# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 22-1-05 _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordination (UMR 7177 CNRS), Universite Louis Pasteur, 4 rue Blaise Pascal, F-67070 Strasbourg Cedex, FRANCE ; _publ_contact_author_phone '+33 (0)3 90 24 13 08' _publ_contact_author_fax '+33 (0)3 90 24 13 22' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_requested_category FM _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; _publ_section_title ; Structurally Characterized Intermediates in the Stepwise Insertion of CO/Ethylene or CO/Methyl Acrylate into the Metal-Carbon Bond of Pd(II) Complexes Stabilised by (Phosphinomethyl)Oxazoline Ligands ; loop_ _publ_author_name _publ_author_address 'Magno Agostinho' ; Laboratoire de Chimie de Coordination UMR CNRS 7177 Universite Louis Pasteur 4 rue Blaise Pascal 67070 Strasbourg Cedex France ; P.Braunstein ; Laboratoire de Chimie de Coordination UMR CNRS 7177 Universite Louis Pasteur 4 rue Blaise Pascal 67070 Strasbourg Cedex France ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_compound_2a _database_code_depnum_ccdc_archive 'CCDC 622170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 Cl N O P Pd' _chemical_formula_sum 'C17 H19 Cl N O P Pd' _chemical_formula_weight 426.15 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5550(4) _cell_length_b 8.8270(5) _cell_length_c 22.6280(9) _cell_angle_alpha 82.744(4) _cell_angle_beta 83.051(4) _cell_angle_gamma 86.4320(16) _cell_volume 1680.70(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2108 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8059 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6429 _reflns_number_gt 4199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^2^+50.0000P] 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_number_reflns 6429 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2694 _refine_ls_wR_factor_gt 0.2505 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 Pd1 Pd 0.44031(13) 0.47446(12) 0.10033(5) 0.0306(3) Uani 1 1 d . . . Pd2 Pd 0.49983(12) 0.57848(12) 0.40350(5) 0.0293(3) Uani 1 1 d . . . Cl1 Cl 0.3147(5) 0.7206(4) 0.07903(18) 0.0474(10) Uani 1 1 d . . . Cl2 Cl 0.2563(4) 0.7115(5) 0.42972(18) 0.0433(9) Uani 1 1 d . . . P1 P 0.5365(4) 0.2368(4) 0.11846(15) 0.0255(7) Uani 1 1 d . . . P2 P 0.7400(4) 0.4736(4) 0.38074(16) 0.0262(7) Uani 1 1 d . . . O1 O 0.2698(12) 0.1773(12) -0.0070(5) 0.043(3) Uani 1 1 d . . . O2 O 0.8320(12) 0.7309(12) 0.5033(5) 0.039(2) Uani 1 1 d . . . N1 N 0.3149(13) 0.3751(14) 0.0419(6) 0.036(3) Uani 1 1 d . . . N2 N 0.6165(13) 0.6898(13) 0.4608(5) 0.033(3) Uani 1 1 d . . . C1 C 0.1813(18) 0.432(2) 0.0084(9) 0.051(5) Uani 1 1 d . . . H1A H 0.2081 0.5253 -0.0192 0.062 Uiso 1 1 calc . . . H1B H 0.0867 0.4556 0.0361 0.062 Uiso 1 1 calc . . . C2 C 0.154(2) 0.303(2) -0.0258(8) 0.052(4) Uani 1 1 d . . . H2A H 0.0444 0.2695 -0.0155 0.063 Uiso 1 1 calc . . . H2B H 0.1720 0.3346 -0.0695 0.063 Uiso 1 1 calc . . . C3 C 0.3504(16) 0.2366(17) 0.0306(6) 0.031(3) Uani 1 1 d . . . C4 C 0.4789(15) 0.1429(16) 0.0565(6) 0.029(3) Uani 1 1 d . . . H4A H 0.5701 0.1335 0.0255 0.035 Uiso 1 1 calc . . . H4B H 0.4434 0.0391 0.0717 0.035 Uiso 1 1 calc . . . C5 C 0.4434(15) 0.1305(16) 0.1859(6) 0.028(3) Uani 1 1 d . . . C6 C 0.3589(18) 0.2036(18) 0.2310(7) 0.039(3) Uani 1 1 d . . . H6 H 0.3501 0.3121 0.2269 0.046 Uiso 1 1 calc . . . C7 C 0.288(2) 0.122(2) 0.2813(7) 0.051(5) Uani 1 1 d . . . H7 H 0.2308 0.1754 0.3116 0.062 Uiso 1 1 calc . . . C8 C 0.2981(19) -0.0365(19) 0.2893(8) 0.046(4) Uani 1 1 d . . . H8 H 0.2500 -0.0927 0.3247 0.055 Uiso 1 1 calc . . . C9 C 0.382(2) -0.1105(19) 0.2432(8) 0.048(4) Uani 1 1 d . . . H9 H 0.3869 -0.2191 0.2466 0.058 Uiso 1 1 calc . . . C10 C 0.4550(17) -0.0318(17) 0.1946(7) 0.039(4) Uani 1 1 d . . . H10 H 0.5160 -0.0853 0.1653 0.047 Uiso 1 1 calc . . . C11 C 0.7447(15) 0.1812(16) 0.1222(7) 0.031(3) Uani 1 1 d . . . C12 C 0.8314(17) 0.0897(19) 0.0856(7) 0.042(4) Uani 1 1 d . . . H12 H 0.7845 0.0583 0.0535 0.050 Uiso 1 1 calc . . . C13 C 0.9882(17) 0.0390(19) 0.0930(9) 0.049(4) Uani 1 1 d . . . H13 H 1.0457 -0.0269 0.0672 0.059 Uiso 1 1 calc . . . C14 C 1.0527(17) 0.087(2) 0.1379(9) 0.051(5) Uani 1 1 d . . . H14 H 1.1600 0.0599 0.1426 0.061 Uiso 1 1 calc . . . C15 C 0.968(2) 0.175(3) 0.1771(12) 0.090(8) Uani 1 1 d . . . H15 H 1.0149 0.2042 0.2096 0.108 Uiso 1 1 calc . . . C16 C 0.813(2) 0.223(3) 0.1697(10) 0.071(6) Uani 1 1 d . . . H16 H 0.7541 0.2837 0.1972 0.086 Uiso 1 1 calc . . . C17 C 0.565(2) 0.5583(16) 0.1605(7) 0.043(4) Uani 1 1 d . . . H17A H 0.5004 0.6389 0.1793 0.064 Uiso 1 1 calc . . . H17B H 0.6621 0.6005 0.1394 0.064 Uiso 1 1 calc . . . H17C H 0.5903 0.4754 0.1914 0.064 Uiso 1 1 calc . . . C18 C 0.5670(19) 0.8196(18) 0.4948(7) 0.041(4) Uani 1 1 d . . . H18A H 0.4746 0.7949 0.5245 0.049 Uiso 1 1 calc . . . H18B H 0.5399 0.9118 0.4676 0.049 Uiso 1 1 calc . . . C19 C 0.710(2) 0.8437(19) 0.5258(7) 0.045(4) Uani 1 1 d . . . H19A H 0.7453 0.9493 0.5150 0.054 Uiso 1 1 calc . . . H19B H 0.6858 0.8241 0.5699 0.054 Uiso 1 1 calc . . . C20 C 0.7611(16) 0.6522(15) 0.4678(6) 0.028(3) Uani 1 1 d . . . C21 C 0.8539(16) 0.5284(15) 0.4386(6) 0.031(3) Uani 1 1 d . . . H21A H 0.8718 0.4393 0.4686 0.037 Uiso 1 1 calc . . . H21B H 0.9577 0.5649 0.4199 0.037 Uiso 1 1 calc . . . C22 C 0.7838(16) 0.2720(16) 0.3778(6) 0.031(3) Uani 1 1 d . . . C23 C 0.8968(17) 0.1892(17) 0.4097(7) 0.038(3) Uani 1 1 d . . . H23 H 0.9482 0.2367 0.4370 0.046 Uiso 1 1 calc . . . C24 C 0.9343(19) 0.0368(18) 0.4018(8) 0.044(4) Uani 1 1 d . . . H24 H 1.0091 -0.0195 0.4247 0.053 Uiso 1 1 calc . . . C25 C 0.8657(19) -0.0341(17) 0.3614(8) 0.044(4) Uani 1 1 d . . . H25 H 0.8965 -0.1362 0.3545 0.053 Uiso 1 1 calc . . . C26 C 0.750(3) 0.048(2) 0.3308(10) 0.068(6) Uani 1 1 d . . . H26 H 0.6958 0.0005 0.3043 0.082 Uiso 1 1 calc . . . C27 C 0.713(3) 0.1994(19) 0.3391(10) 0.067(6) Uani 1 1 d . . . H27 H 0.6353 0.2548 0.3170 0.080 Uiso 1 1 calc . . . C28 C 0.8405(15) 0.5578(15) 0.3101(6) 0.027(3) Uani 1 1 d . . . C29 C 0.7651(15) 0.6793(16) 0.2762(7) 0.031(3) Uani 1 1 d . . . H29 H 0.6614 0.7153 0.2894 0.038 Uiso 1 1 calc . . . C30 C 0.8453(17) 0.7456(17) 0.2231(7) 0.038(3) Uani 1 1 d . . . H30 H 0.7955 0.8285 0.2003 0.046 Uiso 1 1 calc . . . C31 C 0.9905(19) 0.6960(18) 0.2032(7) 0.041(4) Uani 1 1 d . . . H31 H 1.0425 0.7420 0.1665 0.049 Uiso 1 1 calc . . . C32 C 1.0653(19) 0.575(2) 0.2373(9) 0.061(5) Uani 1 1 d . . . H32 H 1.1692 0.5404 0.2235 0.073 Uiso 1 1 calc . . . C33 C 0.9924(19) 0.5070(19) 0.2892(8) 0.054(5) Uani 1 1 d . . . H33 H 1.0444 0.4246 0.3115 0.065 Uiso 1 1 calc . . . C34 C 0.3928(16) 0.4717(16) 0.3428(6) 0.031(3) Uani 1 1 d . . . H34A H 0.2937 0.5278 0.3346 0.047 Uiso 1 1 calc . . . H34B H 0.3711 0.3664 0.3599 0.047 Uiso 1 1 calc . . . H34C H 0.4633 0.4707 0.3053 0.047 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0336(6) 0.0293(6) 0.0271(7) -0.0026(4) 0.0007(4) 0.0027(4) Pd2 0.0280(5) 0.0327(6) 0.0262(6) -0.0011(4) -0.0030(4) 0.0004(4) Cl1 0.059(2) 0.0351(19) 0.039(2) 0.0039(16) 0.0112(18) 0.0134(17) Cl2 0.0350(18) 0.053(2) 0.036(2) 0.0058(17) 0.0021(15) 0.0103(16) P1 0.0259(16) 0.0291(17) 0.022(2) -0.0062(14) -0.0038(13) 0.0022(13) P2 0.0256(16) 0.0282(17) 0.024(2) -0.0053(14) -0.0015(13) 0.0035(13) O1 0.043(6) 0.052(7) 0.037(7) -0.005(5) -0.014(5) -0.011(5) O2 0.040(6) 0.045(6) 0.035(6) -0.021(5) -0.004(4) 0.001(5) N1 0.026(6) 0.035(7) 0.048(8) -0.003(6) -0.011(5) 0.003(5) N2 0.032(6) 0.030(6) 0.038(8) -0.016(5) 0.001(5) 0.003(5) C1 0.031(8) 0.051(10) 0.076(14) -0.006(9) -0.027(8) 0.010(7) C2 0.052(10) 0.052(10) 0.053(12) 0.009(9) -0.027(8) -0.005(8) C3 0.033(7) 0.040(8) 0.022(8) 0.000(6) -0.009(6) -0.002(6) C4 0.029(7) 0.038(7) 0.022(8) -0.012(6) 0.000(5) 0.000(6) C5 0.024(6) 0.036(7) 0.027(8) -0.001(6) -0.008(5) -0.005(5) C6 0.040(8) 0.045(9) 0.031(9) -0.007(7) -0.004(6) -0.005(7) C7 0.054(10) 0.072(12) 0.030(10) -0.011(8) 0.005(7) -0.025(9) C8 0.042(9) 0.051(10) 0.039(11) 0.016(8) -0.004(7) -0.001(7) C9 0.049(9) 0.045(9) 0.048(11) 0.009(8) -0.010(8) 0.004(8) C10 0.036(8) 0.032(8) 0.046(10) -0.002(7) 0.003(7) 0.004(6) C11 0.023(6) 0.034(7) 0.037(9) 0.003(6) -0.011(6) 0.001(5) C12 0.034(8) 0.049(9) 0.042(10) -0.009(7) -0.009(6) 0.012(7) C13 0.025(7) 0.051(10) 0.065(13) 0.002(9) 0.001(7) 0.012(7) C14 0.022(7) 0.048(10) 0.081(14) 0.007(9) -0.015(8) 0.001(7) C15 0.049(12) 0.12(2) 0.12(2) -0.057(17) -0.043(13) 0.021(12) C16 0.041(10) 0.102(16) 0.084(16) -0.054(13) -0.026(10) 0.020(10) C17 0.074(11) 0.032(8) 0.029(9) 0.006(7) -0.036(8) -0.017(8) C18 0.048(9) 0.040(8) 0.037(10) -0.018(7) 0.001(7) 0.006(7) C19 0.051(9) 0.049(9) 0.038(10) -0.018(8) -0.001(7) 0.001(8) C20 0.036(7) 0.030(7) 0.019(8) 0.007(6) -0.012(5) -0.002(6) C21 0.037(7) 0.029(7) 0.028(8) -0.001(6) -0.019(6) 0.006(6) C22 0.037(7) 0.034(7) 0.022(8) -0.006(6) -0.006(6) 0.005(6) C23 0.031(7) 0.038(8) 0.047(10) -0.014(7) -0.006(6) -0.002(6) C24 0.044(9) 0.041(9) 0.044(11) 0.005(7) -0.010(7) 0.014(7) C25 0.049(9) 0.027(7) 0.059(11) -0.017(7) 0.000(8) -0.002(7) C26 0.088(15) 0.046(10) 0.083(16) -0.025(10) -0.046(12) 0.011(10) C27 0.090(15) 0.032(9) 0.089(16) -0.013(9) -0.061(13) 0.021(9) C28 0.028(6) 0.029(7) 0.023(8) 0.001(6) -0.005(5) 0.006(5) C29 0.022(6) 0.032(7) 0.040(9) -0.002(6) -0.007(6) 0.003(5) C30 0.039(8) 0.043(8) 0.027(9) 0.007(7) 0.003(6) 0.010(7) C31 0.052(9) 0.044(9) 0.020(9) 0.006(7) 0.011(6) 0.002(7) C32 0.035(9) 0.067(12) 0.067(14) 0.015(10) 0.015(8) 0.016(8) C33 0.040(9) 0.049(10) 0.059(12) 0.013(8) 0.015(8) 0.026(7) C34 0.030(7) 0.041(8) 0.028(8) -0.012(6) -0.013(6) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 2.057(13) . y Pd1 N1 2.103(12) . y Pd1 P1 2.212(4) . y Pd1 Cl1 2.383(4) . y Pd2 C34 2.087(12) . y Pd2 N2 2.098(11) . y Pd2 P2 2.230(3) . y Pd2 Cl2 2.376(4) . y P1 C5 1.811(14) . ? P1 C11 1.827(13) . ? P1 C4 1.847(13) . y P2 C22 1.803(14) . ? P2 C28 1.816(14) . ? P2 C21 1.851(13) . y O1 C3 1.332(16) . ? O1 C2 1.50(2) . ? O2 C20 1.345(16) . ? O2 C19 1.487(19) . ? N1 C3 1.291(18) . y N1 C1 1.475(18) . ? N2 C20 1.284(17) . y N2 C18 1.471(17) . ? C1 C2 1.50(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.468(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.38(2) . ? C5 C10 1.42(2) . ? C6 C7 1.36(2) . ? C6 H6 0.9500 . ? C7 C8 1.39(2) . ? C7 H7 0.9500 . ? C8 C9 1.40(2) . ? C8 H8 0.9500 . ? C9 C10 1.33(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.35(2) . ? C11 C16 1.38(2) . ? C12 C13 1.41(2) . ? C12 H12 0.9500 . ? C13 C14 1.34(3) . ? C13 H13 0.9500 . ? C14 C15 1.37(3) . ? C14 H14 0.9500 . ? C15 C16 1.39(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.52(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.49(2) . y C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.37(2) . ? C22 C23 1.39(2) . ? C23 C24 1.39(2) . ? C23 H23 0.9500 . ? C24 C25 1.38(2) . ? C24 H24 0.9500 . ? C25 C26 1.39(3) . ? C25 H25 0.9500 . ? C26 C27 1.38(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.395(19) . ? C28 C29 1.407(19) . ? C29 C30 1.39(2) . ? C29 H29 0.9500 . ? C30 C31 1.34(2) . ? C30 H30 0.9500 . ? C31 C32 1.40(2) . ? C31 H31 0.9500 . ? C32 C33 1.35(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 176.4(5) . . y C17 Pd1 P1 94.5(4) . . y N1 Pd1 P1 82.2(3) . . y C17 Pd1 Cl1 90.1(5) . . y N1 Pd1 Cl1 93.2(3) . . y P1 Pd1 Cl1 174.66(15) . . y C34 Pd2 N2 176.9(5) . . y C34 Pd2 P2 95.3(4) . . y N2 Pd2 P2 82.8(3) . . y C34 Pd2 Cl2 89.5(4) . . y N2 Pd2 Cl2 92.3(3) . . y P2 Pd2 Cl2 174.38(14) . . y C5 P1 C11 102.1(6) . . ? C5 P1 C4 104.7(6) . . ? C11 P1 C4 105.4(6) . . ? C5 P1 Pd1 114.4(5) . . ? C11 P1 Pd1 125.1(5) . . ? C4 P1 Pd1 103.4(5) . . ? C22 P2 C28 102.3(6) . . ? C22 P2 C21 106.1(6) . . ? C28 P2 C21 104.7(6) . . ? C22 P2 Pd2 124.6(5) . . ? C28 P2 Pd2 113.8(4) . . ? C21 P2 Pd2 103.5(5) . . ? C3 O1 C2 104.4(12) . . ? C20 O2 C19 105.7(11) . . ? C3 N1 C1 107.2(12) . . ? C3 N1 Pd1 120.2(9) . . ? C1 N1 Pd1 132.6(10) . . ? C20 N2 C18 108.1(12) . . ? C20 N2 Pd2 120.0(9) . . ? C18 N2 Pd2 131.7(10) . . ? N1 C1 C2 104.3(13) . . ? N1 C1 H1A 110.9 . . ? C2 C1 H1A 110.9 . . ? N1 C1 H1B 110.9 . . ? C2 C1 H1B 110.9 . . ? H1A C1 H1B 108.9 . . ? O1 C2 C1 105.2(12) . . ? O1 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N1 C3 O1 118.8(13) . . ? N1 C3 C4 122.6(12) . . ? O1 C3 C4 118.6(13) . . ? C3 C4 P1 108.1(9) . . ? C3 C4 H4A 110.1 . . ? P1 C4 H4A 110.1 . . ? C3 C4 H4B 110.1 . . ? P1 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C6 C5 C10 117.2(13) . . ? C6 C5 P1 121.6(11) . . ? C10 C5 P1 121.2(11) . . ? C7 C6 C5 121.0(15) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 121.6(16) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C9 117.4(15) . . ? C7 C8 H8 121.3 . . ? C9 C8 H8 121.3 . . ? C10 C9 C8 121.3(15) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C5 121.4(15) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? C12 C11 C16 117.9(14) . . ? C12 C11 P1 124.7(11) . . ? C16 C11 P1 117.0(12) . . ? C11 C12 C13 123.0(15) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 117.3(16) . . ? C14 C13 H13 121.3 . . ? C12 C13 H13 121.3 . . ? C13 C14 C15 121.5(15) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C16 120.5(19) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 119.6(18) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 104.2(12) . . ? N2 C18 H18A 110.9 . . ? C19 C18 H18A 110.9 . . ? N2 C18 H18B 110.9 . . ? C19 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? O2 C19 C18 104.3(11) . . ? O2 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? O2 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? N2 C20 O2 117.6(13) . . ? N2 C20 C21 123.8(12) . . ? O2 C20 C21 118.6(11) . . ? C20 C21 P2 107.7(9) . . ? C20 C21 H21A 110.2 . . ? P2 C21 H21A 110.2 . . ? C20 C21 H21B 110.2 . . ? P2 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? C27 C22 C23 118.1(13) . . ? C27 C22 P2 118.9(11) . . ? C23 C22 P2 122.8(10) . . ? C22 C23 C24 120.0(13) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 121.5(14) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 118.1(14) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C27 C26 C25 120.0(16) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C22 C27 C26 122.2(16) . . ? C22 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C33 C28 C29 119.2(13) . . ? C33 C28 P2 121.5(11) . . ? C29 C28 P2 119.4(10) . . ? C30 C29 C28 118.7(12) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C31 C30 C29 121.8(14) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 119.2(13) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 121.2(14) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C28 119.9(14) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? Pd2 C34 H34A 109.5 . . ? Pd2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Pd2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C5 79.7(7) . . . . ? N1 Pd1 P1 C5 -98.8(6) . . . . ? Cl1 Pd1 P1 C5 -68.4(16) . . . . ? C17 Pd1 P1 C11 -47.1(8) . . . . ? N1 Pd1 P1 C11 134.3(7) . . . . ? Cl1 Pd1 P1 C11 164.8(15) . . . . ? C17 Pd1 P1 C4 -167.1(7) . . . . ? N1 Pd1 P1 C4 14.3(5) . . . . ? Cl1 Pd1 P1 C4 44.8(16) . . . . ? C34 Pd2 P2 C22 -50.4(7) . . . . ? N2 Pd2 P2 C22 132.0(7) . . . . ? Cl2 Pd2 P2 C22 161.5(14) . . . . ? C34 Pd2 P2 C28 75.7(6) . . . . ? N2 Pd2 P2 C28 -101.9(6) . . . . ? Cl2 Pd2 P2 C28 -72.5(15) . . . . ? C34 Pd2 P2 C21 -171.3(6) . . . . ? N2 Pd2 P2 C21 11.1(6) . . . . ? Cl2 Pd2 P2 C21 40.6(16) . . . . ? C17 Pd1 N1 C3 -33(10) . . . . ? P1 Pd1 N1 C3 -10.1(11) . . . . ? Cl1 Pd1 N1 C3 172.6(11) . . . . ? C17 Pd1 N1 C1 146(10) . . . . ? P1 Pd1 N1 C1 168.6(15) . . . . ? Cl1 Pd1 N1 C1 -8.7(14) . . . . ? C34 Pd2 N2 C20 -59(10) . . . . ? P2 Pd2 N2 C20 -7.3(11) . . . . ? Cl2 Pd2 N2 C20 175.5(11) . . . . ? C34 Pd2 N2 C18 116(10) . . . . ? P2 Pd2 N2 C18 168.0(13) . . . . ? Cl2 Pd2 N2 C18 -9.3(13) . . . . ? C3 N1 C1 C2 -2.6(18) . . . . ? Pd1 N1 C1 C2 178.6(11) . . . . ? C3 O1 C2 C1 -1.7(17) . . . . ? N1 C1 C2 O1 2.6(18) . . . . ? C1 N1 C3 O1 1.7(19) . . . . ? Pd1 N1 C3 O1 -179.3(10) . . . . ? C1 N1 C3 C4 180.0(14) . . . . ? Pd1 N1 C3 C4 -1.0(19) . . . . ? C2 O1 C3 N1 0.1(18) . . . . ? C2 O1 C3 C4 -178.3(13) . . . . ? N1 C3 C4 P1 14.2(17) . . . . ? O1 C3 C4 P1 -167.5(10) . . . . ? C5 P1 C4 C3 101.2(10) . . . . ? C11 P1 C4 C3 -151.5(9) . . . . ? Pd1 P1 C4 C3 -18.8(10) . . . . ? C11 P1 C5 C6 118.1(12) . . . . ? C4 P1 C5 C6 -132.3(12) . . . . ? Pd1 P1 C5 C6 -19.8(13) . . . . ? C11 P1 C5 C10 -61.6(12) . . . . ? C4 P1 C5 C10 48.1(13) . . . . ? Pd1 P1 C5 C10 160.5(10) . . . . ? C10 C5 C6 C7 -1(2) . . . . ? P1 C5 C6 C7 179.4(12) . . . . ? C5 C6 C7 C8 0(3) . . . . ? C6 C7 C8 C9 -1(3) . . . . ? C7 C8 C9 C10 3(3) . . . . ? C8 C9 C10 C5 -4(3) . . . . ? C6 C5 C10 C9 3(2) . . . . ? P1 C5 C10 C9 -177.6(13) . . . . ? C5 P1 C11 C12 109.2(14) . . . . ? C4 P1 C11 C12 0.0(15) . . . . ? Pd1 P1 C11 C12 -119.0(13) . . . . ? C5 P1 C11 C16 -63.8(16) . . . . ? C4 P1 C11 C16 -172.9(15) . . . . ? Pd1 P1 C11 C16 68.0(16) . . . . ? C16 C11 C12 C13 -2(3) . . . . ? P1 C11 C12 C13 -174.6(13) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C12 C13 C14 C15 4(3) . . . . ? C13 C14 C15 C16 -3(4) . . . . ? C12 C11 C16 C15 2(3) . . . . ? P1 C11 C16 C15 176(2) . . . . ? C14 C15 C16 C11 0(4) . . . . ? C20 N2 C18 C19 -3.1(17) . . . . ? Pd2 N2 C18 C19 -178.7(10) . . . . ? C20 O2 C19 C18 -2.8(15) . . . . ? N2 C18 C19 O2 3.5(16) . . . . ? C18 N2 C20 O2 1.4(18) . . . . ? Pd2 N2 C20 O2 177.7(9) . . . . ? C18 N2 C20 C21 -178.1(13) . . . . ? Pd2 N2 C20 C21 -1.8(19) . . . . ? C19 O2 C20 N2 1.0(17) . . . . ? C19 O2 C20 C21 -179.5(12) . . . . ? N2 C20 C21 P2 11.9(17) . . . . ? O2 C20 C21 P2 -167.6(10) . . . . ? C22 P2 C21 C20 -147.5(9) . . . . ? C28 P2 C21 C20 104.8(10) . . . . ? Pd2 P2 C21 C20 -14.7(10) . . . . ? C28 P2 C22 C27 -71.6(16) . . . . ? C21 P2 C22 C27 178.9(16) . . . . ? Pd2 P2 C22 C27 59.2(17) . . . . ? C28 P2 C22 C23 103.0(13) . . . . ? C21 P2 C22 C23 -6.5(14) . . . . ? Pd2 P2 C22 C23 -126.2(11) . . . . ? C27 C22 C23 C24 0(2) . . . . ? P2 C22 C23 C24 -174.7(12) . . . . ? C22 C23 C24 C25 2(2) . . . . ? C23 C24 C25 C26 -4(3) . . . . ? C24 C25 C26 C27 4(3) . . . . ? C23 C22 C27 C26 0(3) . . . . ? P2 C22 C27 C26 174.8(19) . . . . ? C25 C26 C27 C22 -2(4) . . . . ? C22 P2 C28 C33 -43.5(15) . . . . ? C21 P2 C28 C33 67.0(15) . . . . ? Pd2 P2 C28 C33 179.4(12) . . . . ? C22 P2 C28 C29 137.9(11) . . . . ? C21 P2 C28 C29 -111.5(11) . . . . ? Pd2 P2 C28 C29 0.8(12) . . . . ? C33 C28 C29 C30 0(2) . . . . ? P2 C28 C29 C30 178.1(11) . . . . ? C28 C29 C30 C31 1(2) . . . . ? C29 C30 C31 C32 -1(3) . . . . ? C30 C31 C32 C33 1(3) . . . . ? C31 C32 C33 C28 -1(3) . . . . ? C29 C28 C33 C32 0(3) . . . . ? P2 C28 C33 C32 -178.