Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name N.W.Alcock G.J.Clarkson P.B.Glover 'L.Geoffrey A' P.Moore ; M.Napitpulu ; data_cupmpc _database_code_depnum_ccdc_archive 'CCDC 246446' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Cu2 N10 O6.50' _chemical_formula_weight 917.94 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 12.2100(2) _cell_length_b 17.9411(2) _cell_length_c 19.74770(10) _cell_angle_alpha 72.5980(10) _cell_angle_beta 81.2180(10) _cell_angle_gamma 88.8730(10) _cell_volume 4078.01(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7361 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 26331 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 29.13 _reflns_number_total 18850 _reflns_number_gt 12814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18850 _refine_ls_number_parameters 1137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.002 _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 0.27078(3) 0.51795(2) 0.274252(17) 0.02305(9) Uani 1 1 d . . . Cu2 Cu 0.83384(3) 1.12564(2) 0.272480(18) 0.02830(9) Uani 1 1 d . . . Cu3 Cu 0.41040(3) 0.68595(2) 0.257201(18) 0.02685(9) Uani 1 1 d . . . Cu4 Cu 0.69726(3) 0.97089(2) 0.255224(19) 0.02876(9) Uani 1 1 d . . . N41 N 0.18731(18) 0.43869(13) 0.36560(12) 0.0254(5) Uani 1 1 d . . . C42 C 0.2212(2) 0.36845(17) 0.40096(16) 0.0315(7) Uani 1 1 d . . . H42A H 0.2909 0.3514 0.3834 0.038 Uiso 1 1 calc R . . C43 C 0.1591(3) 0.31971(18) 0.46194(16) 0.0367(8) Uani 1 1 d . . . H43A H 0.1851 0.2698 0.4854 0.044 Uiso 1 1 calc R . . C44 C 0.0584(3) 0.3449(2) 0.48808(16) 0.0409(8) Uani 1 1 d . . . H44A H 0.0145 0.3130 0.5304 0.049 Uiso 1 1 calc R . . C45 C 0.0227(2) 0.4173(2) 0.45167(16) 0.0386(8) Uani 1 1 d . . . H45A H -0.0463 0.4357 0.4689 0.046 Uiso 1 1 calc R . . C46 C 0.0881(2) 0.46332(17) 0.38954(15) 0.0283(6) Uani 1 1 d . . . C47 C 0.0528(2) 0.54056(19) 0.34516(16) 0.0342(7) Uani 1 1 d . . . H47A H -0.0221 0.5351 0.3335 0.041 Uiso 1 1 calc R . . H47B H 0.0498 0.5789 0.3724 0.041 Uiso 1 1 calc R . . N48 N 0.13164(18) 0.56771(14) 0.27948(12) 0.0286(5) Uani 1 1 d . . . C49 C 0.1066(2) 0.62763(18) 0.22703(16) 0.0332(7) Uani 1 1 d . . . O410 O 0.01772(18) 0.66248(15) 0.22511(14) 0.0608(8) Uani 1 1 d . . . C411 C 0.1990(2) 0.65073(16) 0.16409(16) 0.0291(6) Uani 1 1 d . . . N412 N 0.30070(18) 0.62582(13) 0.17751(12) 0.0248(5) Uani 1 1 d . . . C413 C 0.3857(2) 0.64410(16) 0.12203(15) 0.0256(6) Uani 1 1 d . . . C414 C 0.3701(3) 0.68319(17) 0.05274(15) 0.0328(7) Uani 1 1 d . . . H41A H 0.4299 0.6916 0.0142 0.039 Uiso 1 1 calc R . . C415 C 0.2657(3) 0.70998(18) 0.04022(17) 0.0396(8) Uani 1 1 d . . . H41B H 0.2538 0.7386 -0.0069 0.047 Uiso 1 1 calc R . . C416 C 0.1792(3) 0.69485(18) 0.09674(17) 0.0381(8) Uani 1 1 d . . . H41C H 0.1076 0.7143 0.0895 0.046 Uiso 1 1 calc R . . C417 C 0.5020(2) 0.62781(16) 0.13945(15) 0.0256(6) Uani 1 1 d . . . O418 O 0.57157(16) 0.60543(13) 0.09670(11) 0.0363(5) Uani 1 1 d . . . N419 N 0.51884(18) 0.64399(13) 0.19792(12) 0.0232(5) Uani 1 1 d . . . C420 C 0.6316(2) 0.63262(17) 0.21509(15) 0.0268(6) Uani 1 1 d . . . H42B H 0.6847 0.6634 0.1735 0.032 Uiso 1 1 calc R . . H42C H 0.6498 0.5768 0.2243 0.032 Uiso 1 1 calc R . . C421 C 0.6429(2) 0.65739(15) 0.27974(14) 0.0240(6) Uani 1 1 d . . . N422 N 0.55177(18) 0.68339(13) 0.31181(12) 0.0258(5) Uani 1 1 d . . . C423 C 0.5581(3) 0.70364(17) 0.37139(16) 0.0321(7) Uani 1 1 d . . . H42D H 0.4930 0.7210 0.3946 0.038 Uiso 1 1 calc R . . C424 C 0.6540(3) 0.70047(18) 0.40021(17) 0.0373(7) Uani 1 1 d . . . H42E H 0.6556 0.7157 0.4422 0.045 Uiso 1 1 calc R . . C425 C 0.7489(3) 0.67443(18) 0.36656(16) 0.0359(7) Uani 1 1 d . . . H42F H 0.8167 0.6718 0.3851 0.043 Uiso 1 1 calc R . . C426 C 0.7431(2) 0.65236(17) 0.30560(16) 0.0314(7) Uani 1 1 d . . . H42G H 0.8068 0.6341 0.2819 0.038 Uiso 1 1 calc R . . N11 N 0.8599(2) 1.23226(14) 0.18545(13) 0.0326(6) Uani 1 1 d . . . C12 C 0.9532(3) 1.2583(2) 0.13878(18) 0.0424(8) Uani 1 1 d . . . H12A H 1.0185 1.2293 0.1460 0.051 Uiso 1 1 calc R . . C13 C 0.9586(3) 1.3239(2) 0.0819(2) 0.0531(10) Uani 1 1 d . . . H13A H 1.0256 1.3402 0.0495 0.064 Uiso 1 1 calc R . . C14 C 0.8637(3) 1.3661(2) 0.0727(2) 0.0646(12) Uani 1 1 d . . . H14A H 0.8644 1.4124 0.0336 0.077 Uiso 1 1 calc R . . C15 C 0.7678(3) 1.3410(2) 0.1205(2) 0.0529(10) Uani 1 1 d . . . H15A H 0.7023 1.3702 0.1152 0.063 Uiso 1 1 calc R . . C16 C 0.7680(2) 1.27303(18) 0.17618(16) 0.0325(7) Uani 1 1 d . . . C17 C 0.6652(2) 1.24117(18) 0.22939(17) 0.0364(7) Uani 1 1 d . . . H17A H 0.6403 1.2793 0.2555 0.044 Uiso 1 1 calc R . . H17B H 0.6051 1.2334 0.2035 0.044 Uiso 1 1 calc R . . N18 N 0.68715(19) 1.16736(14) 0.28033(13) 0.0287(5) Uani 1 1 d . . . C19 C 0.6122(2) 1.13792(19) 0.33742(17) 0.0331(7) Uani 1 1 d . . . O110 O 0.52136(17) 1.16789(15) 0.35350(14) 0.0537(7) Uani 1 1 d . . . C111 C 0.6445(2) 1.06385(18) 0.38873(15) 0.0299(7) Uani 1 1 d . . . N112 N 0.70740(19) 1.01467(15) 0.36069(12) 0.0297(6) Uani 1 1 d . . . C113 C 0.7421(2) 0.94994(18) 0.40659(16) 0.0316(7) Uani 1 1 d . . . C114 C 0.7173(3) 0.9333(2) 0.48031(17) 0.0407(8) Uani 1 1 d . . . H11A H 0.7447 0.8879 0.5111 0.049 Uiso 1 1 calc R . . C115 C 0.6524(3) 0.9837(2) 0.50824(18) 0.0474(9) Uani 1 1 d . . . H11B H 0.6339 0.9734 0.5587 0.057 Uiso 1 1 calc R . . C116 C 0.6144(3) 1.0495(2) 0.46198(17) 0.0418(8) Uani 1 1 d . . . H11C H 0.5682 1.0845 0.4802 0.050 Uiso 1 1 calc R . . C117 C 0.8103(3) 0.89520(18) 0.37403(16) 0.0337(7) Uani 1 1 d . . . O118 O 0.8709(2) 0.84794(14) 0.41057(13) 0.0503(6) Uani 1 1 d . . . N119 N 0.79831(19) 0.90296(14) 0.30658(13) 0.0306(6) Uani 1 1 d . . . C120 C 0.8696(2) 0.85678(17) 0.26989(17) 0.0326(7) Uani 1 1 d . . . H12B H 0.8707 0.8025 0.3017 0.039 Uiso 1 1 calc R . . H12C H 0.9463 0.8789 0.2580 0.039 Uiso 1 1 calc R . . C121 C 0.8275(2) 0.85702(16) 0.20230(16) 0.0297(7) Uani 1 1 d . . . N122 N 0.74728(19) 0.90784(13) 0.18310(13) 0.0281(5) Uani 1 1 d . . . C123 C 0.7061(3) 0.91044(18) 0.12288(17) 0.0356(7) Uani 1 1 d . . . H12D H 0.6500 0.9467 0.1089 0.043 Uiso 1 1 calc R . . C124 C 0.7410(3) 0.86340(19) 0.08084(18) 0.0403(8) Uani 1 1 d . . . H12E H 0.7095 0.8667 0.0389 0.048 Uiso 1 1 calc R . . C125 C 0.8236(3) 0.81077(19) 0.10114(18) 0.0412(8) Uani 1 1 d . . . H12F H 0.8493 0.7771 0.0733 0.049 Uiso 1 1 calc R . . C126 C 0.8682(3) 0.80779(18) 0.16210(17) 0.0365(7) Uani 1 1 d . . . H12G H 0.9256 0.7728 0.1763 0.044 Uiso 1 1 calc R . . N21 N 0.53023(18) 0.94202(13) 0.31195(12) 0.0253(5) Uani 1 1 d . . . C22 C 0.4949(2) 0.88418(17) 0.37257(16) 0.0314(7) Uani 1 1 d . . . H22A H 0.5486 0.8527 0.3971 0.038 Uiso 1 1 calc R . . C23 C 0.3856(3) 0.86867(19) 0.40049(17) 0.0388(8) Uani 1 1 d . . . H23A H 0.3639 0.8269 0.4431 0.047 Uiso 1 1 calc R . . C24 C 0.3070(3) 0.9150(2) 0.36560(17) 0.0392(8) Uani 1 1 d . . . H24A H 0.2303 0.9054 0.3840 0.047 Uiso 1 1 calc R . . C25 C 0.3411(2) 0.97530(18) 0.30370(16) 0.0326(7) Uani 1 1 d . . . H25A H 0.2885 1.0078 0.2790 0.039 Uiso 1 1 calc R . . C26 C 0.4545(2) 0.98743(16) 0.27830(14) 0.0247(6) Uani 1 1 d . . . C27 C 0.4967(2) 1.05258(17) 0.21210(15) 0.0307(7) Uani 1 1 d . . . H27A H 0.4615 1.0480 0.1715 0.037 Uiso 1 1 calc R . . H27B H 0.4764 1.1033 0.2201 0.037 Uiso 1 1 calc R . . N28 N 0.61700(18) 1.05022(13) 0.19404(12) 0.0273(5) Uani 1 1 d . . . C29 C 0.6633(2) 1.09997(17) 0.13344(16) 0.0325(7) Uani 1 1 d . . . O210 O 0.61605(18) 1.14942(14) 0.08885(12) 0.0497(7) Uani 1 1 d . . . C211 C 0.7875(2) 1.09243(17) 0.11614(16) 0.0317(7) Uani 1 1 d . . . N212 N 0.84515(19) 1.07396(14) 0.17167(13) 0.0318(6) Uani 1 1 d . . . C213 C 0.9542(2) 1.06069(17) 0.15833(17) 0.0330(7) Uani 1 1 d . . . C214 C 1.0069(3) 1.0633(2) 0.09057(19) 0.0433(8) Uani 1 1 d . . . H21A H 1.0831 1.0511 0.0832 0.052 Uiso 1 1 calc R . . C215 C 0.9477(3) 1.0837(2) 0.03368(19) 0.0462(9) Uani 1 1 d . . . H21B H 0.9830 1.0868 -0.0134 0.055 Uiso 1 1 calc R . . C216 C 0.8361(3) 1.09975(18) 0.04628(17) 0.0380(8) Uani 1 1 d . . . H21C H 0.7941 1.1154 0.0079 0.046 Uiso 1 1 calc R . . C217 C 1.0166(2) 1.04456(18) 0.22120(18) 0.0368(7) Uani 1 1 d . . . O218 O 1.10596(19) 1.00963(16) 0.21925(15) 0.0630(8) Uani 1 1 d . . . N219 N 0.96876(19) 1.07076(15) 0.27346(13) 0.0332(6) Uani 1 1 d . . . C220 C 1.0221(3) 1.05511(19) 0.33735(18) 0.0391(8) Uani 1 1 d . . . H22B H 1.1020 1.0695 0.3231 0.047 Uiso 1 1 calc R . . H22C H 1.0151 0.9987 0.3639 0.047 Uiso 1 1 calc R . . C221 C 0.9694(2) 1.10105(17) 0.38460(16) 0.0323(7) Uani 1 1 d . . . N222 N 0.87988(19) 1.14171(14) 0.36458(13) 0.0284(5) Uani 1 1 d . . . C223 C 0.8327(2) 1.18720(19) 0.40322(16) 0.0348(7) Uani 1 1 d . . . H22D H 0.7697 1.2159 0.3887 0.042 Uiso 1 1 calc R . . C224 C 0.8715(3) 1.1941(2) 0.46306(17) 0.0415(8) Uani 1 1 d . . . H22E H 0.8368 1.2274 0.4888 0.050 Uiso 1 1 calc R . . C225 C 0.9613(3) 1.1518(2) 0.48455(18) 0.0488(10) Uani 1 1 d . . . H22F H 0.9892 1.1550 0.5260 0.059 Uiso 1 1 calc R . . C226 C 1.0108(3) 1.1047(2) 0.44606(19) 0.0452(9) Uani 1 1 d . . . H22G H 1.0726 1.0747 0.4609 0.054 Uiso 1 1 calc R . . N31 N 0.38667(19) 0.79154(14) 0.18054(13) 0.0292(5) Uani 1 1 d . . . C32 C 0.4500(2) 0.82511(18) 0.11672(17) 0.0345(7) Uani 1 1 d . . . H32A H 0.5106 0.7970 0.1013 0.041 Uiso 1 1 calc R . . C33 C 0.4311(3) 0.89791(19) 0.07293(19) 0.0432(8) Uani 1 1 d . . . H33A H 0.4772 0.9195 0.0281 0.052 Uiso 1 1 calc R . . C34 C 0.3439(3) 0.9391(2) 0.0954(2) 0.0497(9) Uani 1 1 d . . . H34A H 0.3304 0.9904 0.0669 0.060 Uiso 1 1 calc R . . C35 C 0.2764(3) 0.9049(2) 0.15984(19) 0.0447(9) Uani 1 1 d . . . H35A H 0.2144 0.9317 0.1753 0.054 Uiso 1 1 calc R . . C36 C 0.2998(2) 0.83088(18) 0.20205(17) 0.0325(7) Uani 1 1 d . . . C37 C 0.2309(2) 0.79072(18) 0.27196(17) 0.0368(7) Uani 1 1 d . . . H37A H 0.2188 0.8266 0.3018 0.044 Uiso 1 1 calc R . . H37B H 0.1577 0.7755 0.2637 0.044 Uiso 1 1 calc R . . N38 N 0.28660(19) 0.72131(14) 0.30941(13) 0.0304(6) Uani 1 1 d . . . C39 C 0.2454(2) 0.68610(19) 0.37685(17) 0.0347(7) Uani 1 1 d . . . O310 O 0.16807(19) 0.70925(14) 0.41438(12) 0.0504(6) Uani 1 1 d . . . C311 C 0.2997(2) 0.61050(18) 0.40912(15) 0.0307(7) Uani 1 1 d . . . N312 N 0.35604(18) 0.57620(14) 0.36315(12) 0.0258(5) Uani 1 1 d . . . C313 C 0.4066(2) 0.50861(17) 0.39025(15) 0.0280(6) Uani 1 1 d . . . C314 C 0.4021(3) 0.4745(2) 0.46359(16) 0.0372(7) Uani 1 1 d . . . H31A H 0.4392 0.4273 0.4815 0.045 Uiso 1 1 calc R . . C315 C 0.3430(3) 0.5099(2) 0.51043(17) 0.0434(8) Uani 1 1 d . . . H31B H 0.3385 0.4870 0.5608 0.052 Uiso 1 1 calc R . . C316 C 0.2912(3) 0.5783(2) 0.48347(16) 0.0389(8) Uani 1 1 d . . . H31C H 0.2500 0.6034 0.5148 0.047 Uiso 1 1 calc R . . C317 C 0.4651(2) 0.46845(17) 0.33867(15) 0.0274(6) Uani 1 1 d . . . O318 O 0.55030(17) 0.43064(14) 0.35450(12) 0.0447(6) Uani 1 1 d . . . N319 N 0.41726(18) 0.47487(13) 0.28195(11) 0.0233(5) Uani 1 1 d . . . C320 C 0.4689(2) 0.43546(17) 0.23094(15) 0.0281(6) Uani 1 1 d . . . H32B H 0.4803 0.3801 0.2568 0.034 Uiso 1 1 calc R . . H32C H 0.5423 0.4603 0.2079 0.034 Uiso 1 1 calc R . . C321 C 0.3975(2) 0.43953(16) 0.17417(15) 0.0270(6) Uani 1 1 d . . . N322 N 0.2925(2) 0.45916(14) 0.18770(12) 0.0296(5) Uani 1 1 d . . . C323 C 0.2263(3) 0.4623(2) 0.13833(17) 0.0404(8) Uani 1 1 d . . . H32D H 0.1511 0.4755 0.1482 0.048 Uiso 1 1 calc R . . C324 C 0.2620(3) 0.4473(2) 0.07433(18) 0.0470(9) Uani 1 1 d . . . H32E H 0.2127 0.4499 0.0409 0.056 Uiso 1 1 calc R . . C325 C 0.3709(3) 0.4284(2) 0.06005(19) 0.0527(10) Uani 1 1 d . . . H32F H 0.3988 0.4183 0.0161 0.063 Uiso 1 1 calc R . . C326 C 0.4390(3) 0.4243(2) 0.11079(18) 0.0456(9) Uani 1 1 d . . . H32G H 0.5145 0.4111 0.1020 0.055 Uiso 1 1 calc R . . O1 O 0.5146(4) 1.2676(2) 0.44709(18) 0.1157(14) Uani 1 1 d . . . O01 O 1.2964(5) 1.1561(4) 0.3307(4) 0.107(3) Uani 0.587(9) 1 d P A 1 C02 C 1.2833(5) 1.2182(5) 0.2930(4) 0.099(2) Uani 0.587(9) 1 d P A 1 H02A H 1.3313 1.2218 0.2469 0.119 Uiso 0.587(9) 1 calc PR A 1 H02B H 1.3165 1.2549 0.3135 0.119 Uiso 0.587(9) 1 calc PR A 1 C03 C 1.1787(3) 1.2525(2) 0.2735(3) 0.0724(13) Uani 1 1 d . . . H03I H 1.1931 1.3056 0.2406 0.109 Uiso 1 1 calc R A 1 H03J H 1.1292 1.2545 0.3169 0.109 Uiso 1 1 calc R A 1 H03K H 1.1437 1.2205 0.2498 0.109 Uiso 1 1 calc R A 1 C04 C 1.2833(5) 1.2182(5) 0.2930(4) 0.099(2) Uani 0.413(9) 1 d P A 2 H04A H 1.2632 1.1807 0.3415 0.119 Uiso 0.413(9) 1 calc PR A 2 H04B H 1.3053 1.1861 0.2605 0.119 Uiso 0.413(9) 1 calc PR A 2 O05 O 1.3659(6) 1.2496(4) 0.2952(5) 0.097(4) Uani 0.413(9) 1 d P A 2 O011 O 0.2432(6) 0.4727(5) -0.1088(4) 0.049(3) Uani 0.333(7) 1 d P B 1 C012 C 0.1548(7) 0.4356(5) -0.1097(5) 0.171(4) Uani 0.333(7) 1 d P B 1 H01A H 0.1527 0.4577 -0.1618 0.205 Uiso 0.333(7) 1 calc PR B 1 H01E H 0.1019 0.4677 -0.0880 0.205 Uiso 0.333(7) 1 calc PR B 1 C013 C 0.0785(15) 0.3692(11) -0.0972(10) 0.100(6) Uiso 0.333(7) 1 d P B 1 H01B H 0.0019 0.3865 -0.0922 0.150 Uiso 0.333(7) 1 calc PR B 1 H01C H 0.0900 0.3286 -0.0531 0.150 Uiso 0.333(7) 1 calc PR B 1 H01D H 0.0926 0.3479 -0.1379 0.150 Uiso 0.333(7) 1 calc PR B 1 O014 O 0.1951(4) 0.3807(4) -0.0584(2) 0.081(2) Uani 0.667(7) 1 d P B 2 H01F H 0.2626 0.3753 -0.0717 0.121 Uiso 0.667(7) 1 calc PR B 2 C015 C 0.1548(7) 0.4356(5) -0.1097(5) 0.171(4) Uani 0.667(7) 1 d P B 2 H01G H 0.1708 0.4201 -0.1542 0.205 Uiso 0.667(7) 1 calc PR B 2 H01K H 0.1984 0.4844 -0.1182 0.205 Uiso 0.667(7) 1 calc PR B 2 C016 C 0.0411(6) 0.4546(5) -0.1013(5) 0.104(4) Uani 0.667(7) 1 d P B 2 H01H H 0.0180 0.4752 -0.1487 0.156 Uiso 0.667(7) 1 calc PR B 2 H01I H 0.0302 0.4941 -0.0759 0.156 Uiso 0.667(7) 1 calc PR B 2 H01J H -0.0036 0.4076 -0.0735 0.156 Uiso 0.667(7) 1 calc PR B 2 C023 C -0.0713(3) 0.3832(3) 0.2794(3) 0.0759(14) Uani 1 1 d . . . H02C H -0.0131 0.4034 0.2989 0.114 Uiso 1 1 calc R C 1 H02D H -0.0567 0.4021 0.2269 0.114 Uiso 1 1 calc R C 1 H02E H -0.0720 0.3260 0.2955 0.114 Uiso 1 1 calc R C 1 C022 C -0.1810(4) 0.4110(3) 0.3055(3) 0.0806(15) Uani 0.699(9) 1 d P D 1 H02F H -0.1919 0.3933 0.3586 0.097 Uiso 0.699(9) 1 calc PR D 1 H02G H -0.1770 0.4689 0.2901 0.097 Uiso 0.699(9) 1 calc PR D 1 O021 O -0.2652(4) 0.3908(4) 0.2863(4) 0.151(4) Uani 0.699(9) 1 d P D 1 C024 C -0.1810(4) 0.4110(3) 0.3055(3) 0.0806(15) Uani 0.301(9) 1 d P D 2 H02H H -0.2202 0.4226 0.2633 0.097 Uiso 0.301(9) 1 calc PR D 2 H02I H -0.2183 0.3632 0.3400 0.097 Uiso 0.301(9) 1 calc PR D 2 O025 O -0.2092(8) 0.4593(6) 0.3312(6) 0.084(5) Uani 0.301(9) 1 d P D 2 C033 C 0.7524(4) 0.7790(5) -0.0798(4) 0.155(3) Uani 1 1 d . . . H03A H 0.7836 0.8081 -0.0520 0.233 Uiso 1 1 calc R E 1 H03B H 0.7908 0.7954 -0.1294 0.233 Uiso 1 1 calc R E 1 H03C H 0.7619 0.7229 -0.0584 0.233 Uiso 1 1 calc R E 1 C032 C 0.6453(4) 0.7933(4) -0.0791(3) 0.0948(18) Uani 0.877(5) 1 d P F 1 H03F H 0.6043 0.7433 -0.0536 0.114 Uiso 0.877(5) 1 calc PR F 1 H03H H 0.6318 0.8078 -0.1296 0.114 Uiso 0.877(5) 1 calc PR F 1 O031 O 0.5972(2) 0.84808(18) -0.05031(14) 0.0575(10) Uani 0.877(5) 1 d P F 1 H03G H 0.5295 0.8498 -0.0537 0.086 Uiso 0.877(5) 1 calc PR F 1 C035 C 0.6453(4) 0.7933(4) -0.0791(3) 0.0948(18) Uani 0.123(5) 1 d P F 2 H03D H 0.6197 0.7823 -0.0270 0.114 Uiso 0.123(5) 1 calc PR F 2 H03E H 0.6477 0.8510 -0.0982 0.114 Uiso 0.123(5) 1 calc PR F 2 O034 O 0.5660(11) 0.7786(7) -0.0977(7) 0.016(4) Uani 0.123(5) 1 d P F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01883(17) 0.02923(19) 0.01882(17) -0.00469(13) -0.00158(12) 0.00468(14) Cu2 0.02339(18) 0.0344(2) 0.02613(19) -0.00706(15) -0.00621(14) 0.01036(15) Cu3 0.02398(18) 0.0332(2) 0.02587(19) -0.01389(15) -0.00210(14) 0.00709(15) Cu4 0.02494(19) 0.0304(2) 0.02621(19) -0.00164(15) -0.00411(14) 0.00736(15) N41 0.0218(12) 0.0294(13) 0.0237(12) -0.0064(10) -0.0022(9) -0.0025(10) C42 0.0266(16) 0.0314(16) 0.0343(17) -0.0052(13) -0.0075(12) -0.0017(13) C43 0.0396(18) 0.0340(17) 0.0302(17) 0.0026(13) -0.0093(14) -0.0093(14) C44 0.045(2) 0.050(2) 0.0214(16) -0.0005(14) -0.0021(14) -0.0206(16) C45 0.0256(16) 0.057(2) 0.0314(17) -0.0142(15) 0.0044(13) -0.0058(15) C46 0.0223(15) 0.0390(17) 0.0241(15) -0.0114(13) -0.0013(11) -0.0020(12) C47 0.0204(15) 0.0460(19) 0.0327(17) -0.0102(14) 0.0025(12) 0.0046(13) N48 0.0214(12) 0.0337(14) 0.0273(13) -0.0058(10) -0.0009(10) 0.0064(10) C49 0.0283(16) 0.0332(17) 0.0360(17) -0.0065(13) -0.0080(13) 0.0099(13) O410 0.0328(13) 0.0634(17) 0.0636(17) 0.0087(13) 0.0019(11) 0.0264(12) C411 0.0263(15) 0.0248(15) 0.0339(16) -0.0051(12) -0.0054(12) 0.0033(12) N412 0.0259(12) 0.0259(12) 0.0227(12) -0.0073(10) -0.0047(9) 0.0061(10) C413 0.0313(16) 0.0228(14) 0.0244(15) -0.0097(11) -0.0045(12) 0.0030(12) C414 0.0359(17) 0.0349(17) 0.0235(15) -0.0033(13) -0.0033(12) -0.0039(14) C415 0.0441(19) 0.0354(18) 0.0324(18) 0.0048(14) -0.0154(14) 0.0005(15) C416 0.0313(17) 0.0349(18) 0.0396(19) 0.0051(14) -0.0127(14) 0.0031(14) C417 0.0266(15) 0.0243(15) 0.0239(15) -0.0059(11) -0.0003(11) 0.0006(12) O418 0.0314(12) 0.0545(14) 0.0286(11) -0.0227(10) -0.0018(9) 0.0093(10) N419 0.0221(12) 0.0265(12) 0.0219(12) -0.0094(10) -0.0025(9) 0.0035(10) C420 0.0194(14) 0.0341(16) 0.0270(15) -0.0108(12) -0.0014(11) 0.0047(12) C421 0.0229(14) 0.0214(14) 0.0243(14) -0.0037(11) 0.0006(11) -0.0017(11) N422 0.0244(12) 0.0285(13) 0.0245(12) -0.0089(10) -0.0014(9) 0.0017(10) C423 0.0359(17) 0.0313(17) 0.0299(16) -0.0117(13) -0.0024(13) -0.0001(13) C424 0.049(2) 0.0366(18) 0.0281(17) -0.0100(13) -0.0124(14) 0.0017(15) C425 0.0336(17) 0.0399(18) 0.0331(17) -0.0042(14) -0.0153(13) -0.0011(14) C426 0.0262(15) 0.0340(17) 0.0311(16) -0.0048(13) -0.0053(12) 0.0031(13) N11 0.0304(14) 0.0346(14) 0.0316(14) -0.0073(11) -0.0074(11) 0.0066(11) C12 0.0354(18) 0.048(2) 0.0398(19) -0.0077(16) -0.0059(14) 0.0069(16) C13 0.050(2) 0.051(2) 0.047(2) 0.0009(18) -0.0019(17) -0.0050(18) C14 0.067(3) 0.051(2) 0.058(3) 0.014(2) -0.016(2) 0.002(2) C15 0.046(2) 0.044(2) 0.058(2) 0.0044(18) -0.0175(18) 0.0141(17) C16 0.0311(16) 0.0330(17) 0.0358(17) -0.0094(13) -0.0153(13) 0.0059(13) C17 0.0285(16) 0.0390(18) 0.0430(19) -0.0110(15) -0.0138(13) 0.0137(14) N18 0.0242(13) 0.0329(14) 0.0297(13) -0.0086(11) -0.0083(10) 0.0069(10) C19 0.0214(15) 0.0453(19) 0.0371(18) -0.0178(14) -0.0070(12) 0.0023(13) O110 0.0234(12) 0.0668(17) 0.0657(17) -0.0171(14) 0.0026(11) 0.0114(11) C111 0.0203(14) 0.0424(18) 0.0282(16) -0.0123(13) -0.0030(11) -0.0045(13) N112 0.0248(13) 0.0394(15) 0.0229(13) -0.0051(11) -0.0057(10) -0.0028(11) C113 0.0280(16) 0.0353(17) 0.0289(16) -0.0020(13) -0.0113(12) -0.0060(13) C114 0.044(2) 0.045(2) 0.0279(17) -0.0004(14) -0.0109(14) -0.0092(16) C115 0.050(2) 0.064(2) 0.0250(17) -0.0089(16) -0.0043(15) -0.0131(19) C116 0.0383(19) 0.055(2) 0.0329(18) -0.0184(16) 0.0029(14) -0.0080(16) C117 0.0338(17) 0.0318(17) 0.0328(17) -0.0012(13) -0.0136(13) -0.0042(13) O118 0.0579(16) 0.0468(14) 0.0472(15) -0.0043(11) -0.0323(12) 0.0155(12) N119 0.0297(13) 0.0285(13) 0.0309(14) -0.0031(11) -0.0087(10) 0.0049(11) C120 0.0284(16) 0.0247(15) 0.0418(18) -0.0029(13) -0.0115(13) 0.0066(13) C121 0.0230(15) 0.0243(15) 0.0371(17) -0.0031(12) -0.0032(12) 0.0003(12) N122 0.0240(12) 0.0245(13) 0.0338(14) -0.0048(10) -0.0067(10) 0.0048(10) C123 0.0339(17) 0.0351(18) 