Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Andreas Danopoulos' _publ_contact_author_name 'Andreas Danopoulos' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email AD1@SOTON.AC.UK _publ_section_title ; A Method for the Synthesis of Nickel(0) Bis(Carbene) Complexes ; _publ_requested_category FM # Attachment 'CombinedCIF.cif' data_Ni(SIPri)2 _database_code_depnum_ccdc_archive 'CCDC 662510' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H76 N4 Ni' _chemical_formula_sum 'C54 H76 N4 Ni' _chemical_formula_weight 839.90 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 P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.8554(3) _cell_length_b 27.1710(7) _cell_length_c 13.9453(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.5160(10) _cell_angle_gamma 90.00 _cell_volume 4866.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 79791 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41469 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.61 _reflns_number_total 11110 _reflns_number_gt 8329 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SIR-92 (Altomare, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+16.2545P] 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 11109 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6219(3) 0.07791(14) 0.9258(2) 0.0215(7) Uani 1 1 d . . . C2 C 0.6116(3) 0.11811(13) 0.9878(2) 0.0214(7) Uani 1 1 d . . . C3 C 0.5122(3) 0.13068(14) 1.0147(3) 0.0264(8) Uani 1 1 d . . . H3 H 0.5035 0.1578 1.0567 0.032 Uiso 1 1 calc R . . C4 C 0.4258(3) 0.10447(15) 0.9814(3) 0.0288(8) Uani 1 1 d . . . H4 H 0.3586 0.1134 1.0012 0.035 Uiso 1 1 calc R . . C5 C 0.4371(3) 0.06502(14) 0.9189(3) 0.0242(8) Uani 1 1 d . . . H5 H 0.3772 0.0477 0.8952 0.029 Uiso 1 1 calc R . . C6 C 0.5354(3) 0.05073(13) 0.8905(2) 0.0203(7) Uani 1 1 d . . . C7 C 0.7053(3) 0.14684(14) 1.0264(3) 0.0262(8) Uani 1 1 d . . . H7 H 0.7684 0.1333 0.9962 0.031 Uiso 1 1 calc R . . C8 C 0.6951(4) 0.20078(15) 0.9982(3) 0.0388(10) Uani 1 1 d . . . H8A H 0.6896 0.2035 0.9281 0.058 Uiso 1 1 calc R . . H8B H 0.7565 0.2189 1.0228 0.058 Uiso 1 1 calc R . . H8C H 0.6325 0.2147 1.0254 0.058 Uiso 1 1 calc R . . C9 C 0.7207(3) 0.14068(16) 1.1356(3) 0.0342(9) Uani 1 1 d . . . H9A H 0.6604 0.1543 1.1671 0.051 Uiso 1 1 calc R . . H9B H 0.7838 0.1582 1.1581 0.051 Uiso 1 1 calc R . . H9C H 0.7276 0.1056 1.1513 0.051 Uiso 1 1 calc R . . C10 C 0.5502(3) 0.00673(13) 0.8244(2) 0.0225(7) Uani 1 1 d . . . H10 H 0.6127 -0.0120 0.8495 0.027 Uiso 1 1 calc R . . C11 C 0.4579(3) -0.02853(15) 0.8205(3) 0.0305(8) Uani 1 1 d . . . H11A H 0.4422 -0.0386 0.8858 0.046 Uiso 1 1 calc R . . H11B H 0.4750 -0.0576 0.7828 0.046 Uiso 1 1 calc R . . H11C H 0.3970 -0.0120 0.7903 0.046 Uiso 1 1 calc R . . C12 C 0.5722(3) 0.02449(16) 0.7233(3) 0.0352(10) Uani 1 1 d . . . H12A H 0.5110 0.0419 0.6960 0.053 Uiso 1 1 calc R . . H12B H 0.5875 -0.0039 0.6828 0.053 Uiso 1 1 calc R . . H12C H 0.6321 0.0468 0.7262 0.053 Uiso 1 1 calc R . . C13 C 0.7966(3) 0.07557(12) 0.8521(2) 0.0177(7) Uani 1 1 d . . . C14 C 0.7621(3) 0.02317(14) 0.9855(3) 0.0249(8) Uani 1 1 d . . . H14A H 0.7217 -0.0079 0.9827 0.030 Uiso 1 1 calc R . . H14B H 0.7591 0.0375 1.0506 0.030 Uiso 1 1 calc R . . C15 C 0.8728(3) 0.01498(14) 0.9583(3) 0.0243(8) Uani 1 1 d . . . H15A H 0.9223 0.0222 1.0128 0.029 Uiso 1 1 calc R . . H15B H 0.8834 -0.0193 0.9368 0.029 Uiso 1 1 calc R . . C16 C 0.9849(3) 0.05190(13) 0.8385(3) 0.0215(7) Uani 1 1 d . . . C17 C 1.0593(3) 0.08583(14) 0.8758(3) 0.0242(7) Uani 1 1 d . . . C18 C 1.1579(3) 0.08540(16) 0.8383(3) 0.0312(9) Uani 1 1 d . . . H18 H 1.2085 0.1087 0.8604 0.037 Uiso 1 1 calc R . . C19 C 1.1828(3) 0.05138(17) 0.7691(3) 0.0355(10) Uani 1 1 d . . . H19 H 1.2499 0.0520 0.7432 0.043 Uiso 1 1 calc R . . C20 C 1.1109(3) 0.01665(16) 0.7376(3) 0.0338(9) Uani 1 1 d . . . H20 H 1.1303 -0.0075 0.6925 0.041 Uiso 1 1 calc R . . C21 C 1.0108(3) 0.01635(15) 0.7706(3) 0.0276(8) Uani 1 1 d . . . C22 C 1.0315(3) 0.12108(14) 0.9559(3) 0.0273(8) Uani 1 1 d . . . H22 H 0.9779 0.1046 0.9946 0.033 Uiso 1 1 calc R . . C23 C 1.1249(3) 0.13380(15) 1.0244(3) 0.0358(10) Uani 1 1 d . . . H23A H 1.1583 0.1034 1.0476 0.054 Uiso 1 1 calc R . . H23B H 1.1007 0.1526 1.0791 0.054 Uiso 1 1 calc R . . H23C H 1.1752 0.1535 0.9901 0.054 Uiso 1 1 calc R . . C24 C 0.9831(3) 0.16814(15) 0.9144(3) 0.0336(9) Uani 1 1 d . . . H24A H 1.0348 0.1858 0.8778 0.050 Uiso 1 1 calc R . . H24B H 0.9606 0.1891 0.9668 0.050 Uiso 1 1 calc R . . H24C H 0.9229 0.1598 0.8719 0.050 Uiso 1 1 calc R . . C25 C 0.9320(3) -0.02198(16) 0.7344(3) 0.0355(9) Uani 1 1 d . . . H25 H 0.8704 -0.0198 0.7755 0.043 Uiso 1 1 calc R . . C26 C 0.9743(4) -0.07418(18) 0.7428(4) 0.0557(14) Uani 1 1 d . . . H26A H 1.0343 -0.0777 0.7023 0.084 Uiso 1 1 calc R . . H26B H 0.9199 -0.0976 0.7217 0.084 Uiso 1 1 calc R . . H26C H 0.9959 -0.0809 0.8097 0.084 Uiso 1 1 calc R . . C27 C 0.8945(5) -0.0105(2) 0.6318(4) 0.0703(18) Uani 1 1 d . . . H27A H 0.8627 0.0223 0.6293 0.106 Uiso 1 1 calc R . . H27B H 0.8429 -0.0351 0.6101 0.106 Uiso 1 1 calc R . . H27C H 0.9537 -0.0113 0.5899 0.106 Uiso 1 1 calc R . . C28 C 0.5847(3) 0.14608(13) 0.5897(2) 0.0219(7) Uani 1 1 d . . . C29 C 0.4940(3) 0.16041(14) 0.6336(2) 0.0242(8) Uani 1 1 d . . . C30 C 0.4028(3) 0.13379(15) 0.6126(3) 0.0294(8) Uani 1 1 d . . . H30 H 0.3405 0.1425 0.6425 0.035 Uiso 1 1 calc R . . C31 C 0.4023(3) 0.09475(15) 0.5485(3) 0.0298(9) Uani 1 1 d . . . H31 H 0.3392 0.0779 0.5324 0.036 