Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_contact_author_name 'Prof Gaetano Verani' _publ_contact_author_address ; Prof Gaetano Verani Dipartimento di Chimica Inorganica ed Analitica Cittadella Universitaria S.P. per Sestu Km 0.700 09042 Monserrato Cagliari ITALY ; _publ_contact_author_email 'VERANI@UNICA.IT' #-------------------------------------- # Publication details loop_ _publ_author_name 'Aragoni, M. C.' 'Arca, M.' 'Demartin, F.' 'Devillanova, F. A.' 'Graiff, C.' 'Isaia, F.' 'Lippolis, V.' 'Tiripicchio, A.' 'Verani, G.' _journal_name_full 'Journal of Chemical Society, Dalton Transactions' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2001' _publ_section_title ; Reactivity of phosphonodithioate Ni(II) complexes: solution equilibria, solid state study, and theoretical calculations on the adduct formation with some pyridine derivatives ; #-------------------------------------- #Data for compound (10) data_g24bh _database_code_CSD 157796 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 N4 Ni O4 P2 S4' _chemical_formula_weight 713.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' -3.0029 0.5091 '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' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.266(5) _cell_length_b 10.992(5) _cell_length_c 8.302(4) _cell_angle_alpha 85.410(4) _cell_angle_beta 73.060(5) _cell_angle_gamma 64.180(3) _cell_volume 805.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 370 _exptl_absorpt_coefficient_mu 4.552 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _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 'Enraf Nonius CAD 4' _diffrn_measurement_method '\q/2\q scan method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2964 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 69.99 _reflns_number_total 2964 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0716P)^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 2964 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.185 _refine_ls_shift/su_mean 0.009 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.5000 1.0000 0.0428(2) Uani 1 2 d S . . S1 S 0.26335(9) 0.71360(8) 1.08550(10) 0.0474(2) Uani 1 1 d . . . S2 S 0.51875(10) 0.60540(9) 0.71874(10) 0.0528(2) Uani 1 1 d . . . P1 P 0.32291(10) 0.75236(9) 0.84240(11) 0.0470(2) Uani 1 1 d . . . O1 O 0.3256(3) 0.8977(2) 0.8262(3) 0.0610(7) Uani 1 1 d . . . O2 O -0.1646(3) 0.8619(3) 0.5245(4) 0.0775(8) Uani 1 1 d . . . N1 N 0.6236(3) 0.5919(3) 1.0586(3) 0.0458(6) Uani 1 1 d . . . N2 N 0.8970(5) 0.7392(4) 1.1823(6) 0.0764(11) Uani 1 1 d . . . C1 C 0.1770(4) 0.7872(3) 0.7446(4) 0.0499(8) Uani 1 1 d . . . C2 C 0.0501(4) 0.9101(4) 0.7758(5) 0.0571(9) Uani 1 1 d . . . C3 C -0.0651(5) 0.9390(4) 0.7046(5) 0.0609(9) Uani 1 1 d . . . C4 C -0.0545(4) 0.8423(4) 