# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Vincent Ritleng' _publ_contact_author_email vritleng@unistra.fr loop_ _publ_author_name 'Vincent Ritleng' 'Anna Magdalena Oertel' 'Michael J. Chetcuti' # Attachment '- CCDC 767229.cif' data_chet11a _database_code_depnum_ccdc_archive 'CCDC 767229' #TrackingRef '- CCDC 767229.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H54 N3 Ni, F6 P' _chemical_formula_sum 'C39 H54 F6 N3 Ni P' _chemical_formula_weight 768.53 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 13.7019(5) _cell_length_b 18.0171(7) _cell_length_c 16.5430(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4083.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25173 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26294 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4829 _reflns_number_gt 3025 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _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^)+(0.0373P)^2^+3.2120P] 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 4829 _refine_ls_number_parameters 261 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1337 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 C1 C 0.7196(3) 0.7500 0.4990(2) 0.0279(10) Uani 1 2 d S . . C2 C 0.5784(2) 0.78693(17) 0.43798(19) 0.0357(8) Uani 1 1 d . . . H2 H 0.5290 0.8182 0.4164 0.043 Uiso 1 1 calc R . . C3 C 0.6825(2) 0.88681(17) 0.4944(2) 0.0360(8) Uani 1 1 d . . . C4 C 0.6385(2) 0.91613(19) 0.5648(2) 0.0451(9) Uani 1 1 d . . . C5 C 0.6558(3) 0.9911(2) 0.5799(3) 0.0657(12) Uani 1 1 d . . . H5 H 0.6277 1.0133 0.6265 0.079 Uiso 1 1 calc R . . C6 C 0.7122(3) 1.0336(2) 0.5295(3) 0.0747(14) Uani 1 1 d . . . H6 H 0.7240 1.0842 0.5423 0.090 Uiso 1 1 calc R . . C7 C 0.7518(3) 1.00380(19) 0.4608(3) 0.0616(11) Uani 1 1 d . . . H7 H 0.7901 1.0342 0.4263 0.074 Uiso 1 1 calc R . . C8 C 0.7366(3) 0.92953(17) 0.4406(2) 0.0438(9) Uani 1 1 d . . . C9 C 0.5740(3) 0.8709(2) 0.6193(2) 0.0578(11) Uani 1 1 d . . . H9 H 0.5926 0.8175 0.6133 0.069 Uiso 1 1 calc R . . C10 C 0.4661(3) 0.8791(3) 0.5950(3) 0.0879(16) Uani 1 1 d . . . H10A H 0.4466 0.9313 0.5996 0.132 Uiso 1 1 calc R . . H10B H 0.4255 0.8487 0.6308 0.132 Uiso 1 1 calc R . . H10C H 0.4576 0.8625 0.5390 0.132 Uiso 1 1 calc R . . C11 C 0.5851(3) 0.8924(3) 0.7094(2) 0.0860(15) Uani 1 1 d . . . H11A H 0.6545 0.8970 0.7228 0.129 Uiso 1 1 calc R . . H11B H 0.5554 0.8540 0.7433 0.129 Uiso 1 1 calc R . . H11C H 0.5524 0.9400 0.7192 0.129 Uiso 1 1 calc R . . C12 C 0.7708(3) 0.90046(18) 0.3592(2) 0.0510(10) Uani 1 1 d . . . H12 H 0.7684 0.8450 0.3610 0.061 Uiso 1 1 calc R . . C13 C 0.8758(3) 0.9234(2) 0.3390(3) 0.0814(15) Uani 1 1 d . . . H13A H 0.8806 0.9777 0.3388 0.122 Uiso 1 1 calc R . . H13B H 0.8934 0.9042 0.2855 0.122 Uiso 1 1 calc R . . H13C H 0.9203 0.9031 0.3796 0.122 Uiso 1 1 calc R . . C14 C 0.6995(4) 0.9266(2) 0.2938(2) 0.0789(14) Uani 1 1 d . . . H14A H 0.6337 0.9089 0.3067 0.118 Uiso 1 1 calc R . . H14B H 0.7197 0.9068 0.2413 0.118 Uiso 1 1 calc R . . H14C H 0.6995 0.9810 0.2917 0.118 Uiso 1 1 calc R . . C15 C 0.9860(2) 0.79068(18) 0.5856(2) 0.0403(8) Uani 1 1 d . . . C16 C 0.9063(2) 0.8157(2) 0.6303(2) 0.0448(9) Uani 1 1 d . . . C17 C 0.8528(3) 0.7500 0.6542(3) 0.0477(13) Uani 1 2 d S . . C18 C 1.0639(3) 0.8371(2) 0.5472(2) 0.0588(11) Uani 1 1 d . . . H18A H 1.0418 0.8887 0.5438 0.088 Uiso 1 1 calc R . . H18B H 1.0774 0.8184 0.4927 0.088 Uiso 1 1 calc R . . H18C H 1.1235 0.8345 0.5798 0.088 Uiso 1 1 calc R . . C19 C 0.8802(3) 0.8942(2) 0.6502(3) 0.0687(13) Uani 1 1 d . . . H19A H 0.9253 0.9280 0.6226 0.103 Uiso 1 1 calc R . . H19B H 0.8849 0.9017 0.7088 0.103 Uiso 1 1 calc R . . H19C H 0.8134 0.9044 0.6324 0.103 Uiso 1 1 calc R . . C20 C 0.7678(4) 0.7500 0.7123(4) 0.081(2) Uani 1 2 d S . . C21 C 0.9521(3) 0.7500 0.3669(3) 0.0378(11) Uani 1 2 d S . . C22 C 1.0088(5) 0.7500 0.2923(4) 0.0542(16) Uani 1 2 d S . . F1 F 0.20504(13) 0.81260(10) 0.37776(12) 0.0501(5) Uani 1 1 d . . . F2 F 0.3039(2) 0.7500 0.46359(17) 0.0692(9) Uani 1 2 d S . . F3 F 0.36878(13) 0.81287(11) 0.35842(13) 0.0541(6) Uani 1 1 d . . . F4 F 0.27035(19) 0.7500 0.27280(15) 0.0452(7) Uani 1 2 d S . . N1 N 0.66374(17) 0.80961(13) 0.47536(15) 0.0292(6) Uani 1 1 d . . . N2 N 0.9074(3) 0.7500 0.4246(2) 0.0367(9) Uani 1 2 d S . . Ni1 Ni 0.85416(4) 0.7500 0.52945(3) 0.03182(18) Uani 1 2 d S . . P1 P 0.28668(8) 0.7500 0.36842(7) 0.0364(3) Uani 1 2 d S . . H22B