data_finescreekite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'finescreekite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H4 O10 Pb4 S4' _chemical_formula_weight 1121.03 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 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.2330(9) _cell_length_b 10.7128(13) _cell_length_c 14.8256(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1307.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4335 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 23.3 _exptl_crystal_description 'blade' _exptl_crystal_colour 'colorless' _exptl_crystal_density_diffrn 5.694 _exptl_crystal_F_000 1904 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 52.021 _shelx_estimated_absorpt_T_min 0.056 _shelx_estimated_absorpt_T_max 0.423 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.188 _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 4466 _diffrn_reflns_av_unetI/netI 0.1329 _diffrn_reflns_av_R_equivalents 0.1826 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.121 _diffrn_reflns_theta_max 22.212 _diffrn_reflns_theta_full 22.212 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measured_fraction_theta_full 0.968 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_Laue_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_point_group_measured_fraction_full 0.960 _reflns_number_total 1588 _reflns_number_gt 1440 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.670 _reflns_Friedel_fraction_max 0.948 _reflns_Friedel_fraction_full 0.948 _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^)+(0.0644P)^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_abs_structure_details ; Flack x determined using 473 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 1588 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.5288(3) 0.46920(17) 0.40954(17) 0.0320(6) Uani 1 1 d . . . . . Pb2 Pb 0.5729(3) 0.28370(18) 0.63933(16) 0.0335(7) Uani 1 1 d . . . . . Pb3 Pb 0.3270(3) 0.57895(18) 0.63324(17) 0.0361(7) Uani 1 1 d . . . . . Pb4 Pb 0.7935(3) 0.59033(18) 0.60469(17) 0.0353(6) Uani 1 1 d . . . . . S1 S 0.0827(17) 0.5336(11) 0.4275(10) 0.029(3) Uani 1 1 d . . . . . S1A S 0.8725(16) 0.6112(11) 0.3848(9) 0.028(3) Uani 1 1 d . . . . . S2 S 0.0037(19) 0.3111(11) 0.7295(11) 0.035(4) Uani 1 1 d . . . . . S2A S 0.2221(19) 0.2224(14) 0.7160(10) 0.039(4) Uani 1 1 d . . . . . O1 O 0.188(5) 0.502(3) 0.352(3) 0.042(11) Uani 1 1 d . . . . . O2 O 0.159(6) 0.624(3) 0.488(3) 0.053(13) Uani 1 1 d . . . . . O3 O 0.044(5) 0.419(3) 0.482(3) 0.045(11) Uani 1 1 d . . . . . O4 O 0.965(4) 0.298(3) 0.822(2) 0.027(9) Uani 1 1 d . . . . . O5 O 0.892(4) 0.250(3) 0.668(4) 0.059(14) Uani 1 1 d . . . . . O6 O 0.018(5) 0.448(3) 0.708(4) 0.058(14) Uani 1 1 d . . . . . OH7 O 0.703(5) 0.385(3) 0.530(3) 0.044(10) Uani 1 1 d . . . . . OH8 O 0.378(5) 0.397(3) 0.549(3) 