Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Jose Ruiz' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Universidad de Murcia Murcia 30071 SPAIN ; _publ_contact_author_email JRUIZ@UM.ES _publ_section_title ; Pentafluorophenyl imidato palladium(II) complexes: catalysts for the Suzuki cross-coupling reactions ; loop_ _publ_author_name 'Jose Ruiz' 'Natalia Cutillas' 'Jose Perez' 'Consuelo Vicente' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 265321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H41 Cl3 F10 N6 O6 Pd2' _chemical_formula_weight 1126.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2880(10) _cell_length_b 14.3170(10) _cell_length_c 20.7880(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.000(10) _cell_angle_gamma 90.00 _cell_volume 4351.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 6.48 _cell_measurement_theta_max 12.41 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.6311 _exptl_absorpt_correction_T_max 0.8884 _exptl_absorpt_process_details PSI-SCAN _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10391 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7639 _reflns_number_gt 5268 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7639 _refine_ls_number_parameters 585 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 0.774 _refine_ls_restrained_S_all 0.831 _refine_ls_shift/su_max 0.203 _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 0.02353(3) 0.15907(3) 0.28719(2) 0.01899(14) Uani 1 1 d . . . F4 F -0.1147(3) -0.0195(3) 0.46197(18) 0.0376(10) Uani 1 1 d . . . F2 F -0.0590(3) 0.3028(3) 0.50011(18) 0.0438(10) Uani 1 1 d . . . F5 F -0.0545(2) -0.0112(2) 0.35419(18) 0.0310(8) Uani 1 1 d . . . C1 C -0.0213(4) 0.1513(4) 0.3687(3) 0.0241(13) Uani 1 1 d . . . F3 F -0.1200(3) 0.1369(3) 0.53521(19) 0.0448(11) Uani 1 1 d . . . F1 F 0.0047(3) 0.3122(3) 0.39329(18) 0.0356(9) Uani 1 1 d . . . C2 C -0.0240(4) 0.2278(4) 0.4086(3) 0.0264(14) Uani 1 1 d . . . C4 C -0.0875(4) 0.1415(5) 0.4819(3) 0.0316(15) Uani 1 1 d . . . C3 C -0.0568(4) 0.2252(5) 0.4639(3) 0.0299(15) Uani 1 1 d . . . C5 C -0.0862(4) 0.0634(5) 0.4438(3) 0.0285(15) Uani 1 1 d . . . C6 C -0.0547(4) 0.0691(4) 0.3885(3) 0.0253(14) Uani 1 1 d . . . Pd2 Pd 0.48422(3) 0.38925(3) 0.22467(2) 0.01928(14) Uani 1 1 d . . . O2 O -0.0814(3) 0.3647(3) 0.2427(2) 0.0360(11) Uani 1 1 d . . . O1 O -0.1788(3) 0.0646(3) 0.2094(3) 0.0432(13) Uani 1 1 d . . . N1 N -0.1018(3) 0.2049(4) 0.2342(2) 0.0237(11) Uani 1 1 d . . . C7 C -0.1765(4) 0.1485(5) 0.2072(3) 0.0290(15) Uani 1 1 d . . . C10 C -0.1289(4) 0.2966(4) 0.2243(3) 0.0261(14) Uani 1 1 d . . . C8 C -0.2573(4) 0.2098(5) 0.1742(3) 0.0345(16) Uani 1 1 d . . . H8 H -0.3173 0.1896 0.1507 0.041 Uiso 1 1 calc R . . C9 C -0.2281(4) 0.2977(5) 0.1843(3) 0.0367(16) Uani 1 1 d . . . H9 H -0.2639 0.3519 0.1689 0.044 Uiso 1 1 calc R . . N2 N 0.1549(3) 0.1146(4) 0.3388(2) 0.0247(11) Uani 1 1 d . . . N3 N 0.0725(3) 0.1623(3) 0.2011(2) 0.0235(11) Uani 1 1 d . . . C14 C 0.1731(4) 0.1567(5) 0.2287(3) 0.0323(15) Uani 1 1 d . . . H14A H 0.1980 0.2191 0.2447 0.039 Uiso 1 1 calc R . . H14B H 0.1998 0.1366 0.1930 0.039 Uiso 1 1 calc R . . C11 C 0.1578(4) 0.0321(4) 0.3819(3) 0.0291(15) Uani 1 1 d . . . H11A H 0.1231 -0.0190 0.3547 0.044 Uiso 1 1 calc R . . H11B H 0.1308 0.0480 0.4178 0.044 Uiso 1 1 calc R . . H11C H 0.2215 0.0127 0.4017 0.044 Uiso 1 1 calc R . . C15 C 0.0350(5) 0.0801(5) 0.1585(3) 0.0365(16) Uani 1 1 d . . . H15A H -0.0317 0.0857 0.1412 0.055 Uiso 1 1 calc R . . H15B H 0.0507 0.0230 0.1853 0.055 Uiso 1 1 calc R . . H15C H 0.0611 0.0774 0.1207 0.055 Uiso 1 1 calc R . . C13 C 0.1988(4) 0.0881(5) 0.2861(3) 0.0332(16) Uani 1 1 d . . . H13A H 0.1788 0.0246 0.2692 0.040 Uiso 1 1 calc R . . H13B H 0.2661 0.0872 0.3058 0.040 Uiso 1 1 calc R . . C16 C 0.0494(5) 0.2485(5) 0.1593(3) 0.0349(16) Uani 1 1 d . . . H16A H -0.0172 0.2535 0.1406 0.052 Uiso 1 1 calc R . . H16B H 0.0774 0.2455 0.1226 0.052 Uiso 1 1 calc R . . H16C H 0.0726 0.3033 0.1874 0.052 Uiso 1 1 calc R . . C12 C 0.2070(4) 0.1917(5) 0.3812(4) 0.0378(17) Uani 1 1 d . . . H12A H 0.2049 0.2474 0.3533 0.057 Uiso 1 1 calc R . . H12B H 0.2707 0.1725 0.4010 0.057 Uiso 1 1 calc R . . H12C H 0.1795 0.2061 0.4172 0.057 Uiso 1 1 calc R . . F8 F 0.6115(3) 0.3423(4) -0.0299(2) 0.0602(14) Uani 1 1 d . . . F6 F 0.4870(3) 0.2131(3) 0.1307(2) 0.0418(10) Uani 1 1 d . . . F10 F 0.5622(3) 0.5340(3) 0.13845(19) 0.0362(9) Uani 1 1 d . . . N4 N 0.6109(3) 0.3514(3) 0.2800(2) 0.0216(11) Uani 1 1 d . . . N5 N 0.4406(3) 0.4089(4) 0.3120(2) 0.0253(12) Uani 1 1 d . . . F7 F 0.5461(3) 0.1933(3) 0.0230(2) 0.0576(13) Uani 1 1 d . . . F9 F 0.6168(3) 0.5143(3) 0.02919(19) 0.0461(11) Uani 1 1 d . . . O3 O 0.5913(3) 0.1913(3) 0.2788(2) 0.0375(12) Uani 1 1 d . . . C17 C 0.5225(4) 0.3737(5) 0.1402(3) 0.0251(14) Uani 1 1 d . . . N6 N 0.3505(3) 