# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. #==================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _publ_contact_author_name 'Ye-Gao Yin' _publ_contact_author_address # Name and address of author for correspondence ; Yin, Ye-Gao Department of Chemistry Shantou University Shantou, Guangdong, 515063 P. R. China ; _publ_contact_author_phone 86-754-2903699 _publ_contact_author_fax 86-754-2902767 _publ_contact_author_email ygyin@stu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a paper submitted to Chem. Commun.. Thanks. Ye-Gao, Yin ; _publ_section_title ; Design and solvothermal synthesis of luminescent copper(I)-pyrazolate coordination oligomer and polymer frameworks ; loop_ _publ_author_name _publ_author_address 'Jun He' ; Department of Chemistry Shantou University Shantou 515063 P. R. China ; 'Ye-Gao Yin' ; Department of Chemistry Shantou University Shantou 515063 P. R. China ; 'Tao Wu' ; Department of Chemistry Shantou University Shantou 515063 P. R. China ; 'Dan Li' ; Department of Chemistry Shantou University Shantou 515063 P. R. China ; #===============================END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 286905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H72 Cu12 N24' _chemical_formula_weight 1891.90 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 18.6363(13) _cell_length_b 46.435(3) _cell_length_c 34.874(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 30179(4) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15168 _exptl_absorpt_coefficient_mu 3.359 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4872 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 153632 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -57 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14827 _reflns_number_gt 10779 _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^)+(0.0566P)^2^+54.5501P] 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 14827 _refine_ls_number_parameters 891 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.006 _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 0.30411(3) 0.846861(11) 0.272564(15) 0.03778(14) Uani 1 1 d . . . Cu2 Cu 0.17003(3) 0.846956(11) 0.220529(15) 0.03893(15) Uani 1 1 d . . . Cu3 Cu 0.23011(3) 0.907432(12) 0.255496(14) 0.03919(15) Uani 1 1 d . . . Cu4 Cu 0.53721(3) 0.957093(15) 0.454881(15) 0.04692(17) Uani 1 1 d . . . Cu5 Cu 0.40742(3) 0.931258(16) 0.500105(14) 0.05384(19) Uani 1 1 d . . . Cu6 Cu 0.51712(3) 0.973940(14) 0.543730(15) 0.04317(16) Uani 1 1 d . . . Cu7 Cu 0.05653(3) 0.085782(12) 0.781031(16) 0.04209(15) Uani 1 1 d . . . Cu8 Cu 0.0000 0.148135(17) 0.7500 0.0390(2) Uani 1 2 d S . . Cu9 Cu 0.16168(3) 0.179603(16) 1.000077(15) 0.05464(19) Uani 1 1 d . . . Cu10 Cu 0.28580(3) 0.206800(14) 0.952324(15) 0.04575(17) Uani 1 1 d . . . Cu11 Cu 0.26847(3) 0.225097(14) 1.040718(15) 0.04482(16) Uani 1 1 d . . . Cu12 Cu 0.0000 0.167550(16) 1.2500 0.03554(19) Uani 1 2 d S . . Cu13 Cu 0.07276(3) 0.107826(11) 1.227517(15) 0.03815(14) Uani 1 1 d . . . N1 N 0.26894(19) 0.81185(7) 0.25463(9) 0.0321(8) Uani 1 1 d . . . N2 N 0.20482(19) 0.81136(7) 0.23584(10) 0.0336(8) Uani 1 1 d . . . N3 N 0.14820(19) 0.88205(7) 0.19804(9) 0.0335(8) Uani 1 1 d . . . N4 N 0.17395(19) 0.90799(7) 0.21147(9) 0.0326(8) Uani 1 1 d . . . N5 N 0.29321(19) 0.90467(7) 0.29665(9) 0.0342(8) Uani 1 1 d . . . N6 N 0.3295(2) 0.87905(7) 0.30091(9) 0.0351(9) Uani 1 1 d . . . N7 N 0.4126(2) 0.92490(10) 0.44797(10) 0.0489(11) Uani 1 1 d . . . N8 N 0.46776(19) 0.93731(8) 0.42761(9) 0.0380(9) Uani 1 1 d . . . N9 N 0.0976(2) 0.93572(10) 0.05246(10) 0.0492(11) Uani 1 1 d . . . N10 N 0.05364(19) 0.95474(9) 0.07119(10) 0.0407(10) Uani 1 1 d . . . N11 N 0.59864(18) 0.98612(9) 0.51770(10) 0.0392(9) Uani 1 1 d . . . N12 N 0.6102(2) 0.97492(9) 0.48160(10) 0.0459(10) Uani 1 1 d . . . N13 N 0.02977(19) 0.05027(7) 0.76138(10) 0.0340(8) Uani 1 1 d . . . N14 N 0.0754(2) 0.11957(7) 0.80709(10) 0.0380(9) Uani 1 1 d . . . N15 N 0.05799(19) 0.14657(7) 0.79386(9) 0.0339(8) Uani 1 1 d . . . N16 N 0.1642(2) 0.17255(10) 0.94818(10) 0.0500(11) Uani 1 1 d . . . N17 N 0.21629(19) 0.18577(8) 0.92668(10) 0.0395(9) Uani 1 1 d . . . N18 N 0.3593(2) 0.22551(9) 0.97776(10) 0.0449(10) Uani 1 1 d . . . N19 N 0.34871(19) 0.23709(9) 1.01354(10) 0.0402(9) Uani 1 1 d . . . N20 N 0.2000(2) 0.20580(9) 1.06948(10) 0.0421(10) Uani 1 1 d . . . N21 N 0.1585(2) 0.18544(9) 1.05213(10) 0.0483(11) Uani 1 1 d . . . N22 N 0.06276(19) 0.16664(7) 1.20901(9) 0.0322(8) Uani 1 1 d . . . N23 N 0.09917(19) 0.14130(7) 1.20246(10) 0.0349(9) Uani 1 1 d . . . N24 N -0.03434(18) -0.07303(7) 0.75726(10) 0.0323(8) Uani 1 1 d . . . C1 C 0.3559(2) 0.77811(10) 0.28356(13) 0.0417(11) Uani 1 1 d . . . H1A H 0.3649 0.7930 0.3020 0.063 Uiso 1 1 calc R . . H1B H 0.3950 0.7772 0.2657 0.063 Uiso 1 1 calc R . . H1C H 0.3513 0.7600 0.2965 0.063 Uiso 1 1 calc R . . C2 C 0.2877(2) 0.78465(9) 0.26242(11) 0.0298(9) Uani 1 1 d . . . C3 C 0.2360(2) 0.76595(8) 0.24884(11) 0.0302(9) Uani 1 1 d . . . C4 C 0.1847(2) 0.78366(9) 0.23192(12) 0.0322(10) Uani 1 1 d . . . C5 C 0.1179(3) 0.77612(10) 0.21048(15) 0.0493(13) Uani 1 1 d . . . H5A H 0.1081 0.7907 0.1917 0.074 Uiso 1 1 calc R . . H5B H 0.0784 0.7749 0.2281 0.074 Uiso 1 1 calc R . . H5C H 0.1241 0.7579 0.1979 0.074 Uiso 1 1 calc R . . C6 C 0.0894(3) 0.86198(10) 0.14090(14) 0.0512(13) Uani 1 1 d . . . H6A H 0.0572 0.8516 0.1574 0.077 Uiso 1 1 calc R . . H6B H 0.1264 0.8492 0.1319 0.077 Uiso 1 1 calc R . . H6C H 0.0633 0.8695 0.1194 0.077 Uiso 1 1 calc R . . C7 C 0.1226(2) 0.88618(9) 0.16265(11) 0.0316(9) Uani 1 1 d . . . C8 C 0.1304(2) 0.91490(9) 0.15218(11) 0.0292(9) Uani 1 1 d . . . C9 C 0.1632(2) 0.92784(9) 0.18379(11) 0.0312(9) Uani 1 1 d . . . C10 C 0.1844(3) 0.95840(10) 0.18943(14) 0.0520(14) Uani 1 1 d . . . H10A H 0.2181 0.9597 0.2101 0.078 Uiso 1 1 calc R . . H10B