# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 #TrackingRef '- CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Dr. Wen-Hua Sun Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; loop_ _publ_author_name _publ_author_address 'Zihong Zhou' ; College of Chemistry Xiangtan University Xiangtan 411105 China ; 'Xiang Hao' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Langqiu Chen' ; School of Chemistry University of East Anglia Norwich NR4 7TJ UK ; 'Carl Redshaw' ; College of Chemistry Xiangtan University Xiangtan 411105 China ; 'Wen-Hua Sun' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; _publ_contact_author_email whsun@iccas.ac.cn _publ_contact_author_name 'Dr. Wen-Hua Sun' data_Ni3 _database_code_depnum_ccdc_archive 'CCDC 862949' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H84 Br0 N2 Ni O2' _chemical_formula_weight 1284.30 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' 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 10.515(2) _cell_length_b 13.887(3) _cell_length_c 15.272(3) _cell_angle_alpha 80.61(3) _cell_angle_beta 71.05(3) _cell_angle_gamma 70.10(3) _cell_volume 1979.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 371 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 682 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7508 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17859 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9014 _reflns_number_gt 7073 _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^)+(0.1040P)^2^+0.6578P] 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 9014 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0985 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.5000 0.0000 0.01950(16) Uani 1 2 d S . . O1 O 0.4533(2) 0.56862(15) 0.10654(14) 0.0243(4) Uani 1 1 d . . . N1 N 0.4916(2) 0.62246(19) -0.07770(16) 0.0210(5) Uani 1 1 d . . . C1 C 0.4033(3) 0.6678(2) 0.1189(2) 0.0236(6) Uani 1 1 d . . . C2 C 0.3608(3) 0.7034(2) 0.2105(2) 0.0257(6) Uani 1 1 d . . . C3 C 0.3058(4) 0.8073(2) 0.2213(2) 0.0309(7) Uani 1 1 d . . . H3 H 0.2752 0.8297 0.2824 0.037 Uiso 1 1 calc R . . C4 C 0.2915(4) 0.8824(2) 0.1490(2) 0.0302(7) Uani 1 1 d . . . C5 C 0.3357(3) 0.8494(2) 0.0614(2) 0.0280(7) Uani 1 1 d . . . H4 H 0.3297 0.8983 0.0103 0.034 Uiso 1 1 calc R . . C6 C 0.3907(3) 0.7430(2) 0.0455(2) 0.0229(6) Uani 1 1 d . . . C7 C 0.4425(3) 0.7153(2) -0.0484(2) 0.0239(6) Uani 1 1 d . . . H1 H 0.4412 0.7701 -0.0947 0.029 Uiso 1 1 calc R . . C8 C 0.3854(4) 0.6300(3) 0.2929(2) 0.0311(7) Uani 1 1 d . . . H5 H 0.3897 0.5610 0.2786 0.037 Uiso 1 1 calc R . . C9 C 0.2400(4) 0.9953(2) 0.1719(2) 0.0353(8) Uani 1 1 d . . . H2 H 0.1592 1.0019 0.2300 0.042 Uiso 1 1 calc R . . C10 C 0.2614(4) 0.6622(3) 0.3806(2) 0.0344(8) Uani 1 1 d . . . C11 C 0.1396(4) 0.6387(3) 0.3932(3) 0.0466(9) Uani 1 1 d . . . H11A H 0.1345 0.6008 0.3487 0.056 Uiso 1 1 calc R . . C12 C 0.0239(5) 0.6697(3) 0.4702(3) 0.0570(11) Uani 1 1 d . . . H12A H -0.0587 0.6518 0.4778 0.068 Uiso 1 1 calc R . . C13 C 0.0261(5) 0.7247(4) 0.5344(3) 0.0590(12) Uani 1 1 d . . . H13A H -0.0538 0.7456 0.5867 0.071 Uiso 1 1 calc R . . C14 C 0.1465(5) 0.7496(4) 0.5225(3) 0.0583(12) Uani 1 1 d . . . H14A H 0.1494 0.7886 0.5670 0.070 Uiso 1 1 calc R . . C15 C 0.2638(5) 0.7189(3) 0.4466(2) 0.0464(9) Uani 1 1 d . . . H15A H 0.3462 0.7368 0.4397 0.056 Uiso 1 1 calc R . . C16 C 0.5267(4) 0.6189(3) 0.3089(2) 0.0356(8) Uani 1 1 d . . . C17 C 0.5713(4) 0.5456(3) 0.3759(3) 0.0403(8) Uani 1 1 d . . . H17A H 0.5135 0.5043 0.4098 0.048 Uiso 1 1 calc R . . C18 C 0.6976(5) 0.5314(3) 0.3944(3) 0.0515(10) Uani 1 1 d . . . H18A H 0.7266 0.4804 0.4396 0.062 Uiso 1 1 calc R . . C19 C 0.7797(5) 0.5922(4) 0.3462(3) 0.0669(14) Uani 1 1 d . . . H19A H 0.8656 0.5842 0.3588 0.080 Uiso 1 1 calc R . . C20 C 0.7385(6) 0.6640(5) 0.2802(4) 0.0793(17) Uani 1 1 d . . . H20 H 0.7963 0.7054 0.2470 0.095 Uiso 1 1 calc R . . C21 C 0.6125(5) 0.6773(4) 0.2610(3) 0.0566(12) Uani 1 1 d . . . H21 H 0.5858 0.7272 0.2144 0.068 Uiso 1 1 calc R . . C22 C 0.3537(5) 1.0217(3) 0.1958(2) 0.0405(9) Uani 1 1 d . . . C22A C 0.1808(4) 1.0691(3) 0.0988(3) 0.0447(9) Uani 1 1 d . . . C23 C 0.3159(6) 1.0909(3) 0.2621(3) 0.0582(12) Uani 1 1 d . . . H23A H 0.2188 1.1213 0.2933 0.070 Uiso 1 1 calc R . . C23A C 0.2402(5) 1.1449(3) 0.0491(3) 0.0544(11) Uani 1 1 d . . . H23B H 0.3217 1.1510 0.0590 0.065 Uiso 1 1 calc R . . C24 C 0.4190(8) 1.1168(4) 0.2838(4) 0.0740(16) Uani 1 1 d . . . H24A H 0.3914 1.1640 0.3301 0.089 Uiso 1 1 calc R . . C24A C 0.1784(7) 1.2118(4) -0.0152(3) 0.0742(16) Uani 1 1 d . . . H24B H 0.2185 1.2634 -0.0491 0.089 Uiso 1 1 calc R . . C25 C 0.5584(7) 1.0753(4) 0.2394(4) 0.0703(15) Uani 1 1 d . . . H25A H 0.6279 1.0948 0.2530 0.084 Uiso 1 1 calc R . . C25A C 0.0601(7) 1.2038(4) -0.0302(4) 0.0780(17) Uani 1 1 d . . . H25B H 0.0199 1.2493 -0.0746 0.094 Uiso 1 1 calc R . . C26 C 0.5977(6) 1.0046(3) 0.1743(3) 0.0600(12) Uani 1 1 d . . . H26 H 0.6950 0.9732 0.1445 0.072 Uiso 1 1 calc R . . C26A C 0.0008(6) 1.1311(4) 0.0185(4) 0.0709(15) Uani 1 1 d . . . H26A H -0.0813 1.1262 0.0085 0.085 Uiso 1 1 calc R . . C27 C 0.4956(5) 0.9792(3) 0.1523(3) 0.0479(10) Uani 1 1 d . . . H27A H 0.5240 0.9315 0.1063 0.057 Uiso 1 1 calc R . . C27A C 0.0601(5) 1.0636(3) 0.0830(3) 0.0549(11) Uani 1 1 d . . . H27B H 0.0177 1.0131 0.1167 0.066 Uiso 1 1 calc R . . C34 C 0.5447(3) 0.6216(2) -0.17773(19) 0.0233(6) Uani 1 1 d . . . C35 C 0.6904(3) 0.5982(2) -0.2179(2) 0.0290(7) Uani 1 1 d . . . C36 C 0.7404(4) 0.6032(3) -0.3145(2) 0.0351(8) Uani 1 1 d . . . H36A H 0.8392 0.5874 -0.3438 0.042 Uiso 1 1 calc R . . C37 C 0.6485(4) 0.6309(3) -0.3682(2) 0.0389(8) Uani 1 1 d . . . H37A H 0.6846 0.6334 -0.4339 0.047 Uiso 1 1 calc R . . C38 C 0.5037(4) 0.6550(3) -0.3266(2) 0.0342(8) Uani 1 1 d . . . H38A H 0.4418 0.6747 -0.3644 0.041 Uiso 1 1 calc R . . C39 C 0.4475(3) 0.6508(2) -0.2300(2) 0.0279(7) Uani 1 1 d . . . C40 C 0.2896(4) 0.6781(3) -0.1831(2) 0.0340(7) Uani 1 1 d . . . H40A H 0.2677 0.7242 -0.1327 0.041 Uiso 1 1 calc R . . C41 C 0.2430(4) 0.5854(3) -0.1370(3) 0.0455(9) Uani 1 1 d . . . H41A H 0.2973 0.5492 -0.0936 0.068 Uiso 1 1 calc R . . H41B H 0.2594 0.5392 -0.1845 0.068 Uiso 1 1 calc R . . H41C H 0.1421 0.6079 -0.1033 0.068 Uiso 1 1 calc R . . C42 C 0.1992(4) 0.7372(3) -0.2467(3) 0.0448(9) Uani 1 1 d . . . H42A H 0.2291 0.7971 -0.2769 0.067 Uiso 1 1 calc R . . H42B H 0.0996 0.7600 -0.2101 0.067 Uiso 1 1 calc R . . H42C H 0.2108 0.6926 -0.2941 0.067 Uiso 1 1 calc R . . C43 C 0.7923(4) 0.5727(3) -0.1601(2) 0.0390(8) Uani 1 1 d . . . H43A H 0.7347 0.5935 -0.0959 0.047 Uiso 1 1 calc R . . C44 C 0.8697(5) 0.4611(3) -0.1527(3) 0.0590(12) Uani 1 1 d . . . H44A H 0.9377 0.4501 -0.1181 0.088 Uiso 1 1 calc R . . H44B H 0.9200 0.4362 -0.2150 0.088 Uiso 1 1 calc R . . H44C H 0.8022 0.4235 -0.1202 0.088 Uiso 1 1 calc R . . C45 C 0.8983(5) 0.6343(4) -0.1953(4) 0.0590(12) Uani 1 1 d . . . H45A H 0.9491 0.6262 -0.1497 0.089 Uiso 1 1 calc R . . H45B H 0.8473 0.7071 -0.2044 0.089 Uiso 1 1 calc R . . H45C H 0.9659 0.6089 -0.2544 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0215(3) 0.0184(3) 0.0183(3) -0.0018(2) -0.0062(2) -0.0050(2) O1 0.0300(11) 0.0196(10) 0.0224(10) 0.0003(8) -0.0093(9) -0.0055(9) N1 0.0209(12) 0.0238(12) 0.0178(11) -0.0007(9) -0.0063(9) -0.0060(10) C1 0.0243(15) 0.0234(14) 0.0226(14) -0.0044(12) -0.0069(11) -0.0053(12) C2 0.0290(16) 0.0256(15) 0.0201(14) -0.0035(12) -0.0055(12) -0.0059(12) C3 0.0379(18) 0.0278(16) 0.0240(15) -0.0076(13) -0.0044(13) -0.0078(14) C4 0.0358(18) 0.0228(15) 0.0285(16) -0.0050(13) -0.0084(13) -0.0041(13) C5 0.0341(17) 0.0229(15) 0.0237(15) -0.0014(12) -0.0073(13) -0.0056(13) C6 0.0247(15) 0.0200(14) 0.0222(14) -0.0038(11) -0.0063(11) -0.0040(11) C7 0.0251(15) 0.0217(14) 0.0238(15) -0.0013(12) -0.0077(12) -0.0056(12) C8 0.0382(18) 0.0276(16) 0.0256(16) -0.0024(13) -0.0094(14) -0.0072(14) C9 0.046(2) 0.0243(16) 0.0292(17) -0.0065(13) -0.0078(15) -0.0030(14) C10 0.047(2) 0.0300(17) 0.0219(15) 0.0003(13) -0.0098(14) -0.0074(15) C11 0.047(2) 0.045(2) 0.042(2) -0.0082(18) -0.0039(17) -0.0127(18) C12 0.049(3) 0.054(3) 0.055(3) -0.007(2) 0.003(2) -0.014(2) C13 0.062(3) 0.053(3) 0.039(2) -0.007(2) 0.004(2) -0.005(2) C14 0.077(3) 0.056(3) 0.0281(19) -0.0123(18) -0.011(2) -0.003(2) C15 0.061(3) 0.046(2) 0.0304(19) -0.0055(16) -0.0145(18) -0.0112(19) C16 0.0383(19) 0.0379(19) 0.0272(16) -0.0048(14) -0.0114(14) -0.0045(15) C17 0.049(2) 0.038(2) 0.0364(19) -0.0042(16) -0.0190(17) -0.0099(17) C18 0.057(3) 0.054(2) 0.041(2) -0.0056(19) -0.0217(19) -0.005(2) C19 0.047(3) 0.102(4) 0.055(3) -0.001(3) -0.024(2) -0.020(3) C20 0.058(3) 0.116(5) 0.074(4) 0.023(3) -0.026(3) -0.046(3) C21 0.044(2) 0.080(3) 0.044(2) 0.018(2) -0.0142(19) -0.025(2) C22 0.067(3) 0.0216(16) 0.0332(18) 0.0017(14) -0.0194(18) -0.0104(16) C22A 0.054(2) 0.0279(18) 0.040(2) -0.0123(16) -0.0120(18) 0.0046(17) C23 0.098(4) 0.032(2) 0.045(2) -0.0074(18) -0.029(2) -0.011(2) C23A 0.075(3) 0.034(2) 0.043(2) -0.0013(17) -0.014(2) -0.005(2) C24 0.131(5) 0.039(2) 0.072(3) -0.013(2) -0.053(4) -0.026(3) C24A 0.100(4) 0.042(3) 0.058(3) 0.008(2) -0.023(3) 0.000(3) C25 0.114(5) 0.047(3) 0.076(3) 0.014(2) -0.056(3) -0.037(3) C25A 0.091(4) 0.054(3) 0.068(3) -0.006(3) -0.039(3) 0.019(3) C26 0.087(4) 0.047(2) 0.063(3) 0.014(2) -0.038(3) -0.034(2) C26A 0.069(3) 0.055(3) 0.076(3) -0.020(3) -0.033(3) 0.016(3) C27 0.072(3) 0.034(2) 0.046(2) -0.0009(17) -0.024(2) -0.021(2) C27A 0.057(3) 0.040(2) 0.058(3) -0.013(2) -0.022(2) 0.006(2) C34 0.0308(16) 0.0183(13) 0.0194(14) 0.0006(11) -0.0065(12) -0.0071(12) C35 0.0312(17) 0.0281(16) 0.0285(16) -0.0024(13) -0.0092(13) -0.0092(13) C36 0.0357(19) 0.0412(19) 0.0277(16) -0.0077(14) 0.0004(14) -0.0173(15) C37 0.053(2) 0.041(2) 0.0228(16) -0.0034(14) -0.0027(15) -0.0215(18) C38 0.048(2) 0.0347(18) 0.0243(16) -0.0031(14) -0.0155(14) -0.0129(16) C39 0.0326(17) 0.0247(15) 0.0282(16) -0.0045(13) -0.0108(13) -0.0079(13) C40 0.0321(18) 0.0358(18) 0.0336(17) -0.0095(14) -0.0132(14) -0.0031(14) C41 0.0321(19) 0.056(2) 0.048(2) 0.0031(19) -0.0145(16) -0.0142(18) C42 0.043(2) 0.042(2) 0.055(2) -0.0044(18) -0.0261(19) -0.0091(17) C43 0.0235(17) 0.055(2) 0.0353(18) -0.0082(17) -0.0052(14) -0.0090(16) C44 0.047(3) 0.057(3) 0.079(3) 0.016(2) -0.034(2) -0.019(2) C45 0.050(3) 0.052(3) 0.088(3) -0.007(2) -0.034(2) -0.016(2) _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 O1 1.862(2) . ? Ni1 O1 1.862(2) 2_665 ? Ni1 N1 1.901(2) 2_665 ? Ni1 N1 1.901(2) . ? O1 C1 1.317(4) . ? N1 C7 1.310(4) . ? N1 C34 1.447(4) . ? C1 C6 1.408(4) . ? C1 C2 1.439(4) . ? C2 C3 1.375(4) . ? C2 C8 1.518(4) . ? C3 C4 1.398(5) . ? C3 H3 0.9500 . ? C4 C5 1.367(4) . ? C4 C9 1.533(4) . ? C5 C6 1.422(4) . ? C5 H4 0.9500 . ? C6 C7 1.425(4) . ? C7 H1 0.9500 . ? C8 C16 1.536(5) . ? C8 C10 1.536(5) . ? C8 H5 1.0000 . ? C9 C22 1.525(5) . ? C9 C22A 1.526(5) . ? C9 H2 1.0000 . ? C10 C11 1.374(5) . ? C10 C15 1.387(5) . ? C11 C12 1.388(6) . ? C11 H11A 0.9500 . ? C12 C13 1.347(6) . ? C12 H12A 0.9500 . ? C13 C14 1.372(7) . ? C13 H13A 0.9500 . ? C14 C15 1.386(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.372(6) . ? C16 C17 1.396(5) . ? C17 C18 1.389(6) . ? C17 H17A 0.9500 . ? C18 C19 1.371(7) . ? C18 H18A 0.9500 . ? C19 C20 1.363(7) . ? C19 H19A 0.9500 . ? C20 C21 1.394(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.379(6) . ? C22 C23 1.380(5) . ? C22A C27A 1.395(6) . ? C22A C23A 1.397(6) . ? C23 C24 1.398(7) . ? C23 H23A 0.9500 . ? C23A C24A 1.399(6) . ? C23A H23B 0.9500 . ? C24 C25 1.359(8) . ? C24 H24A 0.9500 . ? C24A C25A 1.378(8) . ? C24A H24B 0.9500 . ? C25 C26 1.377(7) . ? C25 H25A 0.9500 . ? C25A C26A 1.358(8) . ? C25A H25B 0.9500 . ? C26 C27 1.386(6) . ? C26 H26 0.9500 . ? C26A C27A 1.391(6) . ? C26A H26A 0.9500 . ? C27 H27A 0.9500 . ? C27A H27B 0.9500 . ? C34 C35 1.395(4) . ? C34 C39 1.409(4) . ? C35 C36 1.394(4) . ? C35 C43 1.519(5) . ? C36 C37 1.384(5) . ? C36 H36A 0.9500 . ? C37 C38 1.388(5) . ? C37 H37A 0.9500 . ? C38 C39 1.400(4) . ? C38 H38A 0.9500 . ? C39 C40 1.518(5) . ? C40 C41 1.518(5) . ? C40 C42 1.526(5) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.490(6) . ? C43 C45 1.541(6) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 180.00(12) . 2_665 ? O1 Ni1 N1 87.24(9) . 