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.836 _refine_diff_density_max 2.790 _refine_diff_density_min -2.706 _refine_diff_density_rms 0.235 # start Validation Reply Form #_vrf_REFLT03_shelxl #; #PROBLEM: Reflection count < 85% complete (theta max?) #RESPONSE: due to the low crystal quality #; #_vrf_PLAT022_shelxl #; #PROBLEM: Ratio Unique / Expected Reflections too Low .... 0.84 #RESPONSE: due to the low crystal quality #; #_vrf_PLAT029_shelxl #; #PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.84 #RESPONSE: due to the low crystal quality #; # end Validation Reply Form # Attachment '2b.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 622171' _audit_creation_date 22-1-05 _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 Cl N O P Pd' _chemical_formula_sum 'C19 H23 Cl N O P Pd' _chemical_formula_weight 454.20 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.7310(10) _cell_length_b 11.711(2) _cell_length_c 21.589(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1954.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10443 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 5650 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5650 _reflns_number_gt 4464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+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 -0.04(4) _refine_ls_number_reflns 5650 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _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 Pd1 Pd 0.99849(4) 0.51105(2) 0.735163(11) 0.02640(10) Uani 1 1 d . . . Cl1 Cl 1.08628(15) 0.46234(10) 0.83737(4) 0.0381(2) Uani 1 1 d . . . P1 P 0.91681(13) 0.55340(9) 0.64089(4) 0.0254(2) Uani 1 1 d . . . O1 O 0.5224(4) 0.6894(3) 0.72478(13) 0.0375(7) Uani 1 1 d . . . N1 N 0.7581(4) 0.5966(3) 0.75867(15) 0.0277(7) Uani 1 1 d . . . C18 C 0.7173(7) 0.6334(6) 0.8706(2) 0.0610(17) Uani 1 1 d . . . H18A H 0.8197 0.5877 0.8807 0.091 Uiso 1 1 calc . . . H18B H 0.6337 0.6285 0.9046 0.091 Uiso 1 1 calc . . . H18C H 0.7515 0.7132 0.8645 0.091 Uiso 1 1 calc . . . C19 C 0.5856(7) 0.4643(5) 0.8188(3) 0.0594(16) Uani 1 1 d . . . H19A H 0.5462 0.4340 0.7789 0.089 Uiso 1 1 calc . . . H19B H 0.4921 0.4579 0.8493 0.089 Uiso 1 1 calc . . . H19C H 0.6861 0.4206 0.8331 0.089 Uiso 1 1 calc . . . C1 C 0.6352(5) 0.5880(4) 0.8114(2) 0.0366(10) Uani 1 1 d . . . C2 C 0.4859(6) 0.6638(4) 0.78947(19) 0.0399(9) Uani 1 1 d . . . H2A H 0.3741 0.6232 0.7935 0.048 Uiso 1 1 calc . . . H2B H 0.4806 0.7350 0.8142 0.048 Uiso 1 1 calc . . . C3 C 0.6828(5) 0.6501(3) 0.71466(18) 0.0267(8) Uani 1 1 d . . . C4 C 0.7621(5) 0.6701(4) 0.65298(18) 0.0303(9) Uani 1 1 d . . . H4A H 0.8221 0.7448 0.6521 0.036 Uiso 1 1 calc . . . H4B H 0.6725 0.6696 0.6202 0.036 Uiso 1 1 calc . . . C17 C 1.2185(5) 0.4375(5) 0.7005(2) 0.0411(11) Uani 1 1 d . . . H17A H 1.1938 0.4042 0.6597 0.062 Uiso 1 1 calc . . . H17B H 1.2580 0.3774 0.7287 0.062 Uiso 1 1 calc . . . H17C H 1.3089 0.4956 0.6963 0.062 Uiso 1 1 calc . . . C5 C 0.7982(5) 0.4429(4) 0.60009(17) 0.0295(8) Uani 1 1 d . . . C6 C 0.8312(6) 0.3290(4) 0.6138(2) 0.0331(9) Uani 1 1 d . . . H6 H 0.9085 0.3099 0.6464 0.040 Uiso 1 1 calc . . . C7 C 0.7510(6) 0.2427(4) 0.5797(2) 0.0452(12) Uani 1 1 d . . . H7 H 0.7763 0.1650 0.5884 0.054 Uiso 1 1 calc . . . C8 C 0.6344(7) 0.2703(5) 0.5332(2) 0.0463(12) Uani 1 1 d . . . H8 H 0.5783 0.2116 0.5104 0.056 Uiso 1 1 calc . . . C9 C 0.6002(6) 0.3835(5) 0.5202(2) 0.0481(12) Uani 1 1 d . . . H9 H 0.5202 0.4023 0.4884 0.058 Uiso 1 1 calc . . . C10 C 0.6809(6) 0.4693(4) 0.5528(2) 0.0404(10) Uani 1 1 d . . . H10 H 0.6569 0.5469 0.5432 0.049 Uiso 1 1 calc . . . C11 C 1.0748(5) 0.6052(3) 0.58544(17) 0.0276(8) Uani 1 1 d . . . C16 C 1.0941(5) 0.5573(4) 0.52650(18) 0.0332(9) Uani 1 1 d . . . H16 H 1.0192 0.4976 0.5135 0.040 Uiso 1 1 calc . . . C15 C 1.2228(6) 0.5968(5) 0.48694(19) 0.0415(11) Uani 1 1 d . . . H15 H 1.2370 0.5634 0.4472 0.050 Uiso 1 1 calc . . . C14 C 1.3295(6) 0.6843(5) 0.5055(2) 0.0403(11) Uani 1 1 d . . . H14 H 1.4161 0.7119 0.4781 0.048 Uiso 1 1 calc . . . C13 C 1.3122(6) 0.7330(4) 0.5639(2) 0.0413(11) Uani 1 1 d . . . H13 H 1.3858 0.7938 0.5762 0.050 Uiso 1 1 calc . . . C12 C 1.1857(6) 0.6917(4) 0.6044(2) 0.0373(10) Uani 1 1 d . . . H12 H 1.1756 0.7228 0.6449 0.045 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02740(16) 0.03013(16) 0.02168(13) 0.00252(9) -0.00133(12) 0.00305(16) Cl1 0.0437(5) 0.0433(6) 0.0274(4) 0.0064(4) -0.0068(4) 0.0041(5) P1 0.0281(4) 0.0275(5) 0.0207(4) 0.0011(4) 0.0007(4) 0.0013(4) O1 0.0324(15) 0.0456(17) 0.0346(14) 0.0061(12) 0.0049(13) 0.0113(14) N1 0.0298(16) 0.0299(18) 0.0235(15) 0.0020(13) 0.0053(13) 0.0021(14) C18 0.062(3) 0.090(5) 0.031(2) -0.008(3) 0.000(2) 0.030(3) C19 0.036(2) 0.058(4) 0.084(4) 0.036(3) 0.010(3) 0.003(3) C1 0.033(2) 0.047(3) 0.031(2) 0.0089(18) 0.0074(16) 0.0037(19) C2 0.035(2) 0.051(3) 0.033(2) 0.0076(18) 0.010(2) 0.007(2) C3 0.0295(19) 0.0232(19) 0.0274(18) -0.0010(15) -0.0002(16) -0.0012(16) C4 0.034(2) 0.031(2) 0.0264(19) 0.0016(16) 0.0025(16) 0.0042(18) C17 0.034(2) 0.057(3) 0.033(2) 0.000(2) 0.0011(17) 0.018(2) C5 0.032(2) 0.031(2) 0.0257(18) 0.0018(16) 0.0045(15) 0.0004(17) C6 0.036(2) 0.031(2) 0.032(2) 0.0014(18) 0.0077(18) -0.0025(18) C7 0.052(3) 0.037(3) 0.047(3) -0.003(2) 0.020(2) -0.013(2) C8 0.048(3) 0.047(3) 0.044(3) -0.011(2) 0.005(2) -0.016(2) C9 0.043(3) 0.061(3) 0.040(2) -0.011(2) -0.006(2) -0.006(3) C10 0.047(2) 0.037(3) 0.037(2) -0.003(2) -0.0066(19) 0.003(2) C11 0.0277(18) 0.027(2) 0.0279(18) 0.0005(15) -0.0004(16) 0.0004(17) C16 0.038(2) 0.035(2) 0.0268(18) -0.0029(17) 0.0051(17) -0.003(2) C15 0.050(3) 0.048(3) 0.026(2) -0.0009(19) 0.0133(19) 0.003(2) C14 0.041(3) 0.043(3) 0.037(2) 0.011(2) 0.010(2) 0.004(2) C13 0.034(2) 0.046(3) 0.044(3) 0.006(2) 0.001(2) -0.006(2) C12 0.038(2) 0.045(3) 0.029(2) -0.0005(19) -0.0048(18) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 2.049(4) . y Pd1 N1 2.171(3) . y Pd1 P1 2.1879(10) . y Pd1 Cl1 2.3780(10) . y P1 C5 1.814(4) . ? P1 C11 1.815(4) . ? P1 C4 1.835(4) . y O1 C3 1.340(5) . ? O1 C2 1.456(5) . ? N1 C3 1.279(5) . y N1 C1 1.486(5) . ? C18 C1 1.523(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C1 1.507(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C1 C2 1.531(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.485(5) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C5 C6 1.390(6) . ? C5 C10 1.399(6) . ? C6 C7 1.395(6) . ? C6 H6 0.9500 . ? C7 C8 1.388(8) . ? C7 H7 0.9500 . ? C8 C9 1.380(8) . ? C8 H8 0.9500 . ? C9 C10 1.377(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.388(6) . ? C11 C16 1.399(5) . ? C16 C15 1.391(6) . ? C16 H16 0.9500 . ? C15 C14 1.375(7) . ? C15 H15 0.9500 . ? C14 C13 1.390(7) . ? C14 H14 0.9500 . ? C13 C12 1.398(7) . ? C13 H13 0.9500 . ? C12 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 171.94(14) . . y C17 Pd1 P1 89.70(13) . . y N1 Pd1 P1 82.29(9) . . y C17 Pd1 Cl1 90.09(13) . . y N1 Pd1 Cl1 97.94(9) . . y P1 Pd1 Cl1 179.21(4) . . y C5 P1 C11 104.99(18) . . ? C5 P1 C4 105.73(19) . . ? C11 P1 C4 106.45(19) . . ? C5 P1 Pd1 115.84(14) . . ? C11 P1 Pd1 119.69(14) . . ? C4 P1 Pd1 102.98(13) . . ? C3 O1 C2 105.4(3) . . ? C3 N1 C1 108.1(3) . . ? C3 N1 Pd1 116.2(3) . . ? C1 N1 Pd1 134.0(3) . . ? C1 C18 H18A 109.5 . . ? C1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C1 C19 108.0(4) . . ? N1 C1 C18 110.6(4) . . ? C19 C1 C18 110.6(5) . . ? N1 C1 C2 101.9(3) . . ? C19 C1 C2 113.5(4) . . ? C18 C1 C2 111.8(4) . . ? O1 C2 C1 105.6(3) . . ? O1 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? O1 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? N1 C3 O1 117.9(4) . . ? N1 C3 C4 123.8(4) . . ? O1 C3 C4 118.3(3) . . ? C3 C4 P1 106.2(3) . . ? C3 C4 H4A 110.5 . . ? P1 C4 H4A 110.5 . . ? C3 C4 H4B 110.5 . . ? P1 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C6 C5 C10 119.1(4) . . ? C6 C5 P1 119.2(3) . . ? C10 C5 P1 121.6(4) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.7(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C5 120.3(5) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C12 C11 C16 119.7(4) . . ? C12 C11 P1 117.7(3) . . ? C16 C11 P1 122.5(3) . . ? C15 C16 C11 120.1(4) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C13 C12 119.5(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C5 86.5(2) . . . . ? N1 Pd1 P1 C5 -94.38(17) . . . . ? Cl1 Pd1 P1 C5 12(3) . . . . ? C17 Pd1 P1 C11 -40.9(2) . . . . ? N1 Pd1 P1 C11 138.26(18) . . . . ? Cl1 Pd1 P1 C11 -115(3) . . . . ? C17 Pd1 P1 C4 -158.7(2) . . . . ? N1 Pd1 P1 C4 20.49(17) . . . . ? Cl1 Pd1 P1 C4 127(3) . . . . ? C17 Pd1 N1 C3 -4.3(14) . . . . ? P1 Pd1 N1 C3 -10.3(3) . . . . ? Cl1 Pd1 N1 C3 170.5(3) . . . . ? C17 Pd1 N1 C1 159.4(12) . . . . ? P1 Pd1 N1 C1 153.3(4) . . . . ? Cl1 Pd1 N1 C1 -25.9(4) . . . . ? C3 N1 C1 C19 112.0(4) . . . . ? Pd1 N1 C1 C19 -52.6(5) . . . . ? C3 N1 C1 C18 -126.8(4) . . . . ? Pd1 N1 C1 C18 68.7(6) . . . . ? C3 N1 C1 C2 -7.8(5) . . . . ? Pd1 N1 C1 C2 -172.3(3) . . . . ? C3 O1 C2 C1 -8.9(4) . . . . ? N1 C1 C2 O1 10.0(4) . . . . ? C19 C1 C2 O1 -105.9(4) . . . . ? C18 C1 C2 O1 128.1(4) . . . . ? C1 N1 C3 O1 2.6(5) . . . . ? Pd1 N1 C3 O1 170.2(3) . . . . ? C1 N1 C3 C4 -176.8(4) . . . . ? Pd1 N1 C3 C4 -9.1(5) . . . . ? C2 O1 C3 N1 4.3(5) . . . . ? C2 O1 C3 C4 -176.3(4) . . . . ? N1 C3 C4 P1 26.9(5) . . . . ? O1 C3 C4 P1 -152.4(3) . . . . ? C5 P1 C4 C3 92.4(3) . . . . ? C11 P1 C4 C3 -156.3(3) . . . . ? Pd1 P1 C4 C3 -29.6(3) . . . . ? C11 P1 C5 C6 104.5(3) . . . . ? C4 P1 C5 C6 -143.1(3) . . . . ? Pd1 P1 C5 C6 -29.8(4) . . . . ? C11 P1 C5 C10 -72.0(4) . . . . ? C4 P1 C5 C10 40.3(4) . . . . ? Pd1 P1 C5 C10 153.6(3) . . . . ? C10 C5 C6 C7 1.4(6) . . . . ? P1 C5 C6 C7 -175.2(3) . . . . ? C5 C6 C7 C8 -1.8(7) . . . . ? C6 C7 C8 C9 1.0(7) . . . . ? C7 C8 C9 C10 0.1(8) . . . . ? C8 C9 C10 C5 -0.4(7) . . . . ? C6 C5 C10 C9 -0.3(6) . . . . ? P1 C5 C10 C9 176.2(4) . . . . ? C5 P1 C11 C12 -179.9(3) . . . . ? C4 P1 C11 C12 68.3(4) . . . . ? Pd1 P1 C11 C12 -47.7(4) . . . . ? C5 P1 C11 C16 -3.5(4) . . . . ? C4 P1 C11 C16 -115.3(4) . . . . ? Pd1 P1 C11 C16 128.7(3) . . . . ? C12 C11 C16 C15 -0.6(7) . . . . ? P1 C11 C16 C15 -176.9(3) . . . . ? C11 C16 C15 C14 -1.0(7) . . . . ? C16 C15 C14 C13 1.0(7) . . . . ? C15 C14 C13 C12 0.5(7) . . . . ? C16 C11 C12 C13 2.1(7) . . . . ? P1 C11 C12 C13 178.6(4) . . . . ? C14 C13 C12 C11 -2.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.954 _refine_diff_density_min -1.864 _refine_diff_density_rms 0.298 data_shelxl_1 _database_code_depnum_ccdc_archive 'CCDC 622172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H19 F3 N O4 P Pd S' _chemical_formula_sum 'C18 H19 F3 N O4 P Pd S' _chemical_formula_weight 539.77 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.4710(2) _cell_length_b 13.1780(2) _cell_length_c 29.3020(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.1200(6) _cell_angle_gamma 90.00 _cell_volume 6447.36(14) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18453 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 33223 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 30.03 _reflns_number_total 18821 _reflns_number_gt 9279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^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_number_reflns 18821 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1742 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1518 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63101(2) 0.44695(3) 0.083432(12) 0.03269(11) Uani 1 1 d . . . Pd2 Pd 0.18990(2) 0.96267(3) 0.081768(12) 0.03120(11) Uani 1 1 d . . . Pd3 Pd 0.46944(2) 0.05039(3) 0.238463(13) 0.03616(12) Uani 1 1 d . . . S1 S 0.67421(7) 0.54160(11) -0.01031(4) 0.0374(3) Uani 1 1 d . . . S2 S 0.14000(8) 1.09062(12) 0.16537(5) 0.0456(4) Uani 1 1 d . . . S3 S 0.50651(7) -0.06948(10) 0.14796(4) 0.0367(3) Uani 1 1 d . . . P1 P 0.60833(7) 0.35104(10) 0.13824(4) 0.0318(3) Uani 1 1 d . . . P2 P 0.20923(7) 0.84387(10) 0.03499(4) 0.0284(3) Uani 1 1 d . . . P3 P 0.44606(8) 0.15864(10) 0.28874(4) 0.0356(3) Uani 1 1 d . . . F1 F 0.81276(19) 0.5908(3) 0.04932(12) 0.0843(12) Uani 1 1 d . . . F2 F 0.80145(18) 0.6219(3) -0.02465(12) 0.0876(13) Uani 1 1 d . . . F3 F 0.7433(2) 0.7178(3) 0.01385(14) 0.0857(12) Uani 1 1 d . . . F4 F 0.0188(3) 1.1914(4) 0.17463(16) 0.142(2) Uani 1 1 d . . . F5 F 0.0087(2) 1.1396(5) 0.10379(18) 0.154(3) Uani 1 1 d . . . F6 F 0.0809(3) 1.2654(4) 0.13178(17) 0.1209(18) Uani 1 1 d . . . F7 F 0.5707(2) -0.2455(3) 0.17655(14) 0.0890(12) Uani 1 1 d . . . F8 F 0.6478(2) -0.1201(3) 0.20434(13) 0.0848(12) Uani 1 1 d . . . F9 F 0.6273(2) -0.1639(3) 0.13199(12) 0.0810(12) Uani 1 1 d . . . O1 O 0.4717(2) 0.2105(3) 0.02267(12) 0.0478(9) Uani 1 1 d . . . O2 O 0.6401(2) 0.5530(3) 0.02924(12) 0.0484(10) Uani 1 1 d . . . O3 O 0.7047(2) 0.4429(3) -0.01458(13) 0.0571(11) Uani 1 1 d . . . O4 O 0.6265(2) 0.5882(3) -0.05319(12) 0.0550(11) Uani 1 1 d . . . O5 O 0.3401(2) 0.7327(3) 0.15981(11) 0.0443(9) Uani 1 1 d . . . O6 O 0.1762(2) 1.0854(3) 0.12712(12) 0.0484(10) Uani 1 1 d . . . O7 O 0.1893(3) 1.1441(4) 0.20573(14) 0.0975(17) Uani 1 1 d . . . O8 O 0.1084(3) 1.0001(4) 0.17636(17) 0.0880(15) Uani 1 1 d . . . O9 O 0.3182(2) 0.2853(3) 0.16597(12) 0.0493(10) Uani 1 1 d . . . O10 O 0.4787(2) -0.0699(3) 0.18958(13) 0.0619(12) Uani 1 1 d . . . O11 O 0.4548(2) -0.1203(3) 0.10800(12) 0.0631(11) Uani 1 1 d . . . O12 O 0.5398(2) 0.0235(3) 0.13827(14) 0.0597(11) Uani 1 1 d . . . N1 N 0.5570(2) 0.3418(3) 0.03471(12) 0.0345(10) Uani 1 1 d . . . N2 N 0.2601(2) 0.8693(3) 0.13757(12) 0.0333(10) Uani 1 1 d . . . N3 N 0.3938(2) 0.1461(3) 0.18493(13) 0.0355(10) Uani 1 1 d . . . C1 C 0.5303(3) 0.3282(5) -0.01775(16) 0.0496(15) Uani 1 1 d . . . H1A H 0.5760 0.3102 -0.0297 0.060 Uiso 1 1 calc . . . H1B H 0.5047 0.3907 -0.0340 0.060 Uiso 1 1 calc . . . C2 C 0.4704(3) 0.2416(5) -0.02556(18) 0.0575(17) Uani 1 1 d . . . H2A H 0.4163 0.2647 -0.0441 0.069 Uiso 1 1 calc . . . H2B H 0.4866 0.1848 -0.0428 0.069 Uiso 1 1 calc . . . C3 C 0.5211(3) 0.2744(4) 0.05231(17) 0.0386(12) Uani 1 1 d . . . C4 C 0.5302(3) 0.2642(4) 0.10380(16) 0.0394(12) Uani 1 1 d . . . H4A H 0.5448 0.1934 0.1140 0.047 Uiso 1 1 calc . . . H4B H 0.4787 0.2801 0.1099 0.047 Uiso 1 1 calc . . . C5 C 0.6877(3) 0.2716(4) 0.17480(16) 0.0378(12) Uani 1 1 d . . . C6 C 0.7670(3) 0.2918(4) 0.17769(17) 0.0441(13) Uani 1 1 d . . . H6 H 0.7804 0.3460 0.1601 0.053 Uiso 1 1 calc . . . C7 C 0.8264(3) 0.2305(5) 0.2071(2) 0.0630(17) Uani 1 1 d . . . H7 H 0.8812 0.2437 0.2101 0.076 Uiso 1 1 calc . . . C8 C 0.8062(4) 0.1517(5) 0.2314(2) 0.0659(18) Uani 1 1 d . . . H8 H 0.8475 0.1112 0.2515 0.079 Uiso 1 1 calc . . . C9 C 0.7281(4) 0.1296(4) 0.22749(19) 0.0586(16) Uani 1 1 d . . . H9 H 0.7151 0.0731 0.2440 0.070 Uiso 1 1 calc . . . C10 C 0.6683(3) 0.1905(4) 0.19921(17) 0.0454(14) Uani 1 1 d . . . H10 H 0.6138 0.1765 0.1966 0.055 Uiso 1 1 calc . . . C11 C 0.5617(3) 0.4132(4) 0.17924(16) 0.0361(12) Uani 1 1 d . . . C12 C 0.5878(3) 0.3986(4) 0.22801(18) 0.0495(15) Uani 1 1 d . . . H12 H 0.6319 0.3556 0.2423 0.059 Uiso 1 1 calc . . . C13 C 0.5466(4) 0.4497(5) 0.2557(2) 0.068(2) Uani 1 1 d . . . H13 H 0.5632 0.4408 0.2894 0.081 Uiso 1 1 calc . . . C14 C 0.4834(4) 0.5116(5) 0.2353(3) 0.070(2) Uani 1 1 d . . . H14 H 0.4569 0.5461 0.2547 0.084 Uiso 1 1 calc . . . C15 C 0.4580(4) 0.5245(5) 0.1867(2) 0.072(2) Uani 1 1 d . . . H15 H 0.4132 0.5665 0.1722 0.087 Uiso 1 1 calc . . . C16 C 0.4983(3) 0.4757(5) 0.15959(19) 0.0539(16) Uani 1 1 d . . . H16 H 0.4816 0.4856 0.1260 0.065 Uiso 1 1 calc . . . C17 C 0.6961(3) 0.5436(4) 0.13385(18) 0.0509(15) Uani 1 1 d . . . H17A H 0.6649 0.6054 0.1340 0.076 Uiso 1 1 calc . . . H17B H 0.7458 0.5611 0.1266 0.076 Uiso 1 1 calc . . . H17C H 0.7089 0.5109 0.1653 0.076 Uiso 1 1 calc . . . C18 C 0.7620(3) 0.6243(5) 0.00789(19) 0.0549(16) Uani 1 1 d . . . C19 C 0.2878(3) 0.8748(4) 0.19035(16) 0.0449(14) Uani 1 1 d . . . H19A H 0.2418 0.8737 0.2037 0.054 Uiso 1 1 calc . . . H19B H 0.3194 0.9371 0.2013 0.054 Uiso 1 1 calc . . . C20 C 0.3397(3) 0.7800(5) 0.20510(17) 0.0508(15) Uani 1 1 d . . . H20A H 0.3946 0.7984 0.2243 0.061 Uiso 1 1 calc . . . H20B H 0.3163 0.7335 0.2240 0.061 Uiso 1 1 calc . . . C21 C 0.2937(3) 0.7906(4) 0.12576(16) 0.0330(11) Uani 1 1 d . . . C22 C 0.2850(3) 0.7619(4) 0.07556(15) 0.0340(11) Uani 1 1 d . . . H22A H 0.2684 0.6900 0.0703 0.041 Uiso 1 1 calc . . . H22B H 0.3371 0.7697 0.0689 0.041 Uiso 1 1 calc . . . C23 C 0.1235(3) 0.7636(4) 0.00965(15) 0.0301(11) Uani 1 1 d . . . C24 C 0.0528(3) 0.7806(4) 0.02093(17) 0.0381(12) Uani 1 1 d . . . H24 H 0.0492 0.8368 0.0405 0.046 Uiso 1 1 calc . . . C25 C -0.0122(3) 0.7178(5) 0.0044(2) 0.0545(16) Uani 1 1 d . . . H25 H -0.0602 0.7307 0.0124 0.065 Uiso 1 1 calc . . . C26 C -0.0074(3) 0.6361(5) -0.0239(2) 0.0598(17) Uani 1 1 d . . . H26 H -0.0521 0.5921 -0.0350 0.072 Uiso 1 1 calc . . . C27 C 0.0616(3) 0.6176(4) -0.03610(18) 0.0496(14) Uani 1 1 d . . . H27 H 0.0640 0.5618 -0.0562 0.060 Uiso 1 1 calc . . . C28 C 0.1278(3) 0.6805(4) -0.01905(17) 0.0422(13) Uani 1 1 d . . . H28 H 0.1759 0.6670 -0.0269 0.051 Uiso 1 1 calc . . . C29 C 0.2501(3) 0.8788(4) -0.01305(17) 0.0375(12) Uani 1 1 d . . . C30 C 0.2047(3) 0.8751(4) -0.06021(17) 0.0492(15) Uani 1 1 d . . . H30 H 0.1512 0.8508 -0.0686 0.059 Uiso 1 1 calc . . . C31 C 0.2377(5) 0.9071(5) -0.0955(2) 0.077(2) Uani 1 1 d . . . H31 H 0.2066 0.9042 -0.1281 0.092 Uiso 1 1 calc . . . C32 C 0.3129(5) 0.9419(6) -0.0841(3) 0.084(3) Uani 1 1 d . . . H32 H 0.3345 0.9628 -0.1087 0.101 Uiso 1 1 