# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 #TrackingRef 'CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Dr. Wen-Hua Sun Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; loop_ _publ_author_name _publ_author_address 'Hao Liu' ; Jiangang Yu & Wei Huang' Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Weizhen Zhao' ; Jiangang Yu & Wei Huang' Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Xiang Hao' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Carl Redshaw' ; School of Chemistry University of East Anglia Norwich NR4 7TJ UK ; 'Langqiu Chen' ; College of Chemistry Xiangtan University Xiangtan 411105 China ; 'Wen-Hua Sun' ;Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; _publ_contact_author_email whsun@iccas.ac.cn _publ_contact_author_name 'Dr. Wen-Hua Sun' data_C3 _database_code_depnum_ccdc_archive 'CCDC 831465' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H50 Br2 N2 Ni' _chemical_formula_weight 981.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.378(2) _cell_length_b 16.008(3) _cell_length_c 31.765(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.61(3) _cell_angle_gamma 90.00 _cell_volume 5251.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12427 _cell_measurement_theta_min 1.2720 _cell_measurement_theta_max 26.3622 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 1.927 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4913 _exptl_absorpt_correction_T_max 0.7609 _exptl_absorpt_process_details ? _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' _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 36252 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.34 _reflns_number_total 10463 _reflns_number_gt 8527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'BCrystalClear (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^)+(0.0779P)^2^+7.6842P] 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 10463 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1894 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _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 Br2 Br 0.50762(5) 0.28256(3) 0.236264(18) 0.04153(17) Uani 1 1 d . . . Ni1 Ni 0.42138(6) 0.29097(4) 0.16553(2) 0.02817(17) Uani 1 1 d . . . Br1 Br 0.52411(5) 0.23619(4) 0.11006(2) 0.0505(2) Uani 1 1 d . . . N2 N 0.2291(4) 0.2638(2) 0.16344(12) 0.0265(8) Uani 1 1 d . . . N1 N 0.3563(3) 0.4104(2) 0.16107(12) 0.0247(8) Uani 1 1 d . . . C15 C 0.1026(4) 0.0542(3) 0.13213(16) 0.0292(10) Uani 1 1 d . . . H15A H 0.0931 0.0196 0.1077 0.035 Uiso 1 1 calc R . . C14 C 0.1528(4) 0.1341(3) 0.12885(15) 0.0262(10) Uani 1 1 d . . . C7 C 0.0165(5) 0.4390(3) 0.16407(15) 0.0313(11) Uani 1 1 d . . . C17 C 0.0838(5) 0.0734(3) 0.20610(16) 0.0345(11) Uani 1 1 d . . . H17A H 0.0589 0.0525 0.2321 0.041 Uiso 1 1 calc R . . C12 C 0.2326(4) 0.4134(3) 0.16114(14) 0.0251(10) Uani 1 1 d . . . C46 C 0.4275(4) 0.4873(3) 0.15855(15) 0.0245(10) Uani 1 1 d . . . C1 C 0.1604(4) 0.3314(3) 0.16355(14) 0.0275(10) Uani 1 1 d . . . C13 C 0.1709(4) 0.1828(3) 0.16593(15) 0.0254(10) Uani 1 1 d . . . C11 C 0.1357(4) 0.4800(3) 0.16001(15) 0.0291(10) Uani 1 1 d . . . C49 C 0.5604(5) 0.6351(3) 0.15106(18) 0.0366(12) Uani 1 1 d . . . H49A H 0.6060 0.6861 0.1488 0.044 Uiso 1 1 calc R . . C51 C 0.4637(4) 0.5329(3) 0.19519(15) 0.0262(10) Uani 1 1 d . . . C57 C 0.5608(6) 0.5070(4) 0.26956(19) 0.0499(15) Uani 1 1 d . . . H57A H 0.6270 0.4723 0.2582 0.075 Uiso 1 1 calc R . . H57B H 0.5427 0.4854 0.2972 0.075 Uiso 1 1 calc R . . H57C H 0.5921 0.5647 0.2727 0.075 Uiso 1 1 calc R . . C6 C -0.1001(5) 0.4831(4) 0.16593(17) 0.0390(13) Uani 1 1 d . . . C18 C 0.1373(5) 0.1529(3) 0.20505(15) 0.0297(10) Uani 1 1 d . . . C50 C 0.5297(5) 0.6083(3) 0.19010(17) 0.0330(11) Uani 1 1 d . . . H50A H 0.5538 0.6419 0.2143 0.040 Uiso 1 1 calc R . . C52 C 0.4184(5) 0.4632(3) 0.07824(16) 0.0397(13) Uani 1 1 d . . . H52A H 0.3823 0.4086 0.0869 0.048 Uiso 1 1 calc R . . C55 C 0.4376(5) 0.5050(3) 0.23945(15) 0.0312(11) Uani 1 1 d . . . H55A H 0.4061 0.4460 0.2376 0.037 Uiso 1 1 calc R . . C32 C 0.0056(5) -0.0633(3) 0.17291(16) 0.0333(11) Uani 1 1 d . . . H32A H 0.0145 -0.0788 0.2036 0.040 Uiso 1 1 calc R . . C27 C 0.1311(6) 0.0898(3) 0.01713(17) 0.0419(13) Uani 1 1 d . . . H27A H 0.0543 0.1214 0.0105 0.050 Uiso 1 1 calc R . . C5 C -0.2101(5) 0.4338(4) 0.1709(2) 0.0504(15) Uani 1 1 d . . . H5A H -0.2915 0.4602 0.1724 0.061 Uiso 1 1 calc R . . C19 C 0.1795(4) 0.1713(3) 0.08645(14) 0.0278(10) Uani 1 1 d . . . H19A H 0.2600 0.2056 0.0920 0.033 Uiso 1 1 calc R . . C16 C 0.0658(5) 0.0235(3) 0.17009(16) 0.0307(11) Uani 1 1 d . . . C31 C 0.3218(5) 0.0582(3) 0.06226(17) 0.0391(12) Uani 1 1 d . . . H31A H 0.3769 0.0680 0.0874 0.047 Uiso 1 1 calc R . . C47 C 0.4578(4) 0.5130(3) 0.11822(15) 0.0272(10) Uani 1 1 d . . . C26 C 0.2087(4) 0.1053(3) 0.05432(15) 0.0286(10) Uani 1 1 d . . . C10 C 0.1398(5) 0.5655(3) 0.15713(18) 0.0380(12) Uani 1 1 d . . . H10A H 0.2191 0.5937 0.1544 0.046 Uiso 1 1 calc R . . C33 C -0.1395(5) -0.0640(3) 0.15854(15) 0.0293(10) Uani 1 1 d . . . C34 C -0.2018(5) -0.0060(4) 0.13201(17) 0.0426(13) Uani 1 1 d . . . H34A H -0.1531 0.0382 0.1214 0.051 Uiso 1 1 calc R . . C20 C 0.0718(4) 0.2318(3) 0.07090(15) 0.0280(10) Uani 1 1 d . . . C45 C 0.1560(6) 0.2056(3) 0.24443(16) 0.0401(13) Uani 1 1 d . . . H45A H 0.1280 0.1741 0.2684 0.060 Uiso 1 1 calc R . . H45B H 0.1045 0.2568 0.2403 0.060 Uiso 1 1 calc R . . H45C H 0.2478 0.2201 0.2502 0.060 Uiso 1 1 calc R . . C25 C -0.0576(5) 0.2105(4) 0.07072(19) 0.0449(14) Uani 1 1 d . . . H25A H -0.0804 0.1566 0.0801 0.054 Uiso 1 1 calc R . . C39 C 0.0824(5) -0.1280(3) 0.15049(18) 0.0369(12) Uani 1 1 d . . . C44 C 0.1940(6) -0.1623(4) 0.1719(2) 0.0492(15) Uani 1 1 d . . . H44A H 0.2164 -0.1476 0.2007 0.059 Uiso 1 1 calc R . . C42 C 0.2392(6) -0.2383(4) 0.1110(3) 0.0616(19) Uani 1 1 d . . . H42A H 0.2935 -0.2756 0.0976 0.074 Uiso 1 1 calc R . . C29 C 0.2758(6) -0.0172(4) -0.00260(19) 0.0483(15) Uani 1 1 d . . . H29A H 0.2982 -0.0584 -0.0222 0.058 Uiso 1 1 calc R . . C24 C -0.1552(6) 0.2673(5) 0.0569(2) 0.0536(17) Uani 1 1 d . . . H24A H -0.2433 0.2507 0.0556 0.064 Uiso 1 1 calc R . . C3 C -0.0855(5) 0.3045(4) 0.17074(18) 0.0424(13) Uani 1 1 d . . . H3A H -0.0832 0.2452 0.1718 0.051 Uiso 1 1 calc R . . C2 C 0.0253(4) 0.3508(3) 0.16639(15) 0.0302(11) Uani 1 1 d . . . C40 C 0.0491(6) -0.1517(3) 0.10884(18) 0.0430(13) Uani 1 1 d . . . H40A H -0.0278 -0.1304 0.0940 0.052 Uiso 1 1 calc R . . C8 C -0.0912(5) 0.5714(4) 0.16272(18) 0.0432(13) Uani 1 1 d . . . H8A H -0.1676 0.6038 0.1637 0.052 Uiso 1 1 calc R . . C9 C 0.0219(5) 0.6109(4) 0.15837(18) 0.0442(14) Uani 1 1 d . . . H9A H 0.0229 0.6701 0.1561 0.053 Uiso 1 1 calc R . . C48 C 0.5254(5) 0.5882(3) 0.11529(17) 0.0343(11) Uani 1 1 d . . . H48A H 0.5473 0.6070 0.0885 0.041 Uiso 1 1 calc R . . C22 C 0.0050(6) 0.3694(4) 0.0455(2) 0.0572(17) Uani 1 1 d . . . H22A H 0.0273 0.4240 0.0371 0.069 Uiso 1 1 calc R . . C54 C 0.3110(7) 0.5093(5) 0.05099(19) 0.0591(18) Uani 1 1 d . . . H54A H 0.2382 0.5200 0.0677 0.089 Uiso 1 1 calc R . . H54B H 0.2815 0.4750 0.0264 0.089 Uiso 1 1 calc R . . H54C H 0.3445 0.5626 0.0414 0.089 Uiso 1 1 calc R . . C38 C -0.2149(6) -0.1272(3) 0.1738(2) 0.0455(14) Uani 1 1 d . . . H38A H -0.1758 -0.1678 0.1928 0.055 Uiso 1 1 calc R . . C21 C 0.1023(5) 0.3125(3) 0.05816(18) 0.0384(12) Uani 1 1 d . . . H21A H 0.1904 0.3285 0.0581 0.046 Uiso 1 1 calc R . . C30 C 0.3558(6) -0.0033(4) 0.0339(2) 0.0513(15) Uani 1 1 d . . . H30A H 0.4330 -0.0349 0.0397 0.062 Uiso 1 1 calc R . . C56 C 0.3310(6) 0.5588(4) 0.25685(18) 0.0452(14) Uani 1 1 d . . . H56A H 0.3159 0.5390 0.2852 0.068 Uiso 1 1 calc R . . H56B H 0.2508 0.5541 0.2380 0.068 Uiso 1 1 calc R . . H56C H 0.3589 0.6173 0.2585 0.068 Uiso 1 1 calc R . . C28 C 0.1655(6) 0.0275(4) -0.01079(18) 0.0469(14) Uani 1 1 d . . . H28A H 0.1104 0.0165 -0.0359 0.056 Uiso 1 1 calc R . . C37 C -0.3474(6) -0.1311(4) 0.1614(2) 0.0531(17) Uani 1 1 d . . . H37A H -0.3974 -0.1748 0.1718 0.064 Uiso 1 1 calc R . . C41 C 0.1272(7) -0.2066(4) 0.0884(2) 0.0548(16) Uani 1 1 d . . . H41A H 0.1048 -0.2220 0.0597 0.066 Uiso 1 1 calc R . . C4 C -0.2021(5) 0.3489(4) 0.1736(2) 0.0514(16) Uani 1 1 d . . . H4A H -0.2783 0.3183 0.1776 0.062 Uiso 1 1 calc R . . C23 C -0.1244(6) 0.3471(4) 0.0451(2) 0.0568(17) Uani 1 1 d . . . H23A H -0.1908 0.3863 0.0368 0.068 Uiso 1 1 calc R . . C43 C 0.2715(6) -0.2160(4) 0.1529(3) 0.0588(18) Uani 1 1 d . . . H43A H 0.3473 -0.2381 0.1681 0.071 Uiso 1 1 calc R . . C35 C -0.3335(6) -0.0101(4) 0.12034(19) 0.0521(16) Uani 1 1 d . . . H35A H -0.3737 0.0316 0.1022 0.062 Uiso 1 1 calc R . . C36 C -0.4065(6) -0.0732(4) 0.13452(19) 0.0470(14) Uani 1 1 d . . . H36A H -0.4966 -0.0767 0.1259 0.056 Uiso 1 1 calc R . . C53 C 0.5335(7) 0.4446(4) 0.0532(2) 0.0593(18) Uani 1 1 d . . . H53A H 0.5997 0.4140 0.0711 0.089 Uiso 1 1 calc R . . H53B H 0.5701 0.4972 0.0440 0.089 Uiso 1 1 calc R . . H53C H 0.5046 0.4106 0.0284 0.089 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 Br2 0.0436(3) 0.0361(3) 0.0441(3) 0.0082(2) 0.0001(2) 0.0024(2) Ni1 