# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Perez, Pedro' 'Belderrain, Tomas' 'Martin, Carmen' 'Sierra, Marta' 'Alvarez, Eleuterio' _publ_contact_author_name 'Dr Pedro Perez' _publ_contact_author_email perez@dqcm.uhu.es _publ_section_title ; Hydrotris(3-mesitylpyrazolyl)borato-copper(I) alkyne complexes: synthesis, structural characterization and rationalization of their activities as alkyne cyclopropenation catalysts ; # Attachment '- complex1.cif' data_ea18410a1 _database_code_depnum_ccdc_archive 'CCDC 849107' #TrackingRef '- complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H50 B Cu N6), 3(C H2 Cl2)' _chemical_formula_sum 'C87 H106 B2 Cl6 Cu2 N12' _chemical_formula_weight 1681.26 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1908(5) _cell_length_b 12.0506(5) _cell_length_c 16.6731(7) _cell_angle_alpha 77.7080(9) _cell_angle_beta 83.1730(10) _cell_angle_gamma 89.2120(10) _cell_volume 2181.19(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9810 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.53 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7142 _exptl_absorpt_correction_T_max 0.7371 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51665 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.53 _reflns_number_total 13139 _reflns_number_gt 10340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2005)' _computing_cell_refinement 'APEX2 Software Suite' _computing_data_reduction 'APEX2 Software Suite' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material 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^)+(0.0697P)^2^+1.6165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13139 _refine_ls_number_parameters 509 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11588(2) 0.262752(18) 0.734530(14) 0.02519(7) Uani 1 1 d . . . N1 N 0.10589(13) 0.42338(12) 0.67236(9) 0.0226(3) Uani 1 1 d . . . N2 N 0.18508(14) 0.45471(13) 0.60240(9) 0.0231(3) Uani 1 1 d . . . N3 N 0.30420(13) 0.26055(13) 0.71929(9) 0.0243(3) Uani 1 1 d . . . N4 N 0.35394(13) 0.32265(13) 0.64455(10) 0.0249(3) Uani 1 1 d . . . N5 N 0.12988(14) 0.20375(13) 0.61689(9) 0.0247(3) Uani 1 1 d . . . N6 N 0.20856(14) 0.26821(13) 0.55654(9) 0.0243(3) Uani 1 1 d . . . C1 C 0.03283(16) 0.51190(15) 0.67665(11) 0.0238(3) Uani 1 1 d . . . C2 C 0.0654(2) 0.60127(16) 0.60887(12) 0.0311(4) Uani 1 1 d . . . H2 H 0.0291 0.6737 0.5965 0.037 Uiso 1 1 calc R . . C3 C 0.16172(18) 0.56102(15) 0.56410(11) 0.0283(4) Uani 1 1 d . . . H3 H 0.2046 0.6020 0.5142 0.034 Uiso 1 1 calc R . . C4 C -0.06571(16) 0.50273(14) 0.74587(11) 0.0230(3) Uani 1 1 d . . . C5 C -0.04063(16) 0.51066(15) 0.82482(11) 0.0255(3) Uani 1 1 d . . . C6 C -0.13385(18) 0.49334(17) 0.88963(12) 0.0300(4) Uani 1 1 d . . . H6 H -0.1171 0.4996 0.9430 0.036 Uiso 1 1 calc R . . C7 C -0.24991(19) 0.46729(18) 0.87864(13) 0.0333(4) Uani 1 1 d . . . C8 C -0.27399(18) 0.46221(17) 0.79972(13) 0.0322(4) Uani 1 1 d . . . H8 H -0.3537 0.4459 0.7911 0.039 Uiso 1 1 calc R . . C9 C -0.18379(17) 0.48051(15) 0.73258(12) 0.0266(3) Uani 1 1 d . . . C10 C 0.08486(18) 0.5362(2) 0.84024(13) 0.0351(4) Uani 1 1 d . . . H10A H 0.0856 0.5365 0.8989 0.053 Uiso 1 1 calc R . . H10B H 0.1110 0.6109 0.8068 0.053 Uiso 1 1 calc R . . H10C H 0.1397 0.4780 0.8251 0.053 Uiso 1 1 calc R . . C11 C -0.3484(2) 0.4469(3) 0.95057(17) 0.0534(7) Uani 1 1 d . . . H11A H -0.4114 0.5036 0.9399 0.080 Uiso 1 1 calc R . . H11B H -0.3148 0.4531 1.0011 0.080 Uiso 1 1 calc R . . H11C H -0.3830 0.3707 0.9574 0.080 Uiso 1 1 calc R . . C12 C -0.2142(2) 0.4750(2) 0.64774(14) 0.0379(5) Uani 1 1 d . . . H12A H -0.2994 0.4549 0.6511 0.057 Uiso 1 1 calc R . . H12B H -0.1646 0.4174 0.6266 0.057 Uiso 1 1 calc R . . H12C H -0.1982 0.5492 0.6103 0.057 Uiso 1 1 calc R . . C13 C 0.39598(16) 0.22090(16) 0.76160(12) 0.0273(4) Uani 1 1 d . . . C14 C 0.50555(18) 0.2583(2) 0.71451(14) 0.0365(4) Uani 1 1 d . . . H14 H 0.5841 0.2431 0.7300 0.044 Uiso 1 1 calc R . . C15 C 0.47532(17) 0.32167(18) 0.64093(13) 0.0317(4) Uani 1 1 d . . . H15 H 0.5303 0.3584 0.5955 0.038 Uiso 1 1 calc R . . C16 C 0.37671(16) 0.14284(17) 0.84402(12) 0.0281(4) Uani 1 1 d . . . C17 C 0.38850(18) 0.02530(18) 0.84905(14) 0.0339(4) Uani 1 1 d . . . C18 C 0.37190(19) -0.04752(19) 0.92633(16) 0.0398(5) Uani 1 1 d . . . H18 H 0.3800 -0.1269 0.9298 0.048 Uiso 1 1 calc R . . C19 C 0.34390(18) -0.0081(2) 0.99832(15) 0.0401(5) Uani 1 1 d . . . C20 C 0.3343(2) 0.1084(2) 0.99204(14) 0.0397(5) Uani 1 1 d . . . H20 H 0.3160 0.1368 1.0410 0.048 Uiso 1 1 calc R . . C21 C 0.35084(18) 0.18463(18) 0.91588(13) 0.0326(4) Uani 1 1 d . . . C22 C 0.4166(3) -0.0218(2) 0.77228(18) 0.0505(6) Uani 1 1 d . . . H22A H 0.3645 0.0136 0.7310 0.076 Uiso 1 1 calc R . . H22B H 0.4026 -0.1041 0.7861 0.076 Uiso 1 1 calc R . . H22C H 0.5010 -0.0055 0.7499 0.076 Uiso 1 1 calc R . . C23 C 0.3241(2) -0.0889(3) 1.08150(17) 0.0556(7) Uani 1 1 d . . . H23A H 0.2756 -0.1541 1.0774 0.083 Uiso 1 1 calc R . . H23B H 0.2819 -0.0497 1.1222 0.083 Uiso 1 1 calc R . . H23C H 0.4020 -0.1154 1.0990 0.083 Uiso 1 1 calc R . . C24 C 0.3423(3) 0.3107(2) 0.91156(17) 0.0475(6) Uani 1 1 d . . . H24A H 0.4139 0.3489 0.8782 0.071 Uiso 1 1 calc R . . H24B H 0.3370 0.3252 0.9675 0.071 Uiso 1 1 calc R . . H24C H 0.2703 0.3398 0.8862 0.071 Uiso 1 1 calc R . . C25 C 0.09207(16) 0.11946(15) 0.58518(12) 0.0253(3) Uani 1 1 d . . . C26 C 0.14662(19) 0.12947(18) 0.50363(13) 0.0327(4) Uani 1 1 d . . . H26 H 0.1356 0.0811 0.4669 0.039 Uiso 1 1 calc R . . C27 C 0.21940(18) 0.22427(17) 0.48837(12) 0.0299(4) Uani 1 1 d . . . H27 H 0.2690 0.2538 0.4382 0.036 Uiso 1 1 calc R . . C28 C 0.00262(17) 0.03375(15) 0.63365(12) 0.0253(3) Uani 1 1 d . . . C29 C -0.11766(17) 0.06437(16) 0.64854(13) 0.0292(4) Uani 1 1 d . . . C30 C -0.20173(18) -0.01766(17) 0.69235(13) 0.0322(4) Uani 1 1 d . . . H30 H -0.2833 0.0035 0.7024 0.039 Uiso 1 1 calc R . . C31 C -0.16955(19) -0.12906(17) 0.72153(13) 0.0312(4) Uani 1 1 d . . . C32 C -0.04987(19) -0.15808(16) 0.70640(13) 0.0313(4) Uani 1 1 d . . . H32 H -0.0263 -0.2340 0.7264 0.038 Uiso 1 1 calc R . . C33 C 0.03703(18) -0.07880(16) 0.66256(13) 0.0291(4) Uani 1 1 d . . . C34 C -0.1576(2) 0.18395(19) 0.61868(19) 0.0472(6) Uani 1 1 d . . . H34A H -0.1321 0.2323 0.6541 0.071 Uiso 1 1 calc R . . H34B H -0.2455 0.1852 0.6209 0.071 Uiso 1 1 calc R . . H34C H -0.1214 0.2124 0.5616 0.071 Uiso 1 1 calc R . . C35 C -0.2624(2) -0.2167(2) 0.76751(16) 0.0451(5) Uani 1 1 d . . . H35A H -0.3175 -0.1832 0.8058 0.068 Uiso 1 1 calc R . . H35B H -0.2220 -0.2817 0.7987 0.068 Uiso 1 1 calc R . . H35C H -0.3079 -0.2423 0.7279 0.068 Uiso 1 1 calc R . . C36 C 0.1652(2) -0.1157(2) 0.64718(19) 0.0456(6) Uani 1 1 d . . . H36A H 0.1771 -0.1882 0.6849 0.068 Uiso 1 1 calc R . . H36B H 0.2198 -0.0581 0.6567 0.068 Uiso 1 1 calc R . . H36C H 0.1823 -0.1248 0.5899 0.068 Uiso 1 1 calc R . . C37 C -0.02901(19) 0.22286(18) 0.81715(14) 0.0362(5) Uani 1 1 d D . . H37 H -0.089(2) 0.271(2) 0.8252(17) 0.043 Uiso 1 1 d D . . C38 C 0.03520(17) 0.14030(16) 0.82549(11) 0.0272(4) Uani 1 1 d . . . C39 C 0.08525(19) 0.02701(17) 0.85446(14) 0.0337(4) Uani 1 1 d . . . H39A H 0.1465 0.0333 0.8915 0.040 Uiso 1 1 calc R . . H39B H 0.1260 -0.0001 0.8063 0.040 Uiso 1 1 calc R . . C40 C -0.01007(18) -0.05974(16) 0.90028(13) 0.0300(4) Uani 1 1 d . . . H40A H -0.0687 -0.0703 0.8624 0.036 Uiso 1 1 calc R . . H40B H -0.0540 -0.0313 0.9468 0.036 Uiso 1 1 calc R . . C41 C 0.0471(2) -0.17365(19) 0.93338(17) 0.0432(5) Uani 1 1 d . . . H41A H 0.0925 -0.2010 0.8868 0.052 Uiso 1 1 calc R . . H41B H 0.1048 -0.1630 0.9719 0.052 Uiso 1 1 calc R . . C42 C -0.0459(3) -0.2620(2) 0.97782(18) 0.0496(6) Uani 1 1 d . . . H42A H -0.0929 -0.2342 1.0228 0.074 Uiso 1 1 calc R . . H42B H -0.0056 -0.3324 1.0006 0.074 Uiso 1 1 calc R . . H42C H -0.0997 -0.2768 0.9389 0.074 Uiso 1 1 calc R . . B1 B 0.27613(18) 0.36901(17) 0.57452(12) 0.0235(4) Uani 1 1 d . . . H1 H 0.3288 0.4072 0.5237 0.028 Uiso 1 1 calc R . . Cl1 Cl 0.40311(8) 0.63026(8) 0.79731(6) 0.0688(2) Uani 1 1 d . . . Cl2 Cl 0.46467(10) 0.64450(12) 0.62061(7) 0.0986(4) Uani 1 1 d . . . C43 C 0.3794(3) 0.5771(3) 0.71017(19) 0.0600(8) Uani 1 1 d . . . H43A H 0.3981 0.4952 0.7208 0.072 Uiso 1 1 calc R . . H43B H 0.2932 0.5850 0.7021 0.072 Uiso 1 1 calc R . . Cl3 Cl 0.5315(2) 0.08593(16) 0.54281(11) 0.1560(8) Uani 1 1 d . . . C44 C 0.4680(17) 0.0258(14) 0.4557(7) 0.201(10) Uani 0.50 1 d P . . H44A H 0.3835 0.0508 0.4544 0.242 Uiso 0.50 1 calc PR . . H44B H 0.5131 0.0640 0.4025 0.242 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02451(11) 0.02283(11) 0.02409(12) 0.00009(8) 0.00477(8) -0.00097(8) N1 0.0243(7) 0.0226(7) 0.0195(6) -0.0040(5) 0.0028(5) -0.0010(5) N2 0.0270(7) 0.0220(7) 0.0185(6) -0.0031(5) 0.0032(5) -0.0031(5) N3 0.0211(7) 0.0254(7) 0.0245(7) -0.0028(6) 0.0005(5) -0.0030(5) N4 0.0217(7) 0.0262(7) 0.0254(7) -0.0055(6) 0.0030(5) -0.0044(5) N5 0.0267(7) 0.0238(7) 0.0233(7) -0.0069(6) 0.0027(5) -0.0070(5) N6 0.0257(7) 0.0243(7) 0.0225(7) -0.0069(6) 0.0027(5) -0.0036(5) C1 0.0279(8) 0.0218(8) 0.0211(8) -0.0043(6) -0.0008(6) 0.0005(6) C2 0.0438(11) 0.0223(8) 0.0239(8) -0.0004(7) 0.0006(7) 0.0030(7) C3 0.0390(10) 0.0214(8) 0.0219(8) -0.0019(6) 0.0019(7) -0.0032(7) C4 0.0274(8) 0.0190(7) 0.0221(8) -0.0044(6) -0.0006(6) 0.0030(6) C5 0.0273(8) 0.0247(8) 0.0245(8) -0.0061(7) -0.0017(6) 0.0019(6) C6 0.0350(10) 0.0307(9) 0.0243(8) -0.0079(7) 0.0003(7) 0.0021(7) C7 0.0317(9) 0.0328(10) 0.0340(10) -0.0101(8) 0.0075(8) -0.0015(7) C8 0.0262(9) 0.0323(10) 0.0383(10) -0.0096(8) -0.0008(7) -0.0015(7) C9 0.0292(9) 0.0221(8) 0.0292(9) -0.0069(7) -0.0040(7) 0.0022(6) C10 0.0298(9) 0.0473(12) 0.0295(10) -0.0097(9) -0.0054(7) -0.0004(8) C11 0.0430(13) 0.0673(18) 0.0473(14) -0.0198(13) 0.0196(11) -0.0105(12) C12 0.0451(12) 0.0374(11) 0.0341(10) -0.0087(9) -0.0137(9) -0.0021(9) C13 0.0209(8) 0.0281(9) 0.0324(9) -0.0058(7) -0.0022(7) -0.0012(6) C14 0.0203(8) 0.0440(12) 0.0419(11) -0.0033(9) -0.0006(8) -0.0038(7) C15 0.0205(8) 0.0382(10) 0.0348(10) -0.0077(8) 0.0043(7) -0.0053(7) C16 0.0192(7) 0.0315(9) 0.0321(9) -0.0021(7) -0.0057(6) -0.0011(6) C17 0.0248(9) 0.0326(10) 0.0432(11) -0.0041(8) -0.0070(8) 0.0008(7) C18 0.0283(9) 0.0315(10) 0.0546(14) 0.0035(9) -0.0086(9) 0.0029(7) C19 0.0223(9) 0.0488(13) 0.0420(12) 0.0101(10) -0.0098(8) -0.0011(8) C20 0.0310(10) 0.0528(13) 0.0331(11) -0.0023(9) -0.0069(8) -0.0025(9) C21 0.0253(8) 0.0368(10) 0.0346(10) -0.0045(8) -0.0048(7) -0.0024(7) C22 0.0511(14) 0.0397(13) 0.0613(16) -0.0161(12) 0.0005(12) 0.0017(10) C23 0.0350(12) 0.0682(18) 0.0494(14) 0.0226(13) -0.0110(10) -0.0033(11) C24 0.0568(15) 0.0391(12) 0.0460(13) -0.0115(10) 0.0016(11) -0.0065(10) C25 0.0263(8) 0.0229(8) 0.0280(8) -0.0091(7) -0.0017(6) -0.0013(6) C26 0.0385(10) 0.0330(10) 0.0296(9) -0.0157(8) 0.0009(8) -0.0056(8) C27 0.0348(10) 0.0321(9) 0.0235(8) -0.0101(7) 0.0021(7) -0.0026(7) C28 0.0284(8) 0.0216(8) 0.0278(8) -0.0095(7) -0.0029(7) -0.0029(6) C29 0.0292(9) 0.0232(8) 0.0352(10) -0.0072(7) -0.0019(7) -0.0009(7) C30 0.0288(9) 0.0297(9) 0.0373(10) -0.0080(8) 0.0009(8) -0.0023(7) C31 0.0370(10) 0.0267(9) 0.0297(9) -0.0070(7) -0.0003(7) -0.0070(7) C32 0.0389(10) 0.0228(9) 0.0332(10) -0.0064(7) -0.0069(8) -0.0007(7) C33 0.0302(9) 0.0247(9) 0.0344(10) -0.0097(7) -0.0063(7) 0.0007(7) C34 0.0351(11) 0.0268(10) 0.0736(17) -0.0005(10) -0.0008(11) 0.0044(8) C35 0.0477(13) 0.0348(11) 0.0481(13) -0.0042(10) 0.0067(10) -0.0131(9) C36 0.0335(11) 0.0328(11) 0.0701(17) -0.0109(11) -0.0045(11) 0.0042(8) C37 0.0304(10) 0.0285(10) 0.0418(11) 0.0013(8) 0.0123(8) -0.0005(7) C38 0.0272(8) 0.0266(9) 0.0245(8) -0.0009(7) 0.0027(6) -0.0041(6) C39 0.0316(9) 0.0275(9) 0.0360(10) 0.0032(8) 0.0030(8) 0.0026(7) C40 0.0323(9) 0.0242(9) 0.0307(9) -0.0011(7) -0.0014(7) -0.0018(7) C41 0.0441(12) 0.0293(10) 0.0502(13) 0.0030(9) -0.0019(10) 0.0031(9) C42 0.0591(16) 0.0295(11) 0.0545(15) 0.0045(10) -0.0074(12) -0.0051(10) B1 0.0245(8) 0.0222(9) 0.0228(9) -0.0059(7) 0.0030(7) -0.0041(6) Cl1 0.0706(5) 0.0684(5) 0.0756(5) -0.0317(4) -0.0097(4) -0.0160(4) Cl2 0.0792(6) 0.1314(9) 0.0726(6) -0.0071(6) 0.0211(5) -0.0471(6) C43 0.0606(17) 0.0609(17) 0.0596(17) -0.0253(14) 0.0132(14) -0.0223(14) Cl3 0.258(3) 0.1201(13) 0.1043(11) -0.0390(10) -0.0508(13) -0.0260(14) C44 0.27(2) 0.183(14) 0.095(8) 0.045(9) 0.060(10) 0.154(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C37 1.991(2) . ? Cu1 N1 2.0002(15) . ? Cu1 C38 2.0127(18) . ? Cu1 N3 2.0930(15) . ? Cu1 N5 2.2124(15) . ? N1 C1 1.344(2) . ? N1 N2 1.3654(19) . ? N2 C3 1.341(2) . ? N2 B1 1.544(2) . ? N3 C13 1.340(2) . ? N3 N4 1.368(2) . ? N4 C15 1.352(2) . ? N4 B1 1.544(3) . ? N5 C25 1.336(2) . ? N5 N6 1.366(2) . ? N6 C27 1.345(2) . ? N6 B1 1.540(2) . ? C1 C2 1.402(2) . ? C1 C4 1.486(2) . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.401(3) . ? C4 C9 1.404(3) . ? C5 C6 1.393(3) . ? C5 C10 1.505(3) . ? C6 C7 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.388(3) . ? C7 C11 1.510(3) . ? C8 C9 1.398(3) . ? C8 H8 0.9500 . ? C9 C12 1.508(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.400(3) . ? C13 C16 1.485(3) . ? C14 C15 1.377(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.394(3) . ? C16 C17 1.406(3) . ? C17 C18 1.390(3) . ? C17 C22 1.506(4) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 C20 1.389(4) . ? C19 C23 1.509(3) . ? C20 C21 1.394(3) . ? C20 H20 0.9500 . ? C21 C24 1.507(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.404(3) . ? C25 C28 1.484(2) . ? C26 C27 1.373(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.398(3) . ? C28 C33 1.404(3) . ? C29 C30 1.397(3) . ? C29 C34 1.501(3) . ? C30 C31 1.385(3) . ? C30 H30 0.9500 . ? C31 C32 1.387(3) . ? C31 C35 1.510(3) . ? C32 C33 1.397(3) . ? C32 H32 0.9500 . ? C33 C36 1.505(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.213(3) . ? C37 H37 0.903(17) . ? C38 C39 1.474(3) . ? C39 C40 1.520(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.528(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.509(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? B1 H1 1.0000 . ? Cl1 C43 1.756(3) . ? Cl2 C43 1.722(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? Cl3 C44 1.342(18) 2_656 ? Cl3 C44 1.96(2) . ? C44 Cl3 1.342(18) 2_656 ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 Cu1 N1 110.03(7) . . ? C37 Cu1 C38 35.26(8) . . ? N1 Cu1 C38 145.24(7) . . ? C37 Cu1 N3 143.61(8) . . ? N1 Cu1 N3 94.42(6) . . ? C38 Cu1 N3 115.49(7) . . ? C37 Cu1 N5 120.00(8) . . ? N1 Cu1 N5 90.00(6) . . ? C38 Cu1 N5 108.81(7) . . ? N3 Cu1 N5 85.29(6) . . ? C1 N1 N2 106.94(14) . . ? C1 N1 Cu1 136.58(12) . . ? N2 N1 Cu1 116.21(11) . . ? C3 N2 N1 109.48(14) . . ? C3 N2 B1 129.60(15) . . ? N1 N2 B1 120.72(14) . . ? C13 N3 N4 106.61(14) . . ? C13 N3 Cu1 140.09(13) . . ? N4 N3 Cu1 113.22(11) . . ? C15 N4 N3 109.73(16) . . ? C15 N4 B1 128.32(16) . . ? N3 N4 B1 121.41(14) . . ? C25 N5 N6 106.58(14) . . ? C25 N5 Cu1 140.74(13) . . ? N6 N5 Cu1 112.49(10) . . ? C27 N6 N5 109.92(15) . . ? C27 N6 B1 129.64(16) . . ? N5 N6 B1 120.28(14) . . ? N1 C1 C2 109.74(16) . . ? N1 C1 C4 119.73(15) . . ? C2 C1 C4 130.52(17) . . ? C3 C2 C1 104.86(17) . . ? C3 C2 H2 127.6 . . ? C1 C2 H2 127.6 . . ? N2 C3 C2 108.99(16) . . ? N2 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? C5 C4 C9 120.04(16) . . ? C5 C4 C1 120.48(16) . . ? C9 C4 C1 119.41(16) . . ? C6 C5 C4 118.91(17) . . ? C6 C5 C10 120.11(17) . . ? C4 C5 C10 120.97(16) . . ? C7 C6 C5 122.06(18) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 118.37(18) . . ? C6 C7 C11 120.7(2) . . ? C8 C7 C11 120.9(2) . . ? C7 C8 C9 121.60(18) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 118.95(18) . . ? C8 C9 C12 119.84(18) . . ? C4 C9 C12 121.21(18) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.05(17) . . ? N3 C13 C16 121.99(16) . . ? C14 C13 C16 127.84(17) . . ? C15 C14 C13 105.37(17) . . ? C15 C14 H14 127.3 . . ? C13 C14 H14 127.3 . . ? N4 C15 C14 108.23(17) . . ? N4 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? C21 C16 C17 120.03(19) . . ? C21 C16 C13 121.03(18) . . ? C17 C16 C13 118.92(18) . . ? C18 C17 C16 118.8(2) . . ? C18 C17 C22 120.2(2) . . ? C16 C17 C22 121.0(2) . . ? C19 C18 C17 122.1(2) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 118.1(2) . . ? C18 C19 C23 121.2(2) . . ? C20 C19 C23 120.7(3) . . ? C19 C20 C21 121.8(2) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C16 119.1(2) . . ? C20 C21 C24 120.3(2) . . ? C16 C21 C24 120.55(19) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 109.94(16) . . ? N5 C25 C28 121.27(16) . . ? C26 C25 C28 128.77(16) . . ? C27 C26 C25 105.17(16) . . ? C27 C26 H26 127.4 . . ? C25 C26 H26 127.4 . . ? N6 C27 C26 108.39(17) . . ? N6 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? C29 C28 C33 119.66(17) . . ? C29 C28 C25 119.78(17) . . ? C33 C28 C25 120.53(17) . . ? C30 C29 C28 119.34(18) . . ? C30 C29 C34 119.55(18) . . ? C28 C29 C34 121.12(18) . . ? C31 C30 C29 121.88(19) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 118.10(18) . . ? C30 C31 C35 120.9(2) . . ? C32 C31 C35 121.0(2) . . ? C31 C32 C33 121.87(18) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C28 119.14(18) . . ? C32 C33 C36 119.43(18) . . ? C28 C33 C36 121.42(18) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 Cu1 73.33(13) . . ? C38 C37 H37 162.3(18) . . ? Cu1 C37 H37 124.2(18) . . ? C37 C38 C39 163.5(2) . . ? C37 C38 Cu1 71.42(13) . . ? C39 C38 Cu1 125.04(14) . . ? C38 C39 C40 112.86(17) . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 C41 110.86(18) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 111.9(2) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 B1 N2 109.88(14) . . ? N6 B1 N4 108.15(15) . . ? N2 B1 N4 109.43(14) . . ? N6 B1 H1 109.8 . . ? N2 B1 H1 109.8 . . ? N4 B1 H1 109.8 . . ? Cl2 C43 Cl1 113.79(16) . . ? Cl2 C43 H43A 108.8 . . ? Cl1 C43 H43A 108.8 . . ? Cl2 C43 H43B 108.8 . . ? Cl1 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C44 Cl3 C44 58.9(8) 2_656 . ? Cl3 C44 Cl3 121.1(8) 2_656 . ? Cl3 C44 H44A 107.1 2_656 . ? Cl3 C44 H44A 107.1 . . ? Cl3 C44 H44B 107.1 2_656 . ? Cl3 C44 H44B 107.1 . . ? H44A C44 H44B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 Cu1 N1 C1 6.7(2) . . . . ? C38 Cu1 N1 C1 4.4(3) . . . . ? N3 Cu1 N1 C1 -145.91(18) . . . . ? N5 Cu1 N1 C1 128.81(18) . . . . ? C37 Cu1 N1 N2 -166.42(13) . . . . ? C38 Cu1 N1 N2 -168.71(13) . . . . ? N3 Cu1 N1 N2 41.01(13) . . . . ? N5 Cu1 N1 N2 -44.26(12) . . . . ? C1 N1 N2 C3 0.2(2) . . . . ? Cu1 N1 N2 C3 175.22(12) . . . . ? C1 N1 N2 B1 -175.05(15) . . . . ? Cu1 N1 N2 B1 0.0(2) . . . . ? C37 Cu1 N3 C13 7.4(3) . . . . ? N1 Cu1 N3 C13 140.5(2) . . . . ? C38 Cu1 N3 C13 -21.2(2) . . . . ? N5 Cu1 N3 C13 -129.8(2) . . . . ? C37 Cu1 N3 N4 -168.55(14) . . . . ? N1 Cu1 N3 N4 -35.40(12) . . . . ? C38 Cu1 N3 N4 162.85(12) . . . . ? N5 Cu1 N3 N4 54.23(12) . . . . ? C13 N3 N4 C15 -0.2(2) . . . . ? Cu1 N3 N4 C15 177.04(12) . . . . ? C13 N3 N4 B1 172.00(16) . . . . ? Cu1 N3 N4 B1 -10.7(2) . . . . ? C37 Cu1 N5 C25 -27.7(2) . . . . ? N1 Cu1 N5 C25 -141.0(2) . . . . ? C38 Cu1 N5 C25 9.2(2) . . . . ? N3 Cu1 N5 C25 124.5(2) . . . . ? C37 Cu1 N5 N6 158.17(12) . . . . ? N1 Cu1 N5 N6 44.88(12) . . . . ? C38 Cu1 N5 N6 -164.91(12) . . . . ? N3 Cu1 N5 N6 -49.56(12) . . . . ? C25 N5 N6 C27 -0.1(2) . . . . ? Cu1 N5 N6 C27 176.02(13) . . . . ? C25 N5 N6 B1 -175.93(16) . . . . ? Cu1 N5 N6 B1 0.2(2) . . . . ? N2 N1 C1 C2 -0.1(2) . . . . ? Cu1 N1 C1 C2 -173.62(14) . . . . ? N2 N1 C1 C4 178.70(15) . . . . ? Cu1 N1 C1 C4 5.2(3) . . . . ? N1 C1 C2 C3 0.0(2) . . . . ? C4 C1 C2 C3 -178.64(19) . . . . ? N1 N2 C3 C2 -0.2(2) . . . . ? B1 N2 C3 C2 174.50(18) . . . . ? C1 C2 C3 N2 0.1(2) . . . . ? N1 C1 C4 C5 76.5(2) . . . . ? C2 C1 C4 C5 -105.0(2) . . . . ? N1 C1 C4 C9 -100.4(2) . . . . ? C2 C1 C4 C9 78.1(3) . . . . ? C9 C4 C5 C6 1.6(3) . . . . ? C1 C4 C5 C6 -175.31(16) . . . . ? C9 C4 C5 C10 -179.03(17) . . . . ? C1 C4 C5 C10 4.0(3) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C10 C5 C6 C7 -178.60(19) . . . . ? C5 C6 C7 C8 -2.2(3) . . . . ? C5 C6 C7 C11 178.9(2) . . . . ? C6 C7 C8 C9 1.2(3) . . . . ? C11 C7 C8 C9 -179.8(2) . . . . ? C7 C8 C9 C4 1.0(3) . . . . ? C7 C8 C9 C12 -179.55(19) . . . . ? C5 C4 C9 C8 -2.5(3) . . . . ? C1 C4 C9 C8 174.47(17) . . . . ? C5 C4 C9 C12 178.12(18) . . . . ? C1 C4 C9 C12 -4.9(3) . . . . ? N4 N3 C13 C14 0.6(2) . . . . ? Cu1 N3 C13 C14 -175.53(16) . . . . ? N4 N3 C13 C16 -175.82(17) . . . . ? Cu1 N3 C13 C16 8.1(3) . . . . ? N3 C13 C14 C15 -0.7(2) . . . . ? C16 C13 C14 C15 175.4(2) . . . . ? N3 N4 C15 C14 -0.2(2) . . . . ? B1 N4 C15 C14 -171.74(18) . . . . ? C13 C14 C15 N4 0.5(2) . . . . ? N3 C13 C16 C21 -85.0(2) . . . . ? C14 C13 C16 C21 99.3(3) . . . . ? N3 C13 C16 C17 96.9(2) . . . . ? C14 C13 C16 C17 -78.8(3) . . . . ? C21 C16 C17 C18 1.1(3) . . . . ? C13 C16 C17 C18 179.21(18) . . . . ? C21 C16 C17 C22 -179.9(2) . . . . ? C13 C16 C17 C22 -1.8(3) . . . . ? C16 C17 C18 C19 0.2(3) . . . . ? C22 C17 C18 C19 -178.9(2) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? C17 C18 C19 C23 178.9(2) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C23 C19 C20 C21 -179.3(2) . . . . ? C19 C20 C21 C16 0.5(3) . . . . ? C19 C20 C21 C24 -178.7(2) . . . . ? C17 C16 C21 C20 -1.4(3) . . . . ? C13 C16 C21 C20 -179.51(18) . . . . ? C17 C16 C21 C24 177.8(2) . . . . ? C13 C16 C21 C24 -0.2(3) . . . . ? N6 N5 C25 C26 0.0(2) . . . . ? Cu1 N5 C25 C26 -174.34(16) . . . . ? N6 N5 C25 C28 -178.59(16) . . . . ? Cu1 N5 C25 C28 7.1(3) . . . . ? N5 C25 C26 C27 0.1(2) . . . . ? C28 C25 C26 C27 178.55(19) . . . . ? N5 N6 C27 C26 0.2(2) . . . . ? B1 N6 C27 C26 175.52(19) . . . . ? C25 C26 C27 N6 -0.2(2) . . . . ? N5 C25 C28 C29 72.2(2) . . . . ? C26 C25 C28 C29 -106.1(2) . . . . ? N5 C25 C28 C33 -109.8(2) . . . . ? C26 C25 C28 C33 72.0(3) . . . . ? C33 C28 C29 C30 0.3(3) . . . . ? C25 C28 C29 C30 178.32(18) . . . . ? C33 C28 C29 C34 179.9(2) . . . . ? C25 C28 C29 C34 -2.0(3) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C34 C29 C30 C31 -179.8(2) . . . . ? C29 C30 C31 C32 0.2(3) . . . . ? C29 C30 C31 C35 -179.0(2) . . . . ? C30 C31 C32 C33 -0.5(3) . . . . ? C35 C31 C32 C33 178.7(2) . . . . ? C31 C32 C33 C28 0.6(3) . . . . ? C31 C32 C33 C36 -179.2(2) . . . . ? C29 C28 C33 C32 -0.5(3) . . . . ? C25 C28 C33 C32 -178.55(18) . . . . ? C29 C28 C33 C36 179.4(2) . . . . ? C25 C28 C33 C36 1.3(3) . . . . ? N1 Cu1 C37 C38 -177.74(13) . . . . ? N3 Cu1 C37 C38 -48.5(2) . . . . ? N5 Cu1 C37 C38 80.10(16) . . . . ? Cu1 C37 C38 C39 179.0(7) . . . . ? N1 Cu1 C38 C37 3.7(2) . . . . ? N3 Cu1 C38 C37 150.52(15) . . . . ? N5 Cu1 C38 C37 -115.68(15) . . . . ? C37 Cu1 C38 C39 -179.7(3) . . . . ? N1 Cu1 C38 C39 -175.94(15) . . . . ? N3 Cu1 C38 C39 -29.1(2) . . . . ? N5 Cu1 C38 C39 64.66(19) . . . . ? C37 C38 C39 C40 21.5(9) . . . . ? Cu1 C38 C39 C40 -159.67(15) . . . . ? C38 C39 C40 C41 -176.68(19) . . . . ? C39 C40 C41 C42 -178.9(2) . . . . ? C27 N6 B1 N2 126.6(2) . . . . ? N5 N6 B1 N2 -58.4(2) . . . . ? C27 N6 B1 N4 -114.0(2) . . . . ? N5 N6 B1 N4 61.0(2) . . . . ? C3 N2 B1 N6 -112.7(2) . . . . ? N1 N2 B1 N6 61.4(2) . . . . ? C3 N2 B1 N4 128.67(19) . . . . ? N1 N2 B1 N4 -57.2(2) . . . . ? C15 N4 B1 N6 114.4(2) . . . . ? N3 N4 B1 N6 -56.3(2) . . . . ? C15 N4 B1 N2 -125.91(19) . . . . ? N3 N4 B1 N2 63.4(2) . . . . ? C44 Cl3 C44 Cl3 0.000(1) 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.055 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.070 # Attachment '- complex2.cif' data_ea07210a2 _database_code_depnum_ccdc_archive 'CCDC 849108' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C41 H46 B Cu N6 O2), C H2 Cl2' _chemical_formula_sum 'C165 H186 B4 Cl2 Cu4 N24 O8' _chemical_formula_weight 3001.68 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0009(7) _cell_length_b 11.2392(9) _cell_length_c 38.765(3) _cell_angle_alpha 97.899(2) _cell_angle_beta 91.176(2) _cell_angle_gamma 93.499(2) _cell_volume 3875.