# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Qing Wu' _publ_contact_author_email CESWUQ@MAIL.SYSU.EDU.CN _publ_section_title ; Longstanding Living Polymerization of Ethylene: Substituent Effect on Bridging Carbon of 2-Pyridinemethanamine Nickel Catalysts ; loop_ _publ_author_name 'Qing Wu' 'Shan Cheng' 'Haiyang Gao' 'Lihua Guo' 'Cong Li' 'Fengshou Liu' ; Shaobo Zai ; 'Ling Zhang' 'Guiyu Zhou' 'Fangming Zhu' #================================================end data_2 _database_code_depnum_ccdc_archive 'CCDC 754729' #TrackingRef 'combined1 and 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H38 Br2 Cl2 N2 Ni O' _chemical_formula_weight 708.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4346(13) _cell_length_b 13.4926(13) _cell_length_c 17.6159(17) _cell_angle_alpha 90.00 _cell_angle_beta 105.588(2) _cell_angle_gamma 90.00 _cell_volume 3075.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4892 _cell_measurement_theta_min 2.4920 _cell_measurement_theta_max 26.9959 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 3.426 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.3411 _exptl_absorpt_correction_T_max 0.4263 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 15490 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.06 _reflns_number_total 6637 _reflns_number_gt 4674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6637 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 0.02210(4) 0.08033(4) 0.63436(3) 0.01836(14) Uani 1 1 d . . . Br1 Br -0.04199(4) -0.09065(3) 0.63231(2) 0.02930(13) Uani 1 1 d . . . Br2 Br -0.10477(3) 0.16907(3) 0.53049(2) 0.02605(13) Uani 1 1 d . . . N1 N -0.0336(3) 0.1220(2) 0.72573(19) 0.0212(7) Uani 1 1 d . . . N2 N 0.1587(2) 0.0694(2) 0.72720(18) 0.0175(7) Uani 1 1 d . . . H2 H 0.1121 0.0304 0.6970 0.021 Uiso 1 1 calc R . . C1 C -0.1352(3) 0.1318(3) 0.7190(3) 0.0294(10) Uani 1 1 d . . . H1A H -0.1824 0.1280 0.6681 0.035 Uiso 1 1 calc R . . C2 C -0.1732(4) 0.1473(4) 0.7833(3) 0.0350(11) Uani 1 1 d . . . H2A H -0.2455 0.1526 0.7769 0.042 Uiso 1 1 calc R . . C3 C -0.1055(4) 0.1549(3) 0.8567(3) 0.0357(11) Uani 1 1 d . . . H3A H -0.1300 0.1667 0.9017 0.043 Uiso 1 1 calc R . . C4 C -0.0003(3) 0.1450(3) 0.8643(2) 0.0292(10) Uani 1 1 d . . . H4A H 0.0483 0.1510 0.9144 0.035 Uiso 1 1 calc R . . C5 C 0.0326(3) 0.1264(3) 0.7974(2) 0.0200(8) Uani 1 1 d . . . C6 C 0.1467(3) 0.1157(3) 0.8021(2) 0.0173(8) Uani 1 1 d . . . H6A H 0.1751 0.1844 0.8040 0.021 Uiso 1 1 calc R . . C7 C 0.2099(3) 0.0628(3) 0.8756(2) 0.0203(8) Uani 1 1 d . . . C8 C 0.2966(3) 0.1102(3) 0.9255(2) 0.0228(9) Uani 1 1 d . . . C9 C 0.3280(4) 0.2139(3) 0.9103(3) 0.0346(11) Uani 1 1 d . . . H9A H 0.3900 0.2329 0.9514 0.052 Uiso 1 1 calc R . . H9B H 0.2717 0.2599 0.9108 0.052 Uiso 1 1 calc R . . H9C H 0.3427 0.2165 0.8588 0.052 Uiso 1 1 calc R . . C10 C 0.3540(3) 0.0618(3) 0.9928(2) 0.0270(9) Uani 1 1 d . . . H10A H 0.4117 0.0945 1.0266 0.032 Uiso 1 1 calc R . . C11 C 0.3288(3) -0.0341(3) 1.0120(2) 0.0256(9) Uani 1 1 d . . . C12 C 0.3908(4) -0.0852(4) 1.0859(3) 0.0406(12) Uani 1 1 d . . . H12A H 0.3619 -0.1512 1.0894 0.061 Uiso 1 1 calc R . . H12B H 0.3878 -0.0460 1.1321 0.061 Uiso 1 1 calc R . . H12C H 0.4628 -0.0915 1.0843 0.061 Uiso 1 1 calc R . . C13 C 0.2434(3) -0.0786(3) 0.9627(2) 0.0264(9) Uani 1 1 d . . . H13A H 0.2246 -0.1431 0.9754 0.032 Uiso 1 1 calc R . . C14 C 0.1837(3) -0.0329(3) 0.8950(2) 0.0253(9) Uani 1 1 d . . . C15 C 0.0929(4) -0.0908(3) 0.8458(3) 0.0355(11) Uani 1 1 d . . . H15A H 0.0897 -0.1556 0.8701 0.053 Uiso 1 1 calc R . . H15B H 0.1012 -0.1001 0.7927 0.053 Uiso 1 1 calc R . . H15C H 0.0289 -0.0542 0.8426 0.053 Uiso 1 1 calc R . . C16 C 0.2557(3) 0.0960(3) 0.7099(2) 0.0193(8) Uani 1 1 d . . . C17 C 0.2667(3) 0.1925(3) 0.6829(2) 0.0223(8) Uani 1 1 d . . . C18 C 0.1812(3) 0.2692(3) 0.6634(2) 0.0238(9) Uani 1 1 d . . . H18A H 0.1179 0.2381 0.6727 0.029 Uiso 1 1 calc R . . C19 C 0.1552(4) 0.3007(3) 0.5769(3) 0.0333(10) Uani 1 1 d . . . H19A H 0.1385 0.2420 0.5431 0.050 Uiso 1 1 calc R . . H19B H 0.2148 0.3348 0.5667 0.050 Uiso 1 1 calc R . . H19C H 0.0957 0.3456 0.5653 0.050 Uiso 1 1 calc R . . C20 C 0.2070(4) 0.3616(3) 0.7164(3) 0.0335(10) Uani 1 1 d . . . H20A H 0.2227 0.3415 0.7719 0.050 Uiso 1 1 calc R . . H20B H 0.1475 0.4067 0.7043 0.050 Uiso 1 1 calc R . . H20C H 0.2670 0.3954 0.7068 0.050 Uiso 1 1 calc R . . C21 C 0.3608(3) 0.2177(3) 0.6696(3) 0.0294(10) Uani 1 1 d . . . H21A H 0.3700 0.2825 0.6516 0.035 Uiso 1 1 calc R . . C22 C 0.4413(3) 0.1509(3) 0.6820(3) 0.0356(11) Uani 1 1 d . . . H22A H 0.5059 0.1706 0.6745 0.043 Uiso 1 1 calc R . . C23 