0.0206(3) 0.0237(3) 0.0406(4) 0.0008(2) 0.0051(3) -0.0007(2) Br1 0.0351(3) 0.0580(4) 0.0615(4) -0.0210(3) 0.0198(3) -0.0087(3) N2 0.026(2) 0.027(2) 0.027(2) 0.0004(16) 0.0047(17) -0.0081(16) N1 0.0199(18) 0.0205(18) 0.034(2) 0.0003(15) 0.0054(16) -0.0033(14) C15 0.028(2) 0.027(2) 0.033(3) 0.005(2) 0.005(2) 0.0006(19) C14 0.020(2) 0.025(2) 0.034(3) -0.0020(19) 0.0048(19) -0.0045(17) C7 0.025(2) 0.038(3) 0.031(3) -0.007(2) 0.004(2) 0.000(2) C17 0.033(3) 0.039(3) 0.033(3) 0.005(2) 0.005(2) -0.011(2) C12 0.024(2) 0.024(2) 0.027(2) 0.0002(18) 0.0035(19) -0.0008(18) C46 0.018(2) 0.024(2) 0.032(3) 0.0015(19) 0.0059(19) -0.0025(17) C1 0.023(2) 0.034(3) 0.026(3) -0.0019(19) 0.0041(19) -0.0036(19) C13 0.022(2) 0.020(2) 0.034(3) 0.0013(18) 0.0038(19) -0.0034(17) C11 0.022(2) 0.034(3) 0.031(3) -0.003(2) 0.003(2) 0.0005(19) C49 0.032(3) 0.020(2) 0.059(4) 0.002(2) 0.011(3) -0.004(2) C51 0.020(2) 0.020(2) 0.038(3) -0.0028(19) 0.003(2) 0.0010(17) C57 0.051(4) 0.054(4) 0.043(3) 0.006(3) -0.002(3) -0.009(3) C6 0.021(2) 0.052(3) 0.045(3) -0.011(3) 0.002(2) 0.006(2) C18 0.031(2) 0.030(2) 0.028(3) -0.001(2) 0.001(2) -0.004(2) C50 0.030(3) 0.024(2) 0.045(3) -0.004(2) 0.005(2) -0.0003(19) C52 0.047(3) 0.037(3) 0.036(3) 0.005(2) 0.012(2) -0.014(2) C55 0.034(3) 0.028(2) 0.033(3) -0.003(2) 0.010(2) -0.004(2) C32 0.037(3) 0.028(2) 0.035(3) 0.009(2) 0.005(2) -0.006(2) C27 0.044(3) 0.041(3) 0.041(3) -0.003(2) 0.001(3) 0.001(2) C5 0.024(3) 0.057(4) 0.070(4) -0.015(3) 0.009(3) 0.001(3) C19 0.027(2) 0.030(2) 0.027(3) 0.0025(19) 0.004(2) -0.0015(19) C16 0.029(2) 0.024(2) 0.038(3) 0.005(2) -0.002(2) -0.0044(19) C31 0.037(3) 0.042(3) 0.038(3) -0.006(2) 0.000(2) 0.009(2) C47 0.027(2) 0.021(2) 0.034(3) 0.0007(19) 0.004(2) -0.0020(18) C26 0.026(2) 0.031(2) 0.029(3) -0.002(2) 0.009(2) -0.0066(19) C10 0.032(3) 0.025(2) 0.058(4) -0.001(2) 0.010(2) 0.003(2) C33 0.034(3) 0.024(2) 0.031(3) -0.0030(19) 0.011(2) -0.0068(19) C34 0.035(3) 0.050(3) 0.044(3) 0.018(3) 0.008(2) -0.007(2) C20 0.023(2) 0.033(3) 0.027(3) 0.000(2) 0.0008(19) -0.0006(19) C45 0.048(3) 0.040(3) 0.032(3) -0.003(2) 0.006(2) -0.016(2) C25 0.028(3) 0.053(4) 0.054(4) 0.015(3) 0.005(3) -0.005(2) C39 0.036(3) 0.020(2) 0.054(4) 0.006(2) 0.003(3) -0.006(2) C44 0.041(3) 0.039(3) 0.063(4) 0.002(3) -0.018(3) -0.002(3) C42 0.048(4) 0.036(3) 0.104(6) -0.002(3) 0.026(4) 0.007(3) C29 0.059(4) 0.041(3) 0.047(4) -0.014(3) 0.015(3) 0.006(3) C24 0.026(3) 0.083(5) 0.052(4) 0.017(3) 0.007(3) 0.007(3) C3 0.027(3) 0.047(3) 0.054(4) -0.012(3) 0.012(2) -0.013(2) C2 0.022(2) 0.039(3) 0.029(3) -0.008(2) 0.001(2) -0.003(2) C40 0.047(3) 0.032(3) 0.051(4) 0.003(2) 0.011(3) 0.005(2) C8 0.030(3) 0.048(3) 0.050(3) -0.010(3) 0.000(3) 0.012(2) C9 0.039(3) 0.041(3) 0.051(4) -0.005(3) 0.001(3) 0.013(2) C48 0.031(3) 0.029(3) 0.044(3) 0.006(2) 0.011(2) -0.003(2) C22 0.051(4) 0.040(3) 0.081(5) 0.017(3) 0.008(3) 0.013(3) C54 0.063(4) 0.075(5) 0.038(3) 0.008(3) 0.000(3) -0.018(4) C38 0.047(3) 0.028(3) 0.063(4) 0.006(3) 0.014(3) -0.006(2) C21 0.034(3) 0.031(3) 0.049(3) 0.005(2) 0.001(2) -0.002(2) C30 0.045(3) 0.050(4) 0.059(4) -0.012(3) 0.007(3) 0.009(3) C56 0.045(3) 0.045(3) 0.048(3) -0.004(3) 0.016(3) -0.005(3) C28 0.056(4) 0.052(3) 0.032(3) -0.009(3) -0.002(3) -0.005(3) C37 0.043(3) 0.033(3) 0.086(5) -0.014(3) 0.023(3) -0.014(3) C41 0.064(4) 0.045(3) 0.058(4) -0.003(3) 0.018(3) 0.000(3) C4 0.020(3) 0.067(4) 0.068(4) -0.004(3) 0.013(3) -0.009(3) C23 0.047(4) 0.068(4) 0.057(4) 0.016(3) 0.007(3) 0.027(3) C43 0.038(3) 0.042(3) 0.094(6) -0.001(3) -0.007(3) 0.005(3) C35 0.039(3) 0.070(4) 0.048(4) 0.010(3) 0.005(3) 0.003(3) C36 0.034(3) 0.058(4) 0.050(4) -0.016(3) 0.007(3) -0.011(3) C53 0.077(5) 0.052(4) 0.054(4) -0.011(3) 0.033(4) -0.010(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 Br2 Ni1 2.3398(10) . ? Ni1 N1 2.028(4) . ? Ni1 N2 2.037(4) . ? Ni1 Br1 2.3188(10) . ? N2 C1 1.295(6) . ? N2 C13 1.435(5) . ? N1 C12 1.285(6) . ? N1 C46 1.442(5) . ? C15 C14 1.389(6) . ? C15 C16 1.390(7) . ? C15 H15A 0.9500 . ? C14 C13 1.410(6) . ? C14 C19 1.523(6) . ? C7 C6 1.407(7) . ? C7 C2 1.416(7) . ? C7 C11 1.418(7) . ? C17 C18 1.391(7) . ? C17 C16 1.393(7) . ? C17 H17A 0.9500 . ? C12 C11 1.464(6) . ? C12 C1 1.518(6) . ? C46 C51 1.394(6) . ? C46 C47 1.410(6) . ? C1 C2 1.448(6) . ? C13 C18 1.407(7) . ? C11 C10 1.371(7) . ? C49 C50 1.379(7) . ? C49 C48 1.380(7) . ? C49 H49A 0.9500 . ? C51 C50 1.406(6) . ? C51 C55 1.524(7) . ? C57 C55 1.521(8) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C6 C5 1.409(8) . ? C6 C8 1.421(8) . ? C18 C45 1.505(7) . ? C50 H50A 0.9500 . ? C52 C47 1.521(7) . ? C52 C53 1.528(8) . ? C52 C54 1.533(9) . ? C52 H52A 1.0000 . ? C55 C56 1.545(7) . ? C55 H55A 1.0000 . ? C32 C39 1.526(7) . ? C32 C16 1.529(6) . ? C32 C33 1.530(7) . ? C32 H32A 1.0000 . ? C27 C26 1.386(7) . ? C27 C28 1.404(8) . ? C27 H27A 0.9500 . ? C5 C4 1.363(9) . ? C5 H5A 0.9500 . ? C19 C26 1.520(6) . ? C19 C20 1.525(6) . ? C19 H19A 1.0000 . ? C31 C26 1.398(7) . ? C31 C30 1.403(8) . ? C31 H31A 0.9500 . ? C47 C48 1.401(6) . ? C10 C9 1.428(7) . ? C10 H10A 0.9500 . ? C33 C34 1.373(7) . ? C33 C38 1.395(7) . ? C34 C35 1.382(8) . ? C34 H34A 0.9500 . ? C20 C25 1.385(7) . ? C20 C21 1.398(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C25 C24 1.400(8) . ? C25 H25A 0.9500 . ? C39 C40 1.387(8) . ? C39 C44 1.397(7) . ? C44 C43 1.360(9) . ? C44 H44A 0.9500 . ? C42 C43 1.385(10) . ? C42 C41 1.402(10) . ? C42 H42A 0.9500 . ? C29 C28 1.354(8) . ? C29 C30 1.375(9) . ? C29 H29A 0.9500 . ? C24 C23 1.377(9) . ? C24 H24A 0.9500 . ? C3 C2 1.387(7) . ? C3 C4 1.414(8) . ? C3 H3A 0.9500 . ? C40 C41 1.398(8) . ? C40 H40A 0.9500 . ? C8 C9 1.352(8) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C48 H48A 0.9500 . ? C22 C23 1.389(9) . ? C22 C21 1.389(8) . ? C22 H22A 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C38 C37 1.395(8) . ? C38 H38A 0.9500 . ? C21 H21A 0.9500 . ? C30 H30A 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C28 H28A 0.9500 . ? C37 C36 1.364(9) . ? C37 H37A 0.9500 . ? C41 H41A 0.9500 . ? C4 H4A 0.9500 . ? C23 H23A 0.9500 . ? C43 H43A 0.9500 . ? C35 C36 1.366(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 83.14(15) . . ? N1 Ni1 Br1 118.56(11) . . ? N2 Ni1 Br1 114.60(12) . . ? N1 Ni1 Br2 102.40(11) . . ? N2 Ni1 Br2 107.48(12) . . ? Br1 Ni1 Br2 123.15(4) . . ? C1 N2 C13 121.3(4) . . ? C1 N2 Ni1 111.0(3) . . ? C13 N2 Ni1 127.4(3) . . ? C12 N1 C46 119.1(4) . . ? C12 N1 Ni1 111.2(3) . . ? C46 N1 Ni1 129.8(3) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C15 C14 C13 117.9(4) . . ? C15 C14 C19 121.9(4) . . ? C13 C14 C19 120.1(4) . . ? C6 C7 C2 123.3(5) . . ? C6 C7 C11 122.2(5) . . ? C2 C7 C11 114.5(4) . . ? C18 C17 C16 121.8(5) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? N1 C12 C11 135.4(4) . . ? N1 C12 C1 117.7(4) . . ? C11 C12 C1 106.9(4) . . ? C51 C46 C47 122.7(4) . . ? C51 C46 N1 119.9(4) . . ? C47 C46 N1 117.4(4) . . ? N2 C1 C2 135.7(4) . . ? N2 C1 C12 116.6(4) . . ? C2 C1 C12 107.6(4) . . ? C18 C13 C14 121.7(4) . . ? C18 C13 N2 119.8(4) . . ? C14 C13 N2 118.4(4) . . ? C10 C11 C7 120.1(5) . . ? C10 C11 C12 134.6(4) . . ? C7 C11 C12 105.3(4) . . ? C50 C49 C48 120.4(5) . . ? C50 C49 H49A 119.8 . . ? C48 C49 H49A 119.8 . . ? C46 C51 C50 116.6(4) . . ? C46 C51 C55 124.0(4) . . ? C50 C51 C55 119.3(4) . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C7 C6 C5 115.7(5) . . ? C7 C6 C8 115.8(5) . . ? C5 C6 C8 128.6(5) . . ? C17 C18 C13 117.8(4) . . ? C17 C18 C45 120.8(4) . . ? C13 C18 C45 121.4(4) . . ? C49 C50 C51 121.9(5) . . ? C49 C50 H50A 119.0 . . ? C51 C50 H50A 119.0 . . ? C47 C52 C53 112.1(5) . . ? C47 C52 C54 109.9(5) . . ? C53 C52 C54 111.2(5) . . ? C47 C52 H52A 107.8 . . ? C53 C52 H52A 107.8 . . ? C54 C52 H52A 107.8 . . ? C57 C55 C51 111.1(4) . . ? C57 C55 C56 110.5(4) . . ? C51 C55 C56 111.4(4) . . ? C57 C55 H55A 107.9 . . ? C51 C55 H55A 107.9 . . ? C56 C55 H55A 107.9 . . ? C39 C32 C16 110.7(4) . . ? C39 C32 C33 113.5(4) . . ? C16 C32 C33 112.7(4) . . ? C39 C32 H32A 106.4 . . ? C16 C32 H32A 106.4 . . ? C33 C32 H32A 106.4 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C26 C19 C14 112.8(4) . . ? C26 C19 C20 114.3(4) . . ? C14 C19 C20 110.1(4) . . ? C26 C19 H19A 106.3 . . ? C14 C19 H19A 106.3 . . ? C20 C19 H19A 106.3 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 C32 121.4(4) . . ? C17 C16 C32 119.7(4) . . ? C26 C31 C30 121.5(5) . . ? C26 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? C48 C47 C46 118.0(4) . . ? C48 C47 C52 119.4(4) . . ? C46 C47 C52 122.6(4) . . ? C27 C26 C31 117.7(5) . . ? C27 C26 C19 124.0(5) . . ? C31 C26 C19 118.2(4) . . ? C11 C10 C9 118.3(5) . . ? C11 C10 H10A 120.9 . . ? C9 C10 H10A 120.9 . . ? C34 C33 C38 117.3(5) . . ? C34 C33 C32 124.6(4) . . ? C38 C33 C32 118.1(5) . . ? C33 C34 C35 121.8(5) . . ? C33 C34 H34A 119.1 . . ? C35 C34 H34A 119.1 . . ? C25 C20 C21 118.2(5) . . ? C25 C20 C19 121.6(5) . . ? C21 C20 C19 120.1(4) . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C20 C25 C24 120.8(5) . . ? C20 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C40 C39 C44 118.4(5) . . ? C40 C39 C32 122.6(5) . . ? C44 C39 C32 119.0(5) . . ? C43 C44 C39 122.0(6) . . ? C43 C44 H44A 119.0 . . ? C39 C44 H44A 119.0 . . ? C43 C42 C41 120.7(6) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C28 C29 C30 120.4(5) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C23 C24 C25 120.6(6) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C2 C3 C4 117.4(5) . . ? C2 C3 H3A 121.3 . . ? C4 C3 H3A 121.3 . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 135.1(5) . . ? C7 C2 C1 105.6(4) . . ? C39 C40 C41 120.9(6) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C9 C8 C6 122.4(5) . . ? C9 C8 H8A 118.8 . . ? C6 C8 H8A 118.8 . . ? C8 C9 C10 121.3(5) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C49 C48 C47 120.4(5) . . ? C49 C48 H48A 119.8 . . ? C47 C48 H48A 119.8 . . ? C23 C22 C21 120.6(6) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C33 C38 C37 120.3(6) . . ? C33 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C22 C21 C20 120.7(5) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C29 C30 C31 119.1(5) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C29 C28 C27 121.1(5) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C36 C37 C38 121.2(5) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C40 C41 C42 118.6(6) . . ? C40 C41 H41A 120.7 . . ? C42 C41 H41A 120.7 . . ? C5 C4 C3 123.0(5) . . ? C5 C4 H4A 118.5 . . ? C3 C4 H4A 118.5 . . ? C24 C23 C22 119.0(5) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C44 C43 C42 119.5(6) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C36 C35 C34 120.8(6) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C37 C36 C35 118.6(6) . . ? C37 C36 H36A 120.7 . . ? C35 C36 H36A 120.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N2 C1 -4.7(3) . . . . ? Br1 Ni1 N2 C1 -123.0(3) . . . . ? Br2 Ni1 N2 C1 96.2(3) . . . . ? N1 Ni1 N2 C13 -178.4(4) . . . . ? Br1 Ni1 N2 C13 63.2(4) . . . . ? Br2 Ni1 N2 C13 -77.5(4) . . . . ? N2 Ni1 N1 C12 3.0(3) . . . . ? Br1 Ni1 N1 C12 117.4(3) . . . . ? Br2 Ni1 N1 C12 -103.4(3) . . . . ? N2 Ni1 N1 C46 -177.8(4) . . . . ? Br1 Ni1 N1 C46 -63.5(4) . . . . ? Br2 Ni1 N1 C46 75.7(4) . . . . ? C16 C15 C14 C13 2.6(7) . . . . ? C16 C15 C14 C19 -173.3(4) . . . . ? C46 N1 C12 C11 -1.5(8) . . . . ? Ni1 N1 C12 C11 177.8(5) . . . . ? C46 N1 C12 C1 179.6(4) . . . . ? Ni1 N1 C12 C1 -1.1(5) . . . . ? C12 N1 C46 C51 84.3(6) . . . . ? Ni1 N1 C46 C51 -94.8(5) . . . . ? C12 N1 C46 C47 -95.8(5) . . . . ? Ni1 N1 C46 C47 85.1(5) . . . . ? C13 N2 C1 C2 1.2(8) . . . . ? Ni1 N2 C1 C2 -173.0(5) . . . . ? C13 N2 C1 C12 179.5(4) . . . . ? Ni1 N2 C1 C12 5.3(5) . . . . ? N1 C12 C1 N2 -3.0(6) . . . . ? C11 C12 C1 N2 177.8(4) . . . . ? N1 C12 C1 C2 175.8(4) . . . . ? C11 C12 C1 C2 -3.4(5) . . . . ? C15 C14 C13 C18 -1.2(7) . . . . ? C19 C14 C13 C18 174.8(4) . . . . ? C15 C14 C13 N2 176.7(4) . . . . ? C19 C14 C13 N2 -7.2(6) . . . . ? C1 N2 C13 C18 -77.5(6) . . . . ? Ni1 N2 C13 C18 95.7(5) . . . . ? C1 N2 C13 C14 104.5(5) . . . . ? Ni1 N2 C13 C14 -82.3(5) . . . . ? C6 C7 C11 C10 -1.0(8) . . . . ? C2 C7 C11 C10 179.5(5) . . . . ? C6 C7 C11 C12 177.6(5) . . . . ? C2 C7 C11 C12 -1.9(6) . . . . ? N1 C12 C11 C10 2.4(10) . . . . ? C1 C12 C11 C10 -178.6(6) . . . . ? N1 C12 C11 C7 -175.8(5) . . . . ? C1 C12 C11 C7 3.2(5) . . . . ? C47 C46 C51 C50 1.8(7) . . . . ? N1 C46 C51 C50 -178.3(4) . . . . ? C47 C46 C51 C55 -177.3(4) . . . . ? N1 C46 C51 C55 2.6(7) . . . . ? C2 C7 C6 C5 0.8(8) . . . . ? C11 C7 C6 C5 -178.7(5) . . . . ? C2 C7 C6 C8 -179.4(5) . . . . ? C11 C7 C6 C8 1.1(8) . . . . ? C16 C17 C18 C13 1.2(8) . . . . ? C16 C17 C18 C45 -179.9(5) . . . . ? C14 C13 C18 C17 -0.6(7) . . . . ? N2 C13 C18 C17 -178.6(4) . . . . ? C14 C13 C18 C45 -179.5(5) . . . . ? N2 C13 C18 C45 2.5(7) . . . . ? C48 C49 C50 C51 0.7(7) . . . . ? C46 C51 C50 C49 -1.7(7) . . . . ? C55 C51 C50 C49 177.5(4) . . . . ? C46 C51 C55 C57 128.0(5) . . . . ? C50 C51 C55 C57 -51.1(6) . . . . ? C46 C51 C55 C56 -108.3(5) . . . . ? C50 C51 C55 C56 72.6(6) . . . . ? C7 C6 C5 C4 -0.1(9) . . . . ? C8 C6 C5 C4 -179.8(6) . . . . ? C15 C14 C19 C26 -27.5(6) . . . . ? C13 C14 C19 C26 156.6(4) . . . . ? C15 C14 C19 C20 101.5(5) . . . . ? C13 C14 C19 C20 -74.3(5) . . . . ? C14 C15 C16 C17 -2.1(7) . . . . ? C14 C15 C16 C32 177.5(4) . . . . ? C18 C17 C16 C15 0.1(8) . . . . ? C18 C17 C16 C32 -179.5(5) . . . . ? C39 C32 C16 C15 46.5(6) . . . . ? C33 C32 C16 C15 -81.9(6) . . . . ? C39 C32 C16 C17 -133.9(5) . . . . ? C33 C32 C16 C17 97.7(5) . . . . ? C51 C46 C47 C48 -1.0(7) . . . . ? N1 C46 C47 C48 179.1(4) . . . . ? C51 C46 C47 C52 180.0(5) . . . . ? N1 C46 C47 C52 0.0(7) . . . . ? C53 C52 C47 C48 54.1(7) . . . . ? C54 C52 C47 C48 -70.2(6) . . . . ? C53 C52 C47 C46 -126.9(5) . . . . ? C54 C52 C47 C46 108.9(5) . . . . ? C28 C27 C26 C31 1.2(8) . . . . ? C28 C27 C26 C19 180.0(5) . . . . ? C30 C31 C26 C27 -0.5(8) . . . . ? C30 C31 C26 C19 -179.4(5) . . . . ? C14 C19 C26 C27 115.3(5) . . . . ? C20 C19 C26 C27 -11.6(7) . . . . ? C14 C19 C26 C31 -65.9(6) . . . . ? C20 C19 C26 C31 167.2(4) . . . . ? C7 C11 C10 C9 0.1(8) . . . . ? C12 C11 C10 C9 -178.0(5) . . . . ? C39 C32 C33 C34 -104.0(6) . . . . ? C16 C32 C33 C34 22.9(7) . . . . ? C39 C32 C33 C38 77.0(6) . . . . ? C16 C32 C33 C38 -156.1(5) . . . . ? C38 C33 C34 C35 -0.8(8) . . . . ? C32 C33 C34 C35 -179.8(5) . . . . ? C26 C19 C20 C25 80.1(6) . . . . ? C14 C19 C20 C25 -48.2(6) . . . . ? C26 C19 C20 C21 -102.9(5) . . . . ? C14 C19 C20 C21 128.9(5) . . . . ? C21 C20 C25 C24 2.0(9) . . . . ? C19 C20 C25 C24 179.1(5) . . . . ? C16 C32 C39 C40 -94.9(6) . . . . ? C33 C32 C39 C40 33.0(7) . . . . ? C16 C32 C39 C44 82.2(6) . . . . ? C33 C32 C39 C44 -149.8(5) . . . . ? C40 C39 C44 C43 1.7(9) . . . . ? C32 C39 C44 C43 -175.6(5) . . . . ? C20 C25 C24 C23 -3.1(10) . . . . ? C4 C3 C2 C7 -1.4(8) . . . . ? C4 C3 C2 C1 178.2(6) . . . . ? C6 C7 C2 C3 0.0(8) . . . . ? C11 C7 C2 C3 179.5(5) . . . . ? C6 C7 C2 C1 -179.7(5) . . . . ? C11 C7 C2 C1 -0.2(6) . . . . ? N2 C1 C2 C3 1.0(10) . . . . ? C12 C1 C2 C3 -177.4(6) . . . . ? N2 C1 C2 C7 -179.3(5) . . . . ? C12 C1 C2 C7 2.2(5) . . . . ? C44 C39 C40 C41 -1.9(8) . . . . ? C32 C39 C40 C41 175.2(5) . . . . ? C7 C6 C8 C9 -0.4(8) . . . . ? C5 C6 C8 C9 179.4(6) . . . . ? C6 C8 C9 C10 -0.5(9) . . . . ? C11 C10 C9 C8 0.7(9) . . . . ? C50 C49 C48 C47 0.2(8) . . . . ? C46 C47 C48 C49 -0.1(7) . . . . ? C52 C47 C48 C49 179.0(5) . . . . ? C34 C33 C38 C37 1.5(8) . . . . ? C32 C33 C38 C37 -179.4(5) . . . . ? C23 C22 C21 C20 -0.4(10) . . . . ? C25 C20 C21 C22 -0.2(8) . . . . ? C19 C20 C21 C22 -177.4(5) . . . . ? C28 C29 C30 C31 -0.4(10) . . . . ? C26 C31 C30 C29 0.1(9) . . . . ? C30 C29 C28 C27 1.1(10) . . . . ? C26 C27 C28 C29 -1.5(9) . . . . ? C33 C38 C37 C36 -0.7(9) . . . . ? C39 C40 C41 C42 1.0(9) . . . . ? C43 C42 C41 C40 0.2(10) . . . . ? C6 C5 C4 C3 -1.4(10) . . . . ? C2 C3 C4 C5 2.2(9) . . . . ? C25 C24 C23 C22 2.5(10) . . . . ? C21 C22 C23 C24 -0.8(10) . . . . ? C39 C44 C43 C42 -0.5(10) . . . . ? C41 C42 C43 C44 -0.4(10) . . . . ? C33 C34 C35 C36 -0.8(10) . . . . ? C38 C37 C36 C35 -0.9(9) . . . . ? C34 C35 C36 C37 1.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.484 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.147 #==END data_C5 _database_code_depnum_ccdc_archive 'CCDC 831466' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 Br2 N2 Ni' _chemical_formula_weight 967.49 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.352(3) _cell_length_b 22.551(5) _cell_length_c 15.380(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.96(3) _cell_angle_gamma 90.00 _cell_volume 5093.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13210 _cell_measurement_theta_min 1.3842 _cell_measurement_theta_max 25.0270 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6691 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details ? _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 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _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 35074 _diffrn_reflns_av_R_equivalents 0.0898 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9011 _reflns_number_gt 6827 _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^)+(0.0660P)^2^+4.7031P] 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 9011 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1664 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.16042(4) 0.55066(3) 0.29211(4) 0.03048(18) Uani 1 1 d . . . N2 N 0.1916(2) 0.63680(16) 0.2746(2) 0.0236(8) Uani 1 1 d . . . Br1 Br 0.15216(5) 0.47618(3) 0.18564(5) 0.0557(2) Uani 1 1 d . . . N1 N 0.0353(3) 0.58501(17) 0.2760(2) 0.0253(9) Uani 1 1 d . . . Br2 Br 0.23978(4) 0.53404(3) 0.44385(4) 0.0558(2) Uani 1 1 d . . . C46 C -0.0460(3) 0.5550(2) 0.2806(3) 0.0253(10) Uani 1 1 d . . . C13 C 0.2786(3) 0.66120(19) 0.2748(3) 0.0235(10) Uani 1 1 d . . . C2 C 0.1073(3) 0.7349(2) 0.2641(3) 0.0254(10) Uani 1 1 d . . . C6 C -0.0285(3) 0.7980(2) 0.2521(3) 0.0320(11) Uani 1 1 d . . . C11 C -0.0339(3) 0.6883(2) 0.2565(3) 0.0270(10) Uani 1 1 d . . . C51 C -0.0664(3) 0.5559(2) 0.3647(3) 0.0263(10) Uani 1 1 d . . . C12 C 0.0342(3) 0.6417(2) 