Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Heaton, B.' 'Clegg, William' 'Eastham, Graham R.' 'Elsegood, Mark R. J.' 'Iggo, J.' 'Tooze, R. P.' 'Whyman, R.' 'Zacchini, Stefano' _publ_contact_author_name 'Prof B Heaton' _publ_contact_author_address ; Department of Chemistry University of Liverpool P O Box 147 LIVERPOOL L69 3BX U.K. ; _publ_contact_author_email 'BTH@LIV.AC.UK' _publ_section_title ; Synthesis and Reactivity of Palladium hydrido-solvento complexes: including a Key intermediate in the Catalytic Methoxycarbonylation of Ethene to Methyl Propanoate ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; data_983_0009_for_s._Zacchini _database_code_CSD 162523 #------------------------------------------------------------------------------ _audit_creation_date '1998-04-06' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 11.87(2) _cell_length_b 15.410(7) _cell_length_c 11.168(6) _cell_angle_alpha 109.17(4) _cell_angle_beta 108.21(7) _cell_angle_gamma 72.06(6) _cell_volume 1784(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 835.36 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H66 O8 P2 Pd S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 884.00 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type none _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 16\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% -14.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -2 2 2 -1 2 1 -2 _diffrn_reflns_number 4940 _reflns_number_total 4668 _reflns_number_observed 3721 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01724 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 22.54 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04127 _diffrn_orient_matrix_UB_12 0.04128 _diffrn_orient_matrix_UB_13 -0.06144 _diffrn_orient_matrix_UB_21 0.02540 _diffrn_orient_matrix_UB_22 0.05520 _diffrn_orient_matrix_UB_23 0.07005 _diffrn_orient_matrix_UB_31 0.07715 _diffrn_orient_matrix_UB_32 -0.01517 _diffrn_orient_matrix_UB_33 -0.02883 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 2 -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) -0.22939(4) 0.34269(3) 0.29194(4) 0.0276(1) 1.000 . Uani d ? S(1) -0.3507(1) 0.5072(1) 0.4309(1) 0.0300(4) 1.000 . Uani d ? S(2) 0.2020(1) 0.1871(1) -0.1602(2) 0.0318(5) 1.000 . Uani d ? S(3) 0.4601(2) 0.1728(1) -0.3664(2) 0.0468(6) 1.000 . Uani d ? P(1) -0.1112(1) 0.3175(1) 0.1527(1) 0.0260(4) 1.000 . Uani d ? P(2) -0.2317(1) 0.1922(1) 0.2733(1) 0.0244(4) 1.000 . Uani d ? O(1) -0.2559(4) 0.4962(3) 0.3622(4) 0.036(1) 1.000 . Uani d ? O(2) -0.3530(4) 0.4089(3) 0.4214(4) 0.036(1) 1.000 . Uani d ? O(3) -0.3341(4) 0.5663(3) 0.5601(4) 0.051(1) 1.000 . Uani d ? O(4) 0.0795(4) 0.1785(3) -0.1780(4) 0.049(1) 1.000 . Uani d ? O(5) 0.2819(4) 0.1731(3) -0.0389(4) 0.052(1) 1.000 . Uani d ? O(6) 0.2529(4) 0.1262(3) -0.2726(4) 0.039(1) 1.000 . Uani d ? O(7) 0.4111(6) 0.2674(4) -0.3054(6) 0.084(2) 1.000 . Uani d ? O(8) 0.4628(4) 0.1072(4) -0.2887(5) 0.057(2) 1.000 . Uani d ? O(9) 0.5778(4) 0.1527(5) -0.3894(6) 0.084(2) 1.000 . Uani d ? C(1) -0.0499(5) 0.1984(4) 0.0594(5) 0.027(2) 1.000 . Uani d ? C(2) 0.0303(5) 0.1240(4) 0.1259(5) 0.033(2) 1.000 . Uani d ? C(3) 0.1560(6) 0.0949(4) 0.1298(6) 0.041(2) 1.000 . Uani d ? C(4) 0.2302(5) 0.0211(4) 0.1805(6) 0.037(2) 1.000 . Uani d ? C(5) 0.1816(6) -0.0277(4) 0.2261(6) 0.038(2) 1.000 . Uani d ? C(6) 0.0574(6) -0.0042(4) 0.2193(6) 0.042(2) 1.000 . Uani d ? C(7) -0.0195(5) 0.0726(4) 0.1715(6) 0.033(2) 1.000 . Uani d ? C(8) -0.1540(5) 0.0921(4) 0.1612(5) 0.029(2) 1.000 . Uani d ? C(9) 0.0244(5) 0.3704(4) 0.2519(6) 0.030(2) 1.000 . Uani d ? C(10) 0.0755(6) 0.3329(5) 0.3737(6) 0.038(2) 1.000 . Uani d ? C(11) 0.1249(6) 0.3401(5) 0.1761(6) 0.041(2) 1.000 . Uani d ? C(12) -0.0114(6) 0.4786(4) 0.2935(7) 0.041(2) 1.000 . Uani d ? C(13) -0.2076(5) 0.3763(4) 0.0167(6) 0.034(2) 1.000 . Uani d ? C(14) -0.2853(6) 0.3103(5) -0.0844(6) 0.050(2) 1.000 . Uani d ? C(15) -0.1295(6) 0.3962(5) -0.0534(6) 0.049(2) 1.000 . Uani d ? C(16) -0.2926(6) 0.4683(5) 0.0699(6) 0.044(2) 1.000 . Uani d ? C(17) -0.1636(5) 0.1708(4) 0.4415(5) 0.029(2) 1.000 . Uani d ? C(18) -0.0286(6) 0.1741(5) 0.4789(6) 0.043(2) 1.000 . Uani d ? C(19) -0.1747(6) 0.0737(4) 0.4404(6) 0.046(2) 1.000 . Uani d ? C(20) -0.2208(6) 0.2459(5) 0.5471(6) 0.045(2) 1.000 . Uani d ? C(21) -0.3962(5) 0.1819(4) 0.2043(6) 0.034(2) 1.000 . Uani d ? C(22) -0.4076(6) 0.0792(5) 0.1489(7) 0.051(2) 1.000 . Uani d ? C(23) -0.4733(6) 0.2316(5) 0.3041(7) 0.051(2) 1.000 . Uani d ? C(24) -0.4460(6) 0.2301(6) 0.0920(8) 0.059(2) 1.000 . Uani d ? C(25) -0.4910(5) 0.5561(4) 0.3405(6) 0.039(2) 1.000 . Uani d ? C(26) 0.1910(8) 0.3024(5) -0.1646(8) 0.066(3) 1.000 . Uani d ? C(27) 0.3590(8) 0.1393(7) -0.5117(8) 0.083(3) 1.000 . Uani d ? H(1) -0.1180 0.1740 0.0033 0.033 1.000 . Uiso c ? H(2) -0.0047 0.2060 0.0078 0.033 1.000 . Uiso c ? H(3) 0.1905 0.1271 0.0955 0.050 1.000 . Uiso c ? H(4) 0.3152 0.0039 0.1840 0.045 1.000 . Uiso c ? H(5) 0.2333 -0.0783 0.2624 0.048 1.000 . Uiso c ? H(6) 0.0247 -0.0409 0.2480 0.052 1.000 . Uiso c ? H(7) -0.1680 0.0369 0.1694 0.036 1.000 . Uiso c ? H(8) -0.1937 0.0998 0.0759 0.036 1.000 . Uiso c ? H(9) 0.0147 0.3527 0.4222 0.048 1.000 . Uiso c ? H(10) 0.0973 0.2659 0.3482 0.048 1.000 . Uiso c ? H(11) 0.1447 0.3566 0.4257 0.048 1.000 . Uiso c ? H(12) 0.1478 0.2735 0.1497 0.052 1.000 . Uiso c ? H(13) 0.0942 0.3646 0.1011 0.052 1.000 . Uiso c ? H(14) 0.1933 0.3646 0.2304 0.052 1.000 . Uiso c ? H(15) 0.0582 0.5022 0.3464 0.050 1.000 . Uiso c ? H(16) -0.0425 0.5024 0.2183 0.050 1.000 . Uiso c ? H(17) -0.0721 0.4982 0.3419 0.050 1.000 . Uiso c ? H(18) -0.3373 0.2987 -0.0441 0.062 1.000 . Uiso c ? H(19) -0.3339 0.3389 -0.1531 0.062 1.000 . Uiso c ? H(20) -0.2343 0.2523 -0.1187 0.062 1.000 . Uiso c ? H(21) -0.0785 0.3386 -0.0894 0.061 1.000 . Uiso c ? H(22) -0.1807 0.4248 -0.1208 0.061 1.000 . Uiso c ? H(23) -0.0802 0.4375 0.0076 0.061 1.000 . Uiso c ? H(24) -0.2460 0.5104 0.1324 0.055 1.000 . Uiso c ? H(25) -0.3413 0.4959 0.0002 0.055 1.000 . Uiso c ? H(26) -0.3439 0.4556 0.1095 0.055 1.000 . Uiso c ? H(27) 0.0089 0.1606 0.5611 0.053 1.000 . Uiso c ? H(28) 0.0110 0.1284 0.4147 0.053 1.000 . Uiso c ? H(29) -0.0224 0.2350 0.4831 0.053 1.000 . Uiso c ? H(30) -0.2581 0.0737 0.4231 0.057 1.000 . Uiso c ? H(31) -0.1394 0.0267 0.3739 0.057 1.000 . Uiso c ? H(32) -0.1330 0.0612 0.5224 0.057 1.000 . Uiso c ? H(33) -0.1812 0.2316 0.6288 0.055 1.000 . Uiso c ? H(34) -0.2124 0.3057 0.5502 0.055 1.000 . Uiso c ? H(35) -0.3050 0.2462 0.5279 0.055 1.000 . Uiso c ? H(36) -0.4910 0.0781 0.1111 0.064 1.000 . Uiso c ? H(37) -0.3621 0.0490 0.0843 0.064 1.000 . Uiso c ? H(38) -0.3773 0.0485 0.2171 0.064 1.000 . Uiso c ? H(39) -0.4689 0.2965 0.3363 0.062 1.000 . Uiso c ? H(40) -0.5556 0.2282 0.2639 0.062 1.000 . Uiso c ? H(41) -0.4438 0.2028 0.3741 0.062 1.000 . Uiso c ? H(42) -0.4402 0.2939 0.1239 0.074 1.000 . Uiso c ? H(43) -0.4001 0.1980 0.0278 0.074 1.000 . Uiso c ? H(44) -0.5291 0.2271 0.0542 0.074 1.000 . Uiso c ? H(45) -0.4915 0.6175 0.3399 0.048 1.000 . Uiso c ? H(46) -0.5041 0.5175 0.2536 0.048 1.000 . Uiso c ? H(47) -0.5539 0.5593 0.3787 0.048 1.000 . Uiso c ? H(48) 0.2799 0.1465 -0.4995 0.100 1.000 . Uiso c ? H(49) 0.3502 0.1749 -0.5714 0.100 1.000 . Uiso c ? H(50) 0.3865 0.0731 -0.5546 0.100 1.000 . Uiso c ? H(51) 0.2697 0.3115 -0.1570 0.079 1.000 . Uiso c ? H(52) 0.1394 0.3145 -0.2457 0.079 1.000 . Uiso c ? H(53) 0.1580 0.3481 -0.0953 0.079 1.000 . Uiso c ? H(54) 0.3722 0.1093 -0.2794 0.048 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0262(3) 0.0238(3) 0.0297(3) -0.0039(2) 0.0045(2) 0.0061(2) S(1) 0.0230(8) 0.0258(8) 0.0361(9) -0.0028(6) 0.0074(7) 0.0030(7) S(2) 0.0316(9) 0.0309(9) 0.0382(9) -0.0111(7) 0.0101(7) 0.0099(7) S(3) 0.0319(10) 0.065(1) 0.052(1) -0.0077(9) 0.0118(8) 0.0267(10) P(1) 0.0267(8) 0.0232(8) 0.0256(8) -0.0043(7) 0.0025(7) 0.0076(7) P(2) 0.0249(8) 0.0209(8) 0.0242(8) -0.0037(7) 0.0025(7) 0.0061(7) O(1) 0.034(2) 0.028(2) 0.046(3) -0.008(2) 0.017(2) 0.002(2) O(2) 0.035(2) 0.028(2) 0.047(3) -0.003(2) 0.013(2) 0.013(2) O(3) 0.040(3) 0.054(3) 0.045(3) -0.012(2) 0.013(2) -0.012(2) O(4) 0.034(3) 0.074(3) 0.048(3) -0.021(2) 0.009(2) 0.021(3) O(5) 0.043(3) 0.070(3) 0.040(3) -0.018(2) 0.000(2) 0.017(2) O(6) 0.046(3) 0.032(2) 0.048(3) -0.013(2) 0.021(2) 0.007(2) O(7) 0.117(5) 0.046(3) 0.116(5) -0.029(3) 0.070(4) 0.006(3) O(8) 0.036(3) 0.074(4) 0.072(3) 0.003(2) 0.018(2) 0.039(3) O(9) 0.031(3) 0.154(6) 0.090(4) -0.006(3) 0.018(3) 0.072(4) C(1) 0.028(3) 0.026(3) 0.024(3) -0.004(3) 0.010(3) 0.001(3) C(2) 0.039(4) 0.032(3) 0.023(3) -0.011(3) 0.002(3) 0.004(3) C(3) 0.044(4) 0.038(4) 0.039(4) -0.012(3) 0.014(3) 0.000(3) C(4) 0.029(3) 0.032(4) 0.034(4) 0.005(3) 0.002(3) 0.007(3) C(5) 0.035(4) 0.033(4) 0.034(4) 0.009(3) 0.005(3) 0.012(3) C(6) 0.062(5) 0.027(4) 0.033(4) -0.007(3) 0.009(3) 0.008(3) C(7) 0.038(4) 0.027(3) 0.027(3) -0.007(3) 0.004(3) 0.003(3) C(8) 0.033(3) 0.022(3) 