Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Marc Fourmigue' _publ_contact_author_address ; Sciences Chimiques de Rennes CNRS Bat 10C Campus de Beaulieu RENNES 35042 FRANCE ; _publ_contact_author_email MARC.FOURMIGUE@UNIV-RENNES1.FR _publ_section_title ; Trifluoromethyl Order-Disorder Transition in Nickel Dithiolene Uniform Spin Chains. ; loop_ _publ_author_name 'Michel Fourmigue' 'Rodolphe Clerac' 'Olivier Jeannin' data_oj133 _database_code_depnum_ccdc_archive 'CCDC 635335' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Me4N+, [Ni(tfadt)2]-' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 F6 N3 Ni S4' _chemical_formula_weight 499.20 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' F F 0.0171 0.0103 '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' _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 24.016(3) _cell_length_b 7.4363(6) _cell_length_c 11.1585(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.587(12) _cell_angle_gamma 90.00 _cell_volume 1975.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4539 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.2 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.022 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5896 _exptl_absorpt_correction_T_max 0.9604 _diffrn_ambient_temperature 293(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 'STOE IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7693 _diffrn_reflns_av_R_equivalents 0.1049 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.82 _reflns_number_total 1940 _reflns_number_gt 1109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1940 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1992 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Ni01 Ni 0.70063(4) 0.0000 0.47476(10) 0.0643(4) Uani 1 2 d S . . S1 S 0.61032(11) 0.0000 0.4656(3) 0.0940(8) Uani 1 2 d S . . S2 S 0.69631(12) 0.0000 0.2828(2) 0.0835(7) Uani 1 2 d S . . S3 S 0.79012(9) 0.0000 0.4872(2) 0.0708(6) Uani 1 2 d S . . S4 S 0.70450(10) 0.0000 0.6666(2) 0.0795(7) Uani 1 2 d S . . C1 C 0.5867(5) 0.0000 0.3183(12) 0.093(3) Uani 1 2 d S . . C2 C 0.6247(4) 0.0000 0.2346(9) 0.082(3) Uani 1 2 d S . . C3 C 0.5274(7) 0.0000 0.2807(17) 0.140(6) Uani 1 2 d S . . C4 C 0.6034(7) 0.0000 0.1020(11) 0.113(4) Uani 1 2 d S . . C5 C 0.8130(3) 0.0000 0.6408(8) 0.064(2) Uani 1 2 d S . . C6 C 0.7742(4) 0.0000 0.7215(8) 0.070(2) Uani 1 2 d S . . C7 C 0.8737(5) 0.0000 0.6715(10) 0.085(3) Uani 1 2 d S . . C8 C 0.7889(6) 0.0000 0.8488(12) 0.104(3) Uani 1 2 d S . . C1B C 0.5602(7) 0.5000 0.6478(14) 0.150(7) Uani 0.86 2 d SP . . H1B1 H 0.5522 0.6216 0.6223 0.224 Uiso 0.43 1 calc PR . . H1B2 H 0.5257 0.4353 0.6482 0.224 Uiso 0.43 1 calc PR . . H1B3 H 0.5824 0.4430 0.5930 0.224 Uiso 0.43 1 calc PR . . C'1B C 0.656(2) 0.5000 0.808(5) 0.060(13) Uani 0.14 2 d SP . . H'1A H 0.6636 0.5000 0.8942 0.090 Uiso 0.14 2 calc SPR . . H'1B H 0.6718 0.6054 0.7762 0.090 Uiso 0.07 1 calc PR . . H'1C H 0.6718 0.3946 0.7762 0.090 Uiso 0.07 1 calc PR . . C2B C 0.5507(5) 0.5000 0.8608(12) 0.125(4) Uani 1 2 d S . . H2B1 H 0.5711 0.5000 0.9408 0.187 Uiso 1 2 calc SR . . H2B2 H 0.5275 0.3946 0.8501 0.187 Uiso 0.50 1 calc PR . . H2B3 H 0.5275 0.6054 0.8501 0.187 Uiso 0.50 1 calc PR . . C3B C 0.6267(5) 0.3389(13) 0.7909(12) 0.133(4) Uani 0.86 1 d P . . H3B1 H 0.6464 0.3426 0.8715 0.199 Uiso 0.86 1 calc PR . . H3B2 H 0.6533 0.3353 0.7338 0.199 Uiso 