data_shelx _audit_creation_method 'SHELXL-2018/1' _shelx_SHELXL_version_number '2018/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cd1.91 H18 Cu6 O25 S2' _chemical_formula_weight 1076.66 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 '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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3200(15) _cell_length_b 25.424(5) _cell_length_c 11.283(2) _cell_angle_alpha 90 _cell_angle_beta 91.62(3) _cell_angle_gamma 90 _cell_volume 2099.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29907 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.55 _exptl_crystal_description blade _exptl_crystal_colour blue _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.374 _exptl_crystal_F_000 2045 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.024 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 8.235 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3773 _exptl_absorpt_correction_T_max 0.4356 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Dectris EigerX 16M' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35699 _diffrn_reflns_av_unetI/netI 0.0148 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.602 _diffrn_reflns_theta_max 29.969 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 6032 _reflns_number_gt 5997 _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_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.0561P)^2^+39.3006P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)' _refine_ls_extinction_coef 0.00000(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6032 _refine_ls_number_parameters 388 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.156 _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 Cd1 Cd 0.64513(5) 0.44492(2) -0.25016(3) 0.01139(15) Uani 1.009(3) 1 d . . P . . Cd2 Cd 0.33181(8) 0.81361(2) 0.25308(4) 0.0195(2) Uani 0.915(3) 1 d . . P . . Cu1 Cu 0.36780(9) 0.68662(3) 0.25295(6) 0.0106(2) Uani 1 1 d . . P . . Cu2 Cu 0.37979(9) 0.74930(2) 0.50325(6) 0.0105(2) Uani 1 1 d . . P . . Cu3 Cu 0.40712(9) 0.61959(3) 0.50764(5) 0.0100(2) Uani 1 1 d . . P . . Cu4 Cu 0.45531(9) 0.56276(3) 0.75963(5) 0.0108(2) Uani 1 1 d . . P . . Cu5 Cu 0.500000 0.500000 0.000000 0.0102(3) Uani 1 2 d S . P . . Cu6 Cu 0.500000 0.500000 0.500000 0.0099(3) Uani 1 2 d S . P . . Cu7 Cu 0.39075(9) 