Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ronan Bellabarba' _publ_contact_author_address ; Sasol Technology UK Limited Purdie Building North Haugh St Andrews Fife Scotland KY16 9ST UNITED KINGDOM ; _publ_contact_author_email RONAN.BELLABARBA@UK.SASOL.COM _publ_section_title ; 1,8-dimethylnapthalene-bridged diphosphine ligands: synthesis and structural comparison of their palladium complexes. ; loop_ _publ_author_name 'Ronan Bellabarba' 'Grant S. Forman' 'Colin Hammond' 'A. Slawin' 'Robert P. Tooze' # Attachment '10_Sasol49_Pd_Napth(iPr2)P_Cl2.CIF' data_sasol49 _database_code_depnum_ccdc_archive 'CCDC 295570' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 Cl2 P2 Pd' _chemical_formula_sum 'C24 H38 Cl2 P2 Pd' _chemical_formula_weight 565.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.743(3) _cell_length_b 15.594(3) _cell_length_c 19.512(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5094.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 13025 _cell_measurement_theta_min 1.6718 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6889 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocol _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24175 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4467 _reflns_number_gt 3846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+20.0000P] 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 idealised _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 4467 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.55464(3) 0.25355(3) 0.68051(2) 0.01925(17) Uani 1 1 d . . . Cl1 Cl 0.54654(16) 0.29258(15) 0.79648(9) 0.0652(8) Uani 1 1 d . . . Cl2 Cl 0.62557(11) 0.38393(10) 0.66356(7) 0.0287(4) Uani 1 1 d . . . P1 P 0.50436(11) 0.12546(12) 0.71596(7) 0.0260(4) Uani 1 1 d . . . C1 C 0.4878(4) 0.0330(4) 0.6591(3) 0.0237(14) Uani 1 1 d . . . H1A H 0.5325 0.0316 0.6259 0.028 Uiso 1 1 calc R . . H1B H 0.4922 -0.0194 0.6875 0.028 Uiso 1 1 calc R . . C2 C 0.4110(4) 0.0256(4) 0.6182(3) 0.0189(13) Uani 1 1 d . . . C3 C 0.3519(5) -0.0213(4) 0.6499(3) 0.0282(16) Uani 1 1 d . . . H3A H 0.3627 -0.0456 0.6936 0.034 Uiso 1 1 calc R . . C4 C 0.2762(5) -0.0347(4) 0.6207(3) 0.0307(17) Uani 1 1 d . . . H4A H 0.2367 -0.0666 0.6446 0.037 Uiso 1 1 calc R . . C5 C 0.2600(5) -0.0013(4) 0.5573(4) 0.0337(17) Uani 1 1 d . . . H5A H 0.2085 -0.0085 0.5377 0.040 Uiso 1 1 calc R . . C6 C 0.3198(4) 0.0441(4) 0.5208(3) 0.0258(15) Uani 1 1 d . . . C7 C 0.3014(4) 0.0705(4) 0.4537(3) 0.0287(16) Uani 1 1 d . . . H7A H 0.2494 0.0608 0.4358 0.034 Uiso 1 1 calc R . . C8 C 0.3580(5) 0.1104(4) 0.4138(3) 0.0298(17) Uani 1 1 d . . . H8A H 0.3456 0.1282 0.3685 0.036 Uiso 1 1 calc R . . C9 C 0.4341(4) 0.1245(4) 0.4410(3) 0.0261(15) Uani 1 1 d . . . H9A H 0.4732 0.1507 0.4126 0.031 Uiso 1 1 calc R . . C10 C 0.4556(4) 0.1021(4) 0.5074(3) 0.0214(14) Uani 1 1 d . . . C11 C 0.3976(4) 0.0593(4) 0.5499(3) 0.0182(13) Uani 1 1 d . . . C12 C 0.5392(4) 0.1255(4) 0.5265(3) 0.0201(13) Uani 1 1 d . . . H12A H 0.5722 0.1215 0.4845 0.024 Uiso 1 1 calc R . . H12B H 0.5590 0.0813 0.5586 0.024 Uiso 1 1 calc R . . P12 P 0.55827(11) 0.23181(10) 0.56583(7) 0.0215(4) Uani 1 1 d . . . C13 C 0.4079(6) 0.1317(6) 0.7628(3) 0.052(3) Uani 1 1 d . . . H13A H 0.3803 0.0758 0.7546 0.062 Uiso 1 1 calc R . . C14 C 0.3554(6) 0.2000(7) 0.7308(6) 0.075(4) Uani 1 1 d . . . H14A H 0.3046 0.2028 0.7556 0.113 Uiso 1 1 calc R . . H14B H 0.3454 0.1856 0.6827 0.113 Uiso 1 1 calc R . . H14C H 0.3824 0.2556 0.7335 0.113 Uiso 1 1 calc R . . C15 C 0.4146(7) 0.1412(7) 0.8417(4) 0.091(5) Uani 1 1 d . . . H15A H 0.3610 0.1445 0.8616 0.137 Uiso 1 1 calc R . . H15B H 0.4442 0.1937 0.8527 0.137 Uiso 1 1 calc R . . H15C H 0.4428 0.0915 0.8606 0.137 Uiso 1 1 calc R . . C16 C 0.5821(6) 0.0822(6) 0.7738(4) 0.059(3) Uani 1 1 d . . . H16A H 0.5849 0.1210 0.8146 0.071 Uiso 1 1 calc R . . C17 C 0.5653(6) -0.0093(7) 0.8007(5) 0.072(4) Uani 1 1 d . . . H17A H 0.6090 -0.0274 0.8309 0.108 Uiso 1 1 calc R . . H17B H 0.5613 -0.0490 0.7619 0.108 Uiso 1 1 calc R . . H17C H 0.5150 -0.0095 0.8264 0.108 Uiso 1 1 calc R . . C18 C 0.6627(6) 0.0861(8) 0.7383(6) 0.101(5) Uani 1 1 d . . . H18A H 0.7040 0.0636 0.7691 0.152 Uiso 1 1 calc R . . H18B H 0.6751 0.1457 0.7265 0.152 Uiso 1 1 calc R . . H18C H 0.6610 0.0514 0.6964 0.152 Uiso 1 1 calc R . . C19 C 0.4854(6) 0.3024(4) 0.5229(3) 0.046(2) Uani 1 1 d . . . H19A H 0.4762 0.2785 0.4760 0.055 Uiso 1 1 calc R . . C20 C 0.4059(6) 0.3005(6) 0.5602(4) 0.063(3) Uani 1 1 d . . . H20A H 0.3680 0.3385 0.5368 0.095 Uiso 1 1 calc R . . H20B H 0.4134 0.3200 0.6075 0.095 Uiso 1 1 calc R . . H20C H 0.3849 0.2418 0.5603 0.095 Uiso 1 1 calc R . . C21 C 0.5158(8) 0.3958(5) 0.5137(4) 0.080(4) Uani 1 1 d . . . H21A H 0.4746 0.4301 0.4909 0.119 Uiso 1 1 calc R . . H21B H 0.5644 0.3957 0.4858 0.119 Uiso 1 1 calc R . . H21C H 0.5275 0.4207 0.5588 0.119 Uiso 1 1 calc R . . C22 C 0.6582(5) 0.2572(4) 0.5323(3) 0.0354(19) Uani 1 1 d . . . H22A H 0.6692 0.3180 0.5455 0.043 Uiso 1 1 calc R . . C23 C 0.6641(6) 0.2536(5) 0.4523(4) 0.057(3) Uani 1 1 d . . . H23A H 0.7187 0.2675 0.4381 0.085 Uiso 1 1 calc R . . H23B H 0.6269 0.2952 0.4323 0.085 Uiso 1 1 calc R . . H23C H 0.6503 0.1958 0.4365 0.085 Uiso 1 1 calc R . . C24 C 0.7221(5) 0.2037(5) 0.5666(4) 0.042(2) Uani 1 1 d . . . H24A H 0.7745 0.2188 0.5476 0.063 Uiso 1 1 calc R . . H24B H 0.7115 0.1427 0.5583 0.063 Uiso 1 1 calc R . . H24C H 0.7218 0.2148 0.6160 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0228(3) 0.0218(3) 0.0132(3) -0.00397(16) 0.00434(17) -0.0010(2) Cl1 0.102(2) 0.0748(15) 0.0190(8) -0.0205(9) 0.0220(10) -0.0620(15) Cl2 0.0475(11) 0.0152(8) 0.0235(8) -0.0036(6) 0.0096(7) -0.0012(7) P1 0.0312(10) 0.0349(10) 0.0118(7) 0.0028(6) 0.0007(6) -0.0138(8) C1 0.028(4) 0.026(4) 0.017(3) 0.006(2) -0.004(3) 0.006(3) C2 0.024(4) 0.014(3) 0.019(3) -0.006(2) -0.002(2) 0.001(3) C3 0.047(5) 0.017(3) 0.021(3) -0.003(2) 0.000(3) -0.005(3) C4 0.034(5) 0.023(4) 0.035(4) -0.010(3) 0.009(3) -0.010(3) C5 0.033(4) 0.027(4) 0.041(4) -0.012(3) 0.000(3) -0.004(3) C6 0.036(4) 0.016(3) 0.026(3) -0.011(2) -0.003(3) 0.009(3) C7 0.031(4) 0.022(3) 0.034(3) -0.005(3) -0.015(3) 0.015(3) C8 0.046(5) 0.023(4) 0.021(3) 0.002(3) -0.011(3) 0.013(3) C9 0.040(4) 0.023(3) 0.015(3) 0.001(2) 0.004(3) 0.006(3) C10 0.031(4) 0.014(3) 0.020(3) -0.007(2) -0.001(3) 0.012(3) C11 0.027(4) 0.011(3) 0.017(3) -0.003(2) 0.003(2) 0.002(3) C12 0.027(4) 0.016(3) 0.018(3) 0.000(2) 0.001(2) 0.003(3) P12 0.0379(11) 0.0143(8) 0.0121(7) -0.0007(5) 0.0031(6) 0.0035(7) C13 0.057(6) 0.066(6) 0.033(4) -0.033(4) 0.031(4) -0.047(5) C14 0.039(6) 0.066(7) 0.120(9) -0.041(7) 0.038(6) -0.020(5) C15 0.127(10) 0.108(9) 0.039(5) -0.047(5) 0.052(6) -0.087(8) C16 0.059(6) 0.070(6) 0.048(5) 0.043(4) -0.033(4) -0.045(5) C17 0.057(6) 0.089(7) 0.069(6) 0.065(5) -0.042(5) -0.050(6) C18 0.040(6) 0.109(9) 0.155(11) 0.109(9) -0.053(7) -0.048(6) C19 0.095(8) 0.017(4) 0.027(4) -0.004(3) -0.028(4) 0.028(4) C20 0.072(7) 0.046(5) 0.072(6) -0.038(4) -0.051(5) 0.049(5) C21 0.177(13) 0.010(4) 0.052(5) -0.001(3) -0.045(6) 0.015(5) C22 0.057(5) 0.023(4) 0.027(3) -0.010(3) 0.025(3) -0.018(4) C23 0.105(8) 0.039(5) 0.026(4) -0.008(3) 0.035(4) -0.028(5) C24 0.036(5) 0.043(5) 0.047(4) -0.019(4) 0.021(4) -0.011(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 Pd1 P12 2.2641(14) . ? Pd1 P1 2.2753(18) . ? Pd1 Cl1 2.3470(16) . ? Pd1 Cl2 2.3777(17) . ? P1 C1 1.841(6) . ? P1 C16 1.850(8) . ? P1 C13 1.858(8) . ? C1 C2 1.516(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.378(9) . ? C2 C11 1.449(8) . ? C3 C4 1.405(10) . ? C3 H3A 0.9500 . ? C4 C5 1.369(10) . ? C4 H4A 0.9500 . ? C5 C6 1.418(10) . ? C5 H5A 0.9500 . ? C6 C7 1.407(9) . ? C6 C11 1.440(9) . ? C7 C8 1.375(10) . ? C7 H7A 0.9500 . ? C8 C9 1.398(10) . ? C8 H8A 0.9500 . ? C9 C10 1.388(8) . ? C9 H9A 0.9500 . ? C10 C11 1.442(9) . ? C10 C12 1.494(9) . ? C12 P12 1.855(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? P12 C22 1.840(7) . ? P12 C19 1.844(7) . ? C13 C14 1.516(14) . ? C13 C15 1.550(10) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.518(14) . ? C16 C17 1.546(11) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(13) . ? C19 C21 1.553(12) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.513(11) . ? C22 C23 1.564(9) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P12 Pd1 P1 100.31(6) . . ? P12 Pd1 Cl1 173.33(8) . . ? P1 Pd1 Cl1 85.02(6) . . ? P12 Pd1 Cl2 88.69(6) . . ? P1 Pd1 Cl2 167.89(6) . . ? Cl1 Pd1 Cl2 86.63(6) . . ? C1 P1 C16 100.9(4) . . ? C1 P1 C13 101.9(3) . . ? C16 P1 C13 109.3(4) . . ? C1 P1 Pd1 124.1(2) . . ? C16 P1 Pd1 104.2(3) . . ? C13 P1 Pd1 115.2(3) . . ? C2 C1 P1 120.3(4) . . ? C2 C1 H1A 107.3 . . ? P1 C1 H1A 107.3 . . ? C2 C1 H1B 107.2 . . ? P1 C1 H1B 107.3 . . ? H1A C1 H1B 106.9 . . ? C3 C2 C11 119.5(6) . . ? C3 C2 C1 114.4(5) . . ? C11 C2 C1 126.0(6) . . ? C2 C3 C4 123.0(6) . . ? C2 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? C5 C4 C3 119.2(7) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 120.3(7) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 117.3(7) . . ? C7 C6 C11 121.2(6) . . ? C5 C6 C11 121.5(6) . . ? C8 C7 C6 120.5(7) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 119.0(6) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? C10 C9 C8 123.4(6) . . ? C10 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? C9 C10 C11 118.7(6) . . ? C9 C10 C12 114.4(6) . . ? C11 C10 C12 126.9(5) . . ? C10 C11 C6 117.2(5) . . ? C10 C11 C2 126.4(6) . . ? C6 C11 C2 116.3(6) . . ? C10 C12 P12 118.9(4) . . ? C10 C12 H12A 107.6 . . ? P12 C12 H12A 107.6 . . ? C10 C12 H12B 107.6 . . ? P12 C12 H12B 107.6 . . ? H12A C12 H12B 107.0 . . ? C22 P12 C19 108.2(4) . . ? C22 P12 C12 101.6(3) . . ? C19 P12 C12 103.4(3) . . ? C22 P12 Pd1 110.1(2) . . ? C19 P12 Pd1 110.0(2) . . ? C12 P12 Pd1 122.58(19) . . ? C14 C13 C15 112.5(9) . . ? C14 C13 P1 109.7(6) . . ? C15 C13 P1 115.6(7) . . ? C14 C13 H13A 106.1 . . ? C15 C13 H13A 106.1 . . ? P1 C13 H13A 106.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 110.7(10) . . ? C18 C16 P1 109.4(5) . . ? C17 C16 P1 114.6(6) . . ? C18 C16 H16A 107.3 . . ? C17 C16 H16A 107.3 . . ? P1 C16 H16A 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 111.1(8) . . ? C20 C19 P12 110.5(5) . . ? C21 C19 P12 113.3(7) . . ? C20 C19 H19A 107.2 . . ? C21 C19 H19A 107.2 . . ? P12 C19 H19A 107.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 112.1(6) . . ? C24 C22 P12 111.6(5) . . ? C23 C22 P12 113.8(6) . . ? C24 C22 H22A 106.2 . . ? C23 C22 H22A 106.2 . . ? P12 C22 H22A 106.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P12 Pd1 P1 C1 6.7(3) . . . . ? Cl1 Pd1 P1 C1 -177.4(3) . . . . ? Cl2 Pd1 P1 C1 -130.8(3) . . . . ? P12 Pd1 P1 C16 120.6(4) . . . . ? Cl1 Pd1 P1 C16 -63.4(4) . . . . ? Cl2 Pd1 P1 C16 -16.9(5) . . . . ? P12 Pd1 P1 C13 -119.7(3) . . . . ? Cl1 Pd1 P1 C13 56.2(3) . . . . ? Cl2 Pd1 P1 C13 102.8(4) . . . . ? C16 P1 C1 C2 159.5(5) . . . . ? C13 P1 C1 C2 46.9(6) . . . . ? Pd1 P1 C1 C2 -85.0(5) . . . . ? P1 C1 C2 C3 -93.2(6) . . . . ? P1 C1 C2 C11 89.8(7) . . . . ? C11 C2 C3 C4 -3.5(9) . . . . ? C1 C2 C3 C4 179.3(6) . . . . ? C2 C3 C4 C5 1.1(10) . . . . ? C3 C4 C5 C6 1.9(10) . . . . ? C4 C5 C6 C7 174.8(6) . . . . ? C4 C5 C6 C11 -2.5(10) . . . . ? C5 C6 C7 C8 -176.2(6) . . . . ? C11 C6 C7 C8 1.1(9) . . . . ? C6 C7 C8 C9 -0.1(10) . . . . ? C7 C8 C9 C10 -1.6(10) . . . . ? C8 C9 C10 C11 2.3(9) . . . . ? C8 C9 C10 C12 -178.1(6) . . . . ? C9 C10 C11 C6 -1.3(8) . . . . ? C12 C10 C11 C6 179.2(5) . . . . ? C9 C10 C11 C2 175.1(6) . . . . ? C12 C10 C11 C2 -4.4(9) . . . . ? C7 C6 C11 C10 -0.4(8) . . . . ? C5 C6 C11 C10 176.8(6) . . . . ? C7 C6 C11 C2 -177.1(5) . . . . ? C5 C6 C11 C2 0.1(8) . . . . ? C3 C2 C11 C10 -173.6(6) . . . . ? C1 C2 C11 C10 3.2(9) . . . . ? C3 C2 C11 C6 2.8(8) . . . . ? C1 C2 C11 C6 179.6(6) . . . . ? C9 C10 C12 P12 90.4(6) . . . . ? C11 C10 C12 P12 -90.1(7) . . . . ? C10 C12 P12 C22 -146.9(5) . . . . ? C10 C12 P12 C19 -34.9(6) . . . . ? C10 C12 P12 Pd1 89.8(5) . . . . ? P1 Pd1 P12 C22 -128.2(3) . . . . ? Cl1 Pd1 P12 C22 89.1(7) . . . . ? Cl2 Pd1 P12 C22 43.6(3) . . . . ? P1 Pd1 P12 C19 112.7(3) . . . . ? Cl1 Pd1 P12 C19 -30.0(8) . . . . ? Cl2 Pd1 P12 C19 -75.5(3) . . . . ? P1 Pd1 P12 C12 -9.0(3) . . . . ? Cl1 Pd1 P12 C12 -151.7(7) . . . . ? Cl2 Pd1 P12 C12 162.9(3) . . . . ? C1 P1 C13 C14 -99.0(6) . . . . ? C16 P1 C13 C14 154.8(6) . . . . ? Pd1 P1 C13 C14 38.0(6) . . . . ? C1 P1 C13 C15 132.4(7) . . . . ? C16 P1 C13 C15 26.3(9) . . . . ? Pd1 P1 C13 C15 -90.5(8) . . . . ? C1 P1 C16 C18 79.3(8) . . . . ? C13 P1 C16 C18 -173.9(7) . . . . ? Pd1 P1 C16 C18 -50.3(8) . . . . ? C1 P1 C16 C17 -45.7(9) . . . . ? C13 P1 C16 C17 61.2(9) . . . . ? Pd1 P1 C16 C17 -175.2(7) . . . . ? C22 P12 C19 C20 -166.0(5) . . . . ? C12 P12 C19 C20 86.8(5) . . . . ? Pd1 P12 C19 C20 -45.7(6) . . . . ? C22 P12 C19 C21 -40.5(7) . . . . ? C12 P12 C19 C21 -147.8(6) . . . . ? Pd1 P12 C19 C21 79.8(6) . . . . ? C19 P12 C22 C24 178.3(5) . . . . ? C12 P12 C22 C24 -73.3(5) . . . . ? Pd1 P12 C22 C24 58.1(5) . . . . ? C19 P12 C22 C23 -53.6(6) . . . . ? C12 P12 C22 C23 54.8(6) . . . . ? Pd1 P12 C22 C23 -173.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.936 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.138 # Attachment '11_CyclohexPnapth_Cl2A.cif' data_sasol42 _database_code_depnum_ccdc_archive 'CCDC 295571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 Cl2 P2 Pd.(C H2 Cl2)1.5' _chemical_formula_sum 'C37.50 H57 Cl5 P2 Pd' _chemical_formula_weight 853.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.898(3) _cell_length_b 17.223(4) _cell_length_c 18.723(4) _cell_angle_alpha 83.18(2) _cell_angle_beta 76.28(2) _cell_angle_gamma 79.56(2) _cell_volume 3960.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11524 _cell_measurement_theta_min 2.1874 _cell_measurement_theta_max 25.3491 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.4271 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24442 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.1733 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13631 _reflns_number_gt 7840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+27.5718P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 13631 _refine_ls_number_parameters 830 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1806 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.2592 _refine_ls_wR_factor_gt 0.2094 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 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 0.64621(7) 0.26666(5) 0.78606(4) 0.0244(2) Uani 1 1 d . . . Cl1 Cl 0.8035(2) 0.18057(17) 0.73497(16) 0.0344(7) Uani 1 1 d . . . Cl2 Cl 0.5576(2) 0.21633(18) 0.70929(16) 0.0362(8) Uani 1 1 d . . . P1 P 0.7427(2) 0.29699(17) 0.86301(15) 0.0241(7) Uani 1 1 d . . . C1 C 0.6649(11) 0.3532(6) 0.9441(6) 0.036(3) Uani 1 1 d . . . H1A H 0.5880 0.3468 0.9530 0.043 Uiso 1 1 calc R . . H1B H 0.6919 0.3292 0.9883 0.043 Uiso 1 1 calc R . . C2 C 0.6716(9) 0.4411(7) 0.9355(6) 0.028(3) Uani 1 1 d . . . C3 C 0.7567(11) 0.4598(8) 0.9607(7) 0.045(4) Uani 1 1 d . . . H3A H 0.7977 0.4195 0.9865 0.054 Uiso 1 1 calc R . . C4 C 0.7832(11) 0.5350(9) 0.9492(8) 0.052(4) Uani 1 1 d . . . H4A H 0.8425 0.5453 0.9666 0.062 Uiso 1 1 calc R . . C5 C 0.7271(11) 0.5937(8) 0.9140(7) 0.044(4) Uani 1 1 d . . . H5A H 0.7491 0.6444 0.9040 0.053 Uiso 1 1 calc R . . C6 C 0.6329(11) 0.5802(8) 0.8911(7) 0.042(3) Uani 1 1 d . . . C7 C 0.5701(13) 0.6425(7) 0.8588(7) 0.050(4) Uani 1 1 d . . . H7A H 0.5914 0.6934 0.8518 0.060 Uiso 1 1 calc R . . C8 C 0.4800(13) 0.6344(7) 0.8368(7) 0.049(4) Uani 1 1 d . . . H8A H 0.4402 0.6776 0.8132 0.059 Uiso 1 1 calc R . . C9 C 0.4486(12) 0.5595(7) 0.8504(7) 0.044(4) Uani 1 1 d . . . H9A H 0.3838 0.5535 0.8375 0.053 Uiso 1 1 calc R . . C10 C 0.5051(10) 0.4947(7) 0.8810(6) 0.032(3) Uani 1 1 d . . . C11 C 0.6030(9) 0.5026(7) 0.9019(5) 0.028(3) Uani 1 1 d . . . C12 C 0.4551(10) 0.4206(7) 0.8947(6) 0.035(3) Uani 1 1 d . . . H12A H 0.3758 0.4372 0.9071 0.042 Uiso 1 1 calc R . . H12B H 0.4751 0.3916 0.9397 0.042 Uiso 1 1 calc R . . P12 P 0.4844(2) 0.34670(17) 0.82337(15) 0.0262(7) Uani 1 1 d . . . C13 C 0.8528(9) 0.3510(6) 0.8147(6) 0.028(3) Uani 1 1 d . . . H13A H 0.8663 0.3833 0.8517 0.034 Uiso 1 1 calc R . . C14 C 0.8192(10) 0.4092(7) 0.7536(6) 0.037(3) Uani 1 1 d . . . H14A H 0.7517 0.4442 0.7746 0.044 Uiso 1 1 calc R . . H14B H 0.8036 0.3793 0.7164 0.044 Uiso 1 1 calc R . . C15 C 0.9045(10) 0.4598(7) 0.7157(8) 0.044(3) Uani 1 1 d . . . H15A H 0.9144 0.4946 0.7512 0.053 Uiso 1 1 calc R . . H15B H 0.8800 0.4939 0.6745 0.053 Uiso 1 1 calc R . . C16 C 1.0136(10) 0.4072(8) 0.6857(7) 0.042(3) Uani 1 1 d . . . H16A H 1.0059 0.3771 0.6459 0.050 Uiso 1 1 calc R . . H16B H 1.0695 0.4412 0.6646 0.050 Uiso 1 1 calc R . . C17 C 1.0490(9) 0.3500(7) 0.7464(7) 0.039(3) Uani 1 1 d . . . H17A H 1.0638 0.3802 0.7837 0.046 Uiso 1 1 calc R . . H17B H 1.1167 0.3152 0.7255 0.046 Uiso 1 1 calc R . . C18 C 0.9622(9) 0.2991(7) 0.7836(7) 0.032(3) Uani 1 1 d . . . H18A H 0.9867 0.2640 0.8243 0.038 Uiso 1 1 calc R . . H18B H 0.9522 0.2653 0.7473 0.038 Uiso 1 1 calc R . . C19 C 0.8062(10) 0.2056(6) 0.9078(6) 0.031(3) Uani 1 1 d . . . H19A H 0.8612 0.1783 0.8677 0.037 Uiso 1 1 calc R . . C20 C 0.8681(10) 0.2176(7) 0.9658(6) 0.032(3) Uani 1 1 d . . . H20A H 0.9210 0.2536 0.9438 0.039 Uiso 1 1 calc R . . H20B H 0.8166 0.2424 1.0081 0.039 Uiso 1 1 calc R . . C21 C 0.9266(9) 0.1392(7) 0.9924(7) 0.034(3) Uani 1 1 d . . . H21A H 0.9837 0.1179 0.9509 0.040 Uiso 1 1 calc R . . H21B H 0.9623 0.1483 1.0313 0.040 Uiso 1 1 calc R . . C22 C 0.8540(11) 0.0786(7) 1.0225(6) 0.039(3) Uani 1 1 d . . . H22A H 0.8038 0.0955 1.0688 0.046 Uiso 1 1 calc R . . H22B H 0.8980 0.0273 1.0340 0.046 Uiso 1 1 calc R . . C23 C 0.7900(11) 0.0686(7) 0.9670(7) 0.037(3) Uani 1 1 d . . . H23A H 0.7378 0.0322 0.9896 0.045 Uiso 1 1 calc R . . H23B H 0.8400 0.0441 0.9239 0.045 Uiso 1 1 calc R . . C24 C 0.7272(11) 0.1487(7) 0.9400(7) 0.037(3) Uani 1 1 d . . . H24A H 0.6895 0.1396 0.9022 0.044 Uiso 1 1 calc R . . H24B H 0.6723 0.1715 0.9819 0.044 Uiso 1 1 calc R . . C25 C 0.4417(10) 0.4111(7) 0.7453(6) 0.035(3) Uani 1 1 d . . . H25A