# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'I L Odinets' 'D.V. Aleksanyan' 'E.I. Gutsul' 'Vladimir A Kozlov' 'Konstantin Lyssenko' 'Yulia V Nelyubina' 'P V Petrovskii' "A.A. Vasil'ev" _publ_contact_author_name 'I L Odinets' _publ_contact_author_email ODINETS@INEOS.AC.RU _publ_section_title ; 5,6-Membered Palladium Pincer Complexes of 1-Thiophosphoryloxy-3-Thiophosphorylbenzenes. Synthesis, X-ray structure, and Catalytic activity ; # Attachment '3b.CIF' data_a _database_code_depnum_ccdc_archive 'CCDC 730242' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 N2 O P2 S2' _chemical_formula_sum 'C26 H34 N2 O P2 S2' _chemical_formula_weight 516.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1250(16) _cell_length_b 11.081(3) _cell_length_c 14.998(3) _cell_angle_alpha 83.718(16) _cell_angle_beta 78.009(16) _cell_angle_gamma 66.27(2) _cell_volume 1357.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 658 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15045 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7182 _reflns_number_gt 4787 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0500P)^2^+0.5700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7182 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.05492(7) 0.67106(5) 0.14400(4) 0.02313(13) Uani 1 1 d . . . S1 S -0.13067(7) 0.53009(5) 0.18292(4) 0.02917(14) Uani 1 1 d . . . P2 P 0.45374(6) 0.28461(5) 0.30673(4) 0.02210(13) Uani 1 1 d . . . S2 S 0.67996(7) 0.17016(6) 0.31284(4) 0.03038(15) Uani 1 1 d . . . O1 O 0.12318(18) 0.61996(14) 0.07808(10) 0.0259(3) Uani 1 1 d . . . N1 N -0.0395(2) 0.74295(17) 0.22933(12) 0.0243(4) Uani 1 1 d . . . N2 N -0.1479(2) 0.78953(18) 0.07493(12) 0.0257(4) Uani 1 1 d . . . C1 C 0.2535(3) 0.5048(2) 0.09417(14) 0.0229(4) Uani 1 1 d . . . C2 C 0.2851(2) 0.4633(2) 0.18146(14) 0.0228(4) Uani 1 1 d . . . H2A H 0.2148 0.5118 0.2329 0.027 Uiso 1 1 calc R . . C3 C 0.4216(2) 0.3495(2) 0.19266(14) 0.0224(4) Uani 1 1 d . . . C4 C 0.5287(3) 0.2811(2) 0.11739(15) 0.0255(5) Uani 1 1 d . . . H4A H 0.6235 0.2053 0.1251 0.031 Uiso 1 1 calc R . . C5 C 0.4944(3) 0.3258(2) 0.03058(15) 0.0287(5) Uani 1 1 d . . . H5A H 0.5669 0.2797 -0.0212 0.034 Uiso 1 1 calc R . . C6 C 0.3563(3) 0.4363(2) 0.01843(15) 0.0256(5) Uani 1 1 d . . . H6A H 0.3326 0.4646 -0.0410 0.031 Uiso 1 1 calc R . . C7 C -0.0991(3) 0.7162(2) 0.32543(15) 0.0324(5) Uani 1 1 d . . . H7A H -0.0327 0.7309 0.3643 0.039 Uiso 1 1 calc R . . H7B H -0.0851 0.6226 0.3333 0.039 Uiso 1 1 calc R . . C8 C -0.2775(3) 0.8034(2) 0.35681(18) 0.0415(6) Uani 1 1 d . . . H8A H -0.3110 0.7833 0.4212 0.062 Uiso 1 1 calc R . . H8B H -0.3443 0.7867 0.3201 0.062 Uiso 1 1 calc R . . H8C H -0.2921 0.8963 0.3493 0.062 Uiso 1 1 calc R . . C9 C 0.0247(3) 0.8480(2) 0.21141(17) 0.0303(5) Uani 1 1 d . . . H9A H -0.0497 0.9245 0.2490 0.036 Uiso 1 1 calc R . . H9B H 0.0259 0.8772 0.1466 0.036 Uiso 1 1 calc R . . C10 C 0.1945(3) 0.8056(2) 0.23175(19) 0.0382(6) Uani 1 1 d . . . H10A H 0.2298 0.8793 0.2183 0.057 Uiso 1 1 calc R . . H10B H 0.2696 0.7310 0.1938 0.057 Uiso 1 1 calc R . . H10C H 0.1939 0.7789 0.2963 0.057 Uiso 1 1 calc R . . C11 C -0.2862(3) 0.9102(2) 0.10949(17) 0.0307(5) Uani 1 1 d . . . H11A H -0.2866 0.9840 0.0658 0.037 Uiso 1 1 calc R . . H11B H -0.2690 0.9312 0.1680 0.037 Uiso 1 1 calc R . . C12 C -0.4521(3) 0.9029(3) 0.1245(2) 0.0460(7) Uani 1 1 d . . . H12A H -0.5357 0.9857 0.1498 0.069 Uiso 1 1 calc R . . H12B H -0.4534 0.8296 0.1672 0.069 Uiso 1 1 calc R . . H12C H -0.4744 0.8886 0.0662 0.069 Uiso 1 1 calc R . . C13 C -0.1260(3) 0.7660(2) -0.02277(15) 0.0302(5) Uani 1 1 d . . . H13A H -0.2339 0.7965 -0.0409 0.036 Uiso 1 1 calc R . . H13B H -0.0694 0.6703 -0.0334 0.036 Uiso 1 1 calc R . . C14 C -0.0277(4) 0.8383(3) -0.08090(19) 0.0522(8) Uani 1 1 d . . . H14A H -0.0178 0.8233 -0.1455 0.078 Uiso 1 1 calc R . . H14B H 0.0809 0.8052 -0.0650 0.078 Uiso 1 1 calc R . . H14C H -0.0828 0.9329 -0.0697 0.078 Uiso 1 1 calc R . . C15 C 0.3164(3) 0.1999(2) 0.34228(14) 0.0227(4) Uani 1 1 d . . . C16 C 0.1719(3) 0.2377(2) 0.30901(15) 0.0290(5) Uani 1 1 d . . . H16A H 0.1425 0.3104 0.2670 0.035 Uiso 1 1 calc R . . C17 C 0.0708(3) 0.1693(3) 0.33718(16) 0.0344(6) Uani 1 1 d . . . H17A H -0.0279 0.1958 0.3146 0.041 Uiso 1 1 calc R . . C18 C 0.1130(3) 0.0633(3) 0.39765(16) 0.0364(6) Uani 1 1 d . . . H18A H 0.0449 0.0156 0.4156 0.044 Uiso 1 1 calc R . . C19 C 0.2544(3) 0.0264(2) 0.43220(17) 0.0371(6) Uani 1 1 d . . . H19A H 0.2819 -0.0453 0.4751 0.045 Uiso 1 1 calc R . . C20 C 0.3563(3) 0.0937(2) 0.40455(16) 0.0292(5) Uani 1 1 d . . . H20A H 0.4539 0.0673 0.4282 0.035 Uiso 1 1 calc R . . C21 C 0.3773(2) 0.4284(2) 0.37694(14) 0.0225(4) Uani 1 1 d . . . C22 C 0.4617(3) 0.5111(2) 0.36110(16) 0.0283(5) Uani 1 1 d . . . H22A H 0.5531 0.4938 0.3130 0.034 Uiso 1 1 calc R . . C23 C 0.4127(3) 0.6188(2) 0.41538(16) 0.0328(5) Uani 1 1 d . . . H23A H 0.4699 0.6756 0.4041 0.039 Uiso 1 1 calc R . . C24 C 0.2805(3) 0.6439(2) 0.48608(16) 0.0330(5) Uani 1 1 d . . . H24A H 0.2477 0.7174 0.5235 0.040 Uiso 1 1 calc R . . C25 C 0.1965(3) 0.5620(2) 0.50205(17) 0.0331(5) Uani 1 1 d . . . H25A H 0.1060 0.5791 0.5506 0.040 Uiso 1 1 calc R . . C26 C 0.2437(3) 0.4546(2) 0.44741(15) 0.0278(5) Uani 1 1 d . . . H26A H 0.1848 0.3990 0.4582 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0231(3) 0.0227(3) 0.0225(3) 0.0009(2) -0.0033(2) -0.0085(2) S1 0.0300(3) 0.0260(3) 0.0332(3) 0.0028(2) -0.0059(2) -0.0135(2) P2 0.0189(3) 0.0211(3) 0.0268(3) -0.0005(2) -0.0051(2) -0.0079(2) S2 0.0201(3) 0.0268(3) 0.0435(4) -0.0008(2) -0.0097(2) -0.0065(2) O1 0.0252(8) 0.0269(8) 0.0222(8) 0.0029(6) -0.0025(6) -0.0084(6) N1 0.0270(10) 0.0235(9) 0.0221(9) 0.0008(7) -0.0039(8) -0.0101(8) N2 0.0260(10) 0.0249(9) 0.0239(9) 0.0022(7) -0.0055(8) -0.0078(8) C1 