Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P. Pringle' 'R. Angharad Baber' 'A. Guy Orpen' 'Matthew J. Wilkinson' 'Richard L. Wingad' _publ_contact_author_name 'Prof P Pringle' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email PAUL.PRINGLE@BRIS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Special effects of ortho-isopropylphenyl groups. Diastereoisomerism in platinum(II) and palladium(II) complexes of helically chiral PAr3 ligands. ; data_2c.2CH2Cl2(vpp2ago) _database_code_depnum_ccdc_archive 'CCDC 254102' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H70 Cl6 P2 Pt' _chemical_formula_weight 1212.85 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' P P 0.1023 0.0942 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6403(19) _cell_length_b 11.055(2) _cell_length_c 14.148(3) _cell_angle_alpha 97.94(3) _cell_angle_beta 95.31(3) _cell_angle_gamma 113.82(3) _cell_volume 1347.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15773 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6182 _reflns_number_gt 6090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS, 2001)' _computing_cell_refinement 'SAINT (Bruker-AXS, 2001)' _computing_data_reduction 'SHELXTL (Bruker-AXS, 2001)' _computing_structure_solution 'SHELXTL (Bruker-AXS, 2001)' _computing_structure_refinement 'SHELXTL (Bruker-AXS, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker-AXS, 2001)' _computing_publication_material 'SHELXTL (Bruker-AXS, 2001)' _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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6182 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Pt1 Pt 0.0000 0.0000 0.0000 0.01038(6) Uani 1 2 d S . . Cl1 Cl 0.13400(9) -0.10190(8) 0.07475(6) 0.01687(17) Uani 1 1 d . . . P1 P 0.00042(9) 0.12629(8) 0.14750(6) 0.01131(17) Uani 1 1 d . . . C1 C 0.1057(4) 0.3056(3) 0.1401(2) 0.0132(6) Uani 1 1 d . . . C2 C 0.0152(4) 0.3753(3) 0.1270(2) 0.0165(7) Uani 1 1 d . . . H2 H -0.0917 0.3315 0.1289 0.020 Uiso 1 1 calc R . . C3 C 0.0759(4) 0.5063(4) 0.1115(3) 0.0213(8) Uani 1 1 d . . . H3 H 0.0116 0.5516 0.1028 0.026 Uiso 1 1 calc R . . C4 C 0.2317(5) 0.5706(4) 0.1087(3) 0.0232(8) Uani 1 1 d . . . H4 H 0.2756 0.6608 0.0989 0.028 Uiso 1 1 calc R . . C5 C 0.3227(4) 0.5025(4) 0.1204(3) 0.0208(8) Uani 1 1 d . . . H5 H 0.4295 0.5478 0.1189 0.025 Uiso 1 1 calc R . . C6 C 0.2636(4) 0.3688(3) 0.1344(2) 0.0162(7) Uani 1 1 d . . . C7 C 0.3743(4) 0.3025(3) 0.1370(3) 0.0175(7) Uani 1 1 d . . . H7 H 0.3189 0.2096 0.1499 0.021 Uiso 1 1 calc R . . C8 C 0.5164(4) 0.3802(4) 0.2158(3) 0.0259(8) Uani 1 1 d . . . H8A H 0.5701 0.4725 0.2053 0.039 Uiso 1 1 calc R . . H8B H 0.5856 0.3353 0.2128 0.039 Uiso 1 1 calc R . . H8C H 0.4843 0.3824 0.2795 0.039 Uiso 1 1 calc R . . C9 C 0.4272(5) 0.2911(4) 0.0392(3) 0.0275(9) Uani 1 1 d . . . H9A H 0.3373 0.2465 -0.0121 0.041 Uiso 1 1 calc R . . H9B H 0.4878 0.2381 0.0385 0.041 Uiso 1 1 calc R . . H9C H 0.4905 0.3814 0.0283 0.041 Uiso 1 1 calc R . . C10 C 0.0814(4) 0.0909(3) 0.2576(2) 0.0129(6) Uani 1 1 d . . . C11 C 0.2108(4) 0.1934(3) 0.3178(2) 0.0162(7) Uani 1 1 d . . . H11 H 0.2558 0.2792 0.3001 0.019 Uiso 1 1 calc R . . C12 C 0.2744(4) 0.1730(4) 0.4022(3) 0.0210(8) Uani 1 1 d . . . H12 H 0.3633 0.2434 0.4415 0.025 Uiso 1 1 calc R . . C13 C 0.2078(5) 0.0492(4) 0.4291(3) 0.0252(8) Uani 1 1 d . . . H13 H 0.2502 0.0340 0.4872 0.030 Uiso 1 1 calc R . . C14 C 0.0789(4) -0.0520(4) 0.3709(3) 0.0222(8) Uani 1 1 d . . . H14 H 0.0339 -0.1365 0.3904 0.027 Uiso 1 1 calc R . . C15 C 0.0127(4) -0.0356(3) 0.2856(2) 0.0150(7) Uani 1 1 d . . . C16 C -0.1314(4) -0.1527(3) 0.2281(3) 0.0182(7) Uani 1 1 d . . . H16 H -0.1516 -0.1317 0.1631 0.022 Uiso 1 1 calc R . . C17 C -0.1118(5) -0.2842(4) 0.2130(3) 0.0271(9) Uani 1 1 d . . . H17A H -0.0121 -0.2677 0.1931 0.041 Uiso 1 1 calc R . . H17B H -0.1942 -0.3511 0.1627 0.041 Uiso 1 1 calc R . . H17C H -0.1166 -0.3181 0.2737 0.041 Uiso 1 1 calc R . . C18 C -0.2716(4) -0.1711(4) 0.2784(3) 0.0211(8) Uani 1 1 d . . . H18A H -0.2557 -0.1949 0.3415 0.032 Uiso 1 1 calc R . . H18B H -0.3640 -0.2433 0.2382 0.032 Uiso 1 1 calc R . . H18C H -0.2843 -0.0869 0.2876 0.032 Uiso 1 1 calc R . . C19 C -0.1877(4) 0.1109(3) 0.1773(2) 0.0142(7) Uani 1 1 d . . . C20 C -0.3173(4) 0.0195(3) 0.1116(3) 0.0163(7) Uani 1 1 d . . . H20 H -0.3044 -0.0223 0.0517 0.020 Uiso 1 1 calc R . . C21 C -0.4649(4) -0.0113(4) 0.1322(3) 0.0185(7) Uani 1 1 d . . . H21 H -0.5519 -0.0725 0.0863 0.022 Uiso 1 1 calc R . . C22 C -0.4843(4) 0.0470(4) 0.2194(3) 0.0206(8) Uani 1 1 d . . . H22 H -0.5846 0.0242 0.2348 0.025 Uiso 1 1 calc R . . C23 C -0.3568(4) 0.1392(4) 0.2845(3) 0.0196(7) Uani 1 1 d . . . H23 H -0.3715 0.1787 0.3446 0.023 Uiso 1 1 calc R . . C24 C -0.2064(4) 0.1763(3) 0.2648(2) 0.0142(7) Uani 1 1 d . . . C25 C -0.0763(4) 0.2853(3) 0.3394(2) 0.0160(7) Uani 1 1 d . . . H25 H 0.0217 0.3045 0.3132 0.019 Uiso 1 1 calc R . . C26 C -0.0610(4) 0.2380(4) 0.4350(3) 0.0209(8) Uani 1 1 d . . . H26A H -0.1526 0.2249 0.4648 0.031 Uiso 1 1 calc R . . H26B H 0.0303 0.3062 0.4788 0.031 Uiso 1 1 calc R . . H26C H -0.0509 0.1528 0.4226 0.031 Uiso 1 1 calc R . . C27 C -0.0970(4) 0.4167(4) 0.3563(3) 0.0222(8) Uani 1 1 d . . . H27A H -0.1026 0.4473 0.2948 0.033 Uiso 1 1 calc R . . H27B H -0.0095 0.4859 0.4023 0.033 Uiso 1 1 calc R . . H27C H -0.1922 0.4010 0.3824 0.033 Uiso 1 1 calc R . . C50 C 0.3353(8) 0.6380(11) 0.3609(5) 0.137(5) Uani 1 1 d . . . H50A H 0.2273 0.6015 0.3283 0.164 Uiso 1 1 calc R . . H50B H 0.3979 0.6280 0.3113 0.164 Uiso 1 1 calc R . . Cl50 Cl 0.4019(3) 0.8216(3) 0.41123(17) 0.1071(9) Uani 1 1 d . . . Cl51 Cl 0.34586(17) 0.54944(16) 0.44044(15) 0.0796(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00926(9) 0.01200(9) 0.00965(10) 0.00121(6) 0.00194(6) 0.00446(7) Cl1 0.0179(4) 