# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Udo Radius' _publ_contact_author_email U.RADIUS@UNI-WUERZBURG.DE _publ_section_title ; Facile C-S-, S-H-, and S-S bond cleavage using a Nickel(0) NHC Complex ; loop_ _publ_author_name 'Udo Radius' 'Marc Backes' 'Peter Fischer' 'Oliver Plietzsch' 'Thomas Schaub' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 726134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (iPr2Im)2(SMe)(pTolyl)Ni(II) ; _chemical_formula_sum 'C30 H46 N4 Ni S' _chemical_formula_weight 553.48 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9551(18) _cell_length_b 9.5880(19) _cell_length_c 19.095(4) _cell_angle_alpha 95.19(3) _cell_angle_beta 99.35(3) _cell_angle_gamma 107.21(3) _cell_volume 1528.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.75 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.8922 _diffrn_ambient_temperature 203(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 1' _diffrn_measurement_method rotation _diffrn_reflns_number 11091 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0856 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.89 _reflns_number_total 5449 _reflns_number_gt 3909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+4.8569P] 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 5449 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.043 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 S1 S 0.7781(2) 1.08954(16) 0.77724(10) 0.0481(5) Uani 1 1 d . . . Ni1 Ni 0.55236(9) 0.90265(7) 0.73591(4) 0.0262(2) Uani 1 1 d . . . N1 N 0.7654(6) 0.7354(5) 0.7053(2) 0.0320(11) Uani 1 1 d . . . N2 N 0.7139(6) 0.7188(5) 0.8099(2) 0.0326(11) Uani 1 1 d . . . N3 N 0.3935(6) 1.1047(5) 0.6750(2) 0.0340(11) Uani 1 1 d . . . N4 N 0.3474(6) 1.0648(5) 0.7783(2) 0.0364(11) Uani 1 1 d . . . C1 C 0.6809(6) 0.7784(5) 0.7501(3) 0.0293(12) Uani 1 1 d . . . C2 C 0.8503(8) 0.6499(6) 0.7370(3) 0.0451(16) Uani 1 1 d . . . H2A H 0.9173 0.6067 0.7162 0.054 Uiso 1 1 calc R . . C3 C 0.8188(8) 0.6408(6) 0.8020(3) 0.0440(16) Uani 1 1 d . . . H3A H 0.8601 0.5906 0.8364 0.053 Uiso 1 1 calc R . . C4 C 0.6550(8) 0.7425(6) 0.8759(3) 0.0433(15) Uani 1 1 d . . . H4A H 0.5696 0.7876 0.8642 0.052 Uiso 1 1 calc R . . C5 C 0.7868(9) 0.8520(8) 0.9324(3) 0.059(2) Uani 1 1 d . . . H5A H 0.8274 0.9431 0.9133 0.088 Uiso 1 1 calc R . . H5B H 0.8725 0.8108 0.9453 0.088 Uiso 1 1 calc R . . H5C H 0.7448 0.8719 0.9746 0.088 Uiso 1 1 calc R . . C6 C 0.5807(10) 0.5966(8) 0.9012(4) 0.066(2) Uani 1 1 d . . . H6A H 0.4964 0.5327 0.8631 0.099 Uiso 1 1 calc R . . H6B H 0.5366 0.6144 0.9430 0.099 Uiso 1 1 calc R . . H6C H 0.6617 0.5497 0.9135 0.099 Uiso 1 1 calc R . . C7 C 0.7745(8) 0.7793(6) 0.6341(3) 0.0404(14) Uani 1 1 d . . . H7A H 0.7019 0.8389 0.6247 0.048 Uiso 1 1 calc R . . C8 C 0.7136(11) 0.6429(8) 0.5771(4) 0.065(2) Uani 1 1 d . . . H8A H 0.6063 0.5862 0.5805 0.097 Uiso 1 1 calc R . . H8B H 0.7831 0.5826 0.5845 0.097 Uiso 1 1 calc R . . H8C H 0.7127 0.6729 0.5299 0.097 Uiso 1 1 calc R . . C9 C 0.9414(9) 0.8770(10) 0.6338(5) 0.071(2) Uani 1 1 d . . . H9A H 0.9712 0.9615 0.6711 0.107 Uiso 1 1 calc R . . H9B H 0.9446 0.9106 0.5875 0.107 Uiso 1 1 calc R . . H9C H 1.0155 0.8215 0.6426 0.107 Uiso 1 1 calc R . . C10 C 0.4220(7) 1.0250(5) 0.7272(3) 0.0308(12) Uani 1 1 d . . . C11 C 0.3071(8) 1.1949(7) 0.6937(4) 0.0461(16) Uani 1 1 d . . . H11A H 0.2751 1.2612 0.6661 0.055 Uiso 1 1 calc R . . C12 C 0.2776(8) 1.1704(7) 0.7582(4) 0.0479(17) Uani 1 1 d . . . H12A H 0.2208 1.2157 0.7849 0.058 Uiso 1 1 calc R . . C13 C 0.3460(9) 1.0080(7) 0.8477(3) 0.0443(16) Uani 1 1 d . . . H13A H 0.3791 0.9184 0.8435 0.053 Uiso 1 1 calc R . . C14 C 0.4683(10) 1.1199(10) 0.9063(4) 0.076(3) Uani 1 1 d . . . H14A H 0.5721 1.1438 0.8931 0.114 Uiso 1 1 calc R . . H14B H 0.4731 1.0788 0.9509 0.114 Uiso 1 1 calc R . . H14C H 0.4381 1.2087 0.9125 0.114 Uiso 1 1 calc R . . C15 C 0.1829(11) 0.9636(10) 0.8642(4) 0.074(2) Uani 1 1 d . . . H15A H 0.1100 0.8913 0.8253 0.112 Uiso 1 1 calc R . . H15B H 0.1476 1.0497 0.8697 0.112 Uiso 1 1 calc R . . H15C H 0.1851 0.9211 0.9084 0.112 Uiso 1 1 calc R . . C16 C 0.4448(8) 1.0954(7) 0.6055(3) 0.0419(15) Uani 1 1 d . . . H16A H 0.5187 1.0361 0.6080 0.050 Uiso 1 1 calc R . . C17 C 0.5332(10) 1.2484(8) 0.5909(4) 0.067(2) Uani 1 1 d . . . H17A H 0.6244 1.2950 0.6296 0.100 Uiso 1 1 calc R . . H17B H 0.4622 1.3078 0.5878 0.100 Uiso 1 1 calc R . . H17C H 0.5695 1.2398 0.5460 0.100 Uiso 1 1 calc R . . C18 C 0.3015(9) 1.0179(8) 0.5455(4) 0.0550(18) Uani 1 1 d . . . H18A H 0.2485 0.9201 0.5556 0.082 Uiso 1 1 calc R . . H18B H 0.3369 1.0097 0.5004 0.082 Uiso 1 1 calc R . . H18C H 0.2277 1.0746 0.5423 0.082 Uiso 1 1 calc R . . C19 C 0.7540(8) 1.2704(6) 0.7811(4) 0.0481(17) Uani 1 1 d . . . H19A H 0.8566 1.3450 0.7995 0.072 Uiso 1 1 calc R . . H19B H 0.6809 1.2778 0.8125 0.072 Uiso 1 1 calc R . . H19C H 0.7115 1.2854 0.7333 0.072 Uiso 1 1 calc R . . C20 C 0.3729(7) 0.7279(6) 0.6964(3) 0.0327(13) Uani 1 1 d . . . C21 C 0.2834(7) 0.6317(6) 0.7360(3) 0.0341(13) Uani 1 1 d . . . H21A H 0.3075 0.6551 0.7863 0.041 Uiso 1 1 calc R . . C22 C 0.1591(7) 0.5017(6) 0.7047(4) 0.0413(15) Uani 1 1 d . . . H22A H 0.1031 0.4426 0.7347 0.050 Uiso 1 1 calc R . . C23 C 0.1166(7) 0.4581(6) 0.6317(4) 0.0418(16) Uani 1 1 d . . . C24 C 0.2049(8) 0.5519(6) 0.5910(3) 0.0428(15) Uani 1 1 d . . . H24A H 0.1811 0.5283 0.5407 0.051 Uiso 1 1 calc R . . C25 C 0.3283(7) 0.6808(6) 0.6234(3) 0.0384(14) Uani 1 1 d . . . H25A H 0.3848 0.7392 0.5934 0.046 Uiso 1 1 calc R . . C26 C -0.0169(8) 0.3176(7) 0.5974(4) 0.063(2) Uani 1 1 d . . . H26A H -0.0626 0.2674 0.6345 0.095 Uiso 1 1 calc R . . H26B H 0.0253 0.2534 0.5699 0.095 Uiso 1 1 calc R . . H26C H -0.0988 0.3421 0.5658 0.095 Uiso 1 1 calc R . . C32 C 0.0772(15) 0.6340(17) 0.0175(8) 0.103(4) Uani 1 1 d . . . C30 C -0.1284(16) 0.556(2) 0.0795(7) 0.144(6) Uani 1 1 d . . . H30A H -0.2116 0.6031 0.0695 0.172 Uiso 1 1 calc R . . H30B H -0.0906 0.5614 0.1311 0.172 Uiso 1 1 calc R . . C31 C -0.026(2) 0.588(3) 0.0454(8) 0.173(10) Uani 1 1 d . . . H31A H -0.0989 0.6140 0.0078 0.208 Uiso 1 1 calc R . . C33 C 0.169(2) 0.616(2) -0.0290(12) 0.190(10) Uani 1 1 d . . . H33A H 0.2433 0.5926 0.0089 0.228 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 S1 0.0401(9) 0.0258(7) 0.0725(11) 0.0004(7) 0.0003(8) 0.0096(6) Ni1 0.0316(4) 0.0193(3) 0.0305(4) 0.0033(2) 0.0056(3) 0.0128(3) N1 0.037(3) 0.030(2) 0.035(2) 0.0035(19) 0.008(2) 0.020(2) N2 0.044(3) 0.028(2) 0.030(2) 0.0069(18) 0.006(2) 0.019(2) N3 0.040(3) 0.031(2) 0.036(3) 0.009(2) 0.006(2) 0.018(2) N4 0.048(3) 0.036(3) 0.031(2) 0.001(2) 0.008(2) 0.023(2) C1 0.032(3) 0.019(2) 0.035(3) 0.001(2) 0.005(3) 0.006(2) C2 0.051(4) 0.041(3) 0.053(4) 0.004(3) 0.002(3) 0.035(3) C3 0.060(4) 0.037(3) 0.045(4) 0.013(3) 0.006(3) 0.030(3) C4 0.055(4) 0.041(3) 0.037(3) 0.012(3) 0.008(3) 0.019(3) C5 0.070(5) 0.059(4) 0.036(3) -0.003(3) 0.000(3) 0.012(4) C6 0.069(5) 0.063(5) 0.069(5) 0.035(4) 0.017(4) 0.015(4) C7 0.048(4) 0.042(3) 0.036(3) 0.002(3) 0.010(3) 0.022(3) C8 0.105(7) 0.056(4) 0.040(4) -0.002(3) 0.012(4) 0.039(4) C9 0.050(5) 0.095(6) 0.070(5) 0.029(5) 0.028(4) 0.012(4) C10 0.036(3) 0.025(3) 0.032(3) 0.000(2) 0.003(3) 0.013(2) C11 0.055(4) 0.037(3) 0.055(4) 0.008(3) 0.005(3) 0.030(3) C12 0.054(4) 0.050(4) 0.056(4) 0.003(3) 0.015(3) 0.038(3) C13 0.066(5) 0.044(3) 0.034(3) 0.005(3) 0.019(3) 0.031(3) C14 0.068(6) 0.112(7) 0.039(4) 0.020(4) 0.009(4) 0.014(5) C15 0.078(6) 0.078(5) 0.056(5) 0.008(4) 0.028(4) 0.001(5) C16 0.046(4) 0.044(3) 0.040(3) 0.015(3) 0.007(3) 0.019(3) C17 0.066(5) 0.066(5) 0.062(5) 0.034(4) 0.014(4) 0.004(4) C18 0.061(5) 0.061(4) 0.044(4) 0.004(3) 0.010(3) 0.021(4) C19 0.056(4) 0.023(3) 0.058(4) 0.002(3) 0.002(3) 0.007(3) C20 0.039(3) 0.034(3) 0.034(3) -0.001(2) 0.003(3) 0.028(3) C21 0.038(3) 0.033(3) 0.034(3) 0.006(2) 0.008(3) 0.015(2) C22 0.036(3) 0.027(3) 0.062(4) 0.009(3) 0.009(3) 0.012(2) C23 0.034(3) 0.030(3) 0.057(4) -0.006(3) -0.009(3) 0.016(3) C24 0.051(4) 0.037(3) 0.036(3) -0.008(3) -0.003(3) 0.017(3) C25 0.038(3) 0.028(3) 0.046(3) -0.001(2) 0.009(3) 0.007(2) C26 0.048(4) 0.036(3) 0.086(5) -0.008(3) -0.019(4) 0.006(3) C32 0.060(7) 0.140(11) 0.104(10) 0.047(9) 0.000(7) 0.024(7) C30 0.081(9) 0.231(19) 0.099(9) 0.054(11) -0.020(8) 0.032(10) C31 0.091(10) 0.35(3) 0.141(13) 0.160(17) 0.036(10) 0.111(14) C33 0.18(2) 0.139(14) 0.194(19) 0.031(14) -0.101(16) 0.040(14) _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 S1 C19 1.806(6) . ? S1 Ni1 2.2370(19) . ? Ni1 C10 1.885(5) . ? Ni1 C1 1.893(5) . ? Ni1 C20 1.934(6) . ? N1 C1 1.344(7) . ? N1 C2 1.388(7) . ? N1 C7 1.467(7) . ? N2 C1 1.351(7) . ? N2 C3 1.381(7) . ? N2 C4 1.467(8) . ? N3 C10 1.345(7) . ? N3 C11 1.381(7) . ? N3 C16 1.476(8) . ? N4 C10 1.356(7) . ? N4 C12 1.390(7) . ? N4 C13 1.478(7) . ? C2 