0.032(3) -0.011(3) 0.006(3) 0.005(3) C(9) 0.026(3) 0.032(3) 0.033(3) -0.009(3) 0.010(3) 0.002(3) C(10) 0.036(4) 0.046(4) 0.028(4) -0.019(3) -0.001(3) 0.002(3) C(11) 0.036(4) 0.047(4) 0.039(4) -0.016(3) 0.011(3) 0.000(3) C(12) 0.036(4) 0.035(4) 0.054(4) -0.017(3) 0.013(3) 0.005(3) C(13) 0.041(4) 0.027(3) 0.031(3) 0.000(3) 0.003(3) 0.014(3) C(14) 0.062(5) 0.039(4) 0.036(4) -0.008(4) -0.011(3) 0.019(3) C(15) 0.051(4) 0.059(5) 0.041(4) -0.004(4) 0.010(3) 0.027(4) C(16) 0.042(4) 0.044(4) 0.045(4) -0.004(3) 0.000(3) 0.023(3) C(17) 0.035(3) 0.025(3) 0.026(3) -0.002(3) 0.007(3) 0.009(3) C(18) 0.038(4) 0.057(4) 0.029(4) -0.007(3) -0.002(3) 0.018(3) C(19) 0.063(5) 0.034(4) 0.041(4) -0.010(3) 0.004(3) 0.017(3) C(20) 0.058(5) 0.042(4) 0.032(4) -0.005(3) 0.015(3) 0.009(3) C(21) 0.025(3) 0.034(4) 0.042(4) -0.010(3) -0.004(3) 0.017(3) C(22) 0.035(4) 0.044(4) 0.070(5) -0.020(3) 0.000(4) 0.009(4) C(23) 0.027(4) 0.050(4) 0.072(5) -0.014(3) 0.013(4) 0.003(4) C(24) 0.037(4) 0.074(5) 0.071(5) -0.025(4) -0.022(4) 0.042(4) C(25) 0.027(3) 0.035(4) 0.053(4) 0.006(3) 0.007(3) 0.022(3) C(26) 0.094(6) 0.032(4) 0.090(6) -0.007(4) 0.064(5) 0.005(4) C(27) 0.056(5) 0.130(8) 0.066(6) -0.025(5) 0.001(4) 0.039(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00031|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3721 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_obs 0.0397 _refine_ls_wR_factor_all 0.0488 _refine_ls_wR_factor_obs 0.0488 _refine_ls_goodness_of_fit_all 1.701 _refine_ls_goodness_of_fit_obs 1.701 _refine_ls_shift/esd_max 0.0001 _refine_ls_shift/esd_mean 0.0111 _refine_diff_density_min -0.72 _refine_diff_density_max 0.64 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) S(1) 2.734(2) . . yes Pd(1) P(1) 2.274(2) . . yes Pd(1) P(2) 2.267(2) . . yes Pd(1) O(1) 2.188(4) . . yes Pd(1) O(2) 2.172(4) . . yes S(1) O(1) 1.490(4) . . yes S(1) O(2) 1.492(4) . . yes S(1) O(3) 1.421(4) . . yes S(1) C(25) 1.741(6) . . yes S(2) O(4) 1.446(5) . . yes S(2) O(5) 1.429(4) . . yes S(2) O(6) 1.475(4) . . yes S(2) C(26) 1.758(7) . . yes S(3) O(7) 1.414(6) . . yes S(3) O(8) 1.522(5) . . yes S(3) O(9) 1.420(5) . . yes S(3) C(27) 1.719(9) . . yes P(1) C(1) 1.839(6) . . yes P(1) C(9) 1.892(6) . . yes P(1) C(13) 1.901(6) . . yes P(2) C(8) 1.837(6) . . yes P(2) C(17) 1.894(6) . . yes P(2) C(21) 1.897(6) . . yes O(8) H(54) 1.10 . . no C(1) C(2) 1.489(8) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) C(3) 1.410(9) . . yes C(2) C(7) 1.406(8) . . yes C(3) C(4) 1.373(9) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.364(9) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.388(9) . . yes C(5) H(5) 0.95 . . no C(6) C(7) 1.402(8) . . yes C(6) H(6) 0.95 . . no C(7) C(8) 1.505(8) . . yes C(8) H(7) 0.95 . . no C(8) H(8) 0.95 . . no C(9) C(10) 1.528(8) . . yes C(9) C(11) 1.544(8) . . yes C(9) C(12) 1.535(8) . . yes C(10) H(9) 0.95 . . no C(10) H(10) 0.95 . . no C(10) H(11) 0.95 . . no C(11) H(12) 0.94 . . no C(11) H(13) 0.95 . . no C(11) H(14) 0.95 . . no C(12) H(15) 0.95 . . no C(12) H(16) 0.95 . . no C(12) H(17) 0.95 . . no C(13) C(14) 1.527(9) . . yes C(13) C(15) 1.534(9) . . yes C(13) C(16) 1.523(9) . . yes C(14) H(18) 0.95 . . no C(14) H(19) 0.95 . . no C(14) H(20) 0.95 . . no C(15) H(21) 0.95 . . no C(15) H(22) 0.95 . . no C(15) H(23) 0.95 . . no C(16) H(24) 0.95 . . no C(16) H(25) 0.95 . . no C(16) H(26) 0.95 . . no C(17) C(18) 1.537(9) . . yes C(17) C(19) 1.538(8) . . yes C(17) C(20) 1.520(8) . . yes C(18) H(27) 0.95 . . no C(18) H(28) 0.95 . . no C(18) H(29) 0.95 . . no C(19) H(30) 0.95 . . no C(19) H(31) 0.95 . . no C(19) H(32) 0.95 . . no C(20) H(33) 0.95 . . no C(20) H(34) 0.95 . . no C(20) H(35) 0.95 . . no C(21) C(22) 1.530(9) . . yes C(21) C(23) 1.520(9) . . yes C(21) C(24) 1.533(9) . . yes C(22) H(36) 0.95 . . no C(22) H(37) 0.95 . . no C(22) H(38) 0.95 . . no C(23) H(39) 0.96 . . no C(23) H(40) 0.95 . . no C(23) H(41) 0.94 . . no C(24) H(42) 0.95 . . no C(24) H(43) 0.95 . . no C(24) H(44) 0.95 . . no C(25) H(45) 0.95 . . no C(25) H(46) 0.95 . . no C(25) H(47) 0.95 . . no C(26) H(51) 0.96 . . no C(26) H(52) 0.96 . . no C(26) H(53) 0.95 . . no C(27) H(48) 0.96 . . no C(27) H(49) 0.96 . . no C(27) H(50) 0.97 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Pd(1) P(1) 130.51(6) . . . yes S(1) Pd(1) P(2) 128.77(6) . . . yes S(1) Pd(1) O(1) 32.9(1) . . . yes S(1) Pd(1) O(2) 32.9(1) . . . yes P(1) Pd(1) P(2) 100.59(6) . . . yes P(1) Pd(1) O(1) 98.2(1) . . . yes P(1) Pd(1) O(2) 163.2(1) . . . yes P(2) Pd(1) O(1) 161.0(1) . . . yes P(2) Pd(1) O(2) 95.8(1) . . . yes O(1) Pd(1) O(2) 65.7(1) . . . yes Pd(1) S(1) O(1) 53.0(2) . . . yes Pd(1) S(1) O(2) 52.4(2) . . . yes Pd(1) S(1) O(3) 138.3(2) . . . yes Pd(1) S(1) C(25) 113.7(2) . . . yes O(1) S(1) O(2) 104.9(2) . . . yes O(1) S(1) O(3) 114.6(3) . . . yes O(1) S(1) C(25) 107.7(3) . . . yes O(2) S(1) O(3) 114.2(3) . . . yes O(2) S(1) C(25) 106.9(3) . . . yes O(3) S(1) C(25) 108.0(3) . . . yes O(4) S(2) O(5) 114.1(3) . . . yes O(4) S(2) O(6) 110.8(3) . . . yes O(4) S(2) C(26) 107.0(3) . . . yes O(5) S(2) O(6) 112.1(3) . . . yes O(5) S(2) C(26) 107.9(4) . . . yes O(6) S(2) C(26) 104.3(3) . . . yes O(7) S(3) O(8) 110.2(3) . . . yes O(7) S(3) O(9) 116.9(4) . . . yes O(7) S(3) C(27) 108.0(5) . . . yes O(8) S(3) O(9) 108.3(3) . . . yes O(8) S(3) C(27) 103.4(4) . . . yes O(9) S(3) C(27) 109.2(4) . . . yes Pd(1) P(1) C(1) 122.0(2) . . . yes Pd(1) P(1) C(9) 106.6(2) . . . yes Pd(1) P(1) C(13) 107.7(2) . . . yes C(1) P(1) C(9) 106.5(3) . . . yes C(1) P(1) C(13) 101.5(3) . . . yes C(9) P(1) C(13) 112.7(3) . . . yes Pd(1) P(2) C(8) 121.2(2) . . . yes Pd(1) P(2) C(17) 106.9(2) . . . yes Pd(1) P(2) C(21) 106.9(2) . . . yes C(8) P(2) C(17) 106.4(3) . . . yes C(8) P(2) C(21) 101.7(3) . . . yes C(17) P(2) C(21) 114.0(3) . . . yes Pd(1) O(1) S(1) 94.1(2) . . . yes Pd(1) O(2) S(1) 94.7(2) . . . yes S(3) O(8) H(54) 113.7 . . . no P(1) C(1) C(2) 121.3(4) . . . yes P(1) C(1) H(1) 106.6 . . . no P(1) C(1) H(2) 106.4 . . . no C(2) C(1) H(1) 106.4 . . . no C(2) C(1) H(2) 106.6 . . . no H(1) C(1) H(2) 109.1 . . . no C(1) C(2) C(3) 120.8(5) . . . yes C(1) C(2) C(7) 120.7(5) . . . yes C(3) C(2) C(7) 117.9(6) . . . yes C(2) C(3) C(4) 122.1(6) . . . yes C(2) C(3) H(3) 119.0 . . . no C(4) C(3) H(3) 118.8 . . . no C(3) C(4) C(5) 119.6(6) . . . yes C(3) C(4) H(4) 120.4 . . . no C(5) C(4) H(4) 120.0 . . . no C(4) C(5) C(6) 120.3(5) . . . yes C(4) C(5) H(5) 119.6 . . . no C(6) C(5) H(5) 120.1 . . . no C(5) C(6) C(7) 121.0(6) . . . yes C(5) C(6) H(6) 119.1 . . . no C(7) C(6) H(6) 119.9 . . . no C(2) C(7) C(6) 118.9(6) . . . yes C(2) C(7) C(8) 122.4(5) . . . yes C(6) C(7) C(8) 118.5(5) . . . yes P(2) C(8) C(7) 122.2(4) . . . yes P(2) C(8) H(7) 106.2 . . . no P(2) C(8) H(8) 106.3 . . . no C(7) C(8) H(7) 106.2 . . . no C(7) C(8) H(8) 106.3 . . . no H(7) C(8) H(8) 109.3 . . . no P(1) C(9) C(10) 106.7(4) . . . yes P(1) C(9) C(11) 111.7(4) . . . yes P(1) C(9) C(12) 112.1(4) . . . yes C(10) C(9) C(11) 108.7(5) . . . yes C(10) C(9) C(12) 109.1(5) . . . yes C(11) C(9) C(12) 108.6(5) . . . yes C(9) C(10) H(9) 109.2 . . . no C(9) C(10) H(10) 109.2 . . . no C(9) C(10) H(11) 109.7 . . . no H(9) C(10) H(10) 109.2 . . . no H(9) C(10) H(11) 109.6 . . . no H(10) C(10) H(11) 109.9 . . . no C(9) C(11) H(12) 109.5 . . . no C(9) C(11) H(13) 109.1 . . . no C(9) C(11) H(14) 109.5 . . . no H(12) C(11) H(13) 109.5 . . . no H(12) C(11) H(14) 110.0 . . . no H(13) C(11) H(14) 109.2 . . . no C(9) C(12) H(15) 109.5 . . . no C(9) C(12) H(16) 109.5 . . . no C(9) C(12) H(17) 109.4 . . . no H(15) C(12) H(16) 109.5 . . . no H(15) C(12) H(17) 109.4 . . . no H(16) C(12) H(17) 109.5 . . . no P(1) C(13) C(14) 108.8(4) . . . yes P(1) C(13) C(15) 112.2(4) . . . yes P(1) C(13) C(16) 110.6(4) . . . yes C(14) C(13) C(15) 107.5(5) . . . yes C(14) C(13) C(16) 108.2(5) . . . yes C(15) C(13) C(16) 109.3(5) . . . yes C(13) C(14) H(18) 109.3 . . . no C(13) C(14) H(19) 109.7 . . . no C(13) C(14) H(20) 109.8 . . . no H(18) C(14) H(19) 109.1 . . . no H(18) C(14) H(20) 109.3 . . . no H(19) C(14) H(20) 109.6 . . . no C(13) C(15) H(21) 109.5 . . . no C(13) C(15) H(22) 109.6 . . . no C(13) C(15) H(23) 109.2 . . . no H(21) C(15) H(22) 109.7 . . . no H(21) C(15) H(23) 109.3 . . . no H(22) C(15) H(23) 109.5 . . . no C(13) C(16) H(24) 109.5 . . . no C(13) C(16) H(25) 109.4 . . . no C(13) C(16) H(26) 109.3 . . . no H(24) C(16) H(25) 109.6 . . . no H(24) C(16) H(26) 109.7 . . . no H(25) C(16) H(26) 109.4 . . . no P(2) C(17) C(18) 107.6(4) . . . yes P(2) C(17) C(19) 110.2(4) . . . yes P(2) C(17) C(20) 113.7(4) . . . yes C(18) C(17) C(19) 109.9(5) . . . yes C(18) C(17) C(20) 106.3(5) . . . yes C(19) C(17) C(20) 109.0(5) . . . yes C(17) C(18) H(27) 109.5 . . . no C(17) C(18) H(28) 109.3 . . . no C(17) C(18) H(29) 109.5 . . . no H(27) C(18) H(28) 109.5 . . . no H(27) C(18) H(29) 109.8 . . . no H(28) C(18) H(29) 109.3 . . . no C(17) C(19) H(30) 109.4 . . . no C(17) C(19) H(31) 109.1 . . . no