data_haywoodite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'haywoodite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H20 O42.89 Pb1.08 S3 Zn12' _chemical_formula_weight 1810.86 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 8.35298(19) _cell_length_b 13.2769(7) _cell_length_c 18.2744(13) _cell_angle_alpha 92.427(8) _cell_angle_beta 90.419(6) _cell_angle_gamma 108.214(4) _cell_volume 1922.94(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31751 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description wedge _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.128 _exptl_crystal_F_000 1719 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 12.333 _shelx_estimated_absorpt_T_min 0.319 _shelx_estimated_absorpt_T_max 0.525 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.668 _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 45031 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.234 _diffrn_reflns_theta_max 27.451 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 8748 _reflns_number_gt 6880 _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^)+(0.0479P)^2^+4.6924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8748 _refine_ls_number_parameters 641 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.46261(3) 0.84452(2) 0.34222(2) 0.03784(10) Uani 0.9267(17) 1 d . . P . . Pb2 Pb 0.2080(3) 0.49411(16) 0.99629(12) 0.0440(8) Uani 0.1283(13) 1 d . . P . . Pb3 Pb 0.8721(10) 0.8245(6) 0.3281(4) 0.034(3) Uiso 0.0287(12) 1 d . . P . . Zn1 Zn 0.55545(7) 0.61863(4) 0.44517(3) 0.01626(14) Uani 1 1 d . . . . . Zn2 Zn 0.77468(7) 0.05099(4) 0.22225(3) 0.01616(14) Uani 1 1 d . . . . . Zn3 Zn 0.89139(7) 0.28133(4) 0.11379(3) 0.01749(14) Uani 1 1 d . . . . . Zn4 Zn 0.17807(7) 0.39935(4) 0.40791(3) 0.01734(14) Uani 1 1 d . . . . . Zn5 Zn 0.15566(7) 0.26577(4) 0.26026(3) 0.01716(14) Uani 1 1 d . . . . . Zn6 Zn 0.50862(7) 0.21777(4) 0.20659(3) 0.01772(14) Uani 1 1 d . . . . . Zn7 Zn 0.15987(7) 0.11927(4) 0.12578(3) 0.01766(14) Uani 1 1 d . . . . . Zn8 Zn 0.51064(7) 0.36651(5) 0.35982(3) 0.01774(14) Uani 1 1 d . . . . . Zn9 Zn 0.82518(7) 0.30498(4) 0.30664(3) 0.01711(14) Uani 1 1 d . . . . . Zn10 Zn 0.17377(7) 0.54596(4) 0.54247(3) 0.01733(14) Uani 1 1 d . . . . . Zn11 Zn 0.51201(7) 0.06827(4) 0.07341(3) 0.01772(14) Uani 1 1 d . . . . . Zn12 Zn 0.84225(7) 0.03085(5) 0.02711(3) 0.01825(14) Uani 1 1 d . . . . . S1 S 0.30260(15) 0.09194(10) 0.35995(7) 0.0185(3) Uani 1 1 d . . . . . S2 S 0.03527(16) 0.57511(10) 0.30443(7) 0.0193(3) Uani 1 1 d . . . . . S3 S 0.63587(16) 0.75995(10) 0.03248(7) 0.0211(3) Uani 1 1 d . . . . . O1 O 0.2599(6) 0.1202(3) 0.4340(2) 0.0366(10) Uani 1 1 d . . . . . O2 O 0.1587(5) 0.0108(3) 0.3243(2) 0.0349(10) Uani 1 1 d . . . . . O3 O 0.4502(5) 0.0543(3) 0.3628(2) 0.0349(10) Uani 1 1 d . . . . . O4 O 0.3461(4) 0.1901(3) 0.31606(18) 0.0195(7) Uani 1 1 d . . . . . O5 O 0.8845(5) 0.6047(4) 0.2881(3) 0.0449(11) Uani 1 1 d . . . . . O6 O 0.1552(5) 0.6603(3) 0.3490(2) 0.0373(10) Uani 1 1 d . . . . . O7 O 0.1118(6) 0.5519(3) 0.2364(2) 0.0384(10) Uani 1 1 d . . . . . O8 O 0.9849(4) 0.4772(3) 0.34821(18) 0.0185(7) Uani 1 1 d . . . . . O9 O 0.4981(7) 0.6766(3) 0.9958(3) 0.0531(14) Uani 1 1 d . . . . . O10 O 0.5853(7) 0.7887(4) 0.1048(2) 0.0545(14) Uani 1 1 d . . . . . O11 O 0.7841(6) 0.7246(4) 0.0401(3) 0.0567(14) Uani 1 1 d . . . . . O12 O 0.6804(4) 0.8559(3) 0.98703(19) 0.0209(7) Uani 1 1 d . . . . . OH1 O 0.6130(5) 0.7419(3) 0.3862(3) 0.0377(10) Uani 1 1 d D . . . . H1 H 0.707(5) 0.776(5) 0.381(4) 0.057 Uiso 1 1 d D U . . . OH2 O 0.3087(4) 0.5572(3) 0.44553(18) 0.0165(7) Uani 1 1 d D . . . . H2 H 0.270(7) 0.598(4) 0.424(3) 0.025 Uiso 1 1 d D U . . . OH3 O 0.6586(4) 0.5168(3) 0.40082(19) 0.0179(7) Uani 1 1 d D . . . . H3 H 0.714(7) 0.546(4) 0.366(2) 0.027 Uiso 1 1 d D U . . . OH4 O 0.6435(4) 0.6597(3) 0.54629(19) 0.0177(7) Uani 1 1 d D . . . . H4 H 0.670(7) 0.723(2) 0.543(3) 0.027 Uiso 1 1 d D U . . . OH5 O 0.7097(5) 0.9323(3) 0.2863(2) 0.0336(9) Uani 1 1 d D . . . . H5 H 0.743(9) 0.883(4) 0.279(4) 0.050 Uiso 1 1 d D U . . . OH6 O 0.6779(4) 0.1574(3) 0.26322(19) 0.0175(7) Uani 1 1 d D . . . . H6 H 0.619(7) 0.125(4) 0.295(3) 0.026 Uiso 1 1 d D U . . . OH7 O 0.6890(4) 0.0082(3) 0.12120(19) 0.0186(7) Uani 1 1 d D . . . . H7 H 0.633(7) -0.055(3) 0.125(3) 0.028 Uiso 1 1 d D U . . . OH8 O 0.0223(4) 0.1089(3) 0.22105(18) 0.0167(7) Uani 1 1 d D . . . . H8 H 0.055(7) 0.068(4) 0.245(3) 0.025 Uiso 1 1 d D U . . . OH9 O 0.6460(4) 0.2288(3) 0.10979(18) 0.0171(7) Uani 1 1 d D . . . . H9 H 0.621(7) 0.267(4) 0.083(3) 0.026 Uiso 1 1 d D U . . . OH10 O 0.9815(4) 0.3292(3) 0.21279(19) 0.0175(7) Uani 1 1 d D . . . . H10 H 1.030(7) 0.392(2) 0.212(3) 0.026 Uiso 1 1 d D U . . . OH11 O 0.9924(4) 0.1804(3) 0.06821(19) 0.0185(7) Uani 1 1 d D . . . . H11 H 1.045(7) 0.209(4) 0.034(2) 0.028 Uiso 1 1 d D U . . . OH12 O 0.6991(4) 0.3157(3) 0.40237(18) 0.0155(7) Uani 1 1 d D . . . . H12 H 0.679(7) 0.270(4) 0.430(3) 0.023 Uiso 1 1 d D U . . . OH13 O 0.0321(4) 0.9805(3) 0.06941(18) 0.0156(7) Uani 1 1 d D . . . . H13 H 0.011(7) 0.930(3) 0.093(3) 0.023 Uiso 1 1 d D U . . . OH14 O 0.6352(4) 0.3556(3) 0.26342(18) 0.0160(7) Uani 1 1 d D . . . . H14 H 0.647(8) 0.403(3) 0.238(3) 0.024 Uiso 1 1 d D U . . . OH15 O 0.3067(4) 0.2645(3) 0.17233(18) 0.0161(7) Uani 1 1 d D . . . . H15 H 0.341(7) 0.317(3) 0.146(3) 0.024 Uiso 1 1 d D U . . . OH16 O 0.3621(4) 0.0745(3) 0.15861(18) 0.0157(7) Uani 1 1 d D . . . . H16 H 0.333(7) 0.020(3) 0.181(3) 0.024 Uiso 1 1 d D U . . . OH17 O 0.3147(4) 0.4022(3) 0.31335(19) 0.0169(7) Uani 1 1 d D . . . . H17 H 0.336(7) 0.453(3) 0.289(3) 0.025 Uiso 1 1 d D U . . . OH18 O 0.0248(4) 0.4036(3) 0.49397(18) 0.0165(7) Uani 1 1 d D . . . . H18 H -0.009(7) 0.350(3) 0.518(3) 0.025 Uiso 1 1 d D U . . . OH19 O 0.6481(4) 0.0682(3) 0.97984(18) 0.0166(7) Uani 1 1 d D . . . . H19 H 0.685(7) 0.123(3) 0.960(3) 0.025 Uiso 1 1 d D U . . . OH20 O 0.0187(4) 0.2667(3) 0.35326(18) 0.0154(7) Uani 1 1 d D . . . . H20 H -0.012(7) 0.214(3) 0.377(3) 0.023 Uiso 1 1 d D U . . . W1 O 0.9659(6) 0.4100(4) 0.0544(3) 0.0468(12) Uani 1 1 d . . . . . W2 O 0.2578(9) 0.8674(5) 0.2122(4) 0.0826(19) Uani 1 1 d . . . . . W3 O 0.3869(15) 0.8550(6) 0.4899(4) 0.146(4) Uani 1 1 d . . . . . W4 O 0.9876(8) 0.8193(5) 0.3952(4) 0.0794(19) Uani 0.9713(12) 1 d . . P . . W5 O 0.1421(16) 0.4386(7) 0.8819(4) 0.151(5) Uani 1 1 d . . . . . W6 O 0.3180(11) 0.4785(6) 0.0598(6) 0.117(4) Uani 0.8717(13) 1 d . . P . . W7 O 0.8796(8) 0.7946(5) 0.2141(4) 0.069(3) Uani 0.926(18) 1 d . . P . . W8 O 0.2023(10) 0.7266(7) 0.0881(4) 0.094(4) Uani 0.89(2) 1 d . . P . . W9A O 0.4473(9) 0.6952(7) 0.2315(4) 0.051(3) Uani 0.678(17) 1 d . . P . . W9B O 0.467(3) 0.6084(19) 0.2480(12) 0.081(9) Uani 0.322(17) 1 d . . P . . W10A O 0.8695(17) 0.0591(11) 0.4210(7) 0.081(5) Uani 0.60(2) 1 d . . P . . W10B O 0.9588(18) 0.1163(12) 0.4617(8) 0.049(6) Uani 0.40(2) 1 d . . P . . W11 O 0.458(3) 0.4828(13) 0.8283(11) 0.223(13) Uani 0.75(3) 1 d . . P . . W12 O 0.6633(14) 0.9625(9) 0.4475(7) 0.067(5) Uani 0.480(17) 1 d . . 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 0.03000(15) 0.03744(16) 0.04802(17) 0.02356(11) 0.00702(11) 0.01043(11) Pb2 0.0343(12) 0.0424(13) 0.0566(15) 0.0330(10) 0.0056(9) 0.0100(9) Zn1 0.0142(3) 0.0182(3) 0.0164(3) -0.0013(2) -0.0010(2) 0.0056(2) Zn2 0.0143(3) 0.0178(3) 0.0165(3) -0.0013(2) -0.0005(2) 0.0054(2) Zn3 0.0146(3) 0.0200(3) 0.0173(3) -0.0032(2) -0.0009(2) 0.0053(2) Zn4 0.0129(3) 0.0219(3) 0.0168(3) -0.0076(2) -0.0013(2) 0.0060(2) Zn5 0.0124(3) 0.0221(3) 0.0165(3) -0.0074(2) -0.0014(2) 0.0058(2) Zn6 0.0132(3) 0.0218(3) 0.0183(3) -0.0078(2) -0.0044(2) 0.0069(2) Zn7 0.0131(3) 0.0217(3) 0.0182(3) -0.0079(2) -0.0043(2) 0.0068(2) Zn8 0.0125(3) 0.0254(3) 0.0163(3) -0.0059(2) -0.0029(2) 0.0083(2) Zn9 0.0121(3) 0.0238(3) 0.0163(3) -0.0057(2) -0.0028(2) 0.0078(2) Zn10 0.0129(3) 0.0212(3) 0.0178(3) -0.0075(2) -0.0041(2) 0.0064(2) Zn11 0.0129(3) 0.0234(3) 0.0163(3) -0.0077(2) -0.0011(2) 0.0059(2) Zn12 0.0125(3) 0.0263(3) 0.0169(3) -0.0071(2) -0.0032(2) 0.0085(2) S1 0.0196(6) 0.0176(6) 0.0180(6) 0.0013(5) -0.0009(5) 0.0054(5) S2 0.0206(6) 0.0179(6) 0.0192(6) 0.0018(5) -0.0001(5) 0.0055(5) S3 0.0221(6) 0.0200(6) 0.0207(6) 0.0013(5) 0.0001(5) 0.0059(5) O1 0.056(3) 0.032(2) 0.023(2) 0.0020(17) 0.0094(19) 0.017(2) O2 0.031(2) 0.022(2) 0.044(2) 0.0027(17) -0.0140(19) -0.0033(17) O3 0.028(2) 0.031(2) 0.053(3) 0.0179(19) 0.0071(19) 0.0178(18) O4 0.0193(18) 0.0192(18) 0.0197(18) 0.0023(14) -0.0021(14) 0.0053(14) O5 0.032(2) 0.055(3) 0.054(3) 0.026(2) 0.002(2) 0.019(2) O6 0.042(3) 0.020(2) 0.040(2) 0.0010(17) -0.0126(19) -0.0039(18) O7 