# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Gonzalez-Sebastian, Lucero' 'Flores-Alamo, Marcos' 'Garcia, Juve' _publ_contact_author_name 'Dr Juve Garcia' _publ_contact_author_email juvent@servidor.unam.mx _publ_section_title ; Reduction of CO2 and SO2 with low valent Nickel compounds under mild conditions ; _publ_requested_category FM # Attachment '- luc-01 y 02 COMP-1 y 5- 23marz2011.cif' #\#CIF_1.1 data_1 _database_code_depnum_ccdc_archive 'CCDC 827160' #TrackingRef '- luc-01 y 02 COMP-1 y 5- 23marz2011.cif' _audit_creation_date 2010-03-03T15:59:46-00:00 _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 ; {[(dippe)Ni(CO)]2(mu-dippe)} ; _chemical_formula_moiety 'C44 H96 Ni2 O2 P6 ' _chemical_formula_sum 'C44 H96 Ni2 O2 P6' _chemical_formula_weight 960.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7220(6) _cell_length_b 11.5158(8) _cell_length_c 14.3744(10) _cell_angle_alpha 102.320(6) _cell_angle_beta 91.092(6) _cell_angle_gamma 112.112(7) _cell_volume 1298.88(18) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5413 _cell_measurement_theta_min 4.2631 _cell_measurement_theta_max 67.9937 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2879 _exptl_crystal_size_mid 0.1852 _exptl_crystal_size_min 0.0495 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 0 0.0352 -1 2 0 0.0433 2 0 0 0.1455 0 -1 3 0.0295 0 1 -3 0.0201 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.881 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.901 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 10.4685 _diffrn_orient_matrix_ub_11 -0.0070891 _diffrn_orient_matrix_ub_12 0.0592171 _diffrn_orient_matrix_ub_13 -0.0856901 _diffrn_orient_matrix_ub_21 -0.0495764 _diffrn_orient_matrix_ub_22 -0.1337837 _diffrn_orient_matrix_ub_23 -0.0689466 _diffrn_orient_matrix_ub_31 -0.1851576 _diffrn_orient_matrix_ub_32 -0.0264376 _diffrn_orient_matrix_ub_33 0.0091898 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_number 8546 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 68.11 _diffrn_reflns_theta_full 68.11 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4721 _reflns_number_gt 4010 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0263P)^2^+2.6979P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4721 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.472 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # 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 0.0181 0.0091 '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' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 Ni1 Ni 0.36555(5) 0.25539(4) 0.29183(3) 0.01202(12) Uani 1 1 d . . . P1 P 0.52992(8) 0.32190(6) 0.18289(5) 0.01450(15) Uani 1 1 d . . . P2 P 0.27197(8) 0.05540(6) 0.20727(5) 0.01427(15) Uani 1 1 d . . . P3 P 0.46353(8) 0.28855(6) 0.44325(4) 0.01084(14) Uani 1 1 d . . . O1 O 0.1190(3) 0.3706(2) 0.29917(16) 0.0295(5) Uani 1 1 d . . . C1 C -0.0414(4) 0.0431(3) 0.1405(2) 0.0302(7) Uani 1 1 d . . . H1A H -0.1589 -0.0109 0.1187 0.045 Uiso 1 1 calc R . . H1B H 0.0137 0.0765 0.0874 0.045 Uiso 1 1 calc R . . H1C H -0.033 0.1154 0.1935 0.045 Uiso 1 1 calc R . . C2 C 0.0434(4) -0.0378(3) 0.1747(2) 0.0228(6) Uani 1 1 d . . . H2 H 0.0266 -0.1142 0.121 0.027 Uiso 1 1 calc R . . C3 C -0.0394(4) -0.0865(3) 0.2588(2) 0.0310(7) Uani 1 1 d . . . H3A H -0.0264 -0.0128 0.3117 0.047 Uiso 1 1 calc R . . H3B H 0.013 -0.1397 0.2798 0.047 Uiso 1 1 calc R . . H3C H -0.1581 -0.1383 0.2389 0.047 