# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ross.harrington@newcastle.ac.uk _publ_contact_author_name 'R. W. Harrington' loop_ _publ_author_name 'Lee Higham' 'Arne Ficks' 'Ross Harrington' 'Rachel M. Hiney' 'Declan G. Gilheany' data_ljh66_compound_7a _database_code_depnum_ccdc_archive 'CCDC 840097' #TrackingRef 'RWHLJHchemcomm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Cl O2 P Pd, C H2 Cl2' _chemical_formula_sum 'C45 H34 Cl3 O2 P Pd' _chemical_formula_weight 850.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 11.9353(3) _cell_length_b 13.7947(4) _cell_length_c 22.2867(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3669.37(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10221 _cell_measurement_theta_min 2.8984 _cell_measurement_theta_max 28.5839 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7279 _exptl_absorpt_correction_T_max 0.7937 _exptl_absorpt_process_details ; 'Tue Nov 30 15:50:14 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 19447 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.65 _reflns_number_total 7808 _reflns_number_gt 6453 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(14) _chemical_absolute_configuration ad _refine_ls_number_reflns 7808 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0444 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.657419(16) 0.968048(14) 0.985217(9) 0.01511(5) Uani 1 1 d . . . Cl1 Cl 0.50585(6) 1.07931(5) 0.97406(3) 0.02347(16) Uani 1 1 d . . . Cl2 Cl 0.40959(7) 0.26794(7) 0.81507(4) 0.0446(2) Uani 1 1 d . . . Cl3 Cl 0.59517(7) 0.33842(6) 0.88804(4) 0.0400(2) Uani 1 1 d . . . P P 0.67466(6) 0.94343(4) 0.88595(3) 0.01351(15) Uani 1 1 d . . . O1 O 0.71007(13) 1.04306(12) 0.85160(7) 0.0147(4) Uani 1 1 d . . . O2 O 0.77871(14) 0.87282(12) 0.86856(8) 0.0142(4) Uani 1 1 d . . . C1 C 0.8129(2) 1.08027(18) 0.87294(11) 0.0151(6) Uani 1 1 d . . . C2 C 0.8095(2) 1.15479(17) 0.91480(12) 0.0165(6) Uani 1 1 d . . . H2A H 0.7398 1.1803 0.9280 0.020 Uiso 1 1 calc R . . C3 C 0.9075(2) 1.19066(18) 0.93667(12) 0.0186(6) Uani 1 1 d . . . H3A H 0.9058 1.2424 0.9648 0.022 Uiso 1 1 calc R . . C4 C 1.0117(2) 1.15223(18) 0.91830(11) 0.0158(6) Uani 1 1 d . . . C5 C 1.1139(2) 1.1866(2) 0.94297(13) 0.0214(7) Uani 1 1 d . . . H5A H 1.1123 1.2385 0.9710 0.026 Uiso 1 1 calc R . . C6 C 1.2132(2) 1.1473(2) 0.92742(12) 0.0235(7) Uani 1 1 d . . . H6A H 1.2807 1.1713 0.9444 0.028 Uiso 1 1 calc R . . C7 C 1.2164(2) 1.06977(19) 0.88552(12) 0.0225(7) Uani 1 1 d . . . H7A H 1.2861 1.0411 0.8750 0.027 Uiso 1 1 calc R . . C8 C 1.12026(19) 1.0366(2) 0.86044(11) 0.0172(6) Uani 1 1 d . . . H8A H 1.1243 0.9852 0.8321 0.021 Uiso 1 1 calc R . . C9 C 1.0144(2) 1.07571(17) 0.87498(11) 0.0133(6) Uani 1 1 d . . . C10 C 0.9107(2) 1.04125(19) 0.85094(10) 0.0141(5) Uani 1 1 d . . . C11 C 0.9029(2) 0.9631(2) 0.80475(10) 0.0136(5) Uani 1 1 d . . . C12 C 0.95991(19) 0.9692(2) 0.74786(10) 0.0140(5) Uani 1 1 d . . . C13 C 1.0213(2) 1.05288(17) 0.73030(11) 0.0157(6) Uani 1 1 d . . . H13A H 1.0252 1.1073 0.7564 0.019 Uiso 1 1 calc R . . C14 C 1.0745(2) 1.05538(19) 0.67613(12) 0.0186(6) Uani 1 1 d . . . H14A H 1.1145 1.1121 0.6648 0.022 Uiso 1 1 calc R . . C15 C 1.0715(2) 0.9769(2) 0.63717(11) 0.0206(6) Uani 1 1 d . . . H15A H 1.1117 0.9792 0.6004 0.025 Uiso 1 1 calc R . . C16 C 1.0114(2) 0.89700(19) 0.65156(12) 0.0183(6) Uani 1 1 d . . . H16A H 1.0084 0.8442 0.6242 0.022 Uiso 1 1 calc R . . C17 C 0.9527(2) 0.89088(18) 0.70674(12) 0.0156(6) Uani 1 1 d . . . C18 C 0.8848(2) 0.81041(19) 0.72047(12) 0.0186(6) Uani 1 1 d . . . H18A H 0.8796 0.7582 0.6928 0.022 Uiso 1 1 calc R . . C19 C 0.8264(2) 0.80671(17) 0.77293(11) 0.0153(6) Uani 1 1 d . . . H19A H 0.7794 0.7528 0.7815 0.018 Uiso 1 1 calc R . . C20 C 0.8361(2) 0.88316(17) 0.81417(10) 0.0142(5) Uani 1 1 d . . . C21 C 0.5555(2) 0.90943(18) 0.83990(11) 0.0146(6) Uani 1 1 d . . . C22 C 0.5068(2) 0.9791(2) 0.80068(11) 0.0194(6) Uani 1 1 d . . . H22A H 0.5431 1.0397 0.7948 0.023 Uiso 1 1 calc R . . C23 C 0.4090(2) 0.9603(2) 0.77137(11) 0.0220(6) Uani 1 1 d . . . H23A H 0.3772 1.0082 0.7459 0.026 Uiso 1 1 calc R . . C24 C 0.3545(2) 0.86991(18) 0.77853(11) 0.0185(6) Uani 1 1 d . . . C25 C 0.2524(2) 0.8487(2) 0.74816(13) 0.0246(7) Uani 1 1 d . . . H25A H 0.2189 0.8964 0.7232 0.030 Uiso 1 1 calc R . . C26 C 0.2025(2) 0.7606(2) 0.75459(14) 0.0292(8) Uani 1 1 d . . . H26A H 0.1342 0.7474 0.7343 0.035 Uiso 1 1 calc R . . C27 C 0.2515(2) 0.6892(2) 0.79101(13) 0.0285(7) Uani 1 1 d . . . H27A H 0.2165 0.6276 0.7948 0.034 Uiso 1 1 calc R . . C28 C 0.3488(3) 0.70735(18) 0.82091(12) 0.0216(6) Uani 1 1 d . . . H28A H 0.3803 0.6586 0.8458 0.026 Uiso 1 1 calc R . . C29 C 0.4036(2) 0.79817(19) 0.81538(12) 0.0167(6) Uani 1 1 d . . . C30 C 0.5051(2) 0.81974(18) 0.84707(11) 0.0148(6) Uani 1 1 d . . . C31 C 0.5554(2) 0.74236(19) 0.88571(13) 0.0159(6) Uani 1 1 d . . . C32 C 0.6135(2) 0.66719(18) 0.85963(13) 0.0191(6) Uani 1 1 d . . . H32A H 0.6210 0.6650 0.8172 0.023 Uiso 1 1 calc R . . C33 C 0.6615(3) 0.59408(18) 0.89455(13) 0.0249(6) Uani 1 1 d . . . H33A H 0.7000 0.5423 0.8755 0.030 Uiso 1 1 calc R . . C34 C 0.6540(3) 0.59596(18) 0.95565(12) 0.0260(7) Uani 1 1 d . . . H34A H 0.6903 0.5475 0.9788 0.031 Uiso 1 1 calc R . . C35 C 0.5922(2) 0.66993(18) 0.98445(15) 0.0200(6) Uani 1 1 d . . . C36 C 0.5783(3) 0.6728(2) 1.04739(14) 0.0314(8) Uani 1 1 d . . . H36A H 0.6145 0.6254 1.0715 0.038 Uiso 1 1 calc R . . C37 C 0.5149(3) 0.7413(2) 1.07405(13) 0.0290(8) Uani 1 1 d . . . H37A H 0.5073 0.7421 1.1165 0.035 Uiso 1 1 calc R . . C38 C 0.4601(3) 0.8113(2) 1.03910(13) 0.0259(7) Uani 1 1 d . . . H38A H 0.4132 0.8578 1.0580 0.031 Uiso 1 1 calc R . . C39 C 0.4732(2) 0.81367(18) 0.97815(13) 0.0200(6) Uani 1 1 d . . . H39A H 0.4371 0.8628 0.9554 0.024 Uiso 1 1 calc R . . C40 C 0.5400(2) 0.74348(19) 0.94860(12) 0.0173(6) Uani 1 1 d . . . C41 C 0.7869(2) 0.9537(2) 1.05340(11) 0.0203(6) Uani 1 1 d . . . C42 C 0.8836(2) 1.0214(2) 1.05437(13) 0.0287(7) Uani 1 1 d . . . H42A H 0.9383 0.9995 1.0842 0.043 Uiso 1 1 calc R . . H42B H 0.8575 1.0866 1.0648 0.043 Uiso 1 1 calc R . . H42C H 0.9189 1.0228 1.0147 0.043 Uiso 1 1 calc R . . C43 C 0.6876(2) 0.9744(2) 1.08280(11) 0.0265(7) Uani 1 1 d . . . H43A H 0.6819 1.0390 1.1019 0.032 Uiso 1 1 calc R . . H43B H 0.6547 0.9216 1.1072 0.032 Uiso 1 1 calc R . . C44 C 0.7830(2) 0.87311(18) 1.01415(14) 0.0227(6) Uani 1 1 d . . . H44A H 0.7573 0.8112 1.0319 0.027 Uiso 1 1 calc R . . H44B H 0.8479 0.8652 0.9869 0.027 Uiso 1 1 calc R . . C45 C 0.5401(3) 0.2402(2) 0.84761(14) 0.0308(8) Uani 1 1 d . . . H45A H 0.5313 0.1840 0.8749 0.037 Uiso 1 1 calc R . . H45B H 0.5935 0.2216 0.8156 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01227(9) 0.01849(9) 0.01458(9) -0.00070(9) -0.00052(10) 0.00143(10) Cl1 0.0205(4) 0.0241(3) 0.0257(4) 0.0011(3) 0.0001(3) 0.0074(3) Cl2 0.0325(5) 0.0613(6) 0.0399(5) 0.0073(4) -0.0045(4) -0.0019(5) Cl3 0.0416(5) 0.0361(5) 0.0422(5) -0.0107(4) -0.0064(4) 0.0094(4) P 0.0130(4) 0.0124(3) 0.0151(3) 0.0009(2) -0.0009(3) 0.0002(3) O1 0.0132(9) 0.0125(9) 0.0184(9) 0.0017(8) 0.0002(7) -0.0016(8) O2 0.0148(10) 0.0111(9) 0.0167(10) 0.0015(8) 0.0029(8) 0.0019(8) C1 0.0156(16) 0.0139(13) 0.0156(14) 0.0044(11) -0.0015(11) -0.0016(12) C2 0.0164(16) 0.0120(13) 0.0211(15) -0.0016(11) 0.0069(11) 0.0022(12) C3 0.0261(17) 0.0107(13) 0.0190(15) -0.0019(12) 0.0044(13) -0.0009(13) C4 0.0176(16) 0.0144(14) 0.0153(14) 0.0056(11) -0.0002(12) -0.0025(13) C5 0.0265(17) 0.0193(15) 0.0183(15) 0.0002(12) -0.0006(13) -0.0088(14) C6 0.0193(17) 0.0295(17) 0.0218(17) 0.0014(13) -0.0047(13) -0.0080(14) C7 0.0194(16) 0.0247(16) 0.0233(16) 0.0040(13) -0.0015(13) 0.0030(13) C8 0.0174(14) 0.0179(13) 0.0162(13) -0.0006(13) 0.0013(10) 0.0010(13) C9 0.0150(14) 0.0143(13) 0.0106(13) 0.0058(10) -0.0006(11) -0.0008(12) C10 0.0183(14) 0.0131(13) 0.0109(12) 0.0036(12) 0.0012(10) -0.0027(13) C11 0.0112(13) 0.0138(13) 0.0157(13) 0.0025(12) -0.0020(10) 0.0032(13) C12 0.0103(13) 0.0160(13) 0.0156(13) 0.0017(13) -0.0028(10) 0.0019(13) C13 0.0150(14) 0.0153(15) 0.0167(14) -0.0002(11) -0.0014(11) -0.0002(12) C14 0.0185(15) 0.0195(16) 0.0178(15) 0.0048(11) -0.0009(12) -0.0006(13) C15 0.0168(14) 0.0328(16) 0.0122(13) 0.0046(14) 0.0010(11) 0.0016(14) C16 0.0187(16) 0.0220(15) 0.0143(14) -0.0048(12) -0.0020(12) 0.0031(13) C17 0.0133(15) 0.0182(15) 0.0152(14) 0.0003(11) -0.0038(11) 0.0050(12) C18 0.0198(16) 0.0151(14) 0.0209(15) -0.0036(12) -0.0032(12) 0.0030(12) C19 0.0106(15) 0.0126(13) 0.0226(15) -0.0023(11) -0.0024(12) -0.0001(12) C20 0.0131(14) 0.0154(13) 0.0141(13) 0.0011(10) -0.0001(13) 0.0053(14) C21 0.0181(15) 0.0162(14) 0.0094(13) -0.0002(11) 0.0002(11) 0.0013(12) C22 0.0218(15) 0.0153(14) 0.0210(14) -0.0007(12) 0.0004(12) -0.0019(14) C23 0.0280(16) 0.0178(14) 0.0202(15) 0.0011(14) -0.0077(12) 0.0075(15) C24 0.0185(16) 0.0211(14) 0.0159(14) -0.0024(11) -0.0023(12) -0.0008(14) C25 0.0219(17) 0.0255(17) 0.0265(17) -0.0020(13) -0.0092(13) 0.0052(14) C26 0.0177(16) 0.0345(18) 0.0353(19) -0.0020(15) -0.0091(14) -0.0048(15) C27 0.0247(18) 0.0273(17) 0.0335(18) 0.0031(14) -0.0042(14) -0.0095(15) C28 0.0194(16) 0.0228(14) 0.0227(15) 0.0027(11) -0.0036(14) -0.0025(15) C29 0.0140(15) 0.0199(15) 0.0162(15) 0.0006(12) 0.0012(12) -0.0015(13) C30 0.0175(15) 0.0146(13) 0.0124(14) -0.0018(11) 0.0034(12) 0.0007(12) C31 0.0105(14) 0.0165(14) 0.0207(15) 0.0009(12) -0.0020(12) -0.0065(12) C32 0.0174(15) 0.0159(14) 0.0239(16) -0.0020(12) 0.0063(12) -0.0025(12) C33 0.0172(15) 0.0166(13) 0.0408(18) 0.0021(12) 0.0061(16) 0.0020(15) C34 0.0169(15) 0.0204(14) 0.0406(18) 0.0136(12) -0.0076(15) -0.0034(15) C35 0.0185(14) 0.0181(14) 0.0234(15) 0.0066(14) -0.0046(15) -0.0084(12) C36 0.034(2) 0.0322(19) 0.0284(19) 0.0192(16) -0.0093(16) -0.0133(17) C37 0.042(2) 0.0313(19) 0.0135(17) 0.0006(14) 0.0006(15) -0.0147(17) C38 0.0273(18) 0.0271(16) 0.0232(17) -0.0072(13) 0.0033(13) -0.0101(14) C39 0.0236(15) 0.0178(14) 0.0184(16) -0.0010(13) -0.0003(14) -0.0087(12) C40 0.0142(15) 0.0173(15) 0.0205(16) 0.0000(12) 0.0016(12) -0.0066(12) C41 0.0167(14) 0.0289(17) 0.0154(14) 0.0030(13) -0.0083(11) 0.0058(14) C42 0.0242(16) 0.0295(16) 0.0325(17) -0.0003(15) -0.0101(12) -0.0037(15) C43 0.0274(18) 0.0391(17) 0.0131(13) 0.0011(14) -0.0040(11) 0.0070(16) C44 0.0180(14) 0.0265(14) 0.0235(14) 0.0079(15) -0.0039(14) 0.0056(12) C45 0.036(2) 0.0236(16) 0.0330(19) 0.0041(14) 0.0022(15) 0.0011(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl1 2.3854(7) . ? Pd P 2.2476(7) . ? Pd C41 2.176(2) . ? Pd C43 2.206(2) . ? Pd C44 2.093(2) . ? Cl2 C45 1.760(3) . ? Cl3 C45 1.755(3) . ? P O1 1.6289(18) . ? P O2 1.6252(18) . ? P C21 1.816(3) . ? O1 C1 1.413(3) . ? O2 C20 1.400(3) . ? C1 C2 1.389(4) . ? C1 C10 1.375(3) . ? C2 H2A 0.950 . ? C2 C3 1.360(4) . ? C3 H3A 0.950 . ? C3 C4 1.412(4) . ? C4 C5 1.420(4) . ? C4 C9 1.431(4) . ? C5 H5A 0.950 . ? C5 C6 1.349(4) . ? C6 H6A 0.950 . ? C6 C7 1.420(4) . ? C7 H7A 0.950 . ? C7 C8 1.356(4) . ? C8 H8A 0.950 . ? C8 C9 1.412(3) . ? C9 C10 1.430(3) . ? C10 C11 1.494(4) . ? C11 C12 1.442(3) . ? C11 C20 1.376(4) . ? C12 C13 1.422(3) . ? C12 C17 1.419(4) . ? C13 H13A 0.950 . ? C13 C14 1.365(3) . ? C14 H14A 0.950 . ? C14 C15 1.388(4) . ? C15 H15A 0.950 . ? C15 C16 1.354(4) . ? C16 H16A 0.950 . ? C16 C17 1.417(4) . ? C17 C18 1.409(4) . ? C18 H18A 0.950 . ? C18 C19 1.362(4) . ? C19 H19A 0.950 . ? C19 C20 1.404(3) . ? C21 C22 1.423(3) . ? C21 C30 1.385(3) . ? C22 H22A 0.950 . ? C22 C23 1.363(3) . ? C23 H23A 0.950 . ? C23 C24 1.415(4) . ? C24 C25 1.424(4) . ? C24 C29 1.413(4) . ? C25 H25A 0.950 . ? C25 C26 1.360(4) . ? C26 H26A 0.950 . ? C26 C27 1.404(4) . ? C27 H27A 0.950 . ? C27 C28 1.362(4) . ? C28 H28A 0.950 . ? C28 C29 1.419(4) . ? C29 C30 1.434(4) . ? C30 C31 1.497(4) . ? C31 C32 1.376(4) . ? C31 C40 1.414(4) . ? C32 H32A 0.950 . ? C32 C33 1.397(4) . ? C33 H33A 0.950 . ? C33 C34 1.365(4) . ? C34 H34A 0.950 . ? C34 C35 1.413(4) . ? C35 C36 1.413(4) . ? C35 C40 1.433(4) . ? C36 H36A 0.950 . ? C36 C37 1.348(4) . ? C37 H37A 0.950 . ? C37 C38 1.403(4) . ? C38 H38A 0.950 . ? C38 C39 1.368(4) . ? C39 H39A 0.950 . ? C39 C40 1.417(4) . ? C41 C42 1.486(4) . ? C41 C43 1.384(4) . ? C41 C44 1.415(4) . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd P 93.67(2) . . ? Cl1 Pd C41 132.07(7) . . ? Cl1 Pd C43 101.60(7) . . ? Cl1 Pd C44 168.01(9) . . ? P Pd C41 127.47(7) . . ? P Pd C43 164.02(7) . . ? P Pd C44 98.23(9) . . ? C41 Pd C43 36.82(9) . . ? C41 Pd C44 38.65(10) . . ? C43 Pd C44 66.68(11) . . ? Pd P O1 111.03(6) . . ? Pd P O2 113.28(7) . . ? Pd P C21 121.58(9) . . ? O1 P O2 101.27(9) . . ? O1 P C21 98.95(10) . . ? O2 P C21 108.00(10) . . ? P O1 C1 111.94(14) . . ? P O2 C20 121.29(15) . . ? O1 C1 C2 118.0(2) . . ? O1 C1 C10 118.3(2) . . ? C2 C1 C10 123.7(2) . . ? C1 C2 H2A 120.5 . . ? C1 C2 C3 119.0(2) . . ? H2A C2 C3 120.5 . . ? C2 C3 H3A 119.5 . . ? C2 C3 C4 121.1(2) . . ? H3A C3 C4 119.5 . . ? C3 C4 C5 121.3(2) . . ? C3 C4 C9 119.5(2) . . ? C5 C4 C9 119.2(2) . . ? C4 C5 H5A 119.3 . . ? C4 C5 C6 121.4(3) . . ? H5A C5 C6 119.3 . . ? C5 C6 H6A 120.2 . . ? C5 C6 C7 119.7(3) . . ? H6A C6 C7 120.2 . . ? C6 C7 H7A 119.9 . . ? C6 C7 C8 120.2(3) . . ? H7A C7 C8 119.9 . . ? C7 C8 H8A 118.9 . . ? C7 C8 C9 122.3(3) . . ? H8A C8 C9 118.9 . . ? C4 C9 C8 117.2(2) . . ? C4 C9 C10 118.6(2) . . ? C8 C9 C10 124.2(2) . . ? C1 C10 C9 118.1(2) . . ? C1 C10 C11 118.4(2) . . ? C9 C10 C11 123.5(2) . . ? C10 C11 C12 122.3(2) . . ? C10 C11 C20 120.6(2) . . ? C12 C11 C20 117.0(2) . . ? C11 C12 C13 122.2(2) . . ? C11 C12 C17 119.7(2) . . ? C13 C12 C17 118.1(2) . . ? C12 C13 H13A 119.9 . . ? C12 C13 C14 120.2(2) . . ? H13A C13 C14 119.9 . . ? C13 C14 H14A 119.3 . . ? C13 C14 C15 121.4(2) . . ? H14A C14 C15 119.3 . . ? C14 C15 H15A 120.0 . . ? C14 C15 C16 120.0(2) . . ? H15A C15 C16 120.0 . . ? C15 C16 H16A 119.5 . . ? C15 C16 C17 121.1(2) . . ? H16A C16 C17 119.5 . . ? C12 C17 C16 119.0(2) . . ? C12 C17 C18 119.6(2) . . ? C16 C17 C18 121.3(2) . . ? C17 C18 H18A 119.6 . . ? C17 C18 C19 120.7(2) . . ? H18A C18 C19 119.6 . . ? C18 C19 H19A 120.3 . . ? C18 C19 C20 119.4(2) . . ? H19A C19 C20 120.3 . . ? O2 C20 C11 119.8(2) . . ? O2 C20 C19 116.7(2) . . ? C11 C20 C19 123.4(2) . . ? P C21 C22 119.49(19) . . ? P C21 C30 120.38(19) . . ? C22 C21 C30 119.8(2) . . ? C21 C22 H22A 119.5 . . ? C21 C22 C23 121.0(3) . . ? H22A C22 C23 119.5 . . ? C22 C23 H23A 119.7 . . ? C22 C23 C24 120.6(3) . . ? H23A C23 C24 119.7 . . ? C23 C24 C25 121.4(2) . . ? C23 C24 C29 119.4(2) . . ? C25 C24 C29 119.1(2) . . ? C24 C25 H25A 119.7 . . ? C24 C25 C26 120.5(3) . . ? H25A C25 C26 119.7 . . ? C25 C26 H26A 119.8 . . ? C25 C26 C27 120.4(3) . . ? H26A C26 C27 119.8 . . ? C26 C27 H27A 119.7 . . ? C26 C27 C28 120.6(3) . . ? H27A C27 C28 119.7 . . ? C27 C28 H28A 119.6 . . ? C27 C28 C29 120.9(3) . . ? H28A C28 C29 119.6 . . ? C24 C29 C28 118.5(2) . . ? C24 C29 C30 119.4(2) . . ? C28 C29 C30 122.0(2) . . ? C21 C30 C29 119.7(2) . . ? C21 C30 C31 121.9(2) . . ? C29 C30 C31 118.3(2) . . ? C30 C31 C32 119.8(2) . . ? C30 C31 C40 120.7(2) . . ? C32 C31 C40 119.5(2) . . ? C31 C32 H32A 119.5 . . ? C31 C32 C33 121.0(3) . . ? H32A C32 C33 119.5 . . ? C32 C33 H33A 119.5 . . ? C32 C33 C34 121.0(3) . . ? H33A C33 C34 119.5 . . ? C33 C34 H34A 120.0 . . ? C33 C34 C35 120.1(3) . . ? H34A C34 C35 120.0 . . ? C34 C35 C36 122.2(3) . . ? C34 C35 C40 119.0(3) . . ? C36 C35 C40 118.9(3) . . ? C35 C36 H36A 119.2 . . ? C35 C36 C37 121.5(3) . . ? H36A C36 C37 119.2 . . ? C36 C37 H37A 120.0 . . ? C36 C37 C38 120.0(3) . . ? H37A C37 C38 120.0 . . ? C37 C38 H38A 119.5 . . ? C37 C38 C39 121.0(3) . . ? H38A C38 C39 119.5 . . ? C38 C39 H39A 119.7 . . ? C38 C39 C40 120.7(3) . . ? H39A C39 C40 119.7 . . ? C31 C40 C35 119.2(2) . . ? C31 C40 C39 122.8(2) . . ? C35 C40 C39 118.0(3) . . ? Pd C41 C42 120.30(18) . . ? Pd C41 C43 72.75(14) . . ? Pd C41 C44 67.47(14) . . ? C42 C41 C43 121.9(3) . . ? C42 C41 C44 121.9(2) . . ? C43 C41 C44 115.3(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Pd C43 C41 70.43(15) . . ? Pd C43 H43A 116.6 . . ? Pd C43 H43B 116.6 . . ? C41 C43 H43A 116.6 . . ? C41 C43 H43B 116.6 . . ? H43A C43 H43B 113.6 . . ? Pd C44 C41 73.88(14) . . ? Pd C44 H44A 116.1 . . ? Pd C44 H44B 116.1 . . ? C41 C44 H44A 116.1 . . ? C41 C44 H44B 116.1 . . ? H44A C44 H44B 113.1 . . ? Cl2 C45 Cl3 112.03(16) . . ? Cl2 C45 H45A 109.2 . . ? Cl2 C45 H45B 109.2 . . ? Cl3 C45 H45A 109.2 . . ? Cl3 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd P O1 63.33(7) . . . . ? Cl1 Pd P O2 176.49(7) . . . . ? Cl1 Pd P C21 -52.26(10) . . . . ? C41 Pd P O1 -90.20(12) . . . . ? C41 Pd P O2 22.96(12) . . . . ? C41 Pd P C21 154.21(13) . . . . ? C43 Pd P O1 -99.5(3) . . . . ? C43 Pd P O2 13.6(3) . . . . ? C43 Pd P C21 144.9(3) . . . . ? C44 Pd P O1 -118.14(10) . . . . ? C44 Pd P O2 -4.98(10) . . . . ? C44 Pd P C21 126.27(12) . . . . ? Pd P O1 C1 59.40(16) . . . . ? O2 P O1 C1 -61.15(17) . . . . ? C21 P O1 C1 -171.65(16) . . . . ? Pd P O2 C20 -149.54(16) . . . . ? O1 P O2 C20 -30.6(2) . . . . ? C21 P O2 C20 72.8(2) . . . . ? P O1 C1 C2 -98.8(2) . . . . ? P O1 C1 C10 81.5(2) . . . . ? O1 C1 C2 C3 179.0(2) . . . . ? C10 C1 C2 C3 -1.4(4) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C2 C3 C4 C5 -177.2(3) . . . . ? C2 C3 C4 C9 1.4(4) . . . . ? C3 C4 C5 C6 177.1(3) . . . . ? C9 C4 C5 C6 -1.5(4) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C5 C6 C7 C8 1.2(4) . . . . ? C6 C7 C8 C9 -0.8(4) . . . . ? C7 C8 C9 C4 -0.7(4) . . . . ? C7 C8 C9 C10 -178.2(2) . . . . ? C3 C4 C9 C8 -176.9(2) . . . . ? C3 C4 C9 C10 0.8(3) . . . . ? C5 C4 C9 C8 1.8(3) . . . . ? C5 C4 C9 C10 179.5(2) . . . . ? O1 C1 C10 C9 -176.8(2) . . . . ? O1 C1 C10 C11 1.2(3) . . . . ? C2 C1 C10 C9 3.6(4) . . . . ? C2 C1 C10 C11 -178.4(2) . . . . ? C4 C9 C10 C1 -3.2(3) . . . . ? C4 C9 C10 C11 178.9(2) . . . . ? C8 C9 C10 C1 174.3(2) . . . . ? C8 C9 C10 C11 -3.6(4) . . . . ? C1 C10 C11 C12 126.0(3) . . . . ? C1 C10 C11 C20 -51.2(3) . . . . ? C9 C10 C11 C12 -56.0(3) . . . . ? C9 C10 C11 C20 126.7(3) . . . . ? C10 C11 C12 C13 -4.3(4) . . . . ? C10 C11 C12 C17 177.6(2) . . . . ? C20 C11 C12 C13 173.0(2) . . . . ? C20 C11 C12 C17 -5.1(4) . . . . ? C11 C12 C13 C14 179.7(2) . . . . ? C17 C12 C13 C14 -2.2(4) . . . . ? C12 C13 C14 C15 -0.7(4) . . . . ? C13 C14 C15 C16 2.6(4) . . . . ? C14 C15 C16 C17 -1.4(4) . . . . ? C15 C16 C17 C12 -1.5(4) . . . . ? C15 C16 C17 C18 176.3(2) . . . . ? C11 C12 C17 C16 -178.6(2) . . . . ? C11 C12 C17 C18 3.6(4) . . . . ? C13 C12 C17 C16 3.3(4) . . . . ? C13 C12 C17 C18 -174.5(2) . . . . ? C12 C17 C18 C19 -0.4(4) . . . . ? C16 C17 C18 C19 -178.1(2) . . . . ? C17 C18 C19 C20 -1.3(4) . . . . ? C10 C11 C20 O2 -2.8(4) . . . . ? C10 C11 C20 C19 -179.1(2) . . . . ? C12 C11 C20 O2 179.8(2) . . . . ? C12 C11 C20 C19 3.5(4) . . . . ? P O2 C20 C11 69.5(3) . . . . ? P O2 C20 C19 -113.9(2) . . . . ? C18 C19 C20 O2 -176.7(2) . . . . ? C18 C19 C20 C11 -0.3(4) . . . . ? Pd P C21 C22 106.2(2) . . . . ? Pd P C21 C30 -67.3(2) . . . . ? O1 P C21 C22 -15.3(2) . . . . ? O1 P C21 C30 171.1(2) . . . . ? O2 P C21 C22 -120.3(2) . . . . ? O2 P C21 C30 66.1(2) . . . . ? P C21 C22 C23 -171.4(2) . . . . ? C30 C21 C22 C23 2.2(4) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? C22 C23 C24 C25 -179.8(3) . . . . ? C22 C23 C24 C29 -1.4(4) . . . . ? C23 C24 C25 C26 178.6(3) . . . . ? C29 C24 C25 C26 0.2(4) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C25 C26 C27 C28 0.8(5) . . . . ? C26 C27 C28 C29 -0.9(4) . . . . ? C23 C24 C29 C28 -178.6(2) . . . . ? C23 C24 C29 C30 2.8(4) . . . . ? C25 C24 C29 C28 -0.2(4) . . . . ? C25 C24 C29 C30 -178.7(2) . . . . ? C27 C28 C29 C24 0.6(4) . . . . ? C27 C28 C29 C30 179.0(3) . . . . ? P C21 C30 C29 172.88(19) . . . . ? P C21 C30 C31 -9.1(3) . . . . ? C22 C21 C30 C29 -0.7(4) . . . . ? C22 C21 C30 C31 177.3(2) . . . . ? C24 C29 C30 C21 -1.8(4) . . . . ? C24 C29 C30 C31 -179.9(2) . . . . ? C28 C29 C30 C21 179.7(2) . . . . ? C28 C29 C30 C31 1.7(4) . . . . ? C21 C30 C31 C32 -101.2(3) . . . . ? C21 C30 C31 C40 81.4(3) . . . . ? C29 C30 C31 C32 76.8(3) . . . . ? C29 C30 C31 C40 -100.5(3) . . . . ? C30 C31 C32 C33 179.9(2) . . . . ? C40 C31 C32 C33 -2.7(4) . . . . ? C31 C32 C33 C34 -1.2(4) . . . . ? C32 C33 C34 C35 3.2(4) . . . . ? C33 C34 C35 C36 177.5(3) . . . . ? C33 C34 C35 C40 -1.3(4) . . . . ? C34 C35 C36 C37 -176.9(3) . . . . ? C40 C35 C36 C37 1.9(4) . . . . ? C35 C36 C37 C38 0.5(5) . . . . ? C36 C37 C38 C39 -2.4(4) . . . . ? C37 C38 C39 C40 1.8(4) . . . . ? C30 C31 C40 C35 -178.2(2) . . . . ? C30 C31 C40 C39 3.0(4) . . . . ? C32 C31 C40 C35 4.5(4) . . . . ? C32 C31 C40 C39 -174.4(2) . . . . ? C38 C39 C40 C31 179.5(3) . . . . ? C38 C39 C40 C35 0.6(4) . . . . ? C34 C35 C40 C31 -2.5(4) . . . . ? C34 C35 C40 C39 176.4(2) . . . . ? C36 C35 C40 C31 178.7(2) . . . . ? C36 C35 C40 C39 -2.4(4) . . . . ? Cl1 Pd C41 C42 -76.3(2) . . . . ? Cl1 Pd C41 C43 41.1(2) . . . . ? Cl1 Pd C41 C44 168.87(13) . . . . ? P Pd C41 C42 66.9(2) . . . . ? P Pd C41 C43 -175.72(16) . . . . ? P Pd C41 C44 -47.95(19) . . . . ? C43 Pd C41 C42 -117.4(3) . . . . ? C43 Pd C41 C44 127.8(3) . . . . ? C44 Pd C41 C42 114.8(3) . . . . ? C44 Pd C41 C43 -127.8(3) . . . . ? C42 C41 C43 Pd 115.4(2) . . . . ? C44 C41 C43 Pd -53.8(2) . . . . ? Cl1 Pd C43 C41 -150.12(17) . . . . ? P Pd C43 C41 12.4(4) . . . . ? C44 Pd C43 C41 32.52(18) . . . . ? C42 C41 C44 Pd -112.7(2) . . . . ? C43 C41 C44 Pd 56.6(2) . . . . ? Cl1 Pd C44 C41 -43.6(4) . . . . ? P Pd C44 C41 143.46(15) . . . . ? C43 Pd C44 C41 -31.06(16) . . . . ? _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.286 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.064 data_ljh63_Compound_7b _database_code_depnum_ccdc_archive 'CCDC 840098' #TrackingRef 'RWHLJHchemcomm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Cl O2 P Pd, C H2 Cl2' _chemical_formula_sum 'C45 H34 Cl3 O2 P Pd' _chemical_formula_weight 850.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 12.0059(4) _cell_length_b 13.8615(4) _cell_length_c 22.5034(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3745.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10610 _cell_measurement_theta_min 2.8778 _cell_measurement_theta_max 28.5576 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7972 _exptl_absorpt_correction_T_max 0.8578 _exptl_absorpt_process_details ; 'Fri Nov 19 12:42:18 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 21950 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 28.62 _reflns_number_total 8064 _reflns_number_gt 6146 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(16) _chemical_absolute_configuration ad _refine_ls_number_reflns 8064 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.839611(18) 0.976528(16) 0.489546(9) 0.01697(6) Uani 1 1 d . . . P P 0.82307(7) 0.95551(5) 0.39145(3) 0.01612(17) Uani 1 1 d . . . Cl1 Cl 0.98473(6) 1.09203(5) 0.48159(4) 0.02488(18) Uani 1 1 d . . . Cl2 Cl 0.90876(9) 0.74730(9) 0.19444(5) 0.0591(3) Uani 1 1 d . . . Cl3 Cl 1.07249(9) 0.81805(8) 0.10927(4) 0.0485(3) Uani 1 1 d . . . O1 O 0.72366(17) 0.88013(14) 0.37431(8) 0.0180(5) Uani 1 1 d . . . O2 O 0.78234(15) 1.05228(14) 0.35722(8) 0.0170(5) Uani 1 1 d . . . C1 C 0.6670(3) 0.88606(19) 0.32002(11) 0.0160(6) Uani 1 1 d . . . C2 C 0.6798(3) 0.8088(2) 0.28064(12) 0.0200(7) Uani 1 1 d . . . H2A H 0.7278 0.7566 0.2903 0.024 Uiso 1 1 calc R . . C3 C 0.6228(3) 0.8093(2) 0.22817(13) 0.0220(7) Uani 1 1 d . . . H3A H 0.6285 0.7556 0.2021 0.026 Uiso 1 1 calc R . . C4 C 0.5557(3) 0.8881(2) 0.21223(13) 0.0195(7) Uani 1 1 d . . . C5 C 0.4991(3) 0.8913(2) 0.15707(13) 0.0240(8) Uani 1 1 d . . . H5A H 0.5025 0.8372 0.1312 0.029 Uiso 1 1 calc R . . C6 C 0.4396(2) 0.9709(3) 0.14039(13) 0.0263(7) Uani 1 1 d . . . H6A H 0.4015 0.9718 0.1034 0.032 Uiso 1 1 calc R . . C7 C 0.4351(2) 1.0505(2) 0.17775(13) 0.0231(8) Uani 1 1 d . . . H7A H 0.3959 1.1065 0.1654 0.028 Uiso 1 1 calc R . . C8 C 0.4862(2) 1.0498(2) 0.23212(12) 0.0194(7) Uani 1 1 d . . . H8A H 0.4820 1.1051 0.2569 0.023 Uiso 1 1 calc R . . C9 C 0.5452(2) 0.9675(2) 0.25169(11) 0.0165(6) Uani 1 1 d . . . C10 C 0.5989(2) 0.9632(2) 0.30873(11) 0.0157(6) Uani 1 1 d . . . C11 C 0.5847(2) 