data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; nickel (0) nitrosyl iodide bipyridine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 I N3 Ni O' _chemical_formula_weight 371.80 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.9792(9) _cell_length_b 11.8611(8) _cell_length_c 7.7282(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.748(4) _cell_angle_gamma 90.00 _cell_volume 1181.73(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 4.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6466 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5461 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 30.57 _reflns_number_total 1883 _reflns_number_gt 1699 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0235P)^2^+0.3828P] 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 1883 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 I1 I 0.691827(13) 0.5000 0.67176(2) 0.01445(5) Uani 1 2 d S . . Ni Ni 0.80683(3) 0.5000 0.47562(5) 0.01552(8) Uani 1 2 d S . . N2 N 0.91643(13) 0.60917(13) 0.6259(2) 0.0156(3) Uani 1 1 d . . . N1 N 0.7242(2) 0.5000 0.2542(4) 0.0206(5) Uani 1 2 d S . . O1 O 0.6526(2) 0.5000 0.1147(3) 0.0328(5) Uani 1 2 d S . . C2 C 1.08434(16) 0.62743(16) 0.8751(3) 0.0168(3) Uani 1 1 d . . . H2 H 1.1441 0.5928 0.9655 0.020 Uiso 1 1 calc R . . C1 C 1.00318(14) 0.56235(15) 0.7547(2) 0.0137(3) Uani 1 1 d . . . C5 C 0.91036(16) 0.72206(17) 0.6139(3) 0.0201(4) Uani 1 1 d . . . H5 H 0.8499 0.7552 0.5231 0.024 Uiso 1 1 calc R . . C3 C 1.07644(16) 0.74424(16) 0.8607(3) 0.0201(4) Uani 1 1 d . . . H3 H 1.1310 0.7906 0.9411 0.024 Uiso 1 1 calc R . . C4 C 0.98826(17) 0.79239(17) 0.7280(3) 0.0216(4) Uani 1 1 d . . . H4 H 0.9814 0.8720 0.7156 0.026 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 I1 0.01303(8) 0.01606(8) 0.01524(8) 0.000 0.00654(6) 0.000 Ni 0.01367(17) 0.01904(16) 0.01452(16) 0.000 0.00619(13) 0.000 N2 0.0132(7) 0.0167(7) 0.0191(7) 0.0027(6) 0.0088(6) 0.0003(6) N1 0.0242(13) 0.0204(11) 0.0214(12) 0.000 0.0133(11) 0.000 O1 0.0358(14) 0.0412(14) 0.0185(10) 0.000 0.0074(10) 0.000 C2 0.0160(9) 0.0179(8) 0.0175(8) -0.0002(7) 0.0077(7) -0.0009(7) C1 0.0152(8) 0.0144(8) 0.0149(8) 0.0013(6) 0.0095(7) 0.0004(6) C5 0.0171(9) 0.0188(8) 0.0264(10) 0.0074(7) 0.0108(8) 0.0018(7) C3 0.0206(10) 0.0190(8) 0.0234(9) -0.0020(8) 0.0115(8) -0.0044(8) C4 0.0233(10) 0.0152(8) 0.0312(10) 0.0024(8) 0.0160(9) -0.0008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ni 2.6013(4) . ? Ni N1 1.653(3) . ? Ni N2 1.9992(17) . ? Ni N2 1.9992(17) 6_565 ? N2 C5 1.343(2) . ? N2 C1 1.355(2) . ? N1 O1 1.153(4) . ? C2 C1 1.390(3) . ? C2 C3 1.391(3) . ? C1 C1 1.479(4) 6_565 ? C5 C4 1.384(3) . ? C3 C4 1.386(3) . ? 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 Ni N2 132.30(6) . . ? N1 Ni N2 132.30(6) . 6_565 ? N2 Ni N2 80.74(9) . 6_565 ? N1 Ni I1 105.12(9) . . ? N2 Ni I1 99.74(5) . . ? N2 Ni I1 99.74(5) 6_565 . ? C5 N2 C1 118.29(17) . . ? C5 N2 Ni 126.31(14) . . ? C1 N2 Ni 115.37(12) . . ? O1 N1 Ni 167.0(2) . . ? C1 C2 C3 118.72(18) . . ? N2 C1 C2 122.08(17) . . ? N2 C1 C1 114.19(10) . 6_565 ? C2 C1 C1 123.73(11) . 6_565 ? N2 C5 C4 122.96(19) . . ? C4 C3 C2 119.35(19) . . ? C5 C4 C3 118.59(18) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.848 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.103 ############################END############################ data_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; nickel (0) nitrosyl bipyridine hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 F6 N3 Ni O P' _chemical_formula_weight 389.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 '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' _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 7.9403(3) _cell_length_b 10.4457(3) _cell_length_c 16.9595(6) _cell_angle_alpha 81.625(2) _cell_angle_beta 86.498(2) _cell_angle_gamma 77.562(2) _cell_volume 1358.35(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 3.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2013 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4976 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 62.87 _reflns_number_total 3382 _reflns_number_gt 3247 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1098P)^2^+0.5950P] 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 3382 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Ni2 Ni 0.63765(8) -0.09910(6) 0.66257(4) 0.0442(3) Uani 1 1 d . A 1 Ni1 Ni 0.23746(7) 0.21961(5) 0.06653(3) 0.0327(2) Uani 1 1 d . B 1 P2 P 0.33844(10) 0.93098(7) 0.84604(5) 0.0278(3) Uani 1 1 d . C 1 P1 P 0.20774(11) 0.61210(9) 0.61854(5) 0.0346(3) Uani 1 1 d . D 1 F11 F 0.2013(3) 1.06747(19) 0.84457(12) 0.0429(5) Uani 1 1 d . C 1 F9 F 0.3926(3) 0.9456(2) 0.93302(11) 0.0460(5) Uani 1 1 d . C 1 F10 F 0.1968(2) 0.85100(19) 0.88435(15) 0.0511(6) Uani 1 1 d . C 1 F12 F 0.4804(2) 0.79429(17) 0.84916(12) 0.0407(5) Uani 1 1 d . C 1 F7 F 0.2873(3) 0.9161(2) 0.75947(12) 0.0507(6) Uani 1 1 d . C 1 N6 N 0.4603(3) 0.0301(3) 0.60158(16) 0.0333(6) Uani 1 1 d . A 1 O2 O 0.6813(4) -0.3701(3) 0.7013(2) 0.0615(8) Uani 1 1 d . A 1 F1 F 0.2735(4) 0.4700(3) 0.66835(14) 0.0672(7) Uani 1 1 d . D 1 F4 F 0.1431(4) 0.7521(2) 0.56692(17) 0.0725(8) Uani 1 1 d . D 1 F8 F 0.4829(2) 1.00953(18) 0.80755(12) 0.0404(5) Uani 1 1 d . C 1 O1 O 0.1720(4) -0.0326(3) 0.1012(2) 0.0655(9) Uani 1 1 d . B 1 N2 N 0.6695(4) -0.2572(3) 0.68712(19) 0.0453(8) Uani 1 1 d . A 1 C19 C 0.2018(4) 0.1025(4) 0.5291(2) 0.0398(8) Uani 1 1 d . A 1 H19 H 0.1030 0.0825 0.5088 0.048 Uiso 1 1 calc R A 1 C5 C 0.2032(4) 0.4954(3) 0.03699(18) 0.0267(6) Uani 1 1 d . B 1 C18 C 0.2314(4) 0.2301(3) 0.5154(2) 0.0371(8) Uani 1 1 d . A 1 H18 H 0.1526 0.2990 0.4857 0.045 Uiso 1 1 calc R A 1 C8 C 0.4495(4) 0.4624(4) -0.1592(2) 0.0388(8) Uani 1 1 d . B 1 H8 H 0.4855 0.5144 -0.2053 0.047 Uiso 1 1 calc R B 1 C15 C 0.6477(4) 0.1696(3) 0.62449(18) 0.0333(7) Uani 1 1 d . A 1 F3A F 0.1736(14) 0.5520(7) 0.5423(3) 0.072(3) Uani 0.597(17) 1 d P D 1 C17 C 0.3767(4) 0.2558(3) 0.54556(19) 0.0352(7) Uani 1 1 d . . . H17 H 0.3991 0.3426 0.5364 0.042 Uiso 1 1 calc R A 1 C1 C 0.0592(4) 0.4384(4) 0.1558(2) 0.0374(8) Uani 1 1 d . B . H1 H 0.0259 