# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Tim Dunn' 'Linus Chiang' 'Caterina Ramogida' 'Michael Webb' 'Didier Savard' 'Miyuki Sakaguchi' 'Takashi Ogura' 'Yuichi Shimazaki' 'Tim Storr' _publ_contact_author_name 'Tim Storr' _publ_contact_author_email tsa34@sfu.ca data_ts002_0m _database_code_depnum_ccdc_archive 'CCDC 869730' #TrackingRef '- cuflat_Storr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H90 Cu2 N4 O4' _chemical_formula_weight 1046.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2468(12) _cell_length_b 15.1120(14) _cell_length_c 15.5449(14) _cell_angle_alpha 71.939(4) _cell_angle_beta 71.130(4) _cell_angle_gamma 85.922(4) _cell_volume 2798.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.90 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max o.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45523 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12299 _reflns_number_gt 9416 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.3420P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12299 _refine_ls_number_parameters 717 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _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 C1 C 0.11253(18) 0.52603(15) 0.12582(16) 0.0206(5) Uani 1 1 d . . . C2 C 0.21018(18) 0.51281(15) 0.14879(17) 0.0215(5) Uani 1 1 d . . . C3 C 0.28876(18) 0.58170(16) 0.10337(17) 0.0227(5) Uani 1 1 d . . . H3 H 0.3537 0.5716 0.1180 0.027 Uiso 1 1 calc R . . C4 C 0.27851(18) 0.66612(16) 0.03655(18) 0.0241(5) Uani 1 1 d . . . C5 C 0.18524(19) 0.67851(16) 0.01562(17) 0.0241(5) Uani 1 1 d . . . H5 H 0.1768 0.7353 -0.0294 0.029 Uiso 1 1 calc R . . C6 C 0.10009(18) 0.61120(15) 0.05738(16) 0.0204(5) Uani 1 1 d . . . C7 C 0.22429(18) 0.42445(16) 0.22560(17) 0.0234(5) Uani 1 1 d . . . C8 C 0.1410(2) 0.42162(18) 0.32138(18) 0.0307(6) Uani 1 1 d . . . H8A H 0.1485 0.4784 0.3369 0.046 Uiso 1 1 calc R . . H8B H 0.1518 0.3672 0.3714 0.046 Uiso 1 1 calc R . . H8C H 0.0693 0.4175 0.3172 0.046 Uiso 1 1 calc R . . C9 C 0.2126(2) 0.33685(16) 0.19908(19) 0.0278(6) Uani 1 1 d . . . H9A H 0.1400 0.3319 0.1973 0.042 Uiso 1 1 calc R . . H9B H 0.2264 0.2817 0.2468 0.042 Uiso 1 1 calc R . . H9C H 0.2641 0.3410 0.1362 0.042 Uiso 1 1 calc R . . C10 C 0.3348(2) 0.42307(18) 0.2374(2) 0.0308(6) Uani 1 1 d . . . H10A H 0.3898 0.4254 0.1768 0.046 Uiso 1 1 calc R . . H10B H 0.3409 0.3658 0.2866 0.046 Uiso 1 1 calc R . . H10C H 0.3443 0.4771 0.2565 0.046 Uiso 1 1 calc R . . C11 C 0.3708(2) 0.73879(17) -0.00758(19) 0.0301(6) Uani 1 1 d . . . C12 C 0.4678(2) 0.69924(19) -0.0680(2) 0.0363(7) Uani 1 1 d . . . H12A H 0.4862 0.6404 -0.0281 0.054 Uiso 1 1 calc R . . H12B H 0.5284 0.7438 -0.0937 0.054 Uiso 1 1 calc R . . H12C H 0.4507 0.6883 -0.1207 0.054 Uiso 1 1 calc R . . C13 C 0.3986(2) 0.7604(2) 0.0724(2) 0.0414(7) Uani 1 1 d . . . H13A H 0.3367 0.7867 0.1101 0.062 Uiso 1 1 calc R . . H13B H 0.4590 0.8053 0.0445 0.062 Uiso 1 1 calc R . . H13C H 0.4177 0.7028 0.1138 0.062 Uiso 1 1 calc R . . C14 C 0.3426(2) 0.82962(18) -0.0718(2) 0.0376(7) Uani 1 1 d . . . H14A H 0.3279 0.8174 -0.1250 0.056 Uiso 1 1 calc R . . H14B H 0.4026 0.8747 -0.0968 0.056 Uiso 1 1 calc R . . H14C H 0.2792 0.8549 -0.0347 0.056 Uiso 1 1 calc R . . C15 C 0.00269(18) 0.63255(15) 0.03157(16) 0.0185(5) Uani 1 1 d . . . C16 C -0.0030(2) 0.72335(17) -0.04327(18) 0.0292(6) Uani 1 1 d . . . H16A H -0.0406 0.7125 -0.0841 0.044 Uiso 1 1 calc R . . H16B H 0.0695 0.7478 -0.0823 0.044 Uiso 1 1 calc R . . H16C H -0.0414 0.7685 -0.0119 0.044 Uiso 1 1 calc R . . C17 C -0.17729(19) 0.59848(16) 0.04405(18) 0.0247(5) Uani 1 1 d . . . H17A H -0.1732 0.5737 -0.0089 0.030 Uiso 1 1 calc R . . H17B H -0.1834 0.6669 0.0216 0.030 Uiso 1 1 calc R . . C18 C -0.27482(19) 0.55604(16) 0.12899(19) 0.0253(5) Uani 1 1 d . . . C19 C -0.2962(2) 0.60934(18) 0.2012(2) 0.0361(7) Uani 1 1 d . . . H19A H -0.3566 0.5795 0.2574 0.054 Uiso 1 1 calc R . . H19B H -0.3132 0.6737 0.1724 0.054 Uiso 1 1 calc R . . H19C H -0.2327 0.6092 0.2205 0.054 Uiso 1 1 calc R . . C20 C -0.3697(2) 0.55950(19) 0.0927(2) 0.0379(7) Uani 1 1 d . . . H20A H -0.3583 0.5175 0.0536 0.057 Uiso 1 1 calc R . . H20B H -0.3765 0.6232 0.0541 0.057 Uiso 1 1 calc R . . H20C H -0.4351 0.5400 0.1471 0.057 Uiso 1 1 calc R . . C21 C -0.31554(18) 0.39325(16) 0.21732(17) 0.0223(5) Uani 1 1 d . . . H21 H -0.3866 