Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Mandal, Swadhin K.' ; Department of Inorganic and Physical Chemistry Indian Institute of Science Bangalore-560012 India ; 'Gowda, G. A. Nagana' ; Sophisticated Instruments Facility Indian Institute of Science Bangalore-560012 India ; 'Krishnamurthy, Setharampattu S.' ; Department of Inorganic and Physical Chemistry Indian Institute of Science Bangalore-560012 India ; 'Nethaji, Munirathinam' ; Department of Inorganic and Physical Chemistry Indian Institute of science Bangalore-560012 India ; _publ_contact_author_name 'Prof Setharampattu S. Krishnamurthy' _publ_contact_author_address ; Inorganic and Physical Chemistry Indian Institute of Science Bangalore 560012 INDIA ; _publ_contact_author_email 'SSKRISH@IPC.IISC.ERNET.IN' _publ_requested_journal ; Journal of Chemical Society, Dalton Transaction ; _publ_section_title ; Palladium(II) Allyl Complexes of Chiral Diphosphazane Ligands Ambident of the Type Ph2P(E)N(R)PPh(N2C3HMe2-3,5) [E == Lone Pair or S; R == CHMe2- or (S)-*CHMePh]: Coordination Behaviour, X-ray Crystal Structure Analyses and Stereodynamic Studies in Solution ; data_complex_5a _database_code_CSD 190877 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta-3-allyl)[eta-2-{N,N-(diphenylphosphino) (phenyl, 3,5-dimethylpyrazolylphosphino) (S)-1-phenylethylamine}-kappa-P,N] palladium(II)hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point '135-138 șC dec.' _chemical_formula_moiety ; [Pd(eta-3-C3H5){eta-2-(SR)-Ph2PN((S)-*CHMePh)PPh(N2C3HMe2-3,5)}](PF6) ; _chemical_formula_sum 'C35.50 H39 F6 N3 O0.50 P3 Pd' _chemical_formula_weight 829.01 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2253(2) _cell_length_b 37.0328(9) _cell_length_c 10.9457(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.5650(10) _cell_angle_gamma 90.00 _cell_volume 3739.29(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15784 _cell_measurement_theta_min 1.10 _cell_measurement_theta_max 23.26 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.685 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\alpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD PLATFORM' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15784 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 10038 _reflns_number_gt 9503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SMART and SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-32 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0673P)^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 SHELXL _refine_ls_extinction_coef 0.0088(5) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 10038 _refine_ls_number_parameters 884 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.40534(5) 0.319677(12) 0.46438(3) 0.04744(14) Uani 1 1 d . . . Pd2 Pd 0.56252(5) 0.066539(11) 0.04375(3) 0.04723(14) Uani 1 1 d . . . P1 P -0.0424(3) 0.34802(6) -0.22488(19) 0.0758(6) Uani 1 1 d . . . P2 P 0.58445(15) 0.33340(4) 0.19688(13) 0.0418(3) Uani 1 1 d . . . P3 P 0.44092(14) 0.06252(4) 0.22523(12) 0.0379(3) Uani 1 1 d . . . P4 P 0.27955(14) 0.32658(3) 0.28373(12) 0.0363(3) Uani 1 1 d . . . P5 P 0.74328(16) 0.04887(4) 0.31243(13) 0.0434(3) Uani 1 1 d . . . P6 P 0.1146(3) 0.04091(6) -0.2833(2) 0.0739(6) Uani 1 1 d . . . F1 F -0.080(2) 0.3634(3) -0.1047(8) 0.308(9) Uani 1 1 d . . . F2 F -0.1420(12) 0.3740(3) -0.2931(8) 0.213(5) Uani 1 1 d . . . F3 F -0.1542(8) 0.3162(3) -0.2020(8) 0.176(3) Uani 1 1 d . . . F4 F 0.0697(7) 0.32256(19) -0.1567(5) 0.1221(18) Uani 1 1 d . . . F5 F -0.0099(10) 0.3287(2) -0.3479(5) 0.149(3) Uani 1 1 d . . . F6 F 0.0732(15) 0.3744(3) -0.2585(11) 0.258(7) Uani 1 1 d . . . F7 F 0.080(3) 0.0248(3) -0.4015(9) 0.360(12) Uani 1 1 d . . . F8 F 0.1867(19) 0.0085(3) -0.2411(12) 0.280(8) Uani 1 1 d . . . F9 F 0.1441(13) 0.0585(2) -0.1611(6) 0.191(4) Uani 1 1 d . . . F10 F 0.2338(11) 0.0623(3) -0.3432(8) 0.204(4) Uani 1 1 d . . . F11 F 0.0263(13) 0.0754(3) -0.3103(14) 0.251(6) Uani 1 1 d . . . F12 F -0.0228(12) 0.0228(3) -0.2384(16) 0.288(8) Uani 1 1 d . . . O1 O 1.045(2) 0.2053(3) -0.4043(11) 0.245(8) Uani 1 1 d . . . N1 N 0.6653(5) 0.01761(13) 0.0941(5) 0.0515(12) Uani 1 1 d . . . N2 N 0.7385(6) 0.01475(13) 0.2038(5) 0.0501(12) Uani 1 1 d . . . N3 N 0.5914(5) 0.36811(13) 0.3031(5) 0.0502(12) Uani 1 1 d . . . N4 N 0.5203(5) 0.36620(13) 0.4138(5) 0.0525(12) Uani 1 1 d . . . N5 N 0.5645(5) 0.05635(12) 0.3407(4) 0.0398(10) Uani 1 1 d . . . N6 N 0.4034(5) 0.32922(11) 0.1681(4) 0.0370(10) Uani 1 1 d . . . C1 C 0.3073(10) 0.2740(2) 0.5476(7) 0.081(2) Uani 1 1 d . . . H1A H 0.2026 0.2723 0.5408 0.097 Uiso 1 1 calc R . . H1B H 0.3562 0.2511 0.5371 0.097 Uiso 1 1 calc R . . C2 C 0.3614(10) 0.2965(3) 0.6384(7) 0.088(3) Uani 1 1 d . . . H2 H 0.2926 0.3088 0.6919 0.106 Uiso 1 1 calc R . . C3 C 0.5057(9) 0.3067(3) 0.6436(6) 0.092(3) Uani 1 1 d . . . H3A H 0.5771 0.2875 0.6450 0.111 Uiso 1 1 calc R . . H3B H 0.5299 0.3270 0.6963 0.111 Uiso 1 1 calc R . . C4 C 0.4624(13) 0.4054(3) 0.5854(11) 0.128(4) Uani 1 1 d . . . H4A H 0.4149 0.3837 0.6114 0.192 Uiso 1 1 calc R . . H4B H 0.3926 0.4246 0.5789 0.192 Uiso 1 1 calc R . . H4C H 0.5359 0.4119 0.6441 0.192 Uiso 1 1 calc R . . C5 C 0.5310(9) 0.3993(2) 0.4629(8) 0.078(2) Uani 1 1 d . . . C6 C 0.6083(9) 0.4216(2) 0.3878(10) 0.088(3) Uani 1 1 d . . . H6 H 0.6320 0.4455 0.4039 0.106 Uiso 1 1 calc R . . C7 C 0.6446(7) 0.40281(18) 0.2859(8) 0.067(2) Uani 1 1 d . . . C8 C 0.7276(10) 0.4129(2) 0.1742(9) 0.092(3) Uani 1 1 d . . . H8A H 0.7330 0.3925 0.1206 0.138 Uiso 1 1 calc R . . H8B H 0.8238 0.4203 0.1975 0.138 Uiso 1 1 calc R . . H8C H 0.6794 0.4324 0.1330 0.138 Uiso 1 1 calc R . . C9 C 0.6297(6) 0.29604(16) 0.3000(5) 0.0434(13) Uani 1 1 d . . . C10 C 0.5698(7) 0.26211(15) 0.2801(6) 0.0495(14) Uani 1 1 d . . . H10 H 0.4951 0.2591 0.2233 0.059 Uiso 1 1 calc R . . C11 C 0.6221(9) 0.23259(19) 0.3456(7) 0.072(2) Uani 1 1 d . . . H11 H 0.5794 0.2101 0.3345 0.086 Uiso 1 1 calc R . . C12 C 0.7362(8) 0.2363(2) 0.4267(7) 0.073(2) Uani 1 1 d . . . H12 H 0.7730 0.2162 0.4678 0.088 Uiso 1 1 calc R . . C13 C 0.7957(8) 0.2704(2) 0.4462(6) 0.069(2) Uani 1 1 d . . . H13 H 0.8711 0.2734 0.5023 0.083 Uiso 1 1 calc R . . C14 C 0.7422(6) 0.29959(17) 0.3819(5) 0.0506(14) Uani 1 1 d . . . H14 H 0.7835 0.3222 0.3943 0.061 Uiso 1 1 calc R . . C15 C 0.3613(6) 0.32571(16) 0.0327(4) 0.0463(13) Uani 1 1 d . . . H15 H 0.2552 0.3248 0.0278 0.056 Uiso 1 1 calc R . . C16 C 0.4109(8) 0.3592(2) -0.0410(6) 0.067(2) Uani 1 1 d . . . H16A H 0.3708 0.3806 -0.0054 0.101 Uiso 1 1 calc R . . H16B H 0.3778 0.3570 -0.1241 0.101 Uiso 1 1 calc R . . H16C H 0.5148 0.3606 -0.0391 0.101 Uiso 1 1 calc R . . C17 C 0.4183(6) 0.2902(2) -0.0171(5) 0.0486(16) Uani 1 1 d . . . C18 C 0.3338(10) 0.2601(2) -0.0103(7) 0.083(2) Uani 1 1 d . . . H18 H 0.2393 0.2621 0.0179 0.100 Uiso 1 1 calc R . . C19 C 0.3865(13) 0.2261(3) -0.0448(9) 0.105(3) Uani 1 1 d . . . H19 H 0.3277 0.2058 -0.0390 0.126 Uiso 1 1 calc R . . C20 C 0.5261(13) 0.2230(3) -0.0876(9) 0.096(3) Uani 1 1 d . . . H20 H 0.5623 0.2005 -0.1097 0.115 Uiso 1 1 calc R . . C21 C 0.6107(9) 0.2529(3) -0.0971(7) 0.083(3) Uani 1 1 d . . . H21 H 0.7037 0.2507 -0.1283 0.100 Uiso 1 1 calc R . . C22 C 0.5610(7) 0.28685(19) -0.0613(5) 0.0542(15) Uani 1 1 d . . . H22 H 0.6210 0.3070 -0.0664 0.065 Uiso 1 1 calc R . . C23 C 0.1368(6) 0.29669(14) 0.2294(5) 0.0406(12) Uani 1 1 d . . . C24 C 0.0282(6) 0.30929(15) 0.1516(5) 0.0438(13) Uani 1 1 d . . . H24 H 0.0239 0.3337 0.1320 0.053 Uiso 1 1 calc R . . C25 C -0.0738(6) 0.28578(18) 0.1029(5) 0.0498(14) Uani 1 1 d . . . H25 H -0.1456 0.2944 0.0504 0.060 Uiso 1 1 calc R . . C26 C -0.0693(7) 0.24978(16) 0.1319(6) 0.0527(15) Uani 1 1 d . . . H26 H -0.1369 0.2339 0.0983 0.063 Uiso 1 1 calc R . . C27 C 0.0352(8) 0.23740(17) 0.2105(7) 0.0625(17) Uani 1 1 d . . . H27 H 0.0362 0.2131 0.2322 0.075 Uiso 1 1 calc R . . C28 C 0.1392(7) 0.26020(15) 0.2581(6) 0.0513(15) Uani 1 1 d . . . H28 H 0.2111 0.2511 0.3097 0.062 Uiso 1 1 calc R . . C29 C 0.1852(6) 0.36895(15) 0.3009(5) 0.0423(13) Uani 1 1 d . . . C30 C 0.2092(9) 0.40036(19) 0.2333(8) 0.081(2) Uani 1 1 d . . . H30 H 0.2748 0.4002 0.1693 0.098 Uiso 1 1 calc R . . C31 C 0.1347(12) 0.4321(2) 0.2618(11) 0.109(4) Uani 1 1 d . . . H31 H 0.1508 0.4529 0.2165 0.131 Uiso 1 1 calc R . . C32 C 0.0392(9) 0.4328(2) 0.3549(8) 0.081(2) Uani 1 1 d . . . H32 H -0.0100 0.4540 0.3724 0.098 Uiso 1 1 calc R . . C33 C 0.0144(9) 0.4029(2) 0.4231(7) 0.074(2) Uani 1 1 d . . . H33 H -0.0502 0.4037 0.4878 0.088 Uiso 1 1 calc R . . C34 C 0.0867(7) 0.37088(18) 0.3951(6) 0.0582(16) Uani 1 1 d . . . H34 H 0.0681 0.3503 0.4410 0.070 Uiso 1 1 calc R . . C35 C 1.1357(16) 0.1661(4) -0.2515(13) 0.153(5) Uani 1 1 d . . . H35A H 1.1582 0.1518 -0.3219 0.229 Uiso 1 1 calc R . . H35B H 1.0728 0.1527 -0.1988 0.229 Uiso 1 1 calc R . . H35C H 1.2235 0.1720 -0.2082 0.229 Uiso 1 1 calc R . . C36 C 1.0604(12) 0.2007(3) -0.2919(12) 0.114(4) Uani 1 1 d . . . C37 C 1.0148(19) 0.2238(6) -0.2147(14) 0.199(8) Uani 1 1 d . . . H37A H 0.9696 0.2436 -0.2573 0.299 Uiso 1 1 calc R . . H37B H 1.0949 0.2327 -0.1668 0.299 Uiso 1 1 calc R . . H37C H 0.9455 0.2126 -0.1620 0.299 Uiso 1 1 calc R . . C38 C 0.4744(11) 0.1133(2) -0.0378(7) 0.083(2) Uani 1 1 d . . . H38A H 0.3703 0.1163 -0.0311 0.099 Uiso 1 1 calc R . . H38B H 0.5281 0.1355 -0.0254 0.099 Uiso 1 1 calc R . . C39 C 0.5217(13) 0.0910(3) -0.1319(8) 0.107(3) Uani 1 1 d . . . H39 H 0.4468 0.0798 -0.1835 0.128 Uiso 1 1 calc R . . C40 C 0.6537(11) 0.0769(3) -0.1368(6) 0.092(3) Uani 1 1 d . . . H40A H 0.7337 0.0938 -0.1401 0.111 Uiso 1 1 calc R . . H40B H 0.6657 0.0561 -0.1896 0.111 Uiso 1 1 calc R . . C41 C 0.5850(12) -0.0209(3) -0.0767(10) 0.125(4) Uani 1 1 d . . . H41A H 0.5490 0.0017 -0.1071 0.187 Uiso 1 1 calc R . . H41B H 0.5056 -0.0373 -0.0654 0.187 Uiso 1 1 calc R . . H41C H 0.6516 -0.0310 -0.1343 0.187 Uiso 1 1 calc R . . C42 C 0.6622(9) -0.0149(2) 0.0442(7) 0.073(2) Uani 1 1 d . . . C43 C 0.7349(10) -0.0395(2) 0.1213(9) 0.092(3) Uani 1 1 d . . . H43 H 0.7483 -0.0640 0.1068 0.110 Uiso 1 1 calc R . . C44 C 0.7823(8) -0.02077(18) 