# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Tilley, T Don' loop_ _publ_author_name T.D.Tilley 'Michael Lipschutz' data_shelxl_a _database_code_depnum_ccdc_archive 'CCDC 879064' #TrackingRef '- X-ray Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(N(SiMe3)(DIPP))2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 N2 Ni Si2' _chemical_formula_weight 555.62 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9248(4) _cell_length_b 9.1680(4) _cell_length_c 10.9493(5) _cell_angle_alpha 102.092(2) _cell_angle_beta 92.571(2) _cell_angle_gamma 114.391(2) _cell_volume 789.11(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.39 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9196 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 15509 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.39 _reflns_number_total 2891 _reflns_number_gt 2713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.3414P] 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 2891 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.58800(17) 0.07697(17) 0.24294(12) 0.0154(3) Uani 1 1 d . . . C2 C 0.73548(17) 0.22771(17) 0.27750(13) 0.0164(3) Uani 1 1 d . . . C3 C 0.86820(18) 0.23724(18) 0.35601(13) 0.0203(3) Uani 1 1 d . . . H3 H 0.9673 0.3375 0.3790 0.024 Uiso 1 1 calc R . . C4 C 0.85905(19) 0.10402(19) 0.40128(14) 0.0221(3) Uani 1 1 d . . . H4 H 0.9509 0.1129 0.4547 0.026 Uiso 1 1 calc R . . C5 C 0.71428(19) -0.04265(19) 0.36780(14) 0.0215(3) Uani 1 1 d . . . H5 H 0.7081 -0.1339 0.3990 0.026 Uiso 1 1 calc R . . C6 C 0.57811(18) -0.05901(17) 0.28965(13) 0.0175(3) Uani 1 1 d . . . C7 C 0.42270(19) -0.22276(17) 0.25268(14) 0.0199(3) Uani 1 1 d . . . H7 H 0.3324 -0.2020 0.2135 0.024 Uiso 1 1 calc R . . C8 C 0.4494(2) -0.35104(19) 0.15332(15) 0.0290(4) Uani 1 1 d . . . H8A H 0.5416 -0.3698 0.1872 0.044 Uiso 1 1 calc R . . H8B H 0.4759 -0.3103 0.0774 0.044 Uiso 1 1 calc R . . H8C H 0.3479 -0.4552 0.1317 0.044 Uiso 1 1 calc R . . C9 C 0.3627(2) -0.29035(19) 0.36692(15) 0.0279(4) Uani 1 1 d . . . H9A H 0.4437 -0.3226 0.4025 0.042 Uiso 1 1 calc R . . H9B H 0.2548 -0.3871 0.3404 0.042 Uiso 1 1 calc R . . H9C H 0.3514 -0.2047 0.4310 0.042 Uiso 1 1 calc R . . C10 C 0.75278(18) 0.37591(17) 0.22786(13) 0.0190(3) Uani 1 1 d . . . H10 H 0.6396 0.3544 0.1892 0.023 Uiso 1 1 calc R . . C11 C 0.8185(2) 0.53667(18) 0.33309(15) 0.0253(3) Uani 1 1 d . . . H11A H 0.7480 0.5210 0.3998 0.038 Uiso 1 1 calc R . . H11B H 0.8164 0.6261 0.2983 0.038 Uiso 1 1 calc R . . H11C H 0.9329 0.5655 0.3683 0.038 Uiso 1 1 calc R . . C12 C 0.8644(2) 0.3956(2) 0.12392(15) 0.0278(4) Uani 1 1 d . . . H12A H 0.9755 0.4134 0.1586 0.042 Uiso 1 1 calc R . . H12B H 0.8728 0.4907 0.0923 0.042 Uiso 1 1 calc R . . H12C H 0.8161 0.2952 0.0545 0.042 Uiso 1 1 calc R . . C13 C 0.10746(19) -0.08443(18) 0.22154(15) 0.0226(3) Uani 1 1 d . . . H13A H 0.0786 -0.1807 0.1502 0.034 Uiso 1 1 calc R . . H13B H 0.0109 -0.0602 0.2312 0.034 Uiso 1 1 calc R . . H13C H 0.1403 -0.1083 0.2989 0.034 Uiso 1 1 calc R . . C14 C 0.2139(2) 0.1519(2) 0.05109(15) 0.0260(3) Uani 1 1 d . . . H14A H 0.3015 0.2546 0.0400 0.039 Uiso 1 1 calc R . . H14B H 0.1127 0.1670 0.0638 0.039 Uiso 1 1 calc R . . H14C H 0.1906 0.0623 -0.0244 0.039 Uiso 1 1 calc R . . C15 C 0.3440(2) 0.27244(19) 0.33496(15) 0.0258(3) Uani 1 1 d . . . H15A H 0.3927 0.2474 0.4053 0.039 Uiso 1 1 calc R . . H15B H 0.2451 0.2873 0.3571 0.039 Uiso 1 1 calc R . . H15C H 0.4257 0.3742 0.3179 0.039 Uiso 1 1 calc R . . N1 N 0.45461(14) 0.06117(14) 0.15574(10) 0.0156(2) Uani 1 1 d . . . Si1 Si 0.28409(5) 0.09839(5) 0.19158(3) 0.01601(11) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.0000 0.01491(9) Uani 1 2 d S . . 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 0.0149(7) 0.0169(7) 0.0141(6) 0.0011(5) 0.0037(5) 0.0077(6) C2 0.0159(7) 0.0176(7) 0.0151(7) 0.0021(5) 0.0046(5) 0.0074(6) C3 0.0139(7) 0.0211(7) 0.0215(7) 0.0019(6) 0.0028(6) 0.0050(6) C4 0.0162(7) 0.0297(8) 0.0226(7) 0.0057(6) 0.0012(6) 0.0127(6) C5 0.0223(8) 0.0231(8) 0.0243(7) 0.0089(6) 0.0064(6) 0.0131(6) C6 0.0174(7) 0.0171(7) 0.0179(7) 0.0029(5) 0.0053(6) 0.0078(6) C7 0.0199(8) 0.0160(7) 0.0239(7) 0.0058(6) 0.0020(6) 0.0076(6) C8 0.0333(9) 0.0201(8) 0.0274(8) 0.0010(6) 0.0037(7) 0.0079(7) C9 0.0275(9) 0.0217(8) 0.0296(8) 0.0080(7) 0.0082(7) 0.0047(7) C10 0.0159(7) 0.0164(7) 0.0203(7) 0.0035(6) 0.0007(6) 0.0034(6) C11 0.0250(8) 0.0176(7) 0.0278(8) 0.0019(6) 0.0011(6) 0.0059(6) C12 0.0291(9) 0.0244(8) 0.0242(8) 0.0071(6) 0.0069(7) 0.0052(7) C13 0.0185(8) 0.0219(8) 0.0277(8) 0.0078(6) 0.0057(6) 0.0079(6) C14 0.0205(8) 0.0270(8) 0.0294(8) 0.0122(7) -0.0014(6) 0.0073(7) C15 0.0231(8) 0.0239(8) 0.0274(8) -0.0013(6) 0.0029(6) 0.0110(7) N1 0.0156(6) 0.0143(6) 0.0147(5) 0.0022(4) 0.0011(5) 0.0050(5) Si1 0.0144(2) 0.0144(2) 0.0173(2) 0.00320(15) 0.00048(15) 0.00491(16) Ni1 0.01554(15) 0.01533(14) 0.01262(13) 0.00204(10) 0.00054(10) 0.00631(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.416(2) . ? C1 C2 1.421(2) . ? C1 N1 1.4309(18) . ? C2 C3 1.393(2) . ? C2 C10 1.519(2) . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.388(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 C7 1.522(2) . ? C7 C8 1.531(2) . ? C7 C9 1.532(2) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.535(2) . ? C10 C12 1.536(2) . ? 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 Si1 1.8699(15) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.8666(15) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.8620(15) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N1 Si1 1.7358(12) . ? N1 Ni1 1.7987(11) . ? Ni1 N1 1.7987(11) 2_655 ? 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 C6 C1 C2 119.66(13) . . ? C6 C1 N1 120.60(12) . . ? C2 C1 N1 119.65(12) . . ? C3 C2 C1 118.83(13) . . ? C3 C2 C10 119.66(13) . . ? C1 C2 C10 121.49(13) . . ? C4 C3 C2 121.58(13) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.33(14) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 121.49(14) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.10(13) . . ? C5 C6 C7 120.08(13) . . ? C1 C6 C7 120.81(13) . . ? C6 C7 C8 111.25(12) . . ? C6 C7 C9 112.40(12) . . ? C8 C7 C9 110.77(12) . . ? C6 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 112.43(12) . . ? C2 C10 C12 110.66(12) . . ? C11 C10 C12 110.48(12) . . ? C2 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? 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 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 N1 Si1 127.16(9) . . ? C1 N1 Ni1 106.66(9) . . ? Si1 N1 Ni1 126.16(7) . . ? N1 Si1 C15 110.44(6) . . ? N1 Si1 C14 105.94(7) . . ? C15 Si1 C14 110.70(8) . . ? N1 Si1 C13 113.40(6) . . ? C15 Si1 C13 107.53(7) . . ? C14 Si1 C13 108.83(7) . . ? N1 Ni1 N1 180.00(8) 2_655 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.380 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.042 data_shelxl_b _database_code_depnum_ccdc_archive 'CCDC 879065' #TrackingRef '- X-ray Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(N(SiMe3)(DIPP))2(DMAP) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H62 N4 Ni Si2' _chemical_formula_weight 677.80 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5555(4) _cell_length_b 12.6703(5) _cell_length_c 16.2859(6) _cell_angle_alpha 84.922(2) _cell_angle_beta 74.854(2) _cell_angle_gamma 69.522(2) _cell_volume 1969.57(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 25.