# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_(TMTBM)Ni=N(dmp) #TrackingRef 'Bent imido complete cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H57 N5 Ni' _chemical_formula_weight 702.64 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.911(2) _cell_length_b 12.339(2) _cell_length_c 15.869(5) _cell_angle_alpha 103.994(4) _cell_angle_beta 97.621(4) _cell_angle_gamma 107.921(3) _cell_volume 1922.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21583 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.9568 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details 'Norton et. al' _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 P4' _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 21583 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6772 _reflns_number_gt 5394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0863P)^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 7264 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.00286(5) 0.41290(4) 0.27303(4) 0.0193(2) Uani 1 1 d . . . C1 C 0.1785(4) 0.5158(3) 0.2974(3) 0.0191(10) Uani 1 1 d . . . N3 N 0.2345(3) 0.5130(3) 0.2245(2) 0.0203(8) Uani 1 1 d . . . C3 C 0.3634(4) 0.5945(4) 0.2466(3) 0.0228(10) Uani 1 1 d . . . C4 C 0.3891(4) 0.6490(4) 0.3341(3) 0.0240(10) Uani 1 1 d . . . C5 C 0.5116(4) 0.7504(4) 0.3877(3) 0.0363(12) Uani 1 1 d . . . H5A H 0.5736 0.7667 0.3507 0.055 Uiso 1 1 calc R . . H5B H 0.5501 0.7296 0.4366 0.055 Uiso 1 1 calc R . . H5C H 0.4899 0.8200 0.4103 0.055 Uiso 1 1 calc R . . N2 N 0.2758(3) 0.6002(3) 0.3655(2) 0.0217(8) Uani 1 1 d . . . C7 C 0.2738(4) 0.6061(4) 0.4613(3) 0.0255(11) Uani 1 1 d . . . C8 C 0.3540(5) 0.5319(4) 0.4860(3) 0.0341(12) Uani 1 1 d . . . H8A H 0.3139 0.4512 0.4477 0.051 Uiso 1 1 calc R . . H8B H 0.3559 0.5328 0.5468 0.051 Uiso 1 1 calc R . . H8C H 0.4426 0.5652 0.4790 0.051 Uiso 1 1 calc R . . C9 C 0.3314(5) 0.7339(4) 0.5228(3) 0.0315(11) Uani 1 1 d . . . H9A H 0.4247 0.7653 0.5262 0.047 Uiso 1 1 calc R . . H9B H 0.3163 0.7350 0.5812 0.047 Uiso 1 1 calc R . . H9C H 0.2895 0.7819 0.4998 0.047 Uiso 1 1 calc R . . C10 C 0.1342(4) 0.5540(4) 0.4711(3) 0.0306(11) Uani 1 1 d . . . H10A H 0.0828 0.5977 0.4517 0.046 Uiso 1 1 calc R . . H10B H 0.1345 0.5591 0.5325 0.046 Uiso 1 1 calc R . . H10C H 0.0962 0.4718 0.4354 0.046 Uiso 1 1 calc R . . C11 C 0.4442(5) 0.6081(4) 0.1792(3) 0.0324(12) Uani 1 1 d . . . H11A H 0.5252 0.6749 0.2055 0.049 Uiso 1 1 calc R . . H11B H 0.3960 0.6215 0.1299 0.049 Uiso 1 1 calc R . . H11C H 0.4637 0.5368 0.1584 0.049 Uiso 1 1 calc R . . C12 C 0.1653(4) 0.4225(3) 0.1397(3) 0.0227(10) Uani 1 1 d . . . H12A H 0.2230 0.4251 0.0981 0.027 Uiso 1 1 calc R . . H12B H 0.0883 0.4375 0.1147 0.027 Uiso 1 1 calc R . . N5 N 0.1245(3) 0.3048(3) 0.1541(2) 0.0215(8) Uani 1 1 d . . . C14 C 0.1602(4) 0.2081(4) 0.1159(3) 0.0242(10) Uani 1 1 d . . . C15 C 0.1052(4) 0.1228(4) 0.1530(3) 0.0248(11) Uani 1 1 d . . . C16 C 0.1159(5) 0.0015(4) 0.1330(3) 0.0341(12) Uani 1 1 d . . . H16A H 0.0336 -0.0571 0.0968 0.051 Uiso 1 1 calc R . . H16B H 0.1359 -0.0163 0.1877 0.051 Uiso 1 1 calc R . . H16C H 0.1851 0.0000 0.1016 0.051 Uiso 1 1 calc R . . N6 N 0.0361(3) 0.1701(3) 0.2131(2) 0.0206(8) Uani 1 1 d . . . C18 C 0.0513(4) 0.2849(3) 0.2154(3) 0.0182(10) Uani 1 1 d . . . C19 C -0.0222(4) 0.1141(4) 0.2796(3) 0.0252(11) Uani 1 1 d . . . C20 C -0.1084(4) 0.1784(4) 0.3210(3) 0.0294(11) Uani 1 1 d . . . H20A H -0.0547 0.2595 0.3539 0.044 Uiso 1 1 calc R . . H20B H -0.1497 0.1387 0.3604 0.044 Uiso 1 1 calc R . . H20C H -0.1752 0.1778 0.2747 0.044 Uiso 1 1 calc R . . C21 C -0.1085(5) -0.0172(4) 0.2347(3) 0.0360(12) Uani 1 1 d . . . H21A H -0.1704 -0.0238 0.1831 0.054 Uiso 1 1 calc R . . H21B H -0.1556 -0.0479 0.2758 0.054 Uiso 1 1 calc R . . H21C H -0.0535 -0.0623 0.2171 0.054 Uiso 1 1 calc R . . C22 C 0.0935(5) 0.1271(4) 0.3526(3) 0.0330(12) Uani 1 1 d . . . H22A H 0.1487 0.0876 0.3265 0.049 Uiso 1 1 calc R . . H22B H 0.0598 0.0917 0.3963 0.049 Uiso 1 1 calc R . . H22C H 0.1444 0.2102 0.3807 0.049 Uiso 1 1 calc R . . C23 C 0.2415(5) 0.2084(4) 0.0479(3) 0.0318(12) Uani 1 1 d . . . H23A H 0.2517 0.1323 0.0293 0.048 Uiso 1 1 calc R . . H23B H 0.3268 0.2698 0.0730 0.048 Uiso 1 1 calc R . . H23C H 0.1985 0.2235 -0.0025 0.048 Uiso 1 1 calc R . . N1 N -0.1392(3) 0.4480(3) 0.2717(2) 0.0206(8) Uani 1 1 d . . . C25 C -0.2010(4) 0.4797(3) 0.2078(3) 0.0177(10) Uani 1 1 d . . . C26 C -0.1584(4) 0.5989(3) 0.2017(3) 0.0181(10) Uani 1 1 d . . . C27 C -0.0409(4) 0.6938(4) 0.2648(3) 0.0232(11) Uani 1 1 d . . . C28 C -0.0439(4) 0.7423(4) 0.3543(3) 0.0262(11) Uani 1 1 d . . . C29 C 0.0649(5) 0.8363(4) 0.4104(3) 0.0333(12) Uani 1 1 d . . . H29 H 0.0608 0.8694 0.4687 0.040 Uiso 1 1 calc R . . C30 C 0.1786(5) 0.8823(4) 0.3827(4) 0.0378(13) Uani 1 1 d . . . C31 C 0.1836(4) 0.8328(4) 0.2961(3) 0.0317(12) Uani 1 1 d . . . H31 H 0.2608 0.8620 0.2771 0.038 Uiso 1 1 calc R . . C32 C 0.0757(4) 0.7398(4) 0.2362(3) 0.0259(11) Uani 1 1 d . . . C33 C 0.0866(5) 0.6899(4) 0.1427(3) 0.0328(12) Uani 1 1 d . . . H33A H 0.0324 0.6068 0.1204 0.049 Uiso 1 1 calc R . . H33B H 0.1770 0.6987 0.1421 0.049 Uiso 1 1 calc R . . H33C H 0.0574 0.7323 0.1056 0.049 Uiso 1 1 calc R . . C34 C 0.2953(5) 0.9873(4) 0.4447(4) 0.0579(17) Uani 1 1 d . . . H34A H 0.3741 0.9891 0.4235 0.087 Uiso 1 1 calc R . . H34B H 0.3058 0.9791 0.5036 0.087 Uiso 1 1 calc R . . H34C H 0.2799 1.0602 0.4462 0.087 Uiso 1 1 calc R . . C35 C -0.1647(5) 0.6930(4) 0.3880(3) 0.0356(12) Uani 1 1 d . . . H35A H -0.2421 0.6797 0.3445 0.053 Uiso 1 1 calc R . . H35B H -0.1619 0.7487 0.4427 0.053 Uiso 1 1 calc R . . H35C H -0.1674 0.6187 0.3982 0.053 Uiso 1 1 calc R . . C36 C -0.2242(4) 0.6242(4) 0.1312(3) 0.0218(10) Uani 1 1 d . . . H36 H -0.1956 0.7018 0.1276 0.026 Uiso 1 1 calc R . . C37 C -0.3288(4) 0.5394(4) 0.0675(3) 0.0234(10) Uani 1 1 d . . . H37 H -0.3691 0.5584 0.0205 0.028 Uiso 1 1 calc R . . C38 C -0.3740(4) 0.4238(4) 0.0741(3) 0.0231(10) Uani 1 1 d . . . H38 H -0.4453 0.3656 0.0310 0.028 Uiso 1 1 calc R . . C39 C -0.3150(4) 0.3938(3) 0.1435(3) 0.0188(10) Uani 1 1 d . . . C40 C -0.3648(4) 0.2696(4) 0.1489(3) 0.0220(10) Uani 1 1 d . . . C41 C -0.4499(4) 0.2391(4) 0.2053(3) 0.0241(10) Uani 1 1 d . . . C42 C -0.4933(4) 0.1236(4) 0.2103(3) 0.0323(12) Uani 1 1 d . . . H42 H -0.5486 0.1045 0.2485 0.039 Uiso 1 1 calc R . . C43 C -0.4558(5) 0.0344(4) 0.1589(3) 0.0337(12) Uani 1 1 d . . . C44 C -0.3736(5) 0.0651(4) 0.1036(3) 0.0327(12) Uani 1 1 d . . . H44 H -0.3490 0.0066 0.0687 0.039 Uiso 1 1 calc R . . C45 C -0.3257(4) 0.1810(4) 0.0978(3) 0.0258(11) Uani 1 1 d . . . C46 C -0.2296(5) 0.2108(4) 0.0403(3) 0.0379(13) Uani 1 1 d . . . H46A H -0.2764 0.2068 -0.0167 0.057 Uiso 1 1 calc R . . H46B H -0.1845 0.1547 0.0324 0.057 Uiso 1 1 calc R . . H46C H -0.1665 0.2900 0.0684 0.057 Uiso 1 1 calc R . . C47 C -0.4996(5) -0.0904(4) 0.1680(4) 0.0533(16) Uani 1 1 d . . . H47A H -0.4792 -0.1428 0.1211 0.080 Uiso 1 1 calc R . . H47B H -0.5932 -0.1186 0.1642 0.080 Uiso 1 1 calc R . . H47C H -0.4542 -0.0890 0.2246 0.080 Uiso 1 1 calc R . . C48 C -0.4908(5) 0.3333(4) 0.2615(3) 0.0315(11) Uani 1 1 d . . . H48A H -0.4136 0.4010 0.2947 0.047 Uiso 1 1 calc R . . H48B H -0.5382 0.3014 0.3021 0.047 Uiso 1 1 calc R . . H48C H -0.5467 0.3574 0.2237 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0239(3) 0.0193(3) 0.0212(3) 0.0078(2) 0.0040(2) 0.0156(3) C1 0.034(3) 0.020(2) 0.012(2) 0.0041(19) 0.002(2) 0.021(2) N3 0.028(2) 0.0151(18) 0.019(2) 0.0030(16) 0.0021(17) 0.0121(17) C3 0.025(3) 0.021(2) 0.030(3) 0.009(2) 0.010(2) 0.014(2) C4 0.024(3) 0.025(2) 0.026(3) 0.006(2) 0.006(2) 0.014(2) C5 0.031(3) 0.038(3) 0.040(3) 0.008(2) 0.009(2) 0.014(2) N2 0.019(2) 0.0220(19) 0.029(2) 0.0095(18) 0.0040(18) 0.0133(17) C7 0.032(3) 0.033(3) 0.022(3) 0.011(2) 0.005(2) 0.023(2) C8 0.042(3) 0.039(3) 0.031(3) 0.014(2) 0.003(2) 0.026(2) C9 0.039(3) 0.036(3) 0.023(3) 0.005(2) 0.003(2) 0.021(2) C10 0.035(3) 0.038(3) 0.022(3) 0.010(2) 0.004(2) 0.018(2) C11 0.038(3) 0.026(3) 0.036(3) 0.009(2) 0.014(2) 0.013(2) C12 0.028(2) 0.022(2) 0.022(2) 0.009(2) 0.004(2) 0.013(2) N5 0.029(2) 0.0155(18) 0.022(2) 0.0040(16) -0.0004(17) 0.0140(17) C14 0.035(3) 0.023(2) 0.021(2) 0.005(2) 0.004(2) 0.020(2) C15 0.035(3) 0.022(2) 0.021(2) 0.005(2) 0.002(2) 0.018(2) C16 0.052(3) 0.029(3) 0.032(3) 0.010(2) 0.016(3) 0.025(2) N6 0.029(2) 0.0175(19) 0.020(2) 0.0051(16) 0.0056(17) 0.0163(16) C18 0.017(2) 0.021(2) 0.015(2) 0.0053(19) 0.0000(19) 0.0066(19) C19 0.034(3) 0.024(2) 0.023(3) 0.010(2) 0.009(2) 0.014(2) C20 0.038(3) 0.027(2) 0.033(3) 0.015(2) 0.016(2) 0.017(2) C21 0.046(3) 0.024(3) 0.044(3) 0.012(2) 0.018(3) 0.016(2) C22 0.048(3) 0.037(3) 0.024(3) 0.013(2) 0.009(2) 0.027(3) C23 0.051(3) 0.027(3) 0.029(3) 0.011(2) 0.016(2) 0.025(2) N1 0.024(2) 0.0168(18) 0.026(2) 0.0051(16) 0.0071(17) 0.0143(16) C25 0.019(2) 0.026(2) 0.015(2) 0.007(2) 0.0061(19) 0.017(2) C26 0.023(2) 0.022(2) 0.014(2) 0.0049(19) 0.0054(19) 0.015(2) C27 0.025(3) 0.021(2) 0.033(3) 0.017(2) 0.005(2) 0.017(2) C28 0.036(3) 0.023(2) 0.027(3) 0.009(2) 0.002(2) 0.020(2) C29 0.048(3) 0.025(3) 0.028(3) 0.008(2) -0.008(3) 0.022(3) C30 0.037(3) 0.027(3) 0.048(4) 0.015(3) -0.012(3) 0.015(2) C31 0.024(3) 0.023(3) 0.053(4) 0.023(3) 0.005(2) 0.008(2) C32 0.030(3) 0.022(2) 0.036(3) 0.016(2) 0.005(2) 0.018(2) C33 0.031(3) 0.031(3) 0.050(3) 0.024(2) 0.018(2) 0.019(2) C34 0.051(4) 0.036(3) 0.070(4) 0.017(3) -0.025(3) 0.007(3) C35 0.048(3) 0.042(3) 0.024(3) 0.007(2) 0.007(2) 0.028(3) C36 0.023(2) 0.021(2) 0.028(3) 0.013(2) 0.007(2) 0.012(2) C37 0.030(3) 0.029(3) 0.019(2) 0.013(2) 0.004(2) 0.018(2) C38 0.024(2) 0.025(2) 0.019(2) 0.001(2) 0.001(2) 0.012(2) C39 0.022(2) 0.023(2) 0.015(2) 0.0035(19) 0.005(2) 0.015(2) C40 0.023(2) 0.022(2) 0.021(2) 0.006(2) -0.002(2) 0.011(2) C41 0.022(2) 0.029(3) 0.021(2) 0.007(2) 0.000(2) 0.011(2) C42 0.027(3) 0.036(3) 0.032(3) 0.016(2) -0.001(2) 0.007(2) C43 0.032(3) 0.027(3) 0.036(3) 0.008(2) -0.004(2) 0.006(2) C44 0.042(3) 0.022(3) 0.029(3) -0.001(2) -0.001(2) 0.017(2) C45 0.031(3) 0.024(2) 0.020(2) 0.001(2) 0.001(2) 0.013(2) C46 0.046(3) 0.039(3) 0.036(3) 0.008(2) 0.013(3) 0.027(3) C47 0.053(4) 0.030(3) 0.068(4) 0.018(3) -0.002(3) 0.007(3) C48 0.031(3) 0.039(3) 0.028(3) 0.010(2) 0.007(2) 0.016(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 Ni1 N1 1.732(3) . ? Ni1 C1 1.872(4) . ? Ni1 C18 1.885(4) . ? C1 N2 1.360(5) . ? C1 N3 1.376(5) . ? N3 C3 1.393(5) . ? N3 C12 1.453(5) . ? C3 C4 1.336(6) . ? C3 C11 1.483(6) . ? C4 N2 1.411(5) . ? C4 C5 1.493(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? N2 C7 1.508(6) . ? C7 C10 1.505(6) . ? C7 C9 1.522(6) . ? C7 C8 1.527(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N5 1.466(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N5 C18 1.358(5) . ? N5 C14 1.393(5) . ? C14 C15 1.348(6) . ? C14 C23 1.485(6) . ? C15 N6 1.418(5) . ? C15 C16 1.498(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N6 C18 1.366(5) . ? N6 C19 1.502(5) . ? C19 C20 1.522(6) . ? C19 C21 1.531(6) . ? C19 C22 1.536(6) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 C25 1.344(5) . ? C25 C39 1.429(6) . ? C25 C26 1.431(5) . ? C26 C36 1.399(6) . ? C26 C27 1.479(6) . ? C27 C32 1.406(6) . ? C27 C28 1.411(6) . ? C28 C29 1.385(6) . ? C28 C35 1.497(6) . ? C29 C30 1.373(7) . ? C29 H29 0.9300 . ? C30 C31 1.378(7) . ? C30 C34 1.518(7) . ? C31 C32 1.396(6) . ? C31 H31 0.9300 . ? C32 C33 1.499(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.367(6) . ? C36 H36 0.9300 . ? C37 C38 1.393(6) . ? C37 H37 0.9300 . ? C38 C39 1.385(6) . ? C38 H38 0.9300 . ? C39 C40 1.489(6) . ? C40 C41 1.405(6) . ? C40 C45 1.408(6) . ? C41 C42 1.382(6) . ? C41 C48 1.507(6) . ? C42 C43 1.405(7) . ? C42 H42 0.9300 . ? C43 C44 1.371(7) . ? C43 C47 1.515(6) . ? C44 C45 1.394(6) . ? C44 H44 0.9300 . ? C45 C46 1.499(6) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 C1 128.70(16) . . ? N1 Ni1 C18 137.51(16) . . ? C1 Ni1 C18 89.79(16) . . ? N2 C1 N3 103.8(3) . . ? N2 C1 Ni1 141.3(3) . . ? N3 C1 Ni1 114.8(3) . . ? C1 N3 C3 111.9(3) . . ? C1 N3 C12 120.2(3) . . ? C3 N3 C12 127.5(4) . . ? C4 C3 N3 106.0(4) . . ? C4 C3 C11 132.0(4) . . ? N3 C3 C11 121.9(4) . . ? C3 C4 N2 107.8(4) . . ? C3 C4 C5 126.1(4) . . ? N2 C4 C5 125.9(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 N2 C4 110.4(4) . . ? C1 N2 C7 121.3(3) . . ? C4 N2 C7 125.3(4) . . ? C10 C7 N2 110.5(4) . . ? C10 C7 C9 107.3(4) . . ? N2 C7 C9 112.0(3) . . ? C10 C7 C8 109.9(4) . . ? N2 C7 C8 106.1(3) . . ? C9 C7 C8 111.1(4) . . ? 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 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 N5 109.0(3) . . ? N3 C12 H12A 109.9 . . ? N5 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? N5 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C18 N5 C14 113.0(3) . . ? C18 N5 C12 119.5(3) . . ? C14 N5 C12 127.3(4) . . ? C15 C14 N5 105.7(4) . . ? C15 C14 C23 131.0(4) . . ? N5 C14 C23 123.3(4) . . ? C14 C15 N6 106.9(3) . . ? C14 C15 C16 125.7(4) . . ? N6 C15 C16 127.4(4) . . ? 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 . . ? C18 N6 C15 110.7(3) . . ? C18 N6 C19 122.7(3) . . ? C15 N6 C19 125.4(3) . . ? N5 C18 N6 103.5(3) . . ? N5 C18 Ni1 116.0(3) . . ? N6 C18 Ni1 140.5(3) . . ? N6 C19 C20 110.2(3) . . ? N6 C19 C21 110.7(3) . . ? C20 C19 C21 108.0(4) . . ? N6 C19 C22 107.2(3) . . ? C20 C19 C22 109.4(4) . . ? C21 C19 C22 111.3(4) . . ? 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 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C14 C23 H23A 109.5 . . ? C14 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C14 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 N1 Ni1 127.3(3) . . ? N1 C25 C39 120.3(3) . . ? N1 C25 C26 122.4(4) . . ? C39 C25 C26 117.3(4) . . ? C36 C26 C25 119.3(4) . . ? C36 C26 C27 119.3(3) . . ? C25 C26 C27 121.3(3) . . ? C32 C27 C28 118.5(4) . . ? C32 C27 C26 120.6(4) . . ? C28 C27 C26 120.9(4) . . ? C29 C28 C27 119.6(4) . . ? C29 C28 C35 120.4(4) . . ? C27 C28 C35 120.0(4) . . ? C30 C29 C28 122.2(5) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C29 C30 C31 118.4(5) . . ? C29 C30 C34 121.2(5) . . ? C31 C30 C34 120.3(5) . . ? C30 C31 C32 121.7(5) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C31 C32 C27 119.5(4) . . ? C31 C32 C33 119.3(4) . . ? C27 C32 C33 121.1(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C28 C35 H35A 109.5 . . ? C28 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C28 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C26 122.6(4) . . ? C37 C36 H36 118.7 . . ? C26 C36 H36 118.7 . . ? C36 C37 C38 118.8(4) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 121.3(4) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C25 120.5(4) . . ? C38 C39 C40 120.3(4) . . ? C25 C39 C40 119.0(3) . . ? C41 C40 C45 119.0(4) . . ? C41 C40 C39 120.8(4) . . ? C45 C40 C39 120.2(4) . . ? C42 C41 C40 119.9(4) . . ? C42 C41 C48 120.4(4) . . ? C40 C41 C48 119.7(4) . . ? C41 C42 C43 121.4(4) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C44 C43 C42 118.2(4) . . ? C44 C43 C47 121.0(5) . . ? C42 C43 C47 120.8(5) . . ? C43 C44 C45 122.2(4) . . ? C43 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C44 C45 C40 119.4(4) . . ? C44 C45 C46 119.7(4) . . ? C40 C45 C46 120.9(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.810 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 901779' ####################################################################### # # 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_(TMTBM)Ni=N(dippp) #TrackingRef 'Bent imido complete cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H77 N5 Ni1' _chemical_formula_weight 878.96 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.2070(10) _cell_length_b 17.6940(14) _cell_length_c 21.9242(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5123.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21555 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.7860 _exptl_absorpt_correction_T_max 0.9204 _exptl_absorpt_process_details 'Norton et. al' _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 P4' _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 21483 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12325 _reflns_number_gt 11030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0504P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(8) _refine_ls_number_reflns 12325 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.090 _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 Ni Ni 0.687833(19) 0.850741(14) 0.183299(12) 0.01548(7) Uani 1 1 d . . . N1 N 0.78051(13) 0.89882(10) 0.14434(8) 0.0170(4) Uani 1 1 d . . . N2 N 0.45656(13) 0.87050(9) 0.18335(8) 0.0175(4) Uani 1 1 d . . . N3 N 0.53709(14) 0.87876(9) 0.26790(8) 0.0185(4) Uani 1 1 d . . . C811 C 0.98944(15) 0.85852(11) 0.17987(11) 0.0205(4) Uani 1 1 d . . . C211 C 0.43271(16) 0.85351(13) 0.11818(9) 0.0196(4) Uani 1 1 d . . . C856 C 0.70204(17) 1.02468(11) 0.04019(10) 0.0197(5) Uani 1 1 d . . . N5 N 0.71393(14) 0.69723(10) 0.24537(8) 0.0201(4) Uani 1 1 d . . . C4 C 0.43574(18) 0.88604(12) 0.28310(10) 0.0203(5) Uani 1 1 d . . . C3 C 0.38357(17) 0.88138(12) 0.23036(10) 0.0209(5) Uani 1 1 d . . . C1 C 0.55135(16) 0.86792(11) 0.20724(9) 0.0166(4) Uani 1 1 d . . . C5 C 0.62147(17) 0.86650(11) 0.30911(10) 0.0204(5) Uani 1 1 d . . . H5A H 0.6745 0.9051 0.3019 0.024 Uiso 1 1 calc R . . H5B H 0.5983 0.8710 0.3519 0.024 Uiso 1 1 calc R . . C853 C 0.56127(18) 1.10197(13) 0.11110(11) 0.0255(5) Uani 1 1 d . . . H85A H 0.5125 1.1278 0.1352 0.031 Uiso 1 1 calc R . . C2 C 0.69212(17) 0.77239(11) 0.24129(9) 0.0187(4) Uani 1 1 d . . . C81 C 0.95352(16) 0.93771(11) 0.16456(9) 0.0180(4) Uani 1 1 d . . . C815 C 1.02624(19) 0.75942(14) 0.25175(12) 0.0304(6) Uani 1 1 d . . . H81A H 1.0241 0.7402 0.2922 0.037 Uiso 1 1 calc R . . N4 N 0.66223(14) 0.79191(10) 0.29853(8) 0.0200(4) Uani 1 1 d . . . C7 C 0.69407(17) 0.67080(11) 0.30523(9) 0.0215(5) Uani 1 1 d . . . C860 C 0.77840(18) 0.98361(12) 0.00000(10) 0.0234(5) Uani 1 1 d . . . H86A H 0.8293 0.9593 0.0275 0.028 Uiso 1 1 calc R . . C851 C 0.72629(17) 1.04483(11) 0.10061(10) 0.0192(4) Uani 1 1 d . . . C857 C 0.6786(2) 1.10613(14) 0.20188(10) 0.0300(5) Uani 1 1 d . . . H85B H 0.7466 1.0853 0.2128 0.036 Uiso 1 1 calc R . . C82 C 1.02359(18) 0.99554(12) 0.16530(11) 0.0239(5) Uani 1 1 d . . . H82A H 1.0907 0.9848 0.1783 0.029 Uiso 1 1 calc R . . C852 C 0.65495(17) 1.08349(12) 0.13686(10) 0.0221(5) Uani 1 1 d . . . C511 C 0.73999(16) 0.64979(12) 0.19103(10) 0.0234(4) Uani 1 1 d . . . C80 C 0.85094(16) 0.95212(11) 0.14607(9) 0.0166(4) Uani 1 1 d . . . C84 C 0.90222(17) 1.08337(12) 0.12730(10) 0.0227(5) Uani 1 1 d . . . H84A H 0.8850 1.1330 0.1144 0.027 Uiso 1 1 calc R . . C816 C 0.98530(17) 0.83086(12) 0.23959(10) 0.0227(5) Uani 1 1 d . . . C820 C 0.9369(2) 0.87667(14) 0.29010(11) 0.0290(6) Uani 1 1 d . . . H82B H 0.8775 0.9039 0.2723 0.035 Uiso 1 1 calc R . . C85 C 0.82922(16) 1.02736(11) 0.12519(9) 0.0180(4) Uani 1 1 d . . . C214 C 0.3683(2) 0.91666(14) 0.09128(11) 0.0303(6) Uani 1 1 d . . . H21A H 0.4053 0.9646 0.0940 0.045 Uiso 1 1 calc R . . H21B H 0.3048 0.9207 0.1141 0.045 Uiso 1 1 calc R . . H21C H 0.3535 0.9054 0.0484 0.045 Uiso 1 1 calc R . . C817 C 1.03078(18) 0.84057(14) 0.06702(10) 0.0266(5) Uani 1 1 d . . . H81B H 1.0282 0.8971 0.0671 0.032 Uiso 1 1 calc R . . C854 C 0.53790(19) 1.08363(13) 0.05161(11) 0.0277(5) Uani 1 1 d . . . H85C H 0.4740 1.0972 0.0350 0.033 Uiso 1 1 calc R . . C60 C 0.6351(2) 0.73910(13) 0.40382(10) 0.0280(5) Uani 1 1 d . . . H60A H 0.6391 0.6898 0.4240 0.042 Uiso 1 1 calc R . . H60B H 0.5660 0.7589 0.4073 0.042 Uiso 1 1 calc R . . H60C H 0.6825 0.7742 0.4233 0.042 Uiso 1 1 calc R . . C514 C 0.7806(2) 0.69920(13) 0.13970(11) 0.0322(6) Uani 1 1 d . . . H51A H 0.7293 0.7368 0.1284 0.048 Uiso 1 1 calc R . . H51B H 0.7964 0.6676 0.1042 0.048 Uiso 1 1 calc R . . H51C H 0.8421 0.7251 0.1534 0.048 Uiso 1 1 calc R . . C6 C 0.66186(17) 0.73059(12) 0.33811(10) 0.0207(5) Uani 1 1 d . . . C855 C 0.60789(19) 1.04530(12) 0.01615(11) 0.0260(5) Uani 1 1 d . . . H85D H 0.5918 1.0329 -0.0249 0.031 Uiso 1 1 calc R . . C813 C 1.07240(19) 0.74349(13) 0.14777(12) 0.0307(6) Uani 1 1 d . . . H81C H 1.1019 0.7132 0.1167 0.037 Uiso 1 1 calc R . . C83 C 0.99973(18) 1.06922(12) 0.14772(11) 0.0255(5) Uani 1 1 d . . . H83A H 1.0488 1.1084 0.1497 0.031 Uiso 1 1 calc R . . C998 C 0.6915(3) 0.39898(14) 0.00779(12) 0.0418(7) Uani 1 1 d . . . C30 C 0.27120(18) 0.88496(14) 0.22365(12) 0.0275(5) Uani 1 1 d . . . H30A H 0.2402 0.8927 0.2638 0.041 Uiso 1 1 calc R . . H30B H 0.2465 0.8375 0.2061 0.041 Uiso 1 1 calc R . . H30C H 0.2532 0.9270 0.1967 0.041 Uiso 1 1 calc R . . C213 C 0.53093(17) 0.84960(16) 0.08114(10) 0.0271(5) Uani 1 1 d . . . H21D H 0.5653 0.8987 0.0827 0.041 Uiso 1 1 calc R . . H21E H 0.5151 0.8370 0.0387 0.041 Uiso 1 1 calc R . . H21F H 0.5752 0.8106 0.0983 0.041 