Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global data_global _audit_creation_date 'Wed Feb 13 13:53:05 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kawaguchi, Hiroyuki' 'Komuro, Takashi' 'Tatsumi, Kazuyuki' _publ_contact_author_name 'Prof Hiroyuki Kawaguchi' _publ_contact_author_address ; Coordination Chemistry Laboratories, Institute for Molecular Science, Myodaiji, Okazaki, 444-8585, Japan ; _publ_contact_author_email ' hkawa@ims.ac.jp ' _publ_contact_author_fax ' +81-564-55-5245 ' _publ_requested_journal ' Chem. Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ _publ_section_title ; Palladium dimethylsilanedithiolato complex: a precursor for Ti-Pd and Ti-Pd2 heterometallic complexes ; _publ_section_references ; Molecular Structure Corporation and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 2.00. MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; data__Pd(S2SiMe2)(PEt3)2 _database_code_CSD 180416 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C14 H36 P2 Pd S2 Si ' _chemical_formula_moiety 'C14 H36 P2 Pd S2 Si ' _chemical_formula_weight 464.99 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 9.443(1) _cell_length_b 17.119(2) _cell_length_c 14.368(2) _cell_angle_alpha 90 _cell_angle_beta 108.271(5) _cell_angle_gamma 90 _cell_volume 2205.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7512 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.885 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 17804 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9952 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9952 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 3387 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0400 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5037 _refine_ls_number_parameters 217 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.94 _refine_diff_density_min -1.00 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Si' 'Si' 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.15989(3) 0.81879(1) 0.16932(2) 0.02434(6) Uani 1.00 d . . . S(1) S -0.05605(8) 0.81340(5) 0.21876(6) 0.0498(3) Uani 1.00 d . . . S(2) S 0.24012(9) 0.92123(4) 0.28739(6) 0.0348(2) Uani 1.00 d . . . P(1) P 0.35996(9) 0.84904(4) 0.11667(6) 0.0277(2) Uani 1.00 d . . . P(2) P 0.07396(9) 0.71297(4) 0.07018(6) 0.0285(2) Uani 1.00 d . . . Si(1) Si 0.03025(9) 0.90983(5) 0.30887(6) 0.0320(3) Uani 1.00 d . . . C(1) C 0.3672(3) 0.8129(2) -0.0019(2) 0.0368(9) Uani 1.00 d . . . C(2) C 0.4999(4) 0.8378(2) -0.0330(2) 0.058(1) Uani 1.00 d . . . C(3) C 0.5420(3) 0.8248(2) 0.2023(2) 0.0378(9) Uani 1.00 d . . . C(4) C 0.5752(3) 0.7377(2) 0.2126(2) 0.047(1) Uani 1.00 d . . . C(5) C 0.3717(4) 0.9542(2) 0.1010(2) 0.054(1) Uani 1.00 d . . . C(6) C 0.2305(4) 0.9887(2) 0.0309(3) 0.090(2) Uani 1.00 d . . . C(7) C -0.0751(3) 0.6570(2) 0.0929(2) 0.043(1) Uani 1.00 d . . . C(8) C -0.0303(4) 0.6103(2) 0.1874(2) 0.069(1) Uani 1.00 d . . . C(9) C -0.0051(3) 0.7379(2) -0.0593(2) 0.0387(10) Uani 1.00 d . . . C(10) C -0.1116(4) 0.8073(2) -0.0772(2) 0.061(1) Uani 1.00 d . . . C(11) C 0.2120(3) 0.6362(2) 0.0738(2) 0.0349(9) Uani 1.00 d . . . C(12) C 0.1631(3) 0.5733(2) -0.0028(2) 0.055(1) Uani 1.00 d . . . C(13) C 0.0386(3) 0.8890(2) 0.4379(2) 0.050(1) Uani 1.00 d . . . C(14) C -0.0844(4) 0.9992(2) 0.2728(3) 0.062(1) Uani 1.00 d . . . H(1) H 0.3665(3) 0.7563(2) 0.0006(2) 0.043(1) Uiso 1.00 calc . . . H(2) H 0.2782(3) 0.8310(2) -0.0519(2) 0.044(1) Uiso 1.00 calc . . . H(3) H 0.5906(4) 0.8205(2) 0.0162(2) 0.069(2) Uiso 1.00 calc . . . H(4) H 0.4936(4) 0.8145(2) -0.0957(2) 0.069(2) Uiso 1.00 calc . . . H(5) H 0.5010(4) 0.8942(2) -0.0384(2) 0.069(2) Uiso 1.00 calc . . . H(6) H 0.6177(3) 0.8494(2) 0.1797(2) 0.043(1) Uiso 1.00 calc . . . H(7) H 0.5477(3) 0.8452(2) 0.2664(2) 0.043(1) Uiso 1.00 calc . . . H(8) H 0.5002(3) 0.7122(2) 0.2353(2) 0.053(1) Uiso 1.00 calc . . . H(9) H 0.5717(3) 0.7165(2) 0.1493(2) 0.053(1) Uiso 1.00 calc . . . H(10) H 0.6731(3) 0.7286(2) 0.2594(2) 0.053(1) Uiso 1.00 calc . . . H(11) H 0.3908(4) 0.9791(2) 0.1644(2) 0.061(2) Uiso 1.00 calc . . . H(12) H 0.4535(4) 0.9650(2) 0.0757(2) 0.061(2) Uiso 1.00 calc . . . H(13) H 0.2416(4) 1.0446(2) 0.0245(3) 0.100(2) Uiso 1.00 calc . . . H(14) H 0.2105(4) 0.9641(2) -0.0328(3) 0.100(2) Uiso 1.00 calc . . . H(15) H 0.1482(4) 0.9786(2) 0.0560(3) 0.100(2) Uiso 1.00 calc . . . H(16) H -0.1522(3) 0.6933(2) 0.0964(2) 0.050(1) Uiso 1.00 calc . . . H(17) H -0.1153(3) 0.6214(2) 0.0385(2) 0.050(2) Uiso 1.00 calc . . . H(18) H -0.1160(4) 0.5830(2) 0.1950(2) 0.081(2) Uiso 1.00 calc . . . H(19) H 0.0450(4) 0.5726(2) 0.1845(2) 0.081(2) Uiso 1.00 calc . . . H(20) H 0.0105(4) 0.6449(2) 0.2427(2) 0.081(2) Uiso 1.00 calc . . . H(21) H 0.0756(3) 0.7509(2) -0.0849(2) 0.046(1) Uiso 1.00 calc . . . H(22) H -0.0590(3) 0.6930(2) -0.0942(2) 0.046(1) Uiso 1.00 calc . . . H(23) H -0.0587(4) 0.8524(2) -0.0422(2) 0.072(2) Uiso 1.00 calc . . . H(24) H -0.1502(4) 0.8191(2) -0.1466(2) 0.072(2) Uiso 1.00 calc . . . H(25) H -0.1936(4) 0.7945(2) -0.0528(2) 0.072(2) Uiso 1.00 calc . . . H(26) H 0.3006(3) 0.6609(2) 0.0670(2) 0.041(1) Uiso 1.00 calc . . . H(27) H 0.2361(3) 0.6109(2) 0.1373(2) 0.041(1) Uiso 1.00 calc . . . H(28) H 0.0745(3) 0.5477(2) 0.0027(2) 0.063(2) Uiso 1.00 calc . . . H(29) H 0.1408(3) 0.5972(2) -0.0670(2) 0.063(2) Uiso 1.00 calc . . . H(30) H 0.2421(3) 0.5351(2) 0.0057(2) 0.063(2) Uiso 1.00 calc . . . H(31) H -0.0616(3) 0.8814(2) 0.4411(2) 0.060(2) Uiso 1.00 calc . . . H(32) H 0.0968(3) 0.8420(2) 0.4602(2) 0.060(2) Uiso 1.00 calc . . . H(33) H 0.0851(3) 0.9326(2) 0.4795(2) 0.060(2) Uiso 1.00 calc . . . H(34) H -0.0371(4) 1.0419(2) 0.3157(3) 0.074(2) Uiso 1.00 calc . . . H(35) H -0.0927(4) 1.0125(2) 0.2057(3) 0.074(2) Uiso 1.00 calc . . . H(36) H -0.1831(4) 0.9901(2) 0.2780(3) 0.074(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0194(1) 0.0248(1) 0.0280(1) -0.0027(1) 0.01136(9) -0.0053(1) S(1) 0.0276(5) 0.0544(5) 0.0609(6) -0.0139(5) 0.0264(4) -0.0266(5) S(2) 0.0305(5) 0.0338(4) 0.0395(5) -0.0086(4) 0.0181(4) -0.0127(4) P(1) 0.0265(5) 0.0254(4) 0.0309(5) -0.0037(4) 0.0151(4) -0.0031(4) P(2) 0.0258(5) 0.0289(4) 0.0307(5) -0.0050(4) 0.0111(4) -0.0062(4) Si(1) 0.0277(5) 0.0319(5) 