Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_letter ; These are the CIF format data (6 compounds) for the paper "Efficient Nickel mediated Carbon Carbon Bond Cleavage of Organonitriles" Thomas Schaub, Christain D\"oring, and Udo Radius ; _publ_section_title ; Efficient Nickel mediated Carbon Carbon Bond Cleavage of Organonitriles ; _publ_contact_author_name 'Dr. Udo Radius' _publ_contact_author_address ; Institut fuer Anorganische Chemie University of Karlsruhe Engesserstr. 15 76131 Karlsruhe GERMANY ; _publ_contact_author_email radius@aoc1.uni-karlsruhe.de _publ_contact_author_phone 'Int + 721 608 8097' _publ_contact_author_fax 'Int + 721 608 8440' _audit_creation_method 'SHELXL-97 + manual editing' loop_ _publ_author_name 'Thomas Schaub' 'Christain Doring' 'Udo Radius' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 637875' # Local code [ NiImiPr2_CN_Ph _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)(Ph)Ni(II) ; _chemical_formula_sum 'C29 H37 N5 Ni O' _chemical_formula_weight 530.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4056(7) _cell_length_b 11.264(5) _cell_length_c 29.3343(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.343(8) _cell_angle_gamma 90.00 _cell_volume 3088.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.885 _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 14265 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5393 _reflns_number_gt 4218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.3648P] 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_number_reflns 5393 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.51562(3) 0.13111(2) 0.853620(8) 0.02941(11) Uani 1 d . . . C1 C 0.5181(3) 0.1855(2) 0.91498(7) 0.0363(5) Uani 1 d . . . C2 C 0.4728(5) 0.2933(3) 0.97652(9) 0.0676(10) Uani 1 d . . . H2 H 0.4296 0.3485 0.9947 0.081 Uiso 1 calc R . . C3 C 0.5831(4) 0.2236(3) 0.98988(8) 0.0614(9) Uani 1 d . . . H3 H 0.6330 0.2201 1.0194 0.074 Uiso 1 calc R . . C4 C 0.3169(4) 0.3285(3) 0.90123(11) 0.0615(8) Uani 1 d . . . H4 H 0.3089 0.2900 0.8707 0.074 Uiso 1 calc R . . C5 C 0.3550(6) 0.4572(4) 0.89469(17) 0.1047(16) Uani 1 d . . . H5A H 0.3660 0.4969 0.9242 0.157 Uiso 1 calc R . . H5B H 0.2794 0.4953 0.8747 0.157 Uiso 1 calc R . . H5C H 0.4440 0.4619 0.8810 0.157 Uiso 1 calc R . . C6 C 0.1761(6) 0.3111(5) 0.92063(17) 0.1093(16) Uani 1 d . . . H6A H 0.1623 0.2273 0.9265 0.164 Uiso 1 calc R . . H6B H 0.0987 0.3395 0.8988 0.164 Uiso 1 calc R . . H6C H 0.1769 0.3551 0.9491 0.164 Uiso 1 calc R . . C7 C 0.7274(4) 0.0714(3) 0.95102(9) 0.0591(8) Uani 1 d . . . H7 H 0.7117 0.0280 0.9215 0.071 Uiso 1 calc R . . C8 C 0.8684(6) 0.1349(5) 0.9524(2) 0.1137(18) Uani 1 d . . . H8A H 0.8665 0.1880 0.9263 0.171 Uiso 1 calc R . . H8B H 0.9445 0.0773 0.9511 0.171 Uiso 1 calc R . . H8C H 0.8852 0.1803 0.9805 0.171 Uiso 1 calc R . . C9 C 0.7260(6) -0.0185(4) 0.98916(14) 0.0956(14) Uani 1 d . . . H9A H 0.7430 0.0215 1.0186 0.143 Uiso 1 calc R . . H9B H 0.8004 -0.0770 0.9866 0.143 Uiso 1 calc R . . H9C H 0.6336 -0.0577 0.9868 0.143 Uiso 1 calc R . . C10 C 0.5064(2) 0.0806(2) 0.79148(6) 0.0293(4) Uani 1 d . . . C11 C 0.4436(3) 0.0700(2) 0.71529(7) 0.0404(6) Uani 1 d . . . H11 H 0.3939 0.0833 0.6861 0.048 Uiso 1 calc R . . C12 C 0.5597(3) 0.0036(2) 0.72435(7) 0.0411(6) Uani 1 d . . . H12 H 0.6072 -0.0397 0.7032 0.049 Uiso 1 calc R . . C13 C 0.2923(3) 0.2000(2) 0.76261(8) 0.0404(6) Uani 1 d . . . H13 H 0.2770 0.1996 0.7955 0.049 Uiso 1 calc R . . C14 C 0.3331(4) 0.3242(3) 0.75025(13) 0.0666(8) Uani 1 d . . . H14A H 0.4184 0.3482 0.7697 0.100 Uiso 1 calc R . . H14B H 0.2554 0.3781 0.7548 0.100 Uiso 1 calc R . . H14C H 0.3516 0.3265 0.7184 0.100 Uiso 1 calc R . . C15 C 0.1547(3) 0.1621(3) 0.73535(13) 0.0658(9) Uani 1 d . . . H15A H 0.1643 0.1686 0.7029 0.099 Uiso 1 calc R . . H15B H 0.0775 0.2129 0.7429 0.099 Uiso 1 calc R . . H15C H 0.1339 0.0805 0.7427 0.099 Uiso 1 calc R . . C16 C 0.7299(3) -0.0389(2) 0.79596(8) 0.0383(5) Uani 1 d . . . H16 H 0.7273 -0.0254 0.8292 0.046 Uiso 1 calc R . . C17 C 0.8578(3) 0.0279(3) 0.78152(10) 0.0556(7) Uani 1 d . . . H17A H 0.8614 0.0178 0.7488 0.083 Uiso 1 calc R . . H17B H 0.9449 -0.0031 0.7981 0.083 Uiso 1 calc R . . H17C H 0.8487 0.1116 0.7884 0.083 Uiso 1 calc R . . C18 C 0.7394(3) -0.1709(3) 0.78841(9) 0.0522(7) Uani 1 d . . . H18A H 0.6563 -0.2094 0.7986 0.078 Uiso 1 calc R . . H18B H 0.8255 -0.2015 0.8057 0.078 Uiso 1 calc R . . H18C H 0.7426 -0.1866 0.7560 0.078 Uiso 1 calc R . . C19 C 0.6437(3) 0.2541(2) 0.84160(7) 0.0463(6) Uani 1 d . . . C20 C 0.3930(3) 0.0013(2) 0.86689(6) 0.0349(5) Uani 1 d . . . C21 C 0.2458(3) 0.0106(3) 0.86875(8) 0.0473(6) Uani 1 d . . . H21 H 0.2011 0.0843 0.8623 0.057 Uiso 1 calc R . . C22 C 0.1624(3) -0.0860(3) 0.87992(9) 0.0591(8) Uani 1 d . . . H22 H 0.0637 -0.0759 0.8813 0.071 Uiso 1 calc R . . C23 C 0.2242(4) -0.1958(3) 0.88897(8) 0.0572(8) Uani 1 d . . . H23 H 0.1685 -0.2609 0.8963 0.069 Uiso 1 calc R . . C24 C 0.3682(4) -0.2079(3) 0.88700(8) 0.0538(7) Uani 1 d . . . H24 H 0.4118 -0.2822 0.8930 0.065 Uiso 1 calc R . . C25 C 0.4507(3) -0.1117(2) 0.87621(8) 0.0447(6) Uani 1 d . . . H25 H 0.5493 -0.1230 0.8751 0.054 Uiso 1 calc R . . N1 N 0.4334(3) 0.2690(2) 0.93033(6) 0.0475(5) Uani 1 d . . . N2 N 0.6114(3) 0.1564(2) 0.95205(6) 0.0453(5) Uani 1 d . . . N3 N 0.5972(2) 0.01099(17) 0.77165(6) 0.0332(4) Uani 1 d . . . N4 N 0.4083(2) 0.11640(17) 0.75653(6) 0.0322(4) Uani 1 d . . . N5 N 0.7230(4) 0.3272(3) 0.83457(9) 0.0796(10) Uani 1 d . . . C27 C 0.1503(12) 0.3318(11) 0.0925(4) 0.194(5) Uani 1 d . . . C29 C 0.2763(13) 0.4292(7) 0.0441(3) 0.166(4) Uani 1 d . . . C28 C 0.1704(14) 0.4534(13) 0.0302(3) 0.098(4) Uani 0.50 d P A 1 C26 C 0.0816(18) 0.3730(17) 0.0460(5) 0.169(8) Uani 0.50 d P A 1 O1 O 0.2595(16) 0.3972(10) 0.1042(4) 0.167(5) Uani 0.50 d P A 1 C30 C 0.236(4) 0.3223(14) 0.0666(9) 0.224(15) Uani 0.50 d P A 2 C31 C 0.0964(15) 0.4665(13) 0.0881(4) 0.123(4) Uani 0.50 d P A 2 O2 O 0.2117(13) 0.5117(6) 0.0613(2) 0.135(3) Uani 0.50 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.03361(17) 0.03069(18) 0.02487(15) 0.00121(10) 0.00740(10) -0.00182(12) C1 0.0465(15) 0.0325(13) 0.0312(10) 0.0024(8) 0.0094(9) -0.0069(10) C2 0.107(3) 0.061(2) 0.0393(14) -0.0144(13) 0.0284(15) -0.0071(19) C3 0.094(3) 0.063(2) 0.0281(12) -0.0055(11) 0.0073(13) -0.0111(18) C4 0.066(2) 0.053(2) 0.0679(18) -0.0070(14) 0.0154(15) 0.0148(15) C5 0.125(4) 0.055(3) 0.128(4) 0.016(2) -0.015(3) 0.014(2) C6 0.077(3) 0.137(5) 0.120(3) -0.026(3) 0.037(3) 0.014(3) C7 0.064(2) 0.062(2) 0.0470(14) 0.0043(12) -0.0101(13) 0.0005(15) C8 0.067(3) 0.105(4) 0.166(5) 0.035(3) -0.003(3) -0.006(3) C9 0.119(4) 0.071(3) 0.093(3) 0.036(2) -0.003(3) 0.007(2) C10 0.0296(12) 0.0302(12) 0.0286(9) 0.0028(8) 0.0056(8) 0.0001(9) C11 0.0424(14) 0.0518(16) 0.0270(10) -0.0006(9) 0.0039(9) 0.0038(11) C12 0.0457(15) 0.0511(16) 0.0274(10) -0.0050(9) 0.0085(9) 0.0061(11) C13 0.0388(14) 0.0453(16) 0.0385(11) 0.0082(9) 0.0099(10) 0.0115(11) C14 0.058(2) 0.0395(18) 0.103(2) -0.0005(16) 0.0093(17) 0.0049(14) C15 0.0362(16) 0.058(2) 0.103(2) 0.0090(16) 0.0048(15) 0.0044(13) C16 0.0321(13) 0.0461(15) 0.0368(11) 0.0037(9) 0.0045(9) 0.0096(10) C17 0.0362(15) 0.0603(19) 0.0707(17) 0.0105(14) 0.0069(12) 0.0029(13) C18 0.0557(18) 0.0434(16) 0.0577(15) 0.0038(12) 0.0070(13) 0.0129(13) C19 0.0624(18) 0.0477(17) 0.0306(11) -0.0036(10) 0.0132(10) -0.0156(13) C20 0.0429(14) 0.0381(14) 0.0242(9) -0.0007(8) 0.0063(8) -0.0064(10) C21 0.0449(16) 0.0512(17) 0.0461(13) 0.0032(11) 0.0058(11) -0.0074(12) C22 0.0466(17) 0.080(2) 0.0510(15) -0.0001(14) 0.0081(12) -0.0228(15) C23 0.077(2) 0.053(2) 0.0416(13) 0.0009(11) 0.0099(13) -0.0323(16) C24 0.080(2) 0.0384(17) 0.0442(13) 0.0039(10) 0.0104(13) -0.0130(14) C25 0.0529(16) 0.0407(16) 0.0420(12) 0.0031(10) 0.0120(11) -0.0042(11) N1 0.0646(16) 0.0423(13) 0.0382(10) -0.0042(8) 0.0172(9) -0.0007(11) N2 0.0591(15) 0.0482(14) 0.0281(9) 0.0026(8) 0.0029(9) -0.0081(10) N3 0.0307(10) 0.0391(12) 0.0300(8) -0.0004(7) 0.0046(7) 0.0039(8) N4 0.0305(10) 0.0379(11) 0.0284(8) 0.0015(7) 0.0044(7) 0.0039(8) N5 0.107(3) 0.079(2) 0.0580(15) -0.0106(13) 0.0319(15) -0.053(2) C27 0.157(9) 0.232(11) 0.190(8) 0.104(8) 0.010(7) -0.062(8) C29 0.239(12) 0.106(6) 0.183(7) -0.005(5) 0.160(8) -0.002(6) C28 0.095(8) 0.138(10) 0.056(4) 0.016(5) -0.007(5) -0.013(7) C26 0.127(12) 0.224(18) 0.139(10) 0.067(11) -0.066(10) -0.086(12) O1 0.180(11) 0.143(9) 0.163(8) 0.048(7) -0.044(8) -0.040(8) C30 0.36(4) 0.066(9) 0.29(2) 0.018(12) 0.24(3) 0.054(14) C31 0.105(9) 0.145(11) 0.127(8) -0.003(8) 0.043(7) 0.035(8) O2 0.255(12) 0.058(4) 0.104(5) -0.020(3) 