0.3721 0.1943 0.045 Uiso 1 1 calc R . . F6A F 0.2275(16) 0.6643(8) 0.6979(5) 0.086(3) Uani 0.597(17) 1 d P D 1 N4 N 0.3434(3) 0.3106(2) -0.02670(15) 0.0273(6) Uani 1 1 d . . . C7 C 0.3594(4) 0.5221(3) -0.09736(19) 0.0330(7) Uani 1 1 d . . . H7 H 0.3341 0.6157 -0.1001 0.040 Uiso 1 1 calc R B 1 F2A F 0.0183(8) 0.5956(9) 0.6502(5) 0.070(2) Uani 0.597(17) 1 d P D 1 N3 N 0.1565(3) 0.4019(3) 0.09206(15) 0.0297(6) Uani 1 1 d . . . N1 N 0.1974(3) 0.0731(3) 0.08924(19) 0.0404(7) Uani 1 1 d . . . F5A F 0.3897(8) 0.6236(19) 0.5880(7) 0.126(5) Uani 0.597(17) 1 d P D 1 N5 N 0.7435(4) 0.0554(3) 0.66088(16) 0.0370(7) Uani 1 1 d . . . C10 C 0.4337(4) 0.2539(3) -0.08600(19) 0.0333(7) Uani 1 1 d . B . H10 H 0.4624 0.1601 -0.0814 0.040 Uiso 1 1 calc R . . C3 C 0.0543(4) 0.6648(3) 0.1116(2) 0.0407(8) Uani 1 1 d . B . H3 H 0.0191 0.7555 0.1184 0.049 Uiso 1 1 calc R . . C20 C 0.3195(5) 0.0050(3) 0.5728(2) 0.0394(8) Uani 1 1 d . . . H20 H 0.2996 -0.0825 0.5828 0.047 Uiso 1 1 calc R A 1 C4 C 0.1546(4) 0.6289(3) 0.0455(2) 0.0345(7) Uani 1 1 d . . . H4 H 0.1894 0.6942 0.0067 0.041 Uiso 1 1 calc R B 1 C2 C 0.0059(4) 0.5697(4) 0.1671(2) 0.0388(8) Uani 1 1 d . . . H2 H -0.0631 0.5934 0.2126 0.047 Uiso 1 1 calc R B . C6 C 0.3067(4) 0.4446(3) -0.03164(18) 0.0274(6) Uani 1 1 d . B . C9 C 0.4865(4) 0.3261(4) -0.1533(2) 0.0390(8) Uani 1 1 d . . . H9 H 0.5476 0.2830 -0.1953 0.047 Uiso 1 1 calc R B 1 C16 C 0.4889(4) 0.1546(3) 0.58900(18) 0.0304(7) Uani 1 1 d . A . C12 C 0.9506(5) 0.1756(4) 0.6919(2) 0.0486(9) Uani 1 1 d . . . H12 H 1.0562 0.1755 0.7154 0.058 Uiso 1 1 calc R A . C11 C 0.8925(5) 0.0591(4) 0.6939(2) 0.0464(9) Uani 1 1 d . A . H11 H 0.9600 -0.0209 0.7193 0.056 Uiso 1 1 calc R . . C14 C 0.6989(4) 0.2887(3) 0.62169(19) 0.0364(7) Uani 1 1 d . . . H14 H 0.6293 0.3682 0.5968 0.044 Uiso 1 1 calc R A 1 C13 C 0.8523(5) 0.2911(4) 0.6554(2) 0.0452(9) Uani 1 1 d . A . H13 H 0.8893 0.3722 0.6534 0.054 Uiso 1 1 calc R . . F2B F 0.116(3) 0.5416(13) 0.5662(13) 0.123(7) Uani 0.403(17) 1 d P D 1 F3B F 0.3790(17) 0.5702(7) 0.5660(8) 0.078(4) Uani 0.403(17) 1 d P D 1 F5B F 0.311(3) 0.6867(11) 0.6675(13) 0.103(7) Uani 0.403(17) 1 d P D 1 F6B F 0.046(2) 0.659(2) 0.6666(11) 0.127(8) Uani 0.403(17) 1 d P D 1 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 0.0384(4) 0.0317(4) 0.0517(4) 0.0107(3) -0.0019(3) 0.0057(3) Ni1 0.0349(4) 0.0217(4) 0.0382(4) 0.0019(3) -0.0024(3) -0.0023(3) P2 0.0276(4) 0.0205(4) 0.0310(5) -0.0012(3) -0.0019(4) 0.0033(4) P1 0.0297(5) 0.0376(5) 0.0332(5) 0.0015(4) -0.0073(4) -0.0021(4) F11 0.0409(10) 0.0283(10) 0.0491(11) -0.0024(9) -0.0021(10) 0.0138(9) F9 0.0570(12) 0.0432(12) 0.0318(10) -0.0040(9) -0.0092(10) 0.0042(10) F10 0.0330(10) 0.0338(11) 0.0788(15) 0.0069(11) 0.0064(11) -0.0021(9) F12 0.0333(10) 0.0234(10) 0.0593(12) -0.0049(9) 0.0023(10) 0.0059(8) F7 0.0570(12) 0.0508(13) 0.0440(11) -0.0160(10) -0.0153(11) -0.0001(11) N6 0.0302(13) 0.0303(15) 0.0341(14) 0.0001(12) -0.0003(12) 0.0019(12) O2 0.0480(16) 0.0368(17) 0.089(2) 0.0189(15) -0.0090(16) -0.0011(13) F1 0.0841(18) 0.0519(15) 0.0493(13) 0.0141(11) -0.0187(13) 0.0124(13) F4 0.094(2) 0.0345(13) 0.0892(18) 0.0113(12) -0.0493(16) -0.0139(13) F8 0.0408(10) 0.0298(10) 0.0479(11) -0.0007(9) 0.0014(10) -0.0055(9) O1 0.0551(16) 0.0259(14) 0.112(3) -0.0002(15) 0.0170(18) -0.0124(12) N2 0.0353(15) 0.0381(19) 0.0507(18) 0.0127(15) -0.0003(15) 0.0056(13) C19 0.0310(16) 0.044(2) 0.0433(18) -0.0105(16) -0.0020(16) -0.0022(16) C5 0.0241(14) 0.0243(15) 0.0295(15) -0.0042(13) -0.0124(14) 0.0031(13) C18 0.0315(16) 0.0396(19) 0.0357(17) -0.0042(15) -0.0070(15) 0.0033(15) C8 0.0385(17) 0.045(2) 0.0318(16) 0.0024(15) -0.0058(16) -0.0109(17) C15 0.0320(16) 0.0390(19) 0.0227(14) -0.0017(14) 0.0012(14) 0.0038(15) F3A 0.131(7) 0.042(4) 0.028(2) -0.012(2) -0.018(3) 0.025(4) C17 0.0386(17) 0.0307(17) 0.0325(16) -0.0023(14) -0.0038(16) 0.0005(15) C1 0.0314(17) 0.045(2) 0.0336(16) -0.0048(15) -0.0078(15) -0.0019(16) F6A 0.144(8) 0.055(4) 0.070(4) -0.016(3) -0.049(4) -0.028(4) N4 0.0278(12) 0.0214(13) 0.0307(13) -0.0026(11) -0.0083(12) 0.0007(11) C7 0.0315(15) 0.0253(16) 0.0402(17) 0.0010(14) -0.0098(15) -0.0029(13) F2A 0.035(2) 0.083(5) 0.082(4) 0.014(4) 0.000(3) -0.011(3) N3 0.0273(12) 0.0297(14) 0.0289(13) -0.0029(11) -0.0078(12) 0.0023(11) N1 0.0293(13) 0.0317(17) 0.0551(18) -0.0004(14) -0.0002(14) 0.0006(12) F5A 0.028(3) 0.212(12) 0.116(8) 0.073(8) -0.014(4) -0.035(5) N5 0.0324(13) 0.0405(16) 0.0294(13) 0.0061(13) -0.0030(12) 0.0048(13) C10 0.0329(15) 0.0290(17) 0.0380(17) -0.0100(14) -0.0056(15) -0.0012(14) C3 0.0344(17) 0.0301(18) 0.057(2) -0.0182(17) -0.0148(18) 0.0068(14) C20 0.0417(18) 0.0325(18) 0.0421(17) -0.0051(15) 0.0038(17) -0.0052(16) C4 0.0339(16) 0.0243(16) 0.0434(18) -0.0040(14) -0.0111(16) 0.0002(14) C2 0.0315(16) 0.046(2) 0.0382(17) -0.0184(16) -0.0076(16) 0.0043(15) C6 0.0266(14) 0.0244(15) 0.0301(15) -0.0022(12) -0.0124(14) -0.0010(13) C9 0.0362(17) 0.045(2) 0.0345(16) -0.0088(15) -0.0029(16) -0.0034(16) C16 0.0298(15) 0.0307(17) 0.0250(14) -0.0022(13) 0.0016(14) 0.0048(14) C12 0.0394(19) 0.070(3) 0.0358(18) -0.0104(18) -0.0095(17) -0.005(2) C11 0.0336(17) 0.059(2) 0.0355(18) 0.0063(17) -0.0055(16) 0.0085(18) C14 0.0399(17) 0.0363(18) 0.0298(15) -0.0024(14) -0.0066(15) -0.0006(15) C13 0.046(2) 0.051(2) 0.0396(18) -0.0110(17) -0.0037(18) -0.0103(19) F2B 0.149(12) 0.070(7) 0.168(15) 0.052(8) -0.137(11) -0.068(8) F3B 0.100(9) 0.024(4) 0.085(7) 0.002(3) 0.055(7) 0.020(4) F5B 0.140(13) 0.037(5) 0.141(13) 0.001(6) -0.116(11) -0.015(6) F6B 0.094(10) 0.115(12) 0.117(11) 0.039(9) 0.073(9) 0.040(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 Ni2 N2 1.611(3) . ? Ni2 N6 1.956(3) . ? Ni2 N5 1.970(3) . ? Ni1 N1 1.617(3) . ? Ni1 N4 1.963(2) . ? Ni1 N3 1.976(3) . ? P2 F7 1.585(2) . ? P2 F10 1.5946(19) . ? P2 F11 1.5949(19) . ? P2 F9 1.599(2) . ? P2 F8 1.6038(19) . ? P2 F12 1.6137(18) . ? P1 F6B 1.507(10) . ? P1 F5A 1.528(6) . ? P1 F2B 1.535(12) . ? P1 F6A 1.553(7) . ? P1 F3A 1.579(6) . ? P1 F5B 1.585(10) . ? P1 F4 1.590(3) . ? P1 F3B 1.595(10) . ? P1 F1 1.595(2) . ? P1 F2A 1.602(6) . ? N6 C20 1.336(5) . ? N6 C16 1.353(4) . ? O2 N2 1.153(4) . ? O1 N1 1.152(4) . ? C19 