data_hexathioplumbite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'hexathioplumbite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H8 O26 Pb10 S12' _chemical_formula_weight 2880.68 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 hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _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' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 10.7213(10) _cell_length_b 10.7213(10) _cell_length_c 8.6541(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 861.49(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4053 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'prism' _exptl_crystal_colour colorless' _exptl_crystal_density_diffrn 5.553 _exptl_crystal_F_000 1228 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.025 _exptl_absorpt_coefficient_mu 49.476 _shelx_estimated_absorpt_T_min 0.036 _shelx_estimated_absorpt_T_max 0.371 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.176 _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 4849 _diffrn_reflns_av_unetI/netI 0.0443 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.218 _diffrn_reflns_theta_max 27.387 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 1151 _reflns_number_gt 1062 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.878 _reflns_Friedel_fraction_max 0.995 _reflns_Friedel_fraction_full 0.994 _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_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.1467P)^2^+20.5677P] 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 0.0011(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.07(6) _refine_ls_number_reflns 1151 _refine_ls_number_parameters 75 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2121 _refine_ls_wR_factor_gt 0.1999 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.150 _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 0.14950(15) 0.44866(15) 0.5000(3) 0.0348(7) Uani 1 1 d . . . . . Pb2 Pb 0.666667 0.333333 0.3634(3) 0.0268(7) Uani 1 3 d S T P . . Pb3 Pb 0.000000 0.000000 0.3000(5) 0.0564(11) Uani 1 3 d S T P . . S1 S 0.8159(9) 0.1274(9) 0.5595(12) 0.0209(17) Uani 1 1 d . . . . . S2 S 0.6917(12) 0.0245(11) 0.3754(14) 0.036(2) Uani 1 1 d . . . . . O1 O 0.832(3) 0.268(3) 0.570(5) 0.033(7) Uani 1 1 d . . . . . O2 O 0.753(3) 0.041(3) 0.700(4) 0.036(7) Uani 1 1 d . . . . . O3 O 0.957(3) 0.136(3) 0.534(4) 0.033(8) Uani 1 1 d . . . . . OH4 O 0.822(3) 0.350(3) 0.154(4) 0.023(6) Uani 1 1 d . . . . . OH5 O 0.333333 0.666667 0.374(9) 0.030(11) Uani 1 3 d S T 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 0.0265(9) 0.0283(8) 0.0366(12) -0.0097(8) -0.0045(7) 0.0038(6) Pb2 0.0320(9) 0.0320(9) 0.0166(12) 0.000 0.000 0.0160(4) Pb3 0.0741(17) 0.0741(17) 0.0208(17) 0.000 0.000 0.0371(8) S1 0.020(4) 0.019(4) 0.020(5) 0.003(3) 0.000(3) 0.008(3) S2 0.047(5) 0.029(4) 0.017(5) 0.005(4) -0.003(5) 0.007(4) O1 0.032(14) 0.023(13) 0.05(2) -0.011(13) -0.010(13) 0.019(11) O2 0.020(12) 0.042(16) 0.017(15) -0.008(14) -0.004(11) -0.007(11) O3 0.035(14) 0.020(12) 0.04(2) -0.001(12) 0.004(13) 0.014(11) OH4 0.013(11) 0.021(12) 0.033(17) 0.009(11) 0.009(10) 0.008(9) OH5 0.025(12) 0.025(12) 0.04(3) 0.000 0.000 0.012(6) _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 OH4 2.30(3) 5_565 ? Pb1 OH4 2.43(3) 4_665 ? Pb1 OH5 2.44(3) . ? Pb1 O3 2.94(3) 1_455 ? Pb1 O2 3.01(3) 5_564 ? Pb1 O1 3.02(3) 1_455 ? Pb1 S2 3.201(10) 3_665 ? Pb1 S2 3.497(12) 5_565 ? Pb1 S1 3.550(9) 1_455 ? Pb1 O2 3.62(3) 3_665 ? Pb1 Pb1 3.771(2) 2_665 ? Pb1 Pb1 3.771(2) 3_565 ? Pb2 OH4 2.41(3) . ? Pb2 OH4 2.41(3) 3_665 ? Pb2 OH4 2.41(3) 2_655 ? Pb2 O1 2.84(3) . ? Pb2 O1 2.84(3) 2_655 ? Pb2 O1 2.84(3) 3_665 ? Pb2 S2 3.454(12) . ? Pb2 S2 3.455(12) 2_655 ? Pb2 S2 3.455(12) 3_665 ? Pb2 S1 3.722(9) . ? Pb2 S1 3.722(9) 2_655 ? Pb2 S1 3.722(9) 3_665 ? Pb3 O3 2.66(3) 3_665 ? Pb3 O3 2.66(3) 1_455 ? Pb3 O3 2.66(3) 2_545 ? Pb3 O3 2.88(3) 6_444 ? Pb3 O3 2.88(3) 4_654 ? Pb3 O3 2.88(3) 5_564 ? Pb3 O2 3.02(3) 6_444 ? Pb3 O2 3.02(3) 5_564 ? Pb3 O2 3.02(3) 4_654 ? Pb3 S2 3.505(13) 3_665 ? Pb3 S2 3.505(13) 2_545 ? Pb3 S2 3.505(13) 1_455 ? S1 O1 1.44(2) . ? S1 O2 1.47(4) . ? S1 O3 1.49(3) . ? S1 S2 2.015(15) . ? 