0.074(6) -0.023(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 Ni C19 1.895(3) . ? Ni C1 1.899(2) . ? Ni C10 1.902(2) . ? Ni C20 1.928(2) . ? C1 N1 1.343(3) . ? C1 N2 1.359(3) . ? C2 C3 1.325(5) . ? C2 N1 1.392(3) . ? C2 H2 0.9400 . ? C3 N2 1.393(4) . ? C3 H3 0.9400 . ? C4 N1 1.474(4) . ? C4 C5 1.510(6) . ? C4 C6 1.511(6) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 N2 1.455(4) . ? C7 C8 1.504(6) . ? C7 C9 1.510(5) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 N3 1.338(3) . ? C10 N4 1.363(3) . ? C11 C12 1.326(4) . ? C11 N4 1.391(3) . ? C11 H11 0.9400 . ? C12 N3 1.396(3) . ? C12 H12 0.9400 . ? C13 N4 1.466(3) . ? C13 C15 1.506(4) . ? C13 C14 1.506(4) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 N3 1.479(3) . ? C16 C18 1.507(4) . ? C16 C17 1.518(4) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 N5 1.144(4) . ? C20 C21 1.395(4) . ? C20 C25 1.398(4) . ? C21 C22 1.402(4) . ? C21 H21 0.9400 . ? C22 C23 1.380(5) . ? C22 H22 0.9400 . ? C23 C24 1.369(5) . ? C23 H23 0.9400 . ? C24 C25 1.390(4) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C27 C30 1.176(18) . ? C27 O1 1.279(12) . ? C27 C26 1.518(14) . ? C27 C31 1.601(17) . ? C29 C28 1.070(13) . ? C29 O2 1.246(10) . ? C29 C30 1.441(19) . ? C29 O1 1.823(14) . ? C29 C26 1.944(18) . ? C28 C26 1.349(18) . ? C31 O2 1.499(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 C19 Ni C1 89.94(10) . . ? C19 Ni C10 90.15(10) . . ? C1 Ni C10 177.66(10) . . ? C19 Ni C20 177.27(12) . . ? C1 Ni C20 89.90(9) . . ? C10 Ni C20 90.12(9) . . ? N1 C1 N2 104.76(19) . . ? N1 C1 Ni 126.73(17) . . ? N2 C1 Ni 128.3(2) . . ? C3 C2 N1 106.7(3) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 107.4(2) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N1 C4 C5 109.8(3) . . ? N1 C4 C6 110.4(3) . . ? C5 C4 C6 113.7(4) . . ? N1 C4 H4 107.5 . . ? C5 C4 H4 107.5 . . ? C6 C4 H4 107.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 110.4(3) . . ? N2 C7 C9 111.0(3) . . ? C8 C7 C9 112.3(3) . . ? N2 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? 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 . . ? N3 C10 N4 104.93(17) . . ? N3 C10 Ni 128.90(15) . . ? N4 C10 Ni 126.02(17) . . ? C12 C11 N4 107.95(19) . . ? C12 C11 H11 126.0 . . ? N4 C11 H11 126.0 . . ? C11 C12 N3 106.1(2) . . ? C11 C12 H12 127.0 . . ? N3 C12 H12 127.0 . . ? N4 C13 C15 111.2(2) . . ? N4 C13 C14 110.8(2) . . ? C15 C13 C14 111.2(2) . . ? N4 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? 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 . . ? N3 C16 C18 111.4(2) . . ? N3 C16 C17 109.2(2) . . ? C18 C16 C17 112.7(2) . . ? N3 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 Ni 178.8(3) . . ? C21 C20 C25 115.2(2) . . ? C21 C20 Ni 124.66(19) . . ? C25 C20 Ni 120.1(2) . . ? C20 C21 C22 122.3(3) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 118.6(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 122.7(3) . . ? C24 C25 H25 118.7 . . ? C20 C25 H25 118.7 . . ? C1 N1 C2 111.1(2) . . ? C1 N1 C4 123.7(2) . . ? C2 N1 C4 125.1(3) . . ? C1 N2 C3 110.1(3) . . ? C1 N2 C7 124.1(2) . . ? C3 N2 C7 125.7(2) . . ? C10 N3 C12 111.36(18) . . ? C10 N3 C16 123.93(17) . . ? C12 N3 C16 124.28(19) . . ? C10 N4 C11 109.6(2) . . ? C10 N4 C13 123.32(18) . . ? C11 N4 C13 126.81(18) . . ? C30 C27 O1 68.7(17) . . ? C30 C27 C26 72.6(18) . . ? O1 C27 C26 108.3(8) . . ? C30 C27 C31 105.6(10) . . ? O1 C27 C31 73.4(11) . . ? C26 C27 C31 62.4(10) . . ? C28 C29 O2 59.3(9) . . ? C28 C29 C30 96.3(18) . . ? O2 C29 C30 106.0(8) . . ? C28 C29 O1 104.1(10) . . ? O2 C29 O1 70.1(7) . . ? C30 C29 O1 48.6(10) . . ? C28 C29 C26 41.7(9) . . ? O2 C29 C26 74.3(10) . . ? C30 C29 C26 54.7(13) . . ? O1 C29 C26 74.1(6) . . ? C29 C28 C26 106.4(13) . . ? C28 C26 C27 107.2(8) . . ? C28 C26 C29 31.9(6) . . ? C27 C26 C29 79.4(7) . . ? C27 O1 C29 90.4(8) . . ? C27 C30 C29 116.9(12) . . ? O2 C31 C27 97.1(8) . . ? C29 O2 C31 111.8(8) . . ? _diffrn_measured_fraction_theta_max 0.845 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.850 _refine_diff_density_max 0.399 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.050 _chemical_name_common (iPr2Im)2(CN)(Ph)Ni(ii) data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 637876' # Local code NiImiPr2_CN_Dimethoxyphenyl _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)(2,4-Dimethoxyphenyl)Ni(II) ; _chemical_formula_sum 'C27 H41 N5 Ni O2' _chemical_formula_weight 526.36 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0661(19) _cell_length_b 9.8684(12) _cell_length_c 38.201(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.117(18) _cell_angle_gamma 90.00 _cell_volume 5671.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 22917 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9450 _reflns_number_gt 5807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9450 _refine_ls_number_parameters 651 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.25313(3) 0.08588(5) 0.191311(14) 0.02525(14) Uani 1 d . . . Ni2 Ni 0.23093(3) -0.87350(5) 0.441165(15) 0.02745(14) Uani 1 d . . . N1 N 0.0737(2) -0.0094(3) 0.16949(10) 0.0303(8) Uani 1 d . . . N2 N 0.0703(2) 0.1435(3) 0.20898(9) 0.0277(8) Uani 1 d . . . N3 N 0.4343(2) 0.2056(3) 0.20074(10) 0.0304(8) Uani 1 d . . . N4 N 0.4314(2) 0.0263(3) 0.16934(10) 0.0296(8) Uani 1 d . . . N5 N 0.2168(4) 0.2869(5) 0.13194(14) 0.0667(14) Uani 1 d . . . N6 N 0.0697(2) -1.0193(3) 0.41724(10) 0.0330(8) Uani 1 d . . . N7 N 0.0411(2) -0.8739(3) 0.45656(10) 0.0326(8) Uani 1 d . . . N8 N 0.4242(2) -0.9109(3) 0.43957(10) 0.0314(8) Uani 1 d . . . N9 N 0.3914(2) -0.7037(3) 0.44947(10) 0.0351(9) Uani 1 d . . . N10 N 0.1928(3) -0.7161(5) 0.37335(13) 0.0551(11) Uani 1 d . . . C1 C 0.1277(3) 0.0695(4) 0.19076(11) 0.0272(9) Uani 1 d . . . C2 C -0.0167(3) 0.1149(4) 0.19869(12) 0.0345(10) Uani 1 d . . . H2 H -0.0676 0.1556 0.2073 0.041 Uiso 1 calc R . . C3 C -0.0156(3) 0.0187(4) 0.17427(12) 0.0321(10) Uani 1 d . . . H3A H -0.0651 -0.0223 0.1626 0.039 Uiso 1 calc R . . C4 C 0.1068(3) -0.1010(4) 0.14272(13) 0.0390(11) Uani 1 d . . . H4 H 0.1715 -0.1131 0.1478 0.047 Uiso 1 calc R . . C5 C 0.0936(5) -0.0387(7) 0.10676(16) 0.0731(18) Uani 1 d . . . H5A H 0.0305 -0.0275 0.1010 0.110 Uiso 1 calc R . . H5B H 0.1191 -0.0975 0.0896 0.110 Uiso 1 calc R . . H5C H 0.1226 0.0490 0.1066 0.110 Uiso 1 calc R . . C6 C 0.0628(4) -0.2396(5) 0.1454(2) 0.0670(18) Uani 1 d . . . H6A H 0.0756 -0.2766 0.1687 0.101 Uiso 1 calc R . . H6B H 0.0858 -0.3002 0.1281 0.101 Uiso 1 calc R . . H6C H -0.0010 -0.2302 0.1412 0.101 Uiso 1 calc R . . C7 C 0.0997(3) 0.2458(4) 0.23531(12) 0.0341(10) Uani 1 d . . . H7 H 0.1654 0.2429 0.2375 0.041 Uiso 1 calc R . . C8 C 0.0732(4) 0.3866(4) 0.22291(17) 0.0628(17) Uani 1 d . . . H8A H 0.0970 0.4036 0.2002 0.094 Uiso 1 calc R . . H8B H 0.0967 0.4531 0.2397 0.094 Uiso 1 calc R . . H8C H 0.0089 0.3935 0.2209 0.094 Uiso 1 calc R . . C9 C 0.0666(5) 0.2091(6) 0.27050(16) 0.0656(16) Uani 1 d . . . H9A H 0.0023 0.2166 0.2697 0.098 Uiso 1 calc R . . H9B H 0.0922 0.2702 0.2882 0.098 Uiso 1 calc R . . H9C H 0.0838 0.1167 0.2763 0.098 Uiso 1 calc R . . C10 C 0.3789(3) 0.1051(4) 0.18851(11) 0.0293(9) Uani 1 d . . . C11 C 0.5183(3) 0.1895(4) 0.18865(13) 0.0366(11) Uani 1 d . . . H11 H 0.5674 0.2465 0.1935 0.044 Uiso 1 calc R . . C12 C 0.5170(3) 0.0786(4) 0.16891(12) 0.0350(10) Uani 1 d . . . H12 H 0.5646 0.0425 0.1570 0.042 Uiso 1 calc R . . C13 C 0.3971(3) -0.0871(4) 0.14725(12) 0.0331(10) Uani 1 d . . . H13 H 0.3427 -0.1216 0.1577 0.040 Uiso 1 calc R . . C14 C 0.4638(4) -0.2025(5) 0.14737(15) 0.0497(13) Uani 1 d . . . H14A H 0.5167 -0.1730 0.1361 0.075 Uiso 1 calc R . . H14B H 0.4377 -0.2791 0.1347 0.075 Uiso 1 calc R . . H14C H 0.4795 -0.2290 0.1714 0.075 Uiso 1 calc R . . C15 C 0.3708(4) -0.0354(5) 0.11103(14) 0.0476(13) Uani 1 d . . . H15A H 0.3270 0.0362 0.1127 0.071 Uiso 1 calc R . . H15B H 0.3455 -0.1089 0.0969 0.071 Uiso 1 calc R . . H15C H 0.4228 -0.0001 0.1002 0.071 Uiso 1 calc R . . C16 C 0.4065(3) 0.3232(4) 0.22168(13) 0.0391(11) Uani 1 d . . . H16 H 0.3461 0.3053 0.2296 0.047 Uiso 1 calc R . . C17 C 0.4699(4) 0.3381(6) 0.25392(17) 0.0673(17) Uani 1 d . . . H17A H 0.4678 0.2568 0.2681 0.101 Uiso 1 calc R . . H17B H 0.4524 0.4156 0.2676 0.101 Uiso 1 calc R . . H17C H 0.5300 0.3514 0.2466 0.101 Uiso 1 calc R . . C18 C 0.4029(4) 0.4491(5) 0.19860(18) 0.0645(17) Uani 1 d . . . H18A H 0.4625 0.4727 0.1924 0.097 Uiso 1 calc R . . H18B H 0.3777 0.5238 0.2113 0.097 Uiso 1 calc R . . H18C H 0.3661 0.4311 0.1775 0.097 Uiso 1 calc R . . C19 C 0.2336(3) 0.2144(4) 0.15518(13) 0.0383(11) Uani 1 d . . . C20 C 0.2631(3) -0.0507(4) 0.22775(12) 0.0282(9) Uani 1 d . . . C21 C 