# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_09mz139_0m _database_code_depnum_ccdc_archive 'CCDC 881837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H80 B2 Co2 N12 O4' _chemical_formula_weight 1052.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.4672(19) _cell_length_b 18.5277(15) _cell_length_c 12.2574(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.2980(10) _cell_angle_gamma 90.00 _cell_volume 5556.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6163 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 30.30 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 31764 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 30.49 _reflns_number_total 8369 _reflns_number_gt 5908 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0336P)^2^+6.3742P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8369 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.23457(9) 0.17101(13) 0.22765(19) 0.0316(5) Uani 1 1 d . . . H1 H 0.2747 0.1658 0.2148 0.038 Uiso 1 1 calc R . . C1 C 0.0000 0.14797(13) 0.2500 0.0248(5) Uani 1 2 d S . . C2 C 0.0000 0.23097(12) 0.2500 0.0196(5) Uani 1 2 d S . . C3 C 0.24111(9) 0.05130(11) 0.33767(18) 0.0393(5) Uani 1 1 d . . . H3 H 0.2785 0.0404 0.3258 0.047 Uiso 1 1 calc R . . C4 C 0.20630(9) 0.01300(11) 0.40240(19) 0.0403(6) Uani 1 1 d . . . H4 H 0.2145 -0.0291 0.4435 0.048 Uiso 1 1 calc R . . C5 C 0.15586(8) 0.04875(10) 0.39553(16) 0.0308(4) Uani 1 1 d . . . C6 C 0.10405(8) 0.03217(10) 0.45361(17) 0.0337(5) Uani 1 1 d . . . H6A H 0.1021 -0.0206 0.4658 0.040 Uiso 1 1 calc R . . H6B H 0.0729 0.0457 0.4059 0.040 Uiso 1 1 calc R . . C7 C 0.09754(9) 0.07084(11) 0.56448(16) 0.0363(5) Uani 1 1 d . . . C8 C 0.14094(11) 0.04552(15) 0.6458(2) 0.0599(8) Uani 1 1 d . . . H8A H 0.1773 0.0584 0.6187 0.090 Uiso 1 1 calc R . . H8B H 0.1385 -0.0070 0.6543 0.090 Uiso 1 1 calc R . . H8C H 0.1349 0.0688 0.7164 0.090 Uiso 1 1 calc R . . C9 C 0.04110(11) 0.05308(15) 0.6097(2) 0.0558(7) Uani 1 1 d . . . H9A H 0.0358 0.0786 0.6788 0.084 Uiso 1 1 calc R . . H9B H 0.0383 0.0010 0.6219 0.084 Uiso 1 1 calc R . . H9C H 0.0130 0.0683 0.5573 0.084 Uiso 1 1 calc R . . C10 C 0.10209(10) 0.15231(11) 0.54825(17) 0.0375(5) Uani 1 1 d . . . H10A H 0.0969 0.1768 0.6183 0.056 Uiso 1 1 calc R . . H10B H 0.0739 0.1684 0.4965 0.056 Uiso 1 1 calc R . . H10C H 0.1383 0.1641 0.5195 0.056 Uiso 1 1 calc R . . C11 C 0.22333(9) 0.16917(12) 0.01691(18) 0.0372(5) Uani 1 1 d . . . H11 H 0.2606 0.1620 -0.0018 0.045 Uiso 1 1 calc R . . C12 C 0.18057(9) 0.17535(12) -0.05569(17) 0.0379(5) Uani 1 1 d . . . H12 H 0.1822 0.1730 -0.1330 0.045 Uiso 1 1 calc R . . C13 C 0.13428(8) 0.18581(10) 0.00834(16) 0.0306(4) Uani 1 1 d . . . C14 C 0.07676(8) 0.20107(11) -0.02677(16) 0.0328(4) Uani 1 1 d . . . H14A H 0.0522 0.1917 0.0355 0.039 Uiso 1 1 calc R . . H14B H 0.0667 0.1670 -0.0858 0.039 Uiso 1 1 calc R . . C15 C 0.06687(8) 0.27901(12) -0.06779(15) 0.0314(4) Uani 1 1 d . . . C16 C 0.09731(9) 0.29322(14) -0.17367(17) 0.0437(6) Uani 1 1 d . . . H16A H 0.0879 0.3414 -0.2009 0.066 Uiso 1 1 calc R . . H16B H 0.0868 0.2569 -0.2280 0.066 Uiso 1 1 calc R . . H16C H 0.1368 0.2905 -0.1602 0.066 Uiso 1 1 calc R . . C17 C 0.00555(8) 0.28757(13) -0.08828(18) 0.0401(5) Uani 1 1 d . . . H17A H -0.0142 0.2812 -0.0195 0.060 Uiso 1 1 calc R . . H17B H -0.0067 0.2511 -0.1409 0.060 Uiso 1 1 calc R . . H17C H -0.0018 0.3358 -0.1175 0.060 Uiso 1 1 calc R . . C18 C 0.08507(9) 0.33295(11) 0.01848(16) 0.0339(5) Uani 1 1 d . . . H18A H 0.0771 0.3820 -0.0067 0.051 Uiso 1 1 calc R . . H18B H 0.1245 0.3279 0.0313 0.051 Uiso 1 1 calc R . . H18C H 0.0654 0.3237 0.0865 0.051 Uiso 1 1 calc R . . C19 C 0.25916(8) 0.28229(12) 0.34758(16) 0.0331(5) Uani 1 1 d . . . H19 H 0.2978 0.2782 0.3443 0.040 Uiso 1 1 calc R . . C20 C 0.23091(8) 0.33222(11) 0.40757(16) 0.0310(4) Uani 1 1 d . . . H20 H 0.2457 0.3690 0.4530 0.037 Uiso 1 1 calc R . . C21 C 0.17573(7) 0.31758(9) 0.38768(15) 0.0243(4) Uani 1 1 d . . . C22 C 0.12625(7) 0.35570(9) 0.42964(15) 0.0248(4) Uani 1 1 d . . . H22A H 0.1294 0.3592 0.5100 0.030 Uiso 1 1 calc R . . H22B H 0.0938 0.3256 0.4132 0.030 Uiso 1 1 calc R . . C23 C 0.11593(7) 0.43228(10) 0.38378(15) 0.0259(4) Uani 1 1 d . . . C24 C 0.11582(10) 0.43073(12) 0.25962(17) 0.0410(5) Uani 1 1 d . . . H24A H 0.0872 0.3978 0.2337 0.062 Uiso 1 1 calc R . . H24B H 0.1515 0.4140 0.2337 0.062 Uiso 1 1 calc R . . H24C H 0.1087 0.4794 0.2315 0.062 Uiso 1 1 calc R . . C25 C 0.05949(8) 0.45624(11) 0.4231(2) 0.0400(5) Uani 1 1 d . . . H25A H 0.0514 0.5046 0.3947 0.060 Uiso 1 1 calc R . . H25B H 0.0591 0.4573 0.5030 0.060 Uiso 1 1 calc R . . H25C H 0.0318 0.4222 0.3966 0.060 Uiso 1 1 calc R . . C26 C 0.15889(8) 0.48607(11) 0.42427(17) 0.0330(4) Uani 1 1 d . . . H26A H 0.1951 0.4710 0.3991 0.050 Uiso 1 1 calc R . . H26B H 0.1586 0.4875 0.5042 0.050 Uiso 1 1 calc R . . H26C H 0.1505 0.5342 0.3954 0.050 Uiso 1 1 calc R . . Co1 Co 0.110896(10) 0.188845(13) 0.26534(2) 0.02314(7) Uani 1 1 d . . . N1 N 0.16072(6) 0.10574(8) 0.32870(13) 0.0267(3) Uani 1 1 d . . . N2 N 0.21358(6) 0.10698(9) 0.29355(13) 0.0308(4) Uani 1 1 d . . . N3 N 0.14848(6) 0.18480(8) 0.11460(13) 0.0281(3) Uani 1 1 d . . . N4 N 0.20390(6) 0.17492(9) 0.11813(13) 0.0303(4) Uani 1 1 d . . . N5 N 0.17108(6) 0.26099(8) 0.31967(12) 0.0233(3) Uani 1 1 d . . . N6 N 0.22324(6) 0.24011(9) 0.29421(13) 0.0276(3) Uani 1 1 d . . . O1 O 0.04589(5) 0.11804(7) 0.25138(12) 0.0319(3) Uani 1 1 d . . . O2 O 0.04558(5) 0.26097(6) 0.26162(10) 0.0229(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 B1 0.0195(10) 0.0384(12) 0.0366(12) -0.0167(10) -0.0065(9) 0.0111(9) C1 0.0280(13) 0.0147(11) 0.0317(14) 0.000 -0.0153(11) 0.000 C2 0.0200(11) 0.0155(11) 0.0231(12) 0.000 -0.0037(9) 0.000 C3 0.0349(11) 0.0340(11) 0.0486(13) -0.0218(10) -0.0227(10) 0.0200(9) C4 0.0462(13) 0.0222(10) 0.0523(13) -0.0131(9) -0.0284(11) 0.0144(9) C5 0.0365(11) 0.0170(8) 0.0388(11) -0.0099(8) -0.0229(9) 0.0068(7) C6 0.0401(11) 0.0159(8) 0.0447(12) 0.0026(8) -0.0242(9) -0.0026(8) C7 0.0476(12) 0.0332(11) 0.0280(10) 0.0118(8) -0.0146(9) -0.0158(9) C8 0.0722(18) 0.0652(17) 0.0419(13) 0.0287(12) -0.0339(13) -0.0304(14) C9 0.0630(17) 0.0641(17) 0.0400(13) 0.0183(12) -0.0093(12) -0.0322(14) C10 0.0551(14) 0.0297(11) 0.0278(10) -0.0063(8) 0.0042(9) -0.0076(10) C11 0.0321(11) 0.0401(12) 0.0393(11) -0.0214(9) -0.0037(9) 0.0133(9) C12 0.0411(12) 0.0408(12) 0.0316(11) -0.0185(9) -0.0069(9) 0.0118(9) C13 0.0317(10) 0.0266(9) 0.0335(10) -0.0143(8) -0.0098(8) 0.0061(8) C14 0.0310(10) 0.0352(11) 0.0320(10) -0.0140(8) -0.0126(8) 0.0033(8) C15 0.0286(10) 0.0404(11) 0.0250(9) -0.0050(8) -0.0094(8) 0.0047(8) C16 0.0344(11) 0.0686(16) 0.0282(10) -0.0063(10) -0.0065(9) 0.0106(11) C17 0.0304(11) 0.0549(14) 0.0349(11) -0.0009(10) -0.0065(9) 0.0062(10) C18 0.0456(12) 0.0281(10) 0.0280(10) 0.0003(8) -0.0093(9) 0.0022(9) C19 0.0186(9) 0.0438(12) 0.0367(11) -0.0165(9) -0.0061(8) 0.0014(8) C20 0.0238(9) 0.0347(10) 0.0345(10) -0.0162(8) -0.0049(8) -0.0013(8) C21 0.0237(9) 0.0219(8) 0.0273(9) -0.0069(7) -0.0023(7) 0.0003(7) C22 0.0233(9) 0.0226(9) 0.0285(9) -0.0058(7) 0.0021(7) -0.0008(7) C23 0.0255(9) 0.0209(8) 0.0312(10) -0.0068(7) -0.0028(7) 0.0000(7) C24 0.0584(15) 0.0330(11) 0.0316(11) -0.0019(9) -0.0106(10) -0.0021(10) C25 0.0282(10) 0.0278(10) 0.0640(15) -0.0088(10) 0.0001(10) 0.0039(8) C26 0.0324(10) 0.0253(10) 0.0413(11) -0.0067(8) -0.0072(9) -0.0027(8) Co1 0.01978(12) 0.01915(12) 0.03039(13) -0.00633(10) -0.00848(9) 0.00462(9) N1 0.0238(8) 0.0235(8) 0.0327(8) -0.0106(6) -0.0129(6) 0.0083(6) N2 0.0251(8) 0.0312(9) 0.0360(9) -0.0163(7) -0.0128(7) 0.0138(7) N3 0.0227(7) 0.0277(8) 0.0337(8) -0.0116(7) -0.0089(6) 0.0067(6) N4 0.0242(8) 0.0327(9) 0.0340(9) -0.0149(7) -0.0064(7) 0.0089(6) N5 0.0174(7) 0.0237(7) 0.0289(8) -0.0074(6) -0.0031(6) 0.0039(6) N6 0.0168(7) 0.0329(9) 0.0332(9) -0.0133(7) -0.0049(6) 0.0054(6) O1 0.0283(7) 0.0165(6) 0.0506(9) -0.0037(6) -0.0188(6) 0.0040(5) O2 0.0185(6) 0.0165(6) 0.0336(7) -0.0015(5) -0.0041(5) 0.0001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N2 1.526(3) . ? B1 N4 1.536(3) . ? B1 N6 1.544(3) . ? B1 H1 1.0000 . ? C1 O1 1.2522(16) 2 ? C1 O1 1.2522(16) . ? C1 C2 1.538(3) . ? C2 O2 1.2534(15) . ? C2 O2 1.2535(15) 2 ? C3 N2 1.344(2) . ? C3 C4 1.366(3) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C4 H4 0.9500 . ? C5 N1 1.342(3) . ? C5 C6 1.489(3) . ? C6 C7 1.545(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.526(3) . ? C7 C9 1.526(3) . ? C7 C10 1.527(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N4 1.335(3) . ? C11 C12 1.375(3) . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C12 H12 0.9500 . ? C13 N3 1.346(2) . ? C13 C14 1.497(3) . ? C14 C15 1.548(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.520(3) . ? C15 C16 1.523(3) . ? C15 C17 1.528(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N6 1.343(2) . ? C19 C20 1.371(3) . ? C19 H19 0.9500 . ? C20 C21 1.397(2) . ? C20 H20 0.9500 . ? C21 N5 1.344(2) . ? C21 C22 1.495(2) . ? C22 C23 1.546(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.522(3) . ? C23 C26 1.529(2) . ? C23 C25 1.531(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Co1 O1 2.0682(13) . ? Co1 N3 2.0694(17) . ? Co1 O2 2.0836(12) . ? Co1 N5 2.0948(15) . ? Co1 N1 2.1096(15) . ? N1 N2 1.365(2) . ? N3 N4 1.369(2) . ? N5 N6 1.371(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 N2 B1 N4 109.57(16) . . ? N2 B1 N6 107.64(17) . . ? N4 B1 N6 109.53(16) . . ? N2 B1 H1 110.0 . . ? N4 B1 H1 110.0 . . ? N6 B1 H1 110.0 . . ? O1 C1 O1 127.4(2) 2 . ? O1 C1 C2 116.29(11) 2 . ? O1 C1 C2 116.29(11) . . ? O2 C2 O2 127.3(2) . 2 ? O2 C2 C1 116.33(11) . . ? O2 C2 C1 116.33(11) 2 . ? N2 C3 C4 108.65(19) . . ? N2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? C3 C4 C5 105.72(19) . . ? C3 C4 H4 127.1 . . ? C5 C4 H4 127.1 . . ? N1 C5 C4 109.1(2) . . ? N1 C5 C6 122.18(16) . . ? C4 C5 C6 128.66(19) . . ? C5 C6 C7 114.63(15) . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C9 108.94(18) . . ? C8 C7 C10 109.76(18) . . ? C9 C7 C10 109.1(2) . . ? C8 C7 C6 110.9(2) . . ? C9 C7 C6 108.47(17) . . ? C10 C7 C6 109.63(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 108.74(18) . . ? N4 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? C11 C12 C13 105.35(18) . . ? C11 C12 H12 127.3 . . ? C13 C12 H12 127.3 . . ? N3 C13 C12 109.65(17) . . ? N3 C13 C14 121.22(18) . . ? C12 C13 C14 129.02(18) . . ? C13 C14 C15 114.51(17) . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C18 C15 C16 109.66(18) . . ? C18 C15 C17 109.26(17) . . ? C16 C15 C17 109.04(16) . . ? C18 C15 C14 110.04(15) . . ? C16 C15 C14 111.22(18) . . ? C17 C15 C14 107.57(18) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 108.86(16) . . ? N6 C19 H19 125.6 . . ? C20 C19 H19 125.6 . . ? C19 C20 C21 105.35(16) . . ? C19 C20 H20 127.3 . . ? C21 C20 H20 127.3 . . ? N5 C21 C20 109.77(16) . . ? N5 C21 C22 121.06(15) . . ? C20 C21 C22 129.17(16) . . ? C21 C22 C23 116.07(15) . . ? C21 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? C21 C22 H22B 108.3 . . ? C23 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C26 109.54(17) . . ? C24 C23 C25 108.86(17) . . ? C26 C23 C25 109.18(16) . . ? C24 C23 C22 110.21(15) . . ? C26 C23 C22 111.67(15) . . ? C25 C23 C22 107.32(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 Co1 N3 104.38(6) . . ? O1 Co1 O2 79.37(5) . . ? N3 Co1 O2 110.36(6) . . ? O1 Co1 N5 165.95(6) . . ? N3 Co1 N5 89.55(6) . . ? O2 Co1 N5 97.79(5) . . ? O1 Co1 N1 90.58(6) . . ? N3 Co1 N1 92.50(6) . . ? O2 Co1 N1 156.62(6) . . ? N5 Co1 N1 86.83(6) . . ? C5 N1 N2 107.04(15) . . ? C5 N1 Co1 138.25(14) . . ? N2 N1 Co1 114.70(12) . . ? C3 N2 N1 109.48(18) . . ? C3 N2 B1 129.82(18) . . ? N1 N2 B1 120.15(15) . . ? C13 N3 N4 106.43(15) . . ? C13 N3 Co1 138.56(13) . . ? N4 N3 Co1 114.92(12) . . ? C11 N4 N3 109.81(16) . . ? C11 N4 B1 129.30(17) . . ? N3 N4 B1 120.88(16) . . ? C21 N5 N6 106.58(14) . . ? C21 N5 Co1 138.77(12) . . ? N6 N5 Co1 113.66(11) . . ? C19 N6 N5 109.42(15) . . ? C19 N6 B1 128.37(16) . . ? N5 N6 B1 121.61(15) . . ? C1 O1 Co1 114.16(12) . . ? C2 O2 Co1 113.57(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O2 173.58(10) 2 . . . ? O1 C1 C2 O2 -6.42(10) . . . . ? O1 C1 C2 O2 -6.41(10) 2 . . 2 ? O1 C1 C2 O2 173.59(10) . . . 2 ? N2 C3 C4 C5 -0.2(2) . . . . ? C3 C4 C5 N1 0.4(2) . . . . ? C3 C4 C5 C6 -177.01(18) . . . . ? N1 C5 C6 C7 -87.0(2) . . . . ? C4 C5 C6 C7 90.0(2) . . . . ? C5 C6 C7 C8 -64.6(2) . . . . ? C5 C6 C7 C9 175.81(17) . . . . ? C5 C6 C7 C10 56.8(2) . . . . ? N4 C11 C12 C13 0.5(2) . . . . ? C11 C12 C13 N3 -0.9(2) . . . . ? C11 C12 C13 C14 175.2(2) . . . . ? N3 C13 C14 C15 101.2(2) . . . . ? C12 C13 C14 C15 -74.5(3) . . . . ? C13 C14 C15 C18 -55.1(2) . . . . ? C13 C14 C15 C16 66.7(2) . . . . ? C13 C14 C15 C17 -173.99(17) . . . . ? N6 C19 C20 C21 0.2(2) . . . . ? C19 C20 C21 N5 0.6(2) . . . . ? C19 C20 C21 C22 -178.7(2) . . . . ? N5 C21 C22 C23 -109.0(2) . . . . ? C20 C21 C22 C23 70.2(3) . . . . ? C21 C22 C23 C24 53.0(2) . . . . ? C21 C22 C23 C26 -69.0(2) . . . . ? C21 C22 C23 C25 171.38(16) . . . . ? C4 C5 N1 N2 -0.37(19) . . . . ? C6 C5 N1 N2 177.20(15) . . . . ? C4 C5 N1 Co1 178.76(14) . . . . ? C6 C5 N1 Co1 -3.7(3) . . . . ? O1 Co1 N1 C5 -37.71(18) . . . . ? N3 Co1 N1 C5 -142.13(18) . . . . ? O2 Co1 N1 C5 26.1(3) . . . . ? N5 Co1 N1 C5 128.47(18) . . . . ? O1 Co1 N1 N2 141.37(12) . . . . ? N3 Co1 N1 N2 36.95(12) . . . . ? O2 Co1 N1 N2 -154.83(12) . . . . ? N5 Co1 N1 N2 -52.46(12) . . . . ? C4 C3 N2 N1 0.0(2) . . . . ? C4 C3 N2 B1 171.31(18) . . . . ? C5 N1 N2 C3 0.24(19) . . . . ? Co1 N1 N2 C3 -179.12(11) . . . . ? C5 N1 N2 B1 -172.07(15) . . . . ? Co1 N1 N2 B1 8.58(19) . . . . ? N4 B1 N2 C3 124.97(19) . . . . ? N6 B1 N2 C3 -116.0(2) . . . . ? N4 B1 N2 N1 -64.5(2) . . . . ? N6 B1 N2 N1 54.6(2) . . . . ? C12 C13 N3 N4 1.0(2) . . . . ? C14 C13 N3 N4 -175.51(17) . . . . ? C12 C13 N3 Co1 -175.26(15) . . . . ? C14 C13 N3 Co1 8.2(3) . . . . ? O1 Co1 N3 C13 45.2(2) . . . . ? O2 Co1 N3 C13 -38.6(2) . . . . ? N5 Co1 N3 C13 -136.8(2) . . . . ? N1 Co1 N3 C13 136.4(2) . . . . ? O1 Co1 N3 N4 -130.84(12) . . . . ? O2 Co1 N3 N4 145.36(12) . . . . ? N5 Co1 N3 N4 47.21(13) . . . . ? N1 Co1 N3 N4 -39.60(13) . . . . ? C12 C11 N4 N3 0.1(2) . . . . ? C12 C11 N4 B1 179.3(2) . . . . ? C13 N3 N4 C11 -0.7(2) . . . . ? Co1 N3 N4 C11 176.59(13) . . . . ? C13 N3 N4 B1 180.00(17) . . . . ? Co1 N3 N4 B1 -2.7(2) . . . . ? N2 B1 N4 C11 -117.8(2) . . . . ? N6 B1 N4 C11 124.3(2) . . . . ? N2 B1 N4 N3 61.4(2) . . . . ? N6 B1 N4 N3 -56.5(2) . . . . ? C20 C21 N5 N6 -1.1(2) . . . . ? C22 C21 N5 N6 178.18(16) . . . . ? C20 C21 N5 Co1 166.05(15) . . . . ? C22 C21 N5 Co1 -14.7(3) . . . . ? O1 Co1 N5 C21 -41.0(3) . . . . ? N3 Co1 N5 C21 146.8(2) . . . . ? O2 Co1 N5 C21 36.3(2) . . . . ? N1 Co1 N5 C21 -120.7(2) . . . . ? O1 Co1 N5 N6 125.6(2) . . . . ? N3 Co1 N5 N6 -46.65(13) . . . . ? O2 Co1 N5 N6 -157.15(12) . . . . ? N1 Co1 N5 N6 45.88(13) . . . . ? C20 C19 N6 N5 -0.9(2) . . . . ? C20 C19 N6 B1 -172.0(2) . . . . ? C21 N5 N6 C19 1.3(2) . . . . ? Co1 N5 N6 C19 -169.53(13) . . . . ? C21 N5 N6 B1 173.04(18) . . . . ? Co1 N5 N6 B1 2.2(2) . . . . ? N2 B1 N6 C19 107.7(2) . . . . ? N4 B1 N6 C19 -133.2(2) . . . . ? N2 B1 N6 N5 -62.4(2) . . . . ? N4 B1 N6 N5 56.7(2) . . . . ? O1 C1 O1 Co1 -175.53(11) 2 . . . ? C2 C1 O1 Co1 4.47(11) . . . . ? N3 Co1 O1 C1 -110.18(10) . . . . ? O2 Co1 O1 C1 -1.67(9) . . . . ? N5 Co1 O1 C1 77.9(2) . . . . ? N1 Co1 O1 C1 157.09(10) . . . . ? O2 C2 O2 Co1 -175.28(9) 2 . . . ? C1 C2 O2 Co1 4.72(9) . . . . ? O1 Co1 O2 C2 -1.97(8) . . . . ? N3 Co1 O2 C2 99.55(9) . . . . ? N5 Co1 O2 C2 -168.03(9) . . . . ? N1 Co1 O2 C2 -67.89(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.393 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.059 data_09mz089_0m _database_code_depnum_ccdc_archive 'CCDC 881838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H80 B2 Co N12 Ni, C7 H8' _chemical_formula_sum 'C60 H88 B2 Co N12 Ni O4' _chemical_formula_weight 1180.67 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.603(5) _cell_length_b 11.1176(13) _cell_length_c 22.138(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.264(2) _cell_angle_gamma 90.00 _cell_volume 12199(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2287 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.36 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5032 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The solvate toluene molecules are disordered over two orientations with equal occupancies. The C-C bonds of the aromatic rings were constrained to be 1.39 Angstrom and the ring to resemble an ideal hexagon. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 36912 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_av_sigmaI/netI 0.1586 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 66 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14928 _reflns_number_gt 7916 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0000P)^2^+48.1722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14928 _refine_ls_number_parameters 771 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1708 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.40536(11) 0.7373(4) 0.4738(2) 0.0243(12) Uani 1 1 d . . . H1A H 0.4118 0.8153 0.4916 0.029 Uiso 1 1 calc R . . B2 B 0.33155(12) -0.0659(5) 0.1914(3) 0.0359(15) Uani 1 1 d . . . H2A H 0.3254 -0.1380 0.1675 0.043 Uiso 1 1 calc R . . C1 C 0.44976(9) 0.6403(4) 0.5193(2) 0.0289(11) Uani 1 1 d . . . H1 H 0.4579 0.7102 0.5367 0.035 Uiso 1 1 calc R . . C2 C 0.46054(9) 0.5276(4) 0.5212(2) 0.0300(12) Uani 1 1 d . . . H2 H 0.4772 0.5039 0.5400 0.036 Uiso 1 1 calc R . . C3 C 0.44198(8) 0.4537(4) 0.4896(2) 0.0223(10) Uani 1 1 d . . . C4 C 0.44418(9) 0.3232(4) 0.4745(2) 0.0261(11) Uani 1 1 d . . . H4 H 0.4410 0.3157 0.4298 0.031 Uiso 1 1 calc R . . C5 C 0.47206(10) 0.2713(4) 0.4896(2) 0.0359(13) Uani 1 1 d . . . H5A H 0.4858 0.3194 0.4692 0.043 Uiso 1 1 calc R . . H5B H 0.4759 0.2764 0.5337 0.043 Uiso 1 1 calc R . . C6 C 0.47383(10) 0.1410(4) 0.4695(2) 0.0396(13) Uani 1 1 d . . . H6A H 0.4723 0.1371 0.4248 0.048 Uiso 1 1 calc R . . H6B H 0.4917 0.1079 0.4825 0.048 Uiso 1 1 calc R . . C7 C 0.45185(10) 0.0652(4) 0.4957(2) 0.0387(13) Uani 1 1 d . . . H7A H 0.4526 -0.0170 0.4787 0.046 Uiso 1 1 calc R . . H7B H 0.4550 0.0590 0.5401 0.046 Uiso 1 1 calc R . . C8 C 0.42421(10) 0.1174(4) 0.4824(2) 0.0336(12) Uani 1 1 d . . . H8A H 0.4106 0.0688 0.5029 0.040 Uiso 1 1 calc R . . H8B H 0.4200 0.1140 0.4384 0.040 Uiso 1 1 calc R . . C9 C 0.42264(10) 0.2479(4) 0.5039(2) 0.0313(12) Uani 1 1 d . . . H9A H 0.4046 0.2812 0.4932 0.038 Uiso 1 1 calc R . . H9B H 0.4253 0.2510 0.5484 0.038 Uiso 1 1 calc R . . C10 C 0.40399(9) 0.8430(4) 0.3685(2) 0.0303(11) Uani 1 1 d . . . H10 H 0.4075 0.9231 0.3815 0.036 Uiso 1 1 calc R . . C11 C 0.40074(9) 0.8064(4) 0.3093(2) 0.0284(11) Uani 1 1 d . . . H11 H 0.4013 0.8552 0.2742 0.034 Uiso 1 1 calc R . . C12 C 0.39653(9) 0.6825(4) 0.3119(2) 0.0238(10) Uani 1 1 d . . . C13 C 0.39453(9) 0.5937(4) 0.2605(2) 0.0260(11) Uani 1 1 d . . . H13 H 0.3996 0.5129 0.2772 0.031 Uiso 1 1 calc R . . C14 C 0.41489(9) 0.6260(4) 0.2129(2) 0.0296(11) Uani 1 1 d . . . H14A H 0.4109 0.7078 0.1973 0.036 Uiso 1 1 calc R . . H14B H 0.4333 0.6269 0.2321 0.036 Uiso 1 1 calc R . . C15 C 0.41415(10) 0.5377(4) 0.1604(2) 0.0324(12) Uani 1 1 d . . . H15A H 0.4266 0.5656 0.1294 0.039 Uiso 1 1 calc R . . H15B H 0.4205 0.4580 0.1750 0.039 Uiso 1 1 calc R . . C16 C 0.38614(10) 0.5252(5) 0.1321(2) 0.0355(13) Uani 1 1 d . . . H16A H 0.3862 0.4626 0.1003 0.043 Uiso 1 1 calc R . . H16B H 0.3806 0.6022 0.1129 0.043 Uiso 1 1 calc R . . C17 C 0.36618(10) 0.4913(5) 0.1791(2) 0.0356(12) Uani 1 1 d . . . H17A H 0.3707 0.4107 0.1956 0.043 Uiso 1 1 calc R . . H17B H 0.3478 0.4872 0.1599 0.043 Uiso 1 1 calc R . . C18 C 0.36650(9) 0.5830(4) 0.2308(2) 0.0314(12) Uani 1 1 d . . . H18A H 0.3607 0.6625 0.2148 0.038 Uiso 1 1 calc R . . H18B H 0.3536 0.5578 0.2613 0.038 Uiso 1 1 calc R . . C19 C 0.36427(9) 0.7534(4) 0.54341(19) 0.0220(10) Uani 1 1 d . . . H19 H 0.3694 0.8235 0.5655 0.026 Uiso 1 1 calc R . . C20 C 0.34111(9) 0.6890(4) 0.55038(19) 0.0230(10) Uani 1 1 d . . . H20 H 0.3272 0.7055 0.5775 0.028 Uiso 1 1 calc R . . C21 C 0.34221(9) 0.5938(4) 0.50933(19) 0.0205(10) Uani 1 1 d . . . C22 C 0.32083(9) 0.5013(4) 0.49535(19) 0.0254(10) Uani 1 1 d . . . H22 H 0.3295 0.4308 0.4760 0.030 Uiso 1 1 calc R . . C23 C 0.29956(9) 0.5534(4) 0.4500(3) 0.0403(14) Uani 1 1 d . . . H23A H 0.2920 0.6281 0.4667 0.048 Uiso 1 1 calc R . . H23B H 0.3083 0.5740 0.4119 0.048 Uiso 1 1 calc R . . C24 C 0.27700(11) 0.4640(5) 0.4370(3) 0.0540(17) Uani 1 1 d . . . H24A H 0.2633 0.5010 0.4091 0.065 Uiso 1 1 calc R . . H24B H 0.2844 0.3924 0.4168 0.065 Uiso 1 1 calc R . . C25 C 0.26395(11) 0.4259(6) 0.4933(3) 0.064(2) Uani 1 1 d . . . H25A H 0.2498 0.3657 0.4832 0.077 Uiso 1 1 calc R . . H25B H 0.2552 0.4964 0.5117 0.077 Uiso 1 1 calc R . . C26 C 0.28405(13) 0.3728(6) 0.5382(3) 0.060(2) Uani 1 1 d . . . H26A H 0.2910 0.2963 0.5220 0.072 Uiso 1 1 calc R . . H26B H 0.2750 0.3546 0.5761 0.072 Uiso 1 1 calc R . . C27 C 0.30770(12) 0.4579(5) 0.5519(2) 0.0547(18) Uani 1 1 d . . . H27A H 0.3012 0.5283 0.5746 0.066 Uiso 1 1 calc R . . H27B H 0.3214 0.4159 0.5780 0.066 Uiso 1 1 calc R . . C28 C 0.35445(8) 0.3544(4) 0.3429(2) 0.0206(10) Uani 1 1 d . . . C29 C 0.38270(9) 0.2990(4) 0.3447(2) 0.0221(10) Uani 1 1 d . . . C30 C 0.37721(10) -0.0832(4) 0.1373(2) 0.0338(12) Uani 1 1 d . . . H30 H 0.3736 -0.1546 0.1149 0.041 Uiso 1 1 calc R . . C31 C 0.40039(10) -0.0171(4) 0.1357(2) 0.0315(12) Uani 1 1 d . . . H31 H 0.4157 -0.0324 0.1123 0.038 Uiso 1 1 calc R . . C32 C 0.39677(10) 0.0779(4) 0.1760(2) 0.0283(11) Uani 1 1 d . . . C33 C 0.41506(10) 0.1822(4) 0.1907(2) 0.0360(13) Uani 1 1 d . . . H33A H 0.4060 0.2339 0.2201 0.043 Uiso 1 1 calc R . . H33B H 0.4168 0.2299 0.1533 0.043 Uiso 1 1 calc R . . C34 C 0.44382(10) 0.1554(5) 0.2166(3) 0.0413(14) Uani 1 1 d . . . C35 C 0.45512(14) 0.2702(6) 0.2434(4) 0.126(4) Uani 1 1 d . . . H35A H 0.4734 0.2557 0.2600 0.188 Uiso 1 1 calc R . . H35B H 0.4437 0.2975 0.2757 0.188 Uiso 1 1 calc R . . H35C H 0.4556 0.3320 0.2119 0.188 Uiso 1 1 calc R . . C36 C 0.44323(12) 0.0632(6) 0.2655(3) 0.067(2) Uani 1 1 d . . . H36A H 0.4384 -0.0152 0.2479 0.101 Uiso 1 1 calc R . . H36B H 0.4298 0.0862 0.2947 0.101 Uiso 1 1 calc R . . H36C H 0.4611 0.0581 0.2860 0.101 Uiso 1 1 calc R . . C37 C 0.46185(12) 0.1148(8) 0.1678(3) 0.095(3) Uani 1 1 d . . . H37A H 0.4800 0.1003 0.1852 0.142 Uiso 1 1 calc R . . H37B H 0.4626 0.1772 0.1367 0.142 Uiso 1 1 calc R . . H37C H 0.4547 0.0403 0.1497 0.142 Uiso 1 1 calc R . . C38 C 0.29214(10) 0.0486(5) 0.1369(2) 0.0397(14) Uani 1 1 d . . . H38 H 0.2854 -0.0153 0.1121 0.048 Uiso 1 1 calc R . . C39 C 0.28209(10) 0.1630(5) 0.1374(2) 0.0371(13) Uani 1 1 d . . . H39 H 0.2675 0.1940 0.1132 0.045 Uiso 1 1 calc R . . C40 C 0.29786(9) 0.2250(4) 0.1813(2) 0.0267(11) Uani 1 1 d . . . C41 C 0.29622(9) 0.3526(4) 0.2010(2) 0.0297(11) Uani 1 1 d . . . H41A H 0.2969 0.4039 0.1646 0.036 Uiso 1 1 calc R . . H41B H 0.3126 0.3705 0.2265 0.036 Uiso 1 1 calc R . . C42 C 0.27151(10) 0.3913(4) 0.2363(2) 0.0317(12) Uani 1 1 d . . . C43 C 0.27738(11) 0.5153(5) 0.2625(3) 0.0474(15) Uani 1 1 d . . . H43A H 0.2618 0.5432 0.2844 0.071 Uiso 1 1 calc R . . H43B H 0.2809 0.5716 0.2297 0.071 Uiso 1 1 calc R . . H43C H 0.2932 0.5111 0.2904 0.071 Uiso 1 1 calc R . . C44 C 0.26707(10) 0.3025(4) 0.2873(2) 0.0352(12) Uani 1 1 d . . . H44A H 0.2836 0.2961 0.3129 0.053 Uiso 1 1 calc R . . H44B H 0.2625 0.2234 0.2702 0.053 Uiso 1 1 calc R . . H44C H 0.2522 0.3307 0.3116 0.053 Uiso 1 1 calc R . . C45 C 0.24617(10) 0.3984(6) 0.1943(3) 0.0545(17) Uani 1 1 d . . . H45A H 0.2312 0.4310 0.2166 0.082 Uiso 1 1 calc R . . H45B H 0.2415 0.3177 0.1794 0.082 Uiso 1 1 calc R . . H45C H 0.2497 0.4510 0.1600 0.082 Uiso 1 1 calc R . . C46 C 0.32585(10) -0.1965(4) 0.2879(3) 0.0433(15) Uani 1 1 d . . . H46 H 0.3199 -0.2689 0.2689 0.052 Uiso 1 1 calc R . . C47 C 0.33020(10) -0.1813(5) 0.3486(3) 0.0445(15) Uani 1 1 d . . . H47 H 0.3278 -0.2389 0.3796 0.053 Uiso 1 1 calc R . . C48 C 0.33895(9) -0.0625(4) 0.3551(2) 0.0329(12) Uani 1 1 d . . . C49 C 0.34636(10) 0.0028(5) 0.4122(2) 0.0391(13) Uani 1 1 d . . . H49A H 0.3570 0.0747 0.4020 0.047 Uiso 1 1 calc R . . H49B H 0.3581 -0.0500 0.4378 0.047 Uiso 1 1 calc R . . C50 C 0.32232(11) 0.0433(5) 0.4493(2) 0.0394(13) Uani 1 1 d . . . C51 C 0.30446(10) 0.1298(4) 0.4127(2) 0.0355(13) Uani 1 1 d . . . H51A H 0.3148 0.2023 0.4036 0.053 Uiso 1 1 calc R . . H51B H 0.2888 0.1517 0.4360 0.053 Uiso 1 1 calc R . . H51C H 0.2983 0.0910 0.3748 0.053 Uiso 1 1 calc R . . C52 C 0.33431(12) 0.1035(6) 0.5060(2) 0.0596(18) Uani 1 1 d . . . H52A H 0.3450 0.1733 0.4946 0.089 Uiso 1 1 calc R . . H52B H 0.3459 0.0462 0.5285 0.089 Uiso 1 1 calc R . . H52C H 0.3197 0.1299 0.5315 0.089 Uiso 1 1 calc R . . C53 C 0.30540(12) -0.0649(5) 0.4677(3) 0.0550(17) Uani 1 1 d . . . H53A H 0.2925 -0.0396 0.4976 0.083 Uiso 1 1 calc R . . H53B H 0.3173 -0.1272 0.4853 0.083 Uiso 1 1 calc R . . H53C H 0.2956 -0.0972 0.4320 0.083 Uiso 1 1 calc R . . Ni1 Ni 0.386267(11) 