H 0.1426 0.9696 0.1954 0.078 Uiso 1 1 calc R . . H10C H 0.2060 0.9656 0.1664 0.078 Uiso 1 1 calc R . . C11 C 0.1096(2) 0.92823(9) 0.11526(11) 0.0320(10) Uani 1 1 d . . . C12 C 0.2829(3) 0.95182(10) 0.33031(14) 0.0537(14) Uani 1 1 d . . . H12A H 0.2703 0.9592 0.3055 0.081 Uiso 1 1 calc R . . H12B H 0.3188 0.9639 0.3417 0.081 Uiso 1 1 calc R . . H12C H 0.2411 0.9515 0.3464 0.081 Uiso 1 1 calc R . . C13 C 0.3117(2) 0.92183(9) 0.32625(11) 0.0334(10) Uani 1 1 d . . . C14 C 0.3596(2) 0.90749(9) 0.34968(11) 0.0305(9) Uani 1 1 d . . . C15 C 0.3692(2) 0.88076(9) 0.33270(11) 0.0328(10) Uani 1 1 d . . . C16 C 0.4157(3) 0.85650(11) 0.34607(15) 0.0582(15) Uani 1 1 d . . . H16A H 0.4028 0.8392 0.3327 0.087 Uiso 1 1 calc R . . H16B H 0.4090 0.8537 0.3731 0.087 Uiso 1 1 calc R . . H16C H 0.4650 0.8610 0.3410 0.087 Uiso 1 1 calc R . . C17 C 0.3015(3) 0.89772(17) 0.43581(16) 0.097(3) Uani 1 1 d . . . H17A H 0.3132 0.8854 0.4570 0.146 Uiso 1 1 calc R . . H17B H 0.2826 0.8863 0.4152 0.146 Uiso 1 1 calc R . . H17C H 0.2662 0.9116 0.4437 0.146 Uiso 1 1 calc R . . C18 C 0.3670(3) 0.91292(11) 0.42270(12) 0.0470(13) Uani 1 1 d . . . C19 C 0.3924(2) 0.91730(9) 0.38596(11) 0.0307(9) Uani 1 1 d . . . C20 C 0.4559(2) 0.93269(9) 0.39052(11) 0.0333(10) Uani 1 1 d . . . C21 C 0.5066(3) 0.94330(13) 0.36040(13) 0.0590(15) Uani 1 1 d . . . H21A H 0.5518 0.9480 0.3720 0.089 Uiso 1 1 calc R . . H21B H 0.4868 0.9601 0.3484 0.089 Uiso 1 1 calc R . . H21C H 0.5136 0.9285 0.3415 0.089 Uiso 1 1 calc R . . C22 C 0.1837(3) 0.89689(14) 0.06718(14) 0.0697(18) Uani 1 1 d . . . H22A H 0.2082 0.8897 0.0894 0.105 Uiso 1 1 calc R . . H22B H 0.2180 0.9051 0.0498 0.105 Uiso 1 1 calc R . . H22C H 0.1587 0.8814 0.0547 0.105 Uiso 1 1 calc R . . C23 C 0.1310(2) 0.91954(11) 0.07907(12) 0.0425(12) Uani 1 1 d . . . C24 C 0.0608(2) 0.95026(10) 0.10900(11) 0.0352(10) Uani 1 1 d . . . C25 C 0.0197(3) 0.96761(12) 0.13711(13) 0.0594(16) Uani 1 1 d . . . H25A H 0.0191 0.9579 0.1614 0.089 Uiso 1 1 calc R . . H25B H -0.0286 0.9701 0.1281 0.089 Uiso 1 1 calc R . . H25C H 0.0421 0.9861 0.1400 0.089 Uiso 1 1 calc R . . C26 C 0.6650(3) 1.01076(12) 0.56876(13) 0.0505(13) Uani 1 1 d . . . H26A H 0.6186 1.0177 0.5763 0.076 Uiso 1 1 calc R . . H26B H 0.6984 1.0265 0.5684 0.076 Uiso 1 1 calc R . . H26C H 0.6811 0.9965 0.5867 0.076 Uiso 1 1 calc R . . C27 C 0.6604(2) 0.99770(10) 0.52969(12) 0.0352(10) Uani 1 1 d . . . C28 C 0.7128(2) 0.99472(10) 0.50138(11) 0.0367(11) Uani 1 1 d . . . C29 C 0.6781(2) 0.98008(11) 0.47183(12) 0.0435(12) Uani 1 1 d . . . C30 C 0.7064(3) 0.96915(15) 0.43408(15) 0.075(2) Uani 1 1 d . . . H30A H 0.6894 0.9499 0.4298 0.112 Uiso 1 1 calc R . . H30B H 0.7579 0.9692 0.4346 0.112 Uiso 1 1 calc R . . H30C H 0.6899 0.9814 0.4138 0.112 Uiso 1 1 calc R . . C31 C 0.0000 -0.02727(13) 0.7500 0.0306(13) Uani 1 2 d S . . C32 C 0.0000 0.00454(12) 0.7500 0.0280(13) Uani 1 2 d S . . C33 C 0.0476(2) 0.02289(9) 0.76848(11) 0.0310(9) Uani 1 1 d . . . C34 C 0.1106(3) 0.01543(10) 0.79329(14) 0.0479(12) Uani 1 1 d . . . H34A H 0.1168 0.0300 0.8125 0.072 Uiso 1 1 calc R . . H34B H 0.1531 0.0143 0.7778 0.072 Uiso 1 1 calc R . . H34C H 0.1024 -0.0028 0.8055 0.072 Uiso 1 1 calc R . . C35 C 0.1313(3) 0.09680(10) 0.86335(15) 0.0650(17) Uani 1 1 d . . . H35A H 0.1395 0.0811 0.8460 0.097 Uiso 1 1 calc R . . H35B H 0.0954 0.0914 0.8817 0.097 Uiso 1 1 calc R . . H35C H 0.1752 0.1014 0.8764 0.097 Uiso 1 1 calc R . . C36 C 0.1063(2) 0.12249(9) 0.84130(12) 0.0369(10) Uani 1 1 d . . . C37 C 0.1105(2) 0.15139(9) 0.85130(11) 0.0295(9) Uani 1 1 d . . . C38 C 0.0800(2) 0.16575(9) 0.82044(11) 0.0316(9) Uani 1 1 d . . . C39 C 0.0702(3) 0.19735(10) 0.81477(14) 0.0522(14) Uani 1 1 d . . . H39A H 0.0330 0.2006 0.7962 0.078 Uiso 1 1 calc R . . H39B H 0.1143 0.2056 0.8058 0.078 Uiso 1 1 calc R . . H39C H 0.0570 0.2061 0.8387 0.078 Uiso 1 1 calc R . . C40 C 0.0564(3) 0.14290(16) 0.93912(15) 0.088(2) Uani 1 1 d . . . H40A H 0.0711 0.1311 0.9604 0.132 Uiso 1 1 calc R . . H40B H 0.0372 0.1309 0.9192 0.132 Uiso 1 1 calc R . . H40C H 0.0204 0.1563 0.9475 0.132 Uiso 1 1 calc R . . C41 C 0.1195(3) 0.15900(11) 0.92410(12) 0.0462(12) Uani 1 1 d . . . C42 C 0.1416(2) 0.16329(9) 0.88668(11) 0.0311(9) Uani 1 1 d . . . C43 C 0.2030(2) 0.18044(9) 0.88961(11) 0.0324(10) Uani 1 1 d . . . C44 C 0.2501(3) 0.19177(12) 0.85895(13) 0.0575(15) Uani 1 1 d . . . H44A H 0.2957 0.1970 0.8697 0.086 Uiso 1 1 calc R . . H44B H 0.2282 0.2084 0.8476 0.086 Uiso 1 1 calc R . . H44C H 0.2568 0.1773 0.8397 0.086 Uiso 1 1 calc R . . C45 C 0.4551(3) 0.21886(15) 0.93011(14) 0.075(2) Uani 1 1 d . . . H45A H 0.4352 0.2001 0.9253 0.113 Uiso 1 1 calc R . . H45B H 0.5065 0.2175 0.9313 0.113 Uiso 1 1 calc R . . H45C H 0.4417 0.2317 0.9098 0.113 Uiso 1 1 calc R . . C46 C 0.4271(2) 0.23009(12) 0.96741(12) 0.0449(13) Uani 1 1 d . . . C47 C 0.4624(2) 0.24511(10) 0.99657(11) 0.0375(11) Uani 1 1 d . . . C48 C 0.4107(2) 0.24868(10) 1.02512(12) 0.0359(10) Uani 1 1 d . . . C49 C 0.4160(3) 0.26273(11) 1.06369(13) 0.0504(13) Uani 1 1 d . . . H49A H 0.3698 0.2699 1.0711 0.076 Uiso 1 1 calc R . . H49B H 0.4496 0.2784 1.0625 0.076 Uiso 1 1 calc R . . H49C H 0.4321 0.2489 1.0822 0.076 Uiso 1 1 calc R . . C50 C 0.2308(3) 0.22168(12) 1.13491(14) 0.0695(18) Uani 1 1 d . . . H50A H 0.2164 0.2414 1.1316 0.104 Uiso 1 1 calc R . . H50B H 0.2814 0.2200 1.1303 0.104 Uiso 1 1 calc R . . H50C H 0.2202 0.2157 1.1606 0.104 Uiso 1 1 calc R . . C51 C 0.1912(2) 0.20322(10) 1.10744(11) 0.0378(11) Uani 1 1 d . . . C52 C 0.1431(2) 0.18124(9) 1.11513(11) 0.0323(10) Uani 1 1 d . . . C53 C 0.1240(3) 0.17046(11) 1.07973(12) 0.0437(12) Uani 1 1 d . . . C54 C 0.0738(3) 0.14634(14) 1.06983(15) 0.077(2) Uani 1 1 d . . . H54A H 0.0391 0.1530 1.0515 0.115 Uiso 1 1 calc R . . H54B H 0.0497 0.1399 1.0926 0.115 Uiso 1 1 calc R . . H54C H 0.1006 0.1306 1.0590 0.115 Uiso 1 1 calc R . . C55 C 0.0398(3) 