0.2774(3) -0.0156(4) 0.26342(12) 0.0298(9) Uani 1 d . . . C22 C 0.2748(3) -0.1087(4) 0.29069(12) 0.0342(10) Uani 1 d . . . H22 H 0.2836 -0.0801 0.3141 0.041 Uiso 1 calc R . . C23 C 0.2591(3) -0.2447(4) 0.28293(13) 0.0347(10) Uani 1 d . . . C24 C 0.2465(3) -0.2869(4) 0.24903(13) 0.0379(11) Uani 1 d . . . H24 H 0.2367 -0.3789 0.2438 0.045 Uiso 1 calc R . . C25 C 0.2486(3) -0.1893(4) 0.22187(13) 0.0360(10) Uani 1 d . . . H25 H 0.2398 -0.2193 0.1986 0.043 Uiso 1 calc R . . C26 C 0.2517(3) -0.4698(4) 0.30575(16) 0.0489(13) Uani 1 d . . . H26A H 0.1981 -0.4901 0.2915 0.073 Uiso 1 calc R . . H26B H 0.2502 -0.5174 0.3279 0.073 Uiso 1 calc R . . H26C H 0.3032 -0.4987 0.2936 0.073 Uiso 1 calc R . . C27 C 0.3065(5) 0.1617(5) 0.30537(15) 0.0611(16) Uani 1 d . . . H27A H 0.2548 0.1365 0.3180 0.092 Uiso 1 calc R . . H27B H 0.3145 0.2592 0.3065 0.092 Uiso 1 calc R . . H27C H 0.3588 0.1174 0.3159 0.092 Uiso 1 calc R . . C28 C 0.1095(3) -0.9254(4) 0.43897(11) 0.0290(9) Uani 1 d . . . C29 C -0.0394(3) -0.9349(4) 0.44602(14) 0.0411(11) Uani 1 d . . . H29 H -0.0955 -0.9161 0.4545 0.049 Uiso 1 calc R . . C30 C -0.0208(3) -1.0253(5) 0.42149(14) 0.0427(12) Uani 1 d . . . H30 H -0.0617 -1.0825 0.4093 0.051 Uiso 1 calc R . . C31 C 0.1187(3) -1.0993(4) 0.39173(13) 0.0402(11) Uani 1 d . . . H31 H 0.1822 -1.0735 0.3944 0.048 Uiso 1 calc R . . C32 C 0.1115(4) -1.2508(5) 0.39986(18) 0.0646(16) Uani 1 d . . . H32A H 0.1293 -1.2667 0.4243 0.097 Uiso 1 calc R . . H32B H 0.1500 -1.3015 0.3851 0.097 Uiso 1 calc R . . H32C H 0.0505 -1.2802 0.3953 0.097 Uiso 1 calc R . . C33 C 0.0853(4) -1.0652(6) 0.35483(15) 0.0611(15) Uani 1 d . . . H33A H 0.0229 -1.0886 0.3517 0.092 Uiso 1 calc R . . H33B H 0.1189 -1.1161 0.3383 0.092 Uiso 1 calc R . . H33C H 0.0928 -0.9690 0.3507 0.092 Uiso 1 calc R . . C34 C 0.0532(3) -0.7678(4) 0.48390(13) 0.0375(11) Uani 1 d . . . H34 H 0.1043 -0.7944 0.4998 0.045 Uiso 1 calc R . . C35 C 0.0752(4) -0.6334(5) 0.46747(16) 0.0578(15) Uani 1 d . . . H35A H 0.1256 -0.6447 0.4530 0.087 Uiso 1 calc R . . H35B H 0.0899 -0.5677 0.4858 0.087 Uiso 1 calc R . . H35C H 0.0243 -0.6017 0.4531 0.087 Uiso 1 calc R . . C36 C -0.0277(4) -0.7557(5) 0.50559(16) 0.0586(15) Uani 1 d . . . H36A H -0.0769 -0.7183 0.4913 0.088 Uiso 1 calc R . . H36B H -0.0141 -0.6964 0.5254 0.088 Uiso 1 calc R . . H36C H -0.0438 -0.8447 0.5140 0.088 Uiso 1 calc R . . C37 C 0.3534(3) -0.8278(4) 0.44343(12) 0.0307(9) Uani 1 d . . . C38 C 0.4833(3) -0.7119(4) 0.44985(13) 0.0381(11) Uani 1 d . . . H38 H 0.5235 -0.6401 0.4539 0.046 Uiso 1 calc R . . C39 C 0.5040(3) -0.8405(5) 0.44335(13) 0.0395(11) Uani 1 d . . . H39 H 0.5613 -0.8766 0.4417 0.047 Uiso 1 calc R . . C40 C 0.3411(3) -0.5776(4) 0.45248(14) 0.0438(12) Uani 1 d . . . H40 H 0.2785 -0.6019 0.4560 0.053 Uiso 1 calc R . . C41 C 0.3762(5) -0.4986(5) 0.48462(19) 0.0692(18) Uani 1 d . . . H41A H 0.3797 -0.5581 0.5048 0.104 Uiso 1 calc R . . H41B H 0.3364 -0.4239 0.4889 0.104 Uiso 1 calc R . . H41C H 0.4349 -0.4635 0.4806 0.104 Uiso 1 calc R . . C42 C 0.3428(4) -0.4934(5) 0.41931(17) 0.0585(15) Uani 1 d . . . H42A H 0.4038 -0.4721 0.4146 0.088 Uiso 1 calc R . . H42B H 0.3099 -0.4101 0.4223 0.088 Uiso 1 calc R . . H42C H 0.3157 -0.5443 0.3998 0.088 Uiso 1 calc R . . C43 C 0.4158(3) -1.0553(4) 0.42994(13) 0.0404(11) Uani 1 d . . . H43 H 0.3538 -1.0837 0.4333 0.048 Uiso 1 calc R . . C45 C 0.4336(6) -1.0720(6) 0.3917(2) 0.096(3) Uani 1 d . . . H45A H 0.3947 -1.0123 0.3777 0.144 Uiso 1 calc R . . H45B H 0.4224 -1.1652 0.3847 0.144 Uiso 1 calc R . . H45C H 0.4950 -1.0493 0.3881 0.144 Uiso 1 calc R . . C46 C 0.2096(3) -0.7782(4) 0.39842(14) 0.0377(11) Uani 1 d . . . C47 C 0.2482(3) -0.9663(4) 0.48575(12) 0.0309(10) Uani 1 d . . . C48 C 0.2587(3) -0.8953(4) 0.51782(11) 0.0278(9) Uani 1 d . . . C49 C 0.2654(3) -0.9580(4) 0.55061(12) 0.0322(10) Uani 1 d . . . H49 H 0.2700 -0.9060 0.5712 0.039 Uiso 1 calc R . . C50 C 0.2651(3) -1.0987(4) 0.55217(13) 0.0333(10) Uani 1 d . . . C51 C 0.2576(3) -1.1732(4) 0.52130(13) 0.0359(11) Uani 1 d . . . H51 H 0.2592 -1.2684 0.5221 0.043 Uiso 1 calc R . . C52 C 0.2480(3) -1.1071(4) 0.48954(13) 0.0362(10) Uani 1 d . . . H52 H 0.2407 -1.1601 0.4691 0.043 Uiso 1 calc R . . C53 C 0.2702(4) -1.0960(5) 0.61466(14) 0.0526(13) Uani 1 d . . . H53A H 0.3221 -1.0376 0.6164 0.079 Uiso 1 calc R . . H53B H 0.2719 -1.1577 0.6344 0.079 Uiso 1 calc R . . H53C H 0.2168 -1.0412 0.6148 0.079 Uiso 1 calc R . . C54 C 0.2481(5) -0.6792(5) 0.54640(15) 0.0597(16) Uani 1 d . . . H54A H 0.1981 -0.7149 0.5585 0.090 Uiso 1 calc R . . H54B H 0.2372 -0.5849 0.5405 0.090 Uiso 1 calc R . . H54C H 0.3017 -0.6862 0.5616 0.090 Uiso 1 calc R . . O1 O 0.2939(2) 0.1208(3) 0.26982(8) 0.0390(7) Uani 1 d . . . O2 O 0.2567(2) -0.3281(3) 0.31200(9) 0.0446(8) Uani 1 d . . . O3 O 0.2588(2) -0.7550(3) 0.51515(8) 0.0365(7) Uani 1 d . . . O4 O 0.2702(2) -1.1709(3) 0.58318(10) 0.0475(9) Uani 1 d . . . C55 C 0.4763(5) -1.1405(6) 0.4534(2) 0.081(2) Uani 1 d . . . H55A H 0.5375 -1.1243 0.4480 0.121 Uiso 1 calc R . . H55B H 0.4621 -1.2355 0.4498 0.121 Uiso 1 calc R . . H55C H 0.4684 -1.1168 0.4777 0.121 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0232(3) 0.0292(3) 0.0234(3) -0.0006(2) 0.0016(2) -0.0025(2) Ni2 0.0212(3) 0.0342(3) 0.0271(3) -0.0041(2) 0.0029(2) -0.0034(2) N1 0.026(2) 0.0336(17) 0.031(2) -0.0031(15) 0.0027(16) -0.0020(14) N2 0.0255(19) 0.0302(16) 0.0277(19) -0.0012(14) 0.0035(15) 0.0005(14) N3 0.027(2) 0.0362(18) 0.027(2) -0.0030(15) 0.0000(16) -0.0043(14) N4 0.0244(19) 0.0366(17) 0.028(2) -0.0012(15) 0.0007(16) -0.0010(14) N5 0.085(4) 0.058(3) 0.056(3) 0.022(2) -0.007(3) -0.001(2) N6 0.024(2) 0.0451(19) 0.031(2) -0.0027(16) 0.0054(16) -0.0059(15) N7 0.025(2) 0.0425(19) 0.031(2) -0.0025(16) 0.0061(16) -0.0001(15) N8 0.0228(19) 0.0388(18) 0.033(2) -0.0031(16) 0.0077(16) -0.0021(14) N9 0.030(2) 0.0362(18) 0.040(2) -0.0058(16) 0.0071(17) -0.0061(15) N10 0.058(3) 0.072(3) 0.036(3) 0.008(2) 0.006(2) -0.009(2) C1 0.029(2) 0.0280(19) 0.024(2) 0.0052(17) -0.0017(18) -0.0003(16) C2 0.022(2) 0.040(2) 0.042(3) 0.000(2) 0.005(2) -0.0001(17) C3 0.021(2) 0.043(2) 0.032(3) -0.0033(19) 0.0013(19) -0.0061(17) C4 0.032(3) 0.047(2) 0.038(3) -0.017(2) 0.004(2) -0.0016(19) C5 0.076(5) 0.101(5) 0.041(4) -0.022(3) -0.007(3) 0.012(4) C6 0.053(3) 0.053(3) 0.096(5) -0.038(3) 0.017(3) -0.010(3) C7 0.035(2) 0.031(2) 0.036(3) -0.0057(18) 0.003(2) -0.0002(17) C8 0.083(4) 0.036(3) 0.066(4) -0.010(2) -0.025(3) 0.005(2) C9 0.081(4) 0.071(3) 0.046(4) -0.018(3) 0.011(3) -0.021(3) C10 0.031(2) 0.032(2) 0.025(2) -0.0001(17) 0.0009(18) -0.0034(17) C11 0.027(2) 0.043(2) 0.040(3) 0.002(2) -0.001(2) -0.0072(18) C12 0.022(2) 0.050(2) 0.034(3) -0.002(2) 0.0056(19) -0.0022(18) C13 0.034(3) 0.033(2) 0.032(2) -0.0053(18) 0.0008(19) -0.0012(17) C14 0.059(3) 0.044(3) 0.046(3) -0.008(2) -0.001(3) 0.011(2) C15 0.054(3) 0.044(2) 0.043(3) -0.011(2) -0.014(3) 0.010(2) C16 0.038(3) 0.043(2) 0.036(3) -0.009(2) 0.003(2) -0.0082(19) C17 0.063(4) 0.086(4) 0.053(4) -0.028(3) -0.001(3) -0.009(3) C18 0.081(5) 0.035(3) 0.078(5) -0.006(3) 0.011(4) 0.000(2) C19 0.036(3) 0.039(2) 0.041(3) 0.002(2) 0.004(2) -0.0055(19) C20 0.020(2) 0.032(2) 0.033(2) 0.0000(17) 0.0064(18) 0.0005(15) C21 0.028(2) 0.031(2) 0.031(3) -0.0028(18) 0.0036(19) 0.0016(16) C22 0.033(3) 0.040(2) 0.029(2) 0.0032(19) 0.0055(19) 0.0037(18) C23 0.028(2) 0.033(2) 0.043(3) 0.011(2) 0.006(2) 0.0014(17) C24 0.038(3) 0.029(2) 0.047(3) 0.002(2) 0.004(2) -0.0004(18) C25 0.036(3) 0.036(2) 0.036(3) -0.0025(19) 0.006(2) 0.0003(18) C26 0.037(3) 0.044(2) 0.066(4) 0.024(3) 0.004(3) 0.002(2) C27 0.103(5) 0.040(3) 0.039(3) -0.006(2) -0.004(3) -0.003(3) C28 0.030(2) 0.033(2) 0.024(2) 0.0022(17) 0.0023(18) 0.0016(17) C29 0.020(2) 0.050(3) 0.053(3) -0.002(2) 0.003(2) -0.0026(18) C30 0.022(2) 0.053(3) 0.052(3) -0.003(2) -0.004(2) -0.012(2) C31 0.035(3) 0.049(3) 0.037(3) -0.017(2) 0.004(2) -0.001(2) C32 0.078(4) 0.050(3) 0.066(4) -0.020(3) 0.001(3) 0.008(3) C33 0.067(4) 0.079(4) 0.037(3) -0.013(3) 0.006(3) 0.004(3) C34 0.033(3) 0.041(2) 0.038(3) -0.006(2) -0.006(2) 0.0096(18) C35 0.066(4) 0.049(3) 0.060(4) -0.013(3) 0.020(3) -0.011(3) C36 0.075(4) 0.056(3) 0.048(3) -0.007(2) 0.030(3) 0.000(3) C37 0.029(2) 0.034(2) 0.029(2) -0.0039(17) 0.0025(19) -0.0037(17) C38 0.026(2) 0.048(3) 0.041(3) -0.010(2) 0.005(2) -0.0152(19) C39 0.020(2) 0.060(3) 0.039(3) -0.002(2) 0.001(2) -0.0073(19) C40 0.034(3) 0.043(2) 0.056(3) -0.011(2) 0.013(2) -0.008(2) C41 0.080(5) 0.050(3) 0.078(5) -0.024(3) 0.012(4) -0.011(3) C42 0.054(4) 0.051(3) 0.070(4) 0.008(3) 0.000(3) -0.002(2) C43 0.038(3) 0.040(2) 0.044(3) -0.005(2) 0.011(2) 0.0014(19) C45 0.159(8) 0.063(4) 0.070(5) -0.023(3) 