data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michel Fourmigue' 'Narcis Avarvari' _publ_contact_author_name 'Dr Marc Fourmigue' _publ_contact_author_address ; Laboratoire 'Chemie, Ingenierie Moleculaire et Materiaux d'Angers CNRS-Universite d'Angers 2 Bd. Lavoisier, UFR Sciences, Bat. ANGERS 49045 FRANCE ; _publ_contact_author_email MARC.FOURMIGUE@UNIV-ANGERS.FR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A Series of Neutral Radicalar CpNi(dithiolene) Complexes. ; data_mf297 _database_code_depnum_ccdc_archive 'CCDC 258291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CpNi(dmit) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H5 Ni S5' _chemical_formula_weight 320.13 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.9185(14) _cell_length_b 7.9334(12) _cell_length_c 11.732(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.86(3) _cell_angle_gamma 90.00 _cell_volume 545.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1974 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 24.95 _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 322 _exptl_absorpt_coefficient_mu 2.685 _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 0.7566 _exptl_absorpt_correction_T_max 0.7736 _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. 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 4152 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.1509 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.92 _reflns_number_total 1949 _reflns_number_gt 1101 _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^)+(0.0070P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1949 _refine_ls_number_parameters 127 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 0.737 _refine_ls_restrained_S_all 0.737 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.006 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 1.06087(17) 0.32550(16) 0.27132(8) 0.0353(3) Uani 1 1 d . . . S1 S 0.9379(3) 0.2449(3) 0.42552(17) 0.0427(6) Uani 1 1 d . . . S2 S 1.3751(4) 0.4247(3) 0.35771(16) 0.0439(6) Uani 1 1 d . . . S3 S 1.1649(3) 0.2596(3) 0.67272(15) 0.0404(6) Uani 1 1 d . . . S4 S 1.5663(3) 0.4188(3) 0.61119(17) 0.0420(6) Uani 1 1 d . . . S5 S 1.5475(3) 0.3315(5) 0.85683(14) 0.0503(6) Uani 1 1 d . . . C1 C 1.1642(11) 0.2955(12) 0.5273(5) 0.025(2) Uani 1 1 d . . . C2 C 1.3536(14) 0.3726(9) 0.5000(5) 0.030(3) Uani 1 1 d . . . C3 C 1.4312(13) 0.3360(19) 0.7200(6) 0.0383(19) Uani 1 1 d . . . C4 C 0.785(2) 0.244(2) 0.1556(9) 0.063(4) Uani 1 1 d . . . H4 H 0.6569 0.1952 0.1795 0.076 Uiso 1 1 calc R . . C5 C 0.813(2) 0.4101(19) 0.1388(9) 0.061(3) Uani 1 1 d . . . H5 H 0.7056 0.4935 0.1458 0.073 Uiso 1 1 calc R . . C6 C 1.034(3) 0.436(2) 0.1086(8) 0.099(6) Uani 1 1 d . . . H6 H 1.1039 0.5377 0.0941 0.119 Uiso 1 1 calc R . . C7 C 1.1253(19) 0.268(3) 0.1056(9) 0.079(5) Uani 1 1 d . . . H7 H 1.2692 0.2411 0.0876 0.095 Uiso 1 1 calc