Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _audit_creation_date 10-07-02 _journal_coden_Cambridge 0186 loop_ _publ_author_name 'P. Braunstein' 'Richard Welter' 'Jing Zhang' _publ_contact_author_name 'Prof P Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordn. UMR 7513 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg cedex 67070 FRANCE ; _publ_contact_author_email BRAUNST@CHIMIE.U-STRASBG.FR _publ_section_title ; Monohapto-allyl Pd(II) complexes with bidentate hydrid P,N ligands ; _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. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_cristal_1 _database_code_CSD 193036 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 Cl N O2 P Pd' _chemical_formula_sum 'C23 H29 Cl N O2 P Pd' _chemical_formula_weight 524.29 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.952(5) _cell_length_b 12.957(5) _cell_length_c 18.271(5) _cell_angle_alpha 89.915(5) _cell_angle_beta 89.447(5) _cell_angle_gamma 86.007(5) _cell_volume 2350.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18374 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.990 _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 13632 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.04 _reflns_number_total 13631 _reflns_number_gt 11528 _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^)+(0.0338P)^2^+0.3862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13631 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.276041(13) 0.191279(10) 0.613999(7) 0.02015(4) Uani 1 1 d . . . Pd2 Pd 0.249915(15) -0.286025(11) 0.860637(8) 0.02458(5) Uani 1 1 d . . . Cl1 Cl 0.11043(5) 0.08084(4) 0.65754(3) 0.03764(12) Uani 1 1 d . . . Cl3 Cl 0.42605(7) -0.40782(5) 0.82332(3) 0.04770(15) Uani 1 1 d . . . P1 P 0.42959(4) 0.29027(4) 0.57116(3) 0.01840(9) Uani 1 1 d . . . P2 P 0.08584(5) -0.17793(4) 0.90145(3) 0.02230(10) Uani 1 1 d . . . O3 O 0.13792(13) -0.06522(10) 0.92126(8) 0.0255(3) Uani 1 1 d . . . O1 O 0.36456(12) 0.40548(10) 0.55227(8) 0.0232(3) Uani 1 1 d . . . O4 O 0.38398(16) -0.11525(12) 1.04411(9) 0.0358(4) Uani 1 1 d . . . O2 O 0.11759(16) 0.36805(12) 0.43184(8) 0.0340(3) Uani 1 1 d . . . N1 N 0.16337(16) 0.24916(13) 0.51893(9) 0.0241(3) Uani 1 1 d . . . N2 N 0.35433(16) -0.23205(13) 0.95641(9) 0.0259(3) Uani 1 1 d . . . C1 C 0.49823(18) 0.24380(15) 0.48396(10) 0.0227(4) Uani 1 1 d . . . C13 C 0.21989(18) 0.42985(14) 0.54324(11) 0.0231(4) Uani 1 1 d . . . C24 C 0.02921(19) -0.22572(15) 0.98919(11) 0.0248(4) Uani 1 1 d . . . C36 C 0.28014(19) -0.04851(15) 0.93200(12) 0.0267(4) Uani 1 1 d . . . C7 C 0.57528(18) 0.32412(15) 0.62204(10) 0.0231(4) Uani 1 1 d . . . C25 C 0.0424(2) -0.16950(17) 1.05323(11) 0.0293(4) Uani 1 1 d . . . H25 H 0.0724 -0.1032 1.0511 0.035 Uiso 1 1 calc . . . C8 C 0.5689(2) 0.41263(17) 0.66527(12) 0.0318(4) Uani 1 1 d . . . H8 H 0.4904 0.4560 0.6669 0.038 Uiso 1 1 calc . . . C14 C 0.2106(2) 0.53199(16) 0.50204(13) 0.0330(5) Uani 1 1 d . . . H14A H 0.2467 0.5845 0.5316 0.050 Uiso 1 1 calc . . . H14B H 0.1180 0.5515 0.4914 0.050 Uiso 1 1 calc . . . H14C H 0.2611 0.5246 0.4571 0.050 Uiso 1 1 calc . . . C41 C 0.4238(2) -0.29387(17) 1.01665(12) 0.0315(4) Uani 1 1 d . . . C30 C -0.0642(2) -0.13718(16) 0.85122(11) 0.0265(4) Uani 1 1 d . . . C18 C 0.0990(2) 0.18994(17) 0.45965(12) 0.0302(4) Uani 1 1 d . . . C39 C 0.34249(19) -0.13771(15) 0.97678(11) 0.0258(4) Uani 1 1 d . . . C35 C -0.0579(2) -0.05874(18) 0.79926(12) 0.0345(5) Uani 1 1 d . . . H35 H 0.0221 -0.0271 0.7918 0.041 Uiso 1 1 calc . . . C45 C 0.0701(3) -0.41963(19) 0.79466(13) 0.0395(5) Uani 1 1 d . . . H45 H 0.1242 -0.4789 0.8058 0.047 Uiso 1 1 calc . . . C21 C 0.3883(2) 0.15282(17) 0.70614(11) 0.0301(4) Uani 1 1 d . . . H21A H 0.3859 0.0800 0.7180 0.036 Uiso 1 1 calc . . . H21B H 0.4812 0.1697 0.7000 0.036 Uiso 1 1 calc . . . C10 C 0.7965(3) 0.3713(2) 0.70359(16) 0.0491(7) Uani 1 1 d . . . H10 H 0.8709 0.3876 0.7306 0.059 Uiso 1 1 calc . . . C37 C 0.2797(2) 0.05294(17) 0.97324(15) 0.0386(5) Uani 1 1 d . . . H37A H 0.2396 0.1077 0.9435 0.058 Uiso 1 1 calc . . . H37B H 0.3706 0.0673 0.9845 0.058 Uiso 1 1 calc . . . H37C H 0.2287 0.0481 1.0178 0.058 Uiso 1 1 calc . . . C29 C -0.0174(2) -0.32508(17) 0.99314(12) 0.0312(4) Uani 1 1 d . . . H29 H -0.0254 -0.3635 0.9507 0.037 Uiso 1 1 calc . . . C38 C 0.3511(2) -0.04104(18) 0.85836(14) 0.0385(5) Uani 1 1 d . . . H38A H 0.3097 0.0157 0.8310 0.058 Uiso 1 1 calc . . . H38B H 0.3441 -0.1042 0.8317 0.058 Uiso 1 1 calc . . . H38C H 0.4443 -0.0300 0.8659 0.058 Uiso 1 1 calc . . . C15 C 0.1518(2) 0.43974(17) 0.61824(12) 0.0306(4) Uani 1 1 d . . . H15A H 0.1887 0.4946 0.6451 0.046 Uiso 1 1 calc . . . H15B H 0.1672 0.3759 0.6446 0.046 Uiso 1 1 calc . . . H15C H 0.0568 0.4549 0.6123 0.046 Uiso 1 1 calc . . . C26 C 0.0104(2) -0.2128(2) 1.12055(12) 0.0375(5) Uani 1 1 d . . . H26 H 0.0209 -0.1757 1.1634 0.045 Uiso 1 1 calc . . . C22 C 0.3177(2) 0.21855(19) 0.76224(12) 0.0358(5) Uani 1 1 d . . . H22 H 0.2334 0.1996 0.7774 0.043 Uiso 1 1 calc . . . C27 C -0.0364(3) -0.3100(2) 1.12375(13) 0.0396(5) Uani 1 1 d . . . H27 H -0.0579 -0.3383 1.1688 0.048 Uiso 1 1 calc . . . C6 C 0.5025(2) 0.30895(19) 0.42373(12) 0.0346(5) Uani 1 1 d . . . H6 H 0.4702 0.3778 0.4276 0.042 Uiso 1 1 calc . . . C40 C 0.4149(3) -0.2143(2) 1.07924(13) 0.0409(5) Uani 1 1 d . . . H40A H 0.3444 -0.2294 1.1139 0.049 Uiso 1 1 calc . . . H40B H 0.4997 -0.2147 1.1049 0.049 Uiso 1 1 calc . . . C44 C 0.1393(3) -0.32904(19) 0.77249(12) 0.0376(5) Uani 1 1 d . . . H44A H 0.0746 -0.2732 0.7587 0.045 Uiso 1 1 calc . . . H44B H 0.1982 -0.3455 0.7309 0.045 Uiso 1 1 calc . . . C43 C 0.5693(2) -0.3202(2) 0.99213(15) 0.0419(6) Uani 1 1 d . . . H43A H 0.6120 -0.2576 0.9818 0.063 Uiso 1 1 calc . . . H43B H 0.5703 -0.3621 0.9488 0.063 Uiso 1 1 calc . . . H43C H 0.6171 -0.3577 1.0303 0.063 Uiso 1 1 calc . . . C46 C -0.0616(3) -0.4264(2) 0.80057(17) 0.0536(7) Uani 1 1 d . . . H46A H -0.1200 -0.3693 0.7900 0.064 Uiso 1 1 calc . . . H46B H -0.0957 -0.4882 0.8153 0.064 Uiso 1 1 calc . . . C20 C -0.0418(2) 0.1669(2) 0.48494(16) 0.0449(6) Uani 1 1 d . . . H20A H -0.0934 0.2307 0.4954 0.067 Uiso 1 1 calc . . . H20B H -0.0359 0.1250 0.5283 0.067 Uiso 1 1 calc . . . H20C H -0.0851 0.1306 0.4470 0.067 Uiso 1 1 calc . . . C3 C 0.6031(2) 0.1044(2) 0.41171(14) 0.0427(6) Uani 1 1 d . . . H3 H 0.6380 0.0361 0.4079 0.051 Uiso 1 1 calc . . . C31 C -0.1834(2) -0.18602(19) 0.85979(12) 0.0336(5) Uani 1 1 d . . . H31 H -0.1886 -0.2391 0.8938 0.040 Uiso 1 1 calc . . . C28 C -0.0517(2) -0.36621(18) 1.06039(13) 0.0372(5) Uani 1 1 d . . . H28 H -0.0850 -0.4315 1.0629 0.045 Uiso 1 1 calc . . . C9 C 0.6795(3) 0.4361(2) 0.70590(15) 0.0451(6) Uani 1 1 d . . . H9 H 0.6753 0.4954 0.7347 0.054 