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 OH4 Pb1 OH4 71.1(12) 5_565 4_665 ? OH4 Pb1 OH5 75.4(14) 5_565 . ? OH4 Pb1 OH5 73.2(15) 4_665 . ? OH4 Pb1 O3 110.7(9) 5_565 1_455 ? OH4 Pb1 O3 131.6(9) 4_665 1_455 ? OH5 Pb1 O3 155.2(15) . 1_455 ? OH4 Pb1 O2 137.2(8) 5_565 5_564 ? OH4 Pb1 O2 145.5(9) 4_665 5_564 ? OH5 Pb1 O2 93.4(18) . 5_564 ? O3 Pb1 O2 65.5(10) 1_455 5_564 ? OH4 Pb1 O1 131.7(10) 5_565 1_455 ? OH4 Pb1 O1 93.3(8) 4_665 1_455 ? OH5 Pb1 O1 144.8(8) . 1_455 ? O3 Pb1 O1 47.8(7) 1_455 1_455 ? O2 Pb1 O1 79.5(9) 5_564 1_455 ? OH4 Pb1 S2 71.8(7) 5_565 3_665 ? OH4 Pb1 S2 140.5(6) 4_665 3_665 ? OH5 Pb1 S2 84.7(6) . 3_665 ? O3 Pb1 S2 75.1(6) 1_455 3_665 ? O2 Pb1 S2 66.0(5) 5_564 3_665 ? O1 Pb1 S2 121.8(5) 1_455 3_665 ? OH4 Pb1 S2 73.3(7) 5_565 5_565 ? OH4 Pb1 S2 70.1(8) 4_665 5_565 ? OH5 Pb1 S2 137.7(16) . 5_565 ? O3 Pb1 S2 65.0(7) 1_455 5_565 ? O2 Pb1 S2 128.9(7) 5_564 5_565 ? O1 Pb1 S2 58.4(8) 1_455 5_565 ? S2 Pb1 S2 111.2(3) 3_665 5_565 ? OH4 Pb1 S1 125.1(7) 5_565 1_455 ? OH4 Pb1 S1 113.6(6) 4_665 1_455 ? OH5 Pb1 S1 159.3(14) . 1_455 ? O3 Pb1 S1 24.3(5) 1_455 1_455 ? O2 Pb1 S1 69.9(7) 5_564 1_455 ? O1 Pb1 S1 23.5(5) 1_455 1_455 ? S2 Pb1 S1 98.6(3) 3_665 1_455 ? S2 Pb1 S1 60.0(3) 5_565 1_455 ? OH4 Pb1 O2 49.8(8) 5_565 3_665 ? OH4 Pb1 O2 111.2(9) 4_665 3_665 ? OH5 Pb1 O2 114.2(8) . 3_665 ? O3 Pb1 O2 62.2(8) 1_455 3_665 ? O2 Pb1 O2 103.3(8) 5_564 3_665 ? O1 Pb1 O2 100.9(8) 1_455 3_665 ? S2 Pb1 O2 49.3(6) 3_665 3_665 ? S2 Pb1 O2 62.7(6) 5_565 3_665 ? S1 Pb1 O2 82.4(6) 1_455 3_665 ? OH4 Pb1 Pb1 38.2(7) 5_565 2_665 ? OH4 Pb1 Pb1 76.9(6) 4_665 2_665 ? OH5 Pb1 Pb1 39.3(10) . 2_665 ? O3 Pb1 Pb1 135.6(6) 1_455 2_665 ? O2 Pb1 Pb1 112.8(6) 5_564 2_665 ? O1 Pb1 Pb1 167.7(7) 1_455 2_665 ? S2 Pb1 Pb1 65.6(2) 3_665 2_665 ? S2 Pb1 Pb1 110.62(19) 5_565 2_665 ? S1 Pb1 Pb1 158.62(15) 1_455 2_665 ? O2 Pb1 Pb1 76.4(6) 3_665 2_665 ? OH4 Pb1 Pb1 78.1(6) 5_565 3_565 ? OH4 Pb1 Pb1 36.0(7) 4_665 3_565 ? OH5 Pb1 Pb1 39.3(10) . 3_565 ? O3 Pb1 Pb1 163.1(5) 1_455 3_565 ? O2 Pb1 Pb1 118.4(7) 5_564 3_565 ? O1 Pb1 Pb1 115.5(5) 1_455 3_565 ? S2 Pb1 Pb1 121.8(2) 3_665 3_565 ? S2 Pb1 Pb1 105.9(2) 5_565 3_565 ? S1 Pb1 Pb1 139.04(16) 1_455 3_565 ? O2 Pb1 Pb1 127.9(5) 3_665 3_565 ? Pb1 Pb1 Pb1 60.0 2_665 3_565 ? OH4 Pb2 OH4 69.7(11) . 3_665 ? OH4 Pb2 OH4 69.7(11) . 2_655 ? OH4 Pb2 OH4 69.7(11) 3_665 2_655 ? OH4 Pb2 O1 89.9(9) . . ? OH4 Pb2 O1 123.4(8) 3_665 . ? OH4 Pb2 O1 151.0(9) 2_655 . ? OH4 Pb2 O1 123.4(8) . 2_655 ? OH4 Pb2 O1 151.0(9) 3_665 2_655 ? OH4 Pb2 O1 89.9(9) 2_655 2_655 ? O1 Pb2 O1 84.4(11) . 2_655 ? OH4 Pb2 O1 151.0(9) . 3_665 ? OH4 Pb2 O1 89.9(10) 3_665 3_665 ? OH4 Pb2 O1 123.4(8) 2_655 3_665 ? O1 Pb2 O1 84.4(11) . 3_665 ? O1 Pb2 O1 84.4(11) 2_655 3_665 ? OH4 Pb2 S2 73.2(6) . . ? OH4 Pb2 S2 71.1(6) 3_665 . ? OH4 Pb2 S2 133.0(7) 2_655 . ? O1 Pb2 S2 52.3(6) . . ? O1 Pb2 S2 135.3(8) 2_655 . ? O1 Pb2 S2 81.0(6) 3_665 . ? OH4 Pb2 S2 71.1(6) . 2_655 ? OH4 Pb2 S2 133.0(7) 3_665 2_655 ? OH4 Pb2 S2 73.2(6) 2_655 2_655 ? O1 Pb2 S2 81.0(6) . 2_655 ? O1 Pb2 S2 52.3(6) 2_655 2_655 ? O1 Pb2 S2 135.3(8) 3_665 2_655 ? S2 Pb2 S2 119.91(2) . 2_655 ? OH4 Pb2 S2 133.0(7) . 3_665 ? OH4 Pb2 S2 73.2(6) 3_665 3_665 ? OH4 Pb2 S2 71.1(6) 2_655 3_665 ? O1 Pb2 S2 135.3(8) . 3_665 ? O1 Pb2 S2 81.0(6) 2_655 3_665 ? O1 Pb2 S2 52.3(6) 3_665 3_665 ? S2 Pb2 S2 119.91(2) . 3_665 ? S2 Pb2 S2 119.91(2) 2_655 3_665 ? OH4 Pb2 S1 84.2(6) . . ? OH4 Pb2 S1 103.4(6) 3_665 . ? OH4 Pb2 S1 153.8(7) 2_655 . ? O1 Pb2 S1 20.1(6) . . ? O1 Pb2 S1 103.7(8) 2_655 . ? O1 Pb2 S1 80.8(6) 3_665 . ? S2 Pb2 S1 32.3(2) . . ? S2 Pb2 S1 97.3(2) 2_655 . ? S2 Pb2 S1 132.5(2) 3_665 . ? OH4 Pb2 S1 103.4(6) . 2_655 ? OH4 Pb2 S1 153.8(7) 3_665 2_655 ? OH4 Pb2 S1 84.2(6) 2_655 2_655 ? O1 Pb2 S1 80.8(6) . 2_655 ? O1 Pb2 S1 20.1(6) 2_655 2_655 ? O1 Pb2 S1 103.7(8) 3_665 2_655 ? S2 Pb2 S1 132.5(2) . 2_655 ? S2 Pb2 S1 32.3(2) 2_655 2_655 ? S2 Pb2 S1 97.3(2) 3_665 2_655 ? S1 Pb2 S1 100.8(2) . 2_655 ? OH4 Pb2 S1 153.8(7) . 3_665 ? OH4 Pb2 S1 84.2(6) 3_665 3_665 ? OH4 Pb2 S1 103.4(6) 2_655 3_665 ? O1 Pb2 S1 103.7(8) . 