# 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_requested_category FM _publ_contact_author_email rpnchemist@gmail.com _publ_contact_author_name 'R. Prabhakaran' loop_ _publ_author_name 'Rathinasabapathi Prabhakaran' 'Kalaivani Palaniappan' 'Karuppannan Natarajan' data_pp20 _database_code_depnum_ccdc_archive 'CCDC 815366' #TrackingRef '[Pd(H-Msal-etsc)Cl(PPh3)].cif' _audit_creation_date 2010-05-06T10:13:11-00:00 _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 'C29 H29 Cl1 N3 O2 P1 Pd1 S1' _chemical_formula_sum 'C29 H29 Cl N3 O2 P Pd S' _chemical_formula_weight 656.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9284(3) _cell_length_b 10.2817(2) _cell_length_c 18.9004(3) _cell_angle_alpha 90 _cell_angle_beta 102.443(1) _cell_angle_gamma 90 _cell_volume 2832.87(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23720 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.72 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 0.847 #----------------------------------------------------------------------------# # 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 0.069 _diffrn_reflns_av_unetI/netI 0.1141 _diffrn_reflns_number 23720 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 28.72 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 7187 _reflns_number_gt 4239 _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^)+(0.0589P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7187 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.093 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.741 _refine_diff_density_min -0.93 _refine_diff_density_rms 0.152 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 0.1834(2) 0.2699(4) 1.03725(19) 0.0350(8) Uani 1 1 d . . . C2 C 0.1280(3) 0.3787(4) 1.0310(2) 0.0480(10) Uani 1 1 d . . . H2 H 0.1185 0.428 0.9888 0.058 Uiso 1 1 calc R . . C3 C 0.0867(3) 0.4154(5) 1.0863(3) 0.0584(12) Uani 1 1 d . . . H3 H 0.0498 0.4892 1.0814 0.07 Uiso 1 1 calc R . . C4 C 0.0998(3) 0.3430(4) 1.1490(2) 0.0516(11) Uani 1 1 d . . . H4 H 0.0718 0.3676 1.1864 0.062 Uiso 1 1 calc R . . C5 C 0.1541(3) 0.2347(4) 1.1560(2) 0.0518(11) Uani 1 1 d . . . H5 H 0.163 0.1857 1.1983 0.062 Uiso 1 1 calc R . . C6 C 0.1959(3) 0.1976(4) 1.1006(2) 0.0470(10) Uani 1 1 d . . . H6 H 0.2326 0.1237 1.1059 0.056 Uiso 1 1 calc R . . C7 C 0.1809(3) 0.0824(4) 0.9191(2) 0.0392(9) Uani 1 1 d . . . C8 C 0.1145(3) 0.0137(4) 0.9442(2) 0.0493(11) Uani 1 1 d . . . H8 H 0.0991 0.0375 0.9875 0.059 Uiso 1 1 calc R . . C9 C 0.0709(3) -0.0904(5) 0.9049(3) 0.0629(13) Uani 1 1 d . . . H9 H 0.0258 -0.1358 0.9217 0.075 Uiso 1 1 calc R . . C10 C 0.0935(4) -0.1271(5) 0.8418(3) 0.0669(14) Uani 1 1 d . . . H10 H 0.0641 -0.1976 0.8159 0.08 Uiso 1 1 calc R . . C11 C 0.1590(4) -0.0611(5) 0.8165(3) 0.0774(17) Uani 1 1 d . . . H11 H 0.1746 -0.0865 0.7734 0.093 Uiso 1 1 calc R . . C12 C 0.2025(4) 0.0441(5) 0.8550(3) 0.0664(14) Uani 1 1 d . . . H12 H 0.2469 0.0895 0.8373 0.08 Uiso 1 1 calc R . . C13 C 0.3480(3) 0.1549(4) 1.0181(2) 0.0379(9) Uani 1 1 d . . . C14 C 0.3642(3) 0.0229(4) 1.0262(2) 0.0496(10) Uani 1 1 d . . . H14 H 0.3197 -0.0359 1.0038 0.06 Uiso 1 1 calc R . . C15 C 0.4467(4) -0.0226(5) 1.0679(3) 0.0670(14) Uani 1 1 d . . . H15 H 0.457 -0.1116 1.0737 0.08 Uiso 1 1 calc R . . C16 C 0.5132(3) 0.0641(6) 1.1007(2) 0.0668(14) Uani 1 1 d . . . H16 H 0.5689 0.0333 1.1272 0.08 Uiso 1 1 calc R . . C17 C 0.4978(3) 0.1948(6) 1.0944(2) 0.0584(12) Uani 1 1 d . . . H17 H 0.5424 0.2528 1.1175 0.07 Uiso 1 1 calc R . . C18 C 0.4160(3) 0.2405(5) 1.05376(19) 0.0471(10) Uani 1 1 d . . . H18 H 0.4057 0.3297 1.0499 0.057 Uiso 1 1 calc R . . C19 C 0.2063(3) 0.6427(3) 0.6933(2) 0.0370(9) Uani 1 1 d . . . C20 C 0.1158(3) 0.6574(4) 0.6531(2) 0.0492(11) Uani 1 1 d . . . H20 H 0.0678 0.6237 0.6717 0.059 Uiso 1 1 calc R . . C21 C 0.0963(3) 0.7189(5) 0.5880(2) 0.0609(13) Uani 1 1 d . . . H21 H 0.0358 0.7261 0.5625 0.073 Uiso 1 1 calc R . . C22 C 0.1665(3) 0.7709(4) 0.5599(2) 0.0514(11) Uani 1 1 d . . . H22 H 0.1534 0.8125 0.5152 0.062 Uiso 1 1 calc R . . C23 C 0.2556(3) 0.7615(4) 0.5978(2) 0.0414(9) Uani 1 1 d . . . C24 C 0.2768(3) 0.7014(4) 0.6658(2) 0.0390(9) Uani 1 1 d . . . C25 C 0.2127(3) 0.5655(4) 0.7589(2) 0.0382(9) Uani 1 1 d . . . H25 H 0.1567 0.5565 0.7723 0.046 Uiso 1 1 calc R . . C26 C 0.4297(3) 0.4519(4) 0.8332(2) 0.0403(9) Uani 1 1 d . . . C27 C 0.5477(3) 0.5534(5) 0.7784(2) 0.0576(12) Uani 1 1 d . . . H27A H 0.5277 0.6407 0.7869 0.069 Uiso 1 1 calc R . . H27B H 0.5197 0.5296 0.729 0.069 Uiso 1 1 calc R . . C28 C 0.6490(3) 0.5518(6) 0.7881(3) 0.0766(16) Uani 1 1 d . . . H28A H 0.6767 0.575 0.8371 0.115 Uiso 1 1 calc R . . H28B H 0.667 0.6131 0.7555 0.115 Uiso 1 1 calc R . . H28C H 0.6686 0.4662 0.778 0.115 Uiso 1 1 calc R . . C29 C 0.3163(4) 0.8599(5) 0.5037(3) 0.0717(15) Uani 1 1 d . . . H29A H 0.2865 0.7951 0.4702 0.108 Uiso 1 1 calc R . . H29B H 0.3744 0.8818 0.4928 0.108 Uiso 1 1 calc R . . H29C H 0.2786 0.9363 0.4995 0.108 Uiso 1 1 calc R . . N1 N 0.2787(2) 0.5069(3) 0.80248(16) 0.0342(7) Uani 1 1 d . . . N2 N 0.3672(2) 0.5223(3) 0.79124(16) 0.0396(7) Uani 1 1 d . . . N3 N 0.5174(2) 0.4632(4) 0.82823(18) 0.0507(9) Uani 1 1 d . . . H3A H 0.5578 0.4152 0.8556 0.061 Uiso 1 1 calc R . . O1 O 0.3648(2) 0.7069(3) 0.70048(18) 0.0658(10) Uani 1 1 d . . . H1 H 0.3747 0.6514 0.7324 0.099 Uiso 1 1 calc R . . O2 O 0.3303(2) 0.8109(3) 0.57489(16) 0.0562(8) Uani 1 1 d . . . P1 P 0.24193(7) 0.22092(9) 0.96574(5) 0.0335(2) Uani 1 1 d . . . S1 S 0.40906(7) 0.34408(11) 0.89917(6) 0.0458(3) Uani 1 1 d . . . Cl1 Cl 0.09635(7) 0.38534(12) 0.84856(6) 0.0557(3) Uani 1 1 d . . . Pd1 Pd 0.256488(18) 0.37197(3) 0.881403(14) 0.03193(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 0.034(2) 0.0311(19) 0.042(2) -0.0035(16) 0.0144(16) -0.0051(16) C2 0.052(3) 0.045(2) 0.051(2) 0.002(2) 0.0194(19) 0.009(2) C3 0.058(3) 0.053(3) 0.071(3) -0.007(2) 0.029(2) 0.010(2) C4 