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9025 _exptl_absorpt_correction_T_max 0.9659 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 37916 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.40 _reflns_number_total 7213 _reflns_number_gt 6101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.2003P] 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 7213 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.81270(18) 0.44646(16) 0.73955(12) 0.0151(4) Uani 1 1 d . . . C2 C 0.78240(19) 0.49411(16) 0.66205(12) 0.0166(4) Uani 1 1 d . . . C3 C 0.8215(2) 0.58625(17) 0.62839(13) 0.0221(5) Uani 1 1 d . . . H3 H 0.8036 0.6167 0.5755 0.026 Uiso 1 1 calc R . . C4 C 0.8859(2) 0.63405(17) 0.67036(14) 0.0248(5) Uani 1 1 d . . . H4 H 0.9098 0.6980 0.6472 0.030 Uiso 1 1 calc R . . C5 C 0.9151(2) 0.58873(17) 0.74592(13) 0.0226(5) Uani 1 1 d . . . H5 H 0.9592 0.6223 0.7746 0.027 Uiso 1 1 calc R . . C6 C 0.88179(19) 0.49463(16) 0.78156(12) 0.0177(4) Uani 1 1 d . . . C7 C 0.9237(2) 0.44225(18) 0.86267(13) 0.0224(5) Uani 1 1 d . . . H7 H 0.9402 0.3598 0.8600 0.027 Uiso 1 1 calc R . . C8 C 0.8089(2) 0.4882(2) 0.94297(14) 0.0352(6) Uani 1 1 d . . . H8A H 0.7219 0.4808 0.9378 0.053 Uiso 1 1 calc R . . H8B H 0.7947 0.5679 0.9502 0.053 Uiso 1 1 calc R . . H8C H 0.8363 0.4455 0.9924 0.053 Uiso 1 1 calc R . . C9 C 1.0588(2) 0.4540(2) 0.87167(15) 0.0355(6) Uani 1 1 d . . . H9A H 1.1331 0.4250 0.8203 0.053 Uiso 1 1 calc R . . H9B H 1.0857 0.4110 0.9211 0.053 Uiso 1 1 calc R . . H9C H 1.0442 0.5336 0.8794 0.053 Uiso 1 1 calc R . . C10 C 0.7116(2) 0.44512(17) 0.61310(13) 0.0213(4) Uani 1 1 d . . . H10 H 0.6839 0.3847 0.6489 0.026 Uiso 1 1 calc R . . C11 C 0.8108(3) 0.3911(2) 0.52982(15) 0.0375(6) Uani 1 1 d . . . H11A H 0.7625 0.3595 0.5001 0.056 Uiso 1 1 calc R . . H11B H 0.8921 0.3308 0.5419 0.056 Uiso 1 1 calc R . . H11C H 0.8416 0.4481 0.4939 0.056 Uiso 1 1 calc R . . C12 C 0.5787(2) 0.5336(2) 0.59567(15) 0.0334(6) Uani 1 1 d . . . H12A H 0.5155 0.5676 0.6495 0.050 Uiso 1 1 calc R . . H12B H 0.5324 0.4974 0.5680 0.050 Uiso 1 1 calc R . . H12C H 0.6033 0.5922 0.5584 0.050 Uiso 1 1 calc R . . C13 C 0.6095(3) 0.2895(2) 0.93507(15) 0.0388(6) Uani 1 1 d . . . H13A H 0.6626 0.2093 0.9239 0.058 Uiso 1 1 calc R . . H13B H 0.5133 0.2986 0.9663 0.058 Uiso 1 1 calc R . . H13C H 0.6528 0.3201 0.9691 0.058 Uiso 1 1 calc R . . C14 C 0.5027(2) 0.3154(2) 0.77935(17) 0.0383(6) Uani 1 1 d . . . H14A H 0.5498 0.2349 0.7664 0.057 Uiso 1 1 calc R . . H14B H 0.4927 0.3572 0.7265 0.057 Uiso 1 1 calc R . . H14C H 0.4101 0.3273 0.8176 0.057 Uiso 1 1 calc R . . C15 C 0.5058(2) 0.51995(18) 0.85281(14) 0.0261(5) Uani 1 1 d . . . H15A H 0.5544 0.5533 0.8810 0.039 Uiso 1 1 calc R . . H15B H 0.4131 0.5281 0.8895 0.039 Uiso 1 1 calc R . . H15C H 0.4962 0.5586 0.7988 0.039 Uiso 1 1 calc R . . C16 C 1.16306(18) 0.02500(16) 0.75333(12) 0.0156(4) Uani 1 1 d . . . C17 C 1.18296(19) -0.08026(17) 0.71897(12) 0.0183(4) Uani 1 1 d . . . C18 C 1.2181(2) -0.17768(17) 0.76744(13) 0.0226(5) Uani 1 1 d . . . H18 H 1.2313 -0.2479 0.7439 0.027 Uiso 1 1 calc R . . C19 C 1.2343(2) -0.17509(18) 0.84861(13) 0.0252(5) Uani 1 1 d . . . H19 H 1.2559 -0.2421 0.8812 0.030 Uiso 1 1 calc R . . C20 C 1.2184(2) -0.07327(18) 0.88144(13) 0.0227(5) Uani 1 1 d . . . H20 H 1.2306 -0.0712 0.9370 0.027 Uiso 1 1 calc R . . C21 C 1.18497(19) 0.02673(17) 0.83551(12) 0.0178(4) Uani 1 1 d . . . C22 C 1.1712(2) 0.13465(17) 0.87692(12) 0.0196(4) Uani 1 1 d . . . H22 H 1.1551 0.1967 0.8343 0.023 Uiso 1 1 calc R . . C23 C 1.0457(2) 0.16628(19) 0.95407(13) 0.0264(5) Uani 1 1 d . . . H23A H 1.0378 0.2365 0.9791 0.040 Uiso 1 1 calc R . . H23B H 1.0584 0.1060 0.9964 0.040 Uiso 1 1 calc R . . H23C H 0.9604 0.1766 0.9361 0.040 Uiso 1 1 calc R . . C24 C 1.3053(2) 0.1240(2) 0.90229(14) 0.0277(5) Uani 1 1 d . . . H24A H 1.2939 0.1948 0.9280 0.042 Uiso 1 1 calc R . . H24B H 1.3836 0.1075 0.8516 0.042 Uiso 1 1 calc R . . H24C H 1.3240 0.0627 0.9435 0.042 Uiso 1 1 calc R . . C25 C 1.1668(2) -0.09103(17) 0.63058(13) 0.0212(4) Uani 1 1 d . . . H25 H 1.1225 -0.0136 0.6097 0.025 Uiso 1 1 calc R . . C26 C 1.3096(2) -0.14428(19) 0.56900(13) 0.0270(5) Uani 1 1 d . . . H26A H 1.2970 -0.1502 0.5123 0.040 Uiso 1 1 calc R . . H26B H 1.3561 -0.2196 0.5892 0.040 Uiso 1 1 calc R . . H26C H 1.3670 -0.0971 0.5662 0.040 Uiso 1 1 calc R . . C27 C 1.0739(2) -0.16024(19) 0.62974(15) 0.0290(5) Uani 1 1 d . . . H27A H 1.0655 -0.1639 0.5716 0.044 Uiso 1 1 calc R . . H27B H 0.9812 -0.1245 0.6671 0.044 Uiso 1 1 calc R . . H27C H 1.1156 -0.2366 0.6500 0.044 Uiso 1 1 calc R . . C28 C 1.2220(2) 0.14880(19) 0.51790(13) 0.0273(5) Uani 1 1 d . . . H28A H 1.2473 0.0676 0.5100 0.041 Uiso 1 1 calc R . . H28B H 1.2887 0.1765 0.4763 0.041 Uiso 1 1 calc R . . H28C H 1.1279 0.1876 0.5098 0.041 Uiso 1 1 calc R . . C29 C 1.4105(2) 0.11327(19) 0.63643(14) 0.0252(5) Uani 1 1 d . . . H29A H 1.4396 0.0310 0.6330 0.038 Uiso 1 1 calc R . . H29B H 1.4181 0.1346 0.6909 0.038 Uiso 1 1 calc R . . H29C H 1.4707 0.1407 0.5897 0.038 Uiso 1 1 calc R . . C30 C 1.1758(2) 0.33259(17) 0.63517(14) 0.0263(5) Uani 1 1 d . . . H30A H 1.0791 0.3682 0.6309 0.039 Uiso 1 1 calc R . . H30B H 1.2376 0.3587 0.5885 0.039 Uiso 1 1 calc R . . H30C H 1.1844 0.3529 0.6897 0.039 Uiso 1 1 calc R . . C31 C 0.77700(19) 0.07916(17) 0.70365(12) 0.0184(4) Uani 1 1 d . . . H31 H 0.7792 0.1240 0.6537 0.022 Uiso 1 1 calc R . . C32 C 0.71069(19) 0.00184(16) 0.71210(12) 0.0180(4) Uani 1 1 d . . . H32 H 0.6701 -0.0063 0.6684 0.022 Uiso 1 1 calc R . . C33 C 0.70258(19) -0.06572(16) 0.78555(12) 0.0174(4) Uani 1 1 d . . . C34 C 0.7717(2) -0.05019(17) 0.84461(12) 0.0199(4) Uani 1 1 d . . . H34 H 0.7724 -0.0941 0.8950 0.024 Uiso 1 1 calc R . . C35 C 0.8377(2) 0.02817(17) 0.82938(12) 0.0191(4) Uani 1 1 d . . . H35 H 0.8854 0.0348 0.8697 0.023 Uiso 1 1 calc R . . C36 C 0.5676(2) -0.16051(18) 0.73667(13) 0.0240(5) Uani 1 1 d . . . H36A H 0.4735 -0.1048 0.7444 0.036 Uiso 1 1 calc R . . H36B H 0.5618 -0.2364 0.7445 0.036 Uiso 1 1 calc R . . H36C H 0.6231 -0.1538 0.6792 0.036 Uiso 1 1 calc R . . C37 C 0.6117(2) -0.1963(2) 0.88066(14) 0.0305(5) Uani 1 1 d . . . H37A H 0.5607 -0.2473 0.8791 0.046 Uiso 1 1 calc R . . H37B H 0.5574 -0.1397 0.9254 0.046 Uiso 1 1 calc R . . H37C H 0.7021 -0.2395 0.8925 0.046 Uiso 1 1 calc R . . N1 N 0.77764(16) 0.34910(13) 0.77341(9) 0.0142(3) Uani 1 1 d . . . N2 N 1.11697(16) 0.12859(13) 0.70918(10) 0.0143(3) Uani 1 1 d . . . N3 N 0.83948(16) 0.09611(13) 0.76127(10) 0.0165(4) Uani 1 1 d . . . N4 N 0.63375(17) -0.14040(14) 0.79892(10) 0.0209(4) Uani 1 1 d . . . Si1 Si 0.60876(6) 0.36673(5) 0.83206(3) 0.01956(13) Uani 1 1 d . . . Si2 Si 1.22606(5) 0.17689(5) 0.62844(3) 0.01619(13) Uani 1 1 d . . . Ni1 Ni 0.92785(2) 0.21704(2) 0.739895(15) 0.01383(8) 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 0.0106(9) 0.0136(10) 0.0162(10) -0.0009(8) 0.0011(7) -0.0010(8) C2 0.0156(9) 0.0149(10) 0.0162(10) -0.0004(8) -0.0009(8) -0.0035(8) C3 0.0229(11) 0.0191(11) 0.0199(11) 0.0032(9) -0.0023(8) -0.0047(9) C4 0.0247(11) 0.0177(11) 0.0309(12) 0.0036(9) -0.0008(9) -0.0113(9) C5 0.0201(10) 0.0219(11) 0.0289(12) -0.0061(9) -0.0038(9) -0.0111(9) C6 0.0152(10) 0.0164(10) 