# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email rpnchemist@gmail.com _publ_contact_author_name 'R. Prabhakaran' loop_ _publ_author_name 'R. Prabhakaran' K.Palaniappan K.Natarajan data_in062507 _database_code_depnum_ccdc_archive 'CCDC 678414' #TrackingRef 'NiSaltsc CCDC 678414.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 N3 Ni O P S' _chemical_formula_weight 514.21 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.5914(15) _cell_length_b 10.200(2) _cell_length_c 16.693(3) _cell_angle_alpha 76.83(3) _cell_angle_beta 81.44(3) _cell_angle_gamma 71.30(3) _cell_volume 1188.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14155 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.24 _exptl_crystal_description chunk _exptl_crystal_colour red _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w,and/f 0.5 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14155 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.24 _reflns_number_total 5511 _reflns_number_gt 4687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COSMO (BRUKER, V1.58, 2006)' _computing_cell_refinement 'APEX2 (BRUKER, V2008.5-0, 2006)' _computing_data_reduction 'SAINT (BRUKER, V7.34A, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 5511 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.705 _refine_ls_restrained_S_all 0.705 _refine_ls_shift/su_max 0.003 _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 S S -0.22218(5) -0.04923(4) -0.18181(2) 0.02246(10) Uani 1 1 d . . . Ni Ni -0.09373(3) -0.273272(18) -0.169780(11) 0.01847(8) Uani 1 1 d . . . P P -0.23698(5) -0.27127(4) -0.27677(2) 0.01837(9) Uani 1 1 d . . . O1 O 0.01172(17) -0.46654(12) -0.16270(7) 0.0285(2) Uani 1 1 d . . . C2 C 0.1380(2) -0.55348(16) -0.11305(9) 0.0240(3) Uani 1 1 d . . . C3 C 0.2013(2) -0.69857(17) -0.11826(11) 0.0304(4) Uani 1 1 d . . . H3A H 0.1526 -0.7293 -0.1560 0.037 Uiso 1 1 calc R . . C4 C 0.3340(3) -0.79530(18) -0.06840(11) 0.0329(4) Uani 1 1 d . . . H4A H 0.3740 -0.8894 -0.0737 0.040 Uiso 1 1 calc R . . C5 C 0.4087(2) -0.75334(18) -0.01015(11) 0.0304(4) Uani 1 1 d . . . H5A H 0.4975 -0.8188 0.0233 0.036 Uiso 1 1 calc R . . C6 C 0.3486(2) -0.61360(17) -0.00316(10) 0.0273(3) Uani 1 1 d . . . H6A H 0.3964 -0.5855 0.0360 0.033 Uiso 1 1 calc R . . C7 C 0.2151(2) -0.51110(16) -0.05443(10) 0.0231(3) Uani 1 1 d . . . C8 C 0.1627(2) -0.36761(16) -0.04475(9) 0.0227(3) Uani 1 1 d . . . H8A H 0.2175 -0.3484 -0.0043 0.027 Uiso 1 1 calc R . . N9 N 0.04452(17) -0.26071(13) -0.08763(8) 0.0195(2) Uani 1 1 d . . . N10 N 0.02217(19) -0.13146(13) -0.06516(8) 0.0226(3) Uani 1 1 d . . . C11 C -0.1021(2) -0.02766(16) -0.10643(9) 0.0208(3) Uani 1 1 d . . . N12 N -0.1368(2) 0.10558(15) -0.09307(9) 0.0271(3) Uani 1 1 d . . . H12A H -0.095(3) 0.112(2) -0.0508(14) 0.041(6) Uiso 1 1 d . . . H12B H -0.231(3) 0.162(2) -0.1093(13) 0.039(6) Uiso 1 1 d . . . C13 C -0.0699(2) -0.26359(16) -0.36818(9) 0.0212(3) Uani 1 1 d . . . C14 C -0.0611(2) -0.33308(18) -0.43243(10) 0.0301(3) Uani 1 1 d . . . H14A H -0.1409 -0.3870 -0.4296 0.036 Uiso 1 1 calc R . . C15 C 0.0672(3) -0.3219(2) -0.50094(11) 0.0377(4) Uani 1 1 d . . . H15A H 0.0730 -0.3693 -0.5432 0.045 Uiso 1 1 calc R . . C16 C 0.1865(3) -0.2403(2) -0.50668(11) 0.0407(4) Uani 1 1 d . . . H16A H 0.2721 -0.2336 -0.5523 0.049 Uiso 1 1 calc R . . C17 C 0.1767(3) -0.1698(2) -0.44414(12) 0.0399(4) Uani 1 1 d . . . H17A H 0.2546 -0.1140 -0.4480 0.048 Uiso 1 1 calc R . . C18 C 0.0501(2) -0.18151(19) -0.37481(10) 0.0295(3) Uani 1 1 d . . . H18A H 0.0456 -0.1343 -0.3327 0.035 Uiso 1 1 calc R . . C19 C -0.3203(2) -0.42098(16) -0.27764(9) 0.0217(3) Uani 1 1 d . . . C20 C -0.1924(2) -0.55585(17) -0.27236(10) 0.0264(3) Uani 1 1 d . . . H20A H -0.0675 -0.5692 -0.2667 0.032 Uiso 1 1 calc R . . C21 C -0.2520(2) -0.67055(17) -0.27558(10) 0.0281(3) Uani 1 1 d . . . H21A H -0.1663 -0.7599 -0.2727 0.034 Uiso 1 1 calc R . . C22 C -0.4397(3) -0.65155(19) -0.28314(11) 0.0334(4) Uani 1 1 d . . . H22A H -0.4791 -0.7281 -0.2851 0.040 Uiso 1 1 calc R . . C23 C -0.5668(3) -0.5187(2) -0.28771(14) 0.0411(5) Uani 1 1 d . . . H23A H -0.6920 -0.5061 -0.2925 0.049 Uiso 1 1 calc R . . C24 C -0.5079(2) -0.40367(18) -0.28515(12) 0.0325(4) Uani 1 1 d . . . H24A H -0.5942 -0.3145 -0.2885 0.039 Uiso 1 1 calc R . . C25 C -0.4384(2) -0.11594(15) -0.30364(9) 0.0202(3) Uiso 1 1 d . . . C26 C -0.4442(2) -0.02526(17) -0.38050(10) 0.0260(3) Uani 1 1 d . . . H26A H -0.3460 -0.0452 -0.4208 0.031 Uiso 1 1 calc R . . C27 C -0.5964(2) 0.09509(19) -0.39712(11) 0.0337(4) Uani 1 1 d . . . H27A H -0.5997 0.1547 -0.4485 0.040 Uiso 1 1 calc R . . C28 C -0.7434(2) 0.12590(19) -0.33672(12) 0.0344(4) Uani 1 1 d . . . H28A H -0.8441 0.2066 -0.3477 0.041 Uiso 1 1 calc R . . C29 C -0.7396(2) 0.03566(19) -0.25976(11) 0.0312(4) Uani 1 1 d . . . H29A H -0.8383 0.0559 -0.2198 0.037 Uiso 1 1 calc R . . C30 C -0.5881(2) -0.08439(17) -0.24299(10) 0.0263(3) Uani 1 1 d . . . H30A H -0.5856 -0.1440 -0.1916 0.032 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 S 0.0289(2) 0.01752(18) 0.02201(19) -0.00456(14) -0.00842(14) -0.00493(15) Ni 0.02226(12) 0.01618(11) 0.01785(11) -0.00433(7) -0.00369(7) -0.00531(8) P 0.02007(18) 0.01783(18) 0.01814(18) -0.00434(14) -0.00217(14) -0.00606(14) O1 0.0362(6) 0.0190(5) 0.0310(6) -0.0081(4) -0.0123(5) -0.0026(5) C2 0.0268(8) 0.0200(7) 0.0241(7) -0.0046(6) -0.0006(6) -0.0057(6) C3 0.0379(9) 0.0211(8) 0.0320(9) -0.0083(6) -0.0034(7) -0.0061(7) C4 0.0381(9) 0.0187(8) 0.0358(9) -0.0043(7) 0.0029(7) -0.0032(7) C5 0.0263(8) 0.0233(8) 0.0327(9) 0.0019(6) -0.0015(7) -0.0008(6) C6 0.0253(8) 0.0272(8) 0.0273(8) -0.0005(6) -0.0037(6) -0.0073(6) C7 0.0214(7) 0.0212(7) 0.0241(7) -0.0023(6) 0.0000(6) -0.0052(6) C8 0.0237(7) 0.0243(8) 0.0218(7) -0.0047(6) -0.0042(6) -0.0081(6) N9 0.0212(6) 0.0182(6) 0.0204(6) -0.0053(5) -0.0018(5) -0.0065(5) N10 0.0279(7) 0.0195(6) 0.0221(6) -0.0061(5) -0.0051(5) -0.0066(5) C11 0.0257(7) 0.0210(7) 0.0176(7) -0.0050(5) -0.0003(5) -0.0094(6) N12 0.0370(8) 0.0188(7) 0.0268(7) -0.0068(5) -0.0120(6) -0.0045(6) C13 0.0205(7) 0.0210(7) 0.0201(7) -0.0041(5) -0.0017(5) -0.0036(6) C14 0.0380(9) 0.0282(8) 0.0268(8) -0.0087(6) 0.0005(7) -0.0124(7) C15 0.0508(11) 0.0367(10) 0.0255(8) -0.0119(7) 0.0033(8) -0.0116(8) C16 0.0385(10) 0.0527(12) 0.0284(9) -0.0085(8) 0.0109(8) -0.0157(9) C17 0.0372(10) 0.0565(12) 0.0338(9) -0.0091(9) 0.0043(8) -0.0275(9) C18 0.0308(8) 0.0381(9) 0.0255(8) -0.0097(7) -0.0008(6) -0.0163(7) C19 0.0262(7) 0.0210(7) 0.0197(7) -0.0040(5) -0.0019(6) -0.0095(6) C20 0.0273(8) 0.0246(8) 0.0290(8) -0.0057(6) -0.0069(6) -0.0077(6) C21 0.0370(9) 0.0213(8) 0.0264(8) -0.0041(6) -0.0045(7) -0.0087(7) C22 0.0410(10) 0.0299(9) 0.0367(9) -0.0100(7) 0.0037(8) -0.0210(8) C23 0.0281(9) 0.0379(10) 0.0644(13) -0.0139(9) -0.0054(8) -0.0159(8) C24 0.0252(8) 0.0263(8) 0.0474(10) -0.0100(7) -0.0048(7) -0.0068(7) C26 0.0247(8) 0.0276(8) 0.0237(7) -0.0032(6) -0.0021(6) -0.0062(6) C27 0.0343(9) 0.0289(9) 0.0322(9) 0.0020(7) -0.0070(7) -0.0049(7) C28 0.0256(8) 0.0273(9) 0.0462(10) -0.0069(7) -0.0081(7) 0.0000(7) C29 0.0228(8) 0.0330(9) 0.0386(9) -0.0137(7) 0.0017(7) -0.0065(7) C30 0.0254(8) 0.0280(8) 0.0255(8) -0.0067(6) 0.0005(6) -0.0081(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 S C11 1.7490(16) . ? S Ni 2.1525(8) . ? Ni O1 1.8576(12) . ? Ni N9 1.8956(13) . ? Ni P 2.2183(7) . ? P C19 1.8342(16) . ? P C13 1.8373(16) . ? P C25 1.8374(17) . ? O1 C2 1.322(2) . ? C2 C7 1.419(2) . ? C2 C3 1.421(2) . ? C3 C4 1.385(3) . ? C4 C5 1.400(3) . ? C5 C6 1.377(2) . ? C6 C7 1.423(2) . ? C7 C8 1.429(2) . ? C8 N9 1.309(2) . ? N9 N10 1.4037(17) . ? N10 C11 1.306(2) . ? C11 N12 1.363(2) . ? C13 C14 1.397(2) . ? C13 C18 