H 1.049(3) 0.710(2) 0.295(3) 0.100(18) Uiso 1 1 d . . . H22A H 0.967(6) 0.7500 0.244(6) 0.16(3) Uiso 1 2 d S . . H20A H 0.705(5) 0.7500 0.690(4) 0.11(3) Uiso 1 2 d SD . . H20B H 0.778(4) 0.7058(6) 0.748(4) 0.21(3) Uiso 1 1 d 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 C1 0.030(2) 0.031(2) 0.023(2) 0.000 0.0034(19) 0.000 C2 0.0309(17) 0.0412(16) 0.0350(19) -0.0008(14) -0.0126(15) 0.0039(14) C3 0.0380(18) 0.0301(17) 0.040(2) -0.0116(15) -0.0108(16) 0.0063(15) C4 0.041(2) 0.053(2) 0.042(2) -0.0163(17) -0.0137(17) 0.0148(18) C5 0.073(3) 0.060(3) 0.064(3) -0.035(2) -0.017(2) 0.024(2) C6 0.090(4) 0.036(2) 0.097(4) -0.031(3) -0.028(3) 0.010(2) C7 0.067(3) 0.0315(18) 0.086(3) -0.007(2) -0.008(2) -0.0009(18) C8 0.051(2) 0.0279(17) 0.052(2) -0.0051(16) -0.0087(19) 0.0039(16) C9 0.053(2) 0.078(3) 0.042(2) -0.019(2) 0.0057(19) 0.014(2) C10 0.049(3) 0.136(4) 0.078(3) -0.032(3) 0.005(2) 0.004(3) C11 0.076(3) 0.131(4) 0.051(3) -0.028(3) 0.009(2) 0.025(3) C12 0.072(3) 0.0310(18) 0.050(2) 0.0029(17) 0.005(2) 0.0018(19) C13 0.094(4) 0.048(2) 0.103(4) 0.016(2) 0.036(3) -0.009(2) C14 0.134(4) 0.054(2) 0.049(3) 0.002(2) -0.007(3) 0.020(3) C15 0.0290(17) 0.054(2) 0.038(2) -0.0036(16) -0.0085(15) -0.0038(15) C16 0.0312(18) 0.063(2) 0.040(2) -0.0137(18) -0.0120(16) 0.0051(18) C17 0.027(2) 0.093(4) 0.023(3) 0.000 -0.009(2) 0.000 C18 0.041(2) 0.065(3) 0.071(3) -0.001(2) -0.006(2) -0.016(2) C19 0.056(3) 0.081(3) 0.069(3) -0.034(2) -0.024(2) 0.015(2) C20 0.034(4) 0.175(8) 0.033(3) 0.000 0.005(3) 0.000 C21 0.027(2) 0.052(3) 0.035(3) 0.000 -0.006(2) 0.000 C22 0.040(3) 0.091(5) 0.031(3) 0.000 0.005(3) 0.000 F1 0.0383(11) 0.0522(12) 0.0599(14) -0.0111(10) 0.0008(10) 0.0059(9) F2 0.063(2) 0.113(3) 0.0320(18) 0.000 -0.0110(15) 0.000 F3 0.0379(11) 0.0590(12) 0.0652(14) -0.0098(11) 0.0011(10) -0.0116(10) F4 0.0565(18) 0.0481(15) 0.0310(16) 0.000 -0.0018(13) 0.000 N1 0.0275(14) 0.0316(13) 0.0285(14) -0.0034(11) -0.0035(11) 0.0016(11) N2 0.030(2) 0.047(2) 0.033(2) 0.000 0.0013(19) 0.000 Ni1 0.0259(3) 0.0433(3) 0.0263(3) 0.000 -0.0015(3) 0.000 P1 0.0284(6) 0.0481(7) 0.0328(7) 0.000 -0.0004(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.376(3) 8_575 ? C1 N1 1.376(3) . ? C1 Ni1 1.911(4) . ? C2 C2 1.331(6) 8_575 ? C2 N1 1.385(4) . ? C2 H2 0.9500 . ? C3 C8 1.391(5) . ? C3 C4 1.414(5) . ? C3 N1 1.449(4) . ? C4 C5 1.393(5) . ? C4 C9 1.502(5) . ? C5 C6 1.372(6) . ? C5 H5 0.9500 . ? C6 C7 1.369(6) . ? C6 H6 0.9500 . ? C7 C8 1.395(5) . ? C7 H7 0.9500 . ? C8 C12 1.519(5) . ? C9 C10 1.538(5) . ? C9 C11 1.548(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.532(5) . ? C12 C13 1.533(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.392(5) . ? C15 C15 1.466(7) 8_575 ? C15 C18 1.498(5) . ? C15 Ni1 2.159(3) . ? C16 C17 1.447(4) . ? C16 C19 1.497(5) . ? C16 Ni1 2.166(3) . ? C17 C16 1.447(4) 8_575 ? C17 C20 1.511(7) . ? C17 Ni1 2.063(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.93(6) . ? C20 H20B 1.00(4) . ? C21 N2 1.135(6) . ? C21 C22 1.458(7) . ? C22 H22B 0.91(4) . ? C22 H22A 0.98(9) . ? F1 P1 1.596(2) . ? F2 P1 1.592(3) . ? F3 P1 1.605(2) . ? F4 P1 1.597(3) . ? N2 Ni1 1.881(4) . ? Ni1 C15 2.159(3) 8_575 ? Ni1 C16 2.166(3) 8_575 ? P1 F1 1.596(2) 8_575 ? P1 F3 1.605(2) 8_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N1 102.6(3) 8_575 . ? N1 C1 Ni1 127.72(17) 8_575 . ? N1 C1 Ni1 127.72(17) . . ? C2 C2 N1 107.16(16) 8_575 . ? C2 C2 H2 126.4 8_575 . ? N1 C2 H2 126.4 . . ? C8 C3 C4 123.2(3) . . ? C8 C3 N1 119.1(3) . . ? C4 C3 N1 117.5(3) . . ? C5 C4 C3 115.9(4) . . ? C5 C4 C9 121.2(4) . . ? C3 C4 C9 122.9(3) . . ? C6 C5 C4 121.9(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 121.1(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C3 C8 C7 117.2(3) . . ? C3 C8 C12 122.7(3) . . ? C7 C8 C12 119.8(3) . . ? C4 C9 C10 110.8(3) . . ? C4 C9 C11 112.6(3) . . ? C10 C9 C11 108.8(3) . . ? C4 C9 H9 108.1 . . ? C10 C9 H9 108.1 . . ? C11 C9 H9 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 C14 108.8(3) . . ? C8 C12 C13 112.9(3) . . ? C14 C12 C13 111.2(3) . . ? C8 C12 H12 107.9 . . ? C14 C12 H12 107.9 . . ? C13 C12 H12 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C15 108.9(2) . 