Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Guo-Xin Jin' _publ_contact_author_address ; Chemistry department Fudan University, Inorganic Chemistry Institute Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis, Molecular Structure and Norbornene Polymerization Behavior of Three-Coordinate Nickel (I) Complexes with Chelating Anilido-Imine Ligands ; loop_ _publ_author_name 'Guo-Xin Jin' 'Xia Meng' 'Hai-Yu Wang' data_f50308c _database_code_depnum_ccdc_archive 'CCDC 289503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H54 N2 Ni P' _chemical_formula_weight 760.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 10.695(3) _cell_length_b 23.306(6) _cell_length_c 17.182(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.975(4) _cell_angle_gamma 90.00 _cell_volume 4259.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 808 _cell_measurement_theta_min 2.515 _cell_measurement_theta_max 17.798 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8794 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17709 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7479 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1559P)^2^+3.1794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7479 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2658 _refine_ls_wR_factor_gt 0.2292 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.39620(7) 0.13533(3) 0.31070(4) 0.0492(3) Uani 1 1 d . . . N1 N 0.4890(4) 0.19027(15) 0.3757(2) 0.0348(9) Uani 1 1 d . . . N2 N 0.5391(4) 0.08238(16) 0.3074(2) 0.0409(10) Uani 1 1 d . . . P1 P 0.20899(17) 0.10800(6) 0.25294(9) 0.0566(5) Uani 1 1 d . . . C1 C 0.6034(5) 0.1841(2) 0.4154(3) 0.0379(11) Uani 1 1 d . . . C2 C 0.6585(6) 0.2259(2) 0.4686(4) 0.0531(15) Uani 1 1 d . . . H2 H 0.6149 0.2598 0.4753 0.064 Uiso 1 1 calc R . . C3 C 0.7725(6) 0.2182(3) 0.5097(4) 0.0640(18) Uani 1 1 d . . . H3 H 0.8038 0.2464 0.5448 0.077 Uiso 1 1 calc R . . C4 C 0.8429(6) 0.1696(3) 0.5007(4) 0.0659(18) Uani 1 1 d . . . H4 H 0.9204 0.1648 0.5299 0.079 Uiso 1 1 calc R . . C5 C 0.7978(6) 0.1287(3) 0.4486(4) 0.0546(15) Uani 1 1 d . . . H5 H 0.8461 0.0963 0.4416 0.066 Uiso 1 1 calc R . . C6 C 0.6796(5) 0.1345(2) 0.4052(3) 0.0396(12) Uani 1 1 d . . . C7 C 0.6434(6) 0.0896(2) 0.3492(3) 0.0457(13) Uani 1 1 d . . . H7 H 0.7048 0.0622 0.3429 0.055 Uiso 1 1 calc R . . C8 C 0.5349(6) 0.0348(2) 0.2549(3) 0.0491(14) Uani 1 1 d . . . C9 C 0.5593(7) 0.0436(3) 0.1778(4) 0.0607(16) Uani 1 1 d . . . C10 C 0.5605(7) -0.0040(3) 0.1294(4) 0.074(2) Uani 1 1 d . . . H10 H 0.5784 0.0007 0.0779 0.089 Uiso 1 1 calc R . . C11 C 0.5360(8) -0.0577(3) 0.1558(4) 0.080(2) Uani 1 1 d . . . H11 H 0.5394 -0.0891 0.1226 0.096 Uiso 1 1 calc R . . C12 C 0.5070(7) -0.0655(3) 0.2291(4) 0.072(2) Uani 1 1 d . . . H12 H 0.4861 -0.1022 0.2449 0.086 Uiso 1 1 calc R . . C13 C 0.5070(6) -0.0205(2) 0.2825(4) 0.0540(15) Uani 1 1 d . . . C14 C 0.4762(7) -0.0303(3) 0.3653(4) 0.069(2) Uani 1 1 d . . . H14 H 0.4444 0.0060 0.3842 0.083 Uiso 1 1 calc R . . C15 C 0.3745(9) -0.0753(3) 0.3712(5) 0.092(3) Uani 1 1 d . . . H15A H 0.3082 -0.0696 0.3297 0.138 Uiso 1 1 calc R . . H15B H 0.3412 -0.0717 0.4207 0.138 Uiso 1 1 calc R . . H15C H 0.4098 -0.1129 0.3668 0.138 Uiso 1 1 calc R . . C16 C 0.5931(10) -0.0467(4) 0.4206(5) 0.101(3) Uani 1 1 d . . . H16A H 0.6342 -0.0788 0.3992 0.152 Uiso 1 1 calc R . . H16B H 0.5682 -0.0569 0.4709 0.152 Uiso 1 1 calc R . . H16C H 0.6499 -0.0147 0.4261 0.152 Uiso 1 1 calc R . . C17 C 0.5856(9) 0.1032(3) 0.1484(4) 0.085(2) Uani 1 1 d . . . H17 H 0.5605 0.1310 0.1866 0.102 Uiso 1 1 calc R . . C18 C 0.5125(10) 0.1167(4) 0.0691(6) 0.109(3) Uani 1 1 d . . . H18A H 0.5476 0.0953 0.0289 0.164 Uiso 1 1 calc R . . H18B H 0.5183 0.1570 0.0585 0.164 Uiso 1 1 calc R . . H18C H 0.4259 0.1062 0.0703 0.164 Uiso 1 1 calc R . . C19 C 0.7262(11) 0.1106(5) 0.1426(7) 0.156(6) Uani 1 1 d . . . H19A H 0.7727 0.0965 0.1895 0.234 Uiso 1 1 calc R . . H19B H 0.7447 0.1505 0.1362 0.234 Uiso 1 1 calc R . . H19C H 0.7495 0.0894 0.0984 0.234 Uiso 1 1 calc R . . C20 C 0.4253(5) 0.2442(2) 0.3824(3) 0.0387(12) Uani 1 1 d . . . C21 C 0.4501(5) 0.2887(2) 0.3324(3) 0.0470(14) Uani 1 1 d . . . C22 C 0.3823(7) 0.3396(3) 0.3362(4) 0.0639(18) Uani 1 1 d . . . H22 H 0.3975 0.3697 0.3030 0.077 Uiso 1 1 calc R . . C23 C 0.2953(7) 0.3462(3) 0.3868(5) 0.073(2) Uani 1 1 d . . . H23 H 0.2502 0.3803 0.3875 0.088 Uiso 1 1 calc R . . C24 C 0.2733(6) 0.3024(3) 0.4376(4) 0.0682(19) Uani 1 1 d . . . H24 H 0.2142 0.3077 0.4730 0.082 Uiso 1 1 calc R . . C25 C 0.3376(5) 0.2502(2) 0.4370(3) 0.0499(14) Uani 1 1 d . . . C26 C 0.5511(6) 0.2834(3) 0.2758(4) 0.0634(17) Uani 1 1 d . . . H26 H 0.5955 0.2471 0.2867 0.076 Uiso 1 1 calc R . . C27 C 0.4904(10) 0.2817(7) 0.1918(5) 0.159(6) Uani 1 1 d . . . H27A H 0.4400 0.3154 0.1812 0.239 Uiso 1 1 calc R . . H27B H 0.4381 0.2482 0.1843 0.239 Uiso 1 1 calc R . . H27C H 0.5546 0.2803 0.1567 0.239 Uiso 1 1 calc R . . C28 C 0.6462(9) 0.3311(4) 0.2850(7) 0.125(4) Uani 1 1 d . . . H28A H 0.7066 0.3259 0.2479 0.188 Uiso 1 1 calc R . . H28B H 0.6884 0.3304 0.3371 0.188 Uiso 1 1 calc R . . H28C