# 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_complex1 _database_code_depnum_ccdc_archive 'CCDC 919307' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H72 Cu6 N30 S6' _chemical_formula_weight 1859.14 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1431(8) _cell_length_b 13.4151(10) _cell_length_c 13.7079(9) _cell_angle_alpha 62.032(2) _cell_angle_beta 64.1690(10) _cell_angle_gamma 83.174(2) _cell_volume 1910.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 1.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6952 _exptl_absorpt_correction_T_max 0.7671 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14062 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7379 _reflns_number_gt 6124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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. ; _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^)+(0.0588P)^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 7379 _refine_ls_number_parameters 514 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.087 _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 0.50980(3) 0.91287(3) 0.67359(3) 0.03822(10) Uani 1 1 d . . . Cu2 Cu 0.65311(3) 0.94478(3) 0.44496(3) 0.03845(10) Uani 1 1 d . . . Cu3 Cu 0.43310(3) 0.84080(3) 0.56307(3) 0.04074(11) Uani 1 1 d . . . S1 S 0.59427(5) 0.75978(5) 0.54070(6) 0.03797(16) Uani 1 1 d . . . S2 S 0.61556(5) 1.07634(6) 0.59610(6) 0.03732(16) Uani 1 1 d . . . S3 S 0.67683(5) 1.06167(5) 0.24849(5) 0.03411(15) Uani 1 1 d . . . N1 N 0.56685(17) 0.75924(18) 0.74627(19) 0.0379(5) Uani 1 1 d . . . N2 N 0.64559(19) 0.60234(19) 0.7146(2) 0.0437(5) Uani 1 1 d . . . N3 N 0.6183(2) 0.61007(19) 0.8956(2) 0.0457(5) Uani 1 1 d . . . N4 N 0.5468(2) 0.7692(2) 0.9158(2) 0.0521(6) Uani 1 1 d . . . H4A H 0.5317 0.8312 0.8799 0.062 Uiso 1 1 d G . . N5 N 0.6986(2) 0.4620(2) 0.8576(2) 0.0581(7) Uani 1 1 d . . . N6 N 0.78233(17) 1.00247(18) 0.45563(18) 0.0357(5) Uani 1 1 d . . . N7 N 0.83650(19) 1.13883(19) 0.4934(2) 0.0412(5) Uani 1 1 d . . . N8 N 0.97892(18) 1.0670(2) 0.3669(2) 0.0439(5) Uani 1 1 d . . . N9 N 0.9178(2) 0.9346(2) 0.3337(2) 0.0460(6) Uani 1 1 d . . . H9B H 0.8596 0.9116 0.3355 0.055 Uiso 1 1 d G . . N10 N 1.0266(2) 1.2031(2) 0.4006(2) 0.0555(6) Uani 1 1 d . . . N11 N 0.71465(17) 1.23274(18) 0.28000(18) 0.0369(5) Uani 1 1 d . . . N12 N 0.87224(17) 1.19068(18) 0.13749(18) 0.0371(5) Uani 1 1 d . . . N13 N 0.89565(18) 1.34034(18) 0.17785(19) 0.0403(5) Uani 1 1 d . . . N14 N 0.7347(2) 1.3754(2) 0.3187(2) 0.0518(6) Uani 1 1 d . . . H14A H 0.6699 1.3494 0.3653 0.062 Uiso 1 1 d G . . N15 N 1.04757(19) 1.28882(19) 0.0511(2) 0.0459(6) Uani 1 1 d . . . C1 C 0.6023(2) 0.7005(2) 0.6821(2) 0.0358(5) Uani 1 1 d . . . C2 C 0.6523(2) 0.5603(2) 0.8219(3) 0.0474(7) Uani 1 1 d . . . C3 C 0.5783(2) 0.7085(2) 0.8532(2) 0.0403(6) Uani 1 1 d . . . C4 C 0.5529(2) 0.7483(3) 1.0239(3) 0.0512(7) Uani 1 1 d . . . C5 C 0.5497(4) 0.8404(4) 1.0439(3) 0.0845(13) Uani 1 1 d . . . H5A H 0.5430 0.9117 0.9875 0.101 Uiso 1 1 calc R . . C6 C 0.5565(5) 0.8281(5) 1.1470(4) 0.1082(18) Uani 1 1 d . . . H6A H 0.5574 0.8915 1.1576 0.130 Uiso 1 1 calc R . . C7 C 0.5618(4) 0.7234(5) 1.2332(4) 0.0918(14) Uani 1 1 d . . . H7A H 0.5644 0.7148 1.3034 0.110 Uiso 1 1 calc R . . C8 C 0.5633(3) 0.6320(4) 1.2149(3) 0.0796(11) Uani 1 1 d . . . H8A H 0.5676 0.5608 1.2732 0.096 Uiso 1 1 calc R . . C9 C 0.5587(3) 0.6421(3) 1.1105(3) 0.0624(9) Uani 1 1 d . . . H9A H 0.5595 0.5785 1.0996 0.075 Uiso 1 1 calc R . . C10 C 0.7429(4) 0.4062(3) 0.7796(4) 0.0780(11) Uani 1 1 d . . . H10A H 0.6845 0.3944 0.7607 0.117 Uiso 1 1 calc R . . H10B H 0.7664 0.3344 0.8219 0.117 Uiso 1 1 calc R . . H10C H 0.8067 0.4534 0.7050 0.117 Uiso 1 1 calc R . . C11 C 0.7120(3) 0.4102(3) 0.9702(3) 0.0716(10) Uani 1 1 d . . . H11A H 0.6541 0.4309 1.0284 0.107 Uiso 1 1 calc R . . H11B H 0.7856 0.4362 0.9536 0.107 Uiso 1 1 calc R . . H11C H 0.7053 0.3291 1.0032 0.107 Uiso 1 1 calc R . . C12 C 0.7600(2) 1.0709(2) 0.5083(2) 0.0343(5) Uani 1 1 d . . . C13 C 0.8952(2) 1.0044(2) 0.3865(2) 0.0375(6) Uani 1 1 d . . . C14 