . . Pb2 Pb 0.55923(18) 0.26894(15) 0.04665(15) 0.0246(6) Uani 1 1 d . . . . . Zn Zn 0.000000 0.000000 0.000000 0.0242(11) Uani 1 2 d S . P . . S S 0.0582(12) 0.7424(10) 0.2688(11) 0.0253(17) Uani 1 1 d . . . . . OH1 O 0.217(3) 0.239(3) 0.183(2) 0.024(5) Uani 1 1 d . . . . . OH2 O 0.280(3) -0.038(3) -0.122(2) 0.025(5) Uani 1 1 d . . . . . OH3 O 0.319(4) 0.561(3) 0.596(3) 0.031(5) Uani 1 1 d . . . . . O4 O -0.195(3) 0.683(3) 0.184(3) 0.030(5) Uani 1 1 d . . . . . O5 O 0.178(4) 0.591(3) 0.216(3) 0.038(5) Uani 1 1 d . . . . . O6 O 0.104(3) 0.827(3) 0.471(3) 0.031(5) Uani 1 1 d . . . . . O7 O 0.169(4) 0.896(3) 0.213(3) 0.027(5) 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 0.0310(9) 0.0210(9) 0.0233(8) 0.0074(6) 0.0079(6) 0.0058(6) Pb2 0.0293(9) 0.0191(9) 0.0265(9) 0.0086(6) 0.0098(6) 0.0061(6) Zn 0.023(2) 0.019(3) 0.023(2) 0.0026(19) 0.0019(17) 0.0006(19) S 0.029(4) 0.019(4) 0.028(4) 0.008(3) 0.010(3) 0.005(3) OH1 0.039(11) 0.021(11) 0.003(9) 0.004(8) -0.002(7) -0.006(9) OH2 0.016(9) 0.018(10) 0.019(10) -0.010(8) -0.008(7) -0.007(8) OH3 0.047(12) 0.029(12) 0.020(10) 0.008(9) 0.022(9) 0.008(10) O4 0.018(10) 0.044(14) 0.045(13) 0.026(11) 0.023(8) 0.017(9) O5 0.064(15) 0.015(11) 0.038(13) 0.004(10) 0.028(11) 0.015(11) O6 0.028(11) 0.014(11) 0.050(13) 0.012(10) 0.008(9) 0.007(9) O7 0.036(11) 0.021(11) 0.027(11) 0.007(9) 0.021(8) 0.004(9) _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 OH3 2.35(2) . ? Pb1 OH1 2.387(16) . ? Pb1 OH3 2.445(19) 2_666 ? Pb1 O7 2.82(2) 1_545 ? Pb1 O6 2.84(2) 2_566 ? Pb1 O4 2.87(2) 2_566 ? Pb1 O5 3.03(2) 2_666 ? Pb1 O6 3.28(2) 2_666 ? Pb1 S 3.398(7) 2_566 ? Pb1 O6 3.44(2) 1_545 ? Pb1 S 3.635(8) 2_666 ? Pb1 Zn 3.771(2) . ? Pb1 S 3.805(7) 1_545 ? Pb1 Pb1 3.815(3) 2_666 ? Pb1 Pb2 3.849(2) . ? Pb2 OH2 2.41(2) 2_655 ? Pb2 OH1 2.44(2) . ? Pb2 OH2 2.467(17) . ? Pb2 OH3 2.602(19) 2_666 ? Pb2 O4 2.78(2) 2_565 ? Pb2 O7 2.89(2) 2_665 ? Pb2 O4 3.07(2) 1_655 ? Pb2 O5 3.15(2) 2_665 ? Pb2 Zn 3.482(2) . ? Pb2 S 3.597(7) 2_665 ? Pb2 Zn 3.6192(19) 1_655 ? Pb2 O5 3.73(2) . ? Pb2 O5 3.81(2) 1_655 ? Pb2 OH1 3.93(2) 1_655 ? Zn OH1 2.005(18) 2 ? Zn OH1 2.005(18) . ? Zn OH2 2.04(2) 2 ? Zn OH2 2.04(2) . ? Zn O7 2.30(2) 2_565 ? Zn O7 2.30(2) 1_545 ? S O4 1.46(2) . ? S O5 1.47(2) . ? S O6 1.47(2) . ? S O7 1.51(2) . ? OH1 O5 2.77(3) . ? OH2 O6 2.98(3) 1_544 ? OH3 O6 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 OH3 Pb1 OH1 87.1(7) . . ? OH3 Pb1 OH3 74.7(7) . 2_666 ? OH1 Pb1 OH3 72.4(7) . 2_666 ? OH3 Pb1 O7 143.5(7) . 1_545 ? OH1 Pb1 O7 64.0(6) . 1_545 ? OH3 Pb1 O7 113.4(6) 2_666 1_545 ? OH3 Pb1 O6 81.9(6) . 2_566 ? OH1 Pb1 O6 89.3(6) . 