0.4078 0.2176 0.027 Uiso 1 1 calc R . . C22 C -0.29802(18) 0.29932(16) 0.26535(16) 0.0201(5) Uani 1 1 d . . . C23 C -0.19633(17) 0.26826(15) 0.27058(15) 0.0179(5) Uani 1 1 d . . . C24 C -0.18624(17) 0.16845(15) 0.31856(15) 0.0169(4) Uani 1 1 d . . . C25 C -0.28139(18) 0.11321(15) 0.36709(16) 0.0186(5) Uani 1 1 d . . . C26 C -0.38159(18) 0.14869(16) 0.35965(17) 0.0229(5) Uani 1 1 d . . . H26 H -0.4437 0.1091 0.3906 0.028 Uiso 1 1 calc R . . C27 C -0.38945(18) 0.23765(17) 0.30935(17) 0.0240(5) Uani 1 1 d . . . H27 H -0.4565 0.2596 0.3031 0.029 Uiso 1 1 calc R . . C28 C -0.28397(17) 0.02193(15) 0.43244(16) 0.0182(5) Uani 1 1 d . . . H28 H -0.3518 -0.0093 0.4643 0.022 Uiso 1 1 calc R . . C29 C -0.21942(17) -0.11445(15) 0.52643(16) 0.0187(5) Uani 1 1 d . . . C30 C -0.2312(2) -0.18839(17) 0.48177(18) 0.0278(6) Uani 1 1 d . . . H30A H -0.2932 -0.1754 0.4590 0.042 Uiso 1 1 calc R . . H30B H -0.2411 -0.2499 0.5296 0.042 Uiso 1 1 calc R . . H30C H -0.1667 -0.1874 0.4280 0.042 Uiso 1 1 calc R . . C31 C -0.31505(18) -0.11787(17) 0.61452(17) 0.0261(5) Uani 1 1 d . . . H31A H -0.3115 -0.0635 0.6353 0.039 Uiso 1 1 calc R . . H31B H -0.3139 -0.1749 0.6659 0.039 Uiso 1 1 calc R . . H31C H -0.3812 -0.1174 0.5990 0.039 Uiso 1 1 calc R . . C32 C -0.11805(17) -0.12858(16) 0.55489(16) 0.0192(5) Uani 1 1 d . . . H32A H -0.1225 -0.0944 0.6009 0.023 Uiso 1 1 calc R . . H32B H -0.1117 -0.1956 0.5866 0.023 Uiso 1 1 calc R . . C33 C 0.06560(17) -0.13920(15) 0.46236(15) 0.0168(4) Uani 1 1 d . . . C34 C 0.06863(19) -0.23313(16) 0.53343(17) 0.0247(5) Uani 1 1 d . . . H34A H 0.0540 -0.2260 0.5968 0.037 Uiso 1 1 calc R . . H34B H 0.1394 -0.2590 0.5141 0.037 Uiso 1 1 calc R . . H34C H 0.0145 -0.2753 0.5355 0.037 Uiso 1 1 calc R . . C35 C 0.16189(17) -0.10273(15) 0.38231(16) 0.0175(4) Uani 1 1 d . . . C36 C 0.26123(18) -0.13937(16) 0.38941(16) 0.0197(5) Uani 1 1 d . . . H36 H 0.2629 -0.1823 0.4483 0.024 Uiso 1 1 calc R . . C37 C 0.35495(18) -0.11607(16) 0.31570(17) 0.0211(5) Uani 1 1 d . . . C38 C 0.34755(18) -0.05690(15) 0.22779(17) 0.0206(5) Uani 1 1 d . . . H38 H 0.4104 -0.0443 0.1739 0.025 Uiso 1 1 calc R . . C39 C 0.25481(17) -0.01635(15) 0.21543(16) 0.0179(5) Uani 1 1 d . . . C40 C 0.15976(17) -0.03246(15) 0.29664(16) 0.0169(4) Uani 1 1 d . . . C41 C 0.46397(19) -0.14990(18) 0.32483(18) 0.0271(5) Uani 1 1 d . . . C42 C 0.5185(3) -0.1987(3) 0.2514(2) 0.0517(9) Uani 1 1 d . . . H42A H 0.4742 -0.2524 0.2613 0.078 Uiso 1 1 calc R . . H42B H 0.5880 -0.2199 0.2581 0.078 Uiso 1 1 calc R . . H42C H 0.5288 -0.1554 0.1873 0.078 Uiso 1 1 calc R . . C43 C 0.5318(3) -0.0665(2) 0.3121(3) 0.0693(12) Uani 1 1 d . . . H43A H 0.6012 -0.0876 0.3190 0.104 Uiso 1 1 calc R . . H43B H 0.4953 -0.0361 0.3606 0.104 Uiso 1 1 calc R . . H43C H 0.5424 -0.0221 0.2485 0.104 Uiso 1 1 calc R . . C44 C 0.4553(2) -0.2173(3) 0.4227(2) 0.0505(9) Uani 1 1 d . . . H44A H 0.4137 -0.2730 0.4335 0.076 Uiso 1 1 calc R . . H44B H 0.4197 -0.1873 0.4718 0.076 Uiso 1 1 calc R . . H44C H 0.5269 -0.2349 0.4259 0.076 Uiso 1 1 calc R . . C45 C 0.25254(18) 0.04823(16) 0.11783(16) 0.0219(5) Uani 1 1 d . . . C46 C 0.1631(2) 0.01918(19) 0.08894(18) 0.0314(6) Uani 1 1 d . . . H46A H 0.1721 -0.0455 0.0880 0.047 Uiso 1 1 calc R . . H46B H 0.1659 0.0599 0.0253 0.047 Uiso 1 1 calc R . . H46C H 0.0939 0.0245 0.1351 0.047 Uiso 1 1 calc R . . C47 C 0.2372(2) 0.14878(17) 0.12199(19) 0.0317(6) Uani 1 1 d . . . H47A H 0.1678 0.1529 0.1685 0.048 Uiso 1 1 calc R . . H47B H 0.2398 0.1907 0.0589 0.048 Uiso 1 1 calc R . . H47C H 0.2942 0.1669 0.1412 0.048 Uiso 1 1 calc R . . C48 C 0.3573(2) 0.04700(18) 0.03884(18) 0.0317(6) Uani 1 1 d . . . H48A H 0.4161 0.0695 0.0527 0.048 Uiso 1 1 calc R . . H48B H 0.3524 0.0875 -0.0225 0.048 Uiso 1 1 calc R . . H48C H 0.3705 -0.0168 0.0357 0.048 Uiso 1 1 calc R . . N1 N -0.08006(15) 0.57610(13) 0.07149(13) 0.0190(4) Uani 1 1 d . . . N2 N -0.24524(15) 0.46028(13) 0.17364(14) 0.0207(4) Uani 1 1 d . . . N3 N -0.20350(14) -0.02197(13) 0.45235(13) 0.0178(4) Uani 1 1 d . . . N4 N -0.02337(14) -0.09527(13) 0.47110(13) 0.0172(4) Uani 1 1 d . . . O1 O 0.04058(13) 0.45806(11) 0.16897(12) 0.0251(4) Uani 1 1 d . . . O2 O -0.11112(12) 0.32139(10) 0.23635(12) 0.0215(3) Uani 1 1 d . . . O3 O -0.09175(12) 0.13754(10) 0.31499(11) 0.0202(3) Uani 1 1 d . . . O4 O 0.07640(12) 0.01672(10) 0.28758(11) 0.0192(3) Uani 