0.2214(8) 0.068(2) Uani 1 1 d . . . C45 C 0.8623(11) -0.0315(2) 0.3324(9) 0.099(3) Uani 1 1 d . . . H45A H 0.8770 -0.0107 0.3835 0.148 Uiso 1 1 calc R . . H45B H 0.9546 -0.0414 0.3102 0.148 Uiso 1 1 calc R . . H45C H 0.8078 -0.0493 0.3758 0.148 Uiso 1 1 calc R . . C46 C 0.7962(6) 0.08591(16) 0.2138(5) 0.0436(13) Uani 1 1 d . . . C47 C 0.9010(7) 0.08089(18) 0.1240(6) 0.0565(15) Uani 1 1 d . . . H47 H 0.9344 0.0578 0.1063 0.068 Uiso 1 1 calc R . . C48 C 0.9562(8) 0.1110(2) 0.0602(6) 0.072(2) Uani 1 1 d . . . H48 H 1.0243 0.1075 -0.0008 0.087 Uiso 1 1 calc R . . C49 C 0.9106(9) 0.1449(2) 0.0871(7) 0.076(2) Uani 1 1 d . . . H49 H 0.9488 0.1646 0.0456 0.091 Uiso 1 1 calc R . . C50 C 0.8081(8) 0.15014(18) 0.1756(6) 0.0651(18) Uani 1 1 d . . . H50 H 0.7755 0.1734 0.1924 0.078 Uiso 1 1 calc R . . C51 C 0.7535(7) 0.12138(16) 0.2393(6) 0.0520(15) Uani 1 1 d . . . H51 H 0.6866 0.1255 0.3008 0.062 Uiso 1 1 calc R . . C52 C 0.5730(8) 0.0248(2) 0.5469(6) 0.062(2) Uani 1 1 d . . . H52A H 0.5384 0.0033 0.5071 0.093 Uiso 1 1 calc R . . H52B H 0.5355 0.0258 0.6283 0.093 Uiso 1 1 calc R . . H52C H 0.6770 0.0244 0.5504 0.093 Uiso 1 1 calc R . . C53 C 0.5224(6) 0.05785(15) 0.4754(5) 0.0428(13) Uani 1 1 d . . . H53 H 0.4162 0.0578 0.4776 0.051 Uiso 1 1 calc R . . C54 C 0.5708(6) 0.09271(18) 0.5322(5) 0.0458(16) Uani 1 1 d . . . C55 C 0.4742(8) 0.12073(18) 0.5527(6) 0.0623(17) Uani 1 1 d . . . H55 H 0.3768 0.1180 0.5319 0.075 Uiso 1 1 calc R . . C56 C 0.5239(11) 0.1533(2) 0.6050(8) 0.083(2) Uani 1 1 d . . . H56 H 0.4578 0.1717 0.6198 0.100 Uiso 1 1 calc R . . C57 C 0.6667(11) 0.1585(2) 0.6346(7) 0.085(2) Uani 1 1 d . . . H57 H 0.6988 0.1803 0.6673 0.102 Uiso 1 1 calc R . . C58 C 0.7620(10) 0.1303(2) 0.6143(7) 0.079(2) Uani 1 1 d . . . H58 H 0.8595 0.1334 0.6340 0.095 Uiso 1 1 calc R . . C59 C 0.7180(8) 0.0984(2) 0.5666(5) 0.0638(18) Uani 1 1 d . . . H59 H 0.7849 0.0799 0.5563 0.077 Uiso 1 1 calc R . . C60 C 0.3182(6) 0.09730(15) 0.2769(5) 0.0442(13) Uani 1 1 d . . . C61 C 0.1912(7) 0.08867(19) 0.3434(6) 0.0570(16) Uani 1 1 d . . . H61 H 0.1647 0.0647 0.3559 0.068 Uiso 1 1 calc R . . C62 C 0.1085(7) 0.1163(2) 0.3886(6) 0.068(2) Uani 1 1 d . . . H62 H 0.0261 0.1108 0.4333 0.081 Uiso 1 1 calc R . . C63 C 0.1441(9) 0.1521(2) 0.3697(7) 0.076(2) Uani 1 1 d . . . H63 H 0.0856 0.1703 0.4005 0.091 Uiso 1 1 calc R . . C64 C 0.2647(9) 0.1605(2) 0.3058(8) 0.077(2) Uani 1 1 d . . . H64 H 0.2895 0.1845 0.2941 0.092 Uiso 1 1 calc R . . C65 C 0.3523(8) 0.13327(17) 0.2575(6) 0.0599(17) Uani 1 1 d . . . H65 H 0.4336 0.1393 0.2122 0.072 Uiso 1 1 calc R . . C66 C 0.3305(6) 0.02232(15) 0.2077(5) 0.0448(13) Uani 1 1 d . . . C67 C 0.3394(10) -0.0081(2) 0.2804(9) 0.096(3) Uani 1 1 d . . . H67 H 0.4008 -0.0081 0.3483 0.115 Uiso 1 1 calc R . . C68 C 0.2574(12) -0.0390(3) 0.2536(12) 0.129(5) Uani 1 1 d . . . H68 H 0.2611 -0.0590 0.3046 0.154 Uiso 1 1 calc R . . C69 C 0.1712(9) -0.0391(2) 0.1501(9) 0.086(2) Uani 1 1 d . . . H69 H 0.1206 -0.0599 0.1289 0.103 Uiso 1 1 calc R . . C70 C 0.1590(9) -0.0094(2) 0.0792(7) 0.076(2) Uani 1 1 d . . . H70 H 0.0960 -0.0092 0.0123 0.091 Uiso 1 1 calc R . . C71 C 0.2414(8) 0.02033(19) 0.1077(6) 0.0653(18) Uani 1 1 d . . . H71 H 0.2362 0.0402 0.0560 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0463(2) 0.0629(3) 0.0331(2) -0.00316(19) -0.00228(17) 0.0036(2) Pd2 0.0526(3) 0.0560(3) 0.0331(2) 0.00200(19) -0.00106(18) -0.0063(2) P1 0.0963(16) 0.0662(12) 0.0650(12) 0.0144(9) 0.0118(11) 0.0078(10) P2 0.0356(8) 0.0498(8) 0.0399(7) 0.0003(6) -0.0022(6) -0.0029(6) P3 0.0398(7) 0.0377(7) 0.0363(7) 0.0033(6) -0.0028(5) 0.0001(6) P4 0.0351(7) 0.0371(7) 0.0368(7) -0.0018(5) -0.0009(5) 0.0005(5) P5 0.0384(8) 0.0505(8) 0.0412(8) 0.0003(6) -0.0020(6) 0.0068(6) P6 0.0833(14) 0.0667(12) 0.0715(12) 0.0090(9) -0.0059(11) -0.0126(10) F1 0.61(3) 0.209(10) 0.108(6) -0.025(6) 0.062(10) 0.181(14) F2 0.245(10) 0.243(10) 0.153(7) 0.087(7) 0.029(7) 0.158(9) F3 0.114(5) 0.210(8) 0.203(8) 0.055(7) 0.017(5) -0.040(6) F4 0.120(4) 0.133(5) 0.113(4) 0.021(4) -0.020(3) 0.015(4) F5 0.226(8) 0.138(6) 0.082(4) -0.004(3) 0.012(4) 0.006(5) F6 0.293(14) 0.202(10) 0.276(12) 0.109(9) -0.089(11) -0.158(10) F7 0.76(4) 0.217(12) 0.106(6) -0.014(7) -0.099(12) -0.190(16) F8 0.41(2) 0.205(10) 0.224(11) 0.007(8) -0.039(12) 0.194(13) F9 0.346(13) 0.127(6) 0.101(5) -0.012(4) -0.010(6) -0.017(7) F10 0.189(8) 0.264(11) 0.162(7) 0.020(7) 0.076(6) -0.060(8) F11 0.202(10) 0.147(8) 0.402(17) 0.050(9) -0.117(11) 0.024(7) F12 0.161(9) 0.222(12) 0.48(2) 0.015(13) 0.110(12) -0.089(9) O1 0.46(3) 0.148(10) 0.123(8) -0.021(7) 0.011(11) -0.013(12) N1 0.049(3) 0.051(3) 0.054(3) -0.009(2) 0.001(2) 0.003(2) N2 0.055(3) 0.042(3) 0.053(3) -0.001(2) 0.009(3) 0.005(2) N3 0.052(3) 0.046(3) 0.053(3) -0.002(2) -0.010(2) -0.003(2) N4 0.046(3) 0.057(3) 0.054(3) -0.016(2) -0.007(2) -0.007(2) N5 0.040(2) 0.049(3) 0.030(2) 0.0024(18) 0.0036(19) -0.0005(19) N6 0.037(2) 0.042(3) 0.031(2) -0.0032(18) -0.0019(18) 0.0028(17) C1 0.094(6) 0.092(6) 0.058(5) 0.027(4) 0.012(4) 0.004(5) C2 0.084(6) 0.141(8) 0.039(4) 0.027(4) 0.004(4) -0.004(5) C3 0.074(5) 0.167(9) 0.036(4) 0.026(4) 0.000(3) 0.020(5) C4 0.123(9) 0.114(8) 0.147(9) -0.083(7) 0.025(7) -0.016(6) C5 0.063(5) 0.069(5) 0.101(6) -0.035(4) -0.008(4) -0.001(4) C6 0.077(5) 0.050(4) 0.138(8) -0.035(5) -0.017(5) -0.010(4) C7 0.050(4) 0.053(4) 0.097(6) 0.002(4) -0.022(4) -0.008(3) C8 0.093(6) 0.069(5) 0.114(7) 0.024(5) -0.020(5) -0.033(4) C9 0.033(3) 0.059(4) 0.038(3) -0.004(3) 0.004(2) 0.006(3) C10 0.043(3) 0.040(3) 0.065(4) -0.009(3) 0.005(3) 0.004(2) C11 0.068(5) 0.053(4) 0.095(6) 0.005(4) 0.010(4) 0.005(3) C12 0.066(5) 0.072(5) 0.081(5) 0.022(4) 0.006(4) 0.022(4) C13 0.057(4) 0.096(6) 0.055(4) 0.012(4) -0.010(3) 0.017(4) C14 0.045(3) 0.058(4) 0.049(3) 0.001(3) -0.001(3) 0.004(3) C15 0.038(3) 0.070(4) 0.031(3) -0.002(3) -0.003(2) 0.000(3) C16 0.092(6) 0.064(5) 0.045(4) 0.010(3) -0.006(4) 0.008(4) C17 0.043(4) 0.074(5) 0.029(3) -0.009(3) 0.001(3) -0.010(3) C18 0.088(6) 0.092(6) 0.071(5) -0.042(4) 0.020(4) -0.025(5) C19 0.132(9) 0.072(6) 0.112(8) -0.038(5) 0.036(7) -0.028(5) C20 0.124(8) 0.081(6) 0.084(6) -0.032(5) 0.008(6) 0.009(6) C21 0.071(5) 0.120(7) 0.059(4) -0.018(4) 0.001(4) 0.036(5) C22 0.053(4) 0.074(4) 0.035(3) -0.006(3) -0.004(3) 0.006(3) C23 0.040(3) 0.037(3) 0.045(3) -0.002(2) -0.002(2) -0.002(2) C24 0.035(3) 0.051(3) 0.045(3) 0.006(2) 0.002(2) 0.005(2) C25 0.035(3) 0.070(4) 0.044(3) -0.002(3) -0.007(2) 0.001(3) C26 0.049(4) 0.050(4) 0.059(4) 0.002(3) -0.008(3) -0.014(3) C27 0.065(4) 0.043(3) 0.079(5) 0.009(3) -0.006(4) -0.011(3) C28 0.057(4) 0.040(3) 0.057(4) 0.009(3) -0.010(3) 0.003(3) C29 0.033(3) 0.047(3) 0.047(3) -0.002(2) -0.006(2) 0.004(2) C30 0.089(6) 0.051(4) 0.105(6) 0.015(4) 0.046(5) 0.009(4) C31 0.122(8) 0.047(4) 0.160(10) 0.022(5) 0.050(8) 0.016(5) C32 0.077(5) 0.063(5) 0.104(6) -0.014(4) -0.004(5) 0.023(4) C33 0.076(5) 0.075(5) 0.071(5) -0.016(4) 0.013(4) 0.021(4) C34 0.070(4) 0.057(4) 0.048(3) 0.004(3) 0.004(3) 0.012(3) C35 0.138(11) 0.153(12) 0.167(13) -0.048(10) -0.042(10) 0.023(9) C36 0.092(7) 0.120(9) 0.130(10) -0.048(8) -0.004(7) -0.006(6) C37 0.177(16) 0.29(2) 0.134(12) -0.076(14) -0.014(11) 0.053(15) C38 0.101(6) 0.075(5) 0.073(5) 0.032(4) -0.009(5) -0.002(4) C39 0.112(9) 0.147(9) 0.062(6) 0.042(6) 0.005(5) -0.012(7) C40 0.095(7) 0.139(8) 0.043(4) 0.023(4) 0.009(4) -0.021(6) C41 0.124(9) 0.115(8) 0.135(9) -0.085(7) -0.028(7) 0.014(6) C42 0.068(5) 0.066(5) 0.087(5) -0.033(4) 0.012(4) -0.001(4) C43 0.086(6) 0.051(4) 0.139(8) -0.036(5) -0.003(5) 0.015(4) C44 0.061(4) 0.048(4) 0.096(5) 0.004(4) 0.023(4) 0.015(3) C45 0.108(7) 0.078(6) 0.110(7) 0.026(5) 0.008(6) 0.046(5) C46 0.029(3) 0.060(4) 0.042(3) -0.009(3) -0.003(2) -0.005(2) C47 0.041(3) 0.063(4) 0.066(4) -0.011(3) 0.006(3) -0.004(3) C48 0.068(5) 0.087(5) 0.063(4) -0.009(4) 0.022(4) -0.027(4) C49 0.092(6) 0.068(5) 0.068(4) 0.001(4) 0.021(4) -0.028(4) C50 0.079(5) 0.047(4) 0.070(4) -0.011(3) 0.004(4) -0.013(3) C51 0.049(4) 0.056(4) 0.050(3) -0.011(3) 0.006(3) -0.013(3) C52 0.079(5) 0.061(5) 0.046(4) 0.011(3) -0.010(4) 0.001(3) C53 0.040(3) 0.054(4) 0.034(3) 0.005(2) 0.000(2) -0.003(2) C54 0.051(4) 0.057(4) 0.029(3) 0.007(2) 0.002(3) -0.002(3) C55 0.067(5) 0.063(4) 0.057(4) -0.005(3) -0.007(3) 0.001(3) C56 0.121(8) 0.053(4) 0.076(5) -0.003(4) -0.006(5) 0.006(4) C57 0.108(7) 0.083(6) 0.065(5) -0.017(4) 0.008(5) -0.028(5) C58 0.075(5) 0.106(6) 0.056(4) -0.018(4) 0.001(4) -0.041(5) C59 0.063(5) 0.090(5) 0.039(3) -0.005(3) 0.011(3) -0.005(4) C60 0.043(3) 0.050(3) 0.039(3) 0.000(2) -0.004(2) 0.007(2) C61 0.054(4) 0.067(4) 0.050(3) 0.002(3) -0.005(3) 0.006(3) C62 0.046(4) 0.108(6) 0.049(4) -0.008(4) 0.004(3) 0.018(4) C63 0.074(5) 0.078(6) 0.076(5) -0.003(4) -0.001(4) 0.030(4) C64 0.079(5) 0.053(4) 0.097(6) 0.004(4) -0.008(5) 0.019(4) C65 0.062(4) 0.045(4) 0.073(4) 0.003(3) -0.003(3) 0.015(3) C66 0.038(3) 0.046(3) 0.050(3) 0.002(3) 0.001(3) 0.001(2) C67 0.092(6) 0.063(5) 0.132(8) 0.035(5) -0.059(6) -0.031(4) C68 0.120(8) 0.071(6) 0.194(12) 0.043(7) -0.075(8) -0.031(5) C69 0.083(6) 0.058(4) 0.116(7) -0.011(4) -0.010(5) -0.018(4) C70 0.075(5) 0.085(5) 0.068(4) -0.009(4) -0.010(4) -0.025(4) C71 0.073(5) 0.067(4) 0.056(4) 0.005(3) -0.007(3) -0.022(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 N4 2.100(5) . ? Pd1 C1 2.127(8) . ? Pd1 C2 2.133(7) . ? Pd1 C3 2.213(7) . ? Pd1 P4 2.2970(14) . ? Pd2 C38 2.107(7) . ? Pd2 N1 2.116(5) . ? Pd2 C39 2.155(8) . ? Pd2 C40 2.189(7) . ? Pd2 P3 2.2958(14) . ? P1 F1 1.478(8) . ? P1 F6 1.495(9) . ? P1 F2 1.521(7) . ? P1 F5 1.557(6) . ? P1 F4 1.581(6) . ? P1 F3 1.588(8) . ? P2 N6 1.704(4) . ? P2 N3 1.734(5) . ? P2 C9 1.832(6) . ? P3 N5 1.710(4) . ? P3 C60 1.809(6) . ? P3 C66 1.813(6) . ? P4 N6 1.716(4) . ? P4 C29 1.805(6) . ? P4 C23 1.816(5) . ? P5 N5 1.703(4) . ? P5 N2 1.736(5) . ? P5 C46 1.815(6) . ? P6 F8 1.444(9) . ? P6 F7 1.457(9) . ? P6 F10 1.509(8) . ? P6 F9 1.510(7) . ? P6 F12 1.519(9) . ? P6 F11 1.543(9) . ? O1 C36 1.249(15) . ? N1 C42 1.322(8) . ? N1 N2 1.376(7) . ? N2 C44 1.389(8) . ? N3 N4 1.385(7) . ? N3 C7 1.389(8) . ? N4 C5 1.341(9) . ? N5 C53 1.529(6) . ? N6 C15 1.534(6) . ? C1 C2 1.386(12) . ? C2 C3 1.385(12) . ? C4 C5 1.506(13) . ? C5 C6 1.370(13) . ? C6 C7 1.359(12) . ? C7 C8 1.496(12) . ? C9 C14 1.371(8) . ? C9 C10 1.389(8) . ? C10 C11 1.391(9) . ? C11 C12 1.377(11) . ? C12 C13 1.393(11) . ? C13 C14 1.380(9) . ? C15 C17 1.518(9) . ? C15 C16 1.550(10) . ? C17 C18 1.364(10) . ? C17 C22 1.413(9) . ? C18 C19 1.402(13) . ? C19 C20 1.379(14) . ? C20 C21 1.361(13) . ? C21 C22 1.394(11) . ? C23 C28 1.388(8) . ? C23 C24 1.389(8) . ? C24 C25 1.385(8) . ? C25 C26 1.371(9) . ? C26 C27 1.365(9) . ? C27 C28 1.376(9) . ? C29 C34 1.382(9) . ? C29 C30 1.398(9) . ? C30 C31 1.398(11) . ? C31 C32 1.353(13) . ? C32 C33 1.356(11) . ? C33 C34 1.396(9) . ? C35 C36 1.520(18) . ? C36 C37 1.277(17) . ? C38 C39 1.392(14) . ? C39 C40 1.326(13) . ? C41 C42 1.513(12) . ? C42 C43 1.406(12) . ? C43 C44 1.364(12) . ? C44 C45 1.470(12) . ? C46 C47 1.398(8) . ? C46 C51 1.400(8) . ? C47 C48 1.413(10) . ? C48 C49 1.357(11) . ? C49 C50 1.374(10) . ? C50 C51 1.372(9) . ? C52 C53 1.524(9) . ? C53 C54 1.499(8) . ? C54 C55 1.388(9) . ? C54 C59 1.420(9) . ? C55 C56 1.409(11) . ? C56 C57 1.367(13) . ? C57 C58 1.384(13) . ? C58 C59 1.355(11) . ? C60 C65 1.386(9) . ? C60 C61 1.422(9) . ? C61 C62 1.372(10) . ? C62 C63 1.382(11) . ? C63 C64 1.356(11) . ? C64 C65 1.399(10) . ? C66 C71 1.364(9) . ? C66 C67 1.381(10) . ? C67 C68 1.401(12) . ? C68 C69 1.377(13) . ? C69 C70 1.348(12) . ? C70 C71 1.374(10) . ? 