# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zuo, Jing-Lin' _publ_contact_author_email zuojl@nju.edu.cn _publ_section_title ; (Hydrogen)cyanamido Bridged Multinuclear Copper(II) Complexes: From Strong Antiferromagnetic Couplings to Weak Ferromagnetic Couplings ; loop_ _publ_author_name 'Ling-Chen Kang' 'Xin Chen' 'Xi-Sen Wang' 'Yizhi Li' 'You Song' ; Jing-Lin Zuo ; 'Xiaozeng You' # Attachment '- 1-5-r.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 787749' #TrackingRef '- 1-5-r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H49 Cu2 N10, 3(Cl O4), H2 O' _chemical_formula_sum 'C49 H51 Cl3 Cu2 N10 O13' _chemical_formula_weight 1221.45 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7121(13) _cell_length_b 18.024(2) _cell_length_c 29.397(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.857(4) _cell_angle_gamma 90.00 _cell_volume 5554.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 22.38 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512.0 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8210 _exptl_absorpt_correction_T_max 0.8672 _exptl_absorpt_process_details SADABS,2000;bruker _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29697 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10869 _reflns_number_gt 6168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10869 _refine_ls_number_parameters 719 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.2001 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.043 _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 0.84385(6) 0.67721(3) 0.855667(19) 0.0606(2) Uani 1 1 d . . . Cu2 Cu 0.71791(6) 0.69490(3) 0.676086(19) 0.0648(2) Uani 1 1 d U . . N1 N 0.8150(5) 0.5963(2) 0.80900(13) 0.0832(12) Uani 1 1 d U . . H1 H 0.8300 0.5512 0.8180 0.100 Uiso 1 1 calc R . . N2 N 0.7376(5) 0.6273(3) 0.72874(14) 0.0888(13) Uani 1 1 d U . . N3 N 0.7749(4) 0.6652(2) 0.91784(12) 0.0555(9) Uani 1 1 d . . . N4 N 0.9884(4) 0.6231(2) 0.89602(12) 0.0624(10) Uani 1 1 d . . . N5 N 0.7079(3) 0.7439(2) 0.82195(12) 0.0590(10) Uani 1 1 d . . . N6 N 0.9373(3) 0.7790(2) 0.86650(12) 0.0565(9) Uani 1 1 d U . . N7 N 0.6179(4) 0.7948(2) 0.66377(12) 0.0560(9) Uani 1 1 d U . . N8 N 0.8461(4) 0.7666(2) 0.70940(13) 0.0646(10) Uani 1 1 d . . . N9 N 0.7920(4) 0.6829(2) 0.61613(12) 0.0573(9) Uani 1 1 d . . . N10 N 0.5823(4) 0.6354(2) 0.63695(13) 0.0701(11) Uani 1 1 d . . . C1 C 0.7748(6) 0.6098(3) 0.76611(17) 0.0774(13) Uani 1 1 d U . . C2 C 0.6616(5) 0.6865(3) 0.92579(18) 0.0699(14) Uani 1 1 d . . . H2 H 0.6022 0.7068 0.9014 0.084 Uiso 1 1 calc R . . C3 C 0.6291(5) 0.6796(3) 0.9685(2) 0.0750(15) Uani 1 1 d . . . H3 H 0.5499 0.6956 0.9729 0.090 Uiso 1 1 calc R . . C4 C 0.7158(5) 0.6485(3) 1.00485(17) 0.0681(13) Uani 1 1 d . . . C5 C 0.6830(6) 0.6411(4) 1.05182(18) 0.0902(18) Uani 1 1 d . . . H5A H 0.6687 0.6894 1.0635 0.135 Uiso 1 1 calc R . . H5B H 0.7522 0.6174 1.0727 0.135 Uiso 1 1 calc R . . H5C H 0.6072 0.6117 1.0493 0.135 Uiso 1 1 calc R . . C6 C 0.8327(5) 0.6272(3) 0.99638(16) 0.0640(13) Uani 1 1 d . . . H6 H 0.8941 0.6069 1.0201 0.077 Uiso 1 1 calc R . . C7 C 0.8583(4) 0.6361(2) 0.95264(15) 0.0546(11) Uani 1 1 d . . . C8 C 0.9837(4) 0.6159(2) 0.94067(15) 0.0558(11) Uani 1 1 d . . . C9 C 1.0893(5) 0.5915(3) 0.97257(17) 0.0658(13) Uani 1 1 d . . . H9 H 1.0834 0.5853 1.0035 0.079 Uiso 1 1 calc R . . C10 C 1.2033(5) 0.5762(3) 0.95958(19) 0.0717(14) Uani 1 1 d . . . C11 C 1.3193(5) 0.5564(4) 0.9949(2) 0.0938(18) Uani 1 1 d . . . H11A H 1.3836 0.5375 0.9796 0.141 Uiso 1 1 calc R . . H11B H 1.2980 0.5192 1.0154 0.141 Uiso 1 1 calc R . . H11C H 1.3510 0.5997 1.0126 0.141 Uiso 1 1 calc R . . C12 C 1.2019(6) 0.5821(4) 0.9126(2) 0.0872(17) Uani 1 1 d . . . H12 H 1.2750 0.5702 0.9017 0.105 Uiso 1 1 calc R . . C13 C 1.0967(6) 0.6047(3) 0.88219(19) 0.0839(17) Uani 1 1 d . . . H13 H 1.0989 0.6077 0.8508 0.101 Uiso 1 1 calc R . . C14 C 0.5910(5) 0.7226(3) 0.79829(17) 0.0762(15) Uani 1 1 d . . . H14 H 0.5712 0.6723 0.7969 0.091 Uiso 1 1 calc R . . C15 C 0.5021(5) 0.7708(4) 0.77669(18) 0.0773(15) Uani 1 1 d . . . H15 H 0.4230 0.7535 0.7612 0.093 Uiso 1 1 calc R . . C16 C 0.5282(5) 0.8460(4) 0.77756(17) 0.0784(16) Uani 1 1 d . . . C17 C 0.4313(6) 0.9026(4) 0.7559(2) 0.118(3) Uani 1 1 d . . . H17A H 0.3650 0.8788 0.7338 0.178 Uiso 1 1 calc R . . H17B H 0.4718 0.9396 0.7404 0.178 Uiso 1 1 calc R . . H17C H 0.3952 0.9257 0.7797 0.178 Uiso 1 1 calc R . . C18 C 0.6482(5) 0.8680(3) 0.80124(16) 0.0637(13) Uani 1 1 d . . . H18 H 0.6701 0.9180 0.8024 0.076 Uiso 1 1 calc R . . C19 C 0.7342(4) 0.8170(3) 0.82289(15) 0.0570(12) Uani 1 1 d . . . C20 C 0.8626(4) 0.8368(3) 0.85006(15) 0.0564(11) Uani 1 1 d U . . C21 C 0.9034(6) 0.9099(3) 0.85822(19) 0.0747(14) Uani 1 1 d . . . H21 H 0.8495 0.9491 0.8470 0.090 Uiso 1 1 calc R . . C22 C 1.0256(6) 0.9232(3) 0.88328(19) 0.0778(15) Uani 1 1 d . . . C23 C 1.0739(7) 1.0013(4) 0.8933(3) 0.131(3) Uani 1 1 d . . . H23A H 1.0611 1.0161 0.9234 0.197 Uiso 1 1 calc R . . H23B H 1.0280 1.0342 0.8701 0.197 Uiso 1 1 calc R . . H23C H 1.1632 1.0032 0.8929 0.197 Uiso 1 1 calc R . . C24 C 1.0991(6) 0.8639(4) 0.89914(19) 0.0823(16) Uani 1 1 d . . . H24 H 1.1813 0.8716 0.9162 0.099 Uiso 1 1 calc R . . C25 C 1.0560(5) 0.7942(3) 0.89079(18) 0.0689(13) Uani 1 1 d . . . H25 H 1.1098 0.7549 0.9021 0.083 Uiso 1 1 calc R . . C26 C 0.4991(5) 0.8076(3) 0.63938(18) 0.0690(14) Uani 1 1 d . . . H26 H 0.4485 0.7668 0.6285 0.083 Uiso 1 1 calc R . . C27 C 0.4488(5) 0.8756(3) 0.62965(18) 0.0745(14) Uani 1 1 d . . . H27 H 0.3655 0.8803 0.6130 0.089 Uiso 1 1 calc R . . C28 C 0.5197(5) 0.9382(3) 0.64415(18) 0.0729(14) Uani 1 1 d . . . C29 C 0.4675(6) 1.0144(3) 0.6339(2) 0.101(2) Uani 1 1 d . . . H29A H 0.4569 1.0242 0.6013 0.151 Uiso 1 1 calc R . . H29B H 0.5256 1.0499 0.6511 0.151 Uiso 1 1 calc R . . H29C H 0.3865 1.0182 0.6429 0.151 Uiso 1 1 calc R . . C30 C 0.6446(5) 0.9268(3) 0.66936(17) 0.0653(13) Uani 1 1 d . . . H30 H 0.6973 0.9669 0.6798 0.078 Uiso 1 1 calc R . . C31 C 0.6878(4) 0.8549(3) 0.67837(15) 0.0576(12) Uani 1 1 d . . . C32 C 0.8170(4) 0.8382(3) 0.70619(15) 0.0547(11) Uani 1 1 d . . . C33 C 0.8991(4) 0.8919(3) 0.72695(15) 0.0615(12) Uani 1 1 d . . . H33 H 0.8754 0.9415 0.7235 0.074 Uiso 1 1 calc R . . C34 C 1.0197(5) 0.8726(3) 0.75357(16) 0.0687(14) Uani 1 1 d . . . C35 C 1.1104(5) 0.9328(4) 0.7752(2) 0.0899(18) Uani 1 1 d . . . H35A H 1.1763 0.9117 0.7987 0.135 Uiso 1 1 calc R . . H35B H 1.0647 0.9695 0.7890 0.135 Uiso 1 1 calc R . . H35C H 1.1478 0.9556 0.7517 0.135 Uiso 1 1 calc R . . C36 C 1.0475(5) 0.7991(4) 0.75663(17) 0.0738(15) Uani 1 1 d . . . H36 H 1.1262 0.7838 0.7738 0.089 Uiso 1 1 calc R . . C37 C 0.9620(5) 0.7466(3) 0.73490(18) 0.0755(15) Uani 1 1 d . . . H37 H 0.9839 0.6967 0.7377 0.091 Uiso 1 1 calc R . . C38 C 0.9059(5) 0.7059(3) 0.60876(18) 0.0689(13) Uani 1 1 d . . . H38 H 0.9643 0.7264 0.6333 0.083 Uiso 1 1 calc R . . C39 C 0.9385(5) 0.7000(3) 0.56580(19) 0.0714(14) Uani 1 1 d . . . H39 H 1.0178 0.7165 0.5617 0.086 Uiso 1 1 calc R . . C40 C 0.8536(5) 0.6698(3) 0.52916(17) 0.0635(13) Uani 1 1 d . . . C41 C 0.8855(6) 0.6614(3) 0.48170(19) 0.0885(17) Uani 1 1 d . . . H41A H 0.9303 0.7047 0.4747 0.133 Uiso 1 1 calc R . . H41B H 0.8082 0.6557 0.4588 0.133 Uiso 1 1 calc R . . H41C H 0.9383 0.6184 0.4814 0.133 Uiso 1 1 calc R . . C42 C 0.7350(5) 0.6464(3) 0.53636(15) 0.0601(12) Uani 1 1 d . . . H42 H 0.6749 0.6265 0.5121 0.072 Uiso 1 1 calc R . . C43 C 0.7087(4) 0.6533(2) 0.58021(16) 0.0561(11) Uani 1 1 d . . . C44 C 0.5879(5) 0.6271(3) 0.59192(15) 0.0592(12) Uani 1 1 d . . . C45 C 0.4873(5) 0.5973(3) 0.56012(18) 0.0749(15) Uani 1 1 d . . . H45 H 0.4932 0.5926 0.5291 0.090 Uiso 1 1 calc R . . C46 C 0.3774(6) 0.5742(3) 0.5741(2) 0.0877(17) Uani 1 1 d . . . C47 C 0.2682(7) 0.5401(5) 0.5407(3) 0.134(3) Uani 1 1 d . . . H47A H 0.2975 0.5223 0.5139 0.200 Uiso 1 1 d R . . H47B H 0.2029 0.5767 0.5312 0.200 Uiso 1 1 d R . . H47C H 0.2343 0.4995 0.5554 0.200 Uiso 1 1 d R . . C48 C 0.3754(7) 0.5820(4) 0.6207(2) 0.097(2) Uani 1 1 d . . . H48 H 0.3041 0.5664 0.6316 0.116 Uiso 1 1 calc R . . C49 C 0.4751(6) 0.6118(3) 0.65056(19) 0.0859(17) Uani 1 1 d . . . H49 H 0.4704 0.6165 0.6817 0.103 Uiso 1 1 calc R . . Cl1 Cl 0.91092(14) 0.40821(9) 0.87831(5) 0.0808(4) Uani 1 1 d . . . O1 O 0.8347(6) 0.4328(4) 0.83861(17) 0.152(2) Uani 1 1 d . . . O2 O 0.8721(6) 0.4523(4) 0.9127(2) 0.171(3) Uani 1 1 d . . . O3 O 1.0363(5) 0.4108(5) 0.8808(2) 0.193(3) Uani 1 1 d . . . O4 O 0.8790(8) 0.3394(4) 0.8885(4) 0.242(5) Uani 1 1 d . . . Cl2 Cl 0.46051(17) 0.87676(14) 0.90845(6) 0.1060(6) Uani 1 1 d . . . O5 O 0.4278(7) 0.8972(6) 0.9473(2) 0.224(4) Uani 1 1 d . . . O6 O 0.5932(5) 0.8784(4) 0.9127(2) 0.180(3) Uani 1 1 d . . . O7 O 0.3945(6) 0.9171(5) 0.8731(2) 0.207(4) Uani 1 1 d . . . O8 O 0.4137(8) 0.8080(5) 0.9008(5) 0.251(5) Uani 1 1 d . . . Cl3 Cl 0.23447(16) 0.59745(8) 0.74024(6) 0.0844(4) Uani 1 1 d . . . O9 O 0.1775(8) 0.5929(4) 0.7768(3) 0.209(4) Uani 1 1 d . . . O10 O 0.2454(7) 0.6656(3) 0.7232(3) 0.190(3) Uani 1 1 d . . . O11 O 0.3395(9) 0.5573(6) 0.7423(3) 0.253(5) Uani 1 1 d . . . O12 O 0.1604(13) 0.5615(7) 0.7073(4) 0.337(7) Uani 1 1 d . . . O13 O 0.686(2) 0.2511(8) 0.9903(8) 0.256(11) Uani 0.40 1 d P . . H13A H 0.6599 0.2128 1.0023 0.307 Uiso 0.40 1 d PR . . H13B H 0.7021 0.2393 0.9641 0.307 Uiso 0.40 1 d PR . . O14 O 0.230(2) 0.7221(14) 0.6281(10) 0.213(11) Uani 0.30 1 d P . . H14A H 0.2318 0.7079 0.6559 0.255 Uiso 0.30 1 d PR . . H14B H 0.1905 0.7633 0.6239 0.255 Uiso 0.30 1 d PR . . O15 O 0.338(2) 0.6905(13) 0.8563(8) 0.186(10) Uani 0.30 1 d P . . H15A H 0.3408 0.7368 0.8616 0.223 Uiso 0.30 1 d PR . . H15B H 0.2835 0.6822 0.8313 0.223 Uiso 0.30 1 d PR . . 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 0.0686(4) 0.0685(4) 0.0429(3) -0.0023(3) 0.0072(3) -0.0007(3) Cu2 0.0771(4) 0.0736(4) 0.0412(3) 0.0018(3) 0.0067(3) 0.0015(3) N1 0.141(4) 0.053(2) 0.048(2) 0.0034(18) 0.002(2) 0.003(2) N2 0.142(4) 0.068(3) 0.047(2) 0.0017(19) -0.002(2) 0.000(2) N3 0.058(2) 0.063(2) 0.045(2) -0.0018(18) 0.0108(18) -0.0038(19) N4 0.071(3) 0.070(3) 0.047(2) -0.0025(19) 0.0137(19) 0.007(2) N5 0.059(2) 0.072(3) 0.045(2) -0.0042(18) 0.0077(17) -0.010(2) N6 0.060(2) 0.065(2) 0.044(2) 0.0052(18) 0.0064(17) -0.0002(19) N7 0.058(2) 0.065(2) 0.043(2) -0.0069(18) 0.0054(17) 0.0042(19) N8 0.060(2) 0.082(3) 0.048(2) 0.001(2) 0.0039(18) 0.009(2) N9 0.070(3) 0.056(2) 0.045(2) -0.0014(17) 0.0102(19) 0.0044(19) N10 0.090(3) 0.077(3) 0.047(2) 0.004(2) 0.021(2) -0.010(2) C1 0.128(3) 0.052(2) 0.047(2) -0.002(2) 0.007(2) 0.000(2) C2 0.068(3) 0.078(4) 0.064(3) 0.000(3) 0.013(3) -0.007(3) C3 0.070(3) 0.086(4) 0.072(4) -0.003(3) 0.023(3) -0.011(3) C4 0.082(4) 0.074(3) 0.055(3) -0.004(2) 0.027(3) -0.014(3) C5 0.104(4) 0.118(5) 0.056(3) -0.009(3) 0.036(3) -0.010(4) C6 0.077(3) 0.067(3) 0.047(3) -0.004(2) 0.012(2) -0.012(3) C7 0.068(3) 0.052(3) 0.045(2) -0.005(2) 0.014(2) -0.012(2) C8 0.066(3) 0.056(3) 0.044(2) -0.002(2) 0.008(2) -0.003(2) C9 0.068(3) 0.073(3) 0.055(3) 0.001(2) 0.010(2) -0.004(3) C10 0.069(3) 0.068(3) 0.072(4) 0.000(3) 0.001(3) 0.003(3) C11 0.079(4) 0.100(5) 0.094(4) 0.010(4) -0.003(3) 0.016(3) C12 0.074(4) 0.109(5) 0.082(4) -0.004(3) 0.023(3) 0.019(3) C13 0.092(4) 0.104(5) 0.059(3) 0.001(3) 0.025(3) 0.026(3) C14 0.071(3) 0.095(4) 0.058(3) -0.001(3) 0.004(3) -0.023(3) C15 0.055(3) 0.116(5) 0.060(3) -0.004(3) 0.009(2) -0.011(3) C16 0.065(3) 0.126(5) 0.048(3) 0.014(3) 0.021(3) 0.018(3) C17 0.085(4) 0.189(8) 0.084(4) 0.016(5) 0.020(4) 0.049(5) C18 0.063(3) 0.081(4) 0.052(3) 0.006(2) 0.022(2) 0.008(3) C19 0.059(3) 0.070(3) 0.045(2) 0.001(2) 0.015(2) -0.002(2) C20 0.059(3) 0.067(3) 0.046(3) -0.009(2) 0.018(2) -0.008(2) C21 0.092(4) 0.062(3) 0.075(4) -0.006(3) 0.028(3) -0.004(3) C22 0.077(4) 0.084(4) 0.071(3) -0.025(3) 0.014(3) -0.025(3) C23 0.130(6) 0.095(5) 0.164(7) -0.033(5) 0.020(5) -0.037(5) C24 0.067(4) 0.111(5) 0.068(3) -0.014(3) 0.012(3) -0.019(4) C25 0.052(3) 0.084(4) 0.069(3) -0.003(3) 0.010(2) -0.004(3) C26 0.063(3) 0.076(4) 0.067(3) -0.010(3) 0.013(3) -0.004(3) C27 0.061(3) 0.091(4) 0.069(3) -0.002(3) 0.005(3) 0.007(3) C28 0.065(3) 0.088(4) 0.067(3) 0.003(3) 0.017(3) 0.017(3) C29 0.084(4) 0.095(5) 0.119(5) 0.010(4) 0.013(4) 0.031(4) C30 0.064(3) 0.071(3) 0.061(3) 0.002(2) 0.014(2) 0.007(3) C31 0.053(3) 0.079(3) 0.041(2) -0.004(2) 0.011(2) 0.008(3) C32 0.057(3) 0.066(3) 0.041(2) -0.002(2) 0.011(2) 0.008(2) C33 0.054(3) 0.078(3) 0.053(3) -0.001(2) 0.013(2) 0.008(2) C34 0.065(3) 0.096(4) 0.048(3) -0.001(3) 0.018(2) 0.004(3) C35 0.058(3) 0.123(5) 0.088(4) -0.009(4) 0.015(3) -0.020(3) C36 0.051(3) 0.111(5) 0.054(3) -0.001(3) 0.001(2) 0.013(3) C37 0.070(3) 0.089(4) 0.065(3) 0.005(3) 0.006(3) 0.018(3) C38 0.072(3) 0.066(3) 0.068(3) -0.008(3) 0.014(3) -0.002(3) C39 0.073(3) 0.072(3) 0.076(4) -0.002(3) 0.030(3) -0.005(3) C40 0.085(4) 0.056(3) 0.054(3) 0.005(2) 0.023(3) 0.007(3) C41 0.099(4) 0.106(5) 0.069(4) -0.005(3) 0.037(3) 0.000(4) C42 0.078(3) 0.060(3) 0.042(2) 0.001(2) 0.012(2) 0.004(2) C43 0.067(3) 0.051(3) 0.050(3) 0.004(2) 0.011(2) 0.008(2) C44 0.078(3) 0.054(3) 0.046(3) 0.002(2) 0.012(2) -0.003(2) C45 0.094(4) 0.077(4) 0.053(3) -0.008(3) 0.013(3) -0.015(3) C46 0.097(4) 0.090(4) 0.077(4) -0.013(3) 0.018(3) -0.027(3) C47 0.115(6) 0.181(8) 0.106(5) -0.029(5) 0.025(5) -0.063(5) C48 0.119(5) 0.098(5) 0.081(4) -0.008(3) 0.037(4) -0.039(4) C49 0.097(4) 0.108(5) 0.056(3) -0.001(3) 0.023(3) -0.028(4) Cl1 0.0806(10) 0.0925(11) 0.0649(8) 0.0127(7) 0.0048(7) 0.0080(8) O1 0.172(5) 0.182(5) 0.083(3) 0.031(3) -0.018(3) 0.019(4) O2 0.163(5) 0.240(8) 