C 0.4276(3) 0.0560(4) 0.7050(3) 0.0309(10) Uani 1 1 d . . . H23A H 0.4825 0.0096 0.7114 0.037 Uiso 1 1 calc R . . C24 C 0.3340(3) 0.0255(3) 0.7194(2) 0.0235(9) Uani 1 1 d . . . C25 C 0.3253(3) -0.0833(3) 0.7415(3) 0.0284(9) Uani 1 1 d . . . H25A H 0.2535 -0.0947 0.7459 0.034 Uiso 1 1 calc R . . C26 C 0.3998(4) -0.1080(4) 0.8202(3) 0.0401(12) Uani 1 1 d . . . H26A H 0.3875 -0.0636 0.8608 0.060 Uiso 1 1 calc R . . H26B H 0.4709 -0.0997 0.8168 0.060 Uiso 1 1 calc R . . H26C H 0.3892 -0.1768 0.8341 0.060 Uiso 1 1 calc R . . C27 C 0.3423(4) -0.1512(3) 0.6761(3) 0.0409(12) Uani 1 1 d . . . H27A H 0.2933 -0.1336 0.6258 0.061 Uiso 1 1 calc R . . H27B H 0.3314 -0.2203 0.6889 0.061 Uiso 1 1 calc R . . H27C H 0.4131 -0.1430 0.6718 0.061 Uiso 1 1 calc R . . C28 C 0.6465(4) 0.4581(4) 0.0244(3) 0.0446(12) Uani 1 1 d . . . H28A H 0.7201 0.4587 0.0242 0.053 Uiso 1 1 calc R . . H28B H 0.6059 0.4906 -0.0244 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.63173(12) 0.52382(11) 0.10633(10) 0.0590(4) Uani 1 1 d . . . Cl2 Cl 0.60463(13) 0.33452(11) 0.02660(10) 0.0618(4) Uani 1 1 d . . . O1W O 0.1078(2) 0.0464(2) 0.55722(16) 0.0240(6) Uani 1 1 d . . . H1WA H 0.1389 0.0973 0.5485 0.036 Uiso 1 1 calc R . . H2WB H 0.106(4) -0.010(4) 0.543(3) 0.051(18) Uiso 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 Ni1 0.0197(3) 0.0205(3) 0.0152(2) -0.00215(19) 0.0052(2) 0.0003(2) Br1 0.0425(3) 0.0252(2) 0.0221(2) -0.00392(16) 0.01200(19) -0.00958(18) Br2 0.0295(2) 0.0257(2) 0.0212(2) -0.00136(16) 0.00389(17) 0.00689(17) N1 0.0238(18) 0.0198(16) 0.0205(16) -0.0009(13) 0.0071(14) -0.0008(14) N2 0.0137(16) 0.0224(16) 0.0169(15) -0.0046(13) 0.0046(12) -0.0068(13) C1 0.021(2) 0.040(3) 0.027(2) -0.0052(19) 0.0060(18) 0.0035(19) C2 0.025(2) 0.047(3) 0.038(3) -0.011(2) 0.017(2) 0.004(2) C3 0.041(3) 0.042(3) 0.031(2) -0.012(2) 0.022(2) 0.000(2) C4 0.031(2) 0.037(2) 0.021(2) -0.0091(18) 0.0089(18) -0.001(2) C5 0.030(2) 0.0182(18) 0.0141(17) -0.0022(14) 0.0097(16) -0.0037(16) C6 0.021(2) 0.0181(18) 0.0132(17) -0.0022(14) 0.0055(15) -0.0065(15) C7 0.025(2) 0.0211(19) 0.0170(18) 0.0024(15) 0.0085(16) -0.0025(16) C8 0.026(2) 0.024(2) 0.0198(19) -0.0028(16) 0.0096(17) -0.0043(17) C9 0.034(3) 0.028(2) 0.034(2) -0.001(2) -0.003(2) -0.015(2) C10 0.030(2) 0.028(2) 0.022(2) -0.0022(17) 0.0050(18) -0.0020(18) C11 0.030(2) 0.027(2) 0.0169(19) 0.0021(16) 0.0024(17) 0.0033(18) C12 0.042(3) 0.045(3) 0.029(2) 0.012(2) 0.000(2) 0.001(2) C13 0.034(3) 0.023(2) 0.023(2) 0.0053(16) 0.0086(18) -0.0042(18) C14 0.025(2) 0.028(2) 0.0218(19) 0.0022(17) 0.0052(17) -0.0043(18) C15 0.034(3) 0.032(2) 0.034(2) 0.008(2) -0.002(2) -0.016(2) C16 0.017(2) 0.024(2) 0.0183(18) -0.0009(15) 0.0062(15) -0.0052(16) C17 0.023(2) 0.025(2) 0.0198(19) -0.0033(16) 0.0066(16) -0.0028(17) C18 0.025(2) 0.022(2) 0.027(2) 0.0022(17) 0.0107(17) -0.0037(17) C19 0.043(3) 0.029(2) 0.028(2) 0.0087(19) 0.011(2) -0.002(2) C20 0.043(3) 0.030(2) 0.030(2) -0.0004(19) 0.013(2) -0.002(2) C21 0.027(2) 0.026(2) 0.039(2) 0.0026(19) 0.016(2) -0.0084(18) C22 0.021(2) 0.040(3) 0.049(3) 0.002(2) 0.016(2) -0.008(2) C23 0.019(2) 0.038(3) 0.037(2) 0.000(2) 0.0105(19) 0.0000(19) C24 0.021(2) 0.026(2) 0.023(2) -0.0005(17) 0.0054(16) -0.0012(17) C25 0.025(2) 0.027(2) 0.035(2) 0.0008(18) 0.0120(19) 0.0001(18) C26 0.050(3) 0.036(3) 0.036(3) 0.006(2) 0.014(2) 0.013(2) C27 0.053(3) 0.029(2) 0.040(3) -0.007(2) 0.011(2) -0.006(2) C28 0.038(3) 0.050(3) 0.047(3) 0.006(3) 0.015(2) 0.003(2) Cl1 0.0595(10) 0.0498(8) 0.0696(10) -0.0160(7) 0.0208(8) -0.0061(7) Cl2 0.0678(10) 0.0526(9) 0.0732(10) -0.0169(8) 0.0333(9) -0.0157(8) O1W 0.0227(16) 0.0258(16) 0.0248(15) -0.0074(13) 0.0088(12) -0.0052(13) _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 2.028(3) . ? Ni1 O1W 2.055(3) . ? Ni1 N2 2.110(3) . ? Ni1 Br2 2.4516(6) . ? Ni1 Br1 2.4594(7) . ? N1 C5 1.336(5) . ? N1 C1 1.344(5) . ? N2 C16 1.460(5) . ? N2 C6 1.507(4) . ? N2 H2 0.8800 . ? C1 C2 1.378(6) . ? C1 H1A 0.9500 . ? C2 C3 1.370(7) . ? C2 H2A 0.9500 . ? C3 C4 1.390(6) . ? C3 H3A 0.9500 . ? C4 C5 1.388(5) . ? C4 H4A 0.9500 . ? C5 C6 1.520(5) . ? C6 C7 1.522(5) . ? C6 H6A 1.0000 . ? C7 C14 1.404(5) . ? C7 C8 1.411(6) . ? C8 C10 1.391(6) . ? C8 C9 1.506(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.401(6) . ? C10 H10A 0.9500 . ? C11 C13 1.377(6) . ? C11 C12 1.510(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.390(6) . ? C13 H13A 0.9500 . ? C14 C15 1.511(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C24 1.394(6) . ? C16 C17 1.408(5) . ? C17 C21 1.389(6) . ? C17 C18 1.515(6) . ? C18 C19 1.531(6) . ? C18 C20 1.540(6) . ? C18 H18A 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 C22 1.379(6) . ? C21 H21A 0.9500 . ? C22 C23 1.371(6) . ? C22 H22A 0.9500 . ? C23 C24 1.409(6) . ? C23 H23A 0.9500 . ? C24 C25 1.531(6) . ? C25 C26 1.514(6) . ? C25 C27 1.536(6) . ? C25 H25A 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 Cl1 1.750(5) . ? C28 Cl2 1.763(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O1W H1WA 0.8400 . ? O1W H2WB 0.80(5) . ? 