2_665 ? O1 Ni1 N1 92.76(9) 2_665 2_665 ? O1 Ni1 N1 92.76(9) . . ? O1 Ni1 N1 87.24(9) 2_665 . ? N1 Ni1 N1 180.00(16) 2_665 . ? C1 O1 Ni1 129.59(19) . . ? C7 N1 C34 112.5(2) . . ? C7 N1 Ni1 125.1(2) . . ? C34 N1 Ni1 122.39(19) . . ? O1 C1 C6 123.0(3) . . ? O1 C1 C2 119.9(3) . . ? C6 C1 C2 117.0(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C8 119.9(3) . . ? C1 C2 C8 121.5(3) . . ? C2 C3 C4 124.8(3) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C9 124.5(3) . . ? C3 C4 C9 118.2(3) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H4 119.5 . . ? C6 C5 H4 119.5 . . ? C1 C6 C5 121.6(3) . . ? C1 C6 C7 121.0(3) . . ? C5 C6 C7 117.3(3) . . ? N1 C7 C6 127.0(3) . . ? N1 C7 H1 116.5 . . ? C6 C7 H1 116.5 . . ? C2 C8 C16 112.1(3) . . ? C2 C8 C10 110.9(3) . . ? C16 C8 C10 111.2(3) . . ? C2 C8 H5 107.4 . . ? C16 C8 H5 107.4 . . ? C10 C8 H5 107.4 . . ? C22 C9 C22A 114.0(3) . . ? C22 C9 C4 110.3(3) . . ? C22A C9 C4 113.5(3) . . ? C22 C9 H2 106.1 . . ? C22A C9 H2 106.1 . . ? C4 C9 H2 106.1 . . ? C11 C10 C15 117.8(4) . . ? C11 C10 C8 119.4(3) . . ? C15 C10 C8 122.8(4) . . ? C10 C11 C12 120.8(4) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 121.5(5) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C14 118.4(4) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? C13 C14 C15 121.2(4) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C10 120.3(4) . . ? C14 C15 H15A 119.9 . . ? C10 C15 H15A 119.9 . . ? C21 C16 C17 117.7(4) . . ? C21 C16 C8 123.6(3) . . ? C17 C16 C8 118.7(3) . . ? C18 C17 C16 121.9(4) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C16 C21 C20 120.5(4) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C27 C22 C23 117.9(4) . . ? C27 C22 C9 122.0(3) . . ? C23 C22 C9 120.0(4) . . ? C27A C22A C23A 118.4(4) . . ? C27A C22A C9 119.1(4) . . ? C23A C22A C9 122.4(4) . . ? C22 C23 C24 120.6(5) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C22A C23A C24A 119.4(5) . . ? C22A C23A H23B 120.3 . . ? C24A C23A H23B 120.3 . . ? C25 C24 C23 120.8(4) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C25A C24A C23A 120.9(5) . . ? C25A C24A H24B 119.5 . . ? C23A C24A H24B 119.5 . . ? C24 C25 C26 119.2(5) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C26A C25A C24A 120.1(5) . . ? C26A C25A H25B 120.0 . . ? C24A C25A H25B 120.0 . . ? C25 C26 C27 120.1(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C25A C26A C27A 120.2(5) . . ? C25A C26A H26A 119.9 . . ? C27A C26A H26A 119.9 . . ? C22 C27 C26 121.3(4) . . ? C22 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? C26A C27A C22A 121.0(5) . . ? C26A C27A H27B 119.5 . . ? C22A C27A H27B 119.5 . . ? C35 C34 C39 123.1(3) . . ? C35 C34 N1 117.7(3) . . ? C39 C34 N1 119.0(3) . . ? C36 C35 C34 117.6(3) . . ? C36 C35 C43 120.2(3) . . ? C34 C35 C43 122.1(3) . . ? C37 C36 C35 121.0(3) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 120.4(3) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C37 C38 C39 121.1(3) . . ? C37 C38 H38A 119.5 . . ? C39 C38 H38A 119.5 . . ? C38 C39 C34 116.8(3) . . ? C38 C39 C40 121.9(3) . . ? C34 C39 C40 121.3(3) . . ? C39 C40 C41 112.8(3) . . ? C39 C40 C42 114.2(3) . . ? C41 C40 C42 109.1(3) . . ? C39 C40 H40A 106.8 . . ? C41 C40 H40A 106.8 . . ? C42 C40 H40A 106.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C35 113.4(3) . . ? C44 C43 C45 109.9(3) . . ? C35 C43 C45 112.1(3) . . ? C44 C43 H43A 107.0 . . ? C35 C43 H43A 107.0 . . ? C45 C43 H43A 107.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.422 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.146 _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 -0.262 0.159 0.868 414.0 113.4 2 0.108 0.666 0.366 26.9 7.1 _platon_squeeze_details ; ? ; #==END data_Ni6 _database_code_depnum_ccdc_archive 'CCDC 862950' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H56 F4 N2 Ni O2' _chemical_formula_weight 1187.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.225(9) _cell_length_b 16.333(3) _cell_length_c 17.278(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.26(3) _cell_angle_gamma 90.00 _cell_volume 12503(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19101 _cell_measurement_theta_min 1.2562 _cell_measurement_theta_max 27.4717 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4944 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6700 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34999 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10994 _reflns_number_gt 9129 _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^)+(0.0864P)^2^+58.6397P] 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 10994 _refine_ls_number_parameters 786 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1155 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2436 _refine_ls_wR_factor_gt 0.2313 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni2 Ni 0.2500 0.7500 0.0000 0.0286(2) Uani 1 2 d S . . F4 F 0.25194(6) 0.80284(17) 0.17760(18) 0.0375(7) Uani 1 1 d . . . F3 F 0.18445(7) 0.59312(19) 0.04538(18) 0.0417(8) Uani 1 1 d . . . Ni1 Ni 0.0000 0.24959(6) 0.2500 0.0360(3) Uani 1 2 d S . . O2 O 0.26888(7) 0.67047(19) 0.0765(2) 0.0275(7) Uani 1 1 d . . . O1 O 0.03708(7) 0.2549(2) 0.3334(2) 0.0344(8) Uani 1 1 d . . . F1 F 0.00601(7) 0.3244(2) 0.0141(2) 0.0518(9) Uani 1 1 d . . . F2 F -0.00221(8) 0.0892(2) 0.1607(2) 0.0540(9) Uani 1 1 d . . . N2 N 0.21495(9) 0.7375(2) 0.0317(2) 0.0259(9) Uani 1 1 d . . . N1 N 0.01906(9) 0.2452(3) 0.1684(2) 0.0316(10) Uani 1 1 d . . . C1 C 0.06098(10) 0.2939(3) 0.3290(3) 0.0276(10) Uani 1 1 d . . . C2 C 0.08351(10) 0.3193(3) 0.4040(3) 0.0266(10) Uani 1 1 d . . . C75 C 0.21752(10) 0.7011(3) 0.1085(3) 0.0267(10) Uani 1 1 d . . . C41 C 0.29783(10) 0.6599(3) 0.1153(3) 0.0263(10) Uani 1 1 d . . . C46 C 0.32044(10) 0.6960(3) 0.0897(3) 0.0262(10) Uani 1 1 d . . . C7 C 0.04538(10) 0.2774(3) 0.1773(3) 0.0268(10) Uani 1 1 d . . . H7A H 0.0514 0.2796 0.1303 0.032 Uiso 1 1 calc R . . C3 C 0.10851(10) 0.3609(3) 0.4001(3) 0.0263(10) Uani 1 1 d . . . H3A H 0.1233 0.3784 0.4504 0.032 Uiso 1 1 calc R . . C8 C 0.07956(10) 0.2998(3) 0.4858(3) 0.0287(11) Uani 1 1 d . . . H8A H 0.0619 0.2617 0.4716 0.034 Uiso 1 1 calc R . . C34 C 0.00323(11) 0.2074(3) 0.0911(3) 0.0323(11) Uani 1 1 d . . . C79 C 0.23869(11) 0.7052(3) 0.2578(3) 