Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Syntheses, Structures and Magnetism of Linear Tri- and Tetra-copper Chains Containing Anions of N,N'-bis(pyrimidine-2-yl)formamidine ; _publ_contact_author_email JDCHEN@CYCU.EDU.TW _publ_contact_author_name 'Prof. Jhy-Der Chen' loop_ _publ_author_name 'Zhi-Kai Chen' 'Chia-Her Lin' 'Jhy-Der Chen' 'Chih-Chieh Wang' ; Ju-Chun Wang ; # Attachment 'all.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 662456' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 B2 Cu3 F8 N25' _chemical_formula_weight 1202.12 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.707(2) _cell_length_b 11.940(3) _cell_length_c 32.952(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.870(18) _cell_angle_gamma 90.00 _cell_volume 4551.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 979 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.01 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6088 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 16151 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7782 _reflns_number_gt 5397 _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^)+(0.0453P)^2^+20.6841P] 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 7782 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 0.15162(7) 0.19721(7) -0.14319(3) 0.0388(2) Uani 1 1 d . . . Cu2 Cu 0.18505(7) 0.23688(7) -0.06064(3) 0.0417(2) Uani 1 1 d . . . Cu3 Cu 0.26139(7) 0.27420(7) 0.02386(3) 0.0362(2) Uani 1 1 d . . . N1 N 0.2610(5) 0.0914(5) -0.18857(18) 0.0439(15) Uani 1 1 d . . . N2 N 0.3994(6) -0.0306(5) -0.1500(2) 0.0547(17) Uani 1 1 d . . . N3 N 0.2726(5) 0.0856(4) -0.11961(16) 0.0333(13) Uani 1 1 d . . . N4 N 0.2795(4) 0.0980(4) -0.04988(17) 0.0317(12) Uani 1 1 d . . . N5 N 0.3529(5) -0.0581(5) -0.01094(18) 0.0382(14) Uani 1 1 d . . . N6 N 0.3006(4) 0.1076(4) 0.02106(17) 0.0330(13) Uani 1 1 d . . . N7 N 0.0338(5) 0.3201(4) -0.15208(18) 0.0377(13) Uani 1 1 d . . . N8 N -0.0407(5) 0.4861(5) -0.12658(19) 0.0463(15) Uani 1 1 d . . . N9 N 0.0847(4) 0.3689(4) -0.08407(17) 0.0331(13) Uani 1 1 d . . . N10 N 0.1541(4) 0.4162(4) -0.01895(16) 0.0305(12) Uani 1 1 d . . . N11 N 0.1496(5) 0.5970(5) 0.01184(18) 0.0376(13) Uani 1 1 d . . . N12 N 0.2452(5) 0.4397(5) 0.04523(17) 0.0354(13) Uani 1 1 d . . . N13 N 0.0218(5) 0.0831(5) -0.15677(18) 0.0410(14) Uani 1 1 d . . . N14 N -0.1231(5) 0.0052(6) -0.1216(2) 0.0507(16) Uani 1 1 d . . . N15 N 0.0291(5) 0.1217(4) -0.08949(18) 0.0350(13) Uani 1 1 d . . . N16 N 0.0624(4) 0.1731(4) -0.02392(17) 0.0329(13) Uani 1 1 d . . . N17 N -0.0684(5) 0.1442(5) 0.02294(19) 0.0406(14) Uani 1 1 d . . . N18 N 0.1137(5) 0.2351(4) 0.04208(16) 0.0335(12) Uani 1 1 d . . . N19 N 0.2751(5) 0.3171(5) -0.14221(17) 0.0363(13) Uani 1 1 d . . . N20 N 0.4316(5) 0.4304(5) -0.11225(17) 0.0427(15) Uani 1 1 d . . . N21 N 0.3277(4) 0.3211(4) -0.07121(16) 0.0319(12) Uani 1 1 d . . . N22 N 0.3978(4) 0.3153(4) -0.00179(16) 0.0315(12) Uani 1 1 d . . . N23 N 0.5964(5) 0.3534(5) 0.02284(17) 0.0373(13) Uani 1 1 d . . . N24 N 0.4632(5) 0.2893(5) 0.06590(17) 0.0363(13) Uani 1 1 d . . . C1 C 0.2995(9) 0.0607(8) -0.2234(3) 0.066(3) Uani 1 1 d . . . H1A H 0.2669 0.0924 -0.2482 0.080 Uiso 1 1 calc R . . C2 C 0.3846(9) -0.0153(9) -0.2226(3) 0.076(3) Uani 1 1 d . . . H2B H 0.4095 -0.0378 -0.2468 0.091 Uiso 1 1 calc R . . C3 C 0.4337(8) -0.0588(8) -0.1858(3) 0.071(3) Uani 1 1 d . . . H3A H 0.4936 -0.1102 -0.1854 0.086 Uiso 1 1 calc R . . C4 C 0.3157(6) 0.0435(6) -0.1543(2) 0.0391(16) Uani 1 1 d . . . C5 C 0.3111(5) 0.0491(5) -0.0829(2) 0.0329(15) Uani 1 1 d . . . H5B H 0.3612 -0.0118 -0.0796 0.040 Uiso 1 1 calc R . . C6 C 0.3133(5) 0.0466(5) -0.0124(2) 0.0302(14) Uani 1 1 d . . . C7 C 0.3809(6) -0.1042(6) 0.0258(2) 0.0457(19) Uani 1 1 d . . . H7A H 0.4106 -0.1766 0.0275 0.055 Uiso 1 1 calc R . . C8 C 0.3679(7) -0.0494(6) 0.0618(2) 0.0472(19) Uani 1 1 d . . . H8B H 0.3850 -0.0843 0.0873 0.057 Uiso 1 1 calc R . . C9 C 0.3293(6) 0.0572(6) 0.0582(2) 0.0396(16) Uani 1 1 d . . . H9A H 0.3221 0.0973 0.0819 0.047 Uiso 1 1 calc R . . C10 C -0.0289(6) 0.3383(6) -0.1890(2) 0.0450(18) Uani 1 1 d . . . H10A H -0.0252 0.2878 -0.2102 0.054 Uiso 1 1 calc R . . C11 C -0.0984(7) 0.4308(7) -0.1957(3) 0.057(2) Uani 1 1 d . . . H11B H -0.1432 0.4437 -0.2211 0.068 Uiso 1 1 calc R . . C12 C -0.0996(7) 0.5038(7) -0.1636(3) 0.058(2) Uani 1 1 d . . . H12A H -0.1438 0.5687 -0.1681 0.070 Uiso 1 1 calc R . . C13 C 0.0225(6) 0.3937(6) -0.1217(2) 0.0343(15) Uani 1 1 d . . . C14 C 0.0933(5) 0.4447(5) -0.0537(2) 0.0319(15) Uani 1 1 d . . . H14B H 0.0575 0.5143 -0.0575 0.038 Uiso 1 1 calc R . . C15 C 0.1813(5) 0.4896(5) 0.0133(2) 0.0318(15) Uani 1 1 d . . . C16 C 0.1916(6) 0.6573(6) 0.0443(2) 0.0455(18) Uani 1 1 d . . . H16A H 0.1732 0.7331 0.0443 0.055 Uiso 1 1 calc R . . C17 C 0.2611(7) 0.6138(6) 0.0783(2) 0.0486(19) Uani 1 1 d . . . H17B H 0.2903 0.6584 0.1007 0.058 Uiso 1 1 calc R . . C18 C 0.2849(6) 0.5012(7) 0.0775(2) 0.0445(18) Uani 1 1 d . . . H18A H 0.3298 0.4680 0.1000 0.053 Uiso 1 1 calc R . . C19 C -0.0245(7) 0.0324(7) -0.1908(2) 0.053(2) Uani 1 1 d . . . H19A H 0.0090 0.0415 -0.2144 0.063 Uiso 1 1 calc R . . C20 C -0.1203(7) -0.0333(7) -0.1922(3) 0.060(2) Uani 1 1 d . . . H20B H -0.1522 -0.0699 -0.2162 0.072 Uiso 1 1 calc R . . C21 C -0.1676(7) -0.0430(8) -0.1571(3) 0.063(2) Uani 1 1 d . . . H21A H -0.2344 -0.0856 -0.1579 0.076 Uiso 1 1 calc R . . C22 C -0.0280(6) 0.0662(6) -0.1225(2) 0.0405(17) Uani 1 1 d . . . C23 C -0.0029(6) 0.1158(5) -0.0531(2) 0.0372(16) Uani 1 1 d . . . H23B H -0.0667 0.0746 -0.0481 0.045 Uiso 1 1 calc R . . C24 C 0.0334(6) 0.1826(5) 0.0146(2) 0.0348(15) Uani 1 1 d . . . C25 C -0.0909(7) 0.1652(6) 0.0607(3) 0.0479(19) Uani 1 1 d . . . H25A H -0.1602 0.1389 0.0676 0.057 Uiso 1 1 calc R . . C26 C -0.0176(6) 0.2234(6) 0.0900(2) 0.0479(19) Uani 1 1 d . . . H26A H -0.0378 0.2404 0.1155 0.057 Uiso 1 1 calc R . . C27 C 0.0865(6) 0.2548(6) 0.0796(2) 0.0437(17) Uani 1 1 d . . . H27A H 0.1400 0.2909 0.0991 0.052 Uiso 1 1 calc R . . C28 C 0.2925(6) 0.3530(6) -0.1797(2) 0.0433(18) Uani 1 1 d . . . H28A H 0.2452 0.3261 -0.2029 0.052 Uiso 1 1 calc R . . C29 C 0.3772(7) 0.4275(7) -0.1842(2) 0.0473(19) Uani 1 1 d . . . H29A H 0.3888 0.4521 -0.2101 0.057 Uiso 1 1 calc R . . C30 C 0.4437(7) 0.4643(7) -0.1499(3) 0.055(2) Uani 1 1 d . . . H30A H 0.5014 0.5162 -0.1525 0.066 Uiso 1 1 calc R . . C31 C 0.3460(5) 0.3573(5) -0.1096(2) 0.0301(14) Uani 1 1 d . . . C32 C 0.4100(6) 0.3400(5) -0.0395(2) 0.0318(15) Uani 1 1 d . . . H32A H 0.4791 0.3721 -0.0443 0.038 Uiso 1 1 calc R . . C33 C 0.4923(6) 0.3219(5) 0.0299(2) 0.0324(15) Uani 1 1 d . . . C34 C 0.6783(7) 0.3490(7) 0.0555(2) 0.050(2) Uani 1 1 d . . . H34A H 0.7524 0.3719 0.0524 0.060 Uiso 1 1 calc R . . C35 C 0.6606(6) 0.3131(7) 0.0930(3) 0.051(2) Uani 1 1 d . . . H35A H 0.7210 0.3073 0.1148 0.061 Uiso 1 1 calc R . . C36 C 0.5490(6) 0.2857(6) 0.0973(2) 0.0416(17) Uani 1 1 d . . . H36A H 0.5332 0.2640 0.1230 0.050 Uiso 1 1 calc R . . B1 B 0.8553(11) 0.2387(11) 0.1938(4) 0.074(3) Uani 1 1 d . . . F1 F 0.9384(12) 0.3056(10) 0.1900(3) 0.225(7) Uani 1 1 d . . . F2 F 0.8728(8) 0.1880(8) 0.23056(19) 0.147(3) Uani 1 1 d . . . F3 F 0.7590(12) 0.2973(11) 0.1914(3) 0.233(7) Uani 1 1 d . . . F4 F 0.8405(5) 0.1630(5) 0.16208(17) 0.0851(16) Uani 1 1 d . . . B2 B -0.1286(9) 0.1802(10) -0.2970(3) 0.062(3) Uani 1 1 d . . . F5 F -0.1737(8) 0.0913(9) -0.2838(3) 0.185(5) Uani 1 1 d . . . F6 F -0.0122(6) 0.1770(7) -0.2832(3) 0.133(3) Uani 1 1 d . . . F7 F -0.1531(6) 0.1904(7) -0.33855(19) 0.115(2) Uani 1 1 d . . . F8 F -0.1615(8) 0.2752(8) -0.2802(2) 0.148(3) Uani 1 1 d . . . C37 C 0.6267(12) 0.2138(19) -0.2219(5) 0.179(9) Uani 1 1 d . . . H37A H 0.7004 0.1805 -0.2236 0.268 Uiso 1 1 calc R . . H37B H 0.6270 0.2905 -0.2306 0.268 Uiso 1 1 calc R . . H37C H 0.5672 0.1737 -0.2394 0.268 Uiso 1 1 calc R . . C38 C 0.6053(14) 0.2088(11) -0.1811(4) 0.116(5) Uani 1 1 d . . . N25 N 0.5799(16) 0.2036(10) -0.1496(4) 0.168(7) 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 0.0394(5) 0.0348(5) 0.0392(5) 0.0003(4) -0.0033(4) -0.0011(4) Cu2 0.0335(4) 0.0383(5) 0.0553(6) 0.0182(4) 0.0128(4) 0.0064(4) Cu3 0.0414(5) 0.0308(4) 0.0409(5) 0.0007(4) 0.0203(4) 0.0012(4) N1 0.056(4) 0.047(4) 0.030(3) -0.004(3) 0.011(3) -0.007(3) N2 0.063(4) 0.050(4) 0.055(4) -0.009(3) 0.021(4) 0.009(3) N3 0.034(3) 0.040(3) 0.025(3) 0.001(3) 0.004(3) 0.003(2) N4 0.030(3) 0.034(3) 0.032(3) 0.001(2) 0.010(3) 0.003(2) N5 0.043(3) 0.037(3) 0.035(3) 0.003(3) 0.008(3) 0.007(3) N6 0.033(3) 0.032(3) 0.035(3) 0.006(3) 0.009(3) 0.003(2) N7 0.040(3) 0.035(3) 0.038(4) 0.002(3) 0.005(3) -0.001(3) N8 0.046(4) 0.051(4) 0.039(4) -0.004(3) -0.002(3) 0.010(3) N9 0.031(3) 0.033(3) 0.035(3) 0.002(3) 0.005(3) 0.001(2) N10 0.030(3) 0.032(3) 0.031(3) -0.006(2) 0.011(3) -0.001(2) N11 0.038(3) 0.037(3) 0.038(3) -0.003(3) 0.006(3) 0.004(3) N12 0.034(3) 0.038(3) 0.035(3) 0.002(3) 0.010(3) 0.000(2) N13 0.043(3) 0.041(3) 0.036(4) -0.004(3) -0.002(3) -0.003(3) N14 0.039(4) 0.061(4) 0.050(4) -0.002(3) 0.000(3) -0.017(3) N15 0.029(3) 0.035(3) 0.040(4) -0.002(3) 0.005(3) -0.002(2) N16 0.033(3) 0.032(3) 0.033(3) -0.001(3) 0.006(3) 0.000(2) N17 0.035(3) 0.039(3) 0.050(4) 0.001(3) 0.013(3) 0.001(3) N18 0.038(3) 0.034(3) 0.029(3) -0.002(2) 0.008(3) 0.006(2) N19 0.043(3) 0.038(3) 0.027(3) 0.006(3) 0.002(3) -0.003(3) N20 0.047(4) 0.058(4) 0.023(3) 0.002(3) 0.004(3) -0.014(3) N21 0.033(3) 0.037(3) 0.026(3) 0.006(2) 0.003(3) 0.004(2) N22 0.032(3) 0.035(3) 0.028(3) 0.004(2) 