1 1 d . . . Cu1 Cu -0.09685(2) 0.451716(18) 0.164128(19) 0.01742(7) Uani 1 1 d . . . Cu2 Cu -0.05711(2) 0.013766(18) 0.379425(19) 0.01604(7) Uani 1 1 d . . . C50 C 0.8399(5) 0.0109(3) 0.1468(4) 0.0458(14) Uani 0.681(7) 1 d PD A 1 H50A H 0.8171 0.0572 0.1810 0.069 Uiso 0.681(7) 1 calc PR A 1 H50B H 0.7814 -0.0032 0.1268 0.069 Uiso 0.681(7) 1 calc PR A 1 H50C H 0.9020 0.0357 0.0904 0.069 Uiso 0.681(7) 1 calc PR A 1 C51 C 0.8694(6) -0.0777(4) 0.2121(5) 0.0323(13) Uani 0.681(7) 1 d PD A 1 H51A H 0.9263 -0.0624 0.2341 0.039 Uiso 0.681(7) 1 calc PR A 1 H51B H 0.8063 -0.1021 0.2690 0.039 Uiso 0.681(7) 1 calc PR A 1 C52 C 0.9077(5) -0.1531(3) 0.1641(4) 0.0361(14) Uani 0.681(7) 1 d PD A 1 H52A H 0.9687 -0.1276 0.1056 0.043 Uiso 0.681(7) 1 calc PR A 1 H52B H 0.8495 -0.1702 0.1445 0.043 Uiso 0.681(7) 1 calc PR A 1 C53 C 0.9420(4) -0.2410(3) 0.2278(4) 0.0356(12) Uani 0.681(7) 1 d PD A 1 H53A H 0.8838 -0.2628 0.2892 0.043 Uiso 0.681(7) 1 calc PR A 1 H53B H 0.9535 -0.2906 0.1966 0.043 Uiso 0.681(7) 1 calc PR A 1 C54 C 1.0434(5) -0.2256(4) 0.2475(5) 0.0440(15) Uani 0.681(7) 1 d PD A 1 H54A H 1.0317 -0.1766 0.2794 0.053 Uiso 0.681(7) 1 calc PR A 1 H54B H 1.1015 -0.2032 0.1861 0.053 Uiso 0.681(7) 1 calc PR A 1 C55 C 1.0779(7) -0.3134(4) 0.3099(6) 0.068(2) Uani 0.681(7) 1 d PD A 1 H55A H 1.1438 -0.2999 0.3198 0.102 Uiso 0.681(7) 1 calc PR A 1 H55B H 1.0903 -0.3621 0.2785 0.102 Uiso 0.681(7) 1 calc PR A 1 H55C H 1.0217 -0.3348 0.3717 0.102 Uiso 0.681(7) 1 calc PR A 1 C56 C 0.8439(5) 0.4929(4) 0.4009(5) 0.0540(17) Uani 0.592(5) 1 d P B 1 H56A H 0.8540 0.5309 0.3347 0.081 Uiso 0.592(5) 1 calc PR B 1 H56B H 0.8693 0.4302 0.4021 0.081 Uiso 0.592(5) 1 calc PR B 1 H56C H 0.8843 0.5215 0.4288 0.081 Uiso 0.592(5) 1 calc PR B 1 C57 C 0.7300(6) 0.4872(5) 0.4562(5) 0.065(2) Uani 0.592(5) 1 d P B 1 H57 H 0.6891 0.4587 0.4271 0.078 Uiso 0.592(5) 1 calc PR B 1 C58 C 0.7026(4) 0.4346(4) 0.5609(4) 0.0513(16) Uani 0.592(5) 1 d P B 1 H58A H 0.7533 0.4517 0.5884 0.062 Uiso 0.592(5) 1 calc PR B 1 H58B H 0.7040 0.3666 0.5713 0.062 Uiso 0.592(5) 1 calc PR B 1 C59 C 0.5898(4) 0.4643(4) 0.6055(4) 0.0493(15) Uani 0.592(5) 1 d P B 1 H59A H 0.5362 0.4281 0.5971 0.059 Uiso 0.592(5) 1 calc PR B 1 H59B H 0.5750 0.4538 0.6746 0.059 Uiso 0.592(5) 1 calc PR B 1 C60 C 0.5857(5) 0.5662(4) 0.5546(4) 0.0511(16) Uani 0.592(5) 1 d P B 1 H60A H 0.5920 0.6048 0.5939 0.061 Uiso 0.592(5) 1 calc PR B 1 H60B H 0.5183 0.5803 0.5392 0.061 Uiso 0.592(5) 1 calc PR B 1 C61 C 0.6805(6) 0.5836(5) 0.4647(5) 0.067(2) Uani 0.592(5) 1 d P B 1 H61A H 0.7346 0.6240 0.4670 0.080 Uiso 0.592(5) 1 calc PR B 1 H61B H 0.6576 0.6157 0.4084 0.080 Uiso 0.592(5) 1 calc PR B 1 C50B C 0.8497(15) -0.0426(12) 0.1909(12) 0.058(5) Uani 0.319(7) 1 d P A 2 H50D H 0.7802 -0.0138 0.2069 0.087 Uiso 0.319(7) 1 calc PR A 2 H50E H 0.8920 -0.0097 0.1251 0.087 Uiso 0.319(7) 1 calc PR A 2 H50F H 0.8875 -0.0387 0.2344 0.087 Uiso 0.319(7) 1 calc PR A 2 C51B C 0.8326(10) -0.1479(10) 0.2008(8) 0.060(4) Uani 0.319(7) 1 d P A 2 H51C H 0.7874 -0.1800 0.2667 0.072 Uiso 0.319(7) 1 calc PR A 2 H51D H 0.7939 -0.1512 0.1570 0.072 Uiso 0.319(7) 1 calc PR A 2 C52B C 0.9345(15) -0.1978(15) 0.1790(12) 0.073(5) Uani 0.319(7) 1 d P A 2 H52C H 0.9841 -0.1593 0.1180 0.087 Uiso 0.319(7) 1 calc PR A 2 H52D H 0.9195 -0.2567 0.1694 0.087 Uiso 0.319(7) 1 calc PR A 2 C53B C 0.9900(12) -0.2205(13) 0.2535(12) 0.075(6) Uani 0.319(7) 1 d P A 2 H53C H 0.9404 -0.2574 0.3154 0.089 Uiso 0.319(7) 1 calc PR A 2 H53D H 1.0093 -0.1619 0.2610 0.089 Uiso 0.319(7) 1 calc PR A 2 C54B C 1.0899(10) -0.2749(11) 0.2275(10) 0.065(4) Uani 0.319(7) 1 d P A 2 H54C H 1.0694 -0.3340 0.2218 0.078 Uiso 0.319(7) 1 calc PR A 2 H54D H 1.1373 -0.2387 0.1640 0.078 Uiso 0.319(7) 1 calc PR A 2 C55B C 1.1520(13) -0.2973(9) 0.2963(11) 0.068(4) Uani 0.319(7) 1 d P A 2 H55D H 1.2143 -0.3329 0.2739 0.103 Uiso 0.319(7) 1 calc PR A 2 H55E H 1.1066 -0.3342 0.3593 0.103 Uiso 0.319(7) 1 calc PR A 2 H55F H 1.1757 -0.2393 0.3007 0.103 Uiso 0.319(7) 1 calc PR A 2 C62 C 0.815(4) 0.512(3) 0.438(3) 0.34(3) Uiso 0.408(5) 1 d PD B 2 H62A H 0.8298 0.5226 0.3693 0.512 Uiso 0.408(5) 1 calc PR B 2 H62B H 0.8311 0.4478 0.4677 0.512 Uiso 0.408(5) 1 calc PR B 2 H62C H 0.8605 0.5549 0.4467 0.512 Uiso 0.408(5) 1 calc PR B 2 C63 C 0.678(2) 0.533(3) 0.491(3) 0.28(2) Uiso 0.408(5) 1 d PD B 2 H63A H 0.6805 0.5258 0.5560 0.336 Uiso 0.408(5) 1 calc PR B 2 H63B H 0.6803 0.6009 0.4612 0.336 Uiso 0.408(5) 1 calc PR B 2 C64 C 0.537(2) 0.514(2) 0.523(2) 0.223(12) Uiso 0.408(5) 1 d PD . 