# Copyright The Royal Society of Chemistry, 1998 data_l4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(cdsalpd)]' _chemical_formula_moiety ' ' _chemical_formula_structural 'C17 H20 N2 Ni S2' _chemical_formula_analytical 'C17 H20 N2 Ni S2' _chemical_formula_sum 'C17 H20 N2 Ni O S2' _chemical_formula_weight 391.16 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.2850 1.1130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting '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 8.924(5) _cell_length_b 16.889(8) _cell_length_c 12.051(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.94(2) _cell_angle_gamma 90.00 _cell_volume 1798.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 3707 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 26.99 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method none _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min **** _exptl_absorpt_correction_T_max **** _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe stadi IV 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted 2\q/\w scans (Clegg, 1981)' _diffrn_standards_number 15 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4091 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3713 _reflns_number_observed 3289 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3707 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_obs 0.0271 _refine_ls_wR_factor_all 0.0749 _refine_ls_wR_factor_obs 0.0687 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.03130(2) 0.532642(14) 0.20029(2) 0.03296(9) Uani 1 d . . S2 S -0.16471(5) 0.60074(3) 0.23654(4) 0.04040(12) Uani 1 d . . S1 S -0.45897(7) 0.56839(5) 0.32051(6) 0.0650(2) Uani 1 d . . N1 N 0.0327(2) 0.45796(9) 0.31876(12) 0.0359(3) Uani 1 d . . N2 N 0.1611(2) 0.46368(9) 0.12850(13) 0.0363(3) Uani 1 d . . C1 C -0.0784(2) 0.43250(12) 0.37034(14) 0.0374(4) Uani 1 d . . C2 C -0.0668(3) 0.3632(2) 0.4550(2) 0.0500(5) Uani 1 d . . H2A H -0.0089(29) 0.3189(16) 0.4346(21) 0.063(7) Uiso 1 d . . H2B H -0.0148(30) 0.3827(16) 0.5235(23) 0.068(8) Uiso 1 d . . C3A C -0.2321(4) 0.3346(2) 0.4498(3) 0.0565(8) Uiso 0.74 d P 1 H3A1 H -0.2505(4) 0.3125(2) 0.5219(3) 0.068 Uiso 0.74 calc PR 1 H3A2 H -0.2563(4) 0.2945(2) 0.3914(3) 0.068 Uiso 0.74 calc PR 1 C3B C -0.2226(11) 0.3589(6) 0.4967(9) 0.058(2) Uiso 0.26 d P 2 H3B1 H -0.2605(11) 0.3044(6) 0.4927(9) 0.070 Uiso 0.26 calc PR 2 H3B2 H -0.2148(11) 0.3770(6) 0.5745(9) 0.070 Uiso 0.26 calc PR 2 C4 C -0.3270(3) 0.4119(2) 0.4213(2) 0.0555(6) Uani 1 d . . H4A H -0.4096(31) 0.3952(16) 0.3750(23) 0.069(8) Uiso 1 d . . H4B H -0.3636(34) 