C 0.9454(2) 1.1340(2) 0.4211(2) 0.0426(6) Uani 1 1 d . . . C15 C 1.0229(2) 0.9258(2) 0.2466(2) 0.0437(6) Uani 1 1 d . . . C16 C 1.1245(3) 0.9279(3) 0.2540(3) 0.0618(9) Uani 1 1 d . . . H16A H 1.1260 0.9376 0.3163 0.074 Uiso 1 1 calc R . . C17 C 1.2242(3) 0.9155(3) 0.1672(3) 0.0705(10) Uani 1 1 d . . . H17A H 1.2924 0.9159 0.1722 0.085 Uiso 1 1 calc R . . C18 C 1.2225(3) 0.9026(3) 0.0741(3) 0.0673(10) Uani 1 1 d . . . H18A H 1.2899 0.8965 0.0151 0.081 Uiso 1 1 calc R . . C19 C 1.1225(3) 0.8987(3) 0.0684(3) 0.0596(8) Uani 1 1 d . . . H19A H 1.1213 0.8883 0.0065 0.071 Uiso 1 1 calc R . . C20 C 1.0223(3) 0.9104(2) 0.1546(3) 0.0501(7) Uani 1 1 d . . . H20A H 0.9541 0.9077 0.1502 0.060 Uiso 1 1 calc R . . C21 C 1.0001(3) 1.2869(3) 0.4445(4) 0.0748(11) Uani 1 1 d . . . H21A H 0.9194 1.2810 0.4910 0.112 Uiso 1 1 calc R . . H21B H 1.0261 1.3615 0.3759 0.112 Uiso 1 1 calc R . . H21C H 1.0373 1.2736 0.4955 0.112 Uiso 1 1 calc R . . C22 C 1.1453(3) 1.2018(3) 0.3268(3) 0.0746(11) Uani 1 1 d . . . H22A H 1.1549 1.1343 0.3173 0.112 Uiso 1 1 calc R . . H22B H 1.1897 1.2029 0.3664 0.112 Uiso 1 1 calc R . . H22C H 1.1700 1.2674 0.2477 0.112 Uiso 1 1 calc R . . C23 C 0.7632(2) 1.1743(2) 0.2164(2) 0.0316(5) Uani 1 1 d . . . C24 C 0.9357(2) 1.2726(2) 0.1236(2) 0.0382(6) Uani 1 1 d . . . C25 C 0.7862(2) 1.3155(2) 0.2548(2) 0.0380(6) Uani 1 1 d . . . C26 C 0.7826(3) 1.4516(2) 0.3349(3) 0.0545(8) Uani 1 1 d . . . C27 C 0.8874(3) 1.5144(3) 0.2544(3) 0.0649(9) Uani 1 1 d . . . H27A H 0.9325 1.5063 0.1847 0.078 Uiso 1 1 calc R . . C28 C 0.9259(4) 1.5904(3) 0.2776(4) 0.0846(12) Uani 1 1 d U . . H28A H 0.9971 1.6317 0.2240 0.102 Uiso 1 1 calc R . . C29 C 0.8594(5) 1.6041(4) 0.3786(5) 0.0995(15) Uani 1 1 d U . . H29A H 0.8848 1.6554 0.3930 0.119 Uiso 1 1 calc R . . C30 C 0.7554(5) 1.5422(4) 0.4587(4) 0.1010(16) Uani 1 1 d U . . H30A H 0.7107 1.5511 0.5280 0.121 Uiso 1 1 calc R . . C31 C 0.7156(4) 1.4659(3) 0.4373(4) 0.0814(12) Uani 1 1 d . . . H31A H 0.6444 1.4248 0.4917 0.098 Uiso 1 1 calc R . . C32 C 1.1212(3) 1.3740(3) 0.0343(3) 0.0616(9) Uani 1 1 d . . . H32A H 1.0926 1.3809 0.1081 0.092 Uiso 1 1 calc R . . H32B H 1.1228 1.4457 -0.0321 0.092 Uiso 1 1 calc R . . H32C H 1.1967 1.3516 0.0158 0.092 Uiso 1 1 calc R . . C33 C 1.1034(2) 1.2146(3) -0.0033(3) 0.0610(9) Uani 1 1 d . . . H33A H 1.0468 1.1650 0.0094 0.092 Uiso 1 1 calc R . . H33B H 1.1510 1.1702 0.0347 0.092 Uiso 1 1 calc R . . H33C H 1.1489 1.2597 -0.0895 0.092 Uiso 1 1 calc R . . 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 0.03407(17) 0.0433(2) 0.04007(18) -0.02291(15) -0.01463(15) 0.00456(13) Cu2 0.03586(18) 0.0443(2) 0.03534(18) -0.01876(14) -0.01344(15) -0.00341(13) Cu3 0.03184(17) 0.0566(2) 0.04014(19) -0.02806(16) -0.01538(15) 0.00704(14) S1 0.0360(3) 0.0398(4) 0.0421(3) -0.0231(3) -0.0165(3) 0.0065(3) S2 0.0360(3) 0.0449(4) 0.0362(3) -0.0235(3) -0.0142(3) 0.0020(3) S3 0.0307(3) 0.0411(3) 0.0325(3) -0.0203(3) -0.0112(3) 0.0006(2) N1 0.0345(11) 0.0378(12) 0.0393(11) -0.0169(9) -0.0152(9) 0.0032(9) N2 0.0469(13) 0.0378(12) 0.0521(13) -0.0213(10) -0.0265(11) 0.0074(10) N3 0.0449(12) 0.0407(13) 0.0474(13) -0.0154(10) -0.0222(11) 0.0042(10) N4 0.0642(16) 0.0538(16) 0.0452(13) -0.0254(12) -0.0290(13) 0.0147(13) N5 0.0694(17) 0.0415(14) 0.0711(17) -0.0220(12) -0.0442(15) 0.0165(12) N6 0.0305(10) 0.0441(12) 0.0353(11) -0.0195(9) -0.0150(9) 0.0011(9) N7 0.0415(12) 0.0441(13) 0.0452(12) -0.0201(10) -0.0242(10) -0.0008(9) N8 0.0350(11) 0.0512(14) 0.0411(12) -0.0171(10) -0.0162(10) -0.0014(10) N9 0.0325(11) 0.0690(17) 0.0500(13) -0.0372(12) -0.0189(11) 0.0073(11) N10 0.0468(13) 0.0499(15) 0.0665(15) -0.0148(12) -0.0321(13) -0.0086(11) N11 0.0370(11) 0.0375(12) 0.0345(11) -0.0193(9) -0.0112(9) 0.0027(9) N12 0.0337(11) 0.0397(12) 0.0329(10) -0.0174(9) -0.0087(9) -0.0014(9) N13 0.0417(12) 0.0374(12) 0.0397(11) -0.0174(9) -0.0152(10) -0.0018(9) N14 0.0548(14) 0.0474(15) 0.0534(15) -0.0323(12) -0.0134(12) 0.0024(11) N15 0.0353(11) 0.0460(13) 0.0460(12) -0.0184(10) -0.0103(10) -0.0043(9) C1 0.0283(11) 0.0331(13) 0.0437(14) -0.0170(11) -0.0139(11) 