Uiso 1 1 calc R . . C32 C 0.4936(3) 0.08043(14) 0.5081(3) 0.0285(8) Uani 1 1 d . . . H32 H 0.4925 0.0530 0.4659 0.034 Uiso 1 1 calc R . . C33 C 0.5873(3) 0.10503(14) 0.5273(2) 0.0244(8) Uani 1 1 d . . . C34 C 0.4925(3) 0.20274(15) 0.7051(3) 0.0289(8) Uani 1 1 d . . . H34 H 0.5650 0.2159 0.7138 0.035 Uiso 1 1 calc R . . C35 C 0.4584(4) 0.18450(17) 0.8024(3) 0.0429(11) Uani 1 1 d . . . H35A H 0.3859 0.1733 0.7963 0.064 Uiso 1 1 calc R . . H35B H 0.4642 0.2114 0.8492 0.064 Uiso 1 1 calc R . . H35C H 0.5031 0.1571 0.8241 0.064 Uiso 1 1 calc R . . C36 C 0.4213(3) 0.24505(16) 0.6689(3) 0.0375(10) Uani 1 1 d . . . H36A H 0.4423 0.2557 0.6055 0.056 Uiso 1 1 calc R . . H36B H 0.4273 0.2727 0.7139 0.056 Uiso 1 1 calc R . . H36C H 0.3490 0.2336 0.6642 0.056 Uiso 1 1 calc R . . C37 C 0.6888(3) 0.08833(15) 0.4864(3) 0.0282(8) Uani 1 1 d . . . H37 H 0.7456 0.0953 0.5358 0.034 Uiso 1 1 calc R . . C38 C 0.7140(4) 0.11717(18) 0.3959(3) 0.0450(11) Uani 1 1 d . . . H38A H 0.6580 0.1124 0.3468 0.067 Uiso 1 1 calc R . . H38B H 0.7798 0.1053 0.3716 0.067 Uiso 1 1 calc R . . H38C H 0.7203 0.1522 0.4115 0.067 Uiso 1 1 calc R . . C39 C 0.6908(3) 0.03334(15) 0.4658(3) 0.0360(10) Uani 1 1 d . . . H39A H 0.6706 0.0152 0.5228 0.054 Uiso 1 1 calc R . . H39B H 0.7612 0.0236 0.4493 0.054 Uiso 1 1 calc R . . H39C H 0.6418 0.0258 0.4119 0.054 Uiso 1 1 calc R . . C40 C 0.7574(3) 0.17350(12) 0.6645(2) 0.0194(7) Uani 1 1 d . . . C41 C 0.6699(3) 0.22439(14) 0.5472(3) 0.0305(9) Uani 1 1 d . . . H41A H 0.6179 0.2466 0.5745 0.037 Uiso 1 1 calc R . . H41B H 0.6530 0.2198 0.4779 0.037 Uiso 1 1 calc R . . C42 C 0.7785(3) 0.24372(15) 0.5646(3) 0.0326(9) Uani 1 1 d . . . H42A H 0.8221 0.2371 0.5093 0.039 Uiso 1 1 calc R . . H42B H 0.7784 0.2795 0.5779 0.039 Uiso 1 1 calc R . . C43 C 0.9195(3) 0.22433(14) 0.6843(3) 0.0233(7) Uani 1 1 d . . . C44 C 0.9384(3) 0.26351(14) 0.7487(3) 0.0241(8) Uani 1 1 d . . . C45 C 1.0411(3) 0.27379(15) 0.7771(3) 0.0285(8) Uani 1 1 d . . . H45 H 1.0554 0.3002 0.8204 0.034 Uiso 1 1 calc R . . C46 C 1.1222(3) 0.24677(17) 0.7441(3) 0.0346(9) Uani 1 1 d . . . H46 H 1.1917 0.2539 0.7660 0.042 Uiso 1 1 calc R . . C47 C 1.1026(3) 0.20899(16) 0.6787(3) 0.0319(9) Uani 1 1 d . . . H47 H 1.1590 0.1903 0.6562 0.038 Uiso 1 1 calc R . . C48 C 1.0013(3) 0.19814(14) 0.6454(3) 0.0255(8) Uani 1 1 d . . . C49 C 0.8508(3) 0.29430(15) 0.7870(3) 0.0310(9) Uani 1 1 d . . . H49 H 0.7832 0.2783 0.7672 0.037 Uiso 1 1 calc R . . C50 C 0.8579(4) 0.29738(17) 0.8967(3) 0.0401(10) Uani 1 1 d . . . H50A H 0.8633 0.2641 0.9237 0.060 Uiso 1 1 calc R . . H50B H 0.7954 0.3135 0.9194 0.060 Uiso 1 1 calc R . . H50C H 0.9196 0.3165 0.9173 0.060 Uiso 1 1 calc R . . C51 C 0.8510(4) 0.34645(18) 0.7459(4) 0.0509(13) Uani 1 1 d . . . H51A H 0.9156 0.3632 0.7668 0.076 Uiso 1 1 calc R . . H51B H 0.7913 0.3647 0.7689 0.076 Uiso 1 1 calc R . . H51C H 0.8461 0.3449 0.6756 0.076 Uiso 1 1 calc R . . C52 C 0.9831(3) 0.16071(15) 0.5649(3) 0.0325(9) Uani 1 1 d . . . H52 H 0.9062 0.1573 0.5530 0.039 Uiso 1 1 calc R . . C53 C 1.0292(4) 0.17949(19) 0.4710(3) 0.0506(13) Uani 1 1 d . . . H53A H 1.1051 0.1818 0.4797 0.076 Uiso 1 1 calc R . . H53B H 1.0004 0.2120 0.4552 0.076 Uiso 1 1 calc R . . H53C H 1.0113 0.1565 0.4187 0.076 Uiso 1 1 calc R . . C54 C 1.0256(5) 0.11084(18) 0.5918(4) 0.0581(15) Uani 1 1 d . . . H54A H 1.1014 0.1129 0.6018 0.087 Uiso 1 1 calc R . . H54B H 1.0083 0.0874 0.5400 0.087 Uiso 1 1 calc R . . H54C H 0.9948 0.0997 0.6511 0.087 Uiso 1 1 calc R . . N1 N 0.7235(2) 0.05847(11) 0.9110(2) 0.0192(6) Uani 1 1 d . . . N2 N 0.8852(2) 0.04991(11) 0.8793(2) 0.0202(6) Uani 1 1 d . . . N3 N 0.6748(2) 0.17704(11) 0.5981(2) 0.0219(6) Uani 1 1 d . . . N4 N 0.8146(2) 0.21540(11) 0.6499(2) 0.0224(6) Uani 1 1 d . . . Ni1 Ni 0.77919(3) 0.124106(17) 0.75601(3) 0.01934(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0179(17) 0.0271(19) 0.0194(16) 0.0073(14) 0.0008(13) 0.0007(14) C2 0.0234(17) 0.0224(18) 0.0183(16) 0.0038(13) -0.0015(13) -0.0002(14) C3 0.0282(19) 0.029(2) 0.0224(17) 0.0005(15) 0.0024(14) 0.0041(15) C4 0.0205(18) 0.036(2) 0.030(2) 0.0030(16) 0.0041(15) 0.0061(16) C5 0.0182(17) 0.030(2) 0.0245(18) 0.0025(15) -0.0010(14) 0.0004(14) C6 0.0225(17) 0.0200(17) 0.0181(16) 0.0022(13) -0.0021(13) -0.0001(14) C7 0.0258(19) 0.026(2) 0.0265(19) -0.0060(15) 0.0005(15) -0.0019(15) C8 0.050(3) 0.030(2) 0.036(2) 0.0017(18) -0.0073(19) -0.0139(19) C9 0.041(2) 0.033(2) 0.027(2) -0.0014(16) -0.0099(17) -0.0033(18) C10 0.0262(18) 0.0215(18) 0.0197(17) 0.0006(13) -0.0008(14) 0.0004(14) C11 0.033(2) 0.029(2) 0.030(2) 0.0036(16) -0.0013(16) -0.0048(17) C12 0.045(2) 0.040(2) 0.0207(18) -0.0021(16) 0.0003(17) -0.014(2) C13 0.0190(16) 0.0155(16) 0.0184(15) -0.0032(12) -0.0024(12) -0.0023(13) C14 0.0219(18) 0.031(2) 0.0215(17) 0.0092(15) -0.0004(14) 0.0018(15) C15 0.0233(18) 0.0243(19) 0.0253(18) 0.0090(14) 0.0017(14) 0.0019(14) C16 0.0176(16) 0.0223(18) 0.0246(17) 0.0029(14) 0.0004(13) 0.0051(14) C17 0.0208(17) 0.0260(19) 0.0257(18) 0.0029(15) 0.0010(14) 0.0025(14) C18 0.0203(18) 0.038(2) 0.036(2) 0.0056(17) 0.0022(16) -0.0024(16) C19 0.0208(19) 0.048(3) 0.038(2) 0.0076(19) 0.0089(17) 0.0078(18) C20 0.032(2) 0.040(2) 0.030(2) -0.0001(17) 0.0061(16) 0.0104(18) C21 0.028(2) 0.030(2) 0.0247(18) 0.0027(15) 0.0011(15) 0.0070(16) C22 0.0274(19) 0.026(2) 0.0282(19) 0.0024(15) -0.0004(15) -0.0046(16) C23 0.039(2) 0.030(2) 0.037(2) -0.0033(17) -0.0115(18) -0.0019(18) C24 0.038(2) 0.029(2) 0.034(2) -0.0016(17) -0.0026(17) 