0.114(4) -0.038(5) 0.038(4) -0.001(5) O3 0.086(4) 0.328(10) 0.166(6) -0.020(6) 0.030(4) -0.023(5) O4 0.200(7) 0.127(5) 0.385(13) 0.127(7) 0.029(8) 0.030(5) Cl2 0.0831(12) 0.1565(18) 0.0734(10) -0.0020(11) 0.0045(8) 0.0237(11) O5 0.158(6) 0.418(14) 0.104(4) -0.064(6) 0.046(4) -0.009(7) O6 0.095(4) 0.266(8) 0.174(6) 0.022(6) 0.016(4) 0.028(4) O7 0.141(5) 0.319(11) 0.143(5) 0.095(6) -0.011(4) 0.029(6) O8 0.145(6) 0.156(7) 0.434(16) -0.040(9) 0.020(8) 0.011(5) Cl3 0.1011(11) 0.0557(9) 0.1037(12) -0.0047(7) 0.0380(9) -0.0026(8) O9 0.312(9) 0.185(6) 0.187(6) 0.036(5) 0.183(7) 0.085(6) O10 0.228(7) 0.103(4) 0.259(8) 0.050(5) 0.093(7) -0.011(4) O11 0.253(9) 0.288(10) 0.263(10) 0.152(8) 0.158(8) 0.165(8) O12 0.387(16) 0.343(15) 0.273(13) -0.095(12) 0.048(12) -0.200(14) O13 0.30(2) 0.119(14) 0.30(3) 0.024(16) -0.04(2) -0.061(15) O14 0.19(2) 0.19(2) 0.25(3) 0.03(2) 0.04(2) 0.003(19) O15 0.21(2) 0.19(2) 0.17(2) 0.021(16) 0.042(18) -0.064(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.983(4) . ? Cu1 N5 1.989(4) . ? Cu1 N4 2.000(4) . ? Cu1 N6 2.083(4) . ? Cu1 N3 2.118(4) . ? Cu2 N2 1.947(4) . ? Cu2 N10 1.974(4) . ? Cu2 N8 1.990(4) . ? Cu2 N9 2.088(4) . ? Cu2 N7 2.088(4) . ? N1 C1 1.269(6) . ? N1 H1 0.8600 . ? N2 C1 1.134(6) . ? N3 C7 1.321(5) . ? N3 C2 1.338(6) . ? N4 C8 1.330(5) . ? N4 C13 1.347(6) . ? N5 C19 1.345(6) . ? N5 C14 1.358(6) . ? N6 C20 1.342(6) . ? N6 C25 1.352(6) . ? N7 C31 1.337(6) . ? N7 C26 1.346(6) . ? N8 C32 1.327(6) . ? N8 C37 1.360(6) . ? N9 C43 1.345(6) . ? N9 C38 1.347(6) . ? N10 C44 1.346(6) . ? N10 C49 1.360(7) . ? C2 C3 1.376(7) . ? C2 H2 0.9300 . ? C3 C4 1.382(7) . ? C3 H3 0.9300 . ? C4 C6 1.381(7) . ? C4 C5 1.499(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 C8 1.501(6) . ? C8 C9 1.385(6) . ? C9 C10 1.380(7) . ? C9 H9 0.9300 . ? C10 C12 1.383(7) . ? C10 C11 1.490(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.349(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.348(8) . ? C14 H14 0.9300 . ? C15 C16 1.383(8) . ? C15 H15 0.9300 . ? C16 C18 1.388(7) . ? C16 C17 1.500(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.364(6) . ? C18 H18 0.9300 . ? C19 C20 1.485(6) . ? C20 C21 1.394(7) . ? C21 C22 1.384(7) . ? C21 H21 0.9300 . ? C22 C24 1.352(8) . ? C22 C23 1.508(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.344(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.345(7) . ? C26 H26 0.9300 . ? C27 C28 1.378(7) . ? C27 H27 0.9300 . ? C28 C30 1.405(7) . ? C28 C29 1.491(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.383(7) . ? C30 H30 0.9300 . ? C31 C32 1.486(6) . ? C32 C33 1.364(6) . ? C33 C34 1.409(7) . ? C33 H33 0.9300 . ? C34 C36 1.356(7) . ? C34 C35 1.508(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.380(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.382(7) . ? C38 H38 0.9300 . ? C39 C40 1.372(7) . ? C39 H39 0.9300 . ? C40 C42 1.395(7) . ? C40 C41 1.511(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.381(6) . ? C42 H42 0.9300 . ? C43 C44 1.483(6) . ? C44 C45 1.382(7) . ? C45 C46 1.388(7) . ? C45 H45 0.9300 . ? C46 C48 1.380(8) . ? C46 C47 1.496(8) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.348(8) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? Cl1 O3 1.331(5) . ? Cl1 O4 1.337(7) . ? Cl1 O1 1.354(5) . ? Cl1 O2 1.414(6) . ? Cl2 O5 1.315(6) . ? Cl2 O8 1.339(8) . ? Cl2 O7 1.344(6) . ? Cl2 O6 1.402(6) . ? Cl3 O12 1.292(10) . ? Cl3 O11 1.329(7) . ? Cl3 O10 1.340(6) . ? Cl3 O9 1.344(5) . ? O13 H13A 0.8500 . ? O13 H13B 0.8498 . ? O14 H14A 0.8498 . ? O14 H14B 0.8500 . ? O15 H15A 0.8500 . ? O15 H15B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N5 96.08(17) . . ? N1 Cu1 N4 92.50(17) . . ? N5 Cu1 N4 171.33(16) . . ? N1 Cu1 N6 139.05(17) . . ? N5 Cu1 N6 79.83(15) . . ? N4 Cu1 N6 92.82(16) . . ? N1 Cu1 N3 119.32(17) . . ? N5 Cu1 N3 98.18(15) . . ? N4 Cu1 N3 78.66(15) . . ? N6 Cu1 N3 101.53(14) . . ? N2 Cu2 N10 94.03(18) . . ? N2 Cu2 N8 93.66(18) . . ? N10 Cu2 N8 171.92(17) . . ? N2 Cu2 N9 127.49(18) . . ? N10 Cu2 N9 79.25(16) . . ? N8 Cu2 N9 97.99(16) . . ? N2 Cu2 N7 130.17(18) . . ? N10 Cu2 N7 94.43(17) . . ? N8 Cu2 N7 78.66(16) . . ? N9 Cu2 N7 102.33(14) . . ? C1 N1 Cu1 121.3(4) . . ? C1 N1 H1 119.3 . . ? Cu1 N1 H1 119.3 . . ? C1 N2 Cu2 154.7(5) . . ? C7 N3 C2 118.2(4) . . ? C7 N3 Cu1 114.1(3) . . ? C2 N3 Cu1 127.7(3) . . ? C8 N4 C13 118.9(4) . . ? C8 N4 Cu1 116.8(3) . . ? C13 N4 Cu1 123.4(3) . . ? C19 N5 C14 117.1(4) . . ? C19 N5 Cu1 116.9(3) . . ? C14 N5 Cu1 126.0(4) . . ? C20 N6 C25 117.4(4) . . ? C20 N6 Cu1 113.3(3) . . ? C25 N6 Cu1 129.0(3) . . ? C31 N7 C26 115.9(4) . . ? C31 N7 Cu2 114.2(3) . . ? C26 N7 Cu2 129.5(3) . . ? C32 N8 C37 118.1(4) . . ? C32 N8 Cu2 117.9(3) . . ? C37 N8 Cu2 124.0(4) . . ? C43 N9 C38 118.2(4) . . ? C43 N9 Cu2 113.4(3) . . ? C38 N9 Cu2 128.2(3) . . ? C44 N10 C49 117.7(4) . . ? C44 N10 Cu2 117.3(3) . . ? C49 N10 Cu2 124.3(3) . . ? N2 C1 N1 174.7(6) . . ? N3 C2 C3 122.8(5) . . ? N3 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C6 C4 C3 117.6(4) . . ? C6 C4 C5 122.3(5) . . ? C3 C4 C5 120.0(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 119.8(5) . . ? C7 C6 H6 120.1 . . ? C4 C6 H6 120.1 . . ? N3 C7 C6 122.4(4) . . ? N3 C7 C8 114.2(4) . . ? C6 C7 C8 123.3(4) . . ? N4 C8 C9 120.5(4) . . ? N4 C8 C7 115.1(4) . . ? C9 C8 C7 124.4(4) . . ? C10 C9 C8 121.5(5) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C12 115.6(5) . . ? C9 C10 C11 120.9(5) . . ? C12 C10 C11 123.5(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C10 121.4(5) . . ? C13 C12 H12 119.3 . . ? C10 C12 H12 119.3 . . ? N4 C13 C12 121.9(5) . . ? N4 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C15 C14 N5 123.1(5) . . ? C15 C14 H14 118.5 . . ? N5 C14 H14 118.5 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C18 116.9(5) . . ? C15 C16 C17 122.6(6) . . ? C18 C16 C17 120.4(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C16 120.5(5) . . ? C19 C18 H18 119.7 . . ? C16 C18 H18 119.7 . . ? N5 C19 C18 122.2(5) . . ? N5 C19 C20 114.4(4) . . ? C18 C19 C20 123.4(5) . . ? N6 C20 C21 121.9(5) . . ? N6 C20 C19 115.1(4) . . ? C21 C20 C19 122.9(5) . . ? C22 C21 C20 119.0(5) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C24 C22 C21 117.8(5) . . ? C24 C22 C23 121.2(6) . . ? C21 C22 C23 121.0(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C22 121.5(5) . . ? C25 C24 H24 119.3 . . ? C22 C24 H24 119.3 . . ? C24 C25 N6 122.4(5) . . ? C24 C25 H25 118.8 . . ? N6 C25 H25 118.8 . . ? C27 C26 N7 124.3(5) . . ? C27 C26 H26 117.9 . . ? N7 C26 H26 117.9 . . ? C26 C27 C28 120.6(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C30 116.6(5) . . ? C27 C28 C29 122.2(5) . . ? C30 C28 C29 121.2(6) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C28 118.9(5) . . ? C31 C30 H30 120.6 . . ? C28 C30 H30 120.6 . . ? N7 C31 C30 123.7(4) . . ? N7 C31 C32 114.2(4) . . ? C30 C31 C32 122.1(5) . . ? N8 C32 C33 122.5(4) . . ? N8 C32 C31 114.5(4) . . ? C33 C32 C31 123.0(4) . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C36 C34 C33 116.2(5) . . ? C36 C34 C35 124.1(5) . . ? C33 C34 C35 119.6(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 C37 121.5(5) . . ? C34 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? N8 C37 C36 121.2(5) . . ? N8 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? N9 C38 C39 122.1(5) . . ? N9 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C40 C39 C38 119.8(5) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C42 118.6(4) . . ? C39 C40 C41 121.7(5) . . ? C42 C40 C41 119.7(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C40 118.8(5) . . ? C43 C42 H42 120.6 . . ? C40 C42 H42 120.6 . . ? N9 C43 C42 122.6(4) . . ? N9 C43 C44 114.5(4) . . ? C42 C43 C44 122.9(4) . . ? N10 C44 C45 121.5(5) . . ? N10 C44 C43 114.2(4) . . ? C45 C44 C43 124.3(4) . . ? C44 C45 C46 120.5(5) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C48 C46 C45 116.8(5) . . ? C48 C46 C47 121.6(6) . . ? C45 C46 C47 121.6(5) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C46 121.0(6) . . ? C49 C48 H48 119.5 . . ? C46 C48 H48 119.5 . . ? C48 C49 N10 122.5(5) . . ? C48 C49 H49 118.8 . . ? N10 C49 H49 118.8 . . ? O3 Cl1 O4 108.7(5) . . ? O3 Cl1 O1 117.4(4) . . ? O4 Cl1 O1 111.2(5) . . ? O3 Cl1 O2 112.5(4) . . ? O4 Cl1 O2 103.6(6) . . ? O1 Cl1 O2 102.6(4) . . ? O5 Cl2 O8 104.4(7) . . ? O5 Cl2 O7 109.2(6) . . ? O8 Cl2 O7 104.6(6) . . ? O5 Cl2 O6 111.3(4) . . ? O8 Cl2 O6 111.8(5) . . ? O7 Cl2 O6 114.9(5) . . ? O12 Cl3 O11 98.4(8) . . ? O12 Cl3 O10 105.5(7) . . ? O11 Cl3 O10 112.2(5) . . ? O12 Cl3 O9 105.0(7) . . ? O11 Cl3 O9 116.7(5) . . ? O10 Cl3 O9 116.3(4) . . ? H13A O13 H13B 108.6 . . ? H14A O14 H14B 108.5 . . ? H15A O15 H15B 109.0 . . ? 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 N5 Cu1 N1 C1 30.8(5) . . . . ? N4 Cu1 N1 C1 -147.9(5) . . . . ? N6 Cu1 N1 C1 -50.7(6) . . . . ? N3 Cu1 N1 C1 133.7(5) . . . . ? N10 Cu2 N2 C1 -169.8(12) . . . . ? N8 Cu2 N2 C1 7.7(12) . . . . ? N9 Cu2 N2 C1 110.7(12) . . . . ? N7 Cu2 N2 C1 -70.5(13) . . . . ? N1 Cu1 N3 C7 92.0(3) . . . . ? N5 Cu1 N3 C7 -166.2(3) . . . . ? N4 Cu1 N3 C7 5.6(3) . . . . ? N6 Cu1 N3 C7 -85.0(3) . . . . ? N1 Cu1 N3 C2 -91.2(4) . . . . ? N5 Cu1 N3 C2 10.6(4) . . . . ? N4 Cu1 N3 C2 -177.6(4) . . . . ? N6 Cu1 N3 C2 91.8(4) . . . . ? N1 Cu1 N4 C8 -128.8(4) . . . . ? N5 Cu1 N4 C8 59.9(12) . . . . ? N6 Cu1 N4 C8 91.8(4) . . . . ? N3 Cu1 N4 C8 -9.4(3) . . . . ? N1 Cu1 N4 C13 61.9(5) . . . . ? N5 Cu1 N4 C13 -109.3(10) . . . . ? N6 Cu1 N4 C13 -77.5(4) . . . . ? N3 Cu1 N4 C13 -178.7(5) . . . . ? N1 Cu1 N5 C19 -140.9(3) . . . . ? N4 Cu1 N5 C19 30.3(12) . . . . ? N6 Cu1 N5 C19 -2.1(3) . . . . ? N3 Cu1 N5 C19 98.2(3) . . . . ? N1 Cu1 N5 C14 39.4(4) . . . . ? N4 Cu1 N5 C14 -149.4(9) . . . . ? N6 Cu1 N5 C14 178.2(4) . . . . ? N3 Cu1 N5 C14 -81.4(4) . . . . ? N1 Cu1 N6 C20 92.5(4) . . . . ? N5 Cu1 N6 C20 4.9(3) . . . . ? N4 Cu1 N6 C20 -170.4(3) . . . . ? N3 Cu1 N6 C20 -91.4(3) . . . . ? N1 Cu1 N6 C25 -93.9(4) . . . . ? N5 Cu1 N6 C25 178.5(4) . . . . ? N4 Cu1 N6 C25 3.1(4) . . . . ? N3 Cu1 N6 C25 82.1(4) . . . . ? N2 Cu2 N7 C31 92.1(4) . . . . ? N10 Cu2 N7 C31 -168.8(3) . . . . ? N8 Cu2 N7 C31 6.9(3) . . . . ? N9 Cu2 N7 C31 -88.9(3) . . . . ? N2 Cu2 N7 C26 -95.6(4) . . . . ? N10 Cu2 N7 C26 3.5(4) . . . . ? N8 Cu2 N7 C26 179.3(4) . . . . ? N9 Cu2 N7 C26 83.4(4) . . . . ? N2 Cu2 N8 C32 -134.8(3) . . . . ? N10 Cu2 N8 C32 27.1(13) . . . . ? N9 Cu2 N8 C32 96.6(3) . . . . ? N7 Cu2 N8 C32 -4.5(3) . . . . ? N2 Cu2 N8 C37 45.8(4) . . . . ? N10 Cu2 N8 C37 -152.3(11) . . . . ? N9 Cu2 N8 C37 -82.9(4) . . . . ? N7 Cu2 N8 C37 176.1(4) . . . . ? N2 Cu2 N9 C43 96.3(4) . . . . ? N10 Cu2 N9 C43 9.5(3) . . . . ? N8 Cu2 N9 C43 -162.8(3) . . . . ? N7 Cu2 N9 C43 -82.8(3) . . . . ? N2 Cu2 N9 C38 -89.1(4) . . . . ? N10 Cu2 N9 C38 -175.9(4) . . . . ? N8 Cu2 N9 C38 11.8(4) . . . . ? N7 Cu2 N9 C38 91.8(4) . . . . ? N2 Cu2 N10 C44 -138.2(4) . . . . ? N8 Cu2 N10 C44 60.0(13) . . . . ? N9 Cu2 N10 C44 -10.7(4) . . . . ? N7 Cu2 N10 C44 91.0(4) . . . . ? N2 Cu2 N10 C49 51.9(5) . . . . ? N8 Cu2 N10 C49 -110.0(11) . . . . ? N9 Cu2 N10 C49 179.3(5) . . . . ? N7 Cu2 N10 C49 -79.0(5) . . . . ? Cu2 N2 C1 N1 37(8) . . . . ? Cu1 N1 C1 N2 -7(8) . . . . ? C7 N3 C2 C3 0.3(7) . . . . ? Cu1 N3 C2 C3 -176.4(4) . . . . ? N3 C2 C3 C4 -0.9(8) . . . . ? C2 C3 C4 C6 1.3(8) . . . . ? C2 C3 C4 C5 179.4(5) . . . . ? C3 C4 C6 C7 -1.2(7) . . . . ? C5 C4 C6 C7 -179.2(5) . . . . ? C2 N3 C7 C6 -0.1(7) . . . . ? Cu1 N3 C7 C6 177.0(3) . . . . ? C2 N3 C7 C8 -178.5(4) . . . . ? Cu1 N3 C7 C8 -1.4(5) . . . . ? C4 C6 C7 N3 0.6(7) . . . . ? C4 C6 C7 C8 178.8(4) . . . . ? C13 N4 C8 C9 1.5(7) . . . . ? Cu1 N4 C8 C9 -168.3(4) . . . . ? C13 N4 C8 C7 -178.7(4) . . . . ? Cu1 N4 C8 C7 11.5(5) . . . . ? N3 C7 C8 N4 -6.4(6) . . . . ? C6 C7 C8 N4 175.3(4) . . . . ? N3 C7 C8 C9 173.4(4) . . . . ? C6 C7 C8 C9 -4.9(7) . . . . ? N4 C8 C9 C10 2.0(7) . . . . ? C7 C8 C9 C10 -177.8(4) . . . . ? C8 C9 C10 C12 -4.1(8) . . . . ? C8 C9 C10 C11 174.6(5) . . . . ? C9 C10 C12 C13 2.9(9) . . . . ? C11 C10 C12 C13 -175.8(6) . . . . ? C8 N4 C13 C12 -2.8(9) . . . . ? Cu1 N4 C13 C12 166.3(5) . . . . ? C10 C12 C13 N4 0.5(10) . . . . ? C19 N5 C14 C15 -0.7(7) . . . . ? Cu1 N5 C14 C15 179.0(4) . . . . ? N5 C14 C15 C16 0.6(8) . . . . ? C14 C15 C16 C18 0.2(7) . . . . ? C14 C15 C16 C17 -177.3(5) . . . . ? C15 C16 C18 C19 -0.8(7) . . . . ? C17 C16 C18 C19 176.8(4) . . . . ? C14 N5 C19 C18 0.0(6) . . . . ? Cu1 N5 C19 C18 -179.6(3) . . . . ? C14 N5 C19 C20 178.9(4) . . . . ? Cu1 N5 C19 C20 -0.8(5) . . . . ? C16 C18 C19 N5 0.7(7) . . . . ? C16 C18 C19 C20 -178.0(4) . . . . ? C25 N6 C20 C21 -1.2(6) . . . . ? Cu1 N6 C20 C21 173.1(4) . . . . ? C25 N6 C20 C19 178.9(4) . . . . ? Cu1 N6 C20 C19 -6.7(5) . . . . ? N5 C19 C20 N6 5.1(5) . . . . ? C18 C19 C20 N6 -176.0(4) . . . . ? N5 C19 C20 C21 -174.7(4) . . . . ? C18 C19 C20 C21 4.1(7) . . . . ? N6 C20 C21 C22 1.2(7) . . . . ? C19 C20 C21 C22 -178.9(4) . . . . ? C20 C21 C22 C24 -0.7(8) . . . . ? C20 C21 C22 C23 -179.5(5) . . . . ? C21 C22 C24 C25 0.4(8) . . . . ? C23 C22 C24 C25 179.2(6) . . . . ? C22 C24 C25 N6 -0.4(8) . . . . ? C20 N6 C25 C24 0.9(7) . . . . ? Cu1 N6 C25 C24 -172.5(4) . . . . ? C31 N7 C26 C27 -0.6(7) . . . . ? Cu2 N7 C26 C27 -172.8(4) . . . . ? N7 C26 C27 C28 1.0(8) . . . . ? C26 C27 C28 C30 -0.4(8) . . . . ? C26 C27 C28 C29 179.8(5) . . . . ? C27 C28 C30 C31 -0.6(7) . . . . ? C29 C28 C30 C31 179.2(5) . . . . ? C26 N7 C31 C30 -0.5(6) . . . . ? Cu2 N7 C31 C30 172.9(3) . . . . ? C26 N7 C31 C32 178.5(4) . . . . ? Cu2 N7 C31 C32 -8.1(5) . . . . ? C28 C30 C31 N7 1.1(7) . . . . ? C28 C30 C31 C32 -177.8(4) . . . . ? C37 N8 C32 C33 0.8(6) . . . . ? Cu2 N8 C32 C33 -178.7(3) . . . . ? C37 N8 C32 C31 -179.0(4) . . . . ? Cu2 N8 C32 C31 1.5(5) . . . . ? N7 C31 C32 N8 4.5(5) . . . . ? C30 C31 C32 N8 -176.4(4) . . . . ? N7 C31 C32 C33 -175.2(4) . . . . ? C30 C31 C32 C33 3.8(7) . . . . ? N8 C32 C33 C34 -0.8(7) . . . . ? C31 C32 C33 C34 178.9(4) . . . . ? C32 C33 C34 C36 0.5(7) . . . . ? C32 C33 C34 C35 178.4(4) . . . . ? C33 C34 C36 C37 -0.2(7) . . . . ? C35 C34 C36 C37 -178.0(5) . . . . ? C32 N8 C37 C36 -0.4(7) . . . . ? Cu2 N8 C37 C36 179.0(4) . . . . ? C34 C36 C37 N8 0.2(8) . . . . ? C43 N9 C38 C39 0.1(7) . . . . ? Cu2 N9 C38 C39 -174.2(4) . . . . ? N9 C38 C39 C40 -0.2(8) . . . . ? C38 C39 C40 C42 0.7(7) . . . . ? C38 C39 C40 C41 -179.3(5) . . . . ? C39 C40 C42 C43 -1.2(7) . . . . ? C41 C40 C42 C43 178.8(5) . . . . ? C38 N9 C43 C42 -0.7(7) . . . . ? Cu2 N9 C43 C42 174.5(3) . . . . ? C38 N9 C43 C44 177.9(4) . . . . ? Cu2 N9 C43 C44 -6.9(5) . . . . ? C40 C42 C43 N9 1.2(7) . . . . ? C40 C42 C43 C44 -177.2(4) . . . . ? C49 N10 C44 C45 1.5(7) . . . . ? Cu2 N10 C44 C45 -169.1(4) . . . . ? C49 N10 C44 C43 -179.2(4) . . . . ? Cu2 N10 C44 C43 10.2(5) . . . . ? N9 C43 C44 N10 -1.6(6) . . . . ? C42 C43 C44 N10 176.9(4) . . . . ? N9 C43 C44 C45 177.6(5) . . . . ? C42 C43 C44 C45 -3.8(7) . . . . ? N10 C44 C45 C46 -0.7(8) . . . . ? C43 C44 C45 C46 -179.9(5) . . . . ? C44 C45 C46 C48 -0.6(9) . . . . ? C44 C45 C46 C47 -178.6(6) . . . . ? C45 C46 C48 C49 1.1(10) . . . . ? C47 C46 C48 C49 179.1(7) . . . . ? C46 C48 C49 N10 -0.3(11) . . . . ? C44 N10 C49 C48 -1.0(9) . . . . ? Cu2 N10 C49 C48 168.