0.0330(11) Uani 1 1 d . . . H79A H 0.2513 0.7315 0.3066 0.040 Uiso 1 1 calc R . . C49 C 0.39389(11) 0.6166(3) 0.2509(3) 0.0302(11) Uani 1 1 d . . . H49A H 0.4055 0.6513 0.2247 0.036 Uiso 1 1 calc R . . C48 C 0.28422(10) 0.5567(3) 0.2074(3) 0.0260(10) Uani 1 1 d . . . H48A H 0.2646 0.5868 0.1845 0.031 Uiso 1 1 calc R . . C45 C 0.35124(10) 0.6819(3) 0.1334(3) 0.0280(10) Uani 1 1 d . . . H45A H 0.3659 0.7063 0.1145 0.034 Uiso 1 1 calc R . . C63 C 0.40349(10) 0.6438(3) 0.3412(3) 0.0290(11) Uani 1 1 d . . . C22 C 0.13994(11) 0.5170(3) 0.3514(3) 0.0313(11) Uani 1 1 d . . . C4 C 0.11327(10) 0.3787(3) 0.3259(3) 0.0267(10) Uani 1 1 d . . . C50 C 0.27978(11) 0.4742(3) 0.1629(3) 0.0279(10) Uani 1 1 d . . . C80 C 0.23596(11) 0.7356(3) 0.1823(3) 0.0317(11) Uani 1 1 d . . . C43 C 0.33809(10) 0.5962(3) 0.2265(3) 0.0284(10) Uani 1 1 d . . . H43A H 0.3442 0.5617 0.2736 0.034 Uiso 1 1 calc R . . C9 C 0.14172(10) 0.4266(3) 0.3295(3) 0.0280(11) Uani 1 1 d . . . H9A H 0.1589 0.4021 0.3754 0.034 Uiso 1 1 calc R . . C28 C 0.14960(10) 0.4182(3) 0.2516(3) 0.0294(11) Uani 1 1 d . . . C77 C 0.20429(12) 0.5964(3) 0.1908(3) 0.0388(13) Uani 1 1 d . . . H77A H 0.1934 0.5481 0.1934 0.047 Uiso 1 1 calc R . . C42 C 0.30752(10) 0.6067(3) 0.1853(3) 0.0263(10) Uani 1 1 d . . . C10 C 0.07060(10) 0.3733(3) 0.5268(3) 0.0317(11) Uani 1 1 d . . . C64 C 0.38824(11) 0.7068(3) 0.3655(3) 0.0358(12) Uani 1 1 d . . . H64A H 0.3703 0.7289 0.3267 0.043 Uiso 1 1 calc R . . C5 C 0.09183(11) 0.3516(3) 0.2536(3) 0.0278(10) Uani 1 1 d . . . H5A H 0.0947 0.3614 0.2026 0.033 Uiso 1 1 calc R . . C6 C 0.06568(10) 0.3095(3) 0.2539(3) 0.0266(10) Uani 1 1 d . . . C52 C 0.30008(13) 0.3460(3) 0.1380(3) 0.0396(13) Uani 1 1 d . . . H52A H 0.3168 0.3097 0.1496 0.048 Uiso 1 1 calc R . . C44 C 0.36058(10) 0.6331(3) 0.2034(3) 0.0277(10) Uani 1 1 d . . . C51 C 0.30371(12) 0.4200(3) 0.1769(3) 0.0347(12) Uani 1 1 d . . . H51A H 0.3230 0.4348 0.2143 0.042 Uiso 1 1 calc R . . C76 C 0.20222(11) 0.6299(3) 0.1160(3) 0.0331(11) Uani 1 1 d . . . C39 C -0.00778(12) 0.1283(3) 0.0882(3) 0.0394(13) Uani 1 1 d . . . C69 C 0.40160(11) 0.5288(3) 0.2393(3) 0.0355(12) Uani 1 1 d . . . C47 C 0.18748(11) 0.7593(3) -0.0148(3) 0.0286(11) Uani 1 1 d . . . H47 H 0.1715 0.7436 0.0035 0.034 Uiso 1 1 calc R . . C58 C 0.27769(12) 0.4815(3) 0.3281(3) 0.0333(11) Uani 1 1 d . . . H58A H 0.2655 0.4431 0.2896 0.040 Uiso 1 1 calc R . . C33 C 0.13365(11) 0.4611(3) 0.1800(3) 0.0341(12) Uani 1 1 d . . . H33A H 0.1179 0.4972 0.1802 0.041 Uiso 1 1 calc R . . C15 C 0.06878(13) 0.3655(4) 0.6050(4) 0.0460(14) Uani 1 1 d . . . H15A H 0.0757 0.3164 0.6352 0.055 Uiso 1 1 calc R . . C53 C 0.27248(14) 0.3235(4) 0.0823(4) 0.0486(15) Uani 1 1 d . . . H53A H 0.2700 0.2719 0.0554 0.058 Uiso 1 1 calc R . . C57 C 0.29065(11) 0.5465(3) 0.3000(3) 0.0299(11) Uani 1 1 d . . . C78 C 0.22259(12) 0.6348(3) 0.2624(3) 0.0394(13) Uani 1 1 d . . . H78A H 0.2242 0.6130 0.3147 0.047 Uiso 1 1 calc R . . C17 C 0.12992(11) 0.2809(4) 0.6053(3) 0.0412(13) Uani 1 1 d . . . H17A H 0.1293 0.3365 0.6210 0.049 Uiso 1 1 calc R . . C68 C 0.42970(12) 0.6131(3) 0.4006(3) 0.0385(12) Uani 1 1 d . . . H68A H 0.4404 0.5701 0.3859 0.046 Uiso 1 1 calc R . . C21 C 0.10812(13) 0.1690(4) 0.5168(4) 0.0452(14) Uani 1 1 d . . . H21A H 0.0921 0.1461 0.4722 0.054 Uiso 1 1 calc R . . C35 C -0.00349(12) 0.2460(4) 0.0147(3) 0.0398(13) Uani 1 1 d . . . C29 C 0.17285(12) 0.3675(3) 0.2505(4) 0.0399(13) Uani 1 1 d . . . H29A H 0.1841 0.3378 0.2987 0.048 Uiso 1 1 calc R . . C27 C 0.16613(13) 0.5634(4) 0.3740(4) 0.0463(14) Uani 1 1 d . . . H27A H 0.1848 0.5384 0.3786 0.056 Uiso 1 1 calc R . . C16 C 0.10643(11) 0.2498(3) 0.5397(3) 0.0341(12) Uani 1 1 d . . . C59 C 0.28227(15) 0.4720(4) 0.4108(4) 0.0469(15) Uani 1 1 d . . . H59A H 0.2731 0.4273 0.4284 0.056 Uiso 1 1 calc R . . C70 C 0.39429(12) 0.4638(3) 0.2807(4) 0.0486(15) Uani 1 1 d . . . H70A H 0.3856 0.4751 0.3216 0.058 Uiso 1 1 calc R . . C67 C 0.44046(13) 0.6438(4) 0.4802(3) 0.0465(15) Uani 1 1 d . . . H67A H 0.4583 0.6215 0.5192 0.056 Uiso 1 1 calc R . . C31 C 0.16373(14) 0.4009(4) 0.1083(4) 0.0514(16) Uani 1 1 d . . . H31A H 0.1685 0.3946 0.0595 0.062 Uiso 1 1 calc R . . C65 C 0.39883(14) 0.7375(4) 0.4449(4) 0.0455(14) Uani 1 1 d . . . H65A H 0.3880 0.7798 0.4602 0.055 Uiso 1 1 calc R . . C66 C 0.42545(14) 0.7067(4) 0.5032(4) 0.0482(15) Uani 1 1 d . . . H66A H 0.4330 0.7286 0.5574 0.058 Uiso 1 1 calc R . . C61 C 0.31207(16) 0.5925(4) 0.4404(4) 0.0562(17) Uani 1 1 d . . . H61A H 0.3236 0.6319 0.4791 0.067 Uiso 1 1 calc R . . C71 C 0.39923(15) 0.3836(4) 0.2644(5) 0.0620(19) Uani 1 1 d . . . H71A H 0.3943 0.3403 0.2942 0.074 Uiso 1 1 calc R . . C38 C -0.02387(14) 0.0898(4) 0.0162(4) 0.0521(16) Uani 1 1 d . . . H38A H -0.0311 0.0357 0.0171 0.063 Uiso 1 1 calc R . . C60 C 0.29987(16) 0.5263(4) 0.4681(4) 0.0578(17) Uani 1 1 d . . . H60A H 0.3036 0.5186 0.5253 0.069 Uiso 1 1 calc R . . C23 C 0.11353(13) 0.5548(3) 0.3492(4) 0.0423(13) Uani 1 1 d . . . H23A H 0.0954 0.5238 0.3352 0.051 Uiso 1 1 calc R . . C36 C -0.01969(13) 0.2082(4) -0.0593(4) 0.0513(16) Uani 1 1 d . . . H36A H -0.0239 0.2364 -0.1102 0.062 Uiso 1 1 calc R . . C62 C 0.30784(13) 0.6023(3) 0.3580(3) 0.0403(13) Uani 1 1 d . . . H62A H 0.3168 0.6476 0.3407 0.048 Uiso 1 1 calc R . . C24 C 0.11307(15) 0.6374(4) 0.3670(4) 0.0577(17) Uani 1 1 d . . . H24A H 0.0948 0.6625 0.3658 0.069 Uiso 1 1 calc R . . C37 C -0.02943(14) 0.1298(4) -0.0576(4) 0.0580(18) Uani 1 1 d . . . H37A H -0.0402 0.1027 -0.1079 0.070 Uiso 1 1 calc R . . C55 C 0.24842(14) 0.3773(4) 0.0661(4) 0.0577(18) Uani 1 1 d . . . H55A H 0.2293 0.3629 0.0271 0.069 Uiso 1 1 calc R . . C56 C 0.25210(12) 0.4521(3) 0.1065(4) 0.0430(14) Uani 1 1 d . . . H56A H 0.2354 0.4883 0.0953 0.052 Uiso 1 1 calc R . . C13 C 0.04696(15) 0.4999(4) 0.5956(4) 0.0578(18) Uani 1 1 d . . . H13A H 0.0385 0.5423 0.6185 0.069 Uiso 1 1 calc R . . C30 C 0.17982(14) 0.3597(4) 0.1785(4) 0.0482(15) Uani 1 1 d . . . H30A H 0.1960 0.3253 0.1784 0.058 Uiso 1 1 calc R . . C32 C 0.14042(13) 0.4517(4) 0.1088(4) 0.0439(14) Uani 1 1 d . . . H32A H 0.1290 0.4804 0.0601 0.053 Uiso 1 1 calc R . . C14 C 0.05724(14) 0.4271(4) 0.6398(4) 0.0537(17) Uani 1 1 d . . . H14A