Uiso 1 1 calc R . . C4 C 0.2548(5) -0.2069(3) 0.1736(2) 0.0336(8) Uani 1 1 d . . . H4A H 0.2777 -0.2061 0.1072 0.05 Uiso 1 1 calc R . . H4B H 0.1343 -0.2381 0.1768 0.05 Uiso 1 1 calc R . . H4C H 0.2985 -0.2641 0.1962 0.05 Uiso 1 1 calc R . . C5 C 0.3387(4) -0.0702(3) 0.2369(2) 0.0202(6) Uani 1 1 d . . . H5 H 0.3115 -0.0755 0.3035 0.024 Uiso 1 1 calc R . . C6 C 0.5276(4) -0.0260(3) 0.2392(2) 0.0301(7) Uani 1 1 d . . . H6A H 0.5646 -0.0811 0.2694 0.045 Uiso 1 1 calc R . . H6B H 0.581 0.0637 0.2761 0.045 Uiso 1 1 calc R . . H6C H 0.5583 -0.0324 0.1737 0.045 Uiso 1 1 calc R . . C7 C 0.2963(4) 0.3410(3) 0.0549(2) 0.0306(7) Uani 1 1 d . . . H7A H 0.2159 0.3142 0.1006 0.046 Uiso 1 1 calc R . . H7B H 0.2951 0.2644 0.0087 0.046 Uiso 1 1 calc R . . H7C H 0.266 0.3958 0.0208 0.046 Uiso 1 1 calc R . . C8 C 0.4707(4) 0.4167(3) 0.1087(2) 0.0221(6) Uani 1 1 d . . . H8 H 0.5518 0.435 0.0601 0.027 Uiso 1 1 calc R . . C9 C 0.4799(5) 0.5457(3) 0.1695(2) 0.0325(8) Uani 1 1 d . . . H9A H 0.4475 0.5926 0.1286 0.049 Uiso 1 1 calc R . . H9B H 0.5939 0.597 0.1998 0.049 Uiso 1 1 calc R . . H9C H 0.404 0.5302 0.219 0.049 Uiso 1 1 calc R . . C10 C 0.8239(4) 0.5237(3) 0.2834(2) 0.0318(7) Uani 1 1 d . . . H10A H 0.939 0.5433 0.3075 0.048 Uiso 1 1 calc R . . H10B H 0.7529 0.5096 0.3353 0.048 Uiso 1 1 calc R . . H10C H 0.8193 0.5962 0.2598 0.048 Uiso 1 1 calc R . . C11 C 0.7625(4) 0.4022(3) 0.2019(2) 0.0217(6) Uani 1 1 d . . . H11 H 0.801 0.3401 0.224 0.026 Uiso 1 1 calc R . . C12 C 0.8521(4) 0.4296(4) 0.1131(2) 0.0384(9) Uani 1 1 d . . . H12A H 0.8303 0.4983 0.0926 0.058 Uiso 1 1 calc R . . H12B H 0.8111 0.3511 0.0612 0.058 Uiso 1 1 calc R . . H12C H 0.9722 0.4569 0.129 0.058 Uiso 1 1 calc R . . C13 C 0.5086(4) 0.1748(3) 0.0905(2) 0.0199(6) Uani 1 1 d . . . H13A H 0.5196 0.1958 0.027 0.024 Uiso 1 1 calc R . . H13B H 0.6002 0.148 0.1044 0.024 Uiso 1 1 calc R . . C14 C 0.3421(4) 0.0623(3) 0.08640(19) 0.0200(6) Uani 1 1 d . . . H14A H 0.3531 -0.0196 0.0567 0.024 Uiso 1 1 calc R . . H14B H 0.2566 0.0714 0.0454 0.024 Uiso 1 1 calc R . . C15 C 0.6878(4) 0.2698(3) 0.5842(2) 0.0236(6) Uani 1 1 d . . . H15A H 0.7724 0.2356 0.5943 0.035 Uiso 1 1 calc R . . H15B H 0.59 0.2282 0.6156 0.035 Uiso 1 1 calc R . . H15C H 0.7333 0.3632 0.6114 0.035 Uiso 1 1 calc R . . C16 C 0.6372(3) 0.2421(3) 0.47679(19) 0.0167(6) Uani 1 1 d . . . H16 H 0.5973 0.1465 0.4518 0.02 Uiso 1 1 calc R . . C17 C 0.7897(4) 0.3020(3) 0.4263(2) 0.0290(7) Uani 1 1 d . . . H17A H 0.8413 0.3952 0.454 0.043 Uiso 1 1 calc R . . H17B H 0.7557 0.2859 0.3578 0.043 Uiso 1 1 calc R . . H17C H 0.8701 0.2632 0.4347 0.043 Uiso 1 1 calc R . . C18 C 0.1455(3) 0.2293(3) 0.5062(2) 0.0191(6) Uani 1 1 d . . . H18A H 0.0926 0.186 0.4406 0.029 Uiso 1 1 calc R . . H18B H 0.1711 0.322 0.5172 0.029 Uiso 1 1 calc R . . H18C H 0.0697 0.1935 0.5517 0.029 Uiso 1 1 calc R . . C19 C 0.3060(3) 0.2084(3) 0.52055(18) 0.0153(5) Uani 1 1 d . . . H19 H 0.3538 0.2491 0.5889 0.018 Uiso 1 1 calc R . . C20 C 0.2669(4) 0.0639(3) 0.5029(2) 0.0220(6) Uani 1 1 d . . . H20A H 0.1824 0.0258 0.5436 0.033 Uiso 1 1 calc R . . H20B H 0.3684 0.0511 0.5183 0.033 Uiso 1 1 calc R . . H20C H 0.2248 0.0223 0.4354 0.033 Uiso 1 1 calc R . . C21 C 0.5412(3) 0.4579(2) 0.51524(19) 0.0143(5) Uani 1 1 d . . . H21A H 0.5246 0.4567 0.583 0.017 Uiso 1 1 calc R . . H21B H 0.6624 0.4987 0.5118 0.017 Uiso 1 1 calc R . . C22 C 0.2152(3) 0.3236(3) 0.29744(18) 0.0168(6) 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 