C3 1.322(9) . ? C4 C5 1.519(9) . ? C4 C6 1.519(9) . ? C7 C9 1.512(10) . ? C7 C8 1.524(8) . ? C11 C12 1.326(9) . ? C13 C15 1.489(11) . ? C13 C14 1.514(10) . ? C16 C17 1.522(9) . ? C16 C18 1.522(9) . ? C20 C25 1.380(8) . ? C20 C21 1.398(8) . ? C21 C22 1.406(8) . ? C22 C23 1.376(9) . ? C23 C24 1.394(9) . ? C23 C26 1.519(8) . ? C24 C25 1.402(8) . ? C32 C31 1.134(16) . ? C32 C33 1.33(3) . ? C30 C31 1.195(19) . ? C30 C33 1.74(2) 2_565 ? C31 C33 1.96(3) 2_565 ? C33 C30 1.74(2) 2_565 ? C33 C31 1.96(3) 2_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 C19 S1 Ni1 114.5(2) . . ? C10 Ni1 C1 176.6(2) . . ? C10 Ni1 C20 91.8(2) . . ? C1 Ni1 C20 88.2(2) . . ? C10 Ni1 S1 94.42(17) . . ? C1 Ni1 S1 85.75(16) . . ? C20 Ni1 S1 173.16(16) . . ? C1 N1 C2 110.8(5) . . ? C1 N1 C7 124.9(4) . . ? C2 N1 C7 124.2(5) . . ? C1 N2 C3 110.7(5) . . ? C1 N2 C4 124.5(5) . . ? C3 N2 C4 124.7(5) . . ? C10 N3 C11 111.6(5) . . ? C10 N3 C16 124.7(5) . . ? C11 N3 C16 123.7(5) . . ? C10 N4 C12 111.1(5) . . ? C10 N4 C13 124.6(5) . . ? C12 N4 C13 124.2(5) . . ? N1 C1 N2 104.5(4) . . ? N1 C1 Ni1 128.4(4) . . ? N2 C1 Ni1 127.0(4) . . ? C3 C2 N1 106.8(6) . . ? C2 C3 N2 107.2(5) . . ? N2 C4 C5 110.2(5) . . ? N2 C4 C6 110.9(5) . . ? C5 C4 C6 113.6(6) . . ? N1 C7 C9 110.0(5) . . ? N1 C7 C8 109.9(5) . . ? C9 C7 C8 114.3(6) . . ? N3 C10 N4 103.8(4) . . ? N3 C10 Ni1 130.1(4) . . ? N4 C10 Ni1 125.8(4) . . ? C12 C11 N3 107.0(5) . . ? C11 C12 N4 106.5(5) . . ? N4 C13 C15 111.7(6) . . ? N4 C13 C14 109.8(5) . . ? C15 C13 C14 113.0(6) . . ? N3 C16 C17 110.6(5) . . ? N3 C16 C18 110.2(5) . . ? C17 C16 C18 111.1(5) . . ? C25 C20 C21 112.9(5) . . ? C25 C20 Ni1 121.2(5) . . ? C21 C20 Ni1 125.7(4) . . ? C20 C21 C22 123.5(5) . . ? C23 C22 C21 122.2(6) . . ? C22 C23 C24 115.4(5) . . ? C22 C23 C26 122.6(7) . . ? C24 C23 C26 122.0(6) . . ? C23 C24 C25 121.4(6) . . ? C20 C25 C24 124.6(6) . . ? C31 C32 C33 151(2) . . ? C31 C30 C33 81.5(18) . 2_565 ? C32 C31 C30 172(3) . . ? C32 C31 C33 126(2) . 2_565 ? C30 C31 C33 61.4(16) . 2_565 ? C32 C33 C30 120.0(17) . 2_565 ? C32 C33 C31 82.9(15) . 2_565 ? C30 C33 C31 37.1(7) 2_565 2_565 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.860 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.090 _chemical_name_common (iPr2Im)2(SMe)(pTolyl)Ni(ii) data_compound5 _database_code_depnum_ccdc_archive 'CCDC 726135' _chemical_name_systematic ; (iPr2Im)2(CS-Dibenzothiophenylato)Ni(II) ; _chemical_formula_sum 'C30 H40 N4 Ni S' _chemical_formula_weight 547.43 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' 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 P2(1)/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 9.9882(6) _cell_length_b 14.4104(11) _cell_length_c 20.4776(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.962(7) _cell_angle_gamma 90.00 _cell_volume 2931.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.85 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 13951 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4558 _reflns_number_gt 3795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0697P)^2^+0.2032P] 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 4558 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 S1 S 0.30779(7) 0.80633(4) 0.27896(3) 0.03613(18) Uani 1 1 d . . . Ni1 Ni 0.21955(3) 0.935005(18) 0.244497(14) 0.02155(12) Uani 1 1 d . . . C1 C 0.1958(2) 1.06457(15) 0.23438(12) 0.0243(5) Uani 1 1 d . . . C2 C 0.2150(3) 1.21735(17) 0.25578(15) 0.0482(8) Uani 1 1 d . . . H2A H 0.2414 1.2721 0.2786 0.058 Uiso 1 1 calc R . . C3 C 0.1472(3) 1.21100(17) 0.20325(15) 0.0487(8) Uani 1 1 d . . . H3A H 0.1099 1.2599 0.1769 0.058 Uiso 1 1 calc R . . C4 C 0.0760(3) 1.07935(17) 0.13292(14) 0.0357(6) Uani 1 1 d . . . H4A H 0.0682 1.0116 0.1396 0.043 Uiso 1 1 calc R . . C5 C -0.0640(3) 1.1199(2) 0.12861(18) 0.0576(9) Uani 1 1 d . . . H5A H -0.1053 1.1043 0.1680 0.086 Uiso 1 1 calc R . . H5B H -0.1177 1.0946 0.0906 0.086 Uiso 1 1 calc R . . H5C H -0.0589 1.1868 0.1245 0.086 Uiso 1 1 calc R . . C6 C 0.1680(3) 1.0958(2) 0.07074(16) 0.0555(9) Uani 1 1 d . . . H6A H 0.2547 1.0658 0.0804 0.083 Uiso 1 1 calc R . . H6B H 0.1812 1.1618 0.0646 0.083 Uiso 1 1 calc R . . H6C H 0.1218 1.0695 0.0310 0.083 Uiso 1 1 calc R . . C7 C 0.3196(3) 1.10508(17) 0.33130(13) 0.0343(6) Uani 1 1 d . . . H7A H 0.3281 1.0366 0.3322 0.041 Uiso 1 1 calc R . . C8 C 0.2434(3) 1.1357(2) 0.39509(15) 0.0490(8) Uani 1 1 d . . . H8A H 0.1574 1.1041 0.3937 0.074 Uiso 1 1 calc R . . H8B H 0.2289 1.2022 0.3943 0.074 Uiso 1 1 calc R . . H8C H 0.2988 1.1188 0.4351 0.074 Uiso 1 1 calc R . . C9 C 0.4614(3) 1.1458(2) 0.32262(17) 0.0546(9) Uani 1 1 d . . . H9A H 0.4928 1.1210 0.2829 0.082 Uiso 1 1 calc R . . H9B H 0.5241 1.1288 0.3601 0.082 Uiso 1 1 calc R . . H9C H 0.4556 1.2129 0.3195 0.082 Uiso 1 1 calc R . . C10 C 0.3120(2) 0.90991(15) 0.15905(12) 0.0264(5) Uani 1 1 d . . . C11 C 0.4650(3) 0.89367(19) 0.07014(14) 0.0417(7) Uani 1 1 d . . . H11A H 0.5381 0.9019 0.0453 0.050 Uiso 1 1 calc R . . C12 C 0.3594(3) 0.84008(19) 0.06035(14) 0.0452(7) Uani 1 1 d . . . H12A H 0.3431 0.7996 0.0244 0.054 Uiso 1 1 calc R . . C13 C 0.1345(3) 0.80316(17) 0.12484(14) 0.0394(7) Uani 1 1 d . . . H13A H 0.0939 0.8339 0.1613 0.047 Uiso 1 1 calc R . . C14 C 0.0546(4) 0.8195(2) 0.06589(19) 0.0705(12) Uani 1 1 d . . . H14A H 0.0458 0.8858 0.0586 0.106 Uiso 1 1 calc R . . H14B H -0.0338 0.7925 0.0681 0.106 Uiso 1 1 calc R . . H14C H 0.0962 0.7914 0.0300 0.106 Uiso 1 1 calc R . . C15 C 0.1522(3) 0.70107(18) 0.13955(16) 0.0503(8) Uani 1 1 d . . . H15A H 0.0657 0.6740 0.1462 0.075 Uiso 1 1 calc R . . H15B H 0.2139 0.6931 0.1789 0.075 Uiso 1 1 calc R . . H15C H 0.1883 0.6705 0.1030 0.075 Uiso 1 1 calc R . . C16 C 0.5238(3) 0.99886(18) 0.16282(15) 0.0374(6) Uani 1 1 d . . . H16A H 0.4805 1.0269 0.1994 0.045 Uiso 1 1 calc R . . C17 C 0.5717(4) 1.0784(2) 0.1190(2) 0.0689(12) Uani 1 1 d . . . H17A H 0.4948 1.1151 0.1016 0.103 Uiso 1 1 calc R . . H17B H 0.6148 1.0518 0.0830 0.103 Uiso 1 1 calc R . . H17C H 0.6354 1.1177 0.1451 0.103 Uiso 1 1 calc R . . C18 C 0.6369(4) 0.9470(3) 0.1892(2) 0.0845(15) Uani 1 1 d . . . H18A H 0.6077 0.8978 0.2168 0.127 Uiso 1 1 calc R . . H18B H 0.6991 0.9874 0.2153 0.127 Uiso 1 1 calc R . . H18C H 0.6813 0.9202 0.1538 0.127 Uiso 1 1 calc R . . C19 C 0.0860(2) 0.93534(13) 0.31909(12) 0.0251(5) Uani 1 1 d . . . C20 C -0.0462(2) 0.95648(16) 0.30588(14) 0.0327(6) Uani 1 1 d . . . H20A H -0.0728 0.9795 0.2636 0.039 Uiso 1 1 calc R . . C21 C -0.1572(3) 0.94741(17) 0.35157(16) 0.0404(7) Uani 1 1 d . . . H21A H -0.2448 0.9646 0.3347 0.048 Uiso 1 1 calc R . . C22 C -0.1395(3) 0.91648(18) 0.41451(16) 0.0423(7) Uani 1 1 d . . . H22A H -0.2077 0.9105 0.4426 0.051 Uiso 1 1 calc R . . C23 C -0.0117(3) 0.89627(18) 0.42987(14) 0.0395(7) Uani 1 1 d . . . H23A H 0.0134 0.8747 0.4727 0.047 Uiso 1 1 calc R . . C24 C 0.1014(3) 0.90479(15) 0.38358(12) 0.0277(5) Uani 1 1 d . . . C25 C 0.2371(3) 0.88240(15) 0.40308(12) 0.0321(6) Uani 1 1 d . . . C26 C 0.2698(4) 0.90758(19) 0.46590(15) 0.0486(8) Uani 1 1 d . . . H26A H 0.2095 0.9353 0.4923 0.058 Uiso 1 1 calc R . . C27 C 0.3947(4) 0.8892(2) 0.48576(18) 0.0667(12) Uani 1 1 d . . . H27A H 0.4269 0.9052 0.5290 0.080 Uiso 1 1 calc R . . C28 C 0.4901(4) 0.8441(2) 0.4442(2) 0.0668(12) Uani 1 1 d . . . H28A H 0.5778 0.8323 0.4637 0.080 Uiso 1 1 calc R . . C29 C 0.4613(3) 0.8190(2) 0.38138(17) 0.0486(8) Uani 1 1 d . . . H29A H 0.5232 0.7911 0.3559 0.058 Uiso 1 1 calc R . . C30 C 0.3345(3) 0.83826(15) 0.35957(13) 0.0337(6) Uani 1 1 d . . . N1 N 0.2450(2) 1.12820(13) 0.27476(11) 0.0320(5) Uani 1 1 d . . . N2 N 0.1361(2) 1.11681(13) 0.19014(11) 0.0325(5) Uani 1 1 d . . . N3 N 0.4352(2) 0.93621(13) 0.13047(11) 0.0301(5) Uani 1 1 d . . . N4 N 0.2661(2) 0.85104(13) 0.11398(10) 0.0321(5) Uani 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 S1 0.0514(4) 0.0277(3) 0.0285(4) 0.0031(2) 0.0006(3) 0.0146(3) Ni1 0.02618(17) 0.01803(16) 0.0191(2) 0.00100(10) -0.00386(12) -0.00004(11) C1 0.0247(11) 0.0229(11) 0.0237(14) 0.0040(9) -0.0045(10) -0.0011(9) C2 0.072(2) 0.0175(12) 0.050(2) 0.0034(11) -0.0201(16) -0.0081(12) C3 0.068(2) 0.0199(12) 0.052(2) 0.0091(11) -0.0234(17) -0.0003(12) C4 0.0386(14) 0.0343(13) 0.0305(16) 0.0049(10) -0.0129(12) -0.0011(10) C5 0.0384(16) 0.069(2) 0.060(2) 0.0070(16) -0.0198(15) 0.0021(15) C6 0.0506(18) 0.075(2) 0.0371(19) 0.0091(15) -0.0153(15) 0.0037(16) C7 0.0414(14) 0.0279(12) 0.0303(16) 0.0010(10) -0.0120(12) -0.0069(10) C8 0.0643(19) 0.0474(16) 0.0328(18) -0.0043(12) -0.0066(15) -0.0030(14) C9 0.0477(17) 0.066(2) 0.046(2) -0.0007(15) -0.0167(15) -0.0218(15) C10 0.0320(12) 0.0221(11) 0.0230(14) 0.0014(9) -0.0074(11) 0.0002(9) C11 0.0505(17) 0.0446(15) 0.0325(18) -0.0038(12) 0.0165(13) -0.0034(13) C12 0.0669(19) 0.0418(15) 0.0268(17) -0.0084(11) 