0.0358(5) 0.0016(4) 0.0155(4) -0.0064(4) C(1) 0.044(2) 0.035(2) 0.030(2) -0.004(2) 0.019(2) -0.002(2) C(2) 0.066(3) 0.052(2) 0.054(2) -0.011(2) 0.045(2) -0.007(2) C(3) 0.025(2) 0.051(2) 0.032(2) -0.011(2) 0.012(1) -0.002(2) C(4) 0.030(2) 0.066(2) 0.037(2) 0.007(2) 0.010(2) 0.008(2) C(5) 0.063(3) 0.025(2) 0.063(3) -0.009(2) 0.044(2) -0.005(2) C(6) 0.093(3) 0.038(2) 0.119(4) 0.017(2) 0.048(3) 0.028(2) C(7) 0.033(2) 0.039(2) 0.054(2) -0.014(2) 0.021(2) -0.016(2) C(8) 0.080(3) 0.050(2) 0.073(3) -0.012(2) 0.052(2) 0.001(2) C(9) 0.034(2) 0.045(2) 0.036(2) -0.002(2) 0.007(2) -0.006(2) C(10) 0.058(3) 0.074(3) 0.047(2) 0.031(2) 0.002(2) -0.001(2) C(11) 0.032(2) 0.026(2) 0.044(2) -0.001(2) 0.017(2) 0.001(1) C(12) 0.046(2) 0.035(2) 0.075(3) 0.003(2) 0.022(2) -0.014(2) C(13) 0.047(2) 0.054(2) 0.049(2) -0.009(2) 0.026(2) -0.005(2) C(14) 0.057(3) 0.057(2) 0.072(3) 0.018(2) 0.019(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ORTEP-3 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(1) 2.362(1) . . yes Pd(1) S(2) 2.3919(8) . . yes Pd(1) P(1) 2.303(1) . . yes Pd(1) P(2) 2.2901(7) . . yes S(1) Si(1) 2.099(1) . . yes S(2) Si(1) 2.108(1) . . yes P(1) C(1) 1.834(3) . . yes P(1) C(3) 1.821(3) . . yes P(1) C(5) 1.823(3) . . yes P(2) C(7) 1.815(3) . . yes P(2) C(9) 1.825(3) . . yes P(2) C(11) 1.840(3) . . yes Si(1) C(13) 1.865(3) . . yes Si(1) C(14) 1.852(3) . . yes C(1) C(2) 1.517(5) . . yes C(3) C(4) 1.521(4) . . yes C(5) C(6) 1.516(4) . . yes C(7) C(8) 1.517(4) . . yes C(9) C(10) 1.525(4) . . yes C(11) C(12) 1.505(4) . . yes C(12) C(13) 1.377(4) . 4_564 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Pd(1) S(2) 85.80(3) . . . yes S(1) Pd(1) P(1) 169.06(3) . . . yes S(1) Pd(1) P(2) 89.15(3) . . . yes S(2) Pd(1) P(1) 87.60(3) . . . yes S(2) Pd(1) P(2) 173.11(3) . . . yes P(1) Pd(1) P(2) 98.09(3) . . . yes Pd(1) S(1) Si(1) 87.13(4) . . . yes Pd(1) S(2) Si(1) 86.14(4) . . . yes Pd(1) P(1) C(1) 120.17(10) . . . yes Pd(1) P(1) C(3) 115.1(1) . . . yes Pd(1) P(1) C(5) 110.5(1) . . . yes C(1) P(1) C(3) 104.4(1) . . . yes C(1) P(1) C(5) 101.4(2) . . . yes C(3) P(1) C(5) 103.2(1) . . . yes Pd(1) P(2) C(7) 116.7(1) . . . yes Pd(1) P(2) C(9) 113.64(10) . . . yes Pd(1) P(2) C(11) 115.95(9) . . . yes C(7) P(2) C(9) 102.4(1) . . . yes C(7) P(2) C(11) 101.6(1) . . . yes C(9) P(2) C(11) 104.8(1) . . . yes S(1) Si(1) S(2) 100.58(5) . . . yes S(1) Si(1) C(13) 110.5(1) . . . yes S(1) Si(1) C(14) 113.42(10) . . . yes S(2) Si(1) C(13) 114.5(1) . . . yes S(2) Si(1) C(14) 112.1(1) . . . yes C(13) Si(1) C(14) 105.9(2) . . . yes P(1) C(1) C(2) 117.0(2) . . . yes P(1) C(3) C(4) 114.3(2) . . . yes P(1) C(5) C(6) 113.1(2) . . . yes P(2) C(7) C(8) 115.1(2) . . . yes P(2) C(9) C(10) 113.0(2) . . . yes P(2) C(11) C(12) 116.0(2) . . . yes C(11) C(12) C(13) 97.1(2) . . 4_564 yes Si(1) C(13) C(12) 106.7(2) . . 4_565 yes #------------------------------------------------------------------------------ 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 Pd(1) S(1) Si(1) S(2) -4.87(4) . . . . yes Pd(1) S(1) Si(1) C(13) -126.2(1) . . . . yes Pd(1) S(1) Si(1) C(14) 115.0(1) . . . . yes Pd(1) S(2) Si(1) S(1) 4.81(4) . . . . yes Pd(1) S(2) Si(1) C(13) 123.3(1) . . . . yes Pd(1) S(2) Si(1) C(14) -116.0(1) . . . . yes Pd(1) P(1) C(1) C(2) 177.9(2) . . . . yes Pd(1) P(1) C(3) C(4) 71.5(2) . . . . yes Pd(1) P(1) C(5) C(6) -56.8(3) . . . . yes Pd(1) P(2) C(7) C(8) -70.1(2) . . . . yes Pd(1) P(2) C(9) C(10) -46.4(2) . . . . yes Pd(1) P(2) C(11) C(12) -170.3(2) . . . . yes S(1) Pd(1) S(2) Si(1) -4.21(3) . . . . yes S(1) Pd(1) P(1) C(1) -111.4(2) . . . . yes S(1) Pd(1) P(1) C(3) 122.4(2) . . . . yes S(1) Pd(1) P(1) C(5) 6.0(2) . . . . yes S(1) Pd(1) P(2) C(7) -15.8(1) . . . . yes S(1) Pd(1) P(2) C(9) 103.0(1) . . . . yes S(1) Pd(1) P(2) C(11) -135.4(1) . . . . yes S(1) Si(1) C(13) C(12) 145.6(2) . . . 4_565 yes S(2) Pd(1) S(1) Si(1) 4.23(3) . . . . yes S(2) Pd(1) P(1) C(1) -164.3(1) . . . . yes S(2) Pd(1) P(1) C(3) 69.5(1) . . . . yes S(2) Pd(1) P(1) C(5) -46.8(1) . . . . yes S(2) Pd(1) P(2) C(7) 26.9(3) . . . . yes S(2) Pd(1) P(2) C(9) 145.8(2) . . . . yes S(2) Pd(1) P(2) C(11) -92.7(3) . . . . yes S(2) Si(1) C(13) C(12) 32.9(2) . . . 4_565 yes P(1) Pd(1) S(1) Si(1) -48.8(2) . . . . yes P(1) Pd(1) S(2) Si(1) 167.06(3) . . . . yes P(1) Pd(1) P(2) C(7) 172.4(1) . . . . yes P(1) Pd(1) P(2) C(9) -68.8(1) . . . . yes P(1) Pd(1) P(2) C(11) 52.8(1) . . . . yes P(2) Pd(1) S(1) Si(1) 179.54(4) . . . . yes P(2) Pd(1) S(2) Si(1) -47.1(3) . . . . yes P(2) Pd(1) P(1) C(1) 19.6(1) . . . . yes P(2) Pd(1) P(1) C(3) -106.5(1) . . . . yes P(2) Pd(1) P(1) C(5) 137.1(1) . . . . yes P(2) C(11) C(12) C(13) 13.8(3) . . . 4_564 yes C(1) P(1) C(3) C(4) -62.4(3) . . . . yes C(1) P(1) C(5) C(6) 71.8(3) . . . . yes C(2) C(1) P(1) C(3) -51.2(2) . . . . yes C(2) C(1) P(1) C(5) 55.8(2) . . . . yes C(3) P(1) C(5) C(6) 179.7(3) . . . . yes C(4) C(3) P(1) C(5) -168.0(2) . . . . yes C(7) P(2) C(9) C(10) 80.4(2) . . . . yes C(7) P(2) C(11) C(12) 62.2(3) . . . . yes C(8) C(7) P(2) C(9) 165.1(2) . . . . yes C(8) C(7) P(2) C(11) 57.0(3) . . . . yes C(9) P(2) C(11) C(12) -44.1(3) . . . . yes C(10) C(9) P(2) C(11) -173.9(2) . . . . yes C(10) C(9) P(2) C(11) -173.9(2) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Si(1) C(8) 3.432(3) . 2_555 ? C(4) C(10) 3.586(4) . 4_665 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_CpTiClS2Pd(PEt3)2 _database_code_CSD 180417 _audit_creation_date 'Wed Feb 13 19:09:29 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H35 Cl P2 Pd S2 Ti ' _chemical_formula_moiety '?' _chemical_formula_weight 555.28 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.417(5) _cell_length_b 17.174(8) _cell_length_c 12.419(6) _cell_angle_alpha 90 _cell_angle_beta 99.558(7) _cell_angle_gamma 90 _cell_volume 2401(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8638 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 153.