0.0003(9) C2 0.0433(15) 0.0349(15) 0.0589(17) -0.0159(13) -0.0239(14) 0.0009(11) C3 0.0346(13) 0.0419(15) 0.0379(13) -0.0157(11) -0.0122(11) -0.0015(11) C4 0.0433(15) 0.067(2) 0.0422(15) -0.0267(14) -0.0156(13) 0.0042(13) C5 0.128(4) 0.076(3) 0.063(2) -0.043(2) -0.042(2) 0.020(2) C6 0.169(5) 0.102(4) 0.071(3) -0.056(3) -0.047(3) 0.013(3) C7 0.103(3) 0.130(4) 0.057(2) -0.053(3) -0.036(2) 0.014(3) C8 0.078(3) 0.098(3) 0.052(2) -0.025(2) -0.0322(19) 0.013(2) C9 0.066(2) 0.072(2) 0.0437(16) -0.0212(15) -0.0247(16) 0.0069(16) C10 0.093(3) 0.054(2) 0.104(3) -0.042(2) -0.056(2) 0.0346(19) C11 0.075(2) 0.055(2) 0.084(2) -0.0173(18) -0.052(2) 0.0101(17) C12 0.0343(12) 0.0395(14) 0.0322(12) -0.0147(10) -0.0190(11) 0.0027(10) C13 0.0321(12) 0.0481(15) 0.0309(12) -0.0154(11) -0.0156(11) 0.0030(11) C14 0.0410(14) 0.0410(15) 0.0448(14) -0.0091(11) -0.0281(13) -0.0017(11) C15 0.0393(14) 0.0499(16) 0.0380(14) -0.0219(12) -0.0129(12) 0.0085(11) C16 0.0433(16) 0.098(3) 0.0548(18) -0.0454(18) -0.0213(15) 0.0173(16) C17 0.0410(17) 0.105(3) 0.069(2) -0.049(2) -0.0190(17) 0.0159(17) C18 0.0525(19) 0.083(2) 0.061(2) -0.0455(18) -0.0080(17) 0.0095(17) C19 0.067(2) 0.066(2) 0.0524(18) -0.0397(16) -0.0171(17) 0.0064(16) C20 0.0525(17) 0.0555(18) 0.0500(16) -0.0311(14) -0.0217(15) 0.0063(13) C21 0.085(3) 0.049(2) 0.107(3) -0.0243(19) -0.065(2) -0.0059(17) C22 0.0437(17) 0.083(3) 0.072(2) -0.0077(18) -0.0296(17) -0.0172(16) C23 0.0310(12) 0.0354(13) 0.0267(11) -0.0128(9) -0.0122(10) 0.0005(9) C24 0.0390(13) 0.0343(14) 0.0328(12) -0.0104(10) -0.0128(11) -0.0026(10) C25 0.0469(15) 0.0330(13) 0.0355(12) -0.0158(10) -0.0191(12) 0.0044(11) C26 0.089(2) 0.0363(16) 0.0553(17) -0.0264(13) -0.0416(18) 0.0160(15) C27 0.092(3) 0.0479(19) 0.078(2) -0.0348(17) -0.049(2) 0.0070(17) C28 0.120(3) 0.060(2) 0.111(3) -0.043(2) -0.076(3) 0.006(2) C29 0.165(5) 0.076(3) 0.124(4) -0.066(3) -0.100(4) 0.029(3) C30 0.167(5) 0.078(3) 0.096(3) -0.068(3) -0.064(3) 0.036(3) C31 0.119(3) 0.065(2) 0.075(2) -0.049(2) -0.040(2) 0.022(2) C32 0.0483(17) 0.063(2) 0.0599(18) -0.0194(16) -0.0171(15) -0.0151(15) C33 0.0382(15) 0.059(2) 0.0649(19) -0.0281(16) -0.0046(15) 0.0000(13) _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 Cu1 N1 2.040(2) . ? Cu1 S2 2.2632(7) . ? Cu1 S3 2.2658(7) 2_676 ? Cu1 Cu3 2.6802(5) . ? Cu1 Cu2 2.7097(4) . ? Cu2 N6 2.035(2) . ? Cu2 S1 2.2353(8) . ? Cu2 S3 2.2874(7) . ? Cu2 Cu3 2.7730(5) . ? Cu2 Cu3 2.9338(5) 2_676 ? Cu3 N11 2.048(2) 2_676 ? Cu3 S1 2.2275(7) . ? Cu3 S2 2.2753(7) 2_676 ? Cu3 Cu2 2.9338(5) 2_676 ? S1 C1 1.764(3) . ? S2 C12 1.766(2) . ? S2 Cu3 2.2753(7) 2_676 ? S3 C23 1.764(3) . ? S3 Cu1 2.2658(7) 2_676 ? N1 C1 1.349(3) . ? N1 C3 1.366(3) . ? N2 C1 1.322(3) . ? N2 C2 1.346(4) . ? N3 C3 1.319(3) . ? N3 C2 1.355(4) . ? N4 C3 1.355(4) . ? N4 C4 1.411(4) . ? N4 H4A 0.80(3) . ? N5 C2 1.346(4) . ? N5 C11 1.449(4) . ? N5 C10 1.465(4) . ? N6 C12 1.350(3) . ? N6 C13 1.364(3) . ? N7 C12 1.321(3) . ? N7 C14 1.356(4) . ? N8 C13 1.319(3) . ? N8 C14 1.343(4) . ? N9 C13 1.367(3) . ? N9 C15 1.416(3) . ? N9 H9B 0.84(3) . ? N10 C14 1.343(4) . ? N10 C22 1.447(4) . ? N10 C21 1.451(5) . ? N11 C23 1.349(3) . ? N11 C25 1.357(3) . ? N11 Cu3 2.048(2) 2_676 ? N12 C23 1.332(3) . ? N12 C24 1.351(3) . ? N13 C25 1.324(3) . ? N13 C24 1.354(3) . ? N14 C25 1.373(3) . ? N14 C26 1.407(4) . ? N14 H14A 0.80(3) . ? N15 C24 1.340(3) . ? N15 C32 1.455(4) . ? N15 C33 1.460(4) . ? C4 C5 1.378(5) . ? C4 C9 1.383(4) . ? C5 C6 1.385(6) . ? C5 H5A 0.9300 . ? C6 C7 1.366(6) . ? C6 H6A 0.9300 . ? C7 C8 1.359(6) . ? C7 H7A 0.9300 . ? C8 C9 1.401(5) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C15 C20 1.374(4) . ? C15 C16 1.387(4) . ? C16 C17 1.391(4) . ? C16 H16A 0.9300 . ? C17 C18 1.375(5) . ? C17 H17A 0.9300 . ? C18 C19 1.359(5) . ? C18 H18A 0.9300 . ? C19 C20 1.388(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C26 C27 1.380(5) . ? C26 C31 1.385(5) . ? C27 C28 1.402(5) . ? C27 H27A 0.9300 . ? C28 C29 1.363(6) . ? C28 H28A 0.9300 . ? C29 C30 1.368(7) . ? C29 H29A 0.9300 . ? C30 C31 1.396(6) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 N1 Cu1 S2 120.93(6) . . ? N1 Cu1 S3 121.82(6) . 