0.051(3) 0.055(3) 0.058(3) -0.013(2) 0.031(2) -0.013(2) C5 0.057(3) 0.057(3) 0.044(2) 0.009(2) 0.018(2) -0.004(2) C6 0.048(3) 0.049(3) 0.048(2) 0.007(2) 0.0193(19) 0.002(2) C7 0.040(2) 0.033(2) 0.044(2) 0.0016(17) 0.0064(17) 0.0006(17) C8 0.046(3) 0.053(3) 0.053(2) -0.010(2) 0.0194(19) -0.013(2) C9 0.055(3) 0.069(3) 0.067(3) -0.014(3) 0.020(2) -0.023(2) C10 0.072(4) 0.055(3) 0.072(3) -0.020(3) 0.011(3) -0.019(3) C11 0.107(5) 0.070(4) 0.065(3) -0.032(3) 0.041(3) -0.027(3) C12 0.089(4) 0.059(3) 0.064(3) -0.021(2) 0.043(3) -0.026(3) C13 0.034(2) 0.044(2) 0.038(2) 0.0067(17) 0.0136(16) 0.0035(17) C14 0.048(3) 0.045(2) 0.060(3) 0.014(2) 0.019(2) 0.011(2) C15 0.075(4) 0.062(3) 0.069(3) 0.020(3) 0.027(3) 0.030(3) C16 0.050(3) 0.101(4) 0.050(3) 0.022(3) 0.011(2) 0.022(3) C17 0.046(3) 0.087(4) 0.040(2) -0.002(2) 0.0067(19) -0.001(3) C18 0.045(3) 0.058(3) 0.039(2) 0.003(2) 0.0107(18) 0.004(2) C19 0.036(2) 0.034(2) 0.042(2) 0.0036(16) 0.0100(16) 0.0019(16) C20 0.035(2) 0.052(3) 0.061(3) 0.014(2) 0.0125(19) 0.0037(19) C21 0.036(3) 0.075(3) 0.068(3) 0.025(3) 0.001(2) 0.003(2) C22 0.049(3) 0.054(3) 0.049(2) 0.016(2) 0.0035(19) -0.002(2) C23 0.040(2) 0.036(2) 0.050(2) 0.0084(18) 0.0142(18) 0.0002(17) C24 0.029(2) 0.039(2) 0.047(2) 0.0094(18) 0.0052(16) -0.0014(17) C25 0.037(2) 0.037(2) 0.045(2) 0.0022(17) 0.0165(17) -0.0013(17) C26 0.037(2) 0.045(2) 0.042(2) -0.0024(18) 0.0147(17) -0.0018(18) C27 0.045(3) 0.085(4) 0.047(2) 0.009(2) 0.019(2) -0.007(2) C28 0.055(3) 0.106(4) 0.074(3) 0.009(3) 0.025(3) -0.018(3) C29 0.067(3) 0.085(4) 0.069(3) 0.036(3) 0.028(3) 0.005(3) N1 0.0272(17) 0.0361(17) 0.0415(16) 0.0047(14) 0.0123(13) -0.0007(13) N2 0.0305(18) 0.0475(19) 0.0431(17) 0.0081(15) 0.0133(14) -0.0019(15) N3 0.0281(18) 0.068(2) 0.059(2) 0.0156(19) 0.0164(15) 0.0026(17) O1 0.0377(18) 0.077(2) 0.077(2) 0.0414(18) 0.0010(15) -0.0143(16) O2 0.0468(18) 0.065(2) 0.0594(18) 0.0263(16) 0.0161(14) -0.0049(15) P1 0.0334(5) 0.0302(5) 0.0390(5) 0.0010(4) 0.0126(4) 0.0000(4) S1 0.0312(5) 0.0500(6) 0.0593(6) 0.0194(5) 0.0167(4) 0.0088(4) Cl1 0.0278(5) 0.0828(8) 0.0574(6) 0.0216(6) 0.0115(4) 0.0008(5) Pd1 0.02884(17) 0.03192(16) 0.03691(17) 0.00248(12) 0.01123(11) 0.00011(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 C2 1.380(5) . ? C1 C6 1.388(5) . ? C1 P1 1.832(4) . ? C2 C3 1.376(6) . ? C2 H2 0.93 . ? C3 C4 1.376(6) . ? C3 H3 0.93 . ? C4 C5 1.366(6) . ? C4 H4 0.93 . ? C5 C6 1.383(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.377(6) . ? C7 C8 1.381(5) . ? C7 P1 1.813(4) . ? C8 C9 1.383(6) . ? C8 H8 0.93 . ? C9 C10 1.360(7) . ? C9 H9 0.93 . ? C10 C11 1.359(7) . ? C10 H10 0.93 . ? C11 C12 1.385(7) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.381(6) . ? C13 C18 1.402(6) . ? C13 P1 1.809(4) . ? C14 C15 1.393(6) . ? C14 H14 0.93 . ? C15 C16 1.377(7) . ? C15 H15 0.93 . ? C16 C17 1.364(8) . ? C16 H16 0.93 . ? C17 C18 1.378(6) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C24 1.406(5) . ? C19 C20 1.409(5) . ? C19 C25 1.458(5) . ? C20 C21 1.357(6) . ? C20 H20 0.93 . ? C21 C22 1.381(6) . ? C21 H21 0.93 . ? C22 C23 1.371(6) . ? C22 H22 0.93 . ? C23 O2 1.378(5) . ? C23 C24 1.399(5) . ? C24 O1 1.336(5) . ? C25 N1 1.289(5) . ? C25 H25 0.93 . ? C26 N2 1.306(5) . ? C26 N3 1.338(5) . ? C26 S1 1.745(4) . ? C27 N3 1.461(5) . ? C27 C28 1.483(6) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 O2 1.410(5) . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? N1 N2 1.391(4) . ? N1 Pd1 2.115(3) . ? N3 H3A 0.86 . ? O1 H1 0.82 . ? P1 Pd1 2.2692(10) . ? S1 Pd1 2.2479(10) . ? Cl1 Pd1 2.3409(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 C2 C1 C6 118.3(4) . . ? C2 C1 P1 122.2(3) . . ? C6 C1 P1 119.5(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 118.4(4) . . ? C12 C7 P1 117.7(3) . . ? C8 C7 P1 123.9(3) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 120 . . ? C9 C8 H8 120 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 121.0(4) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C18 118.2(4) . . ? C14 C13 P1 122.8(3) . . ? C18 C13 P1 119.0(3) . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.0(5) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 121.1(4) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C24 C19 C20 117.5(3) . . ? C24 C19 C25 129.1(4) . . ? C20 C19 C25 113.4(3) . . ? C21 C20 C19 122.2(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 119.7(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 O2 124.7(4) . . ? C22 C23 C24 120.9(4) . . ? O2 C23 C24 114.4(3) . . ? O1 C24 C23 115.8(3) . . ? O1 C24 C19 124.8(3) . . ? C23 C24 C19 119.3(3) . . ? N1 C25 C19 134.3(3) . . ? N1 C25 H25 112.8 . . ? C19 C25 H25 112.8 . . ? N2 C26 N3 119.4(4) . . ? N2 C26 S1 125.0(3) . . ? N3 C26 S1 115.6(3) . . ? N3 C27 C28 111.2(4) . . ? N3 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N3 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 H29A 109.5 . . ? O2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 N1 N2 118.0(3) . . ? C25 N1 Pd1 122.9(2) . . ? N2 N1 Pd1 118.7(2) . . ? C26 N2 N1 115.0(3) . . ? C26 N3 C27 123.0(4) . . ? C26 N3 H3A 118.5 . . ? C27 N3 H3A 118.5 . . ? C24 O1 H1 109.5 . . ? C23 O2 C29 118.0(3) . . ? C13 P1 C7 105.05(18) . . ? C13 P1 C1 101.55(17) . . ? C7 P1 C1 107.76(17) . . ? C13 P1 Pd1 115.88(13) . . ? C7 P1 Pd1 108.07(13) . . ? C1 P1 Pd1 117.60(12) . . ? C26 S1 Pd1 98.13(14) . . ? N1 Pd1 S1 83.16(8) . . ? N1 Pd1 P1 176.10(8) . . ? S1 Pd1 P1 93.16(4) . . ? N1 Pd1 Cl1 94.65(8) . . ? S1 Pd1 Cl1 172.35(4) . . ? P1 Pd1 Cl1 88.83(4) . . ? # END of CIF # Attachment '[Pd(H-Msal-mtsc)Cl(PPh3)].cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-01-14 at 10:35:35 # Using CIFtbx version 2.6.2 16 Jun 1998 data_pp18 _database_code_depnum_ccdc_archive 'CCDC 815367' #TrackingRef '[Pd(H-Msal-mtsc)Cl(PPh3)].cif' _audit_creation_date 2011-01-14T10:35:35-00:00 _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 