Ni1 0.0109(2) 0.0137(2) 0.0109(2) 0.00105(17) 0.00118(16) 0.00522(18) P1 0.0141(4) 0.0160(3) 0.0133(3) 0.0037(3) 0.0037(3) 0.0055(3) P2 0.0136(4) 0.0140(3) 0.0124(3) -0.0002(2) 0.0016(2) 0.0040(3) P3 0.0100(3) 0.0103(3) 0.0116(3) 0.0014(2) 0.0001(2) 0.0040(2) O1 0.0232(12) 0.0353(12) 0.0366(13) 0.0062(10) 0.0017(9) 0.0201(10) C1 0.0145(16) 0.0390(19) 0.0287(17) -0.0015(14) -0.0055(12) 0.0067(14) C2 0.0171(15) 0.0224(15) 0.0185(14) -0.0043(12) -0.0016(11) 0.0013(12) C3 0.0157(16) 0.0351(18) 0.0301(17) 0.0038(14) 0.0069(13) -0.0015(13) C4 0.045(2) 0.0228(16) 0.0333(18) -0.0009(14) 0.0059(15) 0.0169(15) C5 0.0254(16) 0.0186(14) 0.0206(14) 0.0065(11) 0.0073(12) 0.0116(12) C6 0.0313(18) 0.0307(17) 0.0352(18) 0.0069(14) 0.0029(14) 0.0203(15) C7 0.0292(18) 0.0380(18) 0.0292(17) 0.0194(14) 0.0011(13) 0.0120(15) C8 0.0238(16) 0.0265(16) 0.0202(14) 0.0115(12) 0.0071(12) 0.0110(13) C9 0.041(2) 0.0281(17) 0.0367(19) 0.0153(14) 0.0080(15) 0.0189(16) C10 0.0244(18) 0.0244(16) 0.0370(18) 0.0005(14) -0.0053(14) 0.0029(14) C11 0.0166(15) 0.0242(15) 0.0223(15) 0.0082(12) 0.0037(11) 0.0043(12) C12 0.0198(17) 0.057(2) 0.0330(19) 0.0166(17) 0.0093(14) 0.0060(16) C13 0.0198(15) 0.0233(15) 0.0156(13) 0.0014(11) 0.0067(11) 0.0091(12) C14 0.0227(16) 0.0195(14) 0.0136(13) -0.0008(11) 0.0038(11) 0.0060(12) C15 0.0229(16) 0.0254(15) 0.0249(15) 0.0059(12) -0.0049(12) 0.0126(13) C16 0.0137(14) 0.0169(13) 0.0205(14) 0.0029(11) -0.0003(11) 0.0079(11) C17 0.0195(16) 0.0434(19) 0.0337(17) 0.0152(15) 0.0051(13) 0.0194(15) C18 0.0161(15) 0.0174(14) 0.0211(14) 0.0033(11) 0.0047(11) 0.0041(11) C19 0.0135(14) 0.0164(13) 0.0130(12) 0.0015(10) 0.0010(10) 0.0037(11) C20 0.0226(16) 0.0172(14) 0.0259(15) 0.0081(12) 0.0050(12) 0.0057(12) C21 0.0135(14) 0.0119(12) 0.0155(13) 0.0010(10) -0.0032(10) 0.0042(11) C22 0.0152(14) 0.0179(13) 0.0133(13) 0.0016(10) 0.0006(10) 0.0032(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C22 1.759(3) . ? Ni1 P2 2.1909(8) . ? Ni1 P1 2.2057(8) . ? Ni1 P3 2.2231(8) . ? P1 C13 1.861(3) . ? P1 C8 1.870(3) . ? P1 C11 1.872(3) . ? P2 C14 1.861(3) . ? P2 C2 1.867(3) . ? P2 C5 1.870(3) . ? P3 C21 1.857(3) . ? P3 C16 1.872(3) . ? P3 C19 1.875(3) . ? O1 C22 1.155(3) . ? C1 C2 1.535(4) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.521(4) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C5 1.529(4) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.528(4) . ? C5 H5 1 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.530(4) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.527(4) . ? C8 H8 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.526(4) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.538(4) . ? C11 H11 1 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.529(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.529(4) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.527(4) . ? C16 H16 1 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.525(4) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.529(4) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C21 1.530(5) 2_666 ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? 