3_665 ? O1 Pb2 S1 80.8(6) 2_655 3_665 ? O1 Pb2 S1 20.1(6) 3_665 3_665 ? S2 Pb2 S1 97.3(2) . 3_665 ? S2 Pb2 S1 132.5(2) 2_655 3_665 ? S2 Pb2 S1 32.3(2) 3_665 3_665 ? S1 Pb2 S1 100.8(2) . 3_665 ? S1 Pb2 S1 100.8(2) 2_655 3_665 ? O3 Pb3 O3 68.4(11) 3_665 1_455 ? O3 Pb3 O3 68.4(11) 3_665 2_545 ? O3 Pb3 O3 68.4(11) 1_455 2_545 ? O3 Pb3 O3 176.4(10) 3_665 6_444 ? O3 Pb3 O3 114.4(7) 1_455 6_444 ? O3 Pb3 O3 114.4(7) 2_545 6_444 ? O3 Pb3 O3 114.4(7) 3_665 4_654 ? O3 Pb3 O3 176.4(10) 1_455 4_654 ? O3 Pb3 O3 114.4(7) 2_545 4_654 ? O3 Pb3 O3 62.7(9) 6_444 4_654 ? O3 Pb3 O3 114.4(7) 3_665 5_564 ? O3 Pb3 O3 114.4(7) 1_455 5_564 ? O3 Pb3 O3 176.4(10) 2_545 5_564 ? O3 Pb3 O3 62.7(9) 6_444 5_564 ? O3 Pb3 O3 62.7(9) 4_654 5_564 ? O3 Pb3 O2 134.4(9) 3_665 6_444 ? O3 Pb3 O2 108.5(9) 1_455 6_444 ? O3 Pb3 O2 68.6(9) 2_545 6_444 ? O3 Pb3 O2 47.6(8) 6_444 6_444 ? O3 Pb3 O2 71.3(9) 4_654 6_444 ? O3 Pb3 O2 108.1(9) 5_564 6_444 ? O3 Pb3 O2 108.5(9) 3_665 5_564 ? O3 Pb3 O2 68.6(9) 1_455 5_564 ? O3 Pb3 O2 134.4(9) 2_545 5_564 ? O3 Pb3 O2 71.3(9) 6_444 5_564 ? O3 Pb3 O2 108.1(9) 4_654 5_564 ? O3 Pb3 O2 47.6(8) 5_564 5_564 ? O2 Pb3 O2 112.2(6) 6_444 5_564 ? O3 Pb3 O2 68.6(9) 3_665 4_654 ? O3 Pb3 O2 134.4(9) 1_455 4_654 ? O3 Pb3 O2 108.5(9) 2_545 4_654 ? O3 Pb3 O2 108.1(9) 6_444 4_654 ? O3 Pb3 O2 47.6(8) 4_654 4_654 ? O3 Pb3 O2 71.3(9) 5_564 4_654 ? O2 Pb3 O2 112.2(6) 6_444 4_654 ? O2 Pb3 O2 112.2(6) 5_564 4_654 ? O3 Pb3 S2 52.5(7) 3_665 3_665 ? O3 Pb3 S2 73.4(7) 1_455 3_665 ? O3 Pb3 S2 117.9(7) 2_545 3_665 ? O3 Pb3 S2 125.5(6) 6_444 3_665 ? O3 Pb3 S2 106.4(6) 4_654 3_665 ? O3 Pb3 S2 65.4(6) 5_564 3_665 ? O2 Pb3 S2 173.1(7) 6_444 3_665 ? O2 Pb3 S2 62.0(6) 5_564 3_665 ? O2 Pb3 S2 68.7(6) 4_654 3_665 ? O3 Pb3 S2 73.4(7) 3_665 2_545 ? O3 Pb3 S2 117.9(7) 1_455 2_545 ? O3 Pb3 S2 52.5(7) 2_545 2_545 ? O3 Pb3 S2 106.4(6) 6_444 2_545 ? O3 Pb3 S2 65.4(6) 4_654 2_545 ? O3 Pb3 S2 125.5(6) 5_564 2_545 ? O2 Pb3 S2 68.7(6) 6_444 2_545 ? O2 Pb3 S2 173.1(7) 5_564 2_545 ? O2 Pb3 S2 62.0(6) 4_654 2_545 ? S2 Pb3 S2 116.62(13) 3_665 2_545 ? O3 Pb3 S2 117.9(7) 3_665 1_455 ? O3 Pb3 S2 52.5(7) 1_455 1_455 ? O3 Pb3 S2 73.4(7) 2_545 1_455 ? O3 Pb3 S2 65.4(6) 6_444 1_455 ? O3 Pb3 S2 125.5(6) 4_654 1_455 ? O3 Pb3 S2 106.4(6) 5_564 1_455 ? O2 Pb3 S2 62.0(6) 6_444 1_455 ? O2 Pb3 S2 68.7(6) 5_564 1_455 ? O2 Pb3 S2 173.1(7) 4_654 1_455 ? S2 Pb3 S2 116.62(13) 3_665 1_455 ? S2 Pb3 S2 116.62(13) 2_545 1_455 ? O1 S1 O2 113(2) . . ? O1 S1 O3 111.3(18) . . ? O2 S1 O3 107.1(19) . . ? O1 S1 S2 109.0(15) . . ? O2 S1 S2 109.8(12) . . ? O3 S1 S2 106.9(15) . . ? O1 S1 Pb1 57.1(13) . 1_655 ? O2 S1 Pb1 130.8(11) . 1_655 ? O3 S1 Pb1 54.5(11) . 1_655 ? S2 S1 Pb1 119.1(5) . 1_655 ? O1 S1 Pb3 124.4(14) . 4_655 ? O2 S1 Pb3 56.5(13) . 4_655 ? O3 S1 Pb3 50.9(14) . 4_655 ? S2 S1 Pb3 126.2(5) . 4_655 ? Pb1 S1 Pb3 88.53(19) 1_655 4_655 ? O1 S1 Pb3 128.9(16) . 1_655 ? O2 S1 Pb3 115.7(15) . 1_655 ? O3 S1 Pb3 38.1(13) . 1_655 ? S2 S1 Pb3 69.1(5) . 1_655 ? Pb1 S1 Pb3 78.70(19) 1_655 1_655 ? Pb3 S1 Pb3 73.27(16) 4_655 1_655 ? O1 S1 Pb2 42.8(13) . . ? O2 S1 Pb2 123.4(14) . . ? O3 S1 Pb2 128.6(13) . . ? S2 S1 Pb2 66.5(4) . . ? Pb1 S1 Pb2 83.20(19) 1_655 . ? Pb3 S1 Pb2 167.2(3) 4_655 . ? Pb3 S1 Pb2 114.3(3) 1_655 . ? O1 S1 Pb1 148.0(12) . 2_655 ? O2 S1 Pb1 63.3(12) . 2_655 ? O3 S1 Pb1 99.6(11) . 2_655 ? S2 S1 Pb1 51.7(4) . 2_655 ? Pb1 S1 Pb1 151.4(3) 1_655 2_655 ? Pb3 S1 Pb1 81.42(18) 4_655 2_655 ? Pb3 S1 Pb1 72.80(16) 1_655 2_655 ? Pb2 S1 Pb1 110.3(2) . 2_655 ? O1 S1 Pb1 75.9(16) . 6_655 ? O2 S1 Pb1 37.1(13) . 6_655 ? O3 S1 Pb1 117.8(15) . 6_655 ? S2 S1 Pb1 129.7(5) . 6_655 ? Pb1 S1 Pb1 105.6(2) 1_655 6_655 ? Pb3 S1 Pb1 73.6(2) 4_655 6_655 ? Pb3 S1 Pb1 146.4(3) 1_655 6_655 ? Pb2 S1 Pb1 99.2(2) . 6_655 ? Pb1 S1 Pb1 97.2(2) 2_655 6_655 ? S1 S2 Pb1 98.7(5) . 2_655 ? S1 S2 Pb2 81.1(4) . . ? Pb1 S2 Pb2 146.0(4) 2_655 . ? S1 S2 Pb1 129.9(5) . 6_654 ? Pb1 S2 Pb1 129.5(4) 2_655 6_654 ? Pb2 S2 Pb1 66.8(2) . 6_654 ? S1 S2 Pb3 78.4(5) . 1_655 ? Pb1 S2 Pb3 86.1(3) 2_655 1_655 ? Pb2 S2 Pb3 126.5(3) . 1_655 ? Pb1 S2 Pb3 90.5(3) 6_654 1_655 ? S1 S2 Pb1 108.1(5) . 