0.005(3) 0.006(2) N23 0.033(3) 0.051(3) 0.027(3) 0.008(3) 0.003(3) 0.000(3) N24 0.041(3) 0.040(3) 0.027(3) 0.001(3) 0.003(3) 0.000(3) C1 0.097(7) 0.071(6) 0.031(4) -0.012(4) 0.010(5) -0.023(6) C2 0.094(8) 0.090(7) 0.053(6) -0.023(6) 0.045(6) -0.005(6) C3 0.068(6) 0.066(6) 0.089(8) -0.018(6) 0.040(6) 0.008(5) C4 0.043(4) 0.040(4) 0.036(4) -0.004(3) 0.012(3) -0.004(3) C5 0.030(3) 0.034(3) 0.035(4) 0.001(3) 0.004(3) -0.002(3) C6 0.030(3) 0.030(3) 0.031(4) 0.005(3) 0.003(3) 0.004(3) C7 0.053(5) 0.038(4) 0.048(5) 0.009(4) 0.013(4) 0.015(3) C8 0.061(5) 0.047(4) 0.032(4) 0.013(3) 0.003(4) 0.009(4) C9 0.048(4) 0.044(4) 0.026(4) 0.001(3) 0.006(3) 0.001(3) C10 0.043(4) 0.052(5) 0.038(4) 0.006(4) -0.001(4) 0.006(3) C11 0.062(5) 0.058(5) 0.044(5) 0.002(4) -0.013(4) 0.009(4) C12 0.055(5) 0.064(5) 0.054(6) 0.007(4) 0.002(4) 0.019(4) C13 0.034(4) 0.038(4) 0.032(4) 0.003(3) 0.006(3) 0.000(3) C14 0.025(3) 0.036(4) 0.036(4) 0.004(3) 0.011(3) 0.001(3) C15 0.028(3) 0.033(3) 0.036(4) 0.000(3) 0.010(3) 0.000(3) C16 0.047(4) 0.038(4) 0.052(5) -0.008(4) 0.011(4) 0.001(3) C17 0.055(5) 0.053(5) 0.036(4) -0.016(4) 0.002(4) -0.001(4) C18 0.042(4) 0.059(5) 0.028(4) 0.007(4) -0.007(3) -0.005(4) C19 0.057(5) 0.061(5) 0.037(5) -0.003(4) 0.003(4) 0.000(4) C20 0.059(5) 0.071(6) 0.047(5) -0.019(4) -0.004(4) -0.011(4) C21 0.050(5) 0.074(6) 0.060(6) -0.002(5) -0.008(5) -0.022(4) C22 0.047(4) 0.033(4) 0.043(4) 0.005(3) 0.009(4) 0.007(3) C23 0.036(4) 0.032(4) 0.045(5) 0.004(3) 0.007(3) 0.002(3) C24 0.043(4) 0.027(3) 0.037(4) 0.002(3) 0.012(3) 0.001(3) C25 0.046(4) 0.043(4) 0.059(5) 0.008(4) 0.023(4) 0.004(3) C26 0.052(4) 0.054(5) 0.043(4) -0.001(4) 0.025(4) -0.001(4) C27 0.054(4) 0.043(4) 0.037(4) 0.001(3) 0.016(4) 0.001(3) C28 0.049(4) 0.048(4) 0.032(4) -0.001(3) 0.003(4) -0.003(3) C29 0.054(5) 0.062(5) 0.025(4) 0.007(4) 0.005(4) -0.011(4) C30 0.061(5) 0.061(5) 0.046(5) 0.010(4) 0.018(4) -0.021(4) C31 0.033(3) 0.029(3) 0.029(4) 0.002(3) 0.008(3) 0.002(3) C32 0.032(3) 0.035(4) 0.031(4) 0.005(3) 0.012(3) 0.004(3) C33 0.039(4) 0.032(3) 0.028(4) 0.003(3) 0.010(3) 0.001(3) C34 0.042(4) 0.059(5) 0.048(5) 0.002(4) 0.005(4) -0.007(4) C35 0.040(4) 0.062(5) 0.045(5) -0.002(4) -0.012(4) 0.005(4) C36 0.049(4) 0.051(4) 0.024(4) 0.007(3) 0.004(3) 0.006(3) B1 0.084(8) 0.087(8) 0.050(7) 0.005(6) 0.012(6) 0.021(7) F1 0.358(17) 0.221(11) 0.098(6) -0.015(7) 0.045(8) -0.216(12) F2 0.198(8) 0.188(8) 0.049(4) 0.042(5) 0.005(5) -0.028(7) F3 0.274(13) 0.295(14) 0.110(7) -0.082(8) -0.035(8) 0.187(12) F4 0.102(4) 0.093(4) 0.063(4) -0.003(3) 0.025(3) -0.001(3) B2 0.060(6) 0.073(7) 0.058(7) -0.009(6) 0.022(5) -0.007(5) F5 0.176(8) 0.205(9) 0.145(7) 0.089(7) -0.063(6) -0.125(7) F6 0.083(5) 0.155(7) 0.163(8) 0.002(6) 0.022(5) -0.010(5) F7 0.145(6) 0.146(6) 0.057(4) -0.010(4) 0.025(4) -0.007(5) F8 0.178(8) 0.182(8) 0.082(5) -0.040(5) 0.010(5) 0.081(7) C37 0.102(11) 0.34(3) 0.091(11) 0.052(15) 0.018(9) 0.000(14) C38 0.181(14) 0.093(9) 0.059(8) 0.009(7) -0.028(9) -0.002(9) N25 0.33(2) 0.100(9) 0.065(8) 0.007(7) -0.015(10) -0.033(10) _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 N7 2.005(6) . ? Cu1 N3 2.012(5) . ? Cu1 N19 2.031(6) . ? Cu1 N13 2.040(6) . ? Cu1 N1 2.462(6) . ? Cu1 Cu2 2.7292(15) . ? Cu2 N4 1.994(5) . ? Cu2 N21 2.025(5) . ? Cu2 N9 2.045(5) . ? Cu2 N16 2.154(5) . ? Cu2 N15 2.365(5) . ? Cu2 Cu3 2.8254(15) . ? Cu3 N18 1.972(5) . ? Cu3 N22 1.980(5) . ? Cu3 N6 2.047(5) . ? Cu3 N12 2.116(6) . ? Cu3 N10 2.429(5) . ? N1 C4 1.339(9) . ? N1 C1 1.347(10) . ? N2 C4 1.312(9) . ? N2 C3 1.347(11) . ? N3 C5 1.298(8) . ? N3 C4 1.409(8) . ? N4 C5 1.338(8) . ? N4 C6 1.381(8) . ? N5 C7 1.324(9) . ? N5 C6 1.332(8) . ? N6 C6 1.349(8) . ? N6 C9 1.360(8) . ? N7 C10 1.336(9) . ? N7 C13 1.353(9) . ? N8 C12 1.322(10) . ? N8 C13 1.324(9) . ? N9 C14 1.341(8) . ? N9 C13 1.370(9) . ? N10 C14 1.298(8) . ? N10 C15 1.375(8) . ? N11 C16 1.321(9) . ? N11 C15 1.334(8) . ? N12 C18 1.316(9) . ? N12 C15 1.335(8) . ? N13 C19 1.315(9) . ? N13 C22 1.362(9) . ? N14 C21 1.335(10) . ? N14 C22 1.335(9) . ? N15 C23 1.313(9) . ? N15 C22 1.359(9) . ? N16 C23 1.322(9) . ? N16 C24 1.369(8) . ? N17 C25 1.334(10) . ? N17 C24 1.344(8) . ? N18 C27 1.345(9) . ? N18 C24 1.354(9) . ? N19 C31 1.341(8) . ? N19 C28 1.352(9) . ? N20 C30 1.333(9) . ? N20 C31 1.342(8) . ? N21 C32 1.327(8) . ? N21 C31 1.385(8) . ? N22 C32 1.307(8) . ? N22 C33 1.400(9) . ? N23 C34 1.328(9) . ? N23 C33 1.330(8) . ? N24 C36 1.326(9) . ? N24 C33 1.343(8) . ? C1 C2 1.344(13) . ? C2 C3 1.362(14) . ? C7 C8 1.384(10) . ? C8 C9 1.349(10) . ? C10 C11 1.371(11) . ? C11 C12 1.372(12) . ? C16 C17 1.381(11) . ? C17 C18 1.374(10) . ? C19 C20 1.364(11) . ? C20 C21 1.361(12) . ? C25 C26 1.378(11) . ? C26 C27 1.369(10) . ? C28 C29 1.357(10) . ? C29 C30 1.345(11) . ? C34 C35 1.353(11) . ? C35 C36 1.376(10) . ? B1 F1 1.279(15) . ? B1 F3 1.320(14) . ? B1 F2 1.342(13) . ? B1 F4 1.372(13) . ? B2 F5 1.291(13) . ? B2 F8 1.343(13) . ? B2 F7 1.361(12) . ? B2 F6 1.369(12) . ? C37 C38 1.408(19) . ? C38 N25 1.123(18) . ? 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 N7 Cu1 N3 165.8(2) . . ? N7 Cu1 N19 87.6(2) . . ? N3 Cu1 N19 90.2(2) . . ? N7 Cu1 N13 89.1(2) . . ? N3 Cu1 N13 95.7(2) . . ? N19 Cu1 N13 168.3(2) . . ? N7 Cu1 N1 134.2(2) . . ? N3 Cu1 N1 59.6(2) . . ? N19 Cu1 N1 86.3(2) . . ? N13 Cu1 N1 87.9(2) . . ? N7 Cu1 Cu2 90.48(17) . . ? N3 Cu1 Cu2 75.28(15) . . ? N19 Cu1 Cu2 82.51(16) . . ? N13 Cu1 Cu2 108.79(18) . . ? N1 Cu1 Cu2 133.34(15) . . ? N4 Cu2 N21 89.7(2) . . ? N4 Cu2 N9 168.1(2) . . ? N21 Cu2 N9 89.6(2) . . ? N4 Cu2 N16 90.3(2) . . ? N21 Cu2 N16 155.6(2) . . ? N9 Cu2 N16 95.2(2) . . ? N4 Cu2 N15 87.7(2) . . ? N21 Cu2 N15 145.7(2) . . ? N9 Cu2 N15 86.2(2) . . ? N16 Cu2 N15 58.7(2) . . ? N4 Cu2 Cu1 91.34(16) . . ? N21 Cu2 Cu1 84.85(16) . . ? N9 Cu2 Cu1 76.81(16) . . ? N16 Cu2 Cu1 119.54(15) . . ? N15 Cu2 Cu1 61.00(14) . . ? N4 Cu2 Cu3 82.72(16) . . ? N21 Cu2 Cu3 86.97(16) . . ? N9 Cu2 Cu3 109.06(16) . . ? N16 Cu2 Cu3 68.84(15) . . ? N15 Cu2 Cu3 126.52(15) . . ? Cu1 Cu2 Cu3 169.92(4) . . ? N18 Cu3 N22 172.4(2) . . ? N18 Cu3 N6 89.8(2) . . ? N22 Cu3 N6 91.2(2) . . ? N18 Cu3 N12 89.5(2) . . ? N22 Cu3 N12 91.7(2) . . ? N6 Cu3 N12 162.7(2) . . ? N18 Cu3 N10 86.73(19) . . ? N22 Cu3 N10 87.60(19) . . ? N6 Cu3 N10 138.8(2) . . ? N12 Cu3 N10 58.4(2) . . ? N18 Cu3 Cu2 95.96(16) . . ? N22 Cu3 Cu2 76.81(16) . . ? N6 Cu3 Cu2 80.87(16) . . ? N12 Cu3 Cu2 116.39(16) . . ? N10 Cu3 Cu2 58.74(12) . . ? C4 N1 C1 115.0(7) . . ? C4 N1 Cu1 86.1(4) . . ? C1 N1 Cu1 158.6(6) . . ? C4 N2 C3 113.2(8) . . ? C5 N3 C4 121.2(6) . . ? C5 N3 Cu1 134.8(5) . . ? C4 N3 Cu1 104.0(4) . . ? C5 N4 C6 117.2(5) . . ? C5 N4 Cu2 115.7(4) . . ? C6 N4 Cu2 127.1(4) . . ? C7 N5 C6 117.3(6) . . ? C6 N6 C9 117.0(6) . . ? C6 N6 Cu3 128.0(4) . . ? C9 N6 Cu3 114.6(5) . . ? C10 N7 C13 117.7(6) . . ? C10 N7 Cu1 121.4(5) . . ? C13 N7 Cu1 120.7(5) . . ? C12 N8 C13 116.6(7) . . ? C14 N9 C13 119.8(6) . . ? C14 N9 Cu2 105.4(4) . . ? C13 N9 Cu2 134.6(5) . . ? C14 N10 C15 123.1(6) . . ? C14 N10 Cu3 149.3(4) . . ? C15 N10 Cu3 87.6(4) . . ? C16 N11 C15 115.4(6) . . ? C18 N12 C15 118.2(6) . . ? C18 N12 Cu3 138.7(5) . . ? C15 N12 Cu3 102.8(4) . . ? C19 N13 C22 117.8(7) . . ? C19 N13 Cu1 133.6(6) . . ? C22 N13 Cu1 108.5(5) . . ? C21 N14 C22 115.4(7) . . ? C23 N15 C22 122.1(6) . . ? C23 N15 Cu2 88.6(4) . . ? C22 N15 Cu2 149.3(5) . . ? C23 N16 C24 121.2(6) . . ? C23 N16 Cu2 97.8(4) . . ? C24 N16 Cu2 140.7(4) . . ? C25 N17 C24 115.8(6) . . ? C27 N18 C24 117.3(6) . . ? C27 N18 Cu3 125.6(5) . . ? C24 N18 Cu3 117.2(4) . . ? C31 N19 C28 117.1(6) . . ? C31 N19 Cu1 128.0(4) . . ? C28 N19 Cu1 114.6(5) . . ? C30 N20 C31 116.5(6) . . ? C32 N21 C31 118.1(5) . . ? C32 N21 Cu2 117.9(4) . . ? C31 N21 Cu2 124.0(4) . . ? C32 N22 C33 120.4(6) . . ? C32 N22 Cu3 132.5(5) . . ? C33 N22 Cu3 107.0(4) . . ? C34 N23 C33 114.5(6) . . ? C36 N24 C33 115.8(6) . . ? C2 C1 N1 120.9(9) . . ? C1 C2 C3 118.9(8) . . ? N2 C3 C2 122.9(9) . . ? N2 C4 N1 129.1(7) . . ? N2 C4 N3 120.5(7) . . ? N1 C4 N3 110.3(6) . . ? N3 C5 N4 120.8(6) . . ? N5 C6 N6 124.0(6) . . ? N5 C6 N4 120.0(6) . . ? N6 C6 N4 116.0(5) . . ? N5 C7 C8 122.9(7) . . ? C9 C8 C7 116.8(7) . . ? C8 C9 N6 121.9(7) . . ? N7 C10 C11 120.5(7) . . ? C10 C11 C12 117.6(8) . . ? N8 C12 C11 122.9(8) . . ? N8 C13 N7 124.6(6) . . ? N8 C13 N9 119.9(6) . . ? N7 C13 N9 115.5(6) . . ? N10 C14 N9 116.7(6) . . ? N11 C15 N12 125.2(6) . . ? N11 C15 N10 123.7(6) . . ? N12 C15 N10 111.1(6) . . ? N11 C16 C17 123.5(7) . . ? C18 C17 C16 116.6(7) . . ? N12 C18 C17 121.0(7) . . ? N13 C19 C20 121.4(8) . . ? C21 C20 C19 117.4(8) . . ? N14 C21 C20 123.5(8) . . ? N14 C22 N15 123.8(7) . . ? N14 C22 N13 124.4(7) . . ? N15 C22 N13 111.8(6) . . ? N15 C23 N16 115.0(6) . . ? N17 C24 N18 124.6(6) . . ? N17 C24 N16 121.1(6) . . ? N18 C24 N16 114.4(6) . . ? N17 C25 C26 123.9(7) . . ? C27 C26 C25 116.4(7) . . ? N18 C27 C26 121.9(7) . . ? N19 C28 C29 121.7(7) . . ? C30 C29 C28 117.3(7) . . ? N20 C30 C29 123.6(7) . . ? N19 C31 N20 123.9(6) . . ? N19 C31 N21 117.2(6) . . ? N20 C31 N21 119.0(6) . . ? N22 C32 N21 122.5(6) . . ? N23 C33 N24 126.9(6) . . ? N23 C33 N22 121.8(6) . . ? N24 C33 N22 111.3(6) . . ? N23 C34 C35 124.0(7) . . ? C34 C35 C36 116.8(7) . . ? N24 C36 C35 122.0(7) . . ? F1 B1 F3 108.6(14) . . ? F1 B1 F2 110.9(11) . . ? F3 B1 F2 107.6(11) . . ? F1 B1 F4 110.2(10) . . ? F3 B1 F4 107.3(10) . . ? F2 B1 F4 112.0(11) . . ? F5 B2 F8 113.5(10) . . ? F5 B2 F7 112.3(10) . . ? F8 B2 F7 108.0(10) . . ? F5 B2 F6 107.6(10) . . ? F8 B2 F6 102.8(9) . . ? F7 B2 F6 112.4(9) . . ? N25 C38 C37 174.9(19) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.702 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.094 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 662457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H33 Cu3 N27 O7' _chemical_formula_weight 1170.53 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6294(4) _cell_length_b 11.9689(4) _cell_length_c 32.9002(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.8830(10) _cell_angle_gamma 90.00 _cell_volume 4536.