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 N4 Pd1 C1 169.5(3) . . ? N4 Pd1 C2 131.8(3) . . ? C1 Pd1 C2 38.0(3) . . ? N4 Pd1 C3 101.7(3) . . ? C1 Pd1 C3 67.9(4) . . ? C2 Pd1 C3 37.1(3) . . ? N4 Pd1 P4 86.20(14) . . ? C1 Pd1 P4 104.1(2) . . ? C2 Pd1 P4 135.7(2) . . ? C3 Pd1 P4 172.0(3) . . ? C38 Pd2 N1 169.7(3) . . ? C38 Pd2 C39 38.1(4) . . ? N1 Pd2 C39 131.8(4) . . ? C38 Pd2 C40 67.9(4) . . ? N1 Pd2 C40 102.1(3) . . ? C39 Pd2 C40 35.5(3) . . ? C38 Pd2 P3 103.3(3) . . ? N1 Pd2 P3 86.61(14) . . ? C39 Pd2 P3 135.8(3) . . ? C40 Pd2 P3 171.0(3) . . ? F1 P1 F6 98.2(9) . . ? F1 P1 F2 92.7(7) . . ? F6 P1 F2 84.0(7) . . ? F1 P1 F5 174.8(7) . . ? F6 P1 F5 86.8(6) . . ? F2 P1 F5 89.2(5) . . ? F1 P1 F4 88.2(6) . . ? F6 P1 F4 92.4(6) . . ? F2 P1 F4 176.3(6) . . ? F5 P1 F4 90.2(4) . . ? F1 P1 F3 89.2(8) . . ? F6 P1 F3 171.9(7) . . ? F2 P1 F3 99.0(6) . . ? F5 P1 F3 85.8(5) . . ? F4 P1 F3 84.6(4) . . ? N6 P2 N3 102.8(2) . . ? N6 P2 C9 105.2(2) . . ? N3 P2 C9 98.0(2) . . ? N5 P3 C60 106.2(2) . . ? N5 P3 C66 109.8(2) . . ? C60 P3 C66 105.4(3) . . ? N5 P3 Pd2 108.69(15) . . ? C60 P3 Pd2 122.48(19) . . ? C66 P3 Pd2 103.93(19) . . ? N6 P4 C29 110.7(2) . . ? N6 P4 C23 106.2(2) . . ? C29 P4 C23 102.4(3) . . ? N6 P4 Pd1 107.87(15) . . ? C29 P4 Pd1 104.31(19) . . ? C23 P4 Pd1 124.93(19) . . ? N5 P5 N2 103.0(2) . . ? N5 P5 C46 104.6(2) . . ? N2 P5 C46 98.5(2) . . ? F8 P6 F7 92.4(9) . . ? F8 P6 F10 103.8(9) . . ? F7 P6 F10 89.1(8) . . ? F8 P6 F9 89.8(6) . . ? F7 P6 F9 177.3(11) . . ? F10 P6 F9 91.9(6) . . ? F8 P6 F12 85.1(9) . . ? F7 P6 F12 86.0(9) . . ? F10 P6 F12 170.0(8) . . ? F9 P6 F12 92.7(8) . . ? F8 P6 F11 171.6(8) . . ? F7 P6 F11 93.3(9) . . ? F10 P6 F11 82.4(7) . . ? F9 P6 F11 84.4(6) . . ? F12 P6 F11 89.2(7) . . ? C42 N1 N2 107.4(5) . . ? C42 N1 Pd2 131.7(5) . . ? N2 N1 Pd2 120.5(3) . . ? N1 N2 C44 109.5(5) . . ? N1 N2 P5 123.4(4) . . ? C44 N2 P5 126.1(5) . . ? N4 N3 C7 109.7(5) . . ? N4 N3 P2 122.3(4) . . ? C7 N3 P2 127.3(5) . . ? C5 N4 N3 105.7(6) . . ? C5 N4 Pd1 132.8(5) . . ? N3 N4 Pd1 121.1(3) . . ? C53 N5 P5 115.9(3) . . ? C53 N5 P3 122.3(3) . . ? P5 N5 P3 121.8(2) . . ? C15 N6 P2 115.1(3) . . ? C15 N6 P4 123.0(3) . . ? P2 N6 P4 121.8(2) . . ? C2 C1 Pd1 71.2(5) . . ? C3 C2 C1 122.2(8) . . ? C3 C2 Pd1 74.6(4) . . ? C1 C2 Pd1 70.8(4) . . ? C2 C3 Pd1 68.3(4) . . ? N4 C5 C6 110.3(7) . . ? N4 C5 C4 117.7(8) . . ? C6 C5 C4 132.0(8) . . ? C7 C6 C5 108.6(7) . . ? C6 C7 N3 105.7(7) . . ? C6 C7 C8 132.5(7) . . ? N3 C7 C8 121.8(7) . . ? C14 C9 C10 119.1(5) . . ? C14 C9 P2 119.8(4) . . ? C10 C9 P2 119.9(4) . . ? C9 C10 C11 119.6(6) . . ? C12 C11 C10 120.9(7) . . ? C11 C12 C13 119.1(6) . . ? C14 C13 C12 119.6(6) . . ? C9 C14 C13 121.5(6) . . ? C17 C15 N6 109.6(4) . . ? C17 C15 C16 113.6(5) . . ? N6 C15 C16 111.2(5) . . ? C18 C17 C22 118.8(7) . . ? C18 C17 C15 119.3(6) . . ? C22 C17 C15 121.8(6) . . ? C17 C18 C19 121.3(8) . . ? C20 C19 C18 119.6(8) . . ? C21 C20 C19 119.7(8) . . ? C20 C21 C22 121.5(8) . . ? C21 C22 C17 119.1(7) . . ? C28 C23 C24 118.4(5) . . ? C28 C23 P4 120.6(4) . . ? C24 C23 P4 120.8(4) . . ? C25 C24 C23 120.5(5) . . ? C26 C25 C24 120.3(6) . . ? C27 C26 C25 119.5(6) . . ? C26 C27 C28 121.2(6) . . ? C27 C28 C23 120.1(6) . . ? C34 C29 C30 117.4(6) . . ? C34 C29 P4 116.4(4) . . ? C30 C29 P4 126.1(5) . . ? C31 C30 C29 119.9(7) . . ? C32 C31 C30 120.7(8) . . ? C31 C32 C33 120.9(7) . . ? C32 C33 C34 119.2(7) . . ? C29 C34 C33 121.8(6) . . ? O1 C36 C37 121.7(15) . . ? O1 C36 C35 116.7(12) . . ? C37 C36 C35 121.6(15) . . ? C39 C38 Pd2 72.8(5) . . ? C40 C39 C38 123.9(10) . . ? C40 C39 Pd2 73.6(5) . . ? C38 C39 Pd2 69.1(4) . . ? C39 C40 Pd2 70.8(5) . . ? N1 C42 C43 109.5(7) . . ? N1 C42 C41 120.2(8) . . ? C43 C42 C41 130.3(7) . . ? C44 C43 C42 107.5(6) . . ? C43 C44 N2 106.2(7) . . ? C43 C44 C45 132.9(7) . . ? N2 C44 C45 120.9(7) . . ? C47 C46 C51 117.6(6) . . ? C47 C46 P5 120.6(5) . . ? C51 C46 P5 120.8(4) . . ? C46 C47 C48 119.8(6) . . ? C49 C48 C47 120.6(6) . . ? C48 C49 C50 120.1(7) . . ? C51 C50 C49 120.5(7) . . ? C50 C51 C46 121.4(6) . . ? C54 C53 C52 113.0(5) . . ? C54 C53 N5 110.7(4) . . ? C52 C53 N5 112.7(5) . . ? C55 C54 C59 117.4(6) . . ? C55 C54 C53 121.4(6) . . ? C59 C54 C53 121.1(6) . . ? C54 C55 C56 119.9(7) . . ? C57 C56 C55 121.8(8) . . ? C56 C57 C58 117.9(7) . . ? C59 C58 C57 122.2(8) . . ? C58 C59 C54 120.9(8) . . ? C65 C60 C61 119.0(5) . . ? C65 C60 P3 119.5(5) . . ? C61 C60 P3 121.4(5) . . ? C62 C61 C60 118.8(7) . . ? C61 C62 C63 121.8(7) . . ? C64 C63 C62 119.6(7) . . ? C63 C64 C65 120.7(7) . . ? C60 C65 C64 120.1(7) . . ? C71 C66 C67 116.7(6) . . ? C71 C66 P3 117.5(5) . . ? C67 C66 P3 125.4(5) . . ? C66 C67 C68 121.1(8) . . ? C69 C68 C67 118.7(8) . . ? C70 C69 C68 121.1(7) . . ? C69 C70 C71 118.6(7) . . ? C66 C71 C70 123.6(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.685 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.201 # ====== END data_complex_7a _database_code_CSD 190878 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta-3-dimethylallyl)[eta-2-{N,N-(diphenylphosphino) (phenyl, 3,5-dimethylpyrazolylphosphino) (S)-1-phenylethylamine}-kappa-P,N] palladium(II)hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point '204-206 0C dec.' _chemical_formula_moiety ; [Pd(eta-3-Me2-C3H3){eta-2-(SR)-Ph2PN((S)-*CHMePh)PPh(N2C3HMe2-3,5)}](PF6) ; _chemical_formula_sum 'C36 H40 F6 N3 P3 Pd' _chemical_formula_weight 828.02 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' '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 'P212121' 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 9.474(4) _cell_length_b 19.627(4) _cell_length_c 19.837(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3688.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.694 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\alpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6 _diffrn_reflns_number 3638 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3638 _reflns_number_gt 2912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-32 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines(Farrugia, 1999)' _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^)+(0.0786P)^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 -0.08(5) _refine_ls_number_reflns 3638 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1081 _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 -0.17938(6) -0.92521(2) -0.92239(3) 0.05571(18) Uani 1 1 d . . . P1 P -0.38202(16) -1.07024(9) -0.92558(9) 0.0489(4) Uani 1 1 d . . . P2 P -0.07946(17) -1.03039(8) -0.94202(8) 0.0432(4) Uani 1 1 d . . . P3 P -0.2237(3) -0.27389(15) -0.68906(13) 0.0864(7) Uani 1 1 d . . . F1 F -0.2012(18) -0.2119(8) -0.7306(7) 0.297(9) Uani 1 1 d . . . F2 F -0.3450(16) -0.2430(8) -0.6533(8) 0.266(7) Uani 1 1 d . . . F3 F -0.1129(18) -0.3110(11) -0.7269(11) 0.346(11) Uani 1 1 d . . . F4 F -0.122(2) -0.2444(7) -0.6410(8) 0.307(11) Uani 1 1 d . . . F5 F -0.224(3) -0.3373(5) -0.6525(7) 0.315(10) Uani 1 1 d . . . F6 F -0.3243(18) -0.2961(8) -0.7399(8) 0.281(8) Uani 1 1 d . . . N1 N -0.2116(6) -1.0899(3) -0.9464(3) 0.0479(13) Uani 1 1 d . . . N2 N -0.3655(6) -1.0302(3) -0.8475(3) 0.0568(15) Uani 1 1 d . . . N3 N -0.2778(6) -0.9754(3) -0.8383(3) 0.0561(14) Uani 1 1 d . . . C1 C -0.3108(18) -0.7863(6) -0.8535(7) 0.144(6) Uani 1 1 d . . . H1A H -0.4052 -0.8031 -0.8482 0.217 Uiso 1 1 calc R . . H1B H -0.3130 -0.7377 -0.8593 0.217 Uiso 1 1 calc R . . H1C H -0.2563 -0.7974 -0.8142 0.217 Uiso 1 1 calc R . . C2 C -0.250(2) -0.8158(5) -0.9092(8) 0.140(6) Uani 1 1 d . . . H2 H -0.3316 -0.8155 -0.9398 0.168 Uiso 1 1 calc R . . C3 C -0.1542(17) -0.8213(4) -0.9509(6) 0.109(4) Uani 1 1 d . . . H3 H -0.0717 -0.8080 -0.9241 0.131 Uiso 1 1 calc R . . C4 C -0.0978(16) -0.8581(5) -0.9966(6) 0.112(4) Uani 1 1 d . . . H4 H -0.1753 -0.8593 -1.0293 0.135 Uiso 1 1 calc R . . C5 C 0.0181(19) -0.8675(7) -1.0404(8) 0.170(8) Uani 1 1 d . . . H5A H 0.0005 -0.9059 -1.0692 0.255 Uiso 1 1 calc R . . H5B H 0.1019 -0.8755 -1.0144 0.255 Uiso 1 1 calc R . . H5C H 0.0306 -0.8273 -1.0675 0.255 Uiso 1 1 calc R . . C6 C -0.1595(14) -0.9203(5) -0.7425(5) 0.104(4) Uani 1 1 d . . . H6A H -0.1265 -0.8912 -0.7781 0.156 Uiso 1 1 calc R . . H6B H -0.0805 -0.9424 -0.7215 0.156 Uiso 1 1 calc R . . H6C H -0.2090 -0.8936 -0.7096 0.156 Uiso 1 1 calc R . . C7 C -0.2559(9) -0.9724(4) -0.7707(4) 0.068(2) Uani 1 1 d . . . C8 C -0.3279(10) -1.0228(4) -0.7391(4) 0.075(2) Uani 1 1 d . . . H8 H -0.3296 -1.0305 -0.6929 0.090 Uiso 1 1 calc R . . C9 C -0.3965(9) -1.0599(4) -0.7858(4) 0.065(2) Uani 1 1 d . . . C10 C -0.4888(10) -1.1216(5) -0.7811(5) 0.084(3) Uani 1 1 d . . . H10A