0.0225(4) 0.0144(4) 0.0043(3) 0.0032(3) 0.0124(3) P1 0.0109(4) 0.0120(4) 0.0109(4) 0.0020(3) 0.0025(3) 0.0047(3) C1 0.0171(16) 0.0120(15) 0.0088(15) -0.0002(12) 0.0014(13) 0.0052(13) C2 0.0206(17) 0.0189(17) 0.0109(16) 0.0014(13) 0.0020(13) 0.0099(14) C3 0.033(2) 0.0207(18) 0.0163(18) 0.0064(15) 0.0057(16) 0.0163(16) C4 0.037(2) 0.0151(17) 0.0168(18) 0.0064(14) 0.0030(16) 0.0094(16) C5 0.0230(18) 0.0164(17) 0.0183(18) 0.0050(14) 0.0035(15) 0.0029(15) C6 0.0194(17) 0.0158(16) 0.0109(16) 0.0019(13) 0.0016(13) 0.0053(14) C7 0.0159(16) 0.0131(16) 0.0217(19) 0.0048(14) 0.0058(14) 0.0032(13) C8 0.0174(18) 0.0225(19) 0.033(2) 0.0070(17) 0.0015(16) 0.0038(15) C9 0.027(2) 0.0236(19) 0.030(2) 0.0040(17) 0.0140(17) 0.0073(17) C10 0.0136(15) 0.0156(16) 0.0112(16) 0.0032(13) 0.0044(12) 0.0072(13) C11 0.0163(16) 0.0174(16) 0.0151(17) 0.0036(14) 0.0035(13) 0.0070(14) C12 0.0194(18) 0.0259(19) 0.0162(18) 0.0011(15) -0.0012(14) 0.0099(15) C13 0.029(2) 0.031(2) 0.0198(19) 0.0103(16) 0.0014(16) 0.0147(17) C14 0.029(2) 0.0205(18) 0.023(2) 0.0112(15) 0.0091(16) 0.0139(16) C15 0.0153(16) 0.0158(16) 0.0148(17) 0.0021(13) 0.0058(13) 0.0071(13) C16 0.0185(17) 0.0119(16) 0.0219(19) 0.0021(14) 0.0071(15) 0.0038(14) C17 0.028(2) 0.0165(18) 0.038(2) 0.0033(17) 0.0134(18) 0.0096(16) C18 0.0201(18) 0.0179(17) 0.024(2) 0.0056(15) 0.0088(15) 0.0050(15) C19 0.0135(16) 0.0153(16) 0.0154(17) 0.0045(13) 0.0037(13) 0.0070(13) C20 0.0169(17) 0.0183(17) 0.0146(17) 0.0028(14) 0.0042(13) 0.0080(14) C21 0.0144(16) 0.0203(17) 0.0194(18) 0.0038(14) 0.0016(14) 0.0063(14) C22 0.0159(17) 0.0256(19) 0.024(2) 0.0076(16) 0.0064(15) 0.0115(15) C23 0.0239(19) 0.0229(18) 0.0184(18) 0.0051(15) 0.0097(15) 0.0147(15) C24 0.0180(16) 0.0147(16) 0.0132(16) 0.0045(13) 0.0037(13) 0.0092(13) C25 0.0200(17) 0.0173(17) 0.0122(16) 0.0012(13) 0.0032(13) 0.0098(14) C26 0.0263(19) 0.0255(19) 0.0137(18) 0.0036(15) 0.0057(15) 0.0132(16) C27 0.028(2) 0.0208(18) 0.0195(19) 0.0000(15) 0.0023(15) 0.0133(16) C50 0.043(4) 0.215(11) 0.037(4) -0.045(5) 0.006(3) -0.039(5) Cl50 0.1090(15) 0.190(2) 0.1230(17) 0.1195(18) 0.0882(14) 0.1210(17) Cl51 0.0426(8) 0.0567(9) 0.1057(14) -0.0372(9) 0.0098(8) 0.0042(7) _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 Pt1 Cl1 2.3039(10) 2 ? Pt1 Cl1 2.3039(10) . ? Pt1 P1 2.3436(11) 2 ? Pt1 P1 2.3436(11) . ? P1 C10 1.839(3) . ? P1 C19 1.846(3) . ? P1 C1 1.850(3) . ? C1 C2 1.393(5) . ? C1 C6 1.411(5) . ? C2 C3 1.384(5) . ? C3 C4 1.386(5) . ? C4 C5 1.380(6) . ? C5 C6 1.404(5) . ? C6 C7 1.520(5) . ? C7 C9 1.524(5) . ? C7 C8 1.537(5) . ? C10 C11 1.400(5) . ? C10 C15 1.415(5) . ? C11 C12 1.380(5) . ? C12 C13 1.382(5) . ? C13 C14 1.381(6) . ? C14 C15 1.382(5) . ? C15 C16 1.521(5) . ? C16 C17 1.530(5) . ? C16 C18 1.539(5) . ? C19 C20 1.398(5) . ? C19 C24 1.409(5) . ? C20 C21 1.393(5) . ? C21 C22 1.376(5) . ? C22 C23 1.385(5) . ? C23 C24 1.405(5) . ? C24 C25 1.524(5) . ? C25 C26 1.532(5) . ? C25 C27 1.535(5) . ? C50 Cl51 1.612(11) . ? C50 Cl50 1.872(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pt1 Cl1 180.00(5) 2 . ? Cl1 Pt1 P1 92.29(4) 2 2 ? Cl1 Pt1 P1 87.71(4) . 2 ? Cl1 Pt1 P1 87.71(4) 2 . ? Cl1 Pt1 P1 92.29(4) . . ? P1 Pt1 P1 180.00(4) 2 . ? C10 P1 C19 100.78(15) . . ? C10 P1 C1 110.34(15) . . ? C19 P1 C1 104.84(15) . . ? C10 P1 Pt1 116.60(11) . . ? C19 P1 Pt1 117.18(12) . . ? C1 P1 Pt1 106.49(11) . . ? C2 C1 C6 119.1(3) . . ? C2 C1 P1 115.6(2) . . ? C6 C1 P1 124.7(3) . . ? C3 C2 C1 122.2(3) . . ? C2 C3 C4 119.1(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 122.6(3) . . ? C5 C6 C1 117.5(3) . . ? C5 C6 C7 116.8(3) . . ? C1 C6 C7 125.7(3) . . ? C6 C7 C9 109.8(3) . . ? C6 C7 C8 112.7(3) . . ? C9 C7 C8 108.7(3) . . ? C11 C10 C15 118.9(3) . . ? C11 C10 P1 119.2(2) . . ? C15 C10 P1 121.8(3) . . ? C12 C11 C10 121.6(3) . . ? C11 C12 C13 119.5(4) . . ? C14 C13 C12 119.4(4) . . ? C13 C14 C15 122.7(3) . . ? C14 C15 C10 117.9(3) . . ? C14 C15 C16 118.5(3) . . ? C10 C15 C16 123.7(3) . . ? C15 C16 C17 111.7(3) . . ? C15 C16 C18 111.0(3) . . ? C17 C16 C18 109.7(3) . . ? C20 C19 C24 119.6(3) . . ? C20 C19 P1 116.4(3) . . ? C24 C19 P1 123.7(3) . . ? C21 C20 C19 121.1(3) . . ? C22 C21 C20 119.8(3) . . ? C21 C22 C23 119.6(3) . . ? C22 C23 C24 122.2(3) . . ? C23 C24 C19 117.6(3) . . ? C23 C24 C25 117.3(3) . . ? C19 C24 C25 125.1(3) . . ? C24 C25 C26 111.5(3) . . ? C24 C25 C27 111.4(3) . . ? C26 C25 C27 110.6(3) . . ? Cl51 C50 Cl50 114.3(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.260 _refine_diff_density_min -1.967 _refine_diff_density_rms 0.130 data_3b.4CH2Cl2(taliesins) _database_code_depnum_ccdc_archive 'CCDC 254103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Cl2 O6 P2 Pd, 4(C H2 Cl2)' _chemical_formula_sum 'C52 H62 Cl10 O6 P2 Pd' _chemical_formula_weight 1305.86 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' 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 11.035(2) _cell_length_b 12.020(2) _cell_length_c 12.441(3) _cell_angle_alpha 63.49(3) _cell_angle_beta 77.64(3) _cell_angle_gamma 89.59(3) _cell_volume 1435.