# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mor20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'hydrated compound 1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Cu3 N2 O18 S2' _chemical_formula_weight 905.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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' Cu Cu 0.2862 1.4771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1434 0.1473 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.017(5) _cell_length_b 11.814(5) _cell_length_c 12.135(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 109.701(5) _cell_angle_gamma 90.000(5) _cell_volume 1487.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4736 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 34.65 _exptl_crystal_description Chip _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 2.890 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Bruker SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source '11.3.1 ALS, LBNL. CA' _diffrn_radiation_monochromator 'Si(111) Crystal' _diffrn_measurement_device_type 'Bruker AXS APEXII' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21375 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 34.65 _reflns_number_total 4736 _reflns_number_gt 4201 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEXII (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX restrain was used to fix the hydrogen atoms on the coordinated water molecules.Other hydrogen atoms were fixed based on idealized coordinates and refined with values of Uiso set to 1.2 times that of the carrier atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.2719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4736 _refine_ls_number_parameters 244 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.024 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.68186(2) 0.865763(19) 0.49489(2) 0.01249(7) Uani 1 1 d . . . Cu2 Cu 1.5000 1.0000 1.0000 0.00987(8) Uani 1 2 d S . . S1 S 1.38017(4) 0.92323(4) 0.71439(4) 0.01154(9) Uani 1 1 d . . . N1 N 1.32306(15) 0.99624(13) 1.00573(14) 0.0115(3) Uani 1 1 d . . . O1W O 0.70366(14) 0.75937(14) 0.37733(14) 0.0205(3) Uani 1 1 d D . . H1A H 0.6271(18) 0.731(3) 0.328(2) 0.031 Uiso 1 1 d D . . H1B H 0.765(2) 0.757(3) 0.343(2) 0.031 Uiso 1 1 d D . . O2W O 0.65072(14) 0.95708(12) 0.62065(13) 0.0164(3) Uani 1 1 d D . . H2A H 0.608(3) 0.9101(19) 0.655(2) 0.025 Uiso 1 1 d D . . H2B H 0.603(3) 1.0232(17) 0.599(3) 0.025 Uiso 1 1 d D . . O3 O 0.86627(14) 0.86743(13) 0.57383(13) 0.0171(3) Uani 1 1 d . . . O4 O 0.82478(14) 0.77433(13) 0.71737(14) 0.0188(3) Uani 1 1 d . . . O5 O 1.49230(13) 0.65387(11) 0.91923(13) 0.0145(3) Uani 1 1 d . . . O6 O 1.51371(13) 0.82814(11) 0.98913(12) 0.0136(2) Uani 1 1 d . . . O7 O 1.42411(14) 1.01377(12) 0.80019(12) 0.0151(3) Uani 1 1 d . . . O8 O 1.48285(14) 0.84355(13) 0.71709(14) 0.0186(3) Uani 1 1 d . . . O9 O 1.31193(14) 0.96651(12) 0.59758(12) 0.0163(3) Uani 1 1 d . . . C1 C 0.90032(18) 0.81713(16) 0.67288(17) 0.0147(3) Uani 1 1 d . . . C2 C 1.04385(17) 0.80515(16) 0.73569(17) 0.0132(3) Uani 1 1 d . . . C3 C 1.08590(18) 0.73539(17) 0.83404(17) 0.0155(3) Uani 1 1 d . . . H3 H 1.0245 0.7002 0.8622 0.019 Uiso 1 1 calc R . . C4 C 1.13440(18) 0.85870(15) 0.69621(17) 0.0132(3) Uani 1 1 d . . . H4 