2_566 ? OH3 Pb1 O6 150.7(7) 2_666 2_566 ? O7 Pb1 O6 76.3(6) 1_545 2_566 ? OH3 Pb1 O4 72.0(6) . 2_566 ? OH1 Pb1 O4 135.8(6) . 2_566 ? OH3 Pb1 O4 133.4(7) 2_666 2_566 ? O7 Pb1 O4 112.8(6) 1_545 2_566 ? O6 Pb1 O4 50.3(6) 2_566 2_566 ? OH3 Pb1 O5 85.8(6) . 2_666 ? OH1 Pb1 O5 140.7(6) . 2_666 ? OH3 Pb1 O5 68.4(6) 2_666 2_666 ? O7 Pb1 O5 130.6(6) 1_545 2_666 ? O6 Pb1 O5 127.7(6) 2_566 2_666 ? O4 Pb1 O5 77.5(6) 2_566 2_666 ? OH3 Pb1 O6 121.6(6) . 2_666 ? OH1 Pb1 O6 111.8(7) . 2_666 ? OH3 Pb1 O6 61.5(7) 2_666 2_666 ? O7 Pb1 O6 91.0(6) 1_545 2_666 ? O6 Pb1 O6 147.8(8) 2_566 2_666 ? O4 Pb1 O6 112.3(6) 2_566 2_666 ? O5 Pb1 O6 44.3(6) 2_666 2_666 ? OH3 Pb1 S 73.4(5) . 2_566 ? OH1 Pb1 S 112.1(5) . 2_566 ? OH3 Pb1 S 147.4(5) 2_666 2_566 ? O7 Pb1 S 96.4(4) 1_545 2_566 ? O6 Pb1 S 25.3(5) 2_566 2_566 ? O4 Pb1 S 25.1(4) 2_566 2_566 ? O5 Pb1 S 102.7(4) 2_666 2_566 ? O6 Pb1 S 134.0(4) 2_666 2_566 ? OH3 Pb1 O6 138.4(6) . 1_545 ? OH1 Pb1 O6 103.3(6) . 1_545 ? OH3 Pb1 O6 147.0(6) 2_666 1_545 ? O7 Pb1 O6 43.0(5) 1_545 1_545 ? O6 Pb1 O6 58.4(7) 2_566 1_545 ? O4 Pb1 O6 72.8(6) 2_566 1_545 ? O5 Pb1 O6 107.5(5) 2_666 1_545 ? O6 Pb1 O6 92.1(5) 2_666 1_545 ? S Pb1 O6 65.3(4) 2_566 1_545 ? OH3 Pb1 S 108.4(5) . 2_666 ? OH1 Pb1 S 134.3(5) . 2_666 ? OH3 Pb1 S 71.0(5) 2_666 2_666 ? O7 Pb1 S 107.7(4) 1_545 2_666 ? O6 Pb1 S 134.4(5) 2_566 2_666 ? O4 Pb1 S 89.8(4) 2_566 2_666 ? O5 Pb1 S 23.2(4) 2_666 2_666 ? O6 Pb1 S 23.9(4) 2_666 2_666 ? S Pb1 S 113.5(2) 2_566 2_666 ? O6 Pb1 S 92.9(4) 1_545 2_666 ? OH3 Pb1 Zn 108.7(5) . . ? OH1 Pb1 Zn 28.0(4) . . ? OH3 Pb1 Zn 95.4(5) 2_666 . ? O7 Pb1 Zn 37.5(4) 1_545 . ? O6 Pb1 Zn 75.5(5) 2_566 . ? O4 Pb1 Zn 125.6(4) 2_566 . ? O5 Pb1 Zn 155.2(4) 2_666 . ? O6 Pb1 Zn 111.8(4) 2_666 . ? S Pb1 Zn 100.82(14) 2_566 . ? O6 Pb1 Zn 75.3(4) 1_545 . ? S Pb1 Zn 135.01(12) 2_666 . ? OH3 Pb1 S 145.7(5) . 1_545 ? OH1 Pb1 S 82.1(5) . 1_545 ? OH3 Pb1 S 131.1(5) 2_666 1_545 ? O7 Pb1 S 20.3(4) 1_545 1_545 ? O6 Pb1 S 65.6(4) 2_566 1_545 ? O4 Pb1 S 93.7(5) 2_566 1_545 ? O5 Pb1 S 122.2(4) 2_666 1_545 ? O6 Pb1 S 92.5(4) 2_666 1_545 ? S Pb1 S 80.82(18) 2_566 1_545 ? O6 Pb1 S 22.7(4) 1_545 1_545 ? S Pb1 S 102.30(14) 2_666 1_545 ? Zn Pb1 S 54.30(12) . 1_545 ? OH3 Pb1 Pb1 38.2(4) . 2_666 ? OH1 Pb1 Pb1 77.0(5) . 2_666 ? OH3 Pb1 Pb1 36.5(5) 2_666 2_666 ? O7 Pb1 Pb1 138.6(4) 1_545 2_666 ? O6 Pb1 Pb1 118.2(4) 2_566 2_666 ? O4 Pb1 Pb1 104.5(5) 2_566 2_666 ? O5 Pb1 Pb1 73.7(4) 2_666 2_666 ? O6 Pb1 Pb1 91.0(4) 2_666 2_666 ? S Pb1 Pb1 111.31(13) 2_566 2_666 ? O6 Pb1 Pb1 176.5(3) 1_545 2_666 ? S Pb1 Pb1 89.24(12) 2_666 2_666 ? Zn Pb1 Pb1 104.96(5) . 