R . . C8 C 0.975(2) 0.1584(17) 0.1322(8) 0.064(3) Uani 1 1 d . . . H8 H 0.9934 0.0420 0.1348 0.077 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 0.0354(6) 0.0423(8) 0.0268(5) 0.0005(7) -0.0009(4) 0.0017(8) S1 0.0316(11) 0.0592(17) 0.0360(12) 0.0037(12) 0.0001(9) -0.0133(12) S2 0.0409(13) 0.0635(18) 0.0271(11) 0.0062(12) 0.0037(9) -0.0121(13) S3 0.0404(12) 0.0505(18) 0.0297(11) 0.0054(11) 0.0024(9) -0.0045(12) S4 0.0353(12) 0.0549(16) 0.0336(11) -0.0006(12) -0.0033(9) -0.0113(12) S5 0.0580(14) 0.0572(17) 0.0315(11) 0.0004(16) -0.0091(10) -0.0017(19) C1 0.023(4) 0.023(7) 0.030(4) 0.001(4) 0.007(3) 0.004(4) C2 0.052(5) 0.016(7) 0.021(4) 0.003(3) 0.004(3) -0.007(4) C3 0.033(4) 0.033(5) 0.048(4) -0.015(6) 0.003(3) 0.009(6) C4 0.041(7) 0.101(13) 0.045(6) -0.006(8) 0.000(5) -0.005(8) C5 0.086(9) 0.037(8) 0.049(7) 0.007(6) -0.030(6) 0.011(8) C6 0.174(16) 0.109(14) 0.006(5) 0.024(7) -0.020(7) -0.100(13) C7 0.043(6) 0.152(16) 0.040(6) -0.003(7) -0.003(4) 0.015(9) C8 0.073(9) 0.071(9) 0.040(6) -0.011(6) -0.020(6) -0.006(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 C4 2.077(11) . ? Ni1 C7 2.082(11) . ? Ni1 C5 2.096(10) . ? Ni1 C6 2.088(10) . ? Ni1 C8 2.110(11) . ? Ni1 S1 2.138(2) . ? Ni1 S2 2.143(2) . ? S1 C1 1.716(7) . ? S2 C2 1.741(7) . ? S3 C3 1.708(9) . ? S3 C1 1.729(7) . ? S4 C3 1.726(10) . ? S4 C2 1.724(7) . ? S5 C3 1.659(7) . ? C1 C2 1.354(8) . ? C4 C5 1.343(13) . ? C4 C8 1.371(16) . ? C5 C6 1.417(19) . ? C6 C7 1.442(17) . ? C7 C8 1.313(17) . ? 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 C4 Ni1 C7 63.2(4) . . ? C4 Ni1 C5 37.6(3) . . ? C7 Ni1 C5 64.9(5) . . ? C4 Ni1 C6 65.1(5) . . ? C7 Ni1 C6 40.5(5) . . ? C5 Ni1 C6 39.6(5) . . ? C4 Ni1 C8 38.2(4) . . ? C7 Ni1 C8 36.5(5) . . ? C5 Ni1 C8 63.7(5) . . ? C6 Ni1 C8 65.0(5) . . ? C4 Ni1 S1 97.6(3) . . ? C7 Ni1 S1 148.4(6) . . ? C5 Ni1 S1 116.0(4) . . ? C6 Ni1 S1 155.2(6) . . ? C8 Ni1 S1 113.1(4) . . ? C4 Ni1 S2 167.6(3) . . ? C7 Ni1 S2 105.3(4) . . ? C5 Ni1 S2 135.0(4) . . ? C6 Ni1 S2 103.3(4) . . ? C8 Ni1 S2 134.3(4) . . ? S1 Ni1 S2 94.79(9) . . ? C1 S1 Ni1 101.3(3) . . ? C2 S2 Ni1 101.2(3) . . ? C3 S3 C1 98.0(4) . . ? C3 S4 C2 96.6(4) . . ? C2 C1 S1 122.3(5) . . ? C2 C1 S3 114.7(5) . . ? S1 C1 S3 123.0(4) . . ? C1 C2 S4 117.3(5) . . ? C1 C2 S2 120.4(5) . . ? S4 C2 S2 122.3(5) . . ? S5 C3 S3 123.3(6) . . ? S5 C3 S4 123.4(6) . . ? S3 C3 S4 113.3(4) . . ? C5 C4 C8 109.7(14) . . ? C5 C4 Ni1 72.0(8) . . ? C8 C4 Ni1 72.2(6) . . ? C4 C5 C6 108.5(14) . . ? C4 C5 Ni1 70.4(7) . . ? C6 C5 Ni1 69.9(6) . . ? C5 C6 C7 103.4(12) . . ? C5 C6 Ni1 70.5(6) . . ? C7 C6 Ni1 69.5(7) . . ? C8 C7 C6 109.8(12) . . ? C8 C7 Ni1 72.9(7) . . ? C6 C7 Ni1 70.0(7) . . ? C7 C8 C4 108.6(15) . . ? C7 C8 Ni1 70.6(7) . . ? C4 C8 Ni1 69.6(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.391 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.095 #===END data_mf344fac _database_code_depnum_ccdc_archive 