H 1.1068 0.9051 0.6283 0.016 Uiso 1 1 calc R . . C5 C 1.21637(18) 0.71682(17) 0.89115(17) 0.0148(3) Uani 1 1 d . . . H5 H 1.2436 0.6664 0.9559 0.018 Uiso 1 1 calc R . . C6 C 1.26568(17) 0.84384(15) 0.75682(16) 0.0116(3) Uani 1 1 d . . . C7 C 1.30790(17) 0.77169(15) 0.85411(16) 0.0118(3) Uani 1 1 d . . . C8 C 1.44803(16) 0.75250(15) 0.92556(16) 0.0112(3) Uani 1 1 d . . . C9 C 1.23126(18) 1.05273(17) 0.92261(18) 0.0156(3) Uani 1 1 d . . . H9 H 1.2547 1.0935 0.8653 0.019 Uiso 1 1 calc R . . C10 C 1.28955(18) 0.94270(19) 1.08869(18) 0.0188(4) Uani 1 1 d . . . H10 H 1.3538 0.9026 1.1482 0.023 Uiso 1 1 calc R . . C11 C 1.16497(19) 0.9439(2) 1.09053(19) 0.0211(4) Uani 1 1 d . . . H11 H 1.1450 0.9068 1.1518 0.025 Uiso 1 1 calc R . . C12 C 1.10408(18) 1.05388(17) 0.91706(18) 0.0166(4) Uani 1 1 d . . . H12 H 1.0411 1.0920 0.8547 0.020 Uiso 1 1 calc R . . C13 C 1.06840(17) 0.99959(16) 1.00214(17) 0.0133(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00751(11) 0.01421(12) 0.01472(12) 0.00041(7) 0.00239(9) 0.00009(7) Cu2 0.00531(14) 0.01123(14) 0.01344(15) -0.00076(10) 0.00367(11) -0.00032(10) S1 0.00932(18) 0.01355(19) 0.01163(19) 0.00102(14) 0.00339(15) -0.00061(14) N1 0.0073(6) 0.0124(7) 0.0150(7) -0.0011(5) 0.0043(5) -0.0005(5) O1W 0.0133(6) 0.0269(8) 0.0229(7) -0.0074(6) 0.0081(6) -0.0036(6) O2W 0.0144(6) 0.0162(6) 0.0187(7) 0.0019(5) 0.0060(5) 0.0034(5) O3 0.0091(6) 0.0237(7) 0.0165(6) 0.0031(5) 0.0017(5) 0.0008(5) O4 0.0100(6) 0.0225(7) 0.0241(7) 0.0038(6) 0.0058(5) 0.0006(5) O5 0.0089(6) 0.0125(6) 0.0200(7) 0.0003(5) 0.0022(5) 0.0011(5) O6 0.0094(6) 0.0132(6) 0.0165(6) -0.0005(5) 0.0021(5) -0.0003(5) O7 0.0131(6) 0.0181(6) 0.0134(6) -0.0027(5) 0.0037(5) -0.0045(5) O8 0.0150(6) 0.0201(7) 0.0246(7) 0.0044(6) 0.0116(6) 0.0045(5) O9 0.0181(6) 0.0168(6) 0.0117(6) 0.0013(5) 0.0020(5) -0.0037(5) C1 0.0098(7) 0.0145(8) 0.0177(8) -0.0010(6) 0.0021(6) 0.0011(6) C2 0.0077(7) 0.0146(8) 0.0159(8) -0.0007(6) 0.0023(6) 0.0002(6) C3 0.0106(8) 0.0179(8) 0.0172(8) 0.0021(7) 0.0035(6) -0.0009(6) C4 0.0094(8) 0.0144(8) 0.0141(8) 0.0010(6) 0.0017(6) 0.0008(6) C5 0.0106(8) 0.0168(8) 0.0158(8) 0.0033(6) 0.0031(6) -0.0006(6) C6 0.0091(7) 0.0121(7) 0.0131(8) -0.0008(6) 0.0032(6) -0.0012(6) C7 0.0077(7) 0.0134(7) 0.0134(7) -0.0004(6) 0.0025(6) 0.0003(6) C8 0.0071(7) 0.0133(7) 0.0126(7) 0.0022(6) 0.0025(6) 0.0001(6) C9 0.0101(8) 0.0181(8) 0.0199(9) 0.0049(7) 0.0067(7) 0.0019(6) C10 0.0085(8) 0.0277(10) 0.0197(9) 0.0074(7) 0.0041(7) 0.0003(7) C11 0.0091(8) 0.0345(11) 0.0208(9) 0.0086(8) 0.0063(7) 0.0005(8) C12 0.0086(7) 0.0203(9) 0.0214(9) 0.0058(7) 0.0059(7) 0.0021(7) C13 0.0074(7) 0.0163(8) 0.0166(8) -0.0001(6) 0.0046(6) -0.0005(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 O3 1.9321(17) . ? Cu1 O1W 1.9758(16) . ? Cu1 O2W 1.9909(16) . ? Cu1 O5 1.9914(16) 4_475 ? Cu1 O9 2.2895(16) 3_776 ? Cu2 N1 1.9744(18) 3_877 ? Cu2 N1 1.9744(18) . ? Cu2 O6 2.0435(16) . ? Cu2 O6 2.0435(16) 3_877 ? Cu2 O7 2.2886(17) . ? Cu2 O7 2.2886(17) 3_877 ? S1 O9 1.4552(15) . ? S1 O7 1.4570(15) . ? S1 O8 1.4636(16) . ? S1 C6 1.7815(19) . ? N1 C9 1.341(2) . ? N1 C10 1.342(2) . ? O1W H1A 0.920(17) . ? O1W H1B 0.912(17) . ? O2W H2A 0.917(16) . ? O2W H2B 0.932(16) . ? O3 C1 1.278(2) . ? O4 C1 1.242(2) . ? O5 C8 1.275(2) . ? O5 Cu1 1.9914(16) 4_676 ? O6 C8 1.241(2) . ? O9 Cu1 2.2895(16) 3_776 ? C1 C2 1.513(3) . ? C2 C3 1.395(3) . ? C2 C4 1.395(3) . ? C3 C5 1.387(3) . ? C3 H3 0.9500 . ? C4 C6 1.395(3) . ? C4 H4 0.9500 . ? C5 C7 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.402(3) . ? C7 C8 1.511(2) . ? C9 C12 1.380(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C13 1.395(3) . ? C11 H11 0.9500 . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C13 1.491(4) 3_777 ? 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 O3 Cu1 O1W 90.06(7) . . ? O3 Cu1 O2W 92.21(7) . . ? O1W Cu1 O2W 172.98(6) . . ? O3 Cu1 O5 173.60(6) . 4_475 ? O1W Cu1 O5 87.53(6) . 4_475 ? O2W Cu1 O5 89.52(6) . 4_475 ? O3 Cu1 O9 91.95(6) . 3_776 ? O1W Cu1 O9 99.54(7) . 3_776 ? O2W Cu1 O9 87.02(6) . 3_776 ? O5 Cu1 O9 94.29(6) 4_475 3_776 ? N1 Cu2 N1 180.000(1) 3_877 . ? N1 Cu2 O6 85.69(6) 3_877 . ? N1 Cu2 O6 94.32(6) . . ? N1 Cu2 O6 94.31(6) 3_877 3_877 ? N1 Cu2 O6 85.68(6) . 3_877 ? O6 Cu2 O6 180.000(1) . 3_877 ? N1 Cu2 O7 88.48(6) 3_877 . ? N1 Cu2 O7 91.52(6) . . ? O6 Cu2 O7 90.62(5) . . ? O6 Cu2 O7 89.38(5) 3_877 . ? N1 Cu2 O7 91.52(6) 3_877 3_877 ? N1 Cu2 O7 88.48(6) . 3_877 ? O6 Cu2 O7 89.38(5) . 3_877 ? O6 Cu2 O7 90.62(5) 3_877 3_877 ? O7 Cu2 O7 180.000(1) . 3_877 ? O9 S1 O7 112.10(9) . . ? O9 S1 O8 112.92(9) . . ? O7 S1 O8 112.84(9) . . ? O9 S1 C6 106.44(9) . . ? O7 S1 C6 106.08(9) . . ? O8 S1 C6 105.79(9) . . ? C9 N1 C10 118.07(16) . . ? C9 N1 Cu2 117.75(13) . . ? C10 N1 Cu2 124.17(13) . . ? Cu1 O1W H1A 113.5(18) . . ? Cu1 O1W H1B 130.1(19) . . ? H1A O1W H1B 110(2) . . ? Cu1 O2W H2A 105.8(18) . . ? Cu1 O2W H2B 117.6(18) . . ? H2A O2W H2B 108(2) . . ? C1 O3 Cu1 112.81(13) . . ? C8 O5 Cu1 116.20(12) . 4_676 ? C8 O6 Cu2 135.65(12) . . ? S1 O7 Cu2 128.29(9) . . ? S1 O9 Cu1 133.68(9) . 3_776 ? O4 C1 O3 124.79(18) . . ? O4 C1 C2 118.86(17) . . ? O3 C1 C2 116.28(17) . . ? C3 C2 C4 119.47(17) . . ? C3 C2 C1 118.40(17) . . ? C4 C2 C1 122.10(17) . . ? C5 C3 C2 120.70(18) . . ? C5 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C6 C4 C2 119.74(17) . . ? C6 C4 H4 120.1 . . ? C2 C4 H4 120.1 . . ? C3 C5 C7 120.38(18) . . ? C3 C5 H5 119.8 . . ? C7 C5 H5 119.8 . . ? C4 C6 C7 120.74(17) . . ? C4 C6 S1 119.38(14) . . ? C7 C6 S1 119.81(14) . . ? C5 C7 C6 118.90(17) . . ? C5 C7 C8 117.07(16) . . ? C6 C7 C8 123.99(16) . . ? O6 C8 O5 122.72(17) . . ? O6 C8 C7 121.15(16) . . ? O5 C8 C7 116.10(16) . . ? N1 C9 C12 122.52(18) . . ? N1 C9 H9 118.7 . . ? C12 C9 H9 118.7 . . ? N1 C10 C11 122.27(18) . . ? N1 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C13 119.81(19) . . ? C10 C11 H11 120.1 . . ? C13 C11 H11 120.1 . . ? C9 C12 C13 119.96(18) . . ? C9 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C11 117.30(17) . . ? C12 C13 C13 120.7(2) . 3_777 ? C11 C13 C13 122.0(2) . 3_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu2 N1 C9 55(100) 3_877 . . . ? O6 Cu2 N1 C9 -121.75(15) . . . . ? O6 Cu2 N1 C9 58.25(15) 3_877 . . . ? O7 Cu2 N1 C9 -31.01(15) . . . . ? O7 Cu2 N1 C9 148.99(15) 3_877 . . . ? N1 Cu2 N1 C10 -124(100) 3_877 . . . ? O6 Cu2 N1 C10 59.62(17) . . . . ? O6 Cu2 N1 C10 -120.38(17) 3_877 . . . ? O7 Cu2 N1 C10 150.36(17) . . . . ? O7 Cu2 N1 C10 -29.64(17) 3_877 . . . ? O1W Cu1 O3 C1 -109.92(14) . . . . ? O2W Cu1 O3 C1 63.44(14) . . . . ? O5 Cu1 O3 C1 -42.2(6) 4_475 . . . ? O9 Cu1 O3 C1 