Uiso 1 1 calc R . . C812 C 1.03310(17) 0.81425(12) 0.13293(11) 0.0233(5) Uani 1 1 d . . . C70 C 0.70555(18) 0.59178(13) 0.32854(11) 0.0290(6) Uani 1 1 d . . . H70A H 0.6858 0.5899 0.3716 0.043 Uiso 1 1 calc R . . H70B H 0.7763 0.5759 0.3244 0.043 Uiso 1 1 calc R . . H70C H 0.6620 0.5578 0.3049 0.043 Uiso 1 1 calc R . . C40 C 0.4007(2) 0.89741(14) 0.34711(11) 0.0288(5) Uani 1 1 d . . . H40A H 0.3268 0.9019 0.3478 0.043 Uiso 1 1 calc R . . H40B H 0.4309 0.9437 0.3636 0.043 Uiso 1 1 calc R . . H40C H 0.4215 0.8541 0.3721 0.043 Uiso 1 1 calc R . . C821 C 1.0101(2) 0.93644(16) 0.31584(14) 0.0431(7) Uani 1 1 d . . . H82C H 1.0352 0.9682 0.2825 0.065 Uiso 1 1 calc R . . H82D H 1.0672 0.9112 0.3358 0.065 Uiso 1 1 calc R . . H82E H 0.9743 0.9680 0.3456 0.065 Uiso 1 1 calc R . . C993 C 0.6261(2) 0.34229(18) -0.00751(13) 0.0471(7) Uani 1 1 d . . . H99A H 0.5671 0.3555 -0.0299 0.057 Uiso 1 1 calc R . . C814 C 1.0693(2) 0.71671(14) 0.20653(13) 0.0368(6) Uani 1 1 d . . . H81D H 1.0971 0.6685 0.2158 0.044 Uiso 1 1 calc R . . C819 C 0.9351(2) 0.81186(14) 0.03587(11) 0.0328(6) Uani 1 1 d . . . H81E H 0.9340 0.8291 -0.0066 0.049 Uiso 1 1 calc R . . H81F H 0.8755 0.8315 0.0573 0.049 Uiso 1 1 calc R . . H81G H 0.9341 0.7565 0.0369 0.049 Uiso 1 1 calc R . . C212 C 0.3800(2) 0.77663(13) 0.11519(12) 0.0311(6) Uani 1 1 d . . . H21G H 0.3169 0.7786 0.1386 0.047 Uiso 1 1 calc R . . H21H H 0.4246 0.7378 0.1324 0.047 Uiso 1 1 calc R . . H21I H 0.3648 0.7642 0.0726 0.047 Uiso 1 1 calc R . . C997 C 0.7797(3) 0.37813(18) 0.04173(13) 0.0489(8) Uani 1 1 d . . . H99B H 0.8280 0.4153 0.0531 0.059 Uiso 1 1 calc R . . C818 C 1.1243(2) 0.81640(18) 0.03002(12) 0.0420(7) Uani 1 1 d . . . H81H H 1.1856 0.8356 0.0498 0.063 Uiso 1 1 calc R . . H81I H 1.1196 0.8371 -0.0114 0.063 Uiso 1 1 calc R . . H81J H 1.1273 0.7611 0.0280 0.063 Uiso 1 1 calc R . . C996 C 0.7941(2) 0.30236(18) 0.05803(12) 0.0441(7) Uani 1 1 d . . . H99C H 0.8518 0.2875 0.0809 0.053 Uiso 1 1 calc R . . C822 C 0.8984(2) 0.82863(16) 0.34354(11) 0.0362(6) Uani 1 1 d . . . H82F H 0.8509 0.7905 0.3283 0.054 Uiso 1 1 calc R . . H82G H 0.8640 0.8612 0.3731 0.054 Uiso 1 1 calc R . . H82H H 0.9558 0.8035 0.3633 0.054 Uiso 1 1 calc R . . C858 C 0.6006(4) 1.0730(2) 0.24582(15) 0.104(2) Uani 1 1 d . . . H85E H 0.6170 1.0884 0.2876 0.157 Uiso 1 1 calc R . . H85F H 0.6018 1.0177 0.2430 0.157 Uiso 1 1 calc R . . H85G H 0.5330 1.0915 0.2350 0.157 Uiso 1 1 calc R . . C513 C 0.6440(2) 0.61005(15) 0.16996(13) 0.0392(7) Uani 1 1 d . . . H51D H 0.5920 0.6478 0.1605 0.059 Uiso 1 1 calc R . . H51E H 0.6195 0.5767 0.2024 0.059 Uiso 1 1 calc R . . H51F H 0.6587 0.5801 0.1334 0.059 Uiso 1 1 calc R . . C994 C 0.6393(3) 0.26994(17) 0.00679(14) 0.0490(8) Uani 1 1 d . . . H99D H 0.5917 0.2328 -0.0059 0.059 Uiso 1 1 calc R . . C859 C 0.6808(4) 1.18853(17) 0.21111(14) 0.0829(15) Uani 1 1 d . . . H85H H 0.7330 1.2109 0.1850 0.124 Uiso 1 1 calc R . . H85I H 0.6962 1.1996 0.2539 0.124 Uiso 1 1 calc R . . H85J H 0.6146 1.2100 0.2006 0.124 Uiso 1 1 calc R . . C512 C 0.8233(2) 0.59246(15) 0.20658(12) 0.0387(6) Uani 1 1 d . . . H51G H 0.7998 0.5591 0.2393 0.058 Uiso 1 1 calc R . . H51H H 0.8842 0.6194 0.2200 0.058 Uiso 1 1 calc R . . H51I H 0.8392 0.5623 0.1704 0.058 Uiso 1 1 calc R . . C995 C 0.7233(3) 0.24979(19) 0.04040(13) 0.0457(8) Uani 1 1 d . . . H99E H 0.7325 0.1984 0.0516 0.055 Uiso 1 1 calc R . . C861 C 0.7315(2) 0.92181(17) -0.03869(13) 0.0414(7) Uani 1 1 d . . . H86B H 0.6960 0.8859 -0.0123 0.062 Uiso 1 1 calc R . . H86C H 0.7849 0.8954 -0.0613 0.062 Uiso 1 1 calc R . . H86D H 0.6834 0.9442 -0.0675 0.062 Uiso 1 1 calc R . . C862 C 0.8347(2) 1.03999(16) -0.04012(13) 0.0463(8) Uani 1 1 d . . . H86E H 0.8649 1.0794 -0.0145 0.069 Uiso 1 1 calc R . . H86F H 0.7872 1.0631 -0.0690 0.069 Uiso 1 1 calc R . . H86G H 0.8882 1.0137 -0.0627 0.069 Uiso 1 1 calc R . . C999 C 0.6743(3) 0.48013(17) -0.00491(16) 0.0677(11) Uani 1 1 d . . . H99F H 0.6117 0.4861 -0.0284 0.101 Uiso 1 1 calc R . . H99G H 0.7314 0.5003 -0.0284 0.101 Uiso 1 1 calc R . . H99H H 0.6684 0.5077 0.0337 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01385(12) 0.01578(12) 0.01680(12) 0.00145(11) 0.00036(11) -0.00068(11) N1 0.0137(9) 0.0183(9) 0.0189(9) 0.0033(7) 0.0000(7) 0.0027(7) N2 0.0162(9) 0.0183(8) 0.0180(9) 0.0012(7) 0.0017(8) 0.0002(6) N3 0.0209(10) 0.0181(9) 0.0166(9) -0.0001(7) 0.0015(7) 0.0008(7) C811 0.0144(10) 0.0166(10) 0.0305(12) -0.0004(10) -0.0060(9) -0.0006(8) C211 0.0175(10) 0.0221(10) 0.0192(10) -0.0040(9) -0.0015(8) -0.0016(10) C856 0.0207(12) 0.0168(10) 0.0217(11) 0.0020(8) 0.0001(9) -0.0017(9) N5 0.0159(9) 0.0188(8) 0.0255(10) 0.0030(7) -0.0010(7) -0.0006(7) C4 0.0228(12) 0.0143(10) 0.0240(12) -0.0005(9) 0.0053(9) 0.0010(9) C3 0.0204(12) 0.0171(10) 0.0252(12) -0.0014(9) 0.0063(9) 0.0005(9) C1 0.0166(11) 0.0146(10) 0.0187(10) 0.0016(8) -0.0014(8) -0.0004(8) C5 0.0233(11) 0.0229(11) 0.0150(10) -0.0005(8) -0.0024(9) -0.0033(8) C853 0.0224(12) 0.0243(11) 0.0297(13) -0.0005(10) 0.0026(10) 0.0016(9) C2 0.0134(10) 0.0198(10) 0.0231(11) 0.0008(8) -0.0022(9) -0.0017(9) C81 0.0172(11) 0.0172(10) 0.0196(11) -0.0009(8) -0.0012(8) 0.0010(8) C815 0.0255(14) 0.0317(13) 0.0341(14) 0.0088(11) -0.0063(11) -0.0019(10) N4 0.0215(10) 0.0198(9) 0.0187(9) 0.0041(7) -0.0026(7) -0.0019(7) C7 0.0157(10) 0.0235(10) 0.0253(12) 0.0069(8) -0.0043(9) -0.0017(9) C860 0.0249(12) 0.0236(11) 0.0217(12) 0.0015(9) -0.0009(9) 0.0018(9) C851 0.0189(11) 0.0151(10) 0.0235(11) 0.0045(9) -0.0017(9) -0.0011(8) C857 0.0233(13) 0.0419(14) 0.0249(12) -0.0028(10) 0.0017(10) 0.0145(11) C82 0.0178(11) 0.0224(11) 0.0315(13) -0.0013(9) -0.0033(9) -0.0008(9) C852 0.0209(12) 0.0222(11) 0.0233(12) 0.0047(9) -0.0019(9) 0.0003(9) C511 0.0251(11) 0.0178(10) 0.0273(12) -0.0010(10) 0.0007(9) 0.0016(9) C80 0.0171(10) 0.0189(10) 0.0137(10) -0.0031(8) 0.0000(8) 0.0011(8) C84 0.0238(13) 0.0161(10) 0.0280(12) 0.0030(9) 0.0005(10) -0.0002(9) C816 0.0169(11) 0.0247(12) 0.0266(12) 0.0031(9) -0.0048(9) -0.0029(8) C820 0.0265(13) 0.0355(14) 0.0249(12) 0.0035(10) 0.0025(10) -0.0034(10) C85 0.0180(12) 0.0194(10) 0.0166(10) -0.0014(8) -0.0005(8) 0.0006(8) C214 0.0310(14) 0.0310(13) 0.0289(13) 0.0006(10) -0.0077(11) 0.0045(11) C817 0.0277(13) 0.0263(12) 0.0256(12) -0.0052(10) -0.0004(9) 0.0014(10) C854 0.0215(13) 0.0259(12) 0.0357(14) 0.0040(10) -0.0062(10) 0.0027(10) C60 0.0316(14) 0.0291(12) 0.0234(12) 0.0055(10) -0.0046(10) -0.0071(10) C514 0.0416(16) 0.0232(12) 0.0319(14) -0.0009(10) 0.0078(11) 0.0036(11) C6 0.0178(12) 0.0236(11) 0.0207(11) 0.0079(9) -0.0052(8) -0.0067(9) C855 0.0301(13) 0.0228(11) 0.0250(12) -0.0001(10) -0.0073(10) -0.0005(10) C813 0.0250(13) 0.0243(12) 0.0429(16) -0.0092(11) -0.0013(12) 0.0043(10) C83 0.0208(12) 0.0191(11) 0.0365(14) 0.0002(10) -0.0029(10) -0.0048(9) C998 0.060(2) 0.0338(13) 0.0317(14) 0.0071(11) 0.0243(15) 0.0075(14) C30 0.0190(12) 0.0288(12) 0.0348(14) -0.0011(10) 0.0050(10) 0.0010(10) C213 0.0233(12) 0.0411(13) 0.0170(11) -0.0022(11) 0.0005(9) 0.0006(11) C812 0.0188(12) 0.0209(11) 0.0300(13) -0.0040(10) -0.0027(9) -0.0012(9) C70 0.0235(13) 0.0253(11) 0.0380(14) 0.0111(10) -0.0009(10) -0.0004(9) C40 0.0335(15) 0.0285(12) 0.0245(12) 0.0006(10) 0.0082(10) 0.0046(11) C821 0.0488(17) 0.0471(16) 0.0335(15) -0.0123(14) 0.0112(15) -0.0194(13) C993 0.0531(19) 0.0552(18) 0.0329(15) 0.0002(14) 0.0135(13) -0.0084(16) C814 0.0307(15) 0.0210(12) 0.0586(18) 0.0071(12) -0.0104(13) 0.0049(11) C819 0.0325(15) 0.0357(14) 0.0302(14) -0.0075(11) -0.0029(11) 0.0061(12) C212 0.0349(15) 0.0257(12) 0.0326(14) -0.0081(11) 0.0042(11) -0.0061(11) C997 0.052(2) 0.061(2) 0.0343(16) -0.0097(14) 0.0250(14) -0.0052(15) C818 0.0311(15) 0.0587(19) 0.0361(15) -0.0075(13) 0.0035(12) -0.0077(13) C996 0.0450(19) 0.0583(18) 0.0289(14) 0.0006(13) 0.0135(13) 0.0070(15) C822 0.0282(14) 0.0533(17) 0.0269(13) 0.0062(12) -0.0011(11) -0.0075(12) C858 0.210(6) 0.075(3) 0.0285(17) -0.0081(17) 0.021(3) -0.083(3) C513 0.0390(16) 0.0342(14) 0.0444(17) -0.0082(12) 0.0010(13) -0.0100(12) C994 0.060(2) 0.0467(18) 0.0402(17) 0.0010(14) 0.0104(16) -0.0024(15) C859 0.170(5) 0.0376(17) 0.0411(18) -0.0032(14) -0.030(3) -0.029(2) C512 0.0415(17) 0.0313(13) 0.0432(15) 0.0072(11) 0.0078(13) 0.0148(13) C995 0.051(2) 0.0561(18) 0.0304(15) 0.0058(14) 0.0117(13) 0.0096(15) C861 0.0369(16) 0.0489(17) 0.0385(15) -0.0210(13) -0.0006(13) 0.0040(13) C862 0.0441(19) 0.0458(16) 0.0491(17) 0.0107(14) 0.0224(14) 0.0068(14) C999 0.095(3) 0.0504(19) 0.057(2) 0.0069(16) 0.027(2) -0.006(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 Ni N1 1.7180(17) . ? Ni C2 1.882(2) . ? Ni C1 1.902(2) . ? N1 C80 1.325(3) . ? N2 C1 1.358(3) . ? N2 C3 1.424(3) . ? N2 C211 1.494(3) . ? N3 C1 1.357(3) . ? N3 C4 1.385(3) . ? N3 C5 1.451(3) . ? C811 C816 1.399(3) . ? C811 C812 1.416(3) . ? C811 C81 1.517(3) . ? C211 C214 1.523(3) . ? C211 C212 1.529(3) . ? C211 C213 1.532(3) . ? C856 C855 1.399(3) . ? C856 C851 1.409(3) . ? C856 C860 1.524(3) . ? N5 C2 1.364(3) . ? N5 C7 1.418(3) . ? N5 C511 1.497(3) . ? C4 C3 1.349(3) . ? C4 C40 1.491(3) . ? C3 C30 1.493(3) . ? C5 N4 1.444(3) . ? C853 C854 1.379(3) . ? C853 C852 1.399(3) . ? C2 N4 1.360(3) . ? C81 C82 1.380(3) . ? C81 C80 1.437(3) . ? C815 C814 1.370(4) . ? C815 C816 1.401(3) . ? N4 C6 1.389(3) . ? C7 C6 1.349(3) . ? C7 C70 1.496(3) . ? C860 C861 1.516(3) . ? C860 C862 1.524(3) . ? C851 C852 1.410(3) . ? C851 C85 1.495(3) . ? C857 C859 1.472(4) . ? C857 C852 1.513(3) . ? C857 C858 1.527(5) . ? C82 C83 1.396(3) . ? C511 C513 1.522(3) . ? C511 C514 1.522(3) . ? C511 C512 1.535(3) . ? C80 C85 1.437(3) . ? C84 C85 1.384(3) . ? C84 C83 1.386(3) . ? C816 C820 1.514(3) . ? C820 C822 1.534(3) . ? C820 C821 1.539(3) . ? C817 C812 1.519(3) . ? C817 C819 1.524(3) . ? C817 C818 1.538(3) . ? C854 C855 1.385(3) . ? C60 C6 1.491(3) . ? C813 C814 1.373(4) . ? C813 C812 1.394(3) . ? C998 C993 1.366(4) . ? C998 C997 1.431(5) . ? C998 C999 1.480(4) . ? C993 C994 1.330(4) . ? C997 C996 1.400(4) . ? C996 C995 1.374(5) . ? C994 C995 1.379(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 N1 Ni C2 132.79(9) . . ? N1 Ni C1 137.17(8) . . ? C2 Ni C1 87.70(9) . . ? C80 N1 Ni 146.96(15) . . ? C1 N2 C3 110.45(18) . . ? C1 N2 C211 123.83(17) . . ? C3 N2 C211 125.22(17) . . ? C1 N3 C4 112.51(18) . . ? C1 N3 C5 118.86(18) . . ? C4 N3 C5 127.32(18) . . ? C816 C811 C812 120.2(2) . . ? C816 C811 C81 121.2(2) . . ? C812 C811 C81 118.5(2) . . ? N2 C211 C214 109.91(18) . . ? N2 C211 C212 108.42(18) . . ? C214 C211 C212 112.45(19) . . ? N2 C211 C213 109.73(17) . . ? C214 C211 C213 107.50(19) . . ? C212 C211 C213 108.8(2) . . ? C855 C856 C851 119.4(2) . . ? C855 C856 C860 119.7(2) . . ? C851 C856 C860 120.9(2) . . ? C2 N5 C7 110.08(18) . . ? C2 N5 C511 122.89(18) . . ? C7 N5 C511 126.46(17) . . ? C3 C4 N3 106.37(19) . . ? C3 C4 C40 131.1(2) . . ? N3 C4 C40 122.6(2) . . ? C4 C3 N2 106.44(19) . . ? C4 C3 C30 126.1(2) . . ? N2 C3 C30 127.4(2) . . ? N3 C1 N2 104.21(18) . . ? N3 C1 Ni 115.12(15) . . ? N2 C1 Ni 140.60(16) . . ? N4 C5 N3 108.84(17) . . ? C854 C853 C852 121.7(2) . . ? N4 C2 N5 104.38(18) . . ? N4 C2 Ni 115.31(14) . . ? N5 C2 Ni 140.28(17) . . ? C82 C81 C80 120.27(19) . . ? C82 C81 C811 118.21(19) . . ? C80 C81 C811 121.41(18) . . ? C814 C815 C816 121.4(2) . . ? C2 N4 C6 112.27(18) . . ? C2 N4 C5 119.24(17) . . ? C6 N4 C5 127.74(18) . . ? C6 C7 N5 107.12(17) . . ? C6 C7 C70 125.6(2) . . ? N5 C7 C70 127.3(2) . . ? C861 C860 C856 113.4(2) . . ? C861 C860 C862 110.4(2) . . ? C856 C860 C862 110.15(19) . . ? C856 C851 C852 120.1(2) . . ? C856 C851 C85 119.56(19) . . ? C852 C851 C85 120.34(19) . . ? C859 C857 C852 113.3(2) . . ? C859 C857 C858 107.9(3) . . ? C852 C857 C858 110.7(2) . . ? C81 C82 C83 122.6(2) . . ? C853 C852 C851 118.5(2) . . ? C853 C852 C857 120.1(2) . . ? C851 C852 C857 121.4(2) . . ? N5 C511 C513 108.00(19) . . ? N5 C511 C514 110.30(18) . . ? C513 C511 C514 109.5(2) . . ? N5 C511 C512 111.00(18) . . ? C513 C511 C512 111.1(2) . . ? C514 C511 C512 106.9(2) . . ? N1 C80 C85 120.68(19) . . ? N1 C80 C81 122.93(18) . . ? C85 C80 C81 116.27(19) . . ? C85 C84 C83 121.9(2) . . ? C811 C816 C815 118.6(2) . . ? C811 C816 C820 120.92(19) . . ? C815 C816 C820 120.5(2) . . ? C816 C820 C822 113.7(2) . . ? C816 C820 C821 111.8(2) . . ? C822 C820 C821 108.0(2) . . ? C84 C85 C80 120.93(19) . . ? C84 C85 C851 119.85(19) . . ? C80 C85 C851 119.22(18) . . ? C812 C817 C819 109.9(2) . . ? C812 C817 C818 113.6(2) . . ? C819 C817 C818 109.7(2) . . ? C853 C854 C855 119.8(2) . . ? C7 C6 N4 106.12(18) . . ? C7 C6 C60 132.1(2) . . ? N4 C6 C60 121.7(2) . . ? C854 C855 C856 120.6(2) . . ? C814 C813 C812 121.2(2) . . ? C84 C83 C82 117.9(2) . . ? C993 C998 C997 117.0(3) . . ? C993 C998 C999 124.7(3) . . ? C997 C998 C999 118.2(3) . . ? C813 C812 C811 118.6(2) . . ? C813 C812 C817 120.3(2) . . ? C811 C812 C817 120.9(2) . . ? C994 C993 C998 124.5(3) . . ? C815 C814 C813 120.0(2) . . ? C996 C997 C998 119.3(3) . . ? C995 C996 C997 119.0(3) . . ? C993 C994 C995 118.7(3) . . ? C996 C995 C994 121.5(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.643 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 901780' ####################################################################### # # 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_[(TMTBM)Ni=N(dippp)]FABA #TrackingRef 'Bent imido complete cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C146 H136 B2 F40 N10 Ni2' _chemical_formula_weight 2929.65 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.779(2) _cell_length_b 15.500(2) _cell_length_c 16.733(3) _cell_angle_alpha 92.788(4) _cell_angle_beta 98.247(3) _cell_angle_gamma 100.522(4) _cell_volume 3718.6(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21565 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details 'Norton et. al.' _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 _d_diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23669 _diffrn_reflns_av_R_equivalents 0.1595 _diffrn_reflns_av_sigmaI/netI 0.5988 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13101 _reflns_number_gt 12806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0926P)^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 6295 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.2498 _refine_ls_wR_factor_gt 0.2298 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Ni1 Ni 0.37708(10) 0.74552(9) 0.27537(8) 0.0248(4) Uani 1 1 d . . . N1 N 0.4325(6) 0.6987(5) 0.2055(5) 0.028(2) Uani 1 1 d . . . N2 N 0.4115(8) 0.7362(6) 0.4582(6) 0.041(3) Uani 1 1 d . . . N3 N 0.2804(8) 0.6757(6) 0.3917(6) 0.035(3) Uani 1 1 d . . . N4 N 0.1906(7) 0.7386(6) 0.2905(6) 0.040(3) Uani 1 1 d . . . N5 N 0.2334(7) 0.8634(6) 0.2422(6) 0.037(3) Uani 1 1 d . . . C1 C 0.3617(8) 0.7227(7) 0.3825(7) 0.026(3) Uani 1 1 d . . . C2 C 0.2647(8) 0.7917(7) 0.2648(6) 0.030(3) Uani 1 1 d . . . C3 C 0.2038(8) 0.6555(7) 0.3256(8) 0.039(3) Uani 1 1 d . . . H3A H 0.1464 0.6275 0.3455 0.047 Uiso 1 1 calc R . . H3B H 0.2177 0.6142 0.2841 0.047 Uiso 1 1 calc R . . C4 C 0.3654(12) 0.6983(8) 0.5170(9) 0.051(4) Uani 1 1 d . . . C5 C 0.2790(12) 0.6568(8) 0.4730(9) 0.051(4) Uani 1 1 d . . . C6 C 0.1114(9) 0.7750(9) 0.2806(8) 0.050(4) Uani 1 1 d . . . C7 C 0.1397(9) 0.8518(9) 0.2501(7) 0.042(3) Uani 1 1 d . . . C11 C 0.4528(7) 0.6465(7) 0.1506(7) 0.026(3) Uani 1 1 d . . . C12 C 0.4288(8) 0.6588(7) 0.0657(6) 0.026(3) Uani 1 1 d . . . C13 C 0.4470(8) 0.6002(7) 0.0121(7) 0.031(3) Uani 1 1 d . . . H13A H 0.4281 0.6073 -0.0436 0.037 Uiso 1 1 calc R . . C14 C 0.4916(8) 0.5285(6) 0.0300(6) 0.031(3) Uani 1 1 d . . . C15 C 0.5193(7) 0.5217(6) 0.1140(6) 0.021(2) Uani 1 1 d . . . H15A H 0.5518 0.4763 0.1298 0.025 Uiso 1 1 calc R . . C16 C 0.5016(7) 0.5770(6) 0.1729(6) 0.021(3) Uani 1 1 d . . . C21 C 0.5062(7) 0.7932(6) 0.4763(6) 0.068(5) Uani 1 1 d . . . C40 C 0.3863(11) 0.6980(8) 0.6057(7) 0.068(5) Uani 1 1 d . . . H40A H 0.3517 0.6437 0.6230 0.103 Uiso 1 1 calc R . . H40B H 0.3677 0.7489 0.6311 0.103 Uiso 1 1 calc R . . H40C H 0.4532 0.7010 0.6220 0.103 Uiso 1 1 calc R . . C50 C 0.1939(11) 0.5975(8) 0.4984(7) 0.068(5) Uani 1 1 d . . . H50A H 0.2066 0.5895 0.5564 0.140 Uiso 1 1 calc R . . H50B H 0.1816 0.5401 0.4676 0.140 Uiso 1 1 calc R . . H50C H 0.1393 0.6253 0.4875 0.140 Uiso 1 1 calc R . . C51 C 0.2911(9) 0.9441(7) 0.2185(7) 0.037(3) Uani 1 1 d . . . C60 C 0.0234(8) 0.7281(10) 0.3038(9) 0.080(5) Uani 1 1 d . . . H60A H -0.0296 0.7459 0.2711 0.119 Uiso 1 1 calc R . . H60B H 0.0226 0.7429 0.3612 0.119 Uiso 1 1 calc R . . H60C H 0.0190 0.6645 0.2943 0.119 Uiso 1 1 calc R . . C70 C 0.0784(9) 0.9176(9) 0.2253(9) 0.074(5) Uani 1 1 d . . . H70A H 0.0239 0.9081 0.2532 0.111 Uiso 1 1 calc R . . H70B H 0.0578 0.9097 0.1666 0.111 Uiso 1 1 calc R . . H70C H 0.1138 0.9775 0.2399 0.111 Uiso 1 1 calc R . . C121 C 0.3898(8) 0.7368(7) 0.0389(6) 0.024(3) Uani 1 1 d . . . C122 C 0.2944(8) 0.7303(6) 0.0228(6) 0.024(3) Uani 1 1 d . . . C123 C 0.2580(8) 0.7975(7) -0.0144(6) 0.027(3) Uani 1 1 d . . . H12B H 0.1925 0.7923 -0.0285 0.033 Uiso 1 1 calc R . . C124 C 0.3174(8) 0.8714(8) -0.0308(6) 0.033(3) Uani 1 1 d . . . H12C H 0.2930 0.9178 -0.0557 0.040 Uiso 1 1 calc R . . C125 C 0.4125(8) 0.8781(7) -0.0109(6) 0.027(3) Uani 1 1 d . . . H12A H 0.4531 0.9306 -0.0199 0.032 Uiso 1 1 calc R . . C126 C 0.4503(7) 0.8080(7) 0.0226(6) 0.021(2) Uani 1 1 d . . . C127 C 0.5544(7) 0.8214(7) 0.0449(7) 0.027(3) Uani 1 1 d . . . H12D H 0.5688 0.7623 0.0567 0.033 Uiso 1 1 calc R . . C128 C 0.6081(8) 0.8526(8) -0.0229(7) 0.047(4) Uani 1 1 d . . . H12E H 0.5932 0.8074 -0.0683 0.071 Uiso 1 1 calc R . . H12F H 0.6751 0.8633 -0.0028 0.071 Uiso 1 1 calc R . . H12G H 0.5906 0.9073 -0.0411 0.071 Uiso 1 1 calc R . . C129 C 0.5892(8) 0.8802(7) 0.1222(7) 0.045(3) Uani 1 1 d . . . H12H H 0.5567 0.8561 0.1657 0.067 Uiso 1 1 calc R . . H12I H 0.5771 0.9394 0.1136 0.067 Uiso 1 1 calc R . . H12J H 0.6563 0.8832 0.1374 0.067 Uiso 1 1 calc R . . C130 C 0.2251(8) 0.6476(7) 0.0381(7) 0.036(3) Uani 1 1 d . . . H13B H 0.2602 0.6151 0.0782 0.043 Uiso 1 1 calc R . . C131 C 0.1448(8) 0.6709(7) 0.0769(7) 0.040(3) Uani 1 1 d . . . H13C H 0.1693 0.7151 0.1224 0.061 Uiso 1 1 calc R . . H13D H 0.1105 0.6179 0.0965 0.061 Uiso 1 1 calc R . . H13E H 0.1029 0.6947 0.0367 0.061 Uiso 1 1 calc R . . C132 C 0.1914(9) 0.5847(7) -0.0390(8) 0.049(4) Uani 1 1 d . . . H13F H 0.1495 0.5322 -0.0264 0.074 Uiso 1 1 calc R . . H13G H 0.2451 0.5673 -0.0590 0.074 Uiso 1 1 calc R . . H13H H 0.1580 0.6145 -0.0807 0.074 Uiso 1 1 calc R . . C161 C 0.5408(8) 0.5656(6) 0.2616(6) 0.017(2) Uani 1 1 d . . . C162 C 0.6296(7) 0.6005(6) 0.2943(6) 0.017(2) Uani 1 1 d . . . C163 C 0.6647(8) 0.5827(7) 0.3705(6) 0.032(3) Uani 1 1 d . . . H16B H 0.7277 0.6055 0.3932 0.038 Uiso 1 1 calc R . . C164 C 0.6064(9) 0.5309(8) 0.4132(7) 0.044(3) Uani 1 1 d . . . H16G H 0.6306 0.5180 0.4661 0.053 Uiso 1 1 calc R . . C165 C 0.5162(8) 0.4972(7) 0.3839(6) 0.033(3) Uani 1 1 d . . . H16C H 0.4778 0.4637 0.4167 0.040 Uiso 1 1 calc R . . C166 C 0.4798(7) 0.5116(6) 0.3062(6) 0.022(3) Uani 1 1 d . . . C167 C 0.3820(8) 0.4692(7) 0.2714(7) 0.036(3) Uani 1 1 d . . . H16A H 0.3600 0.5055 0.2275 0.044 Uiso 1 1 calc R . . C168 C 0.3794(8) 0.3733(7) 0.2311(7) 0.042(3) Uani 1 1 d . . . H16H H 0.4181 0.3777 0.1880 0.064 Uiso 1 1 calc R . . H16I H 0.3151 0.3463 0.2082 0.064 Uiso 1 1 calc R . . H16J H 0.4035 0.3369 0.2724 0.064 Uiso 1 1 calc R . . C169 C 0.3133(8) 0.4625(7) 0.3309(7) 0.041(3) Uani 1 1 d . . . H16D H 0.3197 0.5198 0.3608 0.062 Uiso 1 1 calc R . . H16E H 0.3260 0.4186 0.3690 0.062 Uiso 1 1 calc R . . H16F H 0.2498 0.4448 0.3014 0.062 Uiso 1 1 calc R . . C170 C 0.6959(8) 0.6617(8) 0.2500(7) 0.040(3) Uani 1 1 d . . . H17A H 0.6569 0.6790 0.2017 0.048 Uiso 1 1 calc R . . C171 C 0.7440(11) 0.7466(7) 0.2997(9) 0.081(5) Uani 1 1 d . . . H17B H 0.7862 0.7819 0.2684 0.122 Uiso 1 1 calc R . . H17C H 0.7796 0.7327 0.3499 0.122 Uiso 1 1 calc R . . H17D H 0.6971 0.7800 0.3129 0.122 Uiso 1 1 calc R . . C172 C 0.7638(9) 0.6113(8) 0.2178(8) 0.057(4) Uani 1 1 d . . . H17E H 0.8010 0.6485 0.1840 0.086 Uiso 1 1 calc R . . H17F H 0.7291 0.5581 0.1853 0.086 Uiso 1 1 calc R . . H17G H 0.8051 0.5948 0.2632 0.086 Uiso 1 1 calc R . . C211 C 0.5061(13) 0.8734(11) 0.5353(12) 0.138(9) Uani 1 1 d . . . H21G H 0.4555 0.9031 0.5146 0.207 Uiso 1 1 calc R . . H21H H 0.5659 0.9144 0.5400 0.207 Uiso 1 1 calc R . . H21I H 0.4969 0.8533 0.5887 0.207 Uiso 1 1 calc R . . C212 C 0.5371(12) 0.8295(11) 0.3984(11) 0.138(9) Uani 1 1 d . . . H21A H 0.4882 0.8568 0.3700 0.194 Uiso 1 1 calc R . . H21B H 0.5481 0.7813 0.3632 0.194 Uiso 1 1 calc R . . H21C H 0.5947 0.8736 0.4124 0.194 Uiso 1 1 calc R . . C213 C 0.5746(12) 0.7407(12) 0.5118(13) 0.142(9) Uani 1 1 d . . . H21D H 0.5785 0.6936 0.4720 0.213 Uiso 1 1 calc R . . H21E H 0.5544 0.7149 0.5602 0.213 Uiso 1 1 calc R . . H21F H 0.6359 0.7790 0.5268 0.213 Uiso 1 1 calc R . . C511 