H 0.6045 0.3673 0.2758 0.188 Uiso 1 1 calc R . . C29 C 0.3175(6) 0.2041(3) 0.4950(3) 0.0564(15) Uani 1 1 d . . . H29 H 0.3645 0.1703 0.4808 0.068 Uiso 1 1 calc R . . C30 C 0.3683(9) 0.2211(4) 0.5770(4) 0.093(3) Uani 1 1 d . . . H30A H 0.4505 0.2375 0.5763 0.140 Uiso 1 1 calc R . . H30B H 0.3734 0.1878 0.6101 0.140 Uiso 1 1 calc R . . H30C H 0.3132 0.2488 0.5968 0.140 Uiso 1 1 calc R . . C31 C 0.1799(8) 0.1870(5) 0.4919(5) 0.112(3) Uani 1 1 d . . . H31A H 0.1307 0.2198 0.5035 0.168 Uiso 1 1 calc R . . H31B H 0.1706 0.1574 0.5297 0.168 Uiso 1 1 calc R . . H31C H 0.1516 0.1730 0.4405 0.168 Uiso 1 1 calc R . . C32 C 0.1046(6) 0.1705(2) 0.2614(3) 0.0497(14) Uani 1 1 d . . . C33 C 0.1528(6) 0.2229(3) 0.2435(4) 0.0623(17) Uani 1 1 d . . . H33 H 0.2307 0.2247 0.2240 0.075 Uiso 1 1 calc R . . C34 C 0.0893(7) 0.2715(3) 0.2537(5) 0.069(2) Uani 1 1 d . . . H34 H 0.1226 0.3065 0.2397 0.082 Uiso 1 1 calc R . . C35 C -0.0221(7) 0.2704(2) 0.2840(4) 0.0641(18) Uani 1 1 d . . . H35 H -0.0636 0.3045 0.2926 0.077 Uiso 1 1 calc R . . C36 C -0.0741(6) 0.2191(3) 0.3022(4) 0.0644(17) Uani 1 1 d . . . H36 H -0.1518 0.2179 0.3218 0.077 Uiso 1 1 calc R . . C37 C -0.0090(6) 0.1689(2) 0.2908(4) 0.0575(16) Uani 1 1 d . . . H37 H -0.0431 0.1338 0.3033 0.069 Uiso 1 1 calc R . . C38 C 0.1233(7) 0.0526(3) 0.3001(4) 0.0654(18) Uani 1 1 d . . . C39 C 0.1578(9) 0.0406(4) 0.3780(5) 0.094(3) Uani 1 1 d . . . H39 H 0.2265 0.0595 0.4039 0.112 Uiso 1 1 calc R . . C40 C 0.0944(13) 0.0020(6) 0.4179(8) 0.133(4) Uani 1 1 d . . . H40 H 0.1187 -0.0049 0.4706 0.160 Uiso 1 1 calc R . . C41 C -0.0052(15) -0.0267(4) 0.3802(9) 0.126(5) Uani 1 1 d . . . H41 H -0.0461 -0.0543 0.4074 0.151 Uiso 1 1 calc R . . C42 C -0.0482(12) -0.0156(4) 0.3007(8) 0.131(4) Uani 1 1 d . . . H42 H -0.1185 -0.0336 0.2751 0.158 Uiso 1 1 calc R . . C43 C 0.0236(9) 0.0244(3) 0.2637(5) 0.084(2) Uani 1 1 d . . . H43 H 0.0011 0.0320 0.2110 0.101 Uiso 1 1 calc R . . C44 C 0.1770(6) 0.0872(2) 0.1490(3) 0.0520(14) Uani 1 1 d . . . C45 C 0.1101(8) 0.1207(3) 0.0935(4) 0.077(2) Uani 1 1 d . . . H45 H 0.0770 0.1555 0.1082 0.092 Uiso 1 1 calc R . . C46 C 0.0915(9) 0.1035(4) 0.0167(5) 0.096(3) Uani 1 1 d . . . H46 H 0.0443 0.1262 -0.0201 0.115 Uiso 1 1 calc R . . C47 C 0.1419(9) 0.0537(4) -0.0054(5) 0.093(3) Uani 1 1 d . . . H47 H 0.1315 0.0427 -0.0577 0.112 Uiso 1 1 calc R . . C48 C 0.2083(9) 0.0193(3) 0.0487(5) 0.086(2) Uani 1 1 d . . . H48 H 0.2397 -0.0157 0.0335 0.103 Uiso 1 1 calc R . . C49 C 0.2285(7) 0.0366(3) 0.1256(4) 0.0678(18) Uani 1 1 d . . . H49 H 0.2769 0.0141 0.1619 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0536(5) 0.0455(4) 0.0470(5) -0.0052(3) -0.0011(3) 0.0028(3) N1 0.041(2) 0.029(2) 0.034(2) -0.0039(17) 0.0023(18) 0.0024(17) N2 0.059(3) 0.029(2) 0.036(2) 0.0019(17) 0.009(2) 0.003(2) P1 0.0823(12) 0.0449(8) 0.0432(9) 0.0033(7) 0.0093(8) 0.0124(8) C1 0.044(3) 0.037(3) 0.032(3) 0.001(2) 0.003(2) -0.005(2) C2 0.057(4) 0.043(3) 0.058(4) -0.007(3) -0.004(3) 0.005(3) C3 0.063(4) 0.064(4) 0.060(4) -0.010(3) -0.018(3) -0.008(3) C4 0.050(4) 0.082(5) 0.062(4) 0.010(4) -0.008(3) -0.001(3) C5 0.053(3) 0.063(4) 0.049(4) 0.016(3) 0.007(3) 0.010(3) C6 0.042(3) 0.039(3) 0.038(3) 0.010(2) 0.006(2) 0.003(2) C7 0.063(4) 0.032(3) 0.045(3) 0.010(2) 0.020(3) 0.015(3) C8 0.071(4) 0.037(3) 0.041(3) -0.003(2) 0.016(3) 0.008(3) C9 0.090(5) 0.048(3) 0.047(4) -0.005(3) 0.023(3) -0.002(3) C10 0.110(6) 0.069(4) 0.048(4) -0.016(3) 0.033(4) -0.006(4) C11 0.123(7) 0.052(4) 0.066(5) -0.027(3) 0.020(4) 0.002(4) C12 0.108(6) 0.039(3) 0.073(5) -0.016(3) 0.028(4) -0.004(3) C13 0.077(4) 0.034(3) 0.053(4) -0.007(2) 0.019(3) 0.004(3) C14 0.114(6) 0.039(3) 0.060(4) 0.004(3) 0.034(4) 0.002(3) C15 0.126(7) 0.067(5) 0.091(6) 0.006(4) 0.048(5) -0.011(5) C16 0.143(8) 0.091(6) 0.068(5) 0.025(4) 0.006(5) 0.002(6) C17 0.145(8) 0.067(4) 0.050(4) 0.000(3) 0.043(4) -0.019(5) C18 0.125(8) 0.112(7) 0.095(7) 0.038(6) 0.027(6) -0.010(6) C19 0.153(11) 0.141(9) 0.157(11) 0.063(8) -0.056(9) -0.085(8) C20 0.040(3) 0.037(3) 0.038(3) -0.010(2) -0.005(2) 0.003(2) C21 0.053(3) 0.038(3) 0.047(3) 0.001(2) -0.008(3) 0.000(2) C22 0.073(4) 0.041(3) 0.073(5) 0.001(3) -0.014(4) 0.011(3) C23 0.084(5) 0.054(4) 0.078(5) -0.020(4) -0.012(4) 0.029(4) C24 0.066(4) 0.068(4) 0.070(5) -0.023(4) 0.006(3) 0.025(3) C25 0.052(4) 0.053(3) 0.043(3) -0.012(3) -0.002(3) 0.010(3) C26 0.069(4) 0.057(4) 0.063(4) 0.018(3) 0.004(3) 0.009(3) C27 0.102(7) 0.331(18) 0.047(5) 0.006(8) 0.018(5) -0.035(9) C28 0.075(6) 0.103(7) 0.201(12) 0.024(7) 0.029(6) -0.019(5) C29 0.061(4) 0.061(4) 0.049(4) -0.009(3) 0.014(3) 0.003(3) C30 0.123(7) 0.095(6) 0.057(5) 0.009(4) -0.011(4) -0.014(5) C31 0.089(6) 0.160(9) 0.086(6) 0.023(6) 0.004(5) -0.039(6) C32 0.066(4) 0.043(3) 0.040(3) 0.007(2) 0.003(3) 0.015(3) C33 0.053(4) 0.059(4) 0.074(5) 0.016(3) 0.005(3) 0.005(3) C34 0.067(5) 0.039(3) 0.096(5) 0.013(3) -0.010(4) -0.003(3) C35 0.066(4) 0.038(3) 0.087(5) 0.002(3) 0.003(4) 0.015(3) C36 0.058(4) 0.062(4) 0.076(5) 0.008(3) 0.019(3) 0.015(3) C37 0.064(4) 0.041(3) 0.067(4) 0.011(3) 0.006(3) 0.004(3) C38 0.091(5) 0.045(3) 0.062(4) 