# 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H32 Cu4 N4 O20, 3(C H2 Cl2)' _chemical_formula_sum 'C29 H38 Cl6 Cu4 N4 O20' _chemical_formula_weight 1229.49 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3277(5) _cell_length_b 13.9177(5) _cell_length_c 14.9095(5) _cell_angle_alpha 69.705(3) _cell_angle_beta 72.104(3) _cell_angle_gamma 87.298(3) _cell_volume 2278.11(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8466 _cell_measurement_theta_min 2.9550 _cell_measurement_theta_max 28.7490 _exptl_crystal_description prism _exptl_crystal_colour bluem _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 2.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6005 _exptl_absorpt_correction_T_max 0.7722 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20777 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8452 _reflns_number_gt 6800 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0534P)^2^+1.6471P] 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 8452 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.57947(4) 0.06198(4) 0.22135(3) 0.02192(13) Uani 1 1 d . . . Cu2 Cu 0.30344(4) 0.22944(4) 0.29444(3) 0.02216(13) Uani 1 1 d . . . Cu3 Cu 0.50343(4) 0.32502(4) 0.33712(3) 0.02317(13) Uani 1 1 d . . . Cu4 Cu 0.66375(4) 0.29887(4) 0.09041(3) 0.02265(13) Uani 1 1 d . . . Cl3 Cl 0.73702(16) 0.87527(18) -0.05318(14) 0.0922(6) Uani 1 1 d . . . Cl4 Cl 0.80493(16) 0.80758(16) 0.12710(13) 0.0920(6) Uani 1 1 d . . . Cl5 Cl 0.08881(17) 0.84852(14) 0.16642(17) 0.0975(6) Uani 1 1 d . . . Cl6 Cl -0.02288(11) 0.64342(11) 0.24644(9) 0.0549(4) Uani 1 1 d . . . O1 O 0.5595(2) -0.1179(2) 0.2621(2) 0.0286(6) Uani 1 1 d . . . O2 O 0.4150(2) -0.2390(2) 0.3245(2) 0.0298(7) Uani 1 1 d . . . O3 O 0.1091(2) 0.1636(2) 0.3273(2) 0.0305(7) Uani 1 1 d . . . O4 O 0.0252(2) 0.0065(2) 0.3743(2) 0.0399(8) Uani 1 1 d . . . O5 O 0.5903(2) 0.4158(2) 0.42139(19) 0.0305(7) Uani 1 1 d . . . O6 O 0.7285(2) 0.5426(2) 0.3642(2) 0.0313(7) Uani 1 1 d . . . O7 O 0.8053(3) 0.4513(2) -0.0569(2) 0.0371(7) Uani 1 1 d . . . O8 O 0.9080(3) 0.5779(2) -0.0522(2) 0.0357(7) Uani 1 1 d . . . O9 O 0.2685(2) 0.1723(2) 0.44084(19) 0.0308(7) Uani 1 1 d . . . O10 O 0.3930(2) 0.2631(2) 0.46711(19) 0.0277(6) Uani 1 1 d . . . O11 O 0.2649(2) 0.3644(2) 0.3010(2) 0.0315(7) Uani 1 1 d . . . O12 O 0.4173(2) 0.4466(2) 0.3006(2) 0.0287(6) Uani 1 1 d . . . O13 O 0.8049(2) 0.2362(2) 0.1064(2) 0.0338(7) Uani 1 1 d . . . O14 O 0.7443(2) 0.0704(2) 0.1638(2) 0.0344(7) Uani 1 1 d . . . O15 O 0.6556(2) 0.2372(2) -0.00452(19) 0.0277(6) Uani 1 1 d . . . O16 O 0.5609(2) 0.0848(2) 0.09037(19) 0.0297(7) Uani 1 1 d . . . O17 O 0.6040(2) 0.0387(2) 0.35175(19) 0.0279(6) Uani 1 1 d . . . O18 O 0.5544(2) 0.1972(2) 0.31824(19) 0.0269(6) Uani 1 1 d . . . O19 O 0.4998(2) 0.3140(2) 0.13531(19) 0.0291(7) Uani 1 1 d . . . O20 O 0.3208(2) 0.2887(2) 0.1497(2) 0.0289(6) Uani 1 1 d . . . N1 N 0.4104(3) 0.0297(2) 0.2799(2) 0.0206(7) Uani 1 1 d . . . N2 N 0.3207(3) 0.0868(2) 0.2924(2) 0.0217(7) Uani 1 1 d . . . N3 N 0.6453(3) 0.3993(2) 0.2380(2) 0.0222(7) Uani 1 1 d . . . N4 N 0.6914(3) 0.4018(2) 0.1441(2) 0.0223(7) Uani 1 1 d . . . C1 C 0.4576(4) -0.1426(3) 0.2938(3) 0.0241(9) Uani 1 1 d . . . C2 C 0.3706(3) -0.0679(3) 0.3016(3) 0.0226(8) Uani 1 1 d . . . C3 C 0.2533(3) -0.0745(3) 0.3283(3) 0.0232(8) Uani 1 1 d . . . H3 H 0.2035 -0.1330 0.3468 0.028 Uiso 1 1 calc R . . C4 C 0.2249(3) 0.0252(3) 0.3216(3) 0.0251(9) Uani 1 1 d . . . C5 C 0.1153(3) 0.0741(3) 0.3402(3) 0.0268(9) Uani 1 1 d . . . C6 C 0.5002(4) -0.3146(3) 0.3215(4) 0.0400(11) Uani 1 1 d . . . H6A H 0.5527 -0.2968 0.2529 0.060 Uiso 1 1 calc R . . H6B H 0.4621 -0.3827 0.3425 0.060 Uiso 1 1 calc R . . H6C H 0.5431 -0.3155 0.3673 0.060 Uiso 1 1 calc R . . C7 C -0.0852(4) 0.0497(4) 0.3994(4) 0.0473(13) Uani 1 1 d . . . H7A H -0.0852 0.0897 0.4421 0.071 Uiso 1 1 calc R . . H7B H -0.1455 -0.0059 0.4355 0.071 Uiso 1 1 calc R . . H7C H -0.0993 0.0945 0.3375 0.071 Uiso 1 1 calc R . . C8 C 0.6664(3) 0.4741(3) 0.3540(3) 0.0245(9) Uani 1 1 d . . . C9 C 0.7006(3) 0.4723(3) 0.2509(3) 0.0223(8) Uani 1 1 d . . . C10 C 0.7834(3) 0.5261(3) 0.1616(3) 0.0263(9) Uani 1 1 d . . . H10 H 0.8341 0.5822 0.1484 0.032 Uiso 1 1 calc R . . C11 C 0.7748(3) 0.4786(3) 0.0964(3) 0.0248(9) Uani 1 1 d . . . C12 C 0.8312(3) 0.5004(3) -0.0119(3) 0.0278(9) Uani 1 1 d . . . C13 C 0.7070(4) 0.5383(4) 0.4670(3) 0.0395(11) Uani 1 1 d . . . H13A H 0.6297 0.5589 0.4922 0.059 Uiso 1 1 calc R . . H13B H 0.7627 0.5850 0.4688 0.059 Uiso 1 1 calc R . . H13C H 0.7140 0.4680 0.5095 0.059 Uiso 1 1 calc R . . C14 C 0.9580(4) 0.6127(4) -0.1607(3) 0.0455(13) Uani 1 1 d . . . H14A H 0.9912 0.5550 -0.1807 0.068 Uiso 1 1 calc R . . H14B H 1.0179 0.6671 -0.1822 0.068 Uiso 1 1 calc R . . H14C H 0.8987 0.6393 -0.1923 0.068 Uiso 1 1 calc R . . C15 C 0.3048(3) 0.2041(3) 0.4966(3) 0.0239(9) Uani 1 1 d . . . C16 C 0.2397(4) 0.1688(3) 0.6072(3) 0.0320(10) Uani 1 1 d . . . H16A H 0.1578 0.1615 0.6167 0.048 Uiso 1 1 calc R . . H16B H 0.2534 0.2195 0.6352 0.048 Uiso 1 1 calc R . . H16C H 0.2654 0.1025 0.6416 0.048 Uiso 1 1 calc R . . C17 C 0.3191(4) 0.4432(3) 0.2924(3) 0.0266(9) Uani 1 1 d . . . C18 C 0.2591(4) 0.5415(3) 0.2730(4) 0.0376(11) Uani 1 1 d . . . H18A H 0.3097 0.5976 0.2661 0.056 Uiso 1 1 calc R . . H18B H 0.1894 0.5339 0.3295 0.056 Uiso 1 1 calc R . . H18C H 0.2392 0.5569 0.2110 0.056 Uiso 1 1 calc R . . C19 C 0.8209(3) 0.1413(3) 0.1304(3) 0.0295(10) Uani 1 1 d . . . C20 C 0.9418(4) 0.1110(4) 0.1161(4) 0.0474(13) Uani 1 1 d . . . H20A H 0.9446 0.0508 0.1739 0.071 Uiso 1 1 calc R . . H20B H 0.9901 0.1680 0.1106 0.071 Uiso 1 1 calc R . . H20C H 0.9696 0.0943 0.0546 0.071 Uiso 1 1 calc R . . C21 C 0.6037(3) 0.1552(3) 0.0084(3) 0.0257(9) Uani 1 1 d . . . C22 C 0.5915(4) 0.1416(4) -0.0848(3) 0.0391(11) Uani 1 1 d . . . H22A H 0.5981 0.0692 -0.0785 0.059 Uiso 1 1 calc R . . H22B H 0.6518 0.1839 -0.1443 0.059 Uiso 1 1 calc R . . H22C H 0.5166 0.1627 -0.0917 0.059 Uiso 1 1 calc R . . C23 C 0.5880(3) 0.1184(3) 0.3742(3) 0.0222(9) Uani 1 1 d . . . C24 C 0.6112(4) 0.1199(4) 0.4671(3) 0.0335(10) Uani 1 1 d . . . H24A H 0.6466 0.0569 0.4957 0.050 Uiso 1 1 calc R . . H24B H 0.5392 0.1243 0.5166 0.050 Uiso 1 1 calc R . . H24C H 0.6630 0.1796 0.4494 0.050 Uiso 1 1 calc R . . C25 C 0.4210(3) 0.3227(3) 0.0962(3) 0.0246(9) Uani 1 1 d . . . C26 C 0.4424(4) 0.3760(4) -0.0148(3) 0.0426(12) Uani 1 1 d . . . H26A H 0.4000 0.3380 -0.0391 0.064 Uiso 1 1 calc R . . H26B H 0.5243 0.3789 -0.0502 0.064 Uiso 1 1 calc R . . H26C H 0.4170 0.4459 -0.0275 0.064 Uiso 1 1 calc R . . C28 C 0.7573(5) 0.9066(5) 0.0435(4) 0.0563(14) Uani 1 1 d . . . H28A H 0.8134 0.9664 0.0142 0.068 Uiso 1 1 calc R . . H28B H 0.6841 0.9271 0.0807 0.068 Uiso 1 1 calc R . . C29 C 0.0818(5) 0.7307(5) 0.1502(4) 0.0643(16) Uani 1 1 d . . . H29A H 0.0667 0.7426 0.0858 0.077 Uiso 1 1 calc R . . H29B H 0.1568 0.7006 0.1457 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.14043(12) 0.69094(11) 0.57907(12) 0.0614(4) Uani 1 1 d . . . C27 C 0.0044(10) 0.6972(11) 0.5543(9) 0.061(3) Uiso 0.50 1 d P A 1 H27A H -0.0521 0.6467 0.6121 0.073 Uiso 0.50 1 calc PR A 1 H27B H -0.0237 0.7664 0.5473 0.073 Uiso 0.50 1 calc PR A 1 Cl2 Cl 0.0152(3) 0.6735(3) 0.4517(3) 0.0625(9) Uiso 0.50 1 d P A 1 C27A C 0.0106(8) 0.6485(9) 0.5831(8) 0.041(2) Uiso 0.50 1 d P A 2 H27C H -0.0460 0.6973 0.6001 0.049 Uiso 0.50 1 calc PR A 2 H27D H -0.0121 0.5816 0.6388 0.049 Uiso 0.50 1 calc PR A 2 Cl2A Cl 0.0011(4) 0.6331(4) 0.4749(3) 0.0796(12) Uiso 0.50 1 d P 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 Cu1 0.0218(3) 0.0234(3) 0.0198(2) -0.0081(2) -0.00472(19) 0.00140(19) Cu2 0.0223(3) 0.0213(3) 0.0237(2) -0.0105(2) -0.0051(2) 0.00030(19) Cu3 0.0208(3) 0.0217(3) 0.0250(2) -0.0096(2) -0.0025(2) 0.00012(19) Cu4 0.0218(3) 0.0252(3) 0.0241(2) -0.0123(2) -0.0073(2) 0.00169(19) Cl3 0.0727(12) 0.1445(19) 0.0864(12) -0.0716(13) -0.0267(10) 0.0110(11) Cl4 0.0787(12) 0.1055(15) 0.0682(10) -0.0160(10) -0.0116(9) 0.0393(11) Cl5 0.0813(13) 0.0621(11) 0.1344(17) -0.0343(11) -0.0110(12) -0.0108(9) Cl6 0.0468(8) 0.0643(9) 0.0475(7) -0.0158(6) -0.0085(6) -0.0089(6) O1 0.0277(17) 0.0249(15) 0.0314(15) -0.0108(12) -0.0054(13) 0.0016(12) O2 0.0321(16) 0.0200(15) 0.0348(15) -0.0072(12) -0.0090(13) -0.0008(12) O3 0.0259(16) 0.0281(17) 0.0367(16) -0.0131(13) -0.0066(13) 0.0020(12) O4 0.0205(16) 0.0332(17) 0.067(2) -0.0242(16) -0.0067(15) -0.0018(12) O5 0.0270(16) 0.0377(17) 0.0257(14) -0.0147(13) -0.0016(12) -0.0052(13) O6 0.0343(17) 0.0339(17) 0.0296(14) -0.0184(13) -0.0059(13) -0.0042(13) O7 0.0452(19) 0.0416(19) 0.0256(15) -0.0138(14) -0.0095(14) -0.0011(14) O8 0.0370(18) 0.0336(17) 0.0272(14) -0.0048(13) -0.0019(13) -0.0088(13) O9 0.0380(17) 0.0303(16) 0.0230(13) -0.0120(12) -0.0041(13) -0.0060(13) O10 0.0253(15) 0.0296(16) 0.0256(14) -0.0109(12) -0.0021(12) -0.0031(12) O11 0.0297(16) 0.0277(16) 0.0441(17) -0.0193(14) -0.0138(13) 0.0053(12) O12 0.0230(16) 0.0237(15) 0.0395(16) -0.0121(13) -0.0088(13) 0.0023(11) O13 0.0271(16) 