0.86 1 calc PR . . H3B3 H 0.6035 0.2334 0.7816 0.199 Uiso 0.86 1 calc PR . . C'3B C 0.573(2) 0.331(5) 0.702(6) 0.10(2) Uani 0.14 1 d P . . H'3A H 0.5864 0.2288 0.7501 0.155 Uiso 0.14 1 calc PR . . H'3B H 0.5880 0.3287 0.6269 0.155 Uiso 0.14 1 calc PR . . H'3C H 0.5327 0.3278 0.6873 0.155 Uiso 0.14 1 calc PR . . F1 F 0.6450(4) 0.0000 0.0354(8) 0.152(3) Uani 1 2 d S . . F2 F 0.5715(4) -0.1418(9) 0.0694(6) 0.193(3) Uani 1 1 d . . . F3 F 0.7700(4) 0.1357(8) 0.9041(5) 0.179(3) Uani 1 1 d . . . F4 F 0.8411(4) 0.0000 0.8887(8) 0.252(8) Uani 1 2 d S . . N1 N 0.4835(6) 0.0000 0.2641(16) 0.176(6) Uani 1 2 d S . . N2 N 0.9199(4) 0.0000 0.6920(12) 0.132(4) Uani 1 2 d S . . N1B N 0.5914(3) 0.5000 0.7693(7) 0.0722(18) Uani 1 2 d S . . 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 Ni01 0.0729(7) 0.0579(5) 0.0616(7) 0.000 0.0075(5) 0.000 S1 0.0771(15) 0.1042(17) 0.101(2) 0.000 0.0121(13) 0.000 S2 0.1016(18) 0.0841(14) 0.0633(16) 0.000 0.0055(12) 0.000 S3 0.0732(13) 0.0808(13) 0.0601(14) 0.000 0.0153(10) 0.000 S4 0.0831(15) 0.0856(14) 0.0735(17) 0.000 0.0236(12) 0.000 C1 0.093(7) 0.076(5) 0.109(9) 0.000 0.005(6) 0.000 C2 0.103(7) 0.059(4) 0.077(7) 0.000 -0.012(5) 0.000 C3 0.103(10) 0.120(9) 0.182(16) 0.000 -0.039(11) 0.000 C4 0.161(12) 0.102(8) 0.068(9) 0.000 -0.017(8) 0.000 C5 0.075(5) 0.053(4) 0.065(6) 0.000 0.012(4) 0.000 C6 0.088(6) 0.072(5) 0.052(6) 0.000 0.016(4) 0.000 C7 0.088(7) 0.075(5) 0.087(8) 0.000 0.000(5) 0.000 C8 0.134(10) 0.099(7) 0.078(9) 0.000 0.009(7) 0.000 C1B 0.115(12) 0.27(2) 0.063(10) 0.000 -0.004(8) 0.000 C'1B 0.08(4) 0.04(2) 0.06(4) 0.000 0.02(3) 0.000 C2B 0.096(8) 0.186(12) 0.103(10) 0.000 0.051(7) 0.000 C3B 0.138(9) 0.116(7) 0.151(11) 0.002(7) 0.048(7) 0.027(7) C'3B 0.09(3) 0.06(2) 0.15(6) -0.02(3) -0.03(3) 0.01(2) F1 0.156(7) 0.208(8) 0.093(7) 0.000 0.026(5) 0.000 F2 0.277(9) 0.152(5) 0.128(6) -0.029(4) -0.055(5) -0.050(5) F3 0.325(10) 0.141(4) 0.067(4) -0.031(3) 0.012(4) 0.035(5) F4 0.132(7) 0.55(3) 0.067(6) 0.000 -0.017(5) 0.000 N1 0.097(9) 0.210(14) 0.219(19) 0.000 0.019(10) 0.000 N2 0.068(6) 0.150(9) 0.171(12) 0.000 -0.009(6) 0.000 N1B 0.068(4) 0.078(4) 0.072(5) 0.000 0.015(3) 0.000 _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 Ni01 S4 2.130(3) . ? Ni01 S2 2.131(3) . ? Ni01 S3 2.136(2) . ? Ni01 S1 2.158(3) . ? S1 C1 1.666(13) . ? S2 C2 1.733(10) . ? S3 C5 1.730(9) . ? S4 C6 1.706(9) . ? C1 C2 1.389(16) . ? C1 C3 1.429(17) . ? C2 C4 1.500(15) . ? C3 N1 1.047(17) . ? C4 F1 1.321(17) . ? C4 F2 1.326(10) . ? C4 F2 1.326(10) 6 ? C5 C6 1.377(12) . ? C5 C7 1.454(13) . ? C6 C8 1.418(15) . ? C7 N2 1.102(13) . ? C8 F4 1.272(15) . ? C8 F3 1.296(10) . ? C8 F3 1.296(10) 6 ? C1B N1B 1.459(16) . ? C'1B N1B 1.55(6) . ? C2B N1B 1.504(12) . ? C3B N1B 1.470(10) . ? C'3B N1B 1.50(4) . ? N1B C3B 1.470(10) 6_565 ? N1B C'3B 1.50(4) 6_565 ? 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 S4 Ni01 S2 179.72(11) . . ? S4 Ni01 S3 91.41(10) . . ? S2 Ni01 S3 88.87(10) . . ? S4 Ni01 S1 87.58(11) . . ? S2 Ni01 S1 92.14(12) . . ? S3 Ni01 S1 178.99(12) . . ? C1 S1 Ni01 104.8(4) . . ? C2 S2 Ni01 103.1(4) . . ? C5 S3 Ni01 104.4(3) . . ? C6 S4 Ni01 105.8(3) . . ? C2 C1 C3 121.3(12) . . ? C2 C1 S1 119.7(9) . . ? C3 C1 S1 119.1(11) . . ? C1 C2 C4 119.7(11) . . ? C1 C2 S2 120.3(8) . . ? C4 C2 S2 120.0(10) . . ? N1 C3 C1 173(2) . . ? F1 C4 F2 107.4(9) . . ? F1 C4 F2 107.4(9) . 6 ? F2 C4 F2 105.3(12) . 