# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Ni1 _database_code_depnum_ccdc_archive 'CCDC 917315' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Br2 N2 Ni' _chemical_formula_weight 663.13 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' _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 10.642(2) _cell_length_b 20.891(4) _cell_length_c 13.085(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.26(3) _cell_angle_gamma 90.00 _cell_volume 2885.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 3.465 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.2163 _exptl_absorpt_correction_T_max 1.0000 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19252 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6546 _reflns_number_gt 5421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+5.9122P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6546 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0811 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Br1 Br 0.14045(5) 0.12985(3) 0.81450(4) 0.04233(16) Uani 1 1 d . . . N1 N -0.1725(3) 0.14808(18) 0.7090(3) 0.0260(7) Uani 1 1 d . . . Ni1 Ni -0.03417(5) 0.19852(3) 0.79411(4) 0.03077(16) Uani 1 1 d . . . N2 N -0.1458(3) 0.18586(17) 0.9079(3) 0.0259(8) Uani 1 1 d . . . Br2 Br -0.02583(6) 0.30698(3) 0.75893(5) 0.05323(19) Uani 1 1 d . . . C10 C -0.3557(4) 0.1295(2) 0.9192(3) 0.0286(9) Uani 1 1 d . . . C13 C -0.1248(4) 0.2079(2) 1.0133(3) 0.0276(9) Uani 1 1 d . . . C25 C -0.1799(4) 0.1266(2) 0.6029(3) 0.0271(9) Uani 1 1 d . . . C26 C -0.1411(4) 0.0643(2) 0.5833(4) 0.0315(10) Uani 1 1 d . . . C1 C -0.2584(4) 0.1305(2) 0.7640(3) 0.0271(9) Uani 1 1 d . . . C3 C -0.4300(4) 0.0561(2) 0.6645(4) 0.0355(11) Uani 1 1 d . . . H3A H -0.3967 0.0549 0.6005 0.043 Uiso 1 1 calc R . . C11 C -0.4253(4) 0.0925(2) 0.8405(4) 0.0300(9) Uani 1 1 d . . . C12 C -0.2455(4) 0.1537(2) 0.8742(3) 0.0263(9) Uani 1 1 d . . . C31 C -0.2704(6) 0.2354(3) 0.5484(4) 0.0475(13) Uani 1 1 d . . . H31A H -0.2611 0.2416 0.6231 0.071 Uiso 1 1 calc R . . H31B H -0.3599 0.2393 0.5203 0.071 Uiso 1 1 calc R . . H31C H -0.2209 0.2678 0.5170 0.071 Uiso 1 1 calc R . . C16 C -0.0809(5) 0.2500(2) 1.2152(4) 0.0396(12) Uani 1 1 d . . . H16A H -0.0660 0.2645 1.2844 0.048 Uiso 1 1 calc R . . C18 C -0.0548(4) 0.1686(2) 1.0870(3) 0.0283(9) Uani 1 1 d . . . C22 C -0.2478(5) 0.3109(3) 0.9604(4) 0.0427(13) Uani 1 1 d . . . H22A H -0.2474 0.2916 0.8905 0.051 Uiso 1 1 calc R . . C27 C -0.1485(4) 0.0455(3) 0.4805(4) 0.0355(11) Uani 1 1 d . . . H27A H -0.1248 0.0032 0.4643 0.043 Uiso 1 1 calc R . . C2 C -0.3727(4) 0.0913(2) 0.7454(3) 0.0291(9) Uani 1 1 d . . . C9 C -0.3990(4) 0.1342(2) 1.0140(4) 0.0357(11) Uani 1 1 d . . . H9A H -0.3539 0.1584 1.0682 0.043 Uiso 1 1 calc R . . C28 C -0.1898(5) 0.0875(3) 0.4019(4) 0.0418(13) Uani 1 1 d . . . H28A H -0.1927 0.0741 0.3323 0.050 Uiso 1 1 calc R . . C29 C -0.2268(5) 0.1484(3) 0.4235(4) 0.0419(12) Uani 1 1 d . . . H29A H -0.2552 0.1766 0.3685 0.050 Uiso 1 1 calc R . . C30 C -0.2232(4) 0.1696(2) 0.5246(3) 0.0335(10) Uani 1 1 d . . . C19 C -0.0056(4) 0.1025(2) 1.0619(3) 0.0307(10) Uani 1 1 d . . . H19A H -0.0127 0.0986 0.9852 0.037 Uiso 1 1 calc R . . C32 C -0.0965(5) 0.0187(2) 0.6687(4) 0.0421(12) Uani 1 1 d . . . H32A H -0.0737 -0.0222 0.6394 0.063 Uiso 1 1 calc R . . H32B H -0.1644 0.0118 0.7116 0.063 Uiso 1 1 calc R . . H32C H -0.0223 0.0367 0.7109 0.063 Uiso 1 1 calc R . . C17 C -0.0354(5) 0.1907(2) 1.1885(4) 0.0356(11) Uani 1 1 d . . . H17A H 0.0099 0.1647 1.2402 0.043 Uiso 1 1 calc R . . C21 C 0.1322(5) 0.0931(3) 1.1041(4) 0.0423(12) Uani 1 1 d . . . H21A H 0.1833 0.1268 1.0775 0.063 Uiso 1 1 calc R . . H21B H 0.1609 0.0512 1.0827 0.063 Uiso 1 1 calc R . . H21C H 0.1417 0.0954 1.1795 0.063 Uiso 1 1 calc R . . C6 C -0.5367(4) 0.0598(2) 0.8543(4) 0.0345(10) Uani 1 1 d . . . C14 C -0.1712(4) 0.2678(2) 1.0381(4) 0.0322(10) Uani 1 1 d . . . C4 C -0.5410(5) 0.0214(3) 0.6793(4) 0.0438(13) Uani 1 1 d . . . H4A H -0.5806 -0.0040 0.6242 0.053 Uiso 1 1 calc R . . C7 C -0.5781(5) 0.0657(3) 0.9526(4) 0.0412(12) Uani 1 1 d . . . H7A H -0.6529 0.0443 0.9663 0.049 Uiso 1 1 calc R . . C15 C -0.1475(5) 0.2872(3) 1.1410(4) 0.0383(11) Uani 1 1 d . . . H15A H -0.1786 0.3275 1.1600 0.046 Uiso 1 1 calc R . . C8 C -0.5117(5) 0.1021(3) 1.0283(4) 0.0423(12) Uani 1 1 d . . . H8A H -0.5431 0.1058 1.0929 0.051 Uiso 1 1 calc R . . C20 C -0.0890(5) 0.0509(2) 1.1007(4) 0.0399(11) Uani 1 1 d . . . H20A H -0.0574 0.0086 1.0840 0.060 Uiso 1 1 calc R . . H20B H -0.1762 0.0561 1.0674 0.060 Uiso 1 1 calc R . . H20C H -0.0870 0.0548 1.1755 0.060 Uiso 1 1 calc R . . C5 C -0.5935(4) 0.0228(3) 0.7697(4) 0.0429(12) Uani 1 1 d . . . H5A H -0.6682 -0.0010 0.7758 0.051 Uiso 1 1 calc R . . C23 C -0.3859(6) 0.3150(3) 0.9823(5) 0.0591(17) Uani 1 1 d . . . H23A H -0.4220 0.2718 0.9821 0.089 Uiso 1 1 calc R . . H23B H -0.4349 0.3409 0.9290 0.089 Uiso 1 1 calc R . . H23C H -0.3889 0.3348 1.0499 0.089 Uiso 1 1 calc R . . C24 C -0.1894(7) 0.3778(3) 0.9588(5) 0.0644(18) Uani 1 1 d . . . H24A H -0.1015 0.3743 0.9443 0.097 Uiso 1 1 calc R . . H24B H -0.1912 0.3983 1.0260 0.097 Uiso 1 1 calc R . . H24C H -0.2380 0.4036 0.9051 0.097 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 Br1 0.0311(2) 0.0529(3) 0.0447(3) 0.0071(2) 0.0113(2) 0.0024(2) N1 0.0255(17) 0.0320(19) 0.0214(17) 0.0034(15) 0.0064(14) 0.0029(15) Ni1 0.0273(3) 0.0384(3) 0.0273(3) 0.0006(2) 0.0061(2) -0.0067(2) N2 0.0255(17) 0.0313(19) 0.0214(17) -0.0010(15) 0.0046(14) 0.0016(15) Br2 0.0583(4) 0.0427(3) 0.0581(4) 0.0128(3) 0.0047(3) -0.0084(3) C10 0.023(2) 0.035(2) 0.028(2) 0.0000(18) 0.0054(17) 0.0026(18) C13 0.0223(19) 0.035(2) 0.026(2) -0.0031(18) 0.0048(16) -0.0015(18) C25 0.0236(19) 0.034(2) 0.024(2) 0.0001(18) 0.0053(16) -0.0035(18) C26 0.026(2) 0.036(2) 0.033(2) -0.002(2) 0.0055(18) -0.0030(19) C1 0.027(2) 0.030(2) 0.024(2) -0.0018(17) 0.0031(17) 0.0021(18) C3 0.030(2) 0.048(3) 0.029(2) -0.009(2) 0.0060(18) -0.006(2) C11 0.023(2) 0.034(2) 0.033(2) 0.0001(19) 0.0059(17) -0.0016(18) C12 0.0223(19) 0.031(2) 0.026(2) -0.0007(18) 0.0024(16) 0.0011(17) C31 0.051(3) 0.045(3) 0.044(3) 0.004(2) -0.002(2) 0.011(3) C16 0.045(3) 0.045(3) 0.029(2) -0.010(2) 0.003(2) -0.003(2) C18 0.028(2) 0.032(2) 0.025(2) -0.0009(18) 0.0077(17) -0.0013(18) C22 0.046(3) 0.046(3) 0.034(3) -0.006(2) -0.004(2) 0.021(2) C27 0.027(2) 0.048(3) 0.033(2) -0.010(2) 0.0098(19) -0.008(2) C2 0.0231(19) 0.034(2) 0.031(2) -0.0038(19) 0.0054(17) -0.0005(18) C9 0.030(2) 0.046(3) 0.032(2) -0.009(2) 0.0077(19) 0.000(2) C28 0.033(2) 0.070(4) 0.023(2) -0.014(2) 0.0071(19) -0.012(2) C29 0.031(2) 0.071(4) 0.023(2) 0.006(2) 0.0015(19) -0.009(2) C30 0.029(2) 0.047(3) 0.024(2) 0.001(2) 0.0023(17) 0.002(2) C19 0.038(2) 0.028(2) 0.027(2) 0.0022(18) 0.0096(19) 0.0058(19) C32 0.048(3) 0.037(3) 0.041(3) 0.001(2) 0.004(2) 0.002(2) C17 0.042(3) 0.039(3) 0.025(2) 0.001(2) 0.003(2) 0.002(2) C21 0.042(3) 0.042(3) 0.044(3) 0.006(2) 0.009(2) 0.006(2) C6 0.023(2) 0.041(3) 0.041(3) -0.002(2) 0.0090(19) -0.001(2) C14 0.029(2) 0.037(2) 0.030(2) -0.005(2) 0.0041(18) 0.003(2) C4 0.032(2) 0.059(3) 0.040(3) -0.013(3) 0.002(2) -0.013(2) C7 0.031(2) 0.052(3) 0.044(3) -0.004(2) 0.017(2) -0.006(2) C15 0.038(3) 0.040(3) 0.038(3) -0.006(2) 0.006(2) 0.005(2) C8 0.035(2) 0.059(3) 0.037(3) -0.007(2) 0.018(2) -0.002(2) C20 0.044(3) 0.038(3) 0.040(3) 0.002(2) 0.011(2) -0.003(2) C5 0.025(2) 0.055(3) 0.050(3) -0.011(3) 0.008(2) -0.014(2) C23 0.045(3) 0.073(4) 0.055(4) -0.018(3) -0.007(3) 0.028(3) C24 0.092(5) 0.041(3) 0.056(4) 0.001(3) -0.005(4) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ni1 2.3361(9) . ? N1 C1 1.286(5) . ? N1 C25 1.451(5) . ? N1 Ni1 2.026(4) . ? Ni1 N2 2.035(4) . ? Ni1 Br2 2.3161(10) . ? N2 C12 1.286(5) . ? N2 C13 1.445(5) . ? C10 C9 1.380(6) . ? C10 C11 1.419(6) . ? C10 C12 1.467(6) . ? C13 C14 1.398(6) . ? C13 C18 1.406(6) . ? C25 C30 1.397(6) . ? C25 C26 1.399(6) . ? C26 C27 1.393(6) . ? C26 C32 1.498(7) . ? C1 C2 1.461(6) . ? C1 C12 1.511(6) . ? C3 C2 1.368(6) . ? C3 C4 1.420(7) . ? C3 H3A 0.9500 . ? C11 C6 1.400(6) . ? C11 C2 1.428(6) . ? C31 C30 1.507(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C16 C15 1.370(7) . ? C16 C17 1.391(7) . ? C16 H16A 0.9500 . ? C18 C17 1.396(6) . ? C18 C19 1.528(6) . ? C22 C14 1.517(7) . ? C22 C24 1.530(8) . ? C22 C23 1.535(8) . ? C22 H22A 1.0000 . ? C27 C28 1.381(7) . ? C27 H27A 0.9500 . ? C9 C8 1.407(7) . ? C9 H9A 0.9500 . ? C28 C29 1.372(8) . ? C28 H28A 0.9500 . ? C29 C30 1.391(7) . ? C29 H29A 0.9500 . ? C19 C21 1.513(7) . ? C19 C20 1.523(7) . ? C19 H19A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C17 H17A 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C6 C7 1.418(7) . ? C6 C5 1.420(7) . ? C14 C15 1.398(7) . ? C4 C5 1.370(7) . ? C4 H4A 0.9500 . ? C7 C8 1.371(7) . ? C7 H7A 0.9500 . ? C15 H15A 0.9500 . ? C8 H8A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C5 H5A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C25 119.4(4) . . ? C1 N1 Ni1 111.0(3) . . ? C25 N1 Ni1 129.4(3) . . ? N1 Ni1 N2 83.33(14) . . ? N1 Ni1 Br2 116.29(11) . . ? N2 Ni1 Br2 108.24(11) . . ? N1 Ni1 Br1 104.82(11) . . ? N2 Ni1 Br1 111.47(10) . . ? Br2 Ni1 Br1 125.00(3) . . ? C12 N2 C13 121.0(4) . . ? C12 N2 Ni1 110.5(3) . . ? C13 N2 Ni1 128.5(3) . . ? C9 C10 C11 119.2(4) . . ? C9 C10 C12 135.3(4) . . ? C11 C10 C12 105.5(4) . . ? C14 C13 C18 122.4(4) . . ? C14 C13 N2 119.3(4) . . ? C18 C13 N2 118.3(4) . . ? C30 C25 C26 122.8(4) . . ? C30 C25 N1 118.4(4) . . ? C26 C25 N1 118.8(4) . . ? C27 C26 C25 117.2(4) . . ? C27 C26 C32 121.0(5) . . ? C25 C26 C32 121.8(4) . . ? N1 C1 C2 134.6(4) . . ? N1 C1 C12 117.2(4) . . ? C2 C1 C12 108.2(4) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 H3A 121.1 . . ? C4 C3 H3A 121.1 . . ? C6 C11 C10 123.1(4) . . ? C6 C11 C2 122.4(4) . . ? C10 C11 C2 114.6(4) . . ? N2 C12 C10 135.2(4) . . ? N2 C12 C1 117.8(4) . . ? C10 C12 C1 107.0(4) . . ? 