Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Fabrice Pointillart' _publ_contact_author_address ; 263 Avenue du General Leclerc Rennes Cedex 35042 ; _publ_contact_author_email lahcene.ouahab@univ-rennes1.fr loop_ _publ_author_name F.Pointillart T.Cauchy 'Y.Le Gal' S.Golhen O.Cador L.Ouahab data_calcul _database_code_depnum_ccdc_archive 'CCDC 753763' #TrackingRef '- complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H20 Cu2 N8 O8 S8' _chemical_formula_weight 1076.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.231(3) _cell_length_b 12.153(3) _cell_length_c 27.846(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.300(10) _cell_angle_gamma 90.00 _cell_volume 4666.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 61438 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54489 _diffrn_reflns_av_R_equivalents 0.1499 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10627 _reflns_number_gt 5601 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare al, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.314 -0.157 0.116 213 46 ' ' 2 0.685 0.157 0.883 212 47 ' ' 3 0.686 0.343 0.384 212 47 ' ' 4 0.315 0.657 0.617 212 46 ' ' _platon_squeeze_details ; SQUEEZE procedure was used and revealed a total potential solvent area vol of 850.2 Ang^3^ corresponding to 18.2% of the unit cell vol. These solvent correspond to disordered CH2Cl2 solvent molecules used during crystallization process. ; _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^)+(0.0814P)^2^+0.0000P] 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 10627 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 C1 C 0.1785(3) 0.1553(4) 0.96393(17) 0.0539(11) Uani 1 1 d . . . H1 H 0.1144 0.1790 0.9565 0.065 Uiso 1 1 calc R . . C2 C 0.2343(4) 0.1669(4) 1.01039(18) 0.0662(13) Uani 1 1 d . . . H2 H 0.2097 0.1989 1.0351 0.079 Uiso 1 1 calc R . . C3 C 0.3295(4) 0.1297(5) 1.02051(18) 0.0745(15) Uani 1 1 d . . . H3 H 0.3688 0.1358 1.0525 0.089 Uiso 1 1 calc R . . C4 C 0.3661(3) 0.0841(4) 0.98390(17) 0.0613(13) Uani 1 1 d . . . H4 H 0.4299 0.0595 0.9911 0.074 Uiso 1 1 calc R . . C5 C 0.3075(3) 0.0745(3) 0.93563(15) 0.0432(10) Uani 1 1 d . . . C6 C 0.4239(3) 0.0014(3) 0.89542(16) 0.0477(10) Uani 1 1 d . . . C7 C 0.4341(3) -0.0937(3) 0.86352(16) 0.0445(10) Uani 1 1 d . . . C8 C 0.5102(3) -0.1101(4) 0.84567(19) 0.0609(13) Uani 1 1 d . . . H8 H 0.5602 -0.0588 0.8508 0.073 Uiso 1 1 calc R . . C9 C 0.4085(3) -0.2866(4) 0.82342(18) 0.0570(12) Uani 1 1 d . . . C10 C 0.3789(3) -0.3895(4) 0.81216(19) 0.0582(12) Uani 1 1 d . . . C11 C 