0.50211(5) 0.41794(3) 0.02069(13) Uani 1 1 d . . . Co2 Co 0.350356(13) 0.15360(6) 0.26648(3) 0.02442(15) Uani 1 1 d . . . N1 N 0.42580(7) 0.6363(3) 0.48888(16) 0.0222(8) Uani 1 1 d . . . N2 N 0.42094(7) 0.5211(3) 0.47033(16) 0.0224(9) Uani 1 1 d . . . N3 N 0.40146(7) 0.7479(3) 0.40469(16) 0.0231(9) Uani 1 1 d . . . N4 N 0.39641(7) 0.6476(3) 0.37014(16) 0.0224(8) Uani 1 1 d . . . N5 N 0.37848(7) 0.7009(3) 0.50018(16) 0.0215(8) Uani 1 1 d . . . N6 N 0.36510(7) 0.6017(3) 0.47894(16) 0.0226(9) Uani 1 1 d . . . N7 N 0.36039(8) -0.0315(3) 0.17536(18) 0.0308(10) Uani 1 1 d . . . N8 N 0.37253(7) 0.0688(3) 0.19995(17) 0.0266(9) Uani 1 1 d . . . N9 N 0.31298(8) 0.0408(4) 0.17690(18) 0.0342(10) Uani 1 1 d . . . N10 N 0.31666(7) 0.1502(4) 0.20473(17) 0.0278(9) Uani 1 1 d . . . N11 N 0.33121(8) -0.0934(3) 0.25931(19) 0.0332(10) Uani 1 1 d . . . N12 N 0.33939(8) -0.0090(3) 0.30113(17) 0.0302(9) Uani 1 1 d . . . O1 O 0.35129(6) 0.4469(3) 0.37358(13) 0.0249(7) Uani 1 1 d . . . O2 O 0.40070(6) 0.3553(3) 0.37384(14) 0.0272(7) Uani 1 1 d . . . O3 O 0.33665(6) 0.3020(3) 0.31043(14) 0.0258(7) Uani 1 1 d . . . O4 O 0.38506(6) 0.2024(3) 0.31619(14) 0.0317(8) Uani 1 1 d . . . C54 C 0.5008(2) 0.8576(7) 0.3532(6) 0.087(8) Uani 0.50 1 d PG A 1 H54 H 0.5051 0.9407 0.3562 0.105 Uiso 0.50 1 calc PR A 1 C55 C 0.4770(2) 0.8148(10) 0.3762(7) 0.099(12) Uani 0.50 1 d PG A 1 H55 H 0.4650 0.8686 0.3950 0.119 Uiso 0.50 1 calc PR A 1 C56 C 0.47064(16) 0.6932(10) 0.3719(5) 0.055(5) Uani 0.50 1 d PG A 1 H56 H 0.4543 0.6640 0.3876 0.066 Uiso 0.50 1 calc PR A 1 C57 C 0.48815(19) 0.6144(7) 0.3444(4) 0.039(3) Uani 0.50 1 d PG A 1 C58 C 0.51199(18) 0.6572(8) 0.3214(5) 0.056(5) Uani 0.50 1 d PG A 1 H58 H 0.5240 0.6034 0.3027 0.067 Uiso 0.50 1 calc PR A 1 C59 C 0.51831(17) 0.7788(9) 0.3258(5) 0.065(4) Uani 0.50 1 d PG A 1 H59 H 0.5346 0.8081 0.3100 0.078 Uiso 0.50 1 calc PR A 1 C60 C 0.4816(4) 0.4873(15) 0.3423(9) 0.061(5) Uani 0.50 1 d P A 1 H60A H 0.4698 0.4676 0.3753 0.091 Uiso 0.50 1 calc PR A 1 H60B H 0.4982 0.4400 0.3466 0.091 Uiso 0.50 1 calc PR A 1 H60C H 0.4724 0.4685 0.3035 0.091 Uiso 0.50 1 calc PR A 1 C54B C 0.4908(2) 0.4698(7) 0.3355(5) 0.059(7) Uani 0.50 1 d PG B 2 H54B H 0.4919 0.3853 0.3297 0.071 Uiso 0.50 1 calc PR B 2 C55B C 0.51359(15) 0.5410(10) 0.3301(5) 0.077(5) Uani 0.50 1 d PG B 2 H55B H 0.5303 0.5051 0.3206 0.092 Uiso 0.50 1 calc PR B 2 C56B C 0.51197(16) 0.6646(9) 0.3385(5) 0.055(6) Uani 0.50 1 d PG B 2 H56B H 0.5276 0.7133 0.3348 0.066 Uiso 0.50 1 calc PR B 2 C57B C 0.48754(19) 0.7171(6) 0.3523(5) 0.044(3) Uani 0.50 1 d PG B 2 C58B C 0.46472(14) 0.6460(8) 0.3577(5) 0.044(4) Uani 0.50 1 d PG B 2 H58B H 0.4480 0.6818 0.3672 0.053 Uiso 0.50 1 calc PR B 2 C59B C 0.46634(16) 0.5223(8) 0.3493(5) 0.049(4) Uani 0.50 1 d PG B 2 H59B H 0.4507 0.4737 0.3530 0.059 Uiso 0.50 1 calc PR B 2 C60B C 0.4865(4) 0.8435(15) 0.3613(12) 0.064(5) Uani 0.50 1 d P B 2 H60D H 0.4976 0.8651 0.3973 0.096 Uiso 0.50 1 calc PR B 2 H60E H 0.4678 0.8681 0.3669 0.096 Uiso 0.50 1 calc PR B 2 H60F H 0.4934 0.8846 0.3259 0.096 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.026(3) 0.015(2) 0.032(3) -0.002(2) 0.000(3) -0.004(2) B2 0.027(3) 0.033(3) 0.048(4) -0.022(3) 0.007(3) -0.006(3) C1 0.021(2) 0.031(3) 0.034(3) -0.006(2) 0.003(2) -0.001(2) C2 0.023(3) 0.031(3) 0.035(3) -0.003(2) -0.004(2) -0.001(2) C3 0.017(2) 0.020(2) 0.030(3) 0.001(2) -0.001(2) 0.0003(18) C4 0.029(3) 0.021(2) 0.028(3) -0.002(2) -0.005(2) -0.002(2) C5 0.032(3) 0.029(3) 0.047(3) 0.002(2) -0.002(3) -0.002(2) C6 0.033(3) 0.034(3) 0.052(4) 0.002(3) 0.000(3) 0.004(2) C7 0.042(3) 0.021(3) 0.053(4) 0.004(2) 0.002(3) 0.000(2) C8 0.039(3) 0.022(2) 0.040(3) 0.003(2) 0.001(3) -0.009(2) C9 0.033(3) 0.034(3) 0.028(3) 0.000(2) 0.008(2) -0.003(2) C10 0.030(3) 0.021(2) 0.040(3) 0.000(2) 0.010(2) 0.000(2) C11 0.033(3) 0.023(2) 0.031(3) 0.005(2) 0.012(2) 0.003(2) C12 0.022(2) 0.023(2) 0.026(3) -0.001(2) 0.002(2) 0.0026(19) C13 0.027(3) 0.025(2) 0.026(3) 0.004(2) 0.002(2) 0.002(2) C14 0.028(3) 0.033(3) 0.028(3) -0.003(2) 0.007(2) -0.003(2) C15 0.036(3) 0.032(3) 0.030(3) 0.002(2) 0.010(2) 0.000(2) C16 0.042(3) 0.039(3) 0.026(3) -0.003(2) 0.006(2) -0.006(2) C17 0.037(3) 0.043(3) 0.027(3) -0.004(3) 0.002(2) -0.012(3) C18 0.032(3) 0.031(3) 0.032(3) 0.003(2) 0.004(2) 0.003(2) C19 0.027(3) 0.020(2) 0.018(2) -0.0005(19) 0.001(2) 0.0020(19) C20 0.027(3) 0.025(2) 0.017(2) 0.000(2) 0.009(2) 0.001(2) C21 0.020(2) 0.025(2) 0.017(2) 0.0005(19) 0.0034(19) 0.0010(19) C22 0.024(2) 0.030(2) 0.023(3) 0.000(2) 0.005(2) 0.000(2) C23 0.024(3) 0.030(3) 0.066(4) -0.010(3) -0.012(3) -0.002(2) C24 0.038(3) 0.047(4) 0.076(5) -0.007(3) -0.009(3) 0.003(3) C25 0.026(3) 0.061(4) 0.107(6) -0.044(4) 0.018(4) -0.013(3) C26 0.069(5) 0.073(5) 0.041(4) -0.021(3) 0.031(3) -0.042(4) C27 0.070(4) 0.060(4) 0.035(3) -0.015(3) 0.018(3) -0.041(3) C28 0.016(2) 0.023(2) 0.023(3) 0.000(2) 0.0039(19) -0.0074(19) C29 0.019(2) 0.026(2) 0.022(3) 0.001(2) 0.003(2) 0.001(2) C30 0.039(3) 0.034(3) 0.029(3) -0.010(2) 0.006(2) 0.005(2) C31 0.030(3) 0.036(3) 0.029(3) -0.003(2) 0.010(2) 0.002(2) C32 0.028(3) 0.034(3) 0.023(3) 0.003(2) -0.001(2) 0.000(2) C33 0.034(3) 0.035(3) 0.038(3) 0.006(2) 0.000(3) -0.005(2) C34 0.023(3) 0.048(3) 0.053(4) 0.004(3) -0.002(3) 0.001(3) C35 0.066(5) 0.063(5) 0.242(12) -0.020(6) -0.074(7) -0.014(4) C36 0.045(4) 0.097(6) 0.059(4) 0.031(4) -0.013(3) 0.004(4) C37 0.032(4) 0.183(9) 0.070(5) 0.006(6) 0.015(4) 0.008(5) C38 0.023(3) 0.067(4) 0.030(3) -0.023(3) 0.003(2) -0.006(3) C39 0.022(3) 0.065(4) 0.024(3) -0.010(3) -0.005(2) -0.011(3) C40 0.014(2) 0.045(3) 0.022(3) -0.001(2) 0.007(2) -0.003(2) C41 0.026(3) 0.039(3) 0.024(3) 0.011(2) 0.001(2) -0.007(2) C42 0.024(3) 0.031(3) 0.041(3) 0.007(2) 0.005(2) 0.004(2) C43 0.042(3) 0.034(3) 0.066(4) 0.005(3) 0.004(3) 0.008(3) C44 0.029(3) 0.038(3) 0.040(3) -0.003(3) 0.012(2) -0.004(2) C45 0.028(3) 0.071(4) 0.064(4) 0.011(4) -0.006(3) 0.008(3) C46 0.033(3) 0.024(3) 0.074(4) -0.013(3) 0.024(3) -0.007(2) C47 0.040(3) 0.031(3) 0.064(4) 0.008(3) 0.028(3) 0.004(2) C48 0.024(3) 0.033(3) 0.043(3) 0.006(3) 0.014(2) 0.007(2) C49 0.037(3) 0.041(3) 0.040(3) 0.014(3) 0.008(3) 0.005(3) C50 0.038(3) 0.046(3) 0.034(3) 0.008(3) 0.006(3) 0.013(3) C51 0.040(3) 0.038(3) 0.029(3) 0.003(2) 0.002(2) 0.010(2) C52 0.060(4) 0.090(5) 0.029(3) -0.002(3) -0.002(3) 0.018(4) C53 0.059(4) 0.054(4) 0.053(4) 0.021(3) 0.019(3) 0.016(3) Ni1 0.0195(3) 0.0201(3) 0.0226(3) -0.0032(3) 0.0024(2) -0.0023(3) Co2 0.0237(3) 0.0241(3) 0.0254(4) -0.0059(3) 0.0010(3) -0.0023(3) N1 0.019(2) 0.0209(19) 0.026(2) -0.0047(17) -0.0018(17) -0.0032(16) N2 0.020(2) 0.020(2) 0.027(2) -0.0049(17) 0.0033(17) -0.0059(16) N3 0.027(2) 0.0165(18) 0.027(2) -0.0045(17) 0.0092(18) -0.0051(16) N4 0.023(2) 0.0206(19) 0.024(2) -0.0048(17) 0.0010(17) -0.0002(17) N5 0.024(2) 0.0176(18) 0.022(2) -0.0053(16) -0.0004(17) -0.0021(16) N6 0.023(2) 0.023(2) 0.021(2) -0.0044(17) -0.0021(17) -0.0032(16) N7 0.022(2) 0.036(2) 0.033(2) -0.015(2) -0.0004(19) -0.0056(18) N8 0.022(2) 0.028(2) 0.030(2) -0.0049(18) 0.0008(18) -0.0039(17) N9 0.025(2) 0.045(3) 0.032(3) -0.019(2) -0.001(2) -0.0066(19) N10 0.022(2) 0.036(2) 0.026(2) -0.0095(19) 0.0008(18) -0.0022(19) N11 0.030(2) 0.022(2) 0.048(3) -0.010(2) 0.011(2) -0.0040(18) N12 0.037(2) 0.026(2) 0.029(2) -0.0045(19) 0.0071(19) -0.0029(19) O1 0.0188(17) 0.0273(17) 0.0287(19) -0.0104(15) 0.0019(14) -0.0012(14) O2 0.0185(17) 0.0310(18) 0.0318(19) -0.0087(16) -0.0036(15) 0.0013(15) O3 0.0186(16) 0.0270(17) 0.0317(19) -0.0080(15) -0.0008(15) -0.0023(14) O4 0.0250(18) 0.0311(18) 0.039(2) -0.0147(16) 0.0002(16) 0.0045(15) C54 0.055(12) 0.079(13) 0.124(18) 0.025(12) -0.048(14) -0.007(11) C55 0.028(10) 0.16(3) 0.105(18) -0.063(19) -0.009(10) 0.020(12) C56 0.030(8) 0.094(13) 0.041(10) 0.005(10) 0.007(7) -0.012(9) C57 0.028(6) 0.056(8) 0.033(7) 0.004(6) 0.006(5) -0.004(6) C58 0.049(12) 0.073(14) 0.046(9) -0.016(8) 0.004(7) 0.012(10) C59 0.046(8) 0.058(9) 0.091(11) 0.002(8) 0.011(8) 0.000(7) C60 0.074(13) 0.065(12) 0.043(10) -0.002(9) -0.011(9) -0.022(10) C54B 0.042(10) 0.055(10) 0.080(15) -0.020(9) -0.011(9) 0.031(8) C55B 0.035(8) 0.101(13) 0.093(12) -0.047(10) -0.007(8) 0.008(8) C56B 0.024(8) 0.081(14) 0.062(10) -0.039(9) 0.023(7) -0.022(8) C57B 0.040(7) 0.060(8) 0.033(7) -0.003(6) 0.000(6) 0.008(6) C58B 0.028(7) 0.067(10) 0.037(8) -0.009(7) 0.005(6) 0.009(7) C59B 0.051(9) 0.060(10) 0.037(8) 0.009(7) 0.014(7) -0.009(7) C60B 0.066(14) 0.041(8) 0.083(13) -0.003(9) -0.029(11) 0.027(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N5 1.531(6) . ? B1 N3 1.539(6) . ? B1 N1 1.540(6) . ? B1 H1A 1.0000 . ? B2 N9 1.528(7) . ? B2 N11 1.535(7) . ? B2 N7 1.536(7) . ? B2 H2A 1.0000 . ? C1 N1 1.343(5) . ? C1 C2 1.362(6) . ? C1 H1 0.9500 . ? C2 C3 1.400(6) . ? C2 H2 0.9500 . ? C3 N2 1.341(5) . ? C3 C4 1.494(6) . ? C4 C5 1.523(6) . ? C4 C9 1.523(6) . ? C4 H4 1.0000 . ? C5 C6 1.519(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.507(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.529(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.335(5) . ? C10 C11 1.374(6) . ? C10 H10 0.9500 . ? C11 C12 1.394(6) . ? C11 H11 0.9500 . ? C12 N4 1.347(5) . ? C12 C13 1.507(6) . ? C13 C18 1.519(6) . ? C13 C14 1.531(6) . ? C13 H13 1.0000 . ? C14 C15 1.521(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.507(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.512(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.532(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N5 1.344(5) . ? C19 C20 1.367(6) . ? C19 H19 0.9500 . ? C20 C21 1.397(6) . ? C20 H20 0.9500 . ? C21 N6 1.345(5) . ? C21 C22 1.501(6) . ? C22 C27 1.513(6) . ? C22 C23 1.540(6) . ? C22 H22 1.0000 . ? C23 C24 1.515(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.490(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.529(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O1 1.246(5) . ? C28 O3 1.259(5) . ? C28 C29 1.529(6) . ? C29 O2 1.249(5) . ? C29 O4 1.253(5) . ? C30 N7 1.338(6) . ? C30 C31 1.366(6) . ? C30 H30 0.9500 . ? C31 C32 1.399(6) . ? C31 H31 0.9500 . ? C32 N8 1.336(6) . ? C32 C33 1.500(6) . ? C33 C34 1.545(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C36 1.492(7) . ? C34 C37 1.497(8) . ? C34 C35 1.507(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 N9 1.337(6) . ? C38 C39 1.367(7) . ? C38 H38 0.9500 . ? C39 C40 1.404(6) . ? C39 H39 0.9500 . ? C40 N10 1.339(6) . ? C40 C41 1.487(6) . ? C41 C42 1.540(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.519(7) . ? C42 C44 1.522(6) . ? C42 C45 1.536(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N11 1.341(6) . ? C46 C47 1.361(7) . ? C46 H46 0.9500 . ? C47 C48 1.397(7) . ? C47 H47 0.9500 . ? C48 N12 1.335(6) . ? C48 C49 1.490(7) . ? C49 C50 1.542(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.520(6) . ? C50 C52 1.523(7) . ? C50 C53 1.531(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? Ni1 N4 2.008(4) . ? Ni1 O2 2.045(3) . ? Ni1 N2 2.047(4) . ? Ni1 O1 2.054(3) . ? Ni1 N6 2.065(4) . ? Co2 O3 2.045(3) . ? Co2 N12 2.045(4) . ? Co2 O4 2.078(3) . ? Co2 N8 2.096(4) . ? Co2 N10 2.117(4) . ? N1 N2 1.364(5) . ? N3 N4 1.370(5) . ? N5 N6 1.361(5) . ? N7 N8 1.370(5) . ? N9 N10 1.372(5) . ? N11 N12 1.369(5) . ? C54 C55 1.3900 . ? C54 C59 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 C58 1.3900 . ? C57 C60 1.450(17) . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C54B C55B 1.3900 . ? C54B C59B 1.3900 . ? C54B H54B 0.9500 . ? C55B C56B 1.3900 . ? C55B H55B 0.9500 . ? C56B C57B 1.3900 . ? C56B H56B 0.9500 . ? C57B C58B 1.3900 . ? C57B C60B 1.420(17) . ? C58B C59B 1.3900 . ? C58B H58B 0.9500 . ? C59B H59B 0.9500 . ? C60B H60D 0.9800 . ? C60B H60E 0.9800 . ? C60B H60F 0.9800 . ? 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 N5 B1 N3 108.8(4) . . ? N5 B1 N1 107.5(4) . . ? N3 B1 N1 109.1(4) . . ? N5 B1 H1A 110.4 . . ? N3 B1 H1A 110.4 . . ? N1 B1 H1A 110.4 . . ? N9 B2 N11 109.3(4) . . ? N9 B2 N7 108.5(4) . . ? N11 B2 N7 108.8(4) . . ? N9 B2 H2A 110.1 . . ? N11 B2 H2A 110.1 . . ? N7 B2 H2A 110.1 . . ? N1 C1 C2 108.9(4) . . ? N1 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? C1 C2 C3 106.0(4) . . ? C1 C2 H2 127.0 . . ? C3 C2 H2 127.0 . . ? N2 C3 C2 108.6(4) . . ? N2 C3 C4 122.3(4) . . ? C2 C3 C4 129.0(4) . . ? C3 C4 C5 113.1(4) . . ? C3 C4 C9 112.3(4) . . ? C5 C4 C9 110.2(4) . . ? C3 C4 H4 107.0 . . ? C5 C4 H4 107.0 . . ? C9 C4 H4 107.0 . . ? C6 C5 C4 111.0(4) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.6(4) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 112.0(4) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 111.2(4) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C4 C9 C8 110.1(4) . . ? C4 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C4 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? N3 C10 C11 109.1(4) . . ? N3 C10 H10 125.4 . . ? C11 C10 H10 125.4 . . ? C10 C11 C12 105.4(4) . . ? C10 C11 H11 127.3 . . ? C12 C11 H11 127.3 . . ? N4 C12 C11 109.2(4) . . ? N4 C12 C13 122.1(4) . . ? C11 C12 C13 128.5(4) . . ? C12 C13 C18 114.2(4) . . ? C12 C13 C14 109.9(4) . . ? C18 C13 C14 109.7(4) . . ? C12 C13 H13 107.6 . . ? C18 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C15 C14 C13 112.2(4) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 111.8(4) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 110.8(4) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.1(4) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C13 C18 C17 110.9(4) . . ? C13 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.0 . . ? N5 C19 C20 108.7(4) . . ? N5 C19 H19 125.7 . . ? C20 C19 H19 125.7 . . ? C19 C20 C21 105.6(4) . . ? C19 C20 H20 127.2 . . ? C21 C20 H20 127.2 . . ? N6 C21 C20 109.4(4) . . ? N6 C21 C22 123.0(4) . . ? C20 C21 C22 127.4(4) . . ? C21 C22 C27 111.8(4) . . ? C21 C22 C23 109.7(4) . . ? C27 C22 C23 110.7(4) . . ? C21 C22 H22 108.2 . . ? C27 C22 H22 108.2 . . ? C23 C22 H22 108.2 . . ? C24 C23 C22 111.1(4) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 111.7(5) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.5(5) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 111.9(5) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C22 C27 C26 112.6(4) . . ? C22 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C22 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? O1 C28 O3 126.3(4) . . ? O1 C28 C29 116.9(4) . . ? O3 C28 C29 116.7(4) . . ? O2 C29 O4 127.6(4) . . ? O2 C29 C28 116.6(4) . . ? O4 C29 C28 115.8(4) . . ? N7 C30 C31 109.4(4) . . ? N7 C30 H30 125.3 . . ? C31 C30 H30 125.3 . . ? C30 C31 C32 105.1(4) . . ? C30 C31 H31 127.5 . . ? C32 C31 H31 127.5 . . ? N8 C32 C31 109.7(4) . . ? N8 C32 C33 121.2(4) . . ? C31 C32 C33 129.0(5) . . ? C32 C33 C34 118.2(4) . . ? C32 C33 H33A 107.8 . . ? C34 C33 H33A 107.8 . . ? C32 C33 H33B 107.8 . . ? C34 C33 H33B 107.8 . . ? H33A C33 H33B 107.1 . . ? C36 C34 C37 110.2(5) . . ? C36 C34 C35 108.3(6) . . ? C37 C34 C35 108.4(6) . . ? C36 C34 C33 110.9(5) . . ? C37 C34 C33 111.1(5) . . ? C35 C34 C33 107.8(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N9 C38 C39 109.1(5) . . ? N9 C38 H38 125.5 . . ? C39 C38 H38 125.5 . . ? C38 C39 C40 105.7(5) . . ? C38 C39 H39 127.2 . . ? C40 C39 H39 127.2 . . ? N10 C40 C39 108.9(4) . . ? N10 C40 C41 121.6(4) . . ? C39 C40 C41 129.6(5) . . ? C40 C41 C42 118.0(4) . . ? C40 C41 H41A 107.8 . . ? C42 C41 H41A 107.8 . . ? C40 C41 H41B 107.8 . . ? C42 C41 H41B 107.8 . . ? H41A C41 H41B 107.1 . . ? C43 C42 C44 109.7(4) . . ? C43 C42 C45 109.0(4) . . ? C44 C42 C45 110.1(4) . . ? C43 C42 C41 107.6(4) . . ? C44 C42 C41 109.6(4) . . ? C45 C42 C41 110.8(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N11 C46 C47 109.5(5) . . ? N11 C46 H46 125.3 . . ? C47 C46 H46 125.3 . . ? C46 C47 C48 104.8(5) . . ? C46 C47 H47 127.6 . . ? C48 C47 H47 127.6 . . ? N12 C48 C47 110.2(5) . . ? N12 C48 C49 122.0(4) . . ? C47 C48 C49 127.8(5) . . ? C48 C49 C50 115.1(4) . . ? C48 C49 H49A 108.5 . . ? C50 C49 H49A 108.5 . . ? C48 C49 H49B 108.5 . . ? C50 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C51 C50 C52 111.2(5) . . ? C51 C50 C53 109.0(4) . . ? C52 C50 C53 109.0(5) . . ? C51 C50 C49 110.3(4) . . ? C52 C50 C49 106.4(4) . . ? C53 C50 C49 110.9(4) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 Ni1 O2 106.94(13) . . ? N4 Ni1 N2 89.61(14) . . ? O2 Ni1 N2 92.91(13) . . ? N4 Ni1 O1 102.32(13) . . ? O2 Ni1 O1 80.69(12) . . ? N2 Ni1 O1 167.66(13) . . ? N4 Ni1 N6 93.27(14) . . ? O2 Ni1 N6 159.48(14) . . ? N2 Ni1 N6 90.66(14) . . ? O1 Ni1 N6 91.79(13) . . ? O3 Co2 N12 115.85(14) . . ? O3 Co2 O4 79.70(12) . . ? N12 Co2 O4 105.03(15) . . ? O3 Co2 N8 152.91(14) . . ? N12 Co2 N8 91.20(15) . . ? O4 Co2 N8 92.46(13) . . ? O3 Co2 N10 93.03(13) . . ? N12 Co2 N10 90.66(16) . . ? O4 Co2 N10 164.30(15) . . ? N8 Co2 N10 87.76(14) . . ? C1 N1 N2 108.9(4) . . ? C1 N1 B1 130.3(4) . . ? N2 N1 B1 120.8(3) . . ? C3 N2 N1 107.6(3) . . ? C3 N2 Ni1 138.5(3) . . ? N1 N2 Ni1 113.7(3) . . ? C10 N3 N4 109.2(4) . . ? C10 N3 B1 130.3(4) . . ? N4 N3 B1 120.4(3) . . ? C12 N4 N3 107.0(3) . . ? C12 N4 Ni1 138.4(3) . . ? N3 N4 Ni1 113.9(3) . . ? C19 N5 N6 109.6(4) . . ? C19 N5 B1 130.3(4) . . ? N6 N5 B1 120.1(4) . . ? C21 N6 N5 106.8(3) . . ? C21 N6 Ni1 138.9(3) . . ? N5 N6 Ni1 114.0(3) . . ? C30 N7 N8 108.9(4) . . ? C30 N7 B2 130.4(4) . . ? N8 N7 B2 120.6(4) . . ? C32 N8 N7 107.0(4) . . ? C32 N8 Co2 138.6(3) . . ? N7 N8 Co2 114.2(3) . . ? C38 N9 N10 109.0(4) . . ? C38 N9 B2 129.2(4) . . ? N10 N9 B2 121.7(4) . . ? C40 N10 N9 107.4(4) . . ? C40 N10 Co2 139.4(3) . . ? N9 N10 Co2 113.2(3) . . ? C46 N11 N12 109.0(4) . . ? C46 N11 B2 130.0(4) . . ? N12 N11 B2 120.7(4) . . ? C48 N12 N11 106.5(4) . . ? C48 N12 Co2 138.0(3) . . ? N11 N12 Co2 115.4(3) . . ? C28 O1 Ni1 112.7(3) . . ? C29 O2 Ni1 113.0(3) . . ? C28 O3 Co2 114.0(3) . . ? C29 O4 Co2 113.5(3) . . ? C55 C54 C59 120.0 . . ? C55 C54 H54 120.0 . . ? C59 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 C60 120.9(10) . . ? C56 C57 C60 119.0(10) . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C58 C59 C54 120.0 . . ? C58 C59 H59 120.0 . . ? C54 C59 H59 120.0 . . ? C55B C54B C59B 120.0 . . ? C55B C54B H54B 120.0 . . ? C59B C54B H54B 120.0 . . ? C54B C55B C56B 120.0 . . ? C54B C55B H55B 120.0 . . ? C56B C55B H55B 120.0 . . ? C57B C56B C55B 120.0 . . ? C57B C56B H56B 120.0 . . ? C55B C56B H56B 120.0 . . ? C56B C57B C58B 120.0 . . ? C56B C57B C60B 118.9(11) . . ? C58B C57B C60B 121.1(11) . . ? C57B C58B C59B 120.0 . . ? C57B C58B H58B 120.0 . . ? C59B C58B H58B 120.0 . . ? C58B C59B C54B 120.0 . . ? C58B C59B H59B 120.0 . . ? C54B C59B H59B 120.0 . . ? C57B C60B H60D 109.5 . . ? C57B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? C57B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.6(6) . . . . ? C1 C2 C3 N2 -0.5(5) . . . . ? C1 C2 C3 C4 176.2(5) . . . . ? N2 C3 C4 C5 168.0(4) . . . . ? C2 C3 C4 C5 -8.3(7) . . . . ? N2 C3 C4 C9 -66.6(6) . . . . ? C2 C3 C4 C9 117.2(5) . . . . ? C3 C4 C5 C6 -176.1(4) . . . . ? C9 C4 C5 C6 57.3(5) . . . . ? C4 C5 C6 C7 -54.9(6) . . . . ? C5 C6 C7 C8 53.7(6) . . . . ? C6 C7 C8 C9 -54.8(6) . . . . ? C3 C4 C9 C8 174.8(4) . . . . ? C5 C4 C9 C8 -58.1(5) . . . . ? C7 C8 C9 C4 57.0(5) . . . . ? N3 C10 C11 C12 -1.0(5) . . . . ? C10 C11 C12 N4 1.9(5) . . . . ? C10 C11 C12 C13 -173.3(4) . . . . ? N4 C12 C13 C18 100.1(5) . . . . ? C11 C12 C13 C18 -85.2(6) . . . . ? N4 C12 C13 C14 -136.1(4) . . . . ? C11 C12 C13 C14 38.6(6) . . . . ? C12 C13 C14 C15 178.9(4) . . . . ? C18 C13 C14 C15 -54.7(5) . . . . ? C13 C14 C15 C16 54.6(5) . . . . ? C14 C15 C16 C17 -54.8(5) . . . . ? C15 C16 C17 C18 56.5(6) . . . . ? C12 C13 C18 C17 179.9(4) . . . . ? C14 C13 C18 C17 56.0(5) . . . . ? C16 C17 C18 C13 -57.9(5) . . . . ? N5 C19 C20 C21 0.6(5) . . . . ? C19 C20 C21 N6 -0.3(5) . . . . ? C19 C20 C21 C22 -175.1(4) . . . . ? N6 C21 C22 C27 144.2(5) . . . . ? C20 C21 C22 C27 -41.6(6) . . . . ? N6 C21 C22 C23 -92.6(5) . . . . ? C20 C21 C22 C23 81.6(6) . . . . ? C21 C22 C23 C24 -177.5(4) . . . . ? C27 C22 C23 C24 -53.7(6) . . . . ? C22 C23 C24 C25 56.7(6) . . . . ? C23 C24 C25 C26 -57.1(6) . . . . ? C24 C25 C26 C27 54.5(7) . . . . ? C21 C22 C27 C26 174.5(5) . . . . ? C23 C22 C27 C26 51.8(7) . . . . ? C25 C26 C27 C22 -52.6(7) . . . . ? O1 C28 C29 O2 -4.4(6) . . . . ? O3 C28 C29 O2 175.6(4) . . . . ? O1 C28 C29 O4 176.2(4) . . . . ? O3 C28 C29 O4 -3.8(6) . . . . ? N7 C30 C31 C32 0.7(6) . . . . ? C30 C31 C32 N8 -0.4(5) . . . . ? C30 C31 C32 C33 -176.8(5) . . . . ? N8 C32 C33 C34 124.4(5) . . . . ? C31 C32 C33 C34 -59.6(7) . . . . ? C32 C33 C34 C36 -46.0(7) . . . . ? C32 C33 C34 C37 77.0(7) . . . . ? C32 C33 C34 C35 -164.4(6) . . . . ? N9 C38 C39 C40 -1.0(6) . . . . ? C38 C39 C40 N10 0.9(6) . . . . ? C38 C39 C40 C41 179.6(5) . . . . ? N10 C40 C41 C42 -112.5(5) . . . . ? C39 C40 C41 C42 69.0(7) . . . . ? C40 C41 C42 C43 168.1(4) . . . . ? C40 C41 C42 C44 48.9(6) . . . . ? C40 C41 C42 C45 -72.8(6) . . . . ? N11 C46 C47 C48 -0.8(6) . . . . ? C46 C47 C48 N12 0.9(6) . . . . ? C46 C47 C48 C49 179.3(5) . . . . ? N12 C48 C49 C50 102.2(5) . . . . ? C47 C48 C49 C50 -76.0(7) . . . . ? C48 C49 C50 C51 -61.1(6) . . . . ? C48 C49 C50 C52 178.1(5) . . . . ? C48 C49 C50 C53 59.7(6) . . . . ? C2 C1 N1 N2 -0.5(5) . . . . ? C2 C1 N1 B1 179.9(4) . . . . ? N5 B1 N1 C1 -122.3(5) . . . . ? N3 B1 N1 C1 119.8(5) . . . . ? N5 B1 N1 N2 58.0(5) . . . . ? N3 B1 N1 N2 -59.8(5) . . . . ? C2 C3 N2 N1 0.2(5) . . . . ? C4 C3 N2 N1 -176.7(4) . . . . ? C2 C3 N2 Ni1 174.8(3) . . . . ? C4 C3 N2 Ni1 -2.2(7) . . . . ? C1 N1 N2 C3 0.1(5) . . . . ? B1 N1 N2 C3 179.8(4) . . . . ? C1 N1 N2 Ni1 -175.9(3) . . . . ? B1 N1 N2 Ni1 3.8(5) . . . . ? N4 Ni1 N2 C3 -128.7(5) . . . . ? O2 Ni1 N2 C3 -21.8(5) . . . . ? O1 Ni1 N2 C3 36.5(9) . . . . ? N6 Ni1 N2 C3 138.0(5) . . . . ? N4 Ni1 N2 N1 45.6(3) . . . . ? O2 Ni1 N2 N1 152.6(3) . . . . ? O1 Ni1 N2 N1 -149.2(5) . . . . ? N6 Ni1 N2 N1 -47.6(3) . . . . ? C11 C10 N3 N4 -0.3(5) . . . . ? C11 C10 N3 B1 174.9(4) . . . . ? N5 B1 N3 C10 117.5(5) . . . . ? N1 B1 N3 C10 -125.5(5) . . . . ? N5 B1 N3 N4 -67.9(5) . . . . ? N1 B1 N3 N4 49.2(5) . . . . ? C11 C12 N4 N3 -2.1(5) . . . . ? C13 C12 N4 N3 173.5(4) . . . . ? C11 C12 N4 Ni1 167.2(3) . . . . ? C13 C12 N4 Ni1 -17.2(7) . . . . ? C10 N3 N4 C12 1.5(5) . . . . ? B1 N3 N4 C12 -174.2(4) . . . . ? C10 N3 N4 Ni1 -170.8(3) . . . . ? B1 N3 N4 Ni1 13.5(5) . . . . ? O2 Ni1 N4 C12 43.6(5) . . . . ? N2 Ni1 N4 C12 136.6(5) . . . . ? O1 Ni1 N4 C12 -40.2(5) . . . . ? N6 Ni1 N4 C12 -132.8(5) . . . . ? O2 Ni1 N4 N3 -147.6(3) . . . . ? N2 Ni1 N4 N3 -54.6(3) . . . . ? O1 Ni1 N4 N3 128.6(3) . . . . ? N6 Ni1 N4 N3 36.0(3) . . . . ? C20 C19 N5 N6 -0.7(5) . . . . ? C20 C19 N5 B1 178.5(4) . . . . ? N3 B1 N5 C19 -125.3(5) . . . . ? N1 B1 N5 C19 116.7(5) . . . . ? N3 B1 N5 N6 53.8(5) . . . . ? N1 B1 N5 N6 -64.2(5) . . . . ? C20 C21 N6 N5 -0.2(5) . . . . ? C22 C21 N6 N5 175.0(4) . . . . ? C20 C21 N6 Ni1 172.8(3) . . . . ? C22 C21 N6 Ni1 -12.1(7) . . . . ? C19 N5 N6 C21 0.5(5) . . . . ? B1 N5 N6 C21 -178.8(4) . . . . ? C19 N5 N6 Ni1 -174.4(3) . . . . ? B1 N5 N6 Ni1 6.3(5) . . . . ? N4 Ni1 N6 C21 140.5(4) . . . . ? O2 Ni1 N6 C21 -29.7(7) . . . . ? N2 Ni1 N6 C21 -129.9(4) . . . . ? O1 Ni1 N6 C21 38.1(5) . . . . ? N4 Ni1 N6 N5 -46.9(3) . . . . ? O2 Ni1 N6 N5 142.9(3) . . . . ? N2 Ni1 N6 N5 42.7(3) . . . . ? O1 Ni1 N6 N5 -149.4(3) . . . . ? C31 C30 N7 N8 -0.7(5) . . . . ? C31 C30 N7 B2 177.1(5) . . . . ? N9 B2 N7 C30 -121.8(5) . . . . ? N11 B2 N7 C30 119.4(5) . . . . ? N9 B2 N7 N8 55.8(6) . . . . ? N11 B2 N7 N8 -63.0(6) . . . . ? C31 C32 N8 N7 0.0(5) . . . . ? C33 C32 N8 N7 176.7(4) . . . . ? C31 C32 N8 Co2 173.8(4) . . . . ? C33 C32 N8 Co2 -9.4(7) . . . . ? C30 N7 N8 C32 0.4(5) . . . . ? B2 N7 N8 C32 -177.6(4) . . . . ? C30 N7 N8 Co2 -175.1(3) . . . . ? B2 N7 N8 Co2 6.8(5) . . . . ? O3 Co2 N8 C32 43.6(6) . . . . ? N12 Co2 N8 C32 -133.5(5) . . . . ? O4 Co2 N8 C32 -28.4(5) . . . . ? N10 Co2 N8 C32 135.8(5) . . . . ? O3 Co2 N8 N7 -142.9(3) . . . . ? N12 Co2 N8 N7 40.0(3) . . . . ? O4 Co2 N8 N7 145.1(3) . . . . ? N10 Co2 N8 N7 -50.6(3) . . . . ? C39 C38 N9 N10 0.6(6) . . . . ? C39 C38 N9 B2 -177.4(5) . . . . ? N11 B2 N9 C38 -124.5(5) . . . . ? N7 B2 N9 C38 117.0(5) . . . . ? N11 B2 N9 N10 57.6(6) . . . . ? N7 B2 N9 N10 -60.9(6) . . . . ? C39 C40 N10 N9 -0.6(5) . . . . ? C41 C40 N10 N9 -179.4(4) . . . . ? C39 C40 N10 Co2 175.4(4) . . . . ? C41 C40 N10 Co2 -3.4(7) . . . . ? C38 N9 N10 C40 0.0(5) . . . . ? B2 N9 N10 C40 178.2(4) . . . . ? C38 N9 N10 Co2 -177.2(3) . . . . ? B2 N9 N10 Co2 1.1(5) . . . . ? O3 Co2 N10 C40 23.4(5) . . . . ? N12 Co2 N10 C40 139.4(5) . . . . ? O4 Co2 N10 C40 -38.3(8) . . . . ? N8 Co2 N10 C40 -129.4(5) . . . . ? O3 Co2 N10 N9 -160.8(3) . . . . ? N12 Co2 N10 N9 -44.8(3) . . . . ? O4 Co2 N10 N9 137.5(5) . . . . ? N8 Co2 N10 N9 46.3(3) . . . . ? C47 C46 N11 N12 0.4(6) . . . . ? C47 C46 N11 B2 174.9(5) . . . . ? N9 B2 N11 C46 125.6(5) . . . . ? N7 B2 N11 C46 -116.1(6) . . . . ? N9 B2 N11 N12 -60.5(6) . . . . ? N7 B2 N11 N12 57.8(6) . . . . ? C47 C48 N12 N11 -0.7(5) . . . . ? C49 C48 N12 N11 -179.2(4) . . . . ? C47 C48 N12 Co2 -176.7(4) . . . . ? C49 C48 N12 Co2 4.8(8) . . . . ? C46 N11 N12 C48 0.2(5) . . . . ? B2 N11 N12 C48 -174.9(4) . . . . ? C46 N11 N12 Co2 177.2(3) . . . . ? B2 N11 N12 Co2 2.2(5) . . . . ? O3 Co2 N12 C48 -47.4(5) . . . . ? O4 Co2 N12 C48 38.3(5) . . . . ? N8 Co2 N12 C48 131.1(5) . . . . ? N10 Co2 N12 C48 -141.1(5) . . . . ? O3 Co2 N12 N11 136.8(3) . . . . ? O4 Co2 N12 N11 -137.5(3) . . . . ? N8 Co2 N12 N11 -44.6(3) . . . . ? N10 Co2 N12 N11 43.1(3) . . . . ? O3 C28 O1 Ni1 -178.8(4) . . . . ? C29 C28 O1 Ni1 1.2(5) . . . . ? N4 Ni1 O1 C28 106.5(3) . . . . ? O2 Ni1 O1 C28 1.0(3) . . . . ? N2 Ni1 O1 C28 -58.4(7) . . . . ? N6 Ni1 O1 C28 -159.8(3) . . . . ? O4 C29 O2 Ni1 -175.7(4) . . . . ? C28 C29 O2 Ni1 5.0(5) . . . . ? N4 Ni1 O2 C29 -103.6(3) . . . . ? N2 Ni1 O2 C29 165.9(3) . . . . ? O1 Ni1 O2 C29 -3.5(3) . . . . ? N6 Ni1 O2 C29 66.2(5) . . . . ? O1 C28 O3 Co2 179.3(4) . . . . ? C29 C28 O3 Co2 -0.7(5) . . . . ? N12 Co2 O3 C28 104.7(3) . . . . ? O4 Co2 O3 C28 2.9(3) . . . . ? N8 Co2 O3 C28 -72.1(4) . . . . ? N10 Co2 O3 C28 -163.1(3) . . . . ? O2 C29 O4 Co2 -173.3(4) . . . . ? C28 C29 O4 Co2 6.1(5) . . . . ? O3 Co2 O4 C29 -5.1(3) . . . . ? N12 Co2 O4 C29 -119.3(3) . . . . ? N8 Co2 O4 C29 148.8(3) . . . . ? N10 Co2 O4 C29 58.4(6) . . . . ? C59 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C58 0.0 . . . . ? C55 C56 C57 C60 177.9(12) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C60 C57 C58 C59 -177.8(12) . . . . ? C57 C58 C59 C54 0.0 . . . . ? C55 C54 C59 C58 0.0 . . . . ? C59B C54B C55B C56B 0.0 . . . . ? C54B C55B C56B C57B 0.0 . . . . ? C55B C56B C57B C58B 0.0 . . . . ? C55B C56B C57B C60B 179.3(14) . . . . ? C56B C57B C58B C59B 0.0 . . . . ? C60B C57B C58B C59B -179.3(15) . . . . ? C57B C58B C59B C54B 0.0 . . . . ? C55B C54B C59B C58B 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.572 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.093 data_09mz142_0m _database_code_depnum_ccdc_archive 'CCDC 881839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H86 B2 N14 Ni2 O4' _chemical_formula_weight 1206.