0.049(5) -0.014(4) C46 0.031(3) 0.044(2) 0.038(3) -0.006(2) 0.004(2) -0.0084(19) C47 0.019(2) 0.036(2) 0.039(3) -0.0001(19) 0.0042(19) 0.0005(16) C48 0.023(2) 0.034(2) 0.026(2) -0.0039(17) 0.0028(17) -0.0008(16) C49 0.021(2) 0.044(2) 0.031(3) -0.0031(19) 0.0010(19) 0.0025(17) C50 0.020(2) 0.037(2) 0.044(3) 0.009(2) 0.0075(19) 0.0055(17) C51 0.030(2) 0.029(2) 0.050(3) -0.001(2) 0.009(2) 0.0060(17) C52 0.033(3) 0.033(2) 0.043(3) -0.007(2) 0.006(2) 0.0009(17) C53 0.060(4) 0.059(3) 0.039(3) 0.009(2) 0.004(3) 0.007(3) C54 0.103(5) 0.037(2) 0.040(3) -0.008(2) 0.011(3) -0.003(3) O1 0.052(2) 0.0321(15) 0.0320(18) -0.0035(13) -0.0023(15) -0.0003(13) O2 0.051(2) 0.0372(16) 0.046(2) 0.0158(14) 0.0069(17) 0.0002(14) O3 0.0458(19) 0.0363(15) 0.0276(18) -0.0056(13) 0.0057(14) -0.0038(13) O4 0.052(2) 0.0437(17) 0.047(2) 0.0119(15) 0.0002(17) 0.0089(15) C55 0.067(4) 0.053(3) 0.121(7) 0.021(4) -0.012(4) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C19 1.886(5) . ? Ni1 C1 1.896(4) . ? Ni1 C10 1.913(4) . ? Ni1 C20 1.937(4) . ? Ni2 C46 1.896(5) . ? Ni2 C28 1.897(4) . ? Ni2 C37 1.897(4) . ? Ni2 C47 1.939(5) . ? N1 C1 1.362(5) . ? N1 C3 1.395(5) . ? N1 C4 1.473(6) . ? N2 C1 1.353(5) . ? N2 C2 1.378(5) . ? N2 C7 1.476(5) . ? N3 C10 1.363(5) . ? N3 C11 1.379(6) . ? N3 C16 1.483(6) . ? N4 C10 1.352(5) . ? N4 C12 1.390(5) . ? N4 C13 1.478(5) . ? N5 C19 1.158(6) . ? N6 C28 1.362(5) . ? N6 C30 1.383(6) . ? N6 C31 1.482(6) . ? N7 C28 1.359(5) . ? N7 C29 1.393(6) . ? N7 C34 1.483(6) . ? N8 C37 1.360(5) . ? N8 C39 1.388(5) . ? N8 C43 1.475(5) . ? N9 C37 1.366(5) . ? N9 C38 1.385(6) . ? N9 C40 1.466(6) . ? N10 C46 1.154(6) . ? C2 C3 1.332(6) . ? C4 C5 1.509(8) . ? C4 C6 1.526(7) . ? C7 C9 1.504(8) . ? C7 C8 1.514(6) . ? C11 C12 1.329(6) . ? C13 C15 1.508(7) . ? C13 C14 1.518(6) . ? C16 C18 1.523(7) . ? C16 C17 1.525(7) . ? C20 C25 1.401(6) . ? C20 C21 1.411(6) . ? C21 O1 1.388(5) . ? C21 C22 1.391(6) . ? C22 C23 1.391(6) . ? C23 C24 1.364(7) . ? C23 O2 1.384(5) . ? C24 C25 1.417(6) . ? C26 O2 1.420(6) . ? C27 O1 1.420(6) . ? C29 C30 1.334(7) . ? C31 C33 1.509(7) . ? C31 C32 1.533(7) . ? C34 C35 1.511(7) . ? C34 C36 1.515(7) . ? C38 C39 1.334(6) . ? C40 C42 1.516(8) . ? C40 C41 1.524(8) . ? C43 C55 1.501(8) . ? C43 C45 1.508(8) . ? C47 C52 1.397(6) . ? C47 C48 1.412(6) . ? C48 O3 1.389(5) . ? C48 C49 1.396(6) . ? C49 C50 1.390(6) . ? C50 O4 1.381(6) . ? C50 C51 1.389(7) . ? C51 C52 1.379(7) . ? C53 O4 1.412(6) . ? C54 O3 1.426(6) . ? 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 C19 Ni1 C1 86.18(18) . . ? C19 Ni1 C10 90.47(19) . . ? C1 Ni1 C10 176.09(18) . . ? C19 Ni1 C20 175.27(18) . . ? C1 Ni1 C20 89.24(17) . . ? C10 Ni1 C20 94.07(17) . . ? C46 Ni2 C28 88.73(18) . . ? C46 Ni2 C37 92.31(19) . . ? C28 Ni2 C37 178.10(17) . . ? C46 Ni2 C47 177.34(19) . . ? C28 Ni2 C47 89.69(17) . . ? C37 Ni2 C47 89.33(18) . . ? C1 N1 C3 110.9(3) . . ? C1 N1 C4 123.5(4) . . ? C3 N1 C4 125.4(3) . . ? C1 N2 C2 111.5(3) . . ? C1 N2 C7 122.9(3) . . ? C2 N2 C7 125.5(3) . . ? C10 N3 C11 111.0(3) . . ? C10 N3 C16 124.6(4) . . ? C11 N3 C16 124.2(3) . . ? C10 N4 C12 111.3(3) . . ? C10 N4 C13 123.2(3) . . ? C12 N4 C13 124.7(4) . . ? C28 N6 C30 111.2(4) . . ? C28 N6 C31 123.0(4) . . ? C30 N6 C31 125.8(4) . . ? C28 N7 C29 111.5(4) . . ? C28 N7 C34 123.0(3) . . ? C29 N7 C34 125.4(4) . . ? C37 N8 C39 111.5(3) . . ? C37 N8 C43 123.5(3) . . ? C39 N8 C43 124.8(4) . . ? C37 N9 C38 111.0(3) . . ? C37 N9 C40 124.1(4) . . ? C38 N9 C40 124.7(3) . . ? N2 C1 N1 103.8(3) . . ? N2 C1 Ni1 127.8(3) . . ? N1 C1 Ni1 128.1(3) . . ? C3 C2 N2 107.3(4) . . ? C2 C3 N1 106.4(4) . . ? N1 C4 C5 110.4(4) . . ? N1 C4 C6 109.8(4) . . ? C5 C4 C6 113.0(5) . . ? N2 C7 C9 110.0(4) . . ? N2 C7 C8 110.5(4) . . ? C9 C7 C8 114.0(4) . . ? N4 C10 N3 103.8(4) . . ? N4 C10 Ni1 125.7(3) . . ? N3 C10 Ni1 130.1(3) . . ? C12 C11 N3 107.4(4) . . ? C11 C12 N4 106.5(4) . . ? N4 C13 C15 109.5(3) . . ? N4 C13 C14 110.8(4) . . ? C15 C13 C14 113.4(4) . . ? N3 C16 C18 109.2(4) . . ? N3 C16 C17 109.1(4) . . ? C18 C16 C17 113.0(4) . . ? N5 C19 Ni1 174.9(4) . . ? C25 C20 C21 114.1(4) . . ? C25 C20 Ni1 124.0(3) . . ? C21 C20 Ni1 121.7(3) . . ? O1 C21 C22 121.4(4) . . ? O1 C21 C20 115.1(4) . . ? C22 C21 C20 123.5(4) . . ? C23 C22 C21 119.3(4) . . ? C24 C23 O2 124.9(4) . . ? C24 C23 C22 120.7(4) . . ? O2 C23 C22 114.5(4) . . ? C23 C24 C25 118.7(4) . . ? C20 C25 C24 123.7(4) . . ? N7 C28 N6 103.6(3) . . ? N7 C28 Ni2 129.2(3) . . ? N6 C28 Ni2 127.1(3) . . ? C30 C29 N7 106.2(4) . . ? C29 C30 N6 107.5(4) . . ? N6 C31 C33 110.1(4) . . ? N6 C31 C32 110.0(4) . . ? C33 C31 C32 112.5(4) . . ? N7 C34 C35 110.4(4) . . ? N7 C34 C36 111.7(4) . . ? C35 C34 C36 111.1(4) . . ? N8 C37 N9 103.6(3) . . ? N8 C37 Ni2 128.2(3) . . ? N9 C37 Ni2 128.2(3) . . ? C39 C38 N9 107.3(4) . . ? C38 C39 N8 106.6(4) . . ? N9 C40 C42 111.5(4) . . ? N9 C40 C41 109.8(4) . . ? C42 C40 C41 111.9(4) . . ? N8 C43 C55 110.6(4) . . ? N8 C43 C45 109.3(4) . . ? C55 C43 C45 112.5(6) . . ? N10 C46 Ni2 176.0(5) . . ? C52 C47 C48 113.8(4) . . ? C52 C47 Ni2 124.0(3) . . ? C48 C47 Ni2 122.1(3) . . ? O3 C48 C49 120.5(4) . . ? O3 C48 C47 115.6(4) . . ? C49 C48 C47 123.9(4) . . ? C50 C49 C48 118.7(4) . . ? O4 C50 C51 116.9(4) . . ? O4 C50 C49 123.5(4) . . ? C51 C50 C49 119.5(4) . . ? C52 C51 C50 119.7(4) . . ? C51 C52 C47 124.2(4) . . ? C21 O1 C27 117.2(3) . . ? C23 O2 C26 117.0(4) . . ? C48 O3 C54 117.5(3) . . ? C50 O4 C53 117.2(3) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.457 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.118 _chemical_name_common (iPr2Im)2(CN)(2,4-Dimethoxyphenyl)Ni(ii) data_compound_9 _database_code_depnum_ccdc_archive 'CCDC 637877' # Local code NiImiPr2_CN_2Pyridyl _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)(2-Pyridyl)Ni(II) ; _chemical_formula_sum 'C27.50 H37 N6 Ni' _chemical_formula_weight 510.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9864(18) _cell_length_b 9.6288(19) _cell_length_c 16.850(3) _cell_angle_alpha 104.83(3) _cell_angle_beta 92.53(3) _cell_angle_gamma 92.19(3) _cell_volume 1406.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_reflns_number 12961 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5081 _reflns_number_gt 4238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.5916P] 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 5081 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni -0.09621(3) 0.34037(3) 0.242206(16) 0.02172(11) Uani 1 d . . . N1 N 0.1975(2) 0.4725(2) 0.31192(11) 0.0262(4) Uani 1 d . . . N2 N 0.1110(2) 0.3317(2) 0.38127(11) 0.0250(4) Uani 1 d . . . N3 N -0.2837(2) 0.3570(2) 0.09893(11) 0.0279(4) Uani 1 d . . . N4 N -0.3750(2) 0.1997(2) 0.15608(12) 0.0287(4) Uani 1 d . . . N5 N -0.2925(3) 0.5341(3) 0.36435(15) 0.0521(7) Uani 1 d . . . N6 N 0.0782(2) 0.2456(2) 0.10320(12) 0.0285(4) Uani 1 d . . . H6 H 0.0733 0.3335 0.0989 0.034 Uiso 1 calc R . . C1 C 0.0788(2) 0.3822(2) 0.31445(12) 0.0236(5) Uani 1 d . . . C2 C 0.2999(3) 0.4790(3) 0.37663(14) 0.0311(5) Uani 1 d . . . H2 H 0.3903 0.5346 0.3881 0.037 Uiso 1 calc R . . C3 C 0.2463(3) 0.3911(3) 0.42004(14) 0.0307(5) Uani 1 d . . . H3 H 0.2918 0.3734 0.4676 0.037 Uiso 1 calc R . . C4 C 0.2073(3) 0.5590(3) 0.25149(14) 0.0327(5) Uani 1 d . . . H4 H 0.1383 0.5130 0.2037 0.039 Uiso 1 calc R . . C5 C 0.1555(5) 0.7092(4) 0.2890(2) 0.0628(10) Uani 1 d . . . H5A H 0.0549 0.7022 0.3067 0.094 Uiso 1 calc R . . H5B H 0.1569 0.7644 0.2483 0.094 Uiso 1 calc R . . H5C H 0.2218 0.7567 0.3359 0.094 Uiso 1 calc R . . C6 C 0.3637(4) 0.5618(4) 0.2210(2) 0.0553(8) Uani 1 d . . . H6A H 0.4330 0.6096 0.2665 0.083 Uiso 1 calc R . . H6B H 0.3656 0.6136 0.1787 0.083 Uiso 1 calc R . . H6C H 0.3926 0.4641 0.1985 0.083 Uiso 1 calc R . . C7 C 0.0170(3) 0.2245(3) 0.40738(14) 0.0304(5) Uani 1 d . . . H7 H -0.0735 0.2016 0.3699 0.036 Uiso 1 calc R . . C8 C -0.0321(4) 0.2856(4) 0.49435(18) 0.0534(8) Uani 1 d . . . H8A H 0.0551 0.3142 0.5319 0.080 Uiso 1 calc R . . H8B H -0.0920 0.2128 0.5108 0.080 Uiso 1 calc R . . H8C H -0.0908 0.3686 0.4957 0.080 Uiso 1 calc R . . C9 C 0.0992(4) 0.0865(3) 0.3993(2) 0.0487(7) Uani 1 d . . . H9A H 0.1321 0.0536 0.3439 0.073 Uiso 1 calc R . . H9B H 0.0328 0.0131 0.4109 0.073 Uiso 1 calc R . . H9C H 0.1851 0.1048 0.4382 0.073 Uiso 1 calc R . . C10 C -0.2588(2) 0.2967(2) 0.16280(13) 0.0235(5) Uani 1 d . . . C11 C -0.4146(3) 0.2980(3) 0.05389(16) 0.0393(6) Uani 1 d . . . H11 H -0.4559 0.3225 0.0074 0.047 Uiso 1 calc R . . C12 C -0.4704(3) 0.2000(3) 0.08930(16) 0.0395(6) Uani 1 d . . . H12 H -0.5583 0.1419 0.0721 0.047 Uiso 1 calc R . . C13 C -0.4011(3) 0.1110(3) 0.21434(16) 0.0343(6) Uani 1 d . . . H13 H -0.3139 