C(17) C(19) H(32) 109.3 . . . no H(30) C(19) H(31) 109.5 . . . no H(30) C(19) H(32) 110.0 . . . no H(31) C(19) H(32) 109.6 . . . no C(17) C(20) H(33) 109.2 . . . no C(17) C(20) H(34) 109.6 . . . no C(17) C(20) H(35) 109.2 . . . no H(33) C(20) H(34) 109.9 . . . no H(33) C(20) H(35) 109.2 . . . no H(34) C(20) H(35) 109.7 . . . no P(2) C(21) C(22) 112.5(4) . . . yes P(2) C(21) C(23) 112.5(4) . . . yes P(2) C(21) C(24) 106.0(4) . . . yes C(22) C(21) C(23) 109.0(5) . . . yes C(22) C(21) C(24) 108.1(5) . . . yes C(23) C(21) C(24) 108.6(6) . . . yes C(21) C(22) H(36) 109.0 . . . no C(21) C(22) H(37) 108.9 . . . no C(21) C(22) H(38) 109.2 . . . no H(36) C(22) H(37) 109.7 . . . no H(36) C(22) H(38) 109.9 . . . no H(37) C(22) H(38) 110.1 . . . no C(21) C(23) H(39) 109.1 . . . no C(21) C(23) H(40) 109.6 . . . no C(21) C(23) H(41) 109.7 . . . no H(39) C(23) H(40) 109.0 . . . no H(39) C(23) H(41) 109.3 . . . no H(40) C(23) H(41) 110.1 . . . no C(21) C(24) H(42) 109.8 . . . no C(21) C(24) H(43) 109.1 . . . no C(21) C(24) H(44) 109.3 . . . no H(42) C(24) H(43) 109.8 . . . no H(42) C(24) H(44) 109.6 . . . no H(43) C(24) H(44) 109.3 . . . no S(1) C(25) H(45) 109.6 . . . no S(1) C(25) H(46) 109.4 . . . no S(1) C(25) H(47) 109.4 . . . no H(45) C(25) H(46) 109.6 . . . no H(45) C(25) H(47) 109.6 . . . no H(46) C(25) H(47) 109.3 . . . no S(2) C(26) H(51) 110.8 . . . no S(2) C(26) H(52) 110.7 . . . no S(2) C(26) H(53) 111.2 . . . no H(51) C(26) H(52) 107.6 . . . no H(51) C(26) H(53) 108.3 . . . no H(52) C(26) H(53) 108.2 . . . no S(3) C(27) H(48) 111.9 . . . no S(3) C(27) H(49) 111.9 . . . no S(3) C(27) H(50) 110.9 . . . no H(48) C(27) H(49) 108.2 . . . no H(48) C(27) H(50) 106.9 . . . no H(49) C(27) H(50) 106.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(2) H(54) 2.5367 . . no S(2) O(8) 3.526(6) . . no S(3) O(6) 3.295(5) . . no O(1) H(11) 2.9759 . 2_566 no O(2) H(47) 2.6339 . 2_466 no O(2) C(25) 3.509(8) . 2_466 no O(3) H(14) 2.5333 . 2_566 no O(3) H(11) 2.7893 . 2_566 no O(3) H(39) 2.8847 . 2_466 no O(3) H(47) 3.0016 . 2_466 no O(3) C(11) 3.430(8) . 2_566 no O(3) C(23) 3.451(8) . 2_466 no O(4) H(2) 2.4379 . . no O(4) H(6) 2.5614 . 2 no O(4) H(21) 2.7001 . . no O(4) H(27) 2.7113 . 1_554 no O(4) C(1) 3.347(7) . . no O(4) C(6) 3.388(8) . 2 no O(5) H(44) 2.4359 . 1_655 no O(5) H(3) 2.4743 . . no O(5) H(12) 2.7939 . . no O(5) H(36) 2.9283 . 1_655 no O(5) H(54) 2.9570 . . no O(5) C(24) 3.360(9) . 1_655 no O(5) C(3) 3.406(8) . . no O(5) C(11) 3.413(8) . . no O(6) H(54) 1.3806 . . no O(6) O(8) 2.474(7) . . no O(6) H(48) 2.7771 . . no O(6) H(38) 2.8073 . 2 no O(6) H(31) 2.8101 . 2 no O(6) H(27) 2.9082 . 1_554 no O(6) H(30) 2.9766 . 2 no O(6) C(19) 3.278(8) . 2 no O(6) C(27) 3.372(10) . . no O(6) O(7) 3.445(7) . . no O(7) H(45) 2.4342 . 2_565 no O(7) H(51) 2.5144 . . no O(7) C(26) 3.276(10) . . no O(7) C(25) 3.313(8) . 2_565 no O(8) H(4) 2.8023 . 2_655 no O(9) H(5) 2.4196 . 2_655 no O(9) H(35) 2.7891 . 1_654 no O(9) H(41) 2.9036 . 1_654 no O(9) H(30) 3.0131 . 1_654 no O(9) C(5) 3.295(8) . 2_655 no O(9) C(20) 3.482(9) . 1_654 no C(1) C(6) 3.539(8) . 2 no C(3) C(8) 3.565(8) . 2 no C(4) H(8) 2.8417 . 2 no C(4) H(50) 2.9605 . 1_556 no C(4) C(27) 3.43(1) . 1_556 no C(4) C(8) 3.587(8) . 2 no C(5) H(1) 2.8742 . 2 no C(6) H(1) 3.0388 . 2 no C(25) H(19) 2.9590 . 2_465 no C(26) H(24) 3.0342 . 2_565 no H(5) H(20) 2.6333 . 2 no H(6) H(32) 2.5576 . 2_556 no H(13) H(53) 2.4488 . . no H(16) H(52) 2.6512 . 2_565 no H(19) H(45) 2.5419 . 2_465 no H(24) H(51) 2.6009 . 2_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd(1) P(1) C(1) C(2) . . . . -58.8(5) no Pd(1) P(1) C(9) C(10) . . . . 49.5(4) no Pd(1) P(1) C(9) C(11) . . . . 168.1(4) no Pd(1) P(1) C(9) C(12) . . . . -69.8(4) no Pd(1) P(1) C(13) C(14) . . . . -82.1(4) no Pd(1) P(1) C(13) C(15) . . . . 159.0(4) no Pd(1) P(1) C(13) C(16) . . . . 36.7(5) no Pd(1) P(2) C(8) C(7) . . . . 58.8(5) no Pd(1) P(2) C(17) C(18) . . . . -66.4(4) no Pd(1) P(2) C(17) C(19) . . . . 173.8(4) no Pd(1) P(2) C(17) C(20) . . . . 51.1(5) no Pd(1) P(2) C(21) C(22) . . . . 163.0(4) no Pd(1) P(2) C(21) C(23) . . . . -73.5(4) no Pd(1) P(2) C(21) C(24) . . . . 45.1(5) no Pd(1) O(1) S(1) O(2) . . . . 7.0(2) no Pd(1) O(1) S(1) O(3) . . . . 133.1(3) no Pd(1) O(1) S(1) C(25) . . . . -106.7(3) no Pd(1) O(2) S(1) O(1) . . . . -7.0(2) no Pd(1) O(2) S(1) O(3) . . . . -133.4(2) no Pd(1) O(2) S(1) C(25) . . . . 107.2(3) no S(1) Pd(1) P(1) C(1) . . . . -174.5(2) no S(1) Pd(1) P(1) C(9) . . . . 63.1(2) no S(1) Pd(1) P(1) C(13) . . . . -58.1(2) no S(1) Pd(1) P(2) C(8) . . . . 174.0(2) no S(1) Pd(1) P(2) C(17) . . . . -64.0(2) no S(1) Pd(1) P(2) C(21) . . . . 58.5(2) no S(1) O(1) Pd(1) P(1) . . . . 170.0(2) no S(1) O(1) Pd(1) P(2) . . . . -19.1(5) no S(1) O(1) Pd(1) O(2) . . . . -5.1(2) no S(1) O(2) Pd(1) P(1) . . . . -11.9(5) no S(1) O(2) Pd(1) P(2) . . . . -179.5(2) no S(1) O(2) Pd(1) O(1) . . . . 5.1(2) no P(1) Pd(1) S(1) O(1) . . . . -13.0(2) no P(1) Pd(1) S(1) O(2) . . . . 175.5(2) no P(1) Pd(1) S(1) O(3) . . . . -99.5(3) no P(1) Pd(1) S(1) C(25) . . . . 81.9(3) no P(1) Pd(1) P(2) C(8) . . . . -2.0(2) no P(1) Pd(1) P(2) C(17) . . . . 120.0(2) no P(1) Pd(1) P(2) C(21) . . . . -117.5(2) no P(1) C(1) C(2) C(3) . . . . -107.7(6) no P(1) C(1) C(2) C(7) . . . . 80.6(6) no P(2) Pd(1) S(1) O(1) . . . . 172.2(2) no P(2) Pd(1) S(1) O(2) . . . . 0.7(2) no P(2) Pd(1) S(1) O(3) . . . . 85.7(3) no P(2) Pd(1) S(1) C(25) . . . . -93.0(3) no P(2) Pd(1) P(1) C(1) . . . . 1.4(2) no P(2) Pd(1) P(1) C(9) . . . . -121.0(2) no P(2) Pd(1) P(1) C(13) . . . . 117.8(2) no P(2) C(8) C(7) C(2) . . . . -77.8(7) no P(2) C(8) C(7) C(6) . . . . 107.0(6) no O(1) Pd(1) S(1) O(2) . . . . -171.5(3) no O(1) Pd(1) S(1) O(3) . . . . -86.5(4) no O(1) Pd(1) S(1) C(25) . . . . 94.9(3) no O(1) Pd(1) P(1) C(1) . . . . 178.4(2) no O(1) Pd(1) P(1) C(9) . . . . 56.0(2) no O(1) Pd(1) P(1) C(13) . . . . -65.2(2) no O(1) Pd(1) P(2) C(8) . . . . -172.8(4) no O(1) Pd(1) P(2) C(17) . . . . -50.8(4) no O(1) Pd(1) P(2) C(21) . . . . 71.6(4) no O(1) S(1) Pd(1) O(2) . . . . 171.5(3) no O(2) Pd(1) S(1) O(3) . . . . 85.0(4) no O(2) Pd(1) S(1) C(25) . . . . -93.6(3) no O(2) Pd(1) P(1) C(1) . . . . -166.0(4) no O(2) Pd(1) P(1) C(9) . . . . 71.6(4) no O(2) Pd(1) P(1) C(13) . . . . -49.6(4) no O(2) Pd(1) P(2) C(8) . . . . 174.4(2) no O(2) Pd(1) P(2) C(17) . . . . -63.6(2) no O(2) Pd(1) P(2) C(21) . . . . 58.8(2) no C(1) P(1) C(9) C(10) . . . . -82.2(4) no C(1) P(1) C(9) C(11) . . . . 36.4(5) no C(1) P(1) C(9) C(12) . . . . 158.5(4) no C(1) P(1) C(13) C(14) . . . . 47.0(5) no C(1) P(1) C(13) C(15) . . . . -71.8(5) no C(1) P(1) C(13) C(16) . . . . 165.8(4) no C(1) C(2) C(3) C(4) . . . . -174.3(5) no C(1) C(2) C(7) C(6) . . . . 172.4(5) no C(1) C(2) C(7) C(8) . . . . -2.7(8) no C(2) C(1) P(1) C(9) . . . . 63.7(5) no C(2) C(1) P(1) C(13) . . . . -178.3(5) no C(2) C(3) C(4) C(5) . . . . 1.5(10) no C(2) C(7) C(6) C(5) . . . . 2.1(9) no C(3) C(2) C(7) C(6) . . . . 0.5(8) no C(3) C(2) C(7) C(8) . . . . -174.6(5) no C(3) C(4) C(5) C(6) . . . . 1.2(9) no C(4) C(3) C(2) C(7) . . . . -2.4(9) no C(4) C(5) C(6) C(7) . . . . -3.0(9) no C(5) C(6) C(7) C(8) . . . . 177.4(5) no C(7) C(8) P(2) C(17) . . . . -63.5(5) no C(7) C(8) P(2) C(21) . . . . 176.9(4) no C(8) P(2) C(17) C(18) . . . . 64.5(4) no C(8) P(2) C(17) C(19) . . . . -55.3(5) no C(8) P(2) C(17) C(20) . . . . -178.0(4) no C(8) P(2) C(21) C(22) . . . . 35.0(5) no C(8) P(2) C(21) C(23) . . . . 158.5(4) no C(8) P(2) C(21) C(24) . . . . -82.9(5) no C(9) P(1) C(13) C(14) . . . . 160.5(4) no C(9) P(1) C(13) C(15) . . . . 41.7(5) no C(9) P(1) C(13) C(16) . . . . -80.6(5) no C(10) C(9) P(1) C(13) . . . . 167.4(4) no C(11) C(9) P(1) C(13) . . . . -74.0(5) no C(12) C(9) P(1) C(13) . . . . 48.1(5) no C(17) P(2) C(21) C(22) . . . . -79.1(5) no C(17) P(2) C(21) C(23) . . . . 44.4(5) no C(17) P(2) C(21) C(24) . . . . 163.0(4) no C(18) C(17) P(2) C(21) . . . . 175.7(4) no C(19) C(17) P(2) C(21) . . . . 55.9(5) no C(20) C(17) P(2) C(21) . . . . -66.7(5) no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'O(8)' 'H(54)' 'O(6)' '1.10' '1.38' '2.474(7)' '170.5' '.' data_zac2 _database_code_CSD 162524 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Heaton, B.' 'Clegg, William' 'Eastham, Graham R.' 'Elsegood, Mark R. J.' 'Iggo, J.' 'Tooze, R. P.' 'Whyman, R.' 'Zacchini, Stefano' _publ_contact_author_name 'Prof B Heaton' _publ_contact_author_address ; Department of Chemistry University of Liverpool P O Box 147 LIVERPOOL L69 3BX U.K. ; _publ_contact_author_email 'BTH@LIV.AC.UK' _publ_section_title ; Synthesis and Reactivity of Palladium hydrido-solvento complexes: including a Key intermediate in the Catalytic Methoxycarbonylation of Ethene to Methyl Propanoate ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H90 O9 P2 Pd S2' _chemical_formula_weight 1175.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -1.1770 1.