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 . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C17 C18 C13 117.5(4) . . ? C17 C18 C19 119.3(4) . . ? C13 C18 C19 123.2(4) . . ? C14 C22 C24 111.5(5) . . ? C14 C22 C23 110.7(5) . . ? C24 C22 C23 110.6(5) . . ? C14 C22 H22A 108.0 . . ? C24 C22 H22A 108.0 . . ? C23 C22 H22A 108.0 . . ? C28 C27 C26 120.9(5) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C3 C2 C11 119.9(4) . . ? C3 C2 C1 135.3(4) . . ? C11 C2 C1 104.8(4) . . ? C10 C9 C8 118.2(4) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 121.1(5) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C30 C25 117.4(5) . . ? C29 C30 C31 121.1(5) . . ? C25 C30 C31 121.5(4) . . ? C21 C19 C20 111.5(4) . . ? C21 C19 C18 112.4(4) . . ? C20 C19 C18 109.8(4) . . ? C21 C19 H19A 107.7 . . ? C20 C19 H19A 107.7 . . ? C18 C19 H19A 107.7 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C16 C17 C18 121.2(4) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C6 C7 116.1(4) . . ? C11 C6 C5 116.7(4) . . ? C7 C6 C5 127.2(4) . . ? C13 C14 C15 117.2(4) . . ? C13 C14 C22 123.5(4) . . ? C15 C14 C22 119.3(4) . . ? C5 C4 C3 122.9(5) . . ? C5 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? C8 C7 C6 120.9(5) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C16 C15 C14 122.2(5) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C7 C8 C9 122.6(5) . . ? C7 C8 H8A 118.7 . . ? C9 C8 H8A 118.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? 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 . . ? 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 C1 N1 Ni1 N2 -2.4(3) . . . . ? C25 N1 Ni1 N2 -177.1(4) . . . . ? C1 N1 Ni1 Br2 -109.5(3) . . . . ? C25 N1 Ni1 Br2 75.8(4) . . . . ? C1 N1 Ni1 Br1 108.1(3) . . . . ? C25 N1 Ni1 Br1 -66.6(4) . . . . ? N1 Ni1 N2 C12 0.1(3) . . . . ? Br2 Ni1 N2 C12 115.6(3) . . . . ? Br1 Ni1 N2 C12 -103.3(3) . . . . ? N1 Ni1 N2 C13 -179.9(4) . . . . ? Br2 Ni1 N2 C13 -64.3(4) . . . . ? Br1 Ni1 N2 C13 76.8(4) . . . . ? C12 N2 C13 C14 -89.6(5) . . . . ? Ni1 N2 C13 C14 90.3(5) . . . . ? C12 N2 C13 C18 92.2(5) . . . . ? Ni1 N2 C13 C18 -87.9(5) . . . . ? C1 N1 C25 C30 102.7(5) . . . . ? Ni1 N1 C25 C30 -83.0(5) . . . . ? C1 N1 C25 C26 -78.5(5) . . . . ? Ni1 N1 C25 C26 95.8(5) . . . . ? C30 C25 C26 C27 -0.7(7) . . . . ? N1 C25 C26 C27 -179.5(4) . . . . ? C30 C25 C26 C32 -179.2(4) . . . . ? N1 C25 C26 C32 2.1(6) . . . . ? C25 N1 C1 C2 -0.6(7) . . . . ? Ni1 N1 C1 C2 -175.9(4) . . . . ? C25 N1 C1 C12 179.4(4) . . . . ? Ni1 N1 C1 C12 4.1(5) . . . . ? C9 C10 C11 C6 -0.3(7) . . . . ? C12 C10 C11 C6 178.5(4) . . . . ? C9 C10 C11 C2 179.5(4) . . . . ? C12 C10 C11 C2 -1.6(5) . . . . ? C13 N2 C12 C10 -1.4(8) . . . . ? Ni1 N2 C12 C10 178.7(4) . . . . ? C13 N2 C12 C1 -178.1(4) . . . . ? Ni1 N2 C12 C1 2.0(5) . . . . ? C9 C10 C12 N2 3.8(9) . . . . ? C11 C10 C12 N2 -174.8(5) . . . . ? C9 C10 C12 C1 -179.3(5) . . . . ? C11 C10 C12 C1 2.1(5) . . . . ? N1 C1 C12 N2 -4.3(6) . . . . ? C2 C1 C12 N2 175.7(4) . . . . ? N1 C1 C12 C10 178.1(4) . . . . ? C2 C1 C12 C10 -1.9(5) . . . . ? C14 C13 C18 C17 1.7(7) . . . . ? N2 C13 C18 C17 179.9(4) . . . . ? C14 C13 C18 C19 178.8(4) . . . . ? N2 C13 C18 C19 -3.1(6) . . . . ? C25 C26 C27 C28 1.4(7) . . . . ? C32 C26 C27 C28 179.9(4) . . . . ? C4 C3 C2 C11 -0.3(7) . . . . ? C4 C3 C2 C1 177.1(5) . . . . ? C6 C11 C2 C3 -1.6(7) . . . . ? C10 C11 C2 C3 178.6(4) . . . . ? C6 C11 C2 C1 -179.7(4) . . . . ? C10 C11 C2 C1 0.5(5) . . . . ? N1 C1 C2 C3 3.2(9) . . . . ? C12 C1 C2 C3 -176.8(5) . . . . ? N1 C1 C2 C11 -179.1(5) . . . . ? C12 C1 C2 C11 0.9(5) . . . . ? C11 C10 C9 C8 -0.4(7) . . . . ? C12 C10 C9 C8 -178.9(5) . . . . ? C26 C27 C28 C29 -1.2(7) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? C28 C29 C30 C25 0.4(7) . . . . ? C28 C29 C30 C31 -176.7(5) . . . . ? C26 C25 C30 C29 -0.2(7) . . . . ? N1 C25 C30 C29 178.6(4) . . . . ? C26 C25 C30 C31 176.9(5) . . . . ? N1 C25 C30 C31 -4.3(7) . . . . ? C17 C18 C19 C21 -50.6(6) . . . . ? C13 C18 C19 C21 132.4(5) . . . . ? C17 C18 C19 C20 74.1(5) . . . . ? C13 C18 C19 C20 -102.9(5) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? C13 C18 C17 C16 -1.5(7) . . . . ? C19 C18 C17 C16 -178.6(5) . . . . ? C10 C11 C6 C7 0.3(7) . . . . ? C2 C11 C6 C7 -179.5(4) . . . . ? C10 C11 C6 C5 -177.8(5) . . . . ? C2 C11 C6 C5 2.4(7) . . . . ? C18 C13 C14 C15 -1.2(7) . . . . ? N2 C13 C14 C15 -179.4(4) . . . . ? C18 C13 C14 C22 -179.5(5) . . . . ? N2 C13 C14 C22 2.3(7) . . . . ? C24 C22 C14 C13 -125.9(5) . . . . ? C23 C22 C14 C13 110.4(5) . . . . ? C24 C22 C14 C15 55.8(7) . . . . ? C23 C22 C14 C15 -67.8(6) . . . . ? C2 C3 C4 C5 1.3(8) . . . . ? C11 C6 C7 C8 0.5(8) . . . . ? C5 C6 C7 C8 178.4(5) . . . . ? C17 C16 C15 C14 -0.3(8) . . . . ? C13 C14 C15 C16 0.5(7) . . . . ? C22 C14 C15 C16 178.9(5) . . . . ? C6 C7 C8 C9 -1.3(9) . . . . ? C10 C9 C8 C7 1.2(8) . . . . ? C3 C4 C5 C6 -0.5(9) . . . . ? C11 C6 C5 C4 -1.4(8) . . . . ? C7 C6 C5 C4 -179.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.673 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.110 data_Ni2-1 _database_code_depnum_ccdc_archive 'CCDC 917316' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H64 Br4 N4 Ni2' _chemical_formula_weight 1338.26 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.690(6) _cell_length_b 15.864(8) _cell_length_c 21.146(9) _cell_angle_alpha 73.538(19) _cell_angle_beta 80.11(2) _cell_angle_gamma 86.028(17) _cell_volume 3387(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10204 _cell_measurement_theta_min 1.8920 _cell_measurement_theta_max 27.3739 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 2.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5190 _exptl_absorpt_correction_T_max 1.0000 _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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28706 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 27.32 _reflns_number_total 14964 _reflns_number_gt 7732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+7.9495P] 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 14964 _refine_ls_number_parameters 678 _refine_ls_number_restraints 918 _refine_ls_R_factor_all 0.1770 _refine_ls_R_factor_gt 0.1090 _refine_ls_wR_factor_ref 0.3112 _refine_ls_wR_factor_gt 0.2659 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.031 _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 Br3 Br 1.12206(13) 1.17571(8) 0.54450(5) 0.0871(4) Uani 1 1 d U . . Ni2 Ni 1.24681(14) 1.27128(8) 0.45415(6) 0.0661(4) Uani 1 1 d U . . Br2 Br 1.70395(13) 0.75931(10) 0.03306(6) 0.0970(4) Uani 1 1 d U . . Ni1 Ni 1.57542(11) 0.67420(8) 0.12630(6) 0.0587(3) Uani 1 1 d U . . Br4 Br 1.40930(13) 1.35701(8) 0.46102(6) 0.0873(4) Uani 1 1 d U . . Br1 Br 1.63927(10) 0.54344(7) 0.19951(6) 0.0744(3) Uani 1 1 d U . . N1 N 1.4018(6) 0.6530(4) 0.1076(3) 0.0512(15) Uani 1 1 d U . . C39 C 1.3482(9) 0.5236(6) 0.0780(5) 0.060(2) Uani 1 1 d U . . C56 C 1.1295(9) 1.2956(6) 0.2378(4) 0.0579(19) Uani 1 1 d U . . N2 N 1.4741(7) 0.7406(4) 0.1884(3) 0.0505(15) Uani 1 1 d U . . N4 N 1.2914(8) 1.2123(5) 0.3787(4) 0.0616(18) Uani 1 1 d U . . C46 C 1.1314(8) 1.3184(6) 0.3414(4) 0.0535(18) Uani 1 1 d U . . C6 C 1.5394(9) 0.7470(6) 0.2949(5) 0.0572(18) Uani 1 1 d U . . C1 C 1.5242(9) 0.7896(6) 0.2287(5) 0.0567(18) Uani 1 1 d U . . C26 C 1.3128(7) 0.6834(5) 0.1463(4) 0.0473(17) Uani 1 1 d U . . N3 N 1.1277(7) 1.3443(5) 0.3942(3) 0.0570(17) Uani 1 1 d U . . C34 C 1.2134(9) 0.8154(6) 0.2717(4) 0.060(2) Uani 1 1 d U . . H34 H 1.2812 0.8369 0.2860 0.072 Uiso 1 1 calc R . . C63 C 1.1075(9) 1.5043(6) 0.3704(4) 0.060(2) Uani 1 1 d U . . C57 C 1.2241(9) 1.2473(6) 0.3314(4) 0.0554(18) Uani 1 1 d U . . C48 C 0.9828(9) 1.4120(7) 0.2588(5) 0.066(2) Uani 1 1 d U . . H48A H 0.9447 1.4481 0.2861 0.079 Uiso 1 1 calc R . . C36 C 1.1365(8) 0.7352(6) 0.2039(4) 0.0570(19) Uani 1 1 d U . . C27 C 1.1755(8) 0.6861(6) 0.1562(4) 0.0572(19) Uani 1 1 d U . . C47 C 1.0713(9) 1.3491(6) 0.2804(4) 0.0583(19) Uani 1 1 d U . . C37 C 1.3559(8) 0.7335(5) 0.1906(4) 0.0482(17) Uani 1 1 d U . . C51 C 1.0965(10) 1.3062(7) 0.1744(5) 0.068(2) Uani 1 1 d U . . C10 C 1.5044(9) 0.6533(6) 0.3309(4) 0.060(2) Uani 1 1 d U . . H10A H 1.4752 0.6264 0.2987 0.072 Uiso 1 1 calc R . . C12 C 1.6202(10) 0.5981(6) 0.3577(5) 0.071(3) Uani 1 1 d U . . H12A H 1.6898 0.6002 0.3205 0.107 Uiso 1 1 calc R . . H12B H 1.5953 0.5370 0.3790 0.107 Uiso 1 1 calc R . . H12C H 1.6484 0.6225 0.3905 0.107 Uiso 1 1 calc R . . C17 C 1.3884(10) 1.1443(6) 0.3707(5) 0.0618(19) Uani 1 1 d U . . C20 C 1.5550(10) 1.2644(6) 0.3133(5) 0.069(2) Uani 1 1 d U . . H20A H 1.4827 1.3032 0.3256 0.082 Uiso 1 1 calc R . . C2 C 1.5571(11) 0.8775(7) 0.1949(6) 0.076(2) Uani 1 1 d U . . C55 C 1.2220(9) 1.2344(6) 0.2650(4) 0.0611(19) Uani 1 1 d U . . C38 C 1.3679(8) 0.6117(6) 0.0590(4) 0.0529(18) Uani 1 1 d U . . C3 C 1.6007(11) 0.9231(7) 0.2353(6) 0.081(3) Uani 1 1 d U . . H3A H 1.6191 0.9836 0.2159 0.098 Uiso 1 1 calc R . . C35 C 1.2369(8) 0.7666(5) 0.2259(4) 0.0526(18) Uani 1 1 d U . . C52 C 1.1678(10) 1.2477(7) 0.1373(5) 0.071(2) Uani 1 1 d U . . H52A H 1.1506 1.2501 0.0942 0.085 Uiso 1 1 calc R . . C58 C 1.0513(9) 1.4206(6) 0.4016(4) 0.0585(19) Uani 1 1 d U . . C16 C 1.5100(10) 1.1675(6) 0.3406(5) 0.0604(19) Uani 1 1 d U . . C65 C 1.2363(9) 1.5131(6) 0.3258(5) 0.070(3) Uani 1 1 d U . . H65A H 1.2969 1.4708 0.3483 0.105 Uiso 1 1 calc R . . H65B H 1.2668 1.5729 0.3167 0.105 Uiso 1 1 calc R . . H65C H 1.2284 1.5012 0.2837 0.105 Uiso 1 1 calc R . . C59 C 0.9271(9) 1.4133(6) 0.4394(4) 