3 ? Pb1 S2 Pb1 64.41(19) 2_655 3 ? Pb2 S2 Pb1 83.2(3) . 3 ? Pb1 S2 Pb1 105.3(3) 6_654 3 ? Pb3 S2 Pb1 150.3(3) 1_655 3 ? S1 O1 Pb2 117.1(17) . . ? S1 O1 Pb1 99.4(14) . 1_655 ? Pb2 O1 Pb1 110.9(12) . 1_655 ? S1 O1 Pb1 83.5(16) . 6_655 ? Pb2 O1 Pb1 120.5(9) . 6_655 ? Pb1 O1 Pb1 120.1(10) 1_655 6_655 ? S1 O2 Pb1 125.8(18) . 6_655 ? S1 O2 Pb3 99.6(14) . 4_655 ? Pb1 O2 Pb3 98.9(10) 6_655 4_655 ? S1 O2 Pb1 95.4(14) . 2_655 ? Pb1 O2 Pb1 132.2(9) 6_655 2_655 ? Pb3 O2 Pb1 96.6(9) 4_655 2_655 ? S1 O3 Pb3 121.8(18) . 1_655 ? S1 O3 Pb3 105.4(17) . 4_655 ? Pb3 O3 Pb3 102.6(8) 1_655 4_655 ? S1 O3 Pb1 101.2(13) . 1_655 ? Pb3 O3 Pb1 109.4(11) 1_655 1_655 ? Pb3 O3 Pb1 117.3(11) 4_655 1_655 ? Pb1 OH4 Pb2 108.6(9) 6_654 . ? Pb1 OH4 Pb1 105.8(12) 6_654 4_664 ? Pb2 OH4 Pb1 104.6(9) . 4_664 ? Pb1 OH4 O2 90.7(11) 6_654 5_664 ? Pb2 OH4 O2 120.9(14) . 5_664 ? Pb1 OH4 O2 123.3(12) 4_664 5_664 ? Pb1 OH4 Pb1 67.5(6) 6_654 5_554 ? Pb2 OH4 Pb1 68.3(6) . 5_554 ? Pb1 OH4 Pb1 66.9(6) 4_664 5_554 ? O2 OH4 Pb1 158.2(12) 5_664 5_554 ? Pb1 OH5 Pb1 101(2) . 3_565 ? Pb1 OH5 Pb1 101(2) . 2_665 ? Pb1 OH5 Pb1 101(2) 3_565 2_665 ? _refine_diff_density_max 8.867 _refine_diff_density_min -2.605 _refine_diff_density_rms 0.460 _shelx_res_file ; TITL Redmond20 js72.res created by SHELXL-2016/6 at 19:25:27 on 15-Sep-2021 CELL 0.71075 10.72130 10.72130 8.65414 90.00000 90.00000 120.00000 ZERR 1 0.00100 0.00100 0.00061 0.00000 0.00000 0.00000 LATT -1 SYMM -Y, +X-Y, +Z SYMM -X+Y, -X, +Z SYMM -X, -Y, .50+Z SYMM +Y, -X+Y, .50+Z SYMM +X-Y, +X, .50+Z SFAC O PB S H UNIT 26 10 12 8 L.S. 10 CONN 12 3.0 PB1 CONN 12 3.0 PB2 CONN 12 3.0 PB3 EQIV $1 y+1, -x+y+1, z-1/2 BIND OH4 O2_$1 FMAP 2 PLAN 8 ACTA TWIN SIZE 0.200 0.025 0.025 WGHT 0.146700 20.567699 EXTI 0.001110 BASF 0.06596 FVAR 0.21386 PB1 2 0.149501 0.448657 0.500018 11.00000 0.02651 0.02828 = 0.03657 -0.00969 -0.00452 0.00382 PB2 2 0.666667 0.333333 0.363380 10.33333 0.03197 0.03197 = 0.01659 0.00000 0.00000 0.01599 PB3 2 0.000000 0.000000 0.300041 10.33333 0.07415 0.07415 = 0.02078 0.00000 0.00000 0.03707 S1 3 0.815893 0.127371 0.559547 11.00000 0.02049 0.01949 = 0.02003 0.00258 -0.00015 0.00797 S2 3 0.691734 0.024538 0.375421 11.00000 0.04667 0.02874 = 0.01719 0.00468 -0.00295 0.00716 O1 1 0.831838 0.268264 0.570426 11.00000 0.03232 0.02293 = 0.05008 -0.01094 -0.00984 0.01885 O2 1 0.752576 0.040795 0.700190 11.00000 0.02005 0.04168 = 0.01662 -0.00793 -0.00407 -0.00729 O3 1 0.957437 0.135771 0.534144 11.00000 0.03481 0.01996 = 0.04438 -0.00143 0.00365 0.01365 OH4 1 0.822428 0.349981 0.154329 11.00000 0.01341 0.02130 = 0.03289 0.00927 0.00857 0.00758 OH5 1 0.333333 0.666667 0.373933 10.33333 0.02477 0.02477 = 0.03954 0.00000 0.00000 0.01239 HKLF 4 REM Redmond20 REM R1 = 0.0791 for 1062 Fo > 4sig(Fo) and 0.0843 for all 1151 data REM 75 parameters refined using 1 restraints END WGHT 0.1468 20.4307 REM Highest difference peak 8.867, deepest hole -2.605, 1-sigma level 0.460 Q1 1 1.0000 0.0000 0.5523 10.33333 0.05 1.51 Q2 1 0.3333 0.6667 0.1377 10.33333 0.05 1.46 Q3 1 0.6989 0.1416 0.7163 11.00000 0.05 1.43 Q4 1 0.0481 0.3470 0.4518 11.00000 0.05 1.41 Q5 1 0.0000 0.0000 0.1624 10.33333 0.05 1.28 Q6 1 -0.0366 -0.0005 0.4394 11.00000 0.05 1.20 Q7 1 0.6667 0.3333 0.5045 10.33333 0.05 1.16 Q8 1 0.7079 0.1585 0.2597 11.00000 0.05 1.12 ; _shelx_res_checksum 12590 _shelx_hkl_file ; -1 1 1 970.55 19.33 0 -1 -1 924.35 20.26 1 -1 1 1024.16 21.70 0 1 -1 842.68 16.79 1 -1 -1 864.11 17.93 0 -1 1 1004.31 19.33 0 1 1 995.09 23.46 -1 1 -1 919.60 21.84 -2 1 0 1820.46 43.61 -1 2 0 1744.25 48.40 1 1 0 1807.20 43.73 -1 -1 0 1864.89 44.57 1 -2 0 1724.95 51.95 2 -1 0 1817.96 44.34 0 -2 0 120.57 4.49 2 -2 0 118.77 4.50 0 2 0 116.03 4.46 -2 2 0 122.62 6.36 -1 2 1 633.17 19.18 2 -1 -1 512.36 10.38 2 -1 1 639.45 15.13 1 -2 1 644.74 15.97 -1 2 -1 528.74 14.16 1 -2 -1 529.45 18.07 -2 1 1 656.50 11.88 1 1 -1 496.31 9.71 1 1 1 645.30 15.59 -1 -1 1 643.60 11.38 0 -2 1 1036.01 28.48 2 -2 1 1029.16 27.35 0 2 1 992.87 26.86 -2 2 1 1009.40 25.94 1 -1 -2 1202.76 27.42 0 -1 2 1211.86 27.08 -1 1 2 1145.91 26.67 0 1 2 