0.0368(18) -0.0060(14) -0.0123(14) 0.0058(14) C124 0.043(2) 0.042(2) 0.0361(18) -0.0107(15) -0.0089(14) -0.0014(16) C125 0.045(2) 0.0387(19) 0.0393(19) -0.0157(15) 0.0042(15) 0.0001(15) C126 0.0328(17) 0.0310(17) 0.0411(19) -0.0060(14) -0.0021(14) 0.0074(14) N21 0.0243(12) 0.0262(13) 0.0241(12) -0.0045(10) -0.0056(9) 0.0010(10) C22 0.0375(18) 0.0272(16) 0.0287(16) -0.0061(12) -0.0078(13) 0.0016(13) C23 0.045(2) 0.0359(18) 0.0308(17) -0.0076(14) 0.0054(14) -0.0060(15) C24 0.0271(17) 0.050(2) 0.0404(19) -0.0189(16) 0.0052(14) -0.0036(15) C25 0.0213(15) 0.0433(18) 0.0351(17) -0.0147(14) -0.0041(12) 0.0017(13) C26 0.0232(14) 0.0286(15) 0.0248(15) -0.0110(12) -0.0062(11) 0.0034(12) C27 0.0213(14) 0.0368(17) 0.0305(16) -0.0036(13) -0.0072(12) 0.0066(12) N28 0.0229(12) 0.0284(13) 0.0255(13) -0.0012(10) -0.0027(9) 0.0041(10) C29 0.0325(17) 0.0302(16) 0.0300(16) -0.0016(13) -0.0055(13) 0.0055(13) O210 0.0364(13) 0.0505(14) 0.0421(14) 0.0155(11) -0.0056(10) 0.0080(11) C211 0.0325(16) 0.0243(15) 0.0304(16) 0.0001(12) 0.0021(13) 0.0021(13) N212 0.0264(13) 0.0306(14) 0.0314(14) -0.0025(11) 0.0023(10) 0.0066(11) C213 0.0280(16) 0.0285(16) 0.0409(18) -0.0127(13) 0.0041(13) 0.0041(13) C214 0.0296(17) 0.046(2) 0.054(2) -0.0217(17) 0.0078(15) 0.0008(15) C215 0.044(2) 0.052(2) 0.039(2) -0.0173(17) 0.0114(16) -0.0032(17) C216 0.0397(19) 0.0349(18) 0.0327(17) -0.0043(14) 0.0034(14) -0.0024(14) C217 0.0264(16) 0.0352(18) 0.051(2) -0.0156(15) -0.0058(14) 0.0068(14) O218 0.0392(14) 0.084(2) 0.082(2) -0.0476(16) -0.0175(13) 0.0350(14) N219 0.0260(13) 0.0350(14) 0.0356(15) -0.0065(11) -0.0048(11) 0.0101(11) C220 0.0256(16) 0.0394(19) 0.051(2) -0.0071(15) -0.0155(14) 0.0078(14) C221 0.0255(15) 0.0317(17) 0.0351(17) 0.0006(13) -0.0115(13) -0.0043(13) N222 0.0227(12) 0.0319(14) 0.0293(13) -0.0049(11) -0.0084(10) -0.0011(10) C223 0.0289(16) 0.0409(18) 0.0361(18) -0.0147(14) -0.0029(13) -0.0028(14) C224 0.043(2) 0.049(2) 0.0330(18) -0.0136(15) -0.0004(15) -0.0160(16) C225 0.055(2) 0.059(2) 0.0300(18) -0.0033(17) -0.0158(16) -0.0222(19) C226 0.0391(19) 0.048(2) 0.044(2) 0.0028(16) -0.0239(16) -0.0057(16) N31 0.0266(13) 0.0269(13) 0.0360(14) -0.0127(11) -0.0043(10) 0.0023(10) C32 0.0311(17) 0.0333(17) 0.0381(18) -0.0120(14) 0.0007(13) 0.0003(13) C33 0.049(2) 0.0354(19) 0.041(2) -0.0082(15) -0.0026(15) 0.0026(16) C34 0.060(2) 0.0358(19) 0.051(2) -0.0073(16) -0.0120(18) 0.0134(17) C35 0.043(2) 0.0399(19) 0.056(2) -0.0199(17) -0.0114(16) 0.0172(16) C36 0.0282(16) 0.0339(17) 0.0403(18) -0.0182(14) -0.0061(13) 0.0071(13) C37 0.0290(17) 0.0399(18) 0.047(2) -0.0233(15) -0.0021(14) 0.0103(14) N38 0.0276(13) 0.0353(14) 0.0285(13) -0.0132(11) 0.0018(10) 0.0043(11) C39 0.0284(16) 0.0426(19) 0.0368(18) -0.0212(15) 0.0033(13) -0.0050(14) O310 0.0428(14) 0.0612(16) 0.0435(14) -0.0224(12) 0.0174(11) 0.0075(12) C311 0.0238(15) 0.0427(18) 0.0264(15) -0.0152(13) 0.0046(12) -0.0071(13) N312 0.0201(12) 0.0350(14) 0.0228(12) -0.0107(10) -0.0005(9) -0.0041(10) C313 0.0204(14) 0.0396(17) 0.0244(15) -0.0100(13) -0.0037(11) -0.0060(12) C314 0.0363(18) 0.0451(19) 0.0276(16) -0.0055(14) -0.0073(13) -0.0028(15) C315 0.047(2) 0.060(2) 0.0205(16) -0.0091(15) -0.0024(14) -0.0114(18) C316 0.0356(18) 0.054(2) 0.0288(17) -0.0185(15) 0.0050(13) -0.0107(16) C317 0.0240(15) 0.0299(16) 0.0251(15) -0.0029(12) -0.0048(11) -0.0002(12) O318 0.0330(12) 0.0619(16) 0.0434(14) -0.0165(11) -0.0198(10) 0.0180(11) N319 0.0226(12) 0.0260(12) 0.0203(12) -0.0063(9) -0.0018(9) 0.0030(10) C320 0.0248(15) 0.0326(16) 0.0282(15) -0.0120(12) -0.0028(11) 0.0089(12) C321 0.0305(16) 0.0243(15) 0.0261(15) -0.0086(12) -0.0023(12) 0.0037(12) N322 0.0306(13) 0.0327(14) 0.0259(13) -0.0101(10) -0.0037(10) 0.0032(11) C323 0.0379(19) 0.051(2) 0.0360(19) -0.0153(15) -0.0133(14) 0.0053(16) C324 0.057(2) 0.055(2) 0.038(2) -0.0209(17) -0.0217(16) 0.0083(18) C325 0.068(3) 0.066(3) 0.034(2) -0.0297(18) -0.0086(17) 0.014(2) C326 0.044(2) 0.063(2) 0.0370(19) -0.0270(17) -0.0063(15) 0.0185(18) O1 0.200(4) 0.082(2) 0.058(2) -0.0194(18) -0.007(2) 0.044(3) O01 0.075(4) 0.093(5) 0.118(6) 0.026(4) -0.033(3) 0.037(4) C02 0.063(4) 0.138(6) 0.130(5) -0.081(5) -0.044(3) 0.039(4) C03 0.060(3) 0.062(3) 0.089(3) -0.004(2) -0.030(2) 0.007(2) C04 0.063(4) 0.138(6) 0.130(5) -0.081(5) -0.044(3) 0.039(4) O05 0.041(5) 0.040(4) 0.189(10) 0.008(5) -0.039(5) -0.007(3) O011 0.022(4) 0.068(6) 0.067(5) -0.034(4) -0.011(3) 0.005(4) C012 0.147(8) 0.132(7) 0.179(9) -0.019(6) 0.078(7) 0.053(7) O014 0.051(3) 0.148(5) 0.044(3) -0.031(3) -0.010(2) 0.024(3) C015 0.147(8) 0.132(7) 0.179(9) -0.019(6) 0.078(7) 0.053(7) C016 0.047(4) 0.102(6) 0.127(7) 0.024(5) -0.021(4) 0.010(4) C023 0.044(2) 0.092(4) 0.102(4) -0.049(3) -0.003(2) 0.005(2) C022 0.047(3) 0.098(4) 0.090(4) -0.024(3) 0.000(2) 0.004(3) O021 0.032(3) 0.266(8) 0.254(8) -0.226(7) -0.024(3) 0.021(4) C024 0.047(3) 0.098(4) 0.090(4) -0.024(3) 0.000(2) 0.004(3) O025 0.074(7) 0.068(7) 0.116(10) -0.056(7) 0.021(6) 0.027(5) C033 0.056(3) 0.240(8) 0.260(9) -0.206(8) -0.036(4) 0.042(4) C032 0.061(3) 0.137(5) 0.091(4) -0.034(4) -0.031(3) 0.029(3) O031 0.0588(19) 0.085(2) 0.0396(17) -0.0314(15) -0.0202(13) 0.0477(17) C035 0.061(3) 0.137(5) 0.091(4) -0.034(4) -0.031(3) 0.029(3) O034 0.018(8) 0.010(7) 0.018(8) 0.004(5) -0.015(6) -0.008(5) _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 N48 1.907(2) . ? Cu1 N319 1.944(2) . ? Cu1 N41 2.068(2) . ? Cu1 N322 2.243(2) . ? Cu1 N412 2.265(2) . ? Cu2 N219 1.902(2) . ? Cu2 N18 1.930(2) . ? Cu2 N222 2.083(2) . ? Cu2 N11 2.146(2) . ? Cu2 N212 2.420(3) . ? Cu3 N38 1.905(2) . ? Cu3 N419 1.925(2) . ? Cu3 N31 2.088(2) . ? Cu3 N422 2.163(2) . ? Cu3 N312 2.420(2) . ? Cu4 N119 1.903(2) . ? Cu4 N28 1.930(2) . ? Cu4 N122 2.086(3) . ? Cu4 N21 2.163(2) . ? Cu4 N112 2.456(2) . ? N41 C42 1.337(3) . ? N41 C46 1.348(3) . ? C42 C43 1.381(4) . ? C42 H42A 0.9500 . ? C43 C44 1.380(5) . ? C43 H43A 0.9500 . ? C44 C45 1.381(5) . ? C44 H44A 0.9500 . ? C45 C46 1.395(4) . ? C45 H45A 0.9500 . ? C46 C47 1.496(4) . ? C47 N48 1.451(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N48 C49 1.319(3) . ? C49 O410 1.242(3) . ? C49 C411 1.507(4) . ? C411 N412 1.349(3) . ? C411 C416 1.384(4) . ? N412 C413 1.355(3) . ? C413 C414 1.379(4) . ? C413 C417 1.514(4) . ? C414 C415 1.384(4) . ? C414 H41A 0.9500 . ? C415 C416 1.381(4) . ? C415 H41B 0.9500 . ? C416 H41C 0.9500 . ? C417 O418 1.251(3) . ? C417 N419 1.317(4) . ? N419 C420 1.463(3) . ? C420 C421 1.498(4) . ? C420 H42B 0.9900 . ? C420 H42C 0.9900 . ? C421 N422 1.341(3) . ? C421 C426 1.387(4) . ? N422 C423 1.344(4) . ? C423 C424 1.371(4) . ? C423 H42D 0.9500 . ? C424 C425 1.389(4) . ? C424 H42E 0.9500 . ? C425 C426 1.387(4) . ? C425 H42F 0.9500 . ? C426 H42G 0.9500 . ? N11 C16 1.333(4) . ? N11 C12 1.344(4) . ? C12 C13 1.358(4) . ? C12 H12A 0.9500 . ? C13 C14 1.376(5) . ? C13 H13A 0.9500 . ? C14 C15 1.377(5) . ? C14 H14A 0.9500 . ? C15 C16 1.375(4) . ? C15 H15A 0.9500 . ? C16 C17 1.507(4) . ? C17 N18 1.452(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N18 C19 1.318(4) . ? C19 O110 1.261(3) . ? C19 C111 1.498(4) . ? C111 N112 1.345(4) . ? C111 C116 1.383(4) . ? N112 C113 1.349(4) . ? C113 C114 1.382(4) . ? C113 C117 1.501(4) . ? C114 C115 1.373(5) . ? C114 H11A 0.9500 . ? C115 C116 1.380(5) . ? C115 H11B 0.9500 . ? C116 H11C 0.9500 . ? C117 O118 1.249(3) . ? C117 N119 1.327(4) . ? N119 C120 1.452(4) . ? C120 C121 1.501(4) . ? C120 H12B 0.9900 . ? C120 H12C 0.9900 . ? C121 N122 1.344(3) . ? C121 C126 1.393(4) . ? N122 C123 1.348(4) . ? C123 C124 1.371(4) . ? C123 H12D 0.9500 . ? C124 C125 1.389(4) . ? C124 H12E 0.9500 . ? C125 C126 1.382(5) . ? C125 H12F 0.9500 . ? C126 H12G 0.9500 . ? N21 C26 1.339(3) . ? N21 C22 1.347(3) . ? C22 C23 1.364(4) . ? C22 H22A 0.9500 . ? C23 C24 1.383(4) . ? C23 H23A 0.9500 . ? C24 C25 1.382(4) . ? C24 H24A 0.9500 . ? C25 C26 1.397(4) . ? C25 H25A 0.9500 . ? C26 C27 1.498(4) . ? C27 N28 1.460(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N28 C29 1.313(3) . ? C29 O210 1.250(3) . ? C29 C211 1.516(4) . ? C211 N212 1.348(4) . ? C211 C216 1.385(4) . ? N212 C213 1.348(4) . ? C213 C214 1.381(4) . ? C213 C217 1.507(5) . ? C214 C215 1.382(5) . ? C214 H21A 0.9500 . ? C215 C216 1.388(4) . ? C215 H21B 0.9500 . ? C216 H21C 0.9500 . ? C217 O218 1.248(3) . ? C217 N219 1.312(4) . ? N219 C220 1.459(4) . ? C220 C221 1.490(5) . ? C220 H22B 0.9900 . ? C220 H22C 0.9900 . ? C221 N222 1.346(4) . ? C221 C226 1.403(4) . ? N222 C223 1.342(4) . ? C223 C224 1.377(4) . ? C223 H22D 0.9500 . ? C224 C225 1.369(5) . ? C224 H22E 0.9500 . ? C225 C226 1.371(5) . ? C225 H22F 0.9500 . ? C226 H22G 0.9500 . ? N31 C32 1.348(4) . ? N31 C36 1.348(3) . ? C32 C33 1.371(4) . ? C32 H32A 0.9500 . ? C33 C34 1.378(5) . ? C33 H33A 0.9500 . ? C34 C35 1.382(5) . ? C34 H34A 0.9500 . ? C35 C36 1.391(4) . ? C35 H35A 0.9500 . ? C36 C37 1.486(4) . ? C37 N38 1.459(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N38 C39 1.315(4) . ? C39 O310 1.252(3) . ? C39 C311 1.504(4) . ? C311 N312 1.343(4) . ? C311 C316 1.396(4) . ? N312 C313 1.350(4) . ? C313 C314 1.386(4) . ? C313 C317 1.504(4) . ? C314 C315 1.382(5) . ? C314 H31A 0.9500 . ? C315 C316 1.368(5) . ? C315 H31B 0.9500 . ? C316 H31C 0.9500 . ? C317 O318 1.259(3) . ? C317 N319 1.315(4) . ? N319 C320 1.458(3) . ? C320 C321 1.506(4) . ? C320 H32B 0.9900 . ? C320 H32C 0.9900 . ? C321 N322 1.332(3) . ? C321 C326 1.379(4) . ? N322 C323 1.346(4) . ? C323 C324 1.375(5) . ? C323 H32D 0.9500 . ? C324 C325 1.373(5) . ? C324 H32E 0.9500 . ? C325 C326 1.382(5) . ? C325 H32F 0.9500 . ? C326 H32G 0.9500 . ? O01 C02 1.164(7) . ? C02 C03 1.461(6) . ? C02 H02A 0.9900 . ? C02 H02B 0.9900 . ? C03 H03I 0.9800 . ? C03 H03J 0.9800 . ? C03 H03K 0.9800 . ? O011 C012 1.284(11) . ? C012 C013 1.466(19) . ? C012 H01A 0.9900 . ? C012 H01E 0.9900 . ? C013 H01B 0.9800 . ? C013 H01C 0.9800 . ? C013 H01D 0.9800 . ? O014 H01F 0.8400 . ? C016 H01H 0.9800 . ? C016 H01I 0.9800 . ? C016 H01J 0.9800 . ? C023 C022 1.492(6) . ? C023 H02C 0.9800 . ? C023 H02D 0.9800 . ? C023 H02E 0.9800 . ? C022 O021 1.243(6) . ? C022 H02F 0.9900 . ? C022 H02G 0.9900 . ? C033 C032 1.326(6) . ? C033 H03A 0.9800 . ? C033 H03B 0.9800 . ? C033 H03C 0.9800 . ? C032 O031 1.358(6) . ? C032 H03F 0.9900 . ? C032 H03H 0.9900 . ? O031 H03G 0.8400 . ? 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 N48 Cu1 N319 170.03(10) . . ? N48 Cu1 N41 80.78(9) . . ? N319 Cu1 N41 97.10(9) . . ? N48 Cu1 N322 111.54(10) . . ? N319 Cu1 N322 78.42(9) . . ? N41 Cu1 N322 106.83(9) . . ? N48 Cu1 N412 77.94(9) . . ? N319 Cu1 N412 103.85(8) . . ? N41 Cu1 N412 158.73(9) . . ? N322 Cu1 N412 81.35(8) . . ? N219 Cu2 N18 171.79(10) . . ? N219 Cu2 N222 81.28(10) . . ? N18 Cu2 N222 98.22(10) . . ? N219 Cu2 N11 107.85(10) . . ? N18 Cu2 N11 80.07(10) . . ? N222 Cu2 N11 110.15(10) . . ? N219 Cu2 N212 75.53(10) . . ? N18 Cu2 N212 104.33(9) . . ? N222 Cu2 N212 156.65(9) . . ? N11 Cu2 N212 80.07(9) . . ? N38 Cu3 N419 171.17(10) . . ? N38 Cu3 N31 81.04(10) . . ? N419 Cu3 N31 98.02(9) . . ? N38 Cu3 N422 108.24(10) . . ? N419 Cu3 N422 80.13(9) . . ? N31 Cu3 N422 115.85(9) . . ? N38 Cu3 N312 75.37(9) . . ? N419 Cu3 N312 104.00(9) . . ? N31 Cu3 N312 155.00(8) . . ? N422 Cu3 N312 79.96(8) . . ? N119 Cu4 N28 170.23(10) . . ? N119 Cu4 N122 80.60(10) . . ? N28 Cu4 N122 97.80(10) . . ? N119 Cu4 N21 109.64(9) . . ? N28 Cu4 N21 79.88(9) . . ? N122 Cu4 N21 113.88(9) . . ? N119 Cu4 N112 74.94(10) . . ? N28 Cu4 N112 105.45(9) . . ? N122 Cu4 N112 155.03(9) . . ? N21 Cu4 N112 79.65(8) . . ? C42 N41 C46 119.2(2) . . ? C42 N41 Cu1 127.23(19) . . ? C46 N41 Cu1 113.57(18) . . ? N41 C42 C43 122.8(3) . . ? N41 C42 H42A 118.6 . . ? C43 C42 H42A 118.6 . . ? C44 C43 C42 118.7(3) . . ? C44 C43 H43A 120.7 . . ? C42 C43 H43A 120.7 . . ? C43 C44 C45 118.9(3) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? C44 C45 C46 119.9(3) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? N41 C46 C45 120.6(3) . . ? N41 C46 C47 116.3(2) . . ? C45 C46 C47 123.1(3) . . ? N48 C47 C46 109.1(2) . . ? N48 C47 H47A 109.9 . . ? C46 C47 H47A 109.9 . . ? N48 C47 H47B 109.9 . . ? C46 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C49 N48 C47 119.1(2) . . ? C49 N48 Cu1 122.51(19) . . ? C47 N48 Cu1 118.35(18) . . ? O410 C49 N48 126.9(3) . . ? O410 C49 C411 120.5(3) . . ? N48 C49 C411 112.5(2) . . ? N412 C411 C416 122.6(3) . . ? N412 C411 C49 116.1(2) . . ? C416 C411 C49 121.2(3) . . ? C411 N412 C413 118.0(2) . . ? C411 N412 Cu1 105.41(17) . . ? C413 N412 Cu1 129.77(18) . . ? N412 C413 C414 122.2(3) . . ? N412 C413 C417 117.6(2) . . ? C414 C413 C417 119.9(2) . . ? C413 C414 C415 118.9(3) . . ? C413 C414 H41A 120.5 . . ? C415 C414 H41A 120.5 . . ? C416 C415 C414 119.5(3) . . ? C416 C415 H41B 120.3 . . ? C414 C415 H41B 120.3 . . ? C415 C416 C411 118.6(3) . . ? C415 C416 H41C 120.7 . . ? C411 C416 H41C 120.7 . . ? O418 C417 N419 127.4(3) . . ? O418 C417 C413 118.8(3) . . ? N419 C417 C413 113.7(2) . . ? C417 N419 C420 115.7(2) . . ? C417 N419 Cu3 125.09(19) . . ? C420 N419 Cu3 119.14(17) . . ? N419 C420 C421 111.1(2) . . ? N419 C420 H42B 109.4 . . ? C421 C420 H42B 109.4 . . ? N419 C420 H42C 109.4 . . ? C421 C420 H42C 109.4 . . ? H42B C420 H42C 108.0 . . ? N422 C421 C426 121.8(3) . . ? N422 C421 C420 117.0(2) . . ? C426 C421 C420 121.2(2) . . ? C421 N422 C423 118.6(3) . . ? C421 N422 Cu3 112.65(19) . . ? C423 N422 Cu3 128.79(19) . . ? N422 C423 C424 123.1(3) . . ? N422 C423 H42D 118.5 . . ? C424 C423 H42D 118.5 . . ? C423 C424 C425 118.4(3) . . ? C423 C424 H42E 120.8 . . ? C425 C424 H42E 120.8 . . ? C426 C425 C424 119.1(3) . . ? C426 C425 H42F 120.5 . . ? C424 C425 H42F 120.5 . . ? C425 C426 C421 119.0(3) . . ? C425 C426 H42G 120.5 . . ? C421 C426 H42G 120.5 . . ? C16 N11 C12 118.8(3) . . ? C16 N11 Cu2 113.13(19) . . ? C12 N11 Cu2 127.9(2) . . ? N11 C12 C13 123.3(3) . . ? N11 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 H13A 121.1 . . ? C14 C13 H13A 121.1 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? N11 C16 C15 121.2(3) . . ? N11 C16 C17 116.9(3) . . ? C15 C16 C17 122.0(3) . . ? N18 C17 C16 110.6(2) . . ? N18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C19 N18 C17 118.4(2) . . ? C19 N18 Cu2 121.3(2) . . ? C17 N18 Cu2 119.25(18) . . ? O110 C19 N18 126.4(3) . . ? O110 C19 C111 118.9(3) . . ? N18 C19 C111 114.6(2) . . ? N112 C111 C116 122.2(3) . . ? N112 C111 C19 117.3(2) . . ? C116 C111 C19 120.4(3) . . ? C111 N112 C113 117.8(3) . . ? C111 N112 Cu4 131.45(19) . . ? C113 N112 Cu4 101.73(19) . . ? N112 C113 C114 122.7(3) . . ? N112 C113 C117 116.8(3) . . ? C114 C113 C117 120.4(3) . . ? C115 C114 C113 118.9(3) . . ? C115 C114 H11A 120.6 . . ? C113 C114 H11A 120.6 . . ? C114 C115 C116 119.1(3) . . ? C114 C115 H11B 120.4 . . ? C116 C115 H11B 120.4 . . ? C115 C116 C111 119.2(3) . . ? C115 C116 H11C 120.4 . . ? C111 C116 H11C 120.4 . . ? O118 C117 N119 126.3(3) . . ? O118 C117 C113 119.6(3) . . ? N119 C117 C113 114.1(3) . . ? C117 N119 C120 116.7(2) . . ? C117 N119 Cu4 124.7(2) . . ? C120 N119 Cu4 118.53(19) . . ? N119 C120 C121 109.7(2) . . ? N119 C120 H12B 109.7 . . ? C121 C120 H12B 109.7 . . ? N119 C120 H12C 109.7 . . ? C121 C120 H12C 109.7 . . ? H12B C120 H12C 108.2 . . ? N122 C121 C126 122.0(3) . . ? N122 C121 C120 115.5(3) . . ? C126 C121 C120 122.5(3) . . ? C121 N122 C123 118.1(3) . . ? C121 N122 Cu4 114.0(2) . . ? C123 N122 Cu4 127.9(2) . . ? N122 C123 C124 123.4(3) . . ? N122 C123 H12D 118.3 . . ? C124 C123 H12D 118.3 . . ? C123 C124 C125 118.2(3) . . ? C123 C124 H12E 120.9 . . ? C125 C124 H12E 120.9 . . ? C126 C125 C124 119.4(3) . . ? C126 C125 H12F 120.3 . . ? C124 C125 H12F 120.3 . . ? C125 C126 C121 118.8(3) . . ? C125 C126 H12G 120.6 . . ? C121 C126 H12G 120.6 . . ? C26 N21 C22 118.4(2) . . ? C26 N21 Cu4 112.75(17) . . ? C22 N21 Cu4 128.80(19) . . ? N21 C22 C23 123.1(3) . . ? N21 C22 H22A 118.4 . . ? C23 C22 H22A 118.4 . . ? C22 C23 C24 118.7(3) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C26 118.6(3) . . ? C24 C25 H25A 120.7 . . ? C26 C25 H25A 120.7 . . ? N21 C26 C25 121.8(3) . . ? N21 C26 C27 117.1(2) . . ? C25 C26 C27 121.1(2) . . ? N28 C27 C26 110.8(2) . . ? N28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? N28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 N28 C27 116.8(2) . . ? C29 N28 Cu4 123.65(19) . . ? C27 N28 Cu4 119.33(17) . . ? O210 C29 N28 127.4(3) . . ? O210 C29 C211 118.2(3) . . ? N28 C29 C211 114.4(2) . . ? N212 C211 C216 122.8(3) . . ? N212 C211 C29 117.2(3) . . ? C216 C211 C29 120.0(3) . . ? C211 N212 C213 118.2(3) . . ? C211 N212 Cu2 129.85(19) . . ? C213 N212 Cu2 102.5(2) . . ? N212 C213 C214 122.2(3) . . ? N212 C213 C217 116.3(3) . . ? C214 C213 C217 121.5(3) . . ? C213 C214 C215 119.3(3) . . ? C213 C214 H21A 120.4 . . ? C215 C214 H21A 120.4 . . ? C214 C215 C216 119.1(3) . . ? C214 C215 H21B 120.4 . . ? C216 C215 H21B 120.4 . . ? C211 C216 C215 118.4(3) . . ? C211 C216 H21C 120.8 . . ? C215 C216 H21C 120.8 . . ? O218 C217 N219 126.6(3) . . ? O218 C217 C213 119.3(3) . . ? N219 C217 C213 114.0(3) . . ? C217 N219 C220 117.3(3) . . ? C217 N219 Cu2 124.7(2) . . ? C220 N219 Cu2 117.9(2) . . ? N219 C220 C221 110.0(2) . . ? N219 C220 H22B 109.7 . . ? C221 C220 H22B 109.7 . . ? N219 C220 H22C 109.7 . . ? C221 C220 H22C 109.7 . . ? H22B C220 H22C 108.2 . . ? N222 C221 C226 120.4(3) . . ? N222 C221 C220 116.6(3) . . ? C226 C221 C220 123.0(3) . . ? C223 N222 C221 119.0(3) . . ? C223 N222 Cu2 128.0(2) . . ? C221 N222 Cu2 113.0(2) . . ? N222 C223 C224 122.9(3) . . ? N222 C223 H22D 118.6 . . ? C224 C223 H22D 118.6 . . ? C225 C224 C223 118.5(3) . . ? C225 C224 H22E 120.8 . . ? C223 C224 H22E 120.8 . . ? C224 C225 C226 119.7(3) . . ? C224 C225 H22F 120.1 . . ? C226 C225 H22F 120.1 . . ? C225 C226 C221 119.5(3) . . ? C225 C226 H22G 120.2 . . ? C221 C226 H22G 120.2 . . ? C32 N31 C36 118.5(3) . . ? C32 N31 Cu3 128.2(2) . . ? C36 N31 Cu3 113.12(19) . . ? N31 C32 C33 123.1(3) . . ? N31 C32 H32A 118.4 . . ? C33 C32 H32A 118.4 . . ? C32 C33 C34 118.6(3) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C34 C35 C36 119.7(3) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? N31 C36 C35 120.9(3) . . ? N31 C36 C37 116.6(3) . . ? C35 C36 C37 122.5(3) . . ? N38 C37 C36 109.7(2) . . ? N38 C37 H37A 109.7 . . ? C36 C37 H37A 109.7 . . ? N38 C37 H37B 109.7 . . ? C36 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C39 N38 C37 117.2(2) . . ? C39 N38 Cu3 124.4(2) . . ? C37 N38 Cu3 118.29(18) . . ? O310 C39 N38 126.7(3) . . ? O310 C39 C311 119.4(3) . . ? N38 C39 C311 113.9(3) . . ? N312 C311 C316 122.2(3) . . ? N312 C311 C39 116.8(2) . . ? C316 C311 C39 120.9(3) . . ? C311 N312 C313 118.4(2) . . ? C311 N312 Cu3 102.47(18) . . ? C313 N312 Cu3 131.36(18) . . ? N312 C313 C314 121.8(3) . . ? N312 C313 C317 118.2(2) . . ? C314 C313 C317 120.0(3) . . ? C315 C314 C313 119.3(3) . . ? C315 C314 H31A 120.3 . . ? C313 C314 H31A 120.3 . . ? C316 C315 C314 119.3(3) . . ? C316 C315 H31B 120.3 . . ? C314 C315 H31B 120.3 . . ? C315 C316 C311 118.9(3) . . ? C315 C316 H31C 120.5 . . ? C311 C316 H31C 120.5 . . ? O318 C317 N319 126.9(3) . . ? O318 C317 C313 118.4(3) . . ? N319 C317 C313 114.7(2) . . ? C317 N319 C320 117.1(2) . . ? C317 N319 Cu1 121.78(19) . . ? C320 N319 Cu1 120.21(18) . . ? N319 C320 C321 110.9(2) . . ? N319 C320 H32B 109.5 . . ? C321 C320 H32B 109.5 . . ? N319 C320 H32C 109.5 . . ? C321 C320 H32C 109.5 . . ? H32B C320 H32C 108.0 . . ? N322 C321 C326 121.4(3) . . ? N322 C321 C320 116.9(2) . . ? C326 C321 C320 121.7(3) . . ? C321 N322 C323 118.2(3) . . ? C321 N322 Cu1 110.76(19) . . ? C323 N322 Cu1 128.0(2) . . ? N322 C323 C324 123.4(3) . . ? N322 C323 H32D 118.3 . . ? C324 C323 H32D 118.3 . . ? C325 C324 C323 118.2(3) . . ? C325 C324 H32E 120.9 . . ? C323 C324 H32E 120.9 . . ? C324 C325 C326 118.7(3) . . ? C324 C325 H32F 120.6 . . ? C326 C325 H32F 120.6 . . ? C321 C326 C325 120.0(3) . . ? C321 C326 H32G 120.0 . . ? C325 C326 H32G 120.0 . . ? O01 C02 C03 127.6(7) . . ? O01 C02 H02A 105.4 . . ? C03 C02 H02A 105.4 . . ? O01 C02 H02B 105.4 . . ? C03 C02 H02B 105.4 . . ? H02A C02 H02B 106.0 . . ? C02 C03 H03I 109.5 . . ? C02 C03 H03J 109.5 . . ? H03I C03 H03J 109.5 . . ? C02 C03 H03K 109.5 . . ? H03I C03 H03K 109.5 . . ? H03J C03 H03K 109.5 . . ? O011 C012 C013 158.5(12) . . ? O011 C012 H01A 96.6 . . ? C013 C012 H01A 96.6 . . ? O011 C012 H01E 96.6 . . ? C013 C012 H01E 96.6 . . ? H01A C012 H01E 103.5 . . ? H01H C016 H01I 109.5 . . ? H01H C016 H01J 109.5 . . ? H01I C016 H01J 109.5 . . ? C022 C023 H02C 109.5 . . ? C022 C023 H02D 109.5 . . ? H02C C023 H02D 109.5 . . ? C022 C023 H02E 109.5 . . ? H02C C023 H02E 109.5 . . ? H02D C023 H02E 109.5 . . ? O021 C022 C023 118.5(5) . . ? O021 C022 H02F 107.7 . . ? C023 C022 H02F 107.7 . . ? O021 C022 H02G 107.7 . . ? C023 C022 H02G 107.7 . . ? H02F C022 H02G 107.1 . . ? C032 C033 H03A 109.5 . . ? C032 C033 H03B 109.5 . . ? H03A C033 H03B 109.5 . . ? C032 C033 H03C 109.5 . . ? H03A C033 H03C 109.5 . . ? H03B C033 H03C 109.5 . . ? C033 C032 O031 121.1(5) . . ? C033 C032 H03F 107.0 . . ? O031 C032 H03F 107.0 . . ? C033 C032 H03H 107.0 . . ? O031 C032 H03H 107.0 . . ? H03F C032 H03H 106.8 . . ? C032 O031 H03G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.545 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.070 data_cupy3b _database_code_depnum_ccdc_archive 'CCDC 246447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H55 Cu4 N12 O20' _chemical_formula_weight 1470.