H 0.3975 0.4600 0.7673 0.042 Uiso 1 1 calc R . . C26 C 0.3700(10) 0.3804(7) 0.7029(6) 0.035(3) Uani 1 1 d . . . H26A H 0.4114 0.3340 0.6765 0.042 Uiso 1 1 calc R . . H26B H 0.3061 0.3635 0.7380 0.042 Uiso 1 1 calc R . . C27 C 0.3337(10) 0.4458(8) 0.6479(6) 0.040(3) Uani 1 1 d . . . H27A H 0.2875 0.4260 0.6211 0.048 Uiso 1 1 calc R . . H27B H 0.2897 0.4909 0.6750 0.048 Uiso 1 1 calc R . . C28 C 0.4272(10) 0.4742(7) 0.5932(6) 0.042(3) Uani 1 1 d . . . H28A H 0.3997 0.5183 0.5601 0.050 Uiso 1 1 calc R . . H28B H 0.4673 0.4306 0.5627 0.050 Uiso 1 1 calc R . . C29 C 0.5045(10) 0.5028(7) 0.6324(6) 0.035(3) Uani 1 1 d . . . H29A H 0.4680 0.5517 0.6565 0.042 Uiso 1 1 calc R . . H29B H 0.5693 0.5155 0.5955 0.042 Uiso 1 1 calc R . . C30 C 0.5395(9) 0.4384(7) 0.6911(7) 0.031(3) Uani 1 1 d . . . H30A H 0.5852 0.3925 0.6661 0.037 Uiso 1 1 calc R . . H30B H 0.5834 0.4600 0.7185 0.037 Uiso 1 1 calc R . . C31 C 0.3824(9) 0.2820(6) 0.8628(6) 0.026(3) Uani 1 1 d . . . H31A H 0.3777 0.2518 0.8215 0.031 Uiso 1 1 calc R . . C32 C 0.4186(10) 0.2194(7) 0.9222(6) 0.033(3) Uani 1 1 d . . . H32A H 0.4918 0.1911 0.9021 0.039 Uiso 1 1 calc R . . H32B H 0.4220 0.2461 0.9654 0.039 Uiso 1 1 calc R . . C33 C 0.3401(10) 0.1605(8) 0.9462(7) 0.040(3) Uani 1 1 d . . . H33A H 0.3611 0.1238 0.9871 0.048 Uiso 1 1 calc R . . H33B H 0.3444 0.1288 0.9045 0.048 Uiso 1 1 calc R . . C34 C 0.2239(11) 0.2020(8) 0.9715(7) 0.046(4) Uani 1 1 d . . . H34A H 0.1749 0.1620 0.9818 0.055 Uiso 1 1 calc R . . H34B H 0.2174 0.2262 1.0180 0.055 Uiso 1 1 calc R . . C35 C 0.1880(9) 0.2658(8) 0.9152(6) 0.035(3) Uani 1 1 d . . . H35A H 0.1839 0.2412 0.8710 0.042 Uiso 1 1 calc R . . H35B H 0.1151 0.2940 0.9364 0.042 Uiso 1 1 calc R . . C36 C 0.2665(9) 0.3238(7) 0.8935(6) 0.032(3) Uani 1 1 d . . . H36A H 0.2659 0.3514 0.9371 0.038 Uiso 1 1 calc R . . H36B H 0.2435 0.3641 0.8557 0.038 Uiso 1 1 calc R . . Pd41 Pd 0.78829(7) 0.18994(5) 0.31567(5) 0.0284(3) Uani 1 1 d . . . Cl41 Cl 0.6749(3) 0.31339(19) 0.31042(17) 0.0529(10) Uani 1 1 d . . . Cl42 Cl 0.8034(3) 0.19516(17) 0.18611(15) 0.0358(7) Uani 1 1 d . . . P41 P 0.7617(2) 0.20030(17) 0.43912(16) 0.0270(7) Uani 1 1 d . . . C41 C 0.8399(10) 0.1348(6) 0.4998(6) 0.031(3) Uani 1 1 d . . . H41A H 0.9160 0.1253 0.4720 0.037 Uiso 1 1 calc R . . H41B H 0.8383 0.1648 0.5420 0.037 Uiso 1 1 calc R . . C42 C 0.8090(10) 0.0543(7) 0.5313(6) 0.034(3) Uani 1 1 d . . . C43 C 0.7374(10) 0.0554(7) 0.5984(6) 0.036(3) Uani 1 1 d . . . H43A H 0.7130 0.1044 0.6201 0.043 Uiso 1 1 calc R . . C44 C 0.6974(10) -0.0138(7) 0.6374(6) 0.033(3) Uani 1 1 d . . . H44A H 0.6446 -0.0103 0.6824 0.039 Uiso 1 1 calc R . . C45 C 0.7362(10) -0.0830(7) 0.6087(6) 0.032(3) Uani 1 1 d . . . H45A H 0.7112 -0.1296 0.6341 0.038 Uiso 1 1 calc R . . C46 C 0.8160(9) -0.0894(6) 0.5393(6) 0.025(3) Uani 1 1 d . . . C47 C 0.8559(9) -0.1653(7) 0.5154(6) 0.029(3) Uani 1 1 d . . . H47A H 0.8299 -0.2102 0.5438 0.034 Uiso 1 1 calc R . . C48 C 0.9326(9) -0.1749(6) 0.4510(6) 0.026(3) Uani 1 1 d . . . H48A H 0.9605 -0.2261 0.4342 0.032 Uiso 1 1 calc R . . C49 C 0.9683(10) -0.1085(7) 0.4110(6) 0.033(3) Uani 1 1 d . . . H49A H 1.0220 -0.1158 0.3668 0.040 Uiso 1 1 calc R . . C50 C 0.9311(8) -0.0321(6) 0.4312(6) 0.025(3) Uani 1 1 d . . . C51 C 0.8521(9) -0.0198(6) 0.4999(6) 0.026(3) Uani 1 1 d . . . C52 C 0.9808(9) 0.0325(7) 0.3779(7) 0.038(3) Uani 1 1 d . . . H52A H 1.0558 0.0098 0.3549 0.045 Uiso 1 1 calc R . . H52B H 0.9852 0.0753 0.4074 0.045 Uiso 1 1 calc R . . P52 P 0.9140(2) 0.07813(17) 0.30332(16) 0.0254(7) Uani 1 1 d . . . C53 C 0.7918(9) 0.2970(6) 0.4540(6) 0.025(3) Uani 1 1 d . . . H53A H 0.7376 0.3374 0.4339 0.030 Uiso 1 1 calc R . . C54 C 0.7782(10) 0.3152(6) 0.5337(6) 0.030(3) Uani 1 1 d . . . H54A H 0.8307 0.2776 0.5568 0.037 Uiso 1 1 calc R . . H54B H 0.7045 0.3086 0.5617 0.037 Uiso 1 1 calc R . . C55 C 0.7964(9) 0.4007(6) 0.5369(6) 0.030(3) Uani 1 1 d . . . H55A H 0.7397 0.4384 0.5178 0.036 Uiso 1 1 calc R . . H55B H 0.7903 0.4108 0.5888 0.036 Uiso 1 1 calc R . . C56 C 0.9064(10) 0.4143(7) 0.4918(6) 0.034(3) Uani 1 1 d . . . H56A H 0.9631 0.3807 0.5142 0.041 Uiso 1 1 calc R . . H56B H 0.9140 0.4703 0.4927 0.041 Uiso 1 1 calc R . . C57 C 0.9228(11) 0.3948(6) 0.4110(6) 0.037(3) Uani 1 1 d . . . H57A H 0.8728 0.4333 0.3864 0.044 Uiso 1 1 calc R . . H57B H 0.9976 0.3997 0.3843 0.044 Uiso 1 1 calc R . . C58 C 0.9021(10) 0.3117(7) 0.4073(7) 0.039(3) Uani 1 1 d . . . H58A H 0.9595 0.2731 0.4247 0.047 Uiso 1 1 calc R . . H58B H 0.9061 0.3030 0.3554 0.047 Uiso 1 1 calc R . . C59 C 0.6206(9) 0.1929(6) 0.4884(6) 0.028(3) Uani 1 1 d . . . H59A H 0.6221 0.1758 0.5411 0.034 Uiso 1 1 calc R . . C60 C 0.5809(9) 0.1263(7) 0.4577(6) 0.031(3) Uani 1 1 d . . . H60A H 0.5775 0.1413 0.4055 0.037 Uiso 1 1 calc R . . H60B H 0.6332 0.0767 0.4596 0.037 Uiso 1 1 calc R . . C61 C 0.4695(10) 0.1119(7) 0.5021(7) 0.039(3) Uani 1 1 d . . . H61A H 0.4435 0.0729 0.4786 0.047 Uiso 1 1 calc R . . H61B H 0.4750 0.0896 0.5525 0.047 Uiso 1 1 calc R . . C62 C 0.3882(10) 0.1891(7) 0.5066(7) 0.041(3) Uani 1 1 d . . . H62A H 0.3188 0.1790 0.5395 0.049 Uiso 1 1 calc R . . H62B H 0.3747 0.2071 0.4569 0.049 Uiso 1 1 calc R . . C63 C 0.4295(10) 0.2544(8) 0.5359(8) 0.047(4) Uani 1 1 d . . . H63A H 0.4362 0.2386 0.5874 0.056 Uiso 1 1 calc R . . H63B H 0.3766 0.3038 0.5358 0.056 Uiso 1 1 calc R . . C64 C 0.5404(10) 0.2696(7) 0.4882(7) 0.039(3) Uani 1 1 d . . . H64A H 0.5337 0.2879 0.4371 0.047 Uiso 1 1 calc R . . H64B H 0.5662 0.3113 0.5084 0.047 Uiso 1 1 calc R . . C65 C 0.8678(10) -0.0063(7) 0.2765(7) 0.039(3) Uani 1 1 d . . . H65A H 0.9203 -0.0534 0.2887 0.047 Uiso 1 1 calc R . . C66 C 0.8705(12) -0.0097(8) 0.1962(7) 0.048(4) Uani 1 1 d . . . H66A H 0.9439 -0.0045 0.1666 0.058 Uiso 1 1 calc R . . H66B H 0.8192 0.0352 0.1800 0.058 Uiso 1 1 calc R . . C67 C 0.8403(10) -0.0876(8) 0.1827(6) 0.038(3) Uani 1 1 d . . . H67A H 0.8360 -0.0861 0.1305 0.045 Uiso 1 1 calc R . . H67B H 0.8979 -0.1317 0.1917 0.045 Uiso 1 1 calc R . . C68 C 0.7328(11) -0.1038(9) 0.2320(7) 0.047(4) Uani 1 1 d . . . H68A H 0.6734 -0.0650 0.2172 0.057 Uiso 1 1 calc R . . H68B H 0.7212 -0.1574 0.2249 0.057 Uiso 1 1 calc R . . C69 C 0.7291(13) -0.0985(9) 0.3107(7) 0.053(4) Uani 1 1 d . . . H69A H 0.7804 -0.1429 0.3275 0.064 Uiso 1 1 calc R . . H69B H 0.6556 -0.1042 0.3398 0.064 Uiso 1 1 calc R . . C70 C 0.7571(10) -0.0210(8) 0.3258(7) 0.043(4) Uani 1 1 d . . . H70A H 0.7599 -0.0227 0.3784 0.052 Uiso 1 1 calc R . . H70B H 0.7002 0.0232 0.3160 0.052 Uiso 1 1 calc R . . C71 C 1.0302(9) 0.1053(6) 0.2322(6) 0.026(3) Uani 1 1 d . . . H71A H 1.0048 0.1192 0.1851 0.031 Uiso 1 1 calc R . . C72 C 1.0639(10) 0.1805(7) 0.2514(6) 0.034(3) Uani 1 1 d . . . H72A H 0.9999 0.2225 0.2609 0.041 Uiso 1 1 calc R . . H72B H 1.0922 0.1686 0.2969 0.041 Uiso 1 1 calc R . . C73 C 1.1505(11) 0.2105(7) 0.1887(7) 0.039(3) Uani 1 1 d . . . H73A H 1.1716 0.2579 0.2029 0.047 Uiso 1 1 calc R . . H73B H 1.1202 0.2262 0.1442 0.047 Uiso 1 1 calc R . . C74 C 1.2513(11) 0.1470(8) 0.1702(8) 0.047(4) Uani 1 1 d . . . H74A H 1.3033 0.1667 0.1269 0.056 Uiso 1 1 calc R . . H74B H 1.2870 0.1354 0.2124 0.056 Uiso 1 1 calc R . . C75 C 1.2175(10) 0.0719(7) 0.1533(6) 0.034(3) Uani 1 1 d . . . H75A H 1.1887 0.0830 0.1080 0.040 Uiso 1 1 calc R . . H75B H 1.2821 0.0304 0.1437 0.040 Uiso 1 1 calc R . . C76 C 1.1318(9) 0.0405(6) 0.2163(6) 0.027(3) Uani 1 1 d . . . H76A H 1.1613 0.0261 0.2612 0.033 Uiso 1 1 calc R . . H76B H 1.1118 -0.0075 0.2024 0.033 Uiso 1 1 calc R . . C81 C 0.4376(14) 0.8649(12) 0.8406(13) 0.112(9) Uani 1 1 d . . . H81A H 0.3584 0.8680 0.8478 0.134 Uiso 1 1 calc R . . H81B H 0.4645 0.8158 0.8684 0.134 Uiso 1 1 calc R . . Cl3 Cl 0.4604(5) 0.9384(4) 0.8748(3) 0.1085(19) Uani 1 1 d . . . Cl4 Cl 0.5000(4) 0.8569(4) 0.7408(3) 0.0965(18) Uani 1 1 d . . . C82 C 0.6856(15) 0.6359(8) 0.6515(8) 0.065(5) Uani 1 1 d . . . H82A H 0.6153 0.6678 0.6465 0.078 Uiso 1 1 calc R . . H82B H 0.6712 0.5874 0.6838 0.078 Uiso 1 1 calc R . . Cl5 Cl 0.7567(4) 0.6903(2) 0.6906(2) 0.0731(13) Uani 1 1 d . . . Cl6 Cl 0.7627(4) 0.6097(2) 0.5634(2) 0.0707(12) Uani 1 1 d . . . C83 C 1.0977(13) 0.6259(8) 0.8389(7) 0.058(4) Uani 1 1 d . . . Cl7 Cl 1.1492(4) 0.5236(2) 0.8428(4) 0.074(2) Uani 0.67 1 d P . . Cl8 Cl 1.0278(3) 0.6515(2) 0.92895(19) 0.0234(9) Uani 0.67 1 d P . . Cl9 Cl 1.0128(10) 0.6102(7) 0.7877(5) 0.142(4) Uani 0.67 1 d P . . 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 0.0250(5) 0.0247(5) 0.0230(5) -0.0085(4) -0.0037(4) -0.0006(4) Cl1 0.0307(16) 0.0350(16) 0.0356(16) -0.0177(14) -0.0053(13) 0.0066(13) Cl2 0.0331(17) 0.0414(17) 0.0372(16) -0.0220(15) -0.0113(13) 0.0028(14) P1 0.0267(16) 0.0234(15) 0.0215(15) -0.0056(13) -0.0032(12) -0.0022(13) C1 0.052(8) 0.027(6) 0.023(6) -0.013(5) -0.003(6) 0.006(6) C2 0.024(6) 0.041(7) 0.017(5) -0.014(5) 0.002(5) -0.003(5) C3 0.039(8) 0.056(9) 0.047(8) -0.030(7) -0.018(6) 0.004(7) C4 0.036(8) 0.067(10) 0.059(9) -0.048(9) -0.003(7) -0.007(8) C5 0.049(9) 0.038(8) 0.047(8) -0.027(7) 0.007(7) -0.019(7) C6 0.056(9) 0.041(8) 0.031(7) -0.023(6) -0.002(6) -0.011(7) C7 0.087(12) 0.018(6) 0.042(8) 0.000(6) -0.009(8) -0.009(7) C8 0.087(12) 0.021(7) 0.049(8) -0.009(6) -0.037(8) 0.003(7) C9 0.078(11) 0.022(6) 0.040(7) -0.004(6) -0.032(7) -0.004(7) C10 0.042(8) 0.022(6) 0.035(7) -0.008(5) -0.011(6) -0.010(5) C11 0.034(7) 0.038(7) 0.014(5) -0.014(5) -0.004(5) -0.004(6) C12 0.031(7) 0.038(7) 0.030(6) -0.011(6) -0.005(5) 0.009(6) P12 0.0272(16) 0.0283(16) 0.0233(15) -0.0112(13) -0.0036(13) -0.0019(13) C13 0.036(7) 0.027(6) 0.024(6) -0.016(5) -0.008(5) -0.001(5) C14 0.042(8) 0.037(7) 0.025(6) 0.001(6) -0.001(6) 0.001(6) C15 0.028(7) 0.037(7) 0.054(8) 0.012(7) 0.004(6) -0.002(6) C16 0.040(8) 0.046(8) 0.033(7) 0.020(6) 0.001(6) -0.017(6) C17 0.012(6) 0.047(8) 0.049(8) -0.009(7) 0.002(5) 0.007(5) C18 0.032(7) 0.024(6) 0.036(7) 0.000(5) 0.003(5) -0.013(5) C19 0.042(7) 0.025(6) 0.024(6) -0.006(5) 0.000(5) -0.006(5) C20 0.040(7) 0.030(6) 0.032(6) -0.016(6) -0.010(6) -0.005(6) C21 0.030(7) 0.036(7) 0.033(7) -0.011(6) -0.007(5) 0.004(6) C22 0.055(9) 0.031(7) 0.023(6) 0.001(6) 0.003(6) -0.009(6) C23 0.047(8) 0.025(6) 0.032(7) 0.006(6) 0.000(6) -0.004(6) C24 0.053(8) 0.028(6) 0.038(7) -0.004(6) -0.027(6) -0.007(6) C25 0.035(7) 0.027(6) 0.034(7) -0.006(6) 0.000(6) 0.008(5) C26 0.037(7) 0.037(7) 0.033(7) -0.010(6) -0.012(6) -0.001(6) C27 0.047(8) 0.048(8) 0.018(6) -0.011(6) -0.005(6) 0.011(6) C28 0.045(8) 0.036(7) 0.026(6) 0.005(6) 0.012(6) 0.005(6) C29 0.043(8) 0.027(6) 0.034(7) -0.008(6) -0.007(6) -0.003(6) C30 0.019(6) 0.033(7) 0.042(7) -0.007(6) -0.004(5) -0.007(5) C31 0.033(7) 0.024(6) 0.021(6) -0.005(5) -0.001(5) -0.009(5) C32 0.045(8) 0.032(7) 0.022(6) -0.001(5) -0.010(5) -0.004(6) C33 0.029(7) 0.054(8) 0.045(8) 0.000(7) -0.016(6) -0.022(6) C34 0.048(9) 0.061(9) 0.036(7) -0.010(7) -0.004(7) -0.028(7) C35 0.018(6) 0.058(8) 0.032(7) -0.015(6) 0.001(5) -0.013(6) C36 0.029(7) 0.040(7) 0.024(6) -0.012(6) 0.001(5) -0.004(6) Pd41 0.0343(5) 0.0259(5) 0.0259(5) -0.0095(4) -0.0108(4) 0.0033(4) Cl41 0.075(3) 0.0418(19) 0.0387(18) -0.0177(16) -0.0302(17) 0.0324(18) Cl42 0.0469(19) 0.0343(16) 0.0272(15) -0.0098(13) -0.0126(14) 0.0019(14) P41 0.0299(17) 0.0252(15) 0.0270(15) -0.0084(13) -0.0097(13) 0.0014(13) C41 0.039(7) 0.024(6) 0.035(7) -0.002(5) -0.019(6) -0.007(5) C42 0.039(7) 0.034(7) 0.026(6) -0.007(6) -0.013(5) 0.012(6) C43 0.042(8) 0.036(7) 0.031(7) -0.013(6) -0.016(6) 0.009(6) C44 0.043(7) 0.037(7) 0.009(5) -0.003(5) -0.007(5) 0.018(6) C45 0.042(7) 0.035(7) 0.023(6) 0.008(5) -0.013(5) -0.017(6) C46 0.028(6) 0.033(6) 0.021(6) 0.004(5) -0.016(5) -0.012(5) C47 0.025(6) 0.025(6) 0.039(7) 0.001(5) -0.015(5) -0.001(5) C48 0.035(7) 0.023(6) 0.022(6) -0.001(5) -0.014(5) 0.002(5) C49 0.039(7) 0.033(7) 0.018(6) 0.000(5) 0.000(5) 0.008(6) C50 0.016(6) 0.021(6) 0.034(6) 0.005(5) -0.005(5) -0.002(5) C51 0.024(6) 0.021(6) 0.030(6) -0.003(5) -0.004(5) -0.002(5) C52 0.021(6) 0.043(7) 0.042(7) -0.001(6) -0.003(6) 0.006(6) P52 0.0289(17) 0.0219(15) 0.0263(15) -0.0041(13) -0.0080(13) -0.0021(13) C53 0.021(6) 0.026(6) 0.027(6) -0.004(5) -0.011(5) 0.007(5) C54 0.031(7) 0.030(6) 0.033(6) -0.013(6) -0.008(5) -0.004(5) C55 0.035(7) 0.025(6) 0.027(6) -0.009(5) -0.008(5) 0.011(5) C56 0.034(7) 0.033(7) 0.037(7) 0.002(6) -0.010(6) -0.008(6) C57 0.057(9) 0.021(6) 0.031(7) -0.004(5) -0.006(6) -0.007(6) C58 0.030(7) 0.044(8) 0.036(7) -0.007(6) -0.005(6) 0.009(6) C59 0.027(6) 0.026(6) 0.030(6) -0.012(5) -0.007(5) 0.005(5) C60 0.032(7) 0.035(7) 0.029(6) -0.014(6) -0.008(5) -0.002(6) C61 0.044(8) 0.041(7) 0.031(7) 0.001(6) -0.012(6) -0.004(6) C62 0.036(8) 0.041(8) 0.050(8) -0.021(7) -0.014(6) 0.001(6) C63 0.032(7) 0.051(8) 0.060(9) -0.029(7) -0.016(7) 0.010(6) C64 0.033(7) 0.034(7) 0.056(8) -0.021(7) -0.014(6) -0.004(6) C65 0.033(7) 0.041(7) 0.045(7) -0.026(7) 0.005(6) -0.013(6) C66 0.059(9) 0.053(9) 0.037(7) -0.023(7) -0.004(7) -0.019(7) C67 0.039(7) 0.051(8) 0.027(6) -0.014(6) 0.003(6) -0.024(6) C68 0.051(9) 0.055(9) 0.035(7) -0.012(7) 0.003(6) -0.019(7) C69 0.062(10) 0.066(10) 0.036(8) -0.017(7) 0.003(7) -0.032(8) C70 0.039(8) 0.047(8) 0.040(7) -0.021(7) 0.016(6) -0.016(6) C71 0.032(7) 0.017(5) 0.026(6) -0.006(5) -0.001(5) -0.004(5) C72 0.033(7) 0.036(7) 0.032(6) -0.006(6) 0.002(5) -0.013(6) C73 0.057(9) 0.036(7) 0.032(7) -0.004(6) -0.008(6) -0.028(6) C74 0.043(8) 0.053(9) 0.044(8) -0.007(7) -0.003(7) -0.012(7) C75 0.041(8) 0.034(7) 0.021(6) 0.000(5) -0.003(5) -0.001(6) C76 0.026(6) 0.030(6) 0.021(6) -0.006(5) 0.004(5) -0.004(5) C81 0.034(10) 0.089(14) 0.20(2) -0.063(16) 0.024(12) -0.014(9) Cl3 0.089(4) 0.126(5) 0.109(4) -0.041(4) -0.010(3) -0.007(3) Cl4 0.060(3) 0.167(5) 0.067(3) -0.030(3) -0.003(2) -0.032(3) C82 0.102(14) 0.036(8) 0.066(10) 0.000(8) -0.022(10) -0.033(9) Cl5 0.104(4) 0.065(3) 0.059(2) -0.004(2) -0.018(2) -0.039(3) Cl6 0.092(3) 0.048(2) 0.080(3) -0.017(2) -0.034(3) -0.006(2) C83 0.085(12) 0.051(9) 0.029(7) -0.026(7) -0.002(7) 0.007(8) Cl7 0.055(3) 0.007(2) 0.128(5) -0.019(3) 0.045(4) -0.002(2) Cl8 0.031(2) 0.030(2) 0.0118(17) -0.0125(17) -0.0058(16) -0.0015(18) Cl9 0.171(11) 0.161(10) 0.101(7) -0.014(7) -0.025(7) -0.046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.272(3) . ? Pd1 P12 2.289(3) . ? Pd1 Cl1 2.357(3) . ? Pd1 Cl2 2.357(3) . ? P1 C13 1.835(13) . ? P1 C19 1.842(12) . ? P1 C1 1.877(10) . ? C1 C2 1.520(16) . ? C2 C3 1.392(17) . ? C2 C11 1.439(16) . ? C3 C4 1.38(2) . ? C4 C5 1.33(2) . ? C5 C6 1.445(19) . ? C6 C7 1.392(19) . ? C6 C11 1.436(17) . ? C7 C8 1.36(2) . ? C8 C9 1.398(18) . ? C9 C10 1.363(16) . ? C10 C11 1.440(16) . ? C10 C12 1.501(16) . ? C12 P12 1.881(11) . ? P12 C31 1.841(12) . ? P12 C25 1.855(12) . ? C13 C14 1.518(16) . ? C13 C18 1.552(15) . ? C14 C15 1.519(17) . ? C15 C16 1.550(16) . ? C16 C17 1.512(17) . ? C17 C18 1.532(16) . ? C19 C24 1.514(17) . ? C19 C20 1.543(16) . ? C20 C21 1.514(16) . ? C21 C22 1.498(17) . ? C22 C23 1.515(17) . ? C23 C24 1.560(16) . ? C25 C30 1.530(16) . ? C25 C26 1.547(17) . ? C26 C27 1.520(16) . ? C27 C28 1.500(17) . ? C28 C29 1.545(18) . ? C29 C30 1.551(16) . ? C31 C36 1.544(15) . ? C31 C32 1.549(15) . ? C32 C33 1.518(17) . ? C33 C34 1.529(18) . ? C34 C35 1.518(18) . ? C35 C36 1.505(16) . ? Pd41 P52 2.278(3) . ? Pd41 P41 2.278(3) . ? Pd41 Cl41 2.358(3) . ? Pd41 Cl42 2.379(3) . ? P41 C53 1.843(11) . ? P41 C41 1.846(12) . ? P41 C59 1.855(12) . ? C41 C42 1.524(16) . ? C42 C43 1.371(16) . ? C42 C51 1.431(14) . ? C43 C44 1.433(17) . ? C44 C45 1.331(15) . ? C45 C46 1.455(15) . ? C46 C47 1.400(15) . ? C46 C51 1.423(15) . ? C47 C48 1.373(15) . ? C48 C49 1.379(16) . ? C49 C50 1.381(14) . ? C50 C51 1.450(14) . ? C50 C52 1.528(16) . ? C52 P52 1.836(13) . ? P52 C65 1.830(12) . ? P52 C71 1.842(11) . ? C53 C54 1.524(14) . ? C53 C58 1.531(16) . ? C54 C55 1.542(15) . ? C55 C56 1.511(16) . ? C56 C57 1.546(15) . ? C57 C58 1.513(16) . ? C59 C64 1.523(15) . ? C59 C60 1.555(15) . ? C60 C61 1.526(17) . ? C61 C62 1.533(16) . ? C62 C63 1.534(17) . ? C63 C64 1.545(18) . ? C65 C66 1.503(17) . ? C65 C70 1.552(16) . ? C66 C67 1.529(17) . ? C67 C68 1.524(17) . ? C68 C69 1.477(17) . ? C69 C70 1.517(17) . ? C71 C72 1.545(15) . ? C71 C76 1.554(14) . ? C72 C73 1.529(16) . ? C73 C74 1.537(18) . ? C74 C75 1.527(17) . ? C75 C76 1.533(15) . ? C81 Cl3 1.586(18) . ? C81 Cl4 1.86(2) . ? C82 Cl5 1.746(15) . ? C82 Cl6 1.775(16) . ? C83 Cl9 1.691(19) . ? C83 Cl7 1.766(14) . ? C83 Cl8 1.778(12) . ? Cl7 Cl9 2.434(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P12 100.92(10) . . ? P1 Pd1 Cl1 86.50(10) . . ? P12 Pd1 Cl1 172.51(11) . . ? P1 Pd1 Cl2 171.82(11) . . ? P12 Pd1 Cl2 85.30(10) . . ? Cl1 Pd1 Cl2 87.41(10) . . ? C13 P1 C19 106.5(5) . . ? C13 P1 C1 107.3(5) . . ? C19 P1 C1 102.2(5) . . ? C13 P1 Pd1 112.8(4) . . ? C19 P1 Pd1 110.1(4) . . ? C1 P1 Pd1 116.9(4) . . ? C2 C1 P1 114.8(8) . . ? C3 C2 C11 119.9(12) . . ? C3 C2 C1 113.9(11) . . ? C11 C2 C1 126.1(10) . . ? C4 C3 C2 121.9(13) . . ? C5 C4 C3 121.2(13) . . ? C4 C5 C6 120.0(13) . . ? C7 C6 C11 119.5(13) . . ? C7 C6 C5 120.2(13) . . ? C11 C6 C5 120.3(12) . . ? C8 C7 C6 123.4(13) . . ? C7 C8 C9 116.8(12) . . ? C10 C9 C8 124.2(13) . . ? C9 C10 C11 119.0(11) . . ? C9 C10 C12 116.1(11) . . ? C11 C10 C12 124.8(11) . . ? C6 C11 C2 116.4(11) . . ? C6 C11 C10 117.0(11) . . ? C2 C11 C10 126.5(11) . . ? C10 C12 P12 121.9(8) . . ? C31 P12 C25 108.6(6) . . ? C31 P12 C12 101.8(5) . . ? C25 P12 C12 100.3(5) . . ? C31 P12 Pd1 107.4(4) . . ? C25 P12 Pd1 111.9(4) . . ? C12 P12 Pd1 125.5(4) . . ? C14 C13 C18 109.4(9) . . ? C14 C13 P1 111.2(8) . . ? C18 C13 P1 115.8(8) . . ? C13 C14 C15 113.3(11) . . ? C14 C15 C16 110.7(10) . . ? C17 C16 C15 110.7(10) . . ? C16 C17 C18 111.4(10) . . ? C17 C18 C13 111.5(9) . . ? C24 C19 C20 110.0(10) . . ? C24 C19 P1 112.4(9) . . ? C20 C19 P1 115.6(8) . . ? C21 C20 C19 110.7(9) . . ? C22 C21 C20 113.6(10) . . ? C21 C22 C23 110.3(10) . . ? C22 C23 C24 112.8(10) . . ? C19 C24 C23 109.2(10) . . ? C30 C25 C26 109.8(10) . . ? C30 C25 P12 110.6(8) . . ? C26 C25 P12 118.4(9) . . ? C27 C26 C25 109.5(10) . . ? C28 C27 C26 112.4(11) . . ? C27 C28 C29 111.2(10) . . ? C28 C29 C30 110.9(10) . . ? C25 C30 C29 111.5(9) . . ? C36 C31 C32 109.3(9) . . ? C36 C31 P12 116.4(8) . . ? C32 C31 P12 111.9(8) . . ? C33 C32 C31 110.5(10) . . ? C32 C33 C34 111.7(11) . . ? C35 C34 C33 113.3(11) . . ? C36 C35 C34 110.1(10) . . ? C35 C36 C31 111.5(9) . . ? P52 Pd41 P41 99.85(11) . . ? P52 Pd41 Cl41 170.77(13) . . ? P41 Pd41 Cl41 87.21(11) . . ? P52 Pd41 Cl42 87.14(10) . . ? P41 Pd41 Cl42 172.90(11) . . ? Cl41 Pd41 Cl42 85.71(11) . . ? C53 P41 C41 99.9(5) . . ? C53 P41 C59 108.3(5) . . ? C41 P41 C59 101.9(6) . . ? C53 P41 Pd41 109.1(4) . . ? C41 P41 Pd41 124.1(4) . . ? C59 P41 Pd41 112.1(4) . . ? C42 C41 P41 120.5(8) . . ? C43 C42 C51 119.2(12) . . ? C43 C42 C41 114.3(10) . . ? C51 C42 C41 126.4(10) . . ? C42 C43 C44 123.3(10) . . ? C45 C44 C43 118.1(10) . . ? C44 C45 C46 121.7(11) . . ? C47 C46 C51 123.0(10) . . ? C47 C46 C45 117.4(10) . . ? C51 C46 C45 119.5(10) . . ? C48 C47 C46 119.9(11) . . ? C47 C48 C49 118.6(10) . . ? C48 C49 C50 124.2(10) . . ? C49 C50 C51 118.8(10) . . ? C49 C50 C52 115.2(9) . . ? C51 C50 C52 126.0(9) . . ? C46 C51 C42 118.1(10) . . ? C46 C51 C50 115.5(9) . . ? C42 C51 C50 126.4(11) . . ? C50 C52 P52 118.7(9) . . ? C65 P52 C52 102.2(6) . . ? C65 P52 C71 109.7(5) . . ? C52 P52 C71 101.1(5) . . ? C65 P52 Pd41 114.4(4) . . ? C52 P52 Pd41 122.5(4) . . ? C71 P52 Pd41 105.9(3) . . ? C54 C53 C58 111.3(9) . . ? C54 C53 P41 116.9(8) . . ? C58 C53 P41 111.4(7) . . ? C53 C54 C55 110.4(10) . . ? C56 C55 C54 111.3(9) . . ? C55 C56 C57 111.6(10) . . ? C58 C57 C56 111.1(10) . . ? C57 C58 C53 112.5(9) . . ? C64 C59 C60 110.8(9) . . ? C64 C59 P41 115.6(9) . . ? C60 C59 P41 109.4(7) . . ? C61 C60 C59 111.3(9) . . ? C62 C61 C60 111.1(11) . . ? C61 C62 C63 111.6(11) . . ? C62 C63 C64 111.2(10) . . ? C59 C64 C63 108.8(10) . . ? C66 C65 C70 111.5(11) . . ? C66 C65 P52 117.9(10) . . ? C70 C65 P52 111.8(7) . . ? C65 C66 C67 110.9(11) . . ? C68 C67 C66 112.7(10) . . ? C69 C68 C67 112.1(12) . . ? C68 C69 C70 113.0(12) . . ? C69 C70 C65 110.8(9) . . ? C72 C71 C76 108.8(9) . . ? C72 C71 P52 110.0(7) . . ? C76 C71 P52 116.7(7) . . ? C73 C72 C71 111.1(9) . . ? C72 C73 C74 111.8(10) . . ? C75 C74 C73 109.2(11) . . ? C76 C75 C74 112.9(9) . . ? C75 C76 C71 109.5(9) . . ? Cl3 C81 Cl4 115.1(12) . . ? Cl5 C82 Cl6 109.5(9) . . ? Cl9 C83 Cl7 89.5(8) . . ? Cl9 C83 Cl8 112.1(10) . . ? Cl7 C83 Cl8 108.7(8) . . ? C83 Cl7 Cl9 44.0(6) . . ? C83 Cl9 Cl7 46.5(6) . . ? 