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.928 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 19287 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.9863 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.9863 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 4148 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0780 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5430 _refine_ls_number_parameters 252 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.88 _refine_diff_density_min -0.83 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ti' 'Ti' 0.278 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.20794(2) 0.24234(1) 0.07601(2) 0.01525(6) Uani 1.00 d . . . Ti(1) Ti 0.27109(5) 0.07734(3) 0.02612(5) 0.0171(1) Uani 1.00 d . . . Cl(1) Cl 0.38067(8) 0.03681(5) 0.19239(7) 0.0294(2) Uani 1.00 d . . . S(1) S 0.10325(7) 0.12378(5) 0.06981(8) 0.0299(2) Uani 1.00 d . . . S(2) S 0.36009(7) 0.18715(5) -0.00982(7) 0.0239(2) Uani 1.00 d . . . P(1) P 0.05107(7) 0.29549(5) 0.14860(6) 0.0167(2) Uani 1.00 d . . . P(2) P 0.33307(8) 0.34877(5) 0.08297(7) 0.0245(2) Uani 1.00 d . . . C(1) C 0.2210(3) 0.0435(2) -0.1594(3) 0.0277(9) Uani 1.00 d . . . C(2) C 0.1451(3) 0.0003(2) -0.1039(3) 0.0322(10) Uani 1.00 d . . . C(3) C 0.2154(3) -0.0515(2) -0.0334(3) 0.036(1) Uani 1.00 d . . . C(4) C 0.3344(3) -0.0419(2) -0.0480(3) 0.0315(10) Uani 1.00 d . . . C(5) C 0.3384(3) 0.0166(2) -0.1249(3) 0.0283(9) Uani 1.00 d . . . C(6) C -0.0113(3) 0.3865(2) 0.0878(3) 0.0274(9) Uani 1.00 d . . . C(7) C -0.0675(4) 0.3779(3) -0.0314(3) 0.046(1) Uani 1.00 d . . . C(8) C -0.0832(3) 0.2346(2) 0.1401(3) 0.0259(9) Uani 1.00 d . . . C(9) C -0.1921(3) 0.2722(2) 0.1771(3) 0.037(1) Uani 1.00 d . . . C(10) C 0.0902(3) 0.3176(2) 0.2943(3) 0.0260(9) Uani 1.00 d . . . C(11) C 0.1500(4) 0.2506(3) 0.3618(3) 0.049(1) Uani 1.00 d . . . C(12) C 0.4835(3) 0.3266(2) 0.1516(3) 0.033(1) Uani 1.00 d . . . C(13) C 0.4885(5) 0.2888(4) 0.2619(4) 0.068(2) Uani 1.00 d . . . C(14) C 0.3541(4) 0.3827(2) -0.0519(3) 0.040(1) Uani 1.00 d . . . C(15) C 0.2381(5) 0.4057(4) -0.1252(5) 0.079(2) Uani 1.00 d . . . C(16) C 0.3004(4) 0.4366(2) 0.1556(5) 0.069(1) Uani 1.00 d . . . C(17) C 0.3771(4) 0.5085(2) 0.1473(4) 0.048(1) Uani 1.00 d . . . H(1) H 0.1959(3) 0.0797(2) -0.2187(3) 0.033(1) Uiso 1.00 calc . . . H(2) H 0.0590(3) 0.0021(2) -0.1176(3) 0.037(1) Uiso 1.00 calc . . . H(3) H 0.1863(3) -0.0916(2) 0.0105(3) 0.041(1) Uiso 1.00 calc . . . H(4) H 0.4013(3) -0.0734(2) -0.0149(3) 0.037(1) Uiso 1.00 calc . . . H(5) H 0.4076(3) 0.0320(2) -0.1557(3) 0.034(1) Uiso 1.00 calc . . . H(6) H -0.0715(3) 0.4046(2) 0.1286(3) 0.032(1) Uiso 1.00 calc . . . H(7) H 0.0518(3) 0.4248(2) 0.0928(3) 0.032(1) Uiso 1.00 calc . . . H(8) H -0.0995(4) 0.4275(3) -0.0599(3) 0.054(2) Uiso 1.00 calc . . . H(9) H -0.0078(4) 0.3605(3) -0.0732(3) 0.054(2) Uiso 1.00 calc . . . H(10) H -0.1310(4) 0.3398(3) -0.0373(3) 0.054(2) Uiso 1.00 calc . . . H(11) H -0.1063(3) 0.2190(2) 0.0644(3) 0.030(1) Uiso 1.00 calc . . . H(12) H -0.0621(3) 0.1888(2) 0.1848(3) 0.030(1) Uiso 1.00 calc . . . H(13) H -0.1721(3) 0.2868(2) 0.2534(3) 0.043(2) Uiso 1.00 calc . . . H(14) H -0.2152(3) 0.3182(2) 0.1334(3) 0.043(2) Uiso 1.00 calc . . . H(15) H -0.2574(3) 0.2354(2) 0.1681(3) 0.043(2) Uiso 1.00 calc . . . H(16) H 0.1444(3) 0.3615(2) 0.3029(3) 0.031(1) Uiso 1.00 calc . . . H(17) H 0.0185(3) 0.3314(2) 0.3222(3) 0.031(1) Uiso 1.00 calc . . . H(18) H 0.0968(4) 0.2062(3) 0.3532(3) 0.054(2) Uiso 1.00 calc . . . H(19) H 0.2230(4) 0.2371(3) 0.3357(3) 0.055(2) Uiso 1.00 calc . . . H(20) H 0.1681(4) 0.2649(3) 0.4383(3) 0.055(2) Uiso 1.00 calc . . . H(21) H 0.5200(3) 0.2917(2) 0.1054(3) 0.040(1) Uiso 1.00 calc . . . H(22) H 0.5284(3) 0.3747(2) 0.1618(3) 0.040(1) Uiso 1.00 calc . . . H(23) H 0.4523(5) 0.3231(4) 0.3090(4) 0.078(2) Uiso 1.00 calc . . . H(24) H 0.4451(5) 0.2401(4) 0.2528(4) 0.078(2) Uiso 1.00 calc . . . H(25) H 0.5703(5) 0.2788(4) 0.2944(4) 0.078(2) Uiso 1.00 calc . . . H(26) H 0.4063(4) 0.4276(2) -0.0429(3) 0.048(2) Uiso 1.00 calc . . . H(27) H 0.3905(4) 0.3413(2) -0.0878(3) 0.048(2) Uiso 1.00 calc . . . H(28) H 0.2009(5) 0.4472(4) -0.0900(5) 0.095(2) Uiso 1.00 calc . . . H(29) H 0.2535(5) 0.4235(4) -0.1957(5) 0.095(2) Uiso 1.00 calc . . . H(30) H 0.1855(5) 0.3609(4) -0.1354(5) 0.095(2) Uiso 1.00 calc . . . H(31) H 0.2185(4) 0.4509(2) 0.1289(5) 0.073(2) Uiso 1.00 calc . . . H(32) H 0.3094(4) 0.4233(2) 0.2324(5) 0.073(2) Uiso 1.00 calc . . . H(33) H 0.4596(4) 0.4961(2) 0.1740(4) 0.054(2) Uiso 1.00 calc . . . H(34) H 0.3681(4) 0.5242(2) 0.0713(4) 0.054(2) Uiso 1.00 calc . . . H(35) H 0.3522(4) 0.5508(2) 0.1901(4) 0.054(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0143(1) 0.0130(1) 0.0180(1) -0.0004(1) 0.00578(8) -0.00011(9) Ti(1) 0.0154(3) 0.0150(3) 0.0204(3) 0.0001(2) 0.0046(2) -0.0019(2) Cl(1) 0.0323(5) 0.0326(5) 0.0221(4) 0.0068(4) 0.0042(3) 0.0035(4) S(1) 0.0182(4) 0.0171(4) 0.0454(5) -0.0020(4) 0.0134(4) -0.0042(3) S(2) 0.0232(4) 0.0182(4) 0.0292(5) -0.0012(3) 0.0143(4) -0.0025(3) P(1) 0.0150(4) 0.0175(4) 0.0175(4) 0.0013(3) 0.0032(3) -0.0014(3) P(2) 0.0208(4) 0.0175(4) 0.0326(5) -0.0037(4) 0.0114(4) -0.0006(3) C(1) 0.032(2) 0.030(2) 0.020(2) 0.000(1) 0.000(1) -0.008(2) C(2) 0.019(2) 0.036(2) 0.039(2) -0.005(2) 0.001(2) -0.015(2) C(3) 0.044(2) 0.020(2) 0.038(2) -0.010(2) 0.004(2) -0.009(2) C(4) 0.033(2) 0.023(2) 0.037(2) 0.010(2) -0.003(2) -0.017(2) C(5) 0.024(2) 0.031(2) 0.030(2) -0.003(2) 0.008(1) -0.016(1) C(6) 0.026(2) 0.020(2) 0.034(2) 0.003(1) -0.001(1) 0.001(1) C(7) 0.052(3) 0.054(3) 0.029(2) 0.013(2) -0.002(2) 0.013(2) C(8) 0.016(2) 0.027(2) 0.032(2) -0.001(1) 0.007(1) -0.002(1) C(9) 0.022(2) 0.046(2) 0.038(2) 0.000(2) 0.012(2) -0.009(2) C(10) 0.023(2) 0.032(2) 0.021(2) 0.001(1) 0.006(1) -0.003(1) C(11) 0.045(2) 0.067(3) 0.025(2) 0.020(2) 0.004(2) 0.010(2) C(12) 0.027(2) 0.031(2) 0.041(2) -0.007(2) 0.004(2) -0.005(2) C(13) 0.059(3) 0.091(4) 0.045(3) -0.023(3) -0.016(2) 0.019(3) C(14) 0.043(2) 0.033(2) 0.042(2) -0.013(2) 0.014(2) 0.013(2) C(15) 0.081(4) 0.084(4) 0.073(4) -0.013(3) -0.006(3) 0.050(3) C(16) 0.049(3) 0.026(2) 0.107(4) -0.016(2) 0.049(3) -0.025(2) C(17) 0.045(2) 0.025(2) 0.065(3) -0.013(2) 0.025(2) -0.009(2) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ORTEP-3 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Ti(1) 3.0137(6) . . yes Pd(1) S(1) 2.3559(9) . . yes Pd(1) S(2) 2.381(1) . . yes Pd(1) P(1) 2.322(1) . . yes Pd(1) P(2) 2.313(1) . . yes Ti(1) Cl(1) 2.336(1) . . yes Ti(1) S(1) 