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.9193(6) _cell_length_b 22.0981(7) _cell_length_c 13.0496(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.4380(10) _cell_angle_gamma 90.00 _cell_volume 5950.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4508 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 15270 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5227 _reflns_number_gt 3409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0530P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5227 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.090 _refine_ls_shift/su_mean 0.003 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 0.92565(3) 0.30420(3) 0.23633(5) 0.01842(19) Uani 1 1 d . . . Cu2 Cu 0.75614(3) 0.32779(3) 0.21730(5) 0.0210(2) Uani 1 1 d . . . O100 O 0.6573(2) 0.29610(18) 0.1253(3) 0.0380(11) Uani 1 1 d . . . N101 N 0.7693(2) 0.2610(2) 0.3174(3) 0.0194(11) Uani 1 1 d . . . C102 C 0.7340(3) 0.2098(3) 0.3009(4) 0.0258(14) Uani 1 1 d . . . H10B H 0.7022 0.2070 0.2401 0.031 Uiso 1 1 calc R . . C103 C 0.7423(3) 0.1615(3) 0.3687(5) 0.0280(14) Uani 1 1 d . . . H10C H 0.7162 0.1262 0.3557 0.034 Uiso 1 1 calc R . . C104 C 0.7896(3) 0.1655(3) 0.4563(4) 0.0265(14) Uani 1 1 d . . . H10D H 0.7967 0.1329 0.5041 0.032 Uiso 1 1 calc R . . C105 C 0.8259(3) 0.2173(3) 0.4730(4) 0.0246(14) Uani 1 1 d . . . H10E H 0.8589 0.2202 0.5322 0.029 Uiso 1 1 calc R . . C106 C 0.8149(2) 0.2654(2) 0.4040(4) 0.0183(12) Uani 1 1 d . . . C107 C 0.8507(3) 0.3236(2) 0.4236(4) 0.0227(13) Uani 1 1 d . . . H10F H 0.8221 0.3538 0.4491 0.027 Uiso 1 1 calc R . . H10G H 0.8886 0.3173 0.4790 0.027 Uiso 1 1 calc R . . N108 N 0.8733(2) 0.34775(19) 0.3315(3) 0.0176(10) Uani 1 1 d . . . C109 C 0.8759(3) 0.4088(3) 0.3275(4) 0.0210(13) Uani 1 1 d . . . O110 O 0.85837(19) 0.44606(17) 0.3881(3) 0.0293(10) Uani 1 1 d . . . C111 C 0.9035(2) 0.4307(2) 0.2347(4) 0.0197(13) Uani 1 1 d . . . N112 N 0.9284(2) 0.3859(2) 0.1847(3) 0.0188(10) Uani 1 1 d . . . C113 C 0.9526(2) 0.3952(3) 0.0976(4) 0.0202(13) Uani 1 1 d . . . C114 C 0.9503(3) 0.4527(3) 0.0547(4) 0.0247(14) Uani 1 1 d . . . H11A H 0.9646 0.4596 -0.0097 0.030 Uiso 1 1 calc R . . C115 C 0.9267(3) 0.4999(3) 0.1075(5) 0.0279(14) Uani 1 1 d . . . H11B H 0.9263 0.5398 0.0803 0.033 Uiso 1 1 calc R . . C116 C 0.9038(3) 0.4894(3) 0.1997(4) 0.0242(13) Uani 1 1 d . . . H11C H 0.8887 0.5217 0.2374 0.029 Uiso 1 1 calc R . . C117 C 0.9775(3) 0.3384(3) 0.0538(4) 0.0223(13) Uani 1 1 d . . . O118 O 0.99634(19) 0.34071(18) -0.0317(3) 0.0298(10) Uani 1 1 d . . . N119 N 0.9763(2) 0.2907(2) 0.1170(3) 0.0199(11) Uani 1 1 d . . . C120 C 0.9928(3) 0.2327(3) 0.0737(4) 0.0254(14) Uani 1 1 d . . . H12A H 1.0135 0.2408 0.0121 0.030 Uiso 1 1 calc R . . H12B H 0.9522 0.2102 0.0497 0.030 Uiso 1 1 calc R . . C121 C 1.0372(3) 0.1929(3) 0.1473(4) 0.0209(13) Uani 1 1 d . . . N122 N 1.0781(2) 0.2178(2) 0.2246(4) 0.0205(11) Uani 1 1 d . . . C123 C 1.1209(3) 0.1816(2) 0.2876(4) 0.0248(14) Uani 1 1 d . . . H12C H 1.1502 0.1993 0.3428 0.030 Uiso 1 1 calc R . . C124 C 1.1224(3) 0.1199(3) 0.2723(5) 0.0304(15) Uani 1 1 d . . . H12D H 1.1525 0.0954 0.3165 0.036 Uiso 1 1 calc R . . C125 C 1.0798(3) 0.0938(3) 0.1923(5) 0.0340(16) Uani 1 1 d . . . H12E H 1.0800 0.0513 0.1809 0.041 Uiso 1 1 calc R . . C126 C 1.0373(3) 0.1306(3) 0.1299(5) 0.0281(14) Uani 1 1 d . . . H12F H 1.0076 0.1136 0.0744 0.034 Uiso 1 1 calc R . . O201 O 0.71010(18) 0.38670(17) 0.3004(3) 0.0249(9) Uani 1 1 d . . . C202 C 0.7005(3) 0.4389(3) 0.2584(4) 0.0266(14) Uani 1 1 d . . . O203 O 0.6709(2) 0.48156(18) 0.2914(3) 0.0380(11) Uani 1 1 d . . . C204 C 0.7282(3) 0.4475(2) 0.1594(4) 0.0218(13) Uani 1 1 d . . . N205 N 0.7550(2) 0.3972(2) 0.1302(3) 0.0189(10) Uani 1 1 d . . . C206 C 0.7808(2) 0.3932(3) 0.0432(4) 0.0205(13) Uani 1 1 d . . . C207 C 0.7816(3) 0.4436(3) -0.0188(4) 0.0263(14) Uani 1 1 d . . . H20A H 0.8005 0.4419 -0.0801 0.032 Uiso 1 1 calc R . . C208 C 0.7539(3) 0.4971(3) 0.0104(5) 0.0311(15) Uani 1 1 d . . . H20B H 0.7542 0.5322 -0.0315 0.037 Uiso 1 1 calc R . . C209 C 0.7265(3) 0.4994(3) 0.0987(5) 0.0296(15) Uani 1 1 d . . . H20C H 0.7068 0.5355 0.1180 0.036 Uiso 1 1 calc R . . C210 C 0.8073(3) 0.3305(3) 0.0297(4) 0.0228(13) Uani 1 1 d . . . O211 O 0.80496(18) 0.29427(17) 0.1047(3) 0.0261(9) Uani 1 1 d . . . O212 O 0.83102(19) 0.31934(17) -0.0494(3) 0.0289(10) Uani 1 1 d . . . O011 O 0.4110(4) 0.4920(4) 0.0610(7) 0.050(3) Uani 0.50 1 d P . . C011 C 0.4303(15) 0.4332(15) 0.119(2) 0.184(13) Uiso 0.50 1 d P A -1 H01D H 0.4261 0.4000 0.0673 0.221 Uiso 0.50 1 calc PR A -1 H01E H 0.3984 0.4252 0.1656 0.221 Uiso 0.50 1 calc PR A -1 C012 C 0.5028(7) 0.4292(7) 0.1885(13) 0.072(5) Uani 0.50 1 d P A -1 H01A H 0.5089 0.3893 0.2216 0.107 Uiso 0.50 1 calc PR A -1 H01B H 0.5076 0.4607 0.2421 0.107 Uiso 0.50 1 calc PR A -1 H01C H 0.5355 0.4352 0.1435 0.107 Uiso 0.50 1 calc PR A -1 O021 O 0.5789(7) 0.3374(9) 0.2934(17) 0.155(9) Uani 0.50 1 d P B -1 C021 C 0.5724(9) 0.2759(15) 0.2955(13) 0.117(11) Uani 0.50 1 d P B -1 H02D H 0.5630 0.2709 0.2191 0.141 Uiso 0.50 1 calc PR B -1 H02E H 0.6194 0.2674 0.3125 0.141 Uiso 0.50 1 calc PR B -1 C022 C 0.5536(5) 0.2205(5) 0.3173(9) 0.022(3) Uiso 0.50 1 d P B -1 H02A H 0.5771 0.1906 0.2825 0.033 Uiso 0.50 1 calc PR B -1 H02B H 0.5069 0.2163 0.2929 0.033 Uiso 0.50 1 calc PR B -1 H02C H 0.5628 0.2140 0.3925 0.033 Uiso 0.50 1 calc PR B -1 O001 O 0.5885(4) 0.4014(4) 0.0657(6) 0.145(3) Uani 1 1 d . . . O002 O 0.5998(3) 0.1272(2) 0.1981(4) 0.0679(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0204(4) 0.0159(4) 0.0203(4) 0.0006(3) 0.0076(3) 0.0003(3) Cu2 0.0259(4) 0.0176(4) 0.0207(4) 0.0030(3) 0.0078(3) 0.0030(3) O100 0.037(3) 0.028(3) 0.045(3) -0.002(2) -0.004(2) -0.004(2) N101 0.019(2) 0.020(3) 0.021(3) 0.002(2) 0.007(2) 0.002(2) C102 0.024(3) 0.028(4) 0.026(3) 0.001(3) 0.006(3) -0.002(3) C103 0.033(4) 0.022(4) 0.033(4) 0.001(3) 0.016(3) -0.003(3) C104 0.028(3) 0.026(4) 0.028(3) 0.013(3) 0.013(3) 0.005(3) C105 0.025(3) 0.027(3) 0.022(3) 0.003(3) 0.005(3) 0.002(3) C106 0.018(3) 0.020(3) 0.020(3) -0.001(2) 0.012(2) 0.004(2) C107 0.026(3) 0.027(3) 0.016(3) -0.001(3) 0.005(2) -0.003(3) N108 0.021(3) 0.015(3) 0.018(3) 0.0002(19) 0.008(2) -0.001(2) C109 0.020(3) 0.025(4) 0.018(3) 0.001(3) 0.004(2) 0.002(3) O110 0.039(3) 0.019(2) 0.033(3) -0.0074(19) 0.017(2) 0.0002(19) C111 0.018(3) 0.018(3) 0.023(3) -0.001(2) 0.002(3) -0.005(2) N112 0.017(2) 0.021(3) 0.018(3) 0.004(2) 0.004(2) -0.001(2) C113 0.014(3) 0.026(3) 0.021(3) -0.001(3) 0.002(2) -0.003(2) C114 0.028(3) 0.025(4) 0.022(3) 0.009(3) 0.009(3) -0.001(3) C115 0.022(3) 0.020(3) 0.043(4) 0.010(3) 0.007(3) 0.001(3) C116 0.028(3) 0.020(3) 0.028(3) 0.001(3) 0.011(3) 0.000(3) C117 0.016(3) 0.029(4) 0.021(3) -0.001(3) 0.001(2) 0.002(3) O118 0.032(2) 0.039(3) 0.022(2) 0.0059(19) 0.0128(18) 0.008(2) N119 0.022(3) 0.019(3) 0.019(3) -0.001(2) 0.004(2) 0.001(2) C120 0.029(3) 0.026(4) 0.023(3) -0.003(3) 0.007(3) 0.004(3) C121 0.017(3) 0.023(3) 0.024(3) -0.003(3) 0.009(2) -0.002(3) N122 0.020(3) 0.018(3) 0.026(3) -0.001(2) 0.011(2) -0.001(2) C123 0.023(3) 0.023(4) 0.028(3) -0.002(3) 0.004(3) -0.004(3) C124 0.026(4) 0.021(4) 0.043(4) 0.003(3) 0.003(3) 0.004(3) C125 0.036(4) 0.009(3) 0.057(5) -0.006(3) 0.010(3) 0.000(3) C126 0.021(3) 0.029(4) 0.034(4) -0.008(3) 0.002(3) -0.004(3) O201 0.032(2) 0.021(2) 0.023(2) 0.0023(18) 0.0104(18) 0.0064(18) C202 0.036(4) 0.022(3) 0.022(3) 0.006(3) 0.005(3) 0.001(3) O203 0.057(3) 0.025(3) 0.037(3) 0.002(2) 0.024(2) 0.016(2) C204 0.021(3) 0.020(3) 0.024(3) -0.003(3) 0.003(2) 0.002(3) N205 0.017(2) 0.020(3) 0.020(3) 0.001(2) 0.001(2) 0.000(2) C206 0.016(3) 0.024(3) 0.021(3) 0.000(3) 0.000(2) -0.001(2) C207 0.025(3) 0.032(4) 0.024(3) 0.008(3) 0.007(3) -0.003(3) C208 0.035(4) 0.030(4) 0.029(4) 0.012(3) 0.006(3) 0.000(3) C209 0.036(4) 0.018(3) 0.034(4) 0.001(3) 0.003(3) -0.001(3) C210 0.020(3) 0.027(3) 0.019(3) -0.002(3) -0.003(3) -0.003(3) O211 0.030(2) 0.025(2) 0.025(2) 0.0032(19) 0.0073(18) 0.0047(18) O212 0.034(2) 0.032(3) 0.023(2) -0.0042(18) 0.0120(19) 0.0001(19) O011 0.050(6) 0.062(7) 0.047(6) 0.000(5) 0.033(5) 0.002(5) C012 0.050(10) 0.059(11) 0.109(15) 0.030(10) 0.025(10) 0.020(9) O021 0.046(9) 0.166(18) 0.26(2) 0.108(17) 0.059(11) 0.035(11) C021 0.049(12) 0.28(4) 0.023(9) 0.022(15) -0.001(8) 0.046(19) O001 0.125(7) 0.145(8) 0.143(7) 0.009(6) -0.044(5) -0.014(6) O002 0.084(4) 0.045(3) 0.069(4) 0.014(3) -0.003(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N112 1.932(4) . y Cu1 N122 1.980(4) 2_755 y Cu1 N108 2.028(4) . y Cu1 N119 2.044(4) . y Cu2 N205 1.908(4) . y Cu2 N101 1.960(4) . y Cu2 O201 2.035(4) . y Cu2 O211 2.059(4) . y Cu2 O100 2.322(4) . y N101 C102 1.348(7) . ? N101 C106 1.357(7) . ? C102 C103 1.380(8) . ? C103 C104 1.386(8) . ? C104 C105 1.370(8) . ? C105 C106 1.389(7) . ? C106 C107 1.489(7) . ? C107 N108 1.463(6) . ? N108 C109 1.352(7) . ? C109 O110 1.238(6) . ? C109 C111 1.503(7) . ? C111 N112 1.337(7) . ? C111 C116 1.376(7) . ? N112 C113 1.332(7) . ? C113 C114 1.387(7) . ? C113 C117 1.506(8) . ? C114 C115 1.384(8) . ? C115 C116 1.387(7) . ? C117 O118 1.244(6) . ? C117 N119 1.340(7) . ? N119 C120 1.466(7) . ? C120 C121 1.505(8) . ? C121 N122 1.330(7) . ? C121 C126 1.395(8) . ? N122 C123 1.370(7) . ? N122 Cu1 1.981(4) 2_755 ? C123 C124 1.379(7) . ? C124 C125 1.382(8) . ? C125 C126 1.371(8) . ? O201 C202 1.278(6) . ? C202 O203 1.243(7) . ? C202 C204 1.512(8) . ? C204 N205 1.328(7) . ? C204 C209 1.391(8) . ? N205 C206 1.337(7) . ? C206 C207 1.378(7) . ? C206 C210 1.514(8) . ? C207 C208 1.396(8) . ? C208 C209 1.370(8) . ? C210 O212 1.241(6) . ? C210 O211 1.272(6) . ? O011 C011 1.52(3) . ? C011 C012 1.64(3) . ? O021 C021 1.37(3) . ? C021 C022 1.33(3) . ? 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 N112 Cu1 N122 174.59(18) . 2_755 y N112 Cu1 N108 79.64(18) . . y N122 Cu1 N108 104.53(18) 2_755 . y N112 Cu1 N119 79.70(18) . . y N122 Cu1 N119 95.96(18) 2_755 . y N108 Cu1 N119 159.23(17) . . y N205 Cu2 N101 171.69(18) . . y N205 Cu2 O201 80.91(17) . . y N101 Cu2 O201 98.82(17) . . y N205 Cu2 O211 79.85(17) . . y N101 Cu2 O211 99.95(16) . . y O201 Cu2 O211 160.67(15) . . y N205 Cu2 O100 90.64(16) . . y N101 Cu2 O100 97.67(17) . . y O201 Cu2 O100 90.53(15) . . y O211 Cu2 O100 91.51(15) . . y C102 N101 C106 119.0(5) . . ? C102 N101 Cu2 120.8(4) . . ? C106 N101 Cu2 120.3(4) . . ? N101 C102 C103 122.7(5) . . ? C102 C103 C104 118.4(5) . . ? C105 C104 C103 119.2(5) . . ? C104 C105 C106 120.5(5) . . ? N101 C106 C105 120.3(5) . . ? N101 C106 C107 118.1(5) . . ? C105 C106 C107 121.6(5) . . ? N108 C107 C106 113.3(4) . . ? C109 N108 C107 114.6(4) . . ? C109 N108 Cu1 114.9(3) . . ? C107 N108 Cu1 127.6(3) . . ? O110 C109 N108 128.4(5) . . ? O110 C109 C111 119.6(5) . . ? N108 C109 C111 112.0(5) . . ? N112 C111 C116 120.8(5) . . ? N112 C111 C109 112.8(5) . . ? C116 C111 C109 126.4(5) . . ? C113 N112 C111 122.4(5) . . ? C113 N112 Cu1 118.5(4) . . ? C111 N112 Cu1 119.0(4) . . ? N112 C113 C114 119.4(5) . . ? N112 C113 C117 113.6(5) . . ? C114 C113 C117 127.0(5) . . ? C115 C114 C113 118.8(5) . . ? C114 C115 C116 120.5(5) . . ? C111 C116 C115 117.9(5) . . ? O118 C117 N119 128.6(5) . . ? O118 C117 C113 119.1(5) . . ? N119 C117 C113 112.2(5) . . ? C117 N119 C120 115.0(5) . . ? C117 N119 Cu1 114.7(4) . . ? C120 N119 Cu1 127.2(4) . . ? N119 C120 C121 115.2(5) . . ? N122 C121 C126 120.9(5) . . ? N122 C121 C120 119.7(5) . . ? C126 C121 C120 119.3(5) . . ? C121 N122 C123 119.3(5) . . ? C121 N122 Cu1 123.1(4) . 2_755 ? C123 N122 Cu1 117.3(4) . 2_755 ? N122 C123 C124 121.2(5) . . ? C123 C124 C125 119.7(6) . . ? C126 C125 C124 118.4(5) . . ? C125 C126 C121 120.4(5) . . ? C202 O201 Cu2 113.7(4) . . ? O203 C202 O201 126.0(5) . . ? O203 C202 C204 118.8(5) . . ? O201 C202 C204 115.2(5) . . ? N205 C204 C209 119.9(5) . . ? N205 C204 C202 112.2(5) . . ? C209 C204 C202 127.8(5) . . ? C204 N205 C206 123.2(5) . . ? C204 N205 Cu2 117.8(4) . . ? C206 N205 Cu2 119.0(4) . . ? N205 C206 C207 119.4(5) . . ? N205 C206 C210 111.5(5) . . ? C207 C206 C210 129.1(5) . . ? C206 C207 C208 118.6(5) . . ? C209 C208 C207 120.7(6) . . ? C208 C209 C204 118.2(6) . . ? O212 C210 O211 125.9(5) . . ? O212 C210 C206 118.9(5) . . ? O211 C210 C206 115.2(5) . . ? C210 O211 Cu2 114.1(4) . . ? O011 C011 C012 118(2) . . ? C022 C021 O021 162.4(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.042 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.109 data_gl6 _database_code_depnum_ccdc_archive 'CCDC 246448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H51 Co N10 O14' _chemical_formula_weight 930.82 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' Co Co 0.3494 0.9721 '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 14.4465(9) _cell_length_b 15.0309(9) _cell_length_c 21.0726(13) _cell_angle_alpha 91.2960(10) _cell_angle_beta 97.0280(10) _cell_angle_gamma 106.3940(10) _cell_volume 4348.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6539 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 23401 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.1816 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.50 _reflns_number_total 15862 _reflns_number_gt 7255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15862 _refine_ls_number_parameters 1240 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.27522(5) 0.80476(5) 0.48695(3) 0.01987(19) Uani 1 1 d . A . Co2 Co 0.73827(5) -0.30193(5) 0.02628(3) 0.01967(19) Uani 1 1 d . . . N11 N 1.2571(6) 1.0366(7) 0.4041(5) 0.0362(18) Uani 0.90 1 d P A 1 C12 C 1.1938(9) 1.0858(10) 0.3901(7) 0.058(3) Uani 0.90 1 d P A 1 H12A H 1.1547 1.0739 0.3494 0.069 Uiso 0.90 1 calc PR A 1 C13 C 1.1826(12) 1.1527(12) 0.4318(9) 0.089(4) Uani 0.90 1 d PU A 1 H13A H 1.1379 1.1872 0.4200 0.107 Uiso 0.90 1 calc PR A 1 C14 C 1.2378(13) 1.1679(12) 0.4907(9) 0.118(6) Uani 0.90 1 d P A 1 H14A H 1.2320 1.2136 0.5206 0.142 Uiso 0.90 1 calc PR A 1 C15 C 1.3015(9) 1.1169(8) 0.5062(6) 0.076(3) Uani 0.90 1 d P A 1 H15A H 1.3386 1.1257 0.5475 0.092 Uiso 0.90 1 calc PR A 1 C16 C 1.3118(6) 1.0528(6) 0.4619(5) 0.0419(18) Uani 0.90 1 d P A 1 N11A N 1.260(4) 1.052(7) 0.403(3) 0.0362(18) Uani 0.10 1 d PG A 2 C12A C 1.192(7) 1.101(10) 0.392(6) 0.058(3) Uani 0.10 1 d PG A 2 H12F H 1.1525 1.0942 0.3522 0.069 Uiso 0.10 1 calc PR A 2 C13A C 1.182(9) 1.160(10) 0.441(7) 0.089(4) Uani 0.10 1 d PGU A 2 H13D H 1.1354 1.1941 0.4339 0.107 Uiso 0.10 1 calc PR A 2 C14A C 1.240(9) 1.170(8) 0.500(7) 0.118(6) Uani 0.10 1 d PG A 2 H14B H 1.2327 1.2108 0.5332 0.142 Uiso 0.10 1 calc PR A 2 C15A C 1.308(7) 1.121(5) 0.510(4) 0.076(3) Uani 0.10 1 d PG A 2 H15C H 1.3471 1.1276 0.5508 0.092 Uiso 0.10 1 calc PR A 2 C16A C 1.318(3) 1.061(4) 0.462(3) 0.0419(18) Uani 0.10 1 d PG A 2 C17 C 1.3890(4) 1.0060(4) 0.4754(3) 0.0379(16) Uani 1 1 d G . . H17A H 1.4473 1.0410 0.4566 0.045 Uiso 1 1 calc R A 1 H17B H 1.4075 1.0079 0.5223 0.045 Uiso 1 1 calc R A 1 N18 N 1.3603(3) 0.9093(3) 0.4500(2) 0.0264(11) Uani 1 1 d . A . O19 O 1.4585(3) 0.9441(3) 0.36892(17) 0.0492(12) Uani 1 1 d . A . C19 C 1.3998(4) 0.8897(4) 0.3995(3) 0.0315(14) Uani 1 1 d . . . C110 C 1.3603(3) 0.7886(4) 0.3780(2) 0.0236(13) Uani 1 1 d . A . N111 N 1.2951(3) 0.7424(3) 0.41482(19) 0.0190(10) Uani 1 1 d . . . C112 C 1.2520(3) 0.6508(4) 0.4054(2) 0.0222(13) Uani 1 1 d . A . C113 C 1.2730(4) 0.6006(4) 0.3571(3) 0.0311(14) Uani 1 1 d . . . H11A H 1.2431 0.5355 0.3506 0.037 Uiso 1 1 calc R A . C114 C 1.3391(4) 0.6466(4) 0.3176(3) 0.0372(16) Uani 1 1 d . A . H11B H 1.3535 0.6134 0.2830 0.045 Uiso 1 1 calc R . . C115 C 1.3844(4) 0.7418(4) 0.3286(3) 0.0322(14) Uani 1 1 d . . . H11C H 1.4309 0.7736 0.3026 0.039 Uiso 1 1 calc R A . O116 O 1.1366(2) 0.5307(2) 0.45349(17) 0.0330(10) Uani 1 1 d . A . C116 C 1.1870(3) 0.6143(3) 0.4552(2) 0.0207(12) Uani 1 1 d . . . N117 N 1.1936(3) 0.6802(3) 0.50098(19) 0.0200(10) Uani 1 1 d . A . C118 C 1.1435(3) 0.6515(3) 0.5563(2) 0.0229(13) Uani 1 1 d . . . H11D H 1.0900 0.5936 0.5443 0.027 Uiso 1 1 calc R A . H11E H 1.1143 0.7001 0.5693 0.027 Uiso 1 1 calc R . . C119 C 1.2115(4) 0.6352(3) 0.6123(3) 0.0258(13) Uani 1 1 d . A . N120 N 1.1973(3) 0.6618(3) 0.6713(2) 0.0359(12) Uani 1 1 d . . . C121 C 1.2565(4) 0.6455(4) 0.7220(3) 0.0396(16) Uani 1 1 d . A . H12B H 1.2483 0.6646 0.7638 0.048 Uiso 1 1 calc R . . C122 C 1.3272(4) 0.6029(4) 0.7159(3) 0.0432(16) Uani 1 1 d . . . H12C H 1.3664 0.5921 0.7528 0.052 Uiso 1 1 calc R A . C123 C 1.3410(4) 0.5762(4) 0.6566(3) 0.0389(16) Uani 1 1 d . A . H12D H 1.3905 0.5473 0.6516 0.047 Uiso 1 1 calc R . . C124 C 1.2821(4) 0.5916(3) 0.6036(3) 0.0297(14) Uani 1 1 d . . . H12E H 1.2900 0.5725 0.5618 0.036 Uiso 1 1 calc R A . N21 N 1.3862(3) 0.7850(3) 0.5407(2) 0.0224(10) Uani 