6 ? F1 C4 C2 111.8(12) . . ? F2 C4 C2 112.3(8) . . ? F2 C4 C2 112.3(8) 6 . ? C6 C5 C7 126.1(8) . . ? C6 C5 S3 119.7(7) . . ? C7 C5 S3 114.2(6) . . ? C5 C6 C8 123.7(10) . . ? C5 C6 S4 118.7(7) . . ? C8 C6 S4 117.6(8) . . ? N2 C7 C5 178.4(12) . . ? F4 C8 F3 103.0(9) . . ? F4 C8 F3 103.0(9) . 6 ? F3 C8 F3 102.3(12) . 6 ? F4 C8 C6 117.0(12) . . ? F3 C8 C6 114.9(8) . . ? F3 C8 C6 114.9(8) 6 . ? C1B N1B C3B 111.5(7) . 6_565 ? C1B N1B C3B 111.5(7) . . ? C3B N1B C3B 109.2(11) 6_565 . ? C1B N1B C'3B 57(2) . . ? C3B N1B C'3B 153(3) 6_565 . ? C3B N1B C'3B 61.6(18) . . ? C1B N1B C'3B 57(2) . 6_565 ? C3B N1B C'3B 61.6(18) 6_565 6_565 ? C3B N1B C'3B 153(3) . 6_565 ? C'3B N1B C'3B 114(4) . 6_565 ? C1B N1B C2B 109.4(10) . . ? C3B N1B C2B 107.5(6) 6_565 . ? C3B N1B C2B 107.5(6) . . ? C'3B N1B C2B 99(3) . . ? C'3B N1B C2B 99(3) 6_565 . ? C1B N1B C'1B 129(2) . . ? C3B N1B C'1B 54.6(5) 6_565 . ? C3B N1B C'1B 54.6(5) . . ? C'3B N1B C'1B 111(2) . . ? C'3B N1B C'1B 111(2) 6_565 . ? C2B N1B C'1B 122(2) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.82 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.456 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.080 # Attachment 'oj2b60.cif' data_oj2b60 _database_code_depnum_ccdc_archive 'CCDC 635336' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Et4N+, [Ni(tfadt)2]-' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 F6 N3 Ni S4' _chemical_formula_weight 555.30 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6741(6) _cell_length_b 18.8293(19) _cell_length_c 16.2154(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.860(10) _cell_angle_gamma 90.00 _cell_volume 2321.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5972 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.1 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.252 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used ; _exptl_absorpt_correction_T_min 0.7377 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_correction_T_ave 0.8538 _diffrn_ambient_temperature 293(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 'STOE IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1.2 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22061 _diffrn_reflns_av_R_equivalents 0.1074 _diffrn_reflns_av_sigmaI/netI 0.1079 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.95 _reflns_number_total 4478 _reflns_number_gt 1794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4478 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.795 _refine_ls_restrained_S_all 0.795 _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 Ni Ni 0.27229(10) 0.54613(4) 0.97536(4) 0.0701(2) Uani 1 1 d . . . S1 S 0.3222(3) 0.64302(8) 0.91303(10) 0.0876(5) Uani 1 1 d . . . S2 S 0.2439(2) 0.48762(8) 0.86104(9) 0.0788(4) Uani 1 1 d . . . S3 S 0.2257(2) 0.45001(8) 1.03978(9) 0.0777(4) Uani 1 1 d . . . S4 S 0.2931(3) 0.60678(8) 1.08802(10) 0.0913(5) Uani 1 1 d . . . C1 C 0.3053(8) 0.6188(3) 0.8104(3) 0.0738(16) Uani 1 1 d . . . C2 C 0.2690(8) 0.5518(3) 0.7872(3) 0.0743(15) Uani 1 1 d . . . C3 C 0.3272(13) 0.6772(4) 0.7503(5) 0.101(2) Uani 1 1 d . . . C4 C 0.2429(11) 0.5290(4) 0.7024(4) 0.099(2) Uani 1 1 d . . . C5 C 0.2294(8) 0.4768(3) 1.1415(3) 0.0712(15) Uani 1 1 d . . . C6 C 0.2583(8) 0.5453(3) 1.1620(3) 0.0755(15) Uani 1 1 d . . . C7 C 0.1967(10) 0.4222(4) 1.1986(4) 0.0875(19) Uani 1 1 d . . . C8 C 0.2691(15) 0.5722(5) 1.2498(5) 0.100(2) Uani 1 1 d . . . C1A