calc . . . C33 C 0.3593(4) 0.9481(6) -0.0374(3) 0.088(3) Uani 1 1 d . . . H33 H 0.4124 0.9736 -0.0296 0.106 Uiso 1 1 calc . . . C34 C 0.3273(3) 0.9164(5) -0.0017(2) 0.0603(17) Uani 1 1 d . . . H34 H 0.3587 0.9207 0.0308 0.072 Uiso 1 1 calc . . . C35 C 0.1280(3) 1.0439(4) 0.02442(18) 0.0505(15) Uani 1 1 d . . . H35A H 0.1650 1.0868 0.0136 0.076 Uiso 1 1 calc . . . H35B H 0.0887 1.0867 0.0332 0.076 Uiso 1 1 calc . . . H35C H 0.1003 0.9976 -0.0013 0.076 Uiso 1 1 calc . . . C36 C 0.0572(5) 1.1774(7) 0.1426(3) 0.084(2) Uani 1 1 d . . . C37 C 0.3602(3) 0.1403(4) 0.13217(17) 0.0418(13) Uani 1 1 d . . . H37A H 0.3253 0.0802 0.1224 0.050 Uiso 1 1 calc . . . H37B H 0.4033 0.1378 0.1166 0.050 Uiso 1 1 calc . . . C38 C 0.3119(3) 0.2391(5) 0.11994(19) 0.0508(15) Uani 1 1 d . . . H38A H 0.3347 0.2842 0.1003 0.061 Uiso 1 1 calc . . . H38B H 0.2553 0.2247 0.1023 0.061 Uiso 1 1 calc . . . C39 C 0.3653(3) 0.2261(4) 0.19891(18) 0.0394(13) Uani 1 1 d . . . C40 C 0.3804(3) 0.2548(4) 0.24989(18) 0.0472(14) Uani 1 1 d . . . H40A H 0.3290 0.2591 0.2576 0.057 Uiso 1 1 calc . . . H40B H 0.4064 0.3223 0.2557 0.057 Uiso 1 1 calc . . . C41 C 0.5265(3) 0.2304(4) 0.32851(16) 0.0400(12) Uani 1 1 d . . . C42 C 0.6048(3) 0.2115(4) 0.3295(2) 0.0513(15) Uani 1 1 d . . . H42 H 0.6166 0.1601 0.3099 0.062 Uiso 1 1 calc . . . C43 C 0.6669(4) 0.2693(5) 0.3600(3) 0.072(2) Uani 1 1 d . . . H43 H 0.7210 0.2566 0.3611 0.087 Uiso 1 1 calc . . . C44 C 0.6493(4) 0.3437(5) 0.3879(2) 0.075(2) Uani 1 1 d . . . H44 H 0.6914 0.3825 0.4084 0.090 Uiso 1 1 calc . . . C45 C 0.5719(4) 0.3626(5) 0.38671(19) 0.0630(18) Uani 1 1 d . . . H45 H 0.5608 0.4140 0.4066 0.076 Uiso 1 1 calc . . . C46 C 0.5096(3) 0.3077(4) 0.35689(18) 0.0469(14) Uani 1 1 d . . . H46 H 0.4557 0.3224 0.3557 0.056 Uiso 1 1 calc . . . C47 C 0.3864(3) 0.1064(4) 0.32447(17) 0.0371(12) Uani 1 1 d . . . C48 C 0.4094(3) 0.1079(4) 0.37385(18) 0.0453(14) Uani 1 1 d . . . H48 H 0.4585 0.1389 0.3912 0.054 Uiso 1 1 calc . . . C49 C 0.3601(4) 0.0636(4) 0.39789(19) 0.0543(16) Uani 1 1 d . . . H49 H 0.3755 0.0642 0.4318 0.065 Uiso 1 1 calc . . . C50 C 0.2887(4) 0.0188(5) 0.3725(2) 0.0577(17) Uani 1 1 d . . . H50 H 0.2553 -0.0113 0.3892 0.069 Uiso 1 1 calc . . . C51 C 0.2655(3) 0.0175(5) 0.3235(2) 0.0581(16) Uani 1 1 d . . . H51 H 0.2161 -0.0127 0.3062 0.070 Uiso 1 1 calc . . . C52 C 0.3148(3) 0.0604(4) 0.29993(18) 0.0477(14) Uani 1 1 d . . . H52 H 0.2994 0.0585 0.2660 0.057 Uiso 1 1 calc . . . C53 C 0.5364(4) -0.0355(4) 0.29338(18) 0.0576(16) Uani 1 1 d . . . H53A H 0.5515 0.0052 0.3227 0.086 Uiso 1 1 calc . . . H53B H 0.5848 -0.0587 0.2861 0.086 Uiso 1 1 calc . . . H53C H 0.5051 -0.0943 0.2979 0.086 Uiso 1 1 calc . . . C54 C 0.5931(4) -0.1569(5) 0.16630(19) 0.0530(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0398(2) 0.0314(2) 0.02980(19) -0.00032(17) 0.01490(17) -0.00216(18) Pd2 0.0374(2) 0.0300(2) 0.02892(19) -0.00132(17) 0.01394(16) 0.00148(18) Pd3 0.0426(2) 0.0331(3) 0.0341(2) 0.00032(18) 0.01326(18) 0.00713(19) S1 0.0369(7) 0.0461(9) 0.0320(6) 0.0063(6) 0.0147(6) 0.0016(7) S2 0.0533(9) 0.0517(10) 0.0374(7) -0.0043(7) 0.0222(7) 0.0101(7) S3 0.0394(7) 0.0368(8) 0.0370(7) -0.0027(6) 0.0159(6) -0.0034(6) P1 0.0340(7) 0.0308(8) 0.0294(6) 0.0018(6) 0.0075(6) -0.0037(6) P2 0.0292(7) 0.0298(8) 0.0261(6) -0.0017(6) 0.0082(5) 0.0010(6) P3 0.0383(8) 0.0322(8) 0.0345(7) -0.0040(6) 0.0079(6) 0.0047(6) F1 0.058(2) 0.130(4) 0.051(2) -0.009(2) -0.0052(18) -0.004(2) F2 0.053(2) 0.151(4) 0.069(2) -0.017(2) 0.0334(19) -0.037(2) F3 0.089(3) 0.066(3) 0.101(3) -0.017(2) 0.026(2) -0.019(2) F4 0.126(4) 0.187(5) 0.153(4) 0.056(4) 0.102(4) 0.100(4) F5 0.058(3) 0.272(8) 0.110(4) 0.012(4) -0.009(3) 0.008(4) F6 0.138(4) 0.100(4) 0.137(4) 0.052(3) 0.060(3) 0.057(3) F7 0.101(3) 0.046(2) 0.106(3) 0.011(2) 0.008(2) 0.003(2) F8 0.069(2) 0.091(3) 0.076(3) -0.002(2) -0.006(2) 0.001(2) F9 0.069(2) 0.096(3) 0.082(2) -0.006(2) 0.028(2) 0.029(2) O1 0.047(2) 0.043(2) 0.045(2) -0.0093(19) 0.0007(18) -0.0074(19) O2 0.065(2) 0.042(2) 0.052(2) 0.0116(18) 0.0396(19) 0.0078(19) O3 0.063(3) 0.048(3) 0.065(3) -0.008(2) 0.027(2) 0.016(2) O4 0.045(2) 0.073(3) 0.044(2) 0.020(2) 0.0069(18) -0.003(2) O5 0.051(2) 0.040(2) 0.0348(19) 0.0109(17) 0.0030(17) 0.0037(19) O6 0.062(2) 0.037(2) 0.060(2) -0.0134(19) 0.041(2) -0.0038(19) O7 0.102(4) 0.126(5) 0.047(2) -0.029(3) -0.004(2) 0.026(3) O8 0.100(4) 0.072(3) 0.121(4) 0.012(3) 0.078(3) -0.005(3) O9 0.047(2) 0.041(2) 0.052(2) 0.017(2) 0.0019(18) 0.0084(19) O10 0.098(3) 0.042(3) 0.065(3) -0.010(2) 0.053(2) -0.002(2) O11 0.054(2) 0.079(3) 0.050(2) -0.015(2) 0.0043(19) -0.005(2) O12 0.057(2) 0.048(3) 0.081(3) 0.014(2) 0.032(2) -0.002(2) N1 0.033(2) 0.042(3) 0.027(2) -0.0086(19) 0.0060(18) -0.002(2) N2 0.042(2) 0.033(3) 0.026(2) 0.0000(19) 0.0115(19) -0.005(2) N3 0.036(2) 0.038(3) 0.030(2) 0.006(2) 0.0070(19) -0.001(2) C1 0.044(3) 0.078(5) 0.027(3) -0.011(3) 0.010(2) 0.002(3) C2 0.057(4) 0.068(5) 0.041(3) -0.017(3) 0.006(3) 0.012(3) C3 0.034(3) 0.037(3) 0.040(3) -0.007(3) 0.004(2) -0.001(3) C4 0.038(3) 0.038(3) 0.038(3) 0.003(2) 0.004(2) -0.004(2) C5 0.044(3) 0.035(3) 0.028(3) -0.005(2) 0.002(2) -0.002(3) C6 0.036(3) 0.043(4) 0.045(3) -0.005(3) -0.003(2) -0.006(3) C7 0.044(4) 0.067(5) 0.070(4) -0.014(4) 0.003(3) 0.004(3) C8 0.071(5) 0.049(4) 0.057(4) -0.006(3) -0.013(3) 0.015(4) C9 0.079(5) 0.034(4) 0.047(3) 0.006(3) -0.006(3) -0.005(3) C10 0.048(3) 0.039(4) 0.040(3) 0.003(3) -0.003(3) 0.000(3) C11 0.041(3) 0.038(3) 0.035(3) 0.000(2) 0.019(2) -0.009(3) C12 0.075(4) 0.038(4) 0.042(3) 0.006(3) 0.028(3) 0.003(3) C13 0.115(6) 0.057(5) 0.045(3) -0.006(3) 0.046(4) -0.025(4) C14 0.090(5) 0.059(5) 0.086(5) -0.013(4) 0.064(5) -0.008(4) C15 0.058(4) 0.082(6) 0.086(5) 0.001(4) 0.034(4) 0.015(4) C16 0.048(3) 0.070(5) 0.048(3) 0.007(3) 0.020(3) 0.014(3) C17 0.072(4) 0.040(4) 0.045(3) -0.011(3) 0.023(3) -0.019(3) C18 0.048(4) 0.074(5) 0.039(3) 0.000(3) 0.007(3) 0.000(3) C19 0.054(3) 0.056(4) 0.027(3) 0.001(3) 0.016(3) -0.006(3) C20 0.060(4) 0.057(4) 0.032(3) 0.012(3) 0.008(3) -0.009(3) C21 0.028(3) 0.036(3) 0.033(3) 0.002(2) 0.006(2) -0.008(2) C22 0.035(3) 0.032(3) 0.031(2) -0.002(2) 0.003(2) 0.003(2) C23 0.033(3) 0.025(3) 0.031(2) 0.001(2) 0.007(2) -0.001(2) C24 0.030(3) 0.035(3) 0.048(3) 0.003(3) 0.009(2) 0.002(2) C25 0.033(3) 0.048(4) 0.081(4) 0.010(3) 0.015(3) -0.005(3) C26 0.036(3) 0.047(4) 0.081(4) 0.003(3) -0.006(3) -0.011(3) C27 0.053(4) 0.037(4) 0.050(3) -0.004(3) 0.003(3) 0.003(3) C28 0.038(3) 0.044(4) 0.038(3) 0.005(3) 0.000(2) 0.002(3) C29 0.042(3) 0.032(3) 0.043(3) -0.002(2) 0.019(3) 0.008(2) C30 0.073(4) 0.041(4) 0.039(3) 0.000(3) 0.025(3) -0.009(3) C31 0.138(7) 0.056(5) 0.053(4) -0.001(3) 0.054(5) 0.003(5) C32 0.117(7) 0.062(5) 0.109(6) 0.029(5) 0.089(6) 0.034(5) C33 0.055(4) 0.078(6) 0.149(7) 0.048(6) 0.055(5) 0.017(4) C34 0.039(3) 0.067(5) 0.076(4) 0.022(4) 0.019(3) 0.001(3) C35 0.065(4) 0.045(4) 0.045(3) 0.006(3) 0.020(3) 0.018(3) C36 0.071(5) 0.118(8) 0.072(5) 0.017(5) 0.035(4) 0.036(5) C37 0.038(3) 0.052(4) 0.039(3) 0.015(3) 0.015(2) -0.006(3) C38 0.043(3) 0.060(4) 0.048(3) 0.021(3) 0.011(3) -0.005(3) C39 0.036(3) 0.037(3) 0.044(3) 0.007(3) 0.010(3) -0.004(3) C40 0.051(3) 0.037(3) 0.049(3) -0.002(3) 0.008(3) 0.013(3) C41 0.047(3) 0.031(3) 0.037(3) 0.002(2) 0.003(2) 0.002(3) C42 0.042(3) 0.037(4) 0.068(4) 0.002(3) 0.006(3) 0.003(3) C43 0.051(4) 0.050(5) 0.103(6) 0.005(4) 0.001(4) 0.000(3) C44 0.071(5) 0.049(5) 0.077(5) 0.019(4) -0.024(4) -0.019(4) C45 0.097(5) 0.044(4) 0.038(3) -0.003(3) 0.005(3) -0.024(4) C46 0.062(4) 0.038(3) 0.044(3) 0.000(3) 0.021(3) -0.002(3) C47 0.037(3) 0.031(3) 0.043(3) -0.006(2) 0.010(2) 0.005(2) C48 0.056(3) 0.038(3) 0.044(3) -0.006(3) 0.017(3) -0.005(3) C49 0.077(4) 0.045(4) 0.044(3) 0.003(3) 0.024(3) 0.006(3) C50 0.067(4) 0.046(4) 0.072(4) 0.002(3) 0.039(4) 0.003(3) C51 0.049(4) 0.058(4) 0.070(4) -0.005(3) 0.020(3) 0.001(3) C52 0.049(3) 0.046(4) 0.051(3) -0.004(3) 0.020(3) 0.001(3) C53 0.082(4) 0.041(4) 0.046(3) 0.012(3) 0.011(3) 0.022(3) C54 0.069(4) 0.048(4) 0.042(3) -0.012(3) 0.017(3) -0.012(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 Pd1 C17 2.026(5) . y Pd1 N1 2.131(4) . y Pd1 O2 2.156(3) . y Pd1 P1 2.1699(12) . y Pd2 C35 2.017(5) . y Pd2 N2 2.124(4) . y Pd2 O6 2.151(3) . y Pd2 P2 2.1716(12) . y Pd3 C53 2.032(5) . y Pd3 N3 2.139(4) . y Pd3 P3 2.1741(13) . y Pd3 O10 2.175(3) . y S1 O3 1.424(4) . ? S1 O4 1.427(3) . ? S1 O2 1.459(3) . ? S1 C18 1.828(6) . ? S2 O8 1.391(5) . ? S2 O7 1.427(4) . ? S2 O6 1.442(3) . ? S2 C36 1.811(7) . ? S3 O11 1.419(4) . ? S3 O12 1.421(4) . ? S3 O10 1.439(3) . ? S3 C54 1.850(6) . ? P1 C5 1.814(5) . ? P1 C11 1.832(5) . ? P1 C4 1.839(5) . y P2 C23 1.806(5) . ? P2 C29 1.815(4) . ? P2 C22 1.846(5) . y P3 C41 1.807(5) . ? P3 C47 1.816(5) . ? P3 C40 1.858(5) . y F1 C18 1.350(6) . ? F2 C18 1.332(6) . ? F3 C18 1.300(7) . ? F4 C36 1.317(7) . ? F5 C36 1.300(9) . ? F6 C36 1.301(9) . ? F7 C54 1.294(6) . ? F8 C54 1.328(6) . ? F9 C54 1.315(6) . ? O1 C3 1.329(5) . ? O1 C2 1.465(6) . ? O5 C21 1.327(5) . ? O5 C20 1.468(6) . ? O9 C39 1.323(6) . ? O9 C38 1.454(6) . ? N1 C3 1.281(6) . y N1 C1 1.480(5) . ? N2 C21 1.288(6) . y N2 C19 1.480(5) . ? N3 C39 1.284(6) . y N3 C37 1.485(6) . ? C1 C2 1.520(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.476(6) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.383(7) . ? C5 C6 1.389(6) . ? C6 C7 1.395(7) . ? C6 H6 0.9500 . ? C7 C8 1.363(8) . ? C7 H7 0.9500 . ? C8 C9 1.367(8) . ? C8 H8 0.9500 . ? C9 C10 1.383(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.364(7) . ? C11 C12 1.380(6) . ? C12 C13 1.404(7) . ? C12 H12 0.9500 . ? C13 C14 1.362(9) . ? C13 H13 0.9500 . ? C14 C15 1.370(9) . ? C14 H14 0.9500 . ? C15 C16 1.368(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.530(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.483(6) . y C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.388(6) . ? C23 C28 1.396(7) . ? C24 C25 1.373(7) . ? C24 H24 0.9500 . ? C25 C26 1.374(8) . ? C25 H25 0.9500 . ? C26 C27 1.378(7) . ? C26 H26 0.9500 . ? C27 C28 1.391(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.377(6) . ? C29 C34 1.383(7) . ? C30 C31 1.390(7) . ? C30 H30 0.9500 . ? C31 C32 1.337(10) . ? C31 H31 0.9500 . ? C32 C33 1.373(10) . ? C32 H32 0.9500 . ? C33 C34 1.386(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C37 C38 1.536(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.487(7) . y C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.382(7) . ? C41 C46 1.401(7) . ? C42 C43 1.408(8) . ? C42 H42 0.9500 . ? C43 C44 1.369(9) . ? C43 H43 0.9500 . ? C44 C45 1.365(8) . ? C44 H44 0.9500 . ? C45 C46 1.383(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.383(6) . ? C47 C52 1.385(7) . ? C48 C49 1.392(7) . ? C48 H48 0.9500 . ? C49 C50 1.383(8) . ? C49 H49 0.9500 . ? C50 C51 1.371(8) . ? C50 H50 0.9500 . ? C51 C52 1.376(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 174.97(17) . . y C17 Pd1 O2 89.00(18) . . y N1 Pd1 O2 95.14(14) . . y C17 Pd1 P1 90.68(15) . . y N1 Pd1 P1 84.85(11) . . y O2 Pd1 P1 172.64(9) . . y C35 Pd2 N2 174.38(17) . . y C35 Pd2 O6 89.19(18) . . y N2 Pd2 O6 95.97(14) . . y C35 Pd2 P2 90.08(15) . . y N2 Pd2 P2 84.63(11) . . y O6 Pd2 P2 176.65(9) . . y C53 Pd3 N3 174.96(18) . . y C53 Pd3 P3 90.44(16) . . y N3 Pd3 P3 84.93(11) . . y C53 Pd3 O10 88.77(19) . . y N3 Pd3 O10 95.54(15) . . y P3 Pd3 O10 171.95(10) . . y O3 S1 O4 116.9(2) . . ? O3 S1 O2 114.5(2) . . ? O4 S1 O2 112.7(2) . . ? O3 S1 C18 105.5(3) . . ? O4 S1 C18 102.9(3) . . ? O2 S1 C18 102.2(2) . . ? O8 S2 O7 114.6(3) . . ? O8 S2 O6 115.7(2) . . ? O7 S2 O6 111.8(3) . . ? O8 S2 C36 107.4(4) . . ? O7 S2 C36 102.4(4) . . ? O6 S2 C36 103.2(3) . . ? O11 S3 O12 116.2(2) . . ? O11 S3 O10 113.9(2) . . ? O12 S3 O10 115.6(2) . . ? O11 S3 C54 102.3(3) . . ? O12 S3 C54 104.3(2) . . ? O10 S3 C54 101.6(2) . . ? C5 P1 C11 106.3(2) . . ? C5 P1 C4 106.3(2) . . ? C11 P1 C4 103.7(2) . . ? C5 P1 Pd1 119.93(16) . . ? C11 P1 Pd1 116.01(17) . . ? C4 P1 Pd1 102.97(15) . . ? C23 P2 C29 107.3(2) . . ? C23 P2 C22 105.9(2) . . ? C29 P2 C22 106.0(2) . . ? C23 P2 Pd2 114.69(15) . . ? C29 P2 Pd2 118.47(17) . . ? C22 P2 Pd2 103.34(15) . . ? C41 P3 C47 107.2(2) . . ? C41 P3 C40 105.1(2) . . ? C47 P3 C40 104.9(2) . . ? C41 P3 Pd3 121.00(17) . . ? C47 P3 Pd3 113.31(17) . . ? C40 P3 Pd3 103.76(16) . . ? C3 O1 C2 106.0(4) . . ? S1 O2 Pd1 130.9(2) . . ? C21 O5 C20 105.7(4) . . ? S2 O6 Pd2 132.1(2) . . ? C39 O9 C38 106.9(4) . . ? S3 O10 Pd3 131.6(2) . . ? C3 N1 C1 107.0(4) . . ? C3 N1 Pd1 117.0(3) . . ? C1 N1 Pd1 135.9(3) . . ? C21 N2 C19 106.6(4) . . ? C21 N2 Pd2 117.7(3) . . ? C19 N2 Pd2 135.5(3) . . ? C39 N3 C37 107.6(4) . . ? C39 N3 Pd3 117.6(3) . . ? C37 N3 Pd3 134.7(3) . . ? N1 C1 C2 103.9(4) . . ? N1 C1 H1A 111.0 . . ? C2 C1 H1A 111.0 . . ? N1 C1 H1B 111.0 . . ? C2 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? O1 C2 C1 104.5(4) . . ? O1 C2 H2A 110.8 . . ? C1 C2 H2A 110.8 . . ? O1 C2 H2B 110.8 . . ? C1 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? N1 C3 O1 118.5(4) . . ? N1 C3 C4 123.8(5) . . ? O1 C3 C4 117.6(4) . . ? C3 C4 P1 110.1(3) . . ? C3 C4 H4A 109.6 . . ? P1 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? P1 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? C10 C5 C6 120.5(5) . . ? C10 C5 P1 119.4(4) . . ? C6 C5 P1 120.1(4) . . ? C5 C6 C7 118.4(5) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C8 C7 C6 120.2(5) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.7(6) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C5 C10 C9 120.2(5) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C16 C11 C12 120.1(5) . . ? C16 C11 P1 117.1(4) . . ? C12 C11 P1 122.8(4) . . ? C11 C12 C13 117.6(5) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 118.7(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 122.1(5) . . ? C11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F3 C18 F2 108.8(5) . . ? F3 C18 F1 108.3(5) . . ? F2 C18 F1 107.1(5) . . ? F3 C18 S1 112.4(4) . . ? F2 C18 S1 110.1(4) . . ? F1 C18 S1 109.9(4) . . ? N2 C19 C20 103.9(4) . . ? N2 C19 H19A 111.0 . . ? C20 C19 H19A 111.0 . . ? N2 C19 H19B 111.0 . . ? C20 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? O5 C20 C19 104.6(4) . . ? O5 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? O5 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? N2 C21 O5 119.2(4) . . ? N2 C21 C22 123.4(4) . . ? O5 C21 C22 117.4(4) . . ? C21 C22 P2 109.5(3) . . ? C21 C22 H22A 109.8 . . ? P2 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? P2 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C28 118.7(4) . . ? C24 C23 P2 119.8(4) . . ? C28 C23 P2 121.4(3) . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.6(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C28 120.0(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 119.8(4) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C30 C29 C34 119.1(5) . . ? C30 C29 P2 121.8(4) . . ? C34 C29 P2 118.9(4) . . ? C29 C30 C31 119.6(5) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 120.6(6) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 121.2(6) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C34 118.9(6) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C29 C34 C33 120.6(6) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? Pd2 C35 H35A 109.5 . . ? Pd2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Pd2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? F5 C36 F6 107.5(7) . . ? F5 C36 F4 109.9(7) . . ? F6 C36 F4 108.3(7) . . ? F5 C36 S2 109.0(6) . . ? F6 C36 S2 112.1(6) . . ? F4 C36 S2 110.1(5) . . ? N3 C37 C38 102.8(4) . . ? N3 C37 H37A 111.2 . . ? C38 C37 H37A 111.2 . . ? N3 C37 H37B 111.2 . . ? C38 C37 H37B 111.2 . . ? H37A C37 H37B 109.1 . . ? O9 C38 C37 104.6(4) . . ? O9 C38 H38A 110.8 . . ? C37 C38 H38A 110.8 . . ? O9 C38 H38B 110.8 . . ? C37 C38 H38B 110.8 . . ? H38A C38 H38B 108.9 . . ? N3 C39 O9 117.9(5) . . ? N3 C39 C40 124.0(5) . . ? O9 C39 C40 118.1(5) . . ? C39 C40 P3 109.7(4) . . ? C39 C40 H40A 109.7 . . ? P3 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? P3 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 C41 C46 119.9(5) . . ? C42 C41 P3 119.8(4) . . ? C46 C41 P3 120.2(4) . . ? C41 C42 C43 119.3(5) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.0(6) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.6(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 120.8(6) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 119.3(5) . . ? C45 C46 H46 120.3 . . ? C41 C46 H46 120.3 . . ? C48 C47 C52 119.3(5) . . ? C48 C47 P3 123.9(4) . . ? C52 C47 P3 116.8(4) . . ? C47 C48 C49 119.4(5) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C50 C49 C48 120.1(5) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C51 C50 C49 120.7(5) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 119.0(5) . . ? C50 C51 H51 120.5 . . ? C52 C51 H51 120.5 . . ? C51 C52 C47 121.5(5) . . ? C51 C52 H52 119.2 . . ? C47 C52 H52 119.2 . . ? Pd3 C53 H53A 109.5 . . ? Pd3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Pd3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? F7 C54 F9 110.5(5) . . ? F7 C54 F8 109.1(5) . . ? F9 C54 F8 106.9(5) . . ? F7 C54 S3 110.6(4) . . ? F9 C54 S3 109.8(4) . . ? F8 C54 S3 110.