150.53(14) 3_776 . . . ? N1 Cu2 O6 C8 -127.43(19) 3_877 . . . ? N1 Cu2 O6 C8 52.57(19) . . . . ? O6 Cu2 O6 C8 144(100) 3_877 . . . ? O7 Cu2 O6 C8 -39.00(18) . . . . ? O7 Cu2 O6 C8 141.00(18) 3_877 . . . ? O9 S1 O7 Cu2 166.85(9) . . . . ? O8 S1 O7 Cu2 -64.32(12) . . . . ? C6 S1 O7 Cu2 51.07(12) . . . . ? N1 Cu2 O7 S1 97.46(11) 3_877 . . . ? N1 Cu2 O7 S1 -82.54(11) . . . . ? O6 Cu2 O7 S1 11.80(11) . . . . ? O6 Cu2 O7 S1 -168.20(11) 3_877 . . . ? O7 Cu2 O7 S1 141(100) 3_877 . . . ? O7 S1 O9 Cu1 25.94(15) . . . 3_776 ? O8 S1 O9 Cu1 -102.85(13) . . . 3_776 ? C6 S1 O9 Cu1 141.51(11) . . . 3_776 ? Cu1 O3 C1 O4 -2.2(3) . . . . ? Cu1 O3 C1 C2 174.64(12) . . . . ? O4 C1 C2 C3 7.4(3) . . . . ? O3 C1 C2 C3 -169.71(18) . . . . ? O4 C1 C2 C4 -174.62(18) . . . . ? O3 C1 C2 C4 8.3(3) . . . . ? C4 C2 C3 C5 -1.5(3) . . . . ? C1 C2 C3 C5 176.61(18) . . . . ? C3 C2 C4 C6 -1.3(3) . . . . ? C1 C2 C4 C6 -179.35(17) . . . . ? C2 C3 C5 C7 2.8(3) . . . . ? C2 C4 C6 C7 2.8(3) . . . . ? C2 C4 C6 S1 -173.91(14) . . . . ? O9 S1 C6 C4 -16.86(17) . . . . ? O7 S1 C6 C4 102.70(16) . . . . ? O8 S1 C6 C4 -137.21(15) . . . . ? O9 S1 C6 C7 166.39(15) . . . . ? O7 S1 C6 C7 -74.05(17) . . . . ? O8 S1 C6 C7 46.04(17) . . . . ? C3 C5 C7 C6 -1.4(3) . . . . ? C3 C5 C7 C8 176.31(17) . . . . ? C4 C6 C7 C5 -1.5(3) . . . . ? S1 C6 C7 C5 175.25(14) . . . . ? C4 C6 C7 C8 -178.95(17) . . . . ? S1 C6 C7 C8 -2.2(3) . . . . ? Cu2 O6 C8 O5 163.24(13) . . . . ? Cu2 O6 C8 C7 -19.1(3) . . . . ? Cu1 O5 C8 O6 -10.5(2) 4_676 . . . ? Cu1 O5 C8 C7 171.76(12) 4_676 . . . ? C5 C7 C8 O6 -107.7(2) . . . . ? C6 C7 C8 O6 69.8(3) . . . . ? C5 C7 C8 O5 70.1(2) . . . . ? C6 C7 C8 O5 -112.4(2) . . . . ? C10 N1 C9 C12 -2.6(3) . . . . ? Cu2 N1 C9 C12 178.71(16) . . . . ? C9 N1 C10 C11 0.2(3) . . . . ? Cu2 N1 C10 C11 178.84(17) . . . . ? N1 C10 C11 C13 1.8(4) . . . . ? N1 C9 C12 C13 2.9(3) . . . . ? C9 C12 C13 C11 -0.8(3) . . . . ? C9 C12 C13 C13 179.7(2) . . . 3_777 ? C10 C11 C13 C12 -1.4(3) . . . . ? C10 C11 C13 C13 178.1(2) . . . 3_777 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 34.65 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.625 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 941460' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mor21 # start Validation Reply Form _vrf_PLAT201_mor21 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 26 Why ? RESPONSE: Refining all non-hydrongen atoms anisotropically gave a data/parameter ratio of approximately 6. This is too low to give satisfactory refinement. This may be because of the difficulty of the data collection at high temperature and the atoms would have a large thermal motion as well. Refining all carbon atoms isotropically extended this ratio out to approximately 8.7, which is more suitable. ; _vrf_PLAT213_mor21 ; PROBLEM: Atom N1 has ADP max/min Ratio ..... 4.5 oblate RESPONSE: Single crystal data collected at high temperature leads to the poor crystal quality and large thermal motion. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'dehydrated compound 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H14.50 Cu3 N2 O14.25 S2' _chemical_formula_weight 837.