2_666 ? S Pb1 Pb1 158.57(13) 1_545 2_666 ? OH3 Pb1 Pb2 96.3(4) . . ? OH1 Pb1 Pb2 37.5(5) . . ? OH3 Pb1 Pb2 41.8(5) 2_666 . ? O7 Pb1 Pb2 74.6(4) 1_545 . ? O6 Pb1 Pb2 126.5(5) 2_566 . ? O4 Pb1 Pb2 167.9(4) 2_566 . ? O5 Pb1 Pb2 105.3(4) 2_666 . ? O6 Pb1 Pb2 76.1(4) 2_666 . ? S Pb1 Pb2 149.39(14) 2_566 . ? O6 Pb1 Pb2 116.6(4) 1_545 . ? S Pb1 Pb2 97.08(12) 2_666 . ? Zn Pb1 Pb2 54.38(4) . . ? S Pb1 Pb2 94.60(12) 1_545 . ? Pb1 Pb1 Pb2 65.80(4) 2_666 . ? OH2 Pb2 OH1 96.5(6) 2_655 . ? OH2 Pb2 OH2 70.7(6) 2_655 . ? OH1 Pb2 OH2 68.7(7) . . ? OH2 Pb2 OH3 80.9(6) 2_655 2_666 ? OH1 Pb2 OH3 68.9(6) . 2_666 ? OH2 Pb2 OH3 124.9(6) . 2_666 ? OH2 Pb2 O4 143.5(6) 2_655 2_565 ? OH1 Pb2 O4 74.8(6) . 2_565 ? OH2 Pb2 O4 73.2(7) . 2_565 ? OH3 Pb2 O4 125.5(7) 2_666 2_565 ? OH2 Pb2 O7 68.8(7) 2_655 2_665 ? OH1 Pb2 O7 149.8(6) . 2_665 ? OH2 Pb2 O7 81.3(6) . 2_665 ? OH3 Pb2 O7 130.4(6) 2_666 2_665 ? O4 Pb2 O7 100.9(6) 2_565 2_665 ? OH2 Pb2 O4 125.9(5) 2_655 1_655 ? OH1 Pb2 O4 108.2(6) . 1_655 ? OH2 Pb2 O4 163.2(6) . 1_655 ? OH3 Pb2 O4 65.6(6) 2_666 1_655 ? O4 Pb2 O4 90.0(6) 2_565 1_655 ? O7 Pb2 O4 101.6(5) 2_665 1_655 ? OH2 Pb2 O5 112.6(6) 2_655 2_665 ? OH1 Pb2 O5 149.7(6) . 2_665 ? OH2 Pb2 O5 112.1(6) . 2_665 ? OH3 Pb2 O5 122.2(6) 2_666 2_665 ? O4 Pb2 O5 76.7(6) 2_565 2_665 ? O7 Pb2 O5 47.4(6) 2_665 2_665 ? O4 Pb2 O5 61.7(5) 1_655 2_665 ? OH2 Pb2 Zn 87.2(4) 2_655 . ? OH1 Pb2 Zn 34.1(4) . . ? OH2 Pb2 Zn 35.2(5) . . ? OH3 Pb2 Zn 99.7(4) 2_666 . ? O4 Pb2 Zn 65.6(4) 2_565 . ? O7 Pb2 Zn 116.4(4) 2_665 . ? O4 Pb2 Zn 137.4(3) 1_655 . ? O5 Pb2 Zn 135.2(4) 2_665 . ? OH2 Pb2 S 89.3(5) 2_655 2_665 ? OH1 Pb2 S 164.4(4) . 2_665 ? OH2 Pb2 S 100.0(5) . 2_665 ? OH3 Pb2 S 126.4(4) 2_666 2_665 ? O4 Pb2 S 92.0(4) 2_565 2_665 ? O7 Pb2 S 24.0(4) 2_665 2_665 ? O4 Pb2 S 79.4(4) 1_655 2_665 ? O5 Pb2 S 23.9(4) 2_665 2_665 ? Zn Pb2 S 132.54(12) . 2_665 ? OH2 Pb2 Zn 32.4(5) 2_655 1_655 ? OH1 Pb2 Zn 128.7(5) . 1_655 ? OH2 Pb2 Zn 83.3(5) . 1_655 ? OH3 Pb2 Zn 97.1(5) 2_666 1_655 ? O4 Pb2 Zn 137.4(5) 2_565 1_655 ? O7 Pb2 Zn 39.5(4) 2_665 1_655 ? O4 Pb2 Zn 109.6(3) 1_655 1_655 ? O5 Pb2 Zn 80.2(4) 2_665 1_655 ? Zn Pb2 Zn 111.85(5) . 1_655 ? S Pb2 Zn 57.25(12) 2_665 1_655 ? OH2 Pb2 O5 139.4(6) 2_655 . ? OH1 Pb2 O5 47.9(6) . . ? OH2 Pb2 O5 104.8(6) . . ? OH3 Pb2 O5 68.9(6) 2_666 . ? O4 Pb2 O5 56.6(6) 2_565 . ? O7 Pb2 O5 151.8(5) 2_665 . ? O4 Pb2 O5 65.0(5) 1_655 . ? O5 Pb2 O5 106.5(4) 2_665 . ? Zn Pb2 O5 72.4(3) . . ? S Pb2 O5 130.4(3) 2_665 . ? Zn Pb2 O5 166.0(4) 1_655 . ? OH2 Pb2 O5 89.1(5) 2_655 1_655 ? OH1 Pb2 O5 134.1(5) . 1_655 ? OH2 Pb2 O5 152.5(6) . 1_655 ? OH3 Pb2 O5 67.1(5) 2_666 1_655 ? O4 Pb2 O5 122.6(5) 2_565 1_655 ? O7 Pb2 O5 73.8(5) 2_665 1_655 ? O4 Pb2 O5 39.8(5) 1_655 1_655 ? O5 Pb2 O5 57.7(7) 2_665 1_655 ? Zn Pb2 O5 166.7(3) . 