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C5 -73.8(2) . . . . ? N1 Pd1 P1 C5 108.4(2) . . . . ? O2 Pd1 P1 C5 -161.3(8) . . . . ? C17 Pd1 P1 C11 56.0(2) . . . . ? N1 Pd1 P1 C11 -121.7(2) . . . . ? O2 Pd1 P1 C11 -31.4(9) . . . . ? C17 Pd1 P1 C4 168.5(2) . . . . ? N1 Pd1 P1 C4 -9.21(19) . . . . ? O2 Pd1 P1 C4 81.1(8) . . . . ? C35 Pd2 P2 C23 -76.7(2) . . . . ? N2 Pd2 P2 C23 105.22(19) . . . . ? O6 Pd2 P2 C23 -154.3(18) . . . . ? C35 Pd2 P2 C29 51.7(2) . . . . ? N2 Pd2 P2 C29 -126.3(2) . . . . ? O6 Pd2 P2 C29 -25.8(19) . . . . ? C35 Pd2 P2 C22 168.6(2) . . . . ? N2 Pd2 P2 C22 -9.50(18) . . . . ? O6 Pd2 P2 C22 91.0(18) . . . . ? C53 Pd3 P3 C41 63.7(3) . . . . ? N3 Pd3 P3 C41 -118.3(2) . . . . ? O10 Pd3 P3 C41 148.0(8) . . . . ? C53 Pd3 P3 C47 -65.8(2) . . . . ? N3 Pd3 P3 C47 112.2(2) . . . . ? O10 Pd3 P3 C47 18.6(9) . . . . ? C53 Pd3 P3 C40 -178.9(2) . . . . ? N3 Pd3 P3 C40 -0.9(2) . . . . ? O10 Pd3 P3 C40 -94.6(8) . . . . ? O3 S1 O2 Pd1 2.0(4) . . . . ? O4 S1 O2 Pd1 138.8(3) . . . . ? C18 S1 O2 Pd1 -111.5(3) . . . . ? C17 Pd1 O2 S1 120.4(3) . . . . ? N1 Pd1 O2 S1 -62.4(3) . . . . ? P1 Pd1 O2 S1 -152.0(6) . . . . ? O8 S2 O6 Pd2 1.1(4) . . . . ? O7 S2 O6 Pd2 134.7(3) . . . . ? C36 S2 O6 Pd2 -115.9(4) . . . . ? C35 Pd2 O6 S2 121.0(3) . . . . ? N2 Pd2 O6 S2 -61.3(3) . . . . ? P2 Pd2 O6 S2 -161.5(16) . . . . ? O11 S3 O10 Pd3 -132.9(3) . . . . ? O12 S3 O10 Pd3 5.5(4) . . . . ? C54 S3 O10 Pd3 117.8(3) . . . . ? C53 Pd3 O10 S3 -125.0(4) . . . . ? N3 Pd3 O10 S3 57.6(3) . . . . ? P3 Pd3 O10 S3 150.5(6) . . . . ? C17 Pd1 N1 C3 -19(2) . . . . ? O2 Pd1 N1 C3 -164.9(4) . . . . ? P1 Pd1 N1 C3 7.7(3) . . . . ? C17 Pd1 N1 C1 156(2) . . . . ? O2 Pd1 N1 C1 10.5(4) . . . . ? P1 Pd1 N1 C1 -176.9(4) . . . . ? C35 Pd2 N2 C21 -13(2) . . . . ? O6 Pd2 N2 C21 -169.4(3) . . . . ? P2 Pd2 N2 C21 7.3(3) . . . . ? C35 Pd2 N2 C19 161.2(19) . . . . ? O6 Pd2 N2 C19 4.6(4) . . . . ? P2 Pd2 N2 C19 -178.7(4) . . . . ? C53 Pd3 N3 C39 25(2) . . . . ? P3 Pd3 N3 C39 1.3(3) . . . . ? O10 Pd3 N3 C39 173.2(4) . . . . ? C53 Pd3 N3 C37 -151(2) . . . . ? P3 Pd3 N3 C37 -174.6(4) . . . . ? O10 Pd3 N3 C37 -2.7(4) . . . . ? C3 N1 C1 C2 1.7(5) . . . . ? Pd1 N1 C1 C2 -174.0(3) . . . . ? C3 O1 C2 C1 3.3(5) . . . . ? N1 C1 C2 O1 -3.0(5) . . . . ? C1 N1 C3 O1 0.5(6) . . . . ? Pd1 N1 C3 O1 177.1(3) . . . . ? C1 N1 C3 C4 -178.5(4) . . . . ? Pd1 N1 C3 C4 -1.9(6) . . . . ? C2 O1 C3 N1 -2.5(6) . . . . ? C2 O1 C3 C4 176.5(4) . . . . ? N1 C3 C4 P1 -6.7(6) . . . . ? O1 C3 C4 P1 174.3(3) . . . . ? C5 P1 C4 C3 -115.9(4) . . . . ? C11 P1 C4 C3 132.3(4) . . . . ? Pd1 P1 C4 C3 11.0(4) . . . . ? C11 P1 C5 C10 64.9(4) . . . . ? C4 P1 C5 C10 -45.1(4) . . . . ? Pd1 P1 C5 C10 -161.1(3) . . . . ? C11 P1 C5 C6 -115.9(4) . . . . ? C4 P1 C5 C6 134.2(4) . . . . ? Pd1 P1 C5 C6 18.2(5) . . . . ? C10 C5 C6 C7 -2.2(8) . . . . ? P1 C5 C6 C7 178.5(4) . . . . ? C5 C6 C7 C8 1.3(8) . . . . ? C6 C7 C8 C9 0.8(10) . . . . ? C7 C8 C9 C10 -1.9(9) . . . . ? C6 C5 C10 C9 1.2(8) . . . . ? P1 C5 C10 C9 -179.6(4) . . . . ? C8 C9 C10 C5 0.9(8) . . . . ? C5 P1 C11 C16 -178.4(4) . . . . ? C4 P1 C11 C16 -66.6(5) . . . . ? Pd1 P1 C11 C16 45.5(5) . . . . ? C5 P1 C11 C12 1.2(5) . . . . ? C4 P1 C11 C12 113.0(5) . . . . ? Pd1 P1 C11 C12 -135.0(4) . . . . ? C16 C11 C12 C13 0.2(8) . . . . ? P1 C11 C12 C13 -179.3(4) . . . . ? C11 C12 C13 C14 -0.2(9) . . . . ? C12 C13 C14 C15 0.8(10) . . . . ? C13 C14 C15 C16 -1.3(10) . . . . ? C12 C11 C16 C15 -0.8(9) . . . . ? P1 C11 C16 C15 178.8(5) . . . . ? C14 C15 C16 C11 1.4(10) . . . . ? O3 S1 C18 F3 -179.2(4) . . . . ? O4 S1 C18 F3 57.8(4) . . . . ? O2 S1 C18 F3 -59.2(4) . . . . ? O3 S1 C18 F2 59.3(5) . . . . ? O4 S1 C18 F2 -63.7(5) . . . . ? O2 S1 C18 F2 179.3(4) . . . . ? O3 S1 C18 F1 -58.5(4) . . . . ? O4 S1 C18 F1 178.5(4) . . . . ? O2 S1 C18 F1 61.5(5) . . . . ? C21 N2 C19 C20 -3.0(5) . . . . ? Pd2 N2 C19 C20 -177.4(3) . . . . ? C21 O5 C20 C19 -1.8(5) . . . . ? N2 C19 C20 O5 2.8(5) . . . . ? C19 N2 C21 O5 2.1(6) . . . . ? Pd2 N2 C21 O5 177.7(3) . . . . ? C19 N2 C21 C22 -176.3(4) . . . . ? Pd2 N2 C21 C22 -0.7(6) . . . . ? C20 O5 C21 N2 -0.2(6) . . . . ? C20 O5 C21 C22 178.3(4) . . . . ? N2 C21 C22 P2 -8.1(6) . . . . ? O5 C21 C22 P2 173.5(3) . . . . ? C23 P2 C22 C21 -109.1(3) . . . . ? C29 P2 C22 C21 137.1(3) . . . . ? Pd2 P2 C22 C21 11.8(3) . . . . ? C29 P2 C23 C24 -134.1(4) . . . . ? C22 P2 C23 C24 113.0(4) . . . . ? Pd2 P2 C23 C24 -0.3(4) . . . . ? C29 P2 C23 C28 49.6(4) . . . . ? C22 P2 C23 C28 -63.2(4) . . . . ? Pd2 P2 C23 C28 -176.5(3) . . . . ? C28 C23 C24 C25 -0.2(7) . . . . ? P2 C23 C24 C25 -176.5(4) . . . . ? C23 C24 C25 C26 0.2(8) . . . . ? C24 C25 C26 C27 -0.8(9) . . . . ? C25 C26 C27 C28 1.3(9) . . . . ? C26 C27 C28 C23 -1.3(8) . . . . ? C24 C23 C28 C27 0.7(7) . . . . ? P2 C23 C28 C27 177.0(4) . . . . ? C23 P2 C29 C30 21.7(5) . . . . ? C22 P2 C29 C30 134.5(4) . . . . ? Pd2 P2 C29 C30 -110.1(4) . . . . ? C23 P2 C29 C34 -162.7(4) . . . . ? C22 P2 C29 C34 -49.9(5) . . . . ? Pd2 P2 C29 C34 65.5(5) . . . . ? C34 C29 C30 C31 1.4(8) . . . . ? P2 C29 C30 C31 177.0(4) . . . . ? C29 C30 C31 C32 -0.4(10) . . . . ? C30 C31 C32 C33 -0.6(11) . . . . ? C31 C32 C33 C34 0.6(12) . . . . ? C30 C29 C34 C33 -1.4(9) . . . . ? P2 C29 C34 C33 -177.1(5) . . . . ? C32 C33 C34 C29 0.4(11) . . . . ? O8 S2 C36 F5 -62.0(6) . . . . ? O7 S2 C36 F5 177.0(6) . . . . ? O6 S2 C36 F5 60.7(6) . . . . ? O8 S2 C36 F6 179.1(5) . . . . ? O7 S2 C36 F6 58.2(6) . . . . ? O6 S2 C36 F6 -58.1(6) . . . . ? O8 S2 C36 F4 58.6(7) . . . . ? O7 S2 C36 F4 -62.4(7) . . . . ? O6 S2 C36 F4 -178.7(6) . . . . ? C39 N3 C37 C38 4.0(5) . . . . ? Pd3 N3 C37 C38 -179.8(3) . . . . ? C39 O9 C38 C37 2.6(5) . . . . ? N3 C37 C38 O9 -3.9(4) . . . . ? C37 N3 C39 O9 -2.8(6) . . . . ? Pd3 N3 C39 O9 -179.7(3) . . . . ? C37 N3 C39 C40 175.7(4) . . . . ? Pd3 N3 C39 C40 -1.2(6) . . . . ? C38 O9 C39 N3 0.0(6) . . . . ? C38 O9 C39 C40 -178.6(4) . . . . ? N3 C39 C40 P3 0.3(6) . . . . ? O9 C39 C40 P3 178.8(3) . . . . ? C41 P3 C40 C39 128.7(4) . . . . ? C47 P3 C40 C39 -118.4(4) . . . . ? Pd3 P3 C40 C39 0.7(4) . . . . ? C47 P3 C41 C42 127.4(4) . . . . ? C40 P3 C41 C42 -121.3(4) . . . . ? Pd3 P3 C41 C42 -4.6(5) . . . . ? C47 P3 C41 C46 -55.0(5) . . . . ? C40 P3 C41 C46 56.2(5) . . . . ? Pd3 P3 C41 C46 172.9(3) . . . . ? C46 C41 C42 C43 1.2(8) . . . . ? P3 C41 C42 C43 178.8(4) . . . . ? C41 C42 C43 C44 -0.4(9) . . . . ? C42 C43 C44 C45 0.1(10) . . . . ? C43 C44 C45 C46 -0.7(10) . . . . ? C44 C45 C46 C41 1.5(9) . . . . ? C42 C41 C46 C45 -1.8(8) . . . . ? P3 C41 C46 C45 -179.3(4) . . . . ? C41 P3 C47 C48 -10.6(5) . . . . ? C40 P3 C47 C48 -122.0(5) . . . . ? Pd3 P3 C47 C48 125.5(4) . . . . ? C41 P3 C47 C52 171.1(4) . . . . ? C40 P3 C47 C52 59.7(5) . . . . ? Pd3 P3 C47 C52 -52.8(4) . . . . ? C52 C47 C48 C49 -0.3(8) . . . . ? P3 C47 C48 C49 -178.5(4) . . . . ? C47 C48 C49 C50 -0.2(9) . . . . ? C48 C49 C50 C51 -0.1(9) . . . . ? C49 C50 C51 C52 0.7(9) . . . . ? C50 C51 C52 C47 -1.2(9) . . . . ? C48 C47 C52 C51 0.9(8) . . . . ? P3 C47 C52 C51 179.3(4) . . . . ? O11 S3 C54 F7 -58.9(4) . . . . ? O12 S3 C54 F7 179.6(4) . . . . ? O10 S3 C54 F7 59.0(4) . . . . ? O11 S3 C54 F9 63.2(5) . . . . ? O12 S3 C54 F9 -58.2(5) . . . . ? O10 S3 C54 F9 -178.8(4) . . . . ? O11 S3 C54 F8 -179.4(4) . . . . ? O12 S3 C54 F8 59.1(4) . . . . ? O10 S3 C54 F8 -61.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.189 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.146 # Attachment '3b.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 622173' _audit_creation_date 22-1-05 _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 N O P Pd, C F3 S O3' _chemical_formula_sum 'C20 H23 F3 N O4 P Pd S' _chemical_formula_weight 567.82 _chemical_absolute_configuration . 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3330(10) _cell_length_b 9.827(2) _cell_length_c 14.261(3) _cell_angle_alpha 92.55(5) _cell_angle_beta 100.18(5) _cell_angle_gamma 98.93(5) _cell_volume 1132.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6897 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8568 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 30.05 _reflns_number_total 6592 _reflns_number_gt 5724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0175P)^2^+0.5690P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6592 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Pd1 Pd 0.141586(17) -0.003752(14) 0.229153(10) 0.01909(5) Uani 1 1 d . . . S1 S 0.30508(6) 0.28371(5) 0.14258(3) 0.02360(11) Uani 1 1 d . . . P1 P -0.02924(6) -0.16429(5) 0.27759(3) 0.01850(10) Uani 1 1 d . . . F1 F 0.5167(2) 0.51325(17) 0.18069(16) 0.0755(6) Uani 1 1 d . . . F2 F 0.5110(2) 0.38675(18) 0.29904(11) 0.0570(4) Uani 1 1 d . . . F3 F 0.62941(18) 0.33129(19) 0.18473(14) 0.0621(5) Uani 1 1 d . . . O2 O 0.31698(18) 0.14829(14) 0.17859(11) 0.0274(3) Uani 1 1 d . . . O4 O 0.3179(2) 0.28935(19) 0.04422(11) 0.0429(4) Uani 1 1 d . . . O3 O 0.1825(2) 0.35098(17) 0.17481(11) 0.0360(4) Uani 1 1 d . . . O1 O 0.02022(18) -0.37192(14) 0.05042(10) 0.0261(3) Uani 1 1 d . . . N1 N 0.1260(2) -0.15612(16) 0.11303(11) 0.0202(3) Uani 1 1 d . . . C17 C 0.1489(3) 0.1241(2) 0.34628(15) 0.0310(5) Uani 1 1 d . . . H17A H 0.1088 0.0702 0.3962 0.046 Uiso 1 1 calc . . . H17B H 0.0785 0.1937 0.3292 0.046 Uiso 1 1 calc . . . H17C H 0.2629 0.1700 0.3700 0.046 Uiso 1 1 calc . . . C1 C 0.2353(2) -0.1828(2) 0.04380(14) 0.0228(4) Uani 1 1 d . . . C20 C 0.4121(3) -0.1677(3) 0.09700(18) 0.0385(6) Uani 1 1 d . . . H20A H 0.4492 -0.0725 0.1248 0.058 Uiso 1 1 calc . . . H20B H 0.4834 -0.1894 0.0526 0.058 Uiso 1 1 calc . . . H20C H 0.4181 -0.2312 0.1481 0.058 Uiso 1 1 calc . . . C19 C 0.2165(3) -0.0833(3) -0.03457(16) 0.0394(6) Uani 1 1 d . . . H19A H 0.1000 -0.0943 -0.0656 0.059 Uiso 1 1 calc . . . H19B H 0.2834 -0.1032 -0.0819 0.059 Uiso 1 1 calc . . . H19C H 0.2538 0.0117 -0.0067 0.059 Uiso 1 1 calc . . . C2 C 0.1634(3) -0.3337(2) 0.00519(16) 0.0297(5) Uani 1 1 d . . . H2A H 0.1297 -0.3401 -0.0652 0.036 Uiso 1 1 calc . . . H2B H 0.2460 -0.3950 0.0226 0.036 Uiso 1 1 calc . . . C3 C 0.0164(2) -0.2635(2) 0.10853(13) 0.0202(4) Uani 1 1 d . . . C4 C -0.1160(2) -0.2748(2) 0.16739(14) 0.0238(4) Uani 1 1 d . . . H4A H -0.1470 -0.3717 0.1822 0.029 Uiso 1 1 calc . . . H4B H -0.2155 -0.2429 0.1327 0.029 Uiso 1 1 calc . . . C5 C 0.0678(2) -0.2762(2) 0.35985(14) 0.0214(4) Uani 1 1 d . . . C6 C 0.1165(3) -0.3961(2) 0.32715(16) 0.0296(5) Uani 1 1 d . . . H6 H 0.0960 -0.4223 0.2606 0.036 Uiso 1 1 calc . . . C7 C 0.1951(3) -0.4774(2) 0.39139(18) 0.0368(5) Uani 1 1 d . . . H7 H 0.2278 -0.5593 0.3687 0.044 Uiso 1 1 calc . . . C8 C 0.2259(3) -0.4400(2) 0.48806(18) 0.0369(5) Uani 1 1 d . . . H8 H 0.2797 -0.4961 0.5318 0.044 Uiso 1 1 calc . . . C9 C 0.1786(3) -0.3209(3) 0.52148(16) 0.0357(5) Uani 1 1 d . . . H9 H 0.1995 -0.2954 0.5881 0.043 Uiso 1 1 calc . . . C10 C 0.1006(3) -0.2388(2) 0.45751(15) 0.0298(5) Uani 1 1 d . . . H10 H 0.0694 -0.1564 0.4805 0.036 Uiso 1 1 calc . . . C11 C -0.2078(2) -0.1277(2) 0.32423(13) 0.0218(4) Uani 1 1 d . . . C12 C -0.2940(3) -0.2263(2) 0.37170(19) 0.0370(5) Uani 1 1 d . . . H12 H -0.2555 -0.3111 0.3834 0.044 Uiso 1 1 calc . . . C13 C -0.4369(3) -0.2008(3) 0.4021(2) 0.0449(6) Uani 1 1 d . . . H13 H -0.4952 -0.2680 0.4351 0.054 Uiso 1 1 calc . . . C14 C -0.4940(3) -0.0790(3) 0.38477(17) 0.0361(5) Uani 1 1 d . . . H14 H -0.5911 -0.0616 0.4062 0.043 Uiso 1 1 calc . . . C15 C -0.4102(3) 0.0180(2) 0.33621(18) 0.0338(5) Uani 1 1 d . . . H15 H -0.4513 0.1014 0.3229 0.041 Uiso 1 1 calc . . . C16 C -0.2663(3) -0.0051(2) 0.30667(15) 0.0280(4) Uani 1 1 d . . . H16 H -0.2079 0.0631 0.2744 0.034 Uiso 1 1 calc . . . C18 C 0.5009(3) 0.3841(2) 0.20486(19) 0.0384(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01952(8) 0.01668(8) 0.02090(8) -0.00248(5) 0.00653(6) 0.00044(6) S1 0.0242(2) 0.0224(2) 0.0234(2) -0.00125(19) 0.00467(19) 0.00182(19) P1 0.0190(2) 0.0183(2) 0.0186(2) -0.00078(18) 0.00653(18) 0.00150(18) F1 0.0730(12) 0.0273(8) 0.1129(16) 0.0141(9) 0.0010(11) -0.0163(8) F2 0.0529(10) 0.0649(11) 0.0410(9) -0.0160(8) -0.0129(7) 0.0029(8) F3 0.0259(7) 0.0683(12) 0.0894(13) -0.0050(10) 0.0147(8) -0.0019(7) O2 0.0262(7) 0.0188(7) 0.0389(8) 0.0025(6) 0.0143(6) -0.0011(6) O4 0.0545(11) 0.0512(11) 0.0252(8) 0.0039(8) 0.0085(8) 0.0146(9) O3 0.0343(9) 0.0381(9) 0.0385(9) -0.0008(7) 0.0081(7) 0.0144(7) O1 0.0292(7) 0.0203(7) 0.0277(7) -0.0076(6) 0.0103(6) -0.0023(6) N1 0.0212(8) 0.0193(8) 0.0204(8) -0.0029(6) 0.0082(6) 0.0008(6) C17 0.0341(11) 0.0275(11) 0.0294(11) -0.0130(9) 0.0109(9) -0.0021(9) C1 0.0231(9) 0.0224(10) 0.0232(9) -0.0046(8) 0.0092(8) 0.0015(8) C20 0.0236(11) 0.0463(15) 0.0438(14) -0.0148(11) 0.0070(10) 0.0046(10) C19 0.0614(16) 0.0324(13) 0.0265(11) 0.0009(9) 0.0171(11) 0.0042(11) C2 0.0282(11) 0.0275(11) 0.0337(11) -0.0086(9) 0.0145(9) -0.0013(8) C3 0.0218(9) 0.0195(9) 0.0187(9) -0.0021(7) 0.0035(7) 0.0030(7) C4 0.0222(9) 0.0246(10) 0.0226(9) -0.0025(8) 0.0065(8) -0.0035(8) C5 0.0209(9) 0.0208(9) 0.0232(9) 0.0013(7) 0.0064(7) 0.0027(7) C6 0.0356(12) 0.0219(10) 0.0323(11) -0.0015(8) 0.0086(9) 0.0060(9) C7 0.0405(13) 0.0248(11) 0.0480(14) 0.0042(10) 0.0095(11) 0.0127(10) C8 0.0365(12) 0.0310(12) 0.0431(13) 0.0146(10) 0.0040(10) 0.0054(10) C9 0.0405(13) 0.0389(13) 0.0253(11) 0.0040(9) 0.0011(9) 0.0043(10) C10 0.0367(12) 0.0284(11) 0.0251(10) -0.0006(8) 0.0067(9) 0.0077(9) C11 0.0195(9) 0.0246(10) 0.0218(9) -0.0002(7) 0.0070(7) 0.0024(7) C12 0.0327(12) 0.0318(12) 0.0531(15) 0.0146(11) 0.0210(11) 0.0076(10) C13 0.0321(13) 0.0529(16) 0.0555(16) 0.0157(13) 0.0232(12) 0.0043(12) C14 0.0196(10) 0.0544(16) 0.0340(12) -0.0094(11) 0.0062(9) 0.0071(10) C15 0.0225(10) 0.0342(12) 0.0462(13) -0.0002(10) 0.0053(10) 0.0114(9) C16 0.0253(10) 0.0285(11) 0.0309(11) 0.0030(9) 0.0065(8) 0.0049(8) C18 0.0333(12) 0.0285(12) 0.0485(15) -0.0013(10) 0.0034(11) -0.0043(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 2.031(2) . y Pd1 N1 2.1550(18) . y Pd1 O2 2.1631(17) . y Pd1 P1 2.1771(12) . y S1 O3 1.4282(16) . ? S1 O4 1.4283(16) . ? S1 O2 1.4589(16) . ? S1 C18 1.826(3) . ? P1 C11 1.8113(19) . ? P1 C5 1.815(2) . ? P1 C4 1.837(2) . y F1 C18 1.323(3) . ? F2 C18 1.330(3) . ? F3 C18 1.329(3) . ? O1 C3 1.328(2) . ? O1 C2 1.461(2) . ? N1 C3 1.275(2) . y N1 C1 1.497(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C1 C20 1.515(3) . ? C1 C19 1.521(3) . ? C1 C2 1.548(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.493(3) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.392(3) . ? C5 C10 1.392(3) . ? C6 C7 1.386(3) . ? C6 H6 0.9500 . ? C7 C8 1.379(4) . ? C7 H7 0.9500 . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.385(3) . ? C11 C12 1.388(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.371(4) . ? C13 H13 0.9500 . ? C14 C15 1.378(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 174.30(8) . . y C17 Pd1 O2 90.42(8) . . y N1 Pd1 O2 94.79(7) . . y C17 Pd1 P1 91.69(8) . . y N1 Pd1 P1 83.03(6) . . y O2 Pd1 P1 177.32(4) . . y O3 S1 O4 117.46(11) . . ? O3 S1 O2 114.66(10) . . ? O4 S1 O2 113.53(11) . . ? O3 S1 C18 104.11(11) . . ? O4 S1 C18 103.31(12) . . ? O2 S1 C18 100.97(11) . . ? C11 P1 C5 105.71(9) . . ? C11 P1 C4 104.66(10) . . ? C5 P1 C4 105.07(10) . . ? C11 P1 Pd1 122.35(7) . . ? C5 P1 Pd1 114.87(7) . . ? C4 P1 Pd1 102.34(8) . . ? S1 O2 Pd1 132.49(9) . . ? C3 O1 C2 105.85(15) . . ? C3 N1 C1 107.56(15) . . ? C3 N1 Pd1 116.36(13) . . ? C1 N1 Pd1 134.83(12) . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C1 C20 109.12(16) . . ? N1 C1 C19 109.00(17) . . ? C20 C1 C19 112.1(2) . . ? N1 C1 C2 102.08(15) . . ? C20 C1 C2 112.33(19) . . ? C19 C1 C2 111.67(18) . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C2 C1 105.18(15) . . ? O1 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N1 C3 O1 119.21(17) . . ? N1 C3 C4 122.96(17) . . ? O1 C3 C4 117.81(17) . . ? C3 C4 P1 106.23(13) . . ? C3 C4 H4A 110.5 . . ? P1 C4 H4A 110.5 . . ? C3 C4 H4B 110.5 . . ? P1 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C6 C5 C10 119.1(2) . . ? C6 C5 P1 121.38(16) . . ? C10 C5 P1 119.50(15) . . ? C7 C6 C5 120.2(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 120.3(2) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.1(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C5 120.5(2) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C16 C11 C12 119.48(18) . . ? C16 C11 P1 120.08(15) . . ? C12 C11 P1 120.27(16) . . ? C11 C12 C13 119.9(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 119.9(2) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? F1 C18 F3 107.9(2) . . ? F1 C18 F2 107.8(2) . . ? F3 C18 F2 107.3(2) . . ? F1 C18 S1 110.92(19) . . ? F3 C18 S1 111.65(17) . . ? F2 C18 S1 111.13(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C11 45.30(11) . . . . ? N1 Pd1 P1 C11 -136.86(9) . . . . ? O2 Pd1 P1 C11 -172.7(9) . . . . ? C17 Pd1 P1 C5 -85.01(11) . . . . ? N1 Pd1 P1 C5 92.83(9) . . . . ? O2 Pd1 P1 C5 57.0(9) . . . . ? C17 Pd1 P1 C4 161.74(10) . . . . ? N1 Pd1 P1 C4 -20.42(9) . . . . ? O2 Pd1 P1 C4 -56.3(9) . . . . ? O3 S1 O2 Pd1 24.84(16) . . . . ? O4 S1 O2 Pd1 -114.03(14) . . . . ? C18 S1 O2 Pd1 136.08(13) . . . . ? C17 Pd1 O2 S1 -68.69(14) . . . . ? N1 Pd1 O2 S1 113.61(13) . . . . ? P1 Pd1 O2 S1 149.3(8) . . . . ? C17 Pd1 N1 C3 31.5(8) . . . . ? O2 Pd1 N1 C3 -172.41(15) . . . . ? P1 Pd1 N1 C3 9.16(14) . . . . ? C17 Pd1 N1 C1 -133.8(7) . . . . ? O2 Pd1 N1 C1 22.27(19) . . . . ? P1 Pd1 N1 C1 -156.16(18) . . . . ? C3 N1 C1 C20 -122.0(2) . . . . ? Pd1 N1 C1 C20 44.2(3) . . . . ? C3 N1 C1 C19 115.2(2) . . . . ? Pd1 N1 C1 C19 -78.5(2) . . . . ? C3 N1 C1 C2 -3.0(2) . . . . ? Pd1 N1 C1 C2 163.22(15) . . . . ? C3 O1 C2 C1 -2.6(2) . . . . ? N1 C1 C2 O1 3.3(2) . . . . ? C20 C1 C2 O1 120.08(19) . . . . ? C19 C1 C2 O1 -113.0(2) . . . . ? C1 N1 C3 O1 1.6(2) . . . . ? Pd1 N1 C3 O1 -167.52(14) . . . . ? C1 N1 C3 C4 -179.61(18) . . . . ? Pd1 N1 C3 C4 11.2(3) . . . . ? C2 O1 C3 N1 0.7(2) . . . . ? C2 O1 C3 C4 -178.12(18) . . . . ? N1 C3 C4 P1 -28.9(2) . . . . ? O1 C3 C4 P1 149.87(15) . . . . ? C11 P1 C4 C3 158.91(14) . . . . ? C5 P1 C4 C3 -89.98(15) . . . . ? Pd1 P1 C4 C3 30.34(15) . . . . ? C11 P1 C5 C6 132.73(17) . . . . ? C4 P1 C5 C6 22.37(19) . . . . ? Pd1 P1 C5 C6 -89.28(18) . . . . ? C11 P1 C5 C10 -50.00(19) . . . . ? C4 P1 C5 C10 -160.36(16) . . . . ? Pd1 P1 C5 C10 87.99(17) . . . . ? C10 C5 C6 C7 0.7(3) . . . . ? P1 C5 C6 C7 177.97(18) . . . . ? C5 C6 C7 C8 -0.2(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C8 C9 C10 C5 0.8(4) . . . . ? C6 C5 C10 C9 -1.0(3) . . . . ? P1 C5 C10 C9 -178.31(18) . . . . ? C5 P1 C11 C16 151.74(17) . . . . ? C4 P1 C11 C16 -97.60(18) . . . . ? Pd1 P1 C11 C16 17.7(2) . . . . ? C5 P1 C11 C12 -33.0(2) . . . . ? C4 P1 C11 C12 77.7(2) . . . . ? Pd1 P1 C11 C12 -167.02(16) . . . . ? C16 C11 C12 C13 -0.7(4) . . . . ? P1 C11 C12 C13 -176.0(2) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C12 C11 C16 C15 -0.2(3) . . . . ? P1 C11 C16 C15 175.11(17) . . . . ? C14 C15 C16 C11 1.3(3) . . . . ? O3 S1 C18 F1 -61.8(2) . . . . ? O4 S1 C18 F1 61.5(2) . . . . ? O2 S1 C18 F1 179.10(18) . . . . ? O3 S1 C18 F3 177.89(18) . . . . ? O4 S1 C18 F3 -58.9(2) . . . . ? O2 S1 C18 F3 58.7(2) . . . . ? O3 S1 C18 F2 58.2(2) . . . . ? O4 S1 C18 F2 -178.61(17) . . . . ? O2 S1 C18 F2 -60.99(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.534 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.088 # Attachment '4b.cif' data_4b _database_code_depnum_ccdc_archive 'CCDC 622174' _audit_creation_date 22-1-05 _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 Cl N O2 P Pd' _chemical_formula_sum 'C20 H23 Cl N O2 P Pd' _chemical_formula_weight 482.21 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.962(5) _cell_length_b 10.100(5) _cell_length_c 12.534(5) _cell_angle_alpha 82.414(5) _cell_angle_beta 80.486(5) _cell_angle_gamma 64.312(5) _cell_volume 1006.