0.3621(4) -0.5910(4) 0.7847(2) 0.0823(18) Uani 1 1 d . . . H11 H 0.3725 -0.6600 0.7726 0.099 Uiso 1 1 calc R . . C12 C 0.2857(3) -0.5728(3) 0.80260(16) 0.0495(11) Uani 1 1 d . . . C13 C 0.2090(3) -0.6571(4) 0.80228(18) 0.0531(11) Uani 1 1 d . . . C14 C 0.0638(3) -0.6786(3) 0.82770(15) 0.0437(10) Uani 1 1 d . . . C15 C 0.0043(3) -0.7232(3) 0.78341(18) 0.0532(11) Uani 1 1 d . . . H15 H 0.0298 -0.7355 0.7562 0.064 Uiso 1 1 calc R . . C16 C -0.0906(4) -0.7482(4) 0.7809(2) 0.0633(13) Uani 1 1 d . . . H16 H -0.1295 -0.7768 0.7518 0.076 Uiso 1 1 calc R . . C17 C -0.1287(4) -0.7317(4) 0.8208(2) 0.0713(14) Uani 1 1 d . . . H17 H -0.1935 -0.7479 0.8185 0.086 Uiso 1 1 calc R . . C18 C -0.0716(3) -0.6911(4) 0.8640(2) 0.0682(14) Uani 1 1 d . . . H18 H -0.0967 -0.6810 0.8915 0.082 Uiso 1 1 calc R . . C19 C 0.4871(4) -0.6927(5) 0.9623(2) 0.0784(16) Uani 1 1 d . . . H19 H 0.5067 -0.7281 0.9368 0.094 Uiso 1 1 calc R . . C20 C 0.5492(4) -0.6827(5) 1.0078(3) 0.096(2) Uani 1 1 d . . . H20 H 0.6115 -0.7118 1.0140 0.115 Uiso 1 1 calc R . . C21 C 0.5184(5) -0.6288(6) 1.0446(3) 0.097(2) Uani 1 1 d . . . H21 H 0.5607 -0.6206 1.0757 0.117 Uiso 1 1 calc R . . C22 C 0.4275(4) -0.5877(5) 1.0363(2) 0.0781(15) Uani 1 1 d . . . H22 H 0.4074 -0.5522 1.0616 0.094 Uiso 1 1 calc R . . C23 C 0.3637(4) -0.5988(4) 0.98918(17) 0.0594(12) Uani 1 1 d . . . C24 C 0.2222(4) -0.5180(4) 1.00601(19) 0.0694(14) Uani 1 1 d . . . C25 C 0.1498(3) -0.4313(4) 0.98678(16) 0.0548(11) Uani 1 1 d . . . C26 C 0.0805(4) -0.4037(4) 1.00820(19) 0.0689(14) Uani 1 1 d . . . H26 H 0.0714 -0.4434 1.0353 0.083 Uiso 1 1 calc R . . C27 C 0.0646(3) -0.2638(4) 0.93741(17) 0.0549(12) Uani 1 1 d . . . C28 C 0.0339(3) -0.1856(4) 0.90446(19) 0.0609(13) Uani 1 1 d . . . C29 C -0.0665(3) -0.0356(4) 0.8488(2) 0.0717(15) Uani 1 1 d . . . H29 H -0.1152 0.0139 0.8345 0.086 Uiso 1 1 calc R . . C30 C 0.0052(3) -0.0583(3) 0.82697(18) 0.0519(11) Uani 1 1 d . . . C31 C 0.0148(3) -0.0024(3) 0.78083(17) 0.0484(10) Uani 1 1 d . . . C32 C 0.1338(3) 0.0431(3) 0.73718(16) 0.0472(10) Uani 1 1 d . . . C33 C 0.0744(4) 0.0636(4) 0.68931(18) 0.0630(13) Uani 1 1 d . . . H33 H 0.0072 0.0633 0.6839 0.076 Uiso 1 1 calc R . . C34 C 0.1164(5) 0.0839(5) 0.6507(2) 0.0818(17) Uani 1 1 d . . . H34 H 0.0771 0.0951 0.6191 0.098 Uiso 1 1 calc R . . C35 C 0.2159(5) 0.0881(5) 0.6582(2) 0.0856(18) Uani 1 1 d . . . H35 H 0.2433 0.1037 0.6319 0.103 Uiso 1 1 calc R . . C36 C 0.2732(4) 0.0695(5) 0.70394(19) 0.0719(14) Uani 1 1 d . . . H36 H 0.3403 0.0723 0.7096 0.086 Uiso 1 1 calc R . . N1 N 0.2149(2) 0.1097(3) 