0.0010(17) C25 0.041(2) 0.031(2) 0.035(2) -0.0113(18) 0.0056(18) -0.0043(18) C26 0.071(4) 0.033(3) 0.063(3) -0.008(2) 0.006(3) -0.006(2) C27 0.083(4) 0.064(4) 0.060(4) -0.001(3) -0.036(3) -0.019(3) C28 0.0219(17) 0.0224(18) 0.0211(17) 0.0054(14) -0.0040(13) -0.0033(14) C29 0.0280(19) 0.0246(19) 0.0197(17) 0.0046(14) -0.0031(14) -0.0013(15) C30 0.0234(19) 0.033(2) 0.032(2) 0.0052(16) -0.0002(15) 0.0007(16) C31 0.027(2) 0.029(2) 0.033(2) 0.0062(16) -0.0074(16) -0.0051(16) C32 0.036(2) 0.026(2) 0.0227(18) -0.0004(15) -0.0072(15) -0.0049(16) C33 0.0297(19) 0.0240(19) 0.0192(17) 0.0042(14) -0.0017(14) -0.0002(15) C34 0.030(2) 0.031(2) 0.0256(19) -0.0019(15) -0.0016(15) 0.0055(16) C35 0.066(3) 0.038(3) 0.025(2) 0.0010(18) 0.000(2) 0.008(2) C36 0.043(2) 0.030(2) 0.039(2) 0.0026(18) -0.0008(19) 0.0102(19) C37 0.030(2) 0.030(2) 0.0237(18) -0.0031(15) -0.0033(15) -0.0009(16) C38 0.052(3) 0.046(3) 0.039(2) 0.009(2) 0.017(2) 0.006(2) C39 0.042(2) 0.033(2) 0.032(2) -0.0053(17) -0.0006(18) 0.0027(19) C40 0.0183(16) 0.0181(17) 0.0216(16) -0.0039(13) 0.0001(13) 0.0005(13) C41 0.032(2) 0.025(2) 0.033(2) 0.0077(16) -0.0104(17) -0.0033(16) C42 0.035(2) 0.029(2) 0.033(2) 0.0139(17) -0.0112(17) -0.0074(17) C43 0.0232(18) 0.0243(19) 0.0221(17) 0.0055(14) -0.0016(14) -0.0032(14) C44 0.0253(19) 0.0246(19) 0.0224(17) 0.0035(14) 0.0001(14) -0.0023(15) C45 0.027(2) 0.034(2) 0.0240(18) -0.0021(16) -0.0020(15) -0.0053(16) C46 0.0224(19) 0.049(3) 0.032(2) 0.0072(19) -0.0006(16) -0.0087(18) C47 0.0226(19) 0.039(2) 0.034(2) 0.0042(18) 0.0058(16) 0.0021(17) C48 0.030(2) 0.0226(19) 0.0237(18) -0.0002(14) 0.0028(15) -0.0023(15) C49 0.031(2) 0.032(2) 0.031(2) -0.0071(16) 0.0033(16) -0.0054(17) C50 0.051(3) 0.041(3) 0.029(2) -0.0073(18) 0.0114(19) 0.000(2) C51 0.064(3) 0.042(3) 0.047(3) 0.004(2) 0.015(2) 0.013(2) C52 0.034(2) 0.033(2) 0.031(2) -0.0034(17) 0.0099(17) -0.0031(17) C53 0.070(3) 0.050(3) 0.033(2) -0.004(2) 0.010(2) -0.014(3) C54 0.090(4) 0.036(3) 0.048(3) -0.006(2) -0.006(3) 0.015(3) N1 0.0167(14) 0.0225(15) 0.0182(14) 0.0058(11) -0.0003(11) 0.0017(11) N2 0.0207(15) 0.0184(15) 0.0216(14) 0.0021(11) 0.0018(11) 0.0016(11) N3 0.0248(15) 0.0176(15) 0.0226(15) 0.0044(11) -0.0061(12) -0.0033(12) N4 0.0228(15) 0.0222(16) 0.0216(15) 0.0049(12) -0.0050(12) -0.0031(12) Ni1 0.0205(2) 0.0196(2) 0.0177(2) 0.00213(18) -0.00126(16) 0.00022(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.402(5) . ? C1 C6 1.406(5) . ? C1 N1 1.433(4) . ? C2 C3 1.390(5) . ? C2 C7 1.515(5) . ? C3 C4 1.382(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.395(5) . ? C5 H5 0.9500 . ? C6 C10 1.527(5) . ? C7 C8 1.522(6) . ? C7 C9 1.536(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.525(5) . ? C10 C12 1.528(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.357(4) . ? C13 N2 1.374(4) . ? C13 Ni1 1.886(3) . ? C14 N1 1.483(4) . ? C14 C15 1.505(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N2 1.468(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.402(5) . ? C16 C17 1.411(5) . ? C16 N2 1.427(4) . ? C17 C18 1.392(5) . ? C17 C22 1.526(5) . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 C20 1.380(6) . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 C25 1.524(6) . ? C22 C24 1.525(5) . ? C22 C23 1.541(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.522(7) . ? C25 C26 1.522(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.395(5) . ? C28 C33 1.416(5) . ? C28 N3 1.432(4) . ? C29 C30 1.398(5) . ? C29 C34 1.523(5) . ? C30 C31 1.387(6) . ? C30 H30 0.9500 . ? C31 C32 1.379(6) . ? C31 H31 0.9500 . ? C32 C33 1.394(5) . ? C32 H32 0.9500 . ? C33 C37 1.516(5) . ? C34 C35 1.526(6) . ? C34 C36 1.541(5) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.522(6) . ? C37 C38 1.532(6) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N4 1.375(4) . ? C40 N3 1.381(4) . ? C40 Ni1 1.865(3) . ? C41 N3 1.469(5) . ? C41 C42 1.501(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N4 1.474(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.398(5) . ? C43 C44 1.408(5) . ? C43 N4 1.432(4) . ? C44 C45 1.389(5) . ? C44 C49 1.518(5) . ? C45 C46 1.372(6) . ? C45 H45 0.9500 . ? C46 C47 1.390(6) . ? C46 H46 0.9500 . ? C47 C48 1.395(5) . ? C47 H47 0.9500 . ? C48 C52 1.525(5) . ? C49 C51 1.529(6) . ? C49 C50 1.531(5) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.502(6) . ? C52 C53 1.547(6) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 122.1(3) . . ? C2 C1 N1 119.2(3) . . ? C6 C1 N1 117.9(3) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C7 120.2(3) . . ? C1 C2 C7 121.7(3) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C10 121.9(3) . . ? C1 C6 C10 120.3(3) . . ? C2 C7 C8 110.2(3) . . ? C2 C7 C9 111.2(3) . . ? C8 C7 C9 111.6(3) . . ? C2 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 113.3(3) . . ? C11 C10 C12 109.9(3) . . ? C6 C10 C12 110.1(3) . . ? C11 C10 H10 107.8 . . ? C6 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 N2 104.3(3) . . ? N1 C13 Ni1 127.3(2) . . ? N2 C13 Ni1 128.5(3) . . ? N1 C14 C15 102.1(3) . . ? N1 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? N1 C14 H14B 111.3 . . ? C15 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? N2 C15 C14 103.2(3) . . ? N2 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? N2 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C21 C16 C17 121.4(3) . . ? C21 C16 N2 119.1(3) . . ? C17 C16 N2 119.0(3) . . ? C18 C17 C16 118.0(4) . . ? C18 C17 C22 121.8(3) . . ? C16 C17 C22 120.2(3) . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 120.4(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.2(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 118.1(4) . . ? C20 C21 C25 120.5(4) . . ? C16 C21 C25 121.4(3) . . ? C24 C22 C17 110.7(3) . . ? C24 C22 C23 109.9(3) . . ? C17 C22 C23 113.1(3) . . ? C24 C22 H22 107.6 . . ? C17 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 111.2(4) . . ? C27 C25 C21 110.5(4) . . ? C26 C25 C21 112.4(4) . . ? C27 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C21 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 122.1(3) . . ? C29 C28 N3 119.2(3) . . ? C33 C28 N3 118.2(3) . . ? C28 C29 C30 118.2(3) . . ? C28 C29 C34 122.2(3) . . ? C30 C29 C34 119.5(3) . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.9(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 122.0(4) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C32 C33 C28 116.9(3) . . ? C32 C33 C37 122.3(3) . . ? C28 C33 C37 120.7(3) . . ? C29 C34 C35 110.4(3) . . ? C29 C34 C36 111.9(3) . . ? C35 C34 C36 110.1(3) . . ? C29 C34 H34 108.1 . . ? C35 C34 H34 108.1 . . ? C36 C34 H34 108.1 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 C39 112.7(3) . . ? C33 C37 C38 111.9(3) . . ? C39 C37 C38 109.9(3) . . ? C33 C37 H37 107.3 . . ? C39 C37 H37 107.3 . . ? C38 C37 H37 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 N3 104.1(3) . . ? N4 C40 Ni1 129.2(2) . . ? N3 C40 Ni1 126.6(3) . . ? N3 C41 C42 102.1(3) . . ? N3 C41 H41A 111.4 . . ? C42 C41 H41A 111.4 . . ? N3 C41 H41B 111.4 . . ? C42 C41 H41B 111.4 . . ? H41A C41 H41B 109.2 . . ? N4 C42 C41 101.8(3) . . ? N4 C42 H42A 111.4 . . ? C41 C42 H42A 111.4 . . ? N4 C42 H42B 111.4 . . ? C41 C42 H42B 111.4 . . ? H42A C42 H42B 109.3 . . ? C48 C43 C44 121.4(3) . . ? C48 C43 N4 119.8(3) . . ? C44 C43 N4 118.4(3) . . ? C45 C44 C43 118.0(3) . . ? C45 C44 C49 119.9(3) . . ? C43 C44 C49 122.1(3) . . ? C46 C45 C44 121.6(4) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 119.8(4) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C48 121.0(4) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C43 118.0(3) . . ? C47 C48 C52 119.7(4) . . ? C43 C48 C52 122.1(3) . . ? C44 C49 C51 111.5(3) . . ? C44 C49 C50 111.7(3) . . ? C51 C49 C50 108.9(4) . . ? C44 C49 H49 108.3 . . ? C51 C49 H49 108.3 . . ? C50 C49 H49 108.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C48 112.1(4) . . ? C54 C52 C53 111.1(4) . . ? C48 C52 C53 110.5(3) . . ? C54 C52 H52 107.6 . . ? C48 C52 H52 107.6 . . ? C53 C52 H52 107.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C13 N1 C1 128.4(3) . . ? C13 N1 C14 115.2(3) . . ? C1 N1 C14 114.6(3) . . ? C13 N2 C16 128.2(3) . . ? C13 N2 C15 114.8(3) . . ? C16 N2 C15 116.9(3) . . ? C40 N3 C28 127.5(3) . . ? C40 N3 C41 113.6(3) . . ? C28 N3 C41 117.2(3) . . ? C40 N4 C43 126.3(3) . . ? C40 N4 C42 113.6(3) . . ? C43 N4 C42 116.1(3) . . ? C40 Ni1 C13 177.35(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.4(5) . . . . ? N1 C1 C2 C3 -168.6(3) . . . . ? C6 C1 C2 C7 179.3(3) . . . . ? N1 C1 C2 C7 10.4(5) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C7 C2 C3 C4 -179.0(3) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C4 C5 C6 C1 -1.1(5) . . . . ? C4 C5 C6 C10 178.2(3) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? N1 C1 C6 C5 169.3(3) . . . . ? C2 C1 C6 C10 -179.1(3) . . . . ? N1 C1 C6 C10 -10.0(5) . . . . ? C3 C2 C7 C8 -59.5(4) . . . . ? C1 C2 C7 C8 121.6(4) . . . . ? C3 C2 C7 C9 64.8(4) . . . . ? C1 C2 C7 C9 -114.1(4) . . . . ? C5 C6 C10 C11 -19.1(5) . . . . ? C1 C6 C10 C11 160.2(3) . . . . ? C5 C6 C10 C12 104.4(4) . . . . ? C1 C6 C10 C12 -76.4(4) . . . . ? N1 C14 C15 N2 5.4(4) . . . . ? C21 C16 C17 C18 4.5(5) . . . . ? N2 C16 C17 C18 176.7(3) . . . . ? C21 C16 C17 C22 -174.6(3) . . . . ? N2 C16 C17 C22 -2.3(5) . . . . ? C16 C17 C18 C19 -2.4(6) . . . . ? C22 C17 C18 C19 176.7(4) . . . . ? C17 C18 C19 C20 -1.3(6) . . . . ? C18 C19 C20 C21 3.2(6) . . . . ? C19 C20 C21 C16 -1.1(6) . . . . ? C19 C20 C21 C25 179.4(4) . . . . ? C17 C16 C21 C20 -2.7(5) . . . . ? N2 C16 C21 C20 -175.0(3) . . . . ? C17 C16 C21 C25 176.7(3) . . . . ? N2 C16 C21 C25 4.5(5) . . . . ? C18 C17 C22 C24 93.0(4) . . . . ? C16 C17 C22 C24 -88.0(4) . . . . ? C18 C17 C22 C23 -30.9(5) . . . . ? C16 C17 C22 C23 148.1(3) . . . . ? C20 C21 C25 C27 -73.4(5) . . . . ? C16 C21 C25 C27 107.1(5) . . . . ? C20 C21 C25 C26 51.5(5) . . . . ? C16 C21 C25 C26 -128.0(4) . . . . ? C33 C28 C29 C30 -1.7(5) . . . . ? N3 C28 C29 C30 170.4(3) . . . . ? C33 C28 C29 C34 176.4(3) . . . . ? N3 C28 C29 C34 -11.4(5) . . . . ? C28 C29 C30 C31 -1.1(5) . . . . ? C34 C29 C30 C31 -179.3(3) . . . . ? C29 C30 C31 C32 2.9(6) . . . . ? C30 C31 C32 C33 -2.0(6) . . . . ? C31 C32 C33 C28 -0.8(5) . . . . ? C31 C32 C33 C37 177.5(3) . . . . ? C29 C28 C33 C32 2.6(5) . . . . ? N3 C28 C33 C32 -169.6(3) . . . . ? C29 C28 C33 C37 -175.7(3) . . . . ? N3 C28 C33 C37 12.1(5) . . . . ? C28 C29 C34 C35 -119.6(4) . . . . ? C30 C29 C34 C35 58.6(5) . . . . ? C28 C29 C34 C36 117.4(4) . . . . ? C30 C29 C34 C36 -64.5(5) . . . . ? C32 C33 C37 C39 -27.3(5) . . . . ? C28 C33 C37 C39 150.9(3) . . . . ? C32 C33 C37 C38 97.3(4) . . . . ? C28 C33 C37 C38 -84.5(4) . . . . ? N3 C41 C42 N4 -20.8(4) . . . . ? C48 C43 C44 C45 -3.6(5) . . . . ? N4 C43 C44 C45 -176.1(3) . . . . ? C48 C43 C44 C49 176.3(3) . . . . ? N4 C43 C44 C49 3.7(5) . . . . ? C43 C44 C45 C46 -0.2(6) . . . . ? C49 C44 C45 C46 179.9(4) . . . . ? C44 