1.0411(2) 0.35358(12) 0.0158(7) Uani 1 1 d . . . C12 C 0.4781(2) 1.0708(2) 0.37557(12) 0.0162(7) Uani 1 1 d . . . C13 C 0.3759(2) 1.0284(2) 0.35822(11) 0.0195(6) Uani 1 1 d . . . H13A H 0.3765 0.9766 0.3306 0.023 Uiso 1 1 calc R . . C14 C 0.2766(3) 1.0601(2) 0.38010(13) 0.0250(8) Uani 1 1 d . . . H14A H 0.2093 1.0307 0.3672 0.030 Uiso 1 1 calc R . . C15 C 0.2728(3) 1.1365(2) 0.42191(13) 0.0266(8) Uani 1 1 d . . . H15A H 0.2033 1.1587 0.4367 0.032 Uiso 1 1 calc R . . C16 C 0.3688(3) 1.1778(2) 0.44071(13) 0.0254(8) Uani 1 1 d . . . H16A H 0.3656 1.2285 0.4691 0.030 Uiso 1 1 calc R . . C17 C 0.4741(3) 1.1471(2) 0.41894(12) 0.0179(7) Uani 1 1 d . . . C18 C 0.5736(3) 1.1891(2) 0.43939(13) 0.0208(7) Uani 1 1 d . . . H18A H 0.5704 1.2398 0.4678 0.025 Uiso 1 1 calc R . . C19 C 0.6749(3) 1.1583(2) 0.41910(12) 0.0197(7) Uani 1 1 d . . . H19A H 0.7419 1.1866 0.4333 0.024 Uiso 1 1 calc R . . C20 C 0.6775(2) 1.0846(2) 0.37711(12) 0.0160(7) Uani 1 1 d . . . C21 C 0.9409(2) 0.9250(2) 0.34511(12) 0.0165(7) Uani 1 1 d . . . C22 C 0.9592(2) 0.9735(2) 0.29036(12) 0.0225(7) Uani 1 1 d . . . H22A H 0.9070 1.0201 0.2768 0.027 Uiso 1 1 calc R . . C23 C 1.0514(3) 0.9532(2) 0.25728(14) 0.0258(8) Uani 1 1 d . . . H23A H 1.0643 0.9882 0.2217 0.031 Uiso 1 1 calc R . . C24 C 1.1278(2) 0.8816(2) 0.27475(13) 0.0211(7) Uani 1 1 d . . . C25 C 1.2222(3) 0.8583(3) 0.24007(14) 0.0294(8) Uani 1 1 d . . . H25A H 1.2371 0.8938 0.2049 0.035 Uiso 1 1 calc R . . C26 C 1.2922(3) 0.7856(3) 0.25631(14) 0.0324(8) Uani 1 1 d . . . H26A H 1.3545 0.7700 0.2321 0.039 Uiso 1 1 calc R . . C27 C 1.2722(3) 0.7336(3) 0.30894(15) 0.0362(9) Uani 1 1 d . . . H27A H 1.3207 0.6824 0.3200 0.043 Uiso 1 1 calc R . . C28 C 1.1838(3) 0.7562(2) 0.34413(13) 0.0273(8) Uani 1 1 d . . . H28A H 1.1720 0.7211 0.3799 0.033 Uiso 1 1 calc R . . C29 C 1.1089(3) 0.8310(2) 0.32847(13) 0.0195(7) Uani 1 1 d . . . C30 C 1.0158(2) 0.8558(2) 0.36472(12) 0.0165(7) Uani 1 1 d . . . C31 C 1.0022(2) 0.8074(2) 0.42396(12) 0.0170(7) Uani 1 1 d . . . C32 C 1.0518(3) 0.8467(2) 0.47296(13) 0.0225(8) Uani 1 1 d . . . H32A H 1.0964 0.9029 0.4688 0.027 Uiso 1 1 calc R . . C33 C 1.0378(3) 0.8051(2) 0.52976(13) 0.0259(8) Uani 1 1 d . . . H33A H 1.0738 0.8327 0.5632 0.031 Uiso 1 1 calc R . . C34 C 0.9732(3) 0.7261(3) 0.53661(14) 0.0266(8) Uani 1 1 d . . . H34A H 0.9618 0.7006 0.5753 0.032 Uiso 1 1 calc R . . C35 C 0.9226(2) 0.6807(2) 0.48791(14) 0.0213(7) Uani 1 1 d . . . C36 C 0.8595(2) 0.5954(2) 0.49314(16) 0.0305(8) Uani 1 1 d . . . H36A H 0.8479 0.5687 0.5315 0.037 Uiso 1 1 calc R . . C37 C 0.8150(3) 0.5504(2) 0.44564(16) 0.0339(9) Uani 1 1 d . . . H37A H 0.7727 0.4931 0.4506 0.041 Uiso 1 1 calc R . . C38 C 0.8319(3) 0.5893(2) 0.38848(14) 0.0295(7) Uani 1 1 d . . . H38A H 0.8018 0.5570 0.3549 0.035 Uiso 1 1 calc R . . C39 C 0.8907(2) 0.6723(2) 0.38060(14) 0.0220(7) Uani 1 1 d . . . H39A H 0.8996 0.6981 0.3418 0.026 Uiso 1 1 calc R . . C40 C 0.9387(2) 0.7207(2) 0.43006(13) 0.0173(7) Uani 1 1 d . . . C42 C 0.8160(3) 0.9686(3) 0.58628(12) 0.0289(8) Uani 1 1 d . . . H42A H 0.8517 0.9137 0.6069 0.035 Uiso 1 1 calc R . . H42B H 0.8211 1.0302 0.6084 0.035 Uiso 1 1 calc R . . C43 C 0.7158(3) 0.9498(2) 0.55787(13) 0.0236(8) Uani 1 1 d . . . C44 C 0.7182(2) 0.8773(2) 0.51401(15) 0.0243(7) Uani 1 1 d . . . H44A H 0.6521 0.8735 0.4878 0.029 Uiso 1 1 calc R . . H44B H 0.7454 0.8133 0.5270 0.029 Uiso 1 1 calc R . . C45 C 1.0318(3) 0.7202(3) 0.15462(15) 0.0398(10) Uani 1 1 d . . . H45A H 1.0923 0.7050 0.1830 0.048 Uiso 1 1 calc R . . H45B H 1.0191 0.6626 0.1295 0.048 Uiso 1 1 calc R . . C41 C 0.6179(3) 1.0167(3) 0.56354(15) 0.0387(9) Uani 1 1 d . . . H41A H 0.5668 0.9921 0.5939 0.058 Uiso 1 1 calc R . . H41B H 0.5790 1.0207 0.5253 0.058 Uiso 1 1 calc R . . H41C H 0.6441 1.0810 0.5750 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 Pd 0.01565(10) 0.02092(10) 0.01434(10) -0.00138(10) 0.00105(10) -0.00289(11) P 0.0159(4) 0.0161(4) 0.0163(4) 0.0003(3) 0.0001(3) 0.0008(4) Cl1 0.0249(4) 0.0249(4) 0.0249(4) -0.0019(4) 0.0009(4) -0.0085(3) Cl2 0.0415(6) 0.0708(8) 0.0650(7) -0.0314(6) 0.0119(5) -0.0073(5) Cl3 0.0612(7) 0.0451(6) 0.0392(6) 0.0046(5) 0.0009(5) 0.0181(5) O1 0.0224(12) 0.0163(11) 0.0153(11) 0.0004(9) -0.0048(9) -0.0012(10) O2 0.0146(11) 0.0178(11) 0.0185(11) 0.0014(8) 0.0010(9) 0.0017(9) C1 0.0185(15) 0.0154(14) 0.0140(14) 0.0007(11) -0.0021(15) -0.0016(16) C2 0.0197(18) 0.0165(15) 0.0237(17) -0.0039(12) 0.0001(14) 0.0003(14) C3 0.0259(19) 0.0193(17) 0.0208(17) -0.0071(13) 0.0032(14) -0.0051(14) C4 0.0179(17) 0.0244(18) 0.0161(17) -0.0008(13) 0.0018(14) -0.0075(15) C5 0.0245(19) 0.034(2) 0.0137(16) -0.0080(14) 0.0024(14) -0.0082(17) C6 0.0194(16) 0.043(2) 0.0162(16) 0.0018(18) 0.0001(13) -0.0024(19) C7 0.0175(16) 0.034(2) 0.0180(17) 0.0054(14) 0.0007(14) 0.0059(15) C8 0.0170(16) 0.0264(19) 0.0147(16) -0.0045(13) 0.0010(13) 0.0003(15) C9 0.0157(15) 0.0212(16) 0.0125(14) -0.0003(14) 0.0027(12) -0.0032(15) C10 0.0163(14) 0.0172(16) 0.0135(15) -0.0027(13) 0.0015(12) -0.0063(14) C11 0.0173(15) 0.0170(17) 0.0131(15) 0.0022(12) -0.0030(12) 0.0017(14) C12 0.0203(17) 0.0177(16) 0.0107(15) 0.0071(12) 0.0005(13) -0.0001(14) C13 0.0233(16) 0.0226(16) 0.0127(14) -0.0015(14) -0.0008(12) -0.0006(16) C14 0.0228(18) 0.035(2) 0.0174(17) 0.0022(14) -0.0030(14) -0.0038(15) C15 0.0199(19) 0.037(2) 0.0232(19) 0.0058(16) 0.0056(15) 0.0064(16) C16 0.031(2) 0.0282(18) 0.0166(16) -0.0038(14) 0.0004(15) 0.0065(16) C17 0.0225(18) 0.0209(17) 0.0103(15) -0.0004(12) -0.0003(13) 0.0029(14) C18 0.0289(19) 0.0166(17) 0.0168(16) -0.0016(13) -0.0018(14) 0.0024(15) C19 0.0196(18) 0.0186(15) 0.0209(15) -0.0004(12) -0.0066(15) 0.0000(15) C20 0.0162(17) 0.0138(14) 0.0181(15) 0.0040(12) 0.0016(14) 0.0003(14) C21 0.0208(17) 0.0156(16) 0.0133(16) -0.0029(12) -0.0026(13) -0.0010(14) C22 0.0272(17) 0.0211(16) 0.0193(16) -0.0022(15) 0.0015(13) -0.0012(17) C23 0.033(2) 0.0236(19) 0.0210(17) 0.0077(14) 0.0083(15) 0.0035(16) C24 0.0184(18) 0.0255(17) 0.0195(17) -0.0004(14) 0.0013(13) -0.0026(14) C25 0.026(2) 0.037(2) 0.0260(19) 0.0068(16) 0.0078(16) -0.0008(18) C26 0.0237(18) 0.044(2) 0.0293(19) 0.0011(17) 0.0112(15) 0.0007(18) C27 0.028(2) 0.044(2) 0.036(2) 0.0114(18) 0.0098(17) 0.0150(18) C28 0.026(2) 0.0349(19) 0.0206(16) 0.0083(14) 0.0034(15) 0.0121(17) C29 0.0182(16) 0.0237(17) 0.0165(17) -0.0025(14) -0.0014(13) -0.0034(15) C30 0.0165(16) 0.0178(16) 0.0153(16) -0.0009(13) -0.0031(13) -0.0046(14) C31 0.0149(16) 0.0205(17) 0.0156(16) 0.0012(13) 0.0009(13) 0.0082(14) C32 0.0212(17) 0.0207(17) 0.026(2) 0.0003(13) -0.0024(14) 0.0081(14) C33 0.032(2) 0.032(2) 0.0140(17) -0.0049(14) -0.0047(14) 0.0123(17) C34 0.027(2) 0.034(2) 0.0187(17) 0.0084(15) 0.0046(15) 0.0119(18) C35 0.0180(16) 0.0250(16) 0.0208(16) 0.0053(16) 0.0024(15) 0.0081(13) C36 0.0258(19) 0.0306(17) 0.035(2) 0.0172(16) 0.0082(17) 0.0051(15) C37 0.024(2) 0.0266(19) 0.051(2) 0.0135(16) 0.0016(17) -0.0062(16) C38 0.0205(17) 0.0251(17) 0.043(2) -0.0029(15) -0.0069(18) 0.0003(17) C39 0.0187(17) 0.0244(18) 0.0228(18) -0.0004(14) -0.0018(14) 0.0023(15) C40 0.0131(16) 0.0196(16) 0.0193(17) 0.0045(13) 0.0017(13) 0.0056(14) C42 0.033(2) 0.042(2) 0.0119(14) 0.0037(15) 0.0036(13) -0.0096(19) C43 0.0228(17) 0.028(2) 0.0197(16) 0.0000(14) 0.0115(15) -0.0090(15) C44 0.0213(16) 0.0245(16) 0.0272(17) 0.0062(16) 0.0039(16) -0.0033(14) C45 0.041(2) 0.044(2) 0.034(2) -0.0051(18) 0.0001(18) 0.011(2) C41 0.0278(18) 0.043(2) 0.045(2) -0.003(2) 0.0145(15) -0.0007(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd P 2.2354(7) . ? Pd Cl1 2.3730(8) . ? Pd C42 2.198(3) . ? Pd C43 2.171(3) . ? Pd C44 2.078(3) . ? P O1 1.633(2) . ? P O2 1.622(2) . ? P C21 1.808(3) . ? Cl2 C45 1.768(4) . ? Cl3 C45 1.767(4) . ? O1 C1 1.401(3) . ? O2 C20 1.408(3) . ? C1 C2 1.399(4) . ? C1 C10 1.369(4) . ? C2 H2A 0.950 . ? C2 C3 1.365(4) . ? C3 H3A 0.950 . ? C3 C4 1.404(4) . ? C4 C5 1.416(4) . ? C4 C9 1.420(4) . ? C5 H5A 0.950 . ? C5 C6 1.368(5) . ? C6 H6A 0.950 . ? C6 C7 1.387(4) . ? C7 H7A 0.950 . ? C7 C8 1.369(4) . ? C8 H8A 0.950 . ? C8 C9 1.413(4) . ? C9 C10 1.438(4) . ? C10 C11 1.489(4) . ? C11 C12 1.432(4) . ? C11 C20 1.373(4) . ? C12 C13 1.416(4) . ? C12 C17 1.440(4) . ? C13 H13A 0.950 . ? C13 C14 1.363(4) . ? C14 H14A 0.950 . ? C14 C15 1.418(4) . ? C15 H15A 0.950 . ? C15 C16 1.354(4) . ? C16 H16A 0.950 . ? C16 C17 1.421(4) . ? C17 C18 1.406(4) . ? C18 H18A 0.950 . ? C18 C19 1.368(4) . ? C19 H19A 0.950 . ? C19 C20 1.392(4) . ? C21 C22 1.420(4) . ? C21 C30 1.387(4) . ? C22 H22A 0.950 . ? C22 C23 1.363(4) . ? C23 H23A 0.950 . ? C23 C24 1.408(4) . ? C24 C25 1.414(4) . ? C24 C29 1.416(4) . ? C25 H25A 0.950 . ? C25 C26 1.362(5) . ? C26 H26A 0.950 . ? C26 C27 1.407(5) . ? C27 H27A 0.950 . ? C27 C28 1.361(4) . ? C28 H28A 0.950 . ? C28 C29 1.417(4) . ? C29 C30 1.426(4) . ? C30 C31 1.502(4) . ? C31 C32 1.366(4) . ? C31 C40 1.429(4) . ? C32 H32A 0.950 . ? C32 C33 1.412(4) . ? C33 H33A 0.950 . ? C33 C34 1.351(5) . ? C34 H34A 0.950 . ? C34 C35 1.402(4) . ? C35 C36 1.409(4) . ? C35 C40 1.428(4) . ? C36 H36A 0.950 . ? C36 C37 1.348(4) . ? C37 H37A 0.950 . ? C37 C38 1.409(4) . ? C38 H38A 0.950 . ? C38 C39 1.362(4) . ? C39 H39A 0.950 . ? C39 C40 1.422(4) . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C42 C43 1.387(4) . ? C43 C44 1.409(4) . ? C43 C41 1.502(4) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? 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 P Pd Cl1 94.51(3) . . ? P Pd C42 163.75(8) . . ? P Pd C43 128.05(9) . . ? P Pd C44 96.49(9) . . ? Cl1 Pd C42 101.72(9) . . ? Cl1 Pd C43 132.18(8) . . ? Cl1 Pd C44 168.94(10) . . ? C42 Pd C43 37.02(11) . . ? C42 Pd C44 67.30(13) . . ? C43 Pd C44 38.64(12) . . ? Pd P O1 112.44(8) . . ? Pd P O2 112.83(8) . . ? Pd P C21 122.04(10) . . ? O1 P O2 101.34(10) . . ? O1 P C21 106.64(12) . . ? O2 P C21 98.93(12) . . ? P O1 C1 121.58(18) . . ? P O2 C20 112.41(16) . . ? O1 C1 C2 117.0(2) . . ? O1 C1 C10 119.8(2) . . ? C2 C1 C10 123.1(3) . . ? C1 C2 H2A 120.4 . . ? C1 C2 C3 119.3(3) . . ? H2A C2 C3 120.4 . . ? C2 C3 H3A 119.6 . . ? C2 C3 C4 120.8(3) . . ? H3A C3 C4 119.6 . . ? C3 C4 C5 121.6(3) . . ? C3 C4 C9 119.7(3) . . ? C5 C4 C9 118.8(3) . . ? C4 C5 H5A 119.5 . . ? C4 C5 C6 121.1(3) . . ? H5A C5 C6 119.5 . . ? C5 C6 H6A 120.1 . . ? C5 C6 C7 119.7(3) . . ? H6A C6 C7 120.1 . . ? C6 C7 H7A 119.4 . . ? C6 C7 C8 121.2(3) . . ? H7A C7 C8 119.4 . . ? C7 C8 H8A 119.7 . . ? C7 C8 C9 120.6(3) . . ? H8A C8 C9 119.7 . . ? C4 C9 C8 118.4(2) . . ? C4 C9 C10 119.1(3) . . ? C8 C9 C10 122.5(3) . . ? C1 C10 C9 117.8(3) . . ? C1 C10 C11 120.6(2) . . ? C9 C10 C11 121.6(3) . . ? C10 C11 C12 123.1(3) . . ? C10 C11 C20 119.1(2) . . ? C12 C11 C20 117.8(3) . . ? C11 C12 C13 124.1(3) . . ? C11 C12 C17 118.4(3) . . ? C13 C12 C17 117.6(3) . . ? C12 C13 H13A 119.1 . . ? C12 C13 C14 121.7(3) . . ? H13A C13 C14 119.1 . . ? C13 C14 H14A 119.7 . . ? C13 C14 C15 120.5(3) . . ? H14A C14 C15 119.7 . . ? C14 C15 H15A 120.1 . . ? C14 C15 C16 119.8(3) . . ? H15A C15 C16 120.1 . . ? C15 C16 H16A 119.3 . . ? C15 C16 C17 121.5(3) . . ? H16A C16 C17 119.3 . . ? C12 C17 C16 118.9(3) . . ? C12 C17 C18 119.8(3) . . ? C16 C17 C18 121.3(3) . . ? C17 C18 H18A 119.4 . . ? C17 C18 C19 121.1(3) . . ? H18A C18 C19 119.4 . . ? C18 C19 H19A 120.8 . . ? C18 C19 C20 118.4(3) . . ? H19A C19 C20 120.8 . . ? O2 C20 C11 117.6(2) . . ? O2 C20 C19 118.0(3) . . ? C11 C20 C19 124.4(3) . . ? P C21 C22 120.7(2) . . ? P C21 C30 119.0(2) . . ? C22 C21 C30 120.2(3) . . ? C21 C22 H22A 119.9 . . ? C21 C22 C23 120.1(3) . . ? H22A C22 C23 119.9 . . ? C22 C23 H23A 119.3 . . ? C22 C23 C24 121.5(3) . . ? H23A C23 C24 119.3 . . ? C23 C24 C25 122.0(3) . . ? C23 C24 C29 118.9(3) . . ? C25 C24 C29 119.1(3) . . ? C24 C25 H25A 119.5 . . ? C24 C25 C26 121.0(3) . . ? H25A C25 C26 119.5 . . ? C25 C26 H26A 120.0 . . ? C25 C26 C27 120.0(3) . . ? H26A C26 C27 120.0 . . ? C26 C27 H27A 119.8 . . ? C26 C27 C28 120.3(3) . . ? H27A C27 C28 119.8 . . ? C27 C28 H28A 119.4 . . ? C27 C28 C29 121.2(3) . . ? H28A C28 C29 119.4 . . ? C24 C29 C28 118.2(3) . . ? C24 C29 C30 119.6(3) . . ? C28 C29 C30 