C 0.175(4) 0.1233(12) 0.9549(11) 0.116(11) Uani 0.30 1 d P . . H1A1 H 0.0920 0.0875 0.9678 0.139 Uiso 0.30 1 calc PR . . H1A2 H 0.1366 0.1391 0.8984 0.139 Uiso 0.30 1 calc PR . . C'1A C 0.3292(12) 0.1450(5) 1.0221(5) 0.089(3) Uani 0.70 1 d P . . H'1A H 0.4264 0.1779 1.0220 0.106 Uiso 0.70 1 calc PR . . H'1B H 0.3438 0.1216 1.0759 0.106 Uiso 0.70 1 calc PR . . C2A C 0.3431(12) 0.0891(4) 0.9556(4) 0.116(3) Uani 1 1 d . . . C3A C 0.292(3) 0.2529(16) 0.979(3) 0.168(19) Uani 0.30 1 d P . . H3A1 H 0.2838 0.2934 1.0150 0.202 Uiso 0.30 1 calc PR . . H3A2 H 0.4116 0.2353 0.9916 0.202 Uiso 0.30 1 calc PR . . C'3A C 0.1357(15) 0.2295(5) 0.9342(5) 0.096(3) Uani 0.70 1 d P . . H'3A H 0.1074 0.1961 0.8889 0.115 Uiso 0.70 1 calc PR . . H'3B H 0.0333 0.2596 0.9349 0.115 Uiso 0.70 1 calc PR . . C4A C 0.2821(17) 0.2758(5) 0.9126(5) 0.146(5) Uani 1 1 d . . . C5A C 0.203(4) 0.1650(19) 1.1056(16) 0.139(11) Uani 0.30 1 d P . . H5A1 H 0.1392 0.1211 1.1108 0.167 Uiso 0.30 1 calc PR . . H5A2 H 0.3269 0.1525 1.1135 0.167 Uiso 0.30 1 calc PR . . C'5A C 0.1657(14) 0.2391(5) 1.0878(5) 0.088(3) Uani 0.70 1 d P . . H'5A H 0.2663 0.2702 1.0872 0.106 Uiso 0.70 1 calc PR . . H'5B H 0.0611 0.2686 1.0792 0.106 Uiso 0.70 1 calc PR . . C6A C 0.1773(13) 0.2059(5) 1.1737(4) 0.131(3) Uani 1 1 d . . . C7A C -0.032(4) 0.2178(16) 1.0008(16) 0.125(10) Uani 0.30 1 d P . . H7A1 H -0.0335 0.2604 1.0343 0.150 Uiso 0.30 1 calc PR . . H7A2 H -0.0601 0.2318 0.9430 0.150 Uiso 0.30 1 calc PR . . C'7A C 0.0066(13) 0.1357(5) 1.0161(6) 0.095(3) Uani 0.70 1 d P . . H'7A H 0.0355 0.1045 1.0636 0.114 Uiso 0.70 1 calc PR . . H'7B H -0.0034 0.1064 0.9665 0.114 Uiso 0.70 1 calc PR . . C8A C -0.1740(10) 0.1695(5) 1.0217(5) 0.125(3) Uani 1 1 d . . . N1 N 0.2119(12) 0.5128(4) 0.6380(4) 0.154(3) Uani 1 1 d . . . N2 N 0.1684(10) 0.3781(4) 1.2427(4) 0.123(2) Uani 1 1 d . . . N1A N 0.1593(6) 0.1877(2) 1.0137(2) 0.0648(12) Uani 1 1 d . . . F1 F 0.4307(9) 0.7293(3) 0.7801(4) 0.190(3) Uani 1 1 d . . . F2 F 0.1824(9) 0.7108(4) 0.7237(4) 0.209(3) Uani 1 1 d . . . F3 F 0.3885(11) 0.6607(3) 0.6844(4) 0.214(3) Uani 1 1 d . . . F4 F 0.151(3) 0.5396(12) 1.2904(9) 0.133(6) Uani 0.50 1 d P . . F5 F 0.420(3) 0.571(4) 1.288(2) 0.30(2) Uani 0.50 1 d P . . F6 F 0.207(7) 0.6355(9) 1.2554(11) 0.193(16) Uani 0.50 1 d P . . F'4 F 0.379(3) 0.6194(11) 1.2711(9) 0.123(5) Uani 0.50 1 d P . . F'5 F 0.126(3) 0.609(3) 1.255(3) 0.28(3) Uani 0.50 1 d P . . F'6 F 0.316(8) 0.5249(9) 1.3055(10) 0.25(2) Uani 0.50 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 Ni 0.0641(5) 0.0670(4) 0.0785(4) -0.0094(4) 0.0069(3) 0.0043(4) S1 0.1053(14) 0.0709(9) 0.0861(10) -0.0126(8) 0.0108(9) -0.0110(10) S2 0.0857(12) 0.0656(9) 0.0848(10) -0.0121(8) 0.0103(9) 0.0036(9) S3 0.0826(11) 0.0654(8) 0.0839(10) -0.0093(8) 0.0076(8) 0.0084(9) S4 0.1171(16) 0.0707(10) 0.0884(10) -0.0149(8) 0.0226(10) -0.0132(10) C1 0.067(4) 0.074(4) 0.079(4) 0.000(3) 0.005(3) 0.005(3) C2 0.068(4) 0.075(4) 0.080(4) -0.008(3) 0.009(3) 0.002(3) C3 0.107(7) 0.091(5) 0.102(6) -0.009(4) 0.005(5) -0.012(5) C4 0.129(7) 0.098(5) 0.073(4) -0.010(4) 0.017(4) -0.002(4) C5 0.061(4) 0.072(4) 0.079(4) -0.003(3) 0.001(3) 0.009(3) C6 0.077(4) 0.078(4) 0.071(3) -0.009(3) 0.013(3) 0.002(4) C7 0.096(5) 0.081(5) 0.084(4) -0.003(4) 0.004(4) 0.008(4) C8 0.110(8) 0.093(6) 0.097(6) -0.017(5) 0.022(6) -0.011(6) C1A 0.21(3) 0.089(16) 0.051(11) -0.022(11) 0.028(15) -0.075(19) C'1A 0.078(7) 