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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' Cu Cu 0.2862 1.4771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1434 0.1473 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.075(5) _cell_length_b 12.806(5) _cell_length_c 19.502(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 95.342(5) _cell_angle_gamma 90.000(5) _cell_volume 2505.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 500(2) _cell_measurement_reflns_used 2610 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 22.79 _exptl_crystal_description Chip _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1670 _exptl_absorpt_coefficient_mu 3.411 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Bruker SADABS ; _exptl_special_details ; Data of dehydrated compound were collected at 500 K. Variation in crystal temperature was achieved via the cryostream with a ramp rate of 360K/h. ; _diffrn_ambient_temperature 500(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source '11.3.1 ALS, LBNL. CA' _diffrn_radiation_monochromator 'Si(111) Crystal' _diffrn_measurement_device_type 'Bruker AXS APEXII' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23264 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_unetI/netI 0.0454 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 22.79 _reflns_number_total 2610 _reflns_number_gt 1836 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEXII (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All carbon atoms were refined isotropically for a satisfactory refinement at high temperature. Other non-hydrogen atoms of the dehydrated structure were refined anisotropically. Hydrogen atoms were fixed based on idealized coordinates and refined with values of Uiso set to 1.2 times that of the carrier atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+22.9504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2610 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1854 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8223(12) 0.6357(10) 0.6304(7) 0.039(3) Uiso 1 1 d . . . C2 C 0.8199(14) 0.6278(11) 0.7002(8) 0.052(4) Uiso 1 1 d . . . H2 H 0.7501 0.5933 0.7186 0.062 Uiso 1 1 calc R . . C3 C 0.9176(14) 0.6696(12) 0.7416(8) 0.053(4) Uiso 1 1 d . . . C4 C 1.0132(17) 0.7192(13) 0.7160(9) 0.068(5) Uiso 1 1 d . . . H4 H 1.0834 0.7459 0.7451 0.082 Uiso 1 1 calc R . . C5 C 1.0122(15) 0.7324(12) 0.6479(8) 0.060(4) Uiso 1 1 d . . . H5 H 1.0792 0.7710 0.6300 0.072 Uiso 1 1 calc R . . C6 C 0.9145(13) 0.6898(10) 0.6055(7) 0.043(3) Uiso 1 1 d . . . C7 C 0.9301(12) 0.7125(11) 0.5318(7) 0.034(3) Uiso 1 1 d . . . C9 C 1.2825(12) 0.6318(10) 1.1050(7) 0.038(3) Uiso 1 1 d . . . C10 C 1.2680(13) 0.6198(10) 1.1699(7) 0.043(3) Uiso 1 1 d . . . H10 H 1.2018 0.5759 1.1835 0.052 Uiso 1 1 calc R . . C11 C 1.3489(13) 0.6712(10) 1.2177(7) 0.043(3) Uiso 1 1 d . . . C12 C 1.4403(15) 0.7331(12) 1.1979(8) 0.056(4) Uiso 1 1 d . . . H12 H 1.4974 0.7675 1.2307 0.067 Uiso 1 1 calc R . . C13 C 1.4534(14) 0.7481(11) 1.1306(7) 0.052(4) Uiso 1 1 d . . . H13 H 1.5176 0.7938 1.1169 0.063 Uiso 1 1 calc R . . C14 C 1.3728(12) 0.6962(10) 1.0831(7) 0.040(3) Uiso 1 1 d . . . C15 C 1.3932(13) 0.7163(11) 1.0100(7) 0.036(3) Uiso 1 1 d . . . C16 C 1.3335(15) 0.6652(11) 1.2902(8) 0.048(4) Uiso 1 1 d . . . C17 C 1.0485(15) 0.4553(11) 0.6383(8) 0.053(4) Uiso 1 1 d . . . H17 H 0.9607 0.4322 0.6317 0.063 Uiso 1 1 calc R . . C18 C 