0.0191(10) -0.0039(8) -0.0015(8) -0.0033(8) C7 0.0243(11) 0.0208(11) 0.0243(11) -0.0039(9) -0.0099(9) -0.0065(9) C8 0.0351(13) 0.0476(16) 0.0201(12) 0.0012(11) -0.0102(10) -0.0086(12) C9 0.0307(13) 0.0474(16) 0.0351(13) -0.0051(11) -0.0160(11) -0.0144(12) C10 0.0252(11) 0.0215(11) 0.0190(10) 0.0044(8) -0.0094(9) -0.0083(9) C11 0.0393(14) 0.0366(14) 0.0357(14) -0.0135(11) -0.0125(11) -0.0062(12) C12 0.0296(12) 0.0410(15) 0.0301(13) -0.0017(11) -0.0155(10) -0.0061(11) C13 0.0375(14) 0.0291(13) 0.0298(13) 0.0080(10) 0.0117(11) -0.0034(11) C14 0.0201(11) 0.0396(15) 0.0539(16) -0.0153(12) 0.0030(11) -0.0136(11) C15 0.0224(11) 0.0228(12) 0.0277(12) -0.0006(9) -0.0008(9) -0.0050(9) C16 0.0098(9) 0.0181(10) 0.0167(10) 0.0018(8) 0.0007(7) -0.0054(8) C17 0.0107(9) 0.0198(11) 0.0230(11) -0.0003(8) -0.0004(8) -0.0063(8) C18 0.0194(10) 0.0156(11) 0.0309(12) 0.0013(9) -0.0019(9) -0.0069(9) C19 0.0230(11) 0.0203(12) 0.0271(12) 0.0093(9) -0.0025(9) -0.0062(9) C20 0.0200(10) 0.0272(12) 0.0177(10) 0.0057(9) -0.0027(8) -0.0067(9) C21 0.0134(9) 0.0197(11) 0.0186(10) 0.0026(8) -0.0016(8) -0.0055(8) C22 0.0222(10) 0.0218(11) 0.0143(10) 0.0027(8) -0.0051(8) -0.0071(9) C23 0.0281(12) 0.0286(12) 0.0197(11) -0.0017(9) -0.0056(9) -0.0060(10) C24 0.0292(12) 0.0357(13) 0.0221(11) -0.0001(10) -0.0080(9) -0.0146(10) C25 0.0188(10) 0.0177(11) 0.0268(11) -0.0038(9) -0.0052(9) -0.0054(9) C26 0.0261(11) 0.0285(12) 0.0249(11) -0.0048(9) -0.0015(9) -0.0099(10) C27 0.0232(11) 0.0250(12) 0.0394(13) -0.0104(10) -0.0048(10) -0.0084(10) C28 0.0322(12) 0.0288(12) 0.0175(11) 0.0030(9) -0.0058(9) -0.0073(10) C29 0.0168(10) 0.0304(12) 0.0266(11) 0.0059(9) -0.0036(9) -0.0082(9) C30 0.0256(11) 0.0231(12) 0.0255(11) 0.0036(9) 0.0019(9) -0.0094(9) C31 0.0141(9) 0.0192(11) 0.0200(10) 0.0046(8) -0.0042(8) -0.0045(8) C32 0.0160(10) 0.0184(11) 0.0201(10) 0.0013(8) -0.0058(8) -0.0058(8) C33 0.0128(9) 0.0151(10) 0.0210(10) -0.0018(8) 0.0002(8) -0.0036(8) C34 0.0205(10) 0.0202(11) 0.0179(10) 0.0042(8) -0.0030(8) -0.0077(9) C35 0.0183(10) 0.0203(11) 0.0188(10) 0.0004(8) -0.0048(8) -0.0066(8) C36 0.0233(11) 0.0231(12) 0.0287(12) -0.0014(9) -0.0053(9) -0.0119(9) C37 0.0392(13) 0.0311(13) 0.0275(12) 0.0070(10) -0.0062(10) -0.0229(11) N1 0.0155(8) 0.0142(8) 0.0132(8) 0.0020(6) -0.0038(6) -0.0056(7) N2 0.0152(8) 0.0135(8) 0.0144(8) 0.0018(6) -0.0037(6) -0.0053(7) N3 0.0136(8) 0.0167(9) 0.0186(9) 0.0012(7) -0.0036(7) -0.0048(7) N4 0.0245(9) 0.0211(9) 0.0208(9) 0.0029(7) -0.0037(7) -0.0142(8) Si1 0.0169(3) 0.0172(3) 0.0203(3) -0.0006(2) 0.0024(2) -0.0055(2) Si2 0.0143(3) 0.0181(3) 0.0145(3) 0.0024(2) -0.0018(2) -0.0053(2) Ni1 0.01225(13) 0.01356(14) 0.01519(13) 0.00113(10) -0.00258(9) -0.00462(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 C1 C2 1.414(3) . ? C1 C6 1.421(3) . ? C1 N1 1.434(2) . ? C2 C3 1.393(3) . ? C2 C10 1.517(3) . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.525(3) . ? C7 C8 1.527(3) . ? C7 C9 1.530(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.525(3) . ? C10 C12 1.535(3) . ? 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 Si1 1.866(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.878(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.874(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.418(3) . ? C16 C21 1.420(3) . ? C16 N2 1.430(2) . ? C17 C18 1.395(3) . ? C17 C25 1.516(3) . ? C18 C19 1.381(3) . ? C18 H18 0.9500 . ? C19 C20 1.379(3) . ? C19 H19 0.9500 . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C22 1.522(3) . ? C22 C23 1.530(3) . ? C22 C24 1.535(3) . ? 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 1.530(3) . ? C25 C26 1.533(3) . ? 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 Si2 1.880(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si2 1.863(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Si2 1.860(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N3 1.349(2) . ? C31 C32 1.369(3) . ? C31 H31 0.9500 . ? C32 C33 1.410(3) . ? C32 H32 0.9500 . ? C33 N4 1.354(2) . ? C33 C34 1.413(3) . ? C34 C35 1.372(3) . ? C34 H34 0.9500 . ? C35 N3 1.343(2) . ? C35 H35 0.9500 . ? C36 N4 1.456(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N4 1.454(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N1 Si1 1.7347(16) . ? N1 Ni1 1.8614(15) . ? N2 Si2 1.7289(16) . ? N2 Ni1 1.8717(15) . ? N3 Ni1 2.0187(16) . ? 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 C2 C1 C6 118.92(17) . . ? C2 C1 N1 120.18(17) . . ? C6 C1 N1 120.88(16) . . ? C3 C2 C1 119.53(18) . . ? C3 C2 C10 118.94(17) . . ? C1 C2 C10 121.51(17) . . ? C4 C3 C2 121.25(19) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.65(19) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.65(19) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.96(18) . . ? C5 C6 C7 120.24(18) . . ? C1 C6 C7 120.76(17) . . ? C6 C7 C8 112.76(17) . . ? C6 C7 C9 113.63(18) . . ? C8 C7 C9 108.91(18) . . ? C6 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? C9 C7 H7 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 111.42(17) . . ? C2 C10 C12 112.07(17) . . ? C11 C10 C12 110.06(18) . . ? C2 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? 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 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 118.33(17) . . ? C17 C16 N2 122.02(17) . . ? C21 C16 N2 119.60(17) . . ? C18 C17 C16 119.57(18) . . ? C18 C17 C25 118.29(18) . . ? C16 C17 C25 122.14(17) . . ? C19 C18 C17 121.91(19) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C20 C19 C18 118.68(19) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 121.95(19) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 119.49(18) . . ? C20 C21 C22 118.01(18) . . ? C16 C21 C22 122.49(17) . . ? C21 C22 C23 110.84(17) . . ? C21 C22 C24 111.25(17) . . ? C23 C22 C24 110.63(16) . . ? C21 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? 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 . . ? C17 C25 C27 112.47(17) . . ? C17 C25 C26 110.75(16) . . ? C27 C25 C26 109.24(17) . . ? C17 C25 H25 108.1 . . ? C27 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? 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 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 124.58(18) . . ? N3 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C31 C32 C33 120.04(18) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? N4 C33 C32 122.66(18) . . ? N4 C33 C34 122.09(18) . . ? C32 C33 C34 115.25(17) . . ? C35 C34 C33 120.18(18) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? N3 C35 C34 124.33(18) . . ? N3 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C1 N1 Si1 119.08(12) . . ? C1 N1 Ni1 111.26(11) . . ? Si1 N1 Ni1 129.56(9) . . ? C16 N2 Si2 123.71(12) . . ? C16 N2 Ni1 118.41(11) . . ? Si2 N2 Ni1 117.89(8) . . ? C35 N3 C31 115.51(16) . . ? C35 N3 Ni1 125.24(13) . . ? C31 N3 Ni1 119.24(13) . . ? C33 N4 C37 120.37(17) . . ? C33 N4 C36 122.39(17) . . ? C37 N4 C36 116.98(16) . . ? N1 Si1 C13 110.85(9) . . ? N1 Si1 C15 110.52(9) . . ? C13 Si1 C15 109.72(10) . . ? N1 Si1 C14 115.41(9) . . ? C13 Si1 C14 105.64(12) . . ? C15 Si1 C14 104.35(11) . . ? N2 Si2 C30 110.48(9) . . ? N2 Si2 C29 110.73(9) . . ? C30 Si2 C29 107.84(10) . . ? N2 Si2 C28 114.83(9) . . ? C30 Si2 C28 105.09(10) . . ? C29 Si2 C28 107.51(10) . . ? N1 Ni1 N2 155.07(7) . . ? N1 