# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #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 'Wen Hua Sun' ; 'Carl Redshaw' School of Chemistry University of East Anglia Norwich NR4 7TJ UK ; 'Shengju Song' ; 'Xiang Hao' 'Fosong Wang' Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Baixiang Li' Dalton_Transactions 'Carl Redshaw' '' 'Xiang Hao' '' 'Yuesheng Li' '' 'Fosong Wang' '' _publ_contact_author_name 'Dr. Wen-Hua Sun' data_C1 _database_code_depnum_ccdc_archive 'CCDC 877850' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H70 Cl4 N4 Ni2 O2' _chemical_formula_weight 1380.64 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' 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' O O 0.0106 0.0060 '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 18.888(4) _cell_length_b 10.107(2) _cell_length_c 20.625(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.49(3) _cell_angle_gamma 90.00 _cell_volume 3903.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19692 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8411 _exptl_absorpt_correction_T_max 0.9070 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 19692 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8898 _reflns_number_gt 7461 _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^)+(0.0760P)^2^+4.0505P] 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 8898 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0763 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1779 _refine_ls_wR_factor_gt 0.1680 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 0.53754(2) 0.37715(4) 0.047626(19) 0.02288(13) Uani 1 1 d . . . N1 N 0.60787(15) 0.2185(3) 0.04765(13) 0.0276(6) Uani 1 1 d . . . C1 C 0.6481(2) 0.1856(4) 0.00176(17) 0.0342(8) Uani 1 1 d . . . H1A H 0.6380 0.2239 -0.0394 0.041 Uiso 1 1 calc R . . Cl2 Cl 0.45658(4) 0.55492(7) 0.06391(4) 0.02588(17) Uani 1 1 d . . . N2 N 0.53114(14) 0.2933(3) 0.14001(12) 0.0232(5) Uani 1 1 d . . . C2 C 0.7045(2) 0.0965(4) 0.0125(2) 0.0408(9) Uani 1 1 d . . . H2A H 0.7315 0.0757 -0.0207 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.63918(4) 0.51185(8) 0.08157(4) 0.03068(19) Uani 1 1 d . . . C3 C 0.7195(2) 0.0398(4) 0.0735(2) 0.0383(8) Uani 1 1 d . . . H3A H 0.7569 -0.0203 0.0821 0.046 Uiso 1 1 calc R . . C4 C 0.67847(19) 0.0731(4) 0.12177(18) 0.0333(7) Uani 1 1 d . . . H4A H 0.6880 0.0365 0.1634 0.040 Uiso 1 1 calc R . . C5 C 0.62318(18) 0.1614(3) 0.10718(16) 0.0263(6) Uani 1 1 d . . . C6 C 0.57706(18) 0.2030(3) 0.15530(16) 0.0263(6) Uani 1 1 d . . . H6A H 0.5813 0.1639 0.1964 0.032 Uiso 1 1 calc R . . C7 C 0.48254(17) 0.3309(3) 0.18586(15) 0.0237(6) Uani 1 1 d . . . C8 C 0.41802(18) 0.2646(3) 0.18433(16) 0.0275(7) Uani 1 1 d . . . C9 C 0.36910(19) 0.3130(3) 0.22426(18) 0.0323(7) Uani 1 1 d . . . H9A H 0.3253 0.2708 0.2238 0.039 Uiso 1 1 calc R . . C10 C 0.3842(2) 0.4216(4) 0.26423(18) 0.0337(8) Uani 1 1 d . . . C11 C 0.45106(19) 0.4823(3) 0.26604(17) 0.0301(7) Uani 1 1 d . . . H11A H 0.4620 0.5544 0.2936 0.036 Uiso 1 1 calc R . . C12 C 0.50099(17) 0.4379(3) 0.22804(15) 0.0241(6) Uani 1 1 d . . . C13 C 0.3994(2) 0.1445(4) 0.14211(19) 0.0362(8) Uani 1 1 d . . . H13A H 0.4381 0.1245 0.1179 0.054 Uiso 1 1 calc R . . H13B H 0.3570 0.1620 0.1123 0.054 Uiso 1 1 calc R . . H13C H 0.3912 0.0704 0.1693 0.054 Uiso 1 1 calc R . . C14 C 0.3322(2) 0.4766(4) 0.3088(2) 0.0529(12) Uani 1 1 d . . . H14A H 0.3308 0.5725 0.3015 0.063 Uiso 1 1 calc R . . C22 C 0.2557(2) 0.4279(4) 0.2894(3) 0.0504(11) Uani 1 1 d . . . C23 C 0.2166(3) 0.4804(5) 0.2334(3) 0.0641(14) Uani 1 1 d . . . H23A H 0.2366 0.5471 0.2106 0.077 Uiso 1 1 calc R . . C24 C 0.1490(3) 0.4356(6) 0.2111(4) 0.0750(17) Uani 1 1 d . . . H24A H 0.1239 0.4711 0.1732 0.090 Uiso 1 1 calc R . . C25 C 0.1189(3) 0.3389(6) 0.2447(3) 0.0706(16) Uani 1 1 d . . . H25A H 0.0733 0.3082 0.2297 0.085 Uiso 1 1 calc R . . C26 C 0.1556(3) 0.2871(5) 0.3005(3) 0.0668(16) Uani 1 1 d . . . H26A H 0.1347 0.2212 0.3231 0.080 Uiso 1 1 calc R . . C27 C 0.2239(3) 0.3318(4) 0.3238(3) 0.0562(13) Uani 1 1 d . . . H27A H 0.2481 0.2973 0.3622 0.067 Uiso 1 1 calc R . . C28 C 0.62739(18) 0.3980(3) 0.27514(17) 0.0295(7) Uani 1 1 d . . . C29 C 0.6073(2) 0.3307(4) 0.32837(19) 0.0371(8) Uani 1 1 d . . . H29A H 0.5624 0.3452 0.3409 0.045 Uiso 1 1 calc R . . C30 C 0.6535(3) 0.2422(4) 0.3629(2) 0.0525(11) Uani 1 1 d . . . H30A H 0.6403 0.1990 0.3993 0.063 Uiso 1 1 calc R . . C31 C 0.7204(3) 0.2176(4) 0.3429(3) 0.0613(15) Uani 1 1 d . . . H31A H 0.7512 0.1563 0.3652 0.074 Uiso 1 1 calc R . . C32 C 0.7405(2) 0.2841(5) 0.2904(3) 0.0554(13) Uani 1 1 d . . . H32A H 0.7851 0.2689 0.2773 0.067 Uiso 1 1 calc R . . C33 C 0.6941(2) 0.3742(4) 0.2567(2) 0.0406(9) Uani 1 1 d . . . H33A H 0.7080 0.4194 0.2211 0.049 Uiso 1 1 calc R . . C34 C 0.58311(18) 0.6364(3) 0.25666(17) 0.0279(7) Uani 1 1 d . . . C35 C 0.55595(19) 0.7332(3) 0.21316(19) 0.0335(7) Uani 1 1 d . . . H35A H 0.5334 0.7087 0.1721 0.040 Uiso 1 1 calc R . . C36 C 0.5617(2) 0.8655(4) 0.2293(2) 0.0438(9) Uani 1 1 d . . . H36A H 0.5423 0.9291 0.1996 0.053 Uiso 1 1 calc R . . C37 C 0.5958(3) 0.9035(4) 0.2891(2) 0.0526(11) Uani 1 1 d . . . H37A H 0.6002 0.9928 0.2998 0.063 Uiso 1 1 calc R . . C38 C 0.6236(3) 0.8086(4) 0.3332(2) 0.0601(13) Uani 1 1 d . . . H38A H 0.6463 0.8342 0.3740 0.072 Uiso 1 1 calc R . . C39 C 0.6180(3) 0.6742(4) 0.31716(18) 0.0439(10) Uani 1 1 d . . . H39A H 0.6376 0.6107 0.3468 0.053 Uiso 1 1 calc R . . C15 C 0.57621(17) 0.4927(3) 0.23421(15) 0.0250(6) Uani 1 1 d . . . H15A H 0.5900 0.4911 0.1900 0.030 Uiso 1 1 calc R . . O1 O 0.44412(13) 0.2760(2) 0.00822(12) 0.0316(5) Uani 1 1 d . . . C99 C 0.4467(3) 0.1631(4) -0.0341(2) 0.0460(10) Uani 1 1 d . . . H99A H 0.3992 0.1307 -0.0470 0.069 Uiso 1 1 calc R . . H99B H 0.4751 0.0947 -0.0112 0.069 Uiso 1 1 calc R . . H99C H 0.4676 0.1886 -0.0722 0.069 Uiso 1 1 calc R . . C18 C 0.3615(2) 0.4579(5) 0.37964(17) 0.088(2) Uani 1 1 d G . . C16 C 0.3912(3) 0.3383(6) 0.4026(2) 0.120(3) Uani 1 1 d G . . H16A H 0.3940 0.2681 0.3739 0.144 Uiso 1 1 calc R . . C17 C 0.4169(3) 0.3237(8) 0.4685(3) 0.206(8) Uani 1 1 d G . . H17A H 0.4368 0.2437 0.4839 0.247 Uiso 1 1 calc R . . C19 C 0.4128(3) 0.4286(11) 0.51144(17) 0.214(10) Uani 1 1 d G . . H19A H 0.4299 0.4188 0.5555 0.256 Uiso 1 1 calc R . . C20 C 0.3830(4) 0.5482(9) 0.4884(3) 0.221(10) Uani 1 1 d G . . H20A H 0.3803 0.6184 0.5172 0.265 Uiso 1 1 calc R . . C21 C 0.3574(3) 0.5629(6) 0.4226(3) 0.158(5) Uani 1 1 d G . . H21A H 0.3375 0.6429 0.4072 0.190 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 0.0244(2) 0.0222(2) 0.0216(2) 0.00204(15) 0.00131(15) 0.00149(15) N1 0.0307(14) 0.0262(13) 0.0257(13) 0.0008(11) 0.0033(11) 0.0009(11) C1 0.0384(19) 0.0364(18) 0.0293(17) 0.0046(14) 0.0102(15) 0.0098(16) Cl2 0.0294(4) 0.0258(4) 0.0222(3) 0.0014(3) 0.0025(3) 0.0030(3) N2 0.0243(13) 0.0231(12) 0.0220(12) 0.0019(10) 0.0025(10) -0.0029(10) C2 0.043(2) 0.040(2) 0.041(2) -0.0004(17) 0.0167(17) 0.0113(17) Cl1 0.0282(4) 0.0360(4) 0.0266(4) 0.0022(3) -0.0009(3) -0.0052(3) C3 0.0309(18) 0.0334(18) 0.051(2) -0.0016(17) 0.0071(16) 0.0102(15) C4 0.0324(18) 0.0333(17) 0.0329(18) 0.0043(14) -0.0003(14) 0.0066(15) C5 0.0300(16) 0.0226(14) 0.0259(15) 0.0012(12) 0.0018(13) 0.0007(13) C6 0.0306(16) 0.0224(14) 0.0247(15) 0.0023(12) -0.0004(13) 0.0011(13) C7 0.0260(15) 0.0232(14) 0.0222(14) 0.0044(12) 0.0047(12) 0.0035(12) C8 0.0328(17) 0.0237(15) 0.0266(15) 0.0023(12) 0.0061(13) -0.0027(13) C9 0.0297(17) 0.0310(17) 0.0379(18) 0.0000(15) 0.0114(14) -0.0063(14) C10 0.0337(18) 0.0309(17) 0.0396(19) -0.0007(15) 0.0163(15) 0.0005(15) C11 0.0307(17) 0.0287(16) 0.0321(17) -0.0026(13) 0.0084(14) -0.0012(14) C12 0.0261(15) 0.0265(15) 0.0197(14) 0.0048(12) 0.0032(12) 0.0014(13) C13 0.0362(19) 0.0349(18) 0.040(2) -0.0049(15) 0.0128(16) -0.0130(15) C14 0.046(2) 0.047(2) 0.074(3) -0.022(2) 0.039(2) -0.018(2) C22 0.046(2) 0.038(2) 0.075(3) -0.015(2) 0.038(2) -0.0064(19) C23 0.058(3) 0.047(3) 0.094(4) -0.005(3) 0.034(3) 0.000(2) C24 0.041(3) 0.068(3) 0.118(5) -0.003(3) 0.020(3) 0.004(2) C25 0.042(3) 0.066(3) 0.110(5) -0.018(3) 0.030(3) -0.006(2) C26 0.056(3) 0.056(3) 0.099(4) -0.024(3) 0.050(3) -0.017(2) C27 0.057(3) 0.046(2) 0.074(3) -0.016(2) 0.040(3) -0.009(2) C28 0.0288(17) 0.0261(15) 0.0319(17) -0.0058(13) -0.0025(14) 0.0032(13) C29 0.0369(19) 0.0341(18) 0.0383(19) 0.0004(15) -0.0027(16) 0.0015(16) C30 0.062(3) 0.037(2) 0.052(3) 0.0052(19) -0.017(2) 0.003(2) C31 0.056(3) 0.036(2) 0.080(4) -0.010(2) -0.034(3) 0.012(2) C32 0.030(2) 0.052(3) 0.080(3) -0.023(2) -0.010(2) 0.0127(19) C33 0.0273(18) 0.041(2) 0.051(2) -0.0157(18) -0.0015(16) 0.0042(15) C34 0.0262(16) 0.0280(16) 0.0307(17) -0.0023(13) 0.0076(13) -0.0019(13) C35 0.0309(17) 0.0295(17) 0.0391(19) 0.0007(15) 0.0002(15) -0.0041(14) C36 0.045(2) 0.0300(18) 0.056(3) 0.0057(17) 0.0037(19) -0.0001(17) C37 0.068(3) 0.0315(19) 0.060(3) -0.0074(19) 0.015(2) -0.006(2) C38 0.094(4) 0.041(2) 0.042(2) -0.0134(19) -0.004(2) -0.008(2) C39 0.067(3) 0.0344(19) 0.0282(18) -0.0028(15) -0.0019(18) -0.0043(19) C15 0.0254(15) 0.0275(15) 0.0224(15) -0.0024(12) 0.0047(12) -0.0006(13) O1 0.0341(13) 0.0270(11) 0.0326(12) 0.0011(10) -0.0005(10) -0.0052(10) C99 0.061(3) 0.0300(18) 0.044(2) -0.0029(16) -0.005(2) -0.0097(18) C18 0.082(4) 0.133(6) 0.059(3) -0.040(4) 0.046(3) -0.065(4) C16 0.118(7) 0.197(10) 0.045(3) 0.026(5) 0.011(4) -0.028(7) C17 0.156(10) 0.39(2) 0.068(5) 0.062(9) -0.003(6) -0.095(13) C19 0.144(10) 0.45(3) 0.051(5) -0.015(9) 0.027(5) -0.173(14) C20 0.208(14) 0.38(2) 0.090(7) -0.115(11) 0.083(8) -0.206(15) C21 0.151(8) 0.222(10) 0.123(7) -0.119(7) 0.101(6) -0.126(8) _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 2.082(3) . ? Ni1 N2 2.103(3) . ? Ni1 O1 2.108(2) . ? Ni1 Cl1 2.3831(10) . ? Ni1 Cl2 2.4111(9) . ? Ni1 Cl2 2.4171(9) 3_665 ? N1 C1 1.331(4) . ? N1 C5 1.353(4) . ? C1 C2 1.390(5) . ? C1 H1A 0.9300 . ? Cl2 Ni1 2.4171(9) 3_665 ? N2 C6 1.270(4) . ? N2 C7 1.452(4) . ? C2 C3 1.378(6) . ? C2 H2A 0.9300 . ? C3 C4 1.381(5) . ? C3 H3A 0.9300 . ? C4 C5 1.377(5) . ? C4 H4A 0.9300 . ? C5 C6 1.465(5) . ? C6 H6A 0.9300 . ? C7 C8 1.388(4) . ? C7 C12 1.403(4) . ? C8 C9 1.404(5) . ? C8 C13 1.508(5) . ? C9 C10 1.380(5) . ? C9 H9A 0.9300 . ? C10 C11 1.400(5) . ? C10 C14 1.535(5) . ? C11 C12 1.378(4) . ? C11 H11A 0.9300 . ? C12 C15 1.515(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C18 1.506(6) . ? C14 C22 1.530(6) . ? C14 H14A 0.9800 . ? C22 C27 1.385(6) . ? C22 C23 1.392(8) . ? C23 C24 1.377(7) . ? C23 H23A 0.9300 . ? C24 C25 1.364(8) . ? C24 H24A 0.9300 . ? C25 C26 1.368(9) . ? C25 H25A 0.9300 . ? C26 C27 1.392(7) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C33 1.384(5) . ? C28 C29 1.386(5) . ? C28 C15 1.533(5) . ? C29 C30 1.381(5) . ? C29 H29A 0.9300 . ? C30 C31 1.403(7) . ? C30 H30A 0.9300 . ? C31 C32 1.370(8) . ? C31 H31A 0.9300 . ? C32 C33 1.386(6) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.380(5) . ? C34 C39 1.387(5) . ? C34 C15 1.525(4) . ? C35 C36 1.379(5) . ? C35 H35A 0.9300 . ? C36 C37 1.369(7) . ? C36 H36A 0.9300 . ? C37 C38 1.379(7) . ? C37 H37A 0.9300 . ? C38 C39 1.399(6) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C15 H15A 0.9800 . ? O1 C99 1.442(4) . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? C18 C16 1.3900 . ? C18 C21 1.3900 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 C19 1.3900 . ? C17 H17A 0.9300 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 78.55(11) . . ? N1 Ni1 O1 97.39(10) . . ? N2 Ni1 O1 90.57(10) . . ? N1 Ni1 Cl1 87.16(8) . . ? N2 Ni1 Cl1 95.92(8) . . ? O1 Ni1 Cl1 172.72(7) . . ? N1 Ni1 Cl2 171.90(8) . . ? N2 Ni1 Cl2 93.54(8) . . ? O1 Ni1 Cl2 84.30(7) . . ? Cl1 Ni1 Cl2 91.99(3) . . ? N1 Ni1 Cl2 96.35(8) . 3_665 ? N2 Ni1 Cl2 172.70(7) . 3_665 ? O1 Ni1 Cl2 84.88(7) . 3_665 ? Cl1 Ni1 Cl2 88.98(4) . 3_665 ? Cl2 Ni1 Cl2 91.69(3) . 3_665 ? C1 N1 C5 117.7(3) . . ? C1 N1 Ni1 128.0(2) . . ? C5 N1 Ni1 112.9(2) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? Ni1 Cl2 Ni1 88.31(3) . 3_665 ? C6 N2 C7 119.7(3) . . ? C6 N2 Ni1 113.3(2) . . ? C7 N2 Ni1 126.91(19) . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 122.6(3) . . ? N2 C6 C5 119.0(3) . . ? N2 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C8 C7 C12 122.2(3) . . ? C8 C7 N2 119.1(3) . . ? C12 C7 N2 118.6(3) . . ? C7 C8 C9 117.5(3) . . ? C7 C8 C13 122.7(3) . . ? C9 C8 C13 119.8(3) . . ? C10 C9 C8 121.8(3) . . ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? C9 C10 C11 118.7(3) . . ? C9 C10 C14 123.2(3) . . ? C11 C10 C14 118.1(3) . . ? C12 C11 C10 121.6(3) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C7 118.1(3) . . ? C11 C12 C15 122.5(3) . . ? C7 C12 C15 119.2(3) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C18 C14 C22 115.4(4) . . ? C18 C14 C10 110.7(4) . . ? C22 C14 C10 112.5(3) . . ? C18 C14 H14A 105.8 . . ? C22 C14 H14A 105.8 . . ? C10 C14 H14A 105.8 . . ? C27 C22 C23 118.3(5) . . ? C27 C22 C14 123.3(5) . . ? C23 C22 C14 118.4(4) . . ? C24 C23 C22 121.4(5) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C23 119.6(6) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C22 C27 C26 119.7(6) . . ? C22 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C33 C28 C29 119.1(4) . . ? C33 C28 C15 119.2(3) . . ? C29 C28 C15 121.6(3) . . ? C30 C29 C28 120.4(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.7(5) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 119.9(4) . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C33 119.8(4) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C28 C33 C32 121.0(4) . . ? C28 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C35 C34 C39 118.8(3) . . ? C35 C34 C15 117.9(3) . . ? C39 C34 C15 123.2(3) . . ? C36 C35 C34 121.3(4) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 119.6(4) . . ? C36 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C37 C38 C39 120.6(4) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C34 C39 C38 119.5(4) . . ? C34 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C12 C15 C34 114.6(3) . . ? C12 C15 C28 109.6(3) . . ? C34 C15 C28 113.9(3) . . ? C12 C15 H15A 106.0 . . ? C34 C15 H15A 106.0 . . ? C28 C15 H15A 106.0 . . ? C99 O1 Ni1 121.6(2) . . ? O1 C99 H99A 109.5 . . ? O1 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O1 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C16 C18 C21 120.0 . . ? C16 C18 C14 121.4(4) . . ? C21 C18 C14 118.6(4) . . ? C17 C16 C18 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C16 H16A 120.0 . . ? C16 C17 C19 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C17 H17A 120.0 . . ? C20 C19 C17 120.0 . . ? C20 C19 H19A 120.0 . . ? C17 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C18 120.0 . . ? C20 C21 H21A 120.0 . . ? C18 C21 H21A 120.0 . . ? 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 C1 -177.1(3) . . . . ? O1 Ni1 N1 C1 93.8(3) . . . . ? Cl1 Ni1 N1 C1 -80.5(3) . . . . ? Cl2 Ni1 N1 C1 -164.6(4) . . . . ? Cl2 Ni1 N1 C1 8.2(3) 3_665 . . . ? N2 Ni1 N1 C5 -11.1(2) . . . . ? O1 Ni1 N1 C5 -100.2(2) . . . . ? Cl1 Ni1 N1 C5 85.5(2) . . . . ? Cl2 Ni1 N1 C5 1.4(7) . . . . ? Cl2 Ni1 N1 C5 174.1(2) 3_665 . . . ? C5 N1 C1 C2 -0.2(5) . . . . ? Ni1 N1 C1 C2 165.2(3) . . . . ? N1 Ni1 Cl2 Ni1 172.8(6) . . . 3_665 ? N2 Ni1 Cl2 Ni1 -174.90(7) . . . 3_665 ? O1 Ni1 Cl2 Ni1 -84.68(7) . . . 3_665 ? Cl1 Ni1 Cl2 Ni1 89.04(4) . . . 3_665 ? Cl2 Ni1 Cl2 Ni1 0.0 3_665 . . 