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12472 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.972 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8736 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 35.00 _reflns_number_total 8735 _reflns_number_gt 8240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+0.1708P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8735 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.572982(8) 0.332646(8) 0.680935(5) 0.01728(3) Uani 1 1 d . . . Cl1 Cl 0.83637(3) 0.33680(4) 0.62060(2) 0.02974(6) Uani 1 1 d . . . P1 P 0.31039(3) 0.35149(3) 0.72387(2) 0.01618(5) Uani 1 1 d . . . O1 O 0.38223(11) 0.22271(10) 0.43152(7) 0.02555(15) Uani 1 1 d . . . O2 O 0.63003(18) 0.29492(14) 0.89651(9) 0.0474(3) Uani 1 1 d . . . N1 N 0.54688(11) 0.25279(10) 0.53402(7) 0.01981(15) Uani 1 1 d . . . C20 C 0.78943(16) 0.01815(15) 0.50327(16) 0.0393(3) Uani 1 1 d . . . H20A H 0.8503 0.0431 0.5496 0.059 Uiso 1 1 calc . . . H20B H 0.8686 -0.0454 0.4477 0.059 Uiso 1 1 calc . . . H20C H 0.7278 -0.0337 0.5476 0.059 Uiso 1 1 calc . . . C19 C 0.7571(2) 0.24304(18) 0.37813(11) 0.0375(3) Uani 1 1 d . . . H19A H 0.6744 0.3367 0.3499 0.056 Uiso 1 1 calc . . . H19B H 0.8278 0.1848 0.3175 0.056 Uiso 1 1 calc . . . H19C H 0.8264 0.2623 0.4213 0.056 Uiso 1 1 calc . . . C1 C 0.66812(14) 0.15806(12) 0.44908(9) 0.02376(19) Uani 1 1 d . . . C2 C 0.55204(16) 0.12961(14) 0.38567(10) 0.0294(2) Uani 1 1 d . . . H2A H 0.5706 0.1567 0.3074 0.035 Uiso 1 1 calc . . . H2B H 0.5724 0.0245 0.3951 0.035 Uiso 1 1 calc . . . C3 C 0.39974(12) 0.27887(11) 0.51733(8) 0.01739(15) Uani 1 1 d . . . C4 C 0.24617(12) 0.36619(11) 0.58859(8) 0.01861(16) Uani 1 1 d . . . H4A H 0.1620 0.3262 0.5926 0.022 Uiso 1 1 calc . . . H4B H 0.1973 0.4704 0.5600 0.022 Uiso 1 1 calc . . . C17 C 0.59275(15) 0.38642(14) 0.82175(10) 0.0270(2) Uani 1 1 d . . . C18 C 0.5714(2) 0.54123(18) 0.82983(12) 0.0398(3) Uani 1 1 d . . . H18A H 0.5921 0.5511 0.9021 0.060 Uiso 1 1 calc . . . H18B H 0.4574 0.6107 0.8178 0.060 Uiso 1 1 calc . . . H18C H 0.6508 0.5627 0.7749 0.060 Uiso 1 1 calc . . . C11 C 0.29152(12) 0.18831(11) 0.79318(8) 0.01764(15) Uani 1 1 d . . . C12 C 0.42493(13) 0.07918(12) 0.84302(8) 0.02127(17) Uani 1 1 d . . . H12 H 0.5268 0.0885 0.8391 0.026 Uiso 1 1 calc . . . C13 C 0.40726(15) -0.04345(12) 0.89849(9) 0.0253(2) Uani 1 1 d . . . H13 H 0.4972 -0.1172 0.9331 0.030 Uiso 1 1 calc . . . C14 C 0.25981(16) -0.05861(13) 0.90359(9) 0.0261(2) Uani 1 1 d . . . H14 H 0.2490 -0.1425 0.9415 0.031 Uiso 1 1 calc . . . C15 C 0.12748(15) 0.04929(13) 0.85312(10) 0.0262(2) Uani 1 1 d . . . H15 H 0.0268 0.0383 0.8558 0.031 Uiso 1 1 calc . . . C16 C 0.14247(13) 0.17291(12) 0.79889(9) 0.02255(18) Uani 1 1 d . . . H16 H 0.0513 0.2472 0.7656 0.027 Uiso 1 1 calc . . . C5 C 0.14389(13) 0.50419(11) 0.79373(9) 0.02043(17) Uani 1 1 d . . . C10 C 0.17180(16) 0.53464(15) 0.89204(10) 0.0296(2) Uani 1 1 d . . . H10 H 0.2722 0.4727 0.9219 0.035 Uiso 1 1 calc . . . C9 C 0.05352(19) 0.65520(18) 0.94666(12) 0.0386(3) Uani 1 1 d . . . H9 H 0.0733 0.6757 1.0135 0.046 Uiso 1 1 calc . . . C8 C -0.09338(18) 0.74535(17) 0.90333(14) 0.0404(3) Uani 1 1 d . . . H8 H -0.1735 0.8287 0.9399 0.048 Uiso 1 1 calc . . . C7 C -0.12320(16) 0.71392(16) 0.80689(13) 0.0370(3) Uani 1 1 d . . . H7 H -0.2248 0.7752 0.7781 0.044 Uiso 1 1 calc . . . C6 C -0.00573(14) 0.59318(13) 0.75140(11) 0.0276(2) Uani 1 1 d . . . H6 H -0.0273 0.5717 0.6855 0.033 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01560(4) 0.02082(4) 0.01606(4) -0.00071(3) -0.00292(2) -0.00805(3) Cl1 0.01891(10) 0.04401(16) 0.02942(13) 0.00158(11) -0.00522(9) -0.01648(11) P1 0.01582(10) 0.01790(10) 0.01450(10) -0.00253(8) -0.00025(8) -0.00695(8) O1 0.0270(4) 0.0339(4) 0.0219(3) -0.0111(3) 0.0011(3) -0.0174(3) O2 0.0719(8) 0.0499(6) 0.0265(5) 0.0092(4) -0.0239(5) -0.0283(6) N1 0.0178(3) 0.0231(4) 0.0177(3) -0.0047(3) 0.0008(3) -0.0079(3) C20 0.0219(5) 0.0236(5) 0.0704(10) -0.0073(6) -0.0019(6) -0.0078(4) C19 0.0500(8) 0.0485(8) 0.0281(6) -0.0131(5) 0.0142(5) -0.0376(7) C1 0.0228(4) 0.0235(4) 0.0263(5) -0.0092(4) 0.0079(4) -0.0127(4) C2 0.0327(5) 0.0339(6) 0.0265(5) -0.0153(4) 0.0081(4) -0.0189(5) C3 0.0210(4) 0.0184(4) 0.0142(4) -0.0013(3) -0.0010(3) -0.0099(3) C4 0.0164(4) 0.0220(4) 0.0162(4) -0.0014(3) -0.0025(3) -0.0067(3) C17 0.0296(5) 0.0342(6) 0.0209(5) -0.0017(4) -0.0078(4) -0.0153(4) C18 0.0548(9) 0.0428(7) 0.0350(7) -0.0097(6) -0.0083(6) -0.0297(7) C11 0.0199(4) 0.0184(4) 0.0147(4) -0.0023(3) -0.0018(3) -0.0079(3) C12 0.0213(4) 0.0215(4) 0.0198(4) -0.0018(3) -0.0045(3) -0.0070(3) C13 0.0306(5) 0.0209(4) 0.0223(5) -0.0001(4) -0.0072(4) -0.0078(4) C14 0.0362(6) 0.0230(5) 0.0206(4) 0.0001(4) -0.0018(4) -0.0148(4) C15 0.0294(5) 0.0290(5) 0.0250(5) 0.0008(4) -0.0033(4) -0.0176(4) C16 0.0216(4) 0.0250(4) 0.0224(4) 0.0013(4) -0.0045(3) -0.0112(4) C5 0.0203(4) 0.0199(4) 0.0217(4) -0.0058(3) 0.0047(3) -0.0103(3) C10 0.0308(5) 0.0356(6) 0.0228(5) -0.0111(4) 0.0046(4) -0.0145(5) C9 0.0393(7) 0.0442(7) 0.0345(7) -0.0232(6) 0.0123(5) -0.0197(6) C8 0.0321(6) 0.0356(7) 0.0516(8) -0.0246(6) 0.0163(6) -0.0140(5) C7 0.0229(5) 0.0309(6) 0.0507(8) -0.0152(6) 0.0054(5) -0.0052(4) C6 0.0195(4) 0.0259(5) 0.0344(6) -0.0098(4) 0.0022(4) -0.0065(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 1.9701(13) . y Pd1 N1 2.1896(11) . y Pd1 P1 2.2549(13) . y Pd1 Cl1 2.3734(13) . y P1 C5 1.8169(12) . ? P1 C11 1.8205(13) . ? P1 C4 1.8468(12) . y O1 C3 1.3406(13) . ? O1 C2 1.4640(16) . ? O2 C17 1.2046(16) . y N1 C3 1.2757(15) . y N1 C1 1.4882(14) . ? C20 C1 1.516(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 C1 1.5237(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C1 C2 1.5457(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.4897(15) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C17 C18 1.506(2) . y C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C11 C12 1.3990(14) . ? C11 C16 1.3997(16) . ? C12 C13 1.3960(17) . ? C12 H12 0.9500 . ? C13 C14 1.3851(19) . ? C13 H13 0.9500 . ? C14 C15 1.3928(18) . ? C14 H14 0.9500 . ? C15 C16 1.3893(17) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C5 C10 1.3944(17) . ? C5 C6 1.3970(17) . ? C10 C9 1.3915(18) . ? C10 H10 0.9500 . ? C9 C8 1.387(2) . ? C9 H9 0.9500 . ? C8 C7 1.384(2) . ? C8 H8 0.9500 . ? C7 C6 1.3958(17) . ? C7 H7 0.9500 . ? C6 H6 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 173.83(4) . . y C17 Pd1 P1 96.35(4) . . y N1 Pd1 P1 80.66(3) . . y C17 Pd1 Cl1 86.48(4) . . y N1 Pd1 Cl1 97.09(3) . . y P1 Pd1 Cl1 173.211(11) . . y C5 P1 C11 104.50(6) . . ? C5 P1 C4 105.04(5) . . ? C11 P1 C4 104.99(5) . . ? C5 P1 Pd1 123.11(4) . . ? C11 P1 Pd1 115.56(3) . . ? C4 P1 Pd1 101.74(4) . . ? C3 O1 C2 105.46(9) . . ? C3 N1 C1 108.65(9) . . ? C3 N1 Pd1 117.35(7) . . ? C1 N1 Pd1 133.71(7) . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C1 C20 109.07(11) . . ? N1 C1 C19 109.51(10) . . ? C20 C1 C19 111.89(12) . . ? N1 C1 C2 101.74(9) . . ? C20 C1 C2 112.58(11) . . ? C19 C1 C2 111.53(11) . . ? O1 C2 C1 105.44(9) . . ? O1 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N1 C3 O1 118.16(9) . . ? N1 C3 C4 123.85(9) . . ? O1 C3 C4 117.98(9) . . ? C3 C4 P1 106.46(7) . . ? C3 C4 H4A 110.4 . . ? P1 C4 H4A 110.4 . . ? C3 C4 H4B 110.4 . . ? P1 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? O2 C17 C18 121.72(12) . . ? O2 C17 Pd1 120.25(11) . . ? C18 C17 Pd1 117.90(9) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C11 C16 119.70(10) . . ? C12 C11 P1 120.05(8) . . ? C16 C11 P1 120.23(8) . . ? C13 C12 C11 119.50(10) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.63(10) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.91(11) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.09(11) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.16(10) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C10 C5 C6 119.67(10) . . ? C10 C5 P1 117.43(9) . . ? C6 C5 P1 122.86(9) . . ? C9 C10 C5 120.40(13) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C8 C9 C10 119.84(13) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C7 C8 C9 119.99(12) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C7 C6 120.73(14) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C6 C5 119.33(12) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C5 44.80(6) . . . . ? N1 Pd1 P1 C5 -140.65(5) . . . . ? Cl1 Pd1 P1 C5 -69.49(10) . . . . ? C17 Pd1 P1 C11 -85.23(6) . . . . ? N1 Pd1 P1 C11 89.32(5) . . . . ? Cl1 Pd1 P1 C11 160.47(9) . . . . ? C17 Pd1 P1 C4 161.68(5) . . . . ? N1 Pd1 P1 C4 -23.77(4) . . . . ? Cl1 Pd1 P1 C4 47.38(10) . . . . ? C17 Pd1 N1 C3 77.1(4) . . . . ? P1 Pd1 N1 C3 15.77(7) . . . . ? Cl1 Pd1 N1 C3 -157.76(8) . . . . ? C17 Pd1 N1 C1 -95.8(4) . . . . ? P1 Pd1 N1 C1 -157.21(10) . . . . ? Cl1 Pd1 N1 C1 29.26(10) . . . . ? C3 N1 C1 C20 -122.75(10) . . . . ? Pd1 N1 C1 C20 50.67(13) . . . . ? C3 N1 C1 C19 114.51(12) . . . . ? Pd1 N1 C1 C19 -72.08(14) . . . . ? C3 N1 C1 C2 -3.61(12) . . . . ? Pd1 N1 C1 C2 169.80(8) . . . . ? C3 O1 C2 C1 -7.33(12) . . . . ? N1 C1 C2 O1 6.57(12) . . . . ? C20 C1 C2 O1 123.18(12) . . . . ? C19 C1 C2 O1 -110.09(12) . . . . ? C1 N1 C3 O1 -1.15(13) . . . . ? Pd1 N1 C3 O1 -175.80(7) . . . . ? C1 N1 C3 C4 177.85(9) . . . . ? Pd1 N1 C3 C4 3.20(13) . . . . ? C2 O1 C3 N1 5.67(13) . . . . ? C2 O1 C3 C4 -173.39(9) . . . . ? N1 C3 C4 P1 -25.02(12) . . . . ? O1 C3 C4 P1 153.98(8) . . . . ? C5 P1 C4 C3 161.03(7) . . . . ? C11 P1 C4 C3 -89.07(8) . . . . ? Pd1 P1 C4 C3 31.71(7) . . . . ? N1 Pd1 C17 O2 22.3(5) . . . . ? P1 Pd1 C17 O2 82.93(12) . . . . ? Cl1 Pd1 C17 O2 -103.27(12) . . . . ? N1 Pd1 C17 C18 -161.7(3) . . . . ? P1 Pd1 C17 C18 -101.13(11) . . . . ? Cl1 Pd1 C17 C18 72.67(11) . . . . ? C5 P1 C11 C12 -120.69(9) . . . . ? C4 P1 C11 C12 129.02(8) . . . . ? Pd1 P1 C11 C12 17.82(9) . . . . ? C5 P1 C11 C16 57.92(10) . . . . ? C4 P1 C11 C16 -52.36(9) . . . . ? Pd1 P1 C11 C16 -163.56(7) . . . . ? C16 C11 C12 C13 -0.40(15) . . . . ? P1 C11 C12 C13 178.22(8) . . . . ? C11 C12 C13 C14 0.67(17) . . . . ? C12 C13 C14 C15 -0.06(18) . . . . ? C13 C14 C15 C16 -0.82(18) . . . . ? C14 C15 C16 C11 1.09(17) . . . . ? C12 C11 C16 C15 -0.48(16) . . . . ? P1 C11 C16 C15 -179.10(9) . . . . ? C11 P1 C5 C10 79.93(10) . . . . ? C4 P1 C5 C10 -169.82(9) . . . . ? Pd1 P1 C5 C10 -54.56(10) . . . . ? C11 P1 C5 C6 -102.20(10) . . . . ? C4 P1 C5 C6 8.05(11) . . . . ? Pd1 P1 C5 C6 123.32(9) . . . . ? C6 C5 C10 C9 -1.68(19) . . . . ? P1 C5 C10 C9 176.27(11) . . . . ? C5 C10 C9 C8 0.3(2) . . . . ? C10 C9 C8 C7 1.0(2) . . . . ? C9 C8 C7 C6 -0.9(2) . . . . ? C8 C7 C6 C5 -0.5(2) . . . . ? C10 C5 C6 C7 1.78(18) . . . . ? P1 C5 C6 C7 -176.05(10) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.457 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.071 # Attachment '6b_revised.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 622175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 F3 N O5 P Pd S' _chemical_formula_weight 623.89 _chemical_absolute_configuration ? 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4740(5) _cell_length_b 13.9030(7) _cell_length_c 18.0810(10) _cell_angle_alpha 92.4860(15) _cell_angle_beta 96.7650(15) _cell_angle_gamma 112.951(3) _cell_volume 2624.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20669 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24511 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.07 _reflns_number_total 15294 _reflns_number_gt 8608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0965P)^2^+2.1850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15294 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Pd2 Pd 0.01558(5) 0.61133(3) 0.29734(3) 0.05463(16) Uani 1 1 d . . . Pd1 Pd 0.86966(4) 0.04645(3) 0.195015(18) 0.03663(13) Uani 1 1 d . . . S1 S 0.46119(17) 0.75812(17) 0.10878(9) 0.0670(5) Uani 1 1 d . . . S2 S 0.2119(4) 0.2553(2) 0.43826(15) 0.1267(12) Uani 1 1 d . . . P2 P 0.21091(18) 0.68747(12) 0.35869(8) 0.0510(4) Uani 1 1 d . . . P1 P 1.04072(14) 0.01217(11) 0.19849(7) 0.0377(3) Uani 1 1 d . . . F1 F 0.4393(11) 0.5808(8) 0.0494(6) 0.237(6) Uani 1 1 d . . . F2 F 0.3615(6) 0.6608(6) -0.0224(3) 0.163(3) Uani 1 1 d . . . F3 F 0.2648(7) 0.5877(5) 0.0622(4) 0.159(3) Uani 1 1 d . . . F4 F 0.3751(7) 0.4159(6) 0.3993(4) 0.156(3) Uani 1 1 d . . . F5 F 0.3571(11) 0.3843(17) 0.5161(5) 0.412(13) Uani 1 1 d . . . F6 F 0.2118(10) 0.4342(5) 0.4434(6) 0.219(4) Uani 1 1 d . . . O3 O 0.2516(6) 0.4640(4) 0.2334(3) 0.0781(16) Uani 1 1 d . . . O4 O -0.1787(5) 0.5456(3) 0.2424(3) 0.0690(13) Uani 1 1 d . . . O1 O 0.9725(4) -0.0314(3) 0.40698(18) 0.0493(10) Uani 1 1 d . . . O2 O 0.6980(4) 0.0723(3) 0.18157(18) 0.0432(9) Uani 1 1 d . . . O5 O 0.5808(6) 0.8093(7) 0.0829(3) 0.131(3) Uani 1 1 d . . . O6 O 0.4662(9) 0.7268(5) 0.1799(3) 0.128(3) Uani 1 1 d . . . O7 O 0.3851(7) 0.8198(5) 0.0970(4) 0.128(3) Uani 1 1 d . . . O8 O 0.1098(8) 0.2349(5) 0.4873(4) 0.148(3) Uani 1 1 d . . . O9 O 0.1157(9) 0.2454(8) 0.3570(4) 0.174(4) Uani 1 1 d . . . O10 O 0.2804(8) 0.1994(6) 0.4294(4) 0.137(3) Uani 1 1 d . . . N2 N 0.0874(6) 0.5076(4) 0.2486(3) 0.0593(14) Uani 1 1 d . . . N1 N 0.8743(4) 0.0077(3) 0.3062(2) 0.0379(9) Uani 1 1 d . . . C23 C 0.0256(9) 0.4095(5) 0.1970(4) 0.073(2) Uani 1 1 d . . . C24 C 0.1365(11) 0.3768(6) 0.1921(5) 0.097(3) Uani 1 1 d . . . H24A H 0.1215 0.3106 0.2154 0.117 Uiso 1 1 calc . . . H24B H 0.1473 0.3663 0.1393 0.117 Uiso 1 1 calc . . . C25 C 0.2044(8) 0.5288(5) 0.2630(3) 0.0612(19) Uani 1 1 d . . . C26 C 0.3025(7) 0.6248(5) 0.3118(3) 0.0626(18) Uani 1 1 d . . . H26A H 0.3592 0.6741 0.2808 0.075 Uiso 1 1 calc . . . H26B H 0.3558 0.6038 0.3494 0.075 Uiso 1 1 calc . . . C27 C 0.2949(6) 0.8268(4) 0.3542(3) 0.0458(13) Uani 1 1 d . . . C32 C 0.3306(6) 0.8646(5) 0.2873(3) 0.0468(13) Uani 1 1 d . . . H32 H 0.3139 0.8177 0.2439 0.056 Uiso 1 1 calc . . . C31 C 0.3919(6) 0.9733(6) 0.2846(4) 0.0614(17) Uani 1 1 d . . . H31 H 0.4182 0.9992 0.2389 0.074 Uiso 1 1 calc . . . C30 C 0.4149(6) 1.0432(5) 0.3458(4) 0.0607(17) Uani 1 1 d . . . H30 H 0.4564 1.1165 0.3428 0.073 Uiso 1 1 calc . . . C29 C 0.3773(7) 1.0055(5) 0.4109(4) 0.0607(17) Uani 1 1 d . . . H29 H 0.3922 1.0533 0.4536 0.073 Uiso 1 1 calc . . . C28 C 0.3169(7) 0.8978(5) 0.4161(3) 0.0562(16) Uani 1 1 d . . . H28 H 0.2909 0.8729 0.4620 0.067 Uiso 1 1 calc . . . C33 C 0.2342(8) 0.6683(5) 0.4574(3) 0.0587(17) Uani 1 1 d . . . C34 C 0.1289(8) 0.6300(5) 0.4949(4) 0.072(2) Uani 1 1 d . . . H34 H 0.0450 0.6142 0.4699 0.087 Uiso 1 1 calc . . . C35 C 0.1498(12) 0.6153(6) 0.5711(5) 0.099(3) Uani 1 1 d . . . H35 H 0.0793 0.5897 0.5980 0.119 Uiso 1 1 calc . . . C36 C 0.2704(13) 0.6375(7) 0.6067(5) 0.097(3) Uani 1 1 d . . . H36 H 0.2825 0.6270 0.6581 0.116 Uiso 1 1 calc . . . C37 C 0.3745(10) 0.6745(7) 0.5694(4) 0.088(3) Uani 1 1 d . . . H37 H 0.4576 0.6884 0.5947 0.106 Uiso 1 1 calc . . . C38 C 0.3572(9) 0.6916(6) 0.4943(4) 0.076(2) Uani 1 1 d . . . H38 H 0.4288 0.7190 0.4684 0.091 Uiso 1 1 calc . . . C39 C -0.0494(8) 0.7122(7) 0.3424(6) 0.105(3) Uani 1 1 d . . . H39A H -0.0300 0.7176 0.3976 0.126 Uiso 1 1 calc . . . H39B H -0.0042 0.7827 0.3261 0.126 Uiso 1 1 calc . . . C40 C -0.1798(9) 0.6811(8) 0.3218(6) 0.108(3) Uani 1 1 d . . . H40A H -0.1955 0.7420 0.3041 0.130 Uiso 1 1 calc . . . H40B H -0.2217 0.6621 0.3670 0.130 Uiso 1 1 calc . . . C41 C -0.2426(8) 0.5916(5) 0.2629(4) 0.072(2) Uani 1 1 d . . . C42 C -0.3807(10) 0.5612(7) 0.2321(7) 0.117(4) Uani 1 1 d . . . H42A H -0.4083 0.5014 0.1939 0.176 Uiso 1 1 calc . . . H42B H -0.3913 0.6206 0.2095 0.176 Uiso 1 1 calc . . . H42C H -0.4327 0.5417 0.2726 0.176 Uiso 1 1 calc . . . C43 C -0.0271(9) 0.4340(6) 0.1215(4) 0.084(2) Uani 1 1 d . . . H43A H 0.0431 0.4852 0.0999 0.126 Uiso 1 1 calc . . . H43B H -0.0906 0.4631 0.1290 0.126 Uiso 1 1 calc . . . H43C H -0.0675 0.3694 0.0875 0.126 Uiso 1 1 calc . . . C44 C -0.0807(10) 0.3306(5) 0.2319(5) 0.100(3) Uani 1 1 d . . . H44A H -0.0453 0.3163 0.2802 0.150 Uiso 1 1 calc . . . H44B H -0.1211 0.2653 0.1986 0.150 Uiso 1 1 calc . . . H44C H -0.1447 0.3590 0.2396 0.150 Uiso 1 1 calc . . . C1 C 0.7875(5) 0.0009(5) 0.3632(3) 0.0482(14) Uani 1 1 d . . . C2 C 0.8651(6) -0.0151(6) 0.4337(3) 0.0586(17) Uani 1 1 d . . . H2A H 0.8965 0.0475 0.4706 0.070 Uiso 1 1 calc . . . H2B H 0.8121 -0.0769 0.4575 0.070 Uiso 1 1 calc . . . C3 C 0.9695(5) -0.0094(4) 0.3360(3) 0.0382(11) Uani 1 1 d . . . C4 C 1.0779(5) -0.0057(4) 0.2975(3) 0.0426(12) Uani 1 1 d . . . H4A H 1.0908 -0.0718 0.3015 0.051 Uiso 1 1 calc . . . H4B H 1.1574 0.0533 0.3210 0.051 Uiso 1 1 calc . . . C11 C 1.1839(5) 0.1096(4) 0.1723(3) 0.0424(12) Uani 1 1 d . . . C12 C 1.2746(7) 0.1879(5) 0.2251(3) 0.0561(16) Uani 1 1 d . . . H12 H 1.2656 0.1853 0.2766 0.067 Uiso 1 1 calc . . . C13 C 1.3762(8) 0.2683(5) 0.2033(4) 0.073(2) Uani 1 1 d . . . H13 H 1.4364 0.3206 0.2399 0.087 Uiso 1 1 calc . . . C14 C 1.3914(8) 0.2738(5) 0.1288(4) 0.071(2) Uani 1 1 d . . . H14 H 1.4609 0.3302 0.1140 0.085 Uiso 1 1 calc . . . C15 C 1.3037(7) 0.1956(5) 0.0753(3) 0.0607(17) Uani 1 1 d . . . H15 H 1.3146 0.1975 0.0240 0.073 Uiso 1 1 calc . . . C16 C 1.2001(6) 0.1150(5) 0.0974(3) 0.0543(15) Uani 1 1 d . . . H16 H 1.1397 0.0630 0.0608 0.065 Uiso 1 1 calc . . . C5 C 1.0090(5) -0.1120(4) 0.1451(3) 0.0432(12) Uani 