C45 C46 C47 1.8(6) . . . . ? C45 C46 C47 C48 0.3(6) . . . . ? C46 C47 C48 C43 -3.9(6) . . . . ? C46 C47 C48 C52 172.8(4) . . . . ? C44 C43 C48 C47 5.6(5) . . . . ? N4 C43 C48 C47 178.0(3) . . . . ? C44 C43 C48 C52 -171.0(3) . . . . ? N4 C43 C48 C52 1.5(5) . . . . ? C45 C44 C49 C51 69.8(5) . . . . ? C43 C44 C49 C51 -110.0(4) . . . . ? C45 C44 C49 C50 -52.2(5) . . . . ? C43 C44 C49 C50 128.0(4) . . . . ? C47 C48 C52 C54 60.0(5) . . . . ? C43 C48 C52 C54 -123.5(4) . . . . ? C47 C48 C52 C53 -64.6(5) . . . . ? C43 C48 C52 C53 111.9(4) . . . . ? N2 C13 N1 C1 168.4(3) . . . . ? Ni1 C13 N1 C1 -11.0(5) . . . . ? N2 C13 N1 C14 4.4(4) . . . . ? Ni1 C13 N1 C14 -174.9(2) . . . . ? C2 C1 N1 C13 -80.8(4) . . . . ? C6 C1 N1 C13 109.8(4) . . . . ? C2 C1 N1 C14 83.3(4) . . . . ? C6 C1 N1 C14 -86.1(4) . . . . ? C15 C14 N1 C13 -6.5(4) . . . . ? C15 C14 N1 C1 -172.7(3) . . . . ? N1 C13 N2 C16 177.3(3) . . . . ? Ni1 C13 N2 C16 -3.3(5) . . . . ? N1 C13 N2 C15 -0.4(4) . . . . ? Ni1 C13 N2 C15 179.0(3) . . . . ? C21 C16 N2 C13 -96.7(4) . . . . ? C17 C16 N2 C13 90.9(4) . . . . ? C21 C16 N2 C15 80.9(4) . . . . ? C17 C16 N2 C15 -91.5(4) . . . . ? C14 C15 N2 C13 -3.5(4) . . . . ? C14 C15 N2 C16 178.5(3) . . . . ? N4 C40 N3 C28 -171.9(3) . . . . ? Ni1 C40 N3 C28 5.1(5) . . . . ? N4 C40 N3 C41 -7.2(4) . . . . ? Ni1 C40 N3 C41 169.9(3) . . . . ? C29 C28 N3 C40 95.0(4) . . . . ? C33 C28 N3 C40 -92.6(4) . . . . ? C29 C28 N3 C41 -69.2(4) . . . . ? C33 C28 N3 C41 103.2(4) . . . . ? C42 C41 N3 C40 18.6(4) . . . . ? C42 C41 N3 C28 -175.0(3) . . . . ? N3 C40 N4 C43 -164.6(3) . . . . ? Ni1 C40 N4 C43 18.4(5) . . . . ? N3 C40 N4 C42 -8.1(4) . . . . ? Ni1 C40 N4 C42 174.9(3) . . . . ? C48 C43 N4 C40 69.7(5) . . . . ? C44 C43 N4 C40 -117.6(4) . . . . ? C48 C43 N4 C42 -86.3(4) . . . . ? C44 C43 N4 C42 86.4(4) . . . . ? C41 C42 N4 C40 19.2(4) . . . . ? C41 C42 N4 C43 178.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.856 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.090 #==END data_Ni(IBut)2 _database_code_depnum_ccdc_archive 'CCDC 662511' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H44 N4 Ni' _chemical_formula_sum 'C22 H44 N4 Ni' _chemical_formula_weight 423.32 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 Tetragonal _symmetry_space_group_name_H-M I41cd _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_Int_Tables_number 110 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' 'x, -y, z+1/2' '-x+1/2, y+1/2, z' '-y, -x+1/2, z+3/4' 'y+1/2, x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' 'x+1/2, -y+1/2, z+1' '-x+1, y+1, z+1/2' '-y+1/2, -x+1, z+5/4' 'y+1, x+1/2, z+3/4' _cell_length_a 11.6779(6) _cell_length_b 11.6779(6) _cell_length_c 35.091(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4785.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 105511 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'intense brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8525 _exptl_absorpt_correction_T_max 0.8795 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26139 _diffrn_reflns_av_R_equivalents 0.1150 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.58 _reflns_number_total 1408 _reflns_number_gt 1100 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _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. 1350 Friedel pairs were merged in the final cycle of refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+65.6720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1350 Friedel pairs' _refine_ls_abs_structure_Flack 0.11(12) _refine_ls_number_reflns 1408 _refine_ls_number_parameters 129 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.1837 _refine_ls_wR_factor_gt 0.1759 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1379(10) 0.1872(10) 0.3971(3) 0.032(3) Uani 1 1 d . . . C2 C -0.0543(11) 0.1671(11) 0.3636(3) 0.037(3) Uani 1 1 d . . . H2A H -0.0161 0.2393 0.3571 0.056 Uiso 1 1 calc R . . H2B H -0.0970 0.1392 0.3414 0.056 Uiso 1 1 calc R . . H2C H 0.0032 0.1102 0.3710 0.056 Uiso 1 1 calc R . . C3 C -0.2283(10) 0.2830(12) 0.3854(4) 0.037(3) Uani 1 1 d . . . H3A H -0.2759 0.3022 0.4075 0.056 Uiso 1 1 calc R . . H3B H -0.2770 0.2541 0.3647 0.056 Uiso 1 1 calc R . . H3C H -0.1876 0.3516 0.3767 0.056 Uiso 1 1 calc R . . C4 C -0.2021(10) 0.0767(11) 0.4062(4) 0.035(3) Uani 1 1 d . . . H4A H -0.1481 0.0195 0.4159 0.053 Uiso 1 1 calc R . . H4B H -0.2387 0.0475 0.3830 0.053 Uiso 1 1 calc R . . H4C H -0.2607 0.0921 0.4255 0.053 Uiso 1 1 calc R . . C5 C -0.0037(9) 0.1602(6) 0.4549(5) 0.0258(18) Uani 1 1 d . . . C6 C -0.0453(10) 0.3492(10) 0.4329(3) 0.031(3) Uani 1 1 d . . . H6A H -0.1139 0.3991 0.4323 0.038 Uiso 1 1 calc R . . H6B H 0.0071 0.3713 0.4120 0.038 Uiso 1 1 calc R . . C7 C 0.0146(9) 0.3538(9) 0.4717(3) 0.028(2) Uani 1 1 d . . . H7A H 0.0767 0.4116 0.4721 0.034 Uiso 1 1 calc R . . H7B H -0.0400 0.3696 0.4926 0.034 Uiso 1 1 calc R . . C8 C 0.1227(11) 0.1968(10) 0.5096(3) 0.036(3) Uani 1 1 d . . . C9 C 0.0306(12) 0.1701(13) 0.5402(3) 0.045(3) Uani 1 1 d . . . H9A H -0.0078 0.2412 0.5477 0.067 Uiso 1 1 calc R . . H9B H 0.0672 0.1355 0.5625 0.067 Uiso 1 1 calc R . . H9C H -0.0259 0.1167 0.5296 0.067 Uiso 1 1 calc R . . C10 C 0.1960(12) 0.0925(11) 0.5015(4) 0.043(3) Uani 1 1 d . . . H10A H 0.1468 0.0283 0.4941 0.065 Uiso 1 1 calc R . . H10B H 0.2394 0.0720 0.5244 0.065 Uiso 1 1 calc R . . H10C H 0.2493 0.1098 0.4807 0.065 Uiso 1 1 calc R . . C11 C 0.1985(12) 0.2925(12) 0.5224(4) 0.046(3) Uani 