Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cupertino, Domenico C.' 'Emeleus, Lucy C.' 'Harris, Steven G.' 'Owens, Susan' 'Parsons, S.' 'Swart, Ronald M.' 'Tasker, P.' 'White, David J.' _publ_contact_author_name 'Prof P Tasker' _publ_contact_author_address ; Prof P Tasker Department of Chemistry University of Edinburgh West Mains Road Edinburgh EH9 3JJ UK ; data_lce131 _database_code_CSD 158372 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu(C20H21N4O)2] _chemical_formula_sum 'C40 H42 Cu N8 O2' _chemical_formula_weight 730.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.603(3) _cell_length_b 23.586(4) _cell_length_c 13.649(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.24(2) _cell_angle_gamma 90.00 _cell_volume 3705.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description lump _exptl_crystal_colour Red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.275 _exptl_absorpt_correction_T_max 0.587 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 5432 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 60.14 _reflns_number_total 5432 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+0.2796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5432 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.03636(5) 0.11888(2) 0.37547(4) 0.0410(2) Uani 1 1 d . . . N1A N 0.0832(3) 0.02814(14) 0.6314(2) 0.0438(8) Uani 1 1 d . . . C11A C 0.1977(4) 0.01916(16) 0.6762(3) 0.0469(10) Uani 1 1 d . . . C12A C 0.2163(5) -0.0010(2) 0.7726(3) 0.0614(13) Uani 1 1 d . . . H12A H 0.1526 -0.0088 0.8067 0.074 Uiso 1 1 calc R . . C13A C 0.3267(5) -0.0095(2) 0.8179(4) 0.0758(16) Uani 1 1 d . . . H13A H 0.3386 -0.0229 0.8833 0.091 Uiso 1 1 calc R . . C14A C 0.4208(5) 0.0014(2) 0.7688(5) 0.0802(18) Uani 1 1 d . . . H14A H 0.4966 -0.0049 0.8001 0.096 Uiso 1 1 calc R . . C15A C 0.4031(5) 0.0216(2) 0.6729(4) 0.0747(15) Uani 1 1 d . . . H15A H 0.4670 0.0293 0.6390 0.090 Uiso 1 1 calc R . . C16A C 0.2918(4) 0.0302(2) 0.6273(4) 0.0646(13) Uani 1 1 d . . . H16A H 0.2801 0.0439 0.5621 0.078 Uiso 1 1 calc R . . N2A N -0.0106(3) 0.00570(14) 0.6763(2) 0.0479(9) Uani 1 1 d . . . C3A C -0.1055(4) 0.02653(16) 0.6271(3) 0.0435(10) Uani 1 1 d . . . C31A C -0.2214(4) 0.01202(19) 0.6530(4) 0.0613(13) Uani 1 1 d . . . H31A H -0.2652 -0.0079 0.5984 0.092 Uiso 1 1 calc R . . H31B H -0.2621 0.0465 0.6667 0.092 Uiso 1 1 calc R . . H31C H -0.2131 -0.0121 0.7111 0.092 Uiso 1 1 calc R . . C4A C -0.0783(3) 0.06232(15) 0.5477(3) 0.0383(9) Uani 1 1 d . . . N41A N -0.1554(3) 0.09454(13) 0.4908(2) 0.0401(8) Uani 1 1 d . . . N42A N -0.1167(3) 0.12502(13) 0.4232(2) 0.0394(7) Uani 1 1 d . . . C43A C -0.2023(3) 0.16249(16) 0.3745(3) 0.0383(9) Uani 1 1 d . . . C44A C -0.1738(4) 0.21898(18) 0.3685(3) 0.0469(10) Uani 1 1 d . . . H44A H -0.0985 0.2314 0.3926 0.056 Uiso 1 1 calc R . . C45A C -0.2557(4) 0.25738(18) 0.3270(3) 0.0492(11) Uani 1 1 d . . . H45A H -0.2353 0.2959 0.3248 0.059 Uiso 1 1 calc R . . C46A C -0.3661(4) 0.24110(18) 0.2888(3) 0.0464(10) Uani 1 1 d . . . C47A C -0.3904(4) 0.18311(19) 0.2917(3) 0.0504(11) Uani 1 1 d . . . H47A H -0.4639 0.1701 0.2641 0.060 Uiso 1 1 calc R . . C48A C -0.3099(4) 0.14444(18) 0.3339(3) 0.0477(10) Uani 1 1 d . . . H48A H -0.3290 0.1057 0.3348 0.057 Uiso 1 1 calc R . . C49A C -0.4612(4) 0.28339(19) 0.2500(3) 0.0516(11) Uani 1 1 d . . . C50A C -0.5113(5) 0.2683(3) 0.1442(4) 0.0808(17) Uani 1 1 d . . . H50A H -0.5400 0.2296 0.1422 0.121 Uiso 1 1 calc R . . H50B H -0.4510 0.2717 0.1013 0.121 Uiso 1 1 calc R . . H50C H -0.5746 0.2939 0.1219 0.121 Uiso 1 1 calc R . . C51A C -0.4169(5) 0.3439(2) 0.2513(5) 0.0777(16) Uani 1 1 d . . . H51A H -0.3849 0.3541 0.3180 0.117 Uiso 1 1 calc R . . H51B H -0.4806 0.3693 0.2286 0.117 Uiso 1 1 calc R . . H51C H -0.3570 0.3471 0.2080 0.117 Uiso 1 1 calc R . . C52A C -0.5575(4) 0.2807(3) 0.3170(4) 0.0782(17) Uani 1 1 d . . . H52A H -0.5875 0.2423 0.3176 0.117 Uiso 1 1 calc R . . H52B H -0.6198 0.3064 0.2923 0.117 Uiso 1 1 calc R . . H52C H -0.5263 0.2916 0.3836 0.117 Uiso 1 1 calc R . . C5A C 0.0442(3) 0.06183(15) 0.5529(3) 0.0384(9) Uani 1 1 d . . . O51A O 0.1087(2) 0.08798(12) 0.49902(19) 0.0444(7) Uani 1 1 d . . . N1B N -0.0239(3) 0.10555(16) 0.0771(2) 0.0523(9) Uani 1 1 d . . . C11B C -0.1397(4) 0.1053(2) 0.0341(3) 0.0546(12) Uani 1 1 d . . . C12B C -0.1718(5) 0.0724(2) -0.0503(3) 0.0706(14) Uani 1 1 d . . . H12B H -0.1162 0.0506 -0.0778 0.085 Uiso 1 1 calc R . . C13B C -0.2848(5) 0.0723(3) -0.0919(4) 0.0820(17) Uani 1 1 d . . . H13B H -0.3059 0.0502 -0.1486 0.098 Uiso 1 1 calc R . . C14B C -0.3690(6) 0.1034(3) -0.0542(4) 0.0827(17) Uani 1 1 d . . . H14B H -0.4467 0.1026 -0.0839 0.099 Uiso 1 1 calc R . . C15B C -0.3355(5) 0.1358(2) 0.0290(4) 0.0718(14) Uani 1 1 d . . . H15B H -0.3913 0.1579 0.0558 0.086 Uiso 1 1 calc R . . C16B C -0.2236(4) 0.1365(2) 0.0729(4) 0.0622(13) Uani 1 1 d . . . H16B H -0.2034 0.1583 0.1300 0.075 Uiso 1 1 calc R . . N2B N 0.0658(4) 0.09605(17) 0.0177(3) 0.0621(11) Uani 1 1 d . . . C3B C 0.1623(4) 0.1013(2) 0.0757(3) 0.0571(12) Uani 1 1 d . . . C31B C 0.2783(5) 0.0965(3) 0.0381(4) 0.0801(17) Uani 1 1 d . . . H31D H 0.3279 0.0710 0.0802 0.120 Uiso 1 1 calc R . . H31E H 0.3143 0.1336 0.0386 0.120 Uiso 1 1 calc R . . H31F H 0.2675 0.0818 -0.0288 0.120 Uiso 1 1 calc R . . C4B C 0.1434(4) 0.11266(17) 0.1756(3) 0.0450(10) Uani 1 1 d . . . N41B N 0.2256(3) 0.12444(13) 0.2506(2) 0.0445(8) Uani 1 1 d . . . N42B N 0.1919(3) 0.13418(13) 0.3371(2) 0.0416(8) Uani 1 1 d . . . C43B C 0.2850(3) 0.14824(17) 0.4107(3) 0.0408(9) Uani 1 1 d . . . C44B C 0.2663(4) 0.18856(18) 0.4806(3) 0.0473(10) Uani 1 1 d . . . H44B H 0.1930 0.2059 0.4782 0.057 Uiso 1 1 calc R . . C45B C 0.3534(4) 0.20344(18) 0.5531(3) 0.0515(11) Uani 1 1 d . . . H45B H 0.3381 0.2309 0.5997 0.062 Uiso 1 1 calc R . . C46B C 0.4636(3) 0.17962(16) 0.5604(3) 0.0432(10) Uani 1 1 d . . . C47B C 0.4801(3) 0.13782(18) 0.4896(3) 0.0444(10) Uani 1 1 d . . . H47B H 0.5527 0.1198 0.4923 0.053 Uiso 1 1 calc R . . C48B C 0.3934(4) 0.12291(17) 0.4171(3) 0.0461(10) Uani 1 1 d . . . H48B H 0.4074 0.0950 0.3709 0.055 Uiso 1 1 calc R . . C49B C 0.5643(4) 0.19880(18) 0.6353(3) 0.0495(10) Uani 1 1 d . . . C50B C 0.6319(4) 0.2445(2) 0.5862(4) 0.0718(14) Uani 1 1 d . . . H50D H 0.5805 0.2759 0.5655 0.108 Uiso 1 1 calc R . . H50E H 0.6621 0.2285 0.5291 0.108 Uiso 1 1 calc R . . H50F H 0.6959 0.2580 0.6330 0.108 Uiso 1 1 calc R . . C51B C 0.5227(5) 0.2242(3) 0.7274(4) 0.0776(16) Uani 1 1 d . . . H51D H 0.4702 0.2555 0.7086 0.116 Uiso 1 1 calc R . . H51E H 0.5890 0.2379 0.7715 0.116 Uiso 1 1 calc R . . H51F H 0.4824 0.1954 0.7608 0.116 Uiso 1 1 calc R . . C52B C 0.6461(4) 0.1500(2) 0.6672(4) 0.0677(14) Uani 1 1 d . . . H52D H 0.7092 0.1636 0.7149 0.102 Uiso 1 1 calc R . . H52E H 0.6774 0.1348 0.6101 0.102 Uiso 1 1 calc R . . H52F H 0.6039 0.1205 0.6971 0.102 Uiso 1 1 calc R . . C5B C 0.0204(4) 0.11470(17) 0.1734(3) 0.0464(10) Uani 1 1 d . . . O51B O -0.0405(2) 0.12529(12) 0.24225(19) 0.0462(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0481(4) 0.0409(4) 0.0355(3) 0.0060(2) 0.0113(3) 0.0023(3) N1A 0.059(2) 0.0343(18) 0.0384(18) 0.0016(14) 0.0064(16) 0.0030(16) C11A 0.069(3) 0.028(2) 0.041(2) 0.0000(17) -0.002(2) -0.002(2) C12A 0.082(4) 0.053(3) 0.046(3) 0.006(2) -0.003(2) -0.007(2) C13A 0.102(4) 0.062(3) 0.056(3) 0.012(3) -0.018(3) -0.011(3) C14A 0.085(4) 0.057(3) 0.088(4) 0.015(3) -0.032(3) -0.010(3) C15A 0.067(3) 0.064(4) 0.090(4) 0.019(3) -0.001(3) -0.006(3) C16A 0.061(3) 0.065(3) 0.065(3) 0.016(2) -0.001(3) 0.003(2) N2A 0.071(2) 0.0353(19) 0.0408(19) 0.0036(15) 0.0196(18) -0.0013(17) C3A 0.065(3) 0.025(2) 0.044(2) -0.0008(16) 0.019(2) 0.0051(19) C31A 0.077(3) 0.043(3) 0.071(3) 0.013(2) 0.036(3) 0.009(2) C4A 0.053(2) 0.026(2) 0.037(2) -0.0009(16) 0.0114(18) 0.0036(17) N41A 0.052(2) 0.0324(17) 0.0384(18) -0.0017(14) 0.0158(15) -0.0012(15) N42A 0.0450(18) 0.0324(18) 0.0421(18) 0.0020(14) 0.0099(15) 0.0006(14) C43A 0.043(2) 0.037(2) 0.037(2) 0.0026(16) 0.0111(17) 0.0031(18) C44A 0.043(2) 0.046(3) 0.053(3) 0.0054(19) 0.0086(19) -0.0029(19) C45A 0.053(3) 0.036(2) 0.060(3) 0.0121(19) 0.011(2) 0.001(2) C46A 0.050(2) 0.047(3) 0.043(2) 0.0122(18) 0.0122(19) 0.005(2) C47A 0.047(2) 0.052(3) 0.052(3) 0.007(2) 0.003(2) -0.004(2) C48A 0.054(3) 0.038(2) 0.053(3) 0.0021(19) 0.012(2) 0.000(2) C49A 0.053(3) 0.054(3) 0.048(3) 0.016(2) 0.011(2) 0.007(2) C50A 0.090(4) 0.083(4) 0.067(4) 0.018(3) -0.001(3) 0.025(3) C51A 0.080(4) 0.056(3) 0.098(4) 0.026(3) 0.012(3) 0.016(3) C52A 0.066(3) 0.086(4) 0.087(4) 0.028(3) 0.025(3) 0.030(3) C5A 0.058(3) 0.026(2) 0.032(2) -0.0036(15) 0.0099(18) 0.0008(18) O51A 0.0506(16) 0.0443(16) 0.0398(15) 0.0091(12) 0.0114(13) -0.0019(13) N1B 0.068(2) 0.057(2) 0.0327(18) -0.0026(16) 0.0114(17) -0.0031(18) C11B 0.075(3) 0.053(3) 0.036(2) 0.0057(19) 0.006(2) -0.006(2) C12B 0.089(4) 0.079(4) 0.043(3) -0.007(2) 0.007(3) -0.009(3) C13B 0.095(4) 0.105(5) 0.042(3) -0.013(3) -0.007(3) -0.012(4) C14B 0.083(4) 0.101(5) 0.060(3) 0.009(3) -0.005(3) -0.006(3) C15B 0.078(4) 0.073(4) 0.062(3) 0.003(3) -0.002(3) 0.003(3) C16B 0.077(3) 0.057(3) 0.049(3) -0.002(2) -0.007(3) 0.002(3) N2B 0.084(3) 0.063(3) 0.043(2) -0.0041(18) 0.022(2) 0.008(2) C3B 0.071(3) 0.056(3) 0.046(3) -0.001(2) 0.016(2) 0.007(2) C31B 0.079(4) 0.107(5) 0.059(3) -0.003(3) 0.032(3) 0.016(3) C4B 0.056(3) 0.040(2) 0.040(2) 0.0030(17) 0.012(2) 0.0022(19) N41B 0.055(2) 0.0357(19) 0.046(2) 0.0062(15) 0.0180(17) 0.0048(15) N42B 0.0494(19) 0.0348(18) 0.0420(19) 0.0044(14) 0.0114(16) 0.0017(15) C43B 0.044(2) 0.037(2) 0.044(2) 0.0028(17) 0.0124(18) -0.0021(18) C44B 0.046(2) 0.041(2) 0.056(3) -0.0015(19) 0.011(2) 0.0088(19) C45B 0.059(3) 0.040(2) 0.058(3) -0.006(2) 0.018(2) 0.010(2) C46B 0.050(2) 0.035(2) 0.048(2) 0.0027(17) 0.0192(19) -0.0003(18) C47B 0.040(2) 0.044(2) 0.051(2) -0.0011(18) 0.0131(19) 0.0056(18) C48B 0.052(3) 0.040(2) 0.050(2) -0.0013(18) 0.020(2) 0.002(2) C49B 0.052(3) 0.042(2) 0.056(3) -0.003(2) 0.012(2) 0.002(2) C50B 0.076(3) 0.060(3) 0.079(4) -0.004(3) 0.010(3) -0.019(3) C51B 0.074(3) 0.098(4) 0.061(3) -0.024(3) 0.007(3) 0.006(3) C52B 