1.2228(17) 0.5253(13) 0.5974(9) 0.062(4) Uiso 1 1 d . . . H18 H 1.2629 0.5558 0.5613 0.075 Uiso 1 1 calc R . . C19 C 1.1129(14) 0.4459(11) 0.7002(8) 0.055(4) Uiso 1 1 d . . . H19 H 1.0698 0.4167 0.7358 0.066 Uiso 1 1 calc R . . C20 C 1.2959(17) 0.5147(12) 0.6598(8) 0.064(4) Uiso 1 1 d . . . H20 H 1.3854 0.5337 0.6648 0.076 Uiso 1 1 calc R . . C21 C 1.2392(13) 0.4778(11) 0.7123(7) 0.045(4) Uiso 1 1 d . . . C22 C 1.3073(13) 0.4755(10) 0.7790(7) 0.043(3) Uiso 1 1 d . . . C23 C 1.4157(15) 0.5335(12) 0.7957(8) 0.056(4) Uiso 1 1 d . . . H23 H 1.4521 0.5726 0.7619 0.067 Uiso 1 1 calc R . . C24 C 1.2654(15) 0.4171(12) 0.8287(8) 0.057(4) Uiso 1 1 d . . . H24 H 1.1925 0.3733 0.8187 0.068 Uiso 1 1 calc R . . C25 C 1.4714(14) 0.5358(11) 0.8591(8) 0.050(4) Uiso 1 1 d . . . H25 H 1.5448 0.5789 0.8694 0.060 Uiso 1 1 calc R . . C26 C 1.3260(14) 0.4196(11) 0.8938(8) 0.050(4) Uiso 1 1 d . . . H26 H 1.2944 0.3781 0.9278 0.060 Uiso 1 1 calc R . . Cu1 Cu 0.68462(19) 0.35621(15) 0.59709(8) 0.0549(6) Uani 1 1 d . . . Cu2 Cu 0.9773(2) 0.64937(16) 0.93583(9) 0.0603(7) Uani 1 1 d . . . Cu3 Cu 1.0000 0.5000 0.5000 0.0492(8) Uani 1 2 d S . . Cu4 Cu 1.5000 0.5000 1.0000 0.0435(7) Uani 1 2 d S . . N1 N 1.1016(13) 0.4950(9) 0.5866(5) 0.050(3) Uani 1 1 d . . . N2 N 1.4284(12) 0.4803(8) 0.9085(5) 0.042(3) Uani 1 1 d . . . O1 O 0.7743(9) 0.4756(7) 0.5590(4) 0.047(2) Uani 1 1 d . . . O2 O 0.6766(11) 0.6347(9) 0.5201(6) 0.072(3) Uani 1 1 d . . . O3 O 0.6012(11) 0.5407(9) 0.6140(6) 0.071(3) Uani 1 1 d . . . O4 O 0.9816(9) 0.6500(7) 0.4980(4) 0.045(2) Uani 1 1 d . . . O5 O 0.9038(10) 0.8000(7) 0.5131(4) 0.054(3) Uani 1 1 d . . . O8 O 1.1512(10) 0.6217(8) 0.9882(5) 0.060(3) Uani 1 1 d . . . O9 O 0.9145(10) 0.4859(8) 0.9248(5) 0.057(3) Uani 1 1 d . . . O10 O 1.2806(11) 0.4788(8) 1.0278(5) 0.058(3) Uani 1 1 d . . . O11 O 1.4558(9) 0.6525(7) 0.9821(4) 0.047(2) Uani 1 1 d . . . O12 O 1.3537(10) 0.7987(7) 0.9884(4) 0.051(3) Uani 1 1 d . . . O13 O 1.2404(10) 0.6183(8) 1.3089(5) 0.061(3) Uani 1 1 d . . . O14 O 1.4071(12) 0.7081(9) 1.3327(4) 0.074(3) Uani 1 1 d . . . S1 S 0.7057(4) 0.5693(3) 0.5766(2) 0.0505(10) Uani 1 1 d . . . S2 S 1.1907(4) 0.5548(3) 1.04403(18) 0.0484(10) Uani 1 1 d . . . O6 O 0.8363(15) 0.6689(12) 0.8468(6) 0.107(5) Uani 1 1 d . . . O7 O 1.0409(14) 0.6540(11) 0.8483(5) 0.093(4) Uani 1 1 d . . . C8 C 0.9271(19) 0.6629(14) 0.8192(10) 0.066(5) Uiso 1 1 d . . . O1W O 0.831(2) 0.6617(19) 0.9242(13) 0.028(6) Uiso 0.30 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 Cu1 0.0797(14) 0.0619(13) 0.0218(11) -0.0020(8) -0.0011(9) -0.0119(10) Cu2 0.0867(15) 0.0696(13) 0.0220(11) -0.0010(9) -0.0082(9) -0.0016(11) Cu3 0.0800(19) 0.0454(15) 0.0171(13) -0.0018(11) -0.0218(12) 0.0057(13) Cu4 0.0661(17) 0.0478(15) 0.0129(13) -0.0022(10) -0.0164(11) 0.0053(12) N1 0.088(10) 0.052(7) 0.008(6) 0.012(5) -0.006(6) -0.003(7) N2 0.066(8) 0.048(7) 0.011(6) 0.004(5) -0.008(5) 0.005(6) O1 0.057(6) 0.049(6) 0.034(5) -0.011(4) -0.006(4) -0.005(5) O2 0.072(7) 0.069(7) 0.071(8) 0.008(6) -0.022(6) 0.003(6) O3 0.062(7) 0.067(7) 0.085(9) 0.001(6) 0.004(6) 0.003(6) O4 0.078(7) 0.038(5) 0.017(5) 0.000(4) -0.003(4) 0.002(5) O5 0.085(7) 0.043(6) 0.032(6) 0.003(5) 0.004(5) 0.012(5) O8 0.074(7) 0.074(7) 0.028(6) 0.012(5) -0.013(5) -0.012(6) O9 0.063(7) 0.070(7) 0.035(6) 