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 P12 Pd1 P1 C13 -111.4(4) . . . . ? Cl1 Pd1 P1 C13 67.6(4) . . . . ? Cl2 Pd1 P1 C13 109.5(9) . . . . ? P12 Pd1 P1 C19 129.8(4) . . . . ? Cl1 Pd1 P1 C19 -51.2(4) . . . . ? Cl2 Pd1 P1 C19 -9.3(9) . . . . ? P12 Pd1 P1 C1 13.8(5) . . . . ? Cl1 Pd1 P1 C1 -167.2(4) . . . . ? Cl2 Pd1 P1 C1 -125.3(8) . . . . ? C13 P1 C1 C2 25.7(11) . . . . ? C19 P1 C1 C2 137.5(9) . . . . ? Pd1 P1 C1 C2 -102.2(9) . . . . ? P1 C1 C2 C3 -90.2(11) . . . . ? P1 C1 C2 C11 86.8(12) . . . . ? C11 C2 C3 C4 -5.3(17) . . . . ? C1 C2 C3 C4 172.0(11) . . . . ? C2 C3 C4 C5 0.9(19) . . . . ? C3 C4 C5 C6 3.7(19) . . . . ? C4 C5 C6 C7 175.8(12) . . . . ? C4 C5 C6 C11 -3.9(17) . . . . ? C11 C6 C7 C8 0.4(19) . . . . ? C5 C6 C7 C8 -179.2(12) . . . . ? C6 C7 C8 C9 2(2) . . . . ? C7 C8 C9 C10 -3(2) . . . . ? C8 C9 C10 C11 0.8(19) . . . . ? C8 C9 C10 C12 177.0(12) . . . . ? C7 C6 C11 C2 180.0(10) . . . . ? C5 C6 C11 C2 -0.4(15) . . . . ? C7 C6 C11 C10 -2.7(16) . . . . ? C5 C6 C11 C10 177.0(10) . . . . ? C3 C2 C11 C6 4.8(15) . . . . ? C1 C2 C11 C6 -172.1(10) . . . . ? C3 C2 C11 C10 -172.3(11) . . . . ? C1 C2 C11 C10 10.9(16) . . . . ? C9 C10 C11 C6 2.1(16) . . . . ? C12 C10 C11 C6 -173.8(10) . . . . ? C9 C10 C11 C2 179.2(10) . . . . ? C12 C10 C11 C2 3.2(17) . . . . ? C9 C10 C12 P12 90.0(12) . . . . ? C11 C10 C12 P12 -94.0(13) . . . . ? C10 C12 P12 C31 -169.0(10) . . . . ? C10 C12 P12 C25 -57.3(11) . . . . ? C10 C12 P12 Pd1 69.3(11) . . . . ? P1 Pd1 P12 C31 -115.2(4) . . . . ? Cl1 Pd1 P12 C31 72.6(10) . . . . ? Cl2 Pd1 P12 C31 59.4(4) . . . . ? P1 Pd1 P12 C25 125.6(4) . . . . ? Cl1 Pd1 P12 C25 -46.6(11) . . . . ? Cl2 Pd1 P12 C25 -59.8(5) . . . . ? P1 Pd1 P12 C12 4.0(5) . . . . ? Cl1 Pd1 P12 C12 -168.2(10) . . . . ? Cl2 Pd1 P12 C12 178.6(5) . . . . ? C19 P1 C13 C14 158.4(7) . . . . ? C1 P1 C13 C14 -92.7(8) . . . . ? Pd1 P1 C13 C14 37.6(8) . . . . ? C19 P1 C13 C18 32.6(9) . . . . ? C1 P1 C13 C18 141.5(8) . . . . ? Pd1 P1 C13 C18 -88.2(8) . . . . ? C18 C13 C14 C15 -55.1(12) . . . . ? P1 C13 C14 C15 175.6(8) . . . . ? C13 C14 C15 C16 55.5(14) . . . . ? C14 C15 C16 C17 -54.9(15) . . . . ? C15 C16 C17 C18 56.1(14) . . . . ? C16 C17 C18 C13 -56.8(13) . . . . ? C14 C13 C18 C17 54.9(13) . . . . ? P1 C13 C18 C17 -178.4(8) . . . . ? C13 P1 C19 C24 -171.1(8) . . . . ? C1 P1 C19 C24 76.4(9) . . . . ? Pd1 P1 C19 C24 -48.5(8) . . . . ? C13 P1 C19 C20 61.4(9) . . . . ? C1 P1 C19 C20 -51.0(10) . . . . ? Pd1 P1 C19 C20 -176.0(7) . . . . ? C24 C19 C20 C21 57.5(12) . . . . ? P1 C19 C20 C21 -173.8(8) . . . . ? C19 C20 C21 C22 -55.7(13) . . . . ? C20 C21 C22 C23 53.3(13) . . . . ? C21 C22 C23 C24 -53.6(13) . . . . ? C20 C19 C24 C23 -57.4(12) . . . . ? P1 C19 C24 C23 172.2(7) . . . . ? C22 C23 C24 C19 56.8(13) . . . . ? C31 P12 C25 C30 -155.4(7) . . . . ? C12 P12 C25 C30 98.3(8) . . . . ? Pd1 P12 C25 C30 -36.9(9) . . . . ? C31 P12 C25 C26 -27.4(9) . . . . ? C12 P12 C25 C26 -133.7(9) . . . . ? Pd1 P12 C25 C26 91.1(8) . . . . ? C30 C25 C26 C27 -58.4(12) . . . . ? P12 C25 C26 C27 173.2(7) . . . . ? C25 C26 C27 C28 59.2(12) . . . . ? C26 C27 C28 C29 -56.6(13) . . . . ? C27 C28 C29 C30 52.8(12) . . . . ? C26 C25 C30 C29 56.7(12) . . . . ? P12 C25 C30 C29 -170.8(7) . . . . ? C28 C29 C30 C25 -53.8(12) . . . . ? C25 P12 C31 C36 -60.2(9) . . . . ? C12 P12 C31 C36 45.1(9) . . . . ? Pd1 P12 C31 C36 178.6(7) . . . . ? C25 P12 C31 C32 173.2(7) . . . . ? C12 P12 C31 C32 -81.5(8) . . . . ? Pd1 P12 C31 C32 51.9(7) . . . . ? C36 C31 C32 C33 57.1(12) . . . . ? P12 C31 C32 C33 -172.5(8) . . . . ? C31 C32 C33 C34 -54.2(13) . . . . ? C32 C33 C34 C35 53.1(14) . . . . ? C33 C34 C35 C36 -53.9(13) . . . . ? C34 C35 C36 C31 57.2(12) . . . . ? C32 C31 C36 C35 -59.4(12) . . . . ? P12 C31 C36 C35 172.7(8) . . . . ? P52 Pd41 P41 C53 122.1(4) . . . . ? Cl41 Pd41 P41 C53 -51.9(4) . . . . ? Cl42 Pd41 P41 C53 -47.4(11) . . . . ? P52 Pd41 P41 C41 5.1(5) . . . . ? Cl41 Pd41 P41 C41 -168.9(5) . . . . ? Cl42 Pd41 P41 C41 -164.4(10) . . . . ? P52 Pd41 P41 C59 -117.9(4) . . . . ? Cl41 Pd41 P41 C59 68.1(4) . . . . ? Cl42 Pd41 P41 C59 72.6(11) . . . . ? C53 P41 C41 C42 155.6(9) . . . . ? C59 P41 C41 C42 44.3(10) . . . . ? Pd41 P41 C41 C42 -83.2(10) . . . . ? P41 C41 C42 C43 -90.7(12) . . . . ? P41 C41 C42 C51 93.3(13) . . . . ? C51 C42 C43 C44 -4.1(18) . . . . ? C41 C42 C43 C44 179.6(11) . . . . ? C42 C43 C44 C45 3.6(18) . . . . ? C43 C44 C45 C46 -0.8(17) . . . . ? C44 C45 C46 C47 176.9(11) . . . . ? C44 C45 C46 C51 -1.4(17) . . . . ? C51 C46 C47 C48 -0.6(17) . . . . ? C45 C46 C47 C48 -178.9(10) . . . . ? C46 C47 C48 C49 -0.2(16) . . . . ? C47 C48 C49 C50 -0.7(18) . . . . ? C48 C49 C50 C51 2.3(18) . . . . ? C48 C49 C50 C52 -179.0(11) . . . . ? C47 C46 C51 C42 -177.3(10) . . . . ? C45 C46 C51 C42 1.0(16) . . . . ? C47 C46 C51 C50 2.2(16) . . . . ? C45 C46 C51 C50 -179.6(10) . . . . ? C43 C42 C51 C46 1.7(17) . . . . ? C41 C42 C51 C46 177.5(10) . . . . ? C43 C42 C51 C50 -177.7(11) . . . . ? C41 C42 C51 C50 -1.9(19) . . . . ? C49 C50 C51 C46 -2.9(15) . . . . ? C52 C50 C51 C46 178.6(11) . . . . ? C49 C50 C51 C42 176.5(11) . . . . ? C52 C50 C51 C42 -2.0(19) . . . . ? C49 C50 C52 P52 90.8(11) . . . . ? C51 C50 C52 P52 -90.7(13) . . . . ? C50 C52 P52 C65 -37.7(9) . . . . ? C50 C52 P52 C71 -150.9(8) . . . . ? C50 C52 P52 Pd41 92.0(9) . . . . ? P41 Pd41 P52 C65 114.4(5) . . . . ? Cl41 Pd41 P52 C65 -106.1(9) . . . . ? Cl42 Pd41 P52 C65 -66.9(5) . . . . ? P41 Pd41 P52 C52 -9.9(5) . . . . ? Cl41 Pd41 P52 C52 129.6(8) . . . . ? Cl42 Pd41 P52 C52 168.8(5) . . . . ? P41 Pd41 P52 C71 -124.6(4) . . . . ? Cl41 Pd41 P52 C71 14.9(9) . . . . ? Cl42 Pd41 P52 C71 54.1(4) . . . . ? C41 P41 C53 C54 -48.8(9) . . . . ? C59 P41 C53 C54 57.4(9) . . . . ? Pd41 P41 C53 C54 179.8(7) . . . . ? C41 P41 C53 C58 80.8(9) . . . . ? C59 P41 C53 C58 -173.0(8) . . . . ? Pd41 P41 C53 C58 -50.7(8) . . . . ? C58 C53 C54 C55 55.5(12) . . . . ? P41 C53 C54 C55 -174.9(7) . . . . ? C53 C54 C55 C56 -56.7(12) . . . . ? C54 C55 C56 C57 55.9(13) . . . . ? C55 C56 C57 C58 -54.0(13) . . . . ? C56 C57 C58 C53 53.3(14) . . . . ? C54 C53 C58 C57 -54.8(13) . . . . ? P41 C53 C58 C57 172.7(8) . . . . ? C53 P41 C59 C64 36.4(10) . . . . ? C41 P41 C59 C64 141.2(9) . . . . ? Pd41 P41 C59 C64 -84.0(8) . . . . ? C53 P41 C59 C60 162.3(8) . . . . ? C41 P41 C59 C60 -92.9(8) . . . . ? Pd41 P41 C59 C60 41.8(9) . . . . ? C64 C59 C60 C61 -57.6(13) . . . . ? P41 C59 C60 C61 173.9(8) . . . . ? C59 C60 C61 C62 53.8(13) . . . . ? C60 C61 C62 C63 -53.7(14) . . . . ? C61 C62 C63 C64 56.4(15) . . . . ? C60 C59 C64 C63 58.8(13) . . . . ? P41 C59 C64 C63 -176.0(8) . . . . ? C62 C63 C64 C59 -58.7(14) . . . . ? C52 P52 C65 C66 -144.0(10) . . . . ? C71 P52 C65 C66 -37.4(12) . . . . ? Pd41 P52 C65 C66 81.4(10) . . . . ? C52 P52 C65 C70 84.8(10) . . . . ? C71 P52 C65 C70 -168.6(9) . . . . ? Pd41 P52 C65 C70 -49.8(11) . . . . ? C70 C65 C66 C67 -54.4(15) . . . . ? P52 C65 C66 C67 174.3(9) . . . . ? C65 C66 C67 C68 53.5(16) . . . . ? C66 C67 C68 C69 -52.7(17) . . . . ? C67 C68 C69 C70 53.2(17) . . . . ? C68 C69 C70 C65 -54.0(17) . . . . ? C66 C65 C70 C69 54.6(16) . . . . ? P52 C65 C70 C69 -171.0(10) . . . . ? C65 P52 C71 C72 175.5(9) . . . . ? C52 P52 C71 C72 -77.1(9) . . . . ? Pd41 P52 C71 C72 51.6(9) . . . . ? C65 P52 C71 C76 -59.9(10) . . . . ? C52 P52 C71 C76 47.5(9) . . . . ? Pd41 P52 C71 C76 176.2(7) . . . . ? C76 C71 C72 C73 58.2(13) . . . . ? P52 C71 C72 C73 -172.8(9) . . . . ? C71 C72 C73 C74 -57.8(14) . . . . ? C72 C73 C74 C75 55.1(14) . . . . ? C73 C74 C75 C76 -56.2(14) . . . . ? C74 C75 C76 C71 58.5(13) . . . . ? C72 C71 C76 C75 -57.7(12) . . . . ? P52 C71 C76 C75 177.1(8) . . . . ? Cl8 C83 Cl7 Cl9 113.2(12) . . . . ? Cl8 C83 Cl9 Cl7 -110.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.321 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.166 # Attachment '1_dbpn_sasol59.CIF' data_sasol59 _database_code_depnum_ccdc_archive 'CCDC 295572' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H46 P2' _chemical_formula_sum 'C28 H46 P2' _chemical_formula_weight 444.59 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' _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 11.244(3) _cell_length_b 17.850(4) _cell_length_c 14.521(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.690(6) _cell_angle_gamma 90.00 _cell_volume 2708.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8586 _cell_measurement_theta_min 1.8925 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Platelet _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0000 _exptl_absorpt_correction_T_max 0.0000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16668 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4776 _reflns_number_gt 3964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.6155P] 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 idealised _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 4776 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.76632(5) 0.31103(3) 0.49808(4) 0.01997(16) Uani 1 1 d . . . C1 C 0.8226(2) 0.27763(12) 0.39865(15) 0.0205(5) Uani 1 1 d . . . H1A H 0.7669 0.3000 0.3349 0.025 Uiso 1 1 calc R . . H1B H 0.9104 0.2968 0.4135 0.025 Uiso 1 1 calc R . . C2 C 0.8240(2) 0.19257(12) 0.38562(15) 0.0207(5) Uani 1 1 d . . . C3 C 0.7372(2) 0.15108(13) 0.41057(16) 0.0282(5) Uani 1 1 d . . . H3A H 0.6732 0.1767 0.4264 0.034 Uiso 1 1 calc R . . C4 C 0.7392(3) 0.07235(14) 0.41362(18) 0.0363(6) Uani 1 1 d . . . H4A H 0.6754 0.0457 0.4286 0.044 Uiso 1 1 calc R . . C5 C 0.8324(3) 0.03465(14) 0.39518(17) 0.0338(6) Uani 1 1 d . . . H5A H 0.8376 -0.0183 0.4023 0.041 Uiso 1 1 calc R . . C6 C 0.9222(2) 0.07326(13) 0.36541(16) 0.0259(5) Uani 1 1 d . . . C7 C 1.0176(2) 0.03116(13) 0.34628(17) 0.0301(6) Uani 1 1 d . . . H7A H 1.0233 -0.0214 0.3574 0.036 Uiso 1 1 calc R . . C8 C 1.1008(2) 0.06554(13) 0.31223(17) 0.0304(6) Uani 1 1 d . . . H8A H 1.1670 0.0376 0.3024 0.036 Uiso 1 1 calc R . . C9 C 1.0884(2) 0.14261(13) 0.29157(17) 0.0260(5) Uani 1 1 d . . . H9A H 1.1440 0.1653 0.2638 0.031 Uiso 1 1 calc R . . C10 C 0.99881(19) 0.18692(12) 0.30986(15) 0.0189(5) Uani 1 1 d . . . C11 C 0.9154(2) 0.15363(12) 0.35378(15) 0.0196(5) Uani 1 1 d . . . C12 C 0.9913(2) 0.26894(12) 0.27854(15) 0.0199(5) Uani 1 1 d . . . H12A H 1.0471 0.2985 0.3359 0.024 Uiso 1 1 calc R . . H12B H 0.9024 0.2865 0.2626 0.024 Uiso 1 1 calc R . . P12 P 1.03792(5) 0.28994(3) 0.17031(4) 0.01963(16) Uani 1 1 d . . . C13 C 0.7066(2) 0.40786(13) 0.44851(17) 0.0257(5) Uani 1 1 d . . . C14 C 0.6916(2) 0.45500(14) 0.53239(19) 0.0358(6) Uani 1 1 d . . . H14A H 0.6612 0.5052 0.5075 0.054 Uiso 1 1 calc R . . H14B H 0.7744 0.4588 0.5874 0.054 Uiso 1 1 calc R . . H14C H 0.6295 0.4309 0.5557 0.054 Uiso 1 1 calc R . . C15 C 0.7842(2) 0.45251(14) 0.40017(19) 0.0345(6) Uani 1 1 d . . . H15A H 0.7433 0.5012 0.3781 0.052 Uiso 1 1 calc R . . H15B H 0.7877 0.4247 0.3430 0.052 Uiso 1 1 calc R . . H15C H 0.8712 0.4602 0.4484 0.052 Uiso 1 1 calc R . . C16 C 0.5714(2) 0.39398(14) 0.37113(18) 0.0330(6) Uani 1 1 d . . . H16A H 0.5334 0.4418 0.3414 0.049 Uiso 1 1 calc R . . H16B H 0.5180 0.3708 0.4034 0.049 Uiso 1 1 calc R . . H16C H 0.5769 0.3605 0.3193 0.049 Uiso 1 1 calc R . . C17 C 0.9223(2) 0.31800(13) 0.60890(16) 0.0248(5) Uani 1 1 d . . . C18 C 0.9850(2) 0.24050(14) 0.61959(17) 0.0327(6) Uani 1 1 d . . . H18A H 1.0667 0.2408 0.6761 0.049 Uiso 1 1 calc R . . H18B H 1.0001 0.2284 0.5590 0.049 Uiso 1 1 calc R . . H18C H 0.9283 0.2028 0.6305 0.049 Uiso 1 1 calc R . . C19 C 0.8886(2) 0.33049(15) 0.70172(17) 0.0328(6) Uani 1 1 d . . . H19A H 0.9676 0.3344 0.7604 0.049 Uiso 1 1 calc R . . H19B H 0.8377 0.2882 0.7096 0.049 Uiso 1 1 calc R . . H19C H 0.8392 0.3769 0.6940 0.049 Uiso 1 1 calc R . . C20 C 1.0185(2) 0.37723(14) 0.60511(18) 0.0299(6) Uani 1 1 d . . . H20A H 1.0945 0.3752 0.6663 0.045 Uiso 1 1 calc R . . H20B H 0.9794 0.4270 0.5983 0.045 Uiso 1 1 calc R . . H20C H 1.0434 0.3675 0.5483 0.045 Uiso 1 1 calc R . . C21 C 0.8781(2) 0.28244(13) 0.06380(15) 0.0231(5) Uani 1 1 d . . . C22 C 0.8299(2) 0.20273(14) 0.06932(18) 0.0322(6) Uani 1 1 d . . . H22A H 0.7467 0.1955 0.0157 0.048 Uiso 1 1 calc R . . H22B H 0.8210 0.1955 0.1334 0.048 Uiso 1 1 calc R . . H22C H 0.8914 0.1664 0.0624 0.048 Uiso 1 1 calc R . . C23 C 0.9026(2) 0.28873(14) -0.03390(16) 0.0281(6) Uani 1 1 d . . . H23A H 0.8211 0.2852 -0.0903 0.042 Uiso 1 1 calc R . . H23B H 0.9592 0.2480 -0.0374 0.042 Uiso 1 1 calc R . . H23C H 0.9431 0.3370 -0.0359 0.042 Uiso 1 1 calc R . . C24 C 0.7743(2) 0.33890(14) 0.06205(17) 0.0284(6) Uani 1 1 d . . . H24A H 0.6965 0.3296 0.0039 0.043 Uiso 1 1 calc R . . H24B H 0.8048 0.3899 0.0588 0.043 Uiso 1 1 calc R . . H24C H 0.7554 0.3333 0.1224 0.043 Uiso 1 1 calc R . . C25 C 1.0834(2) 0.39166(12) 0.19819(16) 0.0223(5) Uani 1 1 d . . . C26 C 1.2242(2) 0.38905(14) 0.27061(17) 0.0286(6) Uani 1 1 d . . . H26A H 1.2556 0.4402 0.2890 0.043 Uiso 1 1 calc R . . H26B H 1.2764 0.3641 0.2386 0.043 Uiso 1 1 calc R . . H26C H 1.2299 0.3612 0.3302 0.043 Uiso 1 1 calc R . . C27 C 1.0058(2) 0.43789(12) 0.24521(17) 0.0265(5) Uani 1 1 d . . . H27A H 1.0381 0.4894 0.2555 0.040 Uiso 1 1 calc R . . H27B H 1.0142 0.4158 0.3091 0.040 Uiso 1 1 calc R . . H27C H 0.9155 0.4380 0.2011 0.040 Uiso 1 1 calc R . . C28 C 1.0806(2) 0.43078(14) 0.10271(17) 0.0325(6) Uani 1 1 d . . . H28A H 1.1036 0.4837 0.1167 0.049 Uiso 1 1 calc R . . H28B H 0.9944 0.4271 0.0518 0.049 Uiso 1 1 calc R . . H28C H 1.1420 0.4065 0.0789 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0196(3) 0.0233(3) 0.0204(3) -0.0012(2) 0.0114(3) -0.0010(2) C1 0.0230(11) 0.0228(12) 0.0193(12) -0.0006(9) 0.0120(10) -0.0014(9) C2 0.0234(11) 0.0233(12) 0.0169(11) -0.0031(9) 0.0092(10) -0.0035(9) C3 0.0324(13) 0.0307(14) 0.0280(13) -0.0077(10) 0.0188(11) -0.0095(10) C4 0.0515(16) 0.0309(14) 0.0384(15) -0.0095(11) 0.0305(13) -0.0179(12) C5 0.0544(17) 0.0209(13) 0.0329(14) -0.0036(10) 0.0242(13) -0.0105(12) C6 0.0350(13) 0.0223(12) 0.0195(12) -0.0022(9) 0.0092(10) -0.0048(10) C7 0.0383(14) 0.0197(12) 0.0309(14) 0.0006(10) 0.0112(12) 0.0036(10) C8 0.0284(13) 0.0274(14) 0.0350(14) -0.0009(10) 0.0113(11) 0.0083(10) C9 0.0236(12) 0.0257(13) 0.0304(13) -0.0015(10) 0.0121(11) 0.0002(9) C10 0.0162(10) 0.0238(12) 0.0172(11) -0.0014(9) 0.0068(9) -0.0019(9) C11 0.0223(11) 0.0205(12) 0.0150(11) -0.0015(8) 0.0057(9) -0.0023(9) C12 0.0220(11) 0.0209(12) 0.0203(12) 0.0002(9) 0.0121(10) -0.0016(9) P12 0.0193(3) 0.0238(3) 0.0194(3) -0.0006(2) 0.0114(2) -0.0004(2) C13 0.0239(12) 0.0241(13) 0.0311(13) -0.0003(10) 0.0123(11) 0.0029(9) C14 0.0362(14) 0.0312(14) 0.0435(16) -0.0058(12) 0.0186(13) 0.0055(11) C15 0.0378(14) 0.0254(13) 0.0445(16) 0.0067(11) 0.0203(13) 0.0010(11) C16 0.0264(13) 0.0357(15) 0.0336(14) 0.0033(11) 0.0073(11) 0.0051(11) C17 0.0215(11) 0.0320(13) 0.0219(12) -0.0010(9) 0.0093(10) 0.0001(10) C18 0.0317(13) 0.0397(15) 0.0241(13) 0.0055(11) 0.0071(11) 0.0076(11) C19 0.0332(13) 0.0452(16) 0.0212(13) -0.0049(11) 0.0112(11) -0.0033(12) C20 0.0234(12) 0.0379(15) 0.0300(14) -0.0084(11) 0.0118(11) -0.0067(10) C21 0.0220(11) 0.0292(13) 0.0197(12) -0.0057(9) 0.0095(10) -0.0032(9) C22 0.0298(13) 0.0382(15) 0.0251(13) -0.0071(10) 0.0061(11) -0.0093(11) C23 0.0288(13) 0.0390(14) 0.0174(12) -0.0041(10) 0.0096(10) 0.0015(11) C24 0.0199(12) 0.0418(15) 0.0233(13) -0.0049(10) 0.0076(10) 0.0025(10) C25 0.0224(11) 0.0239(12) 0.0218(12) 0.0027(9) 0.0095(10) -0.0027(9) C26 0.0241(12) 0.0328(14) 0.0291(13) 0.0014(10) 0.0100(11) -0.0071(10) C27 0.0317(13) 0.0196(12) 0.0289(13) -0.0018(9) 0.0123(11) -0.0028(10) C28 0.0372(14) 0.0332(14) 0.0312(14) 0.0058(11) 0.0175(12) -0.0072(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.875(2) . ? P1 C17 1.896(2) . ? P1 C13 1.897(2) . ? C1 C2 1.531(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.376(3) . ? C2 C11 1.451(3) . ? C3 C4 1.406(3) . ? C3 H3A 0.9500 . ? C4 C5 