0.061(2) Uani 1 1 d U . . C54 C 1.2869(10) 1.1811(7) 0.2277(5) 0.068(2) Uani 1 1 d U . . H54A H 1.3495 1.1394 0.2447 0.082 Uiso 1 1 calc R . . C50 C 1.0054(10) 1.3724(7) 0.1526(5) 0.074(2) Uani 1 1 d U . . H50A H 0.9830 1.3828 0.1094 0.089 Uiso 1 1 calc R . . C19 C 1.4470(12) 0.9925(7) 0.3841(6) 0.079(2) Uani 1 1 d U . . H19A H 1.4243 0.9324 0.3987 0.094 Uiso 1 1 calc R . . C64 C 0.8692(10) 1.3224(7) 0.4705(5) 0.077(3) Uani 1 1 d U . . H64A H 0.7846 1.3284 0.4955 0.116 Uiso 1 1 calc R . . H64B H 0.9237 1.2854 0.5007 0.116 Uiso 1 1 calc R . . H64C H 0.8623 1.2952 0.4350 0.116 Uiso 1 1 calc R . . C32 C 0.9873(10) 0.8032(7) 0.2752(5) 0.068(2) Uani 1 1 d U . . H32A H 0.9025 0.8169 0.2921 0.081 Uiso 1 1 calc R . . C18 C 1.3550(11) 1.0555(7) 0.3961(5) 0.077(2) Uani 1 1 d U . . C49 C 0.9483(10) 1.4227(7) 0.1954(5) 0.072(2) Uani 1 1 d U . . H49A H 0.8846 1.4653 0.1811 0.086 Uiso 1 1 calc R . . C33 C 1.0829(9) 0.8326(6) 0.2971(5) 0.067(2) Uani 1 1 d U . . H33A H 1.0641 0.8648 0.3294 0.081 Uiso 1 1 calc R . . C28 C 1.0843(9) 0.6547(7) 0.1307(5) 0.069(2) Uani 1 1 d U . . H28A H 1.1073 0.6225 0.0987 0.083 Uiso 1 1 calc R . . C21 C 1.6649(11) 1.2790(7) 0.3448(6) 0.086(3) Uani 1 1 d U . . H21A H 1.6905 1.3405 0.3270 0.130 Uiso 1 1 calc R . . H21B H 1.7366 1.2404 0.3347 0.130 Uiso 1 1 calc R . . H21C H 1.6392 1.2656 0.3933 0.130 Uiso 1 1 calc R . . C53 C 1.2562(11) 1.1914(7) 0.1634(5) 0.075(2) Uani 1 1 d U . . H53A H 1.3014 1.1559 0.1373 0.090 Uiso 1 1 calc R . . C40 C 1.3202(10) 0.4862(7) 0.0289(5) 0.071(2) Uani 1 1 d U . . H40A H 1.3051 0.4250 0.0401 0.085 Uiso 1 1 calc R . . C31 C 1.0076(9) 0.7519(7) 0.2274(5) 0.066(2) Uani 1 1 d U . . C41 C 1.3147(11) 0.5379(8) -0.0349(6) 0.078(2) Uani 1 1 d U . . H41A H 1.2991 0.5122 -0.0682 0.094 Uiso 1 1 calc R . . C45 C 1.3561(10) 0.4658(6) 0.1484(5) 0.068(2) Uani 1 1 d U . . H45A H 1.3750 0.5021 0.1759 0.101 Uiso 1 1 calc R . . H45B H 1.4237 0.4211 0.1465 0.101 Uiso 1 1 calc R . . H45C H 1.2748 0.4369 0.1679 0.101 Uiso 1 1 calc R . . C14 C 1.5641(12) 1.0124(7) 0.3535(6) 0.080(2) Uani 1 1 d U . . C7 C 1.5410(12) 0.9230(8) 0.1240(6) 0.091(3) Uani 1 1 d U . . H7A H 1.5234 0.8770 0.1029 0.109 Uiso 1 1 calc R . . C60 C 0.8659(10) 1.4896(7) 0.4494(5) 0.072(2) Uani 1 1 d U . . H60A H 0.7845 1.4864 0.4762 0.086 Uiso 1 1 calc R . . C43 C 1.3618(10) 0.6674(7) -0.0042(5) 0.074(2) Uani 1 1 d U . . C5 C 1.5863(9) 0.7987(6) 0.3292(5) 0.067(2) Uani 1 1 d U . . H5A H 1.5968 0.7727 0.3744 0.080 Uiso 1 1 calc R . . C15 C 1.5999(11) 1.1024(7) 0.3295(5) 0.072(2) Uani 1 1 d U . . H15 H 1.6832 1.1178 0.3066 0.087 Uiso 1 1 calc R . . C30 C 0.9155(11) 0.7191(7) 0.2006(5) 0.079(3) Uani 1 1 d U . . H30A H 0.8280 0.7295 0.2148 0.095 Uiso 1 1 calc R . . C11 C 1.3969(10) 0.6475(8) 0.3899(5) 0.076(3) Uani 1 1 d U . . H11A H 1.3198 0.6756 0.3734 0.114 Uiso 1 1 calc R . . H11B H 1.4215 0.6775 0.4204 0.114 Uiso 1 1 calc R . . H11C H 1.3807 0.5856 0.4136 0.114 Uiso 1 1 calc R . . C61 C 0.9224(10) 1.5700(7) 0.4205(5) 0.070(2) Uani 1 1 d U . . H61A H 0.8780 1.6214 0.4275 0.084 Uiso 1 1 calc R . . C22 C 1.5880(11) 1.2908(8) 0.2374(5) 0.087(3) Uani 1 1 d U . . H22A H 1.6148 1.3521 0.2215 0.130 Uiso 1 1 calc R . . H22B H 1.5132 1.2845 0.2181 0.130 Uiso 1 1 calc R . . H22C H 1.6573 1.2527 0.2238 0.130 Uiso 1 1 calc R . . C4 C 1.6183(11) 0.8870(7) 0.2997(6) 0.076(2) Uani 1 1 d U . . C62 C 1.0388(10) 1.5783(7) 0.3825(5) 0.067(2) Uani 1 1 d U . . H62A H 1.0743 1.6349 0.3637 0.081 Uiso 1 1 calc R . . C29 C 0.9498(10) 0.6725(7) 0.1544(5) 0.075(2) Uani 1 1 d U . . H29A H 0.8856 0.6512 0.1374 0.091 Uiso 1 1 calc R . . C13 C 1.6676(12) 0.9415(7) 0.3398(7) 0.091(3) Uani 1 1 d U . . H13A H 1.7468 0.9709 0.3144 0.109 Uiso 1 1 calc R . . H13B H 1.6870 0.9023 0.3828 0.109 Uiso 1 1 calc R . . C23 C 1.2208(14) 1.0263(8) 0.4316(6) 0.098(3) Uani 1 1 d U . . H23A H 1.1765 1.0795 0.4420 0.117 Uiso 1 1 calc R . . C44 C 1.3821(13) 0.7652(8) -0.0236(6) 0.098(4) Uani 1 1 d U . . H44A H 1.4024 0.7819 0.0146 0.147 Uiso 1 1 calc R . . H44B H 1.3045 0.7966 -0.0371 0.147 Uiso 1 1 calc R . . H44C H 1.4524 0.7806 -0.0609 0.147 Uiso 1 1 calc R . . C42 C 1.3317(12) 0.6271(8) -0.0502(6) 0.087(3) Uani 1 1 d U . . H42A H 1.3227 0.6625 -0.0938 0.105 Uiso 1 1 calc R . . C8 C 1.4184(14) 0.9869(9) 0.1252(7) 0.116(4) Uani 1 1 d U . . H8A H 1.3445 0.9530 0.1514 0.174 Uiso 1 1 calc R . . H8B H 1.4025 1.0138 0.0794 0.174 Uiso 1 1 calc R . . H8C H 1.4331 1.0331 0.1454 0.174 Uiso 1 1 calc R . . C9 C 1.6633(15) 0.9704(10) 0.0829(8) 0.129(5) Uani 1 1 d U . . H9A H 1.7344 0.9278 0.0841 0.193 Uiso 1 1 calc R . . H9B H 1.6823 1.0165 0.1021 0.193 Uiso 1 1 calc R . . H9C H 1.6505 0.9967 0.0365 0.193 Uiso 1 1 calc R . . C25 C 1.2141(18) 0.9538(11) 0.5002(8) 0.144(5) Uani 1 1 d U . . H25A H 1.2592 0.9736 0.5299 0.216 Uiso 1 1 calc R . . H25B H 1.2539 0.8991 0.4928 0.216 Uiso 1 1 calc R . . H25C H 1.1251 0.9435 0.5207 0.216 Uiso 1 1 calc R . . C24 C 1.1423(18) 0.9991(11) 0.3868(9) 0.147(5) Uani 1 1 d U . . H24A H 1.1477 1.0443 0.3439 0.220 Uiso 1 1 calc R . . H24B H 1.0534 0.9927 0.4085 0.220 Uiso 1 1 calc R . . H24C H 1.1755 0.9430 0.3793 0.220 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 Br3 0.1029(9) 0.0768(8) 0.0677(7) -0.0031(5) -0.0029(6) -0.0069(6) Ni2 0.0896(10) 0.0578(7) 0.0533(7) -0.0212(5) -0.0072(6) -0.0035(6) Br2 0.0865(9) 0.1239(11) 0.0742(7) -0.0276(7) 0.0141(6) -0.0261(7) Ni1 0.0441(6) 0.0653(7) 0.0731(8) -0.0361(6) 0.0032(5) -0.0038(5) Br4 0.1010(9) 0.0961(9) 0.0770(7) -0.0447(6) -0.0049(6) -0.0197(7) Br1 0.0644(7) 0.0682(6) 0.1008(8) -0.0433(6) -0.0105(5) 0.0074(5) N1 0.047(3) 0.050(3) 0.057(3) -0.015(3) -0.004(3) -0.012(3) C39 0.051(4) 0.061(4) 0.071(4) -0.031(3) 0.001(3) -0.001(3) C56 0.058(4) 0.061(4) 0.061(4) -0.028(3) -0.008(3) -0.003(3) N2 0.050(3) 0.040(3) 0.061(3) -0.019(3) 0.000(3) -0.001(3) N4 0.074(4) 0.052(4) 0.061(4) -0.018(3) -0.010(3) -0.011(3) C46 0.056(4) 0.053(4) 0.055(4) -0.024(3) 0.001(3) -0.009(3) C6 0.054(4) 0.054(4) 0.073(4) -0.033(3) -0.012(3) 0.002(3) C1 0.056(4) 0.048(4) 0.071(4) -0.028(3) -0.007(3) 0.000(3) C26 0.038(3) 0.049(3) 0.051(3) -0.010(3) -0.001(3) -0.005(3) N3 0.059(4) 0.056(4) 0.055(3) -0.018(3) -0.001(3) -0.004(3) C34 0.054(4) 0.058(4) 0.066(4) -0.026(3) 0.005(3) 0.007(3) C63 0.064(4) 0.057(4) 0.063(4) -0.023(3) -0.009(3) 0.007(3) C57 0.068(4) 0.049(4) 0.055(4) -0.022(3) -0.007(3) -0.013(3) C48 0.056(4) 0.072(4) 0.068(4) -0.022(4) -0.004(4) 0.000(4) C36 0.046(4) 0.061(4) 0.061(4) -0.015(3) -0.002(3) -0.005(3) C27 0.048(4) 0.062(4) 0.060(4) -0.015(3) -0.004(3) -0.002(3) C47 0.059(4) 0.060(4) 0.059(4) -0.024(3) -0.004(3) -0.007(3) C37 0.041(3) 0.043(3) 0.060(4) -0.018(3) 0.000(3) -0.003(3) C51 0.066(4) 0.077(4) 0.065(4) -0.030(3) -0.006(3) 0.000(4) C10 0.059(4) 0.059(4) 0.062(4) -0.021(3) -0.001(4) -0.004(4) C12 0.071(6) 0.065(5) 0.077(5) -0.018(4) -0.013(4) -0.002(4) C17 0.080(4) 0.048(4) 0.069(4) -0.028(3) -0.021(4) -0.007(3) C20 0.074(5) 0.060(4) 0.074(5) -0.026(4) -0.006(4) 0.004(4) C2 0.082(4) 0.058(4) 0.091(4) -0.026(4) -0.015(4) -0.002(4) C55 0.066(4) 0.061(4) 0.061(4) -0.023(3) -0.009(3) -0.007(3) C38 0.041(3) 0.063(4) 0.055(4) -0.020(3) -0.002(3) -0.001(3) C3 0.085(5) 0.062(4) 0.106(5) -0.033(4) -0.022(4) -0.003(4) C35 0.048(4) 0.049(4) 0.057(4) -0.017(3) 0.004(3) 0.003(3) C52 0.073(5) 0.086(5) 0.062(4) -0.035(4) -0.009(4) 0.002(4) C58 0.062(4) 0.060(4) 0.055(4) -0.020(3) -0.008(3) -0.001(3) C16 0.075(4) 0.045(4) 0.068(4) -0.027(3) -0.015(3) 0.003(3) C65 0.074(5) 0.060(5) 0.077(5) -0.022(4) 0.003(4) -0.027(4) C59 0.068(4) 0.067(4) 0.049(4) -0.018(3) -0.009(3) -0.001(4) C54 0.079(5) 0.073(4) 0.068(4) -0.045(4) -0.012(4) 0.004(4) C50 0.073(5) 0.083(5) 0.069(4) -0.030(4) -0.009(4) 0.009(4) C19 0.100(5) 0.057(4) 0.092(5) -0.031(4) -0.034(4) 0.001(4) C64 0.072(6) 0.084(6) 0.072(5) -0.019(5) -0.001(4) -0.004(5) C32 0.055(4) 0.074(5) 0.071(4) -0.022(4) 0.001(4) 0.011(4) C18 0.094(5) 0.059(4) 0.087(4) -0.029(4) -0.019(4) -0.008(4) C49 0.064(4) 0.082(5) 0.071(4) -0.027(4) -0.011(4) 0.012(4) C33 0.061(4) 0.071(4) 0.069(4) -0.027(4) 0.002(4) 0.006(4) C28 0.053(4) 0.077(5) 0.075(4) -0.018(4) -0.012(4) 0.000(4) C21 0.089(6) 0.070(6) 0.108(6) -0.034(5) -0.020(5) -0.006(5) C53 0.082(5) 0.082(5) 0.072(4) -0.042(4) -0.008(4) 0.002(4) C40 0.068(5) 0.064(4) 0.085(5) -0.034(4) -0.001(4) -0.010(4) C31 0.052(4) 0.073(4) 0.069(4) -0.019(3) -0.001(3) 0.004(3) C41 0.079(5) 0.087(5) 0.079(5) -0.041(4) -0.008(4) -0.007(4) C45 0.074(5) 0.054(5) 0.072(5) -0.013(4) -0.006(4) -0.010(4) C14 0.093(5) 0.066(4) 0.096(5) -0.032(4) -0.040(4) 0.009(4) C7 0.100(6) 0.075(5) 0.095(5) -0.026(4) -0.002(5) -0.010(5) C60 0.074(5) 0.078(5) 0.061(4) -0.023(4) -0.006(4) 0.005(4) C43 0.069(5) 0.078(5) 0.076(4) -0.021(4) -0.015(4) -0.003(4) C5 0.069(4) 0.055(4) 0.084(5) -0.030(4) -0.021(4) 0.014(4) C15 0.081(5) 0.063(4) 0.084(5) -0.032(4) -0.025(4) 0.002(4) C30 0.060(5) 0.087(5) 0.086(5) -0.024(4) -0.001(4) -0.002(4) C11 0.070(6) 0.091(6) 0.071(5) -0.034(5) -0.003(4) -0.005(5) C61 0.079(5) 0.067(4) 0.072(4) -0.029(4) -0.021(4) 0.007(4) C22 0.087(6) 0.081(6) 0.085(6) -0.022(5) 0.001(5) 0.008(5) C4 0.077(4) 0.064(4) 0.102(5) -0.037(4) -0.036(4) 0.004(4) C62 0.080(5) 0.059(4) 0.069(4) -0.024(4) -0.017(4) 0.002(4) C29 0.059(4) 0.083(5) 0.088(5) -0.027(4) -0.013(4) -0.004(4) C13 0.097(5) 0.072(5) 0.117(5) -0.035(4) -0.042(5) 0.008(4) C23 0.119(6) 0.079(5) 0.099(5) -0.031(5) -0.010(5) -0.018(5) C44 0.104(7) 0.091(7) 0.095(6) -0.012(5) -0.029(6) -0.009(6) C42 0.091(5) 0.098(5) 0.076(5) -0.029(4) -0.013(4) -0.004(5) C8 0.125(8) 0.099(7) 0.117(7) -0.017(6) -0.030(6) 0.011(6) C9 0.128(8) 0.117(8) 0.133(8) -0.025(6) -0.003(7) -0.026(7) C25 0.162(9) 0.115(8) 0.141(8) -0.021(7) -0.004(7) -0.009(7) C24 