# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DDOLPHIN@QLTINC.COM _publ_contact_author_name 'Dr David Dolphin' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.Dolphin B.O'Patrick Z.Xiao data_dd164 _database_code_CSD 201831 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H36 N5 Ni O0.50' _chemical_formula_weight 761.54 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7125(10) _cell_length_b 14.3732(15) _cell_length_c 14.0565(15) _cell_angle_alpha 94.720(10) _cell_angle_beta 77.440(10) _cell_angle_gamma 76.150(10) _cell_volume 1840.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3525 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.05 _exptl_crystal_description chip _exptl_crystal_colour dark _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4343 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10104 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.06 _reflns_number_total 10104 _reflns_number_gt 5521 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10104 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.224 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3600(5) 0.0759(3) 0.2820(3) 0.0219(11) Uani 1 1 d . A 1 C3 C 0.4892(5) -0.0541(3) 0.1782(3) 0.0274(14) Uani 0.74(4) 1 d P A 1 H3 H 0.5242 -0.1197 0.1479 0.033 Uiso 0.74(4) 1 calc PR A 1 C4 C 0.5447(5) 0.0211(3) 0.1435(3) 0.0247(11) Uani 1 1 d . A 1 C5 C 0.6620(5) 0.0159(3) 0.0628(3) 0.0256(12) Uani 1 1 d . A 1 C6 C 0.6690(5) 0.1012(3) 0.0222(3) 0.0221(11) Uani 1 1 d . A 1 C7 C 0.7907(5) 0.1130(3) -0.0482(3) 0.0259(11) Uani 1 1 d . A 1 H7 H 0.8865 0.0706 -0.0661 0.031 Uiso 1 1 calc R A 1 C8 C 0.7455(5) 0.1949(3) -0.0846(3) 0.0277(12) Uani 1 1 d . A 1 H8 H 0.8036 0.2208 -0.1334 0.033 Uiso 1 1 calc R A 1 C9 C 0.5932(5) 0.2368(3) -0.0371(3) 0.0219(11) Uani 1 1 d . A 1 C10 C 0.5022(5) 0.3150(3) -0.0630(3) 0.0237(11) Uani 1 1 d . A 1 C11 C 0.3626(5) 0.3585(3) -0.0040(3) 0.0237(11) Uani 1 1 d . A 1 C12 C 0.2549(5) 0.4341(3) -0.0274(3) 0.0282(12) Uani 1 1 d . A 1 H12 H 0.2590 0.4558 -0.0898 0.034 Uiso 1 1 calc R A 1 C13 C 0.1473(5) 0.4689(3) 0.0542(3) 0.0266(11) Uani 1 1 d . A 1 H13 H 0.0617 0.5200 0.0609 0.032 Uiso 1 1 calc R A 1 C14 C 0.1862(5) 0.4138(3) 0.1301(3) 0.0212(11) Uani 1 1 d . A 1 C15 C 0.1088(5) 0.4308(3) 0.2273(3) 0.0204(11) Uani 1 1 d . A 1 C16 C 0.1404(5) 0.3671(3) 0.2932(3) 0.0213(11) Uani 1 1 d . A 1 C17 C 0.0753(5) 0.3883(3) 0.3971(3) 0.0272(11) Uani 1 1 d . A 1 H17 H 0.0128 0.4483 0.4320 0.033 Uiso 1 1 calc R A 1 C18 C 0.1200(5) 0.3067(3) 0.4359(3) 0.0289(12) Uani 1 1 d . A 1 H18 H 0.0949 0.2989 0.5034 0.035 Uiso 1 1 calc R A 1 C19 C 0.2122(5) 0.2338(3) 0.3566(3) 0.0241(11) Uani 1 1 d . A 1 C20 C 0.2582(5) 0.1346(3) 0.3615(3) 0.0244(11) Uani 1 1 d . A 1 C21 C 0.4599(5) 0.1099(3) 0.2082(3) 0.0254(12) Uani 1 1 d . A 1 C25 C 0.5435(6) 0.1692(4) 0.2498(4) 0.0367(13) Uani 1 1 d . A 1 C27 C 0.7723(5) -0.0756(3) 0.0222(3) 0.0261(12) Uani 1 1 d . A 1 C28 C 0.8240(5) -0.1410(3) 0.0820(3) 0.0268(12) Uani 1 1 d . A 1 H28 H 0.7821 -0.1280 0.1509 0.032 Uiso 1 1 calc R A 1 C29 C 0.9343(5) -0.2241(3) 0.0439(3) 0.0289(12) Uani 1 1 d . A 1 H29 H 0.9653 -0.2681 0.0867 0.035 Uiso 1 1 calc R A 1 C30 C 1.0010(5) -0.2446(3) -0.0563(3) 0.0274(11) Uani 1 1 d . A 1 C31 C 0.9443(5) -0.1827(3) -0.1161(3) 0.0266(11) Uani 1 1 d . A 1 H31 H 0.9840 -0.1973 -0.1853 0.032 Uiso 1 1 calc R A 1 C32 C 0.8331(5) -0.1013(3) -0.0796(3) 0.0264(11) Uani 1 1 d . A 1 H32 H 0.7960 -0.0612 -0.1237 0.032 Uiso 1 1 calc R A 1 C33 C 1.1353(6) -0.3297(3) -0.0966(4) 0.0396(14) Uani 1 1 d . A 1 H33A H 1.1044 -0.3878 -0.1130 0.059 Uiso 1 1 calc R A 1 H33B H 1.1918 -0.3407 -0.0468 0.059 Uiso 1 1 calc R A 1 H33C H 1.1961 -0.3152 -0.1559 0.059 Uiso 1 1 calc R A 1 C34 C 0.5528(5) 0.3542(4) -0.1555(3) 0.0315(13) Uani 1 1 d . A 1 C35 C 0.6136(5) 0.2923(4) -0.2434(3) 0.0362(14) Uani 1 1 d . A 1 H35 H 0.6264 0.2246 -0.2441 0.043 Uiso 1 1 calc R A 1 C36 C 0.6561(6) 0.3286(5) -0.3310(4) 0.0500(16) Uani 1 1 d . A 1 H36 H 0.6998 0.2855 -0.3907 0.060 Uiso 1 1 calc R A 1 C37 C 0.6345(6) 0.4287(5) -0.3307(4) 0.0464(17) Uani 1 1 d . A 1 C38 C 0.5770(6) 0.4898(4) -0.2425(4) 0.0470(16) Uani 1 1 d . A 1 H38 H 0.5641 0.5575 -0.2413 0.056 Uiso 1 1 calc R A 1 C39 C 0.5378(5) 0.4525(4) -0.1555(4) 0.0361(13) Uani 1 1 d . A 1 H39 H 0.5001 0.4951 -0.0950 0.043 Uiso 1 1 calc R A 1 C40 C 0.6731(7) 0.4694(6) -0.4284(5) 0.088(3) Uani 1 1 d . A 1 H40A H 0.6042 0.5326 -0.4249 0.132 Uiso 1 1 calc R A 1 H40B H 0.6667 0.4247 -0.4828 0.132 Uiso 1 1 calc R A 1 H40C H 0.7728 0.4769 -0.4395 0.132 Uiso 1 1 calc R A 1 C41 C -0.0100(5) 0.5222(3) 0.2640(3) 0.0268(12) Uani 1 1 d . A 1 C42 C 0.0176(5) 0.6128(3) 0.2555(3) 0.0288(12) Uani 1 1 d . A 1 H42 H 0.1138 0.6164 0.2265 0.035 Uiso 1 1 calc R A 1 C43 C -0.0930(6) 0.6967(3) 0.2888(3) 0.0329(12) Uani 1 1 d . A 1 H43 H -0.0710 0.7572 0.2829 0.039 Uiso 1 1 calc R A 1 C44 C -0.2343(6) 0.6955(4) 0.3302(4) 0.0372(13) Uani 1 1 d . A 1 C45 C -0.2631(6) 0.6063(4) 0.3388(4) 0.0380(13) Uani 1 1 d . A 1 H45 H -0.3599 0.6038 0.3676 0.046 Uiso 1 1 calc R A 1 C46 C -0.1533(5) 0.5203(3) 0.3062(3) 0.0315(12) Uani 1 1 d . A 1 H46 H -0.1759 0.4600 0.3127 0.038 Uiso 1 1 calc R A 1 C47 C -0.3539(6) 0.7868(4) 0.3671(4) 0.0544(17) Uani 1 1 d . A 1 H47A H -0.4143 0.7983 0.3195 0.082 Uiso 1 1 calc R A 1 H47B H -0.3110 0.8413 0.3753 0.082 Uiso 1 1 calc R A 1 H47C H -0.4147 0.7808 0.4306 0.082 Uiso 1 1 calc R A 1 C48 C 0.2018(5) 0.0933(3) 0.4505(3) 0.0230(11) Uani 1 1 d . A 1 C49 C 0.0556(5) 0.1241(3) 0.5043(3) 0.0261(11) Uani 1 1 d . A 1 H49 H -0.0125 0.1717 0.4826 0.031 Uiso 1 1 calc R A 1 C50 C 0.0102(5) 0.0855(3) 0.5887(3) 0.0309(12) Uani 1 1 d . A 1 H50 H -0.0886 0.1089 0.6255 0.037 Uiso 1 1 calc R A 1 C51 C 0.1030(6) 0.0148(3) 0.6210(3) 0.0328(13) Uani 1 1 d . A 1 C52 C 0.2488(5) -0.0180(3) 0.5666(3) 0.0332(13) Uani 1 1 d . A 1 H52 H 0.3154 -0.0669 0.5879 0.040 Uiso 1 