0.104(7) 0.084(6) 0.008(5) 0.011(5) 0.004(6) C2A 0.126(7) 0.124(6) 0.103(5) -0.023(4) 0.032(5) 0.047(5) C3A 0.040(16) 0.13(3) 0.34(5) -0.15(3) 0.03(3) -0.017(16) C'3A 0.123(9) 0.086(6) 0.073(5) 0.006(5) -0.008(6) 0.024(6) C4A 0.234(13) 0.111(7) 0.104(6) 0.010(5) 0.062(7) -0.049(7) C5A 0.13(3) 0.18(3) 0.10(2) 0.00(2) 0.000(17) 0.03(2) C'5A 0.113(8) 0.070(6) 0.083(6) -0.024(5) 0.019(5) -0.016(5) C6A 0.185(9) 0.148(7) 0.061(4) -0.024(4) 0.030(5) -0.030(6) C7A 0.12(2) 0.14(3) 0.114(18) -0.010(16) 0.015(17) 0.06(2) C'7A 0.090(8) 0.086(7) 0.108(7) -0.019(5) 0.005(6) -0.018(6) C8A 0.057(5) 0.163(8) 0.158(7) -0.018(6) 0.026(5) -0.003(5) N1 0.236(10) 0.133(6) 0.088(4) -0.006(4) 0.008(5) -0.013(6) N2 0.156(7) 0.101(5) 0.108(5) 0.012(4) 0.009(4) -0.013(4) N1A 0.066(3) 0.063(3) 0.063(3) -0.006(2) 0.002(2) 0.002(3) F1 0.223(7) 0.147(5) 0.184(5) 0.045(4) -0.029(4) -0.082(5) F2 0.130(5) 0.241(7) 0.249(7) 0.147(6) -0.004(5) -0.001(5) F3 0.339(10) 0.165(5) 0.161(5) 0.012(4) 0.119(6) -0.027(5) F4 0.157(13) 0.162(15) 0.089(8) -0.014(9) 0.048(8) -0.029(11) F5 0.143(15) 0.55(5) 0.17(2) -0.22(3) -0.082(13) 0.16(3) F6 0.38(5) 0.098(9) 0.101(9) -0.018(8) 0.047(16) 0.050(17) F'4 0.125(14) 0.103(9) 0.130(8) -0.037(7) -0.022(10) -0.014(10) F'5 0.127(13) 0.48(7) 0.25(3) -0.26(4) 0.056(15) -0.02(2) F'6 0.56(7) 0.104(9) 0.073(7) 0.006(7) 0.002(18) -0.06(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 Ni S2 2.1417(16) . ? Ni S4 2.1418(17) . ? Ni S3 2.1441(17) . ? Ni S1 2.1452(18) . ? S1 C1 1.713(6) . ? S2 C2 1.730(6) . ? S3 C5 1.721(6) . ? S4 C6 1.714(6) . ? C1 C2 1.336(8) . ? C1 C3 1.494(9) . ? C2 C4 1.429(8) . ? C3 F3 1.264(8) . ? C3 F2 1.300(9) . ? C3 F1 1.312(8) . ? C4 N1 1.082(7) . ? C5 C6 1.342(7) . ? C5 C7 1.429(9) . ? C6 C8 1.502(9) . ? C7 N2 1.137(8) . ? C8 F5 1.238(19) . ? C8 F'4 1.240(15) . ? C8 F'6 1.29(3) . ? C8 F6 1.29(2) . ? C8 F'5 1.31(3) . ? C8 F4 1.340(18) . ? C1A C2A 1.44(3) . ? C1A N1A 1.56(2) . ? C'1A C2A 1.522(11) . ? C'1A N1A 1.522(10) . ? C3A C4A 1.15(5) . ? C3A N1A 1.74(4) . ? C'3A C4A 1.501(15) . ? C'3A N1A 1.501(9) . ? C5A C6A 1.38(3) . ? C5A N1A 1.54(3) . ? C5A C'7A 2.02(3) . ? C'5A C6A 1.519(11) . ? C'5A N1A 1.539(8) . ? C'5A C7A 1.96(3) . ? C7A C8A 1.49(3) . ? C7A N1A 1.56(3) . ? C'7A N1A 1.532(10) . ? C'7A C8A 1.539(12) . ? F4 F'6 1.29(5) . ? F4 F'5 1.43(6) . ? F5 F'4 0.99(5) . ? F5 F'6 1.24(5) . ? F6 F'5 0.80(4) . ? F6 F'4 1.34(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 S2 Ni S4 178.05(8) . . ? S2 Ni S3 89.05(6) . . ? S4 Ni S3 91.86(7) . . ? S2 Ni S1 91.90(7) . . ? S4 Ni S1 87.20(7) . . ? S3 Ni S1 178.88(8) . . ? C1 S1 Ni 103.7(2) . . ? C2 S2 Ni 103.4(2) . . ? C5 S3 Ni 103.7(2) . . ? C6 S4 Ni 103.7(2) . . ? C2 C1 C3 123.3(6) . . ? C2 C1 S1 120.7(5) . . ? C3 C1 S1 116.0(5) . . ? C1 C2 C4 123.5(6) . . ? C1 C2 S2 120.2(4) . . ? C4 C2 S2 116.3(5) . . ? F3 C3 F2 103.8(8) . . ? F3 C3 F1 102.6(8) . . ? F2 C3 F1 101.8(7) . . ? F3 C3 C1 117.3(7) . . ? F2 C3 C1 114.0(7) . . ? F1 C3 C1 115.3(7) . . ? N1 C4 C2 175.3(9) . . ? C6 C5 C7 124.6(5) . . ? C6 C5 S3 120.0(5) . . ? C7 C5 S3 115.4(4) . . ? C5 C6 C8 123.0(6) . . ? C5 C6 S4 120.7(4) . . ? C8 C6 S4 116.2(5) . . ? N2 C7 C5 178.5(8) . . ? F5 C8 F'4 47(2) . . ? F5 C8 F'6 59(2) . . ? F'4 C8 F'6 100.7(19) . . ? F5 C8 F6 108(2) . . ? F'4 C8 F6 63.8(17) . . ? F'6 C8 F6 131.4(17) . . ? F5 C8 F'5 135.9(17) . . ? F'4 C8 F'5 98.5(18) . . ? F'6 C8 F'5 119(2) . . ? F6 C8 F'5 