0.62890(3) 0.01125(6) 0.0108(2) 1 1 d . . P . . S1 S 0.79711(17) 0.68912(5) 0.13529(12) 0.0123(4) Uani 1 1 d . . P . . S2 S 0.84439(18) 0.58768(5) 0.53740(13) 0.0140(4) Uani 1 1 d . . P . . O1 O 0.9035(6) 0.71761(18) 0.0470(4) 0.0220(9) Uani 1 1 d . . . . . O2 O 0.8255(6) 0.71373(17) 0.2540(4) 0.0184(8) Uani 1 1 d . . . . . O3 O 0.5986(5) 0.69049(15) 0.1018(4) 0.0134(7) Uani 1 1 d . . . . . O4 O 0.8580(6) 0.63313(16) 0.1405(4) 0.0171(8) Uani 1 1 d . . . . . O5 O 0.9864(6) 0.5554(2) 0.5955(5) 0.0278(11) Uani 1 1 d . . . . . O6 O 0.8812(6) 0.64419(17) 0.5573(4) 0.0214(9) Uani 1 1 d . . . . . O7 O 0.6631(5) 0.57437(15) 0.5834(4) 0.0138(7) Uani 1 1 d . . . . . O8 O 0.8416(7) 0.5790(2) 0.4069(4) 0.0270(10) Uani 1 1 d . . . . . OH9 O 0.2513(5) 0.62934(16) 0.1586(3) 0.0135(7) Uani 1 1 d D . . . . OH10 O 0.3106(5) 0.55193(15) 0.4506(3) 0.0123(7) Uani 1 1 d D . . . . OH11 O 0.6275(5) 0.52147(15) -0.1428(3) 0.0114(7) Uani 1 1 d D . . . . OH12 O 0.5841(5) 0.50159(16) 0.3354(3) 0.0127(7) Uani 1 1 d D . . . . OH13 O 0.5274(5) 0.56950(15) 0.0781(3) 0.0124(7) Uani 1 1 d D . . . . OH14 O 0.4891(5) 0.63065(16) 0.3450(3) 0.0130(7) Uani 1 1 d D . . . . OH15 O 0.2511(6) 0.75705(18) 0.6555(4) 0.0179(8) Uani 1 1 d D . . . . OH16 O 0.2951(6) 0.60950(18) 0.6635(4) 0.0160(8) Uani 1 1 d D . . . . OH17 O 0.2529(6) 0.81285(16) 0.4443(4) 0.0161(8) Uani 1 1 d D . . . . OH18 O 0.5084(6) 0.62612(16) -0.1446(3) 0.0147(8) Uani 1 1 d D . . . . OH19 O 0.4815(6) 0.74416(16) 0.3454(4) 0.0131(7) Uani 1 1 d D . . . . OH20 O 0.4955(6) 0.68680(15) 0.5706(4) 0.0142(8) Uani 1 1 d D . . . . OW21 O 0.1254(6) 0.69165(18) 0.4069(4) 0.0196(9) Uani 1 1 d D . . . . OW22 O 0.9625(6) 0.47196(17) -0.2472(4) 0.0184(8) Uani 1 1 d D . . . . OW23 O 0.9722(8) 0.6821(2) 0.7622(5) 0.0367(13) Uani 1 1 d . . . . . OW24 O 0.2146(6) 0.53142(19) -0.1041(4) 0.0214(9) Uani 1 1 d D . . . . OW25 O 0.9190(7) 0.5971(2) -0.0835(5) 0.0318(12) Uani 1 1 d D . . . . H9 H 0.139(5) 0.629(4) 0.148(10) 0.050 Uiso 1 1 d D U . . . H10 H 0.207(7) 0.549(4) 0.476(9) 0.050 Uiso 1 1 d D U . . . H11 H 0.715(10) 0.540(4) -0.123(9) 0.050 Uiso 1 1 d D U . . . H12 H 0.680(9) 0.518(4) 0.344(10) 0.050 Uiso 1 1 d D U . . . H13 H 0.627(8) 0.582(4) 0.095(10) 0.050 Uiso 1 1 d D U . . . H14 H 0.597(6) 0.639(4) 0.344(10) 0.050 Uiso 1 1 d D U . . . H15 H 0.140(5) 0.760(4) 0.640(10) 0.050 Uiso 1 1 