0.039(10) Uani 1 1 d . . . . . OH9 O 0.537(4) 0.626(3) 0.529(3) 0.034(10) Uani 1 1 d . . . . . OH10 O 0.586(4) 0.493(3) 0.689(2) 0.025(8) Uiso 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 0.0331(12) 0.0266(11) 0.0362(14) -0.0021(10) -0.0005(11) -0.0004(9) Pb2 0.0305(13) 0.0251(10) 0.0448(15) 0.0049(11) -0.0010(12) -0.0012(9) Pb3 0.0298(12) 0.0357(12) 0.0428(14) -0.0036(11) 0.0034(11) 0.0054(10) Pb4 0.0274(12) 0.0353(11) 0.0432(14) -0.0017(10) -0.0001(12) -0.0071(10) S1 0.027(7) 0.020(6) 0.038(9) -0.004(6) -0.001(7) 0.003(6) S1A 0.025(7) 0.030(7) 0.030(8) 0.004(6) -0.004(6) 0.004(6) S2 0.031(9) 0.028(7) 0.047(11) -0.006(7) -0.007(8) -0.003(7) S2A 0.030(9) 0.045(8) 0.042(9) 0.005(8) 0.004(7) 0.005(7) O1 0.04(3) 0.04(2) 0.04(3) -0.007(19) 0.04(2) 0.00(2) O2 0.05(3) 0.019(18) 0.09(3) 0.00(2) -0.02(3) 0.019(19) O3 0.05(3) 0.033(19) 0.05(3) 0.01(2) -0.02(2) -0.001(19) O4 0.012(18) 0.042(19) 0.03(2) -0.003(17) 0.011(18) 0.007(17) O5 0.02(2) 0.03(2) 0.13(4) -0.01(3) -0.01(3) 0.011(17) O6 0.04(3) 0.04(2) 0.09(4) 0.04(2) -0.03(3) 0.01(2) OH7 0.05(3) 0.036(19) 0.05(2) 0.02(2) -0.02(2) -0.02(2) OH8 0.06(3) 0.024(17) 0.04(2) 0.007(18) 0.02(2) -0.002(18) OH9 0.03(2) 0.033(17) 0.04(2) -0.026(19) 0.00(2) -0.015(17) _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 OH9 2.45(3) . ? Pb1 OH7 2.46(4) . ? Pb1 OH8 2.53(4) . ? Pb1 O4 2.81(3) 2_664 ? Pb1 O5 2.85(4) 3_456 ? Pb1 O1 2.96(4) . ? Pb1 O6 3.14(6) 2_564 ? Pb1 S2A 3.195(16) 3_556 ? Pb1 S1A 3.234(13) . ? Pb1 S2 3.568(15) 2_564 ? Pb1 S2 3.649(14) 3_556 ? Pb1 O2 3.65(4) . ? Pb2 OH7 2.23(4) . ? Pb2 OH10 2.36(3) . ? Pb2 OH8 2.42(4) . ? Pb2 O5 2.69(4) . ? Pb2 O3 2.83(4) 3_556 ? Pb2 S2A 3.172(16) . ? Pb2 O1 3.20(3) 3_556 ? Pb2 S1 3.542(12) 3_556 ? Pb2 Pb3 3.757(3) . ? Pb2 Pb4 3.788(3) . ? Pb2 S2 3.802(15) 1_655 ? Pb2 S1A 3.836(14) 2_665 ? Pb3 OH8 2.35(3) . ? Pb3 OH9 2.38(4) . ? Pb3 OH10 2.46(3) . ? Pb3 O2 2.60(4) . ? Pb3 O6 3.11(5) . ? Pb3 S1A 3.351(12) 3_466 ? Pb3 O1 3.35(4) 2_565 ? Pb3 O4 3.42(3) 4_656 ? Pb3 O3 3.66(4) . ? Pb3 S1 3.686(14) . ? Pb3 Pb4 3.866(3) . ? Pb4 OH10 2.36(3) . ? Pb4 OH9 2.42(4) . ? Pb4 OH7 2.58(3) . ? Pb4 O6 2.84(4) 1_655 ? Pb4 S2A 3.015(15) 4_656 ? Pb4 O4 3.18(3) 4_756 ? Pb4 O3 3.31(4) 1_655 ? Pb4 S1A 3.332(14) . ? Pb4 O2 3.49(5) 1_655 ? Pb4 O2 3.54(4) 3_566 ? Pb4 S1 3.597(14) 1_655 ? S1 O1 1.46(4) . ? S1 O2 1.46(4) . ? S1 O3 1.50(4) . ? S1 S1A 2.022(18) 1_455 ? S2 O4 1.41(4) 1_455 ? S2 O5 1.45(5) 1_455 ? S2 O6 1.51(4) . ? S2 S2A 2.04(2) . ? O3 OH8 2.93(6) . ? 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 OH9 Pb1 OH7 73.3(13) . . ? OH9 Pb1 OH8 68.5(12) . . ? OH7 Pb1 OH8 65.4(14) . . ? OH9 Pb1 O4 74.0(12) . 2_664 ? OH7 Pb1 O4 130.6(10) . 2_664 ? OH8 Pb1 O4 131.1(10) . 2_664 ? OH9 Pb1 O5 150.8(13) . 3_456 ? OH7 Pb1 O5 102.8(12) . 3_456 ? OH8 Pb1 O5 83.4(13) . 