data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Piet W.N.M. Van Leeuwen' _publ_contact_author_address ; Chemical Engineering and Chemistry Eindhoven University of Technology Den Dolech 2 Eindhoven 5600 MB Eindhoven NETHERLANDS ; _publ_contact_author_email P.W.N.M.V.LEEUWEN@TUE.NL _publ_section_title ; New diphosphine ligands based on diphenyl ether for the Pd-catalyzed CO/ethene copolymerization ; _publ_section_references ; Beurskens, P.T., Beurskens, G., de Gelder, R., Garcia-Granda, S., Gould, R.O., Israel, R., and Smits, J.M.M. (1999). The DIRDIF-99 program system, Crystallography Laboratory, University of Nijmegen, The Netherlands. Blessing, R.H. (1995). Acta Crystallogr. Sect. A 51, 33. Duisenberg, A.J.M. (1992). J. Appl. Cryst. 25, 92-96. Nonius Collect Software, Nonius B.V., Delft, The Netherlands, 1998. Otwinowski, Z. and Minor, W. "Processing of X-ray Diffraction Data Collected in Oscillation Mode", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press (New York). Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. ; loop_ _publ_author_name 'P.W.N.M.Van Leeuwen' 'Maria Caporali' 'Christian Mueller' 'Anthony L. Spek' 'Bastiaan B. P. Staal' ; D.M.Tooke ; data_1 _database_code_depnum_ccdc_archive 'CCDC 267390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H96 Cl2 O P2 Pd' _chemical_formula_sum 'C70 H96 Cl2 O P2 Pd' _chemical_formula_weight 1192.71 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 25.241(3) _cell_length_b 20.053(4) _cell_length_c 26.004(2) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 13162(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 3.543 _cell_measurement_theta_max 15.557 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'PLATON MULABS (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 164826 _diffrn_reflns_av_R_equivalents 0.1205 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8606 _reflns_number_gt 6404 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius Collect (Nonius, 1998)' _computing_cell_refinement 'DIRAX (Duisenberg, 1992)' _computing_data_reduction 'HKL2000 (Otwinowski et al., 1997)' _computing_structure_solution 'DIRDIF (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0387P)^2^+12.0600P] 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 8606 _refine_ls_number_parameters 742 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.174530(10) 0.145299(12) 0.089428(10) 0.01912(9) Uani 1 1 d . . . Cl1 Cl 0.15625(4) 0.04975(4) 0.04005(4) 0.0315(2) Uani 1 1 d . . . Cl2 Cl 0.26072(4) 0.10881(5) 0.10497(4) 0.0341(3) Uani 1 1 d . . . P1 P 0.09554(4) 0.18447(4) 0.06019(4) 0.0199(2) Uani 1 1 d . . . P2 P 0.18529(3) 0.21779(4) 0.15421(4) 0.0194(2) Uani 1 1 d . . . O1 O 0.08843(9) 0.14076(11) 0.17058(8) 0.0212(6) Uani 1 1 d . . . C1 C 0.09199(14) 0.18316(16) -0.01007(13) 0.0211(9) Uani 1 1 d . . . C2 C 0.04629(14) 0.20609(17) -0.03459(14) 0.0252(9) Uani 1 1 d . . . H2 H 0.0173 0.2214 -0.0145 0.030 Uiso 1 1 calc R . . C3 C 0.04232(14) 0.20689(18) -0.08787(14) 0.0277(9) Uani 1 1 d . . . C4 C 0.08545(15) 0.18403(18) -0.11581(15) 0.0307(10) Uani 1 1 d . . . H4 H 0.0828 0.1828 -0.1522 0.037 Uiso 1 1 calc R . . C5 C 0.13247(15) 0.16279(17) -0.09320(15) 0.0278(9) Uani 1 1 d . A . C6 C 0.13503(15) 0.16398(16) -0.03966(14) 0.0242(9) Uani 1 1 d . . . H6 H 0.1670 0.1514 -0.0231 0.029 Uiso 1 1 calc R . . C7 C 0.17852(15) 0.13540(18) -0.12538(14) 0.0317(10) Uani 1 1 d . . . C8 C 0.1762(10) 0.0633(9) -0.1213(9) 0.049(6) Uani 0.40(2) 1 d PD A 1 H8A H 0.2034 0.0435 -0.1434 0.073 Uiso 0.40(2) 1 calc PR A 1 H8B H 0.1412 0.0477 -0.1323 0.073 Uiso 0.40(2) 1 calc PR A 1 H8C H 0.1824 0.0500 -0.0856 0.073 Uiso 0.40(2) 1 calc PR A 1 C9 C 0.1700(8) 0.1552(11) -0.1837(6) 0.044(5) Uani 0.40(2) 1 d PD A 1 H9A H 0.1632 0.2032 -0.1862 0.066 Uiso 0.40(2) 1 calc PR A 1 H9B H 0.1398 0.1306 -0.1977 0.066 Uiso 0.40(2) 1 calc PR A 1 H9C H 0.2020 0.1442 -0.2034 0.066 Uiso 0.40(2) 1 calc PR A 1 C10 C 0.2291(5) 0.1661(12) -0.1080(7) 0.042(5) Uani 0.40(2) 1 d PD A 1 H10A H 0.2356 0.1542 -0.0720 0.064 Uiso 0.40(2) 1 calc PR A 1 H10B H 0.2267 0.2147 -0.1112 0.064 Uiso 0.40(2) 1 calc PR A 1 H10C H 0.2583 0.1497 -0.1294 0.064 Uiso 0.40(2) 1 calc PR A 1 C8A C 0.1645(7) 0.0661(8) -0.1466(7) 