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6510 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35714 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7488 _reflns_number_gt 5414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0890P)^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 7488 _refine_ls_number_parameters 676 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.017 _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 0.76149(4) 0.72549(4) 1.025291(17) 0.03493(17) Uani 1 1 d . . . Cu2 Cu 0.68884(5) 0.76383(4) 0.940730(18) 0.04004(18) Uani 1 1 d . . . Cu3 Cu 0.66012(5) 0.80812(4) 0.857548(17) 0.03927(18) Uani 1 1 d . . . N1 N 0.7804(4) 0.9197(3) 0.81417(12) 0.0479(10) Uani 1 1 d . . . N2 N 0.9202(4) 1.0326(4) 0.85558(13) 0.0542(11) Uani 1 1 d . . . N3 N 0.7829(3) 0.9166(3) 0.88260(11) 0.0356(9) Uani 1 1 d . . . N4 N 0.7834(3) 0.9019(3) 0.95240(10) 0.0318(8) Uani 1 1 d . . . N5 N 0.8519(3) 1.0582(3) 0.99156(11) 0.0379(9) Uani 1 1 d . . . N6 N 0.8006(3) 0.8910(3) 1.02368(10) 0.0309(8) Uani 1 1 d . . . N7 N 0.5365(3) 0.6884(3) 0.84884(11) 0.0358(9) Uani 1 1 d . . . N8 N 0.4568(3) 0.5227(3) 0.87338(12) 0.0491(10) Uani 1 1 d . . . N9 N 0.5886(3) 0.6341(3) 0.91636(10) 0.0312(8) Uani 1 1 d . . . N10 N 0.6543(3) 0.5843(3) 0.98071(10) 0.0306(8) Uani 1 1 d . . . N11 N 0.6475(3) 0.4036(3) 1.01099(11) 0.0339(8) Uani 1 1 d . . . N12 N 0.7440(3) 0.5613(3) 1.04476(10) 0.0334(8) Uani 1 1 d . . . N13 N 0.5335(3) 0.9247(3) 0.84477(11) 0.0402(9) Uani 1 1 d . . . N14 N 0.3826(3) 0.9990(3) 0.87847(13) 0.0497(10) Uani 1 1 d . . . N15 N 0.5341(3) 0.8822(3) 0.91140(11) 0.0338(8) Uani 1 1 d . . . N16 N 0.5629(3) 0.8271(3) 0.97632(10) 0.0307(8) Uani 1 1 d . . . N17 N 0.4281(3) 0.8559(3) 1.02260(12) 0.0377(9) Uani 1 1 d . . . N18 N 0.6090(3) 0.7641(3) 1.04255(11) 0.0330(8) Uani 1 1 d . . . N19 N 0.7810(3) 0.6878(3) 0.85783(11) 0.0360(9) Uani 1 1 d . . . N20 N 0.9403(3) 0.5760(3) 0.88700(11) 0.0425(10) Uani 1 1 d . . . N21 N 0.8318(3) 0.6821(3) 0.92907(10) 0.0306(8) Uani 1 1 d . . . N22 N 0.8997(3) 0.6849(3) 0.99830(10) 0.0304(8) Uani 1 1 d . . . N23 N 1.0972(3) 0.6459(3) 1.02314(11) 0.0373(9) Uani 1 1 d . . . N24 N 0.9617(3) 0.7070(3) 1.06602(11) 0.0342(9) Uani 1 1 d . . . C1 C 0.8225(5) 0.9559(5) 0.78033(17) 0.0610(15) Uani 1 1 d . . . H1B H 0.7896 0.9303 0.7546 0.073 Uiso 1 1 calc R . . C2 C 0.9130(6) 1.0295(5) 0.7833(2) 0.0735(18) Uani 1 1 d . . . H2B H 0.9433 1.0535 0.7601 0.088 Uiso 1 1 calc R . . C3 C 0.9570(6) 1.0664(5) 0.8210(2) 0.0698(17) Uani 1 1 d . . . H3A H 1.0167 1.1186 0.8230 0.084 Uiso 1 1 calc R . . C4 C 0.8317(4) 0.9616(4) 0.84924(14) 0.0394(11) Uani 1 1 d . . . C5 C 0.8195(4) 0.9508(4) 0.91971(13) 0.0344(10) Uani 1 1 d . . . H5B H 0.8716 1.0100 0.9236 0.041 Uiso 1 1 calc R . . C6 C 0.8140(3) 0.9524(3) 0.99020(13) 0.0306(10) Uani 1 1 d . . . C7 C 0.8752(4) 1.1043(4) 1.02842(15) 0.0426(12) Uani 1 1 d . . . H7A H 0.9025 1.1774 1.0302 0.051 Uiso 1 1 calc R . . C8 C 0.8612(4) 1.0497(4) 1.06408(15) 0.0448(12) Uani 1 1 d . . . H8B H 0.8759 1.0845 1.0895 0.054 Uiso 1 1 calc R . . C9 C 0.8244(4) 0.9418(4) 1.06004(14) 0.0387(11) Uani 1 1 d . . . H9A H 0.8155 0.9017 1.0836 0.046 Uiso 1 1 calc R . . C10 C 0.4683(4) 0.6739(4) 0.81242(14) 0.0466(12) Uani 1 1 d . . . H10A H 0.4711 0.7265 0.7918 0.056 Uiso 1 1 calc R . . C11 C 0.3962(5) 0.5852(5) 0.80518(16) 0.0592(15) Uani 1 1 d . . . H11B H 0.3497 0.5754 0.7801 0.071 Uiso 1 1 calc R . . C12 C 0.3951(5) 0.5098(5) 0.83696(16) 0.0602(15) Uani 1 1 d . . . H12A H 0.3483 0.4468 0.8324 0.072 Uiso 1 1 calc R . . C13 C 0.5254(4) 0.6126(4) 0.87867(13) 0.0344(10) Uani 1 1 d . . . C14 C 0.5942(3) 0.5576(4) 0.94590(13) 0.0334(10) Uani 1 1 d . . . H14B H 0.5571 0.4888 0.9418 0.040 Uiso 1 1 calc R . . C15 C 0.6788(3) 0.5109(3) 1.01254(13) 0.0297(9) Uani 1 1 d . . . C16 C 0.6899(4) 0.3431(4) 1.04382(15) 0.0414(11) Uani 1 1 d . . . H16A H 0.6723 0.2673 1.0437 0.050 Uiso 1 1 calc R . . C17 C 0.7579(4) 0.3863(4) 1.07776(15) 0.0447(12) Uani 1 1 d . . . H17B H 0.7857 0.3417 1.1001 0.054 Uiso 1 1 calc R . . C18 C 0.7827(4) 0.4981(4) 1.07700(14) 0.0419(11) Uani 1 1 d . . . H18A H 0.8275 0.5305 1.0995 0.050 Uiso 1 1 calc R . . C19 C 0.4907(5) 0.9777(4) 0.80972(16) 0.0575(14) Uani 1 1 d . . . H19A H 0.5283 0.9717 0.7866 0.069 Uiso 1 1 calc R . . C20 C 0.3916(5) 1.0405(5) 0.80832(17) 0.0660(16) Uani 1 1 d . . . H20B H 0.3598 1.0765 0.7843 0.079 Uiso 1 1 calc R . . C21 C 0.3416(5) 1.0483(5) 0.84316(18) 0.0617(15) Uani 1 1 d . . . H21A H 0.2743 1.0908 0.8423 0.074 Uiso 1 1 calc R . . C22 C 0.4786(4) 0.9389(4) 0.87749(14) 0.0377(11) Uani 1 1 d . . . C23 C 0.4998(4) 0.8857(3) 0.94698(14) 0.0358(11) Uani 1 1 d . . . H23B H 0.4350 0.9266 0.9518 0.043 Uiso 1 1 calc R . . C24 C 0.5300(4) 0.8174(3) 1.01449(14) 0.0337(10) Uani 1 1 d . . . C25 C 0.4013(4) 0.8339(4) 1.05974(16) 0.0449(12) Uani 1 1 d . . . H25A H 0.3304 0.8600 1.0660 0.054 Uiso 1 1 calc R . . C26 C 0.4710(4) 0.7753(4) 1.08960(16) 0.0460(12) Uani 1 1 d . . . H26A H 0.4482 0.7589 1.1150 0.055 Uiso 1 1 calc R . . C27 C 0.5778(4) 0.7423(4) 1.07921(15) 0.0407(11) Uani 1 1 d . . . H27A H 0.6290 0.7039 1.0985 0.049 Uiso 1 1 calc R . . C28 C 0.7986(4) 0.6531(4) 0.82047(14) 0.0451(12) Uani 1 1 d . . . H28A H 0.7505 0.6798 0.7976 0.054 Uiso 1 1 calc R . . C29 C 0.8848(5) 0.5800(4) 0.81490(15) 0.0528(14) Uani 1 1 d . . . H29A H 0.8955 0.5549 0.7889 0.063 Uiso 1 1 calc R . . C30 C 0.9549(5) 0.5452(4) 0.84937(15) 0.0537(14) Uani 1 1 d . . . H30A H 1.0161 0.4974 0.8462 0.064 Uiso 1 1 calc R . . C31 C 0.8528(4) 0.6468(3) 0.89049(13) 0.0312(10) Uani 1 1 d . . . C32 C 0.9132(4) 0.6617(3) 0.96059(13) 0.0301(10) Uani 1 1 d . . . H32A H 0.9827 0.6295 0.9555 0.036 Uiso 1 1 calc R . . C33 C 0.9920(4) 0.6766(3) 1.03045(13) 0.0304(10) Uani 1 1 d . . . C34 C 1.1781(4) 0.6479(4) 1.05612(14) 0.0438(12) Uani 1 1 d . . . H34A H 1.2531 0.6264 1.0528 0.053 Uiso 1 1 calc R . . C35 C 1.1580(4) 0.6794(4) 1.09432(15) 0.0500(13) Uani 1 1 d . . . H35A H 1.2168 0.6813 1.1165 0.060 Uiso 1 1 calc R . . C36 C 1.0456(4) 0.7080(4) 1.09800(14) 0.0400(11) Uani 1 1 d . . . H36A H 1.0274 0.7287 1.1236 0.048 Uiso 1 1 calc R . . N25 N 1.1099(12) 0.7968(6) 0.8457(2) 0.185(5) Uani 1 1 d . . . C37 C 1.1291(9) 0.8091(10) 0.7686(3) 0.158(5) Uani 1 1 d . . . H37A H 1.1950 0.7685 0.7618 0.237 Uiso 1 1 calc R . . H37B H 1.1359 0.8863 0.7614 0.237 Uiso 1 1 calc R . . H37C H 1.0594 0.7786 0.7537 0.237 Uiso 1 1 calc R . . C38 C 1.1243(9) 0.7998(7) 0.8126(3) 0.115(3) Uani 1 1 d . . . N26 N 0.1581(4) 0.3065(5) 0.80874(19) 0.0671(14) Uani 1 1 d . . . N27 N -0.3423(7) 0.2487(6) 0.80231(16) 0.144(4) Uani 1 1 d D . . O1 O 0.1571(5) 0.2258(4) 0.78598(15) 0.0914(15) Uani 1 1 d . . . O2 O 0.1342(6) 0.4013(5) 0.7950(2) 0.129(2) Uani 1 1 d . . . O3 O 0.1816(5) 0.2960(5) 0.84557(17) 0.0985(16) Uani 1 1 d . . . O4 O -0.4134(11) 0.2393(15) 0.8260(3) 0.514(7) Uani 1 1 d D . . O5 O -0.2588(9) 0.3098(9) 0.8108(2) 0.407(13) Uani 1 1 d D . . O6 O -0.3580(7) 0.2021(5) 0.76915(15) 0.161(3) Uani 1 1 d D . . O7 O -0.0994(5) 0.3060(5) 0.75531(18) 0.127(2) 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 0.0296(3) 0.0303(3) 0.0482(4) -0.0009(2) 0.0171(3) -0.0012(2) Cu2 0.0239(3) 0.0405(3) 0.0575(4) -0.0155(3) 0.0119(3) -0.0048(2) Cu3 0.0309(3) 0.0381(3) 0.0471(4) 0.0007(2) -0.0007(3) 0.0019(2) N1 0.049(3) 0.055(3) 0.042(2) 0.006(2) 0.011(2) 0.003(2) N2 0.051(3) 0.055(3) 0.061(3) 0.003(2) 0.023(2) -0.013(2) N3 0.031(2) 0.038(2) 0.038(2) 0.0038(17) 0.0094(17) -0.0030(16) N4 0.0246(19) 0.0350(19) 0.037(2) -0.0006(16) 0.0067(16) -0.0004(15) N5 0.036(2) 0.034(2) 0.045(2) 0.0004(17) 0.0077(18) -0.0064(16) N6 0.0270(19) 0.0312(18) 0.035(2) -0.0028(15) 0.0078(16) -0.0018(15) N7 0.032(2) 0.041(2) 0.035(2) 0.0002(17) 0.0056(17) 0.0018(16) N8 0.042(2) 0.057(3) 0.049(2) -0.001(2) 0.007(2) -0.019(2) N9 0.0223(18) 0.036(2) 0.035(2) 0.0026(16) 0.0068(16) 0.0004(15) N10 0.0243(18) 0.0303(18) 0.039(2) 0.0026(15) 0.0087(17) -0.0009(14) N11 0.0259(19) 0.033(2) 0.044(2) 0.0027(16) 0.0087(17) -0.0034(15) N12 0.0266(19) 0.0377(19) 0.037(2) 0.0016(16) 0.0091(17) 0.0035(15) N13 0.038(2) 0.042(2) 0.042(2) 0.0058(18) 0.0091(19) 0.0010(17) N14 0.037(2) 0.055(3) 0.057(3) 0.001(2) 0.007(2) 0.010(2) N15 0.0251(19) 0.038(2) 0.039(2) 0.0024(16) 0.0077(17) 0.0011(15) N16 0.0274(19) 0.0326(19) 0.033(2) 0.0022(15) 0.0083(16) 0.0000(15) N17 0.024(2) 0.040(2) 0.051(3) -0.0006(18) 0.0146(18) 0.0000(16) N18 0.029(2) 0.0332(19) 0.039(2) 0.0005(16) 0.0093(17) -0.0011(15) N19 0.035(2) 0.040(2) 0.032(2) -0.0014(16) 0.0033(17) -0.0002(16) N20 0.041(2) 0.050(2) 0.037(2) -0.0018(18) 0.0081(19) 0.0116(19) N21 0.0279(19) 0.0319(19) 0.032(2) -0.0016(15) 0.0049(16) -0.0019(15) N22 0.0258(19) 0.0340(19) 0.032(2) -0.0028(15) 0.0057(16) -0.0021(15) N23 0.023(2) 0.050(2) 0.040(2) -0.0039(17) 0.0070(17) 0.0025(16) N24 0.031(2) 0.042(2) 0.032(2) -0.0031(16) 0.0101(17) -0.0015(16) C1 0.064(4) 0.074(4) 0.047(3) 0.006(3) 0.014(3) 0.009(3) C2 0.081(5) 