3_456 ? O4 Pb1 O5 123.3(13) 2_664 3_456 ? OH9 Pb1 O1 99.0(11) . . ? OH7 Pb1 O1 143.8(13) . . ? OH8 Pb1 O1 78.8(12) . . ? O4 Pb1 O1 77.3(10) 2_664 . ? O5 Pb1 O1 66.6(10) 3_456 . ? OH9 Pb1 O6 119.9(11) . 2_564 ? OH7 Pb1 O6 149.8(13) . 2_564 ? OH8 Pb1 O6 143.3(12) . 2_564 ? O4 Pb1 O6 46.5(9) 2_664 2_564 ? O5 Pb1 O6 78.3(13) 3_456 2_564 ? O1 Pb1 O6 64.8(11) . 2_564 ? OH9 Pb1 S2A 148.2(9) . 3_556 ? OH7 Pb1 S2A 84.0(11) . 3_556 ? OH8 Pb1 S2A 121.6(8) . 3_556 ? O4 Pb1 S2A 106.8(8) 2_664 3_556 ? O5 Pb1 S2A 55.3(9) 3_456 3_556 ? O1 Pb1 S2A 112.3(8) . 3_556 ? O6 Pb1 S2A 71.8(7) 2_564 3_556 ? OH9 Pb1 S1A 74.5(9) . . ? OH7 Pb1 S1A 75.3(9) . . ? OH8 Pb1 S1A 131.8(10) . . ? O4 Pb1 S1A 60.9(7) 2_664 . ? O5 Pb1 S1A 133.4(9) 3_456 . ? O1 Pb1 S1A 138.0(7) . . ? O6 Pb1 S1A 82.3(8) 2_564 . ? S2A Pb1 S1A 78.5(4) 3_556 . ? OH9 Pb1 S2 95.1(9) . 2_564 ? OH7 Pb1 S2 145.9(9) . 2_564 ? OH8 Pb1 S2 140.7(9) . 2_564 ? O4 Pb1 S2 21.6(7) 2_664 2_564 ? O5 Pb1 S2 102.1(11) 3_456 2_564 ? O1 Pb1 S2 68.5(7) . 2_564 ? O6 Pb1 S2 24.9(7) 2_564 2_564 ? S2A Pb1 S2 91.5(4) 3_556 2_564 ? S1A Pb1 S2 70.8(3) . 2_564 ? OH9 Pb1 S2 167.9(9) . 3_556 ? OH7 Pb1 S2 98.0(9) . 3_556 ? OH8 Pb1 S2 100.5(8) . 3_556 ? O4 Pb1 S2 117.9(7) 2_664 3_556 ? O5 Pb1 S2 21.6(9) 3_456 3_556 ? O1 Pb1 S2 83.0(7) . 3_556 ? O6 Pb1 S2 71.8(7) 2_564 3_556 ? S2A Pb1 S2 33.9(4) 3_556 3_556 ? S1A Pb1 S2 111.9(3) . 3_556 ? S2 Pb1 S2 96.66(8) 2_564 3_556 ? OH9 Pb1 O2 58.7(11) . . ? OH7 Pb1 O2 114.8(13) . . ? OH8 Pb1 O2 57.8(11) . . ? O4 Pb1 O2 76.3(10) 2_664 . ? O5 Pb1 O2 100.0(10) 3_456 . ? O1 Pb1 O2 41.4(10) . . ? O6 Pb1 O2 94.3(10) 2_564 . ? S2A Pb1 O2 153.1(7) 3_556 . ? S1A Pb1 O2 123.5(6) . . ? S2 Pb1 O2 83.0(7) 2_564 . ? S2 Pb1 O2 120.4(7) 3_556 . ? OH7 Pb2 OH10 75.2(13) . . ? OH7 Pb2 OH8 70.7(14) . . ? OH10 Pb2 OH8 74.0(12) . . ? OH7 Pb2 O5 73.4(16) . . ? OH10 Pb2 O5 92.0(11) . . ? OH8 Pb2 O5 143.7(13) . . ? OH7 Pb2 O3 87.1(12) . 3_556 ? OH10 Pb2 O3 158.4(12) . 3_556 ? OH8 Pb2 O3 88.7(12) . 3_556 ? O5 Pb2 O3 94.7(12) . 3_556 ? OH7 Pb2 S2A 143.0(11) . . ? OH10 Pb2 S2A 97.2(9) . . ? OH8 Pb2 S2A 72.4(9) . . ? O5 Pb2 S2A 143.6(12) . . ? O3 Pb2 S2A 89.5(9) 3_556 . ? OH7 Pb2 O1 110.7(13) . 3_556 ? OH10 Pb2 O1 151.6(11) . 3_556 ? OH8 Pb2 O1 134.3(10) . 3_556 ? O5 Pb2 O1 64.9(9) . 3_556 ? O3 Pb2 O1 47.1(11) 3_556 3_556 ? S2A Pb2 O1 93.2(8) . 3_556 ? OH7 Pb2 S1 104.5(10) . 3_556 ? OH10 Pb2 S1 175.7(9) . 3_556 ? OH8 Pb2 S1 110.0(9) . 3_556 ? O5 Pb2 S1 83.9(8) . 3_556 ? O3 Pb2 S1 24.1(9) 3_556 3_556 ? S2A Pb2 S1 85.5(4) . 3_556 ? O1 Pb2 S1 24.4(7) 3_556 3_556 ? OH7 Pb2 Pb3 80.3(11) . . ? OH10 Pb2 Pb3 39.8(8) . . ? OH8 Pb2 Pb3 37.4(9) . . ? O5 Pb2 Pb3 130.1(7) . . ? O3 Pb2 Pb3 125.8(9) 3_556 . ? S2A Pb2 Pb3 72.1(3) . . ? O1 Pb2 Pb3 164.6(7) 3_556 . ? S1 Pb2 Pb3 144.5(2) 3_556 . ? OH7 Pb2 Pb4 41.4(10) . . ? OH10 Pb2 Pb4 36.6(9) . . ? OH8 Pb2 Pb4 78.9(8) . . ? O5 Pb2 Pb4 70.7(7) . . ? O3 Pb2 Pb4 128.3(8) 3_556 . ? S2A Pb2 Pb4 131.6(3) . . ? O1 Pb2 Pb4 133.8(7) 3_556 . ? S1 Pb2 Pb4 141.6(2) 3_556 . ? Pb3 Pb2 Pb4 61.64(6) . . ? OH7 Pb2 S2 76.8(11) . 