0.062(5) Uani 0.60(2) 1 d PD A 2 H8D H 0.1949 0.0481 -0.1655 0.093 Uiso 0.60(2) 1 calc PR A 2 H8E H 0.1341 0.0698 -0.1699 0.093 Uiso 0.60(2) 1 calc PR A 2 H8F H 0.1556 0.0362 -0.1181 0.093 Uiso 0.60(2) 1 calc PR A 2 C9A C 0.1944(7) 0.1801(7) -0.1698(6) 0.064(5) Uani 0.60(2) 1 d PD A 2 H9D H 0.2069 0.2230 -0.1565 0.095 Uiso 0.60(2) 1 calc PR A 2 H9E H 0.1637 0.1874 -0.1922 0.095 Uiso 0.60(2) 1 calc PR A 2 H9F H 0.2228 0.1587 -0.1895 0.095 Uiso 0.60(2) 1 calc PR A 2 C10A C 0.2301(4) 0.1226(10) -0.0926(4) 0.056(4) Uani 0.60(2) 1 d PD A 2 H10D H 0.2590 0.1089 -0.1154 0.084 Uiso 0.60(2) 1 calc PR A 2 H10E H 0.2233 0.0873 -0.0674 0.084 Uiso 0.60(2) 1 calc PR A 2 H10F H 0.2401 0.1636 -0.0746 0.084 Uiso 0.60(2) 1 calc PR A 2 C11 C -0.00730(15) 0.2325(2) -0.11548(15) 0.0395(11) Uani 1 1 d . . . C12 C -0.04549(17) 0.2670(3) -0.07828(18) 0.0683(16) Uani 1 1 d . . . H12A H -0.0582 0.2346 -0.0529 0.102 Uiso 1 1 calc R . . H12B H -0.0757 0.2850 -0.0975 0.102 Uiso 1 1 calc R . . H12C H -0.0270 0.3034 -0.0606 0.102 Uiso 1 1 calc R . . C13 C -0.0348(2) 0.1740(3) -0.1414(2) 0.0795(18) Uani 1 1 d . . . H13A H -0.0105 0.1532 -0.1660 0.119 Uiso 1 1 calc R . . H13B H -0.0664 0.1899 -0.1595 0.119 Uiso 1 1 calc R . . H13C H -0.0452 0.1412 -0.1153 0.119 Uiso 1 1 calc R . . C14 C 0.00820(17) 0.2851(2) -0.15568(16) 0.0525(13) Uani 1 1 d . . . H14A H 0.0262 0.3223 -0.1386 0.079 Uiso 1 1 calc R . . H14B H -0.0237 0.3015 -0.1730 0.079 Uiso 1 1 calc R . . H14C H 0.0320 0.2650 -0.1811 0.079 Uiso 1 1 calc R . . C15 C 0.01279(14) 0.27275(17) 0.08261(13) 0.0222(9) Uani 1 1 d . . . H15 H -0.0074 0.2335 0.0885 0.027 Uiso 1 1 calc R . . C16 C -0.01209(14) 0.33423(17) 0.08476(13) 0.0250(9) Uani 1 1 d . . . C17 C 0.01925(15) 0.39078(18) 0.07742(13) 0.0268(9) Uani 1 1 d . . . H17 H 0.0029 0.4334 0.0791 0.032 Uiso 1 1 calc R . . C18 C 0.07313(14) 0.38748(17) 0.06773(13) 0.0238(9) Uani 1 1 d . . . C19 C 0.09634(14) 0.32424(17) 0.06445(13) 0.0211(8) Uani 1 1 d . . . H19 H 0.1330 0.3204 0.0569 0.025 Uiso 1 1 calc R . . C20 C 0.06642(14) 0.26698(16) 0.07205(12) 0.0196(8) Uani 1 1 d . . . C21 C -0.07182(14) 0.34152(18) 0.09424(15) 0.0316(10) Uani 1 1 d . . . C22 C -0.08201(17) 0.3904(2) 0.13828(17) 0.0564(13) Uani 1 1 d . . . H22A H -0.1201 0.3927 0.1452 0.085 Uiso 1 1 calc R . . H22B H -0.0689 0.4347 0.1287 0.085 Uiso 1 1 calc R . . H22C H -0.0635 0.3750 0.1692 0.085 Uiso 1 1 calc R . . C23 C -0.09749(15) 0.2758(2) 0.10819(18) 0.0472(12) Uani 1 1 d . . . H23A H -0.0929 0.2441 0.0798 0.071 Uiso 1 1 calc R . . H23B H -0.1354 0.2827 0.1145 0.071 Uiso 1 1 calc R . . H23C H -0.0808 0.2578 0.1393 0.071 Uiso 1 1 calc R . . C24 C -0.09774(16) 0.3680(2) 0.04536(17) 0.0546(13) Uani 1 1 d . . . H24A H -0.0934 0.3354 0.0176 0.082 Uiso 1 1 calc R . . H24B H -0.0809 0.4101 0.0355 0.082 Uiso 1 1 calc R . . H24C H -0.1356 0.3755 0.0516 0.082 Uiso 1 1 calc R . . C25 C 0.10675(14) 0.45040(17) 0.05906(14) 0.0279(9) Uani 1 1 d . . . C26 C 0.07650(17) 0.51487(17) 0.07107(16) 0.0424(11) Uani 1 1 d . . . H26A H 0.0459 0.5187 0.0480 0.064 Uiso 1 1 calc R . . H26B H 0.1000 0.5532 0.0661 0.064 Uiso 1 1 calc R . . H26C H 0.0642 0.5139 0.1068 0.064 Uiso 1 1 calc R . . C27 C 0.12335(16) 0.45176(19) 0.00273(15) 0.0398(11) Uani 1 1 d . . . H27A H 0.1413 0.4099 -0.0060 0.060 Uiso 1 1 calc R . . H27B H 0.1475 0.4892 -0.0031 0.060 Uiso 1 1 calc R . . H27C H 0.0919 0.4570 -0.0190 0.060 Uiso 1 1 calc R . . C28 C 0.15581(16) 0.44898(19) 0.09329(16) 0.0419(11) Uani 1 1 d . . . H28A H 0.1449 0.4481 0.1295 0.063 Uiso 1 1 calc R . . H28B H 0.1772 0.4889 0.0869 0.063 Uiso 1 1 calc R . . H28C H 0.1768 0.4091 0.0855 0.063 Uiso 1 1 calc R . . C29 C 0.21367(13) 0.18137(16) 0.21241(13) 0.0197(8) Uani 1 1 d . . . C30 C 0.26818(14) 0.17748(17) 0.21805(14) 0.0236(9) Uani 1 1 d . . . H30 H 0.2905 0.1941 0.1916 0.028 Uiso 1 1 calc R . . C31 C 0.29081(14) 0.14965(17) 0.26178(14) 0.0256(9) Uani 1 1 d . . . C32 C 0.25706(15) 0.12452(17) 0.29929(14) 0.0269(9) Uani 1 1 d . . . H32 H 0.2720 0.1055 0.3294 0.032 Uiso 1 1 calc R . . C33 C 0.20224(14) 0.12624(16) 0.29438(13) 0.0222(9) Uani 1 1 d . . . C34 C 0.18097(14) 0.15536(15) 0.25066(13) 0.0205(8) Uani 1 1 d . . . H34 H 0.1436 0.1576 0.2467 0.025 Uiso 1 1 calc R . . C35 C 0.16596(15) 0.09837(17) 