0.007(3) 0.017(4) 0.006(3) C39 0.115(7) 0.102(6) 0.069(5) 0.038(5) 0.031(5) 0.030(5) C40 0.155(11) 0.126(9) 0.127(10) 0.067(8) 0.056(9) 0.032(8) C41 0.182(12) 0.060(5) 0.154(11) 0.042(6) 0.103(10) 0.012(6) C42 0.180(11) 0.062(5) 0.168(12) -0.013(6) 0.095(9) -0.018(6) C43 0.118(7) 0.056(4) 0.083(6) 0.009(4) 0.034(5) -0.010(4) C44 0.057(4) 0.054(3) 0.046(3) 0.003(3) 0.008(3) 0.000(3) C45 0.108(6) 0.072(4) 0.048(4) 0.004(3) 0.002(4) 0.024(4) C46 0.131(8) 0.093(6) 0.057(5) 0.005(4) -0.020(5) 0.009(5) C47 0.121(7) 0.107(7) 0.049(5) -0.014(5) -0.003(4) -0.022(6) C48 0.113(7) 0.072(5) 0.074(6) -0.014(4) 0.015(5) 0.001(4) C49 0.086(5) 0.067(4) 0.051(4) -0.005(3) 0.007(3) 0.013(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 Ni1 N1 1.908(4) . ? Ni1 N2 1.970(4) . ? Ni1 P1 2.233(2) . ? N1 C1 1.345(6) . ? N1 C20 1.441(6) . ? N2 C7 1.274(7) . ? N2 C8 1.426(6) . ? P1 C38 1.821(7) . ? P1 C44 1.848(6) . ? P1 C32 1.850(6) . ? C1 C2 1.421(7) . ? C1 C6 1.436(7) . ? C2 C3 1.356(8) . ? C3 C4 1.378(9) . ? C4 C5 1.360(9) . ? C5 C6 1.405(8) . ? C6 C7 1.447(7) . ? C8 C9 1.392(8) . ? C8 C13 1.417(7) . ? C9 C10 1.388(8) . ? C9 C17 1.514(9) . ? C10 C11 1.366(9) . ? C11 C12 1.341(10) . ? C12 C13 1.393(8) . ? C13 C14 1.511(8) . ? C14 C15 1.522(10) . ? C14 C16 1.538(11) . ? C17 C19 1.527(14) . ? C17 C18 1.531(12) . ? C20 C21 1.390(8) . ? C20 C25 1.400(8) . ? C21 C22 1.394(8) . ? C21 C26 1.533(9) . ? C22 C23 1.346(10) . ? C23 C24 1.378(10) . ? C24 C25 1.399(8) . ? C25 C29 1.495(8) . ? C26 C28 1.503(10) . ? C26 C27 1.521(11) . ? C29 C30 1.509(9) . ? C29 C31 1.520(10) . ? C32 C37 1.365(9) . ? C32 C33 1.372(8) . ? C33 C34 1.343(9) . ? C34 C35 1.350(10) . ? C35 C36 1.369(9) . ? C36 C37 1.385(8) . ? C38 C43 1.350(10) . ? C38 C39 1.380(10) . ? C39 C40 1.355(14) . ? C40 C41 1.362(16) . ? C41 C42 1.420(16) . ? C42 C43 1.402(12) . ? C44 C45 1.373(8) . ? C44 C49 1.379(8) . ? C45 C46 1.374(10) . ? C46 C47 1.351(12) . ? C47 C48 1.368(11) . ? C48 C49 1.378(10) . ? 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 Ni1 N2 94.56(17) . . ? N1 Ni1 P1 147.08(13) . . ? N2 Ni1 P1 118.08(13) . . ? C1 N1 C20 117.7(4) . . ? C1 N1 Ni1 128.0(3) . . ? C20 N1 Ni1 114.3(3) . . ? C7 N2 C8 115.2(5) . . ? C7 N2 Ni1 122.5(3) . . ? C8 N2 Ni1 122.2(4) . . ? C38 P1 C44 101.1(3) . . ? C38 P1 C32 100.8(3) . . ? C44 P1 C32 103.2(3) . . ? C38 P1 Ni1 118.3(2) . . ? C44 P1 Ni1 124.9(2) . . ? C32 P1 Ni1 105.1(2) . . ? N1 C1 C2 123.2(5) . . ? N1 C1 C6 121.5(4) . . ? C2 C1 C6 115.3(5) . . ? C3 C2 C1 122.3(5) . . ? C2 C3 C4 121.5(6) . . ? C5 C4 C3 119.3(6) . . ? C4 C5 C6 121.3(6) . . ? C5 C6 C1 120.2(5) . . ? C5 C6 C7 116.6(5) . . ? C1 C6 C7 123.2(5) . . ? N2 C7 C6 128.9(5) . . ? C9 C8 C13 121.3(5) . . ? C9 C8 N2 119.4(5) . . ? C13 C8 N2 119.4(5) . . ? C10 C9 C8 117.9(6) . . ? C10 C9 C17 121.3(6) . . ? C8 C9 C17 120.8(5) . . ? C11 C10 C9 121.3(6) . . ? C12 C11 C10 120.6(6) . . ? C11 C12 C13 122.1(6) . . ? C12 C13 C8 116.8(6) . . ? C12 C13 C14 121.4(5) . . ? C8 C13 C14 121.8(5) . . ? C13 C14 C15 113.2(6) . . ? C13 C14 C16 112.1(6) . . ? C15 C14 C16 109.2(6) . . ? C9 C17 C19 110.1(7) . . ? C9 C17 C18 112.9(7) . . ? C19 C17 C18 109.4(7) . . ? C21 C20 C25 121.6(5) . . ? C21 C20 N1 118.7(5) . . ? C25 C20 N1 119.7(5) . . ? C20 C21 C22 118.2(6) . . ? C20 C21 C26 121.6(5) . . ? C22 C21 C26 120.2(6) . . ? C23 C22 C21 121.6(7) . . ? C22 C23 C24 120.0(6) . . ? C23 C24 C25 121.5(7) . . ? C24 C25 C20 117.0(6) . . ? C24 C25 C29 121.0(6) . . ? C20 C25 C29 121.9(5) . . ? C28 C26 C27 109.7(8) . . ? C28 C26 C21 112.8(7) . . ? C27 C26 C21 110.2(6) . . ? C25 C29 C30 111.8(5) . . ? C25 C29 C31 111.8(6) . . ? C30 C29 C31 110.8(7) . . ? C37 C32 C33 118.5(5) . . ? C37 C32 P1 125.1(4) . . ? C33 C32 P1 116.0(5) . . ? C34 C33 C32 121.0(7) . . ? C33 C34 C35 120.9(6) . . ? C34 C35 C36 120.0(6) . . ? C35 C36 C37 119.0(6) . . ? C32 C37 C36 120.6(6) . . ? C43 C38 C39 117.9(7) . . ? C43 C38 P1 123.3(6) . . ? C39 C38 P1 118.7(6) . . ? C40 C39 C38 121.9(11) . . ? C39 C40 C41 119.6(11) . . ? C40 C41 C42 121.8(9) . . ? C43 C42 C41 114.8(11) . . ? C38 C43 C42 123.9(10) . . ? C45 C44 C49 118.6(6) . . ? C45 C44 P1 123.5(5) . . ? C49 C44 P1 117.8(5) . . ? C44 C45 C46 120.9(7) . . ? C47 C46 C45 119.8(7) . . ? C46 C47 C48 120.5(7) . . ? C47 C48 C49 119.9(7) . . ? C48 C49 C44 120.1(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.789 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.100 # Attachment 'Complex-2.cif' data_f50319a _database_code_depnum_ccdc_archive 'CCDC 289504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H46 N2 Ni P' _chemical_formula_weight 704.52 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' P P 0.1023 0.0942 '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 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 12.006(5) _cell_length_b 17.966(7) _cell_length_c 18.475(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.793(5) _cell_angle_gamma 90.00 _cell_volume 3886(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16015 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8940 _exptl_absorpt_correction_T_max 0.9449 