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3450 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16217 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6547 _reflns_number_gt 5511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0482P)^2^+3.8525P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6547 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Pd1 Pd 1.0000 1.0000 0.5000 0.01039(12) Uani 1 2 d S . . Cl1 Cl 0.83714(9) 0.93875(9) 0.67221(9) 0.0165(2) Uani 1 1 d . . . P1 P 0.96623(10) 0.81709(9) 0.48030(10) 0.0124(2) Uani 1 1 d . . . Cl2 Cl 0.59685(11) 0.10639(11) 0.27200(11) 0.0284(3) Uani 1 1 d . . . Cl5 Cl -0.00424(12) 0.35762(13) -0.01745(13) 0.0351(3) Uani 1 1 d . . . Cl4 Cl 0.26467(12) 0.41531(14) -0.06407(13) 0.0388(3) Uani 1 1 d . . . Cl3 Cl 0.50019(14) -0.01887(14) 0.14938(14) 0.0437(4) Uani 1 1 d . . . O3 O 0.8041(3) 0.9254(3) 0.0171(3) 0.0198(6) Uani 1 1 d . . . C18 C 0.9208(4) 0.9695(4) 0.2521(4) 0.0138(8) Uani 1 1 d . . . H18 H 0.9482 1.0341 0.2682 0.017 Uiso 1 1 calc R . . O2 O 1.4780(3) 0.6485(3) 0.4355(3) 0.0231(7) Uani 1 1 d . . . C17 C 0.9220(4) 0.8454(4) 0.3380(4) 0.0128(8) Uani 1 1 d . . . C22 C 0.8803(4) 0.7481(4) 0.3147(4) 0.0145(8) Uani 1 1 d . . . C11 C 1.2865(4) 0.6899(4) 0.3606(4) 0.0173(8) Uani 1 1 d . . . H11 H 1.3201 0.6751 0.2917 0.021 Uiso 1 1 calc R . . C1 C 0.8440(4) 0.7021(4) 0.6025(4) 0.0131(8) Uani 1 1 d . . . C7 C 0.6758(4) 0.8419(4) 0.5150(4) 0.0177(9) Uani 1 1 d . . . H7A H 0.6778 0.8314 0.4409 0.026 Uiso 1 1 calc R . . H7B H 0.7320 0.9155 0.4932 0.026 Uiso 1 1 calc R . . H7C H 0.5907 0.8533 0.5490 0.026 Uiso 1 1 calc R . . C10 C 1.1668(4) 0.7245(4) 0.3781(4) 0.0167(8) Uani 1 1 d . . . H10 H 1.1196 0.7346 0.3194 0.020 Uiso 1 1 calc R . . C6 C 0.7173(4) 0.7275(4) 0.6100(4) 0.0157(8) Uani 1 1 d . . . C12 C 1.3574(4) 0.6768(4) 0.4449(4) 0.0168(8) Uani 1 1 d . . . C19 C 0.8812(4) 1.0019(4) 0.1447(4) 0.0153(8) Uani 1 1 d . . . H19 H 0.8801 1.0872 0.0887 0.018 Uiso 1 1 calc R . . C2 C 0.8732(4) 0.5907(4) 0.6929(4) 0.0163(8) Uani 1 1 d . . . H2 H 0.9578 0.5735 0.6875 0.020 Uiso 1 1 calc R . . C13 C 1.3042(4) 0.6942(4) 0.5476(4) 0.0176(9) Uani 1 1 d . . . H13 H 1.3517 0.6826 0.6065 0.021 Uiso 1 1 calc R . . C20 C 0.8430(4) 0.9070(4) 0.1200(4) 0.0162(8) Uani 1 1 d . . . C23 C 0.8717(4) 0.6107(4) 0.4019(4) 0.0196(9) Uani 1 1 d . . . H23A H 0.7962 0.5874 0.4685 0.029 Uiso 1 1 calc R . . H23B H 0.9452 0.5930 0.4371 0.029 Uiso 1 1 calc R . . H23C H 0.8682 0.5622 0.3566 0.029 Uiso 1 1 calc R . . C9 C 1.1132(4) 0.7450(3) 0.4787(4) 0.0138(8) Uani 1 1 d . . . C21 C 0.8427(4) 0.7820(4) 0.2058(4) 0.0152(8) Uani 1 1 d . . . H21 H 0.8158 0.7180 0.1886 0.018 Uiso 1 1 calc R . . O1 O 0.5590(3) 0.4562(3) 0.8876(3) 0.0264(7) Uani 1 1 d . . . C3 C 0.7814(4) 0.5048(4) 0.7901(4) 0.0194(9) Uani 1 1 d . . . H3 H 0.8030 0.4294 0.8499 0.023 Uiso 1 1 calc R . . C5 C 0.6279(4) 0.6419(4) 0.7075(4) 0.0182(9) Uani 1 1 d . . . H5 H 0.5430 0.6585 0.7136 0.022 Uiso 1 1 calc R . . C14 C 1.1835(4) 0.7283(4) 0.5667(4) 0.0163(8) Uani 1 1 d . . . C4 C 0.6577(4) 0.5302(4) 0.7988(4) 0.0199(9) Uani 1 1 d . . . C24 C 0.8023(4) 1.0518(4) -0.0731(4) 0.0208(9) Uani 1 1 d . . . H24A H 0.7425 1.0933 -0.0365 0.031 Uiso 1 1 calc R . . H24B H 0.7775 1.0521 -0.1442 0.031 Uiso 1 1 calc R . . H24C H 0.8856 1.0964 -0.1001 0.031 Uiso 1 1 calc R . . C16 C 1.5318(4) 0.6211(5) 0.3355(5) 0.0259(10) Uani 1 1 d . . . H16A H 1.4805 0.5518 0.3407 0.039 Uiso 1 1 calc R . . H16B H 1.6163 0.5975 0.3408 0.039 Uiso 1 1 calc R . . H16C H 1.5353 0.6951 0.2567 0.039 Uiso 1 1 calc R . . C26 C 0.1313(5) 0.3188(5) 0.0418(5) 0.0272(10) Uani 1 1 d . . . H26A H 0.1189 0.3270 0.1190 0.033 Uiso 1 1 calc R . . H26B H 0.1439 0.2307 0.0620 0.033 Uiso 1 1 calc R . . C8 C 0.5833(5) 0.3460(4) 0.9886(5) 0.0297(11) Uani 1 1 d . . . H8A H 0.6181 0.2872 0.9583 0.044 Uiso 1 1 calc R . . H8B H 0.5053 0.3068 1.0512 0.044 Uiso 1 1 calc R . . H8C H 0.6431 0.3689 1.0252 0.044 Uiso 1 1 calc R . . C25 C 0.4820(5) -0.0042(5) 0.2852(5) 0.0345(12) Uani 1 1 d . . . H25A H 0.4874 -0.0864 0.3541 0.041 Uiso 1 1 calc R . . H25B H 0.3983 0.0219 0.3051 0.041 Uiso 1 1 calc R . . C15 C 1.1358(4) 0.7490(4) 0.6779(4) 0.0216(9) Uani 1 1 d . . . H15A H 1.1518 0.6785 0.7513 0.032 Uiso 1 1 calc R . . H15B H 1.0459 0.7559 0.6890 0.032 Uiso 1 1 calc R . . H15C H 1.1785 0.8263 0.6660 0.032 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 0.0096(2) 0.0104(2) 0.0133(2) -0.00622(17) -0.00519(16) 0.00163(15) Cl1 0.0132(5) 0.0194(5) 0.0183(5) -0.0103(4) -0.0027(4) -0.0005(4) P1 0.0111(5) 0.0126(5) 0.0151(5) -0.0068(4) -0.0052(4) 0.0016(4) Cl2 0.0237(6) 0.0265(6) 0.0340(7) -0.0123(5) -0.0082(5) 0.0043(5) Cl5 0.0261(6) 0.0416(7) 0.0485(8) -0.0285(6) -0.0123(6) 0.0064(5) Cl4 0.0275(7) 0.0506(8) 0.0440(8) -0.0314(7) 0.0027(6) -0.0120(6) Cl3 0.0390(8) 0.0512(8) 0.0377(8) -0.0212(7) 0.0005(6) -0.0156(6) O3 0.0224(17) 0.0221(16) 0.0176(15) -0.0089(13) -0.0105(13) 0.0025(13) C18 0.0102(19) 0.0151(19) 0.018(2) -0.0087(16) -0.0035(16) 0.0004(15) O2 0.0132(15) 0.0292(17) 0.0313(18) -0.0161(15) -0.0085(13) 0.0059(13) C17 0.0115(19) 0.0140(19) 0.016(2) -0.0085(16) -0.0066(16) 0.0036(15) C22 0.0075(19) 0.0155(19) 0.020(2) -0.0074(16) -0.0038(16) 0.0004(15) C11 0.015(2) 0.019(2) 0.019(2) -0.0092(17) -0.0030(17) 0.0007(16) C1 0.0122(19) 0.0129(18) 0.0145(19) -0.0053(16) -0.0057(15) -0.0009(15) C7 0.013(2) 0.022(2) 0.016(2) -0.0051(17) -0.0056(16) 0.0023(16) C10 0.015(2) 0.0156(19) 0.018(2) -0.0059(17) -0.0064(17) 0.0010(15) C6 0.019(2) 0.0119(19) 0.018(2) -0.0076(16) -0.0079(17) 0.0015(16) C12 0.012(2) 0.0148(19) 0.023(2) -0.0074(17) -0.0060(17) 0.0012(15) C19 0.016(2) 0.0105(18) 0.017(2) -0.0041(16) -0.0045(16) 0.0015(15) C2 0.017(2) 0.0110(18) 0.024(2) -0.0090(17) -0.0073(17) 0.0003(15) C13 0.014(2) 0.018(2) 0.025(2) -0.0097(18) -0.0110(17) 0.0012(16) C20 0.010(2) 0.023(2) 0.016(2) -0.0096(17) -0.0040(16) 0.0028(16) C23 0.023(2) 0.015(2) 0.022(2) -0.0075(18) -0.0101(18) -0.0001(17) C9 0.014(2) 0.0091(18) 0.017(2) -0.0040(15) -0.0061(16) -0.0010(14) C21 0.013(2) 0.017(2) 0.019(2) -0.0115(17) -0.0044(16) -0.0017(15) O1 0.0174(17) 0.0259(17) 0.0245(17) -0.0026(14) -0.0020(13) -0.0042(13) C3 0.021(2) 0.014(2) 0.021(2) -0.0055(17) -0.0062(18) 0.0016(16) C5 0.013(2) 0.020(2) 0.023(2) -0.0107(18) -0.0071(17) 0.0030(16) C14 0.017(2) 0.0120(19) 0.021(2) -0.0069(16) -0.0082(17) 0.0006(15) C4 0.019(2) 0.019(2) 0.019(2) -0.0079(18) -0.0033(17) -0.0035(17) C24 0.018(2) 0.022(2) 0.019(2) -0.0042(18) -0.0081(17) 0.0040(17) C16 0.016(2) 0.029(2) 