2_676 ? S2 Cu1 S3 108.97(3) . 2_676 ? N1 Cu1 Cu3 90.33(6) . . ? S2 Cu1 Cu3 129.55(2) . . ? S3 Cu1 Cu3 78.71(2) 2_676 . ? N1 Cu1 Cu2 89.92(6) . . ? S2 Cu1 Cu2 78.324(19) . . ? S3 Cu1 Cu2 129.81(2) 2_676 . ? Cu3 Cu1 Cu2 61.921(12) . . ? N6 Cu2 S1 121.64(6) . . ? N6 Cu2 S3 104.29(6) . . ? S1 Cu2 S3 122.11(3) . . ? N6 Cu2 Cu1 90.25(6) . . ? S1 Cu2 Cu1 78.740(19) . . ? S3 Cu2 Cu1 137.70(2) . . ? N6 Cu2 Cu3 148.21(6) . . ? S1 Cu2 Cu3 51.460(19) . . ? S3 Cu2 Cu3 103.44(2) . . ? Cu1 Cu2 Cu3 58.516(11) . . ? N6 Cu2 Cu3 82.62(6) . 2_676 ? S1 Cu2 Cu3 140.36(2) . 2_676 ? S3 Cu2 Cu3 73.111(19) . 2_676 ? Cu1 Cu2 Cu3 69.649(12) . 2_676 ? Cu3 Cu2 Cu3 90.845(14) . 2_676 ? N11 Cu3 S1 121.85(6) 2_676 . ? N11 Cu3 S2 106.87(7) 2_676 2_676 ? S1 Cu3 S2 119.65(3) . 2_676 ? N11 Cu3 Cu1 90.58(6) 2_676 . ? S1 Cu3 Cu1 79.52(2) . . ? S2 Cu3 Cu1 136.12(2) 2_676 . ? N11 Cu3 Cu2 149.58(6) 2_676 . ? S1 Cu3 Cu2 51.71(2) . . ? S2 Cu3 Cu2 99.66(2) 2_676 . ? Cu1 Cu3 Cu2 59.562(12) . . ? N11 Cu3 Cu2 84.47(6) 2_676 2_676 ? S1 Cu3 Cu2 138.97(2) . 2_676 ? S2 Cu3 Cu2 73.456(19) 2_676 2_676 ? Cu1 Cu3 Cu2 68.478(12) . 2_676 ? Cu2 Cu3 Cu2 89.155(14) . 2_676 ? C1 S1 Cu3 107.49(8) . . ? C1 S1 Cu2 106.80(9) . . ? Cu3 S1 Cu2 76.83(2) . . ? C12 S2 Cu1 111.00(9) . . ? C12 S2 Cu3 96.24(8) . 2_676 ? Cu1 S2 Cu3 90.67(3) . 2_676 ? C23 S3 Cu1 111.23(8) . 2_676 ? C23 S3 Cu2 97.88(8) . . ? Cu1 S3 Cu2 88.09(2) 2_676 . ? C1 N1 C3 114.3(2) . . ? C1 N1 Cu1 118.42(17) . . ? C3 N1 Cu1 127.27(18) . . ? C1 N2 C2 115.0(2) . . ? C3 N3 C2 114.6(2) . . ? C3 N4 C4 130.7(3) . . ? C3 N4 H4A 114(3) . . ? C4 N4 H4A 115(3) . . ? C2 N5 C11 122.0(3) . . ? C2 N5 C10 120.5(3) . . ? C11 N5 C10 117.4(3) . . ? C12 N6 C13 113.9(2) . . ? C12 N6 Cu2 118.66(16) . . ? C13 N6 Cu2 124.99(17) . . ? C12 N7 C14 114.8(2) . . ? C13 N8 C14 114.4(2) . . ? C13 N9 C15 128.4(3) . . ? C13 N9 H9B 113(2) . . ? C15 N9 H9B 115(2) . . ? C14 N10 C22 121.1(3) . . ? C14 N10 C21 122.3(3) . . ? C22 N10 C21 116.5(3) . . ? C23 N11 C25 114.3(2) . . ? C23 N11 Cu3 117.75(16) . 2_676 ? C25 N11 Cu3 124.58(17) . 2_676 ? C23 N12 C24 115.1(2) . . ? C25 N13 C24 114.0(2) . . ? C25 N14 C26 130.1(3) . . ? C25 N14 H14A 111(3) . . ? C26 N14 H14A 117(3) . . ? C24 N15 C32 120.9(3) . . ? C24 N15 C33 122.1(2) . . ? C32 N15 C33 116.6(2) . . ? N2 C1 N1 125.5(2) . . ? N2 C1 S1 116.5(2) . . ? N1 C1 S1 118.05(18) . . ? N2 C2 N5 117.3(3) . . ? N2 C2 N3 125.3(2) . . ? N5 C2 N3 117.4(3) . . ? N3 C3 N4 120.1(3) . . ? N3 C3 N1 125.4(3) . . ? N4 C3 N1 114.5(2) . . ? C5 C4 C9 119.1(3) . . ? C5 C4 N4 116.8(3) . . ? C9 C4 N4 124.1(3) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C7 C6 C5 120.5(4) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C8 C7 C6 119.1(4) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C7 C8 C9 121.8(4) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C4 C9 C8 118.8(4) . . ? C4 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 N6 125.5(2) . . ? N7 C12 S2 117.63(19) . . ? N6 C12 S2 116.77(18) . . ? N8 C13 N6 125.9(2) . . ? N8 C13 N9 120.1(2) . . ? N6 C13 N9 114.0(2) . . ? N10 C14 N8 117.2(3) . . ? N10 C14 N7 117.4(3) . . ? N8 C14 N7 125.4(3) . . ? C20 C15 C16 119.5(3) . . ? C20 C15 N9 118.1(3) . . ? C16 C15 N9 122.3(3) . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C15 C20 C19 120.5(3) . . ? C15 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? N10 C21 H21A 109.5 . . ? N10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N10 C22 H22A 109.5 . . ? N10 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N10 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N12 C23 N11 125.0(2) . . ? N12 C23 S3 117.94(18) . . ? N11 C23 S3 116.92(17) . . ? N15 C24 N12 118.1(2) . . ? N15 C24 N13 116.7(2) . . ? N12 C24 N13 125.2(2) . . ? N13 C25 N11 126.2(2) . . ? N13 C25 N14 120.4(2) . . ? N11 C25 N14 113.3(2) . . ? C27 C26 C31 119.2(3) . . ? C27 C26 N14 124.7(3) . . ? C31 C26 N14 116.0(3) . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 120.3(5) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C31 120.6(4) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C26 C31 C30 119.8(4) . . ? C26 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? N15 C32 H32A 109.5 . . ? N15 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N15 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N15 C33 H33A 109.5 . . ? N15 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N15 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.919 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.075 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 919308' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 Cu N8 S4' _chemical_formula_weight 535.16 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1491(6) _cell_length_b 10.3660(4) _cell_length_c 17.8580(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.330(2) _cell_angle_gamma 90.00 _cell_volume 2042.10(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6694 _exptl_absorpt_correction_T_max 0.7840 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7115 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1984 _reflns_number_gt 1672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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. ; _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^)+(0.0302P)^2^+4.9655P] 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 1984 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.0000 0.80259(5) 0.7500 0.03255(16) Uani 1 2 d S . . S1 S -0.17154(7) 0.70422(8) 0.77486(4) 0.0351(2) Uani 1 1 d . . . S2 S -0.55473(6) 0.45559(7) 0.64618(4) 0.02678(17) Uani 1 1 d . . . N1 N -0.3493(2) 0.5741(2) 0.69833(13) 0.0288(5) Uani 1 1 d . . . H1 H -0.3726 0.5653 0.7419 0.035 Uiso 1 1 calc R . . N2 N -0.38105(19) 0.5368(2) 0.57003(13) 0.0263(5) Uani 1 1 d . . . H2 H -0.4250 0.5114 0.5291 0.032 Uiso 0.50 1 calc PR A -1 N3 N -0.19854(19) 0.6406(2) 0.62812(13) 0.0255(5) Uani 1 1 d . . . N4 N -0.2318(2) 0.5859(2) 0.50010(13) 0.0288(5) Uani 1 1 d . . . H4 H -0.2849 0.5556 0.4648 0.035 Uiso 1 1 calc R . . C1 C -0.2407(2) 0.6363(3) 0.69415(15) 0.0243(6) Uani 1 1 d . . . C2 C -0.4207(2) 0.5264(2) 0.63656(15) 0.0232(5) Uani 1 1 d . . . C3 C -0.2675(2) 0.5895(2) 0.56813(15) 0.0236(5) Uani 1 1 d . . . C4 C -0.1206(2) 0.6237(3) 0.47564(16) 0.0265(6) Uani 1 1 d . . . C5 C -0.0235(3) 0.6790(3) 0.52158(18) 0.0332(7) Uani 1 1 d . . . H5 H -0.0270 0.6934 0.5726 0.040 Uiso 1 1 calc R . . C6 C 0.0792(3) 0.7124(3) 0.4903(2) 0.0423(8) Uani 1 1 d . . . H6 H 0.1444 0.7501 0.5209 0.051 Uiso 1 1 calc R . . C7 C 0.0867(3) 0.6911(3) 0.4149(2) 0.0429(8) Uani 1 1 d . . . H7 H 0.1558 0.7149 0.3947 0.052 Uiso 1 1 calc R . . C8 C -0.0091(3) 0.6344(4) 0.3702(2) 0.0479(9) Uani 1 1 d . . . H8 H -0.0043 0.6181 0.3195 0.057 Uiso 1 1 calc R . . C9 C -0.1133(3) 0.6010(3) 0.39975(18) 0.0392(7) Uani 1 1 d . . . H9 H -0.1782 0.5635 0.3688 0.047 Uiso 1 1 calc R . . 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 0.0226(3) 0.0337(3) 0.0421(3) 0.000 0.0074(2) 0.000 S1 0.0331(4) 0.0526(5) 0.0197(4) -0.0036(3) 0.0047(3) -0.0200(3) S2 0.0214(3) 0.0381(4) 0.0198(3) 0.0028(3) -0.0006(2) -0.0059(3) N1 0.0272(12) 0.0402(14) 0.0190(12) -0.0007(10) 0.0036(9) -0.0118(10) N2 0.0247(11) 0.0358(13) 0.0186(12) -0.0004(10) 0.0031(9) -0.0058(9) N3 0.0236(11) 0.0309(12) 0.0223(12) 0.0002(10) 0.0047(9) -0.0024(9) N4 0.0264(12) 0.0390(14) 0.0214(12) -0.0035(10) 0.0050(9) -0.0058(10) C1 0.0221(13) 0.0283(14) 0.0228(14) 0.0033(11) 0.0036(11) -0.0032(10) C2 0.0262(13) 0.0242(13) 0.0189(13) 0.0020(10) 0.0026(10) -0.0002(10) C3 0.0239(13) 0.0242(13) 0.0227(14) 0.0018(10) 0.0031(11) 0.0015(10) C4 0.0260(14) 0.0290(14) 0.0260(15) 0.0037(11) 0.0083(11) 0.0048(11) C5 0.0321(15) 0.0372(16) 0.0318(17) -0.0036(13) 0.0100(12) -0.0017(12) C6 0.0297(16) 0.0451(19) 0.054(2) -0.0049(16) 0.0118(15) -0.0061(13) C7 0.0356(17) 0.0503(19) 0.048(2) 0.0135(16) 0.0214(15) 0.0060(14) C8 0.0443(19) 0.072(2) 0.0302(18) 0.0078(17) 0.0158(15) 0.0066(17) C9 0.0327(16) 0.061(2) 0.0246(16) 0.0022(14) 0.0052(13) 0.0003(14) _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 Cu1 S1 2.2672(7) . ? Cu1 S1 2.2672(7) 2_556 ? Cu1 S2 2.4489(8) 4_456 ? Cu1 S2 2.4489(8) 3 ? S1 C1 1.687(3) . ? S2 C2 1.696(3) . ? S2 Cu1 2.4489(8) 3_445 ? N1 C2 1.356(3) . ? N1 C1 1.384(3) . ? N1 H1 0.8600 . ? N2 C2 1.331(3) . ? N2 C3 1.383(3) . ? N2 H2 0.8600 . ? N3 C1 1.332(3) . ? N3 C3 1.334(3) . ? N4 C3 1.333(4) . ? N4 C4 1.427(3) . ? N4 H4 0.8600 . ? C4 C5 1.384(4) . ? C4 C9 1.389(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9300 . ? C6 C7 1.379(5) . ? C6 H6 0.9300 . ? C7 C8 1.371(5) . ? C7 H7 0.9300 . ? C8 C9 1.388(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? 