0.33706(13) 0.0285(9) Uani 1 1 d . . . C36 C 0.19043(16) 0.03705(18) 0.36286(15) 0.0370(10) Uani 1 1 d . . . H36A H 0.1985 0.0033 0.3367 0.056 Uiso 1 1 calc R . . H36B H 0.1653 0.0186 0.3879 0.056 Uiso 1 1 calc R . . H36C H 0.2232 0.0500 0.3805 0.056 Uiso 1 1 calc R . . C37 C 0.11210(15) 0.0773(2) 0.31549(15) 0.0382(11) Uani 1 1 d . . . H37A H 0.0939 0.1164 0.3013 0.057 Uiso 1 1 calc R . . H37B H 0.0906 0.0580 0.3431 0.057 Uiso 1 1 calc R . . H37C H 0.1173 0.0441 0.2883 0.057 Uiso 1 1 calc R . . C38 C 0.15714(18) 0.1527(2) 0.37731(15) 0.0452(12) Uani 1 1 d . . . H38A H 0.1913 0.1661 0.3919 0.068 Uiso 1 1 calc R . . H38B H 0.1343 0.1355 0.4047 0.068 Uiso 1 1 calc R . . H38C H 0.1402 0.1913 0.3611 0.068 Uiso 1 1 calc R . . C39 C 0.35139(14) 0.14459(19) 0.26512(16) 0.0359(10) Uani 1 1 d . . . C40 C 0.37032(17) 0.0945(2) 0.2249(2) 0.0710(17) Uani 1 1 d . . . H40A H 0.3584 0.1087 0.1908 0.107 Uiso 1 1 calc R . . H40B H 0.3556 0.0504 0.2327 0.107 Uiso 1 1 calc R . . H40C H 0.4091 0.0922 0.2255 0.107 Uiso 1 1 calc R . . C41 C 0.37587(15) 0.2125(2) 0.25401(17) 0.0435(12) Uani 1 1 d . . . H41A H 0.3667 0.2263 0.2190 0.065 Uiso 1 1 calc R . . H41B H 0.4145 0.2095 0.2573 0.065 Uiso 1 1 calc R . . H41C H 0.3622 0.2453 0.2786 0.065 Uiso 1 1 calc R . . C42 C 0.36945(17) 0.1225(2) 0.31874(18) 0.0575(14) Uani 1 1 d . . . H42A H 0.4082 0.1239 0.3206 0.086 Uiso 1 1 calc R . . H42B H 0.3572 0.0769 0.3253 0.086 Uiso 1 1 calc R . . H42C H 0.3545 0.1526 0.3447 0.086 Uiso 1 1 calc R . . C43 C 0.22847(13) 0.28608(16) 0.13658(13) 0.0197(8) Uani 1 1 d . . . C44 C 0.24384(13) 0.29013(16) 0.08525(14) 0.0223(9) Uani 1 1 d . . . H44 H 0.2311 0.2578 0.0616 0.027 Uiso 1 1 calc R . . C45 C 0.27721(14) 0.34016(17) 0.06781(14) 0.0241(9) Uani 1 1 d . . . C46 C 0.29500(14) 0.38649(17) 0.10443(14) 0.0256(9) Uani 1 1 d . . . H46 H 0.3171 0.4220 0.0933 0.031 Uiso 1 1 calc R . . C47 C 0.28182(13) 0.38280(17) 0.15606(13) 0.0214(9) Uani 1 1 d . . . C48 C 0.24821(14) 0.33178(16) 0.17159(13) 0.0216(9) Uani 1 1 d . . . H48 H 0.2386 0.3282 0.2068 0.026 Uiso 1 1 calc R . . C49 C 0.30156(14) 0.43344(17) 0.19563(13) 0.0251(9) Uani 1 1 d . . . C50 C 0.34194(16) 0.48199(19) 0.17321(15) 0.0375(11) Uani 1 1 d . . . H50A H 0.3724 0.4571 0.1600 0.056 Uiso 1 1 calc R . . H50B H 0.3537 0.5128 0.2001 0.056 Uiso 1 1 calc R . . H50C H 0.3256 0.5073 0.1451 0.056 Uiso 1 1 calc R . . C51 C 0.32792(16) 0.39652(18) 0.24036(14) 0.0361(10) Uani 1 1 d . . . H51A H 0.3020 0.3670 0.2568 0.054 Uiso 1 1 calc R . . H51B H 0.3410 0.4289 0.2656 0.054 Uiso 1 1 calc R . . H51C H 0.3576 0.3700 0.2274 0.054 Uiso 1 1 calc R . . C52 C 0.25392(16) 0.47364(18) 0.21534(15) 0.0376(10) Uani 1 1 d . . . H52A H 0.2376 0.4977 0.1866 0.056 Uiso 1 1 calc R . . H52B H 0.2659 0.5056 0.2414 0.056 Uiso 1 1 calc R . . H52C H 0.2279 0.4432 0.2306 0.056 Uiso 1 1 calc R . . C53 C 0.29494(15) 0.34492(18) 0.01177(14) 0.0307(10) Uani 1 1 d . . . C54 C 0.27714(19) 0.2858(2) -0.01981(16) 0.0592(14) Uani 1 1 d . . . H54A H 0.2937 0.2451 -0.0064 0.089 Uiso 1 1 calc R . . H54B H 0.2876 0.2923 -0.0557 0.089 Uiso 1 1 calc R . . H54C H 0.2385 0.2815 -0.0177 0.089 Uiso 1 1 calc R . . C55 C 0.27096(17) 0.4083(2) -0.01264(16) 0.0494(12) Uani 1 1 d . . . H55A H 0.2322 0.4052 -0.0122 0.074 Uiso 1 1 calc R . . H55B H 0.2833 0.4124 -0.0482 0.074 Uiso 1 1 calc R . . H55C H 0.2822 0.4475 0.0070 0.074 Uiso 1 1 calc R . . C56 C 0.35490(16) 0.3517(2) 0.00935(16) 0.0490(12) Uani 1 1 d . . . H56A H 0.3658 0.3919 0.0280 0.074 Uiso 1 1 calc R . . H56B H 0.3661 0.3550 -0.0266 0.074 Uiso 1 1 calc R . . H56C H 0.3714 0.3124 0.0252 0.074 Uiso 1 1 calc R . . C57 C 0.12306(13) 0.25069(17) 0.17869(12) 0.0191(8) Uani 1 1 d . . . C58 C 0.11521(14) 0.31688(17) 0.19251(13) 0.0231(9) Uani 1 1 d . . . H58 H 0.1439 0.3473 0.1892 0.028 Uiso 1 1 calc R . . C59 C 0.06708(15) 0.34022(17) 0.21091(13) 0.0270(9) Uani 1 1 d . . . C60 C 0.02579(15) 0.29471(19) 0.21610(13) 0.0294(10) Uani 1 1 d . . . H60 H -0.0074 0.3095 0.2290 0.035 Uiso 1 1 calc R . . C61 C 0.03213(14) 0.22869(18) 0.20297(13) 0.0252(9) Uani 1 1 d . . . H61 H 0.0038 0.1980 0.2072 0.030 Uiso 1 1 calc R . . C62 C 0.08013(14) 0.20755(17) 0.18352(13) 0.0194(8) Uani 1 1 d . . . C63 C 0.05898(16) 0.41274(18) 0.22350(15) 