1_655 ? S Pb2 O5 60.1(3) 2_665 1_655 ? Zn Pb2 O5 70.0(3) 1_655 1_655 ? O5 Pb2 O5 102.7(5) . 1_655 ? OH2 Pb2 Pb1 72.9(5) 2_655 . ? OH1 Pb2 Pb1 36.6(4) . . ? OH2 Pb2 Pb1 87.2(5) . . ? OH3 Pb2 Pb1 38.8(4) 2_666 . ? O4 Pb2 Pb1 110.4(4) 2_565 . ? O7 Pb2 Pb1 141.8(4) 2_665 . ? O4 Pb2 Pb1 99.7(4) 1_655 . ? O5 Pb2 Pb1 160.7(4) 2_665 . ? Zn Pb2 Pb1 61.67(3) . . ? S Pb2 Pb1 157.58(13) 2_665 . ? Zn Pb2 Pb1 103.16(4) 1_655 . ? O5 Pb2 Pb1 66.5(3) . . ? O5 Pb2 Pb1 105.1(3) 1_655 . ? OH2 Pb2 OH1 48.5(5) 2_655 1_655 ? OH1 Pb2 OH1 133.5(6) . 1_655 ? OH2 Pb2 OH1 113.1(5) . 1_655 ? OH3 Pb2 OH1 75.1(5) 2_666 1_655 ? O4 Pb2 OH1 151.7(4) 2_565 1_655 ? O7 Pb2 OH1 55.3(5) 2_665 1_655 ? O4 Pb2 OH1 81.4(4) 1_655 1_655 ? O5 Pb2 OH1 75.5(5) 2_665 1_655 ? Zn Pb2 OH1 135.7(3) . 1_655 ? S Pb2 OH1 60.0(3) 2_665 1_655 ? Zn Pb2 OH1 30.4(3) 1_655 1_655 ? O5 Pb2 OH1 138.2(4) . 1_655 ? O5 Pb2 OH1 41.9(4) 1_655 1_655 ? Pb1 Pb2 OH1 97.6(2) . 1_655 ? OH1 Zn OH1 180.0 2 . ? OH1 Zn OH2 86.3(8) 2 2 ? OH1 Zn OH2 93.7(8) . 2 ? OH1 Zn OH2 93.7(8) 2 . ? OH1 Zn OH2 86.3(8) . . ? OH2 Zn OH2 180.0 2 . ? OH1 Zn O7 80.2(7) 2 2_565 ? OH1 Zn O7 99.8(7) . 2_565 ? OH2 Zn O7 87.9(8) 2 2_565 ? OH2 Zn O7 92.1(8) . 2_565 ? OH1 Zn O7 99.8(7) 2 1_545 ? OH1 Zn O7 80.2(7) . 1_545 ? OH2 Zn O7 92.1(8) 2 1_545 ? OH2 Zn O7 87.9(8) . 1_545 ? O7 Zn O7 180.0(8) 2_565 1_545 ? OH1 Zn Pb2 43.0(6) 2 2 ? OH1 Zn Pb2 137.0(6) . 2 ? OH2 Zn Pb2 44.1(5) 2 2 ? OH2 Zn Pb2 135.9(5) . 2 ? O7 Zn Pb2 88.5(5) 2_565 2 ? O7 Zn Pb2 91.5(5) 1_545 2 ? OH1 Zn Pb2 137.0(6) 2 . ? OH1 Zn Pb2 43.0(6) . . ? OH2 Zn Pb2 135.9(5) 2 . ? OH2 Zn Pb2 44.1(5) . . ? O7 Zn Pb2 91.5(5) 2_565 . ? O7 Zn Pb2 88.5(5) 1_545 . ? Pb2 Zn Pb2 180.0 2 . ? OH1 Zn Pb2 96.5(6) 2 1_455 ? OH1 Zn Pb2 83.5(6) . 1_455 ? OH2 Zn Pb2 39.2(6) 2 1_455 ? OH2 Zn Pb2 140.8(6) . 1_455 ? O7 Zn Pb2 53.0(5) 2_565 1_455 ? O7 Zn Pb2 127.0(5) 1_545 1_455 ? Pb2 Zn Pb2 68.15(5) 2 1_455 ? Pb2 Zn Pb2 111.85(5) . 1_455 ? OH1 Zn Pb2 83.5(6) 2 2_655 ? OH1 Zn Pb2 96.5(6) . 2_655 ? OH2 Zn Pb2 140.8(6) 2 2_655 ? OH2 Zn Pb2 39.2(6) . 2_655 ? O7 Zn Pb2 127.0(5) 2_565 2_655 ? O7 Zn Pb2 53.0(5) 1_545 2_655 ? Pb2 Zn Pb2 111.85(5) 2 2_655 ? Pb2 Zn Pb2 68.15(5) . 2_655 ? Pb2 Zn Pb2 180.00(4) 1_455 2_655 ? OH1 Zn Pb1 146.1(5) 2 . ? OH1 Zn Pb1 33.9(5) . . ? OH2 Zn Pb1 84.1(4) 2 . ? OH2 Zn Pb1 95.9(4) . . ? O7 Zn Pb1 131.7(5) 2_565 . ? O7 Zn Pb1 48.3(5) 1_545 . ? Pb2 Zn Pb1 116.05(3) 2 . ? Pb2 Zn Pb1 63.95(3) . . ? Pb2 Zn Pb1 96.39(4) 1_455 . ? Pb2 Zn Pb1 83.61(4) 2_655 . ? OH1 Zn Pb1 33.9(5) 2 2 ? OH1 Zn Pb1 146.1(5) . 2 ? OH2 Zn Pb1 95.9(4) 2 2 ? OH2 Zn Pb1 84.1(4) . 