0.080(4) 0.067(4) 0.024(3) 0.035(4) 0.002(4) C3 0.067(4) 0.071(4) 0.078(4) 0.011(3) 0.036(4) -0.016(3) C4 0.042(3) 0.040(3) 0.039(3) 0.007(2) 0.014(2) 0.004(2) C5 0.025(2) 0.035(2) 0.045(3) -0.003(2) 0.012(2) 0.0001(18) C6 0.018(2) 0.033(2) 0.040(3) -0.0039(19) 0.0044(19) -0.0002(17) C7 0.038(3) 0.035(2) 0.056(3) -0.006(2) 0.008(2) -0.008(2) C8 0.051(3) 0.042(3) 0.042(3) -0.014(2) 0.007(2) -0.002(2) C9 0.036(3) 0.045(3) 0.037(3) 0.000(2) 0.009(2) 0.000(2) C10 0.037(3) 0.060(3) 0.040(3) 0.000(2) -0.004(2) 0.001(2) C11 0.052(3) 0.075(4) 0.047(3) -0.007(3) -0.005(3) -0.013(3) C12 0.055(3) 0.067(4) 0.058(3) -0.006(3) 0.006(3) -0.028(3) C13 0.027(2) 0.039(2) 0.039(3) 0.000(2) 0.011(2) 0.0013(19) C14 0.021(2) 0.037(2) 0.044(3) 0.001(2) 0.013(2) 0.0013(18) C15 0.018(2) 0.031(2) 0.043(3) -0.0009(19) 0.0145(19) 0.0010(17) C16 0.033(2) 0.036(2) 0.057(3) 0.007(2) 0.013(2) -0.004(2) C17 0.040(3) 0.047(3) 0.047(3) 0.015(2) 0.008(2) 0.003(2) C18 0.035(3) 0.052(3) 0.039(3) -0.002(2) 0.008(2) 0.004(2) C19 0.065(4) 0.059(3) 0.049(3) 0.015(3) 0.009(3) 0.007(3) C20 0.069(4) 0.074(4) 0.054(4) 0.018(3) 0.002(3) 0.025(3) C21 0.046(3) 0.068(4) 0.070(4) 0.004(3) 0.002(3) 0.021(3) C22 0.030(2) 0.034(2) 0.049(3) -0.004(2) 0.009(2) -0.0035(19) C23 0.023(2) 0.031(2) 0.053(3) -0.003(2) 0.005(2) 0.0008(18) C24 0.029(2) 0.025(2) 0.048(3) -0.0023(19) 0.006(2) -0.0040(18) C25 0.031(3) 0.045(3) 0.061(3) -0.013(2) 0.017(3) 0.002(2) C26 0.042(3) 0.054(3) 0.047(3) -0.005(2) 0.024(2) -0.006(2) C27 0.036(3) 0.044(3) 0.042(3) -0.002(2) 0.005(2) 0.000(2) C28 0.049(3) 0.053(3) 0.033(3) 0.001(2) 0.003(2) 0.008(2) C29 0.062(4) 0.063(3) 0.035(3) -0.006(2) 0.012(3) 0.009(3) C30 0.052(3) 0.068(3) 0.043(3) -0.011(2) 0.013(3) 0.018(3) C31 0.023(2) 0.037(2) 0.034(2) -0.0017(19) 0.0068(19) -0.0005(18) C32 0.022(2) 0.030(2) 0.039(3) 0.0004(18) 0.009(2) -0.0022(17) C33 0.029(2) 0.031(2) 0.032(2) -0.0014(18) 0.006(2) -0.0049(18) C34 0.025(2) 0.061(3) 0.045(3) -0.005(2) 0.005(2) 0.006(2) C35 0.038(3) 0.065(3) 0.044(3) 0.000(2) -0.008(2) -0.007(2) C36 0.044(3) 0.049(3) 0.029(2) -0.001(2) 0.011(2) -0.004(2) N25 0.375(17) 0.093(5) 0.071(5) -0.003(4) -0.023(7) -0.001(7) C37 0.127(9) 0.253(14) 0.101(7) -0.022(8) 0.039(6) 0.059(9) C38 0.166(9) 0.084(5) 0.085(6) -0.011(5) -0.021(6) 0.016(5) N26 0.045(3) 0.076(4) 0.079(4) -0.013(3) 0.008(3) -0.013(3) N27 0.230(11) 0.153(7) 0.049(4) -0.023(4) 0.017(5) -0.087(7) O1 0.110(4) 0.090(3) 0.076(3) -0.023(3) 0.022(3) -0.017(3) O2 0.128(5) 0.087(4) 0.168(6) 0.006(4) 0.003(4) 0.027(4) O3 0.093(4) 0.123(4) 0.083(4) -0.027(3) 0.023(3) -0.021(3) O4 0.68(2) 0.74(2) 0.170(10) -0.238(12) 0.222(12) -0.511 O5 0.81(4) 0.281(13) 0.083(6) 0.024(6) -0.116(11) -0.254(18) O6 0.250(9) 0.159(6) 0.077(4) -0.020(4) 0.034(5) -0.033(6) O7 0.117(5) 0.140(5) 0.117(4) 0.010(4) -0.005(4) 0.038(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 N18 1.989(4) . ? Cu1 N22 2.000(4) . ? Cu1 N6 2.035(3) . ? Cu1 N12 2.086(4) . ? Cu1 N10 2.461(3) . ? Cu1 Cu2 2.8319(8) . ? Cu2 N4 1.992(3) . ? Cu2 N21 2.011(4) . ? Cu2 N9 2.039(3) . ? Cu2 N16 2.136(4) . ? Cu2 N15 2.388(3) . ? Cu2 Cu3 2.7625(8) . ? Cu3 N19 2.011(4) . ? Cu3 N3 2.020(4) . ? Cu3 N7 2.022(4) . ? Cu3 N13 2.030(4) . ? N1 C4 1.323(6) . ? N1 C1 1.348(6) . ? N2 C4 1.329(6) . ? N2 C3 1.332(7) . ? N3 C5 1.303(5) . ? N3 C4 1.410(6) . ? N4 C5 1.342(5) . ? N4 C6 1.385(5) . ? N5 C7 1.326(6) . ? N5 C6 1.340(5) . ? N6 C9 1.337(5) . ? N6 C6 1.351(5) . ? N7 C10 1.354(5) . ? N7 C13 1.355(5) . ? N8 C12 1.319(6) . ? N8 C13 1.337(6) . ? N9 C14 1.331(5) . ? N9 C13 1.376(5) . ? N10 C14 1.297(5) . ? N10 C15 1.367(5) . ? N11 C15 1.333(5) . ? N11 C16 1.337(5) . ? N12 C18 1.330(5) . ? N12 C15 1.357(5) . ? N13 C22 1.335(6) . ? N13 C19 1.351(6) . ? N14 C21 1.331(6) . ? N14 C22 1.332(6) . ? N15 C23 1.288(6) . ? N15 C22 1.387(5) . ? N16 C23 1.330(5) . ? N16 C24 1.366(6) . ? N17 C25 1.328(6) . ? N17 C24 1.332(6) . ? N18 C27 1.332(6) . ? N18 C24 1.367(5) . ? N19 C28 1.340(6) . ? N19 C31 1.359(5) . ? N20 C30 1.325(6) . ? N20 C31 1.342(5) . ? N21 C32 1.327(5) . ? N21 C31 1.391(5) . ? N22 C32 1.302(5) . ? N22 C33 1.403(5) . ? N23 C33 1.330(5) . ? N23 C34 1.335(5) . ? N24 C33 1.319(5) . ? N24 C36 1.333(6) . ? C1 C2 1.366(8) . ? C2 C3 1.349(8) . ? C7 C8 1.372(6) . ? C8 C9 1.361(6) . ? C10 C11 1.354(7) . ? C11 C12 1.382(7) . ? C16 C17 1.378(7) . ? C17 C18 1.369(6) . ? C19 C20 1.370(8) . ? C20 C21 1.358(8) . ? C25 C26 1.378(7) . ? C26 C27 1.389(7) . ? C28 C29 1.362(7) . ? C29 C30 1.367(7) . ? C34 C35 1.363(7) . ? C35 C36 1.373(7) . ? N25 C38 1.125(11) . ? C37 C38 1.460(12) . ? N26 O3 1.212(7) . ? N26 O1 1.221(6) . ? N26 O2 1.240(7) . ? N27 O4 1.2162(9) . ? N27 O6 1.2166(9) . ? N27 O5 1.2172(9) . ? 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 N18 Cu1 N22 170.21(14) . . ? N18 Cu1 N6 89.57(14) . . ? N22 Cu1 N6 91.64(14) . . ? N18 Cu1 N12 90.17(14) . . ? N22 Cu1 N12 91.48(14) . . ? N6 Cu1 N12 163.13(14) . . ? N18 Cu1 N10 86.05(13) . . ? N22 Cu1 N10 86.62(12) . . ? N6 Cu1 N10 138.55(12) . . ? N12 Cu1 N10 58.22(12) . . ? N18 Cu1 Cu2 94.89(10) . . ? N22 Cu1 Cu2 75.69(10) . . ? N6 Cu1 Cu2 81.62(10) . . ? N12 Cu1 Cu2 115.21(10) . . ? N10 Cu1 Cu2 57.82(8) . . ? N4 Cu2 N21 89.51(14) . . ? N4 Cu2 N9 167.95(14) . . ? N21 Cu2 N9 89.87(13) . . ? N4 Cu2 N16 90.11(14) . . ? N21 Cu2 N16 157.57(13) . . ? N9 Cu2 N16 95.01(13) . . ? N4 Cu2 N15 87.19(13) . . ? N21 Cu2 N15 143.97(13) . . ? N9 Cu2 N15 86.24(13) . . ? N16 Cu2 N15 58.37(13) . . ? N4 Cu2 Cu3 91.17(10) . . ? N21 Cu2 Cu3 83.99(10) . . ? N9 Cu2 Cu3 76.80(10) . . ? N16 Cu2 Cu3 118.44(9) . . ? N15 Cu2 Cu3 60.24(9) . . ? N4 Cu2 Cu1 82.11(10) . . ? N21 Cu2 Cu1 88.02(10) . . ? N9 Cu2 Cu1 109.90(10) . . ? N16 Cu2 Cu1 69.73(9) . . ? N15 Cu2 Cu1 126.87(9) . . ? Cu3 Cu2 Cu1 169.60(3) . . ? N19 Cu3 N3 90.23(15) . . ? N19 Cu3 N7 88.62(15) . . ? N3 Cu3 N7 164.20(14) . . ? N19 Cu3 N13 168.38(15) . . ? N3 Cu3 N13 95.44(15) . . ? N7 Cu3 N13 88.64(15) . . ? N19 Cu3 Cu2 82.45(10) . . ? N3 Cu3 Cu2 74.73(10) . . ? N7 Cu3 Cu2 89.51(10) . . ? N13 Cu3 Cu2 108.82(11) . . ? C4 N1 C1 115.3(5) . . ? C4 N2 C3 113.1(5) . . ? C5 N3 C4 119.7(4) . . ? C5 N3 Cu3 134.9(3) . . ? C4 N3 Cu3 105.4(3) . . ? C5 N4 C6 117.3(4) . . ? C5 N4 Cu2 115.6(3) . . ? C6 N4 Cu2 127.1(3) . . ? C7 N5 C6 116.6(4) . . ? C9 N6 C6 116.7(4) . . ? C9 N6 Cu1 116.0(3) . . ? C6 N6 Cu1 127.0(3) . . ? C10 N7 C13 116.9(4) . . ? C10 N7 Cu3 122.3(3) . . ? C13 N7 Cu3 120.5(3) . . ? C12 N8 C13 116.9(4) . . ? C14 N9 C13 119.7(4) . . ? C14 N9 Cu2 105.6(3) . . ? C13 N9 Cu2 134.6(3) . . ? C14 N10 C15 123.2(4) . . ? C14 N10 Cu1 149.7(3) . . ? C15 N10 Cu1 87.1(2) . . ? C15 N11 C16 115.0(4) . . ? C18 N12 C15 117.5(4) . . ? C18 N12 Cu1 138.1(3) . . ? C15 N12 Cu1 104.3(3) . . ? C22 N13 C19 117.9(4) . . ? C22 N13 Cu3 109.5(3) . . ? C19 N13 Cu3 132.2(4) . . ? C21 N14 C22 114.8(4) . . ? C23 N15 C22 123.1(4) . . ? C23 N15 Cu2 87.8(3) . . ? C22 N15 Cu2 149.0(3) . . ? C23 N16 C24 121.1(4) . . ? C23 N16 Cu2 98.1(3) . . ? C24 N16 Cu2 140.6(3) . . ? C25 N17 C24 116.3(4) . . ? C27 N18 C24 117.5(4) . . ? C27 N18 Cu1 125.3(3) . . ? C24 N18 Cu1 117.3(3) . . ? C28 N19 C31 117.3(4) . . ? C28 N19 Cu3 114.4(3) . . ? C31 N19 Cu3 128.0(3) . . ? C30 N20 C31 116.8(4) . . ? C32 N21 C31 117.5(4) . . ? C32 N21 Cu2 117.4(3) . . ? C31 N21 Cu2 125.1(3) . . ? C32 N22 C33 121.6(4) . . ? C32 N22 Cu1 133.2(3) . . ? C33 N22 Cu1 105.1(3) . . ? C33 N23 C34 114.3(4) . . ? C33 N24 C36 116.5(4) . . ? N1 C1 C2 120.8(5) . . ? C3 C2 C1 118.0(6) . . ? N2 C3 C2 124.0(6) . . ? N1 C4 N2 128.8(5) . . ? N1 C4 N3 110.7(4) . . ? N2 C4 N3 120.5(4) . . ? N3 C5 N4 121.1(4) . . ? N5 C6 N6 124.2(4) . . ? N5 C6 N4 119.1(4) . . ? N6 C6 N4 116.8(4) . . ? N5 C7 C8 123.4(4) . . ? C9 C8 C7 116.1(4) . . ? N6 C9 C8 122.9(4) . . ? N7 C10 C11 122.0(5) . . ? C10 C11 C12 116.6(5) . . ? N8 C12 C11 123.4(5) . . ? N8 C13 N7 124.0(4) . . ? N8 C13 N9 120.2(4) . . ? N7 C13 N9 115.8(4) . . ? N10 C14 N9 116.2(4) . . ? N11 C15 N12 125.3(4) . . ? N11 C15 N10 124.2(4) . . ? N12 C15 N10 110.4(3) . . ? N11 C16 C17 123.9(4) . . ? C18 C17 C16 116.8(4) . . ? N12 C18 C17 121.4(4) . . ? N13 C19 C20 119.7(5) . . ? C21 C20 C19 117.7(5) . . ? N14 C21 C20 124.2(5) . . ? N14 C22 N13 125.7(4) . . ? N14 C22 N15 122.9(4) . . ? N13 C22 N15 111.4(4) . . ? N15 C23 N16 115.7(4) . . ? N17 C24 N16 121.5(4) . . ? N17 C24 N18 124.0(4) . . ? N16 C24 N18 114.4(4) . . ? N17 C25 C26 124.6(4) . . ? C25 C26 C27 115.3(5) . . ? N18 C27 C26 122.1(4) . . ? N19 C28 C29 122.0(4) . . ? C28 C29 C30 116.7(5) . . ? N20 C30 C29 123.5(5) . . ? N20 C31 N19 123.5(4) . . ? N20 C31 N21 120.0(4) . . ? N19 C31 N21 116.5(4) . . ? N22 C32 N21 122.6(4) . . ? N24 C33 N23 126.9(4) . . ? N24 C33 N22 112.3(4) . . ? N23 C33 N22 120.7(4) . . ? N23 C34 C35 124.3(4) . . ? C34 C35 C36 115.9(4) . . ? N24 C36 C35 122.1(4) . . ? N25 C38 C37 173.2(12) . . ? O3 N26 O1 120.9(6) . . ? O3 N26 O2 117.9(6) . . ? O1 N26 O2 121.2(7) . . ? O4 N27 O6 119.99(12) . . ? O4 N27 O5 119.95(12) . . ? O6 N27 O5 119.92(12) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.364 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.084 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 662458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 Cl2 Cu3 N25 O8' _chemical_formula_weight 1227.40 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7753(15) _cell_length_b 11.9599(14) _cell_length_c 33.318(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.027(3) _cell_angle_gamma 90.00 _cell_volume 4634.