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1100 0.1240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.422(3) _cell_length_b 15.236(3) _cell_length_c 15.695(3) _cell_angle_alpha 72.45(3) _cell_angle_beta 85.34(3) _cell_angle_gamma 65.79(2) _cell_volume 2995.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.423 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15324 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 22.39 _reflns_number_total 7168 _reflns_number_gt 5845 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0984P)^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 7168 _refine_ls_number_parameters 672 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.976 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.99557(3) 0.72817(2) 0.27987(2) 0.02220(16) Uani 1 d . . . P1 P 0.94347(10) 0.73897(9) 0.13744(8) 0.0261(3) Uani 1 d . . . P2 P 1.01590(9) 0.87677(9) 0.24963(8) 0.0241(3) Uani 1 d . . . S1 S 0.83732(10) 0.73388(10) 0.63136(8) 0.0356(3) Uani 1 d . . . S2 S 1.07560(15) 0.73787(13) 0.78579(12) 0.0619(5) Uani 1 d . . . C1 C 1.1468(4) 0.6576(4) 0.0976(4) 0.0401(13) Uani 1 d . . . H1A H 1.1376 0.7251 0.0620 0.048 Uiso 1 calc R . . H1B H 1.1633 0.6496 0.1589 0.048 Uiso 1 calc R . . C2 C 1.2352(5) 0.5807(5) 0.0626(4) 0.0553(16) Uani 1 d . . . H2A H 1.2217 0.5924 -0.0003 0.066 Uiso 1 calc R . . H2B H 1.2974 0.5889 0.0684 0.066 Uiso 1 calc R . . C3 C 1.2486(4) 0.4746(4) 0.1146(4) 0.0527(15) Uani 1 d . . . H3A H 1.2682 0.4608 0.1765 0.063 Uiso 1 calc R . . H3B H 1.3024 0.4269 0.0898 0.063 Uiso 1 calc R . . C4 C 1.1505(4) 0.4618(4) 0.1103(4) 0.0502(15) Uani 1 d . . . H4A H 1.1346 0.4696 0.0489 0.060 Uiso 1 calc R . . H4B H 1.1598 0.3943 0.1459 0.060 Uiso 1 calc R . . C5 C 1.0624(4) 0.5373(4) 0.1443(4) 0.0411(13) Uani 1 d . . . H5A H 1.0751 0.5251 0.2074 0.049 Uiso 1 calc R . . H5B H 1.0008 0.5283 0.1377 0.049 Uiso 1 calc R . . C6 C 1.0468(4) 0.6448(4) 0.0938(3) 0.0324(12) Uani 1 d . . . H6 H 1.0290 0.6574 0.0310 0.039 Uiso 1 calc R . . C7 C 0.8004(4) 0.6978(5) 0.0548(4) 0.0444(14) Uani 1 d . . . H7A H 0.7795 0.7618 0.0081 0.053 Uiso 1 calc R . . H7B H 0.8585 0.6489 0.0349 0.053 Uiso 1 calc R . . C8 C 0.7133(4) 0.6635(5) 0.0712(4) 0.0526(16) Uani 1 d . . . H8A H 0.6929 0.6596 0.0155 0.063 Uiso 1 calc R . . H8B H 0.7369 0.5965 0.1135 0.063 Uiso 1 calc R . . C9 C 0.6220(4) 0.7340(5) 0.1072(4) 0.0490(15) Uani 1 d . . . H9A H 0.5704 0.7070 0.1205 0.059 Uiso 1 calc R . . H9B H 0.5932 0.7990 0.0623 0.059 Uiso 1 calc R . . C10 C 0.6525(4) 0.7471(5) 0.1917(4) 0.0434(14) Uani 1 d . . . H10A H 0.5940 0.7955 0.2118 0.052 Uiso 1 calc R . . H10B H 0.6746 0.6833 0.2387 0.052 Uiso 1 calc R . . C11 C 0.7377(4) 0.7833(4) 0.1749(3) 0.0345(12) Uani 1 d . . . H11A H 0.7566 0.7900 0.2298 0.041 Uiso 1 calc R . . H11B H 0.7143 0.8490 0.1305 0.041 Uiso 1 calc R . . C12 C 0.8307(4) 0.7093(4) 0.1417(3) 0.0292(11) Uani 1 d . . . H12 H 0.8482 0.6437 0.1868 0.035 Uiso 1 calc R . . C13 C 0.9195(4) 0.8506(4) 0.0392(3) 0.0333(12) Uani 1 d . . . H13A H 0.9852 0.8497 0.0192 0.040 Uiso 1 calc R . . H13B H 0.8882 0.8415 -0.0081 0.040 Uiso 1 calc R . . C14 C 0.8554(4) 0.9542(3) 0.0464(3) 0.0288(11) Uani 1 d . . . C15 C 0.7569(4) 1.0059(4) 0.0063(3) 0.0400(13) Uani 1 d . . . H15 H 0.7306 0.9731 -0.0198 0.048 Uiso 1 calc R . . C16 C 0.6983(4) 1.1040(4) 0.0047(4) 0.0430(14) Uani 1 d . . . H16 H 0.6332 1.1374 -0.0225 0.052 Uiso 1 calc R . . C17 C 0.7377(4) 1.1525(4) 0.0442(4) 0.0458(14) Uani 1 d . . . H17 H 0.6988 1.2187 0.0436 0.055 Uiso 1 calc R . . C18 C 0.8334(4) 1.1030(4) 0.0839(3) 0.0393(13) Uani 1 d . . . H18 H 0.8591 1.1367 0.1094 0.047 Uiso 1 calc R . . C19 C 0.8935(4) 1.0031(4) 0.0873(3) 0.0300(11) Uani 1 d . . . C20 C 0.9994(4) 0.9536(4) 0.1307(3) 0.0334(12) Uani 1 d . . . H20A H 1.0230 1.0060 0.1260 0.040 Uiso 1 calc R . . H20B H 1.0438 0.9108 0.0963 0.040 Uiso 1 calc R . . C21 C 0.8161(3) 0.9726(4) 0.2983(3) 0.0304(11) Uani 1 d . . . H21A H 0.7970 0.9877 0.2360 0.036 Uiso 1 calc R . . H21B H 0.8128 0.9089 0.3310 0.036 Uiso 1 calc R . . C22 C 0.7419(4) 1.0558(4) 0.3361(4) 0.0409(13) Uani 1 d . . . H22A H 0.7415 1.1201 0.3002 0.049 Uiso 1 calc R . . H22B H 0.6738 1.0589 0.3324 0.049 Uiso 1 calc R . . C23 C 0.7701(4) 1.0380(4) 0.4317(4) 0.0418(13) Uani 1 d . . . H23A H 0.7581 0.9805 0.4692 0.050 Uiso 1 calc R . . H23B H 0.7267 1.0963 0.4505 0.050 Uiso 1 calc R . . C24 C 0.8813(4) 1.0187(4) 0.4454(4) 0.0435(14) Uani 1 d . . . H24A H 0.8905 1.0805 0.4174 0.052 Uiso 1 calc R . . H24B H 0.8980 0.9989 0.5089 0.052 Uiso 1 calc R . . C25 C 0.9532(4) 0.9368(4) 0.4062(3) 0.0302(11) Uani 1 d . . . H25A H 0.9491 0.8733 0.4381 0.036 Uiso 1 calc R . . H25B H 1.0226 0.9291 0.4133 0.036 Uiso 1 calc R . . C26 C 0.9252(3) 0.9640(3) 0.3061(3) 0.0244(10) Uani 1 d . . . H26 H 0.9246 1.0308 0.2768 0.029 Uiso 1 calc R . . C27 C 1.1442(3) 0.8625(4) 0.2803(3) 0.0278(11) Uani 1 d . . . H27 H 1.1577 0.8241 0.3439 0.033 Uiso 1 calc R . . C28 C 1.2271(4) 0.8000(4) 0.2303(3) 0.0359(12) Uani 1 d . . . H28A H 1.2160 0.8346 0.1666 0.043 Uiso 1 calc R . . H28B H 1.2231 0.7356 0.2403 0.043 Uiso 1 calc R . . C29 C 1.3327(4) 0.7821(4) 0.2607(4) 0.0446(14) Uani 1 d . . . H29A H 1.3827 0.7483 0.2232 0.054 Uiso 1 calc R . . H29B H 1.3480 0.7382 0.3217 0.054 Uiso 1 calc R . . C30 C 1.3415(4) 0.8801(5) 0.2562(4) 0.0467(15) Uani 1 d . . . H30A H 1.4072 0.8646 0.2821 0.056 Uiso 1 calc R . . H30B H 1.3371 0.9197 0.1942 0.056 Uiso 1 calc R . . C31 C 1.2581(4) 0.9404(4) 0.3060(4) 0.0436(14) Uani 1 d . . . H31A H 1.2637 1.0033 0.3000 0.052 Uiso 1 calc R . . H31B H 1.2666 0.9032 0.3691 0.052 Uiso 1 calc R . . C32 C 1.1530(4) 0.9631(4) 0.2711(4) 0.0349(12) Uani 1 d . . . H32A H 1.1423 1.0033 0.2089 0.042 Uiso 1 calc R . . H32B H 1.1013 1.0010 0.3051 0.042 Uiso 1 calc R . . C33 C 1.0481(4) 0.6604(4) 0.4187(3) 0.0269(11) Uani 1 d . . . H33 H 0.998(3) 0.701(3) 0.448(3) 0.016(12) Uiso 1 d . . . C34 C 1.1514(4) 0.6413(4) 0.4487(3) 0.0312(12) Uani 1 d . . . C35 C 1.1607(4) 0.6785(4) 0.5180(4) 0.0414(13) Uani 1 d . . . H35 H 1.1026 0.7165 0.5422 0.050 Uiso 1 calc R . . C36 C 1.2560(6) 0.6589(5) 0.5503(4) 0.063(2) Uani 1 d . . . H36 H 1.2616 0.6836 0.5962 0.076 Uiso 1 calc R . . C37 C 1.3428(5) 0.6027(5) 0.5146(5) 0.067(2) Uani 1 d . . . H37 H 1.4066 0.5898 0.5364 0.080 Uiso 1 calc R . . C38 C 1.3351(5) 0.5659(5) 0.4471(5) 0.0569(17) Uani 1 d . . . H38 H 1.3934 0.5279 0.4232 0.068 Uiso 1 calc R . . C39 C 1.2393(4) 0.5860(4) 0.4148(4) 0.0398(13) Uani 1 d . . . H39 H 1.2346 0.5611 0.3687 0.048 Uiso 1 calc R . . C40 C 1.0326(4) 0.5866(4) 0.3904(3) 0.0271(11) Uani 1 d . . . H40 H 1.090(3) 0.530(3) 0.387(3) 0.012(10) Uiso 1 d . . . C41 C 0.9359(4) 0.5889(4) 0.3787(3) 0.0298(11) Uani 1 d . . . C42 C 0.8422(4) 0.6620(4) 0.4001(3) 0.0280(11) Uani 1 d . . . H42 H 0.848(4) 0.719(4) 0.409(3) 0.038(14) Uiso 1 d . . . C43 C 0.7521(4) 0.6548(4) 0.4066(3) 0.0303(11) Uani 1 d . . . H43 H 0.7499 0.5973 0.3992 0.036 Uiso 1 calc R . . C44 C 0.6570(4) 0.7311(4) 0.4245(3) 0.0291(11) Uani 1 d . . . C45 C 0.6458(4) 0.8285(4) 0.4155(3) 0.0369(13) Uani 1 d . . . H45 H 0.6999 0.8465 0.3958 0.044 Uiso 1 calc R . . C46 C 0.5571(4) 0.8991(4) 0.4347(4) 0.0412(13) Uani 1 d . . . H46 H 0.5516 0.9638 0.4281 0.049 Uiso 1 calc R . . C47 C 0.4763(4) 0.8735(5) 0.4637(4) 0.0473(15) Uani 1 d . . . H47 H 0.4166 0.9204 0.4781 0.057 Uiso 1 calc R . . C48 C 0.4842(5) 0.7790(5) 0.4713(5) 0.0584(17) Uani 1 d . . . H48 H 0.4294 0.7620 0.4902 0.070 Uiso 1 calc R . . C49 C 0.5729(4) 0.7089(4) 0.4513(4) 0.0450(14) Uani 1 d . . . H49 H 0.5766 0.6453 0.4556 0.054 Uiso 1 calc R . . C50 C 1.0982(7) 0.6171(5) 0.7931(6) 0.087(3) Uani 1 d . . . H50A H 1.1352 0.5728 0.8484 0.104 Uiso 1 calc R . . H50B H 1.1376 0.5989 0.7439 0.104 Uiso 1 calc R . . H50C H 1.0347 0.6113 0.7909 0.104 Uiso 1 calc R . . C60 C 0.7126(5) 0.7414(7) 0.6433(4) 0.074(2) Uani 1 d . . . H60A H 0.7039 0.7103 0.7047 0.089 Uiso 1 calc R . . H60B H 0.7002 0.7071 0.6061 0.089 Uiso 1 calc R . . H60C H 0.6654 0.8108 0.6257 0.089 Uiso 1 calc R . . O1 O 0.9246(3) 0.5166(3) 0.3535(2) 0.0372(8) Uani 1 d . . . H1 H 0.9774 0.4654 0.3658 0.056 Uiso 1 calc R . . O2 O 0.8477(4) 0.7859(4) 0.6925(3) 0.0648(12) Uani 1 d . . . O3 O 0.9019(4) 0.6288(3) 0.6627(3) 0.0672(13) Uani 1 d . . . O4 O 0.8478(3) 0.7804(3) 0.5401(2) 0.0507(10) Uani 1 d . . . O5 O 1.0163(4) 0.8000(3) 0.6968(3) 0.0629(12) Uani 1 d . . . O6 O 1.0231(6) 0.7698(6) 0.8543(4) 0.117(2) Uani 1 d . . . H6A H 0.9756 0.7523 0.8644 0.175 Uiso 1 calc R . . O7 O 1.1742(4) 0.7455(5) 0.7754(5) 0.110(2) Uani 1 d . . . O50 O 1.3838(4) 0.0910(4) 0.1031(3) 0.0709(13) Uani 1 d DU . . C51 C 1.3665(5) 0.1482(6) 0.1623(5) 0.072(2) Uani 1 d DU . . H51A H 1.3166 0.1370 0.2045 0.087 Uiso 1 calc R . . H51B H 1.3404 0.2193 0.1295 0.087 Uiso 1 calc R . . C52 C 1.4603(8) 0.1185(11) 0.2087(10) 0.176(6) Uani 1 d DU . . H52A H 1.4812 0.1741 0.1924 0.211 Uiso 1 calc R . . H52B H 1.4515 0.1011 0.2727 0.211 Uiso 1 calc R . . C53 C 1.5366(5) 0.0345(6) 0.1870(5) 0.077(2) Uani 1 d DU . . H53A