'C28 H27 Cl1 N3 O2 P1 Pd1 S1' _chemical_formula_sum 'C28 H27 Cl N3 O2 P Pd S' _chemical_formula_weight 642.41 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.8170(2) _cell_length_b 14.5065(3) _cell_length_c 21.6341(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3080.92(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23445 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.39 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.906 #----------------------------------------------------------------------------# # 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 0.0639 _diffrn_reflns_av_unetI/netI 0.1072 _diffrn_reflns_number 23445 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.39 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 6623 _reflns_number_gt 4527 _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^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6623 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.099 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 -0.05(4) _refine_diff_density_max 0.911 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 0.4259(6) 0.5784(4) 0.1839(3) 0.0522(16) Uani 1 1 d . . . C2 C 0.5331(7) 0.5160(4) 0.1917(3) 0.0597(17) Uani 1 1 d . . . H2 H 0.595 0.5242 0.2238 0.072 Uiso 1 1 calc R . . C3 C 0.5469(9) 0.4433(5) 0.1524(4) 0.081(2) Uani 1 1 d . . . H3 H 0.6182 0.402 0.1582 0.097 Uiso 1 1 calc R . . C4 C 0.4587(9) 0.4299(5) 0.1048(4) 0.080(2) Uani 1 1 d . . . H4 H 0.4703 0.3796 0.0786 0.096 Uiso 1 1 calc R . . C5 C 0.3541(9) 0.4892(6) 0.0952(4) 0.086(3) Uani 1 1 d . . . H5 H 0.2938 0.4792 0.0627 0.103 Uiso 1 1 calc R . . C6 C 0.3363(8) 0.5667(5) 0.1348(3) 0.0674(19) Uani 1 1 d . . . H6 H 0.2662 0.6086 0.1279 0.081 Uiso 1 1 calc R . . C7 C 0.3020(6) 0.7582(4) 0.2054(3) 0.0499(15) Uani 1 1 d . . . C8 C 0.3608(7) 0.8442(4) 0.1899(3) 0.0637(18) Uani 1 1 d . . . H8 H 0.4514 0.8557 0.1999 0.076 Uiso 1 1 calc R . . C9 C 0.2852(9) 0.9114(5) 0.1601(4) 0.086(2) Uani 1 1 d . . . H9 H 0.3254 0.9675 0.1502 0.103 Uiso 1 1 calc R . . C10 C 0.1485(9) 0.8954(7) 0.1447(4) 0.091(3) Uani 1 1 d . . . H10 H 0.0976 0.9408 0.125 0.109 Uiso 1 1 calc R . . C11 C 0.0888(8) 0.8088(6) 0.1596(3) 0.087(2) Uani 1 1 d . . . H11 H -0.0013 0.7971 0.1489 0.104 Uiso 1 1 calc R . . C12 C 0.1636(7) 0.7421(5) 0.1899(3) 0.072(2) Uani 1 1 d . . . H12 H 0.1231 0.6862 0.2002 0.086 Uiso 1 1 calc R . . C13 C 0.2901(6) 0.6201(4) 0.2988(3) 0.0466(14) Uani 1 1 d . . . C14 C 0.3070(7) 0.5294(4) 0.3177(3) 0.0528(15) Uani 1 1 d . . . H14 H 0.3682 0.4917 0.2968 0.063 Uiso 1 1 calc R . . C15 C 0.2346(8) 0.4943(5) 0.3669(3) 0.069(2) Uani 1 1 d . . . H15 H 0.2485 0.4339 0.3797 0.083 Uiso 1 1 calc R . . C16 C 0.1414(7) 0.5493(7) 0.3971(3) 0.081(2) Uani 1 1 d . . . H16 H 0.092 0.5255 0.4301 0.098 Uiso 1 1 calc R . . C17 C 0.1209(8) 0.6392(6) 0.3787(4) 0.075(2) Uani 1 1 d . . . H17 H 0.0579 0.6764 0.3988 0.09 Uiso 1 1 calc R . . C18 C 0.1953(6) 0.6722(4) 0.3304(3) 0.0633(18) Uani 1 1 d . . . H18 H 0.1814 0.7328 0.318 0.076 Uiso 1 1 calc R . . C19 C 0.8474(5) 0.8391(4) 0.3008(3) 0.0457(14) Uani 1 1 d . . . H19 H 0.836 0.8423 0.2582 0.055 Uiso 1 1 calc R . . C20 C 0.9475(5) 0.9045(4) 0.3234(3) 0.0416(13) Uani 1 1 d . . . C21 C 0.9846(6) 0.9707(4) 0.2799(3) 0.0549(15) Uani 1 1 d . . . H21 H 0.9477 0.9667 0.2404 0.066 Uiso 1 1 calc R . . C22 C 1.0722(6) 1.0409(4) 0.2925(4) 0.069(2) Uani 1 1 d . . . H22 H 1.0955 1.0827 0.2617 0.082 Uiso 1 1 calc R . . C23 C 1.1264(7) 1.0498(4) 0.3512(4) 0.0659(19) Uani 1 1 d . . . H23 H 1.1838 1.0989 0.3604 0.079 Uiso 1 1 calc R . . C24 C 1.0956(7) 0.9866(4) 0.3952(3) 0.0572(16) Uani 1 1 d . . . C25 C 1.0054(6) 0.9121(4) 0.3816(3) 0.0520(15) Uani 1 1 d . . . C26 C 0.6881(5) 0.7129(4) 0.4143(3) 0.0441(13) Uani 1 1 d . . . C27 C 0.8034(7) 0.7228(6) 0.5133(3) 0.0768(19) Uani 1 1 d . . . H27A H 0.8118 0.7887 0.5116 0.115 Uiso 1 1 calc R . . H27B H 0.8861 0.695 0.4988 0.115 Uiso 1 1 calc R . . H27C H 0.7868 0.704 0.5552 0.115 Uiso 1 1 calc R . . C28 C 1.2324(12) 1.0583(7) 0.4701(5) 0.143(5) Uani 1 1 d . . . H28A H 1.1894 1.1162 0.4611 0.215 Uiso 1 1 calc R . . H28B H 1.3155 1.0534 0.4469 0.215 Uiso 1 1 calc R . . H28C H 1.2522 1.0548 0.5134 0.215 Uiso 1 1 calc R . . N1 N 0.7698(4) 0.7768(3) 0.3262(2) 0.0423(10) Uani 1 1 d . . . N2 N 0.7844(4) 0.7606(3) 0.38950(19) 0.0439(11) Uani 1 1 d . . . N3 N 0.6921(5) 0.6940(3) 0.4751(2) 0.0587(14) Uani 1 1 d . . . H3A H 0.626 0.6638 0.4915 0.07 Uiso 1 1 calc R . . O1 O 0.9848(5) 0.8518(3) 0.4286(2) 0.0811(16) Uani 1 1 d . . . H1 H 0.918 0.8198 0.421 0.122 Uiso 1 1 calc R . . O2 O 1.1458(6) 0.9868(3) 0.4538(2) 0.0921(19) Uani 1 1 d . . . P1 P 0.40170(16) 0.66899(9) 0.24066(6) 0.0424(3) Uani 1 1 d . . . S1 S 0.54437(16) 0.67004(11) 0.37531(7) 0.0519(4) Uani 1 1 d . . . Pd1 Pd 0.60127(4) 0.71931(3) 0.280150(19) 0.03908(12) Uani 1 1 d . . . Cl1 Cl 0.67715(16) 0.75532(10) 0.18061(7) 0.0537(4) 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 0.053(4) 0.049(3) 0.055(4) -0.013(3) 0.011(3) -0.012(3) C2 0.058(4) 0.052(3) 0.070(4) -0.010(3) 0.010(4) 0.003(3) C3 0.076(5) 0.054(4) 0.111(7) -0.013(4) 0.024(5) 0.009(4) C4 0.077(5) 0.059(4) 0.103(7) -0.036(4) 0.034(5) -0.016(4) C5 0.073(6) 0.107(6) 0.078(5) -0.049(5) 0.007(4) -0.025(5) C6 0.067(4) 0.070(4) 0.065(5) -0.024(4) -0.008(4) 0.000(4) C7 0.039(3) 0.052(3) 0.059(4) -0.007(3) -0.004(3) 0.007(3) C8 0.058(4) 0.054(3) 0.079(5) 0.003(3) -0.006(3) 0.011(3) C9 0.098(7) 0.068(4) 0.092(6) 0.014(4) 0.009(5) 0.018(5) C10 0.071(6) 0.118(7) 0.083(6) 0.030(5) 0.000(4) 0.043(5) C11 0.059(5) 0.126(7) 0.075(5) 0.006(5) -0.005(4) 0.034(5) C12 0.049(4) 0.088(5) 0.079(5) -0.005(4) -0.009(3) 0.010(4) C13 0.041(3) 0.050(3) 0.048(4) -0.015(3) -0.002(3) -0.007(3) C14 0.057(4) 0.052(3) 0.049(4) -0.002(3) 0.003(3) -0.003(3) C15 0.073(5) 0.067(4) 0.066(5) 0.000(4) -0.005(4) -0.019(4) C16 0.061(5) 0.131(7) 0.052(5) -0.021(5) 