0.0363(18) 0.0434(17) -0.0174(15) -0.0149(14) 0.0062(13) O14 0.0229(16) 0.0332(17) 0.0377(16) -0.0065(14) -0.0033(13) 0.0032(13) O15 0.0324(16) 0.0292(16) 0.0267(14) -0.0165(12) -0.0085(12) 0.0009(12) O16 0.0327(17) 0.0328(17) 0.0212(13) -0.0096(13) -0.0037(12) -0.0053(13) O17 0.0318(16) 0.0284(16) 0.0272(14) -0.0124(12) -0.0119(12) 0.0066(12) O18 0.0359(17) 0.0224(15) 0.0212(13) -0.0071(12) -0.0083(12) 0.0057(12) O19 0.0224(15) 0.0422(18) 0.0281(14) -0.0171(13) -0.0101(12) 0.0044(12) O20 0.0251(16) 0.0331(16) 0.0289(14) -0.0107(13) -0.0087(12) 0.0004(12) N1 0.0223(17) 0.0209(17) 0.0191(15) -0.0081(13) -0.0060(13) 0.0028(13) N2 0.0213(18) 0.0207(17) 0.0232(16) -0.0087(14) -0.0054(14) 0.0000(13) N3 0.0218(18) 0.0242(17) 0.0218(16) -0.0102(14) -0.0059(14) 0.0005(13) N4 0.0218(18) 0.0253(18) 0.0209(16) -0.0099(14) -0.0062(14) 0.0015(13) C1 0.035(3) 0.024(2) 0.0163(18) -0.0072(16) -0.0113(17) 0.0020(17) C2 0.030(2) 0.022(2) 0.0155(17) -0.0068(16) -0.0069(16) 0.0003(16) C3 0.025(2) 0.023(2) 0.0227(19) -0.0099(16) -0.0051(16) -0.0057(16) C4 0.026(2) 0.026(2) 0.0233(19) -0.0105(17) -0.0051(17) 0.0006(16) C5 0.022(2) 0.030(2) 0.029(2) -0.0117(18) -0.0061(17) -0.0010(17) C6 0.044(3) 0.022(2) 0.051(3) -0.010(2) -0.013(2) 0.0054(19) C7 0.023(2) 0.047(3) 0.070(3) -0.027(3) -0.003(2) 0.000(2) C8 0.026(2) 0.023(2) 0.030(2) -0.0136(18) -0.0095(18) 0.0046(17) C9 0.022(2) 0.022(2) 0.0246(19) -0.0121(16) -0.0061(16) 0.0037(16) C10 0.024(2) 0.026(2) 0.027(2) -0.0085(17) -0.0074(17) -0.0017(17) C11 0.023(2) 0.023(2) 0.028(2) -0.0083(17) -0.0092(17) 0.0005(16) C12 0.027(2) 0.029(2) 0.024(2) -0.0080(18) -0.0066(18) 0.0065(18) C13 0.046(3) 0.045(3) 0.037(2) -0.026(2) -0.012(2) -0.001(2) C14 0.046(3) 0.048(3) 0.027(2) -0.005(2) 0.003(2) -0.001(2) C15 0.024(2) 0.022(2) 0.0239(19) -0.0096(17) -0.0040(17) 0.0060(16) C16 0.035(2) 0.036(2) 0.0208(19) -0.0088(18) -0.0033(18) -0.0016(19) C17 0.032(2) 0.026(2) 0.0196(19) -0.0088(17) -0.0055(17) 0.0046(18) C18 0.040(3) 0.030(2) 0.049(3) -0.017(2) -0.020(2) 0.012(2) C19 0.023(2) 0.042(3) 0.022(2) -0.0109(19) -0.0055(17) 0.0077(19) C20 0.029(3) 0.051(3) 0.053(3) -0.012(3) -0.008(2) 0.008(2) C21 0.024(2) 0.033(2) 0.023(2) -0.0139(18) -0.0068(17) 0.0064(17) C22 0.055(3) 0.044(3) 0.023(2) -0.015(2) -0.014(2) -0.007(2) C23 0.015(2) 0.031(2) 0.0192(18) -0.0090(17) -0.0021(15) -0.0027(16) C24 0.038(3) 0.040(3) 0.027(2) -0.0132(19) -0.0140(19) 0.002(2) C25 0.028(2) 0.020(2) 0.027(2) -0.0090(17) -0.0089(18) 0.0040(16) C26 0.045(3) 0.045(3) 0.030(2) -0.003(2) -0.013(2) 0.007(2) C28 0.055(4) 0.060(4) 0.050(3) -0.021(3) -0.008(3) 0.008(3) C29 0.060(4) 0.054(4) 0.062(3) -0.011(3) -0.006(3) 0.002(3) Cl1 0.0501(8) 0.0575(9) 0.0814(10) -0.0254(8) -0.0267(7) 0.0089(6) _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 O14 1.940(3) . ? Cu1 O16 1.950(3) . ? Cu1 O17 1.973(3) . ? Cu1 N1 2.001(3) . ? Cu1 O1 2.368(3) . ? Cu2 O11 1.943(3) . ? Cu2 O9 1.958(3) . ? Cu2 O20 1.969(3) . ? Cu2 N2 1.997(3) . ? Cu3 O10 1.919(3) . ? Cu3 O18 1.943(3) . ? Cu3 O12 1.958(3) . ? Cu3 N3 1.958(3) . ? Cu4 O15 1.921(3) . ? Cu4 O19 1.950(3) . ? Cu4 O13 1.953(3) . ? Cu4 N4 1.955(3) . ? Cl3 C28 1.731(6) . ? Cl4 C28 1.726(6) . ? Cl5 C29 1.749(7) . ? Cl6 C29 1.732(6) . ? O1 C1 1.218(5) . ? O2 C1 1.333(5) . ? O2 C6 1.454(5) . ? O3 C5 1.195(5) . ? O4 C5 1.341(5) . ? O4 C7 1.457(5) . ? O5 C8 1.214(5) . ? O6 C8 1.326(5) . ? O6 C13 1.453(5) . ? O7 C12 1.220(5) . ? O8 C12 1.311(5) . ? O8 C14 1.450(5) . ? O9 C15 1.261(5) . ? O10 C15 1.261(5) . ? O11 C17 1.260(5) . ? O12 C17 1.258(5) . ? O13 C19 1.267(5) . ? O14 C19 1.252(5) . ? O15 C21 1.261(5) . ? O16 C21 1.246(5) . ? O17 C23 1.256(5) . ? O18 C23 1.266(5) . ? O19 C25 1.260(5) . ? O20 C25 1.254(5) . ? N1 N2 1.335(4) . ? N1 C2 1.360(5) . ? N2 C4 1.355(5) . ? N3 N4 1.327(4) . ? N3 C9 1.348(5) . ? N4 C11 1.353(5) . ? C1 C2 1.465(6) . ? C2 C3 1.376(5) . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C5 1.477(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.473(5) . ? C9 C10 1.386(5) . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 C12 1.474(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.505(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.505(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.501(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.517(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.506(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.502(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? Cl1 C27A 1.709(10) . ? Cl1 C27 1.817(12) . ? C27 Cl2 1.639(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27A Cl2A 1.738(11) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? 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 O14 Cu1 O16 90.87(12) . . ? O14 Cu1 O17 87.17(12) . . ? O16 Cu1 O17 178.03(12) . . ? O14 Cu1 N1 170.49(13) . . ? O16 Cu1 N1 87.18(12) . . ? O17 Cu1 N1 94.72(12) . . ? O14 Cu1 O1 94.27(11) . . ? O16 Cu1 O1 90.43(11) . . ? O17 Cu1 O1 89.53(11) . . ? N1 Cu1 O1 76.45(11) . . ? O11 Cu2 O9 90.51(12) . . ? O11 Cu2 O20 87.29(12) . . ? O9 Cu2 O20 173.83(12) . . ? O11 Cu2 N2 172.33(12) . . ? O9 Cu2 N2 88.43(12) . . ? O20 Cu2 N2 92.98(12) . . ? O10 Cu3 O18 96.15(11) . . ? O10 Cu3 O12 93.63(12) . . ? O18 Cu3 O12 148.07(12) . . ? O10 Cu3 N3 157.74(13) . . ? O18 Cu3 N3 90.97(13) . . ? O12 Cu3 N3 91.32(12) . . ? O15 Cu4 O19 94.43(12) . . ? O15 Cu4 O13 93.63(12) . . ? O19 Cu4 O13 153.76(12) . . ? O15 Cu4 N4 160.27(12) . . ? O19 Cu4 N4 90.31(13) . . ? O13 Cu4 N4 90.46(13) . . ? C1 O1 Cu1 107.3(2) . . ? C1 O2 C6 114.7(3) . . ? C5 O4 C7 114.4(3) . . ? C8 O6 C13 114.8(3) . . ? C12 O8 C14 116.2(4) . . ? C15 O9 Cu2 128.6(3) . . ? C15 O10 Cu3 132.1(3) . . ? C17 O11 Cu2 135.8(3) . . ? C17 O12 Cu3 123.4(3) . . ? C19 O13 Cu4 125.9(3) . . ? C19 O14 Cu1 134.0(3) . . ? C21 O15 Cu4 130.7(2) . . ? C21 O16 Cu1 129.5(3) . . ? C23 O17 Cu1 110.6(2) . . ? C23 O18 Cu3 131.4(3) . . ? C25 O19 Cu4 134.6(3) . . ? C25 O20 Cu2 113.3(2) . . ? N2 N1 C2 108.0(3) . . ? N2 N1 Cu1 133.9(2) . . ? C2 N1 Cu1 117.5(3) . . ? N1 N2 C4 107.9(3) . . ? N1 N2 Cu2 133.1(2) . . ? C4 N2 Cu2 118.4(3) . . ? N4 N3 C9 108.5(3) . . ? N4 N3 Cu3 128.0(3) . . ? C9 N3 Cu3 122.5(2) . . ? N3 N4 C11 108.0(3) . . ? N3 N4 Cu4 126.1(2) . . ? C11 N4 Cu4 125.0(3) . . ? O1 C1 O2 123.6(4) . . ? O1 C1 C2 122.4(4) . . ? O2 C1 C2 114.0(3) . . ? N1 C2 C3 110.5(3) . . ? N1 C2 C1 115.7(3) . . ? C3 C2 C1 133.7(4) . . ? C2 C3 C4 103.3(3) . . ? C2 C3 H3 128.3 . . ? C4 C3 H3 128.3 . . ? N2 C4 C3 110.3(3) . . ? N2 C4 C5 116.4(4) . . ? C3 C4 C5 133.3(4) . . ? O3 C5 O4 124.7(4) . . ? O3 C5 C4 123.1(4) . . ? O4 C5 C4 112.2(4) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 H7A 109.5 . . ? O4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 O6 125.3(4) . . ? O5 C8 C9 121.6(4) . . ? O6 C8 C9 113.1(3) . . ? N3 C9 C10 109.9(3) . . ? N3 C9 C8 115.6(3) . . ? C10 C9 C8 134.5(4) . . ? C11 C10 C9 103.5(3) . . ? C11 C10 H10 128.2 . . ? C9 C10 H10 128.2 . . ? N4 C11 C10 110.0(3) . . ? N4 C11 C12 117.0(4) . . ? C10 C11 C12 132.8(4) . . ? O7 C12 O8 125.5(4) . . ? O7 C12 C11 122.0(4) . . ? O8 C12 C11 112.5(4) . . ? O6 C13 H13A 109.5 . . ? O6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O8 C14 H14A 109.5 . . ? O8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O9 C15 O10 125.0(4) . . ? O9 C15 C16 118.3(4) . . ? O10 C15 C16 116.7(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 . . ? O12 C17 O11 126.1(4) . . ? O12 C17 C18 117.4(4) . . ? O11 C17 C18 116.5(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O14 C19 O13 125.5(4) . . ? O14 C19 C20 117.1(4) . . ? O13 C19 C20 117.3(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O16 C21 O15 126.2(4) . . ? O16 C21 C22 117.1(4) . . ? O15 C21 C22 116.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O17 C23 O18 120.2(3) . . ? O17 C23 C24 119.3(4) . . ? O18 C23 C24 120.4(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O20 C25 O19 120.6(3) . . ? O20 C25 C26 117.8(4) . . ? O19 C25 C26 121.6(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Cl4 C28 Cl3 113.6(3) . . ? Cl4 C28 H28A 108.9 . . ? Cl3 C28 H28A 108.9 . . ? Cl4 C28 H28B 108.9 . . ? Cl3 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? Cl6 C29 Cl5 113.4(3) . . ? Cl6 C29 H29A 108.9 . . ? Cl5 C29 H29A 108.9 . . ? Cl6 C29 H29B 108.9 . . ? Cl5 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C27A Cl1 C27 22.0(5) . . ? Cl2 C27 Cl1 111.9(7) . . ? Cl2 C27 H27A 109.2 . . ? Cl1 C27 H27A 109.2 . . ? Cl2 C27 H27B 109.2 . . ? Cl1 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? Cl1 C27A Cl2A 117.1(6) . . ? Cl1 C27A H27C 108.0 . . ? Cl2A C27A H27C 108.0 . . ? Cl1 C27A H27D 108.0 . . ? Cl2A C27A H27D 108.0 . . ? H27C C27A H27D 107.3 . . ? 