C 0.3112(10) 1.0152(7) 0.2870(8) 0.066(5) Uani 1 1 d . . . H51A H 0.2524 1.0265 0.3018 0.099 Uiso 1 1 calc R . . H51B H 0.3462 1.0693 0.2698 0.099 Uiso 1 1 calc R . . H51C H 0.3481 0.9961 0.3339 0.099 Uiso 1 1 calc R . . C512 C 0.2424(9) 0.9762(8) 0.1410(7) 0.050(4) Uani 1 1 d . . . H51D H 0.1926 1.0057 0.1543 0.076 Uiso 1 1 calc R . . H51E H 0.2157 0.9258 0.1018 0.076 Uiso 1 1 calc R . . H51F H 0.2878 1.0176 0.1175 0.076 Uiso 1 1 calc R . . C513 C 0.3827(8) 0.9230(8) 0.2005(8) 0.052(4) Uani 1 1 d . . . H51G H 0.4224 0.9173 0.2514 0.078 Uiso 1 1 calc R . . H51H H 0.4142 0.9705 0.1719 0.078 Uiso 1 1 calc R . . H51I H 0.3707 0.8676 0.1665 0.078 Uiso 1 1 calc R . . F321 F 0.6821(4) 0.0514(4) 0.2458(4) 0.0385(17) Uani 1 1 d . . . F331 F 0.5416(5) 0.1294(5) 0.1933(4) 0.054(2) Uani 1 1 d . . . F341 F 0.5684(5) 0.3039(5) 0.1758(4) 0.060(2) Uani 1 1 d . . . F351 F 0.7423(5) 0.4020(4) 0.2189(4) 0.059(2) Uani 1 1 d . . . F361 F 0.8830(5) 0.3285(4) 0.2726(4) 0.0404(18) Uani 1 1 d . . . F421 F 0.8973(5) 0.2589(4) 0.4282(4) 0.0438(18) Uani 1 1 d . . . F431 F 1.0525(5) 0.3555(4) 0.5082(4) 0.061(2) Uani 1 1 d . . . F441 F 1.2208(5) 0.3462(5) 0.4625(4) 0.062(2) Uani 1 1 d . . . F451 F 1.2272(5) 0.2336(4) 0.3330(4) 0.0466(19) Uani 1 1 d . . . F461 F 1.0725(4) 0.1348(4) 0.2528(4) 0.0344(16) Uani 1 1 d . . . F621 F 0.9409(4) 0.2092(4) 0.1561(4) 0.0362(17) Uani 1 1 d . . . F631 F 0.9495(4) 0.1313(4) 0.0126(4) 0.0402(17) Uani 1 1 d . . . F641 F 0.8949(5) -0.0469(4) -0.0169(4) 0.0445(18) Uani 1 1 d . . . F651 F 0.8313(5) -0.1420(4) 0.1006(4) 0.0474(19) Uani 1 1 d . . . F661 F 0.8168(4) -0.0675(3) 0.2415(4) 0.0339(16) Uani 1 1 d . . . F721 F 0.9728(4) -0.0040(3) 0.3512(4) 0.0343(16) Uani 1 1 d . . . F731 F 0.9405(5) -0.1096(4) 0.4691(4) 0.053(2) Uani 1 1 d . . . F741 F 0.8040(6) -0.0893(5) 0.5585(5) 0.081(3) Uani 1 1 d . . . F751 F 0.7043(5) 0.0354(5) 0.5269(5) 0.078(3) Uani 1 1 d . . . F761 F 0.7278(4) 0.1363(4) 0.4067(4) 0.0452(19) Uani 1 1 d . . . C31 C 0.7912(8) 0.1857(7) 0.2638(7) 0.029(3) Uani 1 1 d . . . C32 C 0.7023(8) 0.1412(7) 0.2416(6) 0.026(3) Uani 1 1 d . . . C33 C 0.6279(8) 0.1808(8) 0.2111(7) 0.036(3) Uani 1 1 d . . . C34 C 0.6433(8) 0.2670(8) 0.2043(7) 0.036(3) Uani 1 1 d . . . C35 C 0.7281(10) 0.3139(8) 0.2251(8) 0.042(3) Uani 1 1 d . . . C36 C 0.7984(9) 0.2759(7) 0.2534(7) 0.035(3) Uani 1 1 d . . . C41 C 0.9724(8) 0.1932(7) 0.3345(7) 0.028(3) Uani 1 1 d . . . C42 C 0.9778(9) 0.2524(7) 0.4011(7) 0.036(3) Uani 1 1 d . . . C43 C 1.0546(10) 0.3005(8) 0.4451(8) 0.041(3) Uani 1 1 d . . . C44 C 1.1386(10) 0.2970(8) 0.4203(8) 0.046(4) Uani 1 1 d . . . C45 C 1.1426(9) 0.2400(8) 0.3582(8) 0.039(3) Uani 1 1 d . . . C46 C 1.0606(9) 0.1913(7) 0.3148(7) 0.033(3) Uani 1 1 d . . . C61 C 0.8802(7) 0.0753(7) 0.2075(7) 0.025(3) Uani 1 1 d . . . C62 C 0.9129(7) 0.1200(7) 0.1455(7) 0.029(3) Uani 1 1 d . . . C63 C 0.9173(8) 0.0826(8) 0.0709(8) 0.036(3) Uani 1 1 d . . . C64 C 0.8902(7) -0.0082(8) 0.0547(7) 0.030(3) Uani 1 1 d . . . C65 C 0.8556(8) -0.0545(7) 0.1137(8) 0.031(3) Uani 1 1 d . . . C66 C 0.8515(7) -0.0147(7) 0.1870(7) 0.031(3) Uani 1 1 d . . . C71 C 0.8491(7) 0.0682(7) 0.3685(7) 0.028(3) Uani 1 1 d . . . C72 C 0.9021(8) 0.0048(7) 0.3920(7) 0.033(3) Uani 1 1 d . . . C73 C 0.8876(9) -0.0478(7) 0.4522(7) 0.036(3) Uani 1 1 d . . . C74 C 0.8189(9) -0.0392(8) 0.4964(8) 0.049(4) Uani 1 1 d . . . C75 C 0.7673(9) 0.0222(9) 0.4815(9) 0.053(4) Uani 1 1 d . . . C76 C 0.7839(8) 0.0729(8) 0.4186(8) 0.042(3) Uani 1 1 d . . . B1 B 0.8733(9) 0.1315(7) 0.2922(7) 0.0291(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0332(9) 0.0297(8) 0.0159(8) 0.0058(6) 0.0021(7) 0.0182(7) N1 0.041(6) 0.034(5) 0.015(5) 0.006(4) 0.000(5) 0.027(5) N2 0.064(8) 0.037(6) 0.032(7) 0.010(5) 0.008(6) 0.030(6) N3 0.056(7) 0.038(6) 0.020(6) 0.017(5) 0.011(5) 0.027(6) N4 0.036(7) 0.043(6) 0.049(7) 0.008(5) 0.012(6) 0.021(6) N5 0.049(7) 0.034(6) 0.036(7) 0.011(5) 0.006(5) 0.027(6) C1 0.035(8) 0.028(7) 0.018(7) 0.002(5) 0.000(6) 0.014(6) C2 0.040(8) 0.035(7) 0.021(7) 0.001(5) -0.003(6) 0.033(6) C3 0.046(8) 0.025(7) 0.051(9) 0.028(6) 0.020(7) 0.005(6) C4 0.096(13) 0.030(8) 0.048(10) 0.015(7) 0.034(10) 0.045(9) C5 0.096(13) 0.030(8) 0.048(10) 0.015(7) 0.034(10) 0.045(9) C6 0.035(9) 0.067(10) 0.061(10) 0.016(8) 0.020(7) 0.031(8) C7 0.036(8) 0.062(9) 0.041(9) 0.011(7) 0.010(7) 0.035(7) C11 0.031(7) 0.026(6) 0.023(7) 0.002(5) -0.004(5) 0.019(6) C12 0.042(8) 0.030(6) 0.012(6) 0.003(5) 0.007(5) 0.018(6) C13 0.047(8) 0.033(6) 0.015(6) 0.006(5) -0.004(6) 0.016(6) C14 0.047(8) 0.033(6) 0.015(6) 0.006(5) -0.004(6) 0.016(6) C15 0.026(6) 0.023(6) 0.017(6) 0.000(5) -0.002(5) 0.019(5) C16 0.026(7) 0.021(6) 0.018(6) 0.006(5) 0.003(5) 0.008(5) C21 0.131(15) 0.062(9) 0.023(8) 0.011(7) 0.008(9) 0.047(10) C40 0.131(15) 0.062(9) 0.023(8) 0.011(7) 0.008(9) 0.047(10) C50 0.131(15) 0.062(9) 0.023(8) 0.011(7) 0.008(9) 0.047(10) C51 0.055(9) 0.039(7) 0.025(7) 0.001(6) 0.007(6) 0.029(7) C60 0.033(9) 0.127(13) 0.105(14) 0.056(11) 0.033(9) 0.055(10) C70 0.075(11) 0.094(11) 0.082(12) 0.048(10) 0.027(9) 0.071(10) C121 0.042(8) 0.014(6) 0.016(6) 0.009(5) -0.006(5) 0.010(6) C122 0.042(8) 0.014(6) 0.016(6) 0.009(5) -0.006(5) 0.010(6) C123 0.029(7) 0.033(7) 0.025(7) 0.009(5) 0.012(6) 0.009(6) C124 0.037(8) 0.046(8) 0.020(7) 0.012(6) -0.003(6) 0.023(7) C125 0.032(7) 0.023(6) 0.024(7) 0.002(5) 0.003(6) 0.002(6) C126 0.024(7) 0.027(6) 0.011(6) 0.007(5) 0.001(5) 0.005(5) C127 0.033(7) 0.025(6) 0.028(7) 0.015(5) -0.001(6) 0.016(6) C128 0.045(9) 0.060(8) 0.044(9) 0.011(7) 0.005(7) 0.029(7) C129 0.042(8) 0.055(8) 0.039(9) 0.004(7) -0.001(7) 0.017(7) C130 0.044(8) 0.048(8) 0.019(7) -0.006(6) -0.012(6) 0.032(7) C131 0.042(8) 0.040(7) 0.043(9) 0.028(6) 0.001(7) 0.012(7) C132 0.058(9) 0.026(7) 0.062(10) 0.008(7) 0.015(8) -0.005(7) C161 0.027(7) 0.012(5) 0.015(6) 0.006(5) -0.002(5) 0.010(5) C162 0.027(7) 0.012(5) 0.015(6) 0.006(5) -0.002(5) 0.010(5) C163 0.041(8) 0.040(7) 0.019(7) 0.011(6) 0.006(6) 0.015(6) C164 0.060(10) 0.053(8) 0.024(8) 0.013(7) 0.008(7) 0.025(8) C165 0.039(8) 0.052(8) 0.013(7) 0.018(6) -0.002(6) 0.023(7) C166 0.028(7) 0.020(6) 0.022(7) -0.001(5) 0.003(5) 0.017(5) C167 0.047(8) 0.039(7) 0.032(8) 0.014(6) 0.012(7) 0.022(7) C168 0.035(8) 0.065(9) 0.030(8) 0.007(7) 0.004(6) 0.018(7) C169 0.050(9) 0.036(7) 0.040(8) 0.009(6) 0.015(7) 0.007(7) C170 0.046(8) 0.056(8) 0.019(7) 0.007(6) -0.011(6) 0.021(7) C171 0.111(14) 0.020(7) 0.096(14) 0.005(8) 0.004(11) -0.020(9) C172 0.054(9) 0.076(10) 0.052(10) 0.037(8) 0.027(8) 0.017(8) C211 0.130(18) 0.138(17) 0.14(2) -0.084(15) 0.008(15) 0.051(15) C212 0.130(18) 0.138(17) 0.14(2) -0.084(15) 0.008(15) 0.051(15) C213 0.095(15) 0.141(18) 0.19(2) 0.021(17) -0.041(15) 0.076(14) C511 0.121(14) 0.031(7) 0.048(10) -0.013(7) 0.011(9) 0.030(9) C512 0.062(9) 0.068(9) 0.040(9) 0.027(7) 0.019(7) 0.045(8) C513 0.055(9) 0.061(9) 0.041(9) 0.003(7) 0.005(7) 0.015(8) F321 0.037(4) 0.042(4) 0.038(4) 0.011(3) -0.005(3) 0.018(3) F331 0.048(5) 0.080(5) 0.040(5) 0.010(4) -0.002(4) 0.037(5) F341 0.082(6) 0.081(5) 0.035(5) 0.026(4) 0.012(4) 0.056(5) F351 0.092(6) 0.049(4) 0.052(5) 0.030(4) 0.023(5) 0.043(4) F361 0.057(5) 0.023(4) 0.047(5) 0.015(3) 0.015(4) 0.016(4) F421 0.055(5) 0.046(4) 0.037(4) -0.004(3) 0.015(4) 0.021(4) F431 0.092(6) 0.055(4) 0.031(5) -0.014(4) 0.010(4) 0.005(5) F441 0.071(6) 0.067(5) 0.036(5) 0.005(4) 0.000(4) -0.009(5) F451 0.035(4) 0.047(4) 0.052(5) 0.016(4) 0.000(4) -0.005(4) F461 0.030(4) 0.036(4) 0.037(4) 0.004(3) 0.002(3) 0.011(3) F621 0.049(4) 0.032(4) 0.031(4) 0.015(3) 0.008(3) 0.012(3) F631 0.047(4) 0.054(4) 0.025(4) 0.011(3) 0.007(3) 0.021(4) F641 0.056(5) 0.056(4) 0.027(4) -0.005(3) -0.007(4) 0.035(4) F651 0.052(5) 0.028(4) 0.058(5) -0.010(3) -0.010(4) 0.014(4) F661 0.044(4) 0.024(3) 0.031(4) 0.006(3) -0.010(3) 0.010(3) F721 0.046(4) 0.031(4) 0.031(4) 0.017(3) -0.002(3) 0.023(3) F731 0.063(5) 0.045(4) 0.055(5) 0.028(4) 0.000(4) 0.023(4) F741 0.088(6) 0.091(6) 0.086(7) 0.079(5) 0.036(5) 0.039(5) F751 0.062(6) 0.135(7) 0.060(6) 0.075(5) 0.033(5) 0.047(6) F761 0.044(4) 0.060(4) 0.042(5) 0.024(4) 0.016(4) 0.026(4) C31 0.030(7) 0.036(7) 0.026(7) 0.013(6) 0.011(6) 0.012(6) C32 0.025(7) 0.033(7) 0.025(7) 0.006(5) 0.001(5) 0.023(6) C33 0.028(8) 0.054(9) 0.027(7) 0.012(6) -0.007(6) 0.019(7) C34 0.028(8) 0.054(9) 0.027(7) 0.012(6) -0.007(6) 0.019(7) C35 0.056(10) 0.033(8) 0.042(9) 0.016(6) -0.001(7) 0.025(8) C36 0.058(9) 0.022(7) 0.024(7) 0.012(5) -0.002(7) 0.008(7) C41 0.029(7) 0.041(7) 0.019(7) 0.018(6) 0.004(6) 0.015(6) C42 0.039(8) 0.037(7) 0.026(8) 0.001(6) -0.001(6) -0.005(7) C43 0.050(9) 0.033(7) 0.032(8) -0.003(6) 0.005(7) -0.013(7) C44 0.049(10) 0.040(8) 0.031(8) 0.009(7) -0.012(7) -0.027(7) C45 0.038(9) 0.030(7) 0.045(9) 0.016(7) 0.001(7) 0.000(7) C46 0.051(9) 0.016(6) 0.030(8) 0.008(5) -0.003(7) 0.011(6) C61 0.016(6) 0.028(6) 0.037(8) 0.018(6) 0.004(5) 0.014(5) C62 0.025(7) 0.034(7) 0.034(8) 0.011(6) 0.013(6) 0.015(6) C63 0.026(7) 0.044(8) 0.043(9) 0.013(7) 0.007(6) 0.015(7) C64 0.022(7) 0.045(8) 0.026(7) 0.005(6) -0.008(6) 0.019(6) C65 0.028(7) 0.024(7) 0.041(8) 0.002(6) -0.009(6) 0.017(6) C66 0.028(7) 0.024(7) 0.041(8) 0.002(6) -0.009(6) 0.017(6) C71 0.025(7) 0.031(6) 0.028(7) 0.007(5) -0.004(6) 0.011(6) C72 0.034(8) 0.037(7) 0.032(8) 0.005(6) 0.004(6) 0.022(6) C73 0.044(8) 0.044(8) 0.022(7) 0.022(6) -0.006(6) 0.017(7) C74 0.059(10) 0.047(8) 0.045(9) 0.042(7) 0.008(8) 0.010(8) C75 0.041(9) 0.069(9) 0.070(11) 0.052(8) 0.028(8) 0.038(8) C76 0.041(8) 0.053(8) 0.045(9) 0.016(7) 0.014(7) 0.034(7) B1 0.025(3) 0.034(4) 0.035(4) 0.015(3) 0.018(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.725(8) . ? Ni1 C1 1.882(11) . ? Ni1 C2 1.914(10) . ? N1 C11 1.297(12) . ? N2 C1 1.356(14) . ? N2 C4 1.371(14) . ? N2 C21 1.494(16) . ? N3 C1 1.321(13) . ? N3 C5 1.407(15) . ? N3 C3 1.442(14) . ? N4 C2 1.378(13) . ? N4 C6 1.383(13) . ? N4 C3 1.475(12) . ? N5 C2 1.331(11) . ? N5 C7 1.391(14) . ? N5 C51 1.485(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.404(19) . ? C4 C40 1.472(14) . ? C5 C50 1.543(14) . ? C6 C7 1.338(16) . ? C6 C60 1.482(16) . ? C7 C70 1.518(15) . ? C11 C16 1.436(13) . ? C11 C12 1.446(14) . ? C12 C13 1.334(13) . ? C12 C121 1.493(13) . ? C13 C14 1.416(13) . ? C13 H13A 0.9500 . ? C14 C14 1.385(13) 2_665 ? C14 C15 1.420(13) . ? C15 C16 1.359(13) . ? C15 H15A 0.9500 . ? C16 C161 1.545(14) . ? C21 C213 1.487(18) . ? C21 C212 1.541(14) . ? C21 C211 1.550(17) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C511 1.509(15) . ? C51 C513 1.516(15) . ? C51 C512 1.541(15) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C121 C126 1.353(13) . ? C121 C122 1.381(14) . ? C122 C123 1.391(13) . ? C122 C130 1.544(14) . ? C123 C124 1.374(13) . ? C123 H12B 0.9500 . ? C124 C125 1.382(14) . ? C124 H12C 0.9500 . ? C125 C126 1.414(13) . ? C125 H12A 0.9500 . ? C126 C127 1.502(14) . ? C127 C129 1.515(14) . ? C127 C128 1.524(14) . ? C127 H12D 1.0000 . ? C128 H12E 0.9800 . ? C128 H12F 0.9800 . ? C128 H12G 0.9800 . ? C129 H12H 0.9800 . ? C129 H12I 0.9800 . ? C129 H12J 0.9800 . ? C130 C131 1.521(14) . ? C130 C132 1.543(15) . ? C130 H13B 1.0000 . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C132 H13F 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C161 C162 1.350(14) . ? C161 C166 1.431(13) . ? C162 C163 1.366(13) . ? C162 C170 1.533(14) . ? C163 C164 1.371(14) . ? C163 H16B 0.9500 . ? C164 C165 1.350(15) . ? C164 H16G 0.9500 . ? C165 C166 1.378(14) . ? C165 H16C 0.9500 . ? C166 C167 1.495(15) . ? C167 C169 1.514(14) . ? C167 C168 1.595(14) . ? C167 H16A 1.0000 . ? C168 H16H 0.9800 . ? C168 H16I 0.9800 . ? C168 H16J 0.9800 . ? C169 H16D 0.9800 . ? C169 H16E 0.9800 . ? C169 H16F 0.9800 . ? C170 C172 1.520(15) . ? C170 C171 1.520(15) . ? C170 H17A 1.0000 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C171 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C172 H17G 0.9800 . ? C211 H21G 0.9800 . ? C211 H21H 0.9800 . ? C211 H21I 0.9800 . ? C212 H21A 0.9800 . ? C212 H21B 0.9800 . ? C212 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C213 H21F 0.9800 . ? C511 H51A 0.9800 . ? C511 H51B 0.9800 . ? C511 H51C 0.9800 . ? C512 H51D 0.9800 . ? C512 H51E 0.9800 . ? C512 H51F 0.9800 . ? C513 H51G 0.9800 . ? C513 H51H 0.9800 . ? C513 H51I 0.9800 . ? F321 C32 1.377(11) . ? F331 C33 1.360(12) . ? F341 C34 1.372(12) . ? F351 C35 1.354(12) . ? F361 C36 1.348(13) . ? F421 C42 1.352(12) . ? F431 C43 1.332(13) . ? F441 C44 1.386(13) . ? F451 C45 1.394(13) . ? F461 C46 1.376(12) . ? F621 C62 1.365(11) . ? F631 C63 1.351(12) . ? F641 C64 1.330(12) . ? F651 C65 1.337(11) . ? F661 C66 1.349(11) . ? F721 C72 1.350(11) . ? F731 C73 1.359(12) . ? F741 C74 1.347(12) . ? F751 C75 1.319(13) . ? F761 C76 1.402(11) . ? C31 C32 1.357(14) . ? C31 C36 1.403(14) . ? C31 B1 1.629(13) . ? C32 C33 1.400(14) . ? C33 C34 1.328(14) . ? C34 C35 1.318(14) . ? C35 C36 1.327(15) . ? C41 C42 1.392(15) . ? C41 C46 1.395(15) . ? C41 B1 1.638(13) . ? C42 C43 1.336(15) . ? C43 C44 1.373(17) . ? C44 C45 1.345(16) . ? C45 C46 1.388(16) . ? C61 C62 1.372(13) . ? C61 C66 1.392(13) . ? C61 B1 1.652(13) . ? C62 C63 1.365(15) . ? C63 C64 1.394(15) . ? C64 C65 1.352(14) . ? C65 C66 1.360(14) . ? C71 C76 1.373(14) . ? C71 C72 1.402(13) . ? C71 B1 1.687(13) . ? C72 C73 1.344(14) . ? C73 C74 1.360(16) . ? C74 C75 1.336(15) . ? C75 C76 1.367(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 C1 132.9(4) . . ? N1 Ni1 C2 132.4(4) . . ? C1 Ni1 C2 88.6(5) . . ? C11 N1 Ni1 163.7(9) . . ? C1 N2 C4 114.6(12) . . ? C1 N2 C21 122.3(10) . . ? C4 N2 C21 123.0(12) . . ? C1 N3 C5 111.0(11) . . ? C1 N3 C3 121.6(9) . . ? C5 N3 C3 127.3(12) . . ? C2 N4 C6 111.9(9) . . ? C2 N4 C3 119.5(9) . . ? C6 N4 C3 128.5(11) . . ? C2 N5 C7 108.2(10) . . ? C2 N5 C51 125.4(10) . . ? C7 N5 C51 126.3(9) . . ? N3 C1 N2 104.7(10) . . ? N3 C1 Ni1 115.7(8) . . ? N2 C1 Ni1 139.5(10) . . ? N5 C2 N4 105.4(9) . . ? N5 C2 Ni1 139.9(10) . . ? N4 C2 Ni1 114.7(7) . . ? N3 C3 N4 108.0(9) . . ? N3 C3 H3A 110.1 . . ? N4 C3 H3A 110.1 . . ? N3 C3 H3B 110.1 . . ? N4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N2 C4 C5 102.7(12) . . ? N2 C4 C40 135.1(16) . . ? C5 C4 C40 122.1(14) . . ? C4 C5 N3 107.1(12) . . ? C4 C5 C50 132.0(12) . . ? N3 C5 C50 120.9(12) . . ? C7 C6 N4 103.3(11) . . ? C7 C6 C60 136.0(12) . . ? N4 C6 C60 120.6(11) . . ? C6 C7 N5 111.0(11) . . ? C6 C7 C70 125.3(12) . . ? N5 C7 C70 123.6(12) . . ? N1 C11 C16 120.9(10) . . ? N1 C11 C12 120.3(9) . . ? C16 C11 C12 118.7(9) . . ? C13 C12 C11 117.6(10) . . ? C13 C12 C121 121.1(10) . . ? C11 C12 C121 121.2(9) . . ? C12 C13 C14 126.3(9) . . ? C12 C13 H13A 116.9 . . ? C14 C13 H13A 116.9 . . ? C14 C14 C13 122.1(10) 2_665 . ? C14 C14 C15 123.4(9) 2_665 . ? C13 C14 C15 114.4(9) . . ? C16 C15 C14 123.3(9) . . ? C16 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? C15 C16 C11 119.4(10) . . ? C15 C16 C161 117.9(9) . . ? C11 C16 C161 122.6(9) . . ? C213 C21 N2 109.6(12) . . ? C213 C21 C212 108.5(12) . . ? N2 C21 C212 110.7(11) . . ? C213 C21 C211 110.2(14) . . ? N2 C21 C211 110.7(12) . . ? C212 C21 C211 107.2(12) . . ? C4 C40 H40A 109.5 . . ? C4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C5 C50 H50A 109.5 . . ? C5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N5 C51 C511 110.0(9) . . ? N5 C51 C513 109.0(9) . . ? C511 C51 C513 108.7(11) . . ? N5 C51 C512 110.9(10) . . ? C511 C51 C512 110.6(10) . . ? C513 C51 C512 107.6(9) . . ? C6 C60 H60A 109.5 . . ? C6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C7 C70 H70A 109.5 . . ? C7 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C7 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C126 C121 C122 122.6(9) . . ? C126 C121 C12 117.5(9) . . ? C122 C121 C12 119.5(10) . . ? C121 C122 C123 119.5(10) . . ? C121 C122 C130 122.7(9) . . ? C123 C122 C130 117.7(10) . . ? C124 C123 C122 119.5(11) . . ? C124 C123 H12B 120.2 . . ? C122 C123 H12B 120.2 . . ? C123 C124 C125 120.0(10) . . ? C123 C124 H12C 120.0 . . ? C125 C124 H12C 120.0 . . ? C124 C125 C126 120.8(10) . . ? C124 C125 H12A 119.6 . . ? C126 C125 H12A 119.6 . . ? C121 C126 C125 117.5(9) . . ? C121 C126 C127 124.6(9) . . ? C125 C126 C127 117.7(9) . . ? C126 C127 C129 111.8(9) . . ? C126 C127 C128 114.3(9) . . ? C129 C127 C128 111.3(10) . . ? C126 C127 H12D 106.3 . . ? C129 C127 H12D 106.3 . . ? C128 C127 H12D 106.3 . . ? C127 C128 H12E 109.5 . . ? C127 C128 H12F 109.5 . . ? H12E C128 H12F 109.5 . . ? C127 C128 H12G 109.5 . . ? H12E C128 H12G 109.5 . . ? H12F C128 H12G 109.5 . . ? C127 C129 H12H 109.5 . . ? C127 C129 H12I 109.5 . . ? H12H C129 H12I 109.5 . . ? C127 C129 H12J 109.5 . . ? H12H C129 H12J 109.5 . . ? H12I C129 H12J 109.5 . . ? C131 C130 C132 112.4(10) . . ? C131 C130 C122 112.1(9) . . ? C132 C130 C122 112.0(9) . . ? C131 C130 H13B 106.6 . . ? C132 C130 H13B 106.6 . . ? C122 C130 H13B 106.6 . . ? C130 C131 H13C 109.5 . . ? C130 C131 H13D 109.5 . . ? H13C C131 H13D 109.5 . . ? C130 C131 H13E 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? C130 C132 H13F 109.5 . . ? C130 C132 H13G 109.5 . . ? H13F C132 H13G 109.5 . . ? C130 C132 H13H 109.5 . . ? H13F C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? C162 C161 C166 121.4(10) . . ? C162 C161 C16 121.9(9) . . ? C166 C161 C16 116.6(10) . . ? C161 C162 C163 120.5(10) . . ? C161 C162 C170 123.0(9) . . ? C163 C162 C170 116.5(10) . . ? C162 C163 C164 118.1(11) . . ? C162 C163 H16B 120.9 . . ? C164 C163 H16B 120.9 . . ? C165 C164 C163 123.2(12) . . ? C165 C164 H16G 118.4 . . ? C163 C164 H16G 118.4 . . ? C164 C165 C166 119.9(11) . . ? C164 C165 H16C 120.0 . . ? C166 C165 H16C 120.0 . . ? C165 C166 C161 116.8(10) . . ? C165 C166 C167 120.1(10) . . ? C161 C166 C167 123.1(10) . . ? C166 C167 C169 115.0(10) . . ? C166 C167 C168 110.1(9) . . ? C169 C167 C168 108.8(9) . . ? C166 C167 H16A 107.5 . . ? C169 C167 H16A 107.5 . . ? C168 C167 H16A 107.5 . . ? C167 C168 H16H 109.5 . . ? C167 C168 H16I 109.5 . . ? H16H C168 H16I 109.5 . . ? C167 C168 H16J 109.5 . . ? H16H C168 H16J 109.5 . . ? H16I C168 H16J 109.5 . . ? C167 C169 H16D 109.5 . . ? C167 C169 H16E 109.5 . . ? H16D C169 H16E 109.5 . . ? C167 C169 H16F 109.5 . . ? H16D C169 H16F 109.5 . . ? H16E C169 H16F 109.5 . . ? C172 C170 C171 113.0(11) . . ? C172 C170 C162 109.8(9) . . ? C171 C170 C162 113.7(10) . . ? C172 C170 H17A 106.6 . . ? C171 C170 H17A 106.6 . . ? C162 C170 H17A 106.6 . . ? C170 C171 H17B 109.5 . . ? C170 C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C170 C171 H17D 109.5 . . ? H17B C171 H17D 109.5 . . ? H17C C171 H17D 109.5 . . ? C170 C172 H17E 109.5 . . ? C170 C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C170 C172 H17G 109.5 . . ? H17E C172 H17G 109.5 . . ? H17F C172 H17G 109.5 . . ? C21 C211 H21G 109.5 . . ? C21 C211 H21H 109.5 . . ? H21G C211 H21H 109.5 . . ? C21 C211 H21I 109.5 . . ? H21G C211 H21I 109.5 . . ? H21H C211 H21I 109.5 . . ? C21 C212 H21A 109.5 . . ? C21 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C21 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C21 C213 H21D 109.5 . . ? C21 C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C21 C213 H21F 109.5 . . ? H21D C213 H21F 109.5 . . ? H21E C213 H21F 109.5 . . ? C51 C511 H51A 109.5 . . ? C51 C511 H51B 109.5 . . ? H51A C511 H51B 109.5 . . ? C51 C511 H51C 109.5 . . ? H51A C511 H51C 109.5 . . ? H51B C511 H51C 109.5 . . ? C51 C512 H51D 109.5 . . ? C51 C512 H51E 109.5 . . ? H51D C512 H51E 109.5 . . ? C51 C512 H51F 109.5 . . ? H51D C512 H51F 109.5 . . ? H51E C512 H51F 109.5 . . ? C51 C513 H51G 109.5 . . ? C51 C513 H51H 109.5 . . ? H51G C513 H51H 109.5 . . ? C51 C513 H51I 109.5 . . ? H51G C513 H51I 109.5 . . ? H51H C513 H51I 109.5 . . ? C32 C31 C36 111.5(10) . . ? C32 C31 B1 119.4(9) . . ? C36 C31 B1 129.0(9) . . ? C31 C32 F321 119.8(9) . . ? C31 C32 C33 123.8(10) . . ? F321 C32 C33 116.3(10) . . ? C34 C33 F331 122.5(10) . . ? C34 C33 C32 119.2(10) . . ? F331 C33 C32 118.1(10) . . ? C35 C34 C33 119.8(10) . . ? C35 C34 F341 122.5(10) . . ? C33 C34 F341 117.7(10) . . ? C34 C35 C36 120.7(10) . . ? C34 C35 F351 119.1(10) . . ? C36 C35 F351 120.2(13) . . ? C35 C36 F361 116.9(10) . . ? C35 C36 C31 125.0(13) . . ? F361 C36 C31 118.2(11) . . ? C42 C41 C46 111.0(11) . . ? C42 C41 B1 121.7(10) . . ? C46 C41 B1 127.2(10) . . ? C43 C42 F421 115.2(11) . . ? C43 C42 C41 127.5(12) . . ? F421 C42 C41 117.2(10) . . ? F431 C43 C42 122.9(13) . . ? F431 C43 C44 119.0(12) . . ? C42 C43 C44 117.9(12) . . ? C45 C44 C43 119.9(12) . . ? C45 C44 F441 118.9(13) . . ? C43 C44 F441 120.9(12) . . ? C44 C45 C46 119.5(13) . . ? C44 C45 F451 121.2(12) . . ? C46 C45 F451 119.2(12) . . ? F461 C46 C45 114.8(11) . . ? F461 C46 C41 121.1(11) . . ? C45 C46 C41 123.9(11) . . ? C62 C61 C66 112.6(10) . . ? C62 C61 B1 119.0(9) . . ? C66 C61 B1 128.3(9) . . ? C63 C62 F621 115.7(10) . . ? C63 C62 C61 125.1(11) . . ? F621 C62 C61 119.1(10) . . ? F631 C63 C62 121.6(10) . . ? F631 