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3229 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.10 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2476 _exptl_absorpt_coefficient_mu 1.563 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8594 _exptl_absorpt_correction_T_max 0.9845 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 11913 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7852 _reflns_number_gt 5427 _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^)+(0.0878P)^2^+0.9298P] 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 7852 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.26088(5) 0.72608(5) 1.023220(18) 0.03598(15) Uani 1 1 d . . . Cu2 Cu 0.18435(5) 0.76394(5) 0.93959(2) 0.04032(17) Uani 1 1 d . . . Cu3 Cu 0.15134(5) 0.80302(5) 0.857790(19) 0.03744(16) Uani 1 1 d . . . N1 N 0.2599(4) 0.9097(3) 0.81277(12) 0.0426(11) Uani 1 1 d . . . N2 N 0.4012(4) 1.0288(4) 0.85119(14) 0.0520(12) Uani 1 1 d . . . N3 N 0.2715(3) 0.9147(3) 0.88123(11) 0.0328(9) Uani 1 1 d . . . N4 N 0.2789(3) 0.9033(3) 0.95060(11) 0.0290(9) Uani 1 1 d . . . N5 N 0.3516(3) 1.0585(3) 0.98928(12) 0.0386(10) Uani 1 1 d . . . N6 N 0.3009(3) 0.8923(3) 1.02135(11) 0.0321(9) Uani 1 1 d . . . N7 N 0.0351(3) 0.6802(3) 0.84969(12) 0.0345(9) Uani 1 1 d . . . N8 N -0.0407(3) 0.5140(4) 0.87485(13) 0.0463(11) Uani 1 1 d . . . N9 N 0.0855(3) 0.6320(3) 0.91728(11) 0.0315(9) Uani 1 1 d . . . N10 N 0.1542(3) 0.5843(3) 0.98168(11) 0.0296(9) Uani 1 1 d . . . N11 N 0.1493(3) 0.4029(3) 1.01194(12) 0.0370(10) Uani 1 1 d . . . N12 N 0.2468(3) 0.5606(3) 1.04534(11) 0.0335(9) Uani 1 1 d . . . N13 N 0.0211(3) 0.9178(3) 0.84462(12) 0.0368(10) Uani 1 1 d . . . N14 N -0.1222(4) 0.9960(4) 0.87905(14) 0.0524(12) Uani 1 1 d . . . N15 N 0.0288(3) 0.8795(3) 0.91155(12) 0.0337(9) Uani 1 1 d . . . N16 N 0.0617(3) 0.8280(3) 0.97590(12) 0.0353(9) Uani 1 1 d . . . N17 N -0.0683(3) 0.8555(3) 1.02253(13) 0.0408(10) Uani 1 1 d . . . N18 N 0.1129(3) 0.7655(3) 1.04162(11) 0.0325(9) Uani 1 1 d . . . N19 N 0.2746(3) 0.6833(3) 0.85864(11) 0.0336(9) Uani 1 1 d . . . N20 N 0.4292(3) 0.5697(4) 0.88903(12) 0.0416(10) Uani 1 1 d . . . N21 N 0.3266(3) 0.6800(3) 0.92954(11) 0.0282(8) Uani 1 1 d . . . N22 N 0.3972(3) 0.6846(3) 0.99826(11) 0.0316(9) Uani 1 1 d . . . N23 N 0.5942(3) 0.6457(4) 1.02187(12) 0.0394(10) Uani 1 1 d . . . N24 N 0.4643(3) 0.7112(3) 1.06542(12) 0.0384(10) Uani 1 1 d . . . C1 C 0.2977(5) 0.9420(5) 0.77861(16) 0.0566(16) Uani 1 1 d . . . H1B H 0.2632 0.9125 0.7539 0.068 Uiso 1 1 calc R . . C2 C 0.3846(6) 1.0166(6) 0.7792(2) 0.0712(19) Uani 1 1 d . . . H2B H 0.4098 1.0389 0.7553 0.085 Uiso 1 1 calc R . . C3 C 0.4344(5) 1.0581(5) 0.8163(2) 0.0660(18) Uani 1 1 d . . . H3B H 0.4943 1.1092 0.8171 0.079 Uiso 1 1 calc R . . C4 C 0.3147(4) 0.9562(4) 0.84736(14) 0.0365(12) Uani 1 1 d . . . C5 C 0.3101(4) 0.9518(4) 0.91742(14) 0.0347(11) Uani 1 1 d . . . H5B H 0.3600 1.0125 0.9205 0.042 Uiso 1 1 calc R . . C6 C 0.3119(4) 0.9530(4) 0.98791(14) 0.0311(11) Uani 1 1 d . . . C7 C 0.3794(4) 1.1038(4) 1.02551(16) 0.0452(13) Uani 1 1 d . . . H7B H 0.4081 1.1764 1.0271 0.054 Uiso 1 1 calc R . . C8 C 0.3683(5) 1.0495(5) 1.06108(16) 0.0492(14) Uani 1 1 d . . . H8B H 0.3871 1.0838 1.0863 0.059 Uiso 1 1 calc R . . C9 C 0.3283(4) 0.9430(4) 1.05731(14) 0.0412(12) Uani 1 1 d . . . H9A H 0.3195 0.9037 1.0807 0.049 Uiso 1 1 calc R . . C10 C -0.0270(4) 0.6594(4) 0.81288(16) 0.0437(13) Uani 1 1 d . . . H10A H -0.0225 0.7092 0.7918 0.052 Uiso 1 1 calc R . . C11 C -0.0965(5) 0.5672(5) 0.80552(17) 0.0541(15) Uani 1 1 d . . . H11A H -0.1404 0.5543 0.7802 0.065 Uiso 1 1 calc R . . C12 C -0.0977(5) 0.4951(5) 0.83752(18) 0.0552(15) Uani 1 1 d . . . H12A H -0.1405 0.4297 0.8330 0.066 Uiso 1 1 calc R . . C13 C 0.0235(4) 0.6065(4) 0.87986(14) 0.0333(11) Uani 1 1 d . . . C14 C 0.0935(4) 0.5563(4) 0.94706(14) 0.0332(11) Uani 1 1 d . . . H14A H 0.0576 0.4870 0.9433 0.040 Uiso 1 1 calc R . . C15 C 0.1809(4) 0.5109(4) 1.01352(14) 0.0321(11) Uani 1 1 d . . . C16 C 0.1913(4) 0.3429(4) 1.04422(17) 0.0470(14) Uani 1 1 d . . . H16A H 0.1727 0.2674 1.0442 0.056 Uiso 1 1 calc R . . C17 C 0.2612(5) 0.3857(5) 1.07791(17) 0.0509(14) Uani 1 1 d . . . H17A H 0.2903 0.3408 1.0999 0.061 Uiso 1 1 calc R . . C18 C 0.2857(4) 0.4989(5) 1.07725(16) 0.0466(14) Uani 1 1 d . . . H18A H 0.3302 0.5317 1.0997 0.056 Uiso 1 1 calc R . . C19 C -0.0242(5) 0.9680(4) 0.81028(16) 0.0474(14) Uani 1 1 d . . . H19A H 0.0091 0.9581 0.7870 0.057 Uiso 1 1 calc R . . C20 C -0.1198(5) 1.0341(5) 0.80885(18) 0.0556(15) Uani 1 1 d . . . H20A H -0.1519 1.0705 0.7851 0.067 Uiso 1 1 calc R . . C21 C -0.1666(5) 1.0445(5) 0.84425(18) 0.0604(17) Uani 1 1 d . . . H21A H -0.2325 1.0877 0.8437 0.073 Uiso 1 1 calc R . . C22 C -0.0281(4) 0.9338(4) 0.87759(15) 0.0363(12) Uani 1 1 d . . . C23 C -0.0043(4) 0.8836(4) 0.94691(15) 0.0346(11) Uani 1 1 d . . . H23A H -0.0693 0.9227 0.9515 0.042 Uiso 1 1 calc R . . C24 C 0.0334(4) 0.8169(4) 1.01417(14) 0.0312(11) Uani 1 1 d . . . C25 C -0.0901(4) 0.8351(4) 1.05995(16) 0.0434(13) Uani 1 1 d . . . H25A H -0.1586 0.8617 1.0669 0.052 Uiso 1 1 calc R . . C26 C -0.0168(5) 0.7767(5) 1.08886(17) 0.0489(14) Uani 1 1 d . . . H26A H -0.0366 0.7599 1.1141 0.059 Uiso 1 1 calc R . . C27 C 0.0869(4) 0.7443(4) 1.07859(16) 0.0425(13) Uani 1 1 d . . . H27A H 0.1398 0.7071 1.0976 0.051 Uiso 1 1 calc R . . C28 C 0.2914(4) 0.6473(4) 0.82200(15) 0.0423(13) Uani 1 1 d . . . H28A H 0.2443 0.6740 0.7990 0.051 Uiso 1 1 calc R . . C29 C 0.3756(5) 0.5726(4) 0.81749(15) 0.0455(13) Uani 1 1 d . . . H29A H 0.3867 0.5478 0.7919 0.055 Uiso 1 1 calc R . . C30 C 0.4427(5) 0.5357(5) 0.85184(16) 0.0502(14) Uani 1 1 d . . . H30A H 0.5006 0.4844 0.8494 0.060 Uiso 1 1 calc R . . C31 C 0.3449(4) 0.6432(4) 0.89125(14) 0.0313(11) Uani 1 1 d . . . C32 C 0.4097(4) 0.6606(4) 0.96043(14) 0.0297(10) Uani 1 1 d . . . H32A H 0.4784 0.6292 0.9554 0.036 Uiso 1 1 calc R . . C33 C 0.4909(4) 0.6779(4) 1.02928(14) 0.0306(11) Uani 1 1 d . . . C34 C 0.6788(4) 0.6511(5) 1.05421(16) 0.0480(14) Uani 1 1 d . . . H34A H 0.7528 0.6306 1.0508 0.058 Uiso 1 1 calc R . . C35 C 0.6602(5) 0.6854(5) 1.09202(17) 0.0540(15) Uani 1 1 d . . . H35A H 0.7200 0.6882 1.1139 0.065 Uiso 1 1 calc R . . C36 C 0.5512(4) 0.7151(4) 1.09637(16) 0.0442(13) Uani 1 1 d . . . H36A H 0.5369 0.7388 1.1217 0.053 Uiso 1 1 calc R . . C37 C 0.6306(8) 0.7803(12) 0.7816(3) 0.174(6) Uani 1 1 d . . . H37A H 0.5725 0.7363 0.7653 0.261 Uiso 1 1 calc R . . H37B H 0.7040 0.7447 0.7825 0.261 Uiso 1 1 calc R . . H37C H 0.6329 0.8534 0.7698 0.261 Uiso 1 1 calc R . . C38 C 0.6048(10) 0.7898(8) 0.8206(3) 0.119(4) Uani 1 1 d . . . N25 N 0.5747(11) 0.7952(7) 0.8515(3) 0.163(4) Uani 1 1 d . . . Cl1 Cl 0.62597(12) 0.31946(12) 0.79617(4) 0.0545(4) Uani 1 1 d . . . Cl2 Cl 0.14278(15) 0.24229(15) 0.80548(5) 0.0676(4) Uani 1 1 d . . . O1 O 0.5061(4) 0.3226(5) 0.78259(19) 0.109(2) Uani 1 1 d . . . O2 O 0.6722(6) 0.4150(6) 0.7831(2) 0.168(3) Uani 1 1 d . . . O3 O 0.6502(5) 0.3084(5) 0.83842(14) 0.0905(16) Uani 1 1 d . . . O4 O 0.6655(6) 0.2239(6) 0.77866(19) 0.146(3) Uani 1 1 d . . . O5 O 0.0498(8) 0.3063(7) 0.80873(19) 0.209(4) Uani 1 1 d . . . O6 O 0.1279(6) 0.1943(6) 0.76747(15) 0.121(2) Uani 1 1 d . . . O7 O 0.1593(4) 0.1642(4) 0.83751(13) 0.0761(13) Uani 1 1 d . . . O8 O 0.2377(9) 0.3122(9) 0.8093(2) 0.268(5) 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 0.0407(3) 0.0263(3) 0.0451(4) -0.0009(3) 0.0197(3) -0.0020(2) Cu2 0.0326(3) 0.0330(3) 0.0571(4) -0.0165(3) 0.0125(3) -0.0056(3) Cu3 0.0367(3) 0.0293(3) 0.0437(4) 0.0005(3) -0.0017(3) 0.0010(2) N1 0.057(3) 0.039(2) 0.032(2) -0.0002(19) 0.006(2) 0.009(2) N2 0.057(3) 0.045(3) 0.059(3) 0.007(2) 0.025(2) -0.009(2) N3 0.039(2) 0.032(2) 0.026(2) 0.0001(17) 0.0017(17) -0.0029(17) N4 0.0314(18) 0.027(2) 0.027(2) -0.0030(16) 0.0014(16) -0.0017(16) N5 0.045(2) 0.031(2) 0.040(2) -0.0031(19) 0.0090(19) -0.0104(18) N6 0.039(2) 0.026(2) 0.032(2) -0.0036(17) 0.0086(17) 0.0001(16) N7 0.038(2) 0.027(2) 0.036(2) 0.0000(18) -0.0004(18) -0.0009(17) N8 0.045(2) 0.042(3) 0.048(3) 0.003(2) -0.002(2) -0.012(2) N9 0.0305(19) 0.030(2) 0.033(2) 0.0018(18) 0.0020(17) 0.0010(16) N10 0.0314(19) 0.0262(19) 0.031(2) 0.0041(17) 0.0048(17) -0.0022(16) N11 0.038(2) 0.030(2) 0.043(2) 0.0058(19) 0.0050(18) -0.0040(17) N12 0.035(2) 0.034(2) 0.031(2) -0.0017(18) 0.0044(17) 0.0002(17) N13 0.040(2) 0.033(2) 0.036(2) 0.0010(19) 0.0029(18) -0.0004(18) N14 0.050(3) 0.051(3) 0.056(3) -0.003(2) 0.006(2) 0.018(2) N15 0.0317(19) 0.028(2) 0.040(2) -0.0011(18) 0.0023(18) -0.0009(16) N16 0.035(2) 0.033(2) 0.040(2) -0.0003(19) 0.0115(18) -0.0001(17) N17 0.040(2) 0.036(2) 0.048(3) -0.003(2) 0.0130(19) -0.0010(18) N18 0.039(2) 0.028(2) 0.032(2) -0.0094(17) 0.0112(17) -0.0079(17) N19 0.0352(19) 0.034(2) 0.030(2) -0.0024(18) -0.0005(17) 0.0028(17) N20 0.045(2) 0.046(3) 0.034(2) -0.005(2) 0.0053(19) 0.017(2) N21 0.0327(19) 0.0264(19) 0.025(2) -0.0003(16) 0.0042(16) -0.0033(16) N22 0.0316(19) 0.034(2) 0.030(2) -0.0045(17) 0.0050(16) -0.0049(16) N23 0.035(2) 0.046(2) 0.037(2) -0.001(2) 0.0043(18) 0.0039(19) N24 0.044(2) 0.042(2) 0.030(2) 0.0013(19) 0.0075(18) -0.0026(19) C1 0.077(4) 0.065(4) 0.029(3) 0.003(3) 0.013(3) 0.017(3) C2 0.083(4) 0.082(5) 0.057(4) 0.022(4) 0.039(3) 0.003(4) C3 0.066(4) 0.060(4) 0.079(5) 0.015(3) 0.032(3) -0.012(3) C4 0.045(3) 0.029(3) 0.037(3) 0.007(2) 0.012(2) 0.006(2) C5 0.031(2) 0.034(3) 0.040(3) -0.001(2) 0.009(2) -0.002(2) C6 0.029(2) 0.031(2) 0.033(3) -0.002(2) 0.0054(19) -0.0017(19) C7 0.056(3) 0.037(3) 0.043(3) -0.007(2) 