8_575 ? C16 C15 C18 127.1(3) . . ? C15 C15 C18 123.9(2) 8_575 . ? C16 C15 Ni1 71.50(18) . . ? C15 C15 Ni1 70.16(9) 8_575 . ? C18 C15 Ni1 127.1(2) . . ? C15 C16 C17 106.1(3) . . ? C15 C16 C19 127.6(4) . . ? C17 C16 C19 126.3(3) . . ? C15 C16 Ni1 70.95(19) . . ? C17 C16 Ni1 66.2(2) . . ? C19 C16 Ni1 127.4(2) . . ? C16 C17 C16 109.7(4) 8_575 . ? C16 C17 C20 124.4(2) 8_575 . ? C16 C17 C20 124.4(2) . . ? C16 C17 Ni1 73.9(2) 8_575 . ? C16 C17 Ni1 73.9(2) . . ? C20 C17 Ni1 130.0(4) . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 117(4) . . ? C17 C20 H20B 106(4) . . ? H20A C20 H20B 111(3) . . ? N2 C21 C22 179.4(5) . . ? C21 C22 H22B 106(3) . . ? C21 C22 H22A 112(5) . . ? H22B C22 H22A 114(4) . . ? C1 N1 C2 111.5(2) . . ? C1 N1 C3 126.1(2) . . ? C2 N1 C3 122.0(2) . . ? C21 N2 Ni1 170.1(4) . . ? N2 Ni1 C1 97.54(17) . . ? N2 Ni1 C17 157.68(18) . . ? C1 Ni1 C17 104.78(18) . . ? N2 Ni1 C15 94.15(14) . . ? C1 Ni1 C15 156.96(11) . . ? C17 Ni1 C15 64.97(15) . . ? N2 Ni1 C15 94.15(14) . 8_575 ? C1 Ni1 C15 156.96(11) . 8_575 ? C17 Ni1 C15 64.97(15) . 8_575 ? C15 Ni1 C15 39.69(18) . 8_575 ? N2 Ni1 C16 125.57(13) . . ? C1 Ni1 C16 121.43(13) . . ? C17 Ni1 C16 39.91(12) . . ? C15 Ni1 C16 37.54(12) . . ? C15 Ni1 C16 65.03(13) 8_575 . ? N2 Ni1 C16 125.57(13) . 8_575 ? C1 Ni1 C16 121.43(13) . 8_575 ? C17 Ni1 C16 39.91(12) . 8_575 ? C15 Ni1 C16 65.03(13) . 8_575 ? C15 Ni1 C16 37.54(12) 8_575 8_575 ? C16 Ni1 C16 66.2(2) . 8_575 ? F2 P1 F1 90.47(12) . . ? F2 P1 F1 90.47(12) . 8_575 ? F1 P1 F1 89.94(15) . 8_575 ? F2 P1 F4 179.52(17) . . ? F1 P1 F4 89.87(11) . . ? F1 P1 F4 89.87(11) 8_575 . ? F2 P1 F3 89.89(12) . 8_575 ? F1 P1 F3 179.64(14) . 8_575 ? F1 P1 F3 90.14(10) 8_575 8_575 ? F4 P1 F3 89.78(12) . 8_575 ? F2 P1 F3 89.89(12) . . ? F1 P1 F3 90.14(10) . . ? F1 P1 F3 179.64(14) 8_575 . ? F4 P1 F3 89.78(12) . . ? F3 P1 F3 89.78(15) 8_575 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C3 C4 C5 -2.6(5) . . . . ? N1 C3 C4 C5 -178.2(3) . . . . ? C8 C3 C4 C9 175.3(3) . . . . ? N1 C3 C4 C9 -0.2(5) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C9 C4 C5 C6 -178.1(4) . . . . ? C4 C5 C6 C7 1.7(6) . . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? C4 C3 C8 C7 3.6(5) . . . . ? N1 C3 C8 C7 179.1(3) . . . . ? C4 C3 C8 C12 -170.7(3) . . . . ? N1 C3 C8 C12 4.8(5) . . . . ? C6 C7 C8 C3 -1.9(6) . . . . ? C6 C7 C8 C12 172.5(4) . . . . ? C5 C4 C9 C10 85.2(4) . . . . ? C3 C4 C9 C10 -92.7(4) . . . . ? C5 C4 C9 C11 -37.0(5) . . . . ? C3 C4 C9 C11 145.1(3) . . . . ? C3 C8 C12 C14 97.7(4) . . . . ? C7 C8 C12 C14 -76.4(4) . . . . ? C3 C8 C12 C13 -138.3(3) . . . . ? C7 C8 C12 C13 47.5(5) . . . . ? C15 C15 C16 C17 -3.5(3) 8_575 . . . ? C18 C15 C16 C17 180.0(3) . . . . ? Ni1 C15 C16 C17 57.0(2) . . . . ? C15 C15 C16 C19 176.5(3) 8_575 . . . ? C18 C15 C16 C19 -0.1(6) . . . . ? Ni1 C15 C16 C19 -123.0(4) . . . . ? C15 C15 C16 Ni1 -60.50(10) 8_575 . . . ? C18 C15 C16 Ni1 122.9(3) . . . . ? C15 C16 C17 C16 5.7(5) . . . 8_575 ? C19 C16 C17 C16 -174.2(2) . . . 8_575 ? Ni1 C16 C17 C16 65.8(3) . . . 8_575 ? C15 C16 C17 C20 172.1(4) . . . . ? C19 C16 C17 C20 -7.9(7) . . . . ? Ni1 C16 C17 C20 -127.9(5) . . . . ? C15 C16 C17 Ni1 -60.1(2) . . . . ? C19 C16 C17 Ni1 120.0(3) . . . . ? N1 C1 N1 C2 -0.8(4) 8_575 . . . ? Ni1 C1 N1 C2 164.2(3) . . . . ? N1 C1 N1 C3 172.0(2) 8_575 . . . ? Ni1 C1 N1 C3 -23.0(5) . . . . ? C2 C2 N1 C1 0.5(3) 8_575 . . . ? C2 C2 N1 C3 -172.6(2) 8_575 . . . ? C8 C3 N1 C1 92.4(4) . . . . ? C4 C3 N1 C1 -91.8(4) . . . . ? C8 C3 N1 C2 -95.5(4) . . . . ? C4 C3 N1 C2 80.3(4) . . . . ? N1 C1 Ni1 N2 80.7(3) 8_575 . . . ? N1 C1 Ni1 N2 -80.7(3) . . . . ? N1 C1 Ni1 C17 -99.3(3) 8_575 . . . ? N1 C1 Ni1 C17 99.3(3) . . . . ? N1 C1 Ni1 C15 -159.4(3) 8_575 . . . ? N1 C1 Ni1 C15 39.1(6) . . . . ? N1 C1 Ni1 C15 -39.1(6) 8_575 . . 8_575 ? N1 C1 Ni1 C15 159.4(3) . . . 8_575 ? N1 C1 Ni1 C16 -139.1(3) 8_575 . . . ? N1 C1 Ni1 C16 59.5(4) . . . . ? N1 C1 Ni1 C16 -59.5(4) 8_575 . . 8_575 ? N1 C1 Ni1 C16 139.1(3) . . . 8_575 ? C16 C17 Ni1 N2 -58.33(19) 8_575 . . . ? C16 C17 Ni1 N2 58.33(19) . . . . ? C20 C17 Ni1 N2 180.000(2) . . . . ? C16 C17 Ni1 C1 121.67(19) 8_575 . . . ? C16 C17 Ni1 C1 -121.67(19) . . . . ? C20 C17 Ni1 C1 0.0 . . . . ? C16 C17 Ni1 C15 -80.3(2) 8_575 . . . ? C16 C17 Ni1 C15 36.3(2) . . . . ? C20 C17 Ni1 C15 158.00(10) . . . . ? C16 C17 Ni1 C15 -36.3(2) 8_575 . . 8_575 ? C16 C17 Ni1 C15 80.3(2) . . . 8_575 ? C20 C17 Ni1 C15 -158.00(10) . . . 8_575 ? C16 C17 Ni1 C16 -116.7(4) 8_575 . . . ? C20 C17 Ni1 C16 121.67(19) . . . . ? C16 C17 Ni1 C16 116.7(4) . . . 8_575 ? C20 C17 Ni1 C16 -121.67(19) . . . 