3_665 ? N1 Ni1 N2 C6 8.6(2) . . . . ? O1 Ni1 N2 C6 106.0(2) . . . . ? Cl1 Ni1 N2 C6 -77.3(2) . . . . ? Cl2 Ni1 N2 C6 -169.6(2) . . . . ? Cl2 Ni1 N2 C6 54.7(7) 3_665 . . . ? N1 Ni1 N2 C7 -173.2(3) . . . . ? O1 Ni1 N2 C7 -75.8(3) . . . . ? Cl1 Ni1 N2 C7 100.9(2) . . . . ? Cl2 Ni1 N2 C7 8.6(2) . . . . ? Cl2 Ni1 N2 C7 -127.1(5) 3_665 . . . ? N1 C1 C2 C3 -0.1(6) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C1 N1 C5 C4 0.7(5) . . . . ? Ni1 N1 C5 C4 -166.8(3) . . . . ? C1 N1 C5 C6 179.6(3) . . . . ? Ni1 N1 C5 C6 12.1(4) . . . . ? C3 C4 C5 N1 -0.9(5) . . . . ? C3 C4 C5 C6 -179.7(3) . . . . ? C7 N2 C6 C5 176.8(3) . . . . ? Ni1 N2 C6 C5 -4.9(4) . . . . ? N1 C5 C6 N2 -4.9(4) . . . . ? C4 C5 C6 N2 174.0(3) . . . . ? C6 N2 C7 C8 -89.0(4) . . . . ? Ni1 N2 C7 C8 92.9(3) . . . . ? C6 N2 C7 C12 94.2(4) . . . . ? Ni1 N2 C7 C12 -83.8(3) . . . . ? C12 C7 C8 C9 3.5(5) . . . . ? N2 C7 C8 C9 -173.1(3) . . . . ? C12 C7 C8 C13 -176.3(3) . . . . ? N2 C7 C8 C13 7.0(5) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? C13 C8 C9 C10 179.2(3) . . . . ? C8 C9 C10 C11 -1.7(6) . . . . ? C8 C9 C10 C14 -179.6(4) . . . . ? C9 C10 C11 C12 1.3(6) . . . . ? C14 C10 C11 C12 179.3(4) . . . . ? C10 C11 C12 C7 1.4(5) . . . . ? C10 C11 C12 C15 -173.5(3) . . . . ? C8 C7 C12 C11 -3.9(5) . . . . ? N2 C7 C12 C11 172.7(3) . . . . ? C8 C7 C12 C15 171.2(3) . . . . ? N2 C7 C12 C15 -12.2(4) . . . . ? C9 C10 C14 C18 113.2(4) . . . . ? C11 C10 C14 C18 -64.7(5) . . . . ? C9 C10 C14 C22 -17.5(6) . . . . ? C11 C10 C14 C22 164.6(4) . . . . ? C18 C14 C22 C27 -23.6(6) . . . . ? C10 C14 C22 C27 104.7(5) . . . . ? C18 C14 C22 C23 158.1(4) . . . . ? C10 C14 C22 C23 -73.6(5) . . . . ? C27 C22 C23 C24 -2.1(7) . . . . ? C14 C22 C23 C24 176.3(4) . . . . ? C22 C23 C24 C25 0.8(8) . . . . ? C23 C24 C25 C26 0.3(9) . . . . ? C24 C25 C26 C27 0.0(8) . . . . ? C23 C22 C27 C26 2.3(6) . . . . ? C14 C22 C27 C26 -176.0(4) . . . . ? C25 C26 C27 C22 -1.4(7) . . . . ? C33 C28 C29 C30 0.7(5) . . . . ? C15 C28 C29 C30 177.6(3) . . . . ? C28 C29 C30 C31 -1.8(6) . . . . ? C29 C30 C31 C32 1.8(6) . . . . ? C30 C31 C32 C33 -0.8(7) . . . . ? C29 C28 C33 C32 0.3(5) . . . . ? C15 C28 C33 C32 -176.6(3) . . . . ? C31 C32 C33 C28 -0.2(6) . . . . ? C39 C34 C35 C36 -1.4(6) . . . . ? C15 C34 C35 C36 -178.5(3) . . . . ? C34 C35 C36 C37 1.1(6) . . . . ? C35 C36 C37 C38 -0.8(7) . . . . ? C36 C37 C38 C39 0.8(8) . . . . ? C35 C34 C39 C38 1.3(6) . . . . ? C15 C34 C39 C38 178.3(4) . . . . ? C37 C38 C39 C34 -1.1(8) . . . . ? C11 C12 C15 C34 -29.3(4) . . . . ? C7 C12 C15 C34 155.8(3) . . . . ? C11 C12 C15 C28 100.1(4) . . . . ? C7 C12 C15 C28 -74.8(3) . . . . ? C35 C34 C15 C12 -71.5(4) . . . . ? C39 C34 C15 C12 111.6(4) . . . . ? C35 C34 C15 C28 161.3(3) . . . . ? C39 C34 C15 C28 -15.7(5) . . . . ? C33 C28 C15 C12 139.7(3) . . . . ? C29 C28 C15 C12 -37.1(4) . . . . ? C33 C28 C15 C34 -90.5(4) . . . . ? C29 C28 C15 C34 92.7(4) . . . . ? N1 Ni1 O1 C99 -27.5(3) . . . . ? N2 Ni1 O1 C99 -106.0(3) . . . . ? Cl1 Ni1 O1 C99 100.9(6) . . . . ? Cl2 Ni1 O1 C99 160.5(3) . . . . ? Cl2 Ni1 O1 C99 68.3(2) 3_665 . . . ? C22 C14 C18 C16 83.5(5) . . . . ? C10 C14 C18 C16 -45.8(4) . . . . ? C22 C14 C18 C21 -95.6(4) . . . . ? C10 C14 C18 C21 135.1(3) . . . . ? C21 C18 C16 C17 0.0 . . . . ? C14 C18 C16 C17 -179.1(4) . . . . ? C18 C16 C17 C19 0.0 . . . . ? C16 C17 C19 C20 0.0 . . . . ? C17 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C18 0.0 . . . . ? C16 C18 C21 C20 0.0 . . . . ? C14 C18 C21 C20 179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.537 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.124 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # 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 0.500 409.9 16.6 2 0.000 0.500 0.000 409.9 16.4 _platon_squeeze_details ; ? ; #==END data_C5 _database_code_depnum_ccdc_archive 'CCDC 877851' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C246 H230 Cl12 N12 Ni6 O6' _chemical_formula_weight 4228.08 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' 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' O O 0.0106 0.0060 '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 18.912(4) _cell_length_b 20.045(4) _cell_length_c 22.057(4) _cell_angle_alpha 103.16(3) _cell_angle_beta 109.38(3) _cell_angle_gamma 111.43(3) _cell_volume 6738(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54230 _cell_measurement_theta_min 1.07 _cell_measurement_theta_max 25.34 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2210 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9031 _exptl_absorpt_correction_T_max 0.9552 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 54230 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.34 _reflns_number_total 24513 _reflns_number_gt 15340 _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. The following restraints were used: DFIX 1.39 0.01 C205 C231 C231 C232 C232 C233 C235 C234 C234 C205 SIMU C205 C231 C232 C233 C234 C235 The carbon atoms, C205, C231, C232, C233, C234 and C235 were refined isotropically due to their heavy disorder behavior. ; _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^)+(0.1753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24513 _refine_ls_number_parameters 1240 _refine_ls_number_restraints 11 _refine_ls_R_factor_ref 0.1276 _refine_ls_R_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.2996 _refine_ls_wR_factor_gt 0.2709 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _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 0.49154(4) 0.55680(4) 0.06373(3) 0.03185(18) Uani 1 1 d . . . N1 N 0.5662(3) 0.6395(3) 0.1653(2) 0.0426(11) Uani 1 1 d . . . Ni2 Ni 0.89377(4) 0.95720(4) 0.95948(4) 0.0398(2) Uani 1 1 d . . . N2 N 0.4087(3) 0.6036(2) 0.0750(2) 0.0333(9) Uani 1 1 d . . . N3 N 0.7890(3) 0.8594(3) 0.9415(2) 0.0430(11) Uani 1 1 d . . . Cl2 Cl 0.60343(8) 0.52396(7) 0.05629(6) 0.0367(3) Uani 1 1 d . . . N4 N 0.7977(3) 0.9901(2) 0.9279(2) 0.0369(10) Uani 1 1 d . . . Cl5 Cl 0.99750(8) 0.91609(8) 1.00935(7) 0.0416(3) Uani 1 1 d . . . Cl1 Cl 0.44690(9) 0.45613(8) 0.10318(7) 0.0458(3) Uani 1 1 d . . . C12 C 0.2525(3) 0.5294(3) 0.0204(2) 0.0321(10) Uani 1 1 d . . . Cl7 Cl 0.88183(9) 0.90152(9) 0.84676(7) 0.0489(3) Uani 1 1 d . . . C140 C 0.7152(3) 0.8633(3) 0.9195(3) 0.0401(12) Uani 1 1 d . . . C92 C 0.2580(3) 0.4772(3) 0.0613(2) 0.0342(11) Uani 1 1 d . . . H92 H 0.3089 0.4719 0.0661 0.041 Uiso 1 1 calc R . . C94 C 0.7245(3) 0.9361(3) 0.9139(3) 0.0407(12) Uani 1 1 d . . . H94 H 0.6771 0.9440 0.9000 0.049 Uiso 1 1 calc R . . C205 C 0.9421(5) 0.6767(5) 0.4707(4) 0.084(2) Uiso 1 1 d DU . . N6 N 1.0602(3) 0.8630(3) 0.5469(3) 0.0535(13) Uani 1 1 d . . . C206 C 0.9500(4) 0.7209(5) 0.4243(4) 0.070(2) Uani 1 1 d . . . H20A H 0.9288 0.7580 0.4342 0.084 Uiso 1 1 calc R . . C6 C 0.4437(3) 0.6568(3) 0.1359(3) 0.0395(12) Uani 1 1 d . . . H6 H 0.4140 0.6811 0.1480 0.047 Uiso 1 1 calc R . . C15 C 0.3227(3) 0.6338(3) -0.0122(3) 0.0390(12) Uani 1 1 d . . . C16 C 0.8226(3) 1.1247(3) 0.9785(3) 0.0372(11) Uani 1 1 d . . . C7 C 0.3251(3) 0.5875(3) 0.0269(2) 0.0321(10) Uani 1 1 d . . . C19 C 0.4048(3) 0.6970(3) -0.0034(3) 0.0349(11) Uani 1 1 d . . . H19 H 0.4475 0.6794 0.0107 0.042 Uiso 1 1 calc R . . C10 C 0.1653(3) 0.5591(3) -0.0684(2) 0.0370(11) Uani 1 1 d . . . C21 C 0.8221(3) 1.1904(3) 0.9685(3) 0.0434(13) Uani 1 1 d . . . H21 H 0.8341 1.2321 1.0064 0.052 Uiso 1 1 calc R . . C22 C 0.7870(4) 1.1330(3) 0.8491(3) 0.0399(12) Uani 1 1 d . . . H22 H 0.7759 1.1364 0.8058 0.048 Uiso 1 1 calc R . . C5 C 0.5302(3) 0.6802(3) 0.1871(3) 0.0430(13) Uani 1 1 d . . . C24 C 0.1816(3) 0.3950(3) 0.0209(3) 0.0395(12) Uani 1 1 d . . . C25 C 0.8042(3) 1.1964(3) 0.9039(3) 0.0398(12) Uani 1 1 d . . . C26 C 0.7613(4) 0.9962(3) 0.7928(3) 0.0419(12) Uani 1 1 d . . . H26 H 0.7945 0.9715 0.8116 0.050 Uiso 1 1 calc R . . C9 C 0.2416(3) 0.6178(3) -0.0607(3) 0.0404(12) Uani 1 1 d . . . H9 H 0.2383 0.6465 -0.0883 0.048 Uiso 1 1 calc R . . C11 C 0.1726(3) 0.5170(3) -0.0271(3) 0.0404(12) Uani 1 1 d . . . H11B H 0.1230 0.4791 -0.0307 0.049 Uiso 1 1 calc R . . C29 C 0.1283(4) 0.3612(4) 0.0479(4) 0.0541(15) Uani 1 1 d . . . H29 H 0.1391 0.3884 0.0930 0.065 Uiso 1 1 calc R . . C30 C 0.2731(4) 0.5184(3) 0.1365(3) 0.0442(13) Uani 1 1 d . . . C31 C 0.8009(3) 1.0621(3) 0.9199(3) 0.0414(12) Uani 1 1 d . . . C32 C 0.8384(4) 1.1159(3) 1.0479(3) 0.0468(13) Uani 1 1 d . . . H32 H 0.8714 1.0877 1.0526 0.056 Uiso 1 1 calc R . . C33 C 0.7883(4) 1.0191(3) 0.7402(3) 0.0445(13) Uani 1 1 d . . . N8 N 0.9874(4) 0.9094(3) 0.6188(3) 0.0614(14) Uani 1 1 d . . . C35 C 0.4387(4) 0.7731(3) 0.0550(3) 0.0442(13) Uani 1 1 d . . . C36 C 0.6688(4) 0.9363(3) 0.7626(3) 0.0452(13) Uani 1 1 d . . . C37 C 1.0980(4) 0.8371(4) 0.5061(3) 0.0510(15) Uani 1 1 d . . . C38 C 0.0810(4) 0.5457(4) -0.1197(3) 0.0538(15) Uani 1 1 d . . . H38 H 0.0921 0.5819 -0.1428 0.065 Uiso 1 1 calc R . . C39 C 0.8044(4) 1.2698(3) 0.8953(3) 0.0455(13) Uani 1 1 d . . . H39 H 0.8052 1.3015 0.9368 0.055 Uiso 1 1 calc R . . C40 C 0.6379(4) 0.8043(3) 0.9058(3) 0.0472(14) Uani 1 1 d . . . H40 H 0.5891 0.8101 0.8933 0.057 Uiso 1 1 calc R . . C85 C 1.0163(5) 0.8610(4) 0.6354(3) 0.0581(16) Uani 1 1 d . . . C42 C 0.3985(4) 0.7058(3) -0.0722(3) 0.0466(13) Uani 1 1 d . . . C43 C 0.1629(4) 0.3528(4) -0.0451(3) 0.0609(17) Uani 1 1 d . . . H43 H 0.1974 0.3744 -0.0647 0.073 Uiso 1 1 calc R . . C44 C 0.6041(4) 0.9565(4) 0.7542(3) 0.0594(17) Uani 1 1 d . . . H44 H 0.6179 1.0089 0.7674 0.071 Uiso 1 1 calc R . . C45 C 0.6358(4) 0.7358(4) 0.9115(4) 0.0654(19) Uani 1 1 d . . . H45 H 0.5843 0.6937 0.9002 0.079 Uiso 1 1 calc R . . C47 C 0.7853(4) 1.0658(3) 0.8544(3) 0.0425(13) Uani 1 1 d . . . C48 C 0.8833(4) 1.3171(4) 0.8900(3) 0.0547(15) Uani 1 1 d . . . H48B H 0.9331 1.3297 0.9308 0.082 Uiso 1 1 calc R . . H48C H 0.8842 1.3643 0.8870 0.082 Uiso 1 1 calc R . . H48A H 0.8828 1.2873 0.8490 0.082 Uiso 1 1 calc R . . C49 C 0.8960(5) 0.6676(5) 0.3456(4) 0.070(2) Uani 1 1 d . . . C50 C 0.7108(4) 0.7304(4) 0.9341(4) 0.0594(17) Uani 1 1 d . . . H50 H 0.7110 0.6860 0.9400 0.071 Uiso 1 1 calc R . . C51 C 1.2175(4) 0.8521(4) 0.4851(3) 0.0591(17) Uani 1 1 d . . . H51 H 1.2754 0.8809 0.4986 0.071 Uiso 1 1 calc R . . C52 C 0.2164(4) 0.5427(3) 0.1470(3) 0.0479(14) Uani 1 1 d . . . H52 H 0.1703 0.5362 0.1089 0.057 Uiso 1 1 calc R . . C53 C 0.3957(4) 0.6466(5) -0.1207(4) 0.0677(19) Uani 1 1 d . . . H53 H 0.3945 0.6030 -0.1119 0.081 Uiso 1 1 calc R . . C54 C 0.7849(4) 0.7932(4) 0.9474(3) 0.0529(15) Uani 1 1 d . . . H54 H 0.8348 0.7894 0.9613 0.063 Uiso 1 1 calc R . . C55 C 1.0451(4) 0.7689(4) 0.4433(3) 0.0540(15) Uani 1 1 d . . . C56 C 0.7224(4) 1.2487(4) 0.8295(3) 0.0595(17) Uani 1 1 d . . . H56B H 0.6727 1.2189 0.8337 0.089 Uiso 1 1 calc R . . H56A H 0.7211 1.2184 0.7882 0.089 Uiso 1 1 calc R . . H56C H 0.7229 1.2957 0.8262 0.089 Uiso 1 1 calc R . . C57 C 0.8443(6) 1.0669(4) 0.6485(4) 0.071(2) Uani 1 1 d . . . H57 H 0.8629 1.0832 0.6178 0.085 Uiso 1 1 calc R . . C58 C 0.8748(4) 1.0589(4) 0.7593(3) 0.0572(16) Uani 1 1 d . . . H58 H 0.9144 1.0685 0.8032 0.069 Uiso 1 1 calc R . . C59 C 1.0808(4) 0.7441(4) 0.4040(3) 0.0614(18) Uani 1 1 d . . . H59 H 1.0459 0.6990 0.3631 0.074 Uiso 1 1 calc R . . C60 C 0.5260(4) 0.8110(4) 0.1042(4) 0.0636(18) Uani 1 1 d . . . H60 H 0.5612 0.7897 0.1004 0.076 Uiso 1 1 calc R . . C61 C 0.7452(5) 1.0046(4) 1.0692(4) 0.071(2) Uani 1 1 d . . . H61 H 0.7933 0.9992 1.0898 0.085 Uiso 1 1 calc R . . C62 C 1.1669(4) 0.7843(4) 0.4236(3) 0.0608(17) Uani 1 1 d . . . C1 C 0.6444(4) 0.6571(4) 0.2086(3) 0.0596(17) Uani 1 1 d . . . H1 H 0.6694 0.6286 0.1942 0.072 Uiso 1 1 calc R . . C64 C 0.8930(5) 1.1941(4) 1.1124(3) 0.0597(17) Uani 1 1 d . . . C65 C 0.7530(4) 1.0633(4) 1.0448(3) 0.0566(16) Uani 1 1 d . . . C66 C 1.1835(4) 0.8779(4) 0.5268(3) 0.0529(15) Uani 1 1 d . . . C67 C 0.9755(6) 0.8656(5) 0.7275(4) 0.083(2) Uani 1 1 d . . . H67 H 0.9728 0.8514 0.7643 0.099 Uiso 1 1 calc R . . C68 C 0.8898(5) 0.7058(6) 0.3003(4) 0.084(2) Uani 1 1 d . . . H68 H 0.9170 0.7600 0.3171 0.101 Uiso 1 1 calc R . . C69 C 0.3421(5) 0.5305(5) 0.1912(4) 0.076(2) Uani 1 1 d . . . H69 H 0.3794 0.5135 0.1838 0.091 Uiso 1 1 calc R . . C70 C 0.0280(4) 0.5607(5) -0.0842(4) 0.072(2) Uani 1 1 d . . . H70C H 0.0602 0.6131 -0.0491 0.107 Uiso 1 1 calc R . . H70A H 0.0146 0.5245 -0.0627 0.107 Uiso 1 1 calc R . . H70B H -0.0239 0.5541 -0.1186 0.107 Uiso 1 1 calc R . . C71 C 0.7325(5) 1.0042(4) 0.6738(3) 0.0633(18) Uani 1 1 d . . . H71 H 0.6739 0.9780 0.6591 0.076 Uiso 1 1 calc R . . C72 C 0.4000(5) 0.7694(5) -0.0859(4) 0.074(2) Uani 1 1 d . . . H72 H 0.4019 0.8094 -0.0532 0.089 Uiso 1 1 calc R . . C74 C 0.0571(4) 0.2850(4) 0.0071(4) 0.0672(19) Uani 1 1 d . . . H74 H 0.0216 0.2622 0.0254 0.081 Uiso 1 1 calc R . . C75 C 0.0421(5) 0.2479(4) -0.0554(5) 0.077(2) Uani 1 1 d . . . H75 H -0.0053 0.1986 -0.0821 0.092 Uiso 1 1 calc R . . C76 C 0.7624(5) 1.0278(5) 0.6279(4) 0.075(2) Uani 1 1 d . . . H76 H 0.7237 1.0154 0.5826 0.090 Uiso 1 1 calc R . . C77 C 1.2435(6) 0.9426(5) 0.7135(4) 0.093(3) Uani 1 1 d . . . H77 H 1.2330 0.9849 0.7187 0.111 Uiso 1 1 calc R . . C8 C 0.3880(5) 0.8075(4) 0.0644(4) 0.0658(18) Uani 1 1 d . . . H8 H 0.3301 0.7821 0.0333 0.079 Uiso 1 1 calc R . . C80 C 0.4219(6) 0.8768(5) 0.1180(5) 0.083(2) Uani 1 1 d . . . H80 H 0.3871 0.8980 0.1234 0.100 Uiso 1 1 calc R . . C81 C 1.2407(5) 0.9460(4) 0.5995(3) 0.0662(19) Uani 1 1 d . . . H81 H 1.2067 0.9712 0.6062 0.079 Uiso 1 1 calc R . . C84 C 0.9801(6) 1.2293(5) 1.1375(4) 0.086(3) Uani 1 1 d . . . H84 H 1.0053 1.2059 1.1168 0.103 Uiso 1 1 calc R . . C34 C 1.0121(5) 0.8372(4) 0.6881(4) 0.071(2) Uani 1 1 d . . . H34 H 1.0328 0.8033 0.6980 0.085 Uiso 1 1 calc R . . C86 C 0.8027(5) 0.5808(7) 0.2017(5) 0.100(3) Uani 1 1 d . . . H86 H 0.7707 0.5517 0.1536 0.121 Uiso 1 1 calc R . . C87 C 0.8392(6) 0.6577(6) 0.2263(4) 0.087(3) Uani 1 1 d . . . H87 H 0.8321 0.6817 0.1949 0.104 Uiso 1 1 calc R . . C88 C 0.9037(5) 1.0849(5) 0.7145(4) 0.0697(19) Uani 1 1 d . . . H88 H 0.9619 1.1136 0.7287 0.084 Uiso 1 1 calc R . . C89 C 0.5185(5) 0.8998(5) 0.7263(4) 0.077(2) Uani 1 1 d . . . H89 H 0.4764 0.9146 0.7214 0.093 Uiso 1 1 calc R . . C90 C 0.8585(6) 0.5893(6) 0.3205(4) 0.095(3) Uani 1 1 d . . . H90 H 0.8633 0.5648 0.3516 0.114 Uiso 1 1 calc R . . C91 C 1.2546(5) 0.9121(5) 0.6551(4) 0.076(2) Uani 1 1 d . . . C3 C 0.6533(5) 0.7594(5) 0.2960(4) 0.088(3) Uani 1 1 d . . . H3 H 0.6834 0.8013 0.3393 0.106 Uiso 1 1 calc R . . C93 C 0.2287(5) 0.5762(4) 0.2139(4) 0.070(2) Uani 1 1 d . . . H93 H 0.1898 0.5906 0.2213 0.084 Uiso 1 1 calc R . . C4 C 0.5709(4) 0.7396(4) 0.2524(3) 0.0611(18) Uani 1 1 d . . . H4 H 0.5436 0.7656 0.2665 0.073 Uiso 1 1 calc R . . C95 C 0.0273(5) 0.4620(5) -0.1765(4) 0.076(2) Uani 1 1 d . . . H95C H -0.0259 0.4557 -0.2084 0.114 Uiso 1 1 calc R . . H95A H 0.0164 0.4254 -0.1549 0.114 Uiso 1 1 calc R . . H95B H 0.0580 0.4527 -0.2016 0.114 Uiso 1 1 calc R . . C96 C 0.5599(6) 0.8013(5) 0.7146(4) 0.079(2) Uani 1 1 d . . . H96 H 0.5458 0.7489 0.7017 0.095 Uiso 1 1 calc R . . C97 C 0.6428(5) 0.8568(4) 0.7415(3) 0.0600(17) Uani 1 1 d . . . H97 H 0.6839 0.8408 0.7461 0.072 Uiso 1 1 calc R . . C98 C 0.4972(5) 0.8226(5) 0.7064(4) 0.077(2) Uani 1 1 d . . . H98 H 0.4405 0.7847 0.6874 0.093 Uiso 1 1 calc R . . C99 C 1.3163(6) 1.0595(5) 0.5766(5) 0.089(3) Uani 1 1 d . . . H99 H 1.2630 1.0528 0.5487 0.107 Uiso 1 1 calc R . . C100 C 0.6822(5) 1.0681(5) 1.0142(5) 0.090(3) Uani 1 1 d . . . H10 H 0.6857 1.1070 0.9972 0.107 Uiso 1 1 calc R . . C101 C 0.8115(6) 0.5429(7) 0.2468(5) 0.107(3) Uani 1 1 d . . . H10D H 0.7875 0.4888 0.2296 0.128 Uiso 1 1 calc R . . C103 C 0.5082(7) 0.9162(5) 0.1648(5) 0.092(3) Uani 1 1 d . . . H10B H 0.5320 0.9654 0.1996 0.110 Uiso 1 1 calc R . . C104 C 1.2057(6) 0.7545(6) 0.3822(4) 0.084(2) Uani 1 1 d . . . H10E H 1.2666 0.7925 0.4040 0.101 Uiso 1 1 calc R . . C105 C 1.3211(5) 1.0087(5) 0.6071(4) 0.076(2) Uani 1 1 d . . . C108 C 0.6686(6) 0.9534(5) 1.0642(5) 0.089(3) Uani 1 1 d . . . H10A H 0.6657 0.9154 1.0823 0.107 Uiso 1 1 calc R . . C109 C 0.3947(5) 0.6520(7) -0.1841(4) 0.091(3) Uani 1 1 d . . . H10C H 0.3945 0.6128 -0.2164 0.109 Uiso 1 1 calc R . . C111 C 0.8559(7) 1.2293(5) 1.1446(5) 0.099(3) Uani 1 1 d . . . H11 H 0.7969 1.2043 1.1273 0.119 Uiso 1 1 calc R . . C112 C 0.6018(7) 1.0163(7) 1.0066(7) 0.127(4) Uani 1 1 d . . . H11A H 0.5531 1.0204 0.9848 0.152 Uiso 1 1 calc R . . C113 C 1.3930(10) 1.1244(7) 0.5867(7) 0.125(4) Uani 1 1 d . . . H11F H 1.3896 1.1606 0.5675 0.150 Uiso 1 1 calc R . . C114 C 1.1651(6) 0.7462(5) 0.3067(4) 0.085(2) Uani 1 1 d . . . H11H H 1.1709 0.7957 0.3062 0.127 Uiso 1 1 calc R . . H11G H 1.1056 0.7083 0.2841 0.127 Uiso 1 1 calc R . . H11I H 1.1931 0.7294 0.2824 0.127 Uiso 1 1 calc R . . C115 C 0.3579(7) 0.5698(7) 0.2612(5) 0.118(4) Uani 1 1 d . . . H11C H 0.4073 0.5824 0.2999 0.141 Uiso 1 1 calc R . . C116 C 1.2480(8) 0.9107(9) 0.7636(6) 0.124(4) Uani 1 1 d . . . H11J H 1.2369 0.9287 0.8003 0.149 Uiso 1 1 calc R . . C117 C 0.3989(6) 0.7756(6) -0.1493(5) 0.094(3) Uani 1 1 d . . . H11D H 0.4014 0.8195 -0.1578 0.113 Uiso 1 1 calc R . . C118 C 0.0941(5) 0.2788(4) -0.0839(4) 0.074(2) Uani 1 1 d . . . H11E H 0.0831 0.2503 -0.1287 0.089 Uiso 1 1 calc R . . C119 C 1.4700(10) 1.1304(8) 0.6250(6) 0.128(5) Uani 1 1 d . . . H11K H 1.5192 1.1697 0.6295 0.154 Uiso 1 1 calc R . . C120 C 0.2977(7) 0.5880(7) 0.2688(4) 0.102(3) Uani 1 1 d . . . H12 H 0.3045 0.6094 0.3138 0.123 Uiso 1 1 calc R . . C121 C 0.9504(6) 0.9353(5) 0.6553(4) 0.077(2) Uani 1 1 d . . . H12C H 0.9285 0.9677 0.6434 0.093 Uiso 1 1 calc R . . C122 C 0.9445(7) 0.9137(5) 0.7108(5) 0.095(3) Uani 1 1 d . . . H12D H 0.9196 0.9323 0.7356 0.114 Uiso 1 1 calc R . . C123 C 0.3941(6) 0.7150(8) -0.1970(5) 0.102(3) Uani 1 1 d . . . H12A H 0.3903 0.7169 -0.2397 0.123 Uiso 1 1 calc R . . C125 C 1.3994(7) 1.0176(7) 0.6461(5) 0.110(3) Uani 1 1 d . . . H12E H 1.4042 0.9827 0.6666 0.132 Uiso 1 1 calc R . . C126 C 0.5576(6) 0.8826(5) 0.1595(4) 0.083(2) Uani 1 1 d . . . H12B H 0.6143 0.9075 0.1934 0.100 Uiso 1 1 calc R . . C127 C 1.2693(5) 0.8507(6) 0.6499(4) 0.084(3) Uani 1 1 d . . . H12F H 1.2750 0.8282 0.6112 0.101 Uiso 1 1 calc R . . C129 C 1.1984(8) 0.6756(8) 0.3835(5) 0.133(5) Uani 1 1 d . . . H12H H 1.2248 0.6813 0.4311 0.199 Uiso 1 1 calc R . . H12I H 1.2267 0.6595 0.3589 0.199 Uiso 1 1 calc R . . H12G H 1.1393 0.6370 0.3611 0.199 Uiso 1 1 calc R . . C130 C 1.2764(6) 0.8196(7) 0.7017(6) 0.118(4) Uani 1 1 d . . . H13A H 1.2333 0.7650 0.6799 0.141 Uiso 1 1 calc R . . H13B H 1.3318 0.8218 0.7199 0.141 Uiso 1 1 calc R . . C132 C 0.5988(7) 0.9598(6) 1.0327(6) 0.100(3) Uani 1 1 d . . . H13 H 0.5469 0.9251 1.0285 0.120 Uiso 1 1 calc R . . C2 C 0.6914(5) 0.7180(5) 0.2764(4) 0.089(3) Uani 1 1 d . . . H2 H 0.7461 0.7295 0.3064 0.107 Uiso 1 1 calc R . . C142 C 1.0300(8) 1.3013(7) 1.1954(6) 0.122(4) Uani 1 1 d . . . H14 H 1.0891 1.3270 1.2130 0.147 Uiso 1 1 calc R . . C145 C 0.9044(12) 1.2992(8) 1.2005(7) 0.132(5) Uani 1 1 d . . . H14A H 0.8786 1.3225 1.2206 0.158 Uiso 1 1 calc R . . O1 O 0.5531(2) 0.6455(2) 0.02933(19) 0.0452(9) Uani 1 1 d . . . H1A H 0.5247 0.6380 -0.0123 0.068 Uiso 1 1 d R . . H1B H 0.5994 0.6845 0.0511 0.068 Uiso 1 1 d R . . O2 O 0.9190(3) 1.0003(3) 1.0711(2) 0.0593(11) Uani 1 1 d . . . H2A H 0.9095 0.9655 1.0872 0.089 Uiso 1 1 d R . . H2B H 0.9701 1.0335 1.0991 0.089 Uiso 1 1 d R . . C207 C 0.9901(14) 1.3346(8) 1.2265(6) 0.150(7) Uani 1 1 d . . . H20 H 1.0234 1.3816 1.2657 0.181 Uiso 1 1 calc R . . C211 C 1.2672(7) 0.8575(9) 0.7574(6) 0.114(4) Uani 1 1 d . . . H21A H 1.2766 0.8412 0.7942 0.137 Uiso 1 1 calc R . . C212 C 1.4771(8) 1.0835(9) 0.6553(6) 0.139(5) Uani 1 1 d . . . H21B H 1.5310 1.0911 0.6830 0.167 Uiso 1 1 calc R . . C220 C 1.0545(4) 0.8365(4) 0.5928(3) 0.0594(17) Uani 1 1 d . . . H22A H 1.0745 0.8014 0.5995 0.071 Uiso 1 1 calc R . . Ni3 Ni 1.01274(6) 0.94364(5) 0.54350(4) 0.0631(3) Uani 1 1 d . . . Cl10 Cl 1.04988(11) 0.97020(10) 0.45565(8) 0.0596(4) Uani 1 1 d . . . Cl11 Cl 1.14492(13) 1.05817(11) 0.63586(9) 0.0705(5) Uani 1 1 d . . . O3 O 0.8727(3) 0.8470(3) 0.4537(2) 0.0694(13) Uani 1 1 d . . . H3A H 0.8566 0.8514 0.4151 0.104 Uiso 1 1 d R . . H3B H 0.8384 0.8092 0.4572 0.104 Uiso 1 1 d R . . C235 C 0.9909(9) 0.6017(8) 0.5369(6) 0.146(5) Uiso 1 1 d DU . . H23 H 1.0258 0.5795 0.5498 0.175 Uiso 1 1 calc R . . C231 C 0.8823(10) 0.6691(10) 0.4970(8) 0.185(6) Uiso 1 1 d DU . . H23A H 0.8482 0.6921 0.4842 0.222 Uiso 1 1 calc R . . C232 C 0.8695(11) 0.6299(10) 0.5410(8) 0.185(6) Uiso 1 1 d DU . . H23B H 0.8274 0.6241 0.5554 0.223 Uiso 1 1 calc R . . C233 C 0.9262(12) 0.6002(11) 0.5612(10) 0.200(7) Uiso 1 1 d DU . . H23C H 0.9229 0.5772 0.5930 0.240 Uiso 1 1 calc R . . C234 C 0.9926(6) 0.6413(6) 0.4915(5) 0.104(3) Uiso 1 1 d DU . . H23D H 1.0312 