0.067(3) 0.061(3) 0.072(3) -0.009(3) -0.005(3) 0.005(3) C5B 0.063(3) 0.038(2) 0.038(2) 0.0080(17) 0.008(2) 0.002(2) O51B 0.0559(17) 0.0497(17) 0.0344(15) 0.0029(12) 0.0116(13) 0.0026(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 Cu1 O51B 1.928(3) . ? Cu1 O51A 1.930(3) . ? Cu1 N42A 1.972(3) . ? Cu1 N42B 1.974(3) . ? N1A C5A 1.365(5) . ? N1A C11A 1.407(5) . ? N1A N2A 1.418(5) . ? C11A C16A 1.374(6) . ? C11A C12A 1.391(6) . ? C12A C13A 1.366(7) . ? C13A C14A 1.376(8) . ? C14A C15A 1.383(8) . ? C15A C16A 1.376(7) . ? N2A C3A 1.311(5) . ? C3A C4A 1.440(5) . ? C3A C31A 1.474(6) . ? C4A N41A 1.344(5) . ? C4A C5A 1.414(5) . ? N41A N42A 1.294(4) . ? N42A C43A 1.429(5) . ? C43A C48A 1.369(6) . ? C43A C44A 1.378(6) . ? C44A C45A 1.382(6) . ? C45A C46A 1.375(6) . ? C46A C47A 1.398(6) . ? C46A C49A 1.532(6) . ? C47A C48A 1.378(6) . ? C49A C51A 1.517(7) . ? C49A C50A 1.529(7) . ? C49A C52A 1.533(6) . ? C5A O51A 1.273(4) . ? N1B C5B 1.367(5) . ? N1B C11B 1.396(6) . ? N1B N2B 1.415(5) . ? C11B C16B 1.379(7) . ? C11B C12B 1.400(7) . ? C12B C13B 1.361(7) . ? C13B C14B 1.372(8) . ? C14B C15B 1.385(8) . ? C15B C16B 1.359(7) . ? N2B C3B 1.293(6) . ? C3B C4B 1.433(6) . ? C3B C31B 1.504(7) . ? C4B N41B 1.337(5) . ? C4B C5B 1.425(6) . ? N41B N42B 1.311(5) . ? N42B C43B 1.419(5) . ? C43B C44B 1.383(6) . ? C43B C48B 1.385(6) . ? C44B C45B 1.369(6) . ? C45B C46B 1.388(6) . ? C46B C47B 1.411(6) . ? C46B C49B 1.521(6) . ? C47B C48B 1.365(6) . ? C49B C52B 1.520(6) . ? C49B C51B 1.525(6) . ? C49B C50B 1.537(6) . ? C5B O51B 1.269(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O51B Cu1 O51A 162.30(12) . . ? O51B Cu1 N42A 88.68(12) . . ? O51A Cu1 N42A 92.86(12) . . ? O51B Cu1 N42B 93.72(13) . . ? O51A Cu1 N42B 89.38(12) . . ? N42A Cu1 N42B 164.82(13) . . ? C5A N1A C11A 129.1(3) . . ? C5A N1A N2A 111.1(3) . . ? C11A N1A N2A 119.4(3) . . ? C16A C11A C12A 119.1(4) . . ? C16A C11A N1A 121.7(4) . . ? C12A C11A N1A 119.2(4) . . ? C13A C12A C11A 120.2(5) . . ? C12A C13A C14A 120.5(5) . . ? C13A C14A C15A 119.6(5) . . ? C16A C15A C14A 119.9(6) . . ? C11A C16A C15A 120.6(5) . . ? C3A N2A N1A 106.2(3) . . ? N2A C3A C4A 110.9(4) . . ? N2A C3A C31A 121.5(4) . . ? C4A C3A C31A 127.6(4) . . ? N41A C4A C5A 128.7(3) . . ? N41A C4A C3A 125.0(4) . . ? C5A C4A C3A 105.7(3) . . ? N42A N41A C4A 117.4(3) . . ? N41A N42A C43A 113.0(3) . . ? N41A N42A Cu1 127.1(3) . . ? C43A N42A Cu1 119.6(2) . . ? C48A C43A C44A 119.4(4) . . ? C48A C43A N42A 122.7(4) . . ? C44A C43A N42A 117.9(3) . . ? C43A C44A C45A 120.0(4) . . ? C46A C45A C44A 122.1(4) . . ? C45A C46A C47A 116.4(4) . . ? C45A C46A C49A 123.1(4) . . ? C47A C46A C49A 120.5(4) . . ? C48A C47A C46A 122.1(4) . . ? C43A C48A C47A 119.9(4) . . ? C51A C49A C50A 108.6(4) . . ? C51A C49A C46A 112.4(4) . . ? C50A C49A C46A 110.3(4) . . ? C51A C49A C52A 107.7(4) . . ? C50A C49A C52A 109.6(4) . . ? C46A C49A C52A 108.3(3) . . ? O51A C5A N1A 125.0(4) . . ? O51A C5A C4A 128.9(4) . . ? N1A C5A C4A 106.1(3) . . ? C5A O51A Cu1 117.7(2) . . ? C5B N1B C11B 129.1(4) . . ? C5B N1B N2B 111.2(4) . . ? C11B N1B N2B 119.8(4) . . ? C16B C11B N1B 121.7(4) . . ? C16B C11B C12B 118.9(5) . . ? N1B C11B C12B 119.4(5) . . ? C13B C12B C11B 119.1(5) . . ? C12B C13B C14B 122.5(5) . . ? C13B C14B C15B 117.6(5) . . ? C16B C15B C14B 121.4(6) . . ? C15B C16B C11B 120.5(5) . . ? C3B N2B N1B 106.1(4) . . ? N2B C3B C4B 112.1(4) . . ? N2B C3B C31B 121.8(4) . . ? C4B C3B C31B 126.1(5) . . ? N41B C4B C5B 128.7(4) . . ? N41B C4B C3B 126.0(4) . . ? C5B C4B C3B 105.0(4) . . ? N42B N41B C4B 117.4(3) . . ? N41B N42B C43B 113.1(3) . . ? N41B N42B Cu1 126.4(3) . . ? C43B N42B Cu1 119.7(2) . . ? C44B C43B C48B 118.2(4) . . ? C44B C43B N42B 118.5(4) . . ? C48B C43B N42B 123.3(4) . . ? C45B C44B C43B 120.6(4) . . ? C44B C45B C46B 122.6(4) . . ? C45B C46B C47B 115.9(4) . . ? C45B C46B C49B 123.4(4) . . ? C47B C46B C49B 120.6(4) . . ? C48B C47B C46B 121.7(4) . . ? C47B C48B C43B 121.0(4) . . ? C52B C49B C46B 111.5(4) . . ? C52B C49B C51B 108.2(4) . . ? C46B C49B C51B 112.0(4) . . ? C52B C49B C50B 108.7(4) . . ? C46B C49B C50B 107.8(4) . . ? C51B C49B C50B 108.4(4) . . ? O51B C5B N1B 124.5(4) . . ? O51B C5B C4B 129.8(4) . . ? N1B C5B C4B 105.6(4) . . ? C5B O51B Cu1 116.7(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 60.14 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.751 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.078 data_twin-le1611 _database_code_CSD 158373 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety CuL2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H26 Cu N8 O2' _chemical_formula_weight 618.15 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic twin' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.307(4) _cell_length_b 11.311(6) _cell_length_c 16.415(8) _cell_angle_alpha 75.87(4) _cell_angle_beta 75.79(4) _cell_angle_gamma 71.58(4) _cell_volume 1395.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method ? _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.706 _exptl_absorpt_correction_T_max 0.364 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method omega-theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4522 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 70.01 _reflns_number_total 4522 _reflns_number_observed 3565 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Shelxs _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+2.5396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4522 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_obs 0.0616 _refine_ls_wR_factor_all 0.2222 _refine_ls_wR_factor_obs 0.2090 _refine_ls_goodness_of_fit_all 1.132 _refine_ls_goodness_of_fit_obs 1.211 _refine_ls_restrained_S_all 1.132 _refine_ls_restrained_S_obs 1.211 _refine_ls_shift/esd_max 0.034 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.06865(10) 0.47224(7) 0.28931(4) 0.0360(3) Uani 1 d . . N1 N 0.5401(6) 0.4102(4) 0.1287(3) 0.0404(11) Uani 1 d . . C11 C 0.6058(7) 0.5165(6) 0.0881(3) 0.0400(12) Uani 1 d . . C12 C 0.5370(9) 0.6305(7) 0.1170(4) 0.0561(17) Uani 1 d . . H12 H 0.4462 0.6393 0.1643 0.067 Uiso 1 calc R . C13 C 0.6040(9) 0.7309(7) 0.0751(5) 0.0649(19) Uani 1 d . . H13 H 0.5572 0.8089 0.0940 0.078 Uiso 1 calc R . C14 C 0.7387(9) 0.7193(7) 0.0058(4) 0.0576(17) Uani 1 d . . H14 H 0.7843 0.7882 -0.0214 0.069 Uiso 1 calc R . C15 C 0.8047(8) 0.6061(7) -0.0224(4) 0.0547(16) Uani 1 d . . H15 H 0.8951 0.5975 -0.0699 0.066 Uiso 1 calc R . C16 C 0.7393(8) 0.5046(6) 0.0184(4) 0.0487(14) Uani 1 d . . H16 H 0.7856 0.4271 -0.0012 0.058 Uiso 1 calc R . N2 N 0.6385(6) 0.2901(5) 0.1094(3) 0.0464(12) Uani 1 d . . C3 C 0.5439(8) 0.2128(6) 0.1477(4) 0.0462(14) Uani 1 d . . C31 C 0.6059(9) 0.0757(6) 0.1433(5) 0.065(2) Uani 1 d . . H31A H 0.5491 0.0583 0.1043 0.097 Uiso 1 calc R . H31B H 0.5796 0.0265 0.1998 0.097 Uiso 1 calc R . H31C H 0.7297 0.0528 0.1231 0.097 Uiso 1 calc R . C4 C 0.3817(7) 0.2777(5) 0.1937(3) 0.0405(13) Uani 1 d . . N41 N 0.2487(6) 0.2284(4) 0.2298(3) 0.0402(11) Uani 1 d . . N42 N 0.1060(6) 0.3012(4) 0.2638(3) 0.0373(10) Uani 1 d . . C43 C -0.0266(7) 0.2359(5) 0.2949(3) 0.0405(12) Uani 1 d . . C44 C -0.1959(7) 0.3035(6) 0.2894(4) 0.0442(13) Uani 1 d . . H44 H -0.2216 0.3899 0.2645 0.053 Uiso 1 calc R . C45 C -0.3276(8) 0.2446(7) 0.3203(4) 0.0521(15) Uani 1 d . . H45 H -0.4427 0.2909 0.3174 0.063 Uiso 1 calc R . C46 C -0.2873(9) 0.1165(7) 0.3554(4) 0.0574(17) Uani 1 d . . H46 H -0.3755 0.0755 0.3763 0.069 Uiso 1 calc R . C47 C -0.1208(9) 0.0499(6) 0.3597(4) 0.0588(18) Uani 1 d . . H47 H -0.0955 -0.0369 0.3834 0.071 Uiso 1 calc R . C48 C 0.0130(7) 0.1077(5) 0.3297(4) 0.0450(13) Uani 1 d . . H48 H 0.1277 0.0608 0.3329 0.054 Uiso 1 calc R . C5 C 0.3854(6) 0.4057(5) 0.1800(3) 0.0362(11) Uani 1 d . . O5 O 0.2701(5) 0.4996(3) 0.2084(2) 0.0410(9) Uani 1 d . . N1' N -0.2479(6) 0.4832(4) 0.5241(3) 0.0381(10) Uani 1 d . . C11' C -0.3206(7) 0.3809(5) 0.5633(3) 0.0375(12) Uani 1 d . . C12' C -0.2696(8) 0.2706(6) 0.5287(4) 0.0474(14) Uani 1 d . . H12' H -0.1846 0.2620 0.4791 0.057 Uiso 1 calc R . C13' C -0.3466(9) 0.1747(6) 0.5687(4) 0.0532(15) Uani 1 d . . H13' H -0.3124 0.1004 0.5455 0.064 Uiso 1 calc R . C14' C -0.4713(8) 0.1838(6) 0.6409(4) 0.0515(15) Uani 1 d . . H14' H -0.5223 0.1173 0.6668 0.062 Uiso 1 calc R . C15' C -0.5204(8) 0.2932(7) 0.6751(4) 0.0553(16) Uani 1 d . . H15' H -0.6054 0.3009 0.7247 0.066 Uiso 1 calc R . C16' C -0.4454(8) 0.3914(6) 0.6366(4) 0.0500(15) Uani 1 d . . H16' H -0.4793 0.4652 0.6603 0.060 Uiso 1 calc R . N2' N -0.2899(6) 0.5862(4) 0.5671(3) 0.0399(10) Uani 1 d . . C3' C -0.2268(7) 0.6736(5) 0.5135(3) 0.0385(12) Uani 1 d . . C31' C -0.2496(8) 0.7975(6) 0.5373(4) 0.0462(14) Uani 1 d . . H31D H -0.3210 0.8646 0.5016 0.069 Uiso 1 calc R . H31E H -0.1377 0.8129 0.5291 0.069 Uiso 1 calc R . H31F H -0.3049 0.7957 0.5968 0.069 Uiso 1 calc R . C4' C -0.1377(6) 0.6322(5) 0.4349(3) 0.0345(11) Uani 1 d . . N41' N -0.0745(6) 0.7054(4) 0.3644(3) 0.0379(10) Uani 1 d . . N42' N -0.0019(5) 0.6558(4) 0.2973(3) 0.0348(9) Uani 1 d . . C43' C 0.0511(7) 0.7465(5) 0.2256(3) 0.0388(12) Uani 1 d . . C44' C 0.0296(8) 0.7420(6) 0.1458(3) 0.0462(14) Uani 1 d . . H44' H -0.0185 0.6809 0.1389 0.055 Uiso 1 calc R . C45' C 0.0797(8) 0.8286(6) 0.0757(4) 0.0495(15) Uani 1 d . . H45' H 0.0675 0.8252 0.0209 0.059 Uiso 1 calc R . C46' C 0.1468(9) 0.9191(6) 0.0859(4) 0.0598(18) Uani 1 d . . H46' H 0.1777 0.9789 0.0385 0.072 Uiso 1 calc R . C47' C 0.1693(9) 0.9225(6) 0.1661(4) 0.0548(16) Uani 1 d . . H47' H 0.2161 0.9846 0.1725 0.066 Uiso 1 calc R . C48' C 0.1234(7) 0.8349(5) 0.2376(4) 0.0418(13) Uani 1 d . . H48' H 0.1409 0.8357 0.2919 0.050 Uiso 1 calc R . C5' C -0.1529(6) 0.5077(5) 0.4442(3) 0.0350(11) Uani 1 d . . O5' O -0.0951(5) 0.4319(3) 0.3911(2) 0.0393(8) Uani 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 0.0349(4) 0.0347(4) 0.0306(4) -0.0056(3) 0.0040(3) -0.0063(3) N1 0.039(2) 0.040(2) 0.033(2) -0.0073(18) 0.0047(18) -0.007(2) C11 0.036(3) 0.051(3) 0.030(2) -0.003(2) -0.002(2) -0.014(2) C12 0.054(4) 0.063(4) 0.051(4) -0.017(3) 0.010(3) -0.026(3) C13 0.062(4) 