1.353(4) . ? C4 H4A 0.9500 . ? C5 C6 1.416(3) . ? C5 H5A 0.9500 . ? C6 C7 1.419(3) . ? C6 C11 1.443(3) . ? C7 C8 1.355(3) . ? C7 H7A 0.9500 . ? C8 C9 1.404(3) . ? C8 H8A 0.9500 . ? C9 C10 1.382(3) . ? C9 H9A 0.9500 . ? C10 C11 1.443(3) . ? C10 C12 1.526(3) . ? C12 P12 1.869(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? P12 C25 1.889(2) . ? P12 C21 1.894(2) . ? C13 C15 1.530(3) . ? C13 C14 1.540(3) . ? C13 C16 1.540(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.528(3) . ? C17 C18 1.535(3) . ? C17 C19 1.545(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.535(3) . ? C21 C22 1.535(3) . ? C21 C23 1.546(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.533(3) . ? C25 C28 1.542(3) . ? C25 C26 1.543(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 P1 C17 101.82(10) . . ? C1 P1 C13 99.82(10) . . ? C17 P1 C13 110.42(10) . . ? C2 C1 P1 115.60(15) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C3 C2 C11 118.7(2) . . ? C3 C2 C1 117.5(2) . . ? C11 C2 C1 123.71(19) . . ? C2 C3 C4 122.8(2) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.7(2) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C7 118.6(2) . . ? C5 C6 C11 120.4(2) . . ? C7 C6 C11 121.0(2) . . ? C8 C7 C6 120.3(2) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C9 119.6(2) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 122.8(2) . . ? C10 C9 H9A 118.6 . . ? C8 C9 H9A 118.6 . . ? C9 C10 C11 119.2(2) . . ? C9 C10 C12 117.12(19) . . ? C11 C10 C12 123.60(19) . . ? C10 C11 C6 116.5(2) . . ? C10 C11 C2 126.6(2) . . ? C6 C11 C2 116.9(2) . . ? C10 C12 P12 116.16(15) . . ? C10 C12 H12A 108.2 . . ? P12 C12 H12A 108.2 . . ? C10 C12 H12B 108.2 . . ? P12 C12 H12B 108.2 . . ? H12A C12 H12B 107.4 . . ? C12 P12 C25 98.65(10) . . ? C12 P12 C21 101.31(10) . . ? C25 P12 C21 110.06(10) . . ? C15 C13 C14 109.0(2) . . ? C15 C13 C16 109.0(2) . . ? C14 C13 C16 107.3(2) . . ? C15 C13 P1 117.82(16) . . ? C14 C13 P1 108.94(16) . . ? C16 C13 P1 104.23(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C18 108.80(19) . . ? C20 C17 C19 109.67(19) . . ? C18 C17 C19 107.1(2) . . ? C20 C17 P1 117.39(16) . . ? C18 C17 P1 105.85(15) . . ? C19 C17 P1 107.57(15) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 109.21(19) . . ? C24 C21 C23 109.23(19) . . ? C22 C21 C23 107.53(19) . . ? C24 C21 P12 116.96(15) . . ? C22 C21 P12 105.63(15) . . ? C23 C21 P12 107.88(15) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 109.31(19) . . ? C27 C25 C26 108.79(18) . . ? C28 C25 C26 107.54(19) . . ? C27 C25 P12 117.33(15) . . ? C28 C25 P12 109.18(16) . . ? C26 C25 P12 104.19(15) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 C17 P1 C1 C2 92.16(17) . . . . ? C13 P1 C1 C2 -154.39(16) . . . . ? P1 C1 C2 C3 28.3(3) . . . . ? P1 C1 C2 C11 -148.33(17) . . . . ? C11 C2 C3 C4 4.8(3) . . . . ? C1 C2 C3 C4 -171.9(2) . . . . ? C2 C3 C4 C5 2.6(4) . . . . ? C3 C4 C5 C6 -4.9(4) . . . . ? C4 C5 C6 C7 -179.6(2) . . . . ? C4 C5 C6 C11 -0.3(3) . . . . ? C5 C6 C7 C8 176.2(2) . . . . ? C11 C6 C7 C8 -3.0(3) . . . . ? C6 C7 C8 C9 -2.9(3) . . . . ? C7 C8 C9 C10 3.9(3) . . . . ? C8 C9 C10 C11 1.2(3) . . . . ? C8 C9 C10 C12 -176.8(2) . . . . ? C9 C10 C11 C6 -6.8(3) . . . . ? C12 C10 C11 C6 171.02(19) . . . . ? C9 C10 C11 C2 174.4(2) . . . . ? C12 C10 C11 C2 -7.7(3) . . . . ? C5 C6 C11 C10 -171.4(2) . . . . ? C7 C6 C11 C10 7.8(3) . . . . ? C5 C6 C11 C2 7.4(3) . . . . ? C7 C6 C11 C2 -173.3(2) . . . . ? C3 C2 C11 C10 169.2(2) . . . . ? C1 C2 C11 C10 -14.2(3) . . . . ? C3 C2 C11 C6 -9.5(3) . . . . ? C1 C2 C11 C6 167.02(19) . . . . ? C9 C10 C12 P12 29.0(2) . . . . ? C11 C10 C12 P12 -148.93(17) . . . . ? C10 C12 P12 C25 -156.06(16) . . . . ? C10 C12 P12 C21 91.34(17) . . . . ? C1 P1 C13 C15 -38.81(19) . . . . ? C17 P1 C13 C15 67.8(2) . . . . ? C1 P1 C13 C14 -163.61(16) . . . . ? C17 P1 C13 C14 -56.98(18) . . . . ? C1 P1 C13 C16 82.07(17) . . . . ? C17 P1 C13 C16 -171.30(15) . . . . ? C1 P1 C17 C20 66.47(19) . . . . ? C13 P1 C17 C20 -38.8(2) . . . . ? C1 P1 C17 C18 -55.15(17) . . . . ? C13 P1 C17 C18 -160.44(16) . . . . ? C1 P1 C17 C19 -169.35(16) . . . . ? C13 P1 C17 C19 85.35(18) . . . . ? C12 P12 C21 C24 63.43(19) . . . . ? C25 P12 C21 C24 -40.2(2) . . . . ? C12 P12 C21 C22 -58.28(17) . . . . ? C25 P12 C21 C22 -161.95(15) . . . . ? C12 P12 C21 C23 -173.04(16) . . . . ? C25 P12 C21 C23 83.29(17) . . . . ? C12 P12 C25 C27 -35.11(18) . . . . ? C21 P12 C25 C27 70.36(18) . . . . ? C12 P12 C25 C28 -160.14(16) . . . . ? C21 P12 C25 C28 -54.67(18) . . . . ? C12 P12 C25 C26 85.20(16) . . . . ? C21 P12 C25 C26 -169.33(14) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.355 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.053 # Attachment '6_Pd_Napth(iPr2)P_dba2_revised after referee.CIF' data_sasol36 _database_code_depnum_ccdc_archive 'CCDC 295573' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H52 O P2 Pd.C4 H8 O' _chemical_formula_sum 'C45 H60 O2 P2 Pd' _chemical_formula_weight 801.27 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.0551(8) _cell_length_b 19.4716(8) _cell_length_c 15.9493(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.305(4) _cell_angle_gamma 90.00 _cell_volume 4119.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 19745 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 27.65 _exptl_crystal_description PRISM _exptl_crystal_colour red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1831 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23624 _diffrn_reflns_av_R_equivalents 0.1456 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11429 _reflns_number_gt 10439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+191.0101P] 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 0.0046(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(9) _refine_ls_number_reflns 11429 _refine_ls_number_parameters 454 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.1309 _refine_ls_wR_factor_ref 0.3122 _refine_ls_wR_factor_gt 0.3007 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.177 _refine_ls_shift/su_mean 0.029 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 0.51304(10) 0.41828(7) -0.04194(8) 0.0129(4) Uani 1 1 d . . . P1 P 0.5993(4) 0.3859(3) 0.1030(3) 0.0129(10) Uani 1 1 d . . . P2 P 0.5336(4) 0.5372(3) -0.0401(3) 0.0158(10) Uani 1 1 d . . . C1 C 0.6511(13) 0.4559(10) 0.1859(11) 0.012(4) Uiso 1 1 d . . . H1A H 0.6064 0.4964 0.1681 0.015 Uiso 1 1 calc R . . H1B H 0.6488 0.4403 0.2443 0.015 Uiso 1 1 calc R . . C2 C 0.7580(13) 0.4782(10) 0.1972(11) 0.011(3) Uiso 1 1 d . . . C3 C 0.8314(14) 0.4414(11) 0.2599(12) 0.020(4) Uiso 1 1 d . . . H3A H 0.8102 0.4074 0.2927 0.024 Uiso 1 1 calc R . . C4 C 0.9344(16) 0.4506(12) 0.2785(14) 0.025(5) Uiso 1 1 d . . . H4A H 0.9819 0.4237 0.3224 0.030 Uiso 1 1 calc R . . C5 C 0.9656(17) 0.4998(12) 0.2314(14) 0.029(5) Uiso 1 1 d . . . H5A H 1.0354 0.5054 0.2405 0.035 Uiso 1 1 calc R . . C6 C 0.8958(14) 0.5414(11) 0.1708(13) 0.019(4) Uiso 1 1 d . . . C7 C 0.9346(13) 0.5961(9) 0.1341(11) 0.011(4) Uiso 1 1 d . . . H7A H 1.0055 0.6004 0.1485 0.013 Uiso 1 1 calc R . . C8 C 0.8741(15) 0.6424(11) 0.0793(13) 0.023(4) Uiso 1 1 d . . . H8A H 0.9013 0.6783 0.0539 0.028 Uiso 1 1 calc R . . C9 C 0.7707(12) 0.6362(9) 0.0610(10) 0.009(3) Uiso 1 1 d . . . H9A H 0.7277 0.6706 0.0258 0.011 Uiso 1 1 calc R . . C10 C 0.7277(14) 0.5818(10) 0.0921(12) 0.014(4) Uiso 1 1 d . . . C11 C 0.7918(13) 0.5334(10) 0.1535(12) 0.015(4) Uiso 1 1 d . . . C12 C 0.6094(14) 0.5877(11) 0.0574(13) 0.020(4) Uiso 1 1 d . . . H12A H 0.5925 0.6367 0.0437 0.024 Uiso 1 1 calc R . . H12B H 0.5858 0.5755 0.1075 0.024 Uiso 1 1 calc R . . C13 C 0.7080(15) 0.3271(11) 0.1152(14) 0.026(5) Uiso 1 1 d . . . H13A H 0.7531 0.3229 0.1783 0.031 Uiso 1 1 calc R . . C14 C 0.7672(16) 0.3593(12) 0.0505(14) 0.029(5) Uiso 1 1 d . . . H14A H 0.8268 0.3314 0.0555 0.043 Uiso 1 1 calc R . . H14B H 0.7881 0.4065 0.0689 0.043 Uiso 1 1 calc R . . H14C H 0.7219 0.3592 -0.0112 0.043 Uiso 1 1 calc R . . C15 C 0.6695(17) 0.2591(12) 0.0748(14) 0.029(5) Uiso 1 1 d . . . H15A H 0.7263 0.2274 0.0838 0.043 Uiso 1 1 calc R . . H15B H 0.6341 0.2648 0.0111 0.043 Uiso 1 1 calc R . . H15C H 0.6230 0.2403 0.1032 0.043 Uiso 1 1 calc R . . C16 C 0.5236(14) 0.3380(11) 0.1579(13) 0.021(4) Uiso 1 1 d . . . H16A H 0.4914 0.2997 0.1165 0.025 Uiso 1 1 calc R . . C17 C 0.4349(15) 0.3832(11) 0.1651(13) 0.024(4) Uiso 1 1 d . . . H17A H 0.3938 0.3564 0.1922 0.035 Uiso 1 1 calc R . . H17B H 0.3931 0.3981 0.1056 0.035 Uiso 1 1 calc R . . H17C H 0.4621 0.4236 0.2019 0.035 Uiso 1 1 calc R . . C18 C 0.5813(17) 0.3031(13) 0.2481(15) 0.032(5) Uiso 1 1 d . . . H18A H 0.5333 0.2788 0.2702 0.048 Uiso 1 1 calc R . . H18B H 0.6166 0.3382 0.2913 0.048 Uiso 1 1 calc R . . H18C H 0.6303 0.2703 0.2397 0.048 Uiso 1 1 calc R . . C19 C 0.5723(17) 0.5680(12) -0.1358(15) 0.030(5) Uiso 1 1 d . . . H19A H 0.5203 0.5479 -0.1891 0.036 Uiso 1 1 calc R . . C20 C 0.6642(18) 0.5376(14) -0.1368(17) 0.040(6) Uiso 1 1 d . . . H20A H 0.6801 0.5542 -0.1887 0.060 Uiso 1 1 calc R . . H20B H 0.6568 0.4875 -0.1400 0.060 Uiso 1 1 calc R . . H20C H 0.7188 0.5502 -0.0825 0.060 Uiso 1 1 calc R . . C21 C 0.5635(16) 0.6461(11) -0.1537(14) 0.027(5) Uiso 1 1 d . . . H21A H 0.5835 0.6566 -0.2056 0.041 Uiso 1 1 calc R . . H21B H 0.6079 0.6706 -0.1018 0.041 Uiso 1 1 calc R . . H21C H 0.4937 0.6607 -0.1650 0.041 Uiso 1 1 calc R . . C22 C 0.4095(15) 0.5802(12) -0.0533(13) 0.023(4) Uiso 1 1 d . . . H22A H 0.4224 0.6305 -0.0434 0.027 Uiso 1 1 calc R . . C23 C 0.3646(18) 0.5548(13) 0.0150(15) 0.035(5) Uiso 1 1 d . . . H23A H 0.3004 0.5782 0.0067 0.052 Uiso 1 1 calc R . . H23B H 0.4113 0.5644 0.0748 0.052 Uiso 1 1 calc R . . H23C H 0.3530 0.5051 0.0079 0.052 Uiso 1 1 calc R . . C24 C 0.3287(17) 0.5704(13) -0.1479(15) 0.033(5) Uiso 1 1 d . . . H24A H 0.2657 0.5930 -0.1498 0.049 Uiso 1 1 calc R . . H24B H 0.3165 0.5213 -0.1602 0.049 Uiso 1 1 calc R . . H24C H 0.3537 0.5910 -0.1928 0.049 Uiso 1 1 calc R . . O25 O 0.3953(10) 0.2555(8) -0.0272(10) 0.025(3) Uani 1 1 d . . . C25 C 0.3790(15) 0.3088(11) -0.0730(13) 0.020(4) Uiso 1 1 d . . . C26 C 0.4427(15) 0.3298(11) -0.1199(13) 0.021(4) Uiso 1 1 d . . . H26A H 0.5004 0.3024 -0.1145 0.026 Uiso 1 1 calc R . . C27 C 0.4267(14) 0.3914(10) -0.1771(12) 0.016(4) Uiso 1 1 d . . . H27A H 0.3832 0.4273 -0.1717 0.020 Uiso 1 1 calc R . . C28 C 0.4812(15) 0.3963(11) -0.2446(13) 0.025(5) Uiso 1 1 d . . . C29 C 0.4369(17) 0.4429(12) -0.3168(14) 0.031(5) Uiso 1 1 d . . . H29A H 0.3753 0.4657 -0.3225 0.037 Uiso 1 1 calc R . . C30 C 0.4856(18) 0.4539(13) -0.3775(16) 0.037(5) Uiso 1 1 d . . . H30A H 0.4572 0.4835 -0.4267 0.044 Uiso 1 1 calc R . . C31 C 0.5763(19) 0.4214(16) -0.3661(17) 0.047(6) Uiso 1 1 d . . . H31A H 0.6066 0.4279 -0.4107 0.056 Uiso 1 1 calc R . . C32 C 0.626(2) 0.3806(17) -0.295(2) 0.055(7) Uiso 1 1 d . . . H32A H 0.6902 0.3616 -0.2882 0.067 Uiso 1 1 calc R . . C33 C 0.5729(18) 0.3675(13) -0.2302(16) 0.034(5) Uiso 1 1 d . . . H33A H 0.6028 0.3395 -0.1795 0.041 Uiso 1 1 calc R . . C34 C 0.2906(15) 0.3534(11) -0.0746(14) 0.022(4) Uiso 1 1 d . . . H34A H 0.2773 0.3932 -0.1110 0.027 Uiso 1 1 calc R . . C35 C 0.2298(13) 0.3396(10) -0.0272(11) 0.013(4) Uiso 1 1 d . . . H35A H 0.2454 0.2995 0.0088 0.015 Uiso 1 1 calc R . . C36 C 0.1412(17) 0.3797(12) -0.0245(15) 0.029(5) Uiso 1 1 d . . . C37 C 0.0998(16) 0.3681(13) 0.0398(15) 0.029(5) Uiso 1 1 d . . . H37A H 0.1270 0.3330 0.0823 0.035 Uiso 1 1 calc R . . C38 C 0.0161(16) 0.4074(13) 0.0454(14) 0.032(5) Uiso 1 1 d . . . H38A H -0.0121 0.3987 0.0909 0.039 Uiso 1 1 calc R . . C39 C -0.0223(19) 0.4576(14) -0.0158(16) 0.038(6) Uiso 1 1 d . . . H39A H -0.0796 0.4832 -0.0152 0.045 Uiso 1 1 calc R . . C40 C 0.0227(19) 0.4707(15) -0.0783(18) 0.043(6) Uiso 1 1 d . . . H40A H -0.0004 0.5080 -0.1182 0.052 Uiso 1 1 calc R . . C41 C 0.0997(17) 0.4312(12) -0.0843(15) 0.032(5) Uiso 1 1 d . . . H41A H 0.1258 0.4394 -0.1313 0.038 Uiso 1 1 calc R . . O42 O 0.8178(16) 0.2742(13) -0.2278(15) 0.071(7) Uani 1 1 d . . . C43 C 0.759(2) 0.2134(17) -0.231(2) 0.057(7) Uiso 1 1 d . . . H43A H 0.7852 0.1747 -0.2576 0.068 Uiso 1 1 calc R . . H43B H 0.6875 0.2214 -0.2669 0.068 Uiso 1 1 calc R . . C44 C 0.770(2) 0.198(2) -0.132(2) 0.066(8) Uiso 1 1 d . . . H44A H 0.7163 0.2204 -0.1148 0.080 Uiso 1 1 calc R . . H44B H 0.7688 0.1479 -0.1212 0.080 Uiso 1 1 calc R . . C45 C 0.870(2) 0.2272(18) -0.081(2) 0.065(9) Uiso 1 1 d . . . H45A H 0.9257 0.1959 -0.0808 0.078 Uiso 1 1 calc R . . H45B H 0.8751 0.2389 -0.0197 0.078 Uiso 1 1 calc R . . C46 C 0.868(3) 0.291(2) -0.137(2) 0.071(9) Uiso 1 1 d . . . H46A H 0.8315 0.3289 -0.1189 0.085 Uiso 1 1 calc R . . H46B H 0.9374 0.3069 -0.1290 0.085 Uiso 1 1 calc R . . Pd51 Pd 0.94291(9) 0.68751(6) 0.54880(8) 0.0119(3) Uani 1 1 d . . . P51 P 0.8680(4) 0.7195(3) 0.4007(3) 0.0140(10) Uani 1 1 d . . . P52 P 0.9214(4) 0.5714(3) 0.5523(3) 0.0137(10) Uani 1 1 d . . . C51 C 0.8065(15) 0.6546(11) 0.3137(13) 0.020(4) Uiso 1 1 d . . . H51A H 0.8010 0.6744 0.2551 0.024 Uiso 1 1 calc R . . H51B H 0.8517 0.6142 0.3230 0.024 Uiso 1 1 calc R . . C52 C 0.7006(15) 0.6290(12) 0.3094(13) 0.024(4) Uiso 1 1 d . . . C53 C 0.6263(14) 0.6699(10) 0.2502(12) 0.018(4) Uiso 1 1 d . . . H53A H 0.6454 0.7034 0.2154 0.022 Uiso 1 1 calc R . . C54 C 0.5225(16) 0.6623(12) 0.2412(14) 0.028(5) Uiso 1 1 d . . . H54A H 0.4738 0.6937 0.2059 0.033 Uiso 1 1 calc R . . C55 C 0.4939(16) 0.6095(11) 0.2838(13) 0.023(4) Uiso 1 1 d . . . H55A H 0.4248 0.6039 0.2776 0.028 Uiso 1 1 calc R . . C56 C 0.5683(15) 0.5614(11) 0.3388(13) 0.022(4) Uiso 1 1 d . . . C57 C 0.5328(16) 0.5044(11) 0.3716(13) 0.025(5) Uiso 1 1 d . . . H57A H 0.4630 0.5009 0.3642 0.030 Uiso 1 1 calc R . . C58 C 0.5985(14) 0.4520(11) 0.4154(12) 0.019(4) Uiso 1 1 d . . . H58A H 0.5741 0.4111 0.4335 0.023 Uiso 1 1 calc R . . C59 C 0.7027(16) 0.4622(11) 0.4318(14) 0.026(5) Uiso 1 1 d . . . H59A H 0.7478 0.4261 0.4593 0.031 Uiso 1 1 calc R . . C60 C 0.7425(13) 0.5223(10) 0.4098(12) 0.013(4) Uiso 1 1 d . . . C61 C 0.6738(14) 0.5729(11) 0.3555(12) 0.017(4) Uiso 1 1 d . . . C62 C 0.8582(14) 0.5235(11) 0.4428(13) 0.020(4) Uiso 1 1 d . . . H62A H 0.8806 0.5448 0.3962 0.024 Uiso 1 1 calc R . . H62B H 0.8827 0.4755 0.4501 0.024 Uiso 1 1 calc R . . C63 C 0.7725(15) 0.7854(11) 0.3900(13) 0.021(4) Uiso 1 1 d . . . H63A H 0.7310 0.7868 0.3256 0.026 Uiso 1 1 calc R . . C64 C 0.6993(18) 0.7671(14) 0.4401(16) 0.039(6) Uiso 1 1 d . . . H64A H 0.6491 0.8036 0.4315 0.058 Uiso 1 1 calc R . . H64B H 0.7370 0.7622 0.5036 0.058 Uiso 1 1 calc R . . H64C H 0.6652 0.7237 0.4172 0.058 Uiso 1 1 calc R . . C65 C 0.8129(17) 0.8561(11) 0.4136(14) 0.029(5) Uiso 1 1 d . . . H65A H 0.7569 0.8882 0.4052 0.044 Uiso 1 1 calc R . . H65B H 0.8518 0.8694 0.3753 0.044 Uiso 1 1 calc R . . H65C H 0.8567 0.8570 0.4758 0.044 Uiso 1 1 calc R . . C66 C 0.9616(14) 0.7560(10) 0.3549(12) 0.016(4) Uiso 1 1 d . . . H66A H 0.9995 0.7929 0.3961 0.019 Uiso 1 1 calc R . . C67 C 1.0372(15) 0.7014(11) 0.3489(13) 0.026(5) Uiso 1 1 d . . . H67A H 1.0854 0.7218 0.3237 0.039 Uiso 1 1 calc R . . H67B H 1.0013 0.6637 0.3109 0.039 Uiso 1 1 calc R . . H67C H 1.0734 0.6837 0.4085 0.039 Uiso 1 1 calc R . . C68 C 0.9121(18) 0.7889(13) 0.2600(15) 0.036(5) Uiso 1 1 d . . . H68A H 0.9650 0.8080 0.2393 0.054 Uiso 1 1 calc R . . H68B H 0.8659 0.8257 0.2634 0.054 Uiso 1 1 calc R . . H68C H 0.8747 0.7536 0.2183 0.054 Uiso 1 1 calc R . . C69 C 0.8642(15) 0.5413(11) 0.6349(13) 0.023(4) Uiso 1 1 d . . . H69A H 0.9080 0.5617 0.6921 0.027 Uiso 1 1 calc R . . C70 C 0.7598(18) 0.5735(14) 0.6205(16) 0.036(5) Uiso 1 1 d . . . H70A H 0.7323 0.5558 0.6652 0.055 Uiso 1 1 calc R . . H70B H 0.7143 0.5617 0.5610 0.055 Uiso 1 1 calc R . . H70C H 0.7665 0.6236 0.6261 0.055 Uiso 1 1 calc R . . C71 C 0.8644(17) 0.4642(12) 0.6547(15) 0.033(5) Uiso 1 1 d . . . H71A H 0.8314 0.4564 0.6992 0.050 Uiso 1 1 calc R . . H71B H 0.9341 0.4476 0.6775 0.050 Uiso 1 1 calc R . . H71C H 0.8279 0.4395 0.6001 0.050 Uiso 1 1 calc R . . C72 C 1.0408(16) 0.5202(12) 0.5828(14) 0.028(5) Uiso 1 1 d . . . H72A H 1.0240 0.4702 0.5755 0.033 Uiso 1 1 calc R . . C73 C 1.099(2) 0.5406(15) 0.5200(18) 0.045(6) Uiso 1 1 d . . . H73A H 1.1618 0.5143 0.5352 0.068 Uiso 1 1 calc R . . H73B H 1.1143 0.5898 0.5262 0.068 Uiso 1 1 calc R . . H73C H 1.0575 0.5306 0.4585 0.068 Uiso 1 1 calc R . . C74 C 1.1061(16) 0.5340(12) 0.6774(13) 0.026(4) Uiso 1 1 d . . . H74A H 1.1684 0.5071 0.6912 0.039 Uiso 1 1 calc R . . H74B H 1.0697 0.5207 0.7177 0.039 Uiso 1 1 calc R . . H74C H 1.1227 0.5830 0.6847 0.039 Uiso 1 1 calc R . . O75 O 1.0669(11) 0.8575(6) 0.5418(9) 0.022(3) Uani 1 1 d . . . C75 C 1.0744(15) 0.8020(11) 0.5835(13) 0.022(4) Uiso 1 1 d . . . C76 C 1.0022(15) 0.7773(11) 0.6236(13) 0.019(4) Uiso 1 1 d . . . H76A H 0.9401 0.8014 0.6096 0.023 Uiso 1 1 calc R . . C77 C 1.0156(16) 0.7222(12) 0.6801(14) 0.022(4) Uiso 1 1 d . . . H77A H 1.0646 0.6888 0.6792 0.026 Uiso 1 1 calc R . . C78 C 0.9574(16) 0.7112(12) 0.7435(14) 0.027(5) Uiso 1 1 d . . . C79 C 0.9912(16) 0.6709(11) 0.8182(14) 0.028(5) Uiso 1 1 d . . . H79A H 1.0560 0.6503 0.8335 0.034 Uiso 1 1 calc R . . C80 C 0.9326(16) 0.6600(12) 0.8717(15) 0.029(5) Uiso 1 1 d . . . H80A H 0.9598 0.6339 0.9246 0.035 Uiso 1 1 calc R . . C81 C 0.8359(14) 0.6856(12) 0.8509(12) 0.024(4) Uiso 1 1 d . . . H81A H 0.7933 0.6739 0.8842 0.028 Uiso 1 1 calc R . . C82 C 0.8035(17) 0.7314(12) 0.7752(15) 0.031(5) Uiso 1 1 d . . . H82A H 0.7408 0.7546 0.7616 0.037 Uiso 1 1 calc R . . C83 C 0.8606(14) 0.7411(10) 0.7247(13) 0.019(4) Uiso 1 1 d . . . H83A H 0.8355 0.7695 0.6736 0.022 Uiso 1 1 calc R . . C84 C 1.1625(14) 0.7562(11) 0.5853(13) 0.019(4) Uiso 1 1 d . . . H84A H 1.1751 0.7168 0.6225 0.023 Uiso 1 1 calc R . . C85 C 1.2188(18) 0.7670(14) 0.5413(16) 0.035(6) Uiso 1 1 d . . . H85A H 1.2021 0.8066 0.5046 0.042 Uiso 1 1 calc R . . C86 C 1.3106(14) 0.7277(11) 0.5358(13) 0.018(4) Uiso 1 1 d . . . C87 C 1.3537(17) 0.7516(13) 0.4707(16) 0.032(5) Uiso 1 1 d . . . H87A H 1.3252 0.7880 0.4306 0.038 Uiso 1 1 calc R . . C88 C 1.442(2) 0.7162(19) 0.471(2) 0.065(9) Uiso 1 1 d . . . H88A H 1.4750 0.7315 0.4314 0.078 Uiso 1 1 calc R . . C89 C 1.483(2) 0.6644(14) 0.5227(17) 0.039(6) Uiso 1 1 d . . . H89A H 1.5408 0.6420 0.5183 