0.92808(13) 0.0441(8) Uani 1 1 d . . . N2 N 0.3281(2) 0.0240(3) 0.89557(12) 0.0433(8) Uani 1 1 d . . . N3 N 0.1567(2) -0.6395(3) 0.83652(12) 0.0429(8) Uani 1 1 d . . . N4 N 0.0224(2) -0.6658(3) 0.86604(14) 0.0503(9) Uani 1 1 d . . . N5 N 0.3968(3) -0.6507(3) 0.95455(15) 0.0566(10) Uani 1 1 d . . . N6 N 0.2713(3) -0.5552(3) 0.97271(13) 0.0518(9) Uani 1 1 d . . . N7 N 0.1096(2) 0.0155(3) 0.78018(12) 0.0439(8) Uani 1 1 d . . . N8 N 0.2312(3) 0.0465(3) 0.74150(13) 0.0500(9) Uani 1 1 d . . . O1 O 0.1558(2) 0.1039(2) 0.88197(11) 0.0533(7) Uani 1 1 d . . . O2 O 0.4948(2) 0.0494(3) 0.91905(13) 0.0671(9) Uani 1 1 d . . . O3 O 0.1982(3) -0.7326(3) 0.77243(15) 0.0873(12) Uani 1 1 d . . . O4 O 0.0762(2) -0.6217(3) 0.90939(11) 0.0578(8) Uani 1 1 d . . . O5 O 0.3373(2) -0.6621(3) 0.90842(12) 0.0638(8) Uani 1 1 d . . . O6 O 0.2344(3) -0.5501(4) 1.04863(14) 0.1019(14) Uani 1 1 d . . . O7 O -0.0575(2) 0.0202(3) 0.74891(13) 0.0646(9) Uani 1 1 d . . . O8 O 0.2916(2) 0.0316(3) 0.78672(11) 0.0579(8) Uani 1 1 d . . . S1 S 0.34367(8) -0.19559(9) 0.85206(5) 0.0532(3) Uani 1 1 d . . . S2 S 0.51551(12) -0.22968(13) 0.81232(7) 0.0983(6) Uani 1 1 d . . . S3 S 0.44197(13) -0.48502(14) 0.78428(9) 0.1194(8) Uani 1 1 d . . . S4 S 0.27265(7) -0.44139(9) 0.82483(4) 0.0491(3) Uani 1 1 d . . . S5 S 0.16351(8) -0.34988(10) 0.93670(4) 0.0581(3) Uani 1 1 d . . . S6 S 0.00679(11) -0.29302(13) 0.98545(6) 0.0794(4) Uani 1 1 d . . . S7 S 0.08986(8) -0.15721(10) 0.85572(5) 0.0563(3) Uani 1 1 d . . . S8 S -0.06633(12) -0.10066(14) 0.90408(7) 0.0974(6) Uani 1 1 d . . . Cu1 Cu 0.22009(3) 0.03492(4) 0.836612(18) 0.04430(16) Uani 1 1 d . . . Cu2 Cu 0.20984(4) -0.60600(4) 0.905496(19) 0.04784(17) 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 C1 0.051(3) 0.063(3) 0.050(3) 0.006(2) 0.016(2) 0.013(2) C2 0.065(3) 0.085(4) 0.048(3) -0.003(3) 0.014(3) 0.011(3) C3 0.069(3) 0.110(4) 0.037(3) -0.004(3) -0.002(3) 0.017(3) C4 0.051(3) 0.085(3) 0.040(3) -0.002(2) -0.003(2) 0.020(2) C5 0.039(2) 0.050(2) 0.040(2) -0.0006(19) 0.007(2) 0.0053(19) C6 0.040(2) 0.054(3) 0.047(3) 0.002(2) 0.006(2) 0.005(2) C7 0.035(2) 0.051(2) 0.047(2) 0.0015(19) 0.007(2) 0.0006(18) C8 0.056(3) 0.057(3) 0.075(3) -0.013(2) 0.026(3) -0.015(2) C9 0.055(3) 0.056(3) 0.070(3) -0.011(2) 0.034(3) -0.009(2) C10 0.052(3) 0.060(3) 0.071(3) -0.016(2) 0.031(3) -0.007(2) C11 0.079(4) 0.071(3) 0.113(5) -0.042(3) 0.055(4) -0.023(3) C12 0.048(3) 0.052(3) 0.050(3) -0.013(2) 0.014(2) -0.004(2) C13 0.050(3) 0.047(3) 0.062(3) -0.007(2) 0.015(2) 0.001(2) C14 0.043(2) 0.040(2) 0.045(3) 0.0021(18) 0.004(2) 