# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mallayan Palaniandavar' _publ_contact_author_email palanim51@yahoo.com _publ_author_name M.Palaniandavar data_14mpmb _database_code_depnum_ccdc_archive 'CCDC 805447' #TrackingRef '- 1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H27 Cl2 N5 Ni O9' _chemical_formula_weight 587.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8006(12) _cell_length_b 10.4718(8) _cell_length_c 15.1299(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.9420(10) _cell_angle_gamma 90.00 _cell_volume 2394.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1687 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 24.32 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5952 _exptl_absorpt_correction_T_max 0.8710 _exptl_absorpt_process_details BRUKER-SADABS _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 Smart Apex CCD Diffractometer' _diffrn_measurement_method 'Omega-Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14152 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5595 _reflns_number_gt 4888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart ' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+4.1303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5595 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24450(2) 0.25680(3) 0.46240(2) 0.01417(10) Uani 1 d . . . N1 N 0.26599(15) 0.0865(2) 0.40500(15) 0.0181(5) Uani 1 d . . . N2 N 0.17828(15) 0.1382(2) 0.53146(15) 0.0172(4) Uani 1 d . . . N3 N 0.18092(15) 0.3961(2) 0.51867(15) 0.0176(4) Uani 1 d . . . N4 N 0.35636(16) 0.2319(2) 0.57993(16) 0.0204(5) Uani 1 d . . . N5 N 0.31294(15) 0.3783(2) 0.40264(15) 0.0182(5) Uani 1 d . . . C1 C 0.31849(19) 0.0657(3) 0.35017(18) 0.0219(6) Uani 1 d . . . H1 H 0.3551 0.1313 0.3418 0.026 Uiso 1 calc R . . C2 C 0.3198(2) -0.0487(3) 0.3065(2) 0.0277(6) Uani 1 d . . . H2 H 0.3566 -0.0603 0.2690 0.033 Uiso 1 calc R . . C3 C 0.2658(2) -0.1463(3) 0.3190(2) 0.0286(7) Uani 1 d . . . H3 H 0.2645 -0.2238 0.2887 0.034 Uiso 1 calc R . . C4 C 0.2136(2) -0.1276(3) 0.3768(2) 0.0267(6) Uani 1 d . . . H4 H 0.1779 -0.1930 0.3874 0.032 Uiso 1 calc R . . C5 C 0.21526(19) -0.0095(3) 0.41890(19) 0.0211(6) Uani 1 d . . . C6 C 0.1568(2) 0.0165(3) 0.4799(2) 0.0281(7) Uani 1 d . . . H6A H 0.0956 0.0189 0.4420 0.034 Uiso 1 calc R . . H6B H 0.1628 -0.0531 0.5236 0.034 Uiso 1 calc R . . C7 C 0.09883(18) 0.2071(3) 0.5374(2) 0.0208(5) Uani 1 d . . . H7A H 0.0788 0.1718 0.5871 0.025 Uiso 1 calc R . . H7B H 0.0517 0.1966 0.4801 0.025 Uiso 1 calc R . . C8 C 0.11921(18) 0.3474(3) 0.55487(18) 0.0191(5) Uani 1 d . . . C9 C 0.07542(19) 0.4223(3) 0.6025(2) 0.0241(6) Uani 1 d . . . H9 H 0.0340 0.3861 0.6278 0.029 Uiso 1 calc R . . C10 C 0.09351(19) 0.5514(3) 0.6122(2) 0.0256(6) Uani 1 d . . . H10 H 0.0647 0.6031 0.6442 0.031 Uiso 1 calc R . . C11 C 0.15510(19) 0.6024(3) 0.5735(2) 0.0235(6) Uani 1 d . . . H11 H 0.1676 0.6893 0.5780 0.028 Uiso 1 calc R . . C12 C 0.19773(19) 0.5222(3) 0.52797(19) 0.0208(5) Uani 1 d . . . H12 H 0.2398 0.5566 0.5027 0.025 Uiso 1 calc R . . C13 C 0.2404(2) 0.1208(3) 0.6263(2) 0.0316(7) Uani 1 d . . . H13A H 0.2319 0.1901 0.6653 0.038 Uiso 1 calc R . . H13B H 0.2260 0.0416 0.6520 0.038 Uiso 1 calc R . . C14 C 0.3343(2) 0.1174(3) 0.6280(2) 0.0332(7) Uani 1 d . . . H14A H 0.3456 0.0404 0.5976 0.040 Uiso 1 calc R . . H14B H 0.3716 0.1158 0.6915 0.040 Uiso 1 calc R . . C15 C 0.3765(2) 0.3455(3) 0.6383(2) 0.0327(7) Uani 1 d . . . H15A H 0.3260 0.3677 0.6583 0.049 Uiso 1 calc R . . H15B H 0.3905 0.4151 0.6037 0.049 Uiso 1 calc R . . H15C H 0.4261 0.3285 0.6912 0.049 Uiso 1 calc R . . C16 C 0.4388(2) 0.1957(3) 0.5572(2) 0.0336(7) Uani 1 d . . . H16A H 0.4561 0.2641 0.5240 0.050 Uiso 1 calc R . . H16B H 0.4282 0.1201 0.5196 0.050 Uiso 1 calc R . . H16C H 0.4851 0.1795 0.6132 0.050 Uiso 1 calc R . . C17 C 0.34848(17) 0.4556(2) 0.37430(17) 0.0173(5) Uani 1 d . . . C18 C 0.3956(2) 0.5539(3) 0.3399(2) 0.0240(6) Uani 1 d . . . H18A H 0.4072 0.6251 0.3816 0.036 Uiso 1 calc R . . H18B H 0.3602 0.5815 0.2800 0.036 Uiso 1 calc R . . H18C H 0.4506 0.5199 0.3352 0.036 Uiso 1 calc R . . Cl1 Cl 0.07516(4) 0.59015(6) 0.22567(4) 0.01948(15) Uani 1 d . . . O1 O 0.15747(17) 0.5608(2) 0.29160(16) 0.0415(6) Uani 1 d . . . O2 O 0.01608(19) 0.4835(2) 0.2177(2) 0.0505(7) Uani 1 d . . . O4 O 0.08702(17) 0.6145(2) 0.13722(16) 0.0382(6) Uani 1 d . . . O3 O 0.03636(15) 0.7013(2) 0.25446(16) 0.0314(5) Uani 1 d . . . Cl2 Cl 0.41345(4) 0.75379(6) 0.11578(4) 0.01957(15) Uani 1 d . . . O5 O 0.33089(15) 0.7138(2) 0.12951(18) 0.0351(5) Uani 1 d . . . O7 O 0.45985(17) 0.8311(3) 0.19383(17) 0.0437(6) Uani 1 d . . . O8 O 0.46636(17) 0.6452(2) 0.1104(2) 0.0440(6) Uani 1 d . . . O6 O 0.39665(17) 0.8310(2) 0.03478(16) 0.0413(6) Uani 1 d . . . O9 O 0.13876(16) 0.2816(2) 0.33631(16) 0.0281(5) Uani 1 d . . . H9A H 0.094(3) 0.248(4) 0.314(3) 0.054(14) Uiso 1 d . . . H9B H 0.131(3) 0.351(5) 0.323(3) 0.063(16) Uiso 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 0.01610(18) 0.01345(17) 0.01337(17) 0.00132(12) 0.00493(13) -0.00114(12) N1 0.0217(11) 0.0184(11) 0.0136(10) 0.0006(8) 0.0042(9) 0.0015(9) N2 0.0182(11) 0.0155(11) 0.0178(11) 0.0018(8) 0.0054(9) -0.0022(8) N3 0.0173(11) 0.0172(11) 0.0183(11) 0.0011(8) 0.0053(9) 0.0014(8) N4 0.0221(12) 0.0217(12) 0.0165(11) 0.0043(9) 0.0043(9) -0.0069(9) N5 0.0190(11) 0.0184(11) 0.0173(11) 0.0005(9) 0.0055(9) -0.0004(9) C1 0.0238(14) 0.0247(14) 0.0178(13) 0.0020(11) 0.0069(11) 0.0012(11) C2 0.0372(17) 0.0277(15) 0.0196(14) 0.0006(11) 0.0103(13) 0.0103(13) C3 0.0400(18) 0.0193(14) 0.0232(14) -0.0037(11) 0.0043(13) 0.0073(12) C4 0.0336(16) 0.0187(14) 0.0269(15) -0.0017(11) 0.0073(13) -0.0015(12) C5 0.0241(14) 0.0189(13) 0.0189(13) 0.0012(10) 0.0041(11) -0.0008(11) C6 0.0345(17) 0.0176(14) 0.0381(17) -0.0052(12) 0.0200(14) -0.0079(12) C7 0.0180(13) 0.0219(13) 0.0234(14) -0.0017(11) 0.0075(11) -0.0032(11) C8 0.0168(12) 0.0216(13) 0.0169(12) 0.0012(10) 0.0019(10) 0.0003(10) C9 0.0195(13) 0.0296(15) 0.0248(14) -0.0018(12) 0.0091(11) -0.0012(11) C10 0.0240(14) 0.0276(15) 0.0260(15) -0.0052(12) 0.0085(12) 0.0045(12) C11 0.0243(14) 0.0184(13) 0.0263(14) -0.0021(11) 0.0050(12) 0.0009(11) C12 0.0204(13) 0.0187(13) 0.0237(14) 0.0018(10) 0.0072(11) -0.0004(10) C13 0.0242(15) 0.0413(18) 0.0268(15) 0.0182(14) 0.0036(12) -0.0038(13) C14 0.0330(17) 0.0332(17) 0.0307(17) 0.0066(13) 0.0052(14) -0.0043(14) C15 0.0245(15) 0.0394(18) 0.0276(16) -0.0130(14) -0.0029(13) 0.0060(13) C16 0.0266(16) 0.0384(18) 0.0284(16) -0.0087(14) -0.0034(13) 0.0111(14) C17 0.0189(12) 0.0182(13) 0.0134(12) -0.0009(10) 0.0025(10) 0.0004(10) C18 0.0308(15) 0.0214(14) 0.0220(14) -0.0031(11) 0.0110(12) -0.0087(12) Cl1 0.0223(3) 0.0164(3) 0.0214(3) 0.0031(2) 0.0091(3) 0.0037(2) O1 0.0408(14) 0.0406(14) 0.0334(13) 0.0013(11) -0.0046(11) 0.0187(11) O2 0.0553(17) 0.0260(13) 0.075(2) -0.0009(12) 0.0274(15) -0.0104(12) O4 0.0469(15) 0.0432(14) 0.0301(12) 0.0107(10) 0.0202(11) 0.0144(11) O3 0.0308(12) 0.0232(11) 0.0438(13) -0.0032(10) 0.0165(10) 0.0065(9) Cl2 0.0212(3) 0.0184(3) 0.0200(3) 0.0030(2) 0.0074(3) 0.0032(2) O5 0.0254(11) 0.0336(12) 0.0502(15) 0.0085(11) 0.0172(11) 0.0014(9) O7 0.0412(14) 0.0506(16) 0.0326(13) -0.0102(11) 0.0001(11) -0.0052(12) O8 0.0449(15) 0.0275(12) 0.0695(18) 0.0049(12) 0.0325(14) 0.0135(11) O6 0.0508(15) 0.0482(15) 0.0282(12) 0.0186(11) 0.0166(11) 0.0121(12) O9 0.0293(12) 0.0224(12) 0.0255(11) 0.0061(9) -0.0033(9) -0.0037(10) _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 N5 2.044(2) . ? Ni1 N1 2.054(2) . ? Ni1 N3 2.088(2) . ? Ni1 N2 2.090(2) . ? Ni1 N4 2.127(2) . ? Ni1 O9 2.154(2) . ? N1 C5 1.340(4) . ? N1 C1 1.351(3) . ? N2 C7 1.473(3) . ? N2 C6 1.481(4) . ? N2 C13 1.495(4) . ? N3 C12 1.346(3) . ? N3 C8 1.350(3) . ? N4 C15 1.461(4) . ? N4 C16 1.490(4) . ? N4 C14 1.495(4) . ? N5 C17 1.138(3) . ? C1 C2 1.371(4) . ? C1 H1 0.9300 . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? C3 C4 1.381(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.509(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.510(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.380(4) . ? C9 C10 1.380(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.380(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.477(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.453(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? Cl1 O1 1.423(2) . ? Cl1 O4 1.427(2) . ? Cl1 O2 1.438(3) . ? Cl1 O3 1.441(2) . ? Cl2 O6 1.427(2) . ? Cl2 O8 1.427(2) . ? Cl2 O5 1.442(2) . ? Cl2 O7 1.443(2) . ? O9 H9A 0.78(5) . ? O9 H9B 0.75(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 N5 Ni1 N1 100.34(9) . . ? N5 Ni1 N3 97.17(9) . . ? N1 Ni1 N3 159.57(9) . . ? N5 Ni1 N2 176.39(9) . . ? N1 Ni1 N2 82.18(9) . . ? N3 Ni1 N2 80.85(9) . . ? N5 Ni1 N4 91.62(9) . . ? N1 Ni1 N4 92.72(9) . . ? N3 Ni1 N4 97.25(9) . . ? N2 Ni1 N4 85.65(9) . . ? N5 Ni1 O9 84.67(9) . . ? N1 Ni1 O9 84.92(9) . . ? N3 Ni1 O9 86.32(9) . . ? N2 Ni1 O9 98.18(9) . . ? N4 Ni1 O9 175.16(9) . . ? C5 N1 C1 118.5(2) . . ? C5 N1 Ni1 113.88(18) . . ? C1 N1 Ni1 127.34(19) . . ? C7 N2 C6 112.6(2) . . ? C7 N2 C13 109.5(2) . . ? C6 N2 C13 112.7(2) . . ? C7 N2 Ni1 107.37(16) . . ? C6 N2 Ni1 108.65(16) . . ? C13 N2 Ni1 105.56(16) . . ? C12 N3 C8 118.2(2) . . ? C12 N3 Ni1 128.62(18) . . ? C8 N3 Ni1 113.05(18) . . ? C15 N4 C16 107.2(2) . . ? C15 N4 C14 113.6(2) . . ? C16 N4 C14 104.6(2) . . ? C15 N4 Ni1 112.75(18) . . ? C16 N4 Ni1 114.04(18) . . ? C14 N4 Ni1 104.48(18) . . ? C17 N5 Ni1 173.0(2) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.9(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.9(3) . . ? N1 C5 C6 117.5(2) . . ? C4 C5 C6 120.5(3) . . ? N2 C6 C5 112.9(2) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 110.2(2) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C9 121.9(3) . . ? N3 C8 C7 116.0(2) . . ? C9 C8 C7 122.1(2) . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 118.9(3) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 118.9(3) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N3 C12 C11 122.6(3) . . ? N3 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C14 C13 N2 113.2(3) . . ? C14 C13 H13A 108.9 . . ? N2 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? N2 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 N4 110.4(3) . . ? C13 C14 H14A 109.6 . . ? N4 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? N4 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C18 178.7(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 Cl1 O4 110.67(15) . . ? O1 Cl1 O2 109.20(17) . . ? O4 Cl1 O2 108.65(17) . . ? O1 Cl1 O3 110.20(14) . . ? O4 Cl1 O3 108.85(14) . . ? O2 Cl1 O3 109.24(15) . . ? O6 Cl2 O8 111.55(15) . . ? O6 Cl2 O5 109.79(15) . . ? O8 Cl2 O5 110.30(14) . . ? O6 Cl2 O7 107.93(16) . . ? O8 Cl2 O7 109.11(17) . . ? O5 Cl2 O7 108.07(15) . . ? Ni1 O9 H9A 135(3) . . ? Ni1 O9 H9B 112(4) . . ? H9A O9 H9B 106(5) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 1.731 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.089 # Attachment '- 2.CIF' data_16mpmbkf _database_code_depnum_ccdc_archive 'CCDC 805448' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H72 B2 N7 Ni' _chemical_formula_weight 1115.70 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.1135(16) _cell_length_b 13.4486(11) _cell_length_c 23.7510(19) _cell_angle_alpha 90.00 _cell_angle_beta 110.286(2) _cell_angle_gamma 90.00 _cell_volume 6026.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5437 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.76 _exptl_crystal_description BLOCKS _exptl_crystal_colour PINK _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2364 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.8687 _exptl_absorpt_correction_T_max 0.9261 _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 SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'omega-phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27937 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.2145 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.00 _reflns_number_total 11414 _reflns_number_gt 5848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_detail 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^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 11414 _refine_ls_number_parameters 732 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.73921(3) 0.78985(3) 0.23098(2) 0.01897(13) Uani 1 d . . . N1 N 0.73330(17) 0.8531(2) 0.14998(14) 0.0227(8) Uani 1 d . . . N2 N 0.83898(16) 0.7472(2) 0.23204(14) 0.0213(7) Uani 1 d . . . N3 N 0.78098(17) 0.7440(2) 0.31993(14) 0.0208(8) Uani 1 d . . . N4 N 0.70494(17) 0.6441(2) 0.18924(14) 0.0216(8) Uani 1 d . . . N5 N 0.78036(16) 0.9336(2) 0.26855(14) 0.0230(8) Uiso 1 d . . . N6 N 0.64218(18) 0.8338(2) 0.22995(15) 0.0266(8) Uani 1 d . . . N7 N 0.8763(4) 0.9473(4) 0.3984(3) 0.104(2) Uani 1 d . . . B1 B 0.5007(2) 0.7265(3) 0.3894(2) 0.0194(10) Uani 1 d . . . B2 B 0.9428(2) 0.3274(3) 0.3456(2) 0.0181(10) Uani 1 d . . . C1 C 0.6764(2) 0.8969(3) 0.10852(17) 0.0238(9) Uani 1 d . . . H1 H 0.6325 0.8936 0.1133 0.029 Uiso 1 calc R . . C2 C 0.6823(2) 0.9460(3) 0.05964(17) 0.0234(9) Uani 1 d . . . H2 H 0.6426 0.9751 0.0316 0.028 Uiso 1 calc R . . C3 C 0.7468(2) 0.9517(3) 0.05245(18) 0.0245(10) Uani 1 d . . . H3 H 0.7516 0.9852 0.0198 0.029 Uiso 1 calc R . . C4 C 0.8053(2) 0.9066(3) 0.09473(18) 0.0229(9) Uani 1 d . . . H4 H 0.8496 0.9087 0.0907 0.028 Uiso 1 