0.052(3) 0.032(2) 0.027(2) 0.0022(17) 0.0193(19) 0.008(2) O8 0.0178(18) 0.0168(17) 0.0199(17) 0.0016(14) -0.0001(14) 0.0039(14) O9 0.061(3) 0.026(2) 0.057(3) 0.005(2) -0.032(3) -0.007(2) O10 0.093(4) 0.031(2) 0.033(2) 0.0039(19) 0.032(3) 0.010(3) O11 0.042(3) 0.069(3) 0.076(4) 0.045(3) 0.016(2) 0.034(3) O12 0.0221(19) 0.0186(18) 0.0214(18) 0.0027(14) 0.0001(14) 0.0052(15) OH1 0.031(2) 0.034(2) 0.052(3) 0.024(2) 0.007(2) 0.0127(19) OH2 0.0145(17) 0.0169(17) 0.0183(17) 0.0002(13) -0.0026(13) 0.0050(14) OH3 0.0156(18) 0.0205(18) 0.0178(17) -0.0028(14) -0.0008(14) 0.0067(14) OH4 0.0160(17) 0.0181(17) 0.0190(17) -0.0027(14) -0.0019(14) 0.0059(15) OH5 0.035(2) 0.026(2) 0.044(2) 0.0156(19) 0.0123(19) 0.0123(18) OH6 0.0156(18) 0.0199(18) 0.0170(17) -0.0015(14) -0.0020(13) 0.0060(14) OH7 0.0137(17) 0.0206(18) 0.0199(18) -0.0032(14) -0.0004(14) 0.0038(14) OH8 0.0126(17) 0.0186(18) 0.0181(17) -0.0010(14) -0.0017(13) 0.0040(14) OH9 0.0154(17) 0.0182(18) 0.0169(17) 0.0005(14) -0.0029(14) 0.0041(14) OH10 0.0131(17) 0.0185(17) 0.0191(17) -0.0057(14) -0.0011(13) 0.0033(14) OH11 0.0164(18) 0.0214(18) 0.0170(17) -0.0013(14) -0.0013(14) 0.0052(15) OH12 0.0157(17) 0.0153(17) 0.0155(17) -0.0032(13) -0.0005(13) 0.0053(14) OH13 0.0163(17) 0.0165(17) 0.0143(16) -0.0041(13) -0.0014(13) 0.0062(14) OH14 0.0164(17) 0.0164(17) 0.0160(17) -0.0017(13) -0.0016(13) 0.0067(14) OH15 0.0127(16) 0.0191(17) 0.0180(17) -0.0008(13) 0.0004(13) 0.0074(14) OH16 0.0152(17) 0.0174(17) 0.0154(17) -0.0039(13) -0.0001(13) 0.0070(14) OH17 0.0136(17) 0.0181(17) 0.0186(17) -0.0016(14) -0.0023(13) 0.0047(14) OH18 0.0121(16) 0.0180(17) 0.0192(17) -0.0016(14) 0.0001(13) 0.0047(14) OH19 0.0119(16) 0.0195(18) 0.0167(17) -0.0051(14) -0.0031(13) 0.0031(14) OH20 0.0118(16) 0.0179(17) 0.0168(17) -0.0023(13) -0.0019(13) 0.0054(14) W1 0.054(3) 0.036(2) 0.049(3) 0.023(2) 0.007(2) 0.009(2) W2 0.095(5) 0.064(4) 0.094(5) 0.027(3) 0.024(4) 0.028(4) W3 0.303(13) 0.068(5) 0.076(5) -0.018(4) -0.080(7) 0.079(7) W4 0.074(4) 0.055(4) 0.106(5) -0.015(4) 0.004(4) 0.018(3) W5 0.293(13) 0.105(6) 0.094(6) -0.030(5) -0.074(7) 0.124(8) W6 0.090(6) 0.061(5) 0.178(10) -0.029(6) 0.057(7) -0.004(4) W7 0.076(5) 0.056(4) 0.081(5) -0.013(3) -0.018(4) 0.033(3) W8 0.087(6) 0.099(7) 0.080(6) -0.006(5) 0.005(4) 0.010(5) W9A 0.047(5) 0.051(6) 0.048(4) 0.007(3) 0.012(3) 0.005(4) W9B 0.061(13) 0.087(19) 0.091(16) -0.006(12) -0.005(11) 0.021(11) W10A 0.080(9) 0.094(10) 0.076(8) -0.009(7) 0.001(7) 0.040(8) W10B 0.051(9) 0.049(9) 0.048(9) 0.014(7) 0.010(7) 0.015(7) W11 0.30(3) 0.145(15) 0.28(2) 0.133(15) 0.124(19) 0.125(15) W12 0.057(8) 0.066(8) 0.080(9) 0.041(6) -0.007(6) 0.019(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 OH1 2.287(4) . ? Pb1 OH5 2.300(4) . ? Pb1 W12 2.650(12) . ? Pb1 W9A 2.746(8) . ? Pb1 W3 2.784(9) . ? Pb1 O3 2.828(4) 1_565 ? Pb1 O6 2.949(4) . ? Pb1 W2 2.999(7) . ? Pb1 W9B 3.52(2) . ? Pb1 Pb3 3.524(8) . ? Pb1 O2 3.870(4) 1_565 ? Pb1 Zn1 3.8789(6) . ? Pb1 Zn2 3.9042(7) 1_565 ? Pb1 W10A 3.908(16) 1_565 ? Pb1 S1 3.9170(12) 1_565 ? Pb2 W6 1.535(13) 1_556 ? Pb2 W5 2.195(8) . ? Pb2 W1 2.277(5) 1_456 ? Pb2 W1 2.414(5) 2_666 ? Pb2 O9 2.841(5) . ? Pb2 O11 2.972(6) 2_666 ? Pb2 W8 3.464(9) 1_556 ? Pb2 Pb2 3.531(4) 2_567 ? Pb2 W11 3.748(17) . ? Pb2 O9 3.831(6) 2_667 ? Pb2 Zn3 3.9386(19) 1_456 ? Pb2 Zn3 3.9568(19) 2_666 ? Pb2 W5 3.984(11) 2_567 ? Pb2 S3 3.995(2) 2_666 ? Pb2 W8 3.997(9) 2_566 ? Pb3 W4 1.571(11) . ? Pb3 W7 2.110(10) . ? Pb3 OH1 2.379(9) . ? Pb3 OH5 2.402(9) . ? Pb3 O2 2.858(9) 1_665 ? Pb3 O5 3.011(9) . ? Pb3 W10A 3.491(15) 1_565 ? Pb3 W12 3.588(15) . ? Pb3 O6 3.710(9) 1_655 ? Pb3 W2 3.774(10) 1_655 ? Pb3 W9A 3.808(11) . ? Pb3 Zn1 3.886(8) . ? Pb3 W9B 3.91(2) . ? Pb3 Zn2 3.931(8) 1_565 ? Pb3 H1 1.67(5) . ? Pb3 H5 1.77(6) . ? Zn1 OH1 1.933(4) . ? Zn1 OH2 1.966(3) . ? Zn1 OH3 1.968(3) . ? Zn1 OH4 1.974(3) . ? Zn2 OH5 1.944(4) 1_545 ? Zn2 OH6 1.961(3) . ? Zn2 OH8 1.969(3) 1_655 ? Zn2 OH7 1.970(3) . ? Zn3 OH9 1.947(3) . ? Zn3 OH11 1.955(3) . ? Zn3 OH10 1.956(3) . ? Zn3 W1 1.997(4) . ? Zn4 OH18 2.045(3) . ? Zn4 OH20 2.058(3) . ? Zn4 OH17 2.073(3) . ? Zn4 OH4 2.075(3) 2_666 ? Zn4 OH2 2.119(3) . ? Zn4 O8 2.444(3) 1_455 ? Zn4 Zn8 3.0725(7) . ? Zn4 Zn10 3.0783(8) . ? Zn4 Zn5 3.1370(8) . ? Zn5 OH15 2.053(3) . ? Zn5 OH20 2.057(3) . ? Zn5 OH17 2.078(3) . ? Zn5 OH10 2.095(3) 1_455 ? Zn5 OH8 2.122(3) . ? Zn5 O4 2.375(3) . ? Zn5 Zn7 3.0762(8) . ? Zn5 Zn9 3.0830(7) 1_455 ? Zn6 OH14 2.039(3) . ? Zn6 OH16 2.067(3) . ? Zn6 OH15 2.072(3) . ? Zn6 OH9 2.101(3) . ? Zn6 OH6 2.114(3) . ? Zn6 O4 2.402(3) . ? Zn6 Zn11 3.0808(8) . ? Zn6 Zn9 3.0841(8) . ? Zn6 Zn7 3.1256(8) . ? Zn7 OH13 2.047(3) 1_545 ? Zn7 OH16 2.052(3) . ? Zn7 OH15 2.077(3) . ? Zn7 OH8 2.079(3) . ? Zn7 OH11 2.118(3) 1_455 ? Zn7 O12 2.442(4) 2_666 ? Zn7 Zn12 3.0776(8) 1_455 ? Zn8 OH17 2.031(3) . ? Zn8 OH12 2.057(3) . ? Zn8 OH14 2.075(3) . ? Zn8 OH3 2.095(4) . ? Zn8 OH4 2.127(4) 2_666 ? Zn8 O4 2.414(3) . ? Zn8 Zn10 3.0543(8) 2_666 ? Zn8 Zn9 3.1346(8) . ? Zn9 OH20 2.031(3) 1_655 ? Zn9 OH14 2.071(3) . ? Zn9 OH12 2.071(3) . ? Zn9 OH6 2.081(3) . ? Zn9 OH10 2.137(3) . ? Zn9 O8 2.349(3) . ? Zn10 OH12 2.031(3) 2_666 ? Zn10 OH18 2.068(3) . ? Zn10 OH18 2.087(3) 2_566 ? Zn10 OH2 2.092(3) . ? Zn10 OH3 2.123(3) 2_666 ? Zn10 O8 2.383(3) 2_666 ? Zn10 Zn10 3.1440(11) 2_566 ? Zn11 OH16 2.020(3) . ? Zn11 OH19 2.061(3) 1_554 ? Zn11 OH19 2.083(3) 2_656 ? Zn11 OH7 2.089(4) . ? Zn11 OH9 2.148(3) . ? Zn11 O12 2.428(3) 2_666 ? Zn11 Zn12 3.0704(7) . ? Zn11 Zn11 3.1429(11) 2_655 ? Zn12 OH19 2.035(3) 1_554 ? Zn12 OH13 2.061(3) 1_645 ? Zn12 OH13 2.083(3) 2_665 ? Zn12 OH11 2.094(4) . ? Zn12 OH7 2.126(4) . ? Zn12 O12 2.374(4) 1_544 ? Zn12 Zn12 3.1492(10) 2_755 ? S1 O1 1.466(4) . ? S1 O2 1.466(4) . ? S1 O3 1.470(4) . ? S1 O4 1.507(4) . ? S2 O5 1.464(4) 1_455 ? S2 O6 1.466(4) . ? S2 O7 1.468(4) . ? S2 O8 1.502(4) 1_455 ? S3 O9 1.459(4) 1_554 ? S3 O10 1.462(4) . ? S3 O11 1.462(4) . ? S3 O12 1.500(4) 1_554 ? OH1 H1 0.78(3) . ? OH2 H2 0.83(3) . ? OH3 H3 0.82(3) . ? OH4 H4 0.80(3) . ? OH5 H5 0.80(3) . ? OH6 H6 0.81(3) . ? OH7 H7 0.83(3) . ? OH8 H8 0.82(3) . ? OH9 H9 0.80(3) . ? OH10 H10 0.81(3) . ? OH11 H11 0.81(3) . ? OH12 H12 0.79(3) . ? OH13 H13 0.79(3) . ? OH14 H14 0.78(3) . ? OH15 H15 0.84(3) . ? OH16 H16 0.81(3) . ? OH17 H17 0.80(3) . ? OH18 H18 0.83(3) . ? OH19 H19 0.80(3) . ? OH20 H20 0.80(3) . ? W9A W9B 1.26(2) . ? W10A W10B 1.129(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 OH1 Pb1 OH5 84.51(14) . . ? OH1 Pb1 W12 74.2(3) . . ? OH5 Pb1 W12 74.3(3) . . ? OH1 Pb1 W9A 75.2(2) . . ? OH5 Pb1 W9A 82.16(18) . . ? W12 Pb1 W9A 142.7(3) . . ? OH1 Pb1 W3 81.1(2) . . ? OH5 Pb1 W3 127.9(3) . . ? W12 Pb1 W3 53.6(3) . . ? W9A Pb1 W3 139.5(2) . . ? OH1 Pb1 O3 138.41(15) . 1_565 ? OH5 Pb1 O3 81.28(13) . 1_565 ? W12 Pb1 O3 64.3(2) . 1_565 ? W9A Pb1 O3 140.0(2) . 1_565 ? W3 Pb1 O3 77.49(17) . 1_565 ? OH1 Pb1 O6 88.50(14) . . ? OH5 Pb1 O6 150.41(14) . . ? W12 Pb1 O6 131.0(3) . . ? W9A Pb1 O6 68.26(17) . . ? W3 Pb1 O6 78.9(2) . . ? O3 Pb1 O6 121.11(12) 1_565 . ? OH1 Pb1 W2 142.45(17) . . ? OH5 Pb1 W2 91.39(16) . . ? W12 Pb1 W2 140.2(2) . . ? W9A Pb1 W2 67.3(2) . . ? W3 Pb1 W2 128.1(2) . . ? O3 Pb1 W2 76.99(15) 1_565 . ? O6 Pb1 W2 76.93(15) . . ? OH1 Pb1 W9B 58.5(4) . . ? OH5 Pb1 W9B 88.8(4) . . ? W12 Pb1 W9B 131.2(4) . . ? W9A Pb1 W9B 18.4(4) . . ? W3 Pb1 W9B 123.2(4) . . ? O3 Pb1 W9B 158.4(4) 1_565 . ? O6 Pb1 W9B 63.3(4) . . ? W2 Pb1 W9B 84.1(4) . . ? OH1 Pb1 Pb3 41.96(17) . . ? OH5 Pb1 Pb3 42.57(17) . . ? W12 Pb1 Pb3 69.4(3) . . ? W9A Pb1 Pb3 73.6(2) . . ? W3 Pb1 Pb3 108.6(3) . . ? O3 Pb1 Pb3 114.64(16) 1_565 . ? O6 Pb1 Pb3 123.92(16) . . ? W2 Pb1 Pb3 123.00(18) . . ? W9B Pb1 Pb3 67.5(4) . . ? OH1 Pb1 O2 163.49(13) . 1_565 ? OH5 Pb1 O2 107.87(11) . 1_565 ? W12 Pb1 O2 98.2(2) . 1_565 ? W9A Pb1 O2 116.55(19) . 1_565 ? W3 Pb1 O2 82.68(19) . 1_565 ? O3 Pb1 O2 38.39(10) 1_565 1_565 ? O6 Pb1 O2 85.67(10) . 1_565 ? W2 Pb1 O2 50.44(14) . 1_565 ? W9B Pb1 O2 130.6(3) . 1_565 ? Pb3 Pb1 O2 149.38(15) . 1_565 ? OH1 Pb1 Zn1 21.20(10) . . ? OH5 Pb1 Zn1 105.68(10) . . ? W12 Pb1 Zn1 81.6(2) . . ? W9A Pb1 Zn1 77.46(18) . . ? W3 Pb1 Zn1 69.01(15) . . ? O3 Pb1 Zn1 142.24(9) 1_565 . ? O6 Pb1 Zn1 69.49(8) . . ? W2 Pb1 Zn1 138.23(12) . . ? W9B Pb1 Zn1 59.1(4) . . ? Pb3 Pb1 Zn1 63.12(13) . . ? O2 Pb1 Zn1 145.03(6) 1_565 . ? OH1 Pb1 Zn2 105.62(10) . 1_565 ? OH5 Pb1 Zn2 21.11(10) . 1_565 ? W12 Pb1 Zn2 80.9(2) . 1_565 ? W9A Pb1 Zn2 87.42(15) . 1_565 ? W3 Pb1 Zn2 130.90(19) . 1_565 ? O3 Pb1 Zn2 65.57(8) 1_565 1_565 ? O6 Pb1 Zn2 148.00(8) . 1_565 ? W2 Pb1 Zn2 74.52(12) . 1_565 ? W9B Pb1 Zn2 99.4(4) . 1_565 ? Pb3 Pb1 Zn2 63.66(13) . 