1 1 d . . . H11A H 0.2538 0.3104 0.5023 0.069 Uiso 1 1 calc R . . H11B H 0.2396 0.2694 0.5455 0.069 Uiso 1 1 calc R . . H11C H 0.1519 0.3603 0.5279 0.069 Uiso 1 1 calc R . . N1 N -0.0763(9) 0.2288(8) 0.4307(3) 0.030(2) Uani 1 1 d . . . N2 N 0.0615(8) 0.2323(8) 0.4736(2) 0.029(2) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.4523(2) 0.0329(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(6) 0.026(6) 0.030(6) 0.004(5) -0.002(5) -0.010(5) C2 0.041(7) 0.035(6) 0.036(7) -0.001(6) -0.008(5) 0.004(5) C3 0.035(6) 0.046(7) 0.031(6) 0.002(5) -0.001(5) 0.012(5) C4 0.025(5) 0.032(6) 0.050(7) -0.005(5) 0.004(5) -0.014(5) C5 0.031(4) 0.023(4) 0.024(4) 0.017(6) 0.005(5) 0.010(4) C6 0.029(6) 0.030(6) 0.035(6) 0.000(5) 0.004(5) -0.004(5) C7 0.026(5) 0.010(4) 0.048(6) -0.006(4) -0.001(5) -0.006(4) C8 0.040(7) 0.030(6) 0.037(7) 0.002(5) -0.004(5) -0.013(5) C9 0.051(8) 0.056(9) 0.028(7) 0.008(6) 0.004(6) -0.011(6) C10 0.064(9) 0.040(7) 0.027(6) -0.003(5) -0.010(6) -0.001(6) C11 0.045(8) 0.053(9) 0.040(7) 0.010(6) -0.004(6) -0.011(6) N1 0.043(5) 0.012(4) 0.035(5) -0.005(4) -0.002(4) 0.005(4) N2 0.038(5) 0.023(5) 0.025(5) -0.001(4) -0.004(4) 0.005(4) Ni1 0.0507(10) 0.0202(7) 0.0279(6) 0.000 0.000 0.0000(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.464(15) . ? C1 C4 1.526(15) . ? C1 C2 1.546(17) . ? C1 C3 1.592(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N2 1.312(15) . ? C5 N1 1.444(15) . ? C5 Ni1 1.874(8) . ? C6 N1 1.453(15) . ? C6 C7 1.532(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.522(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C11 1.494(18) . ? C8 N2 1.509(15) . ? C8 C10 1.516(18) . ? C8 C9 1.551(17) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? Ni1 C5 1.874(8) 10_444 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C4 110.7(10) . . ? N1 C1 C2 110.6(10) . . ? C4 C1 C2 110.0(10) . . ? N1 C1 C3 107.4(10) . . ? C4 C1 C3 108.8(10) . . ? C2 C1 C3 109.2(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 N1 106.3(6) . . ? N2 C5 Ni1 130.7(9) . . ? N1 C5 Ni1 122.6(10) . . ? N1 C6 C7 101.3(10) . . ? N1 C6 H6A 111.5 . . ? C7 C6 H6A 111.5 . . ? N1 C6 H6B 111.5 . . ? C7 C6 H6B 111.5 . . ? H6A C6 H6B 109.3 . . ? N2 C7 C6 99.9(10) . . ? N2 C7 H7A 111.8 . . ? C6 C7 H7A 111.8 . . ? N2 C7 H7B 111.8 . . ? C6 C7 H7B 111.8 . . ? H7A C7 H7B 109.5 . . ? C11 C8 N2 109.1(10) . . ? C11 C8 C10 108.8(11) . . ? N2 C8 C10 109.3(10) . . ? C11 C8 C9 110.7(11) . . ? N2 C8 C9 107.8(10) . . ? C10 C8 C9 111.1(11) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 N1 C6 111.0(9) . . ? C5 N1 C1 125.3(10) . . ? C6 N1 C1 119.1(10) . . ? C5 N2 C8 121.2(10) . . ? C5 N2 C7 111.5(9) . . ? C8 N2 C7 117.7(9) . . ? C5 Ni1 C5 174.5(11) . 10_444 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C6 C7 N2 29.2(8) . . . . ? N2 C5 N1 C6 5.2(15) . . . . ? Ni1 C5 N1 C6 -168.1(9) . . . . ? N2 C5 N1 C1 160.9(10) . . . . ? Ni1 C5 N1 C1 -12.3(17) . . . . ? C7 C6 N1 C5 -23.0(12) . . . . ? C7 C6 N1 C1 179.5(9) . . . . ? C4 C1 N1 C5 48.3(16) . . . . ? C2 C1 N1 C5 -73.9(14) . . . . ? C3 C1 N1 C5 166.9(11) . . . . ? C4 C1 N1 C6 -157.8(11) . . . . ? C2 C1 N1 C6 80.0(13) . . . . ? C3 C1 N1 C6 -39.1(14) . . . . ? N1 C5 N2 C8 161.4(9) . . . . ? Ni1 C5 N2 C8 -26.1(18) . . . . ? N1 C5 N2 C7 16.1(15) . . . . ? Ni1 C5 N2 C7 -171.4(10) . . . . ? C11 C8 N2 C5 174.7(11) . . . . ? C10 C8 N2 C5 55.8(14) . . . . ? C9 C8 N2 C5 -65.1(14) . . . . ? C11 C8 N2 C7 -42.1(14) . . . . ? C10 C8 N2 C7 -160.9(10) . . . . ? C9 C8 N2 C7 78.2(12) . . . . ? C6 C7 N2 C5 -29.6(12) . . . . ? C6 C7 N2 C8 -176.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.941 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.100 #==END data_Ni[I(Me2)Pri]2(CH3)2 _database_code_depnum_ccdc_archive 'CCDC 662512' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H46 N4 Ni' _chemical_formula_sum 'C24 H46 N4 Ni' _chemical_formula_weight 449.36 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 15.6502(2) _cell_length_b 9.70010(10) _cell_length_c 17.3931(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.3870(10) _cell_angle_gamma 90.00 _cell_volume 2557.61(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 55658 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9128 _exptl_absorpt_correction_T_max 0.9903 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31971 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5850 _reflns_number_gt 4872 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.8038P] 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 5850 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.16850(15) 0.4692(3) -0.01345(13) 0.0231(5) Uani 1 1 d . . . H1 H 0.1829 0.3729 0.0060 0.028 Uiso 1 1 calc R . . C2 C 0.24878(17) 0.5229(3) -0.03959(15) 0.0290(6) Uani 1 1 d . . . H2A H 0.2399 0.6202 -0.0545 0.044 Uiso 1 1 calc R . . H2B H 0.2563 0.4694 -0.0853 0.044 Uiso 1 1 calc R . . H2C H 0.3016 0.5133 0.0042 0.044 Uiso 1 1 calc R . . C3 C 0.08668(17) 0.4598(3) -0.08227(15) 0.0339(6) Uani 1 1 d . . . H3A H 0.0351 0.4392 -0.0618 0.051 Uiso 1 1 calc R . . H3B H 0.0946 0.3863 -0.1185 0.051 Uiso 1 1 calc R . . H3C H 0.0776 0.5478 -0.1108 0.051 Uiso 1 1 calc R . . C4 C 0.17609(14) 0.4952(2) 0.12936(13) 0.0186(4) Uani 1 1 d . . . C5 C 0.12329(16) 0.6843(3) 0.05353(14) 0.0240(5) Uani 1 1 d . . . C6 C 0.12551(16) 0.7170(3) 0.12961(14) 0.0240(5) Uani 1 1 d . . . C7 C 0.17074(15) 0.5858(3) 0.26185(13) 0.0223(5) Uani 1 1 d . . . H7 H 0.1948 0.4911 0.2758 0.027 