0.4242(4) 0.1709(2) 0.0254(11) Uani 1 1 d . . . O4 O 0.6866(3) 0.4929(3) 0.3028(3) 0.0401(12) Uani 1 1 d . . . C28 C 0.3025(4) 0.3408(5) 0.1353(3) 0.0351(16) Uani 1 1 d . . . H28A H 0.3333 0.3190 0.1029 0.053 Uiso 1 1 calc R . . H28B H 0.2390 0.3571 0.1116 0.053 Uiso 1 1 calc R . . H28C H 0.3035 0.2912 0.1680 0.053 Uiso 1 1 calc R . . C18 C 0.5201(4) 0.2898(5) 0.1070(3) 0.0291(15) Uani 1 1 d . . . C26 C 0.6841(4) 0.4087(5) 0.3080(3) 0.0262(14) Uani 1 1 d . . . C27 C 0.3445(4) 0.5007(5) 0.1215(3) 0.0309(15) Uani 1 1 d . . . H27A H 0.3760 0.5561 0.1448 0.046 Uiso 1 1 calc R . . H27B H 0.2801 0.5157 0.0996 0.046 Uiso 1 1 calc R . . H27C H 0.3734 0.4807 0.0875 0.046 Uiso 1 1 calc R . . C24 C 0.7366(4) 0.2625(5) 0.3388(3) 0.0349(16) Uani 1 1 d . . . H24 H 0.7728 0.2097 0.3573 0.042 Uiso 1 1 calc R . . C31 C 0.4710(5) 0.3365(5) 0.3649(3) 0.0382(17) Uani 1 1 d . . . H31A H 0.4508 0.2749 0.3457 0.057 Uiso 1 1 calc R . . H31B H 0.4446 0.3495 0.4016 0.057 Uiso 1 1 calc R . . H31C H 0.5379 0.3374 0.3823 0.057 Uiso 1 1 calc R . . C25 C 0.7627(5) 0.3482(5) 0.3462(3) 0.0364(17) Uani 1 1 d . . . H25 H 0.8216 0.3696 0.3715 0.044 Uiso 1 1 calc R . . C19 C 0.5493(5) 0.2785(5) 0.0513(3) 0.0407(18) Uani 1 1 d . . . C23 C 0.6385(4) 0.2604(5) 0.2956(3) 0.0270(14) Uani 1 1 d . . . C21 C 0.5860(4) 0.4392(5) 0.0551(3) 0.0291(15) Uani 1 1 d . . . C30 C 0.3381(4) 0.4042(5) 0.2851(3) 0.0350(16) Uani 1 1 d . . . H30A H 0.3186 0.3383 0.2768 0.042 Uiso 1 1 calc R . . H30B H 0.3104 0.4300 0.3188 0.042 Uiso 1 1 calc R . . C22 C 0.5571(4) 0.4475(5) 0.1118(3) 0.0260(14) Uani 1 1 d . . . C29 C 0.3058(4) 0.4586(5) 0.2212(3) 0.0340(16) Uani 1 1 d . . . H29A H 0.2386 0.4524 0.2027 0.041 Uiso 1 1 calc R . . H29B H 0.3203 0.5255 0.2305 0.041 Uiso 1 1 calc R . . C32 C 0.4709(5) 0.5017(5) 0.3409(3) 0.0372(17) Uani 1 1 d . . . H32A H 0.4513 0.5494 0.3059 0.056 Uiso 1 1 calc R . . H32B H 0.5378 0.5024 0.3588 0.056 Uiso 1 1 calc R . . H32C H 0.4439 0.5147 0.3773 0.056 Uiso 1 1 calc R . . C20 C 0.5823(5) 0.3530(6) 0.0244(3) 0.0386(18) Uani 1 1 d . . . O5 O 0.3913(4) 0.1715(4) 0.2442(3) 0.0413(13) Uani 1 1 d D . . H5A H 0.448(4) 0.178(6) 0.256(4) 0.06(3) Uiso 1 1 d D . . H5B H 0.382(8) 0.117(5) 0.230(6) 0.12(5) Uiso 1 1 d D . . O6 O 0.1174(4) 0.3867(4) 0.3077(3) 0.0427(13) Uani 1 1 d D . . H6A H 0.070(5) 0.373(7) 0.280(4) 0.09(4) Uiso 1 1 d D . . H6B H 0.124(6) 0.439(4) 0.295(4) 0.05(3) Uiso 1 1 d D . . C33 C 0.2145(4) 0.4423(4) 0.4676(3) 0.085(4) Uani 1 1 d D . . H33 H 0.1883 0.4214 0.4200 0.101 Uiso 1 1 calc R A 1 Cl1 Cl 0.2694(5) 0.5525(5) 0.4707(3) 0.135(3) Uani 0.625(7) 1 d PDU B 1 Cl2 Cl 0.1297(3) 0.4706(5) 0.5014(2) 0.115(3) Uani 0.625(7) 1 d PD B 1 Cl3 Cl 0.2995(6) 0.3698(5) 0.5094(4) 0.163(4) Uani 0.625(7) 1 d PDU B 1 Cl1' Cl 0.2030(10) 0.5572(6) 0.4882(7) 0.193(7) Uani 0.375(7) 1 d PDU B 2 Cl2' Cl 0.1788(7) 0.3684(8) 0.5255(4) 0.126(4) Uani 0.375(7) 1 d PDU B 2 Cl3' Cl 0.3299(4) 0.4141(9) 0.4826(4) 0.129(6) Uani 0.375(7) 1 d PD B 2 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 0.0177(2) 0.0148(2) 0.0242(2) 0.00265(19) 0.00571(18) 0.00179(19) F4 0.035(2) 0.038(2) 0.037(2) 0.0161(18) 0.0067(17) -0.0087(18) F2 0.064(3) 0.037(2) 0.033(2) -0.0103(18) 0.018(2) 0.005(2) F5 0.038(2) 0.0158(19) 0.040(2) -0.0001(16) 0.0121(17) -0.0036(16) C1 0.022(3) 0.022(3) 0.026(3) 0.002(3) 0.004(2) -0.004(3) F3 0.053(3) 0.054(3) 0.033(2) 0.0071(19) 0.0209(19) 0.001(2) F1 0.049(2) 0.019(2) 0.040(2) -0.0015(16) 0.0155(18) -0.0020(18) C2 0.023(3) 0.023(3) 0.030(3) 0.004(3) 0.003(3) 0.004(3) C4 0.031(4) 0.039(4) 0.025(3) 0.002(3) 0.010(3) 0.003(3) C3 0.034(4) 0.030(4) 0.024(3) -0.004(3) 0.006(3) 0.005(3) C5 0.023(3) 0.034(4) 0.026(3) 0.009(3) 0.003(3) -0.007(3) C6 0.019(3) 0.021(3) 0.031(3) 0.001(3) 0.001(3) 0.002(3) Pd2 0.0181(2) 0.0157(2) 0.0231(2) 0.00187(18) 0.00459(17) 0.00158(19) O2 0.037(3) 0.017(2) 0.051(3) 0.005(2) 0.007(2) 0.001(2) O1 0.026(2) 0.022(3) 0.078(4) 0.000(3) 0.009(2) -0.001(2) N1 0.021(3) 0.020(3) 0.029(3) 0.003(2) 0.006(2) 0.004(2) C7 0.017(3) 0.028(4) 0.043(4) 0.002(3) 0.011(3) 0.001(3) C10 0.027(3) 0.021(3) 0.030(3) 0.002(3) 0.007(3) 0.003(3) C8 0.020(3) 0.033(4) 0.045(4) 0.004(3) 0.001(3) 0.005(3) C9 0.030(4) 0.027(4) 0.048(4) 0.008(3) 0.004(3) 0.010(3) N2 0.020(3) 0.018(3) 0.034(3) 0.007(2) 0.005(2) 0.003(2) N3 0.024(3) 0.020(3) 0.026(3) 0.001(2) 0.008(2) 0.001(2) C14 0.024(3) 0.033(4) 0.044(4) 0.008(3) 0.016(3) -0.002(3) C11 0.027(3) 0.020(3) 0.036(4) 0.009(3) 0.002(3) 0.006(3) C15 0.046(4) 0.029(4) 0.041(4) -0.004(3) 0.024(3) -0.006(3) C13 0.023(3) 0.038(4) 0.040(4) 0.009(3) 0.011(3) 0.012(3) C16 0.041(4) 0.029(4) 0.036(4) 0.014(3) 0.014(3) 0.006(3) C12 0.028(4) 0.027(4) 0.050(4) -0.004(3) -0.002(3) -0.008(3) F8 0.067(3) 0.088(4) 0.034(2) 0.005(2) 0.027(2) 0.020(3) F6 0.059(3) 0.021(2) 0.044(2) -0.0017(18) 0.012(2) 0.0008(19) F10 0.037(2) 