1 calc R A 1 C53 C 0.2968(5) 0.0200(3) 0.4826(3) 0.0278(12) Uani 1 1 d . A 1 H53 H 0.3956 -0.0039 0.4459 0.033 Uiso 1 1 calc R A 1 C54 C 0.0524(6) -0.0283(4) 0.7132(3) 0.0504(17) Uani 1 1 d . A 1 H54A H 0.0765 0.0042 0.7690 0.076 Uiso 1 1 calc R A 1 H54B H 0.1018 -0.0976 0.7033 0.076 Uiso 1 1 calc R A 1 H54C H -0.0536 -0.0193 0.7268 0.076 Uiso 1 1 calc R A 1 N2 N 0.3809(4) -0.0224(3) 0.2593(3) 0.0264(12) Uani 0.74(4) 1 d P A 1 H2 H 0.3313 -0.0580 0.2926 0.032 Uiso 0.26(4) 1 calc PR A 1 N22 N 0.5491(4) 0.1814(3) 0.0347(2) 0.0236(10) Uani 1 1 d . A 1 N23 N 0.3144(4) 0.3429(3) 0.0918(2) 0.0237(9) Uani 1 1 d . A 1 N24 N 0.2297(4) 0.2747(3) 0.2689(2) 0.0206(9) Uani 1 1 d . A 1 N26 N 0.6101(5) 0.2152(4) 0.2817(3) 0.0546(13) Uani 1 1 d . A 1 Ni Ni 0.38240(7) 0.22797(4) 0.14761(4) 0.02062(18) Uani 1 1 d . A 1 O1 O 0.7678(19) 0.2859(12) -0.6109(11) 0.201(11) Uiso 0.53(2) 1 d P B 1 N2B N 0.4892(5) -0.0541(3) 0.1782(3) 0.0274(14) Uani 0.26(4) 1 d P A 2 C3B C 0.3809(4) -0.0224(3) 0.2593(3) 0.0264(12) Uani 0.26(4) 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 C1 0.017(2) 0.021(3) 0.023(2) 0.014(2) 0.0045(19) -0.002(2) C3 0.027(3) 0.031(3) 0.022(2) 0.011(2) -0.001(2) -0.005(2) C4 0.027(3) 0.022(3) 0.024(2) 0.012(2) -0.006(2) -0.002(2) C5 0.029(3) 0.023(3) 0.022(2) 0.004(2) -0.004(2) -0.004(2) C6 0.018(3) 0.023(3) 0.023(2) 0.009(2) -0.002(2) 0.000(2) C7 0.019(3) 0.025(3) 0.029(3) 0.007(2) -0.003(2) 0.000(2) C8 0.025(3) 0.037(3) 0.024(2) 0.014(2) -0.001(2) -0.016(2) C9 0.021(3) 0.028(3) 0.022(2) 0.012(2) -0.005(2) -0.013(2) C10 0.033(3) 0.020(3) 0.023(2) 0.010(2) -0.008(2) -0.010(2) C11 0.030(3) 0.022(3) 0.023(2) 0.012(2) -0.006(2) -0.011(2) C12 0.035(3) 0.029(3) 0.026(3) 0.016(2) -0.012(2) -0.009(2) C13 0.027(3) 0.030(3) 0.025(2) 0.013(2) -0.010(2) -0.006(2) C14 0.020(3) 0.015(2) 0.030(3) 0.011(2) -0.006(2) -0.005(2) C15 0.017(3) 0.020(3) 0.023(2) 0.007(2) -0.002(2) -0.004(2) C16 0.020(3) 0.019(3) 0.024(2) 0.004(2) 0.000(2) -0.006(2) C17 0.034(3) 0.020(3) 0.024(2) 0.005(2) -0.002(2) -0.005(2) C18 0.037(3) 0.032(3) 0.019(2) 0.007(2) -0.003(2) -0.013(2) C19 0.021(3) 0.032(3) 0.023(2) 0.013(2) -0.007(2) -0.009(2) C20 0.021(3) 0.032(3) 0.023(2) 0.014(2) -0.004(2) -0.010(2) C21 0.023(3) 0.020(3) 0.028(3) 0.010(2) -0.001(2) 0.000(2) C25 0.036(3) 0.035(3) 0.037(3) 0.012(3) -0.008(3) -0.005(3) C27 0.021(3) 0.026(3) 0.029(3) 0.008(2) -0.004(2) 0.000(2) C28 0.021(3) 0.031(3) 0.023(2) 0.008(2) 0.000(2) 0.001(2) C29 0.027(3) 0.028(3) 0.034(3) 0.018(2) -0.006(2) -0.008(2) C30 0.025(3) 0.020(3) 0.037(3) 0.003(2) -0.004(2) -0.010(2) C31 0.027(3) 0.024(3) 0.027(2) 0.004(2) -0.003(2) -0.007(2) C32 0.031(3) 0.022(3) 0.024(2) 0.010(2) -0.004(2) -0.003(2) C33 0.039(3) 0.021(3) 0.050(3) 0.005(3) -0.005(3) 0.002(3) C34 0.015(3) 0.044(4) 0.037(3) 0.023(3) -0.003(2) -0.009(2) C35 0.028(3) 0.049(4) 0.034(3) 0.019(3) -0.004(2) -0.014(3) C36 0.030(3) 0.087(5) 0.038(3) 0.020(3) -0.010(3) -0.020(3) C37 0.029(3) 0.083(5) 0.047(4) 0.041(4) -0.022(3) -0.029(3) C38 0.039(3) 0.053(4) 0.067(4) 0.039(3) -0.024(3) -0.025(3) C39 0.029(3) 0.036(3) 0.048(3) 0.024(3) -0.011(2) -0.010(2) C40 0.069(5) 0.154(8) 0.069(4) 0.080(5) -0.020(4) -0.055(5) C41 0.027(3) 0.023(3) 0.029(3) 0.010(2) -0.006(2) -0.002(2) C42 0.030(3) 0.034(3) 0.024(2) 0.010(2) -0.008(2) -0.008(2) C43 0.050(4) 0.017(3) 0.032(3) 0.005(2) -0.016(3) -0.005(3) C44 0.040(3) 0.030(3) 0.037(3) -0.002(2) -0.018(3) 0.004(3) C45 0.029(3) 0.034(3) 0.047(3) -0.002(3) -0.008(2) -0.004(3) C46 0.027(3) 0.026(3) 0.040(3) 0.003(2) -0.007(2) -0.005(2) C47 0.050(4) 0.035(4) 0.072(4) -0.007(3) -0.029(3) 0.009(3) C48 0.029(3) 0.016(3) 0.022(2) 0.006(2) -0.004(2) -0.004(2) C49 0.023(3) 0.020(3) 0.031(3) 0.003(2) 0.001(2) -0.005(2) C50 0.032(3) 0.027(3) 0.024(2) 0.000(2) 0.009(2) -0.007(2) C51 0.046(3) 0.031(3) 0.019(2) 0.006(2) 0.005(2) -0.017(3) C52 0.041(3) 0.037(3) 0.026(3) 0.020(2) -0.009(2) -0.011(3) C53 0.029(3) 0.029(3) 0.022(2) 0.008(2) -0.001(2) -0.005(2) C54 0.071(4) 0.047(4) 0.032(3) 0.015(3) 0.000(3) -0.021(3) N2 0.029(2) 0.023(2) 0.023(2) 0.0075(18) 0.0013(19) -0.0031(19) N22 0.021(2) 0.025(2) 0.022(2) 0.0141(18) 0.0001(17) -0.0025(18) N23 0.024(2) 0.024(2) 0.023(2) 0.0112(18) -0.0044(17) -0.0060(19) N24 0.023(2) 0.020(2) 0.0182(19) 0.0087(17) -0.0033(16) -0.0047(18) N26 0.049(3) 0.060(4) 0.061(3) 0.013(3) -0.025(3) -0.016(3) Ni 0.0191(3) 0.0199(3) 0.0212(3) 0.0096(2) -0.0021(2) -0.0024(2) N2B 0.027(3) 0.031(3) 0.022(2) 0.011(2) -0.001(2) -0.005(2) C3B 0.029(2) 0.023(2) 0.023(2) 0.0075(18) 0.0013(19) -0.0031(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.378(6) . ? C1 C20 1.380(6) . ? C1 C21 1.459(5) . ? C3 N2 1.332(5) . ? C3 C4 1.396(6) . ? C3 H3 0.9500 . ? C4 C5 1.405(6) . ? C4 C21 1.454(6) . ? C5 C6 1.404(6) . ? C5 C27 1.461(6) . ? C6 N22 1.397(5) . ? C6 C7 1.422(5) . ? C7 C8 1.337(6) . ? C7 H7 0.9500 . ? C8 C9 1.440(6) . ? C8 H8 0.9500 . ? C9 C10 1.382(6) . ? C9 N22 1.393(5) . ? C10 C11 1.392(6) . ? C10 C34 1.493(5) . ? C11 N23 1.381(5) . ? C11 C12 1.431(6) . ? C12 C13 1.339(6) . ? C12 H12 0.9500 . ? C13 C14 1.441(5) . ? C13 H13 0.9500 . ? C14 N23 1.375(5) . ? C14 C15 1.379(6) . ? C15 C16 1.386(5) . ? C15 C41 1.492(6) . ? C16 N24 1.370(5) . ? C16 C17 1.435(6) . ? C17 C18 1.351(6) . ? C17 H17 0.9500 . ? C18 C19 1.438(6) . ? C18 H18 0.9500 . ? C19 C20 1.401(6) . ? C19 N24 1.405(5) . ? C20 C48 1.483(5) . ? C21 C25 1.478(8) . ? C21 Ni 2.019(4) . ? C25 N26 1.157(7) . ? C25 Ni 2.402(6) . ? C27 C28 1.389(6) . ? C27 C32 1.405(6) . ? C28 C29 1.376(6) . ? C28 H28 0.9500 . ? C29 C30 1.391(6) . ? C29 H29 0.9500 . ? C30 C31 1.375(6) . ? C30 C33 1.523(6) . ? C31 C32 1.362(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.385(7) . ? C34 C35 1.385(7) . ? C35 C36 1.394(6) . ? C35 H35 0.9500 . ? C36 C37 1.403(8) . ? C36 H36 0.9500 . ? C37 C38 1.380(8) . ? C37 C40 1.543(7) . ? C38 C39 1.390(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C46 