0.0043(14) -0.0051(14) C13 0.0442(15) 0.0337(13) 0.0369(17) -0.0029(11) -0.0126(13) -0.0092(11) C14 0.079(2) 0.057(2) 0.065(2) 0.0101(16) -0.045(2) -0.0227(17) C15 0.0593(18) 0.0347(14) 0.053(2) -0.0020(12) -0.0118(15) -0.0128(13) C16 0.0297(13) 0.0425(15) 0.0379(17) 0.0006(11) -0.0065(12) -0.0064(11) C17 0.065(2) 0.0416(17) 0.090(3) 0.0222(16) -0.040(2) -0.0158(15) C18 0.065(2) 0.062(2) 0.115(4) 0.034(2) -0.045(2) -0.0097(18) C19 0.0310(12) 0.0156(10) 0.0277(14) -0.0021(8) -0.0016(10) -0.0031(9) C20 0.0339(13) 0.0248(12) 0.0379(16) -0.0001(10) -0.0040(12) -0.0004(10) C21 0.0310(13) 0.0329(13) 0.057(2) -0.0079(12) 0.0005(13) -0.0013(10) C22 0.0434(16) 0.0382(14) 0.048(2) -0.0069(12) 0.0199(14) -0.0068(12) C23 0.0579(18) 0.0328(13) 0.0276(16) -0.0031(10) 0.0032(13) -0.0055(12) C24 0.0399(14) 0.0192(10) 0.0235(14) -0.0012(9) 0.0010(11) -0.0026(9) C25 0.0460(15) 0.0222(11) 0.0256(15) 0.0060(9) -0.0077(12) -0.0064(10) C26 0.072(2) 0.0373(14) 0.0326(18) 0.0063(11) -0.0150(16) -0.0112(14) C27 0.083(3) 0.0561(19) 0.052(2) 0.0131(16) -0.037(2) -0.0242(19) C28 0.057(2) 0.064(2) 0.071(3) 0.0300(18) -0.037(2) -0.0232(17) C29 0.0403(16) 0.0451(16) 0.058(2) 0.0192(14) -0.0084(15) -0.0033(13) C30 0.0385(14) 0.0227(11) 0.0373(17) 0.0108(10) -0.0086(12) -0.0046(10) N1 0.0395(11) 0.0226(10) 0.0300(13) 0.0031(8) -0.0149(10) -0.0063(8) N2 0.0380(12) 0.0242(10) 0.0312(13) 0.0047(8) -0.0152(10) -0.0007(8) N3 0.0320(11) 0.0311(10) 0.0266(13) 0.0013(8) -0.0008(9) -0.0014(8) N4 0.0402(12) 0.0295(10) 0.0248(13) -0.0031(8) -0.0045(10) -0.0056(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 S1 C30 1.708(3) . ? S1 Ni1 2.1410(6) . ? Ni1 C1 1.891(2) . ? Ni1 C10 2.093(3) . ? Ni1 C19 2.130(3) . ? C1 N2 1.277(3) . ? C1 N1 1.297(3) . ? C2 C3 1.214(4) . ? C2 N1 1.366(3) . ? C2 H2A 0.9400 . ? C3 N2 1.386(3) . ? C3 H3A 0.9400 . ? C4 N2 1.371(3) . ? C4 C5 1.509(4) . ? C4 C6 1.663(5) . ? C4 H4A 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 N1 1.352(3) . ? C7 C9 1.560(4) . ? C7 C8 1.639(4) . ? C7 H7A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 N4 1.302(3) . ? C10 N3 1.466(3) . ? C11 C12 1.305(4) . ? C11 N3 1.437(4) . ? C11 H11A 0.9400 . ? C12 N4 1.521(4) . ? C12 H12A 0.9400 . ? C13 C14 1.396(4) . ? C13 C15 1.508(4) . ? C13 N4 1.521(3) . ? C13 H13A 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 N3 1.384(3) . ? C16 C18 1.414(4) . ? C16 C17 1.562(4) . ? C16 H16A 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.354(3) . ? C19 C24 1.385(3) . ? C20 C21 1.529(4) . ? C20 H20A 0.9400 . ? C21 C22 1.358(4) . ? C21 H21A 0.9400 . ? C22 C23 1.315(4) . ? C22 H22A 0.9400 . ? C23 C24 1.553(4) . ? C23 H23A 0.9400 . ? C24 C25 1.410(3) . ? C25 C26 1.344(4) . ? C25 C30 1.525(4) . ? C26 C27 1.298(5) . ? C26 H26A 0.9400 . ? C27 C28 1.491(6) . ? C27 H27A 0.9400 . ? C28 C29 1.338(5) . ? C28 H28A 0.9400 . ? C29 C30 1.328(4) . ? C29 H29A 0.9400 . ? 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 C30 S1 Ni1 95.90(8) . . ? C1 Ni1 C10 98.06(10) . . ? C1 Ni1 C19 89.74(9) . . ? C10 Ni1 C19 164.48(9) . . ? C1 Ni1 S1 159.07(7) . . ? C10 Ni1 S1 85.62(6) . . ? C19 Ni1 S1 91.87(6) . . ? N2 C1 N1 98.84(19) . . ? N2 C1 Ni1 134.74(18) . . ? N1 C1 Ni1 126.40(17) . . ? C3 C2 N1 105.5(2) . . ? C3 C2 H2A 127.3 . . ? N1 C2 H2A 127.3 . . ? C2 C3 N2 105.8(2) . . ? C2 C3 H3A 127.1 . . ? N2 C3 H3A 127.1 . . ? N2 C4 C5 102.6(2) . . ? N2 C4 C6 111.8(2) . . ? C5 C4 C6 118.8(2) . . ? N2 C4 H4A 107.7 . . ? C5 C4 H4A 107.7 . . ? C6 C4 H4A 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C9 103.7(2) . . ? N1 C7 C8 110.8(2) . . ? C9 C7 C8 119.5(2) . . ? N1 C7 H7A 107.4 . . ? C9 C7 H7A 107.4 . . ? C8 C7 H7A 107.4 . . ? 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 . . ? N4 C10 N3 97.7(2) . . ? N4 C10 Ni1 123.47(19) . . ? N3 C10 Ni1 138.63(16) . . ? C12 C11 N3 98.5(2) . . ? C12 C11 H11A 130.7 . . ? N3 C11 H11A 130.7 . . ? C11 C12 N4 111.9(2) . . ? C11 C12 H12A 124.0 . . ? N4 C12 H12A 124.0 . . ? C14 C13 C15 112.4(2) . . ? C14 C13 N4 102.8(3) . . ? C15 C13 N4 112.7(2) . . ? C14 C13 H13A 109.5 . . ? C15 C13 H13A 109.5 . . ? N4 C13 H13A 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 106.5(3) . . ? N3 C16 C17 115.0(2) . . ? C18 C16 C17 109.1(3) . . ? N3 C16 H16A 108.7 . . ? C18 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 105.8(2) . . ? C20 C19 Ni1 121.82(19) . . ? C24 C19 Ni1 131.83(18) . . ? C19 C20 C21 127.7(2) . . ? C19 C20 H20A 116.1 . . ? C21 C20 H20A 116.1 . . ? C22 C21 C20 125.3(3) . . ? C22 C21 H21A 117.3 . . ? C20 C21 H21A 117.3 . . ? C23 C22 C21 109.1(3) . . ? C23 C22 H22A 125.5 . . ? C21 C22 H22A 125.5 . . ? C22 C23 C24 125.9(3) . . ? C22 C23 H23A 117.1 . . ? C24 C23 H23A 117.1 . . ? C19 C24 C25 110.6(2) . . ? C19 C24 C23 126.2(2) . . ? C25 C24 C23 123.2(2) . . ? C26 C25 C24 109.9(3) . . ? C26 C25 C30 124.4(3) . . ? C24 C25 C30 125.7(2) . . ? C27 C26 C25 112.0(3) . . ? C27 C26 H26A 124.0 . . ? C25 C26 H26A 124.0 . . ? C26 C27 C28 124.1(3) . . ? C26 C27 H27A 118.0 . . ? C28 C27 H27A 118.0 . . ? C29 C28 C27 125.5(3) . . ? C29 C28 H28A 117.3 . . ? C27 C28 H28A 117.3 . . ? C30 C29 C28 111.6(3) . . ? C30 C29 H29A 124.2 . . ? C28 C29 H29A 124.2 . . ? C29 C30 C25 122.3(3) . . ? C29 C30 S1 108.5(2) . . ? C25 C30 S1 129.20(18) . . ? C1 N1 C7 120.7(2) . . ? C1 N1 C2 115.2(2) . . ? C7 N1 C2 124.1(2) . . ? C1 N2 C4 120.3(2) . . ? C1 N2 C3 114.7(2) . . ? C4 N2 C3 124.8(2) . . ? C16 N3 C11 120.7(2) . . ? C16 N3 C10 119.9(2) . . ? C11 N3 C10 119.3(2) . . ? C10 N4 C13 116.0(2) . . ? C10 N4 C12 112.5(2) . . ? C13 N4 C12 131.5(2) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 0.538 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.059 _chemical_name_common (iPr2Im)2(CS-Dibenzothiophenylato)Ni(ii) data_compound6 _database_code_depnum_ccdc_archive 'CCDC 726136' _chemical_name_systematic ; (iPr2Im)2(h2-Benzothiophendioxd)Ni(0) ; _chemical_formula_sum 'C30 H48 N4 Ni O3 S' _chemical_formula_weight 603.49 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' O O 0.0106 0.0060 '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 P2(1)/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 14.196(3) _cell_length_b 12.2093(16) _cell_length_c 18.433(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.03(2) _cell_angle_gamma 90.00 _cell_volume 3190.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 1' _diffrn_measurement_method rotation _diffrn_reflns_number 15077 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.16 _reflns_number_total 5487 _reflns_number_gt 3909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1162P)^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 5487 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Ni1 Ni 0.55526(3) 0.26504(4) 0.82629(3) 0.02434(17) Uani 1 1 d . . . S1 S 0.69773(7) 0.26597(10) 0.95849(6) 0.0375(3) Uani 1 1 d . . . N2 N 0.3770(2) 0.2884(3) 0.9027(2) 0.0330(8) Uani 1 1 d . . . N3 N 0.4280(2) 0.2086(3) 0.7027(2) 0.0322(7) Uani 1 1 d . . . N4 N 0.4819(2) 0.0617(3) 0.75131(19) 0.0313(7) Uani 1 1 d . . . C20 C 0.6943(2) 0.2601(3) 0.8188(2) 0.0339(9) Uani 1 1 d . . . H20A H 0.7202 0.2980 0.7767 0.041 Uiso 1 1 calc R . . C7 C 0.4891(3) 0.5310(4) 0.8432(3) 0.0397(10) Uani 1 1 d . . . H7A H 0.5392 0.4951 0.8164 0.048 Uiso 1 1 calc R . . O2 O 0.6212(2) 0.2362(4) 1.0021(2) 0.0646(11) Uani 1 1 d . . . C10 C 0.4886(2) 0.1730(3) 0.7564(2) 0.0262(8) Uani 1 1 d . . . N1 N 0.4287(2) 0.4443(3) 0.8723(2) 0.0319(7) Uani 1 1 d . . . O1 O 0.7729(2) 0.3281(3) 0.9958(2) 0.0622(12) Uani 1 1 d . . . C11 C 0.3847(3) 0.1223(4) 0.6657(3) 0.0423(11) Uani 1 1 d . . . H11A H 0.3403 0.1272 0.6262 0.051 Uiso 1 1 calc R . . C18 C 0.3037(3) 0.3477(5) 0.7052(4) 0.0600(16) Uani 1 1 d . . . H18A H 0.2936 0.3262 0.7548 0.090 Uiso 1 1 calc R . . H18B H 0.2614 0.3067 0.6722 0.090 Uiso 1 1 calc R . . H18C H 0.2914 0.4254 0.6994 0.090 Uiso 1 1 calc R . . C12 C 0.4182(3) 0.0305(4) 0.6969(3) 0.0410(10) Uani 1 1 d . . . H12A H 0.4013 -0.0416 0.6839 0.049 Uiso 1 1 calc R . . C13 C 0.5336(3) -0.0168(3) 0.7991(3) 0.0402(11) Uani 1 1 d . . . H13A H 0.5739 0.0252 0.8347 0.048 Uiso 1 1 calc R . . C25 C 0.7838(3) 0.0589(4) 0.9538(3) 0.0380(10) Uani 1 1 d . . . H25A H 0.7820 0.0524 1.0045 0.046 Uiso 1 1 calc R . . C26 C 0.7455(2) 0.1490(3) 0.9184(2) 0.0302(8) Uani 1 1 d . . . C24 C 0.8251(3) -0.0224(4) 0.9131(3) 0.0491(13) Uani 1 1 d . . . H24A H 0.8503 -0.0855 0.9361 0.059 Uiso 1 1 calc R . . C1 C 0.4495(2) 0.3356(3) 0.8690(2) 0.0277(8) Uani 1 1 d . . . C21 C 0.7436(2) 0.1610(3) 0.8448(2) 0.0326(9) Uani 1 1 d . . . C22 C 0.7877(3) 0.0801(4) 0.8052(3) 0.0423(11) Uani 1 1 d . . . H22A H 0.7895 0.0871 0.7545 0.051 Uiso 1 1 calc R . . C2 C 0.3463(3) 0.4632(4) 0.9066(3) 0.0446(11) Uani 1 1 d . . . H2B H 0.3186 0.5318 0.9148 0.054 Uiso 1 1 calc R . . C8 C 0.5358(4) 0.5959(5) 0.9050(4) 