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16015 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6851 _reflns_number_gt 5354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+1.3684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6851 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.09987(2) 0.672055(18) 0.231109(17) 0.04060(12) Uani 1 1 d . . . P1 P 0.24611(6) 0.73969(4) 0.28942(4) 0.04822(19) Uani 1 1 d . . . N2 N 0.13862(16) 0.60612(11) 0.15773(11) 0.0410(5) Uani 1 1 d . . . N1 N -0.05257(15) 0.63737(11) 0.21904(10) 0.0360(4) Uani 1 1 d . . . C7 C 0.0716(2) 0.55335(14) 0.12575(12) 0.0407(6) Uani 1 1 d . . . H1 H 0.1003 0.5231 0.0933 0.049 Uiso 1 1 calc R . . C6 C -0.04067(19) 0.53623(13) 0.13443(12) 0.0368(5) Uani 1 1 d . . . C1 C -0.10118(18) 0.57883(13) 0.17889(12) 0.0356(5) Uani 1 1 d . . . C2 C -0.2151(2) 0.55518(15) 0.17762(14) 0.0481(6) Uani 1 1 d . . . H4 H -0.2583 0.5816 0.2050 0.058 Uiso 1 1 calc R . . C3 C -0.2627(2) 0.49477(16) 0.13724(16) 0.0567(7) Uani 1 1 d . . . H5 H -0.3367 0.4807 0.1387 0.068 Uiso 1 1 calc R . . C4 C -0.2036(2) 0.45407(15) 0.09433(15) 0.0547(7) Uani 1 1 d . . . H6 H -0.2375 0.4135 0.0668 0.066 Uiso 1 1 calc R . . C5 C -0.0949(2) 0.47475(14) 0.09336(14) 0.0463(6) Uani 1 1 d . . . H7 H -0.0549 0.4475 0.0647 0.056 Uiso 1 1 calc R . . C8 C 0.2466(2) 0.61106(15) 0.13662(14) 0.0484(6) Uani 1 1 d . . . C9 C 0.3364(2) 0.56551(18) 0.17175(17) 0.0611(8) Uani 1 1 d . . . C10 C 0.4407(3) 0.5740(2) 0.1521(2) 0.0859(11) Uani 1 1 d . . . H10 H 0.5019 0.5441 0.1747 0.103 Uiso 1 1 calc R . . C11 C 0.4556(3) 0.6249(3) 0.1007(3) 0.0975(14) Uani 1 1 d . . . H11 H 0.5269 0.6302 0.0894 0.117 Uiso 1 1 calc R . . C12 C 0.3670(4) 0.6681(2) 0.0654(2) 0.0837(12) Uani 1 1 d . . . H12 H 0.3787 0.7024 0.0301 0.100 Uiso 1 1 calc R . . C13 C 0.2579(3) 0.66201(18) 0.08140(16) 0.0616(8) Uani 1 1 d . . . C14 C 0.1579(3) 0.7042(2) 0.03862(18) 0.0787(10) Uani 1 1 d . . . H14A H 0.1168 0.6738 -0.0012 0.118 Uiso 1 1 calc R . . H14B H 0.1840 0.7486 0.0186 0.118 Uiso 1 1 calc R . . H14C H 0.1084 0.7174 0.0709 0.118 Uiso 1 1 calc R . . C15 C 0.3223(3) 0.5096(2) 0.2293(2) 0.0788(10) Uani 1 1 d . . . H15A H 0.2843 0.5324 0.2642 0.118 Uiso 1 1 calc R . . H15B H 0.3961 0.4920 0.2550 0.118 Uiso 1 1 calc R . . H15C H 0.2776 0.4684 0.2057 0.118 Uiso 1 1 calc R . . C16 C -0.11953(18) 0.67971(13) 0.25952(13) 0.0381(5) Uani 1 1 d . . . C17 C -0.1214(2) 0.65940(14) 0.33265(14) 0.0449(6) Uani 1 1 d . . . C18 C -0.1830(3) 0.70339(18) 0.37161(17) 0.0625(8) Uani 1 1 d . . . H18 H -0.1849 0.6906 0.4201 0.075 Uiso 1 1 calc R . . C19 C -0.2408(3) 0.76503(19) 0.3403(2) 0.0729(9) Uani 1 1 d . . . H19 H -0.2824 0.7933 0.3672 0.087 Uiso 1 1 calc R . . C20 C -0.2376(3) 0.78507(18) 0.2696(2) 0.0697(9) Uani 1 1 d . . . H20 H -0.2761 0.8277 0.2492 0.084 Uiso 1 1 calc R . . C21 C -0.1781(2) 0.74334(16) 0.22754(16) 0.0535(7) Uani 1 1 d . . . C22 C -0.0575(2) 0.59141(17) 0.36924(15) 0.0569(7) Uani 1 1 d . . . H22 H -0.0194 0.5683 0.3332 0.068 Uiso 1 1 calc R . . C23 C -0.1363(4) 0.5340(2) 0.3910(3) 0.1010(13) Uani 1 1 d . . . H23A H -0.1745 0.5552 0.4266 0.151 Uiso 1 1 calc R . . H23B H -0.0924 0.4916 0.4125 0.151 Uiso 1 1 calc R . . H23C H -0.1917 0.5187 0.3478 0.151 Uiso 1 1 calc R . . C24 C 0.0345(4) 0.6143(3) 0.4364(2) 0.1094(15) Uani 1 1 d . . . H24A H 0.0860 0.6488 0.4212 0.164 Uiso 1 1 calc R . . H24B H 0.0761 0.5710 0.4578 0.164 Uiso 1 1 calc R . . H24C H -0.0005 0.6375 0.4726 0.164 Uiso 1 1 calc R . . C25 C -0.1758(4) 0.7677(2) 0.1490(2) 0.0887(12) Uani 1 1 d . . . H25 H -0.1341 0.7296 0.1278 0.106 Uiso 1 1 calc R . . C26 C -0.2928(4) 0.7743(3) 0.0992(3) 0.1331(19) Uani 1 1 d . . . H26A H -0.3325 0.7278 0.0985 0.200 Uiso 1 1 calc R . . H26B H -0.2857 0.7864 0.0498 0.200 Uiso 1 1 calc R . . H26C H -0.3347 0.8128 0.1174 0.200 Uiso 1 1 calc R . . C27 C -0.1121(5) 0.8401(4) 0.1493(3) 0.180(3) Uani 1 1 d . . . H27A H -0.1530 0.8792 0.1676 0.271 Uiso 1 1 calc R . . H27B H -0.1056 0.8518 0.0997 0.271 Uiso 1 1 calc R . . H27C H -0.0372 0.8355 0.1808 0.271 Uiso 1 1 calc R . . C28 C 0.3076(2) 0.80935(16) 0.23686(15) 0.0529(7) Uani 1 1 d . . . C29 C 0.2373(3) 0.8348(2) 0.17222(18) 0.0783(10) Uani 1 1 d . . . H29 H 0.1647 0.8145 0.1563 0.094 Uiso 1 1 calc R . . C30 C 0.2734(4) 0.8900(3) 0.1308(2) 0.1080(15) Uani 1 1 d . . . H30 H 0.2252 0.9067 0.0873 0.130 Uiso 1 1 calc R . . C31 C 0.3796(4) 0.9202(3) 0.1535(2) 0.1054(15) Uani 1 1 d . . . H31 H 0.4040 0.9567 0.1249 0.126 Uiso 1 1 calc R . . C32 C 0.4502(3) 0.8971(2) 0.2180(2) 0.0872(11) Uani 1 1 d . . . H32 H 0.5220 0.9185 0.2339 0.105 Uiso 1 1 calc R . . C33 C 0.4142(3) 0.84157(19) 0.25965(19) 0.0697(9) Uani 1 1 d . . . H33 H 0.4624 0.8258 0.3035 0.084 Uiso 1 1 calc R . . C34 C 0.3674(2) 0.68545(17) 0.34046(17) 0.0584(7) Uani 1 1 d . . . C35 C 0.4620(3) 0.66999(19) 0.3112(2) 0.0706(9) Uani 1 1 d . . . H35 H 0.4690 0.6920 0.2669 0.085 Uiso 1 1 calc R . . C36 C 0.5458(3) 0.6220(3) 0.3478(3) 0.0956(13) Uani 1 1 d . . . H36 H 0.6084 0.6115 0.3275 0.115 Uiso 1 1 calc R . . C37 C 0.5378(4) 0.5903(3) 0.4123(3) 0.1129(16) Uani 1 1 