C63 C64 118.8(11) . . ? C62 C63 C64 119.6(11) . . ? F641 C64 C65 121.8(11) . . ? F641 C64 C63 121.1(11) . . ? C65 C64 C63 117.1(11) . . ? F651 C65 C64 118.3(11) . . ? F651 C65 C66 120.0(11) . . ? C64 C65 C66 121.5(10) . . ? F661 C66 C65 116.3(10) . . ? F661 C66 C61 119.7(10) . . ? C65 C66 C61 124.0(10) . . ? C76 C71 C72 110.8(10) . . ? C76 C71 B1 128.1(10) . . ? C72 C71 B1 120.9(9) . . ? C73 C72 F721 117.7(10) . . ? C73 C72 C71 124.5(11) . . ? F721 C72 C71 117.8(10) . . ? C72 C73 F731 120.6(11) . . ? C72 C73 C74 119.6(11) . . ? F731 C73 C74 119.8(10) . . ? C75 C74 F741 118.3(12) . . ? C75 C74 C73 120.6(11) . . ? F741 C74 C73 121.1(11) . . ? F751 C75 C74 121.6(11) . . ? F751 C75 C76 121.0(11) . . ? C74 C75 C76 117.4(12) . . ? C75 C76 C71 127.0(11) . . ? C75 C76 F761 114.4(10) . . ? C71 C76 F761 118.6(10) . . ? C31 B1 C41 114.5(8) . . ? C31 B1 C61 102.7(9) . . ? C41 B1 C61 113.7(9) . . ? C31 B1 C71 112.2(9) . . ? C41 B1 C71 100.3(8) . . ? C61 B1 C71 114.1(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.517 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 901781' ####################################################################### # # 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_(TMTBM)Ni(cod) #TrackingRef 'Bent imido complete cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H44 N4 Ni' _chemical_formula_weight 483.37 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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 17.8294(19) _cell_length_b 42.047(5) _cell_length_c 17.6823(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13256(3) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20306 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3487 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.9568 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details 'Norton et. al' _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 P4' _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 20306 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7756 _reflns_number_gt 7159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1243P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.967(16) _refine_ls_number_reflns 7756 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.022 _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 Ni1 Ni 0.229101(17) 0.993390(8) 0.59949(2) 0.02136(11) Uani 1 1 d . . . N1 N 0.35897(14) 0.96533(6) 0.69535(13) 0.0238(5) Uani 1 1 d . . . N2 N 0.37347(13) 0.97228(6) 0.57587(12) 0.0236(5) Uani 1 1 d . . . N3 N 0.28816(13) 0.96316(6) 0.47373(13) 0.0227(5) Uani 1 1 d . . . N4 N 0.17695(14) 0.94447(6) 0.47846(13) 0.0251(5) Uani 1 1 d . . . C1 C 0.32152(17) 0.97538(7) 0.63178(16) 0.0244(6) Uani 1 1 d . . . C2 C 0.22233(16) 0.96543(7) 0.51423(16) 0.0242(6) Uani 1 1 d . . . C3 C 0.28334(17) 0.94204(8) 0.41345(16) 0.0272(6) Uani 1 1 d . . . C4 C 0.21251(18) 0.93025(8) 0.41557(17) 0.0289(6) Uani 1 1 d . . . C5 C 0.43497(17) 0.95779(7) 0.67850(16) 0.0271(6) Uani 1 1 d . . . C6 C 0.44254(16) 0.96164(7) 0.60216(18) 0.0274(6) Uani 1 1 d . . . C11 C 0.32171(19) 0.96332(8) 0.77108(16) 0.0288(6) Uani 1 1 d . . . C30 C 0.34637(19) 0.93607(9) 0.36085(18) 0.0354(7) Uani 1 1 d . . . H30A H 0.3310 0.9205 0.3227 0.053 Uiso 1 1 calc R . . H30B H 0.3894 0.9278 0.3892 0.053 Uiso 1 1 calc R . . H30C H 0.3605 0.9560 0.3359 0.053 Uiso 1 1 calc R . . C32 C 0.35407(16) 0.98069(8) 0.49803(15) 0.0243(6) Uani 1 1 d . . . H32A H 0.3441 1.0038 0.4947 0.029 Uiso 1 1 calc R . . H32B H 0.3967 0.9757 0.4642 0.029 Uiso 1 1 calc R . . C40 C 0.1789(2) 0.90843(10) 0.3581(2) 0.0460(9) Uani 1 1 d . . . H40A H 0.2171 0.9025 0.3209 0.069 Uiso 1 1 calc R . . H40B H 0.1374 0.9193 0.3323 0.069 Uiso 1 1 calc R . . H40C H 0.1600 0.8893 0.3832 0.069 Uiso 1 1 calc R . . C41 C 0.09792(18) 0.93832(8) 0.50504(18) 0.0313(6) Uani 1 1 d . . . C50 C 0.4952(2) 0.94931(10) 0.7331(2) 0.0386(8) Uani 1 1 d . . . H50A H 0.5418 0.9451 0.7056 0.058 Uiso 1 1 calc R . . H50B H 0.4805 0.9302 0.7613 0.058 Uiso 1 1 calc R . . H50C H 0.5029 0.9670 0.7684 0.058 Uiso 1 1 calc R . . C51 C 0.21830(18) 1.03474(8) 0.64821(16) 0.0273(6) Uani 1 1 d . . . H51A H 0.1961 1.0335 0.7000 0.033 Uiso 1 1 calc R . . C52 C 0.2849(2) 1.05677(8) 0.64333(19) 0.0335(7) Uani 1 1 d . . . H52A H 0.3110 1.0530 0.5948 0.040 Uiso 1 1 calc R . . H52B H 0.3203 1.0514 0.6846 0.040 Uiso 1 1 calc R . . C53 C 0.2648(2) 1.09273(10) 0.6489(2) 0.0445(9) Uani 1 1 d . . . H53A H 0.2150 1.0948 0.6732 0.053 Uiso 1 1 calc R . . H53B H 0.3019 1.1033 0.6821 0.053 Uiso 1 1 calc R . . C54 C 0.2629(2) 1.10980(9) 0.5747(2) 0.0425(8) Uani 1 1 d . . . H54A H 0.3022 1.1246 0.5659 0.051 Uiso 1 1 calc R . . C55 C 0.2128(2) 1.10662(9) 0.5199(2) 0.0409(8) Uani 1 1 d . . . H55A H 0.2192 1.1193 0.4759 0.049 Uiso 1 1 calc R . . C56 C 0.14632(19) 1.08439(8) 0.52204(19) 0.0353(7) Uani 1 1 d . . . H56A H 0.1118 1.0899 0.4802 0.042 Uiso 1 1 calc R . . H56B H 0.1190 1.0877 0.5701 0.042 Uiso 1 1 calc R . . C57 C 0.16778(17) 1.04863(8) 0.51518(16) 0.0265(6) Uani 1 1 d . . . H57A H 0.1334 1.0383 0.4786 0.032 Uiso 1 1 calc R . . H57B H 0.2192 1.0471 0.4945 0.032 Uiso 1 1 calc R . . C58 C 0.16456(16) 1.03050(7) 0.58924(16) 0.0256(6) Uani 1 1 d . . . H58A H 0.1124 1.0270 0.6082 0.031 Uiso 1 1 calc R . . C60 C 0.50827(18) 0.95502(9) 0.55243(19) 0.0331(7) Uani 1 1 d . . . H60A H 0.5506 0.9478 0.5834 0.050 Uiso 1 1 calc R . . H60B H 0.5223 0.9745 0.5253 0.050 Uiso 1 1 calc R . . H60C H 0.4951 0.9384 0.5159 0.050 Uiso 1 1 calc R . . C111 C 0.2380(2) 0.95981(10) 0.7603(2) 0.0395(8) Uani 1 1 d . . . H11A H 0.2275 0.9401 0.7329 0.059 Uiso 1 1 calc R . . H11B H 0.2188 0.9779 0.7313 0.059 Uiso 1 1 calc R . . H11C H 0.2133 0.9592 0.8098 0.059 Uiso 1 1 calc R . . C112 C 0.3492(2) 0.93404(8) 0.81429(18) 0.0331(7) Uani 1 1 d . . . H11D H 0.3374 0.9148 0.7853 0.050 Uiso 1 1 calc R . . H11E H 0.3242 0.9330 0.8636 0.050 Uiso 1 1 calc R . . H11F H 0.4035 0.9355 0.8217 0.050 Uiso 1 1 calc R . . C113 C 0.3381(2) 0.99412(8) 0.8141(2) 0.0404(8) Uani 1 1 d . . . H11G H 0.3195 1.0123 0.7849 0.061 Uiso 1 1 calc R . . H11H H 0.3923 0.9963 0.8217 0.061 Uiso 1 1 calc R . . H11I H 0.3129 0.9935 0.8634 0.061 Uiso 1 1 calc R . . C411 C 0.0896(4) 0.9473(2) 0.5858(4) 0.122(4) Uani 1 1 d . . . H41A H 0.0381 0.9432 0.6022 0.183 Uiso 1 1 calc R . . H41B H 0.1010 0.9700 0.5919 0.183 Uiso 1 1 calc R . . H41C H 0.1244 0.9348 0.6166 0.183 Uiso 1 1 calc R . . C412 C 0.0746(4) 0.90532(17) 0.4962(6) 0.119(3) Uani 1 1 d . . . H41D H 0.0796 0.8991 0.4430 0.178 Uiso 1 1 calc R . . H41E H 0.0222 0.9031 0.5119 0.178 Uiso 1 1 calc R . . H41F H 0.1064 0.8916 0.5276 0.178 Uiso 1 1 calc R . . C413 C 0.0468(3) 0.9585(4) 0.4598(6) 0.195(7) Uani 1 1 d . . . H41G H 0.0514 0.9529 0.4062 0.292 Uiso 1 1 calc R . . H41H H 0.0602 0.9809 0.4669 0.292 Uiso 1 1 calc R . . H41I H -0.0050 0.9550 0.4765 0.292 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01967(16) 0.02403(18) 0.02039(16) -0.00343(14) -0.00139(13) 0.00188(13) N1 0.0244(12) 0.0257(12) 0.0212(11) 0.0002(9) -0.0018(9) 0.0026(10) N2 0.0203(11) 0.0295(12) 0.0210(11) -0.0011(9) -0.0022(8) 0.0022(10) N3 0.0196(11) 0.0291(13) 0.0193(10) -0.0055(9) 0.0007(9) 0.0004(10) N4 0.0230(12) 0.0275(13) 0.0248(11) -0.0026(9) -0.0022(9) 0.0002(10) C1 0.0243(14) 0.0268(14) 0.0220(12) -0.0047(10) -0.0037(11) 0.0009(12) C2 0.0234(13) 0.0263(14) 0.0230(13) -0.0020(11) -0.0020(10) 0.0009(11) C3 0.0278(15) 0.0291(16) 0.0248(13) -0.0068(11) -0.0030(11) 0.0051(12) C4 0.0320(15) 0.0282(15) 0.0266(14) -0.0067(11) -0.0045(11) 0.0021(13) C5 0.0274(14) 0.0278(15) 0.0261(13) 0.0000(11) -0.0032(11) 0.0056(12) C6 0.0215(12) 0.0300(14) 0.0307(14) 0.0035(13) -0.0002(12) 0.0016(11) C11 0.0376(16) 0.0268(15) 0.0221(13) 0.0003(11) 0.0015(12) 0.0043(13) C30 0.0316(16) 0.0452(19) 0.0293(16) -0.0060(13) -0.0009(12) 0.0062(14) C32 0.0201(13) 0.0284(15) 0.0245(13) 0.0017(11) 0.0011(10) -0.0002(11) C40 0.0409(18) 0.055(2) 0.0425(18) -0.0233(17) 0.0007(15) -0.0045(17) C41 0.0252(15) 0.0328(16) 0.0357(16) -0.0002(13) 0.0001(12) -0.0050(13) C50 0.0344(17) 0.049(2) 0.0327(17) -0.0021(14) -0.0049(13) 0.0050(17) C51 0.0319(15) 0.0270(15) 0.0231(13) -0.0017(11) -0.0014(11) 0.0034(12) C52 0.0341(17) 0.0309(16) 0.0357(16) -0.0047(13) -0.0096(13) 0.0008(13) C53 0.059(2) 0.0343(19) 0.0398(19) -0.0081(15) -0.0076(16) -0.0064(17) C54 0.047(2) 0.0327(18) 0.047(2) -0.0047(14) 0.0042(15) -0.0086(16) C55 0.053(2) 0.0322(17) 0.0378(17) 0.0002(14) 0.0022(15) 0.0065(16) C56 0.0402(18) 0.0353(18) 0.0302(15) -0.0033(13) -0.0021(13) 0.0096(15) C57 0.0246(14) 0.0298(15) 0.0250(13) -0.0027(11) -0.0024(11) 0.0037(12) C58 0.0210(12) 0.0287(14) 0.0272(14) -0.0022(11) 0.0017(11) 0.0040(11) C60 0.0238(14) 0.0407(17) 0.0350(16) 0.0011(13) 0.0016(12) 0.0023(14) C111 0.0332(17) 0.052(2) 0.0327(17) 0.0100(15) 0.0077(13) 0.0073(16) C112 0.0412(18) 0.0296(15) 0.0285(15) 0.0010(12) 0.0013(13) 0.0031(14) C113 0.059(2) 0.0329(18) 0.0295(16) -0.0043(13) 0.0015(15) 0.0046(16) C411 0.075(4) 0.194(8) 0.098(5) -0.089(5) 0.050(3) -0.084(5) C412 0.107(6) 0.056(4) 0.193(9) -0.006(4) 0.079(6) -0.016(4) C413 0.022(2) 0.392(18) 0.171(8) 0.189(10) 0.011(3) 0.019(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 Ni1 C1 1.901(3) . ? Ni1 C2 1.916(3) . ? Ni1 C58 1.947(3) . ? Ni1 C51 1.950(3) . ? N1 C1 1.374(4) . ? N1 C5 1.423(4) . ? N1 C11 1.497(4) . ? N2 C1 1.361(4) . ? N2 C6 1.390(4) . ? N2 C32 1.463(4) . ? N3 C2 1.378(4) . ? N3 C3 1.390(4) . ? N3 C32 1.452(4) . ? N4 C2 1.353(4) . ? N4 C4 1.413(4) . ? N4 C41 1.508(4) . ? C3 C4 1.357(5) . ? C3 C30 1.480(4) . ? C4 C40 1.495(4) . ? C5 C6 1.366(4) . ? C5 C50 1.487(4) . ? C6 C60 1.491(4) . ? C11 C111 1.513(5) . ? C11 C113 1.530(4) . ? C11 C112 1.529(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C412 1.457(7) . ? C41 C413 1.479(8) . ? C41 C411 1.485(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C58 1.427(4) . ? C51 C52 1.509(5) . ? C51 H51A 1.0000 . ? C52 C53 1.557(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.495(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.326(6) . ? C54 H54A 0.9500 . ? C55 C56 1.510(6) . ? C55 H55A 0.9500 . ? C56 C57 1.556(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.516(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C412 H41D 0.9800 . ? C412 H41E 0.9800 . ? C412 H41F 0.9800 . ? C413 H41G 0.9800 . ? C413 H41H 0.9800 . ? C413 H41I 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 C1 Ni1 C2 92.66(12) . . ? C1 Ni1 C58 149.24(13) . . ? C2 Ni1 C58 112.42(13) . . ? C1 Ni1 C51 107.95(13) . . ? C2 Ni1 C51 152.71(13) . . ? C58 Ni1 C51 42.96(12) . . ? C1 N1 C5 111.1(2) . . ? C1 N1 C11 122.2(2) . . ? C5 N1 C11 126.7(2) . . ? C1 N2 C6 113.0(2) . . ? C1 N2 C32 120.0(2) . . ? C6 N2 C32 127.0(2) . . ? C2 N3 C3 112.9(2) . . ? C2 N3 C32 120.0(2) . . ? C3 N3 C32 127.0(2) . . ? C2 N4 C4 112.0(2) . . ? C2 N4 C41 121.7(2) . . ? C4 N4 C41 126.3(2) . . ? N2 C1 N1 103.5(2) . . ? N2 C1 Ni1 114.2(2) . . ? N1 C1 Ni1 142.1(2) . . ? N4 C2 N3 102.8(2) . . ? N4 C2 Ni1 143.6(2) . . ? N3 C2 Ni1 113.4(2) . . ? C4 C3 N3 105.7(3) . . ? C4 C3 C30 131.4(3) . . ? N3 C3 C30 122.9(3) . . ? C3 C4 N4 106.5(2) . . ? C3 C4 C40 125.4(3) . . ? N4 C4 C40 127.9(3) . . ? C6 C5 N1 105.9(2) . . ? C6 C5 C50 126.8(3) . . ? N1 C5 C50 127.2(3) . . ? C5 C6 N2 106.3(3) . . ? C5 C6 C60 129.6(3) . . ? N2 C6 C60 124.0(3) . . ? N1 C11 C111 109.3(3) . . ? N1 C11 C113 108.2(3) . . ? C111 C11 C113 109.5(3) . . ? N1 C11 C112 110.5(3) . . ? C111 C11 C112 107.5(3) . . ? C113 C11 C112 111.8(3) . . ? C3 C30 H30A 109.5 . . ? C3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C32 N2 110.3(2) . . ? N3 C32 H32A 109.6 . . ? N2 C32 H32A 109.6 . . ? N3 C32 H32B 109.6 . . ? N2 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C4 C40 H40A 109.5 . . ? C4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C412 C41 C413 108.2(8) . . ? C412 C41 C411 108.6(5) . . ? C413 C41 C411 108.2(7) . . ? C412 C41 N4 113.3(4) . . ? C413 C41 N4 108.0(3) . . ? C411 C41 N4 110.4(3) . . ? C5 C50 H50A 109.5 . . ? C5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C58 C51 C52 124.3(3) . . ? C58 C51 Ni1 68.43(17) . . ? C52 C51 Ni1 116.4(2) . . ? C58 C51 H51A 113.4 . . ? C52 C51 H51A 113.4 . . ? Ni1 C51 H51A 113.4 . . ? C51 C52 C53 114.3(3) . . ? C51 C52 H52A 108.7 . . ? C53 C52 H52A 108.7 . . ? C51 C52 H52B 108.7 . . ? C53 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C54 C53 C52 114.6(3) . . ? C54 C53 H53A 108.6 . . ? C52 C53 H53A 108.6 . . ? C54 C53 H53B 108.6 . . ? C52 C53 H53B 108.6 . . ? H53A C53 H53B 107.6 . . ? C55 C54 C53 127.4(4) . . ? C55 C54 H54A 116.3 . . ? C53 C54 H54A 116.3 . . ? C54 C55 C56 125.0(3) . . ? C54 C55 H55A 117.5 . . ? C56 C55 H55A 117.5 . . ? C55 C56 C57 113.8(3) . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56B 108.8 . . ? C57 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C58 C57 C56 114.1(2) . . ? C58 C57 H57A 108.7 . . ? C56 C57 H57A 108.7 . . ? C58 C57 H57B 108.7 . . ? C56 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? C51 C58 C57 122.9(3) . . ? C51 C58 Ni1 68.61(17) . . ? C57 C58 Ni1 117.4(2) . . ? C51 C58 H58A 113.5 . . ? C57 C58 H58A 113.5 . . ? Ni1 C58 H58A 113.5 . . ? C6 C60 H60A 109.5 . . ? C6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C11 C112 H11D 109.5 . . ? C11 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C11 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C11 C113 H11G 109.5 . . ? C11 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C11 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C41 C411 H41A 109.5 . . ? C41 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C41 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C41 C412 H41D 109.5 . . ? C41 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C41 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? C41 C413 H41G 109.5 . . ? C41 C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? C41 C413 H41I 109.5 . . ? H41G C413 H41I 109.5 . . ? H41H C413 H41I 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 C6 N2 C1 N1 -1.8(3) . . . . ? C32 N2 C1 N1 179.7(3) . . . . ? C6 N2 C1 Ni1 174.8(2) . . . . ? C32 N2 C1 Ni1 -3.7(4) . . . . ? C5 N1 C1 N2 3.2(3) . . . . ? C11 N1 C1 N2 -177.2(3) . . . . ? C5 N1 C1 Ni1 -171.8(3) . . . . ? C11 N1 C1 Ni1 7.8(5) . . . . ? C2 Ni1 C1 N2 48.3(2) . . . . ? C58 Ni1 C1 N2 -97.3(3) . . . . ? C51 Ni1 C1 N2 -113.6(2) . . . . ? C2 Ni1 C1 N1 -137.1(4) . . . . ? C58 Ni1 C1 N1 77.4(5) . . . . ? C51 Ni1 C1 N1 61.1(4) . . . . ? C4 N4 C2 N3 -2.0(3) . . . . ? C41 N4 C2 N3 178.5(3) . . . . ? C4 N4 C2 Ni1 -176.7(3) . . . . ? C41 N4 C2 Ni1 3.8(5) . . . . ? C3 N3 C2 N4 1.5(3) . . . . ? C32 N3 C2 N4 -175.6(3) . . . . ? C3 N3 C2 Ni1 178.1(2) . . . . ? C32 N3 C2 Ni1 1.0(3) . . . . ? C1 Ni1 C2 N4 127.6(4) . . . . ? C58 Ni1 C2 N4 -70.6(4) . . . . ? C51 Ni1 C2 N4 -92.6(5) . . . . ? C1 Ni1 C2 N3 -46.8(2) . . . . ? C58 Ni1 C2 N3 115.0(2) . . . . ? C51 Ni1 C2 N3 93.0(3) . . . . ? C2 N3 C3 C4 -0.4(4) . . . . ? C32 N3 C3 C4 176.5(3) . . . . ? C2 N3 C3 C30 178.8(3) . . . . ? C32 N3 C3 C30 -4.4(5) . . . . ? N3 C3 C4 N4 -0.9(3) . . . . ? C30 C3 C4 N4 -179.9(3) . . . . ? N3 C3 C4 C40 174.9(3) . . . . ? C30 C3 C4 C40 -4.1(6) . . . . ? C2 N4 C4 C3 1.9(4) . . . . ? C41 N4 C4 C3 -178.7(3) . . . . ? C2 N4 C4 C40 -173.8(3) . . . . ? C41 N4 C4 C40 5.7(5) . . . . ? C1 N1 C5 C6 -3.4(4) . . . . ? C11 N1 C5 C6 177.0(3) . . . . ? C1 N1 C5 C50 173.3(3) . . . . ? C11 N1 C5 C50 -6.2(5) . . . . ? N1 C5 C6 N2 2.1(3) . . . . ? C50 C5 C6 N2 -174.6(3) . . . . ? N1 C5 C6 C60 -175.4(3) . . . . ? C50 C5 C6 C60 7.8(6) . . . . ? C1 N2 C6 C5 -0.2(4) . . . . ? C32 N2 C6 C5 178.1(3) . . . . ? C1 N2 C6 C60 177.5(3) . . . . ? C32 N2 C6 C60 -4.1(5) . . . . ? C1 N1 C11 C111 24.0(4) . . . . ? C5 N1 C11 C111 -156.5(3) . . . . ? C1 N1 C11 C113 -95.2(3) . . . . ? C5 N1 C11 C113 84.3(4) . . . . ? C1 N1 C11 C112 142.1(3) . . . . ? C5 N1 C11 C112 -38.4(4) . . . . ? C2 N3 C32 N2 56.8(4) . . . . ? C3 N3 C32 N2 -119.9(3) . . . . ? C1 N2 C32 N3 -55.5(4) . . . . ? C6 N2 C32 N3 126.3(3) . . . . ? C2 N4 C41 C412 -144.1(5) . . . . ? C4 N4 C41 C412 36.5(6) . . . . ? C2 N4 C41 C413 96.1(8) . . . . ? C4 N4 C41 C413 -83.3(8) . . . . ? C2 N4 C41 C411 -22.0(6) . . . . ? C4 N4 C41 C411 158.6(5) . . . . ? C1 Ni1 C51 C58 167.83(18) . . . . ? C2 Ni1 C51 C58 30.6(4) . . . . ? C1 Ni1 C51 C52 49.2(3) . . . . ? C2 Ni1 C51 C52 -88.1(4) . . . . ? C58 Ni1 C51 C52 -118.7(3) . . . . ? C58 C51 C52 C53 73.1(4) . . . . ? Ni1 C51 C52 C53 154.0(2) . . . . ? C51 C52 C53 C54 -100.9(4) . . . . ? C52 C53 C54 C55 70.5(6) . . . . ? C53 C54 C55 C56 -0.2(7) . . . . ? C54 C55 C56 C57 -71.2(5) . . . . ? C55 C56 C57 C58 103.7(3) . . . . ? C52 C51 C58 C57 -1.6(5) . . . . ? Ni1 C51 C58 C57 -109.6(3) . . . . ? C52 C51 C58 Ni1 108.0(3) . . . . ? C56 C57 C58 C51 -72.2(4) . . . . ? C56 C57 C58 Ni1 -153.3(2) . . . . ? C1 Ni1 C58 C51 -23.1(3) . . . . ? C2 Ni1 C58 C51 -165.39(18) . . . . ? C1 Ni1 C58 C57 93.9(3) . . . . ? C2 Ni1 C58 C57 -48.4(3) . . . . ? C51 Ni1 C58 C57 117.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.713 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 901782' ####################################################################### # # 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_(TMTBM)Ni(N3Ar) #TrackingRef 'Bent imido complete cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 N7 Ni' _chemical_formula_weight 578.46 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 12.1740(13) _cell_length_b 26.324(3) _cell_length_c 31.697(3) _cell_angle_alpha 112.359(2) _cell_angle_beta 99.666(2) _cell_angle_gamma 92.719(2) _cell_volume 9191.5(17) _cell_formula_units_Z 10 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 93 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.330 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.9568 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details 'Norton et. al' _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58784 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.4934 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.33 _reflns_number_total 42463 _reflns_number_gt 31531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^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 42463 _refine_ls_number_parameters 1826 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2227 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 0.686 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.94320(10) 0.29385(4) 0.06733(4) 0.044 Uani 1 1 d . . . N1 N 1.0534(5) 0.3055(2) 0.1211(2) 0.043 Uani 1 1 d . . . N2 N 1.0604(6) 0.3441(2) 0.1074(2) 0.041 Uani 1 1 d . . . N3 N 1.1336(6) 0.3888(2) 0.1222(2) 0.049 Uani 1 1 d . . . N4 N 0.8168(6) 0.1780(3) 0.0442(2) 0.051 Uani 1 1 d . . . N5 N 0.8891(5) 0.1935(2) -0.0072(2) 0.041 Uani 1 1 d . . . N6 N 0.8931(6) 0.2736(2) -0.0253(2) 0.044 Uani 1 1 d . . . N7 N 0.8145(6) 0.3447(3) 0.0040(2) 0.048 Uani 1 1 d . . . C1 C 0.8764(7) 0.3092(3) 0.0162(3) 0.045 Uani 1 1 d . . . C2 C 0.8715(7) 0.2197(3) 0.0382(3) 0.040 Uani 1 1 d . . . C3 C 0.7974(7) 0.3330(3) -0.0432(3) 0.044 Uani 1 1 d . . . C4 C 0.8455(7) 0.2890(3) -0.0609(3) 0.041 Uani 1 1 d . . . C5 C 0.8474(7) 0.1370(3) -0.0273(3) 0.048 Uani 1 1 d . . . C6 C 0.8007(7) 0.1269(3) 0.0052(3) 0.050 Uani 1 1 d . . . C7 C 0.9459(7) 0.2253(3) -0.0290(3) 0.041 Uani 1 1 d . . . H7A H 1.0259 0.2361 -0.0134 0.050 Uiso 1 1 calc R . . H7B H 0.9423 0.2018 -0.0623 0.050 Uiso 1 1 calc R . . C30 C 0.7400(8) 0.3650(3) -0.0686(3) 0.071 Uani 1 1 d . . . H30A H 0.7415 0.3468 -0.1018 0.107 Uiso 1 1 calc R . . H30B H 0.7789 0.4027 -0.0562 0.107 Uiso 1 1 calc R . . H30C H 0.6619 0.3663 -0.0647 0.107 Uiso 1 1 calc R . . C40 C 0.8587(8) 0.2563(3) -0.1103(3) 0.057 Uani 1 1 d . . . H40A H 0.8409 0.2781 -0.1291 0.086 Uiso 1 1 calc R . . H40B H 0.8075 0.2217 -0.1236 0.086 Uiso 1 1 calc R . . H40C H 0.9362 0.2478 -0.1101 0.086 Uiso 1 1 calc R . . C50 C 0.8610(7) 0.1015(3) -0.0749(3) 0.052 Uani 1 1 d . . . H50A H 0.8240 0.0640 -0.0837 0.077 Uiso 1 1 calc R . . H50B H 0.9411 0.1001 -0.0754 0.077 Uiso 1 1 calc R . . H50C H 0.8269 0.1168 -0.0970 0.077 Uiso 1 1 calc R . . C60 C 0.7459(8) 0.0721(3) -0.0015(3) 0.072 Uani 1 1 d . . . H60A H 0.7533 0.0446 -0.0318 0.108 Uiso 1 1 calc R . . H60B H 0.6662 0.0743 -0.0005 0.108 Uiso 1 1 calc R . . H60C H 0.7820 0.0613 0.0233 0.108 Uiso 1 1 calc R . . C80 C 1.1220(7) 0.4167(3) 0.0916(3) 0.043 Uani 1 1 d . . . C81 C 1.0943(8) 0.4720(3) 0.1098(3) 0.056 Uani 1 1 d . . . C82 C 1.0898(7) 0.5032(4) 0.0835(3) 0.060 Uani 1 1 d . . . H82B H 1.0744 0.5405 0.0962 0.072 Uiso 1 1 calc R . . C83 C 1.1082(8) 0.4798(4) 0.0374(3) 0.068 Uani 1 1 d . . . H83H H 1.1012 0.5005 0.0185 0.082 Uiso 1 1 calc R . . C84 C 1.1353(8) 0.4285(3) 0.0208(3) 0.066 Uani 1 1 d . . . H84I H 1.1502 0.4138 -0.0098 0.079 Uiso 1 1 calc R . . C85 C 1.1428(7) 0.3959(3) 0.0461(3) 0.046 Uani 1 1 d . . . C87 C 