0.1264 0.2542 0.041 Uiso 1 calc R . . C14 C -0.4138(5) -0.0467(4) 0.1682(2) 0.0655(10) Uani 1 d . . . H14A H -0.4996 -0.0642 0.1293 0.098 Uiso 1 calc R . . H14B H -0.4257 -0.1050 0.2069 0.098 Uiso 1 calc R . . H14C H -0.3241 -0.0718 0.1388 0.098 Uiso 1 calc R . . C15 C -0.5388(4) 0.1573(4) 0.2618(2) 0.0589(9) Uani 1 d . . . H15A H -0.5255 0.2580 0.2911 0.088 Uiso 1 calc R . . H15B H -0.5531 0.0998 0.3007 0.088 Uiso 1 calc R . . H15C H -0.6255 0.1434 0.2237 0.088 Uiso 1 calc R . . C16 C -0.1897(3) 0.4762(3) 0.08530(15) 0.0338(6) Uani 1 d . . . H16 H -0.0853 0.4633 0.1023 0.041 Uiso 1 calc R . . C17 C -0.2374(4) 0.6190(3) 0.13872(19) 0.0516(8) Uani 1 d . . . H17A H -0.3381 0.6358 0.1214 0.077 Uiso 1 calc R . . H17B H -0.1700 0.6964 0.1329 0.077 Uiso 1 calc R . . H17C H -0.2346 0.6155 0.1958 0.077 Uiso 1 calc R . . C18 C -0.1956(4) 0.4756(4) -0.00529(18) 0.0521(8) Uani 1 d . . . H18A H -0.1678 0.3827 -0.0378 0.078 Uiso 1 calc R . . H18B H -0.1267 0.5502 -0.0133 0.078 Uiso 1 calc R . . H18C H -0.2959 0.4935 -0.0224 0.078 Uiso 1 calc R . . C19 C -0.2153(3) 0.4634(3) 0.31951(14) 0.0323(6) Uani 1 d . . . C20 C 0.0126(2) 0.2057(3) 0.16507(13) 0.0249(5) Uani 1 d . . . C21 C 0.0230(3) 0.0632(3) 0.17103(15) 0.0340(6) Uani 1 d . . . H21 H -0.0221 0.0342 0.2139 0.041 Uiso 1 calc R . . C22 C 0.0994(3) -0.0349(3) 0.11411(17) 0.0397(6) Uani 1 d . . . H22 H 0.1066 -0.1299 0.1183 0.048 Uiso 1 calc R . . C23 C 0.1653(3) 0.0089(3) 0.05083(16) 0.0382(6) Uani 1 d . . . H23 H 0.2174 -0.0552 0.0113 0.046 Uiso 1 calc R . . C24 C 0.1514(3) 0.1490(3) 0.04819(15) 0.0337(6) Uani 1 d . . . H24 H 0.1955 0.1794 0.0055 0.040 Uiso 1 calc R . . C26 C 0.5293(12) 0.8544(8) 0.4656(7) 0.171(5) Uani 1 d . . . C27 C 0.5999(10) 0.9694(10) 0.4403(5) 0.161(4) Uani 1 d . . . C25 C 0.4323(10) 0.8830(8) 0.5238(6) 0.178(5) Uani 1 d . . . C28 C 0.6859(11) 0.9377(13) 0.3905(6) 0.083(3) Uani 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02087(16) 0.02271(18) 0.02054(15) 0.00352(10) 0.00025(10) 0.00338(10) N1 0.0255(10) 0.0272(12) 0.0243(9) 0.0040(8) -0.0002(7) 0.0007(8) N2 0.0255(10) 0.0258(12) 0.0235(9) 0.0062(7) -0.0013(7) 0.0016(8) N3 0.0244(10) 0.0328(13) 0.0259(9) 0.0062(8) -0.0015(7) 0.0080(8) N4 0.0230(10) 0.0274(12) 0.0339(10) 0.0049(8) 0.0000(8) 0.0020(8) N5 0.0437(14) 0.0631(19) 0.0400(13) -0.0063(12) 0.0034(11) 0.0194(12) N6 0.0269(10) 0.0258(12) 0.0321(10) 0.0055(8) 0.0028(8) 0.0031(8) C1 0.0261(11) 0.0218(13) 0.0207(10) 0.0005(8) 0.0032(8) 0.0059(9) C2 0.0264(12) 0.0345(15) 0.0287(12) 0.0023(10) -0.0022(9) -0.0022(10) C3 0.0293(12) 0.0358(15) 0.0251(11) 0.0054(10) -0.0053(9) 0.0041(10) C4 0.0393(14) 0.0318(15) 0.0271(11) 0.0088(10) -0.0003(10) -0.0031(10) C5 0.100(3) 0.041(2) 0.0559(19) 0.0226(15) 0.0187(19) 0.0185(18) C6 0.0483(18) 0.075(3) 0.0488(17) 0.0263(16) 0.0136(14) -0.0037(16) C7 0.0340(13) 0.0291(15) 0.0287(12) 0.0095(10) -0.0002(10) -0.0009(10) C8 0.067(2) 0.050(2) 0.0412(16) 0.0062(13) 0.0217(14) -0.0085(15) C9 0.0555(19) 0.0369(19) 0.0578(18) 0.0196(13) 0.0011(14) 0.0072(13) C10 0.0235(11) 0.0220(13) 0.0244(10) 0.0036(8) 0.0056(8) 0.0064(9) C11 0.0311(14) 0.0508(19) 0.0340(13) 0.0082(12) -0.0104(10) 0.0086(12) C12 0.0248(13) 0.0457(18) 0.0426(14) 0.0038(12) -0.0098(11) -0.0016(11) C13 0.0303(13) 0.0295(15) 0.0441(14) 0.0110(11) 0.0038(11) 0.0013(10) C14 0.090(3) 0.032(2) 0.074(2) 0.0095(16) 0.020(2) 0.0019(17) C15 0.057(2) 0.066(2) 0.063(2) 0.0259(17) 0.0292(17) 0.0173(17) C16 0.0293(13) 0.0378(16) 0.0393(13) 0.0176(11) 0.0048(10) 0.0077(10) C17 0.067(2) 0.0345(19) 0.0551(18) 0.0131(13) 0.0122(15) 0.0040(14) C18 0.059(2) 0.061(2) 0.0454(16) 0.0278(15) 0.0132(14) 0.0157(16) C19 0.0292(13) 0.0370(16) 0.0276(12) 0.0031(10) -0.0034(10) 0.0054(10) C20 0.0198(11) 0.0281(14) 0.0243(10) 0.0032(9) -0.0041(8) 0.0032(9) C21 0.0388(14) 0.0300(16) 0.0325(12) 0.0063(10) 0.0007(10) 0.0051(10) C22 0.0427(15) 0.0253(15) 0.0476(15) 0.0034(11) -0.0047(12) 0.0085(11) C23 0.0264(13) 0.0382(17) 0.0405(14) -0.0078(11) 0.0000(10) 0.0094(10) C24 0.0235(12) 0.0451(17) 0.0290(12) 0.0030(10) 0.0033(9) 0.0025(10) C26 0.167(8) 0.078(5) 0.215(9) -0.040(5) -0.156(7) 0.045(5) C27 0.133(7) 0.136(7) 0.163(7) -0.043(6) -0.114(6) 0.065(6) C25 0.167(8) 0.087(5) 0.222(9) -0.047(6) -0.144(7) 0.060(5) C28 0.077(6) 0.103(8) 0.079(6) 0.046(5) -0.001(5) -0.012(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 Ni C10 1.896(2) . ? Ni C1 1.911(2) . ? Ni C20 1.916(2) . ? Ni C19 1.917(3) . ? N1 C1 1.359(3) . ? N1 C2 1.383(3) . ? N1 C4 1.474(3) . ? N2 C1 1.360(3) . ? N2 C3 1.385(3) . ? N2 C7 1.473(3) . ? N3 C10 1.361(3) . ? N3 C11 1.390(3) . ? N3 C16 1.471(3) . ? N4 C10 1.355(3) . ? N4 C12 1.385(3) . ? N4 C13 1.478(3) . ? N5 C19 1.156(3) . ? N6 C24 1.348(3) . ? N6 C20 1.351(3) . ? N6 H6 0.8700 . ? C2 C3 1.341(4) . ? C2 H2 0.9400 . ? C3 H3 0.9400 . ? C4 C6 1.519(4) . ? C4 C5 1.523(4) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C9 1.524(4) . ? C7 C8 1.525(4) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C11 C12 1.333(4) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.516(4) . ? C13 C15 1.521(4) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.523(4) . ? C16 C17 1.526(4) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C20 C21 1.408(4) . ? C21 C22 1.388(4) . ? C21 H21 0.9400 . ? C22 C23 1.390(4) . ? C22 H22 0.9400 . ? C23 C24 1.372(4) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C26 C25 1.324(17) . ? C26 C27 1.422(15) . ? C27 C28 1.157(12) . ? C27 C25 1.441(8) 2_676 ? C25 C27 1.441(8) 2_676 ? 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 C10 Ni C1 175.01(9) . . ? C10 Ni C20 87.02(9) . . ? C1 Ni C20 88.87(9) . . ? C10 Ni C19 90.98(10) . . ? C1 Ni C19 93.30(10) . . ? C20 Ni C19 175.74(11) . . ? C1 N1 C2 110.7(2) . . ? C1 N1 C4 123.6(2) . . ? C2 N1 C4 125.6(2) . . ? C1 N2 C3 110.9(2) . . ? C1 N2 C7 124.58(19) . . ? C3 N2 C7 124.5(2) . . ? C10 N3 C11 110.5(2) . . ? C10 N3 C16 123.5(2) . . ? C11 N3 C16 125.8(2) . . ? C10 N4 C12 110.8(2) . . ? C10 N4 C13 124.8(2) . . ? C12 N4 C13 124.3(2) . . ? C24 N6 C20 119.8(2) . . ? C24 N6 H6 120.1 . . ? C20 N6 H6 120.1 . . ? N1 C1 N2 104.44(19) . . ? N1 C1 Ni 127.66(17) . . ? N2 C1 Ni 127.88(18) . . ? C3 C2 N1 107.3(2) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 106.7(2) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N1 C4 C6 111.1(2) . . ? N1 C4 C5 109.5(2) . . ? C6 C4 C5 112.4(3) . . ? N1 C4 H4 107.9 . . ? C6 C4 H4 107.9 . . ? C5 C4 H4 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C9 110.0(2) . . ? N2 C7 C8 110.8(2) . . ? C9 C7 C8 112.2(2) . . ? N2 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 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 . . ? N4 C10 N3 104.5(2) . . ? N4 C10 Ni 128.52(18) . . ? N3 C10 Ni 126.97(18) . . ? C12 C11 N3 106.9(2) . . ? C12 C11 H11 126.6 . . ? N3 C11 H11 126.6 . . ? C11 C12 N4 107.3(2) . . ? C11 C12 H12 126.4 . . ? N4 C12 H12 126.4 . . ? N4 C13 C14 109.6(2) . . ? N4 C13 C15 110.4(2) . . ? C14 C13 C15 112.1(3) . . ? N4 C13 H13 108.2 . . ? C14 C13 H13 108.2 . . ? C15 C13 H13 108.2 . . ? 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 . . ? N3 C16 C18 111.1(2) . . ? N3 C16 C17 109.8(2) . . ? C18 C16 C17 111.3(2) . . ? N3 C16 H16 108.2 . . ? C18 C16 H16 108.2 . . ? C17 C16 H16 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 Ni 177.0(2) . . ? N6 C20 C21 119.0(2) . . ? N6 C20 Ni 120.38(18) . . ? C21 C20 Ni 120.61(18) . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.3(3) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 117.6(2) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? N6 C24 C23 123.8(2) . . ? N6 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? C25 C26 C27 119.5(7) . . ? C28 C27 C26 116.2(11) . . ? C28 C27 C25 122.2(15) . 2_676 ? C26 C27 C25 121.6(11) . 2_676 ? C26 C25 C27 118.9(11) . 2_676 ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.733 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.060 _chemical_name_common (iPr2Im)2(CN)(2-Pyridyl)Ni(ii) data_compound_11 _database_code_depnum_ccdc_archive 'CCDC 637878' # Local code NiImiPr2_CN_SiMe3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)(SiMe3)Ni(II) ; _chemical_formula_sum 'C29 H49 N5 Ni Si' _chemical_formula_weight 554.53 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' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8825(12) _cell_length_b 9.7080(5) _cell_length_c 23.203(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.665(10) _cell_angle_gamma 90.00 _cell_volume 3243.