0.0222(11) 0.0212(10) 0.0265(11) 0.0004(9) -0.0034(9) -0.0105(9) C2 0.0219(11) 0.0221(10) 0.0233(11) -0.0039(8) 0.0012(8) -0.0091(9) C3 0.0201(10) 0.0217(10) 0.0267(11) -0.0002(8) -0.0023(9) -0.0105(9) C4 0.0207(11) 0.0225(11) 0.0319(12) -0.0043(9) -0.0006(9) -0.0083(9) C5 0.0294(12) 0.0282(12) 0.0267(12) -0.0073(9) 0.0031(9) -0.0118(10) C6 0.0286(12) 0.0298(11) 0.0220(11) -0.0012(9) -0.0011(9) -0.0165(10) C7 0.0424(14) 0.0313(12) 0.0224(11) -0.0005(10) -0.0033(10) -0.0144(11) C8 0.0457(16) 0.0339(13) 0.0345(14) -0.0002(11) 0.0096(12) -0.0134(12) C9 0.0358(13) 0.0246(11) 0.0336(13) -0.0018(10) -0.0071(10) -0.0142(10) C10 0.0330(13) 0.0351(13) 0.0485(16) -0.0048(12) -0.0100(12) -0.0133(11) C11 0.0301(12) 0.0236(11) 0.0361(13) 0.0004(10) -0.0107(10) -0.0062(10) C12 0.0286(13) 0.0444(16) 0.0604(18) -0.0057(14) -0.0078(13) -0.0087(12) C13 0.0344(13) 0.0314(12) 0.0255(12) 0.0033(10) -0.0108(10) -0.0119(10) C14 0.066(2) 0.065(2) 0.0324(15) 0.0112(13) -0.0045(14) -0.0374(17) C15 0.0228(11) 0.0247(11) 0.0224(11) -0.0037(8) -0.0014(8) -0.0115(9) C16 0.0286(12) 0.0343(12) 0.0285(12) 0.0031(10) -0.0074(10) -0.0167(10) C17 0.0305(13) 0.0521(15) 0.0294(12) -0.0025(11) -0.0040(10) -0.0256(12) C18 0.0419(15) 0.0454(15) 0.0322(13) -0.0033(11) 0.0009(11) -0.0307(12) C19 0.0437(15) 0.0315(13) 0.0376(14) 0.0052(11) -0.0022(12) -0.0202(12) C20 0.0274(12) 0.0281(12) 0.0322(12) 0.0012(10) -0.0067(10) -0.0110(10) C21 0.0210(10) 0.0221(10) 0.0250(11) -0.0001(8) -0.0076(9) -0.0075(8) C22 0.0288(12) 0.0300(12) 0.0301(12) 0.0004(10) -0.0071(10) -0.0149(10) C23 0.0395(14) 0.0281(12) 0.0373(14) 0.0022(10) -0.0128(11) -0.0177(11) C24 0.0394(14) 0.0271(12) 0.0338(13) -0.0063(10) -0.0120(11) -0.0103(10) C25 0.0290(12) 0.0323(13) 0.0347(13) -0.0076(10) -0.0031(10) -0.0082(10) C26 0.0277(12) 0.0291(12) 0.0289(12) -0.0008(9) -0.0057(9) -0.0132(10) _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 P1 O1 1.6289(16) . ? P1 N1 1.6371(19) . ? P1 N2 1.6394(19) . ? P1 S1 1.9392(9) . ? P2 C15 1.815(2) . ? P2 C3 1.817(2) . ? P2 C21 1.817(2) . ? P2 S2 1.9555(9) . ? O1 C1 1.389(2) . ? N1 C7 1.474(3) . ? N1 C9 1.479(3) . ? N2 C11 1.474(3) . ? N2 C13 1.475(3) . ? C1 C6 1.386(3) . ? C1 C2 1.388(3) . ? C2 C3 1.395(3) . ? C2 H2A 0.9500 . ? C3 C4 1.392(3) . ? C4 C5 1.394(3) . ? C4 H4A 0.9500 . ? C5 C6 1.388(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.523(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.514(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.517(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.518(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.395(3) . ? C15 C16 1.395(3) . ? C16 C17 1.391(3) . ? C16 H16A 0.9500 . ? C17 C18 1.378(3) . ? C17 H17A 0.9500 . ? C18 C19 1.381(4) . ? C18 H18A 0.9500 . ? C19 C20 1.387(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.391(3) . ? C21 C22 1.392(3) . ? C22 C23 1.384(3) . ? C22 H22A 0.9500 . ? C23 C24 1.385(3) . ? C23 H23A 0.9500 . ? C24 C25 1.380(3) . ? C24 H24A 0.9500 . ? C25 C26 1.388(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 N1 106.59(9) . . ? O1 P1 N2 96.44(9) . . ? N1 P1 N2 106.44(9) . . ? O1 P1 S1 112.49(7) . . ? N1 P1 S1 112.97(7) . . ? N2 P1 S1 120.08(7) . . ? C15 P2 C3 104.77(10) . . ? C15 P2 C21 107.03(10) . . ? C3 P2 C21 105.33(10) . . ? C15 P2 S2 112.64(8) . . ? C3 P2 S2 113.61(8) . . ? C21 P2 S2 112.80(7) . . ? C1 O1 P1 124.17(13) . . ? C7 N1 C9 116.64(18) . . ? C7 N1 P1 123.27(15) . . ? C9 N1 P1 119.92(15) . . ? C11 N2 C13 115.74(18) . . ? C11 N2 P1 121.70(15) . . ? C13 N2 P1 120.73(15) . . ? C6 C1 C2 121.1(2) . . ? C6 C1 O1 116.87(19) . . ? C2 C1 O1 121.95(19) . . ? C1 C2 C3 119.11(19) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 120.7(2) . . ? C4 C3 P2 119.52(16) . . ? C2 C3 P2 119.67(16) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 121.2(2) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C1 C6 C5 119.0(2) . . ? C1 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? N1 C7 C8 112.44(19) . . ? N1 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 113.62(19) . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 115.2(2) . . ? N2 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? N2 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 111.1(2) . . ? N2 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.9(2) . . ? C20 C15 P2 119.19(17) . . ? C16 C15 P2 121.93(17) . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 120.0(2) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 120.2(2) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C15 120.4(2) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? C26 C21 C22 119.6(2) . . ? C26 C21 P2 122.57(17) . . ? C22 C21 P2 117.73(17) . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 119.9(2) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? 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 N1 P1 O1 C1 80.45(17) . . . . ? N2 P1 O1 C1 -170.23(16) . . . . ? S1 P1 O1 C1 -43.89(17) . . . . ? O1 P1 N1 C7 -132.27(17) . . . . ? N2 P1 N1 C7 125.60(17) . . . . ? S1 P1 N1 C7 -8.24(19) . . . . ? O1 P1 N1 C9 52.80(17) . . . . ? N2 P1 N1 C9 -49.32(18) . . . . ? S1 P1 N1 C9 176.84(14) . . . . ? O1 P1 N2 C11 -150.11(17) . . . . ? N1 P1 N2 C11 -40.67(19) . . . . ? S1 P1 N2 C11 89.21(17) . . . . ? O1 P1 N2 C13 45.97(18) . . . . ? N1 P1 N2 C13 155.41(16) . . . . ? S1 P1 N2 C13 -74.71(18) . . . . ? P1 O1 C1 C6 145.38(16) . . . . ? P1 O1 C1 C2 -37.9(3) . . . . ? C6 C1 C2 C3 -1.0(3) . . . . ? O1 C1 C2 C3 -177.54(18) . . . . ? C1 C2 C3 C4 2.6(3) . . . . ? C1 C2 C3 P2 -173.89(15) . . . . ? C15 P2 C3 C4 -98.42(18) . . . . ? C21 P2 C3 C4 148.86(17) . . . . ? S2 P2 C3 C4 24.92(19) . . . . ? C15 P2 C3 C2 78.14(18) . . . . ? C21 P2 C3 C2 -34.59(19) . . . . ? S2 P2 C3 C2 -158.52(15) . . . . ? C2 