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 O1W 168.06(13) . . ? N1 Ni1 N2 80.44(13) . . ? O1W Ni1 N2 88.39(11) . . ? N1 Ni1 Br2 97.25(10) . . ? O1W Ni1 Br2 90.92(9) . . ? N2 Ni1 Br2 153.91(9) . . ? N1 Ni1 Br1 93.95(9) . . ? O1W Ni1 Br1 92.13(9) . . ? N2 Ni1 Br1 100.03(9) . . ? Br2 Ni1 Br1 106.06(2) . . ? C5 N1 C1 118.8(3) . . ? C5 N1 Ni1 117.9(3) . . ? C1 N1 Ni1 122.7(3) . . ? C16 N2 C6 113.1(3) . . ? C16 N2 Ni1 117.4(2) . . ? C6 N2 Ni1 112.0(2) . . ? C16 N2 H2 123.4 . . ? C6 N2 H2 123.4 . . ? Ni1 N2 H2 40.8 . . ? N1 C1 C2 122.3(4) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 118.9(4) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 116.9(3) . . ? C4 C5 C6 121.1(4) . . ? N2 C6 C5 109.6(3) . . ? N2 C6 C7 112.6(3) . . ? C5 C6 C7 114.5(3) . . ? N2 C6 H6A 106.5 . . ? C5 C6 H6A 106.5 . . ? C7 C6 H6A 106.5 . . ? C14 C7 C8 119.0(4) . . ? C14 C7 C6 121.3(4) . . ? C8 C7 C6 119.8(3) . . ? C10 C8 C7 119.6(4) . . ? C10 C8 C9 118.1(4) . . ? C7 C8 C9 122.3(4) . . ? 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 C11 121.7(4) . . ? C8 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C13 C11 C10 117.7(4) . . ? C13 C11 C12 121.1(4) . . ? C10 C11 C12 121.1(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 C14 122.6(4) . . ? C11 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C7 119.5(4) . . ? C13 C14 C15 117.0(4) . . ? C7 C14 C15 123.5(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C24 C16 C17 121.8(4) . . ? C24 C16 N2 119.7(3) . . ? C17 C16 N2 118.5(3) . . ? C21 C17 C16 117.8(4) . . ? C21 C17 C18 117.6(4) . . ? C16 C17 C18 124.5(4) . . ? C17 C18 C19 111.8(3) . . ? C17 C18 C20 112.5(4) . . ? C19 C18 C20 109.4(3) . . ? C17 C18 H18A 107.6 . . ? C19 C18 H18A 107.6 . . ? C20 C18 H18A 107.6 . . ? 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 . . ? C22 C21 C17 121.6(4) . . ? C22 C21 H21A 119.2 . . ? C17 C21 H21A 119.2 . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 121.5(4) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C16 C24 C23 117.4(4) . . ? C16 C24 C25 125.2(4) . . ? C23 C24 C25 117.3(4) . . ? C26 C25 C24 111.5(4) . . ? C26 C25 C27 111.1(4) . . ? C24 C25 C27 110.1(4) . . ? C26 C25 H25A 108.0 . . ? C24 C25 H25A 108.0 . . ? C27 C25 H25A 108.0 . . ? 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 . . ? Cl1 C28 Cl2 110.7(3) . . ? Cl1 C28 H28A 109.5 . . ? Cl2 C28 H28A 109.5 . . ? Cl1 C28 H28B 109.5 . . ? Cl2 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? Ni1 O1W H1WA 109.5 . . ? Ni1 O1W H2WB 116(4) . . ? H1WA O1W H2WB 134.1 . . ? 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 O1W Ni1 N1 C5 -19.6(8) . . . . ? N2 Ni1 N1 C5 1.3(3) . . . . ? Br2 Ni1 N1 C5 -152.4(3) . . . . ? Br1 Ni1 N1 C5 100.8(3) . . . . ? O1W Ni1 N1 C1 169.7(6) . . . . ? N2 Ni1 N1 C1 -169.4(3) . . . . ? Br2 Ni1 N1 C1 36.9(3) . . . . ? Br1 Ni1 N1 C1 -69.9(3) . . . . ? N1 Ni1 N2 C16 -144.7(3) . . . . ? O1W Ni1 N2 C16 31.1(3) . . . . ? Br2 Ni1 N2 C16 -57.7(4) . . . . ? Br1 Ni1 N2 C16 122.9(2) . . . . ? N1 Ni1 N2 C6 -11.4(2) . . . . ? O1W Ni1 N2 C6 164.4(2) . . . . ? Br2 Ni1 N2 C6 75.6(3) . . . . ? Br1 Ni1 N2 C6 -103.7(2) . . . . ? C5 N1 C1 C2 0.7(6) . . . . ? Ni1 N1 C1 C2 171.3(4) . . . . ? N1 C1 C2 C3 1.3(7) . . . . ? C1 C2 C3 C4 -1.1(7) . . . . ? C2 C3 C4 C5 -0.9(7) . . . . ? C1 N1 C5 C4 -2.8(6) . . . . ? Ni1 N1 C5 C4 -173.9(3) . . . . ? C1 N1 C5 C6 -179.5(4) . . . . ? Ni1 N1 C5 C6 9.4(4) . . . . ? C3 C4 C5 N1 2.9(6) . . . . ? C3 C4 C5 C6 179.6(4) . . . . ? C16 N2 C6 C5 153.8(3) . . . . ? Ni1 N2 C6 C5 18.4(3) . . . . ? C16 N2 C6 C7 -77.5(4) . . . . ? Ni1 N2 C6 C7 147.1(3) . . . . ? N1 C5 C6 N2 -18.4(5) . . . . ? C4 C5 C6 N2 164.9(4) . . . . ? N1 C5 C6 C7 -146.0(3) . . . . ? C4 C5 C6 C7 37.2(5) . . . . ? N2 C6 C7 C14 -69.7(5) . . . . ? C5 C6 C7 C14 56.4(5) . . . . ? N2 C6 C7 C8 110.3(4) . . . . ? C5 C6 C7 C8 -123.6(4) . . . . ? C14 C7 C8 C10 -0.2(6) . . . . ? C6 C7 C8 C10 179.8(4) . . . . ? C14 C7 C8 C9 -178.1(4) . . . . ? C6 C7 C8 C9 1.9(6) . . . . ? C7 C8 C10 C11 0.9(6) . . . . ? C9 C8 C10 C11 178.9(4) . . . . ? C8 C10 C11 C13 -1.4(6) . . . . ? C8 C10 C11 C12 -179.0(4) . . . . ? C10 C11 C13 C14 1.1(6) . . . . ? C12 C11 C13 C14 