0.047 Uiso 1 1 calc R . . C90 C 1.4352(18) 0.6416(14) 0.5875(16) 0.037(6) Uiso 1 1 d . . . H90A H 1.4645 0.6049 0.6267 0.044 Uiso 1 1 calc R . . C91 C 1.3484(19) 0.6728(14) 0.5923(17) 0.041(6) Uiso 1 1 d . . . H91A H 1.3163 0.6572 0.6327 0.050 Uiso 1 1 calc R . . O92 O 0.756(2) 0.9859(18) 0.7716(17) 0.117(13) Uani 1 1 d . . . C93 C 0.749(2) 1.0423(18) 0.718(2) 0.058(8) Uiso 1 1 d . . . H93A H 0.6844 1.0659 0.7125 0.070 Uiso 1 1 calc R . . H93B H 0.8039 1.0743 0.7486 0.070 Uiso 1 1 calc R . . C94 C 0.751(2) 1.0325(14) 0.6404(17) 0.044(6) Uiso 1 1 d . . . H94A H 0.8113 1.0555 0.6339 0.053 Uiso 1 1 calc R . . H94B H 0.6905 1.0525 0.5963 0.053 Uiso 1 1 calc R . . C95 C 0.756(3) 0.9617(18) 0.625(2) 0.065(9) Uiso 1 1 d . . . H95A H 0.8154 0.9502 0.6080 0.079 Uiso 1 1 calc R . . H95B H 0.6942 0.9460 0.5775 0.079 Uiso 1 1 calc R . . C96 C 0.763(2) 0.9294(18) 0.714(2) 0.062(8) Uiso 1 1 d . . . H96A H 0.8279 0.9049 0.7393 0.074 Uiso 1 1 calc R . . H96B H 0.7074 0.8964 0.7066 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0157(7) 0.0098(7) 0.0100(6) -0.0033(6) 0.0001(5) -0.0029(6) P1 0.014(2) 0.013(2) 0.012(2) 0.0027(19) 0.0047(17) -0.0041(18) P2 0.017(2) 0.011(2) 0.018(2) -0.002(2) 0.0044(18) -0.003(2) O25 0.020(7) 0.019(8) 0.029(8) -0.014(7) -0.002(6) -0.007(6) O42 0.063(13) 0.089(18) 0.073(14) -0.045(14) 0.040(12) -0.039(12) Pd51 0.0156(7) 0.0094(7) 0.0080(6) -0.0009(5) 0.0002(5) -0.0008(5) P51 0.012(2) 0.016(3) 0.010(2) -0.0039(19) -0.0007(17) 0.0004(19) P52 0.011(2) 0.019(3) 0.007(2) -0.0033(19) -0.0027(16) 0.000(2) O75 0.042(9) 0.001(6) 0.016(7) 0.000(5) -0.001(6) 0.000(6) O92 0.14(3) 0.12(3) 0.060(15) -0.024(18) -0.011(15) 0.07(2) _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 C26 2.16(2) . ? Pd1 C27 2.159(19) . ? Pd1 P1 2.314(5) . ? Pd1 P2 2.332(5) . ? P1 C16 1.84(2) . ? P1 C13 1.87(2) . ? P1 C1 1.871(19) . ? P2 C22 1.88(2) . ? P2 C12 1.85(2) . ? P2 C19 1.88(2) . ? C1 C2 1.52(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.38(3) . ? C2 C11 1.44(3) . ? C3 C4 1.39(3) . ? C3 H3A 0.9500 . ? C4 C5 1.38(3) . ? C4 H4A 0.9500 . ? C5 C6 1.39(3) . ? C5 H5A 0.9500 . ? C6 C11 1.40(3) . ? C6 C7 1.41(3) . ? C7 C8 1.34(3) . ? C7 H7A 0.9500 . ? C8 C9 1.39(3) . ? C8 H8A 0.9500 . ? C9 C10 1.39(2) . ? C9 H9A 0.9500 . ? C10 C11 1.44(3) . ? C10 C12 1.57(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.49(3) . ? C13 C14 1.65(3) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.56(3) . ? C16 C18 1.55(3) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.43(3) . ? C19 C21 1.54(3) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.51(3) . ? C22 C24 1.57(3) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O25 C25 1.25(3) . ? C25 C26 1.40(3) . ? C25 C34 1.51(3) . ? C26 C27 1.48(3) . ? C26 H26A 0.9500 . ? C27 C28 1.52(3) . ? C27 H27A 0.9500 . ? C28 C33 1.35(3) . ? C28 C29 1.44(3) . ? C29 C30 1.37(3) . ? C29 H29A 0.9500 . ? C30 C31 1.38(4) . ? C30 H30A 0.9500 . ? C31 C32 1.37(4) . ? C31 H31A 0.9500 . ? C32 C33 1.48(4) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.34(3) . ? C34 H34A 0.9500 . ? C35 C36 1.48(3) . ? C35 H35A 0.9500 . ? C36 C37 1.36(3) . ? C36 C41 1.37(3) . ? C37 C38 1.43(3) . ? C37 H37A 0.9500 . ? C38 C39 1.36(3) . ? C38 H38A 0.9500 . ? C39 C40 1.37(4) . ? C39 H39A 0.9500 . ? C40 C41 1.36(4) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? O42 C43 1.43(4) . ? O42 C46 1.42(4) . ? C43 C44 1.57(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.48(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.53(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? Pd51 C77 2.11(2) . ? Pd51 C76 2.13(2) . ? Pd51 P52 2.285(6) . ? Pd51 P51 2.330(5) . ? P51 C63 1.82(2) . ? P51 C66 1.847(19) . ? P51 C51 1.87(2) . ? P52 C69 1.85(2) . ? P52 C72 1.87(2) . ? P52 C62 1.92(2) . ? C51 C52 1.55(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.40(3) . ? C52 C61 1.43(3) . ? C53 C54 1.43(3) . ? C53 H53A 0.9500 . ? C54 C55 1.36(3) . ? C54 H54A 0.9500 . ? C55 C56 1.46(3) . ? C55 H55A 0.9500 . ? C56 C57 1.39(3) . ? C56 C61 1.44(3) . ? C57 C58 1.40(3) . ? C57 H57A 0.9500 . ? C58 C59 1.41(3) . ? C58 H58A 0.9500 . ? C59 C60 1.39(3) . ? C59 H59A 0.9500 . ? C60 C61 1.45(3) . ? C60 C62 1.54(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C65 1.49(3) . ? C63 C64 1.54(3) . ? C63 H63A 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.53(3) . ? C66 C68 1.58(3) . ? C66 H66A 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.54(3) . ? C69 C71 1.53(3) . ? C69 H69A 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.54(3) . ? C72 C74 1.51(3) . ? C72 H72A 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? O75 C75 1.26(2) . ? C75 C76 1.45(3) . ? C75 C84 1.52(3) . ? C76 C77 1.37(3) . ? C76 H76A 0.9500 . ? C77 C78 1.51(3) . ? C77 H77A 0.9500 . ? C78 C79 1.37(3) . ? C78 C83 1.42(3) . ? C79 C80 1.38(3) . ? C79 H79A 0.9500 . ? C80 C81 1.38(3) . ? C80 H80A 0.9500 . ? C81 C82 1.45(3) . ? C81 H81A 0.9500 . ? C82 C83 1.33(3) . ? C82 H82A 0.9500 . ? C83 H83A 0.9500 . ? C84 C85 1.24(3) . ? C84 H84A 0.9500 . ? C85 C86 1.53(3) . ? C85 H85A 0.9500 . ? C86 C91 1.39(3) . ? C86 C87 1.44(3) . ? C87 C88 1.42(4) . ? C87 H87A 0.9500 . ? C88 C89 1.30(4) . ? C88 H88A 0.9500 . ? C89 C90 1.47(4) . ? C89 H89A 0.9500 . ? C90 C91 1.39(4) . ? C90 H90A 0.9500 . ? C91 H91A 0.9500 . ? O92 C93 1.38(5) . ? O92 C96 1.46(4) . ? C93 C94 1.26(4) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.41(4) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.52(4) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? 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 C26 Pd1 C27 40.0(8) . . ? C26 Pd1 P1 110.3(6) . . ? C27 Pd1 P1 150.1(6) . . ? C26 Pd1 P2 146.0(6) . . ? C27 Pd1 P2 106.2(6) . . ? P1 Pd1 P2 103.65(18) . . ? C16 P1 C13 102.8(9) . . ? C16 P1 C1 100.6(9) . . ? C13 P1 C1 105.0(9) . . ? C16 P1 Pd1 114.8(6) . . ? C13 P1 Pd1 114.3(7) . . ? C1 P1 Pd1 117.5(6) . . ? C22 P2 C12 96.4(9) . . ? C22 P2 C19 105.9(10) . . ? C12 P2 C19 105.8(10) . . ? C22 P2 Pd1 109.5(7) . . ? C12 P2 Pd1 124.9(7) . . ? C19 P2 Pd1 112.0(8) . . ? C2 C1 P1 115.6(12) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C11 116.8(16) . . ? C3 C2 C1 114.3(16) . . ? C11 C2 C1 128.8(15) . . ? C4 C3 C2 124.4(19) . . ? C4 C3 H3A 117.7 . . ? C2 C3 H3A 117.8 . . ? C3 C4 C5 118(2) . . ? C3 C4 H4A 121.0 . . ? C5 C4 H4A 120.9 . . ? C6 C5 C4 120(2) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C11 121.5(19) . . ? C5 C6 C7 116.7(18) . . ? C11 C6 C7 121.5(17) . . ? C8 C7 C6 121.9(17) . . ? C8 C7 H7A 119.1 . . ? C6 C7 H7A 119.1 . . ? C7 C8 C9 118.1(18) . . ? C7 C8 H8A 121.0 . . ? C9 C8 H8A 120.9 . . ? C10 C9 C8 122.6(17) . . ? C10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? C9 C10 C11 119.6(16) . . ? C9 C10 C12 110.6(16) . . ? C11 C10 C12 129.5(17) . . ? C6 C11 C10 115.9(17) . . ? C6 C11 C2 118.3(16) . . ? C10 C11 C2 125.7(16) . . ? C10 C12 P2 120.3(13) . . ? C10 C12 H12A 107.3 . . ? P2 C12 H12A 107.3 . . ? C10 C12 H12B 107.2 . . ? P2 C12 H12B 107.2 . . ? H12A C12 H12B 106.9 . . ? C15 C13 C14 104.7(17) . . ? C15 C13 P1 109.3(15) . . ? C14 C13 P1 105.5(14) . . ? C15 C13 H13A 112.2 . . ? C14 C13 H13A 112.3 . . ? P1 C13 H13A 112.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 111.3(16) . . ? C17 C16 P1 110.5(14) . . ? C18 C16 P1 117.1(14) . . ? C17 C16 H16A 105.7 . . ? C18 C16 H16A 105.7 . . ? P1 C16 H16A 105.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.4 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 115(2) . . ? C20 C19 P2 112.5(18) . . ? C21 C19 P2 115.9(15) . . ? C20 C19 H19A 103.8 . . ? C21 C19 H19A 103.8 . . ? P2 C19 H19A 103.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.4 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.4 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 108.2(17) . . ? C23 C22 P2 111.5(15) . . ? C24 C22 P2 113.7(14) . . ? C23 C22 H22A 107.8 . . ? C24 C22 H22A 107.8 . . ? P2 C22 H22A 107.8 . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.4 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O25 C25 C26 122.0(19) . . ? O25 C25 C34 118.6(18) . . ? C26 C25 C34 119.3(19) . . ? C25 C26 C27 124.8(19) . . ? C25 C26 Pd1 100.2(14) . . ? C27 C26 Pd1 69.9(11) . . ? C25 C26 H26A 117.6 . . ? C27 C26 H26A 117.6 . . ? Pd1 C26 H26A 100.4 . . ? C28 C27 C26 118.6(17) . . ? C28 C27 Pd1 116.4(13) . . ? C26 C27 Pd1 70.1(11) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? Pd1 C27 H27A 84.2 . . ? C33 C28 C27 122(2) . . ? C33 C28 C29 122(2) . . ? C27 C28 C29 114.9(18) . . ? C30 C29 C28 118(2) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.8 . . ? C29 C30 C31 119(2) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.3 . . ? C32 C31 C30 125(3) . . ? C32 C31 H31A 117.6 . . ? C30 C31 H31A 117.7 . . ? C31 C32 C33 116(3) . . ? C31 C32 H32A 121.9 . . ? C33 C32 H32A 121.9 . . ? C28 C33 C32 119(2) . . ? C28 C33 H33A 120.7 . . ? C32 C33 H33A 120.7 . . ? C35 C34 C25 123(2) . . ? C35 C34 H34A 118.3 . . ? C25 C34 H34A 118.3 . . ? C34 C35 C36 127(2) . . ? C34 C35 H35A 116.3 . . ? C36 C35 H35A 116.3 . . ? C37 C36 C41 117(2) . . ? C37 C36 C35 121(2) . . ? C41 C36 C35 122(2) . . ? C36 C37 C38 122(2) . . ? C36 C37 H37A 119.1 . . ? C38 C37 H37A 119.2 . . ? C39 C38 C37 119(2) . . ? C39 C38 H38A 120.7 . . ? C37 C38 H38A 120.6 . . ? C38 C39 C40 119(2) . . ? C38 C39 H39A 120.4 . . ? C40 C39 H39A 120.5 . . ? C39 C40 C41 121(3) . . ? C39 C40 H40A 119.4 . . ? C41 C40 H40A 119.5 . . ? C36 C41 C40 122(2) . . ? C36 C41 H41A 118.9 . . ? C40 C41 H41A 119.1 . . ? C43 O42 C46 109(3) . . ? O42 C43 C44 105(2) . . ? O42 C43 H43A 110.8 . . ? C44 C43 H43A 110.9 . . ? O42 C43 H43B 110.8 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.9 . . ? C45 C44 C43 104(3) . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44B 111.0 . . ? C43 C44 H44B 111.0 . . ? H44A C44 H44B 109.0 . . ? C44 C45 C46 100(3) . . ? C44 C45 H45A 111.9 . . ? C46 C45 H45A 111.9 . . ? C44 C45 H45B 111.8 . . ? C46 C45 H45B 111.9 . . ? H45A C45 H45B 109.6 . . ? O42 C46 C45 108(3) . . ? O42 C46 H46A 110.2 . . ? C45 C46 H46A 110.1 . . ? O42 C46 H46B 110.1 . . ? C45 C46 H46B 110.1 . . ? H46A C46 H46B 108.4 . . ? C77 Pd51 C76 37.8(8) . . ? C77 Pd51 P52 108.5(6) . . ? C76 Pd51 P52 146.2(5) . . ? C77 Pd51 P51 145.8(6) . . ? C76 Pd51 P51 108.1(6) . . ? P52 Pd51 P51 105.68(18) . . ? C63 P51 C66 106.9(9) . . ? C63 P51 C51 105.1(9) . . ? C66 P51 C51 100.5(9) . . ? C63 P51 Pd51 110.8(7) . . ? C66 P51 Pd51 111.2(6) . . ? C51 P51 Pd51 121.1(7) . . ? C69 P52 C72 102.1(9) . . ? C69 P52 C62 108.3(9) . . ? C72 P52 C62 94.8(9) . . ? C69 P52 Pd51 115.0(7) . . ? C72 P52 Pd51 114.7(7) . . ? C62 P52 Pd51 118.9(7) . . ? C52 C51 P51 116.9(14) . . ? C52 C51 H51A 108.1 . . ? P51 C51 H51A 108.1 . . ? C52 C51 H51B 108.1 . . ? P51 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? C53 C52 C61 121.0(18) . . ? C53 C52 C51 109.7(18) . . ? C61 C52 C51 129.3(18) . . ? C52 C53 C54 121.2(18) . . ? C52 C53 H53A 119.4 . . ? C54 C53 H53A 119.4 . . ? C55 C54 C53 119(2) . . ? C55 C54 H54A 120.4 . . ? C53 C54 H54A 120.4 . . ? C54 C55 C56 120.8(19) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C57 C56 C61 122.2(19) . . ? C57 C56 C55 117.7(18) . . ? C61 C56 C55 120.1(18) . . ? C56 C57 C58 120.7(19) . . ? C56 C57 H57A 119.7 . . ? C58 C57 H57A 119.6 . . ? C57 C58 C59 117.6(19) . . ? C57 C58 H58A 121.2 . . ? C59 C58 H58A 121.2 . . ? C60 C59 C58 123.3(19) . . ? C60 C59 H59A 118.3 . . ? C58 C59 H59A 118.4 . . ? C59 C60 C61 118.7(17) . . ? C59 C60 C62 113.3(17) . . ? C61 C60 C62 127.9(17) . . ? C60 C61 C52 126.1(17) . . ? C60 C61 C56 116.6(17) . . ? C52 C61 C56 117.0(17) . . ? C60 C62 P52 116.0(13) . . ? C60 C62 H62A 108.3 . . ? P52 C62 H62A 108.3 . . ? C60 C62 H62B 108.3 . . ? P52 C62 H62B 108.3 . . ? H62A C62 H62B 107.4 . . ? C65 C63 C64 110.4(18) . . ? C65 C63 P51 114.7(15) . . ? C64 C63 P51 112.7(16) . . ? C65 C63 H63A 106.1 . . ? C64 C63 H63A 106.1 . . ? P51 C63 H63A 106.1 . . ? C63 C64 H64A 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.4 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C68 108.6(16) . . ? C67 C66 P51 111.0(14) . . ? C68 C66 P51 113.0(14) . . ? C67 C66 H66A 108.1 . . ? C68 C66 H66A 108.0 . . ? P51 C66 H66A 108.0 . . ? C66 C67 H67A 109.4 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.4 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 C71 111.5(19) . . ? C70 C69 P52 112.4(15) . . ? C71 C69 P52 119.0(15) . . ? C70 C69 H69A 104.0 . . ? C71 C69 H69A 104.0 . . ? P52 C69 H69A 104.0 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.4 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.6 . . ? C69 C71 H71B 109.4 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.4 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C74 109.1(19) . . ? C73 C72 P52 108.5(16) . . ? C74 C72 P52 111.3(15) . . ? C73 C72 H72A 109.3 . . ? C74 C72 H72A 109.3 . . ? P52 C72 H72A 109.3 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.4 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.4 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O75 C75 C76 125(2) . . ? O75 C75 C84 116.2(18) . . ? C76 C75 C84 118.9(19) . . ? C77 C76 C75 125.8(19) . . ? C77 C76 Pd51 70.6(12) . . ? C75 C76 Pd51 103.1(13) . . ? C77 C76 H76A 117.1 . . ? C75 C76 H76A 117.1 . . ? Pd51 C76 H76A 96.6 . . ? C76 C77 C78 124.2(19) . . ? C76 C77 Pd51 71.6(12) . . ? C78 C77 Pd51 115.2(14) . . ? C76 C77 H77A 117.9 . . ? C78 C77 H77A 117.9 . . ? Pd51 C77 H77A 83.3 . . ? C79 C78 C83 116.8(19) . . ? C79 C78 C77 123.6(19) . . ? C83 C78 C77 119.6(19) . . ? C78 C79 C80 121(2) . . ? C78 C79 H79A 119.5 . . ? C80 C79 H79A 119.4 . . ? C81 C80 C79 122(2) . . ? C81 C80 H80A 118.8 . . ? C79 C80 H80A 118.9 . . ? C80 C81 C82 115.9(18) . . ? C80 C81 H81A 122.1 . . ? C82 C81 H81A 122.1 . . ? C83 C82 C81 121(2) . . ? C83 C82 H82A 119.7 . . ? C81 C82 H82A 119.7 . . ? C82 C83 C78 123(2) . . ? C82 C83 H83A 118.5 . . ? C78 C83 H83A 118.6 . . ? C85 C84 C75 124(2) . . ? C85 C84 H84A 118.0 . . ? C75 C84 H84A 117.9 . . ? C84 C85 C86 131(2) . . ? C84 C85 H85A 114.4 . . ? C86 C85 H85A 114.4 . . ? C91 C86 C85 119.9(19) . . ? C91 C86 C87 124(2) . . ? C85 C86 C87 116(2) . . ? C88 C87 C86 114(2) . . ? C88 C87 H87A 122.7 . . ? C86 C87 H87A 122.9 . . ? C89 C88 C87 125(3) . . ? C89 C88 H88A 117.2 . . ? C87 C88 H88A 117.5 . . ? C88 C89 C90 118(3) . . ? C88 C89 H89A 121.1 . . ? C90 C89 H89A 120.8 . . ? C91 C90 C89 121(2) . . ? C91 C90 H90A 119.3 . . ? C89 C90 H90A 119.5 . . ? C90 C91 C86 117(2) . . ? C90 C91 H91A 121.4 . . ? C86 C91 H91A 121.5 . . ? C93 O92 C96 103(3) . . ? C94 C93 O92 118(3) . . ? C94 C93 H93A 108.0 . . ? O92 C93 H93A 108.0 . . ? C94 C93 H93B 107.7 . . ? O92 C93 H93B 107.7 . . ? H93A C93 H93B 107.2 . . ? C93 C94 C95 110(3) . . ? C93 C94 H94A 109.9 . . ? C95 C94 H94A 109.8 . . ? C93 C94 H94B 109.6 . . ? C95 C94 H94B 109.7 . . ? H94A C94 H94B 108.2 . . ? C94 C95 C96 104(3) . . ? C94 C95 H95A 111.0 . . ? C96 C95 H95A 111.0 . . ? C94 C95 H95B 111.1 . . ? C96 C95 H95B 111.1 . . ? H95A C95 H95B 109.0 . . ? C95 C96 O92 106(3) . . ? C95 C96 H96A 110.6 . . ? O92 C96 H96A 110.5 . . ? C95 C96 H96B 110.4 . . ? O92 C96 H96B 110.5 . . ? H96A C96 H96B 108.7 . . ? 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 C26 Pd1 P1 C16 -53.9(9) . . . . ? C27 Pd1 P1 C16 -58.9(13) . . . . ? P2 Pd1 P1 C16 123.6(8) . . . . ? C26 Pd1 P1 C13 64.5(9) . . . . ? C27 Pd1 P1 C13 59.5(13) . . . . ? P2 Pd1 P1 C13 -118.0(8) . . . . ? C26 Pd1 P1 C1 -171.8(8) . . . . ? C27 Pd1 P1 C1 -176.9(12) . . . . ? P2 Pd1 P1 C1 5.6(7) . . . . ? C26 Pd1 P2 C22 65.7(12) . . . . ? C27 Pd1 P2 C22 71.3(9) . . . . ? P1 Pd1 P2 C22 -110.0(7) . . . . ? C26 Pd1 P2 C12 178.8(12) . . . . ? C27 Pd1 P2 C12 -175.7(9) . . . . ? P1 Pd1 P2 C12 3.1(8) . . . . ? C26 Pd1 P2 C19 -51.4(12) . . . . ? C27 Pd1 P2 C19 -45.9(9) . . . . ? P1 Pd1 P2 C19 132.8(8) . . . . ? C16 P1 C1 C2 143.8(13) . . . . ? C13 P1 C1 C2 37.4(15) . . . . ? Pd1 P1 C1 C2 -90.9(13) . . . . ? P1 C1 C2 C3 -88.6(17) . . . . ? P1 C1 C2 C11 93(2) . . . . ? C11 C2 C3 C4 -5(3) . . . . ? C1 C2 C3 C4 176.8(19) . . . . ? C2 C3 C4 C5 0(3) . . . . ? C3 C4 C5 C6 3(3) . . . . ? C4 C5 C6 C11 -2(3) . . . . ? C4 C5 C6 C7 172.1(19) . . . . ? C5 C6 C7 C8 -175.5(19) . . . . ? C11 C6 C7 C8 -1(3) . . . . ? C6 C7 C8 C9 2(3) . . . . ? C7 C8 C9 C10 -4(3) . . . . ? C8 C9 C10 C11 7(3) . . . . ? C8 C9 C10 C12 -177.9(17) . . . . ? C5 C6 C11 C10 177.3(19) . . . . ? C7 C6 C11 C10 4(3) . . . . ? C5 C6 C11 C2 -3(3) . . . . ? C7 C6 C11 C2 -176.7(17) . . . . ? C9 C10 C11 C6 -6(3) . . . . ? C12 C10 C11 C6 179.6(18) . . . . ? C9 C10 C11 C2 174.2(17) . . . . ? C12 C10 C11 C2 0(3) . . . . ? C3 C2 C11 C6 6(3) . . . . ? C1 C2 C11 C6 -175.9(18) . . . . ? C3 C2 C11 C10 -174.1(18) . . . . ? C1 C2 C11 C10 4(3) . . . . ? C9 C10 C12 P2 98.9(18) . . . . ? C11 C10 C12 P2 -86(2) . . . . ? C22 P2 C12 C10 -171.0(16) . . . . ? C19 P2 C12 C10 -62.4(17) . . . . ? Pd1 P2 C12 C10 69.8(17) . . . . ? C16 P1 C13 C15 56.9(16) . . . . ? C1 P1 C13 C15 161.7(14) . . . . ? Pd1 P1 C13 C15 -68.1(15) . . . . ? C16 P1 C13 C14 169.0(13) . . . . ? C1 P1 C13 C14 -86.2(14) . . . . ? Pd1 P1 C13 C14 44.0(15) . . . . ? C13 P1 C16 C17 172.9(14) . . . . ? C1 P1 C16 C17 64.7(15) . . . . ? Pd1 P1 C16 C17 -62.4(15) . . . . ? C13 P1 C16 C18 44.1(18) . . . . ? C1 P1 C16 C18 -64.1(17) . . . . ? Pd1 P1 C16 C18 168.8(14) . . . . ? C22 P2 C19 C20 -177.8(18) . . . . ? C12 P2 C19 C20 81(2) . . . . ? Pd1 P2 C19 C20 -58.5(19) . . . . ? C22 P2 C19 C21 46.8(18) . . . . ? C12 P2 C19 C21 -54.8(18) . . . . ? Pd1 P2 C19 C21 166.1(13) . . . . ? C12 P2 C22 C23 -76.8(16) . . . . ? C19 P2 C22 C23 174.8(16) . . . . ? Pd1 P2 C22 C23 53.8(16) . . . . ? C12 P2 C22 C24 160.7(16) . . . . ? C19 P2 C22 C24 52.2(18) . . . . ? Pd1 P2 C22 C24 -68.7(16) . . . . ? O25 C25 C26 C27 178.5(18) . . . . ? C34 C25 C26 C27 -4(3) . . . . ? O25 C25 C26 Pd1 -109.1(19) . . . . ? C34 C25 C26 Pd1 68.2(19) . . . . ? C27 Pd1 C26 C25 -123.5(19) . . . . ? P1 Pd1 C26 C25 60.4(14) . . . . ? P2 Pd1 C26 C25 -115.2(13) . . . . ? P1 Pd1 C26 C27 -176.1(9) . . . . ? P2 Pd1 C26 C27 8.3(16) . . . . ? C25 C26 C27 C28 -161.5(19) . . . . ? Pd1 C26 C27 C28 110.0(16) . . . . ? C25 C26 C27 Pd1 88.5(19) . . . . ? C26 Pd1 C27 C28 -112.9(19) . . . . ? P1 