1 1 d . . . C22 C 1.4461(4) 0.7359(4) 0.5231(3) 0.0295(14) Uani 1 1 d . A . H22A H 1.4352 0.7095 0.4806 0.035 Uiso 1 1 calc R . . C23 C 1.5214(4) 0.7234(4) 0.5647(3) 0.0334(15) Uani 1 1 d . . . H23A H 1.5621 0.6891 0.5509 0.040 Uiso 1 1 calc R A . C24 C 1.5372(4) 0.7609(4) 0.6261(3) 0.0380(16) Uani 1 1 d . A . H24A H 1.5889 0.7525 0.6556 0.046 Uiso 1 1 calc R . . C25 C 1.4778(4) 0.8107(4) 0.6452(3) 0.0341(15) Uani 1 1 d . . . H25A H 1.4887 0.8376 0.6876 0.041 Uiso 1 1 calc R A . C26 C 1.4019(4) 0.8214(3) 0.6020(3) 0.0250(13) Uani 1 1 d . A . C27 C 1.3329(4) 0.8726(3) 0.6189(2) 0.0285(14) Uani 1 1 d . . . H27A H 1.3008 0.8452 0.6557 0.034 Uiso 1 1 calc R A . H27B H 1.3681 0.9387 0.6307 0.034 Uiso 1 1 calc R . . N28 N 1.2605(3) 0.8648(3) 0.56260(19) 0.0222(10) Uani 1 1 d . A . O29 O 1.1534(3) 0.9185(3) 0.61452(18) 0.0419(10) Uani 1 1 d . A . C29 C 1.1804(4) 0.8872(4) 0.5659(3) 0.0272(13) Uani 1 1 d . . . C210 C 1.1182(4) 0.8707(3) 0.5028(3) 0.0235(13) Uani 1 1 d . A . N211 N 1.1553(3) 0.8371(3) 0.4533(2) 0.0190(10) Uani 1 1 d . . . C212 C 1.1043(3) 0.8268(3) 0.3947(3) 0.0199(12) Uani 1 1 d . A . C213 C 1.0144(3) 0.8440(3) 0.3832(3) 0.0284(14) Uani 1 1 d . . . H21A H 0.9791 0.8337 0.3413 0.034 Uiso 1 1 calc R A . C214 C 0.9767(4) 0.8763(4) 0.4331(3) 0.0359(15) Uani 1 1 d . A . H21B H 0.9152 0.8883 0.4262 0.043 Uiso 1 1 calc R . . C215 C 1.0300(4) 0.8907(4) 0.4933(3) 0.0325(14) Uani 1 1 d . . . H21C H 1.0061 0.9143 0.5282 0.039 Uiso 1 1 calc R A . O216 O 1.1151(2) 0.7251(2) 0.30724(17) 0.0297(9) Uani 1 1 d . A . C216 C 1.1447(4) 0.8034(4) 0.3357(2) 0.0226(13) Uani 1 1 d . . . N217 N 1.2082(3) 0.8760(3) 0.31474(19) 0.0248(11) Uani 1 1 d . A . H21F H 1.2264 0.9292 0.3376 0.030 Uiso 1 1 calc R . . C218 C 1.2482(4) 0.8699(4) 0.2554(2) 0.0299(14) Uani 1 1 d . . . H21D H 1.2604 0.8086 0.2512 0.036 Uiso 1 1 calc R A . H21E H 1.3116 0.9181 0.2579 0.036 Uiso 1 1 calc R . . C219 C 1.1841(4) 0.8818(3) 0.1966(3) 0.0238(13) Uani 1 1 d . A . N220 N 1.2140(3) 0.8616(3) 0.1414(2) 0.0295(11) Uani 1 1 d . . . C221 C 1.1629(4) 0.8735(4) 0.0867(3) 0.0367(15) Uani 1 1 d . A . H22B H 1.1833 0.8595 0.0474 0.044 Uiso 1 1 calc R . . C222 C 1.0812(4) 0.9054(4) 0.0844(3) 0.0374(16) Uani 1 1 d . . . H22C H 1.0466 0.9128 0.0445 0.045 Uiso 1 1 calc R A . C223 C 1.0515(4) 0.9261(4) 0.1411(3) 0.0380(16) Uani 1 1 d . A . H22D H 0.9960 0.9482 0.1411 0.046 Uiso 1 1 calc R . . C224 C 1.1038(4) 0.9143(4) 0.1978(3) 0.0305(14) Uani 1 1 d . . . H22E H 1.0849 0.9284 0.2375 0.037 Uiso 1 1 calc R A . N31 N 0.7562(3) -0.5184(3) 0.1193(2) 0.0287(11) Uani 1 1 d . . . C32 C 0.8283(4) -0.5588(4) 0.1326(3) 0.0355(15) Uani 1 1 d . . . H32A H 0.8692 -0.5412 0.1724 0.043 Uiso 1 1 calc R . . C33 C 0.8468(4) -0.6238(4) 0.0923(3) 0.0460(17) Uani 1 1 d . . . H33A H 0.8984 -0.6502 0.1042 0.055 Uiso 1 1 calc R . . C34 C 0.7881(4) -0.6490(4) 0.0347(3) 0.0460(18) Uani 1 1 d . . . H34A H 0.7976 -0.6948 0.0064 0.055 Uiso 1 1 calc R . . C35 C 0.7146(4) -0.6075(4) 0.0178(3) 0.0385(16) Uani 1 1 d . . . H35A H 0.6748 -0.6228 -0.0225 0.046 Uiso 1 1 calc R . . C36 C 0.7008(4) -0.5426(3) 0.0617(3) 0.0253(13) Uani 1 1 d . . . C37 C 0.6189(3) -0.4993(3) 0.0460(3) 0.0258(13) Uani 1 1 d . . . H37A H 0.5976 -0.5073 -0.0008 0.031 Uiso 1 1 calc R . . H37B H 0.5630 -0.5325 0.0675 0.031 Uiso 1 1 calc R . . N38 N 0.6468(3) -0.4003(3) 0.06588(19) 0.0211(10) Uani 1 1 d . . . O39 O 0.5355(2) -0.4197(2) 0.13854(17) 0.0323(9) Uani 1 1 d . . . C39 C 0.6030(4) -0.3720(4) 0.1101(2) 0.0232(13) Uani 1 1 d . . . C310 C 0.6445(3) -0.2688(3) 0.1269(2) 0.0218(12) Uani 1 1 d . . . N311 N 0.7120(3) -0.2283(3) 0.08957(19) 0.0181(10) Uani 1 1 d . . . C312 C 0.7569(3) -0.1367(3) 0.0942(2) 0.0214(12) Uani 1 1 d . . . C313 C 0.7349(4) -0.0802(4) 0.1392(2) 0.0266(13) Uani 1 1 d . . . H31A H 0.7661 -0.0152 0.1430 0.032 Uiso 1 1 calc R . . C314 C 0.6660(4) -0.1205(4) 0.1789(2) 0.0286(14) Uani 1 1 d . . . H31B H 0.6512 -0.0832 0.2110 0.034 Uiso 1 1 calc R . . C315 C 0.6193(3) -0.2144(4) 0.1716(2) 0.0253(13) Uani 1 1 d . . . H31C H 0.5701 -0.2415 0.1972 0.030 Uiso 1 1 calc R . . O316 O 0.8721(2) -0.0254(2) 0.04162(17) 0.0272(9) Uani 1 1 d . . . C316 C 0.8238(3) -0.1078(4) 0.0440(2) 0.0212(12) Uani 1 1 d . . . N317 N 0.8204(3) -0.1802(3) 0.00481(19) 0.0208(10) Uani 1 1 d . . . C318 C 0.8758(3) -0.1609(3) -0.0488(2) 0.0240(13) Uani 1 1 d . . . H31D H 0.9055 -0.2116 -0.0551 0.029 Uiso 1 1 calc R . . H31E H 0.9292 -0.1027 -0.0381 0.029 Uiso 1 1 calc R . . C319 C 0.8157(4) -0.1513(4) -0.1105(3) 0.0290(14) Uani 1 1 d . . . N320 N 0.8426(4) -0.1838(3) -0.1643(2) 0.0430(13) Uani 1 1 d . . . C321 C 0.7912(5) -0.1731(4) -0.2210(3) 0.0547(19) Uani 1 1 d . . . H32B H 0.8077 -0.1955 -0.2593 0.066 Uiso 1 1 calc R . . C322 C 0.7181(5) -0.1327(4) -0.2263(3) 0.057(2) Uani 1 1 d . . . H32C H 0.6854 -0.1263 -0.2671 0.068 Uiso 1 1 calc R . . C323 C 0.6921(4) -0.1009(4) -0.1712(3) 0.0441(17) Uani 1 1 d . . . H32D H 0.6405 -0.0729 -0.1735 0.053 Uiso 1 1 calc R . . C324 C 0.7421(4) -0.1101(3) -0.1125(3) 0.0300(14) Uani 1 1 d . . . H32E H 0.7255 -0.0882 -0.0741 0.036 Uiso 1 1 calc R . . N41 N 0.6326(3) -0.2926(3) -0.0364(2) 0.0201(10) Uani 1 1 d . . . C42 C 0.5668(4) -0.2465(3) -0.0282(3) 0.0267(13) Uani 1 1 d . . . H42A H 0.5690 -0.2175 0.0127 0.032 Uiso 1 1 calc R . . C43 C 0.4963(4) -0.2398(4) -0.0770(3) 0.0315(14) Uani 1 1 d . . . H43A H 0.4507 -0.2073 -0.0694 0.038 Uiso 1 1 calc R . . C44 C 0.4928(4) -0.2810(4) -0.1368(3) 0.0329(14) Uani 1 1 d . . . H44A H 0.4470 -0.2749 -0.1716 0.039 Uiso 1 1 calc R . . C45 C 0.5571(4) -0.3307(4) -0.1449(3) 0.0316(14) Uani 1 1 d . . . H45A H 0.5544 -0.3616 -0.1852 0.038 Uiso 1 1 calc R . . C46 C 0.6257(3) -0.3363(3) -0.0946(3) 0.0214(13) Uani 1 1 d . . . C47 C 0.7001(3) -0.3875(3) -0.1003(2) 0.0250(13) Uani 1 1 d . . . H47A H 0.6675 -0.4547 -0.1097 0.030 Uiso 1 1 calc R . . H47B H 0.7381 -0.3640 -0.1355 0.030 Uiso 1 1 calc R . . N48 N 0.7639(3) -0.3728(3) -0.0401(2) 0.0219(10) Uani 1 1 d . . . O49 O 0.8816(2) -0.4308(3) -0.07562(18) 0.0401(10) Uani 1 1 d . . . C49 C 0.8480(4) -0.3924(3) -0.0342(3) 0.0244(13) Uani 1 1 d . . . C410 C 0.9027(4) -0.3643(3) 0.0311(3) 0.0238(13) Uani 1 1 d . . . N411 N 0.8576(3) -0.3265(3) 0.0729(2) 0.0218(10) Uani 1 1 d . . . C412 C 0.9012(4) -0.3072(3) 0.1336(2) 0.0225(13) Uani 1 1 d . . . C413 C 0.9920(4) -0.3202(3) 0.1531(3) 0.0304(14) Uani 1 1 d . . . H41A H 1.0215 -0.3049 0.1963 0.037 Uiso 1 1 calc R . . C414 C 1.0383(4) -0.3547(4) 0.1103(3) 0.0349(15) Uani 1 1 d . . . H41B H 1.1013 -0.3614 0.1229 0.042 Uiso 1 1 calc R . . C415 C 0.9919(4) -0.3801(3) 0.0478(3) 0.0295(14) Uani 1 1 d . . . H41C H 1.0209 -0.4075 0.0176 0.035 Uiso 1 1 calc R . . O416 O 0.8776(2) -0.2032(2) 0.21433(18) 0.0335(10) Uani 1 1 d . . . C416 C 0.8516(3) -0.2810(4) 0.1874(3) 0.0243(13) Uani 1 1 d . . . N417 N 0.7857(3) -0.3555(3) 0.20621(19) 0.0238(10) Uani 1 1 d . . . H41F H 0.7673 -0.4079 0.1823 0.029 Uiso 1 1 calc R . . C418 C 0.7455(3) -0.3501(3) 0.2649(2) 0.0262(13) Uani 1 1 d . . . H41D H 0.6812 -0.3973 0.2615 0.031 Uiso 1 1 calc R . . H41E H 0.7348 -0.2883 0.2698 0.031 Uiso 1 1 calc R . . C419 C 0.8073(3) -0.3649(3) 0.3242(3) 0.0211(12) Uani 1 1 d . . . N420 N 0.7757(3) -0.3497(3) 0.3805(2) 0.0292(11) Uani 1 1 d . . . C421 C 0.8282(4) -0.3638(4) 0.4342(3) 0.0357(15) Uani 1 1 d . . . H42B H 0.8070 -0.3536 0.4740 0.043 Uiso 1 1 calc R . . C422 C 0.9111(4) -0.3921(4) 0.4353(3) 0.0334(15) Uani 1 1 d . . . H42C H 0.9465 -0.4001 0.4748 0.040 Uiso 1 1 calc R . . C423 C 0.9413(4) -0.4085(4) 0.3785(3) 0.0301(14) Uani 1 1 d . . . H42D H 0.9978 -0.4287 0.3778 0.036 Uiso 1 1 calc R . . C424 C 0.8890(3) -0.3954(3) 0.3218(3) 0.0255(13) Uani 1 1 d . . . H42E H 0.9087 -0.4071 0.2818 0.031 Uiso 1 1 calc R . . O001 O -0.0588(3) 0.4677(3) -0.2565(2) 0.0436(11) Uani 1 1 d D . . H01A H -0.076(4) 0.4092(19) -0.271(3) 0.065 Uiso 1 1 d D . . H01B H -0.107(3) 0.445(4) -0.232(2) 0.065 Uiso 1 1 d D . . O002 O 0.8138(3) 1.1022(4) 0.2514(2) 0.0730(15) Uani 1 1 d D . . H02A H 0.8610 1.1351 0.2325 0.109 Uiso 1 1 d D . . H02B H 0.830(3) 1.095(5) 0.2911(13) 0.109 Uiso 1 1 d D . . O003 O 1.1149(3) 0.3544(3) 0.4017(2) 0.0487(12) Uani 1 1 d D . . H03A H 1.076(4) 0.350(5) 0.3657(18) 0.073 Uiso 1 1 d D . . H03B H 1.123(4) 0.410(2) 0.420(3) 0.073 Uiso 1 1 d D . . O004 O 0.7933(3) -0.5236(3) -0.1876(2) 0.0446(11) Uani 1 1 d D . . H4A H 0.823(4) -0.482(3) -0.155(2) 0.067 Uiso 1 1 d D . . H4B H 0.799(5) -0.478(3) -0.214(2) 0.067 Uiso 1 1 d D . . O005 O 1.4008(3) 0.8369(3) 0.15225(19) 0.0381(10) Uani 1 1 d D . . H05A H 1.423(4) 0.859(4) 0.1181(17) 0.057 Uiso 1 1 d D . . H05B H 1.3413(19) 0.838(4) 0.146(3) 0.057 Uiso 1 1 d D . . O006 O 0.4986(3) -0.4729(3) 0.26201(19) 0.0464(11) Uani 1 1 d D . . H06C H 0.508(4) -0.438(4) 0.231(2) 0.070 Uiso 1 1 d D . . O007 O 0.8389(3) 0.1396(3) 0.0732(2) 0.0549(12) Uani 1 1 d D . . H07A H 0.856(4) 0.089(3) 0.066(3) 0.082 Uiso 1 1 d D . . H07B H 0.884(4) 0.159(4) 0.107(2) 0.082 Uiso 1 1 d D . . O008 O 0.9844(3) 0.3497(3) 0.2857(2) 0.0534(12) Uani 1 1 d D . . H08A H 1.015(4) 0.309(4) 0.299(3) 0.080 Uiso 1 1 d D . . O009 O 0.6866(4) -0.4138(3) -0.2591(2) 0.0580(13) Uani 1 1 d D . . H09A H 0.675(5) -0.389(4) -0.2963(19) 0.087 Uiso 1 1 d D . . H09B H 0.712(5) -0.438(4) -0.226(2) 0.087 Uiso 1 1 d D . . O010 O 0.3696(3) 0.6465(3) 0.1539(2) 0.0540(12) Uani 1 1 d D . . H10A H 0.413(3) 0.618(4) 0.151(3) 0.081 Uiso 1 1 d D . . H10B H 0.371(5) 0.703(2) 0.147(3) 0.081 Uiso 1 1 d D . . O011 O 0.5763(3) -0.3535(3) 0.3701(2) 0.0538(12) Uani 1 1 d D . . H01C H 0.599(5) -0.304(3) 0.347(3) 0.081 Uiso 1 1 d D . . H01D H 0.638(2) -0.346(5) 0.385(3) 0.081 Uiso 1 1 d D . . O012 O 1.6352(4) 1.1249(3) 0.1983(2) 0.0678(14) Uani 1 1 d D . . H02C H 1.681(4) 1.104(5) 0.219(3) 0.102 Uiso 1 1 d D . . H02D H 1.589(4) 1.082(4) 0.212(3) 0.102 Uiso 1 1 d D . . O013 O 1.6363(4) 1.0863(3) 0.0688(3) 0.0666(14) Uani 1 1 d D . . H13B H 1.691(3) 1.131(4) 0.086(3) 0.100 Uiso 1 1 d D . . H13C H 1.619(5) 1.027(2) 0.052(3) 0.100 Uiso 1 1 d D . . O014 O 1.4931(3) 0.9833(3) 0.2439(2) 0.0653(14) Uani 1 1 d D . . H04A H 1.469(5) 0.938(3) 0.2132(19) 0.098 Uiso 1 1 d D . . H04B H 1.506(5) 0.952(4) 0.2780(18) 0.098 Uiso 1 1 d D . . O015 O 1.4936(3) 0.9045(3) 0.0479(2) 0.0523(12) Uani 1 1 d D . . H15B H 1.459(4) 0.921(4) 0.017(2) 0.079 Uiso 1 1 d D . . O016 O 0.3090(3) 0.3756(3) 0.3851(2) 0.0575(13) Uani 1 1 d D . . H06A H 0.262(3) 0.383(5) 0.404(3) 0.086 Uiso 1 1 d D . . O017 O 0.5497(3) 0.4673(4) 0.5503(3) 0.0772(15) Uani 1 1 d D . . H17C H 0.500(4) 0.419(4) 0.560(4) 0.116 Uiso 1 1 d D . . H17D H 0.607(3) 0.511(4) 0.556(4) 0.116 Uiso 1 1 d D . . O018 O 0.8113(4) 0.8961(3) 0.3179(3) 0.0780(16) Uani 1 1 d D . . H18A H 0.853(5) 0.902(6) 0.287(3) 0.117 Uiso 1 1 d D . . H18B H 0.800(5) 0.953(3) 0.317(4) 0.117 Uiso 1 1 d D . . O019 O 0.3862(3) 1.1684(4) 0.6681(3) 0.0729(15) Uani 1 1 d D . . H19A H 0.409(5) 1.125(4) 0.654(4) 0.109 Uiso 1 1 d D . . H19B H 0.327(3) 1.130(4) 0.669(4) 0.109 Uiso 1 1 d D . . O020 O 0.9701(3) 1.2141(3) 0.1885(2) 0.0696(14) Uani 1 1 d D . . H20A H 1.028(3) 1.227(5) 0.178(4) 0.104 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0163(4) 0.0189(4) 0.0217(4) -0.0014(3) 0.0004(3) 0.0019(3) Co2 0.0171(4) 0.0179(4) 0.0233(4) -0.0001(3) 0.0019(3) 0.0041(3) N11 0.048(3) 0.019(5) 0.051(4) 0.013(3) 0.027(3) 0.016(3) C12 0.061(5) 0.036(7) 0.093(6) 0.034(5) 0.046(4) 0.025(4) C13 0.074(7) 0.039(6) 0.181(13) 0.018(8) 0.087(8) 0.028(5) C14 0.122(10) 0.044(6) 0.197(14) -0.021(8) 0.124(10) -0.004(6) C15 0.082(6) 0.052(5) 0.079(6) -0.029(5) 0.060(5) -0.027(4) C16 0.056(4) 0.020(4) 0.041(4) -0.005(3) 0.030(4) -0.014(3) N11A 0.048(3) 0.019(5) 0.051(4) 0.013(3) 0.027(3) 0.016(3) C12A 0.061(5) 0.036(7) 0.093(6) 0.034(5) 0.046(4) 0.025(4) C13A 0.074(7) 0.039(6) 0.181(13) 0.018(8) 0.087(8) 0.028(5) C14A 0.122(10) 0.044(6) 0.197(14) -0.021(8) 0.124(10) -0.004(6) C15A 0.082(6) 0.052(5) 0.079(6) -0.029(5) 0.060(5) -0.027(4) C16A 0.056(4) 0.020(4) 0.041(4) -0.005(3) 0.030(4) -0.014(3) C17 0.042(4) 0.024(3) 0.032(4) -0.003(3) 0.005(3) -0.016(3) N18 0.025(3) 0.026(3) 0.021(3) 0.002(2) 0.000(2) -0.002(2) O19 0.040(2) 0.061(3) 0.024(2) 0.003(2) 0.008(2) -0.025(2) C19 0.017(3) 0.047(4) 0.018(3) 0.002(3) -0.008(3) -0.006(3) C110 0.017(3) 0.037(4) 0.016(3) 0.002(3) -0.002(2) 0.009(3) N111 0.018(2) 0.020(2) 0.018(2) -0.008(2) 0.000(2) 0.005(2) C112 0.020(3) 0.026(3) 0.022(3) 0.002(3) -0.006(3) 0.013(3) C113 0.045(4) 0.032(3) 0.025(3) -0.004(3) -0.003(3) 0.029(3) C114 0.047(4) 0.053(4) 0.026(4) -0.001(3) 0.004(3) 0.038(4) C115 0.025(3) 0.052(4) 0.027(3) 0.002(3) 0.008(3) 0.021(3) O116 0.038(2) 0.018(2) 0.037(2) -0.0034(19) -0.001(2) 0.0010(19) C116 0.021(3) 0.015(3) 0.024(3) 0.002(3) -0.006(3) 0.004(2) N117 0.019(2) 0.016(2) 0.024(3) 0.003(2) 0.003(2) 0.003(2) C118 0.022(3) 0.022(3) 0.022(3) 0.005(3) 0.003(3) 0.001(2) C119 0.033(3) 0.012(3) 0.024(3) 0.005(3) 0.005(3) -0.008(3) N120 0.041(3) 0.029(3) 0.032(3) 0.003(2) 0.009(3) -0.001(2) C121 0.054(4) 0.027(4) 0.021(4) -0.001(3) -0.001(3) -0.011(3) C122 0.053(4) 0.029(4) 0.032(4) 0.007(3) -0.011(3) -0.007(3) C123 0.031(3) 0.027(3) 0.047(4) 0.008(3) -0.009(3) -0.006(3) C124 0.031(3) 0.021(3) 0.032(4) 0.001(3) -0.001(3) 0.002(3) N21 0.016(2) 0.026(3) 0.022(3) 0.002(2) 0.004(2) 0.001(2) C22 0.025(3) 0.033(3) 0.031(4) 0.009(3) 0.001(3) 0.008(3) C23 0.023(3) 0.044(4) 0.032(4) 0.005(3) -0.001(3) 0.010(3) C24 0.030(3) 0.029(4) 0.045(4) 0.006(3) -0.010(3) 0.001(3) C25 0.030(3) 0.029(3) 0.034(4) 0.004(3) -0.010(3) 0.000(3) C26 0.024(3) 0.018(3) 0.027(3) 0.005(3) 0.004(3) -0.003(3) C27 0.032(3) 0.025(3) 0.024(3) 0.002(3) 0.002(3) 0.001(3) N28 0.024(2) 0.021(2) 0.019(3) 0.001(2) 0.001(2) 0.003(2) O29 0.047(2) 0.050(3) 0.033(2) -0.004(2) 0.012(2) 0.019(2) C29 0.028(3) 0.026(3) 0.026(4) 0.000(3) 0.009(3) 0.004(3) C210 0.022(3) 0.018(3) 0.033(4) 0.011(3) 0.011(3) 0.006(2) N211 0.023(2) 0.014(2) 0.021(3) 0.004(2) 0.006(2) 0.0058(19) C212 0.022(3) 0.012(3) 0.026(3) 0.003(2) 0.000(3) 0.007(2) C213 0.020(3) 0.027(3) 0.036(4) 0.008(3) -0.004(3) 0.006(3) C214 0.021(3) 0.042(4) 0.048(4) 0.000(3) 0.006(3) 0.015(3) C215 0.027(3) 0.033(3) 0.042(4) 0.003(3) 0.008(3) 0.013(3) O216 0.027(2) 0.024(2) 0.034(2) -0.0054(19) -0.0038(18) 0.0040(18) C216 0.021(3) 0.029(3) 0.022(3) 0.007(3) -0.002(3) 0.015(3) N217 0.025(2) 0.024(3) 0.025(3) 0.005(2) 0.007(2) 0.005(2) C218 0.027(3) 0.041(4) 0.023(3) 0.010(3) 0.001(3) 0.013(3) C219 0.023(3) 0.022(3) 0.022(3) 0.006(3) 0.001(3) 0.000(3) N220 0.026(3) 0.033(3) 0.026(3) 0.010(2) 0.000(2) 0.004(2) C221 0.040(4) 0.034(4) 0.025(4) 0.011(3) -0.001(3) -0.006(3) C222 0.026(3) 0.037(4) 0.034(4) 0.018(3) -0.018(3) -0.008(3) C223 0.023(3) 0.037(4) 0.048(4) 0.020(3) 0.001(3) -0.002(3) C224 0.029(3) 0.034(3) 0.029(4) 0.011(3) 0.003(3) 0.010(3) N31 0.028(3) 0.025(3) 0.033(3) 0.010(2) 0.004(2) 0.008(2) C32 0.032(3) 0.036(4) 0.040(4) 0.014(3) 0.005(3) 0.011(3) C33 0.042(4) 0.038(4) 0.065(5) 0.009(4) 0.012(4) 0.019(3) C34 0.047(4) 0.028(4) 0.067(5) -0.006(4) 0.019(4) 0.014(3) C35 0.038(4) 0.035(4) 0.040(4) 0.002(3) 0.013(3) 0.004(3) C36 0.027(3) 0.016(3) 0.032(4) 0.006(3) 0.008(3) 0.003(3) C37 0.029(3) 0.020(3) 0.029(3) 0.006(3) 0.006(3) 0.007(3) N38 0.020(2) 0.020(2) 0.021(3) 0.002(2) 0.003(2) 0.003(2) O39 0.026(2) 0.032(2) 0.036(2) 0.0115(19) 0.0116(19) -0.0011(18) C39 0.023(3) 0.029(3) 0.019(3) 0.009(3) 0.002(3) 0.008(3) C310 0.016(3) 0.027(3) 0.023(3) 0.008(3) 0.000(2) 0.008(2) N311 0.016(2) 0.021(2) 0.018(2) 0.003(2) 0.002(2) 0.006(2) C312 0.021(3) 0.019(3) 0.022(3) 0.003(3) -0.006(2) 0.007(2) C313 0.034(3) 0.020(3) 0.027(3) 0.001(3) -0.003(3) 0.013(3) C314 0.035(3) 0.031(3) 0.021(3) 0.000(3) -0.001(3) 0.013(3) C315 0.019(3) 0.039(4) 0.022(3) 0.005(3) 0.005(3) 0.014(3) O316 0.027(2) 0.014(2) 0.035(2) 0.0009(18) 0.0006(18) 0.0008(17) C316 0.019(3) 0.024(3) 0.021(3) 0.001(3) -0.001(2) 0.007(3) N317 0.017(2) 0.020(2) 0.022(3) 0.001(2) 0.006(2) 0.001(2) C318 0.026(3) 0.020(3) 0.020(3) 0.004(3) 0.001(3) -0.002(2) C319 0.028(3) 0.024(3) 0.026(4) 0.008(3) 0.004(3) -0.007(3) N320 0.062(4) 0.031(3) 0.028(3) 0.002(3) 0.008(3) -0.001(3) C321 0.081(5) 0.042(4) 0.025(4) 0.006(3) -0.003(4) -0.003(4) C322 0.063(5) 0.045(4) 0.030(4) 0.018(4) -0.029(4) -0.024(4) C323 0.030(4) 0.036(4) 0.051(5) 0.019(4) -0.009(3) -0.010(3) C324 0.028(3) 0.023(3) 0.033(4) 0.014(3) 0.002(3) -0.001(3) N41 0.016(2) 0.015(2) 0.027(3) -0.001(2) -0.001(2) 0.0017(19) C42 0.024(3) 0.028(3) 0.025(3) -0.005(3) -0.002(3) 0.006(3) C43 0.020(3) 0.030(3) 0.043(4) -0.002(3) -0.001(3) 0.007(3) C44 0.032(3) 0.030(3) 0.026(4) -0.001(3) -0.016(3) 0.001(3) C45 0.029(3) 0.030(3) 0.030(4) -0.002(3) -0.008(3) 0.004(3) C46 0.019(3) 0.015(3) 0.027(3) -0.003(3) 0.004(3) -0.001(2) C47 0.030(3) 0.023(3) 0.022(3) 0.000(3) 0.005(3) 0.009(3) N48 0.021(2) 0.017(2) 0.025(3) -0.001(2) -0.001(2) 0.001(2) O49 0.033(2) 0.052(3) 0.039(3) -0.014(2) 0.008(2) 0.017(2) C49 0.023(3) 0.020(3) 0.033(4) 0.005(3) 0.008(3) 0.010(3) C410 0.019(3) 0.020(3) 0.031(4) 0.004(3) 0.005(3) 0.003(2) N411 0.022(2) 0.017(2) 0.029(3) 0.005(2) 0.006(2) 0.008(2) C412 0.020(3) 0.025(3) 0.019(3) 0.010(3) -0.001(3) 0.002(2) C413 0.024(3) 0.030(3) 0.034(4) 0.004(3) -0.007(3) 0.007(3) C414 0.023(3) 0.044(4) 0.040(4) 0.014(3) 0.004(3) 0.012(3) C415 0.024(3) 0.029(3) 0.041(4) 0.005(3) 0.009(3) 0.014(3) O416 0.031(2) 0.024(2) 0.043(3) 0.002(2) 0.0037(19) 0.0028(18) C416 0.017(3) 0.031(4) 0.024(3) 0.012(3) -0.003(3) 0.005(3) N417 0.020(2) 0.022(2) 0.025(3) 0.003(2) 0.000(2) 0.000(2) C418 0.020(3) 0.027(3) 0.032(4) 0.010(3) 0.007(3) 0.005(3) C419 0.011(3) 0.019(3) 0.030(3) 0.008(3) -0.001(3) -0.001(2) N420 0.032(3) 0.031(3) 0.026(3) 0.004(2) 0.004(2) 0.012(2) C421 0.050(4) 0.032(4) 0.023(4) -0.001(3) -0.001(3) 0.011(3) C422 0.026(3) 0.031(3) 0.038(4) 0.012(3) -0.004(3) 0.002(3) C423 0.015(3) 0.032(3) 0.042(4) 0.017(3) -0.001(3) 0.006(3) C424 0.020(3) 0.026(3) 0.027(3) 0.004(3) 0.003(3) 0.001(3) O001 0.036(2) 0.040(3) 0.050(3) -0.004(2) 0.012(2) 0.002(2) O002 0.082(3) 0.080(3) 0.043(3) -0.007(3) 0.017(3) -0.002(3) O003 0.058(3) 0.042(3) 0.050(3) -0.003(3) 0.006(2) 0.023(3) O004 0.043(3) 0.049(3) 0.037(3) -0.013(2) 0.002(2) 0.009(2) O005 0.035(2) 0.050(3) 0.033(3) 0.008(2) 0.010(2) 0.017(2) O006 0.044(2) 0.059(3) 0.038(3) 0.014(2) 0.015(2) 0.013(2) O007 0.082(4) 0.043(3) 0.049(3) -0.001(2) 0.005(3) 0.033(3) O008 0.059(3) 0.054(3) 0.048(3) 0.003(2) 0.007(2) 0.017(2) O009 0.070(3) 0.061(3) 0.041(3) 0.004(3) 0.004(3) 0.017(3) O010 0.048(3) 0.041(3) 0.080(4) 0.009(3) 0.012(3) 0.021(2) O011 0.037(3) 0.066(3) 0.060(3) 0.001(3) -0.001(2) 0.021(3) O012 0.080(4) 0.056(3) 0.061(4) 0.001(3) 0.020(3) 0.004(3) O013 0.085(4) 0.061(4) 0.064(4) 0.007(3) 0.011(3) 0.038(3) O014 0.059(3) 0.084(4) 0.034(3) -0.006(3) 0.014(3) -0.013(3) O015 0.063(3) 0.065(3) 0.041(3) 0.013(2) 0.010(2) 0.035(3) O016 0.047(3) 0.061(3) 0.068(4) 0.018(3) 0.009(3) 0.019(3) O017 0.071(4) 0.078(4) 0.070(4) 0.010(3) -0.004(3) 0.006(3) O018 0.069(4) 0.052(3) 0.098(5) 0.002(3) -0.025(3) 0.009(3) O019 0.065(3) 0.075(4) 0.082(4) 0.009(3) 0.003(3) 0.028(3) O020 0.059(3) 