1.397(6) . ? C41 C42 1.400(6) . ? C42 C43 1.377(6) . ? C42 H42 0.9500 . ? C43 C44 1.374(7) . ? C43 H43 0.9500 . ? C44 C45 1.385(7) . ? C44 C47 1.495(7) . ? C45 C46 1.392(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.399(6) . ? C48 C49 1.400(6) . ? C49 C50 1.382(5) . ? C49 H49 0.9500 . ? C50 C51 1.367(6) . ? C50 H50 0.9500 . ? C51 C52 1.401(6) . ? C51 C54 1.519(5) . ? C52 C53 1.378(5) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N2 H2 0.8800 . ? N22 Ni 1.943(3) . ? N23 Ni 1.923(3) . ? N24 Ni 1.947(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C20 125.5(4) . . ? N2 C1 C21 110.0(4) . . ? C20 C1 C21 124.5(4) . . ? N2 C3 C4 111.5(4) . . ? N2 C3 H3 124.3 . . ? C4 C3 H3 124.3 . . ? C3 C4 C5 128.3(4) . . ? C3 C4 C21 107.4(4) . . ? C5 C4 C21 124.3(4) . . ? C6 C5 C4 117.7(4) . . ? C6 C5 C27 121.3(4) . . ? C4 C5 C27 121.0(4) . . ? N22 C6 C5 124.0(4) . . ? N22 C6 C7 110.3(3) . . ? C5 C6 C7 125.2(4) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 108.1(4) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? C10 C9 N22 125.1(4) . . ? C10 C9 C8 125.7(4) . . ? N22 C9 C8 109.1(4) . . ? C9 C10 C11 121.1(4) . . ? C9 C10 C34 120.1(4) . . ? C11 C10 C34 118.8(4) . . ? N23 C11 C10 124.1(4) . . ? N23 C11 C12 109.6(4) . . ? C10 C11 C12 125.9(4) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 106.8(4) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? N23 C14 C15 124.7(4) . . ? N23 C14 C13 109.9(3) . . ? C15 C14 C13 125.3(4) . . ? C14 C15 C16 122.2(4) . . ? C14 C15 C41 119.2(4) . . ? C16 C15 C41 118.5(4) . . ? N24 C16 C15 125.6(4) . . ? N24 C16 C17 110.8(3) . . ? C15 C16 C17 123.5(4) . . ? C18 C17 C16 106.9(4) . . ? C18 C17 H17 126.6 . . ? C16 C17 H17 126.6 . . ? C17 C18 C19 107.7(4) . . ? C17 C18 H18 126.2 . . ? C19 C18 H18 126.1 . . ? C20 C19 N24 124.3(4) . . ? C20 C19 C18 125.9(4) . . ? N24 C19 C18 109.1(4) . . ? C1 C20 C19 118.4(3) . . ? C1 C20 C48 120.4(4) . . ? C19 C20 C48 121.2(4) . . ? C4 C21 C1 102.8(4) . . ? C4 C21 C25 116.6(4) . . ? C1 C21 C25 114.1(4) . . ? C4 C21 Ni 118.8(3) . . ? C1 C21 Ni 119.7(3) . . ? C25 C21 Ni 85.3(3) . . ? N26 C25 C21 179.4(6) . . ? N26 C25 Ni 123.3(4) . . ? C21 C25 Ni 56.9(2) . . ? C28 C27 C32 116.4(4) . . ? C28 C27 C5 122.0(4) . . ? C32 C27 C5 121.6(4) . . ? C29 C28 C27 121.8(4) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 117.3(4) . . ? C31 C30 C33 121.8(4) . . ? C29 C30 C33 120.8(4) . . ? C32 C31 C30 122.2(4) . . ? C32 C31 H31 118.9 . . ? C30 C31 H31 118.9 . . ? C31 C32 C27 121.2(4) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C39 C34 C35 119.0(4) . . ? C39 C34 C10 120.9(5) . . ? C35 C34 C10 120.0(4) . . ? C34 C35 C36 120.5(5) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.0(6) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.2(5) . . ? C38 C37 C40 120.8(6) . . ? C36 C37 C40 120.0(6) . . ? C37 C38 C39 120.2(5) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C34 C39 C38 121.0(5) . . ? C34 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C46 C41 C42 117.7(4) . . ? C46 C41 C15 121.1(4) . . ? C42 C41 C15 121.2(4) . . ? C43 C42 C41 120.8(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 122.0(5) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C45 117.8(5) . . ? C43 C44 C47 121.8(5) . . ? C45 C44 C47 120.4(5) . . ? C44 C45 C46 121.5(5) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C41 120.3(4) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C53 C48 C49 118.0(4) . . ? C53 C48 C20 119.4(4) . . ? C49 C48 C20 122.6(4) . . ? C50 C49 C48 120.1(4) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 122.0(4) . . ? C51 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? C50 C51 C52 118.3(4) . . ? C50 C51 C54 121.9(4) . . ? C52 C51 C54 119.8(5) . . ? C53 C52 C51 120.7(4) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C48 120.8(4) . . ? C52 C53 H53 119.6 . . ? C48 C53 H53 119.6 . . ? C3 N2 C1 108.3(3) . . ? C3 N2 H2 125.8 . . ? C1 N2 H2 125.8 . . ? C9 N22 C6 104.7(3) . . ? C9 N22 Ni 124.9(3) . . ? C6 N22 Ni 128.2(2) . . ? C14 N23 C11 105.5(3) . . ? C14 N23 Ni 126.1(3) . . ? C11 N23 Ni 126.5(3) . . ? C16 N24 C19 105.2(3) . . ? C16 N24 Ni 124.6(2) . . ? C19 N24 Ni 128.3(3) . . ? N23 Ni N22 90.90(14) . . ? N23 Ni N24 91.84(14) . . ? N22 Ni N24 174.15(17) . . ? N23 Ni C21 177.6(2) . . ? N22 Ni C21 88.69(15) . . ? N24 Ni C21 88.35(15) . . ? N23 Ni C25 139.74(19) . . ? N22 Ni C25 87.84(16) . . ? N24 Ni C25 86.73(15) . . ? C21 Ni C25 37.8(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 N2 C3 C4 C5 177.3(5) . . . . ? N2 C3 C4 C21 -1.6(5) . . . . ? C3 C4 C5 C6 159.7(5) . . . . ? C21 C4 C5 C6 -21.5(7) . . . . ? C3 C4 C5 C27 -20.0(8) . . . . ? C21 C4 C5 C27 158.8(5) . . . . ? C4 C5 C6 N22 -20.8(7) . . . . ? C27 C5 C6 N22 158.9(5) . . . . ? C4 C5 C6 C7 169.2(5) . . . . ? C27 C5 C6 C7 -11.2(8) . . . . ? N22 C6 C7 C8 -4.6(6) . . . . ? C5 C6 C7 C8 166.6(5) . . . . ? C6 C7 C8 C9 0.3(6) . . . . ? C7 C8 C9 C10 -171.5(5) . . . . ? C7 C8 C9 N22 4.1(6) . . . . ? N22 C9 C10 C11 14.2(8) . . . . ? C8 C9 C10 C11 -170.8(5) . . . . ? N22 C9 C10 C34 -165.7(5) . . . . ? C8 C9 C10 C34 9.2(8) . . . . ? C9 C10 C11 N23 14.1(8) . . . . ? C34 C10 C11 N23 -165.9(4) . . . . ? C9 C10 C11 C12 -174.3(5) . . . . ? C34 C10 C11 C12 5.6(8) . . . . ? N23 C11 C12 C13 4.1(6) . . . . ? C10 C11 C12 C13 -168.5(5) . . . . ? C11 C12 C13 C14 -0.8(5) . . . . ? C12 C13 C14 N23 -2.8(5) . . . . ? C12 C13 C14 C15 175.7(5) . . . . ? N23 C14 C15 C16 -11.1(7) . . . . ? C13 C14 C15 C16 170.6(4) . . . . ? N23 C14 C15 C41 166.9(4) . . . . ? C13 C14 C15 C41 -11.4(7) . . . . ? C14 C15 C16 N24 -12.3(7) . . . . ? C41 C15 C16 N24 169.7(4) . . . . ? C14 C15 C16 C17 171.5(4) . . . . ? C41 C15 C16 C17 -6.5(7) . . . . ? N24 C16 C17 C18 -2.8(5) . . . . ? C15 C16 C17 C18 173.9(4) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C17 C18 C19 C20 -166.9(5) . . . . ? C17 