0.0569(14) Uani 1 1 d . . . H8A H 0.5711 0.5466 0.9376 0.085 Uiso 1 1 calc R . . H8B H 0.4880 0.6332 0.9314 0.085 Uiso 1 1 calc R . . H8C H 0.5783 0.6494 0.8857 0.085 Uiso 1 1 calc R . . C3 C 0.3130(3) 0.3651(4) 0.9263(3) 0.0447(11) Uani 1 1 d . . . H3A H 0.2579 0.3512 0.9509 0.054 Uiso 1 1 calc R . . C23 C 0.8289(3) -0.0100(4) 0.8393(3) 0.0500(13) Uani 1 1 d . . . H23A H 0.8596 -0.0629 0.8120 0.060 Uiso 1 1 calc R . . C5 C 0.2760(4) 0.1254(6) 0.8852(4) 0.0702(18) Uani 1 1 d . . . H5A H 0.2660 0.1449 0.8344 0.105 Uiso 1 1 calc R . . H5B H 0.2260 0.1564 0.9126 0.105 Uiso 1 1 calc R . . H5C H 0.2756 0.0463 0.8901 0.105 Uiso 1 1 calc R . . C17 C 0.4299(4) 0.3532(4) 0.6117(3) 0.0516(13) Uani 1 1 d . . . H17A H 0.4954 0.3356 0.6046 0.077 Uiso 1 1 calc R . . H17B H 0.4198 0.4311 0.6041 0.077 Uiso 1 1 calc R . . H17C H 0.3896 0.3123 0.5773 0.077 Uiso 1 1 calc R . . C4 C 0.3705(3) 0.1700(4) 0.9142(3) 0.0406(10) Uani 1 1 d . . . H4A H 0.4201 0.1347 0.8866 0.049 Uiso 1 1 calc R . . C16 C 0.4063(3) 0.3234(4) 0.6879(2) 0.0369(9) Uani 1 1 d . . . H16A H 0.4474 0.3678 0.7215 0.044 Uiso 1 1 calc R . . C9 C 0.4327(4) 0.6039(5) 0.7904(4) 0.0670(17) Uani 1 1 d . . . H9A H 0.4037 0.5596 0.7517 0.101 Uiso 1 1 calc R . . H9B H 0.4743 0.6574 0.7700 0.101 Uiso 1 1 calc R . . H9C H 0.3841 0.6414 0.8158 0.101 Uiso 1 1 calc R . . C15 C 0.5978(4) -0.0884(5) 0.7545(4) 0.0637(16) Uani 1 1 d . . . H15A H 0.6401 -0.0421 0.7285 0.095 Uiso 1 1 calc R . . H15B H 0.5596 -0.1317 0.7201 0.095 Uiso 1 1 calc R . . H15C H 0.6345 -0.1368 0.7868 0.095 Uiso 1 1 calc R . . C14 C 0.4661(4) -0.0869(4) 0.8410(3) 0.0585(14) Uani 1 1 d . . . H14A H 0.4264 -0.0399 0.8688 0.088 Uiso 1 1 calc R . . H14B H 0.5021 -0.1353 0.8738 0.088 Uiso 1 1 calc R . . H14C H 0.4270 -0.1302 0.8072 0.088 Uiso 1 1 calc R . . C6 C 0.3892(4) 0.1417(5) 0.9926(3) 0.0586(14) Uani 1 1 d . . . H6A H 0.4499 0.1712 1.0094 0.088 Uiso 1 1 calc R . . H6B H 0.3896 0.0628 0.9983 0.088 Uiso 1 1 calc R . . H6C H 0.3401 0.1730 1.0209 0.088 Uiso 1 1 calc R . . C19 C 0.6636(3) 0.3285(3) 0.8771(3) 0.0349(9) Uani 1 1 d . . . H19A H 0.6729 0.4086 0.8731 0.042 Uiso 1 1 calc R . . O3 O 0.0983(2) 0.2960(3) 0.0060(2) 0.0528(9) Uani 1 1 d . . . C30 C 0.0195(4) 0.3094(6) -0.0428(4) 0.073(2) Uani 1 1 d . . . H30A H 0.0286 0.3733 -0.0738 0.088 Uiso 1 1 calc R . . H30B H -0.0373 0.3213 -0.0158 0.088 Uiso 1 1 calc R . . C29 C 0.1121(4) 0.3866(6) 0.0533(4) 0.078(2) Uani 1 1 d . . . H29A H 0.0530 0.4038 0.0759 0.093 Uiso 1 1 calc R . . H29B H 0.1308 0.4508 0.0256 0.093 Uiso 1 1 calc R . . C28 C 0.1844(6) 0.3618(8) 0.1088(5) 0.100(3) Uani 1 1 d . . . H28A H 0.1934 0.4243 0.1409 0.150 Uiso 1 1 calc R . . H28B H 0.2430 0.3456 0.0863 0.150 Uiso 1 1 calc R . . H28C H 0.1654 0.2987 0.1366 0.150 Uiso 1 1 calc R . . C27 C 0.0085(5) 0.2098(9) -0.0878(5) 0.097(3) Uani 1 1 d . . . H27A H -0.0457 0.2179 -0.1216 0.145 Uiso 1 1 calc R . . H27B H -0.0007 0.1470 -0.0567 0.145 Uiso 1 1 calc R . . H27C H 0.0648 0.1989 -0.1145 0.145 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 0.0212(2) 0.0224(3) 0.0289(3) -0.00042(19) -0.00299(17) 0.00120(16) S1 0.0305(5) 0.0463(7) 0.0347(6) -0.0120(5) -0.0067(4) 0.0076(4) N2 0.0281(15) 0.038(2) 0.0337(19) -0.0039(14) 0.0045(13) -0.0004(12) N3 0.0291(15) 0.029(2) 0.037(2) 0.0005(14) -0.0073(13) 0.0000(12) N4 0.0311(15) 0.027(2) 0.0349(19) -0.0011(14) -0.0056(13) 0.0003(12) C20 0.0257(17) 0.038(3) 0.038(2) 0.0067(18) 0.0001(15) -0.0027(14) C7 0.043(2) 0.026(2) 0.050(3) -0.0013(18) 0.0028(18) 0.0062(16) O2 0.0445(18) 0.100(3) 0.050(2) 0.000(2) 0.0100(16) 0.0191(18) C10 0.0225(16) 0.026(2) 0.030(2) -0.0028(15) 0.0021(14) 0.0024(12) N1 0.0328(15) 0.027(2) 0.035(2) -0.0049(14) -0.0010(13) 0.0064(12) O1 0.0562(19) 0.056(2) 0.070(3) -0.0281(19) -0.0366(19) 0.0123(16) C11 0.039(2) 0.038(3) 0.048(3) -0.007(2) -0.0125(19) -0.0040(17) C18 0.043(2) 0.045(3) 0.091(5) 0.011(3) -0.006(3) 0.018(2) C12 0.043(2) 0.031(3) 0.048(3) -0.0088(19) -0.0083(18) -0.0057(16) C13 0.044(2) 0.021(2) 0.054(3) 0.0009(18) -0.0120(19) 0.0028(15) C25 0.035(2) 0.040(3) 0.038(2) 0.0050(18) -0.0023(16) -0.0012(16) C26 0.0236(16) 0.032(2) 0.034(2) -0.0053(16) -0.0009(14) -0.0035(13) C24 0.040(2) 0.035(3) 0.071(4) 0.002(2) -0.007(2) 0.0087(17) C1 0.0288(17) 0.027(2) 0.027(2) -0.0025(15) -0.0064(14) 0.0022(13) C21 0.0196(15) 0.038(2) 0.040(2) -0.0002(17) -0.0011(14) -0.0020(13) C22 0.0318(19) 0.063(3) 0.032(2) -0.009(2) 0.0031(16) 0.0104(18) C2 0.038(2) 0.044(3) 0.051(3) -0.013(2) -0.0017(19) 0.0151(18) C8 0.053(3) 0.042(3) 0.076(4) -0.017(3) -0.004(2) -0.005(2) C3 0.032(2) 0.056(3) 0.047(3) -0.013(2) 0.0080(18) 0.0061(18) C23 0.039(2) 0.050(3) 0.060(4) -0.020(2) -0.002(2) 0.0136(19) C5 0.075(4) 0.072(4) 0.061(4) -0.001(3) -0.014(3) -0.038(3) C17 0.061(3) 0.045(3) 0.046(3) 0.011(2) -0.012(2) -0.012(2) C4 0.045(2) 0.036(3) 0.042(3) -0.0047(19) 0.0089(18) -0.0105(17) C16 0.041(2) 0.032(3) 0.037(2) 0.0043(17) -0.0113(17) 0.0022(16) C9 0.083(4) 0.037(3) 0.078(5) 0.014(3) -0.020(3) 0.004(2) C15 0.048(3) 0.043(3) 0.100(5) -0.005(3) 0.001(3) 0.017(2) C14 0.078(3) 0.034(3) 0.064(4) 0.012(2) 0.008(3) 0.004(2) C6 0.069(3) 0.053(4) 0.053(3) 0.006(2) -0.008(3) -0.021(2) C19 0.0281(18) 0.026(2) 0.050(3) -0.0036(17) -0.0067(16) -0.0017(14) O3 0.0411(16) 0.062(2) 0.055(2) -0.0076(17) 0.0040(14) 0.0011(14) C30 0.048(3) 0.098(5) 0.074(5) 0.034(4) 0.002(3) 0.000(3) C29 0.069(4) 0.077(5) 0.090(6) -0.029(4) 0.034(3) -0.002(3) C28 0.097(5) 0.144(8) 0.060(5) -0.043(5) 0.016(4) -0.037(5) C27 0.064(4) 0.149(8) 0.076(5) -0.016(5) -0.014(3) -0.018(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 Ni1 C10 1.920(4) . ? Ni1 C19 1.922(4) . ? Ni1 C1 1.934(4) . ? Ni1 C20 1.987(4) . ? S1 O2 1.432(4) . ? S1 O1 1.452(3) . ? S1 C19 1.729(5) . ? S1 C26 1.760(4) . ? N2 C1 1.359(5) . ? N2 C3 1.390(6) . ? N2 C4 1.466(6) . ? N3 C10 1.349(5) . ? N3 C11 1.382(5) . ? N3 C16 1.457(6) . ? N4 C10 1.365(5) . ? N4 C12 1.368(5) . ? N4 C13 1.471(5) . ? C20 C19 1.447(6) . ? C20 C21 1.466(6) . ? C20 H20A 0.9900 . ? C7 N1 1.481(6) . ? C7 C8 1.512(7) . ? C7 C9 1.515(7) . ? C7 H7A 0.9900 . ? N1 C1 1.362(5) . ? N1 C2 1.379(6) . ? C11 C12 1.335(7) . ? C11 H11A 0.9400 . ? C18 C16 1.536(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C12 H12A 0.9400 . ? C13 C14 1.525(7) . ? C13 C15 1.533(7) . ? C13 H13A 0.9900 . ? C25 C26 1.376(6) . ? C25 C24 1.393(7) . ? C25 H25A 0.9400 . ? C26 C21 1.363(6) . ? C24 C23 1.373(8) . ? C24 H24A 0.9400 . ? C21 C22 1.395(6) . ? C22 C23 1.382(7) . ? C22 H22A 0.9400 . ? C2 C3 1.345(8) . ? C2 H2B 0.9400 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C3 H3A 0.9400 . ? C23 H23A 0.9400 . ? C5 C4 1.519(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C17 C16 1.506(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C4 C6 1.495(8) . ? C4 H4A 0.9900 . ? C16 H16A 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C19 H19A 0.9900 . ? O3 C30 1.407(7) . ? O3 C29 1.416(8) . ? C30 C27 1.476(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C29 C28 1.443(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? 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 C10 Ni1 C19 156.40(17) . . ? C10 Ni1 C1 99.70(15) . . ? C19 Ni1 C1 103.89(17) . . ? C10 Ni1 C20 113.06(17) . . ? C19 Ni1 C20 43.40(18) . . ? C1 Ni1 C20 146.82(17) . . ? O2 S1 O1 115.3(3) . . ? O2 S1 C19 114.4(2) . . ? O1 S1 C19 110.2(2) . . ? O2 S1 C26 110.5(2) . . ? O1 S1 C26 109.44(19) . . ? C19 S1 C26 95.2(2) . . ? C1 N2 C3 112.4(4) . . ? C1 N2 C4 122.7(3) . . ? C3 N2 C4 124.9(4) . . ? C10 N3 C11 111.5(3) . . ? C10 N3 C16 124.6(3) . . ? C11 N3 C16 123.9(3) . . ? C10 N4 C12 111.7(3) . . ? C10 N4 C13 125.2(3) . . ? C12 N4 C13 123.2(4) . . ? C19 C20 C21 113.0(4) . . ? C19 C20 Ni1 65.9(2) . . ? C21 C20 Ni1 117.5(3) . . ? C19 C20 H20A 116.8 . . ? C21 C20 H20A 116.8 . . ? Ni1 C20 H20A 116.8 . . ? N1 C7 C8 109.9(4) . . ? N1 C7 C9 110.9(4) . . ? C8 C7 C9 111.8(5) . . ? N1 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? C9 C7 H7A 108.0 . . ? N3 C10 N4 103.3(3) . . ? N3 C10 Ni1 125.2(3) . . ? N4 C10 Ni1 131.3(3) . . ? C1 N1 C2 112.1(4) . . ? C1 N1 C7 123.3(3) . . ? C2 N1 C7 124.6(4) . . ? C12 C11 N3 106.8(4) . . ? C12 C11 H11A 126.6 . . ? N3 C11 H11A 126.6 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C12 N4 106.8(4) . . ? C11 C12 H12A 126.6 . . ? N4 C12 H12A 126.6 . . ? N4 C13 C14 111.2(4) . . ? N4 C13 C15 110.1(4) . . ? C14 C13 C15 111.0(4) . . ? N4 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? C15 C13 H13A 108.1 . . ? C26 C25 C24 118.8(4) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C21 C26 C25 123.0(4) . . ? C21 C26 S1 110.1(3) . . ? C25 C26 S1 126.9(4) . . ? C23 C24 C25 119.7(4) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? N2 C1 N1 102.8(3) . . ? N2 C1 Ni1 128.4(3) . . ? N1 C1 Ni1 128.9(3) . . ? C26 C21 C22 117.3(4) . . ? C26 C21 C20 113.4(4) . . ? C22 C21 C20 129.3(4) . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C3 C2 N1 107.0(4) . . ? C3 C2 H2B 126.5 . . ? N1 C2 H2B 126.5 . . ? 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 . . ? C2 C3 N2 105.7(4) . . ? C2 C3 H3A 127.1 . . ? N2 C3 H3A 127.1 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C4 C6 111.0(4) . . ? N2 C4 C5 111.3(4) . . ? C6 C4 C5 111.5(4) . . ? N2 C4 H4A 107.6 . . ? C6 C4 H4A 107.6 . . ? C5 C4 H4A 107.6 . . ? N3 C16 C17 110.6(4) . . ? N3 C16 C18 109.9(4) . . ? C17 C16 C18 114.0(4) . . ? N3 C16 H16A 107.4 . . ? C17 C16 H16A 107.4 . . ? C18 C16 H16A 107.4 . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C20 C19 S1 107.9(3) . . ? C20 C19 Ni1 70.7(2) . . ? S1 C19 Ni1 115.1(2) . . ? C20 C19 H19A 117.9 . . ? S1 C19 H19A 117.9 . . ? Ni1 C19 H19A 117.9 . . ? C30 O3 C29 112.4(5) . . ? O3 C30 C27 108.6(6) . . ? O3 C30 H30A 110.0 . . ? C27 C30 H30A 110.0 . . ? O3 C30 H30B 110.0 . . ? C27 C30 H30B 110.0 . . ? H30A C30 H30B 108.3 . . ? O3 C29 C28 110.1(6) . . ? O3 C29 H29A 109.6 . . ? C28 C29 H29A 109.6 . . ? O3 C29 H29B 109.6 . . ? C28 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C27 H27A 109.5 . . ? C30 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C30 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.664 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.136 _chemical_name_common (iPr2Im)2(h2-Benzothiophendioxd)Ni(0) data_compound8 _database_code_depnum_ccdc_archive 'CCDC 726137' _chemical_name_systematic ; (iPr2Im)2(H)(StBu)Ni(II) ; _chemical_formula_sum 'C22 H42 N4 Ni S' _chemical_formula_weight 453.37 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7691(18) _cell_length_b 9.2488(18) _cell_length_c 17.285(4) _cell_angle_alpha 95.40(3) _cell_angle_beta 91.24(3) _cell_angle_gamma 109.25(3) _cell_volume 1315.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5688 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.9 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 1' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 8073 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4755 _reflns_number_gt 3420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0633P)^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 4755 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 S1 S 0.43071(10) 1.06634(9) 0.77578(7) 0.0434(3) Uani 1 1 d . . . Ni1 Ni 0.53653(4) 0.88117(4) 0.74649(3) 0.02269(13) Uani 1 1 d . . . H1 H 0.594(5) 0.755(5) 0.729(3) 0.057(12) Uiso 1 1 d . . . N1 N 0.8875(3) 1.0105(3) 0.75919(17) 0.0285(6) Uani 1 1 d . . . N2 N 0.7966(3) 0.9996(3) 0.64198(17) 0.0313(6) Uani 1 1 d . . . N3 N 0.2224(3) 0.6345(3) 0.72904(17) 0.0305(6) Uani 1 1 d . . . N4 N 0.3076(3) 0.6952(3) 0.84794(18) 0.0311(6) Uani 1 1 d . . . C1 C 0.7474(3) 0.9740(3) 0.7151(2) 0.0255(7) Uani 1 1 d . . . C2 C 1.0210(4) 1.0538(4) 0.7138(2) 0.0378(9) Uani 1 1 d . . . H2A H 1.1302 1.0819 0.7312 0.045 Uiso 1 1 calc R . . C3 C 0.9645(4) 1.0478(4) 0.6408(2) 0.0423(9) Uani 1 1 d . . . H3A H 1.0262 1.0715 0.5971 0.051 Uiso 1 1 calc R . . C4 C 0.6860(4) 0.9548(5) 0.5734(2) 0.0426(9) Uani 1 1 d . . . H4A H 0.5775 0.9507 0.5901 0.051 Uiso 1 1 calc R . . C5 C 0.7355(6) 1.0707(6) 0.5149(3) 0.0611(12) Uani 1 1 d . . . H5A H 0.7404 1.1712 0.5391 0.092 Uiso 1 1 calc R . . H5B H 0.6568 1.0398 0.4710 0.092 Uiso 1 1 calc R . . H5C H 0.8410 1.0757 0.4971 0.092 Uiso 1 1 calc R . . C6 C 0.6742(6) 0.7938(6) 0.5375(3) 0.0662(14) Uani 1 1 d . . . H6A H 0.6415 0.7218 0.5763 0.099 Uiso 1 1 calc R . . H6B H 0.7787 0.7954 0.5195 0.099 Uiso 1 1 calc R . . H6C H 0.5947 0.7618 0.4938 0.099 Uiso 1 1 calc R . . C7 C 0.8931(4) 0.9863(4) 0.8413(2) 0.0356(8) Uani 1 1 d . . . H7A H 0.7876 0.9820 0.8622 0.043 Uiso 1 1 calc R . . C8 C 0.9159(6) 0.8303(5) 0.8484(3) 0.0646(14) Uani 1 1 d . . . H8A H 0.8298 0.7494 0.8181 0.097 Uiso 1 1 calc R . . H8B H 0.9129 0.8105 0.9026 0.097 Uiso 1 1 calc R . . H8C H 1.0195 0.8324 0.8290 0.097 Uiso 1 1 calc R . . C9 C 1.0240(5) 1.1188(5) 0.8876(3) 0.0473(10) Uani 1 1 d . . . H9A H 1.0038 1.2144 0.8822 0.071 Uiso 1 1 calc R . . H9B H 1.1287 1.1252 0.8682 0.071 Uiso 1 1 calc R . . H9C H 1.0232 1.1013 0.9421 0.071 Uiso 1 1 calc R . . C10 C 0.3459(4) 0.7342(3) 0.7760(2) 0.0259(7) Uani 1 1 d . . . C11 C 0.1124(4) 0.5335(4) 0.7722(2) 0.0385(9) Uani 1 1 d . . . H11A H 0.0184 0.4531 0.7527 0.046 Uiso 1 1 calc R . . C12 C 0.1649(4) 0.5717(4) 0.8459(2) 0.0395(9) Uani 1 1 d . . . H12A H 0.1149 0.5243 0.8888 0.047 Uiso 1 1 calc R . . C13 C 0.4042(4) 0.7770(4) 0.9186(2) 0.0369(8) Uani 1 1 d . . . H13A H 0.4933 0.8653 0.9030 0.044 Uiso 1 1 calc R . . C14 C 0.4803(6) 0.6734(6) 0.9572(3) 0.0648(13) Uani 1 1 d . . . H14A H 0.5438 0.6360 0.9201 0.097 Uiso 1 1 calc R . . H14B H 0.3956 0.5867 0.9741 0.097 Uiso 1 1 calc R . . H14C H 0.5497 0.7316 1.0018 0.097 Uiso 1 1 calc R . . C15 C 0.3033(5) 0.8417(5) 0.9741(3) 0.0522(11) Uani 1 1 d . . . H15A H 0.2588 0.9078 0.9474 0.078 Uiso 1 1 calc R . . H15B H 0.3713 0.9008 1.0189 0.078 Uiso 1 1 calc R . . H15C H 0.2158 0.7574 0.9911 0.078 Uiso 1 1 calc R . . C16 C 0.2109(4) 0.6351(4) 0.6445(2) 0.0423(9) Uani 1 1 d . . . H16A H 0.2940 0.7305 0.6316 0.051 Uiso 1 1 calc R . . C17 C 0.2507(7) 0.4999(6) 0.6039(3) 0.0756(16) Uani 1 1 d . . . H17A H 0.3566 0.5028 0.6230 0.113 Uiso 1 1 calc R . . H17B H 0.2508 0.5065 0.5482 0.113 Uiso 1 1 calc R . . H17C H 0.1701 0.4043 0.6146 0.113 Uiso 1 1 calc R . . C18 C 0.0461(6) 0.6422(6) 0.6183(3) 0.0670(14) Uani 1 1 d . . . H18A H 0.0287 0.7309 0.6463 0.101 Uiso 1 1 calc R . . H18B H -0.0383 0.5490 0.6290 0.101 Uiso 1 1 calc R . . H18C H 0.0434 0.6513 0.5629 0.101 Uiso 1 1 calc R . . C19 C 0.5511(4) 1.2685(4) 0.7655(2) 0.0319(8) Uani 1 1 d . . . C20 C 0.6055(7) 1.2919(5) 0.6849(3) 0.0708(15) Uani 1 1 d . . . H20A H 0.6679 1.3995 0.6827 0.106 Uiso 1 1 calc R . . H20B H 0.5117 1.2625 0.6486 0.106 Uiso 1 1 calc R . . H20C H 0.6720 1.2289 0.6711 0.106 Uiso 1 1 calc R . . C21 C 0.6978(5) 1.3211(5) 0.8209(3) 0.0561(12) Uani 1 1 d . . . H21A H 0.7603 1.4272 0.8148 0.084 Uiso 1 1 calc R . . H21B H 0.7637 1.2564 0.8098 0.084 Uiso 1 1 calc R . . H21C H 0.6641 1.3138 0.8739 0.084 Uiso 1 1 calc R . . C22 C 0.4434(5) 1.3645(4) 0.7892(3) 0.0556(12) Uani 1 1 d . . . H22A H 0.5014 1.4722 0.7846 0.083 Uiso 1 1 calc R . . H22B H 0.4150 1.3518 0.8427 0.083 Uiso 1 1 calc R . . H22C H 0.3457 1.3301 0.7554 0.083 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 S1 0.0212(4) 0.0223(4) 0.0876(8) 0.0085(4) 0.0120(4) 0.0072(3) Ni1 0.01889(19) 0.0210(2) 0.0274(3) 0.00364(14) 0.00213(14) 0.00519(14) N1 0.0205(12) 0.0297(14) 0.0342(18) 0.0042(11) 0.0001(11) 0.0067(10) N2 0.0262(13) 0.0409(16) 0.0287(19) 0.0039(12) 0.0082(11) 0.0130(12) N3 0.0261(13) 0.0268(14) 0.0333(19) 0.0029(11) 0.0015(11) 0.0019(11) N4 0.0319(14) 0.0257(14) 0.0330(19) 0.0055(11) 0.0062(12) 0.0051(11) C1 0.0242(15) 0.0225(15) 0.032(2) 0.0028(13) 0.0030(13) 0.0105(12) C2 0.0185(15) 0.048(2) 0.045(3) 0.0034(17) 0.0071(15) 0.0089(14) C3 0.0268(17) 0.055(2) 0.042(3) 0.0060(18) 0.0163(16) 0.0076(16) C4 0.0384(19) 0.070(3) 0.025(2) 0.0062(18) 0.0033(15) 0.0244(18) C5 0.064(3) 0.095(4) 0.037(3) 0.023(2) 0.014(2) 0.039(3) C6 0.081(3) 0.070(3) 0.037(3) -0.010(2) -0.006(2) 0.016(3) C7 0.0313(17) 0.0400(19) 0.034(2) 0.0057(15) -0.0025(14) 0.0089(14) C8 0.077(3) 0.048(3) 0.064(3) 0.012(2) -0.021(3) 0.016(2) C9 0.042(2) 0.056(2) 0.039(3) -0.0021(18) -0.0072(17) 0.0132(18) C10 0.0259(15) 0.0224(15) 0.031(2) 0.0024(13) 0.0024(13) 0.0098(12) C11 0.0276(17) 0.0283(17) 0.052(3) 0.0055(16) 0.0090(16) -0.0019(13) C12 0.0385(19) 0.0290(18) 0.047(3) 0.0108(16) 0.0170(17) 0.0027(14) C13 0.0382(18) 0.0375(19) 0.031(2) 0.0022(15) 0.0013(15) 0.0082(15) C14 0.083(3) 0.074(3) 0.048(3) 0.002(2) -0.009(2) 0.043(3) C15 0.062(3) 0.052(2) 0.044(3) -0.0050(19) 0.006(2) 0.023(2) C16 0.0401(19) 0.037(2) 0.038(3) 0.0015(16) -0.0058(16) -0.0014(15) C17 0.101(4) 0.079(4) 0.045(3) -0.015(3) 0.006(3) 0.034(3) C18 0.058(3) 0.075(3) 0.066(4) 0.017(3) -0.015(2) 0.018(2) C19 0.0323(17) 0.0223(16) 0.042(2) 0.0093(14) 0.0055(15) 0.0089(13) C20 0.119(4) 0.046(3) 0.053(4) 0.017(2) 0.020(3) 0.032(3) C21 0.045(2) 0.040(2) 0.077(4) 0.007(2) -0.004(2) 0.0062(18) C22 0.043(2) 0.0276(19) 0.101(4) 0.008(2) 0.017(2) 0.0176(16) _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 S1 C19 1.847(3) . ? S1 Ni1 2.2260(11) . ? Ni1 C1 1.880(3) . ? Ni1 C10 1.890(3) . ? Ni1 H1 1.43(4) . ? N1 C1 1.358(4) . ? N1 C2 1.392(4) . ? N1 C7 1.460(5) . ? N2 C1 1.360(5) . ? N2 C3 1.391(4) . ? N2 C4 1.453(5) . ? N3 C10 1.358(4) . ? N3 C11 1.389(4) . ? N3 C16 1.462(5) . ? N4 C10 1.347(5) . ? N4 C12 1.385(4) . ? N4 C13 1.463(5) . ? C2 C3 1.334(6) . ? C2 H2A 0.9400 . ? C3 H3A 0.9400 . ? C4 C5 1.508(6) . ? C4 C6 1.528(6) . ? C4 H4A 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C9 1.519(5) . ? C7 C8 1.536(6) . ? C7 H7A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C11 C12 1.319(6) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 C14 1.526(6) . ? C13 C15 1.529(5) . ? C13 H13A 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C17 1.520(6) . ? C16 C18 1.529(6) . ? C16 H16A 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.494(6) . ? C19 C21 1.502(5) . ? C19 C22 1.532(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? 