H 1.5551 -0.0259 0.2377 0.093 Uiso 1 calc R . . H53B H 1.5971 0.0466 0.1679 0.093 Uiso 1 calc R . . C54 C 1.4864(5) 0.0253(5) 0.1114(4) 0.0631(18) Uani 1 d DU . . H54A H 1.5191 0.0421 0.0561 0.076 Uiso 1 calc R . . H54B H 1.4928 -0.0434 0.1238 0.076 Uiso 1 calc R . . O60 O 1.4993(10) 0.5688(9) 0.7041(8) 0.200(4) Uani 1 d DU . . C61 C 1.4675(11) 0.6508(9) 0.7337(9) 0.148(5) Uani 1 d DU . . H61A H 1.4076 0.7037 0.6983 0.178 Uiso 1 calc R . . H61B H 1.5205 0.6757 0.7271 0.178 Uiso 1 calc R . . C62 C 1.4433(10) 0.6241(12) 0.8279(9) 0.154(5) Uani 1 d DU . . H62A H 1.4959 0.6192 0.8661 0.184 Uiso 1 calc R . . H62B H 1.3786 0.6739 0.8382 0.184 Uiso 1 calc R . . C63 C 1.4385(14) 0.5268(13) 0.8448(11) 0.189(6) Uani 1 d DU . . H63A H 1.4769 0.4798 0.8996 0.227 Uiso 1 calc R . . H63B H 1.3686 0.5335 0.8497 0.227 Uiso 1 calc R . . C64 C 1.4827(17) 0.4933(11) 0.7686(11) 0.213(7) Uani 1 d DU . . H64A H 1.5466 0.4349 0.7872 0.255 Uiso 1 calc R . . H64B H 1.4373 0.4735 0.7440 0.255 Uiso 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 0.0309(2) 0.0204(2) 0.0182(2) -0.00804(16) 0.00414(15) -0.01195(17) P1 0.0391(7) 0.0223(7) 0.0198(6) -0.0093(5) 0.0037(5) -0.0134(6) P2 0.0311(7) 0.0248(7) 0.0213(6) -0.0086(5) 0.0055(5) -0.0154(6) S1 0.0412(7) 0.0328(7) 0.0312(7) -0.0147(6) 0.0056(6) -0.0105(6) S2 0.0903(13) 0.0481(10) 0.0553(10) -0.0206(8) -0.0141(10) -0.0290(9) C1 0.045(3) 0.034(3) 0.047(3) -0.020(3) 0.010(3) -0.018(3) C2 0.051(4) 0.061(4) 0.057(4) -0.027(4) 0.019(3) -0.022(3) C3 0.048(3) 0.043(4) 0.061(4) -0.026(3) 0.002(3) -0.005(3) C4 0.055(4) 0.034(3) 0.058(4) -0.017(3) 0.004(3) -0.013(3) C5 0.059(3) 0.025(3) 0.040(3) -0.018(3) 0.012(3) -0.013(3) C6 0.042(3) 0.031(3) 0.025(3) -0.011(2) 0.003(2) -0.014(2) C7 0.050(3) 0.053(4) 0.041(3) -0.028(3) 0.003(3) -0.021(3) C8 0.053(4) 0.058(4) 0.060(4) -0.027(3) -0.006(3) -0.027(3) C9 0.046(3) 0.055(4) 0.049(3) -0.013(3) -0.007(3) -0.024(3) C10 0.036(3) 0.050(3) 0.040(3) -0.012(3) 0.003(3) -0.014(3) C11 0.044(3) 0.028(3) 0.027(3) -0.009(2) 0.001(2) -0.008(2) C12 0.038(3) 0.027(3) 0.024(2) -0.012(2) 0.002(2) -0.012(2) C13 0.055(3) 0.031(3) 0.015(2) -0.004(2) 0.000(2) -0.020(3) C14 0.046(3) 0.022(3) 0.016(2) 0.000(2) 0.006(2) -0.016(2) C15 0.054(3) 0.039(3) 0.028(3) -0.004(3) -0.002(3) -0.024(3) C16 0.039(3) 0.036(3) 0.035(3) 0.009(3) -0.007(2) -0.010(3) C17 0.057(4) 0.025(3) 0.041(3) -0.004(3) 0.008(3) -0.007(3) C18 0.065(4) 0.030(3) 0.025(3) -0.007(2) 0.003(3) -0.023(3) C19 0.045(3) 0.027(3) 0.018(2) -0.006(2) 0.006(2) -0.016(2) C20 0.045(3) 0.035(3) 0.022(3) -0.005(2) 0.008(2) -0.022(3) C21 0.029(3) 0.035(3) 0.031(3) -0.010(2) 0.003(2) -0.017(2) C22 0.028(3) 0.035(3) 0.056(4) -0.015(3) 0.007(3) -0.009(2) C23 0.040(3) 0.039(3) 0.048(3) -0.023(3) 0.017(3) -0.014(3) C24 0.049(3) 0.051(4) 0.046(3) -0.034(3) 0.018(3) -0.024(3) C25 0.031(3) 0.038(3) 0.029(3) -0.019(2) 0.007(2) -0.016(2) C26 0.034(3) 0.021(2) 0.024(2) -0.010(2) 0.009(2) -0.016(2) C27 0.031(3) 0.027(3) 0.030(3) -0.008(2) 0.005(2) -0.018(2) C28 0.043(3) 0.034(3) 0.034(3) -0.013(2) 0.008(2) -0.017(2) C29 0.031(3) 0.048(3) 0.051(3) -0.018(3) 0.015(3) -0.012(3) C30 0.033(3) 0.060(4) 0.050(3) -0.011(3) 0.003(3) -0.025(3) C31 0.041(3) 0.045(3) 0.053(3) -0.017(3) 0.003(3) -0.024(3) C32 0.035(3) 0.033(3) 0.046(3) -0.015(3) 0.006(2) -0.021(2) C33 0.033(3) 0.025(3) 0.024(2) -0.008(2) 0.006(2) -0.013(2) C34 0.037(3) 0.024(3) 0.029(3) -0.001(2) 0.004(2) -0.015(2) C35 0.044(3) 0.044(3) 0.039(3) -0.009(3) -0.007(3) -0.021(3) C36 0.073(5) 0.070(5) 0.052(4) 0.001(4) -0.026(4) -0.042(4) C37 0.045(4) 0.057(4) 0.083(5) 0.012(4) -0.018(4) -0.025(3) C38 0.040(3) 0.044(4) 0.071(4) 0.001(3) 0.003(3) -0.014(3) C39 0.036(3) 0.029(3) 0.047(3) -0.001(3) 0.001(3) -0.014(2) C40 0.031(3) 0.023(3) 0.024(3) -0.010(2) 0.008(2) -0.008(2) C41 0.044(3) 0.023(3) 0.024(2) -0.007(2) 0.006(2) -0.016(2) C42 0.034(3) 0.031(3) 0.023(2) -0.004(2) 0.005(2) -0.020(2) C43 0.039(3) 0.030(3) 0.022(2) -0.003(2) 0.002(2) -0.019(2) C44 0.031(3) 0.038(3) 0.021(2) -0.008(2) 0.000(2) -0.018(2) C45 0.038(3) 0.037(3) 0.039(3) -0.009(3) 0.008(2) -0.022(3) C46 0.039(3) 0.041(3) 0.046(3) -0.017(3) 0.003(3) -0.016(3) C47 0.027(3) 0.056(4) 0.057(4) -0.020(3) 0.009(3) -0.014(3) C48 0.042(3) 0.060(4) 0.081(5) -0.019(4) 0.013(3) -0.032(3) C49 0.037(3) 0.039(3) 0.060(4) -0.011(3) 0.005(3) -0.019(3) C50 0.114(6) 0.042(4) 0.100(6) 0.002(4) -0.047(5) -0.033(4) C60 0.057(4) 0.118(7) 0.037(3) -0.011(4) 0.008(3) -0.034(4) O1 0.047(2) 0.0297(19) 0.043(2) -0.0158(18) 0.0043(18) -0.0194(17) O2 0.080(3) 0.067(3) 0.060(3) -0.045(3) 0.016(2) -0.026(3) O3 0.078(3) 0.035(2) 0.063(3) -0.011(2) 0.012(2) -0.002(2) O4 0.061(2) 0.057(3) 0.038(2) -0.015(2) 0.0146(19) -0.029(2) O5 0.091(3) 0.042(2) 0.053(3) -0.007(2) -0.005(2) -0.028(2) O6 0.150(7) 0.122(6) 0.065(4) -0.038(4) 0.017(4) -0.037(5) O7 0.093(4) 0.098(4) 0.161(6) -0.025(4) -0.025(4) -0.064(4) O50 0.074(3) 0.069(3) 0.061(3) -0.022(3) -0.009(2) -0.017(3) C51 0.068(5) 0.070(5) 0.073(5) -0.033(4) -0.002(4) -0.013(4) C52 0.120(8) 0.195(12) 0.213(12) -0.168(11) -0.063(9) 0.025(8) C53 0.067(4) 0.095(6) 0.061(4) -0.039(4) 0.004(4) -0.013(4) C54 0.057(4) 0.059(4) 0.060(4) -0.012(4) -0.001(3) -0.013(3) O60 0.280(12) 0.138(8) 0.179(10) -0.070(8) 0.044(9) -0.070(9) C61 0.164(11) 0.129(10) 0.174(12) -0.084(10) 0.016(10) -0.054(9) C62 0.128(9) 0.181(13) 0.159(12) -0.102(11) 0.024(9) -0.037(9) C63 0.190(14) 0.184(15) 0.199(15) -0.055(13) 0.046(12) -0.090(12) C64 0.36(2) 0.109(10) 0.160(13) -0.039(10) 0.033(15) -0.094(13) _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 C33 2.158(5) . ? Pd1 C40 2.213(5) . ? Pd1 P2 2.3046(13) . ? Pd1 P1 2.3535(13) . ? P1 C13 1.847(5) . ? P1 C12 1.849(5) . ? P1 C6 1.850(5) . ? P2 C26 1.833(5) . ? P2 C20 1.854(5) . ? P2 C27 1.859(5) . ? S1 O4 1.420(4) . ? S1 O3 1.432(4) . ? S1 O2 1.467(4) . ? S1 C60 1.753(6) . ? S2 O6 1.360(6) . ? S2 O7 1.465(6) . ? S2 O5 1.521(5) . ? S2 C50 1.701(7) . ? C1 C2 1.533(8) . ? C1 C6 1.541(7) . ? C2 C3 1.513(9) . ? C3 C4 1.514(8) . ? C4 C5 1.510(8) . ? C5 C6 1.519(7) . ? C7 C8 1.524(8) . ? C7 C12 1.546(7) . ? C8 C9 1.515(9) . ? C9 C10 1.522(8) . ? C10 C11 1.516(7) . ? C11 C12 1.529(7) . ? C13 C14 1.502(7) . ? C14 C19 1.396(7) . ? C14 C15 1.401(7) . ? C15 C16 1.376(8) . ? C16 C17 1.390(8) . ? C17 C18 1.365(8) . ? C18 C19 1.396(7) . ? C19 C20 1.512(7) . ? C21 C22 1.530(8) . ? C21 C26 1.536(6) . ? C22 C23 1.501(8) . ? C23 C24 1.528(8) . ? C24 C25 1.519(7) . ? C25 C26 1.541(7) . ? C27 C28 1.522(7) . ? C27 C32 1.552(7) . ? C28 C29 1.524(7) . ? C29 C30 1.529(8) . ? C30 C31 1.509(8) . ? C31 C32 1.520(7) . ? C33 C40 1.426(7) . ? C33 C34 1.484(7) . ? C34 C39 1.373(7) . ? C34 C35 1.407(7) . ? C35 C36 1.387(8) . ? C36 C37 1.382(10) . ? C37 C38 1.369(10) . ? C38 C39 1.392(8) . ? C40 C41 1.406(7) . ? C41 O1 1.348(6) . ? C41 C42 1.448(7) . ? C42 C43 1.342(7) . ? C43 C44 1.462(7) . ? C44 C45 1.388(7) . ? C44 C49 1.390(7) . ? C45 C46 1.374(8) . ? C46 C47 1.377(8) . ? C47 C48 1.364(9) . ? C48 C49 1.376(8) . ? O50 C54 1.395(7) . ? O50 C51 1.399(7) . ? C51 C52 1.424(10) . ? C52 C53 1.419(11) . ? C53 C54 1.508(9) . ? O60 C61 1.353(11) . ? O60 C64 1.375(12) . ? C61 C62 1.464(13) . ? C62 C63 1.456(15) . ? C63 C64 1.440(13) . ? 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 C33 Pd1 C40 38.07(18) . . ? C33 Pd1 P2 100.58(13) . . ? C40 Pd1 P2 138.18(13) . . ? C33 Pd1 P1 157.93(14) . . ? C40 Pd1 P1 119.90(13) . . ? P2 Pd1 P1 101.04(5) . . ? C13 P1 C12 105.8(2) . . ? C13 P1 C6 98.5(2) . . ? C12 P1 C6 106.6(2) . . ? C13 P1 Pd1 123.09(16) . . ? C12 P1 Pd1 111.94(15) . . ? C6 P1 Pd1 109.07(16) . . ? C26 P2 C20 103.6(2) . . ? C26 P2 C27 106.0(2) . . ? C20 P2 C27 101.4(2) . . ? C26 P2 Pd1 112.77(14) . . ? C20 P2 Pd1 116.56(17) . . ? C27 P2 Pd1 115.03(16) . . ? O4 S1 O3 114.2(3) . . ? O4 S1 O2 113.8(3) . . ? O3 S1 O2 110.0(3) . . ? O4 S1 C60 108.1(3) . . ? O3 S1 C60 105.5(4) . . ? O2 S1 C60 104.3(3) . . ? O6 S2 O7 113.7(5) . . ? O6 S2 O5 111.1(4) . . ? O7 S2 O5 106.0(3) . . ? O6 S2 C50 114.0(5) . . ? O7 S2 C50 106.9(4) . . ? O5 S2 C50 104.4(3) . . ? C2 C1 C6 111.7(4) . . ? C3 C2 C1 110.5(5) . . ? C2 C3 C4 110.4(5) . . ? C5 C4 C3 112.2(5) . . ? C4 C5 C6 111.7(4) . . ? C5 C6 C1 109.7(4) . . ? C5 C6 P1 112.8(3) . . ? C1 C6 P1 109.7(3) . . ? C8 C7 C12 110.0(5) . . ? C9 C8 C7 112.3(5) . . ? C8 C9 C10 110.7(5) . . ? C11 C10 C9 111.0(4) . . ? C10 C11 C12 110.8(4) . . ? C11 C12 C7 109.5(4) . . ? C11 C12 P1 112.5(3) . . ? C7 C12 P1 116.1(4) . . ? C14 C13 P1 120.3(3) . . ? C19 C14 C15 118.9(5) . . ? C19 C14 C13 121.7(5) . . ? C15 C14 C13 119.3(4) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C17 119.1(5) . . ? C18 C17 C16 120.1(5) . . ? C17 C18 C19 121.6(5) . . ? C18 C19 C14 118.8(5) . . ? C18 C19 C20 118.8(4) . . ? C14 C19 C20 122.4(5) . . ? C19 C20 P2 117.5(3) . . ? C22 C21 C26 110.2(4) . . ? C23 C22 C21 111.9(4) . . ? C22 C23 C24 112.6(4) . . ? C25 C24 C23 111.8(4) . . ? C24 C25 C26 110.4(4) . . ? C21 C26 C25 107.7(4) . . ? C21 C26 P2 112.6(3) . . ? C25 C26 P2 113.7(3) . . ? C28 C27 C32 110.8(4) . . ? C28 C27 P2 111.8(3) . . ? C32 C27 P2 114.5(3) . . ? C27 C28 C29 111.6(4) . . ? C28 C29 C30 112.4(5) . . ? C31 C30 C29 110.9(4) . . ? C30 C31 C32 112.0(5) . . ? C31 C32 C27 109.1(4) . . ? C40 C33 C34 120.0(5) . . ? C40 C33 Pd1 73.1(3) . . ? C34 C33 Pd1 121.9(3) . . ? C39 C34 C35 117.8(5) . . ? C39 C34 C33 123.6(5) . . ? C35 C34 C33 118.6(5) . . ? C36 C35 C34 120.4(6) . . ? C37 C36 C35 120.2(6) . . ? C38 C37 C36 120.2(6) . . ? C37 C38 C39 119.4(6) . . ? C34 C39 C38 122.1(6) . . ? C41 C40 C33 123.4(5) . . ? C41 C40 Pd1 90.6(3) . . ? C33 C40 Pd1 68.9(3) . . ? O1 C41 C40 121.6(5) . . ? O1 C41 C42 114.5(4) . . ? C40 C41 C42 123.7(4) . . ? C43 C42 C41 124.9(5) . . ? C42 C43 C44 124.5(5) . . ? C45 C44 C49 116.8(5) . . ? C45 C44 C43 122.3(4) . . ? C49 C44 C43 120.9(5) . . ? C46 C45 C44 122.0(5) . . ? C45 C46 C47 119.6(5) . . ? C48 C47 C46 119.8(6) . . ? C47 C48 C49 120.4(5) . . ? C48 C49 C44 121.4(5) . . ? C54 O50 C51 108.7(5) . . ? O50 C51 C52 108.4(6) . . ? C53 C52 C51 110.2(7) . . ? C52 C53 C54 103.2(6) . . ? O50 C54 C53 108.6(6) . . ? C61 O60 C64 108.5(11) . . ? O60 C61 C62 109.7(10) . . ? C63 C62 C61 104.5(10) . . ? C64 C63 C62 104.9(10) . . ? O60 C64 C63 110.4(11) . . ? 