1_655 ? OH10 Pb2 S2 77.0(9) . 1_655 ? OH8 Pb2 S2 140.8(9) . 1_655 ? O5 Pb2 S2 16.6(9) . 1_655 ? O3 Pb2 S2 111.2(9) 3_556 1_655 ? S2A Pb2 S2 137.7(4) . 1_655 ? O1 Pb2 S2 77.5(6) 3_556 1_655 ? S1 Pb2 S2 98.7(3) 3_556 1_655 ? Pb3 Pb2 S2 116.5(2) . 1_655 ? Pb4 Pb2 S2 62.2(2) . 1_655 ? OH7 Pb2 S1A 119.6(10) . 2_665 ? OH10 Pb2 S1A 54.7(9) . 2_665 ? OH8 Pb2 S1A 117.1(9) . 2_665 ? O5 Pb2 S1A 76.8(12) . 2_665 ? O3 Pb2 S1A 146.9(8) 3_556 2_665 ? S2A Pb2 S1A 80.1(3) . 2_665 ? O1 Pb2 S1A 101.9(7) 3_556 2_665 ? S1 Pb2 S1A 123.0(3) 3_556 2_665 ? Pb3 Pb2 S1A 80.7(2) . 2_665 ? Pb4 Pb2 S1A 79.5(2) . 2_665 ? S2 Pb2 S1A 62.2(3) 1_655 2_665 ? OH8 Pb3 OH9 72.7(11) . . ? OH8 Pb3 OH10 73.4(13) . . ? OH9 Pb3 OH10 70.6(12) . . ? OH8 Pb3 O2 78.8(13) . . ? OH9 Pb3 O2 79.0(15) . . ? OH10 Pb3 O2 143.6(13) . . ? OH8 Pb3 O6 87.8(12) . . ? OH9 Pb3 O6 157.6(13) . . ? OH10 Pb3 O6 114.8(10) . . ? O2 Pb3 O6 86.7(14) . . ? OH8 Pb3 S1A 139.3(9) . 3_466 ? OH9 Pb3 S1A 69.8(8) . 3_466 ? OH10 Pb3 S1A 107.5(7) . 3_466 ? O2 Pb3 S1A 79.1(8) . 3_466 ? O6 Pb3 S1A 124.5(8) . 3_466 ? OH8 Pb3 O1 107.9(10) . 2_565 ? OH9 Pb3 O1 135.2(11) . 2_565 ? OH10 Pb3 O1 67.2(11) . 2_565 ? O2 Pb3 O1 145.8(12) . 2_565 ? O6 Pb3 O1 60.7(10) . 2_565 ? S1A Pb3 O1 109.6(6) 3_466 2_565 ? OH8 Pb3 O4 142.8(12) . 4_656 ? OH9 Pb3 O4 119.4(10) . 4_656 ? OH10 Pb3 O4 142.9(10) . 4_656 ? O2 Pb3 O4 70.3(10) . 4_656 ? O6 Pb3 O4 70.5(9) . 4_656 ? S1A Pb3 O4 54.2(6) 3_466 4_656 ? O1 Pb3 O4 87.8(8) 2_565 4_656 ? OH8 Pb3 O3 53.0(13) . . ? OH9 Pb3 O3 99.5(11) . . ? OH10 Pb3 O3 125.4(9) . . ? O2 Pb3 O3 40.7(10) . . ? O6 Pb3 O3 59.1(12) . . ? S1A Pb3 O3 119.1(6) 3_466 . ? O1 Pb3 O3 116.6(9) 2_565 . ? O4 Pb3 O3 89.7(9) 4_656 . ? OH8 Pb3 S1 63.1(11) . . ? OH9 Pb3 S1 83.6(9) . . ? OH10 Pb3 S1 134.4(8) . . ? O2 Pb3 S1 18.2(7) . . ? O6 Pb3 S1 77.8(9) . . ? S1A Pb3 S1 97.2(3) 3_466 . ? O1 Pb3 S1 138.2(7) 2_565 . ? O4 Pb3 S1 82.5(6) 4_656 . ? O3 Pb3 S1 23.6(6) . . ? OH8 Pb3 Pb2 38.8(10) . . ? OH9 Pb3 Pb2 78.6(8) . . ? OH10 Pb3 Pb2 37.9(7) . . ? O2 Pb3 Pb2 117.4(8) . . ? O6 Pb3 Pb2 93.0(7) . . ? S1A Pb3 Pb2 140.9(2) 3_466 . ? O1 Pb3 Pb2 77.3(6) 2_565 . ? O4 Pb3 Pb2 161.9(5) 4_656 . ? O3 Pb3 Pb2 87.9(5) . . ? S1 Pb3 Pb2 101.71(19) . . ? OH8 Pb3 Pb4 78.0(10) . . ? OH9 Pb3 Pb4 36.7(9) . . ? OH10 Pb3 Pb4 35.8(8) . . ? O2 Pb3 Pb4 115.5(11) . . ? O6 Pb3 Pb4 150.0(6) . . ? S1A Pb3 Pb4 81.3(2) 3_466 . ? O1 Pb3 Pb4 98.6(6) 2_565 . ? O4 Pb3 Pb4 134.1(5) 4_656 . ? O3 Pb3 Pb4 125.4(7) . . ? S1 Pb3 Pb4 117.1(2) . . ? Pb2 Pb3 Pb4 59.58(5) . . ? OH10 Pb4 OH9 71.6(12) . . ? OH10 Pb4 OH7 68.9(12) . . ? OH9 Pb4 OH7 71.6(12) . . ? OH10 Pb4 O6 87.1(13) . 1_655 ? OH9 Pb4 O6 154.4(12) . 1_655 ? OH7 Pb4 O6 87.9(12) . 1_655 ? OH10 Pb4 S2A 73.2(9) . 4_656 ? OH9 Pb4 S2A 107.3(9) . 4_656 ? OH7 Pb4 S2A 140.3(10) . 