C18 C19 N24 3.4(5) . . . . ? N2 C1 C20 C19 -157.0(5) . . . . ? C21 C1 C20 C19 21.7(7) . . . . ? N2 C1 C20 C48 24.3(7) . . . . ? C21 C1 C20 C48 -157.0(5) . . . . ? N24 C19 C20 C1 18.3(7) . . . . ? C18 C19 C20 C1 -172.7(5) . . . . ? N24 C19 C20 C48 -163.0(4) . . . . ? C18 C19 C20 C48 6.0(8) . . . . ? C3 C4 C21 C1 2.4(5) . . . . ? C5 C4 C21 C1 -176.6(4) . . . . ? C3 C4 C21 C25 128.0(4) . . . . ? C5 C4 C21 C25 -51.0(6) . . . . ? C3 C4 C21 Ni -132.3(3) . . . . ? C5 C4 C21 Ni 48.7(6) . . . . ? N2 C1 C21 C4 -2.6(5) . . . . ? C20 C1 C21 C4 178.6(5) . . . . ? N2 C1 C21 C25 -129.7(4) . . . . ? C20 C1 C21 C25 51.5(6) . . . . ? N2 C1 C21 Ni 131.7(4) . . . . ? C20 C1 C21 Ni -47.2(6) . . . . ? C4 C21 C25 N26 16(53) . . . . ? C1 C21 C25 N26 135(53) . . . . ? Ni C21 C25 N26 -104(53) . . . . ? C4 C21 C25 Ni 119.9(4) . . . . ? C1 C21 C25 Ni -120.5(4) . . . . ? C6 C5 C27 C28 141.6(5) . . . . ? C4 C5 C27 C28 -38.8(7) . . . . ? C6 C5 C27 C32 -37.6(7) . . . . ? C4 C5 C27 C32 142.1(5) . . . . ? C32 C27 C28 C29 3.3(7) . . . . ? C5 C27 C28 C29 -175.9(5) . . . . ? C27 C28 C29 C30 1.6(7) . . . . ? C28 C29 C30 C31 -5.2(7) . . . . ? C28 C29 C30 C33 172.3(5) . . . . ? C29 C30 C31 C32 3.8(7) . . . . ? C33 C30 C31 C32 -173.6(5) . . . . ? C30 C31 C32 C27 1.1(7) . . . . ? C28 C27 C32 C31 -4.7(7) . . . . ? C5 C27 C32 C31 174.5(5) . . . . ? C9 C10 C34 C39 -131.4(5) . . . . ? C11 C10 C34 C39 48.6(7) . . . . ? C9 C10 C34 C35 49.7(7) . . . . ? C11 C10 C34 C35 -130.2(5) . . . . ? C39 C34 C35 C36 -1.3(7) . . . . ? C10 C34 C35 C36 177.5(5) . . . . ? C34 C35 C36 C37 -1.4(8) . . . . ? C35 C36 C37 C38 2.9(8) . . . . ? C35 C36 C37 C40 -176.4(5) . . . . ? C36 C37 C38 C39 -1.5(8) . . . . ? C40 C37 C38 C39 177.7(5) . . . . ? C35 C34 C39 C38 2.7(8) . . . . ? C10 C34 C39 C38 -176.2(5) . . . . ? C37 C38 C39 C34 -1.2(8) . . . . ? C14 C15 C41 C46 122.3(5) . . . . ? C16 C15 C41 C46 -59.6(7) . . . . ? C14 C15 C41 C42 -56.4(7) . . . . ? C16 C15 C41 C42 121.7(5) . . . . ? C46 C41 C42 C43 0.7(7) . . . . ? C15 C41 C42 C43 179.4(4) . . . . ? C41 C42 C43 C44 -0.9(7) . . . . ? C42 C43 C44 C45 0.7(7) . . . . ? C42 C43 C44 C47 179.4(5) . . . . ? C43 C44 C45 C46 -0.4(7) . . . . ? C47 C44 C45 C46 -179.2(5) . . . . ? C44 C45 C46 C41 0.3(8) . . . . ? C42 C41 C46 C45 -0.4(7) . . . . ? C15 C41 C46 C45 -179.1(4) . . . . ? C1 C20 C48 C53 37.6(7) . . . . ? C19 C20 C48 C53 -141.1(5) . . . . ? C1 C20 C48 C49 -141.8(5) . . . . ? C19 C20 C48 C49 39.5(7) . . . . ? C53 C48 C49 C50 2.9(7) . . . . ? C20 C48 C49 C50 -177.7(5) . . . . ? C48 C49 C50 C51 -2.1(8) . . . . ? C49 C50 C51 C52 0.8(8) . . . . ? C49 C50 C51 C54 -179.3(5) . . . . ? C50 C51 C52 C53 -0.3(8) . . . . ? C54 C51 C52 C53 179.8(5) . . . . ? C51 C52 C53 C48 1.2(8) . . . . ? C49 C48 C53 C52 -2.4(7) . . . . ? C20 C48 C53 C52 178.1(5) . . . . ? C4 C3 N2 C1 -0.1(5) . . . . ? C20 C1 N2 C3 -179.4(4) . . . . ? C21 C1 N2 C3 1.7(5) . . . . ? C10 C9 N22 C6 169.0(5) . . . . ? C8 C9 N22 C6 -6.7(5) . . . . ? C10 C9 N22 Ni -26.9(7) . . . . ? C8 C9 N22 Ni 157.4(3) . . . . ? C5 C6 N22 C9 -164.4(5) . . . . ? C7 C6 N22 C9 6.9(5) . . . . ? C5 C6 N22 Ni 32.2(7) . . . . ? C7 C6 N22 Ni -156.4(3) . . . . ? C15 C14 N23 C11 -173.3(5) . . . . ? C13 C14 N23 C11 5.3(5) . . . . ? C15 C14 N23 Ni 21.6(7) . . . . ? C13 C14 N23 Ni -159.9(3) . . . . ? C10 C11 N23 C14 167.0(5) . . . . ? C12 C11 N23 C14 -5.7(5) . . . . ? C10 C11 N23 Ni -27.9(7) . . . . ? C12 C11 N23 Ni 159.3(3) . . . . ? C15 C16 N24 C19 -171.8(4) . . . . ? C17 C16 N24 C19 4.8(5) . . . . ? C15 C16 N24 Ni 22.7(6) . . . . ? C17 C16 N24 Ni -160.7(3) . . . . ? C20 C19 N24 C16 165.6(4) . . . . ? C18 C19 N24 C16 -5.0(5) . . . . ? C20 C19 N24 Ni -29.6(7) . . . . ? C18 C19 N24 Ni 159.8(3) . . . . ? C14 N23 Ni N22 175.4(4) . . . . ? C11 N23 Ni N22 13.3(4) . . . . ? C14 N23 Ni N24 -9.8(4) . . . . ? C11 N23 Ni N24 -171.9(4) . . . . ? C14 N23 Ni C21 -104(4) . . . . ? C11 N23 Ni C21 94(4) . . . . ? C14 N23 Ni C25 -96.9(4) . . . . ? C11 N23 Ni C25 101.0(4) . . . . ? C9 N22 Ni N23 11.9(4) . . . . ? C6 N22 Ni N23 172.1(4) . . . . ? C9 N22 Ni N24 -106.1(15) . . . . ? C6 N22 Ni N24 54.2(17) . . . . ? C9 N22 Ni C21 -165.7(4) . . . . ? C6 N22 Ni C21 -5.5(4) . . . . ? C9 N22 Ni C25 -127.9(4) . . . . ? C6 N22 Ni C25 32.4(4) . . . . ? C16 N24 Ni N23 -10.5(4) . . . . ? C19 N24 Ni N23 -172.7(4) . . . . ? C16 N24 Ni N22 107.3(15) . . . . ? C19 N24 Ni N22 -54.8(17) . . . . ? C16 N24 Ni C21 167.0(4) . . . . ? C19 N24 Ni C21 4.9(4) . . . . ? C16 N24 Ni C25 129.2(4) . . . . ? C19 N24 Ni C25 -32.9(4) . . . . ? C4 C21 Ni N23 -110(4) . . . . ? C1 C21 Ni N23 123(4) . . . . ? C25 C21 Ni N23 8(4) . . . . ? C4 C21 Ni N22 -29.6(4) . . . . ? C1 C21 Ni N22 -156.8(4) . . . . ? C25 C21 Ni N22 88.2(3) . . . . ? C4 C21 Ni N24 155.4(4) . . . . ? C1 C21 Ni N24 28.3(4) . . . . ? C25 C21 Ni N24 -86.8(3) . . . . ? C4 C21 Ni C25 -117.8(5) . . . . ? C1 C21 Ni C25 115.1(5) . . . . ? N26 C25 Ni N23 -0.2(6) . . . . ? C21 C25 Ni N23 -179.5(3) . . . . ? N26 C25 Ni N22 88.6(5) . . . . ? C21 C25 Ni N22 -90.7(3) . . . . ? N26 C25 Ni N24 -89.2(5) . . . . ? C21 C25 Ni N24 91.5(3) . . . . ? N26 C25 Ni C21 179.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.575 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.098 #===END data_shelxl _database_code_CSD 201832 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H37 N5 Ni O' _chemical_formula_weight 782.