d D U . . . H16 H 0.192(7) 0.597(4) 0.662(10) 0.050 Uiso 1 1 d D U . . . H17 H 0.145(6) 0.809(4) 0.460(10) 0.050 Uiso 1 1 d D U . . . H18 H 0.618(5) 0.632(4) -0.133(10) 0.050 Uiso 1 1 d D U . . . H19 H 0.587(6) 0.737(4) 0.331(10) 0.050 Uiso 1 1 d D U . . . H20 H 0.605(5) 0.685(4) 0.558(10) 0.050 Uiso 1 1 d D U . . . H21A H 0.055(11) 0.700(4) 0.353(6) 0.050 Uiso 1 1 d D U . . . H21B H 0.064(12) 0.674(4) 0.452(7) 0.050 Uiso 1 1 d D U . . . H22A H 1.011(14) 0.449(3) -0.285(8) 0.050 Uiso 1 1 d D U . . . H22B H 0.964(15) 0.498(2) -0.287(7) 0.050 Uiso 1 1 d D U . . . H24A H 0.149(11) 0.557(3) -0.086(9) 0.050 Uiso 1 1 d D U . . . H24B H 0.143(11) 0.512(3) -0.141(8) 0.050 Uiso 1 1 d D U . . . H25A H 0.925(16) 0.609(4) -0.016(4) 0.050 Uiso 1 1 d D U . . . 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 Cd1 0.0131(2) 0.0118(2) 0.0093(2) -0.00109(12) 0.00148(13) 0.00125(13) Cd2 0.0401(4) 0.0094(3) 0.0090(2) 0.00075(14) -0.00002(18) -0.00056(18) Cu1 0.0103(3) 0.0114(3) 0.0102(3) 0.0001(2) 0.0002(2) 0.0000(2) Cu2 0.0111(3) 0.0108(3) 0.0098(3) -0.0010(2) 0.0017(2) 0.0005(2) Cu3 0.0105(3) 0.0112(3) 0.0082(3) -0.0014(2) 0.0013(2) 0.0014(2) Cu4 0.0103(3) 0.0128(3) 0.0091(3) -0.0015(2) -0.0002(2) 0.0010(2) Cu5 0.0113(5) 0.0107(5) 0.0089(4) -0.0015(3) 0.0025(3) 0.0002(3) Cu6 0.0100(4) 0.0116(4) 0.0081(4) -0.0008(3) 0.0017(3) 0.0002(3) Cu7 0.0107(3) 0.0110(3) 0.0106(3) -0.0004(2) 0.0006(2) -0.0016(2) S1 0.0084(6) 0.0135(6) 0.0150(7) -0.0007(4) 0.0012(4) -0.0005(4) S2 0.0092(6) 0.0131(7) 0.0200(7) -0.0016(5) 0.0027(4) -0.0004(4) O1 0.017(2) 0.025(2) 0.025(2) 0.0066(17) 0.0066(16) -0.0021(17) O2 0.0153(18) 0.022(2) 0.0181(19) -0.0043(16) -0.0033(15) 0.0041(15) O3 0.0101(17) 0.0148(17) 0.0152(17) -0.0020(14) -0.0005(13) 0.0001(13) O4 0.0173(19) 0.0143(18) 0.0196(19) -0.0005(15) -0.0010(15) 0.0063(15) O5 0.014(2) 0.026(2) 0.044(3) 0.011(2) -0.0045(19) -0.0019(17) O6 0.023(2) 0.0145(19) 0.027(2) 0.0025(16) 0.0030(17) -0.0026(16) O7 0.0104(17) 0.0140(17) 0.0171(18) 0.0003(14) 0.0034(14) 0.0013(13) O8 0.021(2) 0.036(3) 0.024(2) -0.0035(19) 0.0042(18) -0.0046(19) OH9 0.0109(17) 0.0154(18) 0.0142(17) -0.0007(14) 0.0015(13) -0.0024(14) OH10 0.0097(16) 0.0139(17) 0.0133(17) -0.0011(13) 0.0005(13) 0.0004(13) OH11 0.0094(16) 0.0135(17) 0.0113(16) 0.0005(13) 0.0009(13) -0.0004(13) OH12 0.0121(17) 0.0157(17) 0.0102(16) -0.0034(13) 