data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _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 ; The contrasted structural and magnetic behaviour of two single-component paramagnetic dithiolene complexes. ; loop_ _publ_author_name 'Michel Fourmigue' 'Mitsushiro Nomura' # Attachment 'B700278E_mn165abs.cif' data_mn165abs _database_code_depnum_ccdc_archive 'CCDC 630860' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety CpNi(bddt) _chemical_formula_sum 'C11 H13 Ni S4' _chemical_formula_weight 332.16 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' 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5803(12) _cell_length_b 11.9991(15) _cell_length_c 12.9458(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.406(17) _cell_angle_gamma 90.00 _cell_volume 1331.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4012 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.65 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.052 _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 0.7308 _exptl_absorpt_correction_T_max 0.8128 _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. 1.8' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10111 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_sigmaI/netI 0.1119 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2413 _reflns_number_gt 1330 _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^)+(0.0303P)^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 2413 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.842 _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 0.13928(8) 0.82079(5) 0.86837(6) 0.0416(2) Uani 1 1 d . . . S1 S -0.01953(17) 0.77575(12) 0.98361(11) 0.0454(4) Uani 1 1 d . . . S2 S 0.00892(17) 0.73300(12) 0.75124(12) 0.0448(4) Uani 1 1 d . . . S3 S -0.31645(17) 0.65132(12) 0.99024(12) 0.0482(4) Uani 1 1 d . . . S4 S -0.29884(17) 0.62027(11) 0.73427(12) 0.0452(4) Uani 1 1 d . . . C1 C -0.1641(6) 0.7016(4) 0.9152(4) 0.0387(13) Uani 1 1 d . . . C2 C -0.1545(6) 0.6863(4) 0.8134(4) 0.0389(13) Uani 1 1 d . . . C3 C -0.2720(7) 0.5044(4) 1.0063(4) 0.0481(15) Uani 1 1 d . . . H3A H -0.1640 0.4983 1.0309 0.058 Uiso 1 1 calc R . . H3B H -0.3356 0.4758 1.0605 0.058 Uiso 1 1 calc R . . C4 C -0.2949(7) 0.4287(4) 0.9131(5) 0.0508(16) Uani 1 1 d . . . H4A H -0.3027 0.3527 0.9380 0.061 Uiso 1 1 calc R . . H4B H -0.3942 0.4473 0.8788 0.061 Uiso 1 1 calc R . . C5 C -0.1714(7) 0.4315(4) 0.8331(4) 0.0446(15) Uani 1 1 d . . . H5A H -0.0834 0.4744 0.8608 0.053 Uiso 1 1 calc R . . H5B H -0.1352 0.3559 0.8224 0.053 Uiso 1 1 