1_565 ? O2 Pb1 Zn2 87.20(6) 1_565 1_565 ? Zn1 Pb1 Zn2 126.774(13) . 1_565 ? OH1 Pb1 W10A 78.2(2) . 1_565 ? OH5 Pb1 W10A 49.4(2) . 1_565 ? W12 Pb1 W10A 25.0(3) . 1_565 ? W9A Pb1 W10A 126.4(2) . 1_565 ? W3 Pb1 W10A 78.6(3) . 1_565 ? O3 Pb1 W10A 62.91(18) 1_565 1_565 ? O6 Pb1 W10A 155.4(2) . 1_565 ? W2 Pb1 W10A 125.6(2) . 1_565 ? W9B Pb1 W10A 123.2(3) . 1_565 ? Pb3 Pb1 W10A 55.7(2) . 1_565 ? O2 Pb1 W10A 101.27(17) 1_565 1_565 ? Zn1 Pb1 W10A 93.03(17) . 1_565 ? Zn2 Pb1 W10A 56.58(18) 1_565 1_565 ? OH1 Pb1 S1 151.11(13) . 1_565 ? OH5 Pb1 S1 94.97(10) . 1_565 ? W12 Pb1 S1 77.8(2) . 1_565 ? W9A Pb1 S1 133.51(18) . 1_565 ? W3 Pb1 S1 76.56(15) . 1_565 ? O3 Pb1 S1 17.05(8) 1_565 1_565 ? O6 Pb1 S1 104.66(9) . 1_565 ? W2 Pb1 S1 66.38(12) . 1_565 ? W9B Pb1 S1 150.3(4) . 1_565 ? Pb3 Pb1 S1 131.39(14) . 1_565 ? O2 Pb1 S1 21.70(6) 1_565 1_565 ? Zn1 Pb1 S1 145.57(2) . 1_565 ? Zn2 Pb1 S1 76.69(2) 1_565 1_565 ? W10A Pb1 S1 79.65(16) 1_565 1_565 ? W6 Pb2 W5 139.6(4) 1_556 . ? W6 Pb2 W1 92.2(3) 1_556 1_456 ? W5 Pb2 W1 101.9(4) . 1_456 ? W6 Pb2 W1 149.3(3) 1_556 2_666 ? W5 Pb2 W1 70.8(2) . 2_666 ? W1 Pb2 W1 82.38(17) 1_456 2_666 ? W6 Pb2 O9 76.3(3) 1_556 . ? W5 Pb2 O9 107.5(4) . . ? W1 Pb2 O9 146.1(2) 1_456 . ? W1 Pb2 O9 91.50(16) 2_666 . ? W6 Pb2 O11 79.0(3) 1_556 2_666 ? W5 Pb2 O11 65.3(2) . 2_666 ? W1 Pb2 O11 84.22(16) 1_456 2_666 ? W1 Pb2 O11 129.95(18) 2_666 2_666 ? O9 Pb2 O11 123.33(16) . 2_666 ? W6 Pb2 W8 87.6(3) 1_556 1_556 ? W5 Pb2 W8 130.2(2) . 1_556 ? W1 Pb2 W8 87.60(19) 1_456 1_556 ? W1 Pb2 W8 62.07(19) 2_666 1_556 ? O9 Pb2 W8 60.53(18) . 1_556 ? O11 Pb2 W8 163.98(19) 2_666 1_556 ? W6 Pb2 Pb2 127.7(3) 1_556 2_567 ? W5 Pb2 Pb2 84.8(3) . 2_567 ? W1 Pb2 Pb2 42.66(12) 1_456 2_567 ? W1 Pb2 Pb2 39.72(12) 2_666 2_567 ? O9 Pb2 Pb2 123.57(14) . 2_567 ? O11 Pb2 Pb2 111.97(14) 2_666 2_567 ? W8 Pb2 Pb2 69.68(16) 1_556 2_567 ? W6 Pb2 W11 104.6(5) 1_556 . ? W5 Pb2 W11 45.7(5) . . ? W1 Pb2 W11 143.7(4) 1_456 . ? W1 Pb2 W11 97.2(3) 2_666 . ? O9 Pb2 W11 70.1(4) . . ? O11 Pb2 W11 68.2(2) 2_666 . ? W8 Pb2 W11 124.4(3) 1_556 . ? Pb2 Pb2 W11 127.3(3) 2_567 . ? W6 Pb2 O9 49.8(3) 1_556 2_667 ? W5 Pb2 O9 89.8(2) . 2_667 ? W1 Pb2 O9 108.46(15) 1_456 2_667 ? W1 Pb2 O9 159.65(16) 2_666 2_667 ? O9 Pb2 O9 88.44(13) . 2_667 ? O11 Pb2 O9 38.72(12) 2_666 2_667 ? W8 Pb2 O9 133.64(17) 1_556 2_667 ? Pb2 Pb2 O9 147.69(11) 2_567 2_667 ? W11 Pb2 O9 63.7(3) . 2_667 ? W6 Pb2 Zn3 76.1(3) 1_556 1_456 ? W5 Pb2 Zn3 105.2(3) . 1_456 ? W1 Pb2 Zn3 21.30(12) 1_456 1_456 ? W1 Pb2 Zn3 103.34(12) 2_666 1_456 ? O9 Pb2 Zn3 147.05(13) . 1_456 ? O11 Pb2 Zn3 67.77(10) 2_666 1_456 ? W8 Pb2 Zn3 100.68(15) 1_556 1_456 ? Pb2 Pb2 Zn3 63.70(5) 2_567 1_456 ? W11 Pb2 Zn3 134.9(3) . 1_456 ? O9 Pb2 Zn3 87.33(8) 2_667 1_456 ? W6 Pb2 Zn3 141.7(3) 1_556 2_666 ? W5 Pb2 Zn3 70.0(2) . 2_666 ? W1 Pb2 Zn3 105.74(13) 1_456 2_666 ? W1 Pb2 Zn3 23.66(11) 2_666 2_666 ? O9 Pb2 Zn3 70.01(10) . 2_666 ? O11 Pb2 Zn3 135.27(13) 2_666 2_666 ? W8 Pb2 Zn3 60.38(15) 1_556 2_666 ? Pb2 Pb2 Zn3 63.17(5) 2_567 2_666 ? W11 Pb2 Zn3 80.7(2) . 2_666 ? O9 Pb2 Zn3 143.18(10) 2_667 2_666 ? Zn3 Pb2 Zn3 126.87(5) 1_456 2_666 ? W6 Pb2 W5 97.0(3) 1_556 2_567 ? W5 Pb2 W5 118.0(3) . 2_567 ? W1 Pb2 W5 40.03(19) 1_456 2_567 ? W1 Pb2 W5 59.95(16) 2_666 2_567 ? O9 Pb2 W5 108.9(2) . 2_567 ? O11 Pb2 W5 124.20(18) 2_666 2_567 ? W8 Pb2 W5 48.5(2) 1_556 2_567 ? Pb2 Pb2 W5 33.28(13) 2_567 2_567 ? W11 Pb2 W5 157.2(3) . 2_567 ? O9 Pb2 W5 138.69(15) 2_667 2_567 ? Zn3 Pb2 W5 57.53(14) 1_456 2_567 ? Zn3 Pb2 W5 77.78(12) 2_666 2_567 ? W6 Pb2 S3 66.0(3) 1_556 2_666 ? W5 Pb2 S3 74.9(2) . 2_666 ? W1 Pb2 S3 96.28(13) 1_456 2_666 ? W1 Pb2 S3 144.53(15) 2_666 2_666 ? O9 Pb2 S3 107.31(13) . 2_666 ? O11 Pb2 S3 17.44(10) 2_666 2_666 ? W8 Pb2 S3 153.38(16) 1_556 2_666 ? Pb2 Pb2 S3 128.85(9) 2_567 2_666 ? W11 Pb2 S3 63.4(2) . 2_666 ? O9 Pb2 S3 21.36(7) 2_667 2_666 ? Zn3 Pb2 S3 77.05(4) 1_456 2_666 ? Zn3 Pb2 S3 141.53(7) 2_666 2_666 ? W5 Pb2 S3 134.41(14) 2_567 2_666 ? W6 Pb2 W8 125.2(3) 1_556 2_566 ? W5 Pb2 W8 50.2(4) . 2_566 ? W1 Pb2 W8 52.16(17) 1_456 2_566 ? W1 Pb2 W8 74.13(18) 2_666 2_566 ? O9 Pb2 W8 156.20(17) . 2_566 ? O11 Pb2 W8 59.83(17) 2_666 2_566 ? W8 Pb2 W8 124.06(13) 1_556 2_566 ? Pb2 Pb2 W8 54.37(14) 2_567 2_566 ? W11 Pb2 W8 92.6(4) . 2_566 ? O9 Pb2 W8 98.54(15) 2_667 2_566 ? Zn3 Pb2 W8 56.50(12) 1_456 2_566 ? Zn3 Pb2 W8 91.70(14) 2_666 2_566 ? W5 Pb2 W8 80.57(19) 2_567 2_566 ? S3 Pb2 W8 77.25(14) 2_666 2_566 ? W4 Pb3 W7 134.3(6) . . ? W4 Pb3 OH1 95.5(5) . . ? W7 Pb3 OH1 116.9(4) . . ? W4 Pb3 OH5 139.3(5) . . ? W7 Pb3 OH5 80.5(3) . . ? OH1 Pb3 OH5 80.4(3) . . ? W4 Pb3 O2 74.4(4) . 1_665 ? W7 Pb3 O2 91.7(3) . 1_665 ? OH1 Pb3 O2 145.5(4) . 1_665 ? OH5 Pb3 O2 86.5(3) . 1_665 ? W4 Pb3 O5 84.7(4) . . ? W7 Pb3 O5 66.9(3) . . ? OH1 Pb3 O5 87.2(3) . . ? OH5 Pb3 O5 134.9(4) . . ? O2 Pb3 O5 123.4(3) 1_665 . ? W4 Pb3 W10A 82.3(4) . 1_565 ? W7 Pb3 W10A 128.0(4) . 1_565 ? OH1 Pb3 W10A 86.5(3) . 1_565 ? OH5 Pb3 W10A 57.2(3) . 1_565 ? O2 Pb3 W10A 59.8(3) 1_665 1_565 ? O5 Pb3 W10A 164.9(4) . 1_565 ? W4 Pb3 Pb1 124.6(4) . . ? W7 Pb3 Pb1 100.2(3) . . ? OH1 Pb3 Pb1 39.99(16) . . ? OH5 Pb3 Pb1 40.38(16) . . ? O2 Pb3 Pb1 120.7(3) 1_665 . ? O5 Pb3 Pb1 114.7(3) . . ? W10A Pb3 Pb1 67.7(3) 1_565 . ? W4 Pb3 W12 88.1(4) . . ? W7 Pb3 W12 136.2(4) . . ? OH1 Pb3 W12 55.9(3) . . ? OH5 Pb3 W12 56.0(2) . . ? O2 Pb3 W12 90.5(3) 1_665 . ? O5 Pb3 W12 141.5(3) . . ? W10A Pb3 W12 30.7(3) 1_565 . ? Pb1 Pb3 W12 43.7(2) . . ? W4 Pb3 O6 50.7(3) . 1_655 ? W7 Pb3 O6 87.1(3) . 1_655 ? OH1 Pb3 O6 109.1(3) . 1_655 ? OH5 Pb3 O6 167.0(3) . 1_655 ? O2 Pb3 O6 90.0(2) 1_665 1_655 ? O5 Pb3 O6 40.12(14) . 1_655 ? W10A Pb3 O6 130.6(3) 1_565 1_655 ? Pb1 Pb3 O6 147.9(3) . 1_655 ? W12 Pb3 O6 136.7(3) . 1_655 ? W4 Pb3 W2 86.9(4) . 1_655 ? W7 Pb3 W2 52.5(3) . 1_655 ? OH1 Pb3 W2 162.0(3) . 1_655 ? OH5 Pb3 W2 109.3(3) . 1_655 ? O2 Pb3 W2 52.18(19) 1_665 1_655 ? O5 Pb3 W2 75.1(2) . 1_655 ? W10A Pb3 W2 111.5(3) 1_565 1_655 ? Pb1 Pb3 W2 146.7(3) . 1_655 ? W12 Pb3 W2 142.2(3) . 1_655 ? O6 Pb3 W2 59.25(17) 1_655 1_655 ? W4 Pb3 W9A 145.0(5) . . ? W7 Pb3 W9A 64.2(3) . . ? OH1 Pb3 W9A 54.2(2) . . ? OH5 Pb3 W9A 59.9(2) . . ? O2 Pb3 W9A 140.3(3) 1_665 . ? O5 Pb3 W9A 77.6(2) . . ? W10A Pb3 W9A 109.4(3) 1_565 . ? Pb1 Pb3 W9A 43.78(15) . . ? W12 Pb3 W9A 87.4(3) . . ? O6 Pb3 W9A 117.7(3) 1_655 . ? W2 Pb3 W9A 116.6(3) 1_655 . ? W4 Pb3 Zn1 78.9(4) . . ? W7 Pb3 Zn1 119.7(4) . . ? OH1 Pb3 Zn1 22.97(14) . . ? OH5 Pb3 Zn1 103.3(3) . . ? O2 Pb3 Zn1 148.0(3) 1_665 . ? O5 Pb3 Zn1 70.14(18) . . ? W10A Pb3 Zn1 99.8(3) 1_565 . ? Pb1 Pb3 Zn1 62.91(13) . . ? W12 Pb3 Zn1 71.4(2) . . ? O6 Pb3 Zn1 86.23(18) 1_655 . ? W2 Pb3 Zn1 143.4(2) 1_655 . ? W9A Pb3 Zn1 66.84(18) . . ? W4 Pb3 W9B 129.2(6) . . ? W7 Pb3 W9B 66.6(4) . . ? OH1 Pb3 W9B 50.9(4) . . ? OH5 Pb3 W9B 78.6(4) . . ? O2 Pb3 W9B 155.3(5) 1_665 . ? O5 Pb3 W9B 60.5(4) . . ? W10A Pb3 W9B 123.9(4) 1_565 . ? Pb1 Pb3 W9B 56.2(3) . . ? W12 Pb3 W9B 97.2(4) . . ? O6 Pb3 W9B 100.1(4) 1_655 . ? W2 Pb3 W9B 114.7(4) 1_655 . ? W9A Pb3 W9B 18.7(3) . . ? Zn1 Pb3 W9B 56.0(4) . . ? W4 Pb3 Zn2 135.8(4) . 1_565 ? W7 Pb3 Zn2 69.9(3) . 1_565 ? OH1 Pb3 Zn2 102.9(3) . 1_565 ? OH5 Pb3 Zn2 22.51(14) . 1_565 ? O2 Pb3 Zn2 67.77(18) 1_665 1_565 ? O5 Pb3 Zn2 135.4(3) . 1_565 ? W10A Pb3 Zn2 59.5(2) 1_565 1_565 ? Pb1 Pb3 Zn2 62.89(13) . 1_565 ? W12 Pb3 Zn2 70.6(2) . 1_565 ? O6 Pb3 Zn2 146.7(2) 1_655 1_565 ? W2 Pb3 Zn2 87.46(19) 1_655 1_565 ? W9A Pb3 Zn2 74.2(2) . 1_565 ? Zn1 Pb3 Zn2 125.8(2) . 1_565 ? W9B Pb3 Zn2 92.6(4) . 1_565 ? W4 Pb3 H1 88(3) . . ? W7 Pb3 H1 126(2) . . ? OH1 Pb3 H1 9(2) . . ? OH5 Pb3 H1 83(3) . . ? O2 Pb3 H1 138(2) 1_665 . ? O5 Pb3 H1 92(3) . . ? W10A Pb3 H1 80(3) 1_565 . ? Pb1 Pb3 H1 44(3) . . ? W12 Pb3 H1 50(3) . . ? O6 Pb3 H1 108(3) 1_655 . ? W2 Pb3 H1 166(3) 1_655 . ? W9A Pb3 H1 63(2) . . ? Zn1 Pb3 H1 23(3) . . ? W9B Pb3 H1 60(2) . . ? Zn2 Pb3 H1 105(3) 1_565 . ? W4 Pb3 H5 153.0(19) . . ? W7 Pb3 H5 68.2(19) . . ? OH1 Pb3 H5 82(2) . . ? OH5 Pb3 H5 13.7(18) . . ? O2 Pb3 H5 93(2) 1_665 . ? O5 Pb3 H5 121.8(19) . . ? W10A Pb3 H5 70.8(18) 1_565 . ? Pb1 Pb3 H5 43(2) . . ? W12 Pb3 H5 68.0(19) . . ? O6 Pb3 H5 155.1(19) 1_655 . ? W2 Pb3 H5 104(2) 1_655 . ? W9A Pb3 H5 50(2) . . ? Zn1 Pb3 H5 104(2) . . ? W9B Pb3 H5 69(2) . . ? Zn2 Pb3 H5 25(2) 1_565 . ? H1 Pb3 H5 87(4) . . ? OH1 Zn1 OH2 108.58(16) . . ? OH1 Zn1 OH3 107.73(17) . . ? OH2 Zn1 OH3 110.73(15) . . ? OH1 Zn1 OH4 110.04(18) . . ? OH2 Zn1 OH4 109.86(15) . . ? OH3 Zn1 OH4 109.87(14) . . ? OH1 Zn1 Pb1 25.34(12) . . ? OH2 Zn1 Pb1 84.13(10) . . ? OH3 Zn1 Pb1 124.57(10) . . ? OH4 Zn1 Pb1 114.20(10) . . ? OH1 Zn1 Pb3 28.71(17) . . ? OH2 Zn1 Pb3 134.65(16) . . ? OH3 Zn1 Pb3 84.75(16) . . ? OH4 Zn1 Pb3 103.45(16) . . ? Pb1 Zn1 Pb3 53.97(12) . . ? OH5 Zn2 OH6 106.45(16) 1_545 . ? OH5 Zn2 OH8 109.36(16) 1_545 1_655 ? OH6 Zn2 OH8 110.55(15) . 