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.752 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.073 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 787750' #TrackingRef 'cif-all-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H33 Cu2 N10, 3(Cl O4)' _chemical_formula_sum 'C49 H33 Cl3 Cu2 N10 O12' _chemical_formula_weight 1187.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.399(3) _cell_length_b 17.754(3) _cell_length_c 12.3468(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5129.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.8660 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24297 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.1906 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8865 _reflns_number_gt 3862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 8865 _refine_ls_number_parameters 686 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _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 0.64166(5) 0.80850(7) 0.50535(9) 0.0666(4) Uani 1 1 d . . . Cu2 Cu 0.64683(5) 0.53424(7) 0.70366(8) 0.0662(4) Uani 1 1 d . . . C1 C 0.6868(4) 0.6745(7) 0.6006(11) 0.078(2) Uani 1 1 d U . . C2 C 0.6487(6) 0.8142(8) 0.7407(13) 0.115(5) Uani 1 1 d . . . H2 H 0.6881 0.8138 0.7310 0.138 Uiso 1 1 calc R . . C3 C 0.6232(7) 0.8163(8) 0.8452(12) 0.123(5) Uani 1 1 d . . . H3 H 0.6463 0.8151 0.9065 0.148 Uiso 1 1 calc R . . C4 C 0.5676(8) 0.8199(8) 0.8557(13) 0.129(5) Uani 1 1 d . . . H4 H 0.5525 0.8225 0.9252 0.155 Uiso 1 1 calc R . . C5 C 0.5297(7) 0.8201(8) 0.7685(13) 0.111(5) Uani 1 1 d . . . C6 C 0.5573(6) 0.8145(7) 0.6703(10) 0.093(4) Uani 1 1 d . . . C7 C 0.5223(5) 0.8145(7) 0.5678(10) 0.086(4) Uani 1 1 d . . . C8 C 0.4689(7) 0.8213(8) 0.7714(13) 0.123(5) Uani 1 1 d . . . H8 H 0.4502 0.8212 0.8378 0.147 Uiso 1 1 calc R . . C9 C 0.4385(6) 0.8226(8) 0.6806(14) 0.122(5) Uani 1 1 d . . . H9 H 0.3990 0.8257 0.6861 0.147 Uiso 1 1 calc R . . C10 C 0.4631(6) 0.8194(8) 0.5760(13) 0.106(4) Uani 1 1 d . . . C11 C 0.4341(6) 0.8177(7) 0.4757(13) 0.116(5) Uani 1 1 d . . . H11 H 0.3944 0.8204 0.4743 0.139 Uiso 1 1 calc R . . C12 C 0.4630(6) 0.8123(7) 0.3832(12) 0.112(4) Uani 1 1 d . . . H12 H 0.4433 0.8127 0.3178 0.135 Uiso 1 1 calc R . . C13 C 0.5222(5) 0.8060(6) 0.3832(11) 0.096(4) Uani 1 1 d . . . H13 H 0.5419 0.8014 0.3181 0.115 Uiso 1 1 calc R . . C14 C 0.6396(5) 0.9768(8) 0.5630(9) 0.089(4) Uani 1 1 d . . . H14 H 0.6294 0.9614 0.6323 0.107 Uiso 1 1 calc R . . C15 C 0.6419(6) 1.0515(9) 0.5463(12) 0.105(5) Uani 1 1 d . . . H15 H 0.6366 1.0850 0.6033 0.126 Uiso 1 1 calc R . . C16 C 0.6515(6) 1.0758(8) 0.4502(14) 0.106(5) Uani 1 1 d . . . H16 H 0.6480 1.1270 0.4359 0.127 Uiso 1 1 calc R . . C17 C 0.6688(5) 1.0215(8) 0.3576(11) 0.088(4) Uani 1 1 d . . . C18 C 0.6643(4) 0.9448(7) 0.3903(8) 0.063(3) Uani 1 1 d . . . C19 C 0.6734(4) 0.8872(7) 0.3177(8) 0.063(3) Uani 1 1 d . . . C20 C 0.6829(6) 1.0366(8) 0.2552(12) 0.098(5) Uani 1 1 d . . . H20 H 0.6848 1.0865 0.2326 0.118 Uiso 1 1 calc R . . C21 C 0.6938(5) 0.9839(9) 0.1869(10) 0.088(4) Uani 1 1 d . . . H21 H 0.7053 0.9974 0.1174 0.106 Uiso 1 1 calc R . . C22 C 0.6892(4) 0.9051(8) 0.2124(9) 0.074(3) Uani 1 1 d . . . C23 C 0.6979(5) 0.8478(9) 0.1407(10) 0.097(4) Uani 1 1 d . . . H23 H 0.7080 0.8585 0.0695 0.116 Uiso 1 1 calc R . . C24 C 0.6920(5) 0.7764(9) 0.1728(10) 0.102(4) Uani 1 1 d . . . H24 H 0.6989 0.7373 0.1245 0.122 Uiso 1 1 calc R . . C25 C 0.6750(5) 0.7602(8) 0.2817(11) 0.092(4) Uani 1 1 d . . . H25 H 0.6702 0.7105 0.3035 0.111 Uiso 1 1 calc R . . C26 C 0.5303(5) 0.5922(6) 0.8069(9) 0.086(3) Uani 1 1 d . . . H26 H 0.5465 0.5869 0.8753 0.104 Uiso 1 1 calc R . . C27 C 0.4745(5) 0.6217(7) 0.8006(11) 0.094(4) Uani 1 1 d . . . H27 H 0.4551 0.6364 0.8628 0.113 Uiso 1 1 calc R . . C28 C 0.4501(4) 0.6283(6) 0.7023(12) 0.095(3) Uani 1 1 d . . . H28 H 0.4130 0.6469 0.6978 0.115 Uiso 1 1 calc R . . C29 C 0.4784(5) 0.6080(6) 0.6059(10) 0.077(3) Uani 1 1 d . . . C30 C 0.5339(5) 0.5819(6) 0.6225(8) 0.073(3) Uani 1 1 d . . . C31 C 0.5678(5) 0.5589(6) 0.5318(7) 0.064(3) Uani 1 1 d . . . C32 C 0.4577(4) 0.6138(6) 0.5001(10) 0.089(3) Uani 1 1 d . . . H32 H 0.4199 0.6281 0.4890 0.107 Uiso 1 1 calc R . . C33 C 0.4899(5) 0.5998(6) 0.4171(9) 0.080(3) Uani 1 1 d . . . H33 H 0.4754 0.6094 0.3483 0.096 Uiso 1 1 calc R . . C34 C 0.5462(5) 0.5705(6) 0.4260(8) 0.075(3) Uani 1 1 d . . . C35 C 0.5799(5) 0.5500(6) 0.3409(8) 0.087(4) Uani 1 1 d . . . H35 H 0.5662 0.5534 0.2703 0.104 Uiso 1 1 calc R . . C36 C 0.6327(5) 0.5252(7) 0.3599(8) 0.093(4) Uani 1 1 d . . . H36 H 0.6576 0.5152 0.3031 0.112 Uiso 1 1 calc R . . C37 C 0.6492(5) 0.5149(7) 0.4640(9) 0.090(4) Uani 1 1 d . . . H37 H 0.6840 0.4907 0.4755 0.107 Uiso 1 1 calc R . . C38 C 0.6824(5) 0.5794(7) 0.9266(10) 0.090(4) Uani 1 1 d . . . H38 H 0.6789 0.6292 0.9042 0.107 Uiso 1 1 calc R . . C39 C 0.7002(5) 0.5629(8) 1.0383(9) 0.097(4) Uani 1 1 d . . . H39 H 0.7060 0.6015 1.0879 0.117 Uiso 1 1 calc R . . C40 C 0.7077(5) 0.4911(8) 1.0666(8) 0.085(4) Uani 1 1 d . . . H40 H 0.7189 0.4802 1.1372 0.102 Uiso 1 1 calc R . . C41 C 0.6994(4) 0.4319(7) 0.9945(8) 0.062(3) Uani 1 1 d . . . C42 C 0.6801(4) 0.4503(6) 0.8895(7) 0.055(3) Uani 1 1 d . . . C43 C 0.6690(4) 0.3944(7) 0.8130(8) 0.051(3) Uani 1 1 d . . . C44 C 0.7069(4) 0.3561(7) 1.0205(9) 0.070(3) Uani 1 1 d . . . H44 H 0.7187 0.3425 1.0897 0.084 Uiso 1 1 calc R . . C45 C 0.6968(5) 0.3012(7) 0.9433(10) 0.079(4) Uani 1 1 d . . . H45 H 0.7042 0.2511 0.9603 0.094 Uiso 1 1 calc R . . C46 C 0.6748(4) 0.3198(7) 0.8357(10) 0.066(3) Uani 1 1 d . . . C47 C 0.6649(5) 0.2657(8) 0.7564(12) 0.085(4) Uani 1 1 d . . . H47 H 0.6717 0.2147 0.7680 0.102 Uiso 1 1 calc R . . C48 C 0.6449(5) 0.2922(8) 0.6624(12) 0.090(4) Uani 1 1 d . . . H48 H 0.6356 0.2577 0.6085 0.108 Uiso 1 1 calc R . . C49 C 0.6373(4) 0.3678(7) 0.6408(9) 0.072(3) Uani 1 1 d . . . H49 H 0.6238 0.3825 0.5732 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.52895(19) 0.6757(4) 0.0996(3) 0.1231(13) Uani 1 1 d . . . Cl2 Cl 0.69905(13) 0.28235(19) 0.3498(2) 0.0701(8) Uani 1 1 d . . . Cl3 Cl 0.69652(17) 0.0590(2) 0.8512(3) 0.1020(11) Uani 1 1 d . . . N1 N 0.6813(3) 0.7145(5) 0.5280(7) 0.078(2) Uani 1 1 d U . . N2 N 0.6910(3) 0.6287(5) 0.6789(7) 0.083(2) Uani 1 1 d U . . H2A H 0.7160 0.6397 0.7274 0.099 Uiso 1 1 calc R . . N3 N 0.6140(5) 0.8130(6) 0.6616(8) 0.090(3) Uani 1 1 d . . . N4 N 0.5510(4) 0.8064(5) 0.4779(8) 0.079(3) Uani 1 1 d . . . N5 N 0.6502(3) 0.9230(5) 0.4922(7) 0.069(2) Uani 1 1 d . . . N6 N 0.6660(4) 0.8166(6) 0.3526(7) 0.064(2) Uani 1 1 d . . . N7 N 0.5606(3) 0.5720(4) 0.7243(7) 0.069(2) Uani 1 1 d . . . N8 N 0.6202(4) 0.5363(5) 0.5508(5) 0.068(3) Uani 1 1 d . . . N9 N 0.6712(3) 0.5243(5) 0.8577(6) 0.061(2) Uani 1 1 d . . . N10 N 0.6493(3) 0.4207(4) 0.7159(7) 0.0546(19) Uani 1 1 d . . . O1 O 0.5795(6) 0.6821(8) 0.0454(11) 0.235(6) Uani 1 1 d . . . O2 O 0.4942(6) 0.7249(10) 0.0536(12) 0.265(8) Uani 1 1 d . . . O3 O 0.5450(8) 0.6938(8) 0.1944(11) 0.311(10) Uani 1 1 d . . . O4 O 0.5104(7) 0.6034(9) 0.0983(11) 0.261(9) Uani 1 1 d . . . O5 O 0.7419(4) 0.2507(7) 0.4128(7) 0.169(4) Uani 1 1 d . . . O6 O 0.6435(3) 0.2696(5) 0.3896(6) 0.111(3) Uani 1 1 d . . . O7 O 0.7074(5) 0.3494(6) 0.3185(14) 0.244(8) Uani 1 1 d . . . O8 O 0.6998(4) 0.2424(8) 0.2535(8) 0.185(5) Uani 1 1 d . . . O9 O 0.7021(4) 0.0971(5) 0.9498(7) 0.138(3) Uani 1 1 d . . . O10 O 0.6424(4) 0.0717(7) 0.8044(8) 0.168(5) Uani 1 1 d . . . O11 O 0.7352(5) 0.0930(8) 0.7791(8) 0.202(5) Uani 1 1 d . . . O12 O 0.7123(5) -0.0137(7) 0.8559(15) 0.262(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0604(7) 0.0888(10) 0.0507(7) 0.0251(7) -0.0077(7) -0.0113(7) Cu2 0.0805(9) 0.0738(9) 0.0445(6) 0.0173(7) -0.0052(7) 0.0199(7) C1 0.078(5) 0.069(6) 0.088(6) 0.028(4) 0.013(6) -0.016(6) C2 0.095(11) 0.164(14) 0.086(11) 0.020(9) 0.001(9) -0.005(10) C3 0.117(13) 0.169(16) 0.085(11) 0.019(10) -0.006(11) 0.004(11) C4 0.129(14) 0.161(15) 0.096(11) 0.026(10) 0.023(12) -0.002(12) C5 0.098(12) 0.135(14) 0.101(11) 0.032(9) 0.026(10) -0.003(10) C6 0.074(9) 0.118(11) 0.086(10) 0.030(7) 0.018(8) -0.002(8) C7 0.062(9) 0.096(10) 0.101(10) 0.014(8) 0.008(7) -0.006(7) C8 0.107(13) 0.139(15) 0.122(13) 0.034(11) 0.047(10) 0.008(10) C9 0.092(11) 0.137(13) 0.138(14) 0.011(11) 0.031(10) 0.011(9) C10 0.072(10) 0.121(12) 0.124(13) 0.016(10) 0.015(9) 0.001(8) C11 0.061(8) 0.142(13) 0.144(14) 0.017(11) -0.005(9) -0.006(8) C12 0.070(10) 0.138(13) 0.129(12) 0.015(10) -0.022(8) -0.004(9) C13 0.064(8) 0.112(11) 0.112(10) 0.015(8) -0.025(7) -0.007(7) C14 0.119(10) 0.082(10) 0.067(7) -0.009(8) -0.019(7) -0.029(9) C15 0.138(14) 0.083(12) 0.094(12) -0.012(10) -0.021(9) -0.021(10) C16 0.123(12) 0.085(11) 0.109(11) 0.006(10) -0.031(10) -0.015(9) C17 0.098(9) 0.085(11) 0.080(9) 0.024(9) -0.021(7) -0.014(7) C18 0.066(7) 0.074(10) 0.050(6) 0.014(7) -0.021(5) -0.025(6) C19 0.059(7) 0.084(10) 0.046(6) 0.021(7) -0.019(5) -0.023(6) C20 0.106(11) 0.095(13) 0.094(11) 0.039(10) -0.014(8) -0.016(9) C21 0.087(8) 0.113(13) 0.065(9) 0.038(8) -0.009(7) -0.013(9) C22 0.066(7) 0.105(11) 0.053(7) 0.012(8) -0.012(6) -0.023(7) C23 0.095(9) 0.125(14) 0.070(9) -0.004(10) -0.018(6) -0.013(10) C24 0.116(11) 0.116(13) 0.074(10) -0.022(9) -0.017(7) 0.004(9) C25 0.101(10) 0.100(11) 0.076(9) -0.005(9) -0.025(7) 0.001(8) C26 0.083(9) 0.096(10) 0.081(8) 0.006(7) 0.019(7) 0.007(7) C27 0.084(9) 0.108(11) 0.090(9) 0.010(8) 0.030(7) 0.017(8) C28 0.074(8) 0.104(9) 0.108(9) 0.007(9) 0.010(9) 0.020(6) C29 0.059(8) 0.091(9) 0.082(9) 0.019(7) -0.001(7) 0.008(7) C30 0.066(8) 0.078(9) 0.075(8) 0.019(6) 0.004(6) 0.008(6) C31 0.063(7) 0.079(8) 0.050(6) 0.019(5) -0.006(6) 0.015(6) C32 0.068(7) 0.114(10) 0.087(8) 0.022(8) -0.015(8) 0.009(6) C33 0.069(9) 0.103(10) 0.069(7) 0.020(7) -0.017(6) 0.009(7) C34 0.073(8) 0.092(9) 0.059(7) 0.015(6) -0.007(6) 0.007(7) C35 0.097(9) 0.120(10) 0.044(6) 0.034(6) -0.002(6) 0.011(8) C36 0.095(9) 0.136(12) 0.049(7) 0.022(7) 0.014(6) 0.024(8) C37 0.080(9) 0.136(11) 0.053(8) 0.015(7) 0.013(6) 0.027(8) C38 0.119(10) 0.077(10) 0.072(8) 0.000(8) -0.018(7) 0.020(8) C39 0.133(11) 0.094(11) 0.065(9) -0.028(8) -0.026(7) 0.016(9) C40 0.109(9) 0.096(10) 0.050(6) 0.001(8) -0.019(6) 0.011(8) C41 0.056(6) 0.078(8) 0.053(6) 0.010(7) -0.001(5) 0.005(6) C42 0.046(6) 0.070(8) 0.047(6) 0.011(6) -0.002(4) 0.010(5) C43 0.043(6) 0.060(9) 0.050(6) 0.007(6) 0.014(5) 0.011(6) C44 0.053(6) 0.085(10) 0.073(8) 0.044(8) -0.004(5) 0.011(6) C45 0.074(8) 0.073(10) 0.089(9) 0.045(7) 0.006(7) 0.009(7) C46 0.056(7) 0.066(9) 0.076(8) 0.022(8) 0.009(6) 0.007(6) C47 0.079(9) 0.071(10) 0.106(10) 0.012(9) 0.007(7) 0.005(7) C48 0.088(10) 0.077(11) 0.104(12) 0.001(9) 0.001(8) 0.005(8) C49 0.068(8) 0.071(9) 0.077(8) 0.002(7) -0.002(6) 0.011(7) Cl1 0.156(4) 0.170(4) 0.0432(17) 0.010(2) 0.010(2) 0.025(4) Cl2 0.067(2) 0.078(2) 0.0656(18) -0.0003(18) 0.0077(16) -0.0089(18) Cl3 0.126(3) 0.097(3) 0.084(2) -0.005(2) -0.002(2) 0.046(2) N1 0.091(5) 0.064(5) 0.080(5) 0.034(4) 0.011(5) -0.028(5) N2 0.105(6) 0.070(6) 0.073(5) 0.026(4) -0.005(5) -0.014(5) N3 0.072(8) 0.129(9) 0.068(7) 0.044(6) 0.012(6) 0.004(7) N4 0.058(6) 0.090(7) 0.089(8) 0.014(6) -0.008(5) -0.021(5) N5 0.082(6) 0.075(6) 0.050(5) 0.008(5) -0.013(5) -0.022(5) N6 0.074(6) 0.080(8) 0.038(5) 0.011(5) -0.014(4) -0.013(5) N7 0.063(5) 0.082(6) 0.063(6) 0.007(5) 0.011(5) 0.011(4) N8 0.075(6) 0.105(7) 0.025(4) 0.019(4) -0.009(4) 0.014(6) N9 0.077(6) 0.069(7) 0.038(5) 0.010(5) -0.016(4) 0.006(5) N10 0.045(4) 0.067(5) 0.052(5) 0.007(5) 0.005(4) 0.014(4) O1 0.204(13) 0.292(17) 0.208(13) -0.047(12) 0.027(10) -0.015(11) O2 0.201(13) 0.340(19) 0.254(14) 0.188(14) 0.062(10) 0.092(12) O3 0.60(3) 0.176(12) 0.157(11) -0.070(11) -0.004(14) 0.039(13) O4 0.42(2) 0.166(12) 0.202(13) 0.030(11) -0.115(13) -0.115(14) O5 0.111(8) 0.271(13) 0.126(7) 0.039(8) -0.039(6) 0.027(8) O6 0.088(6) 0.164(9) 0.080(5) -0.011(5) 0.009(5) -0.001(6) O7 0.222(13) 0.053(7) 0.46(2) 0.001(11) 