0.4426(18) 0.4821(27) 0.084(9) Uiso 1 d . . C5 C -0.2289(2) 0.46500(12) 0.3574(2) 0.0402(4) Uani 1 d . . C6 C 0.1867(2) 0.42551(13) 0.3548(2) 0.0414(4) Uani 1 d . . H6A H 0.1953(24) 0.4058(13) 0.4313(18) 0.044(6) Uiso 1 d . . H6B H 0.2538(24) 0.4708(12) 0.3552(18) 0.040(5) Uiso 1 d . . C7 C 0.2291(2) 0.35957(13) 0.2755(2) 0.0451(5) Uani 1 d . . H7A H 0.3393(28) 0.3577(14) 0.2804(19) 0.053(6) Uiso 1 d . . H7B H 0.1948(29) 0.3083(16) 0.2977(21) 0.066(8) Uiso 1 d . . C8 C 0.1582(2) 0.37570(12) 0.1550(2) 0.0428(4) Uani 1 d . . H8A H 0.2082(25) 0.3445(13) 0.1020(19) 0.048(6) Uiso 1 d . . H8B H 0.0487(25) 0.3578(13) 0.1425(17) 0.044(6) Uiso 1 d . . C9 C 0.2353(2) 0.48568(13) 0.0489(2) 0.0405(4) Uani 1 d . . H9 H 0.2927(25) 0.4420(13) 0.0125(19) 0.047(6) Uiso 1 d . . C10 C 0.2469(2) 0.56790(13) 0.00901(15) 0.0418(4) Uani 1 d . . C11 C 0.3496(3) 0.5839(2) -0.0683(2) 0.0549(6) Uani 1 d . . H11 H 0.4045(29) 0.5382(14) -0.0890(21) 0.056(7) Uiso 1 d . . C12 C 0.3669(3) 0.6610(2) -0.1079(2) 0.0647(7) Uani 1 d . . H12 H 0.4384(35) 0.6744(18) -0.1576(26) 0.089(9) Uiso 1 d . . C13 C 0.2792(3) 0.7243(2) -0.0745(2) 0.0592(7) Uani 1 d . . H13 H 0.2886(27) 0.7774(16) -0.1033(21) 0.062(7) Uiso 1 d . . C14 C 0.1760(3) 0.71049(14) -0.0016(2) 0.0485(5) Uani 1 d . . H14 H 0.1199(28) 0.7522(16) 0.0181(20) 0.059(7) Uiso 1 d . . C15 C 0.1576(2) 0.63177(12) 0.04294(15) 0.0408(4) Uani 1 d . . C16 C -0.2725(2) 0.53745(12) 0.3070(2) 0.0408(4) Uani 1 d . . C17 C -0.4975(3) 0.6562(2) 0.2330(3) 0.0646(7) Uani 1 d . . H17A H -0.5984(41) 0.6690(20) 0.2328(28) 0.102(11) Uiso 1 d . . H17B H -0.4831(33) 0.6445(18) 0.1590(26) 0.081(9) Uiso 1 d . . H17C H -0.4367(34) 0.7051(18) 0.2640(26) 0.088(9) Uiso 1 d . . O1 O 0.0564(2) 0.62218(8) 0.11101(12) 0.0476(3) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03374(14) 0.03332(14) 0.03161(13) 0.00084(9) 0.00381(9) -0.00081(9) S2 0.0429(3) 0.0403(3) 0.0382(2) -0.0016(2) 0.0062(2) 0.0060(2) S1 0.0401(3) 0.0808(5) 0.0768(4) 0.0021(3) 0.0175(3) 0.0120(3) N1 0.0334(8) 0.0411(9) 0.0319(7) 0.0024(6) 0.0003(6) -0.0011(6) N2 0.0366(8) 0.0372(8) 0.0342(8) -0.0032(6) 0.0014(6) -0.0020(6) C1 0.0411(10) 0.0411(10) 0.0288(8) -0.0006(7) 0.0004(7) -0.0042(8) C2 0.0543(13) 0.0546(13) 0.0408(11) 0.0122(10) 0.0052(9) -0.0032(11) C4 0.0462(12) 0.072(2) 0.0503(12) -0.0012(11) 0.0125(10) -0.0146(11) C5 0.0361(9) 0.0523(12) 0.0327(9) -0.0038(8) 0.0061(7) -0.0053(8) C6 0.0340(9) 0.0482(12) 0.0391(10) 0.0039(9) -0.0051(7) -0.0025(8) C7 0.0384(11) 0.0433(11) 0.0508(11) 0.0045(9) -0.0034(8) 0.0021(9) C8 0.0455(11) 0.0346(10) 0.0468(11) -0.0032(8) 