0.6443 0.4735 0.125 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 0.0300(3) 0.0283(3) 0.0342(3) 0.0086(3) 0.0155(3) 0.0126(3) N1 0.034(2) 0.042(3) 0.040(2) 0.007(2) 0.012(2) 0.018(2) Ni2 0.0371(4) 0.0345(4) 0.0495(4) 0.0181(3) 0.0224(3) 0.0155(3) N2 0.036(2) 0.025(2) 0.041(2) 0.0105(17) 0.0215(19) 0.0149(18) N3 0.043(3) 0.037(2) 0.053(3) 0.020(2) 0.025(2) 0.019(2) Cl2 0.0326(6) 0.0348(6) 0.0360(6) 0.0077(5) 0.0146(5) 0.0146(5) N4 0.032(2) 0.031(2) 0.039(2) 0.0116(18) 0.0153(18) 0.0089(19) Cl5 0.0383(7) 0.0370(7) 0.0501(7) 0.0203(6) 0.0218(6) 0.0157(6) Cl1 0.0507(8) 0.0429(7) 0.0533(8) 0.0222(6) 0.0303(6) 0.0241(7) C12 0.037(3) 0.024(2) 0.034(2) 0.0114(19) 0.017(2) 0.013(2) Cl7 0.0486(8) 0.0509(8) 0.0501(8) 0.0192(6) 0.0262(6) 0.0240(7) C140 0.036(3) 0.032(3) 0.050(3) 0.015(2) 0.020(2) 0.014(2) C92 0.033(3) 0.034(3) 0.038(3) 0.014(2) 0.021(2) 0.015(2) C94 0.033(3) 0.035(3) 0.046(3) 0.011(2) 0.015(2) 0.013(2) N6 0.061(3) 0.053(3) 0.046(3) 0.015(2) 0.033(2) 0.023(3) C206 0.055(4) 0.072(5) 0.061(4) 0.008(3) 0.021(3) 0.026(4) C6 0.035(3) 0.037(3) 0.047(3) 0.014(2) 0.021(2) 0.016(2) C15 0.041(3) 0.034(3) 0.043(3) 0.015(2) 0.022(2) 0.017(2) C16 0.036(3) 0.034(3) 0.040(3) 0.012(2) 0.022(2) 0.014(2) C7 0.036(3) 0.030(2) 0.031(2) 0.0089(19) 0.018(2) 0.016(2) C19 0.032(3) 0.038(3) 0.039(3) 0.019(2) 0.018(2) 0.016(2) C10 0.038(3) 0.038(3) 0.033(3) 0.013(2) 0.017(2) 0.016(2) C21 0.044(3) 0.031(3) 0.052(3) 0.010(2) 0.027(3) 0.013(2) C22 0.052(3) 0.033(3) 0.034(3) 0.015(2) 0.022(2) 0.017(3) C5 0.039(3) 0.049(3) 0.041(3) 0.014(2) 0.022(2) 0.022(3) C24 0.036(3) 0.033(3) 0.052(3) 0.020(2) 0.021(2) 0.015(2) C25 0.042(3) 0.039(3) 0.041(3) 0.014(2) 0.023(2) 0.018(2) C26 0.044(3) 0.037(3) 0.041(3) 0.011(2) 0.017(2) 0.020(3) C9 0.036(3) 0.042(3) 0.045(3) 0.019(2) 0.018(2) 0.019(2) C11 0.031(3) 0.034(3) 0.049(3) 0.012(2) 0.018(2) 0.010(2) C29 0.050(4) 0.047(3) 0.072(4) 0.027(3) 0.034(3) 0.023(3) C30 0.042(3) 0.039(3) 0.053(3) 0.021(3) 0.024(3) 0.017(3) C31 0.041(3) 0.032(3) 0.054(3) 0.017(2) 0.026(3) 0.017(2) C32 0.052(3) 0.040(3) 0.055(3) 0.021(3) 0.032(3) 0.020(3) C33 0.047(3) 0.034(3) 0.052(3) 0.008(2) 0.029(3) 0.018(3) N8 0.083(4) 0.059(3) 0.053(3) 0.023(3) 0.042(3) 0.033(3) C35 0.047(3) 0.039(3) 0.050(3) 0.019(2) 0.027(3) 0.018(3) C36 0.051(3) 0.038(3) 0.043(3) 0.014(2) 0.023(3) 0.018(3) C37 0.050(4) 0.052(4) 0.039(3) 0.012(3) 0.018(3) 0.018(3) C38 0.047(3) 0.051(4) 0.063(4) 0.029(3) 0.025(3) 0.019(3) C39 0.049(3) 0.037(3) 0.055(3) 0.017(2) 0.027(3) 0.023(3) C40 0.040(3) 0.044(3) 0.060(3) 0.025(3) 0.024(3) 0.020(3) C85 0.080(5) 0.062(4) 0.049(3) 0.023(3) 0.042(3) 0.039(4) C42 0.041(3) 0.046(3) 0.048(3) 0.019(3) 0.023(3) 0.015(3) C43 0.059(4) 0.050(4) 0.063(4) 0.015(3) 0.032(3) 0.016(3) C44 0.060(4) 0.045(4) 0.064(4) 0.011(3) 0.027(3) 0.024(3) C45 0.048(4) 0.052(4) 0.099(5) 0.041(4) 0.033(4) 0.020(3) C47 0.045(3) 0.037(3) 0.042(3) 0.011(2) 0.020(2) 0.019(3) C48 0.051(4) 0.042(3) 0.072(4) 0.026(3) 0.030(3) 0.021(3) C49 0.063(4) 0.083(5) 0.055(4) 0.011(4) 0.030(3) 0.034(4) C50 0.054(4) 0.046(4) 0.081(4) 0.034(3) 0.033(3) 0.020(3) C51 0.054(4) 0.064(4) 0.049(3) 0.017(3) 0.021(3) 0.023(3) C52 0.057(4) 0.048(3) 0.050(3) 0.021(3) 0.029(3) 0.030(3) C53 0.055(4) 0.074(5) 0.070(4) 0.030(4) 0.033(3) 0.021(4) C54 0.042(3) 0.046(3) 0.073(4) 0.030(3) 0.025(3) 0.021(3) C55 0.057(4) 0.058(4) 0.041(3) 0.009(3) 0.026(3) 0.026(3) C56 0.059(4) 0.049(4) 0.074(4) 0.023(3) 0.030(3) 0.030(3) C57 0.093(6) 0.069(5) 0.077(5) 0.033(4) 0.057(5) 0.047(5) C58 0.062(4) 0.052(4) 0.056(4) 0.013(3) 0.031(3) 0.026(3) C59 0.053(4) 0.075(5) 0.039(3) 0.005(3) 0.018(3) 0.026(4) C60 0.051(4) 0.052(4) 0.072(4) 0.019(3) 0.028(3) 0.012(3) C61 0.086(5) 0.069(5) 0.077(5) 0.037(4) 0.050(4) 0.039(4) C62 0.062(4) 0.074(5) 0.044(3) 0.017(3) 0.028(3) 0.030(4) C1 0.049(4) 0.066(4) 0.053(4) 0.008(3) 0.020(3) 0.028(3) C64 0.082(5) 0.046(4) 0.046(3) 0.020(3) 0.028(3) 0.025(4) C65 0.058(4) 0.052(4) 0.056(4) 0.018(3) 0.030(3) 0.022(3) C66 0.074(4) 0.053(4) 0.040(3) 0.019(3) 0.032(3) 0.035(3) C67 0.129(7) 0.086(6) 0.087(5) 0.055(5) 0.079(5) 0.065(6) C68 0.074(5) 0.115(7) 0.061(4) 0.018(5) 0.034(4) 0.051(5) C69 0.072(5) 0.109(6) 0.073(5) 0.043(4) 0.039(4) 0.061(5) C70 0.046(4) 0.075(5) 0.069(4) 0.006(4) 0.014(3) 0.030(4) C71 0.072(5) 0.072(5) 0.052(4) 0.018(3) 0.033(3) 0.039(4) C72 0.075(5) 0.066(5) 0.083(5) 0.044(4) 0.032(4) 0.032(4) C74 0.054(4) 0.058(4) 0.096(6) 0.043(4) 0.035(4) 0.024(4) C75 0.062(5) 0.047(4) 0.088(6) 0.021(4) 0.012(4) 0.016(4) C76 0.075(5) 0.077(5) 0.069(5) 0.025(4) 0.035(4) 0.034(4) C77 0.096(6) 0.087(6) 0.052(4) 0.011(4) 0.042(4) 0.005(5) C8 0.058(4) 0.047(4) 0.081(5) 0.015(3) 0.033(4) 0.018(3) C80 0.085(6) 0.063(5) 0.099(6) 0.015(4) 0.056(5) 0.031(5) C81 0.072(5) 0.074(5) 0.050(4) 0.014(3) 0.034(3) 0.033(4) C84 0.078(6) 0.075(5) 0.068(5) 0.021(4) 0.016(4) 0.021(5) C34 0.094(6) 0.065(4) 0.063(4) 0.028(4) 0.044(4) 0.039(4) C86 0.054(5) 0.144(10) 0.076(6) 0.007(6) 0.021(4) 0.050(6) C87 0.092(6) 0.118(8) 0.069(5) 0.029(5) 0.041(5) 0.069(6) C88 0.072(5) 0.075(5) 0.083(5) 0.032(4) 0.050(4) 0.042(4) C89 0.050(4) 0.080(6) 0.081(5) 0.021(4) 0.023(4) 0.024(4) C90 0.098(7) 0.095(7) 0.063(5) 0.014(4) 0.036(5) 0.029(6) C91 0.061(5) 0.082(6) 0.057(4) 0.021(4) 0.024(4) 0.015(4) C3 0.061(5) 0.094(6) 0.068(5) -0.012(4) 0.020(4) 0.031(5) C93 0.083(5) 0.076(5) 0.074(5) 0.033(4) 0.044(4) 0.052(4) C4 0.048(4) 0.061(4) 0.049(3) -0.003(3) 0.012(3) 0.026(3) C95 0.058(4) 0.091(6) 0.062(4) 0.014(4) 0.019(3) 0.037(4) C96 0.086(6) 0.058(5) 0.083(5) 0.030(4) 0.036(5) 0.025(5) C97 0.063(4) 0.050(4) 0.063(4) 0.021(3) 0.027(3) 0.026(3) C98 0.063(5) 0.065(5) 0.084(5) 0.030(4) 0.031(4) 0.015(4) C99 0.104(7) 0.066(5) 0.092(6) 0.020(5) 0.056(5) 0.032(5) C100 0.081(6) 0.096(6) 0.136(8) 0.074(6) 0.071(6) 0.049(5) C101 0.071(6) 0.127(8) 0.064(5) 0.005(5) 0.016(4) 0.025(6) C103 0.116(8) 0.051(4) 0.085(6) 0.010(4) 0.061(6) 0.015(5) C104 0.076(5) 0.098(6) 0.077(5) 0.022(5) 0.044(4) 0.043(5) C105 0.059(5) 0.084(6) 0.061(4) 0.019(4) 0.028(4) 0.016(4) C108 0.101(7) 0.060(5) 0.119(7) 0.045(5) 0.066(6) 0.031(5) C109 0.060(5) 0.128(8) 0.063(5) 0.027(5) 0.031(4) 0.028(5) C111 0.147(9) 0.059(5) 0.100(6) 0.030(5) 0.083(6) 0.035(6) C112 0.109(8) 0.135(10) 0.194(12) 0.090(10) 0.101(9) 0.072(8) C113 0.171(12) 0.086(7) 0.138(10) 0.037(7) 0.114(10) 0.045(9) C114 0.092(6) 0.089(6) 0.076(5) 0.018(4) 0.049(5) 0.044(5) C115 0.123(8) 0.179(11) 0.069(5) 0.031(6) 0.047(6) 0.099(9) C116 0.107(9) 0.178(14) 0.081(7) 0.044(8) 0.053(6) 0.056(9) C117 0.081(6) 0.095(7) 0.087(6) 0.058(6) 0.024(5) 0.024(5) C118 0.080(5) 0.052(4) 0.074(5) 0.022(4) 0.031(4) 0.021(4) C119 0.140(12) 0.119(10) 0.089(8) 0.030(7) 0.063(8) 0.024(9) C120 0.116(8) 0.151(9) 0.062(5) 0.035(5) 0.046(5) 0.085(7) C121 0.114(7) 0.072(5) 0.081(5) 0.041(4) 0.065(5) 0.054(5) C122 0.157(9) 0.087(6) 0.090(6) 0.045(5) 0.091(6) 0.069(6) C123 0.084(6) 0.138(10) 0.075(6) 0.064(7) 0.029(5) 0.038(7) C125 0.114(8) 0.126(9) 0.099(7) 0.060(6) 0.064(7) 0.044(7) C126 0.068(5) 0.063(5) 0.069(5) 0.010(4) 0.018(4) 0.005(4) C127 0.064(5) 0.110(7) 0.064(5) 0.038(5) 0.023(4) 0.031(5) C129 0.154(11) 0.183(13) 0.099(7) 0.042(8) 0.067(7) 0.116(10) C130 0.071(6) 0.147(10) 0.129(9) 0.074(8) 0.034(6) 0.045(7) C132 0.085(7) 0.080(6) 0.144(9) 0.052(6) 0.069(6) 0.029(5) C2 0.056(4) 0.103(6) 0.059(4) -0.015(4) 0.005(3) 0.038(5) C142 0.117(9) 0.095(8) 0.089(7) 0.030(6) 0.008(6) 0.024(7) C145 0.234(16) 0.103(10) 0.110(9) 0.048(8) 0.120(11) 0.090(11) O1 0.049(2) 0.043(2) 0.049(2) 0.0195(17) 0.0261(18) 0.0237(19) O2 0.048(2) 0.063(3) 0.070(3) 0.028(2) 0.031(2) 0.026(2) C207 0.29(2) 0.094(9) 0.071(7) 0.037(6) 0.076(11) 0.096(13) C211 0.099(8) 0.160(12) 0.075(7) 0.055(8) 0.050(6) 0.040(8) C212 0.096(8) 0.169(13) 0.091(8) 0.032(8) 0.041(6) 0.016(8) C220 0.065(4) 0.053(4) 0.049(3) 0.010(3) 0.026(3) 0.024(3) Ni3 0.0863(7) 0.0625(6) 0.0591(5) 0.0272(4) 0.0483(5) 0.0384(5) Cl10 0.0753(11) 0.0578(9) 0.0587(9) 0.0232(7) 0.0440(8) 0.0327(9) Cl11 0.0884(13) 0.0611(10) 0.0632(10) 0.0204(8) 0.0440(9) 0.0313(10) O3 0.116(4) 0.061(3) 0.071(3) 0.042(2) 0.065(3) 0.052(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 Ni1 N1 2.063(4) . ? Ni1 N2 2.150(4) . ? Ni1 O1 2.186(4) . ? Ni1 Cl1 2.3631(16) . ? Ni1 Cl2 2.371(2) 2_665 ? Ni1 Cl2 2.4773(15) . ? N1 C1 1.324(7) . ? N1 C5 1.345(7) . ? Ni2 N3 2.053(5) . ? Ni2 N4 2.114(4) . ? Ni2 O2 2.233(4) . ? Ni2 Cl5 2.3670(19) 2_777 ? Ni2 Cl7 2.3785(18) . ? Ni2 Cl5 2.4288(16) . ? N2 C6 1.274(6) . ? N2 C7 1.446(6) . ? N3 C54 1.339(7) . ? N3 C140 1.355(7) . ? Cl2 Ni1 2.371(2) 2_665 ? N4 C94 1.286(7) . ? N4 C31 1.474(7) . ? Cl5 Ni2 2.3670(19) 2_777 ? C12 C7 1.374(7) . ? C12 C11 1.413(7) . ? C12 C92 1.540(7) . ? C140 C40 1.381(8) . ? C140 C94 1.443(7) . ? C92 C24 1.529(7) . ? C92 C30 1.549(7) . ? C92 H92 0.9800 . ? C94 H94 0.9300 . ? C205 C234 1.408(8) . ? C205 C231 1.410(9) . ? C205 C206 1.507(11) . ? N6 C220 1.263(8) . ? N6 C37 1.440(8) . ? N6 Ni3 2.121(6) . ? C206 C49 1.543(9) . ? C206 C55 1.545(10) . ? C206 H20A 0.9800 . ? C6 C5 1.463(7) . ? C6 H6 0.9300 . ? C15 C7 1.405(7) . ? C15 C9 1.412(7) . ? C15 C19 1.517(7) . ? C16 C21 1.388(7) . ? C16 C31 1.395(7) . ? C16 C32 1.524(8) . ? C19 C35 1.498(7) . ? C19 C42 1.540(7) . ? C19 H19 0.9800 . ? C10 C11 1.384(7) . ? C10 C9 1.414(7) . ? C10 C38 1.499(8) . ? C21 C25 1.394(8) . ? C21 H21 0.9300 . ? C22 C47 1.368(7) . ? C22 C25 1.386(7) . ? C22 H22 0.9300 . ? C5 C4 1.378(8) . ? C24 C43 1.357(8) . ? C24 C29 1.383(8) . ? C25 C39 1.526(7) . ? C26 C47 1.505(7) . ? C26 C36 1.507(8) . ? C26 C33 1.511(8) . ? C26 H26 0.9800 . ? C9 H9 0.9300 . ? C11 H11B 0.9300 . ? C29 C74 1.422(9) . ? C29 H29 0.9300 . ? C30 C69 1.346(9) . ? C30 C52 1.391(8) . ? C31 C47 1.401(8) . ? C32 C64 1.540(8) . ? C32 C65 1.541(9) . ? C32 H32 0.9800 . ? C33 C71 1.374(9) . ? C33 C58 1.388(9) . ? N8 C85 1.338(8) . ? N8 C121 1.362(9) . ? N8 Ni3 2.066(5) . ? C35 C8 1.410(9) . ? C35 C60 1.413(9) . ? C36 C97 1.391(8) . ? C36 C44 1.394(9) . ? C37 C66 1.366(9) . ? C37 C55 1.417(8) . ? C38 C70 1.530(9) . ? C38 C95 1.539(9) . ? C38 H38 0.9800 . ? C39 C48 1.506(8) . ? C39 C56 1.561(8) . ? C39 H39 0.9800 . ? C40 C45 1.396(8) . ? C40 H40 0.9300 . ? C85 C34 1.369(9) . ? C85 C220 1.465(9) . ? C42 C72 1.366(9) . ? C42 C53 1.376(10) . ? C43 C118 1.377(10) . ? C43 H43 0.9300 . ? C44 C89 1.402(10) . ? C44 H44 0.9300 . ? C45 C50 1.392(9) . ? C45 H45 0.9300 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C48 H48A 0.9600 . ? C49 C90 1.343(12) . ? C49 C68 1.389(12) . ? C50 C54 1.379(8) . ? C50 H50 0.9300 . ? C51 C66 1.393(9) . ? C51 C62 1.398(9) . ? C51 H51 0.9300 . ? C52 C93 1.374(9) . ? C52 H52 0.9300 . ? C53 C109 1.423(11) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C59 1.375(9) . ? C56 H56B 0.9600 . ? C56 H56A 0.9600 . ? C56 H56C 0.9600 . ? C57 C76 1.304(11) . ? C57 C88 1.375(10) . ? C57 H57 0.9300 . ? C58 C88 1.391(9) . ? C58 H58 0.9300 . ? C59 C62 1.380(9) . ? C59 H59 0.9300 . ? C60 C126 1.412(10) . ? C60 H60 0.9300 . ? C61 C65 1.381(9) . ? C61 C108 1.386(11) . ? C61 H61 0.9300 . ? C62 C104 1.499(10) . ? C1 C2 1.417(9) . ? C1 H1 0.9300 . ? C64 C84 1.373(11) . ? C64 C111 1.398(11) . ? C65 C100 1.335(10) . ? C66 C81 1.542(9) . ? C67 C122 1.357(11) . ? C67 C34 1.422(10) . ? C67 H67 0.9300 . ? C68 C87 1.444(11) . ? C68 H68 0.9300 . ? C69 C115 1.436(11) . ? C69 H69 0.9300 . ? C70 H70C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C71 C76 1.406(10) . ? C71 H71 0.9300 . ? C72 C117 1.425(11) . ? C72 H72 0.9300 . ? C74 C75 1.285(11) . ? C74 H74 0.9300 . ? C75 C118 1.375(11) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 C116 1.390(14) . ? C77 C91 1.412(11) . ? C77 H77 0.9300 . ? C8 C80 1.354(10) . ? C8 H8 0.9300 . ? C80 C103 1.386(12) . ? C80 H80 0.9300 . ? C81 C105 1.503(11) . ? C81 C91 1.525(11) . ? C81 H81 0.9800 . ? C84 C142 1.403(13) . ? C84 H84 0.9300 . ? C34 H34 0.9300 . ? C86 C87 1.319(13) . ? C86 C101 1.387(14) . ? C86 H86 0.9300 . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? C89 C98 1.366(11) . ? C89 H89 0.9300 . ? C90 C101 1.430(11) . ? C90 H90 0.9300 . ? C91 C127 1.346(12) . ? C3 C2 1.370(11) . ? C3 C4 1.375(10) . ? C3 H3 0.9300 . ? C93 C120 1.350(11) . ? C93 H93 0.9300 . ? C4 H4 0.9300 . ? C95 H95C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C96 C97 1.361(10) . ? C96 C98 1.372(11) . ? C96 H96 0.9300 . ? C97 H97 0.9300 . ? C98 H98 0.9300 . ? C99 C105 1.355(12) . ? C99 C113 1.457(14) . ? C99 H99 0.9300 . ? C100 C112 1.421(13) . ? C100 H10 0.9300 . ? C101 H10D 0.9300 . ? C103 C126 1.356(12) . ? C103 H10B 0.9300 . ? C104 C114 1.524(11) . ? C104 C129 1.544(14) . ? C104 H10E 0.9800 . ? C105 C125 1.363(13) . ? C108 C132 1.341(13) . ? C108 H10A 0.9300 . ? C109 C123 1.359(14) . ? C109 H10C 0.9300 . ? C111 C145 1.361(15) . ? C111 H11 0.9300 . ? C112 C132 1.373(14) . ? C112 H11A 0.9300 . ? C113 C119 1.363(17) . ? C113 H11F 0.9300 . ? C114 H11H 0.9600 . ? C114 H11G 0.9600 . ? C114 H11I 0.9600 . ? C115 C120 1.363(12) . ? C115 H11C 0.9300 . ? C116 C211 1.241(16) . ? C116 H11J 0.9300 . ? C117 C123 1.366(14) . ? C117 H11D 0.9300 . ? C118 H11E 0.9300 . ? C119 C212 1.291(17) . ? C119 H11K 0.9300 . ? C120 H12 0.9300 . ? C121 C122 1.412(10) . ? C121 H12C 0.9300 . ? C122 H12D 0.9300 . ? C123 H12A 0.9300 . ? C125 C212 1.485(15) . ? C125 H12E 0.9300 . ? C126 H12B 0.9300 . ? C127 C130 1.413(12) . ? C127 H12F 0.9300 . ? C129 H12H 0.9600 . ? C129 H12I 0.9600 . ? C129 H12G 0.9600 . ? C130 C211 1.390(16) . ? C130 H13A 0.9700 . ? C130 H13B 0.9700 . ? C132 H13 0.9300 . ? C2 H2 0.9300 . ? C142 C207 1.411(19) . ? C142 H14 0.9300 . ? C145 C207 1.35(2) . ? C145 H14A 0.9300 . ? O1 H1A 0.8401 . ? O1 H1B 0.8121 . ? O2 H2A 0.8401 . ? O2 H2B 0.8400 . ? C207 H20 0.9300 . ? C211 H21A 0.9300 . ? C212 H21B 0.9300 . ? C220 H22A 0.9300 . ? Ni3 Cl10 2.3729(18) . ? Ni3 O3 2.390(6) . ? Ni3 Cl10 2.425(2) 2_776 ? Ni3 Cl11 2.443(3) . ? Cl10 Ni3 2.425(2) 2_776 ? O3 H3A 0.8404 . ? O3 H3B 0.8400 . ? C235 C234 1.413(8) . ? C235 C233 1.48(2) . ? C235 H23 0.9300 . ? C231 C232 1.408(9) . ? C231 H23A 0.9300 . ? C232 C233 1.404(9) . ? C232 H23B 0.9300 . ? C233 H23C 0.9300 . ? C234 H23D 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 79.10(17) . . ? N1 Ni1 O1 88.23(17) . . ? N2 Ni1 O1 91.89(15) . . ? N1 Ni1 Cl1 91.36(14) . . ? N2 Ni1 Cl1 98.71(12) . . ? O1 Ni1 Cl1 169.12(11) . . ? N1 Ni1 Cl2 170.51(13) . 2_665 ? N2 Ni1 Cl2 92.77(12) . 2_665 ? O1 Ni1 Cl2 87.15(11) . 2_665 ? Cl1 Ni1 Cl2 94.73(6) . 2_665 ? N1 Ni1 Cl2 95.71(13) . . ? N2 Ni1 Cl2 171.17(11) . . ? O1 Ni1 Cl2 80.74(11) . . ? Cl1 Ni1 Cl2 88.49(5) . . ? Cl2 Ni1 Cl2 91.73(5) 2_665 . ? C1 N1 C5 118.4(5) . . ? C1 N1 Ni1 127.2(4) . . ? C5 N1 Ni1 114.3(3) . . ? N3 Ni2 N4 79.22(17) . . ? N3 Ni2 O2 87.35(18) . . ? N4 Ni2 O2 92.35(16) . . ? N3 Ni2 Cl5 168.20(14) . 2_777 ? N4 Ni2 Cl5 91.82(12) . 2_777 ? O2 Ni2 Cl5 85.35(13) . 2_777 ? N3 Ni2 Cl7 92.64(15) . . ? N4 Ni2 Cl7 97.24(13) . . ? O2 Ni2 Cl7 170.24(12) . . ? Cl5 Ni2 Cl7 96.12(7) 2_777 . ? N3 Ni2 Cl5 95.79(13) . . ? N4 Ni2 Cl5 171.25(13) . . ? O2 Ni2 Cl5 80.17(12) . . ? Cl5 Ni2 Cl5 92.09(6) 2_777 . ? Cl7 Ni2 Cl5 90.13(6) . . ? C6 N2 C7 116.8(4) . . ? C6 N2 Ni1 110.9(3) . . ? C7 N2 Ni1 132.3(3) . . ? C54 N3 C140 117.4(5) . . ? C54 N3 Ni2 128.2(4) . . ? C140 N3 Ni2 114.4(3) . . ? Ni1 Cl2 Ni1 88.27(5) 2_665 . ? C94 N4 C31 116.8(5) . . ? C94 N4 Ni2 111.6(4) . . ? C31 N4 Ni2 131.6(3) . . ? Ni2 Cl5 Ni2 87.91(6) 2_777 . ? C7 C12 C11 118.1(4) . . ? C7 C12 C92 120.9(4) . . ? C11 C12 C92 121.0(4) . . ? N3 C140 C40 123.5(5) . . ? N3 C140 C94 114.2(5) . . ? C40 C140 C94 122.3(5) . . ? C24 C92 C12 111.7(4) . . ? C24 C92 C30 114.3(4) . . ? C12 C92 C30 110.2(4) . . ? C24 C92 H92 106.7 . . ? C12 C92 H92 106.7 . . ? C30 C92 H92 106.7 . . ? N4 C94 C140 120.6(5) . . ? N4 C94 H94 119.7 . . ? C140 C94 H94 119.7 . . ? C234 C205 C231 115.2(11) . . ? C234 C205 C206 123.9(8) . . ? C231 C205 C206 120.9(10) . . ? C220 N6 C37 118.2(6) . . ? C220 N6 Ni3 112.6(5) . . ? C37 N6 Ni3 129.3(4) . . ? C205 C206 C49 112.9(7) . . ? C205 C206 C55 109.7(6) . . ? C49 C206 C55 111.5(6) . . ? C205 C206 H20A 107.5 . . ? C49 C206 H20A 107.5 . . ? C55 C206 H20A 107.5 . . ? N2 C6 C5 120.8(5) . . ? N2 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C7 C15 C9 117.5(5) . . ? C7 C15 C19 120.6(4) . . ? C9 C15 C19 121.9(5) . . ? C21 C16 C31 117.1(5) . . ? C21 C16 C32 123.2(5) . . ? C31 C16 C32 119.6(5) . . ? C12 C7 C15 122.6(4) . . ? C12 C7 N2 120.7(4) . . ? C15 C7 N2 116.6(4) . . ? C35 C19 C15 112.5(4) . . ? C35 C19 C42 112.6(4) . . ? C15 C19 C42 113.1(4) . . ? C35 C19 H19 105.9 . . ? C15 C19 H19 105.9 . . ? C42 C19 H19 105.9 . . ? C11 C10 C9 117.7(5) . . ? C11 C10 C38 122.9(5) . . ? C9 C10 C38 119.4(5) . . ? C16 C21 C25 122.5(5) . . ? C16 C21 H21 118.7 . . ? C25 C21 H21 118.7 . . ? C47 C22 C25 124.2(5) . . ? C47 C22 H22 117.9 . . ? C25 C22 H22 117.9 . . ? N1 C5 C4 123.1(5) . . ? N1 C5 C6 114.9(5) . . ? C4 C5 C6 122.0(5) . . ? C43 C24 C29 117.5(6) . . ? C43 C24 C92 119.5(5) . . ? C29 C24 C92 123.0(5) . . ? C22 C25 C21 116.8(5) . . ? C22 C25 C39 122.3(5) . . ? C21 C25 C39 120.8(5) . . ? C47 C26 C36 111.0(5) . . ? C47 C26 C33 112.5(5) . . ? C36 C26 C33 115.0(4) . . ? C47 C26 H26 105.9 . . ? C36 C26 H26 105.9 . . ? C33 C26 H26 105.9 . . ? C15 C9 C10 121.6(5) . . ? C15 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C10 C11 C12 122.4(5) . . ? C10 C11 H11B 118.8 . . ? C12 C11 H11B 118.8 . . ? C24 C29 C74 120.2(7) . . ? C24 C29 H29 119.9 . . ? C74 C29 H29 119.9 . . ? C69 C30 C52 120.7(6) . . ? C69 C30 C92 118.8(6) . . ? C52 C30 C92 120.5(5) . . ? C16 C31 C47 122.7(5) . . ? C16 C31 N4 118.7(5) . . ? C47 C31 N4 118.6(5) . . ? C16 C32 C64 113.9(5) . . ? C16 C32 C65 110.0(5) . . ? C64 C32 C65 113.4(5) . . ? C16 C32 H32 106.3 . . ? C64 C32 H32 106.3 . . ? C65 C32 H32 106.3 . . ? C71 C33 C58 116.8(6) . . ? C71 C33 C26 124.3(6) . . ? C58 C33 C26 118.9(5) . . ? C85 N8 C121 118.5(6) . . ? C85 N8 Ni3 114.8(4) . . ? C121 N8 Ni3 126.5(5) . . ? C8 C35 C60 118.7(6) . . ? C8 C35 C19 123.7(5) . . ? C60 C35 C19 117.6(6) . . ? C97 C36 C44 115.7(6) . . ? C97 C36 C26 121.7(6) . . ? C44 C36 C26 