0.018(4) -0.032(5) C17 0.064(5) 0.087(5) 0.074(5) -0.006(4) 0.019(4) -0.005(4) C18 0.056(4) 0.055(3) 0.078(5) -0.011(4) 0.009(4) 0.003(3) C19 0.036(3) 0.058(3) 0.043(3) 0.002(3) 0.000(2) -0.001(3) C20 0.034(3) 0.051(3) 0.040(3) 0.005(3) -0.003(3) 0.004(3) C21 0.038(3) 0.073(4) 0.053(4) 0.014(4) 0.002(3) -0.010(3) C22 0.057(4) 0.062(4) 0.087(5) 0.019(4) -0.002(4) -0.013(3) C23 0.056(4) 0.055(3) 0.087(5) -0.001(4) -0.014(4) -0.017(3) C24 0.043(4) 0.055(3) 0.074(4) 0.005(3) -0.015(4) -0.005(3) C25 0.045(3) 0.052(3) 0.060(4) 0.002(3) -0.007(3) -0.003(3) C26 0.042(3) 0.044(3) 0.046(3) 0.008(3) 0.003(3) 0.001(3) C27 0.068(4) 0.112(5) 0.051(4) 0.011(4) -0.015(3) -0.016(5) C28 0.171(11) 0.143(8) 0.116(9) -0.017(7) -0.052(8) -0.072(9) N1 0.037(2) 0.044(2) 0.046(3) 0.003(2) -0.004(2) 0.003(2) N2 0.039(2) 0.061(3) 0.032(2) 0.005(2) -0.0028(19) 0.003(2) N3 0.055(3) 0.081(4) 0.040(3) 0.016(2) -0.004(2) -0.011(3) O1 0.091(4) 0.082(3) 0.070(3) 0.038(3) -0.042(3) -0.037(3) O2 0.108(5) 0.091(3) 0.077(4) 0.012(3) -0.043(3) -0.051(3) P1 0.0398(7) 0.0408(7) 0.0467(8) -0.0071(6) -0.0019(7) -0.0003(8) S1 0.0486(9) 0.0622(9) 0.0449(9) 0.0052(7) -0.0014(7) -0.0155(8) Pd1 0.0363(2) 0.03994(19) 0.0410(2) -0.0010(2) -0.0005(2) -0.0005(2) Cl1 0.0565(9) 0.0587(9) 0.0460(8) -0.0004(7) 0.0065(7) -0.0023(7) #----------------------------------------------------------------------------# # 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 C6 1.389(9) . ? C1 C2 1.398(9) . ? C1 P1 1.814(6) . ? C2 C3 1.362(9) . ? C2 H2 0.93 . ? C3 C4 1.359(11) . ? C3 H3 0.93 . ? C4 C5 1.356(11) . ? C4 H4 0.93 . ? C5 C6 1.424(10) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.414(8) . ? C7 C12 1.419(8) . ? C7 P1 1.793(6) . ? C8 C9 1.385(9) . ? C8 H8 0.93 . ? C9 C10 1.402(11) . ? C9 H9 0.93 . ? C10 C11 1.423(11) . ? C10 H10 0.93 . ? C11 C12 1.381(9) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.380(8) . ? C13 C14 1.388(8) . ? C13 P1 1.812(6) . ? C14 C15 1.378(9) . ? C14 H14 0.93 . ? C15 C16 1.378(10) . ? C15 H15 0.93 . ? C16 C17 1.378(11) . ? C16 H16 0.93 . ? C17 C18 1.362(9) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 N1 1.303(7) . ? C19 C20 1.452(7) . ? C19 H19 0.93 . ? C20 C25 1.385(8) . ? C20 C21 1.394(8) . ? C21 C22 1.360(8) . ? C21 H21 0.93 . ? C22 C23 1.384(10) . ? C22 H22 0.93 . ? C23 C24 1.357(9) . ? C23 H23 0.93 . ? C24 O2 1.359(8) . ? C24 C25 1.428(8) . ? C25 O1 1.357(7) . ? C26 N2 1.289(7) . ? C26 N3 1.344(7) . ? C26 S1 1.757(6) . ? C27 N3 1.432(8) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 O2 1.387(9) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? N1 N2 1.397(6) . ? N1 Pd1 2.104(4) . ? N3 H3A 0.86 . ? O1 H1 0.82 . ? P1 Pd1 2.2585(15) . ? S1 Pd1 2.2497(16) . ? Pd1 Cl1 2.3378(16) . ? 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 C6 C1 C2 119.3(6) . . ? C6 C1 P1 121.6(5) . . ? C2 C1 P1 119.0(5) . . ? C3 C2 C1 120.0(7) . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 121.4(7) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.1(8) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C1 C6 C5 118.7(7) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 C12 118.8(6) . . ? C8 C7 P1 120.9(4) . . ? C12 C7 P1 120.2(5) . . ? C9 C8 C7 120.8(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.5(8) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.1(7) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120.5(8) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.4(7) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C18 C13 C14 117.0(6) . . ? C18 C13 P1 122.5(4) . . ? C14 C13 P1 120.2(5) . . ? C15 C14 C13 121.0(6) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.5(7) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 118.4(7) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C13 123.3(6) . . ? C17 C18 H18 118.3 . . ? C13 C18 H18 118.3 . . ? N1 C19 C20 135.0(5) . . ? N1 C19 H19 112.5 . . ? C20 C19 H19 112.5 . . ? C25 C20 C21 116.9(5) . . ? C25 C20 C19 129.5(5) . . ? C21 C20 C19 113.5(5) . . ? C22 C21 C20 123.0(6) . . ? C22 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.7(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 O2 124.9(6) . . ? C23 C24 C25 120.3(6) . . ? O2 C24 C25 114.8(6) . . ? O1 C25 C20 124.7(5) . . ? O1 C25 C24 115.1(5) . . ? C20 C25 C24 120.1(6) . . ? N2 C26 N3 119.7(5) . . ? N2 C26 S1 125.4(4) . . ? N3 C26 S1 114.9(4) . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 N1 N2 118.0(5) . . ? C19 N1 Pd1 122.3(4) . . ? N2 N1 Pd1 118.6(3) . . ? C26 N2 N1 115.0(4) . . ? C26 N3 C27 121.9(5) . . ? C26 N3 H3A 119.1 . . ? C27 N3 H3A 119.1 . . ? C25 O1 H1 109.5 . . ? C24 O2 C28 117.5(6) . . ? C7 P1 C13 104.4(3) . . ? C7 P1 C1 107.8(3) . . ? C13 P1 C1 105.4(2) . . ? C7 P1 Pd1 113.64(19) . . ? C13 P1 Pd1 112.87(19) . . ? C1 P1 Pd1 112.1(2) . . ? C26 S1 Pd1 97.32(19) . . ? N1 Pd1 S1 83.56(13) . . ? N1 Pd1 P1 171.68(12) . . ? S1 Pd1 P1 91.61(5) . . ? N1 Pd1 Cl1 95.58(12) . . ? S1 Pd1 Cl1 173.25(6) . . ? P1 Pd1 Cl1 90.01(5) . . ? C26 N2 N1 115.0(4) . . ? C26 N3 C27 121.9(5) . . ? C26 N3 H3A 119.1 . . ? C27 N3 H3A 119.1 . . ? C25 O1 H1 109.5 . . ? C24 O2 C28 117.5(6) . . ? C7 P1 C13 104.4(3) . . ? C7 P1 C1 107.8(3) . . ? C13 P1 C1 105.4(2) . . ? C7 P1 Pd1 113.64(19) . . ? C13 P1 Pd1 112.87(19) . . ? C1 P1 Pd1 112.1(2) . . ? C26 S1 Pd1 97.32(19) . . ? N1 Pd1 S1 83.56(13) . . ? N1 Pd1 P1 171.68(12) . . ? S1 Pd1 P1 91.61(5) . . ? N1 Pd1 Cl1 95.58(12) . . ? S1 Pd1 Cl1 173.25(6) . . ? # Attachment '[Pd(Msal-ptsc)(PPh3)].cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-06-29 at 15:50:27 # Using CIFtbx version 2.6.2 16 Jun 1998 data_ppl16 _database_code_depnum_ccdc_archive 'CCDC 815368' #TrackingRef '[Pd(Msal-ptsc)(PPh3)].cif' _audit_creation_date 2010-06-29T15:50:27-00:00 _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 'C33 H28 N3 O2 P1 Pd1 S1' _chemical_formula_sum 'C33 H28 N3 O2 P Pd