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6213 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.95 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_reflns_number 14855 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5543 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5543 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.52733(3) 0.19051(5) 0.837706(19) 0.02711(13) Uani 1 d . . . Si Si 0.63842(7) 0.33793(11) 0.82361(5) 0.0342(3) Uani 1 d . . . C1 C 0.4532(2) 0.2449(4) 0.76273(15) 0.0280(8) Uani 1 d . . . C2 C 0.3758(3) 0.2342(5) 0.66548(17) 0.0462(12) Uani 1 d . . . H2 H 0.3582 0.2056 0.6255 0.055 Uiso 1 calc R . . C3 C 0.3362(3) 0.3332(5) 0.68984(18) 0.0464(11) Uani 1 d . . . H3 H 0.2852 0.3876 0.6704 0.056 Uiso 1 calc R . . C4 C 0.3650(3) 0.4370(4) 0.79413(18) 0.0418(10) Uani 1 d . . . H4 H 0.4196 0.4379 0.8289 0.050 Uiso 1 calc R . . C5 C 0.2830(4) 0.3899(7) 0.8146(3) 0.0884(19) Uani 1 d . . . H5A H 0.2287 0.3881 0.7811 0.133 Uiso 1 calc R . . H5B H 0.2724 0.4526 0.8447 0.133 Uiso 1 calc R . . H5C H 0.2946 0.2981 0.8314 0.133 Uiso 1 calc R . . C6 C 0.3507(4) 0.5825(5) 0.7687(3) 0.0719(16) Uani 1 d . . . H6A H 0.4025 0.6074 0.7525 0.108 Uiso 1 calc R . . H6B H 0.3469 0.6466 0.8001 0.108 Uiso 1 calc R . . H6C H 0.2935 0.5860 0.7374 0.108 Uiso 1 calc R . . C7 C 0.5126(3) 0.0689(4) 0.70332(18) 0.0411(10) Uani 1 d . . . H7 H 0.5678 0.0750 0.7375 0.049 Uiso 1 calc R . . C8 C 0.4692(3) -0.0701(5) 0.7057(2) 0.0633(14) Uani 1 d . . . H8A H 0.4496 -0.0783 0.7424 0.095 Uiso 1 calc R . . H8B H 0.5143 -0.1415 0.7044 0.095 Uiso 1 calc R . . H8C H 0.4158 -0.0803 0.6719 0.095 Uiso 1 calc R . . C9 C 0.5451(3) 0.0883(6) 0.6473(2) 0.0722(15) Uani 1 d . . . H9A H 0.4933 0.0743 0.6127 0.108 Uiso 1 calc R . . H9B H 0.5936 0.0221 0.6466 0.108 Uiso 1 calc R . . H9C H 0.5692 0.1809 0.6464 0.108 Uiso 1 calc R . . C10 C 0.6109(2) 0.1321(4) 0.90940(15) 0.0296(8) Uani 1 d . . . C11 C 0.7138(3) -0.0007(5) 0.97368(19) 0.0487(12) Uani 1 d . . . H11 H 0.7580 -0.0698 0.9882 0.058 Uiso 1 calc R . . C12 C 0.6809(3) 0.0884(5) 1.00649(18) 0.0465(11) Uani 1 d . . . H12 H 0.6966 0.0942 1.0483 0.056 Uiso 1 calc R . . C13 C 0.5593(3) 0.2761(4) 0.98381(17) 0.0415(10) Uani 1 d . . . H13 H 0.5351 0.3358 0.9488 0.050 Uiso 1 calc R . . C14 C 0.4774(3) 0.2098(5) 0.9997(2) 0.0577(12) Uani 1 d . . . H14A H 0.4442 0.1528 0.9668 0.087 Uiso 1 calc R . . H14B H 0.4362 0.2807 1.0076 0.087 Uiso 1 calc R . . H14C H 0.4990 0.1531 1.0349 0.087 Uiso 1 calc R . . C15 C 0.6147(4) 0.3673(5) 1.0343(2) 0.0698(15) Uani 1 d . . . H15A H 0.6309 0.3147 1.0710 0.105 Uiso 1 calc R . . H15B H 0.5773 0.4461 1.0393 0.105 Uiso 1 calc R . . H15C H 0.6709 0.3989 1.0246 0.105 Uiso 1 calc R . . C16 C 0.6783(3) -0.0634(5) 0.86424(19) 0.0504(11) Uani 1 d . . . H16 H 0.6579 -0.0082 0.8273 0.061 Uiso 1 calc R . . C17 C 0.6111(4) -0.1840(5) 0.8594(2) 0.0768(16) Uani 1 d . . . H17A H 0.6295 -0.2407 0.8948 0.115 Uiso 1 calc R . . H17B H 0.6122 -0.2388 0.8246 0.115 Uiso 1 calc R . . H17C H 0.5488 -0.1491 0.8556 0.115 Uiso 1 calc R . . C18 C 0.7773(4) -0.1103(6) 0.8687(3) 0.0806(17) Uani 1 d . . . H18A H 0.8180 -0.0308 0.8742 0.121 Uiso 1 calc R . . H18B H 0.7798 -0.1579 0.8324 0.121 Uiso 1 calc R . . H18C H 0.7972 -0.1722 0.9023 0.121 Uiso 1 calc R . . C19 C 0.4295(3) 0.0719(4) 0.85016(17) 0.0400(10) Uani 1 d . . . C20 C 0.7410(3) 0.2513(5) 0.8046(2) 0.0630(14) Uani 1 d . . . H20A H 0.7193 0.1935 0.7698 0.094 Uiso 1 calc R . . H20B H 0.7735 0.1951 0.8380 0.094 Uiso 1 calc R . . H20C H 0.7828 0.3209 0.7964 0.094 Uiso 1 calc R . . C21 C 0.6021(3) 0.4694(5) 0.7621(2) 0.0549(12) Uani 1 d . . . H21A H 0.6558 0.5224 0.7589 0.082 Uiso 1 calc R . . H21B H 0.5561 0.5307 0.7712 0.082 Uiso 1 calc R . . H21C H 0.5757 0.4227 0.7247 0.082 Uiso 1 calc R . . C22 C 0.6921(3) 0.4448(5) 0.8920(2) 0.0589(13) Uani 1 d . . . H22A H 0.7344 0.5118 0.8823 0.088 Uiso 1 calc R . . H22B H 0.7260 0.3850 0.9236 0.088 Uiso 1 calc R . . H22C H 0.6435 0.4924 0.9051 0.088 Uiso 1 calc R . . C23 C 1.0647(7) 0.7726(15) 1.0148(6) 0.208(6) Uani 1 d . . . H23A H 1.1142 0.8185 1.0436 0.311 Uiso 1 calc R . . H23B H 1.0512 0.8230 0.9775 0.311 Uiso 1 calc R . . H23C H 1.0839 0.6796 1.0082 0.311 Uiso 1 calc R . . C24 C 0.9790(6) 0.7672(9) 1.0379(4) 0.109(3) Uani 1 d . . . C25 C 0.9135(6) 0.6734(8) 1.0144(3) 0.110(3) Uani 1 d . . . H25 H 0.9239 0.6128 0.9852 0.132 Uiso 1 calc R . . C26 C 0.8341(8) 0.6631(12) 1.0310(5) 0.135(4) Uani 1 d . . . H26 H 0.7896 0.5959 1.0145 0.162 Uiso 1 calc R . . C27 C 0.8198(9) 0.755(2) 1.0735(6) 0.193(8) Uani 1 d . . . H27 H 0.7646 0.7507 1.0861 0.231 Uiso 1 calc R . . C28 C 0.8882(13) 0.8559(15) 1.0982(5) 0.182(8) Uani 1 d . . . H28 H 0.8795 0.9197 1.1268 0.219 Uiso 1 calc R . . C29 C 0.9665(10) 0.8553(11) 1.0784(4) 0.157(6) Uani 1 d . . . H29 H 1.0134 0.9198 1.0941 0.188 Uiso 1 calc R . . N1 N 0.38424(19) 0.3415(3) 0.74973(13) 0.0333(8) Uani 1 d . . . N2 N 0.44824(18) 0.1804(3) 0.70992(13) 0.0354(8) Uani 1 d . . . N3 N 0.6185(2) 0.1714(3) 0.96670(13) 0.0349(8) Uani 1 d . . . N4 N 0.6720(2) 0.0255(3) 0.91442(14) 0.0381(8) Uani 1 d . . . N5 N 0.3708(3) 0.0016(4) 0.85747(16) 0.0633(12) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0278(2) 0.0279(3) 0.0254(2) -0.0010(2) 0.00635(17) -0.0010(2) Si 0.0336(5) 0.0320(7) 0.0383(6) 0.0005(4) 0.0115(5) -0.0042(4) C1 0.0270(17) 0.033(2) 0.0262(19) -0.0062(15) 0.0103(15) -0.0050(14) C2 0.038(2) 0.068(3) 0.027(2) -0.0034(19) -0.0020(18) 0.0020(19) C3 0.036(2) 0.058(3) 0.041(2) 0.003(2) 0.0004(19) 0.0083(19) C4 0.041(2) 0.043(3) 0.042(2) -0.0079(19) 0.0116(19) 0.0064(18) C5 0.096(4) 0.081(4) 0.117(5) -0.035(4) 0.080(4) -0.020(3) C6 0.085(3) 0.048(4) 0.087(4) 0.002(3) 0.029(3) 0.021(3) C7 0.0341(19) 0.054(3) 0.036(2) -0.0162(18) 0.0095(17) 0.0026(18) C8 0.061(3) 0.058(4) 0.074(3) -0.022(3) 0.022(3) 0.004(2) C9 0.067(3) 0.092(4) 0.071(3) -0.015(3) 0.042(3) 0.004(3) C10 0.0284(17) 0.033(2) 0.0297(19) -0.0012(15) 0.0110(15) -0.0057(15) C11 0.047(2) 0.055(3) 0.043(2) 0.018(2) 0.008(2) 0.013(2) C12 0.051(2) 0.053(3) 0.030(2) 0.0102(19) 0.000(2) 0.004(2) C13 0.051(2) 0.041(3) 0.035(2) -0.0042(17) 0.0148(18) 0.0043(18) C14 0.056(2) 0.065(4) 0.062(3) -0.007(2) 0.032(2) 0.003(2) C15 0.094(4) 0.066(4) 0.051(3) -0.032(2) 0.021(3) -0.012(3) C16 0.069(3) 0.044(3) 0.043(2) 0.0072(19) 0.024(2) 0.021(2) C17 0.121(4) 0.039(3) 0.073(3) -0.015(3) 0.031(3) 0.005(3) C18 0.089(4) 0.090(4) 0.076(4) 0.016(3) 0.045(3) 0.049(3) C19 0.036(2) 0.052(3) 0.030(2) 0.0010(18) 0.0052(17) -0.0100(19) C20 0.046(2) 0.062(3) 0.092(4) 0.003(3) 0.037(3) -0.007(2) C21 0.058(3) 0.048(3) 0.063(3) 0.013(2) 0.023(2) -0.011(2) C22 0.070(3) 0.047(3) 0.059(3) -0.008(2) 0.015(3) -0.025(2) C23 0.140(8) 0.300(17) 0.184(11) 0.053(11) 0.043(9) -0.003(9) C24 0.105(6) 0.115(7) 0.092(5) 0.019(5) -0.004(5) -0.008(5) C25 0.132(6) 0.098(6) 0.079(5) 0.029(4) -0.013(5) -0.003(5) C26 0.136(8) 0.147(10) 0.114(8) 0.075(7) 0.014(7) -0.011(7) C27 0.159(10) 0.30(2) 0.131(11) 0.165(13) 0.052(9) 0.093(12) C28 0.29(2) 0.177(13) 0.060(5) 0.028(6) 0.016(9) 0.142(13) C29 0.246(14) 0.115(8) 0.078(6) -0.022(5) -0.016(8) 0.058(8) N1 0.0298(14) 0.038(2) 0.0299(16) -0.0007(13) 0.0035(13) 0.0051(12) N2 0.0285(14) 0.045(2) 0.0313(16) -0.0066(15) 0.0052(13) 0.0000(14) N3 0.0394(16) 0.037(2) 0.0276(16) -0.0013(14) 0.0069(13) -0.0026(14) N4 0.0407(17) 0.036(2) 0.0361(17) 0.0038(14) 0.0076(15) 0.0094(14) N5 0.055(2) 0.086(3) 0.045(2) 0.005(2) 0.0058(19) -0.033(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni C1 1.884(3) . ? Ni C10 1.895(3) . ? Ni C19 1.934(4) . ? Ni Si 2.2722(12) . ? Si C21 1.888(4) . ? Si C20 1.890(5) . ? Si C22 1.895(4) . ? C1 N2 1.361(5) . ? C1 N1 1.367(5) . ? C2 C3 1.327(6) . ? C2 N2 1.391(4) . ? C2 H2 0.9400 . ? C3 N1 1.395(5) . ? C3 H3 0.9400 . ? C4 N1 1.467(5) . ? C4 C5 1.489(7) . ? C4 C6 1.524(7) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 N2 1.478(5) . ? C7 C8 1.503(6) . ? C7 C9 1.510(7) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 N3 1.361(5) . ? C10 N4 1.362(5) . ? C11 C12 1.326(6) . ? C11 N4 1.382(5) . ? C11 H11 0.9400 . ? C12 N3 1.390(4) . ? C12 H12 0.9400 . ? C13 N3 1.464(5) . ? C13 C14 1.504(6) . ? C13 C15 1.532(5) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 N4 1.472(6) . ? C16 C18 1.520(6) . ? C16 C17 1.525(7) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 N5 1.154(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.506(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.318(13) . ? C24 C25 1.344(10) . ? C25 C26 1.336(13) . ? C25 H25 0.9400 . ? C26 C27 1.385(18) . ? C26 H26 0.9400 . ? C27 C28 1.424(18) . ? C27 H27 0.9400 . ? C28 C29 1.357(18) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni C10 174.51(17) . . ? C1 Ni C19 91.02(15) . . ? C10 Ni C19 92.44(15) . . ? C1 Ni Si 88.16(11) . . ? C10 Ni Si 88.56(11) . . ? C19 Ni Si 177.48(14) . . ? C21 Si C20 102.6(2) . . ? C21 Si C22 104.0(2) . . ? C20 Si C22 104.1(2) . . ? C21 Si Ni 117.05(14) . . ? C20 Si Ni 114.42(16) . . ? C22 Si Ni 113.11(17) . . ? N2 C1 N1 104.5(3) . . ? N2 C1 Ni 126.0(3) . . ? N1 C1 Ni 128.9(3) . . ? C3 C2 N2 107.5(3) . . ? C3 C2 H2 126.2 . . ? N2 C2 H2 126.2 . . ? C2 C3 N1 107.1(3) . . ? C2 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? N1 C4 C5 110.6(4) . . ? N1 C4 C6 110.3(4) . . ? C5 C4 C6 111.2(4) . . ? N1 C4 H4 108.2 . . ? C5 C4 H4 108.2 . . ? C6 C4 H4 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 111.0(3) . . ? N2 C7 C9 110.8(4) . . ? C8 C7 C9 112.2(4) . . ? N2 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 . . ? N3 C10 N4 104.0(3) . . ? N3 C10 Ni 130.3(3) . . ? N4 C10 Ni 125.3(3) . . ? C12 C11 N4 108.2(3) . . ? C12 C11 H11 125.9 . . ? N4 C11 H11 125.9 . . ? C11 C12 N3 106.2(3) . . ? C11 C12 H12 126.9 . . ? N3 C12 H12 126.9 . . ? N3 C13 C14 110.5(3) . . ? N3 C13 C15 111.4(3) . . ? C14 C13 C15 111.9(4) . . ? N3 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? 