0.031(2) 0.040(2) -0.0004(18) 0.0093(18) -0.0066(18) N4 0.021(3) 0.018(3) 0.025(2) 0.001(2) 0.005(2) 0.001(2) N5 0.028(3) 0.023(3) 0.026(3) 0.000(2) 0.011(2) -0.001(2) F7 0.084(3) 0.050(3) 0.038(2) -0.012(2) 0.016(2) 0.020(3) F9 0.037(2) 0.064(3) 0.038(2) 0.018(2) 0.0115(18) -0.006(2) O3 0.034(3) 0.018(2) 0.051(3) 0.001(2) -0.002(2) 0.001(2) C17 0.016(3) 0.031(4) 0.024(3) 0.003(3) -0.001(2) 0.003(3) N6 0.021(3) 0.024(3) 0.029(3) 0.004(2) 0.004(2) -0.001(2) O4 0.031(3) 0.021(3) 0.062(3) 0.001(2) 0.004(2) -0.002(2) C28 0.024(3) 0.028(4) 0.047(4) 0.004(3) 0.001(3) -0.003(3) C18 0.036(4) 0.025(4) 0.024(3) 0.005(3) 0.004(3) 0.005(3) C26 0.021(3) 0.026(4) 0.031(3) 0.001(3) 0.006(3) 0.002(3) C27 0.027(3) 0.025(4) 0.037(4) 0.012(3) 0.006(3) 0.005(3) C24 0.029(4) 0.028(4) 0.040(4) 0.005(3) 0.000(3) 0.006(3) C31 0.050(4) 0.036(4) 0.029(3) 0.009(3) 0.012(3) 0.014(4) C25 0.028(3) 0.033(4) 0.040(4) 0.000(3) -0.005(3) 0.000(3) C19 0.048(4) 0.041(5) 0.027(4) -0.006(3) 0.001(3) 0.018(4) C23 0.025(3) 0.023(3) 0.032(3) 0.003(3) 0.007(3) 0.001(3) C21 0.020(3) 0.036(4) 0.026(3) 0.009(3) 0.000(3) 0.003(3) C30 0.024(3) 0.043(4) 0.044(4) 0.006(3) 0.018(3) 0.005(3) C22 0.020(3) 0.031(4) 0.026(3) 0.000(3) 0.005(2) 0.000(3) C29 0.021(3) 0.037(4) 0.044(4) 0.009(3) 0.009(3) 0.007(3) C32 0.044(4) 0.032(4) 0.040(4) -0.013(3) 0.019(3) -0.002(3) C20 0.035(4) 0.058(5) 0.021(3) 0.000(3) 0.006(3) 0.016(4) O5 0.033(3) 0.025(3) 0.064(3) 0.004(3) 0.012(3) -0.001(2) O6 0.033(3) 0.025(3) 0.067(4) 0.012(3) 0.009(3) -0.005(2) C33 0.095(8) 0.108(10) 0.041(5) -0.022(6) 0.005(5) 0.018(7) Cl1 0.156(5) 0.152(5) 0.103(4) 0.013(4) 0.045(4) -0.056(4) Cl2 0.091(4) 0.187(8) 0.073(3) -0.058(4) 0.035(3) -0.038(4) Cl3 0.168(6) 0.109(5) 0.151(6) -0.039(4) -0.048(4) 0.062(5) Cl1' 0.217(9) 0.173(9) 0.174(9) -0.030(7) 0.032(7) 0.084(7) Cl2' 0.125(7) 0.191(8) 0.067(4) -0.016(5) 0.038(4) -0.045(6) Cl3' 0.053(4) 0.266(18) 0.075(6) -0.047(8) 0.030(4) -0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.008(6) . ? Pd1 N1 2.020(5) . ? Pd1 N2 2.081(5) . ? Pd1 N3 2.132(5) . ? F4 C5 1.354(7) . ? F2 C3 1.347(7) . ? F5 C6 1.354(7) . ? C1 C2 1.381(9) . ? C1 C6 1.392(9) . ? F3 C4 1.343(7) . ? F1 C2 1.355(7) . ? C2 C3 1.383(9) . ? C4 C5 1.374(9) . ? C4 C3 1.378(9) . ? C5 C6 1.374(9) . ? Pd2 N4 2.016(5) . ? Pd2 C17 2.019(6) . ? Pd2 N6 2.084(5) . ? Pd2 N5 2.127(5) . ? O2 C10 1.209(8) . ? O1 C7 1.204(8) . ? N1 C10 1.374(8) . ? N1 C7 1.377(8) . ? C7 C8 1.507(9) . ? C10 C9 1.502(8) . ? C8 C9 1.332(10) . ? N2 C11 1.474(7) . ? N2 C12 1.490(8) . ? N2 C13 1.491(8) . ? N3 C14 1.478(7) . ? N3 C15 1.483(8) . ? N3 C16 1.492(8) . ? C14 C13 1.506(9) . ? F8 C20 1.339(8) . ? F6 C18 1.359(7) . ? F10 C22 1.349(7) . ? N4 C26 1.372(8) . ? N4 C23 1.379(8) . ? N5 C32 1.476(8) . ? N5 C31 1.484(8) . ? N5 C30 1.502(8) . ? F7 C19 1.349(8) . ? F9 C21 1.347(7) . ? O3 C23 1.213(8) . ? C17 C18 1.381(9) . ? C17 C22 1.389(9) . ? N6 C28 1.481(8) . ? N6 C27 1.485(8) . ? N6 C29 1.490(8) . ? O4 C26 1.211(8) . ? C18 C19 1.367(9) . ? C26 C25 1.507(9) . ? C24 C25 1.285(9) . ? C24 C23 1.506(8) . ? C19 C20 1.368(11) . ? C21 C22 1.381(9) . ? C21 C20 1.383(10) . ? C30 C29 1.495(9) . ? C33 Cl3 1.692(5) . ? C33 Cl2 1.695(5) . ? C33 Cl1' 1.721(5) . ? C33 Cl3' 1.747(5) . ? C33 Cl1 1.780(5) . ? C33 Cl2' 1.802(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 88.6(2) . . ? C1 Pd1 N2 93.7(2) . . ? N1 Pd1 N2 177.6(2) . . ? C1 Pd1 N3 178.0(2) . . ? N1 Pd1 N3 92.59(19) . . ? N2 Pd1 N3 85.21(19) . . ? C2 C1 C6 114.5(6) . . ? C2 C1 Pd1 122.7(5) . . ? C6 C1 Pd1 122.8(5) . . ? F1 C2 C1 119.8(5) . . ? F1 C2 C3 116.1(6) . . ? C1 C2 C3 124.1(6) . . ? F3 C4 C5 120.4(6) . . ? F3 C4 C3 120.3(6) . . ? C5 C4 C3 119.3(6) . . ? F2 C3 C4 120.0(6) . . ? F2 C3 C2 121.2(6) . . ? C4 C3 C2 118.9(6) . . ? F4 C5 C4 119.6(6) . . ? F4 C5 C6 120.4(6) . . ? C4 C5 C6 120.1(6) . . ? F5 C6 C5 116.4(6) . . ? F5 C6 C1 120.4(5) . . ? C5 C6 C1 123.2(6) . . ? N4 Pd2 C17 89.5(2) . . ? N4 Pd2 N6 177.0(2) . . ? C17 Pd2 N6 92.8(2) . . ? N4 Pd2 N5 92.2(2) . . ? C17 Pd2 N5 178.1(2) . . ? N6 Pd2 N5 85.6(2) . . ? C10 N1 C7 108.8(5) . . ? C10 N1 Pd1 126.0(4) . . ? C7 N1 Pd1 125.0(4) . . ? O1 C7 N1 126.9(6) . . ? O1 C7 C8 124.7(6) . . ? N1 C7 C8 108.4(6) . . ? O2 C10 N1 126.6(6) . . ? O2 C10 C9 125.6(6) . . ? N1 C10 C9 107.7(5) . . ? C9 C8 C7 106.6(6) . . ? C8 C9 C10 108.4(6) . . ? C11 N2 C12 108.5(5) . . ? C11 N2 C13 107.6(5) . . ? C12 N2 C13 110.2(5) . . ? C11 N2 Pd1 114.3(4) . . ? C12 N2 Pd1 110.2(4) . . ? C13 N2 Pd1 105.9(4) . . ? C14 N3 C15 111.4(5) . . ? C14 N3 C16 108.2(5) . . ? C15 N3 C16 108.9(5) . . ? C14 N3 Pd1 104.7(4) . . ? C15 N3 Pd1 108.4(4) . . ? C16 N3 Pd1 115.1(4) . . ? N3 C14 C13 110.1(5) . . ? N2 C13 C14 110.3(5) . . ? C26 N4 C23 108.1(5) . . ? C26 N4 Pd2 127.5(4) . . ? C23 N4 Pd2 124.4(4) . . ? C32 N5 C31 109.4(5) . . ? C32 N5 C30 111.2(5) . . ? C31 