0.0024(13) -0.0012(14) OH13 0.0133(17) 0.0104(16) 0.0136(17) -0.0015(13) 0.0010(13) -0.0011(13) OH14 0.0134(17) 0.0145(17) 0.0110(16) 0.0017(13) 0.0011(13) 0.0017(14) OH15 0.0117(18) 0.028(2) 0.0141(18) -0.0046(16) 0.0004(14) -0.0028(16) OH16 0.0120(17) 0.024(2) 0.0122(17) 0.0027(15) 0.0013(14) 0.0035(15) OH17 0.0098(17) 0.0171(19) 0.022(2) -0.0008(15) 0.0014(15) 0.0024(14) OH18 0.0158(18) 0.0164(18) 0.0119(17) -0.0054(14) -0.0011(14) -0.0006(15) OH19 0.0135(17) 0.0138(17) 0.0122(17) -0.0022(13) 0.0011(14) 0.0015(14) OH20 0.0164(18) 0.0106(17) 0.0157(18) -0.0019(13) 0.0002(14) 0.0017(14) OW21 0.0124(18) 0.023(2) 0.023(2) -0.0010(17) 0.0019(15) -0.0030(16) OW22 0.0157(19) 0.0155(19) 0.024(2) -0.0020(16) 0.0042(16) -0.0004(15) OW23 0.030(3) 0.042(3) 0.038(3) -0.001(2) -0.005(2) 0.002(2) OW24 0.018(2) 0.026(2) 0.020(2) -0.0034(17) -0.0006(16) 0.0004(17) OW25 0.023(2) 0.039(3) 0.034(3) -0.021(2) 0.011(2) -0.012(2) _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 Cd1 OH9 2.272(4) 3_665 ? Cd1 OH10 2.295(4) 3_665 ? Cd1 OH11 2.298(4) . ? Cd1 OH12 2.345(4) 3_665 ? Cd1 OH13 2.374(4) 3_665 ? Cd1 OH14 2.397(4) 3_665 ? Cd1 OW22 2.422(4) . ? Cd2 OH15 2.180(5) 4_575 ? Cd2 OH16 2.213(4) 4_575 ? Cd2 OH17 2.249(4) . ? Cd2 OH18 2.295(4) 4_576 ? Cd2 OH19 2.311(4) . ? Cd2 OH20 2.412(4) 4_575 ? Cd2 OW23 2.640(6) 4_475 ? Cd2 Cu1 3.2393(10) . ? Cd2 Cu2 3.2686(9) 4_575 ? Cu1 OH14 1.960(4) . ? Cu1 OH19 1.968(4) . ? Cu1 OH9 1.983(4) . ? Cu1 OH15 1.984(4) 4_575 ? Cu1 O3 2.436(4) . ? Cu2 OH20 1.945(4) . ? Cu2 OH19 1.954(4) . ? Cu2 OH17 1.970(4) . ? Cu2 OH15 1.992(4) . ? Cu3 OH20 1.953(4) . ? Cu3 OH10 1.961(4) . ? Cu3 OH14 1.967(4) . ? Cu3 OH16 1.978(4) . ? Cu3 O7 2.339(4) . ? Cu4 OH11 1.956(4) 1_556 ? Cu4 OH18 1.973(4) 1_556 ? Cu4 OH16 1.973(4) . ? Cu4 OH12 1.973(4) 3_666 ? Cu5 OH11 1.962(4) . ? Cu5 OH11 1.962(4) 3_665 ? Cu5 OH13 1.982(4) 3_665 ? Cu5 OH13 1.982(4) . ? Cu6 OH12 1.973(4) 3_666 ? Cu6 OH12 1.973(4) . ? Cu6 OH10 1.983(4) . ? Cu6 OH10 1.983(4) 3_666 ? Cu6 O7 2.413(4) 3_666 ? Cu6 O7 2.413(4) . ? Cu7 OH17 1.933(4) 4_575 ? Cu7 OH13 1.951(4) . ? Cu7 OH9 1.975(4) . ? Cu7 OH18 1.981(4) . ? Cu7 O3 2.392(4) . ? S1 O1 1.472(4) . ? S1 O2 1.488(4) 1 ? S1 O2 1.488(4) . ? S1 O3 1.492(4) . ? S1 O4 1.492(4) . ? S1 O4 1.492(4) 1 ? S2 O5 1.465(5) . ? S2 O6 1.478(5) 1 ? S2 O6 1.478(5) . ? S2 O7 1.478(4) . ? S2 