H -0.5210 -1.1340 -0.8253 0.126 Uiso 1 1 calc R . . H10B H -0.5685 -1.1118 -0.7529 0.126 Uiso 1 1 calc R . . H10C H -0.4359 -1.1587 -0.7621 0.126 Uiso 1 1 calc R . . C11 C -0.4292(7) -0.9959(4) -0.9755(3) 0.0519(16) Uani 1 1 d . . . C12 C -0.3948(8) -0.9953(4) -1.0452(4) 0.0617(18) Uani 1 1 d . . . H12 H -0.3366 -1.0288 -1.0631 0.074 Uiso 1 1 calc R . . C13 C -0.4482(10) -0.9448(5) -1.0860(4) 0.079(2) Uani 1 1 d . . . H13 H -0.4253 -0.9444 -1.1316 0.095 Uiso 1 1 calc R . . C14 C -0.5360(11) -0.8945(5) -1.0600(5) 0.087(3) Uani 1 1 d . . . H14 H -0.5703 -0.8601 -1.0878 0.104 Uiso 1 1 calc R . . C15 C -0.5709(10) -0.8960(5) -0.9937(4) 0.081(3) Uani 1 1 d . . . H15 H -0.6308 -0.8628 -0.9763 0.097 Uiso 1 1 calc R . . C16 C -0.5191(8) -0.9461(4) -0.9516(4) 0.064(2) Uani 1 1 d . . . H16 H -0.5452 -0.9463 -0.9064 0.077 Uiso 1 1 calc R . . C17 C -0.1778(8) -1.1645(3) -0.9587(3) 0.0505(15) Uani 1 1 d . . . H17 H -0.0756 -1.1698 -0.9529 0.061 Uiso 1 1 calc R . . C18 C -0.2480(9) -1.2118(3) -0.9081(3) 0.0617(19) Uani 1 1 d . . . H18A H -0.2247 -1.1974 -0.8632 0.093 Uiso 1 1 calc R . . H18B H -0.2151 -1.2575 -0.9151 0.093 Uiso 1 1 calc R . . H18C H -0.3485 -1.2102 -0.9141 0.093 Uiso 1 1 calc R . . C19 C -0.2122(7) -1.1864(3) -1.0307(3) 0.0484(15) Uani 1 1 d . . . C20 C -0.3496(9) -1.1945(4) -1.0524(4) 0.067(2) Uani 1 1 d . . . H20 H -0.4242 -1.1828 -1.0242 0.081 Uiso 1 1 calc R . . C21 C -0.3764(11) -1.2203(5) -1.1163(5) 0.081(3) Uani 1 1 d . . . H21 H -0.4690 -1.2271 -1.1302 0.097 Uiso 1 1 calc R . . C22 C -0.2687(16) -1.2355(5) -1.1586(5) 0.100(4) Uani 1 1 d . . . H22 H -0.2886 -1.2535 -1.2009 0.120 Uiso 1 1 calc R . . C23 C -0.1325(12) -1.2251(5) -1.1404(5) 0.086(3) Uani 1 1 d . . . H23 H -0.0595 -1.2335 -1.1706 0.103 Uiso 1 1 calc R . . C24 C -0.1035(9) -1.2012(4) -1.0748(4) 0.072(2) Uani 1 1 d . . . H24 H -0.0104 -1.1955 -1.0611 0.087 Uiso 1 1 calc R . . C25 C 0.0226(7) -1.0457(3) -0.8653(3) 0.0469(15) Uani 1 1 d . . . C26 C -0.0074(8) -1.0962(4) -0.8194(3) 0.0572(17) Uani 1 1 d . . . H26 H -0.0777 -1.1279 -0.8288 0.069 Uiso 1 1 calc R . . C27 C 0.0669(9) -1.1001(4) -0.7593(4) 0.0631(19) Uani 1 1 d . . . H27 H 0.0455 -1.1344 -0.7285 0.076 Uiso 1 1 calc R . . C28 C 0.1708(9) -1.0544(4) -0.7447(3) 0.0649(19) Uani 1 1 d . . . H28 H 0.2206 -1.0578 -0.7044 0.078 Uiso 1 1 calc R . . C29 C 0.2021(8) -1.0028(5) -0.7898(4) 0.073(2) Uani 1 1 d . . . H29 H 0.2714 -0.9708 -0.7797 0.087 Uiso 1 1 calc R . . C30 C 0.1276(7) -0.9993(4) -0.8513(4) 0.0618(19) Uani 1 1 d . . . H30 H 0.1494 -0.9655 -0.8824 0.074 Uiso 1 1 calc R . . C31 C 0.0419(7) -1.0531(3) -1.0090(3) 0.0494(16) Uani 1 1 d . . . C32 C 0.1744(8) -1.0794(4) -0.9991(4) 0.0585(16) Uani 1 1 d . . . H32 H 0.2057 -1.0876 -0.9554 0.070 Uiso 1 1 calc R . . C33 C 0.2617(8) -1.0941(4) -1.0522(4) 0.072(2) Uani 1 1 d . . . H33 H 0.3523 -1.1103 -1.0438 0.086 Uiso 1 1 calc R . . C34 C 0.2189(9) -1.0855(5) -1.1165(4) 0.075(2) Uani 1 1 d . . . H34 H 0.2764 -1.0985 -1.1523 0.090 Uiso 1 1 calc R . . C35 C 0.0869(10) -1.0569(5) -1.1281(4) 0.085(3) Uani 1 1 d . . . H35 H 0.0576 -1.0484 -1.1720 0.102 Uiso 1 1 calc R . . C36 C 0.0008(8) -1.0413(5) -1.0759(4) 0.074(2) Uani 1 1 d . . . H36 H -0.0873 -1.0223 -1.0846 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0627(3) 0.0434(3) 0.0610(3) 0.0035(3) -0.0053(3) -0.0006(3) P1 0.0404(8) 0.0539(9) 0.0525(9) 0.0016(10) 0.0017(7) -0.0005(8) P2 0.0417(8) 0.0438(8) 0.0440(8) 0.0043(6) -0.0025(7) -0.0026(7) P3 0.0938(18) 0.0946(17) 0.0708(14) 0.0173(13) -0.0013(13) 0.0203(15) F1 0.239(14) 0.339(18) 0.312(16) 0.225(15) -0.065(15) -0.081(15) F2 0.217(12) 0.268(15) 0.312(18) -0.062(14) 0.116(14) 0.038(11) F3 0.252(16) 0.38(3) 0.40(3) -0.07(2) 0.135(17) 0.145(17) F4 0.37(2) 0.219(13) 0.335(18) -0.095(13) -0.228(18) 0.078(14) F5 0.54(3) 0.121(7) 0.286(14) 0.100(9) 0.02(2) 0.030(15) F6 0.265(15) 0.321(17) 0.256(14) -0.066(13) -0.127(14) -0.053(15) N1 0.044(3) 0.047(3) 0.053(3) -0.001(2) -0.002(2) -0.005(2) N2 0.062(4) 0.059(3) 0.049(3) 0.007(3) 0.008(3) 0.016(3) N3 0.059(4) 0.053(3) 0.057(3) -0.002(3) -0.006(3) 0.009(3) C1 0.185(15) 0.084(7) 0.164(12) -0.005(7) 0.012(12) 0.072(10) C2 0.199(16) 0.048(5) 0.173(14) 0.014(7) 0.053(13) 0.021(7) C3 0.161(12) 0.040(4) 0.127(9) 0.027(5) 0.024(9) 0.026(6) C4 0.149(11) 0.062(6) 0.126(9) 0.028(6) 0.025(9) -0.017(7) C5 0.213(18) 0.097(9) 0.199(16) 0.063(10) 0.094(15) 0.007(10) C6 0.142(10) 0.099(7) 0.071(5) -0.026(5) -0.009(6) 0.040(8) C7 0.073(5) 0.078(5) 0.054(4) -0.015(4) -0.003(4) 0.022(4) C8 0.092(6) 0.086(5) 0.046(4) 0.013(4) 0.007(5) 0.023(5) C9 0.070(5) 0.073(5) 0.052(4) 0.014(4) 0.014(4) 0.022(4) C10 0.076(6) 0.090(6) 0.086(6) 0.032(5) 0.030(5) 0.004(5) C11 0.043(3) 0.062(4) 0.051(4) 0.002(3) -0.006(3) 0.005(3) C12 0.052(4) 0.072(5) 0.061(4) 0.003(4) -0.009(3) 0.006(4) C13 0.080(5) 0.102(6) 0.055(4) 0.015(4) -0.011(4) 0.023(5) C14 0.095(7) 0.089(6) 0.077(6) 0.020(5) -0.018(5) 0.017(5) C15 0.076(6) 0.089(6) 0.078(6) -0.001(5) -0.017(5) 0.037(5) C16 0.054(4) 0.085(5) 0.053(4) -0.002(4) 0.005(3) 0.017(4) C17 0.045(3) 0.041(3) 0.065(4) 0.005(3) -0.003(4) 0.001(3) C18 0.070(4) 0.049(4) 0.067(5) 0.010(3) 0.003(4) -0.007(4) C19 0.045(4) 0.041(3) 0.060(4) -0.005(3) 0.001(3) 0.002(3) C20 0.063(5) 0.077(5) 0.061(4) -0.005(4) -0.004(4) -0.013(4) C21 0.084(6) 0.082(6) 0.076(6) 0.000(5) -0.009(5) -0.013(5) C22 0.150(12) 0.071(6) 0.078(6) -0.011(5) -0.006(7) -0.023(7) C23 0.095(7) 0.096(7) 0.066(5) -0.017(5) 0.011(5) 0.005(6) C24 0.064(4) 0.074(5) 0.080(5) -0.013(5) 0.005(5) 0.014(4) C25 0.044(3) 0.050(3) 0.048(4) -0.001(3) -0.009(3) 0.003(3) C26 0.061(4) 0.057(4) 0.054(4) 0.003(3) -0.005(3) 0.004(3) C27 0.076(5) 0.069(4) 0.044(4) 0.005(3) -0.004(4) 0.007(4) C28 0.066(4) 0.086(5) 0.043(3) -0.002(3) -0.006(4) 0.008(5) C29 0.058(5) 0.093(6) 0.067(5) -0.013(4) -0.011(4) -0.003(5) C30 0.058(4) 0.074(5) 0.053(4) 0.006(4) -0.011(3) -0.012(4) C31 0.044(4) 0.055(4) 0.049(3) 0.006(3) 0.001(3) -0.007(3) C32 0.047(4) 0.066(4) 0.062(4) -0.002(3) -0.003(3) 0.013(4) C33 0.045(4) 0.081(5) 0.090(6) -0.008(4) 0.012(4) 0.003(4) C34 0.071(5) 0.089(6) 0.063(5) 0.002(4) 0.020(4) 0.004(5) C35 0.076(6) 0.121(8) 0.058(4) 0.017(5) 0.013(4) -0.002(6) C36 0.055(4) 0.116(6) 0.053(4) 0.015(5) 0.010(4) 0.017(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 C4 2.121(10) . ? Pd1 C3 2.129(8) . ? Pd1 N3 2.150(6) . ? Pd1 C2 2.265(11) . ? Pd1 P2 2.3041(17) . ? P1 N1 1.711(6) . ? P1 N2 1.744(6) . ? P1 C11 1.819(7) . ? P2 N1 1.713(5) . ? P2 C31 1.813(7) . ? P2 C25 1.828(6) . ? P3 F5 1.440(9) . ? P3 F6 1.455(11) . ? P3 F4 1.473(12) . ? P3 F2 1.481(12) . ? P3 F3 1.481(12) . ? P3 F1 1.484(10) . ? N1 C17 1.520(8) . ? N2 N3 1.372(9) . ? N2 C9 1.386(9) . ? N3 C7 1.357(9) . ? C1 C2 1.373(18) . ? C2 C3 1.233(18) . ? C3 C4 1.276(16) . ? C4 C5 1.413(19) . ? C6 C7 1.481(13) . ? C7 C8 1.355(12) . ? C8 C9 1.345(11) . ? C9 C10 1.497(12) . ? C11 C16 1.382(10) . ? C11 C12 1.420(10) . ? C12 C13 1.376(11) . ? C13 C14 1.390(13) . ? C14 C15 1.358(12) . ? C15 C16 1.379(11) . ? C17 C18 1.519(9) . ? C17 C19 1.527(9) . ? C19 C20 1.381(11) . ? C19 C24 1.382(10) . ? C20 C21 1.387(12) . ? C21 C22 1.354(15) . ? C22 C23 1.356(16) . ? C23 C24 1.409(13) . ? C25 C26 1.375(10) . ? C25 C30 1.378(9) . ? C26 C27 1.387(10) . ? C27 C28 1.364(11) . ? C28 C29 1.384(11) . ? C29 C30 1.411(11) . ? C31 C32 1.372(10) . ? C31 C36 1.403(10) . ? C32 C33 1.370(10) . ? C33 C34 1.348(12) . ? C34 C35 1.390(13) . ? C35 C36 1.353(11) . ? 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 C4 Pd1 C3 34.9(4) . . ? C4 Pd1 N3 168.8(4) . . ? C3 Pd1 N3 133.9(4) . . ? C4 Pd1 C2 66.3(5) . . ? C3 Pd1 C2 32.4(5) . . ? N3 Pd1 C2 102.5(4) . . ? C4 Pd1 P2 106.8(4) . . ? C3 Pd1 P2 140.1(4) . . ? N3 Pd1 P2 84.20(15) . . ? C2 Pd1 P2 172.2(4) . . ? N1 P1 N2 103.3(3) . . ? N1 P1 C11 106.3(3) . . ? N2 P1 C11 98.3(3) . . ? N1 P2 C31 105.0(3) . . ? N1 P2 C25 108.4(3) . . ? C31 P2 C25 103.5(3) . . ? N1 P2 Pd1 108.58(19) . . ? C31 P2 Pd1 127.2(2) . . ? C25 P2 Pd1 103.0(2) . . ? F5 P3 F6 95.0(10) . . ? F5 P3 F4 91.0(10) . . ? F6 P3 F4 174.0(9) . . ? F5 P3 F2 96.2(11) . . ? F6 P3 F2 86.9(9) . . ? F4 P3 F2 92.1(9) . . ? F5 P3 F3 80.4(10) . . ? F6 P3 F3 88.0(10) . . ? F4 P3 F3 93.4(11) . . ? F2 P3 F3 173.7(11) . . ? F5 P3 F1 171.2(13) . . ? F6 P3 F1 87.4(9) . . ? F4 P3 F1 86.7(9) . . ? F2 P3 F1 92.4(10) . . ? F3 P3 F1 91.2(12) . . ? C17 N1 P1 117.0(4) . . ? C17 N1 P2 120.7(4) . . ? P1 N1 P2 121.6(3) . . ? N3 N2 C9 109.9(6) . . ? N3 N2 P1 121.7(4) . . ? C9 N2 P1 125.2(6) . . ? C7 N3 N2 104.9(6) . . ? C7 N3 Pd1 132.9(6) . . ? N2 N3 Pd1 121.3(4) . . ? C3 C2 C1 152.1(17) . . ? C3 C2 Pd1 67.7(7) . . ? C1 C2 Pd1 128.1(9) . . ? C2 C3 C4 146.6(14) . . ? C2 C3 Pd1 79.9(8) . . ? C4 C3 Pd1 72.2(6) . . ? C3 C4 C5 146.8(14) . . ? C3 C4 Pd1 72.9(7) . . ? C5 C4 Pd1 129.0(9) . . ? C8 C7 N3 110.4(8) . . ? C8 C7 C6 129.7(8) . . ? N3 C7 C6 119.8(8) . . ? C9 C8 C7 108.6(7) . . ? C8 C9 N2 106.2(7) . . ? C8 C9 C10 132.6(7) . . ? N2 C9 C10 121.2(8) . . ? C16 C11 C12 117.9(7) . . ? C16 C11 P1 122.2(6) . . ? C12 C11 P1 118.8(5) . . ? C13 C12 C11 119.7(8) . . ? C12 C13 C14 120.8(8) . . ? C15 C14 C13 119.3(8) . . ? C14 C15 C16 121.0(8) . . ? C15 C16 C11 121.1(7) . . ? C18 C17 N1 112.9(6) . . ? C18 C17 C19 110.7(6) . . ? N1 C17 C19 112.1(5) . . ? C20 C19 C24 118.7(7) . . ? C20 C19 C17 121.7(6) . . ? C24 C19 C17 119.5(6) . . ? C19 C20 C21 119.9(8) . . ? C22 C21 C20 120.6(9) . . ? C21 C22 C23 121.3(9) . . ? C22 C23 C24 118.8(9) . . ? C19 C24 C23 120.6(8) . . ? C26 C25 C30 119.5(6) . . ? C26 C25 P2 124.1(5) . . ? C30 C25 P2 116.2(5) . . ? C25 C26 C27 120.3(7) . . ? C28 C27 C26 120.9(7) . . ? C27 C28 C29 120.0(7) . . ? C28 C29 C30 119.2(7) . . ? C25 C30 C29 120.3(7) . . ? C32 C31 C36 116.8(7) . . ? C32 C31 P2 124.6(5) . . ? C36 C31 P2 118.5(5) . . ? C33 C32 C31 121.4(7) . . ? C34 C33 C32 121.3(8) . . ? C33 C34 C35 118.5(8) . . ? C36 C35 C34 120.5(8) . . ? C35 C36 C31 121.3(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.610 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.069 # ====== END data_complex_8a _database_code_CSD 190879 