2 H64A H 0.5183 0.4676 0.5873 0.268 Uiso 0.408(5) 1 calc PR B 2 H64B H 0.5073 0.5731 0.5341 0.268 Uiso 0.408(5) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0189(11) 0.0132(11) 0.0251(12) 0.0002(9) -0.0066(10) 0.0013(9) C2 0.0206(11) 0.0138(11) 0.0263(12) -0.0007(9) -0.0079(10) 0.0033(9) C3 0.0191(11) 0.0165(12) 0.0302(13) -0.0026(10) -0.0091(10) 0.0015(9) C4 0.0198(12) 0.0151(11) 0.0317(13) -0.0011(10) -0.0059(10) -0.0011(9) C5 0.0246(12) 0.0127(11) 0.0269(13) 0.0024(10) -0.0056(10) 0.0009(9) C6 0.0184(11) 0.0141(11) 0.0244(12) -0.0014(9) -0.0057(9) 0.0020(9) C7 0.0188(11) 0.0165(12) 0.0298(13) 0.0027(10) -0.0104(10) 0.0014(9) C8 0.0295(14) 0.0245(13) 0.0309(14) 0.0029(11) -0.0111(11) 0.0028(11) C9 0.0292(13) 0.0161(12) 0.0336(14) 0.0033(10) -0.0149(11) 0.0034(10) C10 0.0237(13) 0.0245(13) 0.0386(15) 0.0039(11) -0.0155(11) 0.0001(10) C11 0.0237(13) 0.0180(12) 0.0402(15) 0.0034(11) -0.0093(11) -0.0057(10) C12 0.0210(13) 0.0319(15) 0.0445(17) 0.0026(12) -0.0076(12) -0.0046(11) C13 0.0435(17) 0.0252(15) 0.0520(19) 0.0002(13) -0.0189(15) -0.0132(13) C14 0.0337(15) 0.0191(13) 0.0474(17) 0.0066(12) -0.0104(13) -0.0082(11) C15 0.0190(11) 0.0145(11) 0.0193(11) -0.0035(9) -0.0049(9) 0.0040(9) C16 0.0224(12) 0.0217(13) 0.0331(14) 0.0073(11) -0.0102(11) 0.0011(10) C17 0.0254(12) 0.0153(11) 0.0342(14) -0.0008(10) -0.0177(11) 0.0040(10) C18 0.0209(12) 0.0128(11) 0.0392(14) 0.0004(10) -0.0146(11) 0.0058(9) C19 0.0326(14) 0.0224(14) 0.0493(17) -0.0120(13) -0.0085(13) 0.0096(11) C20 0.0258(14) 0.0227(14) 0.0578(19) 0.0079(13) -0.0229(13) 0.0014(11) C21 0.0152(11) 0.0204(12) 0.0300(13) -0.0037(10) -0.0101(10) 0.0036(9) C22 0.0179(11) 0.0180(11) 0.0220(12) -0.0009(9) -0.0083(9) 0.0017(9) C23 0.0166(11) 0.0166(11) 0.0186(11) -0.0024(9) -0.0065(9) 0.0021(9) C24 0.0158(10) 0.0169(11) 0.0167(11) -0.0031(9) -0.0060(9) 0.0026(9) C25 0.0187(11) 0.0168(11) 0.0187(11) -0.0018(9) -0.0079(9) 0.0022(9) C26 0.0161(11) 0.0215(12) 0.0272(13) 0.0015(10) -0.0093(10) -0.0026(9) C27 0.0163(11) 0.0230(12) 0.0301(13) 0.0000(10) -0.0114(10) 0.0010(9) C28 0.0139(10) 0.0180(11) 0.0194(11) -0.0022(9) -0.0039(9) -0.0011(9) C29 0.0178(11) 0.0129(11) 0.0210(11) 0.0016(9) -0.0068(9) 0.0000(9) C30 0.0341(14) 0.0185(12) 0.0322(14) -0.0016(11) -0.0174(12) -0.0032(10) C31 0.0167(11) 0.0237(13) 0.0266(13) 0.0044(10) -0.0039(10) 0.0020(9) C32 0.0152(11) 0.0210(12) 0.0187(11) -0.0031(9) -0.0046(9) 0.0014(9) C33 0.0185(11) 0.0151(11) 0.0176(11) -0.0042(9) -0.0079(9) 0.0022(9) C34 0.0195(12) 0.0201(12) 0.0264(13) 0.0020(10) -0.0061(10) 0.0039(9) C35 0.0170(11) 0.0143(11) 0.0211(11) -0.0057(9) -0.0062(9) 0.0024(9) C36 0.0218(11) 0.0159(11) 0.0216(12) -0.0043(9) -0.0094(9) 0.0049(9) C37 0.0177(11) 0.0175(11) 0.0288(13) -0.0093(10) -0.0075(10) 0.0065(9) C38 0.0166(11) 0.0159(11) 0.0255(12) -0.0065(9) -0.0019(9) 0.0021(9) C39 0.0181(11) 0.0114(10) 0.0210(11) -0.0035(9) -0.0030(9) 0.0003(8) C40 0.0168(11) 0.0116(10) 0.0230(12) -0.0063(9) -0.0066(9) 0.0015(8) C41 0.0187(12) 0.0269(13) 0.0334(14) -0.0081(11) -0.0081(10) 0.0093(10) C42 0.0447(18) 0.073(2) 0.0433(18) -0.0286(17) -0.0193(15) 0.0411(17) C43 0.0306(17) 0.045(2) 0.140(4) -0.025(2) -0.043(2) 0.0073(15) C44 0.0285(15) 0.079(2) 0.0409(17) -0.0128(17) -0.0174(13) 0.0258(16) C45 0.0193(11) 0.0176(12) 0.0210(12) -0.0002(9) -0.0023(9) 0.0048(9) C46 0.0305(14) 0.0385(16) 0.0214(13) -0.0046(11) -0.0075(11) 0.0017(12) C47 0.0311(14) 0.0164(12) 0.0353(15) 0.0018(11) -0.0044(12) 0.0052(10) C48 0.0276(13) 0.0280(14) 0.0249(13) 0.0027(11) -0.0005(11) 0.0071(11) N1 0.0194(10) 0.0145(9) 0.0237(10) -0.0035(8) -0.0109(8) 0.0057(8) N2 0.0201(10) 0.0146(10) 0.0270(11) -0.0031(8) -0.0109(8) 0.0055(8) N3 0.0162(9) 0.0138(9) 0.0206(10) -0.0020(8) -0.0052(8) 0.0003(7) N4 0.0164(9) 0.0154(9) 0.0173(9) -0.0029(8) -0.0040(7) 0.0005(7) O1 0.0202(8) 0.0147(8) 0.0329(10) 0.0063(7) -0.0111(7) -0.0009(7) O2 0.0147(8) 0.0139(8) 0.0313(9) 0.0001(7) -0.0083(7) 0.0019(6) O3 0.0153(8) 0.0136(8) 0.0266(9) -0.0004(7) -0.0058(7) 0.0030(6) O4 0.0170(8) 0.0156(8) 0.0205(8) -0.0005(6) -0.0056(6) 0.0044(6) Cu1 0.01530(14) 0.01097(14) 0.02342(15) -0.00029(11) -0.00803(11) 0.00295(10) Cu2 0.01317(13) 0.01190(14) 