S' _chemical_formula_weight 668.01 _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 11.9088(3) _cell_length_b 8.0278(2) _cell_length_c 15.6843(5) _cell_angle_alpha 90 _cell_angle_beta 102.480(1) _cell_angle_gamma 90 _cell_volume 1464.01(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13783 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.64 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 0.927 #----------------------------------------------------------------------------# # 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 0.0665 _diffrn_reflns_av_unetI/netI 0.1504 _diffrn_reflns_number 13783 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.64 _diffrn_reflns_theta_full 28.64 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _reflns_number_total 6913 _reflns_number_gt 4927 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6913 _refine_ls_number_parameters 371 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.088 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _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 -0.01(2) _refine_diff_density_max 0.455 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.085 #----------------------------------------------------------------------------# # 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' Pd Pd -0.9988 1.0072 '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 0.3380(4) 0.4044(5) 0.3217(3) 0.0288(10) Uani 1 1 d . . . C2 C 0.3997(5) 0.4674(6) 0.4009(3) 0.0504(14) Uani 1 1 d . . . H2 H 0.4348 0.5711 0.4017 0.06 Uiso 1 1 calc R . . C3 C 0.4103(5) 0.3805(8) 0.4779(4) 0.0663(17) Uani 1 1 d . . . H3 H 0.4489 0.4264 0.5305 0.08 Uiso 1 1 calc R . . C4 C 0.3622(5) 0.2237(7) 0.4752(4) 0.0626(17) Uani 1 1 d . . . H4 H 0.3693 0.1629 0.5265 0.075 Uiso 1 1 calc R . . C5 C 0.3043(5) 0.1565(8) 0.3982(4) 0.0657(18) Uani 1 1 d . . . H5 H 0.2736 0.0498 0.3969 0.079 Uiso 1 1 calc R . . C6 C 0.2919(5) 0.2494(6) 0.3216(3) 0.0489(14) Uani 1 1 d . . . H6 H 0.2512 0.2044 0.2694 0.059 Uiso 1 1 calc R . . C7 C 0.2479(4) 0.4135(5) 0.1336(3) 0.0264(10) Uani 1 1 d . . . C8 C 0.1357(4) 0.4533(6) 0.0916(3) 0.0349(11) Uani 1 1 d . . . H8 H 0.0974 0.5402 0.1124 0.042 Uiso 1 1 calc R . . C9 C 0.0816(4) 0.3643(6) 0.0196(3) 0.0436(13) Uani 1 1 d . . . H9 H 0.0067 0.3913 -0.0083 0.052 Uiso 1 1 calc R . . C10 C 0.1370(4) 0.2360(6) -0.0115(3) 0.0447(13) Uani 1 1 d . . . H10 H 0.1004 0.1787 -0.0613 0.054 Uiso 1 1 calc R . . C11 C 0.2462(4) 0.1916(5) 0.0302(3) 0.0415(12) Uani 1 1 d . . . H11 H 0.2824 0.1017 0.0101 0.05 Uiso 1 1 calc R . . C12 C 0.3022(4) 0.2801(5) 0.1021(3) 0.0355(11) Uani 1 1 d . . . H12 H 0.3767 0.2507 0.1299 0.043 Uiso 1 1 calc R . . C13 C 0.2196(4) 0.6915(5) 0.2397(3) 0.0286(10) Uani 1 1 d . . . C14 C 0.2023(4) 0.8289(5) 0.1840(3) 0.0329(11) Uani 1 1 d . . . H14 H 0.2486 0.8437 0.1438 0.039 Uiso 1 1 calc R . . C15 C 0.1169(4) 0.9435(5) 0.1881(3) 0.0405(12) Uani 1 1 d . . . H15 H 0.1053 1.0339 0.1501 0.049 Uiso 1 1 calc R . . C16 C 0.0488(5) 0.9243(6) 0.2483(4) 0.0532(15) Uani 1 1 d . . . H16 H -0.0088 1.0013 0.2507 0.064 Uiso 1 1 calc R . . C17 C 0.0662(5) 0.7916(7) 0.3045(4) 0.0538(15) Uani 1 1 d . . . H17 H 0.0209 0.7793 0.3456 0.065 Uiso 1 1 calc R . . C18 C 0.1513(4) 0.6755(5) 0.3004(3) 0.0417(14) Uani 1 1 d . . . H18 H 0.1626 0.5858 0.3389 0.05 Uiso 1 1 calc R . . C19 C 0.6422(4) 0.3623(5) 0.1603(3) 0.0288(10) Uani 1 1 d . . . C20 C 0.6458(4) 0.2063(5) 0.1157(3) 0.0356(11) Uani 1 1 d . . . C21 C 0.7458(4) 0.1502(7) 0.0956(3) 0.0434(13) Uani 1 1 d . . . H21 H 0.7467 0.05 0.066 0.052 Uiso 1 1 calc R . . C22 C 0.8467(5) 0.2448(6) 0.1201(4) 0.0504(14) Uani 1 1 d . . . H22 H 0.915 0.2055 0.1078 0.061 Uiso 1 1 calc R . . C23 C 0.8457(4) 0.3933(6) 0.1615(3) 0.0413(12) Uani 1 1 d . . . H23 H 0.9136 0.4538 0.1773 0.05 Uiso 1 1 calc R . . C24 C 0.7444(4) 0.4574(5) 0.1809(3) 0.0310(10) Uani 1 1 d . . . C25 C 0.7517(3) 0.6155(8) 0.2213(3) 0.0341(9) Uani 1 1 d . . . H25 H 0.825 0.6616 0.236 0.041 Uiso 1 1 calc R . . C26 C 0.6207(4) 0.9449(5) 0.2955(3) 0.0344(11) Uani 1 1 d . . . C27 C 0.7403(4) 1.1865(5) 0.3651(3) 0.0325(11) Uani 1 1 d . . . C28 C 0.8484(4) 1.1193(10) 0.3720(3) 0.0534(12) Uani 1 1 d . . . H28 H 0.8568 1.0096 0.3553 0.064 Uiso 1 1 calc R . . C29 C 0.9450(5) 1.2165(7) 0.4040(4) 0.0653(17) Uani 1 1 d . . . H29 H 1.0178 1.1714 0.4077 0.078 Uiso 1 1 calc R . . C30 C 0.9348(5) 1.3774(7) 0.4303(4) 0.0595(16) Uani 1 1 d . . . H30 H 0.9999 1.4416 0.4516 0.071 Uiso 1 1 calc R . . C31 C 0.8276(5) 1.4417(7) 0.4246(4) 0.0638(17) Uani 1 1 d . . . H31 H 0.8195 1.5503 0.4431 0.077 Uiso 1 1 calc R . . C32 C 0.7314(5) 1.3486(6) 0.3921(4) 0.0526(15) Uani 1 1 d . . . H32 H 0.659 1.3955 0.3882 0.063 Uiso 1 1 calc R . . C33 C 0.5403(5) -0.0285(6) 0.0496(4) 0.0566(15) Uani 1 1 d . . . H33A H 0.5923 -0.1068 0.0836 0.085 Uiso 1 1 calc R . . H33B H 0.5627 -0.0085 -0.0048 0.085 Uiso 1 1 calc R . . H33C H 0.4637 -0.0728 0.0383 0.085 Uiso 1 1 calc R . . N1 N 0.6699(3) 0.7054(4) 0.2406(2) 0.0310(9) Uani 1 1 d . . . N2 N 0.7048(3) 0.8594(5) 0.2780(3) 0.0368(9) Uani 1 1 d . . . N3 N 0.6378(3) 1.1003(5) 0.3323(2) 0.0394(10) Uani 1 1 d . . . H3A H 0.5761 1.153 0.3358 0.047 Uiso 1 1 calc R . . O1 O 0.5426(3) 0.4036(4) 0.1772(2) 0.0384(8) Uani 1 1 d . . . O2 O 0.5436(2) 0.1246(6) 0.09667(19) 0.0459(7) Uani 1 1 d . . . P1 P 0.32481(10) 0.53571(13) 0.22620(8) 0.0253(3) Uani 1 1 d . . . S1 S 0.47581(10) 0.87835(14) 0.27704(8) 0.0351(3) Uani 1 1 d . . . Pd1 Pd 0.50571(3) 0.62645(3) 0.22434(2) 0.02563(8) 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 0.030(3) 0.030(3) 0.026(3) -0.0033(18) 0.005(2) 0.0055(19) C2 0.060(4) 0.055(3) 0.032(3) 0.003(2) 0.000(3) -0.016(3) C3 0.073(5) 0.088(4) 0.031(3) 0.009(3) -0.005(3) -0.019(4) C4 0.065(4) 0.075(4) 0.048(4) 0.032(3) 0.012(3) 0.005(3) C5 0.091(5) 0.051(5) 0.056(4) 0.018(3) 0.016(3) -0.008(3) C6 0.065(4) 0.041(3) 0.038(3) 0.001(2) 0.004(3) -0.014(3) C7 