8_575 ? C16 C15 Ni1 N2 149.6(2) . . . . ? C15 C15 Ni1 N2 -91.50(5) 8_575 . . . ? C18 C15 Ni1 N2 26.6(3) . . . . ? C16 C15 Ni1 C1 29.2(5) . . . . ? C15 C15 Ni1 C1 148.1(4) 8_575 . . . ? C18 C15 Ni1 C1 -93.9(5) . . . . ? C16 C15 Ni1 C17 -38.6(2) . . . . ? C15 C15 Ni1 C17 80.30(8) 8_575 . . . ? C18 C15 Ni1 C17 -161.6(3) . . . . ? C16 C15 Ni1 C15 -118.9(2) . . . 8_575 ? C18 C15 Ni1 C15 118.1(3) . . . 8_575 ? C15 C15 Ni1 C16 118.9(2) 8_575 . . . ? C18 C15 Ni1 C16 -123.0(4) . . . . ? C16 C15 Ni1 C16 -82.8(3) . . . 8_575 ? C15 C15 Ni1 C16 36.06(13) 8_575 . . 8_575 ? C18 C15 Ni1 C16 154.1(3) . . . 8_575 ? C15 C16 Ni1 N2 -38.3(3) . . . . ? C17 C16 Ni1 N2 -156.6(2) . . . . ? C19 C16 Ni1 N2 84.9(4) . . . . ? C15 C16 Ni1 C1 -167.08(19) . . . . ? C17 C16 Ni1 C1 74.7(2) . . . . ? C19 C16 Ni1 C1 -43.8(4) . . . . ? C15 C16 Ni1 C17 118.3(3) . . . . ? C19 C16 Ni1 C17 -118.5(4) . . . . ? C17 C16 Ni1 C15 -118.3(3) . . . . ? C19 C16 Ni1 C15 123.3(4) . . . . ? C15 C16 Ni1 C15 38.1(2) . . . 8_575 ? C17 C16 Ni1 C15 -80.2(2) . . . 8_575 ? C19 C16 Ni1 C15 161.3(4) . . . 8_575 ? C15 C16 Ni1 C16 79.4(2) . . . 8_575 ? C17 C16 Ni1 C16 -38.8(2) . . . 8_575 ? C19 C16 Ni1 C16 -157.3(3) . . . 8_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.301 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.060 # Attachment '- CCDC 75553.cif' data_chet21 _database_code_depnum_ccdc_archive 'CCDC 775553' #TrackingRef '- CCDC 75553.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H51 Cl N2 Ni' _chemical_formula_sum 'C37 H51 Cl N2 Ni' _chemical_formula_weight 617.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.9474(8) _cell_length_b 31.263(3) _cell_length_c 10.6055(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.510(4) _cell_angle_gamma 90.00 _cell_volume 3953.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15043 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14280 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7141 _reflns_number_gt 5068 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _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^)+(0.0861P)^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 SHELXL _refine_ls_extinction_coef 0.0043(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(17) _refine_ls_number_reflns 7141 _refine_ls_number_parameters 384 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6327(4) 0.15930(15) 0.2185(4) 0.0274(10) Uani 1 1 d . . . C2 C 0.7444(4) 0.21227(16) 0.1471(4) 0.0303(10) Uani 1 1 d . . . H2 H 0.7677 0.2396 0.1196 0.036 Uiso 1 1 calc R . . C3 C 0.8089(4) 0.17768(16) 0.1658(4) 0.0325(11) Uani 1 1 d . . . H3 H 0.8867 0.1756 0.1527 0.039 Uiso 1 1 calc R . . C4 C 0.5389(4) 0.22816(16) 0.1483(4) 0.0303(10) Uani 1 1 d . . . C5 C 0.5035(4) 0.25456(17) 0.2419(4) 0.0333(12) Uani 1 1 d . . . C6 C 0.4081(4) 0.28003(18) 0.2126(5) 0.0422(13) Uani 1 1 d . . . H6 H 0.3796 0.2980 0.2755 0.051 Uiso 1 1 calc R . . C7 C 0.3556(5) 0.27895(18) 0.0924(5) 0.0441(13) Uani 1 1 d . . . H7 H 0.2902 0.2957 0.0744 0.053 Uiso 1 1 calc R . . C8 C 0.3966(4) 0.25418(18) -0.0008(5) 0.0413(12) Uani 1 1 d . . . H8 H 0.3607 0.2547 -0.0831 0.050 Uiso 1 1 calc R . . C9 C 0.4913(4) 0.22806(16) 0.0238(4) 0.0340(11) Uani 1 1 d . . . C10 C 0.5674(5) 0.2604(2) 0.3683(4) 0.0415(14) Uani 1 1 d . . . H10 H 0.6223 0.2364 0.3791 0.050 Uiso 1 1 calc R . . C11 C 0.4926(6) 0.2590(3) 0.4788(5) 0.072(2) Uani 1 1 d . . . H11A H 0.4351 0.2813 0.4683 0.108 Uiso 1 1 calc R . . H11B H 0.5380 0.2639 0.5576 0.108 Uiso 1 1 calc R . . H11C H 0.4565 0.2309 0.4818 0.108 Uiso 1 1 calc R . . C12 C 0.6345(6) 0.3022(3) 0.3651(7) 0.077(2) Uani 1 1 d . . . H12A H 0.6830 0.3015 0.2939 0.116 Uiso 1 1 calc R . . H12B H 0.6806 0.3054 0.4442 0.116 Uiso 1 1 calc R . . H12C H 0.5827 0.3265 0.3551 0.116 Uiso 1 1 calc R . . C13 C 0.5430(5) 0.2041(2) -0.0819(4) 0.0443(14) Uani 1 1 d . . . H13 H 0.5885 0.1798 -0.0448 0.053 Uiso 1 1 calc R . . C14 C 0.4544(6) 0.1861(2) -0.1802(5) 0.0601(17) Uani 1 1 d . . . H14A H 0.3982 0.1697 -0.1369 0.090 Uiso 1 1 calc R . . H14B H 0.4911 0.1673 -0.2391 0.090 Uiso 1 1 calc R . . H14C H 0.4177 0.2097 -0.2271 0.090 Uiso 1 1 calc R . . C15 C 0.6215(5) 0.2344(2) -0.1519(5) 0.0635(19) Uani 1 1 d . . . H15A H 0.5802 0.2602 -0.1787 0.095 Uiso 1 1 calc R . . H15B H 0.6479 0.2197 -0.2261 0.095 Uiso 1 1 calc R . . H15C H 0.6859 0.2422 -0.0949 0.095 Uiso 1 1 calc R . . C16 C 0.7796(4) 0.10110(16) 0.2164(4) 0.0342(11) Uani 1 1 d . . . C17 C 0.7592(4) 