0.060(4) 0.072(5) -0.018(4) 0.011(4) -0.027(4) C14 0.052(4) 0.063(4) 0.057(4) 0.001(3) -0.003(3) -0.027(3) C15 0.042(3) 0.066(4) 0.045(3) 0.000(3) 0.003(3) -0.015(3) C16 0.040(3) 0.055(4) 0.038(3) -0.005(3) 0.005(2) -0.008(3) N2 0.039(3) 0.044(3) 0.042(2) -0.010(2) 0.008(2) -0.002(2) C3 0.047(3) 0.041(3) 0.038(3) -0.010(2) 0.010(2) -0.005(3) C31 0.056(4) 0.046(4) 0.070(4) -0.014(3) 0.020(3) -0.004(3) C4 0.034(3) 0.046(3) 0.030(2) -0.006(2) 0.007(2) -0.005(2) N41 0.041(2) 0.043(2) 0.027(2) -0.0079(18) 0.0056(18) -0.005(2) N42 0.035(2) 0.037(2) 0.035(2) -0.0062(18) -0.0011(18) -0.0064(19) C43 0.038(3) 0.045(3) 0.033(3) -0.010(2) 0.004(2) -0.010(2) C44 0.040(3) 0.046(3) 0.041(3) -0.005(2) -0.004(2) -0.009(2) C45 0.038(3) 0.066(4) 0.049(3) -0.015(3) 0.001(3) -0.012(3) C46 0.054(4) 0.061(4) 0.059(4) -0.023(3) 0.014(3) -0.028(3) C47 0.058(4) 0.042(3) 0.062(4) -0.011(3) 0.017(3) -0.015(3) C48 0.040(3) 0.037(3) 0.048(3) -0.010(2) 0.008(2) -0.007(2) C5 0.031(2) 0.044(3) 0.026(2) -0.005(2) 0.0017(19) -0.005(2) O5 0.0359(19) 0.040(2) 0.0397(19) -0.0072(16) 0.0051(15) -0.0088(16) N1' 0.035(2) 0.040(2) 0.030(2) -0.0052(18) 0.0057(17) -0.0072(19) C11' 0.032(3) 0.044(3) 0.030(2) 0.000(2) -0.003(2) -0.008(2) C12' 0.050(3) 0.047(3) 0.038(3) -0.007(2) 0.002(2) -0.012(3) C13' 0.070(4) 0.044(3) 0.045(3) -0.006(3) -0.004(3) -0.021(3) C14' 0.054(4) 0.058(4) 0.044(3) 0.004(3) -0.008(3) -0.027(3) C15' 0.047(3) 0.069(4) 0.041(3) -0.007(3) 0.011(3) -0.022(3) C16' 0.041(3) 0.055(4) 0.046(3) -0.009(3) 0.005(3) -0.012(3) N2' 0.040(2) 0.043(3) 0.029(2) -0.0087(18) 0.0040(18) -0.007(2) C3' 0.035(3) 0.044(3) 0.031(2) -0.006(2) -0.001(2) -0.009(2) C31' 0.048(3) 0.045(3) 0.039(3) -0.009(2) 0.003(2) -0.012(3) C4' 0.027(2) 0.038(3) 0.031(2) -0.002(2) 0.0006(19) -0.006(2) N41' 0.036(2) 0.039(2) 0.030(2) -0.0045(18) -0.0028(17) -0.0018(19) N42' 0.033(2) 0.036(2) 0.029(2) -0.0071(17) 0.0005(17) -0.0059(18) C43' 0.040(3) 0.032(3) 0.031(2) -0.001(2) 0.002(2) -0.001(2) C44' 0.049(3) 0.047(3) 0.033(3) -0.004(2) -0.001(2) -0.006(3) C45' 0.058(4) 0.049(3) 0.030(3) -0.002(2) -0.001(2) -0.010(3) C46' 0.064(4) 0.050(4) 0.044(3) 0.002(3) 0.012(3) -0.012(3) C47' 0.062(4) 0.049(4) 0.046(3) -0.006(3) 0.006(3) -0.019(3) C48' 0.046(3) 0.031(3) 0.041(3) -0.007(2) 0.005(2) -0.010(2) C5' 0.026(2) 0.041(3) 0.030(2) -0.003(2) 0.0001(19) -0.005(2) O5' 0.0363(18) 0.0382(19) 0.0349(18) -0.0070(15) 0.0042(15) -0.0063(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.922(4) . ? Cu1 O5' 1.937(4) . ? Cu1 N42 1.992(5) . ? Cu1 N42' 1.999(4) . ? N1 C5 1.361(6) . ? N1 N2 1.413(6) . ? N1 C11 1.425(7) . ? C11 C12 1.384(9) . ? C11 C16 1.384(7) . ? C12 C13 1.380(9) . ? C13 C14 1.385(9) . ? C14 C15 1.370(10) . ? C15 C16 1.379(9) . ? N2 C3 1.304(8) . ? C3 C4 1.439(7) . ? C3 C31 1.485(8) . ? C4 N41 1.338(7) . ? C4 C5 1.419(8) . ? N41 N42 1.295(6) . ? N42 C43 1.440(7) . ? C43 C44 1.385(8) . ? C43 C48 1.388(8) . ? C44 C45 1.386(8) . ? C45 C46 1.387(9) . ? C46 C47 1.360(10) . ? C47 C48 1.392(8) . ? C5 O5 1.281(6) . ? N1' C5' 1.368(6) . ? N1' N2' 1.414(6) . ? N1' C11' 1.416(7) . ? C11' C16' 1.383(7) . ? C11' C12' 1.398(8) . ? C12' C13' 1.379(9) . ? C13' C14' 1.371(9) . ? C14' C15' 1.385(9) . ? C15' C16' 1.387(9) . ? N2' C3' 1.305(7) . ? C3' C4' 1.427(7) . ? C3' C31' 1.489(8) . ? C4' N41' 1.346(6) . ? C4' C5' 1.422(8) . ? N41' N42' 1.286(6) . ? N42' C43' 1.440(6) . ? C43' C44' 1.381(8) . ? C43' C48' 1.391(8) . ? C44' C45' 1.389(8) . ? C45' C46' 1.369(10) . ? C46' C47' 1.385(10) . ? C47' C48' 1.399(8) . ? C5' O5' 1.275(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 O5 Cu1 O5' 165.57(17) . . ? O5 Cu1 N42 92.88(17) . . ? O5' Cu1 N42 88.94(17) . . ? O5 Cu1 N42' 88.37(17) . . ? O5' Cu1 N42' 92.82(17) . . ? N42 Cu1 N42' 168.00(18) . . ? C5 N1 N2 111.8(4) . . ? C5 N1 C11 129.8(5) . . ? N2 N1 C11 118.1(4) . . ? C12 C11 C16 120.1(6) . . ? C12 C11 N1 120.9(5) . . ? C16 C11 N1 119.0(5) . . ? C13 C12 C11 118.7(6) . . ? C12 C13 C14 121.5(7) . . ? C15 C14 C13 119.1(6) . . ? C14 C15 C16 120.4(6) . . ? C15 C16 C11 120.2(6) . . ? C3 N2 N1 105.9(4) . . ? N2 C3 C4 111.2(5) . . ? N2 C3 C31 121.7(5) . . ? C4 C3 C31 127.0(6) . . ? N41 C4 C5 128.4(5) . . ? N41 C4 C3 125.2(5) . . ? C5 C4 C3 105.6(5) . . ? N42 N41 C4 118.3(5) . . ? N41 N42 C43 111.2(4) . . ? N41 N42 Cu1 127.6(4) . . ? C43 N42 Cu1 120.6(3) . . ? C44 C43 C48 120.1(5) . . ? C44 C43 N42 118.8(5) . . ? C48 C43 N42 121.1(5) . . ? C43 C44 C45 120.5(6) . . ? C44 C45 C46 119.1(6) . . ? C47 C46 C45 120.3(6) . . ? C46 C47 C48 121.4(6) . . ? C43 C48 C47 118.6(6) . . ? O5 C5 N1 125.8(5) . . ? O5 C5 C4 128.7(5) . . ? N1 C5 C4 105.4(4) . . ? C5 O5 Cu1 120.0(3) . . ? C5' N1' N2' 111.0(4) . . ? C5' N1' C11' 130.2(5) . . ? N2' N1' C11' 118.4(4) . . ? C16' C11' C12' 119.7(5) . . ? C16' C11' N1' 119.3(5) . . ? C12' C11' N1' 121.0(5) . . ? C13' C12' C11' 118.7(5) . . ? C14' C13' C12' 122.4(6) . . ? C13' C14' C15' 118.6(6) . . ? C14' C15' C16' 120.6(5) . . ? C11' C16' C15' 120.1(6) . . ? C3' N2' N1' 106.3(4) . . ? N2' C3' C4' 111.3(5) . . ? N2' C3' C31' 121.0(5) . . ? C4' C3' C31' 127.7(5) . . ? N41' C4' C5' 128.5(5) . . ? N41' C4' C3' 125.1(5) . . ? C5' C4' C3' 105.8(4) . . ? N42' N41' C4' 118.1(5) . . ? N41' N42' C43' 112.0(4) . . ? N41' N42' Cu1 127.4(3) . . ? C43' N42' Cu1 119.9(3) . . ? C44' C43' C48' 121.7(5) . . ? C44' C43' N42' 118.3(5) . . ? C48' C43' N42' 120.0(5) . . ? C43' C44' C45' 119.3(6) . . ? C46' C45' C44' 120.3(6) . . ? C45' C46' C47' 120.1(6) . . ? C46' C47' C48' 120.9(6) . . ? C43' C48' C47' 117.6(6) . . ? O5' C5' N1' 125.2(5) . . ? O5' C5' C4' 129.2(4) . . ? N1' C5' C4' 105.6(4) . . ? C5' O5' Cu1 118.7(3) . . ? _refine_diff_density_max 0.870 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.171 data_le214a _database_code_CSD 158374 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Zn(C20H21N4O1)2] _chemical_formula_sum 'C40 H42 N8 O2 Zn' _chemical_formula_weight 732.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' -1.5491 0.6778 '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 12.280(5) _cell_length_b 13.615(5) _cell_length_c 14.172(5) _cell_angle_alpha 113.737(16) _cell_angle_beta 95.127(16) _cell_angle_gamma 113.635(14) _cell_volume 1896.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_T_max 0.7963 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8714 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 70.10 _reflns_number_total 6740 _reflns_number_gt 5714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.1602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'Riding or rotating rigid group (Me)' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6740 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.074 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.02507(2) 0.28910(2) 0.17647(2) 0.02726(10) Uani 1 1 d . . . N1A N -0.09584(15) 0.50856(14) 0.12666(13) 0.0288(3) Uani 1 1 d . . . C11A C -0.16049(18) 0.47083(17) 0.01996(16) 0.0281(4) Uani 1 1 d . . . C12A C -0.2215(2) 0.5324(2) 0.00450(18) 0.0380(5) Uani 1 1 d . . . H12A H -0.2212 0.5968 0.0641 0.046 Uiso 1 1 calc R . . C13A C -0.2824(2) 0.4983(2) -0.09896(19) 0.0451(6) Uani 1 1 d . . . H13A H -0.3237 0.5399 -0.1094 0.054 Uiso 1 1 calc R . . C14A C -0.2837(2) 0.4039(2) -0.18740(18) 0.0403(5) Uani 1 1 d . . . H14A H -0.3250 0.3815 -0.2577 0.048 Uiso 1 1 calc R . . C15A C -0.2235(2) 0.3427(2) -0.17129(17) 0.0354(5) Uani 1 1 d . . . H15A H -0.2247 0.2778 -0.2311 0.043 Uiso 1 1 calc R . . C16A C -0.16169(19) 0.37556(19) -0.06837(17) 0.0333(4) Uani 1 1 d . . . H16A H -0.1207 0.3336 -0.0583 0.040 Uiso 1 1 calc R . . N2A N -0.07164(17) 0.62314(15) 0.20975(15) 0.0354(4) Uani 1 1 d . . . C3A C -0.0094(2) 0.63670(19) 0.29742(17) 0.0341(4) Uani 1 1 d . . . C31A C 0.0335(3) 0.7478(2) 0.4037(2) 0.0511(6) Uani 1 1 d . . . H31A H 0.1233 0.7865 0.4329 0.077 Uiso 1 1 calc R . . H31B H -0.0058 0.7247 0.4532 0.077 Uiso 1 1 calc R . . H31C H 0.0110 0.8046 0.3942 0.077 Uiso 1 1 calc R . . C4A C 0.01064(18) 0.53419(17) 0.27697(16) 0.0288(4) Uani 1 1 d . . . N41A N 0.07457(15) 0.52782(15) 0.35411(13) 0.0290(4) Uani 1 1 d . . . N42A N 0.09221(15) 0.43360(15) 0.32715(13) 0.0278(3) Uani 1 1 d . . . C43A C 0.15837(18) 0.43579(18) 0.41668(16) 0.0286(4) Uani 1 1 d . . . C44A C 0.1732(2) 0.5100(2) 0.52306(17) 0.0349(5) Uani 1 1 d . . . H44A H 0.1366 0.5613 0.5396 0.042 Uiso 1 1 calc R . . C45A C 0.2419(2) 0.5094(2) 0.60562(17) 0.0357(5) Uani 1 1 d . . . H45A H 0.2507 0.5603 0.6776 0.043 Uiso 1 1 calc R . . C46A C 0.2982(2) 0.4354(2) 0.58505(17) 0.0348(5) Uani 1 1 d . . . C49A C 0.3856(2) 0.4425(2) 0.67439(18) 0.0447(6) Uani 1 1 d . . . C50A C 0.5166(3) 0.4910(3) 0.6617(2) 0.0667(9) Uani 1 1 d . . . H50A H 0.5738 0.4958 0.7173 0.100 Uiso 1 1 calc R . . H50B H 0.5440 0.5718 0.6687 0.100 Uiso 1 1 calc R . . H50C H 0.5149 0.4362 0.5911 0.100 Uiso 1 1 calc R . . C51A C 0.3416(3) 0.3144(3) 0.6634(3) 0.0723(9) Uani 1 1 d . . . H51A H 0.3984 0.3191 0.7193 0.108 Uiso 1 1 calc R . . H51B H 0.3401 0.2595 0.5930 0.108 Uiso 1 1 calc R . . H51C H 0.2586 0.2838 0.6712 0.108 Uiso 1 1 calc R . . C52A C 0.3910(3) 0.5271(3) 0.78736(19) 0.0584(7) Uani 1 1 d . . . H52A H 0.4459 0.5270 0.8409 0.088 Uiso 1 1 calc R . . H52B H 0.3081 0.4987 0.7956 0.088 Uiso 1 1 calc R . . H52C H 0.4224 0.6095 0.7974 0.088 Uiso 1 1 calc R . . C47A C 0.2779(2) 0.3585(2) 0.47746(18) 0.0461(6) Uani 1 1 d . . . H47A H 0.3121 0.3052 0.4607 0.055 Uiso 1 1 calc R . . C48A C 0.2094(2) 0.3574(2) 0.39408(17) 0.0403(5) Uani 1 1 d . . . H48A H 0.1972 0.3036 0.3220 0.048 Uiso 1 1 calc R . . C5A C -0.04632(18) 0.45323(17) 0.16397(16) 0.0264(4) Uani 1 1 d . . . O5A O -0.05404(13) 0.34928(12) 0.10529(11) 0.0298(3) Uani 1 1 d . . . N1B N 0.21371(16) 0.09869(15) 0.06783(14) 0.0302(4) Uani 1 1 d . . . C11B C 0.30872(19) 0.14293(18) 0.02236(16) 0.0319(4) Uani 1 1 d . . . C12B C 0.4039(2) 0.1125(2) 0.0244(2) 0.0421(5) Uani 1 1 d . . . H12B H 0.4054 0.0637 0.0556 0.051 Uiso 1 1 calc R . . C13B C 0.4964(2) 0.1545(2) -0.0199(2) 0.0519(6) Uani 1 1 d . . . H13B H 0.5605 0.1335 -0.0193 0.062 Uiso 1 1 calc R . . C14B C 0.4954(2) 0.2272(2) -0.0652(2) 