Uiso 1 1 calc . . . C11 C 0.8031(2) 0.2830(2) 0.66162(15) 0.0422(6) Uani 1 1 d . . . H11 H 0.8815 0.2396 0.6606 0.051 Uiso 1 1 calc . . . C34 C -0.1709(3) -0.0276(2) 0.75848(14) 0.0443(6) Uani 1 1 d . . . H34 H -0.1670 0.0261 0.7249 0.053 Uiso 1 1 calc . . . C5 C 0.5556(3) 0.2706(2) 0.35741(13) 0.0496(7) Uani 1 1 d . . . H5 H 0.5561 0.3134 0.3165 0.060 Uiso 1 1 calc . . . C2 C 0.5468(2) 0.14079(17) 0.47721(12) 0.0306(4) Uani 1 1 d . . . H2 H 0.5414 0.0962 0.5169 0.037 Uiso 1 1 calc . . . C32 C -0.2951(2) -0.1558(2) 0.81755(15) 0.0438(6) Uani 1 1 d . . . H32 H -0.3743 -0.1893 0.8230 0.053 Uiso 1 1 calc . . . C12 C 0.6928(2) 0.25873(17) 0.62088(13) 0.0315(4) Uani 1 1 d . . . H12 H 0.6971 0.1988 0.5928 0.038 Uiso 1 1 calc . . . C23 C 0.3623(3) 0.3017(2) 0.79306(14) 0.0487(6) Uani 1 1 d . . . H23A H 0.4460 0.3237 0.7797 0.058 Uiso 1 1 calc . . . H23B H 0.3099 0.3381 0.8281 0.058 Uiso 1 1 calc . . . C33 C -0.2886(3) -0.0762(2) 0.76770(15) 0.0477(6) Uani 1 1 d . . . H33 H -0.3639 -0.0553 0.7402 0.057 Uiso 1 1 calc . . . C17 C 0.0948(3) 0.2691(2) 0.39688(13) 0.0433(6) Uani 1 1 d . . . H17A H 0.1646 0.2510 0.3608 0.052 Uiso 1 1 calc . . . H17B H 0.0080 0.2724 0.3730 0.052 Uiso 1 1 calc . . . C4 C 0.6071(3) 0.1695(3) 0.35236(14) 0.0520(7) Uani 1 1 d . . . H4 H 0.6450 0.1450 0.3084 0.062 Uiso 1 1 calc . . . C42 C 0.3509(3) -0.3895(2) 1.03356(16) 0.0454(6) Uani 1 1 d . . . H42A H 0.3596 -0.4360 0.9927 0.068 Uiso 1 1 calc . . . H42B H 0.2573 -0.3703 1.0427 0.068 Uiso 1 1 calc . . . H42C H 0.3895 -0.4230 1.0761 0.068 Uiso 1 1 calc . . . C19 C 0.1841(3) 0.0919(2) 0.44241(15) 0.0443(6) Uani 1 1 d . . . H19A H 0.2721 0.1090 0.4265 0.066 Uiso 1 1 calc . . . H19B H 0.1424 0.0548 0.4043 0.066 Uiso 1 1 calc . . . H19C H 0.1920 0.0494 0.4855 0.066 Uiso 1 1 calc . . . C16 C 0.16457(18) 0.34331(15) 0.49854(11) 0.0232(4) 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 0.02093(7) 0.01877(7) 0.02056(7) 0.00112(5) 0.00423(5) -0.00074(5) Pd2 0.03071(8) 0.02055(8) 0.02206(8) -0.00337(6) 0.00364(6) 0.00076(6) Cl1 0.0327(3) 0.0331(3) 0.0476(3) 0.0101(2) 0.0103(2) -0.0077(2) Cl3 0.0572(4) 0.0427(3) 0.0397(3) -0.0099(3) 0.0077(3) 0.0208(3) P1 0.0175(2) 0.0176(2) 0.0199(2) -0.00077(16) 0.00196(16) 0.00034(16) P2 0.0229(2) 0.0213(2) 0.0226(2) -0.00209(18) 0.00122(17) -0.00137(17) O3 0.0213(6) 0.0208(6) 0.0344(8) -0.0031(6) 0.0000(5) -0.0001(5) O1 0.0176(6) 0.0186(6) 0.0331(7) 0.0010(5) -0.0004(5) 0.0011(5) O4 0.0363(8) 0.0342(8) 0.0364(9) -0.0093(7) -0.0105(7) 0.0021(6) O2 0.0389(8) 0.0347(8) 0.0286(8) 0.0055(6) -0.0110(6) -0.0023(7) N1 0.0235(7) 0.0262(8) 0.0231(8) -0.0019(6) -0.0003(6) -0.0054(6) N2 0.0243(8) 0.0236(8) 0.0294(9) -0.0005(7) 0.0003(6) 0.0014(6) C1 0.0186(8) 0.0272(9) 0.0224(9) -0.0022(7) 0.0026(6) -0.0029(7) C13 0.0188(8) 0.0199(9) 0.0302(10) 0.0005(7) -0.0005(7) 0.0024(6) C24 0.0234(9) 0.0260(9) 0.0244(9) 0.0005(7) 0.0025(7) 0.0020(7) C36 0.0231(9) 0.0207(9) 0.0364(11) -0.0009(8) 0.0016(8) -0.0018(7) C7 0.0212(8) 0.0243(9) 0.0236(9) -0.0009(7) -0.0002(7) -0.0005(7) C25 0.0300(10) 0.0306(10) 0.0267(10) -0.0032(8) 0.0027(8) 0.0013(8) C8 0.0278(10) 0.0333(11) 0.0337(11) -0.0090(9) -0.0011(8) 0.0019(8) C14 0.0305(10) 0.0219(10) 0.0461(13) 0.0063(9) -0.0042(9) 0.0018(8) C41 0.0294(10) 0.0286(10) 0.0355(11) 0.0029(9) -0.0058(8) 0.0056(8) C30 0.0251(9) 0.0302(10) 0.0242(9) -0.0039(8) 0.0008(7) -0.0012(7) C18 0.0309(10) 0.0318(11) 0.0288(10) -0.0051(8) -0.0045(8) -0.0074(8) C39 0.0200(8) 0.0257(9) 0.0317(10) -0.0034(8) 0.0011(7) -0.0012(7) C35 0.0344(11) 0.0375(12) 0.0319(11) 0.0043(9) -0.0016(9) -0.0055(9) C45 0.0519(14) 0.0345(12) 0.0324(12) -0.0117(9) -0.0062(10) -0.0048(10) C21 0.0331(10) 0.0338(11) 0.0230(9) 0.0089(8) 0.0012(8) -0.0005(8) C10 0.0349(12) 0.0601(17) 0.0523(16) -0.0178(13) -0.0167(11) 0.0000(11) C37 0.0300(11) 0.0226(10) 0.0632(16) -0.0109(10) -0.0057(10) -0.0007(8) C29 0.0365(11) 0.0301(10) 0.0273(10) 0.0000(8) 0.0007(8) -0.0051(8) C38 0.0369(12) 0.0306(11) 0.0475(14) 0.0081(10) 0.0119(10) 0.0001(9) C15 0.0279(10) 0.0291(10) 0.0341(11) -0.0069(8) 0.0043(8) 0.0041(8) C26 0.0421(12) 0.0452(13) 0.0243(10) -0.0055(9) 0.0035(9) 0.0029(10) C22 0.0401(12) 0.0438(13) 0.0226(10) 0.0066(9) -0.0025(8) 0.0038(10) C27 0.0419(13) 0.0479(14) 0.0278(11) 0.0081(10) 0.0062(9) 0.0034(10) C6 0.0407(12) 0.0376(12) 0.0254(10) 0.0042(9) 0.0060(9) -0.0034(9) C40 0.0441(13) 0.0438(14) 0.0334(12) -0.0010(10) -0.0086(10) 0.0078(10) C44 0.0526(14) 0.0379(12) 0.0224(10) -0.0065(9) -0.0033(9) -0.0025(10) C43 0.0304(11) 0.0378(13) 0.0560(16) -0.0032(11) -0.0050(10) 0.0088(9) C46 0.0613(18) 0.0483(16) 0.0528(17) -0.0184(13) -0.0079(13) -0.0130(13) C20 0.0320(12) 0.0479(15) 0.0564(16) -0.0078(12) -0.0047(11) -0.0139(10) C3 0.0399(12) 0.0450(14) 0.0424(13) -0.0218(11) 0.0057(10) 0.0019(10) C31 0.0282(10) 0.0408(12) 0.0319(11) 0.0005(9) 0.0006(8) -0.0040(9) C28 0.0427(13) 0.0333(12) 0.0359(12) 0.0064(9) 0.0043(9) -0.0058(9) C9 0.0404(13) 0.0466(14) 0.0484(15) -0.0237(12) -0.0091(11) -0.0004(11) C11 0.0286(11) 0.0489(14) 0.0479(14) -0.0106(11) -0.0112(10) 0.0070(10) C34 0.0470(14) 0.0489(15) 0.0368(13) 0.0118(11) -0.0100(10) 0.0001(11) C5 0.0585(16) 0.0668(19) 0.0240(11) 0.0043(11) 0.0108(11) -0.0086(14) C2 0.0315(10) 0.0296(10) 0.0302(10) -0.0060(8) 0.0017(8) 0.0011(8) C32 0.0261(11) 0.0599(16) 0.0457(14) -0.0002(12) -0.0026(10) -0.0057(10) C12 0.0260(10) 0.0304(11) 0.0373(11) -0.0081(9) -0.0045(8) 0.0042(8) C23 0.0652(17) 0.0543(16) 0.0267(12) 0.0026(11) -0.0040(11) -0.0034(13) C33 0.0385(13) 0.0648(18) 0.0385(13) 0.0033(12) -0.0105(10) 0.0065(12) C17 0.0565(15) 0.0456(14) 0.0291(11) -0.0022(10) -0.0112(10) -0.0119(12) C4 0.0511(15) 0.075(2) 0.0300(13) -0.0195(13) 0.0132(11) -0.0067(14) C42 0.0461(14) 0.0376(13) 0.0522(15) 0.0174(11) -0.0064(11) -0.0008(11) C19 0.0471(14) 0.0404(13) 0.0456(14) -0.0194(11) -0.0027(11) -0.0031(11) C16 0.0191(8) 0.0258(9) 0.0245(9) 0.0015(7) 0.0006(7) 0.0007(7) _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 C21 2.070(2) . ? Pd1 N1 2.1803(17) . ? Pd1 P1 2.2000(8) . ? Pd1 Cl1 2.3868(9) . ? Pd2 C44 2.059(2) . ? Pd2 N2 2.1842(18) . ? Pd2 P2 2.2012(8) . ? Pd2 Cl3 2.3713(9) . ? P1 O1 1.6231(14) . ? P1 C7 1.810(2) . ? P1 C1 1.8144(19) . ? P2 O3 1.6257(15) . ? P2 C30 1.807(2) . ? P2 C24 1.816(2) . ? O3 C36 1.462(2) . ? O1 C13 1.463(2) . ? O4 C39 1.340(3) . ? O4 C40 1.449(3) . ? O2 C16 1.340(2) . ? O2 C17 1.466(3) . ? N1 C16 1.276(3) . ? N1 C18 1.502(3) . ? N2 C39 1.276(3) . ? N2 C41 1.505(3) . ? C1 C6 1.388(3) . ? C1 C2 1.393(3) . ? C13 C14 1.519(3) . ? C13 C15 1.524(3) . ? C13 C16 1.525(3) . ? C24 C25 1.391(3) . ? C24 C29 1.400(3) . ? C36 C39 1.516(3) . ? C36 C37 1.516(3) . ? C36 C38 1.519(3) . ? C7 C8 1.391(3) . ? C7 C12 1.395(3) . ? C25 C26 