0.035(3) -0.017(2) -0.004(2) 0.0050(18) C26 0.027(3) 0.030(3) 0.025(3) -0.013(2) -0.008(2) 0.000(2) C8 0.032(3) 0.020(2) 0.025(3) -0.0017(19) -0.003(2) -0.006(2) C25 0.016(2) 0.052(3) 0.030(3) -0.014(2) -0.005(2) -0.006(2) C15 0.021(2) 0.026(2) 0.028(2) -0.017(2) -0.0141(19) 0.0106(18) _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 Cl1 2.3076(14) . ? Pd1 Cl1 2.3076(14) 2_776 ? Pd1 P1 2.3589(11) . ? Pd1 P1 2.3589(11) 2_776 ? P1 C1 1.821(4) . ? P1 C17 1.822(4) . ? P1 C9 1.834(4) . ? Cl2 C25 1.771(5) . ? Cl5 C26 1.775(5) . ? Cl4 C26 1.754(5) . ? Cl3 C25 1.746(6) . ? O3 C20 1.360(5) . ? O3 C24 1.434(5) . ? C18 C19 1.383(6) . ? C18 C17 1.397(5) . ? C18 H18 0.9500 . ? O2 C12 1.365(5) . ? O2 C16 1.434(6) . ? C17 C22 1.424(5) . ? C22 C21 1.385(6) . ? C22 C23 1.508(6) . ? C11 C10 1.384(6) . ? C11 C12 1.393(6) . ? C11 H11 0.9500 . ? C1 C2 1.402(6) . ? C1 C6 1.420(6) . ? C7 C6 1.507(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C10 C9 1.390(6) . ? C10 H10 0.9500 . ? C6 C5 1.376(6) . ? C12 C13 1.391(6) . ? C19 C20 1.396(6) . ? C19 H19 0.9500 . ? C2 C3 1.390(6) . ? C2 H2 0.9500 . ? C13 C14 1.393(6) . ? C13 H13 0.9500 . ? C20 C21 1.401(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C9 C14 1.416(6) . ? C21 H21 0.9500 . ? O1 C4 1.349(5) . ? O1 C8 1.435(6) . ? C3 C4 1.389(6) . ? C3 H3 0.9500 . ? C5 C4 1.412(6) . ? C5 H5 0.9500 . ? C14 C15 1.500(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 Cl1 Pd1 Cl1 180.000(1) . 2_776 ? Cl1 Pd1 P1 93.21(5) . . ? Cl1 Pd1 P1 86.79(5) 2_776 . ? Cl1 Pd1 P1 86.79(5) . 2_776 ? Cl1 Pd1 P1 93.21(5) 2_776 2_776 ? P1 Pd1 P1 180.00(5) . 2_776 ? C1 P1 C17 104.41(19) . . ? C1 P1 C9 108.73(18) . . ? C17 P1 C9 106.94(19) . . ? C1 P1 Pd1 114.81(14) . . ? C17 P1 Pd1 113.93(13) . . ? C9 P1 Pd1 107.66(13) . . ? C20 O3 C24 117.7(3) . . ? C19 C18 C17 122.5(4) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C12 O2 C16 116.7(3) . . ? C18 C17 C22 119.0(4) . . ? C18 C17 P1 117.5(3) . . ? C22 C17 P1 123.4(3) . . ? C21 C22 C17 117.9(4) . . ? C21 C22 C23 117.7(4) . . ? C17 C22 C23 124.4(4) . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C2 C1 C6 119.2(4) . . ? C2 C1 P1 120.9(3) . . ? C6 C1 P1 119.8(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C10 C9 122.3(4) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C5 C6 C1 118.3(4) . . ? C5 C6 C7 118.4(4) . . ? C1 C6 C7 123.3(4) . . ? O2 C12 C13 115.7(4) . . ? O2 C12 C11 125.2(4) . . ? C13 C12 C11 119.1(4) . . ? C18 C19 C20 118.8(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C3 C2 C1 121.6(4) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C12 C13 C14 122.1(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? O3 C20 C19 125.0(4) . . ? O3 C20 C21 115.7(4) . . ? C19 C20 C21 119.3(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C10 C9 C14 118.6(4) . . ? C10 C9 P1 119.1(3) . . ? C14 C9 P1 121.5(3) . . ? C22 C21 C20 122.6(4) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C4 O1 C8 117.7(4) . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C6 C5 C4 122.3(4) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C13 C14 C9 118.6(4) . . ? C13 C14 C15 118.2(4) . . ? C9 C14 C15 123.2(4) . . ? O1 C4 C3 126.0(4) . . ? O1 C4 C5 114.8(4) . . ? C3 C4 C5 119.2(4) . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl4 C26 Cl5 112.0(3) . . ? Cl4 C26 H26A 109.2 . . ? Cl5 C26 H26A 109.2 . . ? Cl4 C26 H26B 109.2 . . ? Cl5 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Cl3 C25 Cl2 112.0(3) . . ? Cl3 C25 H25A 109.2 . . ? Cl2 C25 H25A 109.2 . . ? Cl3 C25 H25B 109.2 . . ? Cl2 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 Cl1 Pd1 P1 C1 -3.89(15) . . . . ? Cl1 Pd1 P1 C1 176.11(15) 2_776 . . . ? P1 Pd1 P1 C1 -100(100) 2_776 . . . ? Cl1 Pd1 P1 C17 116.45(15) . . . . ? Cl1 Pd1 P1 C17 -63.55(15) 2_776 . . . ? P1 Pd1 P1 C17 20(100) 2_776 . . . ? Cl1 Pd1 P1 C9 -125.13(14) . . . . ? Cl1 Pd1 P1 C9 54.87(14) 2_776 . . . ? P1 Pd1 P1 C9 139(100) 2_776 . . . ? C19 C18 C17 C22 -0.4(6) . . . . ? C19 C18 C17 P1 -175.8(3) . . . . ? C1 P1 C17 C18 130.3(3) . . . . ? C9 P1 C17 C18 -114.5(3) . . . . ? Pd1 P1 C17 C18 4.3(4) . . . . ? C1 P1 C17 C22 -44.9(4) . . . . ? C9 P1 C17 C22 70.3(4) . . . . ? Pd1 P1 C17 C22 -170.9(3) . . . . ? C18 C17 C22 C21 1.3(6) . . . . ? P1 C17 C22 C21 176.5(3) . . . . ? C18 C17 C22 C23 -177.3(4) . . . . ? P1 C17 C22 C23 -2.2(6) . . . . ? C17 P1 C1 C2 127.1(3) . . . . ? C9 P1 C1 C2 13.2(4) . . . . ? Pd1 P1 C1 C2 -107.4(3) . . . . ? C17 P1 C1 C6 -55.7(4) . . . . ? C9 P1 C1 C6 -169.5(3) . . . . ? Pd1 P1 C1 C6 69.8(3) . . . . ? C12 C11 C10 C9 -1.1(6) . . . . ? C2 C1 C6 C5 0.9(6) . . . . ? P1 C1 C6 C5 -176.4(3) . . . . ? C2 C1 C6 C7 -177.5(4) . . . . ? P1 C1 C6 C7 5.2(5) . . . . ? C16 O2 C12 C13 175.5(4) . . . . ? C16 O2 C12 C11 -5.0(6) . . . . ? C10 C11 C12 O2 -177.0(4) . . . . ? C10 C11 C12 C13 2.5(6) . . . . ? C17 C18 C19 C20 -1.1(6) . . . . ? C6 C1 C2 C3 -0.4(6) . . . . ? P1 C1 C2 C3 176.9(3) . . . . ? O2 C12 C13 C14 177.5(4) . . . . ? C11 C12 C13 C14 -2.1(6) . . . . ? C24 O3 C20 C19 0.1(6) . . . . ? C24 O3 C20 C21 179.8(4) . . . . ? C18 C19 C20 O3 -178.8(4) . . . . ? C18 C19 C20 C21 1.6(6) . . . . ? C11 C10 C9 C14 -0.8(6) . . . . ? C11 C10 C9 P1 169.2(3) . . . . ? C1 P1 C9 C10 112.7(3) . . . . ? C17 P1 C9 C10 0.5(4) . . . . ? Pd1 P1 C9 C10 -122.3(3) . . . . ? C1 P1 C9 C14 -77.6(4) . . . . ? C17 P1 C9 C14 170.2(3) . . . . ? Pd1 P1 C9 C14 47.4(3) . . . . ? C17 C22 C21 C20 -0.8(6) . . . . ? C23 C22 C21 C20 177.9(4) . . . . ? O3 C20 C21 C22 179.7(4) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C1 C6 C5 C4 -0.5(6) . . . . ? C7 C6 C5 C4 178.0(4) . . . . ? C12 C13 C14 C9 0.2(6) . . . . ? C12 C13 C14 C15 -178.0(4) . . . . ? C10 C9 C14 C13 1.2(6) . . . . ? P1 C9 C14 C13 -168.6(3) . . . . ? C10 C9 C14 C15 179.3(4) . . . . ? P1 C9 C14 C15 9.6(6) . . . . ? C8 O1 C4 C3 5.7(7) . . . . ? C8 O1 C4 C5 -175.2(4) . . . . ? C2 C3 C4 O1 -179.9(4) . . . . ? C2 C3 C4 C5 1.0(6) . . . . ? C6 C5 C4 O1 -179.7(4) . . . . ? C6 C5 C4 C3 -0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.364 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.128 data_c3poapex _database_code_depnum_ccdc_archive 'CCDC 254104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H76 Cl2 O6 P2 Pt2' _chemical_formula_weight 1416.