2 ? O7 Zn Pb1 48.3(5) 2_565 2 ? O7 Zn Pb1 131.7(5) 1_545 2 ? Pb2 Zn Pb1 63.95(3) 2 2 ? Pb2 Zn Pb1 116.05(3) . 2 ? Pb2 Zn Pb1 83.61(4) 1_455 2 ? Pb2 Zn Pb1 96.39(4) 2_655 2 ? Pb1 Zn Pb1 180.0 . 2 ? O4 S O5 113.1(13) . . ? O4 S O6 111.7(12) . . ? O5 S O6 108.8(13) . . ? O4 S O7 108.2(13) . . ? O5 S O7 109.9(12) . . ? O6 S O7 104.8(12) . . ? O4 S Pb1 56.7(9) . 2_566 ? O5 S Pb1 122.4(9) . 2_566 ? O6 S Pb1 55.6(8) . 2_566 ? O7 S Pb1 127.5(9) . 2_566 ? O4 S Pb2 115.1(9) . 2_665 ? O5 S Pb2 60.8(9) . 2_665 ? O6 S Pb2 132.1(9) . 2_665 ? O7 S Pb2 50.9(8) . 2_665 ? Pb1 S Pb2 171.6(3) 2_566 2_665 ? O4 S Pb1 159.6(9) . 2_666 ? O5 S Pb1 54.5(9) . 2_666 ? O6 S Pb1 64.5(8) . 2_666 ? O7 S Pb1 91.9(9) . 2_666 ? Pb1 S Pb1 113.5(2) 2_566 2_666 ? Pb2 S Pb1 74.83(14) 2_665 2_666 ? O4 S Pb1 119.9(10) . 1_565 ? O5 S Pb1 124.9(9) . 1_565 ? O6 S Pb1 64.7(8) . 1_565 ? O7 S Pb1 40.2(8) . 1_565 ? Pb1 S Pb1 99.18(18) 2_566 1_565 ? Pb2 S Pb1 83.43(14) 2_665 1_565 ? Pb1 S Pb1 77.70(14) 2_666 1_565 ? O4 S Pb2 43.0(9) . 1_455 ? O5 S Pb2 72.7(9) . 1_455 ? O6 S Pb2 113.5(9) . 1_455 ? O7 S Pb2 138.5(9) . 1_455 ? Pb1 S Pb2 68.26(12) 2_566 1_455 ? Pb2 S Pb2 107.32(19) 2_665 1_455 ? Pb1 S Pb2 118.24(19) 2_666 1_455 ? Pb1 S Pb2 162.3(2) 1_565 1_455 ? O4 S Pb2 22.8(9) . 2_565 ? O5 S Pb2 122.5(10) . 2_565 ? O6 S Pb2 120.4(8) . 2_565 ? O7 S Pb2 85.5(9) . 2_565 ? Pb1 S Pb2 71.51(14) 2_566 2_565 ? Pb2 S Pb2 100.14(19) 2_665 2_565 ? Pb1 S Pb2 174.9(2) 2_666 2_565 ? Pb1 S Pb2 102.87(17) 1_565 2_565 ? Pb2 S Pb2 62.00(11) 1_455 2_565 ? Zn OH1 Pb1 118.1(8) . . ? Zn OH1 Pb2 102.9(8) . . ? Pb1 OH1 Pb2 105.9(7) . . ? Zn OH1 O5 125.8(10) . . ? Pb1 OH1 O5 107.1(8) . . ? Pb2 OH1 O5 91.2(7) . . ? Zn OH1 Pb2 66.1(5) . 1_455 ? Pb1 OH1 Pb2 119.3(7) . 1_455 ? Pb2 OH1 Pb2 133.5(6) . 1_455 ? O5 OH1 Pb2 66.6(6) . 1_455 ? Zn OH1 Pb1 174.1(8) . 2_666 ? Pb1 OH1 Pb1 67.7(4) . 2_666 ? Pb2 OH1 Pb1 75.9(4) . 2_666 ? O5 OH1 Pb1 48.8(6) . 2_666 ? Pb2 OH1 Pb1 110.4(5) 1_455 2_666 ? Zn OH2 Pb2 108.4(9) . 2_655 ? Zn OH2 Pb2 100.6(7) . . ? Pb2 OH2 Pb2 109.3(6) 2_655 . ? Zn OH2 O6 108.5(8) . 1_544 ? Pb2 OH2 O6 109.7(7) 2_655 1_544 ? Pb2 OH2 O6 119.5(9) . 1_544 ? Zn OH2 Pb1 159.3(6) . 2_655 ? Pb2 OH2 Pb1 70.8(5) 2_655 2_655 ? Pb2 OH2 Pb1 99.0(6) . 2_655 ? O6 OH2 Pb1 55.1(5) 1_544 2_655 ? Zn OH2 Pb1 66.2(4) . 2 ? Pb2 OH2 Pb1 113.0(5) 2_655 2 ? Pb2 OH2 Pb1 137.7(7) . 2 ? O6 OH2 Pb1 43.8(4) 1_544 2 ? Pb1 OH2 Pb1 94.7(4) 2_655 2 ? Pb1 OH3 Pb1 105.3(7) . 2_666 ? Pb1 OH3 Pb2 114.2(8) . 2_666 ? Pb1 OH3 Pb2 99.4(7) 2_666 2_666 ? Pb1 OH3 O6 141.7(9) . . ? Pb1 OH3 O6 73.1(7) 2_666 . ? Pb2 OH3 O6 103.5(8) 2_666 . ? S O4 Pb2 145.5(12) . 2_565 ? S O4 Pb1 98.2(11) . 