Pd1 C27 C28 -105.5(15) . . . . ? P2 Pd1 C27 C28 72.0(15) . . . . ? P1 Pd1 C27 C26 7.3(17) . . . . ? P2 Pd1 C27 C26 -175.2(10) . . . . ? C26 C27 C28 C33 -31(3) . . . . ? Pd1 C27 C28 C33 49(3) . . . . ? C26 C27 C28 C29 158.9(18) . . . . ? Pd1 C27 C28 C29 -120.4(17) . . . . ? C33 C28 C29 C30 6(3) . . . . ? C27 C28 C29 C30 176(2) . . . . ? C28 C29 C30 C31 -2(4) . . . . ? C29 C30 C31 C32 -3(4) . . . . ? C30 C31 C32 C33 4(5) . . . . ? C27 C28 C33 C32 -174(2) . . . . ? C29 C28 C33 C32 -5(4) . . . . ? C31 C32 C33 C28 0(4) . . . . ? O25 C25 C34 C35 2(3) . . . . ? C26 C25 C34 C35 -175.5(19) . . . . ? C25 C34 C35 C36 -179.7(19) . . . . ? C34 C35 C36 C37 -166(2) . . . . ? C34 C35 C36 C41 12(3) . . . . ? C41 C36 C37 C38 0(3) . . . . ? C35 C36 C37 C38 178(2) . . . . ? C36 C37 C38 C39 0(4) . . . . ? C37 C38 C39 C40 -3(4) . . . . ? C38 C39 C40 C41 5(4) . . . . ? C37 C36 C41 C40 2(4) . . . . ? C35 C36 C41 C40 -176(2) . . . . ? C39 C40 C41 C36 -5(4) . . . . ? C46 O42 C43 C44 5(3) . . . . ? O42 C43 C44 C45 -28(3) . . . . ? C43 C44 C45 C46 37(3) . . . . ? C43 O42 C46 C45 19(4) . . . . ? C44 C45 C46 O42 -36(3) . . . . ? C77 Pd51 P51 C63 -51.7(13) . . . . ? C76 Pd51 P51 C63 -56.0(9) . . . . ? P52 Pd51 P51 C63 124.0(7) . . . . ? C77 Pd51 P51 C66 67.1(13) . . . . ? C76 Pd51 P51 C66 62.8(9) . . . . ? P52 Pd51 P51 C66 -117.2(7) . . . . ? C77 Pd51 P51 C51 -175.5(12) . . . . ? C76 Pd51 P51 C51 -179.8(9) . . . . ? P52 Pd51 P51 C51 0.3(8) . . . . ? C77 Pd51 P52 C69 49.7(9) . . . . ? C76 Pd51 P52 C69 52.3(12) . . . . ? P51 Pd51 P52 C69 -127.8(7) . . . . ? C77 Pd51 P52 C72 -68.3(10) . . . . ? C76 Pd51 P52 C72 -65.7(12) . . . . ? P51 Pd51 P52 C72 114.2(7) . . . . ? C77 Pd51 P52 C62 -179.5(9) . . . . ? C76 Pd51 P52 C62 -176.9(12) . . . . ? P51 Pd51 P52 C62 3.1(7) . . . . ? C63 P51 C51 C52 -49.2(17) . . . . ? C66 P51 C51 C52 -160.1(15) . . . . ? Pd51 P51 C51 C52 77.2(16) . . . . ? P51 C51 C52 C53 91.5(18) . . . . ? P51 C51 C52 C61 -89(3) . . . . ? C61 C52 C53 C54 7(3) . . . . ? C51 C52 C53 C54 -173.0(18) . . . . ? C52 C53 C54 C55 -7(3) . . . . ? C53 C54 C55 C56 1(3) . . . . ? C54 C55 C56 C57 -173(2) . . . . ? C54 C55 C56 C61 6(3) . . . . ? C61 C56 C57 C58 -6(3) . . . . ? C55 C56 C57 C58 172.1(19) . . . . ? C56 C57 C58 C59 5(3) . . . . ? C57 C58 C59 C60 3(3) . . . . ? C58 C59 C60 C61 -10(3) . . . . ? C58 C59 C60 C62 174.2(18) . . . . ? C59 C60 C61 C52 -164.3(19) . . . . ? C62 C60 C61 C52 11(3) . . . . ? C59 C60 C61 C56 9(3) . . . . ? C62 C60 C61 C56 -176.1(18) . . . . ? C53 C52 C61 C60 172.2(19) . . . . ? C51 C52 C61 C60 -8(3) . . . . ? C53 C52 C61 C56 -1(3) . . . . ? C51 C52 C61 C56 180(2) . . . . ? C57 C56 C61 C60 -1(3) . . . . ? C55 C56 C61 C60 -179.3(18) . . . . ? C57 C56 C61 C52 172.7(19) . . . . ? C55 C56 C61 C52 -6(3) . . . . ? C59 C60 C62 P52 -97.6(18) . . . . ? C61 C60 C62 P52 87(2) . . . . ? C69 P52 C62 C60 49.0(17) . . . . ? C72 P52 C62 C60 153.5(15) . . . . ? Pd51 P52 C62 C60 -84.7(15) . . . . ? C66 P51 C63 C65 -42.5(17) . . . . ? C51 P51 C63 C65 -148.7(15) . . . . ? Pd51 P51 C63 C65 78.8(16) . . . . ? C66 P51 C63 C64 -170.0(15) . . . . ? C51 P51 C63 C64 83.8(17) . . . . ? Pd51 P51 C63 C64 -48.6(16) . . . . ? C63 P51 C66 C67 -172.1(13) . . . . ? C51 P51 C66 C67 -62.6(15) . . . . ? Pd51 P51 C66 C67 66.8(14) . . . . ? C63 P51 C66 C68 -49.9(17) . . . . ? C51 P51 C66 C68 59.6(16) . . . . ? Pd51 P51 C66 C68 -171.0(13) . . . . ? C72 P52 C69 C70 -176.9(16) . . . . ? C62 P52 C69 C70 -77.6(18) . . . . ? Pd51 P52 C69 C70 58.2(17) . . . . ? C72 P52 C69 C71 -43.9(19) . . . . ? C62 P52 C69 C71 55.4(18) . . . . ? Pd51 P52 C69 C71 -168.8(14) . . . . ? C69 P52 C72 C73 -179.1(16) . . . . ? C62 P52 C72 C73 71.0(17) . . . . ? Pd51 P52 C72 C73 -54.0(17) . . . . ? C69 P52 C72 C74 -59.1(18) . . . . ? C62 P52 C72 C74 -169.0(16) . . . . ? Pd51 P52 C72 C74 66.0(16) . . . . ? O75 C75 C76 C77 -170(2) . . . . ? C84 C75 C76 C77 15(3) . . . . ? O75 C75 C76 Pd51 114.6(19) . . . . ? C84 C75 C76 Pd51 -61(2) . . . . ? P52 Pd51 C76 C77 -4.0(18) . . . . ? P51 Pd51 C76 C77 176.0(11) . . . . ? C77 Pd51 C76 C75 124(2) . . . . ? P52 Pd51 C76 C75 119.6(13) . . . . ? P51 Pd51 C76 C75 -60.3(14) . . . . ? C75 C76 C77 C78 159(2) . . . . ? Pd51 C76 C77 C78 -108(2) . . . . ? C75 C76 C77 Pd51 -92(2) . . . . ? P52 Pd51 C77 C76 177.6(10) . . . . ? P51 Pd51 C77 C76 -6.7(18) . . . . ? C76 Pd51 C77 C78 120(2) . . . . ? P52 Pd51 C77 C78 -62.5(16) . . . . ? P51 Pd51 C77 C78 113.2(15) . . . . ? C76 C77 C78 C79 -158(2) . . . . ? Pd51 C77 C78 C79 118(2) . . . . ? C76 C77 C78 C83 25(3) . . . . ? Pd51 C77 C78 C83 -59(2) . . . . ? C83 C78 C79 C80 1(3) . . . . ? C77 C78 C79 C80 -177(2) . . . . ? C78 C79 C80 C81 3(3) . . . . ? C79 C80 C81 C82 -7(3) . . . . ? C80 C81 C82 C83 7(3) . . . . ? C81 C82 C83 C78 -3(3) . . . . ? C79 C78 C83 C82 0(3) . . . . ? C77 C78 C83 C82 177(2) . . . . ? O75 C75 C84 C85 -8(3) . . . . ? C76 C75 C84 C85 168(2) . . . . ? C75 C84 C85 C86 179(2) . . . . ? C84 C85 C86 C91 -6(4) . . . . ? C84 C85 C86 C87 175(3) . . . . ? C91 C86 C87 C88 -3(3) . . . . ? C85 C86 C87 C88 176(2) . . . . ? C86 C87 C88 C89 3(4) . . . . ? C87 C88 C89 C90 -2(5) . . . . ? C88 C89 C90 C91 2(4) . . . . ? C89 C90 C91 C86 -2(4) . . . . ? C85 C86 C91 C90 -176(2) . . . . ? C87 C86 C91 C90 3(4) . . . . ? C96 O92 C93 C94 -1(4) . . . . ? O92 C93 C94 C95 4(4) . . . . ? C93 C94 C95 C96 -4(4) . . . . ? C94 C95 C96 O92 3(3) . . . . ? C93 O92 C96 C95 -1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 2.543 _refine_diff_density_min -1.891 _refine_diff_density_rms 0.250 # Attachment '7_cyclohexPnapth_dba_CH.cif' data_sasol43 _database_code_depnum_ccdc_archive 'CCDC 295574' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H68 O P2 Pd' _chemical_formula_sum 'C53 H68 O P2 Pd' _chemical_formula_weight 889.41 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)/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 11.042(2) _cell_length_b 18.354(4) _cell_length_c 22.234(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.183(6) _cell_angle_gamma 90.00 _cell_volume 4505.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11963 _cell_measurement_theta_min 2.0570 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Platelet _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84736 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26520 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7951 _reflns_number_gt 5884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.8365P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 7951 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.08489(2) 0.252251(17) 0.388461(14) 0.02274(11) Uani 1 1 d . . . P1 P 0.11956(9) 0.13774(6) 0.34790(5) 0.0256(3) Uani 1 1 d . . . C1 C 0.0862(3) 0.0514(2) 0.38877(19) 0.0285(10) Uani 1 1 d . . . H1A H 0.0057 0.0570 0.4077 0.034 Uiso 1 1 calc R . . H1B H 0.0786 0.0123 0.3583 0.034 Uiso 1 1 calc R . . C2 C 0.1732(3) 0.0246(2) 0.4370(2) 0.0288(10) Uani 1 1 d . . . C3 C 0.2618(4) -0.0228(2) 0.4152(2) 0.0355(11) Uani 1 1 d . . . H3A H 0.2604 -0.0354 0.3738 0.043 Uiso 1 1 calc R . . C4 C 0.3527(4) -0.0526(2) 0.4519(2) 0.0398(12) Uani 1 1 d . . . H4A H 0.4125 -0.0838 0.4352 0.048 Uiso 1 1 calc R . . C5 C 0.3546(4) -0.0367(2) 0.5111(2) 0.0371(12) Uani 1 1 d . . . H5A H 0.4165 -0.0566 0.5359 0.045 Uiso 1 1 calc R . . C6 C 0.2659(4) 0.0091(2) 0.5368(2) 0.0327(11) Uani 1 1 d . . . C7 C 0.2694(4) 0.0222(3) 0.5997(2) 0.0365(12) Uani 1 1 d . . . H7A H 0.3335 0.0020 0.6229 0.044 Uiso 1 1 calc R . . C8 C 0.1843(4) 0.0626(3) 0.6272(2) 0.0366(11) Uani 1 1 d . . . H8A H 0.1876 0.0706 0.6694 0.044 Uiso 1 1 calc R . . C9 C 0.0906(4) 0.0927(2) 0.5925(2) 0.0339(11) Uani 1 1 d . . . H9A H 0.0285 0.1189 0.6126 0.041 Uiso 1 1 calc R . . C10 C 0.0837(3) 0.0863(2) 0.5314(2) 0.0298(10) Uani 1 1 d . . . C11 C 0.1711(3) 0.0420(2) 0.50011(19) 0.0269(10) Uani 1 1 d . . . C12 C -0.0177(3) 0.1313(2) 0.5035(2) 0.0322(11) Uani 1 1 d . . . H12A H -0.0872 0.1312 0.5315 0.039 Uiso 1 1 calc R . . H12B H -0.0444 0.1070 0.4660 0.039 Uiso 1 1 calc R . . P2 P 0.02090(9) 0.22815(6) 0.48538(5) 0.0258(3) Uani 1 1 d . . . C13 C 0.2815(3) 0.1286(2) 0.32624(19) 0.0293(10) Uani 1 1 d . . . H13A H 0.2995 0.0761 0.3183 0.035 Uiso 1 1 calc R . . C14 C 0.3598(3) 0.1547(2) 0.3795(2) 0.0316(10) Uani 1 1 d . . . H14A H 0.3343 0.2044 0.3912 0.038 Uiso 1 1 calc R . . H14B H 0.3465 0.1221 0.4144 0.038 Uiso 1 1 calc R . . C15 C 0.4951(4) 0.1553(3) 0.3638(2) 0.0409(12) Uani 1 1 d . . . H15A H 0.5424 0.1731 0.3988 0.049 Uiso 1 1 calc R . . H15B H 0.5222 0.1052 0.3545 0.049 Uiso 1 1 calc R . . C16 C 0.5179(4) 0.2039(3) 0.3104(2) 0.0398(12) Uani 1 1 d . . . H16A H 0.6054 0.2044 0.3009 0.048 Uiso 1 1 calc R . . H16B H 0.4927 0.2544 0.3198 0.048 Uiso 1 1 calc R . . C17 C 0.4464(3) 0.1759(3) 0.2563(2) 0.0393(12) Uani 1 1 d . . . H17A H 0.4754 0.1265 0.2456 0.047 Uiso 1 1 calc R . . H17B H 0.4605 0.2083 0.2214 0.047 Uiso 1 1 calc R . . C18 C 0.3108(3) 0.1728(2) 0.26971(19) 0.0313(10) Uani 1 1 d . . . H18A H 0.2681 0.1510 0.2349 0.038 Uiso 1 1 calc R . . H18B H 0.2800 0.2231 0.2749 0.038 Uiso 1 1 calc R . . C19 C 0.0273(3) 0.1233(2) 0.27915(19) 0.0268(10) Uani 1 1 d . . . H19A H 0.0481 0.1640 0.2511 0.032 Uiso 1 1 calc R . . C20 C 0.0481(4) 0.0520(2) 0.2437(2) 0.0350(11) Uani 1 1 d . . . H20A H 0.1339 0.0492 0.2313 0.042 Uiso 1 1 calc R . . H20B H 0.0312 0.0098 0.2702 0.042 Uiso 1 1 calc R . . C21 C -0.0329(4) 0.0476(3) 0.1882(2) 0.0368(11) Uani 1 1 d . . . H21A H -0.0107 0.0870 0.1599 0.044 Uiso 1 1 calc R . . H21B H -0.0197 0.0004 0.1677 0.044 Uiso 1 1 calc R . . C22 C -0.1645(4) 0.0548(3) 0.2046(2) 0.0405(12) Uani 1 1 d . . . H22A H -0.1887 0.0132 0.2302 0.049 Uiso 1 1 calc R . . H22B H -0.2146 0.0535 0.1675 0.049 Uiso 1 1 calc R . . C23 C -0.1872(4) 0.1258(3) 0.2379(2) 0.0468(14) Uani 1 1 d . . . H23A H -0.2734 0.1282 0.2499 0.056 Uiso 1 1 calc R . . H23B H -0.1707 0.1673 0.2107 0.056 Uiso 1 1 calc R . . C24 C -0.1071(3) 0.1322(3) 0.2940(2) 0.0350(11) Uani 1 1 d . . . H24A H -0.1201 0.1804 0.3128 0.042 Uiso 1 1 calc R . . H24B H -0.1310 0.0944 0.3234 0.042 Uiso 1 1 calc R . . C25 C 0.1167(3) 0.2584(2) 0.54931(19) 0.0285(10) Uani 1 1 d . . . H25A H 0.0866 0.2349 0.5870 0.034 Uiso 1 1 calc R . . C26 C 0.1100(4) 0.3417(3) 0.5567(2) 0.0373(11) Uani 1 1 d . . . H26A H 0.0256 0.3560 0.5658 0.045 Uiso 1 1 calc R . . H26B H 0.1336 0.3653 0.5185 0.045 Uiso 1 1 calc R . . C27 C 0.1941(4) 0.3684(3) 0.6075(2) 0.0442(12) Uani 1 1 d . . . H27A H 0.1916 0.4223 0.6093 0.053 Uiso 1 1 calc R . . H27B H 0.1645 0.3494 0.6465 0.053 Uiso 1 1 calc R . . C28 C 0.3252(4) 0.3435(3) 0.5979(2) 0.0451(13) Uani 1 1 d . . . H28A H 0.3582 0.3664 0.5612 0.054 Uiso 1 1 calc R . . H28B H 0.3758 0.3588 0.6325 0.054 Uiso 1 1 calc R . . C29 C 0.3288(4) 0.2610(3) 0.5917(2) 0.0397(12) Uani 1 1 d . . . H29A H 0.2999 0.2383 0.6294 0.048 Uiso 1 1 calc R . . H29B H 0.4133 0.2450 0.5850 0.048 Uiso 1 1 calc R . . C30 C 0.2495(4) 0.2355(2) 0.5393(2) 0.0329(11) Uani 1 1 d . . . H30A H 0.2544 0.1818 0.5357 0.039 Uiso 1 1 calc R . . H30B H 0.2795 0.2571 0.5013 0.039 Uiso 1 1 calc R . . C31 C -0.1281(3) 0.2724(2) 0.49763(19) 0.0292(10) Uani 1 1 d . . . H31A H -0.1125 0.3260 0.4957 0.035 Uiso 1 1 calc R . . C32 C -0.2145(4) 0.2555(2) 0.4448(2) 0.0324(10) Uani 1 1 d . . . H32A H -0.1728 0.2653 0.4062 0.039 Uiso 1 1 calc R . . H32B H -0.2371 0.2033 0.4456 0.039 Uiso 1 1 calc R . . C33 C -0.3291(4) 0.3027(3) 0.4490(2) 0.0407(12) Uani 1 1 d . . . H33A H -0.3069 0.3547 0.4456 0.049 Uiso 1 1 calc R . . H33B H -0.3846 0.2906 0.4154 0.049 Uiso 1 1 calc R . . C34 C -0.3927(4) 0.2895(3) 0.5088(3) 0.0508(14) Uani 1 1 d . . . H34A H -0.4645 0.3216 0.5115 0.061 Uiso 1 1 calc R . . H34B H -0.4211 0.2384 0.5104 0.061 Uiso 1 1 calc R . . C35 C -0.3094(4) 0.3042(3) 0.5620(2) 0.0493(14) Uani 1 1 d . . . H35A H -0.3519 0.2917 0.5997 0.059 Uiso 1 1 calc R . . H35B H -0.2892 0.3567 0.5633 0.059 Uiso 1 1 calc R . . C36 C -0.1909(4) 0.2591(3) 0.5578(2) 0.0384(12) Uani 1 1 d . . . H36A H -0.1358 0.2730 0.5910 0.046 Uiso 1 1 calc R . . H36B H -0.2099 0.2067 0.5619 0.046 Uiso 1 1 calc R . . O37 O 0.0561(3) 0.29904(19) 0.21963(14) 0.0432(8) Uani 1 1 d . . . C37 C 0.0239(4) 0.3213(2) 0.2699(2) 0.0331(11) Uani 1 1 d . . . C38 C 0.1094(4) 0.3329(2) 0.3195(2) 0.0289(10) Uani 1 1 d . . . H38A H 0.1899 0.3159 0.3140 0.035 Uiso 1 1 calc R . . C39 C 0.0824(4) 0.3674(2) 0.3751(2) 0.0304(10) Uani 1 1 d . . . H39A H 0.0033 0.3627 0.3912 0.037 Uiso 1 1 calc R . . C40 C 0.1733(4) 0.4099(2) 0.4083(2) 0.0339(11) Uani 1 1 d . . . C41 C 0.1344(4) 0.4674(3) 0.4453(2) 0.0374(11) Uani 1 1 d . . . H41A H 0.0504 0.4779 0.4479 0.045 Uiso 1 1 calc R . . C42 C 0.2146(4) 0.5087(3) 0.4778(2) 0.0477(13) Uani 1 1 d . . . H42A H 0.1860 0.5463 0.5035 0.057 Uiso 1 1 calc R . . C43 C 0.3382(5) 0.4954(3) 0.4727(3) 0.0543(15) Uani 1 1 d . . . H43A H 0.3945 0.5249 0.4941 0.065 Uiso 1 1 calc R . . C44 C 0.3789(4) 0.4392(3) 0.4367(2) 0.0480(14) Uani 1 1 d . . . H44A H 0.4634 0.4300 0.4337 0.058 Uiso 1 1 calc R . . C45 C 0.2975(4) 0.3959(3) 0.4048(2) 0.0372(11) Uani 1 1 d . . . H45A H 0.3263 0.3568 0.3807 0.045 Uiso 1 1 calc R . . C46 C -0.1053(4) 0.3425(2) 0.2797(2) 0.0354(11) Uani 1 1 d . . . H46A H -0.1308 0.3544 0.3193 0.042 Uiso 1 1 calc R . . C47 C -0.1860(4) 0.3453(2) 0.2351(2) 0.0368(11) Uani 1 1 d . . . H47A H -0.1601 0.3285 0.1968 0.044 Uiso 1 1 calc R . . C48 C -0.3112(4) 0.3718(3) 0.2395(2) 0.0354(11) Uani 1 1 d . . . C49 C -0.3987(4) 0.3515(3) 0.1976(2) 0.0447(13) Uani 1 1 d . . . H49A H -0.3772 0.3199 0.1656 0.054 Uiso 1 1 calc R . . C50 C -0.5166(4) 0.3767(3) 0.2018(3) 0.0542(15) Uani 1 1 d . . . H50A H -0.5755 0.3617 0.1732 0.065 Uiso 1 1 calc R . . C51 C -0.5480(4) 0.4229(3) 0.2469(3) 0.0568(15) Uani 1 1 d . . . H51A H -0.6291 0.4398 0.2497 0.068 Uiso 1 1 calc R . . C52 C -0.4639(4) 0.4452(3) 0.2881(3) 0.0559(15) Uani 1 1 d . . . H52A H -0.4865 0.4786 0.3188 0.067 Uiso 1 1 calc R . . C53 C -0.3452(4) 0.4195(3) 0.2857(2) 0.0483(13) Uani 1 1 d . . . H53A H -0.2877 0.4342 0.3151 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02533(18) 0.0213(2) 0.02153(19) 0.00240(15) -0.00198(12) -0.00040(13) P1 0.0277(6) 0.0234(7) 0.0256(6) 0.0022(5) -0.0048(4) -0.0004(4) C1 0.033(2) 0.023(3) 0.029(3) 0.000(2) -0.0074(18) -0.0060(18) C2 0.030(2) 0.020(3) 0.036(3) 0.006(2) -0.0042(18) -0.0044(17) C3 0.047(3) 0.027(3) 0.033(3) -0.002(2) -0.004(2) -0.005(2) C4 0.038(3) 0.024(3) 0.057(4) 0.008(2) -0.001(2) 0.0047(19) C5 0.032(2) 0.030(3) 0.050(3) 0.016(2) -0.010(2) 0.0005(19) C6 0.029(2) 0.022(3) 0.046(3) 0.011(2) -0.008(2) -0.0036(18) C7 0.037(3) 0.039(3) 0.033(3) 0.016(2) -0.014(2) -0.005(2) C8 0.043(3) 0.038(3) 0.029(3) 0.008(2) -0.002(2) -0.006(2) C9 0.040(3) 0.028(3) 0.034(3) 0.012(2) 0.008(2) -0.0063(19) C10 0.027(2) 0.025(3) 0.038(3) 0.006(2) -0.0011(18) -0.0043(18) C11 0.029(2) 0.021(2) 0.031(3) 0.006(2) -0.0053(18) -0.0078(17) C12 0.030(2) 0.028(3) 0.039(3) 0.006(2) -0.0017(19) 0.0015(18) P2 0.0261(6) 0.0282(7) 0.0230(6) 0.0029(5) -0.0010(4) -0.0002(4) C13 0.034(2) 0.022(3) 0.031(3) 0.001(2) -0.0064(18) 0.0018(18) C14 0.031(2) 0.029(3) 0.035(3) 0.004(2) -0.0073(19) 0.0001(18) C15 0.039(3) 0.035(3) 0.048(3) -0.001(2) -0.014(2) 0.001(2) C16 0.028(2) 0.050(3) 0.042(3) -0.001(3) -0.004(2) -0.002(2) C17 0.030(2) 0.046(3) 0.042(3) 0.000(2) 0.002(2) 0.000(2) C18 0.033(2) 0.031(3) 0.030(3) -0.004(2) 0.0020(18) -0.0015(19) C19 0.027(2) 0.026(3) 0.028(3) 0.001(2) -0.0026(17) 0.0000(17) C20 0.044(3) 0.027(3) 0.034(3) -0.006(2) -0.006(2) 0.004(2) C21 0.045(3) 0.036(3) 0.030(3) -0.005(2) -0.005(2) -0.003(2) C22 0.044(3) 0.050(3) 0.028(3) -0.004(2) -0.008(2) -0.013(2) C23 0.031(3) 0.070(4) 0.039(3) -0.013(3) -0.012(2) 0.006(2) C24 0.032(2) 0.042(3) 0.031(3) -0.007(2) 0.0001(19) -0.001(2) C25 0.029(2) 0.037(3) 0.019(2) 0.001(2) -0.0034(16) -0.0027(18) C26 0.047(3) 0.040(3) 0.025(3) -0.005(2) -0.008(2) 0.000(2) C27 0.054(3) 0.044(3) 0.034(3) -0.004(2) -0.007(2) -0.003(2) C28 0.046(3) 0.058(4) 0.031(3) -0.005(3) -0.009(2) -0.010(2) C29 0.032(2) 0.057(4) 0.030(3) 0.007(2) -0.0047(19) -0.008(2) C30 0.032(2) 0.040(3) 0.027(3) 0.006(2) -0.0055(18) -0.0056(19) C31 0.029(2) 0.028(3) 0.030(3) 0.002(2) -0.0034(18) 0.0024(18) C32 0.030(2) 0.027(3) 0.040(3) 0.000(2) -0.0004(18) -0.0024(18) C33 0.033(2) 0.033(3) 0.056(3) -0.007(2) -0.005(2) 0.008(2) C34 0.029(3) 0.049(4) 0.074(4) 0.009(3) 0.004(2) 0.009(2) C35 0.054(3) 0.047(4) 0.047(3) 0.013(3) 0.024(2) 0.015(2) C36 0.037(2) 0.045(3) 0.033(3) 0.008(2) 0.0118(19) 0.007(2) O37 0.0498(19) 0.054(2) 0.026(2) 0.0052(17) -0.0005(14) 0.0021(16) C37 0.042(3) 0.029(3) 0.028(3) 0.005(2) 0.001(2) 0.003(2) C38 0.034(2) 0.021(3) 0.032(3) 0.012(2) -0.0003(18) 0.0021(18) C39 0.034(2) 0.026(3) 0.031(3) 0.008(2) -0.0081(19) -0.0014(18) C40 0.045(3) 0.025(3) 0.031(3) 0.005(2) -0.003(2) 0.001(2) C41 0.048(3) 0.032(3) 0.032(3) -0.003(2) -0.003(2) -0.002(2) C42 0.060(3) 0.033(3) 0.050(4) -0.006(3) -0.010(3) 0.003(2) C43 0.056(3) 0.039(4) 0.068(4) -0.010(3) -0.016(3) -0.002(3) C44 0.041(3) 0.043(3) 0.060(4) -0.004(3) -0.016(2) -0.002(2) C45 0.040(3) 0.032(3) 0.039(3) 0.001(2) -0.006(2) 0.001(2) C46 0.036(3) 0.035(3) 0.036(3) 0.008(2) 0.001(2) -0.004(2) C47 0.039(3) 0.033(3) 0.038(3) 0.004(2) -0.002(2) 0.002(2) C48 0.033(2) 0.039(3) 0.034(3) 0.011(2) 0.002(2) 0.001(2) C49 0.045(3) 0.037(3) 0.052(3) 0.000(3) -0.013(2) 0.002(2) C50 0.040(3) 0.051(4) 0.072(4) -0.003(3) -0.017(3) 0.003(2) C51 0.035(3) 0.062(4) 0.074(4) 0.005(3) -0.003(3) 0.007(3) C52 0.050(3) 0.061(4) 0.056(4) -0.006(3) 0.000(3) 0.014(3) C53 0.045(3) 0.052(4) 0.048(3) -0.003(3) -0.004(2) 0.005(2) _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 C39 2.134(4) . ? Pd1 C38 2.149(4) . ? Pd1 P2 2.3127(12) . ? Pd1 P1 2.3194(12) . ? P1 C19 1.853(4) . ? P1 C13 1.861(4) . ? P1 C1 1.864(4) . ? C1 C2 1.520(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.398(6) . ? C2 C11 1.439(6) . ? C3 C4 1.403(6) . ? C3 H3A 0.9500 . ? C4 C5 1.348(7) . ? C4 H4A 0.9500 . ? C5 C6 1.412(6) . ? C5 H5A 0.9500 . ? C6 C7 1.419(6) . ? C6 C11 1.457(5) . ? C7 C8 1.347(6) . ? C7 H7A 0.9500 . ? C8 C9 1.401(6) . ? C8 H8A 0.9500 . ? C9 C10 1.366(6) . ? C9 H9A 0.9500 . ? C10 C11 1.443(6) . ? C10 C12 1.521(5) . ? C12 P2 1.872(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? P2 C25 1.854(4) . ? P2 C31 1.856(4) . ? C13 C18 1.532(6) . ? C13 C14 1.540(6) . ? C13 H13A 1.0000 . ? C14 C15 1.536(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.526(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.529(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.529(5) . ? C19 C20 1.545(6) . ? C19 H19A 1.0000 . ? C20 C21 1.524(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.505(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.520(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.531(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.539(6) . ? C25 C30 1.542(6) . ? C25 H25A 1.0000 . ? C26 C27 1.540(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.534(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.521(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.529(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.527(6) . ? C31 C32 1.543(6) . ? C31 H31A 1.0000 . ? C32 C33 1.537(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.521(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.551(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O37 C37 1.242(5) . ? C37 C38 1.465(6) . ? C37 C46 1.496(6) . ? C38 C39 1.421(6) . ? C38 H38A 0.9500 . ? C39 C40 1.469(6) . ? C39 H39A 0.9500 . ? C40 C45 1.398(6) . ? C40 C41 1.407(6) . ? C41 C42 1.368(6) . ? C41 H41A 0.9500 . ? C42 C43 1.391(7) . ? C42 H42A 0.9500 . ? C43 C44 1.382(7) . ? C43 H43A 0.9500 . ? C44 C45 1.393(6) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.333(6) . ? C46 H46A 0.9500 . ? C47 C48 1.469(6) . ? C47 H47A 0.9500 . ? C48 C49 1.390(6) . ? C48 C53 1.401(7) . ? C49 C50 1.385(6) . ? C49 H49A 0.9500 . ? C50 C51 1.358(7) . ? C50 H50A 0.9500 . ? C51 C52 1.367(7) . ? C51 H51A 0.9500 . ? C52 C53 1.395(6) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C39 Pd1 C38 38.74(16) . . ? C39 Pd1 P2 108.39(13) . . ? C38 Pd1 P2 146.74(12) . . ? C39 Pd1 P1 147.68(13) . . ? C38 Pd1 P1 108.99(13) . . ? P2 Pd1 P1 103.90(4) . . ? C19 P1 C13 107.45(18) . . ? C19 P1 C1 99.87(19) . . ? C13 P1 C1 103.95(19) . . ? C19 P1 Pd1 111.07(14) . . ? C13 P1 Pd1 110.02(14) . . ? C1 P1 Pd1 123.19(15) . . ? C2 C1 P1 119.6(3) . . ? C2 C1 H1A 107.4 . . ? P1 C1 H1A 107.4 . . ? C2 C1 H1B 107.4 . . ? P1 C1 H1B 107.4 . . ? H1A C1 H1B 107.0 . . ? C3 C2 C11 119.3(4) . . ? C3 C2 C1 113.5(4) . . ? C11 C2 C1 127.1(4) . . ? C2 C3 C4 122.8(5) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C7 118.9(4) . . ? C5 C6 C11 121.2(4) . . ? C7 C6 C11 119.9(4) . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C10 C9 C8 123.6(4) . . ? C10 C9 H9A 118.2 . . ? C8 C9 H9A 118.2 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 C12 113.5(4) . . ? C11 C10 C12 127.0(4) . . ? C2 C11 C10 127.5(4) . . ? C2 C11 C6 116.1(4) . . ? C10 C11 C6 116.4(4) . . ? C10 C12 P2 115.8(3) . . ? C10 C12 H12A 108.3 . . ? P2 C12 H12A 108.3 . . ? C10 C12 H12B 108.3 . . ? P2 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C25 P2 C31 105.09(19) . . ? C25 P2 C12 104.42(19) . . ? C31 P2 C12 100.45(19) . . ? C25 P2 Pd1 118.79(14) . . ? C31 P2 Pd1 109.07(14) . . ? C12 P2 Pd1 116.93(15) . . ? C18 C13 C14 110.3(3) . . ? C18 C13 P1 111.7(3) . . ? C14 C13 P1 108.1(3) . . ? C18 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? P1 C13 H13A 108.9 . . ? C15 C14 C13 111.8(4) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 110.4(4) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C17 109.5(4) . . ? C15 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? C15 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? C16 C17 C18 111.3(4) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C13 112.9(4) . . ? C17 C18 H18A 109.0 . . ? C13 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C13 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C24 C19 C20 110.2(3) . . ? C24 C19 P1 109.8(3) . . ? C20 C19 P1 117.4(3) . . ? C24 C19 H19A 106.3 . . ? C20 C19 H19A 106.3 . . ? P1 C19 H19A 106.3 . . ? C21 C20 C19 111.7(4) . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 111.4(4) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 110.7(4) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 111.5(4) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C19 C24 C23 112.0(4) . . ? C19 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C19 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C30 109.4(3) . . ? C26 C25 P2 110.6(3) . . ? C30 C25 P2 110.4(3) . . ? C26 C25 H25A 108.8 . . ? C30 C25 H25A 108.8 . . ? P2 C25 H25A 108.8 . . ? C25 C26 C27 111.4(4) . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.7(4) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 109.5(4) . . ? C29 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? C29 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 111.0(4) . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C25 110.4(4) . . ? C29 C30 H30A 109.6 . . ? C25 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C25 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C36 C31 C32 110.7(3) . . ? C36 C31 P2 117.6(3) . . ? C32 C31 P2 110.3(3) . . ? C36 C31 H31A 105.8 . . ? C32 C31 H31A 105.8 . . ? P2 C31 H31A 105.8 . . ? C33 C32 C31 110.3(4) . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 110.3(4) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 111.8(4) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 111.5(4) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 110.7(4) . . ? C31 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? O37 C37 C38 122.7(4) . . ? O37 C37 C46 119.5(4) . . ? C38 C37 C46 117.7(4) . . ? C39 C38 C37 125.7(4) . . ? C39 C38 Pd1 70.0(2) . . ? C37 C38 Pd1 110.8(3) . . ? C39 C38 H38A 117.2 . . ? C37 C38 H38A 117.2 . . ? Pd1 C38 H38A 89.2 . . ? C38 C39 C40 122.0(4) . . ? C38 C39 Pd1 71.2(2) . . ? C40 C39 Pd1 116.6(3) . . ? C38 C39 H39A 119.0 . . ? C40 C39 H39A 119.0 . . ? Pd1 C39 H39A 82.5 . . ? C45 C40 C41 118.2(4) . . ? C45 C40 C39 122.8(4) . . ? C41 C40 C39 119.0(4) . . ? C42 C41 C40 121.8(4) . . ? C42 C41 H41A 119.1 . . ? C40 C41 H41A 119.1 . . ? C41 C42 C43 119.6(5) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 120.7(5) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C44 C45 C40 119.8(5) . . ? C44 C45 H45A 120.1 . . ? C40 C45 H45A 120.1 . . ? C47 C46 C37 122.5(4) . . ? C47 C46 H46A 118.8 . . ? C37 C46 H46A 118.8 . . ? C46 C47 C48 126.2(5) . . ? C46 C47 H47A 116.9 . . ? C48 C47 H47A 116.9 . . ? C49 C48 C53 118.1(4) . . ? C49 C48 C47 121.2(5) . . ? C53 C48 C47 120.6(4) . . ? C50 C49 C48 121.1(5) . . ? C50 C49 H49A 119.5 . . ? C48 C49 H49A 119.5 . . ? C51 C50 C49 120.1(5) . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C50 C51 C52 120.5(5) . . ? C50 C51 H51A 119.7 . . ? C52 C51 H51A 119.7 . . ? C51 C52 C53 120.6(5) . . ? C51 C52 H52A 119.7 . . ? C53 C52 H52A 119.7 . . ? C52 C53 C48 119.6(5) . . ? C52 C53 H53A 120.2 . . ? C48 C53 H53A 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C39 Pd1 P1 C19 -55.3(2) . . . . ? C38 Pd1 P1 C19 -52.54(18) . . . . ? P2 Pd1 P1 C19 122.44(14) . . . . ? C39 Pd1 P1 C13 63.5(3) . . . . ? C38 Pd1 P1 C13 66.30(18) . . . . ? P2 Pd1 P1 C13 -118.72(15) . . . . ? C39 Pd1 P1 C1 -173.5(2) . . . . ? C38 Pd1 P1 C1 -170.67(18) . . . . ? P2 Pd1 P1 C1 4.31(15) . . . . ? C19 P1 C1 C2 158.3(3) . . . . ? C13 P1 C1 C2 47.3(4) . . . . ? Pd1 P1 C1 C2 -78.4(4) . . . . ? P1 C1 C2 C3 -91.7(4) . . . . ? P1 C1 C2 C11 89.4(5) . . . . ? C11 C2 C3 C4 -2.5(6) . . . . ? C1 C2 C3 C4 178.6(4) . . . . ? C2 C3 C4 C5 1.5(7) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C4 C5 C6 C7 177.9(4) . . . . ? C4 C5 C6 C11 -1.4(7) . . . . ? C5 C6 C7 C8 -176.9(4) . . . . ? C11 C6 C7 C8 2.5(6) . . . . ? C6 C7 C8 C9 -0.5(7) . . . . ? C7 C8 C9 C10 -3.3(7) . . . . ? C8 C9 C10 C11 4.9(6) . . . . ? C8 C9 C10 C12 -173.0(4) . . . . ? C3 C2 C11 C10 -176.4(4) . . . . ? C1 C2 C11 C10 2.4(7) . . . . ? C3 C2 C11 C6 1.4(6) . . . . ? C1 C2 C11 C6 -179.8(4) . . . . ? C9 C10 C11 C2 175.1(4) . . . . ? C12 C10 C11 C2 -7.3(7) . . . . ? C9 C10 C11 C6 -2.7(6) . . . . ? C12 C10 C11 C6 174.9(4) . . . . ? C5 C6 C11 C2 0.5(6) . . . . ? C7 C6 C11 C2 -178.9(4) . . . . ? C5 C6 C11 C10 178.5(4) . . . . ? C7 C6 C11 C10 -0.9(6) . . . . ? C9 C10 C12 P2 86.4(4) . . . . ? C11 C10 C12 P2 -91.3(5) . . . . ? C10 C12 P2 C25 -39.2(4) . . . . ? C10 C12 P2 C31 -147.9(3) . . . . ? C10 C12 P2 Pd1 94.3(3) . . . . ? C39 Pd1 P2 C25 -66.26(19) . . . . ? C38 Pd1 P2 C25 -73.7(3) . . . . ? P1 Pd1 P2 C25 114.99(16) . . . . ? C39 Pd1 P2 C31 54.02(19) . . . . ? C38 Pd1 P2 C31 46.6(3) . . . . ? P1 Pd1 P2 C31 -124.72(15) . . . . ? C39 Pd1 P2 C12 167.02(17) . . . . ? C38 Pd1 P2 C12 159.6(2) . . . . ? P1 Pd1 P2 C12 -11.72(14) . . . . ? C19 P1 C13 C18 47.9(3) . . . . ? C1 P1 C13 C18 153.1(3) . . . . ? Pd1 P1 C13 C18 -73.2(3) . . . . ? C19 P1 C13 C14 169.3(3) . . . . ? C1 P1 C13 C14 -85.4(3) . . . . ? Pd1 P1 C13 C14 48.3(3) . . . . ? C18 C13 C14 C15 -52.7(5) . . . . ? P1 C13 C14 C15 -175.1(3) . . . . ? C13 C14 C15 C16 58.3(5) . . . . ? C14 C15 C16 C17 -60.0(5) . . . . ? C15 C16 C17 C18 58.2(5) . . . . ? C16 C17 C18 C13 -54.5(5) . . . . ? C14 C13 C18 C17 51.0(5) . . . . ? P1 C13 C18 C17 171.2(3) . . . . ? C13 P1 C19 C24 -178.5(3) . . . . ? C1 P1 C19 C24 73.3(3) . . . . ? Pd1 P1 C19 C24 -58.1(3) . . . . ? C13 P1 C19 C20 54.6(4) . . . . ? C1 P1 C19 C20 -53.5(3) . . . . ? Pd1 P1 C19 C20 175.0(3) . . . . ? C24 C19 C20 C21 53.8(5) . . . . ? P1 C19 C20 C21 -179.6(3) . . . . ? C19 C20 C21 C22 -56.6(5) . . . . ? C20 C21 C22 C23 57.3(5) . . . . ? C21 C22 C23 C24 -56.3(5) . . . . ? C20 C19 C24 C23 -53.0(5) . . . . ? P1 C19 C24 C23 176.2(3) . . . . ? C22 C23 C24 C19 54.9(5) . . . . ? C31 P2 C25 C26 -49.7(3) . . . . ? C12 P2 C25 C26 -154.9(3) . . . . ? Pd1 P2 C25 C26 72.6(3) . . . . ? C31 P2 C25 C30 -170.9(3) . . . . ? C12 P2 C25 C30 83.9(3) . . . . ? Pd1 P2 C25 C30 -48.6(3) . . . . ? C30 C25 C26 C27 -55.3(5) . . . . ? P2 C25 C26 C27 -177.1(3) . . . . ? C25 C26 C27 C28 55.3(5) . . . . ? C26 C27 C28 C29 -55.8(5) . . . . ? C27 C28 C29 C30 58.4(5) . . . . ? C28 C29 C30 C25 -60.2(5) . . . . ? C26 C25 C30 C29 57.6(5) . . . . ? P2 C25 C30 C29 179.5(3) . . . . ? C25 P2 C31 C36 -55.5(4) . . . . ? C12 P2 C31 C36 52.7(4) . . . . ? Pd1 P2 C31 C36 176.1(3) . . . . ? C25 P2 C31 C32 176.3(3) . . . . ? C12 P2 C31 C32 -75.6(3) . . . . ? Pd1 P2 C31 C32 47.9(3) . . . . ? C36 C31 C32 C33 58.2(5) . . . . ? P2 C31 C32 C33 -169.9(3) . . . . ? C31 C32 C33 C34 -58.0(5) . . . . ? C32 C33 C34 C35 56.9(5) . . . . ? C33 C34 C35 C36 -55.0(6) . . . . ? C32 C31 C36 C35 -55.9(5) . . . . ? P2 C31 C36 C35 176.1(3) . . . . ? C34 C35 C36 C31 54.4(5) . . . . ? O37 C37 C38 C39 170.9(4) . . . . ? C46 C37 C38 C39 -4.7(6) . . . . ? O37 C37 C38 Pd1 -109.3(4) . . . . ? C46 C37 C38 Pd1 75.1(4) . . . . ? P2 Pd1 C38 C39 11.3(3) . . . . ? P1 Pd1 C38 C39 -177.6(2) . . . . ? C39 Pd1 C38 C37 -121.7(4) . . . . ? P2 Pd1 C38 C37 -110.4(3) . . . . ? P1 Pd1 C38 C37 60.6(3) . . . . ? C37 C38 C39 C40 -148.0(4) . . . . ? Pd1 C38 C39 C40 110.2(4) . . . . ? C37 C38 C39 Pd1 101.8(4) . . . . ? P2 Pd1 C39 C38 -173.5(2) . . . . ? P1 Pd1 C39 C38 4.2(3) . . . . ? C38 Pd1 C39 C40 -117.1(4) . . . . ? P2 Pd1 C39 C40 69.4(3) . . . . ? P1 Pd1 C39 C40 -112.8(3) . . . . ? C38 C39 C40 C45 -28.5(6) . . . . ? Pd1 C39 C40 C45 55.0(5) . . . . ? C38 C39 C40 C41 151.5(4) . . . . ? Pd1 C39 C40 C41 -124.9(4) . . . . ? C45 C40 C41 C42 -0.5(7) . . . . ? C39 C40 C41 C42 179.5(4) . . . . ? C40 C41 C42 C43 2.1(8) . . . . ? C41 C42 C43 C44 -2.1(8) . . . . ? C42 C43 C44 C45 0.5(8) . . . . ? C43 C44 C45 C40 1.1(8) . . . . ? C41 C40 C45 C44 -1.1(7) . . . . ? C39 C40 C45 C44 178.9(4) . . . . ? O37 C37 C46 C47 -6.7(7) . . . . ? C38 C37 C46 C47 169.0(4) . . . . ? C37 C46 C47 C48 -174.0(4) . . . . ? C46 C47 C48 C49 -158.9(5) . . . . ? C46 C47 C48 C53 22.3(7) . . . . ? C53 C48 C49 C50 -1.0(7) . . . . ? C47 C48 C49 C50 -179.9(5) . . . . ? C48 C49 C50 C51 1.0(8) . . . . ? C49 C50 C51 C52 0.4(9) . . . . ? C50 C51 C52 C53 -1.7(9) . . . . ? C51 C52 C53 C48 1.7(8) . . . . ? C49 C48 C53 C52 -0.3(7) . . . . ? C47 C48 C53 C52 178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.984 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.086 # Attachment '8_PhPnapth_dba.CIF' data_sasol48 _database_code_depnum_ccdc_archive 'CCDC 295575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H44 O1 P2 Pd.C4 H10 O1' _chemical_formula_sum 'C57 H54 O2 P2 Pd' _chemical_formula_weight 939.34 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 13.479(8) _cell_length_b 17.557(9) _cell_length_c 20.690(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.030(8) _cell_angle_gamma 90.00 _cell_volume 4629(4) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7533 _cell_measurement_theta_min 1.9752 _cell_measurement_theta_max 25.3491 _exptl_crystal_description needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8453 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31314 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8331 _reflns_number_gt 7178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+11.6717P] 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 idealised _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 8331 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.23848(2) 0.181739(16) 0.832875(14) 0.02014(11) Uani 1 1 d . . . P1 P 0.20470(8) 0.06046(5) 0.79022(5) 0.0221(2) Uani 1 1 d . . . C1 C 0.2918(3) -0.0174(2) 0.8369(2) 0.0250(8) Uani 1 1 d . . . H1A H 0.2870 -0.0217 0.8835 0.030 Uiso 1 1 calc R . . H1B H 0.2681 -0.0663 0.8129 0.030 Uiso 1 1 calc R . . C2 C 0.4041(3) -0.0032(2) 0.8417(2) 0.0244(8) Uani 1 1 d . . . C3 C 0.4340(3) -0.0381(2) 0.7912(2) 0.0324(10) Uani 1 1 d . . . H3A H 0.3865 -0.0728 0.7614 0.039 Uiso 1 1 calc R . . C4 C 0.5301(3) -0.0251(3) 0.7819(2) 0.0370(10) Uani 1 1 d . . . H4A H 0.5475 -0.0507 0.7466 0.044 Uiso 1 1 calc R . . C5 C 0.5987(3) 0.0244(3) 0.8235(2) 0.0343(10) Uani 1 1 d . . . H5A H 0.6624 0.0361 0.8153 0.041 Uiso 1 1 calc R . . C6 C 0.5763(3) 0.0586(2) 0.8787(2) 0.0261(9) Uani 1 1 d . . . C7 C 0.6561(3) 0.1041(2) 0.9237(2) 0.0318(9) Uani 1 1 d . . . H7A H 0.7184 0.1148 0.9134 0.038 Uiso 1 1 calc R . . C8 C 0.6431(3) 0.1326(2) 0.9816(2) 0.0335(10) Uani 1 1 d . . . H8A H 0.6974 0.1616 1.0128 0.040 Uiso 1 1 calc R . . C9 C 0.5499(3) 0.1189(2) 0.9952(2) 0.0271(9) Uani 1 1 d . . . H9A H 0.5427 0.1385 1.0362 0.032 Uiso 1 1 calc R . . C10 C 0.4680(3) 0.0783(2) 0.95179(19) 0.0241(8) Uani 1 1 d . . . C11 C 0.4787(3) 0.0456(2) 0.89043(19) 0.0228(8) Uani 1 1 d . . . C12 C 0.3742(3) 0.0714(2) 0.9757(2) 0.0253(8) Uani 1 1 d . . . H12A H 0.3983 0.0686 1.0262 0.030 Uiso 1 1 calc R . . H12B H 0.3362 0.0237 0.9575 0.030 Uiso 1 1 calc R . . P12 P 0.28398(8) 0.15341(6) 0.94712(5) 0.0216(2) Uani 1 1 d . . . C13 C 0.0763(3) 0.0316(2) 0.7929(2) 0.0269(9) Uani 1 1 d . . . C14 C 0.0481(4) -0.0447(3) 0.7953(2) 0.0357(10) Uani 1 1 d . . . H14A H 0.0988 -0.0837 0.8000 0.043 Uiso 1 1 calc R . . C15 C -0.0534(4) -0.0635(3) 0.7908(3) 0.0413(11) Uani 1 1 d . . . H15A H -0.0726 -0.1155 0.7916 0.050 Uiso 1 1 calc R . . C16 C -0.1273(4) -0.0069(3) 0.7850(3) 0.0414(11) Uani 1 1 d . . . H16A H -0.1973 -0.0200 0.7813 0.050 Uiso 1 1 calc R . . C17 C -0.0992(3) 0.0683(3) 0.7848(2) 0.0359(10) Uani 1 1 d . . . H17A H -0.1497 0.1071 0.7819 0.043 Uiso 1 1 calc R . . C18 C 0.0020(3) 0.0879(2) 0.7888(2) 0.0303(9) Uani 1 1 d . . . H18A H 0.0207 0.1401 0.7886 0.036 Uiso 1 1 calc R . . C19 C 0.1947(3) 0.0394(2) 0.7016(2) 0.0275(9) Uani 1 1 d . . . C20 C 0.2676(4) 0.0700(2) 0.6758(2) 0.0350(10) Uani 1 1 d . . . H20A H 0.3232 0.1000 0.7044 0.042 Uiso 1 1 calc R . . C21 C 0.2607(4) 0.0573(3) 0.6074(2) 0.0422(12) Uani 1 1 d . . . H21A H 0.3115 0.0785 0.5898 0.051 Uiso 1 1 calc R . . C22 C 0.1794(4) 0.0138(3) 0.5660(2) 0.0463(13) Uani 1 1 d . . . H22A H 0.1738 0.0050 0.5196 0.056 Uiso 1 1 calc R . . C23 C 0.1073(4) -0.0167(3) 0.5918(2) 0.0429(12) Uani 1 1 d . . . H23A H 0.0518 -0.0468 0.5632 0.052 Uiso 1 1 calc R . . C24 C 0.1135(4) -0.0045(2) 0.6584(2) 0.0346(10) Uani 1 1 d . . . H24A H 0.0622 -0.0260 0.6754 0.041 Uiso 1 1 calc R . . C25 C 0.3586(3) 0.2238(2) 1.0094(2) 0.0245(8) Uani 1 1 d . . . C26 C 0.3678(3) 0.2193(3) 1.0779(2) 0.0343(10) Uani 1 1 d . . . H26A H 0.3269 0.1833 1.0925 0.041 Uiso 1 1 calc R . . C27 C 0.4361(4) 0.2670(3) 1.1258(2) 0.0412(11) Uani 1 1 d . . . H27A H 0.4428 0.2632 1.1728 0.049 Uiso 1 1 calc R . . C28 C 0.4938(4) 0.3196(3) 1.1041(3) 0.0395(12) Uani 1 1 d . . . H28A H 0.5399 0.3529 1.1364 0.047 Uiso 1 1 calc R . . C29 C 0.4855(3) 0.3248(2) 1.0362(2) 0.0356(11) Uani 1 1 d . . . H29A H 0.5260 0.3613 1.0219 0.043 Uiso 1 1 calc R . . C30 C 0.4187(3) 0.2771(2) 0.9892(2) 0.0284(9) Uani 1 1 d . . . H30A H 0.4136 0.2807 0.9424 0.034 Uiso 1 1 calc R . . C31 C 0.1746(3) 0.1308(2) 0.9772(2) 0.0262(8) Uani 1 1 d . . . C32 C 0.1787(4) 0.0759(3) 1.0266(2) 0.0385(11) Uani 1 1 d . . . H32A H 0.2405 0.0462 1.0453 0.046 Uiso 1 1 calc R . . C33 C 0.0942(4) 0.0642(3) 1.0485(3) 0.0510(13) Uani 1 1 d . . . H33A H 0.0977 0.0262 1.0819 0.061 Uiso 1 1 calc R . . C34 C 0.0044(4) 0.1070(3) 1.0227(3) 0.0515(13) Uani 1 1 d . . . H34A H -0.0532 0.0994 1.0390 0.062 Uiso 1 1 calc R . . C35 C -0.0013(4) 0.1605(3) 0.9734(3) 0.0442(12) Uani 1 1 d . . . H35A H -0.0634 0.1899 0.9551 0.053 Uiso 1 1 calc R . . C36 C 0.0827(3) 0.1718(2) 0.9503(2) 0.0310(9) Uani 1 1 d . . . H36A H 0.0773 0.2083 0.9154 0.037 Uiso 1 1 calc R . . O37 O 0.0437(2) 0.30188(17) 0.80102(15) 0.0305(6) Uani 1 1 d . . . C37 C 0.1353(3) 0.3176(2) 0.8347(2) 0.0245(8) Uani 1 1 d . . . C38 C 0.2234(3) 0.3013(2) 0.8107(2) 0.0241(8) Uani 1 1 d . . . H38A H 0.2914 0.3177 0.8378 0.029 Uiso 1 1 calc R . . C39 C 0.2127(3) 0.2626(2) 0.7495(2) 0.0242(8) Uani 1 1 d . . . H39A H 0.1479 0.2380 0.7267 0.029 Uiso 1 1 calc R . . C40 C 0.2963(3) 0.2583(2) 0.7188(2) 0.0248(8) Uani 1 1 d . . . C41 C 0.4024(3) 0.2531(2) 0.7587(2) 0.0302(9) Uani 1 1 d . . . H41A H 0.4215 0.2552 0.8071 0.036 Uiso 1 1 calc R . . C42 C 0.4790(4) 0.2452(3) 0.7289(2) 0.0373(10) Uani 1 1 d . . . H42A H 0.5503 0.2411 0.7570 0.045 Uiso 1 1 calc R . . C43 C 0.4537(4) 0.2430(3) 0.6584(2) 0.0387(11) Uani 1 1 d . . . H43A H 0.5071 0.2370 