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 C22 Ni1 P2 113.19(9) . . ? C22 Ni1 P1 108.67(9) . . ? P2 Ni1 P1 91.36(3) . . ? C22 Ni1 P3 105.23(9) . . ? P2 Ni1 P3 116.10(3) . . ? P1 Ni1 P3 122.09(3) . . ? C13 P1 C8 101.29(13) . . ? C13 P1 C11 98.84(13) . . ? C8 P1 C11 103.09(13) . . ? C13 P1 Ni1 106.51(9) . . ? C8 P1 Ni1 117.10(10) . . ? C11 P1 Ni1 125.92(9) . . ? C14 P2 C2 100.51(13) . . ? C14 P2 C5 101.83(13) . . ? C2 P2 C5 101.29(14) . . ? C14 P2 Ni1 106.20(9) . . ? C2 P2 Ni1 120.05(10) . . ? C5 P2 Ni1 123.34(10) . . ? C21 P3 C16 100.14(12) . . ? C21 P3 C19 99.63(12) . . ? C16 P3 C19 99.84(12) . . ? C21 P3 Ni1 116.09(8) . . ? C16 P3 Ni1 122.44(9) . . ? C19 P3 Ni1 115.03(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 109.4(3) . . ? C3 C2 P2 111.1(2) . . ? C1 C2 P2 111.7(2) . . ? C3 C2 H2 108.2 . . ? C1 C2 H2 108.2 . . ? P2 C2 H2 108.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C4 109.5(2) . . ? C6 C5 P2 109.9(2) . . ? C4 C5 P2 116.8(2) . . ? C6 C5 H5 106.7 . . ? C4 C5 H5 106.7 . . ? P2 C5 H5 106.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C7 109.5(3) . . ? C9 C8 P1 111.5(2) . . ? C7 C8 P1 111.7(2) . . ? C9 C8 H8 108 . . ? C7 C8 H8 108 . . ? P1 C8 H8 108 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C10 C11 C12 110.3(3) . . ? C10 C11 P1 112.3(2) . . ? C12 C11 P1 116.7(2) . . ? C10 C11 H11 105.5 . . ? C12 C11 H11 105.5 . . ? P1 C11 H11 105.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 112.72(18) . . ? C14 C13 H13A 109 . . ? P1 C13 H13A 109 . . ? C14 C13 H13B 109 . . ? P1 C13 H13B 109 . . ? H13A C13 H13B 107.8 . . ? C13 C14 P2 112.20(18) . . ? C13 C14 H14A 109.2 . . ? P2 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? P2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C15 110.0(2) . . ? C17 C16 P3 111.05(19) . . ? C15 C16 P3 115.76(19) . . ? C17 C16 H16 106.5 . . ? C15 C16 H16 106.5 . . ? P3 C16 H16 106.5 . . ? 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 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18 C19 C20 109.7(2) . . ? C18 C19 P3 111.27(19) . . ? C20 C19 P3 112.31(19) . . ? C18 C19 H19 107.8 . . ? C20 C19 H19 107.8 . . ? P3 C19 H19 107.8 . . ? 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 . . ? C21 C21 P3 115.4(2) 2_666 . ? C21 C21 H21A 108.4 2_666 . ? P3 C21 H21A 108.4 . . ? C21 C21 H21B 108.4 2_666 . ? P3 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? O1 C22 Ni1 177.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Ni1 P1 C13 -119.37(13) . . . . ? P2 Ni1 P1 C13 -4.29(10) . . . . ? P3 Ni1 P1 C13 118.00(10) . . . . ? C22 Ni1 P1 C8 -6.97(14) . . . . ? P2 Ni1 P1 C8 108.11(11) . . . . ? P3 Ni1 P1 C8 -129.60(11) . . . . ? C22 Ni1 P1 C11 126.26(15) . . . . ? P2 Ni1 P1 C11 -118.67(12) . . . . ? P3 Ni1 P1 C11 3.62(13) . . . . ? C22 Ni1 P2 C14 98.26(14) . . . . ? P1 Ni1 P2 C14 -12.75(10) . . . . ? P3 Ni1 P2 C14 -139.86(10) . . . . ? C22 Ni1 P2 C2 -14.55(15) . . . . ? P1 Ni1 P2 C2 -125.56(11) . . . . ? P3 Ni1 P2 C2 107.33(12) . . . . ? C22 Ni1 P2 C5 -145.20(15) . . . . ? P1 Ni1 P2 C5 103.79(11) . . . . ? P3 Ni1 P2 C5 -23.32(12) . . . . ? C22 Ni1 P3 C21 -53.48(14) . . . . ? P2 Ni1 P3 C21 -179.48(10) . . . . ? P1 Ni1 P3 C21 70.74(10) . . . . ? C22 Ni1 P3 C16 -176.41(14) . . . . ? P2 Ni1 P3 C16 57.59(11) . . . . ? P1 Ni1 P3 C16 -52.18(11) . . . . ? C22 Ni1 P3 C19 62.25(13) . . . . ? P2 Ni1 P3 C19 -63.75(10) . . . . ? P1 Ni1 P3 C19 -173.52(9) . . . . ? C14 P2 C2 C3 165.7(2) . . . . ? C5 P2 C2 C3 61.2(2) . . . . ? Ni1 P2 C2 C3 -78.5(2) . . . . ? C14 P2 C2 C1 -71.9(2) . . . . ? C5 P2 C2 C1 -176.3(2) . . . . ? Ni1 P2 C2 C1 43.9(2) . . . . ? C14 P2 C5 C6 61.1(2) . . . . ? C2 P2 C5 C6 164.5(2) . . . . ? Ni1 P2 C5 C6 -57.5(2) . . . . ? C14 P2 C5 C4 -64.4(2) . . . . ? C2 P2 C5 C4 39.0(3) . . . . ? Ni1 