2_566 ? Pb2 O4 Pb1 102.2(6) 2_565 2_566 ? S O4 Pb2 118.1(11) . 1_455 ? Pb2 O4 Pb2 90.0(6) 2_565 1_455 ? Pb1 O4 Pb2 88.9(5) 2_566 1_455 ? S O5 OH1 150.8(14) . . ? S O5 Pb1 102.3(11) . 2_666 ? OH1 O5 Pb1 87.7(8) . 2_666 ? S O5 Pb2 95.2(10) . 2_665 ? OH1 O5 Pb2 112.2(8) . 2_665 ? Pb1 O5 Pb2 90.6(6) 2_666 2_665 ? S O5 Pb2 168.3(12) . . ? OH1 O5 Pb2 40.8(5) . . ? Pb1 O5 Pb2 75.3(5) 2_666 . ? Pb2 O5 Pb2 73.5(4) 2_665 . ? S O5 Pb2 85.7(10) . 1_455 ? OH1 O5 Pb2 71.6(6) . 1_455 ? Pb1 O5 Pb2 145.7(7) 2_666 1_455 ? Pb2 O5 Pb2 122.3(7) 2_665 1_455 ? Pb2 O5 Pb2 102.7(5) . 1_455 ? S O5 Pb1 131.2(11) . . ? OH1 O5 Pb1 33.3(4) . . ? Pb1 O5 Pb1 61.9(4) 2_666 . ? Pb2 O5 Pb1 128.3(7) 2_665 . ? Pb2 O5 Pb1 58.2(3) . . ? Pb2 O5 Pb1 87.5(4) 1_455 . ? S O6 Pb1 99.1(10) . 2_566 ? S O6 OH3 104.1(11) . . ? Pb1 O6 OH3 102.3(7) 2_566 . ? S O6 Pb1 91.6(9) . 2_666 ? Pb1 O6 Pb1 147.8(8) 2_566 2_666 ? OH3 O6 Pb1 45.4(5) . 2_666 ? S O6 Pb1 92.6(10) . 1_565 ? Pb1 O6 Pb1 121.6(6) 2_566 1_565 ? OH3 O6 Pb1 129.8(8) . 1_565 ? Pb1 O6 Pb1 87.9(5) 2_666 1_565 ? S O7 Zn 128.6(12) . 1_565 ? S O7 Pb1 119.5(11) . 1_565 ? Zn O7 Pb1 94.2(7) 1_565 1_565 ? S O7 Pb2 105.1(10) . 2_665 ? Zn O7 Pb2 87.5(6) 1_565 2_665 ? Pb1 O7 Pb2 119.1(7) 1_565 2_665 ? S O7 Pb1 65.8(8) . 2_666 ? Zn O7 Pb1 162.3(7) 1_565 2_666 ? Pb1 O7 Pb1 84.8(5) 1_565 2_666 ? Pb2 O7 Pb1 77.7(5) 2_665 2_666 ? S O7 Pb2 170.4(11) . 1_565 ? Zn O7 Pb2 57.5(4) 1_565 1_565 ? Pb1 O7 Pb2 64.1(4) 1_565 1_565 ? Pb2 O7 Pb2 66.4(4) 2_665 1_565 ? Pb1 O7 Pb2 106.8(4) 2_666 1_565 ? _refine_diff_density_max 8.206 _refine_diff_density_min -7.576 _refine_diff_density_rms 1.125 _shelx_res_file ; TITL zincochenite R14.res created by SHELXL-2016/6 at 11:12:42 on 26-Feb-2022 CELL 0.71075 5.88280 7.93760 7.94800 110.51100 98.49710 100.15200 ZERR 1 0.00360 0.00470 0.00460 0.01230 0.00980 0.00840 LATT 1 SFAC H O PB S ZN UNIT 6 14 4 2 1 L.S. 20 CONN 15 3.0 PB1 CONN 15 3.0 PB2 EQIV $1 x, y-1, z-1 BIND OH1 O5 BIND OH2 O6_$1 BIND OH3 O6 FMAP 2 PLAN 20 ACTA SIZE 0.060 0.040 0.020 WGHT 0.182900 FVAR 0.35385 PB1 3 0.368580 0.256600 0.485905 11.00000 0.03100 0.02097 = 0.02327 0.00738 0.00792 0.00585 PB2 3 0.559228 0.268937 0.046647 11.00000 0.02930 0.01905 = 0.02646 0.00856 0.00980 0.00615 ZN 5 0.000000 0.000000 0.000000 10.50000 0.02324 0.01867 = 0.02314 0.00265 0.00186 0.00059 S 4 0.058185 0.742443 0.268772 11.00000 0.02935 0.01868 = 0.02774 0.00807 0.00965 0.00458 OH1 2 0.217343 0.239359 0.183115 11.00000 0.03857 0.02148 = 0.00307 0.00416 -0.00168 -0.00582 OH2 2 0.279753 -0.038215 -0.121630 11.00000 0.01571 0.01759 = 0.01871 -0.01022 -0.00755 -0.00748 OH3 2 0.318850 0.561165 