178.8(4) . . . . ? C11 C13 C14 C7 -0.5(6) . . . . ? C11 C13 C14 C15 179.3(4) . . . . ? C8 C7 C14 C13 0.0(6) . . . . ? C6 C7 C14 C13 -180.0(4) . . . . ? C8 C7 C14 C15 -179.7(4) . . . . ? C6 C7 C14 C15 0.3(6) . . . . ? C6 N2 C16 C24 107.4(4) . . . . ? Ni1 N2 C16 C24 -119.8(3) . . . . ? C6 N2 C16 C17 -73.6(4) . . . . ? Ni1 N2 C16 C17 59.3(4) . . . . ? C24 C16 C17 C21 -3.4(6) . . . . ? N2 C16 C17 C21 177.6(4) . . . . ? C24 C16 C17 C18 173.5(4) . . . . ? N2 C16 C17 C18 -5.6(6) . . . . ? C21 C17 C18 C19 58.2(5) . . . . ? C16 C17 C18 C19 -118.7(4) . . . . ? C21 C17 C18 C20 -65.5(5) . . . . ? C16 C17 C18 C20 117.7(4) . . . . ? C16 C17 C21 C22 0.3(6) . . . . ? C18 C17 C21 C22 -176.8(4) . . . . ? C17 C21 C22 C23 2.5(7) . . . . ? C21 C22 C23 C24 -2.4(7) . . . . ? C17 C16 C24 C23 3.5(6) . . . . ? N2 C16 C24 C23 -177.5(4) . . . . ? C17 C16 C24 C25 -174.4(4) . . . . ? N2 C16 C24 C25 4.6(6) . . . . ? C22 C23 C24 C16 -0.5(7) . . . . ? C22 C23 C24 C25 177.5(4) . . . . ? C16 C24 C25 C26 -116.6(5) . . . . ? C23 C24 C25 C26 65.6(5) . . . . ? C16 C24 C25 C27 119.6(5) . . . . ? C23 C24 C25 C27 -58.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.871 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.104 # Attachment 'combined1 and 2.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 754730' #TrackingRef 'combined1 and 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H54 Br4 Cl2 N4 Ni2' _chemical_formula_weight 1086.82 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.4583(17) _cell_length_b 15.3616(14) _cell_length_c 15.5084(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.154(2) _cell_angle_gamma 90.00 _cell_volume 4394.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8531 _cell_measurement_theta_min 2.1938 _cell_measurement_theta_max 26.9789 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 4.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1128 _exptl_absorpt_correction_T_max 0.3953 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 29190 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9553 _reflns_number_gt 6612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _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^)+(0.0400P)^2^+3.8753P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9553 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ni2 Ni 0.58985(3) 1.03956(3) 0.03871(3) 0.01565(11) Uani 1 1 d . . . Ni1 Ni -0.01814(3) 0.97000(3) 0.38805(3) 0.01596(11) Uani 1 1 d . . . Br1 Br 0.06105(2) 1.08059(2) 0.47015(3) 0.02149(10) Uani 1 1 d . . . Br2 Br -0.08617(2) 1.08342(3) 0.31343(3) 0.02787(11) Uani 1 1 d . . . Br3 Br 0.46393(2) 1.09296(2) 0.04001(3) 0.02489(11) Uani 1 1 d . . . Br4 Br 0.65243(2) 1.10780(3) -0.07922(3) 0.02498(11) Uani 1 1 d . . . N1 N -0.06983(17) 0.87097(19) 0.3236(2) 0.0178(7) Uani 1 1 d . . . N2 N 0.07157(16) 0.88551(18) 0.3777(2) 0.0161(7) Uani 1 1 d . . . H2 H 0.0480 0.9149 0.4165 0.019 Uiso 1 1 calc R . . N3 N 0.63282(16) 1.12556(19) 0.1263(2) 0.0170(7) Uani 1 1 d . . . N4 N 0.68474(16) 0.96972(18) 0.0746(2) 0.0162(7) Uani 1 1 d . . . H4 H 0.6609 0.9934 0.0303 0.019 Uiso 1 1 calc R . . C1 C -0.1394(2) 0.8729(2) 0.2923(3) 0.0208(9) Uani 1 1 d . . . H1A H -0.1692 0.9207 0.3070 0.025 Uiso 1 1 calc R . . C2 C -0.1683(2) 0.8092(2) 0.2408(3) 0.0229(9) Uani 1 1 d . . . H2A H -0.2176 0.8122 0.2210 0.027 Uiso 1 1 calc R . . C3 C -0.1254(2) 0.7398(2) 0.2174(3) 0.0257(10) Uani 1 1 d . . . H3A H -0.1441 0.6956 0.1799 0.031 Uiso 1 1 calc R . . C4 C -0.0549(2) 0.7364(2) 0.2496(3) 0.0232(9) Uani 1 1 d . . . H4A H -0.0245 0.6892 0.2351 0.028 Uiso 1 1 calc R . . C5 C -0.0287(2) 0.8023(2) 0.3035(2) 0.0155(8) Uani 1 1 d . . . C6 C 0.0464(2) 0.7980(2) 0.3444(3) 0.0211(9) Uani 1 1 d . . . H6A H 0.0806 0.7778 0.3001 0.025 Uiso 1 1 calc R . . C7 C 0.0482(2) 0.7326(3) 0.4189(3) 0.0300(10) Uani 1 1 d . . . H7A H 0.0327 0.6754 0.3972 0.045 Uiso 1 1 calc R . . H7B H 0.0154 0.7520 0.4632 0.045 Uiso 1 1 calc R . . H7C H 0.0976 0.7285 0.4438 0.045 Uiso 1 1 calc R . . C9 C 0.1381(2) 0.9179(2) 0.3408(3) 0.0172(8) Uani 1 1 d . . . C10 C 0.1390(2) 0.9396(2) 0.2527(3) 0.0201(9) Uani 1 1 d . . . C11 C 0.2038(2) 0.9686(3) 0.2200(3) 0.0270(10) Uani 1 1 d . . . H11A H 0.2055 0.9827 0.1605 0.032 Uiso 1 1 calc R . . C12 C 0.2650(2) 0.9774(3) 0.2713(3) 0.0309(11) Uani 1 1 d . . . H12A H 0.3087 0.9974 0.2474 0.037 Uiso 1 1 calc R . . C13 C 0.2634(2) 0.9573(3) 0.3575(3) 0.0284(10) Uani 1 1 d . . . H13A H 0.3061 0.9644 0.3930 0.034 Uiso 1 1 calc R . . C14 C 0.2002(2) 0.9265(2) 0.3942(3) 0.0215(9) Uani 1 1 d . . . C15 C 0.2049(2) 0.9006(3) 0.4893(3) 0.0246(9) Uani 1 1 d . . . H15A H 0.1543 0.8946 0.5095 0.030 Uiso 1 1 calc R . . C17 C 0.6810(2) 0.8780(2) 0.0949(2) 0.0165(8) Uani 1 1 d . . . C19 C 0.0734(2) 0.9308(2) 0.1908(3) 0.0237(9) Uani 1 1 d . . . H19A H 0.0301 0.9190 0.2258 0.028 Uiso 1 1 calc R . . C21 C 0.2437(2) 0.9687(3) 0.5461(3) 0.0400(12) Uani 1 1 d . . . H21A H 0.2191 1.0249 0.5389 0.060 Uiso 1 1 calc R . . H21B H 0.2941 0.9742 0.5291 0.060 Uiso 1 1 calc R . . H21C H 0.2427 0.9507 0.6066 0.060 Uiso 1 1 calc R . . C22 C 0.2422(3) 0.8120(3) 0.5004(3) 0.0426(13) Uani 1 1 d . . . H22A H 0.2169 0.7688 0.4638 0.064 Uiso 1 1 calc R . . H22B H 0.2410 0.7938 0.5609 0.064 Uiso 1 1 calc R . . H22C H 0.2927 0.8166 0.4834 0.064 Uiso 1 1 calc R . . C23 C 0.0820(3) 0.8541(3) 0.1276(3) 0.0383(12) Uani 1 1 d . . . H23A H 0.0909 0.8004 0.1603 0.057 Uiso 1 1 calc R . . H23B H 0.1229 0.8655 0.0907 0.057 Uiso 1 1 calc R . . H23C H 0.0375 0.8479 0.0916 0.057 Uiso 1 1 calc R . . C24 C 0.0586(3) 1.0137(3) 0.1386(3) 0.0384(12) Uani 1 1 d . . . H24A H 0.0526 1.0629 0.1780 0.058 Uiso 1 1 calc R . . H24B H 0.0142 1.0063 0.1026 0.058 Uiso 1 1 calc R . . H24C H 0.0995 1.0252 0.1016 0.058 Uiso 1 1 calc R . . C25 C 0.6028(2) 1.2028(2) 0.1468(3) 0.0220(9) Uani 1 1 d . . . H25A H 0.5558 1.2166 0.1237 0.026 Uiso 1 1 calc R . . C26 C 0.6382(2) 1.2622(3) 0.2003(3) 0.0261(10) Uani 1 1 d . . . H26A H 0.6160 1.3163 0.2127 0.031 Uiso 1 1 calc R . . C27 C 0.7056(2) 1.2427(3) 0.2354(3) 0.0265(10) Uani 1 1 d . . . H27A H 0.7306 1.2825 0.2727 0.032 Uiso 1 1 calc R . . C28 C 0.7362(2) 1.1635(3) 0.2151(3) 0.0259(10) Uani 1 1 d . . . H28A H 0.7825 1.1481 0.2392 0.031 Uiso 1 1 calc R . . C29 C 0.6997(2) 1.1072(2) 0.1601(2) 0.0168(8) Uani 1 1 d . . . C30 C 0.7331(2) 1.0208(2) 0.1361(3) 0.0180(8) Uani 1 1 d . . . H30A H 0.7394 0.9858 0.1902 0.022 Uiso 1 1 calc R . . C31 C 0.8078(2) 1.0323(3) 0.0989(3) 0.0315(11) Uani 1 1 d . . . H31A H 0.8277 0.9751 0.0846 0.047 Uiso 1 1 calc R . . H31B H 0.8401 1.0611 0.1415 0.047 Uiso 1 1 calc R . . H31C H 0.8036 1.0680 0.0465 0.047 Uiso 1 1 calc R . . C32 C 0.5195(2) 0.8933(3) 0.2218(3) 0.0342(11) Uani 1 1 d . . . H32A H 0.4999 0.8942 0.1621 0.051 Uiso 1 1 calc R . . H32B H 0.4946 0.9372 0.2556 0.051 Uiso 1 1 calc R . . H32C H 0.5119 0.8356 0.2468 0.051 Uiso 1 1 calc R . . C33 C 0.6316(2) 0.9128(3) 0.3156(3) 0.0360(11) Uani 1 1 d . . . H33A H 0.6835 0.9263 0.3158 0.054 Uiso 1 1 calc R . . H33B H 0.6246 0.8552 0.3411 0.054 Uiso 1 1 calc R . . H33C H 0.6066 0.9566 0.3495 0.054 Uiso 1 1 calc R . . C34 C 0.6408(2) 0.8504(2) 0.1655(3) 0.0185(8) Uani 1 1 d . . . C35 C 0.7168(2) 0.8176(2) 0.0430(3) 0.0190(8) Uani 1 1 d . . . C36 C 0.7608(2) 0.8426(2) -0.0342(3) 0.0218(9) Uani 1 1 d . . . H36A H 0.7675 0.9072 -0.0327 0.026 Uiso 1 1 calc R . . C37 C 0.8366(2) 0.8008(3) -0.0297(3) 0.0342(11) Uani 1 1 d . . . H37A H 0.8616 0.8166 0.0250 0.051 Uiso 1 1 calc R . . H37B H 0.8647 0.8220 -0.0779 0.051 Uiso 1 1 calc R . . H37C H 0.8319 0.7374 -0.0334 0.051 Uiso 1 1 calc R . . C38 C 0.7102(2) 0.7293(2) 0.0637(3) 0.0257(10) Uani 1 1 d . . . H38A H 0.7333 0.6871 0.0293 0.031 Uiso 1 1 calc R . . C39 C 0.6713(2) 0.7019(2) 0.1324(3) 0.0283(10) Uani 1 1 d . . . H39A H 0.6677 0.6416 0.1449 0.034 Uiso 1 1 calc R . . C40 C 0.6374(2) 0.7620(2) 0.1830(3) 0.0242(9) Uani 1 1 d . . . H40A H 0.6112 0.7425 0.2308 0.029 Uiso 1 1 calc R . . C41 C 0.6005(2) 0.9134(2) 0.2229(3) 0.0210(9) Uani 1 1 d . . . H41A H 0.6066 0.9734 0.1993 0.025 Uiso 1 1 calc R . . C42 C 0.7203(3) 0.8197(3) -0.1194(3) 0.0368(11) Uani 1 1 d . . . H42A H 0.6724 0.8473 -0.1210 0.055 Uiso 1 1 calc R . . H42B H 0.7147 0.7564 -0.1237 0.055 Uiso 1 1 calc R . . H42C H 0.7480 0.8409 -0.1678 0.055 Uiso 1 1 calc R . . C43 C 0.5286(3) 1.3135(3) -0.0717(4) 0.0584(16) Uani 1 1 d . . . H43A H 0.4872 1.2737 -0.0637 0.070 Uiso 1 1 calc R A 1 H43B H 0.5731 1.2779 -0.0759 0.070 Uiso 1 1 calc R A 1 Cl1 Cl 0.5132(6) 1.3780(8) -0.1724(10) 0.0563(19) Uani 0.50 1 d P B 1 Cl2 Cl 0.5376(6) 1.3828(11) 0.0142(11) 0.067(3) Uani 0.50 1 d P B 1 Cl1' Cl 0.5328(6) 1.3699(9) -0.1602(9) 0.076(3) Uani 0.50 1 d P B 2 Cl2' Cl 0.5173(7) 1.3779(11) 0.0224(12) 0.093(4) Uani 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni2 0.0126(2) 0.0173(2) 0.0170(3) -0.0009(2) -0.0009(2) 0.00029(18) Ni1 0.0163(3) 0.0164(2) 0.0152(3) -0.0012(2) 0.0003(2) 0.00045(19) Br1 0.0244(2) 0.02274(19) 0.0175(2) -0.00276(16) 0.00227(17) -0.00684(16) Br2 0.0220(2) 0.0229(2) 0.0383(3) 0.00843(18) -0.00597(19) 0.00014(16) Br3 0.01391(19) 0.0247(2) 0.0357(3) -0.01004(18) -0.00409(18) 0.00228(15) Br4 0.0243(2) 0.0301(2) 0.0208(2) 0.00482(17) 0.00420(18) -0.00067(17) N1 0.0188(17) 