N5 C30 108.1(5) . . ? C32 N5 Pd2 109.1(4) . . ? C31 N5 Pd2 115.6(4) . . ? C30 N5 Pd2 103.3(4) . . ? C18 C17 C22 114.0(6) . . ? C18 C17 Pd2 124.0(5) . . ? C22 C17 Pd2 121.9(5) . . ? C28 N6 C27 109.2(5) . . ? C28 N6 C29 110.8(5) . . ? C27 N6 C29 107.1(5) . . ? C28 N6 Pd2 109.8(4) . . ? C27 N6 Pd2 113.6(4) . . ? C29 N6 Pd2 106.4(4) . . ? F6 C18 C19 117.4(6) . . ? F6 C18 C17 118.7(5) . . ? C19 C18 C17 124.0(7) . . ? O4 C26 N4 126.9(6) . . ? O4 C26 C25 125.3(6) . . ? N4 C26 C25 107.8(5) . . ? C25 C24 C23 108.2(6) . . ? C24 C25 C26 108.2(6) . . ? F7 C19 C18 119.8(7) . . ? F7 C19 C20 119.9(6) . . ? C18 C19 C20 120.3(7) . . ? O3 C23 N4 126.0(6) . . ? O3 C23 C24 126.3(6) . . ? N4 C23 C24 107.6(5) . . ? F9 C21 C22 120.7(6) . . ? F9 C21 C20 120.0(6) . . ? C22 C21 C20 119.3(6) . . ? C29 C30 N5 110.1(5) . . ? F10 C22 C21 115.8(6) . . ? F10 C22 C17 120.5(5) . . ? C21 C22 C17 123.7(6) . . ? N6 C29 C30 110.6(5) . . ? F8 C20 C19 120.6(7) . . ? F8 C20 C21 120.8(7) . . ? C19 C20 C21 118.6(6) . . ? Cl3 C33 Cl2 120.0(5) . . ? Cl3 C33 Cl1' 125.3(7) . . ? Cl2 C33 Cl1' 61.5(5) . . ? Cl3 C33 Cl3' 35.2(4) . . ? Cl2 C33 Cl3' 146.8(6) . . ? Cl1' C33 Cl3' 110.3(5) . . ? Cl3 C33 Cl1 104.0(5) . . ? Cl2 C33 Cl1 100.6(4) . . ? Cl1' C33 Cl1 39.2(5) . . ? Cl3' C33 Cl1 75.9(5) . . ? Cl3 C33 Cl2' 68.5(5) . . ? Cl2 C33 Cl2' 56.3(4) . . ? Cl1' C33 Cl2' 108.8(5) . . ? Cl3' C33 Cl2' 103.5(4) . . ? Cl1 C33 Cl2' 136.7(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O3 0.84(6) 2.10(6) 2.942(7) 177(8) . O5 H5B O4 0.84(6) 2.07(7) 2.870(7) 160(11) 2_645 O6 H6A O2 0.81(6) 2.22(7) 2.960(7) 154(10) . O6 H6B O1 0.81(6) 2.00(6) 2.772(7) 160(8) 2 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.853 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.110 #===END data_complex10 _database_code_depnum_ccdc_archive 'CCDC 265322' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 F5 N3 O6 Pd' _chemical_formula_weight 748.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3563(5) _cell_length_b 41.9620(18) _cell_length_c 24.4230(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.77(1) _cell_angle_gamma 90.00 _cell_volume 10516.1(8) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8133 _exptl_absorpt_correction_T_max 0.8697 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122099 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.18 _reflns_number_total 24434 _reflns_number_gt 23456 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0359P)^2^+68.2378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24434 _refine_ls_number_parameters 1237 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.285 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.002 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 0.23885(4) 0.186444(9) 0.932993(16) 0.01808(9) Uani 1 1 d . . . N1 N 0.0929(5) 0.21903(11) 0.9334(2) 0.0276(10) Uani 1 1 d . . . C1 C 0.0342(6) 0.23398(14) 0.8873(3) 0.0300(12) Uani 1 1 d . . . C2 C -0.0635(7) 0.25865(17) 0.9022(3) 0.0437(17) Uani 1 1 d . . . H2A H -0.0475 0.2797 0.8862 0.052 Uiso 1 1 calc R . . H2B H -0.1540 0.2520 0.8891 0.052 Uiso 1 1 calc R . . C3 C -0.0388(6) 0.25970(15) 0.9648(3) 0.0360(14) Uani 1 1 d . . . H3A H -0.1212 0.2574 0.9808 0.043 Uiso 1 1 calc R . . H3B H 0.0036 0.2800 0.9779 0.043 Uiso 1 1 calc R . . C4 C 0.0513(5) 0.23146(13) 0.9803(2) 0.0255(11) Uani 1 1 d . . . O1 O 0.0534(4) 0.22794(12) 0.83996(18) 0.0397(11) Uani 1 1 d . . . O2 O 0.0809(4) 0.22146(10) 1.02742(16) 0.0296(9) Uani 1 1 d . . . C5 C 0.3700(5) 0.22097(14) 0.9478(2) 0.0254(11) Uani 1 1 d . . . C6 C 0.4210(5) 0.23682(14) 0.9057(3) 0.0300(12) Uani 1 1 d . . . C7 C 0.5143(6) 0.26052(15) 0.9149(3) 0.0357(14) Uani 1 1 d . . . C8 C 0.5594(6) 0.26952(15) 0.9685(3) 0.0380(15) Uani 1 1 d . . . C9 C 0.5110(6) 0.25459(15) 1.0113(3) 0.0347(14) Uani 1 1 d . . . C10 C 0.4197(5) 0.23055(14) 1.0004(3) 0.0284(12) Uani 1 1 d . . . F1 F 0.3790(3) 0.22959(9) 0.85247(15) 0.0353(8) Uani 1 1 d . . . F2 F 0.5616(4) 0.27487(10) 0.87222(19) 0.0491(10) Uani 1 1 d . . . F3 F 0.6499(4) 0.29265(10) 0.9781(2) 0.0547(12) Uani 1 1 d . . . F4 F 0.5565(4) 0.26284(10) 1.06362(18) 0.0467(10) Uani 1 1 d . . . F5 F 0.3814(3) 0.21618(9) 1.04500(14) 0.0342(8) Uani 1 1 d . . . N2 N 0.3841(4) 0.15453(10) 0.93223(19) 0.0224(9) Uani 1 1 d . . . C11 C 0.4381(5) 0.13863(13) 0.9783(2) 0.0248(11) Uani 1 1 d . . . C12 C 0.5422(6) 0.11570(14) 0.9642(3) 0.0319(13) Uani 1 1 d . . . H12A H 0.5171 0.0933 0.9703 0.038 Uiso 1 1 calc R . . H12B H 0.6270 0.1201 0.9868 0.038 Uiso 1 1 calc R . . C13 C 0.5489(6) 0.12200(15) 0.9033(3) 0.0317(13) Uani 1 1 d . . . H13A H 0.6350 0.1307 0.8978 0.038 Uiso 1 1 calc R . . H13B H 0.5330 0.1022 0.8813 0.038 Uiso 1 1 calc R . . C14 C 0.4416(5) 0.14624(13) 0.8869(2) 0.0271(11) Uani 1 1 d . . . O3 O 0.4072(4) 0.14167(11) 1.02453(17) 0.0332(9) Uani 1 1 d . . . O4 O 0.4118(5) 0.15630(11) 0.84040(18) 0.0403(11) Uani 1 1 d . . . O5 O 0.1059(4) 0.14793(10) 0.91819(16) 0.0235(8) Uani 1 1 d . . . H5A H 0.032(7) 0.1498(15) 0.928(3) 0.024(16) Uiso 1 1 d . . . H5B H 0.133(7) 0.1314(18) 0.931(3) 0.034(19) Uiso 1 1 d . . . Pd2 Pd 0.02448(4) 0.127004(9) 0.041194(16) 0.02005(9) Uani 1 1 d . . . N3 N -0.1155(4) 0.16056(11) 0.02811(18) 0.0245(9) Uani 1 1 d . . . C15 C -0.1740(5) 0.16961(14) -0.0221(2) 0.0262(11) Uani 1 1 d . . . C16 C -0.2803(6) 0.19425(14) -0.0172(3) 0.0330(13) Uani 1 1 d . . . H16A H -0.2622 0.2144 -0.0360 0.040 Uiso 1 1 calc R . . H16B H -0.3668 0.1861 -0.0335 0.040 Uiso 1 1 calc R . . C17 C -0.2743(6) 0.19914(16) 0.0442(3) 0.0361(14) Uani 1 1 d . . . H17A H -0.3578 0.1931 0.0569 0.043 Uiso 1 1 calc R . . H17B H -0.2550 0.2217 0.0542 0.043 Uiso 1 1 calc R . . C18 C -0.1644(5) 0.17744(13) 0.0697(2) 0.0274(11) Uani 1 1 d . . . O6 O -0.1457(4) 0.15985(11) -0.06635(17) 0.0331(9) Uani 1 1 d . . . O7 O -0.1254(4) 0.17582(11) 0.11877(17) 0.0359(10) Uani 1 1 d . . . C19 C -0.1126(5) 0.09388(13) 0.0335(3) 0.0309(13) Uani 1 1 d . . . C20 C -0.1896(6) 0.08799(14) 0.0736(3) 0.0342(13) Uani 1 1 d . . . C21 C -0.2834(6) 0.06395(16) 0.0708(3) 0.0444(17) Uani 1 1 d . . . C22 C -0.3025(7) 0.04519(17) 0.0256(5) 0.064(3) Uani 1 1 d . . . C23 C -0.2328(9) 0.0513(2) -0.0176(5) 0.091(4) Uani 1 1 d . . . C24 C -0.1388(7) 0.0749(2) -0.0125(4) 0.064(3) Uani 1 1 d . . . F6 F -0.1749(4) 0.10542(12) 0.12012(17) 0.0554(12) Uani 1 1 d . . . F7 F -0.3531(4) 0.05928(13) 0.1127(2) 0.0717(16) Uani 1 1 d . . . F8 F -0.3919(5) 0.02177(11) 0.0214(3) 0.101(3) Uani 1 1 d . . . F9 F -0.2579(7) 0.0341(2) -0.0645(5) 0.195(6) Uani 1 1 d . . . F10 F -0.0750(6) 0.07980(18) -0.0568(3) 0.111(3) Uani 1 1 d . . . N4 N 0.1626(4) 0.09314(11) 0.05085(19) 0.0260(10) Uani 1 1 d . . . C25 C 0.2054(6) 0.07839(16) 0.0999(3) 0.0363(14) Uani 1 1 d . . . C26 C 0.3096(7) 0.05373(19) 0.0928(3) 0.0482(18) Uani 1 1 d . . . H26A H 0.3930 0.0590 0.1158 0.058 Uiso 1 1 calc R . . H26B H 0.2818 0.0322 0.1027 0.058 Uiso 1 1 calc R . . C27 C 0.3222(7) 0.05580(17) 0.0319(3) 0.0471(18) Uani 1 1 d . . . H27A H 0.2972 0.0354 0.0131 0.057 Uiso 1 1 calc R . . H27B H 0.4127 0.0611 0.0264 0.057 Uiso 1 1 calc R . . C28 C 0.2290(6) 0.08233(14) 0.0101(3) 0.0318(13) Uani 1 1 d . . . O8 O 0.1670(5) 0.08426(13) 0.14400(19) 0.0465(12) Uani 1 1 d . . . O9 O 0.2166(4) 0.09255(10) -0.03719(18) 0.0335(9) Uani 1 1 d . . . O10 O 0.1726(4) 0.16176(11) 0.05423(17) 0.0241(8) Uani 1 1 d . . . H10A H 0.150(7) 0.1788(18) 0.046(3) 0.029(19) Uiso 1 1 d . . . H10B H 0.235(8) 0.1585(18) 0.046(3) 0.04(2) Uiso 1 1 d . . . Pd3 Pd 0.89514(4) 0.032907(9) 0.545840(17) 0.02147(10) Uani 1 1 d . . . N5 N 1.0378(4) 0.06509(11) 0.5416(2) 0.0244(9) Uani 1 1 d . . . C29 C 1.0804(6) 0.07516(13) 0.4940(3) 0.0303(13) Uani 1 1 d . . . C30 C 1.1769(7) 0.10258(16) 0.5064(3) 0.0443(17) Uani 1 1 d . . . H30A H 1.2537 0.0997 0.4867 0.053 Uiso 1 1 calc R . . H30B H 1.1353 0.1233 0.4956 0.053 Uiso 1 1 calc R . . C31 C 1.2149(9) 0.1005(2) 0.5686(4) 0.064(3) Uani 1 1 d . . . H31A H 1.2130 0.1218 0.5860 0.076 Uiso 1 1 calc R . . H31B H 1.3031 0.0912 0.5779 0.076 Uiso 1 1 calc R . . C32 C 1.1111(8) 0.07862(18) 0.5869(3) 0.0496(19) Uani 1 1 d . . . O11 O 1.0465(4) 0.06430(10) 0.44836(18) 0.0352(10) Uani 1 1 d . . . O12 O 1.0958(7) 0.07417(15) 0.6346(2) 0.0691(19) Uani 1 1 d . . . C33 C 0.7635(5) 0.06665(13) 0.5240(3) 0.0306(13) Uani 1 1 d . . . C34 C 0.7146(5) 0.07288(14) 0.4706(3) 0.0304(12) Uani 1 1 d . . . C35 C 0.6209(6) 0.09631(15) 0.4552(3) 0.0395(15) Uani 1 1 d . . . C36 C 0.5742(7) 0.11407(16) 0.4960(4) 0.049(2) Uani 1 1 d . . . C37 C 0.6203(8) 0.10813(19) 0.5502(4) 0.054(2) Uani 1 1 d . . . C38 C 0.7143(7) 0.08500(16) 0.5635(3) 0.0440(17) Uani 1 1 d . . . F11 F 0.7536(4) 0.05599(9) 0.42842(15) 0.0402(9) Uani 1 1 d . . . F12 F 0.5743(4) 0.10110(11) 0.4020(2) 0.0550(12) Uani 1 1 d . . . F13 F 0.4824(4) 0.13662(11) 0.4820(3) 0.0685(15) Uani 1 1 d . . . F14 F 0.5731(6) 0.12548(13) 0.5898(3) 0.0831(18) Uani 1 1 d . . . F15 F 0.7552(5) 0.08108(12) 0.61754(19) 0.0623(13) Uani 1 1 d . . . N6 N 0.7499(4) 0.00101(11) 0.5476(2) 0.0241(9) Uani 1 1 d . . . C39 C 0.6864(6) -0.00524(15) 0.5926(3) 0.0354(14) Uani 1 1 d . . . C40 C 0.5715(6) -0.02754(18) 0.5760(3) 0.0441(17) Uani 1 1 d . . . H40A H 0.4878 -0.0167 0.5788 0.053 Uiso 1 1 calc R . . H40B H 0.5778 -0.0468 0.5996 0.053 Uiso 1 1 calc R . . C41 C 0.5828(6) -0.03624(14) 0.5160(3) 0.0352(14) Uani 1 1 d . . . H41A H 0.6018 -0.0592 0.5124 0.042 Uiso 1 1 calc R . . H41B H 0.5016 -0.0310 0.4914 0.042 Uiso 1 1 calc R . . C42 C 0.6958(5) -0.01589(14) 0.5027(3) 0.0297(12) Uani 1 1 d . . . O13 O 0.7168(5) 0.00561(15) 0.6383(2) 0.0538(14) Uani 1 1 d . . . O14 O 0.7316(4) -0.01565(11) 0.45695(19) 0.0364(10) Uani 1 1 d . . . O15 O 1.0354(4) -0.00235(11) 