d . . . H37 H 0.5952 0.5585 0.4366 0.135 Uiso 1 1 calc R . . C38 C 0.4463(4) 0.6044(3) 0.4425(3) 0.1177(16) Uani 1 1 d . . . H38 H 0.4412 0.5821 0.4871 0.141 Uiso 1 1 calc R . . C39 C 0.3604(4) 0.6523(2) 0.4066(2) 0.0930(12) Uani 1 1 d . . . H39 H 0.2980 0.6619 0.4274 0.112 Uiso 1 1 calc R . . C40 C 0.2089(2) 0.79919(16) 0.36109(14) 0.0495(6) Uani 1 1 d . . . C41 C 0.2902(3) 0.8345(2) 0.41513(18) 0.0737(9) Uani 1 1 d . . . H41 H 0.3673 0.8245 0.4189 0.088 Uiso 1 1 calc R . . C42 C 0.2576(4) 0.8844(2) 0.46347(18) 0.0859(11) Uani 1 1 d . . . H42 H 0.3128 0.9084 0.4990 0.103 Uiso 1 1 calc R . . C43 C 0.1439(4) 0.8988(2) 0.45932(19) 0.0805(10) Uani 1 1 d . . . H43 H 0.1223 0.9328 0.4916 0.097 Uiso 1 1 calc R . . C44 C 0.0634(3) 0.8633(2) 0.40806(19) 0.0744(9) Uani 1 1 d . . . H44 H -0.0137 0.8721 0.4057 0.089 Uiso 1 1 calc R . . C45 C 0.0957(3) 0.81369(17) 0.35904(16) 0.0584(7) Uani 1 1 d . . . H45 H 0.0397 0.7897 0.3240 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03715(18) 0.0436(2) 0.04355(19) -0.01129(14) 0.01423(13) -0.00601(14) P1 0.0422(4) 0.0546(4) 0.0502(4) -0.0122(3) 0.0152(3) -0.0092(3) N2 0.0398(10) 0.0446(12) 0.0433(11) -0.0059(9) 0.0191(9) -0.0035(9) N1 0.0331(9) 0.0399(11) 0.0368(10) -0.0053(9) 0.0117(8) -0.0009(9) C7 0.0471(13) 0.0409(14) 0.0376(12) -0.0037(10) 0.0169(10) 0.0052(11) C6 0.0424(12) 0.0328(13) 0.0349(11) -0.0008(10) 0.0078(10) 0.0012(10) C1 0.0349(11) 0.0368(13) 0.0343(11) 0.0030(10) 0.0061(9) 0.0011(10) C2 0.0392(13) 0.0497(16) 0.0561(15) -0.0101(12) 0.0124(11) -0.0012(12) C3 0.0413(14) 0.0565(18) 0.0720(19) -0.0067(15) 0.0118(13) -0.0100(13) C4 0.0604(17) 0.0404(15) 0.0599(16) -0.0107(13) 0.0061(13) -0.0107(13) C5 0.0552(15) 0.0392(14) 0.0443(13) -0.0043(11) 0.0106(12) 0.0005(12) C8 0.0476(14) 0.0528(16) 0.0522(15) -0.0189(13) 0.0266(12) -0.0114(13) C9 0.0499(16) 0.066(2) 0.0738(19) -0.0208(16) 0.0269(14) -0.0014(15) C10 0.0519(18) 0.110(3) 0.104(3) -0.033(2) 0.0356(19) -0.0018(19) C11 0.067(2) 0.137(4) 0.105(3) -0.045(3) 0.054(2) -0.034(3) C12 0.098(3) 0.098(3) 0.073(2) -0.025(2) 0.057(2) -0.043(2) C13 0.077(2) 0.066(2) 0.0511(16) -0.0173(14) 0.0340(15) -0.0206(16) C14 0.114(3) 0.072(2) 0.0579(19) -0.0016(17) 0.0367(19) -0.011(2) C15 0.0626(19) 0.073(2) 0.101(3) 0.002(2) 0.0177(18) 0.0118(17) C16 0.0297(11) 0.0402(14) 0.0456(13) -0.0087(11) 0.0107(10) -0.0011(10) C17 0.0437(13) 0.0482(15) 0.0463(14) -0.0079(11) 0.0173(11) -0.0027(11) C18 0.0707(19) 0.067(2) 0.0583(17) -0.0135(15) 0.0332(15) 0.0004(17) C19 0.076(2) 0.065(2) 0.089(2) -0.0237(19) 0.0430(18) 0.0079(17) C20 0.0672(19) 0.0527(19) 0.094(2) -0.0025(17) 0.0288(18) 0.0218(15) C21 0.0500(15) 0.0509(17) 0.0610(17) 0.0012(13) 0.0156(13) 0.0106(13) C22 0.0615(17) 0.0668(19) 0.0458(15) 0.0071(13) 0.0189(13) 0.0096(15) C23 0.097(3) 0.078(3) 0.133(3) 0.040(3) 0.035(3) 0.006(2) C24 0.103(3) 0.111(3) 0.094(3) 0.020(3) -0.021(2) -0.002(3) C25 0.106(3) 0.088(3) 0.076(2) 0.030(2) 0.029(2) 0.053(2) C26 0.139(4) 0.152(5) 0.088(3) 0.020(3) -0.019(3) -0.021(4) C27 0.149(5) 0.242(8) 0.138(5) 0.102(5) 0.007(4) -0.074(5) C28 0.0515(15) 0.0576(18) 0.0542(16) -0.0171(13) 0.0217(13) -0.0131(13) C29 0.087(2) 0.085(3) 0.062(2) -0.0043(18) 0.0140(17) -0.031(2) C30 0.134(4) 0.116(4) 0.070(2) 0.015(2) 0.012(2) -0.047(3) C31 0.136(4) 0.098(3) 0.093(3) 0.000(2) 0.046(3) -0.054(3) C32 0.086(2) 0.084(3) 0.100(3) -0.019(2) 0.039(2) -0.039(2) C33 0.065(2) 0.071(2) 0.076(2) -0.0132(17) 0.0211(16) -0.0191(16) C34 0.0475(15) 0.0623(19) 0.0638(18) -0.0130(15) 0.0090(13) -0.0067(14) C35 0.0539(17) 0.070(2) 0.090(2) -0.0110(18) 0.0199(16) -0.0022(16) C36 0.056(2) 0.101(3) 0.128(4) -0.016(3) 0.017(2) 0.006(2) C37 0.086(3) 0.122(4) 0.119(4) -0.004(3) -0.003(3) 0.030(3) C38 0.124(4) 0.138(4) 0.088(3) 0.022(3) 0.015(3) 0.039(3) C39 0.088(3) 0.114(3) 0.082(3) 0.012(2) 0.029(2) 0.024(2) C40 0.0549(16) 0.0517(16) 0.0443(14) -0.0098(12) 0.0159(12) -0.0100(13) C41 0.069(2) 0.088(3) 0.0646(19) -0.0270(18) 0.0163(16) -0.0210(18) C42 0.109(3) 0.091(3) 0.0575(19) -0.0305(18) 0.0171(19) -0.033(2) C43 0.118(3) 0.068(2) 0.065(2) -0.0200(17) 0.041(2) -0.010(2) C44 0.084(2) 0.070(2) 0.077(2) -0.0143(18) 0.0334(19) 0.0073(19) C45 0.0617(17) 0.0575(18) 0.0579(17) -0.0138(14) 0.0176(14) -0.0071(14) _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 N1 1.899(2) . ? Ni1 N2 1.933(2) . ? Ni1 P1 2.2096(9) . ? P1 C34 1.831(3) . ? P1 C40 1.832(3) . ? P1 C28 1.836(3) . ? N2 C7 1.298(3) . ? N2 C8 1.437(3) . ? N1 C1 1.344(3) . ? N1 C16 1.432(3) . ? C7 C6 1.426(3) . ? C7 H1 0.9300 . ? C6 C5 1.414(3) . ? C6 C1 1.433(3) . ? C1 C2 1.428(3) . ? C2 C3 1.368(4) . ? C2 H4 0.9300 . ? C3 C4 1.384(4) . ? C3 H5 0.9300 . ? C4 C5 1.361(4) . ? C4 H6 0.9300 . ? C5 H7 0.9300 . ? C8 C9 1.394(4) . ? C8 C13 1.399(4) . ? C9 C10 1.387(4) . ? C9 C15 1.500(5) . ? C10 C11 1.359(6) . ? C10 H10 0.9300 . ? C11 C12 1.361(6) . ? C11 H11 0.9300 . ? C12 C13 1.409(5) . ? C12 H12 0.9300 . ? C13 C14 1.490(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C21 1.402(4) . ? C16 C17 1.405(3) . ? C17 C18 1.387(4) . ? C17 C22 1.519(4) . ? C18 C19 1.366(5) . ? C18 H18 