0.0516(6) Uani 1 1 d . . . H14B H 0.5593 0.2566 -0.0943 0.062 Uiso 1 1 calc R . . C15B C 0.4001(2) 0.2561(2) -0.0675(2) 0.0472(6) Uani 1 1 d . . . H15B H 0.3988 0.3048 -0.0989 0.057 Uiso 1 1 calc R . . C16B C 0.3061(2) 0.2143(2) -0.02389(17) 0.0370(5) Uani 1 1 d . . . H16B H 0.2413 0.2343 -0.0258 0.044 Uiso 1 1 calc R . . N2B N 0.19378(17) -0.00477(16) 0.07941(15) 0.0356(4) Uani 1 1 d . . . C3B C 0.10391(19) -0.02458(19) 0.12344(17) 0.0326(4) Uani 1 1 d . . . C31B C 0.0571(2) -0.1268(2) 0.1496(2) 0.0470(6) Uani 1 1 d . . . H31D H -0.0070 -0.2005 0.0869 0.070 Uiso 1 1 calc R . . H31E H 0.0224 -0.1061 0.2091 0.070 Uiso 1 1 calc R . . H31F H 0.1253 -0.1402 0.1700 0.070 Uiso 1 1 calc R . . C4B C 0.06109(18) 0.06334(17) 0.14227(16) 0.0278(4) Uani 1 1 d . . . N41B N -0.03583(15) 0.05898(14) 0.18137(13) 0.0282(3) Uani 1 1 d . . . N42B N -0.07042(15) 0.13983(14) 0.19156(13) 0.0275(3) Uani 1 1 d . . . C43B C -0.17385(18) 0.12735(17) 0.23311(16) 0.0287(4) Uani 1 1 d . . . C44B C -0.2408(2) 0.1828(2) 0.21501(19) 0.0366(5) Uani 1 1 d . . . H44B H -0.2184 0.2248 0.1752 0.044 Uiso 1 1 calc R . . C45B C -0.3407(2) 0.1762(2) 0.25559(19) 0.0390(5) Uani 1 1 d . . . H45B H -0.3864 0.2125 0.2412 0.047 Uiso 1 1 calc R . . C46B C -0.3747(2) 0.11768(19) 0.31661(17) 0.0359(5) Uani 1 1 d . . . C49B C -0.4812(2) 0.1135(2) 0.3662(2) 0.0471(6) Uani 1 1 d . . . C50B C -0.5428(3) 0.1819(3) 0.3414(3) 0.0660(8) Uani 1 1 d . . . H50D H -0.4833 0.2682 0.3756 0.099 Uiso 1 1 calc R . . H50E H -0.6140 0.1708 0.3689 0.099 Uiso 1 1 calc R . . H50F H -0.5703 0.1499 0.2639 0.099 Uiso 1 1 calc R . . C51B C -0.5811(3) -0.0197(3) 0.3201(3) 0.0704(9) Uani 1 1 d . . . H51D H -0.6468 -0.0230 0.3540 0.106 Uiso 1 1 calc R . . H51E H -0.5443 -0.0653 0.3341 0.106 Uiso 1 1 calc R . . H51F H -0.6158 -0.0551 0.2427 0.106 Uiso 1 1 calc R . . C52B C -0.4296(3) 0.1721(3) 0.4892(2) 0.0735(9) Uani 1 1 d . . . H52D H -0.3671 0.2568 0.5179 0.110 Uiso 1 1 calc R . . H52E H -0.3924 0.1283 0.5063 0.110 Uiso 1 1 calc R . . H52F H -0.4969 0.1684 0.5211 0.110 Uiso 1 1 calc R . . C47B C -0.3069(2) 0.0613(2) 0.33225(19) 0.0417(5) Uani 1 1 d . . . H47B H -0.3293 0.0191 0.3719 0.050 Uiso 1 1 calc R . . C48B C -0.2083(2) 0.0654(2) 0.29170(18) 0.0382(5) Uani 1 1 d . . . H48B H -0.1646 0.0264 0.3037 0.046 Uiso 1 1 calc R . . C5B C 0.13599(18) 0.14248(17) 0.10567(15) 0.0264(4) Uani 1 1 d . . . O5B O 0.13787(13) 0.23886(12) 0.10792(11) 0.0306(3) 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 Zn1 0.03216(17) 0.02932(15) 0.02876(15) 0.01571(11) 0.01022(11) 0.02014(12) N1A 0.0314(9) 0.0267(8) 0.0312(8) 0.0139(7) 0.0057(7) 0.0172(7) C11A 0.0251(10) 0.0287(9) 0.0316(10) 0.0166(8) 0.0054(8) 0.0125(8) C12A 0.0452(13) 0.0354(11) 0.0377(11) 0.0178(9) 0.0059(10) 0.0242(10) C13A 0.0535(15) 0.0453(13) 0.0457(13) 0.0256(11) 0.0047(11) 0.0299(12) C14A 0.0415(13) 0.0445(12) 0.0358(11) 0.0228(10) 0.0043(10) 0.0192(11) C15A 0.0358(12) 0.0372(11) 0.0341(11) 0.0174(9) 0.0109(9) 0.0179(10) C16A 0.0337(11) 0.0372(11) 0.0369(11) 0.0206(9) 0.0110(9) 0.0211(10) N2A 0.0391(10) 0.0282(8) 0.0386(10) 0.0132(8) 0.0050(8) 0.0200(8) C3A 0.0371(12) 0.0298(10) 0.0354(11) 0.0133(9) 0.0066(9) 0.0192(9) C31A 0.0652(17) 0.0363(12) 0.0413(13) 0.0075(11) 0.0005(12) 0.0295(12) C4A 0.0300(11) 0.0287(10) 0.0319(10) 0.0156(8) 0.0083(8) 0.0168(9) N41A 0.0293(9) 0.0305(8) 0.0299(8) 0.0143(7) 0.0074(7) 0.0172(7) N42A 0.0272(9) 0.0315(8) 0.0290(8) 0.0159(7) 0.0076(7) 0.0168(7) C43A 0.0260(10) 0.0337(10) 0.0293(10) 0.0168(8) 0.0062(8) 0.0159(9) C44A 0.0409(12) 0.0388(11) 0.0317(10) 0.0159(9) 0.0108(9) 0.0259(10) C45A 0.0406(12) 0.0427(12) 0.0266(10) 0.0144(9) 0.0098(9) 0.0247(10) C46A 0.0328(11) 0.0449(12) 0.0306(10) 0.0189(9) 0.0066(9) 0.0221(10) C49A 0.0455(14) 0.0647(16) 0.0349(12) 0.0267(12) 0.0085(10) 0.0339(13) C50A 0.0522(17) 0.116(3) 0.0553(16) 0.0483(18) 0.0144(14) 0.0534(18) C51A 0.096(2) 0.080(2) 0.0612(18) 0.0447(17) 0.0100(17) 0.053(2) C52A 0.0558(16) 0.088(2) 0.0318(12) 0.0239(13) 0.0045(11) 0.0419(16) C47A 0.0608(16) 0.0612(15) 0.0332(11) 0.0188(11) 0.0098(11) 0.0490(14) C48A 0.0504(14) 0.0498(13) 0.0268(10) 0.0121(10) 0.0071(10) 0.0366(12) C5A 0.0255(10) 0.0283(9) 0.0310(10) 0.0174(8) 0.0088(8) 0.0147(8) O5A 0.0361(8) 0.0295(7) 0.0297(7) 0.0149(6) 0.0076(6) 0.0206(6) N1B 0.0324(9) 0.0312(8) 0.0354(9) 0.0175(7) 0.0139(7) 0.0204(8) C11B 0.0310(11) 0.0312(10) 0.0306(10) 0.0100(8) 0.0115(8) 0.0168(9) C12B 0.0390(13) 0.0421(12) 0.0497(13) 0.0194(11) 0.0185(11) 0.0250(11) C13B 0.0388(14) 0.0540(15) 0.0616(16) 0.0203(13) 0.0256(12) 0.0266(12) C14B 0.0443(14) 0.0487(14) 0.0511(15) 0.0163(12) 0.0275(12) 0.0178(12) C15B 0.0501(15) 0.0472(13) 0.0458(13) 0.0242(11) 0.0231(12) 0.0211(12) C16B 0.0359(12) 0.0408(11) 0.0380(11) 0.0192(10) 0.0152(9) 0.0207(10) N2B 0.0393(10) 0.0346(9) 0.0463(10) 0.0228(8) 0.0169(8) 0.0252(8) C3B 0.0326(11) 0.0333(10) 0.0395(11) 0.0192(9) 0.0105(9) 0.0208(9) C31B 0.0552(15) 0.0444(13) 0.0664(16) 0.0370(13) 0.0272(13) 0.0335(12) C4B 0.0295(10) 0.0272(9) 0.0290(9) 0.0131(8) 0.0073(8) 0.0164(8) N41B 0.0300(9) 0.0293(8) 0.0293(8) 0.0151(7) 0.0081(7) 0.0170(7) N42B 0.0299(9) 0.0298(8) 0.0294(8) 0.0155(7) 0.0100(7) 0.0185(7) C43B 0.0289(10) 0.0274(9) 0.0285(10) 0.0110(8) 0.0089(8) 0.0147(8) C44B 0.0358(12) 0.0385(11) 0.0465(12) 0.0251(10) 0.0168(10) 0.0218(10) C45B 0.0358(12) 0.0402(12) 0.0516(13) 0.0240(11) 0.0174(10) 0.0247(10) C46B 0.0325(12) 0.0336(10) 0.0357(11) 0.0108(9) 0.0131(9) 0.0160(9) C49B 0.0414(14) 0.0472(13) 0.0525(14) 0.0203(12) 0.0257(12) 0.0223(11) C50B 0.0606(18) 0.078(2) 0.088(2) 0.0435(18) 0.0481(17) 0.0493(17) C51B 0.0502(17) 0.0606(18) 0.097(2) 0.0342(18) 0.0404(17) 0.0234(15) C52B 0.075(2) 0.099(2) 0.0531(17) 0.0305(17) 0.0393(16) 0.049(2) C47B 0.0454(13) 0.0505(13) 0.0461(13) 0.0319(11) 0.0239(11) 0.0269(11) C48B 0.0402(13) 0.0467(12) 0.0441(12) 0.0284(11) 0.0183(10) 0.0274(11) C5B 0.0271(10) 0.0290(9) 0.0248(9) 0.0116(8) 0.0067(8) 0.0164(8) O5B 0.0374(8) 0.0323(7) 0.0364(7) 0.0205(6) 0.0173(6) 0.0240(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5A 1.9394(14) . ? Zn1 O5B 1.9483(14) . ? Zn1 N42B 2.0087(18) . ? Zn1 N42A 2.0281(18) . ? N1A C5A 1.359(2) . ? N1A N2A 1.413(2) . ? N1A C11A 1.419(2) . ? C11A C16A 1.387(3) . ? C11A C12A 1.391(3) . ? C12A C13A 1.379(3) . ? C13A C14A 1.381(3) . ? C14A C15A 1.382(3) . ? C15A C16A 1.381(3) . ? N2A C3A 1.302(3) . ? C3A C4A 1.433(3) . ? C3A C31A 1.490(3) . ? C4A N41A 1.340(2) . ? C4A C5A 1.425(3) . ? N41A N42A 1.297(2) . ? N42A C43A 1.427(2) . ? C43A C44A 1.380(3) . ? C43A C48A 1.390(3) . ? C44A C45A 1.385(3) . ? C45A C46A 1.391(3) . ? C46A C47A 1.386(3) . ? C46A C49A 1.530(3) . ? C49A C52A 1.527(3) . ? C49A C50A 1.533(4) . ? C49A C51A 1.540(4) . ? C47A C48A 1.379(3) . ? C5A O5A 1.278(2) . ? N1B C5B 1.358(2) . ? N1B N2B 1.410(2) . ? N1B C11B 1.422(3) . ? C11B C16B 1.382(3) . ? C11B C12B 1.390(3) . ? C12B C13B 1.380(3) . ? C13B C14B 1.382(4) . ? C14B C15B 1.379(4) . ? C15B C16B 1.386(3) . ? N2B C3B 1.304(3) . ? C3B C4B 1.433(3) . ? C3B C31B 1.489(3) . ? C4B N41B 1.347(3) . ? C4B C5B 1.420(3) . ? N41B N42B 1.293(2) . ? N42B C43B 1.425(2) . ? C43B C48B 1.386(3) . ? C43B C44B 1.388(3) . ? C44B C45B 1.386(3) . ? C45B C46B 1.382(3) . ? C46B C47B 1.396(3) . ? C46B C49B 1.530(3) . ? C49B C51B 1.529(4) . ? C49B C50B 1.531(4) . ? C49B C52B 1.534(4) . ? C47B C48B 1.377(3) . ? C5B O5B 1.291(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 O5A Zn1 O5B 114.46(6) . . ? O5A Zn1 N42B 123.16(7) . . ? O5B Zn1 N42B 97.33(6) . . ? O5A Zn1 N42A 97.21(7) . . ? O5B Zn1 N42A 120.08(7) . . ? N42B Zn1 N42A 106.05(7) . . ? C5A N1A N2A 111.88(16) . . ? C5A N1A C11A 129.98(16) . . ? N2A N1A C11A 118.08(15) . . ? C16A C11A C12A 119.94(19) . . ? C16A C11A N1A 121.07(17) . . ? C12A C11A N1A 118.98(18) . . ? C13A C12A C11A 119.5(2) . . ? C12A C13A C14A 121.0(2) . . ? C13A C14A C15A 119.2(2) . . ? C16A C15A C14A 120.8(2) . . ? C15A C16A C11A 119.59(19) . . ? C3A N2A N1A 105.68(15) . . ? N2A C3A C4A 111.76(18) . . ? N2A C3A C31A 121.77(19) . . ? C4A C3A C31A 126.47(19) . . ? N41A C4A C5A 131.77(17) . . ? N41A C4A C3A 122.96(18) . . ? C5A C4A C3A 105.23(17) . . ? N42A N41A C4A 118.59(16) . . ? N41A N42A C43A 113.27(16) . . ? N41A N42A Zn1 125.19(13) . . ? C43A N42A Zn1 121.41(13) . . ? C44A C43A C48A 118.82(18) . . ? C44A C43A N42A 123.79(17) . . ? C48A C43A N42A 117.39(18) . . ? C43A C44A C45A 120.29(18) . . ? C44A C45A C46A 121.86(19) . . ? C47A C46A C45A 116.59(19) . . ? C47A C46A C49A 120.35(19) . . ? C45A C46A C49A 122.9(2) . . ? C52A C49A C46A 112.67(19) . . ? C52A C49A C50A 108.7(2) . . ? C46A C49A C50A 107.93(19) . . ? C52A C49A C51A 107.9(2) . . ? C46A C49A C51A 109.8(2) . . ? C50A C49A C51A 109.7(2) . . ? C48A C47A C46A 122.4(2) . . ? C47A C48A C43A 119.9(2) . . ? O5A C5A N1A 124.49(18) . . ? O5A C5A C4A 130.07(17) . . ? N1A C5A C4A 105.44(16) . . ? C5A O5A Zn1 117.11(12) . . ? C5B N1B N2B 111.71(16) . . ? C5B N1B C11B 129.74(17) . . ? N2B N1B C11B 118.54(15) . . ? C16B C11B C12B 120.4(2) . . ? C16B C11B N1B 120.63(18) . . ? C12B C11B N1B 119.00(19) . . ? C13B C12B C11B 119.5(2) . . ? C12B C13B C14B 120.5(2) . . ? C15B C14B C13B 119.5(2) . . ? C14B C15B C16B 120.8(2) . . ? C11B C16B C15B 119.3(2) . . ? C3B N2B N1B 105.92(15) . . ? N2B C3B C4B 111.37(18) . . ? N2B C3B C31B 121.79(18) . . ? C4B C3B C31B 126.84(19) . . ? N41B C4B C5B 131.34(17) . . ? N41B C4B C3B 123.13(18) . . ? C5B C4B C3B 105.43(17) . . ? N42B N41B C4B 118.45(16) . . ? N41B N42B C43B 114.26(16) . . ? N41B N42B Zn1 125.03(13) . . ? C43B N42B Zn1 119.94(12) . . ? C48B C43B C44B 119.23(19) . . ? C48B C43B N42B 123.32(18) . . ? C44B C43B N42B 117.43(18) . . ? C45B C44B C43B 120.1(2) . . ? C46B C45B C44B 121.7(2) . . ? C45B C46B C47B 117.0(2) . . ? C45B C46B C49B 122.8(2) . . ? C47B C46B C49B 120.3(2) . . ? C51B C49B C50B 107.8(2) . . ? C51B C49B C46B 109.2(2) . . ? C50B C49B C46B 112.5(2) . . ? C51B C49B C52B 110.0(3) . . ? C50B C49B C52B 108.5(2) . . ? C46B C49B C52B 109.0(2) . . ? C48B C47B C46B 122.4(2) . . ? C47B C48B C43B 119.6(2) . . ? O5B C5B N1B 124.18(18) . . ? O5B C5B C4B 130.22(17) . . ? N1B C5B C4B 105.57(16) . . ? C5B O5B Zn1 115.92(12) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 70.10 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.261 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.050 data_le214d _database_code_CSD 158375 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [NiL2(MeOH)2].2MeOH _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H60 N6 Ni O6' _chemical_formula_weight 851.71 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 '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 10.5849(12) _cell_length_b 14.896(2) _cell_length_c 15.153(2) _cell_angle_alpha 76.735(6) _cell_angle_beta 79.025(6) _cell_angle_gamma 77.539(7) _cell_volume 2245.