P2 C5 C4 176.94(19) . . . . ? C13 P1 C8 C9 -179.6(2) . . . . ? C11 P1 C8 C9 -77.6(2) . . . . ? Ni1 P1 C8 C9 65.1(2) . . . . ? C13 P1 C8 C7 57.5(2) . . . . ? C11 P1 C8 C7 159.5(2) . . . . ? Ni1 P1 C8 C7 -57.8(2) . . . . ? C13 P1 C11 C10 -174.3(2) . . . . ? C8 P1 C11 C10 81.8(2) . . . . ? Ni1 P1 C11 C10 -56.4(3) . . . . ? C13 P1 C11 C12 56.9(3) . . . . ? C8 P1 C11 C12 -46.9(3) . . . . ? Ni1 P1 C11 C12 174.8(2) . . . . ? C8 P1 C13 C14 -97.8(2) . . . . ? C11 P1 C13 C14 156.8(2) . . . . ? Ni1 P1 C13 C14 25.1(2) . . . . ? P1 C13 C14 P2 -36.9(3) . . . . ? C2 P2 C14 C13 157.4(2) . . . . ? C5 P2 C14 C13 -98.6(2) . . . . ? Ni1 P2 C14 C13 31.6(2) . . . . ? C21 P3 C16 C17 -75.5(2) . . . . ? C19 P3 C16 C17 -177.2(2) . . . . ? Ni1 P3 C16 C17 54.5(2) . . . . ? C21 P3 C16 C15 50.9(2) . . . . ? C19 P3 C16 C15 -50.8(2) . . . . ? Ni1 P3 C16 C15 -179.08(17) . . . . ? C21 P3 C19 C18 78.7(2) . . . . ? C16 P3 C19 C18 -179.14(19) . . . . ? Ni1 P3 C19 C18 -46.2(2) . . . . ? C21 P3 C19 C20 -157.9(2) . . . . ? C16 P3 C19 C20 -55.8(2) . . . . ? Ni1 P3 C19 C20 77.2(2) . . . . ? C16 P3 C21 C21 162.5(3) . . . 2_666 ? C19 P3 C21 C21 -95.6(3) . . . 2_666 ? Ni1 P3 C21 C21 28.5(3) . . . 2_666 ? # END of CIF ############################################################################## #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_5 _database_code_depnum_ccdc_archive 'CCDC 827161' #TrackingRef '- luc-01 y 02 COMP-1 y 5- 23marz2011.cif' _audit_creation_date 2010-04-21T15:22:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; [(dippe)Ni(S2O3)] ; _chemical_formula_moiety 'C14 H32 Ni1 O3 P2 S2' _chemical_formula_sum 'C14 H32 Ni O3 P2 S2' _chemical_formula_weight 433.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system tetragonal _space_group_name_H-M_alt 'P 42/n' _space_group_name_Hall '-P 4bc' _space_group_IT_number 86 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 22.7088(3) _cell_length_b 22.7088(3) _cell_length_c 7.9025(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4075.24(13) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 12863 _cell_measurement_theta_min 3.5816 _cell_measurement_theta_max 25.989 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.2666 _exptl_crystal_size_mid 0.0823 _exptl_crystal_size_min 0.0443 _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -3 0 0.0308 1 -1 0 0.0244 -1 1 0 0.0199 1 0 0 0.0386 -1 0 0 0.0386 0 0 1 0 1 2 -1 0.2283 0 -2 -1 0.2009 1 3 0 0.0308 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.948 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 10.4685 _diffrn_orient_matrix_ub_11 -0.0269773 _diffrn_orient_matrix_ub_12 0.0156513 _diffrn_orient_matrix_ub_13 -0.0059942 _diffrn_orient_matrix_ub_21 0.0154946 _diffrn_orient_matrix_ub_22 0.0270262 _diffrn_orient_matrix_ub_23 0.0064064 _diffrn_orient_matrix_ub_31 0.0029419 _diffrn_orient_matrix_ub_32 0.0009306 _diffrn_orient_matrix_ub_33 -0.0892555 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_number 29432 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 4020 _reflns_number_gt 3187 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0572P)^2^+0.4066P] 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_number_reflns 4020 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.887 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # 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' Ni Ni 0.3393 1.1124 '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' 