# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2246 data_global _publ_contact_author ; Prof. Paola Deplano Dipartimento di Chimica Inorganica ed Analitica Cittadella Universitaria di Monserrato Universit\`a degli Studi di Cagliari 090042 Monserrato, Cagliari Italy ; _publ_contact_letter ; Date July 26, 2000 Re: Paper to be submitted to J. Chem. Soc. Dalton Trans. we are sending you the CIF files of the structure inserted in the paper submitted Yours Sincerely Paola Deplano ; _publ_contact_author_phone '[int.code]039(0)70 6754680' _publ_contact_author_fax '[int.code]039(0)70 6754499' _publ_contact_author_email 'deplano@vaxca1.unica.it' _publ_requested_journal ' J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ' ' _publ_section_title ; Synthesis, Structure and Properties of New Unsymmetrical Nickel Dithiolenes. ; _publ_author_name ; Francesco Bigoli Patrick Cassoux Paola Deplano Maria Laura Mercuri Maria Angela Pellinghelli Gloria Pintus Angela Serpe Emanuele F. Trogu ; _publ_author_address ; 'Prof. Paola Deplano' Dipartimento di Chimica Inorganica ed Analitica Cittadella Universitaria di Monserrato Universit\`a degli Studi di Cagliari 090042 Monserrato, Cagliari Italy ; #-------------------------- data section of block --------------------------- #=BEGIN data_[Ni(dmit)(Pri2timdt)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 N2 Ni S8' _chemical_formula_weight 501.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 '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' _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 16.723(5) _cell_length_b 17.039(5) _cell_length_c 7.124(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.36(2) _cell_angle_gamma 90.00 _cell_volume 1983(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 18 _cell_measurement_theta_max 40 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 9.270 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 4046 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 00 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 00 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 69.99 _reflns_number_total 3743 _reflns_number_gt 1796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _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 w=1/[\s^2^(Fo^2^)+(0.1487P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3743 _refine_ls_number_parameters 214 _refine_ls_number_restraints 00 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.25302(5) 0.12539(5) 0.12655(15) 0.0621(3) Uani 1 d . . . S1 S 0.15758(9) 0.38734(8) 0.0788(2) 0.0689(4) Uani 1 d . . . S2 S 0.33437(9) 0.39150(8) 0.1669(2) 0.0695(4) Uani 1 d . . . S3 S 0.15537(8) 0.20978(7) 