0.01913(14) -0.00087(11) -0.00399(11) 0.00199(10) C50 0.062(3) 0.039(3) 0.038(3) -0.009(2) -0.023(3) 0.017(3) C51 0.037(3) 0.031(3) 0.030(3) -0.008(3) -0.013(2) 0.005(2) C52 0.038(4) 0.041(3) 0.030(3) -0.011(3) -0.013(2) 0.002(2) C53 0.047(3) 0.029(3) 0.037(3) -0.016(2) -0.015(3) 0.004(2) C54 0.048(4) 0.030(3) 0.053(4) -0.010(2) -0.018(3) 0.005(3) C55 0.112(6) 0.036(3) 0.088(5) -0.029(3) -0.071(5) 0.032(4) C56 0.047(3) 0.048(3) 0.053(4) -0.006(3) -0.010(3) 0.020(3) C57 0.051(4) 0.064(4) 0.056(4) 0.002(3) -0.010(3) 0.017(3) C58 0.047(3) 0.034(3) 0.070(4) -0.006(3) -0.024(3) -0.001(2) C59 0.045(3) 0.059(4) 0.050(3) -0.021(3) -0.018(3) -0.005(3) C60 0.081(4) 0.044(3) 0.047(3) -0.015(3) -0.046(3) 0.012(3) C61 0.096(5) 0.053(4) 0.068(4) -0.038(4) -0.036(4) 0.036(4) C50B 0.048(10) 0.071(15) 0.050(11) -0.015(11) -0.010(7) -0.003(10) C51B 0.040(7) 0.093(10) 0.036(6) -0.007(6) -0.006(5) -0.006(6) C52B 0.067(12) 0.100(18) 0.054(11) -0.024(13) -0.018(9) -0.014(12) C53B 0.041(8) 0.110(13) 0.074(10) -0.063(9) 0.021(8) -0.038(9) C54B 0.052(7) 0.069(9) 0.077(10) -0.047(8) 0.000(6) -0.004(7) C55B 0.077(10) 0.055(8) 0.089(10) -0.053(8) -0.018(9) 0.007(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 C1 O1 1.308(3) . ? C1 C6 1.432(3) . ? C1 C2 1.435(3) . ? C2 C3 1.374(3) . ? C2 C7 1.537(3) . ? C3 C4 1.403(3) . ? C3 H3 0.9500 . ? C4 C5 1.363(3) . ? C4 C11 1.534(3) . ? C5 C6 1.417(3) . ? C5 H5 0.9500 . ? C6 C15 1.458(3) . ? C7 C8 1.530(3) . ? C7 C10 1.531(3) . ? C7 C9 1.534(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.529(3) . ? C11 C12 1.532(4) . ? C11 C13 1.534(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N1 1.296(3) . ? C15 C16 1.514(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N1 1.469(3) . ? C17 C18 1.521(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N2 1.484(3) . ? C18 C19 1.521(4) . ? C18 C20 1.527(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N2 1.286(3) . ? C21 C22 1.426(3) . ? C21 H21 0.9500 . ? C22 C23 1.414(3) . ? C22 C27 1.426(3) . ? C23 O2 1.295(3) . ? C23 C24 1.479(3) . ? C24 O3 1.295(3) . ? C24 C25 1.414(3) . ? C25 C26 1.422(3) . ? C25 C28 1.432(3) . ? C26 C27 1.346(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 N3 1.287(3) . ? C28 H28 0.9500 . ? C29 N3 1.487(3) . ? C29 C31 1.525(3) . ? C29 C30 1.526(3) . ? C29 C32 1.526(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N4 1.466(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N4 1.300(3) . ? C33 C35 1.459(3) . ? C33 C34 1.512(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.415(3) . ? C35 C40 1.430(3) . ? C36 C37 1.367(3) . ? C36 H36 0.9500 . ? C37 C38 1.412(3) . ? C37 C41 1.533(3) . ? C38 C39 1.376(3) . ? C38 H38 0.9500 . ? C39 C40 1.436(3) . ? C39 C45 1.537(3) . ? C40 O4 1.308(3) . ? C41 C42 1.510(4) . ? C41 C44 1.519(4) . ? C41 C43 1.525(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.530(4) . ? C45 C48 1.531(3) . ? C45 C47 1.537(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N1 Cu1 1.9571(19) . ? N2 Cu1 1.9211(19) . ? N3 Cu2 1.9195(18) . ? N4 Cu2 1.9485(18) . ? O1 Cu1 1.8566(16) . ? O2 Cu1 1.9287(15) . ? O3 Cu2 1.9303(15) . ? O4 Cu2 1.8726(15) . ? C50 C51 1.522(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.521(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.531(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.518(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.521(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.468(10) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.506(9) . ? C57 C61 1.580(9) . ? C57 H57 1.0000 . ? C58 C59 1.529(8) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.505(8) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.510(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C50B C51B 1.58(2) . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? C51B C52B 1.49(2) . ? C51B H51C 0.9900 . ? C51B H51D 0.9900 . ? C52B C53B 1.51(2) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? C53B C54B 1.51(2) . ? C53B H53C 0.9900 . ? C53B H53D 0.9900 . ? C54B C55B 1.50(2) . ? C54B H54C 0.9900 . ? C54B H54D 0.9900 . ? C55B H55D 0.9800 . ? C55B H55E 0.9800 . ? C55B H55F 0.9800 . ? C62 C63 1.79(2) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.79(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C64 1.53(5) 2_666 ? C64 H64A 0.9900 . ? C64 H64B 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 O1 C1 C6 124.3(2) . . ? O1 C1 C2 117.05(19) . . ? C6 C1 C2 118.7(2) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 C7 121.0(2) . . ? C1 C2 C7 120.2(2) . . ? C2 C3 C4 123.7(2) . . ? C2 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C5 C4 C3 117.1(2) . . ? C5 C4 C11 123.9(2) . . ? C3 C4 C11 119.0(2) . . ? C4 C5 C6 123.5(2) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C1 118.2(2) . . ? C5 C6 C15 119.0(2) . . ? C1 C6 C15 122.8(2) . . ? C8 C7 C10 107.8(2) . . ? C8 C7 C9 110.3(2) . . ? C10 C7 C9 107.05(19) . . ? C8 C7 C2 108.97(19) . . ? C10 C7 C2 111.80(19) . . ? C9 C7 C2 110.9(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 108.4(2) . . ? C14 C11 C4 112.1(2) . . ? C12 C11 C4 108.8(2) . . ? C14 C11 C13 108.5(2) . . ? C12 C11 C13 109.8(2) . . ? C4 C11 C13 109.2(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 121.8(2) . . ? N1 C15 C16 118.8(2) . . ? C6 C15 C16 119.5(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 109.97(19) . . ? N1 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N1 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N2 C18 C19 108.0(2) . . ? N2 C18 C17 105.43(18) . . ? C19 C18 C17 109.9(2) . . ? N2 C18 C20 113.9(2) . . ? C19 C18 C20 111.1(2) . . ? C17 C18 C20 108.3(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 C22 126.8(2) . . ? N2 C21 H21 116.6 . . ? C22 C21 H21 116.6 . . ? C23 C22 C27 121.2(2) . . ? C23 C22 C21 122.5(2) . . ? C27 C22 C21 116.3(2) . . ? O2 C23 C22 124.4(2) . . ? O2 C23 C24 117.57(19) . . ? C22 C23 C24 118.0(2) . . ? O3 C24 C25 124.2(2) . . ? O3 C24 C23 118.35(19) . . ? C25 C24 C23 117.43(19) . . ? C24 C25 C26 121.4(2) . . ? C24 C25 C28 122.2(2) . . ? C26 C25 C28 116.2(2) . . ? C27 C26 C25 120.8(2) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 120.6(2) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? N3 C28 C25 126.5(2) . . ? N3 C28 H28 116.8 . . ? C25 C28 H28 116.8 . . ? N3 C29 C31 112.45(18) . . ? N3 C29 C30 108.46(18) . . ? C31 C29 C30 111.2(2) . . ? N3 C29 C32 105.23(17) . . ? C31 C29 C32 108.90(19) . . ? C30 C29 C32 110.41(18) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 C29 110.91(18) . . ? N4 C32 H32A 109.5 . . ? C29 C32 H32A 109.5 . . ? N4 C32 H32B 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? N4 C33 C35 121.7(2) . . ? N4 C33 C34 119.6(2) . . ? C35 C33 C34 118.65(18) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 118.8(2) . . ? C36 C35 C33 118.5(2) . . ? C40 C35 C33 122.68(19) . . ? C37 C36 C35 123.3(2) . . ? C37 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? C36 C37 C38 116.3(2) . . ? C36 C37 C41 123.6(2) . . ? C38 C37 C41 120.1(2) . . ? C39 C38 C37 123.9(2) . . ? C39 C38 H38 118.0 . . ? C37 C38 H38 118.0 . . ? C38 C39 C40 118.8(2) . . ? C38 C39 C45 121.3(2) . . ? C40 C39 C45 119.88(19) . . ? O4 C40 C35 124.03(19) . . ? O4 C40 C39 118.36(19) . . ? C35 C40 C39 117.60(19) . . ? C42 C41 C44 107.9(2) . . ? C42 C41 C43 110.7(3) . . ? C44 C41 C43 106.5(3) . . ? C42 C41 C37 110.4(2) . . ? C44 C41 C37 112.5(2) . . ? C43 C41 C37 108.9(2) . . ? 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 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C48 107.1(2) . . ? C46 C45 C39 111.56(19) . . ? C48 C45 C39 111.64(19) . . ? C46 C45 C47 109.7(2) . . ? C48 C45 C47 107.5(2) . . ? C39 C45 C47 109.2(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C15 N1 C17 121.01(19) . . ? C15 N1 Cu1 129.21(15) . . ? C17 N1 Cu1 109.63(14) . . ? C21 N2 C18 121.41(19) . . ? C21 N2 Cu1 125.59(15) . . ? C18 N2 Cu1 112.92(15) . . ? C28 N3 C29 120.36(19) . . ? C28 N3 Cu2 124.39(16) . . ? C29 N3 Cu2 114.56(13) . . ? C33 N4 C32 121.62(19) . . ? C33 N4 Cu2 128.24(15) . . ? C32 N4 Cu2 110.03(13) . . ? C1 O1 Cu1 129.80(14) . . ? C23 O2 Cu1 127.31(14) . . ? C24 O3 Cu2 126.75(14) . . ? C40 O4 Cu2 128.67(14) . . ? O1 Cu1 N2 169.35(8) . . ? O1 Cu1 O2 90.98(7) . . ? N2 Cu1 O2 93.28(7) . . ? O1 Cu1 N1 91.89(7) . . ? N2 Cu1 N1 85.62(8) . . ? O2 Cu1 N1 169.79(8) . . ? O4 Cu2 N3 158.64(7) . . ? O4 Cu2 O3 94.24(6) . . ? N3 Cu2 O3 93.26(7) . . ? O4 Cu2 N4 92.60(7) . . ? N3 Cu2 N4 85.38(8) . . ? O3 Cu2 N4 164.22(7) . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C50 113.1(5) . . ? C52 C51 H51A 109.0 . . ? C50 C51 H51A 109.0 . . ? C52 C51 H51B 109.0 . . ? C50 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C51 C52 C53 113.5(4) . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52B 108.9 . . ? C53 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C54 C53 C52 113.0(4) . . ? C54 C53 H53A 109.0 . . ? C52 C53 H53A 109.0 . . ? C54 C53 H53B 109.0 . . ? C52 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 C55 112.8(5) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C56 C57 C58 115.6(6) . . ? C56 C57 C61 114.5(6) . . ? C58 C57 C61 98.8(5) . . ? C56 C57 H57 109.1 . . ? C58 C57 H57 109.1 . . ? C61 C57 H57 109.1 . . ? C57 C58 C59 104.5(5) . . ? C57 C58 H58A 110.9 . . ? C59 C58 H58A 110.9 . . ? C57 C58 H58B 110.9 . . ? C59 C58 H58B 110.9 . . ? H58A C58 H58B 108.9 . . ? C60 C59 C58 106.4(5) . . ? C60 C59 H59A 110.5 . . ? C58 C59 H59A 110.5 . . ? C60 C59 H59B 110.5 . . ? C58 C59 H59B 110.5 . . ? H59A C59 H59B 108.6 . . ? C59 C60 C61 104.0(5) . . ? C59 C60 H60A 111.0 . . ? C61 C60 H60A 111.0 . . ? C59 C60 H60B 111.0 . . ? C61 C60 H60B 111.0 . . ? H60A C60 H60B 109.0 . . ? C60 C61 C57 109.0(6) . . ? C60 C61 H61A 109.9 . . ? C57 C61 H61A 109.9 . . ? C60 C61 H61B 109.9 . . ? C57 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? C51B C50B H50D 109.5 . . ? C51B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C51B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? C52B C51B C50B 113.2(13) . . ? C52B C51B H51C 108.9 . . ? C50B C51B H51C 108.9 . . ? C52B C51B H51D 108.9 . . ? C50B C51B H51D 108.9 . . ? H51C C51B H51D 107.8 . . ? C51B C52B C53B 115.8(14) . . ? C51B C52B H52C 108.3 . . ? C53B C52B H52C 108.3 . . ? C51B C52B H52D 108.3 . . ? C53B C52B H52D 108.3 . . ? H52C C52B H52D 107.4 . . ? C52B C53B C54B 112.2(14) . . ? C52B C53B H53C 109.2 . . ? C54B C53B H53C 109.2 . . ? C52B C53B H53D 109.2 . . ? C54B C53B H53D 109.2 . . ? H53C C53B H53D 107.9 . . ? C55B C54B C53B 115.5(12) . . ? C55B C54B H54C 108.4 . . ? C53B C54B H54C 108.4 . . ? C55B C54B H54D 108.4 . . ? C53B C54B H54D 108.4 . . ? H54C C54B H54D 107.5 . . ? C54B C55B H55D 109.5 . . ? C54B C55B H55E 109.5 . . ? H55D C55B H55E 109.5 . . ? C54B C55B H55F 109.5 . . ? H55D C55B H55F 109.5 . . ? H55E C55B H55F 109.5 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C62 155(3) . . ? C64 C63 H63A 97.7 . . ? C62 C63 H63A 97.7 . . ? C64 C63 H63B 97.7 . . ? C62 C63 H63B 97.7 . . ? H63A C63 H63B 103.7 . . ? C64 C64 C63 135(3) 2_666 . ? C64 C64 H64A 103.4 2_666 . ? C63 C64 H64A 103.4 . . ? C64 C64 H64B 103.5 2_666 . ? C63 C64 H64B 103.5 . . ? H64A C64 H64B 105.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.5(2) . . . . ? C6 C1 C2 C3 -0.9(3) . . . . ? O1 C1 C2 C7 -3.7(3) . . . . ? C6 C1 C2 C7 176.9(2) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? C7 C2 C3 C4 -176.4(2) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C2 C3 C4 C11 178.5(2) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C11 C4 C5 C6 -179.5(2) . . . . ? C4 C5 C6 C1 0.6(4) . . . . ? C4 C5 C6 C15 178.5(2) . . . . ? O1 C1 C6 C5 -179.4(2) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? O1 C1 C6 C15 2.7(4) . . . . ? C2 C1 C6 C15 -177.9(2) . . . . ? C3 C2 C7 C8 115.5(2) . . . . ? C1 C2 C7 C8 -62.3(3) . . . . ? C3 C2 C7 C10 -3.5(3) . . . . ? C1 C2 C7 C10 178.7(2) . . . . ? C3 C2 C7 C9 -122.9(2) . . . . ? C1 C2 C7 C9 59.3(3) . . . . ? C5 C4 C11 C14 4.5(4) . . . . ? C3 C4 C11 C14 -174.9(2) . . . . ? C5 C4 C11 C12 -115.4(3) . . . . ? C3 C4 C11 C12 65.3(3) . . . . ? C5 C4 C11 C13 124.8(3) . . . . ? C3 C4 C11 C13 -54.6(3) . . . . ? C5 C6 C15 N1 -175.9(2) . . . . ? C1 C6 C15 N1 1.9(3) . . . . ? C5 C6 C15 C16 3.6(3) . . . . ? C1 C6 C15 C16 -178.6(2) . . . . ? N1 C17 C18 N2 -43.8(2) . . . . ? N1 C17 C18 C19 72.3(2) . . . . ? N1 C17 C18 C20 -166.1(2) . . . . ? N2 C21 C22 C23 0.2(4) . . . . ? N2 C21 C22 C27 179.5(2) . . . . ? C27 C22 C23 O2 -176.5(2) . . . . ? C21 C22 C23 O2 2.8(4) . . . . ? C27 C22 C23 C24 3.3(3) . . . . ? C21 C22 C23 C24 -177.4(2) . . . . ? O2 C23 C24 O3 -7.3(3) . . . . ? C22 C23 C24 O3 172.9(2) . . . . ? O2 C23 C24 C25 171.6(2) . . . . ? C22 C23 C24 C25 -8.2(3) . . . . ? O3 C24 C25 C26 -173.0(2) . . . . ? C23 C24 C25 C26 8.2(3) . . . . ? O3 C24 C25 C28 12.5(3) . . . . ? C23 C24 C25 C28 -166.3(2) . . . . ? C24 C25 C26 C27 -3.0(4) . . . . ? C28 C25 C26 C27 171.9(2) . . . . ? C25 C26 C27 C22 -2.4(4) . . . . ? C23 C22 C27 C26 2.1(4) . . . . ? C21 C22 C27 C26 -177.2(2) . . . . ? C24 