0.0185(15) 0.0163(18) -0.0007(13) 0.0018(14) 0.0009(13) N2 0.0117(16) 0.0181(15) 0.0188(18) -0.0027(13) 0.0056(14) 0.0025(12) N3 0.0150(17) 0.0190(15) 0.0171(18) 0.0011(13) 0.0023(14) 0.0005(12) N4 0.0119(16) 0.0171(15) 0.0189(18) 0.0014(13) -0.0072(14) 0.0001(12) C1 0.020(2) 0.0199(19) 0.022(2) 0.0007(17) -0.0007(18) 0.0029(15) C2 0.018(2) 0.028(2) 0.022(2) 0.0016(18) -0.0076(18) -0.0015(16) C3 0.030(2) 0.021(2) 0.025(2) -0.0044(18) -0.005(2) -0.0098(17) C4 0.023(2) 0.0189(19) 0.028(3) -0.0028(17) 0.0043(19) 0.0002(16) C5 0.0159(19) 0.0176(18) 0.013(2) 0.0022(15) 0.0047(16) -0.0009(15) C6 0.018(2) 0.0178(18) 0.028(2) 0.0015(17) 0.0005(18) -0.0008(15) C7 0.028(2) 0.024(2) 0.037(3) 0.0091(19) -0.011(2) -0.0023(17) C9 0.0163(19) 0.0160(17) 0.020(2) -0.0014(16) 0.0055(17) 0.0005(15) C10 0.024(2) 0.0175(18) 0.019(2) 0.0024(16) 0.0049(18) 0.0039(15) C11 0.032(3) 0.026(2) 0.024(2) 0.0040(18) 0.014(2) 0.0003(18) C12 0.026(2) 0.032(2) 0.035(3) -0.002(2) 0.014(2) -0.0048(18) C13 0.022(2) 0.028(2) 0.036(3) -0.005(2) 0.006(2) -0.0053(17) C14 0.021(2) 0.0205(19) 0.023(2) -0.0039(17) 0.0056(18) 0.0006(16) C15 0.015(2) 0.038(2) 0.021(2) -0.0040(19) -0.0007(18) -0.0026(17) C17 0.0149(19) 0.0172(18) 0.017(2) 0.0027(16) -0.0046(16) 0.0016(14) C19 0.028(2) 0.024(2) 0.019(2) 0.0035(17) 0.0042(19) 0.0029(17) C21 0.028(3) 0.056(3) 0.035(3) -0.011(2) -0.003(2) -0.007(2) C22 0.043(3) 0.046(3) 0.039(3) 0.004(2) -0.006(3) 0.010(2) C23 0.056(3) 0.037(3) 0.021(3) -0.005(2) -0.001(2) -0.003(2) C24 0.049(3) 0.035(2) 0.032(3) 0.010(2) 0.001(2) 0.005(2) C25 0.017(2) 0.0197(19) 0.030(3) -0.0033(17) 0.0043(18) 0.0033(15) C26 0.024(2) 0.022(2) 0.033(3) -0.0076(18) 0.006(2) 0.0036(17) C27 0.026(2) 0.027(2) 0.026(2) -0.0086(18) -0.0040(19) -0.0012(17) C28 0.024(2) 0.025(2) 0.028(3) -0.0022(18) -0.005(2) -0.0010(17) C29 0.017(2) 0.0191(18) 0.014(2) 0.0008(15) 0.0019(16) -0.0011(15) C30 0.017(2) 0.0169(18) 0.020(2) -0.0027(16) -0.0035(17) 0.0014(15) C31 0.017(2) 0.037(2) 0.040(3) -0.015(2) -0.002(2) -0.0020(18) C32 0.022(2) 0.044(3) 0.037(3) -0.003(2) 0.006(2) 0.0023(19) C33 0.031(3) 0.049(3) 0.027(3) -0.010(2) -0.003(2) 0.005(2) C34 0.0127(19) 0.0220(19) 0.021(2) 0.0007(16) -0.0045(17) -0.0017(15) C35 0.019(2) 0.0195(18) 0.018(2) -0.0015(16) 0.0000(17) -0.0015(15) C36 0.026(2) 0.0179(18) 0.022(2) -0.0034(17) 0.0040(18) 0.0054(16) C37 0.028(3) 0.044(3) 0.032(3) 0.005(2) 0.007(2) 0.008(2) C38 0.030(2) 0.0172(19) 0.030(3) -0.0049(18) 0.004(2) 0.0027(16) C39 0.034(3) 0.0151(19) 0.035(3) 0.0047(18) 0.000(2) -0.0005(17) C40 0.023(2) 0.026(2) 0.023(2) 0.0043(18) -0.0020(19) -0.0020(17) C41 0.015(2) 0.027(2) 0.021(2) 0.0002(17) 0.0027(17) -0.0007(16) C42 0.037(3) 0.049(3) 0.025(3) -0.001(2) 0.003(2) 0.007(2) C43 0.057(4) 0.045(3) 0.072(5) -0.003(3) -0.004(3) 0.007(3) Cl1 0.053(4) 0.050(3) 0.065(4) 0.008(2) 0.005(3) -0.023(2) Cl2 0.065(3) 0.057(3) 0.077(8) -0.005(4) -0.012(4) 0.008(3) Cl1' 0.095(8) 0.078(4) 0.057(5) -0.008(3) 0.025(5) -0.023(5) Cl2' 0.152(11) 0.075(6) 0.051(4) -0.004(4) 0.018(7) 0.057(7) _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 Ni2 N3 2.035(3) . ? Ni2 N4 2.111(3) . ? Ni2 Br4 2.4367(6) . ? Ni2 Br3 2.4657(6) . ? Ni2 Br3 2.5552(6) 3_675 ? Ni1 N1 2.038(3) . ? Ni1 N2 2.115(3) . ? Ni1 Br2 2.4171(6) . ? Ni1 Br1 2.4896(7) 3_576 ? Ni1 Br1 2.5502(6) . ? Br1 Ni1 2.4896(7) 3_576 ? Br3 Ni2 2.5552(6) 3_675 ? N1 C5 1.343(4) . ? N1 C1 1.356(5) . ? N2 C9 1.462(5) . ? N2 C6 1.507(5) . ? N2 H2 0.8800 . ? N3 C25 1.352(5) . ? N3 C29 1.352(5) . ? N4 C17 1.447(4) . ? N4 C30 1.502(5) . ? N4 H4 0.8800 . ? C1 C2 1.360(5) . ? C1 H1A 0.9500 . ? C2 C3 1.385(6) . ? C2 H2A 0.9500 . ? C3 C4 1.377(6) . ? C3 H3A 0.9500 . ? C4 C5 1.389(5) . ? C4 H4A 0.9500 . ? C5 C6 1.504(5) . ? C6 C7 1.530(5) . ? C6 H6A 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C14 1.395(5) . ? C9 C10 1.406(5) . ? C10 C11 1.391(5) . ? C10 C19 1.522(6) . ? C11 C12 1.363(6) . ? C11 H11A 0.9500 . ? C12 C13 1.375(6) . ? C12 H12A 0.9500 . ? C13 C14 1.400(5) . ? C13 H13A 0.9500 . ? C14 C15 1.528(6) . ? C15 C21 1.528(6) . ? C15 C22 1.532(6) . ? C15 H15A 1.0000 . ? C17 C35 1.409(5) . ? C17 C34 1.410(5) . ? C19 C24 1.528(6) . ? C19 C23 1.545(6) . ? C19 H19A 1.0000 . ? 