1199.88 33.65 2 1 0 40.03 2.23 1 -3 0 39.02 5.32 3 -2 0 44.98 4.44 -1 3 0 38.78 3.57 -3 2 0 43.20 2.73 1 2 0 9190.83 412.43 -2 3 0 8204.72 392.32 3 -1 0 9999.00 421.52 2 -3 0 7700.86 382.42 -1 -2 0 9548.78 416.82 1 -2 2 3229.25 107.70 -1 -1 2 3531.92 93.91 1 -2 -2 2891.18 99.68 1 1 -2 3170.72 81.49 -1 2 2 3091.37 106.12 -1 2 -2 2824.78 92.19 -2 1 2 3209.43 90.58 2 -1 -2 2730.84 75.20 -1 3 -1 3847.42 152.93 1 -3 -1 3990.08 159.65 2 1 -1 4557.35 146.95 -1 3 1 4950.55 191.11 -3 2 -1 4491.90 166.86 -3 2 1 5112.64 175.58 3 -2 -1 3867.49 143.49 3 -2 1 4982.39 182.16 1 -3 1 4960.25 186.65 -2 3 -1 510.84 16.97 -1 -2 1 630.04 17.10 1 2 1 606.19 17.15 -1 -2 -1 552.09 16.28 -2 3 1 600.29 18.49 2 -3 1 664.55 19.54 3 -1 -1 506.45 12.97 -3 1 1 645.76 12.28 2 -3 -1 516.94 17.23 1 2 -1 429.28 14.80 -2 2 2 1204.37 31.39 0 2 -2 934.08 24.79 0 -2 -2 1063.42 35.63 -2 2 -2 1047.81 30.53 2 -2 2 1220.34 38.83 2 -2 -2 933.03 25.45 0 -2 2 1208.08 30.30 0 2 2 1198.06 33.79 -3 3 0 1622.08 51.07 0 -3 0 1648.65 57.55 0 3 0 1577.85 51.98 3 -3 0 1640.05 52.76 0 3 1 1032.51 33.56 0 -3 1 1097.90 37.56 -3 3 -1 973.03 30.85 3 -3 1 1069.23 33.10 3 -3 -1 897.64 28.93 0 -3 -1 969.70 31.07 -3 3 1 1052.57 31.75 0 3 -1 893.14 28.33 0 1 3 2655.75 84.06 0 -1 3 2623.85 76.86 -1 1 3 2570.57 80.71 2 -3 -2 2993.87 118.83 2 -3 2 3605.33 129.06 -2 3 2 3462.45 126.72 1 2 2 3547.73 127.63 -2 3 -2 3147.75 114.80 3 -1 -2 2517.37 75.27 -1 -2 2 3477.88 112.13 1 2 -2 2536.62 83.56 -3 1 2 4126.77 109.20 -1 3 -2 1048.58 31.89 3 -2 -2 982.78 26.42 1 -3 2 1157.92 35.17 1 -3 -2 1148.14 41.25 -2 -1 2 1098.73 20.69 -3 2 2 1160.80 29.93 -1 3 2 1139.52 37.88 2 1 -2 1046.30 20.38 3 -2 2 1088.17 34.02 -4 2 0 645.00 18.00 4 -2 0 646.21 18.58 2 -4 0 630.47 23.19 -2 -2 0 663.62 18.06 2 2 0 617.39 17.84 -2 4 0 622.69 22.89 -3 4 0 20.78 3.70 3 -4 0 32.32 3.89 1 3 0 12.79 4.70 -1 -3 0 17.59 2.92 4 -3 0 31.33 3.64 -4 3 0 31.35 3.13 1 -4 0 35.75 6.31 3 1 0 36.12 2.64 -1 4 0 29.66 4.24 -2 -2 1 3653.75 118.11 2 2 1 3696.04 135.14 2 -4 1 3646.48 143.08 -2 4 -1 3348.61 141.45 4 -2 -1 3425.32 122.84 2 -4 -1 3390.13 135.58 -4 2 1 3801.62 124.38 -2 4 1 3497.83 140.18 4 -2 1 3756.23 136.76 2 2 -1 3366.23 120.30 -1 2 3 2260.21 72.02 -1 -1 3 2425.03 63.76 1 -2 -3 1949.47 63.88 1 -2 3 2362.90 71.91 -2 1 3 2197.45 58.54 -3 3 2 6196.64 245.36 3 -3 -2 4370.15 187.84 0 3 -2 4004.20 171.24 -3 3 -2 5115.53 214.51 3 -3 2 6050.93 248.13 0 -3 -2 5268.20 222.11 0 3 2 6030.53 250.84 0 -3 2 6032.82 242.24 1 -4 -1 166.39 9.53 -1 4 -1 164.20 12.48 1 -4 1 214.35 9.53 3 1 -1 163.11 4.60 -1 4 1 195.13 10.37 4 -3 1 209.80 9.04 -4 3 1 215.88 7.59 4 -3 -1 145.43 7.58 -4 3 -1 157.95 7.93 3 -4 -1 2542.72 98.65 -1 -3 -1 2840.48 100.45 -3 4 1 2873.07 107.11 -3 4 -1 2600.14 106.79 1 3 -1 2325.39 91.91 3 -4 1 2973.99 111.44 4 -1 -1 2719.09 84.12 1 3 1 2843.53 103.30 -1 -3 1 2929.09 98.62 0 2 -3 422.71 11.13 -2 2 3 470.08 15.97 2 -2 3 440.29 14.49 0 -2 3 450.48 11.75 -2 0 3 443.27 7.97 0 2 3 441.84 15.39 2 -2 -3 422.80 11.76 0 -4 0 8.57 2.69 0 4 0 2.61 2.82 -4 4 0 12.23 4.15 4 -4 0 5.21 2.81 4 -2 2 2572.32 89.34 4 -2 -2 1877.18 64.18 2 -4 -2 2226.23 94.58 -2 4 2 2601.48 97.51 2 -4 2 2691.27 97.52 2 2 2 2630.45 92.82 -4 2 2 2643.63 75.09 -2 4 -2 2120.31 80.50 2 2 -2 1753.08 58.35 -2 -2 2 2566.81 73.25 4 -4 1 659.32 24.82 4 -4 -1 553.02 21.54 -4 4 1 653.34 23.06 0 4 1 628.05 24.99 0 -4 1 630.39 22.48 0 -4 -1 620.96 23.10 0 4 -1 513.06 26.62 -4 4 -1 600.48 29.59 3 -2 3 521.61 23.90 -2 -1 3 557.04 9.02 -3 2 3 540.73 16.79 1 -3 3 571.83 22.09 -1 3 -3 419.58 18.81 1 -3 -3 443.70 16.83 -1 3 3 538.76 19.08 3 -2 -3 415.75 11.14 -3 1 3 221.22 5.30 -1 -2 3 225.12 8.10 2 -3 -3 216.03 12.00 1 2 -3 203.78 6.84 2 -3 3 218.15 13.53 -2 3 3 218.01 9.49 1 2 3 209.62 10.37 -2 3 -3 216.09 8.98 3 1 -2 154.35 4.37 4 -3 2 215.58 10.84 -4 3 2 242.82 8.58 -1 4 -2 199.34 13.15 -1 4 2 236.91 17.15 4 -3 -2 155.83 7.48 1 -4 -2 189.99 10.80 1 -4 2 254.32 10.48 1 3 -2 1509.27 51.88 -1 -3 2 2038.81 69.24 3 -4 2 2029.90 75.23 4 -1 -2 1554.86 41.25 -3 4 -2 1855.17 67.73 1 3 2 1972.83 72.88 3 -4 -2 1726.11 65.36 -3 4 2 1901.46 