0.151(9) 0.138(8) 0.156(9) -0.050(7) -0.013(7) -0.027(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 Br3 Ni2 2.3433(19) . ? Ni2 N3 2.022(8) . ? Ni2 N4 2.043(8) . ? Ni2 Br4 2.327(2) . ? Br2 Ni1 2.3273(18) . ? Ni1 N1 2.032(7) . ? Ni1 N2 2.036(7) . ? Ni1 Br1 2.3479(19) . ? N1 C26 1.304(10) . ? N1 C38 1.468(11) . ? C39 C38 1.361(12) . ? C39 C40 1.414(13) . ? C39 C45 1.523(13) . ? C56 C51 1.405(13) . ? C56 C55 1.412(13) . ? C56 C47 1.444(12) . ? N2 C37 1.268(10) . ? N2 C1 1.487(11) . ? N4 C57 1.305(11) . ? N4 C17 1.468(12) . ? C46 N3 1.288(10) . ? C46 C47 1.483(13) . ? C46 C57 1.485(12) . ? C6 C5 1.403(12) . ? C6 C1 1.403(12) . ? C6 C10 1.505(12) . ? C1 C2 1.413(13) . ? C26 C27 1.446(12) . ? C26 C37 1.530(11) . ? N3 C58 1.444(11) . ? C34 C35 1.384(12) . ? C34 C33 1.443(12) . ? C34 H34 0.9500 . ? C63 C62 1.403(12) . ? C63 C58 1.427(13) . ? C63 C65 1.520(13) . ? C57 C55 1.479(12) . ? C48 C47 1.363(13) . ? C48 C49 1.413(13) . ? C48 H48A 0.9500 . ? C36 C35 1.412(12) . ? C36 C31 1.416(12) . ? C36 C27 1.433(12) . ? C27 C28 1.373(13) . ? C37 C35 1.501(11) . ? C51 C50 1.414(14) . ? C51 C52 1.472(13) . ? C10 C11 1.530(12) . ? C10 C12 1.560(13) . ? C10 H10A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C17 C16 1.371(13) . ? C17 C18 1.406(13) . ? C20 C21 1.508(14) . ? C20 C22 1.523(14) . ? C20 C16 1.560(13) . ? C20 H20A 1.0000 . ? C2 C3 1.415(14) . ? C2 C7 1.502(16) . ? C55 C54 1.388(12) . ? C38 C43 1.387(13) . ? C3 C4 1.360(15) . ? C3 H3A 0.9500 . ? C52 C53 1.335(14) . ? C52 H52A 0.9500 . ? C58 C59 1.422(13) . ? C16 C15 1.403(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C59 C60 1.386(13) . ? C59 C64 1.530(14) . ? C54 C53 1.414(13) . ? C54 H54A 0.9500 . ? C50 C49 1.407(13) . ? C50 H50A 0.9500 . ? C19 C14 1.321(16) . ? C19 C18 1.396(15) . ? C19 H19A 0.9500 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C32 C33 1.352(14) . ? C32 C31 1.449(13) . ? C32 H32A 0.9500 . ? C18 C23 1.537(17) . ? C49 H49A 0.9500 . ? C33 H33A 0.9500 . ? C28 C29 1.474(14) . ? C28 H28A 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C53 H53A 0.9500 . ? C40 C41 1.375(14) . ? C40 H40A 0.9500 . ? C31 C30 1.410(15) . ? C41 C42 1.376(15) . ? C41 H41A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C14 C15 1.428(15) . ? C14 C13 1.573(15) . ? C7 C9 1.551(18) . ? C7 C8 1.601(17) . ? C7 H7A 1.0000 . ? C60 C61 1.381(14) . ? C60 H60A 0.9500 . ? C43 C42 1.396(15) . ? C43 C44 1.510(15) . ? C5 C4 1.402(14) . ? C5 H5A 0.9500 . ? C15 H15 0.9500 . ? C30 C29 1.373(14) . ? C30 H30A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C61 C62 1.353(14) . ? C61 H61A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C4 C13 1.542(14) . ? C62 H62A 0.9500 . ? C29 H29A 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C23 C24 1.53(2) . ? C23 C25 1.568(18) . ? C23 H23A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C42 H42A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni2 N4 82.9(3) . . ? N3 Ni2 Br4 110.6(2) . . ? N4 Ni2 Br4 113.1(2) . . ? N3 Ni2 Br3 107.3(2) . . ? N4 Ni2 Br3 108.6(2) . . ? Br4 Ni2 Br3 125.92(7) . . ? N1 Ni1 N2 83.9(3) . . ? N1 Ni1 Br2 113.1(2) . . ? N2 Ni1 Br2 115.8(2) . . ? N1 Ni1 Br1 106.9(2) . . ? N2 Ni1 Br1 103.7(2) . . ? Br2 Ni1 Br1 125.38(7) . . ? C26 N1 C38 120.0(7) . . ? C26 N1 Ni1 110.1(6) . . ? C38 N1 Ni1 129.9(5) . . ? C38 C39 C40 117.0(9) . . ? C38 C39 C45 122.9(8) . . ? C40 C39 C45 120.2(9) . . ? C51 C56 C55 124.1(9) . . ? C51 C56 C47 121.5(9) . . ? C55 C56 C47 114.3(8) . . ? C37 N2 C1 121.9(7) . . ? C37 N2 Ni1 110.5(6) . . ? C1 N2 Ni1 127.6(5) . . ? C57 N4 C17 120.1(8) . . ? C57 N4 Ni2 110.4(6) . . ? C17 N4 Ni2 129.4(6) . . ? N3 C46 C47 134.7(8) . . ? N3 C46 C57 118.0(8) . . ? C47 C46 C57 107.0(7) . . ? C5 C6 C1 115.7(8) . . ? C5 C6 C10 119.4(9) . . ? C1 C6 C10 124.8(8) . . ? C6 C1 C2 124.8(9) . . ? C6 C1 N2 119.8(7) . . ? C2 C1 N2 115.3(8) . . ? N1 C26 C27 135.0(8) . . ? N1 C26 C37 116.8(7) . . ? C27 C26 C37 108.1(7) . . ? C46 N3 C58 119.7(8) . . ? C46 N3 Ni2 111.3(6) . . ? C58 N3 Ni2 128.9(6) . . ? C35 C34 C33 118.1(9) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? C62 C63 C58 117.2(9) . . ? C62 C63 C65 121.3(9) . . ? C58 C63 C65 121.5(8) . . ? N4 C57 C55 133.6(9) . . ? N4 C57 C46 117.4(8) . . ? C55 C57 C46 109.0(8) . . ? C47 C48 C49 119.2(9) . . ? C47 C48 H48A 120.4 . . ? C49 C48 H48A 120.4 . . ? C35 C36 C31 121.9(9) . . ? C35 C36 C27 114.9(8) . . ? C31 C36 C27 123.2(9) . . ? C28 C27 C36 119.0(8) . . ? C28 C27 C26 135.2(9) . . ? C36 C27 C26 105.8(8) . . ? C48 C47 C56 119.7(9) . . ? C48 C47 C46 135.4(8) . . ? C56 C47 C46 105.0(8) . . ? N2 C37 C35 135.5(8) . . ? N2 C37 C26 118.3(7) . . ? C35 C37 C26 106.2(7) . . ? C56 C51 C50 118.0(9) . . ? C56 C51 C52 114.1(9) . . ? C50 C51 C52 127.8(9) . . ? C6 C10 C11 112.0(8) . . ? C6 C10 C12 111.5(8) . . ? C11 C10 C12 108.1(8) . . ? C6 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C12 C10 H10A 108.4 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C17 C18 121.0(9) . . ? C16 C17 N4 120.2(8) . . ? C18 C17 N4 118.8(9) . . ? C21 C20 C22 111.2(9) . . ? C21 C20 C16 111.5(8) . . ? C22 C20 C16 111.1(8) . . ? C21 C20 H20A 107.6 . . ? C22 C20 H20A 107.6 . . ? C16 C20 H20A 107.6 . . ? C1 C2 C3 113.9(10) . . ? C1 C2 C7 124.8(10) . . ? C3 C2 C7 121.2(10) . . ? C54 C55 C56 119.4(9) . . ? C54 C55 C57 135.8(9) . . ? C56 C55 C57 104.7(8) . . ? C39 C38 C43 125.3(9) . . ? C39 C38 N1 119.0(8) . . ? C43 C38 N1 115.7(8) . . ? C4 C3 C2 125.0(10) . . ? C4 C3 H3A 117.5 . . ? C2 C3 H3A 117.5 . . ? C34 C35 C36 121.2(8) . . ? C34 C35 C37 133.7(9) . . ? C36 C35 C37 105.0(7) . . ? C53 C52 C51 120.9(9) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C59 C58 C63 121.2(8) . . ? C59 C58 N3 122.0(8) . . ? C63 C58 N3 116.8(8) . . ? C17 C16 C15 119.7(9) . . ? C17 C16 C20 123.9(8) . . ? C15 C16 C20 116.3(9) . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C60 C59 C58 117.9(9) . . ? C60 C59 C64 122.6(9) . . ? C58 C59 C64 119.4(9) . . ? C55 C54 C53 117.4(10) . . ? C55 C54 H54A 121.3 . . ? C53 C54 H54A 121.3 . . ? C49 C50 C51 119.4(10) . . ? C49 C50 H50A 120.3 . . ? C51 C50 H50A 120.3 . . ? C14 C19 C18 123.3(11) . . ? C14 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C33 C32 C31 123.4(9) . . ? C33 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? C19 C18 C17 117.4(11) . . ? C19 C18 C23 119.6(10) . . ? C17 C18 C23 122.8(10) . . ? C50 C49 C48 122.1(10) . . ? C50 C49 H49A 118.9 . . ? C48 C49 H49A 118.9 . . ? C32 C33 C34 120.3(9) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C27 C28 C29 118.2(10) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C52 C53 C54 124.0(10) . . ? C52 C53 H53A 118.0 . . ? C54 C53 H53A 118.0 . . ? C41 C40 C39 120.4(10) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C30 C31 C36 116.9(9) . . ? C30 C31 C32 128.1(9) . . ? C36 C31 C32 115.0(9) . . ? C40 C41 C42 119.7(10) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C19 C14 C15 119.5(11) . . ? C19 C14 C13 123.3(11) . . ? C15 C14 C13 117.2(11) . . ? C2 C7 C9 111.9(12) . . ? C2 C7 C8 108.3(10) . . ? C9 C7 C8 113.6(11) . . ? C2 C7 H7A 107.6 . . ? C9 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C61 C60 C59 120.4(10) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C38 C43 C42 115.2(10) . . ? C38 C43 C44 124.1(10) . . ? C42 C43 C44 120.7(10) . . ? C4 C5 C6 122.9(10) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C16 C15 C14 118.8(11) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C29 C30 C31 121.3(10) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C62 C61 C60 122.3(10) . . ? C62 C61 H61A 118.8 . . ? C60 C61 H61A 118.8 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C4 C5 117.5(10) . . ? C3 C4 C13 121.5(10) . . ? C5 C4 C13 121.0(10) . . ? C61 C62 C63 120.8(10) . . ? C61 C62 H62A 119.6 . . ? C63 C62 H62A 119.6 . . ? C30 C29 C28 121.4(10) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C4 C13 C14 109.6(9) . . ? C4 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C4 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C24 C23 C18 113.0(12) . . ? C24 C23 C25 109.9(12) . . ? C18 C23 C25 115.5(12) . . ? C24 C23 H23A 105.9 . . ? C18 C23 H23A 105.9 . . ? C25 C23 H23A 105.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C42 C43 122.5(11) . . ? C41 C42 H42A 118.8 . . ? C43 C42 H42A 118.