0.071(3) 0.072(4) -0.022(3) 0.019(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N111 1.862(4) . ? Co1 N28 1.877(4) . ? Co1 N21 1.944(4) . ? Co1 N18 1.946(4) . ? Co1 N117 1.962(4) . ? Co1 N211 1.982(4) . ? Co2 N311 1.855(4) . ? Co2 N48 1.873(4) . ? Co2 N41 1.931(4) . ? Co2 N38 1.963(4) . ? Co2 N317 1.976(4) . ? Co2 N411 2.008(4) . ? N11 C12 1.340(8) . ? N11 C16 1.345(8) . ? C12 C13 1.378(11) . ? C12 H12A 0.9500 . ? C13 C14 1.368(14) . ? C13 H13A 0.9500 . ? C14 C15 1.371(13) . ? C14 H14A 0.9500 . ? C15 C16 1.377(9) . ? C15 H15A 0.9500 . ? C16 C17 1.482(9) . ? N11A C12A 1.3900 . ? N11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C12A H12F 0.9500 . ? C13A C14A 1.3900 . ? C13A H13D 0.9500 . ? C14A C15A 1.3900 . ? C14A H14B 0.9500 . ? C15A C16A 1.3900 . ? C15A H15C 0.9500 . ? C16A C17 1.5018 . ? C17 N18 1.463(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N18 C19 1.332(6) . ? O19 C19 1.253(6) . ? C19 C110 1.503(7) . ? C110 N111 1.345(6) . ? C110 C115 1.374(6) . ? N111 C112 1.340(6) . ? C112 C113 1.367(6) . ? C112 C116 1.505(7) . ? C113 C114 1.389(7) . ? C113 H11A 0.9500 . ? C114 C115 1.396(7) . ? C114 H11B 0.9500 . ? C115 H11C 0.9500 . ? O116 C116 1.259(5) . ? C116 N117 1.342(6) . ? N117 C118 1.457(6) . ? C118 C119 1.511(7) . ? C118 H11D 0.9900 . ? C118 H11E 0.9900 . ? C119 N120 1.354(6) . ? C119 C124 1.386(7) . ? N120 C121 1.357(7) . ? C121 C122 1.367(7) . ? C121 H12B 0.9500 . ? C122 C123 1.358(8) . ? C122 H12C 0.9500 . ? C123 C124 1.385(7) . ? C123 H12D 0.9500 . ? C124 H12E 0.9500 . ? N21 C26 1.358(6) . ? N21 C22 1.363(6) . ? C22 C23 1.369(7) . ? C22 H22A 0.9500 . ? C23 C24 1.367(7) . ? C23 H23A 0.9500 . ? C24 C25 1.375(7) . ? C24 H24A 0.9500 . ? C25 C26 1.384(7) . ? C25 H25A 0.9500 . ? C26 C27 1.490(7) . ? C27 N28 1.461(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N28 C29 1.303(6) . ? O29 C29 1.265(6) . ? C29 C210 1.487(7) . ? C210 N211 1.377(6) . ? C210 C215 1.382(6) . ? N211 C212 1.340(6) . ? C212 C213 1.389(6) . ? C212 C216 1.512(7) . ? C213 C214 1.380(7) . ? C213 H21A 0.9500 . ? C214 C215 1.380(7) . ? C214 H21B 0.9500 . ? C215 H21C 0.9500 . ? O216 C216 1.243(6) . ? C216 N217 1.335(6) . ? N217 C218 1.451(6) . ? N217 H21F 0.8800 . ? C218 C219 1.500(7) . ? C218 H21D 0.9900 . ? C218 H21E 0.9900 . ? C219 N220 1.345(6) . ? C219 C224 1.383(6) . ? N220 C221 1.335(6) . ? C221 C222 1.389(7) . ? C221 H22B 0.9500 . ? C222 C223 1.375(7) . ? C222 H22C 0.9500 . ? C223 C224 1.377(7) . ? C223 H22D 0.9500 . ? C224 H22E 0.9500 . ? N31 C36 1.350(6) . ? N31 C32 1.351(6) . ? C32 C33 1.383(7) . ? C32 H32A 0.9500 . ? C33 C34 1.373(8) . ? C33 H33A 0.9500 . ? C34 C35 1.390(7) . ? C34 H34A 0.9500 . ? C35 C36 1.400(7) . ? C35 H35A 0.9500 . ? C36 C37 1.509(6) . ? C37 N38 1.464(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N38 C39 1.314(6) . ? O39 C39 1.262(5) . ? C39 C310 1.513(7) . ? C310 N311 1.348(6) . ? C310 C315 1.381(6) . ? N311 C312 1.341(6) . ? C312 C313 1.383(6) . ? C312 C316 1.508(7) . ? C313 C314 1.394(7) . ? C313 H31A 0.9500 . ? C314 C315 1.378(6) . ? C314 H31B 0.9500 . ? C315 H31C 0.9500 . ? O316 C316 1.244(5) . ? C316 N317 1.337(6) . ? N317 C318 1.450(6) . ? C318 C319 1.506(7) . ? C318 H31D 0.9900 . ? C318 H31E 0.9900 . ? C319 N320 1.367(6) . ? C319 C324 1.370(7) . ? N320 C321 1.366(8) . ? C321 C322 1.353(8) . ? C321 H32B 0.9500 . ? C322 C323 1.378(8) . ? C322 H32C 0.9500 . ? C323 C324 1.385(7) . ? C323 H32D 0.9500 . ? C324 H32E 0.9500 . ? N41 C42 1.349(6) . ? N41 C46 1.357(6) . ? C42 C43 1.383(7) . ? C42 H42A 0.9500 . ? C43 C44 1.382(7) . ? C43 H43A 0.9500 . ? C44 C45 1.369(7) . ? C44 H44A 0.9500 . ? C45 C46 1.381(7) . ? C45 H45A 0.9500 . ? C46 C47 1.503(6) . ? C47 N48 1.448(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N48 C49 1.320(6) . ? O49 C49 1.253(5) . ? C49 C410 1.490(7) . ? C410 N411 1.361(6) . ? C410 C415 1.381(6) . ? N411 C412 1.341(6) . ? C412 C413 1.394(6) . ? C412 C416 1.513(7) . ? C413 C414 1.362(7) . ? C413 H41A 0.9500 . ? C414 C415 1.395(7) . ? C414 H41B 0.9500 . ? C415 H41C 0.9500 . ? O416 C416 1.225(6) . ? C416 N417 1.353(6) . ? N417 C418 1.439(6) . ? N417 H41F 0.8800 . ? C418 C419 1.502(7) . ? C418 H41D 0.9900 . ? C418 H41E 0.9900 . ? C419 N420 1.360(6) . ? C419 C424 1.388(6) . ? N420 C421 1.339(6) . ? C421 C422 1.379(7) . ? C421 H42B 0.9500 . ? C422 C423 1.364(7) . ? C422 H42C 0.9500 . ? C423 C424 1.382(7) . ? C423 H42D 0.9500 . ? C424 H42E 0.9500 . ? O001 H01A 0.883(19) . ? O001 H01B 0.910(19) . ? O002 H02A 0.868(4) . ? O002 H02B 0.856(19) . ? O003 H03A 0.88(2) . ? O003 H03B 0.88(2) . ? O004 H4A 0.89(2) . ? O004 H4B 0.88(2) . ? O005 H05A 0.86(2) . ? O005 H05B 0.860(19) . ? O006 H06C 0.85(2) . ? O007 H07A 0.87(2) . ? O007 H07B 0.89(2) . ? O008 H08A 0.87(2) . ? O009 H09A 0.90(2) . ? O009 H09B 0.88(2) . ? O010 H10A 0.86(2) . ? O010 H10B 0.87(2) . ? O011 H01C 0.89(2) . ? O011 H01D 0.88(2) . ? O012 H02C 0.89(2) . ? O012 H02D 0.87(2) . ? O013 H13B 0.90(2) . ? O013 H13C 0.92(2) . ? O014 H04A 0.887(19) . ? O014 H04B 0.899(19) . ? O015 H15B 0.85(2) . ? O016 H06A 0.86(2) . ? O017 H17C 0.91(2) . ? O017 H17D 0.89(2) . ? O018 H18A 0.92(2) . ? O018 H18B 0.92(2) . ? O019 H19A 0.88(2) . ? O019 H19B 0.89(2) . ? O020 H20A 0.86(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N111 Co1 N28 176.59(18) . . ? N111 Co1 N21 94.19(17) . . ? N28 Co1 N21 82.48(18) . . ? N111 Co1 N18 81.22(18) . . ? N28 Co1 N18 99.51(18) . . ? N21 Co1 N18 90.75(16) . . ? N111 Co1 N117 81.80(17) . . ? N28 Co1 N117 97.50(17) . . ? N21 Co1 N117 91.43(16) . . ? N18 Co1 N117 162.99(17) . . ? N111 Co1 N211 100.42(17) . . ? N28 Co1 N211 82.88(17) . . ? N21 Co1 N211 165.24(17) . . ? N18 Co1 N211 93.52(16) . . ? N117 Co1 N211 88.61(16) . . ? N311 Co2 N48 177.64(18) . . ? N311 Co2 N41 95.10(16) . . ? N48 Co2 N41 83.19(17) . . ? N311 Co2 N38 81.97(17) . . ? N48 Co2 N38 99.62(17) . . ? N41 Co2 N38 89.70(16) . . ? N311 Co2 N317 81.54(17) . . ? N48 Co2 N317 96.84(17) . . ? N41 Co2 N317 90.80(16) . . ? N38 Co2 N317 163.48(16) . . ? N311 Co2 N411 98.92(17) . . ? N48 Co2 N411 82.73(17) . . ? N41 Co2 N411 165.79(17) . . ? N38 Co2 N411 94.47(16) . . ? N317 Co2 N411 89.05(16) . . ? C12 N11 C16 118.5(6) . . ? N11 C12 C13 123.1(9) . . ? N11 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C14 C13 C12 117.9(11) . . ? C14 C13 H13A 121.1 . . ? C12 C13 H13A 121.1 . . ? C13 C14 C15 119.6(11) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C14 C15 C16 119.9(10) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? N11 C16 C15 120.9(8) . . ? N11 C16 C17 118.9(6) . . ? C15 C16 C17 120.1(8) . . ? C12A N11A C16A 120.0 . . ? N11A C12A C13A 120.0 . . ? N11A C12A H12F 120.0 . . ? C13A C12A H12F 120.0 . . ? C14A C13A C12A 120.0 . . ? C14A C13A H13D 120.0 . . ? C12A C13A H13D 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14B 120.0 . . ? C15A C14A H14B 120.0 . . ? C16A C15A C14A 120.00(8) . . ? C16A C15A H15C 120.0 . . ? C14A C15A H15C 120.0 . . ? C15A C16A N11A 120.0 . . ? C15A C16A C17 118.9 . . ? N11A C16A C17 121.0 . . ? N18 C17 C16 113.7(5) . . ? N18 C17 C16A 118(2) . . ? C16 C17 C16A 5(3) . . ? N18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C16A C17 H17A 104.5 . . ? N18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? C16A C17 H17B 108.4 . . ? H17A C17 H17B 107.7 . . ? C19 N18 C17 117.6(5) . . ? C19 N18 Co1 116.7(4) . . ? C17 N18 Co1 125.6(4) . . ? O19 C19 N18 128.5(5) . . ? O19 C19 C110 120.3(5) . . ? N18 C19 C110 111.1(5) . . ? N111 C110 C115 119.9(5) . . ? N111 C110 C19 111.7(4) . . ? C115 C110 C19 128.4(5) . . ? C112 N111 C110 122.1(4) . . ? C112 N111 Co1 118.8(3) . . ? C110 N111 Co1 118.7(3) . . ? N111 C112 C113 120.6(5) . . ? N111 C112 C116 112.0(4) . . ? C113 C112 C116 127.3(5) . . ? C112 C113 C114 118.6(5) . . ? C112 C113 H11A 120.7 . . ? C114 C113 H11A 120.7 . . ? C113 C114 C115 120.0(5) . . ? C113 C114 H11B 120.0 . . ? C115 C114 H11B 120.0 . . ? C110 C115 C114 118.7(5) . . ? C110 C115 H11C 120.7 . . ? C114 C115 H11C 120.7 . . ? O116 C116 N117 126.2(5) . . ? O116 C116 C112 122.1(5) . . ? N117 C116 C112 111.7(4) . . ? C116 N117 C118 117.3(4) . . ? C116 N117 Co1 115.5(3) . . ? C118 N117 Co1 127.1(3) . . ? N117 C118 C119 111.9(4) . . ? N117 C118 H11D 109.2 . . ? C119 C118 H11D 109.2 . . ? N117 C118 H11E 109.2 . . ? C119 C118 H11E 109.2 . . ? H11D C118 H11E 107.9 . . ? N120 C119 C124 121.9(5) . . ? N120 C119 C118 116.6(5) . . ? C124 C119 C118 121.4(5) . . ? C119 N120 C121 117.2(5) . . ? N120 C121 C122 123.1(6) . . ? N120 C121 H12B 118.5 . . ? C122 C121 H12B 118.5 . . ? C123 C122 C121 119.5(6) . . ? C123 C122 H12C 120.3 . . ? C121 C122 H12C 120.3 . . ? C122 C123 C124 119.2(6) . . ? C122 C123 H12D 120.4 . . ? C124 C123 H12D 120.4 . . ? C123 C124 C119 119.1(6) . . ? C123 C124 H12E 120.5 . . ? C119 C124 H12E 120.5 . . ? C26 N21 C22 118.1(4) . . ? C26 N21 Co1 115.8(3) . . ? C22 N21 Co1 126.1(4) . . ? N21 C22 C23 122.3(5) . . ? N21 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C24 C23 C22 119.2(5) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 119.7(6) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 119.6(6) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? N21 C26 C25 121.1(5) . . ? N21 C26 C27 115.7(5) . . ? C25 C26 C27 123.2(5) . . ? N28 C27 C26 107.3(4) . . ? N28 C27 H27A 110.3 . . ? C26 C27 H27A 110.3 . . ? N28 C27 H27B 110.3 . . ? C26 C27 H27B 110.3 . . ? H27A C27 H27B 108.5 . . ? C29 N28 C27 121.6(4) . . ? C29 N28 Co1 119.1(4) . . ? C27 N28 Co1 118.6(3) . . ? O29 C29 N28 127.9(5) . . ? O29 C29 C210 121.0(5) . . ? N28 C29 C210 111.1(5) . . ? N211 C210 C215 121.7(5) . . ? N211 C210 C29 115.8(4) . . ? C215 C210 C29 122.4(5) . . ? C212 N211 C210 117.7(4) . . ? C212 N211 Co1 132.3(3) . . ? C210 N211 Co1 109.9(3) . . ? N211 C212 C213 122.5(5) . . ? N211 C212 C216 122.1(4) . . ? C213 C212 C216 115.2(5) . . ? C214 C213 C212 119.6(5) . . ? C214 C213 H21A 120.2 . . ? C212 C213 H21A 120.2 . . ? C213 C214 C215 118.7(5) . . ? C213 C214 H21B 120.7 . . ? C215 C214 H21B 120.7 . . ? C214 C215 C210 119.7(5) . . ? C214 C215 H21C 120.1 . . ? C210 C215 H21C 120.1 . . ? O216 C216 N217 124.0(5) . . ? O216 C216 C212 122.1(5) . . ? N217 C216 C212 113.6(4) . . ? C216 N217 C218 122.0(4) . . ? C216 N217 H21F 119.0 . . ? C218 N217 H21F 119.0 . . ? N217 C218 C219 114.3(4) . . ? N217 C218 H21D 108.7 . . ? C219 C218 H21D 108.7 . . ? N217 C218 H21E 108.7 . . ? C219 C218 H21E 108.7 . . ? H21D C218 H21E 107.6 . . ? N220 C219 C224 122.2(5) . . ? N220 C219 C218 113.9(4) . . ? C224 C219 C218 123.8(5) . . ? C221 N220 C219 117.7(5) . . ? N220 C221 C222 123.1(6) . . ? N220 C221 H22B 118.4 . . ? C222 C221 H22B 118.4 . . ? C223 C222 C221 118.8(5) . . ? C223 C222 H22C 120.6 . . ? C221 C222 H22C 120.6 . . ? C222 C223 C224 118.6(5) . . ? C222 C223 H22D 120.7 . . ? C224 C223 H22D 120.7 . . ? C223 C224 C219 119.7(6) . . ? C223 C224 H22E 120.2 . . ? C219 C224 H22E 120.2 . . ? C36 N31 C32 116.6(5) . . ? N31 C32 C33 124.5(6) . . ? N31 C32 H32A 117.7 . . ? C33 C32 H32A 117.7 . . ? C34 C33 C32 117.9(6) . . ? C34 C33 H33A 121.1 . . ? C32 C33 H33A 121.1 . . ? C33 C34 C35 119.8(6) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C34 C35 C36 118.5(6) . . ? C34 C35 H35A 120.8 . . ? C36 C35 H35A 120.8 . . ? N31 C36 C35 122.7(5) . . ? N31 C36 C37 117.6(5) . . ? C35 C36 C37 119.7(5) . . ? N38 C37 C36 112.8(4) . . ? N38 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? N38 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C39 N38 C37 119.2(4) . . ? C39 N38 Co2 115.6(3) . . ? C37 N38 Co2 125.0(3) . . ? O39 C39 N38 128.3(5) . . ? O39 C39 C310 119.9(5) . . ? N38 C39 C310 111.9(4) . . ? N311 C310 C315 119.1(5) . . ? N311 C310 C39 111.8(4) . . ? C315 C310 C39 129.0(5) . . ? C312 N311 C310 122.8(4) . . ? C312 N311 Co2 119.0(3) . . ? C310 N311 Co2 118.1(3) . . ? N311 C312 C313 119.8(5) . . ? N311 C312 C316 112.4(4) . . ? C313 C312 C316 127.8(5) . . ? C312 C313 C314 118.7(5) . . ? C312 C313 H31A 120.7 . . ? C314 C313 H31A 120.7 . . ? C315 C314 C313 120.0(5) . . ? C315 C314 H31B 120.0 . . ? C313 C314 H31B 120.0 . . ? C314 C315 C310 119.6(5) . . ? C314 C315 H31C 120.2 . . ? C310 C315 H31C 120.2 . . ? O316 C316 N317 127.6(5) . . ? O316 C316 C312 121.1(4) . . ? N317 C316 C312 111.2(4) . . ? C316 N317 C318 116.9(4) . . ? C316 N317 Co2 115.7(3) . . ? C318 N317 Co2 127.4(3) . . ? N317 C318 C319 113.6(4) . . ? N317 C318 H31D 108.8 . . ? C319 C318 H31D 108.8 . . ? N317 C318 H31E 108.8 . . ? C319 C318 H31E 108.8 . . ? H31D C318 H31E 107.7 . . ? N320 C319 C324 122.7(5) . . ? N320 C319 C318 114.8(5) . . ? C324 C319 C318 122.4(5) . . ? C321 N320 C319 115.8(6) . . ? C322 C321 N320 124.4(7) . . ? C322 C321 H32B 117.8 . . ? N320 C321 H32B 117.8 . . ? C321 C322 C323 118.7(6) . . ? C321 C322 H32C 120.7 . . ? C323 C322 H32C 120.7 . . ? C322 C323 C324 119.2(6) . . ? C322 C323 H32D 120.4 . . ? C324 C323 H32D 120.4 . . ? C319 C324 C323 119.3(6) . . ? C319 C324 H32E 120.4 . . ? C323 C324 H32E 120.4 . . ? C42 N41 C46 117.6(4) . . ? C42 N41 Co2 126.6(4) . . ? C46 N41 Co2 115.8(3) . . ? N41 C42 C43 122.5(5) . . ? N41 C42 H42A 118.7 . . ? C43 C42 H42A 118.7 . . ? C44 C43 C42 119.3(5) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C45 C44 C43 118.5(5) . . ? C45 C44 H44A 120.8 . . ? C43 C44 H44A 120.8 . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? N41 C46 C45 121.8(5) . . ? N41 C46 C47 114.9(4) . . ? C45 C46 C47 123.2(5) . . ? N48 C47 C46 107.9(4) . . ? N48 C47 H47A 110.1 . . ? C46 C47 H47A 110.1 . . ? N48 C47 H47B 110.1 . . ? C46 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C49 N48 C47 122.1(4) . . ? C49 N48 Co2 118.6(4) . . ? C47 N48 Co2 118.1(3) . . ? O49 C49 N48 127.6(5) . . ? O49 C49 C410 121.0(5) . . ? N48 C49 C410 111.4(4) . . ? N411 C410 C415 123.2(5) . . ? N411 C410 C49 115.9(4) . . ? C415 C410 C49 120.9(5) . . ? C412 N411 C410 117.6(4) . . ? C412 N411 Co2 132.5(3) . . ? C410 N411 Co2 109.8(3) . . ? N411 C412 C413 121.9(5) . . ? N411 C412 C416 123.0(4) . . ? C413 C412 C416 114.7(5) . . ? C414 C413 C412 120.0(5) . . ? C414 C413 H41A 120.0 . . ? C412 C413 H41A 120.0 . . ? C413 C414 C415 119.0(5) . . ? C413 C414 H41B 120.5 . . ? C415 C414 H41B 120.5 . . ? C410 C415 C414 118.2(5) . . ? C410 C415 H41C 120.9 . . ? C414 C415 H41C 120.9 . . ? O416 C416 N417 125.3(5) . . ? O416 C416 C412 122.4(5) . . ? N417 C416 C412 111.8(5) . . ? C416 N417 C418 120.7(4) . . ? C416 N417 H41F 119.6 . . ? C418 N417 H41F 119.6 . . ? N417 C418 C419 114.9(4) . . ? N417 C418 H41D 108.5 . . ? C419 C418 H41D 108.5 . . ? N417 C418 H41E 108.5 . . ? C419 C418 H41E 108.5 . . ? H41D C418 H41E 107.5 . . ? N420 C419 C424 122.0(5) . . ? N420 C419 C418 115.5(4) . . ? C424 C419 C418 122.5(5) . . ? C421 N420 C419 117.0(4) . . ? N420 C421 C422 123.9(6) . . ? N420 C421 H42B 118.0 . . ? C422 C421 H42B 118.0 . . ? C423 C422 C421 118.6(5) . . ? C423 C422 H42C 120.7 . . ? C421 C422 H42C 120.7 . . ? C422 C423 C424 119.5(5) . . ? C422 C423 H42D 120.2 . . ? C424 C423 H42D 120.2 . . ? C423 C424 C419 119.0(5) . . ? C423 C424 H42E 120.5 . . ? C419 C424 H42E 120.5 . . ? H01A O001 H01B 83(5) . . ? H02A O002 H02B 114(3) . . ? H03A O003 H03B 106(6) . . ? H4A O004 H4B 90(5) . . ? H05A O005 H05B 102(5) . . ? H07A O007 H07B 93(6) . . ? H09A O009 H09B 166(6) . . ? H10A O010 H10B 131(6) . . ? H01C O011 H01D 85(6) . . ? H02C O012 H02D 92(7) . . ? H13B O013 H13C 138(6) . . ? H04A O014 H04B 103(3) . . ? H17C O017 H17D 158(7) . . ? H18A O018 H18B 101(7) . . ? H19A O019 H19B 95(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N217 H21F N11 0.88 2.03 2.895(12) 168.8 . N417 H41F N31 0.88 2.06 2.924(6) 166.3 . O003 H03B O116 0.88(2) 1.88(2) 2.763(5) 177(6) . O004 H4A O49 0.89(2) 1.83(3) 2.693(5) 162(6) . O005 H05B N220 0.860(19) 1.96(2) 2.809(5) 170(5) . O006 H06C O39 0.85(2) 2.04(4) 2.808(5) 150(6) . O011 H01D N420 0.88(2) 2.02(3) 2.846(6) 156(6) . O014 H04B O19 0.899(19) 2.11(5) 2.787(6) 132(6) . O003 H03A O008 0.88(2) 2.01(2) 2.886(6) 176(6) . O004 H4B O009 0.88(2) 2.24(5) 2.890(6) 130(5) . O005 H05A O015 0.86(2) 1.93(2) 2.779(6) 169(5) . O007 H07A O316 0.87(2) 1.88(2) 2.740(5) 170(7) . O008 H08A O003 0.87(2) 2.42(6) 2.886(6) 114(5) . O009 H09B O004 0.88(2) 2.09(4) 2.890(6) 151(6) . O012 H02D O014 0.87(2) 1.92(2) 2.788(6) 176(7) . O013 H13C O015 0.92(2) 2.18(5) 2.908(7) 136(6) . O014 H04A O005 0.887(19) 1.92(2) 2.806(6) 172(7) . O014 H04B O19 0.899(19) 2.11(5) 2.787(6) 132(6) . O018 H18B O002 0.92(2) 2.64(5) 3.421(7) 144(6) . O002 H02A O020 0.868(4) 2.026(4) 2.895(6) 178.8(4) . O001 H01A O216 0.883(19) 2.04(2) 2.919(5) 179(6) 2_665 O010 H10B O005 0.87(2) 1.93(3) 2.770(6) 164(7) 1_455 O016 H06A O003 0.86(2) 2.04(4) 2.796(6) 147(6) 1_455 O020 H20A N320 0.86(2) 2.19(4) 2.968(6) 150(7) 2_765 O019 H19B O018 0.89(2) 1.97(4) 2.797(7) 153(7) 2_676 O010 H10A O39 0.86(2) 2.05(2) 2.891(5) 167(6) 1_565 O018 H18A O416 0.92(2) 2.31(6) 3.014(7) 133(7) 1_565 O001 H01B O004 0.910(19) 1.96(4) 2.756(6) 145(5) 1_465 O019 H19A O19 0.88(2) 2.50(4) 3.318(6) 155(7) 2_776 O002 H02B O29 0.856(19) 1.997(19) 2.845(6) 170(6) 2_776 O018 H18B O29 0.92(2) 2.27(6) 2.981(6) 134(7) 2_776 O009 H09A O016 0.90(2) 1.92(4) 2.734(6) 150(6) 2_655 O011 H01C O019 0.89(2) 2.03(4) 2.835(7) 149(6) 2_666 O017 H17D O016 0.89(2) 2.07(5) 2.837(7) 145(7) 2_666 O013 H13B O007 0.90(2) 2.16(6) 2.797(7) 127(6) 1_665 O015 H15B O013 0.85(2) 2.12(3) 2.936(7) 161(6) 2_875 O017 H17C O011 0.91(2) 2.05(5) 2.859(7) 147(7) 2_656 O007 H07B O020 0.89(2) 2.00(2) 2.881(7) 170(6) 1_545 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.803 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.081 data_nihela _database_code_depnum_ccdc_archive 'CCDC 246449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.75 H46 N10 Ni3 O11.75' _chemical_formula_weight 1148.10 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' Ni Ni 0.3393 1.1124 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.9970(9) _cell_length_b 22.7871(9) _cell_length_c 21.3414(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.4170(10) _cell_angle_gamma 90.00 _cell_volume 10687.