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 O14 Cu1 O1 C1 -174.6(2) . . . . ? O16 Cu1 O1 C1 -83.7(2) . . . . ? O17 Cu1 O1 C1 98.3(2) . . . . ? N1 Cu1 O1 C1 3.3(2) . . . . ? O11 Cu2 O9 C15 -51.5(3) . . . . ? O20 Cu2 O9 C15 -120.6(11) . . . . ? N2 Cu2 O9 C15 136.1(3) . . . . ? O18 Cu3 O10 C15 -60.7(4) . . . . ? O12 Cu3 O10 C15 88.9(4) . . . . ? N3 Cu3 O10 C15 -168.7(4) . . . . ? O9 Cu2 O11 C17 94.7(4) . . . . ? O20 Cu2 O11 C17 -91.1(4) . . . . ? N2 Cu2 O11 C17 176.7(8) . . . . ? O10 Cu3 O12 C17 -62.6(3) . . . . ? O18 Cu3 O12 C17 45.1(4) . . . . ? N3 Cu3 O12 C17 139.1(3) . . . . ? O15 Cu4 O13 C19 -54.5(3) . . . . ? O19 Cu4 O13 C19 53.2(5) . . . . ? N4 Cu4 O13 C19 144.9(3) . . . . ? O16 Cu1 O14 C19 95.1(4) . . . . ? O17 Cu1 O14 C19 -85.1(4) . . . . ? N1 Cu1 O14 C19 173.1(6) . . . . ? O1 Cu1 O14 C19 -174.4(4) . . . . ? O19 Cu4 O15 C21 -60.8(3) . . . . ? O13 Cu4 O15 C21 94.2(3) . . . . ? N4 Cu4 O15 C21 -164.2(4) . . . . ? O14 Cu1 O16 C21 -53.4(4) . . . . ? O17 Cu1 O16 C21 -59(4) . . . . ? N1 Cu1 O16 C21 135.9(4) . . . . ? O1 Cu1 O16 C21 -147.7(3) . . . . ? O14 Cu1 O17 C23 104.0(3) . . . . ? O16 Cu1 O17 C23 109(3) . . . . ? N1 Cu1 O17 C23 -85.4(3) . . . . ? O1 Cu1 O17 C23 -161.7(3) . . . . ? O10 Cu3 O18 C23 -51.2(3) . . . . ? O12 Cu3 O18 C23 -158.3(3) . . . . ? N3 Cu3 O18 C23 107.6(3) . . . . ? O15 Cu4 O19 C25 -26.0(4) . . . . ? O13 Cu4 O19 C25 -133.5(4) . . . . ? N4 Cu4 O19 C25 134.8(4) . . . . ? O11 Cu2 O20 C25 91.9(3) . . . . ? O9 Cu2 O20 C25 161.1(10) . . . . ? N2 Cu2 O20 C25 -95.8(3) . . . . ? O14 Cu1 N1 N2 -163.4(6) . . . . ? O16 Cu1 N1 N2 -85.0(3) . . . . ? O17 Cu1 N1 N2 95.5(3) . . . . ? O1 Cu1 N1 N2 -176.2(3) . . . . ? O14 Cu1 N1 C2 6.2(9) . . . . ? O16 Cu1 N1 C2 84.5(3) . . . . ? O17 Cu1 N1 C2 -95.0(3) . . . . ? O1 Cu1 N1 C2 -6.6(2) . . . . ? C2 N1 N2 C4 -0.1(4) . . . . ? Cu1 N1 N2 C4 170.1(3) . . . . ? C2 N1 N2 Cu2 170.3(3) . . . . ? Cu1 N1 N2 Cu2 -19.4(5) . . . . ? O11 Cu2 N2 N1 -175.4(8) . . . . ? O9 Cu2 N2 N1 -93.2(3) . . . . ? O20 Cu2 N2 N1 92.8(3) . . . . ? O11 Cu2 N2 C4 -5.7(11) . . . . ? O9 Cu2 N2 C4 76.4(3) . . . . ? O20 Cu2 N2 C4 -97.6(3) . . . . ? O10 Cu3 N3 N4 162.4(3) . . . . ? O18 Cu3 N3 N4 53.5(3) . . . . ? O12 Cu3 N3 N4 -94.7(3) . . . . ? O10 Cu3 N3 C9 -30.5(5) . . . . ? O18 Cu3 N3 C9 -139.4(3) . . . . ? O12 Cu3 N3 C9 72.5(3) . . . . ? C9 N3 N4 C11 -1.4(4) . . . . ? Cu3 N3 N4 C11 167.2(3) . . . . ? C9 N3 N4 Cu4 168.6(3) . . . . ? Cu3 N3 N4 Cu4 -22.8(5) . . . . ? O15 Cu4 N4 N3 159.3(3) . . . . ? O19 Cu4 N4 N3 55.2(3) . . . . ? O13 Cu4 N4 N3 -98.5(3) . . . . ? O15 Cu4 N4 C11 -32.3(6) . . . . ? O19 Cu4 N4 C11 -136.4(3) . . . . ? O13 Cu4 N4 C11 69.9(3) . . . . ? Cu1 O1 C1 O2 -179.7(3) . . . . ? Cu1 O1 C1 C2 0.3(4) . . . . ? C6 O2 C1 O1 2.6(5) . . . . ? C6 O2 C1 C2 -177.4(3) . . . . ? N2 N1 C2 C3 0.2(4) . . . . ? Cu1 N1 C2 C3 -171.9(2) . . . . ? N2 N1 C2 C1 -178.9(3) . . . . ? Cu1 N1 C2 C1 9.0(4) . . . . ? O1 C1 C2 N1 -5.9(5) . . . . ? O2 C1 C2 N1 174.1(3) . . . . ? O1 C1 C2 C3 175.3(4) . . . . ? O2 C1 C2 C3 -4.7(6) . . . . ? N1 C2 C3 C4 -0.2(4) . . . . ? C1 C2 C3 C4 178.6(4) . . . . ? N1 N2 C4 C3 0.0(4) . . . . ? Cu2 N2 C4 C3 -172.1(2) . . . . ? N1 N2 C4 C5 179.6(3) . . . . ? Cu2 N2 C4 C5 7.5(4) . . . . ? C2 C3 C4 N2 0.1(4) . . . . ? C2 C3 C4 C5 -179.4(4) . . . . ? C7 O4 C5 O3 -2.4(6) . . . . ? C7 O4 C5 C4 176.6(4) . . . . ? N2 C4 C5 O3 2.7(6) . . . . ? C3 C4 C5 O3 -177.9(4) . . . . ? N2 C4 C5 O4 -176.4(3) . . . . ? C3 C4 C5 O4 3.1(6) . . . . ? C13 O6 C8 O5 5.4(6) . . . . ? C13 O6 C8 C9 -172.8(3) . . . . ? N4 N3 C9 C10 1.7(4) . . . . ? Cu3 N3 C9 C10 -167.6(3) . . . . ? N4 N3 C9 C8 -175.0(3) . . . . ? Cu3 N3 C9 C8 15.7(5) . . . . ? O5 C8 C9 N3 -2.6(6) . . . . ? O6 C8 C9 N3 175.7(3) . . . . ? O5 C8 C9 C10 -178.3(4) . . . . ? O6 C8 C9 C10 0.0(6) . . . . ? N3 C9 C10 C11 -1.3(4) . . . . ? C8 C9 C10 C11 174.6(4) . . . . ? N3 N4 C11 C10 0.6(4) . . . . ? Cu4 N4 C11 C10 -169.5(3) . . . . ? N3 N4 C11 C12 -175.1(3) . . . . ? Cu4 N4 C11 C12 14.7(5) . . . . ? C9 C10 C11 N4 0.4(4) . . . . ? C9 C10 C11 C12 175.2(4) . . . . ? C14 O8 C12 O7 5.7(6) . . . . ? C14 O8 C12 C11 -172.9(4) . . . . ? N4 C11 C12 O7 -0.7(6) . . . . ? C10 C11 C12 O7 -175.2(4) . . . . ? N4 C11 C12 O8 177.9(3) . . . . ? C10 C11 C12 O8 3.4(6) . . . . ? Cu2 O9 C15 O10 -19.5(6) . . . . ? Cu2 O9 C15 C16 161.2(3) . . . . ? Cu3 O10 C15 O9 -0.7(6) . . . . ? Cu3 O10 C15 C16 178.6(3) . . . . ? Cu3 O12 C17 O11 -3.9(6) . . . . ? Cu3 O12 C17 C18 174.6(3) . . . . ? Cu2 O11 C17 O12 -19.0(6) . . . . ? Cu2 O11 C17 C18 162.5(3) . . . . ? Cu1 O14 C19 O13 -16.2(7) . . . . ? Cu1 O14 C19 C20 164.9(3) . . . . ? Cu4 O13 C19 O14 -12.5(6) . . . . ? Cu4 O13 C19 C20 166.5(3) . . . . ? Cu1 O16 C21 O15 -11.9(6) . . . . ? Cu1 O16 C21 C22 168.6(3) . . . . ? Cu4 O15 C21 O16 -13.9(6) . . . . ? Cu4 O15 C21 C22 165.5(3) . . . . ? Cu1 O17 C23 O18 3.6(4) . . . . ? Cu1 O17 C23 C24 -175.2(3) . . . . ? Cu3 O18 C23 O17 171.3(3) . . . . ? Cu3 O18 C23 C24 -9.9(5) . . . . ? Cu2 O20 C25 O19 2.5(5) . . . . ? Cu2 O20 C25 C26 -176.0(3) . . . . ? Cu4 O19 C25 O20 149.2(3) . . . . ? Cu4 O19 C25 C26 -32.4(6) . . . . ? C27A Cl1 C27 Cl2 -89.6(17) . . . . ? C27 Cl1 C27A Cl2A 74.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.024 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 951174' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Cu6 N12 O30' _chemical_formula_sum 'C48 H60 Cu6 N12 O30' _chemical_formula_weight 1666.32 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.722(3) _cell_length_b 16.304(3) _cell_length_c 16.721(3) _cell_angle_alpha 95.39(3) _cell_angle_beta 115.01(3) _cell_angle_gamma 114.83(3) _cell_volume 3327.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9659 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 31.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5205 _exptl_absorpt_correction_T_max 0.5447 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 184702 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 31.58 _reflns_number_total 22193 _reflns_number_gt 18161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0445P)^2^+1.3303P] 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 22193 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _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 0.823876(14) 0.663827(13) 0.769114(12) 0.02104(4) Uani 1 1 d . . .. Cu2 Cu 0.854080(15) 0.844158(13) 0.705391(13) 0.02297(4) Uani 1 1 d . . .. Cu3 Cu 0.709448(15) 0.923779(13) 0.688693(13) 0.02249(4) Uani 1 1 d . . .. Cu4 Cu 0.523481(15) 0.827086(13) 0.737141(13) 0.02234(4) Uani 1 1 d . . .. Cu5 Cu 0.497061(15) 0.656614(13) 0.802184(13) 0.02163(4) Uani 1 1 d . . .. Cu6 Cu 0.650975(14) 0.572210(13) 0.818926(12) 0.02056(4) Uani 1 1 d . . .. O1 O 0.83210(13) 0.49687(10) 0.68048(11) 0.0432(3) Uani 1 1 d . . . O2 O 0.88717(16) 0.48208(12) 0.57932(13) 0.0586(4) Uani 1 1 d . . . O3 O 0.88100(15) 0.88054(12) 0.56453(13) 0.0534(4) Uani 1 1 d . . . O4 O 0.93940(16) 0.83055(12) 0.48071(13) 0.0587(5) Uani 1 1 d . . . O5 O 0.98314(11) 0.64378(10) 0.90334(11) 0.0434(3) Uani 1 1 d . . . O6 O 1.15899(11) 0.70155(10) 0.94876(10) 0.0422(3) Uani 1 1 d . . . O7 O 1.23597(11) 1.03441(10) 0.83204(11) 0.0447(3) Uani 1 1 d . . . O8 O 1.07313(15) 1.02354(14) 0.76362(15) 0.0685(5) Uani 1 1 d . . . O9 O 0.84555(9) 0.93694(9) 0.77460(8) 0.0316(3) Uani 1 1 d . . . O10 O 0.71421(9) 0.82492(8) 0.62269(8) 0.0287(2) Uani 1 1 d . . . O11 O 0.53603(11) 0.92774(10) 0.38399(9) 0.0370(3) Uani 1 1 d . . . O12 O 0.68776(11) 0.98262(10) 0.52403(10) 0.0404(3) Uani 1 1 d . . . O13 O 0.20150(10) 0.76827(11) 0.47357(10) 0.0437(3) Uani 1 1 d . . . O14 O 0.29373(11) 0.77711(10) 0.62261(10) 0.0411(3) Uani 1 1 d . . . O15 O 0.85731(13) 1.12477(10) 0.74580(12) 0.0494(4) Uani 1 1 d . . . O16 O 0.88440(16) 1.25716(11) 0.83079(15) 0.0668(5) Uani 1 1 d . . . O17 O 0.46003(11) 0.92445(9) 0.82680(10) 0.0367(3) Uani 1 1 d . . . O18 O 0.53999(16) 1.07282(12) 0.92168(13) 0.0626(5) Uani 1 1 d . . . O19 O 0.56462(10) 0.79260(8) 0.84847(8) 0.0303(2) Uani 1 1 d . . . O20 O 0.45917(10) 0.69145(8) 0.69153(8) 0.0286(2) Uani 1 1 d . . . O21 O 0.26869(11) 0.55790(10) 0.70761(11) 0.0430(3) Uani 1 1 d . . . O22 O 0.14285(10) 0.40311(10) 0.65744(11) 0.0441(3) Uani 1 1 d . . . O23 O 0.57930(11) 0.36806(9) 0.77307(10) 0.0363(3) Uani 1 1 d . . . O24 O 0.41463(13) 0.23392(9) 0.69933(11) 0.0451(3) Uani 1 1 d . . . O25 O 0.42399(11) 0.67142(10) 0.93807(9) 0.0365(3) Uani 1 1 d . . . O26 O 0.48883(13) 0.67154(12) 1.08543(10) 0.0478(4) Uani 1 1 d . . . O27 O 0.80593(11) 0.56794(10) 1.12548(9) 0.0368(3) Uani 1 1 d . . . O28 O 0.77715(12) 0.52980(10) 0.98004(10) 0.0386(3) Uani 1 1 d . . . O29 O 0.79507(9) 0.67838(8) 0.86758(8) 0.0280(2) Uani 1 1 d . . . O30 O 0.67889(9) 0.55978(8) 0.71876(8) 0.0275(2) Uani 1 1 d . . . N1 N 0.83332(11) 0.65847(10) 0.65382(10) 0.0263(3) Uani 1 1 d . . . N2 N 0.84441(11) 0.73666(10) 0.62873(10) 0.0272(3) Uani 1 1 d . . . N3 N 0.97304(10) 0.77858(10) 0.83254(10) 0.0253(3) Uani 1 1 d . . . N4 N 0.98816(11) 0.85588(10) 0.80506(10) 0.0274(3) Uani 1 1 d . . . N5 N 0.56022(10) 0.88677(9) 0.59442(9) 0.0247(2) Uani 1 1 d . . . N6 N 0.48181(10) 0.84604(9) 0.61468(9) 0.0241(2) Uani 1 1 d . . . N7 N 0.70288(11) 1.00910(9) 0.77555(10) 0.0268(3) Uani 1 1 d . . . N8 N 0.62386(11) 0.96759(9) 0.79562(9) 0.0262(3) Uani 1 1 d . . . N9 N 0.42778(10) 