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method ? _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 0.584 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; ? ; _diffrn_measurement_method Omega-theta _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -2 _diffrn_reflns_number 8035 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 70.09 _reflns_number_total 7972 _reflns_number_observed 6602 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.5324P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment Riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7967 _refine_ls_number_parameters 567 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_all 0.1335 _refine_ls_wR_factor_obs 0.1252 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.034 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.20323(4) 0.48304(3) 0.24452(3) 0.02676(14) Uani 1 d . . N1 N -0.0434(2) 0.63072(14) 0.43415(13) 0.0292(4) Uani 1 d . . C11 C -0.0045(3) 0.7132(2) 0.4424(2) 0.0323(5) Uani 1 d . . C12 C -0.0986(3) 0.7900(2) 0.4608(2) 0.0394(6) Uani 1 d . . H12 H -0.1879(3) 0.7861(2) 0.4709(2) 0.047 Uiso 1 calc R . C13 C -0.0607(3) 0.8719(2) 0.4642(2) 0.0495(7) Uani 1 d . . H13 H -0.1249(3) 0.9240(2) 0.4757(2) 0.059 Uiso 1 calc R . C14 C 0.0691(4) 0.8788(2) 0.4509(2) 0.0578(9) Uani 1 d . . H14 H 0.0940(4) 0.9351(2) 0.4528(2) 0.069 Uiso 1 calc R . C15 C 0.1624(3) 0.8016(3) 0.4349(3) 0.0635(10) Uani 1 d . . H15 H 0.2516(3) 0.8054(3) 0.4265(3) 0.076 Uiso 1 calc R . C16 C 0.1268(3) 0.7188(2) 0.4309(2) 0.0476(7) Uani 1 d . . H16 H 0.1914(3) 0.6666(2) 0.4203(2) 0.057 Uiso 1 calc R . N2 N -0.1727(2) 0.61821(14) 0.46816(13) 0.0319(5) Uani 1 d . . C3 C -0.1896(2) 0.5484(2) 0.4349(2) 0.0315(5) Uani 1 d . . C31 C -0.3169(3) 0.5153(2) 0.4560(2) 0.0450(7) Uani 1 d . . H31A H -0.3014(3) 0.4473(2) 0.4691(15) 0.067 Uiso 1 calc R . H31B H -0.3635(10) 0.5387(13) 0.4037(6) 0.067 Uiso 1 calc R . H31C H -0.3688(9) 0.5384(13) 0.5089(9) 0.067 Uiso 1 calc R . C4 C -0.0756(2) 0.5142(2) 0.3776(2) 0.0288(5) Uani 1 d . . C41 C -0.0672(2) 0.44289(14) 0.33376(13) 0.0191(4) Uani 1 d . . H41 H -0.1351(2) 0.40824(14) 0.34561(13) 0.023 Uiso 1 calc R . N42 N 0.0346(2) 0.42367(13) 0.27606(13) 0.0283(4) Uani 1 d . . C43 C 0.0321(2) 0.3430(2) 0.2399(2) 0.0281(5) Uani 1 d . . C44 C 0.0588(2) 0.3473(2) 0.1462(2) 0.0341(5) Uani 1 d . . H44 H 0.0751(2) 0.4034(2) 0.1063(2) 0.041 Uiso 1 calc R . C45 C 0.0613(3) 0.2687(2) 0.1114(2) 0.0364(6) Uani 1 d . . H45 H 0.0774(3) 0.2727(2) 0.0475(2) 0.044 Uiso 1 calc R . C46 C 0.0408(2) 0.1839(2) 0.1681(2) 0.0335(5) Uani 1 d . . C461 C 0.0463(3) 0.0967(2) 0.1298(2) 0.0469(7) Uani 1 d D . C462 C 0.0489(17) 0.0079(6) 0.1992(7) 0.085(5) Uani 0.339(9) d PDU 1 H46A H -0.0237(17) 0.0156(6) 0.2483(7) 0.128 Uiso 0.339(9) calc PR 1 H46B H 0.1306(17) -0.0076(6) 0.2240(7) 0.128 Uiso 0.339(9) calc PR 1 H46C H 0.0414(17) -0.0422(6) 0.1705(7) 0.128 Uiso 0.339(9) calc PR 1 C463 C 0.1559(13) 0.0906(11) 0.0512(9) 0.107(7) Uani 0.339(9) d PDU 1 H46D H 0.1497(13) 0.1501(11) 0.0082(9) 0.160 Uiso 0.339(9) calc PR 1 H46E H 0.1498(13) 0.0415(11) 0.0206(9) 0.160 Uiso 0.339(9) calc PR 1 H46F H 0.2390(13) 0.0762(11) 0.0741(9) 0.160 Uiso 0.339(9) calc PR 1 C464 C -0.0848(10) 0.1197(9) 0.0901(12) 0.095(5) Uani 0.339(9) d PDU 1 H46G H -0.0878(10) 0.1775(9) 0.0447(12) 0.142 Uiso 0.339(9) calc PR 1 H46H H -0.1576(10) 0.1268(9) 0.1392(12) 0.142 Uiso 0.339(9) calc PR 1 H46I H -0.0908(10) 0.0690(9) 0.0616(12) 0.142 Uiso 0.339(9) calc PR 1 C465 C 0.0810(9) 0.1111(5) 0.0268(3) 0.081(3) Uani 0.661(9) d PDU 2 H46J H 0.1615(9) 0.1359(5) 0.0079(3) 0.121 Uiso 0.661(9) calc PR 2 H46K H 0.0111(9) 0.1550(5) -0.0014(3) 0.121 Uiso 0.661(9) calc PR 2 H46L H 0.0925(9) 0.0516(5) 0.0078(3) 0.121 Uiso 0.661(9) calc PR 2 C466 C -0.0788(6) 0.0581(6) 0.1617(5) 0.089(3) Uani 0.661(9) d PDU 2 H46M H -0.0992(6) 0.0495(6) 0.2280(5) 0.133 Uiso 0.661(9) calc PR 2 H46N H -0.0682(6) -0.0017(6) 0.1434(5) 0.133 Uiso 0.661(9) calc PR 2 H46O H -0.1496(6) 0.1017(6) 0.1342(5) 0.133 Uiso 0.661(9) calc PR 2 C467 C 0.1582(8) 0.0189(4) 0.1693(5) 0.088(3) Uani 0.661(9) d PDU 2 H46P H 0.2409(8) 0.0408(4) 0.1504(5) 0.132 Uiso 0.661(9) calc PR 2 H46Q H 0.1634(8) -0.0376(4) 0.1461(5) 0.132 Uiso 0.661(9) calc PR 2 H46R H 0.1394(8) 0.0053(4) 0.2357(5) 0.132 Uiso 0.661(9) calc PR 2 C47 C 0.0126(3) 0.1819(2) 0.2621(2) 0.0377(6) Uani 1 d . . H47 H -0.0034(3) 0.1259(2) 0.3022(2) 0.045 Uiso 1 calc R . C48 C 0.0074(3) 0.2603(2) 0.2978(2) 0.0345(5) Uani 1 d . . H48 H -0.0128(3) 0.2573(2) 0.3615(2) 0.041 Uiso 1 calc R . C5 C 0.0183(2) 0.5687(2) 0.37815(15) 0.0274(5) Uani 1 d . . O5 O 0.1354(2) 0.56536(11) 0.33786(11) 0.0306(4) Uani 1 d . . N6 N 0.4148(2) 0.39533(14) 0.00896(13) 0.0304(4) Uani 1 d . . C61 C 0.4842(2) 0.3019(2) 0.0193(2) 0.0312(5) Uani 1 d . . C62 C 0.6032(3) 0.2812(2) -0.0365(2) 0.0391(6) Uani 1 d . . H62 H 0.6392(3) 0.3292(2) -0.0789(2) 0.047 Uiso 1 calc R . C63 C 0.6676(3) 0.1891(2) -0.0286(2) 0.0511(8) Uani 1 d . . H63 H 0.7477(3) 0.1747(2) -0.0662(2) 0.061 Uiso 1 calc R . C64 C 0.6164(3) 0.1182(2) 0.0336(2) 0.0591(9) Uani 1 d . . H64 H 0.6608(3) 0.0558(2) 0.0384(2) 0.071 Uiso 1 calc R . C65 C 0.4990(3) 0.1398(2) 0.0888(2) 0.0576(9) Uani 1 d . . H65 H 0.4642(3) 0.0916(2) 0.1318(2) 0.069 Uiso 1 calc R . C66 C 0.4318(3) 0.2309(2) 0.0820(2) 0.0449(7) Uani 1 d . . H66 H 0.3514(3) 0.2447(2) 0.1196(2) 0.054 Uiso 1 calc R . N7 N 0.4173(2) 0.45305(14) -0.07887(13) 0.0323(5) Uani 1 d . . C8 C 0.3287(2) 0.5280(2) -0.0698(2) 0.0321(5) Uani 1 d . . C81 C 0.3046(3) 0.6069(2) -0.1492(2) 0.0477(7) Uani 1 d . . H81A H 0.3547(17) 0.6545(7) -0.1497(9) 0.072 Uiso 1 calc R . H81B H 0.2122(4) 0.6340(10) -0.1436(8) 0.072 Uiso 1 calc R . H81C H 0.3314(20) 0.5835(4) -0.2058(2) 0.072 Uiso 1 calc R . C9 C 0.2674(2) 0.5239(2) 0.0227(2) 0.0302(5) Uani 1 d . . C91 C 0.1646(2) 0.58764(14) 0.05115(13) 0.0193(4) Uani 1 d . . H91 H 0.1219(2) 0.63511(14) 0.00862(13) 0.023 Uiso 1 calc R . N92 N 0.1273(2) 0.58164(14) 0.13708(13) 0.0297(4) Uani 1 d . . C93 C 0.0087(2) 0.6470(2) 0.1577(2) 0.0287(5) Uani 1 d . . C94 C -0.1096(2) 0.6330(2) 0.1424(2) 0.0350(6) Uani 1 d . . H94 H -0.1123(2) 0.5834(2) 0.1144(2) 0.042 Uiso 1 calc R . C95 C -0.2244(3) 0.6922(2) 0.1686(2) 0.0378(6) Uani 1 d . . H95 H -0.3044(3) 0.6819(2) 0.1581(2) 0.045 Uiso 1 calc R . C96 C -0.2240(2) 0.7666(2) 0.2101(2) 0.0320(5) Uani 1 d . . C961 C -0.3532(3) 0.8284(2) 0.2427(2) 0.0382(6) Uani 1 d . . C962 C -0.3308(3) 0.9184(2) 0.2645(3) 0.0570(9) Uani 1 d . . H96A H -0.2735(3) 0.9027(2) 0.3109(3) 0.086 Uiso 1 calc R . H96B H -0.4140(3) 0.9540(2) 0.2873(3) 0.086 Uiso 1 calc R . H96C H -0.2907(3) 0.9557(2) 0.2094(3) 0.086 Uiso 1 calc R . C963 C -0.4435(3) 0.8551(2) 0.1699(2) 0.0570(8) Uani 1 d . . H96D H -0.4588(3) 0.7986(2) 0.1552(2) 0.085 Uiso 1 calc R . H96E H -0.4029(3) 0.8926(2) 0.1151(2) 0.085 Uiso 1 calc R . H96F H -0.5261(3) 0.8909(2) 0.1930(2) 0.085 Uiso 1 calc R . C964 C -0.4205(3) 0.7730(2) 0.3311(2) 0.0514(8) Uani 1 d . . H96G H -0.3632(3) 0.7560(2) 0.3774(2) 0.077 Uiso 1 calc R . H96H H -0.4393(3) 0.7166(2) 0.3185(2) 0.077 Uiso 1 calc R . H96I H -0.5016(3) 0.8115(2) 0.3530(2) 0.077 Uiso 1 calc R . C97 C -0.1038(2) 0.7799(2) 0.2232(2) 0.0333(5) Uani 1 d . . H97 H -0.1003(2) 0.8303(2) 0.2497(2) 0.040 Uiso 1 calc R . C98 C 0.0119(2) 0.7206(2) 0.1980(2) 0.0320(5) Uani 1 d . . H98 H 0.0920(2) 0.7306(2) 0.2085(2) 0.038 Uiso 1 calc R . C10 C 0.3274(2) 0.4374(2) 0.0731(2) 0.0272(5) Uani 1 d . . O10 O 0.3092(2) 0.40125(11) 0.15746(11) 0.0312(4) Uani 1 d . . O1M O 0.2774(2) 0.37822(13) 0.35002(11) 0.0383(4) Uani 1 d . . H1M10 H 0.2667(2) 0.40409(13) 0.39459(11) 0.057 Uiso 1 d R . C1M C 0.4019(4) 0.3235(3) 0.3488(2) 0.0751(12) Uani 1 d . . H1M1 H 0.4265(13) 0.2994(18) 0.2925(10) 0.113 Uiso 1 calc R . H1M2 H 0.4020(8) 0.2716(13) 0.4009(12) 0.113 Uiso 1 calc R . H1M3 H 0.4641(6) 0.3614(6) 0.3522(21) 0.113 Uiso 1 calc R . O1N O 0.3768(2) 0.54008(13) 0.22260(12) 0.0367(4) Uani 1 d . . H1N H 0.4371(2) 0.52928(13) 0.18042(12) 0.055 Uiso 1 d R . C1N C 0.4124(3) 0.5944(3) 0.2742(2) 0.0676(11) Uani 1 d . . H1N1 H 0.3592(19) 0.6566(7) 0.2650(15) 0.101 Uiso 1 calc R . H1N2 H 0.5040(8) 0.5991(17) 0.2550(14) 0.101 Uiso 1 calc R . H1N3 H 0.3989(26) 0.5653(10) 0.3387(3) 0.101 Uiso 1 calc R . O1S O 0.5879(4) 0.1133(3) 0.4574(3) 0.1043(11) Uani 1 d . . H1S H 0.6105(35) 0.0592(18) 0.4860(28) 0.156 Uiso 1 calc R . C1S C 0.6825(4) 0.1332(4) 0.3810(3) 0.0925(14) Uani 1 d . . H1S1 H 0.6397(4) 0.1644(4) 0.3280(3) 0.139 Uiso 1 d R . H1S2 H 0.7385(4) 0.0753(4) 0.3689(3) 0.139 Uiso 1 d R . H1S3 H 0.7350(4) 0.1738(4) 0.3931(3) 0.139 Uiso 1 d R . O1T O 0.3717(3) 0.0576(3) 0.4318(3) 0.1188(14) Uani 1 d . . H1T H 0.4408(41) 0.0776(47) 0.4260(13) 0.178 Uiso 1 calc R . C1T C 0.3241(5) 0.0821(5) 0.3482(3) 0.119(2) Uani 1 d . . H1T1 H 0.3010(5) 0.0272(5) 0.3356(3) 0.178 Uiso 1 d R . H1T2 H 0.3910(5) 0.1043(5) 0.2998(3) 0.178 Uiso 1 d R . H1T3 H 0.2472(5) 0.1310(5) 0.3511(3) 0.178 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0282(2) 0.0273(2) 0.0220(2) -0.0078(2) 0.0043(2) -0.0029(2) N1 0.0295(10) 0.0311(10) 0.0245(10) -0.0108(8) 0.0051(8) -0.0027(8) C11 0.0410(14) 0.0315(12) 0.0232(11) -0.0091(9) 0.0001(10) -0.0040(10) C12 0.0429(15) 0.0368(14) 0.0371(14) -0.0144(11) -0.0009(11) -0.0010(11) C13 0.064(2) 0.0354(14) 0.048(2) -0.0167(12) -0.0029(14) -0.0012(13) C14 