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9987 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.12 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1578 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8309 _exptl_absorpt_correction_T_max 0.8825 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 100(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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 55916 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.72 _reflns_number_total 23921 _reflns_number_gt 12812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2005)' _computing_cell_refinement 'APEX2 Software Suite' _computing_data_reduction 'APEX2 Software Suite' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material 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^)+(0.0548P)^2^+13.7273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23921 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.085 _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 0.17725(6) 0.65794(4) 0.149730(14) 0.02017(12) Uani 1 1 d . . . O1 O 0.2766(5) 0.9205(3) 0.10426(11) 0.0439(10) Uani 1 1 d . A . N1 N -0.0340(4) 0.6942(3) 0.14109(9) 0.0185(7) Uani 1 1 d . . . N2 N -0.1299(4) 0.6815(3) 0.16731(9) 0.0177(7) Uani 1 1 d . . . N3 N 0.1219(4) 0.5127(3) 0.17255(9) 0.0177(7) Uani 1 1 d . . . N4 N -0.0019(4) 0.5194(3) 0.19239(9) 0.0176(7) Uani 1 1 d . . . N5 N 0.1671(4) 0.7646(3) 0.20447(9) 0.0183(7) Uani 1 1 d . . . N6 N 0.0383(4) 0.7346(3) 0.22043(9) 0.0177(7) Uani 1 1 d . . . C1 C -0.1139(5) 0.7247(4) 0.11442(11) 0.0198(8) Uani 1 1 d . . . C2 C -0.2626(5) 0.7310(4) 0.12363(12) 0.0241(9) Uani 1 1 d . . . H2 H -0.3434 0.7501 0.1097 0.029 Uiso 1 1 calc R . . C3 C -0.2682(5) 0.7037(4) 0.15700(12) 0.0236(9) Uani 1 1 d . . . H3 H -0.3547 0.7010 0.1706 0.028 Uiso 1 1 calc R . . C4 C -0.0462(4) 0.7426(4) 0.08083(11) 0.0211(8) Uani 1 1 d . . . C5 C 0.0066(5) 0.6453(4) 0.05928(12) 0.0258(9) Uani 1 1 d . . . C6 C 0.0674(6) 0.6649(4) 0.02761(12) 0.0306(10) Uani 1 1 d . . . H6 H 0.1066 0.5994 0.0133 0.037 Uiso 1 1 calc R . . C7 C 0.0723(6) 0.7772(4) 0.01641(12) 0.0296(10) Uani 1 1 d . . . C8 C 0.0184(5) 0.8724(4) 0.03834(12) 0.0277(9) Uani 1 1 d . . . H8 H 0.0218 0.9500 0.0312 0.033 Uiso 1 1 calc R . . C9 C -0.0397(5) 0.8569(4) 0.07017(12) 0.0244(9) Uani 1 1 d . . . C10 C -0.0003(6) 0.5198(4) 0.06948(13) 0.0328(11) Uani 1 1 d . . . H10A H 0.0176 0.4613 0.0490 0.049 Uiso 1 1 calc R . . H10B H -0.0990 0.5012 0.0784 0.049 Uiso 1 1 calc R . . H10C H 0.0759 0.5156 0.0876 0.049 Uiso 1 1 calc R . . C11 C 0.1330(7) 0.7951(5) -0.01858(14) 0.0447(14) Uani 1 1 d . . . H11A H 0.2093 0.7380 -0.0248 0.067 Uiso 1 1 calc R . . H11B H 0.1772 0.8775 -0.0175 0.067 Uiso 1 1 calc R . . H11C H 0.0521 0.7817 -0.0363 0.067 Uiso 1 1 calc R . . C12 C -0.0898(6) 0.9642(4) 0.09394(13) 0.0321(10) Uani 1 1 d . . . H12A H -0.0221 0.9818 0.1144 0.048 Uiso 1 1 calc R . . H12B H -0.1910 0.9462 0.1015 0.048 Uiso 1 1 calc R . . H12C H -0.0889 1.0342 0.0814 0.048 Uiso 1 1 calc R . . C13 C 0.1685(4) 0.4021(3) 0.17216(11) 0.0177(8) Uani 1 1 d . . . C14 C 0.0735(4) 0.3361(4) 0.19165(11) 0.0203(8) Uani 1 1 d . . . H14 H 0.0801 0.2548 0.1955 0.024 Uiso 1 1 calc R . . C15 C -0.0317(5) 0.4137(4) 0.20412(11) 0.0203(8) Uani 1 1 d . . . H15 H -0.1117 0.3957 0.2185 0.024 Uiso 1 1 calc R . . C16 C 0.3091(5) 0.3668(3) 0.15533(11) 0.0188(8) Uani 1 1 d . . . C17 C 0.4457(4) 0.4115(4) 0.17166(11) 0.0198(8) Uani 1 1 d . . . C18 C 0.5772(5) 0.3791(4) 0.15602(12) 0.0238(9) Uani 1 1 d . . . H18 H 0.6693 0.4104 0.1671 0.029 Uiso 1 1 calc R . . C19 C 0.5788(5) 0.3026(4) 0.12472(12) 0.0272(9) Uani 1 1 d . . . C20 C 0.4416(6) 0.2583(4) 0.10911(12) 0.0273(10) Uani 1 1 d . . . H20 H 0.4401 0.2054 0.0877 0.033 Uiso 1 1 calc R . . C21 C 0.3077(5) 0.2888(4) 0.12373(12) 0.0239(9) Uani 1 1 d . . . C22 C 0.4514(5) 0.4935(4) 0.20598(12) 0.0278(10) Uani 1 1 d . . . H22A H 0.5555 0.5144 0.2135 0.042 Uiso 1 1 calc R . . H22B H 0.4006 0.4523 0.2235 0.042 Uiso 1 1 calc R . . H22C H 0.4020 0.5670 0.2032 0.042 Uiso 1 1 calc R . . C23 C 0.7230(6) 0.2674(5) 0.10872(15) 0.0387(12) Uani 1 1 d . . . H23A H 0.8064 0.3070 0.1234 0.058 Uiso 1 1 calc R . . H23B H 0.7285 0.2923 0.0855 0.058 Uiso 1 1 calc R . . H23C H 0.7281 0.1799 0.1068 0.058 Uiso 1 1 calc R . . C24 C 0.1619(5) 0.2374(4) 0.10580(13) 0.0317(10) Uani 1 1 d . . . H24A H 0.1147 0.3004 0.0951 0.048 Uiso 1 1 calc R . . H24B H 0.0956 0.2080 0.1229 0.048 Uiso 1 1 calc R . . H24C H 0.1812 0.1707 0.0877 0.048 Uiso 1 1 calc R . . C25 C 0.2419(4) 0.8479(3) 0.22756(10) 0.0170(7) Uani 1 1 d . . . C26 C 0.1615(5) 0.8731(3) 0.25802(10) 0.0188(8) Uani 1 1 d . . . H26 H 0.1889 0.9292 0.2781 0.023 Uiso 1 1 calc R . . C27 C 0.0333(5) 0.7981(3) 0.25220(11) 0.0188(8) Uani 1 1 d . . . H27 H -0.0451 0.7925 0.2681 0.023 Uiso 1 1 calc R . . C28 C 0.3849(5) 0.9071(3) 0.21837(10) 0.0183(8) Uani 1 1 d . . . C29 C 0.3818(5) 0.9942(4) 0.19573(11) 0.0215(8) Uani 1 1 d . . . C30 C 0.5153(5) 1.0533(4) 0.18797(12) 0.0272(10) Uani 1 1 d . . . H30 H 0.5135 1.1129 0.1728 0.033 Uiso 1 1 calc R . . C31 C 0.6507(5) 1.0267(4) 0.20196(12) 0.0279(10) Uani 1 1 d . . . C32 C 0.6511(5) 0.9398(4) 0.22414(12) 0.0244(9) Uani 1 1 d . . . H32 H 0.7435 0.9211 0.2337 0.029 Uiso 1 1 calc R . . C33 C 0.5208(4) 0.8791(3) 0.23285(11) 0.0186(8) Uani 1 1 d . . . C34 C 0.2354(5) 1.0289(4) 0.18199(12) 0.0283(10) Uani 1 1 d . . . H34A H 0.2529 1.0963 0.1687 0.042 Uiso 1 1 calc R . . H34B H 0.1713 1.0530 0.2015 0.042 Uiso 1 1 calc R . . H34C H 0.1867 0.9601 0.1668 0.042 Uiso 1 1 calc R . . C35 C 0.7945(6) 1.0914(5) 0.19353(15) 0.0438(14) Uani 1 1 d . . . H35A H 0.8444 1.1310 0.2152 0.066 Uiso 1 1 calc R . . H35B H 0.7731 1.1519 0.1785 0.066 Uiso 1 1 calc R . . H35C H 0.8594 1.0332 0.1815 0.066 Uiso 1 1 calc R . . C36 C 0.5282(5) 0.7887(4) 0.25813(12) 0.0242(9) Uani 1 1 d . . . H36A H 0.6208 0.7474 0.2550 0.036 Uiso 1 1 calc R . . H36B H 0.4429 0.7297 0.2537 0.036 Uiso 1 1 calc R . . H36C H 0.5257 0.8304 0.2820 0.036 Uiso 1 1 calc R . . C37 C 0.3738(5) 0.6401(4) 0.13018(13) 0.0280(10) Uani 1 1 d D . . H37 H 0.454(4) 0.591(4) 0.1337(13) 0.034 Uiso 1 1 d D . . C38 C 0.3201(5) 0.7260(4) 0.11853(12) 0.0247(9) Uani 1 1 d . A . C39 C 0.3306(5) 0.8256(5) 0.09792(13) 0.0314(11) Uani 1 1 d D . . O2A O 0.4335(11) 0.8160(9) 0.0746(3) 0.034(2) Uani 0.50 1 d PDU A 1 C40A C 0.4597(13) 0.9187(10) 0.0561(3) 0.039(3) Uani 0.50 1 d PDU A 1 H40A H 0.5095 0.9878 0.0715 0.047 Uiso 0.50 1 calc PR A 1 H40B H 0.3652 0.9437 0.0467 0.047 Uiso 0.50 1 calc PR A 1 C41A C 0.5627(14) 0.8715(15) 0.0261(4) 0.061(4) Uani 0.50 1 d PDU A 1 H41A H 0.6262 0.8121 0.0340 0.091 Uiso 0.50 1 calc PR A 1 H41B H 0.6252 0.9389 0.0196 0.091 Uiso 0.50 1 calc PR A 1 H41C H 0.5015 0.8338 0.0059 0.091 Uiso 0.50 1 calc PR A 1 O2B O 0.3972(12) 0.7765(9) 0.0666(3) 0.036(2) Uani 0.50 1 d PDU A 2 C40B C 0.4258(13) 0.8584(13) 0.0411(3) 0.045(3) Uani 0.50 1 d PDU A 2 H40C H 0.3450 0.9145 0.0414 0.054 Uiso 0.50 1 calc PR A 2 H40D H 0.4269 0.8119 0.0175 0.054 Uiso 0.50 1 calc PR A 2 C41B C 0.5728(16) 0.9290(14) 0.0491(5) 0.066(4) Uani 0.50 1 d PDU A 2 H41D H 0.5671 0.9830 0.0711 0.099 Uiso 0.50 1 calc PR A 2 H41E H 0.5957 0.9765 0.0303 0.099 Uiso 0.50 1 calc PR A 2 H41F H 0.6512 0.8734 0.0512 0.099 Uiso 0.50 1 calc PR A 2 B1 B -0.0753(5) 0.6400(4) 0.20134(12) 0.0179(8) Uani 1 1 d . . . H1 H -0.1618 0.6286 0.2166 0.022 Uiso 1 1 calc R . . Cu2 Cu 0.17339(5) 0.20616(4) 0.370826(13) 0.01722(11) Uani 1 1 d . . . O3 O 0.1199(4) 0.5234(3) 0.36933(8) 0.0247(6) Uani 1 1 d . . . O4 O -0.0461(3) 0.5143(2) 0.41187(8) 0.0242(6) Uani 1 1 d . . . N7 N 0.2064(4) 0.0306(3) 0.36746(9) 0.0170(6) Uani 1 1 d . . . N8 N 0.3313(4) -0.0057(3) 0.35081(9) 0.0171(6) Uani 1 1 d . . . N9 N 0.2365(4) 0.2127(3) 0.32072(9) 0.0170(6) Uani 1 1 d . . . N10 N 0.3610(4) 0.1534(3) 0.31116(9) 0.0167(6) Uani 1 1 d . . . N11 N 0.4054(4) 0.2537(3) 0.38676(9) 0.0181(7) Uani 1 1 d . . . N12 N 0.5017(4) 0.1815(3) 0.36844(9) 0.0163(6) Uani 1 1 d . . . C42 C 0.1314(4) -0.0694(3) 0.37510(10) 0.0165(7) Uani 1 1 d . . . C43 C 0.2090(5) -0.1711(3) 0.36345(11) 0.0201(8) Uani 1 1 d . . . H43 H 0.1821 -0.2527 0.3656 0.024 Uiso 1 1 calc R . . C44 C 0.3337(5) -0.1258(3) 0.34811(11) 0.0190(8) Uani 1 1 d . . . H44 H 0.4090 -0.1723 0.3374 0.023 Uiso 1 1 calc R . . C45 C -0.0113(4) -0.0605(3) 0.39352(10) 0.0158(7) Uani 1 1 d . . . C46 C -0.1462(5) -0.0935(3) 0.37523(11) 0.0186(8) Uani 1 1 d . . . C47 C -0.2799(5) -0.0773(4) 0.39267(12) 0.0230(9) Uani 1 1 d . . . H47 H -0.3716 -0.0999 0.3802 0.028 Uiso 1 1 calc R . . C48 C -0.2823(5) -0.0296(4) 0.42737(12) 0.0249(9) Uani 1 1 d . . . C49 C -0.1471(5) -0.0002(4) 0.44534(11) 0.0226(9) Uani 1 1 d . . . H49 H -0.1472 0.0316 0.4693 0.027 Uiso 1 1 calc R . . C50 C -0.0115(5) -0.0157(3) 0.42928(11) 0.0186(8) Uani 1 1 d . . . C51 C -0.1499(5) -0.1472(4) 0.33718(12) 0.0282(10) Uani 1 1 d . . . H51A H -0.0669 -0.1107 0.3255 0.042 Uiso 1 1 calc R . . H51B H -0.2443 -0.1315 0.3262 0.042 Uiso 1 1 calc R . . H51C H -0.1407 -0.2343 0.3353 0.042 Uiso 1 1 calc R . . C52 C -0.4273(6) -0.0139(5) 0.44512(16) 0.0407(13) Uani 1 1 d . . . H52A H -0.4083 0.0201 0.4696 0.061 Uiso 1 1 calc R . . H52B H -0.4828 -0.0923 0.4439 0.061 Uiso 1 1 calc R . . H52C H -0.4858 0.0406 0.4335 0.061 Uiso 1 1 calc R . . C53 C 0.1346(5) 0.0159(4) 0.44939(12) 0.0277(9) Uani 1 1 d . . . H53A H 0.1150 0.0499 0.4734 0.041 Uiso 1 1 calc R . . H53B H 0.1941 0.0752 0.4383 0.041 Uiso 1 1 calc R . . H53C H 0.1893 -0.0568 0.4495 0.041 Uiso 1 1 calc R . . C54 C 0.1922(4) 0.2619(3) 0.29293(10) 0.0176(8) Uani 1 1 d . . . C55 C 0.2901(5) 0.2356(4) 0.26547(11) 0.0216(8) Uani 1 1 d . . . H55 H 0.2857 0.2606 0.2431 0.026 Uiso 1 1 calc R . . C56 C 0.3930(4) 0.1662(3) 0.27803(10) 0.0183(8) Uani 1 1 d . . . H56 H 0.4735 0.1327 0.2655 0.022 Uiso 1 1 calc R . . C57 C 0.0533(4) 0.3266(3) 0.29379(10) 0.0174(7) Uani 1 1 d . . . C58 C 0.0567(5) 0.4511(4) 0.29210(10) 0.0192(8) Uani 1 1 d . . . C59 C -0.0761(5) 0.5080(4) 0.29351(11) 0.0228(9) Uani 1 1 d . . . H59 H -0.0736 0.5921 0.2925 0.027 Uiso 1 1 calc R . . C60 C -0.2124(5) 0.4461(4) 0.29634(11) 0.0218(8) Uani 1 1 d . . . C61 C -0.2147(5) 0.3233(4) 0.29770(11) 0.0231(9) Uani 1 1 d . . . H61 H -0.3074 0.2799 0.2997 0.028 Uiso 1 1 calc R . . C62 C -0.0846(4) 0.2619(4) 0.29622(11) 0.0201(8) Uani 1 1 d . . . C63 C 0.2007(5) 0.5249(4) 0.28904(12) 0.0251(9) Uani 1 1 d . . . H63A H 0.2257 0.5208 0.2644 0.038 Uiso 1 1 calc R . . H63B