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 N2 Ni1 N1 C26 -5.3(5) . . . . ? Br2 Ni1 N1 C26 -120.8(5) . . . . ? Br1 Ni1 N1 C26 97.2(5) . . . . ? N2 Ni1 N1 C38 174.0(7) . . . . ? Br2 Ni1 N1 C38 58.5(7) . . . . ? Br1 Ni1 N1 C38 -83.5(7) . . . . ? N1 Ni1 N2 C37 4.5(6) . . . . ? Br2 Ni1 N2 C37 117.2(5) . . . . ? Br1 Ni1 N2 C37 -101.5(6) . . . . ? N1 Ni1 N2 C1 -177.4(7) . . . . ? Br2 Ni1 N2 C1 -64.6(7) . . . . ? Br1 Ni1 N2 C1 76.7(6) . . . . ? N3 Ni2 N4 C57 -0.9(6) . . . . ? Br4 Ni2 N4 C57 -110.2(6) . . . . ? Br3 Ni2 N4 C57 105.1(6) . . . . ? N3 Ni2 N4 C17 175.2(8) . . . . ? Br4 Ni2 N4 C17 65.8(8) . . . . ? Br3 Ni2 N4 C17 -78.9(8) . . . . ? C5 C6 C1 C2 2.6(14) . . . . ? C10 C6 C1 C2 -180.0(9) . . . . ? C5 C6 C1 N2 -179.5(8) . . . . ? C10 C6 C1 N2 -2.1(13) . . . . ? C37 N2 C1 C6 85.4(10) . . . . ? Ni1 N2 C1 C6 -92.6(9) . . . . ? C37 N2 C1 C2 -96.5(10) . . . . ? Ni1 N2 C1 C2 85.5(9) . . . . ? C38 N1 C26 C27 1.8(14) . . . . ? Ni1 N1 C26 C27 -178.9(8) . . . . ? C38 N1 C26 C37 -174.2(7) . . . . ? Ni1 N1 C26 C37 5.2(8) . . . . ? C47 C46 N3 C58 -0.3(15) . . . . ? C57 C46 N3 C58 171.9(8) . . . . ? C47 C46 N3 Ni2 -176.4(8) . . . . ? C57 C46 N3 Ni2 -4.1(10) . . . . ? N4 Ni2 N3 C46 2.8(6) . . . . ? Br4 Ni2 N3 C46 114.8(6) . . . . ? Br3 Ni2 N3 C46 -104.5(6) . . . . ? N4 Ni2 N3 C58 -172.8(8) . . . . ? Br4 Ni2 N3 C58 -60.8(7) . . . . ? Br3 Ni2 N3 C58 79.9(7) . . . . ? C17 N4 C57 C55 -0.6(15) . . . . ? Ni2 N4 C57 C55 175.9(9) . . . . ? C17 N4 C57 C46 -177.5(8) . . . . ? Ni2 N4 C57 C46 -1.0(10) . . . . ? N3 C46 C57 N4 3.6(12) . . . . ? C47 C46 C57 N4 177.9(8) . . . . ? N3 C46 C57 C55 -174.0(8) . . . . ? C47 C46 C57 C55 0.3(10) . . . . ? C35 C36 C27 C28 -178.4(8) . . . . ? C31 C36 C27 C28 1.4(14) . . . . ? C35 C36 C27 C26 0.8(10) . . . . ? C31 C36 C27 C26 -179.4(8) . . . . ? N1 C26 C27 C28 3.0(18) . . . . ? C37 C26 C27 C28 179.2(10) . . . . ? N1 C26 C27 C36 -176.0(9) . . . . ? C37 C26 C27 C36 0.2(9) . . . . ? C49 C48 C47 C56 0.9(14) . . . . ? C49 C48 C47 C46 179.8(10) . . . . ? C51 C56 C47 C48 -0.4(14) . . . . ? C55 C56 C47 C48 178.4(9) . . . . ? C51 C56 C47 C46 -179.7(9) . . . . ? C55 C56 C47 C46 -0.8(11) . . . . ? N3 C46 C47 C48 -5.9(19) . . . . ? C57 C46 C47 C48 -178.8(10) . . . . ? N3 C46 C47 C56 173.2(10) . . . . ? C57 C46 C47 C56 0.3(9) . . . . ? C1 N2 C37 C35 1.9(14) . . . . ? Ni1 N2 C37 C35 -179.8(8) . . . . ? C1 N2 C37 C26 178.7(7) . . . . ? Ni1 N2 C37 C26 -2.9(9) . . . . ? N1 C26 C37 N2 -1.6(11) . . . . ? C27 C26 C37 N2 -178.6(7) . . . . ? N1 C26 C37 C35 176.1(7) . . . . ? C27 C26 C37 C35 -0.9(9) . . . . ? C55 C56 C51 C50 -177.7(10) . . . . ? C47 C56 C51 C50 1.1(15) . . . . ? C55 C56 C51 C52 -0.3(14) . . . . ? C47 C56 C51 C52 178.4(9) . . . . ? C5 C6 C10 C11 62.0(12) . . . . ? C1 C6 C10 C11 -115.3(10) . . . . ? C5 C6 C10 C12 -59.3(11) . . . . ? C1 C6 C10 C12 123.3(10) . . . . ? C57 N4 C17 C16 88.2(11) . . . . ? Ni2 N4 C17 C16 -87.5(10) . . . . ? C57 N4 C17 C18 -93.4(11) . . . . ? Ni2 N4 C17 C18 90.9(10) . . . . ? C6 C1 C2 C3 -3.9(15) . . . . ? N2 C1 C2 C3 178.1(9) . . . . ? C6 C1 C2 C7 179.9(10) . . . . ? N2 C1 C2 C7 2.0(15) . . . . ? C51 C56 C55 C54 0.7(15) . . . . ? C47 C56 C55 C54 -178.2(9) . . . . ? C51 C56 C55 C57 179.8(9) . . . . ? C47 C56 C55 C57 1.0(11) . . . . ? N4 C57 C55 C54 1.1(19) . . . . ? C46 C57 C55 C54 178.2(11) . . . . ? N4 C57 C55 C56 -177.8(10) . . . . ? C46 C57 C55 C56 -0.7(10) . . . . ? C40 C39 C38 C43 0.5(14) . . . . ? C45 C39 C38 C43 -179.9(9) . . . . ? C40 C39 C38 N1 -177.9(8) . . . . ? C45 C39 C38 N1 1.7(13) . . . . ? C26 N1 C38 C39 -89.8(10) . . . . ? Ni1 N1 C38 C39 91.0(9) . . . . ? C26 N1 C38 C43 91.7(10) . . . . ? Ni1 N1 C38 C43 -87.5(9) . . . . ? C1 C2 C3 C4 3.9(17) . . . . ? C7 C2 C3 C4 -179.8(11) . . . . ? C33 C34 C35 C36 0.7(13) . . . . ? C33 C34 C35 C37 -177.8(9) . . . . ? C31 C36 C35 C34 -0.1(14) . . . . ? C27 C36 C35 C34 179.7(8) . . . . ? C31 C36 C35 C37 178.8(8) . . . . ? C27 C36 C35 C37 -1.3(10) . . . . ? N2 C37 C35 C34 -2.9(17) . . . . ? C26 C37 C35 C34 -179.9(9) . . . . ? N2 C37 C35 C36 178.4(9) . . . . ? C26 C37 C35 C36 1.3(9) . . . . ? C56 C51 C52 C53 -0.8(15) . . . . ? C50 C51 C52 C53 176.3(11) . . . . ? C62 C63 C58 C59 4.1(13) . . . . ? C65 C63 C58 C59 -175.6(9) . . . . ? C62 C63 C58 N3 -174.3(8) . . . . ? C65 C63 C58 N3 6.0(13) . . . . ? C46 N3 C58 C59 97.5(10) . . . . ? Ni2 N3 C58 C59 -87.2(10) . . . . ? C46 N3 C58 C63 -84.1(11) . . . . ? Ni2 N3 C58 C63 91.2(9) . . . . ? C18 C17 C16 C15 5.6(14) . . . . ? N4 C17 C16 C15 -176.1(8) . . . . ? C18 C17 C16 C20 -178.0(9) . . . . ? N4 C17 C16 C20 0.3(14) . . . . ? C21 C20 C16 C17 122.7(11) . . . . ? C22 C20 C16 C17 -112.7(11) . . . . ? C21 C20 C16 C15 -60.8(12) . . . . ? C22 C20 C16 C15 63.8(12) . . . . ? C63 C58 C59 C60 -4.7(14) . . . . ? N3 C58 C59 C60 173.6(8) . . . . ? C63 C58 C59 C64 178.5(9) . . . . ? N3 C58 C59 C64 -3.2(13) . . . . ? C56 C55 C54 C53 0.0(15) . . . . ? C57 C55 C54 C53 -178.7(10) . . . . ? C56 C51 C50 C49 -2.2(16) . . . . ? C52 C51 C50 C49 -179.1(10) . . . . ? C14 C19 C18 C17 3.5(17) . . . . ? C14 C19 C18 C23 179.5(11) . . . . ? C16 C17 C18 C19 -5.5(15) . . . . ? N4 C17 C18 C19 176.1(9) . . . . ? C16 C17 C18 C23 178.6(10) . . . . ? N4 C17 C18 C23 0.3(15) . . . . ? C51 C50 C49 C48 2.7(17) . . . . ? C47 C48 C49 C50 -2.0(16) . . . . ? C31 C32 C33 C34 1.6(15) . . . . ? C35 C34 C33 C32 -1.5(14) . . . . ? C36 C27 C28 C29 -0.7(13) . . . . ? C26 C27 C28 C29 -179.6(10) . . . . ? C51 C52 C53 C54 1.6(17) . . . . ? C55 C54 C53 C52 -1.2(17) . . . . ? C38 C39 C40 C41 0.5(14) . . . . ? C45 C39 C40 C41 -179.1(9) . . . . ? C35 C36 C31 C30 178.5(9) . . . . ? C27 C36 C31 C30 -1.3(14) . . . . ? C35 C36 C31 C32 0.1(13) . . . . ? C27 C36 C31 C32 -179.7(8) . . . . ? C33 C32 C31 C30 -179.0(10) . . . . ? C33 C32 C31 C36 -0.9(14) . . . . ? C39 C40 C41 C42 -2.5(16) . . . . ? C18 C19 C14 C15 -1.5(17) . . . . ? C18 C19 C14 C13 -179.8(10) . . . . ? C1 C2 C7 C9 -131.1(12) . . . . ? C3 C2 C7 C9 52.9(16) . . . . ? C1 C2 C7 C8 102.9(13) . . . . ? C3 C2 C7 C8 -73.0(14) . . . . ? C58 C59 C60 C61 3.0(14) . . . . ? C64 C59 C60 C61 179.7(9) . . . . ? C39 C38 C43 C42 0.5(15) . . . . ? N1 C38 C43 C42 178.9(9) . . . . ? C39 C38 C43 C44 179.0(10) . . . . ? N1 C38 C43 C44 -2.6(15) . . . . ? C1 C6 C5 C4 -1.0(14) . . . . ? C10 C6 C5 C4 -178.5(9) . . . . ? C17 C16 C15 C14 -3.4(14) . . . . ? C20 C16 C15 C14 179.9(9) . . . . ? C19 C14 C15 C16 1.4(16) . . . . ? C13 C14 C15 C16 179.8(9) . . . . ? C36 C31 C30 C29 0.7(15) . . . . ? C32 C31 C30 C29 178.8(10) . . . . ? C59 C60 C61 C62 -0.8(16) . . . . ? C2 C3 C4 C5 -2.5(18) . . . . ? C2 C3 C4 C13 179.3(11) . . . . ? C6 C5 C4 C3 1.0(16) . . . . ? C6 C5 C4 C13 179.1(10) . . . . ? C60 C61 C62 C63 0.3(16) . . . . ? C58 C63 C62 C61 -1.9(14) . . . . ? C65 C63 C62 C61 177.8(9) . . . . ? C31 C30 C29 C28 -0.1(16) . . . . ? C27 C28 C29 C30 0.1(15) . . . . ? C3 C4 C13 C14 68.2(15) . . . . ? C5 C4 C13 C14 -109.9(12) . . . . ? C19 C14 C13 C4 56.5(15) . . . . ? C15 C14 C13 C4 -121.8(11) . . . . ? C19 C18 C23 C24 -74.3(16) . . . . ? C17 C18 C23 C24 101.4(14) . . . . ? C19 C18 C23 C25 53.4(16) . . . . ? C17 C18 C23 C25 -130.8(12) . . . . ? C40 C41 C42 C43 3.7(18) . . . . ? C38 C43 C42 C41 -2.6(17) . . . . ? C44 C43 C42 C41 178.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.002 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.001 0.000 529.2 149.8 2 0.479 0.857 0.509 7.2 1.3 3 0.521 0.143 0.491 7.2 0.7 _platon_squeeze_details ; ? ; data_Ni2-3 _database_code_depnum_ccdc_archive 'CCDC 917317' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H80 Br4 N4 Ni2' _chemical_formula_weight 1450.47 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' _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 20.688(4) _cell_length_b 19.271(4) _cell_length_c 21.750(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.01(3) _cell_angle_gamma 90.00 _cell_volume 8039(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.0095 _cell_measurement_theta_max 27.4855 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2600 _exptl_crystal_size_min 0.2200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 2.493 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6983 _exptl_absorpt_correction_T_max 1.6100 _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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18894 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14117 _reflns_number_gt 9049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+7.5712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14117 _refine_ls_number_parameters 764 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2525 _refine_ls_wR_factor_gt 0.2258 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Br4 Br 0.27148(5) 0.26650(5) 0.82760(5) 0.0590(3) Uani 1 1 d . . . Br3 Br 0.30188(7) 0.45284(9) 0.91111(6) 0.0993(5) Uani 1 1 d . . . Br1 Br 0.68941(5) 0.51171(5) 0.63686(5) 0.0569(3) Uani 1 1 d . . . Br2 Br 0.67079(5) 0.30112(6) 0.63180(5) 0.0667(3) Uani 1 1 d . . . Ni2 Ni 0.30929(5) 0.38072(6) 0.82982(5) 0.0374(3) Uani 1 1 d . . . Ni1 Ni 0.73603(5) 0.40157(6) 0.66985(5) 0.0431(3) Uani 1 1 d . . . N3 N 0.2759(3) 0.4067(3) 0.7326(3) 0.0271(13) Uani 1 1 d . . . N4 N 0.4044(3) 0.3923(3) 0.8235(3) 0.0297(14) Uani 1 1 d . . . N1 N 0.8319(3) 0.3937(3) 0.6661(3) 0.0328(15) Uani 1 1 d . . . N2 N 0.7916(3) 0.3943(3) 0.7689(3) 0.0334(15) Uani 1 1 d . . . C17 C 0.4754(4) 0.3916(4) 0.8737(3) 0.0321(18) Uani 1 1 d . . . C16 C 0.5074(4) 0.4562(4) 0.8937(4) 0.0322(17) Uani 1 1 d . . . C15 C 0.5787(4) 0.4541(4) 0.9328(3) 0.0285(16) Uani 1 1 d . . . H15 H 0.6030 0.4966 0.9473 0.034 Uiso 1 1 calc R . . C14 C 0.6150(4) 0.3927(4) 0.9509(3) 0.0291(17) Uani 1 1 d . . . C19 C 0.5796(3) 0.3309(4) 0.9337(3) 0.0287(16) Uani 1 1 d . . . H19 H 0.6043 0.2888 0.9490 0.034 Uiso 1 1 calc R . . C18 C 0.5067(3) 0.3280(4) 0.8936(4) 0.0319(17) Uani 1 1 d . . . C20 C 0.4692(4) 0.5261(4) 0.8744(4) 0.046(2) Uani 1 1 d . . . H20 H 0.4183 0.5162 0.8523 0.055 Uiso 1 1 calc R . . C21 C 0.4795(7) 0.5720(6) 0.9348(5) 0.085(4) Uani 1 1 d . . . H21A H 0.4547 0.5516 0.9610 0.128 Uiso 1 1 calc R . . H21B H 0.4610 0.6185 0.9200 0.128 Uiso 1 1 calc R . . H21C H 0.5293 0.5752 0.9622 0.128 Uiso 1 1 calc R . . C22 C 0.4915(7) 0.5665(5) 0.8258(5) 0.083(4) Uani 1 1 d . . . H22A H 0.5420 0.5743 0.8451 0.124 Uiso 1 1 calc R . . H22B H 0.4673 0.6113 0.8165 0.124 Uiso 1 1 calc R . . H22C H 0.4795 0.5401 0.7845 0.124 Uiso 1 1 calc R . . C23 C 0.4696(4) 0.2602(4) 0.8698(4) 0.0377(19) Uani 1 1 d . . . H23 H 0.4184 0.2694 0.8544 0.045 Uiso 1 1 calc R . . C25 C 0.4876(5) 0.2051(5) 0.9243(5) 0.057(2) Uani 1 1 d . . . H25A H 0.5367 0.1919 0.9375 0.086 Uiso 1 1 calc R . . H25B H 0.4580 0.1642 0.9075 0.086 Uiso 1 1 calc R . . H25C H 0.4796 0.2239 0.9627 0.086 Uiso 1 1 calc R . . C24 C 0.4846(5) 0.2319(5) 0.8102(5) 0.058(3) Uani 1 1 d . . . H24A H 0.4730 0.2673 0.7755 0.087 Uiso 1 1 calc R . . H24B H 0.4562 0.1904 0.7928 0.087 Uiso 1 1 calc R . . H24C H 0.5341 0.2198 0.8245 0.087 Uiso 1 1 calc R . . C13 C 0.6937(4) 0.3932(5) 0.9834(4) 0.040(2) Uani 1 1 d . . . H13A H 0.7102 0.3513 1.0111 0.048 Uiso 1 1 calc R . . H13B H 0.7096 