4_656 ? O6 Pb4 S2A 78.7(11) 1_655 4_656 ? OH10 Pb4 O4 125.6(10) . 4_756 ? OH9 Pb4 O4 126.4(9) . 4_756 ? OH7 Pb4 O4 158.1(12) . 4_756 ? O6 Pb4 O4 77.5(10) 1_655 4_756 ? S2A Pb4 O4 52.8(7) 4_656 4_756 ? OH10 Pb4 O3 119.8(9) . 1_655 ? OH9 Pb4 O3 112.1(11) . 1_655 ? OH7 Pb4 O3 57.9(12) . 1_655 ? O6 Pb4 O3 66.0(13) 1_655 1_655 ? S2A Pb4 O3 140.6(8) 4_656 1_655 ? O4 Pb4 O3 100.9(9) 4_756 1_655 ? OH10 Pb4 S1A 133.5(9) . . ? OH9 Pb4 S1A 72.9(9) . . ? OH7 Pb4 S1A 72.0(9) . . ? O6 Pb4 S1A 115.8(12) 1_655 . ? S2A Pb4 S1A 147.1(4) 4_656 . ? O4 Pb4 S1A 99.6(6) 4_756 . ? O3 Pb4 S1A 51.5(7) 1_655 . ? OH10 Pb4 O2 158.7(9) . 1_655 ? OH9 Pb4 O2 120.5(12) . 1_655 ? OH7 Pb4 O2 97.1(12) . 1_655 ? O6 Pb4 O2 76.1(12) 1_655 1_655 ? S2A Pb4 O2 115.1(7) 4_656 1_655 ? O4 Pb4 O2 63.8(8) 4_756 1_655 ? O3 Pb4 O2 41.1(8) 1_655 1_655 ? S1A Pb4 O2 48.8(8) . 1_655 ? OH10 Pb4 O2 111.3(10) . 3_566 ? OH9 Pb4 O2 53.8(10) . 3_566 ? OH7 Pb4 O2 118.8(10) . 3_566 ? O6 Pb4 O2 151.3(11) 1_655 3_566 ? S2A Pb4 O2 85.6(8) 4_656 3_566 ? O4 Pb4 O2 73.9(9) 4_756 3_566 ? O3 Pb4 O2 117.5(10) 1_655 3_566 ? S1A Pb4 O2 67.7(8) . 3_566 ? O2 Pb4 O2 89.3(6) 1_655 3_566 ? OH10 Pb4 S1 142.3(8) . 1_655 ? OH9 Pb4 S1 105.4(9) . 1_655 ? OH7 Pb4 S1 74.5(10) . 1_655 ? O6 Pb4 S1 82.7(12) 1_655 1_655 ? S2A Pb4 S1 138.7(4) 4_656 1_655 ? O4 Pb4 S1 87.4(6) 4_756 1_655 ? O3 Pb4 S1 24.7(7) 1_655 1_655 ? S1A Pb4 S1 33.7(3) . 1_655 ? O2 Pb4 S1 23.8(7) 1_655 1_655 ? O2 Pb4 S1 93.9(7) 3_566 1_655 ? OH10 Pb4 Pb2 36.6(7) . . ? OH9 Pb4 Pb2 77.5(8) . . ? OH7 Pb4 Pb2 34.8(9) . . ? O6 Pb4 Pb2 76.9(8) 1_655 . ? S2A Pb4 Pb2 105.5(3) 4_656 . ? O4 Pb4 Pb2 149.4(6) 4_756 . ? O3 Pb4 Pb2 83.8(6) 1_655 . ? S1A Pb4 Pb2 106.5(2) . . ? O2 Pb4 Pb2 124.7(5) 1_655 . ? O2 Pb4 Pb2 130.9(7) 3_566 . ? S1 Pb4 Pb2 105.7(2) 1_655 . ? O1 S1 O2 112(3) . . ? O1 S1 O3 110(2) . . ? O2 S1 O3 108(2) . . ? O1 S1 S1A 111(2) . 1_455 ? O2 S1 S1A 107.0(16) . 1_455 ? O3 S1 S1A 108.8(18) . 1_455 ? O1 S1 Pb2 64.7(13) . 3_456 ? O2 S1 Pb2 144.5(15) . 3_456 ? O3 S1 Pb2 50.2(17) . 3_456 ? S1A S1 Pb2 106.7(6) 1_455 3_456 ? O1 S1 Pb4 174.0(17) . 1_455 ? O2 S1 Pb4 74(2) . 1_455 ? O3 S1 Pb4 66.9(17) . 1_455 ? S1A S1 Pb4 66.0(5) 1_455 1_455 ? Pb2 S1 Pb4 110.6(4) 3_456 1_455 ? O1 S1 Pb3 110.2(19) . . ? O2 S1 Pb3 33.7(14) . . ? O3 S1 Pb3 77.4(17) . . ? S1A S1 Pb3 132.2(7) 1_455 . ? Pb2 S1 Pb3 111.7(3) 3_456 . ? Pb4 S1 Pb3 74.6(3) 1_455 . ? O1 S1 Pb1 47.2(18) . . ? O2 S1 Pb1 75.0(18) . . ? O3 S1 Pb1 95.5(17) . . ? S1A S1 Pb1 153.2(7) 1_455 . ? Pb2 S1 Pb1 80.0(3) 3_456 . ? Pb4 S1 Pb1 137.1(4) 1_455 . ? Pb3 S1 Pb1 63.1(2) . . ? O1 S1 Pb4 84.2(14) . 3_466 ? O2 S1 Pb4 45.2(17) . 3_466 ? O3 S1 Pb4 152.7(18) . 3_466 ? S1A S1 Pb4 85.8(5) 1_455 3_466 ? Pb2 S1 Pb4 148.7(4) 3_456 3_466 ? Pb4 S1 Pb4 100.7(3) 1_455 3_466 ? Pb3 S1 Pb4 75.8(2) . 3_466 ? Pb1 S1 Pb4 77.0(2) . 3_466 ? S1 S1A Pb1 121.3(6) 1_655 . ? S1 S1A Pb4 80.4(6) 1_655 . ? Pb1 S1A Pb4 71.7(3) . . ? S1 S1A Pb3 121.9(6) 1_655 3_566 ? Pb1 S1A Pb3 112.2(4) . 