Ni1 N3 103.71(6) . . ? N2 Ni1 N3 100.47(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.314 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.052 data_shelxl_c _database_code_depnum_ccdc_archive 'CCDC 879066' #TrackingRef '- X-ray Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(N(SiMe3)(DIPP))2(MeCN) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H55 N3 Ni Si2' _chemical_formula_weight 596.68 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6047(3) _cell_length_b 11.1888(4) _cell_length_c 17.6838(5) _cell_angle_alpha 97.4630(10) _cell_angle_beta 97.333(2) _cell_angle_gamma 110.211(2) _cell_volume 1737.61(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9823 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9031 _exptl_absorpt_correction_T_max 0.9620 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR Multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 29585 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.36 _reflns_number_total 6356 _reflns_number_gt 5660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0287P)^2^+0.9904P] 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 6356 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.36191(19) 0.38503(15) 0.15145(9) 0.0167(3) Uani 1 1 d . . . C2 C 0.2518(2) 0.42003(16) 0.10882(9) 0.0203(4) Uani 1 1 d . . . C3 C 0.2794(2) 0.55144(17) 0.11035(10) 0.0248(4) Uani 1 1 d . . . H3 H 0.2058 0.5758 0.0820 0.030 Uiso 1 1 calc R . . C4 C 0.4110(2) 0.64671(17) 0.15199(10) 0.0251(4) Uani 1 1 d . . . H4 H 0.4270 0.7356 0.1529 0.030 Uiso 1 1 calc R . . C5 C 0.5189(2) 0.61173(17) 0.19218(10) 0.0239(4) Uani 1 1 d . . . H5 H 0.6098 0.6775 0.2204 0.029 Uiso 1 1 calc R . . C6 C 0.49816(19) 0.48260(16) 0.19240(9) 0.0192(4) Uani 1 1 d . . . C7 C 0.62029(19) 0.44886(17) 0.23808(10) 0.0225(4) Uani 1 1 d . . . H7 H 0.5990 0.3548 0.2197 0.027 Uiso 1 1 calc R . . C8 C 0.6145(2) 0.4680(2) 0.32429(10) 0.0344(5) Uani 1 1 d . . . H8A H 0.6330 0.5592 0.3438 0.052 Uiso 1 1 calc R . . H8B H 0.6921 0.4434 0.3524 0.052 Uiso 1 1 calc R . . H8C H 0.5148 0.4136 0.3321 0.052 Uiso 1 1 calc R . . C9 C 0.7791(2) 0.5254(2) 0.22522(13) 0.0400(5) Uani 1 1 d . . . H9A H 0.7799 0.5167 0.1694 0.060 Uiso 1 1 calc R . . H9B H 0.8510 0.4913 0.2499 0.060 Uiso 1 1 calc R . . H9C H 0.8080 0.6171 0.2482 0.060 Uiso 1 1 calc R . . C10 C 0.1058(2) 0.31904(17) 0.06161(10) 0.0261(4) Uani 1 1 d . . . H10 H 0.1104 0.2318 0.0645 0.031 Uiso 1 1 calc R . . C11 C -0.0309(2) 0.3253(2) 0.09468(13) 0.0437(5) Uani 1 1 d . . . H11A H -0.0266 0.3015 0.1461 0.066 Uiso 1 1 calc R . . H11B H -0.1235 0.2648 0.0601 0.066 Uiso 1 1 calc R . . H11C H -0.0307 0.4136 0.0991 0.066 Uiso 1 1 calc R . . C12 C 0.0888(3) 0.3317(2) -0.02422(11) 0.0457(6) Uani 1 1 d . . . H12A H 0.0826 0.4161 -0.0290 0.069 Uiso 1 1 calc R . . H12B H -0.0035 0.2624 -0.0537 0.069 Uiso 1 1 calc R . . H12C H 0.1763 0.3245 -0.0447 0.069 Uiso 1 1 calc R . . C13 C 0.5242(2) 0.0907(2) 0.13284(12) 0.0343(5) Uani 1 1 d . . . H13A H 0.6177 0.1612 0.1599 0.052 Uiso 1 1 calc R . . H13B H 0.5472 0.0350 0.0928 0.052 Uiso 1 1 calc R . . H13C H 0.4775 0.0395 0.1701 0.052 Uiso 1 1 calc R . . C14 C 0.2251(2) 0.0227(2) 0.02743(12) 0.0406(5) Uani 1 1 d . . . H14A H 0.1645 -0.0254 0.0619 0.061 Uiso 1 1 calc R . . H14B H 0.2601 -0.0352 -0.0048 0.061 Uiso 1 1 calc R . . H14C H 0.1634 0.0561 -0.0060 0.061 Uiso 1 1 calc R . . C15 C 0.4921(3) 0.2647(2) 0.02150(12) 0.0435(6) Uani 1 1 d . . . H15A H 0.4236 0.2987 -0.0065 0.065 Uiso 1 1 calc R . . H15B H 0.5262 0.2132 -0.0158 0.065 Uiso 1 1 calc R . . H15C H 0.5796 0.3371 0.0526 0.065 Uiso 1 1 calc R . . C16 C 0.12664(18) 0.10478(15) 0.36514(9) 0.0158(3) Uani 1 1 d . . . C17 C 0.23474(19) 0.09025(16) 0.42196(9) 0.0181(3) Uani 1 1 d . . . C18 C 0.1949(2) -0.02197(17) 0.45409(10) 0.0226(4) Uani 1 1 d . . . H18 H 0.2670 -0.0323 0.4921 0.027 Uiso 1 1 calc R . . C19 C 0.0532(2) -0.11804(17) 0.43184(10) 0.0245(4) Uani 1 1 d . . . H19 H 0.0281 -0.1934 0.4545 0.029 Uiso 1 1 calc R . . C20 C -0.0515(2) -0.10362(16) 0.37628(10) 0.0218(4) Uani 1 1 d . . . H20 H -0.1488 -0.1702 0.3609 0.026 Uiso 1 1 calc R . . C21 C -0.01823(19) 0.00640(16) 0.34203(9) 0.0182(3) Uani 1 1 d . . . C22 C -0.13747(19) 0.01522(16) 0.27981(9) 0.0216(4) Uani 1 1 d . . . H22 H -0.1070 0.1081 0.2742 0.026 Uiso 1 1 calc R . . C23 C -0.2931(2) -0.02486(18) 0.30309(10) 0.0267(4) Uani 1 1 d . . . H23A H -0.3308 -0.1179 0.3040 0.040 Uiso 1 1 calc R . . H23B H -0.3632 -0.0062 0.2654 0.040 Uiso 1 1 calc R . . H23C H -0.2848 0.0239 0.3547 0.040 Uiso 1 1 calc R . . C24 C -0.1466(2) -0.06406(19) 0.20030(10) 0.0304(4) Uani 1 1 d . . . H24A H -0.0529 -0.0254 0.1811 0.046 Uiso 1 1 calc R . . H24B H -0.2321 -0.0639 0.1636 0.046 Uiso 1 1 calc R . . H24C H -0.1607 -0.1534 0.2055 0.046 Uiso 1 1 calc R . . C25 C 0.39447(19) 0.18968(17) 0.44613(10) 0.0220(4) Uani 1 1 d . . . H25 H 0.3944 0.2717 0.4295 0.026 Uiso 1 1 calc R . . C26 C 0.5043(2) 0.1459(2) 0.40472(12) 0.0323(4) Uani 1 1 d . . . H26A H 0.4997 0.0613 0.4160 0.048 Uiso 1 1 calc R . . H26B H 0.6071 0.2095 0.4231 0.048 Uiso 1 1 calc R . . H26C H 0.4762 0.1389 0.3486 0.048 Uiso 1 1 calc R . . C27 C 0.4507(2) 0.22075(19) 0.53435(10) 0.0304(4) Uani 1 1 d . . . H27A H 0.3770 0.2437 0.5605 0.046 Uiso 1 1 calc R . . H27B H 0.5479 0.2937 0.5472 0.046 Uiso 1 1 calc R . . H27C H 0.4632 0.1447 0.5516 0.046 Uiso 1 1 calc R . . C28 C -0.0637(2) 0.31970(18) 0.37756(11) 0.0282(4) Uani 1 1 d . . . H28A H -0.1257 0.2964 0.3255 0.042 Uiso 1 1 calc R . . H28B H -0.0720 0.3975 0.4059 0.042 Uiso 1 1 calc R . . H28C H -0.0992 0.2480 0.4055 0.042 Uiso 1 1 calc R . . C29 C 0.2439(2) 0.42222(18) 0.47117(10) 0.0273(4) Uani 1 1 d . . . H29A H 0.2199 0.3547 0.5028 0.041 Uiso 1 1 calc R . . H29B H 0.2147 0.4933 0.4929 0.041 Uiso 1 1 calc R . . H29C H 0.3526 0.4552 0.4711 0.041 Uiso 1 1 calc R . . C30 C 0.1980(2) 0.48158(16) 0.31036(10) 0.0247(4) Uani 1 1 d . . . H30A H 0.3051 0.5036 0.3081 0.037 Uiso 1 1 calc R . . H30B H 0.1822 0.5588 0.3343 0.037 Uiso 1 1 calc R . . H30C H 0.1380 0.4502 0.2577 0.037 Uiso 1 1 calc R . . C31 C 0.2196(2) -0.08019(18) 0.24137(11) 0.0307(4) Uani 1 1 d . . . C32 C 0.1957(3) -0.2087(2) 0.25953(14) 0.0514(7) Uani 1 1 d . . . H32A H 0.1423 -0.2201 0.3033 0.077 Uiso 1 1 calc R . . H32B H 0.2936 -0.2172 0.2734 0.077 Uiso 1 1 calc R . . H32C H 0.1354 -0.2751 0.2141 0.077 Uiso 1 1 calc R . . N1 N 0.33517(15) 0.25196(12) 0.15457(7) 0.0161(3) Uani 1 1 d . . . N2 N 0.16733(15) 0.21572(12) 0.32796(7) 0.0159(3) Uani 1 1 d . . . N3 N 0.23678(18) 0.01992(14) 0.22871(8) 0.0257(3) Uani 1 1 d . . . Si1 Si 0.39100(6) 0.16049(4) 0.08659(3) 0.02062(11) Uani 1 1 d . . . Si2 Si 0.13802(5) 0.35249(4) 0.36946(2) 0.01547(10) Uani 1 1 d . . . Ni1 Ni 0.24709(2) 0.205616(19) 0.238105(11) 0.01537(7) 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 0.0252(9) 0.0168(8) 0.0128(7) 0.0058(6) 0.0115(7) 0.0097(7) C2 0.0293(10) 0.0198(9) 0.0159(8) 0.0059(7) 0.0089(7) 0.0113(8) C3 0.0371(11) 0.0247(10) 0.0212(8) 0.0101(7) 0.0098(8) 0.0183(9) C4 0.0404(11) 0.0150(9) 0.0261(9) 0.0083(7) 0.0172(8) 0.0124(8) C5 0.0269(10) 0.0174(9) 0.0256(9) 0.0031(7) 0.0121(8) 0.0039(8) C6 0.0246(9) 0.0189(9) 0.0167(8) 0.0046(7) 0.0107(7) 0.0085(8) C7 0.0219(9) 0.0185(9) 0.0251(9) 0.0009(7) 0.0052(7) 0.0060(8) C8 0.0342(11) 0.0493(13) 