0.21302(9) 1.17628(13) 0.0433(12) Uani 1 1 d . . . H55A H 0.0325 0.2206 1.2016 0.065 Uiso 1 1 calc R . . H55B H -0.0056 0.2113 1.1635 0.065 Uiso 1 1 calc R . . H55C H 0.0704 0.2258 1.1620 0.065 Uiso 1 1 calc R . . C56 C 0.0741(2) 0.18423(9) 1.17897(11) 0.0282(9) Uani 1 1 d . . . C57 C 0.1184(2) 0.17069(9) 1.15274(11) 0.0295(9) Uani 1 1 d . . . C58 C 0.1333(2) 0.14372(9) 1.16866(12) 0.0339(10) Uani 1 1 d . . . C59 C 0.1777(3) 0.11975(10) 1.15321(15) 0.0532(14) Uani 1 1 d . . . H59A H 0.2049 0.1112 1.1736 0.080 Uiso 1 1 calc R . . H59B H 0.2099 0.1271 1.1341 0.080 Uiso 1 1 calc R . . H59C H 0.1470 0.1055 1.1419 0.080 Uiso 1 1 calc R . . C60 C -0.0546(2) -0.04555(9) 0.76181(12) 0.0322(10) Uani 1 1 d . . . C61 C -0.1258(2) -0.03881(10) 0.77907(14) 0.0450(12) Uani 1 1 d . . . H61A H -0.1269 -0.0190 0.7868 0.068 Uiso 1 1 calc R . . H61B H -0.1336 -0.0509 0.8010 0.068 Uiso 1 1 calc R . . H61C H -0.1629 -0.0422 0.7605 0.068 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 0.0505(3) 0.0329(3) 0.0299(3) -0.0055(2) -0.0099(2) -0.0067(3) Cu2 0.0516(4) 0.0299(3) 0.0352(3) 0.0063(2) -0.0125(3) -0.0007(3) Cu3 0.0563(4) 0.0384(3) 0.0228(3) 0.0026(2) -0.0198(2) -0.0032(3) Cu4 0.0349(3) 0.0785(5) 0.0274(3) -0.0058(3) -0.0052(2) -0.0264(3) Cu5 0.0526(4) 0.0931(5) 0.0157(3) 0.0026(3) -0.0023(2) -0.0337(4) Cu6 0.0343(3) 0.0682(4) 0.0270(3) 0.0072(3) 0.0044(2) -0.0216(3) Cu7 0.0608(4) 0.0294(3) 0.0361(3) -0.0073(2) -0.0133(3) -0.0022(3) Cu8 0.0569(5) 0.0384(4) 0.0217(4) 0.000 -0.0177(3) 0.000 Cu9 0.0535(4) 0.0942(5) 0.0163(3) -0.0012(3) -0.0002(2) -0.0333(4) Cu10 0.0332(3) 0.0760(4) 0.0281(3) -0.0056(3) -0.0036(2) -0.0242(3) Cu11 0.0369(3) 0.0690(4) 0.0285(3) 0.0053(3) 0.0074(2) -0.0217(3) Cu12 0.0484(5) 0.0368(4) 0.0215(4) 0.000 0.0165(3) 0.000 Cu13 0.0498(3) 0.0296(3) 0.0351(3) 0.0059(2) 0.0095(3) -0.0026(2) N1 0.039(2) 0.0295(19) 0.0281(19) -0.0031(15) -0.0086(16) -0.0047(16) N2 0.038(2) 0.030(2) 0.033(2) 0.0008(15) -0.0074(16) -0.0001(16) N3 0.042(2) 0.031(2) 0.0273(19) 0.0062(15) -0.0115(16) -0.0025(16) N4 0.046(2) 0.0300(19) 0.0222(17) -0.0004(14) -0.0115(15) 0.0032(16) N5 0.046(2) 0.034(2) 0.0224(18) 0.0009(15) -0.0147(16) -0.0060(17) N6 0.048(2) 0.032(2) 0.0255(18) -0.0033(15) -0.0108(16) -0.0015(17) N7 0.044(2) 0.085(3) 0.0178(18) 0.0022(19) -0.0036(16) -0.030(2) N8 0.032(2) 0.061(3) 0.0213(18) -0.0037(17) -0.0059(15) -0.0215(18) N9 0.050(2) 0.078(3) 0.0198(19) 0.0038(19) -0.0017(17) 0.029(2) N10 0.038(2) 0.062(3) 0.0223(18) 0.0055(17) -0.0036(16) 0.0242(19) N11 0.029(2) 0.064(3) 0.0249(19) -0.0008(17) 0.0037(15) -0.0180(19) N12 0.037(2) 0.073(3) 0.027(2) -0.0066(19) -0.0034(17) -0.025(2) N13 0.046(2) 0.0248(19) 0.032(2) -0.0031(15) -0.0076(16) -0.0033(16) N14 0.055(2) 0.030(2) 0.0283(19) -0.0067(16) -0.0153(17) -0.0002(18) N15 0.047(2) 0.033(2) 0.0219(18) 0.0011(15) -0.0109(16) -0.0019(17) N16 0.048(2) 0.084(3) 0.0185(18) -0.0007(19) -0.0042(17) -0.032(2) N17 0.032(2) 0.062(3) 0.0239(19) -0.0065(17) -0.0025(15) -0.0174(18) N18 0.031(2) 0.073(3) 0.031(2) -0.0062(19) 0.0004(16) -0.024(2) N19 0.031(2) 0.064(3) 0.0258(19) 0.0013(18) 0.0024(16) -0.0165(19) N20 0.042(2) 0.063(3) 0.0207(18) 0.0011(17) 0.0076(16) -0.023(2) N21 0.051(3) 0.074(3) 0.0199(19) -0.0027(18) 0.0039(17) -0.029(2) N22 0.043(2) 0.033(2) 0.0214(17) 0.0010(15) 0.0142(15) -0.0028(16) N23 0.043(2) 0.033(2) 0.0281(19) 0.0053(15) 0.0149(16) 0.0011(17) N24 0.037(2) 0.0264(19) 0.0331(19) 0.0017(15) 0.0044(16) -0.0038(15) C1 0.038(3) 0.046(3) 0.041(3) -0.003(2) -0.010(2) 0.001(2) C2 0.033(2) 0.033(2) 0.023(2) -0.0024(17) 0.0000(17) -0.0026(19) C3 0.031(2) 0.032(2) 0.027(2) 0.0011(18) -0.0006(18) -0.0023(18) C4 0.036(2) 0.029(2) 0.031(2) -0.0015(18) -0.0033(19) -0.0012(19) C5 0.044(3) 0.042(3) 0.062(3) 0.004(2) -0.018(3) -0.006(2) C6 0.059(3) 0.049(3) 0.045(3) -0.001(2) -0.019(2) -0.010(3) C7 0.032(2) 0.037(2) 0.026(2) -0.0022(18) -0.0095(18) 0.0026(19) C8 0.030(2) 0.037(2) 0.020(2) -0.0007(17) -0.0069(17) 0.0078(19) C9 0.036(2) 0.031(2) 0.027(2) 0.0006(18) -0.0071(18) 0.0044(19) C10 0.076(4) 0.035(3) 0.045(3) 0.003(2) -0.023(3) 0.007(3) C11 0.036(2) 0.043(3) 0.017(2) 0.0008(18) -0.0073(17) 0.005(2) C12 0.073(4) 0.037(3) 0.052(3) -0.004(2) -0.021(3) -0.001(3) C13 0.042(3) 0.031(2) 0.027(2) 0.0009(18) -0.0092(19) -0.007(2) C14 0.032(2) 0.040(2) 0.020(2) -0.0004(18) -0.0035(17) -0.0098(19) C15 0.035(2) 0.036(2) 0.027(2) 0.0002(18) -0.0095(18) -0.0023(19) C16 0.057(3) 0.060(3) 0.058(3) -0.015(3) -0.027(3) 0.016(3) C17 0.082(5) 0.169(7) 0.040(3) 0.005(4) -0.006(3) -0.087(5) C18 0.044(3) 0.075(4) 0.022(2) -0.001(2) -0.008(2) -0.028(3) C19 0.030(2) 0.041(2) 0.021(2) -0.0028(18) -0.0066(17) -0.0037(19) C20 0.034(2) 0.044(3) 0.021(2) -0.0046(18) -0.0034(17) -0.004(2) C21 0.057(3) 0.092(4) 0.029(3) -0.006(3) 0.008(2) -0.031(3) C22 0.069(4) 0.104(5) 0.036(3) -0.002(3) 0.003(3) 0.050(4) C23 0.044(3) 0.061(3) 0.023(2) 0.001(2) -0.0054(19) 0.023(2) C24 0.034(2) 0.051(3) 0.021(2) 0.0042(19) -0.0048(18) 0.012(2) C25 0.075(4) 0.074(4) 0.030(3) -0.002(2) 0.002(2) 0.039(3) C26 0.043(3) 0.072(4) 0.036(3) -0.011(2) 0.001(2) -0.007(3) C27 0.032(2) 0.045(3) 0.029(2) 0.006(2) -0.0016(18) -0.014(2) C28 0.028(2) 0.053(3) 0.029(2) 0.002(2) 0.0003(18) -0.017(2) C29 0.029(2) 0.071(3) 0.031(2) -0.008(2) 0.0035(19) -0.020(2) C30 0.054(4) 0.129(6) 0.041(3) -0.033(3) 0.009(3) -0.031(4) C31 0.028(3) 0.034(3) 0.030(3) 0.000 -0.003(2) 0.000 C32 0.027(3) 0.027(3) 0.030(3) 0.000 0.001(2) 0.000 C33 0.036(2) 0.030(2) 0.027(2) -0.0047(17) -0.0023(18) 0.0026(19) C34 0.046(3) 0.047(3) 0.050(3) -0.007(2) -0.017(2) 0.006(2) C35 0.095(5) 0.040(3) 0.060(4) 0.000(3) -0.037(3) 0.009(3) C36 0.044(3) 0.039(3) 0.027(2) 0.0012(19) -0.0155(19) 0.001(2) C37 0.032(2) 0.035(2) 0.021(2) -0.0021(17) -0.0057(17) -0.0048(19) C38 0.039(2) 0.033(2) 0.022(2) -0.0011(17) -0.0056(18) -0.0038(19) C39 0.074(4) 0.037(3) 0.046(3) 