3_566 ? Pb4 S1A Pb3 97.1(4) . 3_566 ? S1 S1A Pb2 108.5(6) 1_655 2_664 ? Pb1 S1A Pb2 110.4(4) . 2_664 ? Pb4 S1A Pb2 166.2(4) . 2_664 ? Pb3 S1A Pb2 69.3(2) 3_566 2_664 ? O4 S2 O5 115(3) 1_455 1_455 ? O4 S2 O6 109(3) 1_455 . ? O5 S2 O6 111(2) 1_455 . ? O4 S2 S2A 104.5(17) 1_455 . ? O5 S2 S2A 106.7(17) 1_455 . ? O6 S2 S2A 111(2) . . ? O4 S2 Pb1 47.4(15) 1_455 2_565 ? O5 S2 Pb1 136.0(18) 1_455 2_565 ? O6 S2 Pb1 61(2) . 2_565 ? S2A S2 Pb1 116.5(7) . 2_565 ? O4 S2 Pb1 118.6(15) 1_455 3_456 ? O5 S2 Pb1 46.3(14) 1_455 3_456 ? O6 S2 Pb1 133(2) . 3_456 ? S2A S2 Pb1 60.8(6) . 3_456 ? Pb1 S2 Pb1 165.9(5) 2_565 3_456 ? O4 S2 Pb4 54.0(14) 1_455 4_646 ? O5 S2 Pb4 113.7(16) 1_455 4_646 ? O6 S2 Pb4 135.2(19) . 4_646 ? S2A S2 Pb4 52.2(5) . 4_646 ? Pb1 S2 Pb4 87.7(4) 2_565 4_646 ? Pb1 S2 Pb4 80.1(3) 3_456 4_646 ? O4 S2 Pb2 96.9(16) 1_455 1_455 ? O5 S2 Pb2 32.0(16) 1_455 1_455 ? O6 S2 Pb2 94.2(17) . 1_455 ? S2A S2 Pb2 138.6(7) . 1_455 ? Pb1 S2 Pb2 104.1(4) 2_565 1_455 ? Pb1 S2 Pb2 77.9(3) 3_456 1_455 ? Pb4 S2 Pb2 126.1(4) 4_646 1_455 ? O4 S2 Pb4 115.6(15) 1_455 1_455 ? O5 S2 Pb4 76.7(15) 1_455 1_455 ? O6 S2 Pb4 36.0(16) . 1_455 ? S2A S2 Pb4 134.2(8) . 1_455 ? Pb1 S2 Pb4 79.4(3) 2_565 1_455 ? Pb1 S2 Pb4 112.7(4) 3_456 1_455 ? Pb4 S2 Pb4 167.1(4) 4_646 1_455 ? Pb2 S2 Pb4 58.7(2) 1_455 1_455 ? O4 S2 Pb3 123.1(16) 1_455 . ? O5 S2 Pb3 120(2) 1_455 . ? O6 S2 Pb3 37.5(19) . . ? S2A S2 Pb3 74.0(6) . . ? Pb1 S2 Pb3 81.4(2) 2_565 . ? Pb1 S2 Pb3 109.7(4) 3_456 . ? Pb4 S2 Pb3 111.7(4) 4_646 . ? Pb2 S2 Pb3 121.9(4) 1_455 . ? Pb4 S2 Pb3 66.1(2) 1_455 . ? O4 S2 Pb3 47.6(15) 1_455 4_546 ? O5 S2 Pb3 68(2) 1_455 4_546 ? O6 S2 Pb3 137(2) . 4_546 ? S2A S2 Pb3 110.0(6) . 4_546 ? Pb1 S2 Pb3 88.8(4) 2_565 4_546 ? Pb1 S2 Pb3 79.8(2) 3_456 4_546 ? Pb4 S2 Pb3 66.7(2) 4_646 4_546 ? Pb2 S2 Pb3 61.4(2) 1_455 4_546 ? Pb4 S2 Pb3 113.2(4) 1_455 4_546 ? Pb3 S2 Pb3 170.2(4) . 4_546 ? S2 S2A Pb4 95.4(7) . 4_646 ? S2 S2A Pb2 137.7(7) . . ? Pb4 S2A Pb2 116.9(5) 4_646 . ? S2 S2A Pb1 85.3(6) . 3_456 ? Pb4 S2A Pb1 101.0(4) 4_646 3_456 ? Pb2 S2A Pb1 112.2(5) . 3_456 ? S2 S2A Pb3 77.4(6) . . ? Pb4 S2A Pb3 135.2(5) 4_646 . ? Pb2 S2A Pb3 60.6(3) . . ? Pb1 S2A Pb3 121.9(4) 3_456 . ? S1 O1 Pb1 111(2) . . ? S1 O1 Pb2 91.0(15) . 3_456 ? Pb1 O1 Pb2 99.0(10) . 3_456 ? S1 O1 Pb3 142(2) . 2_564 ? Pb1 O1 Pb3 106.6(10) . 2_564 ? Pb2 O1 Pb3 77.6(8) 3_456 2_564 ? S1 O2 Pb3 128.2(18) . . ? S1 O2 Pb4 82(2) . 1_455 ? Pb3 O2 Pb4 91.8(14) . 1_455 ? S1 O2 Pb4 118(2) . 3_466 ? Pb3 O2 Pb4 108.4(13) . 3_466 ? Pb4 O2 Pb4 123.4(10) 1_455 3_466 ? S1 O2 Pb1 82.2(17) . . ? Pb3 O2 Pb1 74.9(9) . . ? Pb4 O2 Pb1 146.1(10) 1_455 . ? Pb4 O2 Pb1 90.5(11) 3_466 . ? S1 O3 Pb2 106(2) . 3_456 ? S1 O3 OH8 93(2) . . ? Pb2 O3 OH8 94.4(13) 3_456 . ? S1 O3 Pb4 88.4(16) . 1_455 ? Pb2 O3 Pb4 146.0(15) 3_456 1_455 ? OH8 O3 Pb4 116.1(15) . 