0.063(13) -0.048(8) O8 0.105(8) 0.303(15) 0.148(10) -0.099(10) 0.011(6) 0.027(8) O9 0.186(10) 0.133(8) 0.094(7) 0.000(6) 0.013(5) 0.020(7) O10 0.137(9) 0.213(12) 0.155(8) -0.083(8) -0.074(7) 0.078(8) O11 0.219(13) 0.270(15) 0.118(7) 0.035(9) 0.066(9) 0.037(11) O12 0.157(10) 0.116(10) 0.51(2) -0.047(14) -0.058(13) 0.049(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 N1 1.930(9) . ? Cu1 N6 1.976(9) . ? Cu1 N3 2.036(9) . ? Cu1 N5 2.048(8) . ? Cu1 N4 2.148(8) . ? Cu2 N8 1.988(7) . ? Cu2 N9 1.993(7) . ? Cu2 N2 1.993(8) . ? Cu2 N10 2.022(7) . ? Cu2 N7 2.141(7) . ? C1 N1 1.151(12) . ? C1 N2 1.267(12) . ? C2 N3 1.270(15) . ? C2 C3 1.421(17) . ? C2 H2 0.9300 . ? C3 C4 1.309(16) . ? C3 H3 0.9300 . ? C4 C5 1.395(18) . ? C4 H4 0.9300 . ? C5 C6 1.377(16) . ? C5 C8 1.423(18) . ? C6 N3 1.331(13) . ? C6 C7 1.508(15) . ? C7 N4 1.305(12) . ? C7 C10 1.391(14) . ? C8 C9 1.327(17) . ? C8 H8 0.9300 . ? C9 C10 1.416(16) . ? C9 H9 0.9300 . ? C10 C11 1.413(16) . ? C11 C12 1.330(15) . ? C11 H11 0.9300 . ? C12 C13 1.391(14) . ? C12 H12 0.9300 . ? C13 N4 1.350(12) . ? C13 H13 0.9300 . ? C14 N5 1.319(12) . ? C14 C15 1.342(16) . ? C14 H14 0.9300 . ? C15 C16 1.281(15) . ? C15 H15 0.9300 . ? C16 C17 1.549(17) . ? C16 H16 0.9300 . ? C17 C20 1.334(14) . ? C17 C18 1.424(14) . ? C18 N5 1.358(11) . ? C18 C19 1.376(13) . ? C19 N6 1.336(11) . ? C19 C22 1.388(13) . ? C20 C21 1.285(15) . ? C20 H20 0.9300 . ? C21 C22 1.437(15) . ? C21 H21 0.9300 . ? C22 C23 1.364(13) . ? C23 C24 1.335(15) . ? C23 H23 0.9300 . ? C24 C25 1.431(15) . ? C24 H24 0.9300 . ? C25 N6 1.347(13) . ? C25 H25 0.9300 . ? C26 N7 1.293(11) . ? C26 C27 1.408(13) . ? C26 H26 0.9300 . ? C27 C28 1.347(13) . ? C27 H27 0.9300 . ? C28 C29 1.409(13) . ? C28 H28 0.9300 . ? C29 C30 1.394(13) . ? C29 C32 1.397(12) . ? C30 N7 1.414(11) . ? C30 C31 1.432(12) . ? C31 N8 1.312(10) . ? C31 C34 1.415(12) . ? C32 C33 1.296(12) . ? C32 H32 0.9300 . ? C33 C34 1.422(13) . ? C33 H33 0.9300 . ? C34 C35 1.363(13) . ? C35 C36 1.333(13) . ? C35 H35 0.9300 . ? C36 C37 1.354(12) . ? C36 H36 0.9300 . ? C37 N8 1.324(11) . ? C37 H37 0.9300 . ? C38 N9 1.323(12) . ? C38 C39 1.470(14) . ? C38 H38 0.9300 . ? C39 C40 1.333(13) . ? C39 H39 0.9300 . ? C40 C41 1.391(13) . ? C40 H40 0.9300 . ? C41 C44 1.393(12) . ? C41 C42 1.412(12) . ? C42 N9 1.388(11) . ? C42 C43 1.395(12) . ? C43 C46 1.360(12) . ? C43 N10 1.366(11) . ? C44 C45 1.385(14) . ? C44 H44 0.9300 . ? C45 C46 1.463(14) . ? C45 H45 0.9300 . ? C46 C47 1.390(14) . ? C47 C48 1.337(14) . ? C47 H47 0.9300 . ? C48 C49 1.379(14) . ? C48 H48 0.9300 . ? C49 N10 1.350(11) . ? C49 H49 0.9300 . ? Cl1 O3 1.271(13) . ? Cl1 O2 1.321(12) . ? Cl1 O4 1.356(12) . ? Cl1 O1 1.363(13) . ? Cl2 O7 1.268(11) . ? Cl2 O8 1.385(9) . ? Cl2 O5 1.388(9) . ? Cl2 O6 1.409(8) . ? Cl3 O12 1.344(11) . ? Cl3 O9 1.398(9) . ? Cl3 O11 1.405(11) . ? Cl3 O10 1.411(9) . ? N2 H2A 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N6 93.6(4) . . ? N1 Cu1 N3 92.8(4) . . ? N6 Cu1 N3 173.3(4) . . ? N1 Cu1 N5 145.4(3) . . ? N6 Cu1 N5 79.9(4) . . ? N3 Cu1 N5 93.8(4) . . ? N1 Cu1 N4 118.8(3) . . ? N6 Cu1 N4 97.8(4) . . ? N3 Cu1 N4 80.6(4) . . ? N5 Cu1 N4 95.8(3) . . ? N8 Cu2 N9 175.7(4) . . ? N8 Cu2 N2 90.0(4) . . ? N9 Cu2 N2 94.1(3) . . ? N8 Cu2 N10 95.7(4) . . ? N9 Cu2 N10 80.4(4) . . ? N2 Cu2 N10 146.6(3) . . ? N8 Cu2 N7 79.2(4) . . ? N9 Cu2 N7 100.6(3) . . ? N2 Cu2 N7 104.1(3) . . ? N10 Cu2 N7 109.3(3) . . ? N1 C1 N2 177.4(12) . . ? N3 C2 C3 115.5(14) . . ? N3 C2 H2 122.2 . . ? C3 C2 H2 122.2 . . ? C4 C3 C2 120.5(15) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 123.8(15) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C6 C5 C4 112.3(14) . . ? C6 C5 C8 119.5(14) . . ? C4 C5 C8 128.1(15) . . ? N3 C6 C5 122.8(12) . . ? N3 C6 C7 118.2(11) . . ? C5 C6 C7 118.9(13) . . ? N4 C7 C10 125.5(12) . . ? N4 C7 C6 115.7(11) . . ? C10 C7 C6 118.7(12) . . ? C9 C8 C5 121.0(13) . . ? C9 C8 H8 119.5 . . ? C5 C8 H8 119.5 . . ? C8 C9 C10 123.5(14) . . ? C8 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? C7 C10 C11 114.5(13) . . ? C7 C10 C9 118.3(14) . . ? C11 C10 C9 127.2(14) . . ? C12 C11 C10 120.6(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.9(13) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N4 C13 C12 119.8(12) . . ? N4 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? N5 C14 C15 127.3(12) . . ? N5 C14 H14 116.3 . . ? C15 C14 H14 116.3 . . ? C16 C15 C14 118.8(15) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 121.3(14) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C20 C17 C18 118.6(13) . . ? C20 C17 C16 129.8(14) . . ? C18 C17 C16 111.5(12) . . ? N5 C18 C19 115.4(10) . . ? N5 C18 C17 123.6(11) . . ? C19 C18 C17 121.0(11) . . ? N6 C19 C18 117.8(10) . . ? N6 C19 C22 123.5(12) . . ? C18 C19 C22 118.7(12) . . ? C21 C20 C17 121.7(14) . . ? C21 C20 H20 119.2 . . ? C17 C20 H20 119.2 . . ? C20 C21 C22 123.3(12) . . ? C20 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C23 C22 C19 118.5(12) . . ? C23 C22 C21 124.9(12) . . ? C19 C22 C21 116.6(12) . . ? C24 C23 C22 120.0(12) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 119.9(13) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N6 C25 C24 120.3(13) . . ? N6 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? N7 C26 C27 124.6(11) . . ? N7 C26 H26 117.7 . . ? C27 C26 H26 117.7 . . ? C28 C27 C26 118.4(10) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 122.6(10) . . ? C27 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? C30 C29 C32 119.1(11) . . ? C30 C29 C28 113.5(10) . . ? C32 C29 C28 127.4(12) . . ? C29 C30 N7 125.7(10) . . ? C29 C30 C31 119.7(10) . . ? N7 C30 C31 114.5(9) . . ? N8 C31 C34 122.9(9) . . ? N8 C31 C30 117.7(9) . . ? C34 C31 C30 118.9(10) . . ? C33 C32 C29 121.6(10) . . ? C33 C32 H32 119.2 . . ? C29 C32 H32 119.2 . . ? C32 C33 C34 123.2(10) . . ? C32 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C35 C34 C31 117.8(10) . . ? C35 C34 C33 125.0(10) . . ? C31 C34 C33 117.1(10) . . ? C36 C35 C34 119.2(10) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 118.5(10) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? N8 C37 C36 125.6(10) . . ? N8 C37 H37 117.2 . . ? C36 C37 H37 117.2 . . ? N9 C38 C39 120.8(11) . . ? N9 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 118.4(11) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? C39 C40 C41 122.4(10) . . ? C39 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C40 C41 C44 124.4(10) . . ? C40 C41 C42 117.2(10) . . ? C44 C41 C42 118.4(11) . . ? N9 C42 C43 117.0(9) . . ? N9 C42 C41 121.9(10) . . ? C43 C42 C41 121.1(10) . . ? C46 C43 N10 123.2(10) . . ? C46 C43 C42 122.3(11) . . ? N10 C43 C42 114.4(10) . . ? C45 C44 C41 120.1(10) . . ? C45 C44 H44 120.0 . . ? C41 C44 H44 120.0 . . ? C44 C45 C46 121.7(11) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C43 C46 C47 120.7(11) . . ? C43 C46 C45 116.3(12) . . ? C47 C46 C45 122.8(13) . . ? C48 C47 C46 115.2(13) . . ? C48 C47 H47 122.4 . . ? C46 C47 H47 122.4 . . ? C47 C48 C49 123.7(13) . . ? C47 C48 H48 118.1 . . ? C49 C48 H48 118.1 . . ? N10 C49 C48 121.2(11) . . ? N10 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? O3 Cl1 O2 114.3(11) . . ? O3 Cl1 O4 110.2(10) . . ? O2 Cl1 O4 115.1(11) . . ? O3 Cl1 O1 100.0(11) . . ? O2 Cl1 O1 105.5(9) . . ? O4 Cl1 O1 110.6(10) . . ? O7 Cl2 O8 102.6(9) . . ? O7 Cl2 O5 116.1(8) . . ? O8 Cl2 O5 105.3(6) . . ? O7 Cl2 O6 113.6(7) . . ? O8 Cl2 O6 103.3(6) . . ? O5 Cl2 O6 114.0(6) . . ? O12 Cl3 O9 113.7(9) . . ? O12 Cl3 O11 105.3(8) . . ? O9 Cl3 O11 106.5(7) . . ? O12 Cl3 O10 114.7(8) . . ? O9 Cl3 O10 111.2(6) . . ? O11 Cl3 O10 104.4(8) . . ? C1 N1 Cu1 134.5(9) . . ? C1 N2 Cu2 128.1(7) . . ? C1 N2 H2A 116.0 . . ? Cu2 N2 H2A 116.0 . . ? C2 N3 C6 125.0(12) . . ? C2 N3 Cu1 121.8(10) . . ? C6 N3 Cu1 113.2(9) . . ? C7 N4 C13 118.7(10) . . ? C7 N4 Cu1 111.8(8) . . ? C13 N4 Cu1 129.0(8) . . ? C14 N5 C18 116.9(9) . . ? C14 N5 Cu1 130.5(8) . . ? C18 N5 Cu1 112.3(8) . . ? C19 N6 C25 117.8(10) . . ? C19 N6 Cu1 114.4(7) . . ? C25 N6 Cu1 127.7(9) . . ? C26 N7 C30 115.0(8) . . ? C26 N7 Cu2 134.2(8) . . ? C30 N7 Cu2 110.5(7) . . ? C31 N8 C37 115.0(8) . . ? C31 N8 Cu2 117.9(7) . . ? C37 N8 Cu2 127.1(7) . . ? C38 N9 C42 119.2(8) . . ? C38 N9 Cu2 127.2(8) . . ? C42 N9 Cu2 113.4(7) . . ? C49 N10 C43 115.7(9) . . ? C49 N10 Cu2 129.5(7) . . ? C43 N10 Cu2 114.6(7) . . ? 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 N3 C2 C3 C4 -3(2) . . . . ? C2 C3 C4 C5 2(3) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C3 C4 C5 C8 177.7(15) . . . . ? C4 C5 C6 N3 -3(2) . . . . ? C8 C5 C6 N3 -180.0(12) . . . . ? C4 C5 C6 C7 -179.6(12) . . . . ? C8 C5 C6 C7 4(2) . . . . ? N3 C6 C7 N4 5.7(17) . . . . ? C5 C6 C7 N4 -177.7(12) . . . . ? N3 C6 C7 C10 -177.3(11) . . . . ? C5 C6 C7 C10 -0.6(18) . . . . ? C6 C5 C8 C9 -5(2) . . . . ? C4 C5 C8 C9 178.8(16) . . . . ? C5 C8 C9 C10 3(2) . . . . ? N4 C7 C10 C11 -2(2) . . . . ? C6 C7 C10 C11 -179.0(11) . . . . ? N4 C7 C10 C9 175.5(12) . . . . ? C6 C7 C10 C9 -1(2) . . . . ? C8 C9 C10 C7 0(2) . . . . ? C8 C9 C10 C11 177.5(16) . . . . ? C7 C10 C11 C12 0(2) . . . . ? C9 C10 C11 C12 -177.9(16) . . . . ? C10 C11 C12 C13 2(2) . . . . ? C11 C12 C13 N4 -1(2) . . . . ? N5 C14 C15 C16 5(2) . . . . ? C14 C15 C16 C17 -9(2) . . . . ? C15 C16 C17 C20 -176.6(14) . . . . ? C15 C16 C17 C18 8.1(18) . . . . ? C20 C17 C18 N5 -179.8(10) . . . . ? C16 C17 C18 N5 -3.9(14) . . . . ? C20 C17 C18 C19 -1.0(16) . . . . ? C16 C17 C18 C19 174.9(9) . . . . ? N5 C18 C19 N6 1.9(12) . . . . ? C17 C18 C19 N6 -177.0(9) . . . . ? N5 C18 C19 C22 -178.8(8) . . . . ? C17 C18 C19 C22 2.3(14) . . . . ? C18 C17 C20 C21 -2(2) . . . . ? C16 C17 C20 C21 -176.9(13) . . . . ? C17 C20 C21 C22 3(2) . . . . ? N6 C19 C22 C23 -0.4(14) . . . . ? C18 C19 C22 C23 -179.7(9) . . . . ? N6 C19 C22 C21 178.3(9) . . . . ? C18 C19 C22 C21 -1.1(13) . . . . ? C20 C21 C22 C23 176.9(12) . . . . ? C20 C21 C22 C19 -1.7(17) . . . . ? C19 C22 C23 C24 -0.9(17) . . . . ? C21 C22 C23 C24 -179.4(11) . . . . ? C22 C23 C24 C25 2(2) . . . . ? C23 C24 C25 N6 -1.3(19) . . . . ? N7 C26 C27 C28 1.4(18) . . . . ? C26 C27 C28 C29 -1.1(17) . . . . ? C27 C28 C29 C30 -0.9(16) . . . . ? C27 C28 C29 C32 -178.6(12) . . . . ? C32 C29 C30 N7 -179.1(9) . . . . ? C28 C29 C30 N7 3.0(17) . . . . ? C32 C29 C30 C31 -2.5(17) . . . . ? C28 C29 C30 C31 179.7(9) . . . . ? C29 C30 C31 N8 178.5(10) . . . . ? N7 C30 C31 N8 -4.4(14) . . . . ? C29 C30 C31 C34 6.5(15) . . . . ? N7 C30 C31 C34 -176.5(9) . . . . ? C30 C29 C32 C33 -4.1(17) . . . . ? C28 C29 C32 C33 173.5(12) . . . . ? C29 C32 C33 C34 6.5(18) . . . . ? N8 C31 C34 C35 6.6(16) . . . . ? C30 C31 C34 C35 178.2(11) . . . . ? N8 C31 C34 C33 -175.9(10) . . . . ? C30 C31 C34 C33 -4.3(15) . . . . ? C32 C33 C34 C35 175.1(12) . . . . ? C32 C33 C34 C31 -2.2(17) . . . . ? C31 C34 C35 C36 -4.6(17) . . . . ? C33 C34 C35 C36 178.1(11) . . . . ? C34 C35 C36 C37 5.8(19) . . . . ? C35 C36 C37 N8 -9(2) . . . . ? N9 C38 C39 C40 3.5(19) . . . . ? C38 C39 C40 C41 0.1(19) . . . . ? C39 C40 C41 C44 179.9(11) . . . . ? C39 C40 C41 C42 -2.7(16) . . . . ? C40 C41 C42 N9 2.0(13) . . . . ? C44 C41 C42 N9 179.6(8) . . . . ? C40 C41 C42 C43 -178.1(8) . . . . ? C44 C41 C42 C43 -0.5(13) . . . . ? N9 C42 C43 C46 -178.3(9) . . . . ? C41 C42 C43 C46 1.7(14) . . . . ? N9 C42 C43 N10 -1.5(12) . . . . ? C41 C42 C43 N10 178.6(7) . . . . ? C40 C41 C44 C45 179.1(10) . . . . ? C42 C41 C44 C45 1.7(14) . . . . ? C41 C44 C45 C46 -4.0(15) . . . . ? N10 C43 C46 C47 5.2(15) . . . . ? C42 C43 C46 C47 -178.2(9) . . . . ? N10 C43 C46 C45 179.7(8) . . . . ? C42 C43 C46 C45 -3.8(14) . . . . ? C44 C45 C46 C43 4.9(15) . . . . ? C44 C45 C46 C47 179.3(10) . . . . ? C43 C46 C47 C48 -5.7(16) . . . . ? C45 C46 C47 C48 -179.8(10) . . . . ? C46 C47 C48 C49 3.7(17) . . . . ? C47 C48 C49 N10 -1.0(18) . . . . ? N2 C1 N1 Cu1 97(31) . . . . ? N6 Cu1 N1 C1 179.7(11) . . . . ? N3 Cu1 N1 C1 1.4(11) . . . . ? N5 Cu1 N1 C1 102.3(12) . . . . ? N4 Cu1 N1 C1 -79.4(12) . . . . ? N1 C1 N2 Cu2 3(31) . . . . ? N8 Cu2 N2 C1 14.8(10) . . . . ? N9 Cu2 N2 C1 -166.1(9) . . . . ? N10 Cu2 N2 C1 115.2(10) . . . . ? N7 Cu2 N2 C1 -64.1(10) . . . . ? C3 C2 N3 C6 1(2) . . . . ? C3 C2 N3 Cu1 -179.1(9) . . . . ? C5 C6 N3 C2 2(2) . . . . ? C7 C6 N3 C2 178.6(14) . . . . ? C5 C6 N3 Cu1 -177.8(11) . . . . ? C7 C6 N3 Cu1 -1.3(14) . . . . ? N1 Cu1 N3 C2 59.6(12) . . . . ? N6 Cu1 N3 C2 -105(4) . . . . ? N5 Cu1 N3 C2 -86.4(12) . . . . ? N4 Cu1 N3 C2 178.4(13) . . . . ? N1 Cu1 N3 C6 -120.4(8) . . . . ? N6 Cu1 N3 C6 75(4) . . . . ? N5 Cu1 N3 C6 93.5(8) . . . . ? N4 Cu1 N3 C6 -1.7(8) . . . . ? C10 C7 N4 C13 3.2(18) . . . . ? C6 C7 N4 C13 -180.0(11) . . . . ? C10 C7 N4 Cu1 176.5(11) . . . . ? C6 C7 N4 Cu1 -6.7(13) . . . . ? C12 C13 N4 C7 -1.5(16) . . . . ? C12 C13 N4 Cu1 -173.5(8) . . . . ? N1 Cu1 N4 C7 92.8(9) . . . . ? N6 Cu1 N4 C7 -168.7(8) . . . . ? N3 Cu1 N4 C7 4.8(8) . . . . ? N5 Cu1 N4 C7 -88.2(8) . . . . ? N1 Cu1 N4 C13 -94.8(10) . . . . ? N6 Cu1 N4 C13 3.7(10) . . . . ? N3 Cu1 N4 C13 177.2(10) . . . . ? N5 Cu1 N4 C13 84.3(10) . . . . ? C15 C14 N5 C18 -0.8(18) . . . . ? C15 C14 N5 Cu1 -174.3(11) . . . . ? C19 C18 N5 C14 -178.2(9) . . . . ? C17 C18 N5 C14 0.7(14) . . . . ? C19 C18 N5 Cu1 -3.5(10) . . . . ? C17 C18 N5 Cu1 175.3(8) . . . . ? N1 Cu1 N5 C14 -101.6(10) . . . . ? N6 Cu1 N5 C14 176.8(9) . . . . ? N3 Cu1 N5 C14 -1.0(10) . . . . ? N4 Cu1 N5 C14 79.9(9) . . . . ? N1 Cu1 N5 C18 84.6(8) . . . . ? N6 Cu1 N5 C18 3.1(6) . . . . ? N3 Cu1 N5 C18 -174.8(7) . . . . ? N4 Cu1 N5 C18 -93.9(6) . . . . ? C18 C19 N6 C25 -179.9(9) . . . . ? C22 C19 