0.51859(9) 0.74032(9) 0.0247(2) Uani 1 1 d . . . N10 N 0.49103(11) 0.48028(9) 0.75001(9) 0.0244(2) Uani 1 1 d . . . N11 N 0.56881(11) 0.63471(9) 0.92118(9) 0.0234(2) Uani 1 1 d . . . N12 N 0.63871(11) 0.60518(9) 0.92814(9) 0.0238(2) Uani 1 1 d . . . C1 C 0.86238(15) 0.52411(13) 0.61982(13) 0.0335(3) Uani 1 1 d . . . C2 C 0.86234(13) 0.61224(12) 0.60817(12) 0.0287(3) Uani 1 1 d . . . C3 C 0.89245(15) 0.66148(13) 0.55282(13) 0.0343(4) Uani 1 1 d . . . H3 H 0.9162 0.6453 0.5134 0.041 Uiso 1 1 calc R . . C4 C 0.88005(14) 0.73946(12) 0.56795(12) 0.0300(3) Uani 1 1 d . . . C5 C 0.90411(16) 0.82039(14) 0.53168(13) 0.0357(4) Uani 1 1 d . . . C6 C 0.8203(2) 0.40663(17) 0.69089(19) 0.0572(6) Uani 1 1 d . . . H6A H 0.7593 0.3546 0.6326 0.086 Uiso 1 1 calc R . . H6B H 0.8058 0.3971 0.7418 0.086 Uiso 1 1 calc R . . H6C H 0.8876 0.4068 0.7054 0.086 Uiso 1 1 calc R . . C7 C 0.8964(2) 0.96303(19) 0.5342(2) 0.0637(7) Uani 1 1 d . . . H7A H 0.9744 1.0110 0.5672 0.096 Uiso 1 1 calc R . . H7B H 0.8575 0.9904 0.5482 0.096 Uiso 1 1 calc R . . H7C H 0.8679 0.9437 0.4668 0.096 Uiso 1 1 calc R . . C8 C 1.07861(14) 0.70764(12) 0.91504(12) 0.0290(3) Uani 1 1 d . . . C9 C 1.07054(12) 0.78481(12) 0.88009(11) 0.0266(3) Uani 1 1 d . . . C10 C 1.15076(13) 0.86769(13) 0.88378(12) 0.0312(3) Uani 1 1 d . . . H10 H 1.2267 0.8903 0.9129 0.037 Uiso 1 1 calc R . . C11 C 1.09533(13) 0.91031(12) 0.83526(12) 0.0291(3) Uani 1 1 d . . . C12 C 1.13114(15) 0.99533(13) 0.80666(14) 0.0374(4) Uani 1 1 d . . . C13 C 0.9818(2) 0.56925(17) 0.94341(19) 0.0513(6) Uani 1 1 d . . . H13A H 0.9973 0.5286 0.9116 0.077 Uiso 1 1 calc R . . H13B H 0.9098 0.5304 0.9359 0.077 Uiso 1 1 calc R . . H13C H 1.0375 0.5980 1.0101 0.077 Uiso 1 1 calc R . . C14 C 1.2783(2) 1.11519(17) 0.8025(2) 0.0651(7) Uani 1 1 d . . . H14A H 1.2388 1.0949 0.7340 0.098 Uiso 1 1 calc R . . H14B H 1.3560 1.1398 0.8261 0.098 Uiso 1 1 calc R . . H14C H 1.2689 1.1656 0.8272 0.098 Uiso 1 1 calc R . . C15 C 0.59014(14) 0.93997(12) 0.47457(12) 0.0284(3) Uani 1 1 d . . . C16 C 0.51572(13) 0.89386(11) 0.50866(11) 0.0251(3) Uani 1 1 d . . . C17 C 0.40474(13) 0.85655(11) 0.47177(11) 0.0271(3) Uani 1 1 d . . . H17 H 0.3529 0.8518 0.4125 0.033 Uiso 1 1 calc R . . C18 C 0.38691(12) 0.82778(11) 0.54148(11) 0.0251(3) Uani 1 1 d . . . C19 C 0.29037(13) 0.78819(12) 0.55151(12) 0.0299(3) Uani 1 1 d . . . C20 C 0.6026(2) 0.96630(16) 0.34285(16) 0.0477(5) Uani 1 1 d . . . H20A H 0.6044 1.0251 0.3328 0.072 Uiso 1 1 calc R . . H20B H 0.5715 0.9192 0.2829 0.072 Uiso 1 1 calc R . . H20C H 0.6769 0.9806 0.3851 0.072 Uiso 1 1 calc R . . C21 C 0.10280(18) 0.7298(2) 0.4783(2) 0.0678(8) Uani 1 1 d . . . H21A H 0.0906 0.6720 0.4960 0.102 Uiso 1 1 calc R . . H21B H 0.0407 0.7136 0.4170 0.102 Uiso 1 1 calc R . . H21C H 0.1104 0.7776 0.5250 0.102 Uiso 1 1 calc R . . C22 C 0.83799(16) 1.17139(13) 0.79836(14) 0.0377(4) Uani 1 1 d . . . C23 C 0.75102(14) 1.10491(11) 0.81209(12) 0.0294(3) Uani 1 1 d . . . C24 C 0.70316(15) 1.12577(12) 0.85762(12) 0.0329(3) Uani 1 1 d . . . H24 H 0.7214 1.1870 0.8902 0.039 Uiso 1 1 calc R . . C25 C 0.62303(14) 1.03744(12) 0.84504(11) 0.0291(3) Uani 1 1 d . . . C26 C 0.53927(16) 1.01532(13) 0.87080(13) 0.0354(4) Uani 1 1 d . . . C27 C 0.9442(3) 1.1800(2) 0.7297(2) 0.0740(8) Uani 1 1 d . . . H27A H 0.9291 1.2246 0.6992 0.111 Uiso 1 1 calc R . . H27B H 0.9495 1.1369 0.6895 0.111 Uiso 1 1 calc R . . H27C H 1.0132 1.2160 0.7896 0.111 Uiso 1 1 calc R . . C28 C 0.3688(2) 0.89572(18) 0.84119(18) 0.0530(5) Uani 1 1 d . . . H28A H 0.3924 0.8972 0.9060 0.080 Uiso 1 1 calc R . . H28B H 0.3108 0.8306 0.7987 0.080 Uiso 1 1 calc R . . H28C H 0.3413 0.9398 0.8286 0.080 Uiso 1 1 calc R . . C29 C 0.23519(13) 0.46486(12) 0.68783(12) 0.0300(3) Uani 1 1 d . . . C30 C 0.32471(12) 0.44686(11) 0.70600(11) 0.0264(3) Uani 1 1 d . . . C31 C 0.32055(13) 0.35987(11) 0.69212(12) 0.0293(3) Uani 1 1 d . . . H31 H 0.2587 0.2976 0.6681 0.035 Uiso 1 1 calc R . . C32 C 0.42686(13) 0.38437(11) 0.72116(11) 0.0259(3) Uani 1 1 d . . . C33 C 0.47083(15) 0.31958(12) 0.72881(12) 0.0305(3) Uani 1 1 d . . . C34 C 0.1841(2) 0.58199(18) 0.67621(19) 0.0525(6) Uani 1 1 d . . . H34A H 0.1311 0.5459 0.6096 0.079 Uiso 1 1 calc R . . H34B H 0.2165 0.6507 0.6856 0.079 Uiso 1 1 calc R . . H34C H 0.1472 0.5657 0.7121 0.079 Uiso 1 1 calc R . . C35 C 0.6299(2) 0.31065(17) 0.79576(18) 0.0513(5) Uani 1 1 d . . . H35A H 0.6036 0.2721 0.8306 0.077 Uiso 1 1 calc R . . H35B H 0.7093 0.3527 0.8341 0.077 Uiso 1 1 calc R . . H35C H 0.6112 0.2683 0.7380 0.077 Uiso 1 1 calc R . . C36 C 0.48978(14) 0.66231(12) 1.01414(12) 0.0278(3) Uani 1 1 d . . . C37 C 0.56411(13) 0.63841(11) 1.00027(11) 0.0245(3) Uani 1 1 d . . . C38 C 0.63389(14) 0.61274(12) 1.06023(11) 0.0276(3) Uani 1 1 d . . . H38 H 0.6477 0.6101 1.1207 0.033 Uiso 1 1 calc R . . C39 C 0.67884(13) 0.59175(11) 1.01145(11) 0.0246(3) Uani 1 1 d . . . C40 C 0.75769(13) 0.55885(12) 1.03481(12) 0.0278(3) Uani 1 1 d . . . C41 C 0.35055(17) 0.69727(16) 0.94802(17) 0.0450(5) Uani 1 1 d . . . H41A H 0.3106 0.6525 0.9715 0.068 Uiso 1 1 calc R . . H41B H 0.2988 0.6944 0.8871 0.068 Uiso 1 1 calc R . . H41C H 0.3926 0.7624 0.9922 0.068 Uiso 1 1 calc R . . C42 C 0.89357(16) 0.54787(15) 1.15842(15) 0.0415(4) Uani 1 1 d . . . H42A H 0.8657 0.4817 1.1239 0.062 Uiso 1 1 calc R . . H42B H 0.9237 0.5565 1.2253 0.062 Uiso 1 1 calc R . . H42C H 0.9509 0.5918 1.1485 0.062 Uiso 1 1 calc R . . C43 C 0.92072(17) 0.99740(16) 0.86845(13) 0.0473(5) Uani 1 1 d . . . H43A H 0.9584 0.9665 0.9034 0.071 Uiso 1 1 calc R . . H43B H 0.8817 1.0094 0.8965 0.071 Uiso 1 1 calc R . . H43C H 0.9741 1.0583 0.8705 0.071 Uiso 1 1 calc R . . C44 C 0.63827(16) 0.75739(15) 0.53213(13) 0.0426(5) Uani 1 1 d . . . H44A H 0.6581 0.7822 0.4877 0.064 Uiso 1 1 calc R . . H44B H 0.5652 0.7457 0.5145 0.064 Uiso 1 1 calc R . . H44C H 0.6386 0.6974 0.5313 0.064 Uiso 1 1 calc R . . C45 C 0.63481(18) 0.85412(13) 0.94211(12) 0.0431(5) Uani 1 1 d . . . H45A H 0.5925 0.8672 0.9654 0.065 Uiso 1 1 calc R . . H45B H 0.6905 0.9144 0.9455 0.065 Uiso 1 1 calc R . . H45C H 0.6702 0.8235 0.9805 0.065 Uiso 1 1 calc R . . C46 C 0.40040(19) 0.63070(13) 0.59849(13) 0.0436(5) Uani 1 1 d . . . H46A H 0.4037 0.5719 0.5977 0.065 Uiso 1 1 calc R . . H46B H 0.4324 0.6633 0.5635 0.065 Uiso 1 1 calc R . . H46C H 0.3242 0.6146 0.5695 0.065 Uiso 1 1 calc R . . C47 C 0.86565(16) 0.75034(14) 0.95605(13) 0.0418(5) Uani 1 1 d . . . H47A H 0.9146 0.7319 0.9985 0.063 Uiso 1 1 calc R . . H47B H 0.8226 0.7584 0.9813 0.063 Uiso 1 1 calc R . . H47C H 0.9088 0.8108 0.9498 0.063 Uiso 1 1 calc R . . C48 C 0.60500(15) 0.49577(15) 0.62663(12) 0.0406(4) Uani 1 1 d . . . H48A H 0.6292 0.5222 0.5849 0.061 Uiso 1 1 calc R . . H48B H 0.5324 0.4863 0.6069 0.061 Uiso 1 1 calc R . . H48C H 0.6020 0.4342 0.6239 0.061 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 0.01953(8) 0.02296(8) 0.02332(8) 0.00943(7) 0.01338(7) 0.01016(7) Cu2 0.02178(9) 0.02468(9) 0.02574(9) 0.01075(7) 0.01241(7) 0.01370(7) Cu3 0.02048(8) 0.02173(8) 0.02368(9) 0.00705(7) 0.00908(7) 0.01181(7) Cu4 0.02525(9) 0.01897(8) 0.02258(8) 0.00867(7) 0.01123(7) 0.01173(7) Cu5 0.02255(9) 0.01910(8) 0.02383(9) 0.00939(7) 0.01184(7) 0.01064(7) Cu6 0.02027(8) 0.02110(8) 0.02240(8) 0.00795(6) 0.01342(7) 0.00951(7) O1 0.0600(9) 0.0393(7) 0.0537(8) 0.0246(6) 0.0392(8) 0.0320(7) O2 0.0853(12) 0.0506(9) 0.0797(12) 0.0246(8) 0.0614(11) 0.0463(9) O3 0.0760(11) 0.0556(9) 0.0842(12) 0.0492(9) 0.0667(10) 0.0463(9) O4 0.0914(13) 0.0470(9) 0.0694(11) 0.0304(8) 0.0666(11) 0.0323(9) O5 0.0400(7) 0.0471(8) 0.0689(10) 0.0401(7) 0.0359(7) 0.0303(7) O6 0.0339(7) 0.0467(8) 0.0509(8) 0.0173(6) 0.0172(6) 0.0286(6) O7 0.0329(7) 0.0357(7) 0.0531(8) 0.0141(6) 0.0255(6) 0.0042(6) O8 0.0564(10) 0.0675(11) 0.1068(15) 0.0639(12) 0.0492(11) 0.0370(9) O9 0.0259(6) 0.0333(6) 0.0259(5) 0.0011(5) 0.0047(5) 0.0177(5) O10 0.0263(5) 0.0314(6) 0.0240(5) 0.0032(4) 0.0074(4) 0.0178(5) O11 0.0438(7) 0.0437(7) 0.0337(6) 0.0216(6) 0.0228(6) 0.0256(6) O12 0.0310(6) 0.0442(7) 0.0458(8) 0.0191(6) 0.0210(6) 0.0168(6) O13 0.0214(6) 0.0525(8) 0.0463(8) 0.0208(7) 0.0123(6) 0.0144(6) O14 0.0385(7) 0.0476(8) 0.0427(7) 0.0214(6) 0.0249(6) 0.0207(6) O15 0.0548(9) 0.0343(7) 0.0638(10) 0.0146(7) 0.0408(8) 0.0162(7) O16 0.0682(11) 0.0261(7) 0.0978(14) 0.0086(8) 0.0547(11) 0.0076(7) O17 0.0406(7) 0.0343(6) 0.0427(7) 0.0129(5) 0.0263(6) 0.0200(6) O18 0.0820(12) 0.0426(8) 0.0758(12) 0.0051(8) 0.0586(11) 0.0263(9) O19 0.0411(7) 0.0204(5) 0.0220(5) 0.0080(4) 0.0119(5) 0.0138(5) O20 0.0352(6) 0.0187(5) 0.0222(5) 0.0069(4) 0.0098(5) 0.0109(5) O21 0.0334(7) 0.0359(7) 0.0667(9) 0.0219(7) 0.0276(7) 0.0202(6) O22 0.0230(6) 0.0417(7) 0.0526(8) 0.0052(6) 0.0172(6) 0.0088(5) O23 0.0385(7) 0.0335(6) 0.0495(8) 0.0188(6) 0.0278(6) 0.0222(6) O24 0.0536(9) 0.0232(6) 0.0540(8) 0.0091(6) 0.0261(7) 0.0181(6) O25 0.0383(7) 0.0468(7) 0.0401(7) 0.0189(6) 0.0237(6) 0.0294(6) O26 0.0590(9) 0.0757(11) 0.0452(8) 0.0308(8) 0.0402(7) 0.0476(9) O27 0.0374(7) 0.0526(8) 0.0363(7) 0.0233(6) 