0.0250(9) 0.0076(9) 0.0041(8) 0.0221(10) C9 0.0269(11) 0.0440(13) 0.0542(13) 0.0162(10) 0.0161(10) 0.0140(10) C10 0.0328(11) 0.0232(10) 0.0234(9) 0.0026(7) -0.0016(8) 0.0146(8) C11 0.0304(12) 0.0382(13) 0.0543(13) -0.0068(10) 0.0018(10) 0.0101(10) C12 0.0623(15) 0.0453(13) 0.0257(10) 0.0052(9) -0.0089(10) 0.0217(12) C13 0.0397(12) 0.0372(12) 0.0388(11) 0.0092(9) 0.0184(9) 0.0251(10) C14 0.0436(13) 0.0356(12) 0.0364(11) -0.0123(9) 0.0055(10) 0.0143(10) C15 0.0737(16) 0.0376(12) 0.0371(11) 0.0166(9) 0.0399(11) 0.0286(12) C16 0.0223(9) 0.0151(8) 0.0165(7) 0.0059(6) 0.0122(7) 0.0107(7) C17 0.0223(9) 0.0184(9) 0.0202(8) 0.0070(7) 0.0121(7) 0.0114(7) C18 0.0266(10) 0.0250(9) 0.0243(8) 0.0118(7) 0.0105(7) 0.0146(8) C19 0.0327(10) 0.0197(9) 0.0283(9) 0.0139(7) 0.0155(8) 0.0117(8) C20 0.0239(9) 0.0172(9) 0.0248(9) 0.0050(7) 0.0122(7) 0.0050(8) C21 0.0232(9) 0.0182(9) 0.0170(8) 0.0038(6) 0.0108(7) 0.0095(7) C22 0.0233(9) 0.0176(9) 0.0213(8) 0.0035(7) 0.0052(7) 0.0042(7) C23 0.0243(10) 0.0288(10) 0.0260(9) 0.0043(8) 0.0048(8) 0.0089(8) C24 0.0319(11) 0.0339(11) 0.0213(9) 0.0024(8) 0.0075(8) 0.0071(9) C25 0.0203(9) 0.0241(9) 0.0275(9) 0.0122(7) 0.0074(7) 0.0118(8) C26 0.0227(10) 0.0375(11) 0.0453(11) 0.0160(9) 0.0133(9) 0.0161(9) C27 0.0289(10) 0.0305(10) 0.0322(10) 0.0129(8) 0.0029(8) 0.0096(9) C28 0.0249(10) 0.0244(10) 0.0387(10) 0.0019(8) 0.0112(8) 0.0126(8) C29 0.0365(11) 0.0266(10) 0.0221(9) 0.0017(7) 0.0039(8) 0.0173(9) C30 0.0359(11) 0.0196(9) 0.0258(9) 0.0086(7) 0.0132(8) 0.0147(8) C31 0.0445(12) 0.0237(10) 0.0367(10) 0.0112(8) 0.0298(9) 0.0185(9) C32 0.0843(18) 0.0264(11) 0.0717(16) 0.0293(11) 0.0551(14) 0.0339(12) N1 0.0212(7) 0.0145(7) 0.0159(6) 0.0058(5) 0.0074(6) 0.0080(6) N2 0.0192(7) 0.0152(7) 0.0171(6) 0.0064(5) 0.0084(6) 0.0081(6) N3 0.0372(9) 0.0202(8) 0.0290(8) 0.0088(6) 0.0214(7) 0.0152(7) Si1 0.0296(3) 0.0187(2) 0.0178(2) 0.00433(18) 0.0120(2) 0.0110(2) Si2 0.0186(2) 0.0152(2) 0.0160(2) 0.00476(17) 0.00694(18) 0.00854(19) Ni1 0.02140(12) 0.01331(11) 0.01578(11) 0.00603(8) 0.01009(8) 0.00830(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.412(2) . ? C1 C2 1.414(2) . ? C1 N1 1.431(2) . ? C2 C3 1.397(2) . ? C2 C10 1.517(2) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(2) . ? C5 H5 0.9500 . ? C6 C7 1.521(2) . ? C7 C8 1.522(2) . ? C7 C9 1.532(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.524(3) . ? C10 C12 1.536(2) . ? 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 Si1 1.8719(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.862(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.8653(19) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.412(2) . ? C16 C17 1.417(2) . ? C16 N2 1.4383(19) . ? C17 C18 1.398(2) . ? C17 C25 1.518(2) . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(2) . ? C19 H19 0.9500 . ? C20 C21 1.398(2) . ? C20 H20 0.9500 . ? C21 C22 1.522(2) . ? C22 C23 1.532(2) . ? C22 C24 1.537(2) . ? 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 C26 1.533(2) . ? C25 C27 1.536(2) . ? 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 Si2 1.8719(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si2 1.8705(17) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Si2 1.8657(17) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N3 1.131(2) . ? C31 C32 1.461(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 Si1 1.7332(13) . ? N1 Ni1 1.8390(13) . ? N2 Si2 1.7373(13) . ? N2 Ni1 1.8569(13) . ? N3 Ni1 2.0293(14) . ? 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 C6 C1 C2 119.62(14) . . ? C6 C1 N1 119.82(14) . . ? C2 C1 N1 120.55(15) . . ? C3 C2 C1 118.68(16) . . ? C3 C2 C10 119.51(15) . . ? C1 C2 C10 121.82(14) . . ? C4 C3 C2 121.58(16) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.37(16) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.62(17) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.09(15) . . ? C5 C6 C7 119.66(15) . . ? C1 C6 C7 121.23(14) . . ? C8 C7 C6 110.79(14) . . ? C8 C7 C9 110.21(16) . . ? C6 C7 C9 112.99(15) . . ? C8 C7 H7 107.5 . . ? C6 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 111.68(15) . . ? C2 C10 C12 111.27(16) . . ? C11 C10 C12 110.88(17) . . ? C2 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 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 119.73(14) . . ? C21 C16 N2 120.16(14) . . ? C17 C16 N2 120.01(14) . . ? C18 C17 C16 118.86(15) . . ? C18 C17 C25 119.09(15) . . ? C16 C17 C25 121.99(14) . . ? C19 C18 C17 121.55(16) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 119.38(15) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 121.69(16) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 118.79(15) . . ? C20 C21 C22 119.18(15) . . ? C16 C21 C22 122.01(14) . . ? C21 C22 C23 111.88(13) . . ? C21 C22 C24 112.25(14) . . ? C23 C22 C24 110.37(14) . . ? C21 C22 H22 107.4 . . ? C23 C22 H22 107.4 . . ? C24 C22 H22 107.4 . . ? 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 . . ? C17 C25 C26 110.98(15) . . ? C17 C25 C27 112.99(14) . . ? C26 C25 C27 110.00(14) . . ? C17 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? 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 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 178.5(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1 Si1 119.92(10) . . ? C1 N1 Ni1 110.78(10) . . ? Si1 N1 Ni1 129.27(8) . . ? C16 N2 Si2 118.01(10) . . ? C16 N2 Ni1 118.65(10) . . ? Si2 N2 Ni1 123.34(7) . . ? C31 N3 Ni1 162.21(14) . . ? N1 Si1 C14 110.89(8) . . ? N1 Si1 C15 109.79(8) . . ? C14 Si1 C15 109.48(11) . . ? N1 Si1 C13 112.20(8) . . ? C14 Si1 C13 107.43(10) . . ? C15 Si1 C13 106.94(10) . . ? N2 Si2 C30 109.76(7) . . ? N2 Si2 C29 113.64(7) . . ? C30 Si2 C29 107.65(8) . . ? N2 Si2 C28 113.01(8) . . ? C30 Si2 C28 108.38(8) . . ? C29 Si2 C28 104.06(9) . . ? N1 Ni1 N2 161.26(6) . . ? N1 Ni1 N3 100.48(6) . . ? N2 Ni1 N3 98.15(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.359 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.044 data_shelxl_d _database_code_depnum_ccdc_archive 'CCDC 879067' #TrackingRef '- X-ray Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni-isonitrile-insertion _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H70 N4 Ni Si2' _chemical_formula_weight 817.97 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.3178(4) _cell_length_b 20.8353(5) _cell_length_c 13.7272(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4667.06(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.33 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9284 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 39140 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8159 _reflns_number_gt 7633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP32 _computing_publication_material WinGX _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^)+(0.0350P)^2^+0.9027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(8) _refine_ls_number_reflns 8159 _refine_ls_number_parameters 514 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.64440(11) 0.53607(9) -0.43451(14) 0.0212(4) Uani 1 1 d . . . C2 C 0.56549(12) 0.55835(10) -0.40870(16) 0.0254(4) Uani 1 1 d . . . C3 C 0.52082(13) 0.59122(11) -0.47932(16) 0.0330(5) Uani 1 1 d . . . H3 H 0.4676 0.6067 -0.4640 0.040 Uiso 1 1 calc R . . C4 C 0.55258(14) 