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5927 _cell_measurement_theta_min 3 _cell_measurement_theta_max 15 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4740 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 48984 _diffrn_reflns_av_R_equivalents 0.1169 _diffrn_reflns_av_sigmaI/netI 0.1525 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.00 _reflns_number_total 16688 _reflns_number_gt 8237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0940P)^2^+2.6700P] 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 16688 _refine_ls_number_parameters 1379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1720 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.1647 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 Ni11 Ni 0.11466(5) 0.47490(5) 0.68823(5) 0.0400(3) Uani 1 1 d . . . Ni12 Ni 0.04284(5) 0.40373(5) 0.78008(5) 0.0316(3) Uani 1 1 d . . . Ni13 Ni -0.02825(5) 0.33059(5) 0.86911(5) 0.0377(3) Uani 1 1 d . . . N11 N 0.1239(3) 0.5411(3) 0.7532(4) 0.051(2) Uani 1 1 d . . . C12 C 0.1066(4) 0.5981(5) 0.7431(6) 0.066(3) Uani 1 1 d . . . H12A H 0.0872 0.6095 0.7044 0.079 Uiso 1 1 calc R . . C13 C 0.1182(5) 0.6403(5) 0.7918(7) 0.075(4) Uani 1 1 d . . . H13A H 0.1059 0.6800 0.7860 0.090 Uiso 1 1 calc R . . C14 C 0.1461(5) 0.6237(6) 0.8449(7) 0.081(4) Uani 1 1 d . . . H14A H 0.1556 0.6521 0.8764 0.097 Uiso 1 1 calc R . . C15 C 0.1612(4) 0.5674(5) 0.8549(5) 0.067(3) Uani 1 1 d . . . H15A H 0.1786 0.5559 0.8945 0.080 Uiso 1 1 calc R . . C16 C 0.1516(4) 0.5257(5) 0.8082(5) 0.053(3) Uani 1 1 d . . . C17 C 0.1729(4) 0.4636(4) 0.8132(4) 0.047(3) Uani 1 1 d . . . H17A H 0.2163 0.4619 0.8028 0.056 Uiso 1 1 calc R . . H17B H 0.1699 0.4504 0.8572 0.056 Uiso 1 1 calc R . . N18 N 0.1382(3) 0.4230(3) 0.7720(3) 0.0367(18) Uani 1 1 d . . . C19 C 0.1694(4) 0.3720(4) 0.7650(4) 0.041(2) Uani 1 1 d . . . O110 O 0.2223(3) 0.3615(3) 0.7821(3) 0.0595(19) Uani 1 1 d . . . C111 C 0.1311(4) 0.3241(4) 0.7352(4) 0.038(2) Uani 1 1 d . . . N112 N 0.0716(4) 0.3310(3) 0.7417(3) 0.0366(18) Uani 1 1 d . . . C113 C 0.0303(4) 0.2905(4) 0.7227(4) 0.038(2) Uani 1 1 d . . . C114 C 0.0495(5) 0.2404(4) 0.6928(4) 0.045(3) Uani 1 1 d . . . H11A H 0.0210 0.2117 0.6784 0.054 Uiso 1 1 calc R . . C115 C 0.1102(5) 0.2329(4) 0.6841(4) 0.054(3) Uani 1 1 d . . . H11B H 0.1232 0.1989 0.6628 0.065 Uiso 1 1 calc R . . C116 C 0.1534(5) 0.2732(4) 0.7054(4) 0.051(3) Uani 1 1 d . . . H11C H 0.1956 0.2671 0.7004 0.062 Uiso 1 1 calc R . . C117 C -0.0340(4) 0.3082(4) 0.7292(4) 0.039(2) Uani 1 1 d . . . O118 O -0.0742(3) 0.2822(3) 0.6975(3) 0.0546(18) Uani 1 1 d . . . N119 N -0.0407(3) 0.3533(3) 0.7698(3) 0.0322(17) Uani 1 1 d . . . C120 C -0.1024(4) 0.3778(4) 0.7648(4) 0.038(2) Uani 1 1 d . . . H12B H -0.1318 0.3452 0.7584 0.045 Uiso 1 1 calc R . . H12C H -0.1058 0.4033 0.7273 0.045 Uiso 1 1 calc R . . C121 C -0.1198(4) 0.4128(4) 0.8210(4) 0.038(2) Uani 1 1 d . . . N122 N -0.0901(3) 0.3973(3) 0.8754(3) 0.0370(18) Uani 1 1 d . . . C123 C -0.1055(4) 0.4254(4) 0.9276(4) 0.047(3) Uani 1 1 d . . . H12D H -0.0849 0.4151 0.9660 0.056 Uiso 1 1 calc R . . C124 C -0.1491(4) 0.4680(4) 0.9290(5) 0.056(3) Uani 1 1 d . . . H12E H -0.1588 0.4867 0.9671 0.067 Uiso 1 1 calc R . . C125 C -0.1784(4) 0.4828(4) 0.8728(5) 0.058(3) Uani 1 1 d . . . H12F H -0.2091 0.5121 0.8715 0.070 Uiso 1 1 calc R . . C126 C -0.1630(4) 0.4552(4) 0.8194(5) 0.048(2) Uani 1 1 d . . . H12G H -0.1827 0.4657 0.7805 0.058 Uiso 1 1 calc R . . C131 C 0.2934(5) 0.5080(5) 0.6239(5) 0.070(3) Uani 1 1 d . . . H13B H 0.3102 0.4792 0.6541 0.106 Uiso 1 1 calc R . . H13C H 0.3120 0.5464 0.6323 0.106 Uiso 1 1 calc R . . H13D H 0.3022 0.4955 0.5813 0.106 Uiso 1 1 calc R . . C132 C 0.2253(4) 0.5122(4) 0.6300(5) 0.049(3) Uani 1 1 d . . . O133 O 0.2043(3) 0.4810(3) 0.6724(3) 0.0501(17) Uani 1 1 d . . . C134 C 0.1920(5) 0.5498(4) 0.5903(5) 0.060(3) Uani 1 1 d . . . H13E H 0.2146 0.5737 0.5632 0.072 Uiso 1 1 calc R . . C135 C 0.1282(6) 0.5560(4) 0.5861(5) 0.061(3) Uani 1 1 d . . . O136 O 0.0915(3) 0.5320(3) 0.6209(3) 0.0573(19) Uani 1 1 d . . . C137 C 0.1001(6) 0.5959(5) 0.5352(5) 0.091(4) Uani 1 1 d . . . H13F H 0.0556 0.5948 0.5368 0.137 Uiso 1 1 calc R . . H13G H 0.1122 0.5824 0.4939 0.137 Uiso 1 1 calc R . . H13H H 0.1144 0.6362 0.5421 0.137 Uiso 1 1 calc R . . N21 N 0.1012(3) 0.4085(3) 0.6224(3) 0.0377(18) Uani 1 1 d . . . C22 C 0.1458(4) 0.3790(4) 0.5953(4) 0.042(2) Uani 1 1 d . . . H22A H 0.1869 0.3865 0.6081 0.051 Uiso 1 1 calc R . . C23 C 0.1328(4) 0.3380(4) 0.5490(4) 0.047(2) Uani 1 1 d . . . H23A H 0.1648 0.3192 0.5283 0.057 Uiso 1 1 calc R . . C24 C 0.0728(5) 0.3246(4) 0.5330(4) 0.056(3) Uani 1 1 d . . . H24A H 0.0631 0.2955 0.5024 0.067 Uiso 1 1 calc R . . C25 C 0.0274(4) 0.3543(4) 0.5624(4) 0.044(2) Uani 1 1 d . . . H25A H -0.0141 0.3457 0.5525 0.052 Uiso 1 1 calc R . . C26 C 0.0431(4) 0.3965(4) 0.6064(4) 0.033(2) Uani 1 1 d . . . C27 C -0.0037(4) 0.4343(4) 0.6358(4) 0.036(2) Uani 1 1 d . . . H27A H -0.0134 0.4679 0.6076 0.043 Uiso 1 1 calc R . . H27B H -0.0415 0.4112 0.6398 0.043 Uiso 1 1 calc R . . N28 N 0.0161(3) 0.4570(3) 0.6981(3) 0.0343(17) Uani 1 1 d . . . C29 C -0.0201(4) 0.5010(4) 0.7169(4) 0.038(2) Uani 1 1 d . . . O210 O -0.0625(3) 0.5260(3) 0.6854(3) 0.0436(16) Uani 1 1 d . . . C211 C -0.0121(4) 0.5177(4) 0.7846(4) 0.033(2) Uani 1 1 d . . . N212 N 0.0151(3) 0.4767(3) 0.8199(3) 0.0296(16) Uani 1 1 d . . . C213 C 0.0232(4) 0.4814(4) 0.8831(4) 0.034(2) Uani 1 1 d . . . C214 C 0.0034(4) 0.5316(4) 0.9118(4) 0.048(3) Uani 1 1 d . . . H21A H 0.0104 0.5370 0.9556 0.058 Uiso 1 1 calc R . . C215 C -0.0270(4) 0.5742(4) 0.8761(5) 0.048(3) Uani 1 1 d . . . H21B H -0.0426 0.6081 0.8958 0.058 Uiso 1 1 calc R . . C216 C -0.0348(4) 0.5673(4) 0.8109(4) 0.040(2) Uani 1 1 d . . . H21C H -0.0551 0.5963 0.7858 0.048 Uiso 1 1 calc R . . C217 C 0.0564(4) 0.4307(4) 0.9130(4) 0.037(2) Uani 1 1 d . . . O218 O 0.0830(3) 0.4415(3) 0.9651(3) 0.0521(18) Uani 1 1 d . . . N219 N 0.0569(3) 0.3818(3) 0.8797(3) 0.0330(17) Uani 1 1 d . . . C220 C 0.1018(4) 0.3404(4) 0.9051(4) 0.040(2) Uani 1 1 d . . . H22B H 0.1009 0.3411 0.9515 0.048 Uiso 1 1 calc R . . H22C H 0.1427 0.3534 0.8934 0.048 Uiso 1 1 calc R . . C221 C 0.0922(4) 0.2789(4) 0.8832(3) 0.035(2) Uani 1 1 d . . . N222 N 0.0356(4) 0.2645(3) 0.8649(3) 0.0395(19) Uani 1 1 d . . . C223 C 0.0229(5) 0.2079(4) 0.8505(4) 0.049(3) Uani 1 1 d . . . H22D H -0.0176 0.1974 0.8377 0.059 Uiso 1 1 calc R . . C224 C 0.0681(6) 0.1641(5) 0.8540(4) 0.059(3) Uani 1 1 d . . . H22E H 0.0589 0.1244 0.8439 0.071 Uiso 1 1 calc R . . C225 C 0.1256(6) 0.1809(5) 0.8723(4) 0.066(3) Uani 1 1 d . . . H22F H 0.1572 0.1526 0.8753 0.079 Uiso 1 1 calc R . . C226 C 0.1377(5) 0.2375(5) 0.8862(4) 0.049(3) Uani 1 1 d . . . H22G H 0.1780 0.2490 0.8983 0.059 Uiso 1 1 calc R . . C231 C -0.1845(5) 0.2195(5) 0.8785(5) 0.084(4) Uani 1 1 d . . . H23B H -0.1902 0.2205 0.8327 0.126 Uiso 1 1 calc R . . H23C H -0.2202 0.2367 0.8975 0.126 Uiso 1 1 calc R . . H23D H -0.1796 0.1788 0.8925 0.126 Uiso 1 1 calc R . . C232 C -0.1282(5) 0.2545(4) 0.8984(5) 0.056(3) Uani 1 1 d . . . O233 O -0.0979(3) 0.2745(3) 0.8553(3) 0.0507(17) Uani 1 1 d . . . C234 C -0.1126(5) 0.2587(4) 0.9632(5) 0.060(3) Uani 1 1 d . . . H23E H -0.1387 0.2392 0.9909 0.072 Uiso 1 1 calc R . . C235 C -0.0631(6) 0.2883(5) 0.9906(4) 0.056(3) Uani 1 1 d . . . O236 O -0.0248(3) 0.3186(3) 0.9620(3) 0.0515(17) Uani 1 1 d . . . C237 C -0.0529(5) 0.2864(5) 1.0608(4) 0.078(4) Uani 1 1 d . . . H23F H -0.0169 0.3098 1.0730 0.117 Uiso 1 1 calc R . . H23G H -0.0466 0.2457 1.0743 0.117 Uiso 1 1 calc R . . H23H H -0.0886 0.3026 1.0807 0.117 Uiso 1 1 calc R . . Ni21 Ni 0.62629(5) 0.65734(5) 0.72218(5) 0.0369(3) Uani 1 1 d . . . Ni22 Ni 0.52539(5) 0.72505(5) 0.78100(5) 0.0357(3) Uani 1 1 d . . . Ni23 Ni 0.42160(5) 0.79125(5) 0.83796(6) 0.0439(3) Uani 1 1 d . . . N31 N 0.6150(3) 0.5878(3) 0.7820(4) 0.0410(19) Uani 1 1 d . . . C32 C 0.6070(4) 0.5314(4) 0.7649(5) 0.045(2) Uani 1 1 d . . . H32A H 0.6028 0.5229 0.7214 0.055 Uiso 1 1 calc R . . C33 C 0.6045(4) 0.4850(4) 0.8064(6) 0.061(3) Uani 1 1 d . . . H33A H 0.5991 0.4457 0.7924 0.073 Uiso 1 1 calc R . . C34 C 0.6102(5) 0.4988(5) 0.8687(6) 0.078(4) Uani 1 1 d . . . H34A H 0.6081 0.4687 0.8994 0.093 Uiso 1 1 calc R . . C35 C 0.6191(5) 0.5572(5) 0.8873(5) 0.061(3) Uani 1 1 d . . . H35A H 0.6231 0.5666 0.9306 0.073 Uiso 1 1 calc R . . C36 C 0.6220(4) 0.6003(4) 0.8439(4) 0.041(2) Uani 1 1 d . . . C37 C 0.6375(4) 0.6616(4) 0.8604(4) 0.038(2) Uani 1 1 d . . . H37A H 0.6184 0.6714 0.9003 0.046 Uiso 1 1 calc R . . H37B H 0.6822 0.6644 0.8679 0.046 Uiso 1 1 calc R . . N38 N 0.6188(3) 0.7050(3) 0.8137(3) 0.0358(18) Uani 1 1 d . . . C39 C 0.6507(4) 0.7558(4) 0.8218(4) 0.037(2) Uani 1 1 d . . . O310 O 0.6956(3) 0.7638(3) 0.8572(3) 0.0485(17) Uani 1 1 d . . . C311 C 0.6237(4) 0.8070(4) 0.7851(4) 0.035(2) Uani 1 1 d . . . N312 N 0.5664(3) 0.7989(3) 0.7638(3) 0.0330(17) Uani 1 1 d . . . C313 C 0.5365(4) 0.8409(4) 0.7326(4) 0.039(2) Uani 1 1 d . . . C314 C 0.5638(5) 0.8955(4) 0.7221(4) 0.049(3) Uani 1 1 d . . . H31A H 0.5422 0.9256 0.6999 0.059 Uiso 1 1 calc R . . C315 C 0.6227(5) 0.9043(4) 0.7447(5) 0.055(3) Uani 1 1 d . . . H31B H 0.6424 0.9406 0.7375 0.066 Uiso 1 1 calc R . . C316 C 0.6531(4) 0.8605(4) 0.7778(4) 0.041(2) Uani 1 1 d . . . H31C H 0.6931 0.8666 0.7951 0.050 Uiso 1 1 calc R . . C317 C 0.4737(4) 0.8251(4) 0.7107(4) 0.042(2) Uani 1 1 d . . . O318 O 0.4487(3) 0.8522(3) 0.6649(3) 0.063(2) Uani 1 1 d . . . N319 N 0.4504(3) 0.7788(3) 0.7397(3) 0.0431(19) Uani 1 1 d . . . C320 C 0.3954(4) 0.7554(4) 0.7064(5) 0.058(3) Uani 1 1 d . . . H32B H 0.4073 0.7350 0.6679 0.069 Uiso 1 1 calc R . . H32C H 0.3683 0.7884 0.6937 0.069 Uiso 1 1 calc R . . C321 C 0.3613(4) 0.7135(4) 0.7464(6) 0.057(3) Uani 1 1 d . . . N322 N 0.3672(3) 0.7222(3) 0.8101(5) 0.057(2) Uani 1 1 d . . . C323 C 0.3368(5) 0.6872(5) 0.8484(6) 0.072(4) Uani 1 1 d . . . H32D H 0.3414 0.6934 0.8924 0.087 Uiso 1 1 calc R . . C324 C 0.2992(5) 0.6427(6) 0.8266(8) 0.092(4) Uani 1 1 d . . . H32E H 0.2788 0.6183 0.8550 0.110 Uiso 1 1 calc R . . C325 C 0.2919(5) 0.6343(6) 0.7625(9) 0.095(5) Uani 1 1 d . . . H32F H 0.2655 0.6043 0.7467 0.114 Uiso 1 1 calc R . . C326 C 0.3229(5) 0.6697(5) 0.7207(7) 0.083(4) Uani 1 1 d . . . H32G H 0.3181 0.6643 0.6766 0.100 Uiso 1 1 calc R . . C331 C 0.3384(8) 0.8202(8) 1.0138(8) 0.205(12) Uani 1 1 d . . . H33B H 0.3669 0.7918 1.0331 0.307 Uiso 1 1 calc R . . H33C H 0.2966 0.8081 1.0214 0.307 Uiso 1 1 calc R . . H33D H 0.3459 0.8590 1.0322 0.307 Uiso 1 1 calc R . . C332 C 0.3472(6) 0.8227(7) 0.9433(7) 0.111(5) Uani 1 1 d . . . O333 O 0.3906(3) 0.7912(3) 0.9256(3) 0.0616(19) Uani 1 1 d . . . C334 C 0.3114(6) 0.8578(7) 0.9040(9) 0.133(7) Uani 1 1 d . . . H33E H 0.2807 0.8798 0.9233 0.159 Uiso 1 1 calc R . . C335 C 0.3152(6) 0.8648(6) 0.8380(9) 0.091(5) Uani 1 1 d . . . O336 O 0.3556(3) 0.8447(3) 0.8059(4) 0.066(2) Uani 1 1 d . . . C337 C 0.2683(5) 0.9039(6) 0.8039(7) 0.127(6) Uani 1 1 d . . . H33F H 0.2384 0.9173 0.8335 0.190 Uiso 1 1 calc R . . H33G H 0.2476 0.8816 0.7700 0.190 Uiso 1 1 calc R . . H33H H 0.2888 0.9379 0.7863 0.190 Uiso 1 1 calc R . . N41 N 0.6356(3) 0.7280(3) 0.6639(3) 0.0366(18) Uani 1 1 d . . . C42 C 0.6841(4) 0.7619(4) 0.6596(4) 0.043(2) Uani 1 1 d . . . H42A H 0.7183 0.7549 0.6873 0.052 Uiso 1 1 calc R . . C43 C 0.6873(5) 0.8072(4) 0.6166(4) 0.054(3) Uani 1 1 d . . . H43A H 0.7229 0.8305 0.6144 0.065 Uiso 1 1 calc R . . C44 C 0.6371(5) 0.8174(5) 0.5769(4) 0.059(3) Uani 1 1 d . . . H44A H 0.6375 0.8484 0.5472 0.070 Uiso 1 1 calc R . . C45 C 0.5872(5) 0.7825(4) 0.5808(4) 0.053(3) Uani 1 1 d . . . H45A H 0.5528 0.7889 0.5532 0.064 Uiso 1 1 calc R . . C46 C 0.5862(4) 0.7377(4) 0.6250(4) 0.045(2) Uani 1 1 d . . . C47 C 0.5335(4) 0.6983(4) 0.6314(4) 0.045(2) Uani 1 1 d . . . H47A H 0.4957 0.7203 0.6203 0.053 Uiso 1 1 calc R . . H47B H 0.5366 0.6655 0.6012 0.053 Uiso 1 1 calc R . . N48 N 0.5294(3) 0.6742(3) 0.6949(3) 0.0372(18) Uani 1 1 d . . . C49 C 0.4908(4) 0.6288(4) 0.6964(5) 0.043(2) Uani 1 1 d . . . O410 O 0.4652(3) 0.6027(3) 0.6509(3) 0.062(2) Uani 1 1 d . . . C411 C 0.4744(3) 0.6107(4) 0.7605(4) 0.036(2) Uani 1 1 d . . . N412 N 0.4861(3) 0.6511(3) 0.8047(3) 0.0372(18) Uani 1 1 d . . . C413 C 0.4726(4) 0.6422(4) 0.8647(5) 0.038(2) Uani 1 1 d . . . C414 C 0.4481(4) 0.5905(4) 0.8832(5) 0.049(3) Uani 1 1 d . . . H41A H 0.4395 0.5835 0.9258 0.059 Uiso 1 1 calc R . . C415 C 0.4361(4) 0.5481(4) 0.8370(5) 0.060(3) Uani 1 1 d . . . H41B H 0.4190 0.5116 0.8486 0.072 Uiso 1 1 calc R . . C416 C 0.4483(4) 0.5577(4) 0.7763(5) 0.054(3) Uani 1 1 d . . . H41C H 0.4393 0.5287 0.7452 0.065 Uiso 1 1 calc R . . C417 C 0.4906(4) 0.6926(4) 0.9085(5) 0.042(2) Uani 1 1 d . . . O418 O 0.4959(3) 0.6828(3) 0.9648(3) 0.0541(18) Uani 1 1 d . . . N419 N 0.5026(3) 0.7436(3) 0.8775(3) 0.0367(18) Uani 1 1 d . . . C420 C 0.5338(4) 0.7862(4) 0.9205(4) 0.039(2) Uani 1 1 d . . . H42B H 0.5778 0.7772 0.9232 0.046 Uiso 1 1 calc R . . H42C H 0.5180 0.7814 0.9630 0.046 Uiso 1 1 calc R . . C421 C 0.5250(4) 0.8492(4) 0.8998(4) 0.041(2) Uani 1 1 d . . . N422 N 0.4763(3) 0.8607(3) 0.8630(3) 0.0391(18) Uani 1 1 d . . . C423 C 0.4638(5) 0.9172(4) 0.8484(5) 0.056(3) Uani 1 1 d . . . H42D H 0.4289 0.9258 0.8222 0.067 Uiso 1 1 calc R . . C424 C 0.5001(5) 0.9630(4) 0.8703(5) 0.064(3) Uani 1 1 d . . . H42E H 0.4904 1.0023 0.8591 0.077 Uiso 1 1 calc R . . C425 C 0.5506(5) 0.9506(5) 0.9086(6) 0.072(3) Uani 1 1 d . . . H42F H 0.5759 0.9814 0.9247 0.086 Uiso 1 1 calc R . . C426 C 0.5640(4) 0.8922(4) 0.9233(5) 0.060(3) Uani 1 1 d . . . H42G H 0.5989 0.8823 0.9488 0.072 Uiso 1 1 calc R . . C431 C 0.6706(5) 0.5339(5) 0.5772(5) 0.073(3) Uani 1 1 d . . . H43C H 0.6294 0.5382 0.5585 0.110 Uiso 1 1 calc R . . H43D H 0.6772 0.4930 0.5901 0.110 Uiso 1 1 calc R . . H43E H 0.7003 0.5448 0.5463 0.110 Uiso 1 1 calc R . . C432 C 0.6782(5) 0.5739(4) 0.6345(4) 0.047(3) Uani 1 1 d . . . O433 O 0.6310(3) 0.6039(3) 0.6471(3) 0.0467(16) Uani 1 1 d . . . C434 C 0.7329(4) 0.5757(4) 0.6685(4) 0.044(2) Uani 1 1 d . . . H43F H 0.7634 0.5493 0.6557 0.052 Uiso 1 1 calc R . . C435 C 0.7488(4) 0.6120(4) 0.7200(4) 0.039(2) Uani 1 1 d . . . O436 O 0.7155(3) 0.6509(2) 0.7423(2) 0.0381(15) Uani 1 1 d . . . C437 C 0.8112(4) 0.6054(4) 0.7516(4) 0.048(3) Uani 1 1 d . . . H43G H 0.8155 0.6331 0.7866 0.072 Uiso 1 1 calc R . . H43H H 0.8423 0.6136 0.7213 0.072 Uiso 1 1 calc R . . H43I H 0.8162 0.5653 0.7675 0.072 Uiso 1 1 calc R . . O011 O -0.1506(3) 0.4917(4) 0.5978(4) 0.094(3) Uani 1 1 d . . . C011 C -0.1460(7) 0.5354(6) 0.5477(6) 0.106(5) Uani 1 1 d . . . O021 O 0.7123(3) 0.8470(3) -0.0499(3) 0.069(2) Uani 1 1 d . . . C021 C 0.7087(5) 0.8141(5) 0.0074(5) 0.074(3) Uani 1 1 d . . . O031 O 0.1494(5) 0.3749(4) 0.0627(4) 0.121(3) Uani 1 1 d . . . C031 C 0.2075(6) 0.3503(9) 0.0453(6) 0.152(8) Uani 1 1 d . . . O041 O 0.3954(8) 0.9157(9) 0.0557(9) 0.122(7) Uani 0.50 1 d P . . C041 C 0.4405(15) 0.9139(14) 0.0059(15) 0.125(11) Uiso 0.50 1 d P . . O001 O 0.4917(11) 0.5907(8) 1.0510(6) 0.138(10) Uani 0.50 1 d P . . O002 O 0.3961(8) 0.8314(10) 0.5501(8) 0.133(8) Uani 0.50 1 d P . . O003 O 0.4606(11) 0.4760(13) 0.9805(10) 0.188(13) Uani 0.50 1 d P . . O004 O 0.2801(15) 0.8741(18) 0.517(2) 0.24(2) Uani 0.50 1 d P . . O005 O 0.2975(10) 1.0184(8) 0.4408(11) 0.143(10) Uani 0.50 1 d P . . O006 O 0.1454(12) 0.6621(13) 0.4018(13) 0.073(8) Uiso 0.25 1 d P . . O007 O 0.1881(13) 0.7745(13) 0.8779(14) 0.080(9) Uiso 0.25 1 d P . . O008 O 0.2730(14) 0.9220(15) 0.4746(14) 0.068(9) Uiso 0.25 1 d P . . O009 O 0.2465(18) 0.8434(17) 0.5013(18) 0.090(12) Uiso 0.25 1 d P . . O010 O 0.3059(16) 0.8813(15) 0.4998(15) 0.050(9) Uiso 0.25 1 d P . . O01X O 0.290(2) 0.980(2) 0.474(2) 0.127(16) Uiso 0.25 1 d P . . 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 Ni11 0.0449(8) 0.0325(7) 0.0423(7) 0.0006(6) -0.0013(6) 0.0053(5) Ni12 0.0405(7) 0.0296(6) 0.0245(6) -0.0056(5) -0.0024(5) 0.0082(5) Ni13 0.0491(8) 0.0405(7) 0.0233(6) -0.0008(5) -0.0035(5) 0.0017(6) N11 0.037(5) 0.033(5) 0.084(7) -0.015(4) 0.013(4) -0.002(4) C12 0.047(7) 0.050(8) 0.102(9) -0.010(7) 0.007(6) 0.000(5) C13 0.046(7) 0.038(7) 0.142(12) -0.041(8) 0.007(7) 0.006(5) C14 0.053(8) 0.068(9) 0.120(12) -0.052(8) -0.020(7) 0.004(6) C15 0.049(7) 0.070(9) 0.082(9) -0.032(7) 0.004(6) -0.003(6) C16 0.037(6) 0.062(8) 0.060(7) -0.028(6) -0.005(5) 0.001(5) C17 0.040(6) 0.057(7) 0.044(6) -0.008(5) 0.003(5) 0.006(5) N18 0.043(5) 0.042(5) 0.025(4) -0.004(3) 0.000(3) 0.007(4) C19 0.043(6) 0.057(7) 0.023(5) 0.003(5) 0.006(4) 0.018(5) O110 0.038(4) 0.074(5) 0.066(5) 0.003(4) -0.002(3) 0.026(4) C111 0.057(7) 0.034(6) 0.023(5) 0.008(4) 0.006(4) 0.022(5) N112 0.060(6) 0.026(4) 0.023(4) 0.004(3) -0.002(4) 0.015(4) C113 0.074(7) 0.022(5) 0.017(5) 0.000(4) -0.012(4) 0.007(5) C114 0.081(8) 0.033(6) 0.021(5) -0.001(4) 0.001(5) 0.013(5) C115 0.104(10) 0.030(6) 0.029(6) -0.006(5) -0.003(6) 0.022(6) C116 0.079(8) 0.041(6) 0.034(6) 0.006(5) 0.010(5) 0.033(6) C117 0.053(7) 0.042(6) 0.019(5) 0.011(4) -0.008(5) 0.008(5) O118 0.072(5) 0.051(4) 0.039(4) -0.018(3) -0.012(3) -0.007(3) N119 0.045(5) 0.031(4) 0.020(4) -0.009(3) -0.002(3) 0.010(3) C120 0.043(6) 0.046(6) 0.024(5) 0.001(4) -0.006(4) -0.004(4) C121 0.044(6) 0.028(5) 0.042(6) -0.001(4) 0.000(5) -0.001(4) N122 0.042(5) 0.040(5) 0.028(4) -0.009(4) 0.004(3) 0.001(3) C123 0.044(6) 0.058(7) 0.038(6) -0.013(5) -0.004(5) -0.006(5) C124 0.056(7) 0.056(7) 0.057(7) -0.016(6) 0.009(6) 0.006(6) C125 0.053(7) 0.040(6) 0.082(9) -0.004(6) 0.007(6) 0.016(5) C126 0.051(7) 0.040(6) 0.052(7) -0.004(5) -0.005(5) 0.000(5) C131 0.063(8) 0.068(8) 0.081(8) 0.022(6) 0.013(6) -0.012(6) C132 0.041(7) 0.038(6) 0.067(7) 0.004(5) 0.001(5) -0.008(5) O133 0.056(4) 0.042(4) 0.052(4) 0.009(3) -0.001(3) 0.004(3) C134 0.069(8) 0.048(7) 0.064(7) 0.025(6) 0.005(6) 0.003(6) C135 0.097(10) 0.030(6) 0.054(7) 0.006(5) -0.018(7) 0.005(6) O136 0.063(5) 0.045(4) 0.064(5) 0.022(4) -0.001(4) 0.007(3) C137 0.123(11) 0.067(9) 0.082(9) 0.039(7) -0.016(8) 0.008(7) N21 0.049(5) 0.036(5) 0.028(4) 0.007(3) -0.001(4) 0.015(4) C22 0.057(7) 0.040(6) 0.031(5) 0.000(4) 0.007(5) 0.007(5) C23 0.049(7) 0.046(6) 0.048(6) 0.005(5) 0.012(5) 0.003(5) C24 0.076(8) 0.057(7) 0.037(6) -0.009(5) 0.013(6) 0.005(6) C25 0.053(7) 0.050(6) 0.028(5) 0.012(5) -0.001(5) 0.001(5) C26 0.041(6) 0.036(5) 0.021(5) 0.007(4) 0.001(4) 0.007(4) C27 0.036(6) 0.038(6) 0.034(5) -0.001(4) -0.007(4) 0.006(4) N28 0.034(4) 0.039(5) 0.029(4) -0.005(3) -0.004(3) 0.011(3) C29 0.043(6) 0.032(5) 0.039(6) 0.001(4) 0.001(5) -0.003(4) O210 0.040(4) 0.047(4) 0.043(4) 0.000(3) -0.010(3) 0.015(3) C211 0.041(6) 0.031(5) 0.027(5) -0.004(4) -0.008(4) 0.005(4) N212 0.029(4) 0.031(4) 0.029(4) -0.003(3) 0.002(3) 0.001(3) C213 0.036(6) 0.040(6) 0.026(5) -0.011(4) -0.001(4) 0.001(4) C214 0.060(7) 0.045(7) 0.039(6) -0.011(5) -0.006(5) 0.003(5) C215 0.056(7) 0.031(6) 0.059(7) -0.019(5) 0.016(5) 0.007(5) C216 0.045(6) 0.031(5) 0.044(6) -0.009(5) -0.004(4) 0.006(4) C217 0.031(5) 0.054(6) 0.025(5) 0.000(5) -0.013(4) 0.004(4) O218 0.063(5) 0.052(4) 0.040(4) -0.019(3) -0.015(3) 0.008(3) N219 0.042(5) 0.031(4) 0.025(4) -0.010(3) -0.005(3) 0.006(3) C220 0.044(6) 0.042(6) 0.032(5) 0.002(4) -0.008(4) 0.004(4) C221 0.048(6) 0.044(6) 0.012(4) 0.005(4) 0.006(4) 0.008(5) N222 0.066(6) 0.034(5) 0.018(4) 0.005(3) 0.003(4) 0.005(4) C223 0.082(8) 0.042(7) 0.022(5) 0.002(4) 0.001(5) -0.002(5) C224 0.107(10) 0.045(7) 0.027(6) -0.003(5) 0.008(6) 0.028(7) C225 0.110(11) 0.059(8) 0.030(6) 0.001(5) 0.008(6) 0.036(7) C226 0.067(7) 0.057(7) 0.025(5) 0.008(5) 0.004(5) 0.027(6) C231 0.092(10) 0.076(9) 0.083(9) -0.008(7) 0.011(7) -0.028(7) C232 0.066(8) 0.042(7) 0.058(8) 0.000(6) -0.001(6) -0.003(5) O233 0.068(5) 0.048(4) 0.035(4) 0.005(3) -0.005(3) -0.015(3) C234 0.075(8) 0.047(7) 0.061(8) 0.010(6) 0.033(6) 0.000(6) C235 0.098(10) 0.041(7) 0.030(6) 0.006(5) 0.011(6) 0.017(6) O236 0.066(5) 0.061(5) 0.027(4) 0.001(3) -0.002(3) 0.005(4) C237 0.141(11) 0.074(9) 0.020(6) 0.000(5) 0.009(6) 0.026(7) Ni21 0.0390(7) 0.0332(7) 0.0375(7) -0.0026(5) -0.0075(5) 0.0015(5) Ni22 0.0364(7) 0.0264(6) 0.0434(7) -0.0002(5) -0.0085(5) 