N6 C25 0.8(15) . . . . ? C18 C19 N6 Cu1 0.9(11) . . . . ? C22 C19 N6 Cu1 -178.5(7) . . . . ? C24 C25 N6 C19 0.1(16) . . . . ? C24 C25 N6 Cu1 179.2(8) . . . . ? N1 Cu1 N6 C19 -147.9(7) . . . . ? N3 Cu1 N6 C19 17(4) . . . . ? N5 Cu1 N6 C19 -2.1(7) . . . . ? N4 Cu1 N6 C19 92.4(7) . . . . ? N1 Cu1 N6 C25 33.0(9) . . . . ? N3 Cu1 N6 C25 -162(4) . . . . ? N5 Cu1 N6 C25 178.7(9) . . . . ? N4 Cu1 N6 C25 -86.8(9) . . . . ? C27 C26 N7 C30 0.4(15) . . . . ? C27 C26 N7 Cu2 174.2(8) . . . . ? C29 C30 N7 C26 -2.8(15) . . . . ? C31 C30 N7 C26 -179.6(10) . . . . ? C29 C30 N7 Cu2 -178.1(10) . . . . ? C31 C30 N7 Cu2 5.1(11) . . . . ? N8 Cu2 N7 C26 -177.5(11) . . . . ? N9 Cu2 N7 C26 6.9(11) . . . . ? N2 Cu2 N7 C26 -90.2(10) . . . . ? N10 Cu2 N7 C26 90.2(10) . . . . ? N8 Cu2 N7 C30 -3.4(7) . . . . ? N9 Cu2 N7 C30 -179.1(7) . . . . ? N2 Cu2 N7 C30 83.9(7) . . . . ? N10 Cu2 N7 C30 -95.7(7) . . . . ? C34 C31 N8 C37 -9.1(16) . . . . ? C30 C31 N8 C37 179.2(10) . . . . ? C34 C31 N8 Cu2 173.0(8) . . . . ? C30 C31 N8 Cu2 1.3(13) . . . . ? C36 C37 N8 C31 10.6(19) . . . . ? C36 C37 N8 Cu2 -171.7(10) . . . . ? N9 Cu2 N8 C31 88(5) . . . . ? N2 Cu2 N8 C31 -103.1(8) . . . . ? N10 Cu2 N8 C31 109.8(8) . . . . ? N7 Cu2 N8 C31 1.3(8) . . . . ? N9 Cu2 N8 C37 -89(5) . . . . ? N2 Cu2 N8 C37 79.3(11) . . . . ? N10 Cu2 N8 C37 -67.8(11) . . . . ? N7 Cu2 N8 C37 -176.4(11) . . . . ? C39 C38 N9 C42 -4.2(16) . . . . ? C39 C38 N9 Cu2 -179.8(8) . . . . ? C43 C42 N9 C38 -178.4(9) . . . . ? C41 C42 N9 C38 1.5(14) . . . . ? C43 C42 N9 Cu2 -2.2(10) . . . . ? C41 C42 N9 Cu2 177.7(6) . . . . ? N8 Cu2 N9 C38 -159(5) . . . . ? N2 Cu2 N9 C38 32.5(10) . . . . ? N10 Cu2 N9 C38 179.4(10) . . . . ? N7 Cu2 N9 C38 -72.7(10) . . . . ? N8 Cu2 N9 C42 25(6) . . . . ? N2 Cu2 N9 C42 -143.3(6) . . . . ? N10 Cu2 N9 C42 3.5(6) . . . . ? N7 Cu2 N9 C42 111.5(6) . . . . ? C48 C49 N10 C43 0.0(14) . . . . ? C48 C49 N10 Cu2 175.9(8) . . . . ? C46 C43 N10 C49 -2.2(13) . . . . ? C42 C43 N10 C49 -179.0(7) . . . . ? C46 C43 N10 Cu2 -178.7(7) . . . . ? C42 C43 N10 Cu2 4.5(10) . . . . ? N8 Cu2 N10 C49 1.2(8) . . . . ? N9 Cu2 N10 C49 179.6(8) . . . . ? N2 Cu2 N10 C49 -97.6(9) . . . . ? N7 Cu2 N10 C49 81.7(8) . . . . ? N8 Cu2 N10 C43 177.1(6) . . . . ? N9 Cu2 N10 C43 -4.4(6) . . . . ? N2 Cu2 N10 C43 78.4(8) . . . . ? N7 Cu2 N10 C43 -102.4(6) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.051 253 68 ' ' 2 0.000 0.500 -0.051 253 69 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.415 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.057 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 787751' #TrackingRef 'cif-all-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Cl2 Cu2 N8 O8' _chemical_formula_sum 'C22 H18 Cl2 Cu2 N8 O8 ' _chemical_formula_weight 720.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2913(18) _cell_length_b 8.9194(19) _cell_length_c 9.332(2) _cell_angle_alpha 94.661(4) _cell_angle_beta 99.624(4) _cell_angle_gamma 101.893(4) _cell_volume 661.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 362.0 _exptl_absorpt_coefficient_mu 1.875 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8494 _exptl_absorpt_correction_T_max 0.8878 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3576 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2535 _reflns_number_gt 2197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2535 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.47693(4) 0.26394(3) 0.63508(3) 0.04058(15) Uani 1 1 d . . . C1 C 0.3599(4) 0.4296(3) 0.3883(3) 0.0418(6) Uani 1 1 d . . . C2 C 0.2068(4) 0.0034(3) 0.4714(3) 0.0467(7) Uani 1 1 d . . . H2 H 0.1773 0.0755 0.4113 0.056 Uiso 1 1 calc R . . C3 C 0.1108(4) -0.1461(4) 0.4461(4) 0.0555(8) Uani 1 1 d . . . H3 H 0.0181 -0.1743 0.3701 0.067 Uiso 1 1 calc R . . C4 C 0.1546(4) -0.2509(4) 0.5345(4) 0.0620(9) Uani 1 1 d . . . H4 H 0.0920 -0.3521 0.5191 0.074 Uiso 1 1 calc R . . C5 C 0.2921(4) -0.2067(3) 0.6471(4) 0.0569(8) Uani 1 1 d . . . H5 H 0.3224 -0.2768 0.7092 0.068 Uiso 1 1 calc R . . C6 C 0.3838(4) -0.0562(3) 0.6655(3) 0.0403(6) Uani 1 1 d . . . C7 C 0.5359(3) 0.0044(3) 0.7802(3) 0.0389(6) Uani 1 1 d . . . C8 C 0.6070(4) -0.0835(3) 0.8747(3) 0.0504(8) Uani 1 1 d . . . H8 H 0.5586 -0.1879 0.8713 0.061 Uiso 1 1 calc R . . C9 C 0.7519(4) -0.0160(4) 0.9756(4) 0.0541(8) Uani 1 1 d . . . H9 H 0.8007 -0.0734 1.0421 0.065 Uiso 1 1 calc R . . C10 C 0.8219(4) 0.1377(4) 0.9752(4) 0.0521(8) Uani 1 1 d . . . H10 H 0.9198 0.1854 1.0409 0.062 Uiso 1 1 calc R . . C11 C 0.7464(4) 0.2202(3) 0.8775(3) 0.0465(7) Uani 1 1 d . . . H11 H 0.7948 0.3241 0.8779 0.056 Uiso 1 1 calc R . . N1 N 0.3525(4) 0.3397(3) 0.4710(3) 0.0562(7) Uani 1 1 d . . . N2 N 0.6315(3) 0.4640(3) 0.6956(3) 0.0473(6) Uani 1 1 d . . . H2A H 0.6952 0.4810 0.7807 0.057 Uiso 1 1 calc R . . N3 N 0.3406(3) 0.0474(3) 0.5795(2) 0.0397(5) Uani 1 1 d . . . N4 N 0.6044(3) 0.1558(3) 0.7806(3) 0.0393(5) Uani 1 1 d . . . Cl1 Cl 0.23383(8) 0.42352(7) 0.86395(7) 0.04258(19) Uani 1 1 d . . . O1 O 0.2800(3) 0.2897(2) 0.7983(3) 0.0616(6) Uani 1 1 d . . . O2 O 0.0961(3) 0.4557(3) 0.7697(3) 0.0772(8) Uani 1 1 d . . . O3 O 0.3718(3) 0.5538(2) 0.8890(3) 0.0605(6) Uani 1 1 d . . . O4 O 0.1876(3) 0.3880(3) 0.9998(3) 0.0661(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0476(2) 0.0276(2) 0.0417(2) 0.00446(14) 0.00374(15) 0.00103(15) C1 0.0427(15) 0.0305(14) 0.0426(15) -0.0019(12) -0.0045(12) -0.0009(12) C2 0.0505(17) 0.0406(16) 0.0454(16) -0.0020(13) 0.0069(13) 0.0063(14) C3 0.0494(18) 0.0449(18) 0.0602(19) -0.0096(15) 0.0007(15) -0.0030(15) C4 0.061(2) 0.0372(17) 0.077(2) -0.0037(16) 0.0090(17) -0.0071(15) C5 0.061(2) 0.0322(16) 0.070(2) 0.0064(14) 0.0070(16) -0.0013(14) C6 0.0462(16) 0.0287(14) 0.0462(15) 0.0016(11) 0.0149(12) 0.0046(12) C7 0.0441(15) 0.0283(14) 0.0452(15) 0.0043(11) 0.0134(12) 0.0066(12) C8 0.0552(19) 0.0337(16) 0.064(2) 0.0121(14) 0.0149(15) 0.0080(14) C9 0.0525(18) 0.0481(18) 0.063(2) 0.0168(15) 0.0051(15) 0.0153(15) C10 0.0448(17) 0.0487(18) 0.0580(19) 0.0084(14) -0.0002(14) 0.0069(14) C11 0.0460(16) 0.0336(15) 0.0559(17) 0.0030(13) 0.0062(13) 0.0033(13) N1 0.0620(17) 0.0372(14) 0.0549(15) 0.0122(12) -0.0090(13) -0.0085(12) N2 0.0564(15) 0.0344(13) 0.0400(13) 0.0056(10) -0.0066(11) -0.0026(11) N3 0.0434(12) 0.0315(12) 0.0422(12) -0.0008(9) 0.0102(10) 0.0042(10) N4 0.0431(13) 0.0273(11) 0.0452(13) 0.0031(9) 0.0080(10) 0.0033(10) Cl1 0.0444(4) 0.0310(4) 0.0463(4) -0.0006(3) 0.0024(3) 0.0017(3) O1 0.0795(16) 0.0397(12) 0.0698(15) 0.0012(10) 0.0297(12) 0.0125(11) O2 0.0625(15) 0.0633(17) 0.0904(19) 0.0030(14) -0.0228(14) 0.0118(13) O3 0.0513(13) 0.0381(12) 0.0805(16) 0.0075(11) -0.0003(11) -0.0064(10) O4 0.0803(16) 0.0545(14) 0.0570(13) -0.0039(11) 0.0241(12) -0.0047(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.947(3) . ? Cu1 N2 1.949(2) . ? Cu1 N3 2.004(2) . ? Cu1 N4 2.011(2) . ? Cu1 O1 2.443(2) . ? C1 N1 1.157(4) . ? C1 N2 1.277(4) 2_666 ? C2 N3 1.336(4) . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.361(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(4) . ? C5 H5 0.9300 . ? C6 N3 1.337(4) . ? C6 C7 1.484(4) . ? C7 N4 1.352(3) . ? C7 C8 1.367(4) . ? C8 C9 1.387(4) . ? C8 H8 0.9300 . ? C9 C10 1.375(4) . ? C9 H9 0.9300 . ? C10 C11 1.368(4) . ? C10 H10 0.9300 . ? C11 N4 1.347(4) . ? C11 H11 0.9300 . ? N2 C1 1.277(4) 2_666 ? N2 H2A 0.8600 . ? Cl1 O2 1.414(2) . ? Cl1 O3 1.425(2) . ? Cl1 O4 1.426(2) . ? Cl1 O1 1.447(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 N1 Cu1 N2 92.48(10) . . ? N1 Cu1 N3 92.78(10) . . ? N2 Cu1 N3 173.43(9) . . ? N1 Cu1 N4 170.57(10) . . ? N2 Cu1 N4 94.05(9) . . ? N3 Cu1 N4 80.28(9) . . ? N1 Cu1 O1 95.14(11) . . ? N2 Cu1 O1 98.28(10) . . ? N3 Cu1 O1 85.17(8) . . ? N4 Cu1 O1 90.66(9) . . ? N1 C1 N2 176.0(3) . 2_666 ? N3 C2 C3 122.0(3) . . ? N3 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 118.6(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N3 C6 C5 121.7(3) . . ? N3 C6 C7 114.5(2) . . ? C5 C6 C7 123.7(3) . . ? N4 C7 C8 121.8(3) . . ? N4 C7 C6 114.0(2) . . ? C8 C7 C6 124.2(2) . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N4 C11 C10 122.1(3) . . ? N4 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C1 N1 Cu1 145.1(2) . . ? C1 N2 Cu1 121.39(19) 2_666 . ? C1 N2 H2A 119.3 2_666 . ? Cu1 N2 H2A 119.3 . . ? C2 N3 C6 119.1(2) . . ? C2 N3 Cu1 125.1(2) . . ? C6 N3 Cu1 115.67(19) . . ? C11 N4 C7 118.4(2) . . ? C11 N4 Cu1 126.39(19) . . ? C7 N4 Cu1 115.17(18) . . ? O2 Cl1 O3 109.76(15) . . ? O2 Cl1 O4 109.94(17) . . ? O3 Cl1 O4 109.71(14) . . ? O2 Cl1 O1 109.28(15) . . ? O3 Cl1 O1 110.42(14) . . ? O4 Cl1 O1 107.69(14) . . ? Cl1 O1 Cu1 131.80(14) . . ? 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 N3 C2 C3 C4 0.0(5) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C4 C5 C6 N3 1.4(5) . . . . ? C4 C5 C6 C7 -178.7(3) . . . . ? N3 C6 C7 N4 1.1(3) . . . . ? C5 C6 C7 N4 -178.8(3) . . . . ? N3 C6 C7 C8 -176.4(3) . . . . ? C5 C6 C7 C8 3.7(5) . . . . ? N4 C7 C8 C9 1.0(4) . . . . ? C6 C7 C8 C9 178.4(3) . . . . ? C7 C8 C9 C10 -1.4(5) . . . . ? C8 C9 C10 C11 0.8(5) . . . . ? C9 C10 C11 N4 0.1(5) . . . . ? N2 C1 N1 Cu1 -71(5) 2_666 . . . ? N2 Cu1 N1 C1 26.6(5) . . . . ? N3 Cu1 N1 C1 -149.4(5) . . . . ? N4 Cu1 N1 C1 -107.1(6) . . . . ? O1 Cu1 N1 C1 125.2(5) . . . . ? N1 Cu1 N2 C1 -13.9(3) . . . 2_666 ? N3 Cu1 N2 C1 129.2(7) . . . 2_666 ? N4 Cu1 N2 C1 159.3(3) . . . 2_666 ? O1 Cu1 N2 C1 -109.5(3) . . . 2_666 ? C3 C2 N3 C6 0.4(4) . . . . ? C3 C2 N3 Cu1 -175.0(2) . . . . ? C5 C6 N3 C2 -1.1(4) . . . . ? C7 C6 N3 C2 179.0(2) . . . . ? C5 C6 N3 Cu1 174.7(2) . . . . ? C7 C6 N3 Cu1 -5.2(3) . . . . ? N1 Cu1 N3 C2 -5.4(2) . . . . ? N2 Cu1 N3 C2 -148.5(8) . . . . ? N4 Cu1 N3 C2 -178.9(2) . . . . ? O1 Cu1 N3 C2 89.6(2) . . . . ? N1 Cu1 N3 C6 179.1(2) . . . . ? N2 Cu1 N3 C6 36.0(9) . . . . ? N4 Cu1 N3 C6 5.51(19) . . . . ? O1 Cu1 N3 C6 -86.0(2) . . . . ? C10 C11 N4 C7 -0.5(4) . . . . ? C10 C11 N4 Cu1 178.2(2) . . . . ? C8 C7 N4 C11 -0.1(4) . . . . ? C6 C7 N4 C11 -177.7(2) . . . . ? C8 C7 N4 Cu1 -178.9(2) . . . . ? C6 C7 N4 Cu1 3.4(3) . . . . ? N1 Cu1 N4 C11 133.4(6) . . . . ? N2 Cu1 N4 C11 -0.2(2) . . . . ? N3 Cu1 N4 C11 176.4(2) . . . . ? O1 Cu1 N4 C11 -98.6(2) . . . . ? N1 Cu1 N4 C7 -47.9(7) . . . . ? N2 Cu1 N4 C7 178.5(2) . . . . ? N3 Cu1 N4 C7 -4.82(19) . . . . ? O1 Cu1 N4 C7 80.2(2) . . . . ? O2 Cl1 O1 Cu1 90.3(2) . . . . ? O3 Cl1 O1 Cu1 -30.6(2) . . . . ? O4 Cl1 O1 Cu1 -150.34(18) . . . . ? N1 Cu1 O1 Cl1 -65.7(2) . . . . ? N2 Cu1 O1 Cl1 27.6(2) . . . . ? N3 Cu1 O1 Cl1 -158.0(2) . . . . ? N4 Cu1 O1 Cl1 121.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.477 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.082 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 787752' #TrackingRef 'cif-all-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H64 Cu6 N16 O12, 4(Cl O4)' _chemical_formula_sum 'C72 H64 Cl4 Cu6 N16 O28' _chemical_formula_weight 2124.49 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5171(16) _cell_length_b 22.228(3) _cell_length_c 18.7540(17) _cell_angle_alpha 90.00 _cell_angle_beta 131.760(5) _cell_angle_gamma 90.00 _cell_volume 4203.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1455 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 16.82 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 1.707 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8213 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22458 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8233 _reflns_number_gt 5780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0600P)^2^+1.9900P] 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 8233 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 -0.07458(6) 0.57364(2) 0.36730(4) 0.03833(16) Uani 1 1 d . . . Cu2 Cu 0.24956(5) 0.56162(2) 0.46864(4) 0.03693(15) Uani 1 1 d . . . Cu3 Cu 0.39267(5) 0.63685(2) 0.64938(4) 0.03463(15) Uani 1 1 d . . . C1 C 0.0941(5) 0.5451(2) 0.5678(3) 0.0400(11) Uani 1 1 d . . . C2 C -0.1488(6) 0.7014(2) 0.2910(4) 0.0564(15) Uani 1 1 d . . . H2 H -0.2141 0.6845 0.2309 0.068 Uiso 1 1 calc R . . C3 C -0.1352(5) 0.7628(2) 0.2974(4) 0.0530(14) Uani 1 1 d . . . H3 H -0.1916 0.7867 0.2432 0.064 Uiso 1 1 calc R . . C4 C -0.0386(5) 0.7878(2) 0.3836(4) 0.0503(13) Uani 1 1 d . . . H4 H -0.0270 0.8293 0.3902 0.060 Uiso 1 1 calc R . . C5 C 0.0433(5) 0.75014(19) 0.4624(3) 0.0392(11) Uani 1 1 d . . . H5 H 0.1127 0.7661 0.5224 0.047 Uiso 1 1 calc R . . C6 C 0.0213(4) 0.69001(19) 0.4513(3) 0.0326(10) Uani 1 1 d . . . C7 C 0.1207(5) 0.64546(19) 0.5303(3) 0.0382(11) Uani 1 1 d . . . C8 C 0.1714(5) 0.66298(19) 0.6299(3) 0.0361(10) Uani 1 1 d . . . C9 C 0.0960(5) 0.67783(19) 0.6504(3) 0.0349(10) Uani 1 1 d . . . H9 H 0.0047 0.6810 0.6008 0.042 Uiso 1 1 calc R . . C10 C 0.1476(5) 0.6880(2) 0.7387(4) 0.0438(12) Uani 1 1 d . . . H10 H 0.0943 0.7009 0.7505 0.053 Uiso 1 1 calc R . . C11 C 0.2764(5) 0.6795(2) 0.8102(4) 0.0450(12) Uani 1 1 d . . . H11 H 0.3127 0.6823 0.8731 0.054 Uiso 1 1 calc R . . C12 C 0.3584(5) 0.6661(2) 0.7905(3) 0.0428(11) Uani 1 1 d . . . H12 H 0.4498 0.6626 0.8399 0.051 Uiso 1 1 calc R . . C13 C -0.3164(5) 0.5724(2) 0.1630(3) 0.0433(11) Uani 1 1 d . . . H13 H -0.3605 0.5848 0.1828 0.052 Uiso 1 1 calc R . . C14 C -0.3876(5) 0.5619(2) 0.0685(4) 0.0504(13) Uani 1 1 d . . . H14 H -0.4793 0.5665 0.0249 0.061 Uiso 1 1 calc R . . C15 C -0.3257(5) 0.5447(2) 0.0378(3) 0.0487(13) Uani 1 1 d . . . H15 H -0.3731 0.5378 -0.0267 0.058 Uiso 1 1 calc R . . C16 C -0.1903(5) 0.53766(19) 0.1050(3) 0.0370(10) Uani 1 1 d . . . H16 H -0.1464 0.5248 0.0852 0.044 Uiso 1 1 calc R . . C17 