0.0007(8) -0.0005(8) C9 0.0399(10) 0.0487(11) 0.0323(9) -0.0071(8) 0.0030(7) -0.0011(8) C10 0.0411(10) 0.0545(12) 0.0286(8) -0.0025(8) 0.0007(7) -0.0119(9) C11 0.0527(13) 0.077(2) 0.0351(10) -0.0030(11) 0.0085(9) -0.0139(12) C12 0.0616(15) 0.094(2) 0.0385(11) 0.0070(12) 0.0084(10) -0.0294(14) C13 0.0624(14) 0.069(2) 0.0407(11) 0.0174(11) -0.0116(10) -0.0322(13) C14 0.0517(12) 0.0479(12) 0.0416(11) 0.0070(9) -0.0088(9) -0.0152(10) C15 0.0407(10) 0.0471(11) 0.0321(9) 0.0025(8) -0.0037(7) -0.0110(8) C16 0.0336(9) 0.0543(12) 0.0339(9) -0.0100(8) 0.0030(7) 0.0006(8) C17 0.0458(13) 0.071(2) 0.072(2) -0.0151(14) -0.0125(12) 0.0164(12) O1 0.0548(8) 0.0405(8) 0.0501(8) 0.0087(6) 0.0167(7) 0.0018(6) _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 O1 1.887(2) . ? Ni1 N1 1.904(2) . ? Ni1 N2 1.930(2) . ? Ni1 S2 2.1873(10) . ? S2 C16 1.736(2) . ? S1 C16 1.773(2) . ? S1 C17 1.824(3) . ? N1 C1 1.313(2) . ? N1 C6 1.487(3) . ? N2 C9 1.293(2) . ? N2 C8 1.521(3) . ? C1 C5 1.439(3) . ? C1 C2 1.546(3) . ? C2 C3B 1.544(10) . ? C2 C3A 1.546(4) . ? C3A C4 1.567(4) . ? C3B C4 1.503(10) . ? C4 C5 1.533(3) . ? C5 C16 1.398(3) . ? C6 C7 1.548(3) . ? C7 C8 1.526(3) . ? C9 C10 1.478(3) . ? C10 C11 1.420(3) . ? C10 C15 1.434(3) . ? C11 C12 1.404(4) . ? C12 C13 1.416(4) . ? C13 C14 1.377(3) . ? C14 C15 1.451(3) . ? C15 O1 1.312(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 165.81(7) . . ? O1 Ni1 N2 95.87(7) . . ? N1 Ni1 N2 89.66(7) . . ? O1 Ni1 S2 81.58(5) . . ? N1 Ni1 S2 96.97(6) . . ? N2 Ni1 S2 162.38(5) . . ? C16 S2 Ni1 106.64(8) . . ? C16 S1 C17 106.90(12) . . ? C1 N1 C6 117.9(2) . . ? C1 N1 Ni1 130.14(13) . . ? C6 N1 Ni1 111.92(12) . . ? C9 N2 C8 117.5(2) . . ? C9 N2 Ni1 124.05(14) . . ? C8 N2 Ni1 117.81(13) . . ? N1 C1 C5 125.3(2) . . ? N1 C1 C2 125.0(2) . . ? C5 C1 C2 109.7(2) . . ? C3B C2 C1 105.6(4) . . ? C3A C2 C1 103.5(2) . . ? C2 C3A C4 103.4(2) . . ? C4 C3B C2 106.6(6) . . ? C3B C4 C5 107.6(4) . . ? C5 C4 C3A 105.6(2) . . ? C16 C5 C1 125.5(2) . . ? C16 C5 C4 125.9(2) . . ? C1 C5 C4 108.1(2) . . ? N1 C6 C7 112.3(2) . . ? C8 C7 C6 110.8(2) . . ? N2 C8 C7 110.9(2) . . ? N2 C9 C10 125.3(2) . . ? C11 C10 C15 118.6(2) . . ? C11 C10 C9 118.2(2) . . ? C15 C10 C9 123.2(2) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 120.9(2) . . ? C14 C13 C12 119.8(2) . . ? C13 C14 C15 120.7(2) . . ? O1 C15 C10 122.9(2) . . ? O1 C15 C14 117.8(2) . . ? C10 C15 C14 119.2(2) . . ? C5 C16 S2 127.7(2) . . ? C5 C16 S1 115.26(15) . . ? S2 C16 S1 117.00(12) . . ? C15 O1 Ni1 126.99(13) . . ? _refine_diff_density_max 0.374 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.046