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 11.359(3) _cell_length_b 11.719(3) _cell_length_c 13.130(6) _cell_angle_alpha 101.28(3) _cell_angle_beta 104.34(2) _cell_angle_gamma 112.02(3) _cell_volume 1486.5(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1081 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 18.71 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 4.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41694 _exptl_absorpt_correction_T_max 0.70925 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8236 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.1812 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6304 _reflns_number_gt 2691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0300P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6304 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1607 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 Pt1 Pt 0.10440(6) 0.17283(5) 0.09458(5) 0.0700(2) Uani 1 1 d . . . Cl1 Cl 0.1082(4) -0.0413(3) 0.0584(3) 0.1041(13) Uani 1 1 d . . . P1 P 0.2819(3) 0.2895(3) 0.2449(3) 0.0605(9) Uani 1 1 d . . . O1 O 0.0964(11) 0.3128(10) 0.6345(9) 0.123(4) Uani 1 1 d . . . O2 O 0.7740(12) 0.1937(12) 0.3700(11) 0.143(4) Uani 1 1 d . . . O3 O 0.4491(10) 0.8321(9) 0.2473(9) 0.108(3) Uani 1 1 d . . . C9 C 0.0992(14) 0.3601(11) -0.0249(10) 0.098(5) Uani 1 1 d . . . H9A H 0.1022 0.4436 -0.0297 0.147 Uiso 1 1 calc R . . H9B H 0.0122 0.2892 -0.0767 0.147 Uiso 1 1 calc R . . H9C H 0.1735 0.3498 -0.0441 0.147 Uiso 1 1 calc R . . C10 C 0.0035(14) 0.3579(14) 0.1248(14) 0.130(6) Uani 1 1 d . . . H10A H -0.0001 0.4403 0.1260 0.195 Uiso 1 1 calc R . . H10B H 0.0149 0.3483 0.1986 0.195 Uiso 1 1 calc R . . H10C H -0.0810 0.2857 0.0706 0.195 Uiso 1 1 calc R . . C11 C 0.1146(14) 0.3568(17) 0.0946(11) 0.115(6) Uani 1 1 d . . . C12 C 0.2486(12) 0.4752(12) 0.1704(10) 0.060(3) Uani 1 1 d . . . C13 C 0.2812(13) 0.6031(14) 0.1714(11) 0.074(4) Uani 1 1 d . . . H13A H 0.2168 0.6217 0.1251 0.089 Uiso 1 1 calc R . . C14 C 0.4059(16) 0.7017(13) 0.2391(12) 0.074(4) Uani 1 1 d . . . C15 C 0.4974(13) 0.6758(13) 0.3053(11) 0.081(4) Uani 1 1 d . . . H15A H 0.5847 0.7441 0.3502 0.097 Uiso 1 1 calc R . . C16 C 0.4652(12) 0.5509(13) 0.3083(10) 0.069(3) Uani 1 1 d . . . H16A H 0.5289 0.5339 0.3571 0.083 Uiso 1 1 calc R . . C17 C 0.3407(12) 0.4515(11) 0.2402(10) 0.058(3) Uani 1 1 d . . . C18 C 0.4300(12) 0.2598(10) 0.2750(12) 0.063(3) Uani 1 1 d . . . C19 C 0.4866(14) 0.2403(12) 0.1953(13) 0.080(4) Uani 1 1 d . . . C20 C 0.6060(15) 0.2206(12) 0.2307(15) 0.089(4) Uani 1 1 d . . . H20A H 0.6518 0.2120 0.1803 0.106 Uiso 1 1 calc R . . C21 C 0.6542(16) 0.2140(13) 0.3309(18) 0.104(6) Uani 1 1 d . . . C22 C 0.5983(15) 0.2324(14) 0.4149(16) 0.101(5) Uani 1 1 d . . . H22A H 0.6353 0.2313 0.4878 0.122 Uiso 1 1 calc R . . C23 C 0.4861(13) 0.2518(11) 0.3797(12) 0.077(4) Uani 1 1 d . . . H23A H 0.4415 0.2607 0.4311 0.093 Uiso 1 1 calc R . . C24 C 0.2346(10) 0.2949(11) 0.3712(9) 0.054(3) Uani 1 1 d . . . C25 C 0.1826(11) 0.1866(12) 0.4041(10) 0.063(3) Uani 1 1 d . . . C26 C 0.1658(12) 0.0535(10) 0.3455(10) 0.070(3) Uani 1 1 d . . . H26A H 0.2114 0.0636 0.2895 0.084 Uiso 1 1 calc R . . C27 C 0.2288(15) -0.0061(12) 0.4200(12) 0.111(5) Uani 1 1 d . . . H27A H 0.3255 0.0529 0.4594 0.166 Uiso 1 1 calc R . . H27B H 0.2187 -0.0890 0.3753 0.166 Uiso 1 1 calc R . . H27C H 0.1835 -0.0213 0.4740 0.166 Uiso 1 1 calc R . . C28 C 0.0142(13) -0.0382(12) 0.2815(12) 0.106(5) Uani 1 1 d . . . H28A H -0.0247 0.0010 0.2317 0.160 Uiso 1 1 calc R . . H28B H -0.0334 -0.0523 0.3342 0.160 Uiso 1 1 calc R . . H28C H 0.0040 -0.1216 0.2379 0.160 Uiso 1 1 calc R . . C29 C 0.1422(12) 0.2005(13) 0.4941(11) 0.077(4) Uani 1 1 d . . . H29A H 0.1109 0.1282 0.5198 0.092 Uiso 1 1 calc R . . C30 C 0.1456(12) 0.3176(14) 0.5497(11) 0.071(3) Uani 1 1 d . . . C31 C 0.1918(11) 0.4225(12) 0.5146(10) 0.067(3) Uani 1 1 d . . . H31A H 0.1931 0.5019 0.5502 0.080 Uiso 1 1 calc R . . C32 C 0.2363(11) 0.4115(12) 0.4277(10) 0.065(3) Uani 1 1 d . . . H32A H 0.2697 0.4852 0.4040 0.078 Uiso 1 1 calc R . . C33 C 0.3541(16) 0.8631(13) 0.1877(13) 0.116(5) Uani 1 1 d . . . H33A H 0.3956 0.9562 0.1973 0.174 Uiso 1 1 calc R . . H33B H 0.2778 0.8418 0.2144 0.174 Uiso 1 1 calc R . . H33C H 0.3214 0.8133 0.1089 0.174 Uiso 1 1 calc R . . C34 C 0.0695(19) 0.4207(15) 0.6752(15) 0.169(9) Uani 1 1 d . . . H34A H 0.0358 0.4095 0.7362 0.254 Uiso 1 1 calc R . . H34B H 0.0010 0.4240 0.6150 0.254 Uiso 1 1 calc R . . H34C H 0.1534 0.5019 0.7020 0.254 Uiso 1 1 calc R . . C35 C 0.4063(17) 0.1373(16) -0.0168(14) 0.144(7) Uani 1 1 d . . . H35A H 0.3724 0.1511 -0.0873 0.217 Uiso 1 1 calc R . . H35B H 0.3375 0.0581 -0.0135 0.217 Uiso 1 1 calc R . . H35C H 0.4897 0.1280 -0.0112 0.217 Uiso 1 1 calc R . . C36 C 0.5364(19) 0.3700(17) 0.0679(15) 0.160(7) Uani 1 1 d . . . H36A H 0.5558 0.4476 0.1266 0.240 Uiso 1 1 calc R . . H36B H 0.4995 0.3780 -0.0048 0.240 Uiso 1 1 calc R . . H36C H 0.6203 0.3616 0.0740 0.240 Uiso 1 1 calc R . . C37 C 0.4363(17) 0.2538(15) 0.0798(14) 0.107(5) Uani 1 1 d . . . H37A H 0.3508 0.2633 0.0711 0.129 Uiso 1 1 calc R . . C38 C 0.8204(19) 0.166(2) 0.2881(17) 0.181(9) Uani 1 1 d . . . H38A H 0.9010 0.1531 0.3178 0.272 Uiso 1 1 calc R . . H38B H 0.8441 0.2376 0.2574 0.272 Uiso 1 1 calc R . . H38C H 0.7497 0.0860 