0.596141 11.00000 0.04715 0.02895 = 0.01975 0.00795 0.02243 0.00776 O4 2 -0.195029 0.683268 0.184282 11.00000 0.01754 0.04422 = 0.04454 0.02623 0.02310 0.01683 O5 2 0.178443 0.591315 0.216131 11.00000 0.06358 0.01506 = 0.03847 0.00404 0.02790 0.01502 O6 2 0.103722 0.827396 0.471378 11.00000 0.02786 0.01400 = 0.04988 0.01175 0.00836 0.00736 O7 2 0.169003 0.896423 0.213375 11.00000 0.03601 0.02079 = 0.02682 0.00695 0.02092 0.00449 HKLF 4 REM zincochenite REM R1 = 0.0874 for 936 Fo > 4sig(Fo) and 0.0959 for all 1152 data REM 97 parameters refined using 0 restraints END WGHT 0.1829 0.0000 REM Highest difference peak 8.206, deepest hole -7.576, 1-sigma level 1.125 Q1 1 0.7078 0.2223 -0.0273 11.00000 0.05 5.52 Q2 1 0.5139 0.2199 0.4141 11.00000 0.05 5.36 Q3 1 0.3961 0.1252 0.4801 11.00000 0.05 5.20 Q4 1 -0.1743 0.7623 0.0790 11.00000 0.05 5.14 Q5 1 0.3059 0.3475 0.4571 11.00000 0.05 4.88 Q6 1 0.6055 0.1634 0.0592 11.00000 0.05 4.82 Q7 1 0.5021 0.3744 0.0388 11.00000 0.05 4.02 Q8 1 0.2655 0.2790 0.6207 11.00000 0.05 3.61 Q9 1 0.4448 0.3536 0.6573 11.00000 0.05 3.55 Q10 1 0.1440 0.2499 0.3755 11.00000 0.05 3.55 Q11 1 0.4689 0.2141 0.6432 11.00000 0.05 2.93 Q12 1 0.6108 0.3479 0.2153 11.00000 0.05 2.90 Q13 1 0.5660 0.5621 0.6270 11.00000 0.05 2.81 Q14 1 0.2461 0.7183 0.4004 11.00000 0.05 2.75 Q15 1 0.0710 0.4934 0.4808 11.00000 0.05 2.72 Q16 1 0.4981 0.1811 -0.1103 11.00000 0.05 2.68 Q17 1 0.4172 0.0271 0.0147 11.00000 0.05 2.63 Q18 1 0.5000 0.0000 0.0000 10.50000 0.05 2.56 Q19 1 0.3530 0.6696 0.5200 11.00000 0.05 2.49 Q20 1 0.2773 0.3496 0.0955 11.00000 0.05 2.44 ; _shelx_res_checksum 66685 _shelx_hkl_file ; 0 -1 1 238.36 20.89 0 1 -1 279.79 22.73 0 1 -1 312.44 15.13 0 -1 1 322.36 13.13 0 1 -1 291.48 23.87 0 -1 1 286.54 21.13 1 0 0 2811.36 103.94 -1 0 0 2592.75 90.08 -1 0 0 2862.76 120.84 -1 0 0 2860.87 97.87 1 0 0 2950.43 120.81 1 0 0 2963.09 97.57 1 -1 0 801.93 45.12 1 -1 0 912.95 54.32 -1 1 0 791.97 41.10 -1 1 0 926.18 60.13 1 -1 0 916.89 58.13 1 0 -1 9.05 2.40 1 0 -1 6.87 2.37 1 0 -1 8.69 4.03 -1 0 1 8.11 4.03 0 -1 -1 31.98 3.48 0 1 1 36.81 3.50 -1 1 -1 4048.56 176.89 1 -1 1 3947.52 194.26 1 -1 1 3725.59 209.56 -1 1 -1 3544.32 173.01 -1 1 -1 4397.26 173.26 1 -1 1 3803.75 152.12 -1 -1 1 876.80 53.18 1 1 -1 917.19 53.65 -1 -1 1 833.14 37.45 1 1 -1 882.50 38.92 -1 1 1 77.81 8.04 1 -1 -1 86.31 12.10 1 -1 -1 130.32 16.95 1 0 1 59.68 7.87 1 0 1 45.44 11.53 -1 0 -1 69.92 6.95 -1 0 -1 45.84 11.29 -1 0 -1 64.90 8.59 1 0 1 65.77 7.31 -1 -1 0 18.73 4.65 1 1 0 20.72 4.90 1 1 0 22.65 7.27 -1 -1 0 16.22 6.92 0 1 -2 596.05 35.51 0 1 -2 600.24 15.96 0 -1 2 497.54 40.73 0 -1 2 343.92 45.44 