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 0.89266(14) 0.40712(13) 0.9618(4) 0.0322(7) Uani 1 1 d . . . H1 H 0.8622 0.3833 1.0168 0.039 Uiso 1 1 calc R . . C2 C 0.90995(16) 0.45568(15) 1.0852(4) 0.0405(8) Uani 1 1 d . . . H2A H 0.925 0.4384 1.1873 0.061 Uiso 1 1 calc R . . H2B H 0.876 0.4792 1.1112 0.061 Uiso 1 1 calc R . . H2C H 0.9397 0.48 1.0349 0.061 Uiso 1 1 calc R . . C3 C 0.94499(15) 0.36602(15) 0.9242(5) 0.0432(9) Uani 1 1 d . . . H3A H 0.9754 0.3878 0.8678 0.065 Uiso 1 1 calc R . . H3B H 0.9321 0.3343 0.853 0.065 Uiso 1 1 calc R . . H3C H 0.96 0.3504 1.0285 0.065 Uiso 1 1 calc R . . C4 C 0.84309(14) 0.37488(13) 0.6297(4) 0.0326(7) Uani 1 1 d . . . H4 H 0.8807 0.3558 0.6035 0.039 Uiso 1 1 calc R . . C5 C 0.80485(18) 0.32864(15) 0.7165(6) 0.0546(11) Uani 1 1 d . . . H5A H 0.7664 0.3447 0.7375 0.082 Uiso 1 1 calc R . . H5B H 0.8226 0.3174 0.8219 0.082 Uiso 1 1 calc R . . H5C H 0.8014 0.2947 0.6447 0.082 Uiso 1 1 calc R . . C6 C 0.81688(16) 0.39401(15) 0.4630(5) 0.0447(9) Uani 1 1 d . . . H6A H 0.8106 0.3601 0.3926 0.067 Uiso 1 1 calc R . . H6B H 0.8434 0.4207 0.4075 0.067 Uiso 1 1 calc R . . H6C H 0.78 0.4134 0.4829 0.067 Uiso 1 1 calc R . . C7 C 0.78626(13) 0.59523(13) 0.4924(4) 0.0266(7) Uani 1 1 d . . . H7 H 0.7513 0.6117 0.5479 0.032 Uiso 1 1 calc R . . C8 C 0.76439(14) 0.54890(15) 0.3686(4) 0.0370(8) Uani 1 1 d . . . H8A H 0.737 0.5665 0.2912 0.055 Uiso 1 1 calc R . . H8B H 0.7452 0.5178 0.4297 0.055 Uiso 1 1 calc R . . H8C H 0.7971 0.5331 0.3066 0.055 Uiso 1 1 calc R . . C9 C 0.81614(17) 0.64614(15) 0.3989(4) 0.0457(9) Uani 1 1 d . . . H9A H 0.8512 0.6321 0.3443 0.069 Uiso 1 1 calc R . . H9B H 0.8263 0.6765 0.4782 0.069 Uiso 1 1 calc R . . H9C H 0.7897 0.6618 0.3154 0.069 Uiso 1 1 calc R . . C10 C 0.85393(12) 0.62414(12) 0.7947(4) 0.0225(6) Uani 1 1 d . . . H10 H 0.8721 0.6539 0.7218 0.027 Uiso 1 1 calc R . . C11 C 0.79984(13) 0.65198(13) 0.8785(4) 0.0310(7) Uani 1 1 d . . . H11A H 0.7799 0.6229 0.9457 0.046 Uiso 1 1 calc R . . H11B H 0.7736 0.6664 0.7928 0.046 Uiso 1 1 calc R . . H11C H 0.8121 0.684 0.9495 0.046 Uiso 1 1 calc R . . C12 C 0.89911(14) 0.60591(13) 0.9264(4) 0.0310(7) Uani 1 1 d . . . H12A H 0.9101 0.6396 0.9929 0.047 Uiso 1 1 calc R . . H12B H 0.9333 0.5904 0.8708 0.047 Uiso 1 1 calc R . . H12C H 0.8825 0.5763 0.9988 0.047 Uiso 1 1 calc R . . C13 C 0.89774(12) 0.53089(12) 0.5596(4) 0.0241(6) Uani 1 1 d . . . H13A H 0.8886 0.5186 0.4451 0.029 Uiso 1 1 calc R . . H13B H 0.9281 0.5609 0.554 0.029 Uiso 1 1 calc R . . C14 C 0.92045(12) 0.47807(13) 0.6608(4) 0.0262(7) Uani 1 1 d . . . H14A H 0.9484 0.4917 0.745 0.031 Uiso 1 1 calc R . . H14B H 0.9409 0.4514 0.5852 0.031 Uiso 1 1 calc R . . Ni1 Ni 0.786233(14) 0.494797(14) 0.80310(4) 0.01836(12) Uani 1 1 d . . . O1 O 0.71378(8) 0.53785(8) 0.8171(3) 0.0273(5) Uani 1 1 d . . . O2 O 0.66390(11) 0.53479(12) 1.0857(3) 0.0519(7) Uani 1 1 d . . . O3 O 0.62787(9) 0.47567(10) 0.8638(3) 0.0397(6) Uani 1 1 d . . . P1 P 0.83135(3) 0.56181(3) 0.65954(9) 0.01863(17) Uani 1 1 d . . . P2 P 0.86011(3) 0.43814(3) 0.76729(10) 0.02315(18) Uani 1 1 d . . . S1 S 0.67918(3) 0.50049(3) 0.94059(9) 0.02371(18) Uani 1 1 d . . . S2 S 0.74128(4) 0.43946(4) 0.98805(13) 0.0442(3) 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 0.0344(17) 0.0280(16) 0.0343(18) 0.0064(14) 0.0036(14) 0.0116(13) C2 0.051(2) 0.0388(19) 0.0319(18) -0.0007(15) -0.0019(16) 0.0216(16) C3 0.046(2) 0.0381(19) 0.045(2) -0.0030(16) -0.0065(17) 