# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ronan M. Bellabarba' 'Alexandra M. Z. Slawin' 'Robert P. Tooze' _publ_contact_author_name 'Dr Ronan M. Bellabarba' _publ_contact_author_address ; Sasol Technology UK Purdie Building North Haugh St Andrews Fife KY 16 9ST UNITED KINGDOM ; _publ_contact_author_email RONAN.BELLABARBA@SASOL.COM _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis, X-ray characterisation and reactions of a trigonal planar palladium (0) carbonyl complex, (tbpx)PdCO. ; data_1 _database_code_CSD 211529 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H44 O P2 Pd' _chemical_formula_sum 'C25 H44 O P2 Pd' _chemical_formula_weight 528.94 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 11.837(3) _cell_length_b 16.063(4) _cell_length_c 14.731(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.358(7) _cell_angle_gamma 90.00 _cell_volume 2796.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6186 _cell_measurement_theta_min 2.4928 _cell_measurement_theta_max 24.7121 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6555 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.85 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10203 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4392 _reflns_number_gt 3478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+7.0627P] 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 SHELXL _refine_ls_extinction_coef 0.0023(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4392 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.12658(3) -0.12608(3) 0.19868(3) 0.0485(2) Uani 1 1 d . . . P1 P -0.05474(12) -0.09585(11) 0.24577(11) 0.0486(4) Uani 1 1 d . . . C2 C -0.0607(5) -0.0470(4) 0.3597(4) 0.0542(15) Uani 1 1 d . . . H2A H -0.1399 -0.0411 0.3720 0.065 Uiso 1 1 calc R . . H2B H -0.0278 -0.0861 0.4039 0.065 Uiso 1 1 calc R . . C3 C -0.0034(5) 0.0383(4) 0.3785(4) 0.0574(16) Uani 1 1 d . . . C4 C 0.1143(5) 0.0483(4) 0.3980(4) 0.0576(16) Uani 1 1 d . . . C5 C 0.1545(7) 0.1286(5) 0.4185(5) 0.073(2) Uani 1 1 d . . . H5A H 0.2313 0.1368 0.4323 0.087 Uiso 1 1 calc R . . C6 C 0.0823(7) 0.1953(4) 0.4186(5) 0.071(2) Uani 1 1 d . . . H6A H 0.1115 0.2478 0.4326 0.085 Uiso 1 1 calc R . . C7 C -0.0303(7) 0.1870(4) 0.3990(5) 0.071(2) Uani 1 1 d . . . H7A H -0.0778 0.2331 0.3977 0.085 Uiso 1 1 calc R . . C8 C -0.0712(6) 0.1107(5) 0.3815(5) 0.072(2) Uani 1 1 d . . . H8A H -0.1489 0.1048 0.3706 0.086 Uiso 1 1 calc R . . C9 C -0.1355(5) -0.0221(5) 0.1645(5) 0.0656(18) Uani 1 1 d . . . C10 C -0.2497(6) 0.0092(6) 0.1947(6) 0.098(3) Uani 1 1 d . . . H10A H -0.2832 0.0459 0.1492 0.147 Uiso 1 1 calc R . . H10B H -0.2384 0.0387 0.2512 0.147 Uiso 1 1 calc R . . H10C H -0.2991 -0.0373 0.2026 0.147 Uiso 1 1 calc R . . C11 C -0.0561(7) 0.0516(5) 0.1526(5) 0.086(2) Uani 1 1 d . . . H11A H -0.0922 0.0913 0.1118 0.128 Uiso 1 1 calc R . . H11B H 0.0125 0.0323 0.1280 0.128 Uiso 1 1 calc R . . H11C H -0.0387 0.0774 0.2105 0.128 Uiso 1 1 calc R . . C12 C -0.1526(8) -0.0633(6) 0.0701(5) 0.097(3) Uani 1 1 d . . . H12A H -0.1931 -0.0260 0.0291 0.145 Uiso 1 1 calc R . . H12B H -0.1951 -0.1139 0.0753 0.145 Uiso 1 1 calc R . . H12C H -0.0802 -0.0758 0.0473 0.145 Uiso 1 1 calc R . . C13 C -0.1382(5) -0.1945(5) 0.2651(5) 0.0684(19) Uani 1 1 d . . . C14 C -0.2527(7) -0.1826(6) 0.3048(8) 0.117(4) Uani 1 1 d . . . H14A H -0.2877 -0.2358 0.3124 0.175 Uiso 1 1 calc R . . H14B H -0.3000 -0.1490 0.2644 0.175 Uiso 1 1 calc R . . H14C H -0.2427 -0.1554 0.3628 0.175 Uiso 1 1 calc R . . C15 C -0.1519(7) -0.2448(5) 0.1767(6) 0.096(3) Uani 1 1 d . . . H15A H -0.1940 -0.2946 0.1871 0.144 Uiso 1 1 calc R . . H15B H -0.0786 -0.2593 0.1568 0.144 Uiso 1 1 calc R . . H15C H -0.1917 -0.2120 0.1307 0.144 Uiso 1 1 calc R . . C16 C -0.0618(8) -0.2476(5) 0.3305(7) 0.100(3) Uani 1 1 d . . . H16A H -0.0997 -0.2988 0.3434 0.149 Uiso 1 1 calc R . . H16B H -0.0459 -0.2175 0.3861 0.149 Uiso 1 1 calc R . . H16C H 0.0078 -0.2597 0.3029 0.149 Uiso 1 1 calc R . . C17 C 0.1958(5) -0.0256(4) 0.4115(4) 0.0557(16) Uani 1 1 d . . . H17A H 0.1563 -0.0685 0.4435 0.067 Uiso 1 1 calc R . . H17B H 0.2583 -0.0072 0.4521 0.067 Uiso 1 1 calc R . . P18 P 0.25782(12) -0.07600(10) 0.31207(11) 0.0471(4) Uani 1 1 d . . . C19 C 0.3539(6) 0.0049(5) 0.2645(5) 0.0691(19) Uani 1 1 d . . . C20 C 0.4232(7) -0.0341(6) 0.1912(7) 0.109(3) Uani 1 1 d . . . H20A H 0.4718 0.0073 0.1672 0.163 Uiso 1 1 calc R . . H20B H 0.3731 -0.0554 0.1431 0.163 Uiso 1 1 calc R . . H20C H 0.4683 -0.0787 0.2172 0.163 Uiso 1 1 calc R . . C21 C 0.2768(7) 0.0685(5) 0.2159(6) 0.094(3) Uani 1 1 d . . . H21A H 0.3218 0.1113 0.1904 0.141 Uiso 1 1 calc R . . H21B H 0.2279 0.0928 0.2584 0.141 Uiso 1 1 calc R . . H21C H 0.2319 0.0416 0.1681 0.141 Uiso 1 1 calc R . . C22 C 0.4343(8) 0.0492(7) 0.3351(7) 0.119(4) Uani 1 1 d . . . H22A H 0.4794 0.0891 0.3049 0.179 Uiso 1 1 calc R . . H22B H 0.4828 0.0089 0.3657 0.179 Uiso 1 