1.0003(8) 0.5418(3) 0.1718(3) 0.076 Uani 1 1 d . . . H87U H 0.9257 0.5254 0.1526 0.113 Uiso 1 1 calc R . . H87V H 1.0266 0.5732 0.1651 0.113 Uiso 1 1 calc R . . H87W H 0.9962 0.5548 0.2048 0.113 Uiso 1 1 calc R . . C88 C 1.1962(7) 0.5225(3) 0.1928(3) 0.056 Uani 1 1 d . . . H88T H 1.2471 0.4940 0.1871 0.084 Uiso 1 1 calc R . . H88U H 1.1876 0.5357 0.2253 0.084 Uiso 1 1 calc R . . H88V H 1.2274 0.5535 0.1867 0.084 Uiso 1 1 calc R . . C89 C 1.1901(8) 0.3410(3) 0.0290(3) 0.055 Uani 1 1 d . . . H8B H 1.1525 0.3155 0.0404 0.066 Uiso 1 1 calc R . . C90 C 1.1688(8) 0.3146(4) -0.0235(3) 0.078 Uani 1 1 d . . . H91R H 1.0900 0.3153 -0.0362 0.117 Uiso 1 1 calc R . . H91S H 1.1854 0.2762 -0.0336 0.117 Uiso 1 1 calc R . . H91T H 1.2172 0.3352 -0.0348 0.117 Uiso 1 1 calc R . . C91 C 1.3156(8) 0.3503(4) 0.0495(3) 0.079 Uani 1 1 d . . . H91A H 1.3278 0.3680 0.0836 0.118 Uiso 1 1 calc R . . H91B H 1.3540 0.3742 0.0378 0.118 Uiso 1 1 calc R . . H91C H 1.3457 0.3146 0.0404 0.118 Uiso 1 1 calc R . . C401 C 0.7894(9) 0.1869(4) 0.0892(3) 0.065 Uani 1 1 d . . . C402 C 0.7711(10) 0.2459(4) 0.1145(3) 0.101 Uani 1 1 d . . . H40D H 0.8381 0.2704 0.1180 0.152 Uiso 1 1 calc R . . H40E H 0.7570 0.2511 0.1454 0.152 Uiso 1 1 calc R . . H40F H 0.7063 0.2546 0.0967 0.152 Uiso 1 1 calc R . . C404 C 0.8880(10) 0.1789(5) 0.1196(4) 0.122 Uani 1 1 d . . . H40G H 0.9506 0.2071 0.1254 0.183 Uiso 1 1 calc R . . H40H H 0.9100 0.1420 0.1042 0.183 Uiso 1 1 calc R . . H40I H 0.8685 0.1823 0.1492 0.183 Uiso 1 1 calc R . . C701 C 0.7586(8) 0.3875(3) 0.0380(3) 0.052 Uani 1 1 d . . . C702 C 0.8032(8) 0.3939(3) 0.0866(3) 0.065 Uani 1 1 d . . . H70A H 0.8841 0.4058 0.0946 0.098 Uiso 1 1 calc R . . H70B H 0.7891 0.3584 0.0892 0.098 Uiso 1 1 calc R . . H70C H 0.7656 0.4217 0.1079 0.098 Uiso 1 1 calc R . . C703 C 0.6309(8) 0.3670(4) 0.0257(3) 0.082 Uani 1 1 d . . . H70G H 0.6197 0.3304 0.0267 0.123 Uiso 1 1 calc R . . H70H H 0.5993 0.3646 -0.0056 0.123 Uiso 1 1 calc R . . H70I H 0.5932 0.3931 0.0483 0.123 Uiso 1 1 calc R . . C704 C 0.7810(8) 0.4442(3) 0.0363(3) 0.067 Uani 1 1 d . . . H70D H 0.8609 0.4518 0.0368 0.101 Uiso 1 1 calc R . . H70E H 0.7605 0.4726 0.0634 0.101 Uiso 1 1 calc R . . H70F H 0.7361 0.4444 0.0077 0.101 Uiso 1 1 calc R . . C841 C 1.0824(7) 0.4983(3) 0.1608(3) 0.051 Uani 1 1 d . . . H84B H 1.0532 0.4676 0.1688 0.061 Uiso 1 1 calc R . . C911 C 0.6825(9) 0.1513(4) 0.0858(4) 0.104 Uani 1 1 d . . . H91F H 0.6314 0.1436 0.0561 0.156 Uiso 1 1 calc R . . H91G H 0.6456 0.1712 0.1115 0.156 Uiso 1 1 calc R . . H91H H 0.7018 0.1164 0.0876 0.156 Uiso 1 1 calc R . . Ni2 Ni 0.80212(9) 0.84559(4) 0.14509(3) 0.035 Uani 1 1 d . . . N8 N 0.9267(6) 0.8293(2) 0.1165(2) 0.044 Uani 1 1 d . . . N9 N 0.8597(5) 0.8500(2) 0.09663(19) 0.035 Uani 1 1 d . . . N10 N 0.8622(6) 0.8618(2) 0.0596(2) 0.044 Uani 1 1 d . . . N11 N 0.8580(5) 0.7976(2) 0.22081(19) 0.033 Uani 1 1 d . . . N12 N 0.8262(5) 0.8830(2) 0.24072(19) 0.031 Uani 1 1 d . . . N13 N 0.6850(5) 0.9201(2) 0.2025(2) 0.035 Uani 1 1 d . . . N14 N 0.5592(6) 0.8783(3) 0.1415(2) 0.051 Uani 1 1 d . . . C808 C 0.6697(7) 0.8788(3) 0.1597(3) 0.038 Uani 1 1 d . . . C823 C 0.8482(6) 0.8738(3) 0.2822(2) 0.030 Uani 1 1 d . . . C824 C 0.7778(7) 0.8916(3) 0.0466(3) 0.043 Uani 1 1 d . . . C826 C 0.8716(6) 0.8216(3) 0.2706(2) 0.033 Uani 1 1 d . . . C835 C 0.7910(6) 0.9320(3) 0.2335(3) 0.036 Uani 1 1 d . . . H83B H 0.7862 0.9612 0.2639 0.044 Uiso 1 1 calc R . . H83C H 0.8482 0.9464 0.2207 0.044 Uiso 1 1 calc R . . C836 C 0.8433(7) 0.9193(3) 0.3286(2) 0.043 Uani 1 1 d . . . H83D H 0.8599 0.9054 0.3533 0.065 Uiso 1 1 calc R . . H83E H 0.7681 0.9311 0.3275 0.065 Uiso 1 1 calc R . . H83F H 0.8988 0.9509 0.3350 0.065 Uiso 1 1 calc R . . C838 C 0.8270(7) 0.8350(3) 0.2009(3) 0.038 Uani 1 1 d . . . C842 C 0.7625(7) 0.9456(3) 0.0759(3) 0.047 Uani 1 1 d . . . C843 C 0.9035(7) 0.7958(3) 0.3026(2) 0.040 Uani 1 1 d . . . H84C H 0.9047 0.8222 0.3344 0.060 Uiso 1 1 calc R . . H84D H 0.9784 0.7843 0.3003 0.060 Uiso 1 1 calc R . . H84E H 0.8493 0.7633 0.2950 0.060 Uiso 1 1 calc R . . C854 C 0.5083(8) 0.9189(4) 0.1743(3) 0.063 Uani 1 1 d . . . C857 C 0.8342(8) 0.9747(3) 0.1241(3) 0.056 Uani 1 1 d . . . H85I H 0.8626 0.9462 0.1355 0.067 Uiso 1 1 calc R . . C862 C 0.8608(9) 0.7373(3) 0.1919(3) 0.069 Uani 1 1 d . . . C869 C 0.6216(8) 0.9483(4) 0.0115(3) 0.062 Uani 1 1 d . . . H86R H 0.5690 0.9679 0.0001 0.075 Uiso 1 1 calc R . . C870 C 0.6387(8) 0.8955(4) -0.0164(3) 0.059 Uani 1 1 d . . . H87A H 0.5983 0.8785 -0.0477 0.071 Uiso 1 1 calc R . . C873 C 0.5890(8) 0.9439(3) 0.2116(3) 0.051 Uani 1 1 d . . . C881 C 0.5029(8) 0.8386(4) 0.0945(3) 0.058 Uani 1 1 d . . . C893 C 0.7148(8) 0.8675(4) 0.0012(3) 0.061 Uani 1 1 d . . . C895 C 0.8287(8) 0.7257(3) 0.1412(2) 0.061 Uani 1 1 d . . . H89M H 0.8849 0.7457 0.1325 0.092 Uiso 1 1 calc R . . H89N H 0.7551 0.7378 0.1348 0.092 Uiso 1 1 calc R . . H89O H 0.8249 0.6858 0.1230 0.092 Uiso 1 1 calc R . . C899 C 0.4714(8) 0.8695(4) 0.0631(3) 0.082 Uani 1 1 d . . . H8A H 0.4163 0.8944 0.0749 0.123 Uiso 1 1 calc R . . H89Y H 0.4390 0.8429 0.0314 0.123 Uiso 1 1 calc R . . H89Z H 0.5387 0.8912 0.0627 0.123 Uiso 1 1 calc R . . C901 C 0.5779(8) 0.7946(3) 0.0721(3) 0.073 Uani 1 1 d . . . H90A H 0.6429 0.8123 0.0662 0.109 Uiso 1 1 calc R . . H90B H 0.5348 0.7669 0.0427 0.109 Uiso 1 1 calc R . . H90C H 0.6038 0.7765 0.0933 0.109 Uiso 1 1 calc R . . C902 C 0.7638(9) 1.0114(3) 0.1587(3) 0.086 Uani 1 1 d . . . H90D H 0.6928 0.9897 0.1553 0.128 Uiso 1 1 calc R . . H90E H 0.7484 1.0438 0.1516 0.128 Uiso 1 1 calc R . . H90F H 0.8063 1.0236 0.1907 0.128 Uiso 1 1 calc R . . C904 C 0.3990(8) 0.8054(4) 0.0985(3) 0.094 Uani 1 1 d . . . H90J H 0.4228 0.7868 0.1194 0.140 Uiso 1 1 calc R . . H90K H 0.3635 0.7778 0.0676 0.140 Uiso 1 1 calc R . . H90L H 0.3452 0.8308 0.1111 0.140 Uiso 1 1 calc R . . C905 C 0.5873(7) 0.9913(3) 0.2573(3) 0.062 Uani 1 1 d . . . H90M H 0.5144 1.0055 0.2556 0.093 Uiso 1 1 calc R . . H90N H 0.6469 1.0210 0.2632 0.093 Uiso 1 1 calc R . . H90O H 0.5994 0.9782 0.2826 0.093 Uiso 1 1 calc R . . C906 C 0.3914(8) 0.9305(4) 0.1648(4) 0.102 Uani 1 1 d . . . H90P H 0.3793 0.9634 0.1908 0.153 Uiso 1 1 calc R . . H90Q H 0.3399 0.8988 0.1612 0.153 Uiso 1 1 calc R . . H90R H 0.3776 0.9372 0.1361 0.153 Uiso 1 1 calc R . . C910 C 0.7324(10) 0.8089(4) -0.0310(3) 0.104 Uani 1 1 d . . . H91E H 0.7500 0.7869 -0.0114 0.125 Uiso 1 1 calc R . . C915 C 0.9720(12) 0.7241(5) 0.2031(3) 0.189 Uani 1 1 d . . . H91U H 1.0233 0.7406 0.1897 0.283 Uiso 1 1 calc R . . H91V H 0.9717 0.6838 0.1903 0.283 Uiso 1 1 calc R . . H91W H 0.9971 0.7389 0.2370 0.283 Uiso 1 1 calc R . . C916 C 0.7646(13) 0.7043(3) 0.2016(3) 0.163 Uani 1 1 d . . . H91X H 0.7685 0.6645 0.1862 0.244 Uiso 1 1 calc R . . H91Y H 0.6918 0.7131 0.1895 0.244 Uiso 1 1 calc R . . H91Z H 0.7735 0.7146 0.2352 0.244 Uiso 1 1 calc R . . C917 C 0.9336(8) 1.0107(3) 0.1231(3) 0.080 Uani 1 1 d . . . H92A H 0.9716 0.9891 0.0984 0.120 Uiso 1 1 calc R . . H92B H 0.9861 1.0241 0.1532 0.120 Uiso 1 1 calc R . . H92C H 0.9073 1.0424 0.1170 0.120 Uiso 1 1 calc R . . C920 C 0.6841(8) 0.9719(3) 0.0569(3) 0.057 Uani 1 1 d . . . H88S H 0.6724 1.0082 0.0761 0.068 Uiso 1 1 calc R . . C993 C 0.6274(12) 0.7786(4) -0.0686(4) 0.186 Uani 1 1 d . . . H99M H 0.6484 0.7477 -0.0938 0.279 Uiso 1 1 calc R . . H99N H 0.5938 0.8044 -0.0811 0.279 Uiso 1 1 calc R . . H99O H 0.5729 0.7645 -0.0550 0.279 Uiso 1 1 calc R . . C999 C 0.8366(13) 0.8148(5) -0.0518(4) 0.182 Uani 1 1 d . . . H99J H 0.8556 0.7780 -0.0697 0.273 Uiso 1 1 calc R . . H99K H 0.9003 0.8357 -0.0266 0.273 Uiso 1 1 calc R . . H99L H 0.8197 0.8345 -0.0724 0.273 Uiso 1 1 calc R . . Ni3 Ni 0.17253(9) 0.48850(4) 0.30679(3) 0.031 Uani 1 1 d . . . N15 N 0.1290(5) 0.5551(2) 0.3048(2) 0.036 Uani 1 1 d . . . N16 N 0.0567(5) 0.5305(2) 0.3152(2) 0.032 Uani 1 1 d . . . N17 N -0.0438(5) 0.5444(2) 0.32153(19) 0.032 Uani 1 1 d . . . N18 N 0.4075(6) 0.4913(2) 0.2810(2) 0.043 Uani 1 1 d . . . N19 N 0.2826(6) 0.4225(2) 0.2402(2) 0.037 Uani 1 1 d . . . N20 N 0.1538(5) 0.3739(2) 0.2644(2) 0.029 Uani 1 1 d . . . N21 N 0.1437(5) 0.3880(2) 0.3349(2) 0.029 Uani 1 1 d . . . C805 C -0.1527(7) 0.5253(3) 0.3719(3) 0.039 Uani 1 1 d . . . C810 C 0.1374(6) 0.3223(3) 0.2659(2) 0.030 Uani 1 1 d . . . C811 C 0.1305(6) 0.3307(3) 0.3088(2) 0.025 Uani 1 1 d . . . C812 C -0.1492(7) 0.4496(3) 0.2986(3) 0.036 Uani 1 1 d . . . C815 C 0.1767(7) 0.3869(3) 0.2257(2) 0.039 Uani 1 1 d . . . H81C H 0.1804 0.3524 0.1989 0.046 Uiso 1 1 calc R . . H81D H 0.1154 0.4059 0.2158 0.046 Uiso 1 1 calc R . . C817 C 0.1556(6) 0.4159(3) 0.3073(2) 0.026 Uani 1 1 d . . . C818 C -0.1111(6) 0.5039(3) 0.3301(2) 0.029 Uani 1 1 d . . . C820 C 0.2979(7) 0.4707(3) 0.2770(3) 0.041 Uani 1 1 d . . . C833 C 0.1424(7) 0.4164(3) 0.3869(2) 0.037 Uani 1 1 d . . . C840 C -0.2195(7) 0.4157(3) 0.3094(3) 0.052 Uani 1 1 d . . . H84A H -0.2417 0.3782 0.2885 0.062 Uiso 1 1 calc R . . C844 C -0.2573(7) 0.4367(3) 0.3505(3) 0.045 Uani 1 1 d . . . H84F H -0.3069 0.4137 0.3578 0.054 Uiso 1 1 calc R . . C845 C -0.1092(7) 0.4277(3) 0.2512(3) 0.045 Uani 1 1 d . . . H84G H -0.0263 0.4389 0.2586 0.054 Uiso 1 1 calc R . . C846 C -0.1181(6) 0.5855(3) 0.4052(3) 0.038 Uani 1 1 d . . . H84H H -0.1224 0.6075 0.3854 0.046 Uiso 1 1 calc R . . C850 C 0.1133(6) 0.2880(3) 0.3275(2) 0.034 Uani 1 1 d . . . H85A H 0.0885 0.2519 0.3017 0.052 Uiso 1 1 calc R . . H85B H 0.0560 0.2975 0.3467 0.052 Uiso 1 1 calc R . . H85C H 0.1840 0.2861 0.3466 0.052 Uiso 1 1 calc R . . C856 C -0.2242(7) 0.4902(3) 0.3809(3) 0.043 Uani 1 1 d . . . H85H H -0.2511 0.5036 0.4092 0.052 Uiso 1 1 calc R . . C858 C 0.3753(7) 0.4127(3) 0.2188(3) 0.049 Uani 1 1 d . . . C861 C 0.1875(7) 0.4771(3) 0.4026(2) 0.050 Uani 1 1 d . . . H86B H 0.1822 0.4972 0.4352 0.075 Uiso 1 1 calc R . . H86C H 0.1430 0.4932 0.3831 0.075 Uiso 1 1 calc R . . H86D H 0.2661 0.4801 0.3996 0.075 Uiso 1 1 calc R . . C864 C 0.1318(7) 0.2709(3) 0.2241(2) 0.045 Uani 1 1 d . . . H86H H 0.1047 0.2392 0.2301 0.067 Uiso 1 1 calc R . . H86I H 0.2067 0.2665 0.2168 0.067 Uiso 1 1 calc R . . H86J H 0.0802 0.2730 0.1977 0.067 Uiso 1 1 calc R . . C865 C 0.4544(7) 0.5469(3) 0.3183(3) 0.044 Uani 1 1 d . . . C868 C 0.0191(6) 0.4120(3) 0.3925(3) 0.043 Uani 1 1 d . . . H86O H 0.0153 0.4320 0.4253 0.064 Uiso 1 1 calc R . . H86P H -0.0100 0.3730 0.3824 0.064 Uiso 1 1 calc R . . H86Q H -0.0261 0.4283 0.3735 0.064 Uiso 1 1 calc R . . C872 C 0.3957(7) 0.5912(3) 0.3062(3) 0.053 Uani 1 1 d . . . H87E H 0.3146 0.5840 0.3037 0.079 Uiso 1 1 calc R . . H87F H 0.4106 0.5901 0.2765 0.079 Uiso 1 1 calc R . . H87G H 0.4243 0.6278 0.3308 0.079 Uiso 1 1 calc R . . C876 C 0.4355(7) 0.5491(3) 0.3649(3) 0.054 Uani 1 1 d . . . H87K H 0.3547 0.5445 0.3641 0.082 Uiso 1 1 calc R . . H87L H 0.4694 0.5850 0.3894 0.082 Uiso 1 1 calc R . . H87M H 0.4701 0.5194 0.3715 0.082 Uiso 1 1 calc R . . C882 C 0.2143(7) 0.3917(3) 0.4141(2) 0.046 Uani 1 1 d . . . H88A H 0.2275 0.4161 0.4472 0.069 Uiso 1 1 calc R . . H88B H 0.2862 0.3871 0.4039 0.069 Uiso 1 1 calc R . . H88C H 0.1772 0.3556 0.4093 0.069 Uiso 1 1 calc R . . C887 C -0.1274(7) 0.3641(3) 0.2276(3) 0.062 Uani 1 1 d . . . H88P H -0.0960 0.3519 0.1993 0.094 Uiso 1 1 calc R . . H88Q H -0.2080 0.3512 0.2194 0.094 Uiso 1 1 calc R . . H88R H -0.0899 0.3486 0.2490 0.094 Uiso 1 1 calc R . . C888 C 0.4529(8) 0.4548(3) 0.2438(3) 0.054 Uani 1 1 d . . . C890 C 0.3723(8) 0.3601(3) 0.1769(3) 0.072 Uani 1 1 d . . . H89A H 0.4414 0.3609 0.1651 0.109 Uiso 1 1 calc R . . H89B H 0.3074 0.3566 0.1527 0.109 Uiso 1 1 calc R . . H89C H 0.3660 0.3284 0.1858 0.109 Uiso 1 1 calc R . . C892 C -0.1602(7) 0.4527(3) 0.2177(3) 0.056 Uani 1 1 d . . . H89G H -0.1470 0.4932 0.2331 0.084 Uiso 1 1 calc R . . H89H H -0.2412 0.4407 0.2080 0.084 Uiso 1 1 calc R . . H89I H -0.1254 0.4404 0.1903 0.084 Uiso 1 1 calc R . . C912 C 0.5672(8) 0.4596(4) 0.2347(4) 0.104 Uani 1 1 d . . . H91I H 0.5752 0.4268 0.2077 0.156 Uiso 1 1 calc R . . H91J H 0.6224 0.4622 0.2620 0.156 Uiso 1 1 calc R . . H91K H 0.5799 0.4928 0.2284 0.156 Uiso 1 1 calc R . . C913 C 0.5812(7) 0.5606(4) 0.3236(3) 0.076 Uani 1 1 d . . . H91L H 0.5968 0.5623 0.2948 0.115 Uiso 1 1 calc R . . H91M H 0.6204 0.5317 0.3299 0.115 Uiso 1 1 calc R . . H91N H 0.6075 0.5964 0.3495 0.115 Uiso 1 1 calc R . . C990 C 0.0005(8) 0.5951(3) 0.4299(3) 0.062 Uani 1 1 d . . . H99S H 0.0214 0.6347 0.4493 0.094 Uiso 1 1 calc R . . H99T H 0.0492 0.5830 0.4071 0.094 Uiso 1 1 calc R . . H99U H 0.0095 0.5741 0.4497 0.094 Uiso 1 1 calc R . . C991 C -0.1897(8) 0.6097(3) 0.4395(3) 0.077 Uani 1 1 d . . . H99V H -0.1710 0.6500 0.4538 0.116 Uiso 1 1 calc R . . H99W H -0.1766 0.5948 0.4637 0.116 Uiso 1 1 calc R . . H99X H -0.2688 0.6003 0.4238 0.116 Uiso 1 1 calc R . . Ni4 Ni 0.99128(8) 0.23844(4) 0.57284(3) 0.029 Uani 1 1 d . . . N22 N 0.8216(5) 0.2016(2) 0.6239(2) 0.033 Uani 1 1 d . . . N23 N 0.9078(5) 0.2845(2) 0.65339(19) 0.025 Uani 1 1 d . . . N24 N 1.0991(5) 0.3143(2) 0.6592(2) 0.030 Uani 1 1 d . . . N25 N 1.2264(5) 0.2629(2) 0.63547(19) 0.033 Uani 1 1 d . . . N26 N 1.0332(5) 0.2450(2) 0.52062(18) 0.031 Uani 1 1 d . . . N27 N 0.9313(6) 0.2296(2) 0.51315(19) 0.036 Uani 1 1 d . . . N28 N 0.8546(5) 0.2205(2) 0.4766(2) 0.033 Uani 1 1 d . . . C801 C 0.6844(6) 0.2401(3) 0.5118(2) 0.032 Uani 1 1 d . . . C802 C 0.8999(6) 0.2359(2) 0.6153(2) 0.022 Uani 1 1 d . . . C803 C 0.7417(6) 0.2041(3) 0.4797(2) 0.029 Uani 1 1 d . . . C804 C 0.9881(6) 0.3318(3) 0.6599(2) 0.030 Uani 1 1 d . . . H80A H 0.9660 0.3450 0.6347 0.036 Uiso 1 1 calc R . . H80B H 0.9881 0.3626 0.6901 0.036 Uiso 1 1 calc R . . C813 C 0.5704(7) 0.2199(3) 0.5086(3) 0.045 Uani 1 1 d . . . H81A H 0.5279 0.2429 0.5292 0.054 Uiso 1 1 calc R . . C814 C 0.7522(7) 0.1187(3) 0.4104(3) 0.046 Uani 1 1 d . . . H81B H 0.8321 0.1360 0.4194 0.055 Uiso 1 1 calc R . . C819 C 0.8391(6) 0.2812(3) 0.6839(2) 0.028 Uani 1 1 d . . . C822 C 0.7328(7) 0.2979(3) 0.5437(2) 0.034 Uani 1 1 d . . . H82A H 0.8165 0.2998 0.5503 0.041 Uiso 1 1 calc R . . C825 C 1.1169(6) 0.2685(3) 0.6218(2) 0.029 Uani 1 1 d . . . C827 C 0.7838(6) 0.2284(3) 0.6646(2) 0.030 Uani 1 1 d . . . C828 C 1.2746(7) 0.3049(3) 0.6795(3) 0.037 Uani 1 1 d . . . C829 C 0.7885(7) 0.1404(3) 0.5915(3) 0.047 Uani 1 1 d . . . C849 C 1.1960(7) 0.3375(3) 0.6943(2) 0.032 Uani 1 1 d . . . C851 C 0.8326(7) 0.3293(3) 0.7263(3) 0.049 Uani 1 1 d . . . H85D H 0.7661 0.3225 0.7379 0.073 Uiso 1 1 calc R . . H85E H 0.8272 0.3622 0.7190 0.073 Uiso 1 1 calc R . . H85F H 0.9001 0.3353 0.7501 0.073 Uiso 1 1 calc R . . C853 C 1.2818(8) 0.2187(4) 0.6035(3) 0.056 Uani 1 1 d . . . C855 C 0.5209(7) 0.1691(3) 0.4773(3) 0.052 Uani 1 1 d . . . H85G H 0.4465 0.1562 0.4771 0.062 Uiso 1 1 calc R . . C859 C 0.7002(7) 0.3374(3) 0.5203(3) 0.050 Uani 1 1 d . . . H85J H 0.7237 0.3251 0.4902 0.075 Uiso 1 1 calc R . . H85K H 0.7372 0.3748 0.5402 0.075 Uiso 1 1 calc R . . H85L H 0.6186 0.3376 0.5153 0.075 Uiso 1 1 calc R . . C863 C 0.8544(8) 0.1226(3) 0.5513(3) 0.073 Uani 1 1 d . . . H86E H 0.8268 0.1390 0.5291 0.110 Uiso 1 1 calc R . . H86F H 0.8435 0.0822 0.5354 0.110 Uiso 1 1 calc R . . H86G H 0.9345 0.1354 0.5641 0.110 Uiso 1 1 calc R . . C867 C 0.5800(7) 0.1365(3) 0.4457(3) 0.047 Uani 1 1 d . . . H86N H 0.5450 0.1013 0.4234 0.057 Uiso 1 1 calc R . . C871 C 0.6976(7) 0.2074(3) 0.6841(3) 0.051 Uani 1 1 d . . . H87B H 0.6897 0.2364 0.7136 0.077 Uiso 1 1 calc R . . H87C H 0.7208 0.1749 0.6894 0.077 Uiso 1 1 calc R . . H87D H 0.6255 0.1972 0.6620 0.077 Uiso 1 1 calc R . . C879 C 1.1957(7) 0.3877(3) 0.7366(3) 0.049 Uani 1 1 d . . . H87R H 1.2721 0.3997 0.7553 0.074 Uiso 1 1 calc R . . H87S H 1.1460 0.3792 0.7550 0.074 Uiso 1 1 calc R . . H87T H 1.1689 0.4173 0.7275 0.074 Uiso 1 1 calc R . . C884 C 0.6929(7) 0.3170(3) 0.5899(2) 0.049 Uani 1 1 d . . . H88G H 0.6978 0.2878 0.6019 0.074 Uiso 1 1 calc R . . H88H H 0.6149 0.3247 0.5849 0.074 Uiso 1 1 calc R . . H88I H 0.7405 0.3506 0.6124 0.074 Uiso 1 1 calc R . . C886 C 1.3927(7) 0.3119(3) 0.7056(3) 0.056 Uani 1 1 d . . . H88M H 1.4064 0.3464 0.7335 0.084 Uiso 1 1 calc R . . H88N H 1.4452 0.3131 0.6856 0.084 Uiso 1 1 calc R . . H88O H 1.4037 0.2806 0.7149 0.084 Uiso 1 1 calc R . . C889 C 0.6879(7) 0.1536(3) 0.4456(3) 0.038 Uani 1 1 d . . . C894 C 1.1999(8) 0.1698(3) 0.5728(3) 0.067 Uani 1 1 d . . . H89J H 1.1646 0.1548 0.5920 0.100 Uiso 1 1 calc R . . H89K H 1.2387 0.1414 0.5527 0.100 Uiso 1 1 calc R . . H89L H 1.1421 0.1808 0.5536 0.100 Uiso 1 1 calc R . . C903 C 0.8265(8) 0.1078(3) 0.6203(3) 0.065 Uani 1 1 d . . . H90G H 0.9080 0.1161 0.6315 0.097 Uiso 1 1 calc R . . H90H H 0.8069 0.0682 0.6011 0.097 Uiso 1 1 calc R . . H90I H 0.7892 0.1180 0.6469 0.097 Uiso 1 1 calc R . . C909 C 1.3695(9) 0.1983(5) 0.6312(4) 0.139 Uani 1 1 d . . . H90Y H 1.3362 0.1885 0.6536 0.208 Uiso 1 1 calc R . . H90Z H 1.4324 0.2277 0.6481 0.208 Uiso 1 1 calc R . . H91D H 1.3967 0.1657 0.6100 0.208 Uiso 1 1 calc R . . C918 C 1.3259(10) 0.2422(4) 0.5733(4) 0.131 Uani 1 1 d . . . H92D H 1.3458 0.2124 0.5469 0.196 Uiso 1 1 calc R . . H92E H 1.3927 0.2687 0.5912 0.196 Uiso 1 1 calc R . . H92F H 1.2684 0.2611 0.5616 0.196 Uiso 1 1 calc R . . C919 C 0.6638(7) 0.1291(4) 0.5724(3) 0.088 Uani 1 1 d . . . H92G H 0.6442 0.1487 0.5519 0.132 Uiso 1 1 calc R . . H92H H 0.6236 0.1419 0.5981 0.132 Uiso 1 1 calc R . . H92I H 0.6426 0.0892 0.5546 0.132 Uiso 1 1 calc R . . C994 C 0.7499(17) 0.0618(5) 0.4069(5) 0.291 Uani 1 1 d . . . H99P H 0.7249 0.0363 0.3743 0.436 Uiso 1 1 calc R . . H99Q H 0.6979 0.0555 0.4254 0.436 Uiso 1 1 calc R . . H99R H 0.8254 0.0554 0.4188 0.436 Uiso 1 1 calc R . . C998 C 0.7071(11) 0.1164(7) 0.3671(4) 0.221 Uani 1 1 d . . . H99G H 0.6650 0.1480 0.3701 0.331 Uiso 1 1 calc R . . H99H H 0.6565 0.0819 0.3496 0.331 Uiso 1 1 calc R . . H99I H 0.7675 0.1177 0.3504 0.331 Uiso 1 1 calc R . . Ni5 Ni 0.00746(8) 0.12444(3) 0.32182(3) 0.026 Uani 1 1 d . . . N29 N -0.1488(5) 0.2129(2) 0.3190(2) 0.038 Uani 1 1 d . . . N30 N -0.0346(5) 0.2258(2) 0.3825(2) 0.032 Uani 1 1 d . . . N31 N 0.1542(5) 0.2065(2) 0.39512(19) 0.028 Uani 1 1 d . . . N32 N 0.2570(5) 0.1748(2) 0.3452(2) 0.030 Uani 1 1 d . . . N33 N -0.1054(5) 0.0633(2) 0.29800(19) 0.029 Uani 1 1 d . . . N34 N -0.0107(5) 0.0513(2) 0.30907(19) 0.025 Uani 1 1 d . . . N35 N 0.0181(5) 0.0023(2) 0.3081(2) 0.036 Uani 1 1 d . . . C800 C -0.0642(6) 0.1890(3) 0.3374(2) 0.024 Uani 1 1 d . . . C806 C 0.0513(6) 0.2140(3) 0.4141(2) 0.035 Uani 1 1 d . . . H80C H 0.0251 0.1800 0.4178 0.042 Uiso 1 1 calc R . . H80D H 0.0665 0.2450 0.4451 0.042 Uiso 1 1 calc R . . C807 C 0.2602(7) 0.2371(3) 0.4161(3) 0.032 Uani 1 1 d . . . C809 C 0.1504(6) 0.1670(2) 0.3514(2) 0.021 Uani 1 1 d . . . C816 C 0.1870(7) -0.0389(3) 0.2928(3) 0.044 Uani 1 1 d . . . C821 C 0.1954(7) 0.0339(3) 0.3702(3) 0.033 Uani 1 1 d . . . C830 C 0.1335(6) 0.0010(3) 0.3241(3) 0.030 Uani 1 1 d . . . C831 C -0.0985(7) 0.2700(3) 0.3934(3) 0.041 Uani 1 1 d . . . C832 C 0.1324(7) 0.0695(3) 0.4067(2) 0.037 Uani 1 1 d . . . H83A H 0.0740 0.0853 0.3907 0.045 Uiso 1 1 calc R . . C834 C 0.3260(6) 0.2161(3) 0.3843(2) 0.029 Uani 1 1 d . . . C837 C 0.2941(7) 0.1426(3) 0.3008(3) 0.034 Uani 1 1 d . . . C839 C 0.1182(8) -0.0764(3) 0.2439(3) 0.051 Uani 1 1 d . . . H83G H 0.0412 -0.0851 0.2483 0.061 Uiso 1 1 calc R . . C847 C -0.1697(7) 0.2615(3) 0.3544(3) 0.046 Uani 1 1 d . . . C860 C 0.2993(7) -0.0444(3) 0.3066(3) 0.049 Uani 1 1 d . . . H86A H 0.3358 -0.0707 0.2855 0.059 Uiso 1 1 calc R . . C866 C -0.0781(7) 0.3160(3) 0.4399(2) 0.051 Uani 1 1 d . . . H86K H -0.1321 0.3425 0.4400 0.076 Uiso 1 1 calc R . . H86L H -0.0016 0.3347 0.4472 0.076 Uiso 1 1 calc R . . H86M H -0.0870 0.3013 0.4634 0.076 Uiso 1 1 calc R . . C875 C 0.2081(7) 0.1176(3) 0.4460(3) 0.059 Uani 1 1 d . . . H87H H 0.1620 0.1438 0.4640 0.089 Uiso 1 1 calc R . . H87I H 0.2558 0.1364 0.4330 0.089 Uiso 1 1 calc R . . H87J H 0.2554 0.1036 0.4664 0.089 Uiso 1 1 calc R . . C877 C 0.3572(7) -0.0116(3) 0.3507(3) 0.056 Uani 1 1 d . . . H87N H 0.4342 -0.0146 0.3600 0.068 Uiso 1 1 calc R . . C878 C 0.2842(7) 0.2810(3) 0.4645(2) 0.045 Uani 1 1 d . . . H87O H 0.3654 0.2920 0.4750 0.067 Uiso 1 1 calc R . . H87P H 0.2562 0.2665 0.4855 0.067 Uiso 1 1 calc R . . H87Q H 0.2467 0.3132 0.4647 0.067 Uiso 1 1 calc R . . C880 C -0.2051(8) 0.1887(3) 0.2687(3) 0.060 Uani 1 1 d . . . C883 C 0.4487(7) 0.2345(3) 0.3912(3) 0.057 Uani 1 1 d . . . H88D H 0.4770 0.2595 0.4238 0.086 Uiso 1 1 calc R . . H88E H 0.4592 0.2539 0.3710 0.086 Uiso 1 1 calc R . . H88F H 0.4898 0.2021 0.3834 0.086 Uiso 1 1 calc R . . C885 C 0.1948(8) 0.1091(3) 0.2644(3) 0.070 Uani 1 1 d . . . H88J H 0.1577 0.0838 0.2751 0.105 Uiso 1 1 calc R . . H88K H 0.2195 0.0878 0.2355 0.105 Uiso 1 1 calc R . . H88L H 0.1421 0.1339 0.2587 0.105 Uiso 1 1 calc R . . C891 C 0.3720(8) 0.1039(3) 0.3087(3) 0.073 Uani 1 1 d . . . H89D H 0.3356 0.0804 0.3214 0.109 Uiso 1 1 calc R . . H89E H 0.4405 0.1251 0.3308 0.109 Uiso 1 1 calc R . . H89F H 0.3912 0.0806 0.2791 0.109 Uiso 1 