2.224(1) . . yes Ti(1) S(2) 2.222(1) . . yes Ti(1) C(1) 2.353(3) . . yes Ti(1) C(2) 2.378(4) . . yes Ti(1) C(3) 2.386(4) . . yes Ti(1) C(4) 2.405(4) . . yes Ti(1) C(5) 2.382(4) . . yes P(1) C(6) 1.828(4) . . yes P(1) C(8) 1.844(3) . . yes P(1) C(10) 1.830(3) . . yes P(2) C(12) 1.827(4) . . yes P(2) C(14) 1.826(4) . . yes P(2) C(16) 1.828(5) . . yes C(1) C(2) 1.406(5) . . yes C(1) C(5) 1.416(5) . . yes C(2) C(3) 1.404(5) . . yes C(3) C(4) 1.410(6) . . yes C(4) C(5) 1.391(5) . . yes C(6) C(7) 1.520(5) . . yes C(8) C(9) 1.537(5) . . yes C(10) C(11) 1.518(5) . . yes C(12) C(13) 1.507(6) . . yes C(14) C(15) 1.529(7) . . yes C(16) C(17) 1.527(6) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ti(1) Pd(1) S(1) 47.00(3) . . . yes Ti(1) Pd(1) S(2) 46.87(2) . . . yes Ti(1) Pd(1) P(1) 132.52(3) . . . yes Ti(1) Pd(1) P(2) 125.69(3) . . . yes S(1) Pd(1) S(2) 92.59(4) . . . yes S(1) Pd(1) P(1) 86.13(4) . . . yes S(1) Pd(1) P(2) 172.41(3) . . . yes S(2) Pd(1) P(1) 176.17(3) . . . yes S(2) Pd(1) P(2) 80.75(4) . . . yes P(1) Pd(1) P(2) 100.74(4) . . . yes Pd(1) Ti(1) Cl(1) 102.11(3) . . . yes Pd(1) Ti(1) S(1) 50.77(3) . . . yes Pd(1) Ti(1) S(2) 51.42(3) . . . yes Pd(1) Ti(1) C(1) 113.94(9) . . . yes Pd(1) Ti(1) C(2) 121.62(9) . . . yes Pd(1) Ti(1) C(3) 151.10(10) . . . yes Pd(1) Ti(1) C(4) 167.59(10) . . . yes Pd(1) Ti(1) C(5) 133.88(9) . . . yes Cl(1) Ti(1) S(1) 104.35(5) . . . yes Cl(1) Ti(1) S(2) 103.58(4) . . . yes Cl(1) Ti(1) C(1) 143.10(9) . . . yes Cl(1) Ti(1) C(2) 127.53(9) . . . yes Cl(1) Ti(1) C(3) 94.21(9) . . . yes Cl(1) Ti(1) C(4) 86.20(9) . . . yes Cl(1) Ti(1) C(5) 111.71(9) . . . yes S(1) Ti(1) S(2) 100.71(4) . . . yes S(1) Ti(1) C(1) 104.37(9) . . . yes S(1) Ti(1) C(2) 85.21(10) . . . yes S(1) Ti(1) C(3) 102.3(1) . . . yes S(1) Ti(1) C(4) 136.44(10) . . . yes S(1) Ti(1) C(5) 138.83(8) . . . yes S(2) Ti(1) C(1) 93.31(9) . . . yes S(2) Ti(1) C(2) 125.52(10) . . . yes S(2) Ti(1) C(3) 146.3(1) . . . yes S(2) Ti(1) C(4) 118.0(1) . . . yes S(2) Ti(1) C(5) 89.74(9) . . . yes C(1) Ti(1) C(2) 34.6(1) . . . yes C(1) Ti(1) C(3) 57.2(1) . . . yes C(1) Ti(1) C(4) 57.0(1) . . . yes C(1) Ti(1) C(5) 34.8(1) . . . yes C(2) Ti(1) C(3) 34.3(1) . . . yes C(2) Ti(1) C(4) 56.8(1) . . . yes C(2) Ti(1) C(5) 57.3(1) . . . yes C(3) Ti(1) C(4) 34.2(1) . . . yes C(3) Ti(1) C(5) 56.9(1) . . . yes C(4) Ti(1) C(5) 33.8(1) . . . yes Pd(1) S(1) Ti(1) 82.24(4) . . . yes Pd(1) S(2) Ti(1) 81.72(4) . . . yes Pd(1) P(1) C(6) 116.6(1) . . . yes Pd(1) P(1) C(8) 116.2(1) . . . yes Pd(1) P(1) C(10) 112.8(1) . . . yes C(6) P(1) C(8) 101.4(2) . . . yes C(6) P(1) C(10) 104.2(2) . . . yes C(8) P(1) C(10) 103.8(2) . . . yes Pd(1) P(2) C(12) 112.3(1) . . . yes Pd(1) P(2) C(14) 113.1(1) . . . yes Pd(1) P(2) C(16) 119.7(2) . . . yes C(12) P(2) C(14) 103.8(2) . . . yes C(12) P(2) C(16) 101.2(2) . . . yes C(14) P(2) C(16) 104.9(2) . . . yes Ti(1) C(1) C(2) 73.7(2) . . . yes Ti(1) C(1) C(5) 73.8(2) . . . yes C(2) C(1) C(5) 108.0(3) . . . yes Ti(1) C(2) C(1) 71.7(2) . . . yes Ti(1) C(2) C(3) 73.2(2) . . . yes C(1) C(2) C(3) 107.8(3) . . . yes Ti(1) C(3) C(2) 72.6(2) . . . yes Ti(1) C(3) C(4) 73.6(2) . . . yes C(2) C(3) C(4) 108.0(3) . . . yes Ti(1) C(4) C(3) 72.1(2) . . . yes Ti(1) C(4) C(5) 72.2(2) . . . yes C(3) C(4) C(5) 108.4(3) . . . yes Ti(1) C(5) C(1) 71.5(2) . . . yes Ti(1) C(5) C(4) 74.0(2) . . . yes C(1) C(5) C(4) 107.8(3) . . . yes P(1) C(6) C(7) 113.1(3) . . . yes P(1) C(8) C(9) 116.8(3) . . . yes P(1) C(10) C(11) 113.7(3) . . . yes P(2) C(12) C(13) 113.9(3) . . . yes P(2) C(14) C(15) 113.3(3) . . . yes P(2) C(16) C(17) 117.9(4) . . . yes #------------------------------------------------------------------------------ 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 Pd(1) Ti(1) C(1) C(2) -111.5(2) . . . . yes Pd(1) Ti(1) C(1) C(5) 133.6(2) . . . . yes Pd(1) Ti(1) C(2) C(1) 86.9(2) . . . . yes Pd(1) Ti(1) C(2) C(3) -157.2(2) . . . . yes Pd(1) Ti(1) C(3) C(2) 43.0(3) . . . . yes Pd(1) Ti(1) C(3) C(4) 158.4(2) . . . . yes Pd(1) Ti(1) C(4) C(3) -124.2(4) . . . . yes Pd(1) Ti(1) C(4) C(5) -7.4(5) . . . . yes Pd(1) Ti(1) C(5) C(1) -66.6(2) . . . . yes Pd(1) Ti(1) C(5) C(4) 177.8(2) . . . . yes Pd(1) S(1) Ti(1) Cl(1) 94.05(4) . . . . yes Pd(1) S(1) Ti(1) S(2) -13.11(4) . . . . yes Pd(1) S(1) Ti(1) C(1) -109.37(10) . . . . yes Pd(1) S(1) Ti(1) C(2) -138.39(10) . . . . yes Pd(1) S(1) Ti(1) C(3) -168.30(9) . . . . yes Pd(1) S(1) Ti(1) C(4) -166.2(1) . . . . yes Pd(1) S(1) Ti(1) C(5) -115.2(1) . . . . yes Pd(1) S(2) Ti(1) Cl(1) -94.78(4) . . . . yes Pd(1) S(2) Ti(1) S(1) 12.99(4) . . . . yes Pd(1) S(2) Ti(1) C(1) 118.29(9) . . . . yes Pd(1) S(2) Ti(1) C(2) 104.7(1) . . . . yes Pd(1) S(2) Ti(1) C(3) 145.3(2) . . . . yes Pd(1) S(2) Ti(1) C(4) 172.29(10) . . . . yes Pd(1) S(2) Ti(1) C(5) 152.91(8) . . . . yes Pd(1) P(1) C(6) C(7) 63.7(3) . . . . yes Pd(1) P(1) C(8) C(9) -174.0(2) . . . . yes Pd(1) P(1) C(10) C(11) -49.8(3) . . . . yes Pd(1) P(2) C(12) C(13) -51.2(3) . . . . yes Pd(1) P(2) C(14) C(15) 58.4(4) . . . . yes Pd(1) P(2) C(16) C(17) -173.2(3) . . . . yes Ti(1) Pd(1) P(1) C(6) -140.2(1) . . . . yes Ti(1) Pd(1) P(1) C(8) -20.6(1) . . . . yes Ti(1) Pd(1) P(1) C(10) 99.2(1) . . . . yes Ti(1) Pd(1) P(2) C(12) -41.8(1) . . . . yes Ti(1) Pd(1) P(2) C(14) 75.3(1) . . . . yes Ti(1) Pd(1) P(2) C(16) -160.2(2) . . . . yes Ti(1) S(1) Pd(1) S(2) 12.02(3) . . . . yes Ti(1) S(1) Pd(1) P(1) -171.60(3) . . . . yes Ti(1) S(1) Pd(1) P(2) -16.4(3) . . . . yes Ti(1) S(2) Pd(1) S(1) -12.05(3) . . . . yes Ti(1) S(2) Pd(1) P(1) -82.6(5) . . . . yes Ti(1) S(2) Pd(1) P(2) 164.30(3) . . . . yes Ti(1) C(1) C(2) C(3) -64.8(3) . . . . yes Ti(1) C(1) C(5) C(4) 65.6(3) . . . . yes Ti(1) C(2) C(1) C(5) 66.3(2) . . . . yes Ti(1) C(2) C(3) C(4) -65.6(3) . . . . yes Ti(1) C(3) C(2) C(1) 63.8(3) . . . . yes Ti(1) C(3) C(4) C(5) -63.6(3) . . . . yes Ti(1) C(4) C(3) C(2) 64.9(3) . . . . yes Ti(1) C(4) C(5) C(1) -63.9(2) . . . . yes Ti(1) C(5) C(1) C(2) -66.3(3) . . . . yes Ti(1) C(5) C(4) C(3) 63.5(3) . . . . yes Cl(1) Ti(1) Pd(1) S(1) -98.75(5) . . . . yes Cl(1) Ti(1) Pd(1) S(2) 97.82(5) . . . . yes Cl(1) Ti(1) Pd(1) P(1) -87.35(5) . . . . yes Cl(1) Ti(1) Pd(1) P(2) 78.61(5) . . . . yes Cl(1) Ti(1) C(1) C(2) 81.7(2) . . . . yes