C20 1.385(5) . ? C19 C18 1.386(5) . ? C5 N3 1.346(4) . ? C5 C4 1.391(4) . ? C5 C6 1.479(4) . ? C18 C17 1.382(5) . ? C8 C9 1.381(5) . ? C8 C7 1.382(5) . ? C15 N5 1.355(5) . ? C15 C14 1.382(5) . ? C15 C16 1.477(5) . ? F3A F2B 0.61(2) . ? F3A F3B 1.759(16) . ? C17 C16 1.379(5) . ? C1 N3 1.342(4) . ? C1 C2 1.383(5) . ? F6A F5B 0.864(19) . ? F6A F6B 1.58(2) . ? N4 C10 1.333(4) . ? N4 C6 1.358(4) . ? C7 C6 1.378(4) . ? F2A F6B 0.83(3) . ? F2A F2B 1.69(2) . ? F5A F3B 0.735(18) . ? F5A F5B 1.620(19) . ? N5 C11 1.350(5) . ? C10 C9 1.369(5) . ? C3 C2 1.366(5) . ? C3 C4 1.385(5) . ? C12 C13 1.372(6) . ? C12 C11 1.387(6) . ? C14 C13 1.384(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni2 N6 133.30(14) . . ? N2 Ni2 N5 143.45(14) . . ? N6 Ni2 N5 82.85(11) . . ? N1 Ni1 N4 134.29(13) . . ? N1 Ni1 N3 140.75(13) . . ? N4 Ni1 N3 82.55(10) . . ? F7 P2 F10 90.18(13) . . ? F7 P2 F11 90.84(12) . . ? F10 P2 F11 90.79(11) . . ? F7 P2 F9 179.26(13) . . ? F10 P2 F9 90.36(12) . . ? F11 P2 F9 89.65(11) . . ? F7 P2 F8 89.82(12) . . ? F10 P2 F8 179.20(11) . . ? F11 P2 F8 90.01(11) . . ? F9 P2 F8 89.63(11) . . ? F7 P2 F12 90.55(11) . . ? F10 P2 F12 89.95(10) . . ? F11 P2 F12 178.42(12) . . ? F9 P2 F12 88.95(11) . . ? F8 P2 F12 89.25(10) . . ? F6B P1 F5A 150.6(9) . . ? F6B P1 F2B 93.6(10) . . ? F5A P1 F2B 113.7(8) . . ? F6B P1 F6A 62.1(10) . . ? F5A P1 F6A 93.3(6) . . ? F2B P1 F6A 151.9(8) . . ? F6B P1 F3A 113.6(11) . . ? F5A P1 F3A 91.9(6) . . ? F2B P1 F3A 22.5(8) . . ? F6A P1 F3A 174.3(4) . . ? F6B P1 F5B 89.7(10) . . ? F5A P1 F5B 62.7(7) . . ? F2B P1 F5B 176.1(9) . . ? F6A P1 F5B 32.0(7) . . ? F3A P1 F5B 153.7(9) . . ? F6B P1 F4 81.3(5) . . ? F5A P1 F4 86.6(5) . . ? F2B P1 F4 92.4(5) . . ? F6A P1 F4 97.1(3) . . ? F3A P1 F4 85.5(3) . . ? F5B P1 F4 86.1(4) . . ? F6B P1 F3B 176.9(9) . . ? F5A P1 F3B 27.1(7) . . ? F2B P1 F3B 87.8(9) . . ? F6A P1 F3B 117.2(6) . . ? F3A P1 F3B 67.3(6) . . ? F5B P1 F3B 88.8(8) . . ? F4 P1 F3B 95.9(4) . . ? F6B P1 F1 99.7(6) . . ? F5A P1 F1 92.9(5) . . ? F2B P1 F1 86.5(5) . . ? F6A P1 F1 84.2(3) . . ? F3A P1 F1 93.2(3) . . ? F5B P1 F1 94.9(4) . . ? F4 P1 F1 178.59(16) . . ? F3B P1 F1 83.1(4) . . ? F6B P1 F2A 30.9(10) . . ? F5A P1 F2A 178.3(7) . . ? F2B P1 F2A 65.2(9) . . ? F6A P1 F2A 87.7(5) . . ? F3A P1 F2A 87.1(4) . . ? F5B P1 F2A 118.5(9) . . ? F4 P1 F2A 94.6(3) . . ? F3B P1 F2A 151.4(5) . . ? F1 P1 F2A 85.8(3) . . ? C20 N6 C16 119.6(3) . . ? C20 N6 Ni2 126.0(2) . . ? C16 N6 Ni2 114.4(2) . . ? O2 N2 Ni2 174.7(3) . . ? C20 C19 C18 118.5(3) . . ? N3 C5 C4 121.3(3) . . ? N3 C5 C6 114.8(3) . . ? C4 C5 C6 123.9(3) . . ? C17 C18 C19 119.3(3) . . ? C9 C8 C7 119.1(3) . . ? N5 C15 C14 121.3(3) . . ? N5 C15 C16 114.5(3) . . ? C14 C15 C16 124.2(3) . . ? F2B F3A P1 74.8(16) . . ? F2B F3A F3B 125.6(18) . . ? P1 F3A F3B 56.8(4) . . ? C16 C17 C18 119.5(3) . . ? N3 C1 C2 122.0(3) . . ? F5B F6A P1 76.1(11) . . ? F5B F6A F6B 123.9(13) . . ? P1 F6A F6B 57.5(6) . . ? C10 N4 C6 119.2(3) . . ? C10 N4 Ni1 126.2(2) . . ? C6 N4 Ni1 114.4(2) . . ? C6 C7 C8 119.4(3) . . ? F6B F2A P1 68.2(10) . . ? F6B F2A F2B 118.9(13) . . ? P1 F2A F2B 55.5(5) . . ? C1 N3 C5 119.3(3) . . ? C1 N3 Ni1 126.6(2) . . ? C5 N3 Ni1 114.0(2) . . ? O1 N1 Ni1 176.2(3) . . ? F3B F5A P1 81.5(12) . . ? F3B F5A F5B 138.4(17) . . ? P1 F5A F5B 60.4(5) . . ? C11 N5 C15 118.7(3) . . ? C11 N5 Ni2 127.5(3) . . ? C15 N5 Ni2 113.8(2) . . ? N4 C10 C9 122.4(3) . . ? C2 C3 C4 120.0(3) . . ? N6 C20 C19 122.0(3) . . ? C3 C4 C5 118.6(3) . . ? C3 C2 C1 118.8(3) . . ? N4 C6 C7 120.9(3) . . ? N4 C6 C5 114.1(3) . . ? C7 C6 C5 125.0(3) . . ? C10 C9 C8 119.0(3) . . ? N6 C16 C17 121.0(3) . . ? N6 C16 C15 114.4(3) . . ? C17 C16 C15 124.6(3) . . ? C13 C12 C11 118.7(4) . . ? N5 C11 C12 122.3(4) . . ? C15 C14 C13 119.5(3) . . ? C12 C13 C14 119.6(4) . . ? F3A F2B P1 82.7(15) . . ? F3A F2B F2A 140(2) . . ? P1 F2B F2A 59.3(7) . . ? F5A F3B P1 71.4(11) . . ? F5A F3B F3A 121.5(15) . . ? P1 F3B F3A 55.9(4) . . ? F6A F5B P1 72.0(10) . . ? F6A F5B F5A 126.0(14) . . ? P1 F5B F5A 56.9(5) . . ? F2A F6B P1 80.9(13) . . ? F2A F6B F6A 127.2(14) . . ? P1 F6B F6A 60.4(6) . . ? _diffrn_measured_fraction_theta_max 0.772 _diffrn_reflns_theta_full 62.87 _diffrn_measured_fraction_theta_full 0.772 _refine_diff_density_max 0.602 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.094 ############################END############################ data_complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cl4 F12 N6 Ni2 O2 P2 S2' _chemical_formula_weight 1167.92 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 10.1213(3) _cell_length_b 10.6254(3) _cell_length_c 12.2737(3) _cell_angle_alpha 75.043(2) _cell_angle_beta 66.164(2) _cell_angle_gamma 67.598(2) _cell_volume 1107.76(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7741 _exptl_absorpt_correction_T_max 0.9606 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10462 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4533 _reflns_number_gt 3790 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0663P)^2^+2.6405P] 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 4533 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 0.19456(5) 0.23353(4) 0.47260(4) 0.01306(14) Uani 1 1 d . . . S1 S 0.11866(9) 0.47003(9) 0.44985(7) 0.01316(19) Uani 1 1 d . . . P1 P 0.12765(10) 0.07682(9) 0.15239(8) 0.0150(2) Uani 1 1 d . . . F1 F 0.0202(3) -0.0137(2) 0.2384(2) 0.0219(5) Uani 1 1 d . . . F2 F 0.0910(3) 0.0658(2) 0.0403(2) 0.0243(5) Uani 1 1 d . . . F3 F -0.0173(2) 0.2141(2) 0.1801(2) 0.0214(5) Uani 1 1 d . . . F4 F 0.2706(3) -0.0597(2) 0.1260(2) 0.0255(5) Uani 1 1 d . . . F5 F 0.2330(3) 0.1690(3) 0.0665(2) 0.0272(5) Uani 1 1 d . . . F6 F 0.1634(3) 0.0881(2) 0.26437(19) 0.0225(5) Uani 1 1 d . . . O1 O -0.0606(3) 0.1598(3) 0.5174(3) 0.0301(7) Uani 1 1 d . . . N1 N 0.3962(3) 0.2080(3) 0.3399(3) 0.0151(6) Uani 1 1 d . . . N2 N 0.3250(3) 0.1979(3) 0.5706(3) 0.0157(6) Uani 1 1 d . . . N3 N 0.0536(4) 0.1753(3) 0.4990(3) 0.0171(6) Uani 1 1 d . . . C1 C 0.4233(4) 0.2119(4) 0.2225(3) 0.0182(7) Uani 1 1 d . . . H1 H 0.3412 0.2350 0.1970 0.022 Uiso 1 1 calc R . . C2 C 0.5674(4) 0.1833(4) 0.1388(3) 0.0208(8) Uani 1 1 d . . . H2 H 0.5823 0.1870 