0.0401(11) Uani 1 1 d . . . H63A H 0.0933 0.4334 0.2311 0.060 Uiso 1 1 calc R . . H63B H 0.0357 0.4167 0.2535 0.060 Uiso 1 1 calc R . . H63C H 0.0427 0.4353 0.1941 0.060 Uiso 1 1 calc R . . C64 C 0.05055(13) 0.11046(16) 0.13890(14) 0.0207(9) Uani 1 1 d . . . C65 C 0.01980(14) 0.06113(17) 0.16012(14) 0.0267(9) Uani 1 1 d . . . H65 H 0.0232 0.0503 0.1955 0.032 Uiso 1 1 calc R . . C66 C -0.01609(14) 0.02740(18) 0.12962(15) 0.0287(9) Uani 1 1 d . . . H66 H -0.0369 -0.0072 0.1443 0.034 Uiso 1 1 calc R . . C67 C -0.02228(13) 0.04291(17) 0.07838(14) 0.0256(9) Uani 1 1 d . . . C68 C 0.00954(13) 0.09263(16) 0.05783(14) 0.0234(9) Uani 1 1 d . . . H68 H 0.0056 0.1039 0.0226 0.028 Uiso 1 1 calc R . . C69 C 0.04705(13) 0.12662(15) 0.08711(13) 0.0189(8) Uani 1 1 d . . . C70 C -0.06238(15) 0.00718(19) 0.04577(15) 0.0357(10) Uani 1 1 d . . . H70A H -0.0614 -0.0406 0.0535 0.053 Uiso 1 1 calc R . . H70B H -0.0541 0.0142 0.0093 0.053 Uiso 1 1 calc R . . H70C H -0.0978 0.0246 0.0532 0.053 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 0.02157(16) 0.01550(16) 0.02029(16) -0.00093(13) -0.00235(13) 0.00056(12) Cl1 0.0442(6) 0.0189(5) 0.0314(6) -0.0050(4) -0.0105(5) 0.0029(4) Cl2 0.0277(6) 0.0327(6) 0.0420(6) -0.0064(5) -0.0054(4) 0.0093(5) P1 0.0227(5) 0.0171(5) 0.0199(6) 0.0002(4) -0.0015(4) -0.0013(4) P2 0.0216(5) 0.0173(5) 0.0193(5) 0.0010(4) -0.0013(4) -0.0028(4) O1 0.0218(13) 0.0195(14) 0.0223(14) 0.0005(11) -0.0026(11) -0.0022(11) C1 0.028(2) 0.015(2) 0.020(2) -0.0015(16) -0.0022(18) -0.0021(17) C2 0.026(2) 0.025(2) 0.025(2) 0.0003(17) 0.0005(18) -0.0048(17) C3 0.030(2) 0.032(2) 0.021(2) 0.0038(18) -0.0022(19) -0.0074(18) C4 0.039(3) 0.032(2) 0.021(2) 0.0004(18) -0.004(2) -0.007(2) C5 0.036(2) 0.021(2) 0.027(3) -0.0015(17) 0.003(2) -0.0072(18) C6 0.029(2) 0.017(2) 0.027(2) -0.0006(17) -0.0024(18) -0.0019(17) C7 0.040(3) 0.030(2) 0.025(2) -0.0081(18) 0.0073(19) 0.001(2) C8 0.049(12) 0.025(8) 0.072(15) -0.017(10) 0.028(12) 0.010(7) C9 0.059(12) 0.048(11) 0.025(8) 0.000(7) 0.025(7) 0.014(8) C10 0.020(6) 0.059(11) 0.049(10) -0.030(9) 0.006(6) 0.004(7) C8A 0.059(9) 0.057(7) 0.071(12) -0.027(8) 0.022(8) -0.005(6) C9A 0.079(11) 0.047(7) 0.064(9) 0.014(6) 0.036(8) 0.022(6) C10A 0.031(5) 0.075(10) 0.062(7) -0.034(6) 0.006(5) 0.008(6) C11 0.031(2) 0.061(3) 0.026(2) 0.011(2) -0.005(2) -0.004(2) C12 0.040(3) 0.114(5) 0.050(3) 0.024(3) -0.006(2) 0.016(3) C13 0.068(4) 0.087(4) 0.083(4) 0.009(3) -0.044(3) -0.018(3) C14 0.046(3) 0.069(3) 0.042(3) 0.016(2) -0.003(2) 0.011(2) C15 0.027(2) 0.021(2) 0.018(2) 0.0038(16) 0.0003(17) -0.0001(17) C16 0.031(2) 0.026(2) 0.018(2) 0.0003(17) 0.0007(18) 0.0025(18) C17 0.034(2) 0.019(2) 0.027(2) 0.0006(17) -0.0007(18) 0.0077(18) C18 0.032(2) 0.020(2) 0.020(2) 0.0013(17) -0.0036(17) 0.0004(18) C19 0.023(2) 0.024(2) 0.016(2) 0.0019(16) 0.0006(16) 0.0037(18) C20 0.027(2) 0.018(2) 0.014(2) 0.0027(15) -0.0037(16) 0.0030(17) C21 0.027(2) 0.033(2) 0.034(2) 0.0040(19) 0.0054(19) 0.0085(18) C22 0.038(3) 0.066(3) 0.064(3) -0.017(3) 0.015(2) 0.014(2) C23 0.027(2) 0.048(3) 0.066(3) 0.013(2) 0.010(2) 0.006(2) C24 0.036(3) 0.072(3) 0.055(3) 0.023(3) 0.001(2) 0.018(2) C25 0.034(2) 0.019(2) 0.031(2) 0.0018(17) 0.0024(19) 0.0005(18) C26 0.059(3) 0.019(2) 0.049(3) 0.002(2) 0.004(2) 0.000(2) C27 0.049(3) 0.032(2) 0.038(3) 0.005(2) 0.006(2) -0.003(2) C28 0.051(3) 0.023(2) 0.051(3) 0.003(2) -0.003(2) -0.011(2) C29 0.022(2) 0.0158(19) 0.022(2) -0.0037(16) -0.0031(17) -0.0016(16) C30 0.027(2) 0.019(2) 0.025(2) -0.0005(17) 0.0030(18) -0.0026(17) C31 0.028(2) 0.0150(19) 0.034(2) -0.0015(18) -0.0077(19) -0.0024(18) C32 0.036(3) 0.017(2) 0.027(2) -0.0001(17) -0.0084(19) 0.0027(18) C33 0.030(2) 0.017(2) 0.019(2) -0.0017(16) -0.0035(18) -0.0003(17) C34 0.020(2) 0.019(2) 0.023(2) -0.0026(17) -0.0028(17) 0.0001(17) C35 0.039(2) 0.025(2) 0.021(2) 0.0045(17) 0.0005(18) 0.0018(19) C36 0.050(3) 0.032(2) 0.029(2) 0.0086(19) -0.002(2) 0.002(2) C37 0.036(3) 0.045(3) 0.033(3) 0.010(2) 0.007(2) -0.004(2) C38 0.072(3) 0.036(3) 0.028(3) -0.001(2) 0.009(2) 0.001(2) C39 0.025(2) 0.028(2) 0.055(3) 0.004(2) -0.009(2) -0.0054(19) C40 0.031(3) 0.069(4) 0.113(5) -0.036(3) -0.012(3) 0.016(3) C41 0.023(2) 0.050(3) 0.057(3) 0.018(2) -0.010(2) -0.008(2) C42 0.035(3) 0.054(3) 