0.071(2) 0.047(2) 0.062(2) -0.027(2) 0.007(2) -0.023(2) C15 0.052(2) 0.068(2) 0.082(2) -0.042(2) 0.014(2) -0.025(2) C16 0.0398(15) 0.049(2) 0.059(2) -0.0293(14) 0.0054(13) -0.0077(12) N2 0.0307(10) 0.0342(11) 0.0265(10) -0.0081(8) 0.0071(8) -0.0043(8) C3 0.0332(12) 0.0326(12) 0.0243(11) -0.0067(9) 0.0038(10) -0.0025(10) C31 0.0366(14) 0.048(2) 0.047(2) -0.0130(13) 0.0104(12) -0.0109(12) C4 0.0302(12) 0.0298(11) 0.0228(11) -0.0056(9) 0.0029(9) -0.0032(9) C41 0.0204(10) 0.0208(10) 0.0153(9) -0.0047(7) 0.0019(8) -0.0049(8) N42 0.0328(10) 0.0266(10) 0.0241(10) -0.0072(8) -0.0003(8) -0.0034(8) C43 0.0281(11) 0.0285(11) 0.0283(12) -0.0104(9) -0.0001(9) -0.0047(9) C44 0.0396(13) 0.0355(13) 0.0262(12) -0.0071(10) 0.0021(10) -0.0098(11) C45 0.0439(14) 0.0425(14) 0.0253(12) -0.0123(10) -0.0003(11) -0.0116(11) C46 0.0339(13) 0.0361(13) 0.0337(13) -0.0138(10) -0.0012(10) -0.0092(10) C461 0.059(2) 0.046(2) 0.043(2) -0.0229(13) 0.0046(14) -0.0211(14) C462 0.151(15) 0.041(6) 0.075(8) -0.019(5) -0.015(9) -0.035(8) C463 0.114(12) 0.090(11) 0.129(14) -0.087(11) 0.054(10) -0.039(10) C464 0.087(9) 0.079(9) 0.153(15) -0.073(10) -0.041(9) -0.018(7) C465 0.149(8) 0.065(4) 0.043(3) -0.033(3) 0.016(4) -0.053(5) C466 0.102(5) 0.097(6) 0.093(5) -0.056(5) 0.028(4) -0.070(5) C467 0.120(6) 0.049(3) 0.100(5) -0.040(4) -0.027(5) 0.010(4) C47 0.048(2) 0.0325(13) 0.0326(13) -0.0056(10) -0.0007(11) -0.0138(11) C48 0.0450(14) 0.0350(13) 0.0233(12) -0.0067(10) -0.0009(10) -0.0095(11) C5 0.0309(12) 0.0276(11) 0.0202(11) -0.0065(9) 0.0010(9) 0.0002(9) O5 0.0280(8) 0.0331(9) 0.0292(8) -0.0125(7) 0.0052(7) -0.0037(7) N6 0.0330(10) 0.0306(10) 0.0236(10) -0.0085(8) 0.0061(8) -0.0031(8) C61 0.0343(13) 0.0300(12) 0.0281(12) -0.0110(9) 0.0019(10) -0.0030(10) C62 0.0369(14) 0.0384(14) 0.0371(14) -0.0108(11) 0.0062(11) -0.0033(11) C63 0.045(2) 0.044(2) 0.052(2) -0.0122(13) 0.0101(13) 0.0064(13) C64 0.067(2) 0.037(2) 0.057(2) -0.0082(14) 0.007(2) 0.0105(14) C65 0.068(2) 0.0351(15) 0.055(2) -0.0020(13) 0.014(2) -0.0041(14) C66 0.047(2) 0.0375(14) 0.0416(15) -0.0090(12) 0.0126(12) -0.0042(12) N7 0.0335(11) 0.0362(11) 0.0235(10) -0.0068(8) 0.0045(8) -0.0048(9) C8 0.0304(12) 0.0369(13) 0.0263(12) -0.0072(10) 0.0034(10) -0.0060(10) C81 0.048(2) 0.053(2) 0.0281(13) 0.0005(12) 0.0068(12) 0.0016(13) C9 0.0308(12) 0.0332(12) 0.0249(12) -0.0083(9) 0.0019(10) -0.0051(10) C91 0.0182(9) 0.0223(10) 0.0144(9) -0.0035(8) 0.0021(8) -0.0014(8) N92 0.0283(10) 0.0289(10) 0.0292(10) -0.0092(8) 0.0031(8) -0.0020(8) C93 0.0286(12) 0.0283(11) 0.0235(11) -0.0049(9) 0.0036(9) 0.0002(9) C94 0.0351(13) 0.0337(13) 0.0366(13) -0.0132(10) 0.0001(11) -0.0052(10) C95 0.0291(12) 0.0365(13) 0.048(2) -0.0131(11) -0.0012(11) -0.0055(10) C96 0.0322(12) 0.0285(12) 0.0303(12) -0.0058(9) 0.0021(10) -0.0005(10) C961 0.0322(13) 0.0331(13) 0.0452(15) -0.0119(11) 0.0015(11) 0.0014(10) C962 0.042(2) 0.038(2) 0.090(3) -0.028(2) -0.003(2) 0.0057(12) C963 0.045(2) 0.055(2) 0.065(2) -0.016(2) -0.014(2) 0.0136(14) C964 0.042(2) 0.054(2) 0.051(2) -0.0145(14) 0.0121(13) -0.0053(13) C97 0.0358(13) 0.0285(12) 0.0340(13) -0.0103(10) -0.0015(10) -0.0014(10) C98 0.0301(12) 0.0313(12) 0.0335(13) -0.0087(10) -0.0021(10) -0.0032(10) C10 0.0277(11) 0.0299(11) 0.0248(11) -0.0102(9) 0.0020(9) -0.0064(9) O10 0.0366(9) 0.0291(8) 0.0232(8) -0.0070(6) 0.0045(7) -0.0021(7) O1M 0.0396(10) 0.0422(10) 0.0241(8) -0.0072(7) 0.0032(7) 0.0059(8) C1M 0.065(2) 0.083(3) 0.042(2) 0.002(2) 0.006(2) 0.034(2) O1N 0.0330(9) 0.0474(10) 0.0311(9) -0.0164(8) 0.0098(7) -0.0137(8) C1N 0.058(2) 0.112(3) 0.052(2) -0.047(2) 0.019(2) -0.046(2) O1S 0.094(2) 0.103(3) 0.103(3) -0.008(2) 0.003(2) -0.020(2) C1S 0.068(3) 0.104(4) 0.095(3) -0.019(3) -0.001(2) -0.001(2) O1T 0.062(2) 0.168(4) 0.101(3) 0.026(2) -0.027(2) -0.010(2) C1T 0.072(3) 0.184(6) 0.075(3) -0.008(3) -0.009(3) 0.011(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 O5 2.012(2) . ? Ni1 O10 2.017(2) . ? Ni1 N92 2.085(2) . ? Ni1 N42 2.088(2) . ? Ni1 O1M 2.101(2) . ? Ni1 O1N 2.126(2) . ? N1 C5 1.374(3) . ? N1 N2 1.403(3) . ? N1 C11 1.415(3) . ? C11 C16 1.386(4) . ? C11 C12 1.388(3) . ? C12 C13 1.379(4) . ? C13 C14 1.373(5) . ? C14 C15 1.380(5) . ? C15 C16 1.382(4) . ? N2 C3 1.313(3) . ? C3 C4 1.418(3) . ? C3 C31 1.486(4) . ? C4 C41 1.355(3) . ? C4 C5 1.415(3) . ? C41 N42 1.277(3) . ? N42 C43 1.438(3) . ? C43 C48 1.383(3) . ? C43 C44 1.383(3) . ? C44 C45 1.384(3) . ? C45 C46 1.389(4) . ? C46 C47 1.394(4) . ? C46 C461 1.525(3) . ? C461 C462 1.488(6) . ? C461 C463 1.500(7) . ? C461 C466 1.509(5) . ? C461 C465 1.510(5) . ? C461 C464 1.557(7) . ? C461 C467 1.570(5) . ? C47 C48 1.382(3) . ? C5 O5 1.269(3) . ? N6 C10 1.372(3) . ? N6 N7 1.408(3) . ? N6 C61 1.415(3) . ? C61 C66 1.386(4) . ? C61 C62 1.394(3) . ? C62 C63 1.383(4) . ? C63 C64 1.376(4) . ? C64 C65 1.379(4) . ? C65 C66 1.381(4) . ? N7 C8 1.310(3) . ? C8 C9 1.422(3) . ? C8 C81 1.494(4) . ? C9 C91 1.354(3) . ? C9 C10 1.423(3) . ? C91 N92 1.275(3) . ? N92 C93 1.444(3) . ? C93 C98 1.381(3) . ? C93 C94 1.382(4) . ? C94 C95 1.388(3) . ? C95 C96 1.396(4) . ? C96 C97 1.386(4) . ? C96 C961 1.540(3) . ? C961 C963 1.524(4) . ? C961 C962 1.528(4) . ? C961 C964 1.538(4) . ? C97 C98 1.391(3) . ? C10 O10 1.263(3) . ? O1M C1M 1.391(3) . ? O1N C1N 1.394(3) . ? O1S C1S 1.401(5) . ? O1T C1T 1.394(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 O5 Ni1 O10 167.63(7) . . ? O5 Ni1 N92 94.65(7) . . ? O10 Ni1 N92 91.52(7) . . ? O5 Ni1 N42 92.19(7) . . ? O10 Ni1 N42 98.41(7) . . ? N92 Ni1 N42 91.10(8) . . ? O5 Ni1 O1M 87.72(7) . . ? O10 Ni1 O1M 86.49(7) . . ? N92 Ni1 O1M 177.03(8) . . ? N42 Ni1 O1M 87.02(8) . . ? O5 Ni1 O1N 85.58(7) . . ? O10 Ni1 O1N 83.44(7) . . ? N92 Ni1 O1N 92.60(8) . . ? N42 Ni1 O1N 175.82(7) . . ? O1M Ni1 O1N 89.36(7) . . ? C5 N1 N2 111.3(2) . . ? C5 N1 C11 128.0(2) . . ? N2 N1 C11 118.9(2) . . ? C16 C11 C12 119.5(2) . . ? C16 C11 N1 120.8(2) . . ? C12 C11 N1 119.8(2) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 121.2(3) . . ? C13 C14 C15 118.9(3) . . ? C14 C15 C16 121.0(3) . . ? C15 C16 C11 119.7(3) . . ? C3 N2 N1 106.0(2) . . ? N2 C3 C4 111.4(2) . . ? N2 C3 C31 121.3(2) . . ? C4 C3 C31 127.2(2) . . ? C41 C4 C5 130.4(2) . . ? C41 C4 C3 123.5(2) . . ? C5 C4 C3 106.1(2) . . ? N42 C41 C4 118.8(2) . . ? C41 N42 C43 111.9(2) . . ? C41 N42 Ni1 128.0(2) . . ? C43 N42 Ni1 119.54(14) . . ? C48 C43 C44 119.7(2) . . ? C48 C43 N42 120.7(2) . . ? C44 C43 N42 119.5(2) . . ? C43 C44 C45 119.7(2) . . ? C44 C45 C46 121.9(2) . . ? C45 C46 C47 117.1(2) . . ? C45 C46 C461 121.9(2) . . ? C47 C46 C461 120.9(2) . . ? C462 C461 C463 112.8(5) . . ? C466 C461 C465 110.9(4) . . ? C462 C461 C46 115.0(5) . . ? C463 C461 C46 109.8(6) . . ? C466 C461 C46 111.4(3) . . ? C465 C461 C46 113.7(3) . . ? C462 C461 C464 108.6(5) . . ? C463 C461 C464 107.7(5) . . ? C46 C461 C464 102.1(4) . . ? C466 C461 C467 106.6(4) . . ? C465 C461 C467 105.9(4) . . ? C46 C461 C467 107.9(3) . . ? C48 C47 C46 121.6(2) . . ? C47 C48 C43 119.9(2) . . ? O5 C5 N1 124.3(2) . . ? O5 C5 C4 130.4(2) . . ? N1 C5 C4 105.2(2) . . ? C5 O5 Ni1 119.3(2) . . ? C10 N6 N7 111.5(2) . . ? C10 N6 C61 128.3(2) . . ? N7 N6 C61 119.7(2) . . ? C66 C61 C62 120.2(2) . . ? C66 C61 N6 120.2(2) . . ? C62 C61 N6 119.6(2) . . ? C63 C62 C61 119.2(3) . . ? C64 C63 C62 121.0(3) . . ? C63 C64 C65 119.2(3) . . ? C64 C65 C66 121.2(3) . . ? C65 C66 C61 119.2(3) . . ? C8 N7 N6 106.0(2) . . ? N7 C8 C9 111.4(2) . . ? N7 C8 C81 121.5(2) . . ? C9 C8 C81 127.1(2) . . ? C91 C9 C8 124.4(2) . . ? C91 C9 C10 129.2(2) . . ? C8 C9 C10 106.1(2) . . ? N92 C91 C9 118.3(2) . . ? C91 N92 C93 112.6(2) . . ? C91 N92 Ni1 128.3(2) . . ? C93 N92 Ni1 118.71(14) . . ? C98 C93 C94 119.7(2) . . ? C98 C93 N92 120.0(2) . . ? C94 C93 N92 120.2(2) . . ? C93 C94 C95 119.9(2) . . ? C94 C95 C96 121.6(2) . . ? C97 C96 C95 117.3(2) . . ? C97 C96 C961 122.1(2) . . ? C95 C96 C961 120.6(2) . . ? C963 C961 C962 108.4(3) . . ? C963 C961 C964 109.4(3) . . ? C962 C961 C964 107.7(2) . . ? C963 C961 C96 110.7(2) . . ? C962 C961 C96 112.0(2) . . ? C964 C961 C96 108.5(2) . . ? C96 C97 C98 121.7(2) . . ? C93 C98 C97 119.9(2) . . ? O10 C10 N6 123.9(2) . . ? O10 C10 C9 131.2(2) . . ? N6 C10 C9 104.9(2) . . ? C10 O10 Ni1 118.03(14) . . ? C1M O1M Ni1 128.0(2) . . ? C1N O1N Ni1 128.6(2) . . ? _refine_diff_density_max 0.616 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.053 data_leco86 _database_code_CSD 158376 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(C20 H21 N4 O)3].3MeOH' _chemical_formula_sum 'C63 H75 Co N12 O6' _chemical_formula_weight 1155.28 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' '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 12.965(6) _cell_length_b 15.604(6) _cell_length_c 15.584(6) _cell_angle_alpha 75.83(3) _cell_angle_beta 85.67(3) _cell_angle_gamma 86.50(4) _cell_volume 3045(2) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 13.0 _exptl_crystal_description wedge _exptl_crystal_colour Red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.8529 _exptl_absorpt_correction_T_max 0.8984 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 ? _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 11442 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10736 _reflns_number_gt 5471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10736 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1758 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19337(6) 0.47229(5) 0.27834(5) 0.0262(2) Uani 1 1 d . . . N1A N 0.3150(4) 0.5284(3) 0.4898(3) 0.0310(12) Uani 1 1 d . . . C11A C 0.3794(5) 0.6004(4) 0.4749(4) 0.0292(14) Uani 1 1 d . . . C12A C 0.4647(5) 0.5970(4) 0.5239(4) 0.0367(15) Uani 1 1 d . . . H12A H 0.4806 0.5454 0.5673 0.044 Uiso 1 1 calc R . . C13A C 0.5258(5) 0.6672(5) 0.5101(5) 0.0452(17) Uani 1 1 d . . . H13A H 0.5831 0.6639 0.5444 0.054 Uiso 1 1 calc R . . C14A C 0.5045(6) 0.7435(5) 0.4458(5) 0.053(2) Uani 1 1 d . . . H14A H 0.5474 0.7919 0.4357 0.063 Uiso 1 1 calc R . . C15A C 0.4199(5) 0.7475(4) 0.3971(4) 0.0459(18) Uani 1 1 d . . . H15A H 0.4053 0.7992 0.3534 0.055 Uiso 1 1 calc R . . C16A C 0.3556(5) 