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 . . ? N4 C16 C18 112.2(4) . . ? N4 C16 C17 109.7(4) . . ? C18 C16 C17 112.4(4) . . ? N4 C16 H16 107.4 . . ? C18 C16 H16 107.4 . . ? C17 C16 H16 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 Ni 179.7(4) . . ? Si C20 H20A 109.5 . . ? Si C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si C21 H21A 109.5 . . ? Si C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si C22 H22A 109.5 . . ? Si C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 120.7(11) . . ? C29 C24 C23 121.1(11) . . ? C25 C24 C23 118.1(11) . . ? C26 C25 C24 122.5(10) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C27 117.6(12) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C26 C27 C28 120.4(15) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 116.6(14) . . ? C29 C28 H28 121.7 . . ? C27 C28 H28 121.7 . . ? C24 C29 C28 122.1(14) . . ? C24 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C1 N1 C3 110.3(3) . . ? C1 N1 C4 123.2(3) . . ? C3 N1 C4 126.4(3) . . ? C1 N2 C2 110.5(3) . . ? C1 N2 C7 122.7(3) . . ? C2 N2 C7 126.8(3) . . ? C10 N3 C12 111.2(3) . . ? C10 N3 C13 123.6(3) . . ? C12 N3 C13 124.7(3) . . ? C10 N4 C11 110.4(3) . . ? C10 N4 C16 123.6(3) . . ? C11 N4 C16 125.2(3) . . ? _diffrn_measured_fraction_theta_max 0.822 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 0.496 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.060 _chemical_name_common (iPr2Im)2(CN)(SiMe3)Ni(ii) data_compound_14 _database_code_depnum_ccdc_archive 'CCDC 637879' # Local code NiImiPr2CN2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)2Ni(II) ; _chemical_formula_sum 'C26 H38 N6 Ni' _chemical_formula_weight 493.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.3397(6) _cell_length_b 13.1546(6) _cell_length_c 9.3845(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.118(9) _cell_angle_gamma 90.00 _cell_volume 1385.85(14) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.9 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7030 _exptl_absorpt_correction_T_max 0.8230 _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 8313 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.95 _reflns_number_total 1394 _reflns_number_gt 1363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.9962P] 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_number_reflns 1394 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.0000 0.0000 0.02816(15) Uani 1 d S . . N1 N -0.06647(12) 0.20768(11) -0.09344(15) 0.0332(3) Uani 1 d . . . N2 N -0.2376(3) 0.0000 0.1118(5) 0.0921(12) Uani 1 d S . . C1 C 0.0000 0.14446(17) 0.0000 0.0293(4) Uani 1 d S . . C2 C -0.04155(17) 0.30875(14) -0.0587(2) 0.0442(4) Uani 1 d . . . H2 H -0.0761 0.3661 -0.1077 0.053 Uiso 1 calc R . . C3 C -0.14713(15) 0.17208(15) -0.22020(18) 0.0371(4) Uani 1 d . . . H3 H -0.1675 0.1002 -0.2039 0.045 Uiso 1 calc R . . C4 C -0.26164(18) 0.2333(2) -0.2397(3) 0.0594(6) Uani 1 d . . . H4A H -0.2985 0.2294 -0.1526 0.089 Uiso 1 calc R . . H4B H -0.3157 0.2061 -0.3199 0.089 Uiso 1 calc R . . H4C H -0.2439 0.3037 -0.2589 0.089 Uiso 1 calc R . . C5 C -0.0842(2) 0.1766(2) -0.3522(2) 0.0687(7) Uani 1 d . . . H5A H -0.0641 0.2465 -0.3707 0.103 Uiso 1 calc R . . H5B H -0.1364 0.1499 -0.4346 0.103 Uiso 1 calc R . . H5C H -0.0120 0.1362 -0.3359 0.103 Uiso 1 calc R . . C11 C -0.1420(2) 0.0000 0.0833(3) 0.0448(6) Uani 1 d S . . C12 C -0.0816(4) 0.5000 -0.4044(5) 0.0725(10) Uani 1 d S . . H12 H -0.1368 0.5000 -0.3385 0.087 Uiso 1 calc SR . . C13 C 0.0390(5) 0.5000 -0.3567(4) 0.0823(12) Uani 1 d S . . H13 H 0.0662 0.5000 -0.2573 0.099 Uiso 1 calc SR . . C14 C 0.1193(4) 0.5000 -0.4515(5) 0.0743(10) Uani 1 d S . . H14 H 0.2013 0.5000 -0.4172 0.089 Uiso 1 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0290(2) 0.0267(2) 0.0295(2) 0.000 0.00642(15) 0.000 N1 0.0322(7) 0.0312(7) 0.0346(7) 0.0013(6) -0.0007(5) 0.0003(5) N2 0.0597(18) 0.0518(17) 0.175(4) 0.000 0.051(2) 0.000 C1 0.0250(10) 0.0341(11) 0.0291(10) 0.000 0.0050(8) 0.000 C2 0.0484(10) 0.0305(9) 0.0505(11) 0.0046(8) -0.0041(8) 0.0011(8) C3 0.0338(8) 0.0419(9) 0.0337(8) 0.0006(7) -0.0023(7) -0.0025(7) C4 0.0388(10) 0.0690(15) 0.0656(13) -0.0068(12) -0.0087(9) 0.0080(10) C5 0.0563(13) 0.110(2) 0.0400(11) -0.0120(12) 0.0075(9) -0.0127(13) C11 0.0479(15) 0.0311(12) 0.0600(17) 0.000 0.0240(13) 0.000 C12 0.093(3) 0.0499(19) 0.082(3) 0.000 0.038(2) 0.000 C13 0.123(4) 0.070(2) 0.0499(19) 0.000 -0.001(2) 0.000 C14 0.070(2) 0.056(2) 0.094(3) 0.000 0.003(2) 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 Ni C11 1.887(3) 5 ? Ni C11 1.887(3) . ? Ni C1 1.900(2) 5 ? Ni C1 1.900(2) . ? N1 C1 1.3572(19) . ? N1 C2 1.389(2) . ? N1 C3 1.471(2) . ? N2 C11 1.153(4) . ? C1 N1 1.3573(19) 2 ? C2 C2 1.344(4) 2 ? C3 C5 1.515(3) . ? C3 C4 1.517(3) . ? C12 C14 1.360(6) 5_564 ? C12 C13 1.378(6) . ? C13 C14 1.360(6) . ? C14 C12 1.360(6) 5_564 ? 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 C11 Ni C11 180.0 5 . ? C11 Ni C1 90.0 5 5 ? C11 Ni C1 90.0 . 5 ? C11 Ni C1 90.0 5 . ? C11 Ni C1 90.0 . . ? C1 Ni C1 180.0 5 . ? C1 N1 C2 111.03(14) . . ? C1 N1 C3 123.54(15) . . ? C2 N1 C3 125.28(15) . . ? N1 C1 N1 104.41(19) . 2 ? N1 C1 Ni 127.79(10) . . ? N1 C1 Ni 127.79(10) 2 . ? C2 C2 N1 106.76(9) 2 . ? N1 C3 C5 109.76(15) . . ? N1 C3 C4 110.62(15) . . ? C5 C3 C4 111.99(18) . . ? N2 C11 Ni 169.1(4) . . ? C14 C12 C13 118.8(4) 5_564 . ? C14 C13 C12 120.9(4) . . ? C12 C14 C13 120.3(4) 5_564 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.335 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.042 _chemical_name_common (iPr2Im)2(CN)2Ni(ii) data_compound_13 _database_code_depnum_ccdc_archive 'CCDC 637880' # Local code NiImiPr2_CN_C4H8CN _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(CN)(C4H8CN)Ni(II) benzene solvate ; _chemical_formula_sum 'C30 H46 N6 Ni' _chemical_formula_weight 549.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 31.961(4) _cell_length_b 10.228(2) _cell_length_c 23.529(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.61(2) _cell_angle_gamma 90.00 _cell_volume 6330(2) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 'STOE IPDS 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 23706 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5777 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+4.8479P] 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_number_reflns 5777 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.164841(9) -0.05141(2) 0.546412(11) 0.02817(10) Uani 1 d . . . C1 C 0.15894(7) -0.08854(17) 0.46316(10) 0.0292(4) Uani 1 d . . . N1 N 0.19177(6) -0.05666(15) 0.44578(9) 0.0324(4) Uani 1 d . . . N2 N 0.12164(6) -0.15734(16) 0.40838(8) 0.0328(4) Uani 1 d . . . C2 C 0.17515(9) -0.1077(2) 0.38146(11) 0.0399(5) Uani 1 d . . . H2 H 0.1915 -0.1003 0.3587 0.048 Uiso 1 calc R . . C3 C 0.13131(8) -0.1694(2) 0.35823(10) 0.0405(5) Uani 1 d . . . H3 H 0.1108 -0.2129 0.3157 0.049 Uiso 1 calc R . . C4 C 0.07755(8) -0.2119(2) 0.40485(12) 0.0413(5) Uani 1 d . . . H4 H 0.0826 -0.1942 0.4497 0.050 Uiso 1 calc R . . C5 C 0.07480(15) -0.3565(3) 0.3955(3) 0.1053(16) Uani 1 d . . . H5A H 0.0662 -0.3770 0.3498 0.158 Uiso 1 calc R . . H5B H 0.0489 -0.3917 0.4007 0.158 Uiso 1 calc R . . H5C H 0.1075 -0.3949 0.4301 0.158 Uiso 1 calc R . . C6 C 0.28191(9) -0.0834(2) 0.53868(14) 0.0515(6) Uani 1 d . . . H6A H 0.2721 -0.1360 0.5636 0.077 Uiso 1 calc R . . H6B H 0.3130 -0.0363 0.5713 0.077 Uiso 1 calc R . . H6C H 0.2875 -0.1398 0.5104 0.077 Uiso 1 calc R . . C7 C 0.23984(8) 0.0134(2) 