0.0211(6) 0.0316(6) O28 0.0455(7) 0.0458(7) 0.0436(7) 0.0181(6) 0.0296(6) 0.0308(6) O29 0.0226(5) 0.0293(6) 0.0232(5) 0.0035(4) 0.0135(4) 0.0054(4) O30 0.0233(5) 0.0277(5) 0.0230(5) 0.0025(4) 0.0139(4) 0.0053(4) N1 0.0292(6) 0.0283(6) 0.0296(6) 0.0120(5) 0.0195(6) 0.0161(5) N2 0.0305(7) 0.0305(7) 0.0307(7) 0.0145(5) 0.0206(6) 0.0177(6) N3 0.0204(6) 0.0282(6) 0.0305(6) 0.0138(5) 0.0145(5) 0.0126(5) N4 0.0221(6) 0.0290(7) 0.0338(7) 0.0153(6) 0.0154(5) 0.0131(5) N5 0.0235(6) 0.0262(6) 0.0276(6) 0.0122(5) 0.0124(5) 0.0152(5) N6 0.0229(6) 0.0236(6) 0.0268(6) 0.0114(5) 0.0118(5) 0.0129(5) N7 0.0264(6) 0.0211(6) 0.0304(7) 0.0074(5) 0.0124(5) 0.0125(5) N8 0.0309(7) 0.0212(6) 0.0280(6) 0.0089(5) 0.0146(6) 0.0147(5) N9 0.0216(6) 0.0209(6) 0.0295(6) 0.0102(5) 0.0125(5) 0.0093(5) N10 0.0245(6) 0.0204(6) 0.0294(6) 0.0102(5) 0.0155(5) 0.0103(5) N11 0.0258(6) 0.0251(6) 0.0266(6) 0.0122(5) 0.0171(5) 0.0144(5) N12 0.0261(6) 0.0274(6) 0.0259(6) 0.0126(5) 0.0169(5) 0.0156(5) C1 0.0323(8) 0.0320(8) 0.0377(9) 0.0087(7) 0.0193(7) 0.0166(7) C2 0.0284(8) 0.0299(8) 0.0309(8) 0.0079(6) 0.0184(7) 0.0144(6) C3 0.0398(9) 0.0357(9) 0.0369(9) 0.0112(7) 0.0281(8) 0.0186(8) C4 0.0317(8) 0.0322(8) 0.0303(8) 0.0121(6) 0.0213(7) 0.0137(7) C5 0.0375(9) 0.0365(9) 0.0365(9) 0.0158(7) 0.0246(8) 0.0149(8) C6 0.0731(16) 0.0455(12) 0.0707(16) 0.0316(12) 0.0409(14) 0.0377(12) C7 0.0826(18) 0.0638(15) 0.105(2) 0.0620(16) 0.0735(18) 0.0526(15) C8 0.0282(8) 0.0341(8) 0.0297(8) 0.0115(6) 0.0148(6) 0.0197(7) C9 0.0222(7) 0.0312(8) 0.0280(7) 0.0113(6) 0.0127(6) 0.0148(6) C10 0.0204(7) 0.0343(8) 0.0357(8) 0.0110(7) 0.0137(6) 0.0120(6) C11 0.0227(7) 0.0287(8) 0.0331(8) 0.0105(6) 0.0152(6) 0.0100(6) C12 0.0338(9) 0.0320(9) 0.0436(10) 0.0153(8) 0.0228(8) 0.0108(7) C13 0.0678(14) 0.0496(12) 0.0795(16) 0.0454(12) 0.0532(13) 0.0437(12) C14 0.0638(16) 0.0417(12) 0.0792(18) 0.0226(12) 0.0500(15) 0.0046(11) C15 0.0352(8) 0.0266(7) 0.0331(8) 0.0155(6) 0.0194(7) 0.0203(7) C16 0.0272(7) 0.0233(7) 0.0267(7) 0.0116(6) 0.0125(6) 0.0149(6) C17 0.0260(7) 0.0272(7) 0.0254(7) 0.0112(6) 0.0089(6) 0.0151(6) C18 0.0221(7) 0.0221(7) 0.0269(7) 0.0083(6) 0.0092(6) 0.0114(6) C19 0.0242(7) 0.0253(7) 0.0359(8) 0.0099(6) 0.0129(7) 0.0116(6) C20 0.0710(15) 0.0494(12) 0.0532(12) 0.0344(10) 0.0463(12) 0.0366(11) C21 0.0249(10) 0.0868(19) 0.0831(19) 0.0387(16) 0.0256(11) 0.0215(11) C22 0.0345(9) 0.0262(8) 0.0434(10) 0.0104(7) 0.0171(8) 0.0114(7) C23 0.0288(8) 0.0209(7) 0.0303(8) 0.0066(6) 0.0102(6) 0.0115(6) C24 0.0386(9) 0.0222(7) 0.0340(8) 0.0057(6) 0.0153(7) 0.0164(7) C25 0.0354(8) 0.0253(7) 0.0265(7) 0.0069(6) 0.0140(7) 0.0177(7) C26 0.0470(10) 0.0320(8) 0.0347(9) 0.0119(7) 0.0236(8) 0.0233(8) C27 0.0747(19) 0.0600(16) 0.102(2) 0.0298(16) 0.0679(19) 0.0230(14) C28 0.0542(13) 0.0550(13) 0.0648(15) 0.0227(11) 0.0435(12) 0.0259(11) C29 0.0251(7) 0.0319(8) 0.0288(8) 0.0101(6) 0.0135(6) 0.0114(6) C30 0.0216(7) 0.0246(7) 0.0269(7) 0.0082(6) 0.0119(6) 0.0075(6) C31 0.0269(7) 0.0214(7) 0.0298(8) 0.0075(6) 0.0141(6) 0.0052(6) C32 0.0291(7) 0.0201(6) 0.0261(7) 0.0078(5) 0.0156(6) 0.0093(6) C33 0.0393(9) 0.0261(7) 0.0314(8) 0.0111(6) 0.0220(7) 0.0165(7) C34 0.0536(13) 0.0602(14) 0.0763(16) 0.0403(13) 0.0425(13) 0.0419(12) C35 0.0559(13) 0.0550(13) 0.0699(15) 0.0284(11) 0.0394(12) 0.0409(11) C36 0.0307(8) 0.0264(7) 0.0345(8) 0.0126(6) 0.0217(7) 0.0156(6) C37 0.0279(7) 0.0261(7) 0.0273(7) 0.0124(6) 0.0186(6) 0.0146(6) C38 0.0333(8) 0.0318(8) 0.0277(7) 0.0153(6) 0.0204(7) 0.0187(7) C39 0.0268(7) 0.0269(7) 0.0267(7) 0.0131(6) 0.0163(6) 0.0155(6) C40 0.0287(8) 0.0275(7) 0.0335(8) 0.0149(6) 0.0188(7) 0.0155(6) C41 0.0400(10) 0.0487(11) 0.0581(13) 0.0174(10) 0.0258(10) 0.0313(9) C42 0.0328(9) 0.0504(11) 0.0507(11) 0.0275(9) 0.0201(9) 0.0276(9) C43 0.0397(10) 0.0507(12) 0.0303(9) -0.0036(8) 0.0009(8) 0.0268(9) C44 0.0367(10) 0.0439(10) 0.0301(9) -0.0048(8) 0.0036(7) 0.0238(9) C45 0.0565(12) 0.0279(8) 0.0252(8) 0.0072(7) 0.0103(8) 0.0167(8) C46 0.0582(12) 0.0278(8) 0.0254(8) 0.0057(7) 0.0133(8) 0.0153(8) C47 0.0337(9) 0.0387(10) 0.0295(8) -0.0030(7) 0.0173(7) 0.0015(8) C48 0.0322(9) 0.0436(10) 0.0253(8) -0.0012(7) 0.0145(7) 0.0055(8) _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 O29 1.9026(11) . ? Cu1 O30 1.9088(16) . ? Cu1 N3 1.9911(19) . ? Cu1 N1 1.9918(14) . ? Cu1 Cu6 3.0087(9) . ? Cu2 O10 1.9011(14) . ? Cu2 O9 1.9022(13) . ? Cu2 N4 1.9720(16) . ? Cu2 N2 1.9817(15) . ? Cu2 Cu3 2.9907(7) . ? Cu3 O9 1.9094(14) . ? Cu3 O10 1.9127(12) . ? Cu3 N5 1.9644(17) . ? Cu3 N7 1.9807(15) . ? Cu4 O20 1.9098(14) . ? Cu4 O19 1.9194(12) . ? Cu4 N6 1.9678(14) . ? Cu4 N8 1.9831(18) . ? Cu4 Cu5 3.0101(8) . ? Cu5 O19 1.9098(14) . ? Cu5 O20 1.9106(12) . ? Cu5 N9 1.9677(16) . ? Cu5 N11 1.9832(14) . ? Cu6 O30 1.9162(11) . ? Cu6 O29 1.9168(16) . ? Cu6 N12 1.9651(13) . ? Cu6 N10 1.9894(18) . ? O1 C1 1.330(2) . ? O1 C6 1.441(3) . ? O2 C1 1.200(2) . ? O3 C5 1.328(2) . ? O3 C7 1.443(3) . ? O4 C5 1.188(2) . ? O5 C8 1.333(2) . ? O5 C13 1.439(2) . ? O6 C8 1.199(2) . ? O7 C12 1.334(2) . ? O7 C14 1.444(3) . ? O8 C12 1.192(3) . ? O9 C43 1.412(2) . ? O10 C44 1.409(2) . ? O11 C15 1.330(2) . ? O11 C20 1.450(2) . ? O12 C15 1.202(2) . ? O13 C19 1.325(2) . ? O13 C21 1.450(3) . ? O14 C19 1.202(2) . ? O15 C22 1.318(2) . ? O15 C27 1.439(3) . ? O16 C22 1.203(2) . ? O17 C26 1.326(2) . ? O17 C28 1.443(2) . ? O18 C26 1.198(2) . ? O19 C45 1.411(2) . ? O20 C46 1.408(2) . ? O21 C29 1.333(2) . ? O21 C34 1.445(2) . ? O22 C29 1.197(2) . ? O23 C33 1.331(2) . ? O23 C35 1.446(2) . ? O24 C33 1.200(2) . ? O25 C36 1.327(2) . ? O25 C41 1.448(2) . ? O26 C36 1.195(2) . ? O27 C40 1.337(2) . ? O27 C42 1.442(2) . ? O28 C40 1.198(2) . ? O29 C47 1.410(2) . ? O30 C48 1.406(2) . ? N1 N2 1.3444(19) . ? N1 C2 1.354(2) . ? N2 C4 1.348(2) . ? N3 N4 1.3436(19) . ? N3 C9 1.347(2) . ? N4 C11 1.350(2) . ? N5 N6 1.3355(19) . ? N5 C16 1.345(2) . ? N6 C18 1.352(2) . ? N7 N8 1.343(2) . ? N7 C23 1.350(2) . ? N8 C25 1.351(2) . ? N9 N10 1.3453(18) . ? N9 C30 1.349(2) . ? N10 C32 1.348(2) . ? N11 N12 1.3416(18) . ? N11 C37 1.3525(19) . ? N12 C39 1.348(2) . ? C1 C2 1.468(2) . ? C2 C3 1.384(2) . ? C3 C4 1.381(2) . ? C3 H3 0.9500 . ? C4 C5 1.475(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.466(2) . ? C9 C10 1.381(2) . ? C10 C11 1.385(2) . ? C10 H10 0.9500 . ? C11 C12 1.471(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.471(2) . ? C16 C17 1.387(2) . ? C17 C18 1.388(2) . ? C17 H17 0.9500 . ? C18 C19 1.470(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.471(3) . ? C23 C24 1.383(3) . ? C24 C25 1.379(3) . ? C24 H24 0.9500 . ? C25 C26 1.470(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.470(2) . ? C30 C31 1.385(2) . ? C31 C32 1.380(2) . ? C31 H31 0.9500 . ? C32 C33 1.475(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.472(2) . ? C37 C38 1.385(2) . ? C38 C39 1.386(2) . ? C38 H38 0.9500 . ? C39 C40 1.471(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 O29 Cu1 O30 76.39(6) . . ? O29 Cu1 N3 97.47(7) . . ? O30 Cu1 N3 173.64(5) . . ? O29 Cu1 N1 168.20(6) . . ? O30 Cu1 N1 100.06(7) . . ? N3 Cu1 N1 85.63(7) . . ? O29 Cu1 Cu6 38.19(5) . . ? O30 Cu1 Cu6 38.22(4) . . ? N3 Cu1 Cu6 135.66(4) . . ? N1 Cu1 Cu6 137.48(5) . . ? O10 Cu2 O9 76.77(7) . . ? O10 Cu2 N4 169.83(6) . . ? O9 Cu2 N4 99.01(7) . . ? O10 Cu2 N2 98.06(7) . . ? O9 Cu2 N2 173.06(6) . . ? N4 Cu2 N2 85.32(7) . . ? O10 Cu2 Cu3 38.49(4) . . ? O9 Cu2 Cu3 38.40(4) . . ? N4 Cu2 Cu3 137.16(5) . . ? N2 Cu2 Cu3 136.54(5) . . ? O9 Cu3 O10 76.33(7) . . ? O9 Cu3 N5 170.25(5) . . ? O10 Cu3 N5 95.78(7) . . ? O9 Cu3 N7 98.28(7) . . ? O10 Cu3 N7 167.34(6) . . ? N5 Cu3 N7 88.26(7) . . ? O9 Cu3 Cu2 38.23(4) . . ? O10 Cu3 Cu2 38.22(4) . . ? N5 Cu3 Cu2 133.97(5) . . ? N7 Cu3 Cu2 136.03(5) . . ? O20 Cu4 O19 76.07(6) . . ? O20 Cu4 N6 96.51(7) . . ? O19 Cu4 N6 171.42(5) . . ? O20 Cu4 N8 166.01(6) . . ? O19 Cu4 N8 98.38(7) . . ? N6 Cu4 N8 87.85(7) . . ? O20 Cu4 Cu5 38.02(4) . . ? O19 Cu4 Cu5 38.07(4) . . ? N6 Cu4 Cu5 134.46(5) . . ? N8 Cu4 Cu5 135.40(5) . . ? O19 Cu5 O20 76.28(6) . . ? O19 Cu5 N9 172.88(5) . . ? O20 Cu5 N9 97.14(6) . . ? O19 Cu5 N11 99.05(7) . . ? O20 Cu5 N11 167.51(5) . . ? N9 Cu5 N11 86.84(7) . . ? O19 Cu5 Cu4 38.29(4) . . ? O20 Cu5 Cu4 38.00(4) . . ? N9 Cu5 Cu4 135.12(4) . . ? N11 Cu5 Cu4 136.48(5) . . ? O30 Cu6 O29 75.89(6) . . ? O30 Cu6 N12 171.49(5) . . ? O29 Cu6 N12 96.29(7) . . ? O30 Cu6 N10 99.54(6) . . ? O29 Cu6 N10 166.28(5) . . ? N12 Cu6 N10 87.31(7) . . ? O30 Cu6 Cu1 38.05(5) . . ? O29 Cu6 Cu1 37.86(4) . . ? N12 Cu6 Cu1 134.12(5) . . ? N10 Cu6 Cu1 136.52(4) . . ? C1 O1 C6 116.42(17) . . ? C5 O3 C7 118.06(17) . . ? C8 O5 C13 116.55(16) . . ? C12 O7 C14 115.83(19) . . ? C43 O9 Cu2 127.47(11) . . ? C43 O9 Cu3 129.10(12) . . ? Cu2 O9 Cu3 103.37(7) . . ? C44 O10 Cu2 126.61(11) . . ? C44 O10 Cu3 129.95(11) . . ? Cu2 O10 Cu3 103.29(7) . . ? C15 O11 C20 115.75(16) . . ? C19 O13 C21 114.82(18) . . ? C22 O15 C27 117.84(19) . . ? C26 O17 C28 116.32(16) . . ? C45 O19 Cu5 128.31(11) . . ? C45 O19 Cu4 127.90(11) . . ? Cu5 O19 Cu4 103.64(7) . . ? C46 O20 