#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100740.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100740 _publ_requested_journal 'Angewandte Chemie International Edition' loop_ _publ_author_name 'Baudron, Stephane A.' 'Avarvari, Narcis' 'Batail, Patrick' _publ_section_title ; A General Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen Bond Donor/Acceptor Groups ; _chemical_name_common '(PPh4)[Ni(midt)2]' _chemical_formula_sum 'C32 H22 N2 Ni O4 P S4' _chemical_formula_weight 716.44 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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9413(17) _cell_length_b 11.9501(17) _cell_length_c 13.0235(16) _cell_angle_alpha 77.422(16) _cell_angle_beta 76.190(17) _cell_angle_gamma 74.858(17) _cell_volume 1574.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7685 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 52.1 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.693 _exptl_crystal_size_mid 0.5775 _exptl_crystal_size_min 0.2694 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5358 _exptl_absorpt_correction_T_max 0.7483 _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS' _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.8' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15845 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5657 _reflns_number_gt 3057 _reflns_threshold_expression >2sigma(I) _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^)+(0.0240P)^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 5657 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 0.781 _refine_ls_restrained_S_all 0.781 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.66767(5) 0.94764(4) 0.70560(4) 0.04092(14) Uani 1 1 d . . . S1 S 0.67352(10) 0.83794(8) 0.86200(7) 0.0480(3) Uani 1 1 d . . . S2 S 0.65111(10) 1.10817(7) 0.76522(8) 0.0476(3) Uani 1 1 d . . . S3 S 0.69541(13) 0.78562(8) 0.64504(8) 0.0682(4) Uani 1 1 d . . . S4 S 0.65844(10) 1.05725(7) 0.54931(7) 0.0470(3) Uani 1 1 d . . . C1 C 0.6825(3) 0.9201(3) 1.0509(3) 0.0400(9) Uani 1 1 d . . . C2 C 0.6705(3) 0.9383(3) 0.9378(3) 0.0362(9) Uani 1 1 d . . . C3 C 0.6619(3) 1.0539(3) 0.8953(3) 0.0367(9) Uani 1 1 d . . . C4 C 0.6709(3) 1.1155(3) 0.9801(3) 0.0437(9) Uani 1 1 d . . . C5 C 0.6984(5) 0.7724(3) 0.4263(3) 0.0672(14) Uani 1 1 d . . . C6 C 0.6900(4) 0.8375(3) 0.5141(3) 0.0483(10) Uani 1 1 d . . . C7 C 0.6740(3) 0.9534(3) 0.4725(3) 0.0389(9) Uani 1 1 d . . . C8 C 0.6761(3) 0.9685(3) 0.3558(3) 0.0415(9) Uani 1 1 d . . . O1 O 0.6940(3) 0.8298(2) 1.1163(2) 0.0572(8) Uani 1 1 d . . . O2 O 0.6738(3) 1.2163(2) 0.9751(2) 0.0656(8) Uani 1 1 d . . . O3 O 0.7083(4) 0.6700(2) 0.4303(2) 0.1163(16) Uani 1 1 d . . . O4 O 0.6651(3) 1.0575(2) 0.2899(2) 0.0542(7) Uani 1 1 d . . . N1 N 0.6833(3) 1.0297(2) 1.0694(2) 0.0462(8) Uani 1 1 d . . . H1 H 0.6906 