H 0.2807 0.4930 0.3019 0.038 Uiso 1 1 calc R . . H63C H 0.1889 0.6089 0.2988 0.038 Uiso 1 1 calc R . . C64 C -0.3555(5) 0.5100(4) 0.29815(13) 0.0309(10) Uani 1 1 d . . . H64A H -0.3451 0.5800 0.3163 0.046 Uiso 1 1 calc R . . H64B H -0.4373 0.4548 0.3037 0.046 Uiso 1 1 calc R . . H64C H -0.3768 0.5366 0.2756 0.046 Uiso 1 1 calc R . . C65 C -0.0932(5) 0.1281(4) 0.29772(13) 0.0272(9) Uani 1 1 d . . . H65A H -0.0565 0.1132 0.3206 0.041 Uiso 1 1 calc R . . H65B H -0.0319 0.0883 0.2796 0.041 Uiso 1 1 calc R . . H65C H -0.1969 0.0960 0.2940 0.041 Uiso 1 1 calc R . . C66 C 0.4894(5) 0.3365(3) 0.40785(11) 0.0191(8) Uani 1 1 d . . . C67 C 0.6403(4) 0.3184(4) 0.40334(12) 0.0220(9) Uani 1 1 d . . . H67 H 0.7230 0.3642 0.4151 0.026 Uiso 1 1 calc R . . C68 C 0.6429(4) 0.2197(3) 0.37807(11) 0.0191(8) Uani 1 1 d . . . H68 H 0.7297 0.1844 0.3690 0.023 Uiso 1 1 calc R . . C69 C 0.4194(4) 0.4341(3) 0.43072(11) 0.0194(8) Uani 1 1 d . . . C70 C 0.3636(5) 0.4159(4) 0.46277(12) 0.0238(9) Uani 1 1 d . . . C71 C 0.2975(6) 0.5097(4) 0.48339(12) 0.0283(10) Uani 1 1 d . . . H71 H 0.2592 0.4966 0.5053 0.034 Uiso 1 1 calc R . . C72 C 0.2872(6) 0.6208(4) 0.47235(13) 0.0326(11) Uani 1 1 d . . . C73 C 0.3479(6) 0.6391(4) 0.44048(12) 0.0303(10) Uani 1 1 d . . . H73 H 0.3443 0.7159 0.4330 0.036 Uiso 1 1 calc R . . C74 C 0.4135(5) 0.5478(4) 0.41940(11) 0.0233(9) Uani 1 1 d . . . C75 C 0.3713(6) 0.2964(4) 0.47627(13) 0.0322(11) Uani 1 1 d . . . H75A H 0.2713 0.2564 0.4756 0.048 Uiso 1 1 calc R . . H75B H 0.4111 0.3099 0.5003 0.048 Uiso 1 1 calc R . . H75C H 0.4366 0.2455 0.4616 0.048 Uiso 1 1 calc R . . C76 C 0.2174(8) 0.7218(5) 0.49519(15) 0.0477(15) Uani 1 1 d . . . H76A H 0.2516 0.7234 0.5194 0.072 Uiso 1 1 calc R . . H76B H 0.1087 0.7083 0.4936 0.072 Uiso 1 1 calc R . . H76C H 0.2466 0.7988 0.4873 0.072 Uiso 1 1 calc R . . C77 C 0.4732(6) 0.5701(4) 0.38490(13) 0.0325(10) Uani 1 1 d . . . H77A H 0.4739 0.6563 0.3831 0.049 Uiso 1 1 calc R . . H77B H 0.4098 0.5248 0.3661 0.049 Uiso 1 1 calc R . . H77C H 0.5749 0.5439 0.3829 0.049 Uiso 1 1 calc R . . C78 C 0.0132(5) 0.2482(4) 0.40273(13) 0.0252(9) Uani 1 1 d D . . H78 H -0.039(5) 0.188(3) 0.4139(12) 0.030 Uiso 1 1 d D . . C79 C 0.0544(4) 0.3382(4) 0.39073(11) 0.0189(8) Uani 1 1 d . . . C80 C 0.0504(5) 0.4677(4) 0.38849(11) 0.0198(8) Uani 1 1 d . . . C81 C -0.0664(6) 0.6418(4) 0.41266(13) 0.0293(10) Uani 1 1 d . . . H81A H -0.1116 0.6577 0.3904 0.035 Uiso 1 1 calc R . . H81B H 0.0301 0.6893 0.4168 0.035 Uiso 1 1 calc R . . C82 C -0.1694(6) 0.6734(4) 0.44243(14) 0.0332(11) Uani 1 1 d . . . H82A H -0.2643 0.6256 0.4378 0.050 Uiso 1 1 calc R . . H82B H -0.1872 0.7592 0.4446 0.050 Uiso 1 1 calc R . . H82C H -0.1235 0.6558 0.4641 0.050 Uiso 1 1 calc R . . B2 B 0.4436(5) 0.0873(4) 0.33765(11) 0.0159(8) Uani 1 1 d . . . H2A H 0.5286 0.0456 0.3263 0.019 Uiso 1 1 calc R . . Cl1 Cl 0.5835(3) 0.4636(3) 0.04407(9) 0.0579(8) Uani 0.50 1 d P . . Cl2 Cl 0.2973(4) 0.3414(4) 0.01986(9) 0.0635(9) Uani 0.50 1 d P . . C83 C 0.3990(15) 0.4601(11) 0.0446(3) 0.052(3) Uani 0.50 1 d P . . H83A H 0.3678 0.5356 0.0370 0.062 Uiso 0.50 1 calc PR . . H83B H 0.3695 0.4613 0.0691 0.062 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0145(2) 0.0210(2) 0.0264(3) 0.00743(19) 0.0036(2) 0.00218(19) O1 0.044(2) 0.0272(18) 0.062(3) 0.0155(17) -0.0095(19) 0.0020(17) N1 0.0141(15) 0.0202(16) 0.0211(16) 0.0025(12) 0.0012(13) 0.0007(13) N2 0.0110(15) 0.0206(16) 0.0222(17) 0.0048(13) 0.0001(13) 0.0018(13) N3 0.0140(15) 0.0160(15) 0.0243(17) 0.0059(12) 0.0024(13) 0.0036(13) N4 0.0117(15) 0.0198(16) 0.0211(17) 0.0032(12) 0.0015(13) -0.0012(13) N5 0.0143(15) 0.0194(16) 0.0209(16) 0.0017(12) 0.0006(13) 0.0009(13) N6 0.0142(15) 0.0181(15) 0.0204(16) 0.0010(12) 0.0024(13) 0.0021(13) C1 0.0148(18) 0.0201(19) 0.025(2) 0.0031(15) 0.0010(16) 0.0013(15) C2 0.0143(19) 0.030(2) 0.030(2) 0.0110(17) -0.0013(17) 0.0013(17) C3 0.0137(18) 0.025(2) 0.034(2) 0.0072(17) -0.0008(17) 0.0033(16) C4 0.0141(18) 0.028(2) 0.022(2) 0.0085(15) -0.0026(15) -0.0010(16) C5 0.025(2) 0.029(2) 0.023(2) 0.0059(16) -0.0025(17) 0.0003(18) C6 0.034(3) 0.034(2) 0.025(2) 0.0054(18) 0.003(2) 0.006(2) C7 0.030(2) 0.037(3) 0.023(2) 0.0096(18) -0.0003(19) 0.003(2) C8 0.027(2) 0.025(2) 0.033(2) 0.0105(17) -0.0001(19) 0.0005(18) C9 0.021(2) 0.026(2) 0.027(2) 0.0071(16) -0.0023(17) 0.0006(17) C10 0.042(3) 0.024(2) 0.033(3) 0.0038(18) 0.003(2) 0.004(2) C11 0.060(4) 0.044(3) 0.034(3) 0.016(2) 0.015(3) 0.010(3) C12 0.041(3) 0.024(2) 0.034(3) 0.0101(18) 0.006(2) 0.005(2) C13 0.0123(17) 0.0177(18) 0.0227(19) 0.0019(14) -0.0011(15) 0.0007(14) C14 0.0153(18) 0.0154(17) 0.031(2) 0.0047(15) 0.0002(16) 0.0015(15) C15 0.0158(18) 0.0209(19) 0.024(2) 0.0058(15) 0.0007(16) -0.0037(15) C16 0.0170(19) 0.0146(17) 0.026(2) 0.0052(14) 0.0021(16) 0.0047(15) C17 0.0140(18) 0.0201(19) 0.026(2) 0.0064(15) 0.0002(16) 0.0023(15) C18 0.0146(18) 0.026(2) 0.034(2) 0.0108(17) 0.0030(17) 0.0067(17) C19 0.026(2) 0.026(2) 0.033(2) 0.0113(17) 0.0070(19) 0.0081(19) C20 0.033(2) 0.020(2) 0.031(2) 0.0021(17) 0.0079(19) 0.0120(18) C21 0.021(2) 0.0197(19) 0.031(2) 0.0046(16) -0.0019(18) 0.0017(17) C22 0.017(2) 0.034(2) 0.032(2) 0.0001(18) -0.0008(18) 0.0009(18) C23 0.033(3) 0.044(3) 0.044(3) 0.010(2) 0.015(2) 0.020(2) C24 0.027(2) 0.029(2) 0.036(3) -0.0013(19) -0.005(2) 0.0010(19) C25 0.0137(17) 0.0134(16) 0.0240(19) 0.0035(14) -0.0006(15) 0.0007(14) C26 0.0196(19) 0.0161(17) 0.0209(19) 0.0025(14) 0.0003(15) 0.0029(15) C27 0.0161(18) 0.0195(18) 0.0216(19) 0.0040(14) 0.0037(15) 0.0056(15) C28 0.0190(19) 0.0163(17) 0.0191(19) -0.0002(14) 0.0007(15) 0.0035(15) C29 0.024(2) 0.0169(18) 0.023(2) 0.0024(15) -0.0015(17) -0.0013(16) C30 0.030(2) 0.025(2) 0.028(2) 0.0083(17) 0.0027(19) -0.0022(19) C31 0.022(2) 0.030(2) 0.030(2) 0.0025(18) 0.0034(18) -0.0077(18) C32 0.0176(19) 0.026(2) 0.029(2) 0.0013(17) 0.0002(17) 0.0004(17) C33 0.0152(18) 0.0171(18) 0.023(2) -0.0005(14) -0.0009(15) 0.0034(15) C34 0.030(2) 0.023(2) 0.033(2) 0.0095(17) -0.0076(19) 0.0043(18) C35 0.030(3) 0.053(3) 0.048(3) 0.013(3) 0.004(2) -0.018(2) C36 0.021(2) 0.023(2) 0.030(2) 0.0064(16) -0.0007(17) 0.0046(17) C37 0.0119(18) 0.032(2) 0.043(3) 0.0130(19) 0.0054(18) 0.0007(18) C38 0.0147(19) 0.030(2) 0.029(2) 0.0062(17) 0.0033(17) -0.0003(17) C39 0.016(2) 0.039(3) 0.043(3) 0.019(2) 0.0011(19) -0.002(2) O2A 0.016(5) 0.043(6) 0.047(5) 0.026(4) 0.004(4) -0.003(4) C40A 0.026(5) 0.043(6) 0.053(7) 0.031(5) -0.007(5) -0.015(5) C41A 0.027(6) 0.109(13) 0.055(8) 0.046(7) -0.004(5) -0.007(7) O2B 0.018(5) 0.051(6) 0.045(6) 0.032(4) 0.002(4) -0.005(4) C40B 0.027(5) 0.074(9) 0.044(7) 0.041(6) 0.001(5) 0.005(5) C41B 0.046(8) 0.074(10) 0.087(11) 0.058(8) -0.022(8) -0.027(7) B1 0.015(2) 0.019(2) 0.020(2) 0.0035(15) 0.0008(16) -0.0002(17) Cu2 0.0150(2) 0.0123(2) 0.0250(3) 0.00265(17) 0.00507(19) 0.00444(18) O3 0.0265(16) 0.0164(13) 0.0317(17) 0.0042(12) 0.0076(13) 0.0011(12) O4 0.0253(16) 0.0120(12) 0.0370(17) 0.0054(11) 0.0138(13) 0.0068(12) N7 0.0139(15) 0.0158(15) 0.0216(16) 0.0020(12) 0.0037(13) 0.0040(13) N8 0.0139(15) 0.0156(15) 0.0221(17) 0.0016(12) 0.0031(13) 0.0054(12) N9 0.0127(15) 0.0157(15) 0.0233(17) 0.0032(12) -0.0004(13) 0.0048(12) N10 0.0122(15) 0.0144(15) 0.0236(17) 0.0016(12) 0.0024(13) 0.0028(12) N11 0.0158(16) 0.0148(15) 0.0228(17) -0.0013(12) 0.0004(13) 0.0020(13) N12 0.0099(14) 0.0160(15) 0.0229(16) 0.0012(12) 0.0008(12) 0.0041(12) C42 0.0175(18) 0.0129(16) 0.0200(18) 0.0047(13) 0.0011(15) 0.0015(14) C43 0.021(2) 0.0096(16) 0.030(2) 0.0040(14) 0.0044(17) 0.0031(15) C44 0.0178(18) 0.0142(17) 0.026(2) 0.0039(14) 0.0004(16) 0.0077(15) C45 0.0184(18) 0.0083(15) 0.0220(19) 0.0055(13) 0.0035(15) 0.0029(14) C46 0.0187(19) 0.0150(17) 0.0228(19) 0.0039(14) -0.0001(15) 0.0039(15) C47 0.0153(19) 0.0172(18) 0.037(2) 0.0059(16) -0.0016(17) 0.0014(16) C48 0.022(2) 0.0160(18) 0.038(2) 0.0066(17) 0.0098(19) 0.0088(17) C49 0.029(2) 0.0143(17) 0.025(2) 0.0019(15) 0.0095(17) 0.0035(17) C50 0.0204(19) 0.0125(16) 0.024(2) 0.0046(14) 0.0018(16) 0.0016(15) C51 0.029(2) 0.028(2) 0.027(2) 0.0028(17) -0.0065(19) -0.0012(18) C52 0.029(3) 0.034(3) 0.059(3) 0.001(2) 0.019(2) 0.009(2) C53 0.030(2) 0.027(2) 0.026(2) 0.0060(17) -0.0030(19) 0.0017(19) C54 0.0161(18) 0.0160(17) 0.0208(19) 0.0022(14) -0.0001(15) 0.0029(15) C55 0.020(2) 0.023(2) 0.023(2) 0.0051(15) -0.0005(16) 0.0022(16) C56 0.0160(18) 0.0177(18) 0.0207(19) 0.0005(14) 0.0016(15) 0.0015(15) C57 0.0161(18) 0.0198(18) 0.0170(18) 0.0037(14) 0.0000(15) 0.0040(15) C58 0.0187(19) 0.0230(19) 0.0169(19) 0.0054(14) 0.0012(15) 0.0023(16) C59 0.024(2) 0.023(2) 0.022(2) 0.0031(15) 0.0018(17) 0.0085(17) C60 0.022(2) 0.027(2) 0.0174(19) 0.0056(15) 0.0004(16) 0.0097(17) C61 0.0143(18) 0.028(2) 0.028(2) 0.0049(16) 0.0016(16) 0.0025(16) C62 0.0141(18) 0.0212(19) 0.025(2) 0.0043(15) -0.0032(16) 0.0008(15) C63 0.023(2) 0.0188(19) 0.034(2) 0.0056(16) 0.0084(18) 0.0018(17) C64 0.025(2) 0.035(2) 0.035(3) 0.0073(19) -0.001(2) 0.016(2) C65 0.023(2) 0.0189(19) 0.040(3) 0.0059(17) -0.0021(19) -0.0022(17) C66 0.0156(18) 0.0181(18) 0.023(2) -0.0005(14) 0.0005(15) 0.0022(15) C67 0.0108(17) 0.0206(19) 0.033(2) -0.0007(16) -0.0026(16) 0.0020(15) C68 0.0109(17) 0.0169(18) 0.029(2) 0.0026(15) 0.0005(15) 0.0000(15) C69 0.0147(18) 0.0171(18) 0.025(2) -0.0023(15) -0.0004(15) 0.0027(15) C70 0.022(2) 0.0191(19) 0.029(2) -0.0009(16) -0.0005(17) 0.0020(16) C71 0.034(3) 0.024(2) 0.026(2) -0.0016(17) 0.0016(19) 0.0093(19) C72 0.042(3) 0.022(2) 0.032(2) -0.0054(18) -0.002(2) 0.011(2) C73 0.041(3) 0.0168(19) 0.033(2) 0.0013(17) -0.006(2) 0.0083(19) C74 0.022(2) 0.0206(19) 0.027(2) 0.0019(16) -0.0033(17) 0.0038(16) C75 0.042(3) 0.019(2) 0.037(3) 0.0063(18) 0.012(2) 0.005(2) C76 0.072(4) 0.028(2) 0.043(3) -0.008(2) 0.005(3) 0.025(3) C77 0.036(3) 0.029(2) 0.034(3) 0.0080(19) 0.000(2) 0.009(2) C78 0.0196(19) 0.022(2) 0.036(2) 0.0050(17) 0.0150(18) 0.0113(17) C79 0.0130(17) 0.0189(18) 0.025(2) 0.0023(15) 0.0036(15) 0.0050(15) C80 0.0172(18) 0.0173(18) 0.025(2) 0.0022(15) 0.0015(16) 0.0031(15) C81 0.040(3) 0.0116(17) 0.038(3) 0.0071(16) 0.014(2) 0.0071(18) C82 0.040(3) 0.0174(19) 0.044(3) 0.0037(19) 0.016(2) 0.011(2) B2 0.0136(19) 0.0148(19) 0.020(2) 0.0021(15) 0.0027(16) 0.0035(16) Cl1 0.0326(14) 0.086(2) 0.063(2) 0.0330(17) -0.0045(14) 0.0114(15) Cl2 0.059(2) 0.085(2) 0.0445(17) 0.0086(16) -0.0026(15) -0.0091(18) C83 0.061(8) 0.048(7) 0.049(7) 0.007(5) -0.017(6) 0.027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C37 1.950(4) . ? Cu1 C38 1.975(4) . ? Cu1 N1 2.000(3) . ? Cu1 N3 2.003(3) . ? Cu1 N5 2.296(3) . ? O1 C39 1.197(6) . ? N1 C1 1.342(5) . ? N1 N2 1.363(5) . ? N2 C3 1.347(5) . ? N2 B1 1.539(6) . ? N3 C13 1.334(5) . ? N3 N4 1.367(5) . ? N4 C15 1.343(5) . ? N4 B1 1.543(6) . ? N5 C25 1.341(5) . ? N5 N6 1.371(5) . ? N6 C27 1.339(5) . ? N6 B1 1.531(5) . ? C1 C2 1.396(6) . ? C1 C4 1.482(6) . ? C2 C3 1.371(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.396(6) . ? C4 C9 1.401(6) . ? C5 C6 1.393(7) . ? C5 C10 1.514(7) . ? C6 C7 1.389(7) . ? C6 H6 0.9500 . ? C7 C8 1.390(7) . ? C7 C11 1.507(7) . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 C12 1.512(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.399(6) . ? C13 C16 1.486(6) . ? C14 C15 1.377(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.404(6) . ? C16 C17 1.404(5) . ? C17 C18 1.387(6) . ? C17 C22 1.509(6) . ? C18 C19 1.388(6) . ? C18 H18 0.9500 . ? C19 C20 1.397(7) . ? C19 C23 1.501(7) . ? C20 C21 1.385(7) . ? C20 H20 0.9500 . ? C21 C24 1.516(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.402(6) . ? C25 C28 1.485(6) . ? C26 C27 1.383(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.403(6) . ? C28 C33 1.406(6) . ? C29 C30 1.395(6) . ? C29 C34 1.504(6) . ? C30 C31 1.389(7) . ? C30 H30 0.9500 . ? C31 C32 1.388(7) . ? C31 C35 1.510(6) . ? C32 C33 1.392(6) . ? C32 H32 0.9500 . ? C33 C36 1.509(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.240(7) . ? C37 H37 0.95(4) . ? C38 C39 1.461(7) . ? C39 O2A 1.306(11) . ? C39 O2B 1.422(11) . ? O2A C40A 1.451(12) . ? C40A C41A 1.558(14) . ? C40A H40A 0.9900 . ? C40A H40B 0.9900 . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? O2B C40B 1.458(12) . ? C40B C41B 1.505(13) . ? C40B H40C 0.9900 . ? C40B H40D 0.9900 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? B1 H1 1.0000 . ? Cu2 C78 1.956(4) . ? Cu2 C79 1.964(4) . ? Cu2 N7 2.000(3) . ? Cu2 N9 2.044(3) . ? Cu2 N11 2.179(3) . ? O3 C80 1.197(5) . ? O4 C80 1.344(5) . ? O4 C81 1.451(5) . ? N7 C42 1.346(5) . ? N7 N8 1.364(5) . ? N8 C44 1.340(5) . ? N8 B2 1.554(5) . ? N9 C54 1.341(5) . ? N9 N10 1.370(5) . ? N10 C56 1.347(5) . ? N10 B2 1.551(6) . ? N11 C66 1.336(5) . ? N11 N12 1.366(5) . ? N12 C68 1.345(5) . ? N12 B2 1.542(5) . ? C42 C43 1.403(5) . ? C42 C45 1.484(6) . ? C43 C44 1.383(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.398(5) . ? C45 C50 1.408(5) . ? C46 C47 1.401(6) . ? C46 C51 1.514(6) . ? C47 C48 1.379(6) . ? C47 H47 0.9500 . ? C48 C49 1.389(6) . ? C48 C52 1.497(7) . ? C49 C50 1.391(6) . ? C49 H49 0.9500 . ? C50 C53 1.513(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.407(6) . ? C54 C57 1.483(6) . ? C55 C56 1.370(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.408(6) . ? C57 C62 1.411(6) . ? C58 C59 1.389(6) . ? C58 C63 1.511(6) . ? C59 C60 1.387(6) . ? C59 H59 0.9500 . ? C60 C61 1.387(6) . ? C60 C64 1.511(6) . ? C61 C62 1.394(6) . ? C61 H61 0.9500 . ? C62 C65 1.510(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.396(6) . ? C66 C69 1.492(6) . ? C67 C68 1.378(5) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.386(6) . ? C69 C74 1.411(6) . ? C70 C71 1.403(6) . ? C70 C75 1.512(6) . ? C71 C72 1.383(7) . ? C71 H71 0.9500 . ? C72 C73 1.397(7) . ? C72 C76 1.517(6) . ? C73 C74 1.389(6) . ? C73 H73 0.9500 . ? C74 C77 1.498(7) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.212(6) . ? C78 H78 0.96(4) . ? C79 C80 1.473(6) . ? C81 C82 1.513(7) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? B2 H2A 1.0000 . ? Cl1 C83 1.659(14) . ? Cl2 C83 1.732(13) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 Cu1 C38 36.84(19) . . ? C37 Cu1 N1 146.29(18) . . ? C38 Cu1 N1 114.01(17) . . ? C37 Cu1 N3 108.51(17) . . ? C38 Cu1 N3 144.21(17) . . ? N1 Cu1 N3 94.07(14) . . ? C37 Cu1 N5 117.05(17) . . ? C38 Cu1 N5 115.32(15) . . ? N1 Cu1 N5 88.62(13) . . ? N3 Cu1 N5 85.67(13) . . ? C1 N1 N2 107.1(3) . . ? C1 N1 Cu1 136.3(3) . . ? N2 N1 Cu1 116.5(3) . . ? C3 N2 N1 109.4(3) . . ? C3 N2 B1 129.9(4) . . ? N1 N2 B1 120.5(3) . . ? C13 N3 N4 107.1(3) . . ? C13 N3 Cu1 136.9(3) . . ? N4 N3 Cu1 115.9(2) . . ? C15 N4 N3 109.6(3) . . ? C15 N4 B1 129.6(4) . . ? N3 N4 B1 120.5(3) . . ? C25 N5 N6 105.4(3) . . ? C25 N5 Cu1 143.3(3) . . ? N6 N5 Cu1 111.3(2) . . ? C27 N6 N5 110.7(3) . . ? C27 N6 B1 129.5(3) . . ? N5 N6 B1 119.7(3) . . ? N1 C1 C2 109.3(4) . . ? N1 C1 C4 122.1(4) . . ? C2 C1 C4 128.6(4) . . ? C3 C2 C1 105.8(4) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N2 C3 C2 108.4(4) . . ? N2 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? C5 C4 C9 119.9(4) . . ? C5 C4 C1 120.3(4) . . ? C9 C4 C1 119.8(4) . . ? C6 C5 C4 118.8(4) . . ? C6 C5 C10 119.5(4) . . ? C4 C5 C10 121.7(4) . . ? C7 C6 C5 122.0(5) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 118.0(4) . . ? C6 C7 C11 121.0(5) . . ? C8 C7 C11 121.0(4) . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 119.6(4) . . ? C8 C9 C12 119.8(4) . . ? C4 C9 C12 120.5(4) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 109.6(3) . . ? N3 C13 C16 121.5(4) . . ? C14 C13 C16 128.7(4) . . ? C15 C14 C13 105.4(4) . . ? C15 C14 H14 127.3 . . ? C13 C14 H14 127.3 . . ? N4 C15 C14 108.3(4) . . ? N4 C15 H15 125.8 . . ? C14 C15 H15 125.8 . . ? C21 C16 C17 119.6(4) . . ? C21 C16 C13 121.4(4) . . ? C17 C16 C13 119.1(4) . . ? C18 C17 C16 119.3(4) . . ? C18 C17 C22 119.6(4) . . ? C16 C17 C22 121.0(4) . . ? C17 C18 C19 122.2(4) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C18 C19 C20 117.5(4) . . ? C18 C19 C23 121.0(4) . . ? C20 C19 C23 121.5(5) . . ? C21 C20 C19 122.2(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C16 119.2(4) . . ? C20 C21 C24 120.0(4) . . ? C16 C21 C24 120.8(4) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 111.0(4) . . ? N5 C25 C28 120.6(3) . . ? C26 C25 C28 128.2(3) . . ? C27 C26 C25 104.4(3) . . ? C27 C26 H26 127.8 . . ? C25 C26 H26 127.8 . . ? N6 C27 C26 108.5(4) . . ? N6 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? C29 C28 C33 120.4(4) . . ? C29 C28 C25 118.8(4) . . ? C33 C28 C25 120.7(4) . . ? C30 C29 C28 119.1(4) . . ? C30 C29 C34 120.6(4) . . ? C28 C29 C34 120.2(4) . . ? C31 C30 C29 121.3(4) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 118.6(4) . . ? C32 C31 C35 120.5(5) . . ? C30 C31 C35 121.0(5) . . ? C31 C32 C33 122.2(4) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C28 118.4(4) . . ? C32 C33 C36 119.6(4) . . ? C28 C33 C36 122.0(4) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 Cu1 72.7(3) . . ? C38 C37 H37 153(3) . . ? Cu1 C37 H37 134(3) . . ? C37 C38 C39 151.4(5) . . ? C37 C38 Cu1 70.5(3) . . ? C39 C38 Cu1 138.0(3) . . ? O1 C39 O2A 117.8(6) . . ? O1 C39 O2B 128.2(6) . . ? O1 C39 C38 126.9(5) . . ? O2A C39 C38 113.8(6) . . ? O2B C39 C38 104.2(6) . . ? C39 O2A C40A 116.0(10) . . ? O2A C40A C41A 103.7(10) . . ? O2A C40A H40A 111.0 . . ? C41A C40A H40A 111.0 . . ? O2A C40A H40B 111.0 . . ? C41A C40A H40B 111.0 . . ? H40A C40A H40B 109.0 . . ? C39 O2B C40B 116.3(10) . . ? O2B C40B C41B 110.5(9) . . ? O2B C40B H40C 109.5 . . ? C41B C40B H40C 109.5 . . ? O2B C40B H40D 109.5 . . ? C41B C40B H40D 109.5 . . ? H40C C40B H40D 108.1 . . ? C40B C41B H41D 109.5 . . ? C40B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C40B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? N6 B1 N2 109.8(3) . . ? N6 B1 N4 109.7(3) . . ? N2 B1 N4 108.9(3) . . ? N6 B1 H1 109.5 . . ? N2 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? C78 Cu2 C79 36.02(18) . . ? C78 Cu2 N7 110.51(17) . . ? C79 Cu2 N7 146.47(16) . . ? C78 Cu2 N9 142.06(17) . . ? C79 Cu2 N9 115.16(16) . . ? N7 Cu2 N9 92.35(13) . . ? C78 Cu2 N11 120.66(17) . . ? C79 Cu2 N11 108.00(14) . . ? N7 Cu2 N11 91.24(13) . . ? N9 Cu2 N11 87.30(13) . . ? C80 O4 C81 115.6(3) . . ? C42 N7 N8 106.8(3) . . ? C42 N7 Cu2 137.1(3) . . ? N8 N7 Cu2 115.9(2) . . ? C44 N8 N7 109.6(3) . . ? C44 N8 B2 129.7(3) . . ? N7 N8 B2 120.7(3) . . ? C54 N9 N10 106.4(3) . . ? C54 N9 Cu2 138.2(3) . . ? N10 N9 Cu2 115.4(3) . . ? C56 N10 N9 109.8(3) . . ? C56 N10 B2 130.0(3) . . ? N9 N10 B2 120.1(3) . . ? C66 N11 N12 106.4(3) . . ? C66 N11 Cu2 140.7(3) . . ? N12 N11 Cu2 112.8(2) . . ? C68 N12 N11 109.9(3) . . ? C68 N12 B2 129.1(3) . . ? N11 N12 B2 120.3(3) . . ? N7 C42 C43 110.0(4) . . ? N7 C42 C45 120.2(3) . . ? C43 C42 C45 129.7(3) . . ? C44 C43 C42 104.4(3) . . ? C44 C43 H43 127.8 . . ? C42 C43 H43 127.8 . . ? N8 C44 C43 109.2(3) . . ? N8 C44 H44 125.4 . . ? C43 C44 H44 125.4 . . ? C46 C45 C50 119.7(4) . . ? C46 C45 C42 120.1(4) . . ? C50 C45 C42 120.2(3) . . ? C45 C46 C47 119.1(4) . . ? C45 C46 C51 121.1(4) . . ? C47 C46 C51 119.8(4) . . ? C48 C47 C46 121.9(4) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C47 C48 C49 118.2(4) . . ? C47 C48 C52 120.4(4) . . ? C49 C48 C52 121.4(4) . . ? C48 C49 C50 122.0(4) . . ? C48 C49 H49 119.0 . . ? C50 C49 H49 119.0 . . ? C49 C50 C45 119.0(4) . . ? C49 C50 C53 121.2(4) . . ? C45 C50 C53 119.8(4) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52A 109.5 . . ? C48 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C48 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N9 C54 C55 109.9(4) . . ? N9 C54 C57 120.3(4) . . ? C55 C54 C57 129.7(4) . . ? C56 C55 C54 105.1(4) . . ? C56 C55 H55 127.4 . . ? C54 C55 H55 127.4 . . ? N10 C56 C55 108.7(4) . . ? N10 C56 H56 125.7 . . ? C55 C56 H56 125.7 . . ? C58 C57 C62 119.6(4) . . ? C58 C57 C54 121.2(4) . . ? C62 C57 C54 119.2(4) . . ? C59 C58 C57 119.1(4) . . ? C59 C58 C63 118.9(4) . . ? C57 C58 C63 122.0(4) . . ? C60 C59 C58 122.1(4) . . ? C60 C59 H59 118.9 . . ? C58 C59 H59 118.9 . . ? C59 C60 C61 118.4(4) . . ? C59 C60 C64 121.2(4) . . ? C61 C60 C64 120.3(4) . . ? C60 C61 C62 121.7(4) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C61 C62 C57 119.1(4) . . ? C61 C62 C65 119.6(4) . . ? C57 C62 C65 121.3(4) . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C64 H64A 109.5 . . ? C60 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C60 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N11 C66 C67 110.5(3) . . ? N11 C66 C69 120.6(4) . . ? C67 C66 C69 128.9(3) . . ? C68 C67 C66 104.9(3) . . ? C68 C67 H67 127.6 . . ? C66 C67 H67 127.6 . . ? N12 C68 C67 108.4(4) . . ? N12 C68 H68 125.8 . . ? C67 C68 H68 125.8 . . ? C70 C69 C74 119.9(4) . . ? C70 C69 C66 121.6(4) . . ? C74 C69 C66 118.5(4) . . ? C69 C70 C71 119.8(4) . . ? C69 C70 C75 121.6(4) . . ? C71 C70 C75 118.6(4) . . ? C72 C71 C70 121.1(5) . . ? C72 C71 H71 119.4 . . ? C70 C71 H71 119.4 . . ? C71 C72 C73 118.5(4) . . ? C71 C72 C76 120.4(5) . . ? C73 C72 C76 121.1(5) . . ? C74 C73 C72 121.8(4) . . ? C74 C73 H73 119.1 . . ? C72 C73 H73 119.1 . . ? C73 C74 C69 118.9(4) . . ? C73 C74 C77 120.0(4) . . ? C69 C74 C77 121.1(4) . . ? C70 C75 H75A 109.5 . . ? C70 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C70 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C72 C76 H76A 109.5 . . ? C72 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C72 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 Cu2 72.3(3) . . ? C79 C78 H78 166(3) . . ? Cu2 C78 H78 121(3) . . ? C78 C79 C80 151.9(4) . . ? C78 C79 Cu2 71.6(3) . . ? C80 C79 Cu2 136.3(3) . . ? O3 C80 O4 125.1(4) . . ? O3 C80 C79 126.8(4) . . ? O4 C80 C79 108.2(4) . . ? O4 C81 C82 105.2(4) . . ? O4 C81 H81A 110.7 . . ? C82 C81 H81A 110.7 . . ? O4 C81 H81B 110.7 . . ? C82 C81 H81B 110.7 . . ? H81A C81 H81B 108.8 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N12 B2 N10 108.2(3) . . ? N12 B2 N8 109.8(3) . . ? N10 B2 N8 108.5(3) . . ? N12 B2 H2A 110.1 . . ? N10 B2 H2A 110.1 . . ? N8 B2 H2A 110.1 . . ? Cl1 C83 Cl2 118.7(7) . . ? Cl1 C83 H83A 107.6 . . ? Cl2 C83 H83A 107.6 . . ? Cl1 C83 H83B 107.6 . . ? Cl2 C83 H83B 107.6 . . ? H83A C83 H83B 107.