0.084(4) 0.031(3) -0.031(3) -0.012(2) C43 0.022(2) 0.018(2) 0.019(2) -0.0006(17) -0.0004(17) -0.0002(16) C44 0.022(2) 0.019(2) 0.026(2) -0.0056(17) -0.0033(18) 0.0013(16) C45 0.025(2) 0.021(2) 0.026(2) 0.0006(18) -0.0006(18) -0.0022(17) C46 0.029(2) 0.019(2) 0.028(3) 0.0035(18) 0.0026(18) -0.0043(18) C47 0.023(2) 0.020(2) 0.021(2) 0.0006(17) -0.0008(17) 0.0028(17) C48 0.026(2) 0.022(2) 0.017(2) 0.0009(17) 0.0021(17) -0.0003(17) C49 0.029(2) 0.018(2) 0.028(2) -0.0010(17) -0.0034(18) -0.0028(17) C50 0.051(3) 0.029(2) 0.032(2) -0.0032(19) -0.005(2) -0.020(2) C51 0.047(3) 0.031(2) 0.030(2) -0.0020(19) -0.009(2) -0.009(2) C52 0.047(3) 0.027(2) 0.038(3) -0.009(2) -0.001(2) -0.004(2) C53 0.035(2) 0.033(2) 0.024(2) -0.0049(19) 0.0065(19) -0.0116(19) C54 0.088(4) 0.057(3) 0.033(3) -0.013(2) 0.025(3) -0.030(3) C55 0.052(3) 0.065(3) 0.031(3) 0.006(2) -0.004(2) -0.004(2) C56 0.043(3) 0.073(3) 0.031(3) 0.003(2) 0.013(2) -0.002(2) C57 0.023(2) 0.020(2) 0.014(2) 0.0030(16) -0.0041(16) 0.0003(17) C58 0.032(2) 0.022(2) 0.016(2) -0.0004(17) -0.0021(17) -0.0028(18) C59 0.035(2) 0.026(2) 0.020(2) -0.0020(17) -0.0013(18) 0.006(2) C60 0.030(2) 0.036(3) 0.022(2) -0.0036(18) 0.0028(18) 0.007(2) C61 0.023(2) 0.033(2) 0.020(2) 0.0007(18) 0.0021(17) -0.0032(18) C62 0.024(2) 0.022(2) 0.012(2) -0.0016(16) -0.0055(16) 0.0003(18) C63 0.047(3) 0.032(2) 0.041(3) -0.007(2) 0.003(2) 0.009(2) C64 0.019(2) 0.017(2) 0.026(2) -0.0005(17) -0.0004(17) 0.0011(17) C65 0.027(2) 0.027(2) 0.026(2) 0.0049(18) 0.0041(18) -0.0008(19) C66 0.024(2) 0.023(2) 0.039(3) 0.0028(19) 0.0019(19) -0.0069(18) C67 0.022(2) 0.020(2) 0.035(3) -0.0038(18) -0.0033(18) -0.0015(17) C68 0.026(2) 0.019(2) 0.025(2) -0.0013(17) -0.0041(18) 0.0025(18) C69 0.021(2) 0.0124(18) 0.023(2) 0.0002(16) -0.0017(17) 0.0028(15) C70 0.034(2) 0.033(2) 0.041(3) 0.000(2) -0.002(2) -0.0087(19) _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 P2 2.2416(10) . ? Pd1 P1 2.2738(10) . ? Pd1 Cl2 2.3306(10) . ? Pd1 Cl1 2.3523(10) . ? P1 C69 1.826(3) . ? P1 C1 1.830(4) . ? P1 C20 1.837(3) . ? P2 C43 1.809(3) . ? P2 C57 1.819(3) . ? P2 C29 1.827(3) . ? O1 C62 1.397(4) . ? O1 C64 1.401(4) . ? C1 C6 1.386(5) . ? C1 C2 1.396(5) . ? C2 C3 1.389(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(5) . ? C3 C11 1.532(5) . ? C4 C5 1.391(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 C7 1.534(5) . ? C6 H6 0.9500 . ? C7 C8 1.450(18) . ? C7 C10 1.487(13) . ? C7 C9A 1.516(11) . ? C7 C8A 1.537(14) . ? C7 C10A 1.578(11) . ? C7 C9 1.583(14) . ? 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 . ? C8A H8D 0.9800 . ? C8A H8E 0.9800 . ? C8A H8F 0.9800 . ? C9A H9D 0.9800 . ? C9A H9E 0.9800 . ? C9A H9F 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C13 1.519(6) . ? C11 C12 1.531(6) . ? C11 C14 1.536(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.385(5) . ? C15 C20 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.396(5) . ? C16 C21 1.535(5) . ? C17 C18 1.385(5) . ? C17 H17 0.9500 . ? C18 C19 1.400(5) . ? C18 C25 1.537(5) . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C21 C23 1.513(5) . ? C21 C24 1.525(5) . ? C21 C22 1.529(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.524(5) . ? C25 C28 1.525(5) . ? C25 C26 1.534(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.386(5) . ? C29 C34 1.394(5) . ? C30 C31 1.390(5) . ? C30 H30 0.9500 . ? C31 C32 1.389(5) . ? C31 C39 1.535(5) . ? C32 C33 1.390(5) . ? C32 H32 0.9500 . ? C33 C34 1.386(5) . ? C33 C35 1.544(5) . ? C34 H34 0.9500 . ? C35 C38 1.527(5) . ? C35 C37 1.530(5) . ? C35 C36 1.531(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.523(5) . ? C39 C40 1.526(6) . ? C39 C42 1.532(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.385(5) . ? C43 C44 1.392(5) . ? C44 C45 1.386(5) . ? C44 H44 0.9500 . ? C45 C46 1.404(5) . ? C45 C53 1.527(5) . ? C46 C47 1.385(5) . ? C46 H46 0.9500 . ? C47 C48 1.389(5) . ? C47 C49 1.529(5) . ? C48 H48 0.9500 . ? C49 C50 1.525(5) . ? C49 C51 1.531(5) . ? C49 C52 1.536(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.511(5) . ? C53 C56 1.521(5) . ? C53 C55 1.544(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.390(5) . ? C57 C62 1.392(5) . ? C58 C59 1.387(5) . ? C58 H58 0.9500 . ? C59 C60 1.392(5) . ? C59 C63 