C3 C4 C5 -2.1(3) . . . . ? P2 C3 C4 C5 174.40(16) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? O1 C1 C6 C5 175.60(19) . . . . ? C4 C5 C6 C1 1.7(3) . . . . ? C9 N1 C7 C8 87.7(2) . . . . ? P1 N1 C7 C8 -87.3(2) . . . . ? C7 N1 C9 C10 77.3(3) . . . . ? P1 N1 C9 C10 -107.4(2) . . . . ? C13 N2 C11 C12 76.4(3) . . . . ? P1 N2 C11 C12 -88.3(2) . . . . ? C11 N2 C13 C14 85.3(3) . . . . ? P1 N2 C13 C14 -109.9(2) . . . . ? C3 P2 C15 C20 151.76(17) . . . . ? C21 P2 C15 C20 -96.73(18) . . . . ? S2 P2 C15 C20 27.79(19) . . . . ? C3 P2 C15 C16 -28.1(2) . . . . ? C21 P2 C15 C16 83.4(2) . . . . ? S2 P2 C15 C16 -152.08(16) . . . . ? C20 C15 C16 C17 -0.6(3) . . . . ? P2 C15 C16 C17 179.29(18) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C16 C17 C18 C19 1.5(4) . . . . ? C17 C18 C19 C20 -1.6(4) . . . . ? C18 C19 C20 C15 0.6(4) . . . . ? C16 C15 C20 C19 0.5(3) . . . . ? P2 C15 C20 C19 -179.37(18) . . . . ? C15 P2 C21 C26 4.0(2) . . . . ? C3 P2 C21 C26 115.12(19) . . . . ? S2 P2 C21 C26 -120.43(17) . . . . ? C15 P2 C21 C22 -178.92(17) . . . . ? C3 P2 C21 C22 -67.80(18) . . . . ? S2 P2 C21 C22 56.65(18) . . . . ? C26 C21 C22 C23 0.0(3) . . . . ? P2 C21 C22 C23 -177.15(17) . . . . ? C21 C22 C23 C24 0.6(3) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C24 C25 C26 C21 0.8(3) . . . . ? C22 C21 C26 C25 -0.7(3) . . . . ? P2 C21 C26 C25 176.35(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.604 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.076 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; The H(C) atom positions were calculated. All hydrogen atoms were refined in isotropic approximation in riding model with the Uiso(H) parameters equal to 1.2 Ueq(Ci), for methyl groups equal to 1.5 Ueq(Cii), where U(Ci) and U(Cii) are respectively the equivalent thermal parameters of the carbon atoms to which corresponding H atoms are bonded. ; # Attachment '4a.CIF' data_b _database_code_depnum_ccdc_archive 'CCDC 730243' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H23 Cl O P2 Pd S2' _chemical_formula_sum 'C30 H23 Cl O P2 Pd S2' _chemical_formula_weight 667.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2080(13) _cell_length_b 8.7616(8) _cell_length_c 26.551(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.341(5) _cell_angle_gamma 90.00 _cell_volume 2774.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 662 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13205 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6636 _reflns_number_gt 4859 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0373P)^2^+0.4903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6636 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.29814(2) 0.22761(3) 0.104789(10) 0.01458(8) Uani 1 1 d . . . Cl1 Cl 0.37826(9) 0.30237(11) 0.03461(4) 0.0333(3) Uani 1 1 d . . . P1 P 0.04252(8) 0.28011(10) 0.09039(4) 0.01664(19) Uani 1 1 d . . . S1 S 0.13187(8) 0.17946(10) 0.04521(4) 0.0226(2) Uani 1 1 d . . . P2 P 0.46937(8) 0.08109(11) 0.19378(4) 0.0203(2) Uani 1 1 d . . . S2 S 0.46936(9) 0.28302(11) 0.16082(4) 0.0315(2) Uani 1 1 d . . . C1 C 0.2574(5) 0.0918(5) 0.20786(19) 0.0172(11) Uani 0.70 1 d P A 1 O1 O 0.3705(3) 0.0524(4) 0.22595(15) 0.0205(9) Uani 0.70 1 d P A 1 C2 C 0.2158(6) 0.1651(7) 0.1615(3) 0.0154(13) Uani 0.70 1 d P A 1 C3 C 0.0994(5) 0.1927(6) 0.1517(2) 0.0156(11) Uani 0.70 1 d P A 1 C4 C 0.0299(4) 0.1516(5) 0.18497(19) 0.0178(10) Uani 0.70 1 d P A 1 H4A H -0.0479 0.1746 0.1766 0.021 Uiso 0.70 1 calc PR A 1 C5 C 0.0767(6) 0.0769(6) 0.2303(2) 0.0205(12) Uani 0.70 1 d P A 1 H5A H 0.0309 0.0456 0.2531 0.025 Uiso 0.70 1 calc PR A 1 C6 C 0.1908(6) 0.0479(8) 0.2421(3) 0.0209(14) Uani 0.70 1 d P A 1 H6A H 0.2237 -0.0018 0.2734 0.025 Uiso 0.70 1 calc PR A 1 O1' O 0.0538(8) 0.2248(12) 0.1504(4) 0.021(3) Uiso 0.30 1 d P A 2 C1' C 0.1475(11) 0.1561(14) 0.1800(5) 0.018(2) Uiso 0.30 1 d P A 2 C2' C 0.2512(13) 0.150(2) 0.1671(7) 0.013(4) Uiso 0.30 1 d P A 2 C3' C 0.3354(12) 0.0751(15) 0.2059(5) 0.012(3) Uiso 0.30 1 d P A 2 C4' C 0.3179(11) 0.0077(14) 0.2490(5) 0.021(3) Uiso 0.30 1 d P A 2 H4'A H 0.3767 -0.0410 0.2728 0.026 Uiso 0.30 1 calc PR A 2 C5' C 0.2083(15) 0.0134(19) 0.2569(7) 0.017(4) Uiso 0.30 1 d P A 2 H5'A H 0.1922 -0.0372 0.2861 0.021 Uiso 0.30 1 calc PR A 2 C6' C 0.1251(15) 0.0869(17) 0.2252(6) 0.019(3) Uiso 0.30 1 d P A 2 H6'A H 0.0526 0.0928 0.2327 0.022 Uiso 0.30 1 calc PR A 2 C7 C 0.0651(3) 0.4833(4) 0.09634(14) 0.0179(8) Uani 1 1 d . A . C8 C 0.0544(7) 0.5545(10) 0.1436(3) 0.0221(17) Uani 0.60 1 d P A 1 H8A H 0.0340 0.4960 0.1703 0.027 Uiso 0.60 1 calc PR A 1 C9 C 0.0741(8) 0.7101(9) 0.1497(4) 0.0243(17) Uani 0.60 1 d P A 1 H9A H 0.0662 0.7611 0.1804 0.029 Uiso 0.60 1 calc PR A 1 C9' C 0.0446(13) 0.723(2) 0.1350(6) 0.033(4) Uiso 0.40 1 d P A 2 H9'A H 0.0127 0.7813 0.1584 0.039 Uiso 0.40 1 calc PR A 2 C8' C 0.0224(11) 0.5653(17) 0.1307(5) 0.019(3) Uiso 0.40 1 d P A 2 H8'A H -0.0219 0.5175 0.1515 0.023 Uiso 0.40 1 calc PR A 2 C10 C 0.1069(4) 0.7922(4) 0.10816(17) 0.0307(10) Uani 1 1 d . . . H10A H 0.1189 0.8992 0.1111 0.037 Uiso 1 1 calc R A 1 C11 C 0.1202(9) 0.7227(11) 0.0670(4) 0.0197(16) Uani 0.60 1 d P A 1 H11A H 0.1442 0.7793 0.0408 0.024 Uiso 0.60 1 calc PR A 1 C12 C 0.1001(10) 0.5645(13) 0.0600(5) 0.0197(16) Uani 0.60 1 d P A 1 H12A H 0.1113 0.5158 0.0296 0.024 Uiso 0.60 1 calc PR A 1 C11' C 0.1455(12) 0.7088(19) 0.0649(7) 0.016(3) Uiso 0.40 1 d P A 2 H11B H 0.1826 0.7605 0.0419 0.019 Uiso 0.40 1 calc PR A 2 C12' C 0.1241(12) 0.555(2) 0.0607(8) 0.013(3) Uiso 0.40 1 d P A 2 H12B H 0.1476 0.4958 0.0349 0.016 Uiso 0.40 1 calc PR A 2 C13 C -0.1046(3) 0.2429(4) 0.06902(13) 0.0176(7) Uani 1 1 d . A . C14 C -0.1371(3) 0.0905(4) 0.05866(14) 0.0212(8) Uani 1 1 d . . . H14A H -0.0823 0.0118 0.0636 0.025 Uiso 1 1 calc R A . C15 C -0.2490(3) 0.0554(5) 0.04132(15) 0.0276(9) Uani 1 1 d . A . H15A H -0.2714 -0.0475 0.0340 0.033 Uiso 1 1 calc R . . C16 C -0.3289(3) 0.1706(5) 0.03464(15) 0.0305(9) Uani 1 1 d . . . H16A H -0.4060 0.1457 0.0234 0.037 Uiso 1 1 calc R A . C17 C -0.2971(3) 0.3225(5) 0.04428(15) 0.0299(9) Uani 1 1 d . A . H17A H -0.3521 0.4009 0.0391 0.036 Uiso 1 1 calc R . . C18 C -0.1845(3) 0.3582(4) 0.06149(14) 0.0241(8) Uani 1 1 d . . . H18A H -0.1622 0.4614 0.0681 0.029 Uiso 1 1 calc R A . C19 C 0.5884(3) 0.0603(4) 0.24668(14) 0.0212(8) Uani 1 1 d . A . C20 C 0.6337(4) 0.1871(5) 0.27463(16) 0.0335(10) Uani 1 1 d . . . H20A H 0.6035 0.2855 0.2653 0.040 Uiso 1 1 calc R A . C21 C 0.7230(4) 0.1704(5) 0.31605(16) 0.0371(11) Uani 1 1 d . A . H21A H 0.7540 0.2578 0.3351 0.044 Uiso 1 1 calc R . . C22 C 0.7674(3) 0.0285(5) 0.32997(16) 0.0336(10) Uani 1 1 d . . . H22A H 0.8291 0.0179 0.3584 0.040 Uiso 1 1 calc R A . C23 C 0.7227(4) -0.0974(5) 0.30273(16) 0.0358(11) Uani 1 1 d . A . H23A H 0.7528 -0.1955 0.3127 0.043 Uiso 1 1 calc R . . C24 C 0.6339(3) -0.0832(5) 0.26072(15) 0.0288(9) Uani 1 1 d . . . H24A H 0.6042 -0.1709 0.2416 0.035 Uiso 1 1 calc R A . C25 C 0.4685(3) -0.0770(4) 0.15117(14) 0.0203(8) Uani 1 1 d . A . C26 C 0.5346(4) -0.0727(4) 0.11447(14) 0.0277(9) Uani 1 1 d . . . H26A H 0.5784 0.0151 0.1115 0.033 Uiso 1 1 calc R A . C27 C 0.5362(4) -0.1959(5) 0.08263(15) 0.0334(10) Uani 1 1 d . A . H27A H 0.5816 -0.1929 0.0577 0.040 Uiso 1 1 calc R . . C28 C 0.4719(4) -0.3254(5) 0.08652(16) 0.0328(10) Uani 1 1 d . . . H28A H 0.4737 -0.4102 0.0644 0.039 Uiso 1 1 calc R A . C29 C 0.4061(4) -0.3295(4) 0.12246(16) 0.0317(10) Uani 1 1 d . A . H29A H 0.3620 -0.4174 0.1250 0.038 Uiso 1 1 calc R . . C30 C 0.4033(3) -0.2066(4) 0.15508(16) 0.0264(9) Uani 1 1 d . . . H30A H 0.3576 -0.2101 0.1799 0.032 Uiso 1 1 calc R A . 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 Pd1 0.01585(13) 0.01292(13) 0.01507(14) -0.00133(11) 0.00350(10) -0.00048(11) Cl1 0.0476(7) 0.0285(5) 0.0317(6) -0.0096(4) 0.0261(5) -0.0161(5) P1 0.0194(5) 0.0131(4) 0.0169(5) -0.0007(4) 0.0027(4) -0.0018(4) S1 0.0208(5) 0.0200(5) 0.0246(5) -0.0073(4) -0.0010(4) 0.0016(4) P2 0.0163(5) 0.0172(5) 0.0262(5) 0.0007(4) 0.0016(4) 0.0001(4) S2 0.0248(5) 0.0164(4) 0.0449(6) 0.0043(5) -0.0111(4) -0.0039(4) C1 0.023(3) 0.016(2) 0.012(3) -0.005(2) 0.002(2) -0.001(2) O1 0.015(2) 0.032(2) 0.012(2) 0.0025(18) -0.0019(17) 0.0045(17) C2 0.017(4) 0.009(3) 0.019(3) -0.005(2) 0.001(3) 0.002(3) C3 0.025(3) 0.008(3) 0.014(3) -0.004(2) 0.003(2) 0.001(2) C4 0.021(3) 0.015(2) 0.018(3) -0.001(2) 0.004(2) -0.001(2) C5 0.026(3) 0.019(3) 0.019(3) -0.005(2) 0.009(3) -0.004(2) C6 0.024(4) 0.022(4) 0.017(4) -0.001(3) 0.006(3) 0.004(3) C7 0.0183(19) 0.0110(16) 0.023(2) -0.0001(14) 0.0006(15) -0.0015(14) C8 0.027(5) 0.022(4) 0.017(4) 0.002(3) 0.004(4) -0.001(3) C9 0.039(5) 0.012(3) 0.021(4) -0.005(3) 0.005(4) 0.000(3) C10 0.034(2) 0.0115(18) 0.044(3) -0.0011(18) 0.002(2) -0.0038(16) C11 0.023(4) 0.015(3) 0.019(3) 0.002(2) 0.001(3) 0.001(3) C12 0.023(4) 0.015(3) 0.019(3) 0.002(2) 0.001(3) 0.001(3) C13 0.0170(17) 0.0235(19) 0.0115(17) -0.0010(14) 0.0013(13) -0.0042(14) C14 0.021(2) 0.0223(19) 0.021(2) 0.0001(16) 0.0065(16) -0.0028(15) C15 0.026(2) 0.031(2) 0.025(2) -0.0015(18) 0.0029(17) -0.0142(17) C16 0.019(2) 0.050(3) 0.021(2) 0.0000(19) 0.0027(16) -0.0102(19) C17 0.022(2) 0.044(3) 0.024(2) 0.0029(19) 0.0047(17) 0.0090(18) C18 0.024(2) 0.025(2) 0.024(2) -0.0017(17) 0.0097(17) -0.0009(16) C19 0.0171(19) 0.030(2) 0.0167(19) 0.0038(16) 0.0032(15) 0.0022(15) C20 0.035(2) 0.034(2) 0.031(2) 0.0016(19) 0.0049(19) -0.0065(19) C21 0.040(3) 0.043(3) 0.026(2) -0.003(2) 0.002(2) -0.015(2) C22 0.021(2) 0.055(3) 0.024(2) 0.004(2) 0.0014(17) 0.000(2) C23 0.031(2) 0.046(3) 0.030(2) 0.007(2) 0.0042(19) 0.013(2) C24 0.029(2) 0.032(2) 0.023(2) -0.0001(18) 0.0019(18) 0.0064(18) C25 0.021(2) 0.0165(18) 0.0189(19) 0.0068(15) -0.0066(15) -0.0001(14) C26 0.039(3) 0.026(2) 0.016(2) -0.0004(17) 0.0001(17) -0.0077(18) C27 0.043(3) 0.038(3) 0.016(2) -0.0020(18) 0.0013(18) -0.005(2) C28 0.041(3) 0.023(2) 0.027(2) -0.0041(18) -0.0103(19) 0.0038(19) C29 0.035(2) 0.0159(18) 0.039(3) 0.0013(18) -0.004(2) -0.0014(17) C30 0.021(2) 0.0195(19) 0.037(2) 0.0040(17) 0.0040(17) 0.0004(15) _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 Pd1 C2' 1.983(19) . ? Pd1 C2 2.055(7) . ? Pd1 S1 2.3298(10) . ? Pd1 S2 2.3428(10) . ? Pd1 Cl1 2.3742(10) . ? P1 O1' 1.643(10) . ? P1 C13 1.794(4) . ? P1 C3 1.798(6) . ? P1 C7 1.803(3) . ? P1 S1 1.9914(13) . ? P2 O1 1.640(4) . ? P2 C3' 1.733(14) . ? P2 C25 1.787(4) . ? P2 C19 1.801(4) . ? P2 S2 1.9738(14) . ? C1 C2 1.386(9) . ? C1 C6 1.397(8) . ? C1 O1 1.405(6) . ? C2 C3 1.410(9) . ? C3 C4 1.397(7) . ? C4 C5 1.381(8) . ? C4 H4A 0.9500 . ? C5 C6 1.384(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O1' C1' 1.379(15) . ? C1' C2' 1.382(19) . ? C1' C6' 1.422(19) . ? C2' C3' 1.45(2) . ? C3' C4' 1.344(18) . ? C4' C5' 1.40(2) . ? C4' H4'A 0.9500 . ? C5' C6' 1.338(19) . ? C5' H5'A 0.9500 . ? C6' H6'A 0.9500 . ? C7 C12 1.340(13) . ? C7 C8' 1.350(15) . ? C7 C8 1.431(9) . ? C7 C12' 1.45(2) . ? C8 C9 1.389(12) . ? C8 H8A 0.9500 . ? C9 C10 1.444(10) . ? C9 H9A 0.9500 . ? C9' C10 1.297(17) . ? C9' C8' 1.41(2) . ? C9' H9'A 0.9500 . ? C8' H8'A 0.9500 . ? C10 C11 1.291(11) . ? C10 C11' 1.519(16) . ? C10 H10A 0.9500 . ? C11 C12 1.413(12) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C11' C12' 1.376(17) . ? C11' H11B 0.9500 . ? C12' H12B 0.9500 . ? C13 C18 1.389(5) . ? C13 C14 1.403(5) . ? C14 C15 1.380(5) . ? C14 H14A 0.9500 . ? C15 C16 1.388(6) . ? C15 H15A 0.9500 . ? C16 C17 1.394(6) . ? C16 H16A 0.9500 . ? C17 C18 1.388(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.384(5) . ? C19 C24 1.393(5) . ? C20 C21 1.380(6) . ? C20 H20A 0.9500 . ? C21 C22 1.376(6) . ? C21 H21A 0.9500 . ? C22 C23 1.367(6) . ? C22 H22A 0.9500 . ? C23 C24 1.385(6) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.392(5) . ? C25 C30 1.403(5) . ? C26 C27 1.374(5) . ? C26 H26A 0.9500 . ? C27 C28 1.396(6) . ? C27 H27A 0.9500 . ? C28 C29 1.373(6) . ? C28 H28A 0.9500 . ? C29 C30 1.387(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? 