O8 1.488(5) . ? S2 O8 1.488(5) 1 ? O2 O2 0.000(16) 1 ? O4 O4 0.000(15) 1 ? O6 O6 0.000(13) 1 ? O8 O8 0.000(11) 1 ? OH9 H9 0.83(3) . ? OH10 H10 0.82(3) . ? OH11 H11 0.82(3) . ? OH12 H12 0.81(3) . ? OH13 H13 0.82(3) . ? OH14 H14 0.82(3) . ? OH15 H15 0.83(3) . ? OH16 H16 0.82(3) . ? OH17 H17 0.82(3) . ? OH18 H18 0.82(3) . ? OH19 H19 0.81(3) . ? OH20 H20 0.82(3) . ? OW21 H21A 0.81(3) . ? OW21 H21B 0.82(3) . ? OW22 H22A 0.81(3) . ? OW22 H22B 0.81(3) . ? OW24 H24A 0.83(3) . ? OW24 H24B 0.83(3) . ? OW25 OW25 0.000(17) 1 ? OW25 H25A 0.82(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OH9 Cd1 OH10 115.00(14) 3_665 3_665 ? OH9 Cd1 OH11 119.14(14) 3_665 . ? OH10 Cd1 OH11 120.11(14) 3_665 . ? OH9 Cd1 OH12 153.40(14) 3_665 3_665 ? OH10 Cd1 OH12 72.23(13) 3_665 3_665 ? OH11 Cd1 OH12 71.03(13) . 3_665 ? OH9 Cd1 OH13 71.23(14) 3_665 3_665 ? OH10 Cd1 OH13 154.73(14) 3_665 3_665 ? OH11 Cd1 OH13 70.15(13) . 3_665 ? OH12 Cd1 OH13 91.95(14) 3_665 3_665 ? OH9 Cd1 OH14 70.38(14) 3_665 3_665 ? OH10 Cd1 OH14 69.84(13) 3_665 3_665 ? OH11 Cd1 OH14 152.37(14) . 3_665 ? OH12 Cd1 OH14 90.12(14) 3_665 3_665 ? OH13 Cd1 OH14 91.18(13) 3_665 3_665 ? OH9 Cd1 OW22 85.53(15) 3_665 . ? OH10 Cd1 OW22 80.90(15) 3_665 . ? OH11 Cd1 OW22 79.66(14) . . ? OH12 Cd1 OW22 121.06(14) 3_665 . ? OH13 Cd1 OW22 124.37(14) 3_665 . ? OH14 Cd1 OW22 127.94(14) 3_665 . ? OH15 Cd2 OH16 118.00(16) 4_575 4_575 ? OH15 Cd2 OH17 113.83(16) 4_575 . ? OH16 Cd2 OH17 114.49(15) 4_575 . ? OH15 Cd2 OH18 160.92(16) 4_575 4_576 ? OH16 Cd2 OH18 72.52(14) 4_575 4_576 ? OH17 Cd2 OH18 71.30(15) . 4_576 ? OH15 Cd2 OH19 73.51(15) 4_575 . ? OH16 Cd2 OH19 158.53(15) 4_575 . ? OH17 Cd2 OH19 72.08(14) . . ? OH18 Cd2 OH19 91.73(14) 4_576 . ? OH15 Cd2 OH20 72.49(15) 4_575 4_575 ? OH16 Cd2 OH20 70.78(14) 4_575 4_575 ? OH17 Cd2 OH20 165.08(15) . 4_575 ? OH18 Cd2 OH20 98.41(14) 4_576 4_575 ? OH19 Cd2 OH20 98.10(14) . 4_575 ? OH15 Cd2 OW23 78.32(18) 4_575 4_475 ? OH16 Cd2 OW23 82.70(17) 4_575 4_475 ? OH17 Cd2 OW23 71.30(17) . 4_475 ? OH18 Cd2 OW23 120.05(17) 4_576 4_475 ? OH19 Cd2 OW23 118.34(17) . 4_475 ? OH20 Cd2 OW23 123.61(17) 4_575 4_475 ? OH15 Cd2 Cu1 36.80(11) 4_575 . ? OH16 Cd2 Cu1 152.73(11) 4_575 . ? OH17 Cd2 Cu1 90.85(11) . . ? OH18 Cd2 Cu1 128.38(10) 4_576 . ? OH19 Cd2 Cu1 36.96(10) . . ? OH20 Cd2 Cu1 87.30(9) 4_575 . ? OW23 Cd2 Cu1 97.03(13) 4_475 . ? OH15 Cd2 Cu2 36.42(11) 4_575 4_575 ? OH16 Cd2 Cu2 93.04(11) 4_575 4_575 ? OH17 Cd2 Cu2 149.29(11) . 