0.9300 . ? C19 C20 1.363(5) . ? C19 H19 0.9300 . ? C20 C21 1.386(4) . ? C20 H20 0.9300 . ? C21 C25 1.521(4) . ? C22 C23 1.513(5) . ? C22 C24 1.524(5) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.504(6) . ? C25 C27 1.509(7) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.378(4) . ? C28 C33 1.383(4) . ? C29 C30 1.380(5) . ? C29 H29 0.9300 . ? C30 C31 1.363(6) . ? C30 H30 0.9300 . ? C31 C32 1.366(6) . ? C31 H31 0.9300 . ? C32 C33 1.385(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.379(5) . ? C34 C35 1.389(4) . ? C35 C36 1.382(5) . ? C35 H35 0.9300 . ? C36 C37 1.344(6) . ? C36 H36 0.9300 . ? C37 C38 1.362(6) . ? C37 H37 0.9300 . ? C38 C39 1.394(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.376(4) . ? C40 C41 1.386(4) . ? C41 C42 1.383(5) . ? C41 H41 0.9300 . ? C42 C43 1.375(5) . ? C42 H42 0.9300 . ? C43 C44 1.354(5) . ? C43 H43 0.9300 . ? C44 C45 1.386(4) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 95.27(8) . . ? N1 Ni1 P1 151.49(6) . . ? N2 Ni1 P1 112.97(6) . . ? C34 P1 C40 103.41(13) . . ? C34 P1 C28 105.55(14) . . ? C40 P1 C28 100.10(13) . . ? C34 P1 Ni1 114.46(10) . . ? C40 P1 Ni1 112.25(9) . . ? C28 P1 Ni1 119.07(9) . . ? C7 N2 C8 115.3(2) . . ? C7 N2 Ni1 123.07(16) . . ? C8 N2 Ni1 121.61(16) . . ? C1 N1 C16 118.60(19) . . ? C1 N1 Ni1 127.67(15) . . ? C16 N1 Ni1 113.72(14) . . ? N2 C7 C6 127.8(2) . . ? N2 C7 H1 116.1 . . ? C6 C7 H1 116.1 . . ? C5 C6 C7 116.3(2) . . ? C5 C6 C1 119.5(2) . . ? C7 C6 C1 124.1(2) . . ? N1 C1 C2 122.6(2) . . ? N1 C1 C6 121.4(2) . . ? C2 C1 C6 115.9(2) . . ? C3 C2 C1 121.8(2) . . ? C3 C2 H4 119.1 . . ? C1 C2 H4 119.1 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H5 119.1 . . ? C4 C3 H5 119.1 . . ? C5 C4 C3 118.5(2) . . ? C5 C4 H6 120.7 . . ? C3 C4 H6 120.7 . . ? C4 C5 C6 122.3(2) . . ? C4 C5 H7 118.8 . . ? C6 C5 H7 118.8 . . ? C9 C8 C13 122.3(3) . . ? C9 C8 N2 119.2(2) . . ? C13 C8 N2 118.5(3) . . ? C10 C9 C8 117.6(3) . . ? C10 C9 C15 120.6(3) . . ? C8 C9 C15 121.8(3) . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 121.3(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C8 C13 C12 116.6(3) . . ? C8 C13 C14 121.5(3) . . ? C12 C13 C14 121.8(3) . . ? 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 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 120.2(2) . . ? C21 C16 N1 120.0(2) . . ? C17 C16 N1 119.7(2) . . ? C18 C17 C16 118.4(3) . . ? C18 C17 C22 120.1(3) . . ? C16 C17 C22 121.5(2) . . ? C19 C18 C17 121.4(3) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 118.5(3) . . ? C20 C21 C25 120.0(3) . . ? C16 C21 C25 121.5(2) . . ? C23 C22 C17 112.5(3) . . ? C23 C22 C24 110.5(3) . . ? C17 C22 C24 110.4(3) . . ? C23 C22 H22 107.7 . . ? C17 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 109.7(4) . . ? C26 C25 C21 113.3(4) . . ? C27 C25 C21 111.1(4) . . ? C26 C25 H25 107.5 . . ? C27 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 118.2(3) . . ? C29 C28 P1 116.3(2) . . ? C33 C28 P1 125.3(2) . . ? C28 C29 C30 120.7(3) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.6(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C28 C33 C32 120.9(3) . . ? C28 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C39 C34 C35 118.3(3) . . ? C39 C34 P1 119.2(3) . . ? C35 C34 P1 122.1(3) . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.7(4) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 120.5(4) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 119.9(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 120.3(4) . . ? C34 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C45 C40 C41 117.9(3) . . ? C45 C40 P1 119.2(2) . . ? C41 C40 P1 122.8(2) . . ? C42 C41 C40 120.4(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 119.8(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C40 C45 C44 121.5(3) . . ? C40 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.498 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.051 # Attachment 'Complex-3.cif' data_f50914a _database_code_depnum_ccdc_archive 'CCDC 289505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 N4 Ni' _chemical_formula_weight 601.37 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 '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 11.050(3) _cell_length_b 19.819(5) _cell_length_c 13.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.116(4) _cell_angle_gamma 90.00 _cell_volume 3024.