0.5988(4) 0.0575(9) Uani 1 1 d . . . C5 C 0.0709(5) 0.7196(4) 0.5649(5) 0.0642(10) Uani 1 1 d . . . C6 C 0.1866(5) 0.6912(4) 0.6349(5) 0.0577(9) Uani 1 1 d . . . C7 C -0.2946(6) 0.9889(6) 0.5569(7) 0.0841(15) Uani 1 1 d . . . C8 C 0.4180(7) 0.9246(5) 0.9050(7) 0.0769(13) Uani 1 1 d . . . C9 C 0.7504(4) 0.5882(3) 0.9469(4) 0.0482(7) Uani 1 1 d . . . C10 C 0.8413(4) 0.6369(4) 0.9809(5) 0.0530(8) Uani 1 1 d . . . C11 C 0.8066(4) 0.6927(3) 1.1422(5) 0.0516(8) Uani 1 1 d . . . C12 C 0.6747(4) 0.6988(4) 1.2591(5) 0.0522(8) Uani 1 1 d . . . C13 C 0.5892(4) 0.6484(3) 1.2120(4) 0.0478(7) Uani 1 1 d . . . H1N H 0.988(6) 0.725(5) 1.106(6) 0.090(16) Uiso 1 1 d . . . H2N H 0.875(5) 0.769(5) 1.286(6) 0.084(16) Uiso 1 1 d . . . H2 H 0.045(4) 0.971(4) 0.856(5) 0.070(12) Uiso 1 1 d . . . H3 H -0.146(5) 1.026(4) 0.728(5) 0.081(13) Uiso 1 1 d . . . H5 H 0.079(5) 0.652(5) 0.489(6) 0.087(14) Uiso 1 1 d . . . H6 H 0.270(4) 0.613(4) 0.613(5) 0.056(10) Uiso 1 1 d . . . H9 H 0.770(4) 0.550(3) 0.840(5) 0.054(10) Uiso 1 1 d . . . H10 H 0.925(4) 0.628(4) 0.906(5) 0.064(12) Uiso 1 1 d . . . H12 H 0.646(4) 0.731(4) 1.365(5) 0.054(10) Uiso 1 1 d . . . H13 H 0.503(4) 0.648(3) 1.289(4) 0.054(10) Uiso 1 1 d . . . H71 H -0.262(7) 1.077(7) 0.507(8) 0.16(3) Uiso 1 1 d . . . H72 H -0.347(6) 0.995(6) 0.688(8) 0.13(2) Uiso 1 1 d . . . H73 H -0.347(6) 0.984(5) 0.491(6) 0.093(16) Uiso 1 1 d . . . H81 H 0.393(6) 1.019(6) 0.899(6) 0.107(17) Uiso 1 1 d . . . H82 H 0.532(7) 0.870(6) 0.830(7) 0.12(2) Uiso 1 1 d . . . H83 H 0.411(7) 0.891(6) 1.010(8) 0.13(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0438(4) 0.0462(4) 0.0407(4) 0.0017(3) -0.0110(3) -0.0221(3) S1 0.0469(5) 0.0497(4) 0.0431(4) -0.0004(3) -0.0105(3) -0.0197(4) S2 0.0531(5) 0.0629(5) 0.0415(4) 0.0038(4) -0.0099(4) -0.0268(4) P1 0.0547(5) 0.0463(4) 0.0451(4) 0.0053(3) -0.0180(4) -0.0246(4) O1 0.0819(18) 0.0519(14) 0.0665(16) 0.0130(11) -0.0352(14) -0.0370(13) O2 0.0746(19) 0.088(2) 0.0734(18) -0.0015(15) -0.0420(15) -0.0241(16) N1 0.0446(15) 0.0503(15) 0.0445(14) 0.0013(11) -0.0109(12) -0.0231(12) N2 0.064(2) 0.094(3) 0.086(3) -0.016(2) -0.017(2) -0.047(2) C1 0.056(2) 0.0459(18) 0.0485(18) 0.0033(14) -0.0201(16) -0.0195(15) C2 0.061(2) 0.058(2) 0.053(2) -0.0032(16) -0.0198(18) -0.0227(18) C3 0.058(2) 0.057(2) 0.058(2) -0.0012(17) -0.0193(19) -0.0138(18) C4 0.064(2) 0.068(2) 0.0479(19) 0.0075(17) -0.0231(17) -0.0315(19) C5 0.077(3) 0.060(2) 0.062(2) -0.0033(18) -0.033(2) -0.026(2) C6 0.061(2) 0.048(2) 0.063(2) -0.0028(16) -0.0262(19) -0.0160(18) C7 0.059(3) 0.110(4) 0.073(3) 0.016(3) -0.029(2) -0.022(3) C8 0.100(4) 0.078(3) 0.084(3) 0.014(3) -0.036(3) -0.061(3) C9 0.0482(19) 0.0509(18) 0.0460(18) 0.0009(14) -0.0121(15) -0.0225(15) C10 0.0442(19) 0.058(2) 0.059(2) 0.0047(16) -0.0100(17) -0.0267(16) C11 0.049(2) 