4_575 ? OH18 Cd2 Cu2 133.46(11) 4_576 4_575 ? OH19 Cd2 Cu2 87.34(10) . 4_575 ? OH20 Cd2 Cu2 36.23(10) 4_575 4_575 ? OW23 Cd2 Cu2 100.69(14) 4_475 4_575 ? Cu1 Cd2 Cu2 60.074(19) . 4_575 ? OH14 Cu1 OH19 94.60(18) . . ? OH14 Cu1 OH9 86.14(17) . . ? OH19 Cu1 OH9 179.25(17) . . ? OH14 Cu1 OH15 178.06(17) . 4_575 ? OH19 Cu1 OH15 85.78(18) . 4_575 ? OH9 Cu1 OH15 93.48(19) . 4_575 ? OH14 Cu1 O3 95.02(15) . . ? OH19 Cu1 O3 92.85(15) . . ? OH9 Cu1 O3 87.12(15) . . ? OH15 Cu1 O3 83.06(16) 4_575 . ? OH14 Cu1 Cd2 139.39(12) . . ? OH19 Cu1 Cd2 44.93(12) . . ? OH9 Cu1 Cd2 134.32(12) . . ? OH15 Cu1 Cd2 41.16(14) 4_575 . ? O3 Cu1 Cd2 91.04(9) . . ? OH20 Cu2 OH19 97.37(17) . . ? OH20 Cu2 OH17 176.28(18) . . ? OH19 Cu2 OH17 86.30(18) . . ? OH20 Cu2 OH15 87.44(19) . . ? OH19 Cu2 OH15 173.83(18) . . ? OH17 Cu2 OH15 88.86(19) . . ? OH20 Cu2 Cd2 47.13(13) . 4_576 ? OH19 Cu2 Cd2 143.73(12) . 4_576 ? OH17 Cu2 Cd2 129.15(13) . 4_576 ? OH15 Cu2 Cd2 40.52(14) . 4_576 ? OH20 Cu3 OH10 177.35(17) . . ? OH20 Cu3 OH14 96.16(18) . . ? OH10 Cu3 OH14 86.31(17) . . ? OH20 Cu3 OH16 86.08(18) . . ? OH10 Cu3 OH16 91.37(18) . . ? OH14 Cu3 OH16 173.27(17) . . ? OH20 Cu3 O7 92.50(16) . . ? OH10 Cu3 O7 88.06(15) . . ? OH14 Cu3 O7 98.55(15) . . ? OH16 Cu3 O7 87.67(16) . . ? OH11 Cu4 OH18 90.90(17) 1_556 1_556 ? OH11 Cu4 OH16 175.22(17) 1_556 . ? OH18 Cu4 OH16 85.08(18) 1_556 . ? OH11 Cu4 OH12 86.73(16) 1_556 3_666 ? OH18 Cu4 OH12 176.99(17) 1_556 3_666 ? OH16 Cu4 OH12 97.20(18) . 3_666 ? OH11 Cu5 OH11 180.0 . 3_665 ? OH11 Cu5 OH13 85.84(16) . 3_665 ? OH11 Cu5 OH13 94.16(16) 3_665 3_665 ? OH11 Cu5 OH13 94.16(16) . . ? OH11 Cu5 OH13 85.84(16) 3_665 . ? OH13 Cu5 OH13 180.0(2) 3_665 . ? OH12 Cu6 OH12 180.0 3_666 . ? OH12 Cu6 OH10 92.54(16) 3_666 . ? OH12 Cu6 OH10 87.46(16) . . ? OH12 Cu6 OH10 87.46(16) 3_666 3_666 ? OH12 Cu6 OH10 92.54(16) . 3_666 ? OH10 Cu6 OH10 180.0 . 3_666 ? OH12 Cu6 O7 100.77(15) 3_666 3_666 ? OH12 Cu6 O7 79.23(15) . 3_666 ? OH10 Cu6 O7 94.47(15) . 3_666 ? OH10 Cu6 O7 85.53(15) 3_666 3_666 ? OH12 Cu6 O7 79.23(15) 3_666 . ? OH12 Cu6 O7 100.77(15) . . ? OH10 Cu6 O7 85.53(15) . . ? OH10 Cu6 O7 94.47(15) 3_666 . ? O7 Cu6 O7 180.00(19) 3_666 . ? OH17 Cu7 OH13 179.26(17) 4_575 . ? OH17 Cu7 OH9 92.76(18) 4_575 . ? OH13 Cu7 OH9 87.16(17) . . ? OH17 Cu7 OH18 85.18(18) 4_575 . ? OH13 Cu7 OH18 94.84(17) . . ? OH9 Cu7 OH18 174.42(17) . . ? OH17 Cu7 O3 89.09(16) 4_575 . ? OH13 Cu7 O3 91.64(15) . . ? OH9 Cu7 O3 88.52(15) . . ? OH18 Cu7 O3 96.62(15) . . ? O1 S1 O2 109.8(3) . 