1.400(2) . ? C14 C15 1.396(2) . ? C15 C16 1.394(3) . ? C16 C17 1.378(3) . ? C17 C18 1.399(2) . ? C19 C20 1.399(2) . ? C19 C24 1.399(2) . ? C20 C21 1.397(2) . ? C21 C22 1.396(2) . ? C22 C23 1.381(3) . ? C23 C24 1.395(2) . ? C25 C26 1.398(2) . ? C25 C30 1.411(2) . ? C26 C27 1.396(2) . ? C27 C28 1.395(3) . ? C28 C29 1.398(3) . ? C29 C30 1.392(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 C11 S Ni 96.03(6) . . ? O1 Ni N9 95.07(6) . . ? O1 Ni S 177.75(4) . . ? N9 Ni S 87.18(5) . . ? O1 Ni P 88.03(5) . . ? N9 Ni P 172.91(4) . . ? S Ni P 89.72(4) . . ? C19 P C13 104.87(7) . . ? C19 P C25 104.11(7) . . ? C13 P C25 104.07(7) . . ? C19 P Ni 119.49(6) . . ? C13 P Ni 107.12(5) . . ? C25 P Ni 115.68(6) . . ? C2 O1 Ni 127.62(10) . . ? O1 C2 C7 124.07(14) . . ? O1 C2 C3 118.43(14) . . ? C7 C2 C3 117.50(15) . . ? C4 C3 C2 121.46(16) . . ? C3 C4 C5 120.90(16) . . ? C6 C5 C4 118.91(16) . . ? C5 C6 C7 121.62(16) . . ? C2 C7 C6 119.59(14) . . ? C2 C7 C8 122.06(14) . . ? C6 C7 C8 118.35(14) . . ? N9 C8 C7 125.98(14) . . ? C8 N9 N10 113.36(13) . . ? C8 N9 Ni 125.14(11) . . ? N10 N9 Ni 121.46(10) . . ? C11 N10 N9 112.08(13) . . ? N10 C11 N12 119.24(14) . . ? N10 C11 S 123.24(12) . . ? N12 C11 S 117.48(12) . . ? C14 C13 C18 118.58(14) . . ? C14 C13 P 122.78(12) . . ? C18 C13 P 118.62(12) . . ? C15 C14 C13 120.23(16) . . ? C16 C15 C14 120.66(17) . . ? C17 C16 C15 119.43(16) . . ? C16 C17 C18 120.38(17) . . ? C17 C18 C13 120.70(16) . . ? C20 C19 C24 118.97(15) . . ? C20 C19 P 119.21(12) . . ? C24 C19 P 121.81(12) . . ? C21 C20 C19 120.11(15) . . ? C22 C21 C20 120.24(16) . . ? C23 C22 C21 119.86(16) . . ? C22 C23 C24 120.15(17) . . ? C23 C24 C19 120.66(16) . . ? C26 C25 C30 119.24(14) . . ? C26 C25 P 122.22(12) . . ? C30 C25 P 118.48(12) . . ? C27 C26 C25 120.38(15) . . ? C28 C27 C26 120.04(16) . . ? C27 C28 C29 120.10(16) . . ? C30 C29 C28 120.02(16) . . ? C29 C30 C25 120.23(15) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.357 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.050 data_npsd _database_code_depnum_ccdc_archive 'CCDC 841841' #TrackingRef 'npsd [Ni(sal-tsc]2(dppe).cif' _audit_creation_date 2011-01-18T10:57:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H26 N4 Ni1 O2 P1 S1' _chemical_formula_sum 'C24 H26 N4 Ni O2 P S' _chemical_formula_weight 524.23 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6356(1) _cell_length_b 10.6275(2) _cell_length_c 14.1718(3) _cell_angle_alpha 89.5995(8) _cell_angle_beta 74.6091(8) _cell_angle_gamma 63.618(1) _cell_volume 1243.08(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17021 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.63 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.838 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI 0.0661 _diffrn_reflns_number 17021 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 28.63 _diffrn_reflns_theta_full 28.63 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 6118 _reflns_number_gt 4535 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6118 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.739 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 C1 C 0.1600(3) -0.2905(2) 0.20369(18) 0.0412(5) Uani 1 1 d . . . C2 C 0.3238(3) -0.3875(3) 0.1611(2) 0.0565(7) Uani 1 1 d . . . H2 H 0.3904 -0.3601 0.1149 0.068 Uiso 1 1 calc R . . C3 C 0.3870(4) -0.5222(3) 0.1868(2) 0.0643(8) Uani 1 1 d . . . H3 H 0.4958 -0.5848 0.1579 0.077 Uiso 1 1 calc R . . C4 C 0.2904(4) -0.5658(3) 0.2553(2) 0.0662(8) Uani 1 1 d . . . H4 H 0.3337 -0.6574 0.2718 0.079 Uiso 1 1 calc R . . C5 C 0.1320(4) -0.4738(3) 0.2981(2) 0.0562(7) Uani 1 1 d . . . H5 H 0.0675 -0.5034 0.3439 0.067 Uiso 1 1 calc R . . C6 C 0.0632(3) -0.3337(2) 0.27438(17) 0.0411(5) Uani 1 1 d . . . C7 C -0.0997(3) -0.2409(2) 0.32830(18) 0.0418(5) Uani 1 1 d . . . H7 H -0.1577 -0.2805 0.3697 