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 C19 S1 Ni1 119.63(12) . . ? C1 Ni1 C10 162.23(12) . . ? C1 Ni1 S1 107.89(10) . . ? C10 Ni1 S1 89.74(10) . . ? C1 Ni1 H1 75.8(16) . . ? C10 Ni1 H1 86.6(17) . . ? S1 Ni1 H1 176.3(17) . . ? C1 N1 C2 111.1(3) . . ? C1 N1 C7 123.2(3) . . ? C2 N1 C7 125.2(3) . . ? C1 N2 C3 111.1(3) . . ? C1 N2 C4 123.0(3) . . ? C3 N2 C4 125.0(3) . . ? C10 N3 C11 110.7(3) . . ? C10 N3 C16 123.6(3) . . ? C11 N3 C16 125.7(3) . . ? C10 N4 C12 111.4(3) . . ? C10 N4 C13 123.4(3) . . ? C12 N4 C13 125.2(3) . . ? N1 C1 N2 104.0(3) . . ? N1 C1 Ni1 126.9(3) . . ? N2 C1 Ni1 128.5(2) . . ? C3 C2 N1 107.0(3) . . ? C3 C2 H2A 126.5 . . ? N1 C2 H2A 126.5 . . ? C2 C3 N2 106.8(3) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N2 C4 C5 111.6(3) . . ? N2 C4 C6 109.9(3) . . ? C5 C4 C6 111.4(4) . . ? N2 C4 H4A 107.9 . . ? C5 C4 H4A 107.9 . . ? C6 C4 H4A 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C9 111.1(3) . . ? N1 C7 C8 109.0(3) . . ? C9 C7 C8 112.3(3) . . ? N1 C7 H7A 108.1 . . ? C9 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? 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 . . ? N4 C10 N3 103.9(3) . . ? N4 C10 Ni1 127.9(2) . . ? N3 C10 Ni1 128.0(3) . . ? C12 C11 N3 107.0(3) . . ? C12 C11 H11A 126.5 . . ? N3 C11 H11A 126.5 . . ? C11 C12 N4 106.9(3) . . ? C11 C12 H12A 126.5 . . ? N4 C12 H12A 126.5 . . ? N4 C13 C14 110.7(3) . . ? N4 C13 C15 110.8(3) . . ? C14 C13 C15 112.4(4) . . ? N4 C13 H13A 107.6 . . ? C14 C13 H13A 107.6 . . ? C15 C13 H13A 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 110.5(4) . . ? N3 C16 C18 110.3(4) . . ? C17 C16 C18 113.8(4) . . ? N3 C16 H16A 107.3 . . ? C17 C16 H16A 107.3 . . ? C18 C16 H16A 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 108.5(4) . . ? C20 C19 C22 111.1(4) . . ? C21 C19 C22 107.9(3) . . ? C20 C19 S1 112.8(3) . . ? C21 C19 S1 110.2(3) . . ? C22 C19 S1 106.3(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.416 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.081 _chemical_name_common (iPr2Im)2(H)(StBu)Ni(ii) data_compound9 _database_code_depnum_ccdc_archive 'CCDC 726138' _chemical_name_systematic ; (iPr2Im)2(StBu)2Ni(II) 9 ; _chemical_formula_sum 'C26 H50 N4 Ni S2' _chemical_formula_weight 541.53 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.226(2) _cell_length_b 10.628(2) _cell_length_c 23.097(5) _cell_angle_alpha 84.85(3) _cell_angle_beta 86.66(3) _cell_angle_gamma 68.22(3) _cell_volume 2320.8(8) _cell_formula_units_Z 3 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 STADI 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 8026 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.06 _reflns_number_total 8026 _reflns_number_gt 5692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1495P)^2^+7.2559P] 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 8026 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2704 _refine_ls_wR_factor_gt 0.2167 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Ni1 Ni -0.40930(8) -0.34031(7) 0.83025(3) 0.0301(3) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.5000 0.0302(3) Uani 1 2 d S . . S1 S -0.58829(18) -0.24841(15) 0.89290(7) 0.0382(4) Uani 1 1 d . . . S2 S -0.2062(2) -0.43217(17) 0.78055(9) 0.0477(5) Uani 1 1 d . . . S3 S 0.17397(19) -0.10772(17) 0.43872(8) 0.0425(4) Uani 1 1 d . . . N1 N -0.3152(6) -0.1176(5) 0.8374(3) 0.0409(13) Uani 1 1 d . . . N2 N -0.4114(6) -0.0954(6) 0.7548(3) 0.0438(14) Uani 1 1 d . . . N3 N -0.5059(6) -0.5721(5) 0.8526(2) 0.0349(12) Uani 1 1 d . . . N4 N -0.3423(6) -0.5825(5) 0.9091(2) 0.0347(12) Uani 1 1 d . . . N5 N 0.0254(6) -0.2211(6) 0.5947(2) 0.0413(13) Uani 1 1 d . . . N6 N -0.0873(5) -0.2282(5) 0.5205(2) 0.0347(12) Uani 1 1 d . . . C1 C -0.3847(7) -0.1734(6) 0.8050(3) 0.0345(14) Uani 1 1 d . . . C2 C -0.3007(9) -0.0059(7) 0.8060(4) 0.057(2) Uani 1 1 d . . . H2A H -0.2565 0.0497 0.8186 0.068 Uiso 1 1 calc R . . C3 C -0.3604(9) 0.0089(7) 0.7546(4) 0.056(2) Uani 1 1 d . . . H3A H -0.3667 0.0764 0.7245 0.068 Uiso 1 1 calc R . . C4 C -0.4827(8) -0.1186(8) 0.7064(3) 0.0521(19) Uani 1 1 d . . . H4A H -0.5198 -0.1905 0.7197 0.063 Uiso 1 1 calc R . . C5 C -0.6072(10) 0.0093(10) 0.6872(4) 0.079(3) Uani 1 1 d . . . H5A H -0.6727 0.0381 0.7198 0.119 Uiso 1 1 calc R . . H5B H -0.6545 -0.0102 0.6559 0.119 Uiso 1 1 calc R . . H5C H -0.5732 0.0811 0.6737 0.119 Uiso 1 1 calc R . . C6 C -0.3778(11) -0.1697(11) 0.6564(4) 0.080(3) Uani 1 1 d . . . H6A H -0.3008 -0.2511 0.6699 0.119 Uiso 1 1 calc R . . H6B H -0.3412 -0.1002 0.6421 0.119 Uiso 1 1 calc R . . H6C H -0.4245 -0.1904 0.6252 0.119 Uiso 1 1 calc R . . C7 C -0.2549(7) -0.1754(6) 0.8937(3) 0.0452(17) Uani 1 1 d . . . H7A H -0.2975 -0.2423 0.9084 0.054 Uiso 1 1 calc R . . C8 C -0.2923(12) -0.0691(10) 0.9374(4) 0.082(3) Uani 1 1 d . . . H8A H -0.3938 -0.0233 0.9399 0.123 Uiso 1 1 calc R . . H8B H -0.2491 -0.0035 0.9252 0.123 Uiso 1 1 calc R . . H8C H -0.2580 -0.1124 0.9752 0.123 Uiso 1 1 calc R . . C9 C -0.0977(9) -0.2527(11) 0.8866(5) 0.080(3) Uani 1 1 d . . . H9A H -0.0807 -0.3195 0.8583 0.120 Uiso 1 1 calc R . . H9B H -0.0601 -0.2984 0.9237 0.120 Uiso 1 1 calc R . . H9C H -0.0518 -0.1898 0.8734 0.120 Uiso 1 1 calc R . . C10 C -0.4189(6) -0.5065(6) 0.8635(3) 0.0311(13) Uani 1 1 d . . . C11 C -0.4835(8) -0.6863(7) 0.8909(3) 0.0436(16) Uani 1 1 d . . . H11A H -0.5311 -0.7471 0.8918 0.052 Uiso 1 1 calc R . . C12 C -0.3816(8) -0.6933(7) 0.9262(3) 0.0429(16) Uani 1 1 d . . . H12A H -0.3437 -0.7598 0.9566 0.051 Uiso 1 1 calc R . . C13 C -0.2372(7) -0.5475(7) 0.9379(3) 0.0458(17) Uani 1 1 d . . . H13A H -0.2130 -0.4802 0.9115 0.055 Uiso 1 1 calc R . . C14 C -0.1024(9) -0.6701(9) 0.9486(5) 0.077(3) Uani 1 1 d . . . H14A H -0.0653 -0.7096 0.9121 0.115 Uiso 1 1 calc R . . H14B H -0.1222 -0.7369 0.9753 0.115 Uiso 1 1 calc R . . H14C H -0.0335 -0.6419 0.9652 0.115 Uiso 1 1 calc R . . C15 C -0.2995(9) -0.4804(9) 0.9939(3) 0.058(2) Uani 1 1 d . . . H15A H -0.3847 -0.4022 0.9854 0.088 Uiso 1 1 calc R . . H15B H -0.2317 -0.4513 1.0108 0.088 Uiso 1 1 calc R . . H15C H -0.3218 -0.5449 1.0212 0.088 Uiso 1 1 calc R . . C16 C -0.6155(8) -0.5245(7) 0.8086(3) 0.0446(17) Uani 1 1 d . . . H16A H -0.6081 -0.4425 0.7870 0.054 Uiso 1 1 calc R . . C17 C -0.7620(8) -0.4829(9) 0.8379(4) 0.061(2) Uani 1 1 d . . . H17A H -0.7722 -0.4155 0.8653 0.092 Uiso 1 1 calc R . . H17B H -0.7735 -0.5620 0.8585 0.092 Uiso 1 1 calc R . . H17C H -0.8332 -0.4448 0.8087 0.092 Uiso 1 1 calc R . . C18 C -0.5937(10) -0.6301(8) 0.7646(4) 0.062(2) Uani 1 1 d . . . H18A H -0.5007 -0.6528 0.7465 0.092 Uiso 1 1 calc R . . H18B H -0.6644 -0.5934 0.7351 0.092 Uiso 1 1 calc R . . H18C H -0.6022 -0.7113 0.7844 0.092 Uiso 1 1 calc R . . C19 C -0.7262(7) -0.0814(7) 0.8726(3) 0.0403(15) Uani 1 1 d . . . C20 C -0.7926(9) -0.0867(9) 0.8164(4) 0.062(2) Uani 1 1 d . . . H20A H -0.8646 0.0013 0.8062 0.094 Uiso 1 1 calc R . . H20B H -0.8349 -0.1551 0.8214 0.094 Uiso 1 1 calc R . . H20C H -0.7209 -0.1096 0.7856 0.094 Uiso 1 1 calc R . . C21 C -0.8360(8) -0.0599(8) 0.9221(4) 0.057(2) Uani 1 1 d . . . H21A H -0.9125 0.0266 0.9147 0.085 Uiso 1 1 calc R . . H21B H -0.7929 -0.0603 0.9584 0.085 Uiso 1 1 calc R . . H21C H -0.8725 -0.1325 0.9246 0.085 Uiso 1 1 calc R . . C22 C -0.6730(8) 0.0360(7) 0.8686(4) 0.058(2) Uani 1 1 d . . . H22A H -0.7498 0.1204 0.8581 0.087 Uiso 1 1 calc R . . H22B H -0.5980 0.0203 0.8393 0.087 Uiso 1 1 calc R . . H22C H -0.6376 0.0417 0.9060 0.087 Uiso 1 1 calc R . . C23 C -0.1500(8) -0.5988(7) 0.7494(3) 0.0458(17) Uani 1 1 d . . . C24 C -0.1726(10) -0.7123(7) 0.7876(4) 0.061(2) Uani 1 1 d . . . H24A H -0.1388 -0.7947 0.7671 0.092 Uiso 1 1 calc R . . H24B H -0.2723 -0.6877 0.7969 0.092 Uiso 1 1 calc R . . H24C H -0.1213 -0.7273 0.8232 0.092 Uiso 1 1 calc R . . C25 C 0.0069(10) -0.6396(9) 0.7363(5) 0.081(3) Uani 1 1 d . . . H25A H 0.0425 -0.7271 0.7197 0.121 Uiso 1 1 calc R . . H25B H 0.0551 -0.6459 0.7720 0.121 Uiso 1 1 calc R . . H25C H 0.0231 -0.5719 0.7089 0.121 Uiso 1 1 calc R . . C26 C -0.2237(14) -0.5806(11) 0.6930(5) 0.100(4) Uani 1 1 d . . . H26A H -0.1946 -0.6672 0.6759 0.149 Uiso 1 1 calc R . . H26B H -0.1993 -0.5162 0.6665 0.149 Uiso 1 1 calc R . . H26C H -0.3248 -0.5466 0.7003 0.149 Uiso 1 1 calc R . . C27 C -0.0161(6) -0.1584(6) 0.5416(3) 