36(2) . . ? F5 C8 F4 114(3) . . ? F'4 C8 F4 132.0(11) . . ? F'6 C8 F4 59(2) . . ? F6 C8 F4 96.2(19) . . ? F'5 C8 F4 65(2) . . ? F5 C8 C6 113.0(11) . . ? F'4 C8 C6 117.0(10) . . ? F'6 C8 C6 113.9(13) . . ? F6 C8 C6 113.9(11) . . ? F'5 C8 C6 107.2(17) . . ? F4 C8 C6 111.0(10) . . ? C2A C1A N1A 119.2(17) . . ? C2A C'1A N1A 116.4(7) . . ? C1A C2A C'1A 63.0(8) . . ? C4A C3A N1A 127(2) . . ? C4A C'3A N1A 120.0(9) . . ? C3A C4A C'3A 61.4(14) . . ? C6A C5A N1A 126(2) . . ? C6A C5A C'7A 123(2) . . ? N1A C5A C'7A 48.7(8) . . ? C6A C'5A N1A 116.7(7) . . ? C6A C'5A C7A 121.1(11) . . ? N1A C'5A C7A 51.1(7) . . ? C5A C6A C'5A 59.6(13) . . ? C8A C7A N1A 116.8(19) . . ? C8A C7A C'5A 118.5(16) . . ? N1A C7A C'5A 50.2(9) . . ? N1A C'7A C8A 115.8(7) . . ? N1A C'7A C5A 49.1(9) . . ? C8A C'7A C5A 115.7(11) . . ? C7A C8A C'7A 63.1(10) . . ? C'3A N1A C'1A 110.8(6) . . ? C'3A N1A C'7A 110.8(7) . . ? C'1A N1A C'7A 108.0(6) . . ? C'3A N1A C'5A 109.1(6) . . ? C'1A N1A C'5A 109.1(6) . . ? C'7A N1A C'5A 109.0(6) . . ? C'3A N1A C5A 163.8(15) . . ? C'1A N1A C5A 72.3(12) . . ? C'7A N1A C5A 82.2(13) . . ? C'5A N1A C5A 56.0(12) . . ? C'3A N1A C1A 83.9(9) . . ? C'1A N1A C1A 60.4(12) . . ? C'7A N1A C1A 69.0(10) . . ? C'5A N1A C1A 166.2(11) . . ? C5A N1A C1A 110.5(15) . . ? C'3A N1A C7A 72.2(11) . . ? C'1A N1A C7A 169.3(13) . . ? C'7A N1A C7A 61.8(12) . . ? C'5A N1A C7A 78.7(11) . . ? C5A N1A C7A 107.9(15) . . ? C1A N1A C7A 110.6(16) . . ? C'3A N1A C3A 50.0(13) . . ? C'1A N1A C3A 82.4(11) . . ? C'7A N1A C3A 160.8(14) . . ? C'5A N1A C3A 81.5(11) . . ? C5A N1A C3A 116.7(19) . . ? C1A N1A C3A 104.6(12) . . ? C7A N1A C3A 106.4(15) . . ? F'6 F4 C8 58.5(12) . . ? F'6 F4 F'5 110(2) . . ? C8 F4 F'5 56.2(12) . . ? F'4 F5 C8 66.6(16) . . ? F'4 F5 F'6 121(3) . . ? C8 F5 F'6 62.5(18) . . ? F'5 F6 C8 73(3) . . ? F'5 F6 F'4 127(5) . . ? C8 F6 F'4 56.2(15) . . ? F5 F'4 C8 66(2) . . ? F5 F'4 F6 122(3) . . ? C8 F'4 F6 59.9(11) . . ? F6 F'5 C8 71(3) . . ? F6 F'5 F4 121(6) . . ? C8 F'5 F4 59(2) . . ? F5 F'6 C8 58.7(16) . . ? F5 F'6 F4 117(4) . . ? C8 F'6 F4 63(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.470 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.055 data_tma_pnma _database_code_depnum_ccdc_archive 'CCDC 635337' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Et4N+, Ni(tfadt)2-' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 N, C8 F6 N2 Ni S4' _chemical_formula_sum 'C16 H20 F6 N3 Ni S4' _chemical_formula_weight 555.30 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' N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.384(3) _cell_length_b 7.7447(15) _cell_length_c 19.192(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2435.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3225 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 19.5 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Stoe-IPDS _diffrn_measurement_method 'oscillation phi incr 1.2 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18225 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 22.37 _reflns_number_total 1696 _reflns_number_gt 559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1696 _refine_ls_number_parameters 148 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1686 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2721 _refine_ls_wR_factor_gt 0.2238 _refine_ls_goodness_of_fit_ref 0.793 _refine_ls_restrained_S_all 0.792 