0.07482(16) 0.1097(5) 0.0391(12) Uani 1 1 d . . . C18 C 0.7992(5) 0.03312(18) 0.1208(6) 0.0508(14) Uani 1 1 d . . . H18 H 0.7866 0.0141 0.0515 0.061 Uiso 1 1 calc R . . C19 C 0.8560(5) 0.01863(19) 0.2279(6) 0.0523(15) Uani 1 1 d . . . H19 H 0.8819 -0.0101 0.2321 0.063 Uiso 1 1 calc R . . C20 C 0.8759(5) 0.0450(2) 0.3288(6) 0.0576(16) Uani 1 1 d . . . H20 H 0.9149 0.0342 0.4029 0.069 Uiso 1 1 calc R . . C21 C 0.8398(4) 0.08816(17) 0.3257(5) 0.0387(12) Uani 1 1 d . . . C22 C 0.7048(5) 0.0922(2) -0.0129(5) 0.0488(14) Uani 1 1 d . . . H22 H 0.6490 0.1147 0.0076 0.059 Uiso 1 1 calc R . . C23 C 0.6446(7) 0.0576(2) -0.0916(6) 0.072(2) Uani 1 1 d . . . H23A H 0.6999 0.0397 -0.1312 0.108 Uiso 1 1 calc R . . H23B H 0.5948 0.0709 -0.1572 0.108 Uiso 1 1 calc R . . H23C H 0.6003 0.0398 -0.0370 0.108 Uiso 1 1 calc R . . C24 C 0.7923(6) 0.1125(2) -0.0956(6) 0.070(2) Uani 1 1 d . . . H24A H 0.8162 0.1402 -0.0597 0.105 Uiso 1 1 calc R . . H24B H 0.7590 0.1168 -0.1815 0.105 Uiso 1 1 calc R . . H24C H 0.8574 0.0935 -0.0983 0.105 Uiso 1 1 calc R . . C25 C 0.8755(5) 0.1182(2) 0.4318(5) 0.0431(13) Uani 1 1 d . . . H25 H 0.8262 0.1440 0.4239 0.052 Uiso 1 1 calc R . . C26 C 0.8610(6) 0.0983(2) 0.5634(5) 0.0619(17) Uani 1 1 d . . . H26A H 0.7830 0.0892 0.5693 0.093 Uiso 1 1 calc R . . H26B H 0.8802 0.1196 0.6290 0.093 Uiso 1 1 calc R . . H26C H 0.9107 0.0735 0.5752 0.093 Uiso 1 1 calc R . . C27 C 0.9963(5) 0.1331(2) 0.4222(6) 0.0568(16) Uani 1 1 d . . . H27A H 1.0473 0.1089 0.4385 0.085 Uiso 1 1 calc R . . H27B H 1.0134 0.1556 0.4846 0.085 Uiso 1 1 calc R . . H27C H 1.0057 0.1443 0.3372 0.085 Uiso 1 1 calc R . . C28 C 0.3435(4) 0.13517(17) 0.2722(5) 0.0349(11) Uani 1 1 d . . . C29 C 0.3612(4) 0.12409(17) 0.3998(5) 0.0361(12) Uani 1 1 d . . . C30 C 0.4282(4) 0.08460(17) 0.4070(5) 0.0402(12) Uani 1 1 d . . . C31 C 0.4510(5) 0.07228(17) 0.2843(5) 0.0444(13) Uani 1 1 d . . . C32 C 0.4056(4) 0.10493(16) 0.2008(4) 0.0357(11) Uani 1 1 d . . . C33 C 0.2751(4) 0.1709(2) 0.2187(6) 0.0495(14) Uani 1 1 d . . . H33A H 0.2030 0.1599 0.1837 0.074 Uiso 1 1 calc R . . H33B H 0.3148 0.1848 0.1516 0.074 Uiso 1 1 calc R . . H33C H 0.2623 0.1917 0.2853 0.074 Uiso 1 1 calc R . . C34 C 0.3181(5) 0.1459(2) 0.5118(5) 0.0532(16) Uani 1 1 d . . . H34A H 0.2665 0.1688 0.4836 0.080 Uiso 1 1 calc R . . H34B H 0.3810 0.1580 0.5635 0.080 Uiso 1 1 calc R . . H34C H 0.2783 0.1252 0.5620 0.080 Uiso 1 1 calc R . . C35 C 0.4636(6) 0.0621(2) 0.5275(6) 0.071(2) Uani 1 1 d . . . H35A H 0.3979 0.0490 0.5629 0.106 Uiso 1 1 calc R . . H35B H 0.4975 0.0827 0.5880 0.106 Uiso 1 1 calc R . . H35C H 0.5185 0.0399 0.5105 0.106 Uiso 1 1 calc R . . C36 C 0.5095(6) 0.0315(2) 0.2459(7) 0.0707(19) Uani 1 1 d . . . H36A H 0.5537 0.0199 0.3189 0.106 Uiso 1 1 calc R . . H36B H 0.5592 0.0380 0.1782 0.106 Uiso 1 1 calc R . . H36C H 0.4533 0.0105 0.2157 0.106 Uiso 1 1 calc R . . C37 C 0.3973(5) 0.1032(2) 0.0611(5) 0.0633(18) Uani 1 1 d . . . H37A H 0.3218 0.0939 0.0316 0.095 Uiso 1 1 calc R . . H37B H 0.4527 0.0830 0.0320 0.095 Uiso 1 1 calc R . . H37C H 0.4119 0.1317 0.0271 0.095 Uiso 1 1 calc R . . N1 N 0.6370(3) 0.20068(12) 0.1755(3) 0.0276(8) Uani 1 1 d . . . N2 N 0.7415(3) 0.14552(12) 0.2076(3) 0.0277(9) Uani 1 1 d . . . Cl1 Cl 0.60993(10) 0.15612(5) 0.49934(10) 0.0462(4) Uani 1 1 d . . . Ni1 Ni 0.52511(4) 0.133996(18) 0.32014(4) 0.03041(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(2) 0.032(3) 0.0225(19) -0.0008(19) -0.0035(17) 0.002(2) C2 0.030(3) 0.031(3) 0.029(2) -0.001(2) 0.0017(19) 0.000(2) C3 0.032(3) 0.031(3) 0.034(2) 0.002(2) 0.002(2) -0.005(2) C4 0.026(2) 0.033(3) 0.031(2) 0.006(2) -0.0016(18) -0.002(2) C5 0.031(3) 0.033(3) 0.036(2) -0.002(2) 0.003(2) 0.004(2) C6 0.036(3) 0.042(3) 0.049(3) -0.001(3) 0.006(2) 0.008(3) C7 0.034(3) 0.046(4) 0.052(3) 0.010(3) -0.003(2) 0.009(3) C8 0.036(3) 0.048(3) 0.039(3) 0.006(2) -0.005(2) 0.002(3) C9 0.043(3) 0.031(3) 0.029(2) 0.006(2) 0.002(2) -0.007(2) C10 0.045(3) 0.044(4) 0.034(2) -0.008(2) -0.004(2) 0.007(3) C11 0.078(5) 0.101(6) 0.036(3) -0.006(3) 0.004(3) 0.045(4) C12 0.069(5) 0.080(6) 0.079(4) -0.024(4) -0.032(4) 0.005(4) C13 0.047(3) 0.059(4) 0.026(2) -0.002(2) -0.002(2) 0.003(3) C14 0.070(4) 0.073(5) 0.036(3) -0.010(3) -0.009(3) -0.002(4) C15 0.053(4) 0.102(6) 0.036(3) 0.008(3) 0.008(3) -0.007(4) C16 0.035(3) 0.032(3) 0.037(2) 0.002(2) 0.012(2) -0.003(2) C17 0.038(3) 0.029(3) 0.052(3) -0.007(2) 0.014(2) 