0.0323(13) Uani 1 1 d . . . C28 C -0.0206(9) -0.3297(8) 0.6053(4) 0.059(2) Uani 1 1 d . . . H28A H -0.0045 -0.3897 0.6389 0.071 Uiso 1 1 calc R . . C29 C -0.0911(8) -0.3327(7) 0.5594(3) 0.0509(18) Uani 1 1 d . . . H29A H -0.1351 -0.3944 0.5544 0.061 Uiso 1 1 calc R . . C30 C -0.1693(7) -0.1837(7) 0.4665(3) 0.0413(15) Uani 1 1 d . . . H30A H -0.1476 -0.1071 0.4465 0.050 Uiso 1 1 calc R . . C31 C -0.1303(11) -0.2961(10) 0.4258(4) 0.076(3) Uani 1 1 d . . . H31A H -0.0305 -0.3256 0.4159 0.114 Uiso 1 1 calc R . . H31B H -0.1841 -0.2629 0.3907 0.114 Uiso 1 1 calc R . . H31C H -0.1514 -0.3719 0.4446 0.114 Uiso 1 1 calc R . . C32 C -0.3237(8) -0.1329(9) 0.4828(4) 0.063(2) Uani 1 1 d . . . H32A H -0.3451 -0.0607 0.5088 0.095 Uiso 1 1 calc R . . H32B H -0.3474 -0.2069 0.5021 0.095 Uiso 1 1 calc R . . H32C H -0.3783 -0.0984 0.4480 0.095 Uiso 1 1 calc R . . C33 C 0.0952(9) -0.1784(9) 0.6383(3) 0.057(2) Uani 1 1 d . . . H33A H 0.1325 -0.1113 0.6188 0.069 Uiso 1 1 calc R . . C34 C -0.0126(11) -0.1075(11) 0.6855(4) 0.076(3) Uani 1 1 d . . . H34A H -0.0901 -0.0330 0.6674 0.115 Uiso 1 1 calc R . . H34B H 0.0324 -0.0725 0.7125 0.115 Uiso 1 1 calc R . . H34C H -0.0481 -0.1721 0.7062 0.115 Uiso 1 1 calc R . . C35 C 0.2167(10) -0.2945(10) 0.6647(4) 0.069(2) Uani 1 1 d . . . H35A H 0.2835 -0.3375 0.6342 0.104 Uiso 1 1 calc R . . H35B H 0.1824 -0.3602 0.6853 0.104 Uiso 1 1 calc R . . H35C H 0.2629 -0.2606 0.6917 0.104 Uiso 1 1 calc R . . C36 C 0.3110(7) -0.2704(7) 0.4644(3) 0.0416(15) Uani 1 1 d . . . C37 C 0.3713(8) -0.2524(10) 0.5215(4) 0.063(2) Uani 1 1 d . . . H37A H 0.4431 -0.3378 0.5349 0.095 Uiso 1 1 calc R . . H37B H 0.2962 -0.2246 0.5507 0.095 Uiso 1 1 calc R . . H37C H 0.4126 -0.1834 0.5146 0.095 Uiso 1 1 calc R . . C38 C 0.4257(8) -0.3005(9) 0.4164(4) 0.057(2) Uani 1 1 d . . . H38A H 0.5018 -0.3854 0.4270 0.086 Uiso 1 1 calc R . . H38B H 0.4616 -0.2275 0.4116 0.086 Uiso 1 1 calc R . . H38C H 0.3863 -0.3078 0.3802 0.086 Uiso 1 1 calc R . . C39 C 0.2582(8) -0.3871(7) 0.4729(4) 0.063(2) Uani 1 1 d . . . H39A H 0.3342 -0.4694 0.4864 0.095 Uiso 1 1 calc R . . H39B H 0.2253 -0.4006 0.4362 0.095 Uiso 1 1 calc R . . H39C H 0.1812 -0.3659 0.5015 0.095 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 0.0356(5) 0.0188(4) 0.0384(5) -0.0076(3) 0.0042(3) -0.0123(3) Ni2 0.0310(6) 0.0216(5) 0.0401(6) -0.0051(4) 0.0023(5) -0.0119(5) S1 0.0409(9) 0.0239(7) 0.0470(9) -0.0054(6) 0.0108(7) -0.0099(7) S2 0.0538(11) 0.0303(8) 0.0633(11) -0.0170(8) 0.0236(9) -0.0210(8) S3 0.0410(10) 0.0315(8) 0.0518(10) -0.0051(7) 0.0109(8) -0.0109(7) N1 0.039(3) 0.026(3) 0.061(4) -0.015(2) 0.008(3) -0.016(2) N2 0.054(4) 0.033(3) 0.048(3) -0.006(2) 0.012(3) -0.022(3) N3 0.037(3) 0.023(2) 0.047(3) -0.010(2) 0.007(2) -0.013(2) N4 0.043(3) 0.024(2) 0.037(3) -0.004(2) 0.005(2) -0.012(2) N5 0.046(3) 0.037(3) 0.043(3) 0.005(2) -0.002(3) -0.020(3) N6 0.036(3) 0.028(3) 0.044(3) -0.007(2) 0.004(2) -0.017(2) C1 0.038(4) 0.029(3) 0.038(3) -0.002(3) 0.008(3) -0.016(3) C2 0.066(5) 0.033(4) 0.083(6) -0.020(4) 0.025(4) -0.032(4) C3 0.075(6) 0.033(4) 0.064(5) -0.007(3) 0.024(4) -0.027(4) C4 0.058(5) 0.048(4) 0.052(4) 0.004(3) 0.007(4) -0.024(4) C5 0.070(6) 0.077(6) 0.077(6) 0.028(5) -0.006(5) -0.019(5) C6 0.092(7) 0.080(7) 0.064(6) -0.013(5) 0.017(5) -0.029(6) C7 0.044(4) 0.027(3) 0.069(5) -0.013(3) -0.006(3) -0.015(3) C8 0.102(8) 0.070(6) 0.079(6) -0.034(5) -0.005(6) -0.031(6) C9 0.042(5) 0.088(7) 0.111(8) -0.032(6) -0.010(5) -0.018(5) C10 0.030(3) 0.024(3) 0.039(3) -0.014(2) 0.008(3) -0.008(3) C11 0.051(4) 0.033(3) 0.056(4) -0.005(3) 0.011(3) -0.027(3) C12 0.059(5) 0.030(3) 0.039(4) -0.002(3) 0.004(3) -0.015(3) C13 0.041(4) 0.043(4) 0.055(4) -0.010(3) 0.000(3) -0.016(3) C14 0.053(5) 0.058(5) 0.108(8) -0.020(5) -0.021(5) -0.002(4) C15 0.065(5) 0.062(5) 0.052(5) -0.018(4) -0.001(4) -0.025(4) C16 0.050(4) 0.028(3) 0.057(4) -0.010(3) -0.006(3) -0.014(3) C17 0.041(4) 0.062(5) 0.081(6) -0.023(4) 0.002(4) -0.015(4) C18 0.072(6) 0.049(4) 0.069(5) -0.024(4) -0.006(4) -0.023(4) C19 0.037(4) 0.034(3) 0.049(4) -0.009(3) 0.009(3) -0.013(3) C20 0.052(5) 0.062(5) 0.063(5) -0.002(4) -0.009(4) -0.009(4) C21 0.045(4) 0.050(4) 0.071(5) -0.015(4) 0.013(4) -0.014(4) C22 0.054(5) 0.027(3) 0.091(6) -0.013(4) 0.025(4) -0.015(3) C23 0.049(4) 0.037(4) 0.053(4) -0.014(3) 0.015(3) -0.017(3) C24 0.077(6) 0.030(4) 0.077(6) -0.017(4) 0.034(5) -0.023(4) C25 0.068(6) 0.052(5) 0.116(8) -0.024(5) 0.045(6) -0.018(5) C26 0.152(12) 0.072(7) 0.084(7) -0.024(6) -0.022(7) -0.045(7) C27 0.029(3) 0.023(3) 0.043(3) -0.004(2) 0.003(3) -0.007(2) C28 0.067(5) 0.046(4) 0.066(5) 0.012(4) 0.002(4) -0.028(4) C29 0.053(5) 0.043(4) 0.064(5) 0.004(3) 0.000(4) -0.028(4) C30 0.039(4) 0.037(3) 0.052(4) -0.010(3) 0.002(3) -0.016(3) C31 0.081(7) 0.075(6) 0.066(6) -0.039(5) -0.003(5) -0.012(5) C32 0.040(4) 0.076(6) 0.071(5) -0.022(5) 0.001(4) -0.016(4) C33 0.056(5) 0.066(5) 0.051(4) -0.002(4) -0.005(4) -0.024(4) C34 0.086(7) 0.083(7) 0.053(5) -0.022(5) -0.009(5) -0.017(6) C35 0.064(6) 0.072(6) 0.066(6) 0.009(5) -0.017(4) -0.020(5) C36 0.037(4) 0.032(3) 0.055(4) -0.008(3) 0.006(3) -0.012(3) C37 0.043(4) 0.079(6) 0.061(5) -0.013(4) -0.001(4) -0.012(4) C38 0.040(4) 0.057(5) 0.073(5) -0.023(4) 0.013(4) -0.013(4) C39 0.044(4) 0.034(4) 0.107(7) -0.018(4) 0.019(4) -0.008(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 C10 1.896(6) . ? Ni1 C1 1.918(6) . ? Ni1 S2 2.236(2) . ? Ni1 S1 2.240(2) . ? Ni2 C27 1.919(6) . ? Ni2 C27 1.919(6) 2_556 ? Ni2 S3 2.2282(19) 2_556 ? Ni2 S3 2.2282(19) . ? S1 C19 1.852(7) . ? S2 C23 1.846(7) . ? S3 C36 1.849(7) . ? N1 C1 1.369(8) . ? N1 C2 1.386(9) . ? N1 C7 1.454(9) . ? N2 C1 1.342(8) . ? N2 C3 1.389(9) . ? N2 C4 1.456(10) . ? N3 C10 1.364(8) . ? N3 C11 1.390(8) . ? N3 C16 1.472(9) . ? N4 C10 1.359(8) . ? N4 C12 1.397(8) . ? N4 C13 1.471(9) . ? N5 C27 1.353(8) . ? N5 C28 1.398(9) . ? N5 C33 1.462(10) . ? N6 C27 1.351(8) . ? N6 C29 1.376(8) . ? N6 C30 1.483(9) . ? C2 C3 1.335(12) . ? C2 H2A 0.9400 . ? C3 H3A 0.9400 . ? C4 C6 1.522(12) . ? C4 C5 1.529(11) . ? C4 H4A 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.510(10) . ? C7 C9 1.516(11) . ? C7 H7A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C11 C12 1.336(10) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 C14 1.519(11) . ? C13 C15 1.522(10) . ? C13 H13A 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.527(9) . ? C16 C17 1.531(11) . ? C16 H16A 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.515(10) . ? C19 C21 1.524(10) . ? C19 C22 1.529(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C26 1.504(12) . ? C23 C24 1.509(10) . ? C23 C25 1.517(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C28 C29 1.326(11) . ? C28 H28A 0.9400 . ? C29 H29A 0.9400 . ? C30 C32 1.504(10) . ? C30 C31 1.509(10) . ? C30 H30A 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C35 1.502(11) . ? C33 C34 1.537(12) . ? C33 H33A 0.9900 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 C39 1.521(10) . ? C36 C38 1.530(10) . ? C36 C37 1.543(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? 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 C10 Ni1 C1 172.5(3) . . ? C10 Ni1 S2 96.41(18) . . ? C1 Ni1 S2 83.1(2) . . ? C10 Ni1 S1 83.52(18) . . ? C1 Ni1 S1 95.63(19) . . ? S2 Ni1 S1 169.79(8) . . ? C27 Ni2 C27 180.0(3) . 2_556 ? C27 Ni2 S3 82.75(19) . 2_556 ? C27 Ni2 S3 97.25(19) 2_556 2_556 ? C27 Ni2 S3 97.25(19) . . ? C27 Ni2 S3 82.75(19) 2_556 . ? S3 Ni2 S3 180.00(7) 2_556 . ? C19 S1 Ni1 119.5(2) . . ? C23 S2 Ni1 123.8(2) . . ? C36 S3 Ni2 119.1(2) . . ? C1 N1 C2 109.3(6) . . ? C1 N1 C7 124.6(5) . . ? C2 N1 C7 125.9(6) . . ? C1 N2 C3 111.3(6) . . ? C1 N2 C4 124.3(6) . . ? C3 N2 C4 124.4(6) . . ? C10 N3 C11 111.2(5) . . ? C10 N3 C16 124.8(5) . . ? C11 N3 C16 123.9(5) . . ? C10 N4 C12 111.1(5) . . ? C10 N4 C13 123.8(5) . . ? C12 N4 C13 125.1(6) . . ? C27 N5 C28 109.6(6) . . ? C27 N5 C33 127.2(6) . . ? C28 N5 C33 122.9(6) . . ? C27 N6 C29 111.3(6) . . ? C27 N6 C30 123.6(5) . . ? C29 N6 C30 124.4(5) . . ? N2 C1 N1 105.1(5) . . ? N2 C1 Ni1 132.5(5) . . ? N1 C1 Ni1 122.0(5) . . ? C3 C2 N1 108.2(6) . . ? C3 C2 H2A 125.9 . . ? N1 C2 H2A 125.9 . . ? C2 C3 N2 106.1(6) . . ? C2 C3 H3A 127.0 . . ? N2 C3 H3A 127.0 . . ? N2 C4 C6 109.8(7) . . ? N2 C4 C5 111.4(7) . . ? C6 C4 C5 111.6(7) . . ? N2 C4 H4A 108.0 . . ? C6 C4 H4A 108.0 . . ? C5 C4 H4A 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 111.7(6) . . ? N1 C7 C9 110.1(7) . . ? C8 C7 C9 113.5(7) . . ? N1 C7 H7A 107.1 . . ? C8 C7 H7A 107.1 . . ? C9 C7 H7A 107.1 . . ? 