1.394(3) . ? C25 H25 0.9300 . ? C8 C9 1.385(3) . ? C8 H8 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C41 C42 1.509(3) . ? C41 C43 1.528(3) . ? C41 C40 1.539(3) . ? C30 C31 1.390(3) . ? C30 C35 1.394(3) . ? C18 C19 1.509(3) . ? C18 C20 1.521(3) . ? C18 C17 1.537(3) . ? C35 C34 1.391(3) . ? C35 H35 0.9300 . ? C45 C46 1.323(4) . ? C45 C44 1.457(4) . ? C45 H45 0.9300 . ? C21 C22 1.475(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C10 C11 1.375(4) . ? C10 C9 1.388(4) . ? C10 H10 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C29 C28 1.388(3) . ? C29 H29 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C26 C27 1.375(4) . ? C26 H26 0.9300 . ? C22 C23 1.322(4) . ? C22 H22 0.9300 . ? C27 C28 1.384(4) . ? C27 H27 0.9300 . ? C6 C5 1.395(3) . ? C6 H6 0.9300 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C46 H46A 0.9300 . ? C46 H46B 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C3 C4 1.375(4) . ? C3 C2 1.386(3) . ? C3 H3 0.9300 . ? C31 C32 1.393(3) . ? C31 H31 0.9300 . ? C28 H28 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.387(3) . ? C11 H11 0.9300 . ? C34 C33 1.376(4) . ? C34 H34 0.9300 . ? C5 C4 1.376(4) . ? C5 H5 0.9300 . ? C2 H2 0.9300 . ? C32 C33 1.379(4) . ? C32 H32 0.9300 . ? C12 H12 0.9300 . ? C23 H23A 0.9300 . ? C23 H23B 0.9300 . ? C33 H33 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C4 H4 0.9300 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 C21 Pd1 N1 173.73(8) . . ? C21 Pd1 P1 92.31(7) . . ? N1 Pd1 P1 83.22(5) . . ? C21 Pd1 Cl1 88.43(7) . . ? N1 Pd1 Cl1 96.15(5) . . ? P1 Pd1 Cl1 178.40(2) . . ? C44 Pd2 N2 175.62(8) . . ? C44 Pd2 P2 92.72(7) . . ? N2 Pd2 P2 82.90(5) . . ? C44 Pd2 Cl3 88.99(8) . . ? N2 Pd2 Cl3 95.39(5) . . ? P2 Pd2 Cl3 176.61(2) . . ? O1 P1 C7 99.45(8) . . ? O1 P1 C1 103.52(8) . . ? C7 P1 C1 104.33(9) . . ? O1 P1 Pd1 111.25(6) . . ? C7 P1 Pd1 124.08(7) . . ? C1 P1 Pd1 111.83(7) . . ? O3 P2 C30 99.39(9) . . ? O3 P2 C24 103.45(9) . . ? C30 P2 C24 106.45(9) . . ? O3 P2 Pd2 112.23(6) . . ? C30 P2 Pd2 125.14(7) . . ? C24 P2 Pd2 108.03(7) . . ? C36 O3 P2 122.56(12) . . ? C13 O1 P1 123.23(11) . . ? C39 O4 C40 105.42(17) . . ? C16 O2 C17 105.29(17) . . ? C16 N1 C18 108.08(17) . . ? C16 N1 Pd1 121.52(13) . . ? C18 N1 Pd1 129.29(13) . . ? C39 N2 C41 107.67(17) . . ? C39 N2 Pd2 121.89(14) . . ? C41 N2 Pd2 129.28(13) . . ? C6 C1 C2 119.40(19) . . ? C6 C1 P1 121.17(16) . . ? C2 C1 P1 119.43(15) . . ? O1 C13 C14 104.35(15) . . ? O1 C13 C15 109.49(16) . . ? C14 C13 C15 111.69(17) . . ? O1 C13 C16 107.91(14) . . ? C14 C13 C16 111.72(17) . . ? C15 C13 C16 111.35(16) . . ? C25 C24 C29 119.41(19) . . ? C25 C24 P2 121.31(16) . . ? C29 C24 P2 119.03(15) . . ? O3 C36 C39 108.32(15) . . ? O3 C36 C37 104.83(16) . . ? C39 C36 C37 111.53(19) . . ? O3 C36 C38 109.98(18) . . ? C39 C36 C38 111.05(17) . . ? C37 C36 C38 110.91(19) . . ? C8 C7 C12 119.58(18) . . ? C8 C7 P1 120.33(15) . . ? C12 C7 P1 120.01(15) . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C41 C42 110.73(18) . . ? N2 C41 C43 107.64(19) . . ? C42 C41 C43 112.0(2) . . ? N2 C41 C40 100.77(17) . . ? C42 C41 C40 113.2(2) . . ? C43 C41 C40 111.78(19) . . ? C31 C30 C35 119.0(2) . . ? C31 C30 P2 121.82(17) . . ? C35 C30 P2 119.04(16) . . ? N1 C18 C19 110.13(18) . . ? N1 C18 C20 108.54(18) . . ? C19 C18 C20 111.5(2) . . ? N1 C18 C17 101.12(17) . . ? C19 C18 C17 113.4(2) . . ? C20 C18 C17 111.6(2) . . ? N2 C39 O4 117.91(19) . . ? N2 C39 C36 125.29(19) . . ? O4 C39 C36 116.76(17) . . ? C34 C35 C30 120.3(2) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C46 C45 C44 126.8(3) . . ? C46 C45 H45 116.6 . . ? C44 C45 H45 116.6 . . ? C22 C21 Pd1 101.49(14) . . ? C22 C21 H21A 111.5 . . ? Pd1 C21 H21A 111.5 . . ? C22 C21 H21B 111.5 . . ? Pd1 C21 H21B 111.5 . . ? H21A C21 H21B 109.3 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C29 C24 120.0(2) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C27 C26 C25 120.2(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C23 C22 C21 126.5(2) . . ? C23 C22 H22 116.8 . . ? C21 C22 H22 116.8 . . ? C26 C27 C28 120.5(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C1 C6 C5 119.7(2) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? O4 C40 C41 105.21(18) . . ? O4 C40 H40A 110.7 . . ? C41 C40 H40A 110.7 . . ? O4 C40 H40B 110.7 . . ? C41 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? C45 C44 Pd2 107.17(16) . . ? C45 C44 H44A 110.3 . . ? Pd2 C44 H44A 110.3 . . ? C45 C44 H44B 110.3 . . ? Pd2 C44 H44B 110.3 . . ? H44A C44 H44B 108.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C46 H46A 120.0 . . ? C45 C46 H46B 120.0 . . ? H46A C46 H46B 120.0 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C3 C2 119.8(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C30 C31 C32 120.2(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C28 C29 119.9(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C8 C9 C10 120.0(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C33 C34 C35 120.2(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C3 C2 C1 120.4(2) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C33 C32 C31 120.1(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C22 C23 H23A 120.0 . . ? C22 C23 H23B 120.0 . . ? H23A C23 H23B 120.0 . . ? C34 C33 C32 120.2(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? O2 C17 C18 104.96(18) . . ? O2 C17 H17A 110.8 . . ? C18 C17 H17A 110.8 . . ? O2 C17 H17B 110.8 . . ? C18 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? 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 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C16 O2 117.87(18) . . ? N1 C16 C13 125.05(17) . . ? O2 C16 C13 117.05(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 C21 Pd1 P1 O1 -126.70(9) . . . . ? N1 Pd1 P1 O1 48.90(7) . . . . ? Cl1 Pd1 P1 O1 115.9(7) . . . . ? C21 Pd1 P1 C7 -8.29(10) . . . . ? N1 Pd1 P1 C7 167.31(9) . . . . ? Cl1 Pd1 P1 C7 -125.7(7) . . . . ? C21 Pd1 P1 C1 118.08(9) . . . . ? N1 Pd1 P1 C1 -66.32(8) . . . . ? Cl1 Pd1 P1 C1 0.7(7) . . . . ? C44 Pd2 P2 O3 -131.61(9) . . . . ? N2 Pd2 P2 O3 48.18(8) . . . . ? Cl3 Pd2 P2 O3 108.0(4) . . . . ? C44 Pd2 P2 C30 -11.39(11) . . . . ? N2 Pd2 P2 C30 168.40(10) . . . . ? Cl3 Pd2 P2 C30 -131.7(4) . . . . ? C44 Pd2 P2 C24 114.99(10) . . . . ? N2 Pd2 P2 C24 -65.22(9) . . . . ? Cl3 Pd2 P2 C24 -5.4(4) . . . . ? C30 P2 O3 C36 -151.64(15) . . . . ? C24 P2 O3 C36 98.81(16) . . . . ? Pd2 P2 O3 C36 -17.39(16) . . . . ? C7 P1 O1 C13 -149.95(14) . . . . ? C1 P1 O1 C13 102.70(15) . . . . ? Pd1 P1 O1 C13 -17.56(15) . . . . ? C21 Pd1 N1 C16 4.8(7) . . . . ? P1 Pd1 N1 C16 -39.84(15) . . . . ? Cl1 Pd1 N1 C16 141.65(15) . . . . ? C21 Pd1 N1 C18 171.2(6) . . . . ? P1 Pd1 N1 C18 126.58(16) . . . . ? Cl1 Pd1 N1 C18 -51.93(16) . . . . ? C44 Pd2 N2 C39 -36.1(11) . . . . ? P2 Pd2 N2 C39 -38.80(15) . . . . ? Cl3 Pd2 N2 C39 144.14(16) . . . . ? C44 Pd2 N2 C41 130.0(10) . . . . ? P2 Pd2 N2 C41 127.28(16) . . . . ? Cl3 Pd2 N2 C41 -49.78(16) . . . . ? O1 P1 C1 C6 8.21(19) . . . . ? C7 P1 C1 C6 -95.43(18) . . . . ? Pd1 P1 C1 C6 128.08(16) . . . . ? O1 P1 C1 C2 -171.43(15) . . . . ? C7 P1 C1 C2 84.94(17) . . . . ? Pd1 P1 C1 C2 -51.56(17) . . . . ? P1 O1 C13 C14 -161.40(14) . . . . ? P1 O1 C13 C15 78.91(18) . . . . ? P1 O1 C13 C16 -42.4(2) . . . . ? O3 P2 C24 C25 -2.83(18) . . . . ? C30 P2 C24 C25 -107.04(18) . . . . ? Pd2 P2 C24 C25 116.30(16) . . . . ? O3 P2 C24 C29 -177.10(16) . . . . ? C30 P2 C24 C29 78.69(18) . . . . ? Pd2 P2 C24 C29 -57.97(17) . . . . ? P2 O3 C36 C39 -42.3(2) . . . . ? P2 O3 C36 C37 -161.49(15) . . . . ? P2 O3 C36 C38 79.22(19) . . . . ? O1 P1 C7 C8 33.33(19) . . . . ? C1 P1 C7 C8 140.02(18) . . . . ? Pd1 P1 C7 C8 -90.47(18) . . . . ? O1 P1 C7 C12 -149.80(17) . . . . ? C1 P1 C7 C12 -43.11(19) . . . . ? Pd1 P1 C7 C12 86.41(18) . . . . ? C29 C24 C25 C26 0.6(3) . . . . ? P2 C24 C25 C26 -173.60(17) . . . . ? C12 C7 C8 C9 1.0(3) . . . . ? P1 C7 C8 C9 177.9(2) . . . . ? C39 N2 C41 C42 132.7(2) . . . . ? Pd2 N2 C41 C42 -35.0(3) . . . . ? C39 N2 C41 C43 -104.6(2) . . . . ? Pd2 N2 C41 C43 87.8(2) . . . . ? C39 N2 C41 C40 12.6(2) . . . . ? Pd2 N2 C41 C40 -155.00(15) . . . . ? O3 P2 C30 C31 -139.22(18) . . . . ? C24 P2 C30 C31 -32.1(2) . . . . ? Pd2 P2 C30 C31 94.95(18) . . . . ? O3 P2 C30 C35 44.70(19) . . . . ? C24 P2 C30 C35 151.84(17) . . . . ? Pd2 P2 C30 C35 -81.12(19) . . . . ? C16 N1 C18 C19 132.0(2) . . . . ? Pd1 N1 C18 C19 -35.9(2) . . . . ? C16 N1 C18 C20 -105.7(2) . . . . ? Pd1 N1 C18 C20 86.4(2) . . . . ? C16 N1 C18 C17 11.7(2) . . . . ? Pd1 N1 C18 C17 -156.10(15) . . . . ? C41 N2 C39 O4 -3.5(2) . . . . ? Pd2 N2 C39 O4 165.23(13) . . . . ? C41 N2 C39 C36 178.95(18) . . . . ? Pd2 N2 C39 C36 -12.3(3) . . . . ? C40 O4 C39 N2 -8.2(2) . . . . ? C40 O4 C39 C36 169.61(18) . . . . ? O3 C36 C39 N2 64.0(2) . . . . ? C37 C36 C39 N2 178.9(2) . . . . ? C38 C36 C39 N2 -56.9(3) . . . . ? O3 C36 C39 O4 -113.58(19) . . . . ? C37 C36 C39 O4 1.3(2) . . . . ? C38 C36 C39 O4 125.5(2) . . . . ? C31 C30 C35 C34 2.2(4) . . . . ? P2 C30 C35 C34 178.4(2) . . . . ? N1 Pd1 C21 C22 58.6(7) . . . . ? P1 Pd1 C21 C22 102.88(14) . . . . ? Cl1 Pd1 C21 C22 -78.54(14) . . . . ? C25 C24 C29 C28 0.8(3) . . . . ? P2 C24 C29 C28 175.20(18) . . . . ? C24 C25 C26 C27 -1.2(3) . . . . ? Pd1 C21 C22 C23 -108.0(2) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? C2 C1 C6 C5 -0.2(3) . . . . ? P1 C1 C6 C5 -179.79(19) . . . . ? C39 O4 C40 C41 15.6(2) . . . . ? N2 C41 C40 O4 -16.8(2) . . . . ? C42 C41 C40 O4 -135.1(2) . . . . ? C43 C41 C40 O4 97.3(2) . . . . ? C46 C45 C44 Pd2 116.0(3) . . . . ? N2 Pd2 C44 C45 -94.9(11) . . . . ? P2 Pd2 C44 C45 -92.20(17) . . . . ? Cl3 Pd2 C44 C45 84.87(17) . . . . ? C35 C30 C31 C32 -0.8(3) . . . . ? P2 C30 C31 C32 -176.88(19) . . . . ? C26 C27 C28 C29 1.2(4) . . . . ? C24 C29 C28 C27 -1.7(4) . . . . ? C7 C8 C9 C10 -0.2(4) . . . . ? C11 C10 C9 C8 -0.6(5) . . . . ? C9 C10 C11 C12 0.5(5) . . . . ? C30 C35 C34 C33 -1.9(4) . . . . ? C1 C6 C5 C4 -2.0(4) . . . . ? C4 C3 C2 C1 -2.1(4) . . . . ? C6 C1 C2 C3 2.2(3) . . . . ? P1 C1 C2 C3 -178.19(17) . . . . ? C30 C31 C32 C33 -0.9(4) . . . . ? C10 C11 C12 C7 0.4(4) . . . . ? C8 C7 C12 C11 -1.1(4) . . . . ? P1 C7 C12 C11 -178.0(2) . . . . ? C35 C34 C33 C32 0.2(4) . . . . ? C31 C32 C33 C34 1.2(4) . . . . ? C16 O2 C17 C18 14.8(2) . . . . ? N1 C18 C17 O2 -15.7(2) . . . . ? C19 C18 C17 O2 -133.6(2) . . . . ? C20 C18 C17 O2 99.5(2) . . . . ? C6 C5 C4 C3 2.1(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C18 N1 C16 O2 -2.9(2) . . . . ? Pd1 N1 C16 O2 166.08(13) . . . . ? C18 N1 C16 C13 179.30(17) . . . . ? Pd1 N1 C16 C13 -11.7(3) . . . . ? C17 O2 C16 N1 -8.0(2) . . . . ? C17 O2 C16 C13 169.97(17) . . . . ? O1 C13 C16 N1 63.8(2) . . . . ? C14 C13 C16 N1 177.97(19) . . . . ? C15 C13 C16 N1 -56.4(2) . . . . ? O1 C13 C16 O2 -114.00(18) . . . . ? C14 C13 C16 O2 0.1(2) . . . . ? C15 C13 C16 O2 125.81(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.688 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.087 data_cristal_2 _database_code_CSD 193037 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 F6 N O2 P2 Pd' _chemical_formula_sum 'C23 H29 F6 N O2 P2 Pd' _chemical_formula_weight 633.81 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' 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' '-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 15.136(5) _cell_length_b 17.392(5) _cell_length_c 20.248(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 5330(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16867 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 33.142 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.879 _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 10142 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 33.15 _reflns_number_total 10141 _reflns_number_gt 6781 _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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10141 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.182729(10) 0.080840(9) 0.600684(8) 0.02718(6) Uani 1 1 d . . . P1 P 0.29611(3) 0.02820(3) 0.54538(2) 0.02352(10) Uani 1 1 d . . . P2 P -0.00240(4) -0.16420(4) 0.65912(3) 0.03634(14) Uani 1 1 d . . . F1 F 0.09643(11) -0.14225(14) 0.67660(10) 0.0808(6) Uani 1 1 d . . . F2 F 0.01426(13) -0.14559(15) 0.58396(9) 0.0818(7) Uani 1 1 d . . . F3 F -0.10116(11) -0.18737(11) 0.64265(9) 0.0623(5) Uani 1 1 d . . . F4 F -0.01927(13) -0.18231(15) 0.73456(8) 0.0821(6) Uani 1 1 d . . . F5 F 0.02761(17) -0.25017(12) 0.64763(11) 0.0887(7) Uani 1 1 d . . . F6 F -0.03496(17) -0.07843(11) 0.67140(13) 0.0877(7) Uani 1 1 d . . . O1 O 0.38681(9) 0.03309(8) 0.58732(7) 0.0272(3) Uani 1 1 d . . . O2 O 0.38290(13) 0.11048(10) 0.74719(8) 0.0454(4) Uani 1 1 d . . . N N 0.26685(12) 0.11394(10) 0.67893(8) 0.0292(4) Uani 1 1 d . . . C13 C 0.39111(14) 0.02049(12) 0.65809(10) 0.0298(4) Uani 1 1 d . . . C7 C 0.28945(15) -0.07069(12) 0.51866(10) 0.0288(4) Uani 1 1 d . . . C1 C 0.33176(17) 0.07927(13) 0.47234(12) 0.0352(5) Uani 1 1 d . . . C15 C 0.35107(19) -0.05655(14) 0.67796(12) 0.0403(5) Uani 1 1 d . . . H15A H 0.3820 -0.0974 0.6560 0.061 Uiso 1 1 calc . . . H15B H 0.2899 -0.0577 0.6656 0.061 Uiso 1 1 calc . . . H15C H 0.3561 -0.0631 0.7249 0.061 Uiso 1 1 calc . . . C18 C 0.24379(17) 0.17027(13) 0.73260(12) 0.0403(6) Uani 1 1 d . . . C14 C 0.48945(17) 0.02359(16) 0.67287(13) 0.0469(6) Uani 1 1 d . . . H14A H 0.5189 -0.0173 0.6498 0.070 Uiso 1 1 calc . . . H14B H 0.4987 0.0179 0.7195 