'CCDC 258292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CpNi(dsit) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H5 Ni S3 Se2' _chemical_formula_weight 413.93 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.0750(12) _cell_length_b 7.9798(11) _cell_length_c 11.8369(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.55(2) _cell_angle_gamma 90.00 _cell_volume 568.85(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3386 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.55 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.0076 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 8.607 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1444 _exptl_absorpt_correction_T_max 0.9033 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _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. 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 4282 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.1053 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.85 _reflns_number_total 2090 _reflns_number_gt 1475 _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^)+(0.0283P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 2090 _refine_ls_number_parameters 127 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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 Ni Ni -0.06424(18) 0.69392(15) 0.73183(9) 0.0328(3) Uani 1 1 d . . . Se1 Se 0.06801(15) 0.77625(14) 0.57184(8) 0.0392(3) Uani 1 1 d . . . Se2 Se -0.38571(15) 0.58984(14) 0.64348(8) 0.0407(3) Uani 1 1 d . . . S1 S -0.1705(4) 0.7589(3) 0.3204(2) 0.0384(6) Uani 1 1 d . . . S2 S -0.5665(4) 0.6020(4) 0.3806(2) 0.0408(6) Uani 1 1 d . . . S3 S -0.5423(4) 0.6870(4) 0.1366(2) 0.0536(7) Uani 1 1 d . . . C1 C -0.1736(13) 0.7223(11) 0.4643(7) 0.029(2) Uani 1 1 d . . . C2 C -0.3615(15) 0.6507(11) 0.4930(8) 0.030(2) Uani 1 1 d . . . C3 C -0.4299(15) 0.6843(14) 0.2743(8) 0.039(2) Uani 1 1 d . . . C4 C 0.1973(18) 0.777(2) 0.8494(9) 0.058(3) Uani 1 1 d . . . H4 H 0.3249 0.8276 0.8299 0.069 Uiso 1 1 calc R . . C5 C 0.1796(19) 0.6081(19) 0.8623(9) 0.056(3) Uani 1 1 d . . . H5 H 0.2883 0.5288 0.8535 0.067 Uiso 1 1 calc R . . C6 C -0.028(3) 0.577(3) 0.8906(10) 0.107(7) Uani 1 1 d . . . H6 H -0.0915 0.4734 0.9038 0.128 Uiso 1 1 calc R . . C7 C -0.130(2) 0.747(3) 0.8951(9) 0.089(6) Uani 1 1 d . . . H7 H -0.2711 0.7701 0.9141 0.107 Uiso 1 1 calc R . . C8 C 0.018(3) 0.8633(19) 0.8669(11) 0.073(4) Uani 1 1 d . . . H8 H -0.0022 0.9787 0.8611 0.088 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 Ni 0.0347(6) 0.0418(7) 0.0210(7) -0.0028(6) -0.0004(5) -0.0002(6) Se1 0.0321(5) 0.0565(6) 0.0280(6) 0.0021(5) 0.0000(4) -0.0116(5) Se2 0.0378(5) 0.0577(6) 0.0264(5) 0.0059(5) 0.0037(4) -0.0123(5) S1 0.0394(12) 0.0511(16) 0.0249(13) 0.0053(13) 0.0053(10) -0.0062(13) S2 0.0391(12) 0.0527(17) 0.0286(14) -0.0025(14) -0.0025(10) -0.0108(14) S3 0.0623(16) 0.0700(18) 0.0250(14) 