Uiso 1 1 calc R . . C8 C 0.23903(17) 0.6866(3) 0.30845(15) 0.0309(6) Uani 1 1 d . . . H8A H 0.2924 0.6825 0.2887 0.046 Uiso 1 1 calc R . . H8B H 0.2537 0.6618 0.3648 0.046 Uiso 1 1 calc R . . H8C H 0.2149 0.7803 0.3018 0.046 Uiso 1 1 calc R . . C9 C 0.08338(17) 0.5935(3) 0.28552(15) 0.0316(6) Uani 1 1 d . . . H9A H 0.0629 0.6894 0.2823 0.047 Uiso 1 1 calc R . . H9B H 0.0916 0.5599 0.3400 0.047 Uiso 1 1 calc R . . H9C H 0.0394 0.5363 0.2494 0.047 Uiso 1 1 calc R . . C10 C 0.0904(2) 0.7701(3) -0.01911(15) 0.0352(6) Uani 1 1 d . . . H10A H 0.0329 0.7355 -0.0489 0.053 Uiso 1 1 calc R . . H10B H 0.1324 0.7651 -0.0525 0.053 Uiso 1 1 calc R . . H10C H 0.0845 0.8661 -0.0036 0.053 Uiso 1 1 calc R . . C11 C 0.0947(2) 0.8477(3) 0.15983(17) 0.0377(7) Uani 1 1 d . . . H11A H 0.0765 0.9133 0.1160 0.057 Uiso 1 1 calc R . . H11B H 0.1429 0.8875 0.2009 0.057 Uiso 1 1 calc R . . H11C H 0.0446 0.8277 0.1825 0.057 Uiso 1 1 calc R . . C12 C 0.4034(2) 0.5205(3) 0.20735(16) 0.0357(6) Uani 1 1 d . . . H12 H 0.3453 0.5142 0.2215 0.043 Uiso 1 1 calc R . . C13 C 0.4690(3) 0.4977(5) 0.2831(2) 0.0676(12) Uani 1 1 d . . . H13A H 0.4573 0.4093 0.3058 0.101 Uiso 1 1 calc R . . H13B H 0.4651 0.5723 0.3200 0.101 Uiso 1 1 calc R . . H13C H 0.5282 0.4964 0.2738 0.101 Uiso 1 1 calc R . . C14 C 0.4022(3) 0.6588(3) 0.1708(2) 0.0513(9) Uani 1 1 d . . . H14A H 0.4552 0.6704 0.1511 0.077 Uiso 1 1 calc R . . H14B H 0.4010 0.7298 0.2107 0.077 Uiso 1 1 calc R . . H14C H 0.3497 0.6676 0.1266 0.077 Uiso 1 1 calc R . . C15 C 0.32745(15) 0.3259(2) 0.12952(13) 0.0204(5) Uani 1 1 d . . . C16 C 0.46173(16) 0.3729(3) 0.10613(15) 0.0273(5) Uani 1 1 d . . . C17 C 0.42642(16) 0.2670(3) 0.05847(15) 0.0275(5) Uani 1 1 d . . . C18 C 0.28135(17) 0.1280(3) 0.03893(15) 0.0283(5) Uani 1 1 d . . . H18 H 0.2273 0.1438 0.0586 0.034 Uiso 1 1 calc R . . C19 C 0.2519(2) 0.1330(3) -0.05159(16) 0.0405(7) Uani 1 1 d . . . H19A H 0.2411 0.2289 -0.0690 0.061 Uiso 1 1 calc R . . H19B H 0.1975 0.0795 -0.0699 0.061 Uiso 1 1 calc R . . H19C H 0.2982 0.0937 -0.0739 0.061 Uiso 1 1 calc R . . C20 C 0.3162(2) -0.0141(3) 0.06864(18) 0.0395(7) Uani 1 1 d . . . H20A H 0.3683 -0.0355 0.0492 0.059 Uiso 1 1 calc R . . H20B H 0.2704 -0.0834 0.0490 0.059 Uiso 1 1 calc R . . H20C H 0.3322 -0.0147 0.1268 0.059 Uiso 1 1 calc R . . C21 C 0.54928(18) 0.4414(3) 0.1142(2) 0.0438(7) Uani 1 1 d . . . H21A H 0.5821 0.3933 0.0811 0.066 Uiso 1 1 calc R . . H21B H 0.5829 0.4382 0.1699 0.066 Uiso 1 1 calc R . . H21C H 0.5401 0.5377 0.0971 0.066 Uiso 1 1 calc R . . C22 C 0.4629(2) 0.1942(3) -0.0022(2) 0.0464(8) Uani 1 1 d . . . H22A H 0.4276 0.2175 -0.0555 0.070 Uiso 1 1 calc R . . H22B H 0.4609 0.0944 0.0059 0.070 Uiso 1 1 calc R . . H22C H 0.5241 0.2230 0.0032 0.070 Uiso 1 1 calc R . . C23 C 0.11726(16) 0.2715(3) 0.20303(15) 0.0275(5) Uani 1 1 d . . . H23A H 0.0950 0.1828 0.1793 0.041 Uiso 1 1 calc R . . H23B H 0.0726 0.3429 0.1847 0.041 Uiso 1 1 calc R . . H23C H 0.1302 0.2644 0.2610 0.041 Uiso 1 1 calc R . . C24 C 0.28085(17) 0.1656(3) 0.23954(15) 0.0314(6) Uani 1 1 d . . . H24A H 0.3385 0.1451 0.2296 0.047 Uiso 1 1 calc R . . H24B H 0.2429 0.0841 0.2275 0.047 Uiso 1 1 calc R . . H24C H 0.2886 0.1910 0.2954 0.047 Uiso 1 1 calc R . . N1 N 0.15396(12) 0.5486(2) 0.05436(11) 0.0197(4) Uani 1 1 d . . . N2 N 0.15784(12) 0.6012(2) 0.17516(11) 0.0198(4) Uani 1 1 d . . . N3 N 0.40021(13) 0.4077(2) 0.14905(11) 0.0231(4) Uani 1 1 d . . . N4 N 0.34424(13) 0.2390(2) 0.07317(11) 0.0216(4) Uani 1 1 d . . . Ni1 Ni 0.225518(19) 0.32032(3) 0.171227(17) 0.01914(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0267(12) 0.0253(13) 0.0191(11) -0.0012(9) 0.0092(9) 0.0014(10) C2 0.0294(13) 0.0356(15) 0.0249(12) 0.0055(11) 0.0121(10) 0.0019(11) C3 0.0308(14) 0.0448(17) 0.0248(12) -0.0079(12) 0.0042(11) 0.0008(12) C4 0.0162(10) 0.0226(12) 0.0178(10) -0.0011(9) 0.0054(8) -0.0015(9) C5 0.0272(12) 0.0203(12) 0.0250(11) 0.0030(10) 0.0074(10) 0.0018(10) C6 0.0257(12) 0.0203(12) 0.0255(12) 0.0001(9) 0.0052(10) 0.0030(10) C7 0.0258(12) 0.0241(12) 0.0167(10) -0.0022(9) 0.0048(9) 0.0025(10) C8 0.0322(13) 0.0334(15) 0.0251(12) -0.0081(11) 0.0035(10) 0.0000(12) C9 0.0287(13) 0.0432(16) 0.0248(12) -0.0014(11) 0.0104(10) 0.0031(12) C10 0.0461(16) 0.0303(14) 0.0279(13) 0.0068(11) 0.0069(12) 0.0063(13) C11 0.0529(18) 0.0251(14) 0.0334(14) -0.0014(11) 0.0073(13) 0.0128(13) C12 0.0518(17) 0.0238(14) 0.0300(14) -0.0054(11) 0.0072(13) -0.0071(13) C13 0.077(3) 0.075(3) 0.0393(18) -0.0160(18) -0.0071(18) 0.026(2) C14 0.086(3) 0.0243(15) 0.0471(18) -0.0066(13) 0.0242(18) -0.0065(16) C15 0.0232(11) 0.0175(11) 0.0199(10) 0.0018(9) 0.0045(9) 0.0040(9) C16 0.0221(12) 0.0271(13) 0.0337(13) 0.0063(11) 0.0089(10) -0.0003(10) C17 0.0268(12) 0.0250(13) 0.0357(14) 0.0061(11) 0.0171(11) 0.0079(10) C18 0.0309(13) 0.0239(13) 0.0297(13) -0.0060(10) 0.0070(11) -0.0050(11) C19 0.0528(18) 0.0349(16) 0.0310(14) -0.0125(12) 0.0048(13) -0.0012(14) C20 0.0481(17) 0.0222(14) 0.0484(17) -0.0033(12) 0.0121(14) -0.0049(13) C21 0.0276(14) 0.0434(18) 0.062(2) 0.0100(15) 0.0135(14) -0.0042(13) C22 0.0556(19) 0.0331(16) 0.066(2) -0.0016(15) 0.0447(17) 0.0064(14) C23 0.0275(12) 0.0265(13) 0.0307(13) 0.0024(11) 0.0112(11) -0.0009(11) C24 0.0339(14) 0.0300(14) 0.0325(13) 0.0072(11) 0.0121(11) 0.0074(12) N1 0.0211(9) 0.0201(10) 0.0182(9) 0.0011(8) 0.0056(8) 0.0004(8) N2 0.0218(9) 0.0183(10) 0.0193(9) -0.0005(8) 0.0050(8) 0.0013(8) N3 0.0270(10) 0.0194(10) 0.0226(10) 0.0005(8) 0.0054(8) -0.0014(8) N4 