calc R . . C5 C 0.7959(2) 0.8589(3) 0.14271(18) 0.0199(9) Uani 1 d . . . C6 C 0.8597(2) 0.8169(3) 0.19266(18) 0.0275(10) Uani 1 d . . . H6A H 0.8901 0.7826 0.1750 0.033 Uiso 1 calc R . . H6B H 0.8866 0.8714 0.2167 0.033 Uiso 1 calc R . . C7 C 0.8880(2) 0.7532(3) 0.29558(17) 0.0285(10) Uani 1 d . . . H7A H 0.9046 0.8210 0.3049 0.034 Uiso 1 calc R . . H7B H 0.9289 0.7109 0.3011 0.034 Uiso 1 calc R . . C8 C 0.8503(2) 0.7205(3) 0.33700(17) 0.0217(9) Uani 1 d . . . C9 C 0.8843(2) 0.6750(3) 0.39156(18) 0.0276(10) Uani 1 d . . . H9 H 0.9315 0.6560 0.4020 0.033 Uiso 1 calc R . . C10 C 0.8487(2) 0.6579(3) 0.43034(18) 0.0274(10) Uani 1 d . . . H10 H 0.8712 0.6258 0.4667 0.033 Uiso 1 calc R . . C11 C 0.7800(2) 0.6881(2) 0.41528(17) 0.0229(9) Uani 1 d . . . H11 H 0.7557 0.6802 0.4419 0.027 Uiso 1 calc R . . C12 C 0.7474(2) 0.7310(3) 0.35925(18) 0.0234(9) Uani 1 d . . . H12 H 0.7004 0.7515 0.3486 0.028 Uiso 1 calc R . . C13 C 0.8340(2) 0.6422(3) 0.21145(19) 0.0275(10) Uani 1 d . . . H13A H 0.8423 0.5983 0.2456 0.033 Uiso 1 calc R . . H13B H 0.8704 0.6295 0.1942 0.033 Uiso 1 calc R . . C14 C 0.7632(2) 0.6202(3) 0.1659(2) 0.0305(11) Uani 1 d . . . H14A H 0.7608 0.5503 0.1552 0.037 Uiso 1 calc R . . H14B H 0.7569 0.6589 0.1300 0.037 Uiso 1 calc R . . C15 C 0.6366(2) 0.6502(3) 0.13744(19) 0.0286(10) Uani 1 d . . . H15A H 0.6417 0.6995 0.1094 0.034 Uiso 1 calc R . . H15B H 0.6000 0.6737 0.1522 0.034 Uiso 1 calc R . . C16 C 0.6114(2) 0.5528(3) 0.1034(2) 0.0424(13) Uani 1 d . . . H16A H 0.6462 0.5298 0.0872 0.064 Uiso 1 calc R . . H16B H 0.5672 0.5638 0.0713 0.064 Uiso 1 calc R . . H16C H 0.6048 0.5037 0.1304 0.064 Uiso 1 calc R . . C17 C 0.7025(2) 0.5660(3) 0.23265(19) 0.0283(10) Uani 1 d . . . H17A H 0.7455 0.5696 0.2676 0.034 Uiso 1 calc R . . H17B H 0.7013 0.5013 0.2143 0.034 Uiso 1 calc R . . C18 C 0.6391(2) 0.5751(3) 0.25288(19) 0.0312(11) Uani 1 d . . . H18A H 0.6320 0.6438 0.2604 0.047 Uiso 1 calc R . . H18B H 0.6474 0.5373 0.2890 0.047 Uiso 1 calc R . . H18C H 0.5976 0.5502 0.2220 0.047 Uiso 1 calc R . . C19A C 0.7481(8) 1.1097(12) 0.2822(7) 0.127(5) Uiso 0.58 d P . . C19 C 0.7815(10) 1.0970(14) 0.2221(8) 0.108(6) Uiso 0.42 d P . . C20 C 0.7652(5) 1.0250(8) 0.2613(5) 0.150(4) Uiso 1 d . . . C21 C 0.53149(19) 0.9345(3) 0.22632(17) 0.0232(9) Uani 1 d . . . H21A H 0.5452 0.9857 0.2563 0.035 Uiso 1 calc R . . H21B H 0.4970 0.8920 0.2336 0.035 Uiso 1 calc R . . H21C H 0.5114 0.9643 0.1873 0.035 Uiso 1 calc R . . C22 C 0.5933(2) 0.8764(3) 0.22890(17) 0.0222(9) Uani 1 d . . . C23 C 1.0003(4) 0.8783(6) 0.4685(3) 0.114(3) Uani 1 d . . . H23A H 1.0103 0.8190 0.4504 0.172 Uiso 1 calc R . . H23B H 0.9990 0.8629 0.5076 0.172 Uiso 1 calc R . . H23C H 1.0365 0.9268 0.4721 0.172 Uiso 1 calc R . . C24 C 0.9299(4) 0.9192(5) 0.4300(3) 0.082(2) Uani 1 d . . . C25 C 0.4583(2) 0.7371(3) 0.31536(17) 0.0198(9) Uani 1 d . . . C26 C 0.3969(2) 0.7938(3) 0.29003(18) 0.0265(10) Uani 1 d . . . H26 H 0.3788 0.8286 0.3154 0.032 Uiso 1 calc R . . C27 C 0.3620(2) 0.8001(3) 0.22861(19) 0.0303(10) Uani 1 d . . . H27 H 0.3214 0.8390 0.2138 0.036 Uiso 1 calc R . . C28 C 0.3862(2) 0.7502(3) 0.18940(18) 0.0264(10) Uani 1 d . . . H28 H 0.3613 0.7521 0.1483 0.032 Uiso 1 calc R . . C29 C 0.4483(2) 0.6970(3) 0.21229(17) 0.0247(9) Uani 1 d . . . H29 H 0.4671 0.6650 0.1865 0.030 Uiso 1 calc R . . C30 C 0.4829(2) 0.6910(2) 0.27414(18) 0.0214(9) Uani 1 d . . . H30 H 0.5246 0.6544 0.2885 0.026 Uiso 1 calc R . . C31 C 0.52894(19) 0.6108(3) 0.40390(16) 0.0170(9) Uani 1 d . . . C32 C 0.4949(2) 0.5377(3) 0.42616(16) 0.0198(9) Uani 1 d . . . H32 H 0.4547 0.5553 0.4348 0.024 Uiso 1 calc R . . C33 C 0.5188(2) 0.4398(3) 0.43590(16) 0.0200(9) Uani 1 d . . . H33 H 0.4942 0.3937 0.4504 0.024 Uiso 1 calc R . . C34 C 0.5780(2) 0.4107(3) 0.42436(17) 0.0215(9) Uani 1 d . . . H34 H 0.5939 0.3453 0.4309 0.026 Uiso 1 calc R . . C35 C 0.6137(2) 0.4796(3) 0.40296(16) 0.0229(9) Uani 1 d . . . H35 H 0.6537 0.4606 0.3945 0.027 Uiso 1 calc R . . C36 C 0.59004(19) 0.5784(3) 0.39369(16) 0.0175(9) Uani 1 d . . . H36 H 0.6159 0.6242 0.3803 0.021 Uiso 1 calc R . . C37 C 0.5690(2) 0.8021(3) 0.40988(17) 0.0193(9) Uani 1 d . . . C38 C 0.6276(2) 0.7858(3) 0.46153(17) 0.0235(9) Uani 1 d . . . H38 H 0.6278 0.7294 0.4842 0.028 Uiso 1 calc R . . C39 C 0.6857(2) 0.8490(3) 0.48118(19) 0.0294(10) Uani 1 d . . . H39 H 0.7236 0.8341 0.5159 0.035 Uiso 1 calc R . . C40 C 0.6870(2) 0.9342(3) 0.4490(2) 0.0341(11) Uani 1 d . . . H40 H 0.7258 0.9768 0.4613 0.041 Uiso 1 calc R . . C41 C 0.6294(2) 0.9545(3) 0.3981(2) 0.0327(11) Uani 1 d . . . H41 H 0.6291 1.0115 0.3759 0.039 Uiso 1 calc R . . C42 C 0.5717(2) 0.8901(3) 0.37984(18) 0.0268(10) Uani 1 d . . . H42 H 0.5332 0.9066 0.3460 0.032 Uiso 1 calc R . . C43 C 0.4469(2) 0.7563(3) 0.42508(17) 0.0198(9) Uani 1 d . . . C44 C 0.3799(2) 0.7126(3) 0.41160(18) 0.0249(9) Uani 1 d . . . H44 H 0.3657 0.6656 0.3810 0.030 Uiso 1 calc R . . C45 C 0.3337(2) 0.7358(3) 0.44129(18) 0.0263(10) Uani 1 d . . . H45 H 0.2905 0.7027 0.4314 0.032 Uiso 1 calc R . . C46 C 0.3511(2) 0.8076(3) 0.4855(2) 0.0336(11) Uani 1 d . . . H46 H 0.3197 0.8248 0.5048 0.040 Uiso 1 calc R . . C47 C 0.4157(2) 0.8527(3) 0.5003(2) 0.0345(11) Uani 1 d . . . H47 H 0.4287 0.9006 0.5304 0.041 Uiso 1 calc R . . C48 C 0.4630(2) 0.8276(3) 0.47038(18) 0.0267(10) Uani 1 d . . . H48 H 0.5065 0.8599 0.4813 0.032 Uiso 1 calc R . . C49 C 0.98974(18) 0.4314(3) 0.36628(16) 0.0166(8) Uani 1 d . . . C50 C 1.01620(19) 0.4617(3) 0.42660(17) 0.0181(9) Uani 1 d . . . H50 H 1.0040 0.4246 0.4546 0.022 Uiso 1 calc R . . C51 C 1.05921(19) 0.5431(3) 0.44636(17) 0.0201(9) Uani 1 d . . . H51 H 1.0755 0.5595 0.4869 0.024 Uiso 1 calc R . . C52 C 1.0784(2) 0.6010(3) 0.40632(18) 0.0218(9) Uani 1 d . . . H52 H 1.1088 0.6549 0.4197 0.026 Uiso 1 calc R . . C53 C 1.0517(2) 0.5771(3) 0.34609(18) 0.0231(9) Uani 1 d . . . H53 H 1.0625 0.6165 0.3183 0.028 Uiso 1 calc R . . C54 C 1.0085(2) 0.4940(3) 0.32700(17) 0.0188(9) Uani 1 d . . . H54 H 0.9913 0.4792 0.2862 0.023 Uiso 1 calc R . . C55 C 0.9012(2) 0.3279(2) 0.27264(18) 0.0186(9) Uani 1 d . . . C56 C 0.8278(2) 0.3422(3) 0.24519(18) 0.0252(10) Uani 1 d . . . H56 H 0.8005 0.3508 0.2694 0.030 Uiso 1 calc R . . C57 C 0.7945(2) 0.3442(3) 0.18328(18) 0.0266(10) Uani 1 d . . . H57 H 0.7456 0.3514 0.1670 0.032 Uiso 1 calc R . . C58 C 0.8334(2) 0.3355(3) 0.14535(18) 0.0233(10) Uani 1 d . . . H58 H 0.8113 0.3392 0.1039 0.028 Uiso 1 calc R . . C59 C 0.9060(2) 0.3212(2) 0.17074(18) 0.0227(9) Uani 1 d . . . H59 H 0.9332 0.3143 0.1463 0.027 Uiso 1 calc R . . C60 C 0.9381(2) 0.3171(2) 0.23268(17) 0.0202(9) Uani 1 d . . . H60 H 0.9868 0.3066 0.2485 0.024 Uiso 1 calc R . . C61 C 0.8865(2) 0.3207(3) 0.38073(17) 0.0204(9) Uani 1 d . . . C62 C 0.8717(2) 0.2356(3) 0.4071(2) 0.0387(12) Uani 1 d . . . H62 H 0.8960 0.1776 0.4054 0.046 Uiso 1 calc R . . C63 C 0.8226(3) 0.2324(4) 0.4358(2) 0.0514(14) Uani 1 d . . . H63 H 0.8150 0.1732 0.4528 0.062 Uiso 1 calc R . . C64 C 0.7848(2) 0.3163(3) 0.4394(2) 0.0384(12) Uani 1 d . . . H64 H 0.7519 0.3149 0.4589 0.046 Uiso 1 calc R . . C65 C 0.7975(2) 0.4020(3) 0.41344(19) 0.0299(11) Uani 1 d . . . H65 H 0.7727 0.4597 0.4149 0.036 Uiso 1 calc R . . C66 C 0.8467(2) 0.4028(3) 0.38517(18) 0.0254(10) Uani 1 d . . . H66 H 0.8538 0.4622 0.3679 0.031 Uiso 1 calc R . . C67 C 0.9973(2) 0.2315(3) 0.36476(17) 0.0192(9) Uani 1 d . . . C68 C 0.9822(2) 0.1410(3) 0.33267(18) 0.0224(9) Uani 1 d . . . H68 H 0.9415 0.1368 0.2987 0.027 Uiso 1 calc R . . C69 C 1.0255(2) 0.0581(3) 0.34981(19) 0.0267(10) Uani 1 d . . . H69 H 1.0136 0.0002 0.3271 0.032 Uiso 1 calc R . . C70 C 1.0852(2) 0.0603(3) 0.39939(18) 0.0277(10) Uani 1 d . . . H70 H 1.1141 0.0045 0.4104 0.033 Uiso 1 calc R . . C71 C 1.1027(2) 0.1461(3) 0.43318(19) 0.0264(10) Uani 1 d . . . H71 H 1.1433 0.1484 0.4673 0.032 Uiso 1 calc R . . C72 C 1.0587(2) 0.2298(3) 0.41561(18) 0.0232(9) Uani 1 d . . . H72 H 1.0710 0.2870 0.4390 0.028 Uiso 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 0.0153(3) 0.0209(3) 0.0206(3) 0.0058(2) 0.0062(2) 0.0054(2) N1 0.0200(19) 0.0225(17) 0.024(2) 0.0029(14) 0.0050(16) 0.0027(15) N2 0.0119(17) 0.0309(18) 0.0201(19) 0.0057(15) 0.0042(15) 0.0025(14) N3 0.028(2) 0.0147(16) 0.0192(19) 0.0024(13) 0.0075(16) 0.0041(14) N4 0.0213(19) 0.0214(17) 0.0212(19) 0.0023(14) 0.0064(15) 0.0023(14) N6 0.019(2) 0.034(2) 0.025(2) 0.0069(16) 0.0060(16) 0.0119(16) N7 0.108(5) 0.081(4) 0.095(5) 0.007(4) 0.000(4) -0.013(4) B1 0.018(2) 0.023(2) 0.015(2) 0.0019(18) 0.0029(19) 0.0055(19) B2 0.016(2) 0.020(2) 0.016(2) -0.0007(18) 0.0027(19) 0.0015(19) C1 0.018(2) 0.026(2) 0.025(2) 0.0051(18) 0.0043(19) 0.0008(17) C2 0.026(2) 0.021(2) 0.018(2) 0.0011(17) 0.0012(19) 0.0058(18) C3 0.031(3) 0.021(2) 0.020(2) 0.0030(17) 0.0077(19) 0.0003(19) C4 0.021(2) 0.021(2) 0.028(2) -0.0022(18) 0.0110(19) -0.0045(17) C5 0.015(2) 0.021(2) 0.023(2) 0.0020(17) 0.0054(18) 0.0009(16) C6 0.016(2) 0.046(3) 0.021(2) 0.0096(19) 0.0063(18) 0.0026(19) C7 0.018(2) 0.040(2) 0.022(2) 0.0031(19) -0.0003(19) 0.0047(19) C8 0.022(2) 0.023(2) 0.018(2) 0.0015(17) 0.0037(18) 0.0025(18) C9 0.021(2) 0.032(2) 0.023(3) 0.0036(18) -0.0015(19) 0.0054(19) C10 0.040(3) 0.021(2) 0.018(2) 0.0012(17) 0.006(2) 0.004(2) C11 0.034(3) 0.020(2) 0.016(2) -0.0022(16) 0.0108(19) 0.0032(18) C12 0.025(2) 0.022(2) 0.025(2) -0.0022(17) 0.0115(19) 0.0042(17) C13 0.025(2) 0.026(2) 0.035(3) -0.0028(19) 0.015(2) 0.0136(18) C14 0.038(3) 0.023(2) 0.035(3) -0.0032(19) 0.019(2) 0.006(2) C15 0.027(2) 0.025(2) 0.033(3) 0.0016(19) 0.008(2) -0.0087(19) C16 0.046(3) 0.036(3) 0.036(3) 0.003(2) 0.002(2) -0.007(2) C17 0.032(3) 0.025(2) 0.029(3) 0.0027(19) 0.011(2) 0.0025(19) C18 0.035(3) 0.032(2) 0.033(3) 0.0027(19) 0.019(2) -0.002(2) C21 0.022(2) 0.025(2) 0.022(2) 0.0053(17) 0.0064(18) 0.0077(18) C22 0.025(2) 0.022(2) 0.020(2) 0.0070(17) 0.0094(19) 0.0042(18) C23 0.094(6) 0.167(7) 0.079(6) 0.020(5) 0.026(5) -0.042(6) C24 0.093(6) 0.103(5) 0.045(4) 0.008(4) 0.019(4) -0.043(5) C25 0.020(2) 0.0150(19) 0.023(2) 0.0041(16) 0.0047(18) 0.0015(16) C26 0.026(2) 0.029(2) 0.026(2) 0.0007(19) 0.011(2) 0.0028(19) C27 0.020(2) 0.040(3) 0.027(3) 0.009(2) 0.0027(19) 0.007(2) C28 0.021(2) 0.036(2) 0.018(2) 0.0060(18) 0.0010(18) -0.0016(19) C29 0.033(3) 0.022(2) 0.018(2) 0.0018(17) 0.0091(19) -0.0006(19) C30 0.021(2) 0.015(2) 0.027(2) 0.0020(16) 0.0065(18) 0.0010(16) C31 0.014(2) 0.021(2) 0.010(2) -0.0013(15) -0.0038(16) 0.0007(16) C32 0.018(2) 0.028(2) 0.011(2) -0.0018(16) 0.0014(17) 0.0003(17) C33 0.023(2) 0.018(2) 0.016(2) 0.0013(16) 0.0045(18) -0.0026(17) C34 0.031(2) 0.0118(19) 0.016(2) -0.0001(16) 0.0012(19) 0.0040(17) C35 0.015(2) 0.032(2) 0.017(2) -0.0058(17) -0.0005(18) 0.0096(18) C36 0.015(2) 0.019(2) 0.015(2) 0.0003(16) 0.0013(17) 0.0000(16) C37 0.022(2) 0.020(2) 0.017(2) -0.0046(16) 0.0079(17) 0.0006(17) C38 0.026(2) 0.021(2) 0.021(2) -0.0016(17) 0.0054(18) 0.0025(18) C39 0.025(3) 0.033(2) 0.026(3) -0.0058(19) 0.003(2) 0.002(2) C40 0.031(3) 0.034(3) 0.041(3) -0.013(2) 0.017(2) -0.013(2) C41 0.044(3) 0.024(2) 0.033(3) 0.0003(19) 0.016(2) -0.008(2) C42 0.031(3) 0.026(2) 0.023(2) 0.0004(18) 0.009(2) -0.0004(19) C43 0.026(2) 0.0163(19) 0.015(2) 0.0059(16) 0.0043(18) 0.0105(17) C44 0.025(2) 0.027(2) 0.019(2) 0.0043(18) 0.0030(18) 0.0082(19) C45 0.024(2) 0.029(2) 0.029(3) 0.0118(19) 0.012(2) 0.0086(18) C46 0.039(3) 0.034(3) 0.036(3) 0.018(2) 0.023(2) 0.021(2) C47 0.044(3) 0.031(2) 0.034(3) -0.007(2) 0.021(2) 0.007(2) C48 0.030(3) 0.029(2) 0.023(2) -0.0006(18) 0.011(2) 0.0010(19) C49 0.011(2) 0.0197(19) 0.017(2) 0.0018(16) 0.0024(16) 0.0074(16) C50 0.014(2) 0.019(2) 0.021(2) -0.0005(16) 0.0057(17) 0.0002(16) C51 0.017(2) 0.023(2) 0.019(2) -0.0010(17) 0.0053(18) 0.0090(17) C52 0.019(2) 0.0154(19) 0.028(2) -0.0053(17) 0.0044(19) 0.0002(16) C53 0.026(2) 0.018(2) 0.026(2) 0.0064(17) 0.0097(19) 0.0005(17) C54 0.021(2) 0.0178(19) 0.016(2) -0.0025(16) 0.0047(17) 0.0028(16) C55 0.022(2) 0.0081(17) 0.024(2) -0.0046(15) 0.0059(18) -0.0048(16) C56 0.024(2) 0.020(2) 0.031(3) -0.0091(18) 0.009(2) 0.0010(18) C57 0.019(2) 0.030(2) 0.022(2) -0.0017(18) -0.0023(19) 0.0015(18) C58 0.025(2) 0.019(2) 0.017(2) -0.0011(16) -0.0038(19) -0.0032(18) C59 0.026(2) 0.016(2) 0.026(2) -0.0049(16) 0.009(2) -0.0045(17) C60 0.012(2) 0.022(2) 0.022(2) -0.0013(16) -0.0009(17) -0.0020(16) C61 0.014(2) 0.027(2) 0.015(2) 0.0017(16) -0.0007(17) -0.0033(17) C62 0.032(3) 0.033(3) 0.056(3) 0.014(2) 0.021(2) 0.007(2) C63 0.044(3) 0.060(4) 0.061(4) 0.025(3) 0.031(3) 0.001(3) C64 0.023(3) 0.058(3) 0.037(3) 0.000(2) 0.014(2) -0.005(2) C65 0.018(2) 0.042(3) 0.028(3) -0.014(2) 0.006(2) -0.005(2) C66 0.017(2) 0.032(2) 0.027(3) -0.0066(19) 0.0082(19) -0.0071(19) C67 0.017(2) 0.024(2) 0.019(2) 0.0037(16) 0.0085(18) -0.0009(16) C68 0.017(2) 0.022(2) 0.027(2) 0.0006(17) 0.0060(18) 0.0002(17) C69 0.034(3) 0.017(2) 0.034(3) 0.0019(18) 0.018(2) 0.0044(18) C70 0.029(3) 0.029(2) 0.029(3) 0.0128(19) 0.015(2) 0.0097(19) C71 0.022(2) 0.028(2) 0.027(2) 0.0089(19) 0.0060(19) 0.0048(18) C72 0.026(2) 0.019(2) 0.027(2) -0.0018(17) 0.0116(19) -0.0006(17) _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 N6 2.031(4) . ? Ni1 N1 2.069(3) . ? Ni1 N3 2.078(3) . ? Ni1 N2 2.079(3) . ? Ni1 N5 2.170(3) . ? Ni1 N4 2.196(3) . ? N1 C5 1.330(5) . ? N1 C1 1.358(4) . ? N2 C6 1.483(5) . ? N2 C13 1.486(5) . ? N2 C7 1.491(4) . ? N3 C12 1.341(5) . ? N3 C8 1.348(5) . ? N4 C17 1.485(5) . ? N4 C14 1.494(5) . ? N4 C15 1.496(5) . ? N5 C20 1.263(10) . ? N6 C22 