0.0015(15) -0.0069(12) -0.0032(16) C1 0.030(4) 0.031(6) 0.025(5) 0.003(4) 0.001(4) 0.004(4) C2 0.038(5) 0.037(6) 0.014(4) 0.000(4) 0.004(4) -0.001(4) C3 0.047(5) 0.040(5) 0.030(5) -0.006(5) 0.001(4) 0.010(5) C4 0.045(6) 0.090(10) 0.033(6) 0.002(8) -0.014(5) -0.012(8) C5 0.069(7) 0.056(8) 0.036(6) 0.006(7) -0.015(6) 0.014(7) C6 0.168(18) 0.122(15) 0.022(7) 0.019(9) -0.021(9) -0.091(15) C7 0.055(7) 0.20(2) 0.012(5) -0.014(9) 0.008(5) 0.017(11) C8 0.088(10) 0.082(10) 0.043(8) -0.018(7) -0.022(7) 0.021(9) _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 C7 2.070(11) . ? Ni C4 2.078(11) . ? Ni C6 2.085(13) . ? Ni C8 2.103(13) . ? Ni C5 2.109(10) . ? Ni Se2 2.2496(15) . ? Ni Se1 2.2502(15) . ? Se1 C1 1.862(8) . ? Se2 C2 1.871(9) . ? S1 C3 1.706(10) . ? S1 C1 1.731(9) . ? S2 C3 1.726(10) . ? S2 C2 1.743(9) . ? S3 C3 1.683(10) . ? C1 C2 1.360(11) . ? C4 C8 1.329(17) . ? C4 C5 1.361(16) . ? C5 C6 1.372(19) . ? C6 C7 1.50(2) . ? C7 C8 1.36(2) . ? 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 C7 Ni C4 62.2(5) . . ? C7 Ni C6 42.3(6) . . ? C4 Ni C6 63.9(5) . . ? C7 Ni C8 38.1(6) . . ? C4 Ni C8 37.1(5) . . ? C6 Ni C8 67.5(6) . . ? C7 Ni C5 65.6(5) . . ? C4 Ni C5 37.9(4) . . ? C6 Ni C5 38.2(5) . . ? C8 Ni C5 65.1(5) . . ? C7 Ni Se2 104.3(4) . . ? C4 Ni Se2 165.8(3) . . ? C6 Ni Se2 103.6(4) . . ? C8 Ni Se2 134.1(4) . . ? C5 Ni Se2 134.7(4) . . ? C7 Ni Se1 149.4(7) . . ? C4 Ni Se1 98.3(3) . . ? C6 Ni Se1 152.0(6) . . ? C8 Ni Se1 112.1(5) . . ? C5 Ni Se1 114.6(4) . . ? Se2 Ni Se1 95.78(5) . . ? C1 Se1 Ni 99.9(3) . . ? C2 Se2 Ni 100.1(3) . . ? C3 S1 C1 97.3(4) . . ? C3 S2 C2 96.2(4) . . ? C2 C1 S1 115.8(7) . . ? C2 C1 Se1 122.6(7) . . ? S1 C1 Se1 121.6(5) . . ? C1 C2 S2 116.2(7) . . ? C1 C2 Se2 121.4(7) . . ? S2 C2 Se2 122.1(5) . . ? S3 C3 S1 123.1(6) . . ? S3 C3 S2 122.6(6) . . ? S1 C3 S2 114.3(5) . . ? C8 C4 C5 114.7(13) . . ? C8 C4 Ni 72.5(7) . . ? C5 C4 Ni 72.3(7) . . ? C4 C5 C6 107.3(14) . . ? C4 C5 Ni 69.8(7) . . ? C6 C5 Ni 70.0(7) . . ? C5 C6 C7 103.9(13) . . ? C5 C6 Ni 71.8(7) . . ? C7 C6 Ni 68.3(7) . . ? C8 C7 C6 108.6(12) . . ? C8 C7 Ni 72.3(7) . . ? C6 C7 Ni 69.4(7) . . ? C4 C8 C7 105.5(15) . . ? C4 C8 Ni 70.4(7) . . ? C7 C8 Ni 69.6(8) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.533 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.119 #===END data_mf308 _database_code_depnum_ccdc_archive 'CCDC 258293' _audit_creation_date 2003-02-25T18:17:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_name_common CpNi(dmid) _chemical_melting_point ? _chemical_formula_moiety 'C8 H5 Ni1 O1 S4' _chemical_formula_sum 'C8 H5 Ni O S4' _chemical_formula_weight 304.07 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 8.0485(7) _cell_length_b 7.2993(7) _cell_length_c 17.7872(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1044.97(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4442 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.7 