1.505(5) . ? C60 C61 1.377(5) . ? C60 H60 0.9500 . ? C61 C62 1.380(5) . ? C61 H61 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.373(5) . ? C64 C69 1.388(5) . ? C65 C66 1.381(5) . ? C65 H65 0.9500 . ? C66 C67 1.377(5) . ? C66 H66 0.9500 . ? C67 C68 1.387(5) . ? C67 C70 1.502(5) . ? C68 C69 1.393(5) . ? C68 H68 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 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 P2 Pd1 P1 97.67(4) . . ? P2 Pd1 Cl2 87.72(4) . . ? P1 Pd1 Cl2 170.05(4) . . ? P2 Pd1 Cl1 164.21(4) . . ? P1 Pd1 Cl1 85.81(4) . . ? Cl2 Pd1 Cl1 91.26(4) . . ? C69 P1 C1 109.93(16) . . ? C69 P1 C20 103.87(15) . . ? C1 P1 C20 99.26(15) . . ? C69 P1 Pd1 103.89(11) . . ? C1 P1 Pd1 111.83(12) . . ? C20 P1 Pd1 127.31(11) . . ? C43 P2 C57 109.54(16) . . ? C43 P2 C29 106.04(15) . . ? C57 P2 C29 101.18(15) . . ? C43 P2 Pd1 111.92(12) . . ? C57 P2 Pd1 113.18(11) . . ? C29 P2 Pd1 114.25(11) . . ? C62 O1 C64 117.1(2) . . ? C6 C1 C2 119.1(3) . . ? C6 C1 P1 121.3(3) . . ? C2 C1 P1 119.5(3) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 117.5(3) . . ? C4 C3 C11 120.5(3) . . ? C2 C3 C11 122.0(3) . . ? C3 C4 C5 123.3(4) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C4 C5 C6 117.2(3) . . ? C4 C5 C7 121.7(3) . . ? C6 C5 C7 121.1(3) . . ? C1 C6 C5 121.5(3) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C10 115.2(10) . . ? C8 C7 C9A 130.9(9) . . ? C10 C7 C9A 76.1(7) . . ? C8 C7 C5 106.7(10) . . ? C10 C7 C5 109.7(5) . . ? C9A C7 C5 113.9(5) . . ? C10 C7 C8A 132.9(10) . . ? C9A C7 C8A 108.7(7) . . ? C5 C7 C8A 110.2(8) . . ? C8 C7 C10A 80.3(9) . . ? C9A C7 C10A 106.9(7) . . ? C5 C7 C10A 112.9(4) . . ? C8A C7 C10A 103.7(8) . . ? C8 C7 C9 108.3(9) . . ? C10 C7 C9 107.6(8) . . ? C5 C7 C9 109.3(7) . . ? C8A C7 C9 81.5(7) . . ? C10A C7 C9 132.1(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C8A H8D 109.5 . . ? C7 C8A H8E 109.5 . . ? H8D C8A H8E 109.5 . . ? C7 C8A H8F 109.5 . . ? H8D C8A H8F 109.5 . . ? H8E C8A H8F 109.5 . . ? C7 C9A H9D 109.5 . . ? C7 C9A H9E 109.5 . . ? H9D C9A H9E 109.5 . . ? C7 C9A H9F 109.5 . . ? H9D C9A H9F 109.5 . . ? H9E C9A H9F 109.5 . . ? C7 C10A H10D 109.5 . . ? C7 C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C7 C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C13 C11 C12 109.9(4) . . ? C13 C11 C3 108.8(4) . . ? C12 C11 C3 111.7(3) . . ? C13 C11 C14 110.2(4) . . ? C12 C11 C14 106.3(4) . . ? C3 C11 C14 109.9(3) . . ? 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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 121.7(3) . . ? C16 C15 H15 119.2 . . ? C20 C15 H15 119.2 . . ? C15 C16 C17 117.4(3) . . ? C15 C16 C21 122.5(3) . . ? C17 C16 C21 120.1(3) . . ? C18 C17 C16 122.9(3) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C19 117.7(3) . . ? C17 C18 C25 122.0(3) . . ? C19 C18 C25 120.2(3) . . ? C20 C19 C18 120.9(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C15 C20 C19 119.4(3) . . ? C15 C20 P1 120.0(3) . . ? C19 C20 P1 120.2(3) . . ? C23 C21 C24 108.6(3) . . ? C23 C21 C22 107.9(3) . . ? C24 C21 C22 109.2(3) . . ? C23 C21 C16 112.1(3) . . ? C24 C21 C16 108.7(3) . . ? C22 C21 C16 110.3(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 109.8(3) . . ? C27 C25 C26 108.5(3) . . ? C28 C25 C26 107.5(3) . . ? C27 C25 C18 107.9(3) . . ? C28 C25 C18 110.3(3) . . ? C26 C25 C18 112.8(3) . . ? 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 . . ? 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 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 119.4(3) . . ? C30 C29 P2 120.0(3) . . ? C34 C29 P2 120.6(3) . . ? C29 C30 C31 121.2(3) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 117.9(3) . . ? C32 C31 C39 123.2(3) . . ? C30 C31 C39 118.8(3) . . ? C31 C32 C33 122.5(3) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C34 C33 C32 118.1(3) . . ? C34 C33 C35 120.8(3) . . ? C32 C33 C35 121.0(3) . . ? C33 C34 C29 120.9(3) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.6 . . ? C38 C35 C37 108.6(3) . . ? C38 C35 C36 109.3(3) . . ? C37 C35 C36 107.3(3) . . ? C38 C35 C33 108.7(3) . . ? C37 C35 C33 111.3(3) . . ? C36 C35 C33 111.5(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 109.4(4) . . ? C41 C39 C42 108.1(3) . . ? C40 C39 C42 109.9(4) . . ? C41 C39 