1 calc R . . C896 C 0.0736(8) 0.0383(3) 0.4295(3) 0.072 Uani 1 1 d . . . H89P H 0.0215 0.0074 0.4055 0.108 Uiso 1 1 calc R . . H89Q H 0.0318 0.0633 0.4509 0.108 Uiso 1 1 calc R . . H89R H 0.1294 0.0241 0.4468 0.108 Uiso 1 1 calc R . . C897 C 0.3484(7) 0.1819(3) 0.2831(3) 0.057 Uani 1 1 d . . . H89S H 0.2984 0.2097 0.2820 0.085 Uiso 1 1 calc R . . H89T H 0.3614 0.1609 0.2517 0.085 Uiso 1 1 calc R . . H89U H 0.4201 0.2003 0.3041 0.085 Uiso 1 1 calc R . . C898 C -0.2644(7) 0.2966(3) 0.3490(3) 0.070 Uani 1 1 d . . . H89V H -0.2708 0.3232 0.3798 0.105 Uiso 1 1 calc R . . H89W H -0.3355 0.2724 0.3339 0.105 Uiso 1 1 calc R . . H89X H -0.2473 0.3165 0.3299 0.105 Uiso 1 1 calc R . . C907 C -0.1309(8) 0.1527(3) 0.2395(3) 0.070 Uani 1 1 d . . . H90S H -0.1152 0.1224 0.2495 0.106 Uiso 1 1 calc R . . H90T H -0.0602 0.1749 0.2433 0.106 Uiso 1 1 calc R . . H90U H -0.1689 0.1374 0.2067 0.106 Uiso 1 1 calc R . . C908 C -0.2280(10) 0.2345(4) 0.2490(3) 0.110 Uani 1 1 d . . . H90V H -0.1576 0.2578 0.2545 0.166 Uiso 1 1 calc R . . H90W H -0.2818 0.2574 0.2648 0.166 Uiso 1 1 calc R . . H90X H -0.2590 0.2169 0.2155 0.166 Uiso 1 1 calc R . . C914 C -0.3131(9) 0.1538(5) 0.2619(4) 0.126 Uani 1 1 d . . . H91O H -0.2975 0.1242 0.2728 0.189 Uiso 1 1 calc R . . H91P H -0.3484 0.1376 0.2288 0.189 Uiso 1 1 calc R . . H91Q H -0.3638 0.1769 0.2797 0.189 Uiso 1 1 calc R . . C930 C 0.3027(7) 0.0256(3) 0.3815(3) 0.048 Uani 1 1 d . . . H93A H 0.3430 0.0464 0.4124 0.058 Uiso 1 1 calc R . . C996 C 0.1037(8) -0.0455(3) 0.2110(3) 0.057 Uani 1 1 d . . . H99A H 0.0511 -0.0685 0.1820 0.085 Uiso 1 1 calc R . . H99B H 0.1765 -0.0380 0.2039 0.085 Uiso 1 1 calc R . . H99C H 0.0742 -0.0105 0.2260 0.085 Uiso 1 1 calc R . . C997 C 0.1628(9) -0.1308(4) 0.2237(3) 0.100 Uani 1 1 d . . . H99D H 0.1121 -0.1546 0.1945 0.151 Uiso 1 1 calc R . . H99E H 0.1679 -0.1488 0.2459 0.151 Uiso 1 1 calc R . . H99F H 0.2375 -0.1246 0.2176 0.151 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.051 0.040 0.042 0.019 0.010 0.005 N1 0.044 0.043 0.036 0.015 -0.002 0.005 N2 0.061 0.030 0.023 0.003 0.006 0.003 N3 0.073 0.033 0.037 0.005 0.023 0.002 N4 0.059 0.048 0.051 0.030 0.007 -0.006 N5 0.046 0.031 0.049 0.024 -0.003 0.002 N6 0.065 0.031 0.049 0.027 0.016 0.018 N7 0.059 0.045 0.036 0.016 -0.001 0.015 C1 0.058 0.035 0.045 0.017 0.011 0.019 C2 0.032 0.061 0.045 0.036 0.013 0.004 C3 0.042 0.046 0.045 0.017 0.009 0.008 C4 0.050 0.033 0.037 0.014 0.000 0.005 C5 0.050 0.029 0.063 0.021 0.004 0.007 C6 0.053 0.055 0.049 0.038 -0.011 -0.004 C7 0.040 0.051 0.035 0.021 0.006 0.002 C30 0.098 0.052 0.050 0.014 -0.009 0.022 C40 0.075 0.047 0.054 0.031 0.000 0.010 C50 0.045 0.038 0.066 0.024 -0.008 -0.003 C60 0.084 0.060 0.076 0.042 -0.002 -0.017 C80 0.058 0.037 0.034 0.016 0.010 -0.008 C81 0.055 0.060 0.054 0.030 0.006 -0.012 C82 0.061 0.063 0.068 0.043 0.003 -0.001 C83 0.094 0.078 0.040 0.038 0.001 -0.006 C84 0.104 0.050 0.042 0.018 0.016 -0.001 C85 0.047 0.060 0.034 0.019 0.013 0.003 C87 0.075 0.038 0.103 0.011 0.026 0.016 C88 0.067 0.062 0.049 0.028 0.022 0.017 C89 0.079 0.051 0.027 0.004 0.023 0.002 C90 0.086 0.091 0.049 0.015 0.030 -0.015 C91 0.053 0.093 0.076 0.025 -0.003 0.004 C401 0.084 0.063 0.053 0.032 0.007 -0.016 C402 0.130 0.097 0.073 0.026 0.040 -0.029 C404 0.114 0.202 0.091 0.101 0.023 0.024 C701 0.060 0.058 0.043 0.025 0.008 0.025 C702 0.063 0.075 0.052 0.021 0.008 0.013 C703 0.056 0.085 0.093 0.027 0.010 0.003 C704 0.079 0.048 0.061 0.013 0.000 0.009 C841 0.062 0.042 0.061 0.027 0.032 0.009 C911 0.130 0.078 0.112 0.044 0.042 -0.035 Ni2 0.053 0.023 0.029 0.011 0.004 0.005 N8 0.061 0.039 0.029 0.016 -0.007 0.013 N9 0.060 0.025 0.014 0.010 -0.009 0.007 N10 0.057 0.039 0.040 0.018 0.005 0.016 N11 0.039 0.037 0.026 0.016 0.009 0.004 N12 0.033 0.030 0.030 0.010 0.007 0.007 N13 0.031 0.024 0.043 0.013 -0.007 -0.002 N14 0.030 0.066 0.055 0.033 -0.017 -0.014 C808 0.061 0.021 0.039 0.018 0.009 0.002 C823 0.028 0.035 0.030 0.015 0.011 0.007 C824 0.065 0.034 0.040 0.023 0.019 0.009 C826 0.043 0.041 0.021 0.018 0.009 0.004 C835 0.036 0.028 0.050 0.021 0.010 0.001 C836 0.048 0.041 0.028 0.001 0.009 -0.001 C838 0.059 0.022 0.035 0.011 0.016 0.003 C842 0.056 0.053 0.045 0.031 0.014 0.001 C843 0.043 0.048 0.026 0.013 0.006 0.005 C854 0.039 0.073 0.075 0.028 0.008 0.019 C857 0.078 0.033 0.068 0.039 0.000 0.003 C862 0.144 0.028 0.034 0.011 0.020 0.016 C869 0.054 0.091 0.059 0.047 0.013 0.009 C870 0.063 0.065 0.058 0.035 0.006 0.018 C873 0.041 0.045 0.082 0.037 0.018 0.015 C881 0.046 0.065 0.066 0.039 -0.008 -0.021 C893 0.086 0.066 0.033 0.025 0.008 0.013 C895 0.131 0.020 0.030 0.002 0.030 0.007 C899 0.060 0.101 0.102 0.069 -0.004 -0.021 C901 0.083 0.071 0.042 0.017 -0.022 -0.027 C902 0.120 0.043 0.073 0.003 0.016 -0.004 C904 0.087 0.105 0.082 0.046 -0.003 -0.051 C905 0.047 0.050 0.098 0.032 0.026 0.014 C906 0.036 0.125 0.124 0.036 -0.003 0.007 C910 0.144 0.098 0.055 0.016 -0.002 0.077 C915 0.266 0.205 0.051 0.005 -0.024 0.207 C916 0.381 0.033 0.068 0.001 0.096 -0.045 C917 0.078 0.046 0.109 0.030 0.002 0.005 C920 0.067 0.048 0.083 0.044 0.038 0.029 C993 0.248 0.084 0.096 -0.047 -0.113 0.030 C999 0.313 0.229 0.063 0.084 0.076 0.220 Ni3 0.035 0.024 0.039 0.015 0.015 0.003 N15 0.037 0.023 0.051 0.014 0.020 -0.001 N16 0.025 0.031 0.043 0.016 0.012 0.001 N17 0.031 0.020 0.042 0.007 0.012 0.001 N18 0.039 0.036 0.064 0.026 0.023 0.004 N19 0.046 0.033 0.045 0.022 0.023 0.006 N20 0.026 0.037 0.036 0.025 0.011 0.008 N21 0.027 0.030 0.039 0.023 0.011 0.005 C805 0.041 0.029 0.040 0.005 0.010 0.001 C810 0.032 0.028 0.036 0.019 0.003 0.006 C811 0.026 0.014 0.041 0.019 0.003 0.004 C812 0.053 0.019 0.040 0.009 0.022 0.008 C815 0.046 0.041 0.026 0.010 0.007 0.001 C817 0.023 0.031 0.036 0.024 0.009 0.004 C818 0.020 0.037 0.027 0.011 0.004 0.004 C820 0.038 0.033 0.066 0.030 0.025 0.007 C833 0.052 0.026 0.031 0.007 0.010 0.012 C840 0.042 0.047 0.060 0.012 0.020 -0.013 C844 0.050 0.034 0.058 0.020 0.027 -0.005 C845 0.042 0.036 0.046 0.003 0.015 -0.006 C846 0.029 0.040 0.039 0.007 0.005 0.007 C850 0.025 0.035 0.045 0.019 0.001 0.006 C856 0.051 0.045 0.038 0.017 0.021 -0.004 C858 0.043 0.058 0.058 0.027 0.032 0.023 C861 0.069 0.041 0.034 0.007 0.014 -0.011 C864 0.064 0.019 0.045 0.008 0.011 0.000 C865 0.036 0.041 0.064 0.033 0.002 0.003 C868 0.039 0.048 0.047 0.018 0.023 0.011 C872 0.046 0.053 0.063 0.027 0.013 0.001 C876 0.050 0.047 0.071 0.035 0.000 -0.011 C882 0.071 0.049 0.024 0.021 0.007 0.010 C887 0.058 0.050 0.063 0.001 0.023 -0.010 C888 0.052 0.053 0.081 0.041 0.040 0.021 C890 0.092 0.064 0.059 0.005 0.052 0.028 C892 0.070 0.064 0.045 0.023 0.031 0.017 C912 0.064 0.130 0.158 0.075 0.082 0.027 C913 0.035 0.084 0.137 0.074 0.014 0.009 C990 0.083 0.041 0.054 0.014 0.004 -0.004 C991 0.089 0.053 0.071 -0.003 0.035 -0.003 Ni4 0.029 0.033 0.026 0.012 0.010 0.006 N22 0.035 0.027 0.042 0.020 0.006 0.000 N23 0.020 0.021 0.037 0.015 0.008 0.003 N24 0.023 0.042 0.039 0.026 0.013 0.007 N25 0.026 0.052 0.023 0.019 0.000 0.001 N26 0.005 0.057 0.020 0.009 -0.006 -0.006 N27 0.048 0.043 0.019 0.014 0.001 0.019 N28 0.028 0.047 0.030 0.019 0.010 0.006 C801 0.027 0.034 0.037 0.015 0.010 -0.003 C802 0.038 0.012 0.021 0.010 0.007 0.002 C803 0.027 0.044 0.028 0.024 0.011 0.008 C804 0.034 0.030 0.023 0.009 0.005 -0.002 C813 0.033 0.061 0.045 0.022 0.017 0.002 C814 0.031 0.039 0.043 -0.004 -0.008 -0.006 C819 0.026 0.043 0.025 0.020 0.010 0.012 C822 0.033 0.044 0.024 0.011 0.006 0.006 C825 0.030 0.043 0.017 0.017 0.001 0.002 C827 0.026 0.034 0.035 0.017 0.011 0.006 C828 0.034 0.049 0.038 0.030 -0.001 -0.005 C829 0.058 0.015 0.067 0.014 0.017 -0.004 C849 0.031 0.033 0.036 0.023 -0.002 -0.005 C851 0.067 0.047 0.054 0.032 0.037 0.023 C853 0.050 0.072 0.049 0.014 0.034 0.035 C855 0.026 0.060 0.052 0.008 0.002 -0.013 C859 0.045 0.043 0.054 0.012 0.010 0.005 C863 0.130 0.032 0.057 0.009 0.041 -0.001 C867 0.033 0.051 0.044 0.006 0.005 -0.006 C871 0.056 0.051 0.065 0.038 0.025 0.004 C879 0.053 0.038 0.048 0.013 -0.002 -0.011 C884 0.052 0.051 0.043 0.018 0.006 0.004 C886 0.031 0.068 0.072 0.038 0.002 -0.012 C889 0.043 0.028 0.039 0.008 0.012 0.003 C894 0.093 0.064 0.041 0.013 0.021 0.029 C903 0.107 0.028 0.063 0.027 0.007 0.000 C909 0.092 0.159 0.101 -0.016 -0.009 0.091 C918 0.154 0.117 0.134 0.029 0.115 0.005 C919 0.036 0.078 0.110 0.006 -0.010 -0.016 C994 0.609 0.164 0.288 0.161 0.349 0.284 C998 0.080 0.433 0.094 0.021 0.050 0.124 Ni5 0.029 0.020 0.029 0.009 0.009 0.003 N29 0.036 0.035 0.046 0.024 0.001 0.000 N30 0.033 0.035 0.037 0.019 0.017 0.014 N31 0.032 0.028 0.028 0.008 0.018 0.010 N32 0.022 0.032 0.040 0.015 0.012 0.003 N33 0.015 0.023 0.042 0.007 0.002 -0.001 N34 0.017 0.022 0.036 0.013 0.003 -0.003 N35 0.044 0.025 0.036 0.010 0.006 -0.002 C800 0.030 0.019 0.026 0.010 0.009 0.003 C806 0.042 0.036 0.029 0.008 0.020 0.016 C807 0.036 0.023 0.037 0.015 0.002 -0.007 C809 0.023 0.014 0.026 0.011 -0.001 -0.001 C816 0.041 0.044 0.053 0.027 0.011 0.007 C821 0.038 0.019 0.042 0.014 0.005 -0.003 C830 0.029 0.022 0.042 0.016 0.009 0.007 C831 0.054 0.041 0.047 0.027 0.032 0.015 C832 0.048 0.029 0.028 0.010 -0.002 -0.010 C834 0.032 0.016 0.037 0.011 0.002 0.006 C837 0.036 0.027 0.050 0.023 0.016 0.008 C839 0.057 0.035 0.041 -0.004 0.000 0.016 C847 0.052 0.025 0.071 0.021 0.029 0.013 C860 0.037 0.044 0.075 0.031 0.016 0.015 C866 0.068 0.041 0.050 0.011 0.044 0.008 C875 0.065 0.058 0.047 0.020 -0.006 -0.010 C877 0.033 0.051 0.082 0.032 -0.008 -0.011 C878 0.049 0.042 0.044 0.019 0.008 -0.002 C880 0.042 0.051 0.076 0.018 0.002 0.001 C883 0.032 0.058 0.080 0.031 0.001 -0.005 C885 0.074 0.076 0.055 0.008 0.042 0.010 C891 0.075 0.071 0.098 0.045 0.048 0.039 C896 0.092 0.066 0.070 0.032 0.042 -0.013 C897 0.070 0.053 0.052 0.022 0.028 -0.011 C898 0.062 0.045 0.116 0.037 0.033 0.022 C907 0.103 0.037 0.056 0.009 0.000 0.006 C908 0.181 0.080 0.083 0.050 0.004 0.063 C914 0.069 0.161 0.124 0.043 0.001 -0.040 C930 0.044 0.035 0.058 0.014 0.000 0.013 C996 0.067 0.051 0.038 0.002 0.009 0.009 C997 0.124 0.068 0.067 -0.014 -0.005 0.045 _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 N2 1.825(7) . ? Ni1 C1 1.882(8) . ? Ni1 N1 1.895(6) . ? Ni1 C2 1.904(8) . ? N1 N2 1.250(7) . ? N2 N3 1.319(8) . ? N3 C80 1.417(9) . ? N4 C2 1.346(8) . ? N4 C6 1.416(9) . ? N4 C401 1.455(9) . ? N5 C2 1.398(8) . ? N5 C5 1.405(9) . ? N5 C7 1.483(8) . ? N6 C1 1.349(8) . ? N6 C4 1.387(9) . ? N6 C7 1.427(8) . ? N7 C1 1.354(8) . ? N7 C3 1.382(9) . ? N7 C701 1.514(9) . ? C3 C4 1.296(9) . ? C3 C30 1.494(10) . ? C4 C40 1.513(9) . ? C5 C6 1.361(10) . ? C5 C50 1.483(9) . ? C6 C60 1.482(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C80 C85 1.407(9) . ? C80 C81 1.429(10) . ? C81 C82 1.372(10) . ? C81 C841 1.534(10) . ? C82 C83 1.413(10) . ? C82 H82B 0.9500 . ? C83 C84 1.329(10) . ? C83 H83H 0.9500 . ? C84 C85 1.375(10) . ? C84 H84I 0.9500 . ? C85 C89 1.518(10) . ? C87 C841 1.535(10) . ? C87 H87U 0.9800 . ? C87 H87V 0.9800 . ? C87 H87W 0.9800 . ? C88 C841 1.519(11) . ? C88 H88T 0.9800 . ? C88 H88U 0.9800 . ? C88 H88V 0.9800 . ? C89 C90 1.509(10) . ? C89 C91 1.525(11) . ? C89 H8B 1.0000 . ? C90 H91R 0.9800 . ? C90 H91S 0.9800 . ? C90 H91T 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C401 C404 1.483(13) . ? C401 C402 1.500(11) . ? C401 C911 1.531(12) . ? C402 H40D 0.9800 . ? C402 H40E 0.9800 . ? C402 H40F 0.9800 . ? C404 H40G 0.9800 . ? C404 H40H 0.9800 . ? C404 H40I 0.9800 . ? C701 C702 1.484(10) . ? C701 C704 1.525(10) . ? C701 C703 1.555(11) . ? C702 H70A 0.9800 . ? C702 H70B 0.9800 . ? C702 H70C 0.9800 . ? C703 H70G 0.9800 . ? C703 H70H 0.9800 . ? C703 H70I 0.9800 . ? C704 H70D 0.9800 . ? C704 H70E 0.9800 . ? C704 H70F 0.9800 . ? C841 H84B 1.0000 . ? C911 H91F 0.9800 . ? C911 H91G 0.9800 . ? C911 H91H 0.9800 . ? Ni2 N9 1.831(6) . ? Ni2 C838 1.870(7) . ? Ni2 N8 1.880(6) . ? Ni2 C808 1.911(8) . ? N8 N9 1.221(7) . ? N9 N10 1.329(7) . ? N10 C824 1.421(9) . ? N11 C838 1.393(8) . ? N11 C826 1.436(8) . ? N11 C862 1.506(9) . ? N12 C838 1.408(8) . ? N12 C823 1.409(8) . ? N12 C835 1.465(8) . ? N13 C808 1.353(8) . ? N13 C873 1.374(9) . ? N13 C835 1.425(9) . ? N14 C808 1.370(9) . ? N14 C854 1.427(9) . ? N14 C881 1.479(10) . ? C823 C826 1.337(8) . ? C823 C836 1.518(8) . ? C824 C893 1.398(10) . ? C824 C842 1.413(9) . ? C826 C843 1.436(9) . ? C835 H83B 0.9900 . ? C835 H83C 0.9900 . ? C836 H83D 0.9800 . ? C836 H83E 0.9800 . ? C836 H83F 0.9800 . ? C842 C920 1.392(10) . ? C842 C857 1.511(11) . ? C843 H84C 0.9800 . ? C843 H84D 0.9800 . ? C843 H84E 0.9800 . ? C854 C873 1.325(11) . ? C854 C906 1.475(11) . ? C857 C917 1.515(11) . ? C857 C902 1.566(10) . ? C857 H85I 1.0000 . ? C862 C915 1.435(14) . ? C862 C895 1.493(10) . ? C862 C916 1.565(13) . ? C869 C870 1.383(10) . ? C869 C920 1.394(11) . ? C869 H86R 0.9500 . ? C870 C893 1.385(11) . ? C870 H87A 0.9500 . ? C873 C905 1.514(10) . ? C881 C899 1.524(10) . ? C881 C901 1.539(11) . ? C881 C904 1.552(11) . ? C893 C910 1.540(11) . ? C895 H89M 0.9800 . ? C895 H89N 0.9800 . ? C895 H89O 0.9800 . ? C899 H8A 0.9800 . ? C899 H89Y 0.9800 . ? C899 H89Z 0.9800 . ? C901 H90A 0.9800 . ? C901 H90B 0.9800 . ? C901 H90C 0.9800 . ? C902 H90D 0.9800 . ? C902 H90E 0.9800 . ? C902 H90F 0.9800 . ? C904 H90J 0.9800 . ? C904 H90K 0.9800 . ? C904 H90L 0.9800 . ? C905 H90M 0.9800 . ? C905 H90N 0.9800 . ? C905 H90O 0.9800 . ? C906 H90P 0.9800 . ? C906 H90Q 0.9800 . ? C906 H90R 0.9800 . ? C910 C993 1.537(14) . ? C910 C999 1.554(16) . ? C910 H91E 1.0000 . ? C915 H91U 0.9800 . ? C915 H91V 0.9800 . ? C915 H91W 0.9800 . ? C916 H91X 0.9800 . ? C916 H91Y 0.9800 . ? C916 H91Z 0.9800 . ? C917 H92A 0.9800 . ? C917 H92B 0.9800 . ? C917 H92C 0.9800 . ? C920 H88S 0.9500 . ? C993 H99M 0.9800 . ? C993 H99N 0.9800 . ? C993 H99O 0.9800 . ? C999 H99J 0.9800 . ? C999 H99K 0.9800 . ? C999 H99L 0.9800 . ? Ni3 N16 1.825(6) . ? Ni3 N15 1.876(5) . ? Ni3 C820 1.912(7) . ? Ni3 C817 1.919(6) . ? N15 N16 1.229(7) . ? N16 N17 1.320(7) . ? N17 C818 1.446(8) . ? N18 C820 1.383(9) . ? N18 C888 1.424(9) . ? N18 C865 1.498(9) . ? N19 C820 1.337(8) . ? N19 C858 1.396(8) . ? N19 C815 1.452(9) . ? N20 C810 1.382(7) . ? N20 C817 1.385(8) . ? N20 C815 1.458(8) . ? N21 C817 1.358(7) . ? N21 C811 1.404(7) . ? N21 C833 1.532(8) . ? C805 C856 1.379(9) . ? C805 C818 1.420(8) . ? C805 C846 1.521(9) . ? C810 C811 1.312(8) . ? C810 C864 1.480(8) . ? C811 C850 1.478(8) . ? C812 C840 1.379(9) . ? C812 C818 1.397(9) . ? C812 C845 1.562(9) . ? C815 H81C 0.9900 . ? C815 H81D 0.9900 . ? C833 C882 1.469(9) . ? C833 C861 1.524(9) . ? C833 C868 1.545(10) . ? C840 C844 1.377(9) . ? C840 H84A 0.9500 . ? C844 C856 1.362(9) . ? C844 H84F 0.9500 . ? C845 C892 1.517(10) . ? C845 C887 1.539(9) . ? C845 H84G 1.0000 . ? C846 C991 1.481(9) . ? C846 C990 1.483(10) . ? C846 H84H 1.0000 . ? C850 H85A 0.9800 . ? C850 H85B 0.9800 . ? C850 H85C 0.9800 . ? C856 H85H 0.9500 . ? C858 C888 1.314(11) . ? C858 C890 1.505(10) . ? C861 H86B 0.9800 . ? C861 H86C 0.9800 . ? C861 H86D 0.9800 . ? C864 H86H 0.9800 . ? C864 H86I 0.9800 . ? C864 H86J 0.9800 . ? C865 C876 1.514(9) . ? C865 C872 1.529(9) . ? C865 C913 1.535(10) . ? C868 H86O 0.9800 . ? C868 H86P 0.9800 . ? C868 H86Q 0.9800 . ? C872 H87E 0.9800 . ? C872 H87F 0.9800 . ? C872 H87G 0.9800 . ? C876 H87K 0.9800 . ? C876 H87L 0.9800 . ? C876 H87M 0.9800 . ? C882 H88A 0.9800 . ? C882 H88B 0.9800 . ? C882 H88C 0.9800 . ? C887 H88P 0.9800 . ? C887 H88Q 0.9800 . ? C887 H88R 0.9800 . ? C888 C912 1.477(11) . ? C890 H89A 0.9800 . ? C890 H89B 0.9800 . ? C890 H89C 0.9800 . ? C892 H89G 0.9800 . ? C892 H89H 0.9800 . ? C892 H89I 0.9800 . ? C912 H91I 0.9800 . ? C912 H91J 0.9800 . ? C912 H91K 0.9800 . ? C913 H91L 0.9800 . ? C913 H91M 0.9800 . ? C913 H91N 0.9800 . ? C990 H99S 0.9800 . ? C990 H99T 0.9800 . ? C990 H99U 0.9800 . ? C991 H99V 0.9800 . ? C991 H99W 0.9800 . ? C991 H99X 0.9800 . ? Ni4 N27 1.830(6) . ? Ni4 N26 1.877(5) . ? Ni4 C825 1.878(7) . ? Ni4 C802 1.902(6) . ? N22 C827 1.381(8) . ? N22 C802 1.411(8) . ? N22 C829 1.533(8) . ? N23 C802 1.371(7) . ? N23 C819 1.405(7) . ? N23 C804 1.472(8) . ? N24 C825 1.389(8) . ? N24 C849 1.406(9) . ? N24 C804 1.449(8) . ? N25 C825 1.364(8) . ? N25 C828 1.416(9) . ? N25 C853 1.498(8) . ? N26 N27 1.241(7) . ? N27 N28 1.296(7) . ? N28 C803 1.452(8) . ? C801 C803 1.409(8) . ? C801 C813 1.437(10) . ? C801 C822 1.494(9) . ? C803 C889 1.398(9) . ? C804 H80A 0.9900 . ? C804 H80B 0.9900 . ? C813 C855 1.360(10) . ? C813 H81A 0.9500 . ? C814 C998 1.369(13) . ? C814 C994 1.457(12) . ? C814 C889 1.511(9) . ? C814 H81B 1.0000 . ? C819 C827 1.371(9) . ? C819 C851 1.472(9) . ? C822 C859 1.521(9) . ? C822 C884 1.526(8) . ? C822 H82A 1.0000 . ? C827 C871 1.487(9) . ? C828 C849 1.340(9) . ? C828 C886 1.499(10) . ? C829 C903 1.507(10) . ? C829 C919 1.507(11) . ? C829 C863 1.554(10) . ? C849 C879 1.481(9) . ? C851 H85D 0.9800 . ? C851 H85E 0.9800 . ? C851 H85F 0.9800 . ? C853 C918 1.477(11) . ? C853 C894 1.482(11) . ? C853 C909 1.517(12) . ? C855 C867 1.380(9) . ? C855 H85G 0.9500 . ? C859 H85J 0.9800 . ? C859 H85K 0.9800 . ? C859 H85L 0.9800 . ? C863 H86E 0.9800 . ? C863 H86F 0.9800 . ? C863 H86G 0.9800 . ? C867 C889 1.368(10) . ? C867 H86N 0.9500 . ? C871 H87B 0.9800 . ? C871 H87C 0.9800 . ? C871 H87D 0.9800 . ? C879 H87R 0.9800 . ? C879 H87S 0.9800 . ? C879 H87T 0.9800 . ? C884 H88G 0.9800 . ? C884 H88H 0.9800 . ? C884 H88I 0.9800 . ? C886 H88M 0.9800 . ? C886 H88N 0.9800 . ? C886 H88O 0.9800 . ? C894 H89J 0.9800 . ? C894 H89K 0.9800 . ? C894 H89L 0.9800 . ? C903 H90G 0.9800 . ? C903 H90H 0.9800 . ? C903 H90I 0.9800 . ? C909 H90Y 0.9800 . ? C909 H90Z 0.9800 . ? C909 H91D 0.9800 . ? C918 H92D 0.9800 . ? C918 H92E 0.9800 . ? C918 H92F 0.9800 . ? C919 H92G 0.9800 . ? C919 H92H 0.9800 . ? C919 H92I 0.9800 . ? C994 H99P 0.9800 . ? C994 H99Q 0.9800 . ? C994 H99R 0.9800 . ? C998 H99G 0.9800 . ? C998 H99H 0.9800 . ? C998 H99I 0.9800 . ? Ni5 N34 1.806(5) . ? Ni5 C800 1.882(6) . ? Ni5 N33 1.888(6) . ? Ni5 C809 1.906(7) . ? N29 C800 1.389(8) . ? N29 C847 1.411(8) . ? N29 C880 1.496(10) . ? N30 C800 1.362(8) . ? N30 C831 1.396(8) . ? N30 C806 1.452(8) . ? N31 C809 1.372(7) . ? N31 C807 1.401(9) . ? N31 C806 1.469(8) . ? N32 C809 1.362(8) . ? N32 C834 1.400(8) . ? N32 C837 1.498(8) . ? N33 N34 1.239(7) . ? N34 N35 1.341(6) . ? N35 C830 1.419(9) . ? C806 H80C 0.9900 . ? C806 H80D 0.9900 . ? C807 C834 1.361(9) . ? C807 C878 1.499(9) . ? C816 C860 1.395(10) . ? C816 C830 1.415(9) . ? C816 C839 1.550(10) . ? C821 C930 1.347(10) . ? C821 C830 1.433(9) . ? C821 C832 1.532(9) . ? C831 C847 1.318(10) . ? C831 C866 1.481(9) . ? C832 C896 1.510(9) . ? C832 C875 1.520(9) . ? C832 H83A 1.0000 . ? C834 C883 1.501(10) . ? C837 C891 1.484(9) . ? C837 C885 1.492(11) . ? C837 C897 1.525(9) . ? C839 C997 1.501(9) . ? C839 C996 1.542(10) . ? C839 H83G 1.0000 . ? C847 C898 1.540(10) . ? C860 C877 1.376(10) . ? C860 H86A 0.9500 . ? C866 H86K 0.9800 . ? C866 H86L 0.9800 . ? C866 H86M 0.9800 . ? C875 H87H 0.9800 . ? C875 H87I 0.9800 . ? C875 H87J 0.9800 . ? C877 C930 1.379(10) . ? C877 H87N 0.9500 . ? C878 H87O 0.9800 . ? C878 H87P 0.9800 . ? C878 H87Q 0.9800 . ? C880 C914 1.502(12) . ? C880 C907 1.505(10) . ? C880 C908 1.573(11) . ? C883 H88D 0.9800 . ? C883 H88E 0.9800 . ? C883 H88F 0.9800 . ? C885 H88J 0.9800 . ? C885 H88K 0.9800 . ? C885 H88L 0.9800 . ? C891 H89D 0.9800 . ? C891 H89E 0.9800 . ? C891 H89F 0.9800 . ? C896 H89P 0.9800 . ? C896 H89Q 0.9800 . ? C896 H89R 0.9800 . ? C897 H89S 0.9800 . ? C897 H89T 0.9800 . ? C897 H89U 0.9800 . ? C898 H89V 0.9800 . ? C898 H89W 0.9800 . ? C898 H89X 0.9800 . ? C907 H90S 0.9800 . ? C907 H90T 0.9800 . ? C907 H90U 0.9800 . ? C908 H90V 0.9800 . ? C908 H90W 0.9800 . ? C908 H90X 0.9800 . ? C914 H91O 0.9800 . ? C914 H91P 0.9800 . ? C914 H91Q 0.9800 . ? C930 H93A 0.9500 . ? C996 H99A 0.9800 . ? C996 H99B 0.9800 . ? C996 H99C 0.9800 . ? C997 H99D 0.9800 . ? C997 H99E 0.9800 . ? C997 H99F 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 N2 Ni1 C1 115.5(3) . . ? N2 Ni1 N1 39.2(2) . . ? C1 Ni1 N1 154.5(3) . . ? N2 Ni1 C2 149.6(3) . . ? C1 Ni1 C2 91.1(3) . . ? N1 Ni1 C2 112.4(3) . . ? N2 N1 Ni1 67.4(4) . . ? N1 N2 N3 131.4(7) . . ? N1 N2 Ni1 73.4(4) . . ? N3 N2 Ni1 154.9(6) . . ? N2 N3 C80 112.6(7) . . ? C2 N4 C6 113.8(7) . . ? C2 N4 C401 119.9(7) . . ? C6 N4 C401 126.1(7) . . ? C2 N5 C5 112.4(6) . . ? C2 N5 C7 120.5(6) . . ? C5 N5 C7 127.1(7) . . ? C1 N6 C4 110.9(7) . . ? C1 N6 C7 120.9(6) . . ? C4 N6 C7 128.0(6) . . ? C1 N7 C3 112.9(6) . . ? C1 N7 C701 122.3(6) . . ? C3 N7 C701 124.4(6) . . ? N6 C1 N7 102.2(7) . . ? N6 C1 Ni1 114.4(6) . . ? N7 C1 Ni1 143.4(6) . . ? N4 C2 N5 102.0(7) . . ? N4 C2 Ni1 145.8(6) . . ? N5 C2 Ni1 111.8(5) . . ? C4 C3 N7 105.4(7) . . ? C4 C3 C30 126.5(8) . . ? N7 C3 C30 128.0(7) . . ? C3 C4 N6 108.5(7) . . ? C3 C4 C40 131.6(8) . . ? N6 C4 C40 119.9(7) . . ? C6 C5 N5 106.0(7) . . ? C6 C5 C50 133.2(8) . . ? N5 C5 C50 120.8(7) . . ? C5 