0.60161(11) -0.57131(17) 0.0353(5) Uani 1 1 d . . . H4 H 0.5212 0.6241 -0.6185 0.042 Uiso 1 1 calc R . . C5 C 0.62950(13) 0.57946(10) -0.59481(16) 0.0304(5) Uani 1 1 d . . . H5 H 0.6504 0.5872 -0.6583 0.036 Uiso 1 1 calc R . . C6 C 0.67743(12) 0.54607(9) -0.52835(15) 0.0237(4) Uani 1 1 d . . . C7 C 0.76393(13) 0.52327(11) -0.55278(15) 0.0273(5) Uani 1 1 d . . . H7 H 0.7720 0.4806 -0.5207 0.033 Uiso 1 1 calc R . . C8 C 0.77898(14) 0.51430(13) -0.66203(17) 0.0368(5) Uani 1 1 d . . . H8A H 0.7361 0.4867 -0.6894 0.055 Uiso 1 1 calc R . . H8B H 0.8326 0.4942 -0.6721 0.055 Uiso 1 1 calc R . . H8C H 0.7778 0.5562 -0.6945 0.055 Uiso 1 1 calc R . . C9 C 0.82786(13) 0.56933(12) -0.51073(16) 0.0345(5) Uani 1 1 d . . . H9A H 0.8228 0.6113 -0.5425 0.052 Uiso 1 1 calc R . . H9B H 0.8829 0.5520 -0.5222 0.052 Uiso 1 1 calc R . . H9C H 0.8189 0.5742 -0.4405 0.052 Uiso 1 1 calc R . . C10 C 0.53153(12) 0.54870(11) -0.30597(15) 0.0287(5) Uani 1 1 d . . . H10 H 0.5589 0.5100 -0.2775 0.034 Uiso 1 1 calc R . . C11 C 0.43869(13) 0.53711(11) -0.30310(17) 0.0349(5) Uani 1 1 d . . . H11A H 0.4226 0.5235 -0.2375 0.052 Uiso 1 1 calc R . . H11B H 0.4242 0.5035 -0.3500 0.052 Uiso 1 1 calc R . . H11C H 0.4100 0.5769 -0.3200 0.052 Uiso 1 1 calc R . . C12 C 0.55347(13) 0.60622(12) -0.24229(17) 0.0399(6) Uani 1 1 d . . . H12A H 0.6130 0.6123 -0.2423 0.060 Uiso 1 1 calc R . . H12B H 0.5346 0.5985 -0.1755 0.060 Uiso 1 1 calc R . . H12C H 0.5269 0.6448 -0.2681 0.060 Uiso 1 1 calc R . . C13 C 0.64760(16) 0.37791(12) -0.57654(16) 0.0376(5) Uani 1 1 d . . . H13A H 0.6431 0.4245 -0.5852 0.056 Uiso 1 1 calc R . . H13B H 0.6068 0.3564 -0.6174 0.056 Uiso 1 1 calc R . . H13C H 0.7026 0.3638 -0.5954 0.056 Uiso 1 1 calc R . . C14 C 0.63260(13) 0.26871(10) -0.43341(17) 0.0338(5) Uani 1 1 d . . . H14A H 0.6860 0.2527 -0.4552 0.051 Uiso 1 1 calc R . . H14B H 0.5892 0.2493 -0.4729 0.051 Uiso 1 1 calc R . . H14C H 0.6244 0.2574 -0.3648 0.051 Uiso 1 1 calc R . . C15 C 0.52793(13) 0.38872(12) -0.4081(2) 0.0421(6) Uani 1 1 d . . . H15A H 0.5212 0.3820 -0.3379 0.063 Uiso 1 1 calc R . . H15B H 0.4844 0.3660 -0.4431 0.063 Uiso 1 1 calc R . . H15C H 0.5247 0.4347 -0.4226 0.063 Uiso 1 1 calc R . . C16 C 0.76109(12) 0.34203(9) -0.32214(15) 0.0221(4) Uani 1 1 d . . . C17 C 0.73673(12) 0.31593(10) -0.23329(15) 0.0268(5) Uani 1 1 d . . . C18 C 0.78442(13) 0.26709(11) -0.19365(17) 0.0325(5) Uani 1 1 d . . . H18 H 0.7688 0.2483 -0.1334 0.039 Uiso 1 1 calc R . . C19 C 0.85401(13) 0.24561(11) -0.24056(16) 0.0334(5) Uani 1 1 d . . . H19 H 0.8848 0.2112 -0.2138 0.040 Uiso 1 1 calc R . . C20 C 0.87884(13) 0.27401(10) -0.32613(17) 0.0311(5) Uani 1 1 d . . . H20 H 0.9277 0.2597 -0.3569 0.037 Uiso 1 1 calc R . . C21 C 0.83371(12) 0.32338(9) -0.36842(15) 0.0248(4) Uani 1 1 d . . . C22 C 0.86396(12) 0.35784(10) -0.45768(16) 0.0294(5) Uani 1 1 d . . . H22A H 0.9175 0.3405 -0.4767 0.044 Uiso 1 1 calc R . . H22B H 0.8693 0.4037 -0.4435 0.044 Uiso 1 1 calc R . . H22C H 0.8248 0.3517 -0.5110 0.044 Uiso 1 1 calc R . . C23 C 0.66217(14) 0.34168(11) -0.18148(16) 0.0348(5) Uani 1 1 d . . . H23A H 0.6650 0.3886 -0.1790 0.052 Uiso 1 1 calc R . . H23B H 0.6604 0.3245 -0.1151 0.052 Uiso 1 1 calc R . . H23C H 0.6127 0.3286 -0.2167 0.052 Uiso 1 1 calc R . . C24 C 0.72308(11) 0.45082(9) -0.34289(13) 0.0177(4) Uani 1 1 d . . . C25 C 0.77283(11) 0.63089(10) -0.18014(14) 0.0232(4) Uani 1 1 d . . . C26 C 0.73707(12) 0.61545(11) -0.08851(15) 0.0258(4) Uani 1 1 d . . . C27 C 0.68218(13) 0.65779(11) -0.04507(16) 0.0311(5) Uani 1 1 d . . . H27 H 0.6590 0.6470 0.0163 0.037 Uiso 1 1 calc R . . C28 C 0.66057(14) 0.71479(11) -0.08854(17) 0.0356(5) Uani 1 1 d . . . H28 H 0.6219 0.7426 -0.0585 0.043 Uiso 1 1 calc R . . C29 C 0.69597(13) 0.73099(11) -0.17647(17) 0.0327(5) Uani 1 1 d . . . H29 H 0.6818 0.7706 -0.2062 0.039 Uiso 1 1 calc R . . C30 C 0.75220(13) 0.69059(10) -0.22308(15) 0.0265(5) Uani 1 1 d . . . C31 C 0.78432(14) 0.71121(11) -0.32225(16) 0.0308(5) Uani 1 1 d . . . H31 H 0.8309 0.6822 -0.3398 0.037 Uiso 1 1 calc R . . C32 C 0.81644(16) 0.78063(10) -0.32303(18) 0.0394(6) Uani 1 1 d . . . H32A H 0.7709 0.8103 -0.3109 0.059 Uiso 1 1 calc R . . H32B H 0.8409 0.7901 -0.3867 0.059 Uiso 1 1 calc R . . H32C H 0.8580 0.7858 -0.2720 0.059 Uiso 1 1 calc R . . C33 C 0.71742(16) 0.70279(12) -0.39891(19) 0.0429(6) Uani 1 1 d . . . H33A H 0.6980 0.6583 -0.3983 0.064 Uiso 1 1 calc R . . H33B H 0.7396 0.7130 -0.4634 0.064 Uiso 1 1 calc R . . H33C H 0.6716 0.7317 -0.3843 0.064 Uiso 1 1 calc R . . C34 C 0.75339(13) 0.55221(11) -0.03806(15) 0.0297(5) Uani 1 1 d . . . H34 H 0.8018 0.5319 -0.0704 0.036 Uiso 1 1 calc R . . C35 C 0.77388(16) 0.56006(14) 0.07028(16) 0.0463(6) Uani 1 1 d . . . H35A H 0.8212 0.5886 0.0774 0.069 Uiso 1 1 calc R . . H35B H 0.7869 0.5180 0.0984 0.069 Uiso 1 1 calc R . . H35C H 0.7267 0.5785 0.1044 0.069 Uiso 1 1 calc R . . C36 C 0.68024(15) 0.50694(11) -0.05109(19) 0.0368(5) Uani 1 1 d . . . H36A H 0.6313 0.5263 -0.0219 0.055 Uiso 1 1 calc R . . H36B H 0.6919 0.4659 -0.0190 0.055 Uiso 1 1 calc R . . H36C H 0.6707 0.4996 -0.1207 0.055 Uiso 1 1 calc R . . C37 C 0.97085(14) 0.56057(12) -0.09093(18) 0.0377(6) Uani 1 1 d . . . H37A H 0.9473 0.5837 -0.0354 0.057 Uiso 1 1 calc R . . H37B H 1.0307 0.5643 -0.0892 0.057 Uiso 1 1 calc R . . H37C H 0.9553 0.5152 -0.0874 0.057 Uiso 1 1 calc R . . C38 C 0.98847(12) 0.55915(11) -0.31220(17) 0.0321(5) Uani 1 1 d . . . H38A H 0.9698 0.5149 -0.3216 0.048 Uiso 1 1 calc R . . H38B H 1.0473 0.5593 -0.2976 0.048 Uiso 1 1 calc R . . H38C H 0.9784 0.5839 -0.3717 0.048 Uiso 1 1 calc R . . C39 C 0.96460(13) 0.68257(11) -0.19969(19) 0.0375(5) Uani 1 1 d . . . H39A H 0.9590 0.7031 -0.2636 0.056 Uiso 1 1 calc R . . H39B H 1.0220 0.6843 -0.1789 0.056 Uiso 1 1 calc R . . H39C H 0.9304 0.7052 -0.1521 0.056 Uiso 1 1 calc R . . C40 C 0.85467(11) 0.45153(9) -0.21024(14) 0.0232(4) Uani 1 1 d . . . C41 C 0.94918(13) 0.37059(10) -0.12688(16) 0.0286(5) Uani 1 1 d . . . C42 C 1.02008(13) 0.35095(11) -0.17632(18) 0.0332(5) Uani 1 1 d . . . C43 C 1.06643(14) 0.30377(11) -0.1313(2) 0.0402(6) Uani 1 1 d . . . H43 H 1.1146 0.2884 -0.1624 0.048 Uiso 1 1 calc R . . C44 C 1.04408(15) 0.27899(11) -0.0431(2) 0.0431(6) Uani 1 1 d . . . H44 H 1.0766 0.2461 -0.0148 0.052 Uiso 1 1 calc R . . C45 C 0.97554(15) 0.30050(12) 0.00588(18) 0.0410(6) Uani 1 1 d . . . H45 H 0.9622 0.2833 0.0680 0.049 Uiso 1 1 calc R . . C46 C 0.92564(13) 0.34776(10) -0.03602(17) 0.0328(5) Uani 1 1 d . . . C47 C 0.85059(15) 0.37324(12) 0.01411(18) 0.0396(5) Uani 1 1 d . . . H47A H 0.8548 0.4200 0.0203 0.059 Uiso 1 1 calc R . . H47B H 0.8461 0.3540 0.0790 0.059 Uiso 1 1 calc R . . H47C H 0.8019 0.3624 -0.0243 0.059 Uiso 1 1 calc R . . C48 C 1.04451(13) 0.37987(11) -0.2719(2) 0.0411(5) Uani 1 1 d . . . H48A H 0.9995 0.3751 -0.3187 0.062 Uiso 1 1 calc R . . H48B H 1.0934 0.3579 -0.2968 0.062 Uiso 1 1 calc R . . H48C H 1.0566 0.4256 -0.2629 0.062 Uiso 1 1 calc R . . N1 N 0.70829(9) 0.38937(8) -0.36981(12) 0.0196(3) Uani 1 1 d . . . N2 N 0.69352(10) 0.50611(8) -0.36244(12) 0.0198(4) Uani 1 1 d . . . N3 N 0.82766(9) 0.58819(8) -0.22752(11) 0.0215(3) Uani 1 1 d . . . N4 N 0.89833(10) 0.41536(8) -0.17225(13) 0.0274(4) Uani 1 1 d . . . Si1 Si 0.62917(3) 0.35734(3) -0.44713(4) 0.02508(13) Uani 1 1 d . . . Si2 Si 0.93086(3) 0.59637(3) -0.20811(4) 