0.0583 0.025 Uiso 1 1 calc R . . C3 C 0.6904(4) 0.1489(4) 0.1764(3) 0.0215(8) Uani 1 1 d . . . H3 H 0.7891 0.1282 0.1215 0.026 Uiso 1 1 calc R . . C4 C 0.6644(4) 0.1455(4) 0.2973(3) 0.0194(7) Uani 1 1 d . . . H4 H 0.7451 0.1232 0.3243 0.023 Uiso 1 1 calc R . . C5 C 0.5160(4) 0.1760(3) 0.3766(3) 0.0156(7) Uani 1 1 d . . . C6 C 0.4751(4) 0.1729(4) 0.5075(3) 0.0165(7) Uani 1 1 d . . . C7 C 0.5795(4) 0.1459(4) 0.5632(4) 0.0217(8) Uani 1 1 d . . . H7 H 0.6822 0.1304 0.5184 0.026 Uiso 1 1 calc R . . C8 C 0.5285(5) 0.1422(4) 0.6875(4) 0.0239(8) Uani 1 1 d . . . H8 H 0.5969 0.1238 0.7266 0.029 Uiso 1 1 calc R . . C9 C 0.3755(5) 0.1662(4) 0.7518(3) 0.0217(8) Uani 1 1 d . . . H9 H 0.3392 0.1631 0.8349 0.026 Uiso 1 1 calc R . . C10 C 0.2773(4) 0.1949(4) 0.6901(3) 0.0197(8) Uani 1 1 d . . . H10 H 0.1738 0.2128 0.7333 0.024 Uiso 1 1 calc R . . C11 C 0.1053(4) 0.5292(4) 0.3040(3) 0.0136(7) Uani 1 1 d . . . C12 C 0.0658(4) 0.4550(4) 0.2497(3) 0.0191(7) Uani 1 1 d . . . H12 H 0.0450 0.3738 0.2895 0.023 Uiso 1 1 calc R . . C13 C 0.0583(5) 0.5046(4) 0.1355(3) 0.0237(8) Uani 1 1 d . . . H13 H 0.0335 0.4558 0.0978 0.028 Uiso 1 1 calc R . . C14 C 0.0876(5) 0.6264(4) 0.0773(3) 0.0216(8) Uani 1 1 d . . . H14 H 0.0808 0.6594 0.0011 0.026 Uiso 1 1 calc R . . C15 C 0.1269(4) 0.6994(4) 0.1315(3) 0.0196(8) Uani 1 1 d . . . H15 H 0.1467 0.7810 0.0918 0.024 Uiso 1 1 calc R . . C16 C 0.1367(4) 0.6503(4) 0.2457(3) 0.0161(7) Uani 1 1 d . . . H16 H 0.1640 0.6983 0.2823 0.019 Uiso 1 1 calc R . . C17 C 0.6795(7) 0.4901(6) 0.2265(5) 0.0480(13) Uani 1 1 d . . . H17A H 0.7261 0.5614 0.1831 0.058 Uiso 1 1 calc R . . H17B H 0.7438 0.4067 0.1898 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.6703(2) 0.46210(17) 0.37765(15) 0.0637(4) Uani 1 1 d . . . Cl2 Cl 0.5038(2) 0.53731(18) 0.2132(2) 0.0845(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0118(2) 0.0158(2) 0.0108(2) -0.00122(16) -0.00387(17) -0.00375(17) S1 0.0132(4) 0.0158(4) 0.0107(4) -0.0007(3) -0.0052(3) -0.0041(3) P1 0.0147(4) 0.0183(4) 0.0133(4) -0.0037(3) -0.0058(3) -0.0042(4) F1 0.0214(11) 0.0189(11) 0.0255(12) -0.0008(9) -0.0071(9) -0.0084(9) F2 0.0293(12) 0.0289(12) 0.0217(11) -0.0075(9) -0.0154(10) -0.0063(10) F3 0.0211(11) 0.0163(10) 0.0252(11) -0.0032(9) -0.0092(9) -0.0023(9) F4 0.0176(11) 0.0296(12) 0.0271(12) -0.0137(10) -0.0090(9) 0.0031(9) F5 0.0278(13) 0.0371(13) 0.0202(11) -0.0035(10) -0.0035(10) -0.0189(11) F6 0.0236(12) 0.0296(12) 0.0180(11) -0.0077(9) -0.0105(9) -0.0055(9) O1 0.0260(16) 0.0426(18) 0.0295(16) -0.0035(13) -0.0090(13) -0.0200(14) N1 0.0141(14) 0.0179(15) 0.0127(14) -0.0025(11) -0.0035(12) -0.0052(12) N2 0.0168(15) 0.0152(14) 0.0133(14) -0.0016(11) -0.0060(12) -0.0023(12) N3 0.0182(16) 0.0190(15) 0.0139(14) -0.0017(12) -0.0049(12) -0.0065(12) C1 0.0219(19) 0.0208(18) 0.0147(17) -0.0015(14) -0.0073(15) -0.0090(15) C2 0.0219(19) 0.0246(19) 0.0148(17) -0.0049(14) -0.0013(15) -0.0099(16) C3 0.0179(18) 0.0226(19) 0.0199(18) -0.0049(15) 0.0008(15) -0.0084(15) C4 0.0164(18) 0.0175(17) 0.0231(19) -0.0032(14) -0.0066(15) -0.0039(14) C5 0.0166(17) 0.0131(16) 0.0170(17) -0.0033(13) -0.0061(14) -0.0033(13) C6 0.0170(17) 0.0144(16) 0.0185(18) -0.0021(13) -0.0084(14) -0.0028(14) C7 0.0163(18) 0.0225(19) 0.0240(19) -0.0037(15) -0.0081(16) -0.0019(15) C8 0.031(2) 0.0199(19) 0.026(2) -0.0022(15) -0.0205(17) -0.0015(16) C9 0.030(2) 0.0200(18) 0.0155(17) -0.0009(14) -0.0119(16) -0.0054(16) C10 0.0202(19) 0.0201(18) 0.0165(17) -0.0011(14) -0.0059(15) -0.0050(15) C11 0.0129(16) 0.0158(16) 0.0107(15) -0.0024(13) -0.0040(13) -0.0026(13) C12 0.025(2) 0.0182(17) 0.0172(18) 0.0016(14) -0.0107(15) -0.0095(15) C13 0.035(2) 0.024(2) 0.0197(19) -0.0007(15) -0.0157(17) -0.0126(17) C14 0.032(2) 0.0220(19) 0.0103(16) 0.0029(14) -0.0104(15) -0.0083(16) C15 0.0245(19) 0.0178(17) 0.0135(17) 0.0015(14) -0.0027(15) -0.0096(15) C16 0.0134(17) 0.0212(18) 0.0128(16) -0.0042(14) -0.0023(13) -0.0055(14) C17 0.048(3) 0.036(3) 0.058(3) -0.013(2) -0.012(3) -0.014(2) Cl1 0.0751(11) 0.0536(9) 0.0537(9) -0.0127(7) -0.0040(8) -0.0267(8) Cl2 0.0497(9) 0.0549(9) 0.166(2) -0.0339(11) -0.0532(12) -0.0034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 1.648(3) . ? Ni1 N2 2.000(3) . ? Ni1 N1 2.002(3) . ? Ni1 S1 2.3071(9) . ? S1 C11 1.780(3) . ? S1 S1 2.1306(17) 2_566 ? P1 F6 1.598(2) . ? P1 F5 1.601(2) . ? P1 F4 1.602(2) . ? P1 F2 1.603(2) . ? P1 F1 1.602(2) . ? P1 F3 1.618(2) . ? O1 N3 1.153(4) . ? N1 C1 1.346(5) . ? N1 C5 1.356(5) . ? N2 C10 1.342(5) . ? N2 C6 1.352(5) . ? C1 C2 1.374(5) . ? C1 H1 0.9300 . ? C2 C3 1.389(6) . ? C2 H2 0.9300 . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 C5 1.385(5) . ? C4 H4 0.9300 . ? C5 C6 1.482(5) . ? C6 C7 1.385(5) . ? C7 C8 1.393(6) . ? C7 H7 0.9300 . ? C8 C9 1.379(6) . ? C8 H8 0.9300 . ? C9 C10 1.383(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.386(5) . ? C11 C12 1.397(5) . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 C14 1.384(6) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 H14 0.9300 . ? C15 C16 1.393(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 Cl2 1.719(6) . ? C17 Cl1 1.771(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 N2 129.76(14) . . ? N3 Ni1 N1 130.90(14) . . ? N2 Ni1 N1 81.31(12) . . ? N3 Ni1 S1 111.90(11) . . ? N2 Ni1 S1 97.99(9) . . ? N1 Ni1 S1 96.50(9) . . ? C11 S1 S1 97.75(12) . 