1_655 ? OH5 Zn2 OH7 111.81(17) 1_545 . ? OH6 Zn2 OH7 109.87(14) . . ? OH8 Zn2 OH7 108.79(14) 1_655 . ? OH5 Zn2 Pb1 25.23(12) 1_545 1_545 ? OH6 Zn2 Pb1 87.62(11) . 1_545 ? OH8 Zn2 Pb1 133.14(10) 1_655 1_545 ? OH7 Zn2 Pb1 104.19(11) . 1_545 ? OH5 Zn2 Pb3 28.24(17) 1_545 1_545 ? OH6 Zn2 Pb3 126.58(16) . 1_545 ? OH8 Zn2 Pb3 82.72(16) 1_655 1_545 ? OH7 Zn2 Pb3 113.92(16) . 1_545 ? Pb1 Zn2 Pb3 53.45(12) 1_545 1_545 ? OH9 Zn3 OH11 112.36(15) . . ? OH9 Zn3 OH10 112.59(15) . . ? OH11 Zn3 OH10 112.41(14) . . ? OH9 Zn3 W1 107.99(18) . . ? OH11 Zn3 W1 105.44(18) . . ? OH10 Zn3 W1 105.43(18) . . ? OH9 Zn3 Pb2 130.04(11) . 1_654 ? OH11 Zn3 Pb2 85.50(11) . 1_654 ? OH10 Zn3 Pb2 101.00(11) . 1_654 ? W1 Zn3 Pb2 24.46(14) . 1_654 ? OH9 Zn3 Pb2 79.40(11) . 2_666 ? OH11 Zn3 Pb2 122.49(11) . 2_666 ? OH10 Zn3 Pb2 113.26(11) . 2_666 ? W1 Zn3 Pb2 29.03(14) . 2_666 ? Pb2 Zn3 Pb2 53.13(5) 1_654 2_666 ? OH18 Zn4 OH20 97.12(14) . . ? OH18 Zn4 OH17 173.12(13) . . ? OH20 Zn4 OH17 81.27(13) . . ? OH18 Zn4 OH4 102.75(14) . 2_666 ? OH20 Zn4 OH4 102.12(13) . 2_666 ? OH17 Zn4 OH4 84.13(13) . 2_666 ? OH18 Zn4 OH2 83.71(13) . . ? OH20 Zn4 OH2 164.41(13) . . ? OH17 Zn4 OH2 96.04(13) . . ? OH4 Zn4 OH2 92.82(13) 2_666 . ? OH18 Zn4 O8 80.87(12) . 1_455 ? OH20 Zn4 O8 79.71(12) . 1_455 ? OH17 Zn4 O8 92.26(12) . 1_455 ? OH4 Zn4 O8 175.62(13) 2_666 1_455 ? OH2 Zn4 O8 85.08(12) . 1_455 ? OH18 Zn4 Zn8 145.79(10) . . ? OH20 Zn4 Zn8 97.06(9) . . ? OH17 Zn4 Zn8 41.01(9) . . ? OH4 Zn4 Zn8 43.69(10) 2_666 . ? OH2 Zn4 Zn8 90.65(9) . . ? O8 Zn4 Zn8 132.37(8) 1_455 . ? OH18 Zn4 Zn10 41.83(10) . . ? OH20 Zn4 Zn10 138.65(10) . . ? OH17 Zn4 Zn10 138.67(10) . . ? OH4 Zn4 Zn10 94.06(9) 2_666 . ? OH2 Zn4 Zn10 42.69(9) . . ? O8 Zn4 Zn10 87.01(8) 1_455 . ? Zn8 Zn4 Zn10 120.06(2) . . ? OH18 Zn4 Zn5 137.23(10) . . ? OH20 Zn4 Zn5 40.33(9) . . ? OH17 Zn4 Zn5 40.96(9) . . ? OH4 Zn4 Zn5 93.19(9) 2_666 . ? OH2 Zn4 Zn5 135.41(10) . . ? O8 Zn4 Zn5 85.66(8) 1_455 . ? Zn8 Zn4 Zn5 64.977(19) . . ? Zn10 Zn4 Zn5 172.61(3) . . ? OH15 Zn5 OH20 175.82(13) . . ? OH15 Zn5 OH17 96.61(14) . . ? OH20 Zn5 OH17 81.18(14) . . ? OH15 Zn5 OH10 100.01(13) . 1_455 ? OH20 Zn5 OH10 83.89(13) . 1_455 ? OH17 Zn5 OH10 99.56(13) . 1_455 ? OH15 Zn5 OH8 84.10(13) . . ? OH20 Zn5 OH8 97.26(13) . . ? OH17 Zn5 OH8 167.09(13) . . ? OH10 Zn5 OH8 92.98(13) 1_455 . ? OH15 Zn5 O4 81.38(13) . . ? OH20 Zn5 O4 94.75(12) . . ? OH17 Zn5 O4 81.37(12) . . ? OH10 Zn5 O4 178.20(13) 1_455 . ? OH8 Zn5 O4 86.01(12) . . ? OH15 Zn5 Zn7 42.15(10) . . ? OH20 Zn5 Zn7 139.55(10) . . ? OH17 Zn5 Zn7 138.44(10) . . ? OH10 Zn5 Zn7 94.11(9) 1_455 . ? OH8 Zn5 Zn7 42.38(9) . . ? O4 Zn5 Zn7 86.15(8) . . ? OH15 Zn5 Zn9 143.34(10) . 1_455 ? OH20 Zn5 Zn9 40.74(9) . 1_455 ? OH17 Zn5 Zn9 95.64(9) . 1_455 ? OH10 Zn5 Zn9 43.77(10) 1_455 1_455 ? OH8 Zn5 Zn9 91.30(9) . 1_455 ? O4 Zn5 Zn9 134.71(9) . 1_455 ? Zn7 Zn5 Zn9 120.42(2) . 1_455 ? OH15 Zn5 Zn4 137.24(10) . . ? OH20 Zn5 Zn4 40.35(9) . . ? OH17 Zn5 Zn4 40.85(10) . . ? OH10 Zn5 Zn4 93.17(9) 1_455 . ? OH8 Zn5 Zn4 135.91(10) . . ? O4 Zn5 Zn4 86.54(8) . . ? Zn7 Zn5 Zn4 172.62(3) . . ? Zn9 Zn5 Zn4 64.763(18) 1_455 . ? OH14 Zn6 OH16 173.62(13) . . ? OH14 Zn6 OH15 96.79(13) . . ? OH16 Zn6 OH15 81.62(13) . . ? OH14 Zn6 OH9 102.47(14) . . ? OH16 Zn6 OH9 83.91(13) . . ? OH15 Zn6 OH9 101.25(13) . . ? OH14 Zn6 OH6 83.40(13) . . ? OH16 Zn6 OH6 96.68(13) . . ? OH15 Zn6 OH6 166.29(14) . . ? OH9 Zn6 OH6 92.06(13) . . ? OH14 Zn6 O4 81.50(13) . . ? OH16 Zn6 O4 92.13(12) . . ? OH15 Zn6 O4 80.34(12) . . ? OH9 Zn6 O4 175.44(12) . . ? OH6 Zn6 O4 86.15(12) . . ? OH14 Zn6 Zn11 145.80(10) . . ? OH16 Zn6 Zn11 40.52(9) . . ? OH15 Zn6 Zn11 97.44(9) . . ? OH9 Zn6 Zn11 44.14(9) . . ? OH6 Zn6 Zn11 89.78(9) . . ? O4 Zn6 Zn11 131.58(9) . . ? OH14 Zn6 Zn9 41.76(9) . . ? OH16 Zn6 Zn9 138.90(9) . . ? OH15 Zn6 Zn9 138.30(10) . . ? OH9 Zn6 Zn9 94.18(9) . . ? OH6 Zn6 Zn9 42.25(9) . . ? O4 Zn6 Zn9 87.31(8) . . ? Zn11 Zn6 Zn9 119.81(2) . . ? OH14 Zn6 Zn7 137.54(10) . . ? OH16 Zn6 Zn7 40.45(9) . . ? OH15 Zn6 Zn7 41.18(9) . . ? OH9 Zn6 Zn7 93.79(9) . . ? OH6 Zn6 Zn7 135.42(10) . . ? O4 Zn6 Zn7 84.60(8) . . ? Zn11 Zn6 Zn7 65.446(19) . . ? Zn9 Zn6 Zn7 171.80(3) . . ? OH13 Zn7 OH16 97.03(13) 1_545 . ? OH13 Zn7 OH15 173.36(13) 1_545 . ? OH16 Zn7 OH15 81.88(13) . . ? OH13 Zn7 OH8 102.03(14) 1_545 . ? OH16 Zn7 OH8 102.53(13) . . ? OH15 Zn7 OH8 84.59(13) . . ? OH13 Zn7 OH11 83.62(13) 1_545 1_455 ? OH16 Zn7 OH11 164.84(14) . 1_455 ? OH15 Zn7 OH11 95.72(13) . 1_455 ? OH8 Zn7 OH11 92.09(13) . 1_455 ? OH13 Zn7 O12 80.58(13) 1_545 2_666 ? OH16 Zn7 O12 80.18(12) . 2_666 ? OH15 Zn7 O12 92.78(12) . 2_666 ? OH8 Zn7 O12 175.88(12) . 2_666 ? OH11 Zn7 O12 85.01(13) 1_455 2_666 ? OH13 Zn7 Zn5 144.94(10) 1_545 . ? OH16 Zn7 Zn5 97.21(9) . . ? OH15 Zn7 Zn5 41.55(9) . . ? OH8 Zn7 Zn5 43.47(9) . . ? OH11 Zn7 Zn5 90.62(9) 1_455 . ? O12 Zn7 Zn5 133.48(8) 2_666 . ? OH13 Zn7 Zn12 41.64(9) 1_545 1_455 ? OH16 Zn7 Zn12 138.38(9) . 1_455 ? OH15 Zn7 Zn12 138.39(9) . 1_455 ? OH8 Zn7 Zn12 93.31(9) . 1_455 ? OH11 Zn7 Zn12 42.74(10) 1_455 1_455 ? O12 Zn7 Zn12 86.54(8) 2_666 1_455 ? Zn5 Zn7 Zn12 119.79(2) . 1_455 ? OH13 Zn7 Zn6 137.56(10) 1_545 . ? OH16 Zn7 Zn6 40.82(9) . . ? OH15 Zn7 Zn6 41.07(9) . . ? OH8 Zn7 Zn6 94.18(9) . . ? OH11 Zn7 Zn6 135.12(10) 1_455 . ? O12 Zn7 Zn6 85.86(9) 2_666 . ? Zn5 Zn7 Zn6 65.391(18) . . ? Zn12 Zn7 Zn6 172.31(3) 1_455 . ? OH17 Zn8 OH12 174.44(13) . . ? OH17 Zn8 OH14 96.65(14) . . ? OH12 Zn8 OH14 81.58(13) . . ? OH17 Zn8 OH3 100.86(14) . . ? OH12 Zn8 OH3 84.66(13) . . ? OH14 Zn8 OH3 99.97(14) . . ? OH17 Zn8 OH4 83.84(13) . 2_666 ? OH12 Zn8 OH4 96.70(13) . 2_666 ? OH14 Zn8 OH4 167.02(13) . 2_666 ? OH3 Zn8 OH4 92.64(13) . 2_666 ? OH17 Zn8 O4 81.36(13) . . ? OH12 Zn8 O4 93.13(12) . . ? OH14 Zn8 O4 80.50(13) . . ? OH3 Zn8 O4 177.63(12) . . ? OH4 Zn8 O4 86.78(13) 2_666 . ? OH17 Zn8 Zn10 144.22(10) . 2_666 ? OH12 Zn8 Zn10 41.34(9) . 2_666 ? OH14 Zn8 Zn10 96.46(10) . 2_666 ? OH3 Zn8 Zn10 43.98(9) . 2_666 ? OH4 Zn8 Zn10 90.48(9) 2_666 2_666 ? O4 Zn8 Zn10 133.70(8) . 2_666 ? OH17 Zn8 Zn4 42.05(10) . . ? OH12 Zn8 Zn4 139.00(10) . . ? OH14 Zn8 Zn4 138.47(9) . . ? OH3 Zn8 Zn4 93.76(9) . . ? OH4 Zn8 Zn4 42.35(9) 2_666 . ? O4 Zn8 Zn4 87.36(8) . . ? Zn10 Zn8 Zn4 119.73(2) 2_666 . ? OH17 Zn8 Zn9 137.26(10) . . ? OH12 Zn8 Zn9 40.75(9) . . ? OH14 Zn8 Zn9 40.83(9) . . ? OH3 Zn8 Zn9 92.89(9) . . ? OH4 Zn8 Zn9 136.11(10) 2_666 . ? O4 Zn8 Zn9 85.96(8) . . ? Zn10 Zn8 Zn9 64.948(18) 2_666 . ? Zn4 Zn8 Zn9 173.25(3) . . ? OH20 Zn9 OH14 175.49(13) 1_655 . ? OH20 Zn9 OH12 96.89(13) 1_655 . ? OH14 Zn9 OH12 81.34(13) . . ? OH20 Zn9 OH6 100.97(14) 1_655 . ? OH14 Zn9 OH6 83.46(13) . . ? OH12 Zn9 OH6 100.72(14) . . ? OH20 Zn9 OH10 83.47(13) 1_655 . ? OH14 Zn9 OH10 97.38(13) . . ? OH12 Zn9 OH10 167.76(13) . . ? OH6 Zn9 OH10 91.19(13) . . ? OH20 Zn9 O8 82.59(13) 1_655 . ? OH14 Zn9 O8 93.02(13) . . ? OH12 Zn9 O8 81.05(13) . . ? OH6 Zn9 O8 175.73(12) . . ? OH10 Zn9 O8 86.88(12) . . ? OH20 Zn9 Zn5 41.38(10) 1_655 1_655 ? OH14 Zn9 Zn5 139.95(10) . 1_655 ? OH12 Zn9 Zn5 138.14(10) . 1_655 ? OH6 Zn9 Zn5 92.62(10) . 1_655 ? OH10 Zn9 Zn5 42.71(9) . 1_655 ? O8 Zn9 Zn5 88.54(8) . 1_655 ? OH20 Zn9 Zn6 143.52(10) 1_655 . ? OH14 Zn9 Zn6 40.98(9) . . ? OH12 Zn9 Zn6 96.53(9) . . ? OH6 Zn9 Zn6 43.09(9) . . ? OH10 Zn9 Zn6 90.22(9) . . ? O8 Zn9 Zn6 133.05(8) . . ? Zn5 Zn9 Zn6 119.20(2) 1_655 . ? OH20 Zn9 Zn8 137.14(10) 1_655 . ? OH14 Zn9 Zn8 40.93(9) . . ? OH12 Zn9 Zn8 40.41(9) . . ? OH6 Zn9 Zn8 92.91(10) . . ? OH10 Zn9 Zn8 137.00(10) . . ? O8 Zn9 Zn8 85.93(9) . . ? Zn5 Zn9 Zn8 174.46(3) 1_655 . ? Zn6 Zn9 Zn8 65.275(18) . . ? OH12 Zn10 OH18 174.10(13) 2_666 . ? OH12 Zn10 OH18 95.85(13) 2_666 2_566 ? OH18 Zn10 OH18 81.67(14) . 2_566 ? OH12 Zn10 OH2 101.89(14) 2_666 . ? OH18 Zn10 OH2 83.83(13) . . ? OH18 Zn10 OH2 99.36(13) 2_566 . ? OH12 Zn10 OH3 84.54(13) 2_666 2_666 ? OH18 Zn10 OH3 96.72(13) . 2_666 ? OH18 Zn10 OH3 167.51(13) 2_566 2_666 ? OH2 Zn10 OH3 92.75(13) . 2_666 ? OH12 Zn10 O8 81.01(13) 2_666 2_666 ? OH18 Zn10 O8 93.30(13) . 2_666 ? OH18 Zn10 O8 81.53(12) 2_566 2_666 ? OH2 Zn10 O8 176.83(12) . 2_666 ? OH3 Zn10 O8 86.21(12) 2_666 2_666 ? OH12 Zn10 Zn8 41.97(9) 2_666 2_666 ? OH18 Zn10 Zn8 139.88(10) . 2_666 ? OH18 Zn10 Zn8 137.70(10) 2_566 2_666 ? OH2 Zn10 Zn8 94.09(9) . 2_666 ? OH3 Zn10 Zn8 43.23(10) 2_666 2_666 ? O8 Zn10 Zn8 87.21(8) 2_666 2_666 ? OH12 Zn10 Zn4 144.61(10) 2_666 . ? OH18 Zn10 Zn4 41.27(9) . . ? OH18 Zn10 Zn4 96.76(9) 2_566 . ? OH2 Zn10 Zn4 43.38(9) . . ? OH3 Zn10 Zn4 89.93(9) 2_666 . ? O8 Zn10 Zn4 133.56(8) 2_666 . ? Zn8 Zn10 Zn4 119.66(2) 2_666 . ? OH12 Zn10 Zn10 136.21(10) 2_666 2_566 ? OH18 Zn10 Zn10 41.07(9) . 