0.000(2) C18 0.058(4) 0.031(3) 0.064(4) -0.012(3) 0.019(3) 0.001(3) C19 0.059(4) 0.029(3) 0.071(4) 0.002(3) 0.022(3) 0.008(3) C20 0.057(4) 0.053(4) 0.064(4) 0.014(3) 0.020(3) 0.008(3) C21 0.033(3) 0.036(3) 0.048(3) 0.008(2) 0.013(2) 0.000(2) C22 0.056(3) 0.047(4) 0.044(3) -0.010(3) 0.006(2) 0.004(3) C23 0.088(5) 0.072(5) 0.055(3) -0.030(3) 0.002(3) 0.003(4) C24 0.113(6) 0.043(4) 0.054(3) -0.015(3) 0.005(4) -0.005(4) C25 0.043(3) 0.049(3) 0.037(3) 0.007(2) 0.003(2) 0.012(3) C26 0.088(5) 0.054(4) 0.043(3) 0.015(3) 0.001(3) 0.012(4) C27 0.045(3) 0.064(4) 0.061(3) 0.011(3) -0.003(3) 0.001(3) C28 0.028(3) 0.037(3) 0.040(3) 0.005(2) 0.005(2) -0.008(2) C29 0.025(3) 0.043(3) 0.039(3) -0.001(2) 0.000(2) -0.010(2) C30 0.037(3) 0.037(3) 0.046(3) 0.007(2) 0.004(2) -0.001(2) C31 0.043(3) 0.035(3) 0.057(3) -0.006(3) 0.011(3) -0.007(3) C32 0.034(3) 0.038(3) 0.036(2) -0.006(2) 0.004(2) -0.010(2) C33 0.030(3) 0.056(4) 0.062(3) 0.017(3) -0.005(2) 0.000(3) C34 0.047(3) 0.073(4) 0.041(3) -0.020(3) 0.013(3) -0.013(3) C35 0.073(4) 0.076(5) 0.064(4) 0.039(4) 0.006(3) 0.000(4) C36 0.081(5) 0.036(3) 0.097(5) -0.002(3) 0.025(4) -0.007(4) C37 0.059(4) 0.089(5) 0.041(3) -0.006(3) 0.004(3) -0.021(4) N1 0.035(2) 0.025(2) 0.0237(17) 0.0002(16) 0.0028(15) -0.0003(18) N2 0.025(2) 0.028(2) 0.0303(19) 0.0038(16) 0.0049(16) 0.0025(17) Cl1 0.0374(7) 0.0684(10) 0.0327(6) -0.0070(6) 0.0009(5) -0.0092(7) Ni1 0.0283(3) 0.0352(3) 0.0279(3) -0.0009(3) 0.0028(2) -0.0032(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 C1 N1 1.374(6) . ? C1 N2 1.381(6) . ? C1 Ni1 1.900(4) . ? C2 C3 1.336(7) . ? C2 N1 1.384(6) . ? C2 H2 0.9500 . ? C3 N2 1.378(6) . ? C3 H3 0.9500 . ? C4 C5 1.377(7) . ? C4 C9 1.406(6) . ? C4 N1 1.468(6) . ? C5 C6 1.409(7) . ? C5 C10 1.513(6) . ? C6 C7 1.386(8) . ? C6 H6 0.9500 . ? C7 C8 1.370(8) . ? C7 H7 0.9500 . ? C8 C9 1.406(7) . ? C8 H8 0.9500 . ? C9 C13 1.511(7) . ? C10 C11 1.517(8) . ? C10 C12 1.534(10) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.547(7) . ? C13 C15 1.552(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.387(7) . ? C16 C17 1.407(7) . ? C16 N2 1.462(6) . ? C17 C18 1.391(7) . ? C17 C22 1.519(8) . ? C18 C19 1.365(8) . ? C18 H18 0.9500 . ? C19 C20 1.360(9) . ? C19 H19 0.9500 . ? C20 C21 1.417(8) . ? C20 H20 0.9500 . ? C21 C25 1.507(8) . ? C22 C23 1.521(9) . ? C22 C24 1.542(9) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.525(8) . ? C25 C26 1.548(7) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.401(7) . ? C28 C32 1.444(7) . ? C28 C33 1.476(8) . ? C28 Ni1 2.198(5) . ? C29 C30 1.471(8) . ? C29 C34 1.488(7) . ? C29 Ni1 2.202(5) . ? C30 C31 1.399(7) . ? C30 C35 1.497(8) . ? C30 Ni1 2.169(5) . ? C31 C32 1.436(7) . ? C31 C36 1.521(8) . ? C31 Ni1 2.147(5) . ? C32 C37 1.480(7) . ? C32 Ni1 2.061(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Cl1 Ni1 2.2094(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 102.2(4) . . ? N1 C1 Ni1 128.4(3) . . ? N2 C1 Ni1 126.2(3) . . ? C3 C2 N1 106.9(4) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 107.2(4) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C5 C4 C9 123.6(5) . . ? C5 C4 N1 119.1(4) . . ? C9 C4 N1 117.1(4) . . ? C4 C5 C6 117.4(4) . . ? C4 C5 C10 123.4(5) . . ? C6 C5 C10 119.0(5) . . ? C7 C6 C5 120.2(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 121.0(5) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C4 116.6(4) . . ? C8 C9 C13 120.8(4) . . ? C4 C9 C13 122.5(5) . . ? C5 C10 C11 113.1(5) . . ? C5 C10 C12 108.6(5) . . ? C11 C10 C12 112.1(6) . . ? C5 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 112.7(5) . . ? C9 C13 C15 109.8(5) . . ? C14 C13 C15 108.0(4) . . ? C9 C13 H13 108.7 . . ? C14 C13 H13 108.7 . . ? C15 C13 H13 108.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.9(5) . . ? C21 C16 N2 118.3(4) . . ? C17 C16 N2 117.7(4) . . ? C18 C17 C16 115.9(5) . . ? C18 C17 C22 122.3(5) . . ? C16 C17 C22 121.6(5) . . ? C19 C18 C17 122.1(5) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C20 C19 C18 120.5(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 121.4(6) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C16 C21 C20 116.0(5) . . ? C16 C21 C25 123.4(5) . . ? C20 C21 C25 120.3(5) . . ? C17 C22 C23 112.1(5) . . ? C17 C22 C24 111.4(5) . . ? C23 C22 C24 107.2(5) . . ? C17 C22 H22 108.7 . . ? C23 C22 H22 108.7 . . ? C24 C22 H22 108.