H 0.0562 0.4204 0.6934 0.064 Uiso 1 1 calc R . . C11 C 0.06120(14) 0.4458(4) 0.4854(4) 0.0490(15) Uani 1 1 d . . . H11A H 0.0628 0.4534 0.4325 0.059 Uiso 1 1 calc R . . C26 C 0.16509(15) 0.6460(4) 0.3898(4) 0.0545(16) Uani 1 1 d . . . H26A H 0.1830 0.6777 0.4035 0.065 Uiso 1 1 calc R . . C19 C 0.15625(16) 0.1537(6) 0.6251(5) 0.070(2) Uani 1 1 d . . . H19A H 0.1734 0.1214 0.6541 0.084 Uiso 1 1 calc R . . C18 C 0.15433(14) 0.2327(5) 0.6488(4) 0.0594(19) Uani 1 1 d . . . H18A H 0.1698 0.2546 0.6953 0.071 Uiso 1 1 calc R . . C25 C 0.13885(15) 0.6828(4) 0.3862(4) 0.0536(16) Uani 1 1 d . . . H25A H 0.1385 0.7397 0.3970 0.064 Uiso 1 1 calc R . . C12 C 0.04924(16) 0.5087(4) 0.5201(4) 0.0585(18) Uani 1 1 d . . . H12A H 0.0427 0.5581 0.4902 0.070 Uiso 1 1 calc R . . C73 C 0.4190(3) 0.4293(6) 0.1648(7) 0.135(5) Uani 1 1 d . . . H73A H 0.4277 0.4168 0.1243 0.162 Uiso 1 1 calc R . . C72 C 0.4109(2) 0.3678(5) 0.2072(6) 0.089(3) Uani 1 1 d . . . H72A H 0.4137 0.3124 0.1948 0.107 Uiso 1 1 calc R . . C74 C 0.4140(2) 0.5111(5) 0.1823(5) 0.094(3) Uani 1 1 d . . . H74A H 0.4196 0.5543 0.1535 0.112 Uiso 1 1 calc R . . C20 C 0.13336(19) 0.1209(5) 0.5592(5) 0.068(2) Uani 1 1 d . . . H20A H 0.1347 0.0659 0.5426 0.082 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 Ni2 0.0254(4) 0.0320(5) 0.0278(5) 0.0054(4) 0.0084(4) 0.0024(4) F4 0.0389(16) 0.0321(15) 0.0357(17) -0.0043(13) 0.0057(13) -0.0051(13) F3 0.0405(17) 0.0457(18) 0.0319(17) 0.0035(14) 0.0037(14) -0.0135(14) Ni1 0.0311(5) 0.0449(6) 0.0294(5) 0.000 0.0073(4) 0.000 O2 0.0198(15) 0.0318(18) 0.0275(18) 0.0068(15) 0.0041(13) 0.0007(13) O1 0.0289(17) 0.048(2) 0.0220(18) 0.0039(16) 0.0038(14) -0.0100(16) F1 0.053(2) 0.059(2) 0.0337(19) 0.0082(16) 0.0027(15) -0.0087(17) F2 0.068(2) 0.0430(19) 0.050(2) 0.0003(17) 0.0188(18) -0.0123(17) N2 0.029(2) 0.025(2) 0.022(2) 0.0060(17) 0.0073(17) 0.0011(16) N1 0.034(2) 0.038(2) 0.017(2) 0.0008(18) 0.0017(17) -0.0069(19) C1 0.027(2) 0.028(2) 0.024(3) -0.001(2) 0.005(2) 0.003(2) C2 0.022(2) 0.029(2) 0.028(3) -0.001(2) 0.008(2) 0.0036(19) C75 0.023(2) 0.029(2) 0.029(3) 0.007(2) 0.008(2) 0.0032(19) C41 0.028(2) 0.027(2) 0.022(2) -0.002(2) 0.008(2) -0.004(2) C46 0.026(2) 0.026(2) 0.024(2) 0.005(2) 0.0049(19) -0.0002(19) C7 0.028(2) 0.028(2) 0.022(2) 0.003(2) 0.005(2) 0.003(2) C3 0.018(2) 0.029(2) 0.026(3) -0.004(2) 0.0004(19) -0.0010(19) C8 0.021(2) 0.041(3) 0.021(2) -0.001(2) 0.0037(19) -0.005(2) C34 0.028(2) 0.043(3) 0.026(3) -0.006(2) 0.010(2) -0.006(2) C79 0.029(2) 0.038(3) 0.027(3) 0.000(2) 0.004(2) 0.005(2) C49 0.027(2) 0.033(3) 0.028(3) 0.004(2) 0.007(2) -0.003(2) C48 0.028(2) 0.025(2) 0.023(3) 0.001(2) 0.008(2) 0.000(2) C45 0.028(2) 0.029(2) 0.027(3) 0.000(2) 0.010(2) -0.004(2) C63 0.026(2) 0.034(3) 0.023(3) 0.006(2) 0.003(2) -0.002(2) C22 0.031(3) 0.038(3) 0.023(3) 0.005(2) 0.007(2) -0.003(2) C4 0.023(2) 0.030(2) 0.026(3) 0.003(2) 0.0065(19) 0.001(2) C50 0.034(3) 0.029(3) 0.021(2) 0.004(2) 0.011(2) -0.005(2) C80 0.029(2) 0.037(3) 0.029(3) -0.001(2) 0.010(2) 0.000(2) C43 0.029(2) 0.030(2) 0.022(3) 0.006(2) 0.004(2) 0.000(2) C9 0.022(2) 0.032(3) 0.026(3) 0.001(2) 0.0031(19) 0.002(2) C28 0.024(2) 0.032(3) 0.032(3) -0.004(2) 0.008(2) -0.005(2) C77 0.034(3) 0.044(3) 0.041(3) 0.016(3) 0.015(2) 0.002(2) C42 0.027(2) 0.027(2) 0.025(3) 0.001(2) 0.008(2) -0.001(2) C10 0.024(2) 0.045(3) 0.026(3) -0.005(2) 0.008(2) -0.005(2) C64 0.029(2) 0.039(3) 0.037(3) 0.005(2) 0.008(2) 0.003(2) C5 0.036(3) 0.023(2) 0.025(3) 0.000(2) 0.011(2) 0.003(2) C6 0.025(2) 0.030(2) 0.022(2) 0.002(2) 0.0057(19) 0.003(2) C52 0.045(3) 0.036(3) 0.035(3) 0.000(2) 0.010(2) 0.011(2) C44 0.026(2) 0.029(2) 0.023(3) 0.000(2) 0.003(2) -0.003(2) C51 0.034(3) 0.039(3) 0.026(3) -0.001(2) 0.004(2) 0.001(2) C76 0.028(2) 0.043(3) 0.024(3) 0.003(2) 0.004(2) 0.000(2) C39 0.038(3) 0.045(3) 0.038(3) -0.003(3) 0.016(2) -0.002(2) C69 0.028(2) 0.040(3) 0.032(3) 0.002(2) 0.002(2) 0.003(2) C47 0.031(2) 0.031(3) 0.025(3) 0.000(2) 0.011(2) -0.003(2) C58 0.043(3) 0.031(3) 0.027(3) 0.001(2) 0.013(2) 0.002(2) C33 0.027(2) 0.040(3) 0.036(3) -0.001(2) 0.013(2) 0.002(2) C15 0.048(3) 0.058(4) 0.033(3) -0.003(3) 0.015(3) -0.004(3) C53 0.054(4) 0.041(3) 0.043(4) -0.014(3) 0.007(3) -0.001(3) C57 0.033(3) 0.031(3) 0.030(3) 0.004(2) 0.016(2) 0.006(2) C78 0.039(3) 0.050(3) 0.027(3) 0.012(3) 0.008(2) 0.008(3) C17 0.027(3) 0.059(4) 0.035(3) 0.014(3) 0.008(2) 0.003(3) C68 0.035(3) 0.042(3) 0.035(3) 0.003(3) 0.007(2) 0.003(2) C21 0.048(3) 0.057(4) 0.030(3) 0.007(3) 0.014(3) 0.011(3) C35 0.036(3) 0.050(3) 0.032(3) 0.000(3) 0.009(2) 0.000(3) C29 0.034(3) 0.038(3) 0.049(4) 0.003(3) 0.015(3) 0.000(2) C27 0.041(3) 0.044(3) 0.047(4) 0.000(3) 0.008(3) -0.011(3) C16 0.032(3) 0.043(3) 0.032(3) 0.007(2) 0.016(2) 0.001(2) C59 0.075(4) 0.038(3) 0.038(3) 0.006(3) 0.033(3) 0.000(3) C70 0.028(3) 0.043(3) 0.069(4) 0.008(3) 0.010(3) 0.002(2) C67 0.042(3) 0.054(4) 0.029(3) 0.007(3) -0.005(2) 0.001(3) C31 0.048(3) 0.068(4) 0.047(4) -0.017(3) 0.028(3) -0.024(3) C65 0.050(3) 0.050(3) 0.037(3) -0.001(3) 0.015(3) 0.006(3) C66 0.056(4) 0.054(4) 0.031(3) -0.004(3) 0.011(3) -0.001(3) C61 0.073(4) 0.062(4) 0.037(4) -0.016(3) 0.024(3) -0.019(4) C71 0.051(4) 0.042(4) 0.083(5) -0.003(4) 0.011(4) 0.001(3) C38 0.049(3) 0.049(4) 0.048(4) -0.026(3) 0.005(3) -0.006(3) C60 0.082(5) 0.068(4) 0.027(3) 0.003(3) 0.024(3) -0.006(4) C23 0.038(3) 0.031(3) 0.054(4) -0.007(3) 0.012(3) -0.006(2) C36 0.045(3) 0.075(5) 0.030(3) -0.010(3) 0.008(3) 0.005(3) C62 0.050(3) 0.042(3) 0.033(3) -0.003(3) 0.018(3) -0.003(3) C24 0.055(4) 0.050(4) 0.067(5) -0.006(3) 0.020(3) 0.000(3) C37 0.049(4) 0.068(4) 0.045(4) -0.028(4) 0.000(3) -0.004(3) C55 0.037(3) 0.054(4) 0.065(5) -0.018(3) -0.003(3) -0.008(3) C56 0.034(3) 0.034(3) 0.053(4) -0.006(3) 0.005(3) 0.002(2) C13 0.059(4) 0.066(4) 0.056(4) -0.026(4) 0.029(3) 0.002(3) C30 0.048(3) 0.048(3) 0.058(4) -0.006(3) 0.030(3) 0.007(3) C32 0.042(3) 0.053(3) 0.037(3) 0.006(3) 0.014(3) -0.008(3) C14 0.050(4) 0.071(4) 0.046(4) -0.020(3) 0.024(3) -0.010(3) C11 0.055(4) 0.053(4) 0.042(3) -0.001(3) 0.020(3) 0.011(3) C26 0.058(4) 0.041(3) 0.056(4) 0.002(3) 0.008(3) -0.015(3) C19 0.054(4) 0.109(7) 0.058(5) 0.055(5) 0.033(4) 0.041(4) C18 