0.2661(3) 0.0262(10) Uani 1 1 d . . . C18 C 0.3354(3) 0.6874(2) 0.3525(3) 0.0275(10) Uani 1 1 d . . . C15 C 0.3900(3) 0.6773(2) 0.1957(3) 0.0261(10) Uani 1 1 d . . . H15A H 0.4090 0.6738 0.1424 0.031 Uiso 1 1 calc R . . C14 C 0.3061(3) 0.65494(18) 0.1955(3) 0.0219(10) Uani 1 1 d . . . C19 C 0.2411(3) 0.6266(2) 0.1107(3) 0.0264(10) Uani 1 1 d . . . H19A H 0.2146 0.5907 0.1313 0.032 Uiso 1 1 calc R . . C17 C 0.4188(3) 0.7094(2) 0.3492(3) 0.0288(11) Uani 1 1 d . . . H17A H 0.4576 0.7282 0.4016 0.035 Uiso 1 1 calc R . . C1 C 0.1241(3) 0.67162(19) 0.2692(3) 0.0235(10) Uani 1 1 d . . . C47 C -0.1010(3) 0.5259(2) 0.2046(3) 0.0281(11) Uani 1 1 d . . . C3 C 0.1604(4) 0.7848(2) 0.2675(3) 0.0330(11) Uani 1 1 d . . . H3A H 0.2233 0.7814 0.2720 0.040 Uiso 1 1 calc R . . C27 C 0.3047(3) 0.6406(2) -0.0241(3) 0.0342(12) Uani 1 1 d . . . H27A H 0.2753 0.6781 -0.0360 0.041 Uiso 1 1 calc R . . C10 C -0.1252(3) 0.6891(2) 0.2494(3) 0.0338(12) Uani 1 1 d . . . H10A H -0.1584 0.6534 0.2483 0.041 Uiso 1 1 calc R . . C48 C -0.1779(3) 0.4970(2) 0.2142(3) 0.0350(12) Uani 1 1 d . . . H48A H -0.2162 0.4766 0.1633 0.042 Uiso 1 1 calc R . . C9 C -0.1680(4) 0.7453(2) 0.2437(4) 0.0416(13) Uani 1 1 d . . . H9A H -0.2312 0.7467 0.2382 0.050 Uiso 1 1 calc R . . C7 C 0.0136(3) 0.7423(2) 0.2567(3) 0.0271(10) Uani 1 1 d . . . C42 C 0.6323(4) 0.6404(3) 0.0665(4) 0.0465(14) Uani 1 1 d . . . H42A H 0.6500 0.6199 0.0205 0.056 Uiso 1 1 calc R . . C49 C -0.2005(3) 0.4970(2) 0.2943(3) 0.0343(12) Uani 1 1 d . . . C26 C 0.2920(3) 0.6056(2) 0.0452(3) 0.0269(10) Uani 1 1 d . . . C32 C 0.5413(3) 0.7282(2) 0.2744(3) 0.0305(11) Uani 1 1 d . . . H32A H 0.5839 0.7164 0.3344 0.037 Uiso 1 1 calc R . . C29 C 0.4024(4) 0.5677(3) -0.0610(4) 0.0425(14) Uani 1 1 d . . . H29A H 0.4410 0.5554 -0.0960 0.051 Uiso 1 1 calc R . . C45 C 0.3093(3) 0.6914(2) 0.4403(3) 0.0345(12) Uani 1 1 d . . . H45A H 0.3579 0.7115 0.4867 0.052 Uiso 1 1 calc R . . H45B H 0.3006 0.6514 0.4612 0.052 Uiso 1 1 calc R . . H45C H 0.2525 0.7140 0.4296 0.052 Uiso 1 1 calc R . . C39 C 0.5766(3) 0.6987(2) 0.2002(3) 0.0293(11) Uani 1 1 d . . . C21 C 0.1731(3) 0.7289(2) 0.0642(3) 0.0330(12) Uani 1 1 d . . . H21A H 0.2317 0.7455 0.0905 0.040 Uiso 1 1 calc R . . C20 C 0.1615(3) 0.6680(2) 0.0661(3) 0.0283(11) Uani 1 1 d . . . C5 C 0.0284(4) 0.8477(2) 0.2571(3) 0.0361(12) Uani 1 1 d . . . H5A H 0.0038 0.8865 0.2553 0.043 Uiso 1 1 calc R . . C50 C -0.1451(3) 0.5269(2) 0.3685(3) 0.0330(12) Uani 1 1 d . . . H50A H -0.1614 0.5277 0.4235 0.040 Uiso 1 1 calc R . . C44 C 0.6153(4) 0.6427(2) 0.2162(4) 0.0408(13) Uani 1 1 d . . . H44A H 0.6230 0.6239 0.2732 0.049 Uiso 1 1 calc R . . C34 C 0.4745(4) 0.8296(2) 0.2163(4) 0.0476(15) Uani 1 1 d . . . H34A H 0.4179 0.8113 0.1865 0.057 Uiso 1 1 calc R . . C54 C -0.0846(4) 0.5291(2) 0.1128(3) 0.0389(13) Uani 1 1 d . . . H54A H -0.0940 0.4894 0.0841 0.047 Uiso 1 1 calc R . . H54B H -0.0206 0.5409 0.1205 0.047 Uiso 1 1 calc R . . C8 C -0.1228(4) 0.7972(2) 0.2458(3) 0.0404(13) Uani 1 1 d . . . H8A H -0.1547 0.8336 0.2429 0.048 Uiso 1 1 calc R . . C31 C 0.3340(3) 0.5506(2) 0.0591(3) 0.0354(12) Uani 1 1 d . . . H31A H 0.3258 0.5254 0.1057 0.043 Uiso 1 1 calc R . . C16 C 0.4473(3) 0.7048(2) 0.2719(3) 0.0282(11) Uani 1 1 d . . . C40 C 0.5671(3) 0.7253(2) 0.1167(3) 0.0350(12) Uani 1 1 d . . . H40A H 0.5405 0.7636 0.1048 0.042 Uiso 1 1 calc R . . C33 C 0.5451(4) 0.7952(2) 0.2693(3) 0.0362(12) Uani 1 1 d . . . C52 C -0.0049(4) 0.5877(2) 0.4448(3) 0.0414(13) Uani 1 1 d . . . H52A H -0.0024 0.6300 0.4281 0.050 Uiso 1 1 calc R . . H52B H 0.0573 0.5714 0.4562 0.050 Uiso 1 1 calc R . . C4 C 0.1189(4) 0.8406(2) 0.2643(3) 0.0366(12) Uani 1 1 d . . . H4A H 0.1553 0.8750 0.2673 0.044 Uiso 1 1 calc R . . C53 C -0.0300(4) 0.5850(3) 0.5333(3) 0.0452(14) Uani 1 1 d . . . H53A H 0.0151 0.6071 0.5805 0.068 Uiso 1 1 calc R . . H53B H -0.0308 0.5436 0.5522 0.068 Uiso 1 1 calc R . . H53C H -0.0904 0.6025 0.5243 0.068 Uiso 1 1 calc R . . C35 C 0.4847(5) 0.8901(3) 0.2057(5) 0.0594(18) Uani 1 1 d . . . H35A H 0.4362 0.9124 0.1671 0.071 Uiso 1 1 calc R . . C23 C 0.0159(4) 0.7416(3) -0.0130(4) 0.0540(16) Uani 1 1 d . . . H23A H -0.0343 0.7668 -0.0399 0.065 Uiso 1 1 calc R . . C30 C 0.3882(4) 0.5316(2) 0.0057(4) 0.0447(14) Uani 1 1 d . . . H30A H 0.4155 0.4934 0.0155 0.054 Uiso 1 1 calc R . . C38 C 0.6254(4) 0.8248(3) 0.3141(4) 0.0504(15) Uani 1 1 d . . . H38A H 0.6754 0.8031 0.3515 0.061 Uiso 1 1 calc R . . C41 C 0.5959(4) 0.6966(3) 0.0506(4) 0.0421(13) Uani 1 1 d . . . H41A H 0.5907 0.7157 -0.0058 0.051 Uiso 1 1 calc R . . C56 C -0.2850(4) 0.4660(3) 0.3023(4) 0.0519(16) Uani 1 1 d . . . H56A H -0.2893 0.4706 0.3643 0.078 Uiso 1 1 calc R . . H56B H -0.2817 0.4238 0.2886 0.078 Uiso 1 1 calc R . . H56C H -0.3388 0.4836 0.2591 0.078 Uiso 1 1 calc R . . C43 C 0.6424(4) 0.6146(3) 0.1489(4) 0.0501(15) Uani 1 1 d . . . H43A H 0.6689 0.5763 0.1603 0.060 Uiso 1 1 calc R . . C24 C 0.0036(4) 0.6817(3) -0.0121(4) 0.0557(17) Uani 1 1 d . . . H24A H -0.0552 0.6655 -0.0391 0.067 Uiso 1 1 calc R . . C36 C 0.5640(6) 0.9176(3) 0.2506(5) 0.068(2) Uani 1 1 d . . . H36A H 0.5707 0.9591 0.2438 0.082 Uiso 1 1 calc R . . C25 C 0.0761(4) 0.6442(3) 0.0280(3) 0.0417(13) Uani 1 1 d . . . H25A H 0.0668 0.6026 0.0291 0.050 Uiso 1 1 calc R . . C37 C 0.6327(5) 0.8858(3) 0.3045(5) 0.0664(19) Uani 1 1 d . . . H37A H 0.6874 0.9053 0.3367 0.080 Uiso 1 1 calc R . . C28 C 0.3594(4) 0.6221(3) -0.0762(3) 0.0409(13) Uani 1 1 d . . . H28A H 0.3674 0.6471 -0.1230 0.049 Uiso 1 1 calc R . . C22 C 0.1008(4) 0.7655(3) 0.0247(4) 0.0447(14) Uani 1 1 d . . . H22A H 0.1096 0.8072 0.0236 0.054 Uiso 1 1 calc R . . C55 C -0.1481(5) 0.5734(3) 0.0508(4) 0.0568(17) Uani 1 1 d . . . H55A H -0.1354 0.5747 -0.0080 0.085 Uiso 1 1 calc R . . H55B H -0.1384 0.6128 0.0788 0.085 Uiso 1 1 calc R . . H55C H -0.2114 0.5613 0.0418 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0320(4) 0.0250(4) 0.0389(4) 0.0028(3) 0.0174(3) 0.0005(3) N2 0.026(2) 0.024(2) 0.0233(19) 0.0007(16) 0.0106(17) -0.0043(17) Br1 0.0647(4) 0.0408(4) 0.0697(4) -0.0168(3) 0.0322(4) 0.0031(3) N1 0.026(2) 0.027(2) 0.024(2) 0.0006(16) 0.0103(17) -0.0035(17) Br2 0.0580(4) 0.0626(4) 0.0443(4) 0.0194(3) 0.0109(3) -0.0043(3) C46 0.027(2) 0.025(3) 0.027(2) -0.0013(19) 0.014(2) -0.003(2) C13 0.023(2) 0.022(2) 0.026(2) 0.0025(19) 0.009(2) 0.0032(19) C2 0.032(3) 0.027(3) 0.020(2) -0.0019(19) 0.013(2) -0.001(2) C6 0.041(3) 0.030(3) 0.023(2) 0.000(2) 0.006(2) 0.003(2) C11 0.030(3) 0.025(3) 0.028(2) -0.001(2) 0.012(2) -0.001(2) C51 0.022(2) 0.030(3) 0.028(2) -0.003(2) 0.008(2) -0.004(2) C12 0.029(3) 0.030(3) 0.023(2) -0.001(2) 0.013(2) -0.005(2) C18 0.027(3) 0.031(3) 0.027(2) -0.003(2) 0.011(2) 0.003(2) C15 0.024(2) 0.030(3) 0.026(2) -0.002(2) 0.009(2) -0.001(2) C14 0.030(3) 0.017(2) 0.022(2) -0.0007(18) 0.013(2) 0.0013(19) C19 0.031(3) 0.025(3) 0.023(2) -0.0014(19) 0.008(2) -0.006(2) C17 0.031(3) 0.036(3) 0.021(2) -0.004(2) 0.009(2) -0.005(2) C1 0.029(2) 0.024(2) 0.021(2) 0.0029(18) 0.012(2) 0.003(2) C47 0.029(3) 0.026(3) 0.031(3) -0.003(2) 0.012(2) 0.001(2) C3 0.037(3) 0.030(3) 0.035(3) 0.004(2) 0.014(2) -0.003(2) C27 0.039(3) 0.038(3) 0.028(3) -0.001(2) 0.012(2) 0.005(2) C10 0.026(3) 0.042(3) 0.036(3) -0.007(2) 0.012(2) -0.001(2) C48 0.033(3) 0.033(3) 0.036(3) -0.002(2) 0.006(2) -0.006(2) C9 0.029(3) 0.046(3) 0.051(3) 0.001(3) 0.013(3) 0.008(3) C7 0.032(3) 0.026(3) 0.026(2) 0.003(2) 0.013(2) 0.001(2) C42 0.040(3) 0.051(4) 0.055(4) -0.013(3) 0.024(3) 0.004(3) C49 0.032(3) 0.035(3) 0.035(3) 0.002(2) 0.009(2) -0.003(2) C26 0.025(2) 0.028(3) 0.027(2) -0.005(2) 0.006(2) -0.005(2) C32 0.027(3) 0.036(3) 0.029(2) -0.003(2) 0.008(2) -0.006(2) C29 0.031(3) 0.061(4) 0.034(3) -0.016(3) 0.005(2) 0.001(3) C45 0.036(3) 0.043(3) 0.029(3) -0.006(2) 0.016(2) -0.004(2) C39 0.021(2) 0.033(3) 0.036(3) -0.006(2) 0.013(2) -0.003(2) C21 0.033(3) 0.040(3) 0.027(2) 0.005(2) 0.009(2) 0.010(2) C20 0.033(3) 0.037(3) 0.018(2) 0.005(2) 0.012(2) 0.000(2) C5 0.056(4) 0.018(3) 0.035(3) -0.001(2) 0.016(3) 0.007(2) C50 0.035(3) 0.037(3) 0.029(3) -0.001(2) 0.011(2) -0.009(2) C44 0.042(3) 0.040(3) 0.042(3) 0.007(2) 0.015(3) 0.009(3) C34 0.045(3) 0.036(3) 0.072(4) -0.006(3) 0.033(3) -0.004(3) C54 0.042(3) 0.046(3) 0.032(3) -0.013(2) 0.017(3) -0.007(3) C8 0.037(3) 0.044(3) 0.039(3) 0.001(2) 0.009(3) 0.013(3) C31 0.038(3) 0.033(3) 0.039(3) 0.001(2) 0.017(3) 0.002(2) C16 0.025(3) 0.024(3) 0.037(3) 0.003(2) 0.012(2) -0.002(2) C40 0.031(3) 0.039(3) 0.037(3) 0.002(2) 0.012(2) 0.006(2) C33 0.035(3) 0.044(3) 0.036(3) -0.008(2) 0.021(2) -0.007(2) C52 0.047(3) 0.045(3) 0.038(3) -0.010(2) 0.023(3) -0.017(3) C4 0.049(3) 0.025(3) 0.038(3) 0.000(2) 0.017(3) -0.002(2) C53 0.053(4) 0.050(4) 0.037(3) -0.008(3) 0.021(3) -0.019(3) C35 0.065(4) 0.039(4) 0.090(5) 0.001(3) 0.048(4) 0.012(3) C23 0.038(3) 0.079(5) 0.047(3) 0.024(3) 0.016(3) 0.017(3) C30 0.033(3) 0.042(3) 0.056(4) -0.011(3) 0.008(3) 0.014(3) C38 0.048(4) 0.053(4) 0.049(3) -0.007(3) 0.013(3) -0.018(3) C41 0.044(3) 0.052(4) 0.036(3) 0.006(3) 0.021(3) 0.005(3) C56 0.042(3) 0.074(4) 0.036(3) -0.003(3) 0.006(3) -0.029(3) C43 0.055(4) 