calc R . . C6 C -0.2215(7) 0.4799(4) 0.7292(4) 0.0452(15) Uani 1 1 d . . . H6A H -0.3004 0.4317 0.6971 0.054 Uiso 1 1 calc R . . H6B H -0.1326 0.4799 0.6853 0.054 Uiso 1 1 calc R . . C7 C 0.2563(8) 0.9637(6) 0.9264(7) 0.072(2) Uani 1 1 d . . . H7 H 0.2157 1.0121 0.9746 0.086 Uiso 1 1 calc R . . C8 C 0.2380(8) 0.9733(6) 0.8207(8) 0.076(2) Uani 1 1 d . . . H8 H 0.1860 1.0304 0.7849 0.091 Uiso 1 1 calc R . . C9 C 0.3106(8) 0.8831(7) 0.7770(5) 0.071(2) Uani 1 1 d . . . H9 H 0.3111 0.8669 0.7068 0.085 Uiso 1 1 calc R . . C10 C 0.3845(6) 0.8193(5) 0.8576(5) 0.0525(16) Uani 1 1 d . . . H10 H 0.4464 0.7565 0.8500 0.063 Uiso 1 1 calc R . . C11 C 0.3463(7) 0.8690(5) 0.9494(5) 0.0607(19) Uani 1 1 d . . . H11 H 0.3755 0.8437 1.0153 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0359(4) 0.0426(4) 0.0463(5) 0.0060(4) 0.0018(3) -0.0023(3) S1 0.0421(8) 0.0547(9) 0.0392(9) -0.0029(7) 0.0006(7) -0.0060(7) S2 0.0467(9) 0.0491(8) 0.0391(8) 0.0027(7) 0.0068(7) -0.0040(7) S3 0.0395(8) 0.0588(10) 0.0473(9) -0.0025(7) 0.0130(8) -0.0005(7) S4 0.0414(8) 0.0498(9) 0.0436(9) 0.0019(7) -0.0066(8) 0.0023(7) C1 0.041(3) 0.036(3) 0.040(4) 0.002(2) 0.007(3) 0.005(2) C2 0.038(3) 0.035(3) 0.043(4) 0.004(3) 0.005(3) 0.004(2) C3 0.042(4) 0.066(4) 0.037(4) 0.010(3) 0.002(3) -0.008(3) C4 0.048(4) 0.045(3) 0.060(4) 0.009(3) 0.005(3) -0.004(3) C5 0.043(3) 0.039(3) 0.052(4) 0.002(3) 0.008(3) 0.009(2) C6 0.046(4) 0.046(3) 0.043(4) -0.005(3) 0.003(3) -0.005(3) C7 0.062(5) 0.055(4) 0.097(7) -0.018(4) 0.005(5) -0.019(3) C8 0.056(5) 0.057(5) 0.114(8) 0.040(5) -0.001(5) -0.013(3) C9 0.054(4) 0.115(6) 0.044(4) 0.024(4) 0.001(4) -0.031(4) C10 0.030(3) 0.062(4) 0.066(5) 0.000(4) 0.009(3) -0.002(3) C11 0.055(4) 0.063(4) 0.063(5) 0.006(3) -0.013(4) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C9 2.065(7) . ? Ni1 C11 2.105(6) . ? Ni1 C7 2.110(6) . ? Ni1 C10 2.114(5) . ? Ni1 C8 2.120(6) . ? Ni1 S2 2.1255(16) . ? Ni1 S1 2.1320(18) . ? S1 C1 1.738(5) . ? S2 C2 1.739(6) . ? S3 C1 1.768(6) . ? S3 C3 1.813(5) . ? S4 C2 1.762(5) . ? S4 C6 1.813(5) . ? C1 C2 1.337(7) . ? C3 C4 1.516(7) . ? C4 C5 1.513(8) . ? C5 C6 1.511(7) . ? C7 C8 1.376(10) . ? C7 C11 1.399(9) . ? C8 C9 1.381(10) . ? C9 C10 1.422(8) . ? C10 C11 1.381(8) . ? 