0.036(3) 0.097(6) 0.043(4) 0.030(4) 0.011(3) 0.006(3) C25 0.069(4) 0.036(3) 0.050(4) -0.006(3) 0.013(3) -0.005(3) C12 0.072(4) 0.048(4) 0.062(5) 0.000(3) 0.032(4) 0.022(3) C73 0.263(16) 0.081(7) 0.115(9) 0.009(6) 0.133(10) 0.050(8) C72 0.122(8) 0.050(5) 0.085(6) -0.016(5) 0.024(6) 0.017(5) C74 0.167(9) 0.063(5) 0.080(6) 0.021(4) 0.079(6) 0.050(6) C20 0.091(6) 0.068(5) 0.062(5) 0.024(4) 0.046(5) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni2 O2 1.847(3) 7_565 ? Ni2 O2 1.847(3) . ? Ni2 N2 1.926(4) . ? Ni2 N2 1.926(4) 7_565 ? F4 C80 1.351(6) . ? F3 C76 1.359(6) . ? Ni1 O1 1.844(3) 2 ? Ni1 O1 1.844(3) . ? Ni1 N1 1.918(4) 2 ? Ni1 N1 1.918(4) . ? O2 C41 1.309(5) . ? O1 C1 1.321(6) . ? F1 C35 1.358(6) . ? F2 C39 1.348(6) . ? N2 C47 1.316(6) . ? N2 C75 1.420(6) . ? N1 C7 1.309(6) . ? N1 C34 1.426(6) . ? C1 C6 1.414(7) . ? C1 C2 1.425(7) . ? C2 C3 1.384(6) . ? C2 C8 1.521(7) . ? C75 C80 1.390(7) . ? C75 C76 1.399(7) . ? C41 C46 1.418(6) . ? C41 C42 1.430(7) . ? C46 C45 1.406(6) . ? C46 C47 1.419(7) 7_565 ? C7 C6 1.438(7) . ? C7 H7A 0.9500 . ? C3 C4 1.407(7) . ? C3 H3A 0.9500 . ? C8 C16 1.525(7) . ? C8 C10 1.527(7) . ? C8 H8A 1.0000 . ? C34 C39 1.386(8) . ? C34 C35 1.398(8) . ? C79 C80 1.360(7) . ? C79 C78 1.396(8) . ? C79 H79A 0.9500 . ? C49 C69 1.510(7) . ? C49 C44 1.526(6) . ? C49 C63 1.532(7) . ? C49 H49A 1.0000 . ? C48 C42 1.521(6) . ? C48 C50 1.530(7) . ? C48 C57 1.532(7) . ? C48 H48A 1.0000 . ? C45 C44 1.388(7) . ? C45 H45A 0.9500 . ? C63 C68 1.398(7) . ? C63 C64 1.401(7) . ? C22 C23 1.380(7) . ? C22 C27 1.387(7) . ? C22 C9 1.534(7) . ? C4 C5 1.381(7) . ? C4 C9 1.537(6) . ? C50 C56 1.381(7) . ? C50 C51 1.389(7) . ? C43 C42 1.382(6) . ? C43 C44 1.394(7) . ? C43 H43A 0.9500 . ? C9 C28 1.522(7) . ? C9 H9A 1.0000 . ? C28 C29 1.380(7) . ? C28 C33 1.393(7) . ? C77 C76 1.374(7) . ? C77 C78 1.390(8) . ? C77 H77A 0.9500 . ? C10 C11 1.375(8) . ? C10 C15 1.389(7) . ? C64 C65 1.382(8) . ? C64 H64A 0.9500 . ? C5 C6 1.415(7) . ? C5 H5A 0.9500 . ? C52 C51 1.364(7) . ? C52 C53 1.375(8) . ? C52 H52A 0.9500 . ? C51 H51A 0.9500 . ? C39 C38 1.367(8) . ? C69 C74 1.341(9) . ? C69 C70 1.388(8) . ? C47 C46 1.419(7) 7_565 ? C47 H47 0.9500 . ? C58 C59 1.376(7) . ? C58 C57 1.394(7) . ? C58 H58A 0.9500 . ? C33 C32 1.384(8) . ? C33 H33A 0.9500 . ? C15 C14 1.377(8) . ? C15 H15A 0.9500 . ? C53 C55 1.386(8) . ? C53 H53A 0.9500 . ? C57 C62 1.389(7) . ? C78 H78A 0.9500 . ? C17 C16 1.380(8) . ? C17 C18 1.383(8) . ? C17 H17A 0.9500 . ? C68 C67 1.385(8) . ? C68 H68A 0.9500 . ? C21 C16 1.388(8) . ? C21 C20 1.404(9) . ? C21 H21A 0.9500 . ? C35 C36 1.387(8) . ? C29 C30 1.399(8) . ? C29 H29A 0.9500 . ? C27 C26 1.381(8) . ? C27 H27A 0.9500 . ? C59 C60 1.374(9) . ? C59 H59A 0.9500 . ? C70 C71 1.377(9) . ? C70 H70A 0.9500 . ? C67 C66 1.382(8) . ? C67 H67A 0.9500 . ? C31 C30 1.365(9) . ? C31 C32 1.382(9) . ? C31 H31A 0.9500 . ? C65 C66 1.404(8) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C61 C62 1.377(8) . ? C61 C60 1.386(9) . ? C61 H61A 0.9500 . ? C71 C72 1.312(11) . ? C71 H71A 0.9500 . ? C38 C37 1.375(10) . ? C38 H38A 0.9500 . ? C60 H60A 0.9500 . ? C23 C24 1.386(8) . ? C23 H23A 0.9500 . ? C36 C37 1.365(9) . ? C36 H36A 0.9500 . ? C62 H62A 0.9500 . ? C24 C25 1.364(9) . ? C24 H24A 0.9500 . ? C37 H37A 0.9500 . ? C55 C56 1.388(8) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C13 C12 1.354(9) . ? C13 C14 1.405(10) . ? C13 H13A 0.9500 . ? C30 H30A 0.9500 . ? C32 H32A 0.9500 . ? C14 H14A 0.9500 . ? C11 C12 1.403(8) . ? C11 H11A 0.9500 . ? C26 C25 1.359(9) . ? C26 H26A 0.9500 . ? C19 C18 1.366(11) . ? C19 C20 1.378(11) . ? C19 H19A 0.9500 . ? C18 H18A 0.9500 . ? C25 H25A 0.9500 . ? C12 H12A 0.9500 . ? C73 C72 1.373(13) . ? C73 C74 1.407(11) . ? C73 H73A 0.9500 . ? C72 H72A 0.9500 . ? C74 H74A 0.9500 . ? C20 H20A 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 O2 Ni2 O2 180.00(14) 7_565 . ? O2 Ni2 N2 91.64(15) 7_565 . ? O2 Ni2 N2 88.36(14) . . ? O2 Ni2 N2 88.36(14) 7_565 7_565 ? O2 Ni2 N2 91.64(15) . 7_565 ? N2 Ni2 N2 180.0(3) . 7_565 ? O1 Ni1 O1 174.6(2) 2 . ? O1 Ni1 N1 90.89(16) 2 2 ? O1 Ni1 N1 89.31(16) . 2 ? O1 Ni1 N1 89.31(16) 2 . ? O1 Ni1 N1 90.89(16) . . ? N1 Ni1 N1 175.7(3) 2 . ? C41 O2 Ni2 128.2(3) . . ? C1 O1 Ni1 125.2(3) . . ? C47 N2 C75 115.5(4) . . ? C47 N2 Ni2 124.1(3) . . ? C75 N2 Ni2 120.4(3) . . ? C7 N1 C34 116.9(4) . . ? C7 N1 Ni1 124.6(3) . . ? C34 N1 Ni1 118.5(3) . . ? O1 C1 C6 123.3(4) . . ? O1 C1 C2 118.2(4) . . ? C6 C1 C2 118.5(4) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C8 122.0(4) . . ? C1 C2 C8 119.4(4) . . ? C80 C75 C76 115.5(4) . . ? C80 C75 N2 120.7(4) . . ? C76 C75 N2 123.7(4) . . ? O2 C41 C46 123.4(4) . . ? O2 C41 C42 119.0(4) . . ? C46 C41 C42 117.5(4) . . ? C45 C46 C41 121.0(4) . . ? C45 C46 C47 118.1(4) . 7_565 ? C41 C46 C47 120.6(4) . 7_565 ? N1 C7 C6 123.9(4) . . ? N1 C7 H7A 118.1 . . ? C6 C7 H7A 118.1 . . ? C2 C3 C4 123.7(4) . . ? C2 C3 H3A 118.2 . . ? C4 C3 H3A 118.2 . . ? C2 C8 C16 109.6(4) . . ? C2 C8 C10 114.1(4) . . ? C16 C8 C10 116.3(4) . . ? C2 C8 H8A 105.2 . . ? C16 C8 H8A 105.2 . . ? C10 C8 H8A 105.2 . . ? C39 C34 C35 115.3(5) . . ? C39 C34 N1 120.4(5) . . ? C35 C34 N1 124.3(5) . . ? C80 C79 C78 118.9(5) . . ? C80 C79 H79A 120.6 . . ? C78 C79 H79A 120.6 . . ? C69 C49 C44 110.3(4) . . ? C69 C49 C63 114.3(4) . . ? C44 C49 C63 112.5(4) . . ? C69 C49 H49A 106.4 . . ? C44 C49 H49A 106.4 . . ? C63 C49 H49A 106.4 . . ? C42 C48 C50 109.4(4) . . ? C42 C48 C57 114.9(4) . . ? C50 C48 C57 111.9(4) . . ? C42 C48 H48A 106.7 . . ? C50 C48 H48A 106.7 . . ? C57 C48 H48A 106.7 . . ? C44 C45 C46 121.3(4) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? C68 C63 C64 117.4(5) . . ? C68 C63 C49 121.2(5) . . ? C64 C63 C49 121.1(4) . . ? C23 C22 C27 118.2(5) . . ? C23 C22 C9 123.4(4) . . ? C27 C22 C9 118.4(5) . . ? C5 C4 C3 117.4(4) . . ? C5 C4 C9 123.8(4) . . ? C3 C4 C9 118.8(4) . . ? C56 C50 C51 118.1(5) . . ? C56 C50 C48 121.1(4) . . ? C51 C50 C48 120.8(4) . . ? F4 C80 C79 119.0(5) . . ? F4 C80 C75 117.4(4) . . ? C79 C80 C75 123.6(5) . . ? C42 C43 C44 124.2(5) . . ? C42 C43 H43A 117.9 . . ? C44 C43 H43A 117.9 . . ? C28 C9 C22 110.9(4) . . ? C28 C9 C4 113.4(4) . . ? C22 C9 C4 112.2(4) . . ? C28 