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [eta-2-{N,N-(diphenylphosphino) (phenyl, 3,5-dimethylpyrazolylphosphino) isopropylamine}-kappa-P,N] palladium(II)hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point '200-202 0C dec.' _chemical_formula_moiety ; [Pd(eta-3-Ph2-C3H3){eta-2-Ph2PN(CHMe2)PPh(N2C3HMe2-3,5)}](PF6) ; _chemical_formula_sum 'C41 H42 F6 N3 P3 Pd' _chemical_formula_weight 890.09 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' '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.826(3) _cell_length_b 18.176(4) _cell_length_c 41.424(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.75(2) _cell_angle_gamma 90.00 _cell_volume 8150(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.634 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\alpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6 _diffrn_reflns_number 15726 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14315 _reflns_number_gt 9998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-32 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0499P)^2^+53.6081P] 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 14315 _refine_ls_number_parameters 967 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.220 _refine_ls_shift/su_mean 0.007 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 0.41491(5) 0.27635(3) -0.195070(13) 0.04055(16) Uani 1 1 d . . . Pd2 Pd 0.43532(5) 0.19211(3) 0.035620(13) 0.04188(16) Uani 1 1 d . . . P1 P 0.44574(16) 0.31115(10) -0.24844(4) 0.0375(4) Uani 1 1 d . . . P2 P 0.56202(19) 0.16235(11) -0.24763(5) 0.0466(5) Uani 1 1 d . . . P3 P 0.46062(18) 0.30213(11) 0.00880(4) 0.0428(4) Uani 1 1 d . . . P4 P 0.18685(19) 0.29072(12) 0.01050(5) 0.0512(5) Uani 1 1 d . . . P5 P 0.8901(3) 0.1502(2) 0.10539(7) 0.0890(9) Uani 1 1 d . . . P6 P 0.0013(3) 0.55830(18) 0.14294(9) 0.0876(9) Uani 1 1 d . . . F1 F 0.8199(13) 0.0963(7) 0.0846(3) 0.217(6) Uani 1 1 d . . . F2 F 0.9228(11) 0.1977(6) 0.0754(2) 0.184(5) Uani 1 1 d . . . F3 F 0.942(3) 0.2014(12) 0.1268(3) 0.428(18) Uani 1 1 d . . . F4 F 0.8450(13) 0.1068(5) 0.13451(18) 0.200(5) Uani 1 1 d . . . F5 F 0.9940(13) 0.1075(15) 0.1007(5) 0.405(15) Uani 1 1 d . . . F6 F 0.7816(19) 0.1941(10) 0.1060(5) 0.368(15) Uani 1 1 d . . . F7 F 0.0997(12) 0.5187(7) 0.1234(3) 0.217(5) Uani 1 1 d . . . F8 F -0.0902(14) 0.5651(7) 0.1168(3) 0.263(8) Uani 1 1 d . . . F9 F -0.0864(9) 0.6004(6) 0.1665(3) 0.179(4) Uani 1 1 d . . . F10 F 0.0873(9) 0.5529(7) 0.1740(2) 0.202(5) Uani 1 1 d . . . F11 F -0.0572(11) 0.4847(5) 0.1527(3) 0.200(5) Uani 1 1 d . . . F12 F 0.0579(11) 0.6321(5) 0.1340(2) 0.200(5) Uani 1 1 d . . . N1 N 0.5313(5) 0.2435(3) -0.26596(14) 0.0404(14) Uani 1 1 d . . . N2 N 0.4190(6) 0.1340(3) -0.23410(14) 0.0467(15) Uani 1 1 d . . . N3 N 0.3427(6) 0.1786(3) -0.21586(14) 0.0466(15) Uani 1 1 d . . . N4 N 0.3188(5) 0.3312(3) -0.00308(15) 0.0463(15) Uani 1 1 d . . . N5 N 0.2134(6) 0.2879(4) 0.05205(16) 0.0530(17) Uani 1 1 d . . . N6 N 0.3159(6) 0.2546(3) 0.06544(15) 0.0465(15) Uani 1 1 d . . . C1 C 0.3919(7) 0.2494(5) -0.14311(17) 0.0495(19) Uani 1 1 d . . . H1 H 0.4707 0.2351 -0.1331 0.059 Uiso 1 1 calc R . . C2 C 0.3858(7) 0.3251(4) -0.14773(17) 0.0486(19) Uani 1 1 d . . . H2 H 0.3102 0.3526 -0.1431 0.058 Uiso 1 1 calc R . . C3 C 0.4883(7) 0.3602(4) -0.16271(18) 0.0477(19) Uani 1 1 d . . . H3 H 0.5662 0.3438 -0.1528 0.057 Uiso 1 1 calc R . . C4 C 0.4920(7) 0.4399(5) -0.16944(18) 0.052(2) Uani 1 1 d . . . C5 C 0.3867(8) 0.4806(5) -0.1783(2) 0.062(2) Uani 1 1 d . . . H5 H 0.3105 0.4572 -0.1802 0.075 Uiso 1 1 calc R . . C6 C 0.3959(12) 0.5549(6) -0.1841(3) 0.087(3) Uani 1 1 d . . . H6 H 0.3259 0.5819 -0.1897 0.104 Uiso 1 1 calc R . . C7 C 0.5105(15) 0.5897(7) -0.1816(3) 0.099(4) Uani 1 1 d . . . H7 H 0.5171 0.6398 -0.1858 0.119 Uiso 1 1 calc R . . C8 C 0.6102(13) 0.5512(7) -0.1732(3) 0.098(4) Uani 1 1 d . . . H8 H 0.6859 0.5750 -0.1713 0.117 Uiso 1 1 calc R . . C9 C 0.6038(9) 0.4765(6) -0.1672(2) 0.077(3) Uani 1 1 d . . . H9 H 0.6750 0.4507 -0.1615 0.092 Uiso 1 1 calc R . . C10 C 0.2902(7) 0.2020(5) -0.13195(18) 0.053(2) Uani 1 1 d . . . C11 C 0.3024(9) 0.1259(5) -0.1331(2) 0.066(2) Uani 1 1 d . . . H11 H 0.3763 0.1056 -0.1400 0.079 Uiso 1 1 calc R . . C12 C 0.2088(11) 0.0808(6) -0.1244(2) 0.081(3) Uani 1 1 d . . . H12 H 0.2194 0.0301 -0.1257 0.097 Uiso 1 1 calc R . . C13 C 0.0981(10) 0.1087(7) -0.1137(2) 0.081(3) Uani 1 1 d . . . H13 H 0.0340 0.0775 -0.1079 0.098 Uiso 1 1 calc R . . C14 C 0.0850(9) 0.1841(7) -0.1119(2) 0.074(3) Uani 1 1 d . . . H14 H 0.0115 0.2039 -0.1044 0.089 Uiso 1 1 calc R . . C15 C 0.1794(8) 0.2309(6) -0.12093(19) 0.062(2) Uani 1 1 d . . . H15 H 0.1687 0.2816 -0.1197 0.074 Uiso 1 1 calc R . . C16 C 0.5152(7) 0.3961(4) -0.26231(19) 0.0468(18) Uani 1 1 d . . . C17 C 0.4786(8) 0.4336(4) -0.2895(2) 0.061(2) Uani 1 1 d . . . H17 H 0.4122 0.4157 -0.3016 0.073 Uiso 1 1 calc R . . C18 C 0.5364(11) 0.4962(6) -0.2993(3) 0.082(3) Uani 1 1 d . . . H18 H 0.5098 0.5205 -0.3179 0.099 Uiso 1 1 calc R . . C19 C 0.6350(14) 0.5233(6) -0.2813(4) 0.105(5) Uani 1 1 d . . . H19 H 0.6749 0.5660 -0.2878 0.126 Uiso 1 1 calc R . . C20 C 0.6734(10) 0.4880(6) -0.2542(3) 0.089(3) Uani 1 1 d . . . H20 H 0.7388 0.5071 -0.2421 0.107 Uiso 1 1 calc R . . C21 C 0.6158(8) 0.4232(5) -0.2443(2) 0.065(2) Uani 1 1 d . . . H21 H 0.6438 0.3985 -0.2259 0.078 Uiso 1 1 calc R . . C22 C 0.2931(6) 0.3105(4) -0.26758(18) 0.0439(17) Uani 1 1 d . . . C23 C 0.2654(8) 0.2894(6) -0.2988(2) 0.074(3) Uani 1 1 d . . . H23 H 0.3298 0.2753 -0.3121 0.089 Uiso 1 1 calc R . . C24 C 0.1482(10) 0.2881(7) -0.3110(3) 0.096(4) Uani 1 1 d . . . H24 H 0.1331 0.2732 -0.3322 0.115 Uiso 1 1 calc R . . C25 C 0.0545(10) 0.3087(6) -0.2920(3) 0.085(3) Uani 1 1 d . . . H25 H -0.0259 0.3082 -0.3003 0.102 Uiso 1 1 calc R . . C26 C 0.0756(9) 0.3305(6) -0.2608(3) 0.078(3) Uani 1 1 d . . . H26 H 0.0099 0.3446 -0.2479 0.094 Uiso 1 1 calc R . . C27 C 0.1934(7) 0.3315(5) -0.2486(2) 0.064(2) Uani 1 1 d . . . H27 H 0.2075 0.3464 -0.2274 0.076 Uiso 1 1 calc R . . C28 C 0.5720(7) 0.2499(5) -0.30069(18) 0.054(2) Uani 1 1 d . . . H28 H 0.5302 0.2930 -0.3100 0.064 Uiso 1 1 calc R . . C29 C 0.7091(8) 0.2642(6) -0.3022(3) 0.085(3) Uani 1 1 d . . . H29A H 0.7292 0.3072 -0.2898 0.127 Uiso 1 1 calc R . . H29B H 0.7323 0.2718 -0.3243 0.127 Uiso 1 1 calc R . . H29C H 0.7532 0.2226 -0.2936 0.127 Uiso 1 1 calc R . . C30 C 0.5326(10) 0.1830(5) -0.3208(2) 0.073(3) Uani 1 1 d . . . H30A H 0.4448 0.1766 -0.3195 0.110 Uiso 1 1 calc R . . H30B H 0.5736 0.1398 -0.3126 0.110 Uiso 1 1 calc R . . H30C H 0.5549 0.1905 -0.3429 0.110 Uiso 1 1 calc R . . C31 C 0.4108(11) 0.0179(6) -0.2663(3) 0.102(4) Uani 1 1 d . . . H31A H 0.4968 0.0289 -0.2690 0.153 Uiso 1 1 calc R . . H31B H 0.3703 0.0167 -0.2870 0.153 Uiso 1 1 calc R . . H31C H 0.4025 -0.0291 -0.2560 0.153 Uiso 1 1 calc R . . C32 C 0.3529(10) 0.0758(5) -0.2458(2) 0.070(3) Uani 1 1 d . . . C33 C 0.2346(9) 0.0838(5) -0.2356(2) 0.073(3) Uani 1 1 d . . . H33 H 0.1684 0.0527 -0.2401 0.087 Uiso 1 1 calc R . . C34 C 0.2315(8) 0.1484(5) -0.21674(19) 0.055(2) Uani 1 1 d . . . C35 C 0.1216(8) 0.1823(6) -0.2011(2) 0.067(2) Uani 1 1 d . . . H35A H 0.1465 0.2260 -0.1898 0.101 Uiso 1 1 calc R . . H35B H 0.0867 0.1479 -0.1861 0.101 Uiso 1 1 calc R . . H35C H 0.0610 0.1947 -0.2173 0.101 Uiso 1 1 calc R . . C36 C 0.6333(7) 0.1863(5) -0.2091(2) 0.055(2) Uani 1 1 d . . . C37 C 0.6195(9) 0.1401(6) -0.1828(2) 0.070(3) Uani 1 1 d . . . H37 H 0.5615 0.1024 -0.1835 0.084 Uiso 1 1 calc R . . C38 C 0.6919(12) 0.1500(8) -0.1553(3) 0.101(5) Uani 1 1 d . . . H38 H 0.6820 0.1190 -0.1377 0.122 Uiso 1 1 calc R . . C39 C 0.7769(13) 0.2046(11) -0.1541(3) 0.124(7) Uani 1 1 d . . . H39 H 0.8241 0.2111 -0.1354 0.149 Uiso 1 1 calc R . . C40 C 0.7947(10) 0.2506(9) -0.1800(4) 0.108(5) Uani 1 1 d . . . H40 H 0.8531 0.2880 -0.1788 0.130 Uiso 1 1 calc R . . C41 C 0.7247(8) 0.2405(6) -0.2078(3) 0.079(3) Uani 1 1 d . . . H41 H 0.7386 0.2700 -0.2257 0.094 Uiso 1 1 calc R . . C42 C 0.4278(7) 0.0816(4) 0.0590(2) 0.053(2) Uani 1 1 d . . . H42 H 0.3744 0.0482 0.0466 0.064 Uiso 1 1 calc R . . C43 C 0.5403(7) 0.0914(4) 0.0437(2) 0.0502(19) Uani 1 1 d . . . H43 H 0.6179 0.0921 0.0561 0.060 Uiso 1 1 calc R . . C44 C 0.5380(7) 0.1100(4) 0.01005(19) 0.0497(19) Uani 1 1 d . . . H44 H 0.4834 0.0772 -0.0023 0.060 Uiso 1 1 calc R . . C45 C 0.6534(8) 0.1254(5) -0.00729(18) 0.051(2) Uani 1 1 d . . . C46 C 0.7483(7) 0.1640(5) 0.0064(2) 0.063(2) Uani 1 1 d . . . H46 H 0.7401 0.1827 0.0272 0.076 Uiso 1 1 calc R . . C47 C 0.8581(9) 0.1761(7) -0.0104(3) 0.091(4) Uani 1 1 d . . . H47 H 0.9230 0.2022 -0.0010 0.110 Uiso 1 1 calc R . . C48 C 0.8677(13) 0.1487(9) -0.0411(3) 0.112(5) Uani 1 1 d . . . H48 H 0.9402 0.1566 -0.0523 0.135 Uiso 1 1 calc R . . C49 C 0.7750(13) 0.1106(7) -0.0554(3) 0.097(4) Uani 1 1 d . . . H49 H 0.7838 0.0922 -0.0762 0.117 Uiso 1 1 calc R . . C50 C 0.6673(11) 0.0993(5) -0.0387(2) 0.077(3) Uani 1 1 d . . . H50 H 0.6026 0.0738 -0.0486 0.092 Uiso 1 1 calc R . . C51 C 0.4113(7) 0.0704(4) 0.0939(2) 0.053(2) Uani 1 1 d . . . C52 C 0.2923(8) 0.0718(5) 0.1059(2) 0.068(3) Uani 1 1 d . . . H52 H 0.2255 0.0785 0.0919 0.082 Uiso 1 1 calc R . . C53 C 0.2725(10) 0.0634(6) 0.1385(3) 0.083(3) Uani 1 1 d . . . H53 H 0.1925 0.0646 0.1464 0.100 Uiso 1 1 calc R . . C54 C 0.3685(11) 0.0534(6) 0.1588(3) 0.079(3) Uani 1 1 d . . . H54 H 0.3541 0.0477 0.1808 0.095 Uiso 1 1 calc R . . C55 C 0.4891(10) 0.0514(5) 0.1478(2) 0.073(3) Uani 1 1 d . . . H55 H 0.5549 0.0447 0.1622 0.088 Uiso 1 1 calc R . . C56 C 0.5098(8) 0.0596(5) 0.1150(2) 0.062(2) Uani 1 1 d . . . H56 H 0.5900 0.0579 0.1072 0.075 Uiso 1 1 calc R . . C57 C 0.5607(7) 0.3163(4) -0.02539(18) 0.0507(19) Uani 1 1 d . . . C58 C 0.6454(8) 0.3736(5) -0.0264(2) 0.072(3) Uani 1 1 d . . . H58 H 0.6527 0.4062 -0.0091 0.086 Uiso 1 1 calc R . . C59 C 0.7194(10) 0.3817(6) -0.0534(3) 0.092(4) Uani 1 1 d . . . H59 H 0.7750 0.4206 -0.0542 0.111 Uiso 1 1 calc R . . C60 C 0.7124(10) 0.3345(6) -0.0786(3) 0.083(3) Uani 1 1 d . . . H60 H 0.7624 0.3408 -0.0964 0.100 Uiso 1 1 calc R . . C61 C 0.6303(9) 0.2770(6) -0.0774(2) 0.076(3) Uani 1 1 d . . . H61 H 0.6260 0.2437 -0.0944 0.091 Uiso 1 1 calc R . . C62 C 0.5537(8) 0.2681(5) -0.05116(19) 0.059(2) Uani 1 1 d . . . H62 H 0.4973 0.2295 -0.0509 0.071 Uiso 1 1 calc R . . C63 C 0.5205(7) 0.3654(4) 0.03935(17) 0.0466(18) Uani 1 1 d . . . C64 C 0.6323(8) 0.3471(6) 0.0538(2) 0.074(3) Uani 1 1 d . . . H64 H 0.6777 0.3075 0.0462 0.089 Uiso 1 1 calc R . . C65 C 0.6767(10) 0.3882(7) 0.0799(3) 0.090(3) Uani 1 1 d . . . H65 H 0.7513 0.3757 0.0898 0.108 Uiso 1 1 calc R . . C66 C 0.6103(10) 0.4469(6) 0.0909(2) 0.078(3) Uani 1 1 d . . . H66 H 0.6411 0.4752 0.1079 0.094 Uiso 1 1 calc R . . C67 C 0.4998(10) 0.4641(6) 0.0771(2) 0.076(3) Uani 1 1 d . . . H67 H 0.4529 0.5028 0.0851 0.092 Uiso 1 1 calc R . . C68 C 0.4582(9) 0.4235(5) 0.05117(19) 0.063(2) Uani 1 1 d . . . H68 H 0.3837 0.4367 0.0413 0.076 Uiso 1 1 calc R . . C69 C 0.3033(8) 0.3965(5) -0.0253(2) 0.061(2) Uani 1 1 d . . . H69 H 0.3830 0.4218 -0.0267 0.073 Uiso 1 1 calc R . . C70 C 0.2651(10) 0.3707(6) -0.0593(2) 0.083(3) Uani 1 1 d . . . H70A H 0.3247 0.3361 -0.0670 0.125 Uiso 1 1 calc R . . H70B H 0.2613 0.4123 -0.0736 0.125 Uiso 1 1 calc R . . H70C H 0.1854 0.3477 -0.0585 0.125 Uiso 1 1 calc R . . C71 C 0.2065(4) 0.4521(3) -0.01388(13) 0.084(3) Uani 1 1 d . . . H71A H 0.2290 0.4696 0.0073 0.126 Uiso 1 1 calc R . . H71B H 0.1271 0.4287 -0.0131 0.126 Uiso 1 1 calc R . . H71C H 0.2028 0.4928 -0.0286 0.126 Uiso 1 1 calc R . . C72 C 0.2013(4) 0.1929(3) 0.00180(13) 0.0516(19) Uani 1 1 d R . . C73 C 0.2451(4) 0.1691(3) -0.02802(13) 0.061(2) Uani 1 1 d R . . H73 H 0.2790 0.2030 -0.0422 0.074 Uiso 1 1 calc R . . C74 C 0.2384(10) 0.0956(6) -0.0366(3) 0.082(3) Uani 1 1 d . . . H74 H 0.2723 0.0797 -0.0559 0.099 Uiso 1 1 calc R . . C75 C 0.1812(11) 0.0459(6) -0.0164(3) 0.088(4) Uani 1 1 d . . . H75 H 0.1731 -0.0031 -0.0225 0.106 Uiso 1 1 calc R . . C76 C 0.1368(9) 0.0687(6) 0.0125(3) 0.080(3) Uani 1 1 d . . . H76 H 0.0998 0.0351 0.0263 0.096 Uiso 1 1 calc R . . C77 C 0.1465(8) 0.1416(5) 0.0215(2) 0.063(2) Uani 1 1 d . . . H77 H 0.1154 0.1564 0.0413 0.076 Uiso 1 1 calc R . . C78 C 0.0425(10) 0.3740(7) 0.0680(3) 0.100(4) Uani 1 1 d . . . H78A H 0.0166 0.3651 0.0461 0.150 Uiso 1 1 calc R . . H78B H 0.0575 0.4256 0.0711 0.150 Uiso 1 1 calc R . . H78C H -0.0209 0.3581 0.0824 0.150 Uiso 1 1 calc R . . C79 C 0.1595(8) 0.3317(5) 0.0751(2) 0.066(2) Uani 1 1 d . . . C80 C 0.2310(9) 0.3268(6) 0.1021(2) 0.072(3) Uani 1 1 d . . . H80 H 0.2180 0.3511 0.1215 0.087 Uiso 1 1 calc R . . C81 C 0.3263(8) 0.2793(5) 0.09551(19) 0.054(2) Uani 1 1 d . . . C82 C 0.4330(9) 0.2566(6) 0.1168(2) 0.070(3) Uani 1 1 d . . . H82A H 0.4850 0.2232 0.1052 0.105 Uiso 1 1 calc R . . H82B H 0.4025 0.2327 0.1357 0.105 Uiso 1 1 calc R . . H82C H 0.4798 0.2993 0.1229 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0377(3) 0.0461(3) 0.0379(3) -0.0061(2) 0.0020(2) -0.0011(3) Pd2 0.0394(3) 0.0466(3) 0.0397(3) 0.0032(3) 0.0020(2) -0.0008(3) P1 0.0351(9) 0.0385(10) 0.0390(9) -0.0041(8) 0.0038(7) -0.0014(8) P2 0.0473(11) 0.0450(11) 0.0475(11) -0.0052(9) 0.0026(9) 0.0060(9) P3 0.0437(11) 0.0455(11) 0.0392(10) 0.0021(8) 0.0034(8) -0.0029(9) P4 0.0409(11) 0.0539(13) 0.0587(13) 0.0014(10) -0.0043(9) -0.0005(9) P5 0.078(2) 0.129(3) 0.0596(16) -0.0063(17) 0.0039(14) -0.023(2) P6 0.0614(17) 0.085(2) 0.116(2) 0.0236(18) -0.0029(17) 0.0030(15) F1 0.284(15) 0.220(12) 0.144(9) 0.027(8) -0.084(9) -0.075(11) F2 0.235(11) 0.213(10) 0.106(6) 0.007(6) 0.058(7) -0.085(9) F3 0.75(4) 0.39(2) 0.133(10) -0.063(13) -0.041(17) -0.42(3) F4 0.376(16) 0.151(8) 0.073(5) 0.021(5) 0.020(7) -0.053(9) F5 0.143(11) 0.70(4) 0.38(2) 0.12(3) 0.075(14) 0.215(19) F6 0.36(2) 0.30(2) 0.45(3) 0.21(2) 0.28(2) 0.233(18) F7 0.225(12) 0.202(11) 0.225(12) -0.061(9) 0.070(10) 0.052(9) F8 0.306(16) 0.234(13) 0.245(13) 0.079(11) -0.212(12) -0.065(11) F9 0.147(8) 0.182(9) 0.208(10) 0.034(8) 0.076(7) 0.037(7) F10 0.126(7) 0.320(15) 0.157(9) 0.023(9) -0.046(6) 0.047(9) F11 0.240(12) 0.119(7) 0.240(12) 0.072(8) -0.014(10) -0.044(8) F12 0.277(13) 0.153(8) 0.173(9) -0.022(7) 0.114(9) -0.114(9) N1 0.038(3) 0.041(3) 0.043(3) -0.005(3) 0.010(3) 0.000(3) N2 0.056(4) 0.042(4) 0.042(3) -0.002(3) -0.002(3) -0.007(3) N3 0.057(4) 0.044(4) 0.039(3) -0.003(3) 0.005(3) -0.010(3) N4 0.042(3) 0.045(4) 0.052(4) 0.002(3) -0.006(3) -0.006(3) N5 0.048(4) 0.059(4) 0.053(4) 0.000(3) 0.006(3) 0.000(3) N6 0.044(4) 0.051(4) 0.044(3) 0.004(3) 0.005(3) -0.002(3) C1 0.053(5) 0.063(5) 0.032(4) -0.007(4) -0.005(3) 0.005(4) C2 0.050(5) 0.057(5) 0.039(4) -0.012(4) -0.006(3) 0.002(4) C3 0.034(4) 0.063(5) 0.046(4) -0.012(4) -0.012(3) 0.006(4) C4 0.053(5) 0.060(5) 0.042(4) -0.016(4) -0.004(4) -0.003(4) C5 0.056(5) 0.062(6) 0.069(6) -0.004(5) -0.006(4) 0.000(4) C6 0.102(9) 0.068(7) 0.090(8) -0.003(6) -0.006(7) 0.012(6) C7 0.151(13) 0.063(7) 0.083(8) -0.014(6) 0.007(8) -0.016(8) C8 0.097(9) 0.085(9) 0.112(10) -0.024(7) 0.001(8) -0.035(7) C9 0.064(6) 0.076(7) 0.090(7) -0.026(6) -0.004(5) -0.012(5) C10 0.052(5) 0.068(6) 0.041(4) 0.005(4) 0.000(4) 0.006(4) C11 0.064(6) 0.070(6) 0.063(6) 0.013(5) 0.009(4) 0.011(5) C12 0.103(9) 0.073(7) 0.067(6) 0.017(5) 0.006(6) -0.013(6) C13 0.072(7) 0.110(9) 0.062(6) 0.023(6) 0.009(5) -0.018(6) C14 0.057(6) 0.109(9) 0.056(5) 0.014(6) 0.011(4) 0.007(6) C15 0.063(6) 0.078(6) 0.045(5) 0.004(4) 0.004(4) 0.009(5) C16 0.041(4) 0.042(4) 0.058(5) -0.007(4) 0.018(4) -0.005(3) C17 0.060(5) 0.042(5) 0.081(6) 0.008(4) 0.021(5) 0.003(4) C18 0.102(9) 0.053(6) 0.092(8) 0.014(5) 0.043(7) 0.009(6) C19 0.128(11) 0.054(7) 0.136(12) -0.008(7) 0.086(10) -0.022(7) C20 0.077(7) 0.081(8) 0.109(9) -0.023(7) 0.025(7) -0.035(6) C21 0.058(5) 0.063(6) 0.075(6) -0.012(5) 0.019(5) -0.018(4) C22 0.039(4) 0.043(4) 0.050(4) 0.006(3) -0.002(3) 0.000(3) C23 0.050(5) 0.116(9) 0.057(5) -0.017(5) -0.003(4) -0.001(5) C24 0.067(7) 0.140(11) 0.081(7) -0.011(7) -0.016(6) -0.012(7) C25 0.055(6) 0.096(8) 0.104(9) 0.021(7) -0.020(6) -0.014(6) C26 0.049(6) 0.085(7) 0.102(8) 0.011(6) 0.010(5) 0.012(5) C27 0.044(5) 0.069(6) 0.077(6) 0.001(5) 0.009(4) 0.012(4) C28 0.057(5) 0.056(5) 0.048(5) -0.001(4) 0.020(4) 0.004(4) C29 0.062(6) 0.105(8) 0.088(7) -0.005(6) 0.036(5) -0.004(6) C30 0.105(8) 0.068(6) 0.047(5) -0.013(4) 0.010(5) 0.009(6) C31 0.113(9) 0.062(7) 0.131(10) -0.041(7) 0.026(8) -0.023(6) C32 0.096(8) 0.049(5) 0.066(6) -0.014(4) 0.010(5) -0.025(5) C33 0.076(7) 0.073(7) 0.070(6) -0.010(5) 0.004(5) -0.039(5) C34 0.054(5) 0.067(6) 0.045(4) 0.007(4) 0.001(4) -0.021(4) C35 0.050(5) 0.092(7) 0.061(5) 0.007(5) 0.000(4) -0.011(5) C36 0.047(5) 0.060(5) 0.058(5) -0.015(4) -0.003(4) 0.018(4) C37 0.067(6) 0.085(7) 0.057(5) -0.006(5) -0.003(4) 0.037(5) C38 0.084(8) 0.157(13) 0.063(7) -0.018(7) -0.019(6) 0.071(9) C39 0.073(8) 0.213(19) 0.085(9) -0.059(11) -0.040(8) 0.071(10) C40 0.057(7) 0.152(13) 0.114(10) -0.066(10) -0.020(7) 0.011(7) C41 0.052(5) 0.097(8) 0.087(7) -0.029(6) -0.013(5) 0.014(5) C42 0.044(5) 0.048(5) 0.067(5) 0.007(4) -0.003(4) -0.005(4) C43 0.038(4) 0.046(5) 0.067(5) 0.006(4) 0.002(4) 0.002(3) C44 0.053(5) 0.044(5) 0.052(5) -0.005(4) 0.004(4) 0.006(4) C45 0.055(5) 0.058(5) 0.041(4) 0.003(4) 0.001(4) 0.015(4) C46 0.044(5) 0.082(7) 0.062(5) 0.010(5) 0.006(4) 0.010(4) C47 0.043(5) 0.128(10) 0.103(9) 0.032(8) 0.009(5) 0.005(6) C48 0.095(10) 0.147(13) 0.097(10) 0.047(9) 0.057(8) 0.049(9) C49 0.118(11) 0.111(10) 0.064(7) 0.005(7) 0.031(7) 0.050(9) C50 0.113(8) 0.061(6) 0.057(6) 0.001(5) 0.024(6) 0.024(6) C51 0.039(4) 0.049(5) 0.071(5) 0.016(4) 0.003(4) -0.007(4) C52 0.044(5) 0.079(7) 0.081(7) 0.016(5) 0.004(4) -0.008(4) C53 0.071(7) 0.086(8) 0.094(8) 0.025(6) 0.027(6) -0.005(6) C54 0.098(8) 0.074(7) 0.067(6) 0.021(5) 0.020(6) 0.002(6) C55 0.079(7) 0.074(7) 0.066(6) 0.021(5) -0.001(5) 0.002(5) C56 0.048(5) 0.067(6) 0.073(6) 0.020(5) 0.006(4) -0.002(4) C57 0.058(5) 0.047(5) 0.047(4) 0.006(4) 0.009(4) -0.001(4) C58 0.068(6) 0.076(7) 0.072(6) -0.005(5) 0.028(5) -0.020(5) C59 0.092(8) 0.087(8) 0.098(8) 0.003(7) 0.046(7) -0.029(6) C60 0.089(8) 0.087(8) 0.074(7) 0.012(6) 0.033(6) 0.005(6) C61 0.085(7) 0.095(8) 0.049(5) -0.001(5) 0.014(5) 0.015(6) C62 0.061(5) 0.070(6) 0.047(5) -0.001(4) 0.003(4) 0.001(4) C63 0.044(4) 0.054(5) 0.042(4) 0.000(4) 0.001(3) -0.009(4) C64 0.056(6) 0.083(7) 0.082(7) -0.024(6) -0.016(5) 0.000(5) C65 0.071(7) 0.116(10) 0.083(7) -0.014(7) -0.022(6) -0.018(7) C66 0.087(8) 0.082(8) 0.065(6) -0.013(5) 0.000(6) -0.020(6) C67 0.078(7) 0.078(7) 0.074(6) -0.022(5) -0.001(5) 0.009(6) C68 0.079(6) 0.067(6) 0.044(5) -0.009(4) -0.005(4) 0.001(5) C69 0.062(5) 0.053(5) 0.068(6) 0.015(4) -0.008(4) -0.004(4) C70 0.101(8) 0.084(7) 0.064(6) 0.012(5) -0.026(6) 0.005(6) C71 0.087(7) 0.054(6) 0.110(9) 0.011(6) -0.014(6) 0.014(5) C72 0.038(4) 0.060(5) 0.056(5) 0.001(4) -0.018(4) -0.006(4) C73 0.051(5) 0.070(6) 0.062(5) -0.004(5) -0.017(4) -0.007(4) C74 0.087(8) 0.079(8) 0.080(7) -0.028(6) -0.022(6) 0.008(6) C75 0.083(8) 0.060(7) 0.121(10) -0.014(7) -0.048(7) 0.001(6) C76 0.057(6) 0.061(7) 0.120(10) 0.017(6) -0.033(6) -0.018(5) C77 0.058(5) 0.060(6) 0.071(6) 0.006(5) -0.006(4) -0.011(4) C78 0.074(7) 0.115(10) 0.111(9) -0.018(8) 0.018(6) 0.032(7) C79 0.060(6) 0.067(6) 0.069(6) -0.002(5) 0.027(5) 0.004(5) C80 0.082(7) 0.079(7) 0.056(6) -0.009(5) 0.026(5) -0.009(5) C81 0.059(5) 0.059(5) 0.045(4) -0.004(4) 0.012(4) -0.013(4) C82 0.077(6) 0.086(7) 0.047(5) -0.002(5) 0.001(4) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3 2.119(6) . ? Pd1 C3 2.173(7) . ? Pd1 C2 2.179(7) . ? Pd1 C1 2.224(7) . ? Pd1 P1 2.3277(19) . ? Pd2 N6 2.128(6) . ? Pd2 C44 2.148(7) . ? Pd2 C43 2.178(8) . ? Pd2 C42 2.232(8) . ? Pd2 P3 2.306(2) . ? P1 N1 1.707(6) . ? P1 C16 1.815(8) . ? P1 C22 1.824(7) . ? P2 N1 1.690(6) . ? P2 N2 1.732(7) . ? P2 C36 1.815(8) . ? P3 N4 1.691(6) . ? P3 C57 1.813(8) . ? P3 C63 1.823(8) . ? P4 N4 1.709(6) . ? P4 N5 1.742(7) . ? P4 C72 1.821(6) . ? P5 F5 1.382(14) . ? P5 F3 1.399(10) . ? P5 F6 1.420(12) . ? P5 F1 1.504(11) . ? P5 F4 1.527(8) . ? P5 F2 1.559(9) . ? P6 F8 1.463(9) . ? P6 F12 1.521(8) . ? P6 F7 1.527(10) . ? P6 F11 1.536(9) . ? P6 F9 1.568(9) . ? P6 F10 1.582(9) . ? N1 C28 1.515(9) . ? N2 C32 1.363(10) . ? N2 