122.1(3) . . ? C21 C30 C29 119.5(3) . . ? C21 C30 C31 121.4(3) . . ? C29 C30 C31 119.0(3) . . ? C30 C31 C32 119.4(3) . . ? C30 C31 C40 121.2(3) . . ? C32 C31 C40 119.4(3) . . ? C31 C32 H32A 119.5 . . ? C31 C32 C33 121.0(3) . . ? H32A C32 C33 119.5 . . ? C32 C33 H33A 119.9 . . ? C32 C33 C34 120.2(3) . . ? H33A C33 C34 119.9 . . ? C33 C34 H34A 119.2 . . ? C33 C34 C35 121.5(3) . . ? H34A C34 C35 119.2 . . ? C34 C35 C36 122.9(3) . . ? C34 C35 C40 118.7(3) . . ? C36 C35 C40 118.3(3) . . ? C35 C36 H36A 118.8 . . ? C35 C36 C37 122.3(3) . . ? H36A C36 C37 118.8 . . ? C36 C37 H37A 120.3 . . ? C36 C37 C38 119.3(3) . . ? H37A C37 C38 120.3 . . ? C37 C38 H38A 119.5 . . ? C37 C38 C39 121.1(3) . . ? H38A C38 C39 119.5 . . ? C38 C39 H39A 119.8 . . ? C38 C39 C40 120.5(3) . . ? H39A C39 C40 119.8 . . ? C31 C40 C35 119.1(3) . . ? C31 C40 C39 122.5(3) . . ? C35 C40 C39 118.4(3) . . ? Pd C42 H42A 116.6 . . ? Pd C42 H42B 116.6 . . ? Pd C42 C43 70.42(16) . . ? H42A C42 H42B 113.6 . . ? H42A C42 C43 116.6 . . ? H42B C42 C43 116.6 . . ? Pd C43 C42 72.56(16) . . ? Pd C43 C44 67.13(16) . . ? Pd C43 C41 119.4(2) . . ? C42 C43 C44 116.1(3) . . ? C42 C43 C41 121.6(3) . . ? C44 C43 C41 121.0(3) . . ? Pd C44 C43 74.23(17) . . ? Pd C44 H44A 116.1 . . ? Pd C44 H44B 116.1 . . ? C43 C44 H44A 116.1 . . ? C43 C44 H44B 116.1 . . ? H44A C44 H44B 113.1 . . ? Cl2 C45 Cl3 111.1(2) . . ? Cl2 C45 H45A 109.4 . . ? Cl2 C45 H45B 109.4 . . ? Cl3 C45 H45A 109.4 . . ? Cl3 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C43 C41 H41A 109.5 . . ? C43 C41 H41B 109.5 . . ? C43 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd P O1 -177.86(8) . . . . ? Cl1 Pd P O2 -63.99(8) . . . . ? Cl1 Pd P C21 53.53(12) . . . . ? C42 Pd P O1 -1.0(3) . . . . ? C42 Pd P O2 112.9(3) . . . . ? C42 Pd P C21 -129.6(4) . . . . ? C43 Pd P O1 -21.35(14) . . . . ? C43 Pd P O2 92.52(13) . . . . ? C43 Pd P C21 -149.96(16) . . . . ? C44 Pd P O1 3.25(12) . . . . ? C44 Pd P O2 117.12(11) . . . . ? C44 Pd P C21 -125.36(14) . . . . ? Pd P O1 C1 152.25(18) . . . . ? O2 P O1 C1 31.5(2) . . . . ? C21 P O1 C1 -71.5(2) . . . . ? Pd P O2 C20 -60.18(18) . . . . ? O1 P O2 C20 60.27(19) . . . . ? C21 P O2 C20 169.37(19) . . . . ? P O1 C1 C2 115.0(3) . . . . ? P O1 C1 C10 -67.7(3) . . . . ? O1 C1 C2 C3 177.3(3) . . . . ? C10 C1 C2 C3 0.2(5) . . . . ? C1 C2 C3 C4 3.0(5) . . . . ? C2 C3 C4 C5 177.7(3) . . . . ? C2 C3 C4 C9 -1.4(4) . . . . ? C3 C4 C5 C6 -175.9(3) . . . . ? C9 C4 C5 C6 3.2(4) . . . . ? C4 C5 C6 C7 0.5(5) . . . . ? C5 C6 C7 C8 -2.2(5) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C7 C8 C9 C4 3.8(4) . . . . ? C7 C8 C9 C10 -179.2(3) . . . . ? C3 C4 C9 C8 173.9(3) . . . . ? C3 C4 C9 C10 -3.3(4) . . . . ? C5 C4 C9 C8 -5.3(4) . . . . ? C5 C4 C9 C10 177.6(3) . . . . ? O1 C1 C10 C9 178.2(2) . . . . ? O1 C1 C10 C11 0.2(4) . . . . ? C2 C1 C10 C9 -4.8(4) . . . . ? C2 C1 C10 C11 177.2(3) . . . . ? C4 C9 C10 C1 6.2(4) . . . . ? C4 C9 C10 C11 -175.8(3) . . . . ? C8 C9 C10 C1 -170.8(3) . . . . ? C8 C9 C10 C11 7.2(4) . . . . ? C1 C10 C11 C12 -125.2(3) . . . . ? C1 C10 C11 C20 52.1(4) . . . . ? C9 C10 C11 C12 56.9(4) . . . . ? C9 C10 C11 C20 -125.8(3) . . . . ? C10 C11 C12 C13 1.4(4) . . . . ? C10 C11 C12 C17 -180.0(3) . . . . ? C20 C11 C12 C13 -176.0(3) . . . . ? C20 C11 C12 C17 2.7(4) . . . . ? C11 C12 C13 C14 -179.4(3) . . . . ? C17 C12 C13 C14 2.0(4) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C14 C15 C16 C17 0.8(5) . . . . ? C15 C16 C17 C12 0.5(4) . . . . ? C15 C16 C17 C18 -178.9(3) . . . . ? C11 C12 C17 C16 179.4(3) . . . . ? C11 C12 C17 C18 -1.2(4) . . . . ? C13 C12 C17 C16 -1.8(4) . . . . ? C13 C12 C17 C18 177.6(3) . . . . ? C12 C17 C18 C19 -0.5(4) . . . . ? C16 C17 C18 C19 178.9(3) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C10 C11 C20 O2 -0.1(4) . . . . ? C10 C11 C20 C19 179.8(3) . . . . ? C12 C11 C20 O2 177.3(2) . . . . ? C12 C11 C20 C19 -2.8(4) . . . . ? C18 C19 C20 O2 -179.0(2) . . . . ? C18 C19 C20 C11 1.1(4) . . . . ? P O2 C20 C11 -82.2(3) . . . . ? P O2 C20 C19 97.9(2) . . . . ? Pd P C21 C22 -134.5(2) . . . . ? Pd P C21 C30 43.3(3) . . . . ? O1 P C21 C22 94.5(2) . . . . ? O1 P C21 C30 -87.7(2) . . . . ? O2 P C21 C22 -10.3(3) . . . . ? O2 P C21 C30 167.5(2) . . . . ? P C21 C22 C23 176.7(2) . . . . ? C30 C21 C22 C23 -1.1(4) . . . . ? C21 C22 C23 C24 2.9(5) . . . . ? C22 C23 C24 C25 178.4(3) . . . . ? C22 C23 C24 C29 -1.2(5) . . . . ? C23 C24 C25 C26 -176.8(3) . . . . ? C29 C24 C25 C26 2.7(5) . . . . ? C24 C25 C26 C27 -1.2(5) . . . . ? C25 C26 C27 C28 -0.7(5) . . . . ? C26 C27 C28 C29 1.0(5) . . . . ? C23 C24 C29 C28 177.2(3) . . . . ? C23 C24 C29 C30 -2.3(4) . . . . ? C25 C24 C29 C28 -2.4(4) . . . . ? C25 C24 C29 C30 178.2(3) . . . . ? C27 C28 C29 C24 0.5(5) . . . . ? C27 C28 C29 C30 -180.0(3) . . . . ? P C21 C30 C29 179.8(2) . . . . ? P C21 C30 C31 -1.3(4) . . . . ? C22 C21 C30 C29 -2.3(4) . . . . ? C22 C21 C30 C31 176.5(3) . . . . ? C24 C29 C30 C21 4.0(4) . . . . ? C24 C29 C30 C31 -174.9(3) . . . . ? C28 C29 C30 C21 -175.5(3) . . . . ? C28 C29 C30 C31 5.6(4) . . . . ? C21 C30 C31 C32 -90.5(4) . . . . ? C21 C30 C31 C40 89.6(4) . . . . ? C29 C30 C31 C32 88.3(3) . . . . ? C29 C30 C31 C40 -91.5(3) . . . . ? C30 C31 C32 C33 177.8(3) . . . . ? C40 C31 C32 C33 -2.4(4) . . . . ? C31 C32 C33 C34 -1.1(5) . . . . ? C32 C33 C34 C35 2.9(5) . . . . ? C33 C34 C35 C36 176.7(3) . . . . ? C33 C34 C35 C40 -1.2(4) . . . . ? C34 C35 C36 C37 -177.3(3) . . . . ? C40 C35 C36 C37 0.5(4) . . . . ? C35 C36 C37 C38 0.2(5) . . . . ? C36 C37 C38 C39 -1.2(5) . . . . ? C37 C38 C39 C40 1.5(5) . . . . ? C38 C39 C40 C31 179.2(3) . . . . ? C38 C39 C40 C35 -0.7(4) . . . . ? C34 C35 C40 C31 -2.3(4) . . . . ? C34 C35 C40 C39 177.7(3) . . . . ? C36 C35 C40 C31 179.8(3) . . . . ? C36 C35 C40 C39 -0.3(4) . . . . ? C30 C31 C40 C35 -176.2(3) . . . . ? C30 C31 C40 C39 3.9(4) . . . . ? C32 C31 C40 C35 4.0(4) . . . . ? C32 C31 C40 C39 -175.9(3) . . . . ? P Pd C42 C43 -27.1(5) . . . . ? Cl1 Pd C42 C43 149.75(18) . . . . ? C44 Pd C42 C43 -31.63(19) . . . . ? Pd C42 C43 C44 52.6(2) . . . . ? Pd C42 C43 C41 -114.2(3) . . . . ? P Pd C43 C42 170.69(17) . . . . ? P Pd C43 C44 41.5(2) . . . . ? P Pd C43 C41 -72.4(3) . . . . ? Cl1 Pd C43 C42 -41.7(2) . . . . ? Cl1 Pd C43 C44 -170.94(15) . . . . ? Cl1 Pd C43 C41 75.2(3) . . . . ? C42 Pd C43 C44 -129.2(3) . . . . ? C42 Pd C43 C41 116.9(3) . . . . ? C44 Pd C43 C42 129.2(3) . . . . ? C44 Pd C43 C41 -113.9(3) . . . . ? C42 C43 C44 Pd -55.4(2) . . . . ? C41 C43 C44 Pd 111.6(3) . . . . ? P Pd C44 C43 -148.34(17) . . . . ? Cl1 Pd C44 C43 37.4(5) . . . . ? C42 Pd C44 C43 30.38(19) . . . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.634 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.073 data_ljh68_compound_8b _database_code_depnum_ccdc_archive 'CCDC 840100' #TrackingRef 'RWHLJHchemcomm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H34 Cl O3 P Pd, C4 H10 O' _chemical_formula_sum 'C49 H44 Cl O4 P Pd' _chemical_formula_weight 869.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 12.1370(2) _cell_length_b 14.4938(3) _cell_length_c 23.2109(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4083.06(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20704 _cell_measurement_theta_min 2.9785 _cell_measurement_theta_max 28.5563 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8395 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details ; 'Tue Dec 07 04:17:38 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 48358 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 28.62 _reflns_number_total 9182 _reflns_number_gt 6798 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.028(16) _chemical_absolute_configuration ad _refine_ls_number_reflns 9182 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.654915(17) 0.350337(14) 0.934711(9) 0.02329(6) Uani 1 1 d . . . Cl Cl 0.72503(6) 0.19821(4) 0.94065(3) 0.03079(16) Uani 1 1 d . . . P P 0.72389(6) 0.38849(5) 0.84774(3) 0.02139(16) Uani 1 1 d . . . O1 O 0.85554(15) 0.36975(11) 0.84379(7) 0.0227(4) Uani 1 1 d . . . O2 O 0.71813(15) 0.49998(12) 0.84012(8) 0.0231(4) Uani 1 1 d . . . O3 O 0.56054(16) 0.13360(13) 0.81198(8) 0.0311(5) Uani 1 1 d . . . O4 O 0.4271(3) 0.6490(3) 1.15255(17) 0.1160(13) Uani 1 1 d . . . C1 C 0.9184(2) 0.41977(19) 0.88333(12) 0.0230(6) Uani 1 1 d . . . C2 C 0.9573(2) 0.37331(17) 0.93227(13) 0.0265(6) Uani 1 1 d . . . H2A H 0.9387 0.3105 0.9388 0.032 Uiso 1 1 calc R . . C3 C 1.0219(2) 0.4197(2) 0.96998(13) 0.0297(7) Uani 1 1 d . . . H3A H 1.0513 0.3880 1.0023 0.036 Uiso 1 1 calc R . . C4 C 1.0466(2) 0.5138(2) 0.96238(12) 0.0256(7) Uani 1 1 d . . . C5 C 1.1127(2) 0.5643(2) 1.00161(13) 0.0350(8) Uani 1 1 d . . . H5A H 1.1437 0.5332 1.0337 0.042 Uiso 1 1 calc R . . C6 C 1.1330(2) 0.6549(3) 0.99487(12) 0.0404(8) Uani 1 1 d . . . H6A H 1.1791 0.6865 1.0214 0.049 Uiso 1 1 calc R . . C7 C 1.0857(2) 0.7021(2) 0.94856(13) 0.0357(8) Uani 1 1 d . . . H7A H 1.0976 0.7666 0.9448 0.043 Uiso 1 1 calc R . . C8 C 1.0227(2) 0.6574(2) 0.90845(11) 0.0269(6) Uani 1 1 d . . . H8A H 0.9920 0.6909 0.8771 0.032 Uiso 1 1 calc R . . C9 C 1.0030(2) 0.56135(19) 0.91339(11) 0.0216(6) Uani 1 1 d . . . C10 C 0.9413(2) 0.51071(18) 0.87173(11) 0.0190(6) Uani 1 1 d . . . C11 C 0.9015(2) 0.55049(19) 0.81658(12) 0.0207(6) Uani 1 1 d . . . C12 C 0.9743(2) 0.58856(17) 0.77460(12) 0.0219(6) Uani 1 1 d . . . C13 C 1.0901(2) 0.58993(19) 0.78248(13) 0.0244(7) Uani 1 1 d . . . H13A H 1.1208 0.5671 0.8173 0.029 Uiso 1 1 calc R . . C14 C 1.1583(3) 0.62378(16) 0.74054(12) 0.0279(6) Uani 1 1 d . . . H14A H 1.2356 0.6242 0.7467 0.033 Uiso 1 1 calc R . . C15 C 1.1159(2) 0.6577(2) 0.68880(12) 0.0324(7) Uani 1 1 d . . . H15A H 1.1644 0.6806 0.6600 0.039 Uiso 1 1 calc R . . C16 C 1.0060(3) 0.6581(2) 0.67970(12) 0.0352(7) Uani 1 1 d . . . H16A H 0.9777 0.6827 0.6448 0.042 Uiso 1 1 calc R . . C17 C 0.9317(2) 0.62205(18) 0.72164(12) 0.0253(7) Uani 1 1 d . . . C18 C 0.8167(3) 0.6178(2) 0.71142(13) 0.0335(8) Uani 1 1 d . . . H18A H 0.7873 0.6427 0.6768 0.040 Uiso 1 1 calc R . . C19 C 0.7486(2) 0.57870(19) 0.75036(13) 0.0273(7) Uani 1 1 d . . . H19A H 0.6718 0.5747 0.7428 0.033 Uiso 1 1 calc R . . C20 C 0.7920(2) 0.54403(18) 0.80208(12) 0.0216(6) Uani 1 1 d . . . C21 C 0.6880(2) 0.34355(19) 0.77763(11) 0.0231(6) Uani 1 1 d . . . C22 C 0.7655(2) 0.3533(2) 0.73213(11) 0.0274(6) Uani 1 1 d . . . H22A H 0.8356 0.3798 0.7398 0.033 Uiso 1 1 calc R . . C23 C 0.7405(2) 0.32539(18) 0.67775(12) 0.0300(7) Uani 1 1 d . . . H23A H 0.7938 0.3321 0.6481 0.036 Uiso 1 1 calc R . . C24 C 0.6372(3) 0.28673(18) 0.66475(11) 0.0259(7) Uani 1 1 d . . . C25 C 0.6093(3) 0.2565(2) 0.60834(13) 0.0340(8) Uani 1 1 d . . . H25A H 0.6616 0.2622 0.5781 0.041 Uiso 1 1 calc R . . C26 C 0.5094(3) 0.2198(2) 0.59723(14) 0.0397(8) Uani 1 1 d . . . H26A H 0.4926 0.1992 0.5594 0.048 Uiso 1 1 calc R . . C27 C 0.4296(3) 0.2116(2) 0.64104(13) 0.0380(8) Uani 1 1 d . . . H27A H 0.3591 0.1864 0.6327 0.046 Uiso 1 1 calc R . . C28 C 0.4544(3) 0.2400(2) 0.69539(13) 0.0306(7) Uani 1 1 d . . . H28A H 0.4001 0.2348 0.7247 0.037 Uiso 1 1 calc R . . C29 C 0.5581(2) 0.27698(18) 0.70949(12) 0.0234(6) Uani 1 1 d . . . C30 C 0.5856(2) 0.30470(18) 0.76679(12) 0.0215(6) Uani 1 1 d . . . C31 C 0.5054(2) 0.28758(18) 0.81474(11) 0.0211(6) Uani 1 1 d . . . C32 C 0.43867(19) 0.3590(2) 0.83645(11) 0.0208(6) Uani 1 1 d . . . C33 C 0.4399(2) 0.44953(19) 0.81391(12) 0.0244(6) Uani 1 1 d . . . H33A H 0.4865 0.4632 0.7821 0.029 Uiso 1 1 calc R . . C34 C 0.3757(2) 0.5180(2) 0.83668(13) 0.0289(7) Uani 1 1 d . . . H34A H 0.3785 0.5782 0.8207 0.035 Uiso 1 1 calc R . . C35 C 0.3056(2) 0.4999(2) 0.88362(13) 0.0337(7) Uani 1 1 d . . . H35A H 0.2612 0.5477 0.8993 0.040 Uiso 1 1 calc R . . C36 C 0.3019(2) 0.4130(2) 0.90656(13) 0.0310(7) Uani 1 1 d . . . H36A H 0.2548 0.4009 0.9384 0.037 Uiso 1 1 calc R . . C37 C 0.36646(19) 0.3412(2) 0.88392(11) 0.0235(6) Uani 1 1 d . . . C38 C 0.3650(2) 0.2512(2) 0.90804(12) 0.0278(7) Uani 1 1 d . . . H38A H 0.3196 0.2387 0.9405 0.033 Uiso 1 1 calc R . . C39 C 0.4283(2) 0.1822(2) 0.88504(12) 0.0275(7) Uani 