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' Pd1 C2 12.5(4) . . ? C2' Pd1 S1 98.0(4) . . ? C2 Pd1 S1 87.6(2) . . ? C2' Pd1 S2 85.3(4) . . ? C2 Pd1 S2 95.7(2) . . ? S1 Pd1 S2 176.64(4) . . ? C2' Pd1 Cl1 172.0(4) . . ? C2 Pd1 Cl1 175.2(2) . . ? S1 Pd1 Cl1 87.85(4) . . ? S2 Pd1 Cl1 88.85(4) . . ? O1' P1 C13 97.1(4) . . ? C13 P1 C3 112.1(2) . . ? O1' P1 C7 103.1(4) . . ? C13 P1 C7 109.34(17) . . ? C3 P1 C7 108.6(2) . . ? O1' P1 S1 120.7(4) . . ? C13 P1 S1 111.67(12) . . ? C3 P1 S1 101.6(2) . . ? C7 P1 S1 113.37(13) . . ? P1 S1 Pd1 91.19(5) . . ? O1 P2 C25 107.79(19) . . ? C3' P2 C25 102.5(4) . . ? O1 P2 C19 97.99(19) . . ? C3' P2 C19 119.2(5) . . ? C25 P2 C19 108.05(17) . . ? O1 P2 S2 115.99(15) . . ? C3' P2 S2 101.5(4) . . ? C25 P2 S2 114.49(13) . . ? C19 P2 S2 111.08(13) . . ? P2 S2 Pd1 90.65(5) . . ? C2 C1 C6 123.4(6) . . ? C2 C1 O1 124.4(5) . . ? C6 C1 O1 112.1(5) . . ? C1 O1 P2 124.3(4) . . ? C1 C2 C3 114.1(6) . . ? C1 C2 Pd1 129.1(5) . . ? C3 C2 Pd1 116.8(5) . . ? C4 C3 C2 124.3(6) . . ? C4 C3 P1 120.9(5) . . ? C2 C3 P1 114.8(4) . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C4 C5 C6 119.5(6) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 120.0(7) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C1' O1' P1 124.6(9) . . ? O1' C1' C2' 124.6(13) . . ? O1' C1' C6' 112.4(12) . . ? C2' C1' C6' 122.9(14) . . ? C1' C2' C3' 113.0(15) . . ? C1' C2' Pd1 129.6(12) . . ? C3' C2' Pd1 117.5(11) . . ? C4' C3' C2' 125.9(14) . . ? C4' C3' P2 120.0(11) . . ? C2' C3' P2 114.1(11) . . ? C3' C4' C5' 116.3(13) . . ? C3' C4' H4'A 121.8 . . ? C5' C4' H4'A 121.8 . . ? C6' C5' C4' 123.0(16) . . ? C6' C5' H5'A 118.5 . . ? C4' C5' H5'A 118.5 . . ? C5' C6' C1' 118.7(16) . . ? C5' C6' H6'A 120.7 . . ? C1' C6' H6'A 120.7 . . ? C12 C7 C8' 115.6(9) . . ? C12 C7 C8 120.1(7) . . ? C8' C7 C12' 122.0(10) . . ? C8 C7 C12' 122.4(9) . . ? C12 C7 P1 121.9(6) . . ? C8' C7 P1 120.7(7) . . ? C8 C7 P1 117.8(4) . . ? C12' C7 P1 117.2(8) . . ? C9 C8 C7 119.1(7) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 117.9(7) . . ? C8 C9 H9A 121.1 . . ? C10 C9 H9A 121.1 . . ? C10 C9' C8' 122.6(15) . . ? C10 C9' H9'A 118.7 . . ? C8' C9' H9'A 118.7 . . ? C7 C8' C9' 118.8(13) . . ? C7 C8' H8'A 120.6 . . ? C9' C8' H8'A 120.6 . . ? C11 C10 C9' 116.1(10) . . ? C11 C10 C9 121.2(6) . . ? C9' C10 C11' 120.2(11) . . ? C9 C10 C11' 121.3(8) . . ? C11 C10 H10A 119.4 . . ? C9' C10 H10A 120.9 . . ? C9 C10 H10A 119.4 . . ? C11' C10 H10A 118.1 . . ? C10 C11 C12 121.6(8) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C7 C12 C11 120.0(9) . . ? C7 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12' C11' C10 116.7(11) . . ? C12' C11' H11B 121.7 . . ? C10 C11' H11B 121.7 . . ? C11' C12' C7 118.9(12) . . ? C11' C12' H12B 120.5 . . ? C7 C12' H12B 120.5 . . ? C18 C13 C14 120.2(3) . . ? C18 C13 P1 122.6(3) . . ? C14 C13 P1 117.2(3) . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 119.5(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C13 120.0(4) . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? C20 C19 C24 119.3(4) . . ? C20 C19 P2 120.0(3) . . ? C24 C19 P2 120.6(3) . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C23 C24 C19 119.7(4) . . ? C23 C24 H24A 120.1 . . ? C19 C24 H24A 120.1 . . ? C26 C25 C30 119.8(4) . . ? C26 C25 P2 119.8(3) . . ? C30 C25 P2 120.5(3) . . ? C27 C26 C25 119.8(4) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 119.7(4) . . ? C29 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? C28 C29 C30 120.6(4) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C29 C30 C25 119.5(4) . . ? C29 C30 H30A 120.2 . . ? C25 C30 H30A 120.2 . . ? 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 O1' P1 S1 Pd1 -54.8(4) . . . . ? C13 P1 S1 Pd1 -167.78(12) . . . . ? C3 P1 S1 Pd1 -48.17(18) . . . . ? C7 P1 S1 Pd1 68.17(14) . . . . ? C2' Pd1 S1 P1 49.2(5) . . . . ? C2 Pd1 S1 P1 42.27(18) . . . . ? Cl1 Pd1 S1 P1 -136.27(5) . . . . ? O1 P2 S2 Pd1 -66.26(17) . . . . ? C3' P2 S2 Pd1 -49.3(5) . . . . ? C25 P2 S2 Pd1 60.30(14) . . . . ? C19 P2 S2 Pd1 -176.98(13) . . . . ? C2' Pd1 S2 P2 45.1(5) . . . . ? C2 Pd1 S2 P2 52.12(19) . . . . ? Cl1 Pd1 S2 P2 -129.40(5) . . . . ? C2 C1 O1 P2 -2.6(7) . . . . ? C6 C1 O1 P2 177.2(4) . . . . ? C3' P2 O1 C1 -6.0(12) . . . . ? C25 P2 O1 C1 -84.9(4) . . . . ? C19 P2 O1 C1 163.2(4) . . . . ? S2 P2 O1 C1 45.0(4) . . . . ? C6 C1 C2 C3 0.2(8) . . . . ? O1 C1 C2 C3 -180.0(4) . . . . ? C6 C1 C2 Pd1 -176.3(5) . . . . ? O1 C1 C2 Pd1 3.5(8) . . . . ? C2' Pd1 C2 C1 0(3) . . . . ? S1 Pd1 C2 C1 146.5(5) . . . . ? S2 Pd1 C2 C1 -34.2(5) . . . . ? C2' Pd1 C2 C3 -177(3) . . . . ? S1 Pd1 C2 C3 -29.9(4) . . . . ? S2 Pd1 C2 C3 149.4(4) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? Pd1 C2 C3 C4 177.2(4) . . . . ? C1 C2 C3 P1 -177.3(4) . . . . ? Pd1 C2 C3 P1 -0.3(6) . . . . ? O1' P1 C3 C4 22.7(11) . . . . ? C13 P1 C3 C4 -21.2(5) . . . . ? C7 P1 C3 C4 99.7(4) . . . . ? S1 P1 C3 C4 -140.5(4) . . . . ? O1' P1 C3 C2 -159.7(14) . . . . ? C13 P1 C3 C2 156.5(4) . . . . ? C7 P1 C3 C2 -82.6(4) . . . . ? S1 P1 C3 C2 37.1(4) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? P1 C3 C4 C5 176.3(4) . . . . ? C3 C4 C5 C6 1.5(8) . . . . ? C4 C5 C6 C1 -1.1(9) . . . . ? C2 C1 C6 C5 0.2(9) . . . . ? O1 C1 C6 C5 -179.6(5) . . . . ? C13 P1 O1' C1' 146.7(10) . . . . ? C3 P1 O1' C1' 7.0(8) . . . . ? C7 P1 O1' C1' -101.5(10) . . . . ? S1 P1 