0.05 Uiso 1 1 calc R . . C8 C -0.4003(3) 0.0997(3) 0.38746(18) 0.0439(5) Uani 1 1 d . . . C9 C 0.2064(3) 0.0890(3) 0.14214(17) 0.0402(5) Uani 1 1 d . . . C10 C 0.2824(3) 0.1563(3) 0.0808(2) 0.0543(7) Uani 1 1 d . . . H10 H 0.2344 0.211 0.0362 0.065 Uiso 1 1 calc R . . C11 C 0.4303(4) 0.1418(4) 0.0864(3) 0.0754(10) Uani 1 1 d . . . H11 H 0.4826 0.1846 0.0437 0.09 Uiso 1 1 calc R . . C12 C 0.4991(4) 0.0659(4) 0.1531(3) 0.0797(11) Uani 1 1 d . . . H12 H 0.5973 0.0586 0.1568 0.096 Uiso 1 1 calc R . . C13 C 0.4253(4) -0.0002(4) 0.2152(3) 0.0771(10) Uani 1 1 d . . . H13 H 0.4734 -0.0523 0.2608 0.093 Uiso 1 1 calc R . . C14 C 0.2776(3) 0.0108(3) 0.2098(2) 0.0605(7) Uani 1 1 d . . . H14 H 0.2274 -0.0343 0.2516 0.073 Uiso 1 1 calc R . . C15 C -0.0980(3) 0.2921(2) 0.12515(17) 0.0370(5) Uani 1 1 d . . . C16 C -0.1317(3) 0.3460(3) 0.03956(19) 0.0497(6) Uani 1 1 d . . . H16 H -0.1004 0.2848 -0.0172 0.06 Uiso 1 1 calc R . . C17 C -0.2121(4) 0.4913(3) 0.0393(2) 0.0648(8) Uani 1 1 d . . . H17 H -0.2345 0.5271 -0.0179 0.078 Uiso 1 1 calc R . . C18 C -0.2591(4) 0.5831(3) 0.1227(3) 0.0671(8) Uani 1 1 d . . . H18 H -0.3125 0.6804 0.1216 0.081 Uiso 1 1 calc R . . C19 C -0.2271(4) 0.5309(3) 0.2071(2) 0.0619(7) Uani 1 1 d . . . H19 H -0.2593 0.5929 0.2635 0.074 Uiso 1 1 calc R . . C20 C -0.1470(3) 0.3861(3) 0.20914(19) 0.0489(6) Uani 1 1 d . . . H20 H -0.126 0.3516 0.2669 0.059 Uiso 1 1 calc R . . C21 C 0.0695(2) 0.0108(2) 0.00899(15) 0.0329(4) Uani 1 1 d . . . H21A H 0.1001 0.0645 -0.0406 0.039 Uiso 1 1 calc R . . H21B H 0.1628 -0.0808 0.0015 0.039 Uiso 1 1 calc R . . C22 C -0.7732(14) 0.7976(8) 0.4377(6) 0.238(5) Uani 1 1 d . . . H22A H -0.8694 0.887 0.454 0.356 Uiso 1 1 calc R . . H22B H -0.7357 0.7705 0.3676 0.356 Uiso 1 1 calc R . . H22C H -0.6907 0.8059 0.459 0.356 Uiso 1 1 calc R . . C23 C -0.9752(10) 0.7615(7) 0.5466(5) 0.175(3) Uani 1 1 d . . . H23A H -1.0269 0.8601 0.5388 0.262 Uiso 1 1 calc R . . H23B H -0.9776 0.7521 0.6144 0.262 Uiso 1 1 calc R . . H23C H -1.0315 0.7154 0.5276 0.262 Uiso 1 1 calc R . . C24 C -0.7213(12) 0.5692(6) 0.4834(5) 0.181(4) Uani 1 1 d . . . H24 H -0.6138 0.5344 0.4455 0.217 Uiso 1 1 calc R . . N1 N -0.1749(2) -0.1051(2) 0.32494(13) 0.0360(4) Uani 1 1 d . . . N2 N -0.3303(2) -0.0368(2) 0.39009(15) 0.0455(5) Uani 1 1 d . . . N3 N -0.5491(3) 0.1788(3) 0.4478(2) 0.0685(7) Uani 1 1 d . . . H3A H -0.5976 0.1397 0.4877 0.082 Uiso 1 1 calc R . . H3B H -0.5964 0.2688 0.4467 0.082 Uiso 1 1 calc R . . N4 N -0.8076(6) 0.6961(4) 0.4844(3) 0.1006(12) Uani 1 1 d . . . O1 O 0.10487(19) -0.16290(18) 0.17580(13) 0.0478(4) Uani 1 1 d . . . O2 O -0.7586(4) 0.4796(3) 0.5269(2) 0.1130(11) Uani 1 1 d . . . P1 P 0.01505(6) 0.10409(6) 0.13190(4) 0.03182(14) Uani 1 1 d . . . S1 S -0.30655(7) 0.18283(6) 0.30620(4) 0.04026(15) Uani 1 1 d . . . Ni1 Ni -0.08780(3) -0.00480(3) 0.238571(19) 0.03196(11) 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 C1 0.0378(12) 0.0344(12) 0.0414(12) 0.0035(9) -0.0122(10) -0.0077(10) C2 0.0388(13) 0.0479(15) 0.0616(17) 0.0073(13) -0.0079(12) -0.0055(12) C3 0.0474(15) 0.0463(15) 0.071(2) 0.0056(14) -0.0149(14) 0.0016(12) C4 0.0665(18) 0.0366(14) 0.0676(19) 0.0098(13) -0.0200(16) 0.0004(14) C5 0.0647(17) 0.0349(13) 0.0544(16) 0.0093(12) -0.0129(14) -0.0130(13) C6 0.0432(12) 0.0320(11) 0.0402(12) 0.0044(9) -0.0121(10) -0.0105(10) C7 0.0479(13) 0.0335(12) 0.0420(13) 0.0098(10) -0.0089(11) -0.0194(11) C8 0.0371(12) 0.0378(12) 0.0444(13) 0.0050(10) -0.0007(10) -0.0128(10) C9 0.0342(11) 0.0447(13) 0.0394(12) -0.0020(10) -0.0095(9) -0.0166(10) C10 0.0449(14) 0.0587(16) 0.0635(17) 0.0037(13) -0.0095(13) -0.0310(13) C11 0.0480(16) 0.092(2) 0.091(2) -0.015(2) -0.0039(16) -0.0454(18) C12 0.0366(15) 0.093(3) 0.101(3) -0.034(2) -0.0150(17) -0.0239(17) C13 0.0545(18) 0.086(2) 0.089(2) -0.0056(19) -0.0421(18) -0.0186(18) C14 0.0516(15) 