0.000(2) -0.018(3) -0.003(3) C40 0.075(4) 0.151(7) 0.038(3) -0.001(4) -0.002(3) -0.074(5) C41 0.047(3) 0.068(3) 0.024(2) -0.001(2) -0.003(2) -0.022(3) C42 0.036(2) 0.037(2) 0.020(2) 0.0018(17) -0.0069(17) -0.007(2) C43 0.032(2) 0.045(3) 0.020(2) -0.0045(18) -0.0014(17) -0.004(2) C44 0.054(3) 0.086(4) 0.032(3) -0.011(3) 0.010(2) -0.026(3) C45 0.051(3) 0.136(6) 0.039(3) -0.033(3) 0.008(3) -0.032(4) C46 0.032(3) 0.074(4) 0.029(2) -0.005(2) -0.0003(19) -0.021(2) C47 0.030(2) 0.057(3) 0.026(2) 0.002(2) 0.0004(18) -0.015(2) C48 0.031(2) 0.045(3) 0.032(2) 0.002(2) 0.0002(19) -0.012(2) C49 0.043(3) 0.066(4) 0.042(3) -0.013(2) 0.003(2) -0.010(3) C50 0.087(4) 0.084(4) 0.038(3) -0.008(3) 0.010(3) -0.051(4) C51 0.041(3) 0.051(3) 0.022(2) 0.0009(19) 0.0057(19) -0.016(2) C52 0.035(2) 0.043(3) 0.019(2) 0.0012(18) 0.0055(17) -0.006(2) C53 0.046(3) 0.061(3) 0.024(2) -0.001(2) 0.008(2) -0.020(2) C54 0.084(4) 0.105(5) 0.041(3) -0.011(3) 0.008(3) -0.060(4) C55 0.053(3) 0.037(3) 0.040(3) 0.004(2) 0.015(2) -0.002(2) C56 0.031(2) 0.029(2) 0.025(2) -0.0011(17) 0.0052(17) -0.0063(18) C57 0.034(2) 0.036(2) 0.019(2) 0.0009(17) 0.0039(17) -0.0083(19) C58 0.036(2) 0.039(3) 0.026(2) -0.0042(19) 0.0078(18) -0.003(2) C59 0.058(3) 0.048(3) 0.054(3) 0.001(2) 0.021(3) 0.013(3) C60 0.035(2) 0.033(2) 0.028(2) -0.0004(18) -0.0034(18) -0.0016(19) C61 0.042(3) 0.041(3) 0.053(3) 0.007(2) 0.011(2) 0.003(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 Cu1 N6 1.853(3) . ? Cu1 N1 1.861(3) . ? Cu2 N2 1.854(3) . ? Cu2 N3 1.854(3) . ? Cu3 N4 1.858(3) . ? Cu3 N5 1.860(3) . ? Cu4 N12 1.844(3) . ? Cu4 N8 1.850(3) . ? Cu5 N9 1.840(4) 12_656 ? Cu5 N7 1.844(3) . ? Cu6 N10 1.858(3) 12_656 ? Cu6 N11 1.858(3) . ? Cu7 N14 1.847(3) . ? Cu7 N13 1.854(3) . ? Cu7 Cu7 3.0207(11) 3_556 ? Cu8 N15 1.874(3) . ? Cu8 N15 1.874(3) 3_556 ? Cu9 N21 1.836(3) . ? Cu9 N16 1.840(3) . ? Cu10 N18 1.849(4) . ? Cu10 N17 1.852(3) . ? Cu11 N20 1.854(3) . ? Cu11 N19 1.856(3) . ? Cu12 N22 1.848(3) 3_557 ? Cu12 N22 1.848(3) . ? Cu13 N24 1.845(3) 9_557 ? Cu13 N23 1.850(3) . ? N1 C2 1.339(5) . ? N1 N2 1.363(5) . ? N2 C4 1.347(5) . ? N3 C7 1.337(5) . ? N3 N4 1.379(5) . ? N4 C9 1.349(5) . ? N5 C13 1.349(5) . ? N5 N6 1.376(5) . ? N6 C15 1.335(5) . ? N7 C18 1.345(5) . ? N7 N8 1.376(5) . ? N8 C20 1.330(5) . ? N9 C23 1.347(5) . ? N9 N10 1.370(5) . ? N9 Cu5 1.840(4) 12_655 ? N10 C24 1.341(5) . ? N10 Cu6 1.858(3) 12_655 ? N11 C27 1.338(5) . ? N11 N12 1.379(5) . ? N12 C29 1.333(5) . ? N13 C33 1.337(5) . ? N13 N13 1.364(7) 3_556 ? N14 C36 1.332(5) . ? N14 N15 1.375(5) . ? N15 C38 1.349(5) . ? N16 C41 1.340(5) . ? N16 N17 1.372(5) . ? N17 C43 1.339(5) . ? N18 C46 1.330(5) . ? N18 N19 1.373(5) . ? N19 C48 1.337(5) . ? N20 C51 1.339(5) . ? N20 N21 1.363(5) . ? N21 C53 1.350(5) . ? N22 C56 1.345(5) . ? N22 N23 1.377(5) . ? N23 C58 1.344(5) . ? N24 C60 1.340(5) . ? N24 N24 1.376(7) 3_556 ? N24 Cu13 1.845(3) 9_557 ? C1 C2 1.499(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.381(5) . ? C3 C4 1.392(6) . ? C3 C3 1.483(8) 8_465 ? C4 C5 1.495(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.490(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.390(6) . ? C8 C9 1.397(5) . ? C8 C11 1.480(5) . ? C9 C10 1.486(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C23 1.384(6) . ? C11 C24 1.386(6) . ? C12 C13 1.499(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.381(6) . ? C14 C15 1.387(6) . ? C14 C19 1.477(5) . ? C15 C16 1.496(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.482(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.381(6) . ? C19 C20 1.392(6) . ? C20 C21 1.495(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.497(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 C25 1.482(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.494(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.395(6) . ? C28 C29 1.393(6) . ? C28 C28 1.472(8) 2_675 ? C29 C30 1.506(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C60 1.388(5) . ? C31 C60 1.388(5) 3_556 ? C31 C32 1.477(8) . ? C32 C33 1.389(5) . ? C32 C33 1.389(5) 3_556 ? C33 C34 1.499(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.495(6) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.388(6) . ? C37 C38 1.388(5) . ? C37 C42 1.471(5) . ? C38 C39 1.491(6) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.487(7) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.383(6) . ? C42 C43 1.398(6) . ? C43 C44 1.480(6) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.496(6) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.398(6) . ? C47 C48 1.395(6) . ? C47 C47 1.473(8) 6 ? C48 C49 1.498(6) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.482(6) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.385(6) . ? C52 C53 1.378(6) . ? C52 C57 1.474(5) . ? C53 C54 1.500(7) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.485(6) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.384(5) . ? C57 C58 1.398(6) . ? C58 C59 1.488(6) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.491(6) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 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 N6 Cu1 N1 166.80(15) . . ? N2 Cu2 N3 169.21(16) . . ? N4 Cu3 N5 174.04(16) . . ? N12 Cu4 N8 176.49(19) . . ? N9 Cu5 N7 177.3(2) 12_656 . ? N10 Cu6 N11 168.07(19) 12_656 . ? N14 Cu7 N13 171.35(17) . . ? N14 Cu7 Cu7 119.03(11) . 3_556 ? N13 Cu7 Cu7 63.09(10) . 3_556 ? N15 Cu8 N15 175.6(2) . 3_556 ? N21 Cu9 N16 178.20(19) . . ? N18 Cu10 N17 175.93(19) . . ? N20 Cu11 N19 167.39(19) . . ? N22 Cu12 N22 177.4(2) 3_557 . ? N24 Cu13 N23 167.14(16) 9_557 . ? C2 N1 N2 108.1(3) . . ? C2 N1 Cu1 131.6(3) . . ? N2 N1 Cu1 119.0(3) . . ? C4 N2 N1 108.0(3) . . ? C4 N2 Cu2 136.5(3) . . ? N1 N2 Cu2 115.5(3) . . ? C7 N3 N4 108.2(3) . . ? C7 N3 Cu2 126.5(3) . . ? N4 N3 Cu2 123.2(2) . . ? C9 N4 N3 107.6(3) . . ? C9 N4 Cu3 133.1(3) . . ? N3 N4 Cu3 117.7(2) . . ? C13 N5 N6 107.6(3) . . ? C13 N5 Cu3 135.4(3) . . ? N6 N5 Cu3 117.0(2) . . ? C15 N6 N5 108.1(3) . . ? C15 N6 Cu1 129.2(3) . . ? N5 N6 Cu1 120.9(3) . . ? C18 N7 N8 107.9(3) . . ? C18 N7 Cu5 132.8(3) . . ? N8 N7 Cu5 118.8(3) . . ? C20 N8 N7 108.1(3) . . ? C20 N8 Cu4 134.1(3) . . ? N7 N8 Cu4 117.7(3) . . ? C23 N9 N10 107.9(3) . . ? C23 N9 Cu5 130.1(3) . 