0.6775(4) 0.4106(4) 0.0398(16) Uani 1 1 d . . . H16A H 0.2972 0.6816 0.3774 0.048 Uiso 1 1 calc R . . N2A N 0.2998(4) 0.4745(3) 0.5767(3) 0.0329(12) Uani 1 1 d . . . C3A C 0.2338(5) 0.4163(4) 0.5726(4) 0.0307(14) Uani 1 1 d . . . C31A C 0.1999(5) 0.3462(4) 0.6522(4) 0.0418(17) Uani 1 1 d . . . H31A H 0.2325 0.3539 0.7037 0.063 Uiso 1 1 calc R . . H31B H 0.2201 0.2884 0.6423 0.063 Uiso 1 1 calc R . . H31C H 0.1253 0.3510 0.6622 0.063 Uiso 1 1 calc R . . C4A C 0.2034(4) 0.4280(4) 0.4838(4) 0.0278(13) Uani 1 1 d . . . N41A N 0.1273(4) 0.3866(3) 0.4597(3) 0.0276(11) Uani 1 1 d . . . N42A N 0.1075(4) 0.4054(3) 0.3785(3) 0.0277(11) Uani 1 1 d . . . C43A C 0.0194(5) 0.3604(4) 0.3624(3) 0.0279(14) Uani 1 1 d . . . C44A C -0.0774(4) 0.4011(4) 0.3610(4) 0.0308(14) Uani 1 1 d . . . H44A H -0.0870 0.4573 0.3730 0.037 Uiso 1 1 calc R . . C45A C -0.1604(5) 0.3598(4) 0.3423(4) 0.0355(15) Uani 1 1 d . . . H45A H -0.2266 0.3879 0.3431 0.043 Uiso 1 1 calc R . . C46A C -0.1495(5) 0.2767(4) 0.3218(4) 0.0345(15) Uani 1 1 d . . . C47A C -0.0516(5) 0.2378(4) 0.3254(4) 0.0388(16) Uani 1 1 d . . . H47A H -0.0412 0.1817 0.3132 0.047 Uiso 1 1 calc R . . C48A C 0.0320(5) 0.2776(4) 0.3460(4) 0.0357(15) Uani 1 1 d . . . H48A H 0.0976 0.2481 0.3489 0.043 Uiso 1 1 calc R . . C49A C -0.2424(5) 0.2351(5) 0.2966(4) 0.0452(17) Uani 1 1 d . . . C50A C -0.3266(7) 0.2228(7) 0.3713(6) 0.104(4) Uani 1 1 d . . . H50A H -0.3444 0.2791 0.3858 0.155 Uiso 1 1 calc R . . H50B H -0.3019 0.1807 0.4231 0.155 Uiso 1 1 calc R . . H50C H -0.3874 0.2008 0.3526 0.155 Uiso 1 1 calc R . . C51A C -0.2147(7) 0.1475(6) 0.2739(8) 0.112(4) Uani 1 1 d . . . H51A H -0.1609 0.1554 0.2263 0.168 Uiso 1 1 calc R . . H51B H -0.2755 0.1255 0.2553 0.168 Uiso 1 1 calc R . . H51C H -0.1899 0.1054 0.3257 0.168 Uiso 1 1 calc R . . C52A C -0.2858(7) 0.2966(6) 0.2133(6) 0.090(3) Uani 1 1 d . . . H52A H -0.3047 0.3541 0.2246 0.135 Uiso 1 1 calc R . . H52B H -0.3466 0.2714 0.1982 0.135 Uiso 1 1 calc R . . H52C H -0.2337 0.3031 0.1644 0.135 Uiso 1 1 calc R . . C5A C 0.2597(4) 0.4998(4) 0.4328(4) 0.0268(13) Uani 1 1 d . . . O5A O 0.2608(3) 0.5334(2) 0.3489(2) 0.0299(9) Uani 1 1 d . . . N1B N 0.0247(4) 0.3789(3) 0.1132(3) 0.0317(12) Uani 1 1 d . . . C11B C 0.0590(5) 0.2972(4) 0.0960(4) 0.0319(14) Uani 1 1 d . . . C12B C 0.0047(6) 0.2624(5) 0.0410(5) 0.055(2) Uani 1 1 d . . . H12B H -0.0538 0.2935 0.0146 0.066 Uiso 1 1 calc R . . C13B C 0.0367(7) 0.1815(5) 0.0246(6) 0.072(2) Uani 1 1 d . . . H13B H -0.0003 0.1577 -0.0130 0.086 Uiso 1 1 calc R . . C14B C 0.1222(7) 0.1355(5) 0.0628(6) 0.070(2) Uani 1 1 d . . . H14B H 0.1427 0.0796 0.0532 0.084 Uiso 1 1 calc R . . C15B C 0.1758(7) 0.1720(5) 0.1140(5) 0.070(2) Uani 1 1 d . . . H15B H 0.2357 0.1418 0.1385 0.084 Uiso 1 1 calc R . . C16B C 0.1464(6) 0.2510(5) 0.1316(5) 0.054(2) Uani 1 1 d . . . H16B H 0.1856 0.2745 0.1680 0.065 Uiso 1 1 calc R . . N2B N -0.0680(4) 0.4205(3) 0.0791(3) 0.0357(12) Uani 1 1 d . . . C3B C -0.0813(5) 0.4934(4) 0.1061(4) 0.0322(14) Uani 1 1 d . . . C31B C -0.1762(5) 0.5530(4) 0.0866(4) 0.0472(18) Uani 1 1 d . . . H31D H -0.2190 0.5302 0.0496 0.071 Uiso 1 1 calc R . . H31E H -0.1559 0.6120 0.0559 0.071 Uiso 1 1 calc R . . H31F H -0.2150 0.5553 0.1418 0.071 Uiso 1 1 calc R . . C4B C 0.0010(4) 0.5028(4) 0.1576(4) 0.0274(13) Uani 1 1 d . . . N41B N 0.0104(4) 0.5687(3) 0.1976(3) 0.0304(12) Uani 1 1 d . . . N42B N 0.0854(4) 0.5658(3) 0.2494(3) 0.0292(12) Uani 1 1 d . . . C43B C 0.0826(4) 0.6474(4) 0.2791(4) 0.0295(14) Uani 1 1 d . . . C44B C 0.0763(4) 0.6469(4) 0.3689(4) 0.0302(14) Uani 1 1 d . . . H44B H 0.0765 0.5929 0.4119 0.036 Uiso 1 1 calc R . . C45B C 0.0700(5) 0.7241(4) 0.3943(4) 0.0368(15) Uani 1 1 d . . . H45B H 0.0665 0.7218 0.4553 0.044 Uiso 1 1 calc R . . C46B C 0.0684(5) 0.8064(4) 0.3349(4) 0.0413(16) Uani 1 1 d . . . C47B C 0.0721(5) 0.8056(4) 0.2447(4) 0.0429(17) Uani 1 1 d . . . H47B H 0.0695 0.8595 0.2016 0.051 Uiso 1 1 calc R . . C48B C 0.0793(5) 0.7282(4) 0.2187(4) 0.0450(18) Uani 1 1 d . . . H48B H 0.0822 0.7300 0.1579 0.054 Uiso 1 1 calc R . . C49B C 0.0599(6) 0.8917(5) 0.3650(5) 0.057(2) Uani 1 1 d . . . C50B C 0.0643(12) 0.9737(5) 0.2907(7) 0.154(6) Uani 1 1 d . . . H50D H 0.0117 0.9727 0.2500 0.231 Uiso 1 1 calc R . . H50E H 0.1321 0.9760 0.2595 0.231 Uiso 1 1 calc R . . H50F H 0.0520 1.0255 0.3147 0.231 Uiso 1 1 calc R . . C51B C 0.1396(9) 0.8896(6) 0.4307(8) 0.118(4) Uani 1 1 d . . . H51D H 0.1342 0.8359 0.4775 0.177 Uiso 1 1 calc R . . H51E H 0.1278 0.9406 0.4559 0.177 Uiso 1 1 calc R . . H51F H 0.2081 0.8910 0.4010 0.177 Uiso 1 1 calc R . . C52B C -0.0439(8) 0.8968(6) 0.4168(7) 0.119(4) Uani 1 1 d . . . H52D H -0.0497 0.8449 0.4658 0.178 Uiso 1 1 calc R . . H52E H -0.0996 0.8993 0.3780 0.178 Uiso 1 1 calc R . . H52F H -0.0483 0.9495 0.4397 0.178 Uiso 1 1 calc R . . C5B C 0.0665(5) 0.4276(4) 0.1625(3) 0.0277(14) Uani 1 1 d . . . O5B O 0.1491(3) 0.4042(2) 0.2035(2) 0.0287(9) Uani 1 1 d . . . N1C N 0.3832(4) 0.2642(3) 0.2515(3) 0.0349(12) Uani 1 1 d . . . C11C C 0.3778(5) 0.1830(4) 0.3187(4) 0.0391(16) Uani 1 1 d . . . C12C C 0.4261(6) 0.1086(4) 0.3045(5) 0.061(2) Uani 1 1 d . . . H12C H 0.4630 0.1105 0.2498 0.073 Uiso 1 1 calc R . . C13C C 0.4232(8) 0.0300(5) 0.3672(6) 0.082(3) Uani 1 1 d . . . H13C H 0.4572 -0.0212 0.3552 0.099 Uiso 1 1 calc R . . C14C C 0.3704(7) 0.0262(5) 0.4477(6) 0.071(3) Uani 1 1 d . . . H14C H 0.3681 -0.0272 0.4915 0.086 Uiso 1 1 calc R . . C15C C 0.3212(6) 0.1019(5) 0.4627(5) 0.062(2) Uani 1 1 d . . . H15C H 0.2845 0.0993 0.5176 0.075 Uiso 1 1 calc R . . C16C C 0.3232(5) 0.1827(4) 0.3997(4) 0.0430(17) Uani 1 1 d . . . H16C H 0.2897 0.2343 0.4112 0.052 Uiso 1 1 calc R . . N2C N 0.4353(4) 0.2595(3) 0.1692(3) 0.0416(14) Uani 1 1 d . . . C3C C 0.4261(5) 0.3410(4) 0.1179(4) 0.0401(16) Uani 1 1 d . . . C31C C 0.4723(6) 0.3628(5) 0.0256(4) 0.060(2) Uani 1 1 d . . . H31G H 0.5093 0.3108 0.0132 0.090 Uiso 1 1 calc R . . H31H H 0.5199 0.4100 0.0184 0.090 Uiso 1 1 calc R . . H31I H 0.4178 0.3819 -0.0152 0.090 Uiso 1 1 calc R . . C4C C 0.3664(5) 0.3969(4) 0.1627(4) 0.0323(14) Uani 1 1 d . . . N41C N 0.3476(4) 0.4843(3) 0.1312(3) 0.0329(12) Uani 1 1 d . . . N42C N 0.2854(4) 0.5278(3) 0.1749(3) 0.0297(12) Uani 1 1 d . . . C43C C 0.2880(4) 0.6203(4) 0.1377(4) 0.0281(14) Uani 1 1 d . . . C44C C 0.2516(5) 0.6565(4) 0.0541(4) 0.0355(15) Uani 1 1 d . . . H44C H 0.2212 0.6208 0.0233 0.043 Uiso 1 1 calc R . . C45C C 0.2610(5) 0.7466(4) 0.0171(4) 0.0388(16) Uani 1 1 d . . . H45C H 0.2353 0.7709 -0.0389 0.047 Uiso 1 1 calc R . . C46C C 0.3063(5) 0.8018(4) 0.0585(4) 0.0360(15) Uani 1 1 d . . . C47C C 0.3408(5) 0.7644(4) 0.1417(4) 0.0429(17) Uani 1 1 d . . . H47C H 0.3710 0.8001 0.1726 0.052 Uiso 1 1 calc R . . C48C C 0.3315(5) 0.6744(4) 0.1804(4) 0.0400(16) Uani 1 1 d . . . H48C H 0.3556 0.6506 0.2371 0.048 Uiso 1 1 calc R . . C49C C 0.3219(6) 0.8989(4) 0.0123(4) 0.0469(18) Uani 1 1 d . . . C50C C 0.4107(7) 0.9019(5) -0.0598(6) 0.095(3) Uani 1 1 d . . . H50G H 0.3943 0.8665 -0.0997 0.143 Uiso 1 1 calc R . . H50H H 0.4744 0.8785 -0.0321 0.143 Uiso 1 1 calc R . . H50I H 0.4193 0.9626 -0.0929 0.143 Uiso 1 1 calc R . . C51C C 0.3461(7) 0.9537(5) 0.0752(6) 0.076(3) Uani 1 1 d . . . H51G H 0.4080 0.9290 0.1052 0.114 Uiso 1 1 calc R . . H51H H 0.2884 0.9534 0.1187 0.114 Uiso 1 1 calc R . . H51I H 0.3574 1.0140 0.0422 0.114 Uiso 1 1 calc R . . C52C C 0.2249(6) 0.9400(4) -0.0328(5) 0.064(2) Uani 1 1 d . . . H52G H 0.2073 0.9062 -0.0738 0.096 Uiso 1 1 calc R . . H52H H 0.2371 1.0005 -0.0650 0.096 Uiso 1 1 calc R . . H52I H 0.1682 0.9397 0.0116 0.096 Uiso 1 1 calc R . . C5C C 0.3407(4) 0.3463(4) 0.2486(4) 0.0278(13) Uani 1 1 d . . . O5C O 0.2913(3) 0.3713(2) 0.3138(2) 0.0316(10) Uani 1 1 d . . . O1L O 0.3967(5) 0.2388(4) 0.8092(5) 0.108(2) Uani 1 1 d . . . H1L H 0.4121 0.2914 0.7927 0.161 Uiso 1 1 d R . . C1L C 0.3282(11) 0.2276(7) 0.8845(7) 0.133(5) Uani 1 1 d . . . H1L1 H 0.3334 0.1667 0.9185 0.199 Uiso 1 1 d R . . H1L2 H 0.2580 0.2421 0.8665 0.199 Uiso 1 1 d R . . H1L3 H 0.3457 0.2665 0.9207 0.199 Uiso 1 1 d R . . O1M O 0.3995(6) 0.4198(4) 0.7374(4) 0.127(3) Uani 1 1 d . . . H1M H 0.4150 0.4224 0.6842 0.190 Uiso 1 1 d R . . C1M C 0.4521(7) 0.4789(6) 0.7635(5) 0.075(3) Uani 1 1 d . . . H1M1 H 0.4180 0.5370 0.7454 0.113 Uiso 1 1 d R . . H1M2 H 0.5221 0.4803 0.7364 0.113 Uiso 1 1 d R . . H1M3 H 0.4545 0.4624 0.8275 0.113 Uiso 1 1 d R . . O1N O 0.4166(10) 0.0953(6) 0.7468(6) 0.169(4) Uani 1 1 d . . . H1N H 0.4177 0.1408 0.7652 0.254 Uiso 1 1 d R . . C1N C 0.3148(14) 0.0861(11) 0.7217(10) 0.176(8) Uani 1 1 d . . . H1N1 H 0.3189 0.0526 0.6767 0.264 Uiso 1 1 d R . . H1N2 H 0.2831 0.1443 0.6983 0.264 Uiso 1 1 d R . . H1N3 H 0.2732 0.0554 0.7732 0.264 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0289(5) 0.0316(5) 0.0170(4) -0.0039(3) 0.0020(3) -0.0045(4) N1A 0.035(3) 0.037(3) 0.019(3) -0.003(2) 0.002(2) -0.007(2) C11A 0.034(4) 0.033(4) 0.025(3) -0.015(3) 0.003(3) -0.005(3) C12A 0.033(4) 0.047(4) 0.033(4) -0.015(3) -0.003(3) -0.002(3) C13A 0.033(4) 0.056(5) 0.053(4) -0.026(4) -0.001(3) -0.011(4) C14A 0.049(5) 0.058(5) 0.055(5) -0.023(4) 0.015(4) -0.025(4) C15A 0.054(5) 0.043(4) 0.039(4) -0.003(3) 0.000(3) -0.017(4) C16A 0.045(4) 0.046(4) 0.030(4) -0.013(3) -0.003(3) -0.005(3) N2A 0.037(3) 0.044(3) 0.018(3) -0.007(2) -0.003(2) -0.005(3) C3A 0.030(4) 0.037(4) 0.023(3) -0.006(3) 0.002(3) -0.002(3) C31A 0.044(4) 0.048(4) 0.027(3) 0.004(3) -0.002(3) -0.008(3) C4A 0.029(3) 0.034(3) 0.021(3) -0.006(3) 0.001(3) -0.006(3) N41A 0.028(3) 0.032(3) 0.022(3) -0.005(2) 0.002(2) -0.004(2) N42A 0.028(3) 0.034(3) 0.020(3) -0.005(2) 0.001(2) -0.003(2) C43A 0.033(4) 0.031(3) 0.020(3) -0.005(3) 0.002(3) -0.009(3) C44A 0.031(4) 0.033(3) 0.030(3) -0.011(3) -0.001(3) -0.001(3) C45A 0.026(4) 0.042(4) 0.039(4) -0.012(3) 0.002(3) 0.000(3) C46A 0.030(4) 0.047(4) 0.027(3) -0.007(3) 0.005(3) -0.017(3) C47A 0.034(4) 0.032(4) 0.055(4) -0.017(3) 0.000(3) -0.012(3) C48A 0.028(4) 0.034(4) 0.043(4) -0.008(3) 0.001(3) -0.001(3) C49A 0.036(4) 0.057(5) 0.048(4) -0.020(4) 0.000(3) -0.013(3) C50A 0.075(7) 0.170(10) 0.081(7) -0.054(7) 