0.02651(13) Uani 1 1 d . . . Ni1 Ni 0.786211(13) 0.504650(10) -0.27054(2) 0.01841(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0234(9) 0.0184(10) 0.0219(10) -0.0021(8) -0.0039(8) 0.0000(8) C2 0.0250(10) 0.0241(11) 0.0271(11) -0.0024(9) -0.0010(8) 0.0020(8) C3 0.0277(10) 0.0369(13) 0.0345(12) 0.0020(11) -0.0032(9) 0.0061(10) C4 0.0358(12) 0.0349(13) 0.0352(13) 0.0117(10) -0.0088(10) 0.0043(10) C5 0.0344(12) 0.0334(12) 0.0233(11) 0.0059(9) -0.0025(9) -0.0032(10) C6 0.0274(10) 0.0215(10) 0.0223(10) -0.0010(9) -0.0017(8) -0.0033(8) C7 0.0290(11) 0.0340(12) 0.0188(11) 0.0011(9) 0.0025(8) -0.0033(9) C8 0.0352(13) 0.0498(15) 0.0254(12) 0.0003(11) 0.0031(9) -0.0022(11) C9 0.0272(11) 0.0446(14) 0.0316(12) -0.0013(11) 0.0046(9) -0.0094(10) C10 0.0218(10) 0.0385(13) 0.0256(10) -0.0016(9) -0.0002(8) 0.0059(9) C11 0.0294(11) 0.0436(14) 0.0316(12) -0.0063(10) 0.0016(9) -0.0022(10) C12 0.0274(11) 0.0553(16) 0.0372(14) -0.0123(11) 0.0015(9) -0.0035(10) C13 0.0468(13) 0.0381(13) 0.0278(12) -0.0015(10) -0.0136(10) -0.0055(11) C14 0.0391(12) 0.0250(12) 0.0372(13) -0.0046(10) -0.0124(10) -0.0051(9) C15 0.0268(11) 0.0397(14) 0.0599(16) -0.0096(12) -0.0086(11) -0.0011(10) C16 0.0247(10) 0.0182(10) 0.0234(10) -0.0019(9) -0.0077(8) -0.0013(8) C17 0.0278(10) 0.0266(11) 0.0260(10) 0.0005(9) -0.0048(9) -0.0059(9) C18 0.0424(13) 0.0302(12) 0.0250(11) 0.0094(10) -0.0112(10) -0.0088(10) C19 0.0345(11) 0.0223(11) 0.0435(14) 0.0063(9) -0.0156(10) 0.0002(9) C20 0.0258(11) 0.0228(12) 0.0448(14) -0.0040(10) -0.0048(10) 0.0010(9) C21 0.0251(10) 0.0202(10) 0.0290(11) -0.0031(9) -0.0049(9) -0.0024(8) C22 0.0274(10) 0.0288(11) 0.0320(12) -0.0026(10) 0.0045(9) 0.0010(9) C23 0.0415(13) 0.0368(13) 0.0262(12) 0.0035(10) 0.0047(10) -0.0043(10) C24 0.0161(9) 0.0207(11) 0.0163(9) 0.0008(8) 0.0038(7) -0.0009(8) C25 0.0215(9) 0.0236(10) 0.0245(11) -0.0075(9) -0.0005(8) -0.0040(8) C26 0.0236(10) 0.0331(12) 0.0206(10) -0.0063(9) -0.0004(8) -0.0041(9) C27 0.0299(11) 0.0372(13) 0.0263(11) -0.0083(10) 0.0038(9) -0.0044(9) C28 0.0316(12) 0.0362(13) 0.0391(13) -0.0125(11) 0.0061(10) 0.0027(10) C29 0.0345(12) 0.0253(12) 0.0382(13) -0.0055(10) -0.0009(10) 0.0028(9) C30 0.0296(11) 0.0254(11) 0.0245(11) -0.0030(9) -0.0013(9) -0.0016(9) C31 0.0433(13) 0.0210(12) 0.0282(12) -0.0012(10) 0.0012(10) -0.0002(9) C32 0.0584(15) 0.0266(12) 0.0332(13) -0.0016(10) 0.0088(11) -0.0053(11) C33 0.0675(17) 0.0278(13) 0.0334(13) 0.0000(11) -0.0092(12) -0.0003(11) C34 0.0332(11) 0.0373(13) 0.0185(11) -0.0028(10) 0.0017(9) 0.0000(10) C35 0.0573(15) 0.0596(18) 0.0221(13) -0.0005(12) -0.0043(11) 0.0055(13) C36 0.0394(13) 0.0370(14) 0.0342(13) 0.0009(11) 0.0092(11) -0.0050(10) C37 0.0299(12) 0.0456(14) 0.0376(13) -0.0060(11) -0.0114(10) -0.0082(10) C38 0.0238(10) 0.0353(13) 0.0372(12) -0.0006(10) 0.0040(9) -0.0023(9) C39 0.0339(12) 0.0353(13) 0.0433(13) -0.0083(11) 0.0011(11) -0.0102(10) C40 0.0226(9) 0.0261(11) 0.0207(10) -0.0029(9) -0.0001(8) -0.0049(9) C41 0.0286(11) 0.0218(11) 0.0354(12) -0.0022(9) -0.0140(9) -0.0009(9) C42 0.0246(10) 0.0264(12) 0.0484(14) -0.0070(10) -0.0114(10) -0.0024(9) C43 0.0275(11) 0.0307(13) 0.0624(17) -0.0033(12) -0.0094(11) 0.0014(10) C44 0.0390(14) 0.0328(13) 0.0575(17) -0.0021(13) -0.0235(12) 0.0081(11) C45 0.0502(15) 0.0361(14) 0.0367(14) 0.0030(11) -0.0181(11) -0.0048(11) C46 0.0346(12) 0.0270(12) 0.0368(13) -0.0039(10) -0.0131(10) -0.0025(9) C47 0.0479(14) 0.0396(13) 0.0314(12) 0.0023(11) -0.0018(11) -0.0005(11) C48 0.0303(11) 0.0354(12) 0.0576(15) -0.0012(14) 0.0042(13) -0.0004(9) N1 0.0197(8) 0.0184(9) 0.0205(8) -0.0005(7) -0.0016(6) 0.0003(6) N2 0.0204(8) 0.0228(9) 0.0163(8) -0.0013(7) -0.0025(7) -0.0007(7) N3 0.0225(8) 0.0225(9) 0.0196(8) -0.0045(7) 0.0001(7) -0.0026(7) N4 0.0233(9) 0.0264(10) 0.0325(10) -0.0012(8) -0.0075(8) -0.0026(8) Si1 0.0244(3) 0.0237(3) 0.0272(3) -0.0027(2) -0.0081(2) -0.0015(2) Si2 0.0221(3) 0.0294(3) 0.0280(3) -0.0055(3) 0.0003(2) -0.0049(2) Ni1 0.01915(11) 0.01965(12) 0.01643(11) -0.00139(11) -0.00136(11) -0.00065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.412(3) . ? C1 C2 1.414(3) . ? C1 N2 1.418(2) . ? C2 C3 1.393(3) . ? C2 C10 1.528(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C7 1.527(3) . ? C7 C8 1.531(3) . ? C7 C9 1.530(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.526(3) . ? C10 C11 1.535(3) . ? 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 Si1 1.852(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si1 1.857(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.856(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.393(3) . ? C16 C21 1.400(3) . ? C16 N1 1.464(2) . ? C17 C18 1.392(3) . ? C17 C23 1.508(3) . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.376(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 C22 1.503(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N2 1.278(2) . ? C24 N1 1.354(3) . ? C24 Ni1 1.8181(19) . ? C25 N3 1.420(2) . ? C25 C30 1.417(3) . ? C25 C26 1.423(3) . ? C26 C27 1.392(3) . ? C26 C34 1.512(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.380(3) . ? C28 H28 0.9500 . ? C29 C30 1.400(3) . ? C29 H29 0.9500 . ? C30 C31 1.521(3) . ? C31 C33 1.526(3) . ? C31 C32 1.539(3) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.533(3) . ? C34 C36 1.532(3) . ? C34 H34 1.0000 . ? 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 Si2 1.889(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Si2 1.878(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 Si2 1.882(2) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N4 1.161(3) . ? C40 Ni1 1.777(2) . ? C41 N4 1.395(3) . ? C41 C46 1.389(3) . ? C41 C42 1.402(3) . ? C42 C43 1.386(3) . ? C42 C48 1.498(4) . ? C43 C44 1.366(4) . ? C43 H43 0.9500 . ? C44 C45 1.380(4) . ? C44 H44 0.9500 . ? C45 C46 1.401(3) . ? C45 H45 0.9500 . ? C46 C47 1.502(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N1 Si1 1.7997(16) . ? N2 Ni1 1.9699(16) . ? N3 Si2 1.7134(16) . ? N3 Ni1 1.9585(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.87(18) . . ? C6 C1 N2 119.06(17) . . ? C2 C1 N2 118.97(18) . . ? C3 C2 C1 117.62(19) . . ? C3 C2 C10 121.14(18) . . ? C1 C2 C10 121.21(18) . . ? C4 C3 C2 121.1(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.9(2) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 117.28(18) . . ? C5 C6 C7 122.17(18) . . ? C1 C6 C7 120.50(18) . . ? C6 C7 C8 113.67(18) . . ? C6 C7 C9 110.63(18) . . ? C8 C7 C9 109.68(18) . . ? C6 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 109.89(18) . . ? C2 C10 C11 113.73(18) . . ? C12 C10 C11 109.89(17) . . ? C2 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? 