78.02 -1 -3 -2 2097.92 72.94 -2 -3 0 76.46 5.22 3 -5 0 88.30 7.93 -3 5 0 92.39 8.09 2 3 0 79.66 6.07 5 -2 0 102.69 5.07 -5 3 0 -0.12 1.56 -2 5 0 3.52 2.44 2 -5 0 4.98 3.76 5 -3 0 -0.40 1.81 3 2 0 -0.18 1.50 0 3 -3 703.43 21.86 3 -3 3 916.61 31.60 -3 3 3 897.13 28.00 3 -3 -3 691.99 23.11 0 -3 -3 835.95 29.72 0 3 3 884.06 31.94 0 -3 3 945.28 27.72 0 -1 4 764.59 21.04 0 1 4 755.05 23.54 -1 1 4 736.39 21.36 3 2 1 372.35 14.80 3 2 -1 434.43 12.47 2 -5 -1 418.12 18.98 2 -5 1 378.42 25.59 5 -3 -1 429.91 18.71 5 -3 1 380.00 15.91 -2 5 1 334.56 18.94 -2 5 -1 412.77 24.20 -3 5 1 1823.71 68.60 -3 5 -1 1416.05 59.00 -2 -3 1 1851.72 54.98 2 3 1 1845.74 64.07 2 3 -1 1396.27 49.76 5 -2 1 1780.37 65.80 3 -5 -1 1452.23 61.85 -2 -3 -1 1628.37 57.33 5 -2 -1 1470.94 46.90 3 -5 1 1916.22 71.09 4 -4 2 834.88 31.21 0 4 -2 557.36 22.69 4 0 -2 725.60 14.20 0 -4 -2 690.26 27.52 4 0 -2 685.73 13.86 4 -4 -2 596.59 24.22 -4 4 2 806.44 28.27 -4 4 -2 709.99 27.64 0 4 2 784.94 30.90 0 -4 2 838.18 27.25 1 4 0 1947.32 84.62 -1 -4 0 2099.73 75.64 -4 5 0 2050.53 80.09 4 -5 0 2062.94 82.39 5 -1 0 2048.45 66.39 -5 4 0 8808.88 453.17 5 -4 0 8849.63 452.08 -1 5 0 8116.41 433.39 1 -5 0 8872.60 477.19 4 1 0 9401.05 438.09 1 -2 4 1163.18 35.62 -2 1 4 1092.68 31.66 -1 -1 4 1149.34 28.68 -1 2 4 1112.48 35.07 -1 5 -1 39.12 6.05 -5 4 -1 55.01 5.57 5 -4 1 51.37 5.98 5 -4 -1 46.58 7.91 -5 4 1 50.58 4.91 1 -5 -1 64.00 6.49 4 1 -1 51.77 3.08 1 -5 1 59.62 6.33 -1 5 1 61.45 6.84 -1 -4 1 256.31 14.87 1 4 -1 235.74 11.56 1 4 1 245.50 19.18 4 -5 1 257.60 15.02 -4 5 1 234.75 13.73 -4 5 -1 252.86 13.52 -1 -4 -1 268.68 12.65 5 -1 -1 265.23 10.42 4 -5 -1 240.25 13.98 2 -4 3 2034.88 72.63 -4 2 3 1989.55 53.42 4 -2 -3 1490.41 42.47 2 2 -3 1592.45 41.12 4 -2 3 1979.43 71.24 -2 4 3 1899.09 72.27 2 -4 -3 1615.73 61.26 -2 -2 3 1961.41 49.89 2 2 3 1918.66 71.49 -2 4 -3 1623.42 60.10 -2 0 4 338.81 7.37 0 2 4 345.52 14.08 -2 2 4 327.91 11.42 0 -2 4 353.03 10.85 2 -2 4 343.03 13.38 -1 -3 3 405.68 12.21 -3 4 -3 349.88 15.23 1 3 3 390.08 17.58 -3 4 3 370.82 16.28 3 -4 3 438.94 18.03 3 -4 -3 307.64 18.94 1 3 -3 307.14 13.21 -1 4 3 1672.71 64.85 -4 3 3 1811.24 60.57 4 -3 3 1736.19 63.23 4 -3 -3 1201.82 41.80 1 -4 3 1795.75 62.20 -1 4 -3 1281.29 48.65 1 -4 -3 1488.70 57.19 5 -2 2 36.81 7.50 -3 5 2 28.11 8.82 3 -5 -2 54.39 5.67 5 -2 -2 36.25 2.72 3 -5 2 42.19 6.05 2 3 2 46.87 5.46 2 3 -2 26.94 4.95 -2 -3 2 35.64 4.36 3 2 -2 422.59 14.98 -2 5 2 506.28 23.91 5 -3 -2 406.40 15.08 2 -5 2 564.91 23.69 3 2 2 511.92 20.74 -3 -2 2 546.79 12.42 5 -3 2 554.30 21.94 2 -5 -2 494.06 21.73 -2 5 -2 464.70 20.32 -5 3 2 538.26 19.49 -5 5 0 316.43 15.38 0 -5 0 317.93 21.92 0 5 0 302.11 16.66 5 -5 0 316.42 16.71 3 -2 4 413.37 17.27 -1 3 4 373.37 22.16 -3 2 4 420.45 12.08 1 -3 4 421.63 14.92 -2 -1 4 426.40 10.13 2 -3 4 6874.46 315.35 -3 1 4 6671.08 245.25 -1 -2 4 6979.18 271.84 1 2 4 6459.89 296.67 -2 3 4 6701.21 299.80 2 -3 -4 5505.67 251.09 5 -1 -2 959.78 24.30 -1 -4 2 1171.46 38.32 1 4 2 1096.83 43.77 -4 5 -2 980.14 40.17 1 4 -2 818.75 32.08 4 -5 -2 913.65 39.88 -4 5 2 1139.41 53.58 4 -5 2 1192.47 48.26 -1 -4 -2 1089.28 41.55 5 -4 -2 2014.10 83.75 -1 5 -2 2035.00 100.32 -1 5 2 2499.84 107.57 1 -5 -2 2431.29 101.88 4 1 -2 2316.80 69.62 1 -5 2 2751.67 107.88 -5 4 -2 2501.33 100.30 5 -4 2 2678.68 107.62 -5 4 2 2737.51 99.27 5 -5 1 1340.78 54.97 -5 5 -1 1268.02 60.36 0 -5 1 1359.02 51.75 -5 5 1 1319.97 51.27 0 5 1 1322.69 67.26 5 -5 -1 1179.33 48.25 0 -5 -1 1325.45 52.03 0 5 -1 1115.68 56.67 0 -4 3 2677.62 92.57 0 4 3 2495.62 99.54 0 -4 -3 2275.70 90.51 4 -4 3 2675.13 114.12 0 4 -3 1605.61 64.69 4 -4 -3 1726.01 71.29 -4 4 -3 2230.67 88.99 -4 4 3 2590.80 101.98 3 3 0 907.84 33.15 -3 6 0 955.87 53.02 6 -3 0 956.25 34.35 3 -6 0 1017.37 43.49 0 3 4 2271.96 87.47 0 3 -4 1701.57 60.79 3 -3 4 2456.65 101.54 -3 0 4 2694.73 53.85 0 -3 4 2479.98 87.51 3 -3 -4 1626.89 60.89 -3 3 4 2413.81 83.01 6 -4 0 123.31 8.94 4 2 0 106.78 6.85 2 -6 0 146.48 15.71 -6 4 0 103.70 10.70 -2 6 0 137.41 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611.13 24.73 -2 -5 -1 587.55 27.28 2 5 -1 477.88 25.27 