0.032(5) -0.077(7) C51A 0.079(7) 0.093(7) 0.197(12) -0.085(8) -0.039(7) -0.009(6) C52A 0.076(7) 0.122(8) 0.080(6) -0.022(6) -0.033(5) -0.037(6) C5A 0.027(3) 0.032(3) 0.021(3) -0.007(3) 0.000(3) -0.001(3) O5A 0.033(2) 0.036(2) 0.021(2) -0.0056(18) -0.0018(18) -0.0065(19) N1B 0.031(3) 0.040(3) 0.025(3) -0.010(2) -0.005(2) -0.005(2) C11B 0.039(4) 0.033(4) 0.025(3) -0.010(3) 0.001(3) -0.008(3) C12B 0.063(5) 0.051(5) 0.060(5) -0.027(4) -0.018(4) 0.000(4) C13B 0.079(6) 0.063(5) 0.090(7) -0.045(5) -0.011(5) -0.007(5) C14B 0.090(7) 0.049(5) 0.079(6) -0.031(4) -0.016(5) 0.010(5) C15B 0.079(6) 0.061(5) 0.078(6) -0.032(5) -0.034(5) 0.021(5) C16B 0.060(5) 0.053(5) 0.061(5) -0.028(4) -0.029(4) 0.009(4) N2B 0.034(3) 0.044(3) 0.029(3) -0.007(2) -0.006(2) -0.004(3) C3B 0.031(4) 0.038(4) 0.026(3) -0.004(3) 0.002(3) -0.006(3) C31B 0.039(4) 0.057(5) 0.044(4) -0.007(3) -0.013(3) 0.004(3) C4B 0.029(3) 0.028(3) 0.021(3) 0.001(3) -0.001(3) -0.002(3) N41B 0.029(3) 0.034(3) 0.023(3) 0.000(2) 0.003(2) 0.001(2) N42B 0.038(3) 0.031(3) 0.019(3) -0.006(2) 0.004(2) -0.009(2) C43B 0.033(4) 0.027(3) 0.028(3) -0.008(3) 0.006(3) -0.002(3) C44B 0.037(4) 0.032(3) 0.022(3) -0.007(3) 0.000(3) -0.003(3) C45B 0.039(4) 0.048(4) 0.026(3) -0.016(3) 0.006(3) -0.004(3) C46B 0.043(4) 0.040(4) 0.043(4) -0.017(3) 0.004(3) 0.000(3) C47B 0.060(5) 0.032(4) 0.034(4) -0.006(3) 0.011(3) -0.002(3) C48B 0.067(5) 0.043(4) 0.023(3) -0.006(3) 0.003(3) -0.001(4) C49B 0.062(5) 0.050(5) 0.066(5) -0.030(4) 0.005(4) 0.004(4) C50B 0.34(2) 0.035(5) 0.084(8) -0.020(5) 0.041(10) -0.019(8) C51B 0.141(10) 0.082(7) 0.161(11) -0.076(7) -0.060(9) 0.006(7) C52B 0.137(10) 0.093(8) 0.135(10) -0.065(7) 0.038(8) 0.019(7) C5B 0.030(4) 0.036(4) 0.015(3) -0.001(3) 0.003(3) -0.008(3) O5B 0.025(2) 0.038(2) 0.024(2) -0.0092(18) -0.0037(18) 0.0007(18) N1C 0.035(3) 0.036(3) 0.031(3) -0.005(2) 0.000(2) 0.006(2) C11C 0.037(4) 0.038(4) 0.041(4) -0.005(3) -0.009(3) 0.001(3) C12C 0.072(6) 0.038(4) 0.066(5) -0.002(4) 0.007(4) 0.006(4) C13C 0.116(8) 0.032(4) 0.084(7) 0.003(4) 0.013(6) 0.012(5) C14C 0.087(7) 0.034(5) 0.077(6) 0.018(4) -0.011(5) -0.003(4) C15C 0.069(6) 0.055(5) 0.053(5) 0.008(4) 0.003(4) -0.024(4) C16C 0.053(5) 0.037(4) 0.037(4) -0.004(3) -0.005(3) -0.007(3) N2C 0.043(3) 0.040(3) 0.040(3) -0.011(3) 0.009(3) 0.004(3) C3C 0.038(4) 0.039(4) 0.041(4) -0.010(3) 0.007(3) 0.004(3) C31C 0.073(6) 0.061(5) 0.040(4) -0.012(4) 0.028(4) 0.009(4) C4C 0.037(4) 0.034(4) 0.025(3) -0.006(3) 0.008(3) -0.007(3) N41C 0.036(3) 0.035(3) 0.029(3) -0.009(2) 0.001(2) -0.006(2) N42C 0.033(3) 0.030(3) 0.024(3) -0.004(2) 0.001(2) 0.000(2) C43C 0.034(4) 0.024(3) 0.025(3) -0.004(3) 0.004(3) 0.001(3) C44C 0.041(4) 0.037(4) 0.032(3) -0.012(3) -0.006(3) -0.005(3) C45C 0.054(4) 0.034(4) 0.025(3) 0.000(3) -0.002(3) -0.005(3) C46C 0.041(4) 0.032(4) 0.034(4) -0.006(3) 0.004(3) -0.003(3) C47C 0.056(5) 0.038(4) 0.036(4) -0.011(3) -0.001(3) -0.012(3) C48C 0.050(4) 0.041(4) 0.027(3) -0.003(3) -0.008(3) -0.001(3) C49C 0.069(5) 0.023(3) 0.043(4) 0.002(3) 0.002(4) -0.005(3) C50C 0.108(8) 0.054(5) 0.101(7) 0.012(5) 0.051(6) -0.019(5) C51C 0.110(7) 0.037(4) 0.081(6) -0.003(4) -0.029(5) -0.016(5) C52C 0.102(7) 0.032(4) 0.054(5) -0.005(4) -0.008(5) 0.002(4) C5C 0.019(3) 0.030(3) 0.036(4) -0.008(3) -0.007(3) -0.002(3) O5C 0.036(2) 0.039(2) 0.020(2) -0.0068(18) 0.0002(18) 0.0000(19) O1L 0.104(6) 0.097(5) 0.110(6) 0.004(4) -0.011(5) -0.026(4) C1L 0.209(15) 0.104(9) 0.078(8) -0.011(7) 0.002(9) -0.010(9) O1M 0.187(8) 0.111(5) 0.077(4) 0.029(4) -0.081(5) -0.084(5) C1M 0.079(6) 0.098(7) 0.051(5) -0.017(5) -0.018(5) -0.004(5) O1N 0.256(13) 0.110(7) 0.121(8) -0.012(6) 0.058(8) 0.013(8) C1N 0.25(2) 0.177(15) 0.113(11) -0.043(10) -0.047(13) -0.065(15) _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 O5B 1.898(4) . ? Co1 O5A 1.909(4) . ? Co1 N42B 1.954(5) . ? Co1 O5C 1.959(4) . ? Co1 N42A 1.962(4) . ? Co1 N42C 1.980(5) . ? N1A C5A 1.354(7) . ? N1A C11A 1.404(7) . ? N1A N2A 1.415(6) . ? C11A C12A 1.381(8) . ? C11A C16A 1.400(8) . ? C12A C13A 1.355(8) . ? C13A C14A 1.384(9) . ? C14A C15A 1.370(9) . ? C15A C16A 1.379(8) . ? N2A C3A 1.301(7) . ? C3A C4A 1.433(7) . ? C3A C31A 1.497(8) . ? C4A N41A 1.335(7) . ? C4A C5A 1.412(7) . ? N41A N42A 1.269(6) . ? N42A C43A 1.445(7) . ? C43A C44A 1.371(8) . ? C43A C48A 1.375(8) . ? C44A C45A 1.372(8) . ? C45A C46A 1.406(8) . ? C46A C47A 1.371(8) . ? C46A C49A 1.523(8) . ? C47A C48A 1.377(8) . ? C49A C51A 1.509(10) . ? C49A C50A 1.520(10) . ? C49A C52A 1.536(10) . ? C5A O5A 1.283(6) . ? N1B C5B 1.365(7) . ? N1B C11B 1.406(7) . ? N1B N2B 1.407(6) . ? C11B C12B 1.374(8) . ? C11B C16B 1.383(9) . ? C12B C13B 1.381(10) . ? C13B C14B 1.375(11) . ? C14B C15B 1.342(10) . ? C15B C16B 1.353(9) . ? N2B C3B 1.304(7) . ? C3B C4B 1.417(8) . ? C3B C31B 1.500(8) . ? C4B N41B 1.342(7) . ? C4B C5B 1.395(8) . ? N41B N42B 1.301(6) . ? N42B C43B 1.454(7) . ? C43B C48B 1.377(8) . ? C43B C44B 1.394(7) . ? C44B C45B 1.353(8) . ? C45B C46B 1.387(8) . ? C46B C47B 1.407(8) . ? C46B C49B 1.510(9) . ? C47B C48B 1.360(8) . ? C49B C51B 1.501(11) . ? C49B C50B 1.502(11) . ? C49B C52B 1.525(11) . ? C5B O5B 1.276(6) . ? N1C C5C 1.356(7) . ? N1C N2C 1.419(6) . ? N1C C11C 1.435(7) . ? C11C C12C 1.343(9) . ? C11C C16C 1.399(9) . ? C12C C13C 1.369(10) . ? C13C C14C 1.371(11) . ? C14C C15C 1.371(11) . ? C15C C16C 1.396(9) . ? N2C C3C 1.330(7) . ? C3C C4C 1.407(8) . ? C3C C31C 1.483(8) . ? C4C N41C 1.345(7) . ? C4C C5C 1.405(8) . ? N41C N42C 1.286(6) . ? N42C C43C 1.419(7) . ? C43C C48C 1.366(8) . ? C43C C44C 1.392(8) . ? C44C C45C 1.391(8) . ? C45C C46C 1.376(8) . ? C46C C47C 1.380(8) . ? C46C C49C 1.528(8) . ? C47C C48C 1.395(8) . ? C49C C51C 1.511(10) . ? C49C C52C 1.518(10) . ? C49C C50C 1.540(10) . ? C5C O5C 1.287(6) . ? O1L C1L 1.399(12) . ? O1M C1M 1.335(9) . ? O1N C1N 1.429(15) . ? 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 O5B Co1 O5A 170.33(17) . . ? O5B Co1 N42B 95.23(18) . . ? O5A Co1 N42B 92.92(18) . . ? O5B Co1 O5C 83.12(16) . . ? O5A Co1 O5C 89.22(17) . . ? N42B Co1 O5C 174.54(18) . . ? O5B Co1 N42A 90.65(18) . . ? O5A Co1 N42A 94.26(18) . . ? N42B Co1 N42A 91.97(19) . . ? O5C Co1 N42A 82.86(18) . . ? O5B Co1 N42C 85.36(18) . . ? O5A Co1 N42C 89.07(18) . . ? N42B Co1 N42C 92.79(19) . . ? O5C Co1 N42C 92.27(18) . . ? N42A Co1 N42C 174.0(2) . . ? C5A N1A C11A 130.3(5) . . ? C5A N1A N2A 110.4(4) . . ? C11A N1A N2A 119.3(4) . . ? C12A C11A C16A 119.4(6) . . ? C12A C11A N1A 121.1(5) . . ? C16A C11A N1A 119.4(5) . . ? C13A C12A C11A 120.9(6) . . ? C12A C13A C14A 120.5(6) . . ? C15A C14A C13A 118.9(6) . . ? C14A C15A C16A 121.8(6) . . ? C15A C16A C11A 118.4(6) . . ? C3A N2A N1A 106.6(4) . . ? N2A C3A C4A 111.1(5) . . ? N2A C3A C31A 122.0(5) . . ? C4A C3A C31A 126.9(5) . . ? N41A C4A C5A 128.8(5) . . ? N41A C4A C3A 125.5(5) . . ? C5A C4A C3A 105.1(5) . . ? N42A N41A C4A 118.4(5) . . ? N41A N42A C43A 112.8(4) . . ? N41A N42A Co1 126.6(4) . . ? C43A N42A Co1 119.9(3) . . ? C44A C43A C48A 119.3(5) . . ? C44A C43A N42A 120.0(5) . . ? C48A C43A N42A 120.6(5) . . ? C43A C44A C45A 120.1(6) . . ? C44A C45A C46A 122.0(6) . . ? C47A C46A C45A 115.9(5) . . ? C47A C46A C49A 123.6(6) . . ? C45A C46A C49A 120.5(6) . . ? C46A C47A C48A 122.7(6) . . ? C43A C48A C47A 119.9(6) . . ? C51A C49A C50A 109.5(7) . . ? C51A C49A C46A 112.7(6) . . ? C50A C49A C46A 110.2(6) . . ? C51A C49A C52A 106.4(7) . . ? C50A C49A C52A 108.6(7) . . ? C46A C49A C52A 109.2(6) . . ? O5A C5A N1A 124.8(5) . . ? O5A C5A C4A 128.5(5) . . ? N1A C5A C4A 106.7(5) . . ? C5A O5A Co1 117.9(3) . . ? C5B N1B C11B 129.9(5) . . ? C5B N1B N2B 110.4(5) . . ? C11B N1B N2B 119.6(5) . . ? C12B C11B C16B 118.7(6) . . ? C12B C11B N1B 119.1(6) . . ? C16B C11B N1B 122.2(5) . . ? C11B C12B C13B 119.6(7) . . ? C14B C13B C12B 120.7(8) . . ? C15B C14B C13B 118.6(8) . . ? C14B C15B C16B 122.1(8) . . ? C15B C16B C11B 120.1(7) . . ? C3B N2B N1B 106.4(5) . . ? N2B C3B C4B 110.8(5) . . ? N2B C3B C31B 121.5(6) . . ? C4B C3B C31B 127.7(6) . . ? N41B C4B C5B 127.1(5) . . ? N41B C4B C3B 126.5(5) . . ? C5B C4B C3B 106.4(5) . . ? N42B N41B C4B 120.5(5) . . ? N41B N42B C43B 109.6(5) . . ? N41B N42B Co1 126.8(4) . . ? C43B N42B Co1 123.4(4) . . ? C48B C43B C44B 117.7(5) . . ? C48B C43B N42B 120.5(5) . . ? C44B C43B N42B 121.7(5) . . ? C45B C44B C43B 120.2(5) . . ? C44B C45B C46B 123.3(6) . . ? C45B C46B C47B 115.7(6) . . ? C45B C46B C49B 122.3(6) . . ? C47B C46B C49B 121.9(6) . . ? C48B C47B C46B 121.2(6) . . ? C47B C48B C43B 121.9(6) . . ? C51B C49B C50B 112.0(8) . . ? C51B C49B C46B 109.7(6) . . ? C50B C49B C46B 114.3(7) . . ? C51B C49B C52B 104.8(8) . . ? C50B C49B C52B 106.8(8) . . ? C46B C49B C52B 108.8(7) . . ? O5B C5B N1B 123.8(5) . . ? O5B C5B C4B 130.2(5) . . ? N1B C5B C4B 106.0(5) . . ? C5B O5B Co1 120.0(4) . . ? C5C N1C N2C 111.4(4) . . ? C5C N1C C11C 131.8(5) . . ? N2C N1C C11C 116.6(5) . . ? C12C C11C C16C 120.5(6) . . ? C12C C11C N1C 120.4(6) . . ? C16C C11C N1C 119.1(6) . . ? C11C C12C C13C 122.0(8) . . ? C12C C13C C14C 119.7(8) . . ? C15C C14C C13C 118.6(7) . . ? C14C C15C C16C 122.7(7) . . ? C15C C16C C11C 116.5(7) . . ? C3C N2C N1C 105.1(5) . . ? N2C C3C C4C 110.8(5) . . ? N2C C3C C31C 121.0(6) . . ? C4C C3C C31C 128.2(6) . . ? N41C C4C C5C 127.1(5) . . ? N41C C4C C3C 125.6(5) . . ? C5C C4C C3C 107.0(5) . . ? N42C N41C C4C 120.3(5) . . ? N41C N42C C43C 111.5(4) . . ? N41C N42C Co1 124.2(4) . . ? C43C N42C Co1 124.3(4) . . ? C48C C43C C44C 118.8(5) . . ? C48C C43C N42C 120.9(5) . . ? C44C C43C N42C 120.2(5) . . ? C45C C44C C43C 118.8(6) . . ? C46C C45C C44C 123.2(6) . . ? C45C C46C C47C 116.9(5) . . ? C45C C46C C49C 121.2(6) . . ? C47C C46C C49C 121.9(6) . . ? C46C C47C C48C 121.0(6) . . ? C43C C48C C47C 121.3(6) . . ? C51C C49C C52C 107.5(6) . . ? C51C C49C C46C 113.0(6) . . ? C52C C49C C46C 110.1(6) . . ? C51C C49C C50C 110.2(7) . . ? C52C C49C C50C 108.1(6) . . ? C46C C49C C50C 107.7(6) . . ? O5C C5C N1C 125.6(5) . . ? O5C C5C C4C 128.7(5) . . ? N1C C5C C4C 105.6(5) . . ? C5C O5C Co1 114.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.691 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.085