0.0718(19) 0.0644(18) 0.0140(15) -0.0303(14) -0.0264(15) C15 0.0338(11) 0.0376(12) 0.0408(12) 0.0092(9) -0.0096(9) -0.0181(10) C16 0.0600(16) 0.0432(14) 0.0448(14) 0.0135(11) -0.0192(12) -0.0208(13) C17 0.079(2) 0.0497(16) 0.0676(19) 0.0251(14) -0.0317(17) -0.0251(16) C18 0.0709(19) 0.0359(14) 0.090(2) 0.0138(15) -0.0255(18) -0.0193(14) C19 0.0701(18) 0.0402(14) 0.0692(19) -0.0038(13) -0.0147(15) -0.0230(14) C20 0.0553(15) 0.0435(14) 0.0466(14) 0.0068(11) -0.0147(12) -0.0218(12) C21 0.0279(10) 0.0391(11) 0.0310(10) 0.0060(9) -0.0051(8) -0.0167(9) C22 0.526(16) 0.187(7) 0.197(7) 0.123(6) -0.247(10) -0.255(10) C23 0.235(8) 0.109(4) 0.112(5) -0.004(4) -0.089(5) 0.001(5) C24 0.341(11) 0.081(4) 0.142(5) 0.031(3) -0.159(7) -0.067(5) N1 0.0320(9) 0.0350(10) 0.0341(9) 0.0044(8) -0.0038(7) -0.0128(8) N2 0.0387(10) 0.0369(11) 0.0445(11) 0.0063(9) 0.0045(9) -0.0125(9) N3 0.0501(13) 0.0427(12) 0.0735(17) 0.0126(11) 0.0204(12) -0.0092(11) N4 0.184(4) 0.0642(19) 0.074(2) 0.0223(16) -0.070(3) -0.057(2) O1 0.0379(8) 0.0387(9) 0.0464(10) 0.0114(8) 0.0007(7) -0.0075(7) O2 0.153(3) 0.0549(16) 0.090(2) 0.0154(14) -0.0238(19) -0.0188(18) P1 0.0293(3) 0.0348(3) 0.0312(3) 0.0069(2) -0.0078(2) -0.0152(2) S1 0.0351(3) 0.0326(3) 0.0420(3) 0.0071(2) -0.0020(2) -0.0112(2) Ni1 0.02888(16) 0.03191(17) 0.03005(17) 0.00683(11) -0.00528(11) -0.01154(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.319(3) . ? C1 C6 1.401(3) . ? C1 C2 1.406(3) . ? C2 C3 1.375(4) . ? C2 H2 0.93 . ? C3 C4 1.386(5) . ? C3 H3 0.93 . ? C4 C5 1.358(4) . ? C4 H4 0.93 . ? C5 C6 1.415(3) . ? C5 H5 0.93 . ? C6 C7 1.421(3) . ? C7 N1 1.303(3) . ? C7 H7 0.93 . ? C8 N2 1.305(3) . ? C8 N3 1.334(3) . ? C8 S1 1.751(2) . ? C9 C14 1.382(4) . ? C9 C10 1.386(4) . ? C9 P1 1.823(2) . ? C10 C11 1.387(4) . ? C10 H10 0.93 . ? C11 C12 1.353(6) . ? C11 H11 0.93 . ? C12 C13 1.370(6) . ? C12 H12 0.93 . ? C13 C14 1.399(4) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C20 1.391(3) . ? C15 C16 1.392(3) . ? C15 P1 1.819(2) . ? C16 C17 1.386(4) . ? C16 H16 0.93 . ? C17 C18 1.375(4) . ? C17 H17 0.93 . ? C18 C19 1.367(4) . ? C18 H18 0.93 . ? C19 C20 1.386(4) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C21 1.539(4) 2 ? C21 P1 1.835(2) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 N4 1.379(7) . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C23 N4 1.458(8) . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 N4 1.227(6) . ? C24 O2 1.264(8) . ? C24 H24 0.93 . ? N1 N2 1.390(3) . ? N1 Ni1 1.8895(18) . ? N3 H3A 0.86 . ? N3 H3B 0.86 . ? O1 Ni1 1.8528(16) . ? P1 Ni1 2.1923(6) . ? S1 Ni1 2.1347(6) . ? 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 C1 C6 123.1(2) . . ? O1 C1 C2 118.5(2) . . ? C6 C1 C2 118.3(2) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.1(2) . . ? C1 C6 C7 123.0(2) . . ? C5 C6 C7 117.7(2) . . ? N1 C7 C6 125.8(2) . . ? N1 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? N2 C8 N3 119.1(2) . . ? N2 C8 S1 122.20(18) . . ? N3 C8 S1 118.64(19) . . ? C14 C9 C10 119.3(2) . . ? C14 C9 P1 121.07(19) . . ? C10 C9 P1 119.60(19) . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 119.8(3) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C20 C15 C16 118.9(2) . . ? C20 C15 P1 117.72(18) . . ? C16 C15 P1 123.29(19) . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.3(2) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C21 C21 P1 112.77(18) 2 . ? C21 C21 H21A 109 2 . ? P1 C21 H21A 109 . . ? C21 C21 H21B 109 2 . ? P1 C21 H21B 109 . . ? H21A C21 H21B 107.8 . . ? N4 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 O2 128.8(9) . . ? N4 C24 H24 115.6 . . ? O2 C24 H24 115.6 . . ? C7 N1 N2 114.32(19) . . ? C7 N1 Ni1 124.49(16) . . ? N2 N1 Ni1 121.18(14) . . ? C8 N2 N1 112.85(19) . . ? C8 N3 H3A 120 . . ? C8 N3 H3B 120 . . ? H3A N3 H3B 120 . . ? C24 N4 C22 131.0(8) . . ? C24 