1.0429 1.1298 0.055 Uiso 1 1 calc R . . N2 N 0.6923(3) 0.8567(2) 0.3352(2) 0.0533(9) Uani 1 1 d . . . H2 H 0.6979 0.8410 0.2726 0.064 Uiso 1 1 calc R . . P1 P 0.84342(9) 1.36932(7) 0.27465(8) 0.0380(2) Uani 1 1 d . . . C9 C 0.8103(4) 1.3775(3) 0.4143(3) 0.0439(9) Uani 1 1 d . . . C10 C 0.6868(4) 1.3837(3) 0.4732(3) 0.0554(11) Uani 1 1 d . . . H10 H 0.6197 1.3841 0.4406 0.066 Uiso 1 1 calc R . . C11 C 0.6635(5) 1.3894(4) 0.5816(4) 0.0771(15) Uani 1 1 d . . . H11 H 0.5803 1.3941 0.6219 0.093 Uiso 1 1 calc R . . C12 C 0.7617(7) 1.3882(5) 0.6292(4) 0.0935(18) Uani 1 1 d . . . H12 H 0.7453 1.3920 0.7019 0.112 Uiso 1 1 calc R . . C13 C 0.8835(6) 1.3815(4) 0.5716(4) 0.0937(17) Uani 1 1 d . . . H13 H 0.9498 1.3811 0.6051 0.112 Uiso 1 1 calc R . . C14 C 0.9102(5) 1.3754(4) 0.4630(4) 0.0704(13) Uani 1 1 d . . . H14 H 0.9940 1.3700 0.4237 0.084 Uiso 1 1 calc R . . C15 C 0.9071(3) 1.2191(3) 0.2555(3) 0.0447(9) Uani 1 1 d . . . C16 C 0.9231(4) 1.1900(4) 0.1556(4) 0.0719(13) Uani 1 1 d . . . H16 H 0.8984 1.2473 0.0989 0.086 Uiso 1 1 calc R . . C17 C 0.9760(5) 1.0755(5) 0.1403(5) 0.0950(18) Uani 1 1 d . . . H17 H 0.9886 1.0555 0.0729 0.114 Uiso 1 1 calc R . . C18 C 1.0100(5) 0.9915(4) 0.2242(6) 0.0874(19) Uani 1 1 d . . . H18 H 1.0456 0.9143 0.2134 0.105 Uiso 1 1 calc R . . C19 C 0.9925(4) 1.0189(4) 0.3229(5) 0.0805(15) Uani 1 1 d . . . H19 H 1.0148 0.9606 0.3796 0.097 Uiso 1 1 calc R . . C20 C 0.9415(4) 1.1334(3) 0.3395(4) 0.0576(11) Uani 1 1 d . . . H20 H 0.9305 1.1525 0.4071 0.069 Uiso 1 1 calc R . . C21 C 0.6995(3) 1.4259(3) 0.2204(3) 0.0353(8) Uani 1 1 d . . . C22 C 0.6252(4) 1.3524(3) 0.2134(3) 0.0590(11) Uani 1 1 d . . . H22 H 0.6478 1.2722 0.2386 0.071 Uiso 1 1 calc R . . C23 C 0.5162(4) 1.3990(4) 0.1684(4) 0.0725(14) Uani 1 1 d . . . H23 H 0.4660 1.3495 0.1627 0.087 Uiso 1 1 calc R . . C24 C 0.4817(4) 1.5169(4) 0.1324(3) 0.0594(12) Uani 1 1 d . . . H24 H 0.4091 1.5470 0.1013 0.071 Uiso 1 1 calc R . . C25 C 0.5528(4) 1.5898(3) 0.1420(3) 0.0569(11) Uani 1 1 d . . . H25 H 0.5274 1.6704 0.1198 0.068 Uiso 1 1 calc R . . C26 C 0.6619(4) 1.5450(3) 0.1843(3) 0.0505(10) Uani 1 1 d . . . H26 H 0.7117 1.5955 0.1888 0.061 Uiso 1 1 calc R . . C27 C 0.9590(3) 1.4564(3) 0.2084(3) 0.0428(9) Uani 1 1 d . . . C28 C 0.9386(4) 1.5695(3) 0.2272(3) 0.0594(11) Uani 1 1 d . . . H28 H 0.8676 1.5982 0.2775 0.071 Uiso 1 1 calc R . . C29 C 1.0221(6) 1.6406(4) 0.1724(4) 0.0817(16) Uani 1 1 d . . . H29 H 1.0063 1.7177 0.1840 0.098 Uiso 1 1 calc R . . C30 C 1.1282(5) 1.5973(6) 0.1010(5) 0.0899(19) Uani 1 1 d . . . H30 H 1.1848 1.6450 0.0638 0.108 Uiso 1 1 calc R . . C31 C 1.1514(5) 1.4862(6) 0.0839(4) 0.0891(17) Uani 1 1 d . . . H31 H 1.2255 1.4569 0.0368 0.107 Uiso 1 1 calc R . . C32 C 1.0672(4) 1.4155(4) 0.1351(3) 0.0656(12) Uani 1 1 d . . . H32 H 1.0829 1.3396 0.1206 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0495(3) 