0.4346 1.0121 0.048 Uiso 1 1 calc R . . C4 C 0.7229(4) 0.3946(4) 0.9286(4) 0.0302(17) Uani 1 1 d . . . C3 C 0.7399(4) 0.4556(4) 0.9060(4) 0.0365(18) Uani 1 1 d . . . H3 H 0.7362 0.4979 0.9269 0.044 Uiso 1 1 calc R . . C2 C 0.7626(4) 0.4575(4) 0.8526(4) 0.0357(18) Uani 1 1 d . . . C1 C 0.7673(4) 0.3950(4) 0.8241(3) 0.0315(17) Uani 1 1 d . . . C6 C 0.7497(4) 0.3311(4) 0.8444(4) 0.0367(18) Uani 1 1 d . . . C5 C 0.7280(4) 0.3332(4) 0.8971(3) 0.0327(18) Uani 1 1 d . . . H5 H 0.7160 0.2909 0.9126 0.039 Uiso 1 1 calc R . . C7 C 0.7793(5) 0.5276(4) 0.8296(5) 0.051(2) Uani 1 1 d . . . H7 H 0.7908 0.5193 0.7895 0.061 Uiso 1 1 calc R . . C8 C 0.8445(6) 0.5604(6) 0.8839(7) 0.089(4) Uani 1 1 d . . . H8A H 0.8333 0.5730 0.9224 0.134 Uiso 1 1 calc R . . H8B H 0.8584 0.6021 0.8661 0.134 Uiso 1 1 calc R . . H8C H 0.8829 0.5269 0.8973 0.134 Uiso 1 1 calc R . . C9 C 0.7188(6) 0.5797(5) 0.8104(5) 0.067(3) Uani 1 1 d . . . H9A H 0.6772 0.5589 0.7770 0.100 Uiso 1 1 calc R . . H9B H 0.7316 0.6217 0.7923 0.100 Uiso 1 1 calc R . . H9C H 0.7088 0.5917 0.8498 0.100 Uiso 1 1 calc R . . C10 C 0.7552(5) 0.2605(4) 0.8138(5) 0.048(2) Uani 1 1 d . . . H10 H 0.7708 0.2685 0.7760 0.058 Uiso 1 1 calc R . . C11 C 0.8081(5) 0.2128(5) 0.8642(5) 0.066(3) Uani 1 1 d . . . H11A H 0.8549 0.2328 0.8772 0.100 Uiso 1 1 calc R . . H11B H 0.8073 0.1671 0.8442 0.100 Uiso 1 1 calc R . . H11C H 0.7960 0.2080 0.9035 0.100 Uiso 1 1 calc R . . C12 C 0.6823(5) 0.2256(6) 0.7865(5) 0.061(3) Uani 1 1 d . . . H12A H 0.6656 0.2191 0.8227 0.091 Uiso 1 1 calc R . . H12B H 0.6856 0.1805 0.7672 0.091 Uiso 1 1 calc R . . H12C H 0.6495 0.2553 0.7523 0.091 Uiso 1 1 calc R . . C50 C 0.3265(3) 0.4163(4) 0.7131(3) 0.0314(17) Uani 1 1 d . . . C51 C 0.3348(4) 0.4398(4) 0.6522(3) 0.0316(17) Uani 1 1 d . . . C52 C 0.2918(4) 0.4637(5) 0.5923(4) 0.043(2) Uani 1 1 d . . . H52 H 0.2430 0.4661 0.5821 0.052 Uiso 1 1 calc R . . C53 C 0.3199(5) 0.4853(5) 0.5446(4) 0.052(2) Uani 1 1 d . . . H53 H 0.2896 0.5036 0.5033 0.063 Uiso 1 1 calc R . . C54 C 0.3896(5) 0.4802(5) 0.5573(4) 0.054(2) Uani 1 1 d . . . H54 H 0.4066 0.4930 0.5240 0.065 Uiso 1 1 calc R . . C55 C 0.4374(4) 0.4560(4) 0.6201(4) 0.0389(19) Uani 1 1 d . . . C56 C 0.5107(4) 0.4508(5) 0.6415(4) 0.050(2) Uani 1 1 d . . . H56 H 0.5331 0.4633 0.6122 0.060 Uiso 1 1 calc R . . C57 C 0.5486(4) 0.4287(5) 0.7023(4) 0.047(2) Uani 1 1 d . . . H57 H 0.5975 0.4245 0.7144 0.056 Uiso 1 1 calc R . . C58 C 0.5200(4) 0.4112(4) 0.7494(4) 0.043(2) Uani 1 1 d . . . H58 H 0.5491 0.3968 0.7927 0.051 Uiso 1 1 calc R . . C59 C 0.4493(3) 0.4155(4) 0.7313(3) 0.0266(16) Uani 1 1 d . . . C60 C 0.4088(4) 0.4374(4) 0.6666(3) 0.0311(17) Uani 1 1 d . . . C61 C 0.3989(4) 0.4045(4) 0.7644(4) 0.0311(17) Uani 1 1 d . . . C62 C 0.2061(4) 0.4176(4) 0.6858(4) 0.0342(18) Uani 1 1 d . . . C67 C 0.1702(4) 0.3644(5) 0.6413(4) 0.043(2) Uani 1 1 d . . . C66 C 0.1028(5) 0.3791(7) 0.5977(4) 0.067(3) Uani 1 1 d . . . H66 H 0.0779 0.3452 0.5659 0.081 Uiso 1 1 calc R . . C65 C 0.0713(5) 0.4413(8) 0.5993(5) 0.073(4) Uani 1 1 d . . . H65 H 0.0249 0.4494 0.5693 0.087 Uiso 1 1 calc R . . C64 C 0.1052(5) 0.4908(6) 0.6428(5) 0.061(3) Uani 1 1 d . . . H64 H 0.0827 0.5339 0.6423 0.073 Uiso 1 1 calc R . . C63 C 0.1735(4) 0.4805(5) 0.6892(4) 0.040(2) Uani 1 1 d . . . C71 C 0.2036(5) 0.2945(5) 0.6415(4) 0.057(3) Uani 1 1 d . . . H71 H 0.2461 0.2916 0.6831 0.068 Uiso 1 1 calc R . . C72 C 0.2279(7) 0.2878(6) 0.5817(6) 0.093(4) Uani 1 1 d . . . H72A H 0.1874 0.2908 0.5400 0.139 Uiso 1 1 calc R . . H72B H 0.2511 0.2430 0.5841 0.139 Uiso 1 1 calc R . . H72C H 0.2606 0.3253 0.5837 0.139 Uiso 1 1 calc R . . C73 C 0.1560(6) 0.2347(6) 0.6425(5) 0.077(3) Uani 1 1 d . . . H73A H 0.1407 0.2407 0.6797 0.116 Uiso 1 1 calc R . . H73B H 0.1814 0.1908 0.6476 0.116 Uiso 1 1 calc R . . H73C H 0.1152 0.2340 0.6008 0.116 Uiso 1 1 calc R . . C68 C 0.2117(5) 0.5354(5) 0.7396(5) 0.059(3) Uani 1 1 d . . . H68 H 0.2467 0.5101 0.7777 0.071 Uiso 1 1 calc R . . C70 C 0.1641(7) 0.5741(9) 0.7681(8) 0.143(7) Uani 1 1 d . . . H70A H 0.1321 0.6043 0.7339 0.214 Uiso 1 1 calc R . . H70B H 0.1926 0.6023 0.8061 0.214 Uiso 1 1 calc R . . H70C H 0.1371 0.5404 0.7824 0.214 Uiso 1 1 calc R . . C69 C 0.2539(8) 0.5831(6) 0.7115(7) 0.110(5) Uani 1 1 d . . . H69A H 0.2802 0.5547 0.6917 0.165 Uiso 1 1 calc R . . H69B H 0.2862 0.6112 0.7474 0.165 Uiso 1 1 calc R . . H69C H 0.2220 0.6136 0.6777 0.165 Uiso 1 1 calc R . . C26 C 0.8800(4) 0.3837(4) 0.7230(4) 0.0333(18) Uani 1 1 d . . . C27 C 0.9556(4) 0.3717(4) 0.7490(4) 0.0344(18) Uani 1 1 d . . . C28 C 1.0057(4) 0.3672(4) 0.7229(4) 0.042(2) Uani 1 1 d . . . H28 H 0.9937 0.3721 0.6765 0.050 Uiso 1 1 calc R . . C29 C 1.0757(4) 0.3554(5) 0.7651(4) 0.046(2) Uani 1 1 d . . . H29 H 1.1107 0.3528 0.7468 0.056 Uiso 1 1 calc R . . C30 C 1.0939(4) 0.3476(5) 0.8324(5) 0.050(2) Uani 1 1 d . . . H30 H 1.1414 0.3392 0.8595 0.060 Uiso 1 1 calc R . . C31 C 1.0437(4) 0.3519(4) 0.8629(4) 0.041(2) Uani 1 1 d . . . C32 C 1.0547(4) 0.3455(5) 0.9303(4) 0.049(2) Uani 1 1 d . . . H32 H 1.1004 0.3362 0.9614 0.059 Uiso 1 1 calc R . . C33 C 1.0009(4) 0.3523(5) 0.9525(5) 0.056(3) Uani 1 1 d . . . H33 H 1.0100 0.3483 0.9986 0.067 Uiso 1 1 calc R . . C34 C 0.9319(4) 0.3653(4) 0.9073(4) 0.0390(19) Uani 1 1 d . . . H34 H 0.8951 0.3702 0.9231 0.047 Uiso 1 1 calc R . . C35 C 0.9185(4) 0.3710(4) 0.8409(4) 0.0369(19) Uani 1 1 d . . . C36 C 0.9759(4) 0.3643(4) 0.8192(4) 0.0370(19) Uani 1 1 d . . . C37 C 0.8569(4) 0.3838(4) 0.7811(4) 0.0363(18) Uani 1 1 d . . . C38 C 0.8478(4) 0.3977(4) 0.6054(4) 0.0348(18) Uani 1 1 d . . . C39 C 0.8625(3) 0.4626(4) 0.5866(4) 0.0300(17) Uani 1 1 d . . . C40 C 0.8749(4) 0.4655(5) 0.5282(4) 0.042(2) Uani 1 1 d . . . H40 H 0.8860 0.5089 0.5139 0.050 Uiso 1 1 calc R . . C41 C 0.8715(5) 0.4078(4) 0.4907(4) 0.046(2) Uani 1 1 d . . . H41 H 0.8806 0.4116 0.4511 0.055 Uiso 1 1 calc R . . C42 C 0.8550(5) 0.3437(5) 0.5097(4) 0.048(2) Uani 1 1 d . . . H42 H 0.8519 0.3042 0.4827 0.058 Uiso 1 1 calc R . . C43 C 0.8430(4) 0.3368(4) 0.5684(4) 0.040(2) Uani 1 1 d . . . C44 C 0.8679(4) 0.5282(5) 0.6271(4) 0.046(2) Uani 1 1 d . . . H44 H 0.8422 0.5199 0.6573 0.055 Uiso 1 1 calc R . . C46 C 0.9425(5) 0.5452(5) 0.6697(5) 0.063(3) Uani 1 1 d . . . H46A H 0.9644 0.5047 0.6968 0.095 Uiso 1 1 calc R . . H46B H 0.9436 0.5845 0.6986 0.095 Uiso 1 1 calc R . . H46C H 0.9680 0.5573 0.6412 0.095 Uiso 1 1 calc R . . C45 C 0.8337(5) 0.5925(5) 0.5824(5) 0.062(3) Uani 1 1 d . . . H45A H 0.8559 0.5999 0.5503 0.093 Uiso 1 1 calc R . . H45B H 0.8399 0.6338 0.6103 0.093 Uiso 1 1 calc R . . H45C H 0.7837 0.5838 0.5587 0.093 Uiso 1 1 calc R . . C47 C 0.8275(5) 0.2656(5) 0.5895(5) 0.052(2) Uani 1 1 d . . . H47 H 0.8098 0.2729 0.6260 0.062 Uiso 1 1 calc R . . C49 C 0.8928(6) 0.2225(5) 0.6176(6) 0.075(3) Uani 1 1 d . . . H49A H 0.9053 0.2046 0.5813 0.112 Uiso 1 1 calc R . . H49B H 0.8847 0.1835 0.6428 0.112 Uiso 1 1 calc R . . H49C H 0.9310 0.2512 0.6470 0.112 Uiso 1 1 calc R . . C48 C 0.7713(6) 0.2268(6) 0.5344(5) 0.073(3) Uani 1 1 d . . . H48A H 0.7285 0.2547 0.5184 0.109 Uiso 1 1 calc R . . H48B H 0.7619 0.1824 0.5515 0.109 Uiso 1 1 calc R . . H48C H 0.7871 0.2183 0.4979 0.109 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 Br4 0.0534(6) 0.0489(6) 0.0746(7) 0.0130(5) 0.0236(5) -0.0047(4) Br3 0.0859(9) 0.1292(13) 0.0823(8) -0.0617(8) 0.0311(7) -0.0046(8) Br1 0.0504(6) 0.0644(7) 0.0632(6) 0.0182(5) 0.0298(5) 0.0139(5) Br2 0.0607(6) 0.0822(8) 0.0573(6) -0.0065(6) 0.0223(5) -0.0211(6) Ni2 0.0290(5) 0.0483(7) 0.0348(5) -0.0015(5) 0.0117(4) -0.0020(5) Ni1 0.0328(6) 0.0586(8) 0.0412(6) 0.0068(5) 0.0177(5) 0.0042(5) N3 0.021(3) 0.023(3) 0.034(3) -0.007(3) 0.007(3) 0.001(2) N4 0.030(3) 0.030(4) 0.024(3) 0.003(3) 0.004(3) -0.004(3) N1 0.029(3) 0.033(4) 0.040(4) 0.010(3) 0.017(3) 0.008(3) N2 0.025(3) 0.045(4) 0.038(4) 0.009(3) 0.022(3) 0.004(3) C17 0.027(4) 0.044(5) 0.026(4) -0.006(4) 0.011(3) -0.010(3) C16 0.030(4) 0.035(5) 0.036(4) 0.000(4) 0.017(3) 0.007(3) C15 0.040(4) 0.023(4) 0.021(3) -0.004(3) 0.010(3) -0.009(3) C14 0.026(4) 0.040(5) 0.029(4) 0.002(3) 0.018(3) 0.005(3) C19 0.024(4) 0.030(4) 0.034(4) 0.011(3) 0.014(3) 0.009(3) C18 0.023(4) 0.031(5) 0.040(4) 0.000(4) 0.009(3) 0.006(3) C20 0.041(5) 0.025(5) 0.061(6) 0.012(4) 0.007(4) 0.003(4) C21 0.142(11) 0.053(7) 0.080(7) 0.032(6) 0.066(8) 0.069(7) C22 0.140(11) 0.036(6) 0.078(8) 0.008(6) 0.047(8) 0.005(7) C23 0.028(4) 0.021(4) 0.059(5) -0.009(4) 0.012(4) 0.006(3) C25 0.045(5) 0.053(6) 0.069(6) 0.001(5) 0.016(5) -0.008(4) C24 0.060(6) 0.040(6) 0.061(6) -0.016(5) 0.008(5) -0.007(5) C13 0.030(4) 0.051(6) 0.041(4) -0.004(4) 0.015(4) 0.000(4) C4 0.023(4) 0.031(5) 0.031(4) -0.001(3) 0.004(3) -0.005(3) C3 0.027(4) 0.038(5) 0.044(5) -0.002(4) 0.012(4) -0.004(3) C2 0.032(4) 0.031(5) 0.049(5) 0.005(4) 0.021(4) 0.007(3) C1 0.026(4) 0.041(5) 0.029(4) 0.002(3) 0.012(3) 0.010(3) C6 0.046(5) 0.030(5) 0.040(4) 0.002(4) 0.023(4) -0.004(4) C5 0.029(4) 0.040(5) 0.028(4) 0.007(3) 0.009(3) -0.003(3) C7 0.070(6) 0.026(5) 0.076(6) -0.003(4) 0.047(6) -0.004(4) C8 0.089(9) 0.056(8) 0.137(11) 0.001(7) 0.058(9) -0.021(7) C9 0.112(9) 0.038(6) 0.063(6) 0.001(5) 0.048(7) 0.018(6) C10 0.060(6) 0.033(5) 0.060(6) -0.011(4) 0.033(5) -0.005(4) C11 0.070(7) 0.040(6) 0.094(8) -0.007(5) 0.037(6) 0.016(5) C12 0.072(7) 0.070(7) 0.055(6) -0.023(5) 0.040(5) -0.018(5) C50 0.018(4) 0.036(5) 0.030(4) -0.007(3) -0.003(3) 0.007(3) C51 0.033(4) 0.033(5) 0.031(4) -0.005(3) 0.014(3) -0.003(3) C52 0.037(5) 0.056(6) 0.034(4) 0.004(4) 0.011(4) -0.005(4) C53 0.051(6) 0.059(6) 0.040(5) 0.015(4) 0.009(4) 0.004(5) C54 0.063(6) 0.066(7) 0.041(5) -0.003(5) 0.029(5) -0.016(5) C55 0.041(5) 0.032(5) 0.040(4) -0.011(4) 0.012(4) -0.012(4) C56 0.045(5) 0.075(7) 0.038(5) -0.007(5) 