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 32.660(3) _cell_length_b 32.660(3) _cell_length_c 11.347(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12104(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1503 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.54 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; One of the cyclohexyl rings shows a large freedom of movement and was refined as disordered over two positions. The occupancy ratio refined to 0.72(2) to 0.28(2). The two moieties were restrained to have similar geometries and the ADPs of disordered atoms were restrained to be approximately isotropic. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 31994 _diffrn_reflns_av_R_equivalents 0.1730 _diffrn_reflns_av_sigmaI/netI 0.1650 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7410 _reflns_number_gt 3674 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7410 _refine_ls_number_parameters 417 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1635 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.91405(14) 0.72264(14) 0.1315(4) 0.0247(11) Uani 1 1 d . . . H1 H 0.9414 0.7133 0.1028 0.030 Uiso 1 1 calc R . . C1 C 0.74728(11) 0.76340(10) 0.1944(3) 0.0164(8) Uani 1 1 d . . . C2 C 0.93918(11) 0.70623(11) 0.3445(4) 0.0208(9) Uani 1 1 d . . . H2 H 0.9654 0.6953 0.3267 0.025 Uiso 1 1 calc R . . C3 C 0.92210(11) 0.70820(11) 0.4535(4) 0.0223(9) Uani 1 1 d . . . H3 H 0.9338 0.6992 0.5256 0.027 Uiso 1 1 calc R . . C4 C 0.88366(11) 0.72633(10) 0.4371(4) 0.0176(9) Uani 1 1 d . . . C5 C 0.85234(11) 0.73662(10) 0.5277(3) 0.0184(8) Uani 1 1 d . . . H5 H 0.8306 0.7535 0.4890 0.022 Uiso 1 1 calc R . . C6 C 0.87098(11) 0.76190(11) 0.6267(3) 0.0227(9) Uani 1 1 d . . . H6A H 0.8937 0.7463 0.6630 0.027 Uiso 1 1 calc R . . H6B H 0.8825 0.7874 0.5934 0.027 Uiso 1 1 calc R . . C7 C 0.83983(12) 0.77266(12) 0.7209(4) 0.0292(10) Uani 1 1 d . . . H7A H 0.8537 0.7873 0.7861 0.035 Uiso 1 1 calc R . . H7B H 0.8190 0.7913 0.6872 0.035 Uiso 1 1 calc R . . C8 C 0.81895(13) 0.73468(12) 0.7690(4) 0.0329(11) Uani 1 1 d . . . H8A H 0.8392 0.7179 0.8125 0.039 Uiso 1 1 calc R . . H8B H 0.7972 0.7429 0.8250 0.039 Uiso 1 1 calc R . . C9 C 0.80049(13) 0.70956(13) 0.6713(4) 0.0356(11) Uani 1 1 d . . . H9A H 0.7779 0.7251 0.6343 0.043 Uiso 1 1 calc R . . H9B H 0.7889 0.6841 0.7046 0.043 Uiso 1 1 calc R . . C10 C 0.83210(12) 0.69879(11) 0.5784(4) 0.0251(10) Uani 1 1 d . . . H10A H 0.8533 0.6809 0.6138 0.030 Uiso 1 1 calc R . . H10B H 0.8187 0.6833 0.5140 0.030 Uiso 1 1 calc R . . C11 C 0.88463(12) 0.65847(12) 0.0289(4) 0.0273(10) Uani 1 1 d . . . H11 H 0.9097 0.6476 0.0003 0.033 Uiso 1 1 calc R . . C12 C 0.84710(11) 0.64110(12) 0.0142(4) 0.0248(10) Uani 1 1 d . . . H12 H 0.8409 0.6163 -0.0255 0.030 Uiso 1 1 calc R . . C13 C 0.81974(12) 0.66750(12) 0.0698(4) 0.0226(9) Uani 1 1 d . A . C14 C 0.77453(11) 0.66444(12) 0.0856(4) 0.0232(10) Uani 1 1 d . . . H14B H 0.7662 0.6871 0.1396 0.028 Uiso 0.28(2) 1 calc PR A 2 H14 H 0.7651 0.6911 0.1143 0.028 Uiso 0.72(2) 1 d PR A 1 C15 C 0.7510(4) 0.6556(4) -0.0314(9) 0.035(3) Uani 0.72(2) 1 d PDU A 1 H15A H 0.7220 0.6633 -0.0202 0.043 Uiso 0.72(2) 1 calc PR A 1 H15B H 0.7623 0.6735 -0.0938 0.043 Uiso 0.72(2) 1 calc PR A 1 C16 C 0.7528(3) 0.6122(4) -0.0735(10) 0.059(4) Uani 0.72(2) 1 d PDU A 1 H16A H 0.7323 0.6081 -0.1366 0.071 Uiso 0.72(2) 1 calc PR A 1 H16B H 0.7802 0.6066 -0.1071 0.071 Uiso 0.72(2) 1 calc PR A 1 C17 C 0.7446(3) 0.5830(3) 0.0243(16) 0.070(5) Uani 0.72(2) 1 d PDU A 1 H17A H 0.7507 0.5549 -0.0039 0.084 Uiso 0.72(2) 1 calc PR A 1 H17B H 0.7151 0.5841 0.0437 0.084 Uiso 0.72(2) 1 calc PR A 1 C18 C 0.7691(3) 0.5906(3) 0.1374(15) 0.065(4) Uani 0.72(2) 1 d PDU A 1 H18A H 0.7595 0.5718 0.2000 0.078 Uiso 0.72(2) 1 calc PR A 1 H18B H 0.7985 0.5849 0.1228 0.078 Uiso 0.72(2) 1 calc PR A 1 C19 C 0.7640(3) 0.6344(3) 0.1775(10) 0.036(2) Uani 0.72(2) 1 d PDU A 1 H19A H 0.7352 0.6387 0.2019 0.043 Uiso 0.72(2) 1 calc PR A 1 H19B H 0.7816 0.6391 0.2472 0.043 Uiso 0.72(2) 1 calc PR A 1 C15B C 0.7524(12) 0.6697(7) -0.021(3) 0.028(6) Uani 0.28(2) 1 d PDU A 2 H15C H 0.7633 0.6939 -0.0631 0.034 Uiso 0.28(2) 1 calc PR A 2 H15D H 0.7234 0.6752 -0.0022 0.034 Uiso 0.28(2) 1 calc PR A 2 C16B C 0.7546(8) 0.6336(9) -0.101(2) 0.051(7) Uani 0.28(2) 1 d PDU A 2 H16C H 0.7834 0.6290 -0.1249 0.061 Uiso 0.28(2) 1 calc PR A 2 H16D H 0.7386 0.6394 -0.1736 0.061 Uiso 0.28(2) 1 calc PR A 2 C17B C 0.7379(9) 0.5950(9) -0.043(3) 0.055(8) Uani 0.28(2) 1 d PDU A 2 H17C H 0.7086 0.5990 -0.0246 0.066 Uiso 0.28(2) 1 calc PR A 2 H17D H 0.7401 0.5719 -0.0990 0.066 Uiso 0.28(2) 1 calc PR A 2 C18B C 0.7607(10) 0.5842(7) 0.070(3) 0.059(10) Uani 0.28(2) 1 d PDU A 2 H18C H 0.7473 0.5608 0.1096 0.071 Uiso 0.28(2) 1 calc PR A 2 H18D H 0.7894 0.5764 0.0517 0.071 Uiso 0.28(2) 1 calc PR A 2 C19B C 0.7599(9) 0.6212(8) 0.148(2) 0.031(7) Uani 0.28(2) 1 d PDU A 2 H19C H 0.7777 0.6159 0.2165 0.037 Uiso 0.28(2) 1 calc PR A 2 H19D H 0.7316 0.6248 0.1773 0.037 Uiso 0.28(2) 1 calc PR A 2 C20 C 0.92665(11) 0.79002(12) 0.0145(4) 0.0245(10) Uani 1 1 d . . . H20 H 0.9533 0.7844 -0.0149 0.029 Uiso 1 1 calc R . . C21 C 0.90468(11) 0.82451(12) -0.0067(3) 0.0234(9) Uani 1 1 d . . . H21 H 0.9128 0.8474 -0.0530 0.028 Uiso 1 1 calc R . . C22 C 0.86803(11) 0.81953(11) 0.0532(3) 0.0205(9) Uani 1 1 d . A . C23 C 0.83180(11) 0.84793(11) 0.0586(4) 0.0209(9) Uani 1 1 d . . . H23 H 0.8149 0.8398 0.1282 0.025 Uiso 1 1 calc R . . C24 C 0.80484(11) 0.84410(11) -0.0512(4) 0.0237(9) Uani 1 1 d . . . H24A H 0.8211 0.8512 -0.1221 0.028 Uiso 1 1 calc R . . H24B H 0.7954 0.8154 -0.0596 0.028 Uiso 1 1 calc R . . C25 C 0.76803(11) 0.87234(11) -0.0425(4) 0.0286(10) Uani 1 1 d . . . H25A H 0.7517 0.8702 -0.1156 0.034 Uiso 1 1 calc R . . H25B H 0.7505 0.8635 0.0241 0.034 Uiso 1 1 calc R . . C26 C 0.78078(12) 0.91658(11) -0.0240(4) 0.0310(11) Uani 1 1 d . . . H26A H 0.7955 0.9265 -0.0947 0.037 Uiso 1 1 calc R . . H26B H 0.7561 0.9338 -0.0131 0.037 Uiso 1 1 calc R . . C27 C 0.80833(12) 0.92065(12) 0.0830(4) 0.0289(10) Uani 1 1 d . . . H27A H 0.8182 0.9492 0.0889 0.035 Uiso 1 1 calc R . . H27B H 0.7924 0.9144 0.1550 0.035 Uiso 1 1 calc R . . C28 C 0.84460(11) 0.89212(11) 0.0760(4) 0.0251(10) Uani 1 1 d . . . H28A H 0.8608 0.8944 0.1495 0.030 Uiso 1 1 calc R . . H28B H 0.8624 0.9006 0.0096 0.030 Uiso 1 1 calc R . . C29 C 0.84909(11) 0.83777(13) 0.3708(4) 0.0232(9) Uani 1 1 d . A . C35 C 0.86870(12) 0.87363(12) 0.4211(4) 0.0321(11) Uani 1 1 d . . . H35A H 0.8979 0.8734 0.4014 0.048 Uiso 1 1 calc R . . H35B H 0.8654 0.8733 0.5070 0.048 Uiso 1 1 calc R . . H35C H 0.8560 0.8984 0.3890 0.048 Uiso 1 1 calc R . . N1 N 0.87821(9) 0.73421(9) 0.3233(3) 0.0193(7) Uani 1 1 d . . . N2 N 0.91300(9) 0.72221(9) 0.2661(3) 0.0211(8) Uani 1 1 d . . . N3 N 0.84044(9) 0.69927(9) 0.1162(3) 0.0220(8) Uani 1 1 d . . . N4 N 0.88066(9) 0.69306(9) 0.0898(3) 0.0216(8) Uani 1 1 d . A . N5 N 0.86826(9) 0.78347(9) 0.1078(3) 0.0203(7) Uani 1 1 d . . . N6 N 0.90459(9) 0.76514(9) 0.0835(3) 0.0205(8) Uani 1 1 d . A . N7 N 0.83360(10) 0.81009(10) 0.3298(3) 0.0239(8) Uani 1 1 d . . . Ni1 Ni 0.830428(14) 0.752677(14) 0.22031(5) 0.01943(14) Uani 1 1 d . . . O1 O 0.77869(7) 0.77259(7) 0.1392(2) 0.0204(6) Uani 1 1 d . . . O2 O 0.71141(7) 0.77350(7) 0.1705(2) 0.0201(6) 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 B1 0.018(3) 0.028(3) 0.028(3) 0.001(2) 0.001(2) 0.004(2) C1 0.018(2) 0.017(2) 0.015(2) -0.0003(16) 0.0006(17) 0.0036(16) C2 0.017(2) 0.017(2) 0.028(3) -0.0014(18) -0.0040(18) 0.0024(16) C3 0.021(2) 0.021(2) 0.025(3) -0.0021(18) -0.0052(18) 0.0011(17) C4 0.022(2) 0.0095(19) 0.021(2) -0.0022(16) -0.0007(17) -0.0015(16) C5 0.016(2) 0.019(2) 0.020(2) 0.0008(17) -0.0013(17) 0.0027(15) C6 0.024(2) 0.025(2) 0.019(2) -0.0001(18) 0.0017(18) -0.0026(17) C7 0.032(3) 0.030(2) 0.025(3) -0.009(2) 0.006(2) -0.0032(19) C8 0.033(3) 0.033(3) 0.032(3) -0.003(2) 0.014(2) -0.007(2) C9 0.035(3) 0.038(3) 0.034(3) -0.003(2) 0.007(2) -0.016(2) C10 0.029(2) 0.024(2) 0.023(3) -0.0035(18) 0.0005(19) -0.0023(18) C11 0.030(3) 0.035(3) 0.017(2) -0.007(2) 0.0018(19) 0.0106(19) C12 0.023(2) 0.025(2) 0.026(3) -0.0117(19) 0.0030(19) 0.0023(18) C13 0.023(2) 0.023(2) 0.022(2) -0.0022(18) -0.0015(18) 0.0001(18) C14 0.019(2) 0.022(2) 0.028(3) -0.0066(19) -0.0018(19) 0.0048(17) C15 0.022(4) 0.051(7) 0.033(5) -0.019(5) 0.001(4) 0.003(6) C16 0.037(5) 0.060(9) 0.080(9) -0.050(7) 0.011(5) -0.005(6) C17 0.033(6) 0.035(5) 0.141(16) -0.032(7) -0.008(7) 0.008(4) C18 0.045(6) 0.027(5) 0.123(12) 0.027(6) 0.039(7) 0.020(4) C19 0.022(4) 0.032(6) 0.053(6) 0.007(5) 0.006(4) 0.005(4) C15B 0.021(8) 0.033(9) 0.031(10) -0.008(8) 0.005(7) -0.002(8) C16B 0.041(9) 0.063(11) 0.049(10) -0.019(8) -0.012(7) -0.006(9) C17B 0.054(11) 0.056(12) 0.055(11) -0.011(8) 0.004(8) -0.005(8) C18B 0.055(13) 0.054(12) 0.067(13) -0.009(9) 0.001(9) 0.004(9) C19B 0.024(9) 0.035(11) 0.034(10) 0.009(8) 0.020(7) -0.002(8) C20 0.015(2) 0.043(3) 0.016(2) 0.0004(19) 0.0025(17) -0.0037(18) C21 0.024(2) 0.028(2) 0.018(2) 0.0032(18) 0.0003(18) -0.0024(18) C22 0.020(2) 0.024(2) 0.018(2) 0.0008(17) -0.0001(17) -0.0013(17) C23 0.015(2) 0.026(2) 0.022(2) 0.0008(18) -0.0007(17) -0.0011(16) C24 0.025(2) 0.022(2) 0.024(3) -0.0001(18) -0.0041(18) -0.0039(17) C25 0.025(2) 0.027(2) 0.033(3) -0.003(2) -0.009(2) -0.0007(18) C26 0.032(3) 0.024(2) 0.037(3) 0.001(2) -0.005(2) 0.0048(18) C27 0.033(3) 0.021(2) 0.032(3) -0.0048(19) -0.004(2) -0.0043(18) C28 0.025(2) 0.026(2) 0.024(2) -0.0009(19) -0.0068(18) -0.0045(18) C29 0.016(2) 0.033(3) 0.020(2) 0.005(2) 0.0036(18) 0.0087(19) C35 0.032(3) 0.033(3) 0.032(3) -0.007(2) -0.002(2) 0.000(2) N1 0.0131(17) 0.0206(18) 0.024(2) -0.0019(15) 0.0032(14) 0.0000(13) N2 0.0134(17) 0.0250(19) 0.025(2) -0.0021(15) 0.0014(15) 0.0036(14) N3 0.0178(19) 0.0247(19) 0.023(2) 0.0009(15) 0.0001(15) 0.0040(14) N4 0.0184(19) 0.028(2) 0.018(2) -0.0028(15) 0.0015(14) 0.0049(14) N5 0.0167(18) 0.026(2) 0.0180(19) -0.0003(15) 0.0004(14) 0.0024(14) N6 0.0151(18) 0.0247(19) 0.022(2) -0.0003(15) 0.0016(14) 0.0023(14) N7 0.025(2) 0.025(2) 0.021(2) 0.0030(16) 0.0010(16) 0.0069(16) Ni1 0.0166(3) 0.0227(3) 0.0191(3) 0.0003(2) 0.0012(2) 0.0024(2) O1 0.0142(14) 0.0245(15) 0.0223(17) 0.0014(12) 0.0032(12) -0.0005(11) O2 0.0156(15) 0.0278(16) 0.0170(16) 0.0020(12) 0.0007(11) 0.0019(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 B1 N6 1.523(5) . ? B1 N2 1.527(6) . ? B1 N4 1.532(5) . ? B1 H1 1.0000 . ? C1 O1 1.239(4) . ? C1 O2 1.247(4) . ? C1 C1 1.545(7) 13_665 ? C2 N2 1.340(5) . ? C2 C3 1.358(5) . ? C2 H2 0.9500 . ? C3 C4 1.400(5) . ? C3 H3 0.9500 . ? C4 N1 1.329(5) . ? C4 C5 1.489(5) . ? C5 C10 1.514(5) . ? C5 C6 1.521(5) . ? C5 H5 1.0000 . ? C6 C7 1.518(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.506(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.517(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N4 1.330(5) . ? C11 C12 1.361(5) . ? C11 H11 0.9500 . ? C12 C13 1.393(5) . ? C12 H12 0.9500 . ? C13 N3 1.346(5) . ? C13 C14 1.491(5) . ? C14 C15B 1.42(3) . ? C14 C19 1.473(10) . ? C14 C15 1.560(12) . ? C14 C19B 1.65(3) . ? C14 H14B 1.0000 . ? C14 H14 0.9800 . ? C15 C16 1.498(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.488(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.533(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.511(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C15B C16B 1.490(18) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17B 1.52(2) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B C18B 1.52(2) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B C19B 1.497(19) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20 N6 1.339(5) . ? C20 C21 1.357(5) . ? C20 H20 0.9500 . ? C21 C22 1.386(5) . ? C21 H21 0.9500 . ? C22 N5 1.331(4) . ? C22 C23 1.505(5) . ? C23 C28 1.515(5) . ? C23 C24 1.531(5) . ? C23 H23 1.0000 . ? C24 C25 1.519(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.518(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.517(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.509(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N7 1.136(5) . ? C29 C35 1.452(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N1 N2 1.366(4) . ? N1 Ni1 2.040(3) . ? N3 N4 1.362(4) . ? N3 Ni1 2.132(3) . ? N5 N6 1.357(4) . ? N5 Ni1 2.041(3) . ? N7 Ni1 2.252(4) . ? Ni1 O1 2.031(2) . ? Ni1 O2 2.033(2) 13_665 ? O2 Ni1 2.033(2) 13_665 ? 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 N6 B1 N2 111.2(3) . . ? N6 B1 N4 108.6(3) . . ? N2 B1 N4 106.7(3) . . ? N6 B1 H1 110.1 . . ? N2 B1 H1 110.1 . . ? N4 B1 H1 110.1 . . ? O1 C1 O2 127.1(3) . . ? O1 C1 C1 117.0(4) . 13_665 ? O2 C1 C1 115.8(4) . 13_665 ? N2 C2 C3 108.9(3) . . ? N2 C2 H2 125.5 . . ? C3 C2 H2 125.5 . . ? C2 C3 C4 105.5(4) . . ? C2 C3 H3 127.2 . . ? C4 C3 H3 127.2 . . ? N1 C4 C3 109.3(3) . . ? N1 C4 C5 122.4(3) . . ? C3 C4 C5 128.3(4) . . ? C4 C5 C10 112.2(3) . . ? C4 C5 C6 110.9(3) . . ? C10 C5 C6 109.7(3) . . ? C4 C5 H5 107.9 . . ? C10 C5 H5 107.9 . . ? C6 C5 H5 107.9 . . ? C7 C6 C5 112.2(3) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 111.4(3) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 111.1(4) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 111.5(3) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C5 C10 C9 111.8(3) . . ? C5 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C5 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? N4 C11 C12 109.2(3) . . ? N4 C11 H11 125.4 . . ? C12 C11 H11 125.4 . . ? C11 C12 C13 105.3(3) . . ? C11 C12 H12 127.3 . . ? C13 C12 H12 127.3 . . ? N3 C13 C12 109.4(3) . . ? N3 C13 C14 120.1(3) . . ? C12 C13 C14 130.4(4) . . ? C15B C14 C13 113.1(15) . . ? C19 C14 C13 111.2(5) . . ? C19 C14 C15 111.4(6) . . ? C13 C14 C15 113.4(6) . . ? C15B C14 C19B 108.6(13) . . ? C13 C14 C19B 113.4(11) . . ? C15B C14 H14B 107.1 . . ? C19 C14 H14B 89.8 . . ? C13 C14 H14B 107.1 . . ? C15 C14 H14B 121.6 . . ? C19 C14 H14 106.6 . . ? C13 C14 H14 106.9 . . ? C15 C14 H14 107.0 . . ? C19B C14 H14 122.0 . . ? C16 C15 C14 115.3(8) . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C17 C16 C15 111.3(8) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 115.2(7) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 110.3(7) . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C14 C19 C18 113.1(8) . . ? C14 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C14 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C14 C15B C16B 114(2) . . ? C14 C15B H15C 108.8 . . ? C16B C15B H15C 108.8 . . ? C14 C15B H15D 108.8 . . ? C16B C15B H15D 108.8 . . ? H15C C15B H15D 107.7 . . ? C15B C16B C17B 111.8(18) . . ? C15B C16B H16C 109.2 . . ? C17B C16B H16C 109.2 . . ? C15B C16B H16D 109.2 . . ? C17B C16B H16D 109.3 . . ? H16C C16B H16D 107.9 . . ? C18B C17B C16B 112.5(18) . . ? C18B C17B H17C 109.1 . . ? C16B C17B H17C 109.1 . . ? C18B C17B H17D 109.1 . . ? C16B C17B H17D 109.1 . . ? H17C C17B H17D 107.8 . . ? C19B C18B C17B 107.3(18) . . ? C19B C18B H18C 110.3 . . ? C17B C18B H18C 110.2 . . ? C19B C18B H18D 110.2 . . ? C17B C18B H18D 110.2 . . ? H18C C18B H18D 108.5 . . ? C18B C19B C14 115.8(19) . . ? C18B C19B H19C 108.3 . . ? C14 C19B H19C 108.3 . . ? C18B C19B H19D 108.3 . . ? C14 C19B H19D 108.3 . . ? H19C C19B H19D 107.4 . . ? N6 C20 C21 108.8(3) . . ? N6 C20 H20 125.6 . . ? C21 C20 H20 125.6 . . ? C20 C21 C22 105.8(4) . . ? C20 C21 H21 127.1 . . ? C22 C21 H21 127.1 . . ? N5 C22 C21 109.1(3) . . ? N5 C22 C23 122.1(3) . . ? C21 C22 C23 128.8(4) . . ? C22 C23 C28 112.1(3) . . ? C22 C23 C24 111.6(3) . . ? C28 C23 C24 110.0(3) . . ? C22 C23 H23 107.6 . . ? C28 C23 H23 107.6 . . ? C24 C23 H23 107.6 . . ? C25 C24 C23 110.6(3) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 111.7(3) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 110.9(3) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.7(3) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C23 112.2(3) . . ? C27 C28 H28A 109.2 . . ? C23 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C23 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? N7 C29 C35 178.8(5) . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C4 N1 N2 107.1(3) . . ? C4 N1 Ni1 135.7(3) . . ? N2 N1 Ni1 116.7(2) . . ? C2 N2 N1 109.1(3) . . ? C2 N2 B1 130.8(3) . . ? N1 N2 B1 119.4(3) . . ? C13 N3 N4 106.4(3) . . ? C13 N3 Ni1 140.4(3) . . ? N4 N3 Ni1 113.1(2) . . ? C11 N4 N3 109.6(3) . . ? C11 N4 B1 128.8(3) . . ? N3 N4 B1 121.6(3) . . ? C22 N5 N6 107.5(3) . . ? C22 N5 Ni1 136.4(2) . . ? N6 N5 Ni1 116.1(2) . . ? C20 N6 N5 108.8(3) . . ? C20 N6 B1 130.8(3) . . ? N5 N6 B1 120.4(3) . . ? C29 N7 Ni1 155.4(3) . . ? O1 Ni1 O2 81.47(10) . 13_665 ? O1 Ni1 N1 172.01(12) . . ? O2 Ni1 N1 92.34(11) 13_665 . ? O1 Ni1 N5 93.59(11) . . ? O2 Ni1 N5 174.30(11) 13_665 . ? N1 Ni1 N5 92.33(12) . . ? O1 Ni1 N3 97.97(11) . . ? O2 Ni1 N3 95.55(11) 13_665 . ? N1 Ni1 N3 87.59(12) . . ? N5 Ni1 N3 87.93(12) . . ? O1 Ni1 N7 91.23(11) . . ? O2 Ni1 N7 92.57(11) 13_665 . ? N1 Ni1 N7 83.98(11) . . ? N5 Ni1 N7 84.65(12) . . ? N3 Ni1 N7 168.52(12) . . ? C1 O1 Ni1 112.5(2) . . ? C1 O2 Ni1 112.8(2) . 13_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 C4 0.1(4) . . . . ? C2 C3 C4 N1 0.7(4) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? N1 C4 C5 C10 109.9(4) . . . . ? C3 C4 C5 C10 -70.9(5) . . . . ? N1 C4 C5 C6 -127.0(4) . . . . ? C3 C4 C5 C6 52.2(5) . . . . ? C4 C5 C6 C7 -179.7(3) . . . . ? C10 C5 C6 C7 -55.1(4) . . . . ? C5 C6 C7 C8 54.9(5) . . . . ? C6 C7 C8 C9 -54.1(5) . . . . ? C7 C8 C9 C10 55.0(5) . . . . ? C4 C5 C10 C9 179.5(3) . . . . ? C6 C5 C10 C9 55.7(4) . . . . ? C8 C9 C10 C5 -56.6(5) . . . . ? N4 C11 C12 C13 0.3(5) . . . . ? C11 C12 C13 N3 -0.3(5) . . . . ? C11 C12 C13 C14 -178.4(4) . . . . ? N3 C13 C14 C15B 112.1(11) . . . . ? C12 C13 C14 C15B -70.0(12) . . . . ? N3 C13 C14 C19 -102.4(7) . . . . ? C12 C13 C14 C19 75.6(8) . . . . ? N3 C13 C14 C15 131.2(6) . . . . ? C12 C13 C14 C15 -50.8(7) . . . . ? N3 C13 C14 C19B -123.7(10) . . . . ? C12 C13 C14 C19B 54.2(11) . . . . ? C15B C14 C15 C16 170(7) . . . . ? C19 C14 C15 C16 -49.1(12) . . . . ? C13 C14 C15 C16 77.3(10) . . . . ? C19B C14 C15 C16 -40.1(13) . . . . ? C14 C15 C16 C17 46.2(13) . . . . ? C15 C16 C17 C18 -48.8(12) . . . . ? C16 C17 C18 C19 52.9(10) . . . . ? C15B C14 C19 C18 66.1(17) . . . . ? C13 C14 C19 C18 -74.8(8) . . . . ? C15 C14 C19 C18 52.7(10) . . . . ? C19B C14 C19 C18 25(4) . . . . ? C17 C18 C19 C14 -54.7(10) . . . . ? C19 C14 C15B C16B -66(3) . . . . ? C13 C14 C15B C16B 75(2) . . . . ? C15 C14 C15B C16B -20(4) . . . . ? C19B C14 C15B C16B -52(3) . . . . ? C14 C15B C16B C17B 59(3) . . . . ? C15B C16B C17B C18B -58(3) . . . . ? C16B C17B C18B C19B 54(3) . . . . ? C17B C18B C19B C14 -51(3) . . . . ? C15B C14 C19B C18B 51(3) . . . . ? C19 C14 C19B C18B -163(6) . . . . ? C13 C14 C19B C18B -75(2) . . . . ? C15 C14 C19B C18B 42(2) . . . . ? N6 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 N5 0.0(4) . . . . ? C20 C21 C22 C23 -178.6(4) . . . . ? N5 C22 C23 C28 137.7(4) . . . . ? C21 C22 C23 C28 -43.8(6) . . . . ? N5 C22 C23 C24 -98.3(4) . . . . ? C21 C22 C23 C24 80.2(5) . . . . ? C22 C23 C24 C25 178.7(3) . . . . ? C28 C23 C24 C25 -56.2(4) . . . . ? C23 C24 C25 C26 56.6(4) . . . . ? C24 C25 C26 C27 -55.2(5) . . . . ? C25 C26 C27 C28 53.9(5) . . . . ? C26 C27 C28 C23 -55.2(5) . . . . ? C22 C23 C28 C27 -179.3(3) . . . . ? C24 C23 C28 C27 55.9(4) . . . . ? C3 C4 N1 N2 -1.3(4) . . . . ? C5 C4 N1 N2 178.1(3) . . . . ? C3 C4 N1 Ni1 170.4(3) . . . . ? C5 C4 N1 Ni1 -10.2(5) . . . . ? C3 C2 N2 N1 -0.9(4) . . . . ? C3 C2 N2 B1 -170.9(4) . . . . ? C4 N1 N2 C2 1.4(4) . . . . ? Ni1 N1 N2 C2 -172.2(2) . . . . ? C4 N1 N2 B1 172.7(3) . . . . ? Ni1 N1 N2 B1 -0.9(4) . . . . ? N6 B1 N2 C2 -133.5(4) . . . . ? N4 B1 N2 C2 108.2(4) . . . . ? N6 B1 N2 N1 57.4(4) . . . . ? N4 B1 N2 N1 -60.9(4) . . . . ? C12 C13 N3 N4 0.2(4) . . . . ? C14 C13 N3 N4 178.6(3) . . . . ? C12 C13 N3 Ni1 -176.3(3) . . . . ? C14 C13 N3 Ni1 2.0(6) . . . . ? C12 C11 N4 N3 -0.1(5) . . . . ? C12 C11 N4 B1 177.9(4) . . . . ? C13 N3 N4 C11 -0.1(4) . . . . ? Ni1 N3 N4 C11 177.6(3) . . . . ? C13 N3 N4 B1 -178.3(4) . . . . ? Ni1 N3 N4 B1 -0.6(4) . . . . ? N6 B1 N4 C11 123.5(4) . . . . ? N2 B1 N4 C11 -116.5(4) . . . . ? N6 B1 N4 N3 -58.7(5) . . . . ? N2 B1 N4 N3 61.3(4) . . . . ? C21 C22 N5 N6 -0.2(4) . . . . ? C23 C22 N5 N6 178.6(3) . . . . ? C21 C22 N5 Ni1 175.7(3) . . . . ? C23 C22 N5 Ni1 -5.6(6) . . . . ? C21 C20 N6 N5 -0.3(4) . . . . ? C21 C20 N6 B1 178.7(4) . . . . ? C22 N5 N6 C20 0.3(4) . . . . ? Ni1 N5 N6 C20 -176.5(2) . . . . ? C22 N5 N6 B1 -178.8(3) . . . . ? Ni1 N5 N6 B1 4.4(4) . . . . ? N2 B1 N6 C20 121.2(4) . . . . ? N4 B1 N6 C20 -121.6(4) . . . . ? N2 B1 N6 N5 -59.9(4) . . . . ? N4 B1 N6 N5 57.2(5) . . . . ? C4 N1 Ni1 O2 -28.5(4) . . . 13_665 ? N2 N1 Ni1 O2 142.6(2) . . . 13_665 ? C4 N1 Ni1 N5 148.2(4) . . . . ? N2 N1 Ni1 N5 -40.7(2) . . . . ? C4 N1 Ni1 N3 -124.0(4) . . . . ? N2 N1 Ni1 N3 47.2(2) . . . . ? C4 N1 Ni1 N7 63.8(4) . . . . ? N2 N1 Ni1 N7 -125.0(2) . . . . ? C22 N5 Ni1 O1 37.8(4) . . . . ? N6 N5 Ni1 O1 -146.6(2) . . . . ? C22 N5 Ni1 N1 -136.9(4) . . . . ? N6 N5 Ni1 N1 38.8(3) . . . . ? C22 N5 Ni1 N3 135.6(4) . . . . ? N6 N5 Ni1 N3 -48.7(3) . . . . ? C22 N5 Ni1 N7 -53.1(4) . . . . ? N6 N5 Ni1 N7 122.5(3) . . . . ? C13 N3 Ni1 O1 -43.8(4) . . . . ? N4 N3 Ni1 O1 139.8(2) . . . . ? C13 N3 Ni1 O2 38.3(4) . . . 13_665 ? N4 N3 Ni1 O2 -138.1(2) . . . 13_665 ? C13 N3 Ni1 N1 130.4(4) . . . . ? N4 N3 Ni1 N1 -46.0(2) . . . . ? C13 N3 Ni1 N5 -137.1(4) . . . . ? N4 N3 Ni1 N5 46.4(2) . . . . ? C13 N3 Ni1 N7 173.2(5) . . . . ? N4 N3 Ni1 N7 -3.3(8) . . . . ? C29 N7 Ni1 O1 -132.7(8) . . . . ? C29 N7 Ni1 O2 145.8(8) . . . 13_665 ? C29 N7 Ni1 N1 53.7(8) . . . . ? C29 N7 Ni1 N5 -39.2(8) . . . . ? C29 N7 Ni1 N3 10.8(12) . . . . ? O2 C1 O1 Ni1 175.3(3) . . . . ? C1 C1 O1 Ni1 -4.5(5) 13_665 . . . ? O2 Ni1 O1 C1 5.4(2) 13_665 . . . ? N5 Ni1 O1 C1 -171.8(2) . . . . ? N3 Ni1 O1 C1 99.8(2) . . . . ? N7 Ni1 O1 C1 -87.1(2) . . . . ? O1 C1 O2 Ni1 175.5(3) . . . 13_665 ? C1 C1 O2 Ni1 -4.7(5) 13_665 . . 13_665 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.606 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.088 data_09mz295_0m _database_code_depnum_ccdc_archive 'CCDC 881840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H82 B2 Co2 N14 O2' _chemical_formula_weight 1050.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.6000(14) _cell_length_b 18.5456(11) _cell_length_c 12.3149(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.0550(10) _cell_angle_gamma 90.00 _cell_volume 5618.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7914 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 31.23 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The oxygen atom and the amide unit are disordered with each other in a one to one ratio. Atoms on the same position were constrained to have exactly the same position and ADP. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21788 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6987 _reflns_number_gt 5849 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0380P)^2^+4.4064P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6987 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.23486(7) 0.32814(9) 0.72645(14) 0.0244(3) Uani 1 1 d . A . H1A H 0.2748 0.3330 0.7133 0.029 Uiso 1 1 calc R . . C1 C 0.25889(6) 0.21735(9) 0.84638(12) 0.0263(3) Uani 1 1 d . A . H1 H 0.2973 0.2214 0.8429 0.032 Uiso 1 1 calc R . . C2 C 0.23063(6) 0.16764(9) 0.90703(12) 0.0272(3) Uani 1 1 d . . . H2 H 0.2453 0.1312 0.9527 0.033 Uiso 1 1 calc R . . C3 C 0.17566(6) 0.18226(7) 0.88697(11) 0.0222(3) Uani 1 1 d . . . C4 C 0.12633(6) 0.14424(8) 0.92925(12) 0.0251(3) Uani 1 1 d . . . H4A H 0.0941 0.1743 0.9130 0.030 Uiso 1 1 calc R . . H4B H 0.1295 0.1408 1.0092 0.030 Uiso 1 1 calc R . . C5 C 0.11615(6) 0.06744(8) 0.88346(12) 0.0265(3) Uani 1 1 d . . . C6 C 0.05986(7) 0.04353(10) 0.92231(17) 0.0410(4) Uani 1 1 d . . . H6A H 0.0323 0.0771 0.8948 0.061 Uiso 1 1 calc R . . H6B H 0.0590 0.0433 1.0019 0.061 Uiso 1 1 calc R . . H6C H 0.0522 -0.0051 0.8951 0.061 Uiso 1 1 calc R . . C7 C 0.15885(7) 0.01384(9) 0.92404(15) 0.0336(4) Uani 1 1 d . . . H7A H 0.1585 0.0128 1.0036 0.050 Uiso 1 1 calc R . . H7D H 0.1949 0.0288 0.8987 0.050 Uiso 1 1 calc R . . H7C H 0.1505 -0.0343 0.8958 0.050 Uiso 1 1 calc R . . C8 C 0.11681(8) 0.06861(10) 0.75939(13) 0.0389(4) Uani 1 1 d . . . H8A H 0.1084 0.0203 0.7316 0.058 Uiso 1 1 calc R . . H8B H 0.1529 0.0833 0.7340 0.058 Uiso 1 1 calc R . . H8C H 0.0895 0.1029 0.7330 0.058 Uiso 1 1 calc R . . C9 C 0.24182(6) 0.44788(8) 0.83637(13) 0.0274(3) Uani 1 1 d . A . H9 H 0.2791 0.4587 0.8240 0.033 Uiso 1 1 calc R . . C10 C 0.20724(7) 0.48610(8) 0.90196(13) 0.0285(3) Uani 1 1 d . . . H10 H 0.2156 0.5278 0.9435 0.034 Uiso 1 1 calc R . . C11 C 0.15697(6) 0.45068(7) 0.89480(11) 0.0230(3) Uani 1 1 d . . . C12 C 0.10530(6) 0.46791(8) 0.95315(12) 0.0263(3) Uani 1 1 d . . . H12A H 0.0743 0.4546 0.9059 0.032 Uiso 1 1 calc R . . H12B H 0.1036 0.5206 0.9652 0.032 Uiso 1 1 calc R . . C13 C 0.09849(7) 0.42956(9) 1.06357(12) 0.0302(3) Uani 1 1 d . . . C14 C 0.10376(8) 0.34808(9) 1.04870(13) 0.0349(4) Uani 1 1 d . . . H14A H 0.1403 0.3366 1.0221 0.052 Uiso 1 1 calc R . . H14B H 0.0766 0.3314 0.9960 0.052 Uiso 1 1 calc R . . H14C H 0.0977 0.3240 1.1185 0.052 Uiso 1 1 calc R . . C15 C 0.04188(8) 0.44700(12) 1.10760(16) 0.0469(5) Uani 1 1 d . . . H15A H 0.0371 0.4239 1.1786 0.070 Uiso 1 1 calc R . . H15B H 0.0143 0.4289 1.0571 0.070 Uiso 1 1 calc R . . H15C H 0.0380 0.4993 1.1154 0.070 Uiso 1 1 calc R . . C16 C 0.14119(8) 0.45592(12) 1.14489(15) 0.0461(5) Uani 1 1 d . . . H16A H 0.1356 0.4319 1.2149 0.069 Uiso 1 1 calc R . . H16B H 0.1377 0.5082 1.1542 0.069 Uiso 1 1 calc R . . H16C H 0.1776 0.4445 1.1176 0.069 Uiso 1 1 calc R . . C17 C 0.22379(6) 0.33071(8) 0.51605(12) 0.0267(3) Uani 1 1 d . A . H17 H 0.2608 0.3378 0.4972 0.032 Uiso 1 1 calc R . . C18 C 0.18132(7) 0.32488(8) 0.44403(12) 0.0277(3) Uani 1 1 d . . . H18 H 0.1830 0.3274 0.3671 0.033 Uiso 1 1 calc R . . C19 C 0.13498(6) 0.31439(8) 0.50816(12) 0.0233(3) Uani 1 1 d . . . C20 C 0.07770(6) 0.30007(8) 0.47383(12) 0.0259(3) Uani 1 1 d . . . H20A H 0.0679 0.3344 0.4155 0.031 Uiso 1 1 calc R . . H20B H 0.0534 0.3096 0.5362 0.031 Uiso 1 1 calc R . . C21 C 0.06701(6) 0.22230(9) 0.43243(11) 0.0253(3) Uani 1 1 d . . . C22 C 0.09681(7) 0.20826(11) 0.32564(13) 0.0346(4) Uani 1 1 d . . . H22A H 0.1361 0.2111 0.3378 0.052 Uiso 1 1 calc R . . H22B H 0.0860 0.2446 0.2720 0.052 Uiso 1 1 calc R . . H22C H 0.0874 0.1601 0.2987 0.052 Uiso 1 1 calc R . . C23 C 0.08532(7) 0.16738(9) 0.51728(13) 0.0312(3) Uani 1 1 d . . . H23A H 0.0759 0.1187 0.4926 0.047 Uiso 1 1 calc R . . H23B H 0.0670 0.1773 0.5863 0.047 Uiso 1 1 calc R . . H23C H 0.1248 0.1709 0.5273 0.047 Uiso 1 1 calc R . . C24 C 0.00587(7) 0.21452(11) 0.41337(14) 0.0363(4) Uani 1 1 d . . . H24A H -0.0018 0.1668 0.3829 0.054 Uiso 1 1 calc R . . H24B H -0.0064 0.2518 0.3625 0.054 Uiso 1 1 calc R . . H24C H -0.0134 0.2200 0.4825 0.054 Uiso 1 1 calc R . . C25 C 0.0000 0.35142(10) 0.7500 0.0202(4) Uani 1 2 d S . . C26 C 0.0000 0.26862(10) 0.7500 0.0188(4) Uani 1 2 d S . . Co1 Co 0.110949(8) 0.310885(10) 0.763726(15) 0.01902(6) Uani 1 1 d . . . N1 N 0.22328(5) 0.25930(7) 0.79292(10) 0.0222(2) Uani 1 1 d . . . N2 N 0.17122(5) 0.23850(6) 0.81827(10) 0.0210(2) Uani 1 1 d . A . N3 N 0.21413(5) 0.39250(7) 0.79251(10) 0.0233(3) Uani 1 1 d . . . N4 N 0.16149(5) 0.39385(6) 0.82779(9) 0.0211(2) Uani 1 1 d . A . N5 N 0.20427(5) 0.32465(7) 0.61745(10) 0.0232(3) Uani 1 1 d . . . N6 N 0.14924(5) 0.31498(6) 0.61390(10) 0.0222(2) Uani 1 1 d . A . N7 N 0.04661(4) 0.38117(6) 0.75148(9) 0.0220(2) Uani 0.50 1 d P A 1 H7 H 0.0510 0.4282 0.7476 0.026 Uiso 0.50 1 calc PR A 1 O1 O 0.04584(4) 0.23862(5) 0.76106(8) 0.0183(2) Uani 0.50 1 d P A 1 N7B N 0.04584(4) 0.23862(5) 0.76106(8) 0.0183(2) Uani 0.50 1 d P A 2 H7B H 0.0499 0.1917 0.7671 0.022 Uiso 0.50 1 calc PR A 2 O1B O 0.04661(4) 0.38117(6) 0.75148(9) 0.0220(2) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0168(8) 0.0289(9) 0.0275(8) 0.0061(6) -0.0008(6) -0.0033(6) C1 0.0180(7) 0.0329(8) 0.0279(7) 0.0041(6) -0.0029(6) 0.0021(6) C2 0.0254(8) 0.0289(8) 0.0274(7) 0.0072(6) -0.0027(6) 0.0024(6) C3 0.0243(7) 0.0207(7) 0.0214(6) 0.0011(5) 0.0004(5) 0.0012(5) C4 0.0250(8) 0.0231(7) 0.0271(7) 0.0037(6) 0.0028(6) -0.0011(6) C5 0.0277(8) 0.0214(7) 0.0305(7) 0.0049(6) -0.0025(6) -0.0012(6) C6 0.0305(9) 0.0290(9) 0.0634(12) 0.0081(8) -0.0009(8) -0.0046(7) C7 0.0326(9) 0.0241(8) 0.0440(9) 0.0060(7) -0.0055(7) 0.0010(7) C8 0.0582(12) 0.0280(9) 0.0304(8) 0.0000(7) -0.0089(8) 0.0002(8) C9 0.0241(8) 0.0252(8) 0.0329(8) 0.0093(6) -0.0086(6) -0.0093(6) C10 0.0311(8) 0.0194(7) 0.0350(8) 0.0028(6) -0.0112(6) -0.0060(6) C11 0.0262(8) 0.0173(7) 0.0256(7) 0.0048(5) -0.0094(6) -0.0012(5) C12 0.0276(8) 0.0189(7) 0.0324(8) -0.0027(6) -0.0079(6) 0.0032(6) C13 0.0339(9) 0.0320(8) 0.0249(7) -0.0073(6) -0.0016(6) 0.0049(7) C14 0.0452(10) 0.0317(9) 0.0279(8) 0.0059(6) 0.0060(7) 0.0007(7) C15 0.0418(11) 0.0562(13) 0.0427(10) -0.0114(9) 0.0066(8) 0.0106(9) C16 0.0500(12) 0.0570(12) 0.0313(9) -0.0178(8) -0.0113(8) 0.0105(9) C17 0.0249(8) 0.0262(7) 0.0290(7) 0.0068(6) 0.0048(6) -0.0033(6) C18 0.0316(9) 0.0273(8) 0.0242(7) 0.0073(6) 0.0013(6) -0.0028(6) C19 0.0258(8) 0.0210(7) 0.0231(7) 0.0047(5) -0.0015(6) 0.0014(6) C20 0.0254(8) 0.0280(8) 0.0243(7) 0.0053(6) -0.0044(6) 0.0038(6) C21 0.0227(7) 0.0324(8) 0.0207(6) -0.0008(6) -0.0041(5) 0.0005(6) C22 0.0291(9) 0.0510(10) 0.0238(7) -0.0049(7) -0.0012(6) -0.0026(7) C23 0.0406(10) 0.0263(8) 0.0266(7) -0.0019(6) -0.0054(7) 0.0010(7) C24 0.0251(8) 0.0494(11) 0.0344(8) -0.0050(8) -0.0032(7) -0.0017(7) C25 0.0237(10) 0.0179(9) 0.0188(9) 0.000 -0.0054(7) 0.000 C26 0.0209(10) 0.0171(9) 0.0185(8) 0.000 -0.0008(7) 0.000 Co1 0.01596(10) 0.01911(10) 0.02199(10) 0.00141(7) -0.00175(7) -0.00181(7) N1 0.0162(6) 0.0250(6) 0.0255(6) 0.0044(5) -0.0010(5) -0.0010(5) N2 0.0169(6) 0.0208(6) 0.0253(6) 0.0027(5) 0.0002(4) -0.0024(4) N3 0.0185(6) 0.0252(6) 0.0261(6) 0.0056(5) -0.0029(5) -0.0050(5) N4 0.0185(6) 0.0208(6) 0.0240(6) 0.0039(5) -0.0033(5) -0.0020(5) N5 0.0193(6) 0.0246(6) 0.0257(6) 0.0047(5) 0.0002(5) -0.0028(5) N6 0.0181(6) 0.0232(6) 0.0252(6) 0.0036(5) -0.0018(5) -0.0010(5) N7 0.0188(5) 0.0156(5) 0.0317(6) 0.0007(4) -0.0054(4) -0.0027(4) O1 0.0141(5) 0.0137(5) 0.0272(5) 0.0012(4) -0.0022(4) 0.0015(4) N7B 0.0141(5) 0.0137(5) 0.0272(5) 0.0012(4) -0.0022(4) 0.0015(4) O1B 0.0188(5) 0.0156(5) 0.0317(6) 0.0007(4) -0.0054(4) -0.0027(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N3 1.532(2) . ? B1 N5 1.539(2) . ? B1 N1 1.543(2) . ? B1 H1A 1.0000 . ? C1 N1 1.3435(19) . ? C1 C2 1.376(2) . ? C1 H1 0.9500 . ? C2 C3 1.401(2) . ? C2 H2 0.9500 . ? C3 N2 1.3472(18) . ? C3 C4 1.497(2) . ? C4 C5 1.552(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.528(2) . ? C5 C7 1.530(2) . ? C5 C6 1.531(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7D 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N3 1.3454(19) . ? C9 C10 1.371(2) . ? C9 H9 0.9500 . ? C10 C11 1.403(2) . ? C10 H10 0.9500 . ? C11 N4 1.3433(19) . ? C11 C12 1.495(2) . ? C12 C13 1.544(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.528(2) . ? C13 C15 1.530(2) . ? C13 C16 1.531(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N5 1.3431(19) . ? C17 C18 1.374(2) . ? C17 H17 0.9500 . ? C18 C19 1.401(2) . ? C18 H18 0.9500 . ? C19 N6 1.3483(18) . ? C19 C20 1.494(2) . ? C20 C21 1.552(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C23 1.527(2) . ? C21 C22 1.529(2) . ? C21 C24 1.529(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O1B 1.2725(13) 2_556 ? C25 N7 1.2725(13) 2_556 ? C25 N7 1.2725(13) . ? C25 C26 1.536(3) . ? C26 O1 1.2647(13) . ? C26 N7B 1.2648(13) 2_556 ? C26 O1 1.2648(13) 2_556 ? Co1 N7 2.0558(11) . ? Co1 N6 2.0739(12) . ? Co1 O1 2.0886(10) . ? Co1 N2 2.1094(12) . ? Co1 N4 2.1293(12) . ? N1 N2 1.3738(16) . ? N3 N4 1.3663(17) . ? N5 N6 1.3662(17) . ? N7 H7 0.8800 . ? 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 N3 B1 N5 109.46(12) . . ? N3 B1 N1 107.52(12) . . ? N5 B1 N1 109.72(12) . . ? N3 B1 H1A 110.0 . . ? N5 B1 H1A 110.0 . . ? N1 B1 H1A 110.0 . . ? N1 C1 C2 108.93(13) . . ? N1 C1 H1 125.5 . . ? C2 C1 H1 125.5 . . ? C1 C2 C3 105.23(13) . . ? C1 C2 H2 127.4 . . ? C3 C2 H2 127.4 . . ? N2 C3 C2 109.77(13) . . ? N2 C3 C4 121.17(13) . . ? C2 C3 C4 129.05(13) . . ? C3 C4 C5 115.87(12) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? C5 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C8 C5 C7 109.14(14) . . ? C8 C5 C6 109.09(14) . . ? C7 C5 C6 109.31(13) . . ? C8 C5 C4 110.39(12) . . ? C7 C5 C4 111.54(13) . . ? C6 C5 C4 107.33(13) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7D 109.5 . . ? H7A C7 H7D 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7D C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 108.48(14) . . ? N3 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? C9 C10 C11 105.56(14) . . ? C9 C10 H10 127.2 . . ? C11 C10 H10 127.2 . . ? N4 C11 C10 109.42(14) . . ? N4 C11 C12 122.26(13) . . ? C10 C11 C12 128.28(14) . . ? C11 C12 C13 114.70(12) . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? C11 C12 H12B 108.6 . . ? C13 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C15 109.21(15) . . ? C14 C13 C16 109.64(15) . . ? C15 C13 C16 108.96(14) . . ? C14 C13 C12 109.92(12) . . ? C15 C13 C12 108.32(14) . . ? C16 C13 C12 110.75(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 108.74(14) . . ? N5 C17 H17 125.6 . . ? C18 C17 H17 125.6 . . ? C17 C18 C19 105.41(13) . . ? C17 C18 H18 127.3 . . ? C19 C18 H18 127.3 . . ? N6 C19 C18 109.40(13) . . ? N6 C19 C20 121.26(13) . . ? C18 C19 C20 129.25(13) . . ? C19 C20 C21 114.68(12) . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C23 C21 C22 109.50(14) . . ? C23 C21 C24 109.37(14) . . ? C22 C21 C24 108.92(13) . . ? C23 C21 C20 110.20(12) . . ? C22 C21 C20 111.08(13) . . ? C24 C21 C20 107.73(13) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1B C25 N7 128.62(18) 2_556 . ? N7 C25 N7 128.62(18) 2_556 . ? O1B C25 C26 115.69(9) 2_556 . ? N7 C25 C26 115.69(9) 2_556 . ? N7 C25 C26 115.69(9) . . ? O1 C26 N7B 127.80(18) . 2_556 ? O1 C26 O1 127.80(18) . 2_556 ? O1 C26 C25 116.10(9) . . ? N7B C26 C25 116.10(9) 2_556 . ? O1 C26 C25 116.10(9) 2_556 . ? N7 Co1 N6 105.18(5) . . ? N7 Co1 O1 79.36(4) . . ? N6 Co1 O1 111.01(4) . . ? N7 Co1 N2 165.40(5) . . ? N6 Co1 N2 89.25(5) . . ? O1 Co1 N2 97.78(4) . . ? N7 Co1 N4 91.05(4) . . ? N6 Co1 N4 92.16(5) . . ? O1 Co1 N4 156.49(4) . . ? N2 Co1 N4 86.10(5) . . ? C1 N1 N2 109.49(12) . . ? C1 N1 B1 128.19(13) . . ? N2 N1 B1 121.70(11) . . ? C3 N2 N1 106.56(11) . . ? C3 N2 Co1 138.52(10) . . ? N1 N2 Co1 113.83(8) . . ? C9 N3 N4 109.75(13) . . ? C9 N3 B1 129.74(13) . . ? N4 N3 B1 119.94(12) . . ? C11 N4 N3 106.79(11) . . ? C11 N4 Co1 138.24(10) . . ? N3 N4 Co1 114.97(9) . . ? C17 N5 N6 109.65(12) . . ? C17 N5 B1 129.22(13) . . ? N6 N5 B1 121.12(12) . . ? C19 N6 N5 106.79(12) . . ? C19 N6 Co1 137.81(10) . . ? N5 N6 Co1 115.29(9) . . ? C25 N7 Co1 114.82(10) . . ? C25 N7 H7 122.6 . . ? Co1 N7 H7 122.6 . . ? C26 O1 Co1 113.77(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.09(18) . . . . ? C1 C2 C3 N2 -0.51(18) . . . . ? C1 C2 C3 C4 178.54(15) . . . . ? N2 C3 C4 C5 108.44(16) . . . . ? C2 C3 C4 C5 -70.5(2) . . . . ? C3 C4 C5 C8 -52.30(18) . . . . ? C3 C4 C5 C7 69.21(17) . . . . ? C3 C4 C5 C6 -171.08(13) . . . . ? N3 C9 C10 C11 -0.21(16) . . . . ? C9 C10 C11 N4 -0.01(16) . . . . ? C9 C10 C11 C12 177.53(14) . . . . ? N4 C11 C12 C13 87.44(17) . . . . ? C10 C11 C12 C13 -89.82(18) . . . . ? C11 C12 C13 C14 -55.52(18) . . . . ? C11 C12 C13 C15 -174.78(14) . . . . ? C11 C12 C13 C16 65.79(17) . . . . ? N5 C17 C18 C19 -0.42(17) . . . . ? C17 C18 C19 N6 0.82(17) . . . . ? C17 C18 C19 C20 -175.78(15) . . . . ? N6 C19 C20 C21 -101.28(16) . . . . ? C18 C19 C20 C21 74.97(19) . . . . ? C19 C20 C21 C23 54.38(17) . . . . ? C19 C20 C21 C22 -67.15(16) . . . . ? C19 C20 C21 C24 173.64(13) . . . . ? O1B C25 C26 O1 -174.02(7) 2_556 . . . ? N7 C25 C26 O1 -174.02(7) 2_556 . . . ? N7 C25 C26 O1 5.98(7) . . . . ? O1B C25 C26 N7B 5.98(7) 2_556 . . 2_556 ? N7 C25 C26 N7B 5.98(7) 2_556 . . 2_556 ? N7 C25 C26 N7B -174.02(7) . . . 2_556 ? O1B C25 C26 O1 5.98(7) 2_556 . . 2_556 ? N7 C25 C26 O1 5.98(7) 2_556 . . 2_556 ? N7 C25 C26 O1 -174.02(7) . . . 2_556 ? C2 C1 N1 N2 0.64(18) . . . . ? C2 C1 N1 B1 171.64(15) . . . . ? N3 B1 N1 C1 -107.22(16) . . . . ? N5 B1 N1 C1 133.81(15) . . . . ? N3 B1 N1 N2 62.79(17) . . . . ? N5 B1 N1 N2 -56.17(18) . . . . ? C2 C3 N2 N1 0.89(16) . . . . ? C4 C3 N2 N1 -178.24(12) . . . . ? C2 C3 N2 Co1 -165.68(12) . . . . ? C4 C3 N2 Co1 15.2(2) . . . . ? C1 N1 N2 C3 -0.95(16) . . . . ? B1 N1 N2 C3 -172.64(13) . . . . ? C1 N1 N2 Co1 169.37(10) . . . . ? B1 N1 N2 Co1 -2.32(16) . . . . ? N7 Co1 N2 C3 40.9(3) . . . . ? N6 Co1 N2 C3 -147.75(15) . . . . ? O1 Co1 N2 C3 -36.65(15) . . . . ? N4 Co1 N2 C3 120.04(15) . . . . ? N7 Co1 N2 N1 -124.96(16) . . . . ? N6 Co1 N2 N1 46.34(10) . . . . ? O1 Co1 N2 N1 157.44(9) . . . . ? N4 Co1 N2 N1 -45.88(10) . . . . ? C10 C9 N3 N4 0.36(16) . . . . ? C10 C9 N3 B1 -170.81(14) . . . . ? N5 B1 N3 C9 -125.02(15) . . . . ? N1 B1 N3 C9 115.85(16) . . . . ? N5 B1 N3 N4 64.58(16) . . . . ? N1 B1 N3 N4 -54.55(16) . . . . ? C10 C11 N4 N3 0.23(15) . . . . ? C12 C11 N4 N3 -177.50(12) . . . . ? C10 C11 N4 Co1 -178.65(11) . . . . ? C12 C11 N4 Co1 3.6(2) . . . . ? C9 N3 N4 C11 -0.37(15) . . . . ? B1 N3 N4 C11 171.81(12) . . . . ? C9 N3 N4 Co1 178.81(9) . . . . ? B1 N3 N4 Co1 -9.02(15) . . . . ? N7 Co1 N4 C11 37.22(14) . . . . ? N6 Co1 N4 C11 142.45(14) . . . . ? O1 Co1 N4 C11 -27.9(2) . . . . ? N2 Co1 N4 C11 -128.45(14) . . . . ? N7 Co1 N4 N3 -141.60(9) . . . . ? N6 Co1 N4 N3 -36.36(9) . . . . ? O1 Co1 N4 N3 153.29(10) . . . . ? N2 Co1 N4 N3 52.74(9) . . . . ? C18 C17 N5 N6 -0.11(17) . . . . ? C18 C17 N5 B1 -179.35(14) . . . . ? N3 B1 N5 C17 117.51(16) . . . . ? N1 B1 N5 C17 -124.73(16) . . . . ? N3 B1 N5 N6 -61.66(17) . . . . ? N1 B1 N5 N6 56.11(18) . . . . ? C18 C19 N6 N5 -0.89(16) . . . . ? C20 C19 N6 N5 176.03(12) . . . . ? C18 C19 N6 Co1 175.00(11) . . . . ? C20 C19 N6 Co1 -8.1(2) . . . . ? C17 N5 N6 C19 0.63(16) . . . . ? B1 N5 N6 C19 179.94(13) . . . . ? C17 N5 N6 Co1 -176.33(10) . . . . ? B1 N5 N6 Co1 2.99(16) . . . . ? N7 Co1 N6 C19 -44.87(15) . . . . ? O1 Co1 N6 C19 39.35(15) . . . . ? N2 Co1 N6 C19 137.40(15) . . . . ? N4 Co1 N6 C19 -136.54(15) . . . . ? N7 Co1 N6 N5 130.79(9) . . . . ? O1 Co1 N6 N5 -145.00(9) . . . . ? N2 Co1 N6 N5 -46.95(10) . . . . ? N4 Co1 N6 N5 39.11(10) . . . . ? O1B C25 N7 Co1 176.14(8) 2_556 . . . ? N7 C25 N7 Co1 176.14(8) 2_556 . . . ? C26 C25 N7 Co1 -3.86(8) . . . . ? N6 Co1 N7 C25 110.25(8) . . . . ? O1 Co1 N7 C25 1.17(7) . . . . ? N2 Co1 N7 C25 -78.77(19) . . . . ? N4 Co1 N7 C25 -157.23(8) . . . . ? N7B C26 O1 Co1 175.21(8) 2_556 . . . ? O1 C26 O1 Co1 175.21(8) 2_556 . . . ? C25 C26 O1 Co1 -4.79(8) . . . . ? N7 Co1 O1 C26 2.25(7) . . . . ? N6 Co1 O1 C26 -100.06(7) . . . . ? N2 Co1 O1 C26 167.74(7) . . . . ? N4 Co1 O1 C26 69.59(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.448 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.048 data_09mz204_0m _database_code_depnum_ccdc_archive 'CCDC 881841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H85 B2 N15 Ni2 O2' _chemical_formula_weight 1163.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.181(3) _cell_length_b 18.2903(17) _cell_length_c 13.4544(13) _cell_angle_alpha 90.00 _cell_angle_beta 105.867(2) _cell_angle_gamma 90.00 _cell_volume 5960.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.55 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The coordinated acetonitrile molecule partially occupies the same space as one of its counterparts in a neighboring molecule and is half occupied. The central ligand is disordered across a two fold axis. Positions of N and O atoms were undistinguishable and each one N and O atom were refined to reside on the same position and with the same ADP. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 23403 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7223 _reflns_number_gt 5111 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0374P)^2^+7.6386P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7223 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.20182(13) 0.22905(17) 0.1359(3) 0.0332(8) Uani 1 1 d . . . H1A H 0.2338 0.2242 0.1058 0.040 Uiso 1 1 calc R . . C1 C 0.23609(10) 0.10934(15) 0.2383(2) 0.0334(7) Uani 1 1 d . . . H1 H 0.2686 0.1012 0.2170 0.040 Uiso 1 1 calc R . . C2 C 0.21773(11) 0.06634(15) 0.3054(2) 0.0308(6) Uani 1 1 d . . . H2 H 0.2348 0.0235 0.3396 0.037 Uiso 1 1 calc R . . C3 C 0.16887(10) 0.09854(14) 0.31324(19) 0.0245(5) Uani 1 1 d . . . C4 C 0.13074(10) 0.07132(14) 0.37314(18) 0.0255(5) Uani 1 1 d . . . H4 H 0.1054 0.1122 0.3790 0.031 Uiso 1 1 calc R . . C5 C 0.09548(11) 0.00743(15) 0.3173(2) 0.0321(6) Uani 1 1 d . . . H5A H 0.0741 0.0234 0.2476 0.039 Uiso 1 1 calc R . . H5B H 0.1199 -0.0332 0.3091 0.039 Uiso 1 1 calc R . . C6 C 0.05595(12) -0.01965(17) 0.3770(2) 0.0382(7) Uani 1 1 d . . . H6A H 0.0349 -0.0620 0.3404 0.046 Uiso 1 1 calc R . . H6B H 0.0293 0.0196 0.3797 0.046 Uiso 1 1 calc R . . C7 C 0.08676(12) -0.04233(16) 0.4870(2) 0.0359(7) Uani 1 1 d . . . H7A H 0.0598 -0.0561 0.5253 0.043 Uiso 1 1 calc R . . H7B H 0.1100 -0.0856 0.4847 0.043 Uiso 1 1 calc R . . C8 C 0.12273(11) 0.01956(16) 0.5430(2) 0.0338(7) Uani 1 1 d . . . H8A H 0.1445 0.0023 0.6118 0.041 Uiso 1 1 calc R . . H8B H 0.0989 0.0603 0.5535 0.041 Uiso 1 1 calc R . . C9 C 0.16199(10) 0.04736(15) 0.48235(19) 0.0300(6) Uani 1 1 d . . . H9A H 0.1834 0.0892 0.5195 0.036 Uiso 1 1 calc R . . H9B H 0.1884 0.0081 0.4782 0.036 Uiso 1 1 calc R . . C10 C 0.13893(14) 0.22867(15) -0.0535(2) 0.0380(7) Uani 1 1 d . . . H10 H 0.1667 0.2240 -0.0887 0.046 Uiso 1 1 calc R . . C11 C 0.08402(14) 0.23374(15) -0.0991(2) 0.0394(8) Uani 1 1 d . . . H11 H 0.0660 0.2328 -0.1710 0.047 Uiso 1 1 calc R . . C12 C 0.05936(11) 0.24065(14) -0.01788(18) 0.0278(6) Uani 1 1 d . . . C13 C -0.00027(11) 0.25217(15) -0.02421(18) 0.0299(6) Uani 1 1 d . . . H13 H -0.0057 0.2456 0.0462 0.036 Uiso 1 1 calc R . . C14 C -0.03593(13) 0.19601(17) -0.0979(3) 0.0554(10) Uani 1 1 d . . . H14A H -0.0284 0.1992 -0.1663 0.066 Uiso 1 1 calc R . . H14B H -0.0262 0.1461 -0.0704 0.066 Uiso 1 1 calc R . . C15 C -0.09709(14) 0.2101(2) -0.1100(4) 0.0774(14) Uani 1 1 d . . . H15A H -0.1191 0.1760 -0.1623 0.093 Uiso 1 1 calc R . . H15B H -0.1052 0.1994 -0.0435 0.093 Uiso 1 1 calc R . . C16 C -0.11497(16) 0.2868(2) -0.1417(3) 0.0600(11) Uani 1 1 d . . . H16A H -0.1135 0.2948 -0.2136 0.072 Uiso 1 1 calc R . . H16B H -0.1537 0.2935 -0.1397 0.072 Uiso 1 1 calc R . . C17 C -0.07918(15) 0.34212(18) -0.0726(3) 0.0510(9) Uani 1 1 d . . . H17A H -0.0857 0.3400 -0.0033 0.061 Uiso 1 1 calc R . . H17B H -0.0894 0.3917 -0.1010 0.061 Uiso 1 1 calc R . . C18 C -0.01832(15) 0.32877(16) -0.0622(3) 0.0501(9) Uani 1 1 d . . . H18A H -0.0111 0.3364 -0.1302 0.060 Uiso 1 1 calc R . . H18B H 0.0039 0.3648 -0.0133 0.060 Uiso 1 1 calc R . . C19 C 0.24697(10) 0.35036(14) 0.2196(2) 0.0295(6) Uani 1 1 d . . . H19 H 0.2799 0.3484 0.1982 0.035 Uiso 1 1 calc R . . C20 C 0.23320(10) 0.40482(14) 0.27750(19) 0.0260(6) Uani 1 1 d . . . H20 H 0.2542 0.4471 0.3041 0.031 Uiso 1 1 calc R . . C21 C 0.18152(10) 0.38486(13) 0.28915(18) 0.0219(5) Uani 1 1 d . . . C22 C 0.14627(10) 0.42795(14) 0.34109(18) 0.0225(5) Uani 1 1 d . . . H22 H 0.1193 0.3940 0.3596 0.027 Uiso 1 1 calc R . . C23 C 0.11381(10) 0.48679(15) 0.2675(2) 0.0289(6) Uani 1 1 d . . . H23A H 0.1399 0.5177 0.2431 0.035 Uiso 1 1 calc R . . H23B H 0.0888 0.4628 0.2065 0.035 Uiso 1 1 calc R . . C24 C 0.07998(11) 0.53493(16) 0.3198(2) 0.0357(7) Uani 1 1 d . . . H24A H 0.0609 0.5732 0.2710 0.043 Uiso 1 1 calc R . . H24B H 0.0515 0.5049 0.3388 0.043 Uiso 1 1 calc R . . C25 C 0.11670(13) 0.57070(15) 0.4163(2) 0.0378(7) Uani 1 1 d . . . H25A H 0.1435 0.6035 0.3969 0.045 Uiso 1 1 calc R . . H25B H 0.0938 0.6006 0.4500 0.045 Uiso 1 1 calc R . . C26 C 0.14740(12) 0.51338(15) 0.4910(2) 0.0342(6) Uani 1 1 d . . . H26A H 0.1206 0.4834 0.5152 0.041 Uiso 1 1 calc R . . H26B H 0.1723 0.5376 0.5519 0.041 Uiso 1 1 calc R . . C27 C 0.18124(11) 0.46386(15) 0.4401(2) 0.0311(6) Uani 1 1 d . . . H27A H 0.1990 0.4252 0.4897 0.037 Uiso 1 1 calc R . . H27B H 0.2109 0.4931 0.4237 0.037 Uiso 1 1 calc R . . N9 N 0.04236(7) 0.17496(9) 0.23337(12) 0.0156(4) Uani 0.50 1 d P A . H9 H 0.0450 0.1274 0.2260 0.019 Uiso 0.50 1 calc PR . . N8 N 0.04348(7) 0.31858(9) 0.23564(13) 0.0174(4) Uani 0.50 1 d P A . H8 H 0.0474 0.3661 0.2307 0.021 Uiso 0.50 1 calc PR . . C29 C 0.0000 0.20537(17) 0.2500 0.0149(4) Uani 1 2 d S . . C28 C 0.0000 0.28856(18) 0.2500 0.0149(4) Uani 1 2 d S . . O2 O 0.04236(7) 0.17496(9) 0.23337(12) 0.0156(4) Uani 0.50 1 d P A . O1 O 0.04348(7) 0.31858(9) 0.23564(13) 0.0174(4) Uani 0.50 1 d P A . N7 N 0.14256(17) 0.2526(2) 0.4094(3) 0.0262(9) Uani 0.50 1 d P A -1 C30 C 0.1863(2) 0.2549(3) 0.4622(3) 0.0210(10) Uani 0.50 1 d P A -1 C31 C 0.2423(3) 0.2581(4) 0.5267(5) 0.0392(16) Uani 0.50 1 d P A -1 H31A H 0.2678 0.2580 0.4832 0.059 Uiso 0.50 1 calc PR A -1 H31B H 0.2497 0.2156 0.5728 0.059 Uiso 0.50 1 calc PR A -1 H31C H 0.2475 0.3030 0.5680 0.059 Uiso 0.50 1 calc PR A -1 N1 N 0.20087(8) 0.16457(12) 0.20789(18) 0.0289(5) Uani 1 1 d . . . N2 N 0.15907(8) 0.15925(12) 0.25456(17) 0.0252(5) Uani 1 1 d . A . N3 N 0.14781(9) 0.23128(12) 0.04932(17) 0.0278(5) Uani 1 1 d . . . N4 N 0.09815(8) 0.23904(11) 0.07176(15) 0.0222(4) Uani 1 1 d . A . N5 N 0.20671(8) 0.30005(12) 0.19776(18) 0.0281(5) Uani 1 1 d . . . N6 N 0.16579(8) 0.32099(11) 0.24124(17) 0.0246(5) Uani 1 1 d . A . Ni1 Ni 0.102529(11) 0.244957(17) 0.22543(2) 0.01705(9) 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 B1 0.0251(15) 0.0283(18) 0.057(2) -0.0121(15) 0.0286(15) -0.0059(12) C1 0.0188(13) 0.0338(17) 0.0453(16) -0.0175(13) 0.0051(12) 0.0034(11) C2 0.0270(14) 0.0271(15) 0.0322(14) -0.0083(12) -0.0022(11) 0.0080(11) C3 0.0212(12) 0.0208(14) 0.0267(12) -0.0072(10) -0.0015(10) -0.0002(10) C4 0.0247(13) 0.0223(14) 0.0247(12) -0.0022(10) -0.0015(10) 0.0022(10) C5 0.0362(15) 0.0313(16) 0.0252(13) -0.0030(12) 0.0023(11) -0.0087(12) C6 0.0427(17) 0.0377(18) 0.0296(14) 0.0009(13) 0.0021(13) -0.0155(14) C7 0.0452(17) 0.0311(16) 0.0300(14) 0.0041(12) 0.0079(13) 0.0002(13) C8 0.0361(16) 0.0376(17) 0.0241(13) 0.0014(12) 0.0023(11) 0.0099(13) C9 0.0273(14) 0.0320(16) 0.0252(13) -0.0034(11) -0.0023(11) 0.0042(11) C10 0.066(2) 0.0231(15) 0.0391(16) -0.0091(12) 0.0390(16) -0.0143(14) C11 0.072(2) 0.0306(17) 0.0213(13) -0.0061(11) 0.0216(14) -0.0177(15) C12 0.0427(15) 0.0217(14) 0.0201(11) -0.0004(10) 0.0102(11) -0.0106(11) C13 0.0375(14) 0.0326(15) 0.0157(11) 0.0057(11) 0.0009(10) -0.0057(12) C14 0.0422(19) 0.0290(18) 0.073(2) -0.0042(16) -0.0220(16) 0.0084(14) C15 0.041(2) 0.044(2) 0.117(4) -0.012(2) -0.029(2) 0.0088(17) C16 0.070(2) 0.058(2) 0.0385(17) 0.0017(17) -0.0074(17) 0.041(2) C17 0.082(3) 0.0287(18) 0.056(2) 0.0081(15) 0.042(2) 0.0170(17) C18 0.079(3) 0.0211(16) 0.066(2) 0.0021(15) 0.048(2) 0.0044(16) C19 0.0177(12) 0.0256(15) 0.0450(16) 0.0030(12) 0.0082(11) -0.0042(10) C20 0.0214(12) 0.0202(14) 0.0324(14) 0.0022(11) 0.0006(10) -0.0042(10) C21 0.0196(12) 0.0173(13) 0.0253(12) 0.0005(10) 0.0003(10) 0.0002(9) C22 0.0233(12) 0.0192(13) 0.0228(12) 0.0008(10) 0.0023(10) 0.0027(10) C23 0.0258(13) 0.0313(16) 0.0288(13) 0.0080(12) 0.0061(11) 0.0092(11) C24 0.0328(15) 0.0341(17) 0.0436(16) 0.0132(13) 0.0159(13) 0.0142(13) C25 0.0459(18) 0.0214(15) 0.0524(18) 0.0027(13) 0.0238(15) 0.0076(13) C26 0.0453(17) 0.0250(15) 0.0319(14) -0.0074(12) 0.0097(13) -0.0018(12) C27 0.0367(15) 0.0203(14) 0.0293(13) -0.0029(11) -0.0025(11) 0.0053(11) N9 0.0155(8) 0.0123(9) 0.0203(9) 0.0006(7) 0.0071(7) 0.0024(7) N8 0.0189(9) 0.0129(9) 0.0220(9) 0.0007(7) 0.0082(7) -0.0031(7) C29 0.0164(10) 0.0159(12) 0.0115(9) 0.000 0.0023(7) 0.000 C28 0.0164(10) 0.0159(12) 0.0115(9) 0.000 0.0023(7) 0.000 O2 0.0155(8) 0.0123(9) 0.0203(9) 0.0006(7) 0.0071(7) 0.0024(7) O1 0.0189(9) 0.0129(9) 0.0220(9) 0.0007(7) 0.0082(7) -0.0031(7) N7 0.028(2) 0.024(2) 0.029(2) 0.0011(19) 0.0122(18) 0.0042(19) C30 0.033(3) 0.014(2) 0.017(2) -0.0001(19) 0.0093(19) -0.001(2) C31 0.034(3) 0.034(4) 0.040(4) 0.000(3) -0.004(3) 