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5384 _exptl_absorpt_correction_T_max 0.6005 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _diffrn_measurement_device_type Stoe-IPDS _diffrn_measurement_method 'oscillation, phi incr. 1.3 deg.' _diffrn_detector_area_resol_mean 6.66 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_reflns_number 5997 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 1075 _reflns_number_gt 823 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1075 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0615 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.007 _refine_diff_density_max 0.573 _refine_diff_density_min -0.292 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Ni1 Ni 0.17565(6) 0.25 0.60354(2) 0.03973(16) Uani 1 d S . . S2 S 0.44164(11) 0.25 0.59577(4) 0.0408(2) Uani 1 d S . . S4 S 0.66480(11) 0.25 0.45936(5) 0.0474(3) Uani 1 d S . . S1 S 0.13595(11) 0.25 0.48470(5) 0.0478(3) Uani 1 d S . . S3 S 0.37782(13) 0.25 0.35616(5) 0.0468(3) Uani 1 d S . . O1 O 0.6889(4) 0.25 0.31141(16) 0.0657(9) Uani 1 d S . . C1 C 0.3365(4) 0.25 0.45268(17) 0.0349(8) Uani 1 d S . . C2 C 0.4681(4) 0.25 0.49994(17) 0.0326(8) Uani 1 d S . . C3 C 0.5973(5) 0.25 0.3647(2) 0.0443(9) Uani 1 d S . . C4 C 0.1426(8) 0.1637(18) 0.7170(4) 0.055(3) Uani 0.5 d PG . . H4 H 0.2244 0.113 0.7475 0.066 Uiso 0.5 calc PR . . C5 C 0.0307(8) 0.0670(9) 0.6727(5) 0.039(2) Uani 0.5 d PG . . H5 H 0.0243 -0.0598 0.6684 0.047 Uiso 0.5 calc PR . . C6 C -0.0702(5) 0.1929(7) 0.6360(3) 0.065(5) Uani 0.5 d PG . . H6 H -0.1559 0.1653 0.6028 0.078 Uiso 0.5 calc PR . . C7 C -0.0205(11) 0.3674(12) 0.6576(6) 0.076(4) Uani 0.5 d PG . . H7 H -0.0672 0.4771 0.6414 0.091 Uiso 0.5 calc PR . . C8 C 0.1110(9) 0.349(2) 0.7076(4) 0.076(5) Uani 0.5 d PG . . H8 H 0.1678 0.4448 0.7308 0.092 Uiso 0.5 calc PR . . 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 0.0348(3) 0.0560(3) 0.0284(2) 0 0.00290(18) 0 S2 0.0359(4) 0.0567(6) 0.0297(4) 0 -0.0049(4) 0 S4 0.0334(4) 0.0596(6) 0.0492(5) 0 0.0061(4) 0 S1 0.0318(5) 0.0804(8) 0.0311(4) 0 -0.0032(4) 0 S3 0.0541(5) 0.0591(6) 0.0272(4) 0 0.0022(4) 0 O1 0.071(2) 0.072(2) 0.0543(17) 0 0.0327(15) 0 C1 0.0357(17) 0.0397(19) 0.0292(16) 0 0.0012(14) 0 C2 0.0289(16) 0.036(2) 0.0327(16) 0 -0.0002(14) 0 C3 0.051(2) 0.036(2) 0.046(2) 0 0.0149(18) 0 C4 0.048(4) 0.082(8) 0.035(4) 0.003(4) -0.007(4) -0.014(4) C5 0.037(5) 0.047(5) 0.033(3) 0.004(4) 0.003(3) -0.001(3) C6 0.029(3) 0.118(16) 0.047(3) 0.020(4) 0.006(2) 0.018(3) C7 0.063(8) 0.062(7) 0.103(11) 0.035(8) 0.050(7) 0.030(8) C8 0.109(10) 0.080(9) 0.040(6) -0.023(5) 0.041(6) -0.031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C7 2.038(4) 8_565 ? Ni1 C7 2.038(9) . ? Ni1 C8 2.055(6) . ? Ni1 C8 2.055(9) 8_565 ? Ni1 C6 2.103(4) . ? Ni1 C6 2.103(8) 8_565 ? Ni1 S1 2.1379(10) . ? Ni1 S2 2.1453(10) . ? Ni1 C4 2.130(6) 8_565 ? Ni1 C4 2.130(6) . ? Ni1 C5 2.159(12) 8_565 ? Ni1 C5 2.159(8) . ? S2 C2 1.718(3) . ? S4 C2 1.740(3) . ? S4 C3 1.770(4) . ? S1 C1 1.712(3) . ? S3 C1 1.749(3) . ? S3 C3 1.773(4) . ? O1 C3 1.200(4) . ? C1 C2 1.352(4) . ? C4 C5 1.389(4) . ? C4 C8 1.389(4) . ? C5 C6 1.389(4) . ? C6 C7 1.389(4) . ? C7 C8 1.389(4) . ? 