0.0773(2) 0.0664(4) Uani 1 d . . . S4 S 0.34673(8) 0.21363(7) 0.1735(2) 0.0641(4) Uani 1 d . . . S5 S 0.24263(10) 0.54230(9) 0.1208(3) 0.0848(5) Uani 1 d . . . S6 S 0.15655(8) 0.03754(8) 0.0782(2) 0.0664(4) Uani 1 d . . . S7 S 0.35053(8) 0.03854(8) 0.1749(2) 0.0653(4) Uani 1 d . . . S8 S 0.25489(9) -0.26771(9) 0.1276(3) 0.0784(4) Uani 1 d . . . N1 N 0.1857(3) -0.1227(2) 0.0935(7) 0.0608(11) Uani 1 d . . . N2 N 0.3230(2) -0.1226(2) 0.1618(6) 0.0600(11) Uani 1 d . . . C1 C 0.2092(4) 0.2977(3) 0.1041(8) 0.0650(13) Uani 1 d . . . C2 C 0.2881(4) 0.2996(3) 0.1438(7) 0.0596(13) Uani 1 d . . . C3 C 0.2453(3) 0.4480(3) 0.1216(7) 0.0599(12) Uani 1 d . . . C4 C 0.2119(3) -0.0465(3) 0.1052(8) 0.0612(13) Uani 1 d . . . C5 C 0.2961(3) -0.0462(3) 0.1492(8) 0.0579(12) Uani 1 d . . . C6 C 0.2541(3) -0.1708(3) 0.1270(8) 0.0649(13) Uani 1 d . . . C7 C 0.1005(3) -0.1520(4) 0.0493(9) 0.0730(16) Uani 1 d . . . H7 H 0.1036 -0.2094 0.0510 0.14(2) Uiso 1 calc R . . C8 C 0.0578(4) -0.1285(4) 0.2077(10) 0.088(2) Uani 1 d . . . H8A H 0.0918 -0.1418 0.3300 0.116(7) Uiso 1 calc R . . H8B H 0.0066 -0.1558 0.1915 0.116(7) Uiso 1 calc R . . H8C H 0.0480 -0.0729 0.2020 0.116(7) Uiso 1 calc R . . C9 C 0.0575(4) -0.1288(4) -0.1508(9) 0.0852(19) Uani 1 d . . . H9A H 0.0465 -0.0735 -0.1544 0.116(7) Uiso 1 calc R . . H9B H 0.0070 -0.1571 -0.1865 0.116(7) Uiso 1 calc R . . H9C H 0.0918 -0.1410 -0.2391 0.116(7) Uiso 1 calc R . . C10 C 0.4087(3) -0.1514(4) 0.2051(10) 0.0789(17) Uani 1 d . . . H10 H 0.4057 -0.2088 0.2035 0.14(2) Uiso 1 calc R . . C11 C 0.4508(4) -0.1287(4) 0.4024(10) 0.094(2) Uani 1 d . . . H11A H 0.5007 -0.1580 0.4393 0.116(7) Uiso 1 calc R . . H11B H 0.4159 -0.1399 0.4899 0.116(7) Uiso 1 calc R . . H11C H 0.4630 -0.0736 0.4057 0.116(7) Uiso 1 calc R . . C12 C 0.4507(4) -0.1285(4) 0.0482(10) 0.096(2) Uani 1 d . . . H12A H 0.4161 -0.1407 -0.0741 0.116(7) Uiso 1 calc R . . H12B H 0.5012 -0.1569 0.0625 0.116(7) Uiso 1 calc R . . H12C H 0.4618 -0.0732 0.0553 0.116(7) Uiso 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 0.0650(6) 0.0558(6) 0.0649(6) -0.0001(4) 0.0127(4) -0.0004(4) S1 0.0688(8) 0.0594(8) 0.0773(10) 0.0018(7) 0.0133(7) 0.0037(6) S2 0.0722(9) 0.0596(8) 0.0758(10) -0.0024(7) 0.0140(7) -0.0082(6) S3 0.0626(8) 0.0547(8) 0.0810(10) -0.0008(6) 0.0134(7) -0.0047(5) S4 0.0621(8) 0.0564(8) 0.0730(9) 0.0008(6) 0.0126(7) 0.0006(5) S5 0.1086(13) 0.0538(8) 0.0918(11) -0.0005(9) 0.0210(10) 0.0002(8) S6 0.0588(7) 0.0580(8) 0.0808(10) 0.0005(6) 0.0115(7) 0.0027(5) S7 0.0588(7) 0.0595(8) 0.0765(10) -0.0024(6) 0.0121(6) -0.0060(5) S8 0.0773(10) 0.0584(8) 0.0978(11) -0.0002(10) 0.0148(8) -0.0020(7) N1 0.053(2) 0.055(3) 0.073(3) 0.001(2) 0.011(2) -0.0020(19) N2 