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 C9 Ni1 C11 65.2(3) . . ? C9 Ni1 C7 64.5(3) . . ? C11 Ni1 C7 38.8(2) . . ? C9 Ni1 C10 39.7(2) . . ? C11 Ni1 C10 38.2(2) . . ? C7 Ni1 C10 64.5(3) . . ? C9 Ni1 C8 38.5(3) . . ? C11 Ni1 C8 64.5(3) . . ? C7 Ni1 C8 38.0(3) . . ? C10 Ni1 C8 65.0(3) . . ? C9 Ni1 S2 97.9(2) . . ? C11 Ni1 S2 154.0(2) . . ? C7 Ni1 S2 152.3(2) . . ? C10 Ni1 S2 116.37(19) . . ? C8 Ni1 S2 115.1(3) . . ? C9 Ni1 S1 169.7(2) . . ? C11 Ni1 S1 105.8(2) . . ? C7 Ni1 S1 105.4(2) . . ? C10 Ni1 S1 135.32(18) . . ? C8 Ni1 S1 134.2(3) . . ? S2 Ni1 S1 92.34(6) . . ? C1 S1 Ni1 103.7(2) . . ? C2 S2 Ni1 103.90(19) . . ? C1 S3 C3 103.8(3) . . ? C2 S4 C6 100.9(2) . . ? C2 C1 S1 120.1(4) . . ? C2 C1 S3 124.9(4) . . ? S1 C1 S3 115.0(3) . . ? C1 C2 S2 119.7(4) . . ? C1 C2 S4 124.4(4) . . ? S2 C2 S4 115.9(3) . . ? C4 C3 S3 118.2(4) . . ? C5 C4 C3 117.4(5) . . ? C6 C5 C4 115.9(5) . . ? C5 C6 S4 114.6(4) . . ? C8 C7 C11 108.5(7) . . ? C8 C7 Ni1 71.4(4) . . ? C11 C7 Ni1 70.4(3) . . ? C7 C8 C9 107.9(6) . . ? C7 C8 Ni1 70.6(4) . . ? C9 C8 Ni1 68.6(4) . . ? C8 C9 C10 108.5(7) . . ? C8 C9 Ni1 72.9(4) . . ? C10 C9 Ni1 72.0(4) . . ? C11 C10 C9 106.5(6) . . ? C11 C10 Ni1 70.5(3) . . ? C9 C10 Ni1 68.3(3) . . ? C10 C11 C7 108.5(6) . . ? C10 C11 Ni1 71.3(3) . . ? C7 C11 Ni1 70.8(3) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.563 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.092 data_mn157abs _database_code_depnum_ccdc_archive 'CCDC 630861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety CpNi(oxddt) _chemical_formula_sum 'C15 H13 Ni S4' _chemical_formula_weight 380.20 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7690(10) _cell_length_b 9.3180(12) _cell_length_c 10.3604(15) _cell_angle_alpha 87.844(16) _cell_angle_beta 83.577(15) _cell_angle_gamma 62.422(13) _cell_volume 745.55(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3994 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 390 _exptl_absorpt_coefficient_mu 1.845 _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 0.7061 _exptl_absorpt_correction_T_max 0.8691 _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. 1.1' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7319 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.92 _reflns_number_total 2714 _reflns_number_gt 1577 _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^)+(0.1278P)^2^+1.8906P] 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 2714 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.22515(14) 0.73618(15) 0.70982(12) 0.0389(4) Uani 1 1 d . . . S1 S -0.0412(3) 0.8052(3) 0.6983(2) 0.0460(7) Uani 1 1 d . . . S2 S 0.2844(3) 0.6917(3) 0.5065(2) 0.0446(6) Uani 1 1 d . . . S3 S -0.2714(3) 0.8824(3) 0.4916(3) 0.0458(7) Uani 1 1 d . . . S4 S 0.0931(3) 0.7638(3) 0.2775(2) 0.0416(6) Uani 1 1 d . . . C1 C -0.0570(11) 0.8065(10) 0.5328(9) 0.037(2) Uani 1 1 d . . . C2 C 0.0875(11) 