C -0.1198(4) 0.54863(19) 0.1976(3) 0.0345(10) Uani 1 1 d . . . C18 C 0.0290(5) 0.5392(2) 0.2757(3) 0.0407(11) Uani 1 1 d . . . C19 C 0.0093(6) 0.4315(2) 0.2546(4) 0.0497(13) Uani 1 1 d . . . H19A H 0.0611 0.4189 0.3197 0.075 Uiso 1 1 calc R . . H19B H 0.0113 0.4008 0.2196 0.075 Uiso 1 1 calc R . . H19C H -0.0807 0.4382 0.2261 0.075 Uiso 1 1 calc R . . C20 C 0.1122(5) 0.5887(2) 0.2771(3) 0.0408(11) Uani 1 1 d . . . C21 C 0.0837(5) 0.6100(2) 0.1974(4) 0.0474(12) Uani 1 1 d . . . H21 H 0.0053 0.5987 0.1374 0.057 Uiso 1 1 calc R . . C22 C 0.1707(5) 0.6484(2) 0.2052(4) 0.0559(15) Uani 1 1 d . . . H22 H 0.1532 0.6629 0.1513 0.067 Uiso 1 1 calc R . . C23 C 0.2822(5) 0.6641(2) 0.2942(4) 0.0516(14) Uani 1 1 d . . . H23 H 0.3431 0.6899 0.3021 0.062 Uiso 1 1 calc R . . C24 C 0.3062(5) 0.6420(2) 0.3737(4) 0.0471(12) Uani 1 1 d . . . H24 H 0.3815 0.6541 0.4347 0.057 Uiso 1 1 calc R . . C25 C 0.6607(5) 0.6377(2) 0.8480(4) 0.0503(13) Uani 1 1 d . . . H25 H 0.6320 0.6692 0.8630 0.060 Uiso 1 1 calc R . . C26 C 0.7880(5) 0.6173(2) 0.9153(3) 0.0383(10) Uani 1 1 d . . . H26 H 0.8446 0.6351 0.9755 0.046 Uiso 1 1 calc R . . C27 C 0.8331(5) 0.5718(2) 0.8960(3) 0.0406(11) Uani 1 1 d . . . H27 H 0.9199 0.5581 0.9417 0.049 Uiso 1 1 calc R . . C28 C 0.7469(5) 0.5465(2) 0.8071(3) 0.0410(11) Uani 1 1 d . . . H28 H 0.7748 0.5148 0.7918 0.049 Uiso 1 1 calc R . . C29 C 0.6193(5) 0.5676(2) 0.7402(3) 0.0388(11) Uani 1 1 d . . . C30 C 0.5158(5) 0.5432(2) 0.6363(4) 0.0432(12) Uani 1 1 d . . . C31 C 0.6380(5) 0.5700(2) 0.5897(3) 0.0453(12) Uani 1 1 d . . . H31A H 0.5692 0.5880 0.5285 0.068 Uiso 1 1 calc R . . H31B H 0.7039 0.5528 0.5905 0.068 Uiso 1 1 calc R . . H31C H 0.6782 0.6001 0.6387 0.068 Uiso 1 1 calc R . . C32 C 0.4426(5) 0.4883(2) 0.6286(3) 0.0388(11) Uani 1 1 d . . . C33 C 0.5011(5) 0.4410(2) 0.6911(3) 0.0388(11) Uani 1 1 d . . . H33 H 0.5905 0.4418 0.7462 0.047 Uiso 1 1 calc R . . C34 C 0.4216(5) 0.3917(2) 0.6689(3) 0.0394(11) Uani 1 1 d . . . H34 H 0.4587 0.3585 0.7094 0.047 Uiso 1 1 calc R . . C35 C 0.2906(5) 0.3913(2) 0.5892(3) 0.0476(13) Uani 1 1 d . . . H35 H 0.2377 0.3577 0.5724 0.057 Uiso 1 1 calc R . . C36 C 0.2398(5) 0.4427(2) 0.5346(3) 0.0424(11) Uani 1 1 d . . . H36 H 0.1493 0.4442 0.4820 0.051 Uiso 1 1 calc R . . N1 N -0.0733(4) 0.66462(18) 0.3665(3) 0.0462(10) Uani 1 1 d . . . N2 N 0.3015(4) 0.65852(17) 0.6986(3) 0.0385(9) Uani 1 1 d . . . N3 N -0.1821(4) 0.56544(17) 0.2295(3) 0.0404(9) Uani 1 1 d . . . N4 N 0.2208(4) 0.60340(17) 0.3626(3) 0.0400(9) Uani 1 1 d . . . N5 N 0.5760(4) 0.61280(18) 0.7603(3) 0.0385(9) Uani 1 1 d . . . N6 N 0.3119(4) 0.48949(17) 0.5526(3) 0.0420(9) Uani 1 1 d . . . N7 N 0.1297(4) 0.50704(16) 0.6192(3) 0.0353(8) Uani 1 1 d . . . N8 N 0.0410(4) 0.58980(16) 0.5035(3) 0.0422(10) Uani 1 1 d . . . Cl1 Cl 0.28075(13) 0.88740(6) 0.54888(9) 0.0454(3) Uani 1 1 d . . . O1 O 0.0691(3) 0.53684(14) 0.3643(2) 0.0394(7) Uani 1 1 d . . . O2 O 0.2193(3) 0.63864(15) 0.5300(2) 0.0458(8) Uani 1 1 d . . . O3 O 0.4294(3) 0.59005(14) 0.5800(2) 0.0408(8) Uani 1 1 d . . . O4 O 0.0637(3) 0.48660(14) 0.2520(2) 0.0383(7) Uani 1 1 d . . . O5 O 0.5812(3) 0.52279(15) 0.6072(2) 0.0416(8) Uani 1 1 d . . . O6 O 0.4642(3) 0.73012(15) 0.6486(2) 0.0477(8) Uani 1 1 d . . . H6A H 0.5242 0.7375 0.6467 0.057 Uiso 1 1 d R . . H6B H 0.4307 0.7635 0.6453 0.057 Uiso 1 1 d R . . O7 O 0.3110(4) 0.84134(15) 0.6113(3) 0.0567(10) Uani 1 1 d . . . O8 O 0.1671(4) 0.91612(16) 0.5186(3) 0.0550(10) Uani 1 1 d . . . O9 O 0.3838(3) 0.92864(14) 0.5958(2) 0.0459(8) Uani 1 1 d . . . O10 O 0.2586(4) 0.86303(17) 0.4717(3) 0.0592(10) Uani 1 1 d . . . Cl2 Cl 0.6852(4) 0.75426(18) 0.0319(3) 0.0394(8) Uani 0.595(8) 1 d P A 1 O11 O 0.7731(10) 0.8044(5) 0.0753(7) 0.054(2) Uani 0.595(8) 1 d P A 1 O12 O 0.6127(11) 0.7547(4) -0.0680(8) 0.052(3) Uani 0.595(8) 1 d P A 1 O13 O 0.7625(9) 0.7011(3) 0.0741(5) 0.055(2) Uani 0.595(8) 1 d P A 1 O14 O 0.5975(6) 0.7578(3) 0.0494(5) 0.054(2) Uani 0.595(8) 1 d P A 1 Cl2' Cl 0.7180(7) 0.7488(3) 0.0210(4) 0.0549(16) Uani 0.405(8) 1 d P A 2 O11' O 0.7778(15) 0.7868(6) 0.1043(10) 0.051(3) Uani 0.405(8) 1 d P A 2 O12' O 0.5989(14) 0.7781(6) -0.0586(10) 0.042(3) Uani 0.405(8) 1 d P A 2 O13' O 0.6816(12) 0.6924(4) 0.0326(8) 0.048(3) Uani 0.405(8) 1 d P A 2 O14' O 0.8030(9) 0.7438(4) 0.0038(6) 0.054(3) Uani 0.405(8) 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 0.0334(3) 0.0266(3) 0.0421(3) -0.0029(2) 0.0198(3) 0.0034(2) Cu2 0.0286(3) 0.0352(3) 0.0390(3) 0.0003(2) 0.0191(3) -0.0016(2) Cu3 0.0307(3) 0.0400(3) 0.0314(3) -0.0071(2) 0.0199(3) -0.0011(2) C1 0.032(2) 0.037(3) 0.041(3) 0.007(2) 0.021(2) 0.007(2) C2 0.048(3) 0.033(3) 0.054(3) 0.005(2) 0.020(3) 0.012(2) C3 0.042(3) 0.035(3) 0.046(3) 0.001(2) 0.015(3) 0.009(2) C4 0.038(3) 0.036(3) 0.045(3) 0.008(2) 0.015(2) -0.005(2) C5 0.035(2) 0.029(2) 0.044(3) 0.0027(19) 0.022(2) 0.0018(19) C6 0.034(2) 0.028(2) 0.045(3) -0.0024(19) 0.030(2) 0.0003(18) C7 0.031(2) 0.027(2) 0.041(3) -0.0057(19) 0.017(2) 0.0006(18) C8 0.036(3) 0.026(2) 0.045(3) -0.0029(19) 0.026(2) -0.0092(18) C9 0.031(2) 0.030(2) 0.037(3) 0.0095(18) 0.019(2) -0.0013(18) C10 0.046(3) 0.033(2) 0.047(3) -0.001(2) 0.029(3) 0.006(2) C11 0.043(3) 0.050(3) 0.038(3) -0.011(2) 0.026(2) 0.002(2) C12 0.045(3) 0.050(3) 0.039(3) -0.008(2) 0.030(3) -0.006(2) C13 0.036(3) 0.049(3) 0.040(3) 0.004(2) 0.023(2) 0.010(2) C14 0.035(3) 0.046(3) 0.045(3) -0.019(2) 0.016(2) -0.005(2) C15 0.045(3) 0.045(3) 0.030(2) -0.013(2) 0.014(2) -0.003(2) C16 0.041(3) 0.029(2) 0.038(3) -0.0040(18) 0.025(2) -0.0100(19) C17 0.031(2) 0.029(2) 0.033(2) 0.0066(18) 0.017(2) 0.0010(18) C18 0.031(3) 0.036(3) 0.041(3) 0.004(2) 0.018(2) 0.0056(19) C19 0.051(3) 0.041(3) 0.044(3) -0.006(2) 0.026(3) -0.004(2) C20 0.034(3) 0.038(3) 0.041(3) 0.000(2) 0.021(2) 0.001(2) C21 0.047(3) 0.038(3) 0.039(3) -0.001(2) 0.020(3) -0.009(2) C22 0.041(3) 0.050(3) 0.040(3) 0.023(2) 0.012(3) -0.003(2) C23 0.046(3) 0.047(3) 0.046(3) 0.004(2) 0.024(3) -0.015(2) C24 0.040(3) 0.041(3) 0.037(3) 0.005(2) 0.016(2) -0.007(2) C25 0.033(3) 0.046(3) 0.047(3) -0.015(2) 0.016(2) 0.000(2) C26 0.033(3) 0.051(3) 0.032(2) 0.000(2) 0.022(2) -0.004(2) C27 0.031(2) 0.038(3) 0.037(3) 0.008(2) 0.016(2) 0.003(2) C28 0.039(3) 0.043(3) 0.033(2) 0.007(2) 0.021(2) 0.010(2) C29 0.030(2) 0.048(3) 0.035(2) -0.003(2) 0.021(2) -0.001(2) C30 0.032(3) 0.039(3) 0.044(3) -0.009(2) 0.020(2) 0.002(2) C31 0.032(3) 0.043(3) 0.039(3) 0.006(2) 0.014(2) 0.009(2) C32 0.038(3) 0.042(3) 0.024(2) -0.0026(18) 0.016(2) 0.002(2) C33 0.030(2) 0.048(3) 0.035(2) -0.003(2) 0.021(2) -0.001(2) C34 0.039(3) 0.037(3) 0.045(3) 0.018(2) 0.029(2) 0.019(2) C35 0.049(3) 0.040(3) 0.037(3) 0.002(2) 0.022(3) -0.010(2) C36 0.035(3) 0.033(2) 0.043(3) 0.003(2) 0.020(2) 0.008(2) N1 0.039(2) 0.034(2) 0.043(2) 0.0011(18) 0.018(2) 0.0000(18) N2 0.035(2) 0.037(2) 0.039(2) -0.0102(16) 0.023(2) -0.0005(16) N3 0.034(2) 0.039(2) 0.039(2) 0.0059(17) 0.0202(19) 0.0088(17) N4 0.039(2) 0.034(2) 0.036(2) 0.0045(16) 0.020(2) 0.0000(17) N5 0.035(2) 0.043(2) 0.031(2) 0.0030(16) 0.0195(19) 0.0038(17) N6 0.035(2) 0.038(2) 0.036(2) 0.0070(17) 0.0165(19) 0.0049(17) N7 0.032(2) 0.032(2) 0.038(2) 0.0051(17) 0.0217(18) 0.0130(16) N8 0.034(2) 0.028(2) 0.039(2) 0.0020(16) 0.0137(19) 0.0040(16) Cl1 0.0420(7) 0.0463(7) 0.0455(7) 0.0024(5) 0.0282(6) -0.0042(5) O1 0.0262(16) 0.0363(17) 0.0378(18) -0.0030(13) 0.0138(15) -0.0025(13) O2 0.0332(18) 0.0451(19) 0.0386(18) -0.0067(15) 0.0154(16) 0.0023(15) O3 0.0351(18) 0.0404(18) 0.0342(17) -0.0099(14) 0.0178(15) 0.0014(14) O4 0.0290(17) 0.0403(18) 0.0299(16) -0.0014(13) 0.0130(14) -0.0021(13) O5 0.0288(17) 0.048(2) 0.0370(18) -0.0072(14) 0.0175(15) -0.0003(14) O6 0.0396(19) 0.0398(18) 0.050(2) -0.0063(15) 0.0243(17) -0.0033(15) O7 0.041(2) 0.0386(19) 0.046(2) 0.0049(15) 0.0109(18) -0.0100(16) O8 0.044(2) 0.047(2) 0.053(2) 0.0168(17) 0.0229(19) 0.0097(16) O9 0.0409(19) 0.0363(18) 0.0419(19) 0.0125(14) 0.0199(17) 0.0068(15) O10 0.049(2) 0.053(2) 0.046(2) -0.0066(17) 0.0194(19) 0.0051(18) Cl2 0.0397(17) 0.0383(13) 0.0423(15) -0.0107(10) 0.0282(13) -0.0092(11) O11 0.052(4) 0.053(6) 0.039(5) 0.000(4) 0.023(4) -0.023(4) O12 0.053(5) 0.045(6) 0.040(4) -0.009(4) 0.023(4) 0.005(4) O13 0.056(5) 0.048(4) 0.037(4) -0.011(3) 0.021(4) 0.010(4) O14 0.047(4) 0.057(4) 0.061(4) -0.014(3) 0.037(4) -0.010(3) Cl2' 0.054(4) 0.052(3) 0.040(2) -0.0045(18) 0.023(2) -0.017(2) O11' 0.049(6) 0.044(8) 0.041(8) -0.004(5) 0.022(6) -0.019(5) O12' 0.040(6) 0.045(8) 0.039(6) -0.009(6) 0.026(5) -0.022(6) O13' 0.051(7) 0.044(5) 0.028(5) -0.013(4) 0.017(5) -0.013(5) O14' 0.039(5) 0.047(5) 0.046(5) -0.013(4) 0.016(5) -0.013(4) _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 N8 1.944(4) . ? Cu1 N3 1.955(4) . ? Cu1 N7 2.021(4) 3_566 ? Cu1 N1 2.022(4) . ? Cu1 O1 2.143(3) . ? Cu2 O1 1.930(3) . ? Cu2 O3 1.976(3) . ? Cu2 N4 1.984(4) . ? Cu2 N6 1.998(4) . ? Cu2 O2 2.247(3) . ? Cu2 Cu3 3.0485(8) . ? Cu3 O2 1.876(3) . ? Cu3 O3 1.970(3) . ? Cu3 N5 1.972(4) . ? Cu3 N2 2.029(4) . ? Cu3 O6 2.292(3) . ? C1 N7 1.122(6) . ? C1 N8 1.343(6) . ? C2 N1 1.338(6) . ? C2 C3 1.371(7) . ? C2 H2 0.9300 . ? C3 C4 1.348(7) . ? C3 H3 0.9300 . ? C4 C5 1.390(6) . ? C4 H4 0.9300 . ? C5 C6 1.355(6) . ? C5 H5 0.9300 . ? C6 N1 1.332(6) . ? C6 C7 1.526(6) . ? C7 O2 1.345(6) . ? C7 N8 1.492(6) . ? C7 C8 1.551(7) . ? C8 N2 1.321(6) . ? C8 C9 1.349(7) . ? C9 C10 1.319(7) . ? C9 H9 0.9300 . ? C10 C11 1.325(7) . ? C10 H10 0.9300 . ? C11 C12 1.415(7) . ? C11 H11 0.9300 . ? C12 N2 1.352(6) . ? C12 H12 0.9300 . ? C13 C14 1.361(7) . ? C13 N3 1.363(6) . ? C13 H13 0.9300 . ? C14 C15 1.348(8) . ? C14 H14 0.9300 . ? C15 C16 1.375(7) . ? C15 H15 0.9300 . ? C16 C17 1.334(6) . ? C16 H16 0.9300 . ? C17 N3 1.370(6) . ? C17 C18 1.520(6) . ? C18 O1 1.363(6) . ? C18 O4 1.436(6) . ? C18 C20 1.560(7) . ? C19 O4 1.446(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.303(6) . ? C20 C21 1.357(7) . ? C21 C22 1.379(7) . ? C21 H21 0.9300 . ? C22 C23 1.353(7) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 H23 0.9300 . ? C24 N4 1.339(6) . ? C24 H24 0.9300 . ? C25 N5 1.347(6) . ? C25 C26 1.367(7) . ? C25 H25 0.9300 . ? C26 C27 1.347(7) . ? C26 H26 0.9300 . ? C27 C28 1.366(7) . ? C27 H27 0.9300 . ? C28 C29 1.375(6) . ? C28 H28 0.9300 . ? C29 N5 1.337(6) . ? C29 C30 1.555(7) . ? C30 O3 1.387(6) . ? C30 O5 1.388(6) . ? C30 C32 1.515(7) . ? C31 O5 1.460(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N6 1.341(6) . ? C32 C33 1.366(6) . ? C33 C34 1.392(7) . ? C33 H33 0.9300 . ? C34 C35 1.358(7) . ? C34 H34 0.9300 . ? C35 C36 1.374(7) . ? C35 H35 0.9300 . ? C36 N6 1.307(6) . ? C36 H36 0.9300 . ? N7 Cu1 2.021(4) 3_566 ? Cl1 O10 1.378(4) . ? Cl1 O9 1.386(4) . ? Cl1 O8 1.389(4) . ? Cl1 O7 1.395(4) . ? O6 H6A 0.8499 . ? O6 H6B 0.8499 . ? Cl2 O13 1.418(8) . ? Cl2 O12 1.423(12) . ? Cl2 O11 1.424(11) . ? Cl2 O14 1.427(7) . ? Cl2' O14' 1.390(14) . ? Cl2' O13' 1.414(12) . ? Cl2' O12' 1.430(17) . ? Cl2' O11' 1.457(17) . ? 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 N8 Cu1 N3 173.55(17) . . ? N8 Cu1 N7 92.30(16) . 3_566 ? N3 Cu1 N7 94.08(16) . 3_566 ? N8 Cu1 N1 79.73(16) . . ? N3 Cu1 N1 94.91(16) . . ? N7 Cu1 N1 153.37(17) 3_566 . ? N8 Cu1 O1 98.98(15) . . ? N3 Cu1 O1 79.55(14) . . ? N7 Cu1 O1 94.63(13) 3_566 . ? N1 Cu1 O1 111.64(16) . . ? O1 Cu2 O3 175.53(14) . . ? O1 Cu2 N4 81.14(15) . . ? O3 Cu2 N4 101.02(15) . . ? O1 Cu2 N6 98.91(15) . . ? O3 Cu2 N6 81.23(15) . . ? N4 Cu2 N6 149.72(17) . . ? O1 Cu2 O2 101.45(13) . . ? O3 Cu2 O2 74.37(12) . . ? N4 Cu2 O2 100.10(15) . . ? N6 Cu2 O2 109.44(15) . . ? O1 Cu2 Cu3 136.18(10) . . ? O3 Cu2 Cu3 39.36(9) . . ? N4 Cu2 Cu3 114.40(12) . . ? N6 Cu2 Cu3 86.64(12) . . ? O2 Cu2 Cu3 37.80(8) . . ? O2 Cu3 O3 83.47(14) . . ? O2 Cu3 N5 163.42(15) . . ? O3 Cu3 N5 82.04(15) . . ? O2 Cu3 N2 83.32(15) . . ? O3 Cu3 N2 157.24(15) . . ? N5 Cu3 N2 107.56(16) . . ? O2 Cu3 O6 99.78(14) . . ? O3 Cu3 O6 100.39(14) . . ? N5 Cu3 O6 90.74(15) . . ? N2 Cu3 O6 100.06(15) . . ? O2 Cu3 Cu2 47.24(10) . . ? O3 Cu3 Cu2 39.50(9) . . ? N5 Cu3 Cu2 116.45(12) . . ? N2 Cu3 Cu2 120.53(11) . . ? O6 Cu3 Cu2 116.55(9) . . ? N7 C1 N8 175.0(5) . . ? N1 C2 C3 123.5(5) . . ? N1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? C4 C3 C2 118.8(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 118.5(5) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 119.5(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 122.7(4) . . ? N1 C6 C7 114.1(4) . . ? C5 C6 C7 121.9(4) . . ? O2 C7 N8 113.7(4) . . ? O2 C7 C6 107.6(4) . . ? N8 C7 C6 103.9(4) . . ? O2 C7 C8 112.9(4) . . ? N8 C7 C8 104.7(4) . . ? C6 C7 C8 113.8(4) . . ? N2 C8 C9 120.5(4) . . ? N2 C8 C7 112.9(4) . . ? C9 C8 C7 126.4(4) . . ? C10 C9 C8 122.1(5) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119.1(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? N2 C12 C11 118.7(5) . . ? N2 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 N3 121.9(5) . . ? C14 C13 H13 119.1 . . ? N3 C13 H13 119.1 . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 117.9(5) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 122.1(5) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 N3 120.3(4) . . ? C16 C17 C18 124.6(4) . . ? N3 C17 C18 114.9(4) . . ? O1 C18 O4 113.5(4) . . ? O1 C18 C17 112.2(4) . . ? O4 C18 C17 108.0(4) . . ? O1 C18 C20 108.0(4) . . ? O4 C18 C20 101.5(4) . . ? C17 C18 C20 113.3(4) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 C21 121.9(5) . . ? N4 C20 C18 114.0(4) . . ? C21 C20 C18 123.7(4) . . ? C20 C21 C22 120.2(5) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 117.5(5) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 C23 C24 120.3(5) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? N4 C24 C23 120.0(5) . . ? N4 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? N5 C25 C26 121.0(5) . . ? N5 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 121.2(5) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 117.8(5) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? N5 C29 C28 121.2(4) . . ? N5 C29 C30 114.8(4) . . ? C28 C29 C30 124.0(4) . . ? O3 C30 O5 112.3(4) . . ? O3 C30 C32 111.5(4) . . ? O5 C30 C32 104.2(4) . . ? O3 C30 C29 106.9(4) . . ? O5 C30 C29 109.3(4) . . ? C32 C30 C29 112.7(4) . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C33 121.8(4) . . ? N6 C32 C30 113.6(4) . . ? C33 C32 C30 124.6(4) . . ? C32 C33 C34 117.3(4) . . ? C32 C33 H33 121.3 . . ? C34 C33 H33 121.3 . . ? C35 C34 C33 121.0(4) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 116.9(5) . . ? C34 C35 H35 121.6 . . ? C36 C35 H35 121.6 . . ? N6 C36 C35 123.6(5) . . ? N6 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C6 N1 C2 117.0(4) . . ? C6 N1 Cu1 114.9(3) . . ? C2 N1 Cu1 127.9(4) . . ? C8 N2 C12 119.5(4) . . ? C8 N2 Cu3 113.1(3) . . ? C12 N2 Cu3 127.4(3) . . ? C13 N3 C17 117.6(4) . . ? C13 N3 Cu1 124.3(3) . . ? C17 N3 Cu1 118.1(3) . . ? C20 N4 C24 120.0(4) . . ? C20 N4 Cu2 115.0(3) . . ? C24 N4 Cu2 124.9(3) . . ? C29 N5 C25 118.6(4) . . ? C29 N5 Cu3 112.6(3) . . ? C25 N5 Cu3 128.7(3) . . ? C36 N6 C32 119.1(4) . . ? C36 N6 Cu2 125.8(3) . . ? C32 N6 Cu2 114.7(3) . . ? C1 N7 Cu1 142.5(4) . 3_566 ? C1 N8 C7 118.5(4) . . ? C1 N8 Cu1 121.6(3) . . ? C7 N8 Cu1 111.3(3) . . ? O10 Cl1 O9 110.6(3) . . ? O10 Cl1 O8 110.1(2) . . ? O9 Cl1 O8 109.0(2) . . ? O10 Cl1 O7 109.2(2) . . ? O9 Cl1 O7 110.1(2) . . ? O8 Cl1 O7 107.9(2) . . ? C18 O1 Cu2 115.7(3) . . ? C18 O1 Cu1 112.7(3) . . ? Cu2 O1 Cu1 114.85(15) . . ? C7 O2 Cu3 116.8(3) . . ? C7 O2 Cu2 127.3(3) . . ? Cu3 O2 Cu2 94.96(14) . . ? C30 O3 Cu3 110.4(3) . . ? C30 O3 Cu2 112.6(3) . . ? Cu3 O3 Cu2 101.14(15) . . ? C18 O4 C19 113.7(4) . . ? C30 O5 C31 114.9(4) . . ? Cu3 O6 H6A 126.4 . . ? Cu3 O6 H6B 125.7 . . ? H6A O6 H6B 107.7 . . ? O13 Cl2 O12 110.2(5) . . ? O13 Cl2 O11 107.9(6) . . ? O12 Cl2 O11 109.2(6) . . ? O13 Cl2 O14 109.6(6) . . ? O12 Cl2 O14 110.7(6) . . ? O11 Cl2 O14 109.2(6) . . ? O14' Cl2' O13' 112.9(9) . . ? O14' Cl2' O12' 108.8(9) . . ? O13' Cl2' O12' 107.5(9) . . ? O14' Cl2' O11' 109.9(8) . . ? O13' Cl2' O11' 110.5(8) . . ? O12' Cl2' O11' 106.9(10) . . ? 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 O1 Cu2 Cu3 O2 -28.9(2) . . . . ? O3 Cu2 Cu3 O2 151.5(2) . . . . ? N4 Cu2 Cu3 O2 74.3(2) . . . . ? N6 Cu2 Cu3 O2 -128.3(2) . . . . ? O1 Cu2 Cu3 O3 179.6(2) . . . . ? N4 Cu2 Cu3 O3 -77.2(2) . . . . ? N6 Cu2 Cu3 O3 80.3(2) . . . . ? O2 Cu2 Cu3 O3 -151.5(2) . . . . ? O1 Cu2 Cu3 N5 147.48(19) . . . . ? O3 Cu2 Cu3 N5 -32.2(2) . . . . ? N4 Cu2 Cu3 N5 -109.32(18) . . . . ? N6 Cu2 Cu3 N5 48.10(18) . . . . ? O2 Cu2 Cu3 N5 176.4(2) . . . . ? O1 Cu2 Cu3 N2 14.3(2) . . . . ? O3 Cu2 Cu3 N2 -165.4(2) . . . . ? N4 Cu2 Cu3 N2 117.47(19) . . . . ? N6 Cu2 Cu3 N2 -85.12(18) . . . . ? O2 Cu2 Cu3 N2 43.2(2) . . . . ? O1 Cu2 Cu3 O6 -107.17(17) . . . . ? O3 Cu2 Cu3 O6 73.20(19) . . . . ? N4 Cu2 Cu3 O6 -3.97(17) . . . . ? N6 Cu2 Cu3 O6 153.45(16) . . . . ? O2 Cu2 Cu3 O6 -78.27(18) . . . . ? N1 C2 C3 C4 1.8(10) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? C3 C4 C5 C6 -2.2(8) . . . . ? C4 C5 C6 N1 2.7(7) . . . . ? C4 C5 C6 C7 169.2(5) . . . . ? N1 C6 C7 O2 89.3(5) . . . . ? C5 C6 C7 O2 -78.3(5) . . . . ? N1 C6 C7 N8 -31.5(5) . . . . ? C5 C6 C7 N8 160.9(4) . . . . ? N1 C6 C7 C8 -144.8(4) . . . . ? C5 C6 C7 C8 47.7(6) . . . . ? O2 C7 C8 N2 -10.2(5) . . . . ? N8 C7 C8 N2 114.0(4) . . . . ? C6 C7 C8 N2 -133.3(4) . . . . ? O2 C7 C8 C9 173.9(4) . . . . ? N8 C7 C8 C9 -61.9(5) . . . . ? C6 C7 C8 C9 50.8(6) . . . . ? N2 C8 C9 C10 -0.5(7) . . . . ? C7 C8 C9 C10 175.1(4) . . . . ? C8 C9 C10 C11 -4.6(7) . . . . ? C9 C10 C11 C12 6.8(8) . . . . ? C10 C11 C12 N2 -4.2(7) . . . . ? N3 C13 C14 C15 -0.9(8) . . . . ? C13 C14 C15 C16 0.8(8) . . . . ? C14 C15 C16 C17 -1.6(7) . . . . ? C15 C16 C17 N3 2.4(7) . . . . ? C15 C16 C17 C18 177.3(4) . . . . ? C16 C17 C18 O1 -162.1(4) . . . . ? N3 C17 C18 O1 13.0(5) . . . . ? C16 C17 C18 O4 -36.4(6) . . . . ? N3 C17 C18 O4 138.8(4) . . . . ? C16 C17 C18 C20 75.2(6) . . . . ? N3 C17 C18 C20 -109.6(5) . . . . ? O1 C18 C20 N4 18.5(5) . . . . ? O4 C18 C20 N4 -101.0(4) . . . . ? C17 C18 C20 N4 143.4(4) . . . . ? O1 C18 C20 C21 -168.7(5) . . . . ? O4 C18 C20 C21 71.8(6) . . . . ? C17 C18 C20 C21 -43.8(7) . . . . ? N4 C20 C21 C22 0.0(8) . . . . ? C18 C20 C21 C22 -172.2(5) . . . . ? C20 C21 C22 C23 -1.0(9) . . . . ? C21 C22 C23 C24 -0.1(9) . . . . ? C22 C23 C24 N4 2.2(9) . . . . ? N5 C25 C26 C27 0.2(8) . . . . ? C25 C26 C27 C28 -0.4(7) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? C27 C28 C29 N5 -0.5(7) . . . . ? C27 C28 C29 C30 177.8(5) . . . . ? N5 C29 C30 O3 26.7(6) . . . . ? C28 C29 C30 O3 -151.7(5) . . . . ? N5 C29 C30 O5 148.5(4) . . . . ? C28 C29 C30 O5 -30.0(7) . . . . ? N5 C29 C30 C32 -96.1(5) . . . . ? C28 C29 C30 C32 85.4(6) . . . . ? O3 C30 C32 N6 16.8(6) . . . . ? O5 C30 C32 N6 -104.6(4) . . . . ? C29 C30 C32 N6 137.0(4) . . . . ? O3 C30 C32 C33 -163.8(4) . . . . ? O5 C30 C32 C33 74.8(5) . . . . ? C29 C30 C32 C33 -43.6(6) . . . . ? N6 C32 C33 C34 4.9(7) . . . . ? C30 C32 C33 C34 -174.4(4) . . . . ? C32 C33 C34 C35 -1.2(7) . . . . ? C33 C34 C35 C36 -3.1(8) . . . . ? C34 C35 C36 N6 4.0(8) . . . . ? C5 C6 N1 C2 -0.8(7) . . . . ? C7 C6 N1 C2 -168.3(5) . . . . ? C5 C6 N1 Cu1 174.6(4) . . . . ? C7 C6 N1 Cu1 7.1(5) . . . . ? C3 C2 N1 C6 -1.5(9) . . . . ? C3 C2 N1 Cu1 -176.1(5) . . . . ? N8 Cu1 N1 C6 14.4(4) . . . . ? N3 Cu1 N1 C6 -161.9(4) . . . . ? N7 Cu1 N1 C6 88.8(5) 3_566 . . . ? O1 Cu1 N1 C6 -81.2(4) . . . . ? N8 Cu1 N1 C2 -170.8(5) . . . . ? N3 Cu1 N1 C2 12.8(5) . . . . ? N7 Cu1 N1 C2 -96.5(6) 3_566 . . . ? O1 Cu1 N1 C2 93.5(5) . . . . ? C9 C8 N2 C12 3.2(6) . . . . ? C7 C8 N2 C12 -173.0(4) . . . . ? C9 C8 N2 Cu3 -179.2(3) . . . . ? C7 C8 N2 Cu3 4.7(4) . . . . ? C11 C12 N2 C8 -0.9(7) . . . . ? C11 C12 N2 Cu3 -178.1(4) . . . . ? O2 Cu3 N2 C8 0.8(3) . . . . ? O3 Cu3 N2 C8 -54.1(5) . . . . ? N5 Cu3 N2 C8 -166.4(3) . . . . ? O6 Cu3 N2 C8 99.6(3) . . . . ? Cu2 Cu3 N2 C8 -29.6(3) . . . . ? O2 Cu3 N2 C12 178.2(4) . . . . ? O3 Cu3 N2 C12 123.3(4) . . . . ? N5 Cu3 N2 C12 11.0(4) . . . . ? O6 Cu3 N2 C12 -83.0(4) . . . . ? Cu2 Cu3 N2 C12 147.8(4) . . . . ? C14 C13 N3 C17 1.5(7) . . . . ? C14 C13 N3 Cu1 -175.0(4) . . . . ? C16 C17 N3 C13 -2.3(6) . . . . ? C18 C17 N3 C13 -177.7(4) . . . . ? C16 C17 N3 Cu1 174.5(3) . . . . ? C18 C17 N3 Cu1 -0.9(5) . . . . ? N8 Cu1 N3 C13 -112.8(15) . . . . ? N7 Cu1 N3 C13 75.8(4) 3_566 . . . ? N1 Cu1 N3 C13 -79.1(4) . . . . ? O1 Cu1 N3 C13 169.8(4) . . . . ? N8 Cu1 N3 C17 70.6(16) . . . . ? N7 Cu1 N3 C17 -100.7(3) 3_566 . . . ? N1 Cu1 N3 C17 104.4(3) . . . . ? O1 Cu1 N3 C17 -6.8(3) . . . . ? C21 C20 N4 C24 2.1(8) . . . . ? C18 C20 N4 C24 175.1(4) . . . . ? C21 C20 N4 Cu2 -175.0(4) . . . . ? C18 C20 N4 Cu2 -2.0(5) . . . . ? C23 C24 N4 C20 -3.2(8) . . . . ? C23 C24 N4 Cu2 173.6(4) . . . . ? O1 Cu2 N4 C20 -10.0(3) . . . . ? O3 Cu2 N4 C20 174.0(3) . . . . ? N6 Cu2 N4 C20 82.6(5) . . . . ? O2 Cu2 N4 C20 -110.1(4) . . . . ? Cu3 Cu2 N4 C20 -146.9(3) . . . . ? O1 Cu2 N4 C24 173.1(4) . . . . ? O3 Cu2 N4 C24 -2.9(4) . . . . ? N6 Cu2 N4 C24 -94.4(5) . . . . ? O2 Cu2 N4 C24 72.9(4) . . . . ? Cu3 Cu2 N4 C24 36.1(4) . . . . ? C28 C29 N5 C25 0.3(7) . . . . ? C30 C29 N5 C25 -178.2(5) . . . . ? C28 C29 N5 Cu3 176.9(4) . . . . ? C30 C29 N5 Cu3 -1.7(5) . . . . ? C26 C25 N5 C29 -0.1(8) . . . . ? C26 C25 N5 Cu3 -176.1(4) . . . . ? O2 Cu3 N5 C29 13.5(8) . . . . ? O3 Cu3 N5 C29 -15.8(3) . . . . ? N2 Cu3 N5 C29 143.0(3) . . . . ? O6 Cu3 N5 C29 -116.2(3) . . . . ? Cu2 Cu3 N5 C29 4.2(4) . . . . ? O2 Cu3 N5 C25 -170.3(5) . . . . ? O3 Cu3 N5 C25 160.4(5) . . . . ? N2 Cu3 N5 C25 -40.8(5) . . . . ? O6 Cu3 N5 C25 60.0(5) . . . . ? Cu2 Cu3 N5 C25 -179.7(4) . . . . ? C35 C36 N6 C32 -0.4(8) . . . . ? C35 C36 N6 Cu2 172.4(4) . . . . ? C33 C32 N6 C36 -4.2(7) . . . . ? C30 C32 N6 C36 175.2(4) . . . . ? C33 C32 N6 Cu2 -177.9(4) . . . . ? C30 C32 N6 Cu2 1.5(5) . . . . ? O1 Cu2 N6 C36 -1.5(4) . . . . ? O3 Cu2 N6 C36 174.0(4) . . . . ? N4 Cu2 N6 C36 -89.2(5) . . . . ? O2 Cu2 N6 C36 104.1(4) . . . . ? Cu3 Cu2 N6 C36 134.8(4) . . . . ? O1 Cu2 N6 C32 171.7(3) . . . . ? O3 Cu2 N6 C32 -12.9(3) . . . . ? N4 Cu2 N6 C32 84.0(5) . . . . ? O2 Cu2 N6 C32 -82.8(3) . . . . ? Cu3 Cu2 N6 C32 -52.1(3) . . . . ? N8 C1 N7 Cu1 36(7) . . . 3_566 ? N7 C1 N8 C7 142(6) . . . . ? N7 C1 N8 Cu1 -73(6) . . . . ? O2 C7 N8 C1 74.8(6) . . . . ? C6 C7 N8 C1 -168.5(4) . . . . ? C8 C7 N8 C1 -48.9(5) . . . . ? O2 C7 N8 Cu1 -73.6(4) . . . . ? C6 C7 N8 Cu1 43.1(4) . . . . ? C8 C7 N8 Cu1 162.7(3) . . . . ? N3 Cu1 N8 C1 -145.9(13) . . . . ? N7 Cu1 N8 C1 25.5(4) 3_566 . . . ? N1 Cu1 N8 C1 179.9(4) . . . . ? O1 Cu1 N8 C1 -69.6(4) . . . . ? N3 Cu1 N8 C7 1.4(16) . . . . ? N7 Cu1 N8 C7 172.7(3) 3_566 . . . ? N1 Cu1 N8 C7 -32.9(3) . . . . ? O1 Cu1 N8 C7 77.7(3) . . . . ? O4 C18 O1 Cu2 84.5(4) . . . . ? C17 C18 O1 Cu2 -152.8(3) . . . . ? C20 C18 O1 Cu2 -27.2(4) . . . . ? O4 C18 O1 Cu1 -140.6(3) . . . . ? C17 C18 O1 Cu1 -17.9(4) . . . . ? C20 C18 O1 Cu1 107.7(3) . . . . ? O3 Cu2 O1 C18 141.1(17) . . . . ? N4 Cu2 O1 C18 21.9(3) . . . . ? N6 Cu2 O1 C18 -127.5(3) . . . . ? O2 Cu2 O1 C18 120.5(3) . . . . ? Cu3 Cu2 O1 C18 138.1(3) . . . . ? O3 Cu2 O1 Cu1 7.2(19) . . . . ? N4 Cu2 O1 Cu1 -112.04(19) . . . . ? N6 Cu2 O1 Cu1 98.62(18) . . . . ? O2 Cu2 O1 Cu1 -13.44(19) . . . . ? Cu3 Cu2 O1 Cu1 4.2(2) . . . . ? N8 Cu1 O1 C18 -159.5(3) . . . . ? N3 Cu1 O1 C18 14.1(3) . . . . ? N7 Cu1 O1 C18 107.4(3) 3_566 . . . ? N1 Cu1 O1 C18 -77.1(3) . . . . ? N8 Cu1 O1 Cu2 -24.2(2) . . . . ? N3 Cu1 O1 Cu2 149.4(2) . . . . ? N7 Cu1 O1 Cu2 -117.30(18) 3_566 . . . ? N1 Cu1 O1 Cu2 58.2(2) . . . . ? N8 C7 O2 Cu3 -107.9(4) . . . . ? C6 C7 O2 Cu3 137.6(3) . . . . ? C8 C7 O2 Cu3 11.2(5) . . . . ? N8 C7 O2 Cu2 12.6(6) . . . . ? C6 C7 O2 Cu2 -101.9(4) . . . . ? C8 C7 O2 Cu2 131.7(3) . . . . ? O3 Cu3 O2 C7 154.4(3) . . . . ? N5 Cu3 O2 C7 125.1(5) . . . . ? N2 Cu3 O2 C7 -7.1(3) . . . . ? O6 Cu3 O2 C7 -106.2(3) . . . . ? Cu2 Cu3 O2 C7 136.6(4) . . . . ? O3 Cu3 O2 Cu2 17.81(14) . . . . ? N5 Cu3 O2 Cu2 -11.4(6) . . . . ? N2 Cu3 O2 Cu2 -143.61(16) . . . . ? O6 Cu3 O2 Cu2 117.28(13) . . . . ? O1 Cu2 O2 C7 30.6(4) . . . . ? O3 Cu2 O2 C7 -147.8(4) . . . . ? N4 Cu2 O2 C7 113.5(4) . . . . ? N6 Cu2 O2 C7 -73.3(4) . . . . ? Cu3 Cu2 O2 C7 -129.5(4) . . . . ? O1 Cu2 O2 Cu3 160.03(14) . . . . ? O3 Cu2 O2 Cu3 -18.34(14) . . . . ? N4 Cu2 O2 Cu3 -117.07(17) . . . . ? N6 Cu2 O2 Cu3 56.20(19) . . . . ? O5 C30 O3 Cu3 -158.4(3) . . . . ? C32 C30 O3 Cu3 85.1(4) . . . . ? C29 C30 O3 Cu3 -38.6(4) . . . . ? O5 C30 O3 Cu2 89.4(4) . . . . ? C32 C30 O3 Cu2 -27.1(5) . . . . ? C29 C30 O3 Cu2 -150.8(3) . . . . ? O2 Cu3 O3 C30 -140.0(3) . . . . ? N5 Cu3 O3 C30 31.9(3) . . . . ? N2 Cu3 O3 C30 -85.2(5) . . . . ? O6 Cu3 O3 C30 121.2(3) . . . . ? Cu2 Cu3 O3 C30 -119.4(3) . . . . ? O2 Cu3 O3 Cu2 -20.67(16) . . . . ? N5 Cu3 O3 Cu2 151.24(18) . . . . ? N2 Cu3 O3 Cu2 34.2(4) . . . . ? O6 Cu3 O3 Cu2 -119.47(14) . . . . ? O1 Cu2 O3 C30 114.5(17) . . . . ? N4 Cu2 O3 C30 -127.0(3) . . . . ? N6 Cu2 O3 C30 22.4(3) . . . . ? O2 Cu2 O3 C30 135.5(3) . . . . ? Cu3 Cu2 O3 C30 117.8(4) . . . . ? O1 Cu2 O3 Cu3 -3.3(19) . . . . ? N4 Cu2 O3 Cu3 115.23(17) . . . . ? N6 Cu2 O3 Cu3 -95.43(18) . . . . ? O2 Cu2 O3 Cu3 17.70(14) . . . . ? O1 C18 O4 C19 58.8(5) . . . . ? C17 C18 O4 C19 -66.2(5) . . . . ? C20 C18 O4 C19 174.4(4) . . . . ? O3 C30 O5 C31 47.3(5) . . . . ? C32 C30 O5 C31 168.2(3) . . . . ? C29 C30 O5 C31 -71.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.842 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.077 #===END data_cc _database_code_depnum_ccdc_archive 'CCDC 788548' #TrackingRef '5-Co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Co N6 O3, Cl O4, 2(H2 O)' _chemical_formula_sum 'C24 H24 Cl Co N6 O9' _chemical_formula_weight 634.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.1311(16) _cell_length_b 11.9402(15) _cell_length_c 16.985(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.938(2) _cell_angle_gamma 90.00 _cell_volume 2614.