C6 N4 105.8(7) . . ? C5 C6 C60 124.3(8) . . ? N4 C6 C60 129.9(7) . . ? N6 C7 N5 110.2(6) . . ? N6 C7 H7A 109.6 . . ? N5 C7 H7A 109.6 . . ? N6 C7 H7B 109.6 . . ? N5 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C3 C30 H30A 109.5 . . ? C3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C4 C40 H40A 109.5 . . ? C4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C5 C50 H50A 109.5 . . ? C5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C6 C60 H60A 109.5 . . ? C6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C85 C80 N3 125.6(7) . . ? C85 C80 C81 117.4(7) . . ? N3 C80 C81 116.8(7) . . ? C82 C81 C80 120.4(8) . . ? C82 C81 C841 120.1(8) . . ? C80 C81 C841 119.2(7) . . ? C81 C82 C83 119.9(8) . . ? C81 C82 H82B 120.1 . . ? C83 C82 H82B 120.1 . . ? C84 C83 C82 119.5(8) . . ? C84 C83 H83H 120.2 . . ? C82 C83 H83H 120.2 . . ? C83 C84 C85 122.7(8) . . ? C83 C84 H84I 118.7 . . ? C85 C84 H84I 118.7 . . ? C84 C85 C80 120.0(8) . . ? C84 C85 C89 121.3(7) . . ? C80 C85 C89 118.0(7) . . ? C841 C87 H87U 109.5 . . ? C841 C87 H87V 109.5 . . ? H87U C87 H87V 109.5 . . ? C841 C87 H87W 109.5 . . ? H87U C87 H87W 109.5 . . ? H87V C87 H87W 109.5 . . ? C841 C88 H88T 109.5 . . ? C841 C88 H88U 109.5 . . ? H88T C88 H88U 109.5 . . ? C841 C88 H88V 109.5 . . ? H88T C88 H88V 109.5 . . ? H88U C88 H88V 109.5 . . ? C90 C89 C85 111.4(7) . . ? C90 C89 C91 110.7(7) . . ? C85 C89 C91 109.1(7) . . ? C90 C89 H8B 108.6 . . ? C85 C89 H8B 108.6 . . ? C91 C89 H8B 108.6 . . ? C89 C90 H91R 109.5 . . ? C89 C90 H91S 109.5 . . ? H91R C90 H91S 109.5 . . ? C89 C90 H91T 109.5 . . ? H91R C90 H91T 109.5 . . ? H91S C90 H91T 109.5 . . ? C89 C91 H91A 109.5 . . ? C89 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C89 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N4 C401 C404 109.0(8) . . ? N4 C401 C402 111.3(7) . . ? C404 C401 C402 104.1(9) . . ? N4 C401 C911 113.4(8) . . ? C404 C401 C911 112.4(8) . . ? C402 C401 C911 106.3(8) . . ? C401 C402 H40D 109.5 . . ? C401 C402 H40E 109.5 . . ? H40D C402 H40E 109.5 . . ? C401 C402 H40F 109.5 . . ? H40D C402 H40F 109.5 . . ? H40E C402 H40F 109.5 . . ? C401 C404 H40G 109.5 . . ? C401 C404 H40H 109.5 . . ? H40G C404 H40H 109.5 . . ? C401 C404 H40I 109.5 . . ? H40G C404 H40I 109.5 . . ? H40H C404 H40I 109.5 . . ? C702 C701 N7 111.0(7) . . ? C702 C701 C704 107.0(7) . . ? N7 C701 C704 110.9(7) . . ? C702 C701 C703 108.4(7) . . ? N7 C701 C703 107.8(7) . . ? C704 C701 C703 111.7(7) . . ? C701 C702 H70A 109.5 . . ? C701 C702 H70B 109.5 . . ? H70A C702 H70B 109.5 . . ? C701 C702 H70C 109.5 . . ? H70A C702 H70C 109.5 . . ? H70B C702 H70C 109.5 . . ? C701 C703 H70G 109.5 . . ? C701 C703 H70H 109.5 . . ? H70G C703 H70H 109.5 . . ? C701 C703 H70I 109.5 . . ? H70G C703 H70I 109.5 . . ? H70H C703 H70I 109.5 . . ? C701 C704 H70D 109.5 . . ? C701 C704 H70E 109.5 . . ? H70D C704 H70E 109.5 . . ? C701 C704 H70F 109.5 . . ? H70D C704 H70F 109.5 . . ? H70E C704 H70F 109.5 . . ? C88 C841 C81 110.9(7) . . ? C88 C841 C87 109.6(7) . . ? C81 C841 C87 115.8(7) . . ? C88 C841 H84B 106.7 . . ? C81 C841 H84B 106.7 . . ? C87 C841 H84B 106.7 . . ? C401 C911 H91F 109.5 . . ? C401 C911 H91G 109.5 . . ? H91F C911 H91G 109.5 . . ? C401 C911 H91H 109.5 . . ? H91F C911 H91H 109.5 . . ? H91G C911 H91H 109.5 . . ? N9 Ni2 C838 147.8(3) . . ? N9 Ni2 N8 38.4(2) . . ? C838 Ni2 N8 110.1(3) . . ? N9 Ni2 C808 119.8(3) . . ? C838 Ni2 C808 90.5(3) . . ? N8 Ni2 C808 157.6(3) . . ? N9 N8 Ni2 68.6(4) . . ? N8 N9 N10 130.6(7) . . ? N8 N9 Ni2 73.0(4) . . ? N10 N9 Ni2 156.4(5) . . ? N9 N10 C824 118.6(6) . . ? C838 N11 C826 112.2(6) . . ? C838 N11 C862 122.2(6) . . ? C826 N11 C862 125.1(6) . . ? C838 N12 C823 112.7(6) . . ? C838 N12 C835 117.4(6) . . ? C823 N12 C835 129.4(6) . . ? C808 N13 C873 113.0(7) . . ? C808 N13 C835 119.6(7) . . ? C873 N13 C835 127.3(7) . . ? C808 N14 C854 111.0(7) . . ? C808 N14 C881 122.5(7) . . ? C854 N14 C881 126.5(8) . . ? N13 C808 N14 102.7(7) . . ? N13 C808 Ni2 114.3(6) . . ? N14 C808 Ni2 142.9(6) . . ? C826 C823 N12 107.1(6) . . ? C826 C823 C836 132.1(7) . . ? N12 C823 C836 120.8(6) . . ? C893 C824 C842 119.5(8) . . ? C893 C824 N10 117.2(7) . . ? C842 C824 N10 123.1(8) . . ? C823 C826 N11 106.6(6) . . ? C823 C826 C843 125.6(7) . . ? N11 C826 C843 127.8(6) . . ? N13 C835 N12 112.0(6) . . ? N13 C835 H83B 109.2 . . ? N12 C835 H83B 109.2 . . ? N13 C835 H83C 109.2 . . ? N12 C835 H83C 109.2 . . ? H83B C835 H83C 107.9 . . ? C823 C836 H83D 109.5 . . ? C823 C836 H83E 109.5 . . ? H83D C836 H83E 109.5 . . ? C823 C836 H83F 109.5 . . ? H83D C836 H83F 109.5 . . ? H83E C836 H83F 109.5 . . ? N11 C838 N12 101.2(6) . . ? N11 C838 Ni2 144.1(5) . . ? N12 C838 Ni2 114.3(5) . . ? C920 C842 C824 116.8(9) . . ? C920 C842 C857 121.8(8) . . ? C824 C842 C857 121.3(8) . . ? C826 C843 H84C 109.5 . . ? C826 C843 H84D 109.5 . . ? H84C C843 H84D 109.5 . . ? C826 C843 H84E 109.5 . . ? H84C C843 H84E 109.5 . . ? H84D C843 H84E 109.5 . . ? C873 C854 N14 105.5(8) . . ? C873 C854 C906 129.8(9) . . ? N14 C854 C906 124.6(9) . . ? C842 C857 C917 110.4(7) . . ? C842 C857 C902 110.7(8) . . ? C917 C857 C902 109.3(7) . . ? C842 C857 H85I 108.8 . . ? C917 C857 H85I 108.8 . . ? C902 C857 H85I 108.8 . . ? C915 C862 C895 110.9(8) . . ? C915 C862 N11 108.2(9) . . ? C895 C862 N11 110.6(6) . . ? C915 C862 C916 115.8(9) . . ? C895 C862 C916 104.7(8) . . ? N11 C862 C916 106.5(7) . . ? C870 C869 C920 118.0(8) . . ? C870 C869 H86R 121.0 . . ? C920 C869 H86R 121.0 . . ? C869 C870 C893 119.9(9) . . ? C869 C870 H87A 120.0 . . ? C893 C870 H87A 120.0 . . ? C854 C873 N13 107.7(8) . . ? C854 C873 C905 130.4(8) . . ? N13 C873 C905 121.9(8) . . ? N14 C881 C899 109.6(7) . . ? N14 C881 C901 112.2(7) . . ? C899 C881 C901 108.8(8) . . ? N14 C881 C904 109.1(7) . . ? C899 C881 C904 112.2(8) . . ? C901 C881 C904 105.0(7) . . ? C870 C893 C824 121.7(8) . . ? C870 C893 C910 118.7(9) . . ? C824 C893 C910 119.6(8) . . ? C862 C895 H89M 109.5 . . ? C862 C895 H89N 109.5 . . ? H89M C895 H89N 109.5 . . ? C862 C895 H89O 109.5 . . ? H89M C895 H89O 109.5 . . ? H89N C895 H89O 109.5 . . ? C881 C899 H8A 109.5 . . ? C881 C899 H89Y 109.5 . . ? H8A C899 H89Y 109.5 . . ? C881 C899 H89Z 109.5 . . ? H8A C899 H89Z 109.5 . . ? H89Y C899 H89Z 109.5 . . ? C881 C901 H90A 109.5 . . ? C881 C901 H90B 109.5 . . ? H90A C901 H90B 109.5 . . ? C881 C901 H90C 109.5 . . ? H90A C901 H90C 109.5 . . ? H90B C901 H90C 109.5 . . ? C857 C902 H90D 109.5 . . ? C857 C902 H90E 109.5 . . ? H90D C902 H90E 109.5 . . ? C857 C902 H90F 109.5 . . ? H90D C902 H90F 109.5 . . ? H90E C902 H90F 109.5 . . ? C881 C904 H90J 109.5 . . ? C881 C904 H90K 109.5 . . ? H90J C904 H90K 109.5 . . ? C881 C904 H90L 109.5 . . ? H90J C904 H90L 109.5 . . ? H90K C904 H90L 109.5 . . ? C873 C905 H90M 109.5 . . ? C873 C905 H90N 109.5 . . ? H90M C905 H90N 109.5 . . ? C873 C905 H90O 109.5 . . ? H90M C905 H90O 109.5 . . ? H90N C905 H90O 109.5 . . ? C854 C906 H90P 109.5 . . ? C854 C906 H90Q 109.5 . . ? H90P C906 H90Q 109.5 . . ? C854 C906 H90R 109.5 . . ? H90P C906 H90R 109.5 . . ? H90Q C906 H90R 109.5 . . ? C993 C910 C893 112.3(9) . . ? C993 C910 C999 112.6(10) . . ? C893 C910 C999 107.2(10) . . ? C993 C910 H91E 108.2 . . ? C893 C910 H91E 108.2 . . ? C999 C910 H91E 108.2 . . ? C862 C915 H91U 109.5 . . ? C862 C915 H91V 109.5 . . ? H91U C915 H91V 109.5 . . ? C862 C915 H91W 109.5 . . ? H91U C915 H91W 109.5 . . ? H91V C915 H91W 109.5 . . ? C862 C916 H91X 109.5 . . ? C862 C916 H91Y 109.5 . . ? H91X C916 H91Y 109.5 . . ? C862 C916 H91Z 109.5 . . ? H91X C916 H91Z 109.5 . . ? H91Y C916 H91Z 109.5 . . ? C857 C917 H92A 109.5 . . ? C857 C917 H92B 109.5 . . ? H92A C917 H92B 109.5 . . ? C857 C917 H92C 109.5 . . ? H92A C917 H92C 109.5 . . ? H92B C917 H92C 109.5 . . ? C842 C920 C869 124.1(8) . . ? C842 C920 H88S 118.0 . . ? C869 C920 H88S 118.0 . . ? C910 C993 H99M 109.5 . . ? C910 C993 H99N 109.5 . . ? H99M C993 H99N 109.5 . . ? C910 C993 H99O 109.5 . . ? H99M C993 H99O 109.5 . . ? H99N C993 H99O 109.5 . . ? C910 C999 H99J 109.5 . . ? C910 C999 H99K 109.5 . . ? H99J C999 H99K 109.5 . . ? C910 C999 H99L 109.5 . . ? H99J C999 H99L 109.5 . . ? H99K C999 H99L 109.5 . . ? N16 Ni3 N15 38.8(2) . . ? N16 Ni3 C820 145.7(3) . . ? N15 Ni3 C820 108.9(3) . . ? N16 Ni3 C817 119.7(3) . . ? N15 Ni3 C817 157.7(3) . . ? C820 Ni3 C817 90.3(3) . . ? N16 N15 Ni3 68.4(4) . . ? N15 N16 N17 127.4(6) . . ? N15 N16 Ni3 72.9(4) . . ? N17 N16 Ni3 159.3(5) . . ? N16 N17 C818 113.0(5) . . ? C820 N18 C888 109.4(7) . . ? C820 N18 C865 119.1(6) . . ? C888 N18 C865 131.2(7) . . ? C820 N19 C858 113.0(7) . . ? C820 N19 C815 120.1(6) . . ? C858 N19 C815 126.9(7) . . ? C810 N20 C817 111.5(5) . . ? C810 N20 C815 128.1(6) . . ? C817 N20 C815 120.3(6) . . ? C817 N21 C811 110.5(6) . . ? C817 N21 C833 123.7(6) . . ? C811 N21 C833 125.8(5) . . ? C856 C805 C818 118.1(7) . . ? C856 C805 C846 122.1(7) . . ? C818 C805 C846 119.8(7) . . ? C811 C810 N20 106.9(6) . . ? C811 C810 C864 131.7(6) . . ? N20 C810 C864 121.5(6) . . ? C810 C811 N21 108.0(6) . . ? C810 C811 C850 126.9(6) . . ? N21 C811 C850 125.1(6) . . ? C840 C812 C818 120.8(7) . . ? C840 C812 C845 120.6(6) . . ? C818 C812 C845 118.6(6) . . ? N19 C815 N20 109.5(6) . . ? N19 C815 H81C 109.8 . . ? N20 C815 H81C 109.8 . . ? N19 C815 H81D 109.8 . . ? N20 C815 H81D 109.8 . . ? H81C C815 H81D 108.2 . . ? N21 C817 N20 103.1(6) . . ? N21 C817 Ni3 143.6(5) . . ? N20 C817 Ni3 113.4(4) . . ? C812 C818 C805 119.0(7) . . ? C812 C818 N17 125.8(6) . . ? C805 C818 N17 114.6(6) . . ? N19 C820 N18 103.5(6) . . ? N19 C820 Ni3 115.6(6) . . ? N18 C820 Ni3 140.8(6) . . ? C882 C833 C861 109.1(7) . . ? C882 C833 N21 111.1(6) . . ? C861 C833 N21 107.3(5) . . ? C882 C833 C868 112.1(6) . . ? C861 C833 C868 109.3(6) . . ? N21 C833 C868 107.8(6) . . ? C844 C840 C812 119.3(7) . . ? C844 C840 H84A 120.3 . . ? C812 C840 H84A 120.3 . . ? C856 C844 C840 120.7(7) . . ? C856 C844 H84F 119.7 . . ? C840 C844 H84F 119.7 . . ? C892 C845 C887 110.5(7) . . ? C892 C845 C812 113.8(6) . . ? C887 C845 C812 112.0(6) . . ? C892 C845 H84G 106.7 . . ? C887 C845 H84G 106.7 . . ? C812 C845 H84G 106.7 . . ? C991 C846 C990 109.2(7) . . ? C991 C846 C805 116.6(7) . . ? C990 C846 C805 111.8(6) . . ? C991 C846 H84H 106.2 . . ? C990 C846 H84H 106.2 . . ? C805 C846 H84H 106.2 . . ? C811 C850 H85A 109.5 . . ? C811 C850 H85B 109.5 . . ? H85A C850 H85B 109.5 . . ? C811 C850 H85C 109.5 . . ? H85A C850 H85C 109.5 . . ? H85B C850 H85C 109.5 . . ? C844 C856 C805 122.0(7) . . ? C844 C856 H85H 119.0 . . ? C805 C856 H85H 119.0 . . ? C888 C858 N19 106.4(7) . . ? C888 C858 C890 133.6(8) . . ? N19 C858 C890 119.9(8) . . ? C833 C861 H86B 109.5 . . ? C833 C861 H86C 109.5 . . ? H86B C861 H86C 109.5 . . ? C833 C861 H86D 109.5 . . ? H86B C861 H86D 109.5 . . ? H86C C861 H86D 109.5 . . ? C810 C864 H86H 109.5 . . ? C810 C864 H86I 109.5 . . ? H86H C864 H86I 109.5 . . ? C810 C864 H86J 109.5 . . ? H86H C864 H86J 109.5 . . ? H86I C864 H86J 109.5 . . ? N18 C865 C876 109.8(6) . . ? N18 C865 C872 108.6(7) . . ? C876 C865 C872 110.3(6) . . ? N18 C865 C913 113.4(7) . . ? C876 C865 C913 106.7(7) . . ? C872 C865 C913 108.0(6) . . ? C833 C868 H86O 109.5 . . ? C833 C868 H86P 109.5 . . ? H86O C868 H86P 109.5 . . ? C833 C868 H86Q 109.5 . . ? H86O C868 H86Q 109.5 . . ? H86P C868 H86Q 109.5 . . ? C865 C872 H87E 109.5 . . ? C865 C872 H87F 109.5 . . ? H87E C872 H87F 109.5 . . ? C865 C872 H87G 109.5 . . ? H87E C872 H87G 109.5 . . ? H87F C872 H87G 109.5 . . ? C865 C876 H87K 109.5 . . ? C865 C876 H87L 109.5 . . ? H87K C876 H87L 109.5 . . ? C865 C876 H87M 109.5 . . ? H87K C876 H87M 109.5 . . ? H87L C876 H87M 109.5 . . ? C833 C882 H88A 109.5 . . ? C833 C882 H88B 109.5 . . ? H88A C882 H88B 109.5 . . ? C833 C882 H88C 109.5 . . ? H88A C882 H88C 109.5 . . ? H88B C882 H88C 109.5 . . ? C845 C887 H88P 109.5 . . ? C845 C887 H88Q 109.5 . . ? H88P C887 H88Q 109.5 . . ? C845 C887 H88R 109.5 . . ? H88P C887 H88R 109.5 . . ? H88Q C887 H88R 109.5 . . ? C858 C888 N18 107.5(7) . . ? C858 C888 C912 124.2(8) . . ? N18 C888 C912 128.2(9) . . ? C858 C890 H89A 109.5 . . ? C858 C890 H89B 109.5 . . ? H89A C890 H89B 109.5 . . ? C858 C890 H89C 109.5 . . ? H89A C890 H89C 109.5 . . ? H89B C890 H89C 109.5 . . ? C845 C892 H89G 109.5 . . ? C845 C892 H89H 109.5 . . ? H89G C892 H89H 109.5 . . ? C845 C892 H89I 109.5 . . ? H89G C892 H89I 109.5 . . ? H89H C892 H89I 109.5 . . ? C888 C912 H91I 109.5 . . ? C888 C912 H91J 109.5 . . ? H91I C912 H91J 109.5 . . ? C888 C912 H91K 109.5 . . ? H91I C912 H91K 109.5 . . ? H91J C912 H91K 109.5 . . ? C865 C913 H91L 109.5 . . ? C865 C913 H91M 109.5 . . ? H91L C913 H91M 109.5 . . ? C865 C913 H91N 109.5 . . ? H91L C913 H91N 109.5 . . ? H91M C913 H91N 109.5 . . ? C846 C990 H99S 109.5 . . ? C846 C990 H99T 109.5 . . ? H99S C990 H99T 109.5 . . ? C846 C990 H99U 109.5 . . ? H99S C990 H99U 109.5 . . ? H99T C990 H99U 109.5 . . ? C846 C991 H99V 109.5 . . ? C846 C991 H99W 109.5 . . ? H99V C991 H99W 109.5 . . ? C846 C991 H99X 109.5 . . ? H99V C991 H99X 109.5 . . ? H99W C991 H99X 109.5 . . ? N27 Ni4 N26 39.1(2) . . ? N27 Ni4 C825 144.8(3) . . ? N26 Ni4 C825 106.4(3) . . ? N27 Ni4 C802 122.1(3) . . ? N26 Ni4 C802 159.9(3) . . ? C825 Ni4 C802 90.6(3) . . ? C827 N22 C802 113.0(5) . . ? C827 N22 C829 125.3(6) . . ? C802 N22 C829 121.7(6) . . ? C802 N23 C819 112.9(6) . . ? C802 N23 C804 119.6(5) . . ? C819 N23 C804 127.3(6) . . ? C825 N24 C849 112.9(6) . . ? C825 N24 C804 120.0(6) . . ? C849 N24 C804 127.0(6) . . ? C825 N25 C828 111.2(6) . . ? C825 N25 C853 120.0(7) . . ? C828 N25 C853 128.6(7) . . ? N27 N26 Ni4 68.4(4) . . ? N26 N27 N28 129.3(6) . . ? N26 N27 Ni4 72.5(4) . . ? N28 N27 Ni4 158.0(6) . . ? N27 N28 C803 115.3(6) . . ? C803 C801 C813 115.5(7) . . ? C803 C801 C822 123.2(7) . . ? C813 C801 C822 121.0(7) . . ? N23 C802 N22 101.5(5) . . ? N23 C802 Ni4 114.4(5) . . ? N22 C802 Ni4 144.1(5) . . ? C889 C803 C801 121.5(7) . . ? C889 C803 N28 116.4(6) . . ? C801 C803 N28 121.7(7) . . ? N24 C804 N23 108.9(5) . . ? N24 C804 H80A 109.9 . . ? N23 C804 H80A 109.9 . . ? N24 C804 H80B 109.9 . . ? N23 C804 H80B 109.9 . . ? H80A C804 H80B 108.3 . . ? C855 C813 C801 122.6(7) . . ? C855 C813 H81A 118.7 . . ? C801 C813 H81A 118.7 . . ? C998 C814 C994 107.0(11) . . ? C998 C814 C889 110.0(8) . . ? C994 C814 C889 113.1(8) . . ? C998 C814 H81B 108.9 . . ? C994 C814 H81B 108.9 . . ? C889 C814 H81B 108.9 . . ? C827 C819 N23 106.5(6) . . ? C827 C819 C851 131.8(7) . . ? N23 C819 C851 121.6(6) . . ? C801 C822 C859 109.6(6) . . ? C801 C822 C884 112.7(6) . . ? C859 C822 C884 108.6(6) . . ? C801 C822 H82A 108.6 . . ? C859 C822 H82A 108.6 . . ? C884 C822 H82A 108.6 . . ? N25 C825 N24 102.6(6) . . ? N25 C825 Ni4 143.3(6) . . ? N24 C825 Ni4 114.2(5) . . ? C819 C827 N22 106.1(6) . . ? C819 C827 C871 124.9(6) . . ? N22 C827 C871 128.9(7) . . ? C849 C828 N25 108.3(7) . . ? C849 C828 C886 125.4(7) . . ? N25 C828 C886 126.3(7) . . ? C903 C829 C919 112.5(7) . . ? C903 C829 N22 106.2(7) . . ? C919 C829 N22 110.4(7) . . ? C903 C829 C863 105.4(7) . . ? C919 C829 C863 110.5(8) . . ? N22 C829 C863 111.7(6) . . ? C828 C849 N24 105.0(6) . . ? C828 C849 C879 133.6(8) . . ? N24 C849 C879 121.4(7) . . ? C819 C851 H85D 109.5 . . ? C819 C851 H85E 109.5 . . ? H85D C851 H85E 109.5 . . ? C819 C851 H85F 109.5 . . ? H85D C851 H85F 109.5 . . ? H85E C851 H85F 109.5 . . ? C918 C853 C894 107.3(8) . . ? C918 C853 N25 106.7(7) . . ? C894 C853 N25 111.5(7) . . ? C918 C853 C909 114.5(9) . . ? C894 C853 C909 106.4(8) . . ? N25 C853 C909 110.4(7) . . ? C813 C855 C867 119.1(8) . . ? C813 C855 H85G 120.4 . . ? C867 C855 H85G 120.4 . . ? C822 C859 H85J 109.5 . . ? C822 C859 H85K 109.5 . . ? H85J C859 H85K 109.5 . . ? C822 C859 H85L 109.5 . . ? H85J C859 H85L 109.5 . . ? H85K C859 H85L 109.5 . . ? C829 C863 H86E 109.5 . . ? C829 C863 H86F 109.5 . . ? H86E C863 H86F 109.5 . . ? C829 C863 H86G 109.5 . . ? H86E C863 H86G 109.5 . . ? H86F C863 H86G 109.5 . . ? C889 C867 C855 121.7(8) . . ? C889 C867 H86N 119.1 . . ? C855 C867 H86N 119.1 . . ? C827 C871 H87B 109.5 . . ? C827 C871 H87C 109.5 . . ? H87B C871 H87C 109.5 . . ? C827 C871 H87D 109.5 . . ? H87B C871 H87D 109.5 . . ? H87C C871 H87D 109.5 . . ? C849 C879 H87R 109.5 . . ? C849 C879 H87S 109.5 . . ? H87R C879 H87S 109.5 . . ? C849 C879 H87T 109.5 . . ? H87R C879 H87T 109.5 . . ? H87S C879 H87T 109.5 . . ? C822 C884 H88G 109.5 . . ? C822 C884 H88H 109.5 . . ? H88G C884 H88H 109.5 . . ? C822 C884 H88I 109.5 . . ? H88G C884 H88I 109.5 . . ? H88H C884 H88I 109.5 . . ? C828 C886 H88M 109.5 . . ? C828 C886 H88N 109.5 . . ? H88M C886 H88N 109.5 . . ? C828 C886 H88O 109.5 . . ? H88M C886 H88O 109.5 . . ? H88N C886 H88O 109.5 . . ? C867 C889 C803 119.3(7) . . ? C867 C889 C814 122.0(7) . . ? C803 C889 C814 118.7(7) . . ? C853 C894 H89J 109.5 . . ? C853 C894 H89K 109.5 . . ? H89J C894 H89K 109.5 . . ? C853 C894 H89L 109.5 . . ? H89J C894 H89L 109.5 . . ? H89K C894 H89L 109.5 . . ? C829 C903 H90G 109.5 . . ? C829 C903 H90H 109.5 . . ? H90G C903 H90H 109.5 . . ? C829 C903 H90I 109.5 . . ? H90G C903 H90I 109.5 . . ? H90H C903 H90I 109.5 . . ? C853 C909 H90Y 109.5 . . ? C853 C909 H90Z 109.5 . . ? H90Y C909 H90Z 109.5 . . ? C853 C909 H91D 109.5 . . ? H90Y C909 H91D 109.5 . . ? H90Z C909 H91D 109.5 . . ? C853 C918 H92D 109.5 . . ? C853 C918 H92E 109.5 . . ? H92D C918 H92E 109.5 . . ? C853 C918 H92F 109.5 . . ? H92D C918 H92F 109.5 . . ? H92E C918 H92F 109.5 . . ? C829 C919 H92G 109.5 . . ? C829 C919 H92H 109.5 . . ? H92G C919 H92H 109.5 . . ? C829 C919 H92I 109.5 . . ? H92G C919 H92I 109.5 . . ? H92H C919 H92I 109.5 . . ? C814 C994 H99P 109.5 . . ? C814 C994 H99Q 109.5 . . ? H99P C994 H99Q 109.5 . . ? C814 C994 H99R 109.5 . . ? H99P C994 H99R 109.5 . . ? H99Q C994 H99R 109.5 . . ? C814 C998 H99G 109.5 . . ? C814 C998 H99H 109.5 . . ? H99G C998 H99H 109.5 . . ? C814 C998 H99I 109.5 . . ? H99G C998 H99I 109.5 . . ? H99H C998 H99I 109.5 . . ? N34 Ni5 C800 144.4(3) . . ? N34 Ni5 N33 39.1(2) . . ? C800 Ni5 N33 107.6(3) . . ? N34 Ni5 C809 120.4(3) . . ? C800 Ni5 C809 91.1(3) . . ? N33 Ni5 C809 159.2(3) . . ? C800 N29 C847 109.9(7) . . ? C800 N29 C880 122.6(6) . . ? C847 N29 C880 127.5(7) . . ? C800 N30 C831 113.6(6) . . ? C800 N30 C806 118.9(6) . . ? C831 N30 C806 127.4(6) . . ? C809 N31 C807 113.2(6) . . ? C809 N31 C806 119.4(6) . . ? C807 N31 C806 127.3(6) . . ? C809 N32 C834 112.7(6) . . ? C809 N32 C837 122.7(6) . . ? C834 N32 C837 124.6(6) . . ? N34 N33 Ni5 66.8(4) . . ? N33 N34 N35 128.3(6) . . ? N33 N34 Ni5 74.0(4) . . ? N35 N34 Ni5 157.5(5) . . ? N34 N35 C830 116.0(6) . . ? N30 C800 N29 102.3(6) . . ? N30 C800 Ni5 115.9(5) . . ? N29 C800 Ni5 141.5(6) . . ? N30 C806 N31 109.0(5) . . ? N30 C806 H80C 109.9 . . ? N31 C806 H80C 109.9 . . ? N30 C806 H80D 109.9 . . ? N31 C806 H80D 109.9 . . ? H80C C806 H80D 108.3 . . ? C834 C807 N31 105.2(6) . . ? C834 C807 C878 132.6(7) . . ? N31 C807 C878 122.1(6) . . ? N32 C809 N31 102.2(6) . . ? N32 C809 Ni5 143.3(5) . . ? N31 C809 Ni5 114.4(5) . . ? C860 C816 C830 119.8(8) . . ? C860 C816 C839 121.4(7) . . ? C830 C816 C839 118.8(7) . . ? C930 C821 C830 118.2(7) . . ? C930 C821 C832 122.1(7) . . ? C830 C821 C832 118.9(7) . . ? C816 C830 N35 116.2(7) . . ? C816 C830 C821 118.9(7) . . ? N35 C830 C821 124.7(6) . . ? C847 C831 N30 105.5(7) . . ? C847 C831 C866 131.7(8) . . ? N30 C831 C866 122.8(8) . . ? C896 C832 C875 106.2(6) . . ? C896 C832 C821 114.3(6) . . ? C875 C832 C821 112.9(7) . . ? C896 C832 H83A 107.7 . . ? C875 C832 H83A 107.7 . . ? C821 C832 H83A 107.7 . . ? C807 C834 N32 106.6(7) . . ? C807 C834 C883 125.3(7) . . ? N32 C834 C883 128.1(7) . . ? C891 C837 C885 108.1(7) . . ? C891 C837 N32 109.5(6) . . ? C885 C837 N32 109.7(6) . . ? C891 C837 C897 111.7(7) . . ? C885 C837 C897 107.7(7) . . ? N32 C837 C897 110.1(6) . . ? C997 C839 C996 113.5(7) . . ? C997 C839 C816 112.3(7) . . ? C996 C839 C816 111.8(6) . . ? C997 C839 H83G 106.2 . . ? C996 C839 H83G 106.2 . . ? C816 C839 H83G 106.2 . . ? C831 C847 N29 108.7(7) . . ? C831 C847 C898 125.6(8) . . ? N29 C847 C898 125.6(8) . . ? C877 C860 C816 120.0(8) . . ? C877 C860 H86A 120.0 . . ? C816 C860 H86A 120.0 . . ? C831 C866 H86K 109.5 . . ? C831 C866 H86L 109.5 . . ? H86K C866 H86L 109.5 . . ? C831 C866 H86M 109.5 . . ? H86K C866 H86M 109.5 . . ? H86L C866 H86M 109.5 . . ? C832 C875 H87H 109.5 . . ? C832 C875 H87I 109.5 . . ? H87H C875 H87I 109.5 . . ? C832 C875 H87J 109.5 . . ? H87H C875 H87J 109.5 . . ? H87I C875 H87J 109.5 . . ? C860 C877 C930 119.6(8) . . ? C860 C877 H87N 120.2 . . ? C930 C877 H87N 120.2 . . ? C807 C878 H87O 109.5 . . ? C807 C878 H87P 109.5 . . ? H87O C878 H87P 109.5 . . ? C807 C878 H87Q 109.5 . . ? H87O C878 H87Q 109.5 . . ? H87P C878 H87Q 109.5 . . ? N29 C880 C914 110.2(8) . . ? N29 C880 C907 110.7(7) . . ? C914 C880 C907 108.3(8) . . ? N29 C880 C908 112.1(7) . . ? C914 C880 C908 110.0(9) . . ? C907 C880 C908 105.4(8) . . ? C834 C883 H88D 109.5 . . ? C834 C883 H88E 109.5 . . ? H88D C883 