0.57211(17) 0.0251(8) Uani 1 1 d . . . H15A H 1.094(7) 0.0026(17) 0.560(3) 0.031(19) Uiso 1 1 d . . . H15B H 1.018(9) -0.020(2) 0.564(4) 0.06(3) Uiso 1 1 d . . . C51 C 0.0658(5) 0.22721(15) 0.1823(2) 0.0294(12) Uani 1 1 d . . . H51A H 0.0510 0.2271 0.1414 0.035 Uiso 1 1 calc R . . H51B H 0.0298 0.2071 0.1951 0.035 Uiso 1 1 calc R . . C48 C 0.2411(7) 0.26899(15) 0.1259(3) 0.0343(13) Uani 1 1 d . . . H48A H 0.1460 0.2724 0.1169 0.041 Uiso 1 1 calc R . . H48B H 0.2667 0.2519 0.1014 0.041 Uiso 1 1 calc R . . C43 C 0.2675(6) 0.19916(14) 0.1727(2) 0.0290(12) Uani 1 1 d . . . H43A H 0.2139 0.1802 0.1785 0.035 Uiso 1 1 calc R . . H43B H 0.2569 0.2034 0.1325 0.035 Uiso 1 1 calc R . . C47 C 0.2731(6) 0.25876(14) 0.1858(2) 0.0301(12) Uani 1 1 d . . . H47A H 0.3690 0.2568 0.1946 0.036 Uiso 1 1 calc R . . H47B H 0.2449 0.2759 0.2095 0.036 Uiso 1 1 calc R . . C44 C 0.4078(6) 0.19090(17) 0.1911(3) 0.0385(15) Uani 1 1 d . . . H44A H 0.4214 0.1864 0.2312 0.046 Uiso 1 1 calc R . . H44B H 0.4644 0.2090 0.1839 0.046 Uiso 1 1 calc R . . C45 C 0.4427(6) 0.16156(16) 0.1589(3) 0.0381(14) Uani 1 1 d . . . H45A H 0.3781 0.1446 0.1627 0.046 Uiso 1 1 calc R . . H45B H 0.4363 0.1671 0.1193 0.046 Uiso 1 1 calc R . . C46 C 0.5781(7) 0.1486(2) 0.1780(4) 0.0522(19) Uani 1 1 d . . . H46A H 0.5938 0.1299 0.1557 0.078 Uiso 1 1 calc R . . H46B H 0.5849 0.1425 0.2170 0.078 Uiso 1 1 calc R . . H46C H 0.6431 0.1650 0.1734 0.078 Uiso 1 1 calc R . . C52 C -0.0093(6) 0.25492(15) 0.2026(2) 0.0310(13) Uani 1 1 d . . . H52A H 0.0147 0.2574 0.2430 0.037 Uiso 1 1 calc R . . H52B H 0.0139 0.2749 0.1845 0.037 Uiso 1 1 calc R . . C49 C 0.3134(7) 0.29973(16) 0.1157(3) 0.0398(15) Uani 1 1 d . . . H49A H 0.2884 0.3166 0.1406 0.048 Uiso 1 1 calc R . . H49B H 0.4084 0.2961 0.1247 0.048 Uiso 1 1 calc R . . C50 C 0.2832(8) 0.31101(18) 0.0560(3) 0.0497(18) Uani 1 1 d . . . H50A H 0.3316 0.3307 0.0513 0.075 Uiso 1 1 calc R . . H50B H 0.1896 0.3151 0.0472 0.075 Uiso 1 1 calc R . . H50C H 0.3091 0.2945 0.0313 0.075 Uiso 1 1 calc R . . C53 C -0.1549(7) 0.24906(19) 0.1895(3) 0.050(2) Uani 1 1 d . . . H53A H -0.1753 0.2423 0.1504 0.060 Uiso 1 1 calc R . . H53B H -0.2018 0.2693 0.1938 0.060 Uiso 1 1 calc R . . C54 C -0.2041(8) 0.2235(2) 0.2269(5) 0.075(3) Uani 1 1 d . . . H54A H -0.2981 0.2205 0.2166 0.112 Uiso 1 1 calc R . . H54B H -0.1866 0.2303 0.2655 0.112 Uiso 1 1 calc R . . H54C H -0.1590 0.2033 0.2224 0.112 Uiso 1 1 calc R . . C55 C 0.2418(6) 0.22499(14) 0.2634(2) 0.0297(12) Uani 1 1 d . . . H55A H 0.2077 0.2443 0.2799 0.036 Uiso 1 1 calc R . . H55B H 0.3376 0.2249 0.2737 0.036 Uiso 1 1 calc R . . C56 C 0.1868(7) 0.19597(16) 0.2892(3) 0.0384(14) Uani 1 1 d . . . H56A H 0.2074 0.1765 0.2692 0.046 Uiso 1 1 calc R . . H56B H 0.0909 0.1978 0.2866 0.046 Uiso 1 1 calc R . . C63 C 0.8839(8) 0.09561(19) 0.2770(4) 0.058(2) Uani 1 1 d . . . H63A H 0.9362 0.1105 0.2575 0.070 Uiso 1 1 calc R . . H63B H 0.7947 0.0953 0.2564 0.070 Uiso 1 1 calc R . . C59 C 0.9371(9) 0.0548(2) 0.2141(3) 0.060(2) Uani 1 1 d . . . H59A H 0.8447 0.0543 0.1972 0.072 Uiso 1 1 calc R . . H59B H 0.9802 0.0723 0.1963 0.072 Uiso 1 1 calc R . . C71 C 1.0820(8) 0.0614(2) 0.3039(3) 0.063(3) Uani 1 1 d . . . H71A H 1.1166 0.0396 0.3007 0.076 Uiso 1 1 calc R . . H71B H 1.0811 0.0659 0.3436 0.076 Uiso 1 1 calc R . . C67 C 0.8657(9) 0.0381(2) 0.3032(4) 0.062(2) Uani 1 1 d . . . H67A H 0.9086 0.0171 0.3015 0.074 Uiso 1 1 calc R . . H67B H 0.8708 0.0441 0.3426 0.074 Uiso 1 1 calc R . . C60 C 0.9991(9) 0.0243(2) 0.2013(3) 0.064(3) Uani 1 1 d . . . H60A H 0.9718 0.0071 0.2250 0.077 Uiso 1 1 calc R . . H60B H 1.0951 0.0263 0.2087 0.077 Uiso 1 1 calc R . . C57 C 0.2477(7) 0.19379(17) 0.3503(3) 0.0418(15) Uani 1 1 d . . . H57A H 0.3432 0.1914 0.3520 0.050 Uiso 1 1 calc R . . H57B H 0.2308 0.2140 0.3691 0.050 Uiso 1 1 calc R . . C58 C 0.1952(9) 0.1663(2) 0.3809(3) 0.059(2) Uani 1 1 d . . . H58A H 0.2374 0.1662 0.4193 0.088 Uiso 1 1 calc R . . H58B H 0.2135 0.1462 0.3631 0.088 Uiso 1 1 calc R . . H58C H 0.1009 0.1688 0.3801 0.088 Uiso 1 1 calc R . . C72 C 1.1759(8) 0.0855(2) 0.2808(4) 0.063(2) Uani 1 1 d . . . H72A H 1.1760 0.0813 0.2409 0.075 Uiso 1 1 calc R . . H72B H 1.1430 0.1074 0.2848 0.075 Uiso 1 1 calc R . . C68 C 0.7272(10) 0.0347(2) 0.2802(5) 0.077(3) Uani 1 1 d . . . H68A H 0.7199 0.0280 0.2410 0.093 Uiso 1 1 calc R . . H68B H 0.6820 0.0554 0.2818 0.093 Uiso 1 1 calc R . . C73 C 1.3114(10) 0.0833(3) 0.3094(4) 0.077(3) Uani 1 1 d . . . H73A H 1.3136 0.0902 0.3483 0.092 Uiso 1 1 calc R . . H73B H 1.3409 0.0609 0.3096 0.092 Uiso 1 1 calc R . . C64 C 0.8764(10) 0.1086(2) 0.3339(4) 0.068(3) Uani 1 1 d . . . H64A H 0.9646 0.1085 0.3554 0.082 Uiso 1 1 calc R . . H64B H 0.8199 0.0946 0.3531 0.082 Uiso 1 1 calc R . . C65 C 0.8213(9) 0.1432(2) 0.3317(5) 0.072(3) Uani 1 1 d . . . H65A H 0.8781 0.1571 0.3125 0.087 Uiso 