1.131(5) . ? N7 C24 1.143(8) . ? B1 C43 1.639(6) . ? B1 C37 1.642(6) . ? B1 C31 1.651(5) . ? B1 C25 1.673(6) . ? B2 C61 1.626(6) . ? B2 C55 1.643(6) . ? B2 C67 1.651(5) . ? B2 C49 1.663(5) . ? C1 C2 1.376(6) . ? C1 H1 0.9300 . ? C2 C3 1.369(6) . ? C2 H2 0.9300 . ? C3 C4 1.393(5) . ? C3 H3 0.9300 . ? C4 C5 1.377(5) . ? C4 H4 0.9300 . ? C5 C6 1.522(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.500(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.381(5) . ? C9 C10 1.368(6) . ? C9 H9 0.9300 . ? C10 C11 1.364(6) . ? C10 H10 0.9300 . ? C11 C12 1.389(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.489(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.531(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.517(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19A C20 1.335(16) . ? C19 C20 1.46(2) . ? C21 C22 1.451(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C23 C24 1.498(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C25 C30 1.387(6) . ? C25 C26 1.396(5) . ? C26 C27 1.385(5) . ? C26 H26 0.9300 . ? C27 C28 1.367(6) . ? C27 H27 0.9300 . ? C28 C29 1.377(5) . ? C28 H28 0.9300 . ? C29 C30 1.393(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.402(5) . ? C31 C32 1.402(5) . ? C32 C33 1.394(5) . ? C32 H32 0.9300 . ? C33 C34 1.370(6) . ? C33 H33 0.9300 . ? C34 C35 1.372(5) . ? C34 H34 0.9300 . ? C35 C36 1.404(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.393(5) . ? C37 C38 1.392(5) . ? C38 C39 1.388(5) . ? C38 H38 0.9300 . ? C39 C40 1.382(6) . ? C39 H39 0.9300 . ? C40 C41 1.382(5) . ? C40 H40 0.9300 . ? C41 C42 1.390(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.393(5) . ? C43 C44 1.402(5) . ? C44 C45 1.383(6) . ? C44 H44 0.9300 . ? C45 C46 1.380(6) . ? C45 H45 0.9300 . ? C46 C47 1.365(6) . ? C46 H46 0.9300 . ? C47 C48 1.410(6) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.402(5) . ? C49 C50 1.404(5) . ? C50 C51 1.374(5) . ? C50 H50 0.9300 . ? C51 C52 1.384(5) . ? C51 H51 0.9300 . ? C52 C53 1.380(5) . ? C52 H52 0.9300 . ? C53 C54 1.391(5) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.400(6) . ? C55 C56 1.405(5) . ? C56 C57 1.389(5) . ? C56 H56 0.9300 . ? C57 C58 1.387(6) . ? C57 H57 0.9300 . ? C58 C59 1.387(5) . ? C58 H58 0.9300 . ? C59 C60 1.388(5) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.386(5) . ? C61 C66 1.390(5) . ? C62 C63 1.381(7) . ? C62 H62 0.9300 . ? C63 C64 1.380(6) . ? C63 H63 0.9300 . ? C64 C65 1.372(6) . ? C64 H64 0.9300 . ? C65 C66 1.374(6) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.396(5) . ? C67 C68 1.412(5) . ? C68 C69 1.387(5) . ? C68 H68 0.9300 . ? C69 C70 1.360(5) . ? C69 H69 0.9300 . ? C70 C71 1.379(5) . ? C70 H70 0.9300 . ? C71 C72 1.403(5) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ni1 N1 97.12(13) . . ? N6 Ni1 N3 98.43(14) . . ? N1 Ni1 N3 160.05(13) . . ? N6 Ni1 N2 179.11(13) . . ? N1 Ni1 N2 82.46(13) . . ? N3 Ni1 N2 81.80(13) . . ? N6 Ni1 N5 88.49(13) . . ? N1 Ni1 N5 84.63(12) . . ? N3 Ni1 N5 83.36(12) . . ? N2 Ni1 N5 90.69(12) . . ? N6 Ni1 N4 95.98(13) . . ? N1 Ni1 N4 92.26(12) . . ? N3 Ni1 N4 98.45(12) . . ? N2 Ni1 N4 84.83(12) . . ? N5 Ni1 N4 174.86(13) . . ? C5 N1 C1 118.6(4) . . ? C5 N1 Ni1 113.1(3) . . ? C1 N1 Ni1 127.9(3) . . ? C6 N2 C13 113.3(3) . . ? C6 N2 C7 111.9(3) . . ? C13 N2 C7 109.3(3) . . ? C6 N2 Ni1 107.4(2) . . ? C13 N2 Ni1 107.7(2) . . ? C7 N2 Ni1 107.1(2) . . ? C12 N3 C8 118.6(3) . . ? C12 N3 Ni1 128.5(3) . . ? C8 N3 Ni1 112.7(3) . . ? C17 N4 C14 108.9(3) . . ? C17 N4 C15 111.6(3) . . ? C14 N4 C15 108.8(3) . . ? C17 N4 Ni1 113.5(2) . . ? C14 N4 Ni1 101.3(2) . . ? C15 N4 Ni1 112.2(2) . . ? C20 N5 Ni1 140.5(5) . . ? C22 N6 Ni1 166.5(3) . . ? C43 B1 C37 109.2(3) . . ? C43 B1 C31 111.3(3) . . ? C37 B1 C31 109.3(3) . . ? C43 B1 C25 109.6(3) . . ? C37 B1 C25 109.2(3) . . ? C31 B1 C25 108.3(3) . . ? C61 B2 C55 110.5(3) . . ? C61 B2 C67 109.2(3) . . ? C55 B2 C67 109.9(3) . . ? C61 B2 C49 108.7(3) . . ? C55 B2 C49 109.7(3) . . ? C67 B2 C49 108.8(3) . . ? N1 C1 C2 121.5(4) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.4(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 117.2(4) . . ? C4 C5 C6 119.8(4) . . ? N2 C6 C5 112.4(3) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 109.9(3) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C9 120.7(4) . . ? N3 C8 C7 116.1(3) . . ? C9 C8 C7 123.1(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N3 C12 C11 122.4(4) . . ? N3 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? N2 C13 C14 111.5(3) . . ? N2 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N2 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 N4 111.3(3) . . ? C13 C14 H14A 109.4 . . ? N4 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? N4 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N4 C15 C16 115.4(3) . . ? N4 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N4 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? 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 . . ? N4 C17 C18 113.3(3) . . ? N4 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? N4 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C20 C19A 149.4(13) . . ? N5 C20 C19 129.5(13) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C21 177.6(4) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N7 C24 C23 176.6(8) . . ? C30 C25 C26 114.7(3) . . ? C30 C25 B1 121.7(3) . . ? C26 C25 B1 123.5(4) . . ? C27 C26 C25 122.5(4) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 118.3(4) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 123.3(4) . . ? C25 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? C36 C31 C32 114.8(3) . . ? C36 C31 B1 121.0(4) . . ? C32 C31 B1 124.2(3) . . ? C33 C32 C31 122.6(4) . . ? C33 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C34 C33 C32 120.7(4) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 118.9(3) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 122.5(4) . . ? C31 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C42 C37 C38 114.4(3) . . ? C42 C37 B1 123.5(3) . . ? C38 C37 B1 122.0(3) . . ? C39 C38 C37 123.8(4) . . ? C39 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 118.5(4) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 123.1(4) . . ? C41 C42 H42 118.4 . . ? C37 C42 H42 118.4 . . ? C48 C43 C44 114.3(4) . . ? C48 C43 B1 123.4(4) . . ? C44 C43 B1 122.3(3) . . ? C45 C44 C43 123.5(4) . . ? C45 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? C44 C45 C46 120.5(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 118.4(4) . . ? C47 C46 H46 120.8 . . ? C45 C46 H46 120.8 . . ? C46 C47 C48 120.8(4) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C43 C48 C47 122.5(4) . . ? C43 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C54 C49 C50 114.3(3) . . ? C54 C49 B2 124.4(3) . . ? C50 C49 B2 121.3(3) . . ? C51 C50 C49 123.4(4) . . ? C51 C50 H50 118.3 . . ? C49 C50 H50 118.3 . . ? C50 C51 C52 120.4(4) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C53 C52 C51 118.7(3) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C52 C53 C54 120.0(4) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C49 123.1(4) . . ? C53 C54 H54 118.4 . . ? C49 C54 H54 118.4 . . ? C60 C55 C56 114.7(3) . . ? C60 C55 B2 121.3(3) . . ? C56 C55 B2 124.0(4) . . ? C57 C56 C55 122.5(4) . . ? C57 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? C58 C57 C56 120.8(4) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 118.3(4) . . ? C57 C58 H58 120.8 . . ? C59 C58 H58 120.8 . . ? C60 C59 C58 119.9(4) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 123.7(4) . . ? C59 C60 H60 118.2 . . ? C55 C60 H60 118.2 . . ? C62 C61 C66 113.7(4) . . ? C62 C61 B2 125.1(4) . . ? C66 C61 B2 121.1(3) . . ? C63 C62 C61 123.5(5) . . ? C63 C62 H62 118.3 . . ? C61 C62 H62 118.3 . . ? C62 C63 C64 120.6(5) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C65 C64 C63 117.7(4) . . ? C65 C64 H64 121.1 . . ? C63 C64 H64 121.1 . . ? C64 C65 C66 120.3(4) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 124.1(4) . . ? C65 C66 H66 117.9 . . ? C61 C66 H66 117.9 . . ? C72 C67 C68 114.4(3) . . ? C72 C67 B2 123.6(3) . . ? C68 C67 B2 121.8(3) . . ? C69 C68 C67 122.6(4) . . ? C69 C68 H68 118.7 . . ? C67 C68 H68 118.7 . . ? C70 C69 C68 120.8(4) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C71 119.6(4) . . ? C69 C70 H70 120.2 . . ? C71 C70 H70 120.2 . . ? C70 C71 C72 119.4(4) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C67 C72 C71 123.2(4) . . ? C67 C72 H72 118.4 . . ? C71 C72 H72 118.4 . . ? _diffrn_measured_fraction_theta_max 0.831 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.831 _refine_diff_density_max 0.668 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.061 # Attachment '- 3.cif' data_20mpmbf _database_code_depnum_ccdc_archive 'CCDC 805449' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H138 B4 N14 Ni2' _chemical_formula_weight 2105.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.4952(12) _cell_length_b 17.3430(10) _cell_length_c 34.986(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.5370(10) _cell_angle_gamma 90.00 _cell_volume 11817.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5488 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.76 _exptl_crystal_description BLOCKS _exptl_crystal_colour PINK _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.8065 _exptl_absorpt_correction_T_max 0.8707 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58735 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20794 _reflns_number_gt 12409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+5.7682P] 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 20794 _refine_ls_number_parameters 1397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.2019 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0638(2) 0.1994(3) 0.08640(13) 0.0656(12) Uani 1 1 d . . . N2 N 0.0863(3) 0.1864(4) 0.02562(16) 0.0907(17) Uani 1 1 d . . . N3 N 0.0282(3) 0.3514(3) 0.08826(14) 0.0721(14) Uani 1 1 d . . . Ni1 Ni 0.02974(3) 0.26464(3) 0.130230(16) 0.04312(18) Uani 1 1 d . . . N4 N -0.0232(2) 0.3494(2) 0.15861(14) 0.0619(12) Uani 1 1 d . . . N5 N 0.1308(2) 0.3072(2) 0.14537(13) 0.0618(12) Uani 1 1 d . . . N6 N 0.0357(2) 0.1836(2) 0.17234(13) 0.0581(12) Uani 1 1 d . . . N7 N -0.0727(3) 0.2272(2) 0.11212(13) 0.0604(12) Uani 1 1 d . . . C1 C 0.0903(3) 0.1287(4) 0.08008(19) 0.0751(17) Uani 1 1 d . . . H1 H 0.0974 0.0914 0.0989 0.090 Uiso 1 1 calc R . . C2 C 0.1049(3) 0.1190(4) 0.0438(2) 0.0723(17) Uani 1 1 d . . . H2 H 0.1239 0.0755 0.0329 0.087 Uiso 1 1 calc R . . C3 C 0.0600(3) 0.2349(4) 0.05418(18) 0.0725(17) Uani 1 1 d . . . C4 C 0.0303(4) 0.3119(5) 0.04998(17) 0.101(3) Uani 1 1 d . . . H4A H -0.0158 0.3080 0.0386 0.121 Uiso 1 1 calc R . . H4B H 0.0576 0.3424 0.0330 0.121 Uiso 1 1 calc R . . C5 C -0.0339(4) 0.3978(4) 0.0933(2) 0.102(2) Uani 1 1 d . . . H5A H -0.0723 0.3745 0.0790 0.123 Uiso 1 1 calc R . . H5B H -0.0270 0.4491 0.0831 0.123 Uiso 1 1 calc R . . C6 C -0.0503(3) 0.4036(3) 0.1346(2) 0.082(2) Uani 1 1 d . . . C7 C -0.0934(5) 0.4575(5) 0.1483(4) 0.149(4) Uani 1 1 d . . . H7 H -0.1109 0.4933 0.1307 0.179 Uiso 1 1 calc R . . C8 C -0.1111(7) 0.4643(8) 0.1796(4) 0.195(7) Uani 1 1 d . . . H8 H -0.1396 0.5044 0.1867 0.234 Uiso 1 1 calc R . . C9 C -0.0861(5) 0.4069(5) 0.2063(3) 0.117(3) Uani 1 1 d . . . H9 H -0.0999 0.4075 0.2314 0.140 Uiso 1 1 calc R . . C10 C -0.0421(4) 0.3516(4) 0.1947(2) 0.089(2) Uani 1 1 d . . . H10 H -0.0250 0.3151 0.2121 0.106 Uiso 1 1 calc R . . C11 C 0.0892(4) 0.3990(5) 0.0975(2) 0.128(3) Uani 1 1 d . . . H11A H 0.1043 0.4213 0.0738 0.153 Uiso 1 1 calc R . . H11B H 0.0754 0.4413 0.1136 0.153 Uiso 1 1 calc R . . C12 C 0.1430(5) 0.3638(5) 0.1150(3) 0.166(5) Uani 1 1 d . . . H12A H 0.1728 0.4036 0.1260 0.199 Uiso 1 1 calc R . . H12B H 0.1683 0.3379 0.0955 0.199 Uiso 1 1 calc R . . C13 C 0.1854(3) 0.2500(4) 0.1447(2) 0.110(3) Uani 1 1 d . . . H13A H 0.2291 0.2753 0.1475 0.164 Uiso 1 1 calc R . . H13B H 0.1825 0.2228 0.1207 0.164 Uiso 1 1 calc R . . H13C H 0.1807 0.2141 0.1653 0.164 Uiso 1 1 calc R . . C14 C 0.1359(4) 0.3424(5) 0.1827(2) 0.130(3) Uani 1 1 d . . . H14A H 0.1208 0.3065 0.2014 0.195 Uiso 1 1 calc R . . H14B H 0.1076 0.3877 0.1828 0.195 Uiso 1 1 calc R . . H14C H 0.1828 0.3564 0.1887 0.195 Uiso 1 1 calc R . . C15 C 0.0410(3) 0.1369(3) 0.19430(15) 0.0530(13) Uani 1 1 d . . . C16 C 0.0484(3) 0.0754(3) 0.22304(15) 0.0713(17) Uani 1 1 d . . . H16A H 0.0117 0.0390 0.2193 0.107 Uiso 1 1 calc R . . H16B H 0.0470 0.0973 0.2482 0.107 Uiso 1 1 calc R . . H16C H 0.0916 0.0496 0.2204 0.107 Uiso 1 1 calc R . . C17 C -0.1280(3) 0.2125(3) 0.10381(15) 0.0542(13) Uani 1 1 d . . . C18 C -0.1984(3) 0.1956(4) 0.0931(2) 0.100(2) Uani 1 1 d . . . H18A H -0.2277 0.2179 0.1115 0.150 Uiso 1 1 calc R . . H18B H -0.2049 0.1408 0.0924 0.150 Uiso 1 1 calc R . . H18C H -0.2096 0.2170 0.0683 0.150 Uiso 1 1 calc R . . C19 C 0.0911(4) 0.2044(5) -0.0123(2) 0.141(4) Uani 1 1 d . . . H19A H 0.1218 0.1690 -0.0239 0.211 Uiso 1 1 calc R . . H19B H 0.1084 0.2560 -0.0146 0.211 Uiso 1 1 calc R . . H19C H 0.0465 0.2010 -0.0249 0.211 Uiso 1 1 calc R . . Ni2 Ni 0.48152(3) 0.73625(3) 0.625357(16) 0.04370(18) Uani 1 1 d . . . N8 N 0.4615(2) 0.8076(2) 0.57921(12) 0.0589(12) Uani 1 1 d . . . N9 N 0.4903(3) 0.8406(3) 0.52213(14) 0.0817(15) Uani 1 1 d . . . N10 N 0.5178(2) 0.6663(2) 0.58129(11) 0.0557(11) Uani 1 1 d . . . N11 N 0.5296(2) 0.6514(2) 0.65855(11) 0.0538(11) Uani 