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8239(4) _cell_length_b 12.7674(6) _cell_length_c 15.3382(7) _cell_angle_alpha 82.788(8) _cell_angle_beta 81.698(7) _cell_angle_gamma 82.301(8) _cell_volume 1875.39(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8216 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.87 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7797 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7709 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.87 _reflns_number_total 7709 _reflns_number_gt 5006 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7709 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.38032(4) 0.37457(3) 0.20376(2) 0.01761(11) Uani 1 d . A 1 O1 O 0.8363(3) 0.1228(3) 0.2261(2) 0.0262(10) Uani 0.627(4) d P A 1 N22 N 0.4253(2) 0.31938(17) 0.08909(14) 0.0178(5) Uani 1 d . A 1 N23 N 0.2716(2) 0.49907(17) 0.15348(14) 0.0174(5) Uani 1 d . A 1 N24 N 0.3293(2) 0.41784(17) 0.32282(14) 0.0178(5) Uani 1 d . A 1 N25 N 0.2572(3) 0.1549(2) 0.28353(19) 0.0382(7) Uani 1 d . A 1 C1 C 0.5480(3) 0.2449(2) 0.33882(17) 0.0173(6) Uani 1 d . A 1 N2 N 0.6829(3) 0.1981(2) 0.33043(18) 0.0270(6) Uani 0.627(4) d P A 1 C3 C 0.7142(3) 0.1633(2) 0.2480(2) 0.0293(7) Uani 0.627(4) d P A 1 C4 C 0.5995(3) 0.1846(2) 0.20186(18) 0.0196(6) Uani 1 d . A 1 C5 C 0.5888(3) 0.1581(2) 0.11868(18) 0.0186(6) Uani 1 d . A 1 C6 C 0.4875(3) 0.2184(2) 0.07148(18) 0.0189(6) Uani 1 d . A 1 C7 C 0.4488(3) 0.1932(2) -0.00974(18) 0.0237(7) Uani 1 d . A 1 H7 H 0.4709 0.1269 -0.0336 0.028 Uiso 1 calc R A 1 C8 C 0.3758(3) 0.2804(2) -0.04572(19) 0.0236(7) Uani 1 d . A 1 H8 H 0.3392 0.2883 -0.1005 0.028 Uiso 1 calc R A 1 C9 C 0.3635(3) 0.3600(2) 0.01491(17) 0.0187(6) Uani 1 d . A 1 C10 C 0.3019(3) 0.4645(2) -0.00201(18) 0.0191(6) Uani 1 d . A 1 C11 C 0.2711(3) 0.5323(2) 0.06444(18) 0.0191(6) Uani 1 d . A 1 C12 C 0.2160(3) 0.6420(2) 0.05215(18) 0.0217(6) Uani 1 d . A 1 H12 H 0.2098 0.6846 -0.0029 0.026 Uiso 1 calc R A 1 C13 C 0.1745(3) 0.6737(2) 0.13397(19) 0.0232(7) Uani 1 d . A 1 H13 H 0.1320 0.7422 0.1471 0.028 Uiso 1 calc R A 1 C14 C 0.2068(3) 0.5844(2) 0.19661(18) 0.0181(6) Uani 1 d . A 1 C15 C 0.1696(3) 0.5797(2) 0.28839(18) 0.0183(6) Uani 1 d . A 1 C16 C 0.2217(3) 0.4957(2) 0.34607(17) 0.0182(6) Uani 1 d . A 1 C17 C 0.1784(3) 0.4812(2) 0.43942(18) 0.0228(7) Uani 1 d . A 1 H17 H 0.1044 0.5225 0.4711 0.027 Uiso 1 calc R A 1 C18 C 0.2607(3) 0.3990(2) 0.47430(18) 0.0237(7) Uani 1 d . A 1 H18 H 0.2554 0.3708 0.5349 0.028 Uiso 1 calc R A 1 C19 C 0.3587(3) 0.3617(2) 0.40239(18) 0.0212(7) Uani 1 d . A 1 C20 C 0.4756(3) 0.2870(2) 0.41368(18) 0.0205(6) Uani 1 d . A 1 C21 C 0.4872(3) 0.2417(2) 0.25719(17) 0.0170(6) Uani 1 d . A 1 C25 C 0.9452(5) 0.1185(5) 0.2805(4) 0.0327(14) Uani 0.627(4) d P A 1 H25A H 0.9642 0.1909 0.2853 0.049 Uiso 0.627(4) calc PR A 1 H25B H 1.0293 0.0781 0.2536 0.049 Uiso 0.627(4) calc PR A 1 H25C H 0.9164 0.0838 0.3397 0.049 Uiso 0.627(4) calc PR A 1 C26 C 0.6851(3) 0.0718(2) 0.07799(18) 0.0193(6) Uani 1 d . A 1 C27 C 0.7273(3) -0.0214(2) 0.12963(19) 0.0235(7) Uani 1 d . A 1 H27 H 0.6962 -0.0292 0.1914 0.028 Uiso 1 calc R A 1 C28 C 0.8141(3) -0.1028(2) 0.0917(2) 0.0283(7) Uani 1 d . A 1 H28 H 0.8435 -0.1648 0.1285 0.034 Uiso 1 calc R A 1 C29 C 0.8591(3) -0.0963(2) 0.0014(2) 0.0265(7) Uani 1 d . A 1 C30 C 0.8216(3) -0.0018(2) -0.0489(2) 0.0261(7) Uani 1 d . A 1 H30 H 0.8549 0.0065 -0.1104 0.031 Uiso 1 calc R A 1 C31 C 0.7360(3) 0.0810(2) -0.01145(19) 0.0259(7) Uani 1 d . A 1 H31 H 0.7121 0.1450 -0.0477 0.031 Uiso 1 calc R A 1 C32 C 0.9432(4) -0.1886(3) -0.0416(2) 0.0407(9) Uani 1 d . A 1 H32A H 0.8909 -0.2118 -0.0839 0.061 Uiso 1 calc R A 1 H32B H 0.9627 -0.2475 0.0041 0.061 Uiso 1 calc R A 1 H32C H 1.0307 -0.1663 -0.0727 0.061 Uiso 1 calc R A 1 C33 C 0.2604(3) 0.5016(2) -0.09156(17) 0.0183(6) Uani 1 d . A 1 C34 C 0.3560(3) 0.4912(2) -0.16851(18) 0.0227(7) Uani 1 d . A 1 H34 H 0.4494 0.4630 -0.1634 0.027 Uiso 1 calc R A 1 C35 C 0.3153(3) 0.5217(2) -0.25188(19) 0.0265(7) Uani 1 d . A 1 H35 H 0.3815 0.5146 -0.3031 0.032 Uiso 1 calc R A 1 C36 C 0.1790(3) 0.5625(2) -0.26178(19) 0.0260(7) Uani 1 d . A 1 C37 C 0.0849(3) 0.5745(2) -0.18560(19) 0.0264(7) Uani 1 d . A 1 H37 H -0.0083 0.6031 -0.1909 0.032 Uiso 1 calc R A 1 C38 C 0.1254(3) 0.5452(2) -0.10204(19) 0.0246(7) Uani 1 d . A 1 H38 H 0.0596 0.5552 -0.0510 0.030 Uiso 1 calc R A 1 C39 C 0.1340(4) 0.5898(3) -0.3527(2) 0.0402(9) Uani 1 d . A 1 H39A H 0.1256 0.5242 -0.3775 0.060 Uiso 1 calc R A 1 H39B H 0.2031 0.6288 -0.3914 0.060 Uiso 1 calc R A 1 H39C H 0.0443 0.6341 -0.3482 0.060 Uiso 1 calc R A 1 C40 C 0.0708(3) 0.6676(2) 0.32589(18) 0.0205(6) Uani 1 d . A 1 C41 C -0.0577(3) 0.6980(2) 0.29624(19) 0.0258(7) Uani 1 d . A 1 H41 H -0.0829 0.6638 0.2505 0.031 Uiso 1 calc R A 1 C42 C -0.1490(3) 0.7782(2) 0.3333(2) 0.0328(8) Uani 1 d . A 1 H42 H -0.2365 0.7973 0.3126 0.039 Uiso 1 calc R A 1 C43 C -0.1164(3) 0.8313(2) 0.3997(2) 0.0344(9) Uani 1 d . A 1 C44 C 0.0124(3) 0.8007(3) 0.4291(2) 0.0365(8) Uani 1 d . A 1 H44 H 0.0378 0.8357 0.4744 0.044 Uiso 1 calc R A 1 C45 C 0.1039(3) 0.7200(2) 0.3934(2) 0.0298(7) Uani 1 d . A 1 H45 H 0.1906 0.6999 0.4151 0.036 Uiso 1 calc R A 1 C46 C -0.2170(4) 0.9148(3) 0.4428(3) 0.0533(12) Uani 1 d . A 1 H46A H -0.2690 0.8818 0.4963 0.080 Uiso 1 calc R A 1 H46B H -0.2815 0.9480 0.4014 0.080 Uiso 1 calc R A 1 H46C H -0.1663 0.9690 0.4590 0.080 Uiso 1 calc R A 1 C47 C 0.5182(3) 0.2531(2) 0.50341(18) 0.0215(7) Uani 1 d . A 1 C48 C 0.5132(3) 0.3231(2) 0.56643(19) 0.0277(7) Uani 1 d . A 1 H48 H 0.4882 0.3970 0.5516 0.033 Uiso 1 calc R A 1 C49 C 0.5448(3) 0.2854(3) 0.65178(19) 0.0287(7) Uani 1 d . A 1 H49 H 0.5373 0.3340 0.6949 0.034 Uiso 1 calc R A 1 C50 C 0.5869(3) 0.1782(3) 0.67469(19) 0.0281(7) Uani 1 d . A 1 C51 C 0.5954(3) 0.1086(2) 0.61004(19) 0.0298(8) Uani 1 d . A 1 H51 H 0.6243 0.0351 0.6240 0.036 Uiso 1 calc R A 1 C52 C 0.5624(3) 0.1453(2) 0.52613(19) 0.0262(7) Uani 1 d . A 1 H52 H 0.5698 0.0967 0.4831 0.031 Uiso 1 calc R A 1 C53 C 0.6274(4) 0.1395(3) 0.7643(2) 0.0430(9) Uani 1 d . A 1 H53A H 0.7271 0.1160 0.7589 0.065 Uiso 1 calc R A 1 H53B H 0.5763 0.0798 0.7904 0.065 Uiso 1 calc R A 1 H53C H 0.6053 0.1972 0.8024 0.065 Uiso 1 calc R A 1 C54 C 0.3572(3) 0.1943(2) 0.27150(19) 0.0231(7) Uani 1 d . A 1 C3B C 0.6829(3) 0.1981(2) 0.33043(18) 0.0270(6) Uani 0.373(4) d P A 2 N2B N 0.7142(3) 0.1633(2) 0.2480(2) 0.0293(7) Uani 