C31 109.5(3) . . ? C40 C39 C31 108.5(3) . . ? C42 C39 C31 111.5(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 119.4(3) . . ? C48 C43 P2 123.4(3) . . ? C44 C43 P2 117.1(3) . . ? C45 C44 C43 121.7(3) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 116.8(3) . . ? C44 C45 C53 122.4(3) . . ? C46 C45 C53 120.8(3) . . ? C47 C46 C45 123.0(3) . . ? C47 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? C46 C47 C48 117.9(3) . . ? C46 C47 C49 122.6(3) . . ? C48 C47 C49 119.5(3) . . ? C43 C48 C47 121.1(3) . . ? C43 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C50 C49 C47 112.6(3) . . ? C50 C49 C51 108.0(3) . . ? C47 C49 C51 109.4(3) . . ? C50 C49 C52 108.4(3) . . ? C47 C49 C52 108.5(3) . . ? C51 C49 C52 109.9(3) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C56 110.1(3) . . ? C54 C53 C45 112.5(3) . . ? C56 C53 C45 109.7(3) . . ? C54 C53 C55 107.8(3) . . ? C56 C53 C55 107.4(3) . . ? C45 C53 C55 109.2(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C62 117.3(3) . . ? C58 C57 P2 124.1(3) . . ? C62 C57 P2 118.6(3) . . ? C59 C58 C57 122.4(3) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 117.9(3) . . ? C58 C59 C63 121.3(3) . . ? C60 C59 C63 120.7(3) . . ? C61 C60 C59 121.3(3) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C60 C61 C62 119.2(3) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? C61 C62 C57 121.7(3) . . ? C61 C62 O1 121.0(3) . . ? C57 C62 O1 117.2(3) . . ? C59 C63 H63A 109.5 . . ? C59 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C59 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C69 121.5(3) . . ? C65 C64 O1 117.5(3) . . ? C69 C64 O1 120.8(3) . . ? C64 C65 C66 119.5(3) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 121.3(3) . . ? C67 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? C66 C67 C68 118.0(3) . . ? C66 C67 C70 121.0(3) . . ? C68 C67 C70 121.0(3) . . ? C67 C68 C69 122.3(3) . . ? C67 C68 H68 118.8 . . ? C69 C68 H68 118.8 . . ? C64 C69 C68 117.3(3) . . ? C64 C69 P1 118.5(3) . . ? C68 C69 P1 123.8(3) . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 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 P2 Pd1 P1 C69 -100.36(12) . . . . ? Cl1 Pd1 P1 C69 64.14(12) . . . . ? P2 Pd1 P1 C1 141.12(12) . . . . ? Cl1 Pd1 P1 C1 -54.37(12) . . . . ? P2 Pd1 P1 C20 19.57(14) . . . . ? Cl1 Pd1 P1 C20 -175.93(14) . . . . ? P1 Pd1 P2 C43 -98.27(12) . . . . ? Cl2 Pd1 P2 C43 73.33(12) . . . . ? Cl1 Pd1 P2 C43 159.90(15) . . . . ? P1 Pd1 P2 C57 26.10(12) . . . . ? Cl2 Pd1 P2 C57 -162.30(12) . . . . ? Cl1 Pd1 P2 C57 -75.73(18) . . . . ? P1 Pd1 P2 C29 141.20(13) . . . . ? Cl2 Pd1 P2 C29 -47.20(13) . . . . ? Cl1 Pd1 P2 C29 39.37(19) . . . . ? C69 P1 C1 C6 -118.6(3) . . . . ? C20 P1 C1 C6 132.9(3) . . . . ? Pd1 P1 C1 C6 -3.8(3) . . . . ? C69 P1 C1 C2 65.7(3) . . . . ? C20 P1 C1 C2 -42.8(3) . . . . ? Pd1 P1 C1 C2 -179.5(2) . . . . ? C6 C1 C2 C3 3.2(5) . . . . ? P1 C1 C2 C3 179.0(3) . . . . ? C1 C2 C3 C4 0.0(5) . . . . ? C1 C2 C3 C11 -179.4(3) . . . . ? C2 C3 C4 C5 -2.2(5) . . . . ? C11 C3 C4 C5 177.2(3) . . . . ? C3 C4 C5 C6 1.1(5) . . . . ? C3 C4 C5 C7 177.7(3) . . . . ? C2 C1 C6 C5 -4.4(5) . . . . ? P1 C1 C6 C5 179.9(3) . . . . ? C4 C5 C6 C1 2.3(5) . . . . ? C7 C5 C6 C1 -174.3(3) . . . . ? C4 C5 C7 C8 -100.6(12) . . . . ? C6 C5 C7 C8 75.8(12) . . . . ? C4 C5 C7 C10 134.0(12) . . . . ? C6 C5 C7 C10 -49.5(12) . . . . ? C4 C5 C7 C9A 51.0(10) . . . . ? C6 C5 C7 C9A -132.6(10) . . . . ? C4 C5 C7 C8A -71.5(9) . . . . ? C6 C5 C7 C8A 104.9(9) . . . . ? C4 C5 C7 C10A 173.0(9) . . . . ? C6 C5 C7 C10A -10.5(9) . . . . ? C4 C5 C7 C9 16.3(11) . . . . ? C6 C5 C7 C9 -167.3(10) . . . . ? C4 C3 C11 C13 69.0(5) . . . . ? C2 C3 C11 C13 -111.5(4) . . . . ? C4 C3 C11 C12 -169.4(4) . . . . ? C2 C3 C11 C12 10.0(5) . . . . ? C4 C3 C11 C14 -51.7(5) . . . . ? C2 C3 C11 C14 127.7(4) . . . . ? C20 C15 C16 C17 -1.9(5) . . . . ? C20 C15 C16 C21 177.5(3) . . . . ? C15 C16 C17 C18 0.7(5) . . . . ? C21 C16 C17 C18 -178.7(3) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C16 C17 C18 C25 179.2(3) . . . . ? C17 C18 C19 C20 -1.7(5) . . . . ? C25 C18 C19 C20 -179.8(3) . . . . ? C16 C15 C20 C19 1.4(5) . . . . ? C16 C15 C20 P1 -171.0(3) . . . . ? C18 C19 C20 C15 0.5(5) . . . . ? C18 C19 C20 P1 172.8(3) . . . . ? C69 