7 -2 -1 520.55 25.28 2 5 1 626.63 31.35 6 0 -2 849.79 22.02 -6 6 -2 745.46 37.87 0 6 -2 605.53 33.89 0 6 2 944.96 46.57 0 -6 2 993.20 39.84 6 -6 2 998.92 59.82 0 -6 -2 758.04 49.03 6 0 -2 797.52 21.34 -6 6 2 900.85 38.81 6 -6 -2 680.14 36.61 -2 4 5 1017.43 43.10 2 2 5 958.43 55.15 2 -4 5 1069.41 41.61 -2 -2 5 1123.71 31.41 -4 2 5 1095.11 33.96 4 -2 5 1000.52 42.51 1 -6 -3 2161.12 102.90 1 -6 3 2938.08 121.91 -1 6 3 2686.62 123.85 -1 6 -3 1682.67 85.02 6 -5 -3 1635.12 80.35 6 -5 3 2738.74 119.24 -6 5 3 2809.68 119.63 5 -6 -3 18.65 5.96 1 5 3 34.11 7.05 -1 -5 -3 22.14 6.40 5 -6 3 41.59 10.69 -5 6 3 23.64 9.23 -1 -5 3 35.96 4.73 1 5 -3 8.31 6.52 -5 6 -3 9.38 6.41 -3 7 2 11.16 6.08 4 3 2 15.96 7.22 4 3 -2 7.98 2.87 3 -7 -2 25.43 5.83 -7 4 2 15.87 3.26 3 -7 2 13.06 8.21 7 -4 -2 7.64 3.72 7 -4 2 11.43 4.97 -3 7 -2 19.45 5.38 4 -7 -2 852.78 44.12 3 4 2 922.98 42.77 3 4 -2 722.54 37.75 -4 7 -2 796.00 42.07 -3 -4 2 981.56 37.37 4 -7 2 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552.89 22.68 5 2 2 537.95 25.93 5 2 -2 500.08 20.24 7 -5 2 527.32 39.67 2 -7 -2 494.73 29.07 1 6 -1 872.45 42.79 7 -1 -1 1025.54 34.05 1 6 1 999.99 65.32 -1 -6 1 1063.30 54.65 -1 -6 -1 1005.51 45.07 6 -7 1 1051.18 53.43 -6 7 1 995.51 49.15 -6 7 -1 911.47 46.48 6 -7 -1 934.84 49.01 1 -7 -1 430.83 24.38 6 1 1 418.11 20.27 -1 7 1 389.82 27.02 1 -7 1 396.67 24.32 -7 6 1 370.91 21.20 7 -6 -1 408.13 23.46 -7 6 -1 403.85 23.05 7 -6 1 406.63 25.44 -1 7 -1 380.97 24.33 6 1 -1 441.89 15.23 -2 1 6 199.62 8.88 1 1 6 200.11 13.11 -1 2 6 199.18 16.48 -1 -1 6 197.81 8.20 1 -2 6 221.73 15.45 0 4 5 836.03 39.87 4 -4 5 856.23 49.26 4 -4 -5 642.48 26.97 -4 4 5 875.27 34.53 0 -4 5 978.82 34.28 -6 3 4 1332.74 39.34 3 3 4 1261.03 57.72 3 -6 -4 829.51 44.33 3 3 -4 897.38 24.68 -3 -3 4 1286.94 33.48 -3 6 -4 887.36 44.75 3 -6 4 1444.53 59.58 6 -3 -4 815.14 30.72 -3 6 4 1303.59 75.18 6 -3 4 1177.81 53.27 -2 2 6 1072.52 39.54 -2 0 6 1055.73 31.60 0 2 6 1069.10 44.33 0 -2 6 1160.90 39.01 2 -2 6 1069.11 42.13 6 -6 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758.90 27.35 -3 2 8 785.62 33.80 3 -2 8 762.62 42.03 -6 8 -5 32.02 10.86 6 -8 -5 18.35 14.41 8 -2 5 71.58 12.07 -2 -6 5 58.37 6.98 2 6 5 61.87 20.66 -6 8 5 57.08 12.31 2 6 -5 21.88 5.84 6 -8 5 67.98 13.81 8 -6 -5 255.58 19.58 6 2 5 446.01 48.83 -2 8 5 439.54 39.36 2 -8 -5 400.37 32.80 8 -6 5 485.07 38.01 -8 6 5 487.43 24.21 -2 8 -5 293.43 36.07 2 -8 5 479.77 33.21 -9 9 0 339.95 30.76 9 -9 0 370.29 33.82 9 0 0 395.87 22.60 9 0 0 386.01 21.32 0 -9 0 386.74 43.55 0 9 0 358.44 32.87 -5 5 7 243.99 17.71 5 -5 7 220.19 22.47 0 -5 7 261.37 17.17 0 5 7 253.63 23.11 -3 9 4 904.21 62.28 3 -9 -4 626.73 68.77 -3 9 -4 506.12 43.20 3 -9 4 978.51 56.24 9 -6 4 916.30 55.74 -9 6 4 869.35 36.42 9 -6 -4 314.26 40.57 6 3 4 869.31 52.10 -6 9 4 443.95 35.66 -6 9 -4 299.56 31.30 9 -3 4 475.80 47.61 -3 -6 4 495.64 27.06 3 6 -4 129.25 16.22 9 -3 -4 208.74 12.07 3 6 4 453.06 54.20 6 -9 -4 284.94 29.46 6 -9 4 552.83 39.18 -9 9 -1 17.17 9.01 0 9 -1 20.43 14.11 9 -9 -1 13.84 9.68 0 -9 -1 41.32 8.49 9 0 -1 19.84 7.14 9 0 -1 20.42 4.94 0 9 1 25.01 10.22 9 0 1 0.30 6.82 0 -9 1 33.32 8.06 -9 9 1 20.05 8.67 9 -9 1 32.32 10.65 8 -8 4 23.66 10.03 -8 8 4 8.61 7.36 8 -8 -4 1.56 9.96 0 -8 4 26.90 10.23 0 8 -4 11.08 8.97 0 8 4 9.35 10.55 0 -8 -4 13.05 8.61 -3 3 8 22.28 8.51 3 -3 8 12.72 6.91 -3 0 8 12.11 5.00 0 -3 8 15.83 5.00 -3 0 8 16.63 4.66 0 3 8 19.30 7.17 8 -9 -3 58.91 20.37 -8 9 -3 59.24 14.24 -8 9 3 84.90 14.27 8 -9 3 94.61 26.74 1 8 3 69.30 25.48 -1 -8 3 102.54 11.10 9 -1 3 78.83 12.40 9 -1 -3 63.71 3.60 1 8 -3 34.29 11.85 -1 -8 -3 80.48 13.92 9 -1 -3 30.89 5.70 -9 8 -3 130.98 17.64 -1 9 3 90.62 20.79 1 -9 -3 171.52 17.64 9 -8 -3 77.54 15.49 9 -8 3 127.81 21.12 1 -9 3 90.56 16.50 -9 8 3 97.23 14.33 8 1 -3 91.67 6.37 -1 9 -3 87.99 16.09 8 1 3 80.75 15.85 -3 -3 7 292.27 6.47 3 3 7 303.95 26.39 6 -3 7 247.03 23.82 3 -6 7 301.88 23.69 -6 3 7 278.02 9.68 -3 -3 7 246.37 5.59 -3 6 7 274.08 25.15 3 -10 -2 105.84 25.65 -3 10 -2 45.76 16.17 10 -7 -2 91.11 12.88 7 3 -2 81.03 12.98 10 -7 2 104.55 16.40 7 3 