0.070 Uiso 1 1 calc . . . H14C H 0.5128 0.0721 0.6586 0.070 Uiso 1 1 calc . . . C21 C 0.08711(17) 0.0534(2) 0.52918(15) 0.0556(7) Uani 1 1 d . . . H21A H 0.0997 0.0699 0.4844 0.067 Uiso 1 1 calc . . . H21B H 0.0624 0.0020 0.5315 0.067 Uiso 1 1 calc . . . C8 C 0.21870(16) -0.11645(14) 0.53605(13) 0.0396(5) Uani 1 1 d . . . H8 H 0.1722 -0.0962 0.5605 0.048 Uiso 1 1 calc . . . C19 C 0.2140(2) 0.24646(15) 0.70383(15) 0.0550(7) Uani 1 1 d . . . H19A H 0.1588 0.2396 0.6812 0.082 Uiso 1 1 calc . . . H19B H 0.2577 0.2648 0.6733 0.082 Uiso 1 1 calc . . . H19C H 0.2067 0.2832 0.7388 0.082 Uiso 1 1 calc . . . C20 C 0.1729(2) 0.13397(18) 0.77595(14) 0.0554(8) Uani 1 1 d . . . H20A H 0.1187 0.1302 0.7515 0.083 Uiso 1 1 calc . . . H20B H 0.1638 0.1653 0.8144 0.083 Uiso 1 1 calc . . . H20C H 0.1915 0.0835 0.7892 0.083 Uiso 1 1 calc . . . C12 C 0.35914(16) -0.10179(14) 0.48171(12) 0.0379(5) Uani 1 1 d . . . H12 H 0.4068 -0.0710 0.4699 0.045 Uiso 1 1 calc . . . C16 C 0.34174(16) 0.08463(11) 0.69288(10) 0.0294(4) Uani 1 1 d . . . C23 C 0.0449(2) 0.1204(2) 0.62870(19) 0.0698(10) Uani 1 1 d . . . H23A H 0.0099 0.0855 0.6553 0.084 Uiso 1 1 calc . . . H23B H 0.0382 0.1741 0.6408 0.084 Uiso 1 1 calc . . . C17 C 0.3318(2) 0.17732(17) 0.76836(13) 0.0511(7) Uani 1 1 d . . . H17A H 0.3615 0.2246 0.7562 0.061 Uiso 1 1 calc . . . H17B H 0.3232 0.1768 0.8158 0.061 Uiso 1 1 calc . . . C5 C 0.3136(4) 0.1081(3) 0.35746(16) 0.0917(17) Uani 1 1 d . . . H5 H 0.2824 0.1022 0.3182 0.110 Uiso 1 1 calc . . . C22 C 0.0508(2) 0.1057(4) 0.5687(3) 0.140(3) Uani 1 1 d . . . H22 H 0.0206 0.1423 0.5440 0.168 Uiso 1 1 calc . . . C11 C 0.3572(2) -0.17806(14) 0.46278(13) 0.0471(6) Uani 1 1 d . . . H11 H 0.4038 -0.1989 0.4388 0.057 Uiso 1 1 calc . . . C2 C 0.40322(19) 0.12846(14) 0.47438(15) 0.0515(7) Uani 1 1 d . . . H2 H 0.4334 0.1370 0.5137 0.062 Uiso 1 1 calc . . . C4 C 0.3843(4) 0.1539(3) 0.3582(2) 0.102(2) Uani 1 1 d . . . H4 H 0.4030 0.1780 0.3197 0.122 Uiso 1 1 calc . . . C10 C 0.2851(2) -0.22362(15) 0.47976(15) 0.0525(7) Uani 1 1 d . . . H10 H 0.2828 -0.2746 0.4661 0.063 Uiso 1 1 calc . . . C6 C 0.2846(2) 0.06877(18) 0.41346(14) 0.0570(8) Uani 1 1 d . . . H6 H 0.2356 0.0366 0.4118 0.068 Uiso 1 1 calc . . . C9 C 0.2174(2) -0.19349(16) 0.51656(15) 0.0537(7) Uani 1 1 d . . . H9 H 0.1702 -0.2246 0.5287 0.064 Uiso 1 1 calc . . . C3 C 0.4293(3) 0.16532(19) 0.4162(2) 0.0851(14) Uani 1 1 d . . . H3 H 0.4779 0.1980 0.4168 0.102 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 Pd 0.02287(8) 0.02740(9) 0.03127(9) -0.00056(6) 0.00235(6) 0.00242(6) P1 0.0241(2) 0.0237(2) 0.0228(2) -0.00210(18) 0.00003(18) 0.00028(18) P2 0.0329(3) 0.0476(4) 0.0285(3) -0.0034(2) -0.0017(2) -0.0012(3) F1 0.0424(10) 0.1341(19) 0.0660(12) 0.0007(12) -0.0071(9) -0.0266(11) F2 0.0661(12) 0.143(2) 0.0364(9) 0.0242(11) 0.0062(9) 0.0132(13) F3 0.0397(9) 0.0786(12) 0.0684(11) -0.0104(9) -0.0120(8) -0.0097(8) F4 0.0681(12) 0.144(2) 0.0338(9) 0.0073(10) 0.0037(8) -0.0103(13) F5 0.0974(17) 0.0618(12) 0.1069(18) -0.0116(12) -0.0245(12) 0.0347(11) F6 0.0986(18) 0.0510(11) 0.1135(19) -0.0228(11) 0.0010(15) 0.0035(10) O1 0.0243(7) 0.0283(7) 0.0290(7) -0.0034(6) -0.0013(5) 0.0012(5) O2 0.0553(11) 0.0467(10) 0.0341(8) -0.0133(8) -0.0101(8) -0.0084(9) N 0.0358(9) 0.0255(8) 0.0263(8) -0.0061(7) 0.0067(7) -0.0020(7) C13 0.0324(10) 0.0279(10) 0.0292(10) -0.0029(8) -0.0077(8) -0.0006(8) C7 0.0322(10) 0.0286(10) 0.0257(9) -0.0056(8) -0.0013(8) -0.0009(8) C1 0.0438(13) 0.0306(11) 0.0313(11) 0.0071(8) 0.0106(9) 0.0135(9) C15 0.0549(15) 0.0293(11) 0.0368(12) 0.0030(9) -0.0079(11) -0.0002(11) C18 0.0549(15) 0.0293(11) 0.0367(12) -0.0116(9) 0.0169(11) -0.0046(10) C14 0.0358(12) 0.0511(15) 0.0539(16) -0.0098(12) -0.0156(11) 0.0068(11) C21 0.0315(13) 0.077(2) 0.0583(17) -0.0043(15) -0.0175(12) 0.0063(13) C8 0.0385(12) 0.0348(12) 0.0456(13) -0.0086(10) 0.0056(10) -0.0080(10) C19 0.0698(18) 0.0291(12) 0.0660(18) -0.0077(12) 0.0224(16) 0.0005(13) C20 0.0683(19) 0.0545(17) 0.0433(15) -0.0086(13) 0.0290(13) -0.0101(14) C12 0.0368(12) 0.0334(11) 0.0433(13) -0.0099(10) 0.0057(10) 0.0016(9) C16 0.0379(10) 0.0263(9) 0.0239(9) -0.0029(7) -0.0022(8) -0.0073(8) C23 0.0375(15) 0.094(3) 0.078(2) -0.004(2) 0.0062(15) 0.0232(16) C17 0.0681(19) 0.0462(15) 0.0390(14) -0.0203(12) 0.0061(12) -0.0093(13) C5 0.132(4) 0.108(3) 0.0358(16) 0.0274(19) 0.020(2) 0.083(3) C22 0.0273(16) 0.248(7) 0.145(4) -0.109(5) -0.027(2) 0.042(3) C11 0.0556(16) 0.0362(13) 0.0496(15) -0.0161(11) 0.0067(12) 0.0071(11) C2 0.0550(16) 0.0311(12) 0.0683(18) 0.0119(12) 0.0272(14) 0.0039(11) C4 0.143(4) 0.081(3) 0.082(3) 0.059(2) 0.074(3) 0.073(3) C10 0.0703(19) 0.0295(12) 0.0576(16) -0.0174(11) -0.0021(15) -0.0048(12) C6 0.075(2) 0.0638(19) 0.0324(13) 0.0075(12) -0.0021(14) 0.0294(16) C9 0.0591(17) 0.0374(13) 0.0647(18) -0.0114(13) 0.0054(14) -0.0162(13) C3 0.095(3) 0.0467(18) 0.114(3) 0.041(2) 0.069(3) 0.0260(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C21 2.102(3) . ? Pd N 2.1125(18) . ? Pd C22 2.144(4) . ? Pd P1 2.2444(7) . ? Pd C23 2.268(3) . ? P1 O1 1.6164(15) . ? P1 C7 1.806(2) . ? P1 C1 1.807(2) . ? P2 F2 1.5761(18) . ? P2 F5 1.580(2) . ? P2 F4 1.5806(18) . ? P2 F3 1.5837(17) . ? P2 F1 1.5838(18) . ? P2 F6 1.591(2) . ? O1 C13 1.451(2) . ? O2 C16 1.341(3) . ? O2 C17 1.461(3) . ? N C16 1.275(3) . ? N C18 1.504(3) . ? C13 C16 1.516(3) . ? C13 C14 1.519(3) . ? C13 C15 1.524(3) . ? C7 C8 1.380(3) . ? C7 C12 1.402(3) . ? C1 C2 1.380(4) . ? C1 C6 1.401(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C18 C19 1.516(4) . ? C18 C17 1.521(4) . ? C18 C20 1.523(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 C22 1.330(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C8 C9 1.397(3) . ? C8 H8 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C12 C11 1.381(3) . ? C12 H12 0.9300 . ? C23 C22 1.245(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C5 C4 1.335(7) . ? C5 C6 1.395(5) . ? C5 H5 0.9300 . ? C22 H22 0.9300 . ? C11 C10 1.392(4) . ? C11 H11 0.9300 . ? C2 C3 1.399(4) . ? C2 H2 0.9300 . ? C4 C3 1.371(7) . ? C4 H4 0.9300 . ? C10 C9 1.371(4) . ? C10 H10 0.9300 . ? C6 H6 0.9300 . ? C9 H9 0.9300 . ? C3 H3 0.9300 . ? 