0.007(3) -0.008(2) C8 0.061(3) 0.045(3) 0.039(3) -0.014(3) 0.002(3) -0.004(3) C9 0.056(3) 0.041(3) 0.028(3) -0.003(2) 0.010(2) -0.004(2) C10 0.047(3) 0.046(3) 0.035(3) 0.000(2) -0.005(2) -0.005(2) C11 0.060(3) 0.055(4) 0.043(3) -0.002(3) -0.007(3) -0.013(3) C12 0.059(3) 0.048(3) 0.056(4) -0.006(3) 0.000(3) -0.017(3) C13 0.036(2) 0.031(3) 0.032(3) 0.003(2) 0.004(2) 0.004(2) C14 0.033(2) 0.028(2) 0.040(3) 0.005(2) 0.011(2) -0.0012(19) C15 0.029(2) 0.028(2) 0.040(3) 0.001(2) 0.012(2) -0.0019(19) C16 0.049(3) 0.037(3) 0.055(4) 0.015(3) 0.009(3) -0.006(2) C17 0.053(3) 0.050(3) 0.049(3) 0.016(3) 0.004(3) 0.003(3) C18 0.042(3) 0.052(3) 0.044(3) 0.000(3) 0.003(2) 0.004(3) C19 0.056(3) 0.045(3) 0.040(3) 0.006(3) 0.004(3) -0.001(3) C20 0.061(3) 0.054(3) 0.047(3) 0.013(3) -0.006(3) 0.010(3) C21 0.048(3) 0.075(4) 0.055(4) 0.003(3) -0.004(3) 0.022(3) C22 0.037(2) 0.032(3) 0.039(3) -0.004(2) 0.003(2) -0.005(2) C23 0.030(2) 0.030(3) 0.043(3) 0.004(2) 0.004(2) 0.003(2) C24 0.035(2) 0.020(2) 0.038(3) -0.002(2) 0.006(2) -0.0034(19) C25 0.040(3) 0.039(3) 0.055(3) -0.006(3) 0.020(2) -0.002(2) C26 0.057(3) 0.050(3) 0.047(3) -0.004(3) 0.031(3) -0.003(3) C27 0.049(3) 0.039(3) 0.041(3) 0.002(2) 0.011(2) 0.000(2) C28 0.053(3) 0.038(3) 0.034(3) 0.003(2) 0.003(2) 0.002(2) C29 0.061(3) 0.050(3) 0.027(3) -0.007(2) 0.012(2) 0.007(3) C30 0.058(3) 0.051(3) 0.042(3) -0.003(3) 0.010(3) 0.024(3) C31 0.034(2) 0.028(2) 0.033(3) 0.000(2) 0.007(2) -0.002(2) C32 0.031(2) 0.024(2) 0.034(3) -0.001(2) 0.006(2) -0.0009(19) C33 0.035(2) 0.028(2) 0.029(3) 0.004(2) 0.005(2) -0.0042(19) C34 0.040(3) 0.056(3) 0.047(3) -0.002(3) 0.003(2) 0.004(3) C35 0.047(3) 0.069(4) 0.040(3) 0.004(3) -0.010(3) -0.010(3) C36 0.054(3) 0.043(3) 0.034(3) -0.001(2) 0.004(2) -0.002(2) C37 0.093(7) 0.337(19) 0.092(7) -0.039(9) 0.018(6) 0.022(9) C38 0.175(9) 0.098(7) 0.068(6) -0.020(5) -0.030(7) 0.007(6) N25 0.302(13) 0.096(6) 0.077(6) -0.009(5) -0.013(7) 0.038(7) Cl1 0.0551(8) 0.0579(9) 0.0525(9) -0.0029(7) 0.0143(7) -0.0067(7) Cl2 0.0876(11) 0.0723(11) 0.0428(9) -0.0042(8) 0.0098(8) -0.0124(9) O1 0.060(3) 0.117(5) 0.145(5) 0.010(4) 0.005(3) -0.001(3) O2 0.164(5) 0.172(6) 0.141(6) 0.086(5) -0.058(4) -0.113(5) O3 0.109(4) 0.111(4) 0.052(3) -0.005(3) 0.015(3) 0.001(3) O4 0.154(5) 0.189(7) 0.096(4) -0.041(4) 0.021(4) 0.093(5) O5 0.343(10) 0.205(7) 0.084(5) 0.025(5) 0.049(6) 0.204(7) O6 0.151(5) 0.157(6) 0.052(3) -0.038(3) 0.012(3) 0.013(4) O7 0.097(3) 0.073(3) 0.059(3) 0.005(2) 0.018(2) 0.005(3) O8 0.331(10) 0.346(11) 0.101(5) 0.082(6) -0.050(6) -0.275(9) _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 N22 1.983(4) . ? Cu1 N18 1.993(4) . ? Cu1 N6 2.046(4) . ? Cu1 N12 2.127(4) . ? Cu1 N10 2.413(4) . ? Cu1 Cu2 2.8272(9) . ? Cu2 N4 2.006(4) . ? Cu2 N21 2.025(4) . ? Cu2 N9 2.031(4) . ? Cu2 N16 2.164(4) . ? Cu2 N15 2.367(4) . ? Cu2 Cu3 2.7322(9) . ? Cu3 N7 1.997(4) . ? Cu3 N3 2.013(4) . ? Cu3 N19 2.036(4) . ? Cu3 N13 2.054(4) . ? Cu3 N1 2.473(4) . ? N1 C1 1.342(7) . ? N1 C4 1.349(6) . ? N2 C4 1.329(6) . ? N2 C3 1.330(7) . ? N3 C5 1.298(6) . ? N3 C4 1.399(6) . ? N4 C5 1.349(6) . ? N4 C6 1.378(6) . ? N5 C7 1.317(6) . ? N5 C6 1.344(6) . ? N6 C9 1.337(6) . ? N6 C6 1.353(6) . ? N7 C10 1.349(6) . ? N7 C13 1.360(6) . ? N8 C13 1.335(6) . ? N8 C12 1.337(7) . ? N9 C14 1.336(6) . ? N9 C13 1.377(6) . ? N10 C14 1.302(6) . ? N10 C15 1.375(6) . ? N11 C16 1.322(6) . ? N11 C15 1.343(6) . ? N12 C18 1.316(6) . ? N12 C15 1.350(6) . ? N13 C19 1.328(6) . ? N13 C22 1.333(6) . ? N14 C21 1.328(7) . ? N14 C22 1.342(6) . ? N15 C23 1.298(6) . ? N15 C22 1.383(6) . ? N16 C23 1.321(6) . ? N16 C24 1.374(6) . ? N17 C25 1.335(6) . ? N17 C24 1.352(6) . ? N18 C27 1.339(6) . ? N18 C24 1.350(6) . ? N19 C28 1.338(6) . ? N19 C31 1.347(6) . ? N20 C31 1.336(6) . ? N20 C30 1.337(6) . ? N21 C32 1.324(5) . ? N21 C31 1.398(6) . ? N22 C32 1.323(6) . ? N22 C33 1.390(6) . ? N23 C33 1.335(6) . ? N23 C34 1.349(6) . ? N24 C36 1.335(6) . ? N24 C33 1.351(6) . ? C1 C2 1.356(9) . ? C2 C3 1.376(9) . ? C7 C8 1.376(7) . ? C8 C9 1.356(7) . ? C10 C11 1.372(7) . ? C11 C12 1.373(8) . ? C16 C17 1.382(8) . ? C17 C18 1.384(7) . ? C19 C20 1.370(7) . ? C20 C21 1.383(8) . ? C25 C26 1.378(7) . ? C26 C27 1.374(7) . ? C28 C29 1.360(7) . ? C29 C30 1.358(7) . ? C34 C35 1.375(8) . ? C35 C36 1.361(7) . ? C37 C38 1.386(13) . ? C38 N25 1.140(13) . ? Cl1 O2 1.366(6) . ? Cl1 O4 1.396(6) . ? Cl1 O3 1.398(5) . ? Cl1 O1 1.414(5) . ? Cl2 O5 1.355(7) . ? Cl2 O6 1.376(5) . ? Cl2 O8 1.385(7) . ? Cl2 O7 1.409(5) . ? 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 N22 Cu1 N18 173.07(15) . . ? N22 Cu1 N6 91.41(15) . . ? N18 Cu1 N6 89.78(15) . . ? N22 Cu1 N12 91.42(15) . . ? N18 Cu1 N12 89.68(15) . . ? N6 Cu1 N12 160.93(15) . . ? N22 Cu1 N10 88.10(14) . . ? N18 Cu1 N10 86.61(14) . . ? N6 Cu1 N10 140.06(14) . . ? N12 Cu1 N10 58.90(13) . . ? N22 Cu1 Cu2 77.33(11) . . ? N18 Cu1 Cu2 96.11(11) . . ? N6 Cu1 Cu2 81.59(11) . . ? N12 Cu1 Cu2 117.41(10) . . ? N10 Cu1 Cu2 59.36(9) . . ? N4 Cu2 N21 89.57(14) . . ? N4 Cu2 N9 169.15(15) . . ? N21 Cu2 N9 89.74(14) . . ? N4 Cu2 N16 90.21(14) . . ? N21 Cu2 N16 155.44(15) . . ? N9 Cu2 N16 94.89(14) . . ? N4 Cu2 N15 87.69(14) . . ? N21 Cu2 N15 146.43(14) . . ? N9 Cu2 N15 86.90(13) . . ? N16 Cu2 N15 58.06(14) . . ? N4 Cu2 Cu3 91.62(11) . . ? N21 Cu2 Cu3 84.94(10) . . ? N9 Cu2 Cu3 77.54(11) . . ? N16 Cu2 Cu3 119.61(11) . . ? N15 Cu2 Cu3 61.72(10) . . ? N4 Cu2 Cu1 82.59(11) . . ? N21 Cu2 Cu1 86.53(10) . . ? N9 Cu2 Cu1 108.18(11) . . ? N16 Cu2 Cu1 69.10(11) . . ? N15 Cu2 Cu1 126.14(10) . . ? Cu3 Cu2 Cu1 169.73(3) . . ? N7 Cu3 N3 165.02(16) . . ? N7 Cu3 N19 87.51(15) . . ? N3 Cu3 N19 90.29(15) . . ? N7 Cu3 N13 89.43(15) . . ? N3 Cu3 N13 95.46(15) . . ? N19 Cu3 N13 168.50(16) . . ? N7 Cu3 N1 134.92(15) . . ? N3 Cu3 N1 59.59(14) . . ? N19 Cu3 N1 86.32(14) . . ? N13 Cu3 N1 88.01(15) . . ? N7 Cu3 Cu2 89.78(11) . . ? N3 Cu3 Cu2 75.24(11) . . ? N19 Cu3 Cu2 82.89(11) . . ? N13 Cu3 Cu2 108.18(11) . . ? N1 Cu3 Cu2 133.41(10) . . ? C1 N1 C4 115.3(5) . . ? C1 N1 Cu3 159.2(4) . . ? C4 N1 Cu3 85.3(3) . . ? C4 N2 C3 114.5(5) . . ? C5 N3 C4 120.7(4) . . ? C5 N3 Cu3 135.2(3) . . ? C4 N3 Cu3 104.2(3) . . ? C5 N4 C6 118.6(4) . . ? C5 N4 Cu2 114.9(3) . . ? C6 N4 Cu2 126.4(3) . . ? C7 N5 C6 116.9(4) . . ? C9 N6 C6 117.0(4) . . ? C9 N6 Cu1 116.0(3) . . ? C6 N6 Cu1 126.8(3) . . ? C10 N7 C13 116.7(4) . . ? C10 N7 Cu3 121.4(3) . . ? C13 N7 Cu3 121.5(3) . . ? C13 N8 C12 116.7(5) . . ? C14 N9 C13 119.2(4) . . ? C14 N9 Cu2 106.6(3) . . ? C13 N9 Cu2 134.1(3) . . ? C14 N10 C15 123.1(4) . . ? C14 N10 Cu1 148.6(3) . . ? C15 N10 Cu1 88.3(3) . . ? C16 N11 C15 115.1(4) . . ? C18 N12 C15 118.1(4) . . ? C18 N12 Cu1 140.0(3) . . ? C15 N12 Cu1 101.8(3) . . ? C19 N13 C22 118.5(4) . . ? C19 N13 Cu3 132.2(4) . . ? C22 N13 Cu3 109.0(3) . . ? C21 N14 C22 115.1(5) . . ? C23 N15 C22 123.3(4) . . ? C23 N15 Cu2 89.3(3) . . ? C22 N15 Cu2 147.4(3) . . ? C23 N16 C24 121.8(4) . . ? C23 N16 Cu2 97.9(3) . . ? C24 N16 Cu2 139.9(3) . . ? C25 N17 C24 115.9(4) . . ? C27 N18 C24 118.4(4) . . ? C27 N18 Cu1 125.1(3) . . ? C24 N18 Cu1 116.5(3) . . ? C28 N19 C31 117.4(4) . . ? C28 N19 Cu3 114.9(3) . . ? C31 N19 Cu3 127.5(3) . . ? C31 N20 C30 116.7(4) . . ? C32 N21 C31 116.9(4) . . ? C32 N21 Cu2 119.2(3) . . ? C31 N21 Cu2 123.8(3) . . ? C32 N22 C33 120.1(4) . . ? C32 N22 Cu1 132.2(3) . . ? C33 N22 Cu1 107.6(3) . . ? C33 N23 C34 114.7(4) . . ? C36 N24 C33 116.2(4) . . ? N1 C1 C2 121.9(6) . . ? C1 C2 C3 117.7(5) . . ? N2 C3 C2 123.2(6) . . ? N2 C4 N1 127.4(4) . . ? N2 C4 N3 121.6(4) . . ? N1 C4 N3 110.9(4) . . ? N3 C5 N4 120.9(4) . . ? N5 C6 N6 123.6(4) . . ? N5 C6 N4 118.9(4) . . ? N6 C6 N4 117.5(4) . . ? N5 C7 C8 123.5(5) . . ? C9 C8 C7 116.2(5) . . ? N6 C9 C8 122.7(5) . . ? N7 C10 C11 122.3(5) . . ? C10 C11 C12 116.4(5) . . ? N8 C12 C11 123.4(5) . . ? N8 C13 N7 124.4(4) . . ? N8 C13 N9 120.4(4) . . ? N7 C13 N9 115.2(4) . . ? N10 C14 N9 116.6(4) . . ? N11 C15 N12 125.2(4) . . ? N11 C15 N10 123.8(4) . . ? N12 C15 N10 111.0(4) . . ? N11 C16 C17 124.0(5) . . ? C16 C17 C18 116.6(5) . . ? N12 C18 C17 121.0(5) . . ? N13 C19 C20 120.5(5) . . ? C19 C20 C21 117.2(5) . . ? N14 C21 C20 123.4(5) . . ? N13 C22 N14 125.3(4) . . ? N13 C22 N15 112.9(4) . . ? N14 C22 N15 121.8(4) . . ? N15 C23 N16 114.8(4) . . ? N18 C24 N17 123.9(4) . . ? N18 C24 N16 115.4(4) . . ? N17 C24 N16 120.7(4) . . ? N17 C25 C26 123.7(4) . . ? C27 C26 C25 116.9(5) . . ? N18 C27 C26 121.1(5) . . ? N19 C28 C29 121.8(5) . . ? C30 C29 C28 117.3(5) . . ? N20 C30 C29 123.0(5) . . ? N20 C31 N19 123.9(4) . . ? N20 C31 N21 118.7(4) . . ? N19 C31 N21 117.4(4) . . ? N22 C32 N21 121.6(4) . . ? N23 C33 N24 126.5(4) . . ? N23 C33 N22 121.2(4) . . ? N24 C33 N22 112.2(4) . . ? N23 C34 C35 122.9(5) . . ? C36 C35 C34 117.6(5) . . ? N24 C36 C35 122.0(5) . . ? N25 C38 C37 174.4(13) . . ? O2 Cl1 O4 112.1(5) . . ? O2 Cl1 O3 111.7(4) . . ? O4 Cl1 O3 108.4(4) . . ? O2 Cl1 O1 107.7(4) . . ? O4 Cl1 O1 105.7(4) . . ? O3 Cl1 O1 111.1(3) . . ? O5 Cl2 O6 108.8(4) . . ? O5 Cl2 O8 107.6(7) . . ? O6 Cl2 O8 108.7(5) . . ? O5 Cl2 O7 109.4(4) . . ? O6 Cl2 O7 113.8(4) . . ? O8 Cl2 O7 108.5(4) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.796 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.187 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 662459' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cl2 Cu4 N24 O3' _chemical_formula_weight 1175.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 15.449(3) _cell_length_b 9.2458(15) _cell_length_c 17.828(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.658(3) _cell_angle_gamma 90.00 _cell_volume 2350.