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 Cu1 N1 C1 -2.2(6) . . . . ? C38 Cu1 N1 C1 22.2(4) . . . . ? N3 Cu1 N1 C1 -135.1(4) . . . . ? N5 Cu1 N1 C1 139.4(4) . . . . ? C37 Cu1 N1 N2 174.2(3) . . . . ? C38 Cu1 N1 N2 -161.4(3) . . . . ? N3 Cu1 N1 N2 41.4(3) . . . . ? N5 Cu1 N1 N2 -44.2(3) . . . . ? C1 N1 N2 C3 0.1(4) . . . . ? Cu1 N1 N2 C3 -177.3(3) . . . . ? C1 N1 N2 B1 176.8(3) . . . . ? Cu1 N1 N2 B1 -0.6(4) . . . . ? C37 Cu1 N3 C13 -15.8(5) . . . . ? C38 Cu1 N3 C13 -3.9(6) . . . . ? N1 Cu1 N3 C13 138.8(4) . . . . ? N5 Cu1 N3 C13 -132.9(4) . . . . ? C37 Cu1 N3 N4 169.9(3) . . . . ? C38 Cu1 N3 N4 -178.3(3) . . . . ? N1 Cu1 N3 N4 -35.5(3) . . . . ? N5 Cu1 N3 N4 52.8(3) . . . . ? C13 N3 N4 C15 -0.1(4) . . . . ? Cu1 N3 N4 C15 175.9(3) . . . . ? C13 N3 N4 B1 173.8(3) . . . . ? Cu1 N3 N4 B1 -10.2(4) . . . . ? C37 Cu1 N5 C25 22.6(5) . . . . ? C38 Cu1 N5 C25 -18.6(5) . . . . ? N1 Cu1 N5 C25 -134.7(5) . . . . ? N3 Cu1 N5 C25 131.2(5) . . . . ? C37 Cu1 N5 N6 -157.3(3) . . . . ? C38 Cu1 N5 N6 161.5(3) . . . . ? N1 Cu1 N5 N6 45.4(3) . . . . ? N3 Cu1 N5 N6 -48.8(3) . . . . ? C25 N5 N6 C27 0.5(4) . . . . ? Cu1 N5 N6 C27 -179.5(3) . . . . ? C25 N5 N6 B1 -179.7(3) . . . . ? Cu1 N5 N6 B1 0.2(4) . . . . ? N2 N1 C1 C2 -0.4(4) . . . . ? Cu1 N1 C1 C2 176.3(3) . . . . ? N2 N1 C1 C4 -178.2(4) . . . . ? Cu1 N1 C1 C4 -1.5(6) . . . . ? N1 C1 C2 C3 0.4(5) . . . . ? C4 C1 C2 C3 178.1(4) . . . . ? N1 N2 C3 C2 0.2(5) . . . . ? B1 N2 C3 C2 -176.1(4) . . . . ? C1 C2 C3 N2 -0.4(5) . . . . ? N1 C1 C4 C5 67.2(5) . . . . ? C2 C1 C4 C5 -110.2(5) . . . . ? N1 C1 C4 C9 -115.0(5) . . . . ? C2 C1 C4 C9 67.7(6) . . . . ? C9 C4 C5 C6 1.1(6) . . . . ? C1 C4 C5 C6 179.0(4) . . . . ? C9 C4 C5 C10 -179.1(4) . . . . ? C1 C4 C5 C10 -1.2(6) . . . . ? C4 C5 C6 C7 -2.2(7) . . . . ? C10 C5 C6 C7 177.9(5) . . . . ? C5 C6 C7 C8 2.0(7) . . . . ? C5 C6 C7 C11 -177.5(5) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C11 C7 C8 C9 178.9(5) . . . . ? C7 C8 C9 C4 -0.4(7) . . . . ? C7 C8 C9 C12 176.9(4) . . . . ? C5 C4 C9 C8 0.2(6) . . . . ? C1 C4 C9 C8 -177.7(4) . . . . ? C5 C4 C9 C12 -177.1(4) . . . . ? C1 C4 C9 C12 5.0(6) . . . . ? N4 N3 C13 C14 0.5(4) . . . . ? Cu1 N3 C13 C14 -174.2(3) . . . . ? N4 N3 C13 C16 -174.8(3) . . . . ? Cu1 N3 C13 C16 10.5(6) . . . . ? N3 C13 C14 C15 -0.7(5) . . . . ? C16 C13 C14 C15 174.2(4) . . . . ? N3 N4 C15 C14 -0.4(5) . . . . ? B1 N4 C15 C14 -173.5(4) . . . . ? C13 C14 C15 N4 0.6(5) . . . . ? N3 C13 C16 C21 -107.7(5) . . . . ? C14 C13 C16 C21 77.9(6) . . . . ? N3 C13 C16 C17 73.0(5) . . . . ? C14 C13 C16 C17 -101.4(5) . . . . ? C21 C16 C17 C18 0.9(6) . . . . ? C13 C16 C17 C18 -179.8(4) . . . . ? C21 C16 C17 C22 -178.8(4) . . . . ? C13 C16 C17 C22 0.5(6) . . . . ? C16 C17 C18 C19 -0.6(7) . . . . ? C22 C17 C18 C19 179.1(4) . . . . ? C17 C18 C19 C20 0.0(7) . . . . ? C17 C18 C19 C23 -178.9(4) . . . . ? C18 C19 C20 C21 0.3(7) . . . . ? C23 C19 C20 C21 179.3(5) . . . . ? C19 C20 C21 C16 -0.1(7) . . . . ? C19 C20 C21 C24 -179.6(4) . . . . ? C17 C16 C21 C20 -0.5(6) . . . . ? C13 C16 C21 C20 -179.9(4) . . . . ? C17 C16 C21 C24 179.0(4) . . . . ? C13 C16 C21 C24 -0.3(6) . . . . ? N6 N5 C25 C26 -0.9(4) . . . . ? Cu1 N5 C25 C26 179.2(3) . . . . ? N6 N5 C25 C28 -176.5(3) . . . . ? Cu1 N5 C25 C28 3.6(7) . . . . ? N5 C25 C26 C27 0.9(5) . . . . ? C28 C25 C26 C27 176.1(4) . . . . ? N5 N6 C27 C26 0.0(5) . . . . ? B1 N6 C27 C26 -179.6(4) . . . . ? C25 C26 C27 N6 -0.6(4) . . . . ? N5 C25 C28 C29 74.3(5) . . . . ? C26 C25 C28 C29 -100.4(5) . . . . ? N5 C25 C28 C33 -107.5(4) . . . . ? C26 C25 C28 C33 77.7(5) . . . . ? C33 C28 C29 C30 -0.4(6) . . . . ? C25 C28 C29 C30 177.7(4) . . . . ? C33 C28 C29 C34 -176.4(4) . . . . ? C25 C28 C29 C34 1.8(5) . . . . ? C28 C29 C30 C31 0.6(6) . . . . ? C34 C29 C30 C31 176.5(4) . . . . ? C29 C30 C31 C32 -0.3(7) . . . . ? C29 C30 C31 C35 -179.8(4) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C35 C31 C32 C33 179.3(4) . . . . ? C31 C32 C33 C28 0.4(6) . . . . ? C31 C32 C33 C36 -177.8(4) . . . . ? C29 C28 C33 C32 0.0(6) . . . . ? C25 C28 C33 C32 -178.2(4) . . . . ? C29 C28 C33 C36 178.1(4) . . . . ? C25 C28 C33 C36 0.0(5) . . . . ? N1 Cu1 C37 C38 38.9(5) . . . . ? N3 Cu1 C37 C38 168.5(3) . . . . ? N5 Cu1 C37 C38 -96.8(3) . . . . ? Cu1 C37 C38 C39 176.7(10) . . . . ? N1 Cu1 C38 C37 -157.6(3) . . . . ? N3 Cu1 C38 C37 -18.9(5) . . . . ? N5 Cu1 C38 C37 102.0(3) . . . . ? C37 Cu1 C38 C39 -177.6(7) . . . . ? N1 Cu1 C38 C39 24.8(5) . . . . ? N3 Cu1 C38 C39 163.5(4) . . . . ? N5 Cu1 C38 C39 -75.6(5) . . . . ? C37 C38 C39 O1 -144.8(9) . . . . ? Cu1 C38 C39 O1 30.5(8) . . . . ? C37 C38 C39 O2A 20.8(13) . . . . ? Cu1 C38 C39 O2A -164.0(6) . . . . ? C37 C38 C39 O2B 44.3(11) . . . . ? Cu1 C38 C39 O2B -140.4(6) . . . . ? O1 C39 O2A C40A -6.5(12) . . . . ? O2B C39 O2A C40A 116(2) . . . . ? C38 C39 O2A C40A -173.5(7) . . . . ? C39 O2A C40A C41A -169.5(9) . . . . ? O1 C39 O2B C40B 11.1(12) . . . . ? O2A C39 O2B C40B -61.3(19) . . . . ? C38 C39 O2B C40B -178.2(8) . . . . ? C39 O2B C40B C41B 85.1(15) . . . . ? C27 N6 B1 N2 119.6(4) . . . . ? N5 N6 B1 N2 -60.0(5) . . . . ? C27 N6 B1 N4 -120.8(4) . . . . ? N5 N6 B1 N4 59.6(5) . . . . ? C3 N2 B1 N6 -119.3(4) . . . . ? N1 N2 B1 N6 64.8(4) . . . . ? C3 N2 B1 N4 120.7(4) . . . . ? N1 N2 B1 N4 -55.2(4) . . . . ? C15 N4 B1 N6 114.5(4) . . . . ? N3 N4 B1 N6 -58.0(5) . . . . ? C15 N4 B1 N2 -125.3(4) . . . . ? N3 N4 B1 N2 62.2(4) . . . . ? C78 Cu2 N7 C42 17.2(5) . . . . ? C79 Cu2 N7 C42 14.4(6) . . . . ? N9 Cu2 N7 C42 -131.9(4) . . . . ? N11 Cu2 N7 C42 140.8(4) . . . . ? C78 Cu2 N7 N8 -169.2(3) . . . . ? C79 Cu2 N7 N8 -171.9(3) . . . . ? N9 Cu2 N7 N8 41.7(3) . . . . ? N11 Cu2 N7 N8 -45.6(3) . . . . ? C42 N7 N8 C44 0.1(4) . . . . ? Cu2 N7 N8 C44 -175.3(3) . . . . ? C42 N7 N8 B2 179.1(3) . . . . ? Cu2 N7 N8 B2 3.6(4) . . . . ? C78 Cu2 N9 C54 9.2(5) . . . . ? C79 Cu2 N9 C54 -22.5(4) . . . . ? N7 Cu2 N9 C54 137.7(4) . . . . ? N11 Cu2 N9 C54 -131.1(4) . . . . ? C78 Cu2 N9 N10 -172.4(3) . . . . ? C79 Cu2 N9 N10 155.9(2) . . . . ? N7 Cu2 N9 N10 -43.9(3) . . . . ? N11 Cu2 N9 N10 47.3(3) . . . . ? C54 N9 N10 C56 0.1(4) . . . . ? Cu2 N9 N10 C56 -178.7(2) . . . . ? C54 N9 N10 B2 179.0(3) . . . . ? Cu2 N9 N10 B2 0.1(4) . . . . ? C78 Cu2 N11 C66 -28.9(5) . . . . ? C79 Cu2 N11 C66 8.4(5) . . . . ? N7 Cu2 N11 C66 -143.7(5) . . . . ? N9 Cu2 N11 C66 124.0(5) . . . . ? C78 Cu2 N11 N12 156.1(3) . . . . ? C79 Cu2 N11 N12 -166.6(3) . . . . ? N7 Cu2 N11 N12 41.3(3) . . . . ? N9 Cu2 N11 N12 -51.0(3) . . . . ? C66 N11 N12 C68 -0.2(5) . . . . ? Cu2 N11 N12 C68 176.5(3) . . . . ? C66 N11 N12 B2 -170.9(3) . . . . ? Cu2 N11 N12 B2 5.8(4) . . . . ? N8 N7 C42 C43 0.3(4) . . . . ? Cu2 N7 C42 C43 174.3(3) . . . . ? N8 N7 C42 C45 179.9(3) . . . . ? Cu2 N7 C42 C45 -6.0(6) . . . . ? N7 C42 C43 C44 -0.6(5) . . . . ? C45 C42 C43 C44 179.8(4) . . . . ? N7 N8 C44 C43 -0.5(5) . . . . ? B2 N8 C44 C43 -179.4(4) . . . . ? C42 C43 C44 N8 0.7(5) . . . . ? N7 C42 C45 C46 104.6(4) . . . . ? C43 C42 C45 C46 -75.8(6) . . . . ? N7 C42 C45 C50 -73.6(5) . . . . ? C43 C42 C45 C50 105.9(5) . . . . ? C50 C45 C46 C47 2.2(6) . . . . ? C42 C45 C46 C47 -176.0(3) . . . . ? C50 C45 C46 C51 -177.2(4) . . . . ? C42 C45 C46 C51 4.5(6) . . . . ? C45 C46 C47 C48 0.1(6) . . . . ? C51 C46 C47 C48 179.5(4) . . . . ? C46 C47 C48 C49 -1.7(6) . . . . ? C46 C47 C48 C52 -179.9(4) . . . . ? C47 C48 C49 C50 1.0(6) . . . . ? C52 C48 C49 C50 179.2(4) . . . . ? C48 C49 C50 C45 1.3(6) . . . . ? C48 C49 C50 C53 -179.5(4) . . . . ? C46 C45 C50 C49 -2.9(5) . . . . ? C42 C45 C50 C49 175.4(4) . . . . ? C46 C45 C50 C53 177.9(4) . . . . ? C42 C45 C50 C53 -3.9(5) . . . . ? N10 N9 C54 C55 -0.9(4) . . . . ? Cu2 N9 C54 C55 177.6(3) . . . . ? N10 N9 C54 C57 176.1(3) . . . . ? Cu2 N9 C54 C57 -5.4(6) . . . . ? N9 C54 C55 C56 1.3(4) . . . . ? C57 C54 C55 C56 -175.4(4) . . . . ? N9 N10 C56 C55 0.6(4) . . . . ? B2 N10 C56 C55 -178.0(3) . . . . ? C54 C55 C56 N10 -1.1(4) . . . . ? N9 C54 C57 C58 114.8(4) . . . . ? C55 C54 C57 C58 -68.9(6) . . . . ? N9 C54 C57 C62 -65.5(5) . . . . ? C55 C54 C57 C62 110.8(5) . . . . ? C62 C57 C58 C59 1.2(6) . . . . ? C54 C57 C58 C59 -179.1(4) . . . . ? C62 C57 C58 C63 -179.2(4) . . . . ? C54 C57 C58 C63 0.5(6) . . . . ? C57 C58 C59 C60 -0.4(6) . . . . ? C63 C58 C59 C60 -180.0(4) . . . . ? C58 C59 C60 C61 -0.2(6) . . . . ? C58 C59 C60 C64 179.4(4) . . . . ? C59 C60 C61 C62 -0.2(7) . . . . ? C64 C60 C61 C62 -179.8(4) . . . . ? C60 C61 C62 C57 1.0(7) . . . . ? C60 C61 C62 C65 -179.9(4) . . . . ? C58 C57 C62 C61 -1.5(6) . . . . ? C54 C57 C62 C61 178.8(4) . . . . ? C58 C57 C62 C65 179.4(4) . . . . ? C54 C57 C62 C65 -0.4(6) . . . . ? N12 N11 C66 C67 0.0(5) . . . . ? Cu2 N11 C66 C67 -175.2(4) . . . . ? N12 N11 C66 C69 177.4(4) . . . . ? Cu2 N11 C66 C69 2.2(7) . . . . ? N11 C66 C67 C68 0.2(5) . . . . ? C69 C66 C67 C68 -176.9(4) . . . . ? N11 N12 C68 C67 0.3(5) . . . . ? B2 N12 C68 C67 169.9(4) . . . . ? C66 C67 C68 N12 -0.3(5) . . . . ? N11 C66 C69 C70 83.4(5) . . . . ? C67 C66 C69 C70 -99.8(6) . . . . ? N11 C66 C69 C74 -97.9(5) . . . . ? C67 C66 C69 C74 78.9(6) . . . . ? C74 C69 C70 C71 1.8(6) . . . . ? C66 C69 C70 C71 -179.5(4) . . . . ? C74 C69 C70 C75 -178.4(4) . . . . ? C66 C69 C70 C75 0.3(6) . . . . ? C69 C70 C71 C72 -0.2(7) . . . . ? C75 C70 C71 C72 -179.9(5) . . . . ? C70 C71 C72 C73 -1.7(7) . . . . ? C70 C71 C72 C76 -179.2(5) . . . . ? C71 C72 C73 C74 2.0(7) . . . . ? C76 C72 C73 C74 179.4(5) . . . . ? C72 C73 C74 C69 -0.4(7) . . . . ? C72 C73 C74 C77 178.2(5) . . . . ? C70 C69 C74 C73 -1.5(6) . . . . ? C66 C69 C74 C73 179.7(4) . . . . ? C70 C69 C74 C77 179.9(4) . . . . ? C66 C69 C74 C77 1.2(6) . . . . ? N7 Cu2 C78 C79 -177.4(3) . . . . ? N9 Cu2 C78 C79 -54.0(4) . . . . ? N11 Cu2 C78 C79 78.2(3) . . . . ? Cu2 C78 C79 C80 -175.9(9) . . . . ? N7 Cu2 C79 C78 4.4(5) . . . . ? N9 Cu2 C79 C78 146.7(3) . . . . ? N11 Cu2 C79 C78 -117.7(3) . . . . ? C78 Cu2 C79 C80 177.2(6) . . . . ? N7 Cu2 C79 C80 -178.4(3) . . . . ? N9 Cu2 C79 C80 -36.1(5) . . . . ? N11 Cu2 C79 C80 59.5(5) . . . . ? C81 O4 C80 O3 1.2(6) . . . . ? C81 O4 C80 C79 -178.7(4) . . . . ? C78 C79 C80 O3 -177.9(8) . . . . ? Cu2 C79 C80 O3 7.8(7) . . . . ? C78 C79 C80 O4 1.9(11) . . . . ? Cu2 C79 C80 O4 -172.4(3) . . . . ? C80 O4 C81 C82 -175.9(4) . . . . ? C68 N12 B2 N10 -112.3(4) . . . . ? N11 N12 B2 N10 56.4(4) . . . . ? C68 N12 B2 N8 129.5(4) . . . . ? N11 N12 B2 N8 -61.8(5) . . . . ? C56 N10 B2 N12 116.2(4) . . . . ? N9 N10 B2 N12 -62.4(4) . . . . ? C56 N10 B2 N8 -124.8(4) . . . . ? N9 N10 B2 N8 56.7(4) . . . . ? C44 N8 B2 N12 -123.1(4) . . . . ? N7 N8 B2 N12 58.2(5) . . . . ? C44 N8 B2 N10 118.9(4) . . . . ? N7 N8 B2 N10 -59.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.72 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.059 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.093 data_ea04810a _database_code_depnum_ccdc_archive 'CCDC 867111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 B Cu N6, C8 H6' _chemical_formula_sum 'C52 H52 B Cu N6' _chemical_formula_weight 835.35 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' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.1406(6) _cell_length_b 20.6632(15) _cell_length_c 23.8733(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.186(2) _cell_angle_gamma 90.00 _cell_volume 4473.