1 1 d . . . H39A H 0.4255 0.1220 0.9011 0.033 Uiso 1 1 calc R . . C40 C 0.4976(2) 0.20005(18) 0.83766(11) 0.0209(6) Uani 1 1 d . . . C41 C 0.5697(3) 0.0461(2) 0.83892(14) 0.0394(8) Uani 1 1 d . . . H41A H 0.6190 0.0067 0.8163 0.059 Uiso 1 1 calc R . . H41B H 0.4968 0.0174 0.8412 0.059 Uiso 1 1 calc R . . H41C H 0.5997 0.0538 0.8778 0.059 Uiso 1 1 calc R . . C42 C 0.5776(2) 0.3541(2) 1.01933(12) 0.0380(7) Uani 1 1 d . . . H42A H 0.4963 0.3486 1.0203 0.046 Uiso 1 1 calc R . . H42B H 0.6151 0.3196 1.0505 0.046 Uiso 1 1 calc R . . C43 C 0.5836(2) 0.47908(19) 0.95324(12) 0.0295(7) Uani 1 1 d . . . H43A H 0.6238 0.5340 0.9391 0.035 Uiso 1 1 calc R . . H43B H 0.5028 0.4836 0.9482 0.035 Uiso 1 1 calc R . . C44 C 0.6205(2) 0.4414(2) 1.00594(13) 0.0313(7) Uani 1 1 d . . . C45 C 0.7152(3) 0.4826(2) 1.03858(15) 0.0479(9) Uani 1 1 d . . . H45A H 0.6870 0.5247 1.0681 0.072 Uiso 1 1 calc R . . H45B H 0.7627 0.5168 1.0119 0.072 Uiso 1 1 calc R . . H45C H 0.7578 0.4333 1.0570 0.072 Uiso 1 1 calc R . . C46 C 0.3687(7) 0.5828(4) 1.1232(3) 0.150(3) Uani 1 1 d . . . H46A H 0.2893 0.5982 1.1249 0.180 Uiso 1 1 calc R . . H46B H 0.3791 0.5226 1.1426 0.180 Uiso 1 1 calc R . . C47 C 0.3999(4) 0.5745(4) 1.0662(3) 0.127(3) Uani 1 1 d . . . H47A H 0.3694 0.5175 1.0501 0.191 Uiso 1 1 calc R . . H47B H 0.4805 0.5728 1.0637 0.191 Uiso 1 1 calc R . . H47C H 0.3721 0.6275 1.0444 0.191 Uiso 1 1 calc R . . C48 C 0.4297(4) 0.6464(4) 1.2116(2) 0.0933(15) Uani 1 1 d . . . H48A H 0.4739 0.7000 1.2244 0.112 Uiso 1 1 calc R . . H48B H 0.4716 0.5904 1.2226 0.112 Uiso 1 1 calc R . . C49 C 0.3323(4) 0.6465(3) 1.2444(3) 0.141(3) Uani 1 1 d . . . H49A H 0.3505 0.6559 1.2851 0.212 Uiso 1 1 calc R . . H49B H 0.2945 0.5872 1.2398 0.212 Uiso 1 1 calc R . . H49C H 0.2841 0.6964 1.2312 0.212 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02332(9) 0.03012(10) 0.01643(10) 0.00070(11) 0.00254(11) -0.00277(10) Cl 0.0375(4) 0.0294(3) 0.0254(4) 0.0025(3) 0.0093(4) -0.0027(3) P 0.0191(4) 0.0244(4) 0.0207(4) 0.0016(3) 0.0025(3) -0.0015(3) O1 0.0195(9) 0.0237(10) 0.0248(10) 0.0016(8) 0.0017(9) -0.0015(8) O2 0.0173(10) 0.0283(10) 0.0238(11) 0.0031(9) 0.0028(9) -0.0014(8) O3 0.0391(11) 0.0257(12) 0.0287(11) 0.0034(10) 0.0076(10) 0.0012(9) O4 0.169(4) 0.089(2) 0.090(3) 0.013(3) -0.033(3) -0.044(3) C1 0.0176(14) 0.0302(16) 0.0213(16) 0.0026(13) 0.0028(12) 0.0047(12) C2 0.0182(12) 0.0330(16) 0.0282(15) 0.0145(15) 0.0028(15) 0.0062(11) C3 0.0240(15) 0.0422(19) 0.0228(16) 0.0148(15) 0.0012(14) 0.0084(14) C4 0.0188(14) 0.0439(18) 0.0142(15) 0.0041(14) 0.0002(12) 0.0053(13) C5 0.0308(16) 0.056(2) 0.0183(17) 0.0035(16) -0.0019(13) 0.0016(15) C6 0.043(2) 0.057(2) 0.0209(15) -0.0104(18) -0.0026(14) -0.004(2) C7 0.0364(17) 0.0396(17) 0.031(2) -0.0083(15) 0.0031(15) -0.0023(14) C8 0.0269(14) 0.0327(16) 0.0211(14) -0.0022(15) 0.0041(12) 0.0014(14) C9 0.0172(13) 0.0317(16) 0.0160(14) 0.0038(13) 0.0038(11) 0.0019(12) C10 0.0181(14) 0.0237(14) 0.0152(15) 0.0046(12) 0.0068(12) 0.0036(11) C11 0.0234(15) 0.0233(14) 0.0154(15) 0.0038(13) 0.0006(12) 0.0014(12) C12 0.0276(15) 0.0189(13) 0.0193(15) -0.0011(12) 0.0018(13) -0.0013(12) C13 0.0297(16) 0.0266(15) 0.0169(16) 0.0000(13) 0.0041(13) -0.0048(13) C14 0.0276(14) 0.0271(14) 0.0289(16) -0.0019(12) 0.0065(15) -0.0036(14) C15 0.0445(18) 0.0294(15) 0.0234(16) 0.0043(15) 0.0115(14) -0.0105(15) C16 0.053(2) 0.0369(17) 0.0156(14) 0.0035(15) 0.0007(14) -0.0094(17) C17 0.0339(16) 0.0263(16) 0.0155(15) 0.0052(12) -0.0020(13) -0.0050(13) C18 0.044(2) 0.0344(17) 0.0221(16) 0.0057(13) -0.0089(14) 0.0051(14) C19 0.0235(15) 0.0305(16) 0.0278(17) 0.0026(14) -0.0082(13) 0.0019(13) C20 0.0235(15) 0.0205(14) 0.0207(16) 0.0014(12) 0.0053(13) 0.0010(12) C21 0.0274(14) 0.0229(13) 0.0190(13) 0.0035(13) 0.0050(11) -0.0027(13) C22 0.0287(14) 0.0269(14) 0.0267(16) 0.0048(15) 0.0045(12) -0.0008(14) C23 0.0434(18) 0.0284(17) 0.0183(16) 0.0027(12) 0.0143(14) 0.0023(13) C24 0.0377(18) 0.0232(14) 0.0167(15) 0.0038(12) 0.0070(15) 0.0061(13) C25 0.051(2) 0.0335(17) 0.0178(17) 0.0038(13) 0.0063(15) 0.0025(15) C26 0.057(2) 0.0419(19) 0.0196(17) -0.0006(15) -0.0065(17) 0.0048(16) C27 0.042(2) 0.046(2) 0.0266(18) -0.0040(15) -0.0078(16) -0.0046(16) C28 0.0338(16) 0.0340(16) 0.0239(17) 0.0002(14) 0.0016(14) -0.0011(14) C29 0.0301(16) 0.0222(14) 0.0180(15) 0.0016(12) -0.0022(13) 0.0041(12) C30 0.0259(15) 0.0202(13) 0.0183(15) 0.0033(12) 0.0027(12) 0.0066(12) C31 0.0202(14) 0.0274(15) 0.0158(14) -0.0018(12) -0.0016(12) -0.0016(12) C32 0.0144(12) 0.0315(15) 0.0165(14) -0.0036(14) -0.0033(11) -0.0027(13) C33 0.0214(15) 0.0318(16) 0.0200(15) 0.0027(13) -0.0032(13) 0.0007(13) C34 0.0264(17) 0.0307(16) 0.0296(18) 0.0005(14) -0.0074(14) 0.0035(13) C35 0.0242(16) 0.0411(19) 0.0356(19) -0.0093(16) -0.0042(14) 0.0077(13) C36 0.0201(14) 0.0477(19) 0.0252(17) -0.0064(15) 0.0039(13) 0.0000(13) C37 0.0147(13) 0.0388(16) 0.0170(13) -0.0030(14) -0.0024(11) -0.0033(13) C38 0.0225(16) 0.0413(17) 0.0195(14) 0.0012(13) 0.0037(13) -0.0053(14) C39 0.0278(16) 0.0330(16) 0.0216(16) 0.0033(13) -0.0001(13) -0.0089(13) C40 0.0217(14) 0.0250(15) 0.0161(15) 0.0009(12) 0.0005(12) -0.0015(12) C41 0.059(2) 0.0247(16) 0.0349(19) 0.0086(15) 0.0017(17) 0.0043(15) C42 0.0351(17) 0.0530(19) 0.0258(17) 0.0028(17) 0.0125(13) 0.0075(19) C43 0.0259(15) 0.0350(16) 0.0277(18) -0.0043(13) 0.0019(13) 0.0079(13) C44 0.0289(17) 0.0415(18) 0.0234(17) -0.0096(15) -0.0005(13) 0.0135(14) C45 0.052(2) 0.053(2) 0.038(2) -0.0110(17) -0.0168(18) 0.0144(18) C46 0.218(9) 0.088(4) 0.145(7) -0.004(4) -0.046(7) -0.069(5) C47 0.061(3) 0.149(6) 0.171(6) -0.094(6) -0.003(4) 0.003(3) C48 0.062(3) 0.092(3) 0.126(5) 0.018(4) -0.014(3) -0.010(3) C49 0.082(4) 0.055(3) 0.287(9) -0.041(4) 0.063(5) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl 2.3675(7) . ? Pd P 2.2542(7) . ? Pd C42 2.177(3) . ? Pd C43 2.101(3) . ? Pd C44 2.156(3) . ? P O1 1.6234(19) . ? P O2 1.6270(19) . ? P C21 1.806(3) . ? O1 C1 1.397(3) . ? O2 C20 1.411(3) . ? O3 C40 1.366(3) . ? O3 C41 1.418(3) . ? O4 C46 1.373(6) . ? O4 C48 1.371(6) . ? C1 C2 1.402(4) . ? C1 C10 1.374(4) . ? C2 H2A 0.950 . ? C2 C3 1.354(4) . ? C3 H3A 0.950 . ? C3 C4 1.408(4) . ? C4 C5 1.417(4) . ? C4 C9 1.431(4) . ? C5 H5A 0.950 . ? C5 C6 1.344(5) . ? C6 H6A 0.950 . ? C6 C7 1.397(4) . ? C7 H7A 0.950 . ? C7 C8 1.368(4) . ? C8 H8A 0.950 . ? C8 C9 1.417(4) . ? C9 C10 1.426(4) . ? C10 C11 1.485(4) . ? C11 C12 1.426(4) . ? C11 C20 1.375(4) . ? C12 C13 1.417(4) . ? C12 C17 1.419(4) . ? C13 H13A 0.950 . ? C13 C14 1.369(4) . ? C14 H14A 0.950 . ? C14 C15 1.396(4) . ? C15 H15A 0.950 . ? C15 C16 1.351(4) . ? C16 H16A 0.950 . ? C16 C17 1.426(4) . ? C17 C18 1.416(4) . ? C18 H18A 0.950 . ? C18 C19 1.350(4) . ? C19 H19A 0.950 . ? C19 C20 1.404(4) . ? C21 C22 1.421(3) . ? C21 C30 1.388(4) . ? C22 H22A 0.950 . ? C22 C23 1.360(4) . ? C23 H23A 0.950 . ? C23 C24 1.407(4) . ? C24 C25 1.421(4) . ? C24 C29 1.421(4) . ? C25 H25A 0.950 . ? C25 C26 1.349(4) . ? C26 H26A 0.950 . ? C26 C27 1.409(5) . ? C27 H27A 0.950 . ? C27 C28 1.361(4) . ? C28 H28A 0.950 . ? C28 C29 1.406(4) . ? C29 C30 1.429(4) . ? C30 C31 1.499(4) . ? C31 C32 1.408(4) . ? C31 C40 1.379(4) . ? C32 C33 1.412(4) . ? C32 C37 1.431(3) . ? C33 H33A 0.950 . ? C33 C34 1.367(4) . ? C34 H34A 0.950 . ? C34 C35 1.407(4) . ? C35 H35A 0.950 . ? C35 C36 1.369(4) . ? C36 H36A 0.950 . ? C36 C37 1.405(4) . ? C37 C38 1.419(4) . ? C38 H38A 0.950 . ? C38 C39 1.370(4) . ? C39 H39A 0.950 . ? C39 C40 1.408(4) . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C42 C44 1.402(5) . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C43 C44 1.412(4) . ? C44 C45 1.501(4) . ? C45 H45A 0.980 . ? C45 H45B 0.980 . ? C45 H45C 0.980 . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C46 C47 1.382(9) . ? C47 H47A 0.980 . ? C47 H47B 0.980 . ? C47 H47C 0.980 . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? C48 C49 1.407(6) . ? C49 H49A 0.980 . ? C49 H49B 0.980 . ? C49 H49C 0.980 . ? 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 Cl Pd P 98.46(3) . . ? Cl Pd C42 97.23(9) . . ? Cl Pd C43 164.39(8) . . ? Cl Pd C44 126.52(9) . . ? P Pd C42 164.07(10) . . ? P Pd C43 96.80(8) . . ? P Pd C44 127.47(9) . . ? C42 Pd C43 67.39(12) . . ? C42 Pd C44 37.76(12) . . ? C43 Pd C44 38.72(11) . . ? Pd P O1 112.03(7) . . ? Pd P O2 108.97(7) . . ? Pd P C21 128.97(9) . . ? O1 P O2 101.68(9) . . ? O1 P C21 97.23(11) . . ? O2 P C21 104.47(12) . . ? P O1 C1 114.45(15) . . ? P O2 C20 119.35(16) . . ? C40 O3 C41 118.8(2) . . ? C46 O4 C48 119.3(5) . . ? O1 C1 C2 117.8(2) . . ? O1 C1 C10 118.7(2) . . ? C2 C1 C10 123.5(3) . . ? C1 C2 H2A 120.6 . . ? C1 C2 C3 118.7(3) . . ? H2A C2 C3 120.6 . . ? C2 C3 H3A 119.2 . . ? C2 C3 C4 121.5(3) . . ? H3A C3 C4 119.2 . . ? C3 C4 C5 122.7(3) . . ? C3 C4 C9 119.2(3) . . ? C5 C4 C9 118.1(3) . . ? C4 C5 H5A 118.9 . . ? C4 C5 C6 122.2(3) . . ? H5A C5 C6 118.9 . . ? C5 C6 H6A 120.3 . . ? C5 C6 C7 119.5(3) . . ? H6A C6 C7 120.3 . . ? C6 C7 H7A 119.3 . . ? C6 C7 C8 121.4(3) . . ? H7A C7 C8 119.3 . . ? C7 C8 H8A 119.9 . . ? C7 C8 C9 120.3(3) . . ? H8A C8 C9 119.9 . . ? C4 C9 C8 118.3(3) . . ? C4 C9 C10 119.0(3) . . ? C8 C9 C10 122.6(2) . . ? C1 C10 C9 117.8(2) . . ? C1 C10 C11 118.4(2) . . ? C9 C10 C11 123.7(2) . . ? C10 C11 C12 122.6(2) . . ? C10 C11 C20 119.9(3) . . ? C12 C11 C20 117.3(3) . . ? C11 C12 C13 122.1(3) . . ? C11 C12 C17 119.9(2) . . ? C13 C12 C17 117.9(3) . . ? C12 C13 H13A 119.6 . . ? C12 C13 C14 120.9(3) . . ? H13A C13 C14 119.6 . . ? C13 C14 H14A 119.5 . . ? C13 C14 C15 121.0(3) . . ? H14A C14 C15 119.5 . . ? C14 C15 H15A 120.0 . . ? C14 C15 C16 120.0(3) . . ? H15A C15 C16 120.0 . . ? C15 C16 H16A 119.4 . . ? C15 C16 C17 121.1(3) . . ? H16A C16 C17 119.4 . . ? C12 C17 C16 119.1(3) . . ? C12 C17 C18 119.3(3) . . ? C16 C17 C18 121.6(3) . . ? C17 C18 H18A 119.7 . . ? C17 C18 C19 120.6(3) . . ? H18A C18 C19 119.7 . . ? C18 C19 H19A 120.2 . . ? C18 C19 C20 119.5(3) . . ? H19A C19 C20 120.2 . . ? O2 C20 C11 119.5(3) . . ? O2 C20 C19 117.3(2) . . ? C11 C20 C19 123.2(3) . . ? P C21 C22 118.33(19) . . ? P C21 C30 121.70(19) . . ? C22 C21 C30 119.9(2) . . ? C21 C22 H22A 119.6 . . ? C21 C22 C23 120.9(3) . . ? H22A C22 C23 119.6 . . ? C22 C23 H23A 119.5 . . ? C22 C23 C24 121.1(3) . . ? H23A C23 C24 119.5 . . ? C23 C24 C25 122.2(3) . . ? C23 C24 C29 119.0(3) . . ? C25 C24 C29 118.8(3) . . ? C24 C25 H25A 119.6 . . ? C24 C25 C26 120.8(3) . . ? H25A C25 C26 119.6 . . ? C25 C26 H26A 119.6 . . ? C25 C26 C27 120.9(3) . . ? H26A C26 C27 119.6 . . ? C26 C27 H27A 120.3 . . ? C26 C27 C28 119.4(3) . . ? H27A C27 C28 120.3 . . ? C27 C28 H28A 119.0 . . ? C27 C28 C29 122.0(3) . . ? H28A C28 C29 119.0 . . ? C24 C29 C28 118.2(3) . . ? C24 C29 C30 119.6(3) . . ? C28 C29 C30 122.2(3) . . ? C21 C30 C29 119.5(2) . . ? C21 C30 C31 120.9(2) . . ? C29 C30 C31 119.5(2) . . ? C30 C31 C32 121.2(2) . . ? C30 C31 C40 118.9(2) . . ? C32 C31 C40 119.9(2) . . ? C31 C32 C33 123.0(2) . . ? C31 C32 C37 119.6(3) . . ? C33 C32 C37 117.4(2) . . ? C32 C33 H33A 119.2 . . ? C32 C33 C34 121.6(3) . . ? H33A C33 C34 119.2 . . ? C33 C34 H34A 119.7 . . ? C33 C34 C35 120.6(3) . . ? H34A C34 C35 119.7 . . ? C34 C35 H35A 120.2 . . ? C34 C35 C36 119.5(3) . . ? H35A C35 C36 120.2 . . ? C35 C36 H36A 119.4 . . ? C35 C36 C37 121.2(3) . . ? H36A C36 C37 119.4 . . ? C32 C37 C36 119.7(3) . . ? C32 C37 C38 118.5(2) . . ? C36 C37 C38 121.7(3) . . ? C37 C38 H38A 119.7 . . ? C37 C38 C39 120.6(3) . . ? H38A C38 C39 119.7 . . ? C38 C39 H39A 119.8 . . ? C38 C39 C40 120.4(3) . . ? H39A C39 C40 119.8 . . ? O3 C40 C31 116.2(2) . . ? O3 C40 C39 123.0(2) . . ? C31 C40 C39 120.8(2) . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Pd C42 H42A 116.6 . . ? Pd C42 H42B 116.6 . . ? Pd C42 C44 70.30(17) . . ? H42A C42 H42B 113.6 . . ? H42A C42 C44 116.6 . . ? H42B C42 C44 116.6 . . ? Pd C43 H43A 116.3 . . ? Pd C43 H43B 116.3 . . ? Pd C43 C44 72.75(16) . . ? H43A C43 H43B 113.3 . . ? H43A C43 C44 116.3 . . ? H43B C43 C44 116.3 . . ? Pd C44 C42 71.94(17) . . ? Pd C44 C43 68.54(16) . . ? Pd C44 C45 118.8(2) . . ? C42 C44 C43 115.0(3) . . ? C42 C44 C45 122.1(3) . . ? C43 C44 C45 121.7(3) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 C46 H46A 108.9 . . ? O4 C46 H46B 108.9 . . ? O4 C46 C47 113.2(6) . . ? H46A C46 H46B 107.8 . . ? H46A C46 C47 108.9 . . ? H46B C46 C47 108.9 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 H48A 107.0 . . ? O4 C48 H48B 107.0 . . ? O4 C48 C49 121.4(5) . . ? H48A C48 H48B 106.7 . . ? H48A C48 C49 107.0 . . ? H48B C48 C49 107.0 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 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 Cl Pd P O1 -52.23(7) . . . . ? Cl Pd P O2 -163.94(8) . . . . ? Cl Pd P C21 67.90(12) . . . . ? C42 Pd P O1 117.8(3) . . . . ? C42 Pd P O2 6.1(3) . . . . ? C42 Pd P C21 -122.1(3) . . . . ? C43 Pd P O1 124.48(11) . . . . ? C43 Pd P O2 12.77(11) . . . . ? C43 Pd P C21 -115.39(14) . . . . ? C44 Pd P O1 98.47(12) . . . . ? C44 Pd P O2 -13.24(13) . . . . ? C44 Pd P C21 -141.40(15) . . . . ? Pd P O1 C1 -60.67(17) . . . . ? O2 P O1 C1 55.54(18) . . . . ? C21 P O1 C1 162.01(18) . . . . ? Pd P O2 C20 155.17(17) . . . . ? O1 P O2 C20 36.7(2) . . . . ? C21 P O2 C20 -64.0(2) . . . . ? P O1 C1 C2 102.4(2) . . . . ? P O1 C1 C10 -79.2(3) . . . . ? O1 C1 C2 C3 177.5(2) . . . . ? C10 C1 C2 C3 -0.8(4) . . . . ? C1 C2 C3 C4 2.8(4) . . . . ? C2 C3 C4 C5 179.1(3) . . . . ? C2 C3 C4 C9 -0.5(4) . . . . ? C3 C4 C5 C6 -177.9(3) . . . . ? C9 C4 C5 C6 1.7(4) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? C5 C6 C7 C8 -2.7(4) . . . . ? C6 C7 C8 C9 0.6(4) . . . . ? C7 C8 C9 C4 2.6(4) . . . . ? C7 C8 C9 C10 -177.7(3) . . . . ? C3 C4 C9 C8 176.0(2) . . . . ? C3 C4 C9 C10 -3.8(4) . . . . ? C5 C4 C9 C8 -3.7(4) . . . . ? C5 C4 C9 C10 176.6(3) . . . . ? O1 C1 C10 C9 178.2(2) . . . . ? O1 C1 C10 C11 -2.2(4) . . . . ? C2 C1 C10 C9 -3.5(4) . . . . ? C2 C1 C10 C11 176.0(2) . . . . ? C4 C9 C10 C1 5.6(4) . . . . ? C4 C9 C10 C11 -173.8(2) . . . . ? C8 C9 C10 C1 -174.1(2) . . . . ? C8 C9 C10 C11 6.4(4) . . . . ? C1 C10 C11 C12 -120.3(3) . . . . ? C1 C10 C11 C20 53.8(4) . . . . ? C9 C10 C11 C12 59.1(4) . . . . ? C9 C10 C11 C20 -126.8(3) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? C10 C11 C12 C17 177.3(2) . . . . ? C20 C11 C12 C13 -173.5(3) . . . . ? C20 C11 C12 C17 3.1(4) . . . . ? C11 C12 C13 C14 177.5(3) . . . . ? C17 C12 C13 C14 0.9(4) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C17 -1.6(5) . . . . ? C11 C12 C17 C16 -178.7(3) . . . . ? C11 C12 C17 C18 0.5(4) . . . . ? C13 C12 C17 C16 -2.0(4) . . . . ? C13 C12 C17 C18 177.2(2) . . . . ? C15 C16 C17 C12 2.4(5) . . . . ? C15 C16 C17 C18 -176.8(3) . . . . ? C12 C17 C18 C19 -2.9(4) . . . . ? C16 C17 C18 C19 176.2(3) . . . . ? C17 C18 C19 C20 1.6(4) . . . . ? C10 C11 C20 O2 0.4(4) . . . . ? C10 C11 C20 C19 -179.0(2) . . . . ? C12 C11 C20 O2 174.8(2) . . . . ? C12 C11 C20 C19 -4.6(4) . . . . ? C18 C19 C20 O2 -177.1(2) . . . . ? C18 C19 C20 C11 2.3(4) . . . . ? P O2 C20 C11 -71.4(3) . . . . ? P O2 C20 C19 108.0(2) . . . . ? Pd P C21 C22 -158.65(17) . . . . ? Pd P C21 C30 24.8(3) . . . . ? O1 P C21 C22 -32.6(2) . . . . ? O1 P C21 C30 150.9(2) . . . . ? O2 P C21 C22 71.5(2) . . . . ? O2 P C21 C30 -105.0(2) . . . . ? P C21 C22 C23 -176.4(2) . . . . ? C30 C21 C22 C23 0.2(4) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? C22 C23 C24 C25 -179.6(3) . . . . ? C22 C23 C24 C29 0.0(4) . . . . ? C23 C24 C25 C26 -179.9(3) . . . . ? C29 C24 C25 C26 0.4(4) . . . . ? C24 C25 C26 C27 0.9(5) . . . . ? C25 C26 C27 C28 -0.8(5) . . . . ? C26 C27 C28 C29 -0.5(5) . . . . ? C27 C28 C29 C24 1.8(4) . . . . ? C27 C28 C29 C30 -178.3(3) . . . . ? C23 C24 C29 C28 178.6(2) . . . . ? C23 C24 C29 C30 -1.3(4) . . . . ? C25 C24 C29 C28 -1.7(4) . . . . ? C25 C24 C29 C30 178.3(2) . . . . ? P C21 C30 C29 174.9(2) . . . . ? P C21 C30 C31 -7.8(4) . . . . ? C22 C21 C30 C29 -1.6(4) . . . . ? C22 C21 C30 C31 175.7(3) . . . . ? C24 C29 C30 C21 2.1(4) . . . . ? C24 C29 C30 C31 -175.3(2) . . . . ? C28 C29 C30 C21 -177.8(3) . . . . ? C28 C29 C30 C31 4.8(4) . . . . ? C21 C30 C31 C32 81.1(3) . . . . ? C21 C30 C31 C40 -98.9(3) . . . . ? C29 C30 C31 C32 -101.6(3) . . . . ? C29 C30 C31 C40 78.4(3) . . . . ? C30 C31 C32 C33 2.0(4) . . . . ? C30 C31 C32 C37 -177.3(2) . . . . ? C40 C31 C32 C33 -178.0(2) . . . . ? C40 C31 C32 C37 2.7(4) . . . . ? C31 C32 C33 C34 -178.7(3) . . . . ? C37 C32 C33 C34 0.6(4) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? C33 C34 C35 C36 0.0(4) . . . . ? C34 C35 C36 C37 -0.3(4) . . . . ? C35 C36 C37 C32 0.8(4) . . . . ? C35 C36 C37 C38 178.7(3) . . . . ? C31 C32 C37 C36 178.4(2) . . . . ? C31 C32 C37 C38 0.4(4) . . . . ? C33 C32 C37 C36 -0.9(3) . . . . ? C33 C32 C37 C38 -178.9(2) . . . . ? C32 C37 C38 C39 -2.3(4) . . . . ? C36 C37 C38 C39 179.7(3) . . . . ? C37 C38 C39 C40 1.2(4) . . . . ? C41 O3 C40 C31 170.1(3) . . . . ? C41 O3 C40 C39 -9.6(4) . . . . ? C30 C31 C40 O3 -3.6(4) . . . . ? C30 C31 C40 C39 176.1(2) . . . . ? C32 C31 C40 O3 176.4(2) . . . . ? C32 C31 C40 C39 -3.9(4) . . . . ? C38 C39 C40 O3 -178.3(2) . . . . ? C38 C39 C40 C31 2.0(4) . . . . ? Cl Pd C42 C44 144.65(16) . . . . ? P Pd C42 C44 -25.4(4) . . . . ? C43 Pd C42 C44 -32.59(17) . . . . ? Cl Pd C43 C44 21.6(4) . . . . ? P Pd C43 C44 -146.19(16) . . . . ? C42 Pd C43 C44 31.83(17) . . . . ? Pd C42 C44 C43 54.8(2) . . . . ? Pd C42 C44 C45 -113.2(3) . . . . ? Pd C43 C44 C42 -56.5(2) . . . . ? Pd C43 C44 C45 111.5(3) . . . . ? Cl Pd C44 C42 -45.57(19) . . . . ? Cl Pd C44 C43 -172.91(14) . . . . ? Cl Pd C44 C45 71.7(3) . . . . ? P Pd C44 C42 171.47(14) . . . . ? P Pd C44 C43 44.1(2) . . . . ? P Pd C44 C45 -71.2(3) . . . . ? C42 Pd C44 C43 -127.3(3) . . . . ? C42 Pd C44 C45 117.3(3) . . . . ? C43 Pd C44 C42 127.3(3) . . . . ? C43 Pd C44 C45 -115.4(3) . . . . ? C48 O4 C46 C47 -160.5(6) . . . . ? C46 O4 C48 C49 -55.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.419 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.062 #===END data_ljh146 _database_code_depnum_ccdc_archive 'CCDC 854373' #TrackingRef '8a.CIF' # start Validation Reply Form _vrf_CHEMW03_LJH146 ; PROBLEM: The molecular weight ratio outside the range 0.90 <> 1.10 RESPONSE: DCM molecule squeezed, information appended to cif ; _vrf_PLAT043_LJH146 ; PROBLEM: Check Reported Molecular Weight ................ 880.47 RESPONSE: Again due to squeezed DCM ; _vrf_PLAT051_LJH146 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by 18.33 Perc. RESPONSE: Again due to squeezed DCM ; _vrf_PLAT220_LJH146 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) 4.6 Ratio RESPONSE: Methyl allyl shows signs of disorder that could not be resolved ; _vrf_PLAT241_LJH146 ; PROBLEM: Check High Ueq as Compared to Neighbors for C44 RESPONSE: Methyl allyl shows signs of disorder that could not be resolved ; _vrf_PLAT601_LJH146 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 106 A**3 RESPONSE: Void due to squeezed DCM ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H34 Cl O3 P Pd, C H2 Cl2' _chemical_formula_sum 'C46 H36 Cl3 O3 P Pd' _chemical_formula_weight 880.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 10.4065(4) _cell_length_b 17.4563(4) _cell_length_c 21.7841(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3957.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8935 _cell_measurement_theta_min 2.9421 _cell_measurement_theta_max 28.5193 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.8639 _exptl_absorpt_process_details ; 'Thu Nov 10 20:28:29 2011' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 22011 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 28.58 _reflns_number_total 8320 _reflns_number_gt 7461 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; 'Thu Nov 10 20:28:29 2011' ; _computing_cell_refinement ; 'Thu Nov 10 20:28:29 2011' ; _computing_data_reduction ; 'Thu Nov 10 20:28:29 2011' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.1841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 8320 _refine_ls_number_parameters 463 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.81027(3) 0.721039(14) 0.840306(10) 0.03372(8) Uani 1 1 d . . . Cl1 Cl 1.02271(10) 0.76867(6) 0.85195(4) 0.0484(2) Uani 1 1 d . . . P P 0.77236(8) 0.79195(4) 0.75675(3) 0.02520(18) Uani 1 1 d . . . O1 O 0.8854(2) 0.78022(13) 0.70615(8) 0.0261(4) Uani 1 1 d . . . O2 O 0.6474(2) 0.76497(12) 0.71763(9) 0.0260(5) Uani 1 1 d . . . O3 O 0.4279(3) 0.87723(16) 0.77848(14) 0.0505(7) Uani 1 1 d . . . C1 C 0.8881(3) 0.70600(18) 0.68127(14) 0.0270(7) Uani 1 1 d . . . C2 C 0.9736(4) 0.6535(2) 0.70571(15) 0.0345(8) Uani 1 1 d . . . H2A H 1.0300 0.6678 0.7380 0.041 Uiso 1 1 calc R . . C3 C 0.9756(4) 0.5803(2) 0.68245(15) 0.0347(8) Uani 1 1 d . . . H3A H 1.0339 0.5437 0.6988 0.042 Uiso 1 1 calc R . . C4 C 0.8922(4) 0.55937(18) 0.63477(15) 0.0325(8) Uani 1 1 d . . . C5 C 0.8924(4) 0.4839(2) 0.61126(18) 0.0434(9) Uani 1 1 d . . . H5A H 0.9496 0.4471 0.6282 0.052 Uiso 1 1 calc R . . C6 C 0.8128(5) 0.4630(2) 0.56517(19) 0.0529(10) Uani 1 1 d . . . H6A H 0.8169 0.4126 0.5489 0.064 Uiso 1 1 calc R . . C7 C 0.7255(6) 0.5149(2) 0.5418(2) 0.0672(15) Uani 1 1 d . . . H7A H 0.6689 0.4994 0.5099 0.081 Uiso 1 1 calc R . . C8 C 0.7189(5) 0.5892(2) 0.56384(18) 0.0532(12) Uani 1 1 d . . . H8A H 0.6567 0.6236 0.5478 0.064 Uiso 1 1 calc R . . C9 C 0.8038(4) 0.61355(17) 0.60982(14) 0.0323(7) Uani 1 1 d . . . C10 C 0.8042(4) 0.69032(16) 0.63391(13) 0.0284(7) Uani 1 1 d . . . C11 C 0.7145(3) 0.75149(17) 0.61324(13) 0.0279(7) Uani 1 1 d . . . C12 C 0.7078(4) 0.7776(2) 0.55121(13) 0.0349(7) Uani 1 1 d . . . C13 C 0.7924(5) 0.7498(2) 0.50488(16) 0.0533(11) Uani 1 1 d . . . H13A H 0.8545 0.7118 0.5147 0.064 Uiso 1 1 calc R . . C14 C 0.7844(5) 0.7776(3) 0.44652(16) 0.0646(13) Uani 1 1 d . . . H14A H 0.8399 0.7576 0.4159 0.078 Uiso 1 1 calc R . . C15 C 0.6961(6) 0.8349(3) 0.43067(18) 0.0697(14) Uani 1 1 d . . . H15A H 0.6929 0.8536 0.3898 0.084 Uiso 1 1 calc R . . C16 C 0.6144(5) 0.8638(3) 0.47434(18) 0.0525(11) Uani 1 1 d . . . H16A H 0.5546 0.9027 0.4635 0.063 Uiso 1 1 calc R . . C17 C 0.6187(4) 0.8361(2) 0.53575(16) 0.0392(9) Uani 1 1 d . . . C18 C 0.5419(4) 0.8688(2) 0.58186(16) 0.0358(8) Uani 1 1 d . . . H18A H 0.4820 0.9077 0.5714 0.043 Uiso 1 1 calc R . . C19 C 0.5523(4) 0.84561(19) 0.64094(16) 0.0334(8) Uani 1 1 d . . . H19A H 0.5008 0.8685 0.6719 0.040 Uiso 1 1 calc R . . C20 C 0.6394(3) 0.78783(17) 0.65597(13) 0.0273(6) Uani 1 1 d . . . C21 C 0.7594(3) 0.89540(18) 0.75571(14) 0.0282(7) Uani 1 1 d . . . C22 C 0.8254(4) 0.93864(17) 0.71073(13) 0.0305(7) Uani 1 1 d . . . H22A H 0.8845 0.9138 0.6841 0.037 Uiso 1 1 calc R . . C23 C 0.8055(4) 1.01542(17) 0.70514(14) 0.0331(7) Uani 1 1 d . . . H23A H 0.8511 1.0438 0.6750 0.040 Uiso 1 1 calc R . . C24 C 0.7173(3) 1.05271(17) 0.74402(14) 0.0282(7) Uani 1 1 d . . . C25 C 0.6957(4) 1.13332(17) 0.73936(16) 0.0365(8) Uani 1 1 d . . . H25A H 0.7407 1.1624 0.7094 0.044 Uiso 1 1 calc R . . C26 C 0.6111(4) 1.1685(2) 0.7776(2) 0.0454(10) Uani 1 1 d . . . H26A H 0.5960 1.2220 0.7739 0.054 Uiso 1 1 calc R . . C27 C 0.5465(4) 1.1264(2) 0.8223(2) 0.0513(11) Uani 1 1 d . . . H27A H 0.4888 1.1521 0.8491 0.062 Uiso 1 1 calc R . . C28 C 0.5638(4) 1.0491(2) 0.82885(19) 0.0436(9) Uani 1 1 d . . . H28A H 0.5175 1.0216 0.8593 0.052 Uiso 1 1 calc R . . C29 C 0.6517(3) 1.01011(18) 0.78953(15) 0.0303(7) Uani 1 1 d . . . C30 C 0.6742(4) 0.93000(17) 0.79498(14) 0.0299(7) Uani 1 1 d . . . C31 C 0.6032(4) 0.88681(19) 0.84419(18) 0.0410(9) Uani 1 1 d . . . C32 C 0.6621(5) 0.8761(3) 0.90312(18) 0.0552(12) Uani 1 1 d . . . C33 C 0.7860(6) 0.9041(3) 0.9176(2) 0.0742(16) Uani 1 1 d . . . H33A H 0.8352 0.9287 0.8867 0.089 Uiso 1 1 calc R . . C34 C 0.8358(7) 0.8964(5) 0.9746(2) 0.107(2) Uani 1 1 d . . . H34A H 0.9181 0.9168 0.9842 0.128 Uiso 1 1 calc R . . C35 C 0.7622(8) 0.8570(5) 1.0203(3) 0.121(3) Uani 1 1 d . . . H35A H 0.7973 0.8508 1.0603 0.145 Uiso 1 1 calc R . . C36 C 0.6454(8) 0.8288(4) 1.0083(2) 0.095(2) Uani 1 1 d . . . H36A H 0.5995 0.8019 1.0393 0.114 Uiso 1 1 calc R . . C37 C 0.5914(6) 0.8387(3) 0.9508(2) 0.0675(15) Uani 1 1 d . . . C38 C 0.4677(6) 0.8130(3) 