12_655 ? N10 N9 Cu5 121.0(3) . 12_655 ? C24 N10 N9 108.0(3) . . ? C24 N10 Cu6 130.7(3) . 12_655 ? N9 N10 Cu6 119.2(3) . 12_655 ? C27 N11 N12 107.6(3) . . ? C27 N11 Cu6 132.3(3) . . ? N12 N11 Cu6 117.3(3) . . ? C29 N12 N11 108.3(3) . . ? C29 N12 Cu4 130.7(3) . . ? N11 N12 Cu4 121.1(3) . . ? C33 N13 N13 108.1(2) . 3_556 ? C33 N13 Cu7 135.2(3) . . ? N13 N13 Cu7 115.71(12) 3_556 . ? C36 N14 N15 108.0(3) . . ? C36 N14 Cu7 127.6(3) . . ? N15 N14 Cu7 124.4(3) . . ? C38 N15 N14 107.5(3) . . ? C38 N15 Cu8 135.2(3) . . ? N14 N15 Cu8 116.4(2) . . ? C41 N16 N17 107.9(3) . . ? C41 N16 Cu9 133.2(3) . . ? N17 N16 Cu9 118.4(3) . . ? C43 N17 N16 108.3(3) . . ? C43 N17 Cu10 133.8(3) . . ? N16 N17 Cu10 117.8(3) . . ? C46 N18 N19 108.7(3) . . ? C46 N18 Cu10 130.4(3) . . ? N19 N18 Cu10 120.9(3) . . ? C48 N19 N18 107.9(3) . . ? C48 N19 Cu11 131.5(3) . . ? N18 N19 Cu11 117.6(3) . . ? C51 N20 N21 107.9(3) . . ? C51 N20 Cu11 131.5(3) . . ? N21 N20 Cu11 119.1(3) . . ? C53 N21 N20 108.1(3) . . ? C53 N21 Cu9 130.1(3) . . ? N20 N21 Cu9 121.5(3) . . ? C56 N22 N23 108.2(3) . . ? C56 N22 Cu12 133.5(3) . . ? N23 N22 Cu12 117.4(2) . . ? C58 N23 N22 107.9(3) . . ? C58 N23 Cu13 127.6(3) . . ? N22 N23 Cu13 120.6(2) . . ? C60 N24 N24 107.8(2) . 3_556 ? C60 N24 Cu13 133.6(3) . 9_557 ? N24 N24 Cu13 117.82(12) 3_556 9_557 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.9(4) . . ? N1 C2 C1 120.8(4) . . ? C3 C2 C1 129.2(4) . . ? C2 C3 C4 104.7(4) . . ? C2 C3 C3 127.5(3) . 8_465 ? C4 C3 C3 127.8(3) . 8_465 ? N2 C4 C3 109.3(4) . . ? N2 C4 C5 120.4(4) . . ? C3 C4 C5 130.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 110.0(4) . . ? N3 C7 C6 120.6(4) . . ? C8 C7 C6 129.3(4) . . ? C7 C8 C9 104.6(3) . . ? C7 C8 C11 127.0(4) . . ? C9 C8 C11 128.4(4) . . ? N4 C9 C8 109.6(4) . . ? N4 C9 C10 121.2(4) . . ? C8 C9 C10 129.1(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C23 C11 C24 105.1(4) . . ? C23 C11 C8 126.6(4) . . ? C24 C11 C8 128.1(4) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 109.5(4) . . ? N5 C13 C12 122.0(4) . . ? C14 C13 C12 128.6(4) . . ? C13 C14 C15 105.2(4) . . ? C13 C14 C19 128.7(4) . . ? C15 C14 C19 126.1(4) . . ? N6 C15 C14 109.7(4) . . ? N6 C15 C16 122.3(4) . . ? C14 C15 C16 128.0(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 109.3(4) . . ? N7 C18 C17 121.0(4) . . ? C19 C18 C17 129.7(4) . . ? C18 C19 C20 105.1(3) . . ? C18 C19 C14 127.4(4) . . ? C20 C19 C14 127.4(4) . . ? N8 C20 C19 109.6(4) . . ? N8 C20 C21 121.7(4) . . ? C19 C20 C21 128.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C11 109.4(4) . . ? N9 C23 C22 120.3(4) . . ? C11 C23 C22 130.3(4) . . ? N10 C24 C11 109.6(4) . . ? N10 C24 C25 121.0(4) . . ? C11 C24 C25 129.5(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N11 C27 C28 109.9(4) . . ? N11 C27 C26 119.8(4) . . ? C28 C27 C26 130.2(4) . . ? C29 C28 C27 104.4(4) . . ? C29 C28 C28 126.8(3) . 2_675 ? C27 C28 C28 128.8(3) . 2_675 ? N12 C29 C28 109.8(4) . . ? N12 C29 C30 119.7(4) . . ? C28 C29 C30 130.5(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C60 C31 C60 104.6(5) . 3_556 ? C60 C31 C32 127.7(3) . . ? C60 C31 C32 127.7(3) 3_556 . ? C33 C32 C33 104.3(5) . 3_556 ? C33 C32 C31 127.8(3) . . ? C33 C32 C31 127.8(3) 3_556 . ? N13 C33 C32 109.8(4) . . ? N13 C33 C34 121.4(4) . . ? C32 C33 C34 128.8(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N14 C36 C37 110.4(4) . . ? N14 C36 C35 121.0(4) . . ? C37 C36 C35 128.6(4) . . ? C38 C37 C36 104.3(3) . . ? C38 C37 C42 129.1(4) . . ? C36 C37 C42 126.6(4) . . ? N15 C38 C37 109.9(4) . . ? N15 C38 C39 121.4(4) . . ? C37 C38 C39 128.7(4) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N16 C41 C42 109.7(4) . . ? N16 C41 C40 120.4(4) . . ? C42 C41 C40 129.8(4) . . ? C41 C42 C43 104.9(4) . . ? C41 C42 C37 128.3(4) . . ? C43 C42 C37 126.7(4) . . ? N17 C43 C42 109.1(4) . . ? N17 C43 C44 121.5(4) . . ? C42 C43 C44 129.4(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N18 C46 C47 109.2(4) . . ? N18 C46 C45 120.8(4) . . ? C47 C46 C45 129.9(4) . . ? C48 C47 C46 104.6(4) . . ? C48 C47 C47 128.4(3) . 6 ? C46 C47 C47 127.0(3) . 6 ? N19 C48 C47 109.5(4) . . ? N19 C48 C49 120.2(4) . . ? C47 C48 C49 130.3(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N20 C51 C52 109.6(4) . . ? N20 C51 C50 121.8(4) . . ? C52 C51 C50 128.6(4) . . ? C53 C52 C51 105.1(4) . . ? C53 C52 C57 126.6(4) . . ? C51 C52 C57 128.2(4) . . ? N21 C53 C52 109.2(4) . . ? N21 C53 C54 121.1(4) . . ? C52 C53 C54 129.6(4) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N22 C56 C57 109.4(4) . . ? N22 C56 C55 121.9(4) . . ? C57 C56 C55 128.6(4) . . ? C56 C57 C58 105.2(3) . . ? C56 C57 C52 128.6(4) . . ? C58 C57 C52 126.1(4) . . ? N23 C58 C57 109.2(4) . . ? N23 C58 C59 121.2(4) . . ? C57 C58 C59 129.5(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N24 C60 C31 109.9(4) . . ? N24 C60 C61 119.9(4) . . ? C31 C60 C61 130.1(4) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? 