O1' C1' 26.3(11) . . . . ? P1 O1' C1' C2' 12.8(19) . . . . ? P1 O1' C1' C6' -165.4(9) . . . . ? O1' C1' C2' C3' 178.2(12) . . . . ? C6' C1' C2' C3' -4(2) . . . . ? O1' C1' C2' Pd1 -2(2) . . . . ? C6' C1' C2' Pd1 176.2(11) . . . . ? C2 Pd1 C2' C1' -1.2(17) . . . . ? S1 Pd1 C2' C1' -35.0(16) . . . . ? S2 Pd1 C2' C1' 144.7(16) . . . . ? C2 Pd1 C2' C3' 179(4) . . . . ? S1 Pd1 C2' C3' 145.0(12) . . . . ? S2 Pd1 C2' C3' -35.3(12) . . . . ? C1' C2' C3' C4' 4(2) . . . . ? Pd1 C2' C3' C4' -175.8(11) . . . . ? C1' C2' C3' P2 -174.4(11) . . . . ? Pd1 C2' C3' P2 5.6(16) . . . . ? O1 P2 C3' C4' -9.4(8) . . . . ? C25 P2 C3' C4' 97.5(11) . . . . ? C19 P2 C3' C4' -21.7(13) . . . . ? S2 P2 C3' C4' -144.0(10) . . . . ? O1 P2 C3' C2' 169(2) . . . . ? C25 P2 C3' C2' -83.9(11) . . . . ? C19 P2 C3' C2' 156.9(10) . . . . ? S2 P2 C3' C2' 34.6(11) . . . . ? C2' C3' C4' C5' -1(2) . . . . ? P2 C3' C4' C5' 177.4(11) . . . . ? C3' C4' C5' C6' -3(2) . . . . ? C4' C5' C6' C1' 3(3) . . . . ? O1' C1' C6' C5' 178.7(14) . . . . ? C2' C1' C6' C5' 0(2) . . . . ? O1' P1 C7 C12 157.0(7) . . . . ? C13 P1 C7 C12 -100.4(6) . . . . ? C3 P1 C7 C12 137.0(6) . . . . ? S1 P1 C7 C12 24.9(6) . . . . ? O1' P1 C7 C8' -39.2(7) . . . . ? C13 P1 C7 C8' 63.3(6) . . . . ? C3 P1 C7 C8' -59.2(7) . . . . ? S1 P1 C7 C8' -171.4(6) . . . . ? O1' P1 C7 C8 -17.4(6) . . . . ? C13 P1 C7 C8 85.1(5) . . . . ? C3 P1 C7 C8 -37.4(5) . . . . ? S1 P1 C7 C8 -149.6(4) . . . . ? O1' P1 C7 C12' 144.7(8) . . . . ? C13 P1 C7 C12' -112.8(7) . . . . ? C3 P1 C7 C12' 124.7(8) . . . . ? S1 P1 C7 C12' 12.6(7) . . . . ? C12 C7 C8 C9 3.8(12) . . . . ? C8' C7 C8 C9 -78(3) . . . . ? C12' C7 C8 C9 17.2(12) . . . . ? P1 C7 C8 C9 178.4(6) . . . . ? C7 C8 C9 C10 -1.2(12) . . . . ? C12 C7 C8' C9' -16.9(14) . . . . ? C8 C7 C8' C9' 92(3) . . . . ? C12' C7 C8' C9' -5.8(15) . . . . ? P1 C7 C8' C9' 178.3(8) . . . . ? C10 C9' C8' C7 -1.8(18) . . . . ? C8' C9' C10 C11 20.1(16) . . . . ? C8' C9' C10 C9 -90(3) . . . . ? C8' C9' C10 C11' 8.9(17) . . . . ? C8 C9 C10 C11 -1.7(12) . . . . ? C8 C9 C10 C9' 78(3) . . . . ? C8 C9 C10 C11' -14.2(13) . . . . ? C9' C10 C11 C12 -19.5(12) . . . . ? C9 C10 C11 C12 2.0(12) . . . . ? C11' C10 C11 C12 96(6) . . . . ? C8' C7 C12 C11 17.5(12) . . . . ? C8 C7 C12 C11 -3.6(11) . . . . ? C12' C7 C12 C11 -108(6) . . . . ? P1 C7 C12 C11 -177.9(6) . . . . ? C10 C11 C12 C7 0.7(12) . . . . ? C11 C10 C11' C12' -78(6) . . . . ? C9' C10 C11' C12' -8.5(14) . . . . ? C9 C10 C11' C12' 14.2(13) . . . . ? C10 C11' C12' C7 1.3(13) . . . . ? C12 C7 C12' C11' 65(6) . . . . ? C8' C7 C12' C11' 5.6(14) . . . . ? C8 C7 C12' C11' -17.1(13) . . . . ? P1 C7 C12' C11' -178.3(7) . . . . ? O1' P1 C13 C18 103.7(5) . . . . ? C3 P1 C13 C18 117.5(3) . . . . ? C7 P1 C13 C18 -2.9(4) . . . . ? S1 P1 C13 C18 -129.2(3) . . . . ? O1' P1 C13 C14 -77.8(5) . . . . ? C3 P1 C13 C14 -64.0(3) . . . . ? C7 P1 C13 C14 175.5(3) . . . . ? S1 P1 C13 C14 49.2(3) . . . . ? C18 C13 C14 C15 -0.5(6) . . . . ? P1 C13 C14 C15 -179.0(3) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C14 C15 C16 C17 1.3(6) . . . . ? C15 C16 C17 C18 -1.0(6) . . . . ? C16 C17 C18 C13 -0.1(6) . . . . ? C14 C13 C18 C17 0.8(6) . . . . ? P1 C13 C18 C17 179.2(3) . . . . ? O1 P2 C19 C20 -91.9(3) . . . . ? C3' P2 C19 C20 -87.4(6) . . . . ? C25 P2 C19 C20 156.4(3) . . . . ? S2 P2 C19 C20 30.0(4) . . . . ? O1 P2 C19 C24 86.4(4) . . . . ? C3' P2 C19 C24 91.0(6) . . . . ? C25 P2 C19 C24 -25.3(4) . . . . ? S2 P2 C19 C24 -151.7(3) . . . . ? C24 C19 C20 C21 -0.2(6) . . . . ? P2 C19 C20 C21 178.2(3) . . . . ? C19 C20 C21 C22 -0.1(7) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 C24 0.9(7) . . . . ? C22 C23 C24 C19 -1.2(7) . . . . ? C20 C19 C24 C23 0.8(6) . . . . ? P2 C19 C24 C23 -177.5(3) . . . . ? O1 P2 C25 C26 171.8(3) . . . . ? C3' P2 C25 C26 150.0(5) . . . . ? C19 P2 C25 C26 -83.3(3) . . . . ? S2 P2 C25 C26 41.1(3) . . . . ? O1 P2 C25 C30 -9.4(4) . . . . ? C3' P2 C25 C30 -31.1(6) . . . . ? C19 P2 C25 C30 95.6(3) . . . . ? S2 P2 C25 C30 -140.1(3) . . . . ? C30 C25 C26 C27 -0.6(6) . . . . ? P2 C25 C26 C27 178.3(3) . . . . ? C25 C26 C27 C28 0.3(6) . . . . ? C26 C27 C28 C29 0.2(6) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C28 C29 C30 C25 0.0(6) . . . . ? C26 C25 C30 C29 0.4(6) . . . . ? P2 C25 C30 C29 -178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.980 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.110 _publ_section_references ; Bruker (2005). APEX2 softwarwe package, Bruker AXS Inc., 5465, East Cheryl Parkway, Madison, WI 5317. Sheldrick G.M. (1998). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; The H(C) atom positions were calculated. The hydrogen atoms were refined in isotropic approximation in riding model with the Uiso(H) parameters equal to 1.2 Ueq(Ci), for methyl groups equal to 1.5 Ueq(Cii), where U(Ci) and U(Cii) are respectively the equivalent thermal parameters of the carbon atoms to which corresponding H atoms are bonded. ; # Attachment '4d.CIF' data_c _database_code_depnum_ccdc_archive 'CCDC 730244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H25 Cl N2 O P2 Pd S2' _chemical_formula_sum 'C22 H25 Cl N2 O P2 Pd S2' _chemical_formula_weight 601.