0.033(3) 0.067(4) 0.000(3) 0.025(3) 0.011(3) C24 0.021(3) 0.092(5) 0.050(4) 0.025(3) 0.006(3) -0.006(3) C36 0.089(6) 0.035(4) 0.091(5) -0.007(4) 0.043(5) -0.013(4) C25 0.034(3) 0.053(4) 0.038(3) 0.011(3) 0.010(3) -0.006(3) C37 0.068(5) 0.063(5) 0.071(5) -0.017(4) 0.024(4) -0.033(4) C28 0.044(3) 0.054(4) 0.028(3) -0.008(2) 0.014(2) -0.008(3) C22 0.052(4) 0.044(3) 0.043(3) 0.008(3) 0.020(3) 0.012(3) C55 0.076(5) 0.063(4) 0.034(3) -0.003(3) 0.020(3) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.018(4) . ? Ni1 N2 2.037(4) . ? Ni1 Br1 2.3232(9) . ? Ni1 Br2 2.3265(11) . ? N2 C1 1.283(6) . ? N2 C13 1.444(5) . ? N1 C12 1.287(6) . ? N1 C46 1.440(6) . ? C46 C47 1.391(6) . ? C46 C51 1.417(6) . ? C13 C18 1.389(6) . ? C13 C14 1.410(6) . ? C2 C3 1.382(6) . ? C2 C7 1.420(6) . ? C2 C1 1.448(6) . ? C6 C7 1.405(7) . ? C6 C5 1.411(7) . ? C6 C8 1.422(7) . ? C11 C10 1.374(6) . ? C11 C7 1.418(6) . ? C11 C12 1.459(6) . ? C51 C50 1.390(6) . ? C51 C52 1.499(7) . ? C12 C1 1.525(6) . ? C18 C17 1.389(6) . ? C18 C45 1.518(6) . ? C15 C14 1.383(6) . ? C15 C16 1.390(6) . ? C15 H15A 0.9500 . ? C14 C19 1.531(6) . ? C19 C26 1.520(6) . ? C19 C20 1.531(7) . ? C19 H19A 1.0000 . ? C17 C16 1.386(6) . ? C17 H17A 0.9500 . ? C47 C48 1.392(7) . ? C47 C54 1.508(6) . ? C3 C4 1.405(7) . ? C3 H3A 0.9500 . ? C27 C28 1.384(7) . ? C27 C26 1.386(6) . ? C27 H27A 0.9500 . ? C10 C9 1.419(7) . ? C10 H10A 0.9500 . ? C48 C49 1.375(7) . ? C48 H48A 0.9500 . ? C9 C8 1.355(8) . ? C9 H9A 0.9500 . ? C42 C43 1.362(8) . ? C42 C41 1.377(8) . ? C42 H42A 0.9500 . ? C49 C50 1.384(7) . ? C49 C56 1.508(7) . ? C26 C31 1.385(7) . ? C32 C33 1.515(7) . ? C32 C16 1.526(6) . ? C32 C39 1.549(6) . ? C32 H32A 1.0000 . ? C29 C30 1.376(8) . ? C29 C28 1.381(8) . ? C29 H29A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C39 C44 1.385(7) . ? C39 C40 1.386(7) . ? C21 C22 1.374(7) . ? C21 C20 1.385(7) . ? C21 H21A 0.9500 . ? C20 C25 1.381(7) . ? C5 C4 1.370(7) . ? C5 H5A 0.9500 . ? C50 H50A 0.9500 . ? C44 C43 1.378(7) . ? C44 H44A 0.9500 . ? C34 C33 1.388(8) . ? C34 C35 1.388(8) . ? C34 H34A 0.9500 . ? C54 C55 1.522(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C8 H8A 0.9500 . ? C31 C30 1.396(7) . ? C31 H31A 0.9500 . ? C40 C41 1.382(7) . ? C40 H40A 0.9500 . ? C33 C38 1.393(7) . ? C52 C53 1.520(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C4 H4A 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C35 C36 1.361(9) . ? C35 H35A 0.9500 . ? C23 C24 1.364(9) . ? C23 C22 1.373(8) . ? C23 H23A 0.9500 . ? C30 H30A 0.9500 . ? C38 C37 1.391(9) . ? C38 H38A 0.9500 . ? C41 H41A 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C43 H43A 0.9500 . ? C24 C25 1.391(8) . ? C24 H24A 0.9500 . ? C36 C37 1.344(10) . ? C36 H36A 0.9500 . ? C25 H25A 0.9500 . ? C37 H37A 0.9500 . ? C28 H28A 0.9500 . ? C22 H22A 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 82.50(15) . . ? N1 Ni1 Br1 109.68(11) . . ? N2 Ni1 Br1 124.26(10) . . ? N1 Ni1 Br2 112.71(11) . . ? N2 Ni1 Br2 102.21(10) . . ? Br1 Ni1 Br2 119.70(4) . . ? C1 N2 C13 119.7(4) . . ? C1 N2 Ni1 112.1(3) . . ? C13 N2 Ni1 128.0(3) . . ? C12 N1 C46 119.4(4) . . ? C12 N1 Ni1 112.1(3) . . ? C46 N1 Ni1 128.4(3) . . ? C47 C46 C51 122.1(4) . . ? C47 C46 N1 120.2(4) . . ? C51 C46 N1 117.6(4) . . ? C18 C13 C14 121.1(4) . . ? C18 C13 N2 120.8(4) . . ? C14 C13 N2 118.1(4) . . ? C3 C2 C7 118.8(4) . . ? C3 C2 C1 134.9(4) . . ? C7 C2 C1 106.3(4) . . ? C7 C6 C5 116.1(5) . . ? C7 C6 C8 115.9(5) . . ? C5 C6 C8 128.0(5) . . ? C10 C11 C7 120.0(4) . . ? C10 C11 C12 134.6(4) . . ? C7 C11 C12 105.4(4) . . ? C50 C51 C46 117.3(4) . . ? C50 C51 C52 122.5(4) . . ? C46 C51 C52 120.2(4) . . ? N1 C12 C11 135.4(4) . . ? N1 C12 C1 117.1(4) . . ? C11 C12 C1 107.5(4) . . ? C17 C18 C13 118.3(4) . . ? C17 C18 C45 119.8(4) . . ? C13 C18 C45 121.9(4) . . ? C14 C15 C16 121.7(4) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 C19 122.0(4) . . ? C13 C14 C19 119.6(4) . . ? C26 C19 C20 113.1(4) . . ? C26 C19 C14 111.2(4) . . ? C20 C19 C14 111.3(4) . . ? C26 C19 H19A 107.0 . . ? C20 C19 H19A 107.0 . . ? C14 C19 H19A 107.0 . . ? C16 C17 C18 122.0(4) . . ? C16 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? N2 C1 C2 137.3(4) . . ? N2 C1 C12 115.9(4) . . ? C2 C1 C12 106.8(4) . . ? C46 C47 C48 117.2(4) . . ? C46 C47 C54 122.5(4) . . ? C48 C47 C54 120.0(4) . . ? C2 C3 C4 118.1(5) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C28 C27 C26 121.3(5) . . ? C28 C27 H27A 119.4 . . ? C26 C27 H27A 119.4 . . ? C11 C10 C9 117.4(5) . . ? C11 C10 H10A 121.3 . . ? C9 C10 H10A 121.3 . . ? C49 C48 C47 122.6(5) . . ? C49 C48 H48A 118.7 . . ? C47 C48 H48A 118.7 . . ? C8 C9 C10 123.1(5) . . ? C8 C9 H9A 118.5 . . ? C10 C9 H9A 118.5 . . ? C6 C7 C11 122.6(4) . . ? C6 C7 C2 123.3(4) . . ? C11 C7 C2 114.1(4) . . ? C43 C42 C41 119.3(5) . . ? C43 C42 H42A 120.4 . . ? C41 C42 H42A 120.4 . . ? C48 C49 C50 118.9(5) . . ? C48 C49 C56 121.4(5) . . ? C50 C49 C56 119.7(5) . . ? C31 C26 C27 117.8(4) . . ? C31 C26 C19 119.0(4) . . ? C27 C26 C19 123.1(4) . . ? C33 C32 C16 113.2(4) . . ? C33 C32 C39 111.4(4) . . ? C16 C32 C39 111.4(4) . . ? C33 C32 H32A 106.8 . . ? C16 C32 H32A 106.8 . . ? C39 C32 H32A 106.8 . . ? C30 C29 C28 118.7(5) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C39 C40 118.8(4) . . ? C44 C39 C32 119.0(4) . . ? C40 C39 C32 122.1(4) . . ? C22 C21 C20 120.9(5) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C25 C20 C21 119.2(5) . . ? C25 C20 C19 119.2(4) . . ? C21 C20 C19 121.6(4) . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C49 C50 C51 121.9(5) . . ? C49 C50 H50A 119.1 . . ? C51 C50 H50A 119.1 . . ? C43 C44 C39 119.6(5) . . ? C43 C44 H44A 120.2 . . ? C39 C44 H44A 120.2 . . ? C33 C34 C35 121.5(6) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C47 C54 C55 111.5(4) . . ? C47 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C47 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? C9 C8 C6 121.0(5) . . ? C9 C8 H8A 119.5 . . ? C6 C8 H8A 119.5 . . ? C26 C31 C30 120.9(5) . . ? C26 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C17 C16 C15 118.5(4) . . ? C17 C16 C32 119.0(4) . . ? C15 C16 C32 122.4(4) . . ? C41 C40 C39 120.6(5) . . ? C41 C40 H40A 119.7 . . ? C39 C40 H40A 119.7 . . ? C34 C33 C38 116.7(5) . . ? C34 C33 C32 123.5(5) . . ? C38 C33 C32 119.6(5) . . ? C51 C52 C53 116.9(4) . . ? C51 C52 H52A 108.1 . . ? C53 C52 H52A 108.1 . . ? C51 C52 H52B 108.1 . . ? C53 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? C5 C4 C3 123.1(5) . . ? C5 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C36 C35 C34 120.3(7) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C24 C23 C22 120.2(6) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C29 C30 C31 120.5(5) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C37 C38 C33 120.5(6) . . ? C37 C38 H38A 119.7 . . ? C33 C38 H38A 119.7 . . ? C42 C41 C40 120.0(5) . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C49 C56 H56A 109.5 . . ? C49 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C49 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C42 C43 C44 121.7(5) . . ? C42 C43 H43A 119.2 . . ? C44 C43 H43A 119.2 . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C37 C36 C35 119.5(6) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C20 C25 C24 119.3(5) . . ? C20 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C36 C37 C38 121.4(6) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C29 C28 C27 120.7(5) . . ? C29 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C23 C22 C21 119.6(6) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 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 N1 Ni1 N2 C1 4.9(3) . . . . ? Br1 Ni1 N2 C1 113.7(3) . . . . ? Br2 Ni1 N2 C1 -106.8(3) . . . . ? N1 Ni1 N2 C13 -180.0(4) . . . . ? Br1 Ni1 N2 C13 -71.2(4) . . . . ? Br2 Ni1 N2 C13 68.3(3) . . . . ? N2 Ni1 N1 C12 -2.2(3) . . . . ? Br1 Ni1 N1 C12 -126.0(3) . . . . ? Br2 Ni1 N1 C12 98.0(3) . . . . ? N2 Ni1 N1 C46 -177.6(4) . . . . ? Br1 Ni1 N1 C46 58.6(4) . . . . ? Br2 Ni1 N1 C46 -77.4(4) . . . . ? C12 N1 C46 C47 100.6(5) . . . . ? Ni1 N1 C46 C47 -84.3(5) . . . . ? C12 N1 C46 C51 -80.0(5) . . . . ? Ni1 N1 C46 C51 95.1(5) . . . . ? C1 N2 C13 C18 77.1(5) . . . . ? Ni1 N2 C13 C18 -97.6(5) . . . . ? C1 N2 C13 C14 -106.0(5) . . . . ? Ni1 N2 C13 C14 79.2(5) . . . . ? C47 C46 C51 C50 -0.8(7) . . . . ? N1 C46 C51 C50 179.8(4) . . . . ? C47 C46 C51 C52 179.9(5) . . . . ? N1 C46 C51 C52 0.5(7) . . . . ? C46 N1 C12 C11 -0.8(8) . . . . ? Ni1 N1 C12 C11 -176.7(4) . . . . ? C46 N1 C12 C1 175.3(4) . . . . ? Ni1 N1 C12 C1 -0.5(5) . . . . ? C10 C11 C12 N1 -4.3(9) . . . . ? C7 C11 C12 N1 174.8(5) . . . . ? C10 C11 C12 C1 179.3(5) . . . . ? C7 C11 C12 C1 -1.6(5) . . . . ? C14 C13 C18 C17 2.4(7) . . . . ? N2 C13 C18 C17 179.1(4) . . . . ? C14 C13 C18 C45 -176.4(4) . . . . ? N2 C13 C18 C45 0.3(7) . . . . ? C16 C15 C14 C13 0.8(7) . . . . ? C16 C15 C14 C19 177.7(4) . . . . ? C18 C13 C14 C15 -2.1(7) . . . . ? N2 C13 C14 C15 -178.9(4) . . . . ? C18 C13 C14 C19 -179.1(4) . . . . ? N2 C13 C14 C19 4.1(6) . . . . ? C15 C14 C19 C26 21.8(6) . . . . ? C13 C14 C19 C26 -161.3(4) . . . . ? C15 C14 C19 C20 -105.2(5) . . . . ? C13 C14 C19 C20 71.7(5) . . . . ? C13 C18 C17 C16 -1.3(7) . . . . ? C45 C18 C17 C16 177.5(5) . . . . ? C13 N2 C1 C2 -1.4(8) . . . . ? Ni1 N2 C1 C2 174.1(4) . . . . ? C13 N2 C1 C12 178.0(4) . . . . ? Ni1 N2 C1 C12 -6.5(5) . . . . ? C3 C2 C1 N2 -3.9(9) . . . . ? C7 C2 C1 N2 178.4(5) . . . . ? C3 C2 C1 C12 176.7(5) . . . . ? C7 C2 C1 C12 -1.1(5) . . . . ? N1 C12 C1 N2 5.0(6) . . . . ? C11 C12 C1 N2 -177.9(4) . . . . ? N1 C12 C1 C2 -175.5(4) . . . . ? C11 C12 C1 C2 1.7(5) . . . . ? C51 C46 C47 C48 -0.2(7) . . . . ? N1 C46 C47 C48 179.1(4) . . . . ? C51 C46 C47 C54 174.5(5) . . . . ? N1 C46 C47 C54 -6.2(7) . . . . ? C7 C2 C3 C4 0.5(6) . . . . ? C1 C2 C3 C4 -177.0(5) . . . . ? C7 C11 C10 C9 -0.9(7) . . . . ? C12 C11 C10 C9 178.1(5) . . . . ? C46 C47 C48 C49 0.5(7) . . . . ? C54 C47 C48 C49 -174.3(5) . . . . ? C11 C10 C9 C8 -0.6(8) . . . . ? C5 C6 C7 C11 177.2(4) . . . . ? C8 C6 C7 C11 -1.0(7) . . . . ? C5 C6 C7 C2 -1.1(7) . . . . ? C8 C6 C7 C2 -179.4(4) . . . . ? C10 C11 C7 C6 1.7(7) . . . . ? C12 C11 C7 C6 -177.5(4) . . . . ? C10 C11 C7 C2 -179.8(4) . . . . ? C12 C11 C7 C2 1.0(5) . . . . ? C3 C2 C7 C6 0.4(7) . . . . ? C1 C2 C7 C6 178.6(4) . . . . ? C3 C2 C7 C11 -178.1(4) . . . . ? C1 C2 C7 C11 0.1(5) . . . . ? C47 C48 C49 C50 0.3(8) . . . . ? C47 C48 C49 C56 179.2(5) . . . . ? C28 C27 C26 C31 -1.7(7) . . . . ? C28 C27 C26 C19 173.2(4) . . . . ? C20 C19 C26 C31 -150.3(4) . . . . ? C14 C19 C26 C31 83.6(5) . . . . ? C20 C19 C26 C27 34.8(6) . . . . ? C14 C19 C26 C27 -91.3(5) . . . . ? C33 C32 C39 C44 152.0(5) . . . . ? C16 C32 C39 C44 -80.6(6) . . . . ? C33 C32 C39 C40 -30.9(6) . . . . ? C16 C32 C39 C40 96.5(5) . . . . ? C22 C21 C20 C25 -0.2(7) . . . . ? C22 C21 C20 C19 -179.3(4) . . . . ? C26 C19 C20 C25 91.1(5) . . . . ? C14 C19 C20 C25 -143.0(4) . . . . ? C26 C19 C20 C21 -89.8(5) . . . . ? C14 C19 C20 C21 36.2(6) . . . . ? C7 C6 C5 C4 1.0(7) . . . . ? C8 C6 C5 C4 179.1(5) . . . . ? C48 C49 C50 C51 -1.4(8) . . . . ? C56 C49 C50 C51 179.7(5) . . . . ? C46 C51 C50 C49 1.7(7) . . . . ? C52 C51 C50 C49 -179.0(5) . . . . ? C40 C39 C44 C43 -0.7(8) . . . . ? C32 C39 C44 C43 176.5(5) . . . . ? C46 C47 C54 C55 -100.3(6) . . . . ? C48 C47 C54 C55 74.2(6) . . . . ? C10 C9 C8 C6 1.2(8) . . . . ? C7 C6 C8 C9 -0.4(7) . . . . ? C5 C6 C8 C9 -178.5(5) . . . . ? C27 C26 C31 C30 0.8(7) . . . . ? C19 C26 C31 C30 -174.3(5) . . . . ? C18 C17 C16 C15 0.0(7) . . . . ? C18 C17 C16 C32 -178.0(4) . . . . ? C14 C15 C16 C17 0.2(7) . . . . ? C14 C15 C16 C32 178.2(4) . . . . ? C33 C32 C16 C17 -75.9(6) . . . . ? C39 C32 C16 C17 157.7(4) . . . . ? C33 C32 C16 C15 106.1(5) . . . . ? C39 C32 C16 C15 -20.3(6) . . . . ? C44 C39 C40 C41 -0.2(7) . . . . ? C32 C39 C40 C41 -177.3(5) . . . . ? C35 C34 C33 C38 2.4(8) . . . . ? C35 C34 C33 C32 -172.7(5) . . . . ? C16 C32 C33 C34 -37.3(6) . . . . ? C39 C32 C33 C34 89.1(6) . . . . ? C16 C32 C33 C38 147.8(5) . . . . ? C39 C32 C33 C38 -85.8(6) . . . . ? C50 C51 C52 C53 2.6(8) . . . . ? C46 C51 C52 C53 -178.1(5) . . . . ? C6 C5 C4 C3 -0.2(8) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C33 C34 C35 C36 -2.6(9) . . . . ? C28 C29 C30 C31 -2.3(8) . . . . ? C26 C31 C30 C29 1.2(8) . . . . ? C34 C33 C38 C37 -0.4(8) . . . . ? C32 C33 C38 C37 174.8(5) . . . . ? C43 C42 C41 C40 -2.5(9) . . . . ? C39 C40 C41 C42 1.8(8) . . . . ? C41 C42 C43 C44 1.6(9) . . . . ? C39 C44 C43 C42 0.0(9) . . . . ? C22 C23 C24 C25 0.9(9) . . . . ? C34 C35 C36 C37 0.7(10) . . . . ? C21 C20 C25 C24 0.5(7) . . . . ? C19 C20 C25 C24 179.6(5) . . . . ? C23 C24 C25 C20 -0.8(8) . . . . ? C35 C36 C37 C38 1.3(11) . . . . ? C33 C38 C37 C36 -1.5(10) . . . . ? C30 C29 C28 C27 1.4(8) . . . . ? C26 C27 C28 C29 0.6(8) . . . . ? C24 C23 C22 C21 -0.6(8) . . . . ? C20 C21 C22 C23 0.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.679 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.116 # 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 0.500 0.500 446.5 79.1 2 0.500 0.000 1.000 446.4 79.1 3 0.262 0.847 0.113 9.3 0.3 4 0.262 0.653 0.613 9.3 0.1 5 0.738 0.347 0.387 9.4 0.2 6 0.738 0.153 0.887 9.4 0.1 _platon_squeeze_details ; ? ; #==END data_C9 _database_code_depnum_ccdc_archive 'CCDC 831467' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 Cl2 N2 Ni O0' _chemical_formula_weight 850.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.330(3) _cell_length_b 22.285(5) _cell_length_c 14.954(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.33(3) _cell_angle_gamma 90.00 _cell_volume 4902.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13624 _cell_measurement_theta_min 1.4189 _cell_measurement_theta_max 27.4617 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8905 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details ? _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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 39551 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11189 _reflns_number_gt 7858 _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^)+(0.1207P)^2^+13.1397P] 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 11189 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1619 _refine_ls_R_factor_gt 0.1173 _refine_ls_wR_factor_ref 0.3059 _refine_ls_wR_factor_gt 0.2780 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33892(5) 0.45517(3) 0.71902(6) 0.0308(2) Uani 1 1 d . . . Cl2 Cl 0.26418(14) 0.47246(9) 0.57237(13) 0.0525(5) Uani 1 1 d . . . Cl1 Cl 0.35125(12) 0.51975(8) 0.83364(14) 0.0480(5) Uani 1 1 d . . . N2 N 0.3067(3) 0.3673(2) 0.7335(3) 0.0264(10) Uani 1 1 d . . . N1 N 0.4623(3) 0.4197(2) 0.7284(3) 0.0277(11) Uani 1 1 d . . . C7 C 0.4853(4) 0.2598(2) 0.7546(4) 0.0262(12) Uani 1 1 d . . . C2 C 0.3930(4) 0.2672(3) 0.7476(4) 0.0287(12) Uani 1 1 d . . . C12 C 0.4633(4) 0.3616(3) 0.7409(3) 0.0235(11) Uani 1 1 d . . . C11 C 0.5334(4) 0.3154(2) 0.7513(4) 0.0256(12) Uani 1 1 d . . . C46 C 0.5427(4) 0.4507(3) 0.7180(4) 0.0275(12) Uani 1 1 d . . . C19 C 0.2563(4) 0.3779(3) 0.9023(4) 0.0268(12) Uani 1 1 d . . . H19A H 0.2790 0.4154 0.8800 0.032 Uiso 1 1 calc R . . C1 C 0.3756(4) 0.3329(2) 0.7410(3) 0.0205(11) Uani 1 1 d . . . C16 C 0.0507(4) 0.2967(2) 0.7350(4) 0.0252(12) Uani 1 1 d . . . C50 C 0.6793(4) 0.5061(3) 0.7830(4) 0.0303(13) Uani 1 1 d . . . H50A H 0.7203 0.5259 0.8340 0.036 Uiso 1 1 calc R . . C13 C 0.2205(3) 0.3418(3) 0.7340(4) 0.0248(12) Uani 1 1 d . . . C17 C 0.0809(4) 0.2928(3) 0.6568(4) 0.0238(11) Uani 1 1 d . . . H17A H 0.0431 0.2737 0.6029 0.029 Uiso 1 1 calc R . . C48 C 0.6358(4) 0.4786(3) 0.6226(5) 0.0343(14) Uani 1 1 d . . . H48A H 0.6475 0.4791 0.5634 0.041 Uiso 1 1 calc R . . C20 C 0.3392(4) 0.3389(3) 0.9462(4) 0.0291(13) Uani 1 1 d . . . C45 C 0.1916(4) 0.3142(3) 0.5631(4) 0.0333(14) Uani 1 1 d . . . H45A H 0.1442 0.2938 0.5149 0.050 Uiso 1 1 calc R . . H45B H 0.2492 0.2926 0.5731 0.050 Uiso 1 1 calc R . . H45C H 0.1987 0.3554 0.5430 0.050 Uiso 1 1 calc R . . C14 C 0.1932(3) 0.3467(2) 0.8159(4) 0.0214(11) Uani 1 1 d . . . C26 C 0.2034(4) 0.3965(3) 0.9690(4) 0.0260(12) Uani 1 1 d . . . C47 C 0.5584(4) 0.4500(3) 0.6316(4) 0.0290(12) Uani 1 1 d . . . C34 C -0.1324(5) 0.1774(3) 0.6957(5) 0.0392(15) Uani 1 1 d . . . H34A H -0.1817 0.2010 0.6604 0.047 Uiso 1 1 calc R . . C18 C 0.1647(4) 0.3157(3) 0.6532(4) 0.0283(12) Uani 1 1 d . . . C6 C 0.5302(5) 0.2041(3) 0.7632(4) 0.0351(14) Uani 1 1 d . . . C33 C -0.0501(4) 0.2046(3) 0.7376(4) 0.0280(12) Uani 1 1 d . . . C31 C 0.1628(4) 0.4517(3) 0.9592(4) 0.0322(13) Uani 1 1 d . . . H31A H 0.1733 0.4787 0.9142 0.039 Uiso 1 1 calc R . . C49 C 0.6971(4) 0.5068(3) 0.6978(5) 0.0323(14) Uani 1 1 d . . . C27 C 0.1900(4) 0.3588(3) 1.0386(4) 0.0313(13) Uani 1 1 d . . . H27A H 0.2210 0.3214 1.0499 0.038 Uiso 1 1 calc R . . C54 C 0.7811(5) 0.5366(3) 0.6836(6) 0.0484(18) Uani 1 1 d . . . H54A H 0.8166 0.5546 0.7424 0.073 Uiso 1 1 calc R . . H54B H 0.7629 0.5679 0.6360 0.073 Uiso 1 1 calc R . . H54C H 0.8182 0.5065 0.6634 0.073 Uiso 1 1 calc R . . C9 C 0.6686(4) 0.2579(3) 0.7653(5) 0.0410(16) Uani 1 1 d . . . H9A H 0.7313 0.2569 0.7682 0.049 Uiso 1 1 calc R . . C43 C -0.1530(5) 0.3882(3) 0.8542(5) 0.0406(16) Uani 1 1 d . . . H43A H -0.1799 0.4268 0.8409 0.049 Uiso 1 1 calc R . . C3 C 0.3394(4) 0.2173(3) 0.7463(5) 0.0338(14) Uani 1 1 d . . . H3A H 0.2761 0.2208 0.7398 0.041 Uiso 1 1 calc R . . C42 C -0.1463(4) 0.3618(3) 0.9405(4) 0.0369(15) Uani 1 1 d . . . H42A H -0.1684 0.3819 0.9858 0.044 Uiso 1 1 calc R . . C15 C 0.1083(4) 0.3242(2) 0.8156(4) 0.0266(12) Uani 1 1 d . . . H15A H 0.0887 0.3274 0.8703 0.032 Uiso 1 1 calc R . . C40 C -0.0743(4) 0.2766(3) 0.8926(4) 0.0336(14) Uani 1 1 d . . . H40A H -0.0480 0.2379 0.9064 0.040 Uiso 1 1 calc R . . C32 C -0.0437(4) 0.2732(3) 0.7325(4) 0.0242(11) Uani 1 1 d . . . H32A H -0.0854 0.2855 0.6709 0.029 Uiso 1 1 calc R . . C51 C 0.6032(4) 0.4772(3) 0.7978(4) 0.0292(13) Uani 1 1 d . . . C39 C -0.0799(3) 0.3030(2) 0.8073(4) 0.0242(11) Uani 1 1 d . . . C30 C 0.1064(4) 0.4697(3) 1.0130(5) 0.0380(15) Uani 1 1 d . . . H30A H 0.0794 0.5085 1.0050 0.046 Uiso 1 1 calc R . . C29 C 0.0906(4) 