1 1 calc R . . H65B H 0.7335 0.1432 0.3098 0.087 Uiso 1 1 calc R . . C61 C 0.9565(10) 0.0162(3) 0.1397(4) 0.072(3) Uani 1 1 d . . . H61A H 0.8614 0.0123 0.1339 0.087 Uiso 1 1 calc R . . H61B H 0.9742 0.0348 0.1169 0.087 Uiso 1 1 calc R . . C66 C 0.8120(11) 0.1569(2) 0.3883(6) 0.094(4) Uani 1 1 d . . . H66A H 0.7745 0.1783 0.3844 0.141 Uiso 1 1 calc R . . H66B H 0.8992 0.1580 0.4096 0.141 Uiso 1 1 calc R . . H66C H 0.7563 0.1432 0.4077 0.141 Uiso 1 1 calc R . . C74 C 1.4014(11) 0.1034(3) 0.2821(4) 0.092(4) Uani 1 1 d . . . H74A H 1.4901 0.1012 0.3016 0.137 Uiso 1 1 calc R . . H74B H 1.3741 0.1257 0.2830 0.137 Uiso 1 1 calc R . . H74C H 1.3996 0.0965 0.2436 0.137 Uiso 1 1 calc R . . C62 C 1.0210(14) -0.0108(3) 0.1217(6) 0.107(4) Uani 1 1 d . . . H62A H 0.9900 -0.0148 0.0826 0.160 Uiso 1 1 calc R . . H62B H 1.0024 -0.0294 0.1435 0.160 Uiso 1 1 calc R . . H62C H 1.1152 -0.0069 0.1264 0.160 Uiso 1 1 calc R . . N9 N 0.9223(7) 0.12375(14) 0.7610(2) 0.0478(15) Uani 1 1 d . . . C76 C 1.1088(10) 0.0842(2) 0.7821(4) 0.068(3) Uani 1 1 d . . . H76A H 1.1476 0.0889 0.7481 0.081 Uiso 1 1 calc R . . H76B H 1.0478 0.0660 0.7744 0.081 Uiso 1 1 calc R . . C75 C 1.0384(12) 0.1128(2) 0.7998(4) 0.086(4) Uani 1 1 d . . . H75A H 1.1012 0.1307 0.8056 0.104 Uiso 1 1 calc R . . H75B H 1.0096 0.1080 0.8360 0.104 Uiso 1 1 calc R . . C69 C 0.6636(13) 0.0098(3) 0.3135(5) 0.099(4) Uani 1 1 d D . . H69A H 0.7114 -0.0106 0.3142 0.118 Uiso 1 1 calc R . . H69B H 0.6633 0.0172 0.3520 0.118 Uiso 1 1 calc R . . C77 C 1.2173(14) 0.0758(3) 0.8304(5) 0.107(5) Uani 1 1 d . . . H77A H 1.2786 0.0939 0.8369 0.128 Uiso 1 1 calc R . . H77B H 1.1775 0.0723 0.8645 0.128 Uiso 1 1 calc R . . C70 C 0.5435(17) 0.0064(5) 0.2885(8) 0.177(8) Uani 1 1 d DU . . H70A H 0.4967 -0.0087 0.3091 0.266 Uiso 1 1 calc R . . H70B H 0.5456 -0.0016 0.2509 0.266 Uiso 1 1 calc R . . H70C H 0.4990 0.0271 0.2867 0.266 Uiso 1 1 calc R . . C83 C 0.8753(8) 0.1538(2) 0.7883(3) 0.0526(19) Uani 1 1 d . . . H83A H 0.8805 0.1498 0.8285 0.063 Uiso 1 1 calc R . . H83B H 0.9365 0.1714 0.7833 0.063 Uiso 1 1 calc R . . C84 C 0.7444(8) 0.1645(2) 0.7681(3) 0.057(2) Uani 1 1 d . . . H84A H 0.6807 0.1480 0.7756 0.069 Uiso 1 1 calc R . . H84B H 0.7358 0.1679 0.7276 0.069 Uiso 1 1 calc R . . C79 C 0.8203(10) 0.0979(2) 0.7498(4) 0.071(3) Uani 1 1 d . . . H79A H 0.7480 0.1070 0.7238 0.086 Uiso 1 1 calc R . . H79B H 0.8594 0.0807 0.7296 0.086 Uiso 1 1 calc R . . C80 C 0.7618(12) 0.0826(3) 0.7941(5) 0.097(4) Uani 1 1 d . . . H80A H 0.7275 0.0991 0.8174 0.116 Uiso 1 1 calc R . . H80B H 0.8288 0.0702 0.8178 0.116 Uiso 1 1 calc R . . C82 C 0.536(2) 0.0856(5) 0.7379(10) 0.221(11) Uani 1 1 d DU . . H82A H 0.4597 0.0735 0.7212 0.332 Uiso 1 1 calc R . . H82B H 0.5729 0.0974 0.7091 0.332 Uiso 1 1 calc R . . H82C H 0.5097 0.1006 0.7651 0.332 Uiso 1 1 calc R . . C78 C 1.2921(13) 0.0459(4) 0.8175(6) 0.119(5) Uani 1 1 d . . . H78A H 1.3578 0.0409 0.8490 0.179 Uiso 1 1 calc R . . H78B H 1.3351 0.0497 0.7847 0.179 Uiso 1 1 calc R . . H78C H 1.2313 0.0280 0.8104 0.179 Uiso 1 1 calc R . . N7 N 0.2122(5) 0.22765(12) 0.20113(19) 0.0275(10) Uani 1 1 d . . . N8 N 0.9418(7) 0.06249(19) 0.2744(3) 0.0574(19) Uani 1 1 d . . . C86 C 0.5887(7) 0.20981(19) 0.7692(3) 0.0479(18) Uani 1 1 d . . . H86A H 0.5682 0.2297 0.7873 0.072 Uiso 1 1 calc R . . H86B H 0.5189 0.1943 0.7715 0.072 Uiso 1 1 calc R . . H86C H 0.5966 0.2140 0.7304 0.072 Uiso 1 1 calc R . . C85 C 0.7146(8) 0.19670(17) 0.7976(3) 0.0480(17) Uani 1 1 d . . . H85A H 0.7080 0.1927 0.8371 0.058 Uiso 1 1 calc R . . H85B H 0.7859 0.2122 0.7953 0.058 Uiso 1 1 calc R . . C89 C 0.9536(11) 0.1551(2) 0.6137(3) 0.077(3) Uani 1 1 d . . . H89A H 0.9592 0.1337 0.5971 0.092 Uiso 1 1 calc R . . H89B H 1.0430 0.1639 0.6208 0.092 Uiso 1 1 calc R . . C87 C 0.9582(17) 0.1326(2) 0.7070(4) 0.113(6) Uani 1 1 d . . . H87A H 1.0479 0.1410 0.7155 0.136 Uiso 1 1 calc R . . H87B H 0.9667 0.1120 0.6881 0.136 Uiso 1 1 calc R . . C88 C 0.901(2) 0.1518(2) 0.6671(4) 0.163(9) Uani 1 1 d . . . H88A H 0.8993 0.1735 0.6832 0.195 Uiso 1 1 calc R . . H88B H 0.8093 0.1448 0.6584 0.195 Uiso 1 1 calc R . . C81 C 0.6492(14) 0.0602(6) 0.7696(7) 0.189(11) Uani 1 1 d D . . H81A H 0.6144 0.0481 0.7991 0.227 Uiso 1 1 calc R . . H81B H 0.6789 0.0451 0.7428 0.227 Uiso 1 1 calc R . . C90 C 0.8707(3) 0.17649(7) 0.57275(11) 0.144(7) Uani 1 1 d . . . H90A H 0.9117 0.1785 0.5391 0.216 Uiso 1 1 calc R . . H90B H 0.8631 0.1976 0.5892 0.216 Uiso 1 1 calc R . . H90C H 0.7837 0.1671 0.5636 0.216 Uiso 1 1 calc R . . O16 O 0.0554(3) 0.13931(7) 0.18926(11) 0.0383(10) Uani 1 1 d RD . . H161 H 0.0982 0.1303 0.1780 0.04(2) Uiso 1 1 d RD . . H162 H -0.0007 0.1521 0.1684 0.10(4) Uiso 1 1 d RD . . O17 O 0.1938(3) 0.18564(7) 0.77980(11) 0.0470(13) Uani 1 1 d RD . . H171 H 0.1520 0.1811 0.7797 0.17(7) Uiso 1 1 d RD . . H172 H 0.2251 0.1948 