0.001(3) N1 0.0169(10) 0.0239(12) 0.0492(14) -0.0066(10) 0.0148(10) -0.0005(9) N2 0.0152(10) 0.0229(12) 0.0381(12) -0.0042(10) 0.0084(9) -0.0018(8) N3 0.0387(13) 0.0225(12) 0.0316(11) -0.0058(9) 0.0255(10) -0.0084(9) N4 0.0274(11) 0.0214(11) 0.0219(10) -0.0040(8) 0.0136(8) -0.0084(8) N5 0.0156(10) 0.0254(12) 0.0476(14) -0.0075(10) 0.0159(10) -0.0021(8) N6 0.0148(10) 0.0221(12) 0.0382(12) -0.0061(9) 0.0094(9) -0.0007(8) Ni1 0.01409(14) 0.02231(18) 0.01623(14) -0.00035(13) 0.00664(10) -0.00080(12) _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 B1 N5 1.529(4) . ? B1 N3 1.530(4) . ? B1 N1 1.531(4) . ? B1 H1A 1.0000 . ? C1 N1 1.333(3) . ? C1 C2 1.369(4) . ? C1 H1 0.9500 . ? C2 C3 1.393(3) . ? C2 H2 0.9500 . ? C3 N2 1.346(3) . ? C3 C4 1.498(4) . ? C4 C9 1.529(3) . ? C4 C5 1.534(3) . ? C4 H4 1.0000 . ? C5 C6 1.522(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.529(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.530(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.340(3) . ? C10 C11 1.354(5) . ? C10 H10 0.9500 . ? C11 C12 1.402(4) . ? C11 H11 0.9500 . ? C12 N4 1.329(3) . ? C12 C13 1.495(4) . ? C13 C18 1.518(4) . ? C13 C14 1.535(4) . ? C13 H13 1.0000 . ? C14 C15 1.526(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.498(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.498(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N5 1.341(3) . ? C19 C20 1.366(4) . ? C19 H19 0.9500 . ? C20 C21 1.401(3) . ? C20 H20 0.9500 . ? C21 N6 1.341(3) . ? C21 C22 1.495(3) . ? C22 C27 1.530(3) . ? C22 C23 1.537(3) . ? C22 H22 1.0000 . ? C23 C24 1.524(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.520(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.511(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.528(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N9 C29 1.276(2) . ? N9 Ni1 2.0087(17) . ? N9 H9 0.8800 . ? N8 C28 1.286(2) . ? N8 Ni1 2.0383(17) . ? N8 H8 0.8800 . ? C29 O2 1.276(2) 2 ? C29 N9 1.276(2) 2 ? C29 C28 1.522(4) . ? C28 O1 1.286(2) 2 ? C28 N8 1.286(2) 2 ? N7 C30 1.136(6) . ? N7 Ni1 2.408(4) . ? C30 C31 1.441(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N1 N2 1.369(3) . ? N2 Ni1 2.082(2) . ? N3 N4 1.372(3) . ? N4 Ni1 2.0430(19) . ? N5 N6 1.371(3) . ? N6 Ni1 2.081(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 N5 B1 N3 108.3(2) . . ? N5 B1 N1 108.8(2) . . ? N3 B1 N1 109.8(2) . . ? N5 B1 H1A 110.0 . . ? N3 B1 H1A 110.0 . . ? N1 B1 H1A 110.0 . . ? N1 C1 C2 108.8(2) . . ? N1 C1 H1 125.6 . . ? C2 C1 H1 125.6 . . ? C1 C2 C3 105.7(2) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? N2 C3 C2 109.2(2) . . ? N2 C3 C4 123.2(2) . . ? C2 C3 C4 127.5(2) . . ? C3 C4 C9 112.0(2) . . ? C3 C4 C5 111.1(2) . . ? C9 C4 C5 109.2(2) . . ? C3 C4 H4 108.1 . . ? C9 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? C6 C5 C4 111.4(2) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.5(2) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 110.8(2) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 111.7(2) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C4 C9 C8 111.7(2) . . ? C4 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C4 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? N3 C10 C11 109.1(2) . . ? N3 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? C10 C11 C12 105.6(2) . . ? C10 C11 H11 127.2 . . ? C12 C11 H11 127.2 . . ? N4 C12 C11 109.4(3) . . ? N4 C12 C13 122.2(2) . . ? C11 C12 C13 128.3(2) . . ? C12 C13 C18 110.7(2) . . ? C12 C13 C14 110.1(2) . . ? C18 C13 C14 109.4(2) . . ? C12 C13 H13 108.9 . . ? C18 C13 H13 108.9 . . ? C14 C13 H13 108.9 . . ? C15 C14 C13 110.5(3) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 113.9(3) . . ? C16 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? C16 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 111.9(3) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 111.6(3) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C13 C18 C17 112.4(3) . . ? C13 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C13 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? N5 C19 C20 109.3(2) . . ? N5 C19 H19 125.3 . . ? C20 C19 H19 125.3 . . ? C19 C20 C21 105.2(2) . . ? C19 C20 H20 127.4 . . ? C21 C20 H20 127.4 . . ? N6 C21 C20 109.5(2) . . ? N6 C21 C22 123.3(2) . . ? C20 C21 C22 127.1(2) . . ? C21 C22 C27 111.1(2) . . ? C21 C22 C23 110.3(2) . . ? C27 C22 C23 109.8(2) . . ? C21 C22 H22 108.5 . . ? C27 C22 H22 108.5 . . ? C23 C22 H22 108.5 . . ? C24 C23 C22 111.9(2) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 110.9(2) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 110.5(2) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C27 111.1(2) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C22 112.7(2) . . ? C26 C27 H27A 109.1 . . ? C22 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C22 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C29 N9 Ni1 114.23(16) . . ? C29 N9 H9 122.9 . . ? Ni1 N9 H9 122.9 . . ? C28 N8 Ni1 113.26(17) . . ? C28 N8 H8 123.4 . . ? Ni1 N8 H8 123.4 . . ? N9 C29 O2 128.3(3) . 2 ? N9 C29 N9 128.3(3) . 2 ? N9 C29 C28 115.85(15) . . ? O2 C29 C28 115.85(15) 2 . ? N9 C29 C28 115.85(15) 2 . ? O1 C28 N8 129.4(3) 2 . ? N8 C28 N8 129.4(3) 2 . ? O1 C28 C29 115.28(15) 2 . ? N8 C28 C29 115.28(15) 2 . ? N8 C28 C29 115.28(15) . . ? C30 N7 Ni1 134.9(4) . . ? N7 C30 C31 178.4(5) . . ? C1 N1 N2 109.6(2) . . ? C1 N1 B1 130.9(2) . . ? N2 N1 B1 119.5(2) . . ? C3 N2 N1 106.7(2) . . ? C3 N2 Ni1 137.59(17) . . ? N1 N2 Ni1 115.61(16) . . ? C10 N3 N4 109.0(2) . . ? C10 N3 B1 130.3(2) . . ? N4 N3 B1 120.6(2) . . ? C12 N4 N3 106.9(2) . . ? C12 N4 Ni1 137.76(17) . . ? N3 N4 Ni1 115.34(15) . . ? C19 N5 N6 109.0(2) . . ? C19 N5 B1 130.2(2) . . ? N6 N5 B1 120.8(2) . . ? C21 N6 N5 106.90(19) . . ? C21 N6 Ni1 138.47(17) . . ? N5 N6 Ni1 114.40(15) . . ? N9 Ni1 N8 80.95(7) . . ? N9 Ni1 N4 100.79(7) . . ? N8 Ni1 N4 105.35(8) . . ? N9 Ni1 N6 171.06(7) . . ? N8 Ni1 N6 95.95(7) . . ? N4 Ni1 N6 88.11(8) . . ? N9 Ni1 N2 89.83(7) . . ? N8 Ni1 N2 163.50(8) . . ? N4 Ni1 N2 89.75(8) . . ? N6 Ni1 N2 91.09(8) . . ? N9 Ni1 N7 95.29(11) . . ? N8 Ni1 N7 90.02(11) . . ? N4 Ni1 N7 159.23(11) . . ? N6 Ni1 N7 76.26(12) . . ? N2 Ni1 N7 77.16(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.5(3) . . . . ? C1 C2 C3 N2 -1.1(3) . . . . ? C1 C2 C3 C4 177.0(2) . . . . ? N2 C3 C4 C9 -136.1(2) . . . . ? C2 C3 C4 C9 46.0(3) . . . . ? N2 C3 C4 C5 101.5(3) . . . . ? C2 C3 C4 C5 -76.4(3) . . . . ? C3 C4 C5 C6 -179.1(2) . . . . ? C9 C4 C5 C6 56.9(3) . . . . ? C4 C5 C6 C7 -56.9(3) . . . . ? C5 C6 C7 C8 54.9(3) . . . . ? C6 C7 C8 C9 -54.4(3) . . . . ? C3 C4 C9 C8 -179.9(2) . . . . ? C5 C4 C9 C8 -56.4(3) . . . . ? C7 C8 C9 C4 56.2(3) . . . . ? N3 C10 C11 C12 0.8(3) . . . . ? C10 C11 C12 N4 -0.5(3) . . . . ? C10 C11 C12 C13 176.4(3) . . . . ? N4 C12 C13 C18 105.9(3) . . . . ? C11 C12 C13 C18 -70.7(4) . . . . ? N4 C12 C13 C14 -133.1(3) . . . . ? C11 C12 C13 C14 50.3(4) . . . . ? C12 C13 C14 C15 -176.6(3) . . . . ? C18 C13 C14 C15 -54.8(4) . . . . ? C13 C14 C15 C16 53.7(5) . . . . ? C14 C15 C16 C17 -52.1(5) . . . . ? C15 C16 C17 C18 52.0(4) . . . . ? C12 C13 C18 C17 178.5(2) . . . . ? C14 C13 C18 C17 57.0(4) . . . . ? C16 C17 C18 C13 -56.0(4) . . . . ? N5 C19 C20 C21 -0.4(3) . . . . ? C19 C20 C21 N6 0.7(3) . . . . ? C19 C20 C21 C22 -176.2(2) . . . . ? N6 C21 C22 C27 142.6(2) . . . . ? C20 C21 C22 C27 -41.0(3) . . . . ? N6 C21 C22 C23 -95.5(3) . . . . ? C20 C21 C22 C23 81.0(3) . . . . ? C21 C22 C23 C24 -176.6(2) . . . . ? C27 C22 C23 C24 -53.8(3) . . . . ? C22 C23 C24 C25 56.9(3) . . . . ? C23 C24 C25 C26 -57.7(3) . . . . ? C24 C25 C26 C27 56.6(3) . . . . ? C25 C26 C27 C22 -55.4(3) . . . . ? C21 C22 C27 C26 175.4(2) . . . . ? C23 C22 C27 C26 53.1(3) . . . . ? Ni1 N9 C29 O2 -174.09(12) . . . 2 ? Ni1 N9 C29 N9 -174.09(12) . . . 2 ? Ni1 N9 C29 C28 5.91(12) . . . . ? Ni1 N8 C28 O1 176.53(12) . . . 2 ? Ni1 N8 C28 N8 176.53(12) . . . 2 ? Ni1 N8 C28 C29 -3.47(12) . . . . ? N9 C29 C28 O1 178.39(12) . . . 2 ? O2 C29 C28 O1 -1.61(12) 2 . . 2 ? N9 C29 C28 O1 -1.61(12) 2 . . 2 ? N9 C29 C28 N8 178.39(12) . . . 2 ? O2 C29 C28 N8 -1.61(12) 2 . . 2 ? N9 C29 C28 N8 -1.61(12) 2 . . 2 ? N9 C29 C28 N8 -1.61(12) . . . . ? O2 C29 C28 N8 178.39(12) 2 . . . ? N9 C29 C28 N8 178.39(12) 2 . . . ? C2 C1 N1 N2 0.4(3) . . . . ? C2 C1 N1 B1 178.5(3) . . . . ? N5 B1 N1 C1 -116.3(3) . . . . ? N3 B1 N1 C1 125.3(3) . . . . ? N5 B1 N1 N2 61.7(3) . . . . ? N3 B1 N1 N2 -56.7(3) . . . . ? C2 C3 N2 N1 1.4(3) . . . . ? C4 C3 N2 N1 -176.9(2) . . . . ? C2 C3 N2 Ni1 -174.30(19) . . . . ? C4 C3 N2 Ni1 7.5(4) . . . . ? C1 N1 N2 C3 -1.1(3) . . . . ? B1 N1 N2 C3 -179.5(2) . . . . ? C1 N1 N2 Ni1 175.68(16) . . . . ? B1 N1 N2 Ni1 -2.7(3) . . . . ? C11 C10 N3 N4 -0.7(3) . . . . ? C11 C10 N3 B1 -178.9(3) . . . . ? N5 B1 N3 C10 119.3(3) . . . . ? N1 B1 N3 C10 -122.0(3) . . . . ? N5 B1 N3 N4 -58.6(3) . . . . ? N1 B1 N3 N4 60.0(3) . . . . ? C11 C12 N4 N3 0.1(3) . . . . ? C13 C12 N4 N3 -177.0(2) . . . . ? C11 C12 N4 Ni1 -179.99(19) . . . . ? C13 C12 N4 Ni1 2.8(4) . . . . ? C10 N3 N4 C12 0.3(3) . . . . ? B1 N3 N4 C12 178.7(2) . . . . ? C10 N3 N4 Ni1 -179.56(17) . . . . ? B1 N3 N4 Ni1 -1.2(3) . . . . ? C20 C19 N5 N6 0.0(3) . . . . ? C20 C19 N5 B1 180.0(3) . . . . ? N3 B1 N5 C19 -124.2(3) . . . . ? N1 B1 N5 C19 116.6(3) . . . . ? N3 B1 N5 N6 55.8(3) . . . . ? N1 B1 N5 N6 -63.5(3) . . . . ? C20 C21 N6 N5 -0.7(3) . . . . ? C22 C21 N6 N5 176.3(2) . . . . ? C20 C21 N6 Ni1 173.36(19) . . . . ? C22 C21 N6 Ni1 -9.6(4) . . . . ? C19 N5 N6 C21 0.4(3) . . . . ? B1 N5 N6 C21 -179.5(2) . . . . ? C19 N5 N6 Ni1 -175.25(17) . . . . ? B1 N5 N6 Ni1 4.8(3) . . . . ? C29 N9 Ni1 N8 -6.03(10) . . . . ? C29 N9 Ni1 N4 -110.07(12) . . . . ? C29 N9 Ni1 N2 160.22(12) . . . . ? C29 N9 Ni1 N7 83.14(14) . . . . ? C28 N8 Ni1 N9 5.07(10) . . . . ? C28 N8 Ni1 N4 103.87(11) . . . . ? C28 N8 Ni1 N6 -166.47(11) . . . . ? C28 N8 Ni1 N2 -51.7(3) . . . . ? C28 N8 Ni1 N7 -90.28(14) . . . . ? C12 N4 Ni1 N9 46.6(3) . . . . ? N3 N4 Ni1 N9 -133.58(16) . . . . ? C12 N4 Ni1 N8 -36.9(3) . . . . ? N3 N4 Ni1 N8 142.95(16) . . . . ? C12 N4 Ni1 N6 -132.6(3) . . . . ? N3 N4 Ni1 N6 47.30(17) . . . . ? C12 N4 Ni1 N2 136.3(3) . . . . ? N3 N4 Ni1 N2 -43.80(17) . . . . ? C12 N4 Ni1 N7 -173.4(3) . . . . ? N3 N4 Ni1 N7 6.5(4) . . . . ? C21 N6 Ni1 N8 31.8(3) . . . . ? N5 N6 Ni1 N8 -154.51(17) . . . . ? C21 N6 Ni1 N4 137.0(3) . . . . ? N5 N6 Ni1 N4 -49.27(18) . . . . ? C21 N6 Ni1 N2 -133.3(3) . . . . ? N5 N6 Ni1 N2 40.44(18) . . . . ? C21 N6 Ni1 N7 -56.8(3) . . . . ? N5 N6 Ni1 N7 116.9(2) . . . . ? C3 N2 Ni1 N9 -37.5(2) . . . . ? N1 N2 Ni1 N9 147.08(17) . . . . ? C3 N2 Ni1 N8 18.1(4) . . . . ? N1 N2 Ni1 N8 -157.2(2) . . . . ? C3 N2 Ni1 N4 -138.3(2) . . . . ? N1 N2 Ni1 N4 46.29(17) . . . . ? C3 N2 Ni1 N6 133.6(3) . . . . ? N1 N2 Ni1 N6 -41.81(17) . . . . ? C3 N2 Ni1 N7 57.9(3) . . . . ? N1 N2 Ni1 N7 -117.5(2) . . . . ? C30 N7 Ni1 N9 140.1(5) . . . . ? C30 N7 Ni1 N8 -138.9(5) . . . . ? C30 N7 Ni1 N4 -0.6(8) . . . . ? C30 N7 Ni1 N6 -42.8(5) . . . . ? C30 N7 Ni1 N2 51.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.861 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.068 # start Validation Reply Form _vrf_PLAT220_09mz204_0m ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.19 Ratio RESPONSE: The outer C atoms of the cyclohexyl rings show a largere than average thermal motion. ; data_09mz201_0m _database_code_depnum_ccdc_archive 'CCDC 881842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H82 B2 Co2 N14 S2' _chemical_formula_weight 1082.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2726(12) _cell_length_b 15.5651(16) _cell_length_c 30.493(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.370(2) _cell_angle_gamma 90.00 _cell_volume 5807.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1172 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 23.09 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The central ligand is inversion disordered in a ratio of 0.575(2) to 0.425(2). The disordered moieties were restrained to have similar geometries. The N and C atoms of the bridging ligand were restrained to be isotropic within standard deviations of 0.05 and 0.004 Angstrom squared, respectively, and overlapping disordered atoms were constrained to have identical ADPs. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 30514 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14148 _reflns_number_gt 9094 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0448P)^2^+2.4817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14148 _refine_ls_number_parameters 668 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7298(2) 0.57883(18) -0.03315(9) 0.0251(6) Uani 1 1 d . A . H1 H 0.7136 0.5336 -0.0560 0.030 Uiso 1 1 calc R . . B2 B 0.8091(2) 1.1881(2) 0.20484(10) 0.0300(7) Uani 1 1 d . A . H2 H 0.8238 1.2430 0.2213 0.036 Uiso 1 1 calc R . . C1 C 0.3998(4) 1.0203(3) 0.05693(18) 0.115(2) Uani 1 1 d . . . H1A H 0.3896 1.0479 0.0280 0.173 Uiso 1 1 calc R . . H1B H 0.3291 1.0002 0.0658 0.173 Uiso 1 1 calc R . . H1C H 0.4496 0.9714 0.0553 0.173 Uiso 1 1 calc R . . C2 C 0.4487(3) 1.0854(2) 0.09083(12) 0.0591(10) Uani 1 1 d . . . C3 C 0.5574(3) 1.1166(2) 0.07549(9) 0.0476(8) Uani 1 1 d . . . H3A H 0.6016 1.0658 0.0687 0.057 Uiso 1 1 calc R . . H3B H 0.5425 1.1493 0.0478 0.057 Uiso 1 1 calc R . . C4 C 0.6232(2) 1.17134(18) 0.10713(8) 0.0326(6) Uani 1 1 d . . . C5 C 0.6177(2) 1.25956(19) 0.11290(9) 0.0386(7) Uani 1 1 d . . . H5 H 0.5728 1.2989 0.0959 0.046 Uiso 1 1 calc R . . C6 C 0.6896(2) 1.27850(17) 0.14784(9) 0.0361(6) Uani 1 1 d . A . H6 H 0.7034 1.3341 0.1599 0.043 Uiso 1 1 calc R . . C7 C 0.4676(3) 1.0421(3) 0.13594(16) 0.0902(15) Uani 1 1 d . . . H7A H 0.5213 0.9958 0.1343 0.135 Uiso 1 1 calc R . . H7B H 0.3986 1.0182 0.1446 0.135 Uiso 1 1 calc R . . H7C H 0.4951 1.0846 0.1578 0.135 Uiso 1 1 calc R . . C8 C 0.3693(3) 1.1598(3) 0.09355(14) 0.0757(13) Uani 1 1 d . . . H8A H 0.3998 1.2020 0.1149 0.113 Uiso 1 1 calc R . . H8B H 0.2996 1.1384 0.1029 0.113 Uiso 1 1 calc R . . H8C H 0.3573 1.1870 0.0646 0.113 Uiso 1 1 calc R . . C9 C 0.5881(3) 0.8896(2) 0.32104(10) 0.0574(9) Uani 1 1 d . . . H9A H 0.6319 0.9389 0.3318 0.086 Uiso 1 1 calc R . . H9B H 0.5990 0.8418 0.3419 0.086 Uiso 1 1 calc R . . H9C H 0.5107 0.9056 0.3182 0.086 Uiso 1 1 calc R . . C10 C 0.7475(3) 0.8480(2) 0.27985(10) 0.0481(8) Uani 1 1 d . . . H10A H 0.7702 0.8260 0.2518 0.072 Uiso 1 1 calc R . . H10B H 0.7670 0.8063 0.3032 0.072 Uiso 1 1 calc R . . H10C H 0.7845 0.9026 0.2868 0.072 Uiso 1 1 calc R . . C11 C 0.5661(3) 0.7784(2) 0.26280(12) 0.0679(11) Uani 1 1 d . . . H11A H 0.4871 0.7884 0.2589 0.102 Uiso 1 1 calc R . . H11B H 0.5818 0.7352 0.2858 0.102 Uiso 1 1 calc R . . H11C H 0.5924 0.7579 0.2351 0.102 Uiso 1 1 calc R . . C12 C 0.6237(2) 0.8619(2) 0.27618(9) 0.0406(7) Uani 1 1 d . . . C13 C 0.5919(2) 0.92935(18) 0.24033(8) 0.0337(6) Uani 1 1 d . . . H13A H 0.6087 0.9053 0.2116 0.040 Uiso 1 1 calc R . . H13B H 0.5118 0.9380 0.2393 0.040 Uiso 1 1 calc R . . C14 C 0.6454(2) 1.01503(18) 0.24545(8) 0.0291(6) Uani 1 1 d . . . C15 C 0.6320(2) 1.0766(2) 0.27826(9) 0.0422(7) Uani 1 1 d . . . H15 H 0.5872 1.0720 0.3022 0.051 Uiso 1 1 calc R . . C16 C 0.6961(2) 1.14422(19) 0.26869(9) 0.0377(7) Uani 1 1 d . A . H16 H 0.7041 1.1960 0.2851 0.045 Uiso 1 1 calc R . . C17 C 1.1177(3) 0.8174(2) 0.15258(11) 0.0531(9) Uani 1 1 d . . . H17A H 1.1487 0.7721 0.1721 0.080 Uiso 1 1 calc R . . H17B H 1.1673 0.8290 0.1296 0.080 Uiso 1 1 calc R . . H17C H 1.0468 0.7986 0.1390 0.080 Uiso 1 1 calc R . . C18 C 1.2126(3) 0.9267(2) 0.20083(11) 0.0533(9) Uani 1 1 d . . . H18A H 1.2029 0.9778 0.2189 0.080 Uiso 1 1 calc R . . H18B H 1.2623 0.9401 0.1781 0.080 Uiso 1 1 calc R . . H18C H 1.2435 0.8801 0.2195 0.080 Uiso 1 1 calc R . . C19 C 1.1026(2) 0.89893(18) 0.17914(9) 0.0345(6) Uani 1 1 d . . . C20 C 1.0252(3) 0.8802(2) 0.21433(10) 0.0521(9) Uani 1 1 d . . . H20A H 0.9563 0.8577 0.2006 0.078 Uiso 1 1 calc R . . H20B H 1.0111 0.9332 0.2303 0.078 Uiso 1 1 calc R . . H20C H 1.0582 0.8375 0.2349 0.078 Uiso 1 1 calc R . . C21 C 1.0539(2) 0.96800(17) 0.14676(8) 0.0310(6) Uani 1 1 d . . . H21A H 1.1078 0.9805 0.1251 0.037 Uiso 1 1 calc R . . H21B H 0.9881 0.9438 0.1305 0.037 Uiso 1 1 calc R . . C22 C 1.0230(2) 1.05065(17) 0.16743(8) 0.0272(6) Uani 1 1 d . . . C23 C 1.0891(2) 1.11716(17) 0.18445(8) 0.0320(6) Uani 1 1 d . . . H23 H 1.1664 1.1210 0.1847 0.038 Uiso 1 1 calc R . . C24 C 1.0197(2) 1.17576(17) 0.20068(8) 0.0306(6) Uani 1 1 d . A . H24 H 1.0408 1.2284 0.2146 0.037 Uiso 1 1 calc R . . C25 C 0.4427(3) 0.7867(2) 0.13275(11) 0.0563(10) Uani 1 1 d . . . H25A H 0.4171 0.7634 0.1600 0.084 Uiso 1 1 calc R . . H25B H 0.3900 0.8290 0.1203 0.084 Uiso 1 1 calc R . . H25C H 0.5139 0.8143 0.1391 0.084 Uiso 1 1 calc R . . C26 C 0.4538(2) 0.71411(18) 0.09996(8) 0.0309(6) Uani 1 1 d . . . C27 C 0.3437(2) 0.6708(2) 0.09127(10) 0.0442(8) Uani 1 1 d . . . H27A H 0.3510 0.6213 0.0718 0.066 Uiso 1 1 calc R . . H27B H 0.2914 0.7117 0.0772 0.066 Uiso 1 1 calc R . . H27C H 0.3175 0.6513 0.1192 0.066 Uiso 1 1 calc R . . C28 C 0.5362(3) 0.6488(3) 0.11839(11) 0.0590(10) Uani 1 1 d . . . H28A H 0.5103 0.6230 0.1450 0.088 Uiso 1 1 calc R . . H28B H 0.6066 0.6771 0.1256 0.088 Uiso 1 1 calc R . . H28C H 0.5451 0.6038 0.0965 0.088 Uiso 1 1 calc R . . C29 C 0.4929(2) 0.75385(17) 0.05734(8) 0.0292(6) Uani 1 1 d . . . H29A H 0.4350 0.7926 0.0446 0.035 Uiso 1 1 calc R . . H29B H 0.5583 0.7894 0.0653 0.035 Uiso 1 1 calc R . . C30 C 0.5206(2) 0.69117(16) 0.02274(8) 0.0251(5) Uani 1 1 d . . . C31 C 0.4520(2) 0.64114(17) -0.00531(8) 0.0302(6) Uani 1 1 d . . . H31 H 0.3744 0.6406 -0.0074 0.036 Uiso 1 1 calc R . . C32 C 0.5195(2) 0.59277(17) -0.02926(8) 0.0286(6) Uani 1 1 d . A . H32 H 0.4967 0.5515 -0.0510 0.034 Uiso 1 1 calc R . . C33 C 1.1175(3) 0.9015(2) 0.01827(17) 0.0909(16) Uani 1 1 d . . . H33A H 1.1885 0.8900 0.0341 0.136 Uiso 1 1 calc R . . H33B H 1.0662 0.9221 0.0390 0.136 Uiso 1 1 calc R . . H33C H 1.1261 0.9453 -0.0043 0.136 Uiso 1 1 calc R . . C34 C 1.1563(3) 0.7825(2) -0.03357(14) 0.0694(12) Uani 1 1 d . . . H34A H 1.1321 0.7261 -0.0448 0.104 Uiso 1 1 calc R . . H34B H 1.2273 0.7767 -0.0168 0.104 Uiso 1 1 calc R . . H34C H 1.1633 0.8218 -0.0583 0.104 Uiso 1 1 calc R . . C35 C 1.0530(3) 0.7530(2) 0.03211(11) 0.0535(9) Uani 1 1 d . . . H35A H 1.0268 0.6990 0.0186 0.080 Uiso 1 1 calc R . . H35B H 0.9980 0.7756 0.0507 0.080 Uiso 1 1 calc R . . H35C H 1.1214 0.7427 0.0501 0.080 Uiso 1 1 calc R . . C36 C 1.0729(2) 0.8181(2) -0.00378(13) 0.0551(10) Uani 1 1 d . . . C37 C 0.9643(2) 0.83975(17) -0.03035(10) 0.0408(7) Uani 1 1 d . . . H37A H 0.9174 0.8718 -0.0110 0.049 Uiso 1 1 calc R . . H37B H 0.9804 0.8785 -0.0548 0.049 Uiso 1 1 calc R . . C38 C 0.9012(2) 0.76486(16) -0.04915(9) 0.0306(6) Uani 1 1 d . . . C39 C 0.9006(2) 0.73024(18) -0.09151(9) 0.0365(7) Uani 1 1 d . . . H39 H 0.9394 0.7510 -0.1151 0.044 Uiso 1 1 calc R . . C40 C 0.8329(2) 0.66036(18) -0.09205(8) 0.0330(6) Uani 1 1 d . A . H40 H 0.8160 0.6235 -0.1164 0.040 Uiso 1 1 calc R . . C41 C 0.9805(4) 0.5820(2) 0.19084(9) 0.0678(11) Uani 1 1 d . . . H41A H 0.9618 0.5562 0.2186 0.102 Uiso 1 1 calc R . . H41B H 0.9558 0.6419 0.1895 0.102 Uiso 1 1 calc R . . H41C H 1.0599 0.5800 0.1891 0.102 Uiso 1 1 calc R . . C42 C 0.9244(2) 0.53204(19) 0.15233(8) 0.0381(7) Uani 1 1 d . . . C43 C 0.7998(3) 0.5358(2) 0.15395(11) 0.0623(11) Uani 1 1 d . . . H43A H 0.7647 0.5078 0.1278 0.094 Uiso 1 1 calc R . . H43B H 0.7763 0.5959 0.1548 0.094 Uiso 1 1 calc R . . H43C H 0.7788 0.5062 0.1804 0.094 Uiso 1 1 calc R . . C44 C 0.9576(3) 0.4383(2) 0.15602(9) 0.0453(8) Uani 1 1 d . . . H44A H 1.0370 0.4335 0.1550 0.068 Uiso 1 1 calc R . . H44B H 0.9211 0.4060 0.1315 0.068 Uiso 1 1 calc R . . H44C H 0.9361 0.4150 0.1839 0.068 Uiso 1 1 calc R . . C45 C 0.9598(2) 0.57323(18) 0.10947(8) 0.0299(6) Uani 1 1 d . . . H45A H 0.9473 0.6359 0.1112 0.036 Uiso 1 1 calc R . . H45B H 1.0394 0.5643 0.1085 0.036 Uiso 1 1 calc R . . C46 C 0.90466(19) 0.54164(16) 0.06706(8) 0.0240(5) Uani 1 1 d . . . C47 C 0.9164(2) 0.46183(16) 0.04718(8) 0.0264(5) Uani 1 1 d . . . H47 H 0.9608 0.4152 0.0579 0.032 Uiso 1 1 calc R . . C48 C 0.8501(2) 0.46490(15) 0.00887(8) 0.0251(5) Uani 1 1 d . A . H48 H 0.8406 0.4199 -0.0121 0.030 Uiso 1 1 calc R . . Co1 Co 0.77910(3) 0.71903(2) 0.037296(11) 0.02751(9) Uani 1 1 d . . . Co2 Co 0.76491(3) 1.01842(2) 0.154014(11) 0.03124(10) Uani 1 1 d . . . N1 N 0.69723(17) 1.13849(13) 0.13746(7) 0.0278(5) Uani 1 1 d . A . N2 N 0.73746(18) 1.20563(13) 0.16230(7) 0.0292(5) Uani 1 1 d . . . N3 N 0.74618(17) 1.12613(13) 0.23246(6) 0.0268(5) Uani 1 1 d . . . N4 N 0.71484(16) 1.04573(13) 0.21738(7) 0.0264(5) Uani 1 1 d . A . N5 N 0.91715(17) 1.14690(13) 0.19373(7) 0.0273(5) Uani 1 1 d . . . N6 N 0.91779(17) 1.06936(13) 0.17283(6) 0.0265(5) Uani 1 1 d . A . N7 N 0.79452(16) 0.65297(13) -0.05224(6) 0.0247(5) Uani 1 1 d . . . N8 N 0.83537(16) 0.71725(13) -0.02547(6) 0.0244(4) Uani 1 1 d . A . N9 N 0.80113(16) 0.54149(13) 0.00597(6) 0.0225(4) Uani 1 1 d . . . N10 N 0.83440(16) 0.59052(12) 0.04192(6) 0.0222(4) Uani 1 1 d . A . N11 N 0.62284(17) 0.61356(13) -0.01680(6) 0.0247(4) Uani 1 1 d . . . N12 N 0.62569(16) 0.67469(13) 0.01538(6) 0.0243(4) Uani 1 1 d . A . N13 N 0.7622(5) 0.8439(3) 0.03455(17) 0.0263(5) Uani 0.575(2) 1 d PDU A 1 H13C H 0.7461 0.8703 0.0094 0.032 Uiso 0.575(2) 1 calc PR A 1 N14 N 0.7866(4) 0.7480(3) 0.09740(16) 0.0298(5) Uani 0.575(2) 1 d PDU A 1 H14C H 0.7974 0.7073 0.1173 0.036 Uiso 0.575(2) 1 calc PR A 1 N13B N 0.7658(5) 0.9903(4) 0.0944(2) 0.0315(4) Uani 0.425(2) 1 d PD A 2 H13D H 0.7697 1.0318 0.0750 0.038 Uiso 0.425(2) 1 calc PR A 2 N14B N 0.7648(6) 0.8981(4) 0.1571(2) 0.0265(3) Uani 0.425(2) 1 d PD A 2 H14D H 0.7599 0.8719 0.1825 0.032 Uiso 0.425(2) 1 calc PR A 2 C49 C 0.7762(5) 0.8269(3) 0.10987(15) 0.0189(10) Uani 0.575(2) 1 d PDU A 1 C50 C 0.7756(5) 0.8867(3) 0.07114(17) 0.0204(11) Uani 0.575(2) 1 d PDU A 1 S1 S 0.75807(12) 0.86273(8) 0.16174(4) 0.0265(3) Uani 0.575(2) 1 d PD A 1 S2 S 0.79349(12) 0.99347(8) 0.07660(4) 0.0315(4) Uani 0.575(2) 1 d PD A 1 C50B C 0.7608(8) 0.9110(5) 0.0809(2) 0.0204(11) Uani 0.425(2) 1 d PD A 2 C49B C 0.7720(8) 0.8536(4) 0.1210(2) 0.0189(10) Uani 0.425(2) 1 d PD A 2 S2B S 0.74015(17) 0.87389(12) 0.02915(6) 0.0263(5) Uani 0.425(2) 1 d PD A 2 S1B S 0.79686(17) 0.74783(12) 0.11765(6) 0.0298(5) Uani 0.425(2) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0294(16) 0.0235(14) 0.0215(14) -0.0039(11) -0.0026(12) 0.0058(12) B2 0.0309(17) 0.0252(15) 0.0336(16) -0.0070(13) 0.0008(13) 0.0010(13) C1 0.072(3) 0.089(4) 0.173(5) -0.073(3) -0.063(3) 0.018(3) C2 0.0407(19) 0.052(2) 0.079(3) -0.0210(19) -0.0291(18) 0.0093(16) C3 0.051(2) 0.054(2) 0.0350(16) -0.0162(14) -0.0166(14) 0.0228(16) C4 0.0354(15) 0.0378(16) 0.0248(13) 0.0006(12) 0.0035(11) 0.0110(12) C5 0.0452(18) 0.0368(16) 0.0338(15) 0.0090(12) 0.0023(13) 0.0110(13) C6 0.0408(17) 0.0219(13) 0.0462(17) 0.0013(12) 0.0066(13) 0.0043(12) C7 0.056(3) 0.087(3) 0.124(4) 0.031(3) -0.010(3) -0.030(2) C8 0.036(2) 0.082(3) 0.104(3) -0.036(2) -0.025(2) 0.0209(19) C9 0.054(2) 0.082(3) 0.0369(18) 0.0193(17) 0.0097(16) -0.0048(19) C10 0.049(2) 0.054(2) 0.0398(17) 0.0122(15) -0.0035(15) 0.0074(16) C11 0.088(3) 0.050(2) 0.063(2) 0.0167(18) -0.009(2) -0.028(2) C12 0.0444(18) 0.0450(18) 0.0320(15) 0.0108(13) -0.0008(13) -0.0066(14) C13 0.0289(15) 0.0429(17) 0.0292(14) 0.0035(12) 0.0008(11) -0.0019(12) C14 0.0254(14) 0.0377(15) 0.0241(13) -0.0006(11) 0.0009(10) 0.0038(11) C15 0.0421(18) 0.058(2) 0.0284(15) -0.0088(14) 0.0135(13) 0.0000(15) C16 0.0424(17) 0.0424(17) 0.0291(14) -0.0153(13) 0.0068(13) 0.0051(14) C17 0.050(2) 0.0436(19) 0.064(2) -0.0090(16) -0.0086(17) 0.0192(16) C18 0.0424(19) 0.051(2) 0.065(2) 0.0066(17) -0.0107(16) -0.0007(16) C19 0.0304(15) 0.0345(16) 0.0389(16) 0.0006(12) 0.0048(12) 0.0065(12) C20 0.052(2) 0.055(2) 0.0506(19) 0.0266(16) 0.0117(16) 0.0154(16) C21 0.0301(14) 0.0368(16) 0.0274(13) 0.0022(11) 0.0103(11) 0.0065(12) C22 0.0285(14) 0.0303(14) 0.0236(13) 0.0073(11) 0.0071(11) 0.0047(11) C23 0.0280(14) 0.0358(15) 0.0331(14) 0.0098(12) 0.0077(11) -0.0030(12) C24 0.0319(15) 0.0297(14) 0.0302(14) 0.0034(11) 0.0021(11) -0.0054(12) C25 0.050(2) 0.074(2) 0.0479(19) -0.0240(17) 0.0234(16) -0.0232(18) C26 0.0222(13) 0.0432(16) 0.0281(13) -0.0029(12) 0.0066(11) 0.0000(12) C27 0.0336(16) 0.058(2) 0.0409(17) -0.0045(15) 0.0054(13) -0.0126(15) C28 0.0411(19) 0.093(3) 0.0445(18) 0.0342(18) 0.0147(15) 0.0156(18) C29 0.0272(14) 0.0288(14) 0.0319(14) -0.0013(11) 0.0030(11) 0.0060(11) C30 0.0259(13) 0.0257(13) 0.0237(13) 0.0061(10) 0.0018(10) 0.0044(10) C31 0.0231(13) 0.0361(15) 0.0310(14) 0.0040(11) -0.0005(11) 0.0024(11) C32 0.0280(14) 0.0302(14) 0.0265(13) -0.0005(11) -0.0059(11) -0.0016(11) C33 0.055(2) 0.052(2) 0.170(5) -0.059(3) 0.038(3) -0.0239(19) C34 0.0364(19) 0.0411(19) 0.137(4) -0.027(2) 0.045(2) -0.0073(15) C35 0.0331(18) 0.051(2) 0.074(2) -0.0164(18) -0.0106(16) 0.0007(15) C36 0.0287(17) 0.0356(17) 0.104(3) -0.0264(18) 0.0252(18) -0.0081(14) C37 0.0465(18) 0.0199(13) 0.0603(19) 0.0044(13) 0.0322(16) 0.0026(12) C38 0.0335(15) 0.0242(14) 0.0361(15) 0.0117(11) 0.0162(12) 0.0114(11) C39 