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 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.381(5) . ? C25 H25A 0.9500 . ? C26 C27 1.372(6) . ? C26 H26A 0.9500 . ? C27 C28 1.382(5) . ? C27 H27A 0.9500 . ? C28 C29 1.373(5) . ? C28 H28A 0.9500 . ? C29 C30 1.516(5) . ? C30 C31 1.526(5) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C41 1.527(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C41 1.529(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C40 1.387(5) . ? C34 C41 1.528(5) . ? C35 C38 1.401(5) . ? C35 C36 1.520(5) . ? C36 C42 1.534(6) . ? C36 C37 1.538(6) . ? C36 H36A 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.372(6) . ? C38 H38A 0.9500 . ? C39 C40 1.377(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 Cl1' 1.628(15) . ? C43 Cl2 1.708(16) . ? C43 Cl2' 1.783(17) . ? C43 Cl1 1.863(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? 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 Ni2 N4 81.68(12) . . ? N3 Ni2 Br4 92.19(9) . . ? N4 Ni2 Br4 90.25(9) . . ? N3 Ni2 Br3 97.03(9) . . ? N4 Ni2 Br3 160.08(9) . . ? Br4 Ni2 Br3 109.67(2) . . ? N3 Ni2 Br3 166.19(9) . 3_675 ? N4 Ni2 Br3 91.41(8) . 3_675 ? Br4 Ni2 Br3 99.83(2) . 3_675 ? Br3 Ni2 Br3 85.39(2) . 3_675 ? N1 Ni1 N2 81.85(12) . . ? N1 Ni1 Br2 94.47(9) . . ? N2 Ni1 Br2 143.15(9) . . ? N1 Ni1 Br1 92.39(9) . 3_576 ? N2 Ni1 Br1 98.71(9) . 3_576 ? Br2 Ni1 Br1 118.11(2) . 3_576 ? N1 Ni1 Br1 172.42(9) . . ? N2 Ni1 Br1 90.63(8) . . ? Br2 Ni1 Br1 92.10(2) . . ? Br1 Ni1 Br1 87.84(2) 3_576 . ? Ni1 Br1 Ni1 92.16(2) 3_576 . ? Ni2 Br3 Ni2 94.61(2) . 3_675 ? C5 N1 C1 118.1(3) . . ? C5 N1 Ni1 116.2(2) . . ? C1 N1 Ni1 125.4(2) . . ? C9 N2 C6 115.0(3) . . ? C9 N2 Ni1 119.5(2) . . ? C6 N2 Ni1 110.0(2) . . ? C9 N2 H2 122.5 . . ? C6 N2 H2 122.5 . . ? Ni1 N2 H2 39.1 . . ? C25 N3 C29 117.9(3) . . ? C25 N3 Ni2 125.0(3) . . ? C29 N3 Ni2 116.8(2) . . ? C17 N4 C30 113.7(3) . . ? C17 N4 Ni2 120.5(2) . . ? C30 N4 Ni2 111.6(2) . . ? C17 N4 H4 123.1 . . ? C30 N4 H4 123.1 . . ? Ni2 N4 H4 36.8 . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 117.2(3) . . ? C4 C5 C6 121.1(3) . . ? C5 C6 N2 111.8(3) . . ? C5 C6 C7 109.9(3) . . ? N2 C6 C7 109.3(3) . . ? C5 C6 H6A 108.6 . . ? N2 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C14 C9 C10 121.0(4) . . ? C14 C9 N2 118.9(3) . . ? C10 C9 N2 120.1(3) . . ? C11 C10 C9 118.1(4) . . ? C11 C10 C19 118.3(4) . . ? C9 C10 C19 123.6(4) . . ? C12 C11 C10 121.7(4) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C9 C14 C13 118.0(4) . . ? C9 C14 C15 124.4(3) . . ? C13 C14 C15 117.5(4) . . ? C14 C15 C21 112.7(4) . . ? C14 C15 C22 110.4(4) . . ? C21 C15 C22 110.2(4) . . ? C14 C15 H15A 107.8 . . ? C21 C15 H15A 107.8 . . ? C22 C15 H15A 107.8 . . ? C35 C17 C34 121.2(3) . . ? C35 C17 N4 119.3(3) . . ? C34 C17 N4 119.5(3) . . ? C10 C19 C24 112.5(3) . . ? C10 C19 C23 111.7(3) . . ? C24 C19 C23 108.6(4) . . ? C10 C19 H19A 107.9 . . ? C24 C19 H19A 107.9 . . ? C23 C19 H19A 107.9 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 122.2(4) . . ? N3 C25 H25A 118.9 . . ? C26 C25 H25A 118.9 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 118.2(4) . . ? C26 C27 H27A 120.9 . . ? C28 C27 H27A 120.9 . . ? C29 C28 C27 120.1(4) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? N3 C29 C28 121.9(3) . . ? N3 C29 C30 117.4(3) . . ? C28 C29 C30 120.7(3) . . ? N4 C30 C29 112.1(3) . . ? N4 C30 C31 110.1(3) . . ? C29 C30 C31 111.9(3) . . ? N4 C30 H30A 107.5 . . ? C29 C30 H30A 107.5 . . ? C31 C30 H30A 107.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C41 C32 H32A 109.5 . . ? C41 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C41 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C41 C33 H33A 109.5 . . ? C41 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C41 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C40 C34 C17 118.4(4) . . ? C40 C34 C41 118.7(4) . . ? C17 C34 C41 123.0(3) . . ? C38 C35 C17 117.3(4) . . ? C38 C35 C36 118.6(3) . . ? C17 C35 C36 124.1(3) . . ? C35 C36 C42 111.2(3) . . ? C35 C36 C37 111.8(3) . . ? C42 C36 C37 110.9(3) . . ? C35 C36 H36A 107.6 . . ? C42 C36 H36A 107.6 . . ? C37 C36 H36A 107.6 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C35 121.8(4) . . ? C39 C38 H38A 119.1 . . ? C35 C38 H38A 119.1 . . ? C38 C39 C40 119.9(4) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C39 C40 C34 121.3(4) . . ? C39 C40 H40A 119.3 . . ? C34 C40 H40A 119.3 . . ? C32 C41 C34 111.3(3) . . ? C32 C41 C33 110.0(4) . . ? C34 C41 C33 111.8(3) . . ? C32 C41 H41A 107.8 . . ? C34 C41 H41A 107.8 . . ? C33 C41 H41A 107.8 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Cl1' C43 Cl2 108.6(8) . . ? Cl1' C43 Cl2' 113.9(8) . . ? Cl2 C43 Cl2' 13.2(7) . . ? Cl1' C43 Cl1 11.5(7) . . ? Cl2 C43 Cl1 109.2(8) . . ? Cl2' C43 Cl1 111.8(8) . . ? Cl1' C43 H43A 119.7 . . ? Cl2 C43 H43A 109.8 . . ? Cl2' C43 H43A 97.2 . . ? Cl1 C43 H43A 109.8 . . ? Cl1' C43 H43B 100.0 . . ? Cl2 C43 H43B 109.8 . . ? Cl2' C43 H43B 118.9 . . ? Cl1 C43 H43B 109.8 . . ? H43A C43 H43B 108.3 . . ? 