1_455 ? S1 O3 Pb3 79.0(16) . . ? Pb2 O3 Pb3 134.0(14) 3_456 . ? OH8 O3 Pb3 39.9(9) . . ? Pb4 O3 Pb3 78.4(9) 1_455 . ? S2 O4 Pb1 110.9(18) 1_655 2_665 ? S2 O4 Pb4 105.0(17) 1_655 4_746 ? Pb1 O4 Pb4 116.7(12) 2_665 4_746 ? S2 O4 Pb3 114.7(18) 1_655 4_646 ? Pb1 O4 Pb3 122.0(10) 2_665 4_646 ? Pb4 O4 Pb3 83.8(8) 4_746 4_646 ? S2 O5 Pb2 131(2) 1_655 . ? S2 O5 Pb1 112.1(19) 1_655 3_556 ? Pb2 O5 Pb1 115.6(14) . 3_556 ? S2 O5 Pb4 81.9(14) 1_655 . ? Pb2 O5 Pb4 68.1(7) . . ? Pb1 O5 Pb4 139.8(18) 3_556 . ? S2 O5 Pb3 92(2) 1_655 4_646 ? Pb2 O5 Pb3 74.5(10) . 4_646 ? Pb1 O5 Pb3 95.8(10) 3_556 4_646 ? Pb4 O5 Pb3 122.1(11) . 4_646 ? S2 O6 Pb4 126(2) . 1_455 ? S2 O6 Pb3 125(2) . . ? Pb4 O6 Pb3 95.6(12) 1_455 . ? S2 O6 Pb1 94(2) . 2_565 ? Pb4 O6 Pb1 106.3(14) 1_455 2_565 ? Pb3 O6 Pb1 108.2(13) . 2_565 ? Pb2 OH7 Pb1 115.4(18) . . ? Pb2 OH7 Pb4 103.8(16) . . ? Pb1 OH7 Pb4 99.6(12) . . ? Pb2 OH7 O3 134.4(18) . 1_655 ? Pb1 OH7 O3 109.8(16) . 1_655 ? Pb4 OH7 O3 73.7(12) . 1_655 ? Pb2 OH7 Pb3 66.7(11) . . ? Pb1 OH7 Pb3 68.8(10) . . ? Pb4 OH7 Pb3 67.5(9) . . ? O3 OH7 Pb3 140.0(12) 1_655 . ? Pb3 OH8 Pb2 103.8(16) . . ? Pb3 OH8 Pb1 105.6(12) . . ? Pb2 OH8 Pb1 106.2(15) . . ? Pb3 OH8 O3 87.1(14) . . ? Pb2 OH8 O3 148.2(16) . . ? Pb1 OH8 O3 99.2(15) . . ? Pb3 OH8 Pb4 67.8(9) . . ? Pb2 OH8 Pb4 65.5(9) . . ? Pb1 OH8 Pb4 66.4(8) . . ? O3 OH8 Pb4 144.6(12) . . ? Pb3 OH9 Pb4 107.4(15) . . ? Pb3 OH9 Pb1 107.6(12) . . ? Pb4 OH9 Pb1 104.5(13) . . ? Pb3 OH9 O2 120.9(15) . 3_566 ? Pb4 OH9 O2 83.4(14) . 3_566 ? Pb1 OH9 O2 126.0(18) . 3_566 ? Pb3 OH9 Pb2 66.0(8) . . ? Pb4 OH9 Pb2 66.6(8) . . ? Pb1 OH9 Pb2 70.6(7) . . ? O2 OH9 Pb2 149.4(16) 3_566 . ? Pb3 OH9 Pb4 96.6(11) . 3_466 ? Pb4 OH9 Pb4 139.6(11) . 3_466 ? Pb1 OH9 Pb4 98.3(11) . 3_466 ? O2 OH9 Pb4 56.2(12) 3_566 3_466 ? Pb2 OH9 Pb4 153.7(9) . 3_466 ? Pb4 OH10 Pb2 106.8(13) . . ? Pb4 OH10 Pb3 106.6(13) . . ? Pb2 OH10 Pb3 102.3(13) . . ? Pb4 OH10 O1 150.7(13) . 2_565 ? Pb2 OH10 O1 102.3(12) . 2_565 ? Pb3 OH10 O1 69.4(10) . 2_565 ? _refine_diff_density_max 2.298 _refine_diff_density_min -2.981 _refine_diff_density_rms 0.577 _shelx_res_file ; TITL finescreekite JS73.res created by SHELXL-2016/6 at 19:34:11 on 20-Mar-2022 CELL 0.71075 8.23297 10.71280 14.82560 90.00000 90.00000 90.00000 ZERR 4 0.00091 0.00129 0.00134 0.00000 0.00000 0.00000 LATT -1 SYMM .50-X, -Y, .50+Z SYMM .50+X, .50-Y, -Z SYMM -X, .50+Y, .50-Z SFAC O PB S H UNIT 40 16 16 16 SHEL 99999 0.94 L.S. 20 omit 1 0 4 CONN 12 3.0 PB1 CONN 12 3.0 PB2 CONN 12 3.0 PB3 CONN 12 3.0 PB4 EQIV $1 x+1, y, z EQIV $2 x+0.5, -y+1.5, -z+1 EQIV $3 -x+0.5, -y+1, z+0.5 BIND OH7 O3_$1 BIND OH8 O3 BIND OH9 O2_$2 BIND OH10 O1_$3 FMAP 2 PLAN 20 ACTA SIZE 0.130 0.060 0.020 WGHT 0.064400 FVAR 0.17444 PB1 2 0.528805 0.469202 0.409537 11.00000 0.03306 0.02657 = 0.03623 -0.00206 -0.00050 -0.00037 PB2 2 0.572906 0.283696 0.639328 11.00000 0.03052 