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 C33 Pd1 P1 C13 -172.8(4) . . . . ? C40 Pd1 P1 C13 -175.7(2) . . . . ? P2 Pd1 P1 C13 -4.5(2) . . . . ? C33 Pd1 P1 C12 59.4(4) . . . . ? C40 Pd1 P1 C12 56.5(2) . . . . ? P2 Pd1 P1 C12 -132.38(18) . . . . ? C33 Pd1 P1 C6 -58.4(4) . . . . ? C40 Pd1 P1 C6 -61.3(2) . . . . ? P2 Pd1 P1 C6 109.87(16) . . . . ? C33 Pd1 P2 C26 -69.8(2) . . . . ? C40 Pd1 P2 C26 -76.9(3) . . . . ? P1 Pd1 P2 C26 114.62(16) . . . . ? C33 Pd1 P2 C20 170.5(2) . . . . ? C40 Pd1 P2 C20 163.4(3) . . . . ? P1 Pd1 P2 C20 -5.07(19) . . . . ? C33 Pd1 P2 C27 51.9(2) . . . . ? C40 Pd1 P2 C27 44.9(3) . . . . ? P1 Pd1 P2 C27 -123.59(18) . . . . ? C6 C1 C2 C3 -56.7(6) . . . . ? C1 C2 C3 C4 56.3(7) . . . . ? C2 C3 C4 C5 -56.7(7) . . . . ? C3 C4 C5 C6 56.4(6) . . . . ? C4 C5 C6 C1 -54.6(6) . . . . ? C4 C5 C6 P1 -177.2(4) . . . . ? C2 C1 C6 C5 55.3(6) . . . . ? C2 C1 C6 P1 179.6(4) . . . . ? C13 P1 C6 C5 -160.9(4) . . . . ? C12 P1 C6 C5 -51.5(4) . . . . ? Pd1 P1 C6 C5 69.6(4) . . . . ? C13 P1 C6 C1 76.5(4) . . . . ? C12 P1 C6 C1 -174.1(3) . . . . ? Pd1 P1 C6 C1 -53.0(4) . . . . ? C12 C7 C8 C9 56.2(7) . . . . ? C7 C8 C9 C10 -55.3(7) . . . . ? C8 C9 C10 C11 55.8(6) . . . . ? C9 C10 C11 C12 -58.3(6) . . . . ? C10 C11 C12 C7 58.6(5) . . . . ? C10 C11 C12 P1 -170.8(3) . . . . ? C8 C7 C12 C11 -57.0(6) . . . . ? C8 C7 C12 P1 174.4(4) . . . . ? C13 P1 C12 C11 -74.5(4) . . . . ? C6 P1 C12 C11 -178.7(3) . . . . ? Pd1 P1 C12 C11 62.1(3) . . . . ? C13 P1 C12 C7 52.7(5) . . . . ? C6 P1 C12 C7 -51.5(4) . . . . ? Pd1 P1 C12 C7 -170.7(3) . . . . ? C12 P1 C13 C14 82.6(4) . . . . ? C6 P1 C13 C14 -167.3(4) . . . . ? Pd1 P1 C13 C14 -47.8(5) . . . . ? P1 C13 C14 C19 77.1(5) . . . . ? P1 C13 C14 C15 -106.9(5) . . . . ? C19 C14 C15 C16 1.4(7) . . . . ? C13 C14 C15 C16 -174.6(4) . . . . ? C14 C15 C16 C17 -0.3(8) . . . . ? C15 C16 C17 C18 0.1(8) . . . . ? C16 C17 C18 C19 -0.9(8) . . . . ? C17 C18 C19 C14 2.0(7) . . . . ? C17 C18 C19 C20 178.8(4) . . . . ? C15 C14 C19 C18 -2.2(7) . . . . ? C13 C14 C19 C18 173.7(4) . . . . ? C15 C14 C19 C20 -179.0(4) . . . . ? C13 C14 C19 C20 -3.0(7) . . . . ? C18 C19 C20 P2 95.8(5) . . . . ? C14 C19 C20 P2 -87.4(5) . . . . ? C26 P2 C20 C19 -55.6(4) . . . . ? C27 P2 C20 C19 -165.4(4) . . . . ? Pd1 P2 C20 C19 68.9(4) . . . . ? C26 C21 C22 C23 -57.2(5) . . . . ? C21 C22 C23 C24 51.6(6) . . . . ? C22 C23 C24 C25 -51.3(6) . . . . ? C23 C24 C25 C26 56.3(6) . . . . ? C22 C21 C26 C25 60.9(5) . . . . ? C22 C21 C26 P2 -172.9(3) . . . . ? C24 C25 C26 C21 -60.8(5) . . . . ? C24 C25 C26 P2 173.6(3) . . . . ? C20 P2 C26 C21 81.7(3) . . . . ? C27 P2 C26 C21 -172.0(3) . . . . ? Pd1 P2 C26 C21 -45.2(3) . . . . ? C20 P2 C26 C25 -155.4(3) . . . . ? C27 P2 C26 C25 -49.0(4) . . . . ? Pd1 P2 C26 C25 77.7(3) . . . . ? C26 P2 C27 C28 -174.2(3) . . . . ? C20 P2 C27 C28 -66.2(4) . . . . ? Pd1 P2 C27 C28 60.5(4) . . . . ? C26 P2 C27 C32 -47.1(4) . . . . ? C20 P2 C27 C32 60.8(4) . . . . ? Pd1 P2 C27 C32 -172.5(3) . . . . ? C32 C27 C28 C29 55.1(5) . . . . ? P2 C27 C28 C29 -175.9(3) . . . . ? C27 C28 C29 C30 -52.9(6) . . . . ? C28 C29 C30 C31 53.0(6) . . . . ? C29 C30 C31 C32 -56.6(6) . . . . ? C30 C31 C32 C27 58.7(6) . . . . ? C28 C27 C32 C31 -57.5(5) . . . . ? P2 C27 C32 C31 175.0(3) . . . . ? P2 Pd1 C33 C40 -172.3(3) . . . . ? P1 Pd1 C33 C40 -4.1(6) . . . . ? C40 Pd1 C33 C34 115.3(6) . . . . ? P2 Pd1 C33 C34 -57.1(4) . . . . ? P1 Pd1 C33 C34 111.2(4) . . . . ? C40 C33 C34 C39 32.4(7) . . . . ? Pd1 C33 C34 C39 -55.5(6) . . . . ? C40 C33 C34 C35 -145.2(5) . . . . ? Pd1 C33 C34 C35 127.0(4) . . . . ? C39 C34 C35 C36 -0.2(7) . . . . ? C33 C34 C35 C36 177.5(5) . . . . ? C34 C35 C36 C37 0.1(8) . . . . ? C35 C36 C37 C38 -0.1(9) . . . . ? C36 C37 C38 C39 0.2(9) . . . . ? C35 C34 C39 C38 0.3(7) . . . . ? C33 C34 C39 C38 -177.2(5) . . . . ? C37 C38 C39 C34 -0.4(8) . . . . ? C34 C33 C40 C41 166.5(4) . . . . ? Pd1 C33 C40 C41 -76.1(4) . . . . ? C34 C33 C40 Pd1 -117.5(4) . . . . ? C33 Pd1 C40 C41 125.9(5) . . . . ? P2 Pd1 C40 C41 137.2(2) . . . . ? P1 Pd1 C40 C41 -55.9(3) . . . . ? P2 Pd1 C40 C33 11.3(4) . . . . ? P1 Pd1 C40 C33 178.2(3) . . . . ? C33 C40 C41 O1 -178.7(4) . . . . ? Pd1 C40 C41 O1 116.4(4) . . . . ? C33 C40 C41 C42 -4.6(7) . . . . ? Pd1 C40 C41 C42 -69.5(4) . . . . ? O1 C41 C42 C43 8.3(7) . . . . ? C40 C41 C42 C43 -166.2(5) . . . . ? C41 C42 C43 C44 -177.2(4) . . . . ? C42 C43 C44 C45 15.8(7) . . . . ? C42 C43 C44 C49 -164.5(5) . . . . ? C49 C44 C45 C46 2.1(7) . . . . ? C43 C44 C45 C46 -178.3(5) . . . . ? C44 C45 C46 C47 -0.1(8) . . . . ? C45 C46 C47 C48 -1.4(9) . . . . ? C46 C47 C48 C49 0.8(10) . . . . ? C47 C48 C49 C44 1.3(10) . . . . ? C45 C44 C49 C48 -2.7(8) . . . . ? C43 C44 C49 C48 177.7(5) . . . . ? C54 O50 C51 C52 0.4(11) . . . . ? O50 C51 C52 C53 -6.3(16) . . . . ? C51 C52 C53 C54 9.0(15) . . . . ? C51 O50 C54 C53 5.3(8) . . . . ? C52 C53 C54 O50 -8.7(11) . . . . ? C64 O60 C61 C62 9(2) . . . . ? O60 C61 C62 C63 -14.2(18) . . . . ? C61 C62 C63 C64 13(2) . . . . ? C61 O60 C64 C63 0(2) . . . . ? C62 C63 C64 O60 -8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 22.39 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.962 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.097 data_exti23 _database_code_CSD 181821 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 O2 P2 Pd' _chemical_formula_weight 532.93 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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9816(5) _cell_length_b 19.8520(10) _cell_length_c 14.5897(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.199(2) _cell_angle_gamma 90.00 _cell_volume 2542.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 12132 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 28.47 _exptl_crystal_description Block _exptl_crystal_colour Blue/Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15908 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.47 _reflns_number_total 5916 _reflns_number_gt 5338 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0215P)^2^+3.3628P] 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 SHELXL _refine_ls_extinction_coef 0.00112(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5916 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 Pd Pd 0.291611(18) 0.751738(8) 0.478369(11) 0.01669(6) Uani 1 1 d . . . C1 C 0.0024(3) 0.76227(12) 0.21950(16) 0.0222(5) Uani 1 1 d . . . C2 C -0.1449(3) 0.78405(14) 0.17727(17) 0.0297(5) Uani 1 1 d . . . H2 H -0.1625 0.8309 0.1670 0.036 Uiso 1 1 calc R . . C3 C -0.2652(3) 0.74003(15) 0.15012(19) 0.0340(6) Uani 1 1 d . . . H3 H -0.3642 0.7566 0.1236 0.041 Uiso 1 1 calc R . . C4 C -0.2399(3) 0.67180(15) 0.16196(18) 0.0322(6) Uani 1 1 d . . . H4 H -0.3219 0.6409 0.1449 0.039 Uiso 1 1 calc R . . C5 C -0.0944(3) 0.64866(14) 0.19878(17) 0.0279(5) Uani 1 1 d . . . H5 H -0.0772 0.6015 0.2038 0.033 Uiso 1 1 calc R . . C6 C 0.0284(3) 0.69237(12) 0.22883(15) 0.0214(4) Uani 1 1 d . . . C7 C 0.1858(3) 0.66219(12) 0.26109(15) 0.0215(4) Uani 1 1 d . . . H7A H 0.2560 0.6878 0.2303 0.026 Uiso 1 1 calc R . . H7B H 0.1820 0.6156 0.2364 0.026 Uiso 1 1 calc R . . P1 P 0.27318(6) 0.65816(3) 0.38731(4) 0.01757(12) Uani 1 1 d . . . C8 C 0.1641(3) 0.59092(12) 0.43737(16) 0.0229(5) Uani 1 1 d . . . C9 C 0.2405(3) 0.57453(14) 0.53971(17) 0.0299(5) Uani 1 1 d . . . H9A H 0.2709 0.6165 0.5739 0.045 Uiso 1 1 calc R . . H9B H 0.3308 0.5465 0.5408 0.045 Uiso 1 1 calc R . . H9C H 0.1685 0.5501 0.5695 0.045 Uiso 1 1 calc R . . C10 C 0.1427(3) 0.52554(13) 0.3798(2) 0.0345(6) Uani 1 1 d . . . H10A H 0.2424 0.5053 0.3803 0.052 Uiso 1 1 calc R . . H10B H 0.0915 0.5356 0.3150 0.052 Uiso 1 1 calc R . . H10C H 0.0806 0.4939 