C25 C28 N3 -2.9(4) . . . . ? C26 C25 C28 N3 -177.7(2) . . . . ? N3 C29 C32 N4 -40.0(2) . . . . ? C31 C29 C32 N4 -160.79(18) . . . . ? C30 C29 C32 N4 76.8(2) . . . . ? N4 C33 C35 C36 163.5(2) . . . . ? C34 C33 C35 C36 -20.1(3) . . . . ? N4 C33 C35 C40 -17.4(3) . . . . ? C34 C33 C35 C40 159.1(2) . . . . ? C40 C35 C36 C37 -5.0(3) . . . . ? C33 C35 C36 C37 174.2(2) . . . . ? C35 C36 C37 C38 -4.0(3) . . . . ? C35 C36 C37 C41 175.4(2) . . . . ? C36 C37 C38 C39 5.8(3) . . . . ? C41 C37 C38 C39 -173.7(2) . . . . ? C37 C38 C39 C40 1.7(3) . . . . ? C37 C38 C39 C45 179.4(2) . . . . ? C36 C35 C40 O4 -168.6(2) . . . . ? C33 C35 C40 O4 12.2(3) . . . . ? C36 C35 C40 C39 12.4(3) . . . . ? C33 C35 C40 C39 -166.8(2) . . . . ? C38 C39 C40 O4 170.2(2) . . . . ? C45 C39 C40 O4 -7.5(3) . . . . ? C38 C39 C40 C35 -10.8(3) . . . . ? C45 C39 C40 C35 171.5(2) . . . . ? C36 C37 C41 C42 124.4(3) . . . . ? C38 C37 C41 C42 -56.1(3) . . . . ? C36 C37 C41 C44 3.9(4) . . . . ? C38 C37 C41 C44 -176.6(2) . . . . ? C36 C37 C41 C43 -113.8(3) . . . . ? C38 C37 C41 C43 65.6(3) . . . . ? C38 C39 C45 C46 128.9(2) . . . . ? C40 C39 C45 C46 -53.4(3) . . . . ? C38 C39 C45 C48 9.1(3) . . . . ? C40 C39 C45 C48 -173.2(2) . . . . ? C38 C39 C45 C47 -109.6(2) . . . . ? C40 C39 C45 C47 68.0(3) . . . . ? C6 C15 N1 C17 -179.5(2) . . . . ? C16 C15 N1 C17 1.0(3) . . . . ? C6 C15 N1 Cu1 -4.4(3) . . . . ? C16 C15 N1 Cu1 176.15(17) . . . . ? C18 C17 N1 C15 -149.3(2) . . . . ? C18 C17 N1 Cu1 34.7(2) . . . . ? C22 C21 N2 C18 -178.0(2) . . . . ? C22 C21 N2 Cu1 -1.5(4) . . . . ? C19 C18 N2 C21 93.3(3) . . . . ? C17 C18 N2 C21 -149.3(2) . . . . ? C20 C18 N2 C21 -30.6(3) . . . . ? C19 C18 N2 Cu1 -83.6(2) . . . . ? C17 C18 N2 Cu1 33.8(2) . . . . ? C20 C18 N2 Cu1 152.47(19) . . . . ? C25 C28 N3 C29 176.2(2) . . . . ? C25 C28 N3 Cu2 -13.8(3) . . . . ? C31 C29 N3 C28 -42.4(3) . . . . ? C30 C29 N3 C28 81.0(2) . . . . ? C32 C29 N3 C28 -160.8(2) . . . . ? C31 C29 N3 Cu2 146.71(16) . . . . ? C30 C29 N3 Cu2 -89.87(19) . . . . ? C32 C29 N3 Cu2 28.3(2) . . . . ? C35 C33 N4 C32 -175.7(2) . . . . ? C34 C33 N4 C32 7.9(3) . . . . ? C35 C33 N4 Cu2 8.4(3) . . . . ? C34 C33 N4 Cu2 -167.98(16) . . . . ? C29 C32 N4 C33 -141.8(2) . . . . ? C29 C32 N4 Cu2 34.8(2) . . . . ? C6 C1 O1 Cu1 -4.8(3) . . . . ? C2 C1 O1 Cu1 175.81(16) . . . . ? C22 C23 O2 Cu1 -4.0(3) . . . . ? C24 C23 O2 Cu1 176.14(14) . . . . ? C25 C24 O3 Cu2 -4.1(3) . . . . ? C23 C24 O3 Cu2 174.73(14) . . . . ? C35 C40 O4 Cu2 2.1(3) . . . . ? C39 C40 O4 Cu2 -178.91(15) . . . . ? C1 O1 Cu1 N2 -74.0(5) . . . . ? C1 O1 Cu1 O2 172.5(2) . . . . ? C1 O1 Cu1 N1 2.3(2) . . . . ? C21 N2 Cu1 O1 -112.9(4) . . . . ? C18 N2 Cu1 O1 63.8(5) . . . . ? C21 N2 Cu1 O2 0.4(2) . . . . ? C18 N2 Cu1 O2 177.17(16) . . . . ? C21 N2 Cu1 N1 170.3(2) . . . . ? C18 N2 Cu1 N1 -13.00(16) . . . . ? C23 O2 Cu1 O1 172.51(19) . . . . ? C23 O2 Cu1 N2 2.28(19) . . . . ? C23 O2 Cu1 N1 -81.2(4) . . . . ? C15 N1 Cu1 O1 2.3(2) . . . . ? C17 N1 Cu1 O1 177.97(15) . . . . ? C15 N1 Cu1 N2 172.0(2) . . . . ? C17 N1 Cu1 N2 -12.41(15) . . . . ? C15 N1 Cu1 O2 -103.9(4) . . . . ? C17 N1 Cu1 O2 71.7(4) . . . . ? C40 O4 Cu2 N3 -92.2(3) . . . . ? C40 O4 Cu2 O3 157.53(18) . . . . ? C40 O4 Cu2 N4 -8.24(18) . . . . ? C28 N3 Cu2 O4 -93.8(3) . . . . ? C29 N3 Cu2 O4 76.7(3) . . . . ? C28 N3 Cu2 O3 16.60(19) . . . . ? C29 N3 Cu2 O3 -172.90(15) . . . . ? C28 N3 Cu2 N4 -179.16(19) . . . . ? C29 N3 Cu2 N4 -8.66(15) . . . . ? C24 O3 Cu2 O4 151.75(18) . . . . ? C24 O3 Cu2 N3 -8.24(18) . . . . ? C24 O3 Cu2 N4 -92.8(3) . . . . ? C33 N4 Cu2 O4 2.8(2) . . . . ? C32 N4 Cu2 O4 -173.43(14) . . . . ? C33 N4 Cu2 N3 161.5(2) . . . . ? C32 N4 Cu2 N3 -14.73(14) . . . . ? C33 N4 Cu2 O3 -112.8(3) . . . . ? C32 N4 Cu2 O3 70.9(3) . . . . ? C50 C51 C52 C53 177.6(6) . . . . ? C51 C52 C53 C54 -68.7(7) . . . . ? C52 C53 C54 C55 -179.4(5) . . . . ? C56 C57 C58 C59 163.1(6) . . . . ? C61 C57 C58 C59 40.4(7) . . . . ? C57 C58 C59 C60 -38.3(6) . . . . ? C58 C59 C60 C61 17.4(6) . . . . ? C59 C60 C61 C57 8.5(7) . . . . ? C56 C57 C61 C60 -154.1(6) . . . . ? C58 C57 C61 C60 -30.7(7) . . . . ? C50B C51B C52B C53B 73.3(19) . . . . ? C51B C52B C53B C54B 177.4(13) . . . . ? C52B C53B C54B C55B 177.9(13) . . . . ? C62 C63 C64 C64 -32(10) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.607 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.068