0.0480(18) 0.064(2) 0.0034(15) -0.0231(17) -0.0224(15) C12 0.059(2) 0.0501(18) 0.052(2) -0.0023(15) -0.0181(17) -0.0247(16) C13 0.0460(19) 0.0516(18) 0.0463(18) 0.0014(14) -0.0096(15) -0.0236(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.103(3) . ? Ni1 N1 2.103(3) 2_667 ? Ni1 S1 2.4923(12) 2_667 ? Ni1 S1 2.4923(12) . ? Ni1 S2 2.5161(13) 2_667 ? Ni1 S2 2.5162(13) . ? S1 P1 1.9997(14) . ? S2 P1 1.9847(14) . ? P1 O1 1.605(2) . ? P1 C1 1.791(4) . ? O1 C8 1.432(5) . ? O2 C4 1.369(4) . ? O2 C7 1.425(6) . ? N1 C13 1.343(4) . ? N1 C9 1.346(4) . ? N2 C11 1.361(5) . ? C1 C2 1.384(5) . ? C1 C6 1.402(5) . ? C2 C3 1.378(5) . ? C3 C4 1.381(5) . ? C4 C5 1.376(6) . ? C5 C6 1.376(5) . ? C9 C10 1.361(5) . ? C10 C11 1.399(5) . ? C11 C12 1.395(5) . ? C12 C13 1.375(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 179.999(1) . 2_667 ? N1 Ni1 S1 89.24(9) . 2_667 ? N1 Ni1 S1 90.75(9) 2_667 2_667 ? N1 Ni1 S1 90.76(9) . . ? N1 Ni1 S1 89.24(9) 2_667 . ? S1 Ni1 S1 180.0 2_667 . ? N1 Ni1 S2 90.26(8) . 2_667 ? N1 Ni1 S2 89.74(8) 2_667 2_667 ? S1 Ni1 S2 81.88(3) 2_667 2_667 ? S1 Ni1 S2 98.12(3) . 2_667 ? N1 Ni1 S2 89.74(8) . . ? N1 Ni1 S2 90.26(8) 2_667 . ? S1 Ni1 S2 98.12(3) 2_667 . ? S1 Ni1 S2 81.88(3) . . ? S2 Ni1 S2 179.999(1) 2_667 . ? P1 S1 Ni1 83.74(4) . . ? P1 S2 Ni1 83.41(4) . . ? O1 P1 C1 98.28(14) . . ? O1 P1 S2 112.30(12) . . ? C1 P1 S2 112.51(12) . . ? O1 P1 S1 110.00(10) . . ? C1 P1 S1 112.26(12) . . ? S2 P1 S1 110.91(5) . . ? C8 O1 P1 119.2(3) . . ? C4 O2 C7 118.1(4) . . ? C13 N1 C9 115.6(3) . . ? C13 N1 Ni1 122.9(2) . . ? C9 N1 Ni1 121.4(2) . . ? C2 C1 C6 117.7(3) . . ? C2 C1 P1 120.9(3) . . ? C6 C1 P1 121.4(3) . . ? C3 C2 C1 122.3(4) . . ? C2 C3 C4 119.2(4) . . ? O2 C4 C5 117.3(3) . . ? O2 C4 C3 123.0(4) . . ? C5 C4 C3 119.7(4) . . ? C6 C5 C4 121.1(4) . . ? C5 C6 C1 120.1(4) . . ? N1 C9 C10 124.3(3) . . ? C9 C10 C11 119.8(3) . . ? N2 C11 C10 121.5(4) . . ? N2 C11 C12 121.8(4) . . ? C10 C11 C12 116.7(3) . . ? C13 C12 C11 119.2(3) . . ? N1 C13 C12 124.5(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.412 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.064 data_COMPOUND (7) _database_code_CSD 157797 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 N2 Ni O4 P2 S4' _chemical_formula_weight 683.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.944(2) _cell_length_b 9.295(2) _cell_length_c 12.503(3) _cell_angle_alpha 75.70(2) _cell_angle_beta 76.59(3) _cell_angle_gamma 82.95(3) _cell_volume 758.