0.024(4) -0.023(5) C57 0.034(5) 0.067(6) 0.052(5) -0.008(5) 0.031(4) -0.009(4) C58 0.030(4) 0.049(6) 0.043(5) -0.005(4) 0.007(4) -0.005(4) C59 0.025(4) 0.025(4) 0.032(4) -0.011(3) 0.014(3) -0.006(3) C60 0.031(4) 0.033(5) 0.029(4) -0.003(3) 0.012(3) 0.001(3) C61 0.032(4) 0.027(4) 0.034(4) 0.001(3) 0.012(3) 0.001(3) C62 0.029(4) 0.046(5) 0.035(4) 0.010(4) 0.020(3) 0.001(3) C67 0.036(5) 0.058(6) 0.031(4) 0.003(4) 0.005(4) -0.012(4) C66 0.060(7) 0.099(9) 0.034(5) 0.005(5) 0.007(5) -0.045(7) C65 0.033(5) 0.121(11) 0.061(7) 0.050(8) 0.013(5) 0.010(7) C64 0.036(5) 0.075(8) 0.080(7) 0.041(6) 0.032(5) 0.019(5) C63 0.024(4) 0.049(6) 0.043(5) 0.012(4) 0.008(4) 0.002(4) C71 0.075(7) 0.038(6) 0.046(5) -0.012(4) 0.009(5) -0.019(5) C72 0.129(11) 0.052(7) 0.112(10) -0.047(7) 0.062(9) -0.035(7) C73 0.102(9) 0.052(7) 0.059(6) -0.002(5) 0.009(6) -0.028(6) C68 0.067(6) 0.033(5) 0.077(7) 0.016(5) 0.027(6) 0.008(5) C70 0.105(11) 0.136(14) 0.173(16) -0.081(12) 0.034(11) 0.052(10) C69 0.180(15) 0.054(8) 0.096(10) -0.022(7) 0.052(10) -0.036(9) C26 0.031(4) 0.033(5) 0.040(4) -0.005(4) 0.017(4) 0.005(3) C27 0.031(4) 0.032(5) 0.044(5) 0.001(4) 0.019(4) 0.001(3) C28 0.043(5) 0.039(5) 0.052(5) 0.006(4) 0.028(4) 0.005(4) C29 0.032(5) 0.055(6) 0.061(6) 0.014(5) 0.028(4) 0.011(4) C30 0.037(5) 0.049(6) 0.065(6) 0.001(5) 0.020(4) -0.001(4) C31 0.042(5) 0.038(5) 0.048(5) -0.004(4) 0.022(4) 0.004(4) C32 0.039(5) 0.062(7) 0.038(5) -0.003(4) 0.004(4) 0.004(4) C33 0.033(5) 0.080(7) 0.047(5) 0.009(5) 0.006(4) 0.004(5) C34 0.040(5) 0.039(5) 0.038(4) 0.001(4) 0.015(4) 0.006(4) C35 0.044(5) 0.031(5) 0.043(5) -0.001(4) 0.025(4) 0.005(4) C36 0.032(4) 0.041(5) 0.045(5) 0.008(4) 0.022(4) 0.002(3) C37 0.041(5) 0.031(5) 0.039(4) -0.004(4) 0.018(4) 0.000(3) C38 0.030(4) 0.038(5) 0.042(4) 0.009(4) 0.020(4) 0.008(3) C39 0.021(4) 0.032(4) 0.039(4) -0.007(4) 0.014(3) -0.005(3) C40 0.033(4) 0.048(6) 0.047(5) 0.010(4) 0.019(4) 0.010(4) C41 0.062(6) 0.037(5) 0.049(5) 0.007(4) 0.033(5) 0.010(4) C42 0.063(6) 0.034(5) 0.051(5) 0.002(4) 0.026(5) 0.014(4) C43 0.047(5) 0.029(5) 0.052(5) 0.004(4) 0.029(4) 0.007(4) C44 0.048(5) 0.047(6) 0.050(5) -0.007(4) 0.027(4) -0.010(4) C46 0.055(6) 0.045(6) 0.077(7) -0.002(5) 0.010(5) 0.000(5) C45 0.071(7) 0.042(6) 0.075(7) -0.006(5) 0.030(6) 0.003(5) C47 0.053(6) 0.046(6) 0.055(6) 0.005(5) 0.017(5) 0.004(4) C49 0.074(8) 0.043(7) 0.099(9) 0.026(6) 0.022(7) 0.009(5) C48 0.092(8) 0.059(7) 0.078(7) 0.000(6) 0.044(7) -0.016(6) _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 Br4 Ni2 2.3305(15) . ? Br3 Ni2 2.2989(15) . ? Br1 Ni1 2.3306(16) . ? Br2 Ni1 2.3274(17) . ? Ni2 N3 2.027(6) . ? Ni2 N4 2.035(6) . ? Ni1 N1 2.020(6) . ? Ni1 N2 2.031(6) . ? N3 C50 1.283(9) . ? N3 C62 1.437(9) . ? N4 C61 1.270(9) . ? N4 C17 1.465(9) . ? N1 C26 1.279(9) . ? N1 C38 1.478(9) . ? N2 C37 1.292(9) . ? N2 C1 1.465(8) . ? C17 C18 1.379(10) . ? C17 C16 1.400(10) . ? C16 C15 1.401(10) . ? C16 C20 1.538(10) . ? C15 C14 1.378(10) . ? C15 H15 0.9500 . ? C14 C19 1.375(10) . ? C14 C13 1.512(10) . ? C19 C18 1.433(10) . ? C19 H19 0.9500 . ? C18 C23 1.505(10) . ? C20 C22 1.515(13) . ? C20 C21 1.533(13) . ? C20 H20 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 C25 1.529(12) . ? C23 C24 1.542(12) . ? C23 H23 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C13 C4 1.524(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C4 C3 1.370(10) . ? C4 C5 1.390(10) . ? C3 C2 1.406(10) . ? C3 H3 0.9500 . ? C2 C1 1.375(11) . ? C2 C7 1.524(11) . ? C1 C6 1.402(10) . ? C6 C5 1.381(10) . ? C6 C10 1.536(11) . ? C5 H5 0.9500 . ? C7 C9 1.536(13) . ? C7 C8 1.556(15) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.532(13) . ? C10 C12 1.553(12) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C50 C51 1.468(10) . ? C50 C61 1.511(10) . ? C51 C52 1.353(10) . ? C51 C60 1.445(10) . ? C52 C53 1.429(11) . ? C52 H52 0.9500 . ? C53 C54 1.366(12) . ? C53 H53 0.9500 . ? C54 C55 1.432(12) . ? C54 H54 0.9500 . ? C55 C60 1.397(10) . ? C55 C56 1.412(11) . ? C56 C57 1.329(12) . ? C56 H56 0.9500 . ? C57 C58 1.402(11) . ? C57 H57 0.9500 . ? C58 C59 1.369(10) . ? C58 H58 0.9500 . ? C59 C60 1.405(10) . ? C59 C61 1.487(9) . ? C62 C63 1.402(11) . ? C62 C67 1.415(11) . ? C67 C66 1.392(13) . ? C67 C71 1.511(13) . ? C66 C65 1.370(16) . ? C66 H66 0.9500 . ? C65 C64 1.343(16) . ? C65 H65 0.9500 . ? C64 C63 1.409(12) . ? C64 H64 0.9500 . ? C63 C68 1.515(13) . ? C71 C73 1.522(13) . ? C71 C72 1.565(14) . ? C71 H71 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C68 C70 1.539(14) . ? C68 C69 1.541(15) . ? C68 H68 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C26 C27 1.467(10) . ? C26 C37 1.509(10) . ? C27 C28 1.359(10) . ? C27 C36 1.430(10) . ? C28 C29 1.413(11) . ? C28 H28 0.9500 . ? C29 C30 1.377(12) . ? C29 H29 0.9500 . ? C30 C31 1.430(10) . ? C30 H30 0.9500 . ? C31 C36 1.389(11) . ? C31 C32 1.402(11) . ? C32 C33 1.376(11) . ? C32 H32 0.9500 . ? C33 C34 1.421(11) . ? C33 H33 0.9500 . ? C34 C35 1.370(10) . ? C34 H34 0.9500 . ? C35 C36 1.438(9) . ? C35 C37 1.460(11) . ? C38 C39 1.385(10) . ? C38 C43 1.405(11) . ? C39 C40 1.386(10) . ? C39 C44 1.522(11) . ? C40 C41 1.367(12) . ? C40 H40 0.9500 . ? C41 C42 1.385(12) . ? C41 H41 0.9500 . ? C42 C43 1.396(11) . ? C42 H42 0.9500 . ? C43 C47 1.519(12) . ? C44 C46 1.508(12) . ? C44 C45 1.571(13) . ? C44 H44 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C49 1.508(13) . ? C47 C48 1.518(14) . ? C47 H47 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni2 N4 82.1(2) . . ? N3 Ni2 Br3 123.93(17) . . ? N4 Ni2 Br3 109.30(18) . . ? N3 Ni2 Br4 103.38(17) . . ? N4 Ni2 Br4 115.31(18) . . ? Br3 Ni2 Br4 117.93(6) . . ? N1 Ni1 N2 82.2(2) . . ? N1 Ni1 Br2 111.72(19) . . ? N2 Ni1 Br2 110.01(19) . . ? N1 Ni1 Br1 110.83(18) . . ? N2 Ni1 Br1 113.17(19) . . ? Br2 Ni1 Br1 122.01(6) . . ? C50 N3 C62 118.3(6) . . ? C50 N3 Ni2 112.3(5) . . ? C62 N3 Ni2 129.4(4) . . ? C61 N4 C17 116.2(6) . . ? C61 N4 Ni2 111.5(5) . . ? C17 N4 Ni2 132.3(4) . . ? C26 N1 C38 121.2(6) . . ? C26 N1 Ni1 113.1(5) . . ? C38 N1 Ni1 125.6(5) . . ? C37 N2 C1 119.2(6) . . ? C37 N2 Ni1 111.2(5) . . ? C1 N2 Ni1 129.6(4) . . ? C18 C17 C16 125.5(7) . . ? C18 C17 N4 117.6(6) . . ? C16 C17 N4 116.7(7) . . ? C17 C16 C15 115.6(7) . . ? C17 C16 C20 124.0(7) . . ? C15 C16 C20 120.4(7) . . ? C14 C15 C16 122.4(7) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C19 C14 C15 119.2(7) . . ? C19 C14 C13 120.2(7) . . ? C15 C14 C13 120.3(7) . . ? C14 C19 C18 122.2(7) . . ? C14 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C17 C18 C19 114.8(7) . . ? C17 C18 C23 123.0(6) . . ? C19 C18 C23 121.9(6) . . ? C22 C20 C21 108.7(8) . . ? C22 C20 C16 112.5(8) . . ? C21 C20 C16 112.3(7) . . ? C22 C20 H20 107.7 . . ? C21 C20 H20 107.7 . . ? C16 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 C25 113.1(7) . . ? C18 C23 C24 111.0(7) . . ? C25 C23 C24 109.7(7) . . ? C18 C23 H23 107.6 . . ? C25 C23 H23 107.6 . . ? C24 C23 H23 107.6 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C13 C4 107.9(6) . . ? C14 C13 H13A 110.1 . . ? C4 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? C4 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? C3 C4 C5 118.4(7) . . ? C3 C4 C13 121.7(7) . . ? C5 C4 C13 119.7(7) . . ? C4 C3 C2 121.9(7) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C1 C2 C3 116.9(7) . . ? C1 C2 C7 124.4(7) . . ? C3 C2 C7 118.7(7) . . ? C2 C1 C6 123.9(6) . . ? C2 C1 N2 118.8(7) . . ? C6 C1 N2 117.3(6) . . ? C5 C6 C1 116.0(7) . . ? C5 C6 C10 119.2(7) . . ? C1 C6 C10 124.8(6) . . ? C6 C5 C4 122.9(7) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C2 C7 C9 114.0(7) . . ? C2 C7 C8 110.5(8) . . ? C9 C7 C8 109.1(8) . . ? C2 C7 H7 107.7 . . ? C9 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 111.7(8) . . ? C11 C10 C12 110.1(8) . . ? C6 C10 C12 109.2(7) . . ? C11 C10 H10 108.6 . . ? C6 C10 H10 108.6 . . ? C12 C10 H10 108.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C50 C51 136.7(7) . . ? N3 C50 C61 116.1(6) . . ? C51 C50 C61 107.1(6) . . ? C52 C51 C60 118.7(7) . . ? C52 C51 C50 135.7(7) . . ? C60 C51 C50 105.4(6) . . ? C51 C52 C53 120.0(8) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 121.1(8) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C53 C54 C55 121.1(8) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C60 C55 C56 115.9(7) . . ? C60 C55 C54 116.5(7) . . ? C56 C55 C54 127.6(8) . . ? C57 C56 C55 120.7(7) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C58 123.4(8) . . ? C56 C57 H57 118.3 . . ? C58 C57 H57 118.3 . . ? C59 C58 C57 118.3(8) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C58 C59 C60 118.4(7) . . ? C58 C59 C61 136.2(7) . . ? C60 C59 C61 105.3(6) . . ? C55 C60 C59 123.2(7) . . ? C55 C60 C51 122.5(7) . . ? C59 C60 C51 114.3(6) . . ? N4 C61 C59 134.6(7) . . ? N4 C61 C50 117.7(6) . . ? C59 C61 C50 107.5(6) . . ? C63 C62 C67 121.7(7) . . ? C63 C62 N3 117.6(7) . . ? C67 C62 N3 120.5(7) . . ? C66 C67 C62 116.9(9) . . ? C66 C67 C71 121.6(9) . . ? C62 C67 C71 121.5(7) . . ? C65 C66 C67 121.8(10) . . ? C65 C66 H66 119.1 . . ? C67 C66 H66 119.1 . . ? C64 C65 C66 120.8(10) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C65 C64 C63 121.6(10) . . ? C65 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? C62 C63 C64 117.1(9) . . ? C62 C63 C68 120.8(7) . . ? C64 C63 C68 122.1(9) . . ? C67 C71 C73 112.2(9) . . ? C67 C71 C72 111.1(8) . . ? C73 C71 C72 111.1(8) . . ? C67 C71 H71 107.4 . . ? C73 C71 H71 107.4 . . ? C72 C71 H71 107.4 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C63 C68 C70 113.0(9) . . ? C63 C68 C69 110.4(8) . . ? C70 C68 C69 114.4(11) . . ? C63 C68 H68 106.1 . . ? C70 C68 H68 106.1 . . ? C69 C68 H68 106.1 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N1 