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6417(4) _cell_length_b 10.3955(5) _cell_length_c 13.6809(7) _cell_angle_alpha 95.103(5) _cell_angle_beta 98.150(5) _cell_angle_gamma 95.827(5) _cell_volume 1203.64(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 798 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details 'APEX2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8467 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5205 _reflns_number_gt 4534 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0303P)^2^+0.3790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5205 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.30399(2) 0.110908(17) 0.282641(13) 0.01070(6) Uani 1 1 d . . . Cl1 Cl 0.24772(7) -0.11876(6) 0.28985(5) 0.01698(13) Uani 1 1 d . . . P1 P 0.14843(7) 0.25617(6) 0.45071(4) 0.01185(13) Uani 1 1 d . . . S1 S 0.05854(7) 0.14560(6) 0.32640(4) 0.01412(13) Uani 1 1 d . . . P2 P 0.50681(7) 0.21792(6) 0.12928(4) 0.01210(13) Uani 1 1 d . . . S2 S 0.53062(7) 0.07188(6) 0.21476(5) 0.01534(13) Uani 1 1 d . . . O1 O 0.2537(2) 0.38267(16) 0.42877(12) 0.0167(4) Uani 1 1 d . . . N1 N 0.2682(2) 0.1982(2) 0.53525(15) 0.0163(4) Uani 1 1 d . . . N2 N 0.0092(2) 0.3040(2) 0.50815(15) 0.0167(4) Uani 1 1 d . . . C1 C 0.3195(3) 0.4034(2) 0.34262(18) 0.0137(5) Uani 1 1 d . . . C2 C 0.3592(3) 0.3027(2) 0.27938(17) 0.0127(5) Uani 1 1 d . . . C3 C 0.4423(3) 0.3456(2) 0.20485(17) 0.0135(5) Uani 1 1 d . . . C4 C 0.4745(3) 0.4759(2) 0.18965(19) 0.0187(5) Uani 1 1 d . . . H4A H 0.5307 0.4992 0.1378 0.022 Uiso 1 1 calc R . . C5 C 0.4240(3) 0.5708(2) 0.2509(2) 0.0211(6) Uani 1 1 d . . . H5A H 0.4410 0.6598 0.2400 0.025 Uiso 1 1 calc R . . C6 C 0.3478(3) 0.5338(2) 0.32837(19) 0.0170(5) Uani 1 1 d . . . H6A H 0.3147 0.5982 0.3720 0.020 Uiso 1 1 calc R . . C7 C 0.4327(3) 0.1898(3) 0.5223(2) 0.0241(6) Uani 1 1 d . . . H7A H 0.4953 0.1817 0.5866 0.036 Uiso 1 1 calc R . . H7B H 0.4741 0.2685 0.4957 0.036 Uiso 1 1 calc R . . H7C H 0.4385 0.1136 0.4760 0.036 Uiso 1 1 calc R . . C8 C 0.1998(3) 0.0862(3) 0.5797(2) 0.0269(6) Uani 1 1 d . . . H8A H 0.2644 0.0778 0.6433 0.040 Uiso 1 1 calc R . . H8B H 0.1966 0.0069 0.5348 0.040 Uiso 1 1 calc R . . H8C H 0.0927 0.0994 0.5909 0.040 Uiso 1 1 calc R . . C9 C 0.0443(3) 0.3757(3) 0.60787(18) 0.0207(6) Uani 1 1 d . . . H9A H 0.0050 0.4608 0.6059 0.031 Uiso 1 1 calc R . . H9B H 0.1583 0.3879 0.6296 0.031 Uiso 1 1 calc R . . H9C H -0.0071 0.3264 0.6545 0.031 Uiso 1 1 calc R . . C10 C -0.1586(3) 0.2846(2) 0.46756(19) 0.0186(5) Uani 1 1 d . . . H10A H -0.2167 0.2365 0.5120 0.028 Uiso 1 1 calc R . . H10B H -0.1739 0.2351 0.4019 0.028 Uiso 1 1 calc R . . H10C H -0.1977 0.3693 0.4617 0.028 Uiso 1 1 calc R . . C11 C 0.6897(3) 0.2776(2) 0.09107(18) 0.0139(5) Uani 1 1 d . . . C12 C 0.8102(3) 0.3376(3) 0.16541(19) 0.0201(5) Uani 1 1 d . . . H12A H 0.7912 0.3508 0.2321 0.024 Uiso 1 1 calc R . . C13 C 0.9575(3) 0.3778(3) 0.1417(2) 0.0223(6) Uani 1 1 d . . . H13A H 1.0388 0.4194 0.1920 0.027 Uiso 1 1 calc R . . C14 C 0.9855(3) 0.3570(3) 0.0447(2) 0.0236(6) Uani 1 1 d . . . H14A H 1.0866 0.3834 0.0287 0.028 Uiso 1 1 calc R . . C15 C 0.8672(3) 0.2979(3) -0.0291(2) 0.0215(6) Uani 1 1 d . . . H15A H 0.8871 0.2845 -0.0956 0.026 Uiso 1 1 calc R . . C16 C 0.7189(3) 0.2580(2) -0.00632(18) 0.0166(5) Uani 1 1 d . . . H16A H 0.6379 0.2174 -0.0572 0.020 Uiso 1 1 calc R . . C17 C 0.3616(3) 0.1782(2) 0.01932(18) 0.0143(5) Uani 1 1 d . . . C18 C 0.3457(3) 0.2680(3) -0.05008(19) 0.0205(6) Uani 1 1 d . . . H18A H 0.4124 0.3480 -0.0398 0.025 Uiso 1 1 calc R . . C19 C 0.2327(3) 0.2411(3) -0.1343(2) 0.0237(6) Uani 1 1 d . . . H19A H 0.2226 0.3023 -0.1817 0.028 Uiso 1 1 calc R . . C20 C 0.1345(3) 0.1242(3) -0.14896(19) 0.0217(6) Uani 1 1 d . . . H20A H 0.0578 0.1052 -0.2069 0.026 Uiso 1 1 calc R . . C21 C 0.1481(3) 0.0356(3) -0.0794(2) 0.0211(6) Uani 1 1 d . . . H21A H 0.0796 -0.0434 -0.0892 0.025 Uiso 1 1 calc R . . C22 C 0.2621(3) 0.0620(2) 0.00497(19) 0.0169(5) Uani 1 1 d . . . H22A H 0.2718 0.0008 0.0525 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01234(9) 0.00920(9) 0.01078(10) 0.00135(6) 0.00209(7) 0.00153(7) Cl1 0.0161(3) 0.0113(3) 0.0227(3) 0.0035(2) -0.0010(2) 0.0013(2) P1 0.0119(3) 0.0117(3) 0.0125(3) 0.0020(2) 0.0028(2) 0.0017(2) S1 0.0127(3) 0.0151(3) 0.0140(3) -0.0004(2) 0.0022(2) 0.0005(2) P2 0.0137(3) 0.0115(3) 0.0117(3) 0.0023(2) 0.0032(2) 0.0019(2) S2 0.0179(3) 0.0143(3) 0.0165(3) 0.0055(2) 0.0061(2) 0.0063(2) O1 0.0227(9) 0.0122(8) 0.0157(9) -0.0017(7) 0.0093(7) -0.0019(7) N1 0.0145(10) 0.0185(11) 0.0158(11) 0.0024(8) 0.0002(8) 0.0037(8) N2 0.0165(10) 0.0199(11) 0.0146(11) 0.0005(8) 0.0060(8) 0.0029(9) C1 0.0111(11) 0.0149(12) 0.0155(12) 0.0022(9) 0.0043(9) -0.0007(9) C2 0.0112(11) 0.0130(11) 0.0136(12) 0.0011(9) 0.0008(9) 0.0014(9) C3 0.0150(11) 0.0136(12) 0.0123(12) 0.0021(9) 0.0014(9) 0.0039(9) C4 0.0234(13) 0.0169(13) 0.0180(13) 0.0055(10) 0.0083(11) 0.0017(10) C5 0.0276(14) 0.0098(12) 0.0281(15) 0.0047(10) 0.0101(12) 0.0020(11) C6 0.0184(12) 0.0127(12) 0.0206(13) -0.0010(10) 0.0054(10) 0.0037(10) C7 0.0154(13) 0.0349(16) 0.0203(14) -0.0038(12) -0.0036(11) 0.0094(12) C8 0.0333(16) 0.0207(14) 0.0260(15) 0.0116(11) -0.0030(12) 0.0017(12) C9 0.0244(14) 0.0229(14) 0.0159(13) -0.0011(10) 0.0068(11) 0.0049(11) C10 0.0152(12) 0.0196(13) 0.0224(14) 0.0013(10) 0.0067(10) 0.0042(10) C11 0.0137(11) 0.0114(11) 0.0172(12) 0.0039(9) 0.0030(9) 0.0016(9) C12 0.0220(13) 0.0215(13) 0.0163(13) 0.0026(10) 0.0009(10) 0.0031(11) C13 0.0177(13) 0.0221(14) 0.0251(15) 0.0034(11) -0.0022(11) -0.0003(11) C14 0.0169(13) 0.0220(14) 0.0349(16) 0.0101(12) 0.0087(11) 0.0035(11) C15 0.0223(13) 0.0229(14) 0.0230(14) 0.0062(11) 0.0109(11) 0.0073(11) C16 0.0193(12) 0.0166(12) 0.0147(13) 0.0022(10) 0.0035(10) 0.0039(10) C17 0.0126(11) 0.0151(12) 0.0154(12) -0.0002(9) 0.0035(9) 0.0026(9) C18 0.0196(13) 0.0215(13) 0.0199(14) 0.0048(10) 0.0015(11) 0.0003(11) C19 0.0209(13) 0.0311(15) 0.0193(14) 0.0069(11) -0.0001(11) 0.0041(12) C20 0.0153(12) 0.0314(15) 0.0173(14) -0.0046(11) 0.0006(10) 0.0065(11) C21 0.0173(13) 0.0215(14) 0.0228(14) -0.0075(11) 0.0042(11) 0.0005(11) C22 0.0193(13) 0.0132(12) 0.0186(13) 0.0004(10) 0.0044(10) 0.0023(10) _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 Pd1 C2 2.008(2) . ? Pd1 S1 2.3376(6) . ? Pd1 S2 2.3393(6) . ? Pd1 Cl1 2.4013(6) . ? P1 O1 1.5974(17) . ? P1 N2 1.622(2) . ? P1 N1 1.638(2) . ? P1 S1 1.9782(8) . ? P2 C3 1.792(2) . ? P2 C11 1.802(2) . ? P2 C17 1.805(2) . ? P2 S2 2.0065(8) . ? O1 C1 1.403(3) . ? N1 C7 1.467(3) . ? N1 C8 1.471(3) . ? N2 C10 1.465(3) . ? N2 C9 1.472(3) . ? C1 C6 1.389(3) . ? C1 C2 1.399(3) . ? C2 C3 1.406(3) . ? C3 C4 1.395(3) . ? C4 C5 1.382(4) . ? C4 H4A 0.9500 . ? C5 C6 1.387(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.392(3) . ? C11 C12 1.401(3) . ? C12 C13 1.390(4) . ? C12 H12A 0.9500 . ? C13 C14 1.385(4) . ? C13 H13A 0.9500 . ? C14 C15 1.382(4) . ? C14 H14A 0.9500 . ? C15 C16 1.392(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.392(3) . ? C17 C18 1.393(3) . ? C18 C19 1.387(4) . ? C18 H18A 0.9500 . ? C19 C20 1.392(4) . ? C19 H19A 0.9500 . ? C20 C21 1.384(4) . ? C20 H20A 0.9500 . ? C21 C22 1.395(4) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? 