0.373(4) d P A 2 O1B O 0.7875(5) 0.1858(4) 0.3696(3) 0.0201(15) Uani 0.373(4) d P A 2 C25B C 0.9284(8) 0.1480(8) 0.3323(6) 0.027(2) Uani 0.373(4) d P A 2 H25D H 0.9550 0.1927 0.2773 0.041 Uiso 0.373(4) calc PR A 2 H25E H 0.9323 0.0743 0.3196 0.041 Uiso 0.373(4) calc PR A 2 H25F H 0.9925 0.1518 0.3749 0.041 Uiso 0.373(4) calc PR 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 Ni1 0.0197(2) 0.0171(2) 0.01491(18) 0.00020(14) -0.00367(14) 0.00163(15) O1 0.0169(17) 0.038(2) 0.0246(18) -0.0133(15) -0.0038(14) 0.0044(15) N22 0.0189(12) 0.0154(12) 0.0190(12) 0.0000(10) -0.0047(10) -0.0001(10) N23 0.0185(12) 0.0181(12) 0.0153(12) -0.0014(10) -0.0039(10) 0.0008(10) N24 0.0174(12) 0.0196(12) 0.0154(12) -0.0002(10) -0.0043(10) 0.0023(10) N25 0.0277(16) 0.0359(16) 0.0502(19) 0.0038(14) -0.0045(14) -0.0096(13) C1 0.0182(14) 0.0149(13) 0.0180(14) 0.0036(11) -0.0056(11) -0.0002(11) N2 0.0234(15) 0.0221(14) 0.0358(16) 0.0050(12) -0.0135(13) -0.0005(12) C3 0.0220(15) 0.0179(14) 0.0479(19) 0.0060(14) -0.0127(14) -0.0024(12) C4 0.0222(15) 0.0150(14) 0.0209(15) 0.0002(12) -0.0058(12) 0.0020(12) C5 0.0200(15) 0.0137(14) 0.0212(15) 0.0006(12) -0.0033(12) -0.0008(12) C6 0.0253(16) 0.0144(14) 0.0166(14) 0.0019(11) -0.0034(12) -0.0028(12) C7 0.0301(17) 0.0195(15) 0.0227(15) -0.0060(13) -0.0058(13) -0.0009(13) C8 0.0315(17) 0.0227(15) 0.0178(14) -0.0028(12) -0.0071(13) -0.0028(13) C9 0.0218(15) 0.0214(15) 0.0132(13) -0.0025(12) -0.0058(11) 0.0011(12) C10 0.0193(15) 0.0190(14) 0.0189(14) -0.0010(12) -0.0024(12) -0.0025(12) C11 0.0189(15) 0.0207(15) 0.0165(14) 0.0030(12) -0.0037(12) -0.0008(12) C12 0.0289(16) 0.0169(14) 0.0175(14) 0.0048(12) -0.0064(12) 0.0011(13) C13 0.0286(17) 0.0163(14) 0.0238(15) -0.0021(12) -0.0046(13) 0.0025(13) C14 0.0214(15) 0.0139(13) 0.0187(14) -0.0005(11) -0.0067(12) 0.0024(12) C15 0.0180(15) 0.0171(14) 0.0203(14) -0.0001(12) -0.0069(12) -0.0014(12) C16 0.0188(14) 0.0202(14) 0.0147(13) 0.0004(12) -0.0038(11) 0.0003(12) C17 0.0202(15) 0.0271(16) 0.0185(14) 0.0004(13) -0.0001(12) 0.0017(13) C18 0.0269(16) 0.0273(16) 0.0139(14) 0.0024(12) -0.0010(12) 0.0022(13) C19 0.0258(16) 0.0197(15) 0.0161(14) -0.0005(12) -0.0020(12) 0.0024(13) C20 0.0238(16) 0.0187(14) 0.0184(14) 0.0010(12) -0.0043(12) -0.0018(12) C21 0.0156(14) 0.0204(14) 0.0157(13) -0.0004(12) -0.0062(11) -0.0014(12) C25 0.020(3) 0.049(4) 0.031(3) -0.012(3) -0.013(2) 0.003(2) C26 0.0190(15) 0.0174(14) 0.0226(15) -0.0037(12) -0.0059(12) -0.0014(12) C27 0.0289(17) 0.0203(15) 0.0234(15) -0.0045(13) -0.0112(13) 0.0003(13) C28 0.0346(18) 0.0210(15) 0.0310(17) -0.0042(14) -0.0177(14) 0.0060(14) C29 0.0237(16) 0.0267(16) 0.0302(17) -0.0086(14) -0.0098(13) 0.0047(13) C30 0.0237(16) 0.0303(17) 0.0236(15) -0.0059(14) 0.0005(13) -0.0019(13) C31 0.0288(17) 0.0228(16) 0.0242(16) 0.0003(13) -0.0011(13) -0.0013(13) C32 0.036(2) 0.036(2) 0.049(2) -0.0152(17) -0.0071(17) 0.0127(16) C33 0.0245(15) 0.0155(14) 0.0151(13) -0.0011(11) -0.0031(12) -0.0035(12) C34 0.0245(16) 0.0191(15) 0.0229(15) 0.0006(12) -0.0027(12) -0.0001(13) C35 0.0365(18) 0.0224(16) 0.0198(15) -0.0024(13) -0.0012(13) -0.0035(14) C36 0.0396(19) 0.0198(15) 0.0208(15) 0.0001(13) -0.0128(14) -0.0045(14) C37 0.0265(17) 0.0240(16) 0.0289(17) -0.0014(13) -0.0086(13) -0.0001(13) C38 0.0259(16) 0.0242(16) 0.0219(15) 0.0013(13) -0.0028(13) -0.0002(13) C39 0.057(2) 0.045(2) 0.0221(17) -0.0027(16) -0.0190(16) -0.0072(19) C40 0.0203(15) 0.0207(15) 0.0177(14) 0.0004(12) 0.0020(12) 0.0008(12) C41 0.0299(17) 0.0229(16) 0.0202(15) 0.0047(13) -0.0011(13) 0.0039(13) C42 0.0260(17) 0.0279(17) 0.0365(19) 0.0096(15) 0.0019(15) 0.0075(14) C43 0.0326(19) 0.0206(16) 0.043(2) -0.0035(15) 0.0164(16) 0.0000(14) C44 0.035(2) 0.0338(19) 0.040(2) -0.0141(16) 0.0057(16) -0.0037(16) C45 0.0291(18) 0.0287(17) 0.0300(17) -0.0050(14) 0.0005(14) -0.0009(14) C46 0.043(2) 0.032(2) 0.074(3) -0.015(2) 0.023(2) 0.0066(18) C47 0.0222(15) 0.0261(16) 0.0152(14) -0.0012(12) -0.0049(12) 0.0027(13) C48 0.0296(17) 0.0297(17) 0.0227(15) -0.0047(14) -0.0075(13) 0.0070(14) C49 0.0295(17) 0.0371(18) 0.0197(15) -0.0061(14) -0.0075(13) 0.0030(15) C50 0.0263(17) 0.0386(19) 0.0176(15) 0.0017(14) -0.0064(13) 0.0018(15) C51 0.0346(18) 0.0288(17) 0.0218(16) 0.0040(14) -0.0073(14) 0.0092(15) C52 0.0287(17) 0.0273(16) 0.0202(15) -0.0001(13) -0.0036(13) 0.0033(14) C53 0.052(2) 0.059(2) 0.0172(16) 0.0019(16) -0.0124(16) -0.002(2) C54 0.0248(17) 0.0193(15) 0.0229(15) 0.0015(13) -0.0046(13) 0.0034(13) C3B 0.0234(15) 0.0221(14) 0.0358(16) 0.0050(12) -0.0135(13) -0.0005(12) N2B 0.0220(15) 0.0179(14) 0.0479(19) 0.0060(14) -0.0127(14) -0.0024(12) O1B 0.015(3) 0.031(3) 0.013(3) -0.004(2) -0.001(2) 0.001(2) C25B 0.020(4) 0.045(6) 0.017(4) -0.005(4) -0.003(3) -0.002(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 Ni1 N23 1.933(2) . ? Ni1 N22 1.946(2) . ? Ni1 N24 1.951(2) . ? Ni1 C21 2.018(3) . ? Ni1 C54 2.429(3) . ? O1 C3 1.257(4) . ? O1 C25 1.440(6) . ? N22 C9 1.378(3) . ? N22 C6 1.392(3) . ? N23 C11 1.379(3) . ? N23 C14 1.379(3) . ? N24 C19 1.383(3) . ? N24 C16 1.389(3) . ? N25 C54 1.144(4) . ? C1 N2 1.375(4) . ? C1 C20 1.389(4) . ? C1 C21 1.470(4) . ? N2 C3 1.372(4) . ? C3 C4 1.395(4) . ? C4 C5 1.382(4) . ? C4 C21 1.462(3) . ? C5 C6 1.404(4) . ? C5 C26 1.490(3) . ? C6 C7 1.439(4) . ? C7 C8 1.344(4) . ? C7 H7 0.9500 . ? C8 C9 1.443(4) . ? C8 H8 0.9500 . ? C9 C10 1.399(4) . ? C10 C11 1.393(4) . ? C10 C33 1.491(4) . ? C11 C12 1.433(4) . ? C12 C13 1.356(4) . ? C12 H12 0.9500 . ? C13 C14 1.428(4) . ? C13 H13 0.9500 . ? C14 C15 1.398(4) . ? C15 C16 1.393(4) . ? C15 C40 1.497(3) . ? C16 C17 1.430(4) . ? C17 C18 1.340(4) . ? C17 H17 0.9500 . ? C18 C19 1.440(4) . ? C18 H18 0.9500 . ? C19 C20 1.408(4) . ? C20 C47 1.491(4) . ? C21 C54 1.462(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C31 1.387(4) . ? C26 C27 1.394(4) . ? C27 C28 1.384(4) . ? C27 H27 0.9500 . ? C28 C29 1.387(4) . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C29 C32 1.511(4) . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.392(4) . ? C33 C34 1.406(4) . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.392(4) . ? C35 H35 0.9500 . ? C36 C37 1.392(4) . ? C36 C39 1.508(4) . ? C37 C38 1.388(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.393(4) . ? C40 C45 1.398(4) . ? C41 C42 1.389(4) . ? C41 H41 0.9500 . ? C42 C43 1.387(5) . ? C42 H42 0.9500 . ? C43 C44 1.395(5) . ? C43 C46 1.502(4) . ? C44 C45 1.386(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.388(4) . ? C47 C52 1.404(4) . ? C48 C49 1.400(4) . ? C48 H48 0.9500 . ? C49 C50 1.392(4) . ? C49 H49 0.9500 . ? C50 C51 1.399(4) . ? C50 C53 1.492(4) . ? C51 C52 1.382(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O1B C25B 1.463(9) . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 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 N23 Ni1 N22 91.54(9) . . ? N23 Ni1 N24 91.45(9) . . ? N22 Ni1 N24 174.91(10) . . ? N23 Ni1 C21 177.81(11) . . ? N22 Ni1 C21 88.46(10) . . ? N24 Ni1 C21 88.39(10) . . ? N23 Ni1 C54 140.85(10) . . ? N22 Ni1 C54 88.55(9) . . ? N24 Ni1 C54 86.53(9) . . ? C21 Ni1 C54 36.95(10) . . ? C3 O1 C25 123.1(3) . . ? C9 N22 C6 105.0(2) . . ? C9 N22 Ni1 124.62(17) . . ? C6 N22 Ni1 127.67(18) . . ? C11 N23 C14 105.3(2) . . ? C11 N23 Ni1 126.04(17) . . ? C14 N23 Ni1 127.01(18) . . ? C19 N24 C16 104.9(2) . . ? C19 N24 Ni1 128.11(17) . . ? C16 N24 Ni1 124.44(18) . . ? N2 C1 C20 125.9(3) . . ? N2 C1 C21 110.3(2) . . ? C20 C1 C21 123.8(2) . . ? C3 N2 C1 108.1(2) . . ? O1 C3 N2 117.5(3) . . ? O1 C3 C4 131.7(3) . . ? N2 C3 C4 110.7(2) . . ? C5 C4 C3 127.8(3) . . ? C5 C4 C21 124.2(3) . . ? C3 C4 C21 108.0(2) . . ? C4 C5 C6 117.7(2) . . ? C4 C5 C26 121.7(2) . . ? C6 C5 C26 120.5(2) . . ? N22 C6 C5 124.4(2) . . ? N22 C6 C7 109.7(2) . . ? C5 C6 C7 125.2(2) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.9(3) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N22 C9 C10 125.5(2) . . ? N22 C9 C8 110.5(2) . . ? C10 C9 C8 124.0(3) . . ? C11 C10 C9 121.3(3) . . ? C11 C10 C33 119.5(2) . . ? C9 C10 C33 119.0(2) . . ? N23 C11 C10 124.1(2) . . ? N23 C11 C12 110.1(2) . . ? C10 C11 C12 125.2(3) . . ? C13 C12 C11 107.0(2) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 C14 107.0(2) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N23 C14 C15 123.8(2) . . ? N23 C14 C13 110.4(2) . . ? C15 C14 C13 125.6(2) . . ? C16 C15 C14 122.0(2) . . ? C16 C15 C40 119.0(2) . . ? C14 C15 C40 119.1(2) . . ? N24 C16 C15 125.3(2) . . ? N24 C16 C17 109.9(2) . . ? C15 C16 C17 124.7(2) . . ? C18 C17 C16 107.9(2) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? C17 C18 C19 106.9(2) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N24 C19 C20 125.4(2) . . ? N24 C19 C18 110.2(2) . . ? C20 C19 C18 124.1(3) . . ? C1 C20 C19 117.7(3) . . ? C1 C20 C47 121.5(2) . . ? C19 C20 C47 120.8(2) . . ? C4 C21 C54 114.4(2) . . ? C4 C21 C1 102.9(2) . . ? C54 C21 C1 114.0(2) . . ? C4 C21 Ni1 119.51(19) . . ? C54 C21 Ni1 86.98(16) . . ? C1 C21 Ni1 119.30(19) . . ? C31 C26 C27 117.8(2) . . ? C31 C26 C5 121.8(3) . . ? C27 C26 C5 120.4(2) . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 121.8(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 117.3(3) . . ? C30 C29 C32 120.7(3) . . ? C28 C29 C32 122.0(3) . . ? C29 C30 C31 121.4(3) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C26 C31 C30 121.0(3) . . ? C26 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C38 C33 C34 117.7(3) . . ? C38 C33 C10 121.3(2) . . ? C34 C33 C10 121.0(3) . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 121.1(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 118.2(3) . . ? C37 C36 C39 121.1(3) . . ? C35 C36 C39 120.7(3) . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C33 121.3(3) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C41 C40 C45 118.0(3) . . ? C41 C40 C15 121.3(3) . . ? C45 C40 C15 120.7(3) . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 122.0(3) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 117.5(3) . . ? C42 C43 C46 122.3(3) . . ? C44 C43 C46 120.1(3) . . ? C45 C44 C43 121.1(3) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C40 121.0(3) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? C48 C47 C52 118.3(3) . . ? C48 C47 C20 123.0(3) . . ? C52 C47 C20 118.7(2) . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 121.3(3) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 118.0(3) . . ? C49 C50 C53 121.0(3) . . ? C51 C50 C53 121.0(3) . . ? C52 C51 C50 120.9(3) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C47 121.1(3) . . ? C51 C52 H52 119.5 . . ? C47 C52 H52 119.5 . . ? N25 C54 C21 178.3(3) . . ? N25 C54 Ni1 125.6(2) . . ? C21 C54 Ni1 56.07(14) . . ? O1B C25B H25D 109.5 . . ? O1B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? O1B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 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 N23 Ni1 N22 C9 -10.8(2) . . . . ? N24 Ni1 N22 C9 115.2(11) . . . . ? C21 Ni1 N22 C9 167.0(2) . . . . ? C54 Ni1 N22 C9 130.0(2) . . . . ? N23 Ni1 N22 C6 -169.1(2) . . . . ? N24 Ni1 N22 C6 -43.1(12) . . . . ? C21 Ni1 N22 C6 8.7(2) . . . . ? C54 Ni1 N22 C6 -28.3(2) . . . . ? N22 Ni1 N23 C11 -13.3(2) . . . . ? N24 Ni1 N23 C11 170.8(2) . . . . ? C21 Ni1 N23 C11 -103(3) . . . . ? C54 Ni1 N23 C11 -102.9(3) . . . . ? N22 Ni1 N23 C14 -176.5(2) . . . . ? N24 Ni1 N23 C14 7.6(2) . . . . ? C21 Ni1 N23 C14 94(3) . . . . ? C54 Ni1 N23 C14 93.9(3) . . . . ? N23 Ni1 N24 C19 173.7(3) . . . . ? N22 Ni1 N24 C19 47.7(12) . . . . ? C21 Ni1 N24 C19 -4.1(3) . . . . ? C54 Ni1 N24 C19 32.8(3) . . . . ? N23 Ni1 N24 C16 14.7(2) . . . . ? N22 Ni1 N24 C16 -111.3(11) . . . . ? C21 Ni1 N24 C16 -163.1(2) . . . . ? C54 Ni1 N24 C16 -126.2(2) . . . . ? C20 C1 N2 C3 177.7(3) . . . . ? C21 C1 N2 C3 -0.6(3) . . . . ? C25 O1 C3 N2 -4.6(6) . . . . ? C25 O1 C3 C4 172.6(4) . . . . ? C1 N2 C3 O1 176.5(3) . . . . ? C1 N2 C3 C4 -1.3(3) . . . . ? O1 C3 C4 C5 5.4(6) . . . . ? N2 C3 C4 C5 -177.4(3) . . . . ? O1 C3 C4 C21 -174.7(3) . . . . ? N2 C3 C4 C21 2.6(3) . . . . ? C3 C4 C5 C6 -156.9(3) . . . . ? C21 C4 C5 C6 23.2(4) . . . . ? C3 C4 C5 C26 20.4(5) . . . . ? C21 C4 C5 C26 -159.6(3) . . . . ? C9 N22 C6 C5 164.2(3) . . . . ? Ni1 N22 C6 C5 -34.2(4) . . . . ? C9 N22 C6 C7 -6.9(3) . . . . ? Ni1 N22 C6 C7 154.8(2) . . . . ? C4 C5 C6 N22 19.5(4) . . . . ? C26 C5 C6 N22 -157.8(3) . . . . ? C4 C5 C6 C7 -170.8(3) . . . . ? C26 C5 C6 C7 11.9(4) . . . . ? N22 C6 C7 C8 5.9(3) . . . . ? C5 C6 C7 C8 -165.1(3) . . . . ? C6 C7 C8 C9 -2.3(3) . . . . ? C6 N22 C9 C10 -172.1(3) . . . . ? Ni1 N22 C9 C10 25.5(4) . . . . ? C6 N22 C9 C8 5.5(3) . . . . ? Ni1 N22 C9 C8 -156.9(2) . . . . ? C7 C8 C9 N22 -2.0(3) . . . . ? C7 C8 C9 C10 175.6(3) . . . . ? N22 C9 C10 C11 -14.1(5) . . . . ? C8 C9 C10 C11 168.6(3) . . . . ? N22 C9 C10 C33 169.9(3) . . . . ? C8 C9 C10 C33 -7.4(4) . . . . ? C14 N23 C11 C10 -167.0(3) . . . . ? Ni1 N23 C11 C10 26.9(4) . . . . ? C14 N23 C11 C12 4.9(3) . . . . ? Ni1 N23 C11 C12 -161.2(2) . . . . ? C9 C10 C11 N23 -13.3(5) . . . . ? C33 C10 C11 N23 162.7(3) . . . . ? C9 C10 C11 C12 176.0(3) . . . . ? C33 C10 C11 C12 -7.9(4) . . . . ? N23 C11 C12 C13 -4.0(3) . . . . ? C10 C11 C12 C13 167.8(3) . . . . ? C11 C12 C13 C14 1.3(3) . . . . ? C11 N23 C14 C15 171.4(3) . . . . ? Ni1 N23 C14 C15 -22.6(4) . . . . ? C11 N23 C14 C13 -4.1(3) . . . . ? Ni1 N23 C14 C13 161.9(2) . . . . ? C12 C13 C14 N23 1.7(4) . . . . ? C12 C13 C14 C15 -173.7(3) . . . . ? N23 C14 C15 C16 14.6(5) . . . . ? C13 C14 C15 C16 -170.6(3) . . . . ? N23 C14 C15 C40 -165.4(3) . . . . ? C13 C14 C15 C40 9.4(5) . . . . ? C19 N24 C16 C15 171.4(3) . . . . ? Ni1 N24 C16 C15 -25.6(4) . . . . ? C19 N24 C16 C17 -4.7(3) . . . . ? Ni1 N24 C16 C17 158.4(2) . . . . ? C14 C15 C16 N24 10.5(5) . . . . ? C40 C15 C16 N24 -169.4(3) . . . . ? C14 C15 C16 C17 -174.0(3) . . . . ? C40 C15 C16 C17 6.0(5) . . . . ? N24 C16 C17 C18 2.5(4) . . . . ? C15 C16 C17 C18 -173.6(3) . . . . ? C16 C17 C18 C19 0.7(4) . . . . ? C16 N24 C19 C20 -168.4(3) . . . . ? Ni1 N24 C19 C20 29.4(4) . . . . ? C16 N24 C19 C18 5.1(3) . . . . ? Ni1 N24 C19 C18 -157.1(2) . . . . ? C17 C18 C19 N24 -3.7(4) . . . . ? C17 C18 C19 C20 169.8(3) . . . . ? N2 C1 C20 C19 159.1(3) . . . . ? C21 C1 C20 C19 -22.9(4) . . . . ? N2 C1 C20 C47 -22.0(5) . . . . ? C21 C1 C20 C47 156.0(3) . . . . ? N24 C19 C20 C1 -17.9(5) . . . . ? C18 C19 C20 C1 169.4(3) . . . . ? N24 C19 C20 C47 163.1(3) . . . . ? C18 C19 C20 C47 -9.5(5) . . . . ? C5 C4 C21 C54 53.1(4) . . . . ? C3 C4 C21 C54 -126.9(3) . . . . ? C5 C4 C21 C1 177.2(3) . . . . ? C3 C4 C21 C1 -2.7(3) . . . . ? C5 C4 C21 Ni1 -47.8(4) . . . . ? C3 C4 C21 Ni1 132.2(2) . . . . ? N2 C1 C21 C4 2.0(3) . . . . ? C20 C1 C21 C4 -176.3(3) . . . . ? N2 C1 C21 C54 126.4(3) . . . . ? C20 C1 C21 C54 -51.9(4) . . . . ? N2 C1 C21 Ni1 -133.0(2) . . . . ? C20 C1 C21 Ni1 48.7(4) . . . . ? N23 Ni1 C21 C4 117(3) . . . . ? N22 Ni1 C21 C4 26.8(2) . . . . ? N24 Ni1 C21 C4 -157.2(2) . . . . ? C54 Ni1 C21 C4 116.4(3) . . . . ? N23 Ni1 C21 C54 0(3) . . . . ? N22 Ni1 C21 C54 -89.64(16) . . . . ? N24 Ni1 C21 C54 86.36(16) . . . . ? N23 Ni1 C21 C1 -116(3) . . . . ? N22 Ni1 C21 C1 154.5(2) . . . . ? N24 Ni1 C21 C1 -29.5(2) . . . . ? C54 Ni1 C21 C1 -115.9(3) . . . . ? C4 C5 C26 C31 -140.6(3) . . . . ? C6 C5 C26 C31 36.6(4) . . . . ? C4 C5 C26 C27 39.1(4) . . . . ? C6 C5 C26 C27 -143.7(3) . . . . ? C31 C26 C27 C28 -1.8(5) . . . . ? C5 C26 C27 C28 178.4(3) . . . . ? C26 C27 C28 C29 -1.8(5) . . . . ? C27 C28 C29 C30 4.3(5) . . . . ? C27 C28 C29 C32 -174.4(3) . . . . ? C28 C29 C30 C31 -3.4(5) . . . . ? C32 C29 C30 C31 175.4(3) . . . . ? C27 C26 C31 C30 2.7(5) . . . . ? C5 C26 C31 C30 -177.5(3) . . . . ? C29 C30 C31 C26 -0.1(5) . . . . ? C11 C10 C33 C38 -51.2(4) . . . . ? C9 C10 C33 C38 125.0(3) . . . . ? C11 C10 C33 C34 130.3(3) . . . . ? C9 C10 C33 C34 -53.5(4) . . . . ? C38 C33 C34 C35 -1.3(4) . . . . ? C10 C33 C34 C35 177.3(3) . . . . ? C33 C34 C35 C36 -0.5(4) . . . . ? C34 C35 C36 C37 1.6(4) . . . . ? C34 C35 C36 C39 -176.6(3) . . . . ? C35 C36 C37 C38 -0.9(4) . . . . ? C39 C36 C37 C38 177.3(3) . . . . ? C36 C37 C38 C33 -1.0(5) . . . . ? C34 C33 C38 C37 2.0(4) . . . . ? C10 C33 C38 C37 -176.5(3) . . . . ? C16 C15 C40 C41 -126.4(3) . . . . ? C14 C15 C40 C41 53.7(4) . . . . ? C16 C15 C40 C45 52.2(4) . . . . ? C14 C15 C40 C45 -127.8(3) . . . . ? C45 C40 C41 C42 0.0(4) . . . . ? C15 C40 C41 C42 178.6(3) . . . . ? C40 C41 C42 C43 0.7(5) . . . . ? C41 C42 C43 C44 -0.6(5) . . . . ? C41 C42 C43 C46 -177.2(3) . . . . ? C42 C43 C44 C45 -0.2(5) . . . . ? C46 C43 C44 C45 176.6(3) . . . . ? C43 C44 C45 C40 0.8(5) . . . . ? C41 C40 C45 C44 -0.7(4) . . . . ? C15 C40 C45 C44 -179.3(3) . . . . ? C1 C20 C47 C48 141.2(3) . . . . ? C19 C20 C47 C48 -39.9(4) . . . . ? C1 C20 C47 C52 -40.3(4) . . . . ? C19 C20 C47 C52 138.6(3) . . . . ? C52 C47 C48 C49 -3.3(4) . . . . ? C20 C47 C48 C49 175.3(3) . . . . ? C47 C48 C49 C50 2.5(5) . . . . ? C48 C49 C50 C51 -0.7(5) . . . . ? C48 C49 C50 C53 176.8(3) . . . . ? C49 C50 C51 C52 -0.3(5) . . . . ? C53 C50 C51 C52 -177.8(3) . . . . ? C50 C51 C52 C47 -0.6(5) . . . . ? C48 C47 C52 C51 2.3(5) . . . . ? C20 C47 C52 C51 -176.3(3) . . . . ? C4 C21 C54 N25 56(11) . . . . ? C1 C21 C54 N25 -62(11) . . . . ? Ni1 C21 C54 N25 177(100) . . . . ? C4 C21 C54 Ni1 -121.2(2) . . . . ? C1 C21 C54 Ni1 120.9(2) . . . . ? N23 Ni1 C54 N25 0.1(4) . . . . ? N22 Ni1 C54 N25 -90.5(3) . . . . ? N24 Ni1 C54 N25 88.2(3) . . . . ? C21 Ni1 C54 N25 -179.9(4) . . . . ? N23 Ni1 C54 C21 -179.98(17) . . . . ? N22 Ni1 C54 C21 89.36(16) . . . . ? N24 Ni1 C54 C21 -91.94(16) . . . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.303 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.071