0.4303(3) 1.0783(5) 0.0411(16) Uani 1 1 d . . . H29A H 0.0507 0.4415 1.1139 0.049 Uiso 1 1 calc R . . C10 C 0.6234(4) 0.3142(3) 0.7567(4) 0.0329(14) Uani 1 1 d . . . H10A H 0.6555 0.3503 0.7548 0.039 Uiso 1 1 calc R . . C52 C 0.5897(5) 0.4735(3) 0.8921(5) 0.0427(16) Uani 1 1 d . . . H52A H 0.6394 0.4945 0.9368 0.064 Uiso 1 1 calc R . . H52B H 0.5892 0.4313 0.9104 0.064 Uiso 1 1 calc R . . H52C H 0.5317 0.4923 0.8913 0.064 Uiso 1 1 calc R . . C38 C 0.0216(4) 0.1691(3) 0.7892(5) 0.0341(14) Uani 1 1 d . . . H38A H 0.0792 0.1869 0.8167 0.041 Uiso 1 1 calc R . . C37 C 0.0092(5) 0.1083(3) 0.8005(6) 0.0453(17) Uani 1 1 d . . . H37A H 0.0575 0.0848 0.8380 0.054 Uiso 1 1 calc R . . C36 C -0.0732(6) 0.0817(3) 0.7576(6) 0.052(2) Uani 1 1 d . . . H36A H -0.0813 0.0399 0.7645 0.062 Uiso 1 1 calc R . . C8 C 0.6240(4) 0.2048(3) 0.7697(5) 0.0382(15) Uani 1 1 d . . . H8A H 0.6568 0.1681 0.7772 0.046 Uiso 1 1 calc R . . C44 C -0.1211(4) 0.3592(3) 0.7874(4) 0.0333(14) Uani 1 1 d . . . H44A H -0.1272 0.3775 0.7285 0.040 Uiso 1 1 calc R . . C25 C 0.4243(4) 0.3663(3) 0.9808(4) 0.0356(15) Uani 1 1 d . . . H25A H 0.4296 0.4086 0.9773 0.043 Uiso 1 1 calc R . . C21 C 0.3341(4) 0.2772(3) 0.9508(4) 0.0332(14) Uani 1 1 d . . . H21A H 0.2769 0.2581 0.9262 0.040 Uiso 1 1 calc R . . C35 C -0.1441(6) 0.1161(3) 0.7044(5) 0.0479(18) Uani 1 1 d . . . H35A H -0.2007 0.0978 0.6739 0.057 Uiso 1 1 calc R . . C28 C 0.1321(4) 0.3749(3) 1.0920(4) 0.0364(15) Uani 1 1 d . . . H28A H 0.1215 0.3480 1.1371 0.044 Uiso 1 1 calc R . . C41 C -0.1071(4) 0.3064(3) 0.9581(5) 0.0386(15) Uani 1 1 d . . . H41A H -0.1022 0.2878 1.0165 0.046 Uiso 1 1 calc R . . C22 C 0.4107(5) 0.2421(4) 0.9905(5) 0.0463(18) Uani 1 1 d . . . H22A H 0.4056 0.1997 0.9939 0.056 Uiso 1 1 calc R . . C4 C 0.3821(5) 0.1609(3) 0.7549(5) 0.0433(16) Uani 1 1 d . . . H4A H 0.3466 0.1260 0.7553 0.052 Uiso 1 1 calc R . . C23 C 0.4940(5) 0.2700(4) 1.0249(5) 0.055(2) Uani 1 1 d . . . H23A H 0.5468 0.2468 1.0519 0.066 Uiso 1 1 calc R . . C53 C 0.4958(4) 0.4174(3) 0.5490(5) 0.0382(15) Uani 1 1 d . . . H53A H 0.4445 0.4002 0.5673 0.057 Uiso 1 1 calc R . . H53B H 0.5295 0.3852 0.5289 0.057 Uiso 1 1 calc R . . H53C H 0.4729 0.4457 0.4976 0.057 Uiso 1 1 calc R . . C5 C 0.4740(5) 0.1540(3) 0.7630(5) 0.0453(17) Uani 1 1 d . . . H5A H 0.4994 0.1148 0.7685 0.054 Uiso 1 1 calc R . . C24 C 0.5004(5) 0.3320(4) 1.0199(5) 0.052(2) Uani 1 1 d . . . H24A H 0.5577 0.3510 1.0436 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0293(4) 0.0255(4) 0.0410(5) 0.0029(3) 0.0157(3) 0.0005(3) Cl2 0.0558(11) 0.0557(12) 0.0450(11) 0.0164(9) 0.0126(8) 0.0054(9) Cl1 0.0488(10) 0.0384(10) 0.0580(11) -0.0106(8) 0.0169(8) 0.0057(7) N2 0.025(2) 0.028(3) 0.027(3) 0.001(2) 0.0086(19) -0.0027(19) N1 0.021(2) 0.030(3) 0.032(3) -0.003(2) 0.007(2) -0.0085(19) C7 0.030(3) 0.021(3) 0.026(3) 0.001(2) 0.005(2) 0.009(2) C2 0.029(3) 0.030(3) 0.027(3) 0.002(2) 0.007(2) 0.004(2) C12 0.033(3) 0.026(3) 0.010(2) 0.005(2) 0.003(2) 0.001(2) C11 0.031(3) 0.015(3) 0.031(3) 0.005(2) 0.011(2) -0.001(2) C46 0.026(3) 0.025(3) 0.032(3) 0.004(2) 0.009(2) -0.005(2) C19 0.026(3) 0.026(3) 0.026(3) -0.004(2) 0.005(2) -0.003(2) C1 0.030(3) 0.020(3) 0.013(2) -0.006(2) 0.007(2) -0.008(2) C16 0.024(3) 0.021(3) 0.033(3) 0.002(2) 0.011(2) 0.002(2) C50 0.031(3) 0.028(3) 0.034(3) -0.003(3) 0.012(3) -0.002(2) C13 0.018(2) 0.027(3) 0.029(3) 0.005(2) 0.006(2) -0.001(2) C17 0.023(3) 0.028(3) 0.019(3) -0.003(2) 0.003(2) -0.003(2) C48 0.034(3) 0.034(3) 0.040(4) -0.002(3) 0.018(3) -0.007(3) C20 0.038(3) 0.029(3) 0.024(3) -0.003(2) 0.013(2) 0.000(2) C45 0.033(3) 0.045(4) 0.023(3) -0.005(3) 0.009(2) -0.003(3) C14 0.020(2) 0.018(3) 0.028(3) 0.001(2) 0.010(2) 0.000(2) C26 0.025(3) 0.034(3) 0.020(3) 0.003(2) 0.007(2) 0.004(2) C47 0.032(3) 0.028(3) 0.028(3) 0.002(2) 0.009(2) -0.006(2) C34 0.042(4) 0.038(4) 0.042(4) -0.007(3) 0.019(3) -0.014(3) C18 0.031(3) 0.032(3) 0.025(3) 0.004(2) 0.012(2) 0.004(2) C6 0.045(4) 0.030(3) 0.030(3) 0.007(3) 0.009(3) 0.004(3) C33 0.022(3) 0.033(3) 0.034(3) -0.007(3) 0.016(2) -0.008(2) C31 0.038(3) 0.027(3) 0.031(3) 0.004(3) 0.009(3) 0.004(3) C49 0.032(3) 0.022(3) 0.045(4) 0.004(3) 0.015(3) -0.006(2) C27 0.038(3) 0.028(3) 0.030(3) -0.002(3) 0.012(3) 0.000(3) C54 0.042(4) 0.054(5) 0.053(5) -0.010(4) 0.021(3) -0.019(3) C9 0.029(3) 0.045(4) 0.052(4) 0.008(3) 0.018(3) 0.005(3) C43 0.043(4) 0.032(4) 0.046(4) -0.005(3) 0.011(3) 0.007(3) C3 0.036(3) 0.023(3) 0.046(4) -0.006(3) 0.017(3) -0.009(2) C42 0.041(4) 0.040(4) 0.032(3) -0.008(3) 0.014(3) 0.000(3) C15 0.031(3) 0.020(3) 0.027(3) 0.004(2) 0.005(2) 0.003(2) C40 0.038(3) 0.030(3) 0.034(3) 0.004(3) 0.012(3) 0.012(3) C32 0.023(3) 0.033(3) 0.019(3) 0.002(2) 0.009(2) -0.003(2) C51 0.031(3) 0.029(3) 0.029(3) -0.010(2) 0.011(2) -0.008(2) C39 0.020(2) 0.024(3) 0.026(3) -0.003(2) 0.002(2) -0.001(2) C30 0.030(3) 0.031(4) 0.051(4) -0.009(3) 0.007(3) 0.006(3) C29 0.031(3) 0.058(5) 0.033(4) -0.007(3) 0.007(3) 0.002(3) C10 0.028(3) 0.036(4) 0.030(3) 0.003(3) 0.001(2) 0.004(3) C52 0.036(3) 0.057(4) 0.039(4) -0.012(3) 0.015(3) -0.012(3) C38 0.031(3) 0.035(4) 0.041(4) 0.000(3) 0.020(3) -0.001(3) C37 0.050(4) 0.031(4) 0.064(5) 0.004(3) 0.032(4) 0.006(3) C36 0.078(6) 0.032(4) 0.059(5) -0.009(3) 0.042(4) -0.006(4) C8 0.031(3) 0.040(4) 0.043(4) 0.007(3) 0.009(3) 0.021(3) C44 0.030(3) 0.037(4) 0.032(3) 0.000(3) 0.007(3) 0.002(3) C25 0.021(3) 0.053(4) 0.030(3) 0.002(3) 0.002(2) -0.007(3) C21 0.042(3) 0.038(4) 0.021(3) 0.002(3) 0.012(3) 0.010(3) C35 0.061(5) 0.042(4) 0.044(4) -0.005(3) 0.021(4) -0.017(4) C28 0.039(3) 0.046(4) 0.026(3) 0.000(3) 0.012(3) -0.004(3) C41 0.036(3) 0.051(4) 0.031(3) 0.003(3) 0.015(3) 0.009(3) C22 0.058(5) 0.052(5) 0.032(4) 0.011(3) 0.018(3) 0.013(4) C4 0.055(4) 0.029(4) 0.047(4) 0.000(3) 0.015(3) -0.005(3) C23 0.039(4) 0.081(6) 0.044(4) 0.021(4) 0.010(3) 0.021(4) C53 0.027(3) 0.048(4) 0.037(4) -0.007(3) 0.006(3) -0.008(3) C5 0.061(5) 0.021(3) 0.057(5) 0.008(3) 0.023(4) 0.006(3) C24 0.030(3) 0.079(6) 0.040(4) 0.010(4) 0.000(3) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.018(5) . ? Ni1 N2 2.046(5) . ? Ni1 Cl2 2.204(2) . ? Ni1 Cl1 2.205(2) . ? N2 C1 1.284(7) . ? N2 C13 1.442(7) . ? N1 C12 1.308(7) . ? N1 C46 1.459(7) . ? C7 C2 1.399(8) . ? C7 C6 1.408(8) . ? C7 C11 1.449(8) . ? C2 C3 1.379(8) . ? C2 C1 1.488(8) . ? C12 C11 1.465(8) . ? C12 C1 1.489(7) . ? C11 C10 1.359(8) . ? C46 C47 1.380(8) . ? C46 C51 1.417(8) . ? C19 C26 1.510(8) . ? C19 C20 1.527(8) . ? C19 C14 1.544(8) . ? C19 H19A 1.0000 . ? C16 C17 1.377(8) . ? C16 C15 1.418(8) . ? C16 C32 1.530(7) . ? C50 C49 1.377(9) . ? C50 C51 1.403(8) . ? C50 H50A 0.9500 . ? C13 C18 1.396(8) . ? C13 C14 1.405(8) . ? C17 C18 1.398(8) . ? C17 H17A 0.9500 . ? C48 C47 1.388(8) . ? C48 C49 1.395(9) . ? C48 H48A 0.9500 . ? C20 C21 1.380(9) . ? C20 C25 1.399(8) . ? C45 C18 1.517(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C14 C15 1.393(7) . ? C26 C31 1.367(8) . ? C26 C27 1.398(8) . ? C47 C53 1.519(8) . ? C34 C33 1.380(8) . ? C34 C35 1.391(10) . ? C34 H34A 0.9500 . ? C6 C5 1.411(9) . ? C6 C8 1.413(9) . ? C33 C38 1.396(9) . ? C33 C32 1.536(8) . ? C31 C30 1.395(9) . ? C31 H31A 0.9500 . ? C49 C54 1.516(8) . ? C27 C28 1.398(8) . ? C27 H27A 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C9 C8 1.376(10) . ? C9 C10 1.421(9) . ? C9 H9A 0.9500 . ? C43 C44 1.390(9) . ? C43 C42 1.395(10) . ? C43 H43A 0.9500 . ? C3 C4 1.406(9) . ? C3 H3A 0.9500 . ? C42 C41 1.367(9) . ? C42 H42A 0.9500 . ? C15 H15A 0.9500 . ? C40 C39 1.386(8) . ? C40 C41 1.389(8) . ? C40 H40A 0.9500 . ? C32 C39 1.532(8) . ? C32 H32A 1.0000 . ? C51 C52 1.483(9) . ? C39 C44 1.397(8) . ? C30 C29 1.386(10) . ? C30 H30A 0.9500 . ? C29 C28 1.377(10) . ? C29 H29A 0.9500 . ? C10 H10A 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C38 C37 1.387(9) . ? C38 H38A 0.9500 . ? C37 C36 1.379(11) . ? C37 H37A 0.9500 . ? C36 C35 1.383(11) . ? C36 H36A 0.9500 . ? C8 H8A 0.9500 . ? C44 H44A 0.9500 . ? C25 C24 1.379(9) . ? C25 H25A 0.9500 . ? C21 C22 1.398(9) . ? C21 H21A 0.9500 . ? C35 H35A 0.9500 . ? C28 H28A 0.9500 . ? C41 H41A 0.9500 . ? C22 C23 1.383(11) . ? C22 H22A 0.9500 . ? C4 C5 1.388(10) . ? C4 H4A 0.9500 . ? C23 C24 1.389(12) . ? C23 H23A 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C5 H5A 0.9500 . ? C24 H24A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 82.34(19) . . ? N1 Ni1 Cl2 110.63(15) . . ? N2 Ni1 Cl2 101.48(15) . . ? N1 Ni1 Cl1 109.14(15) . . ? N2 Ni1 Cl1 120.88(15) . . ? Cl2 Ni1 Cl1 124.49(8) . . ? C1 N2 C13 119.9(5) . . ? C1 N2 Ni1 111.3(4) . . ? C13 N2 Ni1 128.8(4) . . ? C12 N1 C46 120.5(5) . . ? C12 N1 Ni1 111.8(4) . . ? C46 N1 Ni1 127.6(4) . . ? C2 C7 C6 124.7(6) . . ? C2 C7 C11 114.3(5) . . ? C6 C7 C11 121.1(5) . . ? C3 C2 C7 119.5(5) . . ? C3 C2 C1 134.3(5) . . ? C7 C2 C1 106.1(5) . . ? N1 C12 C11 133.7(5) . . ? N1 C12 C1 116.8(5) . . ? C11 C12 C1 109.5(5) . . ? C10 C11 C7 119.9(5) . . ? C10 C11 C12 136.2(5) . . ? C7 C11 C12 103.9(5) . . ? C47 C46 C51 123.2(5) . . ? C47 C46 N1 118.0(5) . . ? C51 C46 N1 118.7(5) . . ? C26 C19 C20 114.2(5) . . ? C26 C19 C14 110.5(4) . . ? C20 C19 C14 110.7(5) . . ? C26 