0.2293 0.272 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 Pt1 0.0896(4) 0.0696(3) 0.0480(3) 0.0149(2) 0.0091(2) 0.0443(3) Cl1 0.114(3) 0.092(3) 0.085(3) 0.020(2) -0.002(2) 0.052(2) P1 0.074(2) 0.058(2) 0.053(2) 0.0151(16) 0.0189(18) 0.0356(18) O1 0.179(10) 0.114(8) 0.106(9) 0.044(7) 0.095(8) 0.063(8) O2 0.122(9) 0.172(11) 0.144(12) 0.043(9) 0.045(9) 0.081(9) O3 0.126(8) 0.088(7) 0.120(9) 0.046(6) 0.034(7) 0.059(7) C9 0.137(12) 0.071(9) 0.062(10) 0.023(7) 0.006(9) 0.039(9) C10 0.088(11) 0.106(12) 0.148(17) 0.024(11) 0.010(11) 0.025(10) C11 0.060(9) 0.213(18) 0.041(9) -0.004(10) 0.009(7) 0.058(11) C12 0.070(9) 0.076(9) 0.052(8) 0.028(7) 0.029(7) 0.041(8) C13 0.076(9) 0.086(10) 0.065(10) 0.018(8) 0.017(8) 0.049(9) C14 0.104(12) 0.067(10) 0.071(10) 0.032(8) 0.043(9) 0.048(9) C15 0.074(9) 0.084(10) 0.059(10) 0.012(8) 0.013(8) 0.021(8) C16 0.070(9) 0.084(10) 0.067(9) 0.041(8) 0.017(7) 0.045(8) C17 0.053(7) 0.076(8) 0.059(8) 0.024(7) 0.028(7) 0.038(7) C18 0.075(9) 0.049(7) 0.079(10) 0.022(7) 0.040(8) 0.033(7) C19 0.095(11) 0.074(9) 0.086(12) 0.032(8) 0.038(9) 0.047(8) C20 0.094(11) 0.077(10) 0.111(14) 0.027(9) 0.054(11) 0.044(9) C21 0.077(12) 0.069(10) 0.136(18) 0.028(11) -0.005(12) 0.032(9) C22 0.081(11) 0.125(13) 0.119(16) 0.053(12) 0.039(11) 0.059(10) C23 0.079(9) 0.090(10) 0.070(10) 0.028(8) 0.021(8) 0.047(8) C24 0.046(7) 0.055(8) 0.050(8) 0.017(6) 0.011(6) 0.013(6) C25 0.054(7) 0.066(9) 0.055(9) 0.019(7) 0.014(6) 0.018(7) C26 0.091(10) 0.048(8) 0.072(10) 0.019(7) 0.039(8) 0.025(8) C27 0.179(15) 0.089(11) 0.097(13) 0.043(9) 0.065(12) 0.076(11) C28 0.112(12) 0.067(9) 0.120(14) 0.008(9) 0.058(11) 0.019(9) C29 0.082(9) 0.086(10) 0.074(10) 0.041(9) 0.043(8) 0.032(8) C30 0.078(9) 0.083(10) 0.057(9) 0.020(8) 0.037(8) 0.035(8) C31 0.082(9) 0.064(8) 0.054(9) 0.014(7) 0.032(7) 0.031(7) C32 0.080(9) 0.069(9) 0.052(9) 0.025(7) 0.022(7) 0.036(7) C33 0.153(15) 0.099(11) 0.129(16) 0.049(11) 0.064(13) 0.074(12) C34 0.26(2) 0.116(13) 0.154(19) 0.005(13) 0.147(18) 0.079(15) C35 0.182(17) 0.167(17) 0.108(15) 0.034(13) 0.096(14) 0.078(15) C36 0.22(2) 0.170(18) 0.145(19) 0.085(15) 0.105(17) 0.098(17) C37 0.147(14) 0.099(12) 0.112(15) 0.047(11) 0.093(13) 0.056(11) C38 0.170(18) 0.23(2) 0.134(19) -0.009(16) 0.072(16) 0.103(17) _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 Pt1 C11 2.115(18) . ? Pt1 P1 2.177(3) . ? Pt1 Cl1 2.416(4) 2 ? Pt1 Cl1 2.480(4) . ? Cl1 Pt1 2.416(4) 2 ? P1 C17 1.780(12) . ? P1 C18 1.808(12) . ? P1 C24 1.862(12) . ? O1 C30 1.365(14) . ? O1 C34 1.444(15) . ? O2 C38 1.348(18) . ? O2 C21 1.454(17) . ? O3 C33 1.376(14) . ? O3 C14 1.391(14) . ? C9 C11 1.545(17) . ? C10 C11 1.416(17) . ? C11 C12 1.535(17) . ? C12 C17 1.363(14) . ? C12 C13 1.400(15) . ? C13 C14 1.371(16) . ? C14 C15 1.348(15) . ? C15 C16 1.380(15) . ? C16 C17 1.374(14) . ? C18 C19 1.382(16) . ? C18 C23 1.403(16) . ? C19 C20 1.440(17) . ? C19 C37 1.544(19) . ? C20 C21 1.324(19) . ? C21 C22 1.42(2) . ? C22 C23 1.363(16) . ? C24 C25 1.388(14) . ? C24 C32 1.413(14) . ? C25 C29 1.372(15) . ? C25 C26 1.516(15) . ? C26 C27 1.501(15) . ? C26 C28 1.539(15) . ? C29 C30 1.405(16) . ? C30 C31 1.363(15) . ? C31 C32 1.360(15) . ? C35 C37 1.532(19) . ? C36 C37 1.477(18) . ? 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 C11 Pt1 P1 82.5(4) . . ? C11 Pt1 Cl1 97.6(4) . 2 ? P1 Pt1 Cl1 173.32(14) . 2 ? C11 Pt1 Cl1 167.3(4) . . ? P1 Pt1 Cl1 101.67(12) . . ? Cl1 Pt1 Cl1 79.65(13) 2 . ? Pt1 Cl1 Pt1 100.35(13) 2 . ? C17 P1 C18 105.5(5) . . ? C17 P1 C24 105.2(5) . . ? C18 P1 C24 105.7(6) . . ? C17 P1 Pt1 105.4(4) . . ? C18 P1 Pt1 122.4(4) . . ? C24 P1 Pt1 111.3(3) . . ? C30 O1 C34 115.3(12) . . ? C38 O2 C21 112.0(17) . . ? C33 O3 C14 116.1(11) . . ? C10 C11 C12 111.8(12) . . ? C10 C11 C9 113.0(13) . . ? C12 C11 C9 105.9(12) . . ? C10 C11 Pt1 103.9(12) . . ? C12 C11 Pt1 116.1(9) . . ? C9 C11 Pt1 106.2(9) . . ? C17 C12 C13 119.0(12) . . ? C17 C12 C11 116.6(12) . . ? C13 C12 C11 124.5(12) . . ? C14 C13 C12 120.1(12) . . ? C15 C14 C13 120.1(12) . . ? C15 C14 O3 114.8(14) . . ? C13 C14 O3 125.0(13) . . ? C14 C15 C16 120.6(12) . . ? C17 C16 C15 119.7(11) . . ? C12 C17 C16 120.6(11) . . ? C12 C17 P1 115.4(9) . . ? C16 C17 P1 123.8(9) . . ? C19 C18 C23 119.1(12) . . ? C19 C18 P1 121.2(11) . . ? C23 C18 P1 119.6(10) . . ? C18 C19 C20 115.6(13) . . ? C18 C19 C37 122.8(13) . . ? C20 C19 C37 121.2(14) . . ? C21 C20 C19 122.4(15) . . ? C20 C21 C22 123.7(16) . . ? C20 C21 O2 124(2) . . ? C22 C21 O2 112.0(17) . . ? C23 C22 C21 112.8(16) . . ? C22 C23 C18 126.3(14) . . ? C25 C24 C32 118.6(11) . . ? C25 C24 P1 123.3(9) . . ? C32 C24 P1 117.6(9) . . ? C29 C25 C24 118.1(11) . . ? C29 C25 C26 118.0(12) . . ? C24 C25 C26 123.9(11) . . ? C27 C26 C25 114.6(11) . . ? C27 C26 C28 110.5(11) . . ? C25 C26 C28 109.6(10) . . ? C25 C29 C30 122.4(12) . . ? C31 C30 O1 125.8(13) . . ? C31 C30 C29 119.4(12) . . ? O1 C30 C29 114.7(13) . . ? C32 C31 C30 118.9(11) . . ? C31 C32 C24 122.6(11) . . ? C36 C37 C35 106.8(13) . . ? C36 C37 C19 111.6(14) . . ? C35 C37 C19 113.8(13) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.408 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.129 data_4c.4CHCl3(averys) _database_code_depnum_ccdc_archive 'CCDC 254105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H66 Cl4 P2 Pd2, 4(C H Cl3)' _chemical_formula_sum 'C58 H70 Cl16 P2 Pd2' _chemical_formula_weight 1609.08 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' 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' P P 0.1023 0.0942 '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 12.189(3) _cell_length_b 12.331(3) _cell_length_c 12.420(3) _cell_angle_alpha 90.563(4) _cell_angle_beta 94.222(4) _cell_angle_gamma 111.771(4) _cell_volume 1727.