0.7556(10) 0.4479(9) 0.036(2) Uani 1 1 d . . . C3 C -0.2784(12) 0.7077(12) 0.4199(9) 0.043(2) Uani 1 1 d . . . H3A H -0.1773 0.6091 0.4389 0.052 Uiso 1 1 calc R . . H3B H -0.3802 0.7002 0.4589 0.052 Uiso 1 1 calc R . . C4 C 0.0408(11) 0.6043(12) 0.2329(10) 0.045(2) Uani 1 1 d . . . H4A H 0.1263 0.5366 0.1644 0.054 Uiso 1 1 calc R . . H4B H 0.0458 0.5368 0.3075 0.054 Uiso 1 1 calc R . . C5 C -0.2830(11) 0.7225(11) 0.2769(9) 0.035(2) Uani 1 1 d . . . C6 C -0.1352(11) 0.6735(10) 0.1876(9) 0.037(2) Uani 1 1 d . . . C7 C -0.1564(12) 0.6999(11) 0.0557(9) 0.043(2) Uani 1 1 d . . . H7 H -0.0588 0.6684 -0.0040 0.051 Uiso 1 1 calc R . . C8 C -0.3155(13) 0.7703(11) 0.0118(10) 0.045(2) Uani 1 1 d . . . H8 H -0.3250 0.7851 -0.0768 0.054 Uiso 1 1 calc R . . C9 C -0.4612(12) 0.8191(12) 0.0976(10) 0.046(2) Uani 1 1 d . . . H9 H -0.5696 0.8683 0.0674 0.055 Uiso 1 1 calc R . . C10 C -0.4478(12) 0.7956(12) 0.2290(10) 0.045(2) Uani 1 1 d . . . H10 H -0.5474 0.8279 0.2868 0.054 Uiso 1 1 calc R . . C11 C 0.2154(13) 0.7896(13) 0.9033(10) 0.053(3) Uani 1 1 d . . . H11 H 0.1105 0.8388 0.9553 0.063 Uiso 1 1 calc R . . C12 C 0.2933(15) 0.8712(13) 0.8297(11) 0.054(3) Uani 1 1 d . . . H12 H 0.2556 0.9823 0.8291 0.065 Uiso 1 1 calc R . . C13 C 0.4398(16) 0.7525(18) 0.7569(11) 0.064(3) Uani 1 1 d . . . H13 H 0.5127 0.7716 0.6943 0.077 Uiso 1 1 calc R . . C14 C 0.4573(14) 0.5965(14) 0.7959(11) 0.059(3) Uani 1 1 d . . . H14 H 0.5452 0.4964 0.7657 0.071 Uiso 1 1 calc R . . C15 C 0.3186(14) 0.6237(13) 0.8869(10) 0.050(3) Uani 1 1 d . . . H15 H 0.2979 0.5441 0.9301 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0367(6) 0.0447(7) 0.0395(7) 0.0023(5) -0.0119(5) -0.0207(5) S1 0.0385(12) 0.0661(16) 0.0383(13) -0.0025(12) -0.0036(10) -0.0281(12) S2 0.0324(11) 0.0641(15) 0.0397(13) -0.0017(11) -0.0069(9) -0.0235(11) S3 0.0318(11) 0.0569(15) 0.0468(14) -0.0094(12) -0.0076(10) -0.0172(10) S4 0.0408(12) 0.0532(14) 0.0370(13) 0.0019(10) -0.0072(10) -0.0264(11) C1 0.039(4) 0.030(4) 0.043(5) -0.003(4) -0.010(4) -0.015(4) C2 0.037(4) 0.033(4) 0.038(5) -0.003(4) -0.008(4) -0.015(4) C3 0.038(5) 0.063(6) 0.038(5) 0.009(5) -0.012(4) -0.030(5) C4 0.036(5) 0.048(5) 0.042(5) 0.000(4) -0.009(4) -0.012(4) C5 0.034(4) 0.044(5) 0.040(5) 0.000(4) -0.006(4) -0.027(4) C6 0.039(4) 0.035(4) 0.038(5) 0.002(4) -0.009(4) -0.018(4) C7 0.045(5) 0.046(5) 0.039(5) -0.004(4) -0.004(4) -0.023(4) C8 0.054(5) 0.044(5) 0.045(6) 0.003(4) -0.020(5) -0.027(5) C9 0.042(5) 0.045(5) 0.052(6) 0.003(5) -0.019(5) -0.020(4) C10 0.043(5) 0.056(6) 0.045(6) 0.000(5) -0.012(4) -0.028(5) C11 