1 1 d . . . C6 C 1.1073(6) -0.1426(5) 0.1303(3) 0.0528(14) Uani 1 1 d . . . H6 H 1.1943 -0.0965 0.1451 0.063 Uiso 1 1 calc . . . C7 C 1.0757(8) -0.2416(6) 0.0936(4) 0.0671(19) Uani 1 1 d . . . H7 H 1.1417 -0.2635 0.0841 0.081 Uiso 1 1 calc . . . C8 C 0.9486(8) -0.3085(5) 0.0710(4) 0.071(2) Uani 1 1 d . . . H8 H 0.9281 -0.3751 0.0448 0.085 Uiso 1 1 calc . . . C9 C 0.8534(7) -0.2788(5) 0.0861(4) 0.0692(19) Uani 1 1 d . . . H9 H 0.7666 -0.3256 0.0716 0.083 Uiso 1 1 calc . . . C10 C 0.8825(6) -0.1799(5) 0.1228(4) 0.0601(16) Uani 1 1 d . . . H10 H 0.8156 -0.1592 0.1325 0.072 Uiso 1 1 calc . . . C17 C 0.8741(6) 0.0841(5) 0.0879(3) 0.0444(13) Uani 1 1 d . . . H17A H 0.9309 0.1587 0.0865 0.053 Uiso 1 1 calc . . . H17B H 0.9056 0.0398 0.0586 0.053 Uiso 1 1 calc . . . C18 C 0.7363(6) 0.0639(6) 0.0564(3) 0.0561(16) Uani 1 1 d . . . H18A H 0.7371 0.1141 0.0191 0.067 Uiso 1 1 calc . . . H18B H 0.6946 -0.0077 0.0302 0.067 Uiso 1 1 calc . . . C19 C 0.6592(5) 0.0742(4) 0.1144(3) 0.0437(12) Uani 1 1 d . . . C20 C 0.5367(7) 0.0842(6) 0.0947(3) 0.0634(18) Uani 1 1 d . . . H20A H 0.4666 0.0145 0.0889 0.095 Uiso 1 1 calc . . . H20B H 0.5369 0.1164 0.0475 0.095 Uiso 1 1 calc . . . H20C H 0.5249 0.1283 0.1345 0.095 Uiso 1 1 calc . . . C22 C 0.6629(6) -0.0943(5) 0.3380(4) 0.0587(16) Uani 1 1 d . . . H22A H 0.6247 -0.0861 0.2885 0.088 Uiso 1 1 calc . . . H22B H 0.6034 -0.1000 0.3740 0.088 Uiso 1 1 calc . . . H22C H 0.6803 -0.1578 0.3354 0.088 Uiso 1 1 calc . . . C21 C 0.7673(7) 0.1003(6) 0.3719(3) 0.0619(18) Uani 1 1 d . . . H21A H 0.8503 0.1596 0.3852 0.093 Uiso 1 1 calc . . . H21B H 0.7148 0.0965 0.4116 0.093 Uiso 1 1 calc . . . H21C H 0.7237 0.1100 0.3247 0.093 Uiso 1 1 calc . . . C45 C 0.3820(9) 0.6417(9) 0.0478(5) 0.096(3) Uani 1 1 d . . . C46 C 0.2873(15) 0.3859(8) 0.4477(6) 0.1267(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2 0.0687(4) 0.0359(2) 0.0668(3) 0.00252(19) 0.0275(2) 0.0244(2) Pd1 0.0398(2) 0.0536(3) 0.02511(18) 0.00311(15) 0.00137(14) 0.0290(2) S1 0.0557(11) 0.1109(14) 0.0485(8) 0.0275(9) 0.0227(7) 0.0421(11) S2 0.235(4) 0.0803(14) 0.0996(17) 0.0227(12) 0.075(2) 0.084(2) P2 0.0711(11) 0.0479(8) 0.0510(8) 0.0100(6) 0.0286(7) 0.0357(8) P1 0.0386(8) 0.0542(8) 0.0298(6) 0.0077(5) 0.0051(5) 0.0282(7) F1 0.274(11) 0.232(9) 0.251(10) -0.124(8) -0.081(8) 0.199(10) F2 0.111(5) 0.240(8) 0.076(4) -0.007(4) -0.004(3) 0.011(5) F3 0.125(6) 0.127(5) 0.184(7) 0.000(4) 0.069(5) -0.006(4) F4 0.120(5) 0.160(6) 0.179(6) 0.078(5) 0.050(5) 0.031(5) F5 0.174(9) 0.90(4) 0.097(6) -0.078(11) -0.026(6) 0.174(16) F6 0.250(10) 0.100(5) 0.377(13) 0.031(6) 0.114(9) 0.125(6) O3 0.131(5) 0.070(3) 0.071(3) 0.014(2) 0.049(3) 0.069(3) O4 0.076(4) 0.043(2) 0.081(3) 0.002(2) 0.018(3) 0.016(2) O1 0.042(2) 0.080(3) 0.0337(18) 0.0194(17) 0.0053(15) 0.032(2) O2 0.045(2) 0.064(2) 0.0322(17) 0.0055(15) 0.0040(15) 0.035(2) O5 0.060(4) 0.227(8) 0.080(4) -0.026(4) 0.025(3) 0.029(5) O6 0.253(9) 0.114(5) 0.060(3) 0.031(3) 0.062(4) 0.104(6) O7 0.091(5) 0.112(5) 0.181(7) 0.040(4) -0.024(4) 0.051(4) O8 0.169(8) 0.104(5) 0.136(6) -0.006(4) 0.108(6) -0.006(5) O9 0.169(8) 0.211(9) 0.068(4) -0.003(5) 0.013(4) 0.001(7) O10 0.185(8) 0.141(6) 0.157(6) 0.033(5) 0.065(6) 0.128(6) N2 0.093(5) 0.047(3) 0.057(3) 0.004(2) 0.028(3) 0.044(3) N1 0.033(2) 0.059(3) 0.0269(18) 0.0070(17) 0.0031(16) 0.024(2) C23 0.123(7) 0.044(3) 0.066(4) 0.009(3) 0.049(4) 0.039(4) C24 0.159(10) 0.071(5) 0.095(6) 0.009(4) 0.050(6) 0.073(6) C25 0.109(6) 0.057(4) 0.047(3) 0.013(3) 0.035(4) 0.058(4) C26 0.082(5) 0.076(4) 0.055(3) 0.013(3) 0.030(3) 0.052(4) C27 0.054(4) 0.053(3) 0.042(3) 0.009(2) 0.011(2) 0.033(3) C32 0.046(3) 0.057(3) 0.046(3) 0.011(2) 0.012(2) 0.028(3) C31 0.047(4) 0.073(4) 0.073(4) 0.036(4) 0.024(3) 0.026(3) C30 0.047(4) 0.057(4) 0.085(5) 0.024(3) 0.007(3) 0.027(3) C29 0.068(5) 0.058(4) 0.061(4) 0.004(3) 0.001(3) 0.034(4) C28 0.079(5) 0.059(4) 0.043(3) 0.011(3) 0.019(3) 0.037(4) C33 0.092(5) 0.053(3) 0.057(3) 0.019(3) 0.039(4) 0.047(4) C34 0.113(7) 0.047(3) 0.062(4) 0.005(3) 0.046(4) 0.027(4) C35 0.163(10) 0.059(4) 0.069(5) 0.011(4) 0.071(6) 0.021(6) C36 0.182(11) 0.071(5) 0.060(5) 0.022(4) 0.046(6) 0.064(7) C37 0.156(9) 0.100(6) 0.053(4) 0.023(4) 0.037(5) 0.091(6) C38 0.126(7) 0.086(5) 0.056(4) 0.031(3) 0.041(4) 0.075(5) C39 0.063(5) 0.077(5) 0.170(9) -0.058(6) 0.018(6) 0.028(4) C40 0.081(7) 0.120(7) 0.133(8) -0.051(6) -0.024(5) 0.068(6) C41 0.080(6) 0.045(4) 0.085(5) 0.007(3) 0.004(4) 0.021(4) C42 0.086(7) 0.075(6) 0.169(10) 0.003(6) -0.034(7) 0.024(5) C43 0.124(8) 0.066(4) 0.063(4) 0.000(3) 0.023(4) 0.037(5) C44 0.157(9) 0.045(4) 0.105(6) 0.007(4) 0.066(6) 0.034(5) C1 0.042(3) 0.080(4) 0.030(2) 0.007(2) 0.008(2) 0.031(3) C2 0.051(4) 0.106(5) 0.035(3) 0.020(3) 0.011(2) 0.046(4) C3 0.035(3) 0.050(3) 0.030(2) 0.007(2) 0.002(2) 0.018(2) C4 0.045(3) 0.060(3) 0.034(2) 0.013(2) 0.006(2) 0.032(3) C11 0.051(3) 0.055(3) 0.036(2) 0.012(2) 0.015(2) 0.034(3) C12 0.076(5) 0.055(3) 0.045(3) 0.011(3) 0.019(3) 0.030(3) C13 0.084(6) 0.055(4) 0.066(4) 0.002(3) 0.022(4) 0.011(4) C14 0.084(6) 0.055(4) 0.074(4) 0.020(3) 0.036(4) 0.020(4) C15 0.073(5) 0.072(4) 0.056(3) 0.024(3) 0.034(3) 0.040(4) C16 0.062(4) 0.075(4) 0.041(3) 0.012(3) 0.015(3) 0.040(4) C5 0.042(3) 0.055(3) 0.040(3) 0.004(2) 0.006(2) 0.026(3) C6 0.053(4) 0.067(4) 0.051(3) 0.011(3) 0.009(3) 0.036(3) C7 0.084(6) 0.073(5) 0.071(4) 0.018(3) 0.022(4) 0.056(4) C8 0.087(6) 0.056(4) 0.072(4) 0.002(3) 0.000(4) 0.036(4) C9 0.064(5) 0.052(4) 0.087(5) 0.009(3) 0.002(4) 0.021(4) C10 0.050(4) 0.055(4) 0.078(4) 0.005(3) 0.005(3) 0.026(3) C17 0.052(4) 0.061(3) 0.027(2) 0.006(2) 0.003(2) 0.031(3) C18 0.054(4) 0.097(5) 0.032(3) 0.014(3) 0.004(2) 0.046(4) C19 0.044(3) 0.056(3) 0.038(3) 0.006(2) 0.001(2) 0.029(3) C20 0.056(4) 0.098(5) 0.054(3) 0.021(3) 0.004(3) 0.049(4) C22 0.038(3) 0.081(4) 0.065(4) 0.013(3) 0.013(3) 0.030(3) C21 0.081(5) 0.088(5) 0.034(3) -0.005(3) 0.006(3) 0.054(4) C45 0.076(6) 0.143(9) 0.068(5) -0.003(5) 0.019(4) 0.042(6) C46 0.235(4) 0.0803(14) 0.0996(17) 0.0227(12) 0.075(2) 0.084(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd2 C39 2.012(7) . y Pd2 N2 2.127(5) . y Pd2 O4 2.145(5) . y Pd2 P2 2.1992(19) . y Pd1 C17 2.030(5) . y Pd1 N1 2.104(4) . y Pd1 O2 2.125(4) . y Pd1 P1 2.1878(14) . y S1 O6 1.378(5) . ? S1 O5 1.424(6) . ? S1 O7 1.448(6) . ? S1 C45 1.767(10) . ? S2 O10 1.321(6) . ? S2 O8 1.499(7) . ? S2 C46 1.670(10) . ? S2 O9 1.697(8) . ? P2 C27 1.807(6) . ? P2 C33 1.820(6) . ? P2 C26 1.855(6) . y P1 C11 1.806(6) . ? P1 C5 1.824(5) . ? P1 C4 1.841(5) . y F1 C45 1.258(11) . ? F2 C45 1.322(10) . ? F3 C45 1.324(10) . ? F4 C46 1.366(12) . ? F5 C46 1.398(15) . ? F6 C46 1.284(13) . ? O3 C25 1.340(7) . ? O3 C24 1.488(11) . ? O4 C41 1.223(9) . y O1 C3 1.332(5) . ? O1 C2 1.467(7) . ? O2 C19 1.248(6) . y N2 C25 1.249(9) . y N2 C23 1.488(8) . ? N1 C3 1.270(6) . y N1 C1 1.497(6) . ? C23 C44 1.513(11) . ? C23 C24 1.519(12) . ? C23 C43 1.533(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.523(10) . y C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.383(7) . ? C27 C28 1.389(8) . ? C32 C31 1.402(9) . ? C32 H32 0.9500 . ? C31 C30 1.371(10) . ? C31 H31 0.9500 . ? C30 C29 1.357(9) . ? C30 H30 0.9500 . ? C29 C28 1.397(9) . ? C29 H29 0.9500 . ? C28 H28 0.9500 . ? C33 C34 1.389(9) . ? C33 C38 1.394(11) . ? C34 C35 1.407(11) . ? C34 H34 0.9500 . ? C35 C36 1.366(14) . ? C35 H35 0.9500 . ? C36 C37 1.372(13) . ? C36 H36 0.9500 . ? C37 C38 1.393(9) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.383(12) . y C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.485(11) . y C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.499(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C1 C21 1.493(9) . ? C1 C22 1.524(9) . ? C1 C2 1.542(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.480(7) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C11 C16 1.389(7) . ? C11 C12 1.405(8) . ? C12 C13 1.376(9) . ? C12 H12 0.9500 . ? C13 C14 1.381(9) . ? C13 H13 0.9500 . ? C14 C15 1.399(10) . ? C14 H14 0.9500 . ? C15 C16 1.393(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C5 C10 1.386(8) . ? C5 C6 1.400(8) . ? C6 C7 1.392(9) . ? C6 H6 0.9500 . ? C7 C8 1.389(10) . ? C7 H7 0.9500 . ? C8 C9 1.360(10) . ? C8 H8 0.9500 . ? C9 C10 1.398(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C17 C18 1.527(8) . y C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.485(8) . y C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.470(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C39 Pd2 N2 178.7(3) . . y C39 Pd2 O4 80.1(3) . . y N2 Pd2 O4 100.6(2) . . y C39 Pd2 P2 95.5(3) . . y N2 Pd2 P2 83.88(18) . . y O4 Pd2 P2 175.56(13) . . y C17 Pd1 N1 177.1(2) . . y C17 Pd1 O2 82.80(18) . . y N1 Pd1 O2 100.03(14) . . y C17 Pd1 P1 93.30(16) . . y N1 Pd1 P1 83.91(12) . . y O2 Pd1 P1 174.72(10) . . y O6 S1 O5 116.3(5) . . ? O6 S1 O7 113.1(5) . . ? O5 S1 O7 109.7(5) . . ? O6 S1 C45 105.9(4) . . ? O5 S1 C45 104.6(4) . . ? O7 S1 C45 106.3(5) . . ? O10 S2 O8 126.9(5) . . ? O10 S2 C46 118.0(7) . . ? O8 S2 C46 103.5(5) . . ? O10 S2 O9 109.6(5) . . ? O8 S2 O9 95.8(5) . . ? C46 S2 O9 96.9(6) . . ? C27 P2 C33 105.1(3) . . ? C27 P2 C26 105.6(3) . . ? C33 P2 C26 106.1(3) . . ? C27 P2 Pd2 117.52(19) . . ? C33 P2 Pd2 117.4(3) . . ? C26 P2 Pd2 104.0(2) . . ? C11 P1 C5 107.5(2) . . ? C11 P1 C4 107.2(2) . . ? C5 P1 C4 106.5(2) . . ? C11 P1 Pd1 118.77(17) . . ? C5 P1 Pd1 112.25(19) . . ? C4 P1 Pd1 103.76(18) . . ? C25 O3 C24 103.8(6) . . ? C41 O4 Pd2 113.1(5) . . ? C3 O1 C2 106.0(4) . . ? C19 O2 Pd1 111.9(3) . . ? C25 N2 C23 109.0(6) . . ? C25 N2 Pd2 118.2(4) . . ? C23 N2 Pd2 132.8(5) . . ? C3 N1 C1 109.0(4) . . ? C3 N1 Pd1 118.5(3) . . ? C1 N1 Pd1 132.4(3) . . ? N2 C23 C44 109.0(5) . . ? N2 C23 C24 101.7(7) . . ? C44 C23 C24 112.5(6) . . ? N2 C23 C43 109.5(5) . . ? C44 C23 C43 110.7(8) . . ? C24 C23 C43 113.0(6) . . ? O3 C24 C23 105.9(5) . . ? O3 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O3 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? N2 C25 O3 119.2(7) . . ? N2 C25 C26 125.5(5) . . ? O3 C25 C26 115.3(7) . . ? C25 C26 P2 106.6(5) . . ? C25 C26 H26A 110.4 . . ? P2 C26 H26A 110.4 . . ? C25 C26 H26B 110.4 . . ? P2 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C32 C27 C28 119.0(5) . . ? C32 C27 P2 120.0(4) . . ? C28 C27 P2 120.9(4) . . ? C27 C32 C31 119.0(5) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C30 C31 C32 121.9(6) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C29 C30 C31 118.7(6) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C30 C29 C28 121.1(6) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C34 C33 C38 120.8(6) . . ? C34 C33 P2 119.4(6) . . ? C38 C33 P2 119.8(5) . . ? C33 C34 C35 118.1(9) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? C36 C35 C34 120.8(8) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 121.1(8) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C38 119.5(9) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 119.7(8) . . ? C37 C38 H38 120.2 . . ? C33 C38 H38 120.2 . . ? C40 C39 Pd2 112.1(6) . . ? C40 C39 H39A 109.2 . . ? Pd2 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? Pd2 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C41 116.2(7) . . ? C39 C40 H40A 108.2 . . ? C41 C40 H40A 108.2 . . ? C39 C40 H40B 108.2 . . ? C41 C40 H40B 108.2 . . ? H40A C40 H40B 107.4 . . ? O4 C41 C40 117.9(7) . . ? O4 C41 C42 123.1(7) . . ? C40 C41 C42 119.0(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C23 C43 H43A 109.5 . . ? C23 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C23 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C23 C44 H44A 109.5 . . ? C23 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C23 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C21 C1 N1 110.3(5) . . ? C21 C1 C22 112.4(5) . . ? N1 C1 C22 107.6(4) . . ? C21 C1 C2 112.2(5) . . ? N1 C1 C2 101.3(4) . . ? C22 C1 C2 112.4(5) . . ? O1 C2 C1 105.1(4) . . ? O1 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N1 C3 O1 117.7(5) . . ? N1 C3 C4 124.6(4) . . ? O1 C3 C4 117.7(4) . . ? C3 C4 P1 108.3(3) . . ? C3 C4 H4A 110.0 . . ? P1 C4 H4A 110.0 . . ? C3 C4 H4B 110.0 . . ? P1 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C16 C11 C12 118.1(5) . . ? C16 C11 P1 120.1(5) . . ? C12 C11 P1 121.4(4) . . ? C13 C12 C11 121.0(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.7(6) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.4(6) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.8(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C11 C16 C15 121.0(6) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C10 C5 C6 119.8(5) . . ? C10 C5 P1 117.9(4) . . ? C6 C5 P1 122.2(4) . . ? C7 C6 C5 119.1(6) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C8 C7 C6 120.5(6) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.2(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.4(7) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C5 C10 C9 120.0(6) . . ? C5 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C18 C17 Pd1 105.6(4) . . ? C18 C17 H17A 110.6 . . ? Pd1 C17 H17A 110.6 . . ? C18 C17 H17B 110.6 . . ? Pd1 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C19 C18 C17 113.5(4) . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O2 C19 C20 119.0(5) . . ? O2 C19 C18 119.3(5) . . ? C20 C19 C18 121.7(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 C22 H22A 109.5 . . ? C1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 C21 H21A 109.5 . . ? C1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? F1 C45 F2 107.9(9) . . ? F1 C45 F3 107.4(11) . . ? F2 C45 F3 102.6(8) . . ? F1 C45 S1 114.1(8) . . ? F2 C45 S1 112.3(8) . . ? F3 C45 S1 111.9(6) . . ? F6 C46 F4 113.5(9) . . ? F6 C46 F5 121.0(11) . . ? F4 C46 F5 105.0(12) . . ? F6 C46 S2 113.9(11) . . ? F4 C46 S2 109.4(7) . . ? F5 C46 S2 91.6(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C39 Pd2 P2 C27 -52.2(4) . . . . ? N2 Pd2 P2 C27 126.6(2) . . . . ? O4 Pd2 P2 C27 -56.8(17) . . . . ? C39 Pd2 P2 C33 74.8(4) . . . . ? N2 Pd2 P2 C33 -106.4(2) . . . . ? O4 Pd2 P2 C33 70.1(17) . . . . ? C39 Pd2 P2 C26 -168.4(4) . . . . ? N2 Pd2 P2 C26 10.4(3) . . . . ? O4 Pd2 P2 C26 -173.0(17) . . . . ? C17 Pd1 P1 C11 52.5(3) . . . . ? N1 Pd1 P1 C11 -126.9(2) . . . . ? O2 Pd1 P1 C11 94.7(12) . . . . ? C17 Pd1 P1 C5 -74.1(2) . . . . ? N1 Pd1 P1 C5 106.5(2) . . . . ? O2 Pd1 P1 C5 -31.9(12) . . . . ? C17 Pd1 P1 C4 171.3(2) . . . . ? N1 Pd1 P1 C4 -8.1(2) . . . . ? O2 Pd1 P1 C4 -146.5(12) . . . . ? C39 Pd2 O4 C41 -2.7(6) . . . . ? N2 Pd2 O4 C41 178.5(5) . . . . ? P2 Pd2 O4 C41 2(2) . . . . ? C17 Pd1 O2 C19 15.2(4) . . . . ? N1 Pd1 O2 C19 -165.2(4) . . . . ? P1 Pd1 O2 C19 -27.3(14) . . . . ? C39 Pd2 N2 C25 55(15) . . . . ? O4 Pd2 N2 C25 173.3(5) . . . . ? P2 Pd2 N2 C25 -6.9(5) . . . . ? C39 Pd2 N2 C23 -124(15) . . . . ? O4 Pd2 N2 C23 -5.7(5) . . . . ? P2 Pd2 N2 C23 174.0(5) . . . . ? C17 Pd1 N1 C3 -6(4) . . . . ? O2 Pd1 N1 C3 -177.1(4) . . . . ? P1 Pd1 N1 C3 6.4(4) . . . . ? C17 Pd1 N1 C1 170(4) . . . . ? O2 Pd1 N1 C1 -1.2(5) . . . . ? P1 Pd1 N1 C1 -177.7(5) . . . . ? C25 N2 C23 C44 123.8(7) . . . . ? Pd2 N2 C23 C44 -57.0(8) . . . . ? C25 N2 C23 C24 4.8(7) . . . . ? Pd2 N2 C23 C24 -176.0(4) . . . . ? C25 N2 C23 C43 -114.9(7) . . . . ? Pd2 N2 C23 C43 64.2(8) . . . . ? C25 O3 C24 C23 5.8(7) . . . . ? N2 C23 C24 O3 -6.3(7) . . . . ? C44 C23 C24 O3 -122.7(7) . . . . ? C43 C23 C24 O3 111.0(7) . . . . ? C23 N2 C25 O3 -1.3(8) . . . . ? Pd2 N2 C25 O3 179.4(4) . . . . ? C23 N2 C25 C26 178.0(5) . . . . ? Pd2 N2 C25 C26 -1.3(8) . . . . ? C24 O3 C25 N2 -3.0(8) . . . . ? C24 O3 C25 C26 177.6(5) . . . . ? N2 C25 C26 P2 10.5(8) . . . . ? O3 C25 C26 P2 -170.2(4) . . . . ? C27 P2 C26 C25 -137.7(4) . . . . ? C33 P2 C26 C25 111.1(4) . . . . ? Pd2 P2 C26 C25 -13.3(4) . . . . ? C33 P2 C27 C32 160.0(5) . . . . ? C26 P2 C27 C32 48.1(6) . . . . ? Pd2 P2 C27 C32 -67.3(5) . . . . ? C33 P2 C27 C28 -24.3(6) . . . . ? C26 P2 C27 C28 -136.2(5) . . . . ? Pd2 P2 C27 C28 108.4(5) . . . . ? C28 C27 C32 C31 2.1(9) . . . . ? P2 C27 C32 C31 177.9(5) . . . . ? C27 C32 C31 C30 -1.4(9) . . . . ? C32 C31 C30 C29 0.1(10) . . . . ? C31 C30 C29 C28 0.4(10) . . . . ? C32 C27 C28 C29 -1.6(10) . . . . ? P2 C27 C28 C29 -177.3(5) . . . . ? C30 C29 C28 C27 0.3(10) . . . . ? C27 P2 C33 C34 117.2(5) . . . . ? C26 P2 C33 C34 -131.3(5) . . . . ? Pd2 P2 C33 C34 -15.6(5) . . . . ? C27 P2 C33 C38 -63.1(6) . . . . ? C26 P2 C33 C38 48.4(6) . . . . ? Pd2 P2 C33 C38 164.1(5) . . . . ? C38 C33 C34 C35 -0.2(9) . . . . ? P2 C33 C34 C35 179.6(5) . . . . ? C33 C34 C35 C36 -0.4(11) . . . . ? C34 C35 C36 C37 -0.1(13) . . . . ? C35 C36 C37 C38 1.1(13) . . . . ? C36 C37 C38 C33 -1.7(11) . . . . ? C34 C33 C38 C37 1.2(10) . . . . ? P2 C33 C38 C37 -178.5(5) . . . . ? N2 Pd2 C39 C40 125(14) . . . . ? O4 Pd2 C39 C40 6.3(8) . . . . ? P2 Pd2 C39 C40 -173.3(9) . . . . ? Pd2 C39 C40 C41 -9.0(13) . . . . ? Pd2 O4 C41 C40 -1.4(9) . . . . ? Pd2 O4 C41 C42 179.3(7) . . . . ? C39 C40 C41 O4 7.1(14) . . . . ? C39 C40 C41 C42 -173.5(10) . . . . ? C3 N1 C1 C21 123.5(5) . . . . ? Pd1 N1 C1 C21 -52.7(6) . . . . ? C3 N1 C1 C22 -113.5(5) . . . . ? Pd1 N1 C1 C22 70.3(6) . . . . ? C3 N1 C1 C2 4.5(6) . . . . ? Pd1 N1 C1 C2 -171.6(4) . . . . ? C3 O1 C2 C1 9.5(6) . . . . ? C21 C1 C2 O1 -126.0(6) . . . . ? N1 C1 C2 O1 -8.3(6) . . . . ? C22 C1 C2 O1 106.3(6) . . . . ? C1 N1 C3 O1 1.6(7) . . . . ? Pd1 N1 C3 O1 178.4(3) . . . . ? C1 N1 C3 C4 -177.8(5) . . . . ? Pd1 N1 C3 C4 -1.0(7) . . . . ? C2 O1 C3 N1 -7.4(7) . . . . ? C2 O1 C3 C4 172.1(5) . . . . ? N1 C3 C4 P1 -6.4(7) . . . . ? O1 C3 C4 P1 174.1(4) . . . . ? C11 P1 C4 C3 136.3(4) . . . . ? C5 P1 C4 C3 -108.9(4) . . . . ? Pd1 P1 C4 C3 9.8(4) . . . . ? C5 P1 C11 C16 44.5(5) . . . . ? C4 P1 C11 C16 158.7(4) . . . . ? Pd1 P1 C11 C16 -84.3(5) . . . . ? C5 P1 C11 C12 -142.2(5) . . . . ? C4 P1 C11 C12 -28.0(5) . . . . ? Pd1 P1 C11 C12 89.0(5) . . . . ? C16 C11 C12 C13 0.5(9) . . . . ? P1 C11 C12 C13 -172.9(5) . . . . ? C11 C12 C13 C14 -0.1(11) . . . . ? C12 C13 C14 C15 -1.1(12) . . . . ? C13 C14 C15 C16 1.9(11) . . . . ? C12 C11 C16 C15 0.3(9) . . . . ? P1 C11 C16 C15 173.8(5) . . . . ? C14 C15 C16 C11 -1.4(10) . . . . ? C11 P1 C5 C10 -145.9(5) . . . . ? C4 P1 C5 C10 99.4(5) . . . . ? Pd1 P1 C5 C10 -13.5(5) . . . . ? C11 P1 C5 C6 38.0(5) . . . . ? C4 P1 C5 C6 -76.6(5) . . . . ? Pd1 P1 C5 C6 170.5(4) . . . . ? C10 C5 C6 C7 -0.3(9) . . . . ? P1 C5 C6 C7 175.6(4) . . . . ? C5 C6 C7 C8 1.0(9) . . . . ? C6 C7 C8 C9 -1.6(11) . . . . ? C7 C8 C9 C10 1.6(11) . . . . ? C6 C5 C10 C9 0.3(9) . . . . ? P1 C5 C10 C9 -175.8(5) . . . . ? C8 C9 C10 C5 -1.0(11) . . . . ? N1 Pd1 C17 C18 167(4) . . . . ? O2 Pd1 C17 C18 -21.8(4) . . . . ? P1 Pd1 C17 C18 154.6(4) . . . . ? Pd1 C17 C18 C19 27.2(6) . . . . ? Pd1 O2 C19 C20 175.9(4) . . . . ? Pd1 O2 C19 C18 -2.8(7) . . . . ? C17 C18 C19 O2 -17.0(8) . . . . ? C17 C18 C19 C20 164.4(6) . . . . ? O6 S1 C45 F1 -61.9(10) . . . . ? O5 S1 C45 F1 61.5(10) . . . . ? O7 S1 C45 F1 177.6(9) . . . . ? O6 S1 C45 F2 175.0(7) . . . . ? O5 S1 C45 F2 -61.6(8) . . . . ? O7 S1 C45 F2 54.4(8) . . . . ? O6 S1 C45 F3 60.2(9) . . . . ? O5 S1 C45 F3 -176.4(8) . . . . ? O7 S1 C45 F3 -60.4(9) . . . . ? O10 S2 C46 F6 168.9(8) . . . . ? O8 S2 C46 F6 -45.4(10) . . . . ? O9 S2 C46 F6 52.3(9) . . . . ? O10 S2 C46 F4 40.6(11) . . . . ? O8 S2 C46 F4 -173.7(9) . . . . ? O9 S2 C46 F4 -76.0(10) . . . . ? O10 S2 C46 F5 -65.9(9) . . . . ? O8 S2 C46 F5 79.8(9) . . . . ? O9 S2 C46 F5 177.