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 S1 Cu1 S1 126.55(5) . 2_556 ? S1 Cu1 S2 105.53(3) . 4_456 ? S1 Cu1 S2 108.35(3) 2_556 4_456 ? S1 Cu1 S2 108.35(3) . 3 ? S1 Cu1 S2 105.53(3) 2_556 3 ? S2 Cu1 S2 99.27(4) 4_456 3 ? C1 S1 Cu1 108.33(9) . . ? C2 S2 Cu1 103.33(9) . 3_445 ? C2 N1 C1 122.8(2) . . ? C2 N1 H1 118.6 . . ? C1 N1 H1 118.6 . . ? C2 N2 C3 118.5(2) . . ? C2 N2 H2 120.7 . . ? C3 N2 H2 120.7 . . ? C1 N3 C3 117.5(2) . . ? C3 N4 C4 131.2(2) . . ? C3 N4 H4 114.4 . . ? C4 N4 H4 114.4 . . ? N3 C1 N1 119.1(2) . . ? N3 C1 S1 124.5(2) . . ? N1 C1 S1 116.3(2) . . ? N2 C2 N1 117.7(2) . . ? N2 C2 S2 122.5(2) . . ? N1 C2 S2 119.8(2) . . ? N4 C3 N3 121.9(2) . . ? N4 C3 N2 114.0(2) . . ? N3 C3 N2 124.0(2) . . ? C5 C4 C9 119.8(3) . . ? C5 C4 N4 124.9(3) . . ? C9 C4 N4 115.4(3) . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 119.0(3) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 120.0(3) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.681 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.077 data_complex3 _database_code_depnum_ccdc_archive 'CCDC 919309' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H36 Cl3 Co6 N24 S12' _chemical_formula_weight 1865.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Ia-3d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' 'y+5/4, x+3/4, -z+3/4' '-y+5/4, -x+5/4, -z+5/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' 'x+5/4, z+3/4, -y+3/4' '-x+3/4, z+5/4, y+3/4' '-x+5/4, -z+5/4, -y+5/4' 'x+3/4, -z+3/4, y+5/4' 'z+5/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+5/4' '-z+3/4, y+5/4, x+3/4' '-z+5/4, -y+5/4, -x+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' '-y-3/4, -x-1/4, z-1/4' 'y-3/4, x-3/4, z-3/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y-1/4' 'x-1/4, -z-3/4, -y-1/4' 'x-3/4, z-3/4, y-3/4' '-x-1/4, z-1/4, -y-3/4' '-z-3/4, -y-1/4, x-1/4' '-z-1/4, y-1/4, -x-3/4' 'z-1/4, -y-3/4, -x-1/4' 'z-3/4, y-3/4, x-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z, x, y+1/2' 'z, x+1/2, -y' 'z+1/2, -x, y' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z, x' '-y, z, x+1/2' 'y, z+1/2, -x' '-y-1/4, -x+1/4, z+1/4' 'y-1/4, x-1/4, z-1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' '-x-1/4, -z+1/4, y+1/4' 'x+1/4, -z-1/4, -y+1/4' 'x-1/4, z-1/4, y-1/4' '-x+1/4, z+1/4, -y-1/4' '-z-1/4, -y+1/4, x+1/4' '-z+1/4, y+1/4, -x-1/4' 'z+1/4, -y-1/4, -x+1/4' 'z-1/4, y-1/4, x-1/4' _cell_length_a 31.8956(6) _cell_length_b 31.8956(6) _cell_length_c 31.8956(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32448.3(11) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14928 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6277 _exptl_absorpt_correction_T_max 0.7120 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18593 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2652 _reflns_number_gt 1824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998' _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. ; _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^)+(0.0967P)^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 2652 _refine_ls_number_parameters 181 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.167 _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 Co1 Co 0.459144(18) 0.709144(18) 0.1250 0.0475(3) Uani 1 2 d S . . Co2 Co 0.3750 0.6250 0.1250 0.0402(4) Uani 1 6 d S . . Co3 Co 0.453973(18) 0.546027(18) 0.046027(18) 0.0480(4) Uani 1 3 d S . . S1 S 0.42475(3) 0.65938(3) 0.07207(4) 