0.027(3) 0.030(2) 0.022(2) 0.0015(18) 0.006(2) -0.0052(18) C8 0.023(3) 0.043(3) 0.036(3) -0.006(2) 0.001(2) -0.001(2) C9 0.029(3) 0.060(3) 0.035(3) -0.006(3) -0.006(2) -0.009(2) C10 0.041(3) 0.055(3) 0.036(3) -0.012(2) 0.005(3) -0.020(3) C11 0.045(3) 0.041(3) 0.040(3) -0.019(2) 0.013(3) -0.009(2) C12 0.027(3) 0.042(3) 0.037(3) -0.005(2) 0.006(2) -0.004(2) C13 0.026(2) 0.029(2) 0.031(3) -0.0033(17) 0.006(2) -0.0003(17) C14 0.031(3) 0.031(3) 0.036(3) -0.0008(19) 0.005(2) -0.0007(19) C15 0.032(3) 0.029(3) 0.053(3) -0.002(2) -0.007(3) 0.007(2) C16 0.040(3) 0.050(3) 0.071(4) -0.008(3) 0.016(3) 0.020(2) C17 0.046(4) 0.067(4) 0.056(4) -0.004(3) 0.028(3) 0.012(3) C18 0.031(3) 0.047(4) 0.049(3) 0.005(2) 0.014(2) 0.007(2) C19 0.023(3) 0.037(3) 0.027(3) 0.0026(19) 0.007(2) 0.0093(19) C20 0.036(3) 0.039(2) 0.032(3) -0.001(2) 0.007(2) 0.008(2) C21 0.044(3) 0.036(3) 0.055(3) -0.006(3) 0.022(2) 0.016(3) C22 0.039(3) 0.052(3) 0.069(4) 0.005(3) 0.031(3) 0.014(2) C23 0.030(3) 0.037(3) 0.061(4) 0.003(2) 0.018(3) 0.003(2) C24 0.024(3) 0.035(3) 0.037(3) 0.004(2) 0.013(2) 0.0061(19) C25 0.026(2) 0.032(2) 0.045(3) 0.002(3) 0.0085(19) -0.004(3) C26 0.026(3) 0.037(3) 0.038(3) -0.003(2) 0.003(2) -0.005(2) C27 0.032(3) 0.033(3) 0.032(3) -0.0057(18) 0.006(2) -0.0036(19) C28 0.039(3) 0.040(3) 0.078(4) -0.014(4) 0.007(2) -0.003(4) C29 0.035(3) 0.068(4) 0.091(5) -0.022(3) 0.008(3) -0.006(3) C30 0.050(4) 0.063(4) 0.065(4) -0.019(3) 0.010(3) -0.024(3) C31 0.061(4) 0.049(3) 0.076(5) -0.023(3) 0.002(4) -0.006(3) C32 0.044(3) 0.039(3) 0.071(4) -0.024(3) 0.006(3) -0.003(2) C33 0.066(4) 0.047(3) 0.059(4) -0.023(3) 0.018(3) -0.003(3) N1 0.024(2) 0.0270(18) 0.041(2) -0.0022(17) 0.0045(18) -0.0032(16) N2 0.029(2) 0.035(2) 0.045(3) -0.0083(18) 0.006(2) -0.0040(18) N3 0.032(2) 0.029(3) 0.056(2) -0.012(2) 0.0058(18) 0.0005(18) O1 0.031(2) 0.0298(17) 0.057(2) -0.0106(15) 0.0142(18) -0.0001(14) O2 0.0409(18) 0.0400(16) 0.057(2) -0.019(3) 0.0107(15) 0.004(2) P1 0.0223(7) 0.0282(6) 0.0250(6) -0.0007(5) 0.0044(5) 0.0011(5) S1 0.0246(7) 0.0328(6) 0.0493(8) -0.0099(6) 0.0109(6) -0.0003(5) Pd1 0.02145(15) 0.02708(15) 0.02883(16) -0.0028(2) 0.00650(11) 0.0003(2) #----------------------------------------------------------------------------# # 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 C6 1.360(6) . ? C1 C2 1.394(6) . ? C1 P1 1.810(4) . ? C2 C3 1.377(7) . ? C2 H2 0.93 . ? C3 C4 1.380(8) . ? C3 H3 0.93 . ? C4 C5 1.365(8) . ? C4 H4 0.93 . ? C5 C6 1.394(7) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.395(6) . ? C7 C8 1.392(6) . ? C7 P1 1.827(4) . ? C8 C9 1.374(6) . ? C8 H8 0.93 . ? C9 C10 1.368(7) . ? C9 H9 0.93 . ? C10 C11 1.370(7) . ? C10 H10 0.93 . ? C11 C12 1.377(6) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.386(6) . ? C13 C14 1.394(6) . ? C13 P1 1.814(4) . ? C14 C15 1.383(6) . ? C14 H14 0.93 . ? C15 C16 1.380(7) . ? C15 H15 0.93 . ? C16 C17 1.370(7) . ? C16 H16 0.93 . ? C17 C18 1.389(6) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 O1 1.312(5) . ? C19 C24 1.414(6) . ? C19 C20 1.440(6) . ? C20 O2 1.357(6) . ? C20 C21 1.372(6) . ? C21 C22 1.403(7) . ? C21 H21 0.93 . ? C22 C23 1.358(6) . ? C22 H22 0.93 . ? C23 C24 1.405(6) . ? C23 H23 0.93 . ? C24 C25 1.413(7) . ? C25 N1 1.299(6) . ? C25 H25 0.93 . ? C26 N2 1.292(5) . ? C26 N3 1.372(5) . ? C26 S1 1.769(4) . ? C27 C32 1.380(6) . ? C27 C28 1.379(6) . ? C27 N3 1.400(5) . ? C28 C29 1.391(7) . ? C28 H28 0.93 . ? C29 C30 1.369(7) . ? C29 H29 0.93 . ? C30 C31 1.363(8) . ? C30 H30 0.93 . ? C31 C32 1.370(7) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 O2 1.430(6) . ? C33 H33A 0.96 . ? C33 H33B 0.96 . ? C33 H33C 0.96 . ? N1 N2 1.393(5) . ? N1 Pd1 2.019(3) . ? N3 H3A 0.86 . ? O1 Pd1 2.020(3) . ? P1 Pd1 2.2802(12) . ? S1 Pd1 2.2420(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 C6 C1 C2 117.9(4) . . ? C6 C1 P1 124.7(4) . . ? C2 C1 P1 117.4(3) . . ? C3 C2 C1 121.9(5) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 118.5(6) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.3(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C12 C7 C8 118.7(4) . . ? C12 C7 P1 120.2(3) . . ? C8 C7 P1 121.2(3) . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 120.5(5) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C11 C12 C7 120.4(4) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C18 C13 C14 118.3(4) . . ? C18 C13 P1 122.6(3) . . ? C14 C13 P1 119.0(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.2(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.8(4) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? O1 C19 C24 126.0(4) . . ? O1 C19 C20 116.2(4) . . ? C24 C19 C20 117.8(4) . . ? O2 C20 C21 124.9(4) . . ? O2 C20 C19 114.1(4) . . ? C21 C20 C19 121.0(5) . . ? C20 C21 C22 119.6(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 121.5(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 119.3(4) . . ? C23 C24 C25 117.0(4) . . ? C19 C24 C25 123.7(4) . . ? N1 C25 C24 128.8(4) . . ? N1 C25 H25 115.6 . . ? C24 C25 H25 115.6 . . ? N2 C26 N3 121.4(4) . . ? N2 C26 S1 125.4(3) . . ? N3 C26 S1 113.3(3) . . ? C32 C27 C28 118.5(5) . . ? C32 C27 N3 117.4(4) . . ? C28 C27 N3 124.1(4) . . ? C27 C28 C29 119.6(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 121.2(6) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 118.7(5) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C30 C31 C32 120.9(5) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 121.0(5) . . ? C27 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? O2 C33 H33A 109.5 . . ? O2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C25 N1 N2 114.9(4) . . ? C25 N1 Pd1 123.4(3) . . ? N2 N1 Pd1 121.6(3) . . ? C26 N2 N1 112.7(4) . . ? C26 N3 C27 130.0(4) . . ? C26 N3 H3A 115 . . ? C27 N3 H3A 115 . . ? C19 O1 Pd1 125.1(3) . . ? C20 O2 C33 116.9(4) . . ? C1 P1 C13 104.09(19) . . ? C1 P1 C7 106.52(19) . . ? C13 P1 C7 102.9(2) . . ? C1 