0.006(5) -0.007(5) -0.008(5) O10 0.076(7) 0.052(6) 0.044(6) -0.010(5) -0.006(5) 0.002(6) O11 0.071(6) 0.048(6) 0.020(5) 0.005(4) -0.001(4) 0.008(5) O12 0.082(7) 0.042(6) 0.027(5) 0.009(4) -0.003(5) 0.014(5) O13 0.075(7) 0.084(8) 0.022(5) 0.005(5) -0.004(5) -0.005(6) O14 0.108(9) 0.098(9) 0.014(5) -0.010(5) -0.009(5) -0.040(7) S1 0.054(2) 0.051(2) 0.044(2) 0.004(2) -0.0058(19) 0.0028(19) S2 0.063(3) 0.054(2) 0.025(2) -0.0002(18) -0.0110(18) -0.008(2) O6 0.144(13) 0.135(12) 0.047(8) 0.024(8) 0.036(8) 0.052(10) O7 0.113(10) 0.139(12) 0.026(6) 0.014(7) -0.001(6) -0.013(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C6 1.289(17) . ? C1 C2 1.37(2) . ? C1 S1 1.725(14) . ? C2 C3 1.33(2) . ? C3 C4 1.29(2) . ? C3 C8 1.51(2) . ? C4 C5 1.34(2) . ? C5 C6 1.34(2) . ? C6 C7 1.489(19) . ? C7 O4 1.187(15) . ? C7 O5 1.201(15) . ? C9 C10 1.296(18) . ? C9 C14 1.327(17) . ? C9 S2 1.743(13) . ? C10 C11 1.352(19) . ? C11 C12 1.301(19) . ? C11 C16 1.44(2) . ? C12 C13 1.346(19) . ? C13 C14 1.348(19) . ? C14 C15 1.483(18) . ? C15 O12 1.190(15) . ? C15 O11 1.193(15) . ? C16 O14 1.194(17) . ? C16 O13 1.199(16) . ? C16 Cu1 2.240(16) 3_767 ? C17 N1 1.290(18) . ? C17 C19 1.32(2) . ? C18 N1 1.279(19) . ? C18 C20 1.37(2) . ? C19 C21 1.337(19) . ? C20 C21 1.31(2) . ? C21 C22 1.41(2) . ? C22 C24 1.323(19) . ? C22 C23 1.336(19) . ? C23 C25 1.31(2) . ? C24 C26 1.36(2) . ? C25 N2 1.302(18) . ? C26 N2 1.302(18) . ? Cu1 O12 1.831(8) 2_746 ? Cu1 O14 1.908(10) 3_767 ? Cu1 O13 1.944(9) 3_767 ? Cu1 O1 1.958(9) . ? Cu1 C16 2.240(16) 3_767 ? Cu1 S1 2.769(4) . ? Cu2 O1W 1.48(2) . ? Cu2 O5 1.857(9) 4_576 ? Cu2 O7 1.879(11) . ? Cu2 O8 1.977(10) . ? Cu2 O6 2.153(14) . ? Cu2 O9 2.192(10) . ? Cu2 C8 2.290(19) . ? Cu3 N1 1.892(10) 3_766 ? Cu3 N1 1.892(10) . ? Cu3 O4 1.930(9) 3_766 ? Cu3 O4 1.930(9) . ? Cu4 N2 1.879(10) 3_867 ? Cu4 N2 1.879(10) . ? Cu4 O11 2.027(9) 3_867 ? Cu4 O11 2.027(9) . ? Cu4 O10 2.340(11) . ? Cu4 O10 2.340(11) 3_867 ? O1 S1 1.442(10) . ? O2 S1 1.392(12) . ? O3 S1 1.385(12) . ? O5 Cu2 1.857(9) 4_575 ? O8 S2 1.413(10) . ? O9 S2 1.372(10) 3_767 ? O10 S2 1.386(11) . ? O12 Cu1 1.831(8) 2_756 ? O13 Cu1 1.944(9) 3_767 ? O14 Cu1 1.908(10) 3_767 ? S2 O9 1.372(11) 3_767 ? O6 C8 1.107(19) . ? O6 O1W 1.52(3) . ? O7 C8 1.24(2) . ? 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 C6 C1 C2 119.6(13) . . ? C6 C1 S1 120.6(11) . . ? C2 C1 S1 119.7(10) . . ? C3 C2 C1 119.7(14) . . ? C4 C3 C2 120.1(16) . . ? C4 C3 C8 115.8(15) . . ? C2 C3 C8 124.1(14) . . ? C3 C4 C5 120.6(17) . . ? C4 C5 C6 119.8(15) . . ? C1 C6 C5 120.0(14) . . ? C1 C6 C7 127.8(13) . . ? C5 C6 C7 112.2(12) . . ? O4 C7 O5 123.8(13) . . ? O4 C7 C6 119.8(12) . . ? O5 C7 C6 115.8(12) . . ? C10 C9 C14 122.1(13) . . ? C10 C9 S2 119.9(11) . . ? C14 C9 S2 117.9(11) . . ? C9 C10 C11 120.0(13) . . ? C12 C11 C10 119.3(14) . . ? C12 C11 C16 117.9(14) . . ? C10 C11 C16 122.6(13) . . ? C11 C12 C13 120.9(15) . . ? C12 C13 C14 119.5(14) . . ? C9 C14 C13 118.2(13) . . ? C9 C14 C15 125.3(12) . . ? C13 C14 C15 116.5(12) . . ? O12 C15 O11 128.2(13) . . ? O12 C15 C14 115.0(12) . . ? O11 C15 C14 116.4(12) . . ? O14 C16 O13 118.1(15) . . ? O14 C16 C11 122.8(14) . . ? O13 C16 C11 119.1(14) . . ? O14 C16 Cu1 58.4(8) . 3_767 ? O13 C16 Cu1 60.1(8) . 3_767 ? C11 C16 Cu1 175.7(11) . 