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 Ni1 Br1 Ni1 -91.9(7) . . . 3_576 ? N2 Ni1 Br1 Ni1 -98.69(9) . . . 3_576 ? Br2 Ni1 Br1 Ni1 118.06(2) . . . 3_576 ? Br1 Ni1 Br1 Ni1 0.0 3_576 . . 3_576 ? N3 Ni2 Br3 Ni2 -166.33(9) . . . 3_675 ? N4 Ni2 Br3 Ni2 -81.4(2) . . . 3_675 ? Br4 Ni2 Br3 Ni2 98.80(3) . . . 3_675 ? Br3 Ni2 Br3 Ni2 0.0 3_675 . . 3_675 ? N2 Ni1 N1 C5 -0.7(3) . . . . ? Br2 Ni1 N1 C5 142.4(3) . . . . ? Br1 Ni1 N1 C5 -99.2(3) 3_576 . . . ? Br1 Ni1 N1 C5 -7.6(9) . . . . ? N2 Ni1 N1 C1 -173.6(3) . . . . ? Br2 Ni1 N1 C1 -30.6(3) . . . . ? Br1 Ni1 N1 C1 87.9(3) 3_576 . . . ? Br1 Ni1 N1 C1 179(48) . . . . ? N1 Ni1 N2 C9 126.8(3) . . . . ? Br2 Ni1 N2 C9 40.3(3) . . . . ? Br1 Ni1 N2 C9 -142.0(3) 3_576 . . . ? Br1 Ni1 N2 C9 -54.1(3) . . . . ? N1 Ni1 N2 C6 -9.4(2) . . . . ? Br2 Ni1 N2 C6 -95.9(2) . . . . ? Br1 Ni1 N2 C6 81.8(2) 3_576 . . . ? Br1 Ni1 N2 C6 169.7(2) . . . . ? N4 Ni2 N3 C25 179.0(3) . . . . ? Br4 Ni2 N3 C25 89.1(3) . . . . ? Br3 Ni2 N3 C25 -21.0(3) . . . . ? Br3 Ni2 N3 C25 -120.4(4) 3_675 . . . ? N4 Ni2 N3 C29 5.6(3) . . . . ? Br4 Ni2 N3 C29 -84.3(3) . . . . ? Br3 Ni2 N3 C29 165.6(3) . . . . ? Br3 Ni2 N3 C29 66.2(5) 3_675 . . . ? N3 Ni2 N4 C17 132.9(3) . . . . ? Br4 Ni2 N4 C17 -134.9(3) . . . . ? Br3 Ni2 N4 C17 45.2(4) . . . . ? Br3 Ni2 N4 C17 -35.1(3) 3_675 . . . ? N3 Ni2 N4 C30 -4.4(2) . . . . ? Br4 Ni2 N4 C30 87.7(2) . . . . ? Br3 Ni2 N4 C30 -92.1(3) . . . . ? Br3 Ni2 N4 C30 -172.4(2) 3_675 . . . ? C5 N1 C1 C2 -1.1(6) . . . . ? Ni1 N1 C1 C2 171.8(3) . . . . ? N1 C1 C2 C3 -1.2(6) . . . . ? C1 C2 C3 C4 2.1(6) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C1 N1 C5 C4 2.5(6) . . . . ? Ni1 N1 C5 C4 -171.0(3) . . . . ? C1 N1 C5 C6 -175.3(3) . . . . ? Ni1 N1 C5 C6 11.2(4) . . . . ? C3 C4 C5 N1 -1.6(6) . . . . ? C3 C4 C5 C6 176.1(4) . . . . ? N1 C5 C6 N2 -19.1(5) . . . . ? C4 C5 C6 N2 163.1(3) . . . . ? N1 C5 C6 C7 102.5(4) . . . . ? C4 C5 C6 C7 -75.3(5) . . . . ? C9 N2 C6 C5 -121.3(3) . . . . ? Ni1 N2 C6 C5 17.1(4) . . . . ? C9 N2 C6 C7 116.8(4) . . . . ? Ni1 N2 C6 C7 -104.9(3) . . . . ? C6 N2 C9 C14 -113.7(4) . . . . ? Ni1 N2 C9 C14 112.1(3) . . . . ? C6 N2 C9 C10 66.0(4) . . . . ? Ni1 N2 C9 C10 -68.1(4) . . . . ? C14 C9 C10 C11 0.9(5) . . . . ? N2 C9 C10 C11 -178.8(3) . . . . ? C14 C9 C10 C19 179.4(3) . . . . ? N2 C9 C10 C19 -0.4(5) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C19 C10 C11 C12 -179.5(4) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C14 0.9(6) . . . . ? C10 C9 C14 C13 0.0(5) . . . . ? N2 C9 C14 C13 179.7(3) . . . . ? C10 C9 C14 C15 -177.0(3) . . . . ? N2 C9 C14 C15 2.7(5) . . . . ? C12 C13 C14 C9 -0.9(6) . . . . ? C12 C13 C14 C15 176.3(4) . . . . ? C9 C14 C15 C21 -135.8(4) . . . . ? C13 C14 C15 C21 47.2(5) . . . . ? C9 C14 C15 C22 100.5(4) . . . . ? C13 C14 C15 C22 -76.5(5) . . . . ? C30 N4 C17 C35 -106.7(4) . . . . ? Ni2 N4 C17 C35 116.7(3) . . . . ? C30 N4 C17 C34 74.2(4) . . . . ? Ni2 N4 C17 C34 -62.3(4) . . . . ? C11 C10 C19 C24 -51.9(5) . . . . ? C9 C10 C19 C24 129.7(4) . . . . ? C11 C10 C19 C23 70.6(5) . . . . ? C9 C10 C19 C23 -107.8(4) . . . . ? C29 N3 C25 C26 0.1(6) . . . . ? Ni2 N3 C25 C26 -173.3(3) . . . . ? N3 C25 C26 C27 -1.0(6) . . . . ? C25 C26 C27 C28 0.5(6) . . . . ? C26 C27 C28 C29 0.9(7) . . . . ? C25 N3 C29 C28 1.5(6) . . . . ? Ni2 N3 C29 C28 175.3(3) . . . . ? C25 N3 C29 C30 -179.5(3) . . . . ? Ni2 N3 C29 C30 -5.6(4) . . . . ? C27 C28 C29 N3 -2.0(6) . . . . ? C27 C28 C29 C30 179.0(4) . . . . ? C17 N4 C30 C29 -137.5(3) . . . . ? Ni2 N4 C30 C29 2.9(4) . . . . ? C17 N4 C30 C31 97.2(4) . . . . ? Ni2 N4 C30 C31 -122.4(3) . . . . ? N3 C29 C30 N4 1.6(5) . . . . ? C28 C29 C30 N4 -179.3(4) . . . . ? N3 C29 C30 C31 125.9(4) . . . . ? C28 C29 C30 C31 -55.0(5) . . . . ? C35 C17 C34 C40 0.2(6) . . . . ? N4 C17 C34 C40 179.2(3) . . . . ? C35 C17 C34 C41 -179.3(3) . . . . ? N4 C17 C34 C41 -0.3(5) . . . . ? C34 C17 C35 C38 0.6(6) . . . . ? N4 C17 C35 C38 -178.4(3) . . . . ? C34 C17 C35 C36 179.8(4) . . . . ? N4 C17 C35 C36 0.8(6) . . . . ? C38 C35 C36 C42 72.9(5) . . . . ? C17 C35 C36 C42 -106.3(4) . . . . ? C38 C35 C36 C37 -51.7(5) . . . . ? C17 C35 C36 C37 129.1(4) . . . . ? C17 C35 C38 C39 -0.7(6) . . . . ? C36 C35 C38 C39 -179.9(4) . . . . ? C35 C38 C39 C40 0.0(7) . . . . ? C38 C39 C40 C34 0.9(7) . . . . ? C17 C34 C40 C39 -1.0(6) . . . . ? C41 C34 C40 C39 178.5(4) . . . . ? C40 C34 C41 C32 -58.9(5) . . . . ? C17 C34 C41 C32 120.6(4) . . . . ? C40 C34 C41 C33 64.6(5) . . . . ? C17 C34 C41 C33 -115.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.931 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.118