C9 H9A 106.6 . . ? C22 C9 H9A 106.6 . . ? C4 C9 H9A 106.6 . . ? C29 C28 C33 118.6(5) . . ? C29 C28 C9 120.3(5) . . ? C33 C28 C9 121.1(4) . . ? C76 C77 C78 118.5(5) . . ? C76 C77 H77A 120.7 . . ? C78 C77 H77A 120.7 . . ? C43 C42 C41 118.8(4) . . ? C43 C42 C48 121.5(4) . . ? C41 C42 C48 119.4(4) . . ? C11 C10 C15 117.9(5) . . ? C11 C10 C8 121.8(5) . . ? C15 C10 C8 120.0(5) . . ? C65 C64 C63 121.1(5) . . ? C65 C64 H64A 119.4 . . ? C63 C64 H64A 119.4 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 120.4(4) . . ? C1 C6 C7 120.8(4) . . ? C5 C6 C7 118.6(4) . . ? C51 C52 C53 120.5(5) . . ? C51 C52 H52A 119.7 . . ? C53 C52 H52A 119.7 . . ? C45 C44 C43 117.0(4) . . ? C45 C44 C49 121.9(4) . . ? C43 C44 C49 121.0(4) . . ? C52 C51 C50 121.5(5) . . ? C52 C51 H51A 119.2 . . ? C50 C51 H51A 119.2 . . ? F3 C76 C77 119.3(5) . . ? F3 C76 C75 117.5(4) . . ? C77 C76 C75 123.2(5) . . ? F2 C39 C38 119.7(5) . . ? F2 C39 C34 117.2(5) . . ? C38 C39 C34 123.1(6) . . ? C74 C69 C70 117.7(6) . . ? C74 C69 C49 119.3(5) . . ? C70 C69 C49 122.8(5) . . ? N2 C47 C46 126.0(4) . 7_565 ? N2 C47 H47 117.0 . . ? C46 C47 H47 117.0 7_565 . ? C59 C58 C57 121.1(5) . . ? C59 C58 H58A 119.5 . . ? C57 C58 H58A 119.5 . . ? C32 C33 C28 120.9(5) . . ? C32 C33 H33A 119.5 . . ? C28 C33 H33A 119.5 . . ? C14 C15 C10 121.6(6) . . ? C14 C15 H15A 119.2 . . ? C10 C15 H15A 119.2 . . ? C52 C53 C55 118.9(5) . . ? C52 C53 H53A 120.5 . . ? C55 C53 H53A 120.5 . . ? C62 C57 C58 117.8(5) . . ? C62 C57 C48 122.5(4) . . ? C58 C57 C48 119.7(4) . . ? C77 C78 C79 120.2(5) . . ? C77 C78 H78A 119.9 . . ? C79 C78 H78A 119.9 . . ? C16 C17 C18 121.2(6) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C67 C68 C63 121.7(5) . . ? C67 C68 H68A 119.1 . . ? C63 C68 H68A 119.1 . . ? C16 C21 C20 120.4(6) . . ? C16 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? F1 C35 C36 119.4(5) . . ? F1 C35 C34 117.8(5) . . ? C36 C35 C34 122.8(6) . . ? C28 C29 C30 119.9(5) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C26 C27 C22 120.0(6) . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? C17 C16 C21 118.4(5) . . ? C17 C16 C8 124.5(5) . . ? C21 C16 C8 116.9(5) . . ? C60 C59 C58 120.9(5) . . ? C60 C59 H59A 119.5 . . ? C58 C59 H59A 119.5 . . ? C71 C70 C69 122.1(7) . . ? C71 C70 H70A 118.9 . . ? C69 C70 H70A 118.9 . . ? C66 C67 C68 120.4(5) . . ? C66 C67 H67A 119.8 . . ? C68 C67 H67A 119.8 . . ? C30 C31 C32 119.3(6) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C64 C65 C66 120.6(5) . . ? C64 C65 H65A 119.7 . . ? C66 C65 H65A 119.7 . . ? C67 C66 C65 118.7(6) . . ? C67 C66 H66A 120.6 . . ? C65 C66 H66A 120.6 . . ? C62 C61 C60 121.3(6) . . ? C62 C61 H61A 119.4 . . ? C60 C61 H61A 119.4 . . ? C72 C71 C70 119.1(8) . . ? C72 C71 H71A 120.5 . . ? C70 C71 H71A 120.5 . . ? C39 C38 C37 119.5(6) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.2 . . ? C59 C60 C61 118.3(6) . . ? C59 C60 H60A 120.8 . . ? C61 C60 H60A 120.8 . . ? C22 C23 C24 120.9(5) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C37 C36 C35 118.7(6) . . ? C37 C36 H36A 120.7 . . ? C35 C36 H36A 120.7 . . ? C61 C62 C57 120.6(5) . . ? C61 C62 H62A 119.7 . . ? C57 C62 H62A 119.7 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C36 C37 C38 120.6(6) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C53 C55 C56 120.3(5) . . ? C53 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C50 C56 C55 120.5(5) . . ? C50 C56 H56A 119.7 . . ? C55 C56 H56A 119.7 . . ? C12 C13 C14 119.0(6) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C31 C30 C29 121.1(5) . . ? C31 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C31 C32 C33 120.1(6) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C15 C14 C13 119.7(6) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C10 C11 C12 120.8(6) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C25 C26 C27 121.1(6) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C18 C19 C20 120.0(6) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C18 C17 120.3(7) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C13 C12 C11 120.8(6) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C72 C73 C74 118.9(8) . . ? C72 C73 H73A 120.5 . . ? C74 C73 H73A 120.5 . . ? C71 C72 C73 121.6(8) . . ? C71 C72 H72A 119.2 . . ? C73 C72 H72A 119.2 . . ? C69 C74 C73 120.5(8) . . ? C69 C74 H74A 119.7 . . ? C73 C74 H74A 119.7 . . ? C19 C20 C21 119.6(7) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? 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 O2 Ni2 O2 C41 8(64) 7_565 . . . ? N2 Ni2 O2 C41 -154.1(4) . . . . ? N2 Ni2 O2 C41 25.9(4) 7_565 . . . ? O1 Ni1 O1 C1 -56.1(4) 2 . . . ? N1 Ni1 O1 C1 -148.3(4) 2 . . . ? N1 Ni1 O1 C1 36.0(4) . . . . ? O2 Ni2 N2 C47 21.1(4) 7_565 . . . ? O2 Ni2 N2 C47 -158.9(4) . . . . ? N2 Ni2 N2 C47 53(100) 7_565 . . . ? O2 Ni2 N2 C75 -160.4(4) 7_565 . . . ? O2 Ni2 N2 C75 19.6(4) . . . . ? N2 Ni2 N2 C75 -129(100) 7_565 . . . ? O1 Ni1 N1 C7 146.4(4) 2 . . . ? O1 Ni1 N1 C7 -28.2(4) . . . . ? N1 Ni1 N1 C7 -120.9(4) 2 . . . ? O1 Ni1 N1 C34 -30.9(4) 2 . . . ? O1 Ni1 N1 C34 154.4(4) . . . . ? N1 Ni1 N1 C34 61.8(4) 2 . . . ? Ni1 O1 C1 C6 -25.4(6) . . . . ? Ni1 O1 C1 C2 156.4(3) . . . . ? O1 C1 C2 C3 -179.4(4) . . . . ? C6 C1 C2 C3 2.3(7) . . . . ? O1 C1 C2 C8 1.0(7) . . . . ? C6 C1 C2 C8 -177.3(4) . . . . ? C47 N2 C75 C80 -121.2(5) . . . . ? Ni2 N2 C75 C80 60.2(5) . . . . ? C47 N2 C75 C76 58.8(6) . . . . ? Ni2 N2 C75 C76 -119.8(4) . . . . ? Ni2 O2 C41 C46 -16.8(7) . . . . ? Ni2 O2 C41 C42 165.8(3) . . . . ? O2 C41 C46 C45 -179.4(4) . . . . ? C42 C41 C46 C45 -2.0(7) . . . . ? O2 C41 C46 C47 -5.6(7) . . . 7_565 ? C42 C41 C46 C47 171.8(4) . . . 