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 15.2 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 354 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type semiempirical (psi-scan) _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 1.000 _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 CAD 4 _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2443 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2443 _reflns_number_gt 1809 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXL-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^)+(0.0525P)^2^+0.3311P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 2443 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.0000 0.0000 0.0000 0.0305(2) Uani 1 2 d S . . S2 S -0.17562(12) 0.19232(9) -0.12851(8) 0.0381(2) Uani 1 1 d . . . S1 S 0.26560(13) 0.02176(9) -0.17587(8) 0.0406(3) Uani 1 1 d . . . P1 P 0.07455(13) 0.17460(9) -0.24312(8) 0.0344(2) Uani 1 1 d . . . O2 O 0.3987(4) 0.7682(3) -0.4390(3) 0.0647(8) Uani 1 1 d . . . O1 O 0.0249(4) 0.1426(3) -0.3533(2) 0.0471(7) Uani 1 1 d . . . N1 N 0.1141(4) 0.1734(3) 0.0453(2) 0.0342(7) Uani 1 1 d . . . C1 C 0.1820(5) 0.3502(4) -0.3047(3) 0.0355(8) Uani 1 1 d . . . C2 C 0.3620(5) 0.3772(4) -0.2861(3) 0.0463(10) Uani 1 1 d . . . H2 H 0.4317 0.3015 -0.2435 0.056 Uiso 1 1 calc R . . C3 C 0.4399(6) 0.5151(4) -0.3298(3) 0.0500(10) Uani 1 1 d . . . H3 H 0.5611 0.5313 -0.3167 0.060 Uiso 1 1 calc R . . C4 C 0.3375(6) 0.6283(4) -0.3927(3) 0.0464(10) Uani 1 1 d . . . C5 C 0.1578(6) 0.6032(4) -0.4136(3) 0.0473(10) Uani 1 1 d . . . H5 H 0.0893 0.6787 -0.4571 0.057 Uiso 1 1 calc R . . C6 C 0.0820(5) 0.4658(4) -0.3694(3) 0.0426(9) Uani 1 1 d . . . H6 H -0.0389 0.4498 -0.3830 0.051 Uiso 1 1 calc R . . C7 C 0.5784(7) 0.8010(5) -0.4176(5) 0.0780(15) Uani 1 1 d . . . H7A H 0.6053 0.9023 -0.4545 0.117 Uiso 1 1 calc R . . H7B H 0.6852 0.7355 -0.4462 0.117 Uiso 1 1 calc R . . H7C H 0.5665 0.7875 -0.3378 0.117 Uiso 1 1 calc R . . C13 C -0.0074(5) 0.2806(4) 0.0859(3) 0.0405(9) Uani 1 1 d . . . H13 H -0.1432 0.2783 0.0925 0.049 Uiso 1 1 calc R . . C12 C 0.0586(6) 0.3931(4) 0.1181(3) 0.0477(10) Uani 1 1 d . . . H12 H -0.0311 0.4652 0.1454 0.057 Uiso 1 1 calc R . . C11 C 0.2578(6) 0.3983(4) 0.1098(4) 0.0523(10) Uani 1 1 d . . . H11 H 0.3062 0.4729 0.1318 0.063 Uiso 1 1 calc R . . C10 C 0.3836(6) 0.2905(4) 0.0680(4) 0.0566(11) Uani 1 1 d . . . H10 H 0.5199 0.2915 0.0603 0.068 Uiso 1 1 calc R . . C9 C 0.3078(5) 0.1812(4) 0.0377(3) 0.0452(10) Uani 1 1 d . . . H9 H 0.3957 0.1083 0.0102 0.054 Uiso 1 1 calc R . . C8 C -0.0902(8) 0.0201(5) -0.3436(4) 0.0690(14) Uani 1 1 d . . . H8A H -0.1067 0.0167 -0.4171 0.104 Uiso 1 1 calc R . . H8B H -0.2180 0.0329 -0.2958 0.104 Uiso 1 1 calc R . . H8C H -0.0229 -0.0712 -0.3114 0.104 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 0.0326(3) 0.0261(3) 0.0309(4) -0.0059(3) -0.0048(3) -0.0002(2) S2 0.0360(5) 0.0355(4) 0.0393(6) -0.0057(4) -0.0067(4) 0.0025(4) S1 0.0398(5) 0.0356(5) 0.0398(6) -0.0062(4) -0.0015(4) 0.0040(4) P1 0.0403(5) 0.0325(4) 0.0289(5) -0.0045(4) -0.0059(4) -0.0043(4) O2 0.0730(19) 0.0453(15) 0.075(2) 