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 N6 Cu1 N1 C2 -69.3(9) . . . . ? N6 Cu1 N1 N2 96.2(7) . . . . ? C2 N1 N2 C4 -0.4(4) . . . . ? Cu1 N1 N2 C4 -169.1(3) . . . . ? C2 N1 N2 Cu2 -177.8(3) . . . . ? Cu1 N1 N2 Cu2 13.6(4) . . . . ? N3 Cu2 N2 C4 -100.5(9) . . . . ? N3 Cu2 N2 N1 75.8(9) . . . . ? N2 Cu2 N3 C7 64.1(10) . . . . ? N2 Cu2 N3 N4 -97.7(8) . . . . ? C7 N3 N4 C9 0.2(5) . . . . ? Cu2 N3 N4 C9 164.9(3) . . . . ? C7 N3 N4 Cu3 -167.3(3) . . . . ? Cu2 N3 N4 Cu3 -2.6(4) . . . . ? N5 Cu3 N4 C9 -99.5(15) . . . . ? N5 Cu3 N4 N3 64.1(16) . . . . ? N4 Cu3 N5 C13 146.0(14) . . . . ? N4 Cu3 N5 N6 -37.7(16) . . . . ? C13 N5 N6 C15 0.1(5) . . . . ? Cu3 N5 N6 C15 -177.2(3) . . . . ? C13 N5 N6 Cu1 166.3(3) . . . . ? Cu3 N5 N6 Cu1 -11.0(4) . . . . ? N1 Cu1 N6 C15 59.6(9) . . . . ? N1 Cu1 N6 N5 -103.4(7) . . . . ? N9 Cu5 N7 C18 67(4) 12_656 . . . ? N9 Cu5 N7 N8 -123(4) 12_656 . . . ? C18 N7 N8 C20 -0.5(6) . . . . ? Cu5 N7 N8 C20 -172.7(3) . . . . ? C18 N7 N8 Cu4 177.2(4) . . . . ? Cu5 N7 N8 Cu4 5.0(5) . . . . ? N12 Cu4 N8 C20 -79(3) . . . . ? N12 Cu4 N8 N7 104(3) . . . . ? C23 N9 N10 C24 0.5(6) . . . . ? Cu5 N9 N10 C24 170.4(3) 12_655 . . . ? C23 N9 N10 Cu6 -164.7(3) . . . 12_655 ? Cu5 N9 N10 Cu6 5.2(5) 12_655 . . 12_655 ? N10 Cu6 N11 C27 -83.9(9) 12_656 . . . ? N10 Cu6 N11 N12 74.7(8) 12_656 . . . ? C27 N11 N12 C29 -0.8(5) . . . . ? Cu6 N11 N12 C29 -164.4(3) . . . . ? C27 N11 N12 Cu4 -179.7(3) . . . . ? Cu6 N11 N12 Cu4 16.7(5) . . . . ? N8 Cu4 N12 C29 53(3) . . . . ? N8 Cu4 N12 N11 -129(3) . . . . ? N14 Cu7 N13 C33 -71.9(12) . . . . ? Cu7 Cu7 N13 C33 -178.3(5) 3_556 . . . ? N14 Cu7 N13 N13 95.1(11) . . . 3_556 ? Cu7 Cu7 N13 N13 -11.3(3) 3_556 . . 3_556 ? N13 Cu7 N14 C36 57.2(13) . . . . ? Cu7 Cu7 N14 C36 159.1(4) 3_556 . . . ? N13 Cu7 N14 N15 -121.7(10) . . . . ? Cu7 Cu7 N14 N15 -19.8(4) 3_556 . . . ? C36 N14 N15 C38 1.0(5) . . . . ? Cu7 N14 N15 C38 -179.9(3) . . . . ? C36 N14 N15 Cu8 -170.1(3) . . . . ? Cu7 N14 N15 Cu8 9.0(5) . . . . ? N15 Cu8 N15 C38 -167.9(4) 3_556 . . . ? N15 Cu8 N15 N14 -0.1(3) 3_556 . . . ? N21 Cu9 N16 C41 48(7) . . . . ? N21 Cu9 N16 N17 -141(6) . . . . ? C41 N16 N17 C43 0.4(6) . . . . ? Cu9 N16 N17 C43 -172.7(3) . . . . ? C41 N16 N17 Cu10 179.2(3) . . . . ? Cu9 N16 N17 Cu10 6.1(5) . . . . ? N18 Cu10 N17 C43 -85(2) . . . . ? N18 Cu10 N17 N16 96(2) . . . . ? N17 Cu10 N18 C46 57(2) . . . . ? N17 Cu10 N18 N19 -122(2) . . . . ? C46 N18 N19 C48 -0.3(6) . . . . ? Cu10 N18 N19 C48 178.9(3) . . . . ? C46 N18 N19 Cu11 -163.0(3) . . . . ? Cu10 N18 N19 Cu11 16.3(5) . . . . ? N20 Cu11 N19 C48 -82.7(9) . . . . ? N20 Cu11 N19 N18 75.0(8) . . . . ? N19 Cu11 N20 C51 84.4(9) . . . . ? N19 Cu11 N20 N21 -79.4(8) . . . . ? C51 N20 N21 C53 0.2(6) . . . . ? Cu11 N20 N21 C53 167.5(3) . . . . ? C51 N20 N21 Cu9 -174.3(3) . . . . ? Cu11 N20 N21 Cu9 -7.0(5) . . . . ? N16 Cu9 N21 C53 -23(7) . . . . ? N16 Cu9 N21 N20 150(6) . . . . ? N22 Cu12 N22 C56 149.2(4) 3_557 . . . ? N22 Cu12 N22 N23 -18.1(3) 3_557 . . . ? C56 N22 N23 C58 0.8(5) . . . . ? Cu12 N22 N23 C58 171.1(3) . . . . ? C56 N22 N23 Cu13 -158.5(3) . . . . ? Cu12 N22 N23 Cu13 11.8(4) . . . . ? N24 Cu13 N23 C58 -60.8(9) 9_557 . . . ? N24 Cu13 N23 N22 94.0(7) 9_557 . . . ? N2 N1 C2 C3 -0.1(5) . . . . ? Cu1 N1 C2 C3 166.6(3) . . . . ? N2 N1 C2 C1 -179.2(4) . . . . ? Cu1 N1 C2 C1 -12.5(6) . . . . ? N1 C2 C3 C4 0.6(5) . . . . ? C1 C2 C3 C4 179.6(4) . . . . ? N1 C2 C3 C3 179.5(4) . . . 8_465 ? C1 C2 C3 C3 -1.5(8) . . . 8_465 ? N1 N2 C4 C3 0.8(5) . . . . ? Cu2 N2 C4 C3 177.3(3) . . . . ? N1 N2 C4 C5 -176.8(4) . . . . ? Cu2 N2 C4 C5 -0.3(7) . . . . ? C2 C3 C4 N2 -0.8(5) . . . . ? C3 C3 C4 N2 -179.7(4) 8_465 . . . ? C2 C3 C4 C5 176.5(5) . . . . ? C3 C3 C4 C5 -2.4(8) 8_465 . . . ? N4 N3 C7 C8 -0.4(5) . . . . ? Cu2 N3 C7 C8 -164.4(3) . . . . ? N4 N3 C7 C6 -178.7(4) . . . . ? Cu2 N3 C7 C6 17.3(6) . . . . ? N3 C7 C8 C9 0.4(5) . . . . ? C6 C7 C8 C9 178.5(5) . . . . ? N3 C7 C8 C11 179.3(4) . . . . ? C6 C7 C8 C11 -2.7(8) . . . . ? N3 N4 C9 C8 0.0(5) . . . . ? Cu3 N4 C9 C8 164.8(3) . . . . ? N3 N4 C9 C10 179.2(4) . . . . ? Cu3 N4 C9 C10 -16.0(7) . . . . ? C7 C8 C9 N4 -0.3(5) . . . . ? C11 C8 C9 N4 -179.1(4) . . . . ? C7 C8 C9 C10 -179.4(5) . . . . ? C11 C8 C9 C10 1.8(8) . . . . ? C7 C8 C11 C23 -55.0(7) . . . . ? C9 C8 C11 C23 123.6(5) . . . . ? C7 C8 C11 C24 119.4(5) . . . . ? C9 C8 C11 C24 -62.0(7) . . . . ? N6 N5 C13 C14 -0.1(5) . . . . ? Cu3 N5 C13 C14 176.5(3) . . . . ? N6 N5 C13 C12 178.9(4) . . . . ? Cu3 N5 C13 C12 -4.5(7) . . . . ? N5 C13 C14 C15 0.1(5) . . . . ? C12 C13 C14 C15 -178.9(5) . . . . ? N5 C13 C14 C19 -177.7(4) . . . . ? C12 C13 C14 C19 3.3(8) . . . . ? N5 N6 C15 C14 -0.1(5) . . . . ? Cu1 N6 C15 C14 -164.8(3) . . . . ? N5 N6 C15 C16 179.9(4) . . . . ? Cu1 N6 C15 C16 15.2(7) . . . . ? C13 C14 C15 N6 0.0(5) . . . . ? C19 C14 C15 N6 177.8(4) . . . . ? C13 C14 C15 C16 -180.0(5) . . . . ? C19 C14 C15 C16 -2.2(7) . . . . ? N8 N7 C18 C19 0.4(6) . . . . ? Cu5 N7 C18 C19 171.1(4) . . . . ? N8 N7 C18 C17 -180.0(6) . . . . ? Cu5 N7 C18 C17 -9.2(9) . . . . ? N7 C18 C19 C20 -0.1(6) . . . . ? C17 C18 C19 C20 -179.7(6) . . . . ? N7 C18 C19 C14 179.3(4) . . . . ? C17 C18 C19 C14 -0.3(10) . . . . ? C13 C14 C19 C18 91.7(6) . . . . ? C15 C14 C19 C18 -85.6(6) . . . . ? C13 C14 C19 C20 -89.0(6) . . . . ? C15 C14 C19 C20 93.7(6) . . . . ? N7 N8 C20 C19 0.4(5) . . . . ? Cu4 N8 C20 C19 -176.8(3) . . . . ? N7 N8 C20 C21 -179.6(5) . . . . ? Cu4 N8 C20 C21 3.3(7) . . . . ? C18 C19 C20 N8 -0.2(5) . . . . ? C14 C19 C20 N8 -179.6(4) . . . . ? C18 C19 C20 C21 179.8(5) . . . . ? C14 C19 C20 C21 0.4(8) . . . . ? N10 N9 C23 C11 -0.7(6) . . . . ? Cu5 N9 C23 C11 -169.4(4) 12_655 . . . ? N10 N9 C23 C22 -179.2(5) . . . . ? Cu5 N9 C23 C22 12.1(8) 12_655 . . . ? C24 C11 C23 N9 0.7(6) . . . . ? C8 C11 C23 N9 176.2(4) . . . . ? C24 C11 C23 C22 179.0(6) . . . . ? C8 C11 C23 C22 -5.6(9) . . . . ? N9 N10 C24 C11 0.0(5) . . . . ? Cu6 N10 C24 C11 162.9(3) 12_655 . . . ? N9 N10 C24 C25 -179.9(5) . . . . ? Cu6 N10 C24 C25 -17.1(7) 12_655 . . . ? C23 C11 C24 N10 -0.4(5) . . . . ? C8 C11 C24 N10 -175.8(4) . . . . ? C23 C11 C24 C25 179.5(5) . . . . ? C8 C11 C24 C25 4.2(8) . . . . ? N12 N11 C27 C28 1.1(5) . . . . ? Cu6 N11 C27 C28 161.2(4) . . . . ? N12 N11 C27 C26 -178.0(4) . . . . ? Cu6 N11 C27 C26 -17.9(7) . . . . ? N11 C27 C28 C29 -1.0(5) . . . . ? C26 C27 C28 C29 178.0(5) . . . . ? N11 C27 C28 C28 177.1(6) . . . 2_675 ? C26 C27 C28 C28 -3.9(10) . . . 