0.0000(5) Ni23 0.0362(8) 0.0374(7) 0.0573(8) 0.0027(6) -0.0066(6) 0.0037(5) N31 0.036(5) 0.031(5) 0.056(5) 0.002(4) 0.000(4) 0.002(3) C32 0.040(6) 0.036(6) 0.061(7) -0.004(5) 0.005(5) -0.001(4) C33 0.066(8) 0.027(6) 0.091(9) 0.001(6) -0.001(6) -0.009(5) C34 0.101(10) 0.046(8) 0.085(10) 0.025(7) -0.001(8) 0.000(6) C35 0.095(9) 0.046(7) 0.041(6) 0.005(5) -0.003(6) 0.010(6) C36 0.044(6) 0.032(6) 0.045(6) 0.005(5) -0.004(5) 0.008(4) C37 0.040(6) 0.038(6) 0.035(5) -0.002(4) -0.009(4) 0.008(4) N38 0.037(5) 0.032(5) 0.038(4) 0.000(3) -0.004(3) -0.002(3) C39 0.025(5) 0.043(6) 0.044(6) 0.002(5) 0.005(4) 0.001(4) O310 0.040(4) 0.054(4) 0.050(4) -0.005(3) -0.013(3) -0.001(3) C311 0.038(6) 0.036(6) 0.032(5) -0.004(4) -0.003(4) -0.006(4) N312 0.033(5) 0.029(4) 0.037(4) -0.001(3) -0.004(3) 0.000(3) C313 0.050(6) 0.034(6) 0.032(5) -0.005(4) -0.005(4) 0.000(5) C314 0.065(8) 0.034(6) 0.048(6) 0.004(5) 0.003(5) 0.006(5) C315 0.063(8) 0.027(6) 0.075(8) 0.004(5) 0.015(6) -0.013(5) C316 0.039(6) 0.037(6) 0.048(6) -0.003(5) 0.003(4) -0.005(4) C317 0.047(6) 0.035(6) 0.041(6) -0.004(5) -0.008(5) 0.009(5) O318 0.082(5) 0.048(5) 0.055(4) 0.006(4) -0.027(4) 0.011(4) N319 0.039(5) 0.034(5) 0.055(5) -0.003(4) -0.014(4) -0.005(4) C320 0.045(7) 0.039(6) 0.087(8) -0.004(6) -0.023(6) 0.004(5) C321 0.044(7) 0.035(6) 0.090(9) -0.010(6) -0.022(6) 0.012(5) N322 0.036(5) 0.036(5) 0.099(8) 0.004(5) -0.014(5) 0.006(4) C323 0.043(7) 0.059(8) 0.114(11) 0.006(7) -0.009(7) -0.014(6) C324 0.063(9) 0.068(9) 0.143(14) 0.034(9) -0.021(9) -0.012(7) C325 0.056(9) 0.053(9) 0.174(16) 0.006(10) -0.031(10) -0.010(6) C326 0.052(8) 0.064(9) 0.130(12) -0.014(8) -0.047(8) 0.002(6) C331 0.25(2) 0.19(2) 0.190(19) 0.112(16) 0.182(17) 0.124(17) C332 0.090(11) 0.108(12) 0.141(14) 0.044(10) 0.072(10) 0.036(9) O333 0.053(5) 0.058(5) 0.075(5) 0.016(4) 0.021(4) 0.005(4) C334 0.095(12) 0.112(13) 0.196(19) 0.062(13) 0.068(12) 0.083(10) C335 0.042(8) 0.074(10) 0.155(15) 0.028(10) -0.014(9) 0.018(7) O336 0.043(5) 0.049(5) 0.104(6) -0.004(4) -0.013(4) 0.015(4) C337 0.068(10) 0.086(11) 0.223(18) 0.024(11) -0.038(10) 0.035(8) N41 0.042(5) 0.041(5) 0.026(4) -0.002(3) 0.000(4) 0.001(4) C42 0.048(7) 0.047(6) 0.034(6) -0.005(5) -0.006(4) -0.004(5) C43 0.075(8) 0.047(7) 0.042(6) -0.001(5) 0.012(6) -0.014(5) C44 0.079(8) 0.063(8) 0.034(6) 0.018(5) -0.005(6) 0.003(6) C45 0.067(8) 0.060(7) 0.033(6) 0.008(5) -0.006(5) -0.001(6) C46 0.046(6) 0.045(6) 0.042(6) -0.009(5) -0.011(5) 0.000(5) C47 0.044(6) 0.050(6) 0.038(6) -0.006(5) -0.008(4) 0.001(5) N48 0.040(5) 0.034(5) 0.037(5) -0.003(4) -0.004(3) -0.002(4) C49 0.042(6) 0.036(6) 0.050(7) -0.003(5) 0.001(5) 0.006(5) O410 0.059(5) 0.060(5) 0.066(5) -0.025(4) -0.011(4) -0.010(4) C411 0.018(5) 0.032(6) 0.058(7) -0.016(5) -0.002(4) -0.001(4) N412 0.041(5) 0.024(4) 0.046(5) 0.002(4) -0.006(4) -0.003(3) C413 0.025(5) 0.030(5) 0.060(7) 0.001(5) -0.005(4) -0.006(4) C414 0.050(7) 0.038(6) 0.059(7) 0.000(5) 0.010(5) -0.009(5) C415 0.056(7) 0.034(6) 0.091(9) -0.003(6) 0.021(6) -0.013(5) C416 0.053(7) 0.041(7) 0.068(8) -0.016(5) 0.010(6) -0.017(5) C417 0.048(6) 0.024(5) 0.054(7) -0.007(5) -0.013(5) 0.002(4) O418 0.073(5) 0.037(4) 0.050(4) 0.007(3) -0.018(4) -0.007(3) N419 0.032(4) 0.031(4) 0.047(5) -0.005(4) -0.005(3) 0.001(3) C420 0.041(6) 0.033(6) 0.040(5) 0.001(4) -0.019(4) -0.004(4) C421 0.032(6) 0.034(6) 0.058(6) -0.001(5) 0.000(5) 0.004(4) N422 0.043(5) 0.026(4) 0.048(5) -0.002(4) 0.001(4) 0.006(3) C423 0.068(8) 0.029(6) 0.070(8) 0.005(5) -0.002(6) 0.010(5) C424 0.068(8) 0.024(6) 0.100(9) 0.010(6) 0.006(7) -0.001(5) C425 0.053(8) 0.038(7) 0.123(11) -0.016(7) -0.005(7) -0.013(5) C426 0.040(6) 0.042(7) 0.099(9) -0.010(6) -0.005(6) -0.008(5) C431 0.101(9) 0.062(8) 0.055(7) -0.033(6) -0.011(6) 0.004(6) C432 0.065(8) 0.034(6) 0.040(6) -0.008(5) -0.004(5) 0.009(5) O433 0.056(4) 0.044(4) 0.039(4) -0.009(3) -0.013(3) 0.002(3) C434 0.047(6) 0.040(6) 0.044(6) -0.004(5) 0.000(5) 0.009(4) C435 0.044(6) 0.034(6) 0.040(6) 0.014(5) 0.001(5) -0.002(4) O436 0.047(4) 0.031(4) 0.035(4) -0.007(3) -0.005(3) 0.007(3) C437 0.042(6) 0.056(7) 0.046(6) -0.002(5) 0.004(5) 0.007(5) O011 0.083(6) 0.087(7) 0.111(7) -0.028(6) -0.007(5) 0.011(5) C011 0.158(14) 0.076(10) 0.080(10) 0.011(8) -0.025(9) 0.014(9) O021 0.070(5) 0.065(5) 0.072(5) 0.002(4) -0.005(4) 0.002(4) C021 0.096(9) 0.094(10) 0.033(6) 0.023(6) 0.012(6) 0.000(7) O031 0.165(10) 0.121(9) 0.074(6) 0.000(6) -0.015(6) 0.009(7) C031 0.045(8) 0.31(2) 0.098(11) -0.053(13) -0.027(8) 0.093(12) O041 0.074(13) 0.17(2) 0.128(16) -0.034(14) 0.013(11) -0.012(12) O001 0.31(3) 0.088(13) 0.018(8) -0.029(8) 0.031(11) -0.139(16) O002 0.120(16) 0.20(2) 0.082(14) -0.017(14) -0.005(11) 0.036(14) O003 0.22(3) 0.25(3) 0.092(16) 0.089(18) -0.068(16) -0.12(2) O004 0.16(4) 0.25(4) 0.30(5) -0.16(4) -0.01(3) 0.13(3) O005 0.17(2) 0.071(14) 0.18(2) -0.023(14) -0.138(17) 0.003(13) _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 Ni11 O136 1.989(6) . y Ni11 O133 2.018(6) . y Ni11 N11 2.053(8) . y Ni11 N21 2.078(7) . y Ni11 N18 2.187(7) . y Ni11 N28 2.224(7) . y Ni12 N112 1.964(7) . y Ni12 N212 1.976(6) . y Ni12 N18 2.157(7) . y Ni12 N119 2.171(7) . y Ni12 N28 2.189(6) . y Ni12 N219 2.194(6) . y Ni13 O236 1.999(6) . y Ni13 O233 2.007(6) . y Ni13 N122 2.048(7) . y Ni13 N222 2.063(7) . y Ni13 N119 2.188(6) . y Ni13 N219 2.211(7) . y N11 C16 1.346(12) . ? N11 C12 1.368(12) . ? C12 C13 1.431(14) . ? C13 C14 1.321(15) . ? C14 C15 1.341(15) . ? C15 C16 1.386(13) . ? C16 C17 1.492(13) . ? C17 N18 1.467(10) . ? N18 C19 1.361(10) . ? C19 O110 1.230(9) . ? C19 C111 1.504(12) . ? C111 N112 1.333(10) . ? C111 C116 1.418(12) . ? N112 C113 1.347(10) . ? C113 C114 1.383(11) . ? C113 C117 1.483(12) . ? C114 C115 1.366(12) . ? C115 C116 1.384(13) . ? C117 O118 1.240(10) . ? C117 N119 1.357(10) . ? N119 C120 1.466(10) . ? C120 C121 1.504(11) . ? C121 N122 1.354(10) . ? C121 C126 1.356(12) . ? N122 C123 1.342(10) . ? C123 C124 1.364(12) . ? C124 C125 1.380(13) . ? C125 C126 1.356(13) . ? C131 C132 1.514(13) . ? C132 O133 1.254(10) . ? C132 C134 1.392(13) . ? C134 C135 1.411(14) . ? C135 O136 1.245(12) . ? C135 C137 1.528(13) . ? N21 C26 1.335(10) . ? N21 C22 1.340(10) . ? C22 C23 1.381(12) . ? C23 C24 1.383(12) . ? C24 C25 1.378(12) . ? C25 C26 1.379(11) . ? C26 C27 1.501(11) . ? C27 N28 1.478(9) . ? N28 C29 1.351(10) . ? C29 O210 1.262(9) . ? C29 C211 1.496(11) . ? C211 N212 1.326(9) . ? C211 C216 1.366(11) . ? N212 C213 1.357(9) . ? C213 C214 1.377(11) . ? C213 C217 1.496(11) . ? C214 C215 1.388(12) . ? C215 C216 1.403(11) . ? C217 O218 1.258(9) . ? C217 N219 1.321(10) . ? N219 C220 1.453(10) . ? C220 C221 1.491(11) . ? C221 N222 1.329(10) . ? C221 C226 1.374(11) . ? N222 C223 1.354(11) . ? C223 C224 1.408(13) . ? C224 C225 1.362(14) . ? C225 C226 1.349(13) . ? C231 C232 1.519(13) . ? C232 O233 1.244(11) . ? C232 C234 1.415(13) . ? C234 C235 1.389(14) . ? C235 O236 1.265(12) . ? C235 C237 1.506(12) . ? Ni21 O436 1.997(6) . ? Ni21 O433 2.018(6) . ? Ni21 N41 2.051(7) . ? Ni21 N31 2.057(7) . ? Ni21 N48 2.219(7) . ? Ni21 N38 2.248(7) . ? Ni22 N312 1.952(7) . ? Ni22 N412 1.970(7) . ? Ni22 N48 2.177(7) . ? Ni22 N419 2.180(7) . ? Ni22 N38 2.191(7) . ? Ni22 N319 2.208(7) . ? Ni23 O336 1.993(7) . ? Ni23 O333 2.018(7) . ? Ni23 N422 2.046(7) . ? Ni23 N322 2.050(8) . ? Ni23 N419 2.223(6) . ? Ni23 N319 2.233(8) . ? N31 C32 1.346(10) . ? N31 C36 1.354(10) . ? C32 C33 1.381(13) . ? C33 C34 1.367(14) . ? C34 C35 1.399(14) . ? C35 C36 1.354(12) . ? C36 C37 1.477(11) . ? C37 N38 1.452(10) . ? N38 C39 1.361(10) . ? C39 O310 1.230(9) . ? C39 C311 1.513(12) . ? C311 N312 1.333(9) . ? C311 C316 1.392(11) . ? N312 C313 1.324(10) . ? C313 C314 1.403(12) . ? C313 C317 1.485(12) . ? C314 C315 1.379(12) . ? C315 C316 1.379(12) . ? C317 O318 1.262(10) . ? C317 N319 1.335(11) . ? N319 C320 1.478(10) . ? C320 C321 1.503(14) . ? C321 N322 1.374(13) . ? C321 C326 1.404(13) . ? N322 C323 1.340(13) . ? C323 C324 1.376(15) . ? C324 C325 1.384(17) . ? C325 C326 1.402(17) . ? C331 C332 1.526(19) . ? C332 O333 1.266(13) . ? C332 C334 1.381(19) . ? C334 C335 1.423(19) . ? C335 O336 1.234(15) . ? C335 C337 1.524(15) . ? N41 C42 1.323(10) . ? N41 C46 1.357(10) . ? C42 C43 1.385(12) . ? C43 C44 1.383(13) . ? C44 C45 1.361(13) . ? C45 C46 1.391(12) . ? C46 C47 1.476(12) . ? C47 N48 1.470(10) . ? N48 C49 1.340(11) . ? C49 O410 1.251(10) . ? C49 C411 1.487(12) . ? C411 N412 1.334(10) . ? C411 C416 1.385(12) . ? N412 C413 1.343(10) . ? C413 C414 1.360(11) . ? C413 C417 1.524(12) . ? C414 C415 1.397(13) . ? C415 C416 1.353(13) . ? C417 O418 1.223(10) . ? C417 N419 1.369(11) . ? N419 C420 1.483(10) . ? C420 C421 1.513(11) . ? C421 N422 1.327(10) . ? C421 C426 1.383(12) . ? N422 C423 1.351(10) . ? C423 C424 1.382(13) . ? C424 C425 1.381(13) . ? C425 C426 1.395(13) . ? C431 C432 1.530(12) . ? C432 O433 1.281(10) . ? C432 C434 1.380(12) . ? C434 C435 1.408(12) . ? C435 O436 1.255(10) . ? C435 C437 1.512(11) . ? O011 C011 1.467(14) . ? O021 C021 1.439(11) . ? O031 C031 1.458(14) . ? O041 C041 1.48(3) . ? O004 O010 0.71(5) . ? O004 O009 1.06(4) . ? O004 O008 1.42(5) . ? O005 O01X 1.14(5) . ? O006 O007 1.81(4) 4_575 ? O007 O006 1.81(4) 4_576 ? O008 O010 1.28(5) . ? O008 O01X 1.38(5) . ? O009 O010 1.57(6) . ? 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 O136 Ni11 O133 93.2(3) . . y O136 Ni11 N11 91.3(3) . . y O133 Ni11 N11 89.6(3) . . y O136 Ni11 N21 87.9(3) . . y O133 Ni11 N21 92.9(3) . . y N11 Ni11 N21 177.5(3) . . y O136 Ni11 N18 171.4(3) . . y O133 Ni11 N18 88.6(3) . . y N11 Ni11 N18 80.3(3) . . y N21 Ni11 N18 100.4(3) . . y O136 Ni11 N28 88.1(3) . . y O133 Ni11 N28 172.3(3) . . y N11 Ni11 N28 98.0(3) . . y N21 Ni11 N28 79.6(3) . . y N18 Ni11 N28 91.2(2) . . y N112 Ni12 N212 179.0(3) . . y N112 Ni12 N18 78.9(3) . . y N212 Ni12 N18 100.4(3) . . y N112 Ni12 N119 78.3(3) . . y N212 Ni12 N119 102.3(2) . . y N18 Ni12 N119 157.2(3) . . y N112 Ni12 N28 102.4(3) . . y N212 Ni12 N28 78.4(3) . . y N18 Ni12 N28 93.0(2) . . y N119 Ni12 N28 90.9(2) . . y N112 Ni12 N219 100.2(3) . . y N212 Ni12 N219 78.9(3) . . y N18 Ni12 N219 91.5(2) . . y N119 Ni12 N219 93.5(2) . . y N28 Ni12 N219 157.3(2) . . y O236 Ni13 O233 93.2(3) . . y O236 Ni13 N122 92.0(3) . . y O233 Ni13 N122 88.7(3) . . y O236 Ni13 N222 86.9(3) . . y O233 Ni13 N222 92.6(3) . . y N122 Ni13 N222 178.3(3) . . y O236 Ni13 N119 172.2(3) . . y O233 Ni13 N119 86.8(2) . . y N122 Ni13 N119 80.3(3) . . y N222 Ni13 N119 100.9(2) . . y O236 Ni13 N219 88.5(3) . . y O233 Ni13 N219 171.7(3) . . y N122 Ni13 N219 99.4(3) . . y N222 Ni13 N219 79.3(3) . . y N119 Ni13 N219 92.6(2) . . y C16 N11 C12 119.8(9) . . ? C16 N11 Ni11 115.2(6) . . ? C12 N11 Ni11 124.9(8) . . ? N11 C12 C13 119.0(11) . . ? C14 C13 C12 119.5(11) . . ? C13 C14 C15 120.9(11) . . ? C14 C15 C16 120.9(12) . . ? N11 C16 C15 119.8(10) . . ? N11 C16 C17 116.0(8) . . ? C15 C16 C17 124.1(10) . . ? N18 C17 C16 113.6(7) . . ? C19 N18 C17 110.6(7) . . ? C19 N18 Ni12 109.3(6) . . ? C17 N18 Ni12 124.3(5) . . ? C19 N18 Ni11 118.3(5) . . ? C17 N18 Ni11 104.4(5) . . ? Ni12 N18 Ni11 88.7(2) . . ? O110 C19 N18 127.6(9) . . ? O110 C19 C111 119.3(8) . . ? N18 C19 C111 113.1(8) . . ? N112 C111 C116 120.2(9) . . ? N112 C111 C19 113.8(7) . . ? C116 C111 C19 125.9(9) . . ? C111 N112 C113 122.7(8) . . ? C111 N112 Ni12 118.6(6) . . ? C113 N112 Ni12 118.6(6) . . ? N112 C113 C114 119.3(9) . . ? N112 C113 C117 114.8(8) . . ? C114 C113 C117 125.4(9) . . ? C115 C114 C113 119.1(9) . . ? C114 C115 C116 122.2(9) . . ? C115 C116 C111 116.4(9) . . ? O118 C117 N119 128.0(9) . . ? O118 C117 C113 118.7(8) . . ? N119 C117 C113 113.3(8) . . ? C117 N119 C120 111.5(6) . . ? C117 N119 Ni12 110.5(6) . . ? C120 N119 Ni12 125.6(5) . . ? C117 N119 Ni13 115.3(5) . . ? C120 N119 Ni13 103.8(5) . . ? Ni12 N119 Ni13 87.5(2) . . ? N119 C120 C121 114.1(6) . . ? N122 C121 C126 121.4(8) . . ? N122 C121 C120 114.6(7) . . ? C126 C121 C120 124.0(8) . . ? C123 N122 C121 117.2(8) . . ? C123 N122 Ni13 127.0(6) . . ? C121 N122 Ni13 115.8(6) . . ? N122 C123 C124 124.1(9) . . ? C123 C124 C125 117.2(9) . . ? C126 C125 C124 119.6(9) . . ? C125 C126 C121 120.5(9) . . ? O133 C132 C134 126.1(9) . . ? O133 C132 C131 115.0(9) . . ? C134 C132 C131 118.9(9) . . ? C132 O133 Ni11 123.5(6) . . ? C132 C134 C135 126.6(10) . . ? O136 C135 C134 125.9(9) . . ? O136 C135 C137 115.7(11) . . ? C134 C135 C137 118.4(11) . . ? C135 O136 Ni11 124.5(7) . . ? C26 N21 C22 119.8(8) . . ? C26 N21 Ni11 115.4(6) . . ? C22 N21 Ni11 124.7(6) . . ? N21 C22 C23 120.9(9) . . ? C22 C23 C24 119.5(9) . . ? C25 C24 C23 118.8(9) . . ? C24 C25 C26 119.1(9) . . ? N21 C26 C25 121.7(8) . . ? N21 C26 C27 116.3(8) . . ? C25 C26 C27 121.9(8) . . ? N28 C27 C26 113.2(6) . . ? C29 N28 C27 111.8(6) . . ? C29 N28 Ni12 108.5(5) . . ? C27 N28 Ni12 125.8(5) . . ? C29 N28 Ni11 118.8(6) . . ? C27 N28 Ni11 103.3(5) . . ? Ni12 N28 Ni11 87.0(2) . . ? O210 C29 N28 127.6(8) . . ? O210 C29 C211 116.9(8) . . ? N28 C29 C211 115.3(7) . . ? N212 C211 C216 120.8(8) . . ? N212 C211 C29 113.7(7) . . ? C216 C211 C29 125.2(8) . . ? C211 N212 C213 123.1(7) . . ? C211 N212 Ni12 119.2(5) . . ? C213 N212 Ni12 117.6(5) . . ? N212 C213 C214 118.5(8) . . ? N212 C213 C217 113.9(7) . . ? C214 C213 C217 127.5(8) . . ? C213 C214 C215 119.4(8) . . ? C214 C215 C216 120.1(8) . . ? C211 C216 C215 118.0(8) . . ? O218 C217 N219 128.8(8) . . ? O218 C217 C213 115.2(8) . . ? N219 C217 C213 115.9(7) . . ? C217 N219 C220 111.6(6) . . ? C217 N219 Ni12 109.0(5) . . ? C220 N219 Ni12 125.1(5) . . ? C217 N219 Ni13 118.3(5) . . ? C220 N219 Ni13 104.7(5) . . ? Ni12 N219 Ni13 86.3(2) . . ? N219 C220 C221 114.1(7) . . ? N222 C221 C226 121.1(9) . . ? N222 C221 C220 116.2(7) . . ? C226 C221 C220 122.4(9) . . ? C221 N222 C223 118.9(8) . . ? C221 N222 Ni13 116.0(6) . . ? C223 N222 Ni13 124.8(7) . . ? N222 C223 C224 121.6(10) . . ? C225 C224 C223 117.5(11) . . ? C226 C225 C224 120.3(10) . . ? C225 C226 C221 120.6(10) . . ? O233 C232 C234 125.6(10) . . ? O233 C232 C231 116.3(9) . . ? C234 C232 C231 118.0(10) . . ? C232 O233 Ni13 123.7(6) . . ? C235 C234 C232 126.7(9) . . ? O236 C235 C234 126.0(9) . . ? O236 C235 C237 114.9(10) . . ? C234 C235 C237 119.0(11) . . ? C235 O236 Ni13 123.7(6) . . ? O436 Ni21 O433 92.5(2) . . ? O436 Ni21 N41 93.8(3) . . ? O433 Ni21 N41 89.0(3) . . ? O436 Ni21 N31 87.3(2) . . ? O433 Ni21 N31 92.2(3) . . ? N41 Ni21 N31 178.3(3) . . ? O436 Ni21 N48 173.5(3) . . ? O433 Ni21 N48 88.7(2) . . ? N41 Ni21 N48 79.9(3) . . ? N31 Ni21 N48 99.0(3) . . ? O436 Ni21 N38 87.5(2) . . ? O433 Ni21 N38 171.7(3) . . ? N41 Ni21 N38 99.2(3) . . ? N31 Ni21 N38 79.5(3) . . ? N48 Ni21 N38 92.3(2) . . ? N312 Ni22 N412 175.9(3) . . ? N312 Ni22 N48 105.4(3) . . ? N412 Ni22 N48 78.1(3) . . ? N312 Ni22 N419 97.9(3) . . ? N412 Ni22 N419 78.7(3) . . ? N48 Ni22 N419 156.8(3) . . ? N312 Ni22 N38 78.7(3) . . ? N412 Ni22 N38 98.9(3) . . ? N48 Ni22 N38 95.0(2) . . ? N419 Ni22 N38 89.4(2) . . ? N312 Ni22 N319 77.9(3) . . ? N412 Ni22 N319 104.4(3) . . ? N48 Ni22 N319 90.9(3) . . ? N419 Ni22 N319 94.1(3) . . ? N38 Ni22 N319 156.6(3) . . ? O336 Ni23 O333 92.8(3) . . ? O336 Ni23 N422 91.7(3) . . ? O333 Ni23 N422 88.7(3) . . ? O336 Ni23 N322 87.8(3) . . ? O333 Ni23 N322 93.0(4) . . ? N422 Ni23 N322 178.3(4) . . ? O336 Ni23 N419 171.6(3) . . ? O333 Ni23 N419 86.8(3) . . ? N422 Ni23 N419 79.9(3) . . ? N322 Ni23 N419 100.6(3) . . ? O336 Ni23 N319 89.3(3) . . ? O333 Ni23 N319 172.0(3) . . ? N422 Ni23 N319 98.9(3) . . ? N322 Ni23 N319 79.4(3) . . ? N419 Ni23 N319 92.2(3) . . ? C32 N31 C36 118.3(8) . . ? C32 N31 Ni21 125.8(7) . . ? C36 N31 Ni21 115.6(6) . . ? N31 C32 C33 124.4(9) . . ? C34 C33 C32 116.4(10) . . ? C33 C34 C35 119.9(10) . . ? C36 C35 C34 120.5(10) . . ? C35 C36 N31 120.5(9) . . ? C35 C36 C37 122.7(9) . . ? N31 C36 C37 116.6(8) . . ? N38 C37 C36 115.1(7) . . ? C39 N38 C37 111.3(7) . . ? C39 N38 Ni22 109.6(5) . . ? C37 N38 Ni22 126.6(5) . . ? C39 N38 Ni21 117.7(5) . . ? C37 N38 Ni21 103.8(5) . . ? Ni22 N38 Ni21 85.7(2) . . ? O310 C39 N38 126.8(8) . . ? O310 C39 C311 119.5(8) . . ? N38 C39 C311 113.6(7) . . ? N312 C311 C316 121.4(8) . . ? N312 C311 C39 114.5(7) . . ? C316 C311 C39 123.9(8) . . ? C313 N312 C311 120.9(7) . . ? C313 N312 Ni22 119.6(6) . . ? C311 N312 Ni22 119.5(5) . . ? N312 C313 C314 121.0(8) . . ? N312 C313 C317 114.8(8) . . ? C314 C313 C317 124.2(8) . . ? C315 C314 C313 118.3(8) . . ? C316 C315 C314 120.2(9) . . ? C315 C316 C311 118.2(9) . . ? O318 C317 N319 125.6(8) . . ? O318 C317 C313 119.7(9) . . ? N319 C317 C313 114.5(8) . . ? C317 N319 C320 112.5(7) . . ? C317 N319 Ni22 109.2(6) . . ? C320 N319 Ni22 125.0(6) . . ? C317 N319 Ni23 117.7(6) . . ? C320 N319 Ni23 103.8(6) . . ? Ni22 N319 Ni23 86.1(3) . . ? N319 C320 C321 111.9(8) . . ? N322 C321 C326 121.3(11) . . ? N322 C321 C320 116.3(9) . . ? C326 C321 C320 122.4(11) . . ? C323 N322 C321 119.3(9) . . ? C323 N322 Ni23 125.5(8) . . ? C321 N322 Ni23 115.3(7) . . ? N322 C323 C324 122.7(12) . . ? C323 C324 C325 118.6(13) . . ? C324 C325 C326 120.6(12) . . ? C325 C326 C321 117.5(13) . . ? O333 C332 C334 124.5(14) . . ? O333 C332 C331 113.7(13) . . ? C334 C332 C331 121.8(14) . . ? C332 O333 Ni23 124.3(8) . . ? C332 C334 C335 127.6(13) . . ? O336 C335 C334 125.5(11) . . ? O336 C335 C337 116.1(15) . . ? C334 C335 C337 118.2(14) . . ? C335 O336 Ni23 124.6(9) . . ? C42 N41 C46 119.4(8) . . ? C42 N41 Ni21 126.9(6) . . ? C46 N41 Ni21 113.6(6) . . ? N41 C42 C43 122.9(9) . . ? C44 C43 C42 118.1(9) . . ? C45 C44 C43 119.4(10) . . ? C44 C45 C46 120.3(9) . . ? N41 C46 C45 119.9(9) . . ? N41 C46 C47 117.1(8) . . ? C45 C46 C47 122.9(8) . . ? N48 C47 C46 113.1(7) . . ? C49 N48 C47 112.0(7) . . ? C49 N48 Ni22 110.1(6) . . ? C47 N48 Ni22 125.9(6) . . ? C49 N48 Ni21 117.6(6) . . ? C47 N48 Ni21 102.1(5) . . ? Ni22 N48 Ni21 86.8(2) . . ? O410 C49 N48 127.8(9) . . ? O410 C49 C411 117.6(9) . . ? N48 C49 C411 114.4(8) . . ? N412 C411 C416 120.0(9) . . ? N412 C411 C49 114.3(8) . . ? C416 C411 C49 125.7(8) . . ? C411 N412 C413 121.7(7) . . ? C411 N412 Ni22 118.9(6) . . ? C413 N412 Ni22 119.4(6) . . ? N412 C413 C414 120.9(8) . . ? N412 C413 C417 114.2(8) . . ? C414 C413 C417 124.8(9) . . ? C413 C414 C415 117.4(9) . . ? C416 C415 C414 121.6(9) . . ? C415 C416 C411 118.3(9) . . ? O418 C417 N419 128.3(8) . . ? O418 C417 C413 118.4(8) . . ? N419 C417 C413 113.2(8) . . ? C417 N419 C420 110.4(7) . . ? C417 N419 Ni22 110.5(6) . . ? C420 N419 Ni22 126.4(5) . . ? C417 N419 Ni23 115.4(5) . . ? C420 N419 Ni23 104.9(5) . . ? Ni22 N419 Ni23 87.1(2) . . ? N419 C420 C421 112.9(7) . . ? N422 C421 C426 123.2(9) . . ? N422 C421 C420 116.8(7) . . ? C426 C421 C420 119.8(8) . . ? C421 N422 C423 118.5(8) . . ? C421 N422 Ni23 116.9(6) . . ? C423 N422 Ni23 124.4(6) . . ? N422 C423 C424 122.1(9) . . ? C425 C424 C423 119.1(9) . . ? C424 C425 C426 119.0(9) . . ? C421 C426 C425 118.2(9) . . ? O433 C432 C434 124.8(8) . . ? O433 C432 C431 115.1(8) . . ? C434 C432 C431 120.0(9) . . ? C432 O433 Ni21 123.9(6) . . ? C432 C434 C435 127.5(9) . . ? O436 C435 C434 125.6(8) . . ? O436 C435 C437 