0.4072 0.052 Uiso 1 1 calc R . . C11 C 0.0082(3) 0.62193(14) 0.4403(2) 0.0325(6) Uani 1 1 d . . . H11A H 0.0225 0.6605 0.4831 0.049 Uiso 1 1 calc R . . H11B H -0.0555 0.5881 0.4623 0.049 Uiso 1 1 calc R . . H11C H -0.0416 0.6369 0.3772 0.049 Uiso 1 1 calc R . . C12 C 0.4732(3) 0.63068(12) 0.38295(17) 0.0237(5) Uani 1 1 d . . . C13 C 0.5537(3) 0.69377(14) 0.35644(19) 0.0306(5) Uani 1 1 d . . . H13A H 0.5564 0.7284 0.4046 0.046 Uiso 1 1 calc R . . H13B H 0.4981 0.7109 0.2958 0.046 Uiso 1 1 calc R . . H13C H 0.6580 0.6822 0.3520 0.046 Uiso 1 1 calc R . . C14 C 0.5597(3) 0.60768(14) 0.48000(19) 0.0323(6) Uani 1 1 d . . . H14A H 0.6689 0.6055 0.4807 0.048 Uiso 1 1 calc R . . H14B H 0.5235 0.5630 0.4937 0.048 Uiso 1 1 calc R . . H14C H 0.5419 0.6398 0.5276 0.048 Uiso 1 1 calc R . . C15 C 0.4827(3) 0.57556(15) 0.3104(2) 0.0390(7) Uani 1 1 d . . . H15A H 0.5898 0.5646 0.3124 0.059 Uiso 1 1 calc R . . H15B H 0.4350 0.5918 0.2476 0.059 Uiso 1 1 calc R . . H15C H 0.4294 0.5351 0.3249 0.059 Uiso 1 1 calc R . . O1 O 0.3776(2) 0.72280(9) 0.61125(11) 0.0260(4) Uani 1 1 d . . . O2 O 0.3599(2) 0.79503(9) 0.60551(11) 0.0279(4) Uani 1 1 d . . . C16 C 0.3477(3) 0.90021(12) 0.36773(17) 0.0281(5) Uani 1 1 d . . . C17 C 0.4501(3) 0.87507(14) 0.30267(19) 0.0325(6) Uani 1 1 d . . . H17A H 0.5378 0.9052 0.3075 0.049 Uiso 1 1 calc R . . H17B H 0.3919 0.8745 0.2378 0.049 Uiso 1 1 calc R . . H17C H 0.4859 0.8294 0.3212 0.049 Uiso 1 1 calc R . . C18 C 0.4502(4) 0.90778(15) 0.46608(19) 0.0385(7) Uani 1 1 d . . . H18A H 0.5329 0.9394 0.4633 0.058 Uiso 1 1 calc R . . H18B H 0.4934 0.8638 0.4879 0.058 Uiso 1 1 calc R . . H18C H 0.3897 0.9249 0.5096 0.058 Uiso 1 1 calc R . . C19 C 0.2843(4) 0.96939(14) 0.3321(2) 0.0393(7) Uani 1 1 d . . . H19A H 0.2282 0.9888 0.3766 0.059 Uiso 1 1 calc R . . H19B H 0.2156 0.9643 0.2707 0.059 Uiso 1 1 calc R . . H19C H 0.3687 0.9993 0.3264 0.059 Uiso 1 1 calc R . . P2 P 0.19694(7) 0.83389(3) 0.37213(4) 0.02033(12) Uani 1 1 d . . . C20 C 0.0300(3) 0.87236(13) 0.41408(18) 0.0286(5) Uani 1 1 d . . . C21 C 0.0886(4) 0.90882(14) 0.50774(19) 0.0363(6) Uani 1 1 d . . . H21A H 0.1423 0.9500 0.4966 0.054 Uiso 1 1 calc R . . H21B H 0.1585 0.8792 0.5503 0.054 Uiso 1 1 calc R . . H21C H 0.0023 0.9205 0.5360 0.054 Uiso 1 1 calc R . . C22 C -0.0690(3) 0.92116(15) 0.3446(2) 0.0380(6) Uani 1 1 d . . . H22A H -0.1535 0.9375 0.3714 0.057 Uiso 1 1 calc R . . H22B H -0.1095 0.8976 0.2856 0.057 Uiso 1 1 calc R . . H22C H -0.0068 0.9594 0.3326 0.057 Uiso 1 1 calc R . . C23 C -0.0706(3) 0.81330(14) 0.4330(2) 0.0347(6) Uani 1 1 d . . . H23A H -0.0115 0.7838 0.4811 0.052 Uiso 1 1 calc R . . H23B H -0.1053 0.7876 0.3750 0.052 Uiso 1 1 calc R . . H23C H -0.1590 0.8309 0.4548 0.052 Uiso 1 1 calc R . . C24 C 0.1286(3) 0.81345(12) 0.24609(16) 0.0227(5) Uani 1 1 d . . . H24B H 0.0938 0.8559 0.2128 0.027 Uiso 1 1 calc R . . H24A H 0.2170 0.7972 0.2217 0.027 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 Pd 0.01863(10) 0.01793(9) 0.01341(9) 0.00035(6) 0.00313(6) 0.00104(6) C1 0.0218(11) 0.0281(12) 0.0159(10) 0.0009(9) 0.0023(8) -0.0012(9) C2 0.0278(12) 0.0347(14) 0.0238(12) 0.0016(10) -0.0006(10) 0.0063(11) C3 0.0223(12) 0.0519(17) 0.0252(13) 0.0012(11) -0.0007(10) 0.0021(11) C4 0.0250(12) 0.0479(16) 0.0216(12) 0.0011(11) 0.0007(9) -0.0104(12) C5 0.0283(12) 0.0322(13) 0.0215(11) 0.0000(10) 0.0016(9) -0.0053(10) C6 0.0226(11) 0.0272(11) 0.0141(10) -0.0001(8) 0.0034(8) -0.0023(9) C7 0.0245(11) 0.0242(11) 0.0155(10) -0.0007(8) 0.0035(8) 0.0001(9) P1 0.0182(3) 0.0183(3) 0.0159(3) -0.0001(2) 0.0031(2) 0.0005(2) C8 0.0254(11) 0.0219(11) 0.0212(11) 0.0024(9) 0.0045(9) -0.0038(9) C9 0.0346(13) 0.0314(13) 0.0234(12) 0.0077(10) 0.0052(10) -0.0036(11) C10 0.0479(16) 0.0240(12) 0.0326(14) -0.0011(10) 0.0109(12) -0.0081(11) C11 0.0274(13) 0.0373(14) 0.0346(14) 0.0109(11) 0.0108(11) -0.0009(11) C12 0.0194(11) 0.0264(12) 0.0259(12) -0.0014(9) 0.0062(9) 0.0041(9) C13 0.0226(12) 0.0366(14) 0.0344(14) 0.0044(11) 0.0098(10) 0.0009(10) C14 0.0254(12) 0.0352(14) 0.0349(14) 0.0058(11) 0.0037(11) 0.0079(11) C15 0.0334(14) 0.0410(16) 0.0452(17) -0.0138(13) 0.0138(12) 0.0078(12) O1 0.0299(9) 0.0299(9) 0.0168(8) 0.0053(7) 0.0015(7) 0.0009(7) O2 0.0363(10) 0.0282(9) 0.0178(8) -0.0056(7) 0.0023(7) 0.0022(7) C16 0.0367(14) 0.0215(11) 0.0234(12) 0.0012(9) 0.0004(10) -0.0052(10) C17 0.0311(13) 0.0348(14) 0.0319(13) -0.0014(11) 0.0079(11) -0.0098(11) C18 0.0485(17) 0.0354(15) 0.0270(13) 0.0000(11) -0.0021(12) -0.0170(13) C19 0.0551(18) 0.0240(13) 0.0399(15) 0.0073(11) 0.0124(14) -0.0018(12) P2 0.0262(3) 0.0181(3) 0.0162(3) 0.0012(2) 0.0032(2) 0.0018(2) C20 0.0349(13) 0.0270(12) 0.0250(12) 0.0015(10) 0.0088(10) 0.0109(10) C21 0.0515(17) 0.0311(14) 0.0282(13) 0.0014(11) 0.0131(12) 0.0140(12) C22 0.0442(16) 0.0369(15) 0.0331(14) 0.0055(12) 0.0084(12) 0.0169(13) C23 0.0357(14) 0.0373(15) 0.0356(14) 0.0046(12) 0.0179(12) 0.0093(12) C24 0.0239(11) 0.0240(11) 0.0188(10) 0.0022(9) 0.0017(9) 0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.404(3) . ? C1 C6 1.409(3) . ? C1 C24 1.510(3) . ? C2 C3 1.381(4) . ? C3 C4 1.378(4) . ? C4 C5 1.383(4) . ? C5 C6 1.399(3) . ? C6 C7 1.516(3) . ? C7 P1 1.845(2) . ? P1 Pd 2.2694(6) . ? P1 C8 1.892(2) . ? P1 C12 1.891(2) . ? C8 C9 1.541(3) . ? C8 C10 1.536(3) . ? C8 C11 1.538(3) . ? C12 C13 1.536(4) . ? C12 C14 1.534(3) . ? C12 C15 1.538(3) . ? Pd O1 2.0130(16) . ? Pd O2 2.0187(16) . ? Pd P2 2.2865(6) . ? O1 O2 1.443(3) . ? C16 C17 1.538(4) . ? C16 C18 1.540(3) . ? C16 C19 1.535(4) . ? C16 P2 1.899(3) . ? P2 C20 1.895(3) . ? P2 C24 1.856(2) . ? C20 C21 1.538(4) . ? C20 C22 1.541(4) . ? C20 C23 1.540(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.8(2) . . ? C2 C1 C24 119.5(2) . . ? C6 C1 C24 122.5(2) . . ? C1 C2 C3 122.6(3) . . ? C2 C3 C4 119.2(2) . . ? C3 C4 C5 119.5(2) . . ? C4 C5 C6 122.2(3) . . ? C1 C6 C5 118.5(2) . . ? C1 C6 C7 122.9(2) . . ? C5 C6 C7 118.3(2) . . ? C6 C7 P1 119.96(16) . . ? Pd P1 C7 120.79(8) . . ? Pd P1 C8 109.34(8) . . ? Pd P1 C12 107.67(8) . . ? C7 P1 C8 105.67(11) . . ? C7 P1 C12 100.71(11) . . ? C8 P1 C12 112.49(11) . . ? P1 C8 C9 111.24(16) . . ? P1 C8 C10 113.58(17) . . ? P1 C8 C11 106.08(16) . . ? C9 C8 C10 109.3(2) . . ? C9 C8 C11 106.2(2) . . ? C10 C8 C11 110.1(2) . . ? P1 C12 C13 105.92(16) . . ? P1 C12 C14 110.75(17) . . ? P1 C12 C15 114.84(18) . . ? C13 C12 C14 107.6(2) . . ? C13 C12 C15 108.0(2) . . ? C14 C12 C15 109.4(2) . . ? P1 Pd O1 107.21(5) . . ? P1 Pd O2 148.96(5) . . ? P1 Pd P2 102.50(2) . . ? O1 Pd O2 41.95(7) . . ? O1 Pd P2 150.27(5) . . ? O2 Pd P2 108.45(5) . . ? Pd O1 O2 69.24(9) . . ? Pd O2 O1 68.81(9) . . ? C17 C16 C18 106.8(2) . . ? C17 C16 C19 108.0(2) . . ? C17 C16 P2 108.64(17) . . ? C18 C16 C19 109.5(2) . . ? C18 C16 P2 109.05(18) . . ? C19 C16 P2 114.6(2) . . ? Pd P2 C16 110.59(8) . . ? Pd P2 C20 105.94(8) . . ? Pd P2 C24 120.88(8) . . ? C16 P2 C20 110.47(12) . . ? C16 P2 C24 101.95(11) . . ? C20 P2 C24 106.81(11) . . ? P2 C20 C21 109.34(19) . . ? P2 C20 C22 115.26(19) . . ? P2 C20 C23 106.56(17) . . ? C21 C20 C22 109.3(2) . . ? C21 C20 C23 107.6(2) . . ? C22 C20 C23 108.5(2) . . ? C1 C24 P2 118.34(16) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.771 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.074 data_exti43 _database_code_CSD 181822 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 O2 P2 Pd' _chemical_formula_weight 609.02 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.725(3) _cell_length_b 16.465(6) _cell_length_c 21.038(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.544(7) _cell_angle_gamma 90.00 _cell_volume 3012.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 6453 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.67 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.374 _exptl_absorpt_correction_T_max 0.802 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15281 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.1382 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5301 _reflns_number_gt 3207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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 w=1/[\s^2^(Fo^2^)+(0.0866P)^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 except H1&2 coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5301 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.61856(6) 0.80117(3) 0.10994(2) 0.0194(2) Uani 1 d . . . O1 O 0.3090(6) 0.9430(3) 0.1814(3) 0.0430(15) Uani 1 d . . . O2 O 0.2804(6) 0.7637(4) -0.0261(2) 0.0425(15) Uani 1 d . . . C1 C 0.3858(8) 0.8177(5) 0.1385(4) 0.0289(19) Uani 1 d D . . H1 H 0.386(8) 0.792(4) 0.1789(16) 0.035 Uiso 1 d D . . C2 C 0.3794(8) 0.7684(5) 0.0827(3) 0.0239(17) Uani 1 d D . . H2 H 0.364(8) 0.7117(9) 0.088(3) 0.029 Uiso 1 d D . . C3 C 0.3274(8) 0.8055(5) 0.0224(4) 0.0312(19) Uani 1 d . . . C4 C 0.3233(8) 0.8928(5) 0.0178(4) 0.039(2) Uani 1 d . . . H4 H 0.3149 0.9179 -0.0230 0.046 Uiso 1 calc R . . C5 C 0.3312(9) 0.9389(6) 0.0706(4) 0.042(2) Uani 