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 793 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.04 _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7153 _exptl_absorpt_correction_T_max 0.9356 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7035 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.07 _reflns_number_total 4127 _reflns_number_gt 2809 _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^)+(0.1230P)^2^+9.7826P] 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 4127 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.2369 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.27847(5) 0.68588(8) 0.19081(4) 0.0304(3) Uani 1 1 d . . . Cu2 Cu 0.33717(8) 0.68737(13) 0.07536(6) 0.0603(4) Uani 1 1 d . . . Cl Cl 0.38213(18) 0.6905(3) -0.03555(14) 0.0713(7) Uani 1 1 d . . . N1 N 0.4069(4) 0.6508(6) 0.2768(3) 0.0404(13) Uani 1 1 d . . . N2 N 0.5551(4) 0.5409(8) 0.3143(4) 0.0590(18) Uani 1 1 d . . . N3 N 0.4600(4) 0.5959(7) 0.1754(3) 0.0443(14) Uani 1 1 d . . . N4 N 0.2526(4) 0.4740(6) 0.1867(3) 0.0429(13) Uani 1 1 d . . . N5 N 0.2008(5) 0.2645(7) 0.1064(4) 0.0551(17) Uani 1 1 d . . . N6 N 0.2692(4) 0.4641(7) 0.0635(4) 0.0508(15) Uani 1 1 d . . . N7 N 0.2963(4) 0.8982(6) 0.2124(3) 0.0381(12) Uani 1 1 d . . . N8 N 0.3831(4) 1.1088(6) 0.2159(4) 0.0459(14) Uani 1 1 d . . . N9 N 0.3780(4) 0.9106(7) 0.1279(4) 0.0457(14) Uani 1 1 d . . . N10 N 0.1418(4) 0.7169(6) 0.1221(3) 0.0378(12) Uani 1 1 d . . . N11 N 0.0292(5) 0.8026(10) -0.0019(4) 0.076(3) Uani 1 1 d . . . N12 N 0.1889(4) 0.7751(7) 0.0178(3) 0.0474(14) Uani 1 1 d . . . C1 C 0.4261(5) 0.6813(7) 0.3543(4) 0.0407(16) Uani 1 1 d . . . H1A H 0.4876 0.6774 0.3920 0.049 Uiso 1 1 calc R . . C2 C 0.4779(5) 0.5953(8) 0.2548(4) 0.0420(16) Uani 1 1 d . . . C3 C 0.6191(5) 0.4854(11) 0.2880(6) 0.067(2) Uani 1 1 d . . . H3A H 0.6745 0.4491 0.3267 0.081 Uiso 1 1 calc R . . C4 C 0.6080(5) 0.4792(10) 0.2093(6) 0.064(2) Uani 1 1 d . . . H4A H 0.6531 0.4378 0.1934 0.077 Uiso 1 1 calc R . . C5 C 0.5257(5) 0.5378(9) 0.1530(5) 0.056(2) Uani 1 1 d . . . H5B H 0.5159 0.5364 0.0982 0.067 Uiso 1 1 calc R . . C6 C 0.2500 0.4029(12) 0.2500 0.047(2) Uani 1 2 d S . . H6A H 0.2500 0.3023 0.2500 0.056 Uiso 1 2 calc SR . . C7 C 0.2411(5) 0.3962(8) 0.1167(4) 0.0458(17) Uani 1 1 d . . . C8 C 0.1928(6) 0.1960(10) 0.0387(5) 0.065(2) Uani 1 1 d . . . H8B H 0.1664 0.1040 0.0299 0.079 Uiso 1 1 calc R . . C9 C 0.2209(7) 0.2524(11) -0.0180(5) 0.073(3) Uani 1 1 d . . . H9A H 0.2143 0.2015 -0.0649 0.087 Uiso 1 1 calc R . . C10 C 0.2599(7) 0.3890(11) -0.0033(5) 0.074(3) Uani 1 1 d . . . H10A H 0.2804 0.4303 -0.0412 0.088 Uiso 1 1 calc R . . C11 C 0.2500 0.9664(10) 0.2500 0.039(2) Uani 1 2 d S . . H11B H 0.2500 1.0669 0.2500 0.047 Uiso 1 2 calc SR . . C12 C 0.3548(4) 0.9774(7) 0.1848(4) 0.0365(14) Uani 1 1 d . . . C13 C 0.4343(6) 1.1818(9) 0.1831(5) 0.058(2) Uani 1 1 d . . . H13A H 0.4541 1.2746 0.2023 0.069 Uiso 1 1 calc R . . C14 C 0.4589(6) 1.1292(10) 0.1242(5) 0.061(2) Uani 1 1 d . . . H14A H 0.4935 1.1839 0.1018 0.074 Uiso 1 1 calc R . . C15 C 0.4307(6) 0.9896(10) 0.0982(5) 0.059(2) Uani 1 1 d . . . H15A H 0.4488 0.9490 0.0588 0.071 Uiso 1 1 calc R . . C16 C 0.1184(5) 0.7652(9) 0.0426(4) 0.0460(17) Uani 1 1 d . . . C17 C 0.1695(6) 0.8288(10) -0.0565(5) 0.058(2) Uani 1 1 d . . . H17A H 0.2179 0.8390 -0.0748 0.070 Uiso 1 1 calc R . . C18 C 0.0827(7) 0.8683(12) -0.1053(5) 0.073(3) Uani 1 1 d . . . H18A H 0.0703 0.9056 -0.1569 0.088 Uiso 1 1 calc R . . C19 C 0.0123(6) 0.8518(15) -0.0762(6) 0.092(4) Uani 1 1 d . . . H19A H -0.0489 0.8758 -0.1098 0.110 Uiso 1 1 calc R . . O2 O 0.1521(6) 1.1160(8) -0.2395(5) 0.104(3) Uani 1 1 d . . . O1 O 0.7500 0.1168(12) 0.2500 0.231(13) Uani 1 2 d S . . 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 0.0317(4) 0.0328(5) 0.0307(5) -0.0011(3) 0.0162(3) -0.0013(3) Cu2 0.0722(7) 0.0745(8) 0.0516(6) -0.0012(5) 0.0432(6) 0.0007(5) Cl 0.0880(16) 0.0886(17) 0.0602(13) -0.0114(11) 0.0537(12) -0.0090(13) N1 0.036(3) 0.049(3) 0.038(3) -0.001(3) 0.017(2) 0.007(3) N2 0.047(3) 0.081(5) 0.053(4) -0.010(4) 0.024(3) 0.011(3) N3 0.043(3) 0.050(4) 0.045(3) -0.007(3) 0.023(3) -0.002(3) N4 0.046(3) 0.039(3) 0.046(3) -0.008(3) 0.020(3) -0.002(3) N5 0.058(4) 0.044(4) 0.053(4) -0.013(3) 0.012(3) -0.010(3) N6 0.055(4) 0.058(4) 0.039(3) -0.006(3) 0.018(3) -0.001(3) N7 0.042(3) 0.036(3) 0.043(3) 0.001(2) 0.024(2) -0.001(2) N8 0.045(3) 0.041(3) 0.053(4) 0.000(3) 0.021(3) -0.008(3) N9 0.045(3) 0.052(4) 0.050(3) -0.003(3) 0.029(3) -0.008(3) N10 0.033(3) 0.047(3) 0.033(3) 0.004(2) 0.013(2) -0.002(2) N11 0.044(4) 0.133(8) 0.046(4) 0.027(4) 0.013(3) 0.003(4) N12 0.053(3) 0.056(4) 0.037(3) -0.005(3) 0.021(3) -0.011(3) C1 0.035(3) 0.046(4) 0.039(4) 0.000(3) 0.012(3) 0.003(3) C2 0.038(3) 0.044(4) 0.046(4) -0.007(3) 0.019(3) -0.001(3) C3 0.038(4) 0.088(7) 0.073(6) -0.019(5) 0.019(4) 0.014(4) C4 0.046(4) 0.080(6) 0.076(6) -0.024(5) 0.035(4) 0.002(4) C5 0.058(5) 0.064(5) 0.061(5) -0.013(4) 0.040(4) 0.000(4) C6 0.041(5) 0.044(6) 0.052(6) 0.000 0.014(5) 0.000 C7 0.046(4) 0.048(4) 0.042(4) -0.003(3) 0.015(3) 0.004(3) C8 0.070(6) 0.056(5) 0.058(5) -0.017(4) 0.012(4) -0.010(4) C9 0.096(7) 0.067(6) 0.049(5) -0.025(5) 0.023(5) -0.007(5) C10 0.093(7) 0.085(7) 0.048(5) -0.010(5) 0.033(5) 0.000(6) C11 0.050(5) 0.031(5) 0.045(5) 0.000 0.027(5) 0.000 C12 0.035(3) 0.043(4) 0.031(3) 0.003(3) 0.014(3) -0.003(3) C13 0.054(5) 0.051(5) 0.072(5) 0.001(4) 0.027(4) -0.015(4) C14 0.054(5) 0.071(6) 0.068(5) 0.007(5) 0.033(4) -0.019(4) C15 0.062(5) 0.071(6) 0.062(5) -0.005(4) 0.043(4) -0.015(4) C16 0.042(4) 0.059(5) 0.035(4) -0.003(3) 0.012(3) -0.011(3) C17 0.068(5) 0.075(6) 0.038(4) 0.003(4) 0.028(4) -0.006(4) C18 0.075(6) 0.106(8) 0.036(4) 0.011(5) 0.019(4) -0.014(6) C19 0.049(5) 0.163(11) 0.049(5) 0.035(6) 0.002(4) -0.012(6) O2 0.154(7) 0.072(5) 0.094(5) -0.011(4) 0.058(5) 0.036(5) O1 0.170(14) 0.040(6) 0.59(4) 0.000 0.27(2) 0.000 _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 N4 1.995(6) . ? Cu1 N7 1.999(6) . ? Cu1 N1 2.012(6) . ? Cu1 N10 2.012(5) . ? Cu1 Cu2 2.5490(11) . ? Cu1 Cu1 2.5804(14) 2 ? Cu2 N3 2.212(6) . ? Cu2 N9 2.254(6) . ? Cu2 N12 2.269(6) . ? Cu2 N6 2.289(7) . ? Cu2 Cl 2.335(2) . ? N1 C1 1.327(9) . ? N1 C2 1.398(8) . ? N2 C3 1.348(9) . ? N2 C2 1.351(9) . ? N3 C2 1.333(9) . ? N3 C5 1.338(9) . ? N4 C6 1.321(8) . ? N4 C7 1.391(9) . ? N5 C8 1.325(10) . ? N5 C7 1.347(10) . ? N6 C10 1.338(10) . ? N6 C7 1.341(9) . ? N7 C11 1.314(7) . ? N7 C12 1.391(8) . ? N8 C13 1.334(9) . ? N8 C12 1.337(9) . ? N9 C15 1.345(9) . ? N9 C12 1.349(8) . ? N10 C1 1.313(8) 2 ? N10 C16 1.394(9) . ? N11 C19 1.328(11) . ? N11 C16 1.343(10) . ? N12 C16 1.326(9) . ? N12 C17 1.336(9) . ? C1 N10 1.313(8) 2 ? C3 C4 1.348(12) . ? C4 C5 1.391(12) . ? C6 N4 1.321(8) 2 ? C8 C9 1.351(13) . ? C9 C10 1.380(14) . ? C11 N7 1.314(7) 2 ? C13 C14 1.339(12) . ? C14 C15 1.384(12) . ? C17 C18 1.337(12) . ? C18 C19 1.382(13) . ? 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 N4 Cu1 N7 169.2(2) . . ? N4 Cu1 N1 89.7(2) . . ? N7 Cu1 N1 89.4(2) . . ? N4 Cu1 N10 88.2(2) . . ? N7 Cu1 N10 90.7(2) . . ? N1 Cu1 N10 169.2(2) . . ? N4 Cu1 Cu2 95.95(17) . . ? N7 Cu1 Cu2 94.86(15) . . ? N1 Cu1 Cu2 93.61(16) . . ? N10 Cu1 Cu2 97.13(16) . . ? N4 Cu1 Cu1 84.49(16) . 2 ? N7 Cu1 Cu1 84.70(15) . 2 ? N1 Cu1 Cu1 85.62(16) . 2 ? N10 Cu1 Cu1 83.65(15) . 2 ? Cu2 Cu1 Cu1 179.11(5) . 2 ? N3 Cu2 N9 90.0(2) . . ? N3 Cu2 N12 154.8(2) . . ? N9 Cu2 N12 86.1(2) . . ? N3 Cu2 N6 87.1(2) . . ? N9 Cu2 N6 155.4(2) . . ? N12 Cu2 N6 86.2(2) . . ? N3 Cu2 Cl 104.19(16) . . ? N9 Cu2 Cl 102.34(16) . . ? N12 Cu2 Cl 101.00(16) . . ? N6 Cu2 Cl 102.04(16) . . ? N3 Cu2 Cu1 78.94(15) . . ? N9 Cu2 Cu1 78.41(14) . . ? N12 Cu2 Cu1 75.84(15) . . ? N6 Cu2 Cu1 77.07(15) . . ? Cl Cu2 Cu1 176.74(8) . . ? C1 N1 C2 119.1(6) . . ? C1 N1 Cu1 121.2(4) . . ? C2 N1 Cu1 119.7(4) . . ? C3 N2 C2 114.4(7) . . ? C2 N3 C5 116.4(6) . . ? C2 N3 Cu2 128.4(4) . . ? C5 N3 Cu2 115.2(5) . . ? C6 N4 C7 118.3(7) . . ? C6 N4 Cu1 121.9(5) . . ? C7 N4 Cu1 119.7(5) . . ? C8 N5 C7 115.6(7) . . ? C10 N6 C7 115.7(8) . . ? C10 N6 Cu2 116.0(6) . . ? C7 N6 Cu2 128.3(5) . . ? C11 N7 C12 118.9(6) . . ? C11 N7 Cu1 120.5(5) . . ? C12 N7 Cu1 120.6(4) . . ? C13 N8 C12 115.7(7) . . ? C15 N9 C12 115.1(7) . . ? C15 N9 Cu2 116.7(5) . . ? C12 N9 Cu2 128.2(4) . . ? C1 N10 C16 118.6(6) 2 . ? C1 N10 Cu1 123.3(5) 2 . ? C16 N10 Cu1 117.7(4) . . ? C19 N11 C16 116.1(7) . . ? C16 N12 C17 117.1(7) . . ? C16 N12 Cu2 129.8(5) . . ? C17 N12 Cu2 112.5(5) . . ? N10 C1 N1 120.1(6) 2 . ? N3 C2 N2 126.5(6) . . ? N3 C2 N1 115.6(6) . . ? N2 C2 N1 117.8(6) . . ? N2 C3 C4 124.1(8) . . ? C3 C4 C5 116.7(7) . . ? N3 C5 C4 121.9(7) . . ? N4 C6 N4 120.3(10) . 2 ? N6 C7 N5 125.8(7) . . ? N6 C7 N4 115.3(7) . . ? N5 C7 N4 118.8(7) . . ? N5 C8 C9 123.6(8) . . ? C8 C9 C10 117.0(8) . . ? N6 C10 C9 122.2(9) . . ? N7 C11 N7 122.7(9) 2 . ? N8 C12 N9 126.0(6) . . ? N8 C12 N7 119.0(6) . . ? N9 C12 N7 115.0(6) . . ? N8 C13 C14 123.7(8) . . ? C13 C14 C15 117.0(7) . . ? N9 C15 C14 122.3(8) . . ? N12 C16 N11 124.9(7) . . ? N12 C16 N10 115.8(6) . . ? N11 C16 N10 119.2(6) . . ? N12 C17 C18 122.2(8) . . ? C17 C18 C19 117.5(8) . . ? N11 C19 C18 122.1(9) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.569 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.132 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 662460' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Br2 Cu4 N24 O3' _chemical_formula_weight 1264.