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 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.04(19) . . ? C17 C16 N1 119.10(18) . . ? C21 C16 N1 118.84(18) . . ? C18 C17 C16 117.9(2) . . ? C18 C17 C23 121.79(19) . . ? C16 C17 C23 120.27(19) . . ? C19 C18 C17 121.0(2) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 121.2(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 117.6(2) . . ? C20 C21 C22 121.27(18) . . ? C16 C21 C22 121.02(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 N1 136.72(18) . . ? N2 C24 Ni1 76.85(11) . . ? N1 C24 Ni1 146.43(15) . . ? N3 C25 C30 120.61(18) . . ? N3 C25 C26 121.44(18) . . ? C30 C25 C26 117.95(18) . . ? C27 C26 C25 119.9(2) . . ? C27 C26 C34 118.00(19) . . ? C25 C26 C34 121.97(18) . . ? C28 C27 C26 121.8(2) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 118.9(2) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 121.8(2) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 119.56(19) . . ? C29 C30 C31 117.7(2) . . ? C25 C30 C31 122.58(19) . . ? C30 C31 C33 109.77(18) . . ? C30 C31 C32 112.90(18) . . ? C33 C31 C32 110.30(19) . . ? C30 C31 H31 107.9 . . ? C33 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C35 112.9(2) . . ? C26 C34 C36 110.23(18) . . ? C35 C34 C36 110.43(19) . . ? C26 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? C36 C34 H34 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 Ni1 178.02(18) . . ? N4 C41 C46 117.73(19) . . ? N4 C41 C42 118.0(2) . . ? C46 C41 C42 124.2(2) . . ? C43 C42 C41 116.2(2) . . ? C43 C42 C48 122.0(2) . . ? C41 C42 C48 121.7(2) . . ? C44 C43 C42 121.2(2) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 121.7(2) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C45 C46 119.9(2) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 116.7(2) . . ? C41 C46 C47 121.1(2) . . ? C45 C46 C47 122.3(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C24 N1 C16 114.21(15) . . ? C24 N1 Si1 129.74(13) . . ? C16 N1 Si1 115.85(12) . . ? C24 N2 C1 139.20(17) . . ? C24 N2 Ni1 63.99(11) . . ? C1 N2 Ni1 152.58(13) . . ? C25 N3 Si2 119.07(12) . . ? C25 N3 Ni1 118.52(12) . . ? Si2 N3 Ni1 118.34(9) . . ? C40 N4 C41 178.4(2) . . ? N1 Si1 C13 111.31(9) . . ? N1 Si1 C15 109.74(9) . . ? C13 Si1 C15 109.88(12) . . ? N1 Si1 C14 106.70(9) . . ? C13 Si1 C14 108.81(11) . . ? C15 Si1 C14 110.36(11) . . ? N3 Si2 C38 109.43(9) . . ? N3 Si2 C39 113.08(9) . . ? C38 Si2 C39 107.12(10) . . ? N3 Si2 C37 115.63(9) . . ? C38 Si2 C37 108.17(11) . . ? C39 Si2 C37 102.91(11) . . ? C40 Ni1 C24 103.09(8) . . ? C40 Ni1 N3 101.30(7) . . ? C24 Ni1 N3 155.32(8) . . ? C40 Ni1 N2 142.25(8) . . ? C24 Ni1 N2 39.16(7) . . ? N3 Ni1 N2 116.39(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.297 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.038 data_shelxl_e _database_code_depnum_ccdc_archive 'CCDC 879068' #TrackingRef '- X-ray Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common diazo-bis-DIPP _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 N2' _chemical_formula_weight 350.53 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2978(9) _cell_length_b 9.4465(5) _cell_length_c 13.7560(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.003(2) _cell_angle_gamma 90.00 _cell_volume 2085.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6143 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9904 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 13521 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.37 _reflns_number_total 1914 _reflns_number_gt 1482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP32 _computing_publication_material WinGX _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^)+(0.0412P)^2^+1.5696P] 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 1914 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.90486(8) 0.02887(14) 0.16366(10) 0.0147(3) Uani 1 1 d . . . C2 C 0.83367(9) -0.05911(14) 0.15348(10) 0.0166(3) Uani 1 1 d . . . C3 C 0.77470(9) -0.04721(15) 0.06807(10) 0.0203(3) Uani 1 1 d . . . H3 H 0.7278 -0.1085 0.0583 0.024 Uiso 1 1 calc R . . C4 C 0.78326(9) 0.05285(15) -0.00321(11) 0.0213(3) Uani 1 1 d . . . H4 H 0.7425 0.0594 -0.0615 0.026 Uiso 1 1 calc R . . C5 C 0.85109(9) 0.14306(15) 0.01059(10) 0.0190(3) Uani 1 1 d . . . H5 H 0.8550 0.2135 -0.0377 0.023 Uiso 1 1 calc R . . C6 C 0.91399(8) 0.13390(14) 0.09322(10) 0.0159(3) Uani 1 1 d . . . C7 C 0.98529(9) 0.24057(14) 0.10311(10) 0.0173(3) Uani 1 1 d . . . H7 H 1.0221 0.2244 0.1683 0.021 Uiso 1 1 calc R . . C8 C 1.03745(9) 0.21755(17) 0.02230(12) 0.0253(4) Uani 1 1 d . . . H8A H 1.0628 0.1232 0.0296 0.038 Uiso 1 1 calc R . . H8B H 1.0814 0.2895 0.0281 0.038 Uiso 1 1 calc R . . H8C H 1.0017 0.2252 -0.0425 0.038 Uiso 1 1 calc R . . C9 C 0.95281(10) 0.39315(15) 0.10157(12) 0.0261(4) Uani 1 1 d . . . H9A H 1.0000 0.4589 0.1118 0.039 Uiso 1 1 calc R . . H9B H 0.9200 0.4056 0.1543 0.039 Uiso 1 1 calc R . . H9C H 0.9176 0.4124 0.0376 0.039 Uiso 1 1 calc R . . C10 C 0.82490(9) -0.16640(15) 0.23348(11) 0.0196(3) Uani 1 1 d . . . H10 H 0.8507 -0.1243 0.2983 0.023 Uiso 1 1 calc R . . C11 C 0.87277(10) -0.30181(16) 0.21919(13) 0.0305(4) Uani 1 1 d . . . H11A H 0.8475 -0.3475 0.1573 0.046 Uiso 1 1 calc R . . H11B H 0.8706 -0.3664 0.2744 0.046 Uiso 1 1 calc R . . H11C H 0.9309 -0.2783 0.2167 0.046 Uiso 1 1 calc R . . C12 C 0.73467(10) -0.20309(17) 0.23931(12) 0.0275(4) Uani 1 1 d . . . H12A H 0.7105 -0.2587 0.1812 0.041 Uiso 1 1 calc R . . H12B H 0.7026 -0.1157 0.2413 0.041 Uiso 1 1 calc R . . H12C H 0.7330 -0.2585 0.2992 0.041 Uiso 1 1 calc R . . N1 N 0.96233(7) 0.01661(11) 0.25487(8) 0.0159(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(7) 0.0142(7) 0.0160(7) -0.0030(5) 0.0031(6) 0.0026(5) C2 0.0167(7) 0.0146(7) 0.0197(7) -0.0033(6) 0.0063(6) 0.0024(6) C3 0.0159(8) 0.0209(8) 0.0241(8) -0.0034(6) 0.0036(6) -0.0033(6) C4 0.0186(8) 0.0242(8) 0.0197(8) -0.0013(6) -0.0007(6) 0.0027(6) C5 0.0216(8) 0.0174(7) 0.0185(8) 0.0020(6) 0.0045(6) 0.0031(6) C6 0.0160(7) 0.0141(7) 0.0180(7) -0.0030(6) 0.0047(6) 0.0028(6) C7 0.0169(8) 0.0160(7) 0.0192(7) 0.0016(6) 0.0037(6) 0.0005(6) C8 0.0204(8) 0.0277(9) 0.0291(9) -0.0016(7) 0.0082(7) -0.0031(7) C9 0.0244(9) 0.0182(8) 0.0372(9) 0.0011(7) 0.0090(7) -0.0012(6) C10 0.0215(8) 0.0186(8) 0.0184(7) -0.0001(6) 0.0028(6) -0.0037(6) C11 0.0295(9) 0.0227(8) 0.0402(10) 0.0069(7) 0.0086(8) 0.0021(7) C12 0.0260(9) 0.0287(9) 0.0292(9) 0.0041(7) 0.0085(7) -0.0030(7) N1 0.0160(6) 0.0119(6) 0.0192(6) -0.0001(5) 0.0013(5) -0.0017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.4126(19) . ? C1 C2 1.4142(19) . ? C1 N1 1.4342(17) . ? C2 C3 1.387(2) . ? C2 C10 1.5210(19) . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? C4 C5 1.382(2) . ? C4 H4 0.9500 . ? C5 C6 1.395(2) . ? C5 H5 0.9500 . ? C6 C7 1.5263(19) . ? C7 C8 1.528(2) . ? C7 C9 1.534(2) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.527(2) . ? C10 C11 1.529(2) . ? 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 . ? N1 N1 1.258(2) 2_755 ? 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 C6 C1 C2 121.82(12) . . ? C6 C1 N1 121.75(12) . . ? C2 C1 N1 116.05(12) . . ? C3 C2 C1 118.16(13) . . ? C3 C2 C10 121.90(13) . . ? C1 C2 C10 119.90(12) . . ? C2 C3 C4 120.95(13) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.96(13) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 122.05(13) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 116.90(12) . . ? C5 C6 C7 118.17(12) . . ? C1 C6 C7 124.88(12) . . ? C6 C7 C8 110.64(11) . . ? C6 C7 C9 111.31(11) . . ? C8 C7 C9 110.98(12) . . ? C6 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 113.69(12) . . ? C2 C10 C11 110.51(12) . . ? C12 C10 C11 109.55(12) . . ? C2 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C11 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 . . ? N1 N1 C1 114.09(14) 2_755 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.177 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.039