0.9375(2) 0.0745(18) Uani 1 1 d . . . H38A H 0.4214 0.7867 0.9686 0.089 Uiso 1 1 calc R . . C39 C 0.4093(5) 0.8238(2) 0.8814(2) 0.0614(14) Uani 1 1 d . . . H39A H 0.3245 0.8059 0.8741 0.074 Uiso 1 1 calc R . . C40 C 0.4795(4) 0.8624(2) 0.8347(2) 0.0479(10) Uani 1 1 d . . . C41 C 0.2909(5) 0.8709(3) 0.7718(3) 0.0731(14) Uani 1 1 d . . . H41A H 0.2659 0.8876 0.7305 0.110 Uiso 1 1 calc R . . H41B H 0.2485 0.9033 0.8024 0.110 Uiso 1 1 calc R . . H41C H 0.2649 0.8174 0.7778 0.110 Uiso 1 1 calc R . . C42 C 0.6304(4) 0.6665(2) 0.8462(2) 0.0492(10) Uani 1 1 d U . . H42A H 0.5702 0.6868 0.8774 0.059 Uiso 1 1 calc R . . H42B H 0.5882 0.6537 0.8068 0.059 Uiso 1 1 calc R . . C43 C 0.7243(5) 0.6143(2) 0.8675(2) 0.0578(12) Uani 1 1 d U . . C44 C 0.7993(6) 0.6390(3) 0.9159(2) 0.0854(18) Uani 1 1 d U . . H44A H 0.8779 0.6089 0.9246 0.102 Uiso 1 1 calc R . . H44B H 0.7532 0.6560 0.9532 0.102 Uiso 1 1 calc R . . C45 C 0.7534(7) 0.5447(3) 0.8283(4) 0.125(3) Uani 1 1 d U . . H45A H 0.6915 0.5040 0.8375 0.187 Uiso 1 1 calc R . . H45B H 0.8406 0.5266 0.8371 0.187 Uiso 1 1 calc R . . H45C H 0.7469 0.5586 0.7848 0.187 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03889(16) 0.03363(13) 0.02863(12) 0.01182(11) -0.00438(11) -0.00574(12) Cl1 0.0419(5) 0.0634(6) 0.0398(5) 0.0132(4) -0.0095(4) -0.0144(5) P 0.0292(5) 0.0236(4) 0.0228(3) 0.0041(3) 0.0023(3) -0.0001(3) O1 0.0265(12) 0.0269(10) 0.0249(10) 0.0012(10) 0.0021(8) 0.0001(11) O2 0.0283(13) 0.0262(11) 0.0236(9) 0.0038(9) 0.0010(8) 0.0003(9) O3 0.0350(17) 0.0502(16) 0.0663(19) 0.0017(14) 0.0168(14) -0.0070(13) C1 0.0260(18) 0.0303(17) 0.0248(14) 0.0022(13) 0.0033(12) -0.0012(14) C2 0.030(2) 0.044(2) 0.0296(16) 0.0052(16) 0.0001(14) 0.0049(16) C3 0.036(2) 0.0318(18) 0.0363(17) 0.0089(15) 0.0008(15) 0.0112(16) C4 0.035(2) 0.0306(17) 0.0322(16) 0.0090(14) 0.0101(15) 0.0036(15) C5 0.053(3) 0.0326(18) 0.045(2) 0.0039(16) 0.0094(19) 0.0047(18) C6 0.068(3) 0.0341(18) 0.057(2) -0.0100(17) 0.001(2) 0.002(2) C7 0.088(4) 0.051(2) 0.063(3) -0.021(2) -0.029(3) 0.009(3) C8 0.069(3) 0.045(2) 0.046(2) -0.0137(18) -0.020(2) 0.016(2) C9 0.037(2) 0.0315(15) 0.0279(15) 0.0005(13) 0.0033(16) 0.0053(17) C10 0.034(2) 0.0286(14) 0.0229(13) 0.0041(11) 0.0045(14) 0.0069(15) C11 0.030(2) 0.0267(14) 0.0275(14) 0.0021(12) -0.0063(13) 0.0050(13) C12 0.041(2) 0.0387(16) 0.0251(14) 0.0026(14) -0.0037(13) 0.0049(19) C13 0.071(3) 0.059(2) 0.0290(16) 0.0073(16) -0.0033(19) 0.021(2) C14 0.093(4) 0.074(3) 0.0264(16) 0.012(2) 0.0030(19) 0.033(3) C15 0.087(4) 0.093(3) 0.0294(19) 0.017(2) -0.009(2) 0.030(3) C16 0.058(3) 0.063(3) 0.037(2) 0.015(2) -0.0099(19) 0.016(2) C17 0.039(2) 0.043(2) 0.0356(18) 0.0092(16) -0.0073(16) 0.0077(17) C18 0.030(2) 0.0351(18) 0.0423(19) 0.0053(15) -0.0052(15) 0.0052(16) C19 0.027(2) 0.0323(17) 0.0406(18) 0.0041(15) 0.0008(14) 0.0032(15) C20 0.0281(17) 0.0277(15) 0.0261(14) 0.0050(15) -0.0065(12) -0.0055(13) C21 0.0296(19) 0.0312(16) 0.0239(15) 0.0044(13) 0.0007(13) -0.0009(14) C22 0.039(2) 0.0290(15) 0.0229(14) 0.0001(12) 0.0069(15) -0.0020(16) C23 0.038(2) 0.0310(15) 0.0308(15) 0.0056(13) 0.0004(16) -0.0083(17) C24 0.0237(19) 0.0281(14) 0.0327(15) 0.0014(13) -0.0062(13) -0.0027(13) C25 0.031(2) 0.0283(15) 0.0503(19) 0.0049(14) -0.0058(18) -0.0002(16) C26 0.033(2) 0.0286(18) 0.075(3) 0.0032(18) -0.003(2) 0.0093(16) C27 0.042(3) 0.039(2) 0.073(3) -0.007(2) 0.013(2) 0.0112(18) C28 0.041(2) 0.0331(18) 0.057(2) 0.0028(17) 0.0133(18) 0.0061(16) C29 0.028(2) 0.0269(15) 0.0359(17) 0.0012(14) 0.0041(14) 0.0027(13) C30 0.033(2) 0.0274(15) 0.0296(15) 0.0044(12) 0.0054(14) -0.0017(15) C31 0.052(3) 0.0305(17) 0.040(2) 0.0071(16) 0.0261(19) 0.0061(17) C32 0.065(3) 0.061(3) 0.039(2) 0.0156(19) 0.023(2) 0.011(2) C33 0.065(4) 0.113(4) 0.045(2) 0.029(3) 0.014(2) 0.013(3) C34 0.084(5) 0.197(7) 0.040(3) 0.029(4) 0.008(3) 0.005(5) C35 0.122(7) 0.201(8) 0.041(3) 0.048(4) 0.021(3) 0.033(6) C36 0.098(5) 0.137(6) 0.051(3) 0.045(3) 0.035(3) 0.015(4) C37 0.077(4) 0.073(3) 0.052(3) 0.022(2) 0.034(3) 0.011(3) C38 0.097(5) 0.056(3) 0.070(3) 0.029(2) 0.052(3) 0.013(3) C39 0.056(3) 0.044(2) 0.084(4) 0.006(2) 0.041(3) 0.003(2) C40 0.057(3) 0.0313(18) 0.055(2) 0.0033(18) 0.027(2) 0.0012(18) C41 0.047(3) 0.081(3) 0.092(4) 0.005(3) 0.023(3) 0.012(3) C42 0.052(3) 0.043(2) 0.052(2) 0.0082(19) 0.004(2) -0.0142(18) C43 0.054(3) 0.0365(19) 0.083(3) 0.030(2) 0.005(2) -0.0069(19) C44 0.071(4) 0.104(4) 0.081(3) 0.076(3) -0.016(3) -0.024(3) C45 0.117(6) 0.036(2) 0.220(8) 0.000(3) 0.056(6) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl1 2.3755(10) . ? Pd P 2.2363(8) . ? Pd C42 2.104(4) . ? Pd C43 2.151(4) . ? Pd C44 2.185(4) . ? P O1 1.625(2) . ? P O2 1.625(2) . ? P C21 1.811(3) . ? O1 C1 1.405(4) . ? O2 C20 1.404(3) . ? O3 C40 1.361(5) . ? O3 C41 1.438(6) . ? C1 C2 1.384(5) . ? C1 C10 1.379(5) . ? C2 H2A 0.950 . ? C2 C3 1.375(5) . ? C3 H3A 0.950 . ? C3 C4 1.402(5) . ? C4 C5 1.414(5) . ? C4 C9 1.427(5) . ? C5 H5A 0.950 . ? C5 C6 1.352(6) . ? C6 H6A 0.950 . ? C6 C7 1.380(6) . ? C7 H7A 0.950 . ? C7 C8 1.384(6) . ? C8 H8A 0.950 . ? C8 C9 1.402(5) . ? C9 C10 1.439(4) . ? C10 C11 1.488(4) . ? C11 C12 1.428(4) . ? C11 C20 1.371(4) . ? C12 C13 1.425(5) . ? C12 C17 1.419(5) . ? C13 H13A 0.950 . ? C13 C14 1.363(5) . ? C14 H14A 0.950 . ? C14 C15 1.401(6) . ? C15 H15A 0.950 . ? C15 C16 1.373(6) . ? C16 H16A 0.950 . ? C16 C17 1.424(5) . ? C17 C18 1.404(5) . ? C18 H18A 0.950 . ? C18 C19 1.353(5) . ? C19 H19A 0.950 . ? C19 C20 1.395(5) . ? C21 C22 1.415(4) . ? C21 C30 1.373(5) . ? C22 H22A 0.950 . ? C22 C23 1.362(4) . ? C23 H23A 0.950 . ? C23 C24 1.408(5) . ? C24 C25 1.429(4) . ? C24 C29 1.415(5) . ? C25 H25A 0.950 . ? C25 C26 1.359(5) . ? C26 H26A 0.950 . ? C26 C27 1.393(6) . ? C27 H27A 0.950 . ? C27 C28 1.370(5) . ? C28 H28A 0.950 . ? C28 C29 1.426(5) . ? C29 C30 1.423(4) . ? C30 C31 1.504(5) . ? C31 C32 1.435(6) . ? C31 C40 1.371(6) . ? C32 C33 1.414(8) . ? C32 C37 1.430(6) . ? C33 H33A 0.950 . ? C33 C34 1.352(7) . ? C34 H34A 0.950 . ? C34 C35 1.432(9) . ? C35 H35A 0.950 . ? C35 C36 1.338(10) . ? C36 H36A 0.950 . ? C36 C37 1.384(8) . ? C37 C38 1.395(9) . ? C38 H38A 0.950 . ? C38 C39 1.376(8) . ? C39 H39A 0.950 . ? C39 C40 1.424(6) . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C42 C43 1.415(6) . ? C43 C44 1.381(7) . ? C43 C45 1.514(8) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C45 H45A 0.980 . ? C45 H45B 0.980 . ? C45 H45C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd P 93.29(3) . . ? Cl1 Pd C42 168.46(12) . . ? Cl1 Pd C43 131.39(13) . . ? Cl1 Pd C44 101.41(16) . . ? P Pd C42 98.24(12) . . ? P Pd C43 129.07(14) . . ? P Pd C44 165.19(16) . . ? C42 Pd C43 38.82(17) . . ? C42 Pd C44 67.08(19) . . ? C43 Pd C44 37.13(19) . . ? Pd P O1 110.78(8) . . ? Pd P O2 114.06(8) . . ? Pd P C21 125.12(11) . . ? O1 P O2 100.77(11) . . ? O1 P C21 99.85(14) . . ? O2 P C21 102.89(14) . . ? P O1 C1 113.13(19) . . ? P O2 C20 117.84(19) . . ? C40 O3 C41 117.9(3) . . ? O1 C1 C2 118.4(3) . . ? O1 C1 C10 117.3(3) . . ? C2 C1 C10 124.3(3) . . ? C1 C2 H2A 120.5 . . ? C1 C2 C3 118.9(3) . . ? H2A C2 C3 120.5 . . ? C2 C3 H3A 119.8 . . ? C2 C3 C4 120.4(3) . . ? H3A C3 C4 119.8 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 C9 120.6(3) . . ? C5 C4 C9 118.8(3) . . ? C4 C5 H5A 119.4 . . ? C4 C5 C6 121.3(4) . . ? H5A C5 C6 119.4 . . ? C5 C6 H6A 120.0 . . ? C5 C6 C7 120.0(4) . . ? H6A C6 C7 120.0 . . ? C6 C7 H7A 119.4 . . ? C6 C7 C8 121.3(4) . . ? H7A C7 C8 119.4 . . ? C7 C8 H8A 120.0 . . ? C7 C8 C9 120.1(4) . . ? H8A C8 C9 120.0 . . ? C4 C9 C8 118.5(3) . . ? C4 C9 C10 118.5(3) . . ? C8 C9 C10 123.0(3) . . ? C1 C10 C9 117.3(3) . . ? C1 C10 C11 118.8(3) . . ? C9 C10 C11 123.8(3) . . ? C10 C11 C12 123.1(3) . . ? C10 C11 C20 119.0(3) . . ? C12 C11 C20 117.8(3) . . ? C11 C12 C13 122.1(3) . . ? C11 C12 C17 119.1(3) . . ? C13 C12 C17 118.7(3) . . ? C12 C13 H13A 119.9 . . ? C12 C13 C14 120.1(4) . . ? H13A C13 C14 119.9 . . ? C13 C14 H14A 119.2 . . ? C13 C14 C15 121.6(4) . . ? H14A C14 C15 119.2 . . ? C14 C15 H15A 120.1 . . ? C14 C15 C16 119.9(4) . . ? H15A C15 C16 120.1 . . ? C15 C16 H16A 119.8 . . ? C15 C16 C17 120.4(4) . . ? H16A C16 C17 119.8 . . ? C12 C17 C16 119.2(3) . . ? C12 C17 C18 119.6(3) . . ? C16 C17 C18 121.1(3) . . ? C17 C18 H18A 119.6 . . ? C17 C18 C19 120.9(3) . . ? H18A C18 C19 119.6 . . ? C18 C19 H19A 120.3 . . ? C18 C19 C20 119.4(3) . . ? H19A C19 C20 120.3 . . ? O2 C20 C11 119.0(3) . . ? O2 C20 C19 117.9(3) . . ? C11 C20 C19 123.1(3) . . ? P C21 C22 120.3(2) . . ? P C21 C30 118.6(2) . . ? C22 C21 C30 120.7(3) . . ? C21 C22 H22A 119.6 . . ? C21 C22 C23 120.9(3) . . ? H22A C22 C23 119.6 . . ? C22 C23 H23A 120.0 . . ? C22 C23 C24 120.0(3) . . ? H23A C23 C24 120.0 . . ? C23 C24 C25 121.0(3) . . ? C23 C24 C29 119.5(3) . . ? C25 C24 C29 119.4(3) . . ? C24 C25 H25A 119.9 . . ? C24 C25 C26 120.2(3) . . ? H25A C25 C26 119.9 . . ? C25 C26 H26A 119.9 . . ? C25 C26 C27 120.2(3) . . ? H26A C26 C27 119.9 . . ? C26 C27 H27A 119.0 . . ? C26 C27 C28 121.9(4) . . ? H27A C27 C28 119.0 . . ? C27 C28 H28A 120.3 . . ? C27 C28 C29 119.5(4) . . ? H28A C28 C29 120.3 . . ? C24 C29 C28 118.7(3) . . ? C24 C29 C30 119.7(3) . . ? C28 C29 C30 121.6(3) . . ? C21 C30 C29 119.1(3) . . ? C21 C30 C31 122.7(3) . . ? C29 C30 C31 118.1(3) . . ? C30 C31 C32 119.5(4) . . ? C30 C31 C40 120.6(4) . . ? C32 C31 C40 119.7(4) . . ? C31 C32 C33 123.0(4) . . ? C31 C32 C37 119.3(5) . . ? C33 C32 C37 117.6(4) . . ? C32 C33 H33A 119.3 . . ? C32 C33 C34 121.4(5) . . ? H33A C33 C34 119.3 . . ? C33 C34 H34A 120.6 . . ? C33 C34 C35 118.7(7) . . ? H34A C34 C35 120.6 . . ? C34 C35 H35A 119.1 . . ? C34 C35 C36 121.8(6) . . ? H35A C35 C36 119.1 . . ? C35 C36 H36A 120.0 . . ? C35 C36 C37 120.0(5) . . ? H36A C36 C37 120.0 . . ? C32 C37 C36 120.4(6) . . ? C32 C37 C38 118.1(5) . . ? C36 C37 C38 121.5(5) . . ? C37 C38 H38A 118.4 . . ? C37 C38 C39 123.2(4) . . ? H38A C38 C39 118.4 . . ? C38 C39 H39A 120.9 . . ? C38 C39 C40 118.2(5) . . ? H39A C39 C40 120.9 . . ? O3 C40 C31 116.6(3) . . ? O3 C40 C39 122.1(4) . . ? C31 C40 C39 121.3(5) . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Pd C42 H42A 116.3 . . ? Pd C42 H42B 116.3 . . ? Pd C42 C43 72.4(2) . . ? H42A C42 H42B 113.3 . . ? H42A C42 C43 116.3 . . ? H42B C42 C43 116.3 . . ? Pd C43 C42 68.8(2) . . ? Pd C43 C44 72.8(2) . . ? Pd C43 C45 117.1(4) . . ? C42 C43 C44 116.0(4) . . ? C42 C43 C45 118.1(5) . . ? C44 C43 C45 124.6(6) . . ? Pd C44 C43 70.1(2) . . ? Pd C44 H44A 116.6 . . ? Pd C44 H44B 116.6 . . ? C43 C44 H44A 116.6 . . ? C43 C44 H44B 116.6 . . ? H44A C44 H44B 113.6 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd P O1 51.79(10) . . . . ? Cl1 Pd P O2 164.64(9) . . . . ? Cl1 Pd P C21 -67.58(15) . . . . ? C42 Pd P O1 -128.64(16) . . . . ? C42 Pd P O2 -15.79(16) . . . . ? C42 Pd P C21 111.99(19) . . . . ? C43 Pd P O1 -102.32(19) . . . . ? C43 Pd P O2 10.5(2) . . . . ? C43 Pd P C21 138.3(2) . . . . ? C44 Pd P O1 -121.1(7) . . . . ? C44 Pd P O2 -8.2(8) . . . . ? C44 Pd P C21 119.5(7) . . . . ? Pd P O1 C1 66.8(2) . . . . ? O2 P O1 C1 -54.3(2) . . . . ? C21 P O1 C1 -159.6(2) . . . . ? Pd P O2 C20 -159.49(18) . . . . ? O1 P O2 C20 -40.8(2) . . . . ? C21 P O2 C20 62.0(2) . . . . ? P O1 C1 C2 -97.2(3) . . . . ? P O1 C1 C10 82.5(3) . . . . ? O1 C1 C2 C3 178.9(3) . . . . ? C10 C1 C2 C3 -0.8(5) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 -179.0(4) . . . . ? C2 C3 C4 C9 -0.2(5) . . . . ? C3 C4 C5 C6 -179.8(4) . . . . ? C9 C4 C5 C6 1.3(6) . . . . ? C4 C5 C6 C7 -2.6(7) . . . . ? C5 C6 C7 C8 1.2(8) . . . . ? C6 C7 C8 C9 1.5(8) . . . . ? C7 C8 C9 C4 -2.7(6) . . . . ? C7 C8 C9 C10 178.6(4) . . . . ? C3 C4 C9 C8 -177.6(4) . . . . ? C3 C4 C9 C10 1.2(5) . . . . ? C5 C4 C9 C8 1.3(5) . . . . ? C5 C4 C9 C10 -179.9(3) . . . . ? O1 C1 C10 C9 -177.9(3) . . . . ? O1 C1 C10 C11 -1.5(4) . . . . ? C2 C1 C10 C9 1.8(5) . . . . ? C2 C1 C10 C11 178.2(3) . . . . ? C4 C9 C10 C1 -1.9(5) . . . . ? C4 C9 C10 C11 -178.1(3) . . . . ? C8 C9 C10 C1 176.8(4) . . . . ? C8 C9 C10 C11 0.6(6) . . . . ? C1 C10 C11 C12 124.2(3) . . . . ? C1 C10 C11 C20 -52.1(4) . . . . ? C9 C10 C11 C12 -59.6(5) . . . . ? C9 C10 C11 C20 124.1(3) . . . . ? C10 C11 C12 C13 -3.7(6) . . . . ? C10 C11 C12 C17 179.7(3) . . . . ? C20 C11 C12 C13 172.6(4) . . . . ? C20 C11 C12 C17 -4.0(5) . . . . ? C11 C12 C13 C14 -178.6(4) . . . . ? C17 C12 C13 C14 -2.0(7) . . . . ? C12 C13 C14 C15 1.6(8) . . . . ? C13 C14 C15 C16 -0.6(9) . . . . ? C14 C15 C16 C17 0.0(8) . . . . ? C11 C12 C17 C16 178.1(4) . . . . ? C11 C12 C17 C18 2.0(5) . . . . ? C13 C12 C17 C16 1.4(6) . . . . ? C13 C12 C17 C18 -174.7(4) . . . . ? C15 C16 C17 C12 -0.5(7) . . . . ? C15 C16 C17 C18 175.6(4) . . . . ? C12 C17 C18 C19 0.4(6) . . . . ? C16 C17 C18 C19 -175.6(4) . . . . ? C17 C18 C19 C20 -0.7(6) . . . . ? C10 C11 C20 O2 -1.4(4) . . . . ? C10 C11 C20 C19 -179.8(3) . . . . ? C12 C11 C20 O2 -177.9(3) . . . . ? C12 C11 C20 C19 3.8(5) . . . . ? C18 C19 C20 O2 -179.8(3) . . . . ? C18 C19 C20 C11 -1.4(5) . . . . ? P O2 C20 C11 75.6(3) . . . . ? P O2 C20 C19 -106.0(3) . . . . ? Pd P C21 C22 133.2(2) . . . . ? Pd P C21 C30 -53.7(3) . . . . ? O1 P C21 C22 8.9(3) . . . . ? O1 P C21 C30 -177.9(3) . . . . ? O2 P C21 C22 -94.6(3) . . . . ? O2 P C21 C30 78.6(3) . . . . ? P C21 C22 C23 172.7(3) . . . . ? C30 C21 C22 C23 -0.3(5) . . . . ? C21 C22 C23 C24 -0.6(5) . . . . ? C22 C23 C24 C25 179.4(3) . . . . ? C22 C23 C24 C29 1.2(5) . . . . ? C23 C24 C25 C26 -179.4(3) . . . . ? C29 C24 C25 C26 -1.2(5) . . . . ? C24 C25 C26 C27 1.1(6) . . . . ? C25 C26 C27 C28 -1.0(7) . . . . ? C26 C27 C28 C29 1.0(7) . . . . ? C23 C24 C29 C28 179.4(3) . . . . ? C23 C24 C29 C30 -0.8(5) . . . . ? C25 C24 C29 C28 1.1(5) . . . . ? C25 C24 C29 C30 -179.1(3) . . . . ? C27 C28 C29 C24 -1.0(6) . . . . ? C27 C28 C29 C30 179.2(4) . . . . ? P C21 C30 C29 -172.5(3) . . . . ? P C21 C30 C31 7.8(5) . . . . ? C22 C21 C30 C29 0.7(5) . . . . ? C22 C21 C30 C31 -179.0(3) . . . . ? C24 C29 C30 C21 -0.1(5) . . . . ? C24 C29 C30 C31 179.6(3) . . . . ? C28 C29 C30 C21 179.7(3) . . . . ? C28 C29 C30 C31 -0.6(5) . . . . ? C21 C30 C31 C32 86.6(4) . . . . ? C21 C30 C31 C40 -98.0(4) . . . . ? C29 C30 C31 C32 -93.1(4) . . . . ? C29 C30 C31 C40 82.3(4) . . . . ? C30 C31 C32 C33 -0.4(6) . . . . ? C30 C31 C32 C37 176.6(4) . . . . ? C40 C31 C32 C33 -175.8(4) . . . . ? C40 C31 C32 C37 1.1(6) . . . . ? C31 C32 C33 C34 176.5(6) . . . . ? C37 C32 C33 C34 -0.5(8) . . . . ? C32 C33 C34 C35 1.9(11) . . . . ? C33 C34 C35 C36 -1.0(13) . . . . ? C34 C35 C36 C37 -1.4(13) . . . . ? C35 C36 C37 C32 2.8(10) . . . . ? C35 C36 C37 C38 -177.2(7) . . . . ? C31 C32 C37 C36 -178.9(5) . . . . ? C31 C32 C37 C38 1.0(7) . . . . ? C33 C32 C37 C36 -1.9(7) . . . . ? C33 C32 C37 C38 178.1(5) . . . . ? C32 C37 C38 C39 -1.9(7) . . . . ? C36 C37 C38 C39 178.0(5) . . . . ? C37 C38 C39 C40 0.7(7) . . . . ? C41 O3 C40 C31 -164.3(4) . . . . ? C41 O3 C40 C39 15.6(6) . . . . ? C30 C31 C40 O3 2.0(5) . . . . ? C30 C31 C40 C39 -177.8(3) . . . . ? C32 C31 C40 O3 177.4(3) . . . . ? C32 C31 C40 C39 -2.5(5) . . . . ? C38 C39 C40 O3 -178.3(4) . . . . ? C38 C39 C40 C31 1.6(6) . . . . ? Cl1 Pd C42 C43 -35.5(8) . . . . ? P Pd C42 C43 146.7(3) . . . . ? C44 Pd C42 C43 -31.2(3) . . . . ? Pd C42 C43 C44 57.2(4) . . . . ? Pd C42 C43 C45 -110.3(4) . . . . ? Cl1 Pd C43 C42 171.1(2) . . . . ? Cl1 Pd C43 C44 43.4(4) . . . . ? Cl1 Pd C43 C45 -77.3(5) . . . . ? P Pd C43 C42 -44.4(3) . . . . ? P Pd C43 C44 -172.2(3) . . . . ? P Pd C43 C45 67.2(5) . . . . ? C42 Pd C43 C44 -127.8(5) . . . . ? C42 Pd C43 C45 111.6(6) . . . . ? C44 Pd C43 C42 127.8(5) . . . . ? C44 Pd C43 C45 -120.6(6) . . . . ? C42 C43 C44 Pd -55.1(4) . . . . ? C45 C43 C44 Pd 111.5(5) . . . . ? Cl1 Pd C44 C43 -148.3(3) . . . . ? P Pd C44 C43 24.4(10) . . . . ? C42 Pd C44 C43 32.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.380 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.067 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 0.407 0.930 104 22 ' ' 2 0.005 0.907 0.570 104 22 ' ' 3 0.049 0.465 0.382 17 1 ' ' 4 0.495 0.093 0.070 104 22 ' ' 5 0.506 0.593 0.430 104 22 ' ' 6 0.454 0.535 0.881 18 1 ' ' 7 0.546 0.035 0.619 17 1 ' ' 8 0.954 0.964 0.119 17 1 ' ' _platon_squeeze_details ; ; # Contents of RES file _computing_special_details ; TITL ljh146 in P2(1)2(1)2(1) CELL 0.71073 10.4065 17.4563 21.7841 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0005 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O P PD Cl UNIT 184 144 12 4 4 12 TEMP -123 REM 1 DCM molecule squeezed per AU L.S. 8 BOND $H CONF ACTA 50 FMAP 2 PLAN 5 REM colourless block SIZE 0.32 0.20 0.20 SIMU C42 > C45 DELU c42 > c45 OMIT 0 2 3 OMIT 1 0 3 OMIT 2 0 2 REM EXTI 0.000064 WGHT 0.049300 0.184100 FVAR 1.56575 0.52356 PD 5 0.810274 0.721039 0.840306 11.00000 0.03889 0.03363 = 0.02863 0.01182 -0.00438 -0.00574 CL1 6 1.022711 0.768668 0.851955 11.00000 0.04193 0.06335 = 0.03981 0.01317 -0.00949 -0.01443 P 4 0.772362 0.791953 0.756752 11.00000 0.02916 0.02360 = 0.02284 0.00412 0.00232 -0.00008 O1 3 0.885363 0.780222 0.706152 11.00000 0.02646 0.02687 = 0.02494 0.00119 0.00214 0.00011 O2 3 0.647411 0.764967 0.717628 11.00000 0.02829 0.02625 = 0.02361 0.00382 0.00101 0.00032 O3 3 0.427930 0.877234 0.778476 11.00000 0.03504 0.05022 = 0.06631 0.00169 0.01677 -0.00704 C1 1 0.888110 0.705995 0.681265 11.00000 0.02599 0.03032 = 0.02479 0.00221 0.00329 -0.00120 C2 1 0.973616 0.653503 0.705712 11.00000 0.02988 0.04398 = 0.02962 0.00516 0.00015 0.00485 AFIX 43 H2A 2 1.029999 0.667813 0.738036 11.00000 -1.20000 AFIX 0 C3 1 0.975618 0.580309 0.682451 11.00000 0.03582 0.03180 = 0.03635 0.00887 0.00076 0.01116 AFIX 43 H3A 2 1.033878 0.543696 0.698773 11.00000 -1.20000 AFIX 0 C4 1 0.892167 0.559365 0.634767 11.00000 0.03473 0.03061 = 0.03223 0.00904 0.01007 0.00355 C5 1 0.892377 0.483870 0.611263 11.00000 0.05275 0.03262 = 0.04484 0.00391 0.00936 0.00472 AFIX 43 H5A 2 0.949577 0.447091 0.628190 11.00000 -1.20000 AFIX 0 C6 1 0.812757 0.463013 0.565168 11.00000 0.06755 0.03412 = 0.05708 -0.00995 0.00115 0.00155 AFIX 43 H6A 2 0.816852 0.412597 0.548863 11.00000 -1.20000 AFIX 0 C7 1 0.725504 0.514934 0.541778 11.00000 0.08774 0.05101 = 0.06279 -0.02065 -0.02947 0.00945 AFIX 43 H7A 2 0.668891 0.499403 0.509911 11.00000 -1.20000 AFIX 0 C8 1 0.718898 0.589151 0.563840 11.00000 0.06912 0.04503 = 0.04552 -0.01373 -0.02032 0.01589 AFIX 43 H8A 2 0.656737 0.623624 0.547811 11.00000 -1.20000 AFIX 0 C9 1 0.803810 0.613552 0.609817 11.00000 0.03728 0.03153 = 0.02794 0.00046 0.00333 0.00529 C10 1 0.804171 0.690318 0.633911 11.00000 0.03361 0.02862 = 0.02286 0.00407 0.00453 0.00690 C11 1 0.714502 0.751494 0.613242 11.00000 0.02963 0.02674 = 0.02748 0.00210 -0.00628 0.00501 C12 1 0.707766 0.777595 0.551213 11.00000 0.04081 0.03867 = 0.02509 0.00255 -0.00368 0.00487 C13 1 0.792364 0.749794 0.504882 11.00000 0.07129 0.05944 = 0.02904 0.00733 -0.00334 0.02135 AFIX 43 H13A 2 0.854479 0.711831 0.514675 11.00000 -1.20000 AFIX 0 C14 1 0.784359 0.777560 0.446521 11.00000 0.09310 0.07440 = 0.02645 0.01216 0.00304 0.03343 AFIX 43 H14A 2 0.839941 0.757570 0.415858 11.00000 -1.20000 AFIX 0 C15 1 0.696132 0.834871 0.430667 11.00000 0.08676 0.09300 = 0.02938 0.01721 -0.00889 0.03012 AFIX 43 H15A 2 0.692872 0.853643 0.389764 11.00000 -1.20000 AFIX 0 C16 1 0.614420 0.863845 0.474339 11.00000 0.05791 0.06301 = 0.03654 0.01477 -0.00986 0.01627 AFIX 43 H16A 2 0.554644 0.902698 0.463518 11.00000 -1.20000 AFIX 0 C17 1 0.618663 0.836050 0.535753 11.00000 0.03945 0.04260 = 0.03561 0.00916 -0.00732 0.00772 C18 1 0.541949 0.868770 0.581865 11.00000 0.03008 0.03513 = 0.04226 0.00531 -0.00518 0.00517 AFIX 43 H18A 2 0.481972 0.907682 0.571442 11.00000 -1.20000 AFIX 0 C19 1 0.552322 0.845613 0.640939 11.00000 0.02730 0.03230 = 0.04064 0.00406 0.00078 0.00316 AFIX 43 H19A 2 0.500752 0.868500 0.671899 11.00000 -1.20000 AFIX 0 C20 1 0.639427 0.787829 0.655971 11.00000 0.02813 0.02772 = 0.02612 0.00498 -0.00646 -0.00553 C21 1 0.759415 0.895398 0.755710 11.00000 0.02960 0.03123 = 0.02390 0.00438 0.00074 -0.00094 C22 1 0.825449 0.938640 0.710727 11.00000 0.03945 0.02903 = 0.02292 0.00011 0.00695 -0.00199 AFIX 43 H22A 2 0.884461 0.913779 0.684077 11.00000 -1.20000 AFIX 0 C23 1 0.805519 1.015419 0.705138 11.00000 0.03755 0.03098 = 0.03076 0.00565 0.00040 -0.00829 AFIX 43 H23A 2 0.851125 1.043841 0.674998 11.00000 -1.20000 AFIX 0 C24 1 0.717333 1.052714 0.744016 11.00000 0.02367 0.02811 = 0.03269 0.00144 -0.00621 -0.00273 C25 1 0.695749 1.133323 0.739363 11.00000 0.03077 0.02835 = 0.05034 0.00486 -0.00580 -0.00024 AFIX 43 H25A 2 0.740677 1.162435 0.709413 11.00000 -1.20000 AFIX 0 C26 1 0.611139 1.168517 0.777643 11.00000 0.03295 0.02865 = 0.07462 0.00315 -0.00305 0.00928 AFIX 43 H26A 2 0.596031 1.221984 0.773894 11.00000 -1.20000 AFIX 0 C27 1 0.546524 1.126420 0.822349 11.00000 0.04250 0.03888 = 0.07253 -0.00746 0.01349 0.01115 AFIX 43 H27A 2 0.488785 1.152128 0.849119 11.00000 -1.20000 AFIX 0 C28 1 0.563784 1.049052 0.828849 11.00000 0.04110 0.03309 = 0.05664 0.00276 0.01325 0.00614 AFIX 43 H28A 2 0.517541 1.021560 0.859319 11.00000 -1.20000 AFIX 0 C29 1 0.651678 1.010110 0.789534 11.00000 0.02798 0.02693 = 0.03588 0.00121 0.00412 0.00268 C30 1 0.674164 0.930003 0.794982 11.00000 0.03264 0.02741 = 0.02964 0.00445 0.00544 -0.00175 C31 1 0.603188 0.886806 0.844190 11.00000 0.05239 0.03047 = 0.04027 0.00707 0.02614 0.00607 C32 1 0.662142 0.876069 0.903121 11.00000 0.06518 0.06110 = 0.03944 0.01555 0.02304 0.01136 C33 1 0.785959 0.904053 0.917631 11.00000 0.06460 0.11329 = 0.04478 0.02913 0.01419 0.01339 AFIX 43 H33A 2 0.835169 0.928736 0.886680 11.00000 -1.20000 AFIX 0 C34 1 0.835842 0.896433 0.974631 11.00000 0.08350 0.19662 = 0.04004 0.02948 0.00768 0.00512 AFIX 43 H34A 2 0.918089 0.916828 0.984170 11.00000 -1.20000 AFIX 0 C35 1 0.762245 0.857014 1.020335 11.00000 0.12184 0.20068 = 0.04090 0.04782 0.02091 0.03322 AFIX 43 H35A 2 0.797349 0.850750 1.060277 11.00000 -1.20000 AFIX 0 C36 1 0.645388 0.828768 1.008310 11.00000 0.09777 0.13738 = 0.05105 0.04509 0.03530 0.01455 AFIX 43 H36A 2 0.599472 0.801907 1.039252 11.00000 -1.20000 AFIX 0 C37 1 0.591448 0.838688 0.950808 11.00000 0.07712 0.07322 = 0.05211 0.02238 0.03417 0.01122 C38 1 0.467687 0.812970 0.937465 11.00000 0.09723 0.05613 = 0.07007 0.02885 0.05175 0.01332 AFIX 43 H38A 2 0.421355 0.786706 0.968593 11.00000 -1.20000 AFIX 0 C39 1 0.409349 0.823760 0.881420 11.00000 0.05627 0.04380 = 0.08413 0.00625 0.04079 0.00263 AFIX 43 H39A 2 0.324485 0.805880 0.874138 11.00000 -1.20000 AFIX 0 C40 1 0.479534 0.862419 0.834655 11.00000 0.05713 0.03132 = 0.05536 0.00326 0.02663 0.00119 C41 1 0.290895 0.870877 0.771788 11.00000 0.04677 0.08063 = 0.09177 0.00475 0.02331 0.01182 AFIX 137 H41A 2 0.265885 0.887603 0.730540 11.00000 -1.50000 H41B 2 0.248466 0.903255 0.802445 11.00000 -1.50000 H41C 2 0.264931 0.817441 0.777822 11.00000 -1.50000 AFIX 0 C42 1 0.630387 0.666531 0.846233 11.00000 0.05205 0.04318 = 0.05241 0.00824 0.00366 -0.01419 AFIX 23 H42A 2 0.570171 0.686817 0.877436 11.00000 -1.20000 H42B 2 0.588219 0.653690 0.806817 11.00000 -1.20000 AFIX 0 C43 1 0.724282 0.614255 0.867456 11.00000 0.05388 0.03654 = 0.08297 0.03029 0.00508 -0.00686 C44 1 0.799256 0.638961 0.915875 11.00000 0.07101 0.10449 = 0.08068 0.07579 -0.01636 -0.02368 AFIX 23 H44A 2 0.877880 0.608945 0.924596 11.00000 -1.20000 H44B 2 0.753222 0.655962 0.953240 11.00000 -1.20000 AFIX 0 C45 1 0.753406 0.544732 0.828263 11.00000 0.11713 0.03644 = 0.21994 0.00011 0.05616 -0.00570 AFIX 137 H45A 2 0.691533 0.504024 0.837540 11.00000 -1.50000 H45B 2 0.840581 0.526591 0.837109 11.00000 -1.50000 H45C 2 0.746949 0.558595 0.784778 11.00000 -1.50000 HKLF 4 REM ljh146 in P2(1)2(1)2(1) REM R1 = 0.0385 for 7461 Fo > 4sig(Fo) and 0.0455 for all 8320 data REM 463 parameters refined using 24 restraints END WGHT 0.0493 0.1841 REM Highest difference peak 0.380, deepest hole -0.538, 1-sigma level 0.067 Q1 1 0.8043 0.6949 0.8009 11.00000 0.05 0.38 Q2 1 0.8729 0.3985 0.8890 11.00000 0.05 0.37 Q3 1 0.8360 0.6784 0.8266 11.00000 0.05 0.36 Q4 1 0.7411 0.7797 0.8386 11.00000 0.05 0.35 Q5 1 0.4229 0.5607 0.4613 11.00000 0.05 0.31 ; #===END