0.051(2) 0.054(2) 0.074(3) -0.002(2) 0.012(2) 0.0035(18) C1 0.079(4) 0.059(3) 0.059(3) 0.006(2) 0.018(3) 0.009(3) C2 0.087(4) 0.050(3) 0.045(3) 00.000(2) 0.020(3) 0.001(2) C3 0.087(4) 0.048(3) 0.045(3) 0.001(2) 0.015(2) 0.000(3) C4 0.068(3) 0.061(3) 0.055(3) -0.001(2) 0.015(2) -0.007(2) C5 0.064(3) 0.050(3) 0.058(3) 0.000(2) 0.012(2) 0.001(2) C6 0.063(3) 0.057(3) 0.073(3) 0.000(3) 0.010(3) 0.004(2) C7 0.057(3) 0.072(4) 0.089(4) -0.002(3) 0.013(3) -0.019(3) C8 0.065(3) 0.116(6) 0.087(5) 0.012(4) 0.021(3) -0.015(3) C9 0.069(4) 0.107(5) 0.074(4) -0.014(4) 0.004(3) -0.012(3) C10 0.041(3) 0.082(4) 0.111(5) 0.002(4) 0.009(3) 0.010(2) C11 0.063(3) 0.123(6) 0.093(5) 0.020(4) 0.007(3) 0.012(3) C12 0.067(4) 0.124(6) 0.101(6) -0.023(4) 0.026(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S4 2.1457(16) . ? Ni S3 2.1476(16) . ? Ni S6 2.1734(17) . ? Ni S7 2.1741(17) . ? S1 C1 1.744(5) . ? S1 C3 1.766(5) . ? S2 C2 1.739(5) . ? S2 C3 1.745(5) . ? S3 C1 1.737(6) . ? S4 C2 1.751(5) . ? S5 C3 1.607(5) . ? S6 C4 1.693(6) . ? S7 C5 1.695(5) . ? S8 C6 1.651(6) . ? N1 C4 1.367(6) . ? N1 C6 1.387(6) . ? N1 C7 1.479(6) . ? N2 C5 1.375(6) . ? N2 C6 1.393(6) . ? N2 C10 1.483(6) . ? C1 C2 1.289(8) . ? C4 C5 1.377(7) . ? C7 C9 1.505(8) . ? C7 C8 1.513(8) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.482(9) . ? C10 C12 1.493(9) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 Ni S3 93.48(6) . . ? S4 Ni S6 179.04(7) . . ? S3 Ni S6 85.56(6) . . ? S4 Ni S7 87.37(6) . . ? S3 Ni S7 179.13(7) . . ? S6 Ni S7 93.58(6) . . ? C1 S1 C3 96.9(3) . . ? C2 S2 C3 97.7(3) . . ? C1 S3 Ni 101.63(19) . . ? C2 S4 Ni 101.30(19) . . ? C4 S6 Ni 101.26(19) . . ? C5 S7 Ni 101.28(18) . . ? C4 N1 C6 108.0(4) . . ? C4 N1 C7 128.0(5) . . ? C6 N1 C7 124.0(4) . . ? C5 N2 C6 107.5(4) . . ? C5 N2 C10 127.9(5) . . ? C6 N2 C10 124.6(4) . . ? C2 C1 S3 121.8(4) . . ? C2 C1 S1 117.5(4) . . ? S3 C1 S1 120.7(4) . . ? C1 C2 S2 117.2(4) . . ? C1 C2 S4 121.7(4) . . ? S2 C2 S4 121.0(3) . . ? S5 C3 S2 125.0(3) . . ? S5 C3 S1 124.3(3) . . ? S2 C3 S1 110.7(3) . . ? N1 C4 C5 108.4(5) . . ? N1 C4 S6 129.5(4) . . ? C5 C4 S6 122.1(4) . . ? N2 C5 C4 108.4(4) . . ? N2 C5 S7 129.8(4) . . ? C4 C5 S7 121.8(4) . . ? N1 C6 N2 107.6(4) . . ? N1 C6 S8 126.7(4) . . ? N2 C6 S8 125.7(4) . . ? N1 C7 C9 110.8(5) . . ? N1 C7 C8 109.8(5) . . ? C9 C7 C8 115.6(5) . . ? N1 C7 H7 106.7 . . ? C9 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N2 110.7(5) . . ? C11 C10 C12 116.0(5) . . ? N2 C10 C12 110.3(5) . . ? C11 C10 H10 106.5 . . ? N2 C10 H10 106.5 . . ? C12 C10 H10 106.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.961 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.106 #===END