0.0024(18) C15 0.052(3) 0.045(2) 0.057(3) -0.002(2) 0.002(2) 0.001(2) C16 0.059(3) 0.048(3) 0.072(3) -0.003(2) -0.005(3) -0.009(2) C17 0.049(3) 0.070(3) 0.090(4) 0.006(3) 0.009(3) -0.008(3) C18 0.042(3) 0.088(4) 0.074(4) 0.005(3) 0.013(3) -0.007(3) C19 0.048(3) 0.085(4) 0.088(4) -0.003(3) -0.010(3) 0.015(3) C20 0.056(4) 0.094(5) 0.111(6) 0.008(4) -0.031(4) 0.003(3) C21 0.075(4) 0.108(5) 0.078(4) 0.009(4) -0.039(4) 0.004(4) C22 0.073(4) 0.088(4) 0.060(3) 0.007(3) -0.009(3) 0.009(3) C23 0.062(3) 0.061(3) 0.044(3) 0.011(2) -0.007(2) 0.004(2) C24 0.080(4) 0.076(3) 0.049(3) 0.007(3) 0.010(3) 0.010(3) C25 0.068(3) 0.066(3) 0.033(2) 0.000(2) 0.018(2) 0.001(2) C26 0.087(4) 0.077(3) 0.047(3) 0.008(2) 0.024(3) 0.002(3) C27 0.052(3) 0.058(3) 0.061(3) 0.009(2) 0.024(2) 0.009(2) C28 0.051(3) 0.063(3) 0.074(3) 0.002(3) 0.027(3) 0.008(2) C29 0.052(3) 0.073(3) 0.094(4) 0.021(3) 0.024(3) 0.022(3) C30 0.037(2) 0.050(3) 0.067(3) 0.002(2) 0.008(2) 0.0007(19) C31 0.046(3) 0.036(2) 0.055(3) -0.0047(19) -0.002(2) 0.0063(19) C32 0.052(3) 0.040(2) 0.042(3) -0.0022(18) -0.001(2) 0.0002(19) C33 0.071(3) 0.058(3) 0.047(3) -0.002(2) -0.010(3) -0.002(2) C34 0.113(5) 0.088(4) 0.037(3) 0.004(3) 0.004(3) 0.004(4) C35 0.112(5) 0.100(4) 0.049(3) 0.004(3) 0.027(4) 0.012(4) C36 0.079(4) 0.094(4) 0.048(3) -0.001(3) 0.025(3) 0.002(3) N1 0.039(2) 0.049(2) 0.043(2) 0.0028(16) 0.0079(17) 0.0038(16) N2 0.0320(18) 0.052(2) 0.041(2) -0.0017(16) 0.0004(16) 0.0051(15) N3 0.0377(19) 0.0441(19) 0.043(2) -0.0001(15) 0.0025(16) 0.0002(15) N4 0.044(2) 0.052(2) 0.050(2) 0.0062(17) 0.0040(19) 0.0037(17) N5 0.045(2) 0.060(2) 0.058(3) 0.003(2) 0.000(2) 0.0081(18) N6 0.048(2) 0.067(2) 0.035(2) 0.0020(17) 0.0000(18) 0.0105(18) N7 0.042(2) 0.0440(19) 0.041(2) 0.0025(15) 0.0002(16) -0.0023(15) N8 0.054(2) 0.057(2) 0.037(2) 0.0015(17) 0.0076(19) 0.0040(18) O1 0.0396(16) 0.070(2) 0.0441(18) -0.0019(15) -0.0017(14) 0.0134(14) O2 0.0334(17) 0.091(2) 0.072(2) -0.0325(19) 0.0035(16) -0.0095(16) O3 0.082(2) 0.077(2) 0.118(3) -0.054(2) 0.052(2) -0.029(2) O4 0.0490(18) 0.082(2) 0.0415(18) -0.0001(16) 0.0091(15) -0.0032(16) O5 0.0476(18) 0.086(2) 0.0473(19) -0.0079(17) -0.0072(16) 0.0113(16) O6 0.129(4) 0.130(3) 0.047(2) 0.029(2) 0.021(2) 0.043(3) O7 0.0421(18) 0.068(2) 0.068(2) -0.0003(17) -0.0151(17) 0.0048(15) O8 0.0425(17) 0.087(2) 0.0419(18) 0.0113(16) 0.0061(15) 0.0101(15) S1 0.0423(6) 0.0485(6) 0.0730(8) -0.0021(6) 0.0224(6) 0.0005(5) S2 0.0940(11) 0.0811(10) 0.1509(16) -0.0491(10) 0.0897(12) -0.0352(8) S3 0.1054(13) 0.0882(11) 0.204(2) -0.0669(12) 0.1125(15) -0.0360(9) S4 