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4692 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.23 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8208 _exptl_absorpt_correction_T_max 0.8660 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6648 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4231 _reflns_number_gt 3915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1039P)^2^+0.3213P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(3) _refine_ls_number_reflns 4231 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1508 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.228 _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 Co1 Co 0.40797(6) 0.84898(5) 0.39072(5) 0.0318(2) Uani 1 1 d . . . Cl1 Cl 0.11986(18) 0.25400(18) 0.09951(12) 0.0769(6) Uani 1 1 d DU . . C1 C 0.3639(8) 0.7275(8) 0.2377(6) 0.080(2) Uani 1 1 d U . . C2 C 0.5065(5) 1.0678(5) 0.3895(4) 0.0412(13) Uani 1 1 d . . . H2 H 0.5444 1.0523 0.4403 0.049 Uiso 1 1 calc R . . C3 C 0.5192(6) 1.1707(6) 0.3526(5) 0.0519(16) Uani 1 1 d . . . H3 H 0.5657 1.2237 0.3785 0.062 Uiso 1 1 calc R . . C4 C 0.4623(6) 1.1919(6) 0.2779(5) 0.0520(16) Uani 1 1 d . . . H4 H 0.4709 1.2593 0.2526 0.062 Uiso 1 1 calc R . . C5 C 0.3909(6) 1.1126(6) 0.2393(5) 0.0505(16) Uani 1 1 d . . . H5 H 0.3508 1.1266 0.1890 0.061 Uiso 1 1 calc R . . C6 C 0.3827(4) 1.0140(5) 0.2784(4) 0.0374(12) Uani 1 1 d . . . C7 C 0.3071(5) 0.9197(5) 0.2516(4) 0.0432(14) Uani 1 1 d . . . C8 C 0.2278(5) 0.9308(5) 0.3046(4) 0.0436(14) Uani 1 1 d . . . C9 C 0.1267(5) 0.9726(6) 0.2813(5) 0.059(2) Uani 1 1 d . . . H9 H 0.0998 0.9927 0.2285 0.070 Uiso 1 1 calc R . . C10 C 0.0687(6) 0.9825(7) 0.3418(7) 0.071(3) Uani 1 1 d . . . H10 H 0.0013 1.0100 0.3295 0.085 Uiso 1 1 calc R . . C11 C 0.1094(5) 0.9525(6) 0.4181(6) 0.062(2) Uani 1 1 d . . . H11 H 0.0695 0.9586 0.4577 0.075 Uiso 1 1 calc R . . C12 C 0.2118(5) 0.9121(6) 0.4378(5) 0.0535(17) Uani 1 1 d . . . H12 H 0.2406 0.8934 0.4905 0.064 Uiso 1 1 calc R . . C13 C 0.6059(5) 0.7898(5) 0.3444(4) 0.0395(13) Uani 1 1 d . . . H13 H 0.5774 0.8101 0.2920 0.047 Uiso 1 1 calc R . . C14 C 0.7059(6) 0.7521(6) 0.3616(4) 0.0516(16) Uani 1 1 d . . . H14 H 0.7452 0.7454 0.3217 0.062 Uiso 1 1 calc R . . C15 C 0.7468(5) 0.7243(6) 0.4405(5) 0.0558(18) Uani 1 1 d . . . H15 H 0.8151 0.6998 0.4542 0.067 Uiso 1 1 calc R . . C16 C 0.6878(5) 0.7327(6) 0.4978(5) 0.0494(15) Uani 1 1 d . . . H16 H 0.7139 0.7115 0.5505 0.059 Uiso 1 1 calc R . . C17 C 0.5894(4) 0.7730(5) 0.4763(4) 0.0369(12) Uani 1 1 d . . . C18 C 0.5077(5) 0.7857(5) 0.5289(4) 0.0393(13) Uani 1 1 d . . . C19 C 0.4323(5) 0.6877(5) 0.5045(4) 0.0421(13) Uani 1 1 d . . . C20 C 0.4251(6) 0.5906(6) 0.5481(5) 0.0553(18) Uani 1 1 d . . . H20 H 0.4660 0.5800 0.5986 0.066 Uiso 1 1 calc R . . C21 C 0.3577(7) 0.5137(6) 0.5148(6) 0.068(2) Uani 1 1 d . . . H21 H 0.3501 0.4480 0.5425 0.082 Uiso 1 1 calc R . . C22 C 0.2992(7) 0.5300(7) 0.4399(6) 0.069(2) Uani 1 1 d . . . H22 H 0.2536 0.4746 0.4163 0.082 Uiso 1 1 calc R . . C23 C 0.3079(6) 0.6285(5) 0.3995(5) 0.0495(15) Uani 1 1 d . . . H23 H 0.2666 0.6409 0.3494 0.059 Uiso 1 1 calc R . . C24 C 0.6119(10) 0.8816(12) 0.6395(8) 0.105(3) Uani 1 1 d U . . H24A H 0.6579 0.8964 0.6031 0.157 Uiso 1 1 calc R . . H24B H 0.6518 0.8648 0.6916 0.157 Uiso 1 1 calc R . . H24C H 0.5696 0.9463 0.6430 0.157 Uiso 1 1 calc R . . N1 N 0.3648(5) 0.8202(5) 0.2801(3) 0.0397(11) Uani 1 1 d U . . N2 N 0.3813(9) 0.6452(7) 0.1977(7) 0.104(3) Uani 1 1 d U . . N3 N 0.4404(3) 0.9927(4) 0.3517(3) 0.0329(10) Uani 1 1 d . . . N4 N 0.2665(3) 0.9010(4) 0.3805(3) 0.0378(11) Uani 1 1 d . . . N5 N 0.5488(4) 0.7982(4) 0.4001(3) 0.0332(10) Uani 1 1 d . . . N6 N 0.3766(4) 0.7069(4) 0.4331(3) 0.0373(11) Uani 1 1 d . . . O1 O 0.2611(4) 0.9197(4) 0.1737(3) 0.0566(12) Uani 1 1 d . . . H1 H 0.2998 0.9487 0.1470 0.085 Uiso 1 1 calc R . . O2 O 0.4514(3) 0.8835(4) 0.5004(2) 0.0386(9) Uani 1 1 d . . . O3 O 0.5447(4) 0.7848(4) 0.6101(3) 0.0548(12) Uani 1 1 d U . . O4 O 0.1923(10) 0.2990(10) 0.0597(7) 0.209(6) Uani 1 1 d DU . . O5 O 0.1463(10) 0.1517(7) 0.1287(7) 0.180(5) Uani 1 1 d DU . . O6 O 0.0276(8) 0.2436(10) 0.0409(6) 0.175(5) Uani 1 1 d DU . . O7 O 0.0983(9) 0.3285(8) 0.1563(5) 0.146(4) Uani 1 1 d DU . . O8 O 0.3922(5) 0.9408(6) 0.0766(4) 0.0758(16) Uani 1 1 d . . . H8A H 0.4005 0.8870 0.0456 0.091 Uiso 1 1 d R . . H8B H 0.4436 0.9399 0.1155 0.091 Uiso 1 1 d R . . O9 O 0.3202(11) 0.4366(14) 0.2373(9) 0.198(6) Uani 1 1 d . . . H9A H 0.3396 0.4901 0.2107 0.238 Uiso 1 1 d R . . H9B H 0.2739 0.3999 0.2060 0.238 Uiso 1 1 d 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 Co1 0.0320(3) 0.0315(3) 0.0307(3) -0.0008(3) 0.0024(2) -0.0022(3) Cl1 0.1061(16) 0.0746(13) 0.0558(11) 0.0121(9) 0.0303(11) 0.0243(12) C1 0.090(5) 0.068(4) 0.074(5) -0.019(4) -0.004(4) -0.004(4) C2 0.037(3) 0.049(3) 0.038(3) 0.002(3) 0.008(2) -0.002(3) C3 0.059(4) 0.039(3) 0.060(4) -0.007(3) 0.018(3) -0.014(3) C4 0.059(4) 0.037(3) 0.061(4) 0.005(3) 0.015(3) -0.010(3) C5 0.063(4) 0.043(3) 0.042(4) 0.005(3) 0.001(3) 0.004(3) C6 0.039(3) 0.040(3) 0.032(3) 0.001(2) 0.004(2) -0.001(2) C7 0.048(3) 0.041(3) 0.034(3) 0.000(2) -0.008(3) 0.003(3) C8 0.031(3) 0.033(3) 0.060(4) -0.003(3) -0.007(3) -0.005(2) C9 0.039(3) 0.042(4) 0.085(5) 0.002(3) -0.013(4) -0.003(3) C10 0.033(3) 0.050(4) 0.127(9) -0.013(4) 0.009(4) -0.008(3) C11 0.038(3) 0.047(4) 0.104(7) -0.004(4) 0.019(4) -0.002(3) C12 0.047(3) 0.042(3) 0.073(5) -0.002(3) 0.015(3) -0.007(3) C13 0.045(3) 0.035(3) 0.038(3) -0.004(2) 0.007(3) -0.005(2) C14 0.059(4) 0.047(3) 0.055(4) -0.005(3) 0.028(3) 0.001(3) C15 0.045(3) 0.052(4) 0.071(5) 0.007(3) 0.014(3) 0.017(3) C16 0.044(3) 0.049(3) 0.054(4) 0.011(3) 0.004(3) 0.004(3) C17 0.032(3) 0.039(3) 0.039(3) 0.006(2) 0.005(2) 0.002(2) C18 0.043(3) 0.042(3) 0.033(3) -0.001(2) 0.006(3) 0.003(3) C19 0.046(3) 0.041(3) 0.042(3) -0.002(3) 0.015(3) 0.005(3) C20 0.055(4) 0.051(4) 0.064(5) 0.017(3) 0.021(4) 0.000(3) C21 0.080(5) 0.044(4) 0.089(6) 0.019(4) 0.036(5) 0.002(4) C22 0.073(5) 0.044(4) 0.094(6) -0.006(4) 0.027(5) -0.020(4) C23 0.046(3) 0.040(3) 0.059(4) -0.010(3) 0.003(3) -0.002(3) C24 0.087(7) 0.139(9) 0.090(8) -0.001(7) 0.018(6) -0.010(6) N1 0.056(3) 0.031(2) 0.027(2) 0.0006(19) -0.007(2) -0.001(2) N2 0.137(8) 0.058(4) 0.101(7) -0.034(4) -0.014(6) -0.002(4) N3 0.035(2) 0.031(2) 0.032(2) -0.0007(18) 0.0041(19) -0.0020(18) N4 0.028(2) 0.032(2) 0.050(3) 0.001(2) 0.001(2) -0.0015(19) N5 0.037(2) 0.030(2) 0.034(3) -0.0022(18) 0.012(2) -0.0018(19) N6 0.034(2) 0.031(2) 0.047(3) 0.001(2) 0.009(2) -0.0017(19) O1 0.064(3) 0.053(3) 0.044(3) -0.001(2) -0.013(2) -0.006(2) O2 0.041(2) 0.047(2) 0.027(2) -0.0062(19) 0.0029(17) 0.005(2) O3 0.056(3) 0.074(3) 0.034(2) 0.014(2) 0.007(2) 0.006(2) O4 0.267(13) 0.178(11) 0.223(12) -0.053(10) 0.152(11) -0.070(10) O5 0.206(12) 0.158(10) 0.169(11) 0.060(8) 0.021(10) 0.058(8) O6 0.182(10) 0.191(10) 0.122(8) -0.024(7) -0.050(7) 0.065(8) O7 0.225(11) 0.132(7) 0.097(7) -0.017(5) 0.072(7) 0.028(7) O8 0.077(4) 0.080(4) 0.067(4) 0.007(3) 0.006(3) -0.008(3) O9 0.176(13) 0.217(15) 0.189(14) -0.013(11) 0.002(11) -0.041(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.887(4) . ? Co1 N1 1.889(5) . ? Co1 N3 1.916(5) . ? Co1 N6 1.918(5) . ? Co1 N5 1.924(5) . ? Co1 N4 1.936(5) . ? Cl1 O5 1.339(7) . ? Cl1 O4 1.377(8) . ? Cl1 O7 1.381(7) . ? Cl1 O6 1.420(7) . ? C1 N2 1.241(13) . ? C1 N1 1.319(11) . ? C2 N3 1.325(8) . ? C2 C3 1.403(10) . ? C3 C4 1.368(11) . ? C4 C5 1.404(11) . ? C5 C6 1.366(9) . ? C6 N3 1.353(7) . ? C6 C7 1.512(8) . ? C7 O1 1.346(7) . ? C7 N1 1.443(8) . ? C7 C8 1.506(10) . ? C8 N4 1.341(8) . ? C8 C9 1.404(9) . ? C9 C10 1.396(13) . ? C10 C11 1.353(13) . ? C11 C12 1.408(10) . ? C12 N4 1.321(9) . ? C13 N5 1.317(8) . ? C13 C14 1.365(9) . ? C14 C15 1.386(10) . ? C15 C16 1.359(11) . ? C16 C17 1.362(9) . ? C17 N5 1.337(7) . ? C17 C18 1.528(8) . ? C18 O3 1.373(7) . ? C18 O2 1.417(8) . ? C18 C19 1.539(9) . ? C19 N6 1.312(8) . ? C19 C20 1.388(10) . ? C20 C21 1.327(12) . ? C21 C22 1.369(13) . ? C22 C23 1.378(11) . ? C23 N6 1.350(8) . ? C24 O3 1.483(14) . ? 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 O2 Co1 N1 177.9(3) . . ? O2 Co1 N3 95.8(2) . . ? N1 Co1 N3 82.2(2) . . ? O2 Co1 N6 82.4(2) . . ? N1 Co1 N6 99.7(2) . . ? N3 Co1 N6 178.2(2) . . ? O2 Co1 N5 83.22(19) . . ? N1 Co1 N5 97.3(2) . . ? N3 Co1 N5 92.17(19) . . ? N6 Co1 N5 87.80(19) . . ? O2 Co1 N4 97.1(2) . . ? N1 Co1 N4 82.4(2) . . ? N3 Co1 N4 87.4(2) . . ? N6 Co1 N4 92.7(2) . . ? N5 Co1 N4 179.5(2) . . ? O5 Cl1 O4 112.5(6) . . ? O5 Cl1 O7 113.8(5) . . ? O4 Cl1 O7 110.1(5) . . ? O5 Cl1 O6 107.8(5) . . ? O4 Cl1 O6 105.5(5) . . ? O7 Cl1 O6 106.6(5) . . ? N2 C1 N1 168.6(12) . . ? N3 C2 C3 119.9(6) . . ? C4 C3 C2 119.0(6) . . ? C3 C4 C5 120.5(6) . . ? C6 C5 C4 117.5(6) . . ? N3 C6 C5 121.8(5) . . ? N3 C6 C7 111.0(5) . . ? C5 C6 C7 127.1(6) . . ? O1 C7 N1 116.0(5) . . ? O1 C7 C8 110.8(6) . . ? N1 C7 C8 104.5(5) . . ? O1 C7 C6 116.3(5) . . ? N1 C7 C6 103.8(5) . . ? C8 C7 C6 104.1(5) . . ? N4 C8 C9 122.1(7) . . ? N4 C8 C7 111.9(5) . . ? C9 C8 C7 125.9(7) . . ? C10 C9 C8 116.2(8) . . ? C11 C10 C9 120.8(7) . . ? C10 C11 C12 120.3(8) . . ? N4 C12 C11 119.2(8) . . ? N5 C13 C14 121.8(6) . . ? C13 C14 C15 117.8(6) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C17 118.3(6) . . ? N5 C17 C16 121.5(6) . . ? N5 C17 C18 110.5(5) . . ? C16 C17 C18 127.8(6) . . ? O3 C18 O2 114.3(5) . . ? O3 C18 C17 115.7(5) . . ? O2 C18 C17 105.1(5) . . ? O3 C18 C19 110.5(5) . . ? O2 C18 C19 105.4(5) . . ? C17 C18 C19 104.8(5) . . ? N6 C19 C20 123.9(7) . . ? N6 C19 C18 109.4(5) . . ? C20 C19 C18 126.6(6) . . ? C21 C20 C19 117.2(8) . . ? C20 C21 C22 120.7(7) . . ? C21 C22 C23 119.9(7) . . ? N6 C23 C22 119.6(7) . . ? C1 N1 C7 124.0(6) . . ? C1 N1 Co1 131.7(6) . . ? C7 N1 Co1 102.9(4) . . ? C2 N3 C6 121.3(5) . . ? C2 N3 Co1 127.4(4) . . ? C6 N3 Co1 111.3(4) . . ? C12 N4 C8 121.5(6) . . ? C12 N4 Co1 127.8(5) . . ? C8 N4 Co1 110.7(4) . . ? C13 N5 C17 120.1(5) . . ? C13 N5 Co1 129.3(4) . . ? C17 N5 Co1 110.5(4) . . ? C19 N6 C23 118.7(5) . . ? C19 N6 Co1 112.4(4) . . ? C23 N6 Co1 128.9(5) . . ? C18 O2 Co1 101.4(4) . . ? C18 O3 C24 114.0(7) . . ? 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 N3 C2 C3 C4 0.3(10) . . . . ? C2 C3 C4 C5 1.0(11) . . . . ? C3 C4 C5 C6 -1.3(11) . . . . ? C4 C5 C6 N3 0.2(10) . . . . ? C4 C5 C6 C7 175.8(7) . . . . ? N3 C6 C7 O1 -166.6(5) . . . . ? C5 C6 C7 O1 17.4(10) . . . . ? N3 C6 C7 N1 -37.8(7) . . . . ? C5 C6 C7 N1 146.2(7) . . . . ? N3 C6 C7 C8 71.3(6) . . . . ? C5 C6 C7 C8 -104.7(7) . . . . ? O1 C7 C8 N4 163.1(5) . . . . ? N1 C7 C8 N4 37.5(6) . . . . ? C6 C7 C8 N4 -71.2(6) . . . . ? O1 C7 C8 C9 -20.3(8) . . . . ? N1 C7 C8 C9 -145.9(6) . . . . ? C6 C7 C8 C9 105.4(7) . . . . ? N4 C8 C9 C10 0.5(9) . . . . ? C7 C8 C9 C10 -175.7(6) . . . . ? C8 C9 C10 C11 -0.2(10) . . . . ? C9 C10 C11 C12 0.8(11) . . . . ? C10 C11 C12 N4 -1.8(10) . . . . ? N5 C13 C14 C15 -1.1(9) . . . . ? C13 C14 C15 C16 1.2(10) . . . . ? C14 C15 C16 C17 -2.5(11) . . . . ? C15 C16 C17 N5 3.7(10) . . . . ? C15 C16 C17 C18 177.4(6) . . . . ? N5 C17 C18 O3 -167.1(5) . . . . ? C16 C17 C18 O3 18.6(9) . . . . ? N5 C17 C18 O2 -40.0(6) . . . . ? C16 C17 C18 O2 145.7(6) . . . . ? N5 C17 C18 C19 70.9(6) . . . . ? C16 C17 C18 C19 -103.4(7) . . . . ? O3 C18 C19 N6 162.5(5) . . . . ? O2 C18 C19 N6 38.5(6) . . . . ? C17 C18 C19 N6 -72.2(6) . . . . ? O3 C18 C19 C20 -20.1(9) . . . . ? O2 C18 C19 C20 -144.2(6) . . . . ? C17 C18 C19 C20 105.2(7) . . . . ? N6 C19 C20 C21 0.0(11) . . . . ? C18 C19 C20 C21 -177.0(7) . . . . ? C19 C20 C21 C22 0.9(12) . . . . ? C20 C21 C22 C23 -1.9(13) . . . . ? C21 C22 C23 N6 2.1(12) . . . . ? N2 C1 N1 C7 112(5) . . . . ? N2 C1 N1 Co1 -85(6) . . . . ? O1 C7 N1 C1 -8.5(11) . . . . ? C8 C7 N1 C1 113.8(9) . . . . ? C6 C7 N1 C1 -137.4(8) . . . . ? O1 C7 N1 Co1 -176.2(5) . . . . ? C8 C7 N1 Co1 -53.9(5) . . . . ? C6 C7 N1 Co1 54.9(5) . . . . ? O2 Co1 N1 C1 162(6) . . . . ? N3 Co1 N1 C1 149.0(9) . . . . ? N6 Co1 N1 C1 -31.2(9) . . . . ? N5 Co1 N1 C1 57.8(9) . . . . ? N4 Co1 N1 C1 -122.7(9) . . . . ? O2 Co1 N1 C7 -32(7) . . . . ? N3 Co1 N1 C7 -44.7(4) . . . . ? N6 Co1 N1 C7 135.1(4) . . . . ? N5 Co1 N1 C7 -135.9(4) . . . . ? N4 Co1 N1 C7 43.7(4) . . . . ? C3 C2 N3 C6 -1.4(9) . . . . ? C3 C2 N3 Co1 -178.5(5) . . . . ? C5 C6 N3 C2 1.1(9) . . . . ? C7 C6 N3 C2 -175.1(5) . . . . ? C5 C6 N3 Co1 178.7(5) . . . . ? C7 C6 N3 Co1 2.5(6) . . . . ? O2 Co1 N3 C2 22.0(5) . . . . ? N1 Co1 N3 C2 -158.4(5) . . . . ? N6 Co1 N3 C2 28(7) . . . . ? N5 Co1 N3 C2 -61.4(5) . . . . ? N4 Co1 N3 C2 118.9(5) . . . . ? O2 Co1 N3 C6 -155.3(4) . . . . ? N1 Co1 N3 C6 24.2(4) . . . . ? N6 Co1 N3 C6 -150(7) . . . . ? N5 Co1 N3 C6 121.3(4) . . . . ? N4 Co1 N3 C6 -58.5(4) . . . . ? C11 C12 N4 C8 2.2(9) . . . . ? C11 C12 N4 Co1 179.5(5) . . . . ? C9 C8 N4 C12 -1.6(9) . . . . ? C7 C8 N4 C12 175.2(5) . . . . ? C9 C8 N4 Co1 -179.3(5) . . . . ? C7 C8 N4 Co1 -2.6(6) . . . . ? O2 Co1 N4 C12 -23.3(5) . . . . ? N1 Co1 N4 C12 158.8(5) . . . . ? N3 Co1 N4 C12 -118.8(5) . . . . ? N6 Co1 N4 C12 59.4(5) . . . . ? N5 Co1 N4 C12 -148(28) . . . . ? O2 Co1 N4 C8 154.2(4) . . . . ? N1 Co1 N4 C8 -23.7(4) . . . . ? N3 Co1 N4 C8 58.7(4) . . . . ? N6 Co1 N4 C8 -123.1(4) . . . . ? N5 Co1 N4 C8 30(29) . . . . ? C14 C13 N5 C17 2.2(8) . . . . ? C14 C13 N5 Co1 179.7(4) . . . . ? C16 C17 N5 C13 -3.6(8) . . . . ? C18 C17 N5 C13 -178.3(5) . . . . ? C16 C17 N5 Co1 178.5(5) . . . . ? C18 C17 N5 Co1 3.8(6) . . . . ? O2 Co1 N5 C13 -154.6(5) . . . . ? N1 Co1 N5 C13 23.4(5) . . . . ? N3 Co1 N5 C13 -59.0(5) . . . . ? N6 Co1 N5 C13 122.8(5) . . . . ? N4 Co1 N5 C13 -30(29) . . . . ? O2 Co1 N5 C17 23.1(4) . . . . ? N1 Co1 N5 C17 -159.0(4) . . . . ? N3 Co1 N5 C17 118.6(4) . . . . ? N6 Co1 N5 C17 -59.5(4) . . . . ? N4 Co1 N5 C17 147(28) . . . . ? C20 C19 N6 C23 0.2(9) . . . . ? C18 C19 N6 C23 177.7(5) . . . . ? C20 C19 N6 Co1 -179.5(5) . . . . ? C18 C19 N6 Co1 -2.0(6) . . . . ? C22 C23 N6 C19 -1.2(10) . . . . ? C22 C23 N6 Co1 178.4(5) . . . . ? O2 Co1 N6 C19 -24.4(4) . . . . ? N1 Co1 N6 C19 156.1(4) . . . . ? N3 Co1 N6 C19 -30(7) . . . . ? N5 Co1 N6 C19 59.1(4) . . . . ? N4 Co1 N6 C19 -121.2(4) . . . . ? O2 Co1 N6 C23 156.0(6) . . . . ? N1 Co1 N6 C23 -23.6(6) . . . . ? N3 Co1 N6 C23 150(7) . . . . ? N5 Co1 N6 C23 -120.6(6) . . . . ? N4 Co1 N6 C23 59.2(6) . . . . ? O3 C18 O2 Co1 -176.6(4) . . . . ? C17 C18 O2 Co1 55.4(5) . . . . ? C19 C18 O2 Co1 -55.0(4) . . . . ? N1 Co1 O2 C18 -148(7) . . . . ? N3 Co1 O2 C18 -135.8(4) . . . . ? N6 Co1 O2 C18 44.3(4) . . . . ? N5 Co1 O2 C18 -44.3(4) . . . . ? N4 Co1 O2 C18 136.1(4) . . . . ? O2 C18 O3 C24 -56.9(8) . . . . ? C17 C18 O3 C24 65.5(9) . . . . ? C19 C18 O3 C24 -175.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.800 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.106