7_565 ? C34 N1 C7 C6 -172.8(4) . . . . ? Ni1 N1 C7 C6 9.9(7) . . . . ? C1 C2 C3 C4 -0.9(7) . . . . ? C8 C2 C3 C4 178.7(4) . . . . ? C3 C2 C8 C16 -57.5(6) . . . . ? C1 C2 C8 C16 122.1(5) . . . . ? C3 C2 C8 C10 74.9(6) . . . . ? C1 C2 C8 C10 -105.4(5) . . . . ? C7 N1 C34 C39 128.5(5) . . . . ? Ni1 N1 C34 C39 -54.0(6) . . . . ? C7 N1 C34 C35 -54.3(7) . . . . ? Ni1 N1 C34 C35 123.2(5) . . . . ? C41 C46 C45 C44 -0.7(7) . . . . ? C47 C46 C45 C44 -174.7(5) 7_565 . . . ? C69 C49 C63 C68 33.8(6) . . . . ? C44 C49 C63 C68 160.6(5) . . . . ? C69 C49 C63 C64 -153.4(5) . . . . ? C44 C49 C63 C64 -26.5(6) . . . . ? C2 C3 C4 C5 -1.1(7) . . . . ? C2 C3 C4 C9 179.0(4) . . . . ? C42 C48 C50 C56 -118.3(5) . . . . ? C57 C48 C50 C56 113.2(5) . . . . ? C42 C48 C50 C51 60.4(6) . . . . ? C57 C48 C50 C51 -68.1(6) . . . . ? C78 C79 C80 F4 -178.8(4) . . . . ? C78 C79 C80 C75 1.1(8) . . . . ? C76 C75 C80 F4 177.8(4) . . . . ? N2 C75 C80 F4 -2.2(7) . . . . ? C76 C75 C80 C79 -2.1(7) . . . . ? N2 C75 C80 C79 177.9(4) . . . . ? C23 C22 C9 C28 113.8(5) . . . . ? C27 C22 C9 C28 -65.6(6) . . . . ? C23 C22 C9 C4 -14.1(7) . . . . ? C27 C22 C9 C4 166.5(5) . . . . ? C5 C4 C9 C28 -18.6(7) . . . . ? C3 C4 C9 C28 161.3(4) . . . . ? C5 C4 C9 C22 107.9(5) . . . . ? C3 C4 C9 C22 -72.2(5) . . . . ? C22 C9 C28 C29 129.5(5) . . . . ? C4 C9 C28 C29 -103.3(5) . . . . ? C22 C9 C28 C33 -50.6(6) . . . . ? C4 C9 C28 C33 76.7(6) . . . . ? C44 C43 C42 C41 -1.3(8) . . . . ? C44 C43 C42 C48 172.4(5) . . . . ? O2 C41 C42 C43 -179.5(4) . . . . ? C46 C41 C42 C43 2.9(7) . . . . ? O2 C41 C42 C48 6.7(7) . . . . ? C46 C41 C42 C48 -170.9(4) . . . . ? C50 C48 C42 C43 -83.8(6) . . . . ? C57 C48 C42 C43 43.0(6) . . . . ? C50 C48 C42 C41 89.9(5) . . . . ? C57 C48 C42 C41 -143.3(4) . . . . ? C2 C8 C10 C11 12.2(7) . . . . ? C16 C8 C10 C11 141.4(5) . . . . ? C2 C8 C10 C15 -174.5(4) . . . . ? C16 C8 C10 C15 -45.3(6) . . . . ? C68 C63 C64 C65 0.2(8) . . . . ? C49 C63 C64 C65 -172.9(5) . . . . ? C3 C4 C5 C6 1.7(7) . . . . ? C9 C4 C5 C6 -178.4(4) . . . . ? O1 C1 C6 C5 -179.9(4) . . . . ? C2 C1 C6 C5 -1.7(7) . . . . ? O1 C1 C6 C7 -5.1(7) . . . . ? C2 C1 C6 C7 173.1(4) . . . . ? C4 C5 C6 C1 -0.3(7) . . . . ? C4 C5 C6 C7 -175.3(4) . . . . ? N1 C7 C6 C1 12.6(7) . . . . ? N1 C7 C6 C5 -172.5(4) . . . . ? C46 C45 C44 C43 2.4(7) . . . . ? C46 C45 C44 C49 179.4(4) . . . . ? C42 C43 C44 C45 -1.4(8) . . . . ? C42 C43 C44 C49 -178.4(5) . . . . ? C69 C49 C44 C45 -109.4(5) . . . . ? C63 C49 C44 C45 121.6(5) . . . . ? C69 C49 C44 C43 67.5(6) . . . . ? C63 C49 C44 C43 -61.5(6) . . . . ? C53 C52 C51 C50 1.2(9) . . . . ? C56 C50 C51 C52 -1.7(8) . . . . ? C48 C50 C51 C52 179.6(5) . . . . ? C78 C77 C76 F3 179.9(5) . . . . ? C78 C77 C76 C75 -0.4(8) . . . . ? C80 C75 C76 F3 -178.6(4) . . . . ? N2 C75 C76 F3 1.4(7) . . . . ? C80 C75 C76 C77 1.7(7) . . . . ? N2 C75 C76 C77 -178.3(5) . . . . ? C35 C34 C39 F2 -179.0(5) . . . . ? N1 C34 C39 F2 -1.6(7) . . . . ? C35 C34 C39 C38 0.6(8) . . . . ? N1 C34 C39 C38 178.1(5) . . . . ? C44 C49 C69 C74 97.4(7) . . . . ? C63 C49 C69 C74 -134.6(7) . . . . ? C44 C49 C69 C70 -77.5(6) . . . . ? C63 C49 C69 C70 50.4(7) . . . . ? C75 N2 C47 C46 173.1(5) . . . 7_565 ? Ni2 N2 C47 C46 -8.3(7) . . . 7_565 ? C29 C28 C33 C32 1.5(8) . . . . ? C9 C28 C33 C32 -178.4(5) . . . . ? C11 C10 C15 C14 1.7(8) . . . . ? C8 C10 C15 C14 -171.9(5) . . . . ? C51 C52 C53 C55 0.1(9) . . . . ? C59 C58 C57 C62 -1.2(8) . . . . ? C59 C58 C57 C48 -178.0(5) . . . . ? C42 C48 C57 C62 25.4(7) . . . . ? C50 C48 C57 C62 151.0(5) . . . . ? C42 C48 C57 C58 -158.0(4) . . . . ? C50 C48 C57 C58 -32.4(6) . . . . ? C76 C77 C78 C79 -0.7(8) . . . . ? C80 C79 C78 C77 0.4(8) . . . . ? C64 C63 C68 C67 -0.5(8) . . . . ? C49 C63 C68 C67 172.7(5) . . . . ? C39 C34 C35 F1 178.2(5) . . . . ? N1 C34 C35 F1 0.8(8) . . . . ? C39 C34 C35 C36 -0.8(8) . . . . ? N1 C34 C35 C36 -178.1(5) . . . . ? C33 C28 C29 C30 -0.3(8) . . . . ? C9 C28 C29 C30 179.6(5) . . . . ? C23 C22 C27 C26 -2.9(9) . . . . ? C9 C22 C27 C26 176.5(5) . . . . ? C18 C17 C16 C21 -1.4(8) . . . . ? C18 C17 C16 C8 -176.6(5) . . . . ? C20 C21 C16 C17 -0.7(8) . . . . ? C20 C21 C16 C8 174.9(5) . . . . ? C2 C8 C16 C17 102.9(6) . . . . ? C10 C8 C16 C17 -28.5(7) . . . . ? C2 C8 C16 C21 -72.3(6) . . . . ? C10 C8 C16 C21 156.3(5) . . . . ? C57 C58 C59 C60 -0.2(9) . . . . ? C74 C69 C70 C71 -0.5(10) . . . . ? C49 C69 C70 C71 174.5(5) . . . . ? C63 C68 C67 C66 -0.3(9) . . . . ? C63 C64 C65 C66 0.8(9) . . . . ? C68 C67 C66 C65 1.3(9) . . . . ? C64 C65 C66 C67 -1.6(9) . . . . ? C69 C70 C71 C72 -0.9(11) . . . . ? F2 C39 C38 C37 -179.8(5) . . . . ? C34 C39 C38 C37 0.5(9) . . . . ? C58 C59 C60 C61 2.2(10) . . . . ? C62 C61 C60 C59 -2.7(11) . . . . ? C27 C22 C23 C24 1.6(9) . . . . ? C9 C22 C23 C24 -177.8(6) . . . . ? F1 C35 C36 C37 -179.1(5) . . . . ? C34 C35 C36 C37 -0.2(9) . . . . ? C60 C61 C62 C57 1.2(10) . . . . ? C58 C57 C62 C61 0.7(8) . . . . ? C48 C57 C62 C61 177.4(5) . . . . ? C22 C23 C24 C25 0.7(10) . . . . ? C35 C36 C37 C38 1.4(9) . . . . ? C39 C38 C37 C36 -1.6(10) . . . . ? C52 C53 C55 C56 -1.0(10) . . . . ? C51 C50 C56 C55 0.8(9) . . . . ? C48 C50 C56 C55 179.5(5) . . . . ? C53 C55 C56 C50 0.5(10) . . . . ? C32 C31 C30 C29 0.8(9) . . . . ? C28 C29 C30 C31 -0.8(9) . . . . ? C30 C31 C32 C33 0.4(9) . . . . ? C28 C33 C32 C31 -1.6(8) . . . . ? C10 C15 C14 C13 0.1(9) . . . . ? C12 C13 C14 C15 -1.4(10) . . . . ? C15 C10 C11 C12 -2.1(9) . . . . ? C8 C10 C11 C12 171.4(5) . . . . ? C22 C27 C26 C25 2.1(10) . . . . ? C20 C19 C18 C17 -2.0(10) . . . . ? C16 C17 C18 C19 2.8(9) . . . . ? C27 C26 C25 C24 0.3(10) . . . . ? C23 C24 C25 C26 -1.7(11) . . . . ? C14 C13 C12 C11 1.1(11) . . . . ? C10 C11 C12 C13 0.7(10) . . . . ? C70 C71 C72 C73 1.8(15) . . . . ? C74 C73 C72 C71 -1.3(19) . . . . ? C70 C69 C74 C73 1.0(14) . . . . ? C49 C69 C74 C73 -174.2(9) . . . . ? C72 C73 C74 C69 -0.1(19) . . . . ? C18 C19 C20 C21 -0.1(10) . . . . ? C16 C21 C20 C19 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.674 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.087 _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 0.179 0.250 257.0 73.5 2 0.500 -0.179 0.750 257.0 74.2 3 0.280 0.046 0.573 15.1 -1.2 4 0.720 0.046 0.927 15.1 -0.8 5 0.000 0.321 0.750 257.0 74.2 6 0.119 0.060 0.027 12.4 1.5 7 0.881 0.060 0.473 12.4 1.7 8 0.381 0.439 0.973 12.4 2.0 9 0.619 0.439 0.527 12.4 1.8 10 0.000 0.679 0.250 256.9 73.5 11 0.220 0.454 0.427 15.1 -1.0 12 0.780 0.454 0.073 15.1 -1.0 13 0.220 0.546 0.927 15.1 -0.8 14 0.780 0.546 0.573 15.1 -1.2 15 0.381 0.560 0.473 12.4 1.7 16 0.619 0.560 0.027 12.4 1.5 17 0.119 0.939 0.527 12.4 1.8 18 0.881 0.939 0.973 12.4 2.0 19 0.280 0.954 0.073 15.1 -1.0 20 0.720 0.954 0.427 15.1 -1.0 _platon_squeeze_details ; ? ; #==END