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.27 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8922 _exptl_absorpt_correction_T_max 0.9152 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 108788 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 30.53 _reflns_number_total 13516 _reflns_number_gt 8682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2005)' _computing_cell_refinement 'APEX2 Software Suite' _computing_data_reduction 'APEX2 Software Suite' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material 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^)+(0.0433P)^2^+2.6218P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13516 _refine_ls_number_parameters 556 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.70732(3) 0.173015(11) 0.163185(11) 0.02745(7) Uani 1 1 d . . . N1 N 0.65343(17) 0.08077(7) 0.14200(6) 0.0225(3) Uani 1 1 d . . . N2 N 0.53320(17) 0.05648(7) 0.16357(6) 0.0218(3) Uani 1 1 d . . . N3 N 0.68230(17) 0.15024(7) 0.25301(6) 0.0229(3) Uani 1 1 d . . . N4 N 0.55615(17) 0.11580(7) 0.25684(6) 0.0233(3) Uani 1 1 d . . . N5 N 0.48710(17) 0.20397(7) 0.15567(6) 0.0226(3) Uani 1 1 d . . . N6 N 0.39191(17) 0.15948(7) 0.17365(7) 0.0234(3) Uani 1 1 d . . . C1 C 0.7031(2) 0.03382(8) 0.11038(7) 0.0210(4) Uani 1 1 d . . . C2 C 0.6132(2) -0.02097(9) 0.11134(8) 0.0262(4) Uani 1 1 d . . . H2 H 0.6225 -0.0609 0.0924 0.031 Uiso 1 1 calc R . . C3 C 0.5087(2) -0.00453(8) 0.14544(8) 0.0248(4) Uani 1 1 d . . . H3 H 0.4316 -0.0319 0.1547 0.030 Uiso 1 1 calc R . . C4 C 0.8386(2) 0.04413(8) 0.08326(7) 0.0209(4) Uani 1 1 d . . . C5 C 0.9758(2) 0.02564(8) 0.11225(7) 0.0235(4) Uani 1 1 d . . . C6 C 1.1037(2) 0.04265(9) 0.09035(8) 0.0279(4) Uani 1 1 d . . . H6 H 1.1962 0.0310 0.1105 0.033 Uiso 1 1 calc R . . C7 C 1.1012(2) 0.07614(9) 0.03993(8) 0.0287(4) Uani 1 1 d . . . C8 C 0.9644(2) 0.09025(9) 0.01002(8) 0.0279(4) Uani 1 1 d . . . H8 H 0.9606 0.1109 -0.0257 0.033 Uiso 1 1 calc R . . C9 C 0.8334(2) 0.07508(8) 0.03066(7) 0.0242(4) Uani 1 1 d . . . C10 C 0.9852(2) -0.01351(10) 0.16622(8) 0.0338(5) Uani 1 1 d . . . H10A H 0.9609 -0.0588 0.1571 0.051 Uiso 1 1 calc R . . H10B H 0.9153 0.0038 0.1903 0.051 Uiso 1 1 calc R . . H10C H 1.0854 -0.0109 0.1862 0.051 Uiso 1 1 calc R . . C11 C 1.2430(3) 0.09657(11) 0.01895(11) 0.0423(5) Uani 1 1 d . . . H11A H 1.2206 0.1202 -0.0167 0.064 Uiso 1 1 calc R . . H11B H 1.3018 0.0581 0.0129 0.064 Uiso 1 1 calc R . . H11C H 1.2987 0.1247 0.0470 0.064 Uiso 1 1 calc R . . C12 C 0.6871(2) 0.09236(11) -0.00269(9) 0.0363(5) Uani 1 1 d . . . H12A H 0.7037 0.1211 -0.0339 0.054 Uiso 1 1 calc R . . H12B H 0.6250 0.1143 0.0220 0.054 Uiso 1 1 calc R . . H12C H 0.6378 0.0528 -0.0178 0.054 Uiso 1 1 calc R . . C13 C 0.7425(2) 0.16169(8) 0.30656(7) 0.0246(4) Uani 1 1 d . . . C14 C 0.6546(2) 0.13477(10) 0.34450(8) 0.0318(5) Uani 1 1 d . . . H14 H 0.6718 0.1358 0.3846 0.038 Uiso 1 1 calc R . . C15 C 0.5381(2) 0.10657(9) 0.31141(8) 0.0294(4) Uani 1 1 d . . . H15 H 0.4583 0.0843 0.3247 0.035 Uiso 1 1 calc R . . C16 C 0.8824(2) 0.19850(9) 0.31905(7) 0.0257(4) Uani 1 1 d . . . C17 C 0.8849(2) 0.25671(10) 0.34937(8) 0.0296(4) Uani 1 1 d . . . C18 C 1.0151(3) 0.29234(11) 0.35791(8) 0.0351(5) Uani 1 1 d . . . H18 H 1.0165 0.3318 0.3784 0.042 Uiso 1 1 calc R . . C19 C 1.1425(3) 0.27184(12) 0.33743(9) 0.0381(5) Uani 1 1 d . . . C20 C 1.1397(2) 0.21279(11) 0.30958(9) 0.0370(5) Uani 1 1 d . . . H20 H 1.2273 0.1975 0.2964 0.044 Uiso 1 1 calc R . . C21 C 1.0124(2) 0.17522(10) 0.30043(8) 0.0295(4) Uani 1 1 d . . . C22 C 0.7487(3) 0.28339(11) 0.37096(10) 0.0421(5) Uani 1 1 d . . . H22A H 0.6650 0.2808 0.3411 0.063 Uiso 1 1 calc R . . H22B H 0.7656 0.3287 0.3822 0.063 Uiso 1 1 calc R . . H22C H 0.7271 0.2580 0.4036 0.063 Uiso 1 1 calc R . . C23 C 1.2802(3) 0.31345(15) 0.34402(11) 0.0577(8) Uani 1 1 d . . . H23A H 1.2773 0.3432 0.3119 0.087 Uiso 1 1 calc R . . H23B H 1.3675 0.2857 0.3453 0.087 Uiso 1 1 calc R . . H23C H 1.2848 0.3384 0.3791 0.087 Uiso 1 1 calc R . . C24 C 1.0159(3) 0.11045(11) 0.27158(10) 0.0387(5) Uani 1 1 d . . . H24A H 0.9590 0.0790 0.2907 0.058 Uiso 1 1 calc R . . H24B H 1.1182 0.0957 0.2732 0.058 Uiso 1 1 calc R . . H24C H 0.9727 0.1146 0.2320 0.058 Uiso 1 1 calc R . . C25 C 0.4046(2) 0.25554(8) 0.13771(7) 0.0229(4) Uani 1 1 d . . . C26 C 0.2568(2) 0.24419(10) 0.14425(8) 0.0298(4) Uani 1 1 d . . . H26 H 0.1757 0.2726 0.1350 0.036 Uiso 1 1 calc R . . C27 C 0.2540(2) 0.18312(9) 0.16700(8) 0.0271(4) Uani 1 1 d . . . H27 H 0.1688 0.1613 0.1764 0.032 Uiso 1 1 calc R . . C28 C 0.4705(2) 0.31517(8) 0.11688(8) 0.0228(4) Uani 1 1 d . . . C29 C 0.5209(2) 0.31774(9) 0.06417(8) 0.0269(4) Uani 1 1 d . . . C30 C 0.5777(2) 0.37589(10) 0.04629(9) 0.0338(5) Uani 1 1 d . . . H30 H 0.6099 0.3779 0.0100 0.041 Uiso 1 1 calc R . . C31 C 0.5885(2) 0.43063(10) 0.07984(9) 0.0339(5) Uani 1 1 d . . . C32 C 0.5380(2) 0.42689(9) 0.13202(9) 0.0334(5) Uani 1 1 d . . . H32 H 0.5452 0.4641 0.1556 0.040 Uiso 1 1 calc R . . C33 C 0.4772(2) 0.37082(9) 0.15102(8) 0.0291(4) Uani 1 1 d . . . C34 C 0.5154(3) 0.25913(11) 0.02598(9) 0.0420(5) Uani 1 1 d . . . H34A H 0.5211 0.2731 -0.0129 0.063 Uiso 1 1 calc R . . H34B H 0.4227 0.2358 0.0277 0.063 Uiso 1 1 calc R . . H34C H 0.5986 0.2305 0.0385 0.063 Uiso 1 1 calc R . . C35 C 0.6546(3) 0.49275(12) 0.06087(11) 0.0553(7) Uani 1 1 d . . . H35A H 0.5844 0.5283 0.0628 0.083 Uiso 1 1 calc R . . H35B H 0.6765 0.4879 0.0219 0.083 Uiso 1 1 calc R . . H35C H 0.7459 0.5024 0.0856 0.083 Uiso 1 1 calc R . . C36 C 0.4216(3) 0.37030(12) 0.20796(10) 0.0464(6) Uani 1 1 d . . . H36A H 0.4550 0.4095 0.2288 0.070 Uiso 1 1 calc R . . H36B H 0.4600 0.3321 0.2292 0.070 Uiso 1 1 calc R . . H36C H 0.3135 0.3690 0.2027 0.070 Uiso 1 1 calc R . . C37 C 0.8778(2) 0.19904(10) 0.12564(9) 0.0297(4) Uani 1 1 d D . . H37 H 0.925(2) 0.1718(10) 0.1035(9) 0.036 Uiso 1 1 d D . . C38 C 0.8465(2) 0.24688(9) 0.15150(8) 0.0232(4) Uani 1 1 d . . . C39 C 0.8533(2) 0.31219(8) 0.17361(8) 0.0247(4) Uani 1 1 d . . . C40 C 0.7989(3) 0.32728(10) 0.22358(8) 0.0337(5) Uani 1 1 d . . . H40 H 0.7513 0.2949 0.2430 0.040 Uiso 1 1 calc R . . C41 C 0.8137(3) 0.38951(11) 0.24543(10) 0.0466(6) Uani 1 1 d . . . H41 H 0.7771 0.3995 0.2799 0.056 Uiso 1 1 calc R . . C42 C 0.8816(3) 0.43685(11) 0.21708(11) 0.0505(7) Uani 1 1 d . . . H42 H 0.8922 0.4794 0.2322 0.061 Uiso 1 1 calc R . . C43 C 0.9339(3) 0.42249(10) 0.16683(11) 0.0462(6) Uani 1 1 d . . . H43 H 0.9797 0.4553 0.1472 0.055 Uiso 1 1 calc R . . C44 C 0.9202(2) 0.36043(10) 0.14470(10) 0.0356(5) Uani 1 1 d . . . H44 H 0.9563 0.3508 0.1100 0.043 Uiso 1 1 calc R . . C45 C 0.2268(4) 0.51523(17) 0.09513(13) 0.0686(9) Uani 1 1 d D . . H45 H 0.276(3) 0.4789(12) 0.1111(13) 0.082 Uiso 1 1 d D . . C46 C 0.1635(3) 0.55945(13) 0.07242(10) 0.0449(6) Uani 1 1 d . . . C47 C 0.0849(2) 0.61257(11) 0.04473(9) 0.0356(5) Uani 1 1 d . . . C48 C -0.0505(3) 0.60278(13) 0.01281(9) 0.0445(6) Uani 1 1 d . . . H48 H -0.0915 0.5606 0.0086 0.053 Uiso 1 1 calc R . . C49 C -0.1261(3) 0.65576(17) -0.01316(11) 0.0609(8) Uani 1 1 d . . . H49 H -0.2195 0.6496 -0.0348 0.073 Uiso 1 1 calc R . . C50 C -0.0660(4) 0.71691(16) -0.00752(12) 0.0727(10) Uani 1 1 d . . . H50 H -0.1178 0.7528 -0.0252 0.087 Uiso 1 1 calc R . . C51 C 0.0665(4) 0.72567(14) 0.02327(13) 0.0727(10) Uani 1 1 d . . . H51 H 0.1077 0.7679 0.0267 0.087 Uiso 1 1 calc R . . C52 C 0.1434(3) 0.67473(13) 0.04976(11) 0.0535(7) Uani 1 1 d . . . H52 H 0.2363 0.6820 0.0715 0.064 Uiso 1 1 calc R . . B1 B 0.4504(2) 0.09737(10) 0.20380(9) 0.0229(4) Uani 1 1 d . . . H1 H 0.3660 0.0718 0.2151 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02447(14) 0.01767(11) 0.04317(14) -0.00516(10) 0.01583(10) -0.00505(9) N1 0.0204(9) 0.0199(7) 0.0287(8) -0.0003(6) 0.0089(6) -0.0033(6) N2 0.0187(8) 0.0195(7) 0.0281(7) 0.0005(6) 0.0066(6) -0.0034(6) N3 0.0226(9) 0.0223(7) 0.0249(7) 0.0014(6) 0.0072(6) -0.0010(6) N4 0.0232(9) 0.0212(7) 0.0271(7) 0.0031(6) 0.0097(6) -0.0011(6) N5 0.0190(8) 0.0206(7) 0.0288(8) 0.0036(6) 0.0058(6) -0.0009(6) N6 0.0181(8) 0.0222(8) 0.0312(8) 0.0021(6) 0.0079(6) -0.0014(6) C1 0.0211(10) 0.0181(8) 0.0238(8) 0.0000(6) 0.0037(7) 0.0004(6) C2 0.0284(11) 0.0180(8) 0.0325(9) -0.0043(7) 0.0054(8) -0.0029(7) C3 0.0244(10) 0.0181(8) 0.0315(9) 0.0020(7) 0.0014(8) -0.0046(7) C4 0.0244(10) 0.0150(8) 0.0240(8) -0.0044(6) 0.0052(7) -0.0018(6) C5 0.0263(11) 0.0195(8) 0.0253(8) -0.0020(6) 0.0051(7) 0.0007(7) C6 0.0238(11) 0.0249(9) 0.0352(10) -0.0048(7) 0.0049(8) 0.0006(7) C7 0.0318(12) 0.0206(9) 0.0363(10) -0.0076(7) 0.0147(8) -0.0043(7) C8 0.0390(13) 0.0208(9) 0.0254(9) -0.0017(7) 0.0105(8) -0.0025(8) C9 0.0302(11) 0.0185(8) 0.0239(8) -0.0035(6) 0.0038(7) -0.0004(7) C10 0.0339(12) 0.0338(11) 0.0334(10) 0.0081(8) 0.0029(9) 0.0043(9) C11 0.0411(15) 0.0363(12) 0.0542(14) -0.0039(10) 0.0242(11) -0.0073(10) C12 0.0401(13) 0.0358(11) 0.0311(10) 0.0037(8) -0.0026(9) 0.0048(9) C13 0.0271(11) 0.0240(9) 0.0235(8) 0.0007(7) 0.0068(7) 0.0027(7) C14 0.0412(13) 0.0327(10) 0.0232(9) 0.0037(7) 0.0102(8) -0.0013(9) C15 0.0329(12) 0.0267(9) 0.0313(10) 0.0043(7) 0.0148(8) -0.0008(8) C16 0.0271(11) 0.0293(9) 0.0206(8) 0.0032(7) 0.0031(7) 0.0022(8) C17 0.0324(12) 0.0352(11) 0.0210(8) -0.0008(7) 0.0026(8) 0.0001(8) C18 0.0429(14) 0.0372(11) 0.0248(9) -0.0046(8) 0.0018(9) -0.0068(9) C19 0.0339(13) 0.0516(14) 0.0279(10) -0.0006(9) 0.0011(9) -0.0111(10) C20 0.0266(12) 0.0525(14) 0.0326(10) 0.0006(9) 0.0062(9) 0.0024(10) C21 0.0288(11) 0.0354(10) 0.0241(9) 0.0020(8) 0.0032(8) 0.0056(8) C22 0.0476(15) 0.0384(12) 0.0424(12) -0.0129(9) 0.0138(11) -0.0025(10) C23 0.0457(17) 0.079(2) 0.0484(15) -0.0095(13) 0.0057(12) -0.0266(14) C24 0.0338(13) 0.0374(12) 0.0464(12) -0.0021(9) 0.0115(10) 0.0089(9) C25 0.0219(10) 0.0220(8) 0.0252(8) 0.0007(7) 0.0042(7) 0.0026(7) C26 0.0198(11) 0.0321(10) 0.0382(10) 0.0055(8) 0.0066(8) 0.0052(8) C27 0.0174(10) 0.0306(10) 0.0344(10) 0.0021(7) 0.0079(8) -0.0001(7) C28 0.0192(10) 0.0209(9) 0.0284(9) 0.0035(7) 0.0028(7) 0.0030(6) C29 0.0252(11) 0.0276(10) 0.0285(9) 0.0003(7) 0.0057(8) -0.0017(7) C30 0.0334(12) 0.0374(11) 0.0315(10) 0.0059(8) 0.0078(9) -0.0065(9) C31 0.0336(12) 0.0264(10) 0.0413(11) 0.0066(8) 0.0028(9) -0.0045(8) C32 0.0380(13) 0.0215(9) 0.0404(11) -0.0037(8) 0.0030(9) 0.0025(8) C33 0.0311(12) 0.0264(9) 0.0297(9) 0.0002(7) 0.0041(8) 0.0030(8) C34 0.0499(15) 0.0404(12) 0.0384(12) -0.0113(9) 0.0164(10) -0.0103(10) C35 0.0680(19) 0.0395(14) 0.0579(16) 0.0121(11) 0.0053(13) -0.0223(12) C36 0.0592(17) 0.0456(14) 0.0375(12) -0.0106(10) 0.0180(11) -0.0036(12) C37 0.0270(12) 0.0268(10) 0.0379(10) -0.0058(8) 0.0148(8) -0.0084(8) C38 0.0175(10) 0.0230(9) 0.0295(9) 0.0027(7) 0.0044(7) -0.0035(7) C39 0.0217(10) 0.0195(8) 0.0319(9) -0.0010(7) -0.0006(7) -0.0019(6) C40 0.0471(14) 0.0245(9) 0.0285(9) 0.0002(8) 0.0009(9) -0.0006(9) C41 0.0740(19) 0.0300(11) 0.0334(11) -0.0085(9) -0.0034(11) 0.0016(11) C42 0.0709(18) 0.0226(10) 0.0526(14) -0.0073(9) -0.0141(13) -0.0062(11) C43 0.0478(15) 0.0239(11) 0.0656(16) 0.0066(10) 0.0026(12) -0.0101(10) C44 0.0330(13) 0.0258(10) 0.0490(12) 0.0023(9) 0.0092(10) -0.0036(8) C45 0.065(2) 0.077(2) 0.0644(19) 0.0134(16) 0.0097(15) 0.0336(17) C46 0.0376(14) 0.0566(15) 0.0418(12) 0.0000(11) 0.0103(10) 0.0099(11) C47 0.0333(13) 0.0443(12) 0.0315(10) -0.0011(9) 0.0136(9) 0.0053(9) C48 0.0381(14) 0.0628(16) 0.0343(11) 0.0031(10) 0.0115(10) 0.0019(11) C49 0.0461(17) 0.103(3) 0.0344(13) 0.0067(14) 0.0069(11) 0.0273(16) C50 0.109(3) 0.066(2) 0.0468(16) 0.0081(14) 0.0226(17) 0.048(2) C51 0.119(3) 0.0401(15) 0.0631(19) -0.0008(13) 0.026(2) 0.0145(17) C52 0.0591(18) 0.0521(15) 0.0505(14) -0.0125(12) 0.0111(13) -0.0018(13) B1 0.0200(11) 0.0202(9) 0.0299(10) 0.0020(7) 0.0081(8) -0.0023(7) _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 C37 1.967(2) . ? Cu1 N1 2.0171(15) . ? Cu1 C38 2.0284(18) . ? Cu1 N5 2.0983(16) . ? Cu1 N3 2.2349(15) . ? N1 C1 1.343(2) . ? N1 N2 1.366(2) . ? N2 C3 1.343(2) . ? N2 B1 1.546(3) . ? N3 C13 1.348(2) . ? N3 N4 1.368(2) . ? N4 C15 1.347(2) . ? N4 B1 1.542(2) . ? N5 C25 1.344(2) . ? N5 N6 1.371(2) . ? N6 C27 1.343(2) . ? N6 B1 1.534(2) . ? C1 C2 1.401(2) . ? C1 C4 1.483(3) . ? C2 C3 1.373(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.405(2) . ? C4 C5 1.407(2) . ? C5 C6 1.385(3) . ? C5 C10 1.515(3) . ? C6 C7 1.386(3) . ? C6 H6 0.9500 . ? C7 C8 1.391(3) . ? C7 C11 1.506(3) . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 C12 1.511(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.399(3) . ? C13 C16 1.486(3) . ? C14 C15 1.374(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.403(3) . ? C16 C21 1.404(3) . ? C17 C18 1.392(3) . ? C17 C22 1.510(3) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.388(3) . ? C19 C23 1.516(3) . ? C20 C21 1.393(3) . ? C20 H20 0.9500 . ? C21 C24 1.507(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.399(3) . ? C25 C28 1.484(2) . ? C26 C27 1.375(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.394(3) . ? C28 C33 1.406(3) . ? C29 C30 1.397(3) . ? C29 C34 1.513(3) . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 C32 1.384(3) . ? C31 C35 1.512(3) . ? C32 C33 1.386(3) . ? C32 H32 0.9500 . ? C33 C36 1.510(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.218(3) . ? C37 H37 0.918(15) . ? C38 C39 1.448(2) . ? C39 C40 1.384(3) . ? C39 C44 1.396(3) . ? C40 C41 1.388(3) . ? C40 H40 0.9500 . ? C41 C42 1.380(4) . ? C41 H41 0.9500 . ? C42 C43 1.378(4) . ? C42 H42 0.9500 . ? C43 C44 1.387(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.177(4) . ? C45 H45 0.933(17) . ? C46 C47 1.428(3) . ? C47 C48 1.385(3) . ? C47 C52 1.391(3) . ? C48 C49 1.398(4) . ? C48 H48 0.9500 . ? C49 C50 1.377(5) . ? C49 H49 0.9500 . ? C50 C51 1.348(5) . ? C50 H50 0.9500 . ? C51 C52 1.375(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? B1 H1 1.0000 . ? 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 C37 Cu1 N1 109.06(7) . . ? C37 Cu1 C38 35.46(8) . . ? N1 Cu1 C38 144.51(7) . . ? C37 Cu1 N5 133.14(8) . . ? N1 Cu1 N5 93.73(6) . . ? C38 Cu1 N5 111.73(7) . . ? C37 Cu1 N3 132.58(7) . . ? N1 Cu1 N3 89.46(6) . . ? C38 Cu1 N3 115.57(6) . . ? N5 Cu1 N3 86.22(6) . . ? C1 N1 N2 106.91(14) . . ? C1 N1 Cu1 137.27(13) . . ? N2 N1 Cu1 115.81(11) . . ? C3 N2 N1 109.47(15) . . ? C3 N2 B1 129.65(16) . . ? N1 N2 B1 120.85(14) . . ? C13 N3 N4 106.01(15) . . ? C13 N3 Cu1 142.59(13) . . ? N4 N3 Cu1 111.22(10) . . ? C15 N4 N3 110.16(15) . . ? C15 N4 B1 128.25(17) . . ? N3 N4 B1 121.40(15) . . ? C25 N5 N6 106.17(15) . . ? C25 N5 Cu1 139.73(13) . . ? N6 N5 Cu1 114.10(11) . . ? C27 N6 N5 110.02(15) . . ? C27 N6 B1 128.78(16) . . ? N5 N6 B1 120.68(15) . . ? N1 C1 C2 109.54(16) . . ? N1 C1 C4 120.08(15) . . ? C2 C1 C4 130.32(16) . . ? C3 C2 C1 105.25(16) . . ? C3 C2 H2 127.4 . . ? C1 C2 H2 127.4 . . ? N2 C3 C2 108.84(17) . . ? N2 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? C9 C4 C5 119.46(18) . . ? C9 C4 C1 121.25(16) . . ? C5 C4 C1 119.20(16) . . ? C6 C5 C4 119.20(17) . . ? C6 C5 C10 119.76(17) . . ? C4 C5 C10 121.03(18) . . ? C5 C6 C7 122.14(18) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 117.79(19) . . ? C6 C7 C11 120.5(2) . . ? C8 C7 C11 121.73(19) . . ? C9 C8 C7 122.09(18) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C4 119.10(17) . . ? C8 C9 C12 120.40(17) . . ? C4 C9 C12 120.50(18) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.16(17) . . ? N3 C13 C16 121.29(17) . . ? C14 C13 C16 128.54(17) . . ? C15 C14 C13 105.24(17) . . ? C15 C14 H14 127.4 . . ? C13 C14 H14 127.4 . . ? N4 C15 C14 108.43(18) . . ? N4 C15 H15 125.8 . . ? C14 C15 H15 125.8 . . ? C17 C16 C21 119.85(19) . . ? C17 C16 C13 120.02(18) . . ? C21 C16 C13 120.13(17) . . ? C18 C17 C16 119.1(2) . . ? C18 C17 C22 118.88(19) . . ? C16 C17 C22 121.92(19) . . ? C19 C18 C17 121.9(2) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 118.2(2) . . ? C18 C19 C23 120.9(2) . . ? C20 C19 C23 120.8(2) . . ? C19 C20 C21 122.0(2) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.86(19) . . ? C20 C21 C24 120.1(2) . . ? C16 C21 C24 121.05(19) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 110.04(16) . . ? N5 C25 C28 121.98(16) . . ? C26 C25 C28 127.92(16) . . ? C27 C26 C25 105.30(17) . . ? C27 C26 H26 127.3 . . ? C25 C26 H26 127.3 . . ? N6 C27 C26 108.47(17) . . ? N6 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? C29 C28 C33 119.77(17) . . ? C29 C28 C25 121.86(16) . . ? C33 C28 C25 118.33(17) . . ? C28 C29 C30 119.09(18) . . ? C28 C29 C34 121.56(18) . . ? C30 C29 C34 119.35(19) . . ? C31 C30 C29 121.9(2) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 117.93(19) . . ? C30 C31 C35 121.5(2) . . ? C32 C31 C35 120.5(2) . . ? C31 C32 C33 122.27(19) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C28 118.96(19) . . ? C32 C33 C36 119.65(19) . . ? C28 C33 C36 121.39(18) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 Cu1 75.01(14) . . ? C38 C37 H37 161.4(15) . . ? Cu1 C37 H37 123.6(15) . . ? C37 C38 C39 159.9(2) . . ? C37 C38 Cu1 69.53(13) . . ? C39 C38 Cu1 130.59(15) . . ? C40 C39 C44 119.48(18) . . ? C40 C39 C38 121.36(18) . . ? C44 C39 C38 119.13(19) . . ? C39 C40 C41 120.3(2) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.1(2) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120.0(2) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.4(2) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 119.7(2) . . ? C43 C44 H44 120.1 . . ? C39 C44 H44 120.1 . . ? C46 C45 H45 177(2) . . ? C45 C46 C47 179.2(3) . . ? C48 C47 C52 119.3(2) . . ? C48 C47 C46 120.4(2) . . ? C52 C47 C46 120.3(2) . . ? C47 C48 C49 119.2(3) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C50 C49 C48 120.4(3) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C51 C50 C49 119.8(3) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 121.4(3) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C51 C52 C47 119.9(3) . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? N6 B1 N4 108.93(14) . . ? N6 B1 N2 109.54(15) . . ? N4 B1 N2 109.85(15) . . ? N6 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? N2 B1 H1 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 Cu1 N1 C1 0.8(2) . . . . ? C38 Cu1 N1 C1 2.3(2) . . . . ? N5 Cu1 N1 C1 139.20(18) . . . . ? N3 Cu1 N1 C1 -134.63(18) . . . . ? C37 Cu1 N1 N2 -177.95(12) . . . . ? C38 Cu1 N1 N2 -176.50(11) . . . . ? N5 Cu1 N1 N2 -39.57(12) . . . . ? N3 Cu1 N1 N2 46.60(12) . . . . ? C1 N1 N2 C3 -0.15(19) . . . . ? Cu1 N1 N2 C3 178.98(11) . . . . ? C1 N1 N2 B1 178.19(14) . . . . ? Cu1 N1 N2 B1 -2.68(19) . . . . ? C37 Cu1 N3 C13 24.8(2) . . . . ? N1 Cu1 N3 C13 140.5(2) . . . . ? C38 Cu1 N3 C13 -13.4(2) . . . . ? N5 Cu1 N3 C13 -125.7(2) . . . . ? C37 Cu1 N3 N4 -161.32(12) . . . . ? N1 Cu1 N3 N4 -45.54(12) . . . . ? C38 Cu1 N3 N4 160.55(11) . . . . ? N5 Cu1 N3 N4 48.24(11) . . . . ? C13 N3 N4 C15 0.5(2) . . . . ? Cu1 N3 N4 C15 -175.70(12) . . . . ? C13 N3 N4 B1 175.88(16) . . . . ? Cu1 N3 N4 B1 -0.29(19) . . . . ? C37 Cu1 N5 C25 -21.5(2) . . . . ? N1 Cu1 N5 C25 -142.18(19) . . . . ? C38 Cu1 N5 C25 12.6(2) . . . . ? N3 Cu1 N5 C25 128.61(19) . . . . ? C37 Cu1 N5 N6 157.76(12) . . . . ? N1 Cu1 N5 N6 37.12(12) . . . . ? C38 Cu1 N5 N6 -168.15(11) . . . . ? N3 Cu1 N5 N6 -52.09(12) . . . . ? C25 N5 N6 C27 -0.1(2) . . . . ? Cu1 N5 N6 C27 -179.62(12) . . . . ? C25 N5 N6 B1 -172.54(15) . . . . ? Cu1 N5 N6 B1 7.9(2) . . . . ? N2 N1 C1 C2 0.43(19) . . . . ? Cu1 N1 C1 C2 -178.41(13) . . . . ? N2 N1 C1 C4 -176.88(14) . . . . ? Cu1 N1 C1 C4 4.3(3) . . . . ? N1 C1 C2 C3 -0.5(2) . . . . ? C4 C1 C2 C3 176.41(17) . . . . ? N1 N2 C3 C2 -0.2(2) . . . . ? B1 N2 C3 C2 -178.34(16) . . . . ? C1 C2 C3 N2 0.4(2) . . . . ? N1 C1 C4 C9 -85.1(2) . . . . ? C2 C1 C4 C9 98.2(2) . . . . ? N1 C1 C4 C5 91.4(2) . . . . ? C2 C1 C4 C5 -85.3(2) . . . . ? C9 C4 C5 C6 4.8(2) . . . . ? C1 C4 C5 C6 -171.80(16) . . . . ? C9 C4 C5 C10 -174.04(17) . . . . ? C1 C4 C5 C10 9.4(2) . . . . ? C4 C5 C6 C7 -1.5(3) . . . . ? C10 C5 C6 C7 177.32(17) . . . . ? C5 C6 C7 C8 -2.6(3) . . . . ? C5 C6 C7 C11 177.02(18) . . . . ? C6 C7 C8 C9 3.6(3) . . . . ? C11 C7 C8 C9 -176.04(18) . . . . ? C7 C8 C9 C4 -0.4(3) . . . . ? C7 C8 C9 C12 178.87(17) . . . . ? C5 C4 C9 C8 -3.8(2) . . . . ? C1 C4 C9 C8 172.67(16) . . . . ? C5 C4 C9 C12 176.88(16) . . . . ? C1 C4 C9 C12 -6.6(2) . . . . ? N4 N3 C13 C14 -0.2(2) . . . . ? Cu1 N3 C13 C14 173.91(16) . . . . ? N4 N3 C13 C16 -179.90(16) . . . . ? Cu1 N3 C13 C16 -5.8(3) . . . . ? N3 C13 C14 C15 -0.1(2) . . . . ? C16 C13 C14 C15 179.55(19) . . . . ? N3 N4 C15 C14 -0.6(2) . . . . ? B1 N4 C15 C14 -175.56(17) . . . . ? C13 C14 C15 N4 0.4(2) . . . . ? N3 C13 C16 C17 119.0(2) . . . . ? C14 C13 C16 C17 -60.7(3) . . . . ? N3 C13 C16 C21 -60.9(2) . . . . ? C14 C13 C16 C21 119.5(2) . . . . ? C21 C16 C17 C18 3.4(3) . . . . ? C13 C16 C17 C18 -176.43(17) . . . . ? C21 C16 C17 C22 -179.21(18) . . . . ? C13 C16 C17 C22 1.0(3) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? C22 C17 C18 C19 -177.6(2) . . . . ? C17 C18 C19 C20 -2.5(3) . . . . ? C17 C18 C19 C23 176.1(2) . . . . ? C18 C19 C20 C21 2.0(3) . . . . ? C23 C19 C20 C21 -176.6(2) . . . . ? C19 C20 C21 C16 1.2(3) . . . . ? C19 C20 C21 C24 -178.1(2) . . . . ? C17 C16 C21 C20 -3.9(3) . . . . ? C13 C16 C21 C20 175.92(17) . . . . ? C17 C16 C21 C24 175.40(18) . . . . ? C13 C16 C21 C24 -4.8(3) . . . . ? N6 N5 C25 C26 0.1(2) . . . . ? Cu1 N5 C25 C26 179.44(15) . . . . ? N6 N5 C25 C28 177.70(15) . . . . ? Cu1 N5 C25 C28 -3.0(3) . . . . ? N5 C25 C26 C27 -0.1(2) . . . . ? C28 C25 C26 C27 -177.49(18) . . . . ? N5 N6 C27 C26 0.0(2) . . . . ? B1 N6 C27 C26 171.70(18) . . . . ? C25 C26 C27 N6 0.0(2) . . . . ? N5 C25 C28 C29 74.1(2) . . . . ? C26 C25 C28 C29 -108.8(2) . . . . ? N5 C25 C28 C33 -107.9(2) . . . . ? C26 C25 C28 C33 69.2(3) . . . . ? C33 C28 C29 C30 0.1(3) . . . . ? C25 C28 C29 C30 178.08(18) . . . . ? C33 C28 C29 C34 -179.82(19) . . . . ? C25 C28 C29 C34 -1.9(3) . . . . ? C28 C29 C30 C31 1.5(3) . . . . ? C34 C29 C30 C31 -178.6(2) . . . . ? C29 C30 C31 C32 -1.3(3) . . . . ? C29 C30 C31 C35 178.0(2) . . . . ? C30 C31 C32 C33 -0.4(3) . . . . ? C35 C31 C32 C33 -179.8(2) . . . . ? C31 C32 C33 C28 1.9(3) . . . . ? C31 C32 C33 C36 -178.9(2) . . . . ? C29 C28 C33 C32 -1.8(3) . . . . ? C25 C28 C33 C32 -179.79(17) . . . . ? C29 C28 C33 C36 179.05(19) . . . . ? C25 C28 C33 C36 1.0(3) . . . . ? N1 Cu1 C37 C38 178.55(12) . . . . ? N5 Cu1 C37 C38 63.83(16) . . . . ? N3 Cu1 C37 C38 -73.75(16) . . . . ? N1 Cu1 C38 C37 -2.36(19) . . . . ? N5 Cu1 C38 C37 -135.17(13) . . . . ? N3 Cu1 C38 C37 128.40(13) . . . . ? C37 Cu1 C38 C39 -179.6(2) . . . . ? N1 Cu1 C38 C39 178.07(13) . . . . ? N5 Cu1 C38 C39 45.26(18) . . . . ? N3 Cu1 C38 C39 -51.17(18) . . . . ? C37 C38 C39 C40 -153.6(5) . . . . ? Cu1 C38 C39 C40 25.2(3) . . . . ? C37 C38 C39 C44 24.4(6) . . . . ? Cu1 C38 C39 C44 -156.74(15) . . . . ? C44 C39 C40 C41 -1.4(3) . . . . ? C38 C39 C40 C41 176.62(19) . . . . ? C39 C40 C41 C42 0.6(3) . . . . ? C40 C41 C42 C43 0.4(4) . . . . ? C41 C42 C43 C44 -0.6(4) . . . . ? C42 C43 C44 C39 -0.2(3) . . . . ? C40 C39 C44 C43 1.2(3) . . . . ? C38 C39 C44 C43 -176.90(19) . . . . ? C52 C47 C48 C49 -0.7(4) . . . . ? C46 C47 C48 C49 179.0(2) . . . . ? C47 C48 C49 C50 0.6(4) . . . . ? C48 C49 C50 C51 0.0(4) . . . . ? C49 C50 C51 C52 -0.5(5) . . . . ? C50 C51 C52 C47 0.5(5) . . . . ? C48 C47 C52 C51 0.1(4) . . . . ? C46 C47 C52 C51 -179.6(3) . . . . ? C27 N6 B1 N4 -112.9(2) . . . . ? N5 N6 B1 N4 58.0(2) . . . . ? C27 N6 B1 N2 126.91(19) . . . . ? N5 N6 B1 N2 -62.2(2) . . . . ? C15 N4 B1 N6 113.3(2) . . . . ? N3 N4 B1 N6 -61.2(2) . . . . ? C15 N4 B1 N2 -126.74(19) . . . . ? N3 N4 B1 N2 58.7(2) . . . . ? C3 N2 B1 N6 -122.18(19) . . . . ? N1 N2 B1 N6 59.9(2) . . . . ? C3 N2 B1 N4 118.21(19) . . . . ? N1 N2 B1 N4 -59.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.335 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.055