Cu4 128.55(11) . . ? C46 O20 Cu5 127.44(11) . . ? Cu4 O20 Cu5 103.98(7) . . ? C29 O21 C34 116.12(16) . . ? C33 O23 C35 115.18(16) . . ? C36 O25 C41 114.61(15) . . ? C40 O27 C42 115.48(15) . . ? C47 O29 Cu1 127.15(11) . . ? C47 O29 Cu6 128.89(11) . . ? Cu1 O29 Cu6 103.95(7) . . ? C48 O30 Cu1 128.27(11) . . ? C48 O30 Cu6 127.61(11) . . ? Cu1 O30 Cu6 103.73(7) . . ? N2 N1 C2 107.63(13) . . ? N2 N1 Cu1 112.99(10) . . ? C2 N1 Cu1 136.17(12) . . ? N1 N2 C4 108.55(13) . . ? N1 N2 Cu2 120.73(10) . . ? C4 N2 Cu2 127.58(12) . . ? N4 N3 C9 108.23(13) . . ? N4 N3 Cu1 119.18(10) . . ? C9 N3 Cu1 129.27(12) . . ? N3 N4 C11 108.04(13) . . ? N3 N4 Cu2 114.66(11) . . ? C11 N4 Cu2 134.23(12) . . ? N6 N5 C16 108.69(13) . . ? N6 N5 Cu3 117.90(10) . . ? C16 N5 Cu3 133.41(11) . . ? N5 N6 C18 108.11(13) . . ? N5 N6 Cu4 117.78(10) . . ? C18 N6 Cu4 134.10(11) . . ? N8 N7 C23 107.97(14) . . ? N8 N7 Cu3 116.74(10) . . ? C23 N7 Cu3 134.57(12) . . ? N7 N8 C25 108.17(14) . . ? N7 N8 Cu4 118.23(10) . . ? C25 N8 Cu4 132.97(12) . . ? N10 N9 C30 108.46(13) . . ? N10 N9 Cu5 119.21(10) . . ? C30 N9 Cu5 130.29(12) . . ? N9 N10 C32 107.68(13) . . ? N9 N10 Cu6 115.99(10) . . ? C32 N10 Cu6 135.38(12) . . ? N12 N11 C37 107.67(13) . . ? N12 N11 Cu5 115.61(10) . . ? C37 N11 Cu5 136.67(11) . . ? N11 N12 C39 108.60(12) . . ? N11 N12 Cu6 119.73(10) . . ? C39 N12 Cu6 131.01(11) . . ? O2 C1 O1 124.27(18) . . ? O2 C1 C2 123.70(18) . . ? O1 C1 C2 112.03(15) . . ? N1 C2 C3 109.86(15) . . ? N1 C2 C1 123.02(15) . . ? C3 C2 C1 127.12(15) . . ? C4 C3 C2 104.29(14) . . ? C4 C3 H3 127.9 . . ? C2 C3 H3 127.9 . . ? N2 C4 C3 109.68(15) . . ? N2 C4 C5 120.37(16) . . ? C3 C4 C5 129.89(15) . . ? O4 C5 O3 124.82(18) . . ? O4 C5 C4 125.00(19) . . ? O3 C5 C4 110.18(15) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 H7A 109.5 . . ? O3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O6 C8 O5 124.18(17) . . ? O6 C8 C9 125.35(17) . . ? O5 C8 C9 110.47(14) . . ? N3 C9 C10 109.80(15) . . ? N3 C9 C8 120.50(15) . . ? C10 C9 C8 129.62(15) . . ? C9 C10 C11 104.24(14) . . ? C9 C10 H10 127.9 . . ? C11 C10 H10 127.9 . . ? N4 C11 C10 109.68(15) . . ? N4 C11 C12 118.30(16) . . ? C10 C11 C12 131.79(16) . . ? O8 C12 O7 124.48(18) . . ? O8 C12 C11 124.44(18) . . ? O7 C12 C11 111.03(17) . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 C14 H14A 109.5 . . ? O7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O12 C15 O11 125.36(17) . . ? O12 C15 C16 122.88(16) . . ? O11 C15 C16 111.76(15) . . ? N5 C16 C17 109.59(14) . . ? N5 C16 C15 116.98(14) . . ? C17 C16 C15 133.40(15) . . ? C16 C17 C18 104.02(14) . . ? C16 C17 H17 128.0 . . ? C18 C17 H17 128.0 . . ? N6 C18 C17 109.59(14) . . ? N6 C18 C19 117.20(14) . . ? C17 C18 C19 133.12(15) . . ? O14 C19 O13 125.19(17) . . ? O14 C19 C18 123.26(16) . . ? O13 C19 C18 111.53(15) . . ? O11 C20 H20A 109.5 . . ? O11 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O11 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O13 C21 H21A 109.5 . . ? O13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O16 C22 O15 124.9(2) . . ? O16 C22 C23 123.85(19) . . ? O15 C22 C23 111.23(15) . . ? N7 C23 C24 109.78(16) . . ? N7 C23 C22 121.50(16) . . ? C24 C23 C22 128.67(16) . . ? C25 C24 C23 104.31(15) . . ? C25 C24 H24 127.8 . . ? C23 C24 H24 127.8 . . ? N8 C25 C24 109.76(16) . . ? N8 C25 C26 121.41(16) . . ? C24 C25 C26 128.60(15) . . ? O18 C26 O17 124.34(19) . . ? O18 C26 C25 124.45(19) . . ? O17 C26 C25 111.13(15) . . ? O15 C27 H27A 109.5 . . ? O15 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O15 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O17 C28 H28A 109.5 . . ? O17 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O17 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O22 C29 O21 124.05(17) . . ? O22 C29 C30 123.95(17) . . ? O21 C29 C30 111.99(14) . . ? N9 C30 C31 109.51(14) . . ? N9 C30 C29 122.09(15) . . ? C31 C30 C29 128.40(15) . . ? C32 C31 C30 104.20(14) . . ? C32 C31 H31 127.9 . . ? C30 C31 H31 127.9 . . ? N10 C32 C31 110.15(15) . . ? N10 C32 C33 122.41(15) . . ? C31 C32 C33 127.25(15) . . ? O24 C33 O23 125.02(17) . . ? O24 C33 C32 123.43(17) . . ? O23 C33 C32 111.55(14) . . ? O21 C34 H34A 109.5 . . ? O21 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O21 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O23 C35 H35A 109.5 . . ? O23 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O23 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O26 C36 O25 124.47(16) . . ? O26 C36 C37 123.58(16) . . ? O25 C36 C37 111.95(14) . . ? N11 C37 C38 110.08(13) . . ? N11 C37 C36 122.49(14) . . ? C38 C37 C36 127.37(14) . . ? C37 C38 C39 103.92(14) . . ? C37 C38 H38 128.0 . . ? C39 C38 H38 128.0 . . ? N12 C39 C38 109.72(14) . . ? N12 C39 C40 118.41(14) . . ? C38 C39 C40 131.86(14) . . ? O28 C40 O27 124.95(16) . . ? O28 C40 C39 124.25(16) . . ? O27 C40 C39 110.78(14) . . ? O25 C41 H41A 109.5 . . ? O25 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O25 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O27 C42 H42A 109.5 . . ? O27 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O27 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O9 C43 H43A 109.5 . . ? O9 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O9 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O10 C44 H44A 109.5 . . ? O10 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O10 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O19 C45 H45A 109.5 . . ? O19 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O19 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O20 C46 H46A 109.5 . . ? O20 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O20 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O29 C47 H47A 109.5 . . ? O29 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O29 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O30 C48 H48A 109.5 . . ? O30 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O30 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 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 O10 Cu2 Cu3 O9 174.09(9) . . . . ? N4 Cu2 Cu3 O9 8.24(9) . . . . ? N2 Cu2 Cu3 O9 172.73(9) . . . . ? O9 Cu2 Cu3 O10 -174.09(9) . . . . ? N4 Cu2 Cu3 O10 -165.85(9) . . . . ? N2 Cu2 Cu3 O10 -1.36(8) . . . . ? O10 Cu2 Cu3 N5 2.84(8) . . . . ? O9 Cu2 Cu3 N5 -171.25(9) . . . . ? N4 Cu2 Cu3 N5 -163.01(8) . . . . ? N2 Cu2 Cu3 N5 1.48(8) . . . . ? O10 Cu2 Cu3 N7 162.78(9) . . . . ? O9 Cu2 Cu3 N7 -11.32(9) . . . . ? N4 Cu2 Cu3 N7 -3.07(8) . . . . ? N2 Cu2 Cu3 N7 161.41(8) . . . . ? O20 Cu4 Cu5 O19 177.86(9) . . . . ? N6 Cu4 Cu5 O19 173.64(9) . . . . ? N8 Cu4 Cu5 O19 16.65(9) . . . . ? O19 Cu4 Cu5 O20 -177.86(9) . . . . ? N6 Cu4 Cu5 O20 -4.22(8) . . . . ? N8 Cu4 Cu5 O20 -161.20(9) . . . . ? O20 Cu4 Cu5 N9 1.95(8) . . . . ? O19 Cu4 Cu5 N9 -175.91(9) . . . . ? N6 Cu4 Cu5 N9 -2.27(8) . . . . ? N8 Cu4 Cu5 N9 -159.25(8) . . . . ? O20 Cu4 Cu5 N11 162.76(8) . . . . ? O19 Cu4 Cu5 N11 -15.10(8) . . . . ? N6 Cu4 Cu5 N11 158.54(8) . . . . ? N8 Cu4 Cu5 N11 1.55(8) . . . . ? O29 Cu1 Cu6 O30 177.70(9) . . . . ? N3 Cu1 Cu6 O30 177.37(8) . . . . ? N1 Cu1 Cu6 O30 14.70(8) . . . . ? O30 Cu1 Cu6 O29 -177.70(9) . . . . ? N3 Cu1 Cu6 O29 -0.32(8) . . . . ? N1 Cu1 Cu6 O29 -163.00(9) . . . . ? O29 Cu1 Cu6 N12 2.69(8) . . . . ? O30 Cu1 Cu6 N12 -175.00(8) . . . . ? N3 Cu1 Cu6 N12 2.37(8) . . . . ? N1 Cu1 Cu6 N12 -160.30(8) . . . . ? O29 Cu1 Cu6 N10 160.71(8) . . . . ? O30 Cu1 Cu6 N10 -16.98(8) . . . . ? N3 Cu1 Cu6 N10 160.39(8) . . . . ? N1 Cu1 Cu6 N10 -2.28(8) . . . . ? O10 Cu2 O9 C43 173.78(18) . . . . ? N4 Cu2 O9 C43 3.21(18) . . . . ? N2 Cu2 O9 C43 131.5(4) . . . . ? Cu3 Cu2 O9 C43 177.5(2) . . . . ? O10 Cu2 O9 Cu3 -3.77(6) . . . . ? N4 Cu2 O9 Cu3 -174.34(6) . . . . ? N2 Cu2 O9 Cu3 -46.1(5) . . . . ? O10 Cu3 O9 C43 -173.74(19) . . . . ? N5 Cu3 O9 C43 -137.2(3) . . . . ? N7 Cu3 O9 C43 -5.41(18) . . . . ? Cu2 Cu3 O9 C43 -177.5(2) . . . . ? O10 Cu3 O9 Cu2 3.76(6) . . . . ? N5 Cu3 O9 Cu2 40.3(4) . . . . ? N7 Cu3 O9 Cu2 172.09(6) . . . . ? O9 Cu2 O10 C44 179.65(17) . . . . ? N4 Cu2 O10 C44 -113.9(3) . . . . ? N2 Cu2 O10 C44 -5.06(17) . . . . ? Cu3 Cu2 O10 C44 175.89(19) . . . . ? O9 Cu2 O10 Cu3 3.76(6) . . . . ? N4 Cu2 O10 Cu3 70.3(3) . . . . ? N2 Cu2 O10 Cu3 179.05(6) . . . . ? O9 Cu3 O10 C44 -179.45(18) . . . . ? N5 Cu3 O10 C44 6.36(17) . . . . ? N7 Cu3 O10 C44 114.5(3) . . . . ? Cu2 Cu3 O10 C44 -175.7(2) . . . . ? O9 Cu3 O10 Cu2 -3.76(6) . . . . ? N5 Cu3 O10 Cu2 -177.95(6) . . . . ? N7 Cu3 O10 Cu2 -69.8(3) . . . . ? O20 Cu5 O19 C45 -174.43(18) . . . . ? N9 Cu5 O19 C45 -151.8(4) . . . . ? N11 Cu5 O19 C45 -6.25(17) . . . . ? Cu4 Cu5 O19 C45 -175.8(2) . . . . ? O20 Cu5 O19 Cu4 1.36(6) . . . . ? N9 Cu5 O19 Cu4 24.0(5) . . . . ? N11 Cu5 O19 Cu4 169.54(6) . . . . ? O20 Cu4 O19 C45 174.45(17) . . . . ? N6 Cu4 O19 C45 143.8(3) . . . . ? N8 Cu4 O19 C45 7.55(17) . . . . ? Cu5 Cu4 O19 C45 175.8(2) . . . . ? O20 Cu4 O19 Cu5 -1.36(6) . . . . ? N6 Cu4 O19 Cu5 -32.0(4) . . . . ? N8 Cu4 O19 Cu5 -168.26(6) . . . . ? O19 