1 calc R . . H22C H 0.3906 0.0773 0.3788 0.179 Uiso 1 1 calc R . . C23 C 0.3439(5) -0.1607(4) 0.3721(5) 0.0611(17) Uani 1 1 d . . . C24 C 0.4264(9) -0.1330(6) 0.4501(8) 0.130(4) Uani 1 1 d . . . H24A H 0.4657 -0.1807 0.4755 0.195 Uiso 1 1 calc R . . H24B H 0.3852 -0.1065 0.4964 0.195 Uiso 1 1 calc R . . H24C H 0.4800 -0.0945 0.4276 0.195 Uiso 1 1 calc R . . C25 C 0.2571(8) -0.2200(5) 0.4106(7) 0.102(3) Uani 1 1 d . . . H25A H 0.2960 -0.2649 0.4420 0.153 Uiso 1 1 calc R . . H25B H 0.2088 -0.2420 0.3617 0.153 Uiso 1 1 calc R . . H25C H 0.2123 -0.1903 0.4521 0.153 Uiso 1 1 calc R . . C26 C 0.4063(8) -0.2108(6) 0.3050(7) 0.103(3) Uani 1 1 d . . . H26A H 0.4497 -0.2535 0.3366 0.155 Uiso 1 1 calc R . . H26B H 0.4561 -0.1750 0.2738 0.155 Uiso 1 1 calc R . . H26C H 0.3530 -0.2361 0.2617 0.155 Uiso 1 1 calc R . . C30 C 0.1506(6) -0.1803(5) 0.0890(5) 0.070(2) Uani 1 1 d . . . O30 O 0.1597(6) -0.2114(5) 0.0214(4) 0.129(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0380(3) 0.0647(4) 0.0426(3) -0.0085(2) 0.00073(18) -0.0008(2) P1 0.0341(7) 0.0677(11) 0.0437(8) -0.0065(7) 0.0003(6) -0.0033(7) C2 0.046(3) 0.070(4) 0.047(3) -0.004(3) 0.008(3) -0.006(3) C3 0.051(4) 0.068(4) 0.053(4) -0.002(3) 0.003(3) 0.006(3) C4 0.061(4) 0.067(4) 0.044(4) -0.006(3) -0.002(3) -0.001(3) C5 0.072(5) 0.068(5) 0.078(5) -0.014(4) 0.002(4) -0.006(4) C6 0.087(5) 0.050(4) 0.078(5) -0.011(4) 0.010(4) 0.000(4) C7 0.096(6) 0.050(4) 0.066(5) -0.010(3) 0.014(4) 0.022(4) C8 0.060(4) 0.088(6) 0.066(5) -0.008(4) 0.000(3) 0.013(4) C9 0.052(4) 0.083(5) 0.061(4) -0.006(4) -0.003(3) 0.010(4) C10 0.053(4) 0.134(8) 0.106(7) 0.005(6) -0.001(4) 0.034(5) C11 0.094(6) 0.089(6) 0.074(5) 0.019(4) 0.000(4) 0.007(5) C12 0.106(7) 0.117(7) 0.064(5) -0.009(5) -0.026(4) 0.017(6) C13 0.049(4) 0.085(5) 0.071(5) -0.003(4) 0.003(3) -0.015(3) C14 0.060(5) 0.127(8) 0.168(10) 0.001(7) 0.052(6) -0.024(5) C15 0.094(6) 0.090(6) 0.102(7) -0.039(5) -0.009(5) -0.031(5) C16 0.106(7) 0.082(6) 0.109(7) 0.017(5) -0.010(5) -0.021(5) C17 0.055(4) 0.063(4) 0.048(4) -0.013(3) -0.008(3) 0.010(3) P18 0.0348(7) 0.0576(10) 0.0481(9) -0.0074(7) -0.0040(6) 0.0001(7) C19 0.050(4) 0.077(5) 0.080(5) 0.005(4) -0.002(3) -0.011(4) C20 0.075(6) 0.129(8) 0.126(8) 0.011(7) 0.042(5) -0.009(5) C21 0.094(6) 0.088(6) 0.102(7) 0.016(5) 0.027(5) -0.014(5) C22 0.106(7) 0.130(8) 0.117(8) 0.010(6) -0.029(6) -0.069(6) C23 0.057(4) 0.060(4) 0.064(4) -0.003(3) -0.012(3) 0.006(3) C24 0.135(9) 0.110(8) 