1 ? O1 S1 O2 109.8(3) . . ? O2 S1 O2 0.0(5) 1 . ? O1 S1 O3 110.3(3) . . ? O2 S1 O3 109.2(2) 1 . ? O2 S1 O3 109.2(2) . . ? O1 S1 O4 109.4(3) . . ? O2 S1 O4 109.4(2) 1 . ? O2 S1 O4 109.4(2) . . ? O3 S1 O4 108.7(2) . . ? O1 S1 O4 109.4(3) . 1 ? O2 S1 O4 109.4(2) 1 1 ? O2 S1 O4 109.4(2) . 1 ? O3 S1 O4 108.7(2) . 1 ? O4 S1 O4 0.0(5) . 1 ? O5 S2 O6 110.6(3) . 1 ? O5 S2 O6 110.6(3) . . ? O6 S2 O6 0.0(5) 1 . ? O5 S2 O7 110.4(3) . . ? O6 S2 O7 109.3(3) 1 . ? O6 S2 O7 109.3(3) . . ? O5 S2 O8 110.5(3) . . ? O6 S2 O8 106.9(3) 1 . ? O6 S2 O8 106.9(3) . . ? O7 S2 O8 109.0(3) . . ? O5 S2 O8 110.5(3) . 1 ? O6 S2 O8 106.9(3) 1 1 ? O6 S2 O8 106.9(3) . 1 ? O7 S2 O8 109.0(3) . 1 ? O8 S2 O8 0.0(5) . 1 ? O2 O2 S1 0(10) 1 . ? S1 O3 Cu7 134.1(2) . . ? S1 O3 Cu1 120.8(2) . . ? Cu7 O3 Cu1 80.07(12) . . ? O4 O4 S1 0(10) 1 . ? O6 O6 S2 0(10) 1 . ? S2 O7 Cu3 118.5(2) . . ? S2 O7 Cu6 118.8(2) . . ? Cu3 O7 Cu6 81.98(13) . . ? O8 O8 S2 0(10) 1 . ? Cu7 OH9 Cu1 103.39(18) . . ? Cu7 OH9 Cd1 101.80(17) . 3_665 ? Cu1 OH9 Cd1 103.49(17) . 3_665 ? Cu7 OH9 H9 114(8) . . ? Cu1 OH9 H9 119(8) . . ? Cd1 OH9 H9 113(8) 3_665 . ? Cu3 OH10 Cu6 104.43(18) . . ? Cu3 OH10 Cd1 103.50(17) . 3_665 ? Cu6 OH10 Cd1 100.57(16) . 3_665 ? Cu3 OH10 H10 107(8) . . ? Cu6 OH10 H10 119(8) . . ? Cd1 OH10 H10 120(8) 3_665 . ? Cu4 OH11 Cu5 107.33(18) 1_554 . ? Cu4 OH11 Cd1 101.69(16) 1_554 . ? Cu5 OH11 Cd1 103.44(16) . . ? Cu4 OH11 H11 109(8) 1_554 . ? Cu5 OH11 H11 108(8) . . ? Cd1 OH11 H11 125(8) . . ? Cu4 OH12 Cu6 116.7(2) 3_666 . ? Cu4 OH12 Cd1 99.56(16) 3_666 3_665 ? Cu6 OH12 Cd1 99.17(16) . 3_665 ? Cu4 OH12 H12 127(8) 3_666 . ? Cu6 OH12 H12 101(8) . . ? Cd1 OH12 H12 111(8) 3_665 . ? Cu7 OH13 Cu5 118.3(2) . . ? Cu7 OH13 Cd1 99.02(16) . 3_665 ? Cu5 OH13 Cd1 100.16(16) . 3_665 ? Cu7 OH13 H13 104(8) . . ? Cu5 OH13 H13 122(8) . . ? Cd1 OH13 H13 111(8) 3_665 . ? Cu1 OH14 Cu3 116.9(2) . . ? Cu1 OH14 Cd1 99.87(16) . 3_665 ? Cu3 OH14 Cd1 99.78(16) . 3_665 ? Cu1 OH14 H14 104(8) . . ? Cu3 OH14 H14 112(8) . . ? Cd1 OH14 H14 125(8) 3_665 . ? Cu1 OH15 Cu2 110.0(2) 4_576 . ? Cu1 OH15 Cd2 102.04(19) 4_576 4_576 ? Cu2 OH15 Cd2 103.1(2) . 