0.0236(10) 0.0176(10) 0.0253(10) -0.0015(8) 0.0094(8) 0.0000(8) Ni1 0.02114(15) 0.01833(15) 0.01935(14) 0.00186(12) 0.00764(11) 0.00192(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.473(3) . ? C1 C3 1.523(3) . ? C1 C2 1.530(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.366(3) . ? C4 N2 1.373(3) . ? C4 Ni1 1.930(2) . ? C5 C6 1.353(3) . ? C5 N1 1.400(3) . ? C5 C10 1.494(3) . ? C6 N2 1.395(3) . ? C6 C11 1.497(3) . ? C7 N2 1.478(3) . ? C7 C9 1.525(3) . ? C7 C8 1.525(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.471(4) . ? C12 C14 1.483(4) . ? C12 N3 1.484(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N3 1.360(3) . ? C15 N4 1.366(3) . ? C15 Ni1 1.910(2) . ? C16 C17 1.349(4) . ? C16 N3 1.398(3) . ? C16 C21 1.498(4) . ? C17 N4 1.399(3) . ? C17 C22 1.497(4) . ? C18 N4 1.481(3) . ? C18 C20 1.524(4) . ? C18 C19 1.527(4) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Ni1 1.966(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Ni1 1.975(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C3 113.2(2) . . ? N1 C1 C2 111.2(2) . . ? C3 C1 C2 112.3(2) . . ? N1 C1 H1 106.6 . . ? C3 C1 H1 106.6 . . ? C2 C1 H1 106.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 103.32(19) . . ? N1 C4 Ni1 132.56(17) . . ? N2 C4 Ni1 124.09(16) . . ? C6 C5 N1 106.6(2) . . ? C6 C5 C10 128.1(2) . . ? N1 C5 C10 125.3(2) . . ? C5 C6 N2 106.5(2) . . ? C5 C6 C11 127.6(2) . . ? N2 C6 C11 125.8(2) . . ? N2 C7 C9 111.48(19) . . ? N2 C7 C8 112.2(2) . . ? C9 C7 C8 112.5(2) . . ? N2 C7 H7 106.7 . . ? C9 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? 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 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 116.8(3) . . ? C13 C12 N3 113.5(3) . . ? C14 C12 N3 112.3(2) . . ? C13 C12 H12 104.2 . . ? C14 C12 H12 104.2 . . ? N3 C12 H12 104.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 N4 103.92(19) . . ? N3 C15 Ni1 130.39(17) . . ? N4 C15 Ni1 125.64(17) . . ? C17 C16 N3 106.3(2) . . ? C17 C16 C21 128.4(3) . . ? N3 C16 C21 125.3(2) . . ? C16 C17 N4 106.9(2) . . ? C16 C17 C22 128.5(2) . . ? N4 C17 C22 124.5(2) . . ? N4 C18 C20 112.0(2) . . ? N4 C18 C19 113.1(2) . . ? C20 C18 C19 111.7(2) . . ? N4 C18 H18 106.5 . . ? C20 C18 H18 106.5 . . ? C19 C18 H18 106.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Ni1 C23 H23A 109.5 . . ? Ni1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Ni1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Ni1 C24 H24A 109.5 . . ? Ni1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Ni1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 N1 C5 111.80(19) . . ? C4 N1 C1 120.89(19) . . ? C5 N1 C1 127.18(19) . . ? C4 N2 C6 111.81(18) . . ? C4 N2 C7 121.41(19) . . ? C6 N2 C7 126.77(19) . . ? C15 N3 C16 111.7(2) . . ? C15 N3 C12 119.0(2) . . ? C16 N3 C12 129.2(2) . . ? C15 N4 C17 111.2(2) . . ? C15 N4 C18 120.65(19) . . ? C17 N4 C18 128.1(2) . . ? C15 Ni1 C4 97.25(9) . . ? C15 Ni1 C23 166.61(11) . . ? C4 Ni1 C23 91.45(10) . . ? C15 Ni1 C24 88.12(10) . . ? C4 Ni1 C24 165.73(10) . . ? C23 Ni1 C24 85.84(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C5 C6 N2 0.3(3) . . . . ? C10 C5 C6 N2 177.2(2) . . . . ? N1 C5 C6 C11 -176.4(3) . . . . ? C10 C5 C6 C11 0.5(5) . . . . ? N3 C16 C17 N4 -0.1(3) . . . . ? C21 C16 C17 N4 179.2(3) . . . . ? N3 C16 C17 C22 177.2(3) . . . . ? C21 C16 C17 C22 -3.5(5) . . . . ? N2 C4 N1 C5 0.3(2) . . . . ? Ni1 C4 N1 C5 -177.42(18) . . . . ? N2 C4 N1 C1 176.52(19) . . . . ? Ni1 C4 N1 C1 -1.2(3) . . . . ? C6 C5 N1 C4 -0.4(3) . . . . ? C10 C5 N1 C4 -177.4(2) . . . . ? C6 C5 N1 C1 -176.3(2) . . . . ? C10 C5 N1 C1 6.7(4) . . . . ? C3 C1 N1 C4 128.4(2) . . . . ? C2 C1 N1 C4 -104.1(2) . . . . ? C3 C1 N1 C5 -56.0(3) . . . . ? C2 C1 N1 C5 71.4(3) . . . . ? N1 C4 N2 C6 -0.2(2) . . . . ? Ni1 C4 N2 C6 177.86(16) . . . . ? N1 C4 N2 C7 178.65(19) . . . . ? Ni1 C4 N2 C7 -3.3(3) . . . . ? C5 C6 N2 C4 -0.1(3) . . . . ? C11 C6 N2 C4 176.7(2) . . . . ? C5 C6 N2 C7 -178.8(2) . . . . ? C11 C6 N2 C7 -2.1(4) . . . . ? C9 C7 N2 C4 -114.7(2) . . . . ? C8 C7 N2 C4 118.1(2) . . . . ? C9 C7 N2 C6 63.9(3) . . . . ? C8 C7 N2 C6 -63.3(3) . . . . ? N4 C15 N3 C16 -0.2(3) . . . . ? Ni1 C15 N3 C16 177.10(18) . . . . ? N4 C15 N3 C12 177.4(2) . . . . ? Ni1 C15 N3 C12 -5.3(3) . . . . ? C17 C16 N3 C15 0.2(3) . . . . ? C21 C16 N3 C15 -179.1(2) . . . . ? C17 C16 N3 C12 -177.1(2) . . . . ? C21 C16 N3 C12 3.6(4) . . . . ? C13 C12 N3 C15 111.8(3) . . . . ? C14 C12 N3 C15 -113.1(3) . . . . ? C13 C12 N3 C16 -71.1(4) . . . . ? C14 C12 N3 C16 64.1(4) . . . . ? N3 C15 N4 C17 0.2(3) . . . . ? Ni1 C15 N4 C17 -177.33(17) . . . . ? N3 C15 N4 C18 177.1(2) . . . . ? Ni1 C15 N4 C18 -0.3(3) . . . . ? C16 C17 N4 C15 0.0(3) . . . . ? C22 C17 N4 C15 -177.4(2) . . . . ? C16 C17 N4 C18 -176.7(2) . . . . ? C22 C17 N4 C18 5.8(4) . . . . ? C20 C18 N4 C15 -107.5(3) . . . . ? C19 C18 N4 C15 125.3(2) . . . . ? C20 C18 N4 C17 69.0(3) . . . . ? C19 C18 N4 C17 -58.3(3) . . . . ? N3 C15 Ni1 C4 69.2(2) . . . . ? N4 C15 Ni1 C4 -114.0(2) . . . . ? N3 C15 Ni1 C23 -160.7(4) . . . . ? N4 C15 Ni1 C23 16.1(6) . . . . ? N3 C15 Ni1 C24 -97.5(2) . . . . ? N4 C15 Ni1 C24 79.3(2) . . . . ? N1 C4 Ni1 C15 54.8(2) . . . . ? N2 C4 Ni1 C15 -122.57(19) . . . . ? N1 C4 Ni1 C23 -115.0(2) . . . . ? N2 C4 Ni1 C23 67.6(2) . . . . ? N1 C4 Ni1 C24 166.3(3) . . . . ? N2 C4 Ni1 C24 -11.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.104 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.069 #==END