122.6(5) . . ? C66 C37 C55 120.0(6) . . ? C66 C37 N6 120.9(5) . . ? C55 C37 N6 119.1(5) . . ? C10 C38 C70 112.4(5) . . ? C10 C38 C95 111.8(5) . . ? C70 C38 C95 108.3(6) . . ? C10 C38 H38 108.0 . . ? C70 C38 H38 108.0 . . ? C95 C38 H38 108.0 . . ? C48 C39 C25 110.2(5) . . ? C48 C39 C56 110.4(5) . . ? C25 C39 C56 111.0(5) . . ? C48 C39 H39 108.4 . . ? C25 C39 H39 108.4 . . ? C56 C39 H39 108.4 . . ? C140 C40 C45 117.5(5) . . ? C140 C40 H40 121.2 . . ? C45 C40 H40 121.2 . . ? N8 C85 C34 123.4(6) . . ? N8 C85 C220 114.0(6) . . ? C34 C85 C220 122.6(7) . . ? C72 C42 C53 119.3(7) . . ? C72 C42 C19 124.5(6) . . ? C53 C42 C19 116.1(6) . . ? C24 C43 C118 121.6(7) . . ? C24 C43 H43 119.2 . . ? C118 C43 H43 119.2 . . ? C36 C44 C89 121.6(6) . . ? C36 C44 H44 119.2 . . ? C89 C44 H44 119.2 . . ? C50 C45 C40 119.9(6) . . ? C50 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C22 C47 C31 116.5(5) . . ? C22 C47 C26 122.9(5) . . ? C31 C47 C26 120.4(5) . . ? C39 C48 H48B 109.5 . . ? C39 C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C39 C48 H48A 109.5 . . ? H48B C48 H48A 109.5 . . ? H48C C48 H48A 109.5 . . ? C90 C49 C68 120.7(7) . . ? C90 C49 C206 123.7(8) . . ? C68 C49 C206 115.6(7) . . ? C54 C50 C45 117.8(6) . . ? C54 C50 H50 121.1 . . ? C45 C50 H50 121.1 . . ? C66 C51 C62 121.8(6) . . ? C66 C51 H51 119.1 . . ? C62 C51 H51 119.1 . . ? C93 C52 C30 119.8(6) . . ? C93 C52 H52 120.1 . . ? C30 C52 H52 120.1 . . ? C42 C53 C109 119.9(8) . . ? C42 C53 H53 120.0 . . ? C109 C53 H53 120.0 . . ? N3 C54 C50 123.8(6) . . ? N3 C54 H54 118.1 . . ? C50 C54 H54 118.1 . . ? C59 C55 C37 119.3(6) . . ? C59 C55 C206 121.9(6) . . ? C37 C55 C206 118.6(6) . . ? C39 C56 H56B 109.5 . . ? C39 C56 H56A 109.5 . . ? H56B C56 H56A 109.5 . . ? C39 C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? C76 C57 C88 121.9(8) . . ? C76 C57 H57 119.1 . . ? C88 C57 H57 119.1 . . ? C33 C58 C88 121.6(6) . . ? C33 C58 H58 119.2 . . ? C88 C58 H58 119.2 . . ? C55 C59 C62 121.9(6) . . ? C55 C59 H59 119.1 . . ? C62 C59 H59 119.1 . . ? C126 C60 C35 117.5(7) . . ? C126 C60 H60 121.3 . . ? C35 C60 H60 121.3 . . ? C65 C61 C108 122.6(8) . . ? C65 C61 H61 118.7 . . ? C108 C61 H61 118.7 . . ? C59 C62 C51 117.7(6) . . ? C59 C62 C104 121.3(6) . . ? C51 C62 C104 120.9(7) . . ? N1 C1 C2 122.2(6) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C84 C64 C111 120.4(8) . . ? C84 C64 C32 117.9(7) . . ? C111 C64 C32 121.7(7) . . ? C100 C65 C61 117.0(7) . . ? C100 C65 C32 122.1(6) . . ? C61 C65 C32 120.7(6) . . ? C37 C66 C51 119.3(6) . . ? C37 C66 C81 118.4(6) . . ? C51 C66 C81 122.0(6) . . ? C122 C67 C34 119.2(7) . . ? C122 C67 H67 120.4 . . ? C34 C67 H67 120.4 . . ? C49 C68 C87 117.2(9) . . ? C49 C68 H68 121.4 . . ? C87 C68 H68 121.4 . . ? C30 C69 C115 119.5(7) . . ? C30 C69 H69 120.2 . . ? C115 C69 H69 120.2 . . ? C38 C70 H70C 109.5 . . ? C38 C70 H70A 109.5 . . ? H70C C70 H70A 109.5 . . ? C38 C70 H70B 109.5 . . ? H70C C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C33 C71 C76 121.1(7) . . ? C33 C71 H71 119.5 . . ? C76 C71 H71 119.5 . . ? C42 C72 C117 121.4(8) . . ? C42 C72 H72 119.3 . . ? C117 C72 H72 119.3 . . ? C75 C74 C29 119.7(7) . . ? C75 C74 H74 120.2 . . ? C29 C74 H74 120.2 . . ? C74 C75 C118 122.0(7) . . ? C74 C75 H75 119.0 . . ? C118 C75 H75 119.0 . . ? C57 C76 C71 120.2(7) . . ? C57 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? C116 C77 C91 121.4(11) . . ? C116 C77 H77 119.3 . . ? C91 C77 H77 119.3 . . ? C80 C8 C35 121.3(7) . . ? C80 C8 H8 119.4 . . ? C35 C8 H8 119.4 . . ? C8 C80 C103 120.5(8) . . ? C8 C80 H80 119.7 . . ? C103 C80 H80 119.7 . . ? C105 C81 C91 114.5(6) . . ? C105 C81 C66 115.4(6) . . ? C91 C81 C66 108.6(6) . . ? C105 C81 H81 105.8 . . ? C91 C81 H81 105.8 . . ? C66 C81 H81 105.8 . . ? C64 C84 C142 118.2(10) . . ? C64 C84 H84 120.9 . . ? C142 C84 H84 120.9 . . ? C85 C34 C67 118.3(7) . . ? C85 C34 H34 120.8 . . ? C67 C34 H34 120.8 . . ? C87 C86 C101 120.7(9) . . ? C87 C86 H86 119.7 . . ? C101 C86 H86 119.7 . . ? C86 C87 C68 122.0(9) . . ? C86 C87 H87 119.0 . . ? C68 C87 H87 119.0 . . ? C57 C88 C58 118.3(7) . . ? C57 C88 H88 120.8 . . ? C58 C88 H88 120.8 . . ? C98 C89 C44 119.8(8) . . ? C98 C89 H89 120.1 . . ? C44 C89 H89 120.1 . . ? C49 C90 C101 121.2(10) . . ? C49 C90 H90 119.4 . . ? C101 C90 H90 119.4 . . ? C127 C91 C77 117.0(9) . . ? C127 C91 C81 125.0(8) . . ? C77 C91 C81 117.8(9) . . ? C2 C3 C4 120.6(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C120 C93 C52 119.5(7) . . ? C120 C93 H93 120.3 . . ? C52 C93 H93 120.3 . . ? C3 C4 C5 118.0(6) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C38 C95 H95C 109.5 . . ? C38 C95 H95A 109.5 . . ? H95C C95 H95A 109.5 . . ? C38 C95 H95B 109.5 . . ? H95C C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C97 C96 C98 120.1(8) . . ? C97 C96 H96 119.9 . . ? C98 C96 H96 119.9 . . ? C96 C97 C36 123.2(7) . . ? C96 C97 H97 118.4 . . ? C36 C97 H97 118.4 . . ? C89 C98 C96 119.7(8) . . ? C89 C98 H98 120.2 . . ? C96 C98 H98 120.2 . . ? C105 C99 C113 121.3(11) . . ? C105 C99 H99 119.4 . . ? C113 C99 H99 119.4 . . ? C65 C100 C112 122.6(9) . . ? C65 C100 H10 118.7 . . ? C112 C100 H10 118.7 . . ? C86 C101 C90 118.2(10) . . ? C86 C101 H10D 120.9 . . ? C90 C101 H10D 120.9 . . ? C126 C103 C80 119.5(8) . . ? C126 C103 H10B 120.3 . . ? C80 C103 H10B 120.3 . . ? C62 C104 C114 111.7(7) . . ? C62 C104 C129 111.3(8) . . ? C114 C104 C129 109.8(8) . . ? C62 C104 H10E 108.0 . . ? C114 C104 H10E 108.0 . . ? C129 C104 H10E 108.0 . . ? C99 C105 C125 118.9(8) . . ? C99 C105 C81 119.5(8) . . ? C125 C105 C81 121.5(8) . . ? C132 C108 C61 118.7(8) . . ? C132 C108 H10A 120.7 . . ? C61 C108 H10A 120.7 . . ? C123 C109 C53 119.4(10) . . ? C123 C109 H10C 120.3 . . ? C53 C109 H10C 120.3 . . ? C145 C111 C64 121.4(11) . . ? C145 C111 H11 119.3 . . ? C64 C111 H11 119.3 . . ? C132 C112 C100 117.3(10) . . ? C132 C112 H11A 121.3 . . ? C100 C112 H11A 121.3 . . ? C119 C113 C99 117.9(13) . . ? C119 C113 H11F 121.1 . . ? C99 C113 H11F 121.1 . . ? C104 C114 H11H 109.5 . . ? C104 C114 H11G 109.5 . . ? H11H C114 H11G 109.5 . . ? C104 C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? H11G C114 H11I 109.5 . . ? C120 C115 C69 117.5(8) . . ? C120 C115 H11C 121.2 . . ? C69 C115 H11C 121.2 . . ? C211 C116 C77 117.6(12) . . ? C211 C116 H11J 121.2 . . ? C77 C116 H11J 121.2 . . ? C123 C117 C72 117.9(9) . . ? C123 C117 H11D 121.0 . . ? C72 C117 H11D 121.0 . . ? C75 C118 C43 119.0(8) . . ? C75 C118 H11E 120.5 . . ? C43 C118 H11E 120.5 . . ? C212 C119 C113 122.5(14) . . ? C212 C119 H11K 118.7 . . ? C113 C119 H11K 118.7 . . ? C93 C120 C115 122.8(8) . . ? C93 C120 H12 118.6 . . ? C115 C120 H12 118.6 . . ? N8 C121 C122 121.3(7) . . ? N8 C121 H12C 119.4 . . ? C122 C121 H12C 119.4 . . ? C67 C122 C121 119.3(8) . . ? C67 C122 H12D 120.4 . . ? C121 C122 H12D 120.4 . . ? C109 C123 C117 122.0(9) . . ? C109 C123 H12A 119.0 . . ? C117 C123 H12A 119.0 . . ? C105 C125 C212 119.3(11) . . ? C105 C125 H12E 120.4 . . ? C212 C125 H12E 120.4 . . ? C103 C126 C60 122.3(8) . . ? C103 C126 H12B 118.9 . . ? C60 C126 H12B 118.9 . . ? C91 C127 C130 121.8(10) . . ? C91 C127 H12F 119.1 . . ? C130 C127 H12F 119.1 . . ? C104 C129 H12H 109.5 . . ? C104 C129 H12I 109.5 . . ? H12H C129 H12I 109.5 . . ? C104 C129 H12G 109.5 . . ? H12H C129 H12G 109.5 . . ? H12I C129 H12G 109.5 . . ? C211 C130 C127 114.6(11) . . ? C211 C130 H13A 108.6 . . ? C127 C130 H13A 108.6 . . ? C211 C130 H13B 108.6 . . ? C127 C130 H13B 108.6 . . ? H13A C130 H13B 107.6 . . ? C108 C132 C112 121.7(9) . . ? C108 C132 H13 119.1 . . ? C112 C132 H13 119.1 . . ? C3 C2 C1 117.6(7) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C84 C142 C207 119.7(13) . . ? C84 C142 H14 120.2 . . ? C207 C142 H14 120.2 . . ? C207 C145 C111 119.3(14) . . ? C207 C145 H14A 120.3 . . ? C111 C145 H14A 120.3 . . ? Ni1 O1 H1A 115.3 . . ? Ni1 O1 H1B 129.2 . . ? H1A O1 H1B 115.6 . . ? Ni2 O2 H2A 114.4 . . ? Ni2 O2 H2B 113.7 . . ? H2A O2 H2B 103.2 . . ? C145 C207 C142 121.0(13) . . ? C145 C207 H20 119.5 . . ? C142 C207 H20 119.5 . . ? C116 C211 C130 127.2(13) . . ? C116 C211 H21A 116.4 . . ? C130 C211 H21A 116.4 . . ? C119 C212 C125 120.0(13) . . ? C119 C212 H21B 120.0 . . ? C125 C212 H21B 120.0 . . ? N6 C220 C85 120.0(7) . . ? N6 C220 H22A 120.0 . . ? C85 C220 H22A 120.0 . . ? N8 Ni3 N6 78.4(2) . . ? N8 Ni3 Cl10 171.72(18) . . ? N6 Ni3 Cl10 93.36(15) . . ? N8 Ni3 O3 91.5(2) . . ? N6 Ni3 O3 94.12(18) . . ? Cl10 Ni3 O3 88.93(12) . . ? N8 Ni3 Cl10 96.59(17) . 2_776 ? N6 Ni3 Cl10 174.57(15) . 2_776 ? Cl10 Ni3 Cl10 91.67(7) . 2_776 ? O3 Ni3 Cl10 83.94(12) . 2_776 ? N8 Ni3 Cl11 89.58(17) . . ? N6 Ni3 Cl11 96.09(15) . . ? Cl10 Ni3 Cl11 91.45(7) . . ? O3 Ni3 Cl11 169.75(13) . . ? Cl10 Ni3 Cl11 85.81(7) 2_776 . ? Ni3 Cl10 Ni3 88.33(7) . 2_776 ? Ni3 O3 H3A 116.9 . . ? Ni3 O3 H3B 125.8 . . ? H3A O3 H3B 117.2 . . ? C234 C235 C233 111.3(13) . . ? C234 C235 H23 124.4 . . ? C233 C235 H23 124.4 . . ? C232 C231 C205 126.1(15) . . ? C232 C231 H23A 117.0 . . ? C205 C231 H23A 117.0 . . ? C233 C232 C231 113.8(17) . . ? C233 C232 H23B 123.1 . . ? C231 C232 H23B 123.1 . . ? C232 C233 C235 126.7(17) . . ? C232 C233 H23C 116.7 . . ? C235 C233 H23C 116.7 . . ? C205 C234 C235 126.9(11) . . ? C205 C234 H23D 116.6 . . ? C235 C234 H23D 116.6 . . ? 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 C1 -178.9(6) . . . . ? O1 Ni1 N1 C1 -86.6(5) . . . . ? Cl1 Ni1 N1 C1 82.5(5) . . . . ? Cl2 Ni1 N1 C1 -147.5(7) 2_665 . . . ? Cl2 Ni1 N1 C1 -6.1(5) . . . . ? N2 Ni1 N1 C5 -1.0(4) . . . . ? O1 Ni1 N1 C5 91.3(4) . . . . ? Cl1 Ni1 N1 C5 -99.6(4) . . . . ? Cl2 Ni1 N1 C5 30.4(11) 2_665 . . . ? Cl2 Ni1 N1 C5 171.8(4) . . . . ? N1 Ni1 N2 C6 -0.3(4) . . . . ? O1 Ni1 N2 C6 -88.1(4) . . . . ? Cl1 Ni1 N2 C6 89.4(4) . . . . ? Cl2 Ni1 N2 C6 -175.4(4) 2_665 . . . ? Cl2 Ni1 N2 C6 -54.8(9) . . . . ? N1 Ni1 N2 C7 177.5(4) . . . . ? O1 Ni1 N2 C7 89.7(4) . . . . ? Cl1 Ni1 N2 C7 -92.8(4) . . . . ? Cl2 Ni1 N2 C7 2.5(4) 2_665 . . . ? Cl2 Ni1 N2 C7 123.0(7) . . . . ? N4 Ni2 N3 C54 178.8(5) . . . . ? O2 Ni2 N3 C54 -88.3(5) . . . . ? Cl5 Ni2 N3 C54 -140.1(6) 2_777 . . . ? Cl7 Ni2 N3 C54 81.9(5) . . . . ? Cl5 Ni2 N3 C54 -8.5(5) . . . . ? N4 Ni2 N3 C140 0.4(4) . . . . ? O2 Ni2 N3 C140 93.3(4) . . . . ? Cl5 Ni2 N3 C140 41.5(9) 2_777 . . . ? Cl7 Ni2 N3 C140 -96.5(4) . . . . ? Cl5 Ni2 N3 C140 173.1(4) . . . . ? N1 Ni1 Cl2 Ni1 -174.09(14) . . . 2_665 ? N2 Ni1 Cl2 Ni1 -120.6(7) . . . 2_665 ? O1 Ni1 Cl2 Ni1 -86.83(11) . . . 2_665 ? Cl1 Ni1 Cl2 Ni1 94.69(6) . . . 2_665 ? Cl2 Ni1 Cl2 Ni1 0.0 2_665 . . 2_665 ? N3 Ni2 N4 C94 0.3(4) . . . . ? O2 Ni2 N4 C94 -86.5(4) . . . . ? Cl5 Ni2 N4 C94 -171.9(4) 2_777 . . . ? Cl7 Ni2 N4 C94 91.6(4) . . . . ? Cl5 Ni2 N4 C94 -55.4(10) . . . . ? N3 Ni2 N4 C31 180.0(5) . . . . ? O2 Ni2 N4 C31 93.1(5) . . . . ? Cl5 Ni2 N4 C31 7.7(4) 2_777 . . . ? Cl7 Ni2 N4 C31 -88.7(4) . . . . ? Cl5 Ni2 N4 C31 124.2(7) . . . . ? N3 Ni2 Cl5 Ni2 -171.20(14) . . . 2_777 ? N4 Ni2 Cl5 Ni2 -116.5(8) . . . 2_777 ? O2 Ni2 Cl5 Ni2 -84.91(13) . . . 2_777 ? Cl5 Ni2 Cl5 Ni2 0.0 2_777 . . 2_777 ? Cl7 Ni2 Cl5 Ni2 96.13(7) . . . 2_777 ? C54 N3 C140 C40 2.6(8) . . . . ? Ni2 N3 C140 C40 -178.8(4) . . . . ? C54 N3 C140 C94 -179.5(5) . . . . ? Ni2 N3 C140 C94 -0.9(6) . . . . ? C7 C12 C92 C24 -148.5(5) . . . . ? C11 C12 C92 C24 29.0(7) . . . . ? C7 C12 C92 C30 83.4(6) . . . . ? C11 C12 C92 C30 -99.2(5) . . . . ? C31 N4 C94 C140 179.3(5) . . . . ? Ni2 N4 C94 C140 -1.0(6) . . . . ? N3 C140 C94 N4 1.3(8) . . . . ? C40 C140 C94 N4 179.2(5) . . . . ? C234 C205 C206 C49 86.4(10) . . . . ? C231 C205 C206 C49 -94.3(12) . . . . ? C234 C205 C206 C55 -38.6(11) . . . . ? C231 C205 C206 C55 140.7(11) . . . . ? C7 N2 C6 C5 -176.7(5) . . . . ? Ni1 N2 C6 C5 1.5(6) . . . . ? C11 C12 C7 C15 -0.7(7) . . . . ? C92 C12 C7 C15 176.8(4) . . . . ? C11 C12 C7 N2 179.4(4) . . . . ? C92 C12 C7 N2 -3.1(7) . . . . ? C9 C15 C7 C12 -1.3(8) . . . . ? C19 C15 C7 C12 -179.6(5) . . . . ? C9 C15 C7 N2 178.6(4) . . . . ? C19 C15 C7 N2 0.2(7) . . . . ? C6 N2 C7 C12 -93.8(6) . . . . ? Ni1 N2 C7 C12 88.4(5) . . . . ? C6 N2 C7 C15 86.3(6) . . . . ? Ni1 N2 C7 C15 -91.4(5) . . . . ? C7 C15 C19 C35 -86.8(6) . . . . ? C9 C15 C19 C35 95.0(6) . . . . ? C7 C15 C19 C42 144.2(5) . . . . ? C9 C15 C19 C42 -34.1(7) . . . . ? C31 C16 C21 C25 -2.5(8) . . . . ? C32 C16 C21 C25 -177.5(5) . . . . ? C1 N1 C5 C4 0.3(9) . . . . ? Ni1 N1 C5 C4 -177.9(5) . . . . ? C1 N1 C5 C6 -179.9(5) . . . . ? Ni1 N1 C5 C6 1.9(6) . . . . ? N2 C6 C5 N1 -2.4(8) . . . . ? N2 C6 C5 C4 177.4(6) . . . . ? C12 C92 C24 C43 55.0(7) . . . . ? C30 C92 C24 C43 -179.1(5) . . . . ? C12 C92 C24 C29 -123.6(6) . . . . ? C30 C92 C24 C29 2.4(7) . . . . ? C47 C22 C25 C21 1.0(9) . . . . ? C47 C22 C25 C39 -179.3(5) . . . . ? C16 C21 C25 C22 -0.3(8) . . . . ? C16 C21 C25 C39 -179.9(5) . . . . ? C7 C15 C9 C10 2.0(8) . . . . ? C19 C15 C9 C10 -179.7(5) . . . . ? C11 C10 C9 C15 -0.6(8) . . . . ? C38 C10 C9 C15 178.7(5) . . . . ? C9 C10 C11 C12 -1.6(8) . . . . ? C38 C10 C11 C12 179.1(5) . . . . ? C7 C12 C11 C10 2.3(8) . . . . ? C92 C12 C11 C10 -175.3(5) . . . . ? C43 C24 C29 C74 0.1(9) . . . . ? C92 C24 C29 C74 178.7(5) . . . . ? C24 C92 C30 C69 110.4(7) . . . . ? C12 C92 C30 C69 -122.9(6) . . . . ? C24 C92 C30 C52 -69.8(7) . . . . ? C12 C92 C30 C52 56.9(7) . . . . ? C21 C16 C31 C47 4.7(8) . . . . ? C32 C16 C31 C47 179.9(5) . . . . ? C21 C16 C31 N4 -177.8(5) . . . . ? C32 C16 C31 N4 -2.6(8) . . . . ? C94 N4 C31 C16 94.0(6) . . . . ? Ni2 N4 C31 C16 -85.7(6) . . . . ? C94 N4 C31 C47 -88.5(6) . . . . ? Ni2 N4 C31 C47 91.9(6) . . . . ? C21 C16 C32 C64 -27.0(8) . . . . ? C31 C16 C32 C64 158.1(6) . . . . ? C21 C16 C32 C65 101.6(6) . . . . ? C31 C16 C32 C65 -73.3(7) . . . . ? C47 C26 C33 C71 -112.3(6) . . . . ? C36 C26 C33 C71 16.1(8) . . . . ? C47 C26 C33 C58 66.7(7) . . . . ? C36 C26 C33 C58 -164.9(5) . . . . ? C15 C19 C35 C8 -47.3(7) . . . . ? C42 C19 C35 C8 82.0(7) . . . . ? C15 C19 C35 C60 130.8(5) . . . . ? C42 C19 C35 C60 -99.9(6) . . . . ? C47 C26 C36 C97 -138.0(6) . . . . ? C33 C26 C36 C97 92.9(7) . . . . ? C47 C26 C36 C44 41.6(7) . . . . ? C33 C26 C36 C44 -87.5(7) . . . . ? C220 N6 C37 C66 -91.9(8) . . . . ? Ni3 N6 C37 C66 86.8(7) . . . . ? C220 N6 C37 C55 88.8(7) . . . . ? Ni3 N6 C37 C55 -92.6(7) . . . . ? C11 C10 C38 C70 61.2(8) . . . . ? C9 C10 C38 C70 -118.1(6) . . . . ? C11 C10 C38 C95 -60.9(8) . . . . ? C9 C10 C38 C95 119.8(6) . . . . ? C22 C25 C39 C48 -74.0(7) . . . . ? C21 C25 C39 C48 105.6(6) . . . . ? C22 C25 C39 C56 48.6(7) . . . . ? C21 C25 C39 C56 -131.7(6) . . . . ? N3 C140 C40 C45 -3.6(9) . . . . ? C94 C140 C40 C45 178.7(6) . . . . ? C121 N8 C85 C34 -1.4(11) . . . . ? Ni3 N8 C85 C34 174.3(6) . . . . ? C121 N8 C85 C220 179.7(6) . . . . ? Ni3 N8 C85 C220 -4.6(8) . . . . ? C35 C19 C42 C72 -17.1(8) . . . . ? C15 C19 C42 C72 111.9(7) . . . . ? C35 C19 C42 C53 159.3(5) . . . . ? C15 C19 C42 C53 -71.7(7) . . . . ? C29 C24 C43 C118 -0.6(10) . . . . ? C92 C24 C43 C118 -179.3(6) . . . . ? C97 C36 C44 C89 0.0(10) . . . . ? C26 C36 C44 C89 -179.6(6) . . . . ? C140 C40 C45 C50 3.5(10) . . . . ? C25 C22 C47 C31 1.0(9) . . . . ? C25 C22 C47 C26 176.2(5) . . . . ? C16 C31 C47 C22 -4.0(8) . . . . ? N4 C31 C47 C22 178.5(5) . . . . ? C16 C31 C47 C26 -179.4(5) . . . . ? N4 C31 C47 C26 3.2(8) . . . . ? C36 C26 C47 C22 -97.4(7) . . . . ? C33 C26 C47 C22 33.1(8) . . . . ? C36 C26 C47 C31 77.7(7) . . . . ? C33 C26 C47 C31 -151.9(5) . . . . ? C205 C206 C49 C90 -11.6(11) . . . . ? C55 C206 C49 C90 112.5(9) . . . . ? C205 C206 C49 C68 170.2(7) . . . . ? C55 C206 C49 C68 -65.7(9) . . . . ? C40 C45 C50 C54 -2.7(11) . . . . ? C69 C30 C52 C93 -2.9(10) . . . . ? C92 C30 C52 C93 177.3(6) . . . . ? C72 C42 C53 C109 0.2(10) . . . . ? C19 C42 C53 C109 -176.4(6) . . . . ? C140 N3 C54 C50 -1.7(9) . . . . ? Ni2 N3 C54 C50 180.0(5) . . . . ? C45 C50 C54 N3 1.7(11) . . . . ? C66 C37 C55 C59 0.4(10) . . . . ? N6 C37 C55 C59 179.8(6) . . . . ? C66 C37 C55 C206 175.6(6) . . . . ? N6 C37 C55 C206 -5.1(9) . . . . ? C205 C206 C55 C59 101.0(8) . . . . ? C49 C206 C55 C59 -24.8(10) . . . . ? C205 C206 C55 C37 -73.9(8) . . . . ? C49 C206 C55 C37 160.2(6) . . . . ? C71 C33 C58 C88 2.2(9) . . . . ? C26 C33 C58 C88 -176.9(6) . . . . ? C37 C55 C59 C62 -0.7(11) . . . . ? C206 C55 C59 C62 -175.7(7) . . . . ? C8 C35 C60 C126 -1.4(10) . . . . ? C19 C35 C60 C126 -179.6(6) . . . . ? C55 C59 C62 C51 -0.3(11) . . . . ? C55 C59 C62 C104 177.0(7) . . . . ? C66 C51 C62 C59 1.7(10) . . . . ? C66 C51 C62 C104 -175.6(7) . . . . ? C5 N1 C1 C2 -1.1(10) . . . . ? Ni1 N1 C1 C2 176.8(6) . . . . ? C16 C32 C64 C84 -81.0(8) . . . . ? C65 C32 C64 C84 152.2(6) . . . . ? C16 C32 C64 C111 98.5(7) . . . . ? C65 C32 C64 C111 -28.3(9) . . . . ? C108 C61 C65 C100 -1.5(12) . . . . ? C108 C61 C65 C32 -176.7(7) . . . . ? C16 C32 C65 C100 -40.5(9) . . . . ? C64 C32 C65 C100 88.3(8) . . . . ? C16 C32 C65 C61 134.4(6) . . . . ? C64 C32 C65 C61 -96.8(7) . . . . ? C55 C37 C66 C51 0.9(10) . . . . ? N6 C37 C66 C51 -178.5(6) . . . . ? C55 C37 C66 C81 -172.8(6) . . . . ? N6 C37 C66 C81 7.8(9) . . . . ? C62 C51 C66 C37 -1.9(10) . . . . ? C62 C51 C66 C81 171.5(6) . . . . ? C90 C49 C68 C87 2.2(12) . . . . ? C206 C49 C68 C87 -179.5(7) . . . . ? C52 C30 C69 C115 -0.9(12) . . . . ? C92 C30 C69 C115 178.9(8) . . . . ? C58 C33 C71 C76 0.5(10) . . . . ? C26 C33 C71 C76 179.5(6) . . . . ? C53 C42 C72 C117 0.0(10) . . . . ? C19 C42 C72 C117 176.2(6) . . . . ? C24 C29 C74 C75 -0.5(10) . . . . ? C29 C74 C75 C118 1.4(12) . . . . ? C88 C57 C76 C71 1.6(12) . . . . ? C33 C71 C76 C57 -2.4(12) . . . . ? C60 C35 C8 C80 2.2(11) . . . . ? C19 C35 C8 C80 -179.7(7) . . . . ? C35 C8 C80 C103 0.7(13) . . . . ? C37 C66 C81 C105 -153.8(7) . . . . ? C51 C66 C81 C105 32.7(10) . . . . ? C37 C66 C81 C91 76.1(8) . . . . ? C51 C66 C81 C91 -97.4(8) . . . . ? C111 C64 C84 C142 -0.8(12) . . . . ? C32 C64 C84 C142 178.7(7) . . . . ? N8 C85 C34 C67 -0.2(12) . . . . ? C220 C85 C34 C67 178.6(7) . . . . ? C122 C67 C34 C85 1.3(13) . . . . ? C101 C86 C87 C68 0.2(14) . . . . ? C49 C68 C87 C86 -2.5(12) . . . . ? C76 C57 C88 C58 1.1(12) . . . . ? C33 C58 C88 C57 -3.1(10) . . . . ? C36 C44 C89 C98 -0.3(12) . . . . ? C68 C49 C90 C101 0.2(14) . . . . ? C206 C49 C90 C101 -177.9(8) . . . . ? C116 C77 C91 C127 0.2(13) . . . . ? C116 C77 C91 C81 174.6(8) . . . . ? C105 C81 C91 C127 -89.5(10) . . . . ? C66 C81 C91 C127 41.1(10) . . . . ? C105 C81 C91 C77 96.6(9) . . . . ? C66 C81 C91 C77 -132.7(7) . . . . ? C30 C52 C93 C120 2.6(12) . . . . ? C2 C3 C4 C5 -3.7(13) . . . . ? N1 C5 C4 C3 2.1(11) . . . . ? C6 C5 C4 C3 -177.7(7) . . . . ? C98 C96 C97 C36 0.6(12) . . . . ? C44 C36 C97 C96 -0.2(10) . . . . ? C26 C36 C97 C96 179.5(6) . . . . ? C44 C89 C98 C96 0.8(12) . . . . ? C97 C96 C98 C89 -0.9(12) . . . . ? C61 C65 C100 C112 0.3(14) . . . . ? C32 C65 C100 C112 175.4(9) . . . . ? C87 C86 C101 C90 2.2(14) . . . . ? C49 C90 C101 C86 -2.4(15) . . . . ? C8 C80 C103 C126 -4.4(13) . . . . ? C59 C62 C104 C114 59.3(11) . . . . ? C51 C62 C104 C114 -123.5(8) . . . . ? C59 C62 C104 C129 -63.7(10) . . . . ? C51 C62 C104 C129 113.5(9) . . . . ? C113 C99 C105 C125 -2.1(14) . . . . ? C113 C99 C105 C81 175.7(8) . . . . ? C91 C81 C105 C99 -159.1(8) . . . . ? C66 C81 C105 C99 73.7(10) . . . . ? C91 C81 C105 C125 18.7(12) . . . . ? C66 C81 C105 C125 -108.5(9) . . . . ? C65 C61 C108 C132 1.9(14) . . . . ? C42 C53 C109 C123 -1.8(11) . . . . ? C84 C64 C111 C145 1.0(13) . . . . ? C32 C64 C111 C145 -178.5(8) . . . . ? C65 C100 C112 C132 0.5(18) . . . . ? C105 C99 C113 C119 3.2(15) . . . . ? C30 C69 C115 C120 4.9(16) . . . . ? C91 C77 C116 C211 4.3(18) . . . . ? C42 C72 C117 C123 1.6(12) . . . . ? C74 C75 C118 C43 -2.0(12) . . . . ? C24 C43 C118 C75 1.5(12) . . . . ? C99 C113 C119 C212 -3.8(19) . . . . ? C52 C93 C120 C115 1.8(16) . . . . ? C69 C115 C120 C93 -5.4(18) . . . . ? C85 N8 C121 C122 1.9(12) . . . . ? Ni3 N8 C121 C122 -173.2(6) . . . . ? C34 C67 C122 C121 -0.8(14) . . . . ? N8 C121 C122 C67 -0.8(14) . . . . ? C53 C109 C123 C117 3.5(14) . . . . ? C72 C117 C123 C109 -3.3(14) . . . . ? C99 C105 C125 C212 1.5(15) . . . . ? C81 C105 C125 C212 -176.4(9) . . . . ? C80 C103 C126 C60 5.2(14) . . . . ? C35 C60 C126 C103 -2.4(12) . . . . ? C77 C91 C127 C130 -2.1(12) . . . . ? C81 C91 C127 C130 -176.1(8) . . . . ? C91 C127 C130 C211 -0.2(14) . . . . ? C61 C108 C132 C112 -1.1(16) . . . . ? C100 C112 C132 C108 -0.1(18) . . . . ? C4 C3 C2 C1 2.9(15) . . . . ? N1 C1 C2 C3 -0.5(13) . . . . ? C64 C84 C142 C207 1.2(14) . . . . ? C64 C111 C145 C207 -1.6(18) . . . . ? C111 C145 C207 C142 2(2) . . . . ? C84 C142 C207 C145 -1.8(19) . . . . ? C77 C116 C211 C130 -7(2) . . . . ? C127 C130 C211 C116 5(2) . . . . ? C113 C119 C212 C125 3(2) . . . . ? C105 C125 C212 C119 -2.0(18) . . . . ? C37 N6 C220 C85 -179.8(6) . . . . ? Ni3 N6 C220 C85 1.3(8) . . . . ? N8 C85 C220 N6 2.2(9) . . . . ? C34 C85 C220 N6 -176.7(7) . . . . ? C85 N8 Ni3 N6 4.1(5) . . . . ? C121 N8 Ni3 N6 179.4(7) . . . . ? C85 N8 Ni3 Cl10 5.0(15) . . . . ? C121 N8 Ni3 Cl10 -179.7(9) . . . . ? C85 N8 Ni3 O3 98.0(5) . . . . ? C121 N8 Ni3 O3 -86.7(6) . . . . ? C85 N8 Ni3 Cl10 -178.0(5) . . . 2_776 ? C121 N8 Ni3 Cl10 -2.6(6) . . . 2_776 ? C85 N8 Ni3 Cl11 -92.2(5) . . . . ? C121 N8 Ni3 Cl11 83.1(6) . . . . ? C220 N6 Ni3 N8 -2.9(4) . . . . ? C37 N6 Ni3 N8 178.5(5) . . . . ? C220 N6 Ni3 Cl10 177.3(4) . . . . ? C37 N6 Ni3 Cl10 -1.4(5) . . . . ? C220 N6 Ni3 O3 -93.6(4) . . . . ? C37 N6 Ni3 O3 87.8(5) . . . . ? C220 N6 Ni3 Cl10 -24.8(19) . . . 2_776 ? C37 N6 Ni3 Cl10 156.5(13) . . . 2_776 ? C220 N6 Ni3 Cl11 85.5(4) . . . . ? C37 N6 Ni3 Cl11 -93.2(5) . . . . ? N8 Ni3 Cl10 Ni3 177.1(12) . . . 2_776 ? N6 Ni3 Cl10 Ni3 177.96(15) . . . 2_776 ? O3 Ni3 Cl10 Ni3 83.90(12) . . . 2_776 ? Cl10 Ni3 Cl10 Ni3 0.0 2_776 . . 2_776 ? Cl11 Ni3 Cl10 Ni3 -85.85(7) . . . 2_776 ? C234 C205 C231 C232 0(2) . . . . ? C206 C205 C231 C232 -179.5(14) . . . . ? C205 C231 C232 C233 3(3) . . . . ? C231 C232 C233 C235 -5(3) . . . . ? C234 C235 C233 C232 3(2) . . . . ? C231 C205 C234 C235 -2.0(17) . . . . ? C206 C205 C234 C235 177.4(10) . . . . ? C233 C235 C234 C205 0.7(18) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.734 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.150 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; 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 -0.140 0.468 0.500 1776.4 599.7 2 0.188 0.147 0.834 138.7 43.8 3 0.465 0.934 0.851 12.0 1.7 4 0.535 0.066 0.149 12.0 5.7 5 0.812 0.853 0.166 138.7 47.2 _platon_squeeze_details ; ? ; #==END data_D4 _database_code_depnum_ccdc_archive 'CCDC 877852' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Br2 N4 Ni' _chemical_formula_weight 971.49 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.822(3) _cell_length_b 15.439(3) _cell_length_c 9.767(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.39(3) _cell_angle_gamma 90.00 _cell_volume 2225.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11332 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 27.55 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6991 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 11332 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5083 _reflns_number_gt 3897 _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^)+(0.0810P)^2^+4.5228P] 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 5083 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1072 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2149 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _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 0.55376(4) 0.00609(4) 0.26139(6) 0.0363(2) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.5000 0.0274(3) Uani 1 2 d S . . C7 C 0.7172(4) 0.0104(3) 0.6788(6) 0.0290(11) Uani 1 1 d . . . C13 C 0.6665(4) 0.0413(5) 0.9175(6) 0.0492(16) Uani 1 1 d . . . H13A H 0.6897 0.0310 1.0134 0.074 Uiso 1 1 calc R . . H13B H 0.6078 0.0123 0.8985 0.074 Uiso 1 1 calc R . . H13C H 0.6590 0.1036 0.9017 0.074 Uiso 1 1 calc R . . C15 C 0.7726(4) -0.0053(3) 0.4419(6) 0.0311(12) Uani 1 1 d . . . H15A H 0.7062 -0.0090 0.4129 0.037 Uiso 1 1 calc R . . N1 N 0.4837(3) 0.1323(3) 0.4951(4) 0.0303(10) Uani 1 1 d . . . C12 C 0.7835(4) -0.0206(4) 0.5978(6) 0.0312(12) Uani 1 1 d . . . C8 C 0.7319(4) 0.0059(4) 0.8242(6) 0.0353(13) Uani 1 1 d . . . C10 C 0.8784(4) -0.0614(4) 0.8022(6) 0.0379(13) Uani 1 1 d . . . N2 N 0.6349(3) 0.0483(3) 0.6117(4) 0.0304(10) Uani 1 1 d . . . C11 C 0.8622(4) -0.0562(4) 0.6600(6) 0.0368(13) Uani 1 1 d . . . H11A H 0.9065 -0.0777 0.6043 0.044 Uiso 1 1 calc R . . C6 C 0.6268(4) 0.1290(4) 0.6310(6) 0.0344(12) Uani 1 1 d . . . H6A H 0.6730 0.1586 0.6864 0.041 Uiso 1 1 calc R . . C9 C 0.8118(4) -0.0301(4) 0.8813(6) 0.0396(14) Uani 1 1 d . . . H9A H 0.8220 -0.0338 0.9787 0.048 Uiso 1 1 calc R . . C16 C 0.8020(4) 0.0856(4) 0.4046(6) 0.0336(12) Uani 1 1 d . . . C3 C 0.4717(4) 0.3118(4) 0.5141(7) 0.0494(17) Uani 1 1 d . . . H3A H 0.4672 0.3729 0.5220 0.059 Uiso 1 1 calc R . . C22 C 0.8175(4) -0.0750(4) 0.3629(5) 0.0355(13) Uani 1 1 d . . . C2 C 0.4068(4) 0.2652(4) 0.4344(8) 0.0523(17) Uani 1 1 d . . . H2A H 0.3571 0.2937 0.3848 0.063 Uiso 1 1 calc R . . C1 C 0.4159(4) 0.1751(4) 0.4281(6) 0.0390(13) Uani 1 1 d . . . H1A H 0.3712 0.1431 0.3732 0.047 Uiso 1 1 calc R . . C4 C 0.5439(4) 0.2669(4) 0.5824(7) 0.0440(15) Uani 1 1 d . . . H4A H 0.5898 0.2974 0.6371 0.053 Uiso 1 1 calc R . . C5 C 0.5484(4) 0.1781(4) 0.5707(6) 0.0333(12) Uani 1 1 d . . . C21 C 0.8615(5) 0.1341(5) 0.4881(7) 0.060(2) Uani 1 1 d . . . H21A H 0.8859 0.1122 0.5748 0.072 Uiso 1 1 calc R . . C26 C 0.9387(4) -0.1267(5) 0.2345(7) 0.0518(17) Uani 1 1 d . . . H26A H 0.9948 -0.1164 0.1976 0.062 Uiso 1 1 calc R . . C27 C 0.9010(4) -0.0630(5) 0.3116(6) 0.0444(15) Uani 1 1 d . . . H27A H 0.9329 -0.0102 0.3298 0.053 Uiso 1 1 calc R . . C25 C 0.8952(5) -0.2047(5) 0.2113(7) 0.0547(18) Uani 1 1 d . . . H25A H 0.9206 -0.2486 0.1585 0.066 Uiso 1 1 calc R . . C14 C 0.9654(4) -0.1005(5) 0.8696(7) 0.0510(17) Uani 1 1 d . . . H14A H 0.9647 -0.0987 0.9697 0.077 Uiso 1 1 calc R . . H14B H 1.0173 -0.0672 0.8430 0.077 Uiso 1 1 calc R . . H14C H 0.9705 -0.1607 0.8395 0.077 Uiso 1 1 calc R . . C23 C 0.7758(4) -0.1536(4) 0.3378(7) 0.0472(16) Uani 1 1 d . . . H23A H 0.7186 -0.1637 0.3712 0.057 Uiso 1 1 calc R . . C17 C 0.7713(4) 0.1190(4) 0.2775(7) 0.0476(16) Uani 1 1 d . . . H17A H 0.7323 0.0849 0.2165 0.057 Uiso 1 1 calc R . . C24 C 0.8143(5) -0.2177(5) 0.2660(8) 0.0579(19) Uani 1 1 d . . . H24A H 0.7846 -0.2721 0.2539 0.070 Uiso 1 1 calc R . . C19 C 0.8512(5) 0.2495(5) 0.3236(9) 0.065(2) Uani 1 1 d . . . H19A H 0.8650 0.3071 0.2981 0.078 Uiso 1 1 calc R . . C20 C 0.8862(6) 0.2176(6) 0.4433(8) 0.074(3) Uani 1 1 d . . . H20A H 0.9285 0.2512 0.4999 0.089 Uiso 1 1 calc R . . C18 C 0.7952(4) 0.1993(5) 0.2373(8) 0.0553(19) Uani 1 1 d . . . H18A H 0.7731 0.2206 0.1492 0.066 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 0.0297(3) 0.0475(4) 0.0307(3) 0.0019(2) -0.0015(2) -0.0048(2) Ni1 0.0271(5) 0.0260(5) 0.0286(5) 0.0004(4) -0.0010(4) -0.0004(4) C7 0.026(3) 0.029(3) 0.031(3) 0.000(2) -0.004(2) -0.003(2) C13 0.036(3) 0.071(5) 0.038(3) -0.007(3) -0.008(3) -0.002(3) C15 0.028(3) 0.038(3) 0.027(3) 0.003(2) -0.002(2) 0.003(2) N1 0.030(2) 0.029(2) 0.031(2) 0.0043(19) 0.001(2) 0.0021(18) C12 0.029(3) 0.034(3) 0.030(3) -0.003(2) -0.002(2) -0.002(2) C8 0.034(3) 0.043(3) 0.028(3) -0.003(2) -0.002(2) -0.003(2) C10 0.034(3) 0.045(3) 0.033(3) 0.002(3) -0.004(2) 0.005(3) N2 0.023(2) 0.036(3) 0.031(2) 0.0008(19) -0.0040(18) -0.0036(19) C11 0.034(3) 0.040(3) 0.035(3) -0.004(3) -0.001(2) 0.005(2) C6 0.034(3) 0.032(3) 0.036(3) -0.002(2) -0.003(2) -0.006(2) C9 0.042(3) 0.044(3) 0.030(3) 0.002(3) -0.013(3) 0.000(3) C16 0.027(3) 0.042(3) 0.034(3) 0.000(3) 0.009(2) -0.001(2) C3 0.048(4) 0.028(3) 0.069(5) 0.006(3) -0.009(3) 0.001(3) C22 0.033(3) 0.047(3) 0.025(3) -0.001(2) -0.007(2) 0.007(3) C2 0.044(4) 0.041(4) 0.070(5) 0.003(3) -0.010(3) 0.006(3) C1 0.037(3) 0.032(3) 0.046(3) 0.002(3) -0.004(3) 0.000(3) C4 0.035(3) 0.040(3) 0.056(4) -0.001(3) 0.000(3) -0.002(3) C5 0.029(3) 0.027(3) 0.043(3) -0.001(2) 0.003(2) -0.003(2) C21 0.076(5) 0.069(5) 0.034(3) -0.008(3) 0.005(3) -0.027(4) C26 0.035(3) 0.065(5) 0.055(4) 0.005(4) 0.007(3) 0.009(3) C27 0.029(3) 0.056(4) 0.048(4) -0.007(3) 0.004(3) 0.006(3) C25 0.049(4) 0.062(5) 0.052(4) -0.005(4) -0.001(3) 0.019(4) C14 0.047(4) 0.063(4) 0.040(3) 0.003(3) -0.011(3) 0.019(3) C23 0.034(3) 0.047(4) 0.060(4) -0.010(3) 0.002(3) 0.000(3) C17 0.037(3) 0.043(4) 0.060(4) 0.009(3) -0.006(3) -0.004(3) C24 0.051(4) 0.054(4) 0.066(5) -0.019(4) -0.007(4) 0.009(3) C19 0.072(5) 0.048(4) 0.079(6) 0.006(4) 0.020(5) -0.010(4) C20 0.090(6) 0.080(6) 0.055(5) -0.020(4) 0.025(5) -0.051(5) C18 0.034(3) 0.056(4) 0.075(5) 0.025(4) 0.001(3) 0.000(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 2.5346(8) . ? Ni1 N1 2.057(5) . ? Ni1 N1 2.057(5) 3_656 ? Ni1 N2 2.310(4) . ? Ni1 N2 2.310(4) 3_656 ? Ni1 Br1 2.5346(8) 3_656 ? C7 C12 1.403(8) . ? C7 C8 1.418(8) . ? C7 N2 1.452(7) . ? C13 C8 1.494(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C22 1.515(8) . ? C15 C16 1.525(7) . ? C15 C12 1.534(8) . ? C15 H15A 1.0000 . ? N1 C1 1.323(7) . ? N1 C5 1.354(7) . ? C12 C11 1.378(8) . ? C8 C9 1.378(8) . ? C10 C11 1.390(8) . ? C10 C9 1.396(8) . ? C10 C14 1.516(8) . ? N2 C6 1.269(7) . ? C11 H11A 0.9500 . ? C6 C5 1.463(8) . ? C6 H6A 0.9500 . ? C9 H9A 0.9500 . ? C16 C21 1.366(8) . ? C16 C17 1.382(8) . ? C3 C2 1.381(9) . ? C3 C4 1.392(8) . ? C3 H3A 0.9500 . ? C22 C23 1.373(8) . ? C22 C27 1.391(8) . ? C2 C1 1.399(8) . ? C2 H2A 0.9500 . ? C1 H1A 0.9500 . ? C4 C5 1.377(8) . ? C4 H4A 0.9500 . ? C21 C20 1.422(10) . ? C21 H21A 0.9500 . ? C26 C25 1.374(10) . ? C26 C27 1.389(9) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C25 C24 1.373(10) . ? C25 H25A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C23 C24 1.368(9) . ? C23 H23A 0.9500 . ? C17 C18 1.357(9) . ? C17 H17A 0.9500 . ? C24 H24A 0.9500 . ? C19 C20 1.328(12) . ? C19 C18 1.367(11) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C18 H18A 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 N1 180.0 . 3_656 ? N1 Ni1 N2 77.59(17) . . ? N1 Ni1 N2 102.41(17) 3_656 . ? N1 Ni1 N2 102.41(17) . 3_656 ? N1 Ni1 N2 77.59(17) 3_656 3_656 ? N2 Ni1 N2 180.00(12) . 3_656 ? N1 Ni1 Br1 90.67(11) . 3_656 ? N1 Ni1 Br1 89.33(11) 3_656 3_656 ? N2 Ni1 Br1 84.88(11) . 3_656 ? N2 Ni1 Br1 95.12(11) 3_656 3_656 ? N1 Ni1 Br1 89.33(11) . . ? N1 Ni1 Br1 90.67(11) 3_656 . ? N2 Ni1 Br1 95.12(11) . . ? N2 Ni1 Br1 84.88(11) 3_656 . ? Br1 Ni1 Br1 180.0 3_656 . ? C12 C7 C8 119.9(5) . . ? C12 C7 N2 119.1(5) . . ? C8 C7 N2 121.0(5) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C22 C15 C16 112.5(5) . . ? C22 C15 C12 112.7(4) . . ? C16 C15 C12 111.9(5) . . ? C22 C15 H15A 106.4 . . ? C16 C15 H15A 106.4 . . ? C12 C15 H15A 106.4 . . ? C1 N1 C5 118.4(5) . . ? C1 N1 Ni1 126.1(4) . . ? C5 N1 Ni1 115.5(4) . . ? C11 C12 C7 119.8(5) . . ? C11 C12 C15 120.3(5) . . ? C7 C12 C15 119.5(5) . . ? C9 C8 C7 118.1(5) . . ? C9 C8 C13 118.9(5) . . ? C7 C8 C13 123.0(5) . . ? C11 C10 C9 117.9(5) . . ? C11 C10 C14 121.1(5) . . ? C9 C10 C14 120.9(5) . . ? C6 N2 C7 114.6(5) . . ? C6 N2 Ni1 107.3(4) . . ? C7 N2 Ni1 137.4(3) . . ? C12 C11 C10 121.5(5) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? N2 C6 C5 122.2(5) . . ? N2 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C8 C9 C10 122.8(5) . . ? C8 C9 H9A 118.6 . . ? C10 C9 H9A 118.6 . . ? C21 C16 C17 118.2(6) . . ? C21 C16 C15 123.0(6) . . ? C17 C16 C15 118.7(5) . . ? C2 C3 C4 118.3(6) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C23 C22 C27 117.1(6) . . ? C23 C22 C15 120.5(5) . . ? C27 C22 C15 122.5(6) . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? N1 C1 C2 123.1(6) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 121.8(5) . . ? N1 C5 C6 116.3(5) . . ? C4 C5 C6 121.7(5) . . ? C16 C21 C20 118.9(7) . . ? C16 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C25 C26 C27 120.3(6) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C26 C27 C22 121.1(6) . . ? C26 C27 H27A 119.4 . . ? C22 C27 H27A 119.4 . . ? C24 C25 C26 118.6(7) . . ? C24 C25 H25A 120.7 . . ? C26 C25 H25A 120.7 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C23 C22 121.9(6) . . ? C24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C18 C17 C16 121.8(7) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C23 C24 C25 121.0(7) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 121.1(7) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C17 C18 C19 120.0(7) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? 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 N1 C1 45(100) 3_656 . . . ? N2 Ni1 N1 C1 172.8(5) . . . . ? N2 Ni1 N1 C1 -7.2(5) 3_656 . . . ? Br1 Ni1 N1 C1 -102.6(4) 3_656 . . . ? Br1 Ni1 N1 C1 77.4(4) . . . . ? N1 Ni1 N1 C5 -136(100) 3_656 . . . ? N2 Ni1 N1 C5 -8.7(4) . . . . ? N2 Ni1 N1 C5 171.3(4) 3_656 . . . ? Br1 Ni1 N1 C5 75.9(4) 3_656 . . . ? Br1 Ni1 N1 C5 -104.1(4) . . . . ? C8 C7 C12 C11 0.9(8) . . . . ? N2 C7 C12 C11 179.5(5) . . . . ? C8 C7 C12 C15 -172.4(5) . . . . ? N2 C7 C12 C15 6.3(7) . . . . ? C22 C15 C12 C11 35.5(7) . . . . ? C16 C15 C12 C11 -92.5(6) . . . . ? C22 C15 C12 C7 -151.3(5) . . . . ? C16 C15 C12 C7 80.7(6) . . . . ? C12 C7 C8 C9 -0.7(8) . . . . ? N2 C7 C8 C9 -179.4(5) . . . . ? C12 C7 C8 C13 177.0(5) . . . . ? N2 C7 C8 C13 -1.6(9) . . . . ? C12 C7 N2 C6 -112.0(6) . . . . ? C8 C7 N2 C6 66.7(7) . . . . ? C12 C7 N2 Ni1 79.1(6) . . . . ? C8 C7 N2 Ni1 -102.2(6) . . . . ? N1 Ni1 N2 C6 8.9(4) . . . . ? N1 Ni1 N2 C6 -171.1(4) 3_656 . . . ? N2 Ni1 N2 C6 94(100) 3_656 . . . ? Br1 Ni1 N2 C6 -83.0(4) 3_656 . . . ? Br1 Ni1 N2 C6 97.0(4) . . . . ? N1 Ni1 N2 C7 178.3(5) . . . . ? N1 Ni1 N2 C7 -1.7(5) 3_656 . . . ? N2 Ni1 N2 C7 -97(100) 3_656 . . . ? Br1 Ni1 N2 C7 86.5(5) 3_656 . . . ? Br1 Ni1 N2 C7 -93.5(5) . . . . ? C7 C12 C11 C10 -0.8(9) . . . . ? C15 C12 C11 C10 172.3(5) . . . . ? C9 C10 C11 C12 0.7(9) . . . . ? C14 C10 C11 C12 -179.8(6) . . . . ? C7 N2 C6 C5 179.7(5) . . . . ? Ni1 N2 C6 C5 -8.1(6) . . . . ? C7 C8 C9 C10 0.6(9) . . . . ? C13 C8 C9 C10 -177.3(6) . . . . ? C11 C10 C9 C8 -0.5(9) . . . . ? C14 C10 C9 C8 179.9(6) . . . . ? C22 C15 C16 C21 -104.6(7) . . . . ? C12 C15 C16 C21 23.5(8) . . . . ? C22 C15 C16 C17 71.8(7) . . . . ? C12 C15 C16 C17 -160.2(5) . . . . ? C16 C15 C22 C23 -153.3(5) . . . . ? C12 C15 C22 C23 79.1(7) . . . . ? C16 C15 C22 C27 26.1(8) . . . . ? C12 C15 C22 C27 -101.5(6) . . . . ? C4 C3 C2 C1 1.1(10) . . . . ? C5 N1 C1 C2 -1.5(9) . . . . ? Ni1 N1 C1 C2 177.0(5) . . . . ? C3 C2 C1 N1 0.0(10) . . . . ? C2 C3 C4 C5 -0.8(10) . . . . ? C1 N1 C5 C4 1.9(8) . . . . ? Ni1 N1 C5 C4 -176.7(5) . . . . ? C1 N1 C5 C6 -173.8(5) . . . . ? Ni1 N1 C5 C6 7.5(6) . . . . ? C3 C4 C5 N1 -0.8(9) . . . . ? C3 C4 C5 C6 174.7(6) . . . . ? N2 C6 C5 N1 1.4(8) . . . . ? N2 C6 C5 C4 -174.3(6) . . . . ? C17 C16 C21 C20 2.5(10) . . . . ? C15 C16 C21 C20 178.8(6) . . . . ? C25 C26 C27 C22 -2.3(10) . . . . ? C23 C22 C27 C26 2.2(9) . . . . ? C15 C22 C27 C26 -177.2(6) . . . . ? C27 C26 C25 C24 -0.1(10) . . . . ? C27 C22 C23 C24 0.2(10) . . . . ? C15 C22 C23 C24 179.6(6) . . . . ? C21 C16 C17 C18 -3.1(10) . . . . ? C15 C16 C17 C18 -179.6(6) . . . . ? C22 C23 C24 C25 -2.6(11) . . . . ? C26 C25 C24 C23 2.5(11) . . . . ? C18 C19 C20 C21 -4.6(13) . . . . ? C16 C21 C20 C19 1.3(12) . . . . ? C16 C17 C18 C19 -0.1(11) . . . . ? C20 C19 C18 C17 3.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.752 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.141 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; #==END data_D7 _database_code_depnum_ccdc_archive 'CCDC 877853' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H64 Br2 N4 Ni1' _chemical_formula_weight 1275.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.955(2) _cell_length_b 12.075(2) _cell_length_c 14.474(3) _cell_angle_alpha 94.80(3) _cell_angle_beta 112.89(3) _cell_angle_gamma 93.79(3) _cell_volume 1907.