N4 C23 119.3(7) . . ? C22 N4 C23 109.6(6) . . ? C1 O1 Ni1 126.98(15) . . ? C15 P1 C9 102.45(10) . . ? C15 P1 C21 106.96(10) . . ? C9 P1 C21 103.95(9) . . ? C15 P1 Ni1 121.57(7) . . ? C9 P1 Ni1 113.60(8) . . ? C21 P1 Ni1 106.87(7) . . ? C8 S1 Ni1 96.29(8) . . ? O1 Ni1 N1 95.18(8) . . ? O1 Ni1 S1 177.42(5) . . ? N1 Ni1 S1 87.39(6) . . ? O1 Ni1 P1 83.12(5) . . ? N1 Ni1 P1 177.01(6) . . ? S1 Ni1 P1 94.31(2) . . ? # END of CIF data_[Ni(sal-ptsc)(PPh3)] _database_code_depnum_ccdc_archive 'CCDC 849779' #TrackingRef '[Ni(Sal-ptsc)(PPh3)].cif' _audit_creation_date 2011-01-12T11:39:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H26 N3 Ni1 O1 P1 S1' _chemical_formula_sum 'C32 H26 N3 Ni O P S' _chemical_formula_weight 590.3 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.4975(2) _cell_length_b 10.5710(2) _cell_length_c 13.8196(4) _cell_angle_alpha 90 _cell_angle_beta 92.473(1) _cell_angle_gamma 90 _cell_volume 1386.17(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12776 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.7 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_unetI/netI 0.0704 _diffrn_reflns_number 12776 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.7 _diffrn_reflns_theta_full 28.7 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 6653 _reflns_number_gt 5642 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6653 _refine_ls_number_parameters 352 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(13) _refine_diff_density_max 0.702 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.251 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 C1 C 0.3149(4) -0.0779(3) 0.7501(3) 0.0382(7) Uani 1 1 d . . . C2 C 0.4515(4) -0.0863(4) 0.7950(3) 0.0557(10) Uani 1 1 d . . . H2 H 0.4801 -0.0272 0.8417 0.067 Uiso 1 1 calc R . . C3 C 0.5427(5) -0.1817(5) 0.7699(4) 0.0654(13) Uani 1 1 d . . . H3 H 0.633 -0.1845 0.7986 0.078 Uiso 1 1 calc R . . C4 C 0.5011(5) -0.2737(5) 0.7021(4) 0.0608(11) Uani 1 1 d . . . H4 H 0.5621 -0.3388 0.6869 0.073 Uiso 1 1 calc R . . C5 C 0.3693(5) -0.2668(4) 0.6584(3) 0.0541(10) Uani 1 1 d . . . H5 H 0.3417 -0.3283 0.6134 0.065 Uiso 1 1 calc R . . C6 C 0.2740(4) -0.1694(3) 0.6795(3) 0.0399(8) Uani 1 1 d . . . C7 C 0.1393(4) -0.1682(3) 0.6306(3) 0.0409(8) Uani 1 1 d . . . H7 H 0.1189 -0.2339 0.5875 0.049 Uiso 1 1 calc R . . C8 C -0.1726(4) -0.0175(3) 0.5927(3) 0.0380(7) Uani 1 1 d . . . C9 C -0.3646(4) -0.1143(3) 0.4843(3) 0.0390(7) Uani 1 1 d . . . C10 C -0.3020(4) -0.2284(3) 0.4633(3) 0.0425(8) Uani 1 1 d . . . H10 H -0.214 -0.2487 0.4911 0.051 Uiso 1 1 calc R . . C11 C -0.3713(4) -0.3123(4) 0.4008(3) 0.0498(10) Uani 1 1 d . . . H11 H -0.3287 -0.3888 0.3864 0.06 Uiso 1 1 calc R . . C12 C -0.5030(5) -0.2843(4) 0.3593(3) 0.0543(10) Uani 1 1 d . . . H12 H -0.5478 -0.3406 0.3165 0.065 Uiso 1 1 calc R . . C13 C -0.5671(5) -0.1706(5) 0.3825(3) 0.0559(10) Uani 1 1 d . . . H13 H -0.6566 -0.1516 0.3565 0.067 Uiso 1 1 calc R . . C14 C -0.4981(4) -0.0857(4) 0.4442(3) 0.0481(9) Uani 1 1 d . . . H14 H -0.5408 -0.0093 0.4589 0.058 Uiso 1 1 calc R . . C15 C 0.2428(4) 0.2730(3) 0.8609(3) 0.0404(8) Uani 1 1 d . . . C16 C 0.3162(4) 0.3681(4) 0.8180(3) 0.0485(9) Uani 1 1 d . . . H16 H 0.2745 0.413 0.7665 0.058 Uiso 1 1 calc R . . C17 C 0.4534(5) 0.3976(5) 0.8512(4) 0.0646(13) Uani 1 1 d . . . H17 H 0.5027 0.4619 0.8215 0.078 Uiso 1 1 calc R . . C18 C 0.5147(5) 0.3330(6) 0.9264(4) 0.0756(16) Uani 1 1 d . . . H18 H 0.6053 0.3543 0.949 0.091 Uiso 1 1 calc R . . C19 C 0.4431(5) 0.2350(6) 0.9701(4) 0.0714(14) Uani 1 1 d . . . H19 H 0.4856 0.1905 1.0216 0.086 Uiso 1 1 calc R . . C20 C 0.3075(4) 0.2039(4) 0.9361(3) 0.0551(10) Uani 1 1 d . . . H20 H 0.26 0.1369 0.9636 0.066 Uiso 1 1 calc R . . C21 C -0.0146(3) 0.3720(3) 0.7675(2) 0.0351(7) Uani 1 1 d . . . C22 C -0.1005(4) 0.4493(4) 0.8219(3) 0.0465(9) Uani 1 1 d . . . H22 H -0.1201 0.427 0.885 0.056 Uiso 1 1 calc R . . C23 C -0.1560(4) 0.5587(5) 0.7819(3) 0.0537(9) Uani 1 1 d . . . H23 H -0.2131 0.6098 0.8185 0.064 Uiso 1 1 calc R . . C24 C -0.1283(5) 0.5937(4) 0.6885(3) 0.0551(11) Uani 1 1 d . . . H24 H -0.1649 0.6685 0.6625 0.066 Uiso 1 1 calc R . . C25 C -0.0461(5) 0.5165(4) 0.6343(3) 0.0562(10) Uani 1 1 d . . . H25 H -0.0275 0.5391 0.571 0.067 Uiso 1 1 calc R . . C26 C 0.0091(4) 0.4061(4) 0.6726(3) 0.0466(9) Uani 1 1 d . . . H26 H 0.0628 0.3538 0.6346 0.056 Uiso 1 1 calc R . . C27 C -0.0299(4) 0.1968(3) 0.9274(3) 0.0381(7) Uani 1 1 d . . . C28 C -0.1329(4) 0.1041(4) 0.9270(3) 0.0459(9) Uani 1 1 d . . . H28 H -0.1486 0.0536 0.8725 0.055 Uiso 1 1 calc R . . C29 C -0.2121(5) 0.0865(4) 1.0071(3) 0.0561(11) Uani 1 1 d . . . H29 H -0.2804 0.0235 1.0067 0.067 Uiso 1 1 calc R . . C30 C -0.1907(5) 0.1611(5) 1.0868(3) 0.0588(11) Uani 1 1 d . . . H30 H -0.2458 0.1493 1.1401 0.071 Uiso 1 1 calc R . . C31 C -0.0895(5) 0.2531(4) 1.0894(3) 0.0574(11) Uani 1 1 d . . . H31 H -0.0755 0.3032 1.1443 0.069 Uiso 1 1 calc R . . C32 C -0.0078(5) 0.2715(4) 1.0100(3) 0.0493(9) Uani 1 1 d . . . H32 H 0.0617 0.3335 1.0116 0.059 Uiso 1 1 calc R . . N1 N 0.0423(3) -0.0833(3) 0.6407(2) 0.0349(6) Uani 1 1 d . . . N2 N -0.0814(3) -0.1083(3) 0.5846(2) 0.0396(6) Uani 1 1 d . . . N3 N -0.3019(3) -0.0205(3) 0.5451(2) 0.0461(7) Uani 1 1 d . . . H3A H -0.3533 0.0452 0.5536 0.055 Uiso 1 1 calc R . . O1 O 0.2334(3) 0.0149(2) 0.77642(19) 0.0423(6) Uani 1 1 d . . . P1 P 0.06513(9) 0.22730(7) 0.81721(6) 0.03340(19) Uani 1 1 d . . . S1 S -0.13835(11) 0.11940(10) 0.65972(9) 0.0521(3) Uani 1 1 d . . . Ni1 Ni 0.06072(4) 0.06070(4) 0.72070(3) 0.03266(12) 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 C1 0.0371(18) 0.0350(17) 0.0427(19) 0.0066(13) 0.0029(14) 0.0089(13) C2 0.046(2) 0.053(2) 0.066(3) -0.0015(19) -0.009(2) 0.0148(17) C3 0.045(2) 0.069(3) 0.082(4) 0.004(2) -0.003(2) 0.024(2) C4 0.052(2) 0.062(3) 0.069(3) -0.003(2) 0.006(2) 0.025(2) C5 0.056(2) 0.052(2) 0.054(2) -0.0082(18) 0.0032(19) 0.0194(19) C6 0.0427(19) 0.0356(17) 0.0419(19) 0.0046(14) 0.0070(15) 0.0081(13) C7 0.048(2) 0.0335(17) 0.0406(19) -0.0054(13) 0.0014(15) 0.0052(13) C8 0.0391(18) 0.0361(17) 0.0385(18) 0.0016(13) -0.0022(14) 0.0012(13) C9 0.0425(18) 0.0372(17) 0.0371(18) -0.0004(14) -0.0009(14) -0.0071(14) C10 0.0442(19) 0.0420(18) 0.0413(19) -0.0029(14) 0.0033(15) -0.0031(15) C11 0.054(2) 0.046(2) 0.051(2) -0.0106(16) 0.0140(19) -0.0117(17) C12 0.058(2) 0.058(2) 0.047(2) -0.0072(18) -0.0005(18) -0.0224(19) C13 0.047(2) 0.067(3) 0.053(2) -0.001(2) -0.0081(18) -0.0167(19) C14 0.042(2) 0.047(2) 0.054(2) 0.0005(17) -0.0040(17) -0.0031(15) C15 0.0354(17) 0.0389(18) 0.046(2) -0.0127(15) -0.0009(14) 0.0060(14) C16 0.041(2) 0.055(2) 0.051(2) -0.0134(17) 0.0072(16) -0.0046(16) C17 0.043(2) 0.073(3) 0.079(3) -0.021(3) 0.014(2) -0.012(2) C18 0.037(2) 0.110(4) 0.079(4) -0.030(3) -0.006(2) -0.001(2) C19 0.046(2) 0.094(4) 0.073(3) -0.008(3) -0.017(2) 0.011(2) C20 0.044(2) 0.061(3) 0.060(3) -0.0061(19) -0.0074(18) 0.0044(18) C21 0.0320(16) 0.0326(16) 0.0406(18) -0.0019(13) 0.0014(13) 0.0021(12) C22 0.046(2) 0.044(2) 0.050(2) -0.0004(16) 0.0067(17) 0.0121(15) C23 0.052(2) 0.0435(18) 0.066(2) 0.003(2) 0.0061(18) 0.016(2) C24 0.056(2) 0.039(2) 0.070(3) 0.0127(17) -0.007(2) 0.0101(15) C25 0.065(3) 0.055(2) 0.048(2) 0.0161(18) 0.006(2) 0.0030(19) C26 0.051(2) 0.042(2) 0.047(2) -0.0005(15) 0.0109(17) 0.0086(15) C27 0.0374(17) 0.0363(17) 0.0410(18) 0.0007(13) 0.0058(14) 0.0080(13) C28 0.045(2) 0.0410(19) 0.052(2) 0.0022(15) 0.0044(17) 0.0008(14) C29 0.055(2) 0.052(3) 0.062(3) 0.0118(18) 0.010(2) -0.0007(17) C30 0.067(3) 0.061(3) 0.050(2) 0.011(2) 0.024(2) 0.011(2) C31 0.073(3) 0.057(3) 0.043(2) -0.0059(17) 0.010(2) 0.009(2) C32 0.063(2) 0.043(2) 0.042(2) -0.0047(16) 0.0063(17) 0.0010(18) N1 