2_566 ? C11 S1 Ni1 107.50(12) . . ? S1 S1 Ni1 104.81(6) 2_566 . ? F6 P1 F5 90.20(13) . . ? F6 P1 F4 89.98(12) . . ? F5 P1 F4 90.68(13) . . ? F6 P1 F2 179.76(14) . . ? F5 P1 F2 89.93(13) . . ? F4 P1 F2 90.22(12) . . ? F6 P1 F1 89.95(12) . . ? F5 P1 F1 179.22(14) . . ? F4 P1 F1 90.09(13) . . ? F2 P1 F1 89.92(13) . . ? F6 P1 F3 89.82(12) . . ? F5 P1 F3 89.73(13) . . ? F4 P1 F3 179.55(15) . . ? F2 P1 F3 89.98(12) . . ? F1 P1 F3 89.50(12) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 Ni1 126.8(3) . . ? C5 N1 Ni1 114.6(2) . . ? C10 N2 C6 118.8(3) . . ? C10 N2 Ni1 126.2(3) . . ? C6 N2 Ni1 114.9(2) . . ? O1 N3 Ni1 167.4(3) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.9(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 123.4(3) . . ? N2 C6 C7 121.5(3) . . ? N2 C6 C5 114.5(3) . . ? C7 C6 C5 124.1(3) . . ? C6 C7 C8 119.1(4) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 122.7(4) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C16 C11 C12 121.2(3) . . ? C16 C11 S1 117.9(3) . . ? C12 C11 S1 120.9(3) . . ? C13 C12 C11 118.7(3) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 120.5(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 119.2(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? Cl2 C17 Cl1 112.8(3) . . ? Cl2 C17 H17A 109.0 . . ? Cl1 C17 H17A 109.0 . . ? Cl2 C17 H17B 109.0 . . ? Cl1 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.164 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.108 ############################END############################ data_complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2-bipyridine TEMPO nickel(II) hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.50 H27 Cl F6 N3 Ni O P' _chemical_formula_weight 558.57 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 21.240(7) _cell_length_b 9.737(3) _cell_length_c 22.745(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.718(6) _cell_angle_gamma 90.00 _cell_volume 4703(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6885 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33969 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4815 _reflns_number_gt 3972 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0174P)^2^+8.0486P] 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 4815 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.235592(11) 0.89463(2) 0.135879(10) 0.02123(7) Uani 1 1 d . . . Cl1 Cl 0.06004(3) 0.52000(7) 0.22025(3) 0.05620(18) Uani 1 1 d . . . P1 P 0.43788(3) 0.27444(5) 0.07500(2) 0.02965(13) Uani 1 1 d . . . F4A F 0.36328(16) 0.2840(8) 0.06134(16) 0.0563(14) Uani 0.638(13) 1 d P . . F2A F 0.5073(2) 0.2695(6) 0.0943(4) 0.085(2) Uani 0.638(13) 1 d P . . F6 F 0.42772(7) 0.39307(14) 0.12209(6) 0.0475(3) Uani 1 1 d . . . F1 F 0.44886(8) 0.15629(15) 0.02765(8) 0.0634(5) Uani 1 1 d . . . F5A F 0.4201(4) 0.1717(4) 0.12777(17) 0.0734(18) Uani 0.638(13) 1 d P . . F3A F 0.4484(3) 0.3828(7) 0.0267(3) 0.071(2) Uani 0.638(13) 1 d P . . C21 C 0.16312(11) 1.0785(2) 0.28051(9) 0.0350(5) Uani 1 1 d . . . H21A H 0.1392 1.1632 0.2737 0.052 Uiso 1 1 calc R . . H21B H 0.2082 1.0998 0.2823 0.052 Uiso 1 1 calc R . . H21C H 0.1503 1.0372 0.3178 0.052 Uiso 1 1 calc R . . O1 O 0.24720(6) 1.04137(14) 0.18323(6) 0.0246(3) Uani 1 1 d . . . N2 N 0.20346(8) 0.74480(16) 0.09151(7) 0.0223(3) Uani 1 1 d . . . N3 N 0.31488(7) 0.82748(16) 0.11365(7) 0.0224(3) Uani 1 1 d . . . N1 N 0.18323(7) 1.02350(16) 0.17438(7) 0.0209(3) Uani 1 1 d . . . C2 C 0.15550(9) 1.13944(19) 0.13741(8) 0.0220(4) Uani 1 1 d . . . C3 C 0.16945(10) 1.2792(2) 0.16513(9) 0.0309(5) Uani 1 1 d . . . H3A H 0.1478 1.2863 0.2028 0.046 Uiso 1 1 calc R . . H3B H 0.1546 1.3521 0.1387 0.046 Uiso 1 1 calc R . . H3C H 0.2149 1.2888 0.1716 0.046 Uiso 1 1 calc R . . C4 C 0.18699(10) 1.1350(2) 0.07771(9) 0.0282(5) Uani 1 1 d . . . H4A H 0.2320 1.1542 0.0826 0.042 Uiso 1 1 calc R . . H4B H 0.1679 1.2043 0.0518 0.042 Uiso 1 1 calc R . . H4C H 0.1813 1.0438 0.0603 0.042 Uiso 1 1 calc R . . C5 C 0.08510(9) 1.1147(2) 0.12927(9) 0.0267(4) Uani 1 1 d . . . H5A H 0.0661 1.1957 0.1096 0.032 Uiso 1 1 calc R . . H5B H 0.0788 1.0346 0.1030 0.032 Uiso 1 1 calc R . . C6 C 0.05106(9) 1.0888(2) 0.18640(9) 0.0304(5) Uani 1 1 d . . . H6A H 0.0058 1.0725 0.1783 0.036 Uiso 1 1 calc R . . H6B H 0.0550 1.1701 0.2124 0.036 Uiso 1 1 calc R . . C7 C 0.07982(9) 0.9641(2) 0.21642(9) 0.0260(4) Uani 1 1 d . . . H7A H 0.0732 0.8830 0.1908 0.031 Uiso 1 1 calc R . . H7B H 0.0573 0.9472 0.2536 0.031 Uiso 1 1 calc R . . C8 C 0.15007(9) 0.9776(2) 0.23026(8) 0.0241(4) Uani 1 1 d . . . C9 C 0.17637(10) 0.8373(2) 0.24710(9) 0.0332(5) Uani 1 1 d . . . H9A H 0.1564 0.8055 0.2832 0.050 Uiso 1 1 calc R . . H9B H 0.2219 0.8444 0.2536 0.050 Uiso 1 1 calc R . . H9C H 0.1677 0.7718 0.2153 0.050 Uiso 1 1 calc R . . C10 C 0.24875(9) 0.66199(19) 0.06929(8) 0.0223(4) Uani 1 1 d . . . C11 C 0.23330(10) 0.5441(2) 0.03848(8) 0.0284(5) Uani 1 1 d . . . H11 H 0.2655 0.4855 0.0244 0.034 Uiso 1 1 calc R . . C12 C 0.17079(11) 0.5119(2) 0.02818(9) 0.0315(5) Uani 1 1 d . . . H12 H 0.1597 0.4327 0.0060 0.038 Uiso 1 1 calc R . . C13 C 0.12475(10) 0.5963(2) 0.05055(8) 0.0292(4) Uani 1 1 d . . . H13 H 0.0814 0.5762 0.0442 0.035 Uiso 1 1 calc R . . C14 C 0.14298(10) 0.7107(2) 0.08241(8) 0.0265(4) Uani 1 1 d . . . H14 H 0.1113 0.7676 0.0986 0.032 Uiso 1 1 calc R . . C15 C 0.31294(9) 0.71181(19) 0.08038(8) 0.0224(4) Uani 1 1 d . . . C16 C 0.37034(9) 0.8854(2) 0.12601(9) 0.0289(4) Uani 1 1 d . . . H16 H 0.3715 0.9662 0.1494 0.035 Uiso 1 1 calc R . . C17 C 0.42622(10) 0.8313(2) 0.10579(10) 0.0334(5) Uani 1 1 d . . . H17 H 0.4652 0.8746 0.1149 0.040 Uiso 1 1 calc R . . C18 C 0.42439(10) 0.7134(2) 0.07220(9) 0.0337(5) Uani 1 1 d . . . H18 H 0.4622 0.6742 0.0580 0.040 Uiso 1 1 calc R . . C19 C 0.36720(10) 0.6531(2) 0.05938(9) 0.0285(5) Uani 1 1 d . . . H19 H 0.3652 0.5718 0.0363 0.034 Uiso 1 1 calc R . . C20 C 0.0000 0.6221(3) 0.2500 0.0371(7) Uani 1 2 d S . . H20A H 0.0180 0.6818 0.2812 0.044 Uiso 0.50 1 calc PR . . H20B H -0.0180 0.6818 0.2188 0.044 Uiso 0.50 1 calc PR . . F4B F 0.3732(5) 0.2097(12) 0.0787(6) 0.080(4) Uani 0.362(13) 1 d P . . F5B F 0.4672(8) 0.1675(7) 0.1191(3) 0.090(4) Uani 0.362(13) 1 d P . . F2B F 0.5103(4) 0.3285(11) 0.0630(5) 0.070(3) Uani 0.362(13) 1 d P . . F3B F 0.4187(8) 0.3725(13) 0.0241(5) 0.086(5) Uani 0.362(13) 1 d P . . 