2_675 ? N11 N12 C29 C28 0.2(6) . . . . ? Cu4 N12 C29 C28 178.9(4) . . . . ? N11 N12 C29 C30 177.8(5) . . . . ? Cu4 N12 C29 C30 -3.5(8) . . . . ? C27 C28 C29 N12 0.5(6) . . . . ? C28 C28 C29 N12 -177.7(6) 2_675 . . . ? C27 C28 C29 C30 -176.8(6) . . . . ? C28 C28 C29 C30 5.1(10) 2_675 . . . ? C60 C31 C32 C33 122.0(3) . . . . ? C60 C31 C32 C33 -58.0(3) 3_556 . . . ? C60 C31 C32 C33 -58.0(3) . . . 3_556 ? C60 C31 C32 C33 122.0(3) 3_556 . . 3_556 ? N13 N13 C33 C32 0.6(5) 3_556 . . . ? Cu7 N13 C33 C32 168.3(3) . . . . ? N13 N13 C33 C34 -179.2(4) 3_556 . . . ? Cu7 N13 C33 C34 -11.5(7) . . . . ? C33 C32 C33 N13 -0.2(2) 3_556 . . . ? C31 C32 C33 N13 179.8(2) . . . . ? C33 C32 C33 C34 179.5(5) 3_556 . . . ? C31 C32 C33 C34 -0.5(5) . . . . ? N15 N14 C36 C37 -0.5(5) . . . . ? Cu7 N14 C36 C37 -179.5(3) . . . . ? N15 N14 C36 C35 179.9(5) . . . . ? Cu7 N14 C36 C35 0.8(7) . . . . ? N14 C36 C37 C38 -0.2(5) . . . . ? C35 C36 C37 C38 179.5(5) . . . . ? N14 C36 C37 C42 -179.5(4) . . . . ? C35 C36 C37 C42 0.1(8) . . . . ? N14 N15 C38 C37 -1.1(5) . . . . ? Cu8 N15 C38 C37 167.5(3) . . . . ? N14 N15 C38 C39 179.1(4) . . . . ? Cu8 N15 C38 C39 -12.4(7) . . . . ? C36 C37 C38 N15 0.8(5) . . . . ? C42 C37 C38 N15 -180.0(4) . . . . ? C36 C37 C38 C39 -179.4(5) . . . . ? C42 C37 C38 C39 -0.1(8) . . . . ? N17 N16 C41 C42 -0.2(6) . . . . ? Cu9 N16 C41 C42 171.5(4) . . . . ? N17 N16 C41 C40 -179.2(5) . . . . ? Cu9 N16 C41 C40 -7.5(9) . . . . ? N16 C41 C42 C43 0.0(6) . . . . ? C40 C41 C42 C43 178.8(6) . . . . ? N16 C41 C42 C37 177.0(5) . . . . ? C40 C41 C42 C37 -4.1(9) . . . . ? C38 C37 C42 C41 118.1(6) . . . . ? C36 C37 C42 C41 -62.7(7) . . . . ? C38 C37 C42 C43 -65.4(7) . . . . ? C36 C37 C42 C43 113.7(5) . . . . ? N16 N17 C43 C42 -0.4(5) . . . . ? Cu10 N17 C43 C42 -179.0(3) . . . . ? N16 N17 C43 C44 -179.9(5) . . . . ? Cu10 N17 C43 C44 1.6(7) . . . . ? C41 C42 C43 N17 0.3(5) . . . . ? C37 C42 C43 N17 -176.8(4) . . . . ? C41 C42 C43 C44 179.6(5) . . . . ? C37 C42 C43 C44 2.5(8) . . . . ? N19 N18 C46 C47 -0.3(6) . . . . ? Cu10 N18 C46 C47 -179.5(4) . . . . ? N19 N18 C46 C45 177.8(5) . . . . ? Cu10 N18 C46 C45 -1.4(8) . . . . ? N18 C46 C47 C48 0.8(6) . . . . ? C45 C46 C47 C48 -177.1(6) . . . . ? N18 C46 C47 C47 -179.0(6) . . . 6 ? C45 C46 C47 C47 3.1(10) . . . 6 ? N18 N19 C48 C47 0.9(5) . . . . ? Cu11 N19 C48 C47 160.2(4) . . . . ? N18 N19 C48 C49 -179.2(4) . . . . ? Cu11 N19 C48 C49 -19.9(7) . . . . ? C46 C47 C48 N19 -1.0(5) . . . . ? C47 C47 C48 N19 178.8(6) 6 . . . ? C46 C47 C48 C49 179.0(5) . . . . ? C47 C47 C48 C49 -1.1(10) 6 . . . ? N21 N20 C51 C52 -0.6(6) . . . . ? Cu11 N20 C51 C52 -165.7(4) . . . . ? N21 N20 C51 C50 178.1(5) . . . . ? Cu11 N20 C51 C50 13.0(8) . . . . ? N20 C51 C52 C53 0.8(6) . . . . ? C50 C51 C52 C53 -177.8(5) . . . . ? N20 C51 C52 C57 179.1(4) . . . . ? C50 C51 C52 C57 0.5(9) . . . . ? N20 N21 C53 C52 0.3(6) . . . . ? Cu9 N21 C53 C52 174.1(4) . . . . ? N20 N21 C53 C54 -180.0(5) . . . . ? Cu9 N21 C53 C54 -6.1(8) . . . . ? C51 C52 C53 N21 -0.6(6) . . . . ? C57 C52 C53 N21 -179.0(4) . . . . ? C51 C52 C53 C54 179.7(6) . . . . ? C57 C52 C53 C54 1.3(9) . . . . ? N23 N22 C56 C57 -0.6(5) . . . . ? Cu12 N22 C56 C57 -168.7(3) . . . . ? N23 N22 C56 C55 177.6(4) . . . . ? Cu12 N22 C56 C55 9.4(6) . . . . ? N22 C56 C57 C58 0.1(5) . . . . ? C55 C56 C57 C58 -177.8(4) . . . . ? N22 C56 C57 C52 177.6(4) . . . . ? C55 C56 C57 C52 -0.3(7) . . . . ? C53 C52 C57 C56 -111.6(6) . . . . ? C51 C52 C57 C56 70.4(7) . . . . ? C53 C52 C57 C58 65.4(7) . . . . ? C51 C52 C57 C58 -112.6(6) . . . . ? N22 N23 C58 C57 -0.7(5) . . . . ? Cu13 N23 C58 C57 156.7(3) . . . . ? N22 N23 C58 C59 -179.9(4) . . . . ? Cu13 N23 C58 C59 -22.5(6) . . . . ? C56 C57 C58 N23 0.4(5) . . . . ? C52 C57 C58 N23 -177.2(4) . . . . ? C56 C57 C58 C59 179.5(5) . . . . ? C52 C57 C58 C59 1.9(8) . . . . ? N24 N24 C60 C31 0.6(5) 3_556 . . . ? Cu13 N24 C60 C31 170.2(3) 9_557 . . . ? N24 N24 C60 C61 -176.9(4) 3_556 . . . ? Cu13 N24 C60 C61 -7.3(6) 9_557 . . . ? C60 C31 C60 N24 -0.2(2) 3_556 . . . ? C32 C31 C60 N24 179.8(2) . . . . ? C60 C31 C60 C61 177.0(5) 3_556 . . . ? C32 C31 C60 C61 -3.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.098 #End of Crystallographic Information File #====================================== data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 295579' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cu3 N6' _chemical_formula_weight 476.00 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' _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 8.5774(8) _cell_length_b 10.2884(10) _cell_length_c 11.4238(11) _cell_angle_alpha 69.5260(10) _cell_angle_beta 75.178(2) _cell_angle_gamma 81.239(2) _cell_volume 910.82(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 3.479 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4425 _exptl_absorpt_correction_T_max 0.5732 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD' _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7160 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0343 _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 -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3549 _reflns_number_gt 3092 _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^)+(0.0537P)^2^+0.1369P] 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 3549 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.62726(4) 0.91453(3) 0.23600(3) 0.04259(12) Uani 1 1 d . . . Cu2 Cu 0.47450(4) 0.77698(4) 0.53378(3) 0.04073(12) Uani 1 1 d . . . N1 N 0.2347(3) 0.9957(2) 0.5422(2) 0.0378(5) Uani 1 1 d . . . N2 N 0.2945(3) 0.8667(2) 0.6102(2) 0.0368(5) Uani 1 1 d . . . N3 N 0.6396(3) 0.6783(2) 0.4524(2) 0.0409(5) Uani 1 1 d . . . N4 N 0.7033(3) 0.7381(2) 0.3242(2) 0.0395(5) Uani 1 1 d . . . N5 N 0.5441(3) 1.0841(2) 0.1411(2) 0.0406(5) Uani 1 1 d . . . N6 N 0.4170(3) 1.1565(2) 0.1987(2) 0.0406(5) Uani 1 1 d . . . C1 C 0.0037(4) 1.1651(3) 