P1 Pd1 106.46(15) . . ? C13 P1 Pd1 117.33(14) . . ? C7 P1 Pd1 118.30(15) . . ? C26 S1 Pd1 96.07(15) . . ? O1 Pd1 N1 92.45(13) . . ? O1 Pd1 S1 176.53(9) . . ? N1 Pd1 S1 84.09(10) . . ? O1 Pd1 P1 90.15(9) . . ? N1 Pd1 P1 172.19(11) . . ? S1 Pd1 P1 93.31(4) . . ? # END of CIF # Attachment '[Pd(Msal-tsc)(PPh3)].cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-06-23 at 08:49:41 # Using CIFtbx version 2.6.2 16 Jun 1998 data_ppl14 _database_code_depnum_ccdc_archive 'CCDC 815369' #TrackingRef '[Pd(Msal-tsc)(PPh3)].cif' _audit_creation_date 2010-06-23T08:49:41-00:00 _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 'C27 H24 N3 O2 P1 Pd1 S1' _chemical_formula_sum 'C27 H24 N3 O2 P Pd S' _chemical_formula_weight 591.92 _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 10.771(1) _cell_length_b 11.8338(5) _cell_length_c 12.1601(8) _cell_angle_alpha 69.422(2) _cell_angle_beta 85.741(3) _cell_angle_gamma 80.421(6) _cell_volume 1430.61(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16172 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 28.17 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.91 #----------------------------------------------------------------------------# # 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 0.097 _diffrn_reflns_av_unetI/netI 0.178 _diffrn_reflns_number 16172 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.17 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _reflns_number_total 6639 _reflns_number_gt 3276 _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 209 73 ' ' _platon_squeeze_details ; ; _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^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6639 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1692 _refine_ls_R_factor_gt 0.078 _refine_ls_wR_factor_ref 0.2071 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.668 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.122 #----------------------------------------------------------------------------# # 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' Pd Pd -0.9988 1.0072 '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 0.0669(7) 0.2573(7) 0.4703(7) 0.0552(19) Uani 1 1 d . . . C2 C -0.0015(9) 0.1627(8) 0.4949(9) 0.076(3) Uani 1 1 d . . . H2 H -0.0242 0.1409 0.4336 0.092 Uiso 1 1 calc R . . C3 C -0.0374(11) 0.0994(9) 0.6087(11) 0.098(3) Uani 1 1 d . . . H3 H -0.0869 0.0383 0.6223 0.117 Uiso 1 1 calc R . . C4 C -0.0005(11) 0.1260(9) 0.7029(10) 0.089(3) Uani 1 1 d . . . H4 H -0.024 0.0833 0.7796 0.107 Uiso 1 1 calc R . . C5 C 0.0706(9) 0.2159(10) 0.6794(9) 0.080(3) Uani 1 1 d . . . H5 H 0.0982 0.2341 0.7411 0.096 Uiso 1 1 calc R . . C6 C 0.1030(7) 0.2813(8) 0.5654(8) 0.065(2) Uani 1 1 d . . . H6 H 0.1507 0.3436 0.5522 0.078 Uiso 1 1 calc R . . C7 C -0.0495(6) 0.4509(7) 0.2763(7) 0.0456(17) Uani 1 1 d . . . C8 C -0.1472(7) 0.4550(8) 0.3531(8) 0.062(2) Uani 1 1 d . . . H8 H -0.1391 0.405 0.4315 0.075 Uiso 1 1 calc R . . C9 C -0.2580(7) 0.5327(9) 0.3158(10) 0.072(3) Uani 1 1 d . . . H9 H -0.3244 0.5347 0.3688 0.087 Uiso 1 1 calc R . . C10 C -0.2704(8) 0.6061(9) 0.2017(11) 0.083(3) Uani 1 1 d . . . H10 H -0.3455 0.6581 0.177 0.1 Uiso 1 1 calc R . . C11 C -0.1747(9) 0.6044(8) 0.1234(9) 0.078(3) Uani 1 1 d . . . H11 H -0.1829 0.6555 0.0454 0.093 Uiso 1 1 calc R . . C12 C -0.0647(7) 0.5256(8) 0.1614(8) 0.065(2) Uani 1 1 d . . . H12 H 0.0009 0.5229 0.1077 0.078 Uiso 1 1 calc R . . C13 C 0.2127(7) 0.4391(8) 0.3226(8) 0.060(2) Uani 1 1 d . . . C14 C 0.1842(8) 0.5639(8) 0.2936(9) 0.075(3) Uani 1 1 d . . . H14 H 0.104 0.603 0.2679 0.09 Uiso 1 1 calc R . . C15 C 0.2730(9) 0.6311(9) 0.3023(11) 0.099(4) Uani 1 1 d . . . H15 H 0.2523 0.7154 0.2813 0.119 Uiso 1 1 calc R . . C16 C 0.3897(9) 0.5769(10) 0.3410(10) 0.092(3) Uani 1 1 d . . . H16 H 0.4491 0.6238 0.3455 0.111 Uiso 1 1 calc R . . C17 C 0.4211(8) 0.4508(10) 0.3740(11) 0.098(4) Uani 1 1 d . . . H17 H 0.5008 0.4132 0.4027 0.118 Uiso 1 1 calc R . . C18 C 0.3327(7) 0.3802(9) 0.3640(9) 0.081(3) Uani 1 1 d . . . H18 H 0.3534 0.296 0.3845 0.097 Uiso 1 1 calc R . . C19 C 0.4140(8) 0.0929(9) 0.2580(9) 0.082(3) Uani 1 1 d . . . C20 C 0.5332(9) 0.0733(10) 0.3099(12) 0.110(4) Uani 1 1 d . . . C21 C 0.6292(11) -0.0045(14) 0.2896(17) 0.179(8) Uani 1 1 d . . . H21 H 0.7071 -0.0134 0.3223 0.215 Uiso 1 1 calc R . . C22 C 0.6136(12) -0.0734(16) 0.2190(19) 0.205(10) Uani 1 1 d . . . H22 H 0.6816 -0.128 0.2074 0.246 Uiso 1 1 calc R . . C23 C 0.5044(10) -0.0628(14) 0.1680(16) 0.170(8) Uani 1 1 d . . . H23 H 0.496 -0.1106 0.1233 0.204 Uiso 1 1 calc R . . C24 C 0.4021(8) 0.0223(10) 0.1835(11) 0.094(3) Uani 1 1 d . . . C25 C 0.2885(8) 0.0334(9) 0.1214(9) 0.077(3) Uani 1 1 d . . . H25 H 0.2928 -0.0146 0.0746 0.093 Uiso 1 1 calc R . . C26 C -0.0159(7) 0.1551(7) 0.0629(7) 0.058(2) Uani 1 1 d . . . C27 C 0.6533(10) 0.1234(13) 0.4347(14) 0.155(6) Uani 1 1 d . . . H27A H 0.6978 0.0437 0.4426 0.232 Uiso 1 1 calc R . . H27B H 0.6368 0.1298 0.5111 0.232 Uiso 1 1 calc R . . H27C H 0.7034 0.1841 0.389 0.232 Uiso 1 1 calc R . . N1 N 0.1827(5) 0.1012(6) 0.1228(6) 0.0553(16) Uani 1 1 d . . . N2 N 0.0919(6) 0.0880(6) 0.0566(6) 0.0593(17) Uani 1 1 d . . . N3 N -0.1152(7) 0.1457(7) 0.0056(7) 0.085(2) Uani 1 1 d . . . H31 H -0.2173 0.1576 0.0443 0.08(3) Uiso 1 1 d R . . H32 H -0.1118 0.0609 -0.0198 0.23(7) Uiso 1 1 d R . . O1 O 0.3253(5) 0.1715(5) 0.2767(6) 0.0745(18) Uani 1 1 d . . . O2 O 0.5380(6) 0.1418(7) 0.3778(8) 0.122(3) Uani 1 1 d . . . P1 P 0.09657(17) 0.34418(18) 0.31947(19) 0.0502(5) Uani 1 1 d . . . S1 S -0.04499(18) 0.2555(2) 0.1410(2) 0.0658(6) Uani 1 1 d . . . Pd1 Pd 0.14997(5) 0.21726(5) 0.21306(5) 0.0490(2) 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 0.052(4) 0.048(5) 0.072(6) -0.031(4) -0.007(4) 0.001(3) C2 0.110(7) 0.059(6) 0.067(7) -0.026(5) 0.006(5) -0.024(5) C3 0.130(9) 0.061(7) 0.109(10) -0.037(7) 0.022(7) -0.027(6) C4 