Cl(1) Ti(1) C(1) C(5) -33.2(3) . . . . yes Cl(1) Ti(1) C(2) C(1) -131.5(2) . . . . yes Cl(1) Ti(1) C(2) C(3) -15.6(3) . . . . yes Cl(1) Ti(1) C(3) C(2) 167.6(2) . . . . yes Cl(1) Ti(1) C(3) C(4) -76.9(2) . . . . yes Cl(1) Ti(1) C(4) C(3) 103.2(2) . . . . yes Cl(1) Ti(1) C(4) C(5) -140.0(2) . . . . yes Cl(1) Ti(1) C(5) C(1) 159.3(2) . . . . yes Cl(1) Ti(1) C(5) C(4) 43.7(2) . . . . yes S(1) Pd(1) Ti(1) S(2) 163.43(5) . . . . yes S(1) Pd(1) Ti(1) C(1) 89.3(1) . . . . yes S(1) Pd(1) Ti(1) C(2) 51.0(1) . . . . yes S(1) Pd(1) Ti(1) C(3) 24.2(2) . . . . yes S(1) Pd(1) Ti(1) C(4) 130.0(4) . . . . yes S(1) Pd(1) Ti(1) C(5) 124.3(1) . . . . yes S(1) Pd(1) P(1) C(6) -131.9(1) . . . . yes S(1) Pd(1) P(1) C(8) -12.2(1) . . . . yes S(1) Pd(1) P(1) C(10) 107.6(1) . . . . yes S(1) Pd(1) P(2) C(12) -27.0(3) . . . . yes S(1) Pd(1) P(2) C(14) 90.1(3) . . . . yes S(1) Pd(1) P(2) C(16) -145.5(3) . . . . yes S(1) Ti(1) Pd(1) S(2) -163.43(5) . . . . yes S(1) Ti(1) Pd(1) P(1) 11.40(4) . . . . yes S(1) Ti(1) Pd(1) P(2) 177.36(4) . . . . yes S(1) Ti(1) C(1) C(2) -58.4(2) . . . . yes S(1) Ti(1) C(1) C(5) -173.3(2) . . . . yes S(1) Ti(1) C(2) C(1) 124.1(2) . . . . yes S(1) Ti(1) C(2) C(3) -120.1(2) . . . . yes S(1) Ti(1) C(3) C(2) 61.9(2) . . . . yes S(1) Ti(1) C(3) C(4) 177.4(2) . . . . yes S(1) Ti(1) C(4) C(3) -3.7(3) . . . . yes S(1) Ti(1) C(4) C(5) 113.1(2) . . . . yes S(1) Ti(1) C(5) C(1) 9.9(3) . . . . yes S(1) Ti(1) C(5) C(4) -105.7(2) . . . . yes S(2) Pd(1) Ti(1) C(1) -74.1(1) . . . . yes S(2) Pd(1) Ti(1) C(2) -112.4(1) . . . . yes S(2) Pd(1) Ti(1) C(3) -139.2(2) . . . . yes S(2) Pd(1) Ti(1) C(4) -33.4(4) . . . . yes S(2) Pd(1) Ti(1) C(5) -39.2(1) . . . . yes S(2) Pd(1) P(1) C(6) -61.2(5) . . . . yes S(2) Pd(1) P(1) C(8) 58.5(5) . . . . yes S(2) Pd(1) P(1) C(10) 178.3(5) . . . . yes S(2) Pd(1) P(2) C(12) -55.9(1) . . . . yes S(2) Pd(1) P(2) C(14) 61.2(1) . . . . yes S(2) Pd(1) P(2) C(16) -174.3(2) . . . . yes S(2) Ti(1) Pd(1) P(1) 174.84(4) . . . . yes S(2) Ti(1) Pd(1) P(2) -19.20(4) . . . . yes S(2) Ti(1) C(1) C(2) -160.4(2) . . . . yes S(2) Ti(1) C(1) C(5) 84.8(2) . . . . yes S(2) Ti(1) C(2) C(1) 24.3(2) . . . . yes S(2) Ti(1) C(2) C(3) 140.2(2) . . . . yes S(2) Ti(1) C(3) C(2) -70.0(3) . . . . yes S(2) Ti(1) C(3) C(4) 45.4(3) . . . . yes S(2) Ti(1) C(4) C(3) -153.4(2) . . . . yes S(2) Ti(1) C(4) C(5) -36.6(2) . . . . yes S(2) Ti(1) C(5) C(1) -96.2(2) . . . . yes S(2) Ti(1) C(5) C(4) 148.2(2) . . . . yes P(1) Pd(1) Ti(1) C(1) 100.7(1) . . . . yes P(1) Pd(1) Ti(1) C(2) 62.4(1) . . . . yes P(1) Pd(1) Ti(1) C(3) 35.6(2) . . . . yes P(1) Pd(1) Ti(1) C(4) 141.4(4) . . . . yes P(1) Pd(1) Ti(1) C(5) 135.7(1) . . . . yes P(1) Pd(1) P(2) C(12) 127.7(1) . . . . yes P(1) Pd(1) P(2) C(14) -115.2(1) . . . . yes P(1) Pd(1) P(2) C(16) 9.3(2) . . . . yes P(2) Pd(1) Ti(1) C(1) -93.3(1) . . . . yes P(2) Pd(1) Ti(1) C(2) -131.6(1) . . . . yes P(2) Pd(1) Ti(1) C(3) -158.4(2) . . . . yes P(2) Pd(1) Ti(1) C(4) -52.7(4) . . . . yes P(2) Pd(1) Ti(1) C(5) -58.4(1) . . . . yes P(2) Pd(1) P(1) C(6) 51.4(1) . . . . yes P(2) Pd(1) P(1) C(8) 171.0(1) . . . . yes P(2) Pd(1) P(1) C(10) -69.2(1) . . . . yes C(1) Ti(1) C(2) C(3) 115.8(3) . . . . yes C(1) Ti(1) C(3) C(2) -37.4(2) . . . . yes C(1) Ti(1) C(3) C(4) 78.1(2) . . . . yes C(1) Ti(1) C(4) C(3) -78.9(2) . . . . yes C(1) Ti(1) C(4) C(5) 37.9(2) . . . . yes C(1) Ti(1) C(5) C(4) -115.6(3) . . . . yes C(1) C(2) Ti(1) C(3) -115.8(3) . . . . yes C(1) C(2) Ti(1) C(4) -78.5(2) . . . . yes C(1) C(2) Ti(1) C(5) -38.0(2) . . . . yes C(1) C(2) C(3) C(4) -1.8(4) . . . . yes C(1) C(5) Ti(1) C(2) 37.7(2) . . . . yes C(1) C(5) Ti(1) C(3) 78.8(2) . . . . yes C(1) C(5) Ti(1) C(4) 115.6(3) . . . . yes C(1) C(5) C(4) C(3) -0.4(4) . . . . yes C(2) Ti(1) C(1) C(5) -114.9(3) . . . . yes C(2) Ti(1) C(3) C(4) 115.5(3) . . . . yes C(2) Ti(1) C(4) C(3) -37.4(2) . . . . yes C(2) Ti(1) C(4) C(5) 79.4(2) . . . . yes C(2) Ti(1) C(5) C(4) -77.9(2) . . . . yes C(2) C(1) Ti(1) C(3) 37.1(2) . . . . yes C(2) C(1) Ti(1) C(4) 78.1(2) . . . . yes C(2) C(1) Ti(1) C(5) 114.9(3) . . . . yes C(2) C(1) C(5) C(4) -0.7(4) . . . . yes C(2) C(3) Ti(1) C(4) -115.5(3) . . . . yes C(2) C(3) Ti(1) C(5) -79.1(2) . . . . yes C(2) C(3) C(4) C(5) 1.3(4) . . . . yes C(3) Ti(1) C(1) C(5) -77.8(2) . . . . yes C(3) Ti(1) C(4) C(5) 116.8(3) . . . . yes C(3) Ti(1) C(5) C(4) -36.8(2) . . . . yes C(3) C(2) Ti(1) C(4) 37.4(2) . . . . yes C(3) C(2) Ti(1) C(5) 77.9(2) . . . . yes C(3) C(2) C(1) C(5) 1.6(4) . . . . yes C(3) C(4) Ti(1) C(5) -116.8(3) . . . . yes C(4) Ti(1) C(1) C(5) -36.7(2) . . . . yes C(4) C(3) Ti(1) C(5) 36.3(2) . . . . yes C(6) P(1) C(8) C(9) -46.4(3) . . . . yes C(6) P(1) C(10) C(11) -177.2(3) . . . . yes C(7) C(6) P(1) C(8) -63.6(3) . . . . yes C(7) C(6) P(1) C(10) -171.2(3) . . . . yes C(8) P(1) C(10) C(11) 77.0(3) . . . . yes C(9) C(8) P(1) C(10) 61.5(3) . . . . yes C(12) P(2) C(14) C(15) -179.6(3) . . . . yes C(12) P(2) C(16) C(17) 62.8(4) . . . . yes C(13) C(12) P(2) C(14) -173.7(3) . . . . yes C(13) C(12) P(2) C(16) 77.6(4) . . . . yes C(14) P(2) C(16) C(17) -44.9(4) . . . . yes C(15) C(14) P(2) C(16) -73.8(4) . . . . yes C(15) C(14) P(2) C(16) -73.8(4) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd(1) Ti(1) 3.0137(6) . . ? Cl(1) C(5) 3.567(4) . 2_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_Ti(S)Cl2[S2Pd2(PEt3)4]-2 _database_code_CSD 180418 _audit_creation_date 'Wed Feb 13 13:57:44 2002' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C25 H62 Cl4 P4 Pd2 S3 Ti ' _chemical_formula_moiety 'C25 H62 Cl4 P4 Pd2 S3 Ti ' _chemical_formula_weight 985.35 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.305(3) _cell_length_b 20.642(7) _cell_length_c 19.845(7) _cell_angle_alpha 90 _cell_angle_beta 93.913(4) _cell_angle_gamma 90 _cell_volume 4211(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15594 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.601 _exptl_absorpt_correction_type 'REQABA Empirical Absorption Correction' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.726 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 33890 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9949 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 0 _reflns_number_gt 