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 111.5(5) . . ? C21 C25 C26 112.4(5) . . ? C27 C25 C26 110.0(5) . . ? C21 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C32 107.1(5) . . ? C29 C28 C33 127.2(5) . . ? C32 C28 C33 125.7(4) . . ? C29 C28 Ni1 71.6(3) . . ? C32 C28 Ni1 65.1(3) . . ? C33 C28 Ni1 128.1(4) . . ? C28 C29 C30 107.8(4) . . ? C28 C29 C34 128.2(5) . . ? C30 C29 C34 123.9(5) . . ? C28 C29 Ni1 71.3(3) . . ? C30 C29 Ni1 69.1(3) . . ? C34 C29 Ni1 127.0(4) . . ? C31 C30 C29 108.6(4) . . ? C31 C30 C35 127.1(5) . . ? C29 C30 C35 124.2(5) . . ? C31 C30 Ni1 70.2(3) . . ? C29 C30 Ni1 71.6(3) . . ? C35 C30 Ni1 124.6(4) . . ? C30 C31 C32 106.9(4) . . ? C30 C31 C36 126.8(5) . . ? C32 C31 C36 126.3(5) . . ? C30 C31 Ni1 71.9(3) . . ? C32 C31 Ni1 66.8(3) . . ? C36 C31 Ni1 127.5(4) . . ? C31 C32 C28 109.2(4) . . ? C31 C32 C37 126.3(5) . . ? C28 C32 C37 122.9(5) . . ? C31 C32 Ni1 73.3(3) . . ? C28 C32 Ni1 75.4(3) . . ? C37 C32 Ni1 129.2(4) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C1 N1 C2 111.9(4) . . ? C1 N1 C4 124.8(4) . . ? C2 N1 C4 122.9(4) . . ? C3 N2 C1 111.8(4) . . ? C3 N2 C16 121.9(4) . . ? C1 N2 C16 125.5(4) . . ? C1 Ni1 C32 107.61(18) . . ? C1 Ni1 C31 124.04(19) . . ? C32 Ni1 C31 39.8(2) . . ? C1 Ni1 C30 159.2(2) . . ? C32 Ni1 C30 65.10(19) . . ? C31 Ni1 C30 37.83(19) . . ? C1 Ni1 C28 123.65(18) . . ? C32 Ni1 C28 39.47(19) . . ? C31 Ni1 C28 65.4(2) . . ? C30 Ni1 C28 64.24(19) . . ? C1 Ni1 C29 157.65(19) . . ? C32 Ni1 C29 64.82(18) . . ? C31 Ni1 C29 64.83(19) . . ? C30 Ni1 C29 39.3(2) . . ? C28 Ni1 C29 37.13(18) . . ? C1 Ni1 Cl1 93.85(13) . . ? C32 Ni1 Cl1 158.53(13) . . ? C31 Ni1 Cl1 126.59(16) . . ? C30 Ni1 Cl1 94.95(15) . . ? C28 Ni1 Cl1 126.02(13) . . ? C29 Ni1 Cl1 94.92(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -1.1(5) . . . . ? C9 C4 C5 C6 5.7(7) . . . . ? N1 C4 C5 C6 -179.2(4) . . . . ? C9 C4 C5 C10 -168.6(5) . . . . ? N1 C4 C5 C10 6.6(8) . . . . ? C4 C5 C6 C7 -2.0(8) . . . . ? C10 C5 C6 C7 172.5(5) . . . . ? C5 C6 C7 C8 -1.7(8) . . . . ? C6 C7 C8 C9 2.0(8) . . . . ? C7 C8 C9 C4 1.4(7) . . . . ? C7 C8 C9 C13 -174.0(5) . . . . ? C5 C4 C9 C8 -5.3(7) . . . . ? N1 C4 C9 C8 179.4(4) . . . . ? C5 C4 C9 C13 170.0(5) . . . . ? N1 C4 C9 C13 -5.3(7) . . . . ? C4 C5 C10 C11 -135.1(6) . . . . ? C6 C5 C10 C11 50.7(8) . . . . ? C4 C5 C10 C12 99.8(7) . . . . ? C6 C5 C10 C12 -74.3(6) . . . . ? C8 C9 C13 C14 -38.5(7) . . . . ? C4 C9 C13 C14 146.4(5) . . . . ? C8 C9 C13 C15 81.9(6) . . . . ? C4 C9 C13 C15 -93.2(6) . . . . ? C21 C16 C17 C18 2.8(7) . . . . ? N2 C16 C17 C18 178.4(4) . . . . ? C21 C16 C17 C22 -172.6(5) . . . . ? N2 C16 C17 C22 3.0(7) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C22 C17 C18 C19 174.6(5) . . . . ? C17 C18 C19 C20 -0.2(9) . . . . ? C18 C19 C20 C21 -0.7(9) . . . . ? C17 C16 C21 C20 -3.6(7) . . . . ? N2 C16 C21 C20 -179.2(4) . . . . ? C17 C16 C21 C25 170.8(4) . . . . ? N2 C16 C21 C25 -4.7(7) . . . . ? C19 C20 C21 C16 2.5(8) . . . . ? C19 C20 C21 C25 -172.1(5) . . . . ? C18 C17 C22 C23 30.4(7) . . . . ? C16 C17 C22 C23 -154.5(5) . . . . ? C18 C17 C22 C24 -89.7(6) . . . . ? C16 C17 C22 C24 85.4(6) . . . . ? C16 C21 C25 C27 -97.2(6) . . . . ? C20 C21 C25 C27 77.0(6) . . . . ? C16 C21 C25 C26 138.8(5) . . . . ? C20 C21 C25 C26 -47.0(7) . . . . ? C32 C28 C29 C30 -4.1(5) . . . . ? C33 C28 C29 C30 176.0(5) . . . . ? Ni1 C28 C29 C30 -59.7(3) . . . . ? C32 C28 C29 C34 178.3(5) . . . . ? C33 C28 C29 C34 -1.6(9) . . . . ? Ni1 C28 C29 C34 122.8(5) . . . . ? C32 C28 C29 Ni1 55.6(3) . . . . ? C33 C28 C29 Ni1 -124.3(5) . . . . ? C28 C29 C30 C31 0.3(6) . . . . ? C34 C29 C30 C31 178.0(5) . . . . ? Ni1 C29 C30 C31 -60.8(4) . . . . ? C28 C29 C30 C35 -179.2(5) . . . . ? C34 C29 C30 C35 -1.5(9) . . . . ? Ni1 C29 C30 C35 119.8(6) . . . . ? C28 C29 C30 Ni1 61.1(3) . . . . ? C34 C29 C30 Ni1 -121.3(5) . . . . ? C29 C30 C31 C32 3.7(6) . . . . ? C35 C30 C31 C32 -176.9(6) . . . . ? Ni1 C30 C31 C32 -57.9(3) . . . . ? C29 C30 C31 C36 -174.6(5) . . . . ? C35 C30 C31 C36 4.8(10) . . . . ? Ni1 C30 C31 C36 123.8(6) . . . . ? C29 C30 C31 Ni1 61.6(4) . . . . ? C35 C30 C31 Ni1 -119.0(6) . . . . ? C30 C31 C32 C28 -6.3(6) . . . . ? C36 C31 C32 C28 172.0(5) . . . . ? Ni1 C31 C32 C28 -67.5(3) . . . . ? C30 C31 C32 C37 -172.1(5) . . . . ? C36 C31 C32 C37 6.2(9) . . . . ? Ni1 C31 C32 C37 126.7(5) . . . . ? C30 C31 C32 Ni1 61.2(4) . . . . ? C36 C31 C32 Ni1 -120.5(6) . . . . ? C29 C28 C32 C31 6.5(5) . . . . ? C33 C28 C32 C31 -173.6(5) . . . . ? Ni1 C28 C32 C31 66.1(3) . . . . ? C29 C28 C32 C37 172.9(5) . . . . ? C33 C28 C32 C37 -7.3(8) . . . . ? Ni1 C28 C32 C37 -127.5(5) . . . . ? C29 C28 C32 Ni1 -59.6(3) . . . . ? C33 C28 C32 Ni1 120.3(5) . . . . ? N2 C1 N1 C2 -3.4(4) . . . . ? Ni1 C1 N1 C2 157.0(3) . . . . ? N2 C1 N1 C4 169.9(4) . . . . ? Ni1 C1 N1 C4 -29.7(6) . . . . ? C3 C2 N1 C1 3.0(5) . . . . ? C3 C2 N1 C4 -170.5(4) . . . . ? C5 C4 N1 C1 92.3(5) . . . . ? C9 C4 N1 C1 -92.2(5) . . . . ? C5 C4 N1 C2 -95.1(5) . . . . ? C9 C4 N1 C2 80.4(5) . . . . ? C2 C3 N2 C1 -1.1(5) . . . . ? C2 C3 N2 C16 169.1(4) . . . . ? N1 C1 N2 C3 2.7(5) . . . . ? Ni1 C1 N2 C3 -158.3(3) . . . . ? N1 C1 N2 C16 -167.0(4) . . . . ? Ni1 C1 N2 C16 32.0(6) . . . . ? C21 C16 N2 C3 86.0(5) . . . . ? C17 C16 N2 C3 -89.8(5) . . . . ? C21 C16 N2 C1 -105.2(5) . . . . ? C17 C16 N2 C1 78.9(5) . . . . ? N1 C1 Ni1 C32 94.8(4) . . . . ? N2 C1 Ni1 C32 -109.2(4) . . . . ? N1 C1 Ni1 C31 135.5(4) . . . . ? N2 C1 Ni1 C31 -68.5(5) . . . . ? N1 C1 Ni1 C30 160.7(5) . . . . ? N2 C1 Ni1 C30 -43.3(7) . . . . ? N1 C1 Ni1 C28 54.4(5) . . . . ? N2 C1 Ni1 C28 -149.6(4) . . . . ? N1 C1 Ni1 C29 28.5(7) . . . . ? N2 C1 Ni1 C29 -175.5(4) . . . . ? N1 C1 Ni1 Cl1 -84.4(4) . . . . ? N2 C1 Ni1 Cl1 71.6(4) . . . . ? C31 C32 Ni1 C1 122.4(3) . . . . ? C28 C32 Ni1 C1 -121.9(3) . . . . ? C37 C32 Ni1 C1 -1.1(6) . . . . ? C28 C32 Ni1 C31 115.6(4) . . . . ? C37 C32 Ni1 C31 -123.6(7) . . . . ? C31 C32 Ni1 C30 -36.6(3) . . . . ? C28 C32 Ni1 C30 79.0(3) . . . . ? C37 C32 Ni1 C30 -160.2(6) . . . . ? C31 C32 Ni1 C28 -115.6(4) . . . . ? C37 C32 Ni1 C28 120.8(7) . . . . ? C31 C32 Ni1 C29 -80.2(3) . . . . ? C28 C32 Ni1 C29 35.4(3) . . . . ? C37 C32 Ni1 C29 156.2(6) . . . . ? C31 C32 Ni1 Cl1 -59.7(5) . . . . ? C28 C32 Ni1 Cl1 56.0(6) . . . . ? C37 C32 Ni1 Cl1 176.8(4) . . . . ? C30 C31 Ni1 C1 165.7(3) . . . . ? C32 C31 Ni1 C1 -76.1(3) . . . . ? C36 C31 Ni1 C1 42.8(6) . . . . ? C30 C31 Ni1 C32 -118.2(4) . . . . ? C36 C31 Ni1 C32 119.0(6) . . . . ? C32 C31 Ni1 C30 118.2(4) . . . . ? C36 C31 Ni1 C30 -122.9(7) . . . . ? C30 C31 Ni1 C28 -79.1(3) . . . . ? C32 C31 Ni1 C28 39.1(3) . . . . ? C36 C31 Ni1 C28 158.0(6) . . . . ? C30 C31 Ni1 C29 -38.0(3) . . . . ? C32 C31 Ni1 C29 80.2(3) . . . . ? C36 C31 Ni1 C29 -160.9(6) . . . . ? C30 C31 Ni1 Cl1 38.7(4) . . . . ? C32 C31 Ni1 Cl1 156.8(2) . . . . ? C36 C31 Ni1 Cl1 -84.2(5) . . . . ? C31 C30 Ni1 C1 -35.1(7) . . . . ? C29 C30 Ni1 C1 -153.6(5) . . . . ? C35 C30 Ni1 C1 87.0(7) . . . . ? C31 C30 Ni1 C32 38.5(3) . . . . ? C29 C30 Ni1 C32 -80.0(3) . . . . ? C35 C30 Ni1 C32 160.6(6) . . . . ? C29 C30 Ni1 C31 -118.5(4) . . . . ? C35 C30 Ni1 C31 122.1(6) . . . . ? C31 C30 Ni1 C28 82.4(3) . . . . ? C29 C30 Ni1 C28 -36.1(3) . . . . ? C35 C30 Ni1 C28 -155.5(6) . . . . ? C31 C30 Ni1 C29 118.5(4) . . . . ? C35 C30 Ni1 C29 -119.4(6) . . . . ? C31 C30 Ni1 Cl1 -149.8(3) . . . . ? C29 C30 Ni1 Cl1 91.7(3) . . . . ? C35 C30 Ni1 Cl1 -27.6(5) . . . . ? C29 C28 Ni1 C1 -164.0(3) . . . . ? C32 C28 Ni1 C1 76.3(3) . . . . ? C33 C28 Ni1 C1 -40.7(5) . . . . ? C29 C28 Ni1 C32 119.7(4) . . . . ? C33 C28 Ni1 C32 -117.0(6) . . . . ? C29 C28 Ni1 C31 80.2(3) . . . . ? C32 C28 Ni1 C31 -39.4(3) . . . . ? C33 C28 Ni1 C31 -156.5(5) . . . . ? C29 C28 Ni1 C30 38.2(3) . . . . ? C32 C28 Ni1 C30 -81.4(3) . . . . ? C33 C28 Ni1 C30 161.6(5) . . . . ? C32 C28 Ni1 C29 -119.7(4) . . . . ? C33 C28 Ni1 C29 123.3(6) . . . . ? C29 C28 Ni1 Cl1 -38.3(4) . . . . ? C32 C28 Ni1 Cl1 -158.0(2) . . . . ? C33 C28 Ni1 Cl1 85.0(5) . . . . ? C28 C29 Ni1 C1 37.1(6) . . . . ? C30 C29 Ni1 C1 155.5(5) . . . . ? C34 C29 Ni1 C1 -87.2(7) . . . . ? C28 C29 Ni1 C32 -37.6(3) . . . . ? C30 C29 Ni1 C32 80.8(3) . . . . ? C34 C29 Ni1 C32 -161.9(6) . . . . ? C28 C29 Ni1 C31 -81.9(3) . . . . ? C30 C29 Ni1 C31 36.5(3) . . . . ? C34 C29 Ni1 C31 153.9(6) . . . . ? C28 C29 Ni1 C30 -118.4(4) . . . . ? C34 C29 Ni1 C30 117.4(6) . . . . ? C30 C29 Ni1 C28 118.4(4) . . . . ? C34 C29 Ni1 C28 -124.2(6) . . . . ? C28 C29 Ni1 Cl1 149.8(3) . . . . ? C30 C29 Ni1 Cl1 -91.8(3) . . . . ? C34 C29 Ni1 Cl1 25.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.131 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.158 0.000 -0.015 384.1 160.0 2 0.658 0.500 -0.022 384.1 160.0 _platon_squeeze_details ; The residual electron density was assigned to two molecules of the toluene solvent [320/4 = 80 e per asymmetric unit; two molecules of C7H8 would give 100e]. ;