4_576 ? Cu1 OH15 H15 117(8) 4_576 . ? Cu2 OH15 H15 108(8) . . ? Cd2 OH15 H15 116(8) 4_576 . ? Cu4 OH16 Cu3 108.18(19) . . ? Cu4 OH16 Cd2 102.62(18) . 4_576 ? Cu3 OH16 Cd2 104.09(19) . 4_576 ? Cu4 OH16 H16 108(8) . . ? Cu3 OH16 H16 116(8) . . ? Cd2 OH16 H16 117(8) 4_576 . ? Cu7 OH17 Cu2 105.1(2) 4_576 . ? Cu7 OH17 Cd2 102.87(19) 4_576 . ? Cu2 OH17 Cd2 101.51(18) . . ? Cu7 OH17 H17 119(8) 4_576 . ? Cu2 OH17 H17 107(8) . . ? Cd2 OH17 H17 119(8) . . ? Cu4 OH18 Cu7 115.6(2) 1_554 . ? Cu4 OH18 Cd2 99.78(17) 1_554 4_575 ? Cu7 OH18 Cd2 99.78(17) . 4_575 ? Cu4 OH18 H18 114(8) 1_554 . ? Cu7 OH18 H18 107(8) . . ? Cd2 OH18 H18 120(8) 4_575 . ? Cu2 OH19 Cu1 111.5(2) . . ? Cu2 OH19 Cd2 99.88(16) . . ? Cu1 OH19 Cd2 98.11(17) . . ? Cu2 OH19 H19 126(8) . . ? Cu1 OH19 H19 97(8) . . ? Cd2 OH19 H19 121(8) . . ? Cu2 OH20 Cu3 115.9(2) . . ? Cu2 OH20 Cd2 96.64(16) . 4_576 ? Cu3 OH20 Cd2 98.00(17) . 4_576 ? Cu2 OH20 H20 114(8) . . ? Cu3 OH20 H20 101(8) . . ? Cd2 OH20 H20 131(8) 4_576 . ? H21A OW21 H21B 105(5) . . ? Cd1 OW22 H22A 102(8) . . ? Cd1 OW22 H22B 105(8) . . ? H22A OW22 H22B 108(5) . . ? H24A OW24 H24B 103(5) . . ? OW25 OW25 H25A 0(10) 1 . ? 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 _geom_hbond_publ_flag OH9 H9 O4 0.83(3) 2.06(3) 2.883(6) 173(11) 1_455 yes OH10 H10 O5 0.82(3) 2.14(5) 2.921(7) 159(11) 1_455 yes OH16 H16 O5 0.82(3) 1.97(5) 2.736(7) 155(11) 1_455 yes OW21 H21A O2 0.81(3) 2.02(4) 2.810(6) 163(9) 1_455 yes OW21 H21B O6 0.82(3) 1.96(4) 2.775(6) 168(10) 1_455 yes OW24 H24A OW25 0.83(3) 1.98(5) 2.749(7) 155(9) 1_455 yes OW24 H24B OW22 0.83(3) 2.03(3) 2.851(6) 173(10) 1_455 yes OH11 H11 OW25 0.82(3) 2.12(3) 2.936(6) 171(11) 1 yes OH12 H12 O8 0.81(3) 2.07(6) 2.828(6) 154(11) 1 yes OH13 H13 O4 0.82(3) 2.18(4) 2.978(6) 166(11) 1 yes OH14 H14 O8 0.82(3) 2.43(10) 2.961(7) 123(9) 1 yes OW25 H25A O4 0.82(3) 1.94(5) 2.736(6) 162(12) 1 yes OH18 H18 OW25 0.82(3) 2.42(6) 3.151(7) 149(10) 1 yes OH19 H19 O2 0.81(3) 2.06(4) 2.854(6) 166(11) 1 yes OH20 H20 O6 0.82(3) 2.27(5) 3.032(6) 155(10) 1 yes OH15 H15 O1 0.83(3) 2.08(5) 2.866(6) 158(11) 4_476 yes OH17 H17 O1 0.82(3) 2.16(5) 2.942(6) 160(11) 4_476 yes OW22 H22A O8 0.81(3) 1.91(5) 2.671(7) 155(9) 3_765 yes OW22 H22B O5 0.81(3) 1.97(4) 2.775(7) 171(9) 1_554 yes _refine_diff_density_max 7.787 _refine_diff_density_min -5.570 _refine_diff_density_rms 0.246