7776 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0700 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 9626 _refine_ls_number_parameters 414 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.94 _refine_diff_density_min -0.86 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ti' 'Ti' 0.278 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Pd' 'Pd' -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 1.12213(2) 0.18317(1) 0.30591(1) 0.01621(6) Uani 1.00 d . . . Pd(2) Pd 0.91988(2) 0.05811(1) 0.29604(1) 0.01440(5) Uani 1.00 d . . . Ti(1) Ti 1.22692(5) 0.04156(2) 0.29428(3) 0.0170(1) Uani 1.00 d . . . Cl(1) Cl 1.23594(8) -0.02986(4) 0.20147(4) 0.0297(2) Uani 1.00 d . . . Cl(2) Cl 1.26155(8) -0.04347(4) 0.37193(4) 0.0286(2) Uani 1.00 d . . . Cl(3) Cl 0.3084(1) 0.09314(7) 0.02672(6) 0.0748(4) Uani 1.00 d . . . Cl(4) Cl 0.0273(1) 0.10138(6) 0.01490(6) 0.0602(4) Uani 1.00 d . . . S(1) S 1.39687(8) 0.09939(4) 0.29771(5) 0.0323(2) Uani 1.00 d . . . S(2) S 1.06650(7) 0.10389(3) 0.22423(4) 0.0169(2) Uani 1.00 d . . . S(3) S 1.08592(7) 0.09285(3) 0.37478(4) 0.0166(2) Uani 1.00 d . . . P(1) P 1.16486(8) 0.25992(4) 0.22557(4) 0.0241(2) Uani 1.00 d . . . P(2) P 1.13719(8) 0.24664(4) 0.40140(4) 0.0217(2) Uani 1.00 d . . . P(3) P 0.78933(7) 0.03242(4) 0.20125(4) 0.0194(2) Uani 1.00 d . . . P(4) P 0.81421(7) 0.01486(4) 0.38475(4) 0.0177(2) Uani 1.00 d . . . C(1) C 1.0382(4) 0.3210(2) 0.2118(2) 0.037(1) Uani 1.00 d . . . C(2) C 0.9070(4) 0.2919(2) 0.1879(3) 0.060(1) Uani 1.00 d . . . C(3) C 1.1799(4) 0.2239(2) 0.1424(2) 0.045(1) Uani 1.00 d . . . C(4) C 1.2143(5) 0.2706(2) 0.0858(2) 0.071(1) Uani 1.00 d . . . C(5) C 1.3134(3) 0.3076(2) 0.2386(2) 0.0302(9) Uani 1.00 d . . . C(6) C 1.4365(4) 0.2672(2) 0.2431(3) 0.067(1) Uani 1.00 d . . . C(7) C 1.1873(4) 0.3314(2) 0.3984(2) 0.0319(9) Uani 1.00 d . . . C(8) C 1.1771(4) 0.3710(2) 0.4626(2) 0.043(1) Uani 1.00 d . . . C(9) C 1.2411(3) 0.2135(2) 0.4706(2) 0.0317(9) Uani 1.00 d . . . C(10) C 1.3845(4) 0.2134(2) 0.4575(2) 0.048(1) Uani 1.00 d . . . C(11) C 0.9780(3) 0.2501(2) 0.4368(2) 0.0336(10) Uani 1.00 d . . . C(12) C 0.8743(4) 0.2823(2) 0.3899(2) 0.052(1) Uani 1.00 d . . . C(13) C 0.7892(3) 0.0766(2) 0.4479(2) 0.0275(9) Uani 1.00 d . . . C(14) C 0.6963(4) 0.1289(2) 0.4222(2) 0.047(1) Uani 1.00 d . . . C(15) C 0.9191(3) -0.0448(2) 0.4289(2) 0.0241(8) Uani 1.00 d . . . C(16) C 0.9343(4) -0.1074(2) 0.3896(2) 0.036(1) Uani 1.00 d . . . C(17) C 0.6562(3) -0.0255(2) 0.3747(2) 0.0233(8) Uani 1.00 d . . . C(18) C 0.6073(3) -0.0542(2) 0.4392(2) 0.038(1) Uani 1.00 d . . . C(19) C 0.6303(3) -0.0063(2) 0.2047(2) 0.0272(9) Uani 1.00 d . . . C(20) C 0.5573(4) -0.0177(2) 0.1368(2) 0.044(1) Uani 1.00 d . . . C(21) C 0.8762(3) -0.0207(2) 0.1460(2) 0.0268(9) Uani 1.00 d . . . C(22) C 0.9013(4) -0.0877(2) 0.1750(2) 0.040(1) Uani 1.00 d . . . C(23) C 0.7543(3) 0.1038(2) 0.1489(2) 0.0295(9) Uani 1.00 d . . . C(24) C 0.6693(4) 0.1531(2) 0.1814(2) 0.051(1) Uani 1.00 d . . . C(25) C 0.1628(4) 0.0629(2) 0.0542(2) 0.047(1) Uani 1.00 d . . . H(1) H 1.0283(4) 0.3436(2) 0.2540(2) 0.044(1) Uiso 1.00 calc . . . H(2) H 1.0641(4) 0.3516(2) 0.1781(2) 0.044(1) Uiso 1.00 calc . . . H(3) H 0.8417(4) 0.3255(2) 0.1814(3) 0.070(2) Uiso 1.00 calc . . . H(4) H 0.9161(4) 0.2695(2) 0.1455(3) 0.070(2) Uiso 1.00 calc . . . H(5) H 0.8806(4) 0.2612(2) 0.2214(3) 0.070(2) Uiso 1.00 calc . . . H(6) H 1.2481(4) 0.1916(2) 0.1468(2) 0.048(2) Uiso 1.00 calc . . . H(7) H 1.0979(4) 0.2032(2) 0.1286(2) 0.048(2) Uiso 1.00 calc . . . H(8) H 1.2959(5) 0.2922(2) 0.0987(2) 0.073(2) Uiso 1.00 calc . . . H(9) H 1.2222(5) 0.2470(2) 0.0441(2) 0.073(2) Uiso 1.00 calc . . . H(10) H 1.1456(5) 0.3026(2) 0.0794(2) 0.073(2) Uiso 1.00 calc . . . H(11) H 1.3173(3) 0.3379(2) 0.2014(2) 0.035(1) Uiso 1.00 calc . . . H(12) H 1.3099(3) 0.3314(2) 0.2806(2) 0.035(1) Uiso 1.00 calc . . . H(13) H 1.4341(4) 0.2367(2) 0.2802(3) 0.069(2) Uiso 1.00 calc . . . H(14) H 1.4421(4) 0.2436(2) 0.2011(3) 0.069(2) Uiso 1.00 calc . . . H(15) H 1.5118(4) 0.2951(2) 0.2505(3) 0.069(2) Uiso 1.00 calc . . . H(16) H 1.2776(4) 0.3322(2) 0.3875(2) 0.037(1) Uiso 1.00 calc . . . H(17) H 1.1340(4) 0.3525(2) 0.3627(2) 0.037(1) Uiso 1.00 calc . . . H(18) H 1.2300(4) 0.3511(2) 0.4993(2) 0.048(2) Uiso 1.00 calc . . . H(19) H 1.2076(4) 0.4147(2) 0.4555(2) 0.048(1) Uiso 1.00 calc . . . H(20) H 1.0871(4) 0.3722(2) 0.4740(2) 0.048(2) Uiso 1.00 calc . . . H(21) H 1.2300(3) 0.2392(2) 0.5108(2) 0.036(1) Uiso 1.00 calc . . . H(22) H 1.2144(3) 0.1692(2) 0.4785(2) 0.036(1) Uiso 1.00 calc . . . H(23) H 1.4351(4) 0.1948(2) 0.4957(2) 0.057(2) Uiso 1.00 calc . . . H(24) H 1.3967(4) 0.1881(2) 0.4173(2) 0.057(2) Uiso 1.00 calc . . . H(25) H 1.4128(4) 0.2576(2) 0.4505(2) 0.057(2) Uiso 1.00 calc . . . H(26) H 0.9500(3) 0.2062(2) 0.4458(2) 0.040(1) Uiso 1.00 calc . . . H(27) H 0.9860(3) 0.2744(2) 0.4787(2) 0.040(1) Uiso 1.00 calc . . . H(28) H 0.9011(4) 0.3263(2) 0.3808(2) 0.061(2) Uiso 1.00 calc . . . H(29) H 0.8651(4) 0.2581(2) 0.3479(2) 0.061(2) Uiso 1.00 calc . . . H(30) H 0.7916(4) 0.2830(2) 0.4105(2) 0.061(2) Uiso 1.00 calc . . . H(31) H 0.7542(3) 0.0562(2) 0.4868(2) 0.032(1) Uiso 1.00 calc . . . H(32) H 0.8724(3) 0.0964(2) 0.4614(2) 0.032(1) Uiso 1.00 calc . . . H(33) H 0.6859(4) 0.1608(2) 0.4573(2) 0.056(2) Uiso 1.00 calc . . . H(34) H 0.7307(4) 0.1497(2) 0.3834(2) 0.056(2) Uiso 1.00 calc . . . H(35) H 0.6126(4) 0.1096(2) 0.4089(2) 0.056(2) Uiso 1.00 calc . . . H(36) H 1.0045(3) -0.0258(2) 0.4380(2) 0.029(1) Uiso 1.00 calc . . . H(37) H 0.8824(3) -0.0554(2) 0.4713(2) 0.029(1) Uiso 1.00 calc . . . H(38) H 0.8495(4) -0.1270(2) 0.3800(2) 0.042(1) Uiso 1.00 calc . . . H(39) H 0.9727(4) -0.0977(2) 0.3474(2) 0.042(1) Uiso 1.00 calc . . . H(40) H 0.9901(4) -0.1373(2) 0.4158(2) 0.042(1) Uiso 1.00 calc . . . H(41) H 0.5927(3) 0.0057(2) 0.3566(2) 0.028(1) Uiso 1.00 calc . . . H(42) H 0.6629(3) -0.0608(2) 0.3428(2) 0.028(1) Uiso 1.00 calc . . . H(43) H 0.5983(3) -0.0195(2) 0.4715(2) 0.044(1) Uiso 1.00 calc . . . H(44) H 0.5237(3) -0.0750(2) 0.4296(2) 0.044(1) Uiso 1.00 calc . . . H(45) H 0.6695(3) -0.0858(2) 0.4580(2) 0.043(1) Uiso 1.00 calc . . . H(46) H 0.6431(3) -0.0478(2) 0.2271(2) 0.032(1) Uiso 1.00 calc . . . H(47) H 0.5767(3) 