0.0396(6) 0.0468(6) 0.0631(7) -0.0090(5) 0.0168(6) -0.0017(5) S5 0.0529(7) 0.0741(8) 0.0513(7) 0.0136(6) 0.0206(6) 0.0137(6) S6 0.0800(9) 0.0973(10) 0.0744(9) 0.0145(8) 0.0448(8) 0.0238(8) S7 0.0432(6) 0.0604(7) 0.0684(8) 0.0145(6) 0.0197(6) 0.0118(5) S8 0.0858(11) 0.0988(11) 0.1303(15) 0.0414(10) 0.0694(11) 0.0442(9) Cu1 0.0339(3) 0.0563(3) 0.0386(3) 0.0000(2) 0.0012(2) 0.0030(2) Cu2 0.0416(3) 0.0572(3) 0.0398(3) 0.0031(2) 0.0007(2) 0.0037(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 C1 C2 1.348(6) . ? C1 N1 1.351(5) . ? C2 C3 1.388(7) . ? C3 C4 1.371(7) . ? C4 C5 1.401(6) . ? C5 N1 1.353(5) . ? C5 N2 1.366(5) . ? C6 O2 1.209(5) . ? C6 N2 1.392(5) . ? C6 C7 1.486(6) . ? C7 C8 1.313(6) . ? C7 S1 1.757(4) . ? C8 S2 1.736(5) . ? C9 C10 1.332(6) . ? C9 S1 1.753(4) . ? C9 S2 1.768(4) . ? C10 S4 1.753(4) . ? C10 S3 1.761(4) . ? C11 C12 1.321(6) . ? C11 S3 1.720(5) . ? C12 C13 1.496(6) . ? C12 S4 1.740(4) . ? C13 O3 1.222(5) . ? C13 N3 1.364(5) . ? C14 N4 1.349(5) . ? C14 N3 1.369(5) . ? C14 C15 1.420(6) . ? C15 C16 1.370(6) . ? C16 C17 1.364(7) . ? C17 C18 1.367(7) . ? C18 N4 1.361(5) . ? C19 N5 1.349(6) . ? C19 C20 1.360(8) . ? C20 C21 1.376(9) . ? C21 C22 1.352(8) . ? C22 C23 1.406(7) . ? C23 N5 1.333(6) . ? C23 N6 1.387(6) . ? C24 O6 1.221(6) . ? C24 N6 1.368(6) . ? C24 C25 1.479(7) . ? C25 C26 1.316(6) . ? C25 S5 1.759(4) . ? C26 S6 1.727(5) . ? C27 C28 1.319(6) . ? C27 S5 1.757(4) . ? C27 S6 1.771(4) . ? C28 S8 1.758(4) . ? C28 S7 1.769(5) . ? C29 C30 1.338(6) . ? C29 S8 1.731(5) . ? C30 C31 1.489(6) . ? C30 S7 1.750(4) . ? C31 O7 1.214(5) . ? C31 N7 1.370(5) . ? C32 N8 1.363(5) . ? C32 N7 1.367(5) . ? C32 C33 1.413(6) . ? C33 C34 1.375(7) . ? C34 C35 1.381(8) . ? C35 C36 1.351(8) . ? C36 N8 1.355(6) . ? N1 O1 1.351(4) . ? N2 Cu1 1.957(3) . ? N3 Cu2 1.926(3) . ? N4 O4 1.369(4) . ? N5 O5 1.360(5) . ? N6 Cu2 1.960(4) . ? N7 Cu1 1.944(3) . ? N8 O8 1.350(4) . ? O1 Cu1 1.925(3) . ? O4 Cu2 1.941(3) . ? O5 Cu2 1.920(3) . ? O8 Cu1 1.915(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 C2 C1 N1 120.6(4) . . ? C1 C2 C3 118.4(5) . . ? C4 C3 C2 120.7(5) . . ? C3 C4 C5 120.1(4) . . ? N1 C5 N2 114.3(4) . . ? N1 C5 C4 116.7(4) . . ? N2 C5 C4 128.6(4) . . ? O2 C6 N2 126.1(4) . . ? O2 C6 C7 120.6(4) . . ? N2 C6 C7 113.3(4) . . ? C8 C7 C6 123.8(4) . . ? C8 C7 S1 117.3(3) . . ? C6 C7 S1 118.7(3) . . ? C7 C8 S2 118.6(3) . . ? C10 C9 S1 121.9(3) . . ? C10 C9 S2 124.2(3) . . ? S1 C9 S2 113.9(3) . . ? C9 C10 S4 121.9(3) . . ? C9 C10 S3 123.9(3) . . ? S4 C10 S3 114.2(3) . . ? C12 C11 S3 119.0(4) . . ? C11 