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189.28 24.57 -8 6 6 216.23 20.05 -2 8 -6 106.32 16.18 8 -6 6 229.94 37.19 2 -8 6 214.27 20.61 2 -8 -6 159.50 21.50 7 4 1 357.05 29.26 -4 11 -1 312.25 56.43 -4 11 1 359.64 58.16 11 -7 1 373.43 34.37 11 -7 -1 317.54 43.64 4 -11 -1 354.55 38.02 7 4 -1 370.89 35.92 4 -11 1 415.02 54.82 11 -4 -1 15.22 10.57 7 -11 1 23.51 12.47 -7 11 -1 23.03 11.21 11 -4 1 18.19 8.06 -7 11 1 17.88 11.87 4 7 1 38.63 15.38 4 7 -1 17.87 9.00 7 -11 -1 17.04 11.62 0 -1 9 338.02 20.41 1 0 9 336.60 25.32 0 -1 9 327.59 22.46 -1 1 9 321.17 31.24 -1 0 9 338.40 29.16 -1 0 9 353.30 19.86 0 1 9 306.99 24.52 1 -1 9 332.18 32.07 -2 10 3 20.05 12.71 10 -8 3 23.11 11.54 10 -8 -3 26.75 8.29 8 2 3 8.58 13.58 2 -10 -3 26.68 15.69 8 2 -3 17.41 2.40 -2 10 -3 15.02 9.49 2 -10 3 28.78 10.19 -10 8 3 27.59 7.34 8 2 -3 7.89 2.88 -8 10 3 47.70 13.64 -8 10 -3 63.21 13.91 8 -10 3 79.65 16.59 2 8 -3 46.28 10.22 10 -2 -3 22.64 4.65 10 -2 -3 32.55 6.18 2 8 3 72.17 15.77 -2 -8 3 55.00 8.94 10 -2 3 52.71 11.03 8 -10 -3 48.64 13.58 4 6 4 94.82 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17.74 7.72 -3 -8 1 4.27 11.15 3 8 1 11.42 15.31 3 8 -1 30.29 8.92 -8 11 1 14.30 11.03 -8 11 -1 22.02 10.89 8 -11 -1 17.51 11.87 11 -3 -1 12.65 6.44 8 -11 1 18.69 12.14 -11 8 1 4.21 6.40 11 -8 1 3.27 8.78 3 -11 -1 20.49 8.89 3 -11 1 -0.52 13.60 -3 11 1 5.55 10.03 -3 11 -1 19.61 9.20 8 3 1 2.57 6.67 11 -8 -1 3.08 7.76 8 3 -1 13.86 5.43 -1 8 -6 14.09 7.70 -1 8 6 43.08 14.87 1 -8 6 46.45 9.72 8 -7 6 37.27 13.56 7 1 6 31.86 12.91 -8 7 6 30.57 13.53 8 -7 -6 19.56 7.05 -7 8 6 9.63 7.43 1 7 6 4.53 15.74 -1 -7 6 12.30 8.15 7 -8 -6 9.98 5.83 1 7 -6 2.54 4.34 7 -8 6 19.14 14.14 -5 5 8 560.91 43.70 5 -5 8 550.17 41.13 0 -5 8 606.43 31.08 0 5 8 511.45 41.99 6 -7 7 529.51 59.25 6 -7 -7 305.79 26.54 -1 -6 7 565.06 36.89 1 6 7 492.87 60.44 -6 7 7 494.42 48.20 -7 6 7 227.23 25.74 1 -7 7 246.32 20.74 -1 7 7 234.32 29.50 6 1 7 247.82 28.89 7 -6 7 220.47 27.60 -9 9 4 187.92 19.69 0 9 4 163.31 29.66 0 -9 -4 138.28 23.06 0 9 -4 63.19 25.28 0 -9 4 188.79 27.49 9 -9 4 147.48 41.58 9 -9 -4 24.84 27.53 10 0 0 253.55 18.40 10 0 0 269.20 20.26 0 -10 0 310.22 27.40 0 10 0 261.14 32.23 -10 10 0 225.20 29.24 10 -10 0 268.85 32.01 -2 3 9 81.14 11.75 3 -1 9 65.09 13.34 1 2 9 61.93 13.69 -1 -2 9 79.91 8.87 2 -3 9 88.51 12.03 -1 -2 9 60.72 8.38 -3 1 9 62.27 7.22 -3 1 9 67.35 12.65 1 -3 9 367.65 23.66 -1 3 9 315.30 26.66 -2 -1 9 322.22 16.60 3 -2 9 318.47 26.37 -3 2 9 338.55 21.55 2 1 9 290.31 28.61 -2 -1 9 359.10 17.63 6 -3 8 38.77 13.74 -3 6 8 21.72 9.07 3 -6 8 -0.13 8.35 -6 3 8 16.01 4.05 3 3 8 27.05 9.73 -10 10 -1 85.88 17.96 10 0 -1 74.65 10.39 10 -10 -1 76.94 28.38 10 0 -1 67.29 9.85 -10 10 1 80.17 16.49 0 -10 1 93.41 16.95 0 10 1 130.44 19.39 10 -10 1 110.39 20.92 10 0 1 101.87 12.77 10 0 1 118.38 13.51 0 10 -1 69.61 18.48 0 -10 -1 89.91 16.92 5 6 3 78.83 18.05 11 -5 3 84.12 23.48 -6 11 3 72.67 30.52 -6 11 -3 56.24 16.80 6 -11 -3 70.41 16.94 6 -11 3 93.36 20.43 5 6 -3 44.51 9.93 11 -5 -3 36.52 9.82 1 9 3 132.72 24.22 10 -1 -3 74.49 5.45 -1 -9 -3 113.48 19.80 -9 10 3 103.39 19.13 9 -10 -3 85.62 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14.90 11 -12 3 6.54 23.18 -1 -11 3 13.45 9.21 -1 -11 -3 15.50 12.08 -11 12 3 1.99 11.58 1 11 -3 17.54 9.96 12 -1 3 19.65 10.11 12 -1 3 13.63 14.71 10 3 2 7.33 10.94 -3 13 2 17.84 16.84 13 -10 -2 3.05 12.00 -13 10 2 31.01 10.56 3 -13 -2 25.46 13.78 3 -13 2 36.17 21.84 -3 13 -2 -3.85 20.79 13 -10 2 20.23 14.99 10 -13 -2 5.49 10.85 -10 13 -2 -9.44 10.60 -10 13 2 -4.73 10.71 13 -3 2 14.24 8.18 -3 -10 2 1.37 7.27 10 -13 2 11.58 13.24 3 10 2 21.79 16.86 3 10 -2 25.15 13.17 0 12 0 -20.32 9.67 0 -12 0 7.23 8.39 -12 12 0 0.50 13.57 12 -12 0 8.35 10.21 12 0 0 -20.05 8.85 12 0 0 6.28 8.55 -2 11 -6 30.23 14.79 11 -9 6 125.47 24.82 -2 11 6 54.65 41.78 -11 9 6 63.92 19.83 2 -11 -6 2.15 20.73 9 2 6 104.81 33.46 11 -9 -6 8.63 12.04 2 -11 6 105.41 19.10 9 -11 -6 36.81 18.47 11 -2 6 91.27 22.80 9 -11 6 105.17 29.61 -9 11 6 125.46 24.18 2 9 6 108.76 31.71 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 27074