N3 1.388(8) . ? N3 C34 1.324(9) . ? N4 C69 1.510(10) . ? N5 N6 1.375(9) . ? N5 C79 1.378(10) . ? N6 C81 1.328(9) . ? C1 C2 1.391(11) . ? C1 C10 1.477(11) . ? C2 C3 1.428(11) . ? C3 C4 1.477(11) . ? C4 C9 1.382(12) . ? C4 C5 1.404(12) . ? C5 C6 1.377(13) . ? C6 C7 1.395(16) . ? C7 C8 1.329(17) . ? C8 C9 1.382(15) . ? C10 C11 1.389(12) . ? C10 C15 1.393(11) . ? C11 C12 1.357(13) . ? C12 C13 1.380(14) . ? C13 C14 1.381(15) . ? C14 C15 1.385(13) . ? C16 C17 1.369(12) . ? C16 C21 1.402(11) . ? C17 C18 1.364(12) . ? C18 C19 1.385(17) . ? C19 C20 1.353(17) . ? C20 C21 1.397(13) . ? C22 C23 1.377(11) . ? C22 C27 1.397(10) . ? C23 C24 1.361(13) . ? C24 C25 1.345(15) . ? C25 C26 1.371(15) . ? C26 C27 1.366(12) . ? C28 C29 1.509(12) . ? C28 C30 1.532(12) . ? C31 C32 1.493(13) . ? C32 C33 1.363(13) . ? C33 C34 1.410(12) . ? C34 C35 1.496(12) . ? C36 C37 1.387(12) . ? C36 C41 1.397(13) . ? C37 C38 1.384(14) . ? C38 C39 1.35(2) . ? C39 C40 1.38(2) . ? C40 C41 1.382(15) . ? C42 C43 1.391(10) . ? C42 C51 1.473(11) . ? C43 C44 1.435(11) . ? C44 C45 1.476(11) . ? C45 C46 1.362(12) . ? C45 C50 1.397(11) . ? C46 C47 1.404(12) . ? C47 C48 1.368(17) . ? C48 C49 1.351(18) . ? C49 C50 1.378(15) . ? C51 C56 1.384(11) . ? C51 C52 1.387(11) . ? C52 C53 1.380(13) . ? C53 C54 1.340(14) . ? C54 C55 1.389(13) . ? C55 C56 1.387(12) . ? C57 C62 1.382(11) . ? C57 C58 1.389(11) . ? C58 C59 1.394(12) . ? C59 C60 1.352(14) . ? C60 C61 1.373(14) . ? C61 C62 1.385(12) . ? C63 C68 1.349(11) . ? C63 C64 1.384(11) . ? C64 C65 1.393(13) . ? C65 C66 1.369(15) . ? C66 C67 1.355(14) . ? C67 C68 1.376(12) . ? C69 C70 1.534(12) . ? C69 C71 1.535(10) . ? C72 C77 1.380(10) . ? C72 C73 1.3974 . ? C73 C74 1.384(11) . ? C74 C75 1.386(15) . ? C75 C76 1.361(15) . ? C76 C77 1.379(13) . ? C78 C79 1.506(13) . ? C79 C80 1.355(13) . ? C80 C81 1.376(12) . ? C81 C82 1.501(12) . ? 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 N3 Pd1 C3 165.6(3) . . ? N3 Pd1 C2 130.6(3) . . ? C3 Pd1 C2 38.3(3) . . ? N3 Pd1 C1 99.4(3) . . ? C3 Pd1 C1 66.6(3) . . ? C2 Pd1 C1 36.8(3) . . ? N3 Pd1 P1 84.17(16) . . ? C3 Pd1 P1 109.8(2) . . ? C2 Pd1 P1 140.2(2) . . ? C1 Pd1 P1 176.4(2) . . ? N6 Pd2 C44 168.2(3) . . ? N6 Pd2 C43 132.7(3) . . ? C44 Pd2 C43 38.7(3) . . ? N6 Pd2 C42 101.7(3) . . ? C44 Pd2 C42 67.1(3) . . ? C43 Pd2 C42 36.7(3) . . ? N6 Pd2 P3 83.92(17) . . ? C44 Pd2 P3 107.4(2) . . ? C43 Pd2 P3 137.6(2) . . ? C42 Pd2 P3 174.2(2) . . ? N1 P1 C16 104.4(3) . . ? N1 P1 C22 107.7(3) . . ? C16 P1 C22 104.2(4) . . ? N1 P1 Pd1 107.1(2) . . ? C16 P1 Pd1 126.7(3) . . ? C22 P1 Pd1 105.7(2) . . ? N1 P2 N2 103.5(3) . . ? N1 P2 C36 105.3(4) . . ? N2 P2 C36 99.1(4) . . ? N4 P3 C57 106.1(3) . . ? N4 P3 C63 108.5(3) . . ? C57 P3 C63 104.0(4) . . ? N4 P3 Pd2 107.4(2) . . ? C57 P3 Pd2 125.1(3) . . ? C63 P3 Pd2 104.8(3) . . ? N4 P4 N5 102.1(3) . . ? N4 P4 C72 106.3(3) . . ? N5 P4 C72 98.8(3) . . ? F5 P5 F3 98.1(16) . . ? F5 P5 F6 173.1(12) . . ? F3 P5 F6 86.6(15) . . ? F5 P5 F1 87.7(13) . . ? F3 P5 F1 173.0(14) . . ? F6 P5 F1 88.0(13) . . ? F5 P5 F4 95.1(10) . . ? F3 P5 F4 88.4(7) . . ? F6 P5 F4 90.1(7) . . ? F1 P5 F4 87.2(6) . . ? F5 P5 F2 90.3(9) . . ? F3 P5 F2 92.6(7) . . ? F6 P5 F2 84.3(7) . . ? F1 P5 F2 91.3(6) . . ? F4 P5 F2 174.3(8) . . ? F8 P6 F12 91.0(7) . . ? F8 P6 F7 96.8(9) . . ? F12 P6 F7 90.1(7) . . ? F8 P6 F11 89.4(7) . . ? F12 P6 F11 178.6(7) . . ? F7 P6 F11 91.2(7) . . ? F8 P6 F9 90.5(8) . . ? F12 P6 F9 88.3(6) . . ? F7 P6 F9 172.6(7) . . ? F11 P6 F9 90.4(6) . . ? F8 P6 F10 173.2(9) . . ? F12 P6 F10 91.0(7) . . ? F7 P6 F10 89.7(7) . . ? F11 P6 F10 88.4(7) . . ? F9 P6 F10 83.1(6) . . ? C28 N1 P2 115.9(5) . . ? C28 N1 P1 121.0(5) . . ? P2 N1 P1 122.8(3) . . ? C32 N2 N3 109.6(7) . . ? C32 N2 P2 125.6(6) . . ? N3 N2 P2 122.8(5) . . ? C34 N3 N2 106.8(6) . . ? C34 N3 Pd1 133.6(6) . . ? N2 N3 Pd1 119.5(4) . . ? C69 N4 P3 121.1(5) . . ? C69 N4 P4 116.9(5) . . ? P3 N4 P4 121.9(4) . . ? N6 N5 C79 108.8(7) . . ? N6 N5 P4 122.2(5) . . ? C79 N5 P4 127.0(6) . . ? C81 N6 N5 106.7(6) . . ? C81 N6 Pd2 132.9(6) . . ? N5 N6 Pd2 119.6(5) . . ? C2 C1 C10 125.9(7) . . ? C2 C1 Pd1 69.8(4) . . ? C10 C1 Pd1 121.7(5) . . ? C1 C2 C3 117.8(7) . . ? C1 C2 Pd1 73.4(4) . . ? C3 C2 Pd1 70.6(4) . . ? C2 C3 C4 122.9(7) . . ? C2 C3 Pd1 71.1(4) . . ? C4 C3 Pd1 125.6(5) . . ? C9 C4 C5 118.2(9) . . ? C9 C4 C3 119.0(8) . . ? C5 C4 C3 122.8(7) . . ? C6 C5 C4 120.1(9) . . ? C5 C6 C7 119.9(11) . . ? C8 C7 C6 120.0(12) . . ? C7 C8 C9 121.5(11) . . ? C4 C9 C8 120.4(11) . . ? C11 C10 C15 118.1(8) . . ? C11 C10 C1 119.9(8) . . ? C15 C10 C1 122.0(8) . . ? C12 C11 C10 121.4(9) . . ? C11 C12 C13 121.2(10) . . ? C12 C13 C14 118.2(10) . . ? C13 C14 C15 121.3(9) . . ? C14 C15 C10 119.9(9) . . ? C17 C16 C21 118.6(8) . . ? C17 C16 P1 124.5(6) . . ? C21 C16 P1 116.9(7) . . ? C18 C17 C16 122.1(10) . . ? C17 C18 C19 119.3(11) . . ? C20 C19 C18 120.2(10) . . ? C19 C20 C21 120.7(11) . . ? C20 C21 C16 119.0(10) . . ? C23 C22 C27 116.4(8) . . ? C23 C22 P1 126.5(6) . . ? C27 C22 P1 117.1(6) . . ? C24 C23 C22 123.0(9) . . ? C25 C24 C23 119.0(11) . . ? C24 C25 C26 121.0(10) . . ? C27 C26 C25 119.8(10) . . ? C26 C27 C22 120.8(9) . . ? C29 C28 N1 110.6(7) . . ? C29 C28 C30 112.3(7) . . ? N1 C28 C30 111.9(7) . . ? N2 C32 C33 107.2(8) . . ? N2 C32 C31 121.8(9) . . ? C33 C32 C31 131.0(9) . . ? C32 C33 C34 106.9(8) . . ? N3 C34 C33 109.5(8) . . ? N3 C34 C35 123.1(8) . . ? C33 C34 C35 127.4(8) . . ? C37 C36 C41 118.6(9) . . ? C37 C36 P2 119.8(7) . . ? C41 C36 P2 119.8(7) . . ? C38 C37 C36 120.2(11) . . ? C39 C38 C37 120.2(13) . . ? C38 C39 C40 121.2(12) . . ? C39 C40 C41 119.2(13) . . ? C40 C41 C36 120.5(12) . . ? C43 C42 C51 125.7(7) . . ? C43 C42 Pd2 69.5(4) . . ? C51 C42 Pd2 123.8(6) . . ? C42 C43 C44 117.9(7) . . ? C42 C43 Pd2 73.7(5) . . ? C44 C43 Pd2 69.5(4) . . ? C43 C44 C45 120.9(7) . . ? C43 C44 Pd2 71.8(4) . . ? C45 C44 Pd2 123.7(6) . . ? C46 C45 C50 118.3(9) . . ? C46 C45 C44 122.2(7) . . ? C50 C45 C44 119.5(8) . . ? C45 C46 C47 120.8(9) . . ? C48 C47 C46 118.6(11) . . ? C49 C48 C47 122.0(11) . . ? C48 C49 C50 119.0(11) . . ? C49 C50 C45 121.2(11) . . ? C56 C51 C52 119.2(8) . . ? C56 C51 C42 122.5(7) . . ? C52 C51 C42 118.3(8) . . ? C53 C52 C51 120.4(9) . . ? C54 C53 C52 120.0(10) . . ? C53 C54 C55 121.5(10) . . ? C56 C55 C54 118.9(9) . . ? C51 C56 C55 120.0(8) . . ? C62 C57 C58 118.9(8) . . ? C62 C57 P3 119.1(6) . . ? C58 C57 P3 122.0(6) . . ? C57 C58 C59 119.3(9) . . ? C60 C59 C58 121.8(10) . . ? C59 C60 C61 119.0(9) . . ? C60 C61 C62 120.7(10) . . ? C57 C62 C61 120.3(9) . . ? C68 C63 C64 118.0(8) . . ? C68 C63 P3 124.8(6) . . ? C64 C63 P3 116.8(7) . . ? C63 C64 C65 119.9(10) . . ? C66 C65 C64 119.9(10) . . ? C67 C66 C65 120.2(10) . . ? C66 C67 C68 119.0(10) . . ? C63 C68 C67 122.9(9) . . ? N4 C69 C70 110.2(7) . . ? N4 C69 C71 113.6(6) . . ? C70 C69 C71 107.9(7) . . ? C77 C72 C73 117.9(5) . . ? C77 C72 P4 120.3(6) . . ? C73 C72 P4 120.54(19) . . ? C74 C73 C72 120.6(6) . . ? C73 C74 C75 119.7(10) . . ? C76 C75 C74 119.9(10) . . ? C75 C76 C77 120.3(10) . . ? C76 C77 C72 121.4(9) . . ? C80 C79 N5 107.0(8) . . ? C80 C79 C78 131.5(9) . . ? N5 C79 C78 121.5(9) . . ? C79 C80 C81 107.3(8) . . ? N6 C81 C80 110.2(8) . . ? N6 C81 C82 120.8(8) . . ? C80 C81 C82 129.0(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.123 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.109 # ====== END data_complex_12a _database_code_CSD 190880 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta-3-dimethylallyl)[eta-2-{N,N-(diphenylthiophosphinyl) (phenyl, 3,5-dimethylpyrazolylphosphino)isopropyl amine} -kappa-P,S]palladium(II)hexafluorophosphate ; _chemical_name_common ? _chemical_melting_point '155- 159 0C dec.' _chemical_formula_moiety ; [Pd(eta-3-Me2-C3H3){eta-2-Ph2P(S)N(CHMe2)PPh(N2C3HMe2-3,5)}](PF6) ; _chemical_formula_sum 'C31 H38 F6 N3 P3 Pd S' _chemical_formula_weight 798.01 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' '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 'Monoclinic' _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.836(5) _cell_length_b 10.758(2) _cell_length_c 33.860(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.03(3) _cell_angle_gamma 90.00 _cell_volume 3556(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.0 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.773 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\alpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profile omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6 _diffrn_reflns_number 8208 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.98 _reflns_number_total 7756 _reflns_number_gt 4971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4(Harms and Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-32 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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_number_reflns 7756 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.42906(4) 0.17433(3) 0.123627(10) 0.05253(14) Uani 1 1 d . . . S1 S 0.42722(15) 0.07358(11) 0.06237(3) 0.0650(4) Uani 1 1 d . . . P1 P 0.48186(11) -0.00429(9) 0.15730(3) 0.0424(3) Uani 1 1 d . . . P2 P 0.50707(12) -0.09323(10) 0.07743(3) 0.0441(3) Uani 1 1 d . . . P3 P 0.92851(16) 0.37639(16) 0.11751(5) 0.0758(4) Uani 1 1 d . . . N1 N 0.5507(3) -0.1068(3) 0.12673(9) 0.0401(7) Uani 1 1 d . . . N2 N 0.3572(4) -0.0870(3) 0.17730(10) 0.0486(8) Uani 1 1 d . . . N3 N 0.3900(4) -0.2011(3) 0.19468(12) 0.0557(10) Uani 1 1 d . . . C1 C 0.4531(11) 0.3042(7) 0.2098(2) 0.119(3) Uani 1 1 d . . . H1A H 0.3902 0.2483 0.2202 0.178 Uiso 1 1 calc R . . H1B H 0.4471 0.3845 0.2218 0.178 Uiso 1 1 calc R . . H1C H 0.5447 0.2727 0.2157 0.178 Uiso 1 1 calc R . . C2 C 0.4209(13) 0.3140(5) 0.1697(2) 0.142(4) Uani 1 1 d . . . H2 H 0.3211 0.3192 0.1688 0.171 Uiso 1 1 calc R . . C3 C 0.4321(9) 0.3670(5) 0.13772(19) 0.095(2) Uani 1 1 d . . . H3 H 0.5316 0.3792 0.1414 0.114 Uiso 1 1 calc R . . C4 C 0.4139(10) 0.3638(5) 0.0997(2) 0.109(3) Uani 1 1 d . . . H4 H 0.3138 0.3705 0.0962 0.131 Uiso 1 1 calc R . . C5 C 0.4357(11) 0.4051(6) 0.0635(2) 0.147(4) Uani 1 1 d . . . H5A H 