1 d . . . H5 H 0.3293 0.9964 0.0666 0.051 Uiso 1 calc R . . C6 C 0.3428(8) 0.9020(5) 0.1350(4) 0.034(2) Uani 1 d . . . P1 P 0.7753(2) 0.73222(12) 0.04143(8) 0.0206(4) Uani 1 d . . . P2 P 0.7931(2) 0.85787(11) 0.18951(8) 0.0201(4) Uani 1 d . . . C7 C 0.7083(9) 0.6234(5) 0.0300(3) 0.0319(19) Uani 1 d . . . C8 C 0.8214(10) 0.5635(5) 0.0022(4) 0.042(2) Uani 1 d . . . H8A H 0.7758 0.5091 0.0000 0.064 Uiso 1 calc R . . H8B H 0.9175 0.5623 0.0297 0.064 Uiso 1 calc R . . H8C H 0.8426 0.5811 -0.0407 0.064 Uiso 1 calc R . . C9 C 0.5563(9) 0.6212(5) -0.0135(4) 0.036(2) Uani 1 d . . . H9A H 0.5780 0.6325 -0.0576 0.054 Uiso 1 calc R . . H9B H 0.4854 0.6623 0.0008 0.054 Uiso 1 calc R . . H9C H 0.5093 0.5673 -0.0112 0.054 Uiso 1 calc R . . C10 C 0.6719(10) 0.5930(4) 0.0980(4) 0.036(2) Uani 1 d . . . H10A H 0.5872 0.6251 0.1130 0.054 Uiso 1 calc R . . H10B H 0.7634 0.5995 0.1278 0.054 Uiso 1 calc R . . H10C H 0.6424 0.5356 0.0958 0.054 Uiso 1 calc R . . C11 C 0.7885(8) 0.7821(5) -0.0398(3) 0.0290(19) Uani 1 d . . . C12 C 0.6279(8) 0.8135(5) -0.0644(3) 0.0307(19) Uani 1 d . . . H12A H 0.6349 0.8417 -0.1051 0.046 Uiso 1 calc R . . H12B H 0.5900 0.8512 -0.0332 0.046 Uiso 1 calc R . . H12C H 0.5568 0.7676 -0.0705 0.046 Uiso 1 calc R . . C13 C 0.8525(11) 0.7280(5) -0.0909(4) 0.045(2) Uani 1 d . . . H13A H 0.7889 0.6792 -0.0970 0.068 Uiso 1 calc R . . H13B H 0.9584 0.7124 -0.0772 0.068 Uiso 1 calc R . . H13C H 0.8512 0.7580 -0.1312 0.068 Uiso 1 calc R . . C14 C 0.8926(9) 0.8562(5) -0.0308(4) 0.037(2) Uani 1 d . . . H14A H 0.9996 0.8385 -0.0225 0.055 Uiso 1 calc R . . H14B H 0.8624 0.8883 0.0054 0.055 Uiso 1 calc R . . H14C H 0.8829 0.8895 -0.0696 0.055 Uiso 1 calc R . . C15 C 0.9840(8) 0.7240(5) 0.0678(3) 0.0276(18) Uani 1 d . . . H15A H 1.0329 0.6914 0.0354 0.033 Uiso 1 calc R . . H15B H 1.0282 0.7793 0.0666 0.033 Uiso 1 calc R . . C16 C 1.0335(7) 0.6879(4) 0.1327(3) 0.0238(17) Uani 1 d . . . C17 C 1.0938(9) 0.6096(5) 0.1357(4) 0.034(2) Uani 1 d . . . H17 H 1.0955 0.5789 0.0975 0.041 Uiso 1 calc R . . C18 C 1.1519(9) 0.5747(5) 0.1929(4) 0.033(2) Uani 1 d . . . H18 H 1.1893 0.5205 0.1938 0.040 Uiso 1 calc R . . C19 C 1.1543(9) 0.6196(5) 0.2479(4) 0.037(2) Uani 1 d . . . H19 H 1.1922 0.5965 0.2875 0.045 Uiso 1 calc R . . C20 C 1.1017(8) 0.6979(5) 0.2454(3) 0.0311(18) Uani 1 d . . . H20 H 1.1086 0.7291 0.2835 0.037 Uiso 1 calc R . . C21 C 1.0384(8) 0.7338(5) 0.1891(3) 0.0237(17) Uani 1 d . . . C22 C 0.9957(8) 0.8233(4) 0.1881(3) 0.0232(17) Uani 1 d . . . H22A H 1.0356 0.8469 0.1494 0.028 Uiso 1 calc R . . H22B H 1.0543 0.8488 0.2251 0.028 Uiso 1 calc R . . C23 C 0.7366(8) 0.8300(5) 0.2726(3) 0.0265(18) Uani 1 d . . . C24 C 0.5966(8) 0.8794(5) 0.2893(3) 0.0318(19) Uani 1 d . . . H24A H 0.5158 0.8756 0.2544 0.048 Uiso 1 calc R . . H24B H 0.6264 0.9364 0.2959 0.048 Uiso 1 calc R . . H24C H 0.5581 0.8579 0.3285 0.048 Uiso 1 calc R . . C25 C 0.8658(10) 0.8421(5) 0.3277(3) 0.038(2) Uani 1 d . . . H25A H 0.8295 0.8223 0.3678 0.057 Uiso 1 calc R . . H25B H 0.8910 0.9000 0.3318 0.057 Uiso 1 calc R . . H25C H 0.9576 0.8117 0.3181 0.057 Uiso 1 calc R . . C26 C 0.6939(10) 0.7411(5) 0.2696(4) 0.040(2) Uani 1 d . . . H26A H 0.6638 0.7233 0.3113 0.060 Uiso 1 calc R . . H26B H 0.7824 0.7091 0.2581 0.060 Uiso 1 calc R . . H26C H 0.6077 0.7330 0.2374 0.060 Uiso 1 calc R . . C27 C 0.8215(8) 0.9715(4) 0.1824(3) 0.0221(17) Uani 1 d . . . C28 C 0.9129(10) 1.0103(5) 0.2401(4) 0.045(2) Uani 1 d . . . H28A H 1.0107 0.9815 0.2486 0.068 Uiso 1 calc R . . H28B H 0.8533 1.0065 0.2775 0.068 Uiso 1 calc R . . H28C H 0.9331 1.0675 0.2309 0.068 Uiso 1 calc R . . C29 C 0.6639(8) 1.0128(5) 0.1720(4) 0.037(2) Uani 1 d . . . H29A H 0.6780 1.0713 0.1660 0.055 Uiso 1 calc R . . H29B H 0.6056 1.0036 0.2093 0.055 Uiso 1 calc R . . H29C H 0.6074 0.9899 0.1340 0.055 Uiso 1 calc R . . C30 C 0.9042(9) 0.9889(5) 0.1235(4) 0.041(2) Uani 1 d . . . H30A H 0.8919 1.0464 0.1121 0.062 Uiso 1 calc R . . H30B H 0.8607 0.9552 0.0882 0.062 Uiso 1 calc R . . H30C H 1.0138 0.9764 0.1320 0.062 Uiso 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 Pd 0.0141(3) 0.0265(4) 0.0156(3) -0.0002(3) -0.0122(2) -0.0009(3) O1 0.017(3) 0.053(4) 0.057(4) -0.026(3) -0.010(3) 0.003(3) O2 0.026(3) 0.070(4) 0.029(3) -0.007(3) -0.020(3) 0.001(3) C1 0.011(3) 0.045(6) 0.029(4) -0.002(4) -0.005(3) -0.004(4) C2 0.011(3) 0.030(5) 0.029(4) -0.005(4) -0.014(3) -0.007(3) C3 0.010(3) 0.049(6) 0.033(4) -0.003(4) -0.009(3) -0.002(4) C4 0.018(4) 0.049(7) 0.046(5) 0.015(5) -0.020(4) 0.002(4) C5 0.019(4) 0.044(6) 0.061(6) 0.007(5) -0.016(4) 0.005(4) C6 0.011(4) 0.040(6) 0.050(5) -0.010(4) -0.013(4) 0.000(4) P1 0.0180(10) 0.0279(12) 0.0139(9) 0.0007(8) -0.0117(8) 0.0001(8) P2 0.0161(9) 0.0255(12) 0.0163(9) 0.0005(8) -0.0136(8) -0.0011(8) C7 0.028(4) 0.043(5) 0.023(4) -0.005(4) -0.014(3) -0.002(4) C8 0.047(5) 0.033(5) 0.043(5) -0.013(4) -0.023(4) 0.010(4) C9 0.044(5) 0.025(5) 0.035(5) -0.003(4) -0.023(4) -0.008(4) C10 0.050(5) 0.014(5) 0.040(5) 0.009(4) -0.019(4) -0.005(4) C11 0.023(4) 0.042(6) 0.021(4) 0.005(3) -0.006(3) 0.004(4) C12 0.023(4) 0.045(6) 0.022(4) 0.005(4) -0.011(3) 0.006(4) C13 0.054(6) 0.059(6) 0.022(4) 0.009(4) 0.001(4) 0.020(5) C14 0.026(4) 0.050(6) 0.032(4) 0.020(4) -0.013(4) -0.004(4) C15 0.019(4) 0.045(5) 0.018(4) 0.002(3) -0.008(3) 0.010(3) C16 0.013(3) 0.033(5) 0.023(4) -0.001(3) -0.014(3) 0.004(3) C17 0.033(5) 0.032(5) 0.033(4) -0.009(4) -0.020(4) 0.007(4) C18 0.027(4) 0.026(5) 0.044(5) 0.009(4) -0.014(4) 0.011(4) C19 0.034(5) 0.050(6) 0.025(4) 0.013(4) -0.012(4) 0.011(4) C20 0.031(4) 0.035(5) 0.025(4) 0.004(4) -0.014(3) 0.008(4) C21 0.015(4) 0.029(5) 0.026(4) 0.007(3) -0.009(3) 0.004(3) C22 0.017(4) 0.035(5) 0.016(3) -0.002(3) -0.014(3) 0.001(3) C23 0.027(4) 0.035(5) 0.016(4) 0.000(3) -0.009(3) -0.003(4) C24 0.031(5) 0.045(5) 0.018(4) 0.005(4) -0.009(3) 0.001(4) C25 0.044(5) 0.054(6) 0.012(4) 0.004(4) -0.017(4) 0.002(4) C26 0.044(5) 0.045(6) 0.029(5) 0.017(4) -0.002(4) -0.006(4) C27 0.018(4) 0.022(5) 0.024(4) -0.002(3) -0.017(3) 0.001(3) C28 0.056(6) 0.022(5) 0.051(6) -0.007(4) -0.037(5) -0.006(4) C29 0.025(4) 0.030(5) 0.052(5) 0.005(4) -0.013(4) -0.003(4) C30 0.036(5) 0.037(6) 0.050(5) 0.018(4) -0.002(4) 0.004(4) _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 Pd C1 2.179(7) . ? Pd C2 2.187(7) . ? Pd P1 2.3556(19) . ? Pd P2 2.364(2) . ? O1 C6 1.241(9) . ? O2 C3 1.271(9) . ? C1 C2 1.425(10) . ? C1 C6 1.438(11) . ? C2 C3 1.448(11) . ? C3 C4 1.441(11) . ? C4 C5 1.343(11) . ? C5 C6 1.481(11) . ? P1 C7 1.894(8) . ? P1 C11 1.908(7) . ? P1 C15 1.866(7) . ? P2 C22 1.860(7) . ? P2 C23 1.909(7) . ? P2 C27 1.895(7) . ? C7 C8 1.541(10) . ? C7 C9 1.551(11) . ? C7 C10 1.573(10) . ? C11 C12 1.544(10) . ? C11 C13 1.535(10) . ? C11 C14 1.524(11) . ? C15 C16 1.520(10) . ? C16 C17 1.393(10) . ? C16 C21 1.406(10) . ? C17 C18 1.392(10) . ? C18 C19 1.372(11) . ? C19 C20 1.368(10) . ? C20 C21 1.398(10) . ? C21 C22 1.519(10) . ? C23 C24 1.532(10) . ? C23 C25 1.565(10) . ? C23 C26 1.511(11) . ? C27 C28 1.538(10) . ? C27 C29 1.534(10) . ? C27 C30 1.509(9) . ? 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 C1 Pd C2 38.1(3) . . ? C1 Pd P1 145.8(2) . . ? C1 Pd P2 108.5(2) . . ? C2 Pd P1 108.0(2) . . ? C2 Pd P2 146.16(19) . . ? P1 Pd P2 104.53(7) . . ? Pd C1 C2 71.3(4) . . ? Pd C1 C6 110.6(5) . . ? C2 C1 C6 121.1(7) . . ? Pd C2 C1 70.7(4) . . ? Pd C2 C3 110.6(5) . . ? C1 C2 C3 118.0(7) . . ? O2 C3 C2 122.3(8) . . ? O2 C3 C4 118.7(7) . . ? C2 C3 C4 119.0(7) . . ? C3 C4 C5 120.6(8) . . ? C4 C5 C6 121.4(8) . . ? O1 C6 C1 124.2(8) . . ? O1 C6 C5 119.6(8) . . ? C1 C6 C5 116.1(7) . . ? Pd P1 C7 110.2(2) . . ? Pd P1 C11 114.8(2) . . ? Pd P1 C15 117.0(2) . . ? C7 P1 C11 109.4(3) . . ? C7 P1 C15 104.7(4) . . ? C11 P1 C15 99.8(3) . . ? Pd P2 C22 115.3(2) . . ? Pd P2 C23 110.8(2) . . ? Pd P2 C27 114.5(2) . . ? C22 P2 C23 104.8(3) . . ? C22 P2 C27 99.8(3) . . ? C23 P2 C27 110.8(3) . . ? P1 C7 C8 116.9(6) . . ? P1 C7 C9 109.8(6) . . ? P1 C7 C10 105.5(5) . . ? C8 C7 C9 107.7(6) . . ? C8 C7 C10 108.8(7) . . ? C9 C7 C10 107.7(6) . . ? P1 C11 C12 109.1(5) . . ? P1 C11 C13 115.4(5) . . ? P1 C11 C14 108.1(5) . . ? C12 C11 C13 109.3(6) . . ? C12 C11 C14 106.9(6) . . ? C13 C11 C14 107.7(7) . . ? P1 C15 C16 119.8(5) . . ? C15 C16 C17 118.9(6) . . ? C15 C16 C21 122.4(7) . . ? C17 C16 C21 118.3(7) . . ? C16 C17 C18 122.1(7) . . ? C17 C18 C19 119.2(7) . . ? C18 C19 C20 119.5(7) . . ? C19 C20 C21 122.8(7) . . ? C16 C21 C20 118.1(7) . . ? C16 C21 C22 121.3(6) . . ? C20 C21 C22 120.2(7) . . ? P2 C22 C21 121.9(5) . . ? P2 C23 C24 110.5(5) . . ? P2 C23 C25 115.2(5) . . ? P2 C23 C26 106.0(5) . . ? C24 C23 C25 107.6(6) . . ? C24 C23 C26 109.0(6) . . ? C25 C23 C26 108.4(7) . . ? P2 C27 C28 114.2(5) . . ? P2 C27 C29 109.1(5) . . ? P2 C27 C30 109.0(5) . . ? C28 C27 C29 109.4(6) . . ? C28 C27 C30 108.5(6) . . ? C29 C27 C30 106.3(6) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 2.592 _refine_diff_density_min -2.004 _refine_diff_density_rms 0.173