C26 C27 136.6(7) . . ? N1 C26 C37 115.7(6) . . ? C27 C26 C37 107.6(6) . . ? C28 C27 C36 118.3(7) . . ? C28 C27 C26 135.9(8) . . ? C36 C27 C26 105.8(6) . . ? C27 C28 C29 119.7(8) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 121.0(7) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 122.0(8) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C36 C31 C32 117.3(7) . . ? C36 C31 C30 114.5(7) . . ? C32 C31 C30 128.2(8) . . ? C33 C32 C31 121.5(8) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 120.6(8) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 119.9(7) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 118.3(7) . . ? C34 C35 C37 135.8(7) . . ? C36 C35 C37 105.9(6) . . ? C31 C36 C27 124.5(6) . . ? C31 C36 C35 122.4(7) . . ? C27 C36 C35 113.1(7) . . ? N2 C37 C35 134.9(7) . . ? N2 C37 C26 117.6(7) . . ? C35 C37 C26 107.5(6) . . ? C39 C38 C43 124.2(7) . . ? C39 C38 N1 117.4(7) . . ? C43 C38 N1 118.3(6) . . ? C38 C39 C40 116.3(7) . . ? C38 C39 C44 123.7(7) . . ? C40 C39 C44 120.0(7) . . ? C41 C40 C39 121.9(8) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 120.7(8) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C43 120.5(8) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C38 116.4(7) . . ? C42 C43 C47 119.5(7) . . ? C38 C43 C47 124.0(7) . . ? C46 C44 C39 111.8(7) . . ? C46 C44 C45 109.2(8) . . ? C39 C44 C45 112.2(7) . . ? C46 C44 H44 107.8 . . ? C39 C44 H44 107.8 . . ? C45 C44 H44 107.8 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C49 C47 C48 110.7(9) . . ? C49 C47 C43 111.2(8) . . ? C48 C47 C43 113.1(8) . . ? C49 C47 H47 107.2 . . ? C48 C47 H47 107.2 . . ? C43 C47 H47 107.2 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? 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 N4 Ni2 N3 C50 1.3(5) . . . . ? Br3 Ni2 N3 C50 109.3(5) . . . . ? Br4 Ni2 N3 C50 -112.9(5) . . . . ? N4 Ni2 N3 C62 -176.3(6) . . . . ? Br3 Ni2 N3 C62 -68.3(6) . . . . ? Br4 Ni2 N3 C62 69.4(6) . . . . ? N3 Ni2 N4 C61 -4.6(5) . . . . ? Br3 Ni2 N4 C61 -127.9(5) . . . . ? Br4 Ni2 N4 C61 96.5(5) . . . . ? N3 Ni2 N4 C17 172.8(7) . . . . ? Br3 Ni2 N4 C17 49.5(7) . . . . ? Br4 Ni2 N4 C17 -86.1(6) . . . . ? N2 Ni1 N1 C26 4.1(6) . . . . ? Br2 Ni1 N1 C26 -104.4(5) . . . . ? Br1 Ni1 N1 C26 116.0(5) . . . . ? N2 Ni1 N1 C38 -176.5(6) . . . . ? Br2 Ni1 N1 C38 75.0(6) . . . . ? Br1 Ni1 N1 C38 -64.6(6) . . . . ? N1 Ni1 N2 C37 -4.3(6) . . . . ? Br2 Ni1 N2 C37 106.0(5) . . . . ? Br1 Ni1 N2 C37 -113.7(5) . . . . ? N1 Ni1 N2 C1 179.9(7) . . . . ? Br2 Ni1 N2 C1 -69.8(6) . . . . ? Br1 Ni1 N2 C1 70.5(6) . . . . ? C61 N4 C17 C18 -99.5(8) . . . . ? Ni2 N4 C17 C18 83.1(8) . . . . ? C61 N4 C17 C16 76.0(8) . . . . ? Ni2 N4 C17 C16 -101.4(7) . . . . ? C18 C17 C16 C15 5.6(10) . . . . ? N4 C17 C16 C15 -169.5(6) . . . . ? C18 C17 C16 C20 -175.5(7) . . . . ? N4 C17 C16 C20 9.4(10) . . . . ? C17 C16 C15 C14 -0.6(10) . . . . ? C20 C16 C15 C14 -179.6(6) . . . . ? C16 C15 C14 C19 -4.1(10) . . . . ? C16 C15 C14 C13 170.0(6) . . . . ? C15 C14 C19 C18 4.3(10) . . . . ? C13 C14 C19 C18 -169.7(6) . . . . ? C16 C17 C18 C19 -5.4(11) . . . . ? N4 C17 C18 C19 169.7(6) . . . . ? C16 C17 C18 C23 -179.6(7) . . . . ? N4 C17 C18 C23 -4.5(10) . . . . ? C14 C19 C18 C17 0.2(10) . . . . ? C14 C19 C18 C23 174.4(7) . . . . ? C17 C16 C20 C22 -109.6(9) . . . . ? C15 C16 C20 C22 69.2(10) . . . . ? C17 C16 C20 C21 127.3(9) . . . . ? C15 C16 C20 C21 -53.8(10) . . . . ? C17 C18 C23 C25 -140.7(7) . . . . ? C19 C18 C23 C25 45.5(9) . . . . ? C17 C18 C23 C24 95.5(8) . . . . ? C19 C18 C23 C24 -78.3(9) . . . . ? C19 C14 C13 C4 88.2(8) . . . . ? C15 C14 C13 C4 -85.8(8) . . . . ? C14 C13 C4 C3 93.7(8) . . . . ? C14 C13 C4 C5 -81.6(9) . . . . ? C5 C4 C3 C2 -0.5(11) . . . . ? C13 C4 C3 C2 -175.8(7) . . . . ? C4 C3 C2 C1 -0.3(11) . . . . ? C4 C3 C2 C7 179.0(7) . . . . ? C3 C2 C1 C6 1.2(12) . . . . ? C7 C2 C1 C6 -177.9(8) . . . . ? C3 C2 C1 N2 -179.2(6) . . . . ? C7 C2 C1 N2 1.7(11) . . . . ? C37 N2 C1 C2 94.1(9) . . . . ? Ni1 N2 C1 C2 -90.3(8) . . . . ? C37 N2 C1 C6 -86.2(9) . . . . ? Ni1 N2 C1 C6 89.3(8) . . . . ? C2 C1 C6 C5 -1.3(12) . . . . ? N2 C1 C6 C5 179.0(6) . . . . ? C2 C1 C6 C10 -179.3(8) . . . . ? N2 C1 C6 C10 1.0(12) . . . . ? C1 C6 C5 C4 0.5(11) . . . . ? C10 C6 C5 C4 178.7(7) . . . . ? C3 C4 C5 C6 0.3(11) . . . . ? C13 C4 C5 C6 175.8(7) . . . . ? C1 C2 C7 C9 122.8(9) . . . . ? C3 C2 C7 C9 -56.3(11) . . . . ? C1 C2 C7 C8 -113.8(9) . . . . ? C3 C2 C7 C8 67.0(10) . . . . ? C5 C6 C10 C11 -61.3(10) . . . . ? C1 C6 C10 C11 116.7(9) . . . . ? C5 C6 C10 C12 60.8(10) . . . . ? C1 C6 C10 C12 -121.2(9) . . . . ? C62 N3 C50 C51 3.2(13) . . . . ? Ni2 N3 C50 C51 -174.7(8) . . . . ? C62 N3 C50 C61 179.7(6) . . . . ? Ni2 N3 C50 C61 1.8(8) . . . . ? N3 C50 C51 C52 3.4(17) . . . . ? C61 C50 C51 C52 -173.3(9) . . . . ? N3 C50 C51 C60 -180.0(9) . . . . ? C61 C50 C51 C60 3.4(8) . . . . ? C60 C51 C52 C53 0.6(12) . . . . ? C50 C51 C52 C53 177.0(9) . . . . ? C51 C52 C53 C54 2.2(14) . . . . ? C52 C53 C54 C55 -2.9(15) . . . . ? C53 C54 C55 C60 0.7(13) . . . . ? C53 C54 C55 C56 -177.0(9) . . . . ? C60 C55 C56 C57 0.7(13) . . . . ? C54 C55 C56 C57 178.4(9) . . . . ? C55 C56 C57 C58 -1.9(15) . . . . ? C56 C57 C58 C59 1.7(14) . . . . ? C57 C58 C59 C60 -0.2(12) . . . . ? C57 C58 C59 C61 -177.8(8) . . . . ? C56 C55 C60 C59 0.7(12) . . . . ? C54 C55 C60 C59 -177.2(8) . . . . ? C56 C55 C60 C51 -179.9(8) . . . . ? C54 C55 C60 C51 2.2(12) . . . . ? C58 C59 C60 C55 -1.0(12) . . . . ? C61 C59 C60 C55 177.3(7) . . . . ? C58 C59 C60 C51 179.6(7) . . . . ? C61 C59 C60 C51 -2.1(9) . . . . ? C52 C51 C60 C55 -2.9(12) . . . . ? C50 C51 C60 C55 179.8(7) . . . . ? C52 C51 C60 C59 176.6(7) . . . . ? C50 C51 C60 C59 -0.8(9) . . . . ? C17 N4 C61 C59 3.7(12) . . . . ? Ni2 N4 C61 C59 -178.4(7) . . . . ? C17 N4 C61 C50 -171.0(6) . . . . ? Ni2 N4 C61 C50 6.9(8) . . . . ? C58 C59 C61 N4 6.8(15) . . . . ? C60 C59 C61 N4 -171.0(8) . . . . ? C58 C59 C61 C50 -178.1(9) . . . . ? C60 C59 C61 C50 4.1(8) . . . . ? N3 C50 C61 N4 -6.1(10) . . . . ? C51 C50 C61 N4 171.4(7) . . . . ? N3 C50 C61 C59 177.8(6) . . . . ? C51 C50 C61 C59 -4.7(8) . . . . ? C50 N3 C62 C63 -100.5(8) . . . . ? Ni2 N3 C62 C63 77.0(8) . . . . ? C50 N3 C62 C67 84.0(9) . . . . ? Ni2 N3 C62 C67 -98.4(7) . . . . ? C63 C62 C67 C66 4.6(11) . . . . ? N3 C62 C67 C66 179.9(6) . . . . ? C63 C62 C67 C71 -175.1(7) . . . . ? N3 C62 C67 C71 0.2(11) . . . . ? C62 C67 C66 C65 -2.6(12) . . . . ? C71 C67 C66 C65 177.1(8) . . . . ? C67 C66 C65 C64 1.1(14) . . . . ? C66 C65 C64 C63 -1.5(14) . . . . ? C67 C62 C63 C64 -5.0(11) . . . . ? N3 C62 C63 C64 179.6(6) . . . . ? C67 C62 C63 C68 176.9(7) . . . . ? N3 C62 C63 C68 1.4(10) . . . . ? C65 C64 C63 C62 3.3(12) . . . . ? C65 C64 C63 C68 -178.5(8) . . . . ? C66 C67 C71 C73 -48.6(11) . . . . ? C62 C67 C71 C73 131.1(8) . . . . ? C66 C67 C71 C72 76.5(10) . . . . ? C62 C67 C71 C72 -103.9(9) . . . . ? C62 C63 C68 C70 -143.2(11) . . . . ? C64 C63 C68 C70 38.7(13) . . . . ? C62 C63 C68 C69 87.2(11) . . . . ? C64 C63 C68 C69 -90.9(11) . . . . ? C38 N1 C26 C27 -2.5(14) . . . . ? Ni1 N1 C26 C27 176.9(8) . . . . ? C38 N1 C26 C37 177.4(6) . . . . ? Ni1 N1 C26 C37 -3.2(8) . . . . ? N1 C26 C27 C28 1.3(17) . . . . ? C37 C26 C27 C28 -178.6(9) . . . . ? N1 C26 C27 C36 -179.4(9) . . . . ? C37 C26 C27 C36 0.6(9) . . . . ? C36 C27 C28 C29 0.1(12) . . . . ? C26 C27 C28 C29 179.3(9) . . . . ? C27 C28 C29 C30 0.6(13) . . . . ? C28 C29 C30 C31 -0.7(14) . . . . ? C29 C30 C31 C36 0.1(13) . . . . ? C29 C30 C31 C32 -179.6(9) . . . . ? C36 C31 C32 C33 -1.1(13) . . . . ? C30 C31 C32 C33 178.6(10) . . . . ? C31 C32 C33 C34 0.8(15) . . . . ? C32 C33 C34 C35 0.2(14) . . . . ? C33 C34 C35 C36 -0.8(12) . . . . ? C33 C34 C35 C37 -179.8(9) . . . . ? C32 C31 C36 C27 -179.6(8) . . . . ? C30 C31 C36 C27 0.6(12) . . . . ? C32 C31 C36 C35 0.5(13) . . . . ? C30 C31 C36 C35 -179.3(8) . . . . ? C28 C27 C36 C31 -0.8(12) . . . . ? C26 C27 C36 C31 179.8(8) . . . . ? C28 C27 C36 C35 179.2(8) . . . . ? C26 C27 C36 C35 -0.3(9) . . . . ? C34 C35 C36 C31 0.5(12) . . . . ? C37 C35 C36 C31 179.7(8) . . . . ? C34 C35 C36 C27 -179.4(7) . . . . ? C37 C35 C36 C27 -0.2(9) . . . . ? C1 N2 C37 C35 0.4(14) . . . . ? Ni1 N2 C37 C35 -175.9(8) . . . . ? C1 N2 C37 C26 -179.8(6) . . . . ? Ni1 N2 C37 C26 3.9(9) . . . . ? C34 C35 C37 N2 -0.6(17) . . . . ? C36 C35 C37 N2 -179.6(9) . . . . ? C34 C35 C37 C26 179.6(9) . . . . ? C36 C35 C37 C26 0.6(9) . . . . ? N1 C26 C37 N2 -0.6(11) . . . . ? C27 C26 C37 N2 179.4(7) . . . . ? N1 C26 C37 C35 179.3(7) . . . . ? C27 C26 C37 C35 -0.8(9) . . . . ? C26 N1 C38 C39 -90.4(9) . . . . ? Ni1 N1 C38 C39 90.3(8) . . . . ? C26 N1 C38 C43 93.5(9) . . . . ? Ni1 N1 C38 C43 -85.9(8) . . . . ? C43 C38 C39 C40 -1.9(11) . . . . ? N1 C38 C39 C40 -177.8(6) . . . . ? C43 C38 C39 C44 -179.8(7) . . . . ? N1 C38 C39 C44 4.3(11) . . . . ? C38 C39 C40 C41 1.1(11) . . . . ? C44 C39 C40 C41 179.1(8) . . . . ? C39 C40 C41 C42 0.4(13) . . . . ? C40 C41 C42 C43 -1.3(13) . . . . ? C41 C42 C43 C38 0.6(12) . . . . ? C41 C42 C43 C47 -177.9(8) . . . . ? C39 C38 C43 C42 1.0(12) . . . . ? N1 C38 C43 C42 176.9(7) . . . . ? C39 C38 C43 C47 179.4(8) . . . . ? N1 C38 C43 C47 -4.7(12) . . . . ? C38 C39 C44 C46 97.2(9) . . . . ? C40 C39 C44 C46 -80.7(10) . . . . ? C38 C39 C44 C45 -139.7(8) . . . . ? C40 C39 C44 C45 42.4(10) . . . . ? C42 C43 C47 C49 76.0(11) . . . . ? C38 C43 C47 C49 -102.4(10) . . . . ? C42 C43 C47 C48 -49.3(11) . . . . ? C38 C43 C47 C48 132.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.603 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.157 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 864.2 270.6 2 1.000 0.500 1.000 864.1 270.7 _platon_squeeze_details ; ? ; #==END