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 C21 Pd N 173.42(10) . . ? C21 Pd C22 36.50(15) . . ? N Pd C22 137.16(14) . . ? C21 Pd P1 95.17(9) . . ? N Pd P1 91.41(5) . . ? C22 Pd P1 130.08(14) . . ? C21 Pd C23 66.93(13) . . ? N Pd C23 106.49(11) . . ? C22 Pd C23 32.62(17) . . ? P1 Pd C23 162.10(10) . . ? O1 P1 C7 104.78(9) . . ? O1 P1 C1 98.65(10) . . ? C7 P1 C1 103.86(11) . . ? O1 P1 Pd 111.46(6) . . ? C7 P1 Pd 119.69(8) . . ? C1 P1 Pd 115.85(7) . . ? F2 P2 F5 90.35(13) . . ? F2 P2 F4 179.63(15) . . ? F5 P2 F4 90.01(13) . . ? F2 P2 F3 90.00(11) . . ? F5 P2 F3 89.98(12) . . ? F4 P2 F3 90.02(11) . . ? F2 P2 F1 90.87(11) . . ? F5 P2 F1 89.39(13) . . ? F4 P2 F1 89.12(11) . . ? F3 P2 F1 178.93(12) . . ? F2 P2 F6 90.46(14) . . ? F5 P2 F6 178.53(14) . . ? F4 P2 F6 89.18(13) . . ? F3 P2 F6 88.80(12) . . ? F1 P2 F6 91.82(13) . . ? C13 O1 P1 123.29(13) . . ? C16 O2 C17 105.1(2) . . ? C16 N C18 107.86(18) . . ? C16 N Pd 126.39(14) . . ? C18 N Pd 125.42(15) . . ? O1 C13 C16 109.00(17) . . ? O1 C13 C14 103.48(18) . . ? C16 C13 C14 111.42(18) . . ? O1 C13 C15 112.06(17) . . ? C16 C13 C15 109.15(19) . . ? C14 C13 C15 111.6(2) . . ? C8 C7 C12 119.8(2) . . ? C8 C7 P1 121.09(17) . . ? C12 C7 P1 119.04(17) . . ? C2 C1 C6 120.3(3) . . ? C2 C1 P1 121.0(2) . . ? C6 C1 P1 118.7(2) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N C18 C19 111.1(2) . . ? N C18 C17 101.15(19) . . ? C19 C18 C17 111.9(2) . . ? N C18 C20 108.04(19) . . ? C19 C18 C20 112.0(2) . . ? C17 C18 C20 112.1(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 C21 Pd 73.4(2) . . ? C22 C21 H21A 116.2 . . ? Pd C21 H21A 116.2 . . ? C22 C21 H21B 116.2 . . ? Pd C21 H21B 116.2 . . ? H21A C21 H21B 113.2 . . ? C7 C8 C9 119.5(2) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C11 C12 C7 120.2(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? N C16 O2 117.4(2) . . ? N C16 C13 129.01(19) . . ? O2 C16 C13 113.5(2) . . ? C22 C23 Pd 68.2(2) . . ? C22 C23 H23A 116.9 . . ? Pd C23 H23A 116.9 . . ? C22 C23 H23B 116.9 . . ? Pd C23 H23B 116.9 . . ? H23A C23 H23B 113.9 . . ? O2 C17 C18 105.08(19) . . ? O2 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O2 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C23 C22 C21 139.2(6) . . ? C23 C22 Pd 79.2(3) . . ? C21 C22 Pd 70.05(19) . . ? C23 C22 H22 110.4 . . ? C21 C22 H22 110.4 . . ? Pd C22 H22 139.3 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C1 C2 C3 118.7(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C5 C6 C1 117.9(4) . . ? C5 C6 H6 121.0 . . ? C1 C6 H6 121.0 . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? 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 C21 Pd P1 O1 -176.87(11) . . . . ? N Pd P1 O1 2.97(8) . . . . ? C22 Pd P1 O1 171.3(3) . . . . ? C23 Pd P1 O1 -176.2(3) . . . . ? C21 Pd P1 C7 -54.22(13) . . . . ? N Pd P1 C7 125.62(10) . . . . ? C22 Pd P1 C7 -66.1(3) . . . . ? C23 Pd P1 C7 -53.5(4) . . . . ? C21 Pd P1 C1 71.42(14) . . . . ? N Pd P1 C1 -108.74(11) . . . . ? C22 Pd P1 C1 59.6(3) . . . . ? C23 Pd P1 C1 72.1(4) . . . . ? C7 P1 O1 C13 -91.02(16) . . . . ? C1 P1 O1 C13 162.07(15) . . . . ? Pd P1 O1 C13 39.82(16) . . . . ? C21 Pd N C16 156.8(9) . . . . ? C22 Pd N C16 171.4(4) . . . . ? P1 Pd N C16 -21.82(18) . . . . ? C23 Pd N C16 157.9(2) . . . . ? C21 Pd N C18 -15.7(10) . . . . ? C22 Pd N C18 -1.2(4) . . . . ? P1 Pd N C18 165.66(16) . . . . ? C23 Pd N C18 -14.6(2) . . . . ? P1 O1 C13 C16 -66.6(2) . . . . ? P1 O1 C13 C14 174.78(14) . . . . ? P1 O1 C13 C15 54.4(2) . . . . ? O1 P1 C7 C8 120.8(2) . . . . ? C1 P1 C7 C8 -136.2(2) . . . . ? Pd P1 C7 C8 -5.1(2) . . . . ? O1 P1 C7 C12 -56.9(2) . . . . ? C1 P1 C7 C12 46.2(2) . . . . ? Pd P1 C7 C12 177.28(16) . . . . ? O1 P1 C1 C2 -21.0(2) . . . . ? C7 P1 C1 C2 -128.66(19) . . . . ? Pd P1 C1 C2 97.99(19) . . . . ? O1 P1 C1 C6 159.80(19) . . . . ? C7 P1 C1 C6 52.2(2) . . . . ? Pd P1 C1 C6 -81.2(2) . . . . ? C16 N C18 C19 131.5(2) . . . . ? Pd N C18 C19 -54.8(3) . . . . ? C16 N C18 C17 12.6(2) . . . . ? Pd N C18 C17 -173.72(16) . . . . ? C16 N C18 C20 -105.2(2) . . . . ? Pd N C18 C20 68.4(3) . . . . ? N Pd C21 C22 16.7(11) . . . . ? P1 Pd C21 C22 -164.7(4) . . . . ? C23 Pd C21 C22 15.5(4) . . . . ? C12 C7 C8 C9 0.0(4) . . . . ? P1 C7 C8 C9 -177.6(2) . . . . ? C8 C7 C12 C11 -0.1(4) . . . . ? P1 C7 C12 C11 177.6(2) . . . . ? C18 N C16 O2 -2.4(3) . . . . ? Pd N C16 O2 -175.98(14) . . . . ? C18 N C16 C13 174.5(2) . . . . ? Pd N C16 C13 0.9(3) . . . . ? C17 O2 C16 N -9.6(3) . . . . ? C17 O2 C16 C13 173.03(19) . . . . ? O1 C13 C16 N 44.5(3) . . . . ? C14 C13 C16 N 158.1(2) . . . . ? C15 C13 C16 N -78.2(3) . . . . ? O1 C13 C16 O2 -138.54(18) . . . . ? C14 C13 C16 O2 -25.0(3) . . . . ? C15 C13 C16 O2 98.8(2) . . . . ? C21 Pd C23 C22 -17.2(4) . . . . ? N Pd C23 C22 162.9(4) . . . . ? P1 Pd C23 C22 -18.0(6) . . . . ? C16 O2 C17 C18 16.9(3) . . . . ? N C18 C17 O2 -17.5(2) . . . . ? C19 C18 C17 O2 -135.9(2) . . . . ? C20 C18 C17 O2 97.4(2) . . . . ? Pd C23 C22 C21 41.2(6) . . . . ? Pd C21 C22 C23 -43.5(7) . . . . ? C21 Pd C22 C23 152.8(7) . . . . ? N Pd C22 C23 -24.5(6) . . . . ? P1 Pd C22 C23 172.9(2) . . . . ? N Pd C22 C21 -177.23(19) . . . . ? P1 Pd C22 C21 20.1(5) . . . . ? C23 Pd C22 C21 -152.8(7) . . . . ? C7 C12 C11 C10 0.9(4) . . . . ? C6 C1 C2 C3 -2.2(4) . . . . ? P1 C1 C2 C3 178.6(2) . . . . ? C6 C5 C4 C3 -2.1(6) . . . . ? C12 C11 C10 C9 -1.7(5) . . . . ? C4 C5 C6 C1 0.9(5) . . . . ? C2 C1 C6 C5 1.4(4) . . . . ? P1 C1 C6 C5 -179.5(2) . . . . ? C11 C10 C9 C8 1.7(5) . . . . ? C7 C8 C9 C10 -0.8(5) . . . . ? C5 C4 C3 C2 1.2(5) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 33.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.095 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.099 data_cristal_3 _database_code_CSD 193038 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Cl N2 O5 P Pd' _chemical_formula_sum 'C26 H38 Cl N2 O5 P Pd' _chemical_formula_weight 631.40 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.643(2) _cell_length_b 10.970(2) _cell_length_c 18.216(3) _cell_angle_alpha 90.0000(10) _cell_angle_beta 97.017(5) _cell_angle_gamma 90.0000(10) _cell_volume 2904.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26867 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 40.250 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.823 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_reflns_av_R_equivalents 0.042 _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 18224 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 40.26 _reflns_number_total 18223 _reflns_number_gt 13376 _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^)+(0.0684P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18223 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.190165(7) 0.238360(10) 0.740948(6) 0.01871(3) Uani 1 1 d . . . P P 0.24335(3) 0.16650(4) 0.64107(2) 0.01846(7) Uani 1 1 d . . . Cl Cl 0.13446(4) 0.28727(5) 0.85428(2) 0.03302(9) Uani 1 1 d . . . N1 N 0.10983(9) 0.37482(12) 0.66963(7) 0.0222(2) Uani 1 1 d . . . N2 N 0.57830(12) 0.09040(17) 0.64591(15) 0.0509(6) Uani 1 1 d . . . O1 O 0.34957(7) 0.13018(11) 0.65670(6) 0.0227(2) Uani 1 1 d . . . O2 O 0.49776(13) 0.26028(14) 0.61785(15) 0.0562(6) Uani 1 1 d . . . O4 O 0.08579(9) 0.50580(12) 0.57422(7) 0.0307(3) Uani 1 1 d . . . O3 O 0.23381(9) 