0.5686(3) 0.0514(8) Uani 1 1 d . . . H1A H 0.0121 1.1884 0.4782 0.077 Uiso 1 1 calc R . . H1B H 0.0459 1.2370 0.5845 0.077 Uiso 1 1 calc R . . H1C H -0.1076 1.1564 0.6124 0.077 Uiso 1 1 calc R . . C2 C 0.0985(3) 1.0302(3) 0.6161(3) 0.0400(6) Uani 1 1 d . . . C3 C 0.0698(4) 0.9248(3) 0.7323(3) 0.0448(7) Uani 1 1 d . . . H3A H -0.0162 0.9223 0.8016 0.054 Uiso 1 1 calc R . . C4 C 0.1940(4) 0.8241(3) 0.7249(3) 0.0414(6) Uani 1 1 d . . . C5 C 0.2291(4) 0.6872(3) 0.8221(3) 0.0514(7) Uani 1 1 d . . . H5A H 0.3357 0.6838 0.8358 0.077 Uiso 1 1 calc R . . H5B H 0.2226 0.6129 0.7914 0.077 Uiso 1 1 calc R . . H5C H 0.1513 0.6773 0.9013 0.077 Uiso 1 1 calc R . . C6 C 0.6656(5) 0.4570(4) 0.6269(3) 0.0607(9) Uani 1 1 d . . . H6A H 0.5720 0.4986 0.6712 0.091 Uiso 1 1 calc R . . H6B H 0.7538 0.4453 0.6680 0.091 Uiso 1 1 calc R . . H6C H 0.6418 0.3680 0.6288 0.091 Uiso 1 1 calc R . . C7 C 0.7111(4) 0.5494(3) 0.4908(3) 0.0442(7) Uani 1 1 d . . . C8 C 0.8217(4) 0.5263(3) 0.3879(3) 0.0488(7) Uani 1 1 d . . . H8A H 0.8883 0.4461 0.3876 0.059 Uiso 1 1 calc R . . C9 C 0.8137(3) 0.6457(3) 0.2857(3) 0.0432(7) Uani 1 1 d . . . C10 C 0.9057(4) 0.6818(4) 0.1496(3) 0.0613(9) Uani 1 1 d . . . H10A H 0.8762 0.7763 0.1035 0.092 Uiso 1 1 calc R . . H10B H 0.8805 0.6209 0.1107 0.092 Uiso 1 1 calc R . . H10C H 1.0196 0.6714 0.1470 0.092 Uiso 1 1 calc R . . C11 C 0.7131(4) 1.1006(4) -0.0732(3) 0.0618(9) Uani 1 1 d . . . H11A H 0.7118 1.1560 -0.1603 0.093 Uiso 1 1 calc R . . H11B H 0.6980 1.0057 -0.0605 0.093 Uiso 1 1 calc R . . H11C H 0.8151 1.1057 -0.0554 0.093 Uiso 1 1 calc R . . C12 C 0.5789(4) 1.1547(3) 0.0156(3) 0.0450(7) Uani 1 1 d . . . C13 C 0.2415(4) 1.3718(3) 0.1393(3) 0.0617(9) Uani 1 1 d . . . H13A H 0.1990 1.3419 0.2302 0.093 Uiso 1 1 calc R . . H13B H 0.1573 1.3763 0.0962 0.093 Uiso 1 1 calc R . . H13C H 0.2818 1.4621 0.1124 0.093 Uiso 1 1 calc R . . C14 C 0.3759(4) 1.2706(3) 0.1068(3) 0.0449(7) Uani 1 1 d . . . C15 C 0.4748(4) 1.2726(3) -0.0093(3) 0.0500(7) Uani 1 1 d . . . H15A H 0.4722 1.3398 -0.0885 0.060 Uiso 1 1 calc R . . Cu3 Cu 0.33317(4) 1.08127(3) 0.37252(3) 0.04105(12) 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 0.0462(2) 0.0356(2) 0.0396(2) -0.00721(15) -0.00887(16) 0.00303(15) Cu2 0.0407(2) 0.0405(2) 0.0370(2) -0.01317(15) -0.00560(15) 0.00575(15) N1 0.0425(13) 0.0354(12) 0.0341(12) -0.0110(10) -0.0088(10) 0.0017(10) N2 0.0383(12) 0.0385(12) 0.0309(11) -0.0106(9) -0.0067(9) 0.0027(9) N3 0.0425(13) 0.0361(12) 0.0392(13) -0.0108(10) -0.0066(10) 0.0037(10) N4 0.0400(13) 0.0363(12) 0.0371(13) -0.0100(10) -0.0046(10) 0.0009(10) N5 0.0428(13) 0.0396(13) 0.0336(12) -0.0074(10) -0.0064(10) -0.0007(10) N6 0.0449(13) 0.0379(12) 0.0325(12) -0.0049(10) -0.0079(10) -0.0004(10) C1 0.0477(17) 0.0488(18) 0.058(2) -0.0217(15) -0.0156(15) 0.0116(14) C2 0.0391(15) 0.0403(15) 0.0431(16) -0.0191(12) -0.0073(12) 0.0004(12) C3 0.0467(17) 0.0462(17) 0.0379(15) -0.0161(13) 0.0002(13) -0.0025(13) C4 0.0441(16) 0.0458(16) 0.0308(14) -0.0112(12) -0.0037(12) -0.0038(12) C5 0.0572(19) 0.0483(17) 0.0379(16) -0.0038(13) -0.0052(14) -0.0050(14) C6 0.076(2) 0.0480(18) 0.0488(19) -0.0078(15) -0.0163(17) 0.0072(16) C7 0.0517(18) 0.0376(15) 0.0433(16) -0.0114(13) -0.0175(14) 0.0052(13) C8 0.0508(18) 0.0377(16) 0.0572(19) -0.0180(14) -0.0148(15) 0.0111(13) C9 0.0402(15) 0.0428(16) 0.0478(17) -0.0194(13) -0.0089(13) 0.0036(12) C10 0.064(2) 0.059(2) 0.052(2) -0.0202(16) 0.0015(16) 0.0033(17) C11 0.058(2) 0.072(2) 0.0468(19) -0.0170(17) 0.0027(16) -0.0062(17) C12 0.0483(17) 0.0489(17) 0.0316(14) -0.0052(12) -0.0049(12) -0.0100(13) C13 0.069(2) 0.0489(19) 0.060(2) -0.0122(16) -0.0196(18) 0.0133(16) C14 0.0509(18) 0.0391(15) 0.0402(16) -0.0043(12) -0.0148(13) -0.0019(13) C15 0.058(2) 0.0493(18) 0.0320(15) 0.0003(13) -0.0092(14) -0.0077(15) Cu3 0.0473(2) 0.0393(2) 0.03003(19) -0.00629(15) -0.00572(15) -0.00053(15) _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 N5 1.850(2) . ? Cu1 N4 1.852(2) . ? Cu2 N2 1.854(2) . ? Cu2 N3 1.858(2) . ? Cu2 Cu3 2.9534(5) 2_676 ? N1 C2 1.335(3) . ? N1 N2 1.379(3) . ? N1 Cu3 1.855(2) . ? N2 C4 1.337(3) . ? N3 C7 1.345(4) . ? N3 N4 1.373(3) . ? N4 C9 1.341(4) . ? N5 C12 1.339(4) . ? N5 N6 1.380(3) . ? N6 C14 1.344(4) . ? N6 Cu3 1.850(2) . ? C1 C2 1.496(4) . ? C2 C3 1.380(4) . ? C3 C4 1.376(4) . ? C4 C5 1.502(4) . ? C6 C7 1.497(4) . ? C7 C8 1.377(4) . ? C8 C9 1.375(4) . ? C9 C10 1.496(4) . ? C11 C12 1.505(4) . ? C12 C15 1.382(5) . ? C13 C14 1.495(4) . ? C14 C15 1.374(4) . ? Cu3 Cu2 2.9534(5) 2_676 ? 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 N5 Cu1 N4 175.42(11) . . ? N2 Cu2 N3 173.91(11) . . ? N2 Cu2 Cu3 86.23(7) . 2_676 ? N3 Cu2 Cu3 99.85(8) . 2_676 ? C2 N1 N2 108.0(2) . . ? C2 N1 Cu3 131.5(2) . . ? N2 N1 Cu3 120.27(17) . . ? C4 N2 N1 108.0(2) . . ? C4 N2 Cu2 131.2(2) . . ? N1 N2 Cu2 120.59(17) . . ? C7 N3 N4 108.0(2) . . ? C7 N3 Cu2 133.3(2) . . ? N4 N3 Cu2 118.50(18) . . ? C9 N4 N3 107.7(2) . . ? C9 N4 Cu1 131.9(2) . . ? N3 N4 Cu1 120.33(18) . . ? C12 N5 N6 108.0(2) . . ? C12 N5 Cu1 131.4(2) . . ? N6 N5 Cu1 120.49(17) . . ? C14 N6 N5 107.7(2) . . ? C14 N6 Cu3 133.5(2) . . ? N5 N6 Cu3 118.66(17) . . ? N1 C2 C3 108.9(3) . . ? N1 C2 C1 120.8(3) . . ? C3 C2 C1 130.3(3) . . ? C4 C3 C2 106.2(3) . . ? N2 C4 C3 108.9(3) . . ? N2 C4 C5 120.5(3) . . ? C3 C4 C5 130.6(3) . . ? N3 C7 C8 108.8(3) . . ? N3 C7 C6 120.6(3) . . ? C8 C7 C6 130.5(3) . . ? C9 C8 C7 106.1(3) . . ? N4 C9 C8 109.3(3) . . ? N4 C9 C10 120.3(3) . . ? C8 C9 C10 130.4(3) . . ? N5 C12 C15 109.0(3) . . ? N5 C12 C11 120.4(3) . . ? C15 C12 C11 130.6(3) . . ? N6 C14 C15 109.2(3) . . ? N6 C14 C13 120.6(3) . . ? C15 C14 C13 130.2(3) . . ? C14 C15 C12 106.1(3) . . ? N6 Cu3 N1 173.79(10) . . ? N6 Cu3 Cu2 98.66(8) . 2_676 ? N1 Cu3 Cu2 87.55(7) . 2_676 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.414 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.090