0.132(9) -0.016(6) -0.089(7) 0.021(6) C25 0.107(7) 0.083(6) 0.116(8) 0.024(5) 0.003(6) 0.008(5) C26 0.093(6) 0.095(7) 0.123(8) -0.001(6) 0.016(5) 0.053(5) C30 0.060(4) 0.091(6) 0.057(4) -0.016(4) -0.004(3) 0.018(4) O30 0.156(6) 0.163(7) 0.067(4) -0.044(4) -0.006(4) 0.056(5) _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 C30 1.872(7) . ? Pd1 P1 2.3446(16) . ? Pd1 P18 2.3551(15) . ? P1 C2 1.857(6) . ? P1 C13 1.898(7) . ? P1 C9 1.901(7) . ? C2 C3 1.547(9) . ? C3 C8 1.414(9) . ? C3 C4 1.415(8) . ? C4 C5 1.402(9) . ? C4 C17 1.534(9) . ? C5 C6 1.370(10) . ? C6 C7 1.353(10) . ? C7 C8 1.338(10) . ? C9 C11 1.527(10) . ? C9 C10 1.533(9) . ? C9 C12 1.543(10) . ? C13 C14 1.519(10) . ? C13 C15 1.534(10) . ? C13 C16 1.540(11) . ? C17 P18 1.862(6) . ? P18 C23 1.888(7) . ? P18 C19 1.888(7) . ? C19 C21 1.522(11) . ? C19 C20 1.529(11) . ? C19 C22 1.542(11) . ? C23 C26 1.503(10) . ? C23 C24 1.530(10) . ? C23 C25 1.533(11) . ? C30 O30 1.126(8) . ? 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 C30 Pd1 P1 122.7(2) . . ? C30 Pd1 P18 130.1(2) . . ? P1 Pd1 P18 107.26(6) . . ? C2 P1 C13 99.7(3) . . ? C2 P1 C9 105.1(3) . . ? C13 P1 C9 111.6(3) . . ? C2 P1 Pd1 116.0(2) . . ? C13 P1 Pd1 111.4(2) . . ? C9 P1 Pd1 112.2(2) . . ? C3 C2 P1 119.8(4) . . ? C8 C3 C4 117.1(6) . . ? C8 C3 C2 119.3(6) . . ? C4 C3 C2 123.5(6) . . ? C5 C4 C3 117.7(6) . . ? C5 C4 C17 118.8(6) . . ? C3 C4 C17 122.9(6) . . ? C6 C5 C4 121.1(7) . . ? C7 C6 C5 122.0(7) . . ? C8 C7 C6 118.1(7) . . ? C7 C8 C3 124.0(7) . . ? C11 C9 C10 109.8(7) . . ? C11 C9 C12 106.1(7) . . ? C10 C9 C12 109.3(6) . . ? C11 C9 P1 105.4(5) . . ? C10 C9 P1 116.2(5) . . ? C12 C9 P1 109.5(5) . . ? C14 C13 C15 109.9(7) . . ? C14 C13 C16 109.5(7) . . ? C15 C13 C16 105.6(7) . . ? C14 C13 P1 115.9(6) . . ? C15 C13 P1 110.0(5) . . ? C16 C13 P1 105.4(5) . . ? C4 C17 P18 120.5(4) . . ? C17 P18 C23 99.9(3) . . ? C17 P18 C19 105.4(3) . . ? C23 P18 C19 110.5(3) . . ? C17 P18 Pd1 115.6(2) . . ? C23 P18 Pd1 113.7(2) . . ? C19 P18 Pd1 111.0(2) . . ? C21 C19 C20 105.9(7) . . ? C21 C19 C22 109.7(7) . . ? C20 C19 C22 109.3(7) . . ? C21 C19 P18 106.2(5) . . ? C20 C19 P18 109.9(6) . . ? C22 C19 P18 115.4(6) . . ? C26 C23 C24 109.5(7) . . ? C26 C23 C25 106.0(7) . . ? C24 C23 C25 108.3(8) . . ? C26 C23 P18 110.5(5) . . ? C24 C23 P18 116.4(5) . . ? C25 C23 P18 105.4(5) . . ? O30 C30 Pd1 176.4(7) . . ? 