1 1 d . . . N12 N 0.3876(2) 0.6719(3) 0.61860(13) 0.0663(12) Uani 1 1 d . . . N13 N 0.5791(2) 0.7960(2) 0.63011(11) 0.0547(11) Uani 1 1 d . . . N14 N 0.4443(2) 0.8009(3) 0.66949(13) 0.0627(12) Uani 1 1 d . . . C20 C 0.4307(3) 0.8760(3) 0.56968(18) 0.0722(17) Uani 1 1 d . . . H20 H 0.4023 0.9035 0.5854 0.087 Uiso 1 1 calc R . . C21 C 0.4470(4) 0.8982(4) 0.5346(2) 0.091(2) Uani 1 1 d . . . H21 H 0.4326 0.9424 0.5215 0.109 Uiso 1 1 calc R . . C22 C 0.4981(3) 0.7878(3) 0.55017(16) 0.0572(14) Uani 1 1 d . . . C23 C 0.5422(3) 0.7176(3) 0.55064(14) 0.0664(16) Uani 1 1 d . . . H23A H 0.5383 0.6917 0.5261 0.080 Uiso 1 1 calc R . . H23B H 0.5899 0.7315 0.5559 0.080 Uiso 1 1 calc R . . C24 C 0.5719(4) 0.6162(3) 0.59716(16) 0.084(2) Uani 1 1 d . . . H24A H 0.6161 0.6391 0.5924 0.101 Uiso 1 1 calc R . . H24B H 0.5694 0.5670 0.5840 0.101 Uiso 1 1 calc R . . C25 C 0.5676(3) 0.6027(3) 0.63894(16) 0.0623(15) Uani 1 1 d . . . C26 C 0.6045(3) 0.5413(3) 0.65646(19) 0.0773(18) Uani 1 1 d . . . H26 H 0.6296 0.5079 0.6417 0.093 Uiso 1 1 calc R . . C27 C 0.6034(3) 0.5314(4) 0.6930(2) 0.0820(19) Uani 1 1 d . . . H27 H 0.6282 0.4918 0.7051 0.098 Uiso 1 1 calc R . . C28 C 0.5632(3) 0.5830(3) 0.71425(16) 0.0646(15) Uani 1 1 d . . . H28 H 0.5609 0.5770 0.7406 0.077 Uiso 1 1 calc R . . C29 C 0.5284(3) 0.6405(3) 0.69628(15) 0.0584(14) Uani 1 1 d . . . H29 H 0.5026 0.6739 0.7107 0.070 Uiso 1 1 calc R . . C30 C 0.4558(4) 0.6238(4) 0.56649(18) 0.098(2) Uani 1 1 d . . . H30A H 0.4328 0.6545 0.5466 0.118 Uiso 1 1 calc R . . H30B H 0.4704 0.5761 0.5549 0.118 Uiso 1 1 calc R . . C31 C 0.4080(4) 0.6062(4) 0.5946(2) 0.120(3) Uani 1 1 d . . . H31A H 0.4276 0.5663 0.6112 0.143 Uiso 1 1 calc R . . H31B H 0.3670 0.5850 0.5818 0.143 Uiso 1 1 calc R . . C32 C 0.3315(3) 0.7162(4) 0.6013(2) 0.111(3) Uani 1 1 d . . . H32A H 0.2914 0.6844 0.5985 0.166 Uiso 1 1 calc R . . H32B H 0.3440 0.7341 0.5765 0.166 Uiso 1 1 calc R . . H32C H 0.3221 0.7597 0.6172 0.166 Uiso 1 1 calc R . . C33 C 0.3628(4) 0.6408(5) 0.6548(2) 0.123(3) Uani 1 1 d . . . H33A H 0.3472 0.6824 0.6704 0.185 Uiso 1 1 calc R . . H33B H 0.3995 0.6139 0.6683 0.185 Uiso 1 1 calc R . . H33C H 0.3254 0.6058 0.6493 0.185 Uiso 1 1 calc R . . C34 C 0.6279(3) 0.8311(3) 0.63275(14) 0.0522(13) Uani 1 1 d . . . C35 C 0.6912(3) 0.8764(3) 0.63638(16) 0.0746(17) Uani 1 1 d . . . H35A H 0.7300 0.8423 0.6382 0.112 Uiso 1 1 calc R . . H35B H 0.6906 0.9077 0.6590 0.112 Uiso 1 1 calc R . . H35C H 0.6946 0.9090 0.6143 0.112 Uiso 1 1 calc R . . C36 C 0.4278(3) 0.8348(3) 0.69495(16) 0.0579(14) Uani 1 1 d . . . C37 C 0.4082(3) 0.8776(3) 0.72844(16) 0.0813(19) Uani 1 1 d . . . H37A H 0.3815 0.8451 0.7443 0.122 Uiso 1 1 calc R . . H37B H 0.3814 0.9217 0.7205 0.122 Uiso 1 1 calc R . . H37C H 0.4487 0.8944 0.7427 0.122 Uiso 1 1 calc R . . C38 C 0.5242(4) 0.8400(4) 0.48751(19) 0.114(3) Uani 1 1 d . . . H38A H 0.5724 0.8486 0.4926 0.171 Uiso 1 1 calc R . . H38B H 0.5059 0.8801 0.4711 0.171 Uiso 1 1 calc R . . H38C H 0.5175 0.7910 0.4752 0.171 Uiso 1 1 calc R . . B1 B 0.1770(3) 0.5840(3) 0.25138(15) 0.0421(13) Uani 1 1 d . . . B2 B 0.2785(3) 0.5107(3) 0.48407(15) 0.0408(13) Uani 1 1 d . . . B3 B 0.3354(3) 0.4175(3) 0.73347(15) 0.0424(13) Uani 1 1 d . . . B4 B 0.2215(3) 0.4920(3) 0.98702(16) 0.0499(15) Uani 1 1 d . . . C39 C 0.2300(2) 0.6462(2) 0.27241(13) 0.0423(11) Uani 1 1 d . . . C40 C 0.2657(3) 0.6305(3) 0.30676(14) 0.0549(13) Uani 1 1 d . . . H40 H 0.2578 0.5837 0.3188 0.066 Uiso 1 1 calc R . . C41 C 0.3125(3) 0.6814(4) 0.32383(17) 0.0730(17) Uani 1 1 d . . . H41 H 0.3351 0.6684 0.3469 0.088 Uiso 1 1 calc R . . C42 C 0.3255(4) 0.7497(4) 0.3071(2) 0.091(2) Uani 1 1 d . . . H42 H 0.3560 0.7845 0.3190 0.110 Uiso 1 1 calc R . . C43 C 0.2938(4) 0.7673(4) 0.2728(3) 0.100(2) Uani 1 1 d . . . H43 H 0.3032 0.8137 0.2608 0.120 Uiso 1 1 calc R . . C44 C 0.2475(3) 0.7161(3) 0.25575(17) 0.0729(17) Uani 1 1 d . . . H44 H 0.2271 0.7289 0.2321 0.087 Uiso 1 1 calc R . . C45 C 0.2257(2) 0.5340(3) 0.22328(14) 0.0440(12) Uani 1 1 d . . . C46 C 0.2615(2) 0.4675(3) 0.23459(14) 0.0491(12) Uani 1 1 d . . . H46 H 0.2553 0.4483 0.2590 0.059 Uiso 1 1 calc R . . C47 C 0.3055(3) 0.4290(3) 0.21173(17) 0.0612(15) Uani 1 1 d . . . H47 H 0.3285 0.3854 0.2209 0.073 Uiso 1 1 calc R . . C48 C 0.3154(3) 0.4547(4) 0.17560(19) 0.0782(18) Uani 1 1 d . . . H48 H 0.3444 0.4282 0.1598 0.094 Uiso 1 1 calc R . . C49 C 0.2823(3) 0.5199(4) 0.16294(17) 0.0794(18) Uani 1 1 d . . . H49 H 0.2895 0.5384 0.1385 0.095 Uiso 1 1 calc R . . C50 C 0.2382(3) 0.5587(3) 0.18614(16) 0.0644(15) Uani 1 1 d . . . H50 H 0.2160 0.6027 0.1767 0.077 Uiso 1 1 calc R . . C51 C 0.1146(2) 0.6266(3) 0.22630(13) 0.0482(12) Uani 1 1 d . . . C52 C 0.0793(3) 0.5895(3) 0.19614(15) 0.0643(15) Uani 1 1 d . . . H52 H 0.0926 0.5396 0.1902 0.077 Uiso 1 1 calc R . . C53 C 0.0257(3) 0.6219(4) 0.17440(17) 0.0808(18) Uani 1 1 d . . . H53 H 0.0046 0.5943 0.1543 0.097 Uiso 1 1 calc R . . C54 C 0.0040(3) 0.6956(5) 0.18276(19) 0.093(2) Uani 1 1 d . . . H54 H -0.0311 0.7191 0.1681 0.112 Uiso 1 1 calc R . . C55 C 0.0357(4) 0.7331(4) 0.2133(2) 0.111(3) Uani 1 1 d . . . H55 H 0.0209 0.7821 0.2199 0.133 Uiso 1 1 calc R . . C56 C 0.0892(3) 0.6992(3) 0.23445(17) 0.0785(19) Uani 1 1 d . . . H56 H 0.1091 0.7262 0.2550 0.094 Uiso 1 1 calc R . . C57 C 0.1383(2) 0.5316(2) 0.28304(14) 0.0433(11) Uani 1 1 d . . . C58 C 0.1168(3) 0.4558(3) 0.27675(16) 0.0594(14) Uani 1 1 d . . . H58 H 0.1281 0.4316 0.2541 0.071 Uiso 1 1 calc R . . C59 C 0.0793(3) 0.4148(3) 0.3028(2) 0.0770(18) Uani 1 1 d . . . H59 H 0.0660 0.3644 0.2974 0.092 Uiso 1 1 calc R . . C60 C 0.0619(3) 0.4476(4) 0.3360(2) 0.0818(19) Uani 1 1 d . . . H60 H 0.0371 0.4199 0.3535 0.098 Uiso 1 1 calc R . . C61 C 0.0815(3) 0.5226(4) 0.34378(16) 0.0692(16) Uani 1 1 d . . . H61 H 0.0699 0.5458 0.3666 0.083 Uiso 1 1 calc R . . C62 C 0.1180(2) 0.5628(3) 0.31779(14) 0.0519(13) Uani 1 1 d . . . H62 H 0.1301 0.6135 0.3235 0.062 Uiso 1 1 calc R . . C63 C 0.3288(2) 0.4701(2) 0.51741(12) 0.0372(11) Uani 1 1 d . . . C64 C 0.3072(3) 0.4324(3) 0.54970(13) 0.0508(13) Uani 1 1 d . . . H64 H 0.2608 0.4343 0.5548 0.061 Uiso 1 1 calc R . . C65 C 0.3511(3) 0.3919(3) 0.57486(14) 0.0617(15) Uani 1 1 d . . . H65 H 0.3341 0.3687 0.5965 0.074 Uiso 1 1 calc R . . C66 C 0.4196(3) 0.3862(3) 0.56770(15) 0.0606(15) Uani 1 1 d . . . H66 H 0.4491 0.3584 0.5841 0.073 Uiso 1 1 calc R . . C67 C 0.4442(3) 0.4222(3) 0.53588(15) 0.0539(13) Uani 1 1 d . . . H67 H 0.4905 0.4190 0.5307 0.065 Uiso 1 1 calc R . . C68 C 0.3989(2) 0.4631(2) 0.51177(13) 0.0428(11) Uani 1 1 d . . . H68 H 0.4164 0.4874 0.4906 0.051 Uiso 1 1 calc R . . C69 C 0.3162(2) 0.5898(2) 0.46904(12) 0.0399(11) Uani 1 1 d . . . C70 C 0.3083(3) 0.6613(3) 0.48697(14) 0.0535(13) Uani 1 1 d . . . H70 H 0.2803 0.6641 0.5077 0.064 Uiso 1 1 calc R . . C71 C 0.3401(3) 0.7276(3) 0.47527(19) 0.0736(17) Uani 1 1 d . . . H71 H 0.3339 0.7734 0.4885 0.088 Uiso 1 1 calc R . . C72 C 0.3807(3) 0.7268(4) 0.4443(2) 0.0792(19) Uani 1 1 d . . . H72 H 0.4008 0.7718 0.4357 0.095 Uiso 1 1 calc R . . C73 C 0.3908(3) 0.6577(4) 0.42642(17) 0.0687(17) Uani 1 1 d . . . H73 H 0.4194 0.6553 0.4059 0.082 Uiso 1 1 calc R . . C74 C 0.3589(2) 0.5917(3) 0.43860(14) 0.0515(13) Uani 1 1 d . . . H74 H 0.3665 0.5460 0.4256 0.062 Uiso 1 1 calc R . . C75 C 0.2664(2) 0.4457(3) 0.45020(13) 0.0431(11) Uani 1 1 d . . . C76 C 0.2472(3) 0.4632(3) 0.41235(14) 0.0559(14) Uani 1 1 d . . . H76 H 0.2444 0.5148 0.4052 0.067 Uiso 1 1 calc R . . C77 C 0.2322(3) 0.4075(3) 0.38500(15) 0.0672(16) Uani 1 1 d . . . H77 H 0.2197 0.4222 0.3601 0.081 Uiso 1 1 calc R . . C78 C 0.2355(3) 0.3306(4) 0.39430(17) 0.0758(18) Uani 1 1 d . . . H78 H 0.2256 0.2929 0.3760 0.091 Uiso 1 1 calc R . . C79 C 0.2537(3) 0.3109(3) 0.43125(16) 0.0682(16) Uani 1 1 d . . . H79 H 0.2557 0.2592 0.4382 0.082 Uiso 1 1 calc R . . C80 C 0.2692(3) 0.3669(3) 0.45820(14) 0.0517(13) Uani 1 1 d . . . H80 H 0.2821 0.3515 0.4829 0.062 Uiso 1 1 calc R . . C81 C 0.2032(2) 0.5360(2) 0.49994(14) 0.0443(12) Uani 1 1 d . . . C82 C 0.1946(3) 0.5649(3) 0.53679(15) 0.0535(13) Uani 1 1 d . . . H82 H 0.2329 0.5681 0.5535 0.064 Uiso 1 1 calc R . . C83 C 0.1322(3) 0.5891(3) 0.54951(18) 0.0724(17) Uani 1 1 d . . . H83 H 0.1289 0.6065 0.5745 0.087 Uiso 1 1 calc R . . C84 C 0.0751(3) 0.5872(4) 0.5252(2) 0.088(2) Uani 1 1 d . . . H84 H 0.0330 0.6038 0.5336 0.105 Uiso 1 1 calc R . . C85 C 0.0802(3) 0.5610(4) 0.4887(2) 0.0811(18) Uani 1 1 d . . . H85 H 0.0419 0.5606 0.4719 0.097 Uiso 1 1 calc R . . C86 C 0.1430(3) 0.5351(3) 0.47704(16) 0.0593(14) Uani 1 1 d . . . H86 H 0.1451 0.5159 0.4523 0.071 Uiso 1 1 calc R . . C87 C 0.3841(2) 0.4712(2) 0.76286(13) 0.0389(11) Uani 1 1 d . . . C88 C 0.4196(3) 0.4404(3) 0.79437(14) 0.0526(13) Uani 1 1 d . . . H88 H 0.4139 0.3882 0.7994 0.063 Uiso 1 1 calc R . . C89 C 0.4631(3) 0.4822(3) 0.81889(15) 0.0629(15) Uani 1 1 d . . . H89 H 0.4854 0.4584 0.8397 0.076 Uiso 1 1 calc R . . C90 C 0.4729(3) 0.5590(3) 0.81212(16) 0.0601(15) Uani 1 1 d . . . H90 H 0.5017 0.5879 0.8284 0.072 Uiso 1 1 calc R . . C91 C 0.4399(3) 0.5926(3) 0.78132(16) 0.0576(14) Uani 1 1 d . . . H91 H 0.4467 0.6446 0.7763 0.069 Uiso 1 1 calc R . . C92 C 0.3966(3) 0.5497(3) 0.75761(14) 0.0554(14) Uani 1 1 d . . . H92 H 0.3745 0.5743 0.7369 0.067 Uiso 1 1 calc R . . C93 C 0.2799(2) 0.4706(2) 0.70811(14) 0.0439(12) Uani 1 1 d . . . C94 C 0.2439(3) 0.5309(3) 0.72350(15) 0.0567(14) Uani 1 1 d . . . H94 H 0.2528 0.5435 0.7491 0.068 Uiso 1 1 calc R . . C95 C 0.1950(3) 0.5736(3) 0.7027(2) 0.0760(18) Uani 1 1 d . . . H95 H 0.1729 0.6144 0.7142 0.091 Uiso 1 1 calc R . . C96 C 0.1790(3) 0.5561(4) 0.6651(2) 0.084(2) Uani 1 1 d . . . H96 H 0.1456 0.5838 0.6512 0.101 Uiso 1 1 calc R . . C97 C 0.2132(3) 0.4971(4) 0.64838(17) 0.0738(17) Uani 1 1 d . . . H97 H 0.2034 0.4849 0.6228 0.089 Uiso 1 1 calc R . . C98 C 0.2629(3) 0.4548(3) 0.66964(15) 0.0561(14) Uani 1 1 d . . . H98 H 0.2853 0.4147 0.6577 0.067 Uiso 1 1 calc R . . C99 C 0.3862(2) 0.3703(2) 0.70558(12) 0.0416(11) Uani 1 1 d . . . C100 C 0.4487(3) 0.3976(3) 0.69468(14) 0.0597(14) Uani 1 1 d . . . H100 H 0.4622 0.4464 0.7031 0.072 Uiso 1 1 calc R . . C101 C 0.4921(3) 0.3578(4) 0.67238(16) 0.0720(17) Uani 1 1 d . . . H101 H 0.5335 0.3803 0.6661 0.086 Uiso 1 1 calc R . . C102 C 0.4766(3) 0.2869(4) 0.65923(16) 0.0689(16) Uani 1 1 d . . . H102 H 0.5076 0.2592 0.6452 0.083 Uiso 1 1 calc R . . C103 C 0.4141(4) 0.2566(3) 0.66693(15) 0.0705(17) Uani 1 1 d . . . H103 H 0.4009 0.2089 0.6570 0.085 Uiso 1 1 calc R . . C104 C 0.3704(3) 0.2979(3) 0.68986(14) 0.0626(15) Uani 1 1 d . . . H104 H 0.3282 0.2761 0.6950 0.075 Uiso 1 1 calc R . . C105 C 0.2910(2) 0.3536(3) 0.75790(12) 0.0439(12) Uani 1 1 d . . . C106 C 0.2224(3) 0.3602(3) 0.76379(15) 0.0674(16) Uani 1 1 d . . . H106 H 0.1996 0.4042 0.7548 0.081 Uiso 1 1 calc R . . C107 C 0.1847(3) 0.3044(4) 0.78253(18) 0.086(2) Uani 1 1 d . . . H107 H 0.1382 0.3123 0.7859 0.104 Uiso 1 1 calc R . . C108 C 0.2146(3) 0.2396(4) 0.79571(17) 0.0786(19) Uani 1 1 d . . . H108 H 0.1890 0.2020 0.8075 0.094 Uiso 1 1 calc R . . C109 C 0.2843(3) 0.2298(3) 0.79136(15) 0.0655(15) Uani 1 1 d . . . H109 H 0.3064 0.1860 0.8011 0.079 Uiso 1 1 calc R . . C110 C 0.3209(3) 0.2851(3) 0.77257(14) 0.0544(13) Uani 1 1 d . . . H110 H 0.3675 0.2768 0.7694 0.065 Uiso 1 1 calc R . . C111 C 0.1950(3) 0.5670(3) 1.01179(16) 0.0581(14) Uani 1 1 d . . . C112 C 0.1792(3) 0.5613(3) 1.05009(16) 0.0683(16) Uani 1 1 d . . . H112 H 0.1858 0.5140 1.0623 0.082 Uiso 1 1 calc R . . C113 C 0.1544(3) 0.6221(4) 1.07095(18) 0.084(2) Uani 1 1 d . . . H113 H 0.1448 0.6151 1.0965 0.101 Uiso 1 1 calc R . . C114 C 0.1437(4) 0.6929(4) 1.0542(2) 0.099(2) Uani 1 1 d . . . H114 H 0.1269 0.7340 1.0680 0.119 Uiso 1 1 calc R . . C115 C 0.1584(4) 0.7013(3) 1.0166(2) 0.103(2) Uani 1 1 d . . . H115 H 0.1516 0.7488 1.0047 0.123 Uiso 1 1 calc R . . C116 C 0.1831(4) 0.6401(3) 0.99606(18) 0.085(2) Uani 1 1 d . . . H116 H 0.1923 0.6480 0.9705 0.102 Uiso 1 1 calc R . . C117 C 0.2738(3) 0.5189(3) 0.95396(15) 0.0561(14) Uani 1 1 d . . . C118 C 0.2503(4) 0.5614(3) 0.92194(17) 0.0779(19) Uani 1 1 d . . . H118 H 0.2038 0.5735 0.9196 0.094 Uiso 1 1 calc R . . C119 C 0.2923(5) 0.5863(3) 0.89374(18) 0.091(2) Uani 1 1 d . . . H119 H 0.2738 0.6143 0.8731 0.109 Uiso 1 1 calc R . . C120 C 0.3605(5) 0.5701(4) 0.8960(2) 0.098(3) Uani 1 1 d . . . H120 H 0.3890 0.5875 0.8773 0.118 Uiso 1 1 calc R . . C121 C 0.3867(4) 0.5280(4) 0.9261(2) 0.094(2) Uani 1 1 d . . . H121 H 0.4332 0.5158 0.9277 0.113 Uiso 1 1 calc R . . C122 C 0.3438(3) 0.5030(3) 0.95459(15) 0.0711(16) Uani 1 1 d . . . H122 H 0.3629 0.4745 0.9749 0.085 Uiso 1 1 calc R . . C123 C 0.1547(3) 0.4492(3) 0.96566(13) 0.0476(12) Uani 1 1 d . . . C124 C 0.1636(3) 0.3984(3) 0.93505(15) 0.0638(15) Uani 1 1 d . . . H124 H 0.2077 0.3910 0.9267 0.077 Uiso 1 1 calc R . . C125 C 0.1096(3) 0.3585(3) 0.91656(16) 0.0719(17) Uani 1 1 d . . . H125 H 0.1179 0.3255 0.8963 0.086 Uiso 1 1 calc R . . C126 C 0.0442(3) 0.3683(3) 0.92843(17) 0.0702(16) Uani 1 1 d . . . H126 H 0.0077 0.3420 0.9163 0.084 Uiso 1 1 calc R . . C127 C 0.0329(3) 0.4165(3) 0.95799(16) 0.0608(14) Uani 1 1 d . . . H127 H -0.0114 0.4229 0.9663 0.073 Uiso 1 1 calc R . . C128 C 0.0870(3) 0.4564(3) 0.97605(14) 0.0510(13) Uani 1 1 d . . . H128 H 0.0774 0.4896 0.9960 0.061 Uiso 1 1 calc R . . C129 C 0.2606(3) 0.4304(3) 1.01664(13) 0.0482(12) Uani 1 1 d . . . C130 C 0.2498(3) 0.3513(3) 1.01639(15) 0.0582(14) Uani 1 1 d . . . H130 H 