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 0.02032(13) 0.02308(13) 0.02025(12) -0.00408(11) -0.00119(9) 0.00336(11) Cl1 0.0523(4) 0.0504(4) 0.0660(4) -0.0093(3) 0.0052(3) 0.0143(3) P1 0.0299(3) 0.0244(3) 0.0344(3) 0.0000(2) -0.0104(2) -0.0017(2) F4A 0.0285(14) 0.092(4) 0.0479(17) -0.017(2) -0.0122(12) 0.0032(19) F2A 0.0256(19) 0.085(4) 0.143(5) -0.044(4) -0.034(3) 0.012(2) F6 0.0630(9) 0.0458(8) 0.0337(7) -0.0112(6) 0.0036(6) -0.0063(7) F1 0.0648(11) 0.0404(8) 0.0848(12) -0.0326(8) -0.0119(9) 0.0041(8) F5A 0.114(4) 0.0395(18) 0.066(2) 0.0239(14) -0.017(2) -0.021(2) F3A 0.118(5) 0.046(2) 0.049(3) 0.009(2) 0.052(3) 0.008(3) C21 0.0387(13) 0.0455(14) 0.0207(10) -0.0080(10) 0.0000(9) -0.0068(10) O1 0.0171(7) 0.0312(7) 0.0256(7) -0.0073(6) -0.0038(5) 0.0000(6) N2 0.0260(9) 0.0229(8) 0.0180(8) 0.0009(6) -0.0015(6) 0.0019(7) N3 0.0234(9) 0.0229(8) 0.0208(8) 0.0029(7) -0.0006(7) 0.0044(7) N1 0.0185(8) 0.0251(8) 0.0190(8) -0.0047(7) -0.0021(6) -0.0003(7) C2 0.0227(10) 0.0217(10) 0.0216(9) -0.0024(8) -0.0015(8) 0.0018(8) C3 0.0346(12) 0.0249(10) 0.0332(12) -0.0056(9) -0.0012(9) 0.0011(9) C4 0.0335(12) 0.0274(11) 0.0238(10) 0.0023(8) 0.0012(9) 0.0032(9) C5 0.0222(10) 0.0288(10) 0.0291(10) 0.0001(9) -0.0047(8) 0.0035(9) C6 0.0194(10) 0.0345(12) 0.0373(12) 0.0012(10) 0.0009(9) 0.0027(9) C7 0.0243(10) 0.0292(11) 0.0244(10) -0.0018(8) 0.0032(8) 0.0000(8) C8 0.0258(10) 0.0307(11) 0.0157(9) -0.0019(8) 0.0009(8) 0.0005(8) C9 0.0329(12) 0.0404(12) 0.0262(11) 0.0083(10) 0.0000(9) 0.0051(10) C10 0.0327(11) 0.0214(9) 0.0127(9) 0.0043(7) 0.0018(8) 0.0049(8) C11 0.0440(13) 0.0222(10) 0.0191(10) 0.0016(8) 0.0053(9) 0.0051(9) C12 0.0508(14) 0.0222(10) 0.0214(10) 0.0006(8) -0.0032(9) -0.0051(10) C13 0.0365(12) 0.0281(11) 0.0230(10) 0.0022(9) -0.0037(9) -0.0059(9) C14 0.0283(11) 0.0277(10) 0.0234(10) -0.0010(8) -0.0014(8) 0.0009(9) C15 0.0303(11) 0.0222(9) 0.0147(9) 0.0055(8) 0.0011(8) 0.0059(8) C16 0.0271(11) 0.0286(10) 0.0308(11) 0.0027(9) -0.0024(9) 0.0035(9) C17 0.0248(11) 0.0400(12) 0.0354(12) 0.0066(10) -0.0002(9) 0.0040(9) C18 0.0292(12) 0.0418(13) 0.0303(11) 0.0083(10) 0.0036(9) 0.0160(10) C19 0.0342(12) 0.0309(11) 0.0206(10) 0.0035(8) 0.0012(8) 0.0125(9) C20 0.0433(19) 0.0290(16) 0.0389(18) 0.000 0.0029(15) 0.000 F4B 0.051(5) 0.077(6) 0.112(8) -0.050(6) 0.049(5) -0.037(4) F5B 0.159(12) 0.058(4) 0.052(4) 0.018(3) -0.031(5) 0.033(6) F2B 0.035(3) 0.077(5) 0.098(6) -0.041(4) 0.013(4) -0.025(3) F3B 0.162(11) 0.057(6) 0.037(4) -0.008(4) -0.039(6) 0.070(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.8043(14) . ? Ni1 N3 1.8816(17) . ? Ni1 N2 1.8960(16) . ? Ni1 N1 1.8980(16) . ? Cl1 C20 1.7588(19) . ? P1 F4B 1.516(6) . ? P1 F2A 1.534(4) . ? P1 F3A 1.542(6) . ? P1 F3B 1.551(10) . ? P1 F5B 1.569(6) . ? P1 F6 1.5916(14) . ? P1 F1 1.5951(15) . ? P1 F5A 1.611(3) . ? P1 F4A 1.613(3) . ? P1 F2B 1.651(6) . ? F4A F4B 0.850(12) . ? F4A F3B 1.694(15) . ? F2A F2B 0.917(7) . ? F2A F5B 1.429(10) . ? F5A F5B 1.023(11) . ? F5A F4B 1.532(14) . ? F3A F3B 0.641(15) . ? F3A F2B 1.632(10) . ? C21 C8 1.530(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O1 N1 1.382(2) . ? N2 C14 1.341(3) . ? N2 C10 1.358(2) . ? N3 C16 1.333(3) . ? N3 C15 1.357(2) . ? N1 C2 1.522(2) . ? N1 C8 1.528(2) . ? C2 C4 1.522(3) . ? C2 C5 1.524(3) . ? C2 C3 1.527(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.516(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.518(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.527(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.523(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.382(3) . ? C10 C15 1.466(3) . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C19 1.377(3) . ? C16 C17 1.383(3) . ? C16 H16 0.9500 . ? C17 C18 1.379(3) . ? C17 H17 0.9500 . ? C18 C19 1.377(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 Cl1 1.7588(19) 2 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N3 108.64(7) . . ? O1 Ni1 N2 166.54(6) . . ? N3 Ni1 N2 84.67(7) . . ? O1 Ni1 N1 43.75(6) . . ? N3 Ni1 N1 152.29(7) . . ? N2 Ni1 N1 123.03(7) . . ? F4B P1 F2A 147.2(5) . . ? F4B P1 F3A 117.6(6) . . ? F2A P1 F3A 94.5(3) . . ? F4B P1 F3B 93.9(5) . . ? F2A P1 F3B 118.4(5) . . ? F3A P1 F3B 23.9(5) . . ? F4B P1 F5B 92.4(5) . . ? F2A P1 F5B 54.8(4) . . ? F3A P1 F5B 148.2(5) . . ? F3B P1 F5B 169.7(5) . . ? F4B P1 F6 97.7(2) . . ? F2A P1 F6 88.18(18) . . ? F3A P1 F6 90.3(3) . . ? F3B P1 F6 91.1(4) . . ? F5B P1 F6 96.2(3) . . ? F4B P1 F1 83.0(2) . . ? F2A P1 F1 91.27(18) . . ? F3A P1 F1 89.3(3) . . ? F3B P1 F1 88.8(4) . . ? F5B P1 F1 83.9(3) . . ? F6 P1 F1 179.32(9) . . ? F4B P1 F5A 58.6(5) . . ? F2A P1 F5A 90.1(3) . . ? F3A P1 F5A 173.4(3) . . ? F3B P1 F5A 151.2(5) . . ? F5B P1 F5A 37.5(4) . . ? F6 P1 F5A 85.1(2) . . ? F1 P1 F5A 95.3(2) . . ? F4B P1 F4A 31.3(5) . . ? F2A P1 F4A 174.3(3) . . ? F3A P1 F4A 88.5(2) . . ? F3B P1 F4A 64.7(5) . . ? F5B P1 F4A 122.8(5) . . ? F6 P1 F4A 86.9(2) . . ? F1 P1 F4A 93.6(2) . . ? F5A P1 F4A 86.6(2) . . ? F4B P1 F2B 171.4(3) . . ? F2A P1 F2B 33.2(3) . . ? F3A P1 F2B 61.4(4) . . ? F3B P1 F2B 85.2(5) . . ? F5B P1 F2B 87.4(4) . . ? F6 P1 F2B 90.8(2) . . ? F1 P1 F2B 88.5(3) . . ? F5A P1 F2B 123.3(4) . . ? F4A P1 F2B 149.8(4) . . ? F4B F4A P1 68.0(6) . . ? F4B F4A F3B 119.8(7) . . ? P1 F4A F3B 55.9(3) . . ? F2B F2A F5B 142.0(8) . . ? F2B F2A P1 80.4(6) . . ? F5B F2A P1 63.8(3) . . ? F5B F5A F4B 119.9(6) . . ? F5B F5A P1 69.0(4) . . ? F4B F5A P1 57.6(3) . . ? F3B F3A P1 78.8(14) . . ? F3B F3A F2B 141.4(16) . . ? P1 F3A F2B 62.6(3) . . ? C8 C21 H21A 109.5 . . ? C8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 O1 Ni1 71.74(8) . . ? C14 N2 C10 118.51(17) . . ? C14 N2 Ni1 127.65(14) . . ? C10 N2 Ni1 113.77(13) . . ? C16 N3 C15 119.30(17) . . ? C16 N3 Ni1 126.00(14) . . ? C15 N3 Ni1 114.66(13) . . ? O1 N1 C2 111.11(14) . . ? O1 N1 C8 112.22(13) . . ? C2 N1 C8 119.83(14) . . ? O1 N1 Ni1 64.52(8) . . ? C2 N1 Ni1 117.41(12) . . ? C8 N1 Ni1 118.00(12) . . ? C4 C2 C5 109.19(16) . . ? C4 C2 N1 107.51(15) . . ? C5 C2 N1 108.79(15) . . ? C4 C2 C3 107.97(16) . . ? C5 C2 C3 112.09(16) . . ? N1 C2 C3 111.16(15) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C2 113.58(16) . . ? C6 C5 H5A 108.8 . . ? C2 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? C2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 108.96(16) . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 C7 C8 114.23(17) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 109.19(17) . . ? C9 C8 N1 107.47(15) . . ? C7 C8 N1 108.25(15) . . ? C9 C8 C21 109.00(17) . . ? C7 C8 C21 112.14(17) . . ? N1 C8 C21 110.66(16) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 121.14(19) . . ? N2 C10 C15 113.65(17) . . ? C11 C10 C15 125.20(18) . . ? C12 C11 C10 119.74(19) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 119.13(19) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 118.6(2) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? N2 C14 C13 122.87(19) . . ? N2 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? N3 C15 C19 121.21(19) . . ? N3 C15 C10 113.09(16) . . ? C19 C15 C10 125.69(18) . . ? N3 C16 C17 121.9(2) . . ? N3 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 118.9(2) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 119.4(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C15 C19 C18 119.3(2) . . ? C15 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? Cl1 C20 Cl1 111.18(17) 2 . ? Cl1 C20 H20A 109.4 2 . ? Cl1 C20 H20A 109.4 . . ? Cl1 C20 H20B 109.4 2 . ? Cl1 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? F4A F4B P1 80.7(6) . . ? F4A F4B F5A 134.3(8) . . ? P1 F4B F5A 63.8(4) . . ? F5A F5B F2A 129.6(6) . . ? F5A F5B P1 73.5(5) . . ? F2A F5B P1 61.3(3) . . ? F2A F2B F3A 122.2(7) . . ? F2A F2B P1 66.4(5) . . ? F3A F2B P1 56.0(3) . . ? F3A F3B P1 77.2(12) . . ? F3A F3B F4A 136.3(16) . . ? P1 F3B F4A 59.4(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.348 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.051 ############################END############################ data_complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,2-bipyridine)pyridine-N-oxidenickel(0)nitrosyl ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H14 Cl F6 N4 Ni O2 P' _chemical_formula_weight 527.44 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' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.7511(15) _cell_length_b 10.5069(9) _cell_length_c 21.4383(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.663(2) _cell_angle_gamma 90.00 _cell_volume 3994.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.261 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6800 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28805 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4086 _reflns_number_gt 3252 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0195P)^2^+5.0000P] 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 4086 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.299251(14) 0.75120(3) 0.875346(12) 0.02292(8) Uani 1 1 d . . . P1 P 0.59166(3) 0.77493(5) 0.11406(3) 0.02476(13) Uani 1 1 d . . . F1 F 0.58962(7) 0.92495(11) 0.10122(6) 0.0329(3) Uani 1 1 d . . . F2 F 0.55734(7) 0.75020(13) 0.04436(6) 0.0396(3) Uani 1 1 d . . . F3 F 0.50781(7) 0.78140(12) 0.13860(6) 0.0352(3) Uani 1 1 d . . . F4 F 0.59328(7) 0.62429(11) 0.12618(7) 0.0405(4) Uani 1 1 d . . . F5 F 0.67481(7) 0.76740(11) 0.08806(7) 0.0417(4) Uani 1 1 d . . . F6 F 0.62576(8) 0.79959(14) 0.18290(7) 0.0477(4) Uani 1 1 d . . . O2 O 0.24479(8) 0.80079(15) 0.79345(7) 0.0298(3) Uani 1 1 d . . . N3 N 0.23114(8) 0.85244(15) 0.92798(7) 0.0186(3) Uani 1 1 d . . . N4 N 0.22689(9) 0.61284(16) 0.89699(8) 0.0214(4) Uani 1 1 d . . . N2 N 0.19489(9) 0.89612(17) 0.79377(8) 0.0244(4) Uani 1 1 d . . . C1 C 0.23737(11) 0.97737(19) 0.94041(9) 0.0230(4) Uani 1 1 d . . . H1 H 0.2807 1.0216 0.9277 0.028 Uiso 1 1 calc R . . C2 C 0.18298(12) 1.0439(2) 0.97099(10) 0.0290(5) Uani 1 1 d . . . H2 H 0.1890 1.1322 0.9795 0.035 Uiso 1 1 calc R . . C3 C 0.11974(13) 0.9796(2) 0.98893(11) 0.0322(5) Uani 1 1 d . . . H3 H 0.0813 1.0234 1.0097 0.039 Uiso 1 1 calc R . . C4 C 0.11271(11) 0.8508(2) 0.97645(10) 0.0253(5) Uani 1 1 d . . . H4 H 0.0696 0.8052 0.9886 0.030 Uiso 1 1 calc R . . C5 C 0.16951(10) 0.78926(18) 0.94598(9) 0.0183(4) Uani 1 1 d . . . C6 C 0.16847(10) 0.65186(19) 0.93070(9) 0.0187(4) Uani 1 1 d . . . C10 C 0.23192(12) 0.4890(2) 0.88258(10) 0.0280(5) Uani 1 1 d . . . H10 H 0.2731 0.4611 0.8594 0.034 Uiso 1 1 calc R . . C9 C 0.17946(13) 0.4007(2) 0.90020(11) 0.0316(5) Uani 1 1 d . . . H9 H 0.1846 0.3136 0.8892 0.038 Uiso 1 1 calc R . . C8 C 0.11966(12) 0.4404(2) 0.93386(10) 0.0288(5) Uani 1 1 d . . . H8 H 0.0828 0.3811 0.9462 0.035 Uiso 1 1 calc R . . C7 C 0.11376(11) 0.56793(19) 0.94954(10) 0.0231(4) Uani 1 1 d . . . H7 H 0.0729 0.5973 0.9728 0.028 Uiso 1 1 calc R . . N1 N 0.39105(10) 0.7436(2) 0.87737(9) 0.0394(5) Uani 1 1 d . . . O1 O 0.45663(10) 0.7357(3) 0.88237(11) 0.0826(8) Uani 1 1 d . . . C15 C 0.12202(12) 0.8703(2) 0.80492(9) 0.0283(5) Uani 1 1 d . . . H15 H 0.1064 0.7848 0.8109 0.034 Uiso 1 1 calc R . . C14 C 0.07079(12) 0.9676(2) 0.80762(11) 0.0341(5) Uani 1 1 d . . . H14 H 0.0200 0.9500 0.8167 0.041 Uiso 1 1 calc R . . C13 C 0.09324(13) 1.0917(2) 0.79713(11) 0.0364(6) Uani 1 1 d . . . H13 H 0.0580 1.1596 0.7985 0.044 Uiso 1 1 calc R . . C12 C 0.16759(13) 1.1155(2) 0.78461(10) 0.0325(5) Uani 1 1 d . . . H12 H 0.1838 1.1998 0.7766 0.039 Uiso 1 1 calc R . . C11 C 0.21803(12) 1.0163(2) 0.78382(9) 0.0283(5) Uani 1 1 d . . . H11 H 0.2695 1.0325 0.7762 0.034 Uiso 1 1 calc R . . C16 C 0.0000 0.5103(3) 0.7500 0.0836(19) Uani 1 2 d S . . Cl1 Cl 0.08277(9) 0.4595(6) 0.7714(3) 0.0380(12) Uani 0.451(11) 1 d P . . Cl2 Cl 0.07847(11) 0.4094(4) 0.74858(17) 0.0311(7) Uani 0.549(11) 1 d P . . 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 0.01358(12) 0.02785(14) 0.02771(14) 0.00105(12) 0.00506(9) 0.00007(11) P1 0.0191(3) 0.0177(3) 0.0383(3) 0.0044(2) 0.0104(2) -0.0006(2) F1 0.0334(7) 0.0161(6) 0.0506(8) 0.0040(5) 0.0186(6) 0.0023(5) F2 0.0396(8) 0.0388(8) 0.0409(8) -0.0041(6) 0.0077(6) -0.0035(6) F3 0.0252(7) 0.0311(7) 0.0512(8) 0.0069(6) 0.0206(6) 0.0011(5) F4 0.0345(8) 0.0173(6) 0.0712(10) 0.0102(6) 0.0179(7) -0.0008(5) F5 0.0215(6) 0.0221(7) 0.0834(11) 0.0034(7) 0.0233(7) 0.0003(5) F6 0.0502(9) 0.0452(9) 0.0466(9) 0.0051(7) -0.0097(7) -0.0008(7) O2 0.0280(8) 0.0377(9) 0.0240(8) -0.0007(7) 0.0056(6) 0.0070(7) N3 0.0153(8) 0.0210(8) 0.0193(9) 0.0016(7) -0.0014(6) -0.0026(7) N4 0.0180(8) 0.0230(9) 0.0230(9) 0.0009(7) 0.0005(7) 0.0020(7) N2 0.0219(9) 0.0347(10) 0.0166(9) 0.0041(7) 0.0031(7) -0.0002(8) C1 0.0246(11) 0.0216(10) 0.0222(11) 0.0042(8) -0.0030(8) -0.0056(8) C2 0.0367(13) 0.0176(10) 0.0324(12) -0.0012(9) -0.0013(10) -0.0002(9) C3 0.0302(12) 0.0289(12) 0.0382(13) -0.0067(10) 0.0076(10) 0.0044(10) C4 0.0206(10) 0.0258(11) 0.0299(12) -0.0012(9) 0.0061(9) -0.0013(9) C5 0.0173(9) 0.0209(10) 0.0166(10) 0.0026(8) -0.0010(7) -0.0018(8) C6 