0.0436(3) Uani 1 1 d . . . S2 S 0.51782(4) 0.52605(4) 0.07130(5) 0.0630(4) Uani 1 1 d . . . Cl1 Cl 0.5000 0.7500 0.07327(6) 0.0596(5) Uani 1 2 d S . . N1 N 0.49364(11) 0.65369(11) 0.11525(12) 0.0469(9) Uani 1 1 d . A . N2 N 0.47847(11) 0.59366(11) 0.07531(11) 0.0437(9) Uani 1 1 d . . . N3 N 0.53808(13) 0.59343(14) 0.12103(13) 0.0592(11) Uani 1 1 d . A . C1 C 0.46956(13) 0.63270(13) 0.08786(14) 0.0423(10) Uani 1 1 d . . . C2 C 0.51357(14) 0.57592(15) 0.09175(16) 0.0517(12) Uani 1 1 d . . . C3 C 0.52639(14) 0.63157(16) 0.13267(16) 0.0511(12) Uani 1 1 d . . . N4 N 0.54664(14) 0.65271(15) 0.16310(17) 0.0716(14) Uani 0.50 1 d P A 1 H4A H 0.5429 0.6794 0.1627 0.086 Uiso 0.50 1 calc PR A 1 C4 C 0.5728(4) 0.6383(5) 0.1954(4) 0.066(4) Uani 0.50 1 d PGU A 1 C5 C 0.5796(5) 0.5966(4) 0.2062(5) 0.168(8) Uani 0.50 1 d PGU A 1 H5A H 0.5642 0.5755 0.1932 0.201 Uiso 0.50 1 calc PR A 1 C6 C 0.6094(6) 0.5865(5) 0.2363(6) 0.224(13) Uani 0.50 1 d PGU A 1 H6A H 0.6140 0.5587 0.2435 0.269 Uiso 0.50 1 calc PR A 1 C7 C 0.6324(5) 0.6181(8) 0.2557(5) 0.172(10) Uani 0.50 1 d PGU A 1 H7A H 0.6523 0.6114 0.2758 0.206 Uiso 0.50 1 calc PR A 1 C8 C 0.6255(7) 0.6598(7) 0.2449(7) 0.45(4) Uani 0.50 1 d PGU A 1 H8A H 0.6409 0.6809 0.2578 0.539 Uiso 0.50 1 calc PR A 1 C9 C 0.5957(6) 0.6699(4) 0.2147(7) 0.32(2) Uani 0.50 1 d PGU A 1 H9A H 0.5911 0.6977 0.2075 0.383 Uiso 0.50 1 calc PR A 1 N4' N 0.54664(14) 0.65271(15) 0.16310(17) 0.0716(14) Uani 0.50 1 d P A 2 H4'A H 0.5350 0.6754 0.1718 0.086 Uiso 0.50 1 calc PR A 2 C4' C 0.5859(2) 0.6412(2) 0.1826(2) 0.070(4) Uani 0.50 1 d PGU A 2 C5' C 0.6091(2) 0.6049(2) 0.1760(2) 0.109(5) Uani 0.50 1 d PGU A 2 H5'A H 0.6027 0.5874 0.1535 0.130 Uiso 0.50 1 calc PR A 2 C6' C 0.6418(2) 0.5947(2) 0.2029(3) 0.114(5) Uani 0.50 1 d PGU A 2 H6'A H 0.6573 0.5704 0.1985 0.136 Uiso 0.50 1 calc PR A 2 C7' C 0.6513(2) 0.6208(2) 0.2365(2) 0.102(5) Uani 0.50 1 d PGU A 2 H7'A H 0.6731 0.6139 0.2546 0.123 Uiso 0.50 1 calc PR A 2 C8' C 0.6281(2) 0.6571(2) 0.2431(2) 0.089(4) Uani 0.50 1 d PGU A 2 H8'A H 0.6345 0.6746 0.2656 0.106 Uiso 0.50 1 calc PR A 2 C9' C 0.5954(2) 0.6673(2) 0.2162(2) 0.063(3) Uani 0.50 1 d PGU A 2 H9'A H 0.5799 0.6916 0.2206 0.076 Uiso 0.50 1 calc PR A 2 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 Co1 0.0415(4) 0.0415(4) 0.0596(6) -0.0020(3) 0.0020(3) -0.0045(4) Co2 0.0402(4) 0.0402(4) 0.0402(4) -0.0007(3) 0.0007(3) 0.0007(3) Co3 0.0480(4) 0.0480(4) 0.0480(4) -0.0080(3) 0.0080(3) 0.0080(3) S1 0.0406(6) 0.0423(6) 0.0478(7) -0.0007(5) 0.0004(5) 0.0013(5) S2 0.0544(8) 0.0602(8) 0.0745(9) -0.0105(7) 0.0054(6) 0.0200(6) Cl1 0.0600(11) 0.0537(10) 0.0652(12) 0.000 0.000 -0.0158(8) N1 0.042(2) 0.047(2) 0.052(2) -0.0030(17) -0.0005(18) -0.0064(17) N2 0.041(2) 0.042(2) 0.049(2) -0.0041(16) 0.0066(16) 0.0041(16) N3 0.043(2) 0.063(3) 0.072(3) -0.002(2) -0.005(2) 0.003(2) C1 0.036(2) 0.048(3) 0.044(3) 0.001(2) 0.0094(19) -0.0020(19) C2 0.042(3) 0.051(3) 0.063(3) 0.002(2) 0.009(2) 0.009(2) C3 0.033(2) 0.058(3) 0.063(3) 0.003(2) -0.005(2) -0.003(2) N4 0.057(3) 0.068(3) 0.090(4) -0.007(3) -0.021(2) -0.005(2) C4 0.058(6) 0.077(7) 0.063(6) 0.020(5) -0.013(6) -0.012(5) C5 0.172(11) 0.174(12) 0.157(11) -0.016(9) -0.040(9) -0.006(9) C6 0.231(15) 0.219(15) 0.222(15) 0.006(10) -0.036(10) 0.005(10) C7 0.172(12) 0.176(13) 0.168(12) 0.002(9) -0.039(9) -0.010(9) C8 0.45(4) 0.45(4) 0.45(4) 0.002(11) -0.005(11) 0.003(11) C9 0.32(3) 0.32(3) 0.32(3) -0.005(10) -0.007(10) 0.007(10) N4' 0.057(3) 0.068(3) 0.090(4) -0.007(3) -0.021(2) -0.005(2) C4' 0.059(7) 0.075(7) 0.077(8) 0.004(6) -0.001(6) -0.017(6) C5' 0.091(8) 0.108(8) 0.127(9) -0.012(7) -0.032(7) 0.019(7) C6' 0.090(8) 0.121(9) 0.130(9) -0.003(7) -0.043(7) 0.028(7) C7' 0.091(8) 0.104(8) 0.112(9) 0.012(7) -0.040(7) -0.018(7) C8' 0.076(7) 0.092(8) 0.097(8) 0.001(6) -0.062(6) -0.010(6) C9' 0.051(5) 0.076(6) 0.062(6) -0.013(5) -0.036(5) -0.001(5) _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 Co1 N1 2.106(4) 13_455 ? Co1 N1 2.106(4) . ? Co1 Cl1 2.4735(14) 13_455 ? Co1 Cl1 2.4735(14) . ? Co1 S1 2.5639(13) . ? Co1 S1 2.5639(13) 13_455 ? Co2 S1 2.5633(11) 13_455 ? Co2 S1 2.5633(11) 19 ? Co2 S1 2.5633(11) . ? Co2 S1 2.5633(11) 10_655 ? Co2 S1 2.5633(11) 22_564 ? Co2 S1 2.5633(11) 7_564 ? Co3 N2 1.947(4) 10_655 ? Co3 N2 1.947(4) . ? Co3 N2 1.947(4) 7_564 ? Co3 S2 2.2811(14) . ? Co3 S2 2.2811(14) 7_564 ? Co3 S2 2.2811(14) 10_655 ? S1 C1 1.738(5) . ? S2 C2 1.724(5) . ? Cl1 Co1 2.4735(14) 26_564 ? N1 C1 1.342(6) . ? N1 C3 1.378(6) . ? N2 C1 1.338(5) . ? N2 C2 1.360(6) . ? N3 C3 1.325(6) . ? N3 C2 1.340(6) . ? C3 N4 1.347(7) . ? N4 C4 1.402(11) . ? N4 H4A 0.8600 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5A 0.9300 . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C4' C5' 1.3900 . ? C4' C9' 1.3900 . ? C5' C6' 1.3900 . ? C5' H5'A 0.9300 . ? C6' C7' 1.3900 . ? C6' H6'A 0.9300 . ? C7' C8' 1.3900 . ? C7' H7'A 0.9300 . ? C8' C9' 1.3900 . ? C8' H8'A 0.9300 . ? C9' H9'A 0.9300 . ? 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 N1 Co1 N1 154.1(2) 13_455 . ? N1 Co1 Cl1 93.94(10) 13_455 13_455 ? N1 Co1 Cl1 105.40(10) . 13_455 ? N1 Co1 Cl1 105.40(10) 13_455 . ? N1 Co1 Cl1 93.94(10) . . ? Cl1 Co1 Cl1 83.67(7) 13_455 . ? N1 Co1 S1 93.51(10) 13_455 . ? N1 Co1 S1 66.83(10) . . ? Cl1 Co1 S1 172.23(2) 13_455 . ? Cl1 Co1 S1 96.45(4) . . ? N1 Co1 S1 66.83(10) 13_455 13_455 ? N1 Co1 S1 93.51(10) . 13_455 ? Cl1 Co1 S1 96.45(4) 13_455 13_455 ? Cl1 Co1 S1 172.23(2) . 13_455 ? S1 Co1 S1 84.48(6) . 13_455 ? S1 Co2 S1 97.98(3) 13_455 19 ? S1 Co2 S1 84.51(5) 13_455 . ? S1 Co2 S1 79.61(5) 19 . ? S1 Co2 S1 176.78(5) 13_455 10_655 ? S1 Co2 S1 84.51(5) 19 10_655 ? S1 Co2 S1 97.98(3) . 10_655 ? S1 Co2 S1 97.98(3) 13_455 22_564 ? S1 Co2 S1 97.98(3) 19 22_564 ? S1 Co2 S1 176.78(5) . 22_564 ? S1 Co2 S1 79.61(5) 10_655 22_564 ? S1 Co2 S1 79.61(5) 13_455 7_564 ? S1 Co2 S1 176.78(5) 19 7_564 ? S1 Co2 S1 97.98(3) . 7_564 ? S1 Co2 S1 97.98(3) 10_655 7_564 ? S1 Co2 S1 84.51(5) 22_564 7_564 ? N2 Co3 N2 97.55(13) 10_655 . ? N2 Co3 N2 97.55(13) 10_655 7_564 ? N2 Co3 N2 97.55(13) . 7_564 ? N2 Co3 S2 166.52(12) 10_655 . ? N2 Co3 S2 71.95(11) . . ? N2 Co3 S2 92.32(11) 7_564 . ? N2 Co3 S2 92.32(11) 10_655 7_564 ? N2 Co3 S2 166.52(12) . 7_564 ? N2 Co3 S2 71.95(11) 7_564 7_564 ? S2 Co3 S2 99.49(5) . 7_564 ? N2 Co3 S2 71.95(11) 10_655 10_655 ? N2 Co3 S2 92.32(11) . 10_655 ? N2 Co3 S2 166.52(12) 7_564 10_655 ? S2 Co3 S2 99.49(5) . 10_655 ? S2 Co3 S2 99.49(5) 7_564 10_655 ? C1 S1 Co2 96.24(14) . . ? C1 S1 Co1 76.14(15) . . ? Co2 S1 Co1 95.51(4) . . ? C2 S2 Co3 78.80(17) . . ? Co1 Cl1 Co1 96.33(7) 26_564 . ? C1 N1 C3 116.2(4) . . ? C1 N1 Co1 102.5(3) . . ? C3 N1 Co1 140.1(3) . . ? C1 N2 C2 116.6(4) . . ? C1 N2 Co3 141.6(3) . . ? C2 N2 Co3 101.0(3) . . ? C3 N3 C2 114.4(4) . . ? N2 C1 N1 122.5(4) . . ? N2 C1 S1 122.9(3) . . ? N1 C1 S1 114.5(3) . . ? N3 C2 N2 125.1(4) . . ? N3 C2 S2 127.0(4) . . ? N2 C2 S2 107.6(4) . . ? N3 C3 N4 121.8(4) . . ? N3 C3 N1 124.8(4) . . ? N4 C3 N1 113.4(4) . . ? C3 N4 C4 130.5(7) . . ? C3 N4 H4A 114.7 . . ? C4 N4 H4A 114.7 . . ? C5 C4 C9 120.0 . . ? C5 C4 N4 126.1(11) . . ? C9 C4 N4 113.7(11) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 H9A 120.0 . . ? C4 C9 H9A 120.0 . . ? C5' C4' C9' 120.0 . . ? C4' C5' C6' 120.0 . . ? C4' C5' H5'A 120.0 . . ? C6' C5' H5'A 120.0 . . ? C7' C6' C5' 120.0 . . ? C7' C6' H6'A 120.0 . . ? C5' C6' H6'A 120.0 . . ? C8' C7' C6' 120.0 . . ? C8' C7' H7'A 120.0 . . ? C6' C7' H7'A 120.0 . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8'A 120.0 . . ? C9' C8' H8'A 120.0 . . ? C8' C9' C4' 120.0 . . ? C8' C9' H9'A 120.0 . . ? C4' C9' H9'A 120.0 . . ? # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.250 0.000 0.010 507.8 26.0 2 0.750 0.000 0.033 507.8 26.6 3 0.500 -0.012 0.250 508.2 26.4 4 1.000 -0.022 0.250 508.2 26.3 5 0.000 -0.022 0.750 508.2 26.4 6 0.500 -0.012 0.750 508.2 26.3 7 0.017 0.250 0.000 507.6 26.6 8 0.980 0.250 0.500 507.7 26.0 9 0.750 0.500 0.230 507.8 26.0 10 0.250 0.500 0.259 507.7 26.6 11 0.019 0.750 0.000 507.7 26.0 12 0.509 0.750 0.500 507.6 26.6 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.554 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.093