0.0233(16) C4 0.0305(16) 0.0226(15) 0.0448(19) -0.0064(14) 0.0073(15) 0.0035(13) C5 0.066(3) 0.0277(18) 0.070(3) -0.0071(18) 0.013(2) -0.0157(17) C6 0.048(2) 0.0331(18) 0.053(2) -0.0138(17) -0.0101(18) -0.0063(16) C7 0.0273(15) 0.0271(15) 0.0254(15) 0.0018(12) -0.0002(12) 0.0017(12) C8 0.0354(18) 0.0397(19) 0.0358(18) -0.0038(15) -0.0113(15) -0.0034(14) C9 0.070(3) 0.0360(19) 0.0313(19) 0.0127(15) -0.0116(18) -0.0162(18) C10 0.0212(14) 0.0180(14) 0.0282(16) -0.0012(12) 0.0045(12) -0.0057(11) C11 0.0270(16) 0.0291(16) 0.0368(18) -0.0103(14) 0.0081(14) -0.0050(13) C12 0.0343(17) 0.0280(16) 0.0308(17) -0.0050(13) -0.0077(14) -0.0052(13) C13 0.0200(14) 0.0251(15) 0.0274(15) -0.0034(12) 0.0067(12) -0.0046(12) C14 0.0196(14) 0.0305(16) 0.0285(16) -0.0069(13) 0.0057(12) 0.0020(12) Ni1 0.01365(19) 0.01550(19) 0.0259(2) 0.00237(14) 0.00391(14) 0.00014(13) O1 0.0139(9) 0.0235(10) 0.0446(13) 0.0125(9) 0.0067(9) 0.0040(8) O2 0.0429(14) 0.0756(18) 0.0373(14) -0.0137(13) -0.0029(11) 0.0151(13) O3 0.0217(11) 0.0443(13) 0.0532(15) 0.0075(12) -0.0042(10) -0.0105(10) P1 0.0160(3) 0.0175(3) 0.0224(4) 0.0001(3) 0.0029(3) -0.0024(3) P2 0.0194(4) 0.0201(4) 0.0300(4) 0.0012(3) 0.0052(3) 0.0047(3) S1 0.0173(3) 0.0241(4) 0.0297(4) 0.0014(3) 0.0050(3) -0.0007(3) S2 0.0323(5) 0.0369(5) 0.0635(6) 0.0150(4) 0.0167(4) 0.0053(4) #----------------------------------------------------------------------------# # 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 C2 1.524(5) . ? C1 C3 1.540(4) . ? C1 P2 1.845(3) . ? C1 H1 0.98 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 C6 1.509(5) . ? C4 C5 1.526(5) . ? C4 P2 1.843(3) . ? C4 H4 0.98 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 C8 1.520(4) . ? C7 C9 1.531(4) . ? C7 P1 1.835(3) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 C12 1.519(4) . ? C10 C11 1.532(4) . ? C10 P1 1.846(3) . ? C10 H10 0.98 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C14 1.531(4) . ? C13 P1 1.841(3) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 P2 1.846(3) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? Ni1 O1 1.9172(18) . ? Ni1 P2 2.1332(8) . ? Ni1 P1 2.1570(7) . ? Ni1 S2 2.1812(9) . ? Ni1 S1 2.6660(7) . ? O1 S1 1.513(2) . ? O2 S1 1.429(3) . ? O3 S1 1.429(2) . ? S1 S2 2.0125(11) . ? 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 C2 C1 C3 111.3(3) . . ? C2 C1 P2 111.1(2) . . ? C3 C1 P2 112.3(2) . . ? C2 C1 H1 107.3 . . ? C3 C1 H1 107.3 . . ? P2 C1 H1 107.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 111.5(3) . . ? C6 C4 P2 111.9(2) . . ? C5 C4 P2 113.0(2) . . ? C6 C4 H4 106.7 . . ? C5 C4 H4 106.7 . . ? P2 C4 H4 106.7 . . ? 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 . . ? C8 C7 C9 110.9(3) . . ? C8 C7 P1 111.1(2) . . ? C9 C7 P1 114.4(2) . . ? C8 C7 H7 106.7 . . ? C9 C7 H7 106.7 . . ? P1 C7 H7 106.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.9(2) . . ? C12 C10 P1 112.04(19) . . ? C11 C10 P1 110.12(19) . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? P1 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 110.53(19) . . ? C14 C13 H13A 109.5 . . ? P1 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 P2 111.90(19) . . ? C13 C14 H14A 109.2 . . ? P2 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? P2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O1 Ni1 P2 172.00(7) . . ? O1 Ni1 P1 94.49(6) . . ? P2 Ni1 P1 88.98(3) . . ? O1 Ni1 S2 81.57(6) . . ? P2 Ni1 S2 96.29(3) . . ? P1 Ni1 S2 168.88(4) . . ? O1 Ni1 S1 33.81(6) . . ? P2 Ni1 S1 143.18(3) . . ? P1 Ni1 S1 127.83(3) . . ? S2 Ni1 S1 47.78(3) . . ? S1 O1 Ni1 101.36(10) . . ? C7 P1 C13 107.82(14) . . ? C7 P1 C10 104.73(13) . . ? C13 P1 C10 108.25(13) . . ? C7 P1 Ni1 113.90(10) . . ? C13 P1 Ni1 110.21(9) . . ? C10 P1 Ni1 111.63(9) . . ? C4 P2 C1 106.15(15) . . ? C4 P2 C14 105.65(14) . . ? C1 P2 C14 105.66(14) . . ? C4 P2 Ni1 112.55(10) . . ? C1 P2 Ni1 115.76(10) . . ? C14 P2 Ni1 110.36(9) . . ? O2 S1 O3 110.95(15) . . ? O2 S1 O1 109.74(15) . . ? O3 S1 O1 111.76(13) . . ? O2 S1 S2 113.33(11) . . ? O3 S1 S2 112.26(10) . . ? O1 S1 S2 98.19(8) . . ? O2 S1 Ni1 125.09(11) . . ? O3 S1 Ni1 123.45(11) . . ? S2 S1 Ni1 53.38(3) . . ? S1 S2 Ni1 78.83(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C13 C14 P2 30.8(3) . . . . ? P1 Ni1 O1 S1 -171.26(10) . . . . ? S2 Ni1 O1 S1 -1.73(10) . . . . ? C8 C7 P1 C13 64.5(2) . . . . ? C9 C7 P1 C13 -61.9(3) . . . . ? C8 C7 P1 C10 179.6(2) . . . . ? C9 C7 P1 C10 53.2(3) . . . . ? C8 C7 P1 Ni1 -58.1(2) . . . . ? C9 C7 P1 Ni1 175.4(2) . . . . ? C14 C13 P1 C7 -151.1(2) . . . . ? C14 C13 P1 C10 96.1(2) . . . . ? C14 C13 P1 Ni1 -26.2(2) . . . . ? C12 C10 P1 C7 -171.7(2) . . . . ? C11 C10 P1 C7 64.3(2) . . . . ? C12 C10 P1 C13 -56.9(2) . . . . ? C11 C10 P1 C13 179.1(2) . . . . ? C12 C10 P1 Ni1 64.6(2) . . . . ? C11 C10 P1 Ni1 -59.4(2) . . . . ? O1 Ni1 P1 C7 -41.77(13) . . . . ? P2 Ni1 P1 C7 131.02(11) . . . . ? S2 Ni1 P1 C7 -110.5(2) . . . . ? S1 Ni1 P1 C7 -47.91(11) . . . . ? O1 Ni1 P1 C13 -163.09(12) . . . . ? P2 Ni1 P1 C13 9.70(10) . . . . ? S2 Ni1 P1 C13 128.19(19) . . . . ? S1 Ni1 P1 C13 -169.23(10) . . . . ? O1 Ni1 P1 C10 76.59(12) . . . . ? P2 Ni1 P1 C10 -110.62(10) . . . . ? S2 Ni1 P1 C10 7.9(2) . . . . ? S1 Ni1 P1 C10 70.44(10) . . . . ? C6 C4 P2 C1 -179.0(2) . . . . ? C5 C4 P2 C1 54.1(3) . . . . ? C6 C4 P2 C14 -67.1(3) . . . . ? C5 C4 P2 C14 166.0(2) . . . . ? C6 C4 P2 Ni1 53.4(3) . . . . ? C5 C4 P2 Ni1 -73.5(3) . . . . ? C2 C1 P2 C4 178.8(2) . . . . ? C3 C1 P2 C4 53.4(3) . . . . ? C2 C1 P2 C14 66.9(2) . . . . ? C3 C1 P2 C14 -58.5(3) . . . . ? C2 C1 P2 Ni1 -55.5(3) . . . . ? C3 C1 P2 Ni1 179.1(2) . . . . ? C13 C14 P2 C4 98.4(2) . . . . ? C13 C14 P2 C1 -149.3(2) . . . . ? C13 C14 P2 Ni1 -23.5(2) . . . . ? P1 Ni1 P2 C4 -112.01(12) . . . . ? S2 Ni1 P2 C4 77.81(12) . . . . ? S1 Ni1 P2 C4 66.58(13) . . . . ? P1 Ni1 P2 C1 125.66(12) . . . . ? S2 Ni1 P2 C1 -44.52(13) . . . . ? S1 Ni1 P2 C1 -55.75(13) . . . . ? P1 Ni1 P2 C14 5.74(11) . . . . ? S2 Ni1 P2 C14 -164.44(11) . . . . ? S1 Ni1 P2 C14 -175.67(11) . . . . ? Ni1 O1 S1 O2 120.35(13) . . . . ? Ni1 O1 S1 O3 -116.13(13) . . . . ? Ni1 O1 S1 S2 1.88(10) . . . . ? O1 Ni1 S1 O2 -83.05(18) . . . . ? P2 Ni1 S1 O2 109.79(14) . . . . ? P1 Ni1 S1 O2 -71.99(14) . . . . ? S2 Ni1 S1 O2 94.64(15) . . . . ? O1 Ni1 S1 O3 88.03(17) . . . . ? P2 Ni1 S1 O3 -79.13(13) . . . . ? P1 Ni1 S1 O3 99.08(12) . . . . ? S2 Ni1 S1 O3 -94.29(12) . . . . ? P2 Ni1 S1 O1 -167.16(13) . . . . ? P1 Ni1 S1 O1 11.06(12) . . . . ? S2 Ni1 S1 O1 177.69(13) . . . . ? O1 Ni1 S1 S2 -177.69(13) . . . . ? P2 Ni1 S1 S2 15.15(7) . . . . ? P1 Ni1 S1 S2 -166.63(5) . . . . ? O2 S1 S2 Ni1 -117.36(13) . . . . ? O3 S1 S2 Ni1 115.97(12) . . . . ? O1 S1 S2 Ni1 -1.65(9) . . . . ? O1 Ni1 S2 S1 1.30(7) . . . . ? P2 Ni1 S2 S1 -170.93(4) . . . . ? P1 Ni1 S2 S1 71.20(18) . . . . ? # END of CIF ##############################################################################