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 Pd1 S1 90.80(7) . . ? C2 Pd1 S2 89.66(7) . . ? S1 Pd1 S2 171.58(2) . . ? C2 Pd1 Cl1 177.85(7) . . ? S1 Pd1 Cl1 90.74(2) . . ? S2 Pd1 Cl1 89.04(2) . . ? O1 P1 N2 107.82(10) . . ? O1 P1 N1 101.84(10) . . ? N2 P1 N1 105.03(11) . . ? O1 P1 S1 111.21(7) . . ? N2 P1 S1 110.47(8) . . ? N1 P1 S1 119.61(8) . . ? P1 S1 Pd1 94.14(3) . . ? C3 P2 C11 108.88(11) . . ? C3 P2 C17 107.59(11) . . ? C11 P2 C17 107.90(11) . . ? C3 P2 S2 105.65(8) . . ? C11 P2 S2 112.42(8) . . ? C17 P2 S2 114.18(8) . . ? P2 S2 Pd1 91.68(3) . . ? C1 O1 P1 127.94(15) . . ? C7 N1 C8 112.8(2) . . ? C7 N1 P1 120.17(17) . . ? C8 N1 P1 115.54(17) . . ? C10 N2 C9 113.7(2) . . ? C10 N2 P1 124.99(17) . . ? C9 N2 P1 121.31(17) . . ? C6 C1 C2 123.2(2) . . ? C6 C1 O1 113.6(2) . . ? C2 C1 O1 123.2(2) . . ? C1 C2 C3 114.0(2) . . ? C1 C2 Pd1 127.08(17) . . ? C3 C2 Pd1 118.92(17) . . ? C4 C3 C2 124.0(2) . . ? C4 C3 P2 121.58(18) . . ? C2 C3 P2 114.41(18) . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 118.8(2) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 119.5(2) . . ? C16 C11 P2 123.04(18) . . ? C12 C11 P2 117.28(19) . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 119.9(2) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.2(2) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C11 C16 C15 119.9(2) . . ? C11 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C22 C17 C18 119.8(2) . . ? C22 C17 P2 121.07(19) . . ? C18 C17 P2 119.05(18) . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C17 C22 C21 119.8(2) . . ? C17 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? 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 O1 P1 S1 Pd1 60.49(8) . . . . ? N2 P1 S1 Pd1 -179.82(8) . . . . ? N1 P1 S1 Pd1 -57.78(9) . . . . ? C2 Pd1 S1 P1 -60.18(7) . . . . ? Cl1 Pd1 S1 P1 118.32(3) . . . . ? C3 P2 S2 Pd1 39.25(8) . . . . ? C11 P2 S2 Pd1 157.88(9) . . . . ? C17 P2 S2 Pd1 -78.77(9) . . . . ? C2 Pd1 S2 P2 -36.46(7) . . . . ? Cl1 Pd1 S2 P2 145.25(3) . . . . ? N2 P1 O1 C1 -139.8(2) . . . . ? N1 P1 O1 C1 110.0(2) . . . . ? S1 P1 O1 C1 -18.5(2) . . . . ? O1 P1 N1 C7 -45.4(2) . . . . ? N2 P1 N1 C7 -157.72(19) . . . . ? S1 P1 N1 C7 77.6(2) . . . . ? O1 P1 N1 C8 173.89(18) . . . . ? N2 P1 N1 C8 61.6(2) . . . . ? S1 P1 N1 C8 -63.1(2) . . . . ? O1 P1 N2 C10 113.4(2) . . . . ? N1 P1 N2 C10 -138.6(2) . . . . ? S1 P1 N2 C10 -8.3(2) . . . . ? O1 P1 N2 C9 -65.0(2) . . . . ? N1 P1 N2 C9 43.1(2) . . . . ? S1 P1 N2 C9 173.33(17) . . . . ? P1 O1 C1 C6 155.13(18) . . . . ? P1 O1 C1 C2 -27.5(3) . . . . ? C6 C1 C2 C3 5.1(3) . . . . ? O1 C1 C2 C3 -172.0(2) . . . . ? C6 C1 C2 Pd1 -172.75(19) . . . . ? O1 C1 C2 Pd1 10.1(3) . . . . ? S1 Pd1 C2 C1 36.6(2) . . . . ? S2 Pd1 C2 C1 -151.8(2) . . . . ? S1 Pd1 C2 C3 -141.12(18) . . . . ? S2 Pd1 C2 C3 30.46(18) . . . . ? C1 C2 C3 C4 -4.1(3) . . . . ? Pd1 C2 C3 C4 173.94(19) . . . . ? C1 C2 C3 P2 175.48(17) . . . . ? Pd1 C2 C3 P2 -6.5(2) . . . . ? C11 P2 C3 C4 31.8(2) . . . . ? C17 P2 C3 C4 -84.9(2) . . . . ? S2 P2 C3 C4 152.77(19) . . . . ? C11 P2 C3 C2 -147.78(18) . . . . ? C17 P2 C3 C2 95.52(19) . . . . ? S2 P2 C3 C2 -26.83(19) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? P2 C3 C4 C5 -179.1(2) . . . . ? C3 C4 C5 C6 2.5(4) . . . . ? C4 C5 C6 C1 -1.6(4) . . . . ? C2 C1 C6 C5 -2.5(4) . . . . ? O1 C1 C6 C5 174.9(2) . . . . ? C3 P2 C11 C16 -133.4(2) . . . . ? C17 P2 C11 C16 -16.9(2) . . . . ? S2 P2 C11 C16 109.8(2) . . . . ? C3 P2 C11 C12 51.4(2) . . . . ? C17 P2 C11 C12 167.92(19) . . . . ? S2 P2 C11 C12 -65.3(2) . . . . ? C16 C11 C12 C13 0.3(4) . . . . ? P2 C11 C12 C13 175.6(2) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C16 -0.4(4) . . . . ? C12 C11 C16 C15 0.1(4) . . . . ? P2 C11 C16 C15 -175.0(2) . . . . ? C14 C15 C16 C11 0.0(4) . . . . ? C3 P2 C17 C22 -108.5(2) . . . . ? C11 P2 C17 C22 134.2(2) . . . . ? S2 P2 C17 C22 8.4(2) . . . . ? C3 P2 C17 C18 69.1(2) . . . . ? C11 P2 C17 C18 -48.3(2) . . . . ? S2 P2 C17 C18 -174.03(18) . . . . ? C22 C17 C18 C19 -1.1(4) . . . . ? P2 C17 C18 C19 -178.7(2) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C21 0.7(4) . . . . ? C19 C20 C21 C22 -1.1(4) . . . . ? C18 C17 C22 C21 0.7(4) . . . . ? P2 C17 C22 C21 178.21(19) . . . . ? C20 C21 C22 C17 0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.553 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.085 _publ_section_references ; Bruker (2005). APEX2 softwarwe package, Bruker AXS Inc., 5465, East Cheryl Parkway, Madison, WI 5317. Sheldrick G.M. (1998). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; The H(C) atom positions were calculated. The hydrogen atoms were refined in isotropic approximation in riding model with the Uiso(H) parameters equal to 1.2 Ueq(Ci), for methyl groups equal to 1.5 Ueq(Cii), where U(Ci) and U(Cii) are respectively the equivalent thermal parameters of the carbon atoms to which corresponding H atoms are bonded. ;