0.26216(10) 0.57359(7) 0.0239(2) Uani 1 1 d . . . O5 O 0.26744(10) 0.02545(12) 0.81518(8) 0.0325(3) Uani 1 1 d . . . C10 C 0.13879(11) 0.42199(14) 0.61250(9) 0.0228(3) Uani 1 1 d . . . C1 C 0.18270(10) 0.03795(14) 0.59626(8) 0.0213(2) Uani 1 1 d . . . C15 C 0.41132(10) 0.07249(15) 0.60838(10) 0.0252(3) Uani 1 1 d . . . C7 C 0.23018(11) 0.39356(14) 0.58370(9) 0.0234(3) Uani 1 1 d . . . C12 C 0.02048(11) 0.43600(15) 0.67924(9) 0.0234(3) Uani 1 1 d . . . C23 C 0.27851(11) 0.13126(15) 0.80177(9) 0.0243(3) Uani 1 1 d . . . C18 C 0.50202(11) 0.13783(15) 0.62825(10) 0.0251(3) Uani 1 1 d . . . C11 C -0.00169(13) 0.50236(19) 0.60509(10) 0.0328(4) Uani 1 1 d . . . H11A H -0.0478 0.4583 0.5727 0.039 Uiso 1 1 calc . . . H11B H -0.0241 0.5841 0.6125 0.039 Uiso 1 1 calc . . . C14 C 0.03599(14) 0.52623(17) 0.74309(11) 0.0324(4) Uani 1 1 d . . . H14A H 0.0820 0.5844 0.7333 0.049 Uiso 1 1 calc . . . H14B H 0.0563 0.4832 0.7880 0.049 Uiso 1 1 calc . . . H14C H -0.0205 0.5680 0.7481 0.049 Uiso 1 1 calc . . . C2 C 0.14453(12) 0.03851(17) 0.52248(9) 0.0278(3) Uani 1 1 d . . . H2 H 0.1486 0.1078 0.4937 0.033 Uiso 1 1 calc . . . C9 C 0.31034(13) 0.44016(17) 0.63766(11) 0.0319(3) Uani 1 1 d . . . H9A H 0.3065 0.4063 0.6858 0.048 Uiso 1 1 calc . . . H9B H 0.3076 0.5275 0.6403 0.048 Uiso 1 1 calc . . . H9C H 0.3673 0.4160 0.6209 0.048 Uiso 1 1 calc . . . C24 C 0.36409(14) 0.2031(2) 0.83404(12) 0.0357(4) Uani 1 1 d . . . H24A H 0.3804 0.2595 0.7968 0.043 Uiso 1 1 calc . . . H24B H 0.3487 0.2509 0.8756 0.043 Uiso 1 1 calc . . . C4 C 0.09255(16) -0.1676(2) 0.53450(13) 0.0411(5) Uani 1 1 d . . . H4 H 0.0632 -0.2367 0.5135 0.049 Uiso 1 1 calc . . . C6 C 0.17361(14) -0.06565(17) 0.63947(10) 0.0324(4) Uani 1 1 d . . . H6 H 0.1978 -0.0660 0.6891 0.039 Uiso 1 1 calc . . . C17 C 0.42015(14) -0.06099(18) 0.62904(15) 0.0405(5) Uani 1 1 d . . . H17A H 0.3618 -0.1006 0.6168 0.061 Uiso 1 1 calc . . . H17B H 0.4391 -0.0684 0.6812 0.061 Uiso 1 1 calc . . . H17C H 0.4651 -0.0987 0.6022 0.061 Uiso 1 1 calc . . . C25 C 0.44606(14) 0.1262(2) 0.85936(12) 0.0385(4) Uani 1 1 d . . . H25 H 0.4695 0.0777 0.8241 0.046 Uiso 1 1 calc . . . C19 C 0.64787(13) 0.1903(2) 0.65140(13) 0.0367(4) Uani 1 1 d . . . C21 C 0.7030(3) 0.1926(5) 0.7285(2) 0.0911(14) Uani 1 1 d . . . H21A H 0.6618 0.2037 0.7651 0.137 Uiso 1 1 calc . . . H21B H 0.7464 0.2586 0.7314 0.137 Uiso 1 1 calc . . . H21C H 0.7354 0.1169 0.7373 0.137 Uiso 1 1 calc . . . C3 C 0.10012(14) -0.0652(2) 0.49198(11) 0.0365(4) Uani 1 1 d . . . H3 H 0.0754 -0.0653 0.4425 0.044 Uiso 1 1 calc . . . C13 C -0.05210(13) 0.34197(19) 0.69194(12) 0.0347(4) Uani 1 1 d . . . H13A H -0.0355 0.3028 0.7388 0.052 Uiso 1 1 calc . . . H13B H -0.0561 0.2821 0.6532 0.052 Uiso 1 1 calc . . . H13C H -0.1106 0.3815 0.6918 0.052 Uiso 1 1 calc . . . C8 C 0.23448(14) 0.44485(18) 0.50668(11) 0.0329(4) Uani 1 1 d . . . H8A H 0.2927 0.4245 0.4906 0.049 Uiso 1 1 calc . . . H8B H 0.2278 0.5319 0.5078 0.049 Uiso 1 1 calc . . . H8C H 0.1857 0.4105 0.4730 0.049 Uiso 1 1 calc . . . C20 C 0.7076(3) 0.1765(5) 0.5920(3) 0.120(2) Uani 1 1 d . . . H20A H 0.7433 0.1033 0.6000 0.180 Uiso 1 1 calc . . . H20B H 0.7481 0.2454 0.5924 0.180 Uiso 1 1 calc . . . H20C H 0.6701 0.1720 0.5450 0.180 Uiso 1 1 calc . . . C26 C 0.48749(16) 0.1215(2) 0.92696(14) 0.0454(5) Uani 1 1 d . . . H26A H 0.4662 0.1685 0.9638 0.054 Uiso 1 1 calc . . . H26B H 0.5383 0.0710 0.9383 0.054 Uiso 1 1 calc . . . C16 C 0.38031(12) 0.0916(2) 0.52629(11) 0.0369(4) Uani 1 1 d . . . H16A H 0.3225 0.0512 0.5129 0.055 Uiso 1 1 calc . . . H16B H 0.4255 0.0583 0.4979 0.055 Uiso 1 1 calc . . . H16C H 0.3733 0.1772 0.5163 0.055 Uiso 1 1 calc . . . C22 C 0.58966(17) 0.3039(3) 0.64176(19) 0.0573(7) Uani 1 1 d . . . H22A H 0.5916 0.3481 0.6881 0.069 Uiso 1 1 calc . . . H22B H 0.6108 0.3572 0.6048 0.069 Uiso 1 1 calc . . . C5 C 0.12845(18) -0.1681(2) 0.60831(13) 0.0426(5) Uani 1 1 d . . . H5 H 0.1224 -0.2370 0.6371 0.051 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 Pd 0.01875(5) 0.02123(5) 0.01666(5) 0.00064(3) 0.00418(3) 0.00245(3) P 0.01707(14) 0.02026(15) 0.01881(15) -0.00016(12) 0.00526(11) 0.00077(11) Cl 0.0419(2) 0.0384(2) 0.02032(16) -0.00004(15) 0.01016(15) 0.00983(18) N1 0.0220(5) 0.0233(5) 0.0217(5) 0.0013(4) 0.0049(4) 0.0048(4) N2 0.0195(7) 0.0319(8) 0.0994(18) -0.0021(10) 0.0000(9) -0.0003(6) O1 0.0168(4) 0.0276(5) 0.0246(5) -0.0034(4) 0.0062(4) 0.0014(4) O2 0.0298(8) 0.0320(8) 0.1039(19) 0.0086(8) -0.0037(10) -0.0055(6) O4 0.0330(6) 0.0311(6) 0.0289(6) 0.0096(5) 0.0073(5) 0.0112(5) O3 0.0301(6) 0.0229(5) 0.0200(5) 0.0021(4) 0.0083(4) 0.0027(4) O5 0.0339(7) 0.0271(6) 0.0351(7) 0.0053(5) -0.0011(5) 0.0006(5) C10 0.0248(6) 0.0216(6) 0.0223(6) 0.0021(5) 0.0045(5) 0.0043(5) C1 0.0187(6) 0.0237(6) 0.0224(6) -0.0006(5) 0.0056(5) -0.0014(5) C15 0.0176(6) 0.0262(7) 0.0333(8) -0.0048(6) 0.0095(5) -0.0010(5) C7 0.0261(7) 0.0218(6) 0.0236(6) 0.0020(5) 0.0083(5) 0.0012(5) C12 0.0213(6) 0.0237(6) 0.0256(7) 0.0002(5) 0.0040(5) 0.0057(5) C23 0.0245(7) 0.0267(7) 0.0213(6) 0.0016(5) 0.0017(5) 0.0029(5) C18 0.0188(6) 0.0260(7) 0.0313(7) -0.0009(6) 0.0068(5) -0.0002(5) C11 0.0289(8) 0.0401(9) 0.0295(8) 0.0050(7) 0.0043(6) 0.0139(7) C14 0.0372(9) 0.0288(8) 0.0311(8) -0.0060(6) 0.0037(7) 0.0076(7) C2 0.0241(7) 0.0345(8) 0.0247(7) -0.0001(6) 0.0019(5) -0.0026(6) C9 0.0302(8) 0.0303(8) 0.0355(9) -0.0021(7) 0.0058(7) -0.0049(6) C24 0.0319(9) 0.0345(9) 0.0371(9) 0.0013(8) -0.0100(7) -0.0006(7) C4 0.0397(10) 0.0397(11) 0.0443(11) -0.0134(9) 0.0069(8) -0.0164(8) C6 0.0411(10) 0.0293(8) 0.0272(8) 0.0001(6) 0.0051(7) -0.0104(7) C17 0.0300(9) 0.0265(8) 0.0685(15) -0.0047(9) 0.0203(9) -0.0008(7) C25 0.0279(8) 0.0440(11) 0.0422(11) -0.0049(9) -0.0010(7) 0.0017(7) C19 0.0209(7) 0.0364(10) 0.0523(12) -0.0025(8) 0.0024(7) -0.0059(7) C21 0.068(2) 0.105(3) 0.090(3) 0.038(2) -0.0332(19) -0.032(2) C3 0.0309(9) 0.0475(11) 0.0303(8) -0.0095(8) 0.0007(7) -0.0087(8) C13 0.0241(7) 0.0349(9) 0.0467(11) 0.0001(8) 0.0103(7) -0.0001(6) C8 0.0379(9) 0.0326(9) 0.0305(8) 0.0102(7) 0.0139(7) 0.0038(7) C20 0.069(2) 0.161(5) 0.142(4) -0.098(4) 0.066(3) -0.068(3) C26 0.0340(10) 0.0513(13) 0.0479(12) -0.0038(10) -0.0063(9) 0.0122(9) C16 0.0216(7) 0.0598(13) 0.0310(8) -0.0127(8) 0.0107(6) -0.0026(8) C22 0.0343(11) 0.0450(13) 0.090(2) -0.0014(14) -0.0015(12) -0.0136(10) C5 0.0547(13) 0.0330(10) 0.0410(11) 0.0000(8) 0.0098(9) -0.0187(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C23 1.9827(16) . ? Pd P 2.2100(5) . ? Pd N1 2.2224(13) . ? Pd Cl 2.3721(5) . ? P O1 1.5972(12) . ? P O3 1.6094(12) . ? P C1 1.8074(16) . ? N1 C10 1.280(2) . ? N1 C12 1.4997(19) . ? N2 C18 1.239(2) . ? N2 C19 1.491(3) . ? O1 C15 1.4789(19) . ? O2 C18 1.357(2) . ? O2 C22 1.444(3) . ? O4 C10 1.3422(19) . ? O4 C11 1.461(2) . ? O3 C7 1.4550(19) . ? O5 C23 1.201(2) . ? C10 C7 1.528(2) . ? C1 C2 1.391(2) . ? C1 C6 1.398(2) . ? C15 C17 1.514(3) . ? C15 C18 1.514(2) . ? C15 C16 1.523(3) . ? C7 C8 1.520(2) . ? C7 C9 1.524(3) . ? C12 C13 1.519(3) . ? C12 C14 1.523(2) . ? C12 C11 1.534(2) . ? C23 C24 1.535(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C2 C3 1.392(3) . ? C2 H2 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C24 C25 1.493(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C4 C3 1.377(3) . ? C4 C5 1.383(3) . ? C4 H4 0.9300 . ? C6 C5 1.389(3) . ? C6 H6 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C25 C26 1.306(3) . ? C25 H25 0.9300 . ? C19 C20 1.480(4) . ? C19 C22 1.508(4) . ? C19 C21 1.532(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C3 H3 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C26 H26A 0.9300 . ? C26 H26B 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C5 H5 0.9300 . ? 