Cu4 O20 C46 -176.76(17) . . . . ? N6 Cu4 O20 C46 -1.15(17) . . . . ? N8 Cu4 O20 C46 -108.7(3) . . . . ? Cu5 Cu4 O20 C46 -178.1(2) . . . . ? O19 Cu4 O20 Cu5 1.36(6) . . . . ? N6 Cu4 O20 Cu5 176.97(6) . . . . ? N8 Cu4 O20 Cu5 69.4(2) . . . . ? O19 Cu5 O20 C46 176.78(17) . . . . ? N9 Cu5 O20 C46 -0.47(17) . . . . ? N11 Cu5 O20 C46 107.5(3) . . . . ? Cu4 Cu5 O20 C46 178.14(19) . . . . ? O19 Cu5 O20 Cu4 -1.37(6) . . . . ? N9 Cu5 O20 Cu4 -178.61(6) . . . . ? N11 Cu5 O20 Cu4 -70.6(3) . . . . ? O30 Cu1 O29 C47 -179.59(17) . . . . ? N3 Cu1 O29 C47 -1.28(16) . . . . ? N1 Cu1 O29 C47 -105.9(3) . . . . ? Cu6 Cu1 O29 C47 178.95(19) . . . . ? O30 Cu1 O29 Cu6 1.46(5) . . . . ? N3 Cu1 O29 Cu6 179.77(6) . . . . ? N1 Cu1 O29 Cu6 75.2(3) . . . . ? O30 Cu6 O29 C47 179.61(17) . . . . ? N12 Cu6 O29 C47 3.02(17) . . . . ? N10 Cu6 O29 C47 107.6(2) . . . . ? Cu1 Cu6 O29 C47 -178.92(19) . . . . ? O30 Cu6 O29 Cu1 -1.46(5) . . . . ? N12 Cu6 O29 Cu1 -178.05(6) . . . . ? N10 Cu6 O29 Cu1 -73.4(2) . . . . ? O29 Cu1 O30 C48 171.82(17) . . . . ? N3 Cu1 O30 C48 156.5(5) . . . . ? N1 Cu1 O30 C48 3.31(16) . . . . ? Cu6 Cu1 O30 C48 173.28(19) . . . . ? O29 Cu1 O30 Cu6 -1.46(5) . . . . ? N3 Cu1 O30 Cu6 -16.8(5) . . . . ? N1 Cu1 O30 Cu6 -169.97(6) . . . . ? O29 Cu6 O30 C48 -171.88(16) . . . . ? N12 Cu6 O30 C48 -148.4(3) . . . . ? N10 Cu6 O30 C48 -5.10(16) . . . . ? Cu1 Cu6 O30 C48 -173.34(19) . . . . ? O29 Cu6 O30 Cu1 1.46(5) . . . . ? N12 Cu6 O30 Cu1 25.0(4) . . . . ? N10 Cu6 O30 Cu1 168.24(6) . . . . ? O29 Cu1 N1 N2 44.0(3) . . . . ? O30 Cu1 N1 N2 115.34(11) . . . . ? N3 Cu1 N1 N2 -61.79(11) . . . . ? Cu6 Cu1 N1 N2 106.16(11) . . . . ? O29 Cu1 N1 C2 -159.5(2) . . . . ? O30 Cu1 N1 C2 -88.17(17) . . . . ? N3 Cu1 N1 C2 94.70(17) . . . . ? Cu6 Cu1 N1 C2 -97.35(17) . . . . ? C2 N1 N2 C4 -0.01(18) . . . . ? Cu1 N1 N2 C4 163.14(11) . . . . ? C2 N1 N2 Cu2 -161.43(11) . . . . ? Cu1 N1 N2 Cu2 1.72(15) . . . . ? O10 Cu2 N2 N1 -108.20(13) . . . . ? O9 Cu2 N2 N1 -66.8(5) . . . . ? N4 Cu2 N2 N1 62.15(13) . . . . ? Cu3 Cu2 N2 N1 -107.34(12) . . . . ? O10 Cu2 N2 C4 94.21(15) . . . . ? O9 Cu2 N2 C4 135.6(4) . . . . ? N4 Cu2 N2 C4 -95.45(15) . . . . ? Cu3 Cu2 N2 C4 95.06(15) . . . . ? O29 Cu1 N3 N4 -106.41(12) . . . . ? O30 Cu1 N3 N4 -91.4(5) . . . . ? N1 Cu1 N3 N4 62.14(12) . . . . ? Cu6 Cu1 N3 N4 -106.21(11) . . . . ? O29 Cu1 N3 C9 96.76(14) . . . . ? O30 Cu1 N3 C9 111.8(5) . . . . ? N1 Cu1 N3 C9 -94.68(15) . . . . ? Cu6 Cu1 N3 C9 96.97(14) . . . . ? C9 N3 N4 C11 0.22(18) . . . . ? Cu1 N3 N4 C11 -161.07(11) . . . . ? C9 N3 N4 Cu2 163.32(11) . . . . ? Cu1 N3 N4 Cu2 2.03(15) . . . . ? O10 Cu2 N4 N3 47.9(4) . . . . ? O9 Cu2 N4 N3 112.60(12) . . . . ? N2 Cu2 N4 N3 -61.94(12) . . . . ? Cu3 Cu2 N4 N3 107.43(11) . . . . ? O10 Cu2 N4 C11 -154.8(3) . . . . ? O9 Cu2 N4 C11 -90.09(17) . . . . ? N2 Cu2 N4 C11 95.37(17) . . . . ? Cu3 Cu2 N4 C11 -95.26(17) . . . . ? O9 Cu3 N5 N6 72.4(4) . . . . ? O10 Cu3 N5 N6 107.95(11) . . . . ? N7 Cu3 N5 N6 -60.03(11) . . . . ? Cu2 Cu3 N5 N6 106.19(11) . . . . ? O9 Cu3 N5 C16 -108.0(3) . . . . ? O10 Cu3 N5 C16 -72.52(15) . . . . ? N7 Cu3 N5 C16 119.50(15) . . . . ? Cu2 Cu3 N5 C16 -74.29(16) . . . . ? C16 N5 N6 C18 -0.46(17) . . . . ? Cu3 N5 N6 C18 179.18(10) . . . . ? C16 N5 N6 Cu4 -179.62(10) . . . . ? Cu3 N5 N6 Cu4 0.02(15) . . . . ? O20 Cu4 N6 N5 -107.26(12) . . . . ? O19 Cu4 N6 N5 -77.4(4) . . . . ? N8 Cu4 N6 N5 59.41(12) . . . . ? Cu5 Cu4 N6 N5 -104.65(11) . . . . ? O20 Cu4 N6 C18 73.85(16) . . . . ? O19 Cu4 N6 C18 103.7(4) . . . . ? N8 Cu4 N6 C18 -119.48(15) . . . . ? Cu5 Cu4 N6 C18 76.46(16) . . . . ? O9 Cu3 N7 N8 -113.40(12) . . . . ? O10 Cu3 N7 N8 -49.6(3) . . . . ? N5 Cu3 N7 N8 59.35(12) . . . . ? Cu2 Cu3 N7 N8 -106.35(11) . . . . ? O9 Cu3 N7 C23 77.75(17) . . . . ? O10 Cu3 N7 C23 141.5(2) . . . . ? N5 Cu3 N7 C23 -109.50(17) . . . . ? Cu2 Cu3 N7 C23 84.80(17) . . . . ? C23 N7 N8 C25 -0.29(17) . . . . ? Cu3 N7 N8 C25 -171.97(10) . . . . ? C23 N7 N8 Cu4 171.76(11) . . . . ? Cu3 N7 N8 Cu4 0.08(15) . . . . ? O20 Cu4 N8 N7 49.2(3) . . . . ? O19 Cu4 N8 N7 114.64(12) . . . . ? N6 Cu4 N8 N7 -59.44(12) . . . . ? Cu5 Cu4 N8 N7 104.35(11) . . . . ? O20 Cu4 N8 C25 -141.2(2) . . . . ? O19 Cu4 N8 C25 -75.71(16) . . . . ? N6 Cu4 N8 C25 110.22(16) . . . . ? Cu5 Cu4 N8 C25 -86.00(16) . . . . ? O19 Cu5 N9 N10 88.5(5) . . . . ? O20 Cu5 N9 N10 110.59(12) . . . . ? N11 Cu5 N9 N10 -57.52(12) . . . . ? Cu4 Cu5 N9 N10 109.38(11) . . . . ? O19 Cu5 N9 C30 -109.8(4) . . . . ? O20 Cu5 N9 C30 -87.68(15) . . . . ? N11 Cu5 N9 C30 104.22(15) . . . . ? Cu4 Cu5 N9 C30 -88.89(15) . . . . ? C30 N9 N10 C32 0.29(17) . . . . ? Cu5 N9 N10 C32 165.69(10) . . . . ? C30 N9 N10 Cu6 -170.31(10) . . . . ? Cu5 N9 N10 Cu6 -4.91(14) . . . . ? O30 Cu6 N10 N9 -112.74(11) . . . . ? O29 Cu6 N10 N9 -43.5(3) . . . . ? N12 Cu6 N10 N9 62.17(11) . . . . ? Cu1 Cu6 N10 N9 -102.22(11) . . . . ? O30 Cu6 N10 C32 80.06(16) . . . . ? O29 Cu6 N10 C32 149.32(19) . . . . ? N12 Cu6 N10 C32 -105.03(16) . . . . ? Cu1 Cu6 N10 C32 90.58(16) . . . . ? O19 Cu5 N11 N12 -111.75(11) . . . . ? O20 Cu5 N11 N12 -44.8(3) . . . . ? N9 Cu5 N11 N12 64.23(11) . . . . ? Cu4 Cu5 N11 N12 -102.34(11) . . . . ? O19 Cu5 N11 C37 71.11(16) . . . . ? O20 Cu5 N11 C37 138.0(2) . . . . ? N9 Cu5 N11 C37 -112.91(16) . . . . ? Cu4 Cu5 N11 C37 80.52(17) . . . . ? C37 N11 N12 C39 -0.87(17) . . . . ? Cu5 N11 N12 C39 -178.81(10) . . . . ? C37 N11 N12 Cu6 170.83(10) . . . . ? Cu5 N11 N12 Cu6 -7.11(15) . . . . ? O30 Cu6 N12 N11 88.2(4) . . . . ? O29 Cu6 N12 N11 111.10(12) . . . . ? N10 Cu6 N12 N11 -55.63(12) . . . . ? Cu1 Cu6 N12 N11 109.43(11) . . . . ? O30 Cu6 N12 C39 -102.3(4) . . . . ? O29 Cu6 N12 C39 -79.35(15) . . . . ? N10 Cu6 N12 C39 113.93(15) . . . . ? Cu1 Cu6 N12 C39 -81.02(15) . . . . ? C6 O1 C1 O2 -5.4(3) . . . . ? C6 O1 C1 C2 174.79(18) . . . . ? N2 N1 C2 C3 -0.05(19) . . . . ? Cu1 N1 C2 C3 -157.39(14) . . . . ? N2 N1 C2 C1 178.84(15) . . . . ? Cu1 N1 C2 C1 21.5(3) . . . . ? O2 C1 C2 N1 179.46(19) . . . . ? O1 C1 C2 N1 -0.7(2) . . . . ? O2 C1 C2 C3 -1.8(3) . . . . ? O1 C1 C2 C3 177.99(18) . . . . ? N1 C2 C3 C4 0.1(2) . . . . ? C1 C2 C3 C4 -178.74(17) . . . . ? N1 N2 C4 C3 0.1(2) . . . . ? Cu2 N2 C4 C3 159.86(13) . . . . ? N1 N2 C4 C5 -177.33(15) . . . . ? Cu2 N2 C4 C5 -17.6(2) . . . . ? C2 C3 C4 N2 -0.1(2) . . . . ? C2 C3 C4 C5 176.98(19) . . . . ? C7 O3 C5 O4 2.0(4) . . . . ? C7 O3 C5 C4 -178.2(2) . . . . ? N2 C4 C5 O4 177.2(2) . . . . ? C3 C4 C5 O4 0.4(3) . . . . ? N2 C4 C5 O3 -2.6(3) . . . . ? C3 C4 C5 O3 -179.4(2) . . . . ? C13 O5 C8 O6 7.0(3) . . . . ? C13 O5 C8 C9 -173.64(17) . . . . ? N4 N3 C9 C10 0.04(19) . . . . ? Cu1 N3 C9 C10 158.83(12) . . . . ? N4 N3 C9 C8 -177.09(14) . . . . ? Cu1 N3 C9 C8 -18.3(2) . . . . ? O6 C8 C9 N3 171.33(17) . . . . ? O5 C8 C9 N3 -8.0(2) . . . . ? O6 C8 C9 C10 -5.2(3) . . . . ? O5 C8 C9 C10 175.47(18) . . . . ? N3 C9 C10 C11 -0.27(19) . . . . ? C8 C9 C10 C11 176.52(17) . . . . ? N3 N4 C11 C10 -0.40(19) . . . . ? Cu2 N4 C11 C10 -158.76(13) . . . . ? N3 N4 C11 C12 174.76(15) . . . . ? Cu2 N4 C11 C12 16.4(3) . . . . ? C9 C10 C11 N4 0.4(2) . . . . ? C9 C10 C11 C12 -173.87(19) . . . . ? C14 O7 C12 O8 -1.2(3) . . . . ? C14 O7 C12 C11 176.37(18) . . . . ? N4 C11 C12 O8 5.3(3) . . . . ? C10 C11 C12 O8 179.2(2) . . . . ? N4 C11 C12 O7 -172.22(16) . . . . ? C10 C11 C12 O7 1.7(3) . . . . ? C20 O11 C15 O12 2.8(3) . . . . ? C20 O11 C15 C16 -176.78(15) . . . . ? N6 N5 C16 C17 -0.01(18) . . . . ? Cu3 N5 C16 C17 -179.57(11) . . . . ? N6 N5 C16 C15 178.16(13) . . . . ? Cu3 N5 C16 C15 -1.4(2) . . . . ? O12 C15 C16 N5 -11.0(2) . . . . ? O11 C15 C16 N5 168.61(14) . . . . ? O12 C15 C16 C17 166.63(18) . . . . ? O11 C15 C16 C17 -13.8(3) . . . . ? N5 C16 C17 C18 0.46(18) . . . . ? C15 C16 C17 C18 -177.30(17) . . . . ? N5 N6 C18 C17 0.76(17) . . . . ? Cu4 N6 C18 C17 179.72(11) . . . . ? N5 N6 C18 C19 -176.20(13) . . . . ? Cu4 N6 C18 C19 2.8(2) . . . . ? C16 C17 C18 N6 -0.74(18) . . . . ? C16 C17 C18 C19 175.56(17) . . . . ? C21 O13 C19 O14 -0.4(3) . . . . ? C21 O13 C19 C18 -179.37(19) . . . . ? N6 C18 C19 O14 4.6(2) . . . . ? C17 C18 C19 O14 -171.50(18) . . . . ? N6 C18 C19 O13 -176.38(14) . . . . ? C17 C18 C19 O13 7.5(3) . . . . ? C27 O15 C22 O16 3.4(4) . . . . ? C27 O15 C22 C23 -177.0(2) . . . . ? N8 N7 C23 C24 0.75(19) . . . . ? Cu3 N7 C23 C24 170.29(13) . . . . ? N8 N7 C23 C22 -177.05(15) . . . . ? Cu3 N7 C23 C22 -7.5(3) . . . . ? O16 C22 C23 N7 -178.8(2) . . . . ? O15 C22 C23 N7 1.7(3) . . . . ? O16 C22 C23 C24 3.9(3) . . . . ? O15 C22 C23 C24 -175.64(18) . . . . ? N7 C23 C24 C25 -0.9(2) . . . . ? C22 C23 C24 C25 176.71(18) . . . . ? N7 N8 C25 C24 -0.27(19) . . . . ? Cu4 N8 C25 C24 -170.68(12) . . . . ? N7 N8 C25 C26 174.69(15) . . . . ? Cu4 N8 C25 C26 4.3(2) . . . . ? C23 C24 C25 N8 0.7(2) . . . . ? C23 C24 C25 C26 -173.80(17) . . . . ? C28 O17 C26 O18 1.3(3) . . . . ? C28 O17 C26 C25 -175.67(17) . . . . ? N8 C25 C26 O18 172.7(2) . . . . ? C24 C25 C26 O18 -13.4(3) . . . . ? N8 C25 C26 O17 -10.4(2) . . . . ? C24 C25 C26 O17 163.56(18) . . . . ? C34 