0.0166(10) 0.0210(10) 0.0182(10) 0.0008(8) -0.0016(8) 0.0011(8) C10 0.0286(11) 0.0250(11) 0.0304(12) -0.0045(9) 0.0010(9) 0.0045(9) C9 0.0365(13) 0.0194(11) 0.0384(13) -0.0053(10) -0.0049(10) -0.0008(9) C8 0.0268(12) 0.0260(11) 0.0333(13) 0.0027(9) -0.0035(10) -0.0094(9) C7 0.0197(10) 0.0248(11) 0.0246(11) 0.0022(9) 0.0004(8) -0.0018(8) N1 0.0189(10) 0.0552(13) 0.0448(12) -0.0016(11) 0.0088(8) 0.0008(9) O1 0.0141(9) 0.147(2) 0.0877(17) -0.0095(16) 0.0105(10) 0.0071(12) C15 0.0248(11) 0.0385(13) 0.0215(11) 0.0114(9) 0.0022(9) -0.0060(10) C14 0.0221(11) 0.0473(15) 0.0333(13) 0.0191(11) 0.0041(9) 0.0005(10) C13 0.0339(13) 0.0423(14) 0.0334(13) 0.0179(11) 0.0068(10) 0.0076(11) C12 0.0393(13) 0.0327(13) 0.0259(12) 0.0109(10) 0.0057(10) -0.0053(10) C11 0.0259(11) 0.0398(13) 0.0199(11) 0.0035(9) 0.0068(9) -0.0078(10) C16 0.0179(18) 0.0191(19) 0.216(6) 0.000 0.026(3) 0.000 Cl1 0.0233(7) 0.0365(18) 0.054(2) 0.0111(18) -0.0042(7) 0.0046(7) Cl2 0.0292(6) 0.0300(13) 0.0344(11) 0.0039(10) 0.0059(6) 0.0111(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 N1 1.6300(18) . ? Ni1 N3 1.9983(16) . ? Ni1 N4 2.0084(17) . ? Ni1 O2 2.0323(15) . ? P1 F6 1.5902(15) . ? P1 F1 1.6002(12) . ? P1 F3 1.6030(12) . ? P1 F5 1.6037(12) . ? P1 F4 1.6040(13) . ? P1 F2 1.6085(15) . ? O2 N2 1.337(2) . ? N3 C1 1.343(3) . ? N3 C5 1.351(2) . ? N4 C10 1.341(3) . ? N4 C6 1.355(2) . ? N2 C11 1.348(3) . ? N2 C15 1.354(3) . ? C1 C2 1.382(3) . ? C1 H1 0.9500 . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.480(3) . ? C6 C7 1.386(3) . ? C10 C9 1.380(3) . ? C10 H10 0.9500 . ? C9 C8 1.376(3) . ? C9 H9 0.9500 . ? C8 C7 1.387(3) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? N1 O1 1.167(2) . ? C15 C14 1.372(3) . ? C15 H15 0.9500 . ? C14 C13 1.385(3) . ? C14 H14 0.9500 . ? C13 C12 1.382(3) . ? C13 H13 0.9500 . ? C12 C11 1.374(3) . ? C12 H12 0.9500 . ? C11 H11 0.9500 . ? C16 Cl1 1.610(2) 2_556 ? C16 Cl1 1.610(2) . ? C16 Cl2 1.752(3) 2_556 ? C16 Cl2 1.752(3) . ? Cl1 Cl2 0.720(3) . ? 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 N3 129.88(9) . . ? N1 Ni1 N4 127.44(9) . . ? N3 Ni1 N4 81.06(7) . . ? N1 Ni1 O2 118.05(8) . . ? N3 Ni1 O2 94.32(6) . . ? N4 Ni1 O2 95.82(7) . . ? F6 P1 F1 90.22(8) . . ? F6 P1 F3 90.44(8) . . ? F1 P1 F3 90.04(7) . . ? F6 P1 F5 90.80(8) . . ? F1 P1 F5 90.16(6) . . ? F3 P1 F5 178.75(9) . . ? F6 P1 F4 90.42(8) . . ? F1 P1 F4 179.37(9) . . ? F3 P1 F4 89.92(7) . . ? F5 P1 F4 89.87(7) . . ? F6 P1 F2 179.86(9) . . ? F1 P1 F2 89.70(7) . . ? F3 P1 F2 89.67(7) . . ? F5 P1 F2 89.09(8) . . ? F4 P1 F2 89.67(8) . . ? N2 O2 Ni1 118.44(11) . . ? C1 N3 C5 118.93(17) . . ? C1 N3 Ni1 125.87(13) . . ? C5 N3 Ni1 114.76(13) . . ? C10 N4 C6 118.50(17) . . ? C10 N4 Ni1 126.78(14) . . ? C6 N4 Ni1 114.70(13) . . ? O2 N2 C11 119.61(17) . . ? O2 N2 C15 119.28(18) . . ? C11 N2 C15 121.11(19) . . ? N3 C1 C2 122.41(19) . . ? N3 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.7(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.08(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N3 C5 C4 121.44(18) . . ? N3 C5 C6 114.70(16) . . ? C4 C5 C6 123.86(17) . . ? N4 C6 C7 121.81(18) . . ? N4 C6 C5 114.28(17) . . ? C7 C6 C5 123.90(18) . . ? N4 C10 C9 122.4(2) . . ? N4 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C8 C9 C10 119.1(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C9 C8 C7 119.26(19) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C6 C7 C8 118.85(19) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? O1 N1 Ni1 176.0(2) . . ? N2 C15 C14 119.9(2) . . ? N2 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C12 C13 C14 119.1(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C11 C12 C13 119.6(2) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N2 C11 C12 120.3(2) . . ? N2 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? Cl1 C16 Cl1 141.2(5) 2_556 . ? Cl1 C16 Cl2 24.25(14) 2_556 2_556 ? Cl1 C16 Cl2 120.7(4) . 2_556 ? Cl1 C16 Cl2 120.7(4) 2_556 . ? Cl1 C16 Cl2 24.25(14) . . ? Cl2 C16 Cl2 105.5(3) 2_556 . ? Cl2 Cl1 C16 89.0(3) . . ? Cl1 Cl2 C16 66.7(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 N1 Ni1 O2 N2 -127.64(15) . . . . ? N3 Ni1 O2 N2 12.61(14) . . . . ? N4 Ni1 O2 N2 94.05(14) . . . . ? N1 Ni1 N3 C1 49.2(2) . . . . ? N4 Ni1 N3 C1 -178.70(17) . . . . ? O2 Ni1 N3 C1 -83.47(16) . . . . ? N1 Ni1 N3 C5 -138.46(15) . . . . ? N4 Ni1 N3 C5 -6.36(13) . . . . ? O2 Ni1 N3 C5 88.87(14) . . . . ? N1 Ni1 N4 C10 -40.7(2) . . . . ? N3 Ni1 N4 C10 -174.88(18) . . . . ? O2 Ni1 N4 C10 91.65(18) . . . . ? N1 Ni1 N4 C6 137.95(15) . . . . ? N3 Ni1 N4 C6 3.75(14) . . . . ? O2 Ni1 N4 C6 -89.72(14) . . . . ? Ni1 O2 N2 C11 90.40(18) . . . . ? Ni1 O2 N2 C15 -88.74(19) . . . . ? C5 N3 C1 C2 0.0(3) . . . . ? Ni1 N3 C1 C2 172.05(15) . . . . ? N3 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C1 N3 C5 C4 0.5(3) . . . . ? Ni1 N3 C5 C4 -172.45(15) . . . . ? C1 N3 C5 C6 -179.37(17) . . . . ? Ni1 N3 C5 C6 7.7(2) . . . . ? C3 C4 C5 N3 -0.4(3) . . . . ? C3 C4 C5 C6 179.43(19) . . . . ? C10 N4 C6 C7 -1.0(3) . . . . ? Ni1 N4 C6 C7 -179.78(15) . . . . ? C10 N4 C6 C5 177.99(17) . . . . ? Ni1 N4 C6 C5 -0.8(2) . . . . ? N3 C5 C6 N4 -4.6(2) . . . . ? C4 C5 C6 N4 175.59(19) . . . . ? N3 C5 C6 C7 174.42(18) . . . . ? C4 C5 C6 C7 -5.4(3) . . . . ? C6 N4 C10 C9 0.7(3) . . . . ? Ni1 N4 C10 C9 179.32(16) . . . . ? N4 C10 C9 C8 -0.1(3) . . . . ? C10 C9 C8 C7 -0.4(3) . . . . ? N4 C6 C7 C8 0.6(3) . . . . ? C5 C6 C7 C8 -178.29(18) . . . . ? C9 C8 C7 C6 0.1(3) . . . . ? N3 Ni1 N1 O1 60(3) . . . . ? N4 Ni1 N1 O1 -52(3) . . . . ? O2 Ni1 N1 O1 -176(3) . . . . ? O2 N2 C15 C14 177.64(19) . . . . ? C11 N2 C15 C14 -1.5(3) . . . . ? N2 C15 C14 C13 1.9(3) . . . . ? C15 C14 C13 C12 -0.6(4) . . . . ? C14 C13 C12 C11 -1.1(3) . . . . ? O2 N2 C11 C12 -179.36(18) . . . . ? C15 N2 C11 C12 -0.2(3) . . . . ? C13 C12 C11 N2 1.5(3) . . . . ? Cl1 C16 Cl1 Cl2 38.6(2) 2_556 . . . ? Cl2 C16 Cl1 Cl2 56.0(4) 2_556 . . . ? Cl1 C16 Cl2 Cl1 -153.0(2) 2_556 . . . ? Cl2 C16 Cl2 Cl1 -132.3(2) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.760 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.056 ############################END############################