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2796 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.5895 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18068 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1782 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.57 _reflns_number_total 7821 _reflns_number_gt 4050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7821 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1642 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.2136 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.02040(6) 0.11263(6) 0.41123(5) 0.0174(2) Uani 1 1 d . . . Cl1 Cl 0.13970(18) 0.03013(19) 0.50501(18) 0.0252(5) Uani 1 1 d . . . P1 P 0.17152(19) 0.25101(18) 0.33955(18) 0.0181(5) Uani 1 1 d . . . Cl2 Cl -0.10744(18) 0.19555(19) 0.33813(18) 0.0253(5) Uani 1 1 d . . . Cl5 Cl 0.2499(3) 0.1034(3) 0.8345(3) 0.0547(8) Uani 1 1 d . . . Cl6 Cl 0.4206(3) 0.1381(3) 0.6752(2) 0.0583(8) Uani 1 1 d . . . Cl7 Cl 0.4587(4) 0.0525(4) 0.8813(3) 0.0959(15) Uani 1 1 d . . . Cl12 Cl 0.7911(4) 0.2599(3) -0.0286(3) 0.0799(12) Uani 1 1 d . . . Cl8 Cl 0.6885(3) 0.2889(4) 0.1666(3) 0.0867(12) Uani 1 1 d . . . Cl9 Cl 0.9064(4) 0.4612(3) 0.1143(3) 0.0875(12) Uani 1 1 d . . . C19 C 0.3154(7) 0.2390(7) 0.3696(6) 0.0167(17) Uani 1 1 d . . . C20 C 0.4039(8) 0.3268(7) 0.4324(7) 0.0234(19) Uani 1 1 d . . . H20A H 0.3886 0.3927 0.4570 0.028 Uiso 1 1 calc R . . C15 C 0.2324(7) 0.3343(7) 0.1282(7) 0.0210(18) Uani 1 1 d . . . C1 C 0.1754(7) 0.3916(7) 0.3940(7) 0.0190(18) Uani 1 1 d . . . C23 C 0.4514(7) 0.1383(8) 0.3593(7) 0.027(2) Uani 1 1 d . . . H23A H 0.4687 0.0738 0.3345 0.032 Uiso 1 1 calc R . . C6 C 0.1826(7) 0.4158(7) 0.5083(7) 0.0194(18) Uani 1 1 d . . . C7 C 0.1977(7) 0.3344(7) 0.5960(6) 0.0215(19) Uani 1 1 d . . . H7A H 0.2162 0.2712 0.5596 0.026 Uiso 1 1 calc R . . C24 C 0.3393(7) 0.1411(7) 0.3316(7) 0.024(2) Uani 1 1 d . . . C10 C 0.1524(8) 0.2548(7) 0.1925(7) 0.0219(19) Uani 1 1 d . . . C9 C 0.0807(8) 0.2762(8) 0.6474(8) 0.034(2) Uani 1 1 d . . . H9A H 0.0905 0.2236 0.7028 0.051 Uiso 1 1 calc R . . H9B H 0.0188 0.2313 0.5917 0.051 Uiso 1 1 calc R . . H9C H 0.0580 0.3363 0.6807 0.051 Uiso 1 1 calc R . . C11 C 0.0507(7) 0.1652(7) 0.1417(7) 0.0231(19) Uani 1 1 d . . . H11A H -0.0020 0.1088 0.1844 0.028 Uiso 1 1 calc R . . C27 C 0.2456(9) -0.0815(8) 0.2943(8) 0.035(2) Uani 1 1 d . . . H27A H 0.2255 -0.0909 0.3695 0.053 Uiso 1 1 calc R . . H27B H 0.3225 -0.0884 0.2884 0.053 Uiso 1 1 calc R . . H27C H 0.1845 -0.1422 0.2480 0.053 Uiso 1 1 calc R . . C2 C 0.1552(7) 0.4694(8) 0.3227(7) 0.025(2) Uani 1 1 d . . . H2A H 0.1479 0.4517 0.2473 0.029 Uiso 1 1 calc R . . C26 C 0.2840(8) 0.0585(8) 0.1405(7) 0.030(2) Uani 1 1 d . . . H26A H 0.2875 0.1359 0.1188 0.044 Uiso 1 1 calc R . . H26B H 0.2234 -0.0018 0.0934 0.044 Uiso 1 1 calc R . . H26C H 0.3613 0.0527 0.1341 0.044 Uiso 1 1 calc R . . C25 C 0.2524(8) 0.0411(8) 0.2576(7) 0.028(2) Uani 1 1 d . . . H25A H 0.1718 0.0440 0.2608 0.034 Uiso 1 1 calc R . . C5 C 0.1711(7) 0.5189(7) 0.5400(8) 0.026(2) Uani 1 1 d . . . H5A H 0.1747 0.5370 0.6150 0.032 Uiso 1 1 calc R . . C21 C 0.5140(8) 0.3206(8) 0.4600(7) 0.027(2) Uani 1 1 d . . . H21A H 0.5723 0.3804 0.5048 0.033 Uiso 1 1 calc R . . C4 C 0.1545(8) 0.5964(8) 0.4670(8) 0.031(2) Uani 1 1 d . . . H4A H 0.1494 0.6671 0.4926 0.037 Uiso 1 1 calc R . . C14 C 0.2067(8) 0.3258(9) 0.0165(7) 0.030(2) Uani 1 1 d . . . H14A H 0.2598 0.3797 -0.0278 0.036 Uiso 1 1 calc R . . C12 C 0.0276(8) 0.1590(9) 0.0323(7) 0.030(2) Uani 1 1 d . . . H12A H -0.0413 0.0994 -0.0012 0.035 Uiso 1 1 calc R . . C13 C 0.1060(9) 0.2410(9) -0.0302(8) 0.037(3) Uani 1 1 d . . . H13A H 0.0891 0.2379 -0.1064 0.044 Uiso 1 1 calc R . . C3 C 0.1453(8) 0.5722(8) 0.3580(8) 0.028(2) Uani 1 1 d . . . H3A H 0.1325 0.6247 0.3078 0.033 Uiso 1 1 calc R . . C16 C 0.3497(7) 0.4278(7) 0.1731(7) 0.025(2) Uani 1 1 d . . . H16A H 0.3497 0.4309 0.2536 0.030 Uiso 1 1 calc R . . C18 C 0.4541(8) 0.3936(9) 0.1453(8) 0.034(2) Uani 1 1 d . . . H18A H 0.4421 0.3155 0.1712 0.051 Uiso 1 1 calc R . . H18B H 0.5283 0.4502 0.1802 0.051 Uiso 1 1 calc R . . H18C H 0.4584 0.3932 0.0668 0.051 Uiso 1 1 calc R . . C22 C 0.5379(8) 0.2267(8) 0.4218(8) 0.031(2) Uani 1 1 d . . . H22A H 0.6137 0.2229 0.4385 0.037 Uiso 1 1 calc R . . C8 C 0.2969(9) 0.3937(8) 0.6806(8) 0.035(2) Uani 1 1 d . . . H8A H 0.3017 0.3370 0.7337 0.053 Uiso 1 1 calc R . . H8B H 0.2821 0.4572 0.7170 0.053 Uiso 1 1 calc R . . H8C H 0.3718 0.4256 0.6466 0.053 Uiso 1 1 calc R . . C17 C 0.3677(9) 0.5507(8) 0.1335(9) 0.042(3) Uani 1 1 d . . . H17A H 0.4444 0.6065 0.1646 0.062 Uiso 1 1 calc R . . H17B H 0.3041 0.5740 0.1563 0.062 Uiso 1 1 calc R . . H17C H 0.3662 0.5499 0.0545 0.062 Uiso 1 1 calc R . . C28 C 0.3523(9) 0.0526(9) 0.7794(8) 0.038(2) Uani 1 1 d . . . H28A H 0.3090 -0.0293 0.7503 0.045 Uiso 1 1 calc R . . C29 C 0.8194(9) 0.3123(9) 0.1052(9) 0.043(3) Uani 1 1 d . . . H29A H 0.8639 0.2697 0.1457 0.052 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 0.0177(3) 0.0169(4) 0.0188(4) 0.0013(3) 0.0026(3) 0.0074(3) Cl1 0.0183(11) 0.0282(12) 0.0298(13) 0.0101(10) 0.0033(9) 0.0089(9) P1 0.0196(11) 0.0152(11) 0.0195(12) -0.0004(9) 0.0033(9) 0.0062(9) Cl2 0.0242(11) 0.0285(12) 0.0283(12) 0.0031(10) 0.0037(9) 0.0155(10) Cl5 0.0497(17) 0.068(2) 0.062(2) 0.0074(16) 0.0207(14) 0.0378(16) Cl6 0.0485(17) 0.083(2) 0.0491(18) 0.0166(16) 0.0149(14) 0.0283(17) Cl7 0.097(3) 0.177(5) 0.061(2) 0.037(3) 0.016(2) 0.104(3) Cl12 0.122(3) 0.099(3) 0.052(2) -0.0222(19) -0.022(2) 0.085(3) Cl8 0.060(2) 0.123(3) 0.098(3) 0.007(3) 0.018(2) 0.056(2) Cl9 0.102(3) 0.059(2) 0.088(3) -0.002(2) -0.018(2) 0.020(2) C19 0.021(4) 0.016(4) 0.017(4) 0.004(3) 0.004(3) 0.010(3) C20 0.031(5) 0.018(5) 0.020(5) -0.001(4) 0.005(4) 0.007(4) C15 0.028(5) 0.025(5) 0.016(4) -0.001(4) 0.004(4) 0.016(4) C1 0.016(4) 0.019(4) 0.022(5) 0.002(4) 