0 1 -2 417.32 49.04 0 2 -1 235.10 24.04 0 -2 1 153.20 20.05 0 -2 1 177.96 20.24 0 0 -2 7494.55 420.15 0 0 -2 8397.24 367.23 0 0 2 8195.10 386.77 0 -2 0 8429.92 655.73 0 2 0 8448.35 503.58 0 -2 0 8699.65 493.51 -1 2 0 3457.77 242.06 1 -2 0 3149.53 220.93 -1 2 -1 660.47 81.13 1 -2 1 983.68 98.88 1 -2 1 1048.93 72.50 -1 2 -1 935.98 95.82 -1 0 2 6108.64 404.37 1 0 -2 7489.99 297.42 1 0 -2 6798.27 390.77 -1 -1 2 516.94 18.00 1 1 -2 624.59 28.96 1 1 -2 594.87 41.48 -1 -1 2 507.21 29.27 -1 -1 2 508.60 33.60 1 1 -2 513.66 24.13 0 -2 2 3504.67 284.41 0 -2 2 3834.32 173.66 0 2 -2 3978.96 264.37 0 2 -2 4020.13 193.19 0 -2 2 3172.43 239.65 0 2 -2 3556.25 262.79 1 -1 2 497.04 40.80 1 -1 2 554.69 31.93 -1 1 -2 470.95 34.74 -1 1 -2 589.04 25.87 -1 1 -2 643.44 52.93 1 -1 2 482.74 41.02 -1 -1 -1 6035.63 267.45 1 1 1 6036.72 256.23 1 1 1 6032.30 375.34 1 1 1 6454.47 312.37 -1 -1 -1 6034.98 367.22 -1 -2 1 227.62 31.72 -1 -2 1 241.02 23.80 1 2 -1 335.95 27.46 1 2 -1 280.41 35.16 2 -1 0 263.94 23.76 2 -1 0 226.57 28.30 2 -1 0 259.46 30.92 -2 1 0 126.07 33.40 -2 1 0 257.06 20.89 -2 1 0 317.44 32.84 -1 2 1 172.27 20.18 1 -2 -1 187.68 23.30 1 -1 -2 2298.32 54.43 2 0 -1 3080.00 128.48 -2 0 1 3281.32 207.41 2 0 -1 2736.87 128.05 2 0 -1 3272.77 199.34 1 -2 2 4010.45 287.11 -1 2 -2 4641.44 350.63 1 -2 2 3900.30 304.03 1 -2 2 3718.97 177.90 -1 2 -2 3384.83 257.00 0 1 2 218.34 14.20 0 1 2 241.57 13.23 0 -2 -1 172.93 13.92 0 2 1 176.00 14.92 0 -2 -1 202.54 23.31 -2 0 0 689.37 44.15 2 0 0 780.62 59.32 -2 0 0 760.36 43.18 2 0 0 644.36 31.44 2 0 0 672.97 39.28 -2 0 0 757.17 57.75 1 2 -2 9183.60 623.77 -1 -2 2 7076.73 499.52 1 2 -2 9999.00 668.20 -1 -2 2 7928.29 491.90 -1 -2 2 7479.13 462.59 1 0 2 3247.25 175.09 1 0 2 3140.71 142.28 -1 0 -2 3146.21 171.47 -1 0 -2 2924.90 155.47 1 0 2 2804.36 148.87 -1 0 -2 2919.40 166.97 2 -1 -1 5373.69 281.00 -2 1 1 5053.40 254.68 2 -1 -1 4683.55 321.75 -2 1 1 5235.24 361.30 1 2 0 4801.12 256.67 1 2 0 5144.37 344.04 -1 -2 0 4791.76 320.22 -1 -2 0 4676.24 249.69 0 1 -3 3816.44 208.00 0 -1 3 2712.05 221.74 0 1 -3 3097.19 159.52 0 1 -3 3828.06 154.40 0 -1 3 3432.48 179.27 -2 1 -1 6310.47 364.40 2 -1 1 6688.79 373.89 2 -1 1 5391.95 340.16 2 -1 1 5498.74 323.17 -2 1 -1 6242.51 419.48 -2 1 -1 6050.05 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210.75 -1 4 -9 -11.10 54.66 1 -4 9 59.54 39.14 1 -4 9 33.45 34.82 -1 4 -9 50.22 21.03 2 5 -9 10.28 55.61 2 5 -9 48.58 45.81 -2 -5 9 49.57 21.24 6 -1 3 47.02 75.52 -6 1 -3 79.83 71.88 -6 1 -3 140.66 57.65 6 -1 3 87.88 47.26 6 -1 3 136.17 64.70 1 -3 9 510.88 171.35 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 44880