0.0429(17) 0.0404(17) 0.0280(14) 0.0145(12) 0.0147(12) 0.0152(13) C40 0.0361(16) 0.0443(17) 0.0187(13) 0.0032(11) 0.0035(11) 0.0179(13) C41 0.116(3) 0.063(2) 0.0230(16) -0.0073(15) -0.0033(18) 0.007(2) C42 0.0475(18) 0.0470(18) 0.0201(13) -0.0001(12) 0.0042(12) 0.0173(14) C43 0.063(2) 0.068(2) 0.060(2) 0.0321(19) 0.0337(19) 0.0238(19) C44 0.059(2) 0.0499(19) 0.0278(15) 0.0031(13) 0.0062(14) 0.0170(16) C45 0.0263(14) 0.0391(16) 0.0239(13) -0.0030(11) -0.0010(11) 0.0048(11) C46 0.0221(13) 0.0282(13) 0.0221(12) 0.0029(10) 0.0042(10) -0.0015(10) C47 0.0254(13) 0.0262(13) 0.0276(13) 0.0015(10) 0.0013(10) 0.0038(10) C48 0.0250(13) 0.0220(13) 0.0281(13) -0.0037(10) 0.0016(10) 0.0036(10) Co1 0.0335(2) 0.02169(18) 0.02718(19) -0.00436(14) 0.00137(15) -0.00167(15) Co2 0.0404(2) 0.02748(19) 0.02554(19) -0.00723(15) 0.00029(15) -0.00190(16) N1 0.0293(12) 0.0282(12) 0.0257(11) -0.0053(9) 0.0001(9) 0.0024(9) N2 0.0317(12) 0.0240(12) 0.0316(12) -0.0025(9) 0.0008(9) 0.0010(9) N3 0.0283(12) 0.0268(11) 0.0252(11) -0.0077(9) 0.0021(9) 0.0027(9) N4 0.0258(11) 0.0260(11) 0.0275(11) -0.0046(9) 0.0033(9) 0.0008(9) N5 0.0260(12) 0.0266(11) 0.0292(11) -0.0029(9) 0.0014(9) -0.0012(9) N6 0.0294(12) 0.0264(11) 0.0238(11) -0.0009(9) 0.0035(9) 0.0020(9) N7 0.0279(11) 0.0299(12) 0.0162(10) -0.0002(8) 0.0007(8) 0.0067(9) N8 0.0276(11) 0.0206(10) 0.0257(11) 0.0004(9) 0.0064(9) 0.0042(9) N9 0.0231(11) 0.0240(11) 0.0202(10) -0.0035(8) 0.0001(8) 0.0009(8) N10 0.0251(11) 0.0229(10) 0.0186(10) -0.0027(8) 0.0015(8) -0.0004(9) N11 0.0265(11) 0.0248(11) 0.0223(10) -0.0031(8) -0.0016(9) 0.0021(9) N12 0.0259(11) 0.0232(11) 0.0237(10) -0.0025(8) 0.0020(9) 0.0020(9) N13 0.0364(11) 0.0197(11) 0.0233(8) -0.0041(8) 0.0051(7) 0.0026(8) N14 0.0365(8) 0.0217(6) 0.0313(12) -0.0049(9) 0.0040(10) 0.0008(6) N13B 0.0473(8) 0.0232(6) 0.0247(7) -0.0029(5) 0.0066(5) 0.0042(5) N14B 0.0340(6) 0.0254(8) 0.0204(6) -0.0054(6) 0.0046(4) 0.0003(6) C49 0.0185(14) 0.022(3) 0.017(2) 0.0004(17) 0.0026(18) 0.000(2) C50 0.018(2) 0.022(3) 0.022(2) 0.0044(18) 0.0024(17) 0.0048(19) S1 0.0340(6) 0.0254(8) 0.0204(6) -0.0054(6) 0.0046(4) 0.0003(6) S2 0.0473(8) 0.0232(6) 0.0247(7) -0.0029(5) 0.0066(5) 0.0042(5) C50B 0.018(2) 0.022(3) 0.022(2) 0.0044(18) 0.0024(17) 0.0048(19) C49B 0.0185(14) 0.022(3) 0.017(2) 0.0004(17) 0.0026(18) 0.000(2) S2B 0.0364(11) 0.0197(11) 0.0233(8) -0.0041(8) 0.0051(7) 0.0026(8) S1B 0.0365(8) 0.0217(6) 0.0313(12) -0.0049(9) 0.0040(10) 0.0008(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 B1 N11 1.537(3) . ? B1 N9 1.539(3) . ? B1 N7 1.540(3) . ? B1 H1 1.0000 . ? B2 N3 1.528(4) . ? B2 N5 1.534(4) . ? B2 N2 1.535(4) . ? B2 H2 1.0000 . ? C1 C2 1.535(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C8 1.520(5) . ? C2 C3 1.526(5) . ? C2 C7 1.533(5) . ? C3 C4 1.480(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.347(3) . ? C4 C5 1.387(4) . ? C5 C6 1.363(4) . ? C5 H5 0.9500 . ? C6 N2 1.337(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.529(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.530(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.520(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.544(4) . ? C13 C14 1.490(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.341(3) . ? C14 C15 1.404(4) . ? C15 C16 1.359(4) . ? C15 H15 0.9500 . ? C16 N3 1.334(3) . ? C16 H16 0.9500 . ? C17 C19 1.524(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.520(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.515(4) . ? C19 C21 1.549(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.494(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N6 1.345(3) . ? C22 C23 1.391(4) . ? C23 C24 1.366(4) . ? C23 H23 0.9500 . ? C24 N5 1.338(3) . ? C24 H24 0.9500 . ? C25 C26 1.521(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.512(4) . ? C26 C27 1.516(4) . ? C26 C29 1.548(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.495(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N12 1.350(3) . ? C30 C31 1.392(4) . ? C31 C32 1.371(4) . ? C31 H31 0.9500 . ? C32 N11 1.335(3) . ? C32 H32 0.9500 . ? C33 C36 1.543(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.524(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.524(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.543(5) . ? C37 C38 1.490(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N8 1.346(3) . ? C38 C39 1.399(4) . ? C39 C40 1.368(4) . ? C39 H39 0.9500 . ? C40 N7 1.340(3) . ? C40 H40 0.9500 . ? C41 C42 1.528(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.516(4) . ? C42 C43 1.535(4) . ? C42 C45 1.547(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.496(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N10 1.345(3) . ? C46 C47 1.395(3) . ? C47 C48 1.373(3) . ? C47 H47 0.9500 . ? C48 N9 1.335(3) . ? C48 H48 0.9500 . ? Co1 N14 1.883(5) . ? Co1 N13 1.956(5) . ? Co1 N12 2.068(2) . ? Co1 N8 2.0838(19) . ? Co1 N10 2.114(2) . ? Co1 S2B 2.4661(18) . ? Co1 S1B 2.484(2) . ? Co2 N13B 1.869(6) . ? Co2 N14B 1.875(6) . ? Co2 N6 2.077(2) . ? Co2 N1 2.091(2) . ? Co2 N4 2.115(2) . ? Co2 S1 2.4367(14) . ? Co2 S2 2.4439(14) . ? N1 N2 1.361(3) . ? N3 N4 1.378(3) . ? N5 N6 1.365(3) . ? N7 N8 1.362(3) . ? N9 N10 1.372(3) . ? N11 N12 1.365(3) . ? N13 C50 1.299(7) . ? N13 H13C 0.8800 . ? N14 C49 1.296(6) . ? N14 H14C 0.8800 . ? N13B C50B 1.301(8) . ? N13B H13D 0.8800 . ? N14B C49B 1.311(8) . ? N14B H14D 0.8800 . ? C49 C50 1.502(7) . ? C49 S1 1.707(5) . ? C50 S2 1.684(5) . ? C50B C49B 1.510(9) . ? C50B S2B 1.682(7) . ? C49B S1B 1.679(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 N11 B1 N9 109.3(2) . . ? N11 B1 N7 109.7(2) . . ? N9 B1 N7 107.2(2) . . ? N11 B1 H1 110.2 . . ? N9 B1 H1 110.2 . . ? N7 B1 H1 110.2 . . ? N3 B2 N5 109.8(2) . . ? N3 B2 N2 107.2(2) . . ? N5 B2 N2 109.7(2) . . ? N3 B2 H2 110.0 . . ? N5 B2 H2 110.0 . . ? N2 B2 H2 110.0 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C8 C2 C3 110.6(3) . . ? C8 C2 C7 109.9(4) . . ? C3 C2 C7 109.8(3) . . ? C8 C2 C1 108.7(3) . . ? C3 C2 C1 108.0(3) . . ? C7 C2 C1 109.8(4) . . ? C4 C3 C2 115.5(2) . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? N1 C4 C5 109.0(2) . . ? N1 C4 C3 122.4(2) . . ? C5 C4 C3 128.5(3) . . ? C6 C5 C4 106.1(2) . . ? C6 C5 H5 126.9 . . ? C4 C5 H5 126.9 . . ? N2 C6 C5 108.4(2) . . ? N2 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 H9A 109.5 . . ? C12 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C12 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 H10A 109.5 . . ? C12 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C12 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C11 C12 C9 108.8(3) . . ? C11 C12 C10 109.7(3) . . ? C9 C12 C10 108.9(2) . . ? C11 C12 C13 107.7(2) . . ? C9 C12 C13 111.6(3) . . ? C10 C12 C13 110.2(2) . . ? C14 C13 C12 116.6(2) . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? C12 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? N4 C14 C15 109.1(2) . . ? N4 C14 C13 123.3(2) . . ? C15 C14 C13 127.6(2) . . ? C16 C15 C14 105.9(2) . . ? C16 C15 H15 127.0 . . ? C14 C15 H15 127.0 . . ? N3 C16 C15 109.0(2) . . ? N3 C16 H16 125.5 . . ? C15 C16 H16 125.5 . . ? C19 C17 H17A 109.5 . . ? C19 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C19 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C18 109.3(3) . . ? C20 C19 C17 108.9(3) . . ? C18 C19 C17 109.2(2) . . ? C20 C19 C21 110.6(2) . . ? C18 C19 C21 111.5(2) . . ? C17 C19 C21 107.2(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C19 115.3(2) . . ? C22 C21 H21A 108.5 . . ? C19 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? C19 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? N6 C22 C23 109.3(2) . . ? N6 C22 C21 121.0(2) . . ? C23 C22 C21 129.7(2) . . ? C24 C23 C22 105.7(2) . . ? C24 C23 H23 127.2 . . ? C22 C23 H23 127.2 . . ? N5 C24 C23 108.8(2) . . ? N5 C24 H24 125.6 . . ? C23 C24 H24 125.6 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C27 109.1(3) . . ? C28 C26 C25 110.2(3) . . ? C27 C26 C25 108.8(2) . . ? C28 C26 C29 109.8(2) . . ? C27 C26 C29 111.1(2) . . ? C25 C26 C29 107.7(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C26 115.7(2) . . ? C30 C29 H29A 108.4 . . ? C26 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? C26 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? N12 C30 C31 109.4(2) . . ? N12 C30 C29 120.8(2) . . ? C31 C30 C29 129.8(2) . . ? C32 C31 C30 105.8(2) . . ? C32 C31 H31 127.1 . . ? C30 C31 H31 127.1 . . ? N11 C32 C31 108.3(2) . . ? N11 C32 H32 125.8 . . ? C31 C32 H32 125.8 . . ? C36 C33 H33A 109.5 . . ? C36 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C36 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 H34A 109.5 . . ? C36 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C36 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 C35 109.8(3) . . ? C34 C36 C37 111.1(3) . . ? C35 C36 C37 110.1(2) . . ? C34 C36 C33 109.5(3) . . ? C35 C36 C33 108.5(3) . . ? C37 C36 C33 108.0(3) . . ? C38 C37 C36 115.7(2) . . ? C38 C37 H37A 108.4 . . ? C36 C37 H37A 108.4 . . ? C38 C37 H37B 108.4 . . ? C36 C37 H37B 108.4 . . ? H37A C37 H37B 107.4 . . ? N8 C38 C39 108.8(2) . . ? N8 C38 C37 122.7(2) . . ? C39 C38 C37 128.5(2) . . ? C40 C39 C38 106.1(2) . . ? C40 C39 H39 126.9 . . ? C38 C39 H39 126.9 . . ? N7 C40 C39 108.2(2) . . ? N7 C40 H40 125.9 . . ? C39 C40 H40 125.9 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C41 109.3(3) . . ? C44 C42 C43 107.3(3) . . ? C41 C42 C43 110.3(3) . . ? C44 C42 C45 111.7(2) . . ? C41 C42 C45 107.4(3) . . ? C43 C42 C45 110.8(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C42 117.2(2) . . ? C46 C45 H45A 108.0 . . ? C42 C45 H45A 108.0 . . ? C46 C45 H45B 108.0 . . ? C42 C45 H45B 108.0 . . ? H45A C45 H45B 107.2 . . ? N10 C46 C47 109.8(2) . . ? N10 C46 C45 122.3(2) . . ? C47 C46 C45 127.9(2) . . ? C48 C47 C46 105.4(2) . . ? C48 C47 H47 127.3 . . ? C46 C47 H47 127.3 . . ? N9 C48 C47 108.8(2) . . ? N9 C48 H48 125.6 . . ? C47 C48 H48 125.6 . . ? N14 Co1 N13 78.5(2) . . ? N14 Co1 N12 111.75(17) . . ? N13 Co1 N12 103.12(18) . . ? N14 Co1 N8 154.44(17) . . ? N13 Co1 N8 90.88(17) . . ? N12 Co1 N8 93.21(8) . . ? N14 Co1 N10 99.78(16) . . ? N13 Co1 N10 167.38(18) . . ? N12 Co1 N10 89.17(8) . . ? N8 Co1 N10 85.49(7) . . ? N14 Co1 S2B 81.89(16) . . ? N13 Co1 S2B 5.89(19) . . ? N12 Co1 S2B 97.41(8) . . ? N8 Co1 S2B 89.76(7) . . ? N10 Co1 S2B 172.10(7) . . ? N14 Co1 S1B 4.07(18) . . ? N13 Co1 S1B 82.18(16) . . ? N12 Co1 S1B 112.85(7) . . ? N8 Co1 S1B 153.91(8) . . ? N10 Co1 S1B 95.82(7) . . ? S2B Co1 S1B 85.68(6) . . ? N13B Co2 N14B 79.4(3) . . ? N13B Co2 N6 106.6(2) . . ? N14B Co2 N6 111.8(2) . . ? N13B Co2 N1 90.35(19) . . ? N14B Co2 N1 154.5(2) . . ? N6 Co2 N1 93.40(8) . . ? N13B Co2 N4 163.4(2) . . ? N14B Co2 N4 98.8(2) . . ? N6 Co2 N4 89.43(8) . . ? N1 Co2 N4 84.44(8) . . ? N13B Co2 S1 82.18(19) . . ? N14B Co2 S1 3.4(2) . . ? N6 Co2 S1 112.95(7) . . ? N1 Co2 S1 153.65(7) . . ? N4 Co2 S1 95.57(6) . . ? N13B Co2 S2 9.0(2) . . ? N14B Co2 S2 83.7(2) . . ? N6 Co2 S2 97.72(6) . . ? N1 Co2 S2 89.57(6) . . ? N4 Co2 S2 170.94(7) . . ? S1 Co2 S2 86.79(4) . . ? C4 N1 N2 106.7(2) . . ? C4 N1 Co2 137.71(18) . . ? N2 N1 Co2 115.55(15) . . ? C6 N2 N1 109.7(2) . . ? C6 N2 B2 129.7(2) . . ? N1 N2 B2 119.6(2) . . ? C16 N3 N4 109.5(2) . . ? C16 N3 B2 127.4(2) . . ? N4 N3 B2 121.97(19) . . ? C14 N4 N3 106.57(19) . . ? C14 N4 Co2 139.00(17) . . ? N3 N4 Co2 113.22(15) . . ? C24 N5 N6 109.4(2) . . ? C24 N5 B2 130.0(2) . . ? N6 N5 B2 120.6(2) . . ? C22 N6 N5 106.8(2) . . ? C22 N6 Co2 137.59(18) . . ? N5 N6 Co2 115.42(15) . . ? C40 N7 N8 109.9(2) . . ? C40 N7 B1 129.3(2) . . ? N8 N7 B1 120.04(18) . . ? C38 N8 N7 106.95(19) . . ? C38 N8 Co1 137.71(18) . . ? N7 N8 Co1 115.31(14) . . ? C48 N9 N10 109.80(19) . . ? C48 N9 B1 128.0(2) . . ? N10 N9 B1 121.75(19) . . ? C46 N10 N9 106.23(19) . . ? C46 N10 Co1 139.64(16) . . ? N9 N10 Co1 113.50(14) . . ? C32 N11 N12 110.2(2) . . ? C32 N11 B1 129.7(2) . . ? N12 N11 B1 120.15(19) . . ? C30 N12 N11 106.2(2) . . ? C30 N12 Co1 137.77(17) . . ? N11 N12 Co1 115.96(15) . . ? C50 N13 Co1 117.8(4) . . ? C50 N13 H13C 121.1 . . ? Co1 N13 H13C 121.1 . . ? C49 N14 Co1 120.9(4) . . ? C49 N14 H14C 119.5 . . ? Co1 N14 H14C 119.5 . . ? C50B N13B Co2 121.7(5) . . ? C50B N13B H13D 119.1 . . ? Co2 N13B H13D 119.1 . . ? C49B N14B Co2 119.0(5) . . ? C49B N14B H14D 120.5 . . ? Co2 N14B H14D 120.5 . . ? N14 C49 C50 110.5(4) . . ? N14 C49 S1 127.2(4) . . ? C50 C49 S1 122.2(3) . . ? N13 C50 C49 110.6(4) . . ? N13 C50 S2 126.7(4) . . ? C49 C50 S2 122.7(4) . . ? C49 S1 Co2 103.12(18) . . ? C50 S2 Co2 103.00(18) . . ? N13B C50B C49B 107.8(6) . . ? N13B C50B S2B 128.5(6) . . ? C49B C50B S2B 123.6(5) . . ? N14B C49B C50B 111.1(6) . . ? N14B C49B S1B 126.4(6) . . ? C50B C49B S1B 122.5(5) . . ? C50B S2B Co1 103.1(3) . . ? C49B S1B Co1 103.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C2 C3 C4 68.8(4) . . . . ? C7 C2 C3 C4 -52.6(4) . . . . ? C1 C2 C3 C4 -172.3(3) . . . . ? C2 C3 C4 N1 89.8(3) . . . . ? C2 C3 C4 C5 -86.4(4) . . . . ? N1 C4 C5 C6 -0.6(3) . . . . ? C3 C4 C5 C6 176.0(3) . . . . ? C4 C5 C6 N2 0.7(3) . . . . ? C11 C12 C13 C14 -176.1(3) . . . . ? C9 C12 C13 C14 64.6(3) . . . . ? C10 C12 C13 C14 -56.5(3) . . . . ? C12 C13 C14 N4 114.5(3) . . . . ? C12 C13 C14 C15 -67.0(4) . . . . ? N4 C14 C15 C16 -0.4(3) . . . . ? C13 C14 C15 C16 -179.1(3) . . . . ? C14 C15 C16 N3 0.0(3) . . . . ? C20 C19 C21 C22 55.7(3) . . . . ? C18 C19 C21 C22 -66.2(3) . . . . ? C17 C19 C21 C22 174.4(2) . . . . ? C19 C21 C22 N6 -103.4(3) . . . . ? C19 C21 C22 C23 75.0(3) . . . . ? N6 C22 C23 C24 0.7(3) . . . . ? C21 C22 C23 C24 -177.9(2) . . . . ? C22 C23 C24 N5 -0.4(3) . . . . ? C28 C26 C29 C30 53.4(3) . . . . ? C27 C26 C29 C30 -67.5(3) . . . . ? C25 C26 C29 C30 173.5(2) . . . . ? C26 C29 C30 N12 -105.2(3) . . . . ? C26 C29 C30 C31 73.5(3) . . . . ? N12 C30 C31 C32 1.1(3) . . . . ? C29 C30 C31 C32 -177.7(2) . . . . ? C30 C31 C32 N11 -0.9(3) . . . . ? C34 C36 C37 C38 67.9(3) . . . . ? C35 C36 C37 C38 -53.8(3) . . . . ? C33 C36 C37 C38 -172.1(3) . . . . ? C36 C37 C38 N8 81.9(3) . . . . ? C36 C37 C38 C39 -96.0(3) . . . . ? N8 C38 C39 C40 -0.3(3) . . . . ? C37 C38 C39 C40 177.8(3) . . . . ? C38 C39 C40 N7 0.0(3) . . . . ? C44 C42 C45 C46 67.2(3) . . . . ? C41 C42 C45 C46 -172.9(3) . . . . ? C43 C42 C45 C46 -52.4(3) . . . . ? C42 C45 C46 N10 110.5(3) . . . . ? C42 C45 C46 C47 -70.2(3) . . . . ? N10 C46 C47 C48 0.1(3) . . . . ? C45 C46 C47 C48 -179.3(2) . . . . ? C46 C47 C48 N9 -0.3(3) . . . . ? C5 C4 N1 N2 0.3(3) . . . . ? C3 C4 N1 N2 -176.6(2) . . . . ? C5 C4 N1 Co2 -177.7(2) . . . . ? C3 C4 N1 Co2 5.4(4) . . . . ? N13B Co2 N1 C4 38.1(3) . . . . ? N14B Co2 N1 C4 -27.3(6) . . . . ? N6 Co2 N1 C4 144.8(3) . . . . ? N4 Co2 N1 C4 -126.1(3) . . . . ? S1 Co2 N1 C4 -34.8(3) . . . . ? S2 Co2 N1 C4 47.1(3) . . . . ? N13B Co2 N1 N2 -139.8(3) . . . . ? N14B Co2 N1 N2 154.8(5) . . . . ? N6 Co2 N1 N2 -33.14(17) . . . . ? N4 Co2 N1 N2 55.95(17) . . . . ? S1 Co2 N1 N2 147.28(14) . . . . ? S2 Co2 N1 N2 -130.86(16) . . . . ? C5 C6 N2 N1 -0.5(3) . . . . ? C5 C6 N2 B2 -168.4(3) . . . . ? C4 N1 N2 C6 0.1(3) . . . . ? Co2 N1 N2 C6 178.61(17) . . . . ? C4 N1 N2 B2 169.4(2) . . . . ? Co2 N1 N2 B2 -12.0(3) . . . . ? N3 B2 N2 C6 114.1(3) . . . . ? N5 B2 N2 C6 -126.7(3) . . . . ? N3 B2 N2 N1 -52.8(3) . . . . ? N5 B2 N2 N1 66.4(3) . . . . ? C15 C16 N3 N4 0.3(3) . . . . ? C15 C16 N3 B2 168.0(3) . . . . ? N5 B2 N3 C16 134.7(3) . . . . ? N2 B2 N3 C16 -106.2(3) . . . . ? N5 B2 N3 N4 -59.1(3) . . . . ? N2 B2 N3 N4 60.0(3) . . . . ? C15 C14 N4 N3 0.6(3) . . . . ? C13 C14 N4 N3 179.3(2) . . . . ? C15 C14 N4 Co2 -165.3(2) . . . . ? C13 C14 N4 Co2 13.5(4) . . . . ? C16 N3 N4 C14 -0.6(3) . . . . ? B2 N3 N4 C14 -169.0(2) . . . . ? C16 N3 N4 Co2 169.36(17) . . . . ? B2 N3 N4 Co2 1.0(3) . . . . ? N13B Co2 N4 C14 43.7(7) . . . . ? N14B Co2 N4 C14 -38.6(3) . . . . ? N6 Co2 N4 C14 -150.6(3) . . . . ? N1 Co2 N4 C14 116.0(3) . . . . ? S1 Co2 N4 C14 -37.6(3) . . . . ? N13B Co2 N4 N3 -121.5(7) . . . . ? N14B Co2 N4 N3 156.2(3) . . . . ? N6 Co2 N4 N3 44.24(16) . . . . ? N1 Co2 N4 N3 -49.23(16) . . . . ? S1 Co2 N4 N3 157.24(15) . . . . ? C23 C24 N5 N6 -0.1(3) . . . . ? C23 C24 N5 B2 -179.0(2) . . . . ? N3 B2 N5 C24 -125.2(3) . . . . ? N2 B2 N5 C24 117.2(3) . . . . ? N3 B2 N5 N6 56.0(3) . . . . ? N2 B2 N5 N6 -61.6(3) . . . . ? C23 C22 N6 N5 -0.8(3) . . . . ? C21 C22 N6 N5 177.9(2) . . . . ? C23 C22 N6 Co2 173.02(18) . . . . ? C21 C22 N6 Co2 -8.2(4) . . . . ? C24 N5 N6 C22 0.6(3) . . . . ? B2 N5 N6 C22 179.6(2) . . . . ? C24 N5 N6 Co2 -174.81(16) . . . . ? B2 N5 N6 Co2 4.2(3) . . . . ? N13B Co2 N6 C22 -45.0(3) . . . . ? N14B Co2 N6 C22 40.0(3) . . . . ? N1 Co2 N6 C22 -136.4(2) . . . . ? N4 Co2 N6 C22 139.2(2) . . . . ? S1 Co2 N6 C22 43.4(3) . . . . ? S2 Co2 N6 C22 -46.3(2) . . . . ? N13B Co2 N6 N5 128.5(2) . . . . ? N14B Co2 N6 N5 -146.6(3) . . . . ? N1 Co2 N6 N5 37.09(17) . . . . ? N4 Co2 N6 N5 -47.31(16) . . . . ? S1 Co2 N6 N5 -143.12(14) . . . . ? S2 Co2 N6 N5 127.11(15) . . . . ? C39 C40 N7 N8 0.4(3) . . . . ? C39 C40 N7 B1 -169.9(2) . . . . ? N11 B1 N7 C40 -125.0(2) . . . . ? N9 B1 N7 C40 116.4(3) . . . . ? N11 B1 N7 N8 65.6(3) . . . . ? N9 B1 N7 N8 -53.0(3) . . . . ? C39 C38 N8 N7 0.5(3) . . . . ? C37 C38 N8 N7 -177.7(2) . . . . ? C39 C38 N8 Co1 -176.91(19) . . . . ? C37 C38 N8 Co1 4.8(4) . . . . ? C40 N7 N8 C38 -0.6(3) . . . . ? B1 N7 N8 C38 170.7(2) . . . . ? C40 N7 N8 Co1 177.53(15) . . . . ? B1 N7 N8 Co1 -11.2(3) . . . . ? N14 Co1 N8 C38 -24.6(5) . . . . ? N13 Co1 N8 C38 40.0(3) . . . . ? N12 Co1 N8 C38 143.2(2) . . . . ? N10 Co1 N8 C38 -127.9(3) . . . . ? S2B Co1 N8 C38 45.8(2) . . . . ? S1B Co1 N8 C38 -33.9(3) . . . . ? N14 Co1 N8 N7 158.1(4) . . . . ? N13 Co1 N8 N7 -137.3(2) . . . . ? N12 Co1 N8 N7 -34.14(16) . . . . ? N10 Co1 N8 N7 54.77(16) . . . . ? S2B Co1 N8 N7 -131.55(16) . . . . ? S1B Co1 N8 N7 148.81(15) . . . . ? C47 C48 N9 N10 0.4(3) . . . . ? C47 C48 N9 B1 172.6(2) . . . . ? N11 B1 N9 C48 130.2(2) . . . . ? N7 B1 N9 C48 -110.9(3) . . . . ? N11 B1 N9 N10 -58.5(3) . . . . ? N7 B1 N9 N10 60.4(3) . . . . ? C47 C46 N10 N9 0.1(3) . . . . ? C45 C46 N10 N9 179.5(2) . . . . ? C47 C46 N10 Co1 -169.48(18) . . . . ? C45 C46 N10 Co1 9.9(4) . . . . ? C48 N9 N10 C46 -0.3(3) . . . . ? B1 N9 N10 C46 -173.1(2) . . . . ? C48 N9 N10 Co1 172.35(15) . . . . ? B1 N9 N10 Co1 -0.4(3) . . . . ? N14 Co1 N10 C46 -33.7(3) . . . . ? N13 Co1 N10 C46 47.4(8) . . . . ? N12 Co1 N10 C46 -145.7(2) . . . . ? N8 Co1 N10 C46 121.0(2) . . . . ? S1B Co1 N10 C46 -32.8(2) . . . . ? N14 Co1 N10 N9 157.1(2) . . . . ? N13 Co1 N10 N9 -121.8(7) . . . . ? N12 Co1 N10 N9 45.19(15) . . . . ? N8 Co1 N10 N9 -48.09(15) . . . . ? S1B Co1 N10 N9 158.08(15) . . . . ? C31 C32 N11 N12 0.4(3) . . . . ? C31 C32 N11 B1 -179.9(2) . . . . ? N9 B1 N11 C32 -122.4(3) . . . . ? N7 B1 N11 C32 120.2(3) . . . . ? N9 B1 N11 N12 57.2(3) . . . . ? N7 B1 N11 N12 -60.1(3) . . . . ? C31 C30 N12 N11 -0.8(3) . . . . ? C29 C30 N12 N11 178.1(2) . . . . ? C31 C30 N12 Co1 176.28(19) . . . . ? C29 C30 N12 Co1 -4.8(4) . . . . ? C32 N11 N12 C30 0.2(3) . . . . ? B1 N11 N12 C30 -179.5(2) . . . . ? C32 N11 N12 Co1 -177.60(16) . . . . ? B1 N11 N12 Co1 2.7(3) . . . . ? N14 Co1 N12 C30 36.0(3) . . . . ? N13 Co1 N12 C30 -46.7(3) . . . . ? N8 Co1 N12 C30 -138.3(2) . . . . ? N10 Co1 N12 C30 136.2(2) . . . . ? S2B Co1 N12 C30 -48.2(2) . . . . ? S1B Co1 N12 C30 40.3(3) . . . . ? N14 Co1 N12 N11 -147.1(2) . . . . ? N13 Co1 N12 N11 130.2(2) . . . . ? N8 Co1 N12 N11 38.58(16) . . . . ? N10 Co1 N12 N11 -46.86(16) . . . . ? S2B Co1 N12 N11 128.76(16) . . . . ? S1B Co1 N12 N11 -142.82(15) . . . . ? N14 Co1 N13 C50 7.4(5) . . . . ? N12 Co1 N13 C50 117.3(5) . . . . ? N8 Co1 N13 C50 -149.2(5) . . . . ? N10 Co1 N13 C50 -76.1(10) . . . . ? S2B Co1 N13 C50 132(2) . . . . ? S1B Co1 N13 C50 5.5(5) . . . . ? N13 Co1 N14 C49 1.5(5) . . . . ? N12 Co1 N14 C49 -98.2(5) . . . . ? N8 Co1 N14 C49 68.7(7) . . . . ? N10 Co1 N14 C49 168.8(5) . . . . ? S2B Co1 N14 C49 -3.4(5) . . . . ? S1B Co1 N14 C49 155(3) . . . . ? N14B Co2 N13B C50B 3.3(7) . . . . ? N6 Co2 N13B C50B 113.0(7) . . . . ? N1 Co2 N13B C50B -153.3(7) . . . . ? N4 Co2 N13B C50B -81.9(10) . . . . ? S1 Co2 N13B C50B 1.3(7) . . . . ? S2 Co2 N13B C50B 121.7(16) . . . . ? N13B Co2 N14B C49B 4.1(7) . . . . ? N6 Co2 N14B C49B -99.7(7) . . . . ? N1 Co2 N14B C49B 71.8(9) . . . . ? N4 Co2 N14B C49B 167.4(6) . . . . ? S1 Co2 N14B C49B 150(5) . . . . ? S2 Co2 N14B C49B -3.8(7) . . . . ? Co1 N14 C49 C50 -8.5(7) . . . . ? Co1 N14 C49 S1 168.2(4) . . . . ? Co1 N13 C50 C49 -13.2(7) . . . . ? Co1 N13 C50 S2 165.2(4) . . . . ? N14 C49 C50 N13 13.5(8) . . . . ? S1 C49 C50 N13 -163.3(5) . . . . ? N14 C49 C50 S2 -165.0(5) . . . . ? S1 C49 C50 S2 18.2(8) . . . . ? N14 C49 S1 Co2 174.8(6) . . . . ? C50 C49 S1 Co2 -8.9(6) . . . . ? N13B Co2 S1 C49 7.6(3) . . . . ? N14B Co2 S1 C49 -26(4) . . . . ? N6 Co2 S1 C49 -97.2(2) . . . . ? N1 Co2 S1 C49 82.3(3) . . . . ? N4 Co2 S1 C49 171.0(2) . . . . ? S2 Co2 S1 C49 -0.2(2) . . . . ? N13 C50 S2 Co2 166.3(5) . . . . ? C49 C50 S2 Co2 -15.5(6) . . . . ? N13B Co2 S2 C50 -51.6(13) . . . . ? N14B Co2 S2 C50 8.7(3) . . . . ? N6 Co2 S2 C50 120.0(2) . . . . ? N1 Co2 S2 C50 -146.6(2) . . . . ? S1 Co2 S2 C50 7.2(2) . . . . ? Co2 N13B C50B C49B -8.4(10) . . . . ? Co2 N13B C50B S2B 169.1(5) . . . . ? Co2 N14B C49B C50B -9.3(10) . . . . ? Co2 N14B C49B S1B 167.7(5) . . . . ? N13B C50B C49B N14B 10.7(11) . . . . ? S2B C50B C49B N14B -166.9(7) . . . . ? N13B C50B C49B S1B -166.4(7) . . . . ? S2B C50B C49B S1B 16.0(12) . . . . ? N13B C50B S2B Co1 169.8(8) . . . . ? C49B C50B S2B Co1 -13.1(8) . . . . ? N14 Co1 S2B C50B 7.2(4) . . . . ? N13 Co1 S2B C50B -47.6(19) . . . . ? N12 Co1 S2B C50B 118.2(3) . . . . ? N8 Co1 S2B C50B -148.6(3) . . . . ? S1B Co1 S2B C50B 5.7(3) . . . . ? N14B C49B S1B Co1 175.1(8) . . . . ? C50B C49B S1B Co1 -8.2(8) . . . . ? N14 Co1 S1B C49B -21(3) . . . . ? N13 Co1 S1B C49B 5.2(4) . . . . ? N12 Co1 S1B C49B -95.8(3) . . . . ? N8 Co1 S1B C49B 81.0(4) . . . . ? N10 Co1 S1B C49B 172.6(3) . . . . ? S2B Co1 S1B C49B 0.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.766 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.063 data_06mz112m _database_code_depnum_ccdc_archive 'CCDC 881843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H82 B2 Co N14 Ni S2, C2 H3 N' _chemical_formula_sum 'C55 H85 B2 Co N15 Ni S2' _chemical_formula_weight 1159.76 _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' S S 0.1246 0.1234 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2783(12) _cell_length_b 13.6323(13) _cell_length_c 20.460(2) _cell_angle_alpha 98.437(2) _cell_angle_beta 97.964(2) _cell_angle_gamma 116.203(2) _cell_volume 2958.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5885 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 30.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1234 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details 'SADABS in SAINT+ (Bruker, 2003)' _exptl_special_details ; Comments: The central dithiaoxamide ligand is flip disordered with an occupancy ratio of 0.835(2) to 0.165(2). The major orientation is bonded to Ni via the sulfur atoms and to Co via the nitrogen atoms. Associated with this disorder is a disorder of a solvate acetonitrile molecule hydrogen bonded to one of the N-H groups. The atoms of the minor components were restraint to resemble the geometry of the major component within a standard deviation of 0.02, and equivalent atoms were restraint to have identical anisotropic displacement parameters. One of the tert-butyl groups is rotationally disordered. It was refined as statically disordered over two positions with an occupancy ratio of 0.34(2) to 0.66(2). Equivalent C-C distances were restraint to be similar for both orientations within a standard deviation of 0.02 Angstrom, and the anisotropic displacement parameters of the methyl carbon atoms were restrained to be isotropic within a standard deviation of 0.02 Angstrom squared. Treatment of hydrogen atoms: All hydrogen atoms were placed in calculated positions and all hydrogen atoms were refined with an isotropic displacement parameter 1.5 (methyl) or 1.2 (all others) times that of the adjacent carbon atom. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 25950 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12057 _reflns_number_gt 9153 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.630 (Bruker, 1997-2002)' _computing_cell_refinement 'SAINT+ 6.45 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0416P)^2^+7.6707P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12057 _refine_ls_number_parameters 737 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.1032(5) 0.0587(4) 0.6522(3) 0.0282(11) Uani 1 1 d . . . H1B H 0.0122 0.0243 0.6308 0.034 Uiso 1 1 calc R . . B2 B 1.1980(4) 0.5401(4) 0.8972(2) 0.0246(10) Uani 1 1 d . B . H2B H 1.2819 0.5732 0.9287 0.030 Uiso 1 1 calc R . . C1 C 0.0510(4) 0.1389(4) 0.7586(2) 0.0277(10) Uani 1 1 d . . . H1 H -0.0334 0.1179 0.7395 0.033 Uiso 1 1 calc R . . C2 C 0.1126(4) 0.1912(4) 0.8250(2) 0.0278(9) Uani 1 1 d . . . H2 H 0.0800 0.2139 0.8603 0.033 Uiso 1 1 calc R . . C3 C 0.2331(4) 0.2043(3) 0.8300(2) 0.0228(9) Uani 1 1 d . . . C4 C 0.3350(4) 0.2463(3) 0.8931(2) 0.0250(9) Uani 1 1 d . . . H4 H 0.4160 0.2960 0.8828 0.030 Uiso 1 1 calc R . . C5 C 0.3121(4) 0.3139(4) 0.9512(2) 0.0321(10) Uani 1 1 d . . . H5A H 0.3104 0.3800 0.9375 0.039 Uiso 1 1 calc R . . H5B H 0.2297 0.2668 0.9600 0.039 Uiso 1 1 calc R . . C6 C 0.4126(5) 0.3538(4) 1.0162(2) 0.0350(11) Uani 1 1 d . . . H6A H 0.4942 0.4062 1.0087 0.042 Uiso 1 1 calc R . . H6B H 0.3929 0.3948 1.0528 0.042 Uiso 1 1 calc R . . C7 C 0.4209(4) 0.2545(4) 1.0378(2) 0.0317(10) Uani 1 1 d . . . H7A H 0.4896 0.2824 1.0785 0.038 Uiso 1 1 calc R . . H7B H 0.3422 0.2061 1.0498 0.038 Uiso 1 1 calc R . . C8 C 0.4438(4) 0.1863(4) 0.9811(2) 0.0335(10) Uani 1 1 d . . . H8A H 0.4444 0.1201 0.9953 0.040 Uiso 1 1 calc R . . H8B H 0.5267 0.2326 0.9725 0.040 Uiso 1 1 calc R . . C9 C 0.3445(4) 0.1468(4) 0.9161(2) 0.0327(10) Uani 1 1 d . . . H9A H 0.2628 0.0942 0.9235 0.039 Uiso 1 1 calc R . . H9B H 0.3646 0.1056 0.8798 0.039 Uiso 1 1 calc R . . C10 C 0.1454(4) 0.1596(4) 0.5518(2) 0.0333(10) Uani 1 1 d . . . H10 H 0.0623 0.1273 0.5258 0.040 Uiso 1 1 calc R . . C11 C 0.2496(5) 0.2355(4) 0.5352(2) 0.0354(11) Uani 1 1 d . . . H11 H 0.2532 0.2652 0.4959 0.042 Uiso 1 1 calc R . . C12 C 0.3500(4) 0.2602(4) 0.5886(2) 0.0293(10) Uani 1 1 d . . . C13 C 0.4849(4) 0.3371(4) 0.5960(2) 0.0280(10) Uani 1 1 d . . . H13 H 0.5327 0.3240 0.6344 0.034 Uiso 1 1 calc R . . C14 C 0.5293(5) 0.3139(4) 0.5329(3) 0.0433(13) Uani 1 1 d . . . H14A H 0.5120 0.2345 0.5225 0.052 Uiso 1 1 calc R . . H14B H 0.4826 0.3257 0.4940 0.052 Uiso 1 1 calc R . . C15 C 0.6668(5) 0.3895(4) 0.5421(3) 0.0482(14) Uani 1 1 d . . . H15A H 0.6922 0.3738 0.4996 0.058 Uiso 1 1 calc R . . H15B H 0.7138 0.3732 0.5785 0.058 Uiso 1 1 calc R . . C16 C 0.6993(5) 0.5125(4) 0.5603(3) 0.0435(13) Uani 1 1 d . . . H16A H 0.7909 0.5595 0.5695 0.052 Uiso 1 1 calc R . . H16B H 0.6610 0.5313 0.5215 0.052 Uiso 1 1 calc R . . C17 C 0.6537(5) 0.5383(4) 0.6216(3) 0.0483(14) Uani 1 1 d . . . H17A H 0.6697 0.6174 0.6298 0.058 Uiso 1 1 calc R . . H17B H 0.7012 0.5301 0.6618 0.058 Uiso 1 1 calc R . . C18 C 0.5144(5) 0.4612(4) 0.6137(3) 0.0417(12) Uani 1 1 d . . . H18A H 0.4656 0.4759 0.5773 0.050 Uiso 1 1 calc R . . H18B H 0.4899 0.4773 0.6565 0.050 Uiso 1 1 calc R . . C19 C 0.0743(5) -0.1451(4) 0.6270(2) 0.0376(11) Uani 1 1 d . . . H19 H -0.0118 -0.1830 0.6052 0.045 Uiso 1 1 calc R . . C20 C 0.1488(5) -0.1939(4) 0.6377(3) 0.0411(12) Uani 1 1 d . . . H20 H 0.1252 -0.2717 0.6247 0.049 Uiso 1 1 calc R . . C21 C 0.2662(4) -0.1076(4) 0.6712(2) 0.0315(10) Uani 1 1 d . . . C22 C 0.3807(4) -0.1199(4) 0.6934(2) 0.0320(10) Uani 1 1 d . . . H22 H 0.4456 -0.0485 0.7257 0.038 Uiso 1 1 calc R . . C23 C 0.3490(5) -0.2161(4) 0.7300(3) 0.0466(13) Uani 1 1 d . . . H23A H 0.3241 -0.1966 0.7720 0.056 Uiso 1 1 calc R . . H23B H 0.2771 -0.2850 0.7005 0.056 Uiso 1 1 calc R . . C24 C 0.4583(6) -0.2400(5) 0.7483(4) 0.0586(16) Uani 1 1 d . . . H24A H 0.5263 -0.1749 0.7827 0.070 Uiso 1 1 calc R . . H24B H 0.4312 -0.3063 0.7685 0.070 Uiso 1 1 calc R . . C25 C 0.5067(6) -0.2620(5) 0.6869(4) 0.072(2) Uani 1 1 d . . . H25A H 0.5800 -0.2734 0.7008 0.087 Uiso 1 1 calc R . . H25B H 0.4414 -0.3313 0.6542 0.087 Uiso 1 1 calc R . . C26 C 0.5429(5) -0.1646(6) 0.6539(3) 0.065(2) Uani 1 1 d . . . H26A H 0.5740 -0.1803 0.6136 0.078 Uiso 1 1 calc R . . H26B H 0.6116 -0.0966 0.6860 0.078 Uiso 1 1 calc R . . C27 C 0.4332(5) -0.1420(5) 0.6323(3) 0.0472(14) Uani 1 1 d . . . H27A H 0.3668 -0.2077 0.5975 0.057 Uiso 1 1 calc R . . H27B H 0.4613 -0.0759 0.6119 0.057 Uiso 1 1 calc R . . C30 C 1.2451(4) 0.7460(3) 0.8990(2) 0.0259(9) Uani 1 1 d . B . H30 H 1.3271 0.7827 0.9270 0.031 Uiso 1 1 calc R . . C31 C 1.1859(4) 0.7980(4) 0.8684(2) 0.0270(9) Uani 1 1 d . . . H31 H 1.2177 0.8762 0.8708 0.032 Uiso 1 1 calc R . . C32 C 1.0685(4) 0.7110(3) 0.8326(2) 0.0246(9) Uani 1 1 d . . . C33 C 0.9693(4) 0.7202(4) 0.7865(2) 0.0333(11) Uani 1 1 d . A . H33A H 0.9011 0.6430 0.7657 0.040 Uiso 1 1 calc R . . H33B H 1.0050 0.7519 0.7493 0.040 Uiso 1 1 calc R . . C34 C 0.9109(4) 0.7905(4) 0.8167(2) 0.0372(11) Uani 1 1 d D . . C35A C 1.006(2) 0.9143(14) 0.8379(14) 0.050(7) Uani 0.34(2) 1 d PDU A 3 H35A H 0.9667 0.9578 0.8563 0.075 Uiso 0.34(2) 1 calc PR A 3 H35B H 1.0356 0.9396 0.7983 0.075 Uiso 0.34(2) 1 calc PR A 3 H35C H 1.0763 0.9254 0.8726 0.075 Uiso 0.34(2) 1 calc PR A 3 C36A C 0.7933(16) 0.7730(18) 0.7718(10) 0.047(6) Uani 0.34(2) 1 d PDU A 3 H36A H 0.7265 0.6972 0.7684 0.070 Uiso 0.34(2) 1 calc PR A 3 H36B H 0.8072 0.7818 0.7265 0.070 Uiso 0.34(2) 1 calc PR A 3 H36C H 0.7694 0.8287 0.7912 0.070 Uiso 0.34(2) 1 calc PR A 3 C37A C 0.874(2) 0.758(2) 0.8845(10) 0.054(6) Uani 0.34(2) 1 d PDU A 3 H37A H 0.9496 0.7800 0.9189 0.082 Uiso 0.34(2) 1 calc PR A 3 H37B H 0.8199 0.6770 0.8757 0.082 Uiso 0.34(2) 1 calc PR A 3 H37C H 0.8297 0.7980 0.9010 0.082 Uiso 0.34(2) 1 calc PR A 3 C35B C 1.0063(10) 0.9034(8) 0.8618(6) 0.037(3) Uani 0.66(2) 1 d PDU A 4 H35D H 0.9661 0.9505 0.8712 0.055 Uiso 0.66(2) 1 calc PR A 4 H35E H 1.0731 0.9404 0.8388 0.055 Uiso 0.66(2) 1 calc PR A 4 H35F H 1.0414 0.8928 0.9045 0.055 Uiso 0.66(2) 1 calc PR A 4 C36B C 0.8501(14) 0.8176(10) 0.7538(5) 0.057(4) Uani 0.66(2) 1 d PDU A 4 H36D H 0.7882 0.7473 0.7218 0.085 Uiso 0.66(2) 1 calc PR A 4 H36E H 0.9149 0.8611 0.7313 0.085 Uiso 0.66(2) 1 calc PR A 4 H36F H 0.8093 0.8615 0.7690 0.085 Uiso 0.66(2) 1 calc PR A 4 C37B C 0.8146(12) 0.7228(8) 0.8500(8) 0.062(4) Uani 0.66(2) 1 d PDU A 4 H37D H 0.8539 0.7090 0.8902 0.094 Uiso 0.66(2) 1 calc PR A 4 H37E H 0.7561 0.6508 0.8183 0.094 Uiso 0.66(2) 1 calc PR A 4 H37F H 0.7694 0.7634 0.8637 0.094 Uiso 0.66(2) 1 calc PR A 4 C38 C 1.1114(4) 0.4379(4) 0.9902(2) 0.0279(9) Uani 1 1 d . B . H38 H 1.1861 0.4723 1.0246 0.033 Uiso 1 1 calc R . . C39 C 0.9977(4) 0.3578(4) 0.9952(2) 0.0299(10) Uani 1 1 d . . . H39 H 0.9788 0.3267 1.0333 0.036 Uiso 1 1 calc R . . C40 C 0.9154(4) 0.3310(3) 0.9334(2) 0.0255(9) Uani 1 1 d . . . C41 C 0.7796(4) 0.2496(4) 0.9133(2) 0.0281(10) Uani 1 1 d . . . H41A H 0.7415 0.2681 0.8743 0.034 Uiso 1 1 calc R . . H41B H 0.7417 0.2612 0.9514 0.034 Uiso 1 1 calc R . . C42 C 0.7436(4) 0.1222(4) 0.8935(2) 0.0333(10) Uani 1 1 d . . . C43 C 0.8133(6) 0.0898(4) 0.9472(3) 0.0462(13) Uani 1 1 d . . . H43A H 0.7841 0.0086 0.9349 0.069 Uiso 1 1 calc R . . H43B H 0.7975 0.1102 0.9915 0.069 Uiso 1 1 calc R . . H43C H 0.9030 0.1300 0.9494 0.069 Uiso 1 1 calc R . . C44 C 0.6034(5) 0.0555(4) 0.8878(3) 0.0479(14) Uani 1 1 d . . . H44A H 0.5761 -0.0249 0.8718 0.072 Uiso 1 1 calc R . . H44B H 0.5590 0.0794 0.8555 0.072 Uiso 1 1 calc R . . H44C H 0.5852 0.0691 0.9324 0.072 Uiso 1 1 calc R . . C45 C 0.7728(5) 0.0945(4) 0.8254(2) 0.0356(11) Uani 1 1 d . . . H45A H 0.8587 0.1482 0.8260 0.053 Uiso 1 1 calc R . . H45B H 0.7153 0.0993 0.7892 0.053 Uiso 1 1 calc R . . H45C H 0.7632 0.0181 0.8170 0.053 Uiso 1 1 calc R . . C46 C 1.2944(4) 0.4683(4) 0.8077(2) 0.0271(9) Uani 1 1 d . B . H46 H 1.3757 0.4949 0.8348 0.032 Uiso 1 1 calc R . . C47 C 1.2536(4) 0.4145(4) 0.7410(2) 0.0286(10) Uani 1 1 d . . . H47 H 1.3001 0.3962 0.7126 0.034 Uiso 1 1 calc R . . C48 C 1.1300(4) 0.3917(3) 0.7227(2) 0.0260(9) Uani 1 1 d . . . C49 C 1.0413(4) 0.3342(4) 0.6546(2) 0.0291(10) Uani 1 1 d . . . H49A H 0.9563 0.2908 0.6615 0.035 Uiso 1 1 calc R . . H49B H 1.0642 0.2799 0.6307 0.035 Uiso 1 1 calc R . . C50 C 1.0382(5) 0.4134(4) 0.6086(2) 0.0336(11) Uani 1 1 d . . . C51 C 0.9466(5) 0.3407(5) 0.5415(2) 0.0456(13) Uani 1 1 d . . . H51A H 0.8634 0.2981 0.5497 0.068 Uiso 1 1 calc R . . H51B H 0.9737 0.2884 0.5207 0.068 Uiso 1 1 calc R . . H51C H 0.9437 0.3888 0.5108 0.068 Uiso 1 1 calc R . . C52 C 1.1660(5) 0.4811(4) 0.5958(3) 0.0429(12) Uani 1 1 d . . . H52A H 1.1615 0.5286 0.5650 0.064 Uiso 1 1 calc R . . H52B H 1.1947 0.4299 0.5751 0.064 Uiso 1 1 calc R . . H52C H 1.2247 0.5286 0.6389 0.064 Uiso 1 1 calc R . . C53 C 0.9939(5) 0.4926(4) 0.6417(2) 0.0350(11) Uani 1 1 d . . . H53A H 0.9861 0.5389 0.6108 0.052 Uiso 1 1 calc R . . H53B H 1.0544 0.5414 0.6841 0.052 Uiso 1 1 calc R . . H53C H 0.9126 0.4485 0.6517 0.052 Uiso 1 1 calc R . . Co1 Co 0.93584(5) 0.43316(5) 0.80191(3) 0.02303(15) Uani 1 1 d . . . N1 N 0.2441(3) 0.1642(3) 0.76858(17) 0.0237(7) Uani 1 1 d . B . N2 N 0.1306(3) 0.1225(3) 0.72529(18) 0.0260(8) Uani 1 1 d . . . N3 N 0.3066(3) 0.1998(3) 0.63412(18) 0.0251(8) Uani 1 1 d . B . N4 N 0.1808(3) 0.1385(3) 0.61124(18) 0.0275(8) Uani 1 1 d . . . N5 N 0.2639(3) -0.0085(3) 0.68005(18) 0.0275(8) Uani 1 1 d . B . N6 N 0.1438(3) -0.0339(3) 0.65254(18) 0.0293(8) Uani 1 1 d . . . N16 N 0.7822(5) 0.0776(5) 0.6250(3) 0.0496(14) Uani 0.835(2) 1 d PD B 1 C54 C 0.7479(5) 0.0521(5) 0.5678(3) 0.0350(13) Uani 0.835(2) 1 d PD B 1 C55 C 0.7140(12) 0.0252(8) 0.4956(6) 0.058(3) Uani 0.835(2) 1 d PD B 1 H55A H 0.7678 0.0894 0.4789 0.086 Uiso 0.835(2) 1 calc PR B 1 H55B H 0.6269 0.0079 0.4806 0.086 Uiso 0.835(2) 1 calc PR B 1 H55C H 0.7241 -0.0403 0.4777 0.086 Uiso 0.835(2) 1 calc PR B 1 N7 N 0.7952(5) 0.2917(4) 0.7350(3) 0.0274(8) Uani 0.835(2) 1 d PD B 1 H7 H 0.8124 0.2462 0.7084 0.033 Uiso 0.835(2) 1 calc PR B 1 N8 N 0.7797(4) 0.4469(4) 0.8067(2) 0.0274(8) Uani 0.835(2) 1 d PD B 1 H8 H 0.7856 0.5095 0.8298 0.033 Uiso 0.835(2) 1 calc PR B 1 C28 C 0.6822(4) 0.2704(4) 0.7326(3) 0.0198(8) Uani 0.835(2) 1 d PD B 1 C29 C 0.6722(4) 0.3650(4) 0.7765(3) 0.0198(8) Uani 0.835(2) 1 d PD B 1 S1 S 0.55145(12) 0.15069(11) 0.68723(7) 0.0255(3) Uani 0.835(2) 1 d PD B 1 S2 S 0.52904(14) 0.35364(11) 0.78258(9) 0.0255(3) Uani 0.835(2) 1 d PD B 1 N17 N 0.592(2) 0.087(2) 0.5515(14) 0.0496(14) Uani 0.165(2) 1 d PD B 2 C56 C 0.651(2) 0.063(2) 0.5235(15) 0.0350(13) Uani 0.165(2) 1 d PD B 2 C57 C 0.694(7) -0.001(6) 0.484(4) 0.058(3) Uani 0.165(2) 1 d PD B 2 H57A H 0.7445 0.0442 0.4558 0.086 Uiso 0.165(2) 1 calc PR B 2 H57B H 0.6217 -0.0685 0.4541 0.086 Uiso 0.165(2) 1 calc PR B 2 H57C H 0.7437 -0.0234 0.5135 0.086 Uiso 0.165(2) 1 calc PR B 2 S1B S 0.7856(9) 0.2685(8) 0.7190(5) 0.0255(3) Uani 0.165(2) 1 d PD B 2 S2B S 0.7511(7) 0.4593(6) 0.8269(4) 0.0255(3) Uani 0.165(2) 1 d PD B 2 C29B C 0.6239(17) 0.3371(16) 0.7760(13) 0.0198(8) Uani 0.165(2) 1 d PD B 2 N8B N 0.513(2) 0.3222(18) 0.7773(16) 0.0274(8) Uani 0.165(2) 1 d PD B 2 H8B1 H 0.4961 0.3715 0.8000 0.033 Uiso 0.165(2) 1 calc PR B 2 N7B N 0.5236(19) 0.1660(16) 0.7050(11) 0.0274(8) Uani 0.165(2) 1 d PD B 2 H7B1 H 0.5137 0.1042 0.6785 0.033 Uiso 0.165(2) 1 calc PR B 2 C28B C 0.6372(15) 0.2442(19) 0.7289(15) 0.0198(8) Uani 0.165(2) 1 d PD B 2 N9 N 1.0584(3) 0.6114(3) 0.84159(17) 0.0206(7) Uani 1 1 d . B . N10 N 1.1689(3) 0.6355(3) 0.88314(17) 0.0224(7) Uani 1 1 d . . . N11 N 0.9778(3) 0.3947(3) 0.89290(17) 0.0226(7) Uani 1 1 d . B . N12 N 1.0991(3) 0.4594(3) 0.92858(17) 0.0239(7) Uani 1 1 d . . . N13 N 1.0964(3) 0.4296(3) 0.77665(17) 0.0226(7) Uani 1 1 d . B . N14 N 1.1991(3) 0.4774(3) 0.82892(17) 0.0235(7) Uani 1 1 d . . . Ni1 Ni 0.38311(5) 0.16745(4) 0.71909(3) 0.02361(14) 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 B1 0.021(2) 0.030(3) 0.031(3) 0.005(2) 0.006(2) 0.010(2) B2 0.019(2) 0.028(3) 0.027(3) 0.005(2) 0.0028(19) 0.012(2) C1 0.020(2) 0.031(2) 0.036(3) 0.014(2) 0.0086(19) 0.0127(19) C2 0.026(2) 0.029(2) 0.028(2) 0.0081(19) 0.0113(19) 0.0115(19) C3 0.022(2) 0.021(2) 0.025(2) 0.0075(17) 0.0082(17) 0.0084(17) C4 0.022(2) 0.025(2) 0.027(2) 0.0050(17) 0.0073(17) 0.0095(18) C5 0.041(3) 0.030(2) 0.030(2) 0.0055(19) 0.007(2) 0.021(2) C6 0.042(3) 0.035(3) 0.029(2) 0.001(2) 0.006(2) 0.021(2) C7 0.025(2) 0.041(3) 0.029(2) 0.012(2) 0.0057(19) 0.015(2) C8 0.033(3) 0.031(2) 0.037(3) 0.006(2) 0.003(2) 0.017(2) C9 0.033(3) 0.028(2) 0.034(3) 0.002(2) 0.003(2) 0.015(2) C10 0.032(2) 0.037(3) 0.028(2) 0.006(2) 0.0007(19) 0.015(2) C11 0.041(3) 0.036(3) 0.026(2) 0.011(2) 0.005(2) 0.015(2) C12 0.039(3) 0.028(2) 0.023(2) 0.0072(18) 0.0087(19) 0.016(2) C13 0.030(2) 0.030(2) 0.025(2) 0.0105(18) 0.0070(19) 0.014(2) C14 0.043(3) 0.038(3) 0.041(3) 0.002(2) 0.018(2) 0.012(2) C15 0.047(3) 0.045(3) 0.046(3) 0.006(2) 0.027(3) 0.012(3) C16 0.036(3) 0.043(3) 0.045(3) 0.021(2) 0.010(2) 0.010(2) C17 0.044(3) 0.030(3) 0.055(3) -0.002(2) 0.010(3) 0.009(2) C18 0.038(3) 0.032(3) 0.050(3) 0.001(2) 0.008(2) 0.015(2) C19 0.039(3) 0.025(2) 0.033(3) 0.004(2) 0.004(2) 0.003(2) C20 0.049(3) 0.023(2) 0.040(3) 0.005(2) 0.004(2) 0.011(2) C21 0.039(3) 0.025(2) 0.028(2) 0.0080(19) 0.012(2) 0.011(2) C22 0.033(3) 0.025(2) 0.036(3) 0.0038(19) 0.013(2) 0.011(2) C23 0.050(3) 0.034(3) 0.066(4) 0.019(3) 0.020(3) 0.024(3) C24 0.048(3) 0.035(3) 0.094(5) 0.013(3) 0.013(3) 0.022(3) C25 0.034(3) 0.041(3) 0.121(6) -0.021(4) 0.000(4) 0.016(3) C26 0.033(3) 0.069(4) 0.065(4) -0.030(3) 0.013(3) 0.012(3) C27 0.041(3) 0.050(3) 0.036(3) -0.008(2) 0.013(2) 0.013(3) C30 0.021(2) 0.023(2) 0.031(2) 0.0050(18) 0.0055(18) 0.0096(18) C31 0.027(2) 0.022(2) 0.033(2) 0.0063(18) 0.0061(19) 0.0123(18) C32 0.025(2) 0.025(2) 0.026(2) 0.0055(17) 0.0057(18) 0.0143(18) C33 0.030(2) 0.031(2) 0.037(3) 0.001(2) -0.005(2) 0.018(2) C34 0.031(3) 0.029(2) 0.052(3) -0.001(2) 0.000(2) 0.020(2) C35A 0.055(11) 0.043(10) 0.057(14) 0.020(9) 0.011(10) 0.025(9) C36A 0.031(9) 0.045(11) 0.064(11) 0.010(8) -0.003(8) 0.023(8) C37A 0.046(11) 0.060(12) 0.076(13) 0.020(9) 0.007(9) 0.042(10) C35B 0.037(5) 0.028(5) 0.046(6) -0.002(4) -0.002(4) 0.023(4) C36B 0.054(7) 0.042(6) 0.069(7) -0.007(5) -0.024(5) 0.035(6) C37B 0.045(7) 0.049(6) 0.104(10) 0.008(6) 0.038(7) 0.027(5) C38 0.035(2) 0.034(2) 0.018(2) 0.0027(18) 0.0050(18) 0.021(2) C39 0.039(3) 0.035(2) 0.022(2) 0.0080(19) 0.0134(19) 0.020(2) C40 0.033(2) 0.025(2) 0.026(2) 0.0078(18) 0.0152(19) 0.0178(19) C41 0.031(2) 0.028(2) 0.030(2) 0.0103(19) 0.0145(19) 0.015(2) C42 0.037(3) 0.027(2) 0.037(3) 0.008(2) 0.016(2) 0.014(2) C43 0.065(4) 0.037(3) 0.043(3) 0.009(2) 0.011(3) 0.030(3) C44 0.044(3) 0.034(3) 0.066(4) 0.007(3) 0.030(3) 0.015(2) C45 0.037(3) 0.033(3) 0.038(3) 0.002(2) 0.014(2) 0.017(2) C46 0.025(2) 0.030(2) 0.035(2) 0.0139(19) 0.0113(19) 0.0178(19) C47 0.031(2) 0.032(2) 0.034(2) 0.015(2) 0.018(2) 0.019(2) C48 0.032(2) 0.021(2) 0.028(2) 0.0091(17) 0.0128(19) 0.0122(19) C49 0.037(3) 0.028(2) 0.027(2) 0.0066(18) 0.015(2) 0.017(2) C50 0.040(3) 0.032(3) 0.030(2) 0.009(2) 0.012(2) 0.016(2) C51 0.063(4) 0.046(3) 0.031(3) 0.009(2) 0.004(2) 0.031(3) C52 0.048(3) 0.045(3) 0.040(3) 0.021(2) 0.021(2) 0.020(3) C53 0.040(3) 0.025(2) 0.036(3) 0.009(2) 0.005(2) 0.013(2) Co1 0.0228(3) 0.0231(3) 0.0227(3) 0.0050(2) 0.0046(2) 0.0107(2) N1 0.0185(17) 0.0197(17) 0.0264(19) 0.0047(14) 0.0030(14) 0.0042(14) N2 0.0201(18) 0.0259(19) 0.0270(19) 0.0047(15) 0.0046(15) 0.0071(15) N3 0.0259(19) 0.0227(18) 0.0272(19) 0.0062(15) 0.0078(15) 0.0113(15) N4 0.029(2) 0.0282(19) 0.0244(19) 0.0046(15) 0.0066(15) 0.0128(17) N5 0.031(2) 0.0221(18) 0.0234(19) 0.0020(15) 0.0070(16) 0.0081(16) N6 0.029(2) 0.0243(19) 0.027(2) 0.0037(15) 0.0057(16) 0.0073(16) N16 0.045(3) 0.048(3) 0.045(3) 0.006(3) 0.012(3) 0.014(3) C54 0.027(3) 0.028(3) 0.046(4) 0.004(3) 0.015(3) 0.009(2) C55 0.085(7) 0.029(7) 0.041(6) -0.002(4) 0.006(5) 0.018(5) N7 0.0291(19) 0.0251(19) 0.030(2) 0.0018(15) 0.0167(16) 0.0133(16) N8 0.0291(19) 0.0251(19) 0.030(2) 0.0018(15) 0.0167(16) 0.0133(16) C28 0.017(2) 0.018(2) 0.0209(16) 0.0081(15) 0.0052(18) 0.0038(17) C29 0.017(2) 0.018(2) 0.0209(16) 0.0081(15) 0.0052(18) 0.0038(17) S1 0.0202(5) 0.0238(5) 0.0301(5) 0.0026(4) 0.0060(4) 0.0092(4) S2 0.0202(5) 0.0238(5) 0.0301(5) 0.0026(4) 0.0060(4) 0.0092(4) N17 0.045(3) 0.048(3) 0.045(3) 0.006(3) 0.012(3) 0.014(3) C56 0.027(3) 0.028(3) 0.046(4) 0.004(3) 0.015(3) 0.009(2) C57 0.085(7) 0.029(7) 0.041(6) -0.002(4) 0.006(5) 0.018(5) S1B 0.0202(5) 0.0238(5) 0.0301(5) 0.0026(4) 0.0060(4) 0.0092(4) S2B 0.0202(5) 0.0238(5) 0.0301(5) 0.0026(4) 0.0060(4) 0.0092(4) C29B 0.017(2) 0.018(2) 0.0209(16) 0.0081(15) 0.0052(18) 0.0038(17) N8B 0.0291(19) 0.0251(19) 0.030(2) 0.0018(15) 0.0167(16) 0.0133(16) N7B 0.0291(19) 0.0251(19) 0.030(2) 0.0018(15) 0.0167(16) 0.0133(16) C28B 0.017(2) 0.018(2) 0.0209(16) 0.0081(15) 0.0052(18) 0.0038(17) N9 0.0164(17) 0.0236(18) 0.0238(18) 0.0046(14) 0.0040(14) 0.0116(14) N10 0.0172(17) 0.0237(18) 0.0254(18) 0.0037(14) 0.0047(14) 0.0095(15) N11 0.0214(18) 0.0231(18) 0.0239(18) 0.0042(14) 0.0078(14) 0.0107(15) N12 0.0273(19) 0.0245(18) 0.0230(18) 0.0055(14) 0.0052(15) 0.0149(16) N13 0.0259(19) 0.0202(17) 0.0216(18) 0.0046(14) 0.0080(15) 0.0101(15) N14 0.0221(18) 0.0217(18) 0.0251(19) 0.0047(14) 0.0055(15) 0.0093(15) Ni1 0.0231(3) 0.0236(3) 0.0235(3) 0.0054(2) 0.0057(2) 0.0104(2) _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 B1 N2 1.526(6) . ? B1 N4 1.538(6) . ? B1 N6 1.549(6) . ? B1 H1B 1.0000 . ? B2 N12 1.529(6) . ? B2 N14 1.532(6) . ? B2 N10 1.548(6) . ? B2 H2B 1.0000 . ? C1 N2 1.341(5) . ? C1 C2 1.371(6) . ? C1 H1 0.9500 . ? C2 C3 1.397(6) . ? C2 H2 0.9500 . ? C3 N1 1.344(5) . ? C3 C4 1.505(6) . ? C4 C5 1.529(6) . ? C4 C9 1.544(6) . ? C4 H4 1.0000 . ? C5 C6 1.526(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.523(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N4 1.348(6) . ? C10 C11 1.369(7) . ? C10 H10 0.9500 . ? C11 C12 1.406(6) . ? C11 H11 0.9500 . ? C12 N3 1.344(5) . ? C12 C13 1.488(6) . ? C13 C14 1.514(6) . ? C13 C18 1.539(6) . ? C13 H13 1.0000 . ? C14 C15 1.506(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.514(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.500(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.530(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N6 1.341(6) . ? C19 C20 1.362(7) . ? C19 H19 0.9500 . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 N5 1.349(6) . ? C21 C22 1.506(7) . ? C22 C23 1.533(7) . ? C22 C27 1.535(6) . ? C22 H22 1.0000 . ? C23 C24 1.526(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.509(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.497(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.533(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C30 N10 1.333(5) . ? C30 C31 1.374(6) . ? C30 H30 0.9500 . ? C31 C32 1.401(6) . ? C31 H31 0.9500 . ? C32 N9 1.351(5) . ? C32 C33 1.497(6) . ? C33 C34 1.540(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C37B 1.469(9) . ? C34 C36A 1.501(11) . ? C34 C35B 1.511(8) . ? C34 C35A 1.518(13) . ? C34 C36B 1.572(9) . ? C34 C37A 1.580(12) . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38 N12 1.339(5) . ? C38 C39 1.370(6) . ? C38 H38 0.9500 . ? C39 C40 1.391(6) . ? C39 H39 0.9500 . ? C40 N11 1.352(5) . ? C40 C41 1.491(6) . ? C41 C42 1.562(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C45 1.523(6) . ? C42 C44 1.527(7) . ? C42 C43 1.532(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N14 1.351(5) . ? C46 C47 1.358(6) . ? C46 H46 0.9500 . ? C47 C48 1.390(6) . ? C47 H47 0.9500 . ? C48 N13 1.342(5) . ? C48 C49 1.499(6) . ? C49 C50 1.542(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C52 1.513(7) . ? C50 C51 1.523(7) . ? C50 C53 1.527(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? Co1 N8 2.020(5) . ? Co1 N7 2.050(5) . ? Co1 N11 2.066(3) . ? Co1 N13 2.125(3) . ? Co1 N9 2.163(3) . ? Co1 S1B 2.383(9) . ? Co1 S2B 2.552(8) . ? N1 N2 1.364(5) . ? N1 Ni1 2.089(3) . ? N3 N4 1.359(5) . ? N3 Ni1 2.058(4) . ? N5 N6 1.369(5) . ? N5 Ni1 2.133(3) . ? N16 C54 1.133(7) . ? C54 C55 1.422(14) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? N7 C28 1.278(7) . ? N7 H7 0.8800 . ? N8 C29 1.281(6) . ? N8 H8 0.8800 . ? C28 C29 1.521(6) . ? C28 S1 1.712(5) . ? C29 S2 1.719(5) . ? S1 Ni1 2.3444(15) . ? S2 Ni1 2.3898(14) . ? N17 C56 1.113(19) . ? C56 C57 1.42(2) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? S1B C28B 1.750(14) . ? S2B C29B 1.744(15) . ? C29B N8B 1.285(17) . ? C29B C28B 1.558(17) . ? N8B Ni1 2.04(2) . ? N8B H8B1 0.8800 . ? N7B C28B 1.291(16) . ? N7B Ni1 1.80(2) . ? N7B H7B1 0.8800 . ? N9 N10 1.369(4) . ? N11 N12 1.371(5) . ? N13 N14 1.362(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 N2 B1 N4 110.0(4) . . ? N2 B1 N6 108.5(4) . . ? N4 B1 N6 107.4(4) . . ? N2 B1 H1B 110.3 . . ? N4 B1 H1B 110.3 . . ? N6 B1 H1B 110.3 . . ? N12 B2 N14 110.1(3) . . ? N12 B2 N10 110.9(3) . . ? N14 B2 N10 107.0(3) . . ? N12 B2 H2B 109.6 . . ? N14 B2 H2B 109.6 . . ? N10 B2 H2B 109.6 . . ? N2 C1 C2 108.3(4) . . ? N2 C1 H1 125.9 . . ? C2 C1 H1 125.9 . . ? C1 C2 C3 105.9(4) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? N1 C3 C2 109.2(4) . . ? N1 C3 C4 122.8(4) . . ? C2 C3 C4 127.8(4) . . ? C3 C4 C5 111.4(3) . . ? C3 C4 C9 110.5(3) . . ? C5 C4 C9 109.0(4) . . ? C3 C4 H4 108.6 . . ? C5 C4 H4 108.6 . . ? C9 C4 H4 108.6 . . ? C6 C5 C4 112.0(4) . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 110.8(4) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 110.7(4) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 111.6(4) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C4 111.7(4) . . ? C8 C9 H9A 109.3 . . ? C4 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C4 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? N4 C10 C11 108.5(4) . . ? N4 C10 H10 125.8 . . ? C11 C10 H10 125.8 . . ? C10 C11 C12 105.6(4) . . ? C10 C11 H11 127.2 . . ? C12 C11 H11 127.2 . . ? N3 C12 C11 109.1(4) . . ? N3 C12 C13 122.7(4) . . ? C11 C12 C13 128.2(4) . . ? C12 C13 C14 112.0(4) . . ? C12 C13 C18 111.5(4) . . ? C14 C13 C18 109.7(4) . . ? C12 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C18 C13 H13 107.8 . . ? C15 C14 C13 111.4(4) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.6(5) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 111.1(4) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 112.5(4) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 C13 110.4(4) . . ? C17 C18 H18A 109.6 . . ? C13 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C13 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N6 C19 C20 108.0(4) . . ? N6 C19 H19 126.0 . . ? C20 C19 H19 126.0 . . ? C19 C20 C21 106.3(4) . . ? C19 C20 H20 126.8 . . ? C21 C20 H20 126.8 . . ? N5 C21 C20 109.6(4) . . ? N5 C21 C22 124.3(4) . . ? C20 C21 C22 126.1(4) . . ? C21 C22 C23 109.8(4) . . ? C21 C22 C27 110.7(4) . . ? C23 C22 C27 110.3(4) . . ? C21 C22 H22 108.7 . . ? C23 C22 H22 108.7 . . ? C27 C22 H22 108.7 . . ? C24 C23 C22 112.5(5) . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 111.6(6) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 110.0(5) . . ? C26 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? C26 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C25 C26 C27 111.9(5) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C22 110.7(5) . . ? C26 C27 H27A 109.5 . . ? C22 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N10 C30 C31 108.9(4) . . ? N10 C30 H30 125.6 . . ? C31 C30 H30 125.6 . . ? C30 C31 C32 105.2(4) . . ? C30 C31 H31 127.4 . . ? C32 C31 H31 127.4 . . ? N9 C32 C31 109.6(4) . . ? N9 C32 C33 122.7(4) . . ? C31 C32 C33 127.5(4) . . ? C32 C33 C34 118.3(4) . . ? C32 C33 H33A 107.7 . . ? C34 C33 H33A 107.7 . . ? C32 C33 H33B 107.7 . . ? C34 C33 H33B 107.7 . . ? H33A C33 H33B 107.1 . . ? C37B C34 C35B 113.5(7) . . ? C36A C34 C35A 110.7(10) . . ? C37B C34 C33 109.4(5) . . ? C36A C34 C33 114.5(8) . . ? C35B C34 C33 113.3(6) . . ? C35A C34 C33 110.6(13) . . ? C37B C34 C36B 110.2(6) . . ? C35B C34 C36B 105.3(6) . . ? C33 C34 C36B 104.6(5) . . ? C36A C34 C37A 105.5(8) . . ? C35A C34 C37A 104.9(9) . . ? C33 C34 C37A 110.2(8) . . ? C34 C35A H35A 109.5 . . ? C34 C35A H35B 109.5 . . ? C34 C35A H35C 109.5 . . ? C34 C36A H36A 109.5 . . ? C34 C36A H36B 109.5 . . ? C34 C36A H36C 109.5 . . ? C34 C37A H37A 109.5 . . ? C34 C37A H37B 109.5 . . ? C34 C37A H37C 109.5 . . ? C34 C35B H35D 109.5 . . ? C34 C35B H35E 109.5 . . ? C34 C35B H35F 109.5 . . ? C34 C36B H36D 109.5 . . ? C34 C36B H36E 109.5 . . ? C34 C36B H36F 109.5 . . ? C34 C37B H37D 109.5 . . ? C34 C37B H37E 109.5 . . ? C34 C37B H37F 109.5 . . ? N12 C38 C39 108.4(4) . . ? N12 C38 H38 125.8 . . ? C39 C38 H38 125.8 . . ? C38 C39 C40 106.5(4) . . ? C38 C39 H39 126.8 . . ? C40 C39 H39 126.8 . . ? N11 C40 C39 108.7(4) . . ? N11 C40 C41 123.6(4) . . ? C39 C40 C41 127.7(4) . . ? C40 C41 C42 116.7(4) . . ? C40 C41 H41A 108.1 . . ? C42 C41 H41A 108.1 . . ? C40 C41 H41B 108.1 . . ? C42 C41 H41B 108.1 . . ? H41A C41 H41B 107.3 . . ? C45 C42 C44 109.4(4) . . ? C45 C42 C43 109.1(4) . . ? C44 C42 C43 109.4(4) . . ? C45 C42 C41 110.1(4) . . ? C44 C42 C41 107.1(4) . . ? C43 C42 C41 111.6(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N14 C46 C47 108.0(4) . . ? N14 C46 H46 126.0 . . ? C47 C46 H46 126.0 . . ? C46 C47 C48 106.1(4) . . ? C46 C47 H47 127.0 . . ? C48 C47 H47 127.0 . . ? N13 C48 C47 109.8(4) . . ? N13 C48 C49 122.1(4) . . ? C47 C48 C49 128.1(4) . . ? C48 C49 C50 115.0(4) . . ? C48 C49 H49A 108.5 . . ? C50 C49 H49A 108.5 . . ? C48 C49 H49B 108.5 . . ? C50 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C52 C50 C51 109.5(4) . . ? C52 C50 C53 109.7(4) . . ? C51 C50 C53 109.4(4) . . ? C52 C50 C49 110.7(4) . . ? C51 C50 C49 107.7(4) . . ? C53 C50 C49 109.9(4) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N8 Co1 N7 75.3(2) . . ? N8 Co1 N11 103.10(16) . . ? N7 Co1 N11 109.6(2) . . ? N8 Co1 N13 167.52(16) . . ? N7 Co1 N13 101.49(18) . . ? N11 Co1 N13 89.36(13) . . ? N8 Co1 N9 93.69(15) . . ? N7 Co1 N9 156.4(2) . . ? N11 Co1 N9 93.07(13) . . ? N13 Co1 N9 84.72(13) . . ? N8 Co1 S1B 79.8(2) . . ? N7 Co1 S1B 5.0(3) . . ? N11 Co1 S1B 111.1(3) . . ? N13 Co1 S1B 96.7(2) . . ? N9 Co1 S1B 155.8(3) . . ? N8 Co1 S2B 8.5(2) . . ? N7 Co1 S2B 81.5(2) . . ? N11 Co1 S2B 95.6(2) . . ? N13 Co1 S2B 173.00(19) . . ? N9 Co1 S2B 90.13(18) . . ? S1B Co1 S2B 86.1(3) . . ? C3 N1 N2 106.8(3) . . ? C3 N1 Ni1 139.4(3) . . ? N2 N1 Ni1 113.1(3) . . ? C1 N2 N1 109.8(3) . . ? C1 N2 B1 128.0(4) . . ? N1 N2 B1 121.9(3) . . ? C12 N3 N4 107.2(4) . . ? C12 N3 Ni1 136.2(3) . . ? N4 N3 Ni1 116.2(3) . . ? C10 N4 N3 109.7(4) . . ? C10 N4 B1 130.4(4) . . ? N3 N4 B1 119.8(3) . . ? C21 N5 N6 105.8(3) . . ? C21 N5 Ni1 141.2(3) . . ? N6 N5 Ni1 112.9(3) . . ? C19 N6 N5 110.2(4) . . ? C19 N6 B1 128.2(4) . . ? N5 N6 B1 121.6(3) . . ? N16 C54 C55 175.8(8) . . ? C28 N7 Co1 119.1(4) . . ? C28 N7 H7 120.5 . . ? Co1 N7 H7 120.5 . . ? C29 N8 Co1 120.5(4) . . ? C29 N8 H8 119.8 . . ? Co1 N8 H8 119.8 . . ? N7 C28 C29 112.6(4) . . ? N7 C28 S1 126.4(4) . . ? C29 C28 S1 121.0(3) . . ? N8 C29 C28 111.8(4) . . ? N8 C29 S2 127.4(4) . . ? C28 C29 S2 120.8(3) . . ? C28 S1 Ni1 105.58(18) . . ? C29 S2 Ni1 104.38(17) . . ? N17 C56 C57 162(5) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C28B S1B Co1 108.1(8) . . ? C29B S2B Co1 102.4(8) . . ? N8B C29B C28B 117.9(14) . . ? N8B C29B S2B 118.8(17) . . ? C28B C29B S2B 123.3(14) . . ? C29B N8B Ni1 110.4(13) . . ? C29B N8B H8B1 124.8 . . ? Ni1 N8B H8B1 124.8 . . ? C28B N7B Ni1 128.1(15) . . ? C28B N7B H7B1 116.0 . . ? Ni1 N7B H7B1 116.0 . . ? N7B C28B C29B 103.6(13) . . ? N7B C28B S1B 137.2(18) . . ? C29B C28B S1B 119.1(14) . . ? C32 N9 N10 106.1(3) . . ? C32 N9 Co1 139.7(3) . . ? N10 N9 Co1 113.6(2) . . ? C30 N10 N9 110.2(3) . . ? C30 N10 B2 128.5(4) . . ? N9 N10 B2 120.6(3) . . ? C40 N11 N12 106.9(3) . . ? C40 N11 Co1 137.7(3) . . ? N12 N11 Co1 114.8(2) . . ? C38 N12 N11 109.5(3) . . ? C38 N12 B2 129.2(4) . . ? N11 N12 B2 121.3(3) . . ? C48 N13 N14 106.2(3) . . ? C48 N13 Co1 138.9(3) . . ? N14 N13 Co1 114.8(2) . . ? C46 N14 N13 109.9(3) . . ? C46 N14 B2 129.5(4) . . ? N13 N14 B2 120.3(3) . . ? N7B Ni1 N8B 79.8(8) . . ? N7B Ni1 N3 107.0(8) . . ? N8B Ni1 N3 104.9(9) . . ? N7B Ni1 N1 160.0(8) . . ? N8B Ni1 N1 93.3(7) . . ? N3 Ni1 N1 92.93(14) . . ? N7B Ni1 N5 96.0(6) . . ? N8B Ni1 N5 164.9(9) . . ? N3 Ni1 N5 90.26(14) . . ? N1 Ni1 N5 85.78(14) . . ? N7B Ni1 S1 7.2(6) . . ? N8B Ni1 S1 86.1(6) . . ? N3 Ni1 S1 102.07(10) . . ? N1 Ni1 S1 164.65(10) . . ? N5 Ni1 S1 90.86(11) . . ? N7B Ni1 S2 81.7(6) . . ? N8B Ni1 S2 3.8(9) . . ? N3 Ni1 S2 101.20(11) . . ? N1 Ni1 S2 92.53(10) . . ? N5 Ni1 S2 168.50(11) . . ? S1 Ni1 S2 87.78(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7B H7B1 N17 0.88 2.90 3.50(3) 126.6 . N7 H7 N16 0.88 2.50 3.342(8) 160.3 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.961 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.086 data_09mz200_0m _database_code_depnum_ccdc_archive 'CCDC 881844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H82 B2 N14 Ni2 S2, 1.1954(C2 H3 N)' _chemical_formula_sum 'C58.39 H85.59 B2 N15.20 Ni2 S2' _chemical_formula_weight 1203.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.8020(10) _cell_length_b 35.975(3) _cell_length_c 13.2315(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.2830(10) _cell_angle_gamma 90.00 _cell_volume 6273.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5700 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.82 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2561.6 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; The central bridging ligand is disordered across an two fold axis. No restraints or constraints were applied for this disorder. An acetonitrile molecule is partially present in a void close to the metal center. This solvate molecule is in close proximity to a symmetry dependent counterpart of itself, and depending on the presence of either one or two of these acetonitrile moleucles their positions do vary. The sum of the occupancies was restrained so that at least one of the two acetonitrile molecules is present. The occupancies then refined to 0.4027(17) for the case when only one acetonitrile is present, and 0.195(3) for the case that two neighboring ones are present. The geometries of the two molecules were restrained to be similar and the ADPs of equivalent atoms to be indentical. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 22619 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7799 _reflns_number_gt 6230 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0381P)^2^+9.7165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7799 _refine_ls_number_parameters 416 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.59749(17) 0.11188(7) 0.42089(18) 0.0265(5) Uani 1 1 d . . . H1A H 0.5372 0.1084 0.3573 0.032 Uiso 1 1 calc R . . C1 C 0.53154(16) 0.05498(6) 0.5017(2) 0.0363(5) Uani 1 1 d . . . H1B H 0.4707 0.0507 0.4462 0.044 Uiso 1 1 calc R . . C2 C 0.56453(17) 0.03493(7) 0.5934(2) 0.0386(5) Uani 1 1 d . . . H2 H 0.5317 0.0143 0.6138 0.046 Uiso 1 1 calc R . . C3 C 0.65678(16) 0.05112(6) 0.65100(18) 0.0293(4) Uani 1 1 d . . . C4 C 0.72643(17) 0.03891(6) 0.75550(17) 0.0304(5) Uani 1 1 d . . . H4 H 0.7757 0.0595 0.7842 0.037 Uiso 1 1 calc R . . C5 C 0.6689(2) 0.03076(8) 0.8360(2) 0.0455(6) Uani 1 1 d . . . H5A H 0.6316 0.0533 0.8458 0.055 Uiso 1 1 calc R . . H5B H 0.6185 0.0108 0.8081 0.055 Uiso 1 1 calc R . . C6 C 0.7405(2) 0.01877(7) 0.9425(2) 0.0482(7) Uani 1 1 d . . . H6A H 0.7856 0.0398 0.9742 0.058 Uiso 1 1 calc R . . H6B H 0.7003 0.0123 0.9908 0.058 Uiso 1 1 calc R . . C7 C 0.8045(2) -0.01429(7) 0.9321(2) 0.0475(6) Uani 1 1 d . . . H7A H 0.7603 -0.0364 0.9107 0.057 Uiso 1 1 calc R . . H7B H 0.8543 -0.0196 1.0016 0.057 Uiso 1 1 calc R . . C8 C 0.8606(2) -0.00714(7) 0.8504(2) 0.0415(6) Uani 1 1 d . . . H8A H 0.9112 0.0129 0.8762 0.050 Uiso 1 1 calc R . . H8B H 0.8973 -0.0299 0.8412 0.050 Uiso 1 1 calc R . . C9 C 0.78694(17) 0.00416(6) 0.74425(18) 0.0325(5) Uani 1 1 d . . . H9A H 0.7395 -0.0166 0.7160 0.039 Uiso 1 1 calc R . . H9B H 0.8252 0.0092 0.6932 0.039 Uiso 1 1 calc R . . C10 C 0.52612(16) 0.17772(6) 0.43764(19) 0.0342(5) Uani 1 1 d . . . H10 H 0.4690 0.1772 0.3762 0.041 Uiso 1 1 calc R . . C11 C 0.55362(17) 0.20690(6) 0.5066(2) 0.0373(5) Uani 1 1 d . . . H11 H 0.5202 0.2302 0.5027 0.045 Uiso 1 1 calc R . . C12 C 0.64146(15) 0.19520(6) 0.58385(17) 0.0274(4) Uani 1 1 d . . . C13 C 0.70397(15) 0.21624(6) 0.67846(17) 0.0260(4) Uani 1 1 d . . . H13 H 0.7520 0.1983 0.7258 0.031 Uiso 1 1 calc R . . C14 C 0.63785(16) 0.23326(6) 0.74153(18) 0.0308(5) Uani 1 1 d . . . H14A H 0.5882 0.2506 0.6956 0.037 Uiso 1 1 calc R . . H14B H 0.5997 0.2133 0.7644 0.037 Uiso 1 1 calc R . . C15 C 0.70287(17) 0.25413(6) 0.83848(18) 0.0339(5) Uani 1 1 d . . . H15A H 0.6583 0.2659 0.8757 0.041 Uiso 1 1 calc R . . H15B H 0.7477 0.2363 0.8878 0.041 Uiso 1 1 calc R . . C16 C 0.76725(18) 0.28381(7) 0.8079(2) 0.0382(5) Uani 1 1 d . . . H16A H 0.8119 0.2955 0.8727 0.046 Uiso 1 1 calc R . . H16B H 0.7225 0.3033 0.7658 0.046 Uiso 1 1 calc R . . C17 C 0.83214(18) 0.26743(7) 0.74345(19) 0.0374(5) Uani 1 1 d . . . H17A H 0.8694 0.2877 0.7204 0.045 Uiso 1 1 calc R . . H17B H 0.8826 0.2501 0.7884 0.045 Uiso 1 1 calc R . . C18 C 0.76693(16) 0.24676(6) 0.64691(17) 0.0303(4) Uani 1 1 d . . . H18A H 0.8111 0.2355 0.6084 0.036 Uiso 1 1 calc R . . H18B H 0.7209 0.2646 0.5987 0.036 Uiso 1 1 calc R . . C19 C 0.70843(17) 0.10613(6) 0.29272(17) 0.0318(5) Uani 1 1 d . . . H19A H 0.6564 0.1012 0.2287 0.038 Uiso 1 1 calc R . . C20 C 0.80921(18) 0.11025(6) 0.30248(18) 0.0345(5) Uani 1 1 d . . . H20 H 0.8409 0.1088 0.2479 0.041 Uiso 1 1 calc R . . C21 C 0.85577(16) 0.11716(6) 0.41011(18) 0.0284(4) Uani 1 1 d . . . C22 C 0.96349(15) 0.12746(6) 0.46501(19) 0.0313(5) Uani 1 1 d . . . H22 H 0.9768 0.1225 0.5423 0.038 Uiso 1 1 calc R . . C23 C 0.97882(17) 0.16937(6) 0.4508(2) 0.0341(5) Uani 1 1 d . . . H23A H 0.9651 0.1750 0.3746 0.041 Uiso 1 1 calc R . . H23B H 0.9300 0.1837 0.4772 0.041 Uiso 1 1 calc R . . C24 C 1.08615(18) 0.18126(7) 0.5102(2) 0.0418(6) Uani 1 1 d . . . H24A H 1.0984 0.1774 0.5871 0.050 Uiso 1 1 calc R . . H24B H 1.0947 0.2081 0.4980 0.050 Uiso 1 1 calc R . . C25 C 1.16256(19) 0.15890(7) 0.4731(3) 0.0525(7) Uani 1 1 d . . . H25A H 1.2321 0.1661 0.5150 0.063 Uiso 1 1 calc R . . H25B H 1.1545 0.1647 0.3979 0.063 Uiso 1 1 calc R . . C26A C 1.14832(19) 0.11711(7) 0.4851(3) 0.0607(9) Uani 1 1 d . . . H26A H 1.1965 0.1033 0.4566 0.073 Uiso 1 1 calc R . . H26B H 1.1638 0.1109 0.5612 0.073 Uiso 1 1 calc R . . C27 C 1.04007(18) 0.10495(7) 0.4269(3) 0.0484(7) Uani 1 1 d . . . H27A H 1.0320 0.0782 0.4398 0.058 Uiso 1 1 calc R . . H27B H 1.0268 0.1086 0.3498 0.058 Uiso 1 1 calc R . . N9 N 0.699(5) 0.127(4) 0.767(9) 0.045(4) Uani 0.195(3) 1 d PD A -1 C30 C 0.6254(15) 0.1293(11) 0.790(2) 0.044(2) Uani 0.195(3) 1 d PD A -1 C31 C 0.5259(14) 0.1309(5) 0.8034(18) 0.071(4) Uani 0.195(3) 1 d PD A -1 H31A H 0.4749 0.1329 0.7340 0.106 Uiso 0.195(3) 1 calc PR A -1 H31B H 0.5213 0.1527 0.8464 0.106 Uiso 0.195(3) 1 calc PR A -1 H31C H 0.5136 0.1083 0.8391 0.106 Uiso 0.195(3) 1 calc PR A -1 N9B N 0.710(2) 0.1311(17) 0.775(4) 0.045(4) Uani 0.4027(17) 1 d PD B -2 C30B C 0.6495(7) 0.1312(5) 0.8193(7) 0.044(2) Uani 0.4027(17) 1 d PD B -2 C31B C 0.5744(7) 0.1313(2) 0.8753(9) 0.071(4) Uani 0.4027(17) 1 d PD B -2 H31D H 0.6014 0.1183 0.9430 0.106 Uiso 0.4027(17) 1 calc PR B -2 H31E H 0.5130 0.1186 0.8326 0.106 Uiso 0.4027(17) 1 calc PR B -2 H31F H 0.5579 0.1570 0.8884 0.106 Uiso 0.4027(17) 1 calc PR B -2 N1 N 0.59939(12) 0.08171(5) 0.50315(14) 0.0266(4) Uani 1 1 d . . . N2 N 0.67725(12) 0.07981(5) 0.59549(13) 0.0256(4) Uani 1 1 d . C . N3 N 0.59292(12) 0.15010(5) 0.47099(14) 0.0266(4) Uani 1 1 d . . . N4 N 0.66582(12) 0.16070(5) 0.56143(13) 0.0243(3) Uani 1 1 d . C . N5 N 0.69515(12) 0.11018(5) 0.38879(13) 0.0251(3) Uani 1 1 d . . . N6 N 0.78638(12) 0.11705(4) 0.46214(13) 0.0238(3) Uani 1 1 d . C . Ni1 Ni 0.78513(2) 0.122147(8) 0.61676(2) 0.03040(9) Uani 1 1 d . . . N7 N 0.8940(5) 0.15718(17) 0.6896(6) 0.0268(13) Uani 0.50 1 d PD C -1 H7 H 0.902(4) 0.1820(6) 0.699(5) 0.032 Uiso 0.50 1 d PD D -1 N8 N 0.8904(3) 0.08946(13) 0.6932(4) 0.0283(10) Uani 0.50 1 d PD C -1 H8 H 0.896(4) 0.0646(6) 0.698(4) 0.034 Uiso 0.50 1 d PD E -1 C28 C 0.9800(3) 0.14415(10) 0.7466(8) 0.0201(12) Uani 0.50 1 d P C -1 C29 C 0.9779(3) 0.10195(10) 0.7483(5) 0.0197(10) Uani 0.50 1 d P C -1 S1 S 1.08561(14) 0.16895(5) 0.81239(17) 0.0225(3) Uani 0.50 1 d P . -1 S2 S 1.08007(9) 0.07649(4) 0.81710(10) 0.0232(2) Uani 0.50 1 d P . -1 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 B1 0.0190(10) 0.0320(12) 0.0239(11) -0.0026(9) -0.0010(8) 0.0021(9) C1 0.0235(10) 0.0339(12) 0.0502(14) -0.0036(10) 0.0092(10) -0.0051(9) C2 0.0298(11) 0.0312(12) 0.0576(16) 0.0033(11) 0.0175(11) -0.0051(9) C3 0.0297(10) 0.0254(10) 0.0380(12) 0.0000(9) 0.0177(9) 0.0031(8) C4 0.0380(11) 0.0251(10) 0.0329(11) 0.0034(9) 0.0176(9) 0.0018(9) C5 0.0558(16) 0.0447(14) 0.0477(15) 0.0122(12) 0.0335(13) 0.0058(12) C6 0.0727(19) 0.0396(14) 0.0408(14) 0.0072(11) 0.0299(14) -0.0058(13) C7 0.0697(18) 0.0311(13) 0.0396(14) 0.0091(10) 0.0131(13) -0.0023(12) C8 0.0498(14) 0.0291(12) 0.0426(14) 0.0042(10) 0.0092(11) 0.0061(10) C9 0.0375(12) 0.0249(11) 0.0363(12) 0.0001(9) 0.0131(10) 0.0017(9) C10 0.0247(10) 0.0351(12) 0.0372(12) 0.0011(9) 0.0004(9) 0.0054(9) C11 0.0307(11) 0.0309(12) 0.0458(14) -0.0018(10) 0.0042(10) 0.0074(9) C12 0.0254(10) 0.0251(10) 0.0326(11) -0.0005(8) 0.0099(8) 0.0007(8) C13 0.0246(10) 0.0239(10) 0.0307(11) -0.0023(8) 0.0099(8) 0.0004(8) C14 0.0276(10) 0.0265(10) 0.0419(12) -0.0045(9) 0.0156(9) -0.0008(8) C15 0.0360(12) 0.0337(12) 0.0360(12) -0.0057(9) 0.0167(10) 0.0029(9) C16 0.0371(12) 0.0371(13) 0.0401(13) -0.0124(10) 0.0108(10) -0.0068(10) C17 0.0343(12) 0.0429(13) 0.0373(12) -0.0094(10) 0.0140(10) -0.0134(10) C18 0.0298(11) 0.0314(11) 0.0300(11) -0.0022(9) 0.0091(9) -0.0038(9) C19 0.0377(12) 0.0335(11) 0.0214(10) -0.0012(9) 0.0044(9) 0.0026(9) C20 0.0415(12) 0.0347(12) 0.0325(12) 0.0025(9) 0.0187(10) 0.0032(10) C21 0.0268(10) 0.0220(10) 0.0367(12) 0.0042(8) 0.0099(9) 0.0026(8) C22 0.0228(10) 0.0255(11) 0.0462(13) 0.0092(9) 0.0110(9) 0.0001(8) C23 0.0323(11) 0.0247(11) 0.0458(13) 0.0064(9) 0.0126(10) 0.0003(9) C24 0.0371(13) 0.0328(12) 0.0549(15) 0.0124(11) 0.0131(11) -0.0092(10) C25 0.0315(12) 0.0394(14) 0.089(2) 0.0188(14) 0.0211(14) -0.0056(10) C26A 0.0275(12) 0.0412(15) 0.117(3) 0.0277(16) 0.0267(15) 0.0041(10) C27 0.0312(12) 0.0250(12) 0.096(2) 0.0114(13) 0.0288(14) 0.0038(9) N9 0.049(7) 0.038(12) 0.038(8) 0.000(5) -0.002(8) -0.005(6) C30 0.054(5) 0.036(3) 0.042(7) -0.003(5) 0.014(5) -0.003(5) C31 0.069(6) 0.027(3) 0.149(11) 0.005(6) 0.083(7) 0.006(4) N9B 0.049(7) 0.038(12) 0.038(8) 0.000(5) -0.002(8) -0.005(6) C30B 0.054(5) 0.036(3) 0.042(7) -0.003(5) 0.014(5) -0.003(5) C31B 0.069(6) 0.027(3) 0.149(11) 0.005(6) 0.083(7) 0.006(4) N1 0.0202(8) 0.0276(9) 0.0297(9) -0.0040(7) 0.0041(7) -0.0015(7) N2 0.0249(8) 0.0253(9) 0.0263(9) -0.0004(7) 0.0072(7) 0.0008(7) N3 0.0200(8) 0.0300(9) 0.0263(9) -0.0019(7) 0.0013(7) 0.0019(7) N4 0.0212(8) 0.0267(9) 0.0236(8) -0.0026(7) 0.0043(7) -0.0002(6) N5 0.0215(8) 0.0294(9) 0.0202(8) -0.0011(7) -0.0002(6) 0.0012(7) N6 0.0181(7) 0.0240(8) 0.0246(8) 0.0003(6) -0.0006(6) 0.0010(6) Ni1 0.03019(15) 0.02648(15) 0.02353(14) 0.00133(11) -0.00888(11) -0.00380(11) N7 0.022(3) 0.030(4) 0.027(2) 0.003(3) 0.004(2) -0.001(2) N8 0.023(2) 0.027(2) 0.032(2) -0.0006(18) 0.0042(17) 0.0049(17) C28 0.020(4) 0.0206(15) 0.0159(18) -0.0020(17) 0.000(4) -0.0034(13) C29 0.021(3) 0.0208(16) 0.0154(15) 0.0037(16) 0.001(3) 0.0043(12) S1 0.0152(7) 0.0260(9) 0.0224(6) -0.0021(7) -0.0005(5) -0.0004(6) S2 0.0172(6) 0.0220(6) 0.0248(5) 0.0015(5) -0.0023(4) 0.0020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N5 1.530(3) . ? B1 N1 1.532(3) . ? B1 N3 1.536(3) . ? B1 H1A 1.0000 . ? C1 N1 1.338(3) . ? C1 C2 1.368(3) . ? C1 H1B 0.9500 . ? C2 C3 1.402(3) . ? C2 H2 0.9500 . ? C3 N2 1.345(3) . ? C3 C4 1.496(3) . ? C4 C5 1.534(3) . ? C4 C9 1.535(3) . ? C4 H4 1.0000 . ? C5 C6 1.524(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.511(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.528(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.524(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.338(3) . ? C10 C11 1.368(3) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 N4 1.342(3) . ? C12 C13 1.497(3) . ? C13 C18 1.533(3) . ? C13 C14 1.535(3) . ? C13 H13 1.0000 . ? C14 C15 1.527(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.519(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.526(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N5 1.345(3) . ? C19 C20 1.366(3) . ? C19 H19A 0.9500 . ? C20 C21 1.400(3) . ? C20 H20 0.9500 . ? C21 N6 1.335(3) . ? C21 C22 1.495(3) . ? C22 C27 1.531(3) . ? C22 C23 1.542(3) . ? C22 H22 1.0000 . ? C23 C24 1.518(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.519(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26A 1.530(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26A C27 1.527(4) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N9 C30 1.152(18) . ? C30 C31 1.438(15) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N9B C30B 1.149(15) . ? C30B C31B 1.442(9) . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? N1 N2 1.368(2) . ? N2 Ni1 2.0897(17) . ? N3 N4 1.369(2) . ? N4 Ni1 2.1106(16) . ? N5 N6 1.365(2) . ? N6 Ni1 2.0592(17) . ? Ni1 N8 1.908(5) . ? Ni1 N7 1.979(6) . ? Ni1 S1 2.4296(17) 2_756 ? Ni1 S2 2.4409(14) 2_756 ? N7 C28 1.291(9) . ? N7 H7 0.902(19) . ? N8 C29 1.293(6) . ? N8 H8 0.898(19) . ? C28 C29 1.519(5) . ? C28 S1 1.710(5) . ? C29 S2 1.701(4) . ? S1 Ni1 2.4298(17) 2_756 ? S2 Ni1 2.4407(14) 2_756 ? 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 N5 B1 N1 109.79(16) . . ? N5 B1 N3 107.94(17) . . ? N1 B1 N3 108.77(17) . . ? N5 B1 H1A 110.1 . . ? N1 B1 H1A 110.1 . . ? N3 B1 H1A 110.1 . . ? N1 C1 C2 108.6(2) . . ? N1 C1 H1B 125.7 . . ? C2 C1 H1B 125.7 . . ? C1 C2 C3 105.8(2) . . ? C1 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? N2 C3 C2 109.0(2) . . ? N2 C3 C4 123.26(19) . . ? C2 C3 C4 127.7(2) . . ? C3 C4 C5 112.00(19) . . ? C3 C4 C9 111.59(18) . . ? C5 C4 C9 108.68(18) . . ? C3 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? C9 C4 H4 108.1 . . ? C6 C5 C4 111.6(2) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 112.0(2) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C8 111.4(2) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 110.9(2) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C4 111.16(19) . . ? C8 C9 H9A 109.4 . . ? C4 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C4 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N3 C10 C11 108.81(19) . . ? N3 C10 H10 125.6 . . ? C11 C10 H10 125.6 . . ? C10 C11 C12 105.37(19) . . ? C10 C11 H11 127.3 . . ? C12 C11 H11 127.3 . . ? N4 C12 C11 109.66(19) . . ? N4 C12 C13 122.16(18) . . ? C11 C12 C13 128.18(19) . . ? C12 C13 C18 111.52(17) . . ? C12 C13 C14 111.59(17) . . ? C18 C13 C14 109.80(17) . . ? C12 C13 H13 107.9 . . ? C18 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C15 C14 C13 110.91(17) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.48(19) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.36(19) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 111.04(19) . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C13 111.31(18) . . ? C17 C18 H18A 109.4 . . ? C13 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C13 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N5 C19 C20 108.65(19) . . ? N5 C19 H19A 125.7 . . ? C20 C19 H19A 125.7 . . ? C19 C20 C21 105.19(19) . . ? C19 C20 H20 127.4 . . ? C21 C20 H20 127.4 . . ? N6 C21 C20 109.96(18) . . ? N6 C21 C22 120.8(2) . . ? C20 C21 C22 128.9(2) . . ? C21 C22 C27 113.2(2) . . ? C21 C22 C23 109.64(17) . . ? C27 C22 C23 110.11(18) . . ? C21 C22 H22 107.9 . . ? C27 C22 H22 107.9 . . ? C23 C22 H22 107.9 . . ? C24 C23 C22 111.14(18) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 110.3(2) . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26A 111.3(2) . . ? C24 C25 H25A 109.4 . . ? C26A C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26A C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C27 C26A C25 111.4(2) . . ? C27 C26A H26A 109.3 . . ? C25 C26A H26A 109.3 . . ? C27 C26A H26B 109.3 . . ? C25 C26A H26B 109.3 . . ? H26A C26A H26B 108.0 . . ? C26A C27 C22 110.5(2) . . ? C26A C27 H27A 109.6 . . ? C22 C27 H27A 109.6 . . ? C26A C27 H27B 109.6 . . ? C22 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N9 C30 C31 172(6) . . ? N9B C30B C31B 180(4) . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C1 N1 N2 109.73(18) . . ? C1 N1 B1 129.38(18) . . ? N2 N1 B1 120.87(16) . . ? C3 N2 N1 106.82(16) . . ? C3 N2 Ni1 137.98(15) . . ? N1 N2 Ni1 115.02(12) . . ? C10 N3 N4 109.69(17) . . ? C10 N3 B1 129.43(18) . . ? N4 N3 B1 120.85(16) . . ? C12 N4 N3 106.47(16) . . ? C12 N4 Ni1 138.76(14) . . ? N3 N4 Ni1 114.54(12) . . ? C19 N5 N6 109.61(17) . . ? C19 N5 B1 130.19(17) . . ? N6 N5 B1 119.88(16) . . ? C21 N6 N5 106.58(16) . . ? C21 N6 Ni1 136.97(14) . . ? N5 N6 Ni1 116.38(12) . . ? N8 Ni1 N7 77.7(2) . . ? N8 Ni1 N6 104.00(15) . . ? N7 Ni1 N6 108.1(2) . . ? N8 Ni1 N2 91.26(14) . . ? N7 Ni1 N2 159.7(2) . . ? N6 Ni1 N2 90.99(7) . . ? N8 Ni1 N4 168.86(15) . . ? N7 Ni1 N4 98.7(2) . . ? N6 Ni1 N4 87.13(6) . . ? N2 Ni1 N4 88.90(6) . . ? N8 Ni1 S1 82.33(14) . 2_756 ? N7 Ni1 S1 6.4(2) . 2_756 ? N6 Ni1 S1 102.90(7) . 2_756 ? N2 Ni1 S1 165.74(7) . 2_756 ? N4 Ni1 S1 94.95(7) . 2_756 ? N8 Ni1 S2 10.38(14) . 2_756 ? N7 Ni1 S2 82.3(2) . 2_756 ? N6 Ni1 S2 93.77(5) . 2_756 ? N2 Ni1 S2 89.69(5) . 2_756 ? N4 Ni1 S2 178.35(6) . 2_756 ? S1 Ni1 S2 86.21(6) 2_756 2_756 ? C28 N7 Ni1 119.1(4) . . ? C28 N7 H7 103(4) . . ? Ni1 N7 H7 138(4) . . ? C29 N8 Ni1 121.4(3) . . ? C29 N8 H8 105(4) . . ? Ni1 N8 H8 134(4) . . ? N7 C28 C29 110.7(4) . . ? N7 C28 S1 127.2(4) . . ? C29 C28 S1 122.1(4) . . ? N8 C29 C28 111.0(4) . . ? N8 C29 S2 127.0(3) . . ? C28 C29 S2 122.0(4) . . ? C28 S1 Ni1 104.58(15) . 2_756 ? C29 S2 Ni1 104.59(14) . 2_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.0(3) . . . . ? C1 C2 C3 N2 0.3(3) . . . . ? C1 C2 C3 C4 -177.6(2) . . . . ? N2 C3 C4 C5 135.9(2) . . . . ? C2 C3 C4 C5 -46.5(3) . . . . ? N2 C3 C4 C9 -102.0(2) . . . . ? C2 C3 C4 C9 75.6(3) . . . . ? C3 C4 C5 C6 -179.4(2) . . . . ? C9 C4 C5 C6 56.9(3) . . . . ? C4 C5 C6 C7 -55.5(3) . . . . ? C5 C6 C7 C8 53.6(3) . . . . ? C6 C7 C8 C9 -54.6(3) . . . . ? C7 C8 C9 C4 57.7(3) . . . . ? C3 C4 C9 C8 177.75(19) . . . . ? C5 C4 C9 C8 -58.3(3) . . . . ? N3 C10 C11 C12 0.0(3) . . . . ? C10 C11 C12 N4 0.6(3) . . . . ? C10 C11 C12 C13 179.8(2) . . . . ? N4 C12 C13 C18 105.3(2) . . . . ? C11 C12 C13 C18 -73.9(3) . . . . ? N4 C12 C13 C14 -131.5(2) . . . . ? C11 C12 C13 C14 49.3(3) . . . . ? C12 C13 C14 C15 179.20(18) . . . . ? C18 C13 C14 C15 -56.6(2) . . . . ? C13 C14 C15 C16 56.1(2) . . . . ? C14 C15 C16 C17 -55.0(3) . . . . ? C15 C16 C17 C18 55.1(3) . . . . ? C16 C17 C18 C13 -56.5(3) . . . . ? C12 C13 C18 C17 -178.65(18) . . . . ? C14 C13 C18 C17 57.1(2) . . . . ? N5 C19 C20 C21 -0.2(3) . . . . ? C19 C20 C21 N6 0.2(2) . . . . ? C19 C20 C21 C22 -173.5(2) . . . . ? N6 C21 C22 C27 143.9(2) . . . . ? C20 C21 C22 C27 -43.1(3) . . . . ? N6 C21 C22 C23 -92.8(2) . . . . ? C20 C21 C22 C23 80.3(3) . . . . ? C21 C22 C23 C24 177.1(2) . . . . ? C27 C22 C23 C24 -57.8(3) . . . . ? C22 C23 C24 C25 57.5(3) . . . . ? C23 C24 C25 C26A -56.3(3) . . . . ? C24 C25 C26A C27 55.8(4) . . . . ? C25 C26A C27 C22 -55.7(3) . . . . ? C21 C22 C27 C26A 179.4(2) . . . . ? C23 C22 C27 C26A 56.3(3) . . . . ? C2 C1 N1 N2 -0.3(3) . . . . ? C2 C1 N1 B1 -178.9(2) . . . . ? N5 B1 N1 C1 -125.5(2) . . . . ? N3 B1 N1 C1 116.6(2) . . . . ? N5 B1 N1 N2 56.1(2) . . . . ? N3 B1 N1 N2 -61.8(2) . . . . ? C2 C3 N2 N1 -0.5(2) . . . . ? C4 C3 N2 N1 177.48(18) . . . . ? C2 C3 N2 Ni1 174.11(16) . . . . ? C4 C3 N2 Ni1 -7.9(3) . . . . ? C1 N1 N2 C3 0.5(2) . . . . ? B1 N1 N2 C3 179.19(17) . . . . ? C1 N1 N2 Ni1 -175.50(14) . . . . ? B1 N1 N2 Ni1 3.2(2) . . . . ? C11 C10 N3 N4 -0.6(3) . . . . ? C11 C10 N3 B1 -178.6(2) . . . . ? N5 B1 N3 C10 115.8(2) . . . . ? N1 B1 N3 C10 -125.1(2) . . . . ? N5 B1 N3 N4 -62.0(2) . . . . ? N1 B1 N3 N4 57.1(2) . . . . ? C11 C12 N4 N3 -0.9(2) . . . . ? C13 C12 N4 N3 179.76(18) . . . . ? C11 C12 N4 Ni1 172.82(17) . . . . ? C13 C12 N4 Ni1 -6.5(3) . . . . ? C10 N3 N4 C12 1.0(2) . . . . ? B1 N3 N4 C12 179.16(18) . . . . ? C10 N3 N4 Ni1 -174.51(14) . . . . ? B1 N3 N4 Ni1 3.7(2) . . . . ? C20 C19 N5 N6 0.1(2) . . . . ? C20 C19 N5 B1 173.5(2) . . . . ? N1 B1 N5 C19 123.6(2) . . . . ? N3 B1 N5 C19 -118.0(2) . . . . ? N1 B1 N5 N6 -63.6(2) . . . . ? N3 B1 N5 N6 54.9(2) . . . . ? C20 C21 N6 N5 -0.1(2) . . . . ? C22 C21 N6 N5 174.14(17) . . . . ? C20 C21 N6 Ni1 176.74(15) . . . . ? C22 C21 N6 Ni1 -9.0(3) . . . . ? C19 N5 N6 C21 0.0(2) . . . . ? B1 N5 N6 C21 -174.19(18) . . . . ? C19 N5 N6 Ni1 -177.62(14) . . . . ? B1 N5 N6 Ni1 8.2(2) . . . . ? C21 N6 Ni1 N8 -47.0(2) . . . . ? N5 N6 Ni1 N8 129.60(18) . . . . ? C21 N6 Ni1 N7 34.3(3) . . . . ? N5 N6 Ni1 N7 -149.0(2) . . . . ? C21 N6 Ni1 N2 -138.6(2) . . . . ? N5 N6 Ni1 N2 38.06(14) . . . . ? C21 N6 Ni1 N4 132.6(2) . . . . ? N5 N6 Ni1 N4 -50.80(14) . . . . ? C21 N6 Ni1 S1 38.1(2) . . . 2_756 ? N5 N6 Ni1 S1 -145.22(13) . . . 2_756 ? C21 N6 Ni1 S2 -48.8(2) . . . 2_756 ? N5 N6 Ni1 S2 127.81(13) . . . 2_756 ? C3 N2 Ni1 N8 37.9(2) . . . . ? N1 N2 Ni1 N8 -147.85(19) . . . . ? C3 N2 Ni1 N7 -18.4(7) . . . . ? N1 N2 Ni1 N7 155.9(6) . . . . ? C3 N2 Ni1 N6 141.9(2) . . . . ? N1 N2 Ni1 N6 -43.82(13) . . . . ? C3 N2 Ni1 N4 -131.0(2) . . . . ? N1 N2 Ni1 N4 43.29(13) . . . . ? C3 N2 Ni1 S1 -25.0(4) . . . 2_756 ? N1 N2 Ni1 S1 149.3(2) . . . 2_756 ? C3 N2 Ni1 S2 48.1(2) . . . 2_756 ? N1 N2 Ni1 S2 -137.58(13) . . . 2_756 ? C12 N4 Ni1 N8 48.8(8) . . . . ? N3 N4 Ni1 N8 -137.8(7) . . . . ? C12 N4 Ni1 N7 -21.3(3) . . . . ? N3 N4 Ni1 N7 152.1(2) . . . . ? C12 N4 Ni1 N6 -129.2(2) . . . . ? N3 N4 Ni1 N6 44.19(13) . . . . ? C12 N4 Ni1 N2 139.7(2) . . . . ? N3 N4 Ni1 N2 -46.85(14) . . . . ? C12 N4 Ni1 S1 -26.5(2) . . . 2_756 ? N3 N4 Ni1 S1 146.90(13) . . . 2_756 ? N8 Ni1 N7 C28 2.6(6) . . . . ? N6 Ni1 N7 C28 -98.3(7) . . . . ? N2 Ni1 N7 C28 60.9(10) . . . . ? N4 Ni1 N7 C28 171.9(6) . . . . ? S1 Ni1 N7 C28 -134(3) 2_756 . . . ? S2 Ni1 N7 C28 -6.8(6) 2_756 . . . ? N7 Ni1 N8 C29 -3.1(5) . . . . ? N6 Ni1 N8 C29 102.7(5) . . . . ? N2 Ni1 N8 C29 -165.9(5) . . . . ? N4 Ni1 N8 C29 -75.2(9) . . . . ? S1 Ni1 N8 C29 1.3(4) 2_756 . . . ? S2 Ni1 N8 C29 112.7(10) 2_756 . . . ? Ni1 N7 C28 C29 -1.8(10) . . . . ? Ni1 N7 C28 S1 177.5(5) . . . . ? Ni1 N8 C29 C28 3.0(8) . . . . ? Ni1 N8 C29 S2 -177.9(3) . . . . ? N7 C28 C29 N8 -0.7(10) . . . . ? S1 C28 C29 N8 179.9(5) . . . . ? N7 C28 C29 S2 -179.8(6) . . . . ? S1 C28 C29 S2 0.8(10) . . . . ? N7 C28 S1 Ni1 -174.6(8) . . . 2_756 ? C29 C28 S1 Ni1 4.7(7) . . . 2_756 ? N8 C29 S2 Ni1 175.3(5) . . . 2_756 ? C28 C29 S2 Ni1 -5.8(6) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.479 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.054