0.0212(2) 0.2311(2) 0.032(1) Uiso 1.00 calc . . . H(48) H 0.5443(4) 0.0233(2) 0.1135(2) 0.050(2) Uiso 1.00 calc . . . H(49) H 0.6084(4) -0.0462(2) 0.1102(2) 0.050(2) Uiso 1.00 calc . . . H(50) H 0.4736(4) -0.0376(2) 0.1429(2) 0.050(2) Uiso 1.00 calc . . . H(51) H 0.8245(3) -0.0249(2) 0.1035(2) 0.031(1) Uiso 1.00 calc . . . H(52) H 0.9591(3) -0.0009(2) 0.1380(2) 0.031(1) Uiso 1.00 calc . . . H(53) H 0.8189(4) -0.1083(2) 0.1826(2) 0.048(1) Uiso 1.00 calc . . . H(54) H 0.9476(4) -0.1134(2) 0.1436(2) 0.048(1) Uiso 1.00 calc . . . H(55) H 0.9531(4) -0.0842(2) 0.2175(2) 0.047(1) Uiso 1.00 calc . . . H(56) H 0.8360(3) 0.1244(2) 0.1400(2) 0.035(1) Uiso 1.00 calc . . . H(57) H 0.7099(3) 0.0901(2) 0.1066(2) 0.035(1) Uiso 1.00 calc . . . H(58) H 0.7133(4) 0.1676(2) 0.2235(2) 0.060(2) Uiso 1.00 calc . . . H(59) H 0.6532(4) 0.1899(2) 0.1517(2) 0.060(2) Uiso 1.00 calc . . . H(60) H 0.5872(4) 0.1330(2) 0.1906(2) 0.060(2) Uiso 1.00 calc . . . H(61) H 0.1574(4) 0.0170(2) 0.0442(2) 0.055(2) Uiso 1.00 calc . . . H(62) H 0.1624(4) 0.0693(2) 0.1026(2) 0.055(2) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0208(1) 0.0120(1) 0.0146(1) -0.00030(9) 0.00176(8) 0.00049(9) Pd(2) 0.0162(1) 0.0146(1) 0.0121(1) 0.00012(9) 0.00192(8) 0.00064(9) Ti(1) 0.0181(3) 0.0140(3) 0.0186(3) 0.0007(2) 0.0034(2) 0.0005(2) Cl(1) 0.0397(5) 0.0207(4) 0.0253(4) 0.0056(3) 0.0062(4) -0.0042(3) Cl(2) 0.0356(5) 0.0223(4) 0.0261(4) 0.0085(3) 0.0036(3) 0.0063(3) Cl(3) 0.0569(7) 0.104(1) 0.0529(7) 0.0041(7) 0.0210(6) 0.0043(7) Cl(4) 0.0624(7) 0.0713(8) 0.0435(6) 0.0166(6) 0.0016(5) -0.0039(6) S(1) 0.0211(4) 0.0249(4) 0.0455(6) -0.0038(4) 0.0053(4) -0.0007(3) S(2) 0.0207(4) 0.0153(4) 0.0141(3) -0.0012(3) 0.0035(3) 0.0004(3) S(3) 0.0194(4) 0.0154(4) 0.0145(4) -0.0003(3) 0.0014(3) 0.0010(3) P(1) 0.0332(5) 0.0156(4) 0.0198(4) -0.0030(3) 0.0034(3) 0.0026(3) P(2) 0.0286(4) 0.0161(4) 0.0183(4) -0.0005(3) 0.0006(3) -0.0018(3) P(3) 0.0186(4) 0.0240(4) 0.0145(4) 0.0002(3) 0.0008(3) -0.0002(3) P(4) 0.0178(4) 0.0199(4) 0.0149(4) 0.0001(3) 0.0023(3) 0.0021(3) C(1) 0.040(2) 0.028(2) 0.041(2) -0.002(2) -0.003(2) 0.013(2) C(2) 0.047(3) 0.053(3) 0.075(3) -0.001(3) -0.018(2) 0.024(2) C(3) 0.067(3) 0.030(2) 0.023(2) -0.018(2) 0.009(2) 0.001(2) C(4) 0.113(4) 0.044(3) 0.025(2) -0.026(2) 0.016(2) 0.005(3) C(5) 0.038(2) 0.018(2) 0.031(2) -0.005(1) 0.011(2) 0.001(1) C(6) 0.036(2) 0.028(2) 0.107(4) -0.001(2) 0.010(2) 0.014(2) C(7) 0.043(2) 0.021(2) 0.027(2) -0.004(1) -0.002(2) -0.002(1) C(8) 0.060(3) 0.025(2) 0.034(2) -0.006(2) -0.002(2) -0.009(2) C(9) 0.044(2) 0.023(2) 0.024(2) -0.003(1) -0.007(2) -0.001(2) C(10) 0.037(2) 0.056(3) 0.049(3) 0.005(2) -0.010(2) -0.004(2) C(11) 0.037(2) 0.029(2) 0.035(2) 0.000(2) 0.010(2) -0.007(2) C(12) 0.034(2) 0.056(3) 0.062(3) 0.010(2) 0.004(2) -0.006(2) C(13) 0.026(2) 0.034(2) 0.020(2) -0.004(1) 0.006(1) -0.006(1) C(14) 0.043(2) 0.048(2) 0.049(3) 0.017(2) -0.007(2) -0.024(2) C(15) 0.021(2) 0.028(2) 0.023(2) -0.002(1) 0.001(1) 0.008(1) C(16) 0.034(2) 0.027(2) 0.044(2) 0.005(2) -0.003(2) 0.007(2) C(17) 0.020(2) 0.027(2) 0.022(2) 0.000(1) -0.001(1) 0.004(1) C(18) 0.024(2) 0.049(2) 0.036(2) -0.008(2) 0.004(2) 0.013(2) C(19) 0.024(2) 0.033(2) 0.023(2) -0.001(1) 0.004(1) -0.003(1) C(20) 0.030(2) 0.061(3) 0.034(2) -0.011(2) -0.003(2) -0.004(2) C(21) 0.022(2) 0.035(2) 0.021(2) 0.001(1) 0.004(1) -0.009(1) C(22) 0.037(2) 0.033(2) 0.049(2) 0.004(2) 0.008(2) -0.012(2) C(23) 0.026(2) 0.036(2) 0.026(2) 0.000(2) -0.003(1) 0.009(1) C(24) 0.044(2) 0.038(2) 0.068(3) 0.014(2) 0.018(2) 0.016(2) C(25) 0.061(3) 0.042(2) 0.035(2) 0.009(2) 0.012(2) 0.004(2) #------------------------------------------------------------------------------ _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ORTEP-3 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(2) 2.3468(7) . . yes Pd(1) S(3) 2.3564(7) . . yes Pd(1) P(1) 2.3112(8) . . yes Pd(1) P(2) 2.3003(8) . . yes Pd(2) S(2) 2.3454(9) . . yes Pd(2) S(3) 2.3492(8) . . yes Pd(2) P(3) 2.2988(8) . . yes Pd(2) P(4) 2.3117(8) . . yes Ti(1) Cl(1) 2.366(1) . . yes Ti(1) Cl(2) 2.3468(9) . . yes Ti(1) S(1) 2.117(1) . . yes Ti(1) S(2) 2.4509(9) . . yes Ti(1) S(3) 2.470(1) . . yes Cl(3) C(25) 1.747(4) . . yes Cl(4) C(25) 1.744(4) . . yes P(1) C(1) 1.822(4) . . yes P(1) C(3) 1.827(4) . . yes P(1) C(5) 1.824(3) . . yes P(2) C(7) 1.827(3) . . yes P(2) C(9) 1.817(3) . . yes P(2) C(11) 1.829(4) . . yes P(3) C(19) 1.828(3) . . yes P(3) C(21) 1.827(3) . . yes P(3) C(23) 1.825(4) . . yes P(4) C(13) 1.818(3) . . yes P(4) C(15) 1.823(3) . . yes P(4) C(17) 1.828(3) . . yes C(1) C(2) 1.526(6) . . yes C(3) C(4) 1.539(6) . . yes C(5) C(6) 1.516(5) . . yes C(7) C(8) 1.522(5) . . yes C(9) C(10) 1.518(5) . . yes C(11) C(12) 1.521(5) . . yes C(13) C(14) 1.508(5) . . yes C(15) C(16) 1.523(5) . . yes C(17) C(18) 1.527(5) . . yes C(19) C(20) 1.517(5) . . yes C(21) C(22) 1.513(5) . . yes C(23) C(24) 1.515(6) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(2) Pd(1) S(3) 78.93(3) . . . yes S(2) Pd(1) P(1) 92.90(3) . . . yes S(2) Pd(1) P(2) 164.96(3) . . . yes S(3) Pd(1) P(1) 170.98(3) . . . yes S(3) Pd(1) P(2) 88.70(3) . . . yes P(1) Pd(1) P(2) 99.94(3) . . . yes S(2) Pd(2) S(3) 79.11(3) . . . yes S(2) Pd(2) P(3) 87.77(3) . . . yes S(2) Pd(2) P(4) 167.12(3) . . . yes S(3) Pd(2) P(3) 166.84(3) . . . yes S(3) Pd(2) P(4) 88.33(3) . . . yes P(3) Pd(2) P(4) 104.73(3) . . . yes Cl(1) Ti(1) Cl(2) 91.88(3) . . . yes Cl(1) Ti(1) S(1) 107.46(4) . . . yes Cl(1) Ti(1) S(2) 86.92(3) . . . yes Cl(1) Ti(1) S(3) 145.76(4) . . . yes Cl(2) Ti(1) S(1) 108.19(4) . . . yes Cl(2) Ti(1) S(2) 146.25(4) . . . yes Cl(2) Ti(1) S(3) 88.03(3) . . . yes S(1) Ti(1) S(2) 104.29(4) . . . yes S(1) Ti(1) S(3) 105.04(4) . . . yes S(2) Ti(1) S(3) 74.82(3) . . . yes Pd(1) S(2) Pd(2) 89.91(3) . . . yes Pd(1) S(2) Ti(1) 81.42(3) . . . yes Pd(2) S(2) Ti(1) 83.19(3) . . . yes Pd(1) S(3) Pd(2) 89.58(3) . . . yes Pd(1) S(3) Ti(1) 80.83(3) . . . yes Pd(2) S(3) Ti(1) 82.70(3) . . . yes Pd(1) P(1) C(1) 114.2(1) . . . yes Pd(1) P(1) C(3) 112.1(1) . . . yes Pd(1) P(1) C(5) 118.1(1) . . . yes C(1) P(1) C(3) 104.5(2) . . . yes C(1) P(1) C(5) 103.5(2) . . . yes C(3) P(1) C(5) 103.0(2) . . . yes Pd(1) P(2) C(7) 121.5(1) . . . yes Pd(1) P(2) C(9) 