0.0389(2) 0.0302(3) -0.00738(18) -0.0042(2) -0.0047(2) S1 0.0721(7) 0.0362(5) 0.0349(6) -0.0060(4) -0.0084(5) -0.0123(5) S2 0.0671(7) 0.0358(5) 0.0358(6) -0.0027(4) -0.0129(5) -0.0045(5) S3 0.1254(11) 0.0373(5) 0.0327(6) -0.0047(4) -0.0093(7) -0.0084(6) S4 0.0693(7) 0.0376(5) 0.0352(6) -0.0057(4) -0.0122(5) -0.0119(5) C1 0.041(2) 0.038(2) 0.040(2) -0.0084(18) -0.0052(19) -0.0075(17) C2 0.033(2) 0.0385(19) 0.036(2) -0.0088(16) -0.0058(18) -0.0057(16) C3 0.038(2) 0.0341(19) 0.037(2) -0.0056(16) -0.0096(18) -0.0027(16) C4 0.046(2) 0.044(2) 0.041(2) -0.0070(18) -0.012(2) -0.0057(18) C5 0.116(4) 0.041(2) 0.033(2) -0.0111(19) -0.005(3) -0.003(2) C6 0.069(3) 0.037(2) 0.032(2) -0.0071(17) -0.004(2) -0.0063(19) C7 0.043(2) 0.038(2) 0.034(2) -0.0070(16) -0.0081(18) -0.0054(17) C8 0.046(2) 0.040(2) 0.038(2) -0.0093(18) -0.006(2) -0.0086(18) O1 0.095(2) 0.0414(14) 0.0361(16) -0.0017(12) -0.0195(16) -0.0149(14) O2 0.107(2) 0.0380(15) 0.0615(19) -0.0050(13) -0.0306(18) -0.0213(16) O3 0.249(5) 0.0380(17) 0.049(2) -0.0126(14) -0.019(3) -0.015(2) O4 0.086(2) 0.0403(14) 0.0368(16) 0.0013(12) -0.0181(15) -0.0144(14) N1 0.063(2) 0.0409(17) 0.0383(19) -0.0073(14) -0.0176(17) -0.0097(15) N2 0.085(3) 0.0442(18) 0.0280(18) -0.0091(14) -0.0073(18) -0.0094(17) P1 0.0402(6) 0.0386(5) 0.0340(6) -0.0061(4) -0.0059(5) -0.0075(4) C9 0.050(3) 0.042(2) 0.039(2) -0.0049(16) -0.007(2) -0.0115(18) C10 0.064(3) 0.055(2) 0.040(2) -0.0039(18) -0.006(2) -0.008(2) C11 0.088(4) 0.070(3) 0.050(3) -0.006(2) 0.013(3) -0.005(3) C12 0.123(5) 0.114(4) 0.039(3) -0.016(3) -0.002(4) -0.028(4) C13 0.123(5) 0.129(5) 0.049(3) -0.020(3) -0.029(4) -0.048(4) C14 0.066(3) 0.104(3) 0.049(3) -0.013(3) -0.014(3) -0.030(3) C15 0.042(2) 0.043(2) 0.048(3) -0.0083(18) -0.013(2) -0.0045(18) C16 0.084(4) 0.067(3) 0.063(3) -0.028(2) -0.019(3) 0.005(3) C17 0.083(4) 0.098(4) 0.114(5) -0.071(4) -0.008(4) -0.003(3) C18 0.054(3) 0.057(3) 0.150(6) -0.038(4) -0.017(4) 0.005(2) C19 0.071(4) 0.044(3) 0.122(5) 0.000(3) -0.035(3) -0.001(2) C20 0.052(3) 0.046(2) 0.073(3) -0.003(2) -0.020(2) -0.006(2) C21 0.041(2) 0.0339(19) 0.033(2) -0.0069(15) -0.0041(17) -0.0130(16) C22 0.061(3) 0.044(2) 0.077(3) -0.003(2) -0.024(3) -0.016(2) C23 0.061(3) 0.081(3) 0.091(4) -0.016(3) -0.028(3) -0.029(3) C24 0.043(3) 0.074(3) 0.062(3) -0.014(2) -0.020(2) -0.002(2) C25 0.053(3) 0.044(2) 0.071(3) -0.014(2) -0.018(2) 0.004(2) C26 0.049(3) 0.044(2) 0.063(3) -0.0108(19) -0.018(2) -0.0094(19) C27 0.043(2) 0.049(2) 0.037(2) 0.0013(17) -0.015(2) -0.0117(18) C28 0.061(3) 0.061(2) 0.066(3) -0.009(2) -0.014(2) -0.027(2) C29 0.094(4) 0.069(3) 0.099(4) 0.012(3) -0.041(4) -0.048(3) C30 0.060(4) 0.124(5) 0.082(4) 0.046(4) -0.031(3) -0.050(4) C31 0.045(3) 0.123(4) 0.078(4) 0.009(3) 0.005(3) -0.017(3) C32 0.046(3) 0.078(3) 0.062(3) -0.002(2) -0.005(2) -0.007(2)