0.0355(14) 0.0301(13) 0.0389(15) -0.0004(11) -0.0002(12) 0.0025(10) N2 0.0381(15) 0.0367(15) 0.0435(16) -0.0039(12) -0.0043(12) 0.0007(11) N3 0.0415(17) 0.0406(16) 0.055(2) -0.0108(14) -0.0103(14) 0.0071(12) O1 0.0415(13) 0.0373(13) 0.0473(15) -0.0060(10) -0.0070(11) 0.0104(9) P1 0.0343(4) 0.0295(4) 0.0363(4) -0.0033(3) 0.0003(3) 0.0041(3) S1 0.0460(5) 0.0404(5) 0.0681(7) -0.0193(4) -0.0193(5) 0.0143(4) Ni1 0.0338(2) 0.02833(19) 0.0356(2) -0.00263(17) -0.00135(14) 0.00537(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 O1 1.311(4) . ? C1 C6 1.416(5) . ? C1 C2 1.416(5) . ? C2 C3 1.383(6) . ? C2 H2 0.93 . ? C3 C4 1.396(7) . ? C3 H3 0.93 . ? C4 C5 1.368(6) . ? C4 H4 0.93 . ? C5 C6 1.410(5) . ? C5 H5 0.93 . ? C6 C7 1.421(5) . ? C7 N1 1.298(4) . ? C7 H7 0.93 . ? C8 N2 1.301(4) . ? C8 N3 1.367(5) . ? C8 S1 1.742(4) . ? C9 C10 1.381(5) . ? C9 C14 1.395(6) . ? C9 N3 1.415(4) . ? C10 C11 1.385(5) . ? C10 H10 0.93 . ? C11 C12 1.385(6) . ? C11 H11 0.93 . ? C12 C13 1.391(7) . ? C12 H12 0.93 . ? C13 C14 1.383(6) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C16 1.373(6) . ? C15 C20 1.390(6) . ? C15 P1 1.832(4) . ? C16 C17 1.398(6) . ? C16 H16 0.93 . ? C17 C18 1.354(8) . ? C17 H17 0.93 . ? C18 C19 1.392(9) . ? C18 H18 0.93 . ? C19 C20 1.392(6) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C26 1.388(5) . ? C21 C22 1.397(5) . ? C21 P1 1.827(3) . ? C22 C23 1.377(6) . ? C22 H22 0.93 . ? C23 C24 1.379(6) . ? C23 H23 0.93 . ? C24 C25 1.374(6) . ? C24 H24 0.93 . ? C25 C26 1.376(6) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 C28 1.384(5) . ? C27 C32 1.395(5) . ? C27 P1 1.832(4) . ? C28 C29 1.377(6) . ? C28 H28 0.93 . ? C29 C30 1.363(7) . ? C29 H29 0.93 . ? C30 C31 1.367(7) . ? C30 H30 0.93 . ? C31 C32 1.385(6) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? N1 N2 1.405(4) . ? N1 Ni1 1.885(3) . ? N3 H3A 0.86 . ? O1 Ni1 1.846(2) . ? P1 Ni1 2.2085(9) . ? S1 Ni1 2.1290(10) . ? 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 C1 C6 123.7(3) . . ? O1 C1 C2 117.8(3) . . ? C6 C1 C2 118.5(3) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.1(4) . . ? C4 C5 H5 119 . . ? C6 C5 H5 119 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 118.7(4) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 C6 125.7(3) . . ? N1 C7 H7 117.2 . . ? C6 C7 H7 117.2 . . ? N2 C8 N3 121.9(3) . . ? N2 C8 S1 123.3(3) . . ? N3 C8 S1 114.7(2) . . ? C10 C9 C14 119.9(3) . . ? C10 C9 N3 124.2(3) . . ? C14 C9 N3 115.9(3) . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 121.2(4) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.2(4) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C16 C15 C20 119.4(4) . . ? C16 C15 P1 121.9(3) . . ? C20 C15 P1 118.6(3) . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.4(5) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C15 C20 C19 120.1(5) . . ? C15 C20 H20 120 . . ? C19 C20 H20 120 . . ? C26 C21 C22 118.6(3) . . ? C26 C21 P1 119.4(3) . . ? C22 C21 P1 122.0(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 119.0(4) . . ? C28 C27 P1 119.6(3) . . ? C32 C27 P1 121.2(3) . . ? C29 C28 C27 120.2(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.8(4) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C27 119.9(4) . . ? C31 C32 H32 120 . . ? C27 C32 H32 120 . . ? C7 N1 N2 113.0(3) . . ? C7 N1 Ni1 125.0(3) . . ? N2 N1 Ni1 122.0(2) . . ? C8 N2 N1 111.0(3) . . ? C8 N3 C9 130.4(3) . . ? C8 N3 H3A 114.8 . . ? C9 N3 H3A 114.8 . . ? C1 O1 Ni1 127.2(2) . . ? C21 P1 C27 104.40(15) . . ? C21 P1 C15 105.31(16) . . ? C27 P1 C15 104.57(17) . . ? C21 P1 Ni1 116.35(11) . . ? C27 P1 Ni1 111.38(12) . . ? C15 P1 Ni1 113.74(11) . . ? C8 S1 Ni1 96.37(12) . . ? O1 Ni1 N1 95.24(11) . . ? O1 Ni1 S1 177.92(8) . . ? N1 Ni1 S1 86.84(9) . . ? O1 Ni1 P1 87.92(8) . . ? N1 Ni1 P1 175.58(9) . . ? S1 Ni1 P1 90.00(4) . . ? # END of CIF