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17090 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6027 _exptl_absorpt_correction_T_max 0.7217 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 17090 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8677 _reflns_number_gt 7192 _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^)+(0.0679P)^2^+2.4735P] 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 8677 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0635 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 -0.10671(3) -0.17368(3) 0.37525(2) 0.03096(12) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.5000 0.01950(13) Uani 1 2 d S . . N1 N -0.1502(2) 0.0846(2) 0.4496(2) 0.0230(5) Uani 1 1 d . . . N2 N 0.0295(2) 0.0888(2) 0.37747(18) 0.0184(5) Uani 1 1 d . . . C1 C -0.2403(3) 0.0814(3) 0.4830(3) 0.0279(7) Uani 1 1 d . . . H1A H -0.2383 0.0337 0.5307 0.033 Uiso 1 1 calc R . . C2 C -0.3370(3) 0.1469(3) 0.4490(3) 0.0319(8) Uani 1 1 d . . . H2A H -0.3992 0.1415 0.4724 0.038 Uiso 1 1 calc R . . C3 C -0.3388(3) 0.2208(3) 0.3792(3) 0.0326(8) Uani 1 1 d . . . H3A H -0.4006 0.2672 0.3565 0.039 Uiso 1 1 calc R . . C4 C -0.2454(3) 0.2227(3) 0.3446(3) 0.0289(7) Uani 1 1 d . . . H4A H -0.2448 0.2698 0.2971 0.035 Uiso 1 1 calc R . . C5 C -0.1540(3) 0.1549(3) 0.3810(2) 0.0216(6) Uani 1 1 d . . . C6 C -0.0553(3) 0.1537(3) 0.3449(2) 0.0218(6) Uani 1 1 d . . . H6A H -0.0538 0.2006 0.2975 0.026 Uiso 1 1 calc R . . C7 C 0.1150(3) 0.0871(3) 0.3288(2) 0.0202(6) Uani 1 1 d . . . C8 C 0.0826(3) 0.0165(3) 0.2376(2) 0.0211(6) Uani 1 1 d . . . C9 C 0.1683(3) 0.0111(3) 0.1943(2) 0.0231(6) Uani 1 1 d . . . H9A H 0.1482 -0.0354 0.1343 0.028 Uiso 1 1 calc R . . C10 C 0.2828(3) 0.0727(3) 0.2375(2) 0.0238(6) Uani 1 1 d . . . C11 C 0.3092(3) 0.1444(3) 0.3249(2) 0.0217(6) Uani 1 1 d . . . H11A H 0.3843 0.1879 0.3534 0.026 Uiso 1 1 calc R . . C12 C 0.2272(3) 0.1538(2) 0.3715(2) 0.0205(6) Uani 1 1 d . . . C13 C -0.0434(3) -0.0495(3) 0.1877(2) 0.0208(6) Uani 1 1 d . . . H13A H -0.0617 -0.0762 0.2429 0.025 Uiso 1 1 calc R . . C14 C 0.3738(3) 0.0641(3) 0.1893(3) 0.0321(8) Uani 1 1 d . . . H14A H 0.4470 0.1123 0.2293 0.048 Uiso 1 1 calc R . . H14B H 0.3395 0.0862 0.1226 0.048 Uiso 1 1 calc R . . H14C H 0.3928 -0.0117 0.1854 0.048 Uiso 1 1 calc R . . C15 C 0.2558(3) 0.2404(3) 0.4638(2) 0.0236(6) Uani 1 1 d . . . H15A H 0.2173 0.2077 0.5053 0.028 Uiso 1 1 calc R . . C16 C -0.1185(3) -0.1724(3) 0.0182(2) 0.0282(7) Uani 1 1 d . . . H16A H -0.1704 -0.1197 -0.0113 0.034 Uiso 1 1 calc R . . C17 C -0.1157(4) -0.2697(3) -0.0404(3) 0.0369(8) Uani 1 1 d . . . H17A H -0.1677 -0.2826 -0.1084 0.044 Uiso 1 1 calc R . . C18 C -0.0365(4) -0.3457(3) 0.0020(3) 0.0405(9) Uani 1 1 d . . . H18A H -0.0326 -0.4086 -0.0380 0.049 Uiso 1 1 calc R . . C19 C 0.0374(4) -0.3296(3) 0.1035(3) 0.0370(8) Uani 1 1 d . . . H19A H 0.0899 -0.3822 0.1324 0.044 Uiso 1 1 calc R . . C20 C 0.0331(3) -0.2340(3) 0.1629(3) 0.0300(7) Uani 1 1 d . . . H20A H 0.0823 -0.2235 0.2316 0.036 Uiso 1 1 calc R . . C21 C -0.0437(3) -0.1548(3) 0.1205(2) 0.0228(6) Uani 1 1 d . . . C22 C -0.1435(3) 0.0234(3) 0.1359(2) 0.0251(7) Uani 1 1 d . . . C23 C -0.2581(3) 0.0015(3) 0.1370(3) 0.0331(8) Uani 1 1 d . . . H23A H -0.2734 -0.0588 0.1679 0.040 Uiso 1 1 calc R . . C23A C -0.1249(3) 0.1122(3) 0.0858(3) 0.0315(7) Uani 1 1 d . . . H23B H -0.0496 0.1266 0.0819 0.038 Uiso 1 1 calc R . . C24 C -0.3511(4) 0.0685(4) 0.0924(3) 0.0472(11) Uani 1 1 d . . . H24A H -0.4275 0.0529 0.0939 0.057 Uiso 1 1 calc R . . C24A C -0.2159(4) 0.1787(4) 0.0421(3) 0.0444(10) Uani 1 1 d . . . H24B H -0.2014 0.2380 0.0097 0.053 Uiso 1 1 calc R . . C25 C -0.3292(4) 0.1573(4) 0.0464(3) 0.0500(11) Uani 1 1 d . . . H25A H -0.3902 0.2032 0.0182 0.060 Uiso 1 1 calc R . . C28 C 0.1965(3) 0.3463(3) 0.4329(3) 0.0249(6) Uani 1 1 d . . . C29 C 0.1486(3) 0.3730(3) 0.3345(3) 0.0344(8) Uani 1 1 d . . . H29A H 0.1552 0.3257 0.2831 0.041 Uiso 1 1 calc R . . C30 C 0.0905(4) 0.4703(4) 0.3115(4) 0.0492(11) Uani 1 1 d . . . H30A H 0.0564 0.4854 0.2447 0.059 Uiso 1 1 calc R . . C31 C 0.0836(4) 0.5425(4) 0.3855(5) 0.0551(13) Uani 1 1 d . . . H31A H 0.0475 0.6082 0.3702 0.066 Uiso 1 1 calc R . . C32 C 0.1305(4) 0.5177(3) 0.4833(4) 0.0513(12) Uani 1 1 d . . . H32A H 0.1243 0.5666 0.5338 0.062 Uiso 1 1 calc R . . C33 C 0.1872(3) 0.4211(3) 0.5085(3) 0.0372(8) Uani 1 1 d . . . H33A H 0.2189 0.4062 0.5753 0.045 Uiso 1 1 calc R . . C34 C 0.3910(3) 0.2627(3) 0.5296(2) 0.0243(6) Uani 1 1 d . . . C35 C 0.4669(3) 0.3459(3) 0.5146(2) 0.0255(7) Uani 1 1 d . . . H35A H 0.4339 0.3895 0.4625 0.031 Uiso 1 1 calc R . . C35A C 0.4450(4) 0.1991(3) 0.6087(3) 0.0379(9) Uani 1 1 d . . . H35B H 0.3968 0.1435 0.6211 0.045 Uiso 1 1 calc R . . C36 C 0.5900(3) 0.3647(3) 0.5755(3) 0.0350(8) Uani 1 1 d . . . H36A H 0.6388 0.4211 0.5648 0.042 Uiso 1 1 calc R . . C36A C 0.5677(4) 0.2171(4) 0.6686(3) 0.0465(10) Uani 1 1 d . . . H36B H 0.6012 0.1730 0.7202 0.056 Uiso 1 1 calc R . . C37 C 0.6412(4) 0.2987(4) 0.6533(3) 0.0428(10) Uani 1 1 d . . . H37A H 0.7242 0.3103 0.6941 0.051 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 0.0412(2) 0.02857(19) 0.02480(18) -0.00004(13) 0.01707(15) -0.00561(14) Ni1 0.0190(3) 0.0207(3) 0.0202(3) 0.0025(2) 0.0091(2) 0.0031(2) N1 0.0227(13) 0.0256(14) 0.0217(13) 0.0012(10) 0.0100(11) 0.0028(10) N2 0.0161(12) 0.0205(12) 0.0185(12) 0.0013(9) 0.0070(10) 0.0006(9) C1 0.0272(16) 0.0291(17) 0.0320(17) 0.0059(14) 0.0159(14) 0.0062(13) C2 0.0258(17) 0.0365(19) 0.039(2) 0.0057(15) 0.0176(15) 0.0089(14) C3 0.0229(16) 0.0356(19) 0.040(2) 0.0099(15) 0.0100(15) 0.0160(14) C4 0.0357(18) 0.0236(16) 0.0309(17) 0.0068(13) 0.0155(15) 0.0075(13) C5 0.0255(15) 0.0207(15) 0.0222(14) 0.0027(11) 0.0131(12) 0.0028(12) C6 0.0249(15) 0.0213(15) 0.0209(14) 0.0041(11) 0.0107(12) 0.0006(12) C7 0.0211(14) 0.0218(15) 0.0182(14) 0.0054(11) 0.0077(12) 0.0036(11) C8 0.0209(15) 0.0235(15) 0.0185(14) 0.0055(11) 0.0070(12) 0.0013(12) C9 0.0272(16) 0.0233(15) 0.0194(14) 0.0002(12) 0.0106(13) 0.0010(12) C10 0.0234(15) 0.0256(16) 0.0256(16) 0.0057(12) 0.0128(13) 0.0024(12) C11 0.0189(14) 0.0246(15) 0.0213(14) 0.0032(12) 0.0075(12) 0.0011(11) C12 0.0244(15) 0.0188(14) 0.0196(14) 0.0036(11) 0.0099(12) 0.0021(11) C13 0.0191(14) 0.0243(15) 0.0165(13) 0.0034(11) 0.0048(11) -0.0011(11) C14 0.0270(17) 0.041(2) 0.0302(18) -0.0036(15) 0.0160(14) -0.0039(14) C15 0.0245(15) 0.0252(16) 0.0220(15) -0.0002(12) 0.0118(13) -0.0037(12) C16 0.0311(17) 0.0289(17) 0.0224(16) 0.0008(13) 0.0088(14) 0.0024(13) C17 0.050(2) 0.035(2) 0.0210(16) -0.0038(14) 0.0119(16) -0.0036(17) C18 0.055(2) 0.0252(18) 0.043(2) -0.0103(16) 0.026(2) -0.0034(16) C19 0.041(2) 0.0262(18) 0.043(2) 0.0051(15) 0.0155(17) 0.0075(15) C20 0.0260(17) 0.0308(18) 0.0299(17) 0.0026(14) 0.0079(14) 0.0029(13) C21 0.0213(15) 0.0247(16) 0.0235(15) 0.0020(12) 0.0113(12) -0.0025(12) C22 0.0232(15) 0.0287(17) 0.0195(15) -0.0029(12) 0.0055(12) 0.0024(12) C23 0.0261(17) 0.039(2) 0.0330(18) -0.0020(15) 0.0123(15) 0.0009(14) C23A 0.0291(17) 0.0330(19) 0.0305(18) 0.0050(14) 0.0092(15) 0.0050(14) C24 0.0231(18) 0.073(3) 0.041(2) -0.004(2) 0.0088(16) 0.0118(18) C24A 0.046(2) 0.044(2) 0.043(2) 0.0151(18) 0.0138(19) 0.0164(19) C25 0.045(2) 0.057(3) 0.040(2) 0.001(2) 0.0067(19) 0.022(2) C28 0.0192(14) 0.0217(15) 0.0337(17) 0.0007(13) 0.0112(13) 0.0002(11) C29 0.037(2) 0.0303(18) 0.0371(19) 0.0069(15) 0.0149(16) 0.0047(15) C30 0.042(2) 0.043(2) 0.060(3) 0.020(2) 0.013(2) 0.0076(18) C31 0.034(2) 0.032(2) 0.101(4) 0.013(2) 0.027(3) 0.0103(17) C32 0.045(2) 0.029(2) 0.087(4) -0.015(2) 0.038(3) -0.0022(17) C33 0.0337(19) 0.034(2) 0.045(2) -0.0049(16) 0.0195(17) 0.0005(15) C34 0.0269(16) 0.0200(15) 0.0242(15) -0.0006(12) 0.0094(13) -0.0016(12) C35 0.0245(16) 0.0230(16) 0.0268(16) 0.0013(12) 0.0086(13) -0.0006(12) C35A 0.044(2) 0.0316(19) 0.0308(19) 0.0067(15) 0.0075(16) -0.0046(16) C36 0.0290(18) 0.0289(18) 0.043(2) -0.0026(15) 0.0120(16) -0.0009(14) C36A 0.047(2) 0.045(2) 0.033(2) 0.0135(17) -0.0020(18) 0.0049(19) C37 0.0254(18) 0.046(2) 0.040(2) -0.0050(18) -0.0020(16) 0.0011(16) _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 2.5508(11) . ? Ni1 N1 2.037(3) . ? Ni1 N1 2.037(3) 2_556 ? Ni1 N2 2.275(3) 2_556 ? Ni1 N2 2.275(3) . ? Ni1 Br1 2.5508(11) 2_556 ? N1 C1 1.340(4) . ? N1 C5 1.349(4) . ? N2 C6 1.289(4) . ? N2 C7 1.449(4) . ? C1 C2 1.396(5) . ? C1 H1A 0.9300 . ? C2 C3 1.398(5) . ? C2 H2A 0.9300 . ? C3 C4 1.389(5) . ? C3 H3A 0.9300 . ? C4 C5 1.373(5) . ? C4 H4A 0.9300 . ? C5 C6 1.465(4) . ? C6 H6A 0.9300 . ? C7 C12 1.400(4) . ? C7 C8 1.411(4) . ? C8 C9 1.396(4) . ? C8 C13 1.524(4) . ? C9 C10 1.393(4) . ? C9 H9A 0.9300 . ? C10 C11 1.385(4) . ? C10 C14 1.508(4) . ? C11 C12 1.396(4) . ? C11 H11A 0.9300 . ? C12 C15 1.536(4) . ? C13 C22 1.524(4) . ? C13 C21 1.534(4) . ? C13 H13A 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C34 1.514(5) . ? C15 C28 1.519(5) . ? C15 H15A 0.9800 . ? C16 C21 1.389(5) . ? C16 C17 1.401(5) . ? C16 H16A 0.9300 . ? C17 C18 1.368(6) . ? C17 H17A 0.9300 . ? C18 C19 1.378(6) . ? C18 H18A 0.9300 . ? C19 C20 1.397(5) . ? C19 H19A 0.9300 . ? C20 C21 1.382(5) . ? C20 H20A 0.9300 . ? C22 C23 1.384(5) . ? C22 C23A 1.395(5) . ? C23 C24 1.398(6) . ? C23 H23A 0.9300 . ? C23A C24A 1.376(5) . ? C23A H23B 0.9300 . ? C24 C25 1.371(7) . ? C24 H24A 0.9300 . ? C24A C25 1.389(7) . ? C24A H24B 0.9300 . ? C25 H25A 0.9300 . ? C28 C29 1.389(5) . ? C28 C33 1.402(5) . ? C29 C30 1.402(5) . ? C29 H29A 0.9300 . ? C30 C31 1.356(7) . ? C30 H30A 0.9300 . ? C31 C32 1.372(8) . ? C31 H31A 0.9300 . ? C32 C33 1.392(6) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.396(5) . ? C34 C35A 1.398(5) . ? C35 C36 1.381(5) . ? C35 H35A 0.9300 . ? C35A C36A 1.374(6) . ? C35A H35B 0.9300 . ? C36 C37 1.398(6) . ? C36 H36A 0.9300 . ? C36A C37 1.366(6) . ? C36A H36B 0.9300 . ? C37 H37A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.000(1) . 2_556 ? N1 Ni1 N2 101.64(10) . 2_556 ? N1 Ni1 N2 78.36(10) 2_556 2_556 ? N1 Ni1 N2 78.36(10) . . ? N1 Ni1 N2 101.64(10) 2_556 . ? N2 Ni1 N2 180.0 2_556 . ? N1 Ni1 Br1 93.25(8) . . ? N1 Ni1 Br1 86.75(8) 2_556 . ? N2 Ni1 Br1 88.64(7) 2_556 . ? N2 Ni1 Br1 91.36(7) . . ? N1 Ni1 Br1 86.75(8) . 2_556 ? N1 Ni1 Br1 93.25(8) 2_556 2_556 ? N2 Ni1 Br1 91.36(7) 2_556 2_556 ? N2 Ni1 Br1 88.64(7) . 2_556 ? Br1 Ni1 Br1 180.0 . 2_556 ? C1 N1 C5 118.0(3) . . ? C1 N1 Ni1 125.8(2) . . ? C5 N1 Ni1 116.0(2) . . ? C6 N2 C7 116.0(3) . . ? C6 N2 Ni1 107.81(19) . . ? C7 N2 Ni1 136.19(19) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 118.9(3) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3A 121.0 . . ? C2 C3 H3A 121.0 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C5 121.2(3) . . ? N2 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C12 C7 C8 120.8(3) . . ? C12 C7 N2 120.8(3) . . ? C8 C7 N2 118.4(3) . . ? C9 C8 C7 117.9(3) . . ? C9 C8 C13 121.6(3) . . ? C7 C8 C13 120.4(3) . . ? C10 C9 C8 122.5(3) . . ? C10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? C11 C10 C9 117.8(3) . . ? C11 C10 C14 121.0(3) . . ? C9 C10 C14 121.2(3) . . ? C10 C11 C12 122.3(3) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C11 C12 C7 118.5(3) . . ? C11 C12 C15 120.8(3) . . ? C7 C12 C15 120.5(3) . . ? C22 C13 C8 112.7(3) . . ? C22 C13 C21 113.9(2) . . ? C8 C13 C21 112.2(3) . . ? C22 C13 H13A 105.8 . . ? C8 C13 H13A 105.8 . . ? C21 C13 H13A 105.8 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C34 C15 C28 113.0(3) . . ? C34 C15 C12 113.0(3) . . ? C28 C15 C12 111.1(3) . . ? C34 C15 H15A 106.4 . . ? C28 C15 H15A 106.4 . . ? C12 C15 H15A 106.4 . . ? C21 C16 C17 119.9(3) . . ? C21 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C16 119.2(3) . . ? C20 C21 C13 119.0(3) . . ? C16 C21 C13 121.8(3) . . ? C23 C22 C23A 117.9(3) . . ? C23 C22 C13 119.6(3) . . ? C23A C22 C13 122.4(3) . . ? C22 C23 C24 121.1(4) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C24A C23A C22 121.3(4) . . ? C24A C23A H23B 119.4 . . ? C22 C23A H23B 119.4 . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C23A C24A C25 120.0(4) . . ? C23A C24A H24B 120.0 . . ? C25 C24A H24B 120.0 . . ? C24 C25 C24A 119.9(4) . . ? C24 C25 H25A 120.0 . . ? C24A C25 H25A 120.0 . . ? C29 C28 C33 117.8(3) . . ? C29 C28 C15 124.3(3) . . ? C33 C28 C15 117.9(3) . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C31 C30 C29 120.6(4) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C30 C31 C32 119.3(4) . . ? C30 C31 H31A 120.4 . . ? C32 C31 H31A 120.4 . . ? C31 C32 C33 121.5(4) . . ? C31 C32 H32A 119.3 . . ? C33 C32 H32A 119.3 . . ? C32 C33 C28 119.9(4) . . ? C32 C33 H33A 120.1 . . ? C28 C33 H33A 120.1 . . ? C35 C34 C35A 117.1(3) . . ? C35 C34 C15 122.4(3) . . ? C35A C34 C15 120.5(3) . . ? C36 C35 C34 121.4(3) . . ? C36 C35 H35A 119.3 . . ? C34 C35 H35A 119.3 . . ? C36A C35A C34 121.4(4) . . ? C36A C35A H35B 119.3 . . ? C34 C35A H35B 119.3 . . ? C35 C36 C37 119.9(4) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C37 C36A C35A 121.0(4) . . ? C37 C36A H36B 119.5 . . ? C35A C36A H36B 119.5 . . ? C36A C37 C36 119.1(4) . . ? C36A C37 H37A 120.4 . . ? C36 C37 H37A 120.4 . . ? 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 N1 C1 -162(83) 2_556 . . . ? N2 Ni1 N1 C1 -1.5(3) 2_556 . . . ? N2 Ni1 N1 C1 178.5(3) . . . . ? Br1 Ni1 N1 C1 87.8(3) . . . . ? Br1 Ni1 N1 C1 -92.2(3) 2_556 . . . ? N1 Ni1 N1 C5 13(83) 2_556 . . . ? N2 Ni1 N1 C5 174.2(2) 2_556 . . . ? N2 Ni1 N1 C5 -5.8(2) . . . . ? Br1 Ni1 N1 C5 -96.5(2) . . . . ? Br1 Ni1 N1 C5 83.5(2) 2_556 . . . ? N1 Ni1 N2 C6 5.4(2) . . . . ? N1 Ni1 N2 C6 -174.6(2) 2_556 . . . ? N2 Ni1 N2 C6 175(100) 2_556 . . . ? Br1 Ni1 N2 C6 98.4(2) . . . . ? Br1 Ni1 N2 C6 -81.6(2) 2_556 . . . ? N1 Ni1 N2 C7 -172.8(3) . . . . ? N1 Ni1 N2 C7 7.2(3) 2_556 . . . ? N2 Ni1 N2 C7 -3(100) 2_556 . . . ? Br1 Ni1 N2 C7 -79.8(3) . . . . ? Br1 Ni1 N2 C7 100.2(3) 2_556 . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Ni1 N1 C1 C2 176.1(3) . . . . ? N1 C1 C2 C3 -1.5(5) . . . . ? C1 C2 C3 C4 1.9(5) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C1 N1 C5 C4 0.2(5) . . . . ? Ni1 N1 C5 C4 -175.9(3) . . . . ? C1 N1 C5 C6 -178.6(3) . . . . ? Ni1 N1 C5 C6 5.3(4) . . . . ? C3 C4 C5 N1 0.3(5) . . . . ? C3 C4 C5 C6 179.0(3) . . . . ? C7 N2 C6 C5 174.1(3) . . . . ? Ni1 N2 C6 C5 -4.5(3) . . . . ? N1 C5 C6 N2 0.0(4) . . . . ? C4 C5 C6 N2 -178.8(3) . . . . ? C6 N2 C7 C12 96.2(3) . . . . ? Ni1 N2 C7 C12 -85.7(4) . . . . ? C6 N2 C7 C8 -84.0(4) . . . . ? Ni1 N2 C7 C8 94.1(3) . . . . ? C12 C7 C8 C9 3.2(4) . . . . ? N2 C7 C8 C9 -176.6(3) . . . . ? C12 C7 C8 C13 -175.6(3) . . . . ? N2 C7 C8 C13 4.6(4) . . . . ? C7 C8 C9 C10 -0.3(5) . . . . ? C13 C8 C9 C10 178.5(3) . . . . ? C8 C9 C10 C11 -2.3(5) . . . . ? C8 C9 C10 C14 179.4(3) . . . . ? C9 C10 C11 C12 2.0(5) . . . . ? C14 C10 C11 C12 -179.7(3) . . . . ? C10 C11 C12 C7 0.8(5) . . . . ? C10 C11 C12 C15 -175.5(3) . . . . ? C8 C7 C12 C11 -3.5(4) . . . . ? N2 C7 C12 C11 176.3(3) . . . . ? C8 C7 C12 C15 172.9(3) . . . . ? N2 C7 C12 C15 -7.4(4) . . . . ? C9 C8 C13 C22 -103.8(3) . . . . ? C7 C8 C13 C22 74.9(4) . . . . ? C9 C8 C13 C21 26.3(4) . . . . ? C7 C8 C13 C21 -155.0(3) . . . . ? C11 C12 C15 C34 -32.1(4) . . . . ? C7 C12 C15 C34 151.6(3) . . . . ? C11 C12 C15 C28 96.2(3) . . . . ? C7 C12 C15 C28 -80.0(3) . . . . ? C21 C16 C17 C18 -2.2(6) . . . . ? C16 C17 C18 C19 2.7(6) . . . . ? C17 C18 C19 C20 -1.3(6) . . . . ? C18 C19 C20 C21 -0.7(6) . . . . ? C19 C20 C21 C16 1.3(5) . . . . ? C19 C20 C21 C13 -178.5(3) . . . . ? C17 C16 C21 C20 0.2(5) . . . . ? C17 C16 C21 C13 179.9(3) . . . . ? C22 C13 C21 C20 -172.1(3) . . . . ? C8 C13 C21 C20 58.4(4) . . . . ? C22 C13 C21 C16 8.1(4) . . . . ? C8 C13 C21 C16 -121.3(3) . . . . ? C8 C13 C22 C23 -144.1(3) . . . . ? C21 C13 C22 C23 86.7(4) . . . . ? C8 C13 C22 C23A 36.5(4) . . . . ? C21 C13 C22 C23A -92.8(4) . . . . ? C23A C22 C23 C24 -2.2(5) . . . . ? C13 C22 C23 C24 178.4(3) . . . . ? C23 C22 C23A C24A 2.5(5) . . . . ? C13 C22 C23A C24A -178.1(3) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C22 C23A C24A C25 -0.7(6) . . . . ? C23 C24 C25 C24A 1.6(7) . . . . ? C23A C24A C25 C24 -1.3(7) . . . . ? C34 C15 C28 C29 113.6(4) . . . . ? C12 C15 C28 C29 -14.7(4) . . . . ? C34 C15 C28 C33 -67.7(4) . . . . ? C12 C15 C28 C33 164.0(3) . . . . ? C33 C28 C29 C30 -1.5(5) . . . . ? C15 C28 C29 C30 177.2(3) . . . . ? C28 C29 C30 C31 2.4(6) . . . . ? C29 C30 C31 C32 -2.2(7) . . . . ? C30 C31 C32 C33 1.3(7) . . . . ? C31 C32 C33 C28 -0.4(6) . . . . ? C29 C28 C33 C32 0.5(5) . . . . ? C15 C28 C33 C32 -178.2(3) . . . . ? C28 C15 C34 C35 -37.3(4) . . . . ? C12 C15 C34 C35 90.0(4) . . . . ? C28 C15 C34 C35A 142.9(3) . . . . ? C12 C15 C34 C35A -89.8(4) . . . . ? C35A C34 C35 C36 -0.1(5) . . . . ? C15 C34 C35 C36 -180.0(3) . . . . ? C35 C34 C35A C36A -0.6(6) . . . . ? C15 C34 C35A C36A 179.3(4) . . . . ? C34 C35 C36 C37 0.8(5) . . . . ? C34 C35A C36A C37 0.6(7) . . . . ? C35A C36A C37 C36 0.1(7) . . . . ? C35 C36 C37 C36A -0.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.570 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.109 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; 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 -0.230 0.594 0.026 488.1 -1.6 _platon_squeeze_details ; ? ; #==END data_D9 _database_code_depnum_ccdc_archive 'CCDC 877854' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H72 Br2 N4 Ni' _chemical_formula_weight 1331.97 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.921(3) _cell_length_b 12.415(2) _cell_length_c 18.706(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.928(3) _cell_angle_gamma 90.00 _cell_volume 3405.