P1 C20 C15 -18.6(3) . . . . ? C1 P1 C20 C15 94.8(3) . . . . ? Pd1 P1 C20 C15 -138.5(2) . . . . ? C69 P1 C20 C19 169.2(3) . . . . ? C1 P1 C20 C19 -77.5(3) . . . . ? Pd1 P1 C20 C19 49.2(3) . . . . ? C15 C16 C21 C23 8.2(5) . . . . ? C17 C16 C21 C23 -172.5(3) . . . . ? C15 C16 C21 C24 -111.9(4) . . . . ? C17 C16 C21 C24 67.4(4) . . . . ? C15 C16 C21 C22 128.3(4) . . . . ? C17 C16 C21 C22 -52.3(5) . . . . ? C17 C18 C25 C27 -110.4(4) . . . . ? C19 C18 C25 C27 67.7(4) . . . . ? C17 C18 C25 C28 129.7(4) . . . . ? C19 C18 C25 C28 -52.2(4) . . . . ? C17 C18 C25 C26 9.5(5) . . . . ? C19 C18 C25 C26 -172.5(3) . . . . ? C43 P2 C29 C30 -36.8(3) . . . . ? C57 P2 C29 C30 -151.1(3) . . . . ? Pd1 P2 C29 C30 87.0(3) . . . . ? C43 P2 C29 C34 145.3(3) . . . . ? C57 P2 C29 C34 31.0(3) . . . . ? Pd1 P2 C29 C34 -91.0(3) . . . . ? C34 C29 C30 C31 -1.7(5) . . . . ? P2 C29 C30 C31 -179.6(3) . . . . ? C29 C30 C31 C32 1.3(5) . . . . ? C29 C30 C31 C39 178.0(3) . . . . ? C30 C31 C32 C33 0.2(5) . . . . ? C39 C31 C32 C33 -176.4(3) . . . . ? C31 C32 C33 C34 -1.2(5) . . . . ? C31 C32 C33 C35 -179.5(3) . . . . ? C32 C33 C34 C29 0.9(5) . . . . ? C35 C33 C34 C29 179.1(3) . . . . ? C30 C29 C34 C33 0.6(5) . . . . ? P2 C29 C34 C33 178.5(2) . . . . ? C34 C33 C35 C38 -92.9(4) . . . . ? C32 C33 C35 C38 85.4(4) . . . . ? C34 C33 C35 C37 26.7(4) . . . . ? C32 C33 C35 C37 -155.1(3) . . . . ? C34 C33 C35 C36 146.5(3) . . . . ? C32 C33 C35 C36 -35.3(4) . . . . ? C32 C31 C39 C41 -131.5(4) . . . . ? C30 C31 C39 C41 51.9(5) . . . . ? C32 C31 C39 C40 109.2(4) . . . . ? C30 C31 C39 C40 -67.4(5) . . . . ? C32 C31 C39 C42 -11.9(5) . . . . ? C30 C31 C39 C42 171.5(3) . . . . ? C57 P2 C43 C48 64.1(3) . . . . ? C29 P2 C43 C48 -44.3(3) . . . . ? Pd1 P2 C43 C48 -169.5(3) . . . . ? C57 P2 C43 C44 -118.7(3) . . . . ? C29 P2 C43 C44 132.9(3) . . . . ? Pd1 P2 C43 C44 7.7(3) . . . . ? C48 C43 C44 C45 -2.1(5) . . . . ? P2 C43 C44 C45 -179.4(3) . . . . ? C43 C44 C45 C46 0.3(5) . . . . ? C43 C44 C45 C53 179.3(3) . . . . ? C44 C45 C46 C47 1.8(5) . . . . ? C53 C45 C46 C47 -177.3(3) . . . . ? C45 C46 C47 C48 -1.9(5) . . . . ? C45 C46 C47 C49 179.8(3) . . . . ? C44 C43 C48 C47 2.0(5) . . . . ? P2 C43 C48 C47 179.1(3) . . . . ? C46 C47 C48 C43 -0.1(5) . . . . ? C49 C47 C48 C43 178.3(3) . . . . ? C46 C47 C49 C50 -7.0(5) . . . . ? C48 C47 C49 C50 174.7(3) . . . . ? C46 C47 C49 C51 -127.1(4) . . . . ? C48 C47 C49 C51 54.6(4) . . . . ? C46 C47 C49 C52 113.0(4) . . . . ? C48 C47 C49 C52 -65.3(4) . . . . ? C44 C45 C53 C54 -6.3(5) . . . . ? C46 C45 C53 C54 172.7(4) . . . . ? C44 C45 C53 C56 -129.2(4) . . . . ? C46 C45 C53 C56 49.9(5) . . . . ? C44 C45 C53 C55 113.3(4) . . . . ? C46 C45 C53 C55 -67.6(4) . . . . ? C43 P2 C57 C58 -13.5(3) . . . . ? C29 P2 C57 C58 98.1(3) . . . . ? Pd1 P2 C57 C58 -139.2(3) . . . . ? C43 P2 C57 C62 165.7(3) . . . . ? C29 P2 C57 C62 -82.6(3) . . . . ? Pd1 P2 C57 C62 40.1(3) . . . . ? C62 C57 C58 C59 0.5(5) . . . . ? P2 C57 C58 C59 179.8(3) . . . . ? C57 C58 C59 C60 0.9(5) . . . . ? C57 C58 C59 C63 -177.4(3) . . . . ? C58 C59 C60 C61 -0.6(5) . . . . ? C63 C59 C60 C61 177.6(3) . . . . ? C59 C60 C61 C62 -1.0(5) . . . . ? C60 C61 C62 C57 2.5(5) . . . . ? C60 C61 C62 O1 178.9(3) . . . . ? C58 C57 C62 C61 -2.3(5) . . . . ? P2 C57 C62 C61 178.4(3) . . . . ? C58 C57 C62 O1 -178.8(3) . . . . ? P2 C57 C62 O1 2.0(4) . . . . ? C64 O1 C62 C61 50.5(4) . . . . ? C64 O1 C62 C57 -133.0(3) . . . . ? C62 O1 C64 C65 -112.2(3) . . . . ? C62 O1 C64 C69 72.3(4) . . . . ? C69 C64 C65 C66 -1.1(5) . . . . ? O1 C64 C65 C66 -176.5(3) . . . . ? C64 C65 C66 C67 -1.0(5) . . . . ? C65 C66 C67 C68 1.4(5) . . . . ? C65 C66 C67 C70 -178.4(3) . . . . ? C66 C67 C68 C69 0.2(5) . . . . ? C70 C67 C68 C69 180.0(3) . . . . ? C65 C64 C69 C68 2.5(5) . . . . ? O1 C64 C69 C68 177.9(3) . . . . ? C65 C64 C69 P1 -171.6(3) . . . . ? O1 C64 C69 P1 3.7(4) . . . . ? C67 C68 C69 C64 -2.1(5) . . . . ? C67 C68 C69 P1 171.7(3) . . . . ? C1 P1 C69 C64 167.4(3) . . . . ? C20 P1 C69 C64 -87.2(3) . . . . ? Pd1 P1 C69 C64 47.6(3) . . . . ? C1 P1 C69 C68 -6.4(3) . . . . ? C20 P1 C69 C68 99.1(3) . . . . ? Pd1 P1 C69 C68 -126.2(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.155 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.062