115.6(8) . . ? C434 C435 C437 118.7(8) . . ? C435 O436 Ni21 123.6(6) . . ? O010 O004 O009 123(7) . . ? O010 O004 O008 64(6) . . ? O009 O004 O008 104(4) . . ? O010 O008 O01X 123(3) . . ? O010 O008 O004 30(2) . . ? O01X O008 O004 136(4) . . ? O004 O009 O010 22(3) . . ? O004 O010 O008 86(6) . . ? O004 O010 O009 35(5) . . ? O008 O010 O009 87(3) . . ? O005 O01X O008 141(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.850 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.102 data_nipyb _database_code_depnum_ccdc_archive 'CCDC 246450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H15 N5 Ni O2' _chemical_formula_weight 404.07 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' Ni Ni 0.3393 1.1124 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1769(4) _cell_length_b 21.8946(13) _cell_length_c 10.2138(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.0290(10) _cell_angle_gamma 90.00 _cell_volume 1604.95(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4539 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10218 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.14 _reflns_number_total 3941 _reflns_number_gt 2688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0371P)^2^+0.3256P] 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 3941 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 Ni1 Ni 0.18850(5) 0.452999(16) 0.54301(4) 0.01657(11) Uani 1 1 d . . . N1 N 0.2777(3) 0.50720(10) 0.4078(2) 0.0171(5) Uani 1 1 d . . . C2 C 0.2950(4) 0.49726(13) 0.2774(3) 0.0210(6) Uani 1 1 d . . . H2A H 0.2634 0.4581 0.2443 0.025 Uiso 1 1 calc R . . C3 C 0.3555(4) 0.54045(14) 0.1909(3) 0.0253(7) Uani 1 1 d . . . H3A H 0.3623 0.5316 0.1000 0.030 Uiso 1 1 calc R . . C4 C 0.4067(4) 0.59722(14) 0.2377(3) 0.0255(7) Uani 1 1 d . . . H4A H 0.4509 0.6279 0.1797 0.031 Uiso 1 1 calc R . . C5 C 0.3924(4) 0.60878(14) 0.3710(3) 0.0234(7) Uani 1 1 d . . . H5A H 0.4274 0.6475 0.4050 0.028 Uiso 1 1 calc R . . C6 C 0.3271(4) 0.56374(12) 0.4540(3) 0.0175(6) Uani 1 1 d . . . C7 C 0.3092(4) 0.57339(12) 0.5978(3) 0.0186(6) Uani 1 1 d . . . H7A H 0.4326 0.5822 0.6368 0.022 Uiso 1 1 calc R . . H7B H 0.2253 0.6083 0.6159 0.022 Uiso 1 1 calc R . . N8 N 0.2329(3) 0.51777(10) 0.6527(2) 0.0196(5) Uani 1 1 d . . . C9 C 0.2066(4) 0.51160(13) 0.7819(3) 0.0201(6) Uani 1 1 d . . . O10 O 0.2300(3) 0.54977(9) 0.8690(2) 0.0302(5) Uani 1 1 d . . . C11 C 0.1414(4) 0.44738(13) 0.8087(3) 0.0196(6) Uani 1 1 d . . . N12 N 0.1240(3) 0.41561(10) 0.6971(2) 0.0175(5) Uani 1 1 d . . . C13 C 0.0722(4) 0.35707(13) 0.6953(3) 0.0185(6) Uani 1 1 d . . . C14 C 0.0360(4) 0.32682(14) 0.8116(3) 0.0247(7) Uani 1 1 d . . . H14A H -0.0005 0.2851 0.8112 0.030 Uiso 1 1 calc R . . C15 C 0.0540(4) 0.35843(14) 0.9285(3) 0.0264(7) Uani 1 1 d . . . H15A H 0.0308 0.3383 1.0093 0.032 Uiso 1 1 calc R . . C16 C 0.1059(4) 0.41945(15) 0.9274(3) 0.0252(7) Uani 1 1 d . . . H16A H 0.1168 0.4417 1.0069 0.030 Uiso 1 1 calc R . . C17 C 0.0638(4) 0.33272(13) 0.5584(3) 0.0220(7) Uani 1 1 d . . . O18 O 0.0067(3) 0.27994(9) 0.5366(2) 0.0305(5) Uani 1 1 d . . . N19 N 0.1220(3) 0.37448(11) 0.4702(2) 0.0186(5) Uani 1 1 d . . . C20 C 0.1160(4) 0.35328(13) 0.3338(3) 0.0210(7) Uani 1 1 d . . . H20A H 0.0779 0.3876 0.2767 0.025 Uiso 1 1 calc R . . H20B H 0.0208 0.3208 0.3256 0.025 Uiso 1 1 calc R . . C21 C 0.3021(4) 0.32869(13) 0.2868(3) 0.0209(7) Uani 1 1 d . . . N22 N 0.3637(4) 0.35095(11) 0.1721(2) 0.0249(6) Uani 1 1 d . . . C23 C 0.5271(5) 0.32932(15) 0.1284(3) 0.0300(8) Uani 1 1 d . . . H23A H 0.5716 0.3444 0.0470 0.036 Uiso 1 1 calc R . . C24 C 0.6352(4) 0.28690(14) 0.1929(3) 0.0289(8) Uani 1 1 d . . . H24A H 0.7494 0.2728 0.1570 0.035 Uiso 1 1 calc R . . C25 C 0.5705(4) 0.26561(14) 0.3121(3) 0.0283(8) Uani 1 1 d . . . H25A H 0.6417 0.2369 0.3608 0.034 Uiso 1 1 calc R . . C26 C 0.4020(4) 0.28628(13) 0.3600(3) 0.0253(7) Uani 1 1 d . . . H26A H 0.3552 0.2718 0.4412 0.030 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 Ni1 0.01782(18) 0.01711(19) 0.01479(19) -0.00030(18) 0.00005(14) -0.00053(17) N1 0.0154(12) 0.0201(13) 0.0158(12) 0.0004(10) -0.0033(10) 0.0025(10) C2 0.0212(15) 0.0221(15) 0.0198(16) -0.0014(13) -0.0012(13) 0.0035(12) C3 0.0269(16) 0.0331(18) 0.0160(15) 0.0016(14) 0.0011(13) 0.0048(14) C4 0.0313(18) 0.0239(17) 0.0213(17) 0.0078(14) 0.0026(14) 0.0007(14) C5 0.0220(16) 0.0205(16) 0.0277(18) 0.0024(14) 0.0002(14) 0.0004(13) C6 0.0126(13) 0.0193(14) 0.0205(15) 0.0003(12) -0.0015(12) 0.0038(11) C7 0.0202(15) 0.0150(14) 0.0207(16) -0.0015(12) 0.0011(13) 0.0009(12) N8 0.0249(14) 0.0162(12) 0.0178(13) -0.0014(10) 0.0009(11) -0.0002(10) C9 0.0211(15) 0.0218(16) 0.0175(15) -0.0020(13) -0.0008(13) 0.0022(12) O10 0.0427(13) 0.0259(12) 0.0218(11) -0.0068(10) 0.0030(10) -0.0056(11) C11 0.0182(14) 0.0231(16) 0.0176(14) -0.0011(13) 0.0013(12) 0.0047(13) N12 0.0165(12) 0.0169(12) 0.0192(13) 0.0015(10) 0.0004(10) 0.0018(10) C13 0.0142(14) 0.0171(15) 0.0241(16) 0.0021(12) 0.0017(13) 0.0018(12) C14 0.0216(16) 0.0230(16) 0.0295(18) 0.0051(14) -0.0008(14) -0.0012(13) C15 0.0258(17) 0.0318(18) 0.0217(17) 0.0101(14) -0.0015(14) -0.0025(14) C16 0.0267(17) 0.0333(18) 0.0156(16) 0.0047(14) -0.0001(13) -0.0016(14) C17 0.0194(15) 0.0224(16) 0.0243(17) -0.0006(13) 0.0014(13) 0.0007(13) O18 0.0379(13) 0.0206(12) 0.0329(13) -0.0040(10) 0.0058(11) -0.0091(10) N19 0.0172(12) 0.0207(13) 0.0180(13) -0.0016(10) 0.0004(10) -0.0017(10) C20 0.0205(15) 0.0199(15) 0.0225(16) -0.0047(13) -0.0029(13) -0.0002(12) C21 0.0218(15) 0.0215(15) 0.0195(16) -0.0075(13) -0.0016(13) -0.0009(13) N22 0.0270(14) 0.0288(15) 0.0187(14) -0.0040(11) -0.0015(12) 0.0017(12) C23 0.0379(19) 0.0358(19) 0.0164(16) -0.0048(14) 0.0050(15) -0.0017(16) C24 0.0252(17) 0.0270(18) 0.0345(19) -0.0065(15) 0.0044(15) 0.0032(14) C25 0.0279(17) 0.0213(16) 0.036(2) 0.0015(15) 0.0005(16) 0.0049(14) C26 0.0282(17) 0.0220(16) 0.0257(17) 0.0037(14) 0.0044(14) 0.0001(13) _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 Ni1 N12 1.834(2) . Y Ni1 N8 1.835(2) . y Ni1 N1 1.930(2) . y Ni1 N19 1.933(2) . y N1 C2 1.356(4) . ? N1 C6 1.371(3) . ? C2 C3 1.365(4) . ? C3 C4 1.381(4) . ? C4 C5 1.389(4) . ? C5 C6 1.383(4) . ? C6 C7 1.489(4) . ? C7 N8 1.448(3) . ? N8 C9 1.340(4) . ? C9 O10 1.232(3) . ? C9 C11 1.507(4) . ? C11 N12 1.341(4) . ? C11 C16 1.382(4) . ? N12 C13 1.335(3) . ? C13 C14 1.384(4) . ? C13 C17 1.498(4) . ? C14 C15 1.386(4) . ? C15 C16 1.387(4) . ? C17 O18 1.246(3) . ? C17 N19 1.350(4) . ? N19 C20 1.469(4) . ? C20 C21 1.518(4) . ? C21 N22 1.344(4) . ? C21 C26 1.390(4) . ? N22 C23 1.341(4) . ? C23 C24 1.377(4) . ? C24 C25 1.384(4) . ? C25 C26 1.381(4) . ? 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 N12 Ni1 N8 82.22(10) . . y N12 Ni1 N1 166.52(10) . . y N8 Ni1 N1 84.51(10) . . y N12 Ni1 N19 82.59(10) . . y N8 Ni1 N19 164.80(10) . . y N1 Ni1 N19 110.69(10) . . y C2 N1 C6 117.3(3) . . ? C2 N1 Ni1 129.4(2) . . ? C6 N1 Ni1 113.24(18) . . ? C3 C2 N1 123.7(3) . . ? C2 C3 C4 118.9(3) . . ? C3 C4 C5 118.9(3) . . ? C6 C5 C4 119.8(3) . . ? N1 C6 C5 121.4(3) . . ? N1 C6 C7 116.4(2) . . ? C5 C6 C7 122.2(3) . . ? N8 C7 C6 107.2(2) . . ? C9 N8 C7 121.3(2) . . ? C9 N8 Ni1 119.9(2) . . ? C7 N8 Ni1 118.60(18) . . ? O10 C9 N8 128.6(3) . . ? O10 C9 C11 123.0(3) . . ? N8 C9 C11 108.4(2) . . ? N12 C11 C16 119.9(3) . . ? N12 C11 C9 111.0(2) . . ? C16 C11 C9 129.0(3) . . ? C13 N12 C11 122.4(3) . . ? C13 N12 Ni1 119.2(2) . . ? C11 N12 Ni1 118.32(19) . . ? N12 C13 C14 120.0(3) . . ? N12 C13 C17 111.4(2) . . ? C14 C13 C17 128.5(3) . . ? C13 C14 C15 118.9(3) . . ? C14 C15 C16 119.9(3) . . ? C11 C16 C15 118.9(3) . . ? O18 C17 N19 127.6(3) . . ? O18 C17 C13 120.7(3) . . ? N19 C17 C13 111.7(2) . . ? C17 N19 C20 114.2(2) . . ? C17 N19 Ni1 114.92(19) . . ? C20 N19 Ni1 130.77(19) . . ? N19 C20 C21 112.7(2) . . ? N22 C21 C26 122.7(3) . . ? N22 C21 C20 115.9(3) . . ? C26 C21 C20 121.4(3) . . ? C21 N22 C23 116.7(3) . . ? N22 C23 C24 124.8(3) . . ? C23 C24 C25 117.3(3) . . ? C24 C25 C26 119.7(3) . . ? C25 C26 C21 118.7(3) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.372 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.089 data_nipyr _database_code_depnum_ccdc_archive 'CCDC 246451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 N10 Ni3 O12' _chemical_formula_weight 1113.11 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.5075(7) _cell_length_b 9.0184(3) _cell_length_c 22.3163(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4731.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prisms _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 28704 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.09 _reflns_number_total 5990 _reflns_number_gt 3716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0470P)^2^+5.6000P] 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 SHELXL _refine_ls_extinction_coef 0.00033(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5990 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.011 _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 Ni1 Ni 0.406351(18) 0.89583(5) 0.156159(19) 0.02273(13) Uani 1 1 d . . . Ni2 Ni 0.5000 0.89854(7) 0.2500 0.01889(15) Uani 1 2 d S . . N1 N 0.35112(12) 1.0098(3) 0.20906(13) 0.0243(7) Uani 1 1 d . . . C2 C 0.29680(15) 0.9690(4) 0.22030(16) 0.0292(8) Uani 1 1 d . . . H2A H 0.2828 0.8800 0.2030 0.035 Uiso 1 1 calc R . . C3 C 0.26128(16) 1.0516(4) 0.25585(18) 0.0348(9) Uani 1 1 d . . . H3A H 0.2231 1.0213 0.2625 0.042 Uiso 1 1 calc R . . C4 C 0.28206(17) 1.1792(4) 0.28179(19) 0.0392(10) Uani 1 1 d . . . H4A H 0.2586 1.2363 0.3076 0.047 Uiso 1 1 calc R . . C5 C 0.33698(16) 1.2238(4) 0.27011(18) 0.0335(9) Uani 1 1 d . . . H5A H 0.3519 1.3119 0.2873 0.040 Uiso 1 1 calc R . . C6 C 0.36995(15) 1.1368(4) 0.23265(16) 0.0240(8) Uani 1 1 d . . . C7 C 0.42843(15) 1.1871(4) 0.21410(17) 0.0261(8) Uani 1 1 d . . . H7A H 0.4247 1.2639 0.1826 0.031 Uiso 1 1 calc R . . H7B H 0.4475 1.2332 0.2490 0.031 Uiso 1 1 calc R . . N8 N 0.46412(12) 1.0664(3) 0.19134(13) 0.0229(6) Uani 1 1 d . . . C9 C 0.50473(15) 1.1173(4) 0.15282(16) 0.0263(8) Uani 1 1 d . . . O10 O 0.50566(12) 1.2399(3) 0.12818(12) 0.0394(7) Uani 1 1 d . . . C11 C 0.55454(14) 1.0155(4) 0.14449(15) 0.0238(8) Uani 1 1 d . . . N12 N 0.55775(11) 0.9067(3) 0.18567(12) 0.0216(6) Uani 1 1 d . . . C13 C 0.60051(14) 0.8102(4) 0.18592(16) 0.0252(8) Uani 1 1 d . . . C14 C 0.64290(16) 0.8179(5) 0.14292(16) 0.0330(9) Uani 1 1 d . . . H14A H 0.6726 0.7465 0.1420 0.040 Uiso 1 1 calc R . . C15 C 0.64099(16) 0.9318(5) 0.10130(17) 0.0366(10) Uani 1 1 d . . . H15A H 0.6703 0.9411 0.0723 0.044 Uiso 1 1 calc R . . C16 C 0.59680(16) 1.0313(5) 0.10199(16) 0.0325(9) Uani 1 1 d . . . H16A H 0.5953 1.1098 0.0736 0.039 Uiso 1 1 calc R . . C17 C 0.59532(15) 0.6935(4) 0.23402(16) 0.0256(8) Uani 1 1 d . . . O18 O 0.61884(12) 0.5722(3) 0.22642(12) 0.0388(7) Uani 1 1 d . . . N19 N 0.56046(12) 0.7331(3) 0.27990(13) 0.0228(6) Uani 1 1 d . . . C20 C 0.54521(16) 0.6055(4) 0.31772(16) 0.0285(8) Uani 1 1 d . . . H20A H 0.5797 0.5460 0.3260 0.034 Uiso 1 1 calc R . . H20B H 0.5179 0.5417 0.2959 0.034 Uiso 1 1 calc R . . C21 C 0.51920(15) 0.6543(4) 0.37597(16) 0.0258(8) Uani 1 1 d . . . N22 N 0.53846(12) 0.7833(3) 0.39836(12) 0.0247(7) Uani 1 1 d . . . C23 C 0.51940(16) 0.8280(4) 0.45217(16) 0.0296(8) Uani 1 1 d . . . H23A H 0.5330 0.9191 0.4679 0.036 Uiso 1 1 calc R . . C24 C 0.48115(17) 0.7479(4) 0.48533(18) 0.0363(10) Uani 1 1 d . . . H24A H 0.4693 0.7813 0.5237 0.044 Uiso 1 1 calc R . . C25 C 0.46022(18) 0.6172(4) 0.46154(18) 0.0391(10) Uani 1 1 d . . . H25A H 0.4329 0.5605 0.4829 0.047 Uiso 1 1 calc R . . C26 C 0.47960(17) 0.5702(4) 0.40636(17) 0.0338(9) Uani 1 1 d . . . H26A H 0.4658 0.4805 0.3894 0.041 Uiso 1 1 calc R . . O011 O 0.34521(11) 0.7414(3) 0.13506(11) 0.0313(6) Uani 1 1 d . . . O012 O 0.32490(13) 0.7945(3) 0.03937(13) 0.0484(8) Uani 1 1 d . . . C011 C 0.32491(16) 0.7090(4) 0.08431(19) 0.0340(9) Uani 1 1 d . . . C012 C 0.3010(2) 0.5547(5) 0.0780(2) 0.0500(12) Uani 1 1 d . . . H01A H 0.2855 0.5220 0.1166 0.075 Uiso 1 1 calc R . . H01B H 0.3312 0.4867 0.0654 0.075 Uiso 1 1 calc R . . H01C H 0.2706 0.5549 0.0479 0.075 Uiso 1 1 calc R . . O021 O 0.38159(12) 1.0235(3) 0.07925(12) 0.0329(7) Uani 1 1 d . . . H021 H 0.360(2) 0.972(5) 0.064(2) 0.049 Uiso 1 1 d . . . C021 C 0.35376(19) 1.1639(4) 0.07730(19) 0.0406(10) Uani 1 1 d . . . H02A H 0.3392 1.1817 0.0368 0.061 Uiso 1 1 calc R . . H02B H 0.3809 1.2421 0.0880 0.061 Uiso 1 1 calc R . . H02C H 0.3221 1.1644 0.1058 0.061 Uiso 1 1 calc R . . O031 O 0.27200(16) 0.6969(4) -0.06561(15) 0.0665(10) Uani 1 1 d . . . H031 H 0.2863 0.7308 -0.0339 0.100 Uiso 1 1 calc R . . C031 C 0.3058(3) 0.5763(6) -0.0868(2) 0.0741(17) Uani 1 1 d . . . H03A H 0.3455 0.6080 -0.0901 0.111 Uiso 1 1 calc R . . H03B H 0.2919 0.5447 -0.1261 0.111 Uiso 1 1 calc R . . H03C H 0.3031 0.4934 -0.0585 0.111 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 Ni1 0.0231(2) 0.0207(2) 0.0244(2) 0.0019(2) -0.00292(18) -0.0017(2) Ni2 0.0180(3) 0.0172(3) 0.0215(3) 0.000 0.0003(2) 0.000 N1 0.0214(16) 0.0247(16) 0.0267(16) 0.0052(13) -0.0017(12) 0.0000(13) C2 0.023(2) 0.032(2) 0.033(2) 0.0072(17) -0.0041(16) -0.0054(16) C3 0.023(2) 0.035(2) 0.046(2) 0.0100(19) 0.0016(17) 0.0035(16) C4 0.032(2) 0.033(2) 0.053(3) 0.003(2) 0.0079(19) 0.0099(19) C5 0.032(2) 0.0214(19) 0.047(2) -0.0009(17) 0.0014(18) 0.0011(16) C6 0.0237(19) 0.0192(18) 0.0292(19) 0.0049(14) 0.0008(15) 0.0032(14) C7 0.0252(19) 0.0178(17) 0.035(2) 0.0035(16) 0.0004(16) 0.0001(15) N8 0.0196(15) 0.0215(15) 0.0275(16) 0.0015(12) -0.0007(12) -0.0007(12) C9 0.0269(19) 0.0244(19) 0.0275(18) 0.0020(16) -0.0053(15) -0.0044(16) O10 0.0438(17) 0.0299(15) 0.0446(17) 0.0150(13) 0.0069(13) 0.0001(13) C11 0.0212(18) 0.0251(19) 0.0251(19) -0.0005(15) -0.0015(14) -0.0080(15) N12 0.0203(15) 0.0227(15) 0.0219(14) -0.0022(13) -0.0024(11) -0.0025(13) C13 0.0180(18) 0.0309(19) 0.0267(19) -0.0084(16) -0.0030(14) -0.0001(15) C14 0.0230(19) 0.047(2) 0.029(2) -0.0129(19) -0.0008(16) 0.0017(18) C15 0.021(2) 0.062(3) 0.027(2) -0.0073(19) 0.0068(16) -0.0095(19) C16 0.032(2) 0.042(2) 0.0233(19) -0.0002(17) 0.0017(16) -0.0131(19) C17 0.0251(19) 0.0250(18) 0.0267(19) -0.0054(15) -0.0075(15) 0.0039(16) O18 0.0409(17) 0.0290(15) 0.0466(17) -0.0093(13) -0.0027(13) 0.0144(12) N19 0.0251(16) 0.0189(15) 0.0243(16) -0.0033(12) -0.0011(12) 0.0030(12) C20 0.037(2) 0.0194(17) 0.0288(19) -0.0019(16) -0.0022(16) 0.0064(17) C21 0.030(2) 0.0188(17) 0.029(2) 0.0031(15) -0.0061(16) 0.0056(15) N22 0.0277(16) 0.0226(15) 0.0240(16) 0.0002(13) -0.0036(13) 0.0021(13) C23 0.033(2) 0.029(2) 0.026(2) -0.0043(16) -0.0022(16) 0.0001(17) C24 0.042(2) 0.038(2) 0.029(2) 0.0023(18) 0.0029(17) 0.0037(19) C25 0.043(2) 0.034(2) 0.040(2) 0.0111(19) 0.0014(19) -0.003(2) C26 0.039(2) 0.025(2) 0.037(2) 0.0066(17) -0.0045(18) -0.0001(17) O011 0.0306(15) 0.0295(14) 0.0338(15) -0.0031(12) -0.0066(12) -0.0064(11) O012 0.070(2) 0.0369(17) 0.0385(17) -0.0004(14) -0.0215(15) -0.0034(15) C011 0.027(2) 0.034(2) 0.041(2) -0.0072(19) -0.0039(17) -0.0001(17) C012 0.055(3) 0.047(3) 0.048(3) -0.009(2) -0.004(2) -0.016(2) O021 0.0377(17) 0.0293(16) 0.0318(15) 0.0032(12) -0.0068(12) 0.0022(12) C021 0.047(3) 0.034(2) 0.040(2) 0.0053(19) -0.003(2) 0.009(2) O031 0.077(3) 0.064(2) 0.059(2) -0.0135(19) -0.0330(19) 0.006(2) C031 0.117(5) 0.062(4) 0.044(3) -0.008(3) 0.001(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.034(3) . y Ni1 N22 2.048(3) 3_655 y Ni1 O011 2.056(2) . y Ni1 O021 2.147(3) . y Ni1 N19 2.191(3) 3_655 y Ni1 N8 2.197(3) . y Ni2 N12 1.977(3) . y Ni2 N12 1.977(3) 3_655 ? Ni2 N19 2.166(3) 3_655 ? Ni2 N19 2.166(3) . y Ni2 N8 2.172(3) . y Ni2 N8 2.172(3) 3_655 ? N1 C6 1.335(4) . ? N1 C2 1.352(4) . ? C2 C3 1.372(5) . ? C3 C4 1.378(6) . ? C4 C5 1.377(5) . ? C5 C6 1.384(5) . ? C6 C7 1.506(5) . ? C7 N8 1.465(4) . ? N8 C9 1.364(4) . ? C9 O10 1.235(4) . ? C9 C11 1.500(5) . ? C11 N12 1.347(4) . ? C11 C16 1.381(5) . ? N12 C13 1.329(4) . ? C13 C14 1.385(5) . ? C13 C17 1.508(5) . ? C14 C15 1.386(6) . ? C15 C16 1.373(6) . ? C17 O18 1.237(4) . ? C17 N19 1.359(4) . ? N19 C20 1.472(4) . ? N19 Ni1 2.190(3) 3_655 ? C20 C21 1.502(5) . ? C21 N22 1.345(4) . ? C21 C26 1.379(5) . ? N22 C23 1.343(4) . ? N22 Ni1 2.048(3) 3_655 ? C23 C24 1.370(5) . ? C24 C25 1.383(6) . ? C25 C26 1.380(6) . ? O011 C011 1.263(4) . ? O012 C011 1.265(5) . ? C011 C012 1.508(6) . ? O021 C021 1.425(5) . ? O031 C031 1.427(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N22 178.99(11) . 3_655 y N1 Ni1 O011 91.67(11) . . y N22 Ni1 O011 88.35(11) 3_655 . y N1 Ni1 O021 91.13(11) . . y N22 Ni1 O021 87.86(11) 3_655 . y O011 Ni1 O021 89.48(10) . . y N1 Ni1 N19 100.83(11) . 3_655 y N22 Ni1 N19 80.18(11) 3_655 3_655 y O011 Ni1 N19 86.81(10) . 3_655 y O021 Ni1 N19 167.56(11) . 3_655 y N1 Ni1 N8 80.40(11) . . y N22 Ni1 N8 99.65(11) 3_655 . y O011 Ni1 N8 171.20(10) . . y O021 Ni1 N8 94.45(10) . . y N19 Ni1 N8 90.92(10) 3_655 . y N12 Ni2 N12 175.76(17) . 3_655 y N12 Ni2 N19 104.62(11) . 3_655 y N12 Ni2 N19 78.38(11) 3_655 3_655 ? N12 Ni2 N19 78.38(11) . . y N12 Ni2 N19 104.62(11) 3_655 . y N19 Ni2 N19 92.93(15) 3_655 . y N12 Ni2 N8 78.65(11) . . y N12 Ni2 N8 98.35(11) 3_655 . y N19 Ni2 N8 92.27(10) 3_655 . y N19 Ni2 N8 157.03(11) . . y N12 Ni2 N8 98.35(11) . 3_655 ? N12 Ni2 N8 78.65(11) 3_655 3_655 ? N19 Ni2 N8 157.03(11) 3_655 3_655 ? N19 Ni2 N8 92.27(10) . 3_655 ? N8 Ni2 N8 91.62(15) . 3_655 y C6 N1 C2 118.2(3) . . ? C6 N1 Ni1 116.8(2) . . ? C2 N1 Ni1 124.9(2) . . ? N1 C2 C3 122.3(4) . . ? C2 C3 C4 118.7(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 118.3(4) . . ? N1 C6 C5 122.6(3) . . ? N1 C6 C7 116.9(3) . . ? C5 C6 C7 120.4(3) . . ? N8 C7 C6 113.2(3) . . ? C9 N8 C7 111.7(3) . . ? C9 N8 Ni2 110.0(2) . . ? C7 N8 Ni2 122.1(2) . . ? C9 N8 Ni1 116.3(2) . . ? C7 N8 Ni1 106.9(2) . . ? Ni2 N8 Ni1 88.13(10) . . ? O10 C9 N8 126.5(3) . . ? O10 C9 C11 118.6(3) . . ? N8 C9 C11 114.7(3) . . ? N12 C11 C16 120.2(3) . . ? N12 C11 C9 113.9(3) . . ? C16 C11 C9 125.7(3) . . ? C13 N12 C11 121.5(3) . . ? C13 N12 Ni2 119.5(2) . . ? C11 N12 Ni2 118.9(2) . . ? N12 C13 C14 120.6(3) . . ? N12 C13 C17 113.5(3) . . ? C14 C13 C17 125.9(3) . . ? C13 C14 C15 118.5(4) . . ? C16 C15 C14 120.1(3) . . ? C15 C16 C11 119.0(4) . . ? O18 C17 N19 127.2(3) . . ? O18 C17 C13 118.9(3) . . ? N19 C17 C13 113.7(3) . . ? C17 N19 C20 111.9(3) . . ? C17 N19 Ni2 110.2(2) . . ? C20 N19 Ni2 123.7(2) . . ? C17 N19 Ni1 116.9(2) . 3_655 ? C20 N19 Ni1 103.7(2) . 3_655 ? Ni2 N19 Ni1 88.45(10) . 3_655 ? N19 C20 C21 111.5(3) . . ? N22 C21 C26 121.4(3) . . ? N22 C21 C20 116.0(3) . . ? C26 C21 C20 122.6(3) . . ? C23 N22 C21 118.6(3) . . ? C23 N22 Ni1 126.4(2) . 3_655 ? C21 N22 Ni1 114.9(2) . 3_655 ? N22 C23 C24 122.9(4) . . ? C23 C24 C25 118.4(4) . . ? C26 C25 C24 119.1(4) . . ? C21 C26 C25 119.5(4) . . ? C011 O011 Ni1 128.7(3) . . ? O011 C011 O012 124.8(4) . . ? O011 C011 C012 116.0(4) . . ? O012 C011 C012 119.2(4) . . ? C021 O021 Ni1 128.7(2) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.260 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.089