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15957 _cell_measurement_theta_min 1.18 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7733 _exptl_absorpt_correction_T_max 0.9285 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 15957 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11537 _reflns_number_gt 9342 _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. The following restraints were used: SADI 0.02 C13 C14 C13 C14' SADI 0.02 C14 C15 C14' C15' SADI 0.01 C13 C15 C13 C15' SIMU 0.01 0.02 1.7 C14 C14' SIMU 0.01 0.02 1.7 C15 C15' ISOR 0.005 0.01 C14 C14' C15 C15' ; _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^)+(0.0384P)^2^+4.9995P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.497(11) _refine_ls_number_reflns 11537 _refine_ls_number_parameters 822 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _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 0.88597(6) 0.61783(8) 0.70099(5) 0.0323(2) Uani 1 1 d . . . N1 N 0.9637(4) 0.6956(5) 0.8026(3) 0.0307(13) Uani 1 1 d . . . Br1 Br 0.81339(6) 0.69279(7) 0.57361(4) 0.0490(2) Uani 1 1 d . . . N1A N 0.8752(4) 0.4581(5) 0.7237(3) 0.0299(14) Uani 1 1 d . . . C1 C 0.9611(5) 0.7880(7) 0.9193(4) 0.0406(19) Uani 1 1 d . . . H1C H 1.0269 0.7962 0.9338 0.061 Uiso 1 1 calc R . . H1A H 0.9499 0.7478 0.9598 0.061 Uiso 1 1 calc R . . H1B H 0.9327 0.8593 0.9133 0.061 Uiso 1 1 calc R . . C1A C 0.9484(5) 0.2802(6) 0.7414(5) 0.044(2) Uani 1 1 d . . . H1AB H 0.8953 0.2561 0.7512 0.065 Uiso 1 1 calc R . . H1AC H 1.0041 0.2656 0.7871 0.065 Uiso 1 1 calc R . . H1AA H 0.9507 0.2414 0.6965 0.065 Uiso 1 1 calc R . . N2 N 0.7863(4) 0.6669(4) 0.7385(3) 0.0299(13) Uani 1 1 d . . . Br2 Br 1.14852(6) 0.24359(8) 0.93426(5) 0.0601(3) Uani 1 1 d . . . N2A N 0.9982(4) 0.5559(5) 0.6865(4) 0.0348(15) Uani 1 1 d . . . C2A C 0.9411(5) 0.3964(6) 0.7253(4) 0.0301(16) Uani 1 1 d . . . C2 C 0.9210(5) 0.7283(5) 0.8445(4) 0.0302(16) Uani 1 1 d . . . C3 C 0.8206(5) 0.7073(6) 0.8124(4) 0.0281(15) Uani 1 1 d . . . C3A C 1.0145(5) 0.4507(6) 0.7097(5) 0.0381(19) Uani 1 1 d . . . C4 C 0.7631(5) 0.7333(6) 0.8501(4) 0.0377(18) Uani 1 1 d . . . H4 H 0.7871 0.7625 0.9011 0.045 Uiso 1 1 calc R . . C4A C 1.0943(6) 0.4003(7) 0.7173(6) 0.057(3) Uani 1 1 d . . . H4A H 1.1046 0.3274 0.7338 0.068 Uiso 1 1 calc R . . C5 C 0.6706(5) 0.7160(7) 0.8121(5) 0.044(2) Uani 1 1 d . . . H5 H 0.6304 0.7307 0.8374 0.053 Uiso 1 1 calc R . . C5A C 1.1605(6) 0.4572(8) 0.7005(6) 0.062(3) Uani 1 1 d . . . H5A H 1.2160 0.4235 0.7052 0.074 Uiso 1 1 calc R . . C6 C 0.6373(5) 0.6776(7) 0.7379(4) 0.0402(19) Uani 1 1 d . . . H6 H 0.5736 0.6685 0.7103 0.048 Uiso 1 1 calc R . . C6A C 1.1435(6) 0.5624(8) 0.6772(6) 0.059(3) Uani 1 1 d . . . H6A H 1.1877 0.6033 0.6665 0.071 Uiso 1 1 calc R . . C7 C 0.6971(5) 0.6522(6) 0.7036(5) 0.0364(18) Uani 1 1 d . . . H7 H 0.6733 0.6228 0.6527 0.044 Uiso 1 1 calc R . . C7A C 1.0607(5) 0.6089(8) 0.6693(5) 0.048(2) Uani 1 1 d . . . H7A H 1.0483 0.6809 0.6510 0.058 Uiso 1 1 calc R . . C8 C 1.0594(5) 0.7277(6) 0.8242(4) 0.0340(17) Uani 1 1 d . A . C8A C 0.7967(5) 0.4161(6) 0.7373(4) 0.0312(17) Uani 1 1 d . . . C9A C 0.7160(5) 0.3934(6) 0.6739(4) 0.0310(16) Uani 1 1 d . . . C9 C 1.0782(5) 0.8148(6) 0.7865(4) 0.0344(17) Uani 1 1 d . . . C10A C 0.6398(5) 0.3623(6) 0.6895(4) 0.0368(18) Uani 1 1 d . . . H10 H 0.5841 0.3461 0.6475 0.044 Uiso 1 1 calc R . . C10 C 1.1702(5) 0.8399(7) 0.8049(5) 0.043(2) Uani 1 1 d . . . H10A H 1.1847 0.8986 0.7792 0.051 Uiso 1 1 calc R . . C11A C 0.6444(5) 0.3549(6) 0.7654(4) 0.0346(17) Uani 1 1 d . . . C11 C 1.2401(5) 0.7821(7) 0.8591(5) 0.045(2) Uani 1 1 d . . . C12A C 0.7266(5) 0.3774(6) 0.8262(4) 0.0345(17) Uani 1 1 d . . . H12 H 0.7301 0.3713 0.8779 0.041 Uiso 1 1 calc R . . C12 C 1.2187(5) 0.6939(7) 0.8932(5) 0.046(2) Uani 1 1 d . A . H12A H 1.2670 0.6528 0.9294 0.056 Uiso 1 1 calc R . . C13A C 0.8039(5) 0.4085(6) 0.8145(4) 0.0333(17) Uani 1 1 d . . . C13 C 1.1281(5) 0.6620(7) 0.8767(5) 0.046(2) Uani 1 1 d D . . C14A C 0.8911(5) 0.4364(7) 0.8811(4) 0.043(2) Uani 1 1 d . . . H14B H 0.9212 0.4950 0.8641 0.052 Uiso 1 1 calc R . . H14A H 0.9317 0.3728 0.8925 0.052 Uiso 1 1 calc R . . C14 C 1.1036(10) 0.5772(13) 0.9254(11) 0.042(4) Uani 0.55(2) 1 d PDU A 1 H14D H 1.0620 0.6102 0.9471 0.051 Uiso 0.55(2) 1 calc PR A 1 H14C H 1.0704 0.5173 0.8911 0.051 Uiso 0.55(2) 1 calc PR A 1 C14' C 1.1125(13) 0.5488(12) 0.9019(9) 0.034(4) Uani 0.45(2) 1 d PDU A 2 H14F H 1.1536 0.4967 0.8917 0.040 Uiso 0.45(2) 1 calc PR A 2 H14E H 1.0488 0.5261 0.8721 0.040 Uiso 0.45(2) 1 calc PR A 2 C15 C 1.1844(13) 0.5327(15) 0.9903(9) 0.062(5) Uani 0.55(2) 1 d PDU A 1 H15A H 1.1648 0.4760 1.0168 0.094 Uiso 0.55(2) 1 calc PR A 1 H15C H 1.2145 0.5903 1.0272 0.094 Uiso 0.55(2) 1 calc PR A 1 H15B H 1.2273 0.5025 0.9696 0.094 Uiso 0.55(2) 1 calc PR A 1 C15' C 1.1320(19) 0.5509(17) 0.9891(10) 0.064(6) Uani 0.45(2) 1 d PDU A 2 H15D H 1.1228 0.4787 1.0060 0.095 Uiso 0.45(2) 1 calc PR A 2 H15E H 1.0904 0.6017 0.9987 0.095 Uiso 0.45(2) 1 calc PR A 2 H15F H 1.1951 0.5736 1.0182 0.095 Uiso 0.45(2) 1 calc PR A 2 C15A C 0.8835(6) 0.4714(8) 0.9563(5) 0.056(2) Uani 1 1 d . . . H15I H 0.9445 0.4874 0.9952 0.084 Uiso 1 1 calc R . . H15G H 0.8559 0.4133 0.9753 0.084 Uiso 1 1 calc R . . H15H H 0.8454 0.5360 0.9468 0.084 Uiso 1 1 calc R . . C16 C 1.3578(6) 0.8422(8) 0.8095(5) 0.052(2) Uani 1 1 d . . . C17 C 0.4439(6) 0.4482(8) 0.7013(6) 0.059(3) Uani 1 1 d . . . H17 H 0.4798 0.5054 0.7319 0.071 Uiso 1 1 calc R . . C19 C 0.7574(5) 0.3098(6) 0.5673(4) 0.0337(18) Uani 1 1 d . . . C20 C 0.4627(6) 0.3552(10) 0.4523(5) 0.060(3) Uani 1 1 d . . . H20 H 0.4210 0.2968 0.4352 0.072 Uiso 1 1 calc R . . C21 C 0.5636(5) 0.3230(7) 0.7844(4) 0.0375(19) Uani 1 1 d . . . H21 H 0.5654 0.3699 0.8285 0.045 Uiso 1 1 calc R . . C22 C 0.8022(6) 1.0042(8) 0.7598(5) 0.047(2) Uani 1 1 d . . . H22 H 0.7375 1.0002 0.7371 0.056 Uiso 1 1 calc R . . C23 C 0.7106(5) 0.4031(6) 0.5899(4) 0.0316(16) Uani 1 1 d . . . H23 H 0.7455 0.4694 0.5884 0.038 Uiso 1 1 calc R . . C24 C 0.8517(5) 0.9423(7) 0.7296(5) 0.0389(19) Uani 1 1 d . . . H24 H 0.8215 0.8964 0.6866 0.047 Uiso 1 1 calc R . . C25 C 0.9887(5) 1.0137(7) 0.8257(5) 0.042(2) Uani 1 1 d . . . H25 H 1.0534 1.0158 0.8495 0.050 Uiso 1 1 calc R . . C32 C 1.0287(5) 0.9439(7) 0.6699(5) 0.039(2) Uani 1 1 d . . . C33 C 0.5747(5) 0.2057(7) 0.8145(4) 0.0391(18) Uani 1 1 d . . . C34 C 0.4348(7) 0.4573(11) 0.4259(6) 0.069(3) Uani 1 1 d . . . H34 H 0.3735 0.4707 0.3917 0.083 Uiso 1 1 calc R . . C40 C 0.9375(5) 1.0769(7) 0.8545(5) 0.044(2) Uani 1 1 d . . . H40 H 0.9676 1.1240 0.8969 0.053 Uiso 1 1 calc R . . C41 C 1.4674(6) 0.8915(8) 0.9962(5) 0.054(2) Uani 1 1 d . . . H41 H 1.5070 0.8390 0.9893 0.065 Uiso 1 1 calc R . . C42 C 0.5944(6) 0.1194(9) 0.7752(5) 0.056(2) Uani 1 1 d . . . H42 H 0.6039 0.1326 0.7289 0.068 Uiso 1 1 calc R . . C43 C 0.9459(5) 0.9470(6) 0.7621(5) 0.0345(18) Uani 1 1 d . . . C44 C 0.8436(6) 1.0726(7) 0.8227(5) 0.045(2) Uani 1 1 d . . . H44 H 0.8083 1.1150 0.8430 0.054 Uiso 1 1 calc R . . C46 C 0.8049(5) 0.3299(7) 0.5199(5) 0.044(2) Uani 1 1 d . . . H46 H 0.8088 0.4012 0.5031 0.053 Uiso 1 1 calc R . . C47 C 0.7520(5) 0.2041(7) 0.5905(4) 0.0427(19) Uani 1 1 d . . . H47 H 0.7214 0.1890 0.6240 0.051 Uiso 1 1 calc R . . C48 C 0.5522(6) 0.3365(8) 0.5041(5) 0.052(2) Uani 1 1 d . . . H48 H 0.5714 0.2652 0.5211 0.063 Uiso 1 1 calc R . . C50 C 1.1029(6) 1.0957(7) 0.6388(7) 0.063(3) Uani 1 1 d . . . H50 H 1.1362 1.1611 0.6540 0.075 Uiso 1 1 calc R . . C51 C 0.8460(6) 0.2472(8) 0.4976(5) 0.053(2) Uani 1 1 d . . . H51 H 0.8807 0.2624 0.4674 0.064 Uiso 1 1 calc R . . C54 C 0.4723(5) 0.3428(7) 0.7186(4) 0.0371(18) Uani 1 1 d . . . C55 C 1.0300(7) 0.9661(9) 0.5419(6) 0.067(3) Uani 1 1 d . . . H55 H 1.0119 0.9411 0.4901 0.080 Uiso 1 1 calc R . . C56 C 1.0040(6) 0.9079(8) 0.5942(5) 0.050(2) Uani 1 1 d . . . H56 H 0.9695 0.8437 0.5777 0.060 Uiso 1 1 calc R . . C61 C 1.3402(5) 0.8091(7) 0.8811(5) 0.047(2) Uani 1 1 d . . . H61 H 1.3756 0.7415 0.9016 0.056 Uiso 1 1 calc R . . C64 C 1.3558(6) 1.0491(9) 1.0153(5) 0.061(3) Uani 1 1 d . . . H64 H 1.3172 1.1046 1.0202 0.073 Uiso 1 1 calc R . . C70 C 0.6001(7) 0.0159(8) 0.8029(7) 0.066(3) Uani 1 1 d . . . H70 H 0.6116 -0.0420 0.7748 0.080 Uiso 1 1 calc R . . C75 C 0.3354(7) 0.2863(10) 0.6131(6) 0.074(3) Uani 1 1 d . . . H75 H 0.2986 0.2290 0.5836 0.088 Uiso 1 1 calc R . . C77 C 0.4169(6) 0.2636(8) 0.6740(5) 0.064(3) Uani 1 1 d . . . H77 H 0.4351 0.1906 0.6853 0.077 Uiso 1 1 calc R . . C78 C 0.9988(5) 0.8795(6) 0.7252(4) 0.0364(18) Uani 1 1 d . . . H78 H 0.9547 0.8244 0.6925 0.044 Uiso 1 1 calc R . . C79 C 0.3623(7) 0.4706(8) 0.6388(7) 0.069(3) Uani 1 1 d . . . H79 H 0.3444 0.5435 0.6265 0.083 Uiso 1 1 calc R . . C80 C 1.0776(6) 1.0399(7) 0.6922(6) 0.059(3) Uani 1 1 d . . . H80 H 1.0937 1.0671 0.7432 0.071 Uiso 1 1 calc R . . C84 C 0.5892(7) -0.0041(10) 0.8703(7) 0.078(3) Uani 1 1 d . . . H84 H 0.5941 -0.0758 0.8892 0.093 Uiso 1 1 calc R . . C86 C 1.4443(7) 1.0457(9) 1.0651(5) 0.068(3) Uani 1 1 d . . . H86 H 1.4676 1.0972 1.1057 0.081 Uiso 1 1 calc R . . C87 C 1.5005(7) 0.9659(9) 1.0559(6) 0.063(3) Uani 1 1 d . . . H87 H 1.5624 0.9623 1.0911 0.076 Uiso 1 1 calc R . . C89 C 1.3751(5) 0.8941(8) 0.9461(5) 0.048(2) Uani 1 1 d . . . C92 C 1.3471(6) 0.9466(8) 0.7809(6) 0.057(2) Uani 1 1 d . . . H92 H 1.3336 1.0026 0.8094 0.068 Uiso 1 1 calc R . . C96 C 0.8379(6) 0.1409(7) 0.5183(6) 0.055(2) Uani 1 1 d . . . H96 H 0.8642 0.0836 0.5004 0.065 Uiso 1 1 calc R . . C97 C 1.3209(6) 0.9731(8) 0.9578(5) 0.058(3) Uani 1 1 d . . . H97 H 1.2579 0.9751 0.9253 0.070 Uiso 1 1 calc R . . C98 C 1.3556(7) 0.9706(10) 0.7119(6) 0.073(3) Uani 1 1 d . . . H98 H 1.3465 1.0426 0.6932 0.088 Uiso 1 1 calc R . . C100 C 0.3074(7) 0.3906(10) 0.5950(6) 0.070(3) Uani 1 1 d . . . H10B H 0.2515 0.4068 0.5533 0.084 Uiso 1 1 calc R . . C101 C 0.4950(7) 0.5373(10) 0.4490(6) 0.071(3) Uani 1 1 d . . . H10C H 0.4760 0.6076 0.4292 0.085 Uiso 1 1 calc R . . C102 C 0.5850(6) 0.5226(7) 0.5012(5) 0.052(2) Uani 1 1 d . . . H10D H 0.6262 0.5815 0.5161 0.062 Uiso 1 1 calc R . . C108 C 1.3782(6) 0.7639(9) 0.7661(6) 0.069(3) Uani 1 1 d . . . H10E H 1.3859 0.6914 0.7838 0.082 Uiso 1 1 calc R . . C118 C 1.0801(8) 1.0570(10) 0.5636(7) 0.076(4) Uani 1 1 d . . . H11 H 1.0994 1.0939 0.5282 0.091 Uiso 1 1 calc R . . C201 C 1.3766(8) 0.8930(13) 0.6705(7) 0.082(4) Uani 1 1 d . . . H20A H 1.3836 0.9106 0.6237 0.098 Uiso 1 1 calc R . . C202 C 1.3875(7) 0.7890(12) 0.6970(7) 0.085(4) Uani 1 1 d . . . H20B H 1.4016 0.7339 0.6682 0.102 Uiso 1 1 calc R . . C204 C 0.7914(6) 0.1207(8) 0.5648(5) 0.051(2) Uani 1 1 d . . . H20C H 0.7860 0.0488 0.5797 0.061 Uiso 1 1 calc R . . C206 C 0.5634(6) 0.1814(8) 0.8826(5) 0.061(3) Uani 1 1 d . . . H20D H 0.5496 0.2379 0.9106 0.073 Uiso 1 1 calc R . . C208 C 0.6130(5) 0.4207(7) 0.5307(4) 0.0373(19) Uani 1 1 d . . . C209 C 0.5715(8) 0.0777(9) 0.9110(6) 0.072(3) Uani 1 1 d . . . H20E H 0.5648 0.0634 0.9584 0.087 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 0.0356(5) 0.0301(5) 0.0347(5) 0.0040(4) 0.0176(4) 0.0009(5) N1 0.026(3) 0.029(3) 0.036(3) 0.008(3) 0.011(3) 0.000(3) Br1 0.0557(5) 0.0570(6) 0.0338(4) 0.0093(4) 0.0170(4) 0.0058(5) N1A 0.028(3) 0.027(3) 0.033(3) 0.001(3) 0.009(3) -0.004(3) C1 0.044(5) 0.040(5) 0.039(4) -0.006(4) 0.017(4) -0.017(4) C1A 0.043(5) 0.035(5) 0.054(5) 0.014(4) 0.020(4) 0.011(4) N2 0.033(3) 0.023(3) 0.033(3) 0.001(3) 0.012(3) 0.006(3) Br2 0.0577(6) 0.0717(7) 0.0532(6) 0.0086(5) 0.0242(5) -0.0005(5) N2A 0.032(3) 0.039(4) 0.038(4) 0.004(3) 0.019(3) 0.000(3) C2A 0.031(4) 0.029(4) 0.030(4) 0.002(3) 0.013(3) 0.003(3) C2 0.040(4) 0.017(4) 0.036(4) 0.005(3) 0.019(3) -0.002(3) C3 0.039(4) 0.027(4) 0.024(3) 0.007(3) 0.018(3) 0.001(3) C3A 0.031(4) 0.039(5) 0.049(5) 0.007(4) 0.020(4) 0.001(4) C4 0.045(4) 0.043(5) 0.032(4) 0.004(4) 0.022(3) 0.003(4) C4A 0.056(6) 0.033(5) 0.091(8) 0.013(5) 0.039(6) 0.008(5) C5 0.037(4) 0.051(6) 0.054(5) 0.001(4) 0.026(4) 0.002(4) C5A 0.043(5) 0.055(6) 0.099(8) 0.013(6) 0.039(5) 0.006(5) C6 0.024(3) 0.047(5) 0.047(5) 0.008(4) 0.011(3) 0.006(4) C6A 0.057(6) 0.055(6) 0.084(7) 0.009(5) 0.049(6) -0.001(5) C7 0.033(4) 0.037(5) 0.038(4) 0.001(3) 0.013(3) -0.004(3) C7A 0.054(5) 0.044(5) 0.063(6) 0.009(5) 0.040(5) 0.004(5) C8 0.030(4) 0.029(4) 0.041(4) 0.000(3) 0.011(3) -0.003(3) C8A 0.032(4) 0.031(4) 0.028(4) 0.001(3) 0.010(3) -0.014(3) C9A 0.032(4) 0.029(4) 0.030(4) 0.000(3) 0.011(3) -0.003(3) C9 0.032(4) 0.032(4) 0.040(4) 0.006(3) 0.015(4) -0.003(4) C10A 0.037(4) 0.036(5) 0.036(4) -0.006(3) 0.011(4) 0.003(4) C10 0.047(5) 0.033(5) 0.051(5) 0.008(4) 0.021(4) -0.002(4) C11A 0.042(4) 0.034(4) 0.029(4) -0.002(3) 0.016(4) -0.001(4) C11 0.035(4) 0.050(6) 0.052(5) 0.013(4) 0.019(4) 0.003(4) C12A 0.050(5) 0.030(4) 0.023(4) 0.005(3) 0.013(3) -0.001(4) C12 0.031(4) 0.040(5) 0.059(5) 0.012(5) 0.008(4) -0.015(4) C13A 0.038(4) 0.023(4) 0.043(4) -0.001(3) 0.020(4) -0.009(4) C13 0.041(4) 0.044(5) 0.051(5) 0.012(4) 0.014(4) -0.010(4) C14A 0.043(5) 0.046(5) 0.037(4) 0.005(4) 0.011(4) -0.019(4) C14 0.040(5) 0.040(5) 0.045(5) -0.002(4) 0.015(4) -0.001(4) C14' 0.031(5) 0.031(5) 0.039(5) 0.002(4) 0.014(4) -0.004(4) C15 0.066(8) 0.068(8) 0.058(8) 0.004(6) 0.030(7) -0.023(7) C15' 0.071(10) 0.072(9) 0.057(8) 0.004(7) 0.035(7) -0.018(8) C15A 0.059(6) 0.063(7) 0.039(5) 0.004(4) 0.012(4) 0.008(5) C16 0.042(5) 0.057(6) 0.063(6) 0.002(5) 0.028(5) 0.001(5) C17 0.046(5) 0.046(6) 0.083(7) -0.002(5) 0.022(5) 0.003(5) C19 0.032(4) 0.043(5) 0.028(4) 0.007(3) 0.015(3) 0.011(4) C20 0.048(5) 0.085(8) 0.030(5) -0.005(5) -0.003(4) -0.007(6) C21 0.032(4) 0.047(5) 0.039(4) -0.005(4) 0.020(4) -0.009(4) C22 0.042(5) 0.065(6) 0.035(5) 0.015(4) 0.018(4) 0.012(4) C23 0.041(4) 0.035(4) 0.020(3) -0.004(3) 0.012(3) -0.006(4) C24 0.029(4) 0.041(5) 0.050(5) 0.004(4) 0.019(4) -0.005(4) C25 0.035(4) 0.039(5) 0.049(5) 0.011(4) 0.014(4) -0.007(4) C32 0.033(4) 0.043(5) 0.047(5) 0.022(4) 0.020(4) 0.012(4) C33 0.036(4) 0.042(5) 0.043(4) 0.003(4) 0.019(3) -0.007(4) C34 0.040(5) 0.115(10) 0.039(5) -0.007(6) 0.002(4) 0.011(7) C40 0.043(5) 0.034(5) 0.045(5) 0.011(4) 0.007(4) -0.001(4) C41 0.049(5) 0.063(7) 0.050(6) 0.016(5) 0.018(5) -0.005(5) C42 0.060(5) 0.065(6) 0.068(6) -0.008(6) 0.050(5) 0.000(6) C43 0.035(4) 0.027(4) 0.043(5) 0.006(3) 0.018(4) -0.003(4) C44 0.054(5) 0.048(5) 0.043(5) 0.007(4) 0.029(4) 0.009(4) C46 0.043(4) 0.046(5) 0.052(5) 0.002(4) 0.028(4) 0.002(4) C47 0.045(4) 0.039(5) 0.047(5) 0.011(4) 0.021(4) 0.010(4) C48 0.053(5) 0.065(6) 0.036(5) 0.001(4) 0.014(4) 0.002(5) C50 0.059(6) 0.035(6) 0.109(9) 0.018(5) 0.049(6) 0.003(5) C51 0.062(6) 0.049(6) 0.063(6) -0.005(5) 0.041(5) -0.004(5) C54 0.035(4) 0.040(5) 0.041(5) -0.001(4) 0.020(4) -0.005(4) C55 0.084(7) 0.071(7) 0.061(6) 0.034(6) 0.046(6) 0.038(6) C56 0.057(6) 0.052(6) 0.051(5) 0.022(5) 0.031(5) 0.020(5) C61 0.034(4) 0.054(6) 0.052(5) 0.016(4) 0.017(4) -0.001(4) C64 0.053(6) 0.087(8) 0.038(5) -0.001(5) 0.012(4) 0.004(6) C70 0.080(7) 0.044(6) 0.099(8) 0.011(6) 0.059(7) 0.002(5) C75 0.062(6) 0.078(9) 0.053(6) -0.010(6) -0.008(5) -0.008(6) C77 0.072(6) 0.052(6) 0.056(6) 0.007(5) 0.011(5) -0.011(6) C78 0.033(4) 0.036(5) 0.035(4) 0.006(3) 0.008(4) -0.002(4) C79 0.046(6) 0.045(6) 0.107(9) 0.009(6) 0.020(6) 0.010(5) C80 0.057(6) 0.048(6) 0.082(7) 0.023(5) 0.038(5) 0.005(5) C84 0.077(8) 0.075(8) 0.093(9) 0.029(7) 0.047(7) -0.001(7) C86 0.077(7) 0.090(8) 0.035(5) 0.011(5) 0.021(5) -0.004(7) C87 0.047(5) 0.087(8) 0.049(6) 0.012(6) 0.011(5) -0.008(6) C89 0.038(5) 0.056(6) 0.051(5) 0.021(5) 0.021(4) -0.007(4) C92 0.060(6) 0.058(6) 0.062(6) 0.008(5) 0.033(5) -0.007(5) C96 0.056(5) 0.039(6) 0.074(7) -0.013(5) 0.030(5) 0.007(5) C97 0.048(5) 0.080(8) 0.047(6) 0.002(5) 0.020(5) -0.002(5) C98 0.065(7) 0.092(9) 0.068(7) 0.013(7) 0.030(6) -0.018(6) C100 0.056(6) 0.085(9) 0.060(7) 0.006(6) 0.013(5) 0.006(7) C101 0.065(7) 0.082(8) 0.049(6) 0.000(6) 0.004(5) 0.036(7) C102 0.065(6) 0.047(6) 0.035(5) -0.003(4) 0.010(4) 0.018(5) C108 0.049(5) 0.074(8) 0.086(8) 0.003(6) 0.029(5) 0.010(6) C118 0.088(8) 0.070(8) 0.102(9) 0.042(7) 0.074(8) 0.026(7) C201 0.066(7) 0.131(12) 0.061(7) -0.018(8) 0.037(6) -0.044(8) C202 0.065(7) 0.114(12) 0.088(9) -0.034(8) 0.042(7) -0.012(8) C204 0.064(6) 0.038(5) 0.046(5) 0.008(4) 0.016(4) 0.014(5) C206 0.085(7) 0.064(7) 0.043(5) -0.009(5) 0.036(5) -0.021(6) C208 0.032(4) 0.054(6) 0.026(4) -0.002(4) 0.012(3) 0.001(4) C209 0.099(8) 0.059(7) 0.067(7) 0.015(6) 0.040(7) -0.017(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 Ni1 N1A 2.050(6) . ? Ni1 N2A 2.058(6) . ? Ni1 N1 2.059(6) . ? Ni1 N2 2.062(5) . ? Ni1 Br1 2.3945(12) . ? N1 C2 1.287(8) . ? N1 C8 1.471(8) . ? N1A C2A 1.290(9) . ? N1A C8A 1.465(8) . ? C1 C2 1.489(10) . ? C1 H1C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1A C2A 1.469(10) . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1A H1AA 0.9800 . ? N2 C7 1.325(8) . ? N2 C3 1.368(8) . ? N2A C7A 1.331(9) . ? N2A C3A 1.369(9) . ? C2A C3A 1.474(10) . ? C2 C3 1.494(9) . ? C3 C4 1.395(9) . ? C3A C4A 1.373(11) . ? C4 C5 1.380(10) . ? C4 H4 0.9500 . ? C4A C5A 1.403(12) . ? C4A H4A 0.9500 . ? C5 C6 1.364(11) . ? C5 H5 0.9500 . ? C5A C6A 1.370(12) . ? C5A H5A 0.9500 . ? C6 C7 1.376(9) . ? C6 H6 0.9500 . ? C6A C7A 1.393(11) . ? C6A H6A 0.9500 . ? C7 H7 0.9500 . ? C7A H7A 0.9500 . ? C8 C9 1.387(10) . ? C8 C13 1.411(10) . ? C8A C9A 1.396(9) . ? C8A C13A 1.407(10) . ? C9A C10A 1.407(10) . ? C9A C23 1.545(9) . ? C9 C10 1.402(10) . ? C9 C78 1.559(10) . ? C10A C11A 1.397(10) . ? C10A H10 0.9500 . ? C10 C11 1.380(11) . ? C10 H10A 0.9500 . ? C11A C12A 1.388(10) . ? C11A C21 1.515(9) . ? C11 C12 1.376(11) . ? C11 C61 1.519(10) . ? C12A C13A 1.385(9) . ? C12A H12 0.9500 . ? C12 C13 1.409(10) . ? C12 H12A 0.9500 . ? C13A C14A 1.500(10) . ? C13 C14' 1.533(14) . ? C13 C14 1.540(14) . ? C14A C15A 1.521(11) . ? C14A H14B 0.9900 . ? C14A H14A 0.9900 . ? C14 C15 1.489(16) . ? C14 H14D 0.9900 . ? C14 H14C 0.9900 . ? C14' C15' 1.537(18) . ? C14' H14F 0.9900 . ? C14' H14E 0.9900 . ? C15 H15A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C15A H15I 0.9800 . ? C15A H15G 0.9800 . ? C15A H15H 0.9800 . ? C16 C108 1.383(13) . ? C16 C92 1.386(12) . ? C16 C61 1.527(11) . ? C17 C54 1.381(11) . ? C17 C79 1.395(13) . ? C17 H17 0.9500 . ? C19 C46 1.395(10) . ? C19 C47 1.395(11) . ? C19 C23 1.523(10) . ? C20 C34 1.370(14) . ? C20 C48 1.395(11) . ? C20 H20 0.9500 . ? C21 C54 1.515(10) . ? C21 C33 1.546(11) . ? C21 H21 1.0000 . ? C22 C24 1.371(11) . ? C22 C44 1.392(11) . ? C22 H22 0.9500 . ? C23 C208 1.532(10) . ? C23 H23 1.0000 . ? C24 C43 1.382(10) . ? C24 H24 0.9500 . ? C25 C40 1.383(11) . ? C25 C43 1.390(11) . ? C25 H25 0.9500 . ? C32 C56 1.389(12) . ? C32 C80 1.396(12) . ? C32 C78 1.523(10) . ? C33 C206 1.389(10) . ? C33 C42 1.401(12) . ? C34 C101 1.331(15) . ? C34 H34 0.9500 . ? C40 C44 1.379(11) . ? C40 H40 0.9500 . ? C41 C87 1.386(13) . ? C41 C89 1.402(11) . ? C41 H41 0.9500 . ? C42 C70 1.375(13) . ? C42 H42 0.9500 . ? C43 C78 1.530(10) . ? C44 H44 0.9500 . ? C46 C51 1.368(11) . ? C46 H46 0.9500 . ? C47 C204 1.390(11) . ? C47 H47 0.9500 . ? C48 C208 1.379(12) . ? C48 H48 0.9500 . ? C50 C118 1.395(15) . ? C50 C80 1.397(12) . ? C50 H50 0.9500 . ? C51 C96 1.395(12) . ? C51 H51 0.9500 . ? C54 C77 1.366(12) . ? C55 C118 1.349(15) . ? C55 C56 1.401(11) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C89 1.541(12) . ? C61 H61 1.0000 . ? C64 C86 1.354(13) . ? C64 C97 1.374(13) . ? C64 H64 0.9500 . ? C70 C84 1.361(13) . ? C70 H70 0.9500 . ? C75 C100 1.368(14) . ? C75 C77 1.382(12) . ? C75 H75 0.9500 . ? C77 H77 0.9500 . ? C78 H78 1.0000 . ? C79 C100 1.365(14) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C84 C209 1.363(15) . ? C84 H84 0.9500 . ? C86 C87 1.390(14) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C89 C97 1.380(12) . ? C92 C98 1.382(12) . ? C92 H92 0.9500 . ? C96 C204 1.367(11) . ? C96 H96 0.9500 . ? C97 H97 0.9500 . ? C98 C201 1.357(16) . ? C98 H98 0.9500 . ? C100 H10B 0.9500 . ? C101 C102 1.396(12) . ? C101 H10C 0.9500 . ? C102 C208 1.382(11) . ? C102 H10D 0.9500 . ? C108 C202 1.393(15) . ? C108 H10E 0.9500 . ? C118 H11 0.9500 . ? C201 C202 1.369(17) . ? C201 H20A 0.9500 . ? C202 H20B 0.9500 . ? C204 H20C 0.9500 . ? C206 C209 1.379(13) . ? C206 H20D 0.9500 . ? C209 H20E 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 N1A Ni1 N2A 79.3(2) . . ? N1A Ni1 N1 109.3(2) . . ? N2A Ni1 N1 93.2(2) . . ? N1A Ni1 N2 94.4(2) . . ? N2A Ni1 N2 168.1(2) . . ? N1 Ni1 N2 79.2(2) . . ? N1A Ni1 Br1 122.39(17) . . ? N2A Ni1 Br1 96.94(17) . . ? N1 Ni1 Br1 128.30(17) . . ? N2 Ni1 Br1 95.00(16) . . ? C2 N1 C8 118.9(6) . . ? C2 N1 Ni1 116.1(4) . . ? C8 N1 Ni1 124.5(4) . . ? C2A N1A C8A 121.8(6) . . ? C2A N1A Ni1 116.5(5) . . ? C8A N1A Ni1 121.8(5) . . ? C2 C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2A C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A C1A H1AA 109.5 . . ? H1AB C1A H1AA 109.5 . . ? H1AC C1A H1AA 109.5 . . ? C7 N2 C3 118.6(6) . . ? C7 N2 Ni1 127.7(5) . . ? C3 N2 Ni1 113.3(4) . . ? C7A N2A C3A 118.7(6) . . ? C7A N2A Ni1 128.1(6) . . ? C3A N2A Ni1 112.4(4) . . ? N1A C2A C1A 125.9(7) . . ? N1A C2A C3A 115.1(7) . . ? C1A C2A C3A 118.9(6) . . ? N1 C2 C1 126.5(6) . . ? N1 C2 C3 115.9(6) . . ? C1 C2 C3 117.6(6) . . ? N2 C3 C4 120.9(6) . . ? N2 C3 C2 114.4(6) . . ? C4 C3 C2 124.5(6) . . ? N2A C3A C4A 121.4(7) . . ? N2A C3A C2A 115.6(6) . . ? C4A C3A C2A 123.0(7) . . ? C5 C4 C3 118.8(7) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C3A C4A C5A 119.5(8) . . ? C3A C4A H4A 120.2 . . ? C5A C4A H4A 120.2 . . ? C6 C5 C4 119.5(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C6A C5A C4A 118.6(8) . . ? C6A C5A H5A 120.7 . . ? C4A C5A H5A 120.7 . . ? C5 C6 C7 119.3(7) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C5A C6A C7A 119.4(8) . . ? C5A C6A H6A 120.3 . . ? C7A C6A H6A 120.3 . . ? N2 C7 C6 122.8(7) . . ? N2 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? N2A C7A C6A 122.4(8) . . ? N2A C7A H7A 118.8 . . ? C6A C7A H7A 118.8 . . ? C9 C8 C13 122.8(7) . . ? C9 C8 N1 118.5(6) . . ? C13 C8 N1 118.3(6) . . ? C9A C8A C13A 122.6(6) . . ? C9A C8A N1A 119.3(6) . . ? C13A C8A N1A 117.9(6) . . ? C8A C9A C10A 117.5(7) . . ? C8A C9A C23 121.1(6) . . ? C10A C9A C23 121.4(6) . . ? C8 C9 C10 117.4(7) . . ? C8 C9 C78 120.1(6) . . ? C10 C9 C78 122.5(7) . . ? C11A C10A C9A 121.4(7) . . ? C11A C10A H10 119.3 . . ? C9A C10A H10 119.3 . . ? C11 C10 C9 122.1(7) . . ? C11 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C12A C11A C10A 118.6(7) . . ? C12A C11A C21 118.5(6) . . ? C10A C11A C21 122.9(7) . . ? C12 C11 C10 118.7(7) . . ? C12 C11 C61 118.2(7) . . ? C10 C11 C61 123.1(7) . . ? C13A C12A C11A 122.6(7) . . ? C13A C12A H12 118.7 . . ? C11A C12A H12 118.7 . . ? C11 C12 C13 122.6(8) . . ? C11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C12A C13A C8A 117.3(7) . . ? C12A C13A C14A 121.6(7) . . ? C8A C13A C14A 121.1(6) . . ? C12 C13 C8 116.2(7) . . ? C12 C13 C14' 117.7(10) . . ? C8 C13 C14' 124.7(9) . . ? C12 C13 C14 122.4(9) . . ? C8 C13 C14 120.0(8) . . ? C14' C13 C14 23.3(8) . . ? C13A C14A C15A 116.9(7) . . ? C13A C14A H14B 108.1 . . ? C15A C14A H14B 108.1 . . ? C13A C14A H14A 108.1 . . ? C15A C14A H14A 108.1 . . ? H14B C14A H14A 107.3 . . ? C15 C14 C13 113.5(11) . . ? C15 C14 H14D 108.9 . . ? C13 C14 H14D 108.9 . . ? C15 C14 H14C 108.9 . . ? C13 C14 H14C 108.9 . . ? H14D C14 H14C 107.7 . . ? C13 C14' C15' 108.8(12) . . ? C13 C14' H14F 109.9 . . ? C15' C14' H14F 109.9 . . ? C13 C14' H14E 109.9 . . ? C15' C14' H14E 109.9 . . ? H14F C14' H14E 108.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C14' C15' H15D 109.5 . . ? C14' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C14' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C14A C15A H15I 109.5 . . ? C14A C15A H15G 109.5 . . ? H15I C15A H15G 109.5 . . ? C14A C15A H15H 109.5 . . ? H15I C15A H15H 109.5 . . ? H15G C15A H15H 109.5 . . ? C108 C16 C92 116.9(9) . . ? C108 C16 C61 119.3(9) . . ? C92 C16 C61 123.5(8) . . ? C54 C17 C79 119.8(9) . . ? C54 C17 H17 120.1 . . ? C79 C17 H17 120.1 . . ? C46 C19 C47 118.7(7) . . ? C46 C19 C23 119.0(7) . . ? C47 C19 C23 122.3(6) . . ? C34 C20 C48 120.3(10) . . ? C34 C20 H20 119.8 . . ? C48 C20 H20 119.8 . . ? C11A C21 C54 113.6(6) . . ? C11A C21 C33 110.1(6) . . ? C54 C21 C33 112.7(6) . . ? C11A C21 H21 106.6 . . ? C54 C21 H21 106.6 . . ? C33 C21 H21 106.6 . . ? C24 C22 C44 122.1(8) . . ? C24 C22 H22 118.9 . . ? C44 C22 H22 118.9 . . ? C19 C23 C208 112.1(6) . . ? C19 C23 C9A 112.5(6) . . ? C208 C23 C9A 112.7(6) . . ? C19 C23 H23 106.3 . . ? C208 C23 H23 106.3 . . ? C9A C23 H23 106.3 . . ? C22 C24 C43 119.7(8) . . ? C22 C24 H24 120.2 . . ? C43 C24 H24 120.2 . . ? C40 C25 C43 120.3(7) . . ? C40 C25 H25 119.8 . . ? C43 C25 H25 119.8 . . ? C56 C32 C80 118.7(8) . . ? C56 C32 C78 119.1(8) . . ? C80 C32 C78 122.2(8) . . ? C206 C33 C42 116.8(8) . . ? C206 C33 C21 120.1(8) . . ? C42 C33 C21 123.1(7) . . ? C101 C34 C20 118.8(10) . . ? C101 C34 H34 120.6 . . ? C20 C34 H34 120.6 . . ? C44 C40 C25 121.0(8) . . ? C44 C40 H40 119.5 . . ? C25 C40 H40 119.5 . . ? C87 C41 C89 119.6(10) . . ? C87 C41 H41 120.2 . . ? C89 C41 H41 120.2 . . ? C70 C42 C33 120.8(8) . . ? C70 C42 H42 119.6 . . ? C33 C42 H42 119.6 . . ? C24 C43 C25 119.2(7) . . ? C24 C43 C78 118.1(7) . . ? C25 C43 C78 122.7(7) . . ? C40 C44 C22 117.7(8) . . ? C40 C44 H44 121.1 . . ? C22 C44 H44 121.1 . . ? C51 C46 C19 120.2(8) . . ? C51 C46 H46 119.9 . . ? C19 C46 H46 119.9 . . ? C204 C47 C19 120.1(8) . . ? C204 C47 H47 119.9 . . ? C19 C47 H47 119.9 . . ? C208 C48 C20 120.5(9) . . ? C208 C48 H48 119.7 . . ? C20 C48 H48 119.7 . . ? C118 C50 C80 121.0(10) . . ? C118 C50 H50 119.5 . . ? C80 C50 H50 119.5 . . ? C46 C51 C96 121.2(8) . . ? C46 C51 H51 119.4 . . ? C96 C51 H51 119.4 . . ? C77 C54 C17 117.7(8) . . ? C77 C54 C21 124.4(8) . . ? C17 C54 C21 117.8(8) . . ? C118 C55 C56 121.5(11) . . ? C118 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C32 C56 C55 120.3(10) . . ? C32 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C11 C61 C16 110.7(7) . . ? C11 C61 C89 112.5(7) . . ? C16 C61 C89 112.0(7) . . ? C11 C61 H61 107.1 . . ? C16 C61 H61 107.1 . . ? C89 C61 H61 107.1 . . ? C86 C64 C97 120.8(10) . . ? C86 C64 H64 119.6 . . ? C97 C64 H64 119.6 . . ? C84 C70 C42 120.4(10) . . ? C84 C70 H70 119.8 . . ? C42 C70 H70 119.8 . . ? C100 C75 C77 120.5(10) . . ? C100 C75 H75 119.7 . . ? C77 C75 H75 119.7 . . ? C54 C77 C75 122.1(10) . . ? C54 C77 H77 118.9 . . ? C75 C77 H77 118.9 . . ? C32 C78 C43 113.0(6) . . ? C32 C78 C9 113.0(6) . . ? C43 C78 C9 112.5(6) . . ? C32 C78 H78 105.9 . . ? C43 C78 H78 105.9 . . ? C9 C78 H78 105.9 . . ? C100 C79 C17 121.8(10) . . ? C100 C79 H79 119.1 . . ? C17 C79 H79 119.1 . . ? C32 C80 C50 119.6(10) . . ? C32 C80 H80 120.2 . . ? C50 C80 H80 120.2 . . ? C70 C84 C209 120.7(11) . . ? C70 C84 H84 119.7 . . ? C209 C84 H84 119.7 . . ? C64 C86 C87 119.0(10) . . ? C64 C86 H86 120.5 . . ? C87 C86 H86 120.5 . . ? C41 C87 C86 120.9(9) . . ? C41 C87 H87 119.5 . . ? C86 C87 H87 119.5 . . ? C97 C89 C41 117.8(9) . . ? C97 C89 C61 123.9(8) . . ? C41 C89 C61 118.3(8) . . ? C98 C92 C16 121.3(10) . . ? C98 C92 H92 119.3 . . ? C16 C92 H92 119.3 . . ? C204 C96 C51 118.8(8) . . ? C204 C96 H96 120.6 . . ? C51 C96 H96 120.6 . . ? C64 C97 C89 121.7(9) . . ? C64 C97 H97 119.1 . . ? C89 C97 H97 119.1 . . ? C201 C98 C92 121.0(12) . . ? C201 C98 H98 119.5 . . ? C92 C98 H98 119.5 . . ? C79 C100 C75 118.0(10) . . ? C79 C100 H10B 121.0 . . ? C75 C100 H10B 121.0 . . ? C34 C101 C102 122.9(10) . . ? C34 C101 H10C 118.6 . . ? C102 C101 H10C 118.6 . . ? C208 C102 C101 118.9(10) . . ? C208 C102 H10D 120.6 . . ? C101 C102 H10D 120.6 . . ? C16 C108 C202 121.4(11) . . ? C16 C108 H10E 119.3 . . ? C202 C108 H10E 119.3 . . ? C55 C118 C50 118.9(9) . . ? C55 C118 H11 120.6 . . ? C50 C118 H11 120.6 . . ? C98 C201 C202 119.2(11) . . ? C98 C201 H20A 120.4 . . ? C202 C201 H20A 120.4 . . ? C201 C202 C108 120.2(11) . . ? C201 C202 H20B 119.9 . . ? C108 C202 H20B 119.9 . . ? C96 C204 C47 120.9(9) . . ? C96 C204 H20C 119.5 . . ? C47 C204 H20C 119.5 . . ? C209 C206 C33 122.0(10) . . ? C209 C206 H20D 119.0 . . ? C33 C206 H20D 119.0 . . ? C48 C208 C102 118.5(8) . . ? C48 C208 C23 121.6(8) . . ? C102 C208 C23 119.9(8) . . ? C84 C209 C206 119.3(10) . . ? C84 C209 H20E 120.3 . . ? C206 C209 H20E 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Ni1 N1 C2 -85.0(5) . . . . ? N2A Ni1 N1 C2 -164.8(5) . . . . ? N2 Ni1 N1 C2 5.9(5) . . . . ? Br1 Ni1 N1 C2 93.7(5) . . . . ? N1A Ni1 N1 C8 103.4(5) . . . . ? N2A Ni1 N1 C8 23.6(6) . . . . ? N2 Ni1 N1 C8 -165.7(6) . . . . ? Br1 Ni1 N1 C8 -77.8(6) . . . . ? N2A Ni1 N1A C2A 5.2(5) . . . . ? N1 Ni1 N1A C2A -84.5(5) . . . . ? N2 Ni1 N1A C2A -164.6(5) . . . . ? Br1 Ni1 N1A C2A 96.6(5) . . . . ? N2A Ni1 N1A C8A -174.7(5) . . . . ? N1 Ni1 N1A C8A 95.7(5) . . . . ? N2 Ni1 N1A C8A 15.5(5) . . . . ? Br1 Ni1 N1A C8A -83.2(5) . . . . ? N1A Ni1 N2 C7 -72.4(6) . . . . ? N2A Ni1 N2 C7 -129.8(12) . . . . ? N1 Ni1 N2 C7 178.8(6) . . . . ? Br1 Ni1 N2 C7 50.7(6) . . . . ? N1A Ni1 N2 C3 99.3(5) . . . . ? N2A Ni1 N2 C3 41.9(14) . . . . ? N1 Ni1 N2 C3 -9.5(5) . . . . ? Br1 Ni1 N2 C3 -137.6(5) . . . . ? N1A Ni1 N2A C7A -178.2(7) . . . . ? N1 Ni1 N2A C7A -69.1(7) . . . . ? N2 Ni1 N2A C7A -119.4(12) . . . . ? Br1 Ni1 N2A C7A 60.1(7) . . . . ? N1A Ni1 N2A C3A -9.0(5) . . . . ? N1 Ni1 N2A C3A 100.1(5) . . . . ? N2 Ni1 N2A C3A 49.8(15) . . . . ? Br1 Ni1 N2A C3A -130.7(5) . . . . ? C8A N1A C2A C1A -1.1(11) . . . . ? Ni1 N1A C2A C1A 179.1(6) . . . . ? C8A N1A C2A C3A 179.4(6) . . . . ? Ni1 N1A C2A C3A -0.4(8) . . . . ? C8 N1 C2 C1 -6.7(11) . . . . ? Ni1 N1 C2 C1 -178.8(6) . . . . ? C8 N1 C2 C3 170.8(6) . . . . ? Ni1 N1 C2 C3 -1.3(8) . . . . ? C7 N2 C3 C4 -0.4(10) . . . . ? Ni1 N2 C3 C4 -172.9(6) . . . . ? C7 N2 C3 C2 -175.8(6) . . . . ? Ni1 N2 C3 C2 11.6(7) . . . . ? N1 C2 C3 N2 -7.0(9) . . . . ? C1 C2 C3 N2 170.7(6) . . . . ? N1 C2 C3 C4 177.8(7) . . . . ? C1 C2 C3 C4 -4.5(10) . . . . ? C7A N2A C3A C4A 1.6(12) . . . . ? Ni1 N2A C3A C4A -168.7(7) . . . . ? C7A N2A C3A C2A -178.1(7) . . . . ? Ni1 N2A C3A C2A 11.5(8) . . . . ? N1A C2A C3A N2A -7.6(10) . . . . ? C1A C2A C3A N2A 172.8(7) . . . . ? N1A C2A C3A C4A 172.6(8) . . . . ? C1A C2A C3A C4A -6.9(12) . . . . ? N2 C3 C4 C5 1.0(11) . . . . ? C2 C3 C4 C5 175.9(7) . . . . ? N2A C3A C4A C5A -0.4(14) . . . . ? C2A C3A C4A C5A 179.3(9) . . . . ? C3 C4 C5 C6 -2.2(12) . . . . ? C3A C4A C5A C6A 0.3(16) . . . . ? C4 C5 C6 C7 2.9(12) . . . . ? C4A C5A C6A C7A -1.4(16) . . . . ? C3 N2 C7 C6 1.2(11) . . . . ? Ni1 N2 C7 C6 172.5(6) . . . . ? C5 C6 C7 N2 -2.5(12) . . . . ? C3A N2A C7A C6A -2.7(13) . . . . ? Ni1 N2A C7A C6A 165.9(7) . . . . ? C5A C6A C7A N2A 2.6(15) . . . . ? C2 N1 C8 C9 -97.7(8) . . . . ? Ni1 N1 C8 C9 73.7(8) . . . . ? C2 N1 C8 C13 88.5(9) . . . . ? Ni1 N1 C8 C13 -100.1(7) . . . . ? C2A N1A C8A C9A -98.7(9) . . . . ? Ni1 N1A C8A C9A 81.1(8) . . . . ? C2A N1A C8A C13A 86.2(9) . . . . ? Ni1 N1A C8A C13A -94.0(7) . . . . ? C13A C8A C9A C10A 0.3(11) . . . . ? N1A C8A C9A C10A -174.5(7) . . . . ? C13A C8A C9A C23 179.7(7) . . . . ? N1A C8A C9A C23 4.9(11) . . . . ? C13 C8 C9 C10 -2.8(12) . . . . ? N1 C8 C9 C10 -176.3(7) . . . . ? C13 C8 C9 C78 176.1(7) . . . . ? N1 C8 C9 C78 2.6(11) . . . . ? C8A C9A C10A C11A 0.3(11) . . . . ? C23 C9A C10A C11A -179.1(7) . . . . ? C8 C9 C10 C11 -0.9(12) . . . . ? C78 C9 C10 C11 -179.8(8) . . . . ? C9A C10A C11A C12A -0.9(11) . . . . ? C9A C10A C11A C21 179.3(7) . . . . ? C9 C10 C11 C12 3.2(13) . . . . ? C9 C10 C11 C61 -178.8(8) . . . . ? C10A C11A C12A C13A 1.0(12) . . . . ? C21 C11A C12A C13A -179.2(7) . . . . ? C10 C11 C12 C13 -1.8(14) . . . . ? C61 C11 C12 C13 -179.9(8) . . . . ? C11A C12A C13A C8A -0.4(11) . . . . ? C11A C12A C13A C14A 177.7(7) . . . . ? C9A C8A C13A C12A -0.3(11) . . . . ? N1A C8A C13A C12A 174.6(6) . . . . ? C9A C8A C13A C14A -178.4(7) . . . . ? N1A C8A C13A C14A -3.5(11) . . . . ? C11 C12 C13 C8 -1.7(13) . . . . ? C11 C12 C13 C14' 165.2(11) . . . . ? C11 C12 C13 C14 -168.3(12) . . . . ? C9 C8 C13 C12 4.1(12) . . . . ? N1 C8 C13 C12 177.6(7) . . . . ? C9 C8 C13 C14' -161.8(11) . . . . ? N1 C8 C13 C14' 11.7(14) . . . . ? C9 C8 C13 C14 171.1(11) . . . . ? N1 C8 C13 C14 -15.4(14) . . . . ? C12A C13A C14A C15A -23.0(11) . . . . ? C8A C13A C14A C15A 155.0(8) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C8 C13 C14 C15 -166.6(15) . . . . ? C14' C13 C14 C15 85(3) . . . . ? C12 C13 C14' C15' 80(2) . . . . ? C8 C13 C14' C15' -114.8(17) . . . . ? C14 C13 C14' C15' -28.7(19) . . . . ? C12A C11A C21 C54 157.2(7) . . . . ? C10A C11A C21 C54 -23.0(11) . . . . ? C12A C11A C21 C33 -75.2(9) . . . . ? C10A C11A C21 C33 104.6(8) . . . . ? C46 C19 C23 C208 88.7(9) . . . . ? C47 C19 C23 C208 -89.3(8) . . . . ? C46 C19 C23 C9A -143.1(7) . . . . ? C47 C19 C23 C9A 38.9(10) . . . . ? C8A C9A C23 C19 75.6(9) . . . . ? C10A C9A C23 C19 -105.0(8) . . . . ? C8A C9A C23 C208 -156.5(7) . . . . ? C10A C9A C23 C208 22.9(10) . . . . ? C44 C22 C24 C43 0.1(12) . . . . ? C11A C21 C33 C206 130.3(8) . . . . ? C54 C21 C33 C206 -101.7(9) . . . . ? C11A C21 C33 C42 -51.0(10) . . . . ? C54 C21 C33 C42 77.0(9) . . . . ? C48 C20 C34 C101 1.7(15) . . . . ? C43 C25 C40 C44 2.2(12) . . . . ? C206 C33 C42 C70 1.3(13) . . . . ? C21 C33 C42 C70 -177.4(8) . . . . ? C22 C24 C43 C25 0.9(11) . . . . ? C22 C24 C43 C78 -178.1(7) . . . . ? C40 C25 C43 C24 -2.0(11) . . . . ? C40 C25 C43 C78 177.0(7) . . . . ? C25 C40 C44 C22 -1.2(12) . . . . ? C24 C22 C44 C40 0.0(12) . . . . ? C47 C19 C46 C51 -0.6(12) . . . . ? C23 C19 C46 C51 -178.7(7) . . . . ? C46 C19 C47 C204 -1.8(12) . . . . ? C23 C19 C47 C204 176.3(7) . . . . ? C34 C20 C48 C208 1.5(14) . . . . ? C19 C46 C51 C96 3.1(14) . . . . ? C79 C17 C54 C77 -1.7(13) . . . . ? C79 C17 C54 C21 177.0(8) . . . . ? C11A C21 C54 C77 107.2(9) . . . . ? C33 C21 C54 C77 -18.9(11) . . . . ? C11A C21 C54 C17 -71.4(9) . . . . ? C33 C21 C54 C17 162.5(7) . . . . ? C80 C32 C56 C55 1.5(12) . . . . ? C78 C32 C56 C55 179.5(8) . . . . ? C118 C55 C56 C32 0.9(14) . . . . ? C12 C11 C61 C16 138.5(9) . . . . ? C10 C11 C61 C16 -39.5(12) . . . . ? C12 C11 C61 C89 -95.3(10) . . . . ? C10 C11 C61 C89 86.7(10) . . . . ? C108 C16 C61 C11 -88.2(10) . . . . ? C92 C16 C61 C11 86.2(11) . . . . ? C108 C16 C61 C89 145.5(8) . . . . ? C92 C16 C61 C89 -40.2(11) . . . . ? C33 C42 C70 C84 -1.9(15) . . . . ? C17 C54 C77 C75 0.5(14) . . . . ? C21 C54 C77 C75 -178.1(9) . . . . ? C100 C75 C77 C54 0.3(17) . . . . ? C56 C32 C78 C43 -124.9(8) . . . . ? C80 C32 C78 C43 53.0(10) . . . . ? C56 C32 C78 C9 105.9(8) . . . . ? C80 C32 C78 C9 -76.1(10) . . . . ? C24 C43 C78 C32 97.9(8) . . . . ? C25 C43 C78 C32 -81.0(9) . . . . ? C24 C43 C78 C9 -132.6(7) . . . . ? C25 C43 C78 C9 48.4(10) . . . . ? C8 C9 C78 C32 -159.5(7) . . . . ? C10 C9 C78 C32 19.4(11) . . . . ? C8 C9 C78 C43 71.1(9) . . . . ? C10 C9 C78 C43 -110.1(8) . . . . ? C54 C17 C79 C100 2.1(16) . . . . ? C56 C32 C80 C50 -1.8(12) . . . . ? C78 C32 C80 C50 -179.7(8) . . . . ? C118 C50 C80 C32 -0.1(14) . . . . ? C42 C70 C84 C209 0.8(17) . . . . ? C97 C64 C86 C87 1.8(15) . . . . ? C89 C41 C87 C86 -2.5(14) . . . . ? C64 C86 C87 C41 1.0(15) . . . . ? C87 C41 C89 C97 1.2(12) . . . . ? C87 C41 C89 C61 -179.1(8) . . . . ? C11 C61 C89 C97 -29.5(11) . . . . ? C16 C61 C89 C97 95.9(9) . . . . ? C11 C61 C89 C41 150.7(7) . . . . ? C16 C61 C89 C41 -83.8(9) . . . . ? C108 C16 C92 C98 0.6(14) . . . . ? C61 C16 C92 C98 -173.9(8) . . . . ? C46 C51 C96 C204 -3.1(14) . . . . ? C86 C64 C97 C89 -3.1(15) . . . . ? C41 C89 C97 C64 1.6(13) . . . . ? C61 C89 C97 C64 -178.1(8) . . . . ? C16 C92 C98 C201 -1.4(15) . . . . ? C17 C79 C100 C75 -1.2(17) . . . . ? C77 C75 C100 C79 0.0(17) . . . . ? C20 C34 C101 C102 -2.2(16) . . . . ? C34 C101 C102 C208 -0.4(15) . . . . ? C92 C16 C108 C202 0.1(14) . . . . ? C61 C16 C108 C202 174.8(9) . . . . ? C56 C55 C118 C50 -2.8(15) . . . . ? C80 C50 C118 C55 2.4(15) . . . . ? C92 C98 C201 C202 1.4(17) . . . . ? C98 C201 C202 C108 -0.7(18) . . . . ? C16 C108 C202 C201 -0.1(17) . . . . ? C51 C96 C204 C47 0.6(13) . . . . ? C19 C47 C204 C96 1.8(13) . . . . ? C42 C33 C206 C209 0.4(13) . . . . ? C21 C33 C206 C209 179.1(9) . . . . ? C20 C48 C208 C102 -4.0(12) . . . . ? C20 C48 C208 C23 177.7(7) . . . . ? C101 C102 C208 C48 3.5(12) . . . . ? C101 C102 C208 C23 -178.2(7) . . . . ? C19 C23 C208 C48 48.4(9) . . . . ? C9A C23 C208 C48 -79.7(9) . . . . ? C19 C23 C208 C102 -129.8(7) . . . . ? C9A C23 C208 C102 102.1(8) . . . . ? C70 C84 C209 C206 0.8(18) . . . . ? C33 C206 C209 C84 -1.4(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.600 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.314 0.240 0.846 66 24 ' ' 2 0.542 0.375 0.417 8 2 ' ' 3 0.686 0.740 0.154 66 24 ' ' 4 0.458 0.875 0.583 8 2 ' ' _platon_squeeze_details ; ; #==END