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.003 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 0.52530(15) 0.2500 0.54768(10) 0.1407(11) Uani 1 2 d S . . S1 S 0.4576(3) 0.2500 0.4537(2) 0.1574(19) Uani 1 2 d S . . S2 S 0.4167(4) 0.2500 0.6078(2) 0.182(2) Uani 1 2 d S . . S3 S 0.6348(3) 0.2500 0.4883(2) 0.166(2) Uani 1 2 d S . . S4 S 0.5918(4) 0.2500 0.6428(2) 0.185(2) Uani 1 2 d S . . C1 C 0.3590(10) 0.2500 0.4804(10) 0.131(5) Uani 1 2 d SD . . C2 C 0.2987(16) 0.2500 0.4264(12) 0.188(9) Uani 1 2 d SD . . C3 C 0.3399(11) 0.2500 0.5507(11) 0.165(7) Uani 1 2 d SD . . C4 C 0.2526(12) 0.2500 0.5760(12) 0.230(11) Uiso 1 2 d SD . . F1 F 0.2426(10) 0.113(2) 0.6174(8) 0.224(10) Uiso 0.59(3) 1 d PD . . F2 F 0.2112(13) 0.117(3) 0.5475(12) 0.221(14) Uiso 0.41(3) 1 d PD . . F3 F 0.1937(17) 0.2500 0.5279(14) 0.284(14) Uiso 0.59(3) 2 d SPD . . F3' F 0.236(3) 0.2500 0.6435(13) 0.28(2) Uiso 0.41(3) 2 d SPD . . C5 C 0.7132(14) 0.2500 0.5518(11) 0.169(7) Uani 1 2 d SD . . C6 C 0.7955(17) 0.2500 0.5256(14) 0.246(13) Uani 1 2 d SD . . N2 N 0.8544(15) 0.2500 0.5031(17) 0.340(18) Uani 1 2 d SD . . C7 C 0.6927(13) 0.2500 0.6180(11) 0.165(7) Uani 1 2 d SD . . C8 C 0.7516(15) 0.2500 0.6788(13) 0.273(14) Uiso 1 2 d SD . . F4 F 0.7491(11) 0.113(2) 0.7212(9) 0.245(11) Uiso 0.58(3) 1 d PD . . F5 F 0.8050(17) 0.122(4) 0.6703(18) 0.285(18) Uiso 0.42(3) 1 d PD . . F6 F 0.8308(17) 0.2500 0.6620(19) 0.303(18) Uiso 0.58(3) 2 d SPD . . F6' F 0.711(3) 0.2500 0.740(2) 0.36(3) Uiso 0.42(3) 2 d SPD . . N1 N 0.2568(16) 0.2500 0.3841(14) 0.288(14) Uani 1 2 d SD . . N3 N 0.4956(10) 0.2500 0.1937(8) 0.191(7) Uani 1 2 d SD . . C10 C 0.450(3) 0.138(10) 0.247(3) 0.88(16) Uani 0.50 1 d PD . . C11 C 0.379(4) 0.2500 0.220(4) 0.42(3) Uiso 1 2 d SD . . C12 C 0.544(3) 0.130(4) 0.242(2) 0.34(3) Uiso 0.50 1 d PD . . C13 C 0.602(2) 0.2500 0.2808(17) 0.274(13) Uiso 1 2 d SD . . C14 C 0.518(2) 0.137(5) 0.1296(15) 0.49(3) Uiso 1 1 d D . . C15 C 0.483(3) -0.033(7) 0.158(2) 0.55(3) Uiso 1 1 d 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 0.163(2) 0.1410(18) 0.1181(15) 0.000 0.0087(13) 0.000 S1 0.192(5) 0.164(4) 0.116(3) 0.000 0.007(3) 0.000 S2 0.188(5) 0.236(6) 0.124(3) 0.000 0.012(3) 0.000 S3 0.185(4) 0.184(5) 0.130(3) 0.000 0.027(3) 0.000 S4 0.190(6) 0.242(6) 0.124(3) 0.000 0.004(3) 0.000 C1 0.125(14) 0.139(13) 0.129(12) 0.000 0.005(11) 0.000 C2 0.18(2) 0.23(2) 0.156(19) 0.000 0.002(16) 0.000 C3 0.145(16) 0.182(17) 0.170(18) 0.000 0.011(14) 0.000 C5 0.18(2) 0.180(18) 0.144(15) 0.000 0.024(16) 0.000 C6 0.18(3) 0.39(4) 0.168(19) 0.000 0.034(19) 0.000 N2 0.23(3) 0.42(4) 0.37(4) 0.000 0.15(3) 0.000 C7 0.19(2) 0.158(16) 0.150(15) 0.000 -0.012(15) 0.000 N1 0.23(2) 0.39(4) 0.24(3) 0.000 -0.082(19) 0.000 N3 0.163(14) 0.28(2) 0.128(10) 0.000 0.025(9) 0.000 C10 1.1(3) 1.2(4) 0.31(7) 0.23(13) 0.32(13) -0.4(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 S1 2.118(5) . ? Ni1 S2 2.120(6) . ? Ni1 S4 2.125(5) . ? Ni1 S3 2.125(5) . ? S1 C1 1.695(16) . ? S2 C3 1.669(19) . ? S3 C5 1.77(2) . ? S4 C7 1.72(2) . ? C1 C3 1.38(2) . ? C1 C2 1.43(2) . ? C2 N1 1.06(2) . ? C3 C4 1.511(10) . ? C4 F3' 1.326(10) . ? C4 F1 1.335(9) 7_565 ? C4 F1 1.335(9) . ? C4 F3 1.335(10) . ? C4 F2 1.347(10) . ? C4 F2 1.347(10) 7_565 ? F1 F3' 1.18(2) . ? F1 F2 1.44(2) . ? F2 F3 1.13(3) . ? F3 F2 1.13(3) 7_565 ? F3' F1 1.18(2) 7_565 ? C5 C7 1.31(2) . ? C5 C6 1.44(2) . ? C6 N2 1.06(2) . ? C7 C8 1.514(10) . ? C8 F5 1.335(10) 7_565 ? C8 F5 1.335(10) . ? C8 F6 1.336(10) . ? C8 F4 1.340(10) 7_565 ? C8 F4 1.340(10) . ? C8 F6' 1.346(10) . ? F4 F6' 1.28(3) . ? F4 F5 1.34(3) . ? F5 F6 1.09(4) . ? F6 F5 1.09(4) 7_565 ? F6' F4 1.28(3) 7_565 ? N3 C10 1.531(10) 7_565 ? N3 C10 1.531(10) . ? N3 C12 1.535(10) 7_565 ? N3 C12 1.535(10) . ? N3 C14 1.552(10) . ? N3 C14 1.552(10) 7_565 ? C10 C11 1.529(10) . ? C12 C13 1.521(10) . ? C14 C15 1.535(10) . ? 