114.3(1) . . . yes Pd(1) P(2) C(11) 109.0(1) . . . yes C(7) P(2) C(9) 103.4(2) . . . yes C(7) P(2) C(11) 103.8(2) . . . yes C(9) P(2) C(11) 102.8(2) . . . yes Pd(2) P(3) C(19) 123.1(1) . . . yes Pd(2) P(3) C(21) 110.3(1) . . . yes Pd(2) P(3) C(23) 111.2(1) . . . yes C(19) P(3) C(21) 103.7(2) . . . yes C(19) P(3) C(23) 103.4(2) . . . yes C(21) P(3) C(23) 103.2(2) . . . yes Pd(2) P(4) C(13) 110.5(1) . . . yes Pd(2) P(4) C(15) 109.4(1) . . . yes Pd(2) P(4) C(17) 123.7(1) . . . yes C(13) P(4) C(15) 104.4(1) . . . yes C(13) P(4) C(17) 103.2(1) . . . yes C(15) P(4) C(17) 103.8(1) . . . yes P(1) C(1) C(2) 112.6(3) . . . yes P(1) C(3) C(4) 116.3(3) . . . yes P(1) C(5) C(6) 113.7(2) . . . yes P(2) C(7) C(8) 116.8(3) . . . yes P(2) C(9) C(10) 113.6(3) . . . yes P(2) C(11) C(12) 113.2(3) . . . yes P(4) C(13) C(14) 112.6(2) . . . yes P(4) C(15) C(16) 113.9(2) . . . yes P(4) C(17) C(18) 115.4(2) . . . yes P(3) C(19) C(20) 115.2(2) . . . yes P(3) C(21) C(22) 113.4(2) . . . yes P(3) C(23) C(24) 113.4(3) . . . yes Cl(3) C(25) Cl(4) 112.1(2) . . . yes #------------------------------------------------------------------------------ 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 Pd(1) S(2) Pd(2) S(3) -34.93(2) . . . . yes Pd(1) S(2) Pd(2) P(3) 145.93(3) . . . . yes Pd(1) S(2) Pd(2) P(4) -47.8(1) . . . . yes Pd(1) S(2) Ti(1) Cl(1) -162.85(3) . . . . yes Pd(1) S(2) Ti(1) Cl(2) 108.36(6) . . . . yes Pd(1) S(2) Ti(1) S(1) -55.61(4) . . . . yes Pd(1) S(2) Ti(1) S(3) 46.41(2) . . . . yes Pd(1) S(3) Pd(2) S(2) 34.76(2) . . . . yes Pd(1) S(3) Pd(2) P(3) 38.5(1) . . . . yes Pd(1) S(3) Pd(2) P(4) -148.09(3) . . . . yes Pd(1) S(3) Ti(1) Cl(1) -106.43(6) . . . . yes Pd(1) S(3) Ti(1) Cl(2) 163.12(3) . . . . yes Pd(1) S(3) Ti(1) S(1) 54.80(4) . . . . yes Pd(1) S(3) Ti(1) S(2) -46.26(2) . . . . yes Pd(1) P(1) C(1) C(2) -60.1(3) . . . . yes Pd(1) P(1) C(3) C(4) -177.4(3) . . . . yes Pd(1) P(1) C(5) C(6) 59.5(3) . . . . yes Pd(1) P(2) C(7) C(8) 172.4(2) . . . . yes Pd(1) P(2) C(9) C(10) 69.4(3) . . . . yes Pd(1) P(2) C(11) C(12) -63.5(3) . . . . yes Pd(2) S(2) Pd(1) S(3) 34.83(2) . . . . yes Pd(2) S(2) Pd(1) P(1) -149.04(3) . . . . yes Pd(2) S(2) Pd(1) P(2) -0.4(1) . . . . yes Pd(2) S(2) Ti(1) Cl(1) 106.21(3) . . . . yes Pd(2) S(2) Ti(1) Cl(2) 17.42(7) . . . . yes Pd(2) S(2) Ti(1) S(1) -146.55(4) . . . . yes Pd(2) S(2) Ti(1) S(3) -44.53(2) . . . . yes Pd(2) S(3) Pd(1) S(2) -34.76(2) . . . . yes Pd(2) S(3) Pd(1) P(1) -60.2(2) . . . . yes Pd(2) S(3) Pd(1) P(2) 136.63(3) . . . . yes Pd(2) S(3) Ti(1) Cl(1) -15.67(6) . . . . yes Pd(2) S(3) Ti(1) Cl(2) -106.13(3) . . . . yes Pd(2) S(3) Ti(1) S(1) 145.56(3) . . . . yes Pd(2) S(3) Ti(1) S(2) 44.50(2) . . . . yes Pd(2) P(3) C(19) C(20) 178.5(2) . . . . yes Pd(2) P(3) C(21) C(22) 68.6(2) . . . . yes Pd(2) P(3) C(23) C(24) -67.7(3) . . . . yes Pd(2) P(4) C(13) C(14) 66.3(3) . . . . yes Pd(2) P(4) C(15) C(16) -71.9(2) . . . . yes Pd(2) P(4) C(17) C(18) 176.4(2) . . . . yes Ti(1) S(2) Pd(1) S(3) -48.30(3) . . . . yes Ti(1) S(2) Pd(1) P(1) 127.84(3) . . . . yes Ti(1) S(2) Pd(1) P(2) -83.5(1) . . . . yes Ti(1) S(2) Pd(2) S(3) 46.44(2) . . . . yes Ti(1) S(2) Pd(2) P(3) -132.70(3) . . . . yes Ti(1) S(2) Pd(2) P(4) 33.5(1) . . . . yes Ti(1) S(3) Pd(1) S(2) 47.90(3) . . . . yes Ti(1) S(3) Pd(1) P(1) 22.5(2) . . . . yes Ti(1) S(3) Pd(1) P(2) -140.70(3) . . . . yes Ti(1) S(3) Pd(2) S(2) -46.04(2) . . . . yes Ti(1) S(3) Pd(2) P(3) -42.3(1) . . . . yes Ti(1) S(3) Pd(2) P(4) 131.10(3) . . . . yes S(2) Pd(1) P(1) C(1) 104.0(1) . . . . yes S(2) Pd(1) P(1) C(3) -14.6(1) . . . . yes S(2) Pd(1) P(1) C(5) -134.1(1) . . . . yes S(2) Pd(1) P(2) C(7) -153.2(2) . . . . yes S(2) Pd(1) P(2) C(9) 81.7(2) . . . . yes S(2) Pd(1) P(2) C(11) -32.8(2) . . . . yes S(2) Pd(2) P(3) C(19) -177.4(1) . . . . yes S(2) Pd(2) P(3) C(21) 59.8(1) . . . . yes S(2) Pd(2) P(3) C(23) -54.1(1) . . . . yes S(2) Pd(2) P(4) C(13) 68.1(2) . . . . yes S(2) Pd(2) P(4) C(15) -46.4(2) . . . . yes S(2) Pd(2) P(4) C(17) -169.0(2) . . . . yes S(3) Pd(1) P(1) C(1) 128.9(2) . . . . yes S(3) Pd(1) P(1) C(3) 10.3(3) . . . . yes S(3) Pd(1) P(1) C(5) -109.2(2) . . . . yes S(3) Pd(1) P(2) C(7) 172.3(1) . . . . yes S(3) Pd(1) P(2) C(9) 47.2(1) . . . . yes S(3) Pd(1) P(2) C(11) -67.2(1) . . . . yes S(3) Pd(2) P(3) C(19) 178.9(2) . . . . yes S(3) Pd(2) P(3) C(21) 56.1(2) . . . . yes S(3) Pd(2) P(3) C(23) -57.8(2) . . . . yes S(3) Pd(2) P(4) C(13) 55.4(1) . . . . yes S(3) Pd(2) P(4) C(15) -59.1(1) . . . . yes S(3) Pd(2) P(4) C(17) 178.3(1) . . . . yes P(1) Pd(1) P(2) C(7) -5.0(1) . . . . yes P(1) Pd(1) P(2) C(9) -130.1(1) . . . . yes P(1) Pd(1) P(2) C(11) 115.4(1) . . . . yes P(2) Pd(1) P(1) C(1) -68.2(1) . . . . yes P(2) Pd(1) P(1) C(3) 173.3(1) . . . . yes P(2) Pd(1) P(1) C(5) 53.8(1) . . . . yes P(3) Pd(2) P(4) C(13) -126.1(1) . . . . yes P(3) Pd(2) P(4) C(15) 119.4(1) . . . . yes P(3) Pd(2) P(4) C(17) -3.3(1) . . . . yes P(4) Pd(2) P(3) C(19) 5.8(1) . . . . yes P(4) Pd(2) P(3) C(21) -117.1(1) . . . . yes P(4) Pd(2) P(3) C(23) 129.1(1) . . . . yes C(1) P(1) C(3) C(4) 58.4(4) . . . . yes C(1) P(1) C(5) C(6) -173.2(3) . . . . yes C(2) C(1) P(1) C(3) 62.8(3) . . . . yes C(2) C(1) P(1) C(5) 170.3(3) . . . . yes C(3) P(1) C(5) C(6) -64.6(3) . . . . yes C(4) C(3) P(1) C(5) -49.5(4) . . . . yes C(7) P(2) C(9) C(10) -64.8(3) . . . . yes C(7) P(2) C(11) C(12) 67.3(3) . . . . yes C(8) C(7) P(2) C(9) -57.7(3) . . . . yes C(8) C(7) P(2) C(11) 49.4(3) . . . . yes C(9) P(2) C(11) C(12) 174.9(3) . . . . yes C(10) C(9) P(2) C(11) -172.6(3) . . . . yes C(13) P(4) C(15) C(16) 169.8(2) . . . . yes C(13) P(4) C(17) C(18) -57.5(3) . . . . yes C(14) C(13) P(4) C(15) -176.1(2) . . . . yes C(14) C(13) P(4) C(17) -67.9(3) . . . . yes C(15) P(4) C(17) C(18) 51.3(3) . . . . yes C(16) C(15) P(4) C(17) 62.0(3) . . . . yes C(19) P(3) C(21) C(22) -64.9(3) . . . . yes C(19) P(3) C(23) C(24) 66.2(3) . . . . yes C(20) C(19) P(3) C(21) -55.8(3) . . . . yes C(20) C(19) P(3) C(23) 51.7(3) . . . . yes C(21) P(3) C(23) C(24) 174.1(3) . . . . yes C(22) C(21) P(3) C(23) -172.5(2) . . . . yes C(22) C(21) P(3) C(23) -172.5(2) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(25) 3.532(4) . 1_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------