0.3681 0.3705 0.0437 0.220 Uiso 1 1 calc R . . H5B H 0.5254 0.3802 0.0582 0.220 Uiso 1 1 calc R . . H5C H 0.4294 0.4941 0.0629 0.220 Uiso 1 1 calc R . . C6 C 0.6150(5) 0.0188(4) 0.19854(12) 0.0467(10) Uani 1 1 d . . . C7 C 0.7253(5) 0.0913(5) 0.18990(14) 0.0594(12) Uani 1 1 d . . . H7 H 0.7314 0.1161 0.1639 0.071 Uiso 1 1 calc R . . C8 C 0.8261(6) 0.1265(6) 0.22026(18) 0.0754(15) Uani 1 1 d . . . H8 H 0.9007 0.1734 0.2145 0.090 Uiso 1 1 calc R . . C9 C 0.8151(6) 0.0922(6) 0.25801(16) 0.0789(17) Uani 1 1 d . . . H9 H 0.8825 0.1163 0.2783 0.095 Uiso 1 1 calc R . . C10 C 0.7064(6) 0.0222(6) 0.26714(16) 0.0816(17) Uani 1 1 d . . . H10 H 0.7003 0.0003 0.2934 0.098 Uiso 1 1 calc R . . C11 C 0.6060(5) -0.0156(5) 0.23746(13) 0.0606(12) Uani 1 1 d . . . H11 H 0.5330 -0.0638 0.2436 0.073 Uiso 1 1 calc R . . C12 C 0.2173(5) -0.0704(5) 0.17225(15) 0.0634(13) Uani 1 1 d . . . C13 C 0.1467(6) 0.0411(7) 0.1531(2) 0.100(2) Uani 1 1 d . . . H13A H 0.2138 0.0994 0.1462 0.150 Uiso 1 1 calc R . . H13B H 0.0921 0.0795 0.1714 0.150 Uiso 1 1 calc R . . H13C H 0.0889 0.0163 0.1296 0.150 Uiso 1 1 calc R . . C14 C 0.1654(5) -0.1751(5) 0.18676(19) 0.0746(16) Uani 1 1 d . . . H14 H 0.0730 -0.1920 0.1874 0.090 Uiso 1 1 calc R . . C15 C 0.2726(5) -0.2526(5) 0.20035(16) 0.0625(13) Uani 1 1 d . . . C16 C 0.2669(7) -0.3794(6) 0.2182(2) 0.098(2) Uani 1 1 d . . . H16A H 0.3583 -0.4104 0.2250 0.148 Uiso 1 1 calc R . . H16B H 0.2170 -0.4343 0.1993 0.148 Uiso 1 1 calc R . . H16C H 0.2217 -0.3750 0.2417 0.148 Uiso 1 1 calc R . . C17 C 0.6426(4) -0.2111(4) 0.14549(13) 0.0472(10) Uani 1 1 d . . . H17 H 0.6328 -0.2093 0.1739 0.057 Uiso 1 1 calc R . . C18 C 0.7930(5) -0.1889(5) 0.14288(17) 0.0683(14) Uani 1 1 d . . . H18A H 0.8174 -0.1067 0.1523 0.102 Uiso 1 1 calc R . . H18B H 0.8105 -0.1969 0.1157 0.102 Uiso 1 1 calc R . . H18C H 0.8466 -0.2489 0.1590 0.102 Uiso 1 1 calc R . . C19 C 0.5965(5) -0.3386(4) 0.13133(15) 0.0595(12) Uani 1 1 d . . . H19A H 0.5009 -0.3484 0.1337 0.089 Uiso 1 1 calc R . . H19B H 0.6481 -0.4003 0.1472 0.089 Uiso 1 1 calc R . . H19C H 0.6112 -0.3485 0.1040 0.089 Uiso 1 1 calc R . . C20 C 0.3808(5) -0.2082(4) 0.05993(13) 0.0509(11) Uani 1 1 d . . . C21 C 0.2942(5) -0.2580(5) 0.08500(16) 0.0615(12) Uani 1 1 d . . . H21 H 0.3072 -0.2383 0.1119 0.074 Uiso 1 1 calc R . . C22 C 0.1897(6) -0.3359(5) 0.0708(2) 0.0839(18) Uani 1 1 d . . . H22 H 0.1321 -0.3689 0.0879 0.101 Uiso 1 1 calc R . . C23 C 0.1703(7) -0.3655(7) 0.0305(3) 0.096(2) Uani 1 1 d . . . H23 H 0.1016 -0.4210 0.0209 0.115 Uiso 1 1 calc R . . C24 C 0.2511(7) -0.3137(6) 0.0049(2) 0.093(2) Uani 1 1 d . . . H24 H 0.2344 -0.3309 -0.0222 0.112 Uiso 1 1 calc R . . C25 C 0.3585(6) -0.2353(5) 0.01920(16) 0.0721(15) Uani 1 1 d . . . H25 H 0.4149 -0.2012 0.0019 0.087 Uiso 1 1 calc R . . C26 C 0.6601(5) -0.1154(5) 0.05432(14) 0.0587(12) Uani 1 1 d . . . C27 C 0.7502(6) -0.0139(6) 0.05663(18) 0.0808(17) Uani 1 1 d . . . H27 H 0.7247 0.0611 0.0673 0.097 Uiso 1 1 calc R . . C28 C 0.8764(8) -0.0250(9) 0.0432(3) 0.121(3) Uani 1 1 d . . . H28 H 0.9384 0.0407 0.0456 0.145 Uiso 1 1 calc R . . C29 C 0.9083(9) -0.1350(11) 0.0261(3) 0.131(4) Uani 1 1 d . . . H29 H 0.9926 -0.1423 0.0165 0.157 Uiso 1 1 calc R . . C30 C 0.8195(9) -0.2360(8) 0.0224(2) 0.111(3) Uani 1 1 d . . . H30 H 0.8434 -0.3092 0.0104 0.133 Uiso 1 1 calc R . . C31 C 0.6940(6) -0.2254(6) 0.03721(15) 0.0746(15) Uani 1 1 d . . . H31 H 0.6335 -0.2921 0.0355 0.090 Uiso 1 1 calc R . . F1 F 0.8126(6) 0.3885(7) 0.1438(2) 0.188(3) Uani 1 1 d . . . F2 F 0.8627(10) 0.2578(6) 0.1004(2) 0.225(4) Uani 1 1 d . . . F3 F 0.9908(10) 0.4970(7) 0.1350(2) 0.239(4) Uani 1 1 d . . . F4 F 0.9976(9) 0.3045(8) 0.1523(3) 0.252(4) Uani 1 1 d . . . F5 F 0.8527(10) 0.4506(7) 0.08386(18) 0.239(4) Uani 1 1 d . . . F6 F 1.0338(10) 0.3591(11) 0.0912(4) 0.317(7) 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 0.0681(3) 0.03352(18) 0.0551(2) 0.00247(14) 0.00411(16) 0.00459(16) S1 0.0974(10) 0.0452(6) 0.0496(6) 0.0084(5) -0.0019(6) 0.0188(6) P1 0.0481(6) 0.0354(5) 0.0426(5) 0.0013(4) 0.0009(4) -0.0008(4) P2 0.0529(7) 0.0379(5) 0.0405(5) 0.0027(4) 0.0012(5) 0.0039(5) P3 0.0654(9) 0.0706(9) 0.0921(11) 0.0022(8) 0.0126(8) 0.0019(8) N1 0.0458(19) 0.0336(16) 0.0395(17) 0.0051(13) -0.0010(14) 0.0011(14) N2 0.045(2) 0.0445(19) 0.056(2) 0.0034(16) 0.0025(16) 0.0014(16) N3 0.051(2) 0.048(2) 0.067(2) 0.0130(18) 0.0058(19) -0.0007(17) C1 0.205(9) 0.079(4) 0.074(4) -0.013(3) 0.022(5) 0.017(5) C2 0.300(13) 0.040(3) 0.089(5) -0.010(3) 0.037(7) 0.027(5) C3 0.175(7) 0.036(3) 0.075(4) -0.003(3) 0.024(4) 0.005(3) C4 0.211(9) 0.036(3) 0.082(4) 0.008(3) 0.030(5) 0.016(4) C5 0.301(13) 0.047(3) 0.095(5) 0.016(3) 0.034(7) 0.007(6) C6 0.053(3) 0.042(2) 0.043(2) -0.0042(17) -0.0020(18) -0.0028(19) C7 0.066(3) 0.059(3) 0.051(2) -0.004(2) -0.002(2) -0.010(2) C8 0.058(3) 0.080(4) 0.086(4) -0.021(3) 0.001(3) -0.011(3) C9 0.076(4) 0.093(4) 0.062(3) -0.023(3) -0.016(3) -0.010(3) C10 0.092(4) 0.102(5) 0.047(3) -0.008(3) -0.008(3) -0.015(4) C11 0.066(3) 0.066(3) 0.048(2) -0.001(2) 0.000(2) -0.009(2) C12 0.046(3) 0.073(3) 0.071(3) 0.007(3) 0.006(2) 0.005(2) C13 0.057(4) 0.098(5) 0.145(6) 0.040(5) 0.010(4) 0.017(3) C14 0.039(3) 0.086(4) 0.099(4) 0.014(3) 0.011(3) -0.008(3) C15 0.052(3) 0.057(3) 0.079(3) 0.006(2) 0.011(2) -0.005(2) C16 0.095(5) 0.067(4) 0.138(6) 0.030(4) 0.033(4) -0.011(3) C17 0.049(3) 0.041(2) 0.048(2) 0.0046(18) -0.0051(19) 0.0075(18) C18 0.048(3) 0.071(3) 0.082(4) 0.006(3) -0.006(3) 0.008(2) C19 0.074(3) 0.040(2) 0.061(3) 0.004(2) -0.004(2) 0.012(2) C20 0.053(3) 0.048(2) 0.048(2) -0.0046(19) -0.006(2) 0.006(2) C21 0.053(3) 0.060(3) 0.070(3) -0.010(2) 0.000(2) -0.003(2) C22 0.059(3) 0.077(4) 0.113(5) -0.015(4) 0.005(3) -0.014(3) C23 0.069(4) 0.087(5) 0.122(6) -0.028(4) -0.027(4) -0.006(4) C24 0.100(5) 0.090(5) 0.079(4) -0.030(4) -0.034(4) 0.013(4) C25 0.088(4) 0.066(3) 0.057(3) -0.007(2) -0.013(3) 0.010(3) C26 0.064(3) 0.066(3) 0.048(2) 0.014(2) 0.015(2) 0.011(2) C27 0.082(4) 0.077(4) 0.087(4) 0.030(3) 0.026(3) 0.001(3) C28 0.088(5) 0.119(7) 0.161(8) 0.067(6) 0.044(5) 0.007(5) C29 0.104(6) 0.155(8) 0.148(8) 0.068(7) 0.077(6) 0.038(6) C30 0.120(6) 0.114(6) 0.107(5) 0.032(5) 0.052(5) 0.050(5) C31 0.080(4) 0.087(4) 0.059(3) 0.011(3) 0.019(3) 0.025(3) F1 0.139(5) 0.248(7) 0.186(6) -0.047(6) 0.059(4) 0.025(5) F2 0.335(10) 0.135(5) 0.213(7) -0.059(5) 0.072(7) -0.112(6) F3 0.362(11) 0.173(6) 0.161(5) 0.005(5) -0.048(6) -0.151(7) F4 0.251(9) 0.228(8) 0.262(10) 0.098(7) -0.034(7) 0.096(7) F5 0.381(12) 0.180(6) 0.126(5) 0.014(4) -0.092(6) 0.036(7) F6 0.240(9) 0.326(13) 0.438(16) -0.064(11) 0.255(11) -0.026(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C3 2.126(5) . ? Pd1 C2 2.173(6) . ? Pd1 C4 2.192(5) . ? Pd1 P1 2.2622(11) . ? Pd1 S1 2.3383(14) . ? S1 P2 1.9997(16) . ? P1 N1 1.707(3) . ? P1 N2 1.720(4) . ? P1 C6 1.811(4) . ? P2 N1 1.678(3) . ? P2 C26 1.796(5) . ? P2 C20 1.801(5) . ? P3 F6 1.459(7) . ? P3 F4 1.501(7) . ? P3 F5 1.511(6) . ? P3 F2 1.514(6) . ? P3 F3 1.524(6) . ? P3 F1 1.536(5) . ? N1 C17 1.531(5) . ? N2 C12 1.377(6) . ? N2 N3 1.383(5) . ? N3 C15 1.315(6) . ? C1 C2 1.361(10) . ? C2 C3 1.240(9) . ? C3 C4 1.279(9) . ? C4 C5 1.344(9) . ? C6 C11 1.382(6) . ? C6 C7 1.396(6) . ? C7 C8 1.391(7) . ? C8 C9 1.347(8) . ? C9 C10 1.373(8) . ? C10 C11 1.381(7) . ? C12 C14 1.354(7) . ? C12 C13 1.493(8) . ? C14 C15 1.378(7) . ? C15 C16 1.496(8) . ? C17 C19 1.504(6) . ? C17 C18 1.511(7) . ? C20 C21 1.382(7) . ? C20 C25 1.400(7) . ? C21 C22 1.367(7) . ? C22 C23 1.391(10) . ? C23 C24 1.363(10) . ? C24 C25 1.392(8) . ? C26 C31 1.376(8) . ? C26 C27 1.402(8) . ? C27 C28 1.379(9) . ? C28 C29 1.371(13) . ? C29 C30 1.391(13) . ? C30 C31 1.392(9) . ? 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 C3 Pd1 C2 33.5(2) . . ? C3 Pd1 C4 34.4(2) . . ? C2 Pd1 C4 67.4(3) . . ? C3 Pd1 P1 135.96(19) . . ? C2 Pd1 P1 104.6(2) . . ? C4 Pd1 P1 167.8(2) . . ? C3 Pd1 S1 130.49(18) . . ? C2 Pd1 S1 163.7(2) . . ? C4 Pd1 S1 96.34(18) . . ? P1 Pd1 S1 91.70(4) . . ? P2 S1 Pd1 103.28(6) . . ? N1 P1 N2 105.04(17) . . ? N1 P1 C6 104.66(19) . . ? N2 P1 C6 104.51(19) . . ? N1 P1 Pd1 109.05(11) . . ? N2 P1 Pd1 120.47(13) . . ? C6 P1 Pd1 111.83(14) . . ? N1 P2 C26 107.2(2) . . ? N1 P2 C20 110.47(19) . . ? C26 P2 C20 110.3(2) . . ? N1 P2 S1 112.08(13) . . ? C26 P2 S1 109.39(17) . . ? C20 P2 S1 107.38(16) . . ? F6 P3 F4 97.3(7) . . ? F6 P3 F5 85.9(7) . . ? F4 P3 F5 176.8(6) . . ? F6 P3 F2 87.8(6) . . ? F4 P3 F2 89.8(6) . . ? F5 P3 F2 90.5(5) . . ? F6 P3 F3 93.7(6) . . ? F4 P3 F3 90.7(5) . . ? F5 P3 F3 88.9(4) . . ? F2 P3 F3 178.3(5) . . ? F6 P3 F1 176.6(6) . . ? F4 P3 F1 83.4(5) . . ? F5 P3 F1 93.4(5) . . ? F2 P3 F1 88.8(4) . . ? F3 P3 F1 89.6(5) . . ? C17 N1 P2 122.9(3) . . ? C17 N1 P1 118.7(3) . . ? P2 N1 P1 118.36(19) . . ? C12 N2 N3 110.2(4) . . ? C12 N2 P1 129.3(3) . . ? N3 N2 P1 119.1(3) . . ? C15 N3 N2 105.8(4) . . ? C3 C2 C1 150.7(10) . . ? C3 C2 Pd1 71.2(4) . . ? C1 C2 Pd1 129.6(5) . . ? C2 C3 C4 148.2(7) . . ? C2 C3 Pd1 75.3(4) . . ? C4 C3 Pd1 75.6(3) . . ? C3 C4 C5 152.9(9) . . ? C3 C4 Pd1 70.0(3) . . ? C5 C4 Pd1 129.2(5) . . ? C11 C6 C7 119.4(4) . . ? C11 C6 P1 125.0(4) . . ? C7 C6 P1 115.0(3) . . ? C8 C7 C6 120.0(5) . . ? C9 C8 C7 119.6(6) . . ? C8 C9 C10 121.2(5) . . ? C9 C10 C11 120.3(5) . . ? C6 C11 C10 119.5(5) . . ? C14 C12 N2 105.2(4) . . ? C14 C12 C13 130.6(5) . . ? N2 C12 C13 124.2(5) . . ? C12 C14 C15 108.5(4) . . ? N3 C15 C14 110.2(4) . . ? N3 C15 C16 121.3(5) . . ? C14 C15 C16 128.4(5) . . ? C19 C17 C18 112.6(4) . . ? C19 C17 N1 113.4(3) . . ? C18 C17 N1 113.1(4) . . ? C21 C20 C25 119.3(5) . . ? C21 C20 P2 121.1(4) . . ? C25 C20 P2 119.0(4) . . ? C22 C21 C20 121.0(5) . . ? C21 C22 C23 119.5(6) . . ? C24 C23 C22 120.6(6) . . ? C23 C24 C25 120.2(6) . . ? C24 C25 C20 119.3(6) . . ? C31 C26 C27 120.6(5) . . ? C31 C26 P2 123.8(5) . . ? C27 C26 P2 115.5(4) . . ? C28 C27 C26 120.2(7) . . ? C29 C28 C27 118.4(8) . . ? C28 C29 C30 122.6(7) . . ? C29 C30 C31 118.6(8) . . ? C26 C31 C30 119.5(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.849 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.084