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 858 _cell_measurement_theta_min 20.361 _cell_measurement_theta_max 2.338 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15070 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.12 _reflns_number_total 6629 _reflns_number_gt 3404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6629 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.96299(3) 0.231780(16) 0.47663(2) 0.04728(11) Uani 1 1 d . . . N1 N 1.13136(17) 0.25320(9) 0.49447(13) 0.0453(5) Uani 1 1 d . . . N2 N 0.97138(18) 0.14772(10) 0.55192(14) 0.0472(5) Uani 1 1 d . . . N3 N 0.84817(18) 0.29909(10) 0.51280(15) 0.0508(5) Uani 1 1 d . . . N4 N 0.87098(17) 0.20674(9) 0.35932(14) 0.0456(5) Uani 1 1 d . . . C1 C 1.1643(2) 0.31628(13) 0.4531(2) 0.0488(7) Uani 1 1 d . . . C2 C 1.1515(2) 0.32624(14) 0.3546(2) 0.0622(8) Uani 1 1 d . . . H2 H 1.1250 0.2910 0.3152 0.075 Uiso 1 1 calc R . . C3 C 1.1778(2) 0.38836(17) 0.3139(2) 0.0767(9) Uani 1 1 d . . . H3 H 1.1703 0.3943 0.2472 0.092 Uiso 1 1 calc R . . C4 C 1.2146(3) 0.44072(16) 0.3712(3) 0.0786(10) Uani 1 1 d . . . H4 H 1.2317 0.4825 0.3439 0.094 Uiso 1 1 calc R . . C5 C 1.2263(3) 0.43163(15) 0.4682(3) 0.0796(10) Uani 1 1 d . . . H5 H 1.2515 0.4674 0.5071 0.096 Uiso 1 1 calc R . . C6 C 1.2015(2) 0.37042(14) 0.5098(2) 0.0663(8) Uani 1 1 d . . . H6 H 1.2098 0.3652 0.5766 0.080 Uiso 1 1 calc R . . C7 C 1.2152(2) 0.21965(13) 0.54857(17) 0.0477(7) Uani 1 1 d . . . C8 C 1.3386(2) 0.23967(14) 0.55605(18) 0.0593(7) Uani 1 1 d . . . H8 H 1.3640 0.2767 0.5204 0.071 Uiso 1 1 calc R . . C9 C 1.4207(3) 0.20684(16) 0.6132(2) 0.0741(9) Uani 1 1 d . . . H9 H 1.4998 0.2228 0.6172 0.089 Uiso 1 1 calc R . . C10 C 1.3894(3) 0.15026(16) 0.6657(2) 0.0768(9) Uani 1 1 d . . . H10 H 1.4463 0.1282 0.7048 0.092 Uiso 1 1 calc R . . C11 C 1.2740(3) 0.12783(14) 0.6587(2) 0.0689(8) Uani 1 1 d . . . H11 H 1.2525 0.0896 0.6933 0.083 Uiso 1 1 calc R . . C12 C 1.1845(2) 0.16030(13) 0.60067(18) 0.0513(7) Uani 1 1 d . . . C13 C 1.0685(2) 0.12935(13) 0.59985(18) 0.0548(7) Uani 1 1 d . . . H13 H 1.0610 0.0912 0.6384 0.066 Uiso 1 1 calc R . . C14 C 0.8682(2) 0.10424(13) 0.55332(17) 0.0479(6) Uani 1 1 d . . . C15 C 0.8775(3) 0.03461(14) 0.5644(2) 0.0662(8) Uani 1 1 d . . . H15 H 0.9532 0.0153 0.5756 0.079 Uiso 1 1 calc R . . C16 C 0.7768(3) -0.00605(15) 0.5591(2) 0.0804(10) Uani 1 1 d . . . H16 H 0.7845 -0.0524 0.5673 0.096 Uiso 1 1 calc R . . C17 C 0.6653(3) 0.02170(17) 0.5417(2) 0.0792(9) Uani 1 1 d . . . H17 H 0.5972 -0.0058 0.5373 0.095 Uiso 1 1 calc R . . C18 C 0.6541(3) 0.08981(16) 0.53080(19) 0.0661(8) Uani 1 1 d . . . H18 H 0.5781 0.1086 0.5190 0.079 Uiso 1 1 calc R . . C19 C 0.7539(2) 0.13098(13) 0.53713(17) 0.0553(7) Uani 1 1 d . . . H19 H 0.7446 0.1774 0.5304 0.066 Uiso 1 1 calc R . . C20 C 0.8770(3) 0.32882(16) 0.6040(2) 0.0642(8) Uani 1 1 d . . . C21 C 0.8531(3) 0.29532(18) 0.6886(3) 0.0966(12) Uani 1 1 d . . . H21 H 0.8142 0.2537 0.6864 0.116 Uiso 1 1 calc R . . C22 C 0.8868(5) 0.3233(3) 0.7779(3) 0.142(2) Uani 1 1 d . . . H22 H 0.8698 0.3007 0.8350 0.170 Uiso 1 1 calc R . . C23 C 0.9454(5) 0.3848(3) 0.7810(4) 0.161(3) Uani 1 1 d . . . H23 H 0.9690 0.4036 0.8401 0.194 Uiso 1 1 calc R . . C24 C 0.9680(4) 0.4173(3) 0.6980(4) 0.140(2) Uani 1 1 d . . . H24 H 1.0074 0.4587 0.7003 0.167 Uiso 1 1 calc R . . C25 C 0.9337(3) 0.39015(18) 0.6086(3) 0.0914(11) Uani 1 1 d . . . H25 H 0.9494 0.4137 0.5520 0.110 Uiso 1 1 calc R . . C26 C 0.7430(2) 0.31694(12) 0.46783(19) 0.0493(7) Uani 1 1 d . . . C27 C 0.6631(2) 0.36560(13) 0.5067(2) 0.0633(8) Uani 1 1 d . . . H27 H 0.6842 0.3869 0.5646 0.076 Uiso 1 1 calc R . . C28 C 0.5567(3) 0.38187(14) 0.4616(2) 0.0711(9) Uani 1 1 d . . . H28 H 0.5070 0.4141 0.4894 0.085 Uiso 1 1 calc R . . C29 C 0.5200(2) 0.35184(14) 0.3752(2) 0.0683(8) Uani 1 1 d . . . H29 H 0.4468 0.3634 0.3453 0.082 Uiso 1 1 calc R . . C30 C 0.5934(2) 0.30543(13) 0.3359(2) 0.0606(8) Uani 1 1 d . . . H30 H 0.5696 0.2852 0.2778 0.073 Uiso 1 1 calc R . . C31 C 0.7050(2) 0.28615(12) 0.37928(19) 0.0482(7) Uani 1 1 d . . . C32 C 0.7696(2) 0.23453(13) 0.33144(18) 0.0517(7) Uani 1 1 d . . . H32 H 0.7356 0.2188 0.2736 0.062 Uiso 1 1 calc R . . C33 C 0.9104(2) 0.14865(13) 0.30664(17) 0.0478(6) Uani 1 1 d . . . C34 C 0.8299(3) 0.10060(14) 0.27217(19) 0.0653(8) Uani 1 1 d . . . H34 H 0.7473 0.1057 0.2818 0.078 Uiso 1 1 calc R . . C35 C 0.8730(3) 0.04464(15) 0.2229(2) 0.0770(9) Uani 1 1 d . . . H35 H 0.8190 0.0124 0.1993 0.092 Uiso 1 1 calc R . . C36 C 0.9944(4) 0.03678(15) 0.2092(2) 0.0796(10) Uani 1 1 d . . . H36 H 1.0225 -0.0003 0.1751 0.096 Uiso 1 1 calc R . . C37 C 1.0742(3) 0.08315(15) 0.2452(2) 0.0730(9) Uani 1 1 d . . . H37 H 1.1568 0.0773 0.2367 0.088 Uiso 1 1 calc R . . C38 C 1.0323(3) 0.13880(13) 0.29441(19) 0.0584(7) Uani 1 1 d . . . H38 H 1.0872 0.1700 0.3196 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0404(2) 0.04819(19) 0.0530(2) 0.00136(18) -0.00458(14) 0.00559(18) N1 0.0400(13) 0.0477(14) 0.0480(13) 0.0039(10) -0.0036(10) 0.0011(10) N2 0.0397(13) 0.0521(13) 0.0498(14) 0.0028(11) 0.0003(10) 0.0026(11) N3 0.0471(14) 0.0532(13) 0.0519(14) -0.0025(11) -0.0051(11) 0.0101(11) N4 0.0428(13) 0.0467(13) 0.0474(13) 0.0031(10) 0.0007(10) 0.0039(11) C1 0.0378(16) 0.0504(17) 0.0581(19) 0.0024(15) -0.0036(13) 0.0017(13) C2 0.0574(19) 0.065(2) 0.064(2) 0.0082(16) -0.0080(15) -0.0086(15) C3 0.058(2) 0.090(2) 0.081(2) 0.031(2) -0.0135(17) -0.0068(19) C4 0.054(2) 0.064(2) 0.117(3) 0.027(2) -0.003(2) -0.0033(17) C5 0.073(2) 0.058(2) 0.107(3) -0.007(2) -0.004(2) -0.0043(17) C6 0.070(2) 0.061(2) 0.068(2) -0.0027(17) 0.0003(16) -0.0028(17) C7 0.0414(16) 0.0562(18) 0.0456(16) -0.0064(13) 0.0011(12) 0.0060(14) C8 0.0443(17) 0.0692(19) 0.0644(19) 0.0006(15) -0.0023(14) 0.0024(16) C9 0.0420(18) 0.089(2) 0.091(2) -0.0054(19) -0.0104(17) 