0.02513 = 0.04481 0.00495 -0.00097 -0.00118 PB3 2 0.326975 0.578951 0.633243 11.00000 0.02984 0.03569 = 0.04277 -0.00365 0.00342 0.00536 PB4 2 0.793478 0.590326 0.604688 11.00000 0.02738 0.03531 = 0.04318 -0.00174 -0.00006 -0.00705 S1 3 0.082663 0.533599 0.427527 11.00000 0.02729 0.02021 = 0.03809 -0.00407 -0.00141 0.00320 S1A 3 0.872511 0.611242 0.384799 11.00000 0.02508 0.02958 = 0.02961 0.00427 -0.00363 0.00442 S2 3 0.003725 0.311139 0.729529 11.00000 0.03093 0.02808 = 0.04661 -0.00593 -0.00718 -0.00314 S2A 3 0.222141 0.222431 0.715960 11.00000 0.03005 0.04542 = 0.04233 0.00517 0.00443 0.00490 O1 1 0.187827 0.501521 0.351572 11.00000 0.04471 0.03687 = 0.04360 -0.00736 0.03825 -0.00412 O2 1 0.159469 0.623546 0.488301 11.00000 0.05306 0.01909 = 0.08630 -0.00034 -0.01938 0.01896 O3 1 0.043774 0.418705 0.481757 11.00000 0.04736 0.03307 = 0.05485 0.01321 -0.02339 -0.00101 O4 1 0.964621 0.298175 0.821563 11.00000 0.01206 0.04231 = 0.02611 -0.00258 0.01060 0.00682 O5 1 0.892067 0.249956 0.668457 11.00000 0.02010 0.02628 = 0.12936 -0.01098 -0.00922 0.01109 O6 1 0.017978 0.448056 0.707936 11.00000 0.03752 0.04302 = 0.09439 0.03722 -0.03121 0.00918 OH7 1 0.702715 0.384732 0.529593 11.00000 0.04504 0.03556 = 0.05110 0.01731 -0.02106 -0.01506 OH8 1 0.377581 0.397240 0.548864 11.00000 0.05606 0.02408 = 0.03753 0.00704 0.02442 -0.00211 OH9 1 0.537357 0.626485 0.529028 11.00000 0.03233 0.03262 = 0.03834 -0.02569 0.00016 -0.01454 OH10 1 0.585700 0.492889 0.688757 11.00000 0.02480 HKLF 4 REM finescreekite REM R1 = 0.0611 for 1440 Fo > 4sig(Fo) and 0.0669 for all 1588 data REM 158 parameters refined using 0 restraints END WGHT 0.0643 0.0000 REM Highest difference peak 2.298, deepest hole -2.981, 1-sigma level 0.577 Q1 1 0.6370 0.4172 0.3528 11.00000 0.05 2.30 Q2 1 0.6315 0.4383 0.4615 11.00000 0.05 2.24 Q3 1 0.2287 0.6227 0.5782 11.00000 0.05 2.19 Q4 1 0.2211 0.5356 0.5811 11.00000 0.05 2.12 Q5 1 0.6154 0.5351 0.3383 11.00000 0.05 2.06 Q6 1 0.6646 0.2268 0.5709 11.00000 0.05 2.05 Q7 1 0.2417 0.2017 0.6414 11.00000 0.05 2.04 Q8 1 0.2470 0.5414 0.7014 11.00000 0.05 2.01 Q9 1 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98.23 3 11 -3 28.23 49.08 3 -11 -3 1.05 27.42 3 11 3 30.56 41.19 -3 -11 3 15.94 46.69 3 -11 3 43.95 34.23 -3 -11 -3 21.12 30.00 -3 11 -3 74.80 49.90 -9 -2 0 242.26 143.88 -9 2 0 330.30 80.40 -7 -4 9 7.92 8.45 -7 -4 -9 76.51 58.52 -7 4 -9 45.11 28.32 -7 -5 8 26.14 21.60 -7 5 8 25.45 14.87 -7 5 -8 55.46 32.34 -2 1 -16 -6.09 19.05 -2 -1 -16 -31.42 37.77 1 -11 -6 0.08 79.79 -1 -11 -6 -0.65 52.17 -1 -11 6 252.96 53.42 1 -11 6 221.93 55.70 5 -6 -11 54.93 29.76 -5 6 -11 106.94 34.99 -5 -6 11 19.56 13.83 -4 -9 8 168.95 66.09 4 -9 -8 81.66 63.53 4 -9 8 -0.31 130.03 -4 9 -8 284.63 62.79 -9 2 -1 6.31 25.72 -9 2 1 4.77 33.97 -9 -2 1 21.81 25.61 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 54969