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 C23 Pd P 88.69(5) . . ? C23 Pd N1 171.27(6) . . ? P Pd N1 88.49(4) . . ? C23 Pd Cl 85.29(5) . . ? P Pd Cl 172.048(17) . . ? N1 Pd Cl 98.20(4) . . ? O1 P O3 106.89(7) . . ? O1 P C1 107.46(7) . . ? O3 P C1 99.89(7) . . ? O1 P Pd 112.07(5) . . ? O3 P Pd 112.94(5) . . ? C1 P Pd 116.55(5) . . ? C10 N1 C12 107.11(13) . . ? C10 N1 Pd 122.91(11) . . ? C12 N1 Pd 129.81(10) . . ? C18 N2 C19 107.20(18) . . ? C15 O1 P 130.81(11) . . ? C18 O2 C22 105.11(18) . . ? C10 O4 C11 105.11(13) . . ? C7 O3 P 123.40(11) . . ? N1 C10 O4 118.13(14) . . ? N1 C10 C7 125.99(14) . . ? O4 C10 C7 115.87(13) . . ? C2 C1 C6 119.53(15) . . ? C2 C1 P 123.38(12) . . ? C6 C1 P 117.08(12) . . ? O1 C15 C17 107.81(14) . . ? O1 C15 C18 103.74(13) . . ? C17 C15 C18 110.67(15) . . ? O1 C15 C16 113.26(14) . . ? C17 C15 C16 112.52(17) . . ? C18 C15 C16 108.50(14) . . ? O3 C7 C8 104.10(13) . . ? O3 C7 C9 112.13(14) . . ? C8 C7 C9 110.84(15) . . ? O3 C7 C10 107.02(13) . . ? C8 C7 C10 112.22(14) . . ? C9 C7 C10 110.35(14) . . ? N1 C12 C13 110.51(13) . . ? N1 C12 C14 109.22(13) . . ? C13 C12 C14 111.52(15) . . ? N1 C12 C11 101.74(12) . . ? C13 C12 C11 112.32(15) . . ? C14 C12 C11 111.09(15) . . ? O5 C23 C24 122.84(16) . . ? O5 C23 Pd 126.24(13) . . ? C24 C23 Pd 110.86(12) . . ? N2 C18 O2 118.48(17) . . ? N2 C18 C15 126.89(17) . . ? O2 C18 C15 114.28(15) . . ? O4 C11 C12 104.48(13) . . ? O4 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? O4 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 C2 C3 119.67(17) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C25 C24 C23 114.57(18) . . ? C25 C24 H24A 108.6 . . ? C23 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C3 C4 C5 120.21(18) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C5 C6 C1 120.05(18) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C25 C24 125.2(2) . . ? C26 C25 H25 117.4 . . ? C24 C25 H25 117.4 . . ? C20 C19 N2 109.6(2) . . ? C20 C19 C22 112.0(3) . . ? N2 C19 C22 103.17(16) . . ? C20 C19 C21 112.3(3) . . ? N2 C19 C21 110.6(2) . . ? C22 C19 C21 108.7(3) . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C3 C2 120.54(18) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 . . ? C25 C26 H26A 120.0 . . ? C25 C26 H26B 120.0 . . ? H26A C26 H26B 120.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C22 C19 104.70(19) . . ? O2 C22 H22A 110.8 . . ? C19 C22 H22A 110.8 . . ? O2 C22 H22B 110.8 . . ? C19 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C4 C5 C6 119.97(19) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 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 C23 Pd P O1 -31.08(7) . . . . ? N1 Pd P O1 140.66(6) . . . . ? Cl Pd P O1 -71.90(13) . . . . ? C23 Pd P O3 -151.88(8) . . . . ? N1 Pd P O3 19.86(7) . . . . ? Cl Pd P O3 167.30(12) . . . . ? C23 Pd P C1 93.29(8) . . . . ? N1 Pd P C1 -94.97(7) . . . . ? Cl Pd P C1 52.47(14) . . . . ? C23 Pd N1 C10 37.2(4) . . . . ? P Pd N1 C10 -33.99(13) . . . . ? Cl Pd N1 C10 150.32(13) . . . . ? C23 Pd N1 C12 -137.6(4) . . . . ? P Pd N1 C12 151.19(13) . . . . ? Cl Pd N1 C12 -24.50(14) . . . . ? O3 P O1 C15 -59.91(15) . . . . ? C1 P O1 C15 46.57(15) . . . . ? Pd P O1 C15 175.85(12) . . . . ? O1 P O3 C7 -98.24(13) . . . . ? C1 P O3 C7 149.98(13) . . . . ? Pd P O3 C7 25.47(14) . . . . ? C12 N1 C10 O4 -2.6(2) . . . . ? Pd N1 C10 O4 -178.44(11) . . . . ? C12 N1 C10 C7 176.24(15) . . . . ? Pd N1 C10 C7 0.4(2) . . . . ? C11 O4 C10 N1 -9.6(2) . . . . ? C11 O4 C10 C7 171.42(15) . . . . ? O1 P C1 C2 -110.27(14) . . . . ? O3 P C1 C2 1.08(15) . . . . ? Pd P C1 C2 123.05(13) . . . . ? O1 P C1 C6 70.61(15) . . . . ? O3 P C1 C6 -178.05(14) . . . . ? Pd P C1 C6 -56.08(15) . . . . ? P O1 C15 C17 -100.99(18) . . . . ? P O1 C15 C18 141.61(13) . . . . ? P O1 C15 C16 24.2(2) . . . . ? P O3 C7 C8 172.49(12) . . . . ? P O3 C7 C9 52.62(18) . . . . ? P O3 C7 C10 -68.52(17) . . . . ? N1 C10 C7 O3 54.5(2) . . . . ? O4 C10 C7 O3 -126.59(15) . . . . ? N1 C10 C7 C8 168.14(17) . . . . ? O4 C10 C7 C8 -13.0(2) . . . . ? N1 C10 C7 C9 -67.7(2) . . . . ? O4 C10 C7 C9 111.15(17) . . . . ? C10 N1 C12 C13 132.32(16) . . . . ? Pd N1 C12 C13 -52.23(19) . . . . ? C10 N1 C12 C14 -104.63(16) . . . . ? Pd N1 C12 C14 70.82(18) . . . . ? C10 N1 C12 C11 12.86(18) . . . . ? Pd N1 C12 C11 -171.69(12) . . . . ? P Pd C23 O5 -83.31(16) . . . . ? N1 Pd C23 O5 -154.5(3) . . . . ? Cl Pd C23 O5 91.48(16) . . . . ? P Pd C23 C24 99.43(13) . . . . ? N1 Pd C23 C24 28.3(4) . . . . ? Cl Pd C23 C24 -85.77(13) . . . . ? C19 N2 C18 O2 0.5(3) . . . . ? C19 N2 C18 C15 173.28(18) . . . . ? C22 O2 C18 N2 -7.8(3) . . . . ? C22 O2 C18 C15 178.5(2) . . . . ? O1 C15 C18 N2 128.2(2) . . . . ? C17 C15 C18 N2 12.8(3) . . . . ? C16 C15 C18 N2 -111.1(2) . . . . ? O1 C15 C18 O2 -58.8(2) . . . . ? C17 C15 C18 O2 -174.1(2) . . . . ? C16 C15 C18 O2 61.9(2) . . . . ? C10 O4 C11 C12 16.86(19) . . . . ? N1 C12 C11 O4 -17.78(18) . . . . ? C13 C12 C11 O4 -135.96(15) . . . . ? C14 C12 C11 O4 98.35(17) . . . . ? C6 C1 C2 C3 -1.9(3) . . . . ? P C1 C2 C3 179.00(14) . . . . ? O5 C23 C24 C25 21.5(3) . . . . ? Pd C23 C24 C25 -161.15(15) . . . . ? C2 C1 C6 C5 1.4(3) . . . . ? P C1 C6 C5 -179.44(18) . . . . ? C23 C24 C25 C26 -119.4(3) . . . . ? C18 N2 C19 C20 -112.8(3) . . . . ? C18 N2 C19 C22 6.7(3) . . . . ? C18 N2 C19 C21 122.8(3) . . . . ? C5 C4 C3 C2 0.5(3) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C18 O2 C22 C19 11.1(3) . . . . ? C20 C19 C22 O2 107.0(3) . . . . ? N2 C19 C22 O2 -10.8(3) . . . . ? C21 C19 C22 O2 -128.3(3) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C1 C6 C5 C4 0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 40.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.490 _refine_diff_density_min -2.911 _refine_diff_density_rms 0.178