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.433 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.124 # Attachment '7a.cif' data_7a _database_code_depnum_ccdc_archive 'CCDC 622176' _audit_creation_date 22-1-05 _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H50 F6 N2 O14 P2 Pd2 S2' _chemical_formula_sum 'C46 H50 F6 N2 O14 P2 Pd2 S2' _chemical_formula_weight 1307.74 _chemical_absolute_configuration ? 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2740(5) _cell_length_b 14.8270(5) _cell_length_c 17.4450(9) _cell_angle_alpha 73.4310(16) _cell_angle_beta 85.1550(15) _cell_angle_gamma 73.2490(14) _cell_volume 2676.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10765 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23205 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.1106 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 29.16 _reflns_number_total 14401 _reflns_number_gt 8027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0642P)^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_number_reflns 14401 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1231 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.70276(3) 0.68015(2) 0.282367(19) 0.02726(10) Uani 1 1 d . . . Pd2 Pd 1.23068(3) 0.31500(2) 0.20280(2) 0.02875(10) Uani 1 1 d . . . S1 S 0.59708(10) 0.18887(8) 0.59003(8) 0.0380(3) Uani 1 1 d . . . S2 S 0.58300(11) 0.21125(11) 0.09113(9) 0.0509(3) Uani 1 1 d . . . P1 P 0.77601(9) 0.80285(7) 0.28258(6) 0.0248(2) Uani 1 1 d . . . P2 P 1.18037(9) 0.17882(7) 0.21422(7) 0.0247(2) Uani 1 1 d . . . F1 F 0.7621(3) 0.2835(2) 0.5337(2) 0.0805(10) Uani 1 1 d . . . F2 F 0.7954(3) 0.1953(2) 0.6532(2) 0.0870(12) Uani 1 1 d . . . F3 F 0.6515(3) 0.3294(2) 0.6286(2) 0.0887(12) Uani 1 1 d . . . F4 F 0.7375(3) 0.2905(3) 0.1293(3) 0.1145(17) Uani 1 1 d . . . F5 F 0.7392(4) 0.1564(5) 0.2050(3) 0.169(2) Uani 1 1 d . . . F6 F 0.5871(4) 0.2804(5) 0.2089(3) 0.180(3) Uani 1 1 d . . . O1 O 0.5252(2) 0.93311(19) 0.11180(18) 0.0376(7) Uani 1 1 d . . . O2 O 0.6180(2) 0.56978(19) 0.28396(19) 0.0345(7) Uani 1 1 d . . . O3 O 0.8911(3) 0.4407(2) 0.3598(2) 0.0519(9) Uani 1 1 d . . . O4 O 0.9844(3) 0.5500(2) 0.3742(2) 0.0484(9) Uani 1 1 d . . . O5 O 1.4591(2) 0.0808(2) 0.36570(18) 0.0374(7) Uani 1 1 d . . . O6 O 1.3039(3) 0.43561(19) 0.1877(2) 0.0389(7) Uani 1 1 d . . . O7 O 1.0203(3) 0.5415(2) 0.1321(2) 0.0570(10) Uani 1 1 d . . . O8 O 0.9329(3) 0.4250(2) 0.12878(19) 0.0435(8) Uani 1 1 d . . . O9 O 0.5123(3) 0.2612(2) 0.5329(2) 0.0672(11) Uani 1 1 d . . . O10 O 0.5470(4) 0.1623(3) 0.6686(2) 0.0703(11) Uani 1 1 d . . . O11 O 0.6723(3) 0.1071(2) 0.5642(2) 0.0532(9) Uani 1 1 d . . . O12 O 0.5023(5) 0.3055(4) 0.0553(4) 0.145(2) Uani 1 1 d . . . O13 O 0.5174(3) 0.1478(3) 0.1374(3) 0.0835(14) Uani 1 1 d . . . O14 O 0.6759(4) 0.1755(5) 0.0431(4) 0.164(3) Uani 1 1 d . . . N1 N 0.6186(3) 0.7782(2) 0.1776(2) 0.0306(8) Uani 1 1 d . . . N2 N 1.3347(3) 0.2280(2) 0.3045(2) 0.0297(8) Uani 1 1 d . . . C1 C 0.5452(5) 0.7684(3) 0.1163(3) 0.0506(14) Uani 1 1 d . . . H1A H 0.4863 0.7300 0.1410 0.061 Uiso 1 1 calc . . . H1B H 0.5995 0.7360 0.0786 0.061 Uiso 1 1 calc . . . C2 C 0.4764(4) 0.8740(3) 0.0737(3) 0.0482(13) Uani 1 1 d . . . H2A H 0.4943 0.8891 0.0156 0.058 Uiso 1 1 calc . . . H2B H 0.3858 0.8859 0.0819 0.058 Uiso 1 1 calc . . . C3 C 0.6008(3) 0.8700(3) 0.1696(3) 0.0310(10) Uani 1 1 d . . . C4 C 0.6584(4) 0.9080(3) 0.2235(3) 0.0320(10) Uani 1 1 d . . . H4A H 0.5950 0.9369 0.2590 0.038 Uiso 1 1 calc . . . H4B H 0.6972 0.9589 0.1916 0.038 Uiso 1 1 calc . . . C5 C 0.7960(3) 0.8295(3) 0.3746(2) 0.0270(9) Uani 1 1 d . . . C6 C 0.7127(3) 0.9024(3) 0.4020(3) 0.0306(9) Uani 1 1 d . . . H6 H 0.6412 0.9424 0.3714 0.037 Uiso 1 1 calc . . . C7 C 0.7340(4) 0.9170(3) 0.4743(3) 0.0373(11) Uani 1 1 d . . . H7 H 0.6777 0.9679 0.4927 0.045 Uiso 1 1 calc . . . C8 C 0.8364(4) 0.8580(3) 0.5192(3) 0.0364(10) Uani 1 1 d . . . H8 H 0.8512 0.8690 0.5682 0.044 Uiso 1 1 calc . . . C9 C 0.9177(4) 0.7831(3) 0.4937(3) 0.0381(11) Uani 1 1 d . . . H9 H 0.9865 0.7408 0.5259 0.046 Uiso 1 1 calc . . . C10 C 0.8988(4) 0.7699(3) 0.4213(3) 0.0358(10) Uani 1 1 d . . . H10 H 0.9563 0.7196 0.4029 0.043 Uiso 1 1 calc . . . C11 C 0.9207(3) 0.8030(3) 0.2296(2) 0.0278(9) Uani 1 1 d . . . C12 C 0.9745(4) 0.8797(3) 0.2200(3) 0.0369(11) Uani 1 1 d . . . H12 H 0.9349 0.9325 0.2422 0.044 Uiso 1 1 calc . . . C13 C 1.0847(4) 0.8795(3) 0.1787(3) 0.0416(11) Uani 1 1 d . . . H13 H 1.1212 0.9315 0.1726 0.050 Uiso 1 1 calc . . . C14 C 1.1411(4) 0.8022(4) 0.1463(3) 0.0517(13) Uani 1 1 d . . . H14 H 1.2169 0.8013 0.1179 0.062 Uiso 1 1 calc . . . C15 C 1.0885(4) 0.7270(3) 0.1549(3) 0.0502(13) Uani 1 1 d . . . H15 H 1.1279 0.6744 0.1324 0.060 Uiso 1 1 calc . . . C16 C 0.9792(4) 0.7279(3) 0.1958(3) 0.0372(11) Uani 1 1 d . . . H16 H 0.9430 0.6760 0.2011 0.045 Uiso 1 1 calc . . . C17 C 0.7682(4) 0.5871(3) 0.3908(3) 0.0333(10) Uani 1 1 d . . . H17 H 0.7810 0.6227 0.4288 0.040 Uiso 1 1 calc . . . C18 C 0.6651(4) 0.5352(3) 0.4191(3) 0.0404(11) Uani 1 1 d . . . H18A H 0.6996 0.4718 0.4589 0.048 Uiso 1 1 calc . . . H18B H 0.5985 0.5760 0.4455 0.048 Uiso 1 1 calc . . . C19 C 0.6127(4) 0.5181(3) 0.3517(3) 0.0401(11) Uani 1 1 d . . . C20 C 0.5477(5) 0.4396(3) 0.3661(4) 0.0622(16) Uani 1 1 d . . . H20A H 0.4618 0.4647 0.3820 0.093 Uiso 1 1 calc . . . H20B H 0.5900 0.3829 0.4087 0.093 Uiso 1 1 calc . . . H20C H 0.5489 0.4199 0.3169 0.093 Uiso 1 1 calc . . . C21 C 0.8849(4) 0.5164(3) 0.3745(3) 0.0378(11) Uani 1 1 d . . . C22 C 1.1015(5) 0.4893(4) 0.3524(4) 0.0741(19) Uani 1 1 d . . . H22A H 1.1085 0.4203 0.3795 0.111 Uiso 1 1 calc . . . H22B H 1.1702 0.5078 0.3688 0.111 Uiso 1 1 calc . . . H22C H 1.1046 0.4991 0.2944 0.111 Uiso 1 1 calc . . . C23 C 1.4038(4) 0.2478(3) 0.3631(3) 0.0422(12) Uani 1 1 d . . . H23A H 1.3479 0.2698 0.4051 0.051 Uiso 1 1 calc . . . H23B H 1.4464 0.2985 0.3366 0.051 Uiso 1 1 calc . . . C24 C 1.4972(4) 0.1493(3) 0.3983(3) 0.0473(13) Uani 1 1 d . . . H24A H 1.5826 0.1516 0.3813 0.057 Uiso 1 1 calc . . . H24B H 1.4932 0.1303 0.4574 0.057 Uiso 1 1 calc . . . C25 C 1.3716(3) 0.1347(3) 0.3121(2) 0.0291(9) Uani 1 1 d . . . C26 C 1.3209(3) 0.0875(3) 0.2628(3) 0.0300(9) Uani 1 1 d . . . H26A H 1.3003 0.0282 0.2970 0.036 Uiso 1 1 calc . . . H26B H 1.3822 0.0685 0.2221 0.036 Uiso 1 1 calc . . . C27 C 1.1514(3) 0.1431(3) 0.1289(2) 0.0274(9) Uani 1 1 d . . . C28 C 1.2463(4) 0.1057(3) 0.0810(3) 0.0383(11) Uani 1 1 d . . . H28 H 1.3298 0.0987 0.0928 0.046 Uiso 1 1 calc . . . C29 C 1.2202(4) 0.0786(3) 0.0161(3) 0.0417(11) Uani 1 1 d . . . H29 H 1.2859 0.0507 -0.0152 0.050 Uiso 1 1 calc . . . C30 C 1.0998(4) 0.0920(3) -0.0031(3) 0.0436(12) Uani 1 1 d . . . H30 H 1.0821 0.0755 -0.0488 0.052 Uiso 1 1 calc . . . C31 C 1.0047(4) 0.1292(4) 0.0437(3) 0.0531(14) Uani 1 1 d . . . H31 H 0.9214 0.1370 0.0310 0.064 Uiso 1 1 calc . . . C32 C 1.0302(4) 0.1551(4) 0.1087(3) 0.0450(12) Uani 1 1 d . . . H32 H 0.9639 0.1816 0.1404 0.054 Uiso 1 1 calc . . . C33 C 1.0562(3) 0.1584(3) 0.2832(2) 0.0269(9) Uani 1 1 d . . . C34 C 1.0460(4) 0.0638(3) 0.3163(3) 0.0362(11) Uani 1 1 d . . . H34 H 1.1020 0.0107 0.3004 0.043 Uiso 1 1 calc . . . C35 C 0.9551(4) 0.0466(3) 0.3721(3) 0.0414(11) Uani 1 1 d . . . H35 H 0.9484 -0.0182 0.3944 0.050 Uiso 1 1 calc . . . C36 C 0.8735(4) 0.1237(4) 0.3957(3) 0.0415(11) Uani 1 1 d . . . H36 H 0.8124 0.1116 0.4353 0.050 Uiso 1 1 calc . . . C37 C 0.8810(4) 0.2185(3) 0.3616(3) 0.0385(11) Uani 1 1 d . . . H37 H 0.8232 0.2717 0.3763 0.046 Uiso 1 1 calc . . . C38 C 0.9734(4) 0.2357(3) 0.3058(3) 0.0307(10) Uani 1 1 d . . . H38 H 0.9797 0.3005 0.2832 0.037 Uiso 1 1 calc . . . C39 C 1.1451(4) 0.3993(3) 0.0971(3) 0.0363(10) Uani 1 1 d . . . H39 H 1.1297 0.3591 0.0637 0.044 Uiso 1 1 calc . . . C40 C 1.2372(5) 0.4583(4) 0.0573(3) 0.0562(14) Uani 1 1 d . . . H40A H 1.2998 0.4199 0.0269 0.067 Uiso 1 1 calc . . . H40B H 1.1921 0.5198 0.0189 0.067 Uiso 1 1 calc . . . C41 C 1.3003(4) 0.4821(3) 0.1163(3) 0.0451(12) Uani 1 1 d . . . C42 C 1.3669(5) 0.5594(4) 0.0890(4) 0.0761(19) Uani 1 1 d . . . H42A H 1.4076 0.5638 0.1348 0.114 Uiso 1 1 calc . . . H42B H 1.3075 0.6226 0.0654 0.114 Uiso 1 1 calc . . . H42C H 1.4293 0.5427 0.0490 0.114 Uiso 1 1 calc . . . C43 C 1.0295(4) 0.4632(3) 0.1201(3) 0.0414(12) Uani 1 1 d . . . C44 C 0.8217(4) 0.4799(4) 0.1603(3) 0.0589(15) Uani 1 1 d . . . H44A H 0.8383 0.4826 0.2137 0.088 Uiso 1 1 calc . . . H44B H 0.7559 0.4478 0.1636 0.088 Uiso 1 1 calc . . . H44C H 0.7954 0.5465 0.1248 0.088 Uiso 1 1 calc . . . C45 C 0.6652(5) 0.2355(5) 0.1616(4) 0.0696(18) Uani 1 1 d . . . C46 C 0.7064(5) 0.2519(4) 0.6046(4) 0.0501(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03257(18) 0.02139(15) 0.0286(2) -0.00624(14) -0.00099(14) -0.00892(12) Pd2 0.03386(18) 0.02331(16) 0.0296(2) -0.00628(14) 0.00028(14) -0.00968(13) S1 0.0395(6) 0.0344(6) 0.0396(8) -0.0106(6) 0.0011(5) -0.0095(5) S2 0.0430(7) 0.0779(9) 0.0471(9) -0.0271(8) 0.0086(6) -0.0328(7) P1 0.0283(5) 0.0220(5) 0.0257(6) -0.0079(5) -0.0009(4) -0.0081(4) P2 0.0245(5) 0.0237(5) 0.0277(6) -0.0094(5) -0.0010(4) -0.0067(4) F1 0.071(2) 0.077(2) 0.093(3) -0.008(2) 0.016(2) -0.0389(18) F2 0.079(2) 0.074(2) 0.103(3) -0.006(2) -0.057(2) -0.0158(18) F3 0.087(2) 0.067(2) 0.134(4) -0.061(2) -0.007(2) -0.0201(18) F4 0.066(2) 0.117(3) 0.208(5) -0.094(4) 0.018(3) -0.055(2) F5 0.111(4) 0.249(6) 0.113(4) 0.030(4) -0.071(3) -0.055(4) F6 0.085(3) 0.343(8) 0.222(6) -0.233(6) 0.050(3) -0.087(4) O1 0.0420(17) 0.0283(14) 0.039(2) -0.0034(14) -0.0189(15) -0.0053(13) O2 0.0452(17) 0.0286(15) 0.038(2) -0.0111(15) 0.0059(15) -0.0220(13) O3 0.065(2) 0.0242(15) 0.062(3) -0.0152(17) -0.0057(18) -0.0005(14) O4 0.0398(18) 0.0456(18) 0.058(3) -0.0163(18) -0.0036(16) -0.0060(15) O5 0.0347(16) 0.0373(16) 0.039(2) -0.0066(15) -0.0142(14) -0.0077(13) O6 0.0445(17) 0.0270(15) 0.048(2) -0.0092(16) 0.0096(16) -0.0176(13) O7 0.062(2) 0.0302(16) 0.080(3) -0.0229(19) 0.005(2) -0.0072(15) O8 0.0429(18) 0.0411(17) 0.047(2) -0.0167(16) -0.0073(16) -0.0050(14) O9 0.065(2) 0.050(2) 0.083(3) -0.014(2) -0.033(2) -0.0051(18) O10 0.090(3) 0.070(2) 0.052(3) -0.017(2) 0.035(2) -0.033(2) O11 0.061(2) 0.0444(18) 0.059(3) -0.0253(18) 0.0092(18) -0.0132(16) O12 0.090(4) 0.132(4) 0.145(6) 0.073(4) -0.038(4) -0.029(3) O13 0.070(3) 0.064(2) 0.123(4) -0.011(3) 0.008(3) -0.046(2) O14 0.079(3) 0.329(8) 0.203(7) -0.229(7) 0.069(4) -0.105(4) N1 0.0352(19) 0.0252(17) 0.032(2) -0.0074(16) -0.0043(16) -0.0086(14) N2 0.0352(18) 0.0284(17) 0.030(2) -0.0077(16) -0.0014(16) -0.0153(14) C1 0.066(3) 0.038(2) 0.055(4) -0.012(2) -0.029(3) -0.017(2) C2 0.061(3) 0.044(3) 0.046(3) -0.008(2) -0.021(3) -0.022(2) C3 0.029(2) 0.035(2) 0.030(3) -0.009(2) -0.0003(19) -0.0085(17) C4 0.034(2) 0.028(2) 0.033(3) -0.009(2) -0.0042(19) -0.0070(17) C5 0.033(2) 0.028(2) 0.025(2) -0.0078(18) 0.0005(18) -0.0153(17) C6 0.028(2) 0.034(2) 0.029(3) -0.010(2) 0.0041(18) -0.0065(17) C7 0.044(3) 0.040(2) 0.032(3) -0.019(2) 0.008(2) -0.013(2) C8 0.045(3) 0.045(3) 0.026(3) -0.012(2) -0.001(2) -0.020(2) C9 0.041(2) 0.043(2) 0.030(3) -0.009(2) -0.009(2) -0.011(2) C10 0.035(2) 0.038(2) 0.034(3) -0.015(2) -0.006(2) -0.0030(19) C11 0.030(2) 0.029(2) 0.026(2) -0.0094(19) 0.0002(18) -0.0071(17) C12 0.047(3) 0.038(2) 0.035(3) -0.015(2) 0.000(2) -0.020(2) C13 0.045(3) 0.051(3) 0.041(3) -0.016(2) 0.004(2) -0.030(2) C14 0.040(3) 0.069(3) 0.054(4) -0.024(3) 0.012(2) -0.023(2) C15 0.042(3) 0.050(3) 0.065(4) -0.028(3) 0.016(3) -0.014(2) C16 0.035(2) 0.033(2) 0.046(3) -0.015(2) 0.006(2) -0.0102(18) C17 0.044(2) 0.025(2) 0.027(3) -0.0021(19) -0.005(2) -0.0066(18) C18 0.053(3) 0.029(2) 0.032(3) -0.002(2) 0.005(2) -0.009(2) C19 0.039(3) 0.027(2) 0.051(4) -0.008(2) 0.008(2) -0.0090(19) C20 0.067(3) 0.042(3) 0.081(5) -0.008(3) 0.005(3) -0.032(3) C21 0.044(3) 0.030(2) 0.030(3) -0.003(2) -0.007(2) 0.0017(19) C22 0.044(3) 0.068(4) 0.100(6) -0.030(4) 0.001(3) 0.008(3) C23 0.046(3) 0.042(2) 0.046(3) -0.013(2) -0.011(2) -0.020(2) C24 0.047(3) 0.051(3) 0.051(4) -0.016(3) -0.016(2) -0.017(2) C25 0.025(2) 0.038(2) 0.022(2) -0.0037(19) -0.0005(17) -0.0098(17) C26 0.027(2) 0.0231(19) 0.037(3) -0.0052(19) -0.0051(18) -0.0039(16) C27 0.028(2) 0.028(2) 0.027(2) -0.0101(19) -0.0011(17) -0.0071(16) C28 0.024(2) 0.055(3) 0.036(3) -0.017(2) -0.0007(19) -0.0054(19) C29 0.038(2) 0.056(3) 0.033(3) -0.019(2) 0.004(2) -0.009(2) C30 0.051(3) 0.058(3) 0.029(3) -0.020(2) -0.003(2) -0.019(2) C31 0.039(3) 0.095(4) 0.039(3) -0.029(3) 0.003(2) -0.029(3) C32 0.031(2) 0.069(3) 0.037(3) -0.026(3) 0.000(2) -0.006(2) C33 0.026(2) 0.034(2) 0.024(2) -0.0080(19) -0.0021(17) -0.0125(17) C34 0.038(2) 0.032(2) 0.044(3) -0.017(2) 0.004(2) -0.0121(19) C35 0.048(3) 0.042(2) 0.044(3) -0.014(2) 0.009(2) -0.026(2) C36 0.037(2) 0.065(3) 0.035(3) -0.023(3) 0.012(2) -0.027(2) C37 0.032(2) 0.045(3) 0.041(3) -0.021(2) 0.001(2) -0.007(2) C38 0.033(2) 0.030(2) 0.028(3) -0.0107(19) -0.0047(19) -0.0028(17) C39 0.042(2) 0.031(2) 0.029(3) -0.006(2) 0.001(2) -0.0019(19) C40 0.064(3) 0.049(3) 0.035(3) 0.002(3) 0.016(3) -0.003(3) C41 0.045(3) 0.029(2) 0.054(4) -0.006(2) 0.019(3) -0.010(2) C42 0.076(4) 0.044(3) 0.099(6) -0.004(3) 0.038(4) -0.029(3) C43 0.048(3) 0.030(2) 0.036(3) -0.005(2) -0.011(2) 0.003(2) C44 0.042(3) 0.066(3) 0.069(4) -0.032(3) -0.006(3) -0.001(2) C45 0.042(3) 0.108(5) 0.079(5) -0.055(4) 0.014(3) -0.028(3) C46 0.049(3) 0.042(3) 0.058(4) -0.015(3) -0.009(3) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C17 2.046(4) . y Pd1 N1 2.082(3) . y Pd1 O2 2.112(2) . y Pd1 P1 2.2051(10) . y Pd2 C39 2.046(4) . y Pd2 N2 2.088(3) . y Pd2 O6 2.120(3) . y Pd2 P2 2.2022(10) . y S1 O9 1.421(3) . ? S1 O10 1.429(4) . ? S1 O11 1.430(3) . ? S1 C46 1.819(5) . ? S2 O14 1.366(4) . ? S2 O13 1.397(4) . ? S2 O12 1.427(5) . ? S2 C45 1.771(6) . ? P1 C5 1.805(4) . ? P1 C11 1.805(4) . ? P1 C4 1.837(4) . y P2 C27 1.798(4) . ? P2 C33 1.803(4) . ? P2 C26 1.843(4) . y F1 C46 1.360(6) . ? F2 C46 1.297(5) . ? F3 C46 1.304(5) . ? F4 C45 1.300(7) . ? F5 C45 1.296(8) . ? F6 C45 1.324(6) . ? O1 C3 1.329(5) . ? O1 C2 1.479(5) . ? O2 C19 1.220(5) . y O3 C21 1.203(5) . ? O4 C21 1.351(5) . ? O4 C22 1.456(5) . ? O5 C25 1.326(5) . ? O5 C24 1.470(5) . ? O6 C41 1.237(6) . y O7 C43 1.211(5) . ? O8 C43 1.344(5) . ? O8 C44 1.444(5) . ? N1 C3 1.285(5) . y N1 C1 1.469(5) . ? N2 C25 1.295(5) . y N2 C23 1.476(5) . ? C1 C2 1.529(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.496(5) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.382(5) . ? C5 C10 1.395(5) . ? C6 C7 1.390(6) . ? C6 H6 0.9500 . ? C7 C8 1.376(6) . ? C7 H7 0.9500 . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.382(5) . ? C11 C12 1.401(5) . ? C12 C13 1.382(6) . ? C12 H12 0.9500 . ? C13 C14 1.388(6) . ? C13 H13 0.9500 . ? C14 C15 1.375(6) . ? C14 H14 0.9500 . ? C15 C16 1.370(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C21 1.491(5) . ? C17 C18 1.545(6) . y C17 H17 1.0000 . ? C18 C19 1.472(6) . y C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.498(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.526(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.487(5) . y C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.386(5) . ? C27 C32 1.389(5) . ? C28 C29 1.382(6) . ? C28 H28 0.9500 . ? C29 C30 1.371(6) . ? C29 H29 0.9500 . ? C30 C31 1.374(6) . ? C30 H30 0.9500 . ? C31 C32 1.373(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.385(5) . ? C33 C34 1.390(6) . ? C34 C35 1.380(6) . ? C34 H34 0.9500 . ? C35 C36 1.387(6) . ? C35 H35 0.9500 . ? C36 C37 1.385(6) . ? C36 H36 0.9500 . ? C37 C38 1.393(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C43 1.475(6) . ? C39 C40 1.543(7) . y C39 H39 1.0000 . ? C40 C41 1.472(7) . y C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.493(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 174.17(15) . . y C17 Pd1 O2 82.10(14) . . y N1 Pd1 O2 96.10(12) . . y C17 Pd1 P1 99.24(11) . . y N1 Pd1 P1 82.13(9) . . y O2 Pd1 P1 175.29(8) . . y C39 Pd2 N2 174.28(15) . . y C39 Pd2 O6 82.26(15) . . y N2 Pd2 O6 95.33(12) . . y C39 Pd2 P2 99.99(12) . . y N2 Pd2 P2 81.72(9) . . y O6 Pd2 P2 172.10(8) . . y O9 S1 O10 114.7(2) . . ? O9 S1 O11 116.1(2) . . ? O10 S1 O11 113.7(2) . . ? O9 S1 C46 103.8(2) . . ? O10 S1 C46 102.0(3) . . ? O11 S1 C46 104.3(2) . . ? O14 S2 O13 118.0(3) . . ? O14 S2 O12 115.5(4) . . ? O13 S2 O12 111.5(3) . . ? O14 S2 C45 102.2(3) . . ? O13 S2 C45 104.5(3) . . ? O12 S2 C45 102.5(4) . . ? C5 P1 C11 104.72(17) . . ? C5 P1 C4 107.38(17) . . ? C11 P1 C4 106.17(19) . . ? C5 P1 Pd1 121.32(13) . . ? C11 P1 Pd1 114.64(12) . . ? C4 P1 Pd1 101.50(13) . . ? C27 P2 C33 105.07(17) . . ? C27 P2 C26 106.70(17) . . ? C33 P2 C26 104.92(19) . . ? C27 P2 Pd2 122.51(14) . . ? C33 P2 Pd2 115.62(12) . . ? C26 P2 Pd2 100.26(12) . . ? C3 O1 C2 106.4(3) . . ? C19 O2 Pd1 111.2(3) . . ? C21 O4 C22 115.5(3) . . ? C25 O5 C24 106.6(3) . . ? C41 O6 Pd2 110.0(3) . . ? C43 O8 C44 114.9(3) . . ? C3 N1 C1 107.9(3) . . ? C3 N1 Pd1 117.7(3) . . ? C1 N1 Pd1 132.5(3) . . ? C25 N2 C23 107.3(3) . . ? C25 N2 Pd2 116.7(3) . . ? C23 N2 Pd2 134.2(3) . . ? N1 C1 C2 104.0(3) . . ? N1 C1 H1A 111.0 . . ? C2 C1 H1A 111.0 . . ? N1 C1 H1B 111.0 . . ? C2 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? O1 C2 C1 103.7(3) . . ? O1 C2 H2A 111.0 . . ? C1 C2 H2A 111.0 . . ? O1 C2 H2B 111.0 . . ? C1 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 O1 117.8(3) . . ? N1 C3 C4 123.0(4) . . ? O1 C3 C4 119.2(3) . . ? C3 C4 P1 106.6(3) . . ? C3 C4 H4A 110.4 . . ? P1 C4 H4A 110.4 . . ? C3 C4 H4B 110.4 . . ? P1 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? C6 C5 C10 119.2(4) . . ? C6 C5 P1 123.4(3) . . ? C10 C5 P1 117.3(3) . . ? C5 C6 C7 119.8(4) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C5 120.7(4) . . ? C9 C10 H10 119.6 . . ? C5 C10 H10 119.6 . . ? C16 C11 C12 118.5(4) . . ? C16 C11 P1 120.2(3) . . ? C12 C11 P1 121.3(3) . . ? C13 C12 C11 120.8(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 118.9(4) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 121.2(4) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C21 C17 C18 110.5(3) . . ? C21 C17 Pd1 106.6(3) . . ? C18 C17 Pd1 102.3(3) . . ? C21 C17 H17 112.3 . . ? C18 C17 H17 112.3 . . ? Pd1 C17 H17 112.3 . . ? C19 C18 C17 111.4(4) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? O2 C19 C18 120.3(4) . . ? O2 C19 C20 119.2(4) . . ? C18 C19 C20 120.5(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 O4 123.2(4) . . ? O3 C21 C17 125.1(4) . . ? O4 C21 C17 111.6(3) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 C24 103.8(3) . . ? N2 C23 H23A 111.0 . . ? C24 C23 H23A 111.0 . . ? N2 C23 H23B 111.0 . . ? C24 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? O5 C24 C23 103.9(3) . . ? O5 C24 H24A 111.0 . . ? C23 C24 H24A 111.0 . . ? O5 C24 H24B 111.0 . . ? C23 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? N2 C25 O5 117.6(3) . . ? N2 C25 C26 122.5(4) . . ? O5 C25 C26 119.9(3) . . ? C25 C26 P2 106.5(2) . . ? C25 C26 H26A 110.4 . . ? P2 C26 H26A 110.4 . . ? C25 C26 H26B 110.4 . . ? P2 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C28 C27 C32 118.3(4) . . ? C28 C27 P2 122.2(3) . . ? C32 C27 P2 119.4(3) . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.1(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 121.0(4) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C38 C33 C34 119.6(4) . . ? C38 C33 P2 120.6(3) . . ? C34 C33 P2 119.8(3) . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 120.0(4) . . ? C33 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C43 C39 C40 111.2(4) . . ? C43 C39 Pd2 105.0(3) . . ? C40 C39 Pd2 102.7(3) . . ? C43 C39 H39 112.4 . . ? C40 C39 H39 112.4 . . ? Pd2 C39 H39 112.4 . . ? C41 C40 C39 112.0(4) . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40B 109.2 . . ? C39 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? O6 C41 C40 120.8(4) . . ? O6 C41 C42 119.5(5) . . ? C40 C41 C42 119.6(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O7 C43 O8 122.0(4) . . ? O7 C43 C39 124.7(4) . . ? O8 C43 C39 113.3(4) . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? F5 C45 F4 103.9(5) . . ? F5 C45 F6 109.1(7) . . ? F4 C45 F6 107.1(5) . . ? F5 C45 S2 112.2(5) . . ? F4 C45 S2 113.7(5) . . ? F6 C45 S2 110.4(4) . . ? F2 C46 F3 110.0(4) . . ? F2 C46 F1 105.7(4) . . ? F3 C46 F1 106.6(4) . . ? F2 C46 S1 112.8(4) . . ? F3 C46 S1 111.9(4) . . ? F1 C46 S1 109.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.254 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.143 data_wel3 _database_code_depnum_ccdc_archive 'CCDC 622177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H29 N O4 P Pd, C F3 S O3' _chemical_formula_sum 'C25 H29 F3 N O7 P Pd S' _chemical_formula_weight 681.92 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.927(5) _cell_length_b 12.268(5) _cell_length_c 13.682(5) _cell_angle_alpha 76.667(5) _cell_angle_beta 87.664(5) _cell_angle_gamma 75.302(5) _cell_volume 1410.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18109 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 6394 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6394 _reflns_number_gt 5427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0983P)^2^+1.7930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6394 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.27598(3) 0.13152(3) 0.73471(2) 0.02520(13) Uani 1 1 d . . . S1 S 1.01897(19) 0.23419(16) 0.46043(12) 0.0558(4) Uani 1 1 d . . . P1 P 0.14849(12) 0.30420(9) 0.75490(8) 0.0243(2) Uani 1 1 d . . . F1 F 1.1732(7) 0.1272(5) 0.3302(4) 0.1018(17) Uani 1 1 d . . . F2 F 1.0531(8) 0.3031(5) 0.2697(4) 0.116(2) Uani 1 1 d . . . F3 F 1.2560(6) 0.2712(5) 0.3555(6) 0.119(2) Uani 1 1 d . . . O1 O 0.4384(4) 0.3999(3) 0.5509(2) 0.0335(7) Uani 1 1 d . . . O4 O 0.1499(4) 0.0697(3) 0.9771(2) 0.0381(8) Uani 1 1 d . . . O3 O 0.2922(5) -0.0977(3) 0.9439(3) 0.0517(10) Uani 1 1 d . . . O2 O 0.3955(4) -0.0388(3) 0.7212(2) 0.0337(7) Uani 1 1 d . . . O5 O 0.9894(7) 0.3482(5) 0.4744(4) 0.0806(15) Uani 1 1 d . . . O6 O 0.8899(7) 0.1928(8) 0.4387(5) 0.109(3) Uani 1 1 d . . . O7 O 1.1233(8) 0.1422(6) 0.5367(4) 0.094(2) Uani 1 1 d . . . N1 N 0.4150(4) 0.2295(3) 0.6439(3) 0.0256(7) Uani 1 1 d . . . C5 C -0.0609(5) 0.3490(4) 0.7653(3) 0.0264(8) Uani 1 1 d . . . C6 C -0.1252(5) 0.3013(4) 0.8553(3) 0.0301(9) Uani 1 1 d . . . H6 H -0.0602 0.2469 0.9070 0.036 Uiso 1 1 calc . . . C7 C -0.2829(5) 0.3336(4) 0.8686(4) 0.0330(9) Uani 1 1 d . . . H7 H -0.3263 0.2995 0.9289 0.040 Uiso 1 1 calc . . . C8 C -0.3784(5) 0.4151(4) 0.7951(4) 0.0348(10) Uani 1 1 d . . . H8 H -0.4868 0.4376 0.8051 0.042 Uiso 1 1 calc . . . C9 C -0.3145(5) 0.4643(4) 0.7057(4) 0.0366(10) Uani 1 1 d . . . H9 H -0.3794 0.5210 0.6552 0.044 Uiso 1 1 calc . . . C10 C -0.1561(5) 0.4301(4) 0.6910(3) 0.0311(9) Uani 1 1 d . . . H10 H -0.1129 0.4624 0.6299 0.037 Uiso 1 1 calc . . . C11 C 0.2185(5) 0.3453(4) 0.8601(3) 0.0300(9) Uani 1 1 d . . . C12 C 0.3337(5) 0.2681(4) 0.9248(3) 0.0315(9) Uani 1 1 d . . . H12 H 0.3807 0.1943 0.9118 0.038 Uiso 1 1 calc . . . C13 C 0.3808(6) 0.2982(5) 1.0088(4) 0.0408(11) Uani 1 1 d . . . H13 H 0.4574 0.2445 1.0540 0.049 Uiso 1 1 calc . . . C14 C 0.3151(7) 0.4066(6) 1.0255(5) 0.0555(16) Uani 1 1 d . . . H14 H 0.3472 0.4273 1.0825 0.067 Uiso 1 1 calc . . . C15 C 0.2036(8) 0.4853(6) 0.9607(6) 0.0628(18) Uani 1 1 d . . . H15 H 0.1607 0.5603 0.9724 0.075 Uiso 1 1 calc . . . C16 C 0.1541(6) 0.4546(5) 0.8781(5) 0.0456(13) Uani 1 1 d . . . H16 H 0.0762 0.5084 0.8339 0.055 Uiso 1 1 calc . . . C4 C 0.1999(5) 0.3997(4) 0.6415(3) 0.0328(10) Uani 1 1 d . . . H4A H 0.1236 0.4138 0.5866 0.039 Uiso 1 1 calc . . . H4B H 0.2026 0.4749 0.6553 0.039 Uiso 1 1 calc . . . C3 C 0.3571(5) 0.3377(4) 0.6134(3) 0.0269(8) Uani 1 1 d . . . C2 C 0.5817(5) 0.3168(4) 0.5329(4) 0.0340(10) Uani 1 1 d . . . H2A H 0.6735 0.3371 0.5547 0.041 Uiso 1 1 calc . . . H2B H 0.5910 0.3161 0.4607 0.041 Uiso 1 1 calc . . . C1 C 0.5680(5) 0.1979(4) 0.5959(3) 0.0276(8) Uani 1 1 d . . . C23 C 0.6938(6) 0.1459(4) 0.6769(4) 0.0376(10) Uani 1 1 d . . . H23A H 0.6882 0.1992 0.7212 0.056 Uiso 1 1 calc . . . H23B H 0.7955 0.1330 0.6455 0.056 Uiso 1 1 calc . . . H23C H 0.6788 0.0720 0.7163 0.056 Uiso 1 1 calc . . . C24 C 0.5637(6) 0.1131(5) 0.5313(4) 0.0377(11) Uani 1 1 d . . . H24A H 0.5545 0.0394 0.5744 0.056 Uiso 1 1 calc . . . H24B H 0.6593 0.1003 0.4930 0.056 Uiso 1 1 calc . . . H24C H 0.4745 0.1449 0.4847 0.056 Uiso 1 1 calc . . . C17 C 0.1300(5) 0.0401(4) 0.8145(3) 0.0308(9) Uani 1 1 d . . . H17 H 0.0212 0.0882 0.8140 0.037 Uiso 1 1 calc . . . C21 C 0.1988(6) -0.0036(4) 0.9164(3) 0.0351(10) Uani 1 1 d . . . C22 C 0.2249(7) 0.0338(6) 1.0753(4) 0.0515(14) Uani 1 1 d . . . H22A H 0.2204 -0.0457 1.1061 0.077 Uiso 1 1 calc . . . H22B H 0.1718 0.0854 1.1179 0.077 Uiso 1 1 calc . . . H22C H 0.3334 0.0374 1.0683 0.077 Uiso 1 1 calc . . . C18 C 0.1442(6) -0.0581(5) 0.7606(4) 0.0421(11) Uani 1 1 d . . . H18A H 0.1007 -0.1196 0.8025 0.050 Uiso 1 1 calc . . . H18B H 0.0852 -0.0285 0.6961 0.050 Uiso 1 1 calc . . . C19 C 0.3102(6) -0.1062(4) 0.7415(3) 0.0344(10) Uani 1 1 d . . . C20 C 0.3710(7) -0.2318(5) 0.7438(4) 0.0438(12) Uani 1 1 d . . . H20A H 0.4808 -0.2473 0.7266 0.066 Uiso 1 1 calc . . . H20B H 0.3129 -0.2531 0.6951 0.066 Uiso 1 1 calc . . . H20C H 0.3592 -0.2774 0.8113 0.066 Uiso 1 1 calc . . . C25 C 1.1332(7) 0.2342(6) 0.3476(5) 0.0608(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0282(2) 0.0241(2) 0.02199(19) -0.00410(13) 0.00356(12) -0.00575(13) S1 0.0505(8) 0.0663(10) 0.0525(8) -0.0217(7) 0.0049(7) -0.0115(7) P1 0.0241(5) 0.0250(5) 0.0222(5) -0.0034(4) 0.0020(4) -0.0052(4) F1 0.107(4) 0.083(3) 0.116(4) -0.062(3) 0.018(3) 0.009(3) F2 0.143(5) 0.105(4) 0.059(3) 0.022(3) -0.006(3) 0.006(4) F3 0.066(3) 0.116(5) 0.174(6) -0.005(4) 0.017(3) -0.049(3) O1 0.0288(16) 0.0295(16) 0.0369(17) 0.0007(13) 0.0076(13) -0.0061(13) O4 0.0425(19) 0.0379(18) 0.0300(16) -0.0041(14) 0.0055(14) -0.0072(15) O3 0.059(2) 0.037(2) 0.041(2) 0.0039(16) 0.0061(18) 0.0081(18) O2 0.0379(17) 0.0291(16) 0.0318(16) -0.0071(13) 0.0065(13) -0.0049(13) O5 0.103(4) 0.054(3) 0.083(4) -0.029(3) -0.006(3) -0.004(3) O6 0.064(3) 0.208(8) 0.091(4) -0.068(5) 0.026(3) -0.074(4) O7 0.106(5) 0.132(6) 0.042(3) 0.001(3) -0.020(3) -0.040(4) N1 0.0272(17) 0.0284(18) 0.0209(16) -0.0049(14) 0.0046(13) -0.0076(14) C5 0.0252(19) 0.029(2) 0.0257(19) -0.0092(16) 0.0019(15) -0.0064(16) C6 0.029(2) 0.029(2) 0.030(2) -0.0055(17) 0.0000(17) -0.0053(17) C7 0.031(2) 0.035(2) 0.033(2) -0.0094(19) 0.0076(18) -0.0071(18) C8 0.024(2) 0.038(2) 0.046(3) -0.017(2) 0.0045(18) -0.0073(18) C9 0.031(2) 0.035(2) 0.041(3) -0.006(2) -0.0054(19) -0.0052(19) C10 0.029(2) 0.032(2) 0.028(2) -0.0014(18) 0.0003(17) -0.0053(17) C11 0.024(2) 0.034(2) 0.034(2) -0.0113(18) 0.0029(16) -0.0081(17) C12 0.0222(19) 0.037(2) 0.035(2) -0.0114(19) 0.0023(17) -0.0048(17) C13 0.032(2) 0.053(3) 0.039(3) -0.014(2) -0.002(2) -0.011(2) C14 0.049(3) 0.075(4) 0.053(3) -0.039(3) -0.005(3) -0.011(3) C15 0.057(4) 0.060(4) 0.079(5) -0.047(4) -0.010(3) 0.001(3) C16 0.036(3) 0.042(3) 0.058(3) -0.023(3) -0.008(2) 0.003(2) C4 0.029(2) 0.028(2) 0.034(2) 0.0023(18) 0.0072(17) -0.0038(17) C3 0.027(2) 0.030(2) 0.0233(19) -0.0031(16) 0.0029(15) -0.0101(17) C2 0.032(2) 0.037(2) 0.033(2) -0.0070(19) 0.0096(18) -0.0097(19) C1 0.031(2) 0.029(2) 0.0229(19) -0.0064(16) 0.0046(16) -0.0081(17) C23 0.034(2) 0.039(3) 0.039(3) -0.010(2) -0.0055(19) -0.005(2) C24 0.040(3) 0.048(3) 0.032(2) -0.019(2) 0.0087(19) -0.015(2) C17 0.030(2) 0.027(2) 0.033(2) -0.0005(18) 0.0042(17) -0.0082(17) C21 0.037(2) 0.032(2) 0.030(2) 0.0025(18) 0.0101(18) -0.0080(19) C22 0.061(4) 0.063(4) 0.028(2) 0.000(2) 0.004(2) -0.019(3) C18 0.043(3) 0.033(3) 0.052(3) -0.010(2) 0.002(2) -0.014(2) C19 0.045(3) 0.033(2) 0.024(2) -0.0049(18) 0.0023(18) -0.010(2) C20 0.058(3) 0.033(3) 0.042(3) -0.014(2) 0.003(2) -0.009(2) C25 0.049(3) 0.053(4) 0.070(4) -0.003(3) 0.006(3) -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 Pd1 C17 2.052(4) . y Pd1 N1 2.114(3) . y Pd1 O2 2.138(3) . y Pd1 P1 2.2091(14) . y S1 O5 1.412(5) . ? S1 O6 1.438(6) . ? S1 O7 1.494(6) . ? S1 C25 1.815(7) . ? P1 C11 1.813(5) . ? P1 C5 1.819(4) . ? P1 C4 1.835(4) . y F1 C25 1.345(8) . ? F2 C25 1.305(8) . ? F3 C25 1.305(8) . ? O1 C3 1.329(5) . ? O1 C2 1.471(5) . ? O4 C21 1.344(6) . ? O4 C22 1.448(6) . ? O3 C21 1.228(6) . ? O2 C19 1.239(6) . y N1 C3 1.273(6) . y N1 C1 1.491(5) . ? C5 C10 1.386(6) . ? C5 C6 1.403(6) . ? C6 C7 1.378(6) . ? C6 H6 0.9500 . ? C7 C8 1.383(7) . ? C7 H7 0.9500 . ? C8 C9 1.401(7) . ? C8 H8 0.9500 . ? C9 C10 1.390(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.392(7) . ? C11 C12 1.390(6) . ? C12 C13 1.396(7) . ? C12 H12 0.9500 . ? C13 C14 1.377(8) . ? C13 H13 0.9500 . ? C14 C15 1.378(9) . ? C14 H14 0.9500 . ? C15 C16 1.391(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C4 C3 1.498(6) . y C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C2 C1 1.545(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 C24 1.522(6) . ? C1 C23 1.519(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C17 C21 1.471(7) . ? C17 C18 1.528(7) . y C17 H17 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C18 C19 1.486(7) . y C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.491(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Pd1 N1 175.94(15) . . y C17 Pd1 O2 80.57(16) . . y N1 Pd1 O2 100.26(13) . . y C17 Pd1 P1 97.25(14) . . y N1 Pd1 P1 81.99(10) . . y O2 Pd1 P1 177.54(9) . . y O5 S1 O6 118.3(4) . . ? O5 S1 O7 116.4(4) . . ? O6 S1 O7 109.2(5) . . ? O5 S1 C25 105.3(3) . . ? O6 S1 C25 103.4(3) . . ? O7 S1 C25 102.0(3) . . ? C11 P1 C5 103.06(19) . . ? C11 P1 C4 106.0(2) . . ? C5 P1 C4 106.8(2) . . ? C11 P1 Pd1 113.89(15) . . ? C5 P1 Pd1 123.95(15) . . ? C4 P1 Pd1 101.86(15) . . ? C3 O1 C2 105.7(3) . . ? C21 O4 C22 115.0(4) . . ? C19 O2 Pd1 111.3(3) . . ? C3 N1 C1 108.7(3) . . ? C3 N1 Pd1 117.5(3) . . ? C1 N1 Pd1 133.4(3) . . ? C10 C5 C6 119.7(4) . . ? C10 C5 P1 123.1(3) . . ? C6 C5 P1 117.1(3) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C5 C10 C9 120.1(4) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C16 C11 C12 119.3(4) . . ? C16 C11 P1 119.9(4) . . ? C12 C11 P1 120.8(3) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 119.4(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 121.0(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.2(5) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C3 C4 P1 105.9(3) . . ? C3 C4 H4A 110.6 . . ? P1 C4 H4A 110.6 . . ? C3 C4 H4B 110.6 . . ? P1 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? N1 C3 O1 118.6(4) . . ? N1 C3 C4 123.8(4) . . ? O1 C3 C4 117.5(4) . . ? O1 C2 C1 105.4(3) . . ? O1 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? N1 C1 C24 109.6(4) . . ? N1 C1 C23 109.4(3) . . ? C24 C1 C23 111.0(4) . . ? N1 C1 C2 101.7(3) . . ? C24 C1 C2 112.5(4) . . ? C23 C1 C2 112.2(4) . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 C24 H24A 109.5 . . ? C1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C17 C18 111.3(4) . . ? C21 C17 Pd1 105.0(3) . . ? C18 C17 Pd1 102.4(3) . . ? C21 C17 H17 112.5 . . ? C18 C17 H17 112.5 . . ? Pd1 C17 H17 112.5 . . ? O3 C21 O4 122.8(5) . . ? O3 C21 C17 123.7(5) . . ? O4 C21 C17 113.6(4) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C18 C17 109.1(4) . . ? C19 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? C19 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? O2 C19 C18 118.3(4) . . ? O2 C19 C20 121.0(5) . . ? C18 C19 C20 120.6(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F2 C25 F3 107.2(6) . . ? F2 C25 F1 107.5(7) . . ? F3 C25 F1 110.7(6) . . ? F2 C25 S1 110.7(5) . . ? F3 C25 S1 110.9(6) . . ? F1 C25 S1 109.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd1 P1 C11 94.4(2) . . . . ? N1 Pd1 P1 C11 -89.64(19) . . . . ? O2 Pd1 P1 C11 66(2) . . . . ? C17 Pd1 P1 C5 -32.2(2) . . . . ? N1 Pd1 P1 C5 143.8(2) . . . . ? O2 Pd1 P1 C5 -60(2) . . . . ? C17 Pd1 P1 C4 -152.0(2) . . . . ? N1 Pd1 P1 C4 23.96(19) . . . . ? O2 Pd1 P1 C4 180(100) . . . . ? C17 Pd1 O2 C19 17.2(3) . . . . ? N1 Pd1 O2 C19 -158.8(3) . . . . ? P1 Pd1 O2 C19 45(2) . . . . ? C17 Pd1 N1 C3 61(2) . . . . ? O2 Pd1 N1 C3 162.3(3) . . . . ? P1 Pd1 N1 C3 -18.7(3) . . . . ? C17 Pd1 N1 C1 -111(2) . . . . ? O2 Pd1 N1 C1 -9.9(4) . . . . ? P1 Pd1 N1 C1 169.0(4) . . . . ? C11 P1 C5 C10 119.1(4) . . . . ? C4 P1 C5 C10 7.7(4) . . . . ? Pd1 P1 C5 C10 -109.8(4) . . . . ? C11 P1 C5 C6 -58.2(4) . . . . ? C4 P1 C5 C6 -169.6(3) . . . . ? Pd1 P1 C5 C6 72.9(4) . . . . ? C10 C5 C6 C7 1.3(7) . . . . ? P1 C5 C6 C7 178.7(4) . . . . ? C5 C6 C7 C8 -1.8(7) . . . . ? C6 C7 C8 C9 0.8(7) . . . . ? C7 C8 C9 C10 0.7(7) . . . . ? C6 C5 C10 C9 0.2(7) . . . . ? P1 C5 C10 C9 -177.1(4) . . . . ? C8 C9 C10 C5 -1.2(7) . . . . ? C5 P1 C11 C16 -46.6(5) . . . . ? C4 P1 C11 C16 65.4(4) . . . . ? Pd1 P1 C11 C16 176.5(4) . . . . ? C5 P1 C11 C12 131.9(4) . . . . ? C4 P1 C11 C12 -116.1(4) . . . . ? Pd1 P1 C11 C12 -5.0(4) . . . . ? C16 C11 C12 C13 2.1(7) . . . . ? P1 C11 C12 C13 -176.4(4) . . . . ? C11 C12 C13 C14 -1.8(8) . . . . ? C12 C13 C14 C15 0.2(10) . . . . ? C13 C14 C15 C16 1.2(11) . . . . ? C12 C11 C16 C15 -0.8(8) . . . . ? P1 C11 C16 C15 177.8(5) . . . . ? C14 C15 C16 C11 -0.9(11) . . . . ? C11 P1 C4 C3 90.5(3) . . . . ? C5 P1 C4 C3 -160.1(3) . . . . ? Pd1 P1 C4 C3 -28.9(3) . . . . ? C1 N1 C3 O1 -1.6(5) . . . . ? Pd1 N1 C3 O1 -175.7(3) . . . . ? C1 N1 C3 C4 176.7(4) . . . . ? Pd1 N1 C3 C4 2.6(6) . . . . ? C2 O1 C3 N1 1.2(5) . . . . ? C2 O1 C3 C4 -177.2(4) . . . . ? P1 C4 C3 N1 19.3(6) . . . . ? P1 C4 C3 O1 -162.4(3) . . . . ? C3 O1 C2 C1 -0.2(5) . . . . ? C3 N1 C1 C24 -118.1(4) . . . . ? Pd1 N1 C1 C24 54.7(5) . . . . ? C3 N1 C1 C23 120.0(4) . . . . ? Pd1 N1 C1 C23 -67.2(5) . . . . ? C3 N1 C1 C2 1.2(4) . . . . ? Pd1 N1 C1 C2 174.0(3) . . . . ? O1 C2 C1 N1 -0.6(4) . . . . ? O1 C2 C1 C24 116.7(4) . . . . ? O1 C2 C1 C23 -117.3(4) . . . . ? N1 Pd1 C17 C21 -174(2) . . . . ? O2 Pd1 C17 C21 83.9(3) . . . . ? P1 Pd1 C17 C21 -94.9(3) . . . . ? N1 Pd1 C17 C18 70(2) . . . . ? O2 Pd1 C17 C18 -32.5(3) . . . . ? P1 Pd1 C17 C18 148.6(3) . . . . ? C22 O4 C21 O3 4.7(7) . . . . ? C22 O4 C21 C17 -175.1(4) . . . . ? C18 C17 C21 O3 19.3(7) . . . . ? Pd1 C17 C21 O3 -90.9(5) . . . . ? C18 C17 C21 O4 -160.9(4) . . . . ? Pd1 C17 C21 O4 88.9(4) . . . . ? C21 C17 C18 C19 -67.1(5) . . . . ? Pd1 C17 C18 C19 44.7(4) . . . . ? Pd1 O2 C19 C18 5.9(5) . . . . ? Pd1 O2 C19 C20 -176.0(4) . . . . ? C17 C18 C19 O2 -35.5(6) . . . . ? C17 C18 C19 C20 146.3(4) . . . . ? O5 S1 C25 F2 -64.1(6) . . . . ? O6 S1 C25 F2 60.7(7) . . . . ? O7 S1 C25 F2 174.0(6) . . . . ? O5 S1 C25 F3 54.8(6) . . . . ? O6 S1 C25 F3 179.5(6) . . . . ? O7 S1 C25 F3 -67.2(6) . . . . ? O5 S1 C25 F1 177.4(5) . . . . ? O6 S1 C25 F1 -57.9(6) . . . . ? O7 S1 C25 F1 55.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.569 _refine_diff_density_min -1.450 _refine_diff_density_rms 0.184