3_767 ? N1 C17 C19 123.1(15) . . ? N1 C18 C20 122.9(16) . . ? C17 C19 C21 120.8(15) . . ? C21 C20 C18 119.6(16) . . ? C20 C21 C19 116.8(15) . . ? C20 C21 C22 121.3(14) . . ? C19 C21 C22 121.9(13) . . ? C24 C22 C23 116.4(14) . . ? C24 C22 C21 121.7(13) . . ? C23 C22 C21 121.9(13) . . ? C25 C23 C22 120.7(15) . . ? C22 C24 C26 121.7(15) . . ? N2 C25 C23 122.9(14) . . ? N2 C26 C24 119.9(14) . . ? O12 Cu1 O14 113.8(4) 2_746 3_767 ? O12 Cu1 O13 163.1(5) 2_746 3_767 ? O14 Cu1 O13 64.4(4) 3_767 3_767 ? O12 Cu1 O1 92.0(4) 2_746 . ? O14 Cu1 O1 151.8(4) 3_767 . ? O13 Cu1 O1 94.2(4) 3_767 . ? O12 Cu1 C16 144.6(5) 2_746 3_767 ? O14 Cu1 C16 32.2(5) 3_767 3_767 ? O13 Cu1 C16 32.3(4) 3_767 3_767 ? O1 Cu1 C16 123.4(5) . 3_767 ? O12 Cu1 S1 106.1(3) 2_746 . ? O14 Cu1 S1 125.3(4) 3_767 . ? O13 Cu1 S1 86.7(3) 3_767 . ? O1 Cu1 S1 29.7(3) . . ? C16 Cu1 S1 106.1(4) 3_767 . ? O1W Cu2 O5 67.7(10) . 4_576 ? O1W Cu2 O7 106.1(11) . . ? O5 Cu2 O7 157.2(5) 4_576 . ? O1W Cu2 O8 157.1(10) . . ? O5 Cu2 O8 92.5(4) 4_576 . ? O7 Cu2 O8 96.6(5) . . ? O1W Cu2 O6 44.8(10) . . ? O5 Cu2 O6 109.3(5) 4_576 . ? O7 Cu2 O6 61.3(5) . . ? O8 Cu2 O6 157.6(5) . . ? O1W Cu2 O9 79.2(10) . . ? O5 Cu2 O9 106.2(4) 4_576 . ? O7 Cu2 O9 93.5(5) . . ? O8 Cu2 O9 96.5(4) . . ? O6 Cu2 O9 82.5(5) . . ? O1W Cu2 C8 73.5(11) . . ? O5 Cu2 C8 135.4(6) 4_576 . ? O7 Cu2 C8 32.6(6) . . ? O8 Cu2 C8 129.0(6) . . ? O6 Cu2 C8 28.7(5) . . ? O9 Cu2 C8 86.6(5) . . ? N1 Cu3 N1 180.000(3) 3_766 . ? N1 Cu3 O4 95.4(4) 3_766 3_766 ? N1 Cu3 O4 84.6(4) . 3_766 ? N1 Cu3 O4 84.6(4) 3_766 . ? N1 Cu3 O4 95.4(4) . . ? O4 Cu3 O4 180.000(2) 3_766 . ? N2 Cu4 N2 180.000(4) 3_867 . ? N2 Cu4 O11 84.7(4) 3_867 3_867 ? N2 Cu4 O11 95.3(4) . 3_867 ? N2 Cu4 O11 95.3(4) 3_867 . ? N2 Cu4 O11 84.7(4) . . ? O11 Cu4 O11 180.0(5) 3_867 . ? N2 Cu4 O10 94.8(4) 3_867 . ? N2 Cu4 O10 85.2(4) . . ? O11 Cu4 O10 92.6(4) 3_867 . ? O11 Cu4 O10 87.4(4) . . ? N2 Cu4 O10 85.2(4) 3_867 3_867 ? N2 Cu4 O10 94.8(4) . 3_867 ? O11 Cu4 O10 87.4(4) 3_867 3_867 ? O11 Cu4 O10 92.6(4) . 3_867 ? O10 Cu4 O10 180.000(1) . 3_867 ? C18 N1 C17 116.7(13) . . ? C18 N1 Cu3 124.5(10) . . ? C17 N1 Cu3 118.8(11) . . ? C26 N2 C25 118.3(12) . . ? C26 N2 Cu4 121.0(9) . . ? C25 N2 Cu4 120.2(10) . . ? S1 O1 Cu1 108.1(5) . . ? C7 O4 Cu3 134.9(9) . . ? C7 O5 Cu2 118.6(9) . 4_575 ? S2 O8 Cu2 132.8(6) . . ? S2 O9 Cu2 123.1(6) 3_767 . ? S2 O10 Cu4 128.5(6) . . ? C15 O11 Cu4 134.3(9) . . ? C15 O12 Cu1 135.6(9) . 2_756 ? C16 O13 Cu1 87.5(9) . 3_767 ? C16 O14 Cu1 89.4(10) . 3_767 ? O3 S1 O2 117.5(7) . . ? O3 S1 O1 108.0(6) . . ? O2 S1 O1 112.5(7) . . ? O3 S1 C1 108.5(7) . . ? O2 S1 C1 105.5(7) . . ? O1 S1 C1 103.9(6) . . ? O3 S1 Cu1 65.8(5) . . ? O2 S1 Cu1 133.9(5) . . ? O1 S1 Cu1 42.2(4) . . ? C1 S1 Cu1 117.0(5) . . ? O9 S2 O10 112.5(7) 3_767 . ? O9 S2 O8 113.4(6) 3_767 . ? O10 S2 O8 113.1(7) . . ? O9 S2 C9 107.2(6) 3_767 . ? O10 S2 C9 103.7(6) . . ? O8 S2 C9 106.0(6) . . ? C8 O6 O1W 125.9(19) . . ? C8 O6 Cu2 82.6(14) . . ? O1W O6 Cu2 43.3(10) . . ? C8 O7 Cu2 92.3(12) . . ? O6 C8 O7 124(2) . . ? O6 C8 C3 120.4(18) . . ? O7 C8 C3 115.8(16) . . ? O6 C8 Cu2 68.8(13) . . ? O7 C8 Cu2 55.0(9) . . ? C3 C8 Cu2 170.9(13) . . ? Cu2 O1W O6 91.8(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.79 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.866 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 941461'