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 C30 Pd1 P1 C2 176.7(4) . . . . ? P18 Pd1 P1 C2 -3.4(3) . . . . ? C30 Pd1 P1 C13 63.5(4) . . . . ? P18 Pd1 P1 C13 -116.6(2) . . . . ? C30 Pd1 P1 C9 -62.4(4) . . . . ? P18 Pd1 P1 C9 117.5(3) . . . . ? C13 P1 C2 C3 -179.5(5) . . . . ? C9 P1 C2 C3 -63.8(5) . . . . ? Pd1 P1 C2 C3 60.8(5) . . . . ? P1 C2 C3 C8 104.0(6) . . . . ? P1 C2 C3 C4 -79.4(7) . . . . ? C8 C3 C4 C5 0.0(9) . . . . ? C2 C3 C4 C5 -176.7(6) . . . . ? C8 C3 C4 C17 170.5(6) . . . . ? C2 C3 C4 C17 -6.1(9) . . . . ? C3 C4 C5 C6 -0.8(11) . . . . ? C17 C4 C5 C6 -171.7(7) . . . . ? C4 C5 C6 C7 -0.1(12) . . . . ? C5 C6 C7 C8 1.8(12) . . . . ? C6 C7 C8 C3 -2.7(11) . . . . ? C4 C3 C8 C7 1.8(11) . . . . ? C2 C3 C8 C7 178.7(7) . . . . ? C2 P1 C9 C11 75.3(5) . . . . ? C13 P1 C9 C11 -177.5(5) . . . . ? Pd1 P1 C9 C11 -51.7(5) . . . . ? C2 P1 C9 C10 -46.5(7) . . . . ? C13 P1 C9 C10 60.7(7) . . . . ? Pd1 P1 C9 C10 -173.4(5) . . . . ? C2 P1 C9 C12 -170.9(5) . . . . ? C13 P1 C9 C12 -63.7(6) . . . . ? Pd1 P1 C9 C12 62.1(6) . . . . ? C2 P1 C13 C14 51.1(7) . . . . ? C9 P1 C13 C14 -59.6(7) . . . . ? Pd1 P1 C13 C14 174.2(6) . . . . ? C2 P1 C13 C15 176.6(5) . . . . ? C9 P1 C13 C15 65.9(6) . . . . ? Pd1 P1 C13 C15 -60.4(6) . . . . ? C2 P1 C13 C16 -70.1(6) . . . . ? C9 P1 C13 C16 179.3(5) . . . . ? Pd1 P1 C13 C16 53.0(6) . . . . ? C5 C4 C17 P18 -103.9(7) . . . . ? C3 C4 C17 P18 85.6(7) . . . . ? C4 C17 P18 C23 -178.7(5) . . . . ? C4 C17 P18 C19 66.8(6) . . . . ? C4 C17 P18 Pd1 -56.3(6) . . . . ? C30 Pd1 P18 C17 -179.8(4) . . . . ? P1 Pd1 P18 C17 0.3(3) . . . . ? C30 Pd1 P18 C23 -65.1(4) . . . . ? P1 Pd1 P18 C23 115.0(3) . . . . ? C30 Pd1 P18 C19 60.1(4) . . . . ? P1 Pd1 P18 C19 -119.8(3) . . . . ? C17 P18 C19 C21 -74.4(6) . . . . ? C23 P18 C19 C21 178.6(5) . . . . ? Pd1 P18 C19 C21 51.5(6) . . . . ? C17 P18 C19 C20 171.5(6) . . . . ? C23 P18 C19 C20 64.4(7) . . . . ? Pd1 P18 C19 C20 -62.6(6) . . . . ? C17 P18 C19 C22 47.4(7) . . . . ? C23 P18 C19 C22 -59.7(7) . . . . ? Pd1 P18 C19 C22 173.3(6) . . . . ? C17 P18 C23 C26 -178.7(6) . . . . ? C19 P18 C23 C26 -68.0(6) . . . . ? Pd1 P18 C23 C26 57.5(6) . . . . ? C17 P18 C23 C24 -53.1(8) . . . . ? C19 P18 C23 C24 57.6(8) . . . . ? Pd1 P18 C23 C24 -176.8(7) . . . . ? C17 P18 C23 C25 67.1(6) . . . . ? C19 P18 C23 C25 177.8(5) . . . . ? Pd1 P18 C23 C25 -56.7(6) . . . . ? P1 Pd1 C30 O30 25(14) . . . . ? P18 Pd1 C30 O30 -155(13) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.746 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.083