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 . . ? N4 C10 N3 104.0(5) . . ? N4 C10 Ni1 125.1(4) . . ? N3 C10 Ni1 130.8(5) . . ? C12 C11 N3 107.0(6) . . ? C12 C11 H11A 126.5 . . ? N3 C11 H11A 126.5 . . ? C11 C12 N4 106.8(6) . . ? C11 C12 H12A 126.6 . . ? N4 C12 H12A 126.6 . . ? N4 C13 C14 111.8(6) . . ? N4 C13 C15 110.4(6) . . ? C14 C13 C15 111.7(7) . . ? N4 C13 H13A 107.5 . . ? C14 C13 H13A 107.5 . . ? C15 C13 H13A 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C18 111.7(6) . . ? N3 C16 C17 110.3(6) . . ? C18 C16 C17 111.8(6) . . ? N3 C16 H16A 107.6 . . ? C18 C16 H16A 107.6 . . ? C17 C16 H16A 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 109.2(6) . . ? C20 C19 C22 110.9(7) . . ? C21 C19 C22 108.5(6) . . ? C20 C19 S1 110.2(5) . . ? C21 C19 S1 104.5(5) . . ? C22 C19 S1 113.3(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C26 C23 C24 109.3(7) . . ? C26 C23 C25 108.6(8) . . ? C24 C23 C25 108.1(7) . . ? C26 C23 S2 108.4(6) . . ? C24 C23 S2 116.5(5) . . ? C25 C23 S2 105.8(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 N5 104.8(5) . . ? N6 C27 Ni2 122.0(4) . . ? N5 C27 Ni2 133.1(5) . . ? C29 C28 N5 107.5(7) . . ? C29 C28 H28A 126.3 . . ? N5 C28 H28A 126.3 . . ? C28 C29 N6 106.7(6) . . ? C28 C29 H29A 126.6 . . ? N6 C29 H29A 126.6 . . ? N6 C30 C32 108.8(6) . . ? N6 C30 C31 111.7(6) . . ? C32 C30 C31 111.7(7) . . ? N6 C30 H30A 108.2 . . ? C32 C30 H30A 108.2 . . ? C31 C30 H30A 108.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C35 112.4(7) . . ? N5 C33 C34 109.7(7) . . ? C35 C33 C34 110.9(7) . . ? N5 C33 H33A 107.9 . . ? C35 C33 H33A 107.9 . . ? C34 C33 H33A 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C38 109.2(6) . . ? C39 C36 C37 110.2(7) . . ? C38 C36 C37 109.7(6) . . ? C39 C36 S3 113.2(5) . . ? C38 C36 S3 104.9(5) . . ? C37 C36 S3 109.5(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.210 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.148 _chemical_name_common '(iPr2Im)2(StBu)2Ni(ii) 9' data_compound11 _database_code_depnum_ccdc_archive 'CCDC 726139' _chemical_name_systematic ; (iPr2Im)2(Ph)2Ni(II) ; _chemical_formula_sum 'C30 H42 N4 Ni S2' _chemical_formula_weight 581.51 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' 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 P2(1)/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 10.418(2) _cell_length_b 9.6227(19) _cell_length_c 16.036(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.33(3) _cell_angle_gamma 90.00 _cell_volume 1534.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 203(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 STADI 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 8471 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 31.77 _reflns_number_total 3588 _reflns_number_gt 2827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1589P)^2^+3.6494P] 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 3588 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2745 _refine_ls_wR_factor_gt 0.2459 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.0000 0.5000 0.0000 0.0237(3) Uani 1 2 d S . . S1 S 0.1310(2) 0.3410(2) 0.07328(13) 0.0698(6) Uani 1 1 d . . . N1 N 0.1149(4) 0.6542(5) 0.1613(3) 0.0381(10) Uani 1 1 d . . . N2 N -0.0700(4) 0.5564(4) 0.1612(2) 0.0245(7) Uani 1 1 d . . . C1 C 0.0134(4) 0.5740(5) 0.1112(3) 0.0266(9) Uani 1 1 d . . . C2 C 0.0945(5) 0.6854(6) 0.2410(3) 0.0403(12) Uani 1 1 d . . . H2A H 0.1503 0.7400 0.2859 0.048 Uiso 1 1 calc R . . C3 C -0.0202(5) 0.6227(6) 0.2413(3) 0.0344(11) Uani 1 1 d . . . H3A H -0.0595 0.6234 0.2871 0.041 Uiso 1 1 calc R . . C4 C -0.1924(5) 0.4724(5) 0.1338(3) 0.0292(10) Uani 1 1 d . . . H4A H -0.2229 0.4696 0.0691 0.035 Uiso 1 1 calc R . . C5 C -0.1625(6) 0.3250(6) 0.1670(5) 0.0527(15) Uani 1 1 d . . . H5A H -0.0901 0.2874 0.1473 0.079 Uiso 1 1 calc R . . H5B H -0.2423 0.2683 0.1446 0.079 Uiso 1 1 calc R . . H5C H -0.1359 0.3249 0.2303 0.079 Uiso 1 1 calc R . . C6 C -0.3036(5) 0.5361(6) 0.1641(4) 0.0413(12) Uani 1 1 d . . . H6A H -0.3202 0.6304 0.1422 0.062 Uiso 1 1 calc R . . H6B H -0.2770 0.5373 0.2274 0.062 Uiso 1 1 calc R . . H6C H -0.3850 0.4815 0.1421 0.062 Uiso 1 1 calc R . . C7 C 0.2335(6) 0.6981(8) 0.1356(4) 0.060(2) Uani 1 1 d . . . H7A H 0.2233 0.6670 0.0752 0.072 Uiso 1 1 calc R . . C8 C 0.2481(10) 0.8559(12) 0.1406(7) 0.103(4) Uani 1 1 d . . . H8A H 0.1681 0.8984 0.1017 0.154 Uiso 1 1 calc R . . H8B H 0.3261 0.8832 0.1232 0.154 Uiso 1 1 calc R . . H8C H 0.2595 0.8864 0.2000 0.154 Uiso 1 1 calc R . . C9 C 0.3596(6) 0.6382(11) 0.1956(6) 0.086(3) Uani 1 1 d . . . H9A H 0.3531 0.5377 0.1951 0.129 Uiso 1 1 calc R . . H9B H 0.3721 0.6722 0.2545 0.129 Uiso 1 1 calc R . . H9C H 0.4357 0.6659 0.1763 0.129 Uiso 1 1 calc R . . C10 C 0.2134(6) 0.2524(6) 0.0168(3) 0.0435(13) Uani 1 1 d . . . C11 C 0.3500(7) 0.2805(11) 0.0366(4) 0.071(2) Uani 1 1 d . . . H11A H 0.3902 0.3493 0.0776 0.085 Uiso 1 1 calc R . . C12 C 0.4295(11) 0.2016(18) -0.0073(7) 0.139(7) Uani 1 1 d . . . H12A H 0.5222 0.2196 0.0069 0.167 Uiso 1 1 calc R . . C13 C 0.3781(15) 0.1079(14) -0.0650(6) 0.125(6) Uani 1 1 d . . . H13A H 0.4319 0.0608 -0.0936 0.150 Uiso 1 1 calc R . . C14 C 0.2433(15) 0.0777(9) -0.0840(5) 0.100(4) Uani 1 1 d . . . H14A H 0.2070 0.0070 -0.1246 0.120 Uiso 1 1 calc R . . C15 C 0.1565(9) 0.1494(7) -0.0445(4) 0.0602(18) Uani 1 1 d . . . H15A H 0.0644 0.1281 -0.0591 0.072 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 0.0230(5) 0.0333(5) 0.0142(4) -0.0026(3) 0.0044(3) -0.0037(3) S1 0.0798(13) 0.0767(13) 0.0567(11) 0.0092(9) 0.0262(10) 0.0279(10) N1 0.028(2) 0.062(3) 0.0236(19) -0.0122(19) 0.0065(16) -0.0137(19) N2 0.0246(18) 0.0307(19) 0.0182(17) -0.0012(14) 0.0064(14) 0.0020(14) C1 0.024(2) 0.035(2) 0.0194(19) 0.0015(17) 0.0048(16) -0.0019(16) C2 0.035(3) 0.062(3) 0.021(2) -0.015(2) 0.0041(19) -0.010(2) C3 0.038(3) 0.049(3) 0.017(2) -0.0094(19) 0.0098(19) -0.001(2) C4 0.029(2) 0.029(2) 0.033(2) 0.0004(17) 0.012(2) -0.0017(16) C5 0.053(3) 0.036(3) 0.077(4) 0.008(3) 0.031(3) 0.000(2) C6 0.031(3) 0.050(3) 0.047(3) -0.002(2) 0.018(2) 0.002(2) C7 0.043(3) 0.100(5) 0.044(3) -0.030(3) 0.022(3) -0.034(3) C8 0.075(6) 0.131(9) 0.104(7) 0.006(7) 0.032(5) -0.054(6) C9 0.031(3) 0.141(8) 0.091(6) -0.048(6) 0.027(4) -0.019(4) C10 0.059(3) 0.047(3) 0.025(2) 0.009(2) 0.011(2) 0.020(3) C11 0.051(4) 0.122(7) 0.037(3) 0.025(4) 0.011(3) 0.012(4) C12 0.081(7) 0.263(18) 0.086(7) 0.109(10) 0.045(6) 0.096(10) C13 0.165(12) 0.162(12) 0.050(5) 0.035(6) 0.034(7) 0.125(11) C14 0.198(13) 0.060(5) 0.048(4) 0.006(4) 0.045(6) 0.056(7) C15 0.098(5) 0.040(3) 0.036(3) -0.003(2) 0.010(3) 0.015(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 C1 1.887(4) . ? Ni1 C1 1.887(4) 3_565 ? Ni1 S1 2.152(2) 3_565 ? Ni1 S1 2.152(2) . ? S1 C10 1.657(6) . ? N1 C1 1.360(6) . ? N1 C2 1.390(6) . ? N1 C7 1.476(7) . ? N2 C1 1.357(5) . ? N2 C3 1.389(6) . ? N2 C4 1.462(6) . ? C2 C3 1.340(7) . ? C2 H2A 0.9400 . ? C3 H3A 0.9400 . ? C4 C6 1.514(7) . ? C4 C5 1.514(7) . ? C4 H4A 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C9 1.493(11) . ? C7 C8 1.526(13) . ? C7 H7A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.389(10) . ? C10 C15 1.397(9) . ? C11 C12 1.450(14) . ? C11 H11A 0.9400 . ? C12 C13 1.29(2) . ? C12 H12A 0.9400 . ? C13 C14 1.376(18) . ? C13 H13A 0.9400 . ? C14 C15 1.427(12) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? 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 C1 Ni1 C1 180.0 . 3_565 ? C1 Ni1 S1 95.97(15) . 3_565 ? C1 Ni1 S1 84.03(15) 3_565 3_565 ? C1 Ni1 S1 84.03(15) . . ? C1 Ni1 S1 95.97(15) 3_565 . ? S1 Ni1 S1 180.00(10) 3_565 . ? C10 S1 Ni1 114.5(2) . . ? C1 N1 C2 111.1(4) . . ? C1 N1 C7 124.5(4) . . ? C2 N1 C7 124.4(4) . . ? C1 N2 C3 111.2(4) . . ? C1 N2 C4 123.1(4) . . ? C3 N2 C4 125.7(4) . . ? N2 C1 N1 104.1(4) . . ? N2 C1 Ni1 129.1(3) . . ? N1 C1 Ni1 126.7(3) . . ? C3 C2 N1 106.7(4) . . ? C3 C2 H2A 126.7 . . ? N1 C2 H2A 126.7 . . ? C2 C3 N2 106.9(4) . . ? C2 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? N2 C4 C6 111.2(4) . . ? N2 C4 C5 110.0(4) . . ? C6 C4 C5 111.3(4) . . ? N2 C4 H4A 108.1 . . ? C6 C4 H4A 108.1 . . ? C5 C4 H4A 108.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C9 111.0(6) . . ? N1 C7 C8 110.4(6) . . ? C9 C7 C8 107.2(7) . . ? N1 C7 H7A 109.4 . . ? C9 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? 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 C15 119.3(7) . . ? C11 C10 S1 115.9(6) . . ? C15 C10 S1 124.7(6) . . ? C10 C11 C12 118.8(10) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 122.6(11) . . ? C13 C12 H12A 118.7 . . ? C11 C12 H12A 118.7 . . ? C12 C13 C14 119.0(9) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C13 C14 C15 122.6(10) . . ? C13 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C10 C15 C14 117.6(9) . . ? C10 C15 H15A 121.2 . . ? C14 C15 H15A 121.2 . . ? _diffrn_measured_fraction_theta_max 0.688 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.697 _refine_diff_density_min -1.316 _refine_diff_density_rms 0.174 #===END _chemical_name_common (iPr2Im)2(Ph)2Ni(ii)