0.2180 0.3309 0.9985 0.070 Uiso 1 1 calc R . . C131 C 0.2839(3) 0.3013(3) 1.04146(18) 0.0757(18) Uani 1 1 d . . . H131 H 0.2746 0.2488 1.0403 0.091 Uiso 1 1 calc R . . C132 C 0.3320(4) 0.3293(4) 1.06826(17) 0.0777(18) Uani 1 1 d . . . H132 H 0.3554 0.2960 1.0851 0.093 Uiso 1 1 calc R . . C133 C 0.3442(3) 0.4058(4) 1.06943(16) 0.0758(17) Uani 1 1 d . . . H133 H 0.3764 0.4255 1.0872 0.091 Uiso 1 1 calc R . . C134 C 0.3092(3) 0.4555(3) 1.04439(16) 0.0613(15) Uani 1 1 d . . . H134 H 0.3186 0.5080 1.0462 0.074 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 N1 0.054(3) 0.091(4) 0.051(3) -0.010(3) 0.001(2) -0.007(3) N2 0.067(4) 0.144(5) 0.061(4) -0.016(4) 0.002(3) -0.033(4) N3 0.073(4) 0.070(3) 0.072(4) 0.036(3) -0.008(3) -0.017(3) Ni1 0.0423(4) 0.0419(3) 0.0448(4) 0.0084(3) -0.0008(3) -0.0024(3) N4 0.054(3) 0.055(3) 0.078(3) -0.002(2) 0.014(3) 0.004(2) N5 0.048(3) 0.068(3) 0.068(3) 0.001(2) -0.007(2) -0.015(2) N6 0.056(3) 0.056(3) 0.061(3) 0.016(2) -0.009(2) -0.003(2) N7 0.059(3) 0.053(3) 0.069(3) 0.003(2) -0.005(3) -0.009(2) C1 0.063(4) 0.087(5) 0.074(5) -0.020(4) -0.004(3) 0.007(3) C2 0.061(4) 0.069(4) 0.087(5) -0.019(4) -0.002(4) 0.013(3) C3 0.064(4) 0.097(5) 0.057(4) -0.005(4) 0.011(3) -0.018(4) C4 0.110(6) 0.149(7) 0.042(4) 0.043(4) -0.010(4) -0.051(5) C5 0.130(7) 0.059(4) 0.115(6) 0.032(4) -0.030(5) 0.007(4) C6 0.070(4) 0.046(3) 0.128(6) -0.017(4) -0.014(4) 0.010(3) C7 0.108(7) 0.086(6) 0.250(13) -0.078(8) -0.027(8) 0.035(5) C8 0.195(14) 0.186(13) 0.210(15) -0.119(11) 0.092(12) -0.047(11) C9 0.133(8) 0.120(7) 0.102(7) -0.023(5) 0.050(6) -0.004(6) C10 0.086(5) 0.082(4) 0.099(6) -0.010(4) 0.027(4) 0.006(4) C11 0.114(7) 0.130(7) 0.136(7) 0.071(6) -0.035(6) -0.067(6) C12 0.092(7) 0.173(9) 0.228(11) 0.103(8) -0.048(7) -0.084(6) C13 0.047(4) 0.143(6) 0.137(7) -0.042(5) -0.023(4) 0.013(4) C14 0.082(6) 0.183(8) 0.123(7) -0.085(6) -0.009(5) -0.034(5) C15 0.046(3) 0.055(3) 0.057(3) 0.004(3) -0.011(3) -0.002(3) C16 0.062(4) 0.079(4) 0.071(4) 0.042(3) -0.018(3) -0.009(3) C17 0.054(4) 0.051(3) 0.057(3) 0.003(2) 0.000(3) -0.008(3) C18 0.056(4) 0.124(6) 0.117(6) 0.004(5) -0.021(4) -0.029(4) C19 0.121(8) 0.188(9) 0.117(7) -0.042(6) 0.044(6) -0.066(7) Ni2 0.0452(4) 0.0449(3) 0.0408(4) -0.0084(3) 0.0002(3) 0.0037(3) N8 0.065(3) 0.054(3) 0.058(3) 0.002(2) -0.002(2) 0.015(2) N9 0.081(4) 0.102(4) 0.062(3) 0.019(3) -0.004(3) -0.005(3) N10 0.080(3) 0.047(2) 0.039(2) -0.013(2) -0.003(2) 0.018(2) N11 0.055(3) 0.066(3) 0.040(3) 0.007(2) -0.002(2) -0.011(2) N12 0.059(3) 0.076(3) 0.064(3) -0.006(3) -0.004(3) -0.015(3) N13 0.061(3) 0.054(3) 0.049(3) -0.006(2) -0.001(2) -0.003(2) N14 0.045(3) 0.072(3) 0.071(3) -0.022(3) 0.011(2) 0.000(2) C20 0.077(4) 0.061(4) 0.079(4) 0.017(3) 0.008(4) 0.022(3) C21 0.090(5) 0.074(4) 0.109(6) 0.022(4) 0.011(4) 0.032(4) C22 0.057(4) 0.060(3) 0.053(4) 0.014(3) -0.012(3) 0.006(3) C23 0.091(5) 0.075(4) 0.035(3) -0.002(3) 0.018(3) 0.011(3) C24 0.121(6) 0.069(4) 0.062(4) 0.000(3) 0.009(4) 0.053(4) C25 0.071(4) 0.050(3) 0.066(4) 0.007(3) -0.001(3) 0.005(3) C26 0.083(5) 0.075(4) 0.073(5) 0.016(3) -0.002(4) -0.009(3) C27 0.066(4) 0.092(5) 0.087(5) 0.021(4) -0.009(4) -0.020(4) C28 0.050(4) 0.091(4) 0.053(4) 0.004(3) 0.010(3) 0.002(3) C29 0.044(3) 0.078(4) 0.052(4) 0.012(3) -0.003(3) 0.002(3) C30 0.148(7) 0.079(4) 0.067(4) -0.027(4) -0.001(5) -0.044(5) C31 0.117(7) 0.100(6) 0.141(7) -0.046(5) -0.001(6) -0.053(5) C32 0.051(4) 0.123(6) 0.155(7) 0.012(5) -0.027(5) -0.013(4) C33 0.081(5) 0.168(7) 0.120(6) 0.045(5) -0.009(5) -0.062(5) C34 0.062(4) 0.051(3) 0.044(3) 0.003(2) 0.002(3) -0.003(3) C35 0.065(4) 0.079(4) 0.081(4) 0.010(3) 0.016(3) -0.014(3) C36 0.045(3) 0.063(3) 0.067(4) -0.017(3) 0.012(3) 0.003(3) C37 0.069(4) 0.107(5) 0.069(4) -0.036(3) 0.018(3) 0.013(4) C38 0.106(6) 0.150(7) 0.085(5) 0.036(5) 0.005(5) -0.028(5) B1 0.038(3) 0.045(3) 0.043(3) -0.005(3) -0.006(3) 0.003(3) B2 0.034(3) 0.043(3) 0.046(3) 0.001(2) -0.004(3) 0.005(2) B3 0.039(3) 0.045(3) 0.042(3) 0.004(2) -0.002(3) -0.005(3) B4 0.058(4) 0.043(3) 0.049(4) -0.005(3) 0.008(3) -0.010(3) C39 0.037(3) 0.041(3) 0.049(3) -0.004(2) -0.003(2) 0.008(2) C40 0.040(3) 0.068(3) 0.056(3) -0.003(3) -0.005(3) 0.001(3) C41 0.044(4) 0.110(5) 0.063(4) -0.019(4) -0.013(3) -0.017(3) C42 0.074(5) 0.074(5) 0.125(6) -0.034(4) -0.009(4) -0.033(4) C43 0.099(6) 0.054(4) 0.144(7) 0.006(4) -0.022(5) -0.027(4) C44 0.074(4) 0.059(4) 0.083(4) 0.013(3) -0.019(3) -0.010(3) C45 0.037(3) 0.044(3) 0.051(3) -0.010(2) -0.007(2) 0.001(2) C46 0.036(3) 0.056(3) 0.055(3) -0.012(3) -0.006(2) 0.004(2) C47 0.047(3) 0.060(3) 0.075(4) -0.015(3) -0.002(3) 0.013(3) C48 0.058(4) 0.093(5) 0.084(5) -0.030(4) 0.010(4) 0.012(4) C49 0.083(5) 0.096(5) 0.060(4) -0.009(3) 0.016(3) 0.009(4) C50 0.057(4) 0.072(4) 0.065(4) -0.001(3) 0.007(3) 0.016(3) C51 0.041(3) 0.057(3) 0.046(3) -0.009(2) 0.000(2) 0.003(2) C52 0.057(4) 0.067(3) 0.068(4) -0.014(3) -0.018(3) 0.005(3) C53 0.063(4) 0.113(5) 0.064(4) -0.003(4) -0.028(3) 0.004(4) C54 0.069(5) 0.138(6) 0.071(5) 0.003(4) -0.023(4) 0.047(4) C55 0.109(6) 0.119(6) 0.101(6) -0.020(5) -0.035(5) 0.078(5) C56 0.076(4) 0.079(4) 0.077(4) -0.027(3) -0.031(3) 0.041(3) C57 0.031(3) 0.039(3) 0.060(3) -0.008(2) -0.004(2) 0.007(2) C58 0.049(3) 0.047(3) 0.082(4) -0.016(3) 0.001(3) -0.001(3) C59 0.052(4) 0.048(3) 0.131(6) 0.005(4) 0.001(4) -0.010(3) C60 0.060(4) 0.083(5) 0.103(6) 0.028(4) 0.012(4) -0.006(4) C61 0.054(4) 0.086(4) 0.068(4) 0.007(3) 0.008(3) -0.001(3) C62 0.040(3) 0.052(3) 0.064(4) -0.004(3) 0.003(3) -0.004(2) C63 0.040(3) 0.032(2) 0.040(3) -0.005(2) -0.001(2) 0.001(2) C64 0.051(3) 0.051(3) 0.050(3) 0.005(2) 0.006(3) 0.008(3) C65 0.082(5) 0.060(3) 0.044(3) 0.013(3) 0.004(3) 0.013(3) C66 0.066(4) 0.060(3) 0.054(4) 0.005(3) -0.021(3) 0.017(3) C67 0.046(3) 0.052(3) 0.063(4) -0.001(3) -0.009(3) 0.005(3) C68 0.046(3) 0.045(3) 0.037(3) 0.000(2) -0.007(2) -0.002(2) C69 0.031(3) 0.047(3) 0.041(3) 0.004(2) -0.011(2) 0.005(2) C70 0.051(3) 0.053(3) 0.056(3) 0.001(3) -0.005(3) -0.009(3) C71 0.080(5) 0.050(3) 0.088(5) -0.002(3) -0.020(4) -0.009(3) C72 0.065(4) 0.072(4) 0.099(5) 0.043(4) -0.021(4) -0.016(4) C73 0.048(4) 0.086(4) 0.071(4) 0.040(4) -0.006(3) 0.002(3) C74 0.044(3) 0.057(3) 0.054(3) 0.016(3) -0.001(3) 0.009(3) C75 0.037(3) 0.049(3) 0.043(3) 0.000(2) -0.003(2) -0.001(2) C76 0.058(4) 0.057(3) 0.052(3) -0.005(3) -0.014(3) 0.004(3) C77 0.072(4) 0.083(4) 0.045(3) -0.005(3) -0.013(3) 0.004(3) C78 0.095(5) 0.077(4) 0.055(4) -0.023(3) -0.009(3) -0.012(4) C79 0.096(5) 0.052(3) 0.057(4) -0.009(3) 0.004(3) -0.011(3) C80 0.058(3) 0.052(3) 0.044(3) -0.002(2) -0.003(3) -0.006(3) C81 0.038(3) 0.041(3) 0.053(3) 0.008(2) -0.001(2) -0.002(2) C82 0.053(3) 0.045(3) 0.063(4) -0.007(3) 0.004(3) 0.003(2) C83 0.078(5) 0.058(3) 0.083(4) 0.003(3) 0.028(4) 0.021(3) C84 0.053(4) 0.085(5) 0.127(7) 0.024(4) 0.024(5) 0.028(4) C85 0.050(4) 0.097(5) 0.097(5) 0.016(4) -0.004(4) 0.006(3) C86 0.043(3) 0.064(3) 0.070(4) 0.010(3) -0.004(3) 0.001(3) C87 0.031(3) 0.042(3) 0.044(3) 0.003(2) 0.011(2) 0.002(2) C88 0.052(3) 0.046(3) 0.060(3) 0.004(3) -0.003(3) -0.006(2) C89 0.056(4) 0.067(4) 0.064(4) 0.000(3) -0.013(3) 0.002(3) C90 0.049(3) 0.068(4) 0.063(4) -0.024(3) 0.007(3) -0.011(3) C91 0.067(4) 0.045(3) 0.062(4) -0.007(3) 0.016(3) -0.014(3) C92 0.065(4) 0.053(3) 0.048(3) 0.009(3) 0.009(3) -0.003(3) C93 0.038(3) 0.040(3) 0.054(3) 0.011(2) 0.004(2) -0.001(2) C94 0.052(3) 0.066(3) 0.053(3) 0.008(3) 0.005(3) 0.009(3) C95 0.055(4) 0.082(4) 0.092(5) 0.029(4) 0.010(4) 0.024(3) C96 0.057(4) 0.105(5) 0.089(5) 0.038(4) -0.012(4) 0.019(4) C97 0.068(4) 0.085(4) 0.066(4) 0.020(3) -0.016(3) -0.008(4) C98 0.055(4) 0.056(3) 0.058(4) 0.004(3) -0.003(3) -0.003(3) C99 0.042(3) 0.040(3) 0.043(3) 0.008(2) 0.000(2) -0.002(2) C100 0.059(4) 0.057(3) 0.065(4) -0.009(3) 0.018(3) -0.014(3) C101 0.054(4) 0.088(4) 0.076(4) -0.020(3) 0.021(3) -0.009(3) C102 0.062(4) 0.078(4) 0.068(4) 0.001(3) 0.019(3) 0.017(3) C103 0.101(5) 0.048(3) 0.062(4) -0.009(3) 0.009(4) 0.007(3) C104 0.067(4) 0.060(3) 0.062(4) -0.004(3) 0.009(3) -0.015(3) C105 0.038(3) 0.055(3) 0.037(3) 0.004(2) -0.003(2) -0.003(2) C106 0.046(4) 0.087(4) 0.069(4) 0.031(3) -0.002(3) 0.000(3) C107 0.039(4) 0.118(5) 0.102(5) 0.051(4) -0.006(3) -0.020(4) C108 0.071(5) 0.090(5) 0.074(4) 0.019(4) -0.006(3) -0.048(4) C109 0.082(5) 0.048(3) 0.065(4) 0.010(3) -0.002(3) -0.011(3) C110 0.053(3) 0.050(3) 0.060(3) 0.001(3) 0.004(3) -0.004(3) C111 0.053(3) 0.051(3) 0.072(4) -0.003(3) 0.014(3) -0.008(3) C112 0.081(4) 0.058(3) 0.068(4) -0.011(3) 0.032(3) -0.006(3) C113 0.088(5) 0.081(4) 0.086(5) -0.021(4) 0.038(4) -0.013(4) C114 0.109(6) 0.063(4) 0.128(7) -0.029(4) 0.047(5) -0.012(4) C115 0.126(7) 0.048(4) 0.137(7) 0.001(4) 0.047(5) -0.003(4) C116 0.115(6) 0.055(4) 0.089(5) -0.002(3) 0.034(4) 0.002(4) C117 0.063(4) 0.047(3) 0.059(4) -0.007(3) 0.011(3) -0.007(3) C118 0.099(5) 0.062(4) 0.076(4) 0.009(3) 0.037(4) 0.001(3) C119 0.131(7) 0.069(4) 0.076(5) 0.007(3) 0.038(5) -0.004(4) C120 0.121(7) 0.086(5) 0.092(6) -0.028(4) 0.066(5) -0.035(5) C121 0.084(5) 0.123(6) 0.077(5) -0.032(4) 0.028(4) -0.038(5) C122 0.063(4) 0.097(4) 0.054(4) -0.014(3) 0.008(3) -0.020(3) C123 0.054(3) 0.044(3) 0.045(3) 0.007(2) 0.007(3) 0.001(2) C124 0.060(4) 0.075(4) 0.057(4) -0.009(3) 0.009(3) 0.002(3) C125 0.085(5) 0.079(4) 0.051(4) -0.014(3) -0.003(3) -0.008(4) C126 0.067(4) 0.079(4) 0.064(4) 0.004(3) -0.012(3) -0.008(3) C127 0.047(3) 0.068(4) 0.066(4) 0.016(3) -0.003(3) 0.002(3) C128 0.052(3) 0.046(3) 0.056(3) 0.006(2) 0.010(3) 0.006(3) C129 0.047(3) 0.055(3) 0.044(3) -0.014(2) 0.009(2) -0.007(2) C130 0.071(4) 0.053(3) 0.050(3) -0.005(3) 0.002(3) -0.001(3) C131 0.090(5) 0.057(4) 0.081(5) 0.007(3) 0.002(4) 0.012(3) C132 0.086(5) 0.093(5) 0.053(4) 0.012(3) -0.002(4) 0.017(4) C133 0.070(4) 0.102(5) 0.055(4) -0.010(4) -0.004(3) -0.002(4) C134 0.058(4) 0.066(4) 0.060(4) -0.010(3) 0.008(3) -0.005(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 N1 C3 1.284(7) . ? N1 C1 1.352(7) . ? N1 Ni1 2.040(5) . ? N2 C19 1.370(8) . ? N2 C2 1.372(7) . ? N2 C3 1.419(8) . ? N3 C5 1.470(8) . ? N3 C11 1.472(8) . ? N3 C4 1.507(8) . ? N3 Ni1 2.102(4) . ? Ni1 N6 2.036(4) . ? Ni1 N4 2.074(4) . ? Ni1 N5 2.148(4) . ? Ni1 N7 2.167(5) . ? N4 C10 1.331(7) . ? N4 C6 1.353(7) . ? N5 C14 1.441(7) . ? N5 C13 1.458(7) . ? N5 C12 1.474(9) . ? N6 C15 1.118(5) . ? N7 C17 1.134(6) . ? C1 C2 1.324(8) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.460(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.498(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.359(10) . ? C7 C8 1.166(13) . ? C7 H7 0.9300 . ? C8 C9 1.437(16) . ? C8 H8 0.9300 . ? C9 C10 1.361(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.339(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.469(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.435(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Ni2 N8 2.058(4) . ? Ni2 N14 2.065(4) . ? Ni2 N11 2.073(4) . ? Ni2 N10 2.108(4) . ? Ni2 N12 2.148(4) . ? Ni2 N13 2.167(5) . ? N8 C22 1.313(6) . ? N8 C20 1.365(6) . ? N9 C22 1.347(6) . ? N9 C21 1.390(7) . ? N9 C38 1.406(7) . ? N10 C24 1.458(6) . ? N10 C23 1.487(6) . ? N10 C30 1.489(8) . ? N11 C25 1.333(6) . ? N11 C29 1.335(6) . ? N12 C32 1.447(7) . ? N12 C33 1.479(7) . ? N12 C31 1.482(8) . ? N13 C34 1.130(6) . ? N14 C36 1.127(6) . ? C20 C21 1.336(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.488(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.487(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.410(7) . ? C26 C27 1.291(7) . ? C26 H26 0.9300 . ? C27 C28 1.421(8) . ? C27 H27 0.9300 . ? C28 C29 1.346(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.416(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.463(8) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.453(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? B1 C45 1.643(7) . ? B1 C57 1.643(7) . ? B1 C39 1.644(7) . ? B1 C51 1.644(7) . ? B2 C75 1.645(7) . ? B2 C63 1.649(7) . ? B2 C81 1.652(7) . ? B2 C69 1.654(7) . ? B3 C99 1.640(7) . ? B3 C93 1.649(7) . ? B3 C87 1.655(7) . ? B3 C105 1.665(7) . ? B4 C117 1.643(7) . ? B4 C123 1.650(8) . ? B4 C129 1.651(8) . ? B4 C111 1.658(7) . ? C39 C40 1.389(6) . ? C39 C44 1.394(7) . ? C40 C41 1.386(7) . ? C40 H40 0.9300 . ? C41 C42 1.350(8) . ? C41 H41 0.9300 . ? C42 C43 1.361(9) . ? C42 H42 0.9300 . ? C43 C44 1.382(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.396(6) . ? C45 C50 1.399(7) . ? C46 C47 1.371(7) . ? C46 H46 0.9300 . ? C47 C48 1.362(8) . ? C47 H47 0.9300 . ? C48 C49 1.366(8) . ? C48 H48 0.9300 . ? C49 C50 1.383(7) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C56 1.387(6) . ? C51 C52 1.391(6) . ? C52 C53 1.383(7) . ? C52 H52 0.9300 . ? C53 C54 1.382(8) . ? C53 H53 0.9300 . ? C54 C55 1.375(9) . ? C54 H54 0.9300 . ? C55 C56 1.384(8) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.394(6) . ? C57 C62 1.403(6) . ? C58 C59 1.390(8) . ? C58 H58 0.9300 . ? C59 C60 1.350(8) . ? C59 H59 0.9300 . ? C60 C61 1.378(8) . ? C60 H60 0.9300 . ? C61 C62 1.371(7) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.387(6) . ? C63 C68 1.395(6) . ? C64 C65 1.390(7) . ? C64 H64 0.9300 . ? C65 C66 1.373(7) . ? C65 H65 0.9300 . ? C66 C67 1.381(7) . ? C66 H66 0.9300 . ? C67 C68 1.389(6) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C74 1.380(6) . ? C69 C70 1.401(6) . ? C70 C71 1.378(7) . ? C70 H70 0.9300 . ? C71 C72 1.369(8) . ? C71 H71 0.9300 . ? C72 C73 1.370(8) . ? C72 H72 0.9300 . ? C73 C74 