0.49273(12) 0.0389(5) Uani 1 d . . . H7 H 0.2352 0.0704 0.5228 0.047 Uiso 1 calc R . . C8 C 0.02941(11) -0.1456(4) 0.3502(2) 0.0935(12) Uani 1 d . . . H8A H 0.0329 -0.0520 0.3580 0.140 Uiso 1 calc R . . H8B H 0.0016 -0.1774 0.3519 0.140 Uiso 1 calc R . . H8C H 0.0225 -0.1646 0.3052 0.140 Uiso 1 calc R . . C9 C 0.25303(11) 0.1003(3) 0.45258(16) 0.0587(7) Uani 1 d . . . H9A H 0.2603 0.0463 0.4253 0.088 Uiso 1 calc R . . H9B H 0.2827 0.1527 0.4846 0.088 Uiso 1 calc R . . H9C H 0.2245 0.1574 0.4222 0.088 Uiso 1 calc R . . N3 N 0.21184(7) 0.03520(16) 0.68872(9) 0.0354(4) Uani 1 d . . . N4 N 0.13496(6) -0.02773(16) 0.64249(9) 0.0350(4) Uani 1 d . . . C10 C 0.17072(7) -0.01180(18) 0.62890(10) 0.0310(4) Uani 1 d . . . C11 C 0.20197(9) 0.0492(2) 0.73843(11) 0.0437(5) Uani 1 d . . . H11 H 0.2245 0.0806 0.7836 0.052 Uiso 1 calc R . . C12 C 0.15399(9) 0.0092(2) 0.70982(11) 0.0420(5) Uani 1 d . . . H12 H 0.1366 0.0067 0.7313 0.050 Uiso 1 calc R . . C13 C 0.08475(8) -0.0851(3) 0.59242(13) 0.0479(5) Uani 1 d . . . H13 H 0.0771 -0.0724 0.5457 0.058 Uiso 1 calc R . . C14 C 0.27643(12) 0.2038(3) 0.71902(17) 0.0659(7) Uani 1 d . . . H14A H 0.2497 0.2602 0.6841 0.099 Uiso 1 calc R . . H14B H 0.3076 0.2209 0.7223 0.099 Uiso 1 calc R . . H14C H 0.2818 0.2210 0.7633 0.099 Uiso 1 calc R . . C15 C 0.30103(11) -0.0316(4) 0.7527(2) 0.0854(11) Uani 1 d . . . H15A H 0.3044 -0.0200 0.7960 0.128 Uiso 1 calc R . . H15B H 0.3334 -0.0138 0.7595 0.128 Uiso 1 calc R . . H15C H 0.2908 -0.1209 0.7368 0.128 Uiso 1 calc R . . C16 C 0.26116(8) 0.0619(2) 0.69920(12) 0.0449(5) Uani 1 d . . . H16 H 0.2573 0.0456 0.6550 0.054 Uiso 1 calc R . . C17 C 0.08614(11) -0.2306(3) 0.6050(2) 0.0734(9) Uani 1 d . . . H17A H 0.1118 -0.2710 0.6009 0.110 Uiso 1 calc R . . H17B H 0.0532 -0.2683 0.5711 0.110 Uiso 1 calc R . . H17C H 0.0943 -0.2456 0.6510 0.110 Uiso 1 calc R . . C18 C 0.04335(10) -0.0173(3) 0.59461(16) 0.0600(7) Uani 1 d . . . H18A H 0.0493 -0.0311 0.6395 0.090 Uiso 1 calc R . . H18B H 0.0105 -0.0532 0.5589 0.090 Uiso 1 calc R . . H18C H 0.0438 0.0757 0.5868 0.090 Uiso 1 calc R . . C19 C 0.19259(8) -0.2191(2) 0.58261(10) 0.0381(5) Uani 1 d . . . N5 N 0.20851(9) -0.3214(2) 0.60507(11) 0.0586(6) Uani 1 d . . . C20 C 0.13227(10) 0.1194(2) 0.50528(12) 0.0451(5) Uani 1 d . . . H20A H 0.1522 0.1606 0.4904 0.054 Uiso 1 calc R . . H20B H 0.0988 0.1002 0.4632 0.054 Uiso 1 calc R . . C21 C 0.12417(10) 0.2222(2) 0.54390(13) 0.0517(6) Uani 1 d . . . H21A H 0.1574 0.2509 0.5837 0.062 Uiso 1 calc R . . H21B H 0.1057 0.1830 0.5616 0.062 Uiso 1 calc R . . C22 C 0.09490(12) 0.3407(2) 0.50060(15) 0.0607(7) Uani 1 d . . . H22A H 0.0613 0.3125 0.4616 0.073 Uiso 1 calc R . . H22B H 0.1128 0.3784 0.4817 0.073 Uiso 1 calc R . . C23 C 0.08821(13) 0.4467(3) 0.54067(18) 0.0696(9) Uani 1 d . . . H23A H 0.1218 0.4755 0.5796 0.084 Uiso 1 calc R . . H23B H 0.0710 0.5221 0.5104 0.084 Uiso 1 calc R . . C24 C 0.05918(15) 0.4018(4) 0.5664(2) 0.0807(10) Uani 1 d . . . N6 N 0.03602(19) 0.3669(4) 0.5859(3) 0.1301(16) Uani 1 d . . . C25 C 0.0468(3) 0.3936(8) 0.2156(4) 0.160(3) Uani 1 d . . . H25 H 0.0282 0.4588 0.1823 0.192 Uiso 1 calc R . . C26 C 0.0953(3) 0.4200(5) 0.2796(4) 0.136(2) Uani 1 d . . . H26 H 0.1101 0.5036 0.2889 0.164 Uiso 1 calc R . . C27 C 0.11871(19) 0.3233(5) 0.3252(3) 0.1217(18) Uani 1 d . . . H27 H 0.1497 0.3403 0.3675 0.146 Uiso 1 calc R . . C28 C 0.09962(16) 0.2047(4) 0.3125(2) 0.0943(12) Uani 1 d . . . H28 H 0.1174 0.1395 0.3461 0.113 Uiso 1 calc R . . C29 C 0.05669(15) 0.1743(5) 0.2547(2) 0.0933(11) Uani 1 d . . . H29 H 0.0450 0.0875 0.2469 0.112 Uiso 1 calc R . . C30 C 0.02941(18) 0.2645(8) 0.2067(2) 0.124(2) Uani 1 d . . . H30 H -0.0020 0.2414 0.1662 0.149 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.03483(15) 0.02855(15) 0.02437(15) 0.00026(8) 0.01875(11) 0.00541(9) C1 0.0358(9) 0.0268(8) 0.0289(9) 0.0051(7) 0.0207(8) 0.0085(7) N1 0.0416(9) 0.0313(8) 0.0310(8) 0.0018(6) 0.0247(7) 0.0049(6) N2 0.0389(8) 0.0359(8) 0.0260(8) 0.0006(6) 0.0198(7) 0.0038(7) C2 0.0556(13) 0.0416(11) 0.0337(10) 0.0017(8) 0.0321(10) 0.0056(9) C3 0.0519(12) 0.0434(11) 0.0276(10) -0.0015(8) 0.0234(9) 0.0056(9) C4 0.0394(11) 0.0498(12) 0.0367(11) -0.0027(9) 0.0228(9) 0.0009(9) C5 0.098(3) 0.0503(17) 0.213(5) -0.013(2) 0.115(3) -0.0154(17) C6 0.0404(12) 0.0483(13) 0.0551(14) -0.0052(11) 0.0208(11) 0.0002(10) C7 0.0452(11) 0.0314(10) 0.0477(12) -0.0049(9) 0.0309(10) -0.0015(8) C8 0.0480(16) 0.134(3) 0.097(3) 0.040(2) 0.0400(17) 0.0285(19) C9 0.0698(17) 0.0467(13) 0.0788(19) 0.0024(13) 0.0536(15) -0.0078(12) N3 0.0422(9) 0.0377(9) 0.0287(8) -0.0063(7) 0.0217(7) -0.0042(7) N4 0.0399(9) 0.0383(9) 0.0323(9) -0.0041(7) 0.0237(8) 0.0009(7) C10 0.0370(10) 0.0285(9) 0.0304(9) -0.0007(7) 0.0209(8) 0.0034(7) C11 0.0572(13) 0.0469(12) 0.0307(10) -0.0088(9) 0.0273(10) -0.0043(10) C12 0.0536(12) 0.0483(12) 0.0350(11) -0.0055(9) 0.0317(10) 0.0003(10) C13 0.0387(11) 0.0644(14) 0.0419(12) -0.0100(11) 0.0236(10) -0.0044(10) C14 0.0717(18) 0.0619(17) 0.0711(18) -0.0152(14) 0.0448(15) -0.0249(14) C15 0.0458(15) 0.094(2) 0.103(3) 0.031(2) 0.0348(17) 0.0102(15) C16 0.0422(12) 0.0535(13) 0.0402(12) -0.0068(9) 0.0241(10) -0.0082(10) C17 0.0601(17) 0.0554(16) 0.112(3) -0.0305(16) 0.0528(18) -0.0164(13) C18 0.0452(13) 0.0765(18) 0.0643(17) 0.0060(14) 0.0346(13) 0.0102(12) C19 0.0479(11) 0.0442(12) 0.0269(9) 0.0030(8) 0.0241(9) 0.0124(9) N5 0.0879(16) 0.0509(12) 0.0461(11) 0.0169(9) 0.0433(12) 0.0328(11) C20 0.0654(14) 0.0364(11) 0.0449(12) 0.0069(9) 0.0382(12) 0.0151(10) C21 0.0651(15) 0.0402(12) 0.0476(13) 0.0035(10) 0.0308(12) 0.0175(11) C22 0.0820(18) 0.0400(13) 0.0647(16) 0.0089(11) 0.0444(15) 0.0230(12) C23 0.079(2) 0.0459(14) 0.0746(19) -0.0055(13) 0.0379(17) 0.0164(13) C24 0.094(2) 0.0659(19) 0.096(3) -0.0080(18) 0.062(2) 0.0201(18) N6 0.167(4) 0.106(3) 0.196(5) -0.003(3) 0.150(4) 0.022(3) C25 0.234(8) 0.184(6) 0.157(5) 0.112(5) 0.168(6) 0.147(6) C26 0.212(7) 0.075(3) 0.199(7) 0.005(4) 0.163(6) 0.025(4) C27 0.108(3) 0.089(3) 0.129(4) -0.035(3) 0.043(3) 0.005(3) C28 0.095(3) 0.087(3) 0.087(3) -0.013(2) 0.043(2) 0.013(2) C29 0.088(2) 0.124(3) 0.078(2) -0.009(2) 0.053(2) -0.016(2) C30 0.089(3) 0.217(7) 0.070(2) 0.030(3) 0.047(2) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni C10 1.885(2) . ? Ni C19 1.896(2) . ? Ni C1 1.897(2) . ? Ni C20 1.982(2) . ? C1 N2 1.354(3) . ? C1 N1 1.364(3) . ? N1 C2 1.390(3) . ? N1 C7 1.472(3) . ? N2 C3 1.384(3) . ? N2 C4 1.474(3) . ? C2 C3 1.338(3) . ? C4 C5 1.490(4) . ? C4 C8 1.494(4) . ? C6 C7 1.519(3) . ? C7 C9 1.521(3) . ? N3 C10 1.356(3) . ? N3 C11 1.381(3) . ? N3 C16 1.476(3) . ? N4 C10 1.360(3) . ? N4 C12 1.388(3) . ? N4 C13 1.470(3) . ? C11 C12 1.341(3) . ? C13 C17 1.513(4) . ? C13 C18 1.520(3) . ? C14 C16 1.517(4) . ? C15 C16 1.517(4) . ? C19 N5 1.153(3) . ? C20 C21 1.505(3) . ? C21 C22 1.517(3) . ? C22 C23 1.529(4) . ? C23 C24 1.441(6) . ? C24 N6 1.126(5) . ? C25 C30 1.402(9) . ? C25 C26 1.446(10) . ? C26 C27 1.333(8) . ? C27 C28 1.313(6) . ? C28 C29 1.307(5) . ? C29 C30 1.330(7) . ? 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 C10 Ni C19 89.10(8) . . ? C10 Ni C1 179.13(8) . . ? C19 Ni C1 91.69(8) . . ? C10 Ni C20 91.76(9) . . ? C19 Ni C20 176.97(10) . . ? C1 Ni C20 87.46(9) . . ? N2 C1 N1 104.47(16) . . ? N2 C1 Ni 127.22(15) . . ? N1 C1 Ni 128.27(14) . . ? C1 N1 C2 110.68(17) . . ? C1 N1 C7 122.95(17) . . ? C2 N1 C7 126.20(18) . . ? C1 N2 C3 110.85(17) . . ? C1 N2 C4 123.18(17) . . ? C3 N2 C4 125.96(17) . . ? C3 C2 N1 106.61(19) . . ? C2 C3 N2 107.37(18) . . ? N2 C4 C5 111.0(2) . . ? N2 C4 C8 111.2(2) . . ? C5 C4 C8 112.2(3) . . ? N1 C7 C6 109.96(17) . . ? N1 C7 C9 111.0(2) . . ? C6 C7 C9 112.2(2) . . ? C10 N3 C11 111.28(18) . . ? C10 N3 C16 123.54(18) . . ? C11 N3 C16 125.12(18) . . ? C10 N4 C12 110.70(17) . . ? C10 N4 C13 122.69(17) . . ? C12 N4 C13 126.49(18) . . ? N3 C10 N4 104.29(17) . . ? N3 C10 Ni 128.04(15) . . ? N4 C10 Ni 127.64(14) . . ? C12 C11 N3 106.82(19) . . ? C11 C12 N4 106.9(2) . . ? N4 C13 C17 109.8(2) . . ? N4 C13 C18 111.5(2) . . ? C17 C13 C18 111.8(2) . . ? N3 C16 C15 109.6(2) . . ? N3 C16 C14 110.8(2) . . ? C15 C16 C14 112.1(2) . . ? N5 C19 Ni 178.1(2) . . ? C21 C20 Ni 122.93(16) . . ? C20 C21 C22 113.9(2) . . ? C21 C22 C23 113.7(2) . . ? C24 C23 C22 112.5(3) . . ? N6 C24 C23 179.2(5) . . ? C30 C25 C26 115.6(4) . . ? C27 C26 C25 118.6(6) . . ? C28 C27 C26 121.8(5) . . ? C29 C28 C27 122.3(5) . . ? C28 C29 C30 120.8(5) . . ? C29 C30 C25 120.9(5) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 0.401 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.058 # ==> end _chemical_name_common '(iPr2Im)2(CN)(C4H8CN)Ni(ii) benzene solvate'