2_566 ? OH18 Zn10 Zn10 40.60(9) 2_566 2_566 ? OH2 Zn10 Zn10 92.14(9) . 2_566 ? OH3 Zn10 Zn10 136.49(10) 2_666 2_566 ? O8 Zn10 Zn10 86.57(9) 2_666 2_566 ? Zn8 Zn10 Zn10 173.77(3) 2_666 2_566 ? Zn4 Zn10 Zn10 65.40(2) . 2_566 ? OH16 Zn11 OH19 173.81(13) . 1_554 ? OH16 Zn11 OH19 97.31(13) . 2_656 ? OH19 Zn11 OH19 81.32(14) 1_554 2_656 ? OH16 Zn11 OH7 101.87(14) . . ? OH19 Zn11 OH7 84.33(13) 1_554 . ? OH19 Zn11 OH7 100.93(14) 2_656 . ? OH16 Zn11 OH9 83.84(13) . . ? OH19 Zn11 OH9 95.95(13) 1_554 . ? OH19 Zn11 OH9 165.35(13) 2_656 . ? OH7 Zn11 OH9 93.08(13) . . ? OH16 Zn11 O12 81.12(13) . 2_666 ? OH19 Zn11 O12 92.70(13) 1_554 2_666 ? OH19 Zn11 O12 80.38(13) 2_656 2_666 ? OH7 Zn11 O12 176.50(13) . 2_666 ? OH9 Zn11 O12 85.39(12) . 2_666 ? OH16 Zn11 Zn12 145.01(10) . . ? OH19 Zn11 Zn12 41.12(9) 1_554 . ? OH19 Zn11 Zn12 96.16(9) 2_656 . ? OH7 Zn11 Zn12 43.72(10) . . ? OH9 Zn11 Zn12 90.98(9) . . ? O12 Zn11 Zn12 133.07(9) 2_666 . ? OH16 Zn11 Zn6 41.66(10) . . ? OH19 Zn11 Zn6 138.81(10) 1_554 . ? OH19 Zn11 Zn6 138.72(10) 2_656 . ? OH7 Zn11 Zn6 93.93(10) . . ? OH9 Zn11 Zn6 42.93(9) . . ? O12 Zn11 Zn6 87.10(8) 2_666 . ? Zn12 Zn11 Zn6 120.25(2) . . ? OH16 Zn11 Zn11 137.40(10) . 2_655 ? OH19 Zn11 Zn11 40.92(9) 1_554 2_655 ? OH19 Zn11 Zn11 40.40(9) 2_656 2_655 ? OH7 Zn11 Zn11 93.48(10) . 2_655 ? OH9 Zn11 Zn11 135.16(10) . 2_655 ? O12 Zn11 Zn11 85.42(9) 2_666 2_655 ? Zn12 Zn11 Zn11 64.99(2) . 2_655 ? Zn6 Zn11 Zn11 172.45(3) . 2_655 ? OH19 Zn12 OH13 174.90(13) 1_554 1_645 ? OH19 Zn12 OH13 96.44(13) 1_554 2_665 ? OH13 Zn12 OH13 81.08(14) 1_645 2_665 ? OH19 Zn12 OH11 100.97(14) 1_554 . ? OH13 Zn12 OH11 83.88(13) 1_645 . ? OH13 Zn12 OH11 99.72(13) 2_665 . ? OH19 Zn12 OH7 84.01(14) 1_554 . ? OH13 Zn12 OH7 97.49(13) 1_645 . ? OH13 Zn12 OH7 168.10(13) 2_665 . ? OH11 Zn12 OH7 91.84(13) . . ? OH19 Zn12 O12 82.66(13) 1_554 1_544 ? OH13 Zn12 O12 92.54(13) 1_645 1_544 ? OH13 Zn12 O12 81.50(13) 2_665 1_544 ? OH11 Zn12 O12 175.97(13) . 1_544 ? OH7 Zn12 O12 86.78(13) . 1_544 ? OH19 Zn12 Zn11 41.75(10) 1_554 . ? OH13 Zn12 Zn11 140.20(10) 1_645 . ? OH13 Zn12 Zn11 138.03(9) 2_665 . ? OH11 Zn12 Zn11 93.56(10) . . ? OH7 Zn12 Zn11 42.77(9) . . ? O12 Zn12 Zn11 87.99(9) 1_544 . ? OH19 Zn12 Zn7 143.74(10) 1_554 1_655 ? OH13 Zn12 Zn7 41.30(9) 1_645 1_655 ? OH13 Zn12 Zn7 96.38(9) 2_665 1_655 ? OH11 Zn12 Zn7 43.35(10) . 1_655 ? OH7 Zn12 Zn7 90.07(9) . 1_655 ? O12 Zn12 Zn7 132.81(9) 1_544 1_655 ? Zn11 Zn12 Zn7 119.61(2) . 1_655 ? OH19 Zn12 Zn12 136.55(10) 1_554 2_755 ? OH13 Zn12 Zn12 40.81(9) 1_645 2_755 ? OH13 Zn12 Zn12 40.27(9) 2_665 2_755 ? OH11 Zn12 Zn12 92.41(10) . 2_755 ? OH7 Zn12 Zn12 137.11(10) . 2_755 ? O12 Zn12 Zn12 86.06(9) 1_544 2_755 ? Zn11 Zn12 Zn12 174.03(3) . 2_755 ? Zn7 Zn12 Zn12 65.29(2) 1_655 2_755 ? O1 S1 O2 110.6(3) . . ? O1 S1 O3 110.2(3) . . ? O2 S1 O3 110.5(2) . . ? O1 S1 O4 108.2(2) . . ? O2 S1 O4 108.8(2) . . ? O3 S1 O4 108.5(2) . . ? O1 S1 Pb1 115.73(17) . 1_545 ? O2 S1 Pb1 77.34(17) . 1_545 ? O3 S1 Pb1 34.36(17) . 1_545 ? O4 S1 Pb1 129.98(14) . 1_545 ? O1 S1 Pb3 95.3(2) . 1_445 ? O2 S1 Pb3 18.9(2) . 1_445 ? O3 S1 Pb3 107.7(2) . 1_445 ? O4 S1 Pb3 125.81(18) . 1_445 ? Pb1 S1 Pb3 73.40(11) 1_545 1_445 ? O5 S2 O6 109.8(3) 1_455 . ? O5 S2 O7 110.4(3) 1_455 . ? O6 S2 O7 111.1(3) . . ? O5 S2 O8 108.7(2) 1_455 1_455 ? O6 S2 O8 108.0(2) . 1_455 ? O7 S2 O8 108.8(2) . 1_455 ? O5 S2 Pb3 40.8(2) 1_455 1_455 ? O6 S2 Pb3 69.4(2) . 1_455 ? O7 S2 Pb3 121.7(2) . 1_455 ? O8 S2 Pb3 126.96(18) 1_455 1_455 ? O5 S2 Pb1 111.6(2) 1_455 . ? O6 S2 Pb1 24.63(18) . . ? O7 S2 Pb1 88.36(18) . . ? O8 S2 Pb1 126.61(14) 1_455 . ? Pb3 S2 Pb1 72.81(12) 1_455 . ? O9 S3 O10 110.6(3) 1_554 . ? O9 S3 O11 110.2(3) 1_554 . ? O10 S3 O11 109.6(3) . . ? O9 S3 O12 108.7(2) 1_554 1_554 ? O10 S3 O12 108.9(2) . 1_554 ? O11 S3 O12 108.8(2) . 1_554 ? O9 S3 Pb2 73.0(2) 1_554 2_666 ? O10 S3 Pb2 120.3(2) . 2_666 ? O11 S3 Pb2 37.5(2) . 2_666 ? O12 S3 Pb2 126.73(15) 1_554 2_666 ? O9 S3 Pb2 18.3(2) 1_554 1_554 ? O10 S3 Pb2 94.8(2) . 1_554 ? O11 S3 Pb2 109.1(2) . 1_554 ? O12 S3 Pb2 124.42(15) 1_554 1_554 ? Pb2 S3 Pb2 72.32(5) 2_666 1_554 ? S1 O2 Pb3 151.6(3) . 1_445 ? S1 O2 Pb1 80.96(17) . 1_545 ? Pb3 O2 Pb1 91.22(19) 1_445 1_545 ? S1 O3 Pb1 128.6(2) . 1_545 ? S1 O4 Zn5 127.3(2) . . ? S1 O4 Zn6 125.81(19) . . ? Zn5 O4 Zn6 89.06(11) . . ? S1 O4 Zn8 125.77(19) . . ? Zn5 O4 Zn8 88.29(11) . . ? Zn6 O4 Zn8 88.29(12) . . ? S2 O5 Pb3 120.7(3) 1_655 . ? S2 O6 Pb1 143.4(3) . . ? S2 O6 Pb3 89.0(2) . 1_455 ? Pb1 O6 Pb3 93.04(16) . 1_455 ? S2 O8 Zn9 127.00(19) 1_655 . ? S2 O8 Zn10 126.14(19) 1_655 2_666 ? Zn9 O8 Zn10 89.23(12) . 2_666 ? S2 O8 Zn4 125.77(19) 1_655 1_655 ? Zn9 O8 Zn4 88.03(11) . 1_655 ? Zn10 O8 Zn4 88.28(11) 2_666 1_655 ? S3 O9 Pb2 152.4(3) 1_556 . ? S3 O9 Pb2 85.7(2) 1_556 2_667 ? Pb2 O9 Pb2 91.56(13) . 2_667 ? S3 O11 Pb2 125.0(3) . 2_666 ? S3 O12 Zn12 126.0(2) 1_556 1_566 ? S3 O12 Zn11 127.4(2) 1_556 2_666 ? Zn12 O12 Zn11 88.06(11) 1_566 2_666 ? S3 O12 Zn7 126.8(2) 1_556 2_666 ? Zn12 O12 Zn7 88.45(12) 1_566 2_666 ? Zn11 O12 Zn7 87.10(11) 2_666 2_666 ? Zn1 OH1 Pb1 133.5(2) . . ? Zn1 OH1 Pb3 128.3(3) . . ? Pb1 OH1 Pb3 98.1(2) . . ? Zn1 OH1 H1 121(6) . . ? Pb1 OH1 H1 104(6) . . ? Pb3 OH1 H1 20(6) . . ? Zn1 OH2 Zn10 121.70(17) . . ? Zn1 OH2 Zn4 123.38(17) . . ? Zn10 OH2 Zn4 93.92(14) . . ? Zn1 OH2 H2 107(4) . . ? Zn10 OH2 H2 100(4) . . ? Zn4 OH2 H2 108(4) . . ? Zn1 OH3 Zn8 121.29(17) . . ? Zn1 OH3 Zn10 124.07(17) . 2_666 ? Zn8 OH3 Zn10 92.79(14) . 2_666 ? Zn1 OH3 H3 107(4) . . ? Zn8 OH3 H3 106(4) . . ? Zn10 OH3 H3 104(4) 2_666 . ? Zn1 OH4 Zn4 121.80(17) . 2_666 ? Zn1 OH4 Zn8 123.69(17) . 2_666 ? Zn4 OH4 Zn8 93.96(14) 2_666 2_666 ? Zn1 OH4 H4 98(4) . . ? Zn4 OH4 H4 116(4) 2_666 . ? Zn8 OH4 H4 103(4) 2_666 . ? Zn2 OH5 Pb1 133.7(2) 1_565 . ? Zn2 OH5 Pb3 129.2(3) 1_565 . ? Pb1 OH5 Pb3 97.0(2) . . ? Zn2 OH5 H5 120(5) 1_565 . ? Pb1 OH5 H5 98(5) . . ? Pb3 OH5 H5 32(5) . . ? Zn2 OH6 Zn9 122.75(17) . . ? Zn2 OH6 Zn6 124.80(17) . . ? Zn9 OH6 Zn6 94.66(14) . . ? Zn2 OH6 H6 102(4) . . ? Zn9 OH6 H6 109(4) . . ? Zn6 OH6 H6 102(4) . . ? Zn2 OH7 Zn11 121.48(17) . . ? Zn2 OH7 Zn12 124.51(17) . . ? Zn11 OH7 Zn12 93.51(14) . . ? Zn2 OH7 H7 102(4) . . ? Zn11 OH7 H7 101(4) . . ? Zn12 OH7 H7 112(4) . . ? Zn2 OH8 Zn7 123.15(17) 1_455 . ? Zn2 OH8 Zn5 122.49(17) 1_455 . ? Zn7 OH8 Zn5 94.15(14) . . ? Zn2 OH8 H8 104(4) 1_455 . ? Zn7 OH8 H8 103(4) . . ? Zn5 OH8 H8 108(4) . . ? Zn3 OH9 Zn6 120.21(16) . . ? Zn3 OH9 Zn11 121.46(17) . . ? Zn6 OH9 Zn11 92.93(14) . . ? Zn3 OH9 Pb2 72.59(10) . 2_666 ? Zn6 OH9 Pb2 120.22(13) . 2_666 ? Zn11 OH9 Pb2 132.35(13) . 2_666 ? Zn3 OH9 H9 104(4) . . ? Zn6 OH9 H9 111(4) . . ? Zn11 OH9 H9 107(4) . . ? Pb2 OH9 H9 32(4) 2_666 . ? Zn3 OH10 Zn5 120.08(16) . 1_655 ? Zn3 OH10 Zn9 122.36(17) . . ? Zn5 OH10 Zn9 93.52(14) 1_655 . ? Zn3 OH10 H10 107(4) . . ? Zn5 OH10 H10 105(4) 1_655 . ? Zn9 OH10 H10 107(4) . . ? Zn3 OH11 Zn12 121.05(17) . . ? Zn3 OH11 Zn7 122.50(17) . 1_655 ? Zn12 OH11 Zn7 93.91(14) . 1_655 ? Zn3 OH11 H11 107(4) . . ? Zn12 OH11 H11 105(4) . . ? Zn7 OH11 H11 105(4) 1_655 . ? Zn10 OH12 Zn8 96.69(14) 2_666 . ? Zn10 OH12 Zn9 108.23(16) 2_666 . ? Zn8 OH12 Zn9 98.84(14) . . ? Zn10 OH12 H12 109(4) 2_666 . ? Zn8 OH12 H12 121(4) . . ? Zn9 OH12 H12 120(4) . . ? Zn7 OH13 Zn12 97.06(14) 1_565 1_465 ? Zn7 OH13 Zn12 108.86(16) 1_565 2_665 ? Zn12 OH13 Zn12 98.92(14) 1_465 2_665 ? Zn7 OH13 H13 114(4) 1_565 . ? Zn12 OH13 H13 121(4) 1_465 . ? Zn12 OH13 H13 115(4) 2_665 . ? Zn6 OH14 Zn9 97.25(14) . . ? Zn6 OH14 Zn8 109.23(16) . . ? Zn9 OH14 Zn8 98.24(14) . . ? Zn6 OH14 H14 110(4) . . ? Zn9 OH14 H14 126(5) . . ? Zn8 OH14 H14 114(4) . . ? Zn5 OH15 Zn6 108.61(15) . . ? Zn5 OH15 Zn7 96.31(14) . . ? Zn6 OH15 Zn7 97.75(14) . . ? Zn5 OH15 H15 121(4) . . ? Zn6 OH15 H15 110(4) . . ? Zn7 OH15 H15 120(4) . . ? Zn11 OH16 Zn7 110.97(16) . . ? Zn11 OH16 Zn6 97.82(15) . . ? Zn7 OH16 Zn6 98.73(14) . . ? Zn11 OH16 H16 113(4) . . ? Zn7 OH16 H16 112(4) . . ? Zn6 OH16 H16 122(4) . . ? Zn8 OH17 Zn4 96.95(14) . . ? Zn8 OH17 Zn5 108.56(16) . . ? Zn4 OH17 Zn5 98.19(15) . . ? Zn8 OH17 H17 118(4) . . ? Zn4 OH17 H17 119(4) . . ? Zn5 OH17 H17 113(4) . . ? Zn4 OH18 Zn10 96.90(14) . . ? Zn4 OH18 Zn10 108.88(16) . 2_566 ? Zn10 OH18 Zn10 98.33(14) . 2_566 ? Zn4 OH18 H18 118(4) . . ? Zn10 OH18 H18 120(4) . . ? Zn10 OH18 H18 112(4) 2_566 . ? Zn12 OH19 Zn11 97.13(14) 1_556 1_556 ? Zn12 OH19 Zn11 108.34(16) 1_556 2_656 ? Zn11 OH19 Zn11 98.68(14) 1_556 2_656 ? Zn12 OH19 H19 109(4) 1_556 . ? Zn11 OH19 H19 118(4) 1_556 . ? Zn11 OH19 H19 122(4) 2_656 . ? Zn9 OH20 Zn5 97.88(14) 1_455 . ? Zn9 OH20 Zn4 109.09(15) 1_455 . ? Zn5 OH20 Zn4 99.32(14) . . ? Zn9 OH20 H20 113(4) 1_455 . ? Zn5 OH20 H20 120(4) . . ? Zn4 OH20 H20 116(4) . . ? Zn3 W1 Pb2 134.2(2) . 