0.121(9) 0.056(6) 0.079(8) -0.022(6) 0.010(6) 0.008(6) C5 0.077(6) 0.099(8) 0.059(7) -0.035(6) -0.019(5) 0.024(5) C6 0.061(5) 0.069(6) 0.070(6) -0.033(5) -0.020(4) 0.003(4) C7 0.042(4) 0.047(4) 0.057(5) -0.027(4) -0.010(3) -0.007(3) C8 0.045(4) 0.072(6) 0.078(6) -0.038(5) -0.005(4) -0.001(4) C9 0.045(5) 0.084(7) 0.095(8) -0.046(6) 0.005(5) -0.004(4) C10 0.051(5) 0.084(7) 0.118(9) -0.048(7) -0.017(5) 0.015(5) C11 0.077(6) 0.058(6) 0.093(7) -0.025(5) -0.027(5) 0.014(4) C12 0.055(5) 0.063(6) 0.091(7) -0.046(6) 0.004(4) -0.007(4) C13 0.041(4) 0.074(6) 0.078(6) -0.045(5) 0.008(4) -0.010(4) C14 0.047(5) 0.072(6) 0.121(8) -0.055(6) -0.006(5) 0.001(4) C15 0.064(6) 0.068(7) 0.180(12) -0.057(7) -0.009(6) -0.014(5) C16 0.062(6) 0.087(8) 0.150(10) -0.064(7) 0.001(6) -0.023(5) C17 0.045(5) 0.106(9) 0.164(11) -0.072(8) -0.024(6) -0.001(5) C18 0.047(5) 0.081(7) 0.131(9) -0.057(7) -0.016(5) -0.002(4) C19 0.050(5) 0.095(7) 0.116(8) -0.061(7) -0.022(5) 0.008(5) C20 0.068(6) 0.111(9) 0.178(12) -0.093(9) -0.045(7) 0.030(6) C21 0.077(8) 0.203(15) 0.34(2) -0.214(17) -0.098(11) 0.067(8) C22 0.086(9) 0.232(18) 0.38(3) -0.24(2) -0.087(12) 0.087(10) C23 0.073(8) 0.198(15) 0.32(2) -0.210(16) -0.068(10) 0.062(8) C24 0.060(5) 0.111(8) 0.143(10) -0.095(8) -0.021(6) 0.021(5) C25 0.065(6) 0.080(6) 0.109(8) -0.066(6) -0.006(5) 0.003(5) C26 0.058(5) 0.054(5) 0.072(6) -0.032(4) -0.013(4) -0.010(4) C27 0.085(8) 0.190(14) 0.234(17) -0.136(13) -0.089(9) 0.034(8) N1 0.046(3) 0.059(4) 0.072(5) -0.038(4) -0.001(3) -0.002(3) N2 0.049(4) 0.063(4) 0.083(5) -0.046(4) -0.014(3) -0.002(3) N3 0.069(5) 0.091(6) 0.120(7) -0.070(5) -0.034(4) 0.009(4) O1 0.045(3) 0.090(4) 0.110(5) -0.067(4) -0.026(3) 0.015(3) O2 0.069(4) 0.149(7) 0.196(8) -0.132(7) -0.069(5) 0.039(4) P1 0.0427(10) 0.0520(12) 0.0658(14) -0.0341(11) -0.0042(9) -0.0021(8) S1 0.0513(11) 0.0710(15) 0.0919(17) -0.0521(14) -0.0162(10) 0.0048(10) Pd1 0.0415(3) 0.0530(4) 0.0619(4) -0.0338(3) -0.0050(2) 0.0003(2) #----------------------------------------------------------------------------# # 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 1.376(11) . ? C1 C6 1.379(11) . ? C1 P1 1.795(9) . ? C2 C3 1.383(13) . ? C2 H2 0.93 . ? C3 C4 1.391(14) . ? C3 H3 0.93 . ? C4 C5 1.351(14) . ? C4 H4 0.93 . ? C5 C6 1.381(12) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.360(10) . ? C7 C12 1.371(11) . ? C7 P1 1.828(7) . ? C8 C9 1.378(11) . ? C8 H8 0.93 . ? C9 C10 1.356(13) . ? C9 H9 0.93 . ? C10 C11 1.353(13) . ? C10 H10 0.93 . ? C11 C12 1.377(11) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.378(11) . ? C13 C18 1.400(11) . ? C13 P1 1.825(8) . ? C14 C15 1.373(12) . ? C14 H14 0.93 . ? C15 C16 1.349(13) . ? C15 H15 0.93 . ? C16 C17 1.390(13) . ? C16 H16 0.93 . ? C17 C18 1.405(12) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 O1 1.284(9) . ? C19 C20 1.420(12) . ? C19 C24 1.457(12) . ? C20 C21 1.336(13) . ? C20 O2 1.354(12) . ? C21 C22 1.410(17) . ? C21 H21 0.93 . ? C22 C23 1.336(16) . ? C22 H22 0.93 . ? C23 C24 1.413(12) . ? C23 H23 0.93 . ? C24 C25 1.449(12) . ? C25 N1 1.282(9) . ? C25 H25 0.93 . ? C26 N2 1.306(9) . ? C26 N3 1.359(9) . ? C26 S1 1.744(7) . ? C27 O2 1.413(11) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? N1 N2 1.374(8) . ? N1 Pd1 2.014(6) . ? N3 H31 1.1702 . ? N3 H32 1.1432 . ? O1 Pd1 2.010(5) . ? P1 Pd1 2.2867(19) . ? S1 Pd1 2.249(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 C2 C1 C6 116.5(8) . . ? C2 C1 P1 118.6(7) . . ? C6 C1 P1 124.8(7) . . ? C1 C2 C3 121.5(9) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C2 C3 C4 120.8(10) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 117.8(10) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 C6 121.1(10) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 122.2(9) . . ? C1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C8 C7 C12 118.2(7) . . ? C8 C7 P1 122.3(7) . . ? C12 C7 P1 119.3(6) . . ? C7 C8 C9 120.5(9) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.0(8) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C11 C10 C9 120.7(8) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 118.8(9) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C7 C12 C11 121.7(8) . . ? C7 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C14 C13 C18 119.4(7) . . ? C14 C13 P1 122.7(6) . . ? C18 C13 P1 117.7(7) . . ? C15 C14 C13 120.8(8) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 121.1(9) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.9(9) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C16 C17 C18 120.1(9) . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? C13 C18 C17 118.7(9) . . ? C13 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? O1 C19 C20 119.5(8) . . ? O1 C19 C24 124.1(8) . . ? C20 C19 C24 116.4(8) . . ? C21 C20 O2 125.1(10) . . ? C21 C20 C19 121.4(10) . . ? O2 C20 C19 113.4(8) . . ? C20 C21 C22 120.6(11) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 122.3(10) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 118.8(11) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C23 C24 C25 116.0(9) . . ? C23 C24 C19 120.4(9) . . ? C25 C24 C19 123.6(7) . . ? N1 C25 C24 128.2(8) . . ? N1 C25 H25 115.9 . . ? C24 C25 H25 115.9 . . ? N2 C26 N3 118.1(7) . . ? N2 C26 S1 125.5(5) . . ? N3 C26 S1 116.4(6) . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 N1 N2 113.9(6) . . ? C25 N1 Pd1 123.9(6) . . ? N2 N1 Pd1 122.2(4) . . ? C26 N2 N1 112.5(6) . . ? C26 N3 H31 120 . . ? C26 N3 H32 118.7 . . ? H31 N3 H32 102.8 . . ? C19 O1 Pd1 127.4(5) . . ? C20 O2 C27 116.0(8) . . ? C1 P1 C13 105.5(4) . . ? C1 P1 C7 103.3(3) . . ? C13 P1 C7 104.6(3) . . ? C1 P1 Pd1 110.3(2) . . ? C13 P1 Pd1 116.6(2) . . ? C7 P1 Pd1 115.2(2) . . ? C26 S1 Pd1 96.1(3) . . ? O1 Pd1 N1 92.8(2) . . ? O1 Pd1 S1 176.04(17) . . ? N1 Pd1 S1 83.65(18) . . ? O1 Pd1 P1 90.80(15) . . ? N1 Pd1 P1 175.23(18) . . ? S1 Pd1 P1 92.62(7) . . ? # END of CIF