0.004(3) 0.005(3) C23 0.026(5) 0.030(5) 0.033(6) 0.003(4) 0.000(4) 0.021(4) C6 0.019(4) 0.020(4) 0.021(5) -0.008(4) 0.006(3) 0.009(4) C7 0.027(5) 0.024(5) 0.016(4) 0.000(4) 0.008(4) 0.011(4) C24 0.017(4) 0.026(5) 0.031(5) -0.003(4) 0.004(4) 0.009(4) C10 0.031(5) 0.016(4) 0.023(5) -0.002(4) 0.002(4) 0.015(4) C9 0.039(6) 0.033(6) 0.033(6) 0.002(4) 0.014(5) 0.015(5) C11 0.022(4) 0.021(5) 0.027(5) -0.001(4) 0.008(4) 0.008(4) C27 0.038(6) 0.031(6) 0.042(6) -0.006(5) 0.005(5) 0.019(5) C2 0.026(5) 0.031(5) 0.020(5) 0.003(4) 0.007(4) 0.013(4) C26 0.031(5) 0.034(6) 0.029(5) -0.007(4) 0.002(4) 0.019(4) C25 0.030(5) 0.025(5) 0.029(5) -0.005(4) 0.003(4) 0.010(4) C5 0.021(5) 0.025(5) 0.035(6) -0.007(4) 0.004(4) 0.011(4) C21 0.022(5) 0.022(5) 0.031(5) 0.000(4) 0.001(4) 0.001(4) C4 0.038(6) 0.022(5) 0.038(6) -0.006(4) 0.006(5) 0.019(4) C14 0.037(5) 0.050(6) 0.007(4) 0.004(4) 0.007(4) 0.019(5) C12 0.024(5) 0.045(6) 0.023(5) -0.012(4) -0.008(4) 0.020(5) C13 0.046(6) 0.062(7) 0.016(5) 0.003(5) 0.002(5) 0.036(6) C3 0.031(5) 0.019(5) 0.038(6) 0.003(4) 0.008(4) 0.013(4) C16 0.026(5) 0.024(5) 0.030(5) 0.004(4) 0.013(4) 0.014(4) C18 0.026(5) 0.041(6) 0.039(6) -0.007(5) 0.005(4) 0.017(5) C22 0.021(5) 0.034(6) 0.039(6) -0.003(5) 0.002(4) 0.010(4) C8 0.047(6) 0.032(6) 0.029(6) -0.001(4) 0.001(5) 0.018(5) C17 0.042(6) 0.034(6) 0.048(7) 0.009(5) 0.019(5) 0.010(5) C28 0.039(6) 0.039(6) 0.040(6) -0.006(5) 0.005(5) 0.020(5) C29 0.042(6) 0.048(7) 0.051(7) 0.003(5) -0.004(5) 0.031(6) _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 P1 2.244(2) . ? Pd1 Cl2 2.300(2) . ? Pd1 Cl1 2.319(2) . ? Pd1 Cl1 2.403(2) 2_556 ? Cl1 Pd1 2.403(2) 2_556 ? P1 C19 1.826(8) . ? P1 C10 1.827(9) . ? P1 C1 1.838(8) . ? Cl5 C28 1.765(9) . ? Cl6 C28 1.737(10) . ? Cl7 C28 1.744(11) . ? Cl12 C29 1.740(11) . ? Cl8 C29 1.747(11) . ? Cl9 C29 1.744(11) . ? C19 C20 1.392(11) . ? C19 C24 1.426(11) . ? C20 C21 1.391(12) . ? C20 H20A 0.9500 . ? C15 C14 1.394(11) . ? C15 C10 1.404(12) . ? C15 C16 1.527(12) . ? C1 C2 1.388(11) . ? C1 C6 1.437(11) . ? C23 C22 1.383(12) . ? C23 C24 1.398(11) . ? C23 H23A 0.9500 . ? C6 C5 1.386(11) . ? C6 C7 1.535(12) . ? C7 C8 1.498(12) . ? C7 C9 1.530(11) . ? C7 H7A 1.0000 . ? C24 C25 1.533(12) . ? C10 C11 1.419(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.363(12) . ? C11 H11A 0.9500 . ? C27 C25 1.557(12) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C2 C3 1.386(11) . ? C2 H2A 0.9500 . ? C26 C25 1.529(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 1.0000 . ? C5 C4 1.381(13) . ? C5 H5A 0.9500 . ? C21 C22 1.382(12) . ? C21 H21A 0.9500 . ? C4 C3 1.371(13) . ? C4 H4A 0.9500 . ? C14 C13 1.367(14) . ? C14 H14A 0.9500 . ? C12 C13 1.395(14) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C3 H3A 0.9500 . ? C16 C17 1.539(12) . ? C16 C18 1.542(11) . ? C16 H16A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C22 H22A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C28 H28A 1.0000 . ? C29 H29A 1.0000 . ? 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 P1 Pd1 Cl2 89.83(8) . . ? P1 Pd1 Cl1 94.52(8) . . ? Cl2 Pd1 Cl1 172.94(8) . . ? P1 Pd1 Cl1 177.50(9) . 2_556 ? Cl2 Pd1 Cl1 90.19(8) . 2_556 ? Cl1 Pd1 Cl1 85.22(8) . 2_556 ? Pd1 Cl1 Pd1 94.78(7) . 2_556 ? C19 P1 C10 105.7(4) . . ? C19 P1 C1 109.9(4) . . ? C10 P1 C1 106.7(4) . . ? C19 P1 Pd1 114.4(3) . . ? C10 P1 Pd1 113.8(3) . . ? C1 P1 Pd1 106.1(3) . . ? C20 C19 C24 118.9(7) . . ? C20 C19 P1 119.3(6) . . ? C24 C19 P1 121.8(6) . . ? C21 C20 C19 121.7(8) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C14 C15 C10 118.9(8) . . ? C14 C15 C16 117.3(8) . . ? C10 C15 C16 123.7(8) . . ? C2 C1 C6 119.3(7) . . ? C2 C1 P1 118.5(6) . . ? C6 C1 P1 121.6(6) . . ? C22 C23 C24 122.0(8) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C5 C6 C1 116.6(8) . . ? C5 C6 C7 118.5(7) . . ? C1 C6 C7 124.8(7) . . ? C8 C7 C9 110.8(7) . . ? C8 C7 C6 113.7(7) . . ? C9 C7 C6 109.7(7) . . ? C8 C7 H7A 107.5 . . ? C9 C7 H7A 107.5 . . ? C6 C7 H7A 107.5 . . ? C23 C24 C19 118.0(8) . . ? C23 C24 C25 117.4(7) . . ? C19 C24 C25 124.5(7) . . ? C15 C10 C11 119.1(8) . . ? C15 C10 P1 125.3(7) . . ? C11 C10 P1 115.6(6) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 C10 120.8(8) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C3 C2 C1 122.1(8) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C26 C25 C24 110.5(7) . . ? C26 C25 C27 110.7(7) . . ? C24 C25 C27 112.8(8) . . ? C26 C25 H25A 107.5 . . ? C24 C25 H25A 107.5 . . ? C27 C25 H25A 107.5 . . ? C4 C5 C6 122.8(9) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C22 C21 C20 119.4(8) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C3 C4 C5 120.6(8) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C13 C14 C15 120.8(9) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C11 C12 C13 119.4(9) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 121.0(9) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C4 C3 C2 118.6(9) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C15 C16 C17 113.3(8) . . ? C15 C16 C18 110.1(7) . . ? C17 C16 C18 110.1(7) . . ? C15 C16 H16A 107.7 . . ? C17 C16 H16A 107.7 . . ? C18 C16 H16A 107.7 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C22 C23 119.9(8) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? 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 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Cl6 C28 Cl7 110.0(6) . . ? Cl6 C28 Cl5 111.6(5) . . ? Cl7 C28 Cl5 109.2(5) . . ? Cl6 C28 H28A 108.7 . . ? Cl7 C28 H28A 108.7 . . ? Cl5 C28 H28A 108.7 . . ? Cl12 C29 Cl9 111.0(6) . . ? Cl12 C29 Cl8 111.8(6) . . ? Cl9 C29 Cl8 109.1(6) . . ? Cl12 C29 H29A 108.3 . . ? Cl9 C29 H29A 108.3 . . ? Cl8 C29 H29A 108.3 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.229 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.205