1_654 ? Zn3 W1 Pb2 127.3(2) . 2_666 ? Pb2 W1 Pb2 97.61(16) 1_654 2_666 ? Pb1 W2 Pb3 91.0(2) . 1_455 ? Pb3 W4 Pb1 113.9(4) . 1_655 ? Pb2 W5 Pb2 62.0(3) . 2_567 ? Pb2 W6 Pb2 113.7(4) 1_554 2_666 ? Pb2 W8 Pb2 55.94(13) 1_554 2_566 ? W9B W9A Pb1 118.2(11) . . ? W9B W9A Pb3 85.4(10) . . ? Pb1 W9A Pb3 62.59(18) . . ? W9A W9B Pb1 43.4(8) . . ? W9A W9B Pb3 75.9(10) . . ? Pb1 W9B Pb3 56.3(3) . . ? W10B W10A Pb3 133.8(10) . 1_545 ? W10B W10A Pb1 159.6(10) . 1_545 ? Pb3 W10A Pb1 56.5(3) 1_545 1_545 ? W10A W10B Pb3 146.5(10) . 2_766 ? Pb1 W12 Pb3 66.8(3) . . ? 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 OH2 H2 O6 0.83(3) 2.01(3) 2.811(5) 163(6) . OH3 H3 O5 0.82(3) 2.03(3) 2.838(6) 169(6) . OH4 H4 O1 0.80(3) 2.01(3) 2.784(5) 164(6) 2_666 OH5 H5 W7 0.80(3) 2.19(4) 2.923(7) 152(7) . OH6 H6 O3 0.81(3) 1.93(3) 2.727(5) 171(6) . OH7 H7 O10 0.83(3) 2.01(4) 2.771(6) 153(6) 1_545 OH8 H8 O2 0.82(3) 1.98(3) 2.768(5) 161(6) . OH9 H9 O9 0.80(3) 2.03(3) 2.805(6) 163(6) 2_666 OH10 H10 O7 0.81(3) 2.04(3) 2.826(5) 163(6) 1_655 OH11 H11 O11 0.81(3) 2.00(3) 2.791(6) 168(6) 2_765 OH12 H12 W3 0.79(3) 2.20(3) 2.985(9) 177(6) 2_666 OH14 H14 W11 0.78(3) 2.35(4) 3.057(15) 152(6) 2_666 OH16 H16 W2 0.81(3) 2.03(3) 2.832(7) 166(6) 1_545 OH17 H17 W9B 0.80(3) 2.18(4) 2.94(3) 161(6) . OH19 H19 W8 0.80(3) 2.15(3) 2.950(9) 176(6) 2_666 OH20 H20 W10A 0.80(3) 2.18(3) 2.975(14) 169(6) 1_455 OH20 H20 W10B 0.80(3) 2.04(4) 2.808(12) 160(6) 1_455 _refine_diff_density_max 2.553 _refine_diff_density_min -2.946 _refine_diff_density_rms 0.262 _shelx_res_file ; TITL plumbogordaite redmond7.res created by SHELXL-2016/6 at 17:21:01 on 03-Dec-2021 CELL 0.71075 8.35298 13.27690 18.27440 92.42740 90.41890 108.21400 ZERR 2 0.00019 0.00074 0.00128 0.00770 0.00640 0.00420 LATT 1 SFAC H O PB S ZN UNIT 40 85.79 2.16 6 24 L.S. 20 omit -6 6 18 omit -5 1 21 omit -1 16 4 CONN 15 3.0 PB1 CONN 15 3.0 PB2 CONN 15 3.0 PB3 FMAP 2 PLAN 20 HTAB BOND $H HTAB OH2 O6 EQIV $3 x+1, y, z HTAB OH3 O5 EQIV $7 -x+1, -y+1, -z+1 HTAB OH4 O1_$7 EQIV $1 x, y-1, z HTAB OH5 W7 HTAB OH6 O3 HTAB OH7 O10_$1 HTAB OH8 O2 EQIV $21 -x+1, -y+1, -z HTAB OH9 O9_$7 HTAB OH10 O7_$3 EQIV $24 -x+2, -y+1, -z HTAB OH11 O11_$24 HTAB OH12 W3_$7 HTAB OH14 W11_$7 HTAB OH16 W2_$1 EQIV $11 x-1, y, z HTAB OH17 W9B HTAB OH19 W8_$7 HTAB OH20 W10A_$11 HTAB OH20 W10B_$11 DFIX 0.82 0.03 OH1 H1 OH2 H2 OH3 H3 OH4 H4 OH5 H5 OH6 H6 OH7 H7 OH8 H8 DFIX 0.82 0.03 OH9 H9 OH10 H10 OH11 H11 OH12 H12 OH13 H13 OH14 H14 DFIX 0.82 0.03 OH15 H15 OH16 H16 OH17 H17 OH18 H18 OH19 H19 OH20 H20 ACTA SIZE 0.120 0.090 0.060 WGHT 0.047900 4.692400 FVAR 0.11699 0.92669 0.12833 0.02868 0.92568 0.89171 0.67791 FVAR 0.60023 0.75301 0.48018 PB1 3 0.462610 0.844516 0.342221 21.00000 0.03000 0.03744 = 0.04802 0.02356 0.00702 0.01043 PB2 3 0.208042 0.494114 0.996292 31.00000 0.03434 0.04236 = 0.05657 0.03297 0.00562 0.00999 PB3 3 0.872145 0.824465 0.328118 41.00000 0.03365 ZN1 5 0.555452 0.618630 0.445173 11.00000 0.01425 0.01822 = 0.01645 -0.00126 -0.00103 0.00557 ZN2 5 0.774685 0.050992 0.222247 11.00000 0.01433 0.01777 = 0.01646 -0.00129 -0.00049 0.00545 ZN3 5 0.891393 0.281333 0.113786 11.00000 0.01463 0.02004 = 0.01731 -0.00315 -0.00086 0.00526 ZN4 5 0.178069 0.399350 0.407913 11.00000 0.01286 0.02194 = 0.01678 -0.00757 -0.00129 0.00597 ZN5 5 0.155657 0.265773 0.260259 11.00000 0.01243 0.02207 = 0.01648 -0.00740 -0.00136 0.00580 ZN6 5 0.508621 0.217771 0.206593 11.00000 0.01315 0.02179 = 0.01834 -0.00777 -0.00443 0.00689 ZN7 5 0.159869 0.119271 0.125783 11.00000 0.01313 0.02173 = 0.01817 -0.00792 -0.00434 0.00679 ZN8 5 0.510644 0.366506 0.359819 11.00000 0.01251 0.02544 = 0.01625 -0.00588 -0.00287 0.00832 ZN9 5 0.825182 0.304985 0.306644 11.00000 0.01212 0.02375 = 0.01633 -0.00569 -0.00280 0.00779 ZN10 5 0.173768 0.545960 0.542468 11.00000 0.01292 0.02117 = 0.01784 -0.00750 -0.00411 0.00643 ZN11 5 0.512006 0.068269 0.073410 11.00000 0.01285 0.02337 = 0.01632 -0.00765 -0.00106 0.00590 ZN12 5 0.842249 0.030851 0.027114 11.00000 0.01249 0.02632 = 0.01685 -0.00714 -0.00320 0.00851 S1 4 0.302603 0.091937 0.359949 11.00000 0.01955 0.01759 = 0.01796 0.00129 -0.00092 0.00540 S2 4 0.035271 0.575114 0.304430 11.00000 0.02056 0.01790 = 0.01918 0.00176 -0.00007 0.00545 S3 4 0.635875 0.759951 0.032485 11.00000 0.02211 0.02003 = 0.02073 0.00134 0.00007 0.00590 O1 2 0.259881 0.120207 0.434027 11.00000 0.05645 0.03244 = 0.02305 0.00196 0.00939 0.01665 O2 2 0.158709 0.010783 0.324288 11.00000 0.03061 0.02204 = 0.04405 0.00270 -0.01397 -0.00330 O3 2 0.450185 0.054252 0.362763 11.00000 0.02842 0.03052 = 0.05318 0.01793 0.00714 0.01783 O4 2 0.346112 0.190105 0.316059 11.00000 0.01933 0.01920 = 0.01965 0.00229 -0.00215 0.00533 O5 2 0.884549 0.604722 0.288098 11.00000 0.03227 0.05468 = 0.05372 0.02555 0.00160 0.01932 O6 2 0.155157 0.660313 0.349022 11.00000 0.04179 0.02039 = 0.04005 0.00098 -0.01260 -0.00393 O7 2 0.111849 0.551896 0.236359 11.00000 0.05242 0.03190 = 0.02722 0.00221 0.01929 0.00759 O8 2 0.984932 0.477238 0.348214 11.00000 0.01778 0.01680 = 0.01989 0.00162 -0.00011 0.00394 O9 2 0.498103 0.676555 0.995758 11.00000 0.06116 0.02640 = 0.05708 0.00539 -0.03181 -0.00696 O10 2 0.585294 0.788660 0.104797 11.00000 0.09340 0.03144 = 0.03270 0.00385 0.03157 0.00978 O11 2 0.784085 0.724583 0.040089 11.00000 0.04154 0.06852 = 0.07550 0.04500 0.01636 0.03362 O12 2 0.680389 0.855902 0.987031 11.00000 0.02207 0.01862 = 0.02143 0.00269 0.00011 0.00519 OH1 2 0.613029 0.741881 0.386194 11.00000 0.03088 0.03368 = 0.05230 0.02407 0.00684 0.01270 H1 1 0.706661 0.776294 0.381470 11.00000 -1.50000 OH2 2 0.308692 0.557184 0.445528 11.00000 0.01446 0.01687 = 0.01830 0.00016 -0.00263 0.00504 H2 1 0.269603 0.597863 0.423577 11.00000 -1.50000 OH3 2 0.658599 0.516760 0.400816 11.00000 0.01563 0.02051 = 0.01782 -0.00276 -0.00078 0.00671 H3 1 0.714422 0.546087 0.366402 11.00000 -1.50000 OH4 2 0.643490 0.659722 0.546291 11.00000 0.01601 0.01806 = 0.01901 -0.00269 -0.00191 0.00591 H4 1 0.670360 0.722737 0.543131 11.00000 -1.50000 OH5 2 0.709716 0.932347 0.286301 11.00000 0.03459 0.02621 = 0.04351 0.01561 0.01232 0.01232 H5 1 0.742729 0.882758 0.278755 11.00000 -1.50000 OH6 2 0.677860 0.157423 0.263218 11.00000 0.01558 0.01993 = 0.01701 -0.00147 -0.00199 0.00598 H6 1 0.619141 0.125372 0.294913 11.00000 -1.50000 OH7 2 0.689025 0.008169 0.121205 11.00000 0.01372 0.02058 = 0.01988 -0.00319 -0.00035 0.00376 H7 1 0.632829 -0.054804 0.125328 11.00000 -1.50000 OH8 2 0.022281 0.108938 0.221053 11.00000 0.01258 0.01859 = 0.01805 -0.00103 -0.00172 0.00397 H8 1 0.055010 0.068023 0.244903 11.00000 -1.50000 OH9 2 0.646033 0.228798 0.109792 11.00000 0.01543 0.01818 = 0.01688 0.00045 -0.00288 0.00408 H9 1 0.621110 0.266901 0.082537 11.00000 -1.50000 OH10 2 0.981465 0.329230 0.212792 11.00000 0.01306 0.01855 = 0.01914 -0.00568 -0.00106 0.00329 H10 1 1.030082 0.392199 0.212087 11.00000 -1.50000 OH11 2 0.992370 0.180415 0.068211 11.00000 0.01639 0.02139 = 0.01703 -0.00132 -0.00125 0.00518 H11 1 1.044544 0.208683 0.033674 11.00000 -1.50000 OH12 2 0.699135 0.315683 0.402368 11.00000 0.01569 0.01526 = 0.01554 -0.00320 -0.00050 0.00528 H12 1 0.679080 0.269695 0.429920 11.00000 -1.50000 OH13 2 0.032061 0.980505 0.069407 11.00000 0.01627 0.01648 = 0.01427 -0.00409 -0.00140 0.00615 H13 1 0.010739 0.929769 0.093147 11.00000 -1.50000 OH14 2 0.635160 0.355584 0.263417 11.00000 0.01641 0.01641 = 0.01604 -0.00174 -0.00160 0.00674 H14 1 0.646730 0.403295 0.238434 11.00000 -1.50000 OH15 2 0.306651 0.264506 0.172332 11.00000 0.01268 0.01909 = 0.01805 -0.00080 0.00037 0.00738 H15 1 0.340867 0.317105 0.146362 11.00000 -1.50000 OH16 2 0.362085 0.074512 0.158608 11.00000 0.01517 0.01739 = 0.01540 -0.00393 -0.00012 0.00700 H16 1 0.333214 0.020095 0.180937 11.00000 -1.50000 OH17 2 0.314700 0.402250 0.313351 11.00000 0.01356 0.01812 = 0.01857 -0.00157 -0.00228 0.00468 H17 1 0.335792 0.453271 0.289070 11.00000 -1.50000 OH18 2 0.024795 0.403641 0.493970 11.00000 0.01211 0.01803 = 0.01920 -0.00161 0.00011 0.00472 H18 1 -0.008895 0.349797 0.518446 11.00000 -1.50000 OH19 2 0.648146 0.068239 0.979842 11.00000 0.01190 0.01947 = 0.01668 -0.00507 -0.00313 0.00308 H19 1 0.684702 0.123232 0.959877 11.00000 -1.50000 OH20 2 0.018694 0.266717 0.353257 11.00000 0.01179 0.01786 = 0.01682 -0.00233 -0.00185 0.00543 H20 1 -0.012497 0.214305 0.376525 11.00000 -1.50000 W1 2 0.965934 0.409977 0.054363 11.00000 0.05356 0.03637 = 0.04913 0.02251 0.00669 0.00928 W2 2 0.257834 0.867411 0.212183 