O21 C29 O22 -9.9(3) . . . . ? C34 O21 C29 C30 168.99(17) . . . . ? N10 N9 C30 C31 -0.63(18) . . . . ? Cu5 N9 C30 C31 -163.87(12) . . . . ? N10 N9 C30 C29 179.59(14) . . . . ? Cu5 N9 C30 C29 16.4(2) . . . . ? O22 C29 C30 N9 179.99(17) . . . . ? O21 C29 C30 N9 1.1(2) . . . . ? O22 C29 C30 C31 0.3(3) . . . . ? O21 C29 C30 C31 -178.60(17) . . . . ? N9 C30 C31 C32 0.70(18) . . . . ? C29 C30 C31 C32 -179.54(16) . . . . ? N9 N10 C32 C31 0.16(18) . . . . ? Cu6 N10 C32 C31 168.10(12) . . . . ? N9 N10 C32 C33 -175.23(14) . . . . ? Cu6 N10 C32 C33 -7.3(2) . . . . ? C30 C31 C32 N10 -0.53(18) . . . . ? C30 C31 C32 C33 174.59(16) . . . . ? C35 O23 C33 O24 -7.8(3) . . . . ? C35 O23 C33 C32 171.35(16) . . . . ? N10 C32 C33 O24 -176.13(17) . . . . ? C31 C32 C33 O24 9.3(3) . . . . ? N10 C32 C33 O23 4.7(2) . . . . ? C31 C32 C33 O23 -169.91(16) . . . . ? C41 O25 C36 O26 2.0(3) . . . . ? C41 O25 C36 C37 -178.56(15) . . . . ? N12 N11 C37 C38 1.26(18) . . . . ? Cu5 N11 C37 C38 178.55(12) . . . . ? N12 N11 C37 C36 -176.06(14) . . . . ? Cu5 N11 C37 C36 1.2(2) . . . . ? O26 C36 C37 N11 -175.39(17) . . . . ? O25 C36 C37 N11 5.1(2) . . . . ? O26 C36 C37 C38 7.8(3) . . . . ? O25 C36 C37 C38 -171.70(16) . . . . ? N11 C37 C38 C39 -1.11(18) . . . . ? C36 C37 C38 C39 176.04(16) . . . . ? N11 N12 C39 C38 0.17(18) . . . . ? Cu6 N12 C39 C38 -170.26(12) . . . . ? N11 N12 C39 C40 179.87(14) . . . . ? Cu6 N12 C39 C40 9.4(2) . . . . ? C37 C38 C39 N12 0.57(18) . . . . ? C37 C38 C39 C40 -179.07(17) . . . . ? C42 O27 C40 O28 5.2(3) . . . . ? C42 O27 C40 C39 -173.36(15) . . . . ? N12 C39 C40 O28 -11.3(3) . . . . ? C38 C39 C40 O28 168.27(18) . . . . ? N12 C39 C40 O27 167.25(14) . . . . ? C38 C39 C40 O27 -13.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 31.58 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.010 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.078 _database_code_depnum_ccdc_archive 'CCDC 951175' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H28 Cu4 N8 O20), 8(CH3OH), OH2' _chemical_formula_sum 'C64 H90 Cu8 N16 O49' _chemical_formula_weight 2375.84 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.5074(10) _cell_length_b 15.5074(10) _cell_length_c 19.8920(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4783.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.96 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6763 _exptl_absorpt_correction_T_max 0.7568 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35860 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.77 _reflns_number_total 3106 _reflns_number_gt 2337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1157P)^2^+24.4786P] 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 3106 _refine_ls_number_parameters 157 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.05585(3) 0.87975(3) 0.30688(2) 0.0248(2) Uani 1 1 d . . . O1 O 0.1847(2) 0.9556(2) 0.34435(16) 0.0354(7) Uani 1 1 d . . . O2 O 0.2359(2) 1.0009(3) 0.44313(16) 0.0410(9) Uani 1 1 d . . . O3 O -0.1239(2) 0.8179(2) 0.54042(16) 0.0298(7) Uani 1 1 d . . . O4 O -0.0496(2) 0.8828(2) 0.62235(15) 0.0338(7) Uani 1 1 d . . . O5 O -0.0100(2) 0.9892(2) 0.30121(16) 0.0315(7) Uani 1 1 d D . . H5 H 0.012(3) 1.025(3) 0.329(2) 0.038 Uiso 1 1 d D . . O7 O 0.0000 0.2500 0.1250 0.120(10) Uiso 0.50 4 d SP . . N1 N 0.0460(2) 0.8842(2) 0.40566(18) 0.0238(7) Uani 1 1 d . . . N2 N -0.0154(2) 0.8581(2) 0.44778(16) 0.0235(7) Uani 1 1 d . . . C1 C 0.1801(3) 0.9614(3) 0.4045(2) 0.0305(9) Uani 1 1 d . . . C2 C 0.1076(3) 0.9243(3) 0.4424(2) 0.0256(8) Uani 1 1 d . . . C3 C 0.0854(3) 0.9239(3) 0.5103(2) 0.0265(8) Uani 1 1 d . . . H3 H 0.1159 0.9467 0.5464 0.032 Uiso 1 1 calc R . . C4 C 0.0068(3) 0.8816(3) 0.5109(2) 0.0252(8) Uani 1 1 d . . . C5 C -0.0585(3) 0.8595(3) 0.5629(2) 0.0275(9) Uani 1 1 d . . . C6 C 0.3032(4) 1.0481(5) 0.4083(4) 0.0614(18) Uani 1 1 d . . . H6A H 0.3370 1.0087 0.3820 0.092 Uiso 1 1 calc R . . H6B H 0.3396 1.0762 0.4406 0.092 Uiso 1 1 calc R . . H6C H 0.2776 1.0904 0.3794 0.092 Uiso 1 1 calc R . . C7 C -0.0317(4) 1.0320(4) 0.2399(3) 0.0517(14) Uani 1 1 d . . . H7A H 0.0187 1.0594 0.2219 0.078 Uiso 1 1 calc R . . H7B H -0.0752 1.0746 0.2486 0.078 Uiso 1 1 calc R . . H7C H -0.0533 0.9906 0.2082 0.078 Uiso 1 1 calc R . . O6 O 0.8374(10) 0.8111(10) 0.7093(9) 0.111(3) Uiso 0.50 1 d PD A 1 C8 C 0.8788(15) 0.7308(12) 0.7183(14) 0.103(7) Uiso 0.50 1 d PD A 1 O6A O 0.8387(10) 0.7077(10) 0.7760(8) 0.111(3) Uiso 0.50 1 d P B 2 C8A C 0.8467(11) 0.7312(10) 0.7021(8) 0.061(4) Uiso 0.50 1 d P B 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 Cu1 0.0288(3) 0.0288(3) 0.0168(3) -0.00178(18) 0.00089(18) 0.00094(19) O1 0.0333(16) 0.0454(19) 0.0275(17) -0.0039(14) 0.0069(13) -0.0030(14) O2 0.0289(16) 0.059(2) 0.0350(18) -0.0104(16) 0.0005(14) -0.0124(15) O3 0.0333(16) 0.0380(17) 0.0181(14) -0.0012(12) 0.0017(11) -0.0037(13) O4 0.0451(18) 0.0376(17) 0.0186(14) -0.0035(12) 0.0003(13) -0.0049(14) O5 0.0379(17) 0.0306(16) 0.0260(16) -0.0040(12) -0.0040(13) 0.0027(13) N1 0.0273(17) 0.0264(17) 0.0178(16) -0.0027(13) -0.0006(13) -0.0004(13) N2 0.0284(17) 0.0253(16) 0.0169(16) -0.0025(12) 0.0002(13) 0.0004(14) C1 0.027(2) 0.034(2) 0.031(2) -0.0046(18) 0.0017(17) 0.0022(17) C2 0.0249(19) 0.027(2) 0.025(2) -0.0015(15) -0.0033(15) 0.0031(15) C3 0.030(2) 0.028(2) 0.0221(19) -0.0060(16) -0.0024(16) 0.0022(16) C4 0.031(2) 0.026(2) 0.0186(18) -0.0019(15) -0.0040(16) 0.0058(16) C5 0.032(2) 0.027(2) 0.024(2) -0.0013(16) -0.0012(16) 0.0034(17) C6 0.045(3) 0.081(5) 0.058(4) -0.012(3) 0.009(3) -0.026(3) C7 0.069(4) 0.045(3) 0.041(3) 0.001(2) -0.007(3) 0.012(3) _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 O3 1.947(3) 10_566 ? Cu1 N2 1.953(4) 10_566 ? Cu1 N1 1.972(4) . ? Cu1 O5 1.983(3) . ? Cu1 O1 2.436(3) . ? O1 C1 1.202(6) . ? O2 C1 1.309(5) . ? O2 C6 1.450(7) . ? O3 C5 1.282(5) . ? O3 Cu1 1.947(3) 16_666 ? O4 C5 1.244(5) . ? O5 C7 1.428(6) . ? O5 H5 0.857(10) . ? N1 N2 1.330(5) . ? N1 C2 1.355(5) . ? N2 C4 1.351(5) . ? N2 Cu1 1.953(4) 16_666 ? C1 C2 1.471(6) . ? C2 C3 1.394(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.488(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O6 C8 1.412(10) . ? O6A C8A 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 N2 82.55(13) 10_566 10_566 ? O3 Cu1 N1 178.74(14) 10_566 . ? N2 Cu1 N1 96.40(14) 10_566 . ? O3 Cu1 O5 91.89(13) 10_566 . ? N2 Cu1 O5 171.19(14) 10_566 . ? N1 Cu1 O5 89.24(14) . . ? O3 Cu1 O1 104.36(12) 10_566 . ? N2 Cu1 O1 96.46(13) 10_566 . ? N1 Cu1 O1 75.06(12) . . ? O5 Cu1 O1 91.52(12) . . ? C1 O1 Cu1 107.0(3) . . ? C1 O2 C6 115.6(4) . . ? C5 O3 Cu1 115.6(3) . 16_666 ? C7 O5 Cu1 124.6(3) . . ? C7 O5 H5 109(4) . . ? Cu1 O5 H5 109(4) . . ? N2 N1 C2 107.7(3) . . ? N2 N1 Cu1 132.3(3) . . ? C2 N1 Cu1 119.9(3) . . ? N1 N2 C4 108.8(3) . . ? N1 N2 Cu1 138.2(3) . 16_666 ? C4 N2 Cu1 112.7(3) . 16_666 ? O1 C1 O2 125.4(4) . . ? O1 C1 C2 121.8(4) . . ? O2 C1 C2 112.8(4) . . ? N1 C2 C3 110.3(4) . . ? N1 C2 C1 116.3(4) . . ? C3 C2 C1 133.4(4) . . ? C4 C3 C2 103.2(4) . . ? C4 C3 H3 128.4 . . ? C2 C3 H3 128.4 . . ? N2 C4 C3 110.1(4) . . ? N2 C4 C5 114.3(4) . . ? C3 C4 C5 135.6(4) . . ? O4 C5 O3 124.5(4) . . ? O4 C5 C4 121.3(4) . . ? O3 C5 C4 114.3(4) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O5 C7 H7A 109.5 . . ? O5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 O3 Cu1 O1 C1 179.6(3) 10_566 . . . ? N2 Cu1 O1 C1 -96.4(3) 10_566 . . . ? N1 Cu1 O1 C1 -1.5(3) . . . . ? O5 Cu1 O1 C1 87.3(3) . . . . ? O3 Cu1 O5 C7 0.7(4) 10_566 . . . ? N2 Cu1 O5 C7 -49.9(11) 10_566 . . . ? N1 Cu1 O5 C7 -179.8(4) . . . . ? O1 Cu1 O5 C7 105.1(4) . . . . ? O3 Cu1 N1 N2 -121(6) 10_566 . . . ? N2 Cu1 N1 N2 -88.1(4) 10_566 . . . ? O5 Cu1 N1 N2 85.1(4) . . . . ? O1 Cu1 N1 N2 176.9(4) . . . . ? O3 Cu1 N1 C2 64(7) 10_566 . . . ? N2 Cu1 N1 C2 96.2(3) 10_566 . . . ? O5 Cu1 N1 C2 -90.6(3) . . . . ? O1 Cu1 N1 C2 1.2(3) . . . . ? C2 N1 N2 C4 0.2(4) . . . . ? Cu1 N1 N2 C4 -175.8(3) . . . . ? C2 N1 N2 Cu1 173.5(3) . . . 16_666 ? Cu1 N1 N2 Cu1 -2.5(6) . . . 16_666 ? Cu1 O1 C1 O2 -177.4(4) . . . . ? Cu1 O1 C1 C2 1.6(5) . . . . ? C6 O2 C1 O1 6.4(7) . . . . ? C6 O2 C1 C2 -172.7(5) . . . . ? N2 N1 C2 C3 0.0(5) . . . . ? Cu1 N1 C2 C3 176.7(3) . . . . ? N2 N1 C2 C1 -177.5(3) . . . . ? Cu1 N1 C2 C1 -0.9(5) . . . . ? O1 C1 C2 N1 -0.8(6) . . . . ? O2 C1 C2 N1 178.3(4) . . . . ? O1 C1 C2 C3 -177.6(5) . . . . ? O2 C1 C2 C3 1.5(7) . . . . ? N1 C2 C3 C4 -0.3(5) . . . . ? C1 C2 C3 C4 176.7(5) . . . . ? N1 N2 C4 C3 -0.4(5) . . . . ? Cu1 N2 C4 C3 -175.5(3) 16_666 . . . ? N1 N2 C4 C5 177.5(3) . . . . ? Cu1 N2 C4 C5 2.3(4) 16_666 . . . ? C2 C3 C4 N2 0.4(4) . . . . ? C2 C3 C4 C5 -176.8(5) . . . . ? Cu1 O3 C5 O4 170.6(3) 16_666 . . . ? Cu1 O3 C5 C4 -7.3(5) 16_666 . . . ? N2 C4 C5 O4 -174.7(4) . . . . ? C3 C4 C5 O4 2.4(8) . . . . ? N2 C4 C5 O3 3.3(5) . . . . ? C3 C4 C5 O3 -179.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.747 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.157 #===END _database_code_depnum_ccdc_archive 'CCDC 951176'