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 S1 Ni1 S2 91.4(2) . . ? S1 Ni1 S4 179.3(2) . . ? S2 Ni1 S4 87.9(2) . . ? S1 Ni1 S3 89.2(2) . . ? S2 Ni1 S3 179.4(2) . . ? S4 Ni1 S3 91.6(2) . . ? C1 S1 Ni1 104.0(7) . . ? C3 S2 Ni1 106.0(7) . . ? C5 S3 Ni1 104.1(8) . . ? C7 S4 Ni1 104.8(7) . . ? C3 C1 C2 123.3(17) . . ? C3 C1 S1 120.7(14) . . ? C2 C1 S1 116.1(15) . . ? N1 C2 C1 177(3) . . ? C1 C3 C4 121.8(18) . . ? C1 C3 S2 118.0(14) . . ? C4 C3 S2 120.2(17) . . ? F3' C4 F1 52.5(12) . 7_565 ? F3' C4 F1 52.5(12) . . ? F1 C4 F1 105(2) 7_565 . ? F3' C4 F3 122(3) . . ? F1 C4 F3 108.9(16) 7_565 . ? F1 C4 F3 108.9(16) . . ? F3' C4 F2 107(2) . . ? F1 C4 F2 142(2) 7_565 . ? F1 C4 F2 64.9(11) . . ? F3 C4 F2 49.9(14) . . ? F3' C4 F2 107(2) . 7_565 ? F1 C4 F2 64.9(11) 7_565 7_565 ? F1 C4 F2 142(2) . 7_565 ? F3 C4 F2 49.9(14) . 7_565 ? F2 C4 F2 99(3) . 7_565 ? F3' C4 C3 121(3) . . ? F1 C4 C3 107.9(14) 7_565 . ? F1 C4 C3 107.9(14) . . ? F3 C4 C3 118(2) . . ? F2 C4 C3 110.3(15) . . ? F2 C4 C3 110.3(15) 7_565 . ? F3' F1 C4 63.4(8) . . ? F3' F1 F2 110(2) . . ? C4 F1 F2 58.0(7) . . ? F3 F2 C4 64.6(10) . . ? F3 F2 F1 115.0(17) . . ? C4 F2 F1 57.2(7) . . ? F2 F3 F2 131(2) 7_565 . ? F2 F3 C4 65.6(10) 7_565 . ? F2 F3 C4 65.6(10) . . ? F1 F3' F1 128.2(18) 7_565 . ? F1 F3' C4 64.1(9) 7_565 . ? F1 F3' C4 64.1(9) . . ? C7 C5 C6 125(2) . . ? C7 C5 S3 118.7(17) . . ? C6 C5 S3 116.1(16) . . ? N2 C6 C5 176(4) . . ? C5 C7 C8 126(2) . . ? C5 C7 S4 120.8(16) . . ? C8 C7 S4 113.6(17) . . ? F5 C8 F5 96(4) 7_565 . ? F5 C8 F6 48.3(19) 7_565 . ? F5 C8 F6 48(2) . . ? F5 C8 F4 60.2(14) 7_565 7_565 ? F5 C8 F4 133(2) . 7_565 ? F6 C8 F4 100.2(18) . 7_565 ? F5 C8 F4 133(2) 7_565 . ? F5 C8 F4 60.2(14) . . ? F6 C8 F4 100.2(18) . . ? F4 C8 F4 105(3) 7_565 . ? F5 C8 F6' 115(2) 7_565 . ? F5 C8 F6' 115(2) . . ? F6 C8 F6' 134(3) . . ? F4 C8 F6' 57.1(15) 7_565 . ? F4 C8 F6' 57.1(15) . . ? F5 C8 C7 109(2) 7_565 . ? F5 C8 C7 109(2) . . ? F6 C8 C7 116(3) . . ? F4 C8 C7 116.6(14) 7_565 . ? F4 C8 C7 116.6(14) . . ? F6' C8 C7 111(3) . . ? F6' F4 F5 119.5(15) . . ? F6' F4 C8 61.7(9) . . ? F5 F4 C8 59.8(9) . . ? F6 F5 C8 65.9(12) . . ? F6 F5 F4 115(3) . . ? C8 F5 F4 60.1(9) . . ? F5 F6 F5 131(2) 7_565 . ? F5 F6 C8 65.8(12) 7_565 . ? F5 F6 C8 65.8(12) . . ? F4 F6' F4 112(3) 7_565 . ? F4 F6' C8 61.2(10) 7_565 . ? F4 F6' C8 61.2(10) . . ? C10 N3 C10 69(7) 7_565 . ? C10 N3 C12 61(3) 7_565 7_565 ? C10 N3 C12 102(4) . 7_565 ? C10 N3 C12 102(4) 7_565 . ? C10 N3 C12 61(3) . . ? C12 N3 C12 75(3) 7_565 . ? C10 N3 C14 164(3) 7_565 . ? C10 N3 C14 109(4) . . ? C12 N3 C14 134(3) 7_565 . ? C12 N3 C14 91(2) . . ? C10 N3 C14 109(4) 7_565 7_565 ? C10 N3 C14 164(3) . 7_565 ? C12 N3 C14 91(2) 7_565 7_565 ? C12 N3 C14 134(3) . 7_565 ? C14 N3 C14 68(3) . 7_565 ? C11 C10 N3 80(3) . . ? C13 C12 N3 104(2) . . ? C15 C14 N3 96(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 22.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.361 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.077