11.00000 0.09458 0.06356 = 0.09392 0.02660 0.02438 0.02755 W3 2 0.386895 0.855011 0.489911 11.00000 0.30280 0.06847 = 0.07627 -0.01766 -0.08023 0.07855 W4 2 0.987639 0.819337 0.395175 -41.00000 0.07410 0.05484 = 0.10633 -0.01506 0.00360 0.01830 W5 2 0.142117 0.438615 0.881859 11.00000 0.29293 0.10456 = 0.09363 -0.02995 -0.07410 0.12412 W6 2 0.318032 0.478486 0.059771 -31.00000 0.09025 0.06142 = 0.17787 -0.02886 0.05673 -0.00374 W7 2 0.879646 0.794618 0.214097 51.00000 0.07619 0.05565 = 0.08086 -0.01335 -0.01790 0.03295 W8 2 0.202275 0.726601 0.088106 61.00000 0.08666 0.09935 = 0.08027 -0.00555 0.00505 0.00962 W9A 2 0.447315 0.695178 0.231453 71.00000 0.04686 0.05085 = 0.04781 0.00664 0.01213 0.00496 W9B 2 0.467104 0.608420 0.248000 -71.00000 0.06141 0.08672 = 0.09136 -0.00646 -0.00459 0.02137 W10A 2 0.869475 0.059101 0.421046 81.00000 0.08007 0.09358 = 0.07604 -0.00908 0.00132 0.03962 W10B 2 0.958834 0.116340 0.461682 -81.00000 0.05097 0.04949 = 0.04843 0.01357 0.01050 0.01474 W11 2 0.457821 0.482798 0.828335 91.00000 0.29516 0.14534 = 0.27980 0.13282 0.12427 0.12488 W12 2 0.663298 0.962454 0.447524 101.00000 0.05702 0.06572 = 0.08003 0.04076 -0.00744 0.01930 HKLF 4 REM plumbogordaite REM R1 = 0.0372 for 6880 Fo > 4sig(Fo) and 0.0518 for all 8748 data REM 641 parameters refined using 20 restraints END WGHT 0.0480 4.6622 REM Instructions for potential hydrogen bonds HTAB OH2 S2 HTAB OH2 O6 HTAB OH3 S2_$3 HTAB OH3 O5 HTAB OH4 S1_$7 HTAB OH4 O1_$7 HTAB OH6 S1 HTAB OH6 O3 HTAB OH7 S3_$1 HTAB OH7 O10_$1 HTAB OH8 S1 HTAB OH8 O2 HTAB OH9 S3_$21 HTAB OH9 O9_$7 HTAB OH10 S2_$3 HTAB OH10 O7_$3 HTAB OH11 S3_$24 HTAB OH11 O11_$24 HTAB OH12 W3_$7 HTAB OH14 W11_$7 HTAB OH16 W2_$1 HTAB OH17 W9B HTAB OH19 W8_$7 HTAB OH20 W10A_$11 HTAB OH20 W10B_$11 REM Highest difference peak 2.553, deepest hole -2.946, 1-sigma level 0.262 Q1 1 0.4843 0.8760 0.3716 11.00000 0.05 2.55 Q2 1 0.1757 0.4590 0.9601 11.00000 0.05 2.20 Q3 1 0.8482 0.7870 0.3029 11.00000 0.05 2.10 Q4 1 0.6087 0.9154 0.3998 11.00000 0.05 1.92 Q5 1 0.5382 0.2759 0.1896 11.00000 0.05 1.35 Q6 1 0.2019 0.6021 0.5189 11.00000 0.05 1.32 Q7 1 0.5298 0.5586 0.4731 11.00000 0.05 1.32 Q8 1 0.5376 0.4181 0.3369 11.00000 0.05 1.29 Q9 1 0.2175 0.6501 0.1062 11.00000 0.05 1.26 Q10 1 0.8680 0.0849 -0.0008 11.00000 0.05 1.26 Q11 1 0.1401 0.3408 0.4292 11.00000 0.05 1.26 Q12 1 0.8050 0.2521 0.3276 11.00000 0.05 1.26 Q13 1 0.4492 0.8001 0.3540 11.00000 0.05 1.24 Q14 1 0.4603 0.8441 0.3225 11.00000 0.05 1.20 Q15 1 0.1300 0.0695 0.1456 11.00000 0.05 1.20 Q16 1 0.1948 0.3191 0.2393 11.00000 0.05 1.19 Q17 1 0.0464 0.4205 0.9297 11.00000 0.05 1.18 Q18 1 0.1179 0.2072 0.2861 11.00000 0.05 1.15 Q19 1 0.8068 0.1034 0.1959 11.00000 0.05 1.14 Q20 1 0.4780 0.0223 0.0965 11.00000 0.05 1.13 ; _shelx_res_checksum 78055 _shelx_hkl_file ; 0 2 0 14.77 0.90 0 2 0 16.69 0.71 0 -2 0 14.22 0.65 0 2 0 17.27 0.46 0 -2 0 13.76 0.59 0 0 -3 872.38 16.56 0 0 3 862.43 16.63 0 0 3 967.02 18.63 0 0 3 787.43 17.01 0 0 -3 901.31 17.45 0 0 -3 798.14 17.14 1 0 -2 102.16 2.07 -1 0 2 106.51 2.32 -1 0 2 100.74 2.02 1 0 -2 105.61 1.89 1 0 -2 93.13 1.40 -1 0 2 99.34 1.73 0 -2 1 44.34 1.83 0 -2 1 48.39 0.78 0 2 -1 46.53 1.39 0 2 -1 52.01 0.86 0 2 -1 48.75 1.19 0 -2 1 48.42 1.19 1 -1 2 50.47 0.99 -1 1 -2 50.78 1.12 -1 1 -2 53.56 1.15 1 -1 2 50.68 1.13 1 -1 2 51.12 1.10 -1 1 -2 49.79 1.00 1 -1 -2 164.67 2.74 1 -1 -2 161.71 2.90 -1 1 2 161.16 3.28 -1 1 2 165.77 2.70 -1 -1 0 341.29 6.31 1 1 0 342.84 6.19 1 1 0 349.82 6.60 1 1 0 348.50 6.35 -1 -1 0 345.27 6.12 -1 -1 0 334.36 6.11 1 0 2 71.10 1.56 1 0 2 70.92 1.39 1 0 2 72.42 1.26 -1 0 -2 70.50 1.80 -1 0 -2 68.18 1.00 -1 0 -2 74.05 2.05 1 -2 0 189.72 3.39 -1 2 0 188.74 2.58 1 -2 0 187.34 2.99 1 -2 0 198.38 2.89 -1 2 0 191.70 3.04 -1 2 0 200.22 3.52 0 -2 -1 23.96 0.67 0 2 1 27.94 0.75 0 -2 -1 24.73 0.72 0 2 1 27.66 0.55 0 2 1 29.97 0.75 0 -2 -1 26.48 0.73 1 1 -1 196.85 3.65 1 1 -1 192.34 3.45 -1 -1 1 195.89 3.60 -1 -1 1 201.21 3.56 1 1 -1 193.59 3.53 -1 -1 1 196.92 3.65 -1 2 -1 133.96 2.50 1 -2 1 123.57 2.18 -1 2 -1 129.88 1.86 -1 2 -1 128.74 2.25 1 -2 1 121.69 2.33 1 -2 1 127.25 1.85 -1 2 1 168.11 2.63 1 -2 -1 174.44 2.89 1 -2 -1 179.67 3.11 1 -2 -1 172.75 2.49 -1 2 1 181.50 3.13 -1 2 1 172.71 2.81 0 -1 3 13.45 0.66 0 -1 3 14.07 0.57 0 1 -3 12.84 0.59 0 -1 3 12.75 0.69 0 1 -3 16.07 0.73 0 1 -3 13.71 1.02 -1 -1 -1 81.61 1.64 1 1 1 78.98 1.64 -1 -1 -1 78.67 1.67 -1 -1 -1 81.55 1.67 1 1 1 78.46 1.70 1 1 1 80.59 1.35 0 1 3 69.35 0.77 0 -1 -3 68.06 1.51 0 1 3 72.17 1.21 0 1 3 71.02 1.97 0 -1 -3 68.80 1.11 0 1 3 68.39 0.75 0 -2 2 4046.85 137.11 0 -2 2 4492.67 143.26 0 2 -2 4390.54 144.45 0 2 -2 4024.06 135.96 0 -2 2 4209.96 138.79 0 2 -2 4705.93 150.95 0 2 2 64.37 1.07 0 2 2 70.93 1.36 0 -2 -2 71.06 1.36 0 2 2 72.35 1.61 0 -2 -2 66.42 1.25 0 -2 -2 68.82 1.11 -1 -1 2 122.60 2.31 -1 -1 2 120.34 2.50 1 1 -2 117.40 2.46 1 1 -2 115.99 2.19 1 1 -2 122.61 2.51 -1 -1 2 121.11 3.16 1 -2 2 186.85 3.60 1 -2 2 191.13 4.09 1 -2 2 194.14 3.24 -1 2 -2 207.77 3.79 -1 2 -2 193.07 3.18 1 -2 -2 143.23 2.49 -1 2 2 129.66 2.26 -1 2 2 148.97 2.90 -1 2 2 138.42 1.77 1 -2 -2 144.96 2.53 1 -2 -2 137.44 1.78 -1 -1 -2 158.15 3.55 1 1 2 150.81 2.20 1 1 2 154.56 3.08 1 1 2 155.90 2.96 -1 -1 -2 157.51 3.12 -1 -1 -2 157.70 2.57 -1 0 3 154.08 2.43 -1 0 3 161.54 3.42 -1 0 3 167.63 3.10 1 0 -3 152.15 3.26 1 0 -3 151.68 2.40 1 0 -3 166.88 3.07 1 -1 3 60.05 1.37 -1 1 -3 58.52 1.17 -1 1 -3 62.59 1.44 -1 1 -3 65.14 1.51 1 -1 3 60.87 1.94 1 -1 3 60.75 1.18 -1 1 3 149.39 2.96 1 -1 -3 160.91 3.83 -1 1 3 156.28 1.91 -1 1 3 161.13 2.73 -1 0 -3 154.30 2.88 1 0 3 151.49 2.86 1 0 3 155.45 2.38 1 0 3 152.28 3.16 -1 0 -3 146.93 2.29 -1 0 -3 155.03 3.14 0 0 4 68.48 2.35 0 0 -4 63.04 1.11 0 0 -4 69.10 1.78 0 0 -4 63.04 1.60 0 0 4 66.06 1.28 0 0 4 59.78 1.34 0 2 -3 12.34 0.99 0 -2 3 15.66 1.57 0 -2 3 15.50 0.81 0 -2 3 18.89 0.76 0 2 -3 16.73 0.87 0 -1 4 102.56 2.00 0 -1 4 85.93 2.04 0 1 -4 94.30 2.39 0 -1 4 96.69 2.26 0 1 -4 102.24 2.44 0 1 -4 84.96 1.89 -1 -1 3 101.99 2.39 -1 -1 3 100.18 2.34 1 1 -3 89.82 1.89 -1 -1 3 96.33 2.04 1 1 -3 99.15 2.41 1 1 -3 101.08 2.29 1 2 0 74.83 2.27 1 2 0 79.98 1.78 -1 -2 0 81.76 1.92 1 2 0 78.36 1.90 -1 -2 0 78.11 1.72 -1 -2 0 81.94 1.97 -1 3 0 132.77 1.47 -1 3 0 138.03 2.92 1 -3 0 134.98 2.54 1 -3 0 133.59 2.80 -1 3 0 125.39 2.38 -1 2 -3 65.46 1.69 -1 2 -3 68.81 1.72 1 -2 3 69.04 1.67 1 -2 3 68.28 1.53 1 -2 3 66.96 1.64 -1 2 -3 71.32 1.95 0 2 3 1.61 0.39 0 2 3 1.57 0.23 0 -2 -3 1.16 0.57 0 -2 -3 0.72 0.47 0 -2 -3 1.93 0.50 0 -2 -3 1.09 0.15 1 2 -1 3.47 0.53 -1 -2 1 1.37 0.56 1 2 -1 2.02 0.50 1 2 -1 2.63 0.54 -1 -2 1 2.04 0.54 -1 -2 1 0.82 0.45 -1 3 -1 19.96 1.31 1 -3 1 22.93 0.99 -1 3 -1 21.72 0.34 1 -3 1 20.68 0.45 1 -3 1 18.66 0.83 -1 3 -1 22.51 1.04 0 1 4 4.37 0.56 0 -1 -4 4.67 0.62 0 1 4 4.51 0.26 0 1 4 4.53 0.15 0 1 4 4.73 0.60 0 -1 -4 4.46 0.36 0 3 0 6.14 0.30 0 3 0 7.15 0.66 0 -3 0 4.22 0.64 0 -3 0 7.01 0.29 0 3 0 4.61 0.74 1 -2 -3 309.91 5.49 -1 2 3 305.91 5.32 1 -2 -3 315.04 4.40 -1 2 3 283.38 5.59 -1 2 3 317.03 6.03 -2 1 0 36.74 1.31 2 -1 0 36.70 1.27 2 -1 0 34.79 1.27 2 -1 0 32.52 1.09 -2 1 0 31.43 1.07 1 1 3 770.17 16.81 -1 -1 -3 757.64 16.42 -1 -1 -3 918.77 16.18 -1 -1 -3 739.80 16.67 1 1 3 760.19 17.18 -1 -1 -3 956.78 17.25 -1 3 1 89.84 1.65 1 -3 -1 96.57 2.07 -1 3 1 91.96 1.38 -1 3 1 100.56 1.47 -1 3 1 103.16 2.17 1 2 1 135.70 2.56 1 2 1 155.93 3.10 1 2 1 150.63 3.11 -1 -2 -1 147.47 2.91 -1 -2 -1 154.58 3.21 -1 -2 -1 145.61 2.89 0 -3 1 11.66 1.00 0 -3 1 14.24 0.41 0 3 -1 12.55 0.87 0 3 -1 14.18 0.44 0 3 -1 12.97 1.01 0 -3 1 14.24 0.89 -2 1 1 0.97 0.46 -2 1 1 0.56 0.40 -2 1 1 1.02 0.67 2 -1 -1 0.79 0.29 2 -1 -1 0.83 0.47 2 -1 -1 0.72 0.72 -2 1 -1 149.06 2.94 -2 1 -1 150.36 2.91 2 -1 1 148.65 2.94 -2 1 -1 151.83 3.90 2 -1 1 147.78 3.18 2 -1 1 148.94 2.87 0 -3 -1 57.63 1.51 0 3 1 57.49 1.51 0 3 1 58.94 1.05 0 3 1 58.34 1.48 0 -3 -1 53.79 0.99 0 -3 -1 53.04 1.42 -1 0 4 140.75 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4 1.89 1.02 -5 2 4 0.11 0.53 -5 2 4 0.14 0.45 -5 2 4 -0.71 1.00 -5 2 4 0.18 0.92 5 -2 -4 0.34 1.08 -1 8 -4 115.35 5.34 1 -8 4 95.34 6.16 1 -8 4 85.05 4.51 1 -8 4 81.93 2.45 1 -8 4 100.46 2.20 -1 8 -4 106.37 4.36 4 3 -3 70.50 3.92 4 3 -3 67.70 3.14 4 3 -3 63.99 3.22 -4 -3 3 79.69 5.75 -4 -3 3 70.49 5.02 -2 7 6 651.58 15.51 2 -7 -6 647.91 16.28 -2 7 6 745.53 18.41 -2 7 6 585.68 15.38 2 -7 -6 624.44 15.67 -2 7 6 705.76 17.61 5 0 -2 18.21 2.32 -5 0 2 18.79 1.55 -5 0 2 15.83 1.97 -5 0 2 19.96 2.15 -5 0 2 17.53 1.66 0 3 -11 4.82 1.38 0 -3 11 5.12 2.26 0 -3 11 7.38 2.46 0 -3 11 5.29 1.71 0 3 -11 5.29 1.26 0 -3 11 6.76 1.30 -1 3 -11 4.20 1.21 -1 3 -11 5.98 2.10 -1 3 -11 6.63 1.71 1 -3 11 2.89 1.65 1 -3 11 4.55 1.36 1 -3 11 5.10 1.83 -3 -4 -5 273.15 8.30 -3 -4 -5 283.02 6.87 3 4 5 300.91 9.18 -3 -4 -5 276.00 8.52 -3 -4 -5 274.89 8.69 -1 -3 -10 25.21 1.67 -1 -3 -10 25.56 2.37 1 3 10 30.87 2.80 1 3 10 23.89 2.47 5 -3 -4 2107.02 71.30 -5 3 4 2252.95 70.77 5 -3 -4 2299.05 73.20 -5 3 4 2225.60 61.68 -5 3 4 2230.62 63.39 -5 3 4 2198.25 72.14 -2 -5 -6 295.10 8.61 -2 -5 -6 315.14 8.80 -2 -5 -6 318.25 11.47 2 5 6 336.96 9.59 2 5 6 295.87 6.69 -2 -5 -6 274.62 6.39 -3 5 8 22.67 1.97 3 -5 -8 23.83 1.68 -3 5 8 24.97 1.93 -3 5 8 24.59 1.55 1 6 -7 26.94 2.44 -1 -6 7 33.95 4.84 -1 -6 7 25.67 2.53 -1 -6 7 26.96 2.03 1 6 -7 25.48 2.74 1 6 -7 27.01 2.04 0 8 -2 271.48 8.53 0 -8 2 274.90 5.73 0 8 -2 273.47 5.80 0 8 -2 272.80 11.79 0 -8 2 241.57 8.53 0 -8 2 270.31 8.76 5 -5 2 -0.01 0.84 -5 5 -2 0.90 1.04 -5 5 -2 1.02 0.78 5 -5 2 -0.24 0.78 5 -5 2 0.50 1.06 -5 5 -2 1.47 0.83 -5 3 -4 28.11 2.21 -5 3 -4 21.38 1.94 -5 3 -4 21.61 2.90 5 -3 4 23.43 2.99 5 -3 4 26.97 2.25 5 -3 4 26.67 3.06 -4 7 -3 81.13 3.95 -4 7 -3 79.93 2.22 4 -7 3 69.39 3.63 -4 7 -3 83.69 3.23 4 -7 3 76.34 2.24 4 -7 3 73.31 3.10 0 8 1 8.50 1.74 0 8 1 9.36 0.66 0 -8 -1 10.54 1.70 0 -8 -1 7.57 1.61 0 -8 -1 5.98 0.97 0 8 1 10.46 2.49 4 0 7 3301.20 113.72 4 0 7 3478.83 110.99 4 0 7 3192.09 117.57 -4 0 -7 3133.44 110.43 -4 0 -7 3346.39 106.65 -4 0 -7 3140.24 107.01 1 -7 7 100.66 4.92 -1 7 -7 117.75 4.89 1 -7 7 110.46 3.38 1 -7 7 96.77 3.05 -1 7 -7 122.18 7.54 1 -7 7 103.18 4.47 -5 2 -4 310.62 9.53 -5 2 -4 320.93 8.89 -5 2 -4 302.79 8.22 5 -2 4 311.33 8.55 5 -2 4 288.43 9.43 5 -2 4 312.07 9.01 -5 5 2 2011.87 65.34 -5 5 2 1981.62 63.07 5 -5 -2 1813.68 58.26 5 -5 -2 1927.03 60.39 -5 5 2 1960.59 53.81 5 -5 -2 1961.62 54.35 -3 -2 -8 5.68 0.41 3 2 8 6.00 1.66 3 2 8 5.44 1.44 -3 -2 -8 4.39 1.34 -3 -2 -8 2.99 0.46 -3 -2 -8 3.91 1.57 3 4 -6 11.67 2.09 -3 -4 6 16.76 2.42 3 4 -6 11.34 1.88 -3 -4 6 16.40 1.85 3 4 -6 13.05 1.76 -3 -4 6 11.04 1.90 4 -6 -5 262.11 4.47 4 -6 -5 271.47 7.80 4 -6 -5 258.70 7.27 -4 6 5 265.01 4.72 -4 6 5 284.63 8.00 -4 6 5 242.02 6.60 -5 0 -2 225.66 6.38 -5 0 -2 239.64 6.90 -5 0 -2 229.60 7.70 -5 0 -2 243.59 9.24 -5 0 -2 229.04 6.70 5 0 2 231.23 7.99 -2 -5 7 2.72 1.75 2 5 -7 1.47 1.24 2 5 -7 2.10 1.22 2 5 -7 2.61 1.36 -2 -5 7 2.68 1.29 -2 -5 7 1.34 1.16 -3 -5 -2 8.53 1.51 -3 -5 -2 9.02 1.94 3 5 2 7.23 1.15 -3 -5 -2 7.28 1.43 3 5 2 10.76 1.54 3 5 2 6.72 1.62 -3 8 2 45.25 1.84 3 -8 -2 42.54 1.85 3 -8 -2 43.34 2.61 -3 8 2 50.57 1.01 -3 8 2 53.74 2.99 -3 8 2 48.65 0.80 3 5 -3 57.06 3.27 -3 -5 3 55.81 3.72 3 5 -3 48.66 3.05 -3 -5 3 58.51 4.35 3 5 -3 65.74 3.31 -3 -5 3 57.71 3.50 -1 6 8 2806.69 89.29 1 -6 -8 2353.99 78.54 1 -6 -8 2768.15 80.19 -1 6 8 2815.34 82.61 1 -6 -8 2592.22 78.95 1 -6 -8 2582.17 80.38 2 -5 -9 10.57 0.69 2 -5 -9 8.18 1.47 -2 5 9 6.23 1.59 2 -5 -9 10.28 0.51 -2 5 9 8.68 0.93 -2 5 9 12.96 1.51 -4 -2 -5 2858.83 98.25 -4 -2 -5 2968.01 93.08 -4 -2 -5 2953.11 99.61 -4 -2 -5 2747.95 85.40 4 2 5 2944.61 101.96 -4 -2 -5 2806.93 93.99 -3 6 7 27.19 1.76 -3 6 7 31.83 2.69 3 -6 -7 29.14 0.45 3 -6 -7 28.61 1.80 -3 6 7 32.34 1.76 1 5 8 473.08 13.02 1 5 8 412.42 6.95 -1 -5 -8 413.67 7.11 -1 -5 -8 408.03 11.67 -1 -5 -8 439.06 11.73 -1 -5 -8 429.74 11.16 -3 8 -3 28.90 3.31 -3 8 -3 28.05 2.74 3 -8 3 28.85 2.51 3 -8 3 25.26 0.70 3 -8 3 24.35 3.09 -3 8 -3 28.50 0.72 2 -7 7 68.69 3.83 -2 7 -7 88.30 4.04 -2 7 -7 76.21 6.29 2 -7 7 64.89 2.40 2 -7 7 71.85 3.65 2 -7 7 79.39 2.68 5 -1 -4 33.32 2.86 -5 1 4 27.98 1.63 -5 1 4 26.59 2.32 -5 1 4 29.40 1.44 -5 1 4 32.22 2.62 -5 1 4 29.17 2.57 3 -7 6 36.22 2.66 -3 7 -6 38.82 3.22 -3 7 -6 50.34 2.86 3 -7 6 36.15 4.08 -3 7 -6 44.76 1.71 3 -7 6 35.66 2.44 0 -4 -10 1.53 0.69 0 4 10 0.65 1.22 0 -4 -10 1.77 1.16 0 -4 -10 1.65 0.76 2 3 9 24.20 2.35 2 3 9 20.28 1.97 -2 -3 -9 19.12 2.25 -2 -3 -9 20.57 1.82 3 3 7 5.35 1.65 -3 -3 -7 7.58 2.38 -3 -3 -7 6.01 0.51 -3 -3 -7 5.22 1.51 -3 -3 -7 4.70 0.62 -3 -3 -7 4.78 1.40 -3 4 9 32.79 2.53 -3 4 9 32.41 1.85 -3 4 9 30.24 1.75 -3 4 9 31.79 2.31 -4 2 8 52.86 2.74 4 -2 -8 52.21 3.43 -4 2 8 58.10 3.06 -4 2 8 52.89 3.43 -4 2 8 52.84 1.16 -4 2 8 54.98 1.21 -2 1 11 3.05 1.49 -2 1 11 2.98 1.57 2 -1 -11 4.13 0.62 -2 1 11 3.41 0.84 -2 1 11 2.15 0.59 -2 1 11 2.07 1.00 0 -5 -9 25.37 0.71 0 5 9 24.82 2.18 0 5 9 26.39 0.69 0 -5 -9 26.15 1.59 0 -5 -9 24.07 2.07 0 -5 -9 23.47 2.17 4 -7 -3 45.83 1.79 4 -7 -3 47.63 1.98 -4 7 3 46.33 1.56 -4 7 3 47.95 1.64 -4 7 3 56.97 2.88 4 -7 -3 51.58 2.81 -5 0 3 3.53 2.27 5 0 -3 2.09 1.70 -5 0 3 2.71 1.05 -5 0 3 3.41 0.99 -5 0 3 4.42 1.29 -2 0 11 17.59 1.76 2 0 -11 19.42 1.50 -2 0 11 17.80 2.39 2 0 -11 16.32 1.20 -2 0 11 18.71 2.50 -2 0 11 16.85 1.13 5 -4 4 6.80 1.43 5 -4 4 7.10 1.33 -5 4 -4 5.65 2.18 5 -4 4 3.80 1.32 -5 4 -4 4.18 1.27 -5 4 -4 4.93 1.35 -4 -3 -3 92.43 5.37 4 3 3 93.55 4.36 -4 -3 -3 91.47 3.33 -4 -3 -3 82.80 3.99 -4 -3 -3 88.12 4.20 -4 -3 -3 87.79 4.20 0 8 -3 5.66 1.76 0 -8 3 4.98 1.55 0 -8 3 4.43 1.66 0 8 -3 3.57 0.68 0 8 -3 4.15 1.52 0 -8 3 3.84 0.99 -4 1 8 -0.61 0.91 -4 1 8 0.34 0.42 4 -1 -8 2.08 1.16 -4 1 8 0.15 1.53 -4 1 8 -0.36 1.10 4 -1 -8 0.14 0.39 -5 4 4 89.34 5.49 5 -4 -4 88.83 4.07 -5 4 4 84.33 3.71 -5 4 4 83.58 2.05 -5 4 4 85.67 1.92 5 -4 -4 83.86 4.02 4 1 -7 16.85 1.29 4 1 -7 13.71 1.95 -4 -1 7 17.85 1.39 4 1 -7 13.69 2.45 -4 -1 7 14.30 2.31 -4 -1 7 14.43 2.28 0 -8 -2 27.10 1.09 0 8 2 32.69 1.68 0 8 2 34.83 2.22 0 -8 -2 28.70 2.07 0 8 2 34.45 2.44 0 -8 -2 25.73 2.49 2 -6 -8 14.68 0.65 -2 6 8 17.45 1.14 -2 6 8 17.39 1.48 -2 6 8 12.41 1.47 2 -6 -8 13.75 0.74 2 -6 -8 15.40 1.09 -1 -4 10 75.08 3.43 -1 -4 10 81.34 4.57 -1 -4 10 81.58 5.82 1 4 -10 78.13 5.04 1 4 -10 68.43 3.59 -1 -4 10 82.12 5.66 2 -1 11 27.95 2.88 -2 1 -11 32.86 1.46 2 -1 11 28.61 2.38 2 -1 11 30.56 1.73 -2 1 -11 34.89 2.25 -2 1 -11 34.69 2.81 -3 -1 -9 3.99 0.65 -3 -1 -9 4.57 1.60 -3 -1 -9 4.42 2.02 -3 -1 -9 3.17 0.71 3 1 9 5.17 1.45 3 1 9 4.89 1.70 5 -5 3 29.77 2.06 -5 5 -3 30.46 2.41 -5 5 -3 31.95 2.05 -5 5 -3 31.70 2.04 5 -5 3 26.58 2.03 5 -5 3 29.84 2.38 2 -2 11 61.32 2.09 -2 2 -11 55.03 2.34 -2 2 -11 60.06 3.03 -2 2 -11 67.78 3.62 2 -2 11 57.47 3.17 2 -2 11 53.48 3.51 4 -2 8 38.45 1.88 4 -2 8 43.58 2.88 4 -2 8 40.12 3.02 -4 2 -8 42.18 2.98 -4 2 -8 43.54 2.83 -4 2 -8 43.05 2.75 -2 -4 -8 40.25 0.74 -2 -4 -8 40.34 0.81 -2 -4 -8 43.87 2.65 -2 -4 -8 42.34 4.07 -2 -4 -8 41.71 2.38 2 4 8 46.22 4.44 4 3 -4 121.75 4.41 -4 -3 4 137.93 5.73 4 3 -4 121.13 4.76 4 3 -4 132.33 5.67 -4 -3 4 126.80 6.47 5 -1 4 15.14 1.60 5 -1 4 18.79 2.25 -5 1 -4 14.00 2.78 -5 1 -4 15.62 3.38 -5 1 -4 15.25 1.56 5 -1 4 18.24 1.97 -2 4 10 27.89 2.42 -2 4 10 31.46 2.23 2 -4 -10 34.06 0.83 -2 4 10 28.20 2.45 2 -4 -10 28.81 1.06 -2 4 10 31.21 1.38 1 -5 10 16.21 2.04 1 -5 10 19.12 2.02 1 -5 10 16.19 1.87 -1 5 -10 18.28 2.15 -1 5 -10 17.79 2.22 1 -5 10 19.02 3.23 2 -8 -4 4.15 0.87 -2 8 4 2.92 0.43 -2 8 4 3.77 1.19 -2 8 4 3.57 0.79 -2 8 4 2.69 0.68 2 -8 -4 2.80 1.00 -2 -6 5 40.49 3.56 2 6 -5 39.09 2.44 2 6 -5 30.42 4.20 -2 -6 5 33.70 2.25 -2 -6 5 31.88 2.95 2 6 -5 35.42 2.72 -4 -2 6 86.86 3.44 -4 -2 6 90.77 4.25 -4 -2 6 97.76 4.63 4 2 -6 86.86 4.66 4 2 -6 83.00 3.78 4 2 -6 81.24 3.09 3 -1 -10 48.79 3.36 -3 1 10 47.04 2.59 3 -1 -10 39.11 1.31 -3 1 10 34.22 3.14 -3 1 10 41.09 3.29 -3 1 10 42.20 1.23 -2 -6 -4 32.59 2.02 2 6 4 31.20 1.63 -2 -6 -4 41.89 2.82 2 6 4 40.46 2.28 -2 -6 -4 30.98 2.23 2 6 4 31.49 2.38 -1 -5 9 54.26 3.17 -1 -5 9 55.45 3.32 -1 -5 9 60.20 4.11 1 5 -9 48.83 4.85 1 5 -9 55.78 4.58 -1 -5 9 60.65 3.10 5 -5 -3 69.09 3.09 -5 5 3 71.46 2.43 5 -5 -3 70.76 3.62 -5 5 3 72.80 3.65 5 -5 -3 68.74 1.88 -5 5 3 69.28 2.90 1 -3 -11 694.87 16.60 -1 3 11 669.08 19.89 -1 3 11 674.92 15.80 -1 3 11 703.38 14.86 -1 3 11 718.36 16.22 -1 3 11 688.75 20.19 4 -5 7 93.00 4.13 -4 5 -7 94.05 3.88 -4 5 -7 100.98 3.97 -4 5 -7 94.84 4.99 4 -5 7 97.78 3.79 4 -5 7 83.81 3.58 -4 3 -8 77.96 4.07 -4 3 -8 73.14 3.64 4 -3 8 78.62 3.78 4 -3 8 77.16 3.83 4 -3 8 76.59 2.83 -4 3 -8 81.96 3.85 1 7 -5 24.61 2.76 1 7 -5 21.28 1.73 -1 -7 5 27.97 3.11 -1 -7 5 25.51 1.59 -1 -7 5 26.61 2.60 1 7 -5 24.39 2.50 -4 3 8 215.17 7.24 -4 3 8 225.47 6.89 -4 3 8 228.60 6.60 4 -3 -8 216.68 7.91 -2 -2 -10 20.77 1.96 2 2 10 26.67 3.15 -2 -2 -10 24.54 2.57 2 2 10 31.17 2.67 -2 8 -5 25.93 3.06 2 -8 5 27.21 2.28 2 -8 5 23.24 2.55 2 -8 5 23.49 1.38 2 -8 5 25.98 1.51 -2 8 -5 33.85 3.83 -5 0 -3 16.20 1.98 -5 0 -3 14.69 1.59 -5 0 -3 11.17 2.15 -5 0 -3 13.26 1.76 5 0 3 15.45 2.28 -5 0 -3 15.18 1.47 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-3 16 2.04 1.65 7 3 -16 -1.26 1.55 -6 9 -18 1.66 3.21 -6 -10 -5 -1.53 4.33 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68709