0.6381 0.046 Uiso 1 1 calc R . . C44 C 0.3504(4) 0.2497(3) 0.6183(2) 0.0352(10) Uani 1 1 d . . . H44A H 0.3323 0.2493 0.5699 0.042 Uiso 1 1 calc R . . C45 C 0.2722(3) 0.2571(2) 0.6480(2) 0.0284(9) Uani 1 1 d . . . H45A H 0.2011 0.2614 0.6196 0.034 Uiso 1 1 calc R . . C46 C 0.1622(3) 0.3519(2) 0.9033(2) 0.0275(9) Uani 1 1 d . . . H46A H 0.2334 0.3643 0.9269 0.033 Uiso 1 1 calc R . . C47 C 0.0907(3) 0.3662(3) 0.9339(2) 0.0341(10) Uani 1 1 d . . . H47A H 0.0193 0.3577 0.9078 0.041 Uiso 1 1 calc R . . C48 C 0.1125(4) 0.3936(3) 1.0038(2) 0.0359(10) Uani 1 1 d . . . C49 C 0.0308(4) 0.4122(4) 1.0283(3) 0.0593(16) Uani 1 1 d . . . H49A H -0.0395 0.4075 0.9986 0.071 Uiso 1 1 calc R . . C50 C 0.0494(5) 0.4372(4) 1.0945(3) 0.070(2) Uani 1 1 d . . . H50A H -0.0078 0.4484 1.1103 0.085 Uiso 1 1 calc R . . C51 C 0.1499(4) 0.4457(3) 1.1371(3) 0.0492(13) Uani 1 1 d . . . H51A H 0.1630 0.4636 1.1824 0.059 Uiso 1 1 calc R . . C52 C 0.2326(4) 0.4282(3) 1.1143(2) 0.0465(12) Uani 1 1 d . . . H52A H 0.3025 0.4348 1.1441 0.056 Uiso 1 1 calc R . . C53 C 0.2151(4) 0.4014(3) 1.0489(2) 0.0377(10) Uani 1 1 d . . . H53A H 0.2728 0.3881 1.0344 0.045 Uiso 1 1 calc R . . C54 C 0.6421(5) 0.3382(5) 0.9116(3) 0.074(2) Uani 1 1 d . . . H54A H 0.5918 0.3718 0.8792 0.111 Uiso 1 1 calc R . . H54B H 0.6572 0.3580 0.9581 0.111 Uiso 1 1 calc R . . H54C H 0.6121 0.2870 0.9088 0.111 Uiso 1 1 calc R . . C55 C 0.7407(4) 0.3348(4) 0.8944(3) 0.0538(14) Uani 1 1 d . . . H55A H 0.7725 0.3862 0.8988 0.065 Uiso 1 1 calc R . . H55B H 0.7912 0.3004 0.9267 0.065 Uiso 1 1 calc R . . O56 O 0.7197(3) 0.3080(2) 0.82698(19) 0.0531(10) Uani 1 1 d . . . C57 C 0.8053(5) 0.3039(5) 0.8056(4) 0.087(3) Uani 1 1 d . . . H57A H 0.8561 0.2667 0.8342 0.105 Uiso 1 1 calc R . . H57B H 0.8402 0.3543 0.8111 0.105 Uiso 1 1 calc R . . C58 C 0.7741(6) 0.2805(6) 0.7333(4) 0.112(4) Uani 1 1 d . . . H58A H 0.7371 0.2316 0.7275 0.167 Uiso 1 1 calc R . . H58B H 0.8368 0.2750 0.7196 0.167 Uiso 1 1 calc R . . H58C H 0.7277 0.3191 0.7047 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02557(18) 0.01520(17) 0.01695(18) 0.00056(10) 0.00321(12) 0.00045(11) P1 0.0251(5) 0.0168(5) 0.0216(5) -0.0008(4) 0.0036(4) 0.0004(4) C1 0.025(2) 0.0195(19) 0.026(2) -0.0003(16) 0.0033(16) -0.0024(15) C2 0.026(2) 0.0191(19) 0.025(2) 0.0042(15) 0.0034(16) 0.0034(15) C3 0.033(2) 0.027(2) 0.031(2) -0.0078(18) 0.0028(18) 0.0017(18) C4 0.032(2) 0.045(3) 0.033(2) -0.009(2) 0.0095(19) 0.008(2) C5 0.029(2) 0.040(3) 0.034(2) 0.001(2) 0.0111(19) 0.0045(19) C6 0.026(2) 0.0209(19) 0.028(2) 0.0051(16) 0.0042(16) 0.0021(16) C7 0.027(2) 0.029(2) 0.038(2) 0.0001(18) 0.0086(18) -0.0028(17) C8 0.031(2) 0.029(2) 0.032(2) -0.0064(18) -0.0008(18) -0.0029(18) C9 0.034(2) 0.0206(19) 0.022(2) 0.0004(16) 0.0034(17) 0.0075(16) C10 0.029(2) 0.0152(18) 0.0219(19) 0.0038(15) -0.0003(16) 0.0042(15) C11 0.027(2) 0.0159(18) 0.0219(19) 0.0022(15) 0.0039(16) 0.0037(15) C12 0.035(2) 0.0169(18) 0.023(2) 0.0033(15) 0.0071(16) 0.0035(16) P12 0.0263(5) 0.0179(5) 0.0184(5) 0.0012(4) 0.0045(4) 0.0013(4) C13 0.027(2) 0.026(2) 0.025(2) -0.0007(16) 0.0050(16) -0.0004(16) C14 0.031(2) 0.028(2) 0.048(3) 0.002(2) 0.013(2) -0.0014(18) C15 0.031(2) 0.032(2) 0.062(3) 0.004(2) 0.016(2) -0.0060(19) C16 0.027(2) 0.049(3) 0.050(3) 0.005(2) 0.015(2) -0.003(2) C17 0.029(2) 0.043(3) 0.033(2) -0.001(2) 0.0055(18) 0.0083(19) C18 0.032(2) 0.026(2) 0.029(2) -0.0033(17) 0.0050(17) 0.0010(17) C19 0.035(2) 0.0196(19) 0.023(2) 0.0016(16) 0.0035(17) 0.0072(16) C20 0.046(3) 0.019(2) 0.043(3) 0.0026(18) 0.019(2) 0.0051(18) C21 0.055(3) 0.041(3) 0.036(3) 0.007(2) 0.021(2) 0.016(2) C22 0.062(3) 0.040(3) 0.029(2) -0.003(2) 0.005(2) 0.013(2) C23 0.058(3) 0.035(3) 0.028(2) -0.007(2) 0.003(2) 0.004(2) C24 0.039(2) 0.027(2) 0.031(2) -0.0054(18) 0.0011(19) 0.0008(18) C25 0.0234(19) 0.023(2) 0.024(2) 0.0017(16) 0.0027(16) 0.0029(15) C26 0.030(2) 0.042(3) 0.028(2) -0.0034(19) 0.0058(18) -0.0042(19) C27 0.040(3) 0.054(3) 0.026(2) -0.011(2) 0.0055(19) -0.003(2) C28 0.035(2) 0.032(2) 0.037(3) -0.0073(19) -0.009(2) 0.0008(19) C29 0.030(2) 0.026(2) 0.039(3) 0.0045(18) -0.0036(19) -0.0041(17) C30 0.030(2) 0.023(2) 0.027(2) 0.0065(16) 0.0026(17) 0.0007(16) C31 0.029(2) 0.027(2) 0.021(2) -0.0005(16) 0.0071(16) 0.0002(17) C32 0.040(3) 0.041(3) 0.038(3) 0.009(2) 0.016(2) 0.005(2) C33 0.054(3) 0.058(3) 0.048(3) 0.017(3) 0.026(3) 0.002(3) C34 0.046(3) 0.057(3) 0.062(4) 0.008(3) 0.031(3) -0.003(3) C35 0.037(3) 0.040(3) 0.059(3) 0.004(2) 0.021(2) 0.004(2) C36 0.030(2) 0.028(2) 0.035(2) -0.0006(18) 0.0105(19) 0.0002(17) O37 0.0276(15) 0.0339(16) 0.0269(15) 0.0012(12) 0.0048(12) 0.0023(12) C37 0.031(2) 0.0152(18) 0.023(2) 0.0063(14) 0.0026(17) 0.0001(15) C38 0.027(2) 0.0148(18) 0.028(2) 0.0063(16) 0.0055(16) 0.0028(15) C39 0.029(2) 0.0151(18) 0.023(2) 0.0032(15) 0.0018(16) 0.0003(15) C40 0.035(2) 0.0115(17) 0.026(2) 0.0030(15) 0.0076(17) -0.0005(15) C41 0.030(2) 0.030(2) 0.027(2) -0.0004(17) 0.0045(17) -0.0059(17) C42 0.031(2) 0.040(3) 0.040(3) 0.003(2) 0.0106(19) -0.0007(19) C43 0.038(3) 0.041(3) 0.042(3) 0.005(2) 0.019(2) 0.002(2) C44 0.045(3) 0.034(2) 0.030(2) 0.0020(19) 0.016(2) -0.003(2) C45 0.032(2) 0.026(2) 0.026(2) 0.0100(17) 0.0064(17) 0.0015(17) C46 0.033(2) 0.0164(19) 0.031(2) 0.0012(16) 0.0075(18) 0.0007(16) C47 0.029(2) 0.032(2) 0.040(3) -0.0032(19) 0.0087(19) -0.0007(18) C48 0.038(2) 0.032(2) 0.037(3) -0.0056(19) 0.012(2) -0.0018(19) C49 0.032(3) 0.089(5) 0.059(4) -0.030(3) 0.018(2) -0.012(3) C50 0.057(4) 0.107(5) 0.058(4) -0.037(4) 0.033(3) -0.012(4) C51 0.055(3) 0.061(3) 0.035(3) -0.012(2) 0.017(2) -0.002(3) C52 0.051(3) 0.054(3) 0.031(3) -0.004(2) 0.008(2) 0.005(2) C53 0.038(3) 0.046(3) 0.031(2) 0.000(2) 0.014(2) 0.005(2) C54 0.075(5) 0.099(5) 0.048(4) -0.014(3) 0.021(3) 0.023(4) C55 0.048(3) 0.060(3) 0.045(3) -0.005(3) 0.003(2) -0.006(3) O56 0.042(2) 0.065(3) 0.052(2) -0.0039(18) 0.0147(17) 0.0059(17) C57 0.041(3) 0.146(7) 0.082(5) 0.046(5) 0.029(3) 0.025(4) C58 0.079(5) 0.193(10) 0.078(5) 0.041(6) 0.047(4) 0.087(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C38 2.145(4) . ? Pd1 C39 2.174(4) . ? Pd1 P1 2.2930(14) . ? Pd1 P12 2.2947(16) . ? P1 C13 1.821(4) . ? P1 C19 1.831(4) . ? P1 C1 1.855(4) . ? C1 C2 1.504(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.380(6) . ? C2 C11 1.449(5) . ? C3 C4 1.390(6) . ? C3 H3A 0.9500 . ? C4 C5 1.354(6) . ? C4 H4A 0.9500 . ? C5 C6 1.407(6) . ? C5 H5A 0.9500 . ? C6 C7 1.417(6) . ? C6 C11 1.432(6) . ? C7 C8 1.362(6) . ? C7 H7A 0.9500 . ? C8 C9 1.393(6) . ? C8 H8A 0.9500 . ? C9 C10 1.373(6) . ? C9 H9A 0.9500 . ? C10 C11 1.443(6) . ? C10 C12 1.505(6) . ? C12 P12 1.853(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? P12 C31 1.821(4) . ? P12 C25 1.831(4) . ? C13 C18 1.390(6) . ? C13 C14 1.399(6) . ? C14 C15 1.380(6) . ? C14 H14A 0.9500 . ? C15 C16 1.384(7) . ? C15 H15A 0.9500 . ? C16 C17 1.373(7) . ? C16 H16A 0.9500 . ? C17 C18 1.384(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.372(6) . ? C19 C24 1.397(6) . ? C20 C21 1.406(6) . ? C20 H20A 0.9500 . ? C21 C22 1.381(7) . ? C21 H21A 0.9500 . ? C22 C23 1.361(8) . ? C22 H22A 0.9500 . ? C23 C24 1.371(7) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.385(6) . ? C25 C30 1.390(6) . ? C26 C27 1.390(6) . ? C26 H26A 0.9500 . ? C27 C28 1.374(7) . ? C27 H27A 0.9500 . ? C28 C29 1.375(7) . ? C28 H28A 0.9500 . ? C29 C30 1.374(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.384(6) . ? C31 C32 1.393(6) . ? C32 C33 1.372(7) . ? C32 H32A 0.9500 . ? C33 C34 1.375(8) . ? C33 H33A 0.9500 . ? C34 C35 1.371(7) . ? C34 H34A 0.9500 . ? C35 C36 1.380(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O37 C37 1.235(5) . ? C37 C38 1.457(6) . ? C37 C46 1.474(6) . ? C38 C39 1.402(6) . ? C38 H38A 0.9500 . ? C39 C40 1.465(6) . ? C39 H39A 0.9500 . ? C40 C45 1.393(6) . ? C40 C41 1.402(6) . ? C41 C42 1.371(6) . ? C41 H41A 0.9500 . ? C42 C43 1.387(7) . ? C42 H42A 0.9500 . ? C43 C44 1.374(7) . ? C43 H43A 0.9500 . ? C44 C45 1.389(6) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.337(6) . ? C46 H46A 0.9500 . ? C47 C48 1.460(6) . ? C47 H47A 0.9500 . ? C48 C49 1.392(7) . ? C48 C53 1.400(6) . ? C49 C50 1.382(8) . ? C49 H49A 0.9500 . ? C50 C51 1.363(8) . ? C50 H50A 0.9500 . ? C51 C52 1.378(7) . ? C51 H51A 0.9500 . ? C52 C53 1.379(7) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? C54 C55 1.485(9) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O56 1.410(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? O56 C57 1.366(7) . ? C57 C58 1.475(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 Pd1 C39 37.88(15) . . ? C38 Pd1 P1 146.46(12) . . ? C39 Pd1 P1 109.94(11) . . ? C38 Pd1 P12 114.07(11) . . ? C39 Pd1 P12 151.55(11) . . ? P1 Pd1 P12 98.51(4) . . ? C13 P1 C19 102.34(19) . . ? C13 P1 C1 103.05(19) . . ? C19 P1 C1 101.48(18) . . ? C13 P1 Pd1 108.53(14) . . ? C19 P1 Pd1 120.90(13) . . ? C1 P1 Pd1 118.16(13) . . ? C2 C1 P1 111.4(3) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C11 118.8(4) . . ? C3 C2 C1 114.3(4) . . ? C11 C2 C1 126.8(4) . . ? C2 C3 C4 123.2(4) . . ? C2 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C7 117.2(4) . . ? C5 C6 C11 121.5(4) . . ? C7 C6 C11 121.3(4) . . ? C8 C7 C6 119.9(4) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C10 C9 C8 122.9(4) . . ? C10 C9 H9A 118.5 . . ? C8 C9 H9A 118.5 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 C12 114.2(4) . . ? C11 C10 C12 126.3(3) . . ? C6 C11 C10 116.5(3) . . ? C6 C11 C2 116.3(4) . . ? C10 C11 C2 127.0(4) . . ? C10 C12 P12 111.5(3) . . ? C10 C12 H12A 109.3 . . ? P12 C12 H12A 109.3 . . ? C10 C12 H12B 109.3 . . ? P12 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C31 P12 C25 103.10(19) . . ? C31 P12 C12 104.01(19) . . ? C25 P12 C12 98.42(18) . . ? C31 P12 Pd1 115.17(13) . . ? C25 P12 Pd1 118.67(14) . . ? C12 P12 Pd1 115.10(13) . . ? C18 C13 C14 119.0(4) . . ? C18 C13 P1 118.3(3) . . ? C14 C13 P1 122.7(3) . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C13 120.2(4) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C20 C19 C24 118.5(4) . . ? C20 C19 P1 118.9(3) . . ? C24 C19 P1 122.6(4) . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C22 C21 C20 119.3(5) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 121.0(5) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C19 120.5(5) . . ? C23 C24 H24A 119.7 . . ? C19 C24 H24A 119.7 . . ? C26 C25 C30 118.7(4) . . ? C26 C25 P12 121.9(3) . . ? C30 C25 P12 118.9(3) . . ? C25 C26 C27 120.8(4) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 119.1(4) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 120.8(4) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 119.9(4) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 120.6(4) . . ? C29 C30 H30A 119.7 . . ? C25 C30 H30A 119.7 . . ? C36 C31 C32 118.2(4) . . ? C36 C31 P12 117.8(3) . . ? C32 C31 P12 124.0(3) . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 120.8(5) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 120.9(4) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? O37 C37 C38 122.6(4) . . ? O37 C37 C46 121.4(4) . . ? C38 C37 C46 115.9(4) . . ? C39 C38 C37 123.2(4) . . ? C39 C38 Pd1 72.2(2) . . ? C37 C38 Pd1 98.6(2) . . ? C39 C38 H38A 118.4 . . ? C37 C38 H38A 118.4 . . ? Pd1 C38 H38A 99.5 . . ? C38 C39 C40 123.3(4) . . ? C38 C39 Pd1 69.9(2) . . ? C40 C39 Pd1 111.3(2) . . ? C38 C39 H39A 118.3 . . ? C40 C39 H39A 118.3 . . ? Pd1 C39 H39A 88.8 . . ? C45 C40 C41 117.6(4) . . ? C45 C40 C39 120.5(4) . . ? C41 C40 C39 121.9(4) . . ? C42 C41 C40 120.9(4) . . ? C42 C41 H41A 119.5 . . ? C40 C41 H41A 119.5 . . ? C41 C42 C43 120.9(4) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C42 119.1(4) . . ? C44 C43 H43A 120.5 . . ? C42 C43 H43A 120.5 . . ? C43 C44 C45 120.4(4) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C44 C45 C40 121.1(4) . . ? C44 C45 H45A 119.5 . . ? C40 C45 H45A 119.5 . . ? C47 C46 C37 122.9(4) . . ? C47 C46 H46A 118.5 . . ? C37 C46 H46A 118.5 . . ? C46 C47 C48 126.0(4) . . ? C46 C47 H47A 117.0 . . ? C48 C47 H47A 117.0 . . ? C49 C48 C53 117.5(4) . . ? C49 C48 C47 120.6(4) . . ? C53 C48 C47 121.9(4) . . ? C50 C49 C48 121.7(5) . . ? C50 C49 H49A 119.1 . . ? C48 C49 H49A 119.1 . . ? C51 C50 C49 119.8(5) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C50 C51 C52 120.0(5) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C51 C52 C53 120.8(5) . . ? C51 C52 H52A 119.6 . . ? C53 C52 H52A 119.6 . . ? C52 C53 C48 120.3(5) . . ? C52 C53 H53A 119.9 . . ? C48 C53 H53A 119.9 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O56 C55 C54 110.1(5) . . ? O56 C55 H55A 109.6 . . ? C54 C55 H55A 109.6 . . ? O56 C55 H55B 109.6 . . ? C54 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? C57 O56 C55 114.8(5) . . ? O56 C57 C58 110.6(6) . . ? O56 C57 H57A 109.5 . . ? C58 C57 H57A 109.5 . . ? O56 C57 H57B 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C38 Pd1 P1 C13 -88.8(2) . . . . ? C39 Pd1 P1 C13 -102.29(18) . . . . ? P12 Pd1 P1 C13 77.61(14) . . . . ? C38 Pd1 P1 C19 28.8(3) . . . . ? C39 Pd1 P1 C19 15.3(2) . . . . ? P12 Pd1 P1 C19 -164.79(16) . . . . ? C38 Pd1 P1 C1 154.5(2) . . . . ? C39 Pd1 P1 C1 141.00(19) . . . . ? P12 Pd1 P1 C1 -39.10(16) . . . . ? C13 P1 C1 C2 -178.7(3) . . . . ? C19 P1 C1 C2 75.5(3) . . . . ? Pd1 P1 C1 C2 -59.1(3) . . . . ? P1 C1 C2 C3 -95.1(4) . . . . ? P1 C1 C2 C11 81.1(4) . . . . ? C11 C2 C3 C4 -4.2(6) . . . . ? C1 C2 C3 C4 172.3(4) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? C3 C4 C5 C6 4.3(7) . . . . ? C4 C5 C6 C7 174.3(4) . . . . ? C4 C5 C6 C11 -3.5(6) . . . . ? C5 C6 C7 C8 -173.6(4) . . . . ? C11 C6 C7 C8 4.2(6) . . . . ? C6 C7 C8 C9 -2.2(6) . . . . ? C7 C8 C9 C10 -1.0(6) . . . . ? C8 C9 C10 C11 2.3(6) . . . . ? C8 C9 C10 C12 -179.1(4) . . . . ? C5 C6 C11 C10 174.9(4) . . . . ? C7 C6 C11 C10 -2.8(5) . . . . ? C5 C6 C11 C2 -1.1(5) . . . . ? C7 C6 C11 C2 -178.8(4) . . . . ? C9 C10 C11 C6 -0.3(5) . . . . ? C12 C10 C11 C6 -178.9(3) . . . . ? C9 C10 C11 C2 175.1(4) . . . . ? C12 C10 C11 C2 -3.4(6) . . . . ? C3 C2 C11 C6 4.8(5) . . . . ? C1 C2 C11 C6 -171.3(4) . . . . ? C3 C2 C11 C10 -170.7(4) . . . . ? C1 C2 C11 C10 13.2(6) . . . . ? C9 C10 C12 P12 87.3(4) . . . . ? C11 C10 C12 P12 -94.2(4) . . . . ? C10 C12 P12 C31 177.0(3) . . . . ? C10 C12 P12 C25 -77.2(3) . . . . ? C10 C12 P12 Pd1 50.1(3) . . . . ? C38 Pd1 P12 C31 95.72(19) . . . . ? C39 Pd1 P12 C31 103.7(3) . . . . ? P1 Pd1 P12 C31 -76.10(15) . . . . ? C38 Pd1 P12 C25 -27.12(19) . . . . ? C39 Pd1 P12 C25 -19.1(3) . . . . ? P1 Pd1 P12 C25 161.06(15) . . . . ? C38 Pd1 P12 C12 -143.24(19) . . . . ? C39 Pd1 P12 C12 -135.3(3) . . . . ? P1 Pd1 P12 C12 44.93(15) . . . . ? C19 P1 C13 C18 -101.0(3) . . . . ? C1 P1 C13 C18 153.9(3) . . . . ? Pd1 P1 C13 C18 27.9(4) . . . . ? C19 P1 C13 C14 75.5(4) . . . . ? C1 P1 C13 C14 -29.6(4) . . . . ? Pd1 P1 C13 C14 -155.6(3) . . . . ? C18 C13 C14 C15 2.6(7) . . . . ? P1 C13 C14 C15 -173.9(4) . . . . ? C13 C14 C15 C16 -1.1(8) . . . . ? C14 C15 C16 C17 -0.9(8) . . . . ? C15 C16 C17 C18 1.5(7) . . . . ? C16 C17 C18 C13 0.1(7) . . . . ? C14 C13 C18 C17 -2.1(6) . . . . ? P1 C13 C18 C17 174.6(3) . . . . ? C13 P1 C19 C20 164.8(3) . . . . ? C1 P1 C19 C20 -88.9(4) . . . . ? Pd1 P1 C19 C20 44.2(4) . . . . ? C13 P1 C19 C24 -12.8(4) . . . . ? C1 P1 C19 C24 93.5(4) . . . . ? Pd1 P1 C19 C24 -133.5(3) . . . . ? C24 C19 C20 C21 -0.1(6) . . . . ? P1 C19 C20 C21 -177.8(3) . . . . ? C19 C20 C21 C22 0.2(7) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 C24 0.3(8) . . . . ? C22 C23 C24 C19 -0.3(7) . . . . ? C20 C19 C24 C23 0.2(6) . . . . ? P1 C19 C24 C23 177.8(3) . . . . ? C31 P12 C25 C26 35.9(4) . . . . ? C12 P12 C25 C26 -70.7(4) . . . . ? Pd1 P12 C25 C26 164.6(3) . . . . ? C31 P12 C25 C30 -152.6(3) . . . . ? C12 P12 C25 C30 100.8(3) . . . . ? Pd1 P12 C25 C30 -23.9(4) . . . . ? C30 C25 C26 C27 -0.3(6) . . . . ? P12 C25 C26 C27 171.2(4) . . . . ? C25 C26 C27 C28 0.9(7) . . . . ? C26 C27 C28 C29 -0.8(7) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? C28 C29 C30 C25 0.4(7) . . . . ? C26 C25 C30 C29 -0.3(6) . . . . ? P12 C25 C30 C29 -172.1(3) . . . . ? C25 P12 C31 C36 92.7(3) . . . . ? C12 P12 C31 C36 -165.0(3) . . . . ? Pd1 P12 C31 C36 -38.1(4) . . . . ? C25 P12 C31 C32 -85.9(4) . . . . ? C12 P12 C31 C32 16.4(4) . . . . ? Pd1 P12 C31 C32 143.2(3) . . . . ? C36 C31 C32 C33 -1.2(7) . . . . ? P12 C31 C32 C33 177.4(4) . . . . ? C31 C32 C33 C34 -0.7(8) . . . . ? C32 C33 C34 C35 1.5(9) . . . . ? C33 C34 C35 C36 -0.5(8) . . . . ? C34 C35 C36 C31 -1.4(8) . . . . ? C32 C31 C36 C35 2.2(7) . . . . ? P12 C31 C36 C35 -176.5(4) . . . . ? O37 C37 C38 C39 -3.9(6) . . . . ? C46 C37 C38 C39 174.1(3) . . . . ? O37 C37 C38 Pd1 -78.2(4) . . . . ? C46 C37 C38 Pd1 99.8(3) . . . . ? P1 Pd1 C38 C39 -20.9(3) . . . . ? P12 Pd1 C38 C39 173.8(2) . . . . ? C39 Pd1 C38 C37 122.2(4) . . . . ? P1 Pd1 C38 C37 101.3(3) . . . . ? P12 Pd1 C38 C37 -63.9(3) . . . . ? C37 C38 C39 C40 168.4(3) . . . . ? Pd1 C38 C39 C40 -102.9(3) . . . . ? C37 C38 C39 Pd1 -88.7(3) . . . . ? P1 Pd1 C39 C38 167.9(2) . . . . ? P12 Pd1 C39 C38 -11.9(4) . . . . ? C38 Pd1 C39 C40 119.0(4) . . . . ? P1 Pd1 C39 C40 -73.1(3) . . . . ? P12 Pd1 C39 C40 107.1(3) . . . . ? C38 C39 C40 C45 -146.1(4) . . . . ? Pd1 C39 C40 C45 134.5(3) . . . . ? C38 C39 C40 C41 35.6(6) . . . . ? Pd1 C39 C40 C41 -43.7(4) . . . . ? C45 C40 C41 C42 -1.7(6) . . . . ? C39 C40 C41 C42 176.6(4) . . . . ? C40 C41 C42 C43 0.9(7) . . . . ? C41 C42 C43 C44 0.6(7) . . . . ? C42 C43 C44 C45 -1.2(7) . . . . ? C43 C44 C45 C40 0.3(7) . . . . ? C41 C40 C45 C44 1.1(6) . . . . ? C39 C40 C45 C44 -177.2(4) . . . . ? O37 C37 C46 C47 1.8(6) . . . . ? C38 C37 C46 C47 -176.2(4) . . . . ? C37 C46 C47 C48 174.3(4) . . . . ? C46 C47 C48 C49 174.9(5) . . . . ? C46 C47 C48 C53 -6.0(7) . . . . ? C53 C48 C49 C50 -0.1(9) . . . . ? C47 C48 C49 C50 179.0(6) . . . . ? C48 C49 C50 C51 1.4(11) . . . . ? C49 C50 C51 C52 -1.0(11) . . . . ? C50 C51 C52 C53 -0.7(9) . . . . ? C51 C52 C53 C48 1.9(8) . . . . ? C49 C48 C53 C52 -1.5(8) . . . . ? C47 C48 C53 C52 179.3(5) . . . . ? C54 C55 O56 C57 179.0(6) . . . . ? C55 O56 C57 C58 -176.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.045 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.106