0.0037(17) C10 0.051(2) 0.087(2) 0.092(3) 0.013(2) -0.0187(17) 0.0119(18) C11 0.058(2) 0.074(2) 0.074(2) 0.0123(16) -0.0108(16) 0.0046(17) C12 0.0437(17) 0.0603(18) 0.0496(17) 0.0019(14) -0.0052(13) 0.0041(15) C13 0.0542(19) 0.0551(18) 0.0551(18) 0.0100(14) -0.0020(14) 0.0021(15) C14 0.0429(17) 0.0547(17) 0.0460(16) 0.0057(13) -0.0002(12) 0.0021(15) C15 0.052(2) 0.062(2) 0.084(2) 0.0066(17) -0.0043(16) 0.0026(17) C16 0.078(3) 0.062(2) 0.101(3) 0.0114(18) -0.008(2) -0.012(2) C17 0.061(2) 0.083(3) 0.092(3) 0.014(2) -0.0103(18) -0.022(2) C18 0.0471(19) 0.079(2) 0.072(2) 0.0102(17) -0.0033(15) -0.0011(17) C19 0.0482(18) 0.0600(18) 0.0577(18) 0.0091(14) 0.0040(14) -0.0002(16) C20 0.056(2) 0.068(2) 0.068(2) -0.0149(18) -0.0123(16) 0.0244(17) C21 0.123(3) 0.106(3) 0.060(2) -0.008(2) -0.008(2) 0.046(2) C22 0.177(5) 0.188(5) 0.059(3) -0.025(3) -0.023(3) 0.111(4) C23 0.137(5) 0.195(7) 0.149(5) -0.115(6) -0.080(4) 0.103(5) C24 0.094(3) 0.151(5) 0.172(5) -0.094(5) -0.045(4) 0.046(3) C25 0.075(2) 0.086(3) 0.113(3) -0.037(2) -0.015(2) 0.017(2) C26 0.0433(17) 0.0480(16) 0.0566(18) 0.0095(14) 0.0028(14) 0.0034(14) C27 0.0534(19) 0.0617(19) 0.074(2) -0.0049(16) -0.0044(16) 0.0166(16) C28 0.055(2) 0.064(2) 0.094(3) 0.0042(18) 0.0048(18) 0.0190(17) C29 0.0449(19) 0.075(2) 0.085(2) 0.0168(18) -0.0079(17) 0.0130(17) C30 0.0500(18) 0.0654(19) 0.066(2) 0.0127(15) -0.0055(15) 0.0039(16) C31 0.0396(16) 0.0500(17) 0.0551(18) 0.0082(13) -0.0004(13) 0.0046(13) C32 0.0505(17) 0.0548(16) 0.0495(16) 0.0054(14) -0.0034(13) -0.0026(15) C33 0.0527(18) 0.0467(16) 0.0439(16) 0.0060(13) -0.0021(13) 0.0026(15) C34 0.066(2) 0.0617(19) 0.068(2) 0.0001(16) -0.0077(16) -0.0008(17) C35 0.102(3) 0.055(2) 0.072(2) 0.0004(17) -0.016(2) -0.014(2) C36 0.110(3) 0.058(2) 0.071(2) -0.0075(17) 0.001(2) 0.008(2) C37 0.078(2) 0.065(2) 0.076(2) -0.0034(17) 0.0104(18) 0.0148(19) C38 0.058(2) 0.0512(17) 0.066(2) -0.0051(14) 0.0039(15) 0.0030(15) _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 N3 1.9141(19) . ? Ni1 N1 1.9196(19) . ? Ni1 N4 1.960(2) . ? Ni1 N2 1.965(2) . ? N1 C7 1.353(3) . ? N1 C1 1.425(3) . ? N2 C13 1.302(3) . ? N2 C14 1.430(3) . ? N3 C26 1.354(3) . ? N3 C20 1.421(3) . ? N4 C32 1.300(3) . ? N4 C33 1.434(3) . ? C1 C2 1.379(3) . ? C1 C6 1.387(3) . ? C2 C3 1.387(3) . ? C3 C4 1.363(4) . ? C4 C5 1.356(4) . ? C5 C6 1.373(4) . ? C7 C8 1.422(3) . ? C7 C12 1.423(3) . ? C8 C9 1.358(3) . ? C9 C10 1.382(4) . ? C10 C11 1.353(3) . ? C11 C12 1.415(3) . ? C12 C13 1.421(3) . ? C14 C19 1.383(3) . ? C14 C15 1.392(3) . ? C15 C16 1.375(3) . ? C16 C17 1.366(4) . ? C17 C18 1.364(4) . ? C18 C19 1.374(3) . ? C20 C25 1.368(4) . ? C20 C21 1.375(4) . ? C21 C22 1.396(5) . ? C22 C23 1.380(7) . ? C23 C24 1.343(7) . ? C24 C25 1.392(5) . ? C26 C27 1.420(3) . ? C26 C31 1.423(3) . ? C27 C28 1.359(3) . ? C28 C29 1.386(4) . ? C29 C30 1.347(3) . ? C30 C31 1.414(3) . ? C31 C32 1.418(3) . ? C33 C38 1.375(3) . ? C33 C34 1.381(3) . ? C34 C35 1.390(4) . ? C35 C36 1.368(4) . ? C36 C37 1.361(4) . ? C37 C38 1.380(3) . ? 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 N3 Ni1 N1 117.27(8) . . ? N3 Ni1 N4 93.24(9) . . ? N1 Ni1 N4 130.39(8) . . ? N3 Ni1 N2 118.52(8) . . ? N1 Ni1 N2 94.81(8) . . ? N4 Ni1 N2 103.96(8) . . ? C7 N1 C1 118.4(2) . . ? C7 N1 Ni1 127.84(16) . . ? C1 N1 Ni1 113.39(15) . . ? C13 N2 C14 118.3(2) . . ? C13 N2 Ni1 122.43(18) . . ? C14 N2 Ni1 119.26(16) . . ? C26 N3 C20 118.3(2) . . ? C26 N3 Ni1 129.02(18) . . ? C20 N3 Ni1 112.44(16) . . ? C32 N4 C33 117.3(2) . . ? C32 N4 Ni1 124.60(17) . . ? C33 N4 Ni1 117.72(16) . . ? C2 C1 C6 118.1(3) . . ? C2 C1 N1 120.0(2) . . ? C6 C1 N1 121.8(3) . . ? C1 C2 C3 120.6(3) . . ? C4 C3 C2 120.2(3) . . ? C5 C4 C3 119.7(3) . . ? C4 C5 C6 121.1(3) . . ? C5 C6 C1 120.4(3) . . ? N1 C7 C8 123.2(2) . . ? N1 C7 C12 121.2(2) . . ? C8 C7 C12 115.5(2) . . ? C9 C8 C7 122.5(3) . . ? C8 C9 C10 121.5(3) . . ? C11 C10 C9 118.3(3) . . ? C10 C11 C12 122.6(3) . . ? C11 C12 C13 115.4(2) . . ? C11 C12 C7 119.5(3) . . ? C13 C12 C7 125.2(2) . . ? N2 C13 C12 128.2(2) . . ? C19 C14 C15 117.6(3) . . ? C19 C14 N2 119.5(2) . . ? C15 C14 N2 122.8(2) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 C15 120.0(3) . . ? C18 C17 C16 119.8(3) . . ? C17 C18 C19 120.7(3) . . ? C18 C19 C14 120.8(3) . . ? C25 C20 C21 119.0(3) . . ? C25 C20 N3 120.3(3) . . ? C21 C20 N3 120.7(3) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 119.7(5) . . ? C24 C23 C22 119.5(6) . . ? C23 C24 C25 121.3(6) . . ? C20 C25 C24 120.1(4) . . ? N3 C26 C27 122.6(3) . . ? N3 C26 C31 121.3(2) . . ? C27 C26 C31 116.1(2) . . ? C28 C27 C26 121.8(3) . . ? C27 C28 C29 121.9(3) . . ? C30 C29 C28 118.2(3) . . ? C29 C30 C31 122.7(3) . . ? C30 C31 C32 116.1(3) . . ? C30 C31 C26 119.3(2) . . ? C32 C31 C26 124.5(2) . . ? N4 C32 C31 127.3(2) . . ? C38 C33 C34 119.0(3) . . ? C38 C33 N4 118.9(2) . . ? C34 C33 N4 121.9(2) . . ? C33 C34 C35 119.6(3) . . ? C36 C35 C34 120.4(3) . . ? C37 C36 C35 120.2(3) . . ? C36 C37 C38 119.9(3) . . ? C33 C38 C37 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.414 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.042