1.379(7) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C76 1.393(6) . ? C75 C80 1.395(6) . ? C76 C77 1.382(7) . ? C76 H76 0.9300 . ? C77 C78 1.374(7) . ? C77 H77 0.9300 . ? C78 C79 1.369(7) . ? C78 H78 0.9300 . ? C79 C80 1.378(6) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? C81 C86 1.391(7) . ? C81 C82 1.401(6) . ? C82 C83 1.378(7) . ? C82 H82 0.9300 . ? C83 C84 1.371(8) . ? C83 H83 0.9300 . ? C84 C85 1.362(8) . ? C84 H84 0.9300 . ? C85 C86 1.383(8) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 C88 1.383(6) . ? C87 C92 1.397(6) . ? C88 C89 1.384(7) . ? C88 H88 0.9300 . ? C89 C90 1.367(7) . ? C89 H89 0.9300 . ? C90 C91 1.361(7) . ? C90 H90 0.9300 . ? C91 C92 1.376(7) . ? C91 H91 0.9300 . ? C92 H92 0.9300 . ? C93 C94 1.383(6) . ? C93 C98 1.399(6) . ? C94 C95 1.388(7) . ? C94 H94 0.9300 . ? C95 C96 1.372(8) . ? C95 H95 0.9300 . ? C96 C97 1.366(8) . ? C96 H96 0.9300 . ? C97 C98 1.402(7) . ? C97 H97 0.9300 . ? C98 H98 0.9300 . ? C99 C100 1.377(6) . ? C99 C104 1.399(6) . ? C100 C101 1.364(7) . ? C100 H100 0.9300 . ? C101 C102 1.343(7) . ? C101 H101 0.9300 . ? C102 C103 1.364(8) . ? C102 H102 0.9300 . ? C103 C104 1.395(7) . ? C103 H103 0.9300 . ? C104 H104 0.9300 . ? C105 C106 1.367(7) . ? C105 C110 1.411(6) . ? C106 C107 1.396(7) . ? C106 H106 0.9300 . ? C107 C108 1.337(8) . ? C107 H107 0.9300 . ? C108 C109 1.386(8) . ? C108 H108 0.9300 . ? C109 C110 1.379(7) . ? C109 H109 0.9300 . ? C110 H110 0.9300 . ? C111 C112 1.392(7) . ? C111 C116 1.397(7) . ? C112 C113 1.383(7) . ? C112 H112 0.9300 . ? C113 C114 1.371(9) . ? C113 H113 0.9300 . ? C114 C115 1.365(9) . ? C114 H114 0.9300 . ? C115 C116 1.380(8) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C117 C122 1.391(7) . ? C117 C118 1.401(7) . ? C118 C119 1.379(8) . ? C118 H118 0.9300 . ? C119 C120 1.359(10) . ? C119 H119 0.9300 . ? C120 C121 1.361(9) . ? C120 H120 0.9300 . ? C121 C122 1.398(8) . ? C121 H121 0.9300 . ? C122 H122 0.9300 . ? C123 C128 1.390(6) . ? C123 C124 1.403(6) . ? C124 C125 1.396(7) . ? C124 H124 0.9300 . ? C125 C126 1.369(8) . ? C125 H125 0.9300 . ? C126 C127 1.355(7) . ? C126 H126 0.9300 . ? C127 C128 1.391(7) . ? C127 H127 0.9300 . ? C128 H128 0.9300 . ? C129 C130 1.388(6) . ? C129 C134 1.396(7) . ? C130 C131 1.383(7) . ? C130 H130 0.9300 . ? C131 C132 1.384(8) . ? C131 H131 0.9300 . ? C132 C133 1.349(8) . ? C132 H132 0.9300 . ? C133 C134 1.386(8) . ? C133 H133 0.9300 . ? C134 H134 0.9300 . ? 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 C3 N1 C1 107.4(5) . . ? C3 N1 Ni1 112.7(4) . . ? C1 N1 Ni1 139.9(4) . . ? C19 N2 C2 128.0(7) . . ? C19 N2 C3 126.0(7) . . ? C2 N2 C3 106.0(5) . . ? C5 N3 C11 109.1(6) . . ? C5 N3 C4 114.2(5) . . ? C11 N3 C4 113.3(6) . . ? C5 N3 Ni1 107.2(4) . . ? C11 N3 Ni1 105.2(4) . . ? C4 N3 Ni1 107.2(4) . . ? N6 Ni1 N1 98.68(19) . . ? N6 Ni1 N4 98.99(18) . . ? N1 Ni1 N4 159.8(2) . . ? N6 Ni1 N3 176.88(18) . . ? N1 Ni1 N3 82.4(2) . . ? N4 Ni1 N3 80.5(2) . . ? N6 Ni1 N5 92.11(17) . . ? N1 Ni1 N5 92.90(18) . . ? N4 Ni1 N5 96.22(18) . . ? N3 Ni1 N5 84.89(18) . . ? N6 Ni1 N7 91.54(16) . . ? N1 Ni1 N7 86.58(17) . . ? N4 Ni1 N7 83.17(17) . . ? N3 Ni1 N7 91.46(18) . . ? N5 Ni1 N7 176.35(16) . . ? C10 N4 C6 116.9(6) . . ? C10 N4 Ni1 129.7(4) . . ? C6 N4 Ni1 112.6(4) . . ? C14 N5 C13 106.4(5) . . ? C14 N5 C12 111.4(6) . . ? C13 N5 C12 107.4(6) . . ? C14 N5 Ni1 113.3(4) . . ? C13 N5 Ni1 115.1(4) . . ? C12 N5 Ni1 103.1(4) . . ? C15 N6 Ni1 176.4(5) . . ? C17 N7 Ni1 174.8(5) . . ? C2 C1 N1 111.9(6) . . ? C2 C1 H1 124.1 . . ? N1 C1 H1 124.1 . . ? C1 C2 N2 105.8(6) . . ? C1 C2 H2 127.1 . . ? N2 C2 H2 127.1 . . ? N1 C3 N2 109.0(6) . . ? N1 C3 C4 122.3(6) . . ? N2 C3 C4 128.7(6) . . ? C3 C4 N3 110.7(5) . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 111.3(5) . . ? N3 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N4 C6 C7 119.3(8) . . ? N4 C6 C5 117.3(5) . . ? C7 C6 C5 123.3(8) . . ? C8 C7 C6 127.9(15) . . ? C8 C7 H7 116.0 . . ? C6 C7 H7 116.0 . . ? C7 C8 C9 115.7(14) . . ? C7 C8 H8 122.2 . . ? C9 C8 H8 122.2 . . ? C10 C9 C8 119.6(9) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N4 C10 C9 120.5(7) . . ? N4 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 N3 117.0(6) . . ? C12 C11 H11A 108.1 . . ? N3 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? N3 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 N5 119.0(7) . . ? C11 C12 H12A 107.6 . . ? N5 C12 H12A 107.6 . . ? C11 C12 H12B 107.6 . . ? N5 C12 H12B 107.6 . . ? H12A C12 H12B 107.0 . . ? N5 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N6 C15 C16 179.6(6) . . ? 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 . . ? N7 C17 C18 178.8(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N8 Ni2 N14 101.52(17) . . ? N8 Ni2 N11 158.71(17) . . ? N14 Ni2 N11 97.56(18) . . ? N8 Ni2 N10 80.21(16) . . ? N14 Ni2 N10 177.71(17) . . ? N11 Ni2 N10 80.99(16) . . ? N8 Ni2 N12 95.45(18) . . ? N14 Ni2 N12 92.19(17) . . ? N11 Ni2 N12 93.15(17) . . ? N10 Ni2 N12 86.14(18) . . ? N8 Ni2 N13 84.70(17) . . ? N14 Ni2 N13 91.10(16) . . ? N11 Ni2 N13 85.59(16) . . ? N10 Ni2 N13 90.55(17) . . ? N12 Ni2 N13 176.61(17) . . ? C22 N8 C20 106.7(4) . . ? C22 N8 Ni2 111.0(3) . . ? C20 N8 Ni2 141.3(4) . . ? C22 N9 C21 108.1(5) . . ? C22 N9 C38 125.4(6) . . ? C21 N9 C38 126.3(6) . . ? C24 N10 C23 112.5(5) . . ? C24 N10 C30 113.6(5) . . ? C23 N10 C30 109.0(4) . . ? C24 N10 Ni2 109.0(3) . . ? C23 N10 Ni2 108.1(3) . . ? C30 N10 Ni2 104.2(4) . . ? C25 N11 C29 117.0(5) . . ? C25 N11 Ni2 114.2(3) . . ? C29 N11 Ni2 128.8(4) . . ? C32 N12 C33 106.5(6) . . ? C32 N12 C31 112.8(6) . . ? C33 N12 C31 108.2(6) . . ? C32 N12 Ni2 113.2(4) . . ? C33 N12 Ni2 113.9(4) . . ? C31 N12 Ni2 102.3(4) . . ? C34 N13 Ni2 176.0(4) . . ? C36 N14 Ni2 175.5(5) . . ? C21 C20 N8 110.8(5) . . ? C21 C20 H20 124.6 . . ? N8 C20 H20 124.6 . . ? C20 C21 N9 104.7(5) . . ? C20 C21 H21 127.6 . . ? N9 C21 H21 127.6 . . ? N8 C22 N9 109.7(5) . . ? N8 C22 C23 122.6(4) . . ? N9 C22 C23 127.7(5) . . ? N10 C23 C22 107.1(4) . . ? N10 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? N10 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? N10 C24 C25 113.4(5) . . ? N10 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N10 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N11 C25 C26 122.6(5) . . ? N11 C25 C24 117.6(5) . . ? C26 C25 C24 119.8(5) . . ? C27 C26 C25 120.0(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 117.9(6) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C29 C28 C27 120.0(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? N11 C29 C28 122.4(5) . . ? N11 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C31 C30 N10 114.5(5) . . ? C31 C30 H30A 108.6 . . ? N10 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? N10 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 N12 115.4(6) . . ? C30 C31 H31A 108.4 . . ? N12 C31 H31A 108.4 . . ? C30 C31 H31B 108.4 . . ? N12 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? N12 C32 H32A 109.5 . . ? N12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N12 C33 H33A 109.5 . . ? N12 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N12 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N13 C34 C35 179.7(6) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N14 C36 C37 178.3(7) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N9 C38 H38A 109.5 . . ? N9 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N9 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C45 B1 C57 114.0(4) . . ? C45 B1 C39 104.3(4) . . ? C57 B1 C39 111.1(4) . . ? C45 B1 C51 110.5(4) . . ? C57 B1 C51 104.8(4) . . ? C39 B1 C51 112.3(4) . . ? C75 B2 C63 106.2(3) . . ? C75 B2 C81 108.8(4) . . ? C63 B2 C81 112.7(4) . . ? C75 B2 C69 113.0(4) . . ? C63 B2 C69 108.6(4) . . ? C81 B2 C69 107.6(3) . . ? C99 B3 C93 110.9(4) . . ? C99 B3 C87 107.8(4) . . ? C93 B3 C87 111.4(4) . . ? C99 B3 C105 108.3(4) . . ? C93 B3 C105 107.7(4) . . ? C87 B3 C105 110.6(4) . . ? C117 B4 C123 108.1(4) . . ? C117 B4 C129 110.0(4) . . ? C123 B4 C129 109.0(4) . . ? C117 B4 C111 111.3(4) . . ? C123 B4 C111 109.4(4) . . ? C129 B4 C111 109.0(4) . . ? C40 C39 C44 114.2(5) . . ? C40 C39 B1 122.6(4) . . ? C44 C39 B1 123.0(4) . . ? C41 C40 C39 122.9(5) . . ? C41 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C42 C41 C40 120.4(6) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 119.4(6) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C44 120.0(6) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 123.1(6) . . ? C43 C44 H44 118.5 . . ? C39 C44 H44 118.5 . . ? C46 C45 C50 114.2(4) . . ? C46 C45 B1 124.1(4) . . ? C50 C45 B1 121.5(4) . . ? C47 C46 C45 123.7(5) . . ? C47 C46 H46 118.1 . . ? C45 C46 H46 118.1 . . ? C48 C47 C46 120.0(5) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 119.1(5) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C48 C49 C50 120.6(6) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C45 122.3(5) . . ? C49 C50 H50 118.8 . . ? C45 C50 H50 118.8 . . ? C56 C51 C52 114.0(5) . . ? C56 C51 B1 124.1(4) . . ? C52 C51 B1 121.8(4) . . ? C53 C52 C51 124.5(5) . . ? C53 C52 H52 117.8 . . ? C51 C52 H52 117.8 . . ? C54 C53 C52 119.3(6) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C55 C54 C53 118.1(6) . . ? C55 C54 H54 120.9 . . ? C53 C54 H54 120.9 . . ? C54 C55 C56 121.1(6) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C55 C56 C51 123.0(6) . . ? C55 C56 H56 118.5 . . ? C51 C56 H56 118.5 . . ? C58 C57 C62 114.0(5) . . ? C58 C57 B1 124.0(4) . . ? C62 C57 B1 121.7(4) . . ? C59 C58 C57 122.7(5) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C60 C59 C58 120.6(5) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C59 C60 C61 119.3(6) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 C60 119.8(6) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C57 123.6(5) . . ? C61 C62 H62 118.2 . . ? C57 C62 H62 118.2 . . ? C64 C63 C68 114.2(4) . . ? C64 C63 B2 125.8(4) . . ? C68 C63 B2 119.6(4) . . ? C63 C64 C65 123.6(5) . . ? C63 C64 H64 118.2 . . ? C65 C64 H64 118.2 . . ? C66 C65 C64 119.8(5) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C67 119.4(5) . . ? C65 C66 H66 120.3 . . ? C67 C66 H66 120.3 . . ? C66 C67 C68 119.1(5) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? C67 C68 C63 124.0(4) . . ? C67 C68 H68 118.0 . . ? C63 C68 H68 118.0 . . ? C74 C69 C70 114.0(4) . . ? C74 C69 B2 123.9(4) . . ? C70 C69 B2 122.2(4) . . ? C71 C70 C69 123.1(5) . . ? C71 C70 H70 118.5 . . ? C69 C70 H70 118.5 . . ? C72 C71 C70 120.6(6) . . ? C72 C71 H71 119.7 . . ? C70 C71 H71 119.7 . . ? C71 C72 C73 118.1(5) . . ? C71 C72 H72 121.0 . . ? C73 C72 H72 121.0 . . ? C72 C73 C74 120.5(6) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C73 C74 C69 123.7(5) . . ? C73 C74 H74 118.2 . . ? C69 C74 H74 118.2 . . ? C76 C75 C80 114.2(4) . . ? C76 C75 B2 124.0(4) . . ? C80 C75 B2 121.5(4) . . ? C77 C76 C75 123.1(5) . . ? C77 C76 H76 118.5 . . ? C75 C76 H76 118.5 . . ? C78 C77 C76 120.5(5) . . ? C78 C77 H77 119.7 . . ? C76 C77 H77 119.7 . . ? C79 C78 C77 118.2(5) . . ? C79 C78 H78 120.9 . . ? C77 C78 H78 120.9 . . ? C78 C79 C80 120.7(5) . . ? C78 C79 H79 119.7 . . ? C80 C79 H79 119.7 . . ? C79 C80 C75 123.2(5) . . ? C79 C80 H80 118.4 . . ? C75 C80 H80 118.4 . . ? C86 C81 C82 113.7(5) . . ? C86 C81 B2 122.9(5) . . ? C82 C81 B2 123.3(4) . . ? C83 C82 C81 123.3(5) . . ? C83 C82 H82 118.3 . . ? C81 C82 H82 118.3 . . ? C84 C83 C82 119.8(6) . . ? C84 C83 H83 120.1 . . ? C82 C83 H83 120.1 . . ? C85 C84 C83 119.9(6) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C84 C85 C86 119.2(6) . . ? C84 C85 H85 120.4 . . ? C86 C85 H85 120.4 . . ? C85 C86 C81 124.2(6) . . ? C85 C86 H86 117.9 . . ? C81 C86 H86 117.9 . . ? C88 C87 C92 113.4(4) . . ? C88 C87 B3 122.1(4) . . ? C92 C87 B3 124.5(4) . . ? C87 C88 C89 124.2(5) . . ? C87 C88 H88 117.9 . . ? C89 C88 H88 117.9 . . ? C90 C89 C88 119.3(5) . . ? C90 C89 H89 120.3 . . ? C88 C89 H89 120.3 . . ? C91 C90 C89 119.3(5) . . ? C91 C90 H90 120.3 . . ? C89 C90 H90 120.3 . . ? C90 C91 C92 120.1(5) . . ? C90 C91 H91 120.0 . . ? C92 C91 H91 120.0 . . ? C91 C92 C87 123.7(5) . . ? C91 C92 H92 118.2 . . ? C87 C92 H92 118.2 . . ? C94 C93 C98 114.8(4) . . ? C94 C93 B3 123.0(4) . . ? C98 C93 B3 122.0(4) . . ? C93 C94 C95 123.2(5) . . ? C93 C94 H94 118.4 . . ? C95 C94 H94 118.4 . . ? C96 C95 C94 120.4(6) . . ? C96 C95 H95 119.8 . . ? C94 C95 H95 119.8 . . ? C97 C96 C95 118.8(6) . . ? C97 C96 H96 120.6 . . ? C95 C96 H96 120.6 . . ? C96 C97 C98 120.3(6) . . ? C96 C97 H97 119.9 . . ? C98 C97 H97 119.9 . . ? C93 C98 C97 122.5(5) . . ? C93 C98 H98 118.8 . . ? C97 C98 H98 118.8 . . ? C100 C99 C104 112.5(4) . . ? C100 C99 B3 123.9(4) . . ? C104 C99 B3 123.6(4) . . ? C101 C100 C99 124.3(5) . . ? C101 C100 H100 117.9 . . ? C99 C100 H100 117.9 . . ? C102 C101 C100 121.5(6) . . ? C102 C101 H101 119.2 . . ? C100 C101 H101 119.2 . . ? C101 C102 C103 118.4(5) . . ? C101 C102 H102 120.8 . . ? C103 C102 H102 120.8 . . ? C102 C103 C104 119.3(5) . . ? C102 C103 H103 120.3 . . ? C104 C103 H103 120.3 . . ? C103 C104 C99 123.9(5) . . ? C103 C104 H104 118.1 . . ? C99 C104 H104 118.1 . . ? C106 C105 C110 114.0(4) . . ? C106 C105 B3 123.8(4) . . ? C110 C105 B3 122.1(4) . . ? C105 C106 C107 123.5(5) . . ? C105 C106 H106 118.3 . . ? C107 C106 H106 118.3 . . ? C108 C107 C106 121.0(6) . . ? C108 C107 H107 119.5 . . ? C106 C107 H107 119.5 . . ? C107 C108 C109 118.6(5) . . ? C107 C108 H108 120.7 . . ? C109 C108 H108 120.7 . . ? C110 C109 C108 119.8(5) . . ? C110 C109 H109 120.1 . . ? C108 C109 H109 120.1 . . ? C109 C110 C105 123.0(5) . . ? C109 C110 H110 118.5 . . ? C105 C110 H110 118.5 . . ? C112 C111 C116 113.8(5) . . ? C112 C111 B4 122.3(5) . . ? C116 C111 B4 123.8(5) . . ? C113 C112 C111 123.4(6) . . ? C113 C112 H112 118.3 . . ? C111 C112 H112 118.3 . . ? C114 C113 C112 120.5(6) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 118.2(6) . . ? C115 C114 H114 120.9 . . ? C113 C114 H114 120.9 . . ? C114 C115 C116 120.8(6) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C115 C116 C111 123.2(6) . . ? C115 C116 H116 118.4 . . ? C111 C116 H116 118.4 . . ? C122 C117 C118 113.8(5) . . ? C122 C117 B4 124.8(5) . . ? C118 C117 B4 121.4(5) . . ? C119 C118 C117 123.5(7) . . ? C119 C118 H118 118.2 . . ? C117 C118 H118 118.2 . . ? C120 C119 C118 120.2(7) . . ? C120 C119 H119 119.9 . . ? C118 C119 H119 119.9 . . ? C119 C120 C121 119.4(7) . . ? C119 C120 H120 120.3 . . ? C121 C120 H120 120.3 . . ? C120 C121 C122 120.0(7) . . ? C120 C121 H121 120.0 . . ? C122 C121 H121 120.0 . . ? C117 C122 C121 123.0(6) . . ? C117 C122 H122 118.5 . . ? C121 C122 H122 118.5 . . ? C128 C123 C124 114.1(5) . . ? C128 C123 B4 125.5(4) . . ? C124 C123 B4 120.4(5) . . ? C125 C124 C123 123.3(5) . . ? C125 C124 H124 118.4 . . ? C123 C124 H124 118.4 . . ? C126 C125 C124 119.5(5) . . ? C126 C125 H125 120.3 . . ? C124 C125 H125 120.3 . . ? C127 C126 C125 119.5(6) . . ? C127 C126 H126 120.2 . . ? C125 C126 H126 120.2 . . ? C126 C127 C128 120.6(5) . . ? C126 C127 H127 119.7 . . ? C128 C127 H127 119.7 . . ? C123 C128 C127 123.1(5) . . ? C123 C128 H128 118.5 . . ? C127 C128 H128 118.5 . . ? C130 C129 C134 114.3(5) . . ? C130 C129 B4 124.8(5) . . ? C134 C129 B4 121.0(4) . . ? C131 C130 C129 123.1(5) . . ? C131 C130 H130 118.4 . . ? C129 C130 H130 118.4 . . ? C130 C131 C132 120.2(6) . . ? C130 C131 H131 119.9 . . ? C132 C131 H131 119.9 . . ? C133 C132 C131 118.6(6) . . ? C133 C132 H132 120.7 . . ? C131 C132 H132 120.7 . . ? C132 C133 C134 120.8(6) . . ? C132 C133 H133 119.6 . . ? C134 C133 H133 119.6 . . ? C133 C134 C129 123.0(5) . . ? C133 C134 H134 118.5 . . ? C129 C134 H134 118.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.605 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.057 # Attachment '- 4.cif' data_mpmb9 _database_code_depnum_ccdc_archive 'CCDC 805450' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H73 B2 N9 Ni' _chemical_formula_weight 1096.68 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9038(2) _cell_length_b 14.9757(2) _cell_length_c 37.0413(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.7660(10) _cell_angle_gamma 90.00 _cell_volume 6048.01(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6908 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 23.32 _exptl_crystal_description Prism _exptl_crystal_colour Violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.9298 _exptl_absorpt_correction_T_max 0.9535 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 SMART APEX CCD' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64793 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14607 _reflns_number_gt 8622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.2094P] 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 14607 _refine_ls_number_parameters 728 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.25150(3) 0.296536(19) 0.598121(7) 0.03777(9) Uani 1 d . . . N1 N 0.28485(17) 0.16673(13) 0.61558(5) 0.0447(5) Uani 1 d . . . N2 N 0.2416(2) 0.06649(14) 0.65681(6) 0.0563(5) Uani 1 d . . . N3 N 0.24282(15) 0.31205(11) 0.65527(4) 0.0352(4) Uani 1 d . . . N4 N 0.18194(16) 0.42277(12) 0.59936(5) 0.0406(4) Uani 1 d . . . N5 N 0.11411(17) 0.53378(12) 0.63252(5) 0.0437(5) Uani 1 d . . . N6 N 0.43591(17) 0.34523(14) 0.60426(5) 0.0483(5) Uani 1 d . . . N7 N 0.06656(19) 0.24728(14) 0.59066(6) 0.0532(5) Uani 1 d . . . N8 N 0.27257(19) 0.28319(14) 0.54283(5) 0.0534(5) Uani 1 d . . . N9 N 0.6315(4) 0.0493(2) 0.80172(11) 0.1283(14) Uani 1 d . . . B1 B 0.2531(2) 0.78486(18) 0.54900(7) 0.0434(6) Uani 1 d . . . B2 B 0.7992(2) 0.30428(17) 0.71809(6) 0.0366(6) Uani 1 d . . . C1 C 0.3127(2) 0.08330(18) 0.60277(7) 0.0593(7) Uani 1 d . . . H1 H 0.3450 0.0715 0.5802 0.071 Uiso 1 calc R . . C2 C 0.2867(3) 0.02158(19) 0.62753(8) 0.0693(8) Uani 1 d . . . H2 H 0.2970 -0.0398 0.6254 0.083 Uiso 1 calc R . . C3 C 0.1989(3) 0.02636(19) 0.69043(8) 0.0784(9) Uani 1 d . . . H3A H 0.1728 0.0726 0.7066 0.118 Uiso 1 calc R . . H3B H 0.2645 -0.0069 0.7015 0.118 Uiso 1 calc R . . H3C H 0.1313 -0.0129 0.6852 0.118 Uiso 1 calc R . . C4 C 0.2420(2) 0.15330(15) 0.64831(6) 0.0428(5) Uani 1 d . . . C5 C 0.1944(2) 0.22836(15) 0.67063(6) 0.0470(6) Uani 1 d . . . H5A H 0.1054 0.2289 0.6700 0.056 Uiso 1 calc R . . H5B H 0.2216 0.2218 0.6955 0.056 Uiso 1 calc R . . C6 C 0.1659(2) 0.38999(15) 0.66440(6) 0.0430(5) Uani 1 d . . . H6A H 0.2025 0.4222 0.6845 0.052 Uiso 1 calc R . . H6B H 0.0849 0.3701 0.6714 0.052 Uiso 1 calc R . . C7 C 0.15595(19) 0.44936(15) 0.63253(6) 0.0386(5) Uani 1 d . . . C8 C 0.0811(3) 0.58588(18) 0.66410(7) 0.0632(7) Uani 1 d . . . H8A H 0.0334 0.5497 0.6800 0.095 Uiso 1 calc R . . H8B H 0.0338 0.6369 0.6567 0.095 Uiso 1 calc R . . H8C H 0.1543 0.6055 0.6764 0.095 Uiso 1 calc R . . C9 C 0.1127(2) 0.56220(17) 0.59722(7) 0.0504(6) Uani 1 d . . . H9 H 0.0876 0.6179 0.5888 0.061 Uiso 1 calc R . . C10 C 0.1540(2) 0.49461(16) 0.57739(6) 0.0487(6) Uani 1 d . . . H10 H 0.1627 0.4957 0.5525 0.058 Uiso 1 calc R . . C11 C 0.3722(2) 0.32477(18) 0.66694(6) 0.0505(6) Uani 1 d . . . H11A H 0.4122 0.2671 0.6686 0.061 Uiso 1 calc R . . H11B H 0.3743 0.3516 0.6908 0.061 Uiso 1 calc R . . C12 C 0.4408(2) 0.38295(19) 0.64135(6) 0.0579(7) Uani 1 d . . . H12A H 0.4052 0.4423 0.6412 0.069 Uiso 1 calc R . . H12B H 0.5255 0.3880 0.6494 0.069 Uiso 1 calc R . . C13 C 0.5277(2) 0.2733(2) 0.60017(8) 0.0730(9) Uani 1 d . . . H13A H 0.5213 0.2487 0.5763 0.110 Uiso 1 calc R . . H13B H 0.5128 0.2273 0.6176 0.110 Uiso 1 calc R . . H13C H 0.6085 0.2973 0.6040 0.110 Uiso 1 calc R . . C14 C 0.4670(3) 0.4180(2) 0.57889(7) 0.0708(8) Uani 1 d . . . H14A H 0.4076 0.4650 0.5807 0.106 Uiso 1 calc R . . H14B H 0.4666 0.3951 0.5547 0.106 Uiso 1 calc R . . H14C H 0.5470 0.4409 0.5848 0.106 Uiso 1 calc R . . C15 C -0.0194(3) 0.2137(2) 0.58137(7) 0.0654(8) Uani 1 d . . . C16 C -0.1333(4) 0.1717(3) 0.56930(11) 0.145(2) Uani 1 d . . . H16A H -0.1826 0.1579 0.5898 0.217 Uiso 1 calc R . . H16B H -0.1150 0.1177 0.5565 0.217 Uiso 1 calc R . . H16C H -0.1774 0.2118 0.5536 0.217 Uiso 1 calc R . . C17 C 0.2838(3) 0.28186(17) 0.51292(7) 0.0577(7) Uani 1 d . . . C18 C 0.2979(4) 0.2818(2) 0.47397(7) 0.0953(12) Uani 1 d . . . H18A H 0.2220 0.2644 0.4626 0.143 Uiso 1 calc R . . H18B H 0.3611 0.2403 0.4675 0.143 Uiso 1 calc R . . H18C H 0.3201 0.3405 0.4660 0.143 Uiso 1 calc R . . C19 C 0.1370(2) 0.80884(15) 0.57543(6) 0.0431(5) Uani 1 d . . . C20 C 0.1409(2) 0.79763(16) 0.61276(6) 0.0469(6) Uani 1 d . . . H20 H 0.2124 0.7749 0.6232 0.056 Uiso 1 calc R . . C21 C 0.0442(2) 0.81846(17) 0.63516(7) 0.0565(7) Uani 1 d . . . H21 H 0.0523 0.8096 0.6599 0.068 Uiso 1 calc R . . C22 C -0.0627(3) 0.85178(19) 0.62121(8) 0.0680(8) Uani 1 d . . . H22 H -0.1279 0.8653 0.6362 0.082 Uiso 1 calc R . . C23 C -0.0721(3) 0.8650(2) 0.58451(9) 0.0737(8) Uani 1 d . . . H23 H -0.1440 0.8881 0.5745 0.088 Uiso 1 calc R . . C24 C 0.0254(2) 0.84395(19) 0.56253(7) 0.0616(7) Uani 1 d . . . H24 H 0.0165 0.8536 0.5378 0.074 Uiso 1 calc R . . C25 C 0.2797(2) 0.86791(16) 0.52099(6) 0.0463(6) Uani 1 d . . . C26 C 0.2301(3) 0.95293(19) 0.52433(7) 0.0658(8) Uani 1 d . . . H26 H 0.1762 0.9640 0.5431 0.079 Uiso 1 calc R . . C27 C 0.2578(3) 1.0220(2) 0.50084(9) 0.0829(10) Uani 1 d . . . H27 H 0.2221 1.0778 0.5040 0.099 Uiso 1 calc R . . C28 C 0.3367(3) 1.0089(2) 0.47317(9) 0.0779(9) Uani 1 d . . . H28 H 0.3544 1.0551 0.4573 0.094 Uiso 1 calc R . . C29 C 0.3897(3) 0.9269(2) 0.46903(8) 0.0729(9) Uani 1 d . . . H29 H 0.4447 0.9171 0.4505 0.087 Uiso 1 calc R . . C30 C 0.3609(2) 0.85869(19) 0.49260(7) 0.0590(7) Uani 1 d . . . H30 H 0.3980 0.8034 0.4893 0.071 Uiso 1 calc R . . C31 C 0.2234(2) 0.69534(16) 0.52394(6) 0.0482(6) Uani 1 d . . . C32 C 0.1056(3) 0.67501(18) 0.51130(7) 0.0627(7) Uani 1 d . . . H32 H 0.0409 0.7109 0.5186 0.075 Uiso 1 calc R . . C33 C 0.0805(4) 0.6043(2) 0.48858(8) 0.0847(11) Uani 1 d . . . H33 H 0.0003 0.5939 0.4808 0.102 Uiso 1 calc R . . C34 C 0.1727(4) 0.5495(2) 0.47739(7) 0.0861(12) Uani 1 d . . . H34 H 0.1559 0.5015 0.4621 0.103 Uiso 1 calc R . . C35 C 0.2907(3) 0.5664(2) 0.48909(8) 0.0788(9) Uani 1 d . . . H35 H 0.3545 0.5295 0.4819 0.095 Uiso 1 calc R . . C36 C 0.3145(3) 0.63790(18) 0.51145(7) 0.0624(7) Uani 1 d . . . H36 H 0.3953 0.6485 0.5186 0.075 Uiso 1 calc R . . C37 C 0.3773(2) 0.76913(15) 0.57377(6) 0.0393(5) Uani 1 d . . . C38 C 0.4616(2) 0.83717(16) 0.58095(6) 0.0426(5) Uani 1 d . . . H38 H 0.4469 0.8935 0.5712 0.051 Uiso 1 calc R . . C39 C 0.5662(2) 0.82449(17) 0.60199(6) 0.0476(6) Uani 1 d . . . H39 H 0.6194 0.8721 0.6061 0.057 Uiso 1 calc R . . C40 C 0.5923(2) 0.74310(19) 0.61684(6) 0.0522(6) Uani 1 d . . . H40 H 0.6636 0.7344 0.6305 0.063 Uiso 1 calc R . . C41 C 0.5106(2) 0.67409(18) 0.61116(7) 0.0572(7) Uani 1 d . . . H41 H 0.5257 0.6184 0.6214 0.069 Uiso 1 calc R . . C42 C 0.4066(2) 0.68753(17) 0.59036(7) 0.0521(6) Uani 1 d . . . H42 H 0.3528 0.6399 0.5871 0.063 Uiso 1 calc R . . C43 C 0.79943(18) 0.37969(15) 0.68547(5) 0.0362(5) Uani 1 d . . . C44 C 0.7726(2) 0.46978(16) 0.69080(6) 0.0481(6) Uani 1 d . . . H44 H 0.7560 0.4892 0.7141 0.058 Uiso 1 calc R . . C45 C 0.7695(2) 0.53165(18) 0.66307(7) 0.0595(7) Uani 1 d . . . H45 H 0.7485 0.5906 0.6679 0.071 Uiso 1 calc R . . C46 C 0.7972(2) 0.5064(2) 0.62845(7) 0.0615(7) Uani 1 d . . . H46 H 0.7951 0.5477 0.6097 0.074 Uiso 1 calc R . . C47 C 0.8279(2) 0.4196(2) 0.62219(6) 0.0590(7) Uani 1 d . . . H47 H 0.8492 0.4017 0.5991 0.071 Uiso 1 calc R . . C48 C 0.8275(2) 0.35806(17) 0.65004(6) 0.0469(6) Uani 1 d . . . H48 H 0.8471 0.2991 0.6448 0.056 Uiso 1 calc R . . C49 C 0.69560(19) 0.32803(14) 0.74881(5) 0.0344(5) Uani 1 d . . . C50 C 0.7073(2) 0.29770(15) 0.78444(6) 0.0424(5) Uani 1 d . . . H50 H 0.7765 0.2648 0.7909 0.051 Uiso 1 calc R . . C51 C 0.6202(2) 0.31460(17) 0.81037(6) 0.0512(6) Uani 1 d . . . H51 H 0.6314 0.2925 0.8336 0.061 Uiso 1 calc R . . C52 C 0.5176(2) 0.36362(18) 0.80212(6) 0.0533(6) Uani 1 d . . . H52 H 0.4601 0.3763 0.8197 0.064 Uiso 1 calc R . . C53 C 0.5009(2) 0.39371(16) 0.76744(6) 0.0496(6) Uani 1 d . . . H53 H 0.4310 0.4261 0.7612 0.060 Uiso 1 calc R . . C54 C 0.5886(2) 0.37577(15) 0.74167(6) 0.0422(5) Uani 1 d . . . H54 H 0.5751 0.3968 0.7183 0.051 Uiso 1 calc R . . C55 C 0.7642(2) 0.20782(15) 0.69919(6) 0.0423(5) Uani 1 d . . . C56 C 0.8500(3) 0.15138(18) 0.68362(8) 0.0650(8) Uani 1 d . . . H56 H 0.9327 0.1658 0.6861 0.078 Uiso 1 calc R . . C57 C 0.8188(3) 0.0748(2) 0.66464(9) 0.0851(10) Uani 1 d . . . H57 H 0.8798 0.0397 0.6546 0.102 Uiso 1 calc R . . C58 C 0.6995(4) 0.0510(2) 0.66072(9) 0.0852(10) Uani 1 d . . . H58 H 0.6780 -0.0002 0.6479 0.102 Uiso 1 calc R . . C59 C 0.6113(3) 0.1034(2) 0.67586(9) 0.0802(9) Uani 1 d . . . H59 H 0.5291 0.0876 0.6736 0.096 Uiso 1 calc R . . C60 C 0.6442(2) 0.18012(17) 0.69454(7) 0.0559(7) Uani 1 d . . . H60 H 0.5824 0.2147 0.7045 0.067 Uiso 1 calc R . . C61 C 0.93412(19) 0.30222(17) 0.73861(6) 0.0429(5) Uani 1 d . . . C62 C 1.0020(2) 0.37966(19) 0.74451(6) 0.0548(7) Uani 1 d . . . H62 H 0.9714 0.4334 0.7356 0.066 Uiso 1 calc R . . C63 C 1.1140(3) 0.3805(3) 0.76325(7) 0.0765(9) Uani 1 d . . . H63 H 1.1560 0.4339 0.7667 0.092 Uiso 1 calc R . . C64 C 1.1617(3) 0.3025(3) 0.77655(8) 0.0895(12) Uani 1 d . . . H64 H 1.2369 0.3023 0.7887 0.107 Uiso 1 calc R . . C65 C 1.0977(3) 0.2252(3) 0.77182(8) 0.0822(10) Uani 1 d . . . H65 H 1.1291 0.1719 0.7810 0.099 Uiso 1 calc R . . C66 C 0.9861(2) 0.2252(2) 0.75348(7) 0.0616(7) Uani 1 d . . . H66 H 0.9441 0.1714 0.7510 0.074 Uiso 1 calc R . . C67 C 0.4587(3) 0.1360(2) 0.77165(11) 0.0951(11) Uani 1 d . . . H67A H 0.3924 0.1427 0.7882 0.143 Uiso 1 calc R . . H67B H 0.4305 0.1036 0.7508 0.143 Uiso 1 calc R . . H67C H 0.4874 0.1938 0.7644 0.143 Uiso 1 calc R . . C68 C 0.5563(4) 0.0880(2) 0.78874(9) 0.0779(9) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.04366(16) 0.03921(18) 0.03053(14) -0.00524(12) 0.00395(11) -0.00895(13) N1 0.0518(11) 0.0391(12) 0.0434(11) -0.0075(9) 0.0045(9) -0.0030(9) N2 0.0694(14) 0.0378(13) 0.0617(13) 0.0056(10) 0.0056(11) -0.0014(11) N3 0.0379(9) 0.0359(11) 0.0319(9) -0.0011(8) 0.0011(7) -0.0051(8) N4 0.0481(11) 0.0405(11) 0.0332(9) -0.0003(8) 0.0000(8) -0.0099(9) N5 0.0497(11) 0.0350(11) 0.0465(11) -0.0024(9) 0.0021(9) -0.0048(9) N6 0.0427(11) 0.0586(13) 0.0440(11) -0.0080(10) 0.0092(9) -0.0136(10) N7 0.0506(13) 0.0531(14) 0.0559(13) -0.0047(10) -0.0039(10) -0.0078(11) N8 0.0648(14) 0.0572(14) 0.0384(11) -0.0109(10) 0.0065(10) -0.0094(11) N9 0.142(3) 0.067(2) 0.174(4) 0.018(2) -0.058(3) 0.002(2) B1 0.0461(15) 0.0445(17) 0.0393(14) 0.0028(12) -0.0042(11) -0.0121(12) B2 0.0336(12) 0.0403(15) 0.0358(12) 0.0003(11) 0.0001(10) -0.0017(11) C1 0.0674(17) 0.0482(17) 0.0625(17) -0.0162(14) 0.0099(13) -0.0023(14) C2 0.087(2) 0.0391(16) 0.082(2) -0.0100(15) 0.0139(17) -0.0020(15) C3 0.108(2) 0.0504(18) 0.078(2) 0.0203(15) 0.0179(18) -0.0036(17) C4 0.0486(14) 0.0343(14) 0.0455(13) 0.0004(10) 