C19 H19A 107.0 . . ? C20 C19 H19A 107.0 . . ? C14 C19 H19A 107.0 . . ? N2 C1 C2 136.1(5) . . ? N2 C1 C12 117.7(5) . . ? C2 C1 C12 106.2(5) . . ? C17 C16 C15 118.2(5) . . ? C17 C16 C32 119.9(5) . . ? C15 C16 C32 121.9(5) . . ? C49 C50 C51 122.7(6) . . ? C49 C50 H50A 118.6 . . ? C51 C50 H50A 118.6 . . ? C18 C13 C14 121.8(5) . . ? C18 C13 N2 119.9(5) . . ? C14 C13 N2 118.2(5) . . ? C16 C17 C18 122.8(5) . . ? C16 C17 H17A 118.6 . . ? C18 C17 H17A 118.6 . . ? C47 C48 C49 121.9(6) . . ? C47 C48 H48A 119.0 . . ? C49 C48 H48A 119.1 . . ? C21 C20 C25 118.4(6) . . ? C21 C20 C19 122.3(5) . . ? C25 C20 C19 119.2(5) . . ? C18 C45 H45A 109.5 . . ? C18 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C18 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C15 C14 C13 118.4(5) . . ? C15 C14 C19 121.9(5) . . ? C13 C14 C19 119.6(5) . . ? C31 C26 C27 117.6(5) . . ? C31 C26 C19 119.3(5) . . ? C27 C26 C19 123.0(5) . . ? C46 C47 C48 117.7(6) . . ? C46 C47 C53 122.0(5) . . ? C48 C47 C53 120.2(5) . . ? C33 C34 C35 121.0(7) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C13 C18 C17 117.7(5) . . ? C13 C18 C45 121.7(5) . . ? C17 C18 C45 120.6(5) . . ? C7 C6 C5 114.5(6) . . ? C7 C6 C8 117.3(6) . . ? C5 C6 C8 128.2(6) . . ? C34 C33 C38 118.6(6) . . ? C34 C33 C32 118.5(6) . . ? C38 C33 C32 122.6(5) . . ? C26 C31 C30 122.3(6) . . ? C26 C31 H31A 118.8 . . ? C30 C31 H31A 118.8 . . ? C50 C49 C48 118.5(5) . . ? C50 C49 C54 122.1(6) . . ? C48 C49 C54 119.3(6) . . ? C26 C27 C28 121.3(6) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C8 C9 C10 121.8(6) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C44 C43 C42 121.3(6) . . ? C44 C43 H43A 119.3 . . ? C42 C43 H43A 119.3 . . ? C2 C3 C4 117.3(6) . . ? C2 C3 H3A 121.4 . . ? C4 C3 H3A 121.4 . . ? C41 C42 C43 118.3(6) . . ? C41 C42 H42A 120.9 . . ? C43 C42 H42A 120.9 . . ? C14 C15 C16 121.1(5) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C39 C40 C41 120.3(6) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C16 C32 C39 111.6(5) . . ? C16 C32 C33 114.3(5) . . ? C39 C32 C33 110.7(4) . . ? C16 C32 H32A 106.5 . . ? C39 C32 H32A 106.5 . . ? C33 C32 H32A 106.5 . . ? C50 C51 C46 115.8(5) . . ? C50 C51 C52 121.2(5) . . ? C46 C51 C52 123.0(5) . . ? C40 C39 C44 119.0(5) . . ? C40 C39 C32 123.1(5) . . ? C44 C39 C32 117.8(5) . . ? C29 C30 C31 118.9(6) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? C28 C29 C30 120.6(6) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C11 C10 C9 118.9(6) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C37 C38 C33 120.5(6) . . ? C37 C38 H38A 119.8 . . ? C33 C38 H38A 119.8 . . ? C36 C37 C38 120.1(7) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C37 C36 C35 119.9(7) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C9 C8 C6 121.0(6) . . ? C9 C8 H8A 119.5 . . ? C6 C8 H8A 119.5 . . ? C43 C44 C39 119.5(6) . . ? C43 C44 H44A 120.2 . . ? C39 C44 H44A 120.2 . . ? C24 C25 C20 120.3(7) . . ? C24 C25 H25A 119.8 . . ? C20 C25 H25A 119.8 . . ? C20 C21 C22 121.8(7) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C36 C35 C34 119.8(7) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C29 C28 C27 119.1(6) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C42 C41 C40 121.5(6) . . ? C42 C41 H41A 119.2 . . ? C40 C41 H41A 119.2 . . ? C23 C22 C21 118.9(7) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C5 C4 C3 122.9(6) . . ? C5 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C47 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C25 C24 C23 120.7(7) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N2 C1 -0.2(4) . . . . ? Cl2 Ni1 N2 C1 109.4(4) . . . . ? Cl1 Ni1 N2 C1 -107.9(4) . . . . ? N1 Ni1 N2 C13 -178.8(5) . . . . ? Cl2 Ni1 N2 C13 -69.2(5) . . . . ? Cl1 Ni1 N2 C13 73.4(5) . . . . ? N2 Ni1 N1 C12 -1.6(4) . . . . ? Cl2 Ni1 N1 C12 -101.1(4) . . . . ? Cl1 Ni1 N1 C12 118.5(4) . . . . ? N2 Ni1 N1 C46 175.0(5) . . . . ? Cl2 Ni1 N1 C46 75.5(5) . . . . ? Cl1 Ni1 N1 C46 -64.9(5) . . . . ? C6 C7 C2 C3 -1.8(9) . . . . ? C11 C7 C2 C3 177.5(6) . . . . ? C6 C7 C2 C1 179.4(6) . . . . ? C11 C7 C2 C1 -1.4(7) . . . . ? C46 N1 C12 C11 2.6(9) . . . . ? Ni1 N1 C12 C11 179.5(5) . . . . ? C46 N1 C12 C1 -173.9(5) . . . . ? Ni1 N1 C12 C1 3.0(6) . . . . ? C2 C7 C11 C10 -179.5(6) . . . . ? C6 C7 C11 C10 -0.2(9) . . . . ? C2 C7 C11 C12 -0.1(7) . . . . ? C6 C7 C11 C12 179.2(5) . . . . ? N1 C12 C11 C10 4.1(12) . . . . ? C1 C12 C11 C10 -179.2(7) . . . . ? N1 C12 C11 C7 -175.1(6) . . . . ? C1 C12 C11 C7 1.6(6) . . . . ? C12 N1 C46 C47 81.4(7) . . . . ? Ni1 N1 C46 C47 -94.9(6) . . . . ? C12 N1 C46 C51 -95.2(7) . . . . ? Ni1 N1 C46 C51 88.4(6) . . . . ? C13 N2 C1 C2 2.9(10) . . . . ? Ni1 N2 C1 C2 -175.9(5) . . . . ? C13 N2 C1 C12 -179.4(5) . . . . ? Ni1 N2 C1 C12 1.8(6) . . . . ? C3 C2 C1 N2 1.5(12) . . . . ? C7 C2 C1 N2 -179.9(6) . . . . ? C3 C2 C1 C12 -176.4(7) . . . . ? C7 C2 C1 C12 2.2(6) . . . . ? N1 C12 C1 N2 -3.4(7) . . . . ? C11 C12 C1 N2 179.3(5) . . . . ? N1 C12 C1 C2 174.9(5) . . . . ? C11 C12 C1 C2 -2.4(6) . . . . ? C1 N2 C13 C18 -79.8(7) . . . . ? Ni1 N2 C13 C18 98.8(6) . . . . ? C1 N2 C13 C14 103.1(6) . . . . ? Ni1 N2 C13 C14 -78.4(6) . . . . ? C15 C16 C17 C18 -1.2(8) . . . . ? C32 C16 C17 C18 177.2(5) . . . . ? C26 C19 C20 C21 88.0(7) . . . . ? C14 C19 C20 C21 -37.5(7) . . . . ? C26 C19 C20 C25 -93.8(7) . . . . ? C14 C19 C20 C25 140.7(5) . . . . ? C18 C13 C14 C15 0.4(8) . . . . ? N2 C13 C14 C15 177.5(5) . . . . ? C18 C13 C14 C19 -178.0(5) . . . . ? N2 C13 C14 C19 -0.9(8) . . . . ? C26 C19 C14 C15 -17.3(7) . . . . ? C20 C19 C14 C15 110.3(6) . . . . ? C26 C19 C14 C13 161.1(5) . . . . ? C20 C19 C14 C13 -71.4(7) . . . . ? C20 C19 C26 C31 145.5(6) . . . . ? C14 C19 C26 C31 -88.9(7) . . . . ? C20 C19 C26 C27 -37.6(8) . . . . ? C14 C19 C26 C27 88.0(7) . . . . ? C51 C46 C47 C48 -2.3(9) . . . . ? N1 C46 C47 C48 -178.8(5) . . . . ? C51 C46 C47 C53 175.4(6) . . . . ? N1 C46 C47 C53 -1.1(9) . . . . ? C49 C48 C47 C46 0.7(9) . . . . ? C49 C48 C47 C53 -177.1(6) . . . . ? C14 C13 C18 C17 -1.6(8) . . . . ? N2 C13 C18 C17 -178.6(5) . . . . ? C14 C13 C18 C45 175.8(5) . . . . ? N2 C13 C18 C45 -1.2(8) . . . . ? C16 C17 C18 C13 2.0(9) . . . . ? C16 C17 C18 C45 -175.5(5) . . . . ? C2 C7 C6 C5 0.8(9) . . . . ? C11 C7 C6 C5 -178.4(6) . . . . ? C2 C7 C6 C8 -179.9(6) . . . . ? C11 C7 C6 C8 0.9(9) . . . . ? C35 C34 C33 C38 0.0(9) . . . . ? C35 C34 C33 C32 -174.8(6) . . . . ? C27 C26 C31 C30 -2.8(9) . . . . ? C19 C26 C31 C30 174.3(6) . . . . ? C51 C50 C49 C48 1.3(9) . . . . ? C51 C50 C49 C54 -178.1(6) . . . . ? C47 C48 C49 C50 -0.2(10) . . . . ? C47 C48 C49 C54 179.2(6) . . . . ? C31 C26 C27 C28 4.5(9) . . . . ? C19 C26 C27 C28 -172.5(6) . . . . ? C7 C2 C3 C4 1.8(9) . . . . ? C1 C2 C3 C4 -179.8(6) . . . . ? C44 C43 C42 C41 0.2(10) . . . . ? C13 C14 C15 C16 0.4(8) . . . . ? C19 C14 C15 C16 178.8(5) . . . . ? C17 C16 C15 C14 -0.1(8) . . . . ? C32 C16 C15 C14 -178.4(5) . . . . ? C17 C16 C32 C39 -156.9(5) . . . . ? C15 C16 C32 C39 21.4(7) . . . . ? C17 C16 C32 C33 76.4(7) . . . . ? C15 C16 C32 C33 -105.3(6) . . . . ? C34 C33 C32 C16 -151.3(5) . . . . ? C38 C33 C32 C16 34.2(8) . . . . ? C34 C33 C32 C39 81.6(7) . . . . ? C38 C33 C32 C39 -93.0(6) . . . . ? C49 C50 C51 C46 -2.7(9) . . . . ? C49 C50 C51 C52 175.5(6) . . . . ? C47 C46 C51 C50 3.2(9) . . . . ? N1 C46 C51 C50 179.7(5) . . . . ? C47 C46 C51 C52 -174.9(6) . . . . ? N1 C46 C51 C52 1.6(9) . . . . ? C41 C40 C39 C44 -1.7(9) . . . . ? C41 C40 C39 C32 178.9(6) . . . . ? C16 C32 C39 C40 -98.0(6) . . . . ? C33 C32 C39 C40 30.6(7) . . . . ? C16 C32 C39 C44 82.6(6) . . . . ? C33 C32 C39 C44 -148.8(5) . . . . ? C26 C31 C30 C29 -0.4(10) . . . . ? C31 C30 C29 C28 2.1(10) . . . . ? C7 C11 C10 C9 0.2(9) . . . . ? C12 C11 C10 C9 -178.9(6) . . . . ? C8 C9 C10 C11 -1.0(10) . . . . ? C34 C33 C38 C37 -2.1(9) . . . . ? C32 C33 C38 C37 172.4(6) . . . . ? C33 C38 C37 C36 2.8(10) . . . . ? C38 C37 C36 C35 -1.2(11) . . . . ? C10 C9 C8 C6 1.7(11) . . . . ? C7 C6 C8 C9 -1.6(10) . . . . ? C5 C6 C8 C9 177.5(7) . . . . ? C42 C43 C44 C39 -1.2(10) . . . . ? C40 C39 C44 C43 2.0(9) . . . . ? C32 C39 C44 C43 -178.6(5) . . . . ? C21 C20 C25 C24 -1.1(9) . . . . ? C19 C20 C25 C24 -179.4(6) . . . . ? C25 C20 C21 C22 1.4(9) . . . . ? C19 C20 C21 C22 179.5(5) . . . . ? C37 C36 C35 C34 -0.9(11) . . . . ? C33 C34 C35 C36 1.6(10) . . . . ? C30 C29 C28 C27 -0.5(10) . . . . ? C26 C27 C28 C29 -2.9(9) . . . . ? C43 C42 C41 C40 0.1(10) . . . . ? C39 C40 C41 C42 0.7(10) . . . . ? C20 C21 C22 C23 -1.0(10) . . . . ? C2 C3 C4 C5 -1.0(11) . . . . ? C21 C22 C23 C24 0.3(11) . . . . ? C3 C4 C5 C6 0.2(11) . . . . ? C7 C6 C5 C4 0.0(10) . . . . ? C8 C6 C5 C4 -179.2(7) . . . . ? C20 C25 C24 C23 0.5(11) . . . . ? C22 C23 C24 C25 -0.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.598 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.150 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 0.000 0.000 463.5 86.6 2 0.759 0.837 0.123 10.2 0.9 3 0.000 0.500 0.500 463.5 86.7 4 0.241 0.337 0.377 10.2 0.8 5 0.759 0.663 0.623 10.2 0.9 6 0.241 0.163 0.877 10.2 0.8 _platon_squeeze_details ; ? ; #==END