0.0031(15) -0.0211(17) -0.0231(14) O1 0.0627(16) 0.0456(14) 0.0332(15) -0.0047(12) -0.0074(13) -0.0177(12) N1 0.0371(16) 0.0295(14) 0.0344(18) -0.0068(13) -0.0064(13) 0.0004(12) C1 0.043(2) 0.0377(18) 0.025(2) -0.0055(15) -0.0060(16) -0.0052(15) C2 0.042(2) 0.044(2) 0.048(3) 0.0017(18) -0.0141(19) -0.0024(16) C3 0.044(2) 0.051(2) 0.055(3) -0.004(2) -0.0133(19) -0.0141(18) C4 0.053(2) 0.042(2) 0.041(2) -0.0016(18) -0.0063(19) -0.0151(17) C5 0.063(3) 0.0372(19) 0.044(2) -0.0003(18) -0.025(2) -0.0047(17) C6 0.046(2) 0.042(2) 0.043(2) -0.0044(18) -0.0197(18) -0.0084(16) C7 0.069(3) 0.059(3) 0.102(4) 0.003(3) -0.019(3) -0.032(2) C13 0.0400(19) 0.0358(18) 0.045(2) -0.0117(17) -0.0070(17) 0.0032(15) C12 0.062(3) 0.0342(19) 0.049(3) -0.0161(18) -0.011(2) 0.0052(17) C11 0.068(3) 0.041(2) 0.057(3) -0.0157(19) -0.021(2) -0.0103(19) C10 0.044(2) 0.052(2) 0.082(3) -0.021(2) -0.019(2) -0.0092(18) C9 0.038(2) 0.0364(19) 0.061(3) -0.0151(18) -0.0094(19) 0.0023(15) C8 0.103(4) 0.064(3) 0.051(3) -0.012(2) -0.020(3) -0.038(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 Ni N1 2.125(3) . ? Ni N1 2.125(3) 2 ? Ni S2 2.4938(12) . ? Ni S2 2.4938(12) 2 ? Ni S1 2.5036(13) . ? Ni S1 2.5036(13) 2 ? S2 P1 1.9975(14) . ? S1 P1 1.9874(14) . ? P1 O1 1.598(3) . ? P1 C1 1.796(3) . ? O2 C4 1.362(4) . ? O2 C7 1.418(5) . ? O1 C8 1.435(5) . ? N1 C9 1.336(4) . ? N1 C13 1.345(4) . ? C1 C2 1.385(5) . ? C1 C6 1.392(5) . ? C2 C3 1.386(5) . ? C3 C4 1.377(5) . ? C4 C5 1.390(5) . ? C5 C6 1.377(5) . ? C13 C12 1.370(5) . ? C12 C11 1.369(5) . ? C11 C10 1.368(5) . ? C10 C9 1.367(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni N1 180.00(14) . 2 ? N1 Ni S2 89.00(8) . . ? N1 Ni S2 91.00(8) 2 . ? N1 Ni S2 91.00(8) . 2 ? N1 Ni S2 89.00(8) 2 2 ? S2 Ni S2 180.00(3) . 2 ? N1 Ni S1 90.90(8) . . ? N1 Ni S1 89.10(8) 2 . ? S2 Ni S1 81.68(4) . . ? S2 Ni S1 98.32(4) 2 . ? N1 Ni S1 89.10(8) . 2 ? N1 Ni S1 90.90(8) 2 2 ? S2 Ni S1 98.32(4) . 2 ? S2 Ni S1 81.68(4) 2 2 ? S1 Ni S1 180.00(5) . 2 ? P1 S2 Ni 84.08(5) . . ? P1 S1 Ni 84.02(5) . . ? O1 P1 C1 99.10(15) . . ? O1 P1 S1 113.18(11) . . ? C1 P1 S1 111.75(12) . . ? O1 P1 S2 109.96(11) . . ? C1 P1 S2 112.27(12) . . ? S1 P1 S2 110.19(6) . . ? C4 O2 C7 117.4(3) . . ? C8 O1 P1 120.1(2) . . ? C9 N1 C13 116.1(3) . . ? C9 N1 Ni 122.7(2) . . ? C13 N1 Ni 121.2(2) . . ? C2 C1 C6 117.9(3) . . ? C2 C1 P1 121.5(3) . . ? C6 C1 P1 120.5(3) . . ? C1 C2 C3 121.2(3) . . ? C4 C3 C2 119.9(4) . . ? O2 C4 C3 125.0(4) . . ? O2 C4 C5 115.1(3) . . ? C3 C4 C5 119.9(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C1 121.5(3) . . ? N1 C13 C12 123.4(3) . . ? C11 C12 C13 119.3(4) . . ? C10 C11 C12 118.1(4) . . ? C9 C10 C11 119.6(4) . . ? N1 C9 C10 123.5(3) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.882 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.070