0.0004(11) -0.0024(11) C5 0.0588(15) 0.0419(14) 0.0404(12) 0.0064(10) 0.0104(11) -0.0023(11) C6 0.0540(14) 0.0401(14) 0.0349(12) -0.0037(10) 0.0078(10) -0.0020(11) C7 0.0416(12) 0.0374(14) 0.0368(12) -0.0011(10) 0.0032(9) -0.0077(10) C8 0.0762(19) 0.0511(17) 0.0627(17) -0.0128(13) 0.0122(14) 0.0091(14) C9 0.0596(15) 0.0393(15) 0.0522(15) 0.0092(12) -0.0040(12) -0.0070(12) C10 0.0618(15) 0.0469(16) 0.0373(12) 0.0075(11) -0.0033(11) -0.0148(12) C11 0.0457(13) 0.0696(18) 0.0360(12) -0.0082(11) -0.0047(10) -0.0071(12) C12 0.0460(14) 0.0763(19) 0.0514(15) -0.0165(13) 0.0017(11) -0.0209(13) C13 0.0466(15) 0.087(2) 0.085(2) -0.0183(17) 0.0114(14) -0.0027(15) C14 0.0686(18) 0.081(2) 0.0636(17) -0.0021(15) 0.0174(14) -0.0342(16) C15 0.0590(17) 0.085(2) 0.0524(16) 0.0030(15) -0.0054(13) -0.0242(16) C16 0.103(3) 0.228(5) 0.103(3) 0.000(3) -0.026(2) -0.098(3) C17 0.0711(18) 0.0572(18) 0.0449(15) -0.0124(12) 0.0095(13) -0.0141(14) C18 0.133(3) 0.112(3) 0.0410(16) -0.0167(17) 0.0184(17) -0.020(2) C19 0.0432(13) 0.0365(14) 0.0493(13) 0.0006(10) -0.0050(10) -0.0068(10) C20 0.0483(13) 0.0452(15) 0.0471(13) 0.0023(11) -0.0035(11) -0.0034(11) C21 0.0651(17) 0.0520(17) 0.0527(15) -0.0006(12) 0.0074(13) -0.0014(13) C22 0.0597(18) 0.066(2) 0.078(2) -0.0079(16) 0.0120(15) 0.0029(15) C23 0.0482(16) 0.084(2) 0.089(2) -0.0001(18) -0.0054(16) 0.0132(15) C24 0.0566(16) 0.0711(19) 0.0569(16) 0.0052(14) -0.0090(13) 0.0016(14) C25 0.0478(13) 0.0484(16) 0.0425(13) 0.0031(11) -0.0107(11) -0.0151(12) C26 0.086(2) 0.0543(19) 0.0573(16) 0.0066(14) 0.0029(15) -0.0103(15) C27 0.108(3) 0.0547(19) 0.086(2) 0.0217(17) 0.003(2) -0.0086(18) C28 0.080(2) 0.081(2) 0.072(2) 0.0343(18) -0.0070(17) -0.0245(19) C29 0.0647(18) 0.089(2) 0.0648(18) 0.0210(17) 0.0063(15) -0.0201(18) C30 0.0542(15) 0.0630(19) 0.0598(16) 0.0118(14) 0.0019(13) -0.0121(13) C31 0.0622(15) 0.0470(15) 0.0354(12) 0.0053(11) -0.0004(11) -0.0202(13) C32 0.0735(18) 0.0575(18) 0.0565(16) 0.0026(13) -0.0181(14) -0.0222(14) C33 0.116(3) 0.076(2) 0.0607(19) 0.0022(17) -0.0325(19) -0.043(2) C34 0.156(4) 0.066(2) 0.0368(15) -0.0088(14) 0.0043(19) -0.048(2) C35 0.114(3) 0.066(2) 0.0580(18) -0.0088(15) 0.0358(18) -0.0246(19) C36 0.0745(19) 0.0552(18) 0.0578(16) -0.0090(14) 0.0156(14) -0.0217(15) C37 0.0411(12) 0.0395(14) 0.0376(12) -0.0018(10) 0.0032(9) -0.0044(10) C38 0.0473(13) 0.0415(14) 0.0390(12) -0.0032(10) -0.0002(10) -0.0077(11) C39 0.0474(14) 0.0546(17) 0.0406(13) -0.0092(11) -0.0009(11) -0.0125(12) C40 0.0459(14) 0.0688(19) 0.0417(13) -0.0021(13) -0.0051(11) 0.0015(13) C41 0.0595(16) 0.0515(17) 0.0603(16) 0.0089(13) -0.0066(13) 0.0055(13) C42 0.0490(14) 0.0467(16) 0.0605(15) 0.0025(12) -0.0048(12) -0.0075(12) C43 0.0326(11) 0.0393(14) 0.0366(11) 0.0003(10) -0.0024(9) -0.0063(10) C44 0.0588(15) 0.0448(15) 0.0409(13) 0.0007(11) 0.0029(11) -0.0059(12) C45 0.0741(18) 0.0443(16) 0.0601(17) 0.0108(13) -0.0015(14) -0.0044(13) C46 0.0674(17) 0.066(2) 0.0507(16) 0.0234(14) -0.0029(13) -0.0072(15) C47 0.0679(17) 0.073(2) 0.0357(13) 0.0058(13) 0.0018(12) -0.0042(15) C48 0.0497(14) 0.0524(16) 0.0386(12) 0.0014(11) 0.0030(10) -0.0002(11) C49 0.0358(11) 0.0336(12) 0.0338(11) 0.0005(9) -0.0018(9) -0.0070(9) C50 0.0385(12) 0.0481(14) 0.0405(12) 0.0085(11) -0.0031(9) -0.0005(11) C51 0.0525(15) 0.0672(18) 0.0339(12) 0.0126(11) 0.0000(11) -0.0021(13) C52 0.0539(15) 0.0642(18) 0.0422(13) 0.0021(12) 0.0135(11) 0.0024(13) C53 0.0422(13) 0.0533(16) 0.0535(14) 0.0073(12) 0.0031(11) 0.0100(11) C54 0.0428(13) 0.0478(15) 0.0359(12) 0.0055(10) -0.0015(10) 0.0006(11) C55 0.0490(13) 0.0374(13) 0.0405(12) 0.0047(10) 0.0023(10) -0.0016(11) C56 0.0623(17) 0.0518(18) 0.081(2) -0.0111(15) 0.0189(15) -0.0091(14) C57 0.104(3) 0.051(2) 0.101(2) -0.0233(18) 0.029(2) -0.0038(19) C58 0.121(3) 0.0471(19) 0.087(2) -0.0218(16) 0.005(2) -0.020(2) C59 0.078(2) 0.064(2) 0.099(2) -0.0121(18) -0.0177(19) -0.0203(17) C60 0.0543(15) 0.0456(16) 0.0674(17) -0.0053(13) -0.0081(13) -0.0026(12) C61 0.0366(12) 0.0591(16) 0.0330(11) 0.0044(11) 0.0049(9) -0.0008(11) C62 0.0469(14) 0.077(2) 0.0405(13) 0.0027(13) -0.0039(11) -0.0093(13) C63 0.0541(17) 0.124(3) 0.0517(16) -0.0037(18) -0.0052(14) -0.0281(18) C64 0.0425(16) 0.171(4) 0.0550(18) 0.020(2) -0.0076(14) -0.002(2) C65 0.0518(18) 0.127(3) 0.068(2) 0.035(2) 0.0001(15) 0.0238(19) C66 0.0459(14) 0.077(2) 0.0616(16) 0.0178(14) 0.0013(12) 0.0093(13) C67 0.082(2) 0.071(2) 0.133(3) 0.025(2) -0.002(2) -0.0100(19) C68 0.099(3) 0.0448(19) 0.090(2) 0.0059(17) -0.008(2) -0.0156(18) _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 N4 2.0376(19) . ? Ni1 N8 2.0735(19) . ? Ni1 N1 2.079(2) . ? Ni1 N3 2.1330(16) . ? Ni1 N6 2.1481(18) . ? Ni1 N7 2.162(2) . ? N1 C4 1.320(3) . ? N1 C1 1.372(3) . ? N2 C4 1.338(3) . ? N2 C2 1.372(3) . ? N2 C3 1.465(3) . ? N3 C5 1.477(3) . ? N3 C6 1.479(3) . ? N3 C11 1.482(3) . ? N4 C7 1.326(3) . ? N4 C10 1.381(3) . ? N5 C7 1.344(3) . ? N5 C9 1.375(3) . ? N5 C8 1.455(3) . ? N6 C13 1.479(3) . ? N6 C14 1.481(3) . ? N6 C12 1.486(3) . ? N7 C15 1.114(3) . ? N8 C17 1.117(3) . ? N9 C68 1.109(4) . ? B1 C37 1.643(3) . ? B1 C25 1.648(3) . ? B1 C19 1.650(4) . ? B1 C31 1.660(4) . ? B2 C61 1.647(3) . ? B2 C55 1.648(3) . ? B2 C49 1.653(3) . ? B2 C43 1.654(3) . ? C1 C2 1.335(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.493(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.481(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.333(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.495(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.458(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.453(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.393(3) . ? C19 C24 1.403(3) . ? C20 C21 1.386(3) . ? C20 H20 0.9300 . ? C21 C22 1.363(4) . ? C21 H21 0.9300 . ? C22 C23 1.376(4) . ? C22 H22 0.9300 . ? C23 C24 1.384(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.389(4) . ? C25 C30 1.391(3) . ? C26 C27 1.388(4) . ? C26 H26 0.9300 . ? C27 C28 1.361(4) . ? C27 H27 0.9300 . ? C28 C29 1.366(4) . ? C28 H28 0.9300 . ? C29 C30 1.383(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.395(3) . ? C31 C36 1.398(4) . ? C32 C33 1.378(4) . ? C32 H32 0.9300 . ? C33 C34 1.367(5) . ? C33 H33 0.9300 . ? C34 C35 1.376(5) . ? C34 H34 0.9300 . ? C35 C36 1.376(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.395(3) . ? C37 C42 1.403(3) . ? C38 C39 1.386(3) . ? C38 H38 0.9300 . ? C39 C40 1.366(3) . ? C39 H39 0.9300 . ? C40 C41 1.379(4) . ? C40 H40 0.9300 . ? C41 C42 1.377(3) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.390(3) . ? C43 C44 1.395(3) . ? C44 C45 1.383(3) . ? C44 H44 0.9300 . ? C45 C46 1.374(4) . ? C45 H45 0.9300 . ? C46 C47 1.363(4) . ? C46 H46 0.9300 . ? C47 C48 1.384(3) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.391(3) . ? C49 C50 1.400(3) . ? C50 C51 1.383(3) . ? C50 H50 0.9300 . ? C51 C52 1.369(3) . ? C51 H51 0.9300 . ? C52 C53 1.371(3) . ? C52 H52 0.9300 . ? C53 C54 1.386(3) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.381(3) . ? C55 C56 1.392(3) . ? C56 C57 1.385(4) . ? C56 H56 0.9300 . ? C57 C58 1.354(4) . ? C57 H57 0.9300 . ? C58 C59 1.368(4) . ? C58 H58 0.9300 . ? C59 C60 1.386(4) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.392(3) . ? C61 C66 1.396(3) . ? C62 C63 1.396(4) . ? C62 H62 0.9300 . ? C63 C64 1.368(5) . ? C63 H63 0.9300 . ? C64 C65 1.362(5) . ? C64 H64 0.9300 . ? C65 C66 1.385(4) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.425(5) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 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 N4 Ni1 N8 99.09(8) . . ? N4 Ni1 N1 157.51(7) . . ? N8 Ni1 N1 101.30(8) . . ? N4 Ni1 N3 81.67(7) . . ? N8 Ni1 N3 176.12(7) . . ? N1 Ni1 N3 78.64(7) . . ? N4 Ni1 N6 91.77(7) . . ? N8 Ni1 N6 91.23(8) . . ? N1 Ni1 N6 97.17(8) . . ? N3 Ni1 N6 84.94(7) . . ? N4 Ni1 N7 88.43(8) . . ? N8 Ni1 N7 87.49(8) . . ? N1 Ni1 N7 83.09(8) . . ? N3 Ni1 N7 96.34(7) . . ? N6 Ni1 N7 178.72(7) . . ? C4 N1 C1 105.2(2) . . ? C4 N1 Ni1 111.43(15) . . ? C1 N1 Ni1 141.49(17) . . ? C4 N2 C2 106.8(2) . . ? C4 N2 C3 126.9(2) . . ? C2 N2 C3 126.3(2) . . ? C5 N3 C6 112.01(16) . . ? C5 N3 C11 109.91(18) . . ? C6 N3 C11 111.85(18) . . ? C5 N3 Ni1 108.11(12) . . ? C6 N3 Ni1 110.22(12) . . ? C11 N3 Ni1 104.41(12) . . ? C7 N4 C10 105.30(19) . . ? C7 N4 Ni1 112.58(15) . . ? C10 N4 Ni1 142.09(15) . . ? C7 N5 C9 106.92(19) . . ? C7 N5 C8 126.3(2) . . ? C9 N5 C8 126.8(2) . . ? C13 N6 C14 108.0(2) . . ? C13 N6 C12 110.9(2) . . ? C14 N6 C12 107.6(2) . . ? C13 N6 Ni1 112.06(16) . . ? C14 N6 Ni1 113.85(16) . . ? C12 N6 Ni1 104.40(13) . . ? C15 N7 Ni1 166.7(2) . . ? C17 N8 Ni1 175.5(2) . . ? C37 B1 C25 108.01(18) . . ? C37 B1 C19 109.48(18) . . ? C25 B1 C19 110.6(2) . . ? C37 B1 C31 110.5(2) . . ? C25 B1 C31 106.98(18) . . ? C19 B1 C31 111.21(18) . . ? C61 B2 C55 112.32(19) . . ? C61 B2 C49 107.51(17) . . ? C55 B2 C49 108.96(17) . . ? C61 B2 C43 109.86(17) . . ? C55 B2 C43 106.90(17) . . ? C49 B2 C43 111.33(18) . . ? C2 C1 N1 110.0(2) . . ? C2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? C1 C2 N2 106.6(2) . . ? C1 C2 H2 126.7 . . ? N2 C2 H2 126.7 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 111.5(2) . . ? N1 C4 C5 121.6(2) . . ? N2 C4 C5 126.8(2) . . ? N3 C5 C4 107.27(18) . . ? N3 C5 H5A 110.3 . . ? C4 C5 H5A 110.3 . . ? N3 C5 H5B 110.3 . . ? C4 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? N3 C6 C7 109.11(17) . . ? N3 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? N3 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N4 C7 N5 111.05(19) . . ? N4 C7 C6 123.0(2) . . ? N5 C7 C6 125.89(19) . . ? N5 C8 H8A 109.5 . . ? N5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N5 106.8(2) . . ? C10 C9 H9 126.6 . . ? N5 C9 H9 126.6 . . ? C9 C10 N4 109.9(2) . . ? C9 C10 H10 125.0 . . ? N4 C10 H10 125.0 . . ? N3 C11 C12 111.84(19) . . ? N3 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N3 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N6 C12 C11 110.6(2) . . ? N6 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N7 C15 C16 178.7(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 . . ? N8 C17 C18 179.0(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 113.5(2) . . ? C20 C19 B1 123.3(2) . . ? C24 C19 B1 123.2(2) . . ? C21 C20 C19 123.6(2) . . ? C21 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 118.6(3) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 123.7(3) . . ? C23 C24 H24 118.2 . . ? C19 C24 H24 118.2 . . ? C26 C25 C30 114.3(2) . . ? C26 C25 B1 124.3(2) . . ? C30 C25 B1 121.4(2) . . ? C27 C26 C25 122.6(3) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.1(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 119.5(3) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C25 123.8(3) . . ? C29 C30 H30 118.1 . . ? C25 C30 H30 118.1 . . ? C32 C31 C36 114.2(2) . . ? C32 C31 B1 122.4(2) . . ? C36 C31 B1 123.2(2) . . ? C33 C32 C31 123.2(3) . . ? C33 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 118.8(3) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 123.3(3) . . ? C35 C36 H36 118.3 . . ? C31 C36 H36 118.3 . . ? C38 C37 C42 114.1(2) . . ? C38 C37 B1 122.5(2) . . ? C42 C37 B1 123.4(2) . . ? C39 C38 C37 122.8(2) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C40 C39 C38 120.9(2) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 118.5(2) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? C42 C41 C40 120.1(2) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 123.6(2) . . ? C41 C42 H42 118.2 . . ? C37 C42 H42 118.2 . . ? C48 C43 C44 114.1(2) . . ? C48 C43 B2 122.2(2) . . ? C44 C43 B2 123.68(19) . . ? C45 C44 C43 123.1(2) . . ? C45 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C46 C45 C44 120.3(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C47 C46 C45 118.6(2) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C46 C47 C48 120.3(2) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 123.5(2) . . ? C47 C48 H48 118.3 . . ? C43 C48 H48 118.3 . . ? C54 C49 C50 114.30(19) . . ? C54 C49 B2 124.00(18) . . ? C50 C49 B2 121.66(19) . . ? C51 C50 C49 122.7(2) . . ? C51 C50 H50 118.6 . . ? C49 C50 H50 118.6 . . ? C52 C51 C50 120.6(2) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 118.9(2) . . ? C51 C52 H52 120.6 . . ? C53 C52 H52 120.6 . . ? C52 C53 C54 119.8(2) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C49 123.6(2) . . ? C53 C54 H54 118.2 . . ? C49 C54 H54 118.2 . . ? C60 C55 C56 114.0(2) . . ? C60 C55 B2 122.0(2) . . ? C56 C55 B2 123.7(2) . . ? C57 C56 C55 123.4(3) . . ? C57 C56 H56 118.3 . . ? C55 C56 H56 118.3 . . ? C58 C57 C56 120.1(3) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 119.0(3) . . ? C57 C58 H58 120.5 . . ? C59 C58 H58 120.5 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C55 C60 C59 123.3(3) . . ? C55 C60 H60 118.3 . . ? C59 C60 H60 118.3 . . ? C62 C61 C66 114.5(2) . . ? C62 C61 B2 121.8(2) . . ? C66 C61 B2 123.6(2) . . ? C61 C62 C63 123.0(3) . . ? C61 C62 H62 118.5 . . ? C63 C62 H62 118.5 . . ? C64 C63 C62 119.8(3) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C65 C64 C63 119.2(3) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C64 C65 C66 120.5(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C61 122.9(3) . . ? C65 C66 H66 118.6 . . ? C61 C66 H66 118.6 . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N9 C68 C67 178.6(4) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.289 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.043