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 C7 Ni1 C7 49.7(3) 8_565 . ? C7 Ni1 C8 61.8(3) 8_565 . ? C7 Ni1 C8 39.67(14) . . ? C7 Ni1 C8 39.67(14) 8_565 8_565 ? C7 Ni1 C8 61.8(5) . 8_565 ? C8 Ni1 C8 41.3(7) . 8_565 ? C7 Ni1 C6 19.6(2) 8_565 . ? C7 Ni1 C6 39.16(13) . . ? C8 Ni1 C6 65.42(18) . . ? C8 Ni1 C6 56.24(19) 8_565 . ? C7 Ni1 C6 39.16(15) 8_565 8_565 ? C7 Ni1 C6 19.6(3) . 8_565 ? C8 Ni1 C6 56.2(2) . 8_565 ? C8 Ni1 C6 65.4(3) 8_565 8_565 ? C6 Ni1 C6 22.9(3) . 8_565 ? C7 Ni1 S1 110.54(11) 8_565 . ? C7 Ni1 S1 110.5(3) . . ? C8 Ni1 S1 148.5(3) . . ? C8 Ni1 S1 148.52(16) 8_565 . ? C6 Ni1 S1 97.53(13) . . ? C6 Ni1 S1 97.5(2) 8_565 . ? C7 Ni1 S2 143.48(15) 8_565 . ? C7 Ni1 S2 143.5(2) . . ? C8 Ni1 S2 108.11(19) . . ? C8 Ni1 S2 108.11(18) 8_565 . ? C6 Ni1 S2 163.06(12) . . ? C6 Ni1 S2 163.1(2) 8_565 . ? S1 Ni1 S2 94.90(4) . . ? C7 Ni1 C4 65.2(2) 8_565 8_565 ? C7 Ni1 C4 48.1(4) . 8_565 ? C8 Ni1 C4 8.5(5) . 8_565 ? C8 Ni1 C4 38.71(14) 8_565 8_565 ? C6 Ni1 C4 71.39(16) . 8_565 ? C6 Ni1 C4 64.1(3) 8_565 8_565 ? S1 Ni1 C4 156.6(3) . 8_565 ? S2 Ni1 C4 100.70(17) . 8_565 ? C7 Ni1 C4 48.08(19) 8_565 . ? C7 Ni1 C4 65.21(17) . . ? C8 Ni1 C4 38.71(12) . . ? C8 Ni1 C4 8.5(3) 8_565 . ? C6 Ni1 C4 64.1(2) . . ? C6 Ni1 C4 71.39(16) 8_565 . ? S1 Ni1 C4 156.6(3) . . ? S2 Ni1 C4 100.70(17) . . ? C4 Ni1 C4 34.4(7) 8_565 . ? C7 Ni1 C5 64.7(3) 8_565 8_565 ? C7 Ni1 C5 18.5(3) . 8_565 ? C8 Ni1 C5 29.7(3) . 8_565 ? C8 Ni1 C5 64.4(3) 8_565 8_565 ? C6 Ni1 C5 57.1(4) . 8_565 ? C6 Ni1 C5 38.0(2) 8_565 8_565 ? S1 Ni1 C5 118.9(3) . 8_565 ? S2 Ni1 C5 125.2(4) . 8_565 ? C4 Ni1 C5 37.8(5) 8_565 8_565 ? C4 Ni1 C5 64.9(3) . 8_565 ? C7 Ni1 C5 18.54(18) 8_565 . ? C7 Ni1 C5 64.69(19) . . ? C8 Ni1 C5 64.4(2) . . ? C8 Ni1 C5 29.7(3) 8_565 . ? C6 Ni1 C5 38.02(14) . . ? C6 Ni1 C5 57.1(2) 8_565 . ? S1 Ni1 C5 118.9(2) . . ? S2 Ni1 C5 125.18(12) . . ? C4 Ni1 C5 64.9(5) 8_565 . ? C4 Ni1 C5 37.79(17) . . ? C5 Ni1 C5 76.5(4) 8_565 . ? C2 S2 Ni1 100.81(11) . . ? C2 S4 C3 96.63(16) . . ? C1 S1 Ni1 100.84(11) . . ? C1 S3 C3 96.06(17) . . ? C2 C1 S1 122.1(3) . . ? C2 C1 S3 117.5(2) . . ? S1 C1 S3 120.39(19) . . ? C1 C2 S2 121.3(3) . . ? C1 C2 S4 117.1(2) . . ? S2 C2 S4 121.63(19) . . ? O1 C3 S4 124.2(3) . . ? O1 C3 S3 123.0(3) . . ? S4 C3 S3 112.78(19) . . ? C5 C4 C8 108 . . ? C5 C4 Ni1 72.2(2) . . ? C8 C4 Ni1 67.7(4) . . ? C4 C5 C6 108 . . ? C4 C5 Ni1 70.00(16) . . ? C6 C5 Ni1 68.8(3) . . ? C7 C6 C5 108 . . ? C7 C6 Ni1 67.9(3) . . ? C5 C6 Ni1 73.2(4) . . ? C8 C7 C6 108 . . ? C8 C7 Ni1 70.8(2) . . ? C6 C7 Ni1 72.9(3) . . ? C7 C8 C4 108 . . ? C7 C8 Ni1 69.5(3) . . ? C4 C8 Ni1 73.6(4) . . ?