H88E 109.5 . . ? C834 C883 H88F 109.5 . . ? H88D C883 H88F 109.5 . . ? H88E C883 H88F 109.5 . . ? C837 C885 H88J 109.5 . . ? C837 C885 H88K 109.5 . . ? H88J C885 H88K 109.5 . . ? C837 C885 H88L 109.5 . . ? H88J C885 H88L 109.5 . . ? H88K C885 H88L 109.5 . . ? C837 C891 H89D 109.5 . . ? C837 C891 H89E 109.5 . . ? H89D C891 H89E 109.5 . . ? C837 C891 H89F 109.5 . . ? H89D C891 H89F 109.5 . . ? H89E C891 H89F 109.5 . . ? C832 C896 H89P 109.5 . . ? C832 C896 H89Q 109.5 . . ? H89P C896 H89Q 109.5 . . ? C832 C896 H89R 109.5 . . ? H89P C896 H89R 109.5 . . ? H89Q C896 H89R 109.5 . . ? C837 C897 H89S 109.5 . . ? C837 C897 H89T 109.5 . . ? H89S C897 H89T 109.5 . . ? C837 C897 H89U 109.5 . . ? H89S C897 H89U 109.5 . . ? H89T C897 H89U 109.5 . . ? C847 C898 H89V 109.5 . . ? C847 C898 H89W 109.5 . . ? H89V C898 H89W 109.5 . . ? C847 C898 H89X 109.5 . . ? H89V C898 H89X 109.5 . . ? H89W C898 H89X 109.5 . . ? C880 C907 H90S 109.5 . . ? C880 C907 H90T 109.5 . . ? H90S C907 H90T 109.5 . . ? C880 C907 H90U 109.5 . . ? H90S C907 H90U 109.5 . . ? H90T C907 H90U 109.5 . . ? C880 C908 H90V 109.5 . . ? C880 C908 H90W 109.5 . . ? H90V C908 H90W 109.5 . . ? C880 C908 H90X 109.5 . . ? H90V C908 H90X 109.5 . . ? H90W C908 H90X 109.5 . . ? C880 C914 H91O 109.5 . . ? C880 C914 H91P 109.5 . . ? H91O C914 H91P 109.5 . . ? C880 C914 H91Q 109.5 . . ? H91O C914 H91Q 109.5 . . ? H91P C914 H91Q 109.5 . . ? C821 C930 C877 123.5(8) . . ? C821 C930 H93A 118.3 . . ? C877 C930 H93A 118.3 . . ? C839 C996 H99A 109.5 . . ? C839 C996 H99B 109.5 . . ? H99A C996 H99B 109.5 . . ? C839 C996 H99C 109.5 . . ? H99A C996 H99C 109.5 . . ? H99B C996 H99C 109.5 . . ? C839 C997 H99D 109.5 . . ? C839 C997 H99E 109.5 . . ? H99D C997 H99E 109.5 . . ? C839 C997 H99F 109.5 . . ? H99D C997 H99F 109.5 . . ? H99E C997 H99F 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 C1 Ni1 N1 N2 10.5(9) . . . . ? C2 Ni1 N1 N2 166.1(4) . . . . ? Ni1 N1 N2 N3 -175.7(8) . . . . ? C1 Ni1 N2 N1 -175.0(4) . . . . ? C2 Ni1 N2 N1 -26.1(8) . . . . ? C1 Ni1 N2 N3 -2.6(13) . . . . ? N1 Ni1 N2 N3 172.4(15) . . . . ? C2 Ni1 N2 N3 146.3(11) . . . . ? N1 N2 N3 C80 169.3(7) . . . . ? Ni1 N2 N3 C80 -0.9(15) . . . . ? C4 N6 C1 N7 2.1(9) . . . . ? C7 N6 C1 N7 -173.4(7) . . . . ? C4 N6 C1 Ni1 -177.5(6) . . . . ? C7 N6 C1 Ni1 7.0(10) . . . . ? C3 N7 C1 N6 -2.5(9) . . . . ? C701 N7 C1 N6 170.1(7) . . . . ? C3 N7 C1 Ni1 176.9(8) . . . . ? C701 N7 C1 Ni1 -10.6(15) . . . . ? N2 Ni1 C1 N6 111.6(6) . . . . ? N1 Ni1 C1 N6 104.3(8) . . . . ? C2 Ni1 C1 N6 -53.2(6) . . . . ? N2 Ni1 C1 N7 -67.6(12) . . . . ? N1 Ni1 C1 N7 -75.0(14) . . . . ? C2 Ni1 C1 N7 127.5(11) . . . . ? C6 N4 C2 N5 0.9(9) . . . . ? C401 N4 C2 N5 175.4(7) . . . . ? C6 N4 C2 Ni1 -170.0(9) . . . . ? C401 N4 C2 Ni1 4.4(16) . . . . ? C5 N5 C2 N4 -1.2(9) . . . . ? C7 N5 C2 N4 178.6(6) . . . . ? C5 N5 C2 Ni1 173.3(5) . . . . ? C7 N5 C2 Ni1 -6.9(9) . . . . ? N2 Ni1 C2 N4 69.6(13) . . . . ? C1 Ni1 C2 N4 -138.2(11) . . . . ? N1 Ni1 C2 N4 52.1(12) . . . . ? N2 Ni1 C2 N5 -100.9(7) . . . . ? C1 Ni1 C2 N5 51.3(6) . . . . ? N1 Ni1 C2 N5 -118.4(5) . . . . ? C1 N7 C3 C4 1.9(10) . . . . ? C701 N7 C3 C4 -170.4(7) . . . . ? C1 N7 C3 C30 -175.8(9) . . . . ? C701 N7 C3 C30 11.9(13) . . . . ? N7 C3 C4 N6 -0.5(9) . . . . ? C30 C3 C4 N6 177.2(8) . . . . ? N7 C3 C4 C40 -178.5(8) . . . . ? C30 C3 C4 C40 -0.8(16) . . . . ? C1 N6 C4 C3 -1.1(10) . . . . ? C7 N6 C4 C3 174.1(7) . . . . ? C1 N6 C4 C40 177.3(7) . . . . ? C7 N6 C4 C40 -7.6(12) . . . . ? C2 N5 C5 C6 1.0(10) . . . . ? C7 N5 C5 C6 -178.8(7) . . . . ? C2 N5 C5 C50 -178.1(7) . . . . ? C7 N5 C5 C50 2.1(13) . . . . ? N5 C5 C6 N4 -0.4(9) . . . . ? C50 C5 C6 N4 178.6(9) . . . . ? N5 C5 C6 C60 179.7(8) . . . . ? C50 C5 C6 C60 -1.3(16) . . . . ? C2 N4 C6 C5 -0.4(10) . . . . ? C401 N4 C6 C5 -174.4(8) . . . . ? C2 N4 C6 C60 179.5(9) . . . . ? C401 N4 C6 C60 5.5(15) . . . . ? C1 N6 C7 N5 52.1(10) . . . . ? C4 N6 C7 N5 -122.6(8) . . . . ? C2 N5 C7 N6 -51.8(9) . . . . ? C5 N5 C7 N6 128.0(8) . . . . ? N2 N3 C80 C85 -66.2(11) . . . . ? N2 N3 C80 C81 118.4(8) . . . . ? C85 C80 C81 C82 -0.7(13) . . . . ? N3 C80 C81 C82 175.1(8) . . . . ? C85 C80 C81 C841 -174.0(8) . . . . ? N3 C80 C81 C841 1.8(12) . . . . ? C80 C81 C82 C83 2.6(14) . . . . ? C841 C81 C82 C83 175.8(8) . . . . ? C81 C82 C83 C84 -3.4(14) . . . . ? C82 C83 C84 C85 2.3(15) . . . . ? C83 C84 C85 C80 -0.4(15) . . . . ? C83 C84 C85 C89 -171.0(9) . . . . ? N3 C80 C85 C84 -175.8(8) . . . . ? C81 C80 C85 C84 -0.5(13) . . . . ? N3 C80 C85 C89 -4.9(13) . . . . ? C81 C80 C85 C89 170.5(8) . . . . ? C84 C85 C89 C90 -29.8(12) . . . . ? C80 C85 C89 C90 159.3(8) . . . . ? C84 C85 C89 C91 92.6(10) . . . . ? C80 C85 C89 C91 -78.2(9) . . . . ? C2 N4 C401 C404 -84.1(10) . . . . ? C6 N4 C401 C404 89.6(11) . . . . ? C2 N4 C401 C402 30.1(12) . . . . ? C6 N4 C401 C402 -156.1(9) . . . . ? C2 N4 C401 C911 149.9(8) . . . . ? C6 N4 C401 C911 -36.4(13) . . . . ? C1 N7 C701 C702 13.9(11) . . . . ? C3 N7 C701 C702 -174.5(7) . . . . ? C1 N7 C701 C704 132.6(8) . . . . ? C3 N7 C701 C704 -55.7(11) . . . . ? C1 N7 C701 C703 -104.8(9) . . . . ? C3 N7 C701 C703 66.9(10) . . . . ? C82 C81 C841 C88 -89.6(10) . . . . ? C80 C81 C841 C88 83.7(9) . . . . ? C82 C81 C841 C87 36.1(12) . . . . ? C80 C81 C841 C87 -150.6(8) . . . . ? C838 Ni2 N8 N9 -171.6(4) . . . . ? C808 Ni2 N8 N9 -15.8(10) . . . . ? Ni2 N8 N9 N10 -179.7(8) . . . . ? C838 Ni2 N9 N8 14.9(7) . . . . ? C808 Ni2 N9 N8 173.1(4) . . . . ? C838 Ni2 N9 N10 -165.7(11) . . . . ? N8 Ni2 N9 N10 179(100) . . . . ? C808 Ni2 N9 N10 -7.5(14) . . . . ? N8 N9 N10 C824 -173.3(8) . . . . ? Ni2 N9 N10 C824 7.5(17) . . . . ? C873 N13 C808 N14 1.4(8) . . . . ? C835 N13 C808 N14 177.5(6) . . . . ? C873 N13 C808 Ni2 178.7(5) . . . . ? C835 N13 C808 Ni2 -5.3(8) . . . . ? C854 N14 C808 N13 -1.5(8) . . . . ? C881 N14 C808 N13 -179.1(6) . . . . ? C854 N14 C808 Ni2 -177.3(7) . . . . ? C881 N14 C808 Ni2 5.1(13) . . . . ? N9 Ni2 C808 N13 -117.0(5) . . . . ? C838 Ni2 C808 N13 51.6(5) . . . . ? N8 Ni2 C808 N13 -105.8(9) . . . . ? N9 Ni2 C808 N14 58.5(10) . . . . ? C838 Ni2 C808 N14 -132.9(9) . . . . ? N8 Ni2 C808 N14 69.7(13) . . . . ? C838 N12 C823 C826 4.4(9) . . . . ? C835 N12 C823 C826 176.6(7) . . . . ? C838 N12 C823 C836 -175.9(7) . . . . ? C835 N12 C823 C836 -3.6(11) . . . . ? N9 N10 C824 C893 -124.5(8) . . . . ? N9 N10 C824 C842 61.5(10) . . . . ? N12 C823 C826 N11 -2.9(8) . . . . ? C836 C823 C826 N11 177.4(7) . . . . ? N12 C823 C826 C843 177.3(7) . . . . ? C836 C823 C826 C843 -2.4(14) . . . . ? C838 N11 C826 C823 0.6(9) . . . . ? C862 N11 C826 C823 -171.5(8) . . . . ? C838 N11 C826 C843 -179.6(7) . . . . ? C862 N11 C826 C843 8.3(12) . . . . ? C808 N13 C835 N12 -54.6(8) . . . . ? C873 N13 C835 N12 120.8(7) . . . . ? C838 N12 C835 N13 52.7(8) . . . . ? C823 N12 C835 N13 -119.2(8) . . . . ? C826 N11 C838 N12 1.9(8) . . . . ? C862 N11 C838 N12 174.3(7) . . . . ? C826 N11 C838 Ni2 173.5(8) . . . . ? C862 N11 C838 Ni2 -14.2(14) . . . . ? C823 N12 C838 N11 -3.8(8) . . . . ? C835 N12 C838 N11 -177.0(6) . . . . ? C823 N12 C838 Ni2 -178.4(5) . . . . ? C835 N12 C838 Ni2 8.4(8) . . . . ? N9 Ni2 C838 N11 -61.6(12) . . . . ? N8 Ni2 C838 N11 -51.8(11) . . . . ? C808 Ni2 C838 N11 137.1(10) . . . . ? N9 Ni2 C838 N12 109.3(6) . . . . ? N8 Ni2 C838 N12 119.1(6) . . . . ? C808 Ni2 C838 N12 -52.0(6) . . . . ? C893 C824 C842 C920 -0.2(12) . . . . ? N10 C824 C842 C920 173.7(7) . . . . ? C893 C824 C842 C857 -175.9(8) . . . . ? N10 C824 C842 C857 -2.0(12) . . . . ? C808 N14 C854 C873 1.0(10) . . . . ? C881 N14 C854 C873 178.5(7) . . . . ? C808 N14 C854 C906 177.4(8) . . . . ? C881 N14 C854 C906 -5.1(14) . . . . ? C920 C842 C857 C917 -81.2(10) . . . . ? C824 C842 C857 C917 94.2(8) . . . . ? C920 C842 C857 C902 40.0(10) . . . . ? C824 C842 C857 C902 -144.6(7) . . . . ? C838 N11 C862 C915 122.7(9) . . . . ? C826 N11 C862 C915 -65.9(11) . . . . ? C838 N11 C862 C895 1.1(12) . . . . ? C826 N11 C862 C895 172.4(7) . . . . ? C838 N11 C862 C916 -112.2(9) . . . . ? C826 N11 C862 C916 59.2(11) . . . . ? C920 C869 C870 C893 0.9(13) . . . . ? N14 C854 C873 N13 -0.1(9) . . . . ? C906 C854 C873 N13 -176.2(9) . . . . ? N14 C854 C873 C905 178.3(8) . . . . ? C906 C854 C873 C905 2.2(17) . . . . ? C808 N13 C873 C854 -0.9(10) . . . . ? C835 N13 C873 C854 -176.5(7) . . . . ? C808 N13 C873 C905 -179.5(7) . . . . ? C835 N13 C873 C905 4.9(12) . . . . ? C808 N14 C881 C899 -113.9(8) . . . . ? C854 N14 C881 C899 68.9(10) . . . . ? C808 N14 C881 C901 7.1(10) . . . . ? C854 N14 C881 C901 -170.1(7) . . . . ? C808 N14 C881 C904 123.0(8) . . . . ? C854 N14 C881 C904 -54.3(11) . . . . ? C869 C870 C893 C824 -1.5(14) . . . . ? C869 C870 C893 C910 -179.6(9) . . . . ? C842 C824 C893 C870 1.1(13) . . . . ? N10 C824 C893 C870 -173.2(8) . . . . ? C842 C824 C893 C910 179.2(8) . . . . ? N10 C824 C893 C910 5.0(13) . . . . ? C870 C893 C910 C993 -28.2(15) . . . . ? C824 C893 C910 C993 153.6(10) . . . . ? C870 C893 C910 C999 95.9(11) . . . . ? C824 C893 C910 C999 -82.3(11) . . . . ? C824 C842 C920 C869 -0.3(13) . . . . ? C857 C842 C920 C869 175.3(8) . . . . ? C870 C869 C920 C842 0.0(13) . . . . ? C820 Ni3 N15 N16 165.6(5) . . . . ? C817 Ni3 N15 N16 17.5(9) . . . . ? Ni3 N15 N16 N17 -175.5(8) . . . . ? C820 Ni3 N16 N15 -24.7(8) . . . . ? C817 Ni3 N16 N15 -172.5(4) . . . . ? N15 Ni3 N16 N17 169.9(17) . . . . ? C820 Ni3 N16 N17 145.1(13) . . . . ? C817 Ni3 N16 N17 -2.6(16) . . . . ? N15 N16 N17 C818 175.7(7) . . . . ? Ni3 N16 N17 C818 7.9(18) . . . . ? C817 N20 C810 C811 -1.0(8) . . . . ? C815 N20 C810 C811 173.9(7) . . . . ? C817 N20 C810 C864 179.7(7) . . . . ? C815 N20 C810 C864 -5.4(12) . . . . ? N20 C810 C811 N21 -0.5(8) . . . . ? C864 C810 C811 N21 178.7(8) . . . . ? N20 C810 C811 C850 -179.9(7) . . . . ? C864 C810 C811 C850 -0.6(14) . . . . ? C817 N21 C811 C810 1.8(8) . . . . ? C833 N21 C811 C810 -179.5(7) . . . . ? C817 N21 C811 C850 -178.8(6) . . . . ? C833 N21 C811 C850 -0.1(11) . . . . ? C820 N19 C815 N20 -57.0(9) . . . . ? C858 N19 C815 N20 124.4(7) . . . . ? C810 N20 C815 N19 -121.4(7) . . . . ? C817 N20 C815 N19 53.1(8) . . . . ? C811 N21 C817 N20 -2.3(8) . . . . ? C833 N21 C817 N20 179.0(6) . . . . ? C811 N21 C817 Ni3 177.4(7) . . . . ? C833 N21 C817 Ni3 -1.4(13) . . . . ? C810 N20 C817 N21 2.0(8) . . . . ? C815 N20 C817 N21 -173.3(6) . . . . ? C810 N20 C817 Ni3 -177.8(5) . . . . ? C815 N20 C817 Ni3 6.9(8) . . . . ? N16 Ni3 C817 N21 -67.3(10) . . . . ? N15 Ni3 C817 N21 -79.8(12) . . . . ? C820 Ni3 C817 N21 130.3(9) . . . . ? N16 Ni3 C817 N20 112.4(5) . . . . ? N15 Ni3 C817 N20 99.8(8) . . . . ? C820 Ni3 C817 N20 -50.1(6) . . . . ? C840 C812 C818 C805 -4.9(12) . . . . ? C845 C812 C818 C805 175.9(7) . . . . ? C840 C812 C818 N17 -175.4(7) . . . . ? C845 C812 C818 N17 5.4(12) . . . . ? C856 C805 C818 C812 3.9(12) . . . . ? C846 C805 C818 C812 -176.1(7) . . . . ? C856 C805 C818 N17 175.5(7) . . . . ? C846 C805 C818 N17 -4.5(11) . . . . ? N16 N17 C818 C812 -64.5(10) . . . . ? N16 N17 C818 C805 124.7(7) . . . . ? C858 N19 C820 N18 -3.3(9) . . . . ? C815 N19 C820 N18 177.9(6) . . . . ? C858 N19 C820 Ni3 177.6(5) . . . . ? C815 N19 C820 Ni3 -1.2(9) . . . . ? C888 N18 C820 N19 3.0(8) . . . . ? C865 N18 C820 N19 177.9(6) . . . . ? C888 N18 C820 Ni3 -178.3(7) . . . . ? C865 N18 C820 Ni3 -3.5(13) . . . . ? N16 Ni3 C820 N19 -104.1(7) . . . . ? N15 Ni3 C820 N19 -120.2(6) . . . . ? C817 Ni3 C820 N19 48.3(6) . . . . ? N16 Ni3 C820 N18 77.3(11) . . . . ? N15 Ni3 C820 N18 61.3(10) . . . . ? C817 Ni3 C820 N18 -130.3(9) . . . . ? C817 N21 C833 C882 -134.1(7) . . . . ? C811 N21 C833 C882 47.3(10) . . . . ? C817 N21 C833 C861 -15.0(10) . . . . ? C811 N21 C833 C861 166.5(7) . . . . ? C817 N21 C833 C868 102.7(7) . . . . ? C811 N21 C833 C868 -75.9(8) . . . . ? C818 C812 C840 C844 3.6(13) . . . . ? C845 C812 C840 C844 -177.3(8) . . . . ? C812 C840 C844 C856 -1.2(14) . . . . ? C840 C812 C845 C892 109.6(9) . . . . ? C818 C812 C845 C892 -71.3(10) . . . . ? C840 C812 C845 C887 -16.7(11) . . . . ? C818 C812 C845 C887 162.5(8) . . . . ? C856 C805 C846 C991 -18.6(12) . . . . ? C818 C805 C846 C991 161.4(8) . . . . ? C856 C805 C846 C990 107.9(9) . . . . ? C818 C805 C846 C990 -72.1(10) . . . . ? C840 C844 C856 C805 0.3(14) . . . . ? C818 C805 C856 C844 -1.7(13) . . . . ? C846 C805 C856 C844 178.3(8) . . . . ? C820 N19 C858 C888 2.4(10) . . . . ? C815 N19 C858 C888 -178.9(7) . . . . ? C820 N19 C858 C890 179.6(7) . . . . ? C815 N19 C858 C890 -1.7(12) . . . . ? C820 N18 C865 C876 51.7(9) . . . . ? C888 N18 C865 C876 -134.7(8) . . . . ? C820 N18 C865 C872 -69.0(9) . . . . ? C888 N18 C865 C872 104.6(9) . . . . ? C820 N18 C865 C913 170.9(7) . . . . ? C888 N18 C865 C913 -15.5(12) . . . . ? N19 C858 C888 N18 -0.3(10) . . . . ? C890 C858 C888 N18 -177.0(9) . . . . ? N19 C858 C888 C912 176.6(8) . . . . ? C890 C858 C888 C912 0.0(17) . . . . ? C820 N18 C888 C858 -1.7(10) . . . . ? C865 N18 C888 C858 -175.7(8) . . . . ? C820 N18 C888 C912 -178.5(8) . . . . ? C865 N18 C888 C912 7.5(14) . . . . ? C825 Ni4 N26 N27 -171.5(4) . . . . ? C802 Ni4 N26 N27 -24.7(9) . . . . ? Ni4 N26 N27 N28 176.6(7) . . . . ? C825 Ni4 N27 N26 14.3(7) . . . . ? C802 Ni4 N27 N26 170.2(4) . . . . ? N26 Ni4 N27 N28 -173.0(16) . . . . ? C825 Ni4 N27 N28 -158.7(12) . . . . ? C802 Ni4 N27 N28 -2.8(14) . . . . ? N26 N27 N28 C803 -178.3(6) . . . . ? Ni4 N27 N28 C803 -7.0(16) . . . . ? C819 N23 C802 N22 -0.1(7) . . . . ? C804 N23 C802 N22 176.2(6) . . . . ? C819 N23 C802 Ni4 179.9(4) . . . . ? C804 N23 C802 Ni4 -3.9(8) . . . . ? C827 N22 C802 N23 0.7(8) . . . . ? C829 N22 C802 N23 -176.9(6) . . . . ? C827 N22 C802 Ni4 -179.1(7) . . . . ? C829 N22 C802 Ni4 3.3(13) . . . . ? N27 Ni4 C802 N23 -116.0(5) . . . . ? N26 Ni4 C802 N23 -97.9(9) . . . . ? C825 Ni4 C802 N23 50.4(5) . . . . ? N27 Ni4 C802 N22 63.9(9) . . . . ? N26 Ni4 C802 N22 82.0(11) . . . . ? C825 Ni4 C802 N22 -129.7(9) . . . . ? C813 C801 C803 C889 3.6(11) . . . . ? C822 C801 C803 C889 -170.1(7) . . . . ? C813 C801 C803 N28 175.5(6) . . . . ? C822 C801 C803 N28 1.8(11) . . . . ? N27 N28 C803 C889 -122.6(7) . . . . ? N27 N28 C803 C801 65.0(9) . . . . ? C825 N24 C804 N23 54.2(8) . . . . ? C849 N24 C804 N23 -122.7(7) . . . . ? C802 N23 C804 N24 -55.1(8) . . . . ? C819 N23 C804 N24 120.6(7) . . . . ? C803 C801 C813 C855 0.8(12) . . . . ? C822 C801 C813 C855 174.6(8) . . . . ? C802 N23 C819 C827 -0.6(8) . . . . ? C804 N23 C819 C827 -176.6(6) . . . . ? C802 N23 C819 C851 -178.2(7) . . . . ? C804 N23 C819 C851 5.9(11) . . . . ? C803 C801 C822 C859 90.5(9) . . . . ? C813 C801 C822 C859 -82.9(8) . . . . ? C803 C801 C822 C884 -148.5(7) . . . . ? C813 C801 C822 C884 38.1(10) . . . . ? C828 N25 C825 N24 -1.2(7) . . . . ? C853 N25 C825 N24 -177.5(6) . . . . ? C828 N25 C825 Ni4 177.2(7) . . . . ? C853 N25 C825 Ni4 1.0(12) . . . . ? C849 N24 C825 N25 1.9(7) . . . . ? C804 N24 C825 N25 -175.4(5) . . . . ? C849 N24 C825 Ni4 -177.1(4) . . . . ? C804 N24 C825 Ni4 5.6(8) . . . . ? N27 Ni4 C825 N25 -69.7(10) . . . . ? N26 Ni4 C825 N25 -60.4(9) . . . . ? C802 Ni4 C825 N25 130.5(9) . . . . ? N27 Ni4 C825 N24 108.6(6) . . . . ? N26 Ni4 C825 N24 117.9(5) . . . . ? C802 Ni4 C825 N24 -51.2(5) . . . . ? N23 C819 C827 N22 1.0(8) . . . . ? C851 C819 C827 N22 178.3(7) . . . . ? N23 C819 C827 C871 -176.7(7) . . . . ? C851 C819 C827 C871 0.5(14) . . . . ? C802 N22 C827 C819 -1.1(9) . . . . ? C829 N22 C827 C819 176.4(7) . . . . ? C802 N22 C827 C871 176.5(7) . . . . ? C829 N22 C827 C871 -6.0(12) . . . . ? C825 N25 C828 C849 0.1(8) . . . . ? C853 N25 C828 C849 176.0(7) . . . . ? C825 N25 C828 C886 179.6(6) . . . . ? C853 N25 C828 C886 -4.6(12) . . . . ? C827 N22 C829 C903 -60.7(10) . . . . ? C802 N22 C829 C903 116.6(7) . . . . ? C827 N22 C829 C919 61.5(10) . . . . ? C802 N22 C829 C919 -121.2(8) . . . . ? C827 N22 C829 C863 -175.1(7) . . . . ? C802 N22 C829 C863 2.3(11) . . . . ? N25 C828 C849 N24 1.0(7) . . . . ? C886 C828 C849 N24 -178.4(6) . . . . ? N25 C828 C849 C879 -179.1(7) . . . . ? C886 C828 C849 C879 1.4(13) . . . . ? C825 N24 C849 C828 -1.9(8) . . . . ? C804 N24 C849 C828 175.2(6) . . . . ? C825 N24 C849 C879 178.2(6) . . . . ? C804 N24 C849 C879 -4.7(10) . . . . ? C825 N25 C853 C918 86.8(10) . . . . ? C828 N25 C853 C918 -88.7(10) . . . . ? C825 N25 C853 C894 -30.1(10) . . . . ? C828 N25 C853 C894 154.4(7) . . . . ? C825 N25 C853 C909 -148.2(9) . . . . ? C828 N25 C853 C909 36.3(12) . . . . ? C801 C813 C855 C867 -3.1(13) . . . . ? C813 C855 C867 C889 1.1(13) . . . . ? C855 C867 C889 C803 3.1(13) . . . . ? C855 C867 C889 C814 -178.5(7) . . . . ? C801 C803 C889 C867 -5.6(12) . . . . ? N28 C803 C889 C867 -177.9(7) . . . . ? C801 C803 C889 C814 176.0(7) . . . . ? N28 C803 C889 C814 3.7(10) . . . . ? C998 C814 C889 C867 69.1(12) . . . . ? C994 C814 C889 C867 -50.5(14) . . . . ? C998 C814 C889 C803 -112.5(11) . . . . ? C994 C814 C889 C803 127.8(11) . . . . ? C800 Ni5 N33 N34 -164.1(4) . . . . ? C809 Ni5 N33 N34 -11.1(9) . . . . ? Ni5 N33 N34 N35 176.6(7) . . . . ? C800 Ni5 N34 N33 26.7(6) . . . . ? C809 Ni5 N34 N33 175.4(4) . . . . ? C800 Ni5 N34 N35 -146.4(11) . . . . ? N33 Ni5 N34 N35 -173.1(14) . . . . ? C809 Ni5 N34 N35 2.3(12) . . . . ? N33 N34 N35 C830 -178.2(6) . . . . ? Ni5 N34 N35 C830 -6.7(15) . . . . ? C831 N30 C800 N29 1.9(7) . . . . ? C806 N30 C800 N29 178.0(6) . . . . ? C831 N30 C800 Ni5 -173.6(5) . . . . ? C806 N30 C800 Ni5 2.5(8) . . . . ? C847 N29 C800 N30 -2.7(7) . . . . ? C880 N29 C800 N30 176.8(6) . . . . ? C847 N29 C800 Ni5 170.9(6) . . . . ? C880 N29 C800 Ni5 -9.6(12) . . . . ? N34 Ni5 C800 N30 104.9(6) . . . . ? N33 Ni5 C800 N30 122.2(5) . . . . ? C809 Ni5 C800 N30 -48.5(5) . . . . ? N34 Ni5 C800 N29 -68.1(10) . . . . ? N33 Ni5 C800 N29 -50.8(8) . . . . ? C809 Ni5 C800 N29 138.5(8) . . . . ? C800 N30 C806 N31 56.9(8) . . . . ? C831 N30 C806 N31 -127.6(7) . . . . ? C809 N31 C806 N30 -56.8(8) . . . . ? C807 N31 C806 N30 120.7(7) . . . . ? C809 N31 C807 C834 0.0(8) . . . . ? C806 N31 C807 C834 -177.6(6) . . . . ? C809 N31 C807 C878 -177.8(6) . . . . ? C806 N31 C807 C878 4.5(11) . . . . ? C834 N32 C809 N31 2.3(7) . . . . ? C837 N32 C809 N31 -177.2(5) . . . . ? C834 N32 C809 Ni5 -179.6(6) . . . . ? C837 N32 C809 Ni5 0.9(12) . . . . ? C807 N31 C809 N32 -1.4(7) . . . . ? C806 N31 C809 N32 176.4(5) . . . . ? C807 N31 C809 Ni5 179.8(4) . . . . ? C806 N31 C809 Ni5 -2.3(7) . . . . ? N34 Ni5 C809 N32 67.5(9) . . . . ? C800 Ni5 C809 N32 -130.1(8) . . . . ? N33 Ni5 C809 N32 75.6(11) . . . . ? N34 Ni5 C809 N31 -114.6(5) . . . . ? C800 Ni5 C809 N31 47.8(5) . . . . ? N33 Ni5 C809 N31 -106.4(8) . . . . ? C860 C816 C830 N35 -177.6(6) . . . . ? C839 C816 C830 N35 1.7(10) . . . . ? C860 C816 C830 C821 -2.2(11) . . . . ? C839 C816 C830 C821 177.1(6) . . . . ? N34 N35 C830 C816 -124.5(6) . . . . ? N34 N35 C830 C821 60.4(9) . . . . ? C930 C821 C830 C816 0.6(10) . . . . ? C832 C821 C830 C816 -169.1(6) . . . . ? C930 C821 C830 N35 175.5(7) . . . . ? C832 C821 C830 N35 5.8(10) . . . . ? C800 N30 C831 C847 -0.4(9) . . . . ? C806 N30 C831 C847 -176.1(7) . . . . ? C800 N30 C831 C866 -177.7(6) . . . . ? C806 N30 C831 C866 6.6(11) . . . . ? C930 C821 C832 C896 -88.1(9) . . . . ? C830 C821 C832 C896 81.2(9) . . . . ? C930 C821 C832 C875 33.4(10) . . . . ? C830 C821 C832 C875 -157.3(6) . . . . ? N31 C807 C834 N32 1.4(7) . . . . ? C878 C807 C834 N32 178.9(7) . . . . ? N31 C807 C834 C883 -178.3(6) . . . . ? C878 C807 C834 C883 -0.7(13) . . . . ? C809 N32 C834 C807 -2.4(8) . . . . ? C837 N32 C834 C807 177.1(6) . . . . ? C809 N32 C834 C883 177.2(7) . . . . ? C837 N32 C834 C883 -3.3(11) . . . . ? C809 N32 C837 C891 -109.7(8) . . . . ? C834 N32 C837 C891 70.8(8) . . . . ? C809 N32 C837 C885 8.7(9) . . . . ? C834 N32 C837 C885 -170.7(6) . . . . ? C809 N32 C837 C897 127.1(7) . . . . ? C834 N32 C837 C897 -52.4(9) . . . . ? C860 C816 C839 C997 25.7(11) . . . . ? C830 C816 C839 C997 -153.6(8) . . . . ? C860 C816 C839 C996 -103.2(8) . . . . ? C830 C816 C839 C996 77.5(9) . . . . ? N30 C831 C847 N29 -1.4(9) . . . . ? C866 C831 C847 N29 175.6(7) . . . . ? N30 C831 C847 C898 175.2(7) . . . . ? C866 C831 C847 C898 -7.8(15) . . . . ? C800 N29 C847 C831 2.7(9) . . . . ? C880 N29 C847 C831 -176.8(7) . . . . ? C800 N29 C847 C898 -174.0(7) . . . . ? C880 N29 C847 C898 6.6(12) . . . . ? C830 C816 C860 C877 1.1(12) . . . . ? C839 C816 C860 C877 -178.2(7) . . . . ? C816 C860 C877 C930 1.6(12) . . . . ? C800 N29 C880 C914 96.7(9) . . . . ? C847 N29 C880 C914 -83.9(10) . . . . ? C800 N29 C880 C907 -23.1(10) . . . . ? C847 N29 C880 C907 156.3(7) . . . . ? C800 N29 C880 C908 -140.5(7) . . . . ? C847 N29 C880 C908 39.0(11) . . . . ? C830 C821 C930 C877 2.2(12) . . . . ? C832 C821 C930 C877 171.6(7) . . . . ? C860 C877 C930 C821 -3.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.707 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.105 _database_code_depnum_ccdc_archive 'CCDC 901783'