C12 C13 123.4(4) . . ? C11 C12 S4 117.3(3) . . ? C13 C12 S4 119.3(3) . . ? O3 C13 N3 126.5(4) . . ? O3 C13 C12 119.2(4) . . ? N3 C13 C12 114.3(4) . . ? N4 C14 N3 114.1(4) . . ? N4 C14 C15 116.7(4) . . ? N3 C14 C15 129.1(4) . . ? C16 C15 C14 119.8(4) . . ? C17 C16 C15 120.8(5) . . ? C16 C17 C18 120.0(5) . . ? N4 C18 C17 118.9(5) . . ? N5 C19 C20 119.3(6) . . ? C19 C20 C21 118.9(6) . . ? C22 C21 C20 121.0(6) . . ? C21 C22 C23 119.7(6) . . ? N5 C23 N6 114.7(4) . . ? N5 C23 C22 117.3(5) . . ? N6 C23 C22 127.9(5) . . ? O6 C24 N6 125.4(5) . . ? O6 C24 C25 119.9(5) . . ? N6 C24 C25 114.6(4) . . ? C26 C25 C24 123.4(4) . . ? C26 C25 S5 117.3(4) . . ? C24 C25 S5 119.0(3) . . ? C25 C26 S6 119.2(4) . . ? C28 C27 S5 123.4(3) . . ? C28 C27 S6 122.2(3) . . ? S5 C27 S6 114.3(3) . . ? C27 C28 S8 123.8(4) . . ? C27 C28 S7 122.6(3) . . ? S8 C28 S7 113.5(3) . . ? C30 C29 S8 118.4(4) . . ? C29 C30 C31 122.7(4) . . ? C29 C30 S7 116.8(4) . . ? C31 C30 S7 120.5(3) . . ? O7 C31 N7 127.9(4) . . ? O7 C31 C30 119.5(4) . . ? N7 C31 C30 112.6(4) . . ? N8 C32 N7 113.7(4) . . ? N8 C32 C33 115.9(4) . . ? N7 C32 C33 130.4(4) . . ? C34 C33 C32 119.7(5) . . ? C33 C34 C35 121.1(5) . . ? C36 C35 C34 119.6(5) . . ? C35 C36 N8 118.9(5) . . ? C1 N1 O1 117.5(3) . . ? C1 N1 C5 123.4(4) . . ? O1 N1 C5 119.0(3) . . ? C5 N2 C6 119.9(3) . . ? C5 N2 Cu1 111.9(3) . . ? C6 N2 Cu1 125.3(3) . . ? C13 N3 C14 119.3(4) . . ? C13 N3 Cu2 125.6(3) . . ? C14 N3 Cu2 112.1(3) . . ? C14 N4 C18 123.9(4) . . ? C14 N4 O4 119.0(3) . . ? C18 N4 O4 117.1(4) . . ? C23 N5 C19 123.8(4) . . ? C23 N5 O5 118.8(4) . . ? C19 N5 O5 117.4(4) . . ? C24 N6 C23 120.2(4) . . ? C24 N6 Cu2 124.7(3) . . ? C23 N6 Cu2 111.0(3) . . ? C32 N7 C31 120.8(4) . . ? C32 N7 Cu1 110.5(3) . . ? C31 N7 Cu1 127.7(3) . . ? O8 N8 C36 116.5(4) . . ? O8 N8 C32 118.6(3) . . ? C36 N8 C32 124.8(4) . . ? N1 O1 Cu1 111.2(2) . . ? N4 O4 Cu2 109.3(2) . . ? N5 O5 Cu2 111.5(2) . . ? N8 O8 Cu1 110.1(2) . . ? C9 S1 C7 94.8(2) . . ? C8 S2 C9 94.6(2) . . ? C11 S3 C10 94.7(2) . . ? C12 S4 C10 94.9(2) . . ? C27 S5 C25 94.6(2) . . ? C26 S6 C27 94.6(2) . . ? C30 S7 C28 95.5(2) . . ? C29 S8 C28 95.5(2) . . ? O8 Cu1 O1 155.38(14) . . ? O8 Cu1 N7 83.11(14) . . ? O1 Cu1 N7 99.35(13) . . ? O8 Cu1 N2 99.17(13) . . ? O1 Cu1 N2 83.16(13) . . ? N7 Cu1 N2 168.87(14) . . ? O5 Cu2 N3 95.83(13) . . ? O5 Cu2 O4 153.01(14) . . ? N3 Cu2 O4 83.45(13) . . ? O5 Cu2 N6 82.96(14) . . ? N3 Cu2 N6 172.63(15) . . ? O4 Cu2 N6 100.94(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.444 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.129