0.040(5) 0.060(7) 0.047(6) -0.001(5) -0.011(4) -0.013(5) C12 0.066(7) 0.046(6) 0.062(7) 0.006(5) -0.028(6) -0.031(5) C13 0.067(7) 0.111(10) 0.046(6) 0.020(7) -0.022(5) -0.065(8) C14 0.046(5) 0.060(7) 0.059(7) -0.009(6) -0.024(5) -0.009(5) C15 0.064(6) 0.053(6) 0.043(6) 0.020(5) -0.022(5) -0.033(5) _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 C11 2.066(10) . ? Ni1 C13 2.069(11) . ? Ni1 C12 2.112(10) . ? Ni1 C14 2.121(10) . ? Ni1 S2 2.121(3) . ? Ni1 C15 2.129(9) . ? Ni1 S1 2.133(3) . ? S1 C1 1.734(9) . ? S2 C2 1.720(8) . ? S3 C1 1.773(9) . ? S3 C3 1.844(10) . ? S4 C2 1.760(9) . ? S4 C4 1.834(11) . ? C1 C2 1.353(13) . ? C3 C5 1.486(13) . ? C4 C6 1.495(12) . ? C5 C6 1.400(13) . ? C5 C10 1.422(12) . ? C6 C7 1.397(13) . ? C7 C8 1.362(13) . ? C8 C9 1.367(15) . ? C9 C10 1.380(14) . ? C11 C15 1.388(14) . ? C11 C12 1.394(16) . ? C12 C13 1.405(17) . ? C13 C14 1.436(17) . ? C14 C15 1.381(16) . ? 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 C11 Ni1 C13 65.7(5) . . ? C11 Ni1 C12 39.0(5) . . ? C13 Ni1 C12 39.3(5) . . ? C11 Ni1 C14 65.0(4) . . ? C13 Ni1 C14 40.1(5) . . ? C12 Ni1 C14 65.8(4) . . ? C11 Ni1 S2 167.0(3) . . ? C13 Ni1 S2 101.5(4) . . ? C12 Ni1 S2 129.1(4) . . ? C14 Ni1 S2 107.1(3) . . ? C11 Ni1 C15 38.6(4) . . ? C13 Ni1 C15 65.2(5) . . ? C12 Ni1 C15 64.8(4) . . ? C14 Ni1 C15 37.9(4) . . ? S2 Ni1 C15 139.7(3) . . ? C11 Ni1 S1 99.9(3) . . ? C13 Ni1 S1 158.4(4) . . ? C12 Ni1 S1 119.6(3) . . ? C14 Ni1 S1 150.0(4) . . ? S2 Ni1 S1 91.66(10) . . ? C15 Ni1 S1 114.3(3) . . ? C1 S1 Ni1 103.9(3) . . ? C2 S2 Ni1 105.0(3) . . ? C1 S3 C3 105.0(4) . . ? C2 S4 C4 104.6(5) . . ? C2 C1 S1 119.8(7) . . ? C2 C1 S3 125.9(7) . . ? S1 C1 S3 114.3(5) . . ? C1 C2 S2 119.1(7) . . ? C1 C2 S4 125.6(7) . . ? S2 C2 S4 115.0(5) . . ? C5 C3 S3 111.6(7) . . ? C6 C4 S4 111.6(6) . . ? C6 C5 C10 118.5(8) . . ? C6 C5 C3 123.8(7) . . ? C10 C5 C3 117.7(8) . . ? C7 C6 C5 118.5(8) . . ? C7 C6 C4 120.6(9) . . ? C5 C6 C4 120.7(8) . . ? C8 C7 C6 122.1(9) . . ? C7 C8 C9 120.1(9) . . ? C8 C9 C10 120.2(8) . . ? C9 C10 C5 120.6(9) . . ? C15 C11 C12 109.6(10) . . ? C15 C11 Ni1 73.1(6) . . ? C12 C11 Ni1 72.3(6) . . ? C11 C12 C13 106.5(10) . . ? C11 C12 Ni1 68.7(6) . . ? C13 C12 Ni1 68.7(6) . . ? C12 C13 C14 108.1(11) . . ? C12 C13 Ni1 72.1(6) . . ? C14 C13 Ni1 71.9(6) . . ? C15 C14 C13 106.9(10) . . ? C15 C14 Ni1 71.3(6) . . ? C13 C14 Ni1 68.0(6) . . ? C14 C15 C11 108.6(10) . . ? C14 C15 Ni1 70.7(6) . . ? C11 C15 Ni1 68.2(6) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.413 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.219