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 15.8186(17) _cell_length_b 9.2496(10) _cell_length_c 17.972(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.943(2) _cell_angle_gamma 90.00 _cell_volume 2403.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 778 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.00 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.472 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5292 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7985 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4080 _reflns_number_gt 2713 _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^)+(0.0866P)^2^+4.8467P] 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 4080 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Br Br 0.38178(6) 0.68600(8) -0.03797(4) 0.0598(3) Uani 1 1 d . . . Cu1 Cu 0.27755(4) 0.68105(6) 0.19151(3) 0.0255(2) Uani 1 1 d . . . Cu2 Cu 0.33459(6) 0.68161(10) 0.07700(5) 0.0536(3) Uani 1 1 d . . . N1 N 0.4039(3) 0.6464(5) 0.2794(3) 0.0317(11) Uani 1 1 d . . . N2 N 0.5496(4) 0.5364(6) 0.3193(3) 0.0521(15) Uani 1 1 d . . . N3 N 0.4556(3) 0.5905(5) 0.1795(3) 0.0379(12) Uani 1 1 d . . . N4 N 0.2520(3) 0.4692(5) 0.1865(3) 0.0315(11) Uani 1 1 d . . . N5 N 0.1968(4) 0.2608(5) 0.1061(3) 0.0428(13) Uani 1 1 d . . . N6 N 0.2659(4) 0.4571(5) 0.0640(3) 0.0431(13) Uani 1 1 d . . . N7 N 0.2948(3) 0.8941(5) 0.2128(3) 0.0300(10) Uani 1 1 d . . . N8 N 0.3789(3) 1.1059(5) 0.2180(3) 0.0396(12) Uani 1 1 d . . . N9 N 0.3745(4) 0.9091(5) 0.1305(3) 0.0414(12) Uani 1 1 d . . . N10 N 0.1434(3) 0.7129(5) 0.1203(3) 0.0326(11) Uani 1 1 d . . . N11 N 0.0329(4) 0.8032(7) -0.0031(3) 0.0569(16) Uani 1 1 d . . . N12 N 0.1883(4) 0.7731(5) 0.0174(3) 0.0369(11) Uani 1 1 d . . . C1 C 0.4233(4) 0.6781(6) 0.3562(3) 0.0351(13) Uani 1 1 d . . . H1A H 0.4844 0.6761 0.3942 0.042 Uiso 1 1 calc R . . C2 C 0.4742(4) 0.5895(6) 0.2597(3) 0.0354(13) Uani 1 1 d . . . C3 C 0.6132(5) 0.4796(8) 0.2959(5) 0.061(2) Uani 1 1 d . . . H3A H 0.6673 0.4417 0.3353 0.073 Uiso 1 1 calc R . . C4 C 0.6008(5) 0.4755(8) 0.2154(4) 0.0564(18) Uani 1 1 d . . . H4A H 0.6455 0.4356 0.2003 0.068 Uiso 1 1 calc R . . C5 C 0.5212(5) 0.5316(7) 0.1589(4) 0.0487(16) Uani 1 1 d . . . H5B H 0.5116 0.5294 0.1043 0.058 Uiso 1 1 calc R . . C6 C 0.2500 0.3994(8) 0.2500 0.0326(18) Uani 1 2 d S . . H6A H 0.2500 0.2988 0.2500 0.039 Uiso 1 2 calc SR . . C7 C 0.2376(4) 0.3910(6) 0.1160(3) 0.0349(13) Uani 1 1 d . . . C8 C 0.1867(5) 0.1912(7) 0.0378(4) 0.0508(17) Uani 1 1 d . . . H8B H 0.1605 0.0994 0.0290 0.061 Uiso 1 1 calc R . . C9 C 0.2126(6) 0.2473(8) -0.0184(4) 0.061(2) Uani 1 1 d . . . H9A H 0.2029 0.1973 -0.0661 0.073 Uiso 1 1 calc R . . C10 C 0.2541(5) 0.3820(8) -0.0032(4) 0.0558(19) Uani 1 1 d . . . H10A H 0.2743 0.4215 -0.0407 0.067 Uiso 1 1 calc R . . C11 C 0.2500 0.9631(8) 0.2500 0.0326(18) Uani 1 2 d S . . H11B H 0.2500 1.0637 0.2500 0.039 Uiso 1 2 calc SR . . C12 C 0.3520(4) 0.9745(6) 0.1867(3) 0.0311(12) Uani 1 1 d . . . C13 C 0.4288(5) 1.1808(7) 0.1863(4) 0.0492(17) Uani 1 1 d . . . H13A H 0.4470 1.2742 0.2052 0.059 Uiso 1 1 calc R . . C14 C 0.4542(5) 1.1277(8) 0.1279(5) 0.061(2) Uani 1 1 d . . . H14A H 0.4886 1.1822 0.1066 0.073 Uiso 1 1 calc R . . C15 C 0.4265(5) 0.9889(8) 0.1020(4) 0.060(2) Uani 1 1 d . . . H15A H 0.4442 0.9483 0.0632 0.071 Uiso 1 1 calc R . . C16 C 0.1196(4) 0.7641(6) 0.0407(3) 0.0351(13) Uani 1 1 d . . . C17 C 0.1680(5) 0.8316(7) -0.0558(3) 0.0433(15) Uani 1 1 d . . . H17A H 0.2154 0.8430 -0.0735 0.052 Uiso 1 1 calc R . . C18 C 0.0825(5) 0.8748(8) -0.1049(4) 0.0567(19) Uani 1 1 d . . . H18A H 0.0700 0.9157 -0.1556 0.068 Uiso 1 1 calc R . . C19 C 0.0143(5) 0.8558(9) -0.0770(4) 0.061(2) Uani 1 1 d . . . H19A H -0.0463 0.8803 -0.1105 0.073 Uiso 1 1 calc R . . O2 O 0.1480(9) 1.1167(15) -0.2622(10) 0.256(7) Uani 1 1 d . . . O1 O 0.7500 0.101(2) 0.2500 0.263(10) Uani 1 2 d S . . 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 Br 0.0757(6) 0.0717(5) 0.0534(4) -0.0021(4) 0.0482(4) 0.0025(4) Cu1 0.0313(4) 0.0246(3) 0.0249(4) -0.0004(3) 0.0156(3) -0.0002(3) Cu2 0.0666(7) 0.0663(6) 0.0445(5) 0.0041(4) 0.0398(5) 0.0077(4) N1 0.034(3) 0.032(2) 0.031(2) -0.0036(19) 0.016(2) -0.002(2) N2 0.043(3) 0.069(4) 0.045(3) -0.008(3) 0.019(3) 0.016(3) N3 0.043(3) 0.039(3) 0.037(3) -0.006(2) 0.022(2) -0.005(2) N4 0.039(3) 0.026(2) 0.031(2) -0.0029(19) 0.016(2) -0.002(2) N5 0.052(3) 0.035(3) 0.041(3) -0.011(2) 0.017(3) -0.008(2) N6 0.060(4) 0.041(3) 0.032(3) -0.001(2) 0.022(2) -0.001(3) N7 0.036(3) 0.027(2) 0.030(2) -0.0001(19) 0.016(2) -0.003(2) N8 0.040(3) 0.036(3) 0.047(3) -0.002(2) 0.021(2) -0.006(2) N9 0.047(3) 0.042(3) 0.044(3) -0.006(2) 0.027(3) -0.008(2) N10 0.037(3) 0.033(2) 0.030(2) 0.0041(19) 0.016(2) 0.001(2) N11 0.040(3) 0.090(4) 0.038(3) 0.026(3) 0.012(3) 0.005(3) N12 0.043(3) 0.039(3) 0.034(3) 0.000(2) 0.020(2) -0.004(2) C1 0.037(3) 0.034(3) 0.033(3) -0.004(2) 0.013(3) -0.001(3) C2 0.037(4) 0.032(3) 0.040(3) -0.007(2) 0.019(3) -0.002(3) C3 0.040(4) 0.071(5) 0.065(5) -0.012(4) 0.016(3) 0.013(4) C4 0.041(4) 0.074(5) 0.066(5) -0.016(4) 0.033(4) 0.008(4) C5 0.049(4) 0.055(4) 0.053(4) -0.007(3) 0.032(4) 0.005(3) C6 0.038(5) 0.026(4) 0.031(4) 0.000 0.011(4) 0.000 C7 0.037(4) 0.031(3) 0.037(3) -0.003(2) 0.015(3) 0.005(3) C8 0.056(5) 0.044(4) 0.046(4) -0.014(3) 0.014(3) -0.006(3) C9 0.081(6) 0.058(4) 0.043(4) -0.026(3) 0.024(4) -0.011(4) C10 0.082(6) 0.055(4) 0.035(3) -0.004(3) 0.029(4) -0.003(4) C11 0.036(5) 0.028(4) 0.031(4) 0.000 0.011(4) 0.000 C12 0.031(3) 0.027(3) 0.034(3) 0.006(2) 0.013(2) -0.001(2) C13 0.047(4) 0.038(3) 0.060(4) 0.005(3) 0.019(3) -0.010(3) C14 0.070(5) 0.056(4) 0.074(5) 0.005(4) 0.047(4) -0.019(4) C15 0.075(6) 0.069(5) 0.052(4) -0.005(4) 0.044(4) -0.018(4) C16 0.039(4) 0.037(3) 0.030(3) 0.003(2) 0.015(3) -0.005(3) C17 0.053(4) 0.053(4) 0.029(3) 0.004(3) 0.022(3) -0.003(3) C18 0.062(5) 0.078(5) 0.029(3) 0.015(3) 0.017(3) -0.006(4) C19 0.047(4) 0.093(6) 0.037(4) 0.021(4) 0.012(3) 0.002(4) O2 0.187(12) 0.184(11) 0.362(19) -0.107(13) 0.075(13) -0.045(10) O1 0.32(3) 0.205(19) 0.23(2) 0.000 0.078(19) 0.000 _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 Br Cu2 2.4656(9) . ? Cu1 N4 1.996(4) . ? Cu1 N7 2.005(4) . ? Cu1 N10 2.006(5) . ? Cu1 N1 2.007(5) . ? Cu1 Cu2 2.5606(9) . ? Cu1 Cu1 2.5821(11) 2 ? Cu2 N3 2.216(5) . ? Cu2 N12 2.282(5) . ? Cu2 N9 2.293(5) . ? Cu2 N6 2.311(5) . ? N1 C1 1.320(7) . ? N1 C2 1.400(7) . ? N2 C2 1.332(8) . ? N2 C3 1.345(8) . ? N3 C2 1.348(7) . ? N3 C5 1.350(7) . ? N4 C6 1.322(6) . ? N4 C7 1.395(7) . ? N5 C8 1.336(8) . ? N5 C7 1.344(7) . ? N6 C7 1.337(7) . ? N6 C10 1.340(8) . ? N7 C11 1.319(6) . ? N7 C12 1.392(7) . ? N8 C12 1.334(7) . ? N8 C13 1.338(8) . ? N9 C12 1.344(7) . ? N9 C15 1.351(8) . ? N10 C1 1.326(7) 2 ? N10 C16 1.405(7) . ? N11 C16 1.325(8) . ? N11 C19 1.329(8) . ? N12 C16 1.316(7) . ? N12 C17 1.335(7) . ? C1 N10 1.326(7) 2 ? C3 C4 1.380(10) . ? C4 C5 1.360(9) . ? C6 N4 1.322(6) 2 ? C8 C9 1.340(10) . ? C9 C10 1.383(10) . ? C11 N7 1.319(6) 2 ? C13 C14 1.360(10) . ? C14 C15 1.375(10) . ? C17 C18 1.342(9) . ? C18 C19 1.374(10) . ? 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 N4 Cu1 N7 169.48(17) . . ? N4 Cu1 N10 88.46(19) . . ? N7 Cu1 N10 90.25(18) . . ? N4 Cu1 N1 89.84(18) . . ? N7 Cu1 N1 89.53(18) . . ? N10 Cu1 N1 169.47(18) . . ? N4 Cu1 Cu2 95.55(12) . . ? N7 Cu1 Cu2 94.96(12) . . ? N10 Cu1 Cu2 96.52(13) . . ? N1 Cu1 Cu2 93.99(13) . . ? N4 Cu1 Cu1 84.69(12) . 2 ? N7 Cu1 Cu1 84.79(12) . 2 ? N10 Cu1 Cu1 84.28(13) . 2 ? N1 Cu1 Cu1 85.22(13) . 2 ? Cu2 Cu1 Cu1 179.17(5) . 2 ? N3 Cu2 N12 154.29(17) . . ? N3 Cu2 N9 90.12(18) . . ? N12 Cu2 N9 84.89(18) . . ? N3 Cu2 N6 87.37(18) . . ? N12 Cu2 N6 86.58(18) . . ? N9 Cu2 N6 154.82(17) . . ? N3 Cu2 Br 104.47(12) . . ? N12 Cu2 Br 101.23(12) . . ? N9 Cu2 Br 102.16(12) . . ? N6 Cu2 Br 102.72(12) . . ? N3 Cu2 Cu1 78.36(12) . . ? N12 Cu2 Cu1 75.94(12) . . ? N9 Cu2 Cu1 77.98(12) . . ? N6 Cu2 Cu1 76.98(12) . . ? Br Cu2 Cu1 177.15(5) . . ? C1 N1 C2 118.4(5) . . ? C1 N1 Cu1 121.5(4) . . ? C2 N1 Cu1 120.1(3) . . ? C2 N2 C3 115.5(6) . . ? C2 N3 C5 115.6(5) . . ? C2 N3 Cu2 129.1(4) . . ? C5 N3 Cu2 115.2(4) . . ? C6 N4 C7 118.6(5) . . ? C6 N4 Cu1 121.1(4) . . ? C7 N4 Cu1 120.4(3) . . ? C8 N5 C7 115.2(5) . . ? C7 N6 C10 115.5(5) . . ? C7 N6 Cu2 128.1(4) . . ? C10 N6 Cu2 116.4(4) . . ? C11 N7 C12 118.0(5) . . ? C11 N7 Cu1 120.8(4) . . ? C12 N7 Cu1 121.2(3) . . ? C12 N8 C13 115.7(5) . . ? C12 N9 C15 115.3(5) . . ? C12 N9 Cu2 128.1(4) . . ? C15 N9 Cu2 116.7(4) . . ? C1 N10 C16 119.1(5) 2 . ? C1 N10 Cu1 122.3(4) 2 . ? C16 N10 Cu1 118.4(4) . . ? C16 N11 C19 116.7(6) . . ? C16 N12 C17 116.1(5) . . ? C16 N12 Cu2 129.7(4) . . ? C17 N12 Cu2 113.9(4) . . ? N1 C1 N10 120.6(5) . 2 ? N2 C2 N3 126.7(5) . . ? N2 C2 N1 118.6(5) . . ? N3 C2 N1 114.6(5) . . ? N2 C3 C4 122.2(7) . . ? C5 C4 C3 117.8(6) . . ? N3 C5 C4 122.1(6) . . ? N4 C6 N4 121.6(7) 2 . ? N6 C7 N5 126.6(5) . . ? N6 C7 N4 114.8(5) . . ? N5 C7 N4 118.6(5) . . ? N5 C8 C9 123.2(6) . . ? C8 C9 C10 117.7(6) . . ? N6 C10 C9 121.8(6) . . ? N7 C11 N7 122.1(7) . 2 ? N8 C12 N9 126.2(5) . . ? N8 C12 N7 118.9(5) . . ? N9 C12 N7 114.8(5) . . ? N8 C13 C14 123.5(6) . . ? C13 C14 C15 116.5(6) . . ? N9 C15 C14 122.7(6) . . ? N12 C16 N11 125.7(5) . . ? N12 C16 N10 115.5(5) . . ? N11 C16 N10 118.8(5) . . ? N12 C17 C18 122.9(6) . . ? C17 C18 C19 116.9(6) . . ? N11 C19 C18 121.6(7) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.002 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.103 #===END