0.7822 0.23(9) Uiso 1 1 d RD . . O18 O 0.9480(3) 0.03172(7) 0.69340(11) 0.0432(11) Uani 1 1 d R . . H18A H 0.9631 0.0456 0.6823 0.06(3) Uiso 1 1 d R . . H18B H 0.8730 0.0282 0.6747 0.11(4) Uiso 1 1 d 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 0.01650(18) 0.01911(18) 0.01898(18) -0.00022(14) 0.00365(13) 0.00221(14) N1 0.025(2) 0.028(2) 0.030(2) 0.003(2) 0.0041(19) 0.0015(19) C1 0.026(3) 0.026(3) 0.038(3) 0.007(2) 0.005(2) 0.004(2) C2 0.039(4) 0.041(4) 0.052(4) 0.015(3) 0.011(3) 0.018(3) C3 0.027(3) 0.029(3) 0.053(4) -0.003(3) 0.009(3) 0.008(2) C4 0.017(2) 0.026(3) 0.034(3) -0.005(2) 0.006(2) -0.003(2) O1 0.040(3) 0.048(3) 0.031(2) 0.014(2) 0.0072(19) 0.014(2) O2 0.032(2) 0.030(2) 0.028(2) -0.0085(17) 0.0086(17) -0.0004(17) C5 0.019(2) 0.030(3) 0.027(3) -0.001(2) 0.005(2) 0.007(2) C6 0.021(3) 0.030(3) 0.038(3) 0.001(2) 0.003(2) 0.007(2) C7 0.024(3) 0.030(3) 0.054(4) 0.014(3) 0.010(3) 0.001(2) C8 0.019(3) 0.025(3) 0.069(5) -0.003(3) 0.005(3) -0.001(2) C9 0.026(3) 0.031(3) 0.046(4) -0.013(3) 0.001(3) 0.006(2) C10 0.020(3) 0.028(3) 0.038(3) -0.002(2) 0.006(2) 0.003(2) F1 0.0320(18) 0.040(2) 0.0341(19) 0.0090(15) 0.0063(15) 0.0001(15) F2 0.034(2) 0.044(2) 0.072(3) 0.019(2) 0.016(2) -0.0058(17) F3 0.030(2) 0.034(2) 0.099(4) -0.009(2) 0.006(2) -0.0126(16) F4 0.034(2) 0.046(2) 0.057(3) -0.025(2) -0.0055(18) 0.0004(17) F5 0.0298(18) 0.041(2) 0.0316(18) -0.0077(15) 0.0044(14) -0.0008(15) N2 0.020(2) 0.021(2) 0.027(2) -0.0013(18) 0.0065(17) 0.0047(17) C11 0.016(2) 0.022(3) 0.036(3) -0.001(2) 0.005(2) 0.0003(19) C12 0.023(3) 0.030(3) 0.044(3) 0.002(3) 0.007(2) 0.007(2) C13 0.025(3) 0.032(3) 0.040(3) -0.003(3) 0.010(2) 0.005(2) C14 0.027(3) 0.024(3) 0.032(3) -0.003(2) 0.010(2) -0.001(2) O3 0.029(2) 0.042(2) 0.028(2) 0.0008(18) 0.0030(17) 0.0084(18) O4 0.048(3) 0.045(3) 0.030(2) 0.005(2) 0.016(2) 0.010(2) O5 0.023(2) 0.023(2) 0.0250(19) -0.0012(16) 0.0042(16) 0.0011(16) Pd2 0.01759(18) 0.02242(19) 0.02028(19) -0.00078(15) 0.00298(14) 0.00049(14) N3 0.021(2) 0.032(2) 0.020(2) -0.0049(18) 0.0015(17) -0.0019(18) C15 0.020(2) 0.029(3) 0.029(3) -0.001(2) 0.001(2) -0.006(2) C16 0.029(3) 0.020(3) 0.049(4) 0.003(2) -0.001(3) -0.003(2) C17 0.035(3) 0.035(3) 0.036(3) -0.007(3) 0.000(3) 0.013(3) C18 0.024(3) 0.026(3) 0.031(3) -0.003(2) 0.002(2) -0.004(2) O6 0.0200(19) 0.053(3) 0.027(2) -0.0009(19) 0.0035(16) 0.0040(18) O7 0.038(2) 0.040(2) 0.029(2) -0.0051(18) 0.0008(18) 0.0077(19) C19 0.020(3) 0.022(3) 0.050(4) -0.002(2) 0.002(2) 0.002(2) C20 0.026(3) 0.026(3) 0.049(4) 0.008(3) -0.003(3) -0.001(2) C21 0.023(3) 0.033(3) 0.076(5) 0.014(3) 0.004(3) 0.002(3) C22 0.029(4) 0.026(3) 0.138(9) -0.020(4) 0.016(5) -0.005(3) C23 0.048(5) 0.076(7) 0.153(11) -0.088(7) 0.030(6) -0.027(5) C24 0.034(4) 0.067(5) 0.095(7) -0.054(5) 0.029(4) -0.016(4) F6 0.043(2) 0.086(3) 0.038(2) -0.001(2) 0.0098(18) -0.029(2) F7 0.039(2) 0.082(4) 0.094(4) 0.038(3) 0.009(2) -0.022(2) F8 0.037(3) 0.038(3) 0.232(8) -0.046(4) 0.036(4) -0.018(2) F9 0.096(5) 0.229(10) 0.282(11) -0.228(10) 0.108(7) -0.107(6) F10 0.069(4) 0.166(7) 0.110(5) -0.105(5) 0.052(3) -0.062(4) N4 0.023(2) 0.028(2) 0.028(2) 0.0044(19) 0.0052(18) 0.0017(18) C25 0.029(3) 0.039(3) 0.042(4) 0.010(3) 0.006(3) 0.004(3) C26 0.039(4) 0.054(4) 0.054(4) 0.021(4) 0.011(3) 0.020(3) C27 0.047(4) 0.036(4) 0.064(5) 0.018(3) 0.024(4) 0.017(3) C28 0.030(3) 0.025(3) 0.042(3) 0.003(2) 0.014(3) 0.000(2) O8 0.051(3) 0.059(3) 0.031(2) 0.015(2) 0.009(2) 0.017(2) O9 0.042(2) 0.027(2) 0.035(2) 0.0025(17) 0.0158(19) 0.0069(18) O10 0.019(2) 0.027(2) 0.027(2) 0.0012(16) 0.0061(16) -0.0003(16) Pd3 0.01968(19) 0.02113(19) 0.0249(2) -0.00002(15) 0.00770(15) -0.00340(15) N5 0.021(2) 0.020(2) 0.033(2) -0.0030(18) 0.0057(18) -0.0061(17) C29 0.028(3) 0.020(3) 0.046(4) 0.003(2) 0.015(3) -0.001(2) C30 0.042(4) 0.029(3) 0.066(5) -0.002(3) 0.023(3) -0.015(3) C31 0.068(5) 0.060(5) 0.066(5) -0.027(4) 0.021(4) -0.043(4) C32 0.052(4) 0.042(4) 0.057(5) -0.020(3) 0.016(4) -0.023(3) O11 0.039(2) 0.033(2) 0.035(2) 0.0056(18) 0.0089(19) -0.0122(19) O12 0.091(5) 0.079(4) 0.039(3) -0.028(3) 0.018(3) -0.045(4) C33 0.022(3) 0.022(3) 0.050(4) -0.001(2) 0.011(2) -0.002(2) C34 0.022(3) 0.028(3) 0.042(3) 0.001(2) 0.008(2) -0.003(2) C35 0.028(3) 0.031(3) 0.058(4) 0.015(3) -0.001(3) -0.009(2) C36 0.029(3) 0.024(3) 0.097(6) 0.005(4) 0.021(4) 0.001(3) C37 0.053(5) 0.043(4) 0.070(6) -0.003(4) 0.030(4) 0.008(3) C38 0.042(4) 0.033(3) 0.061(5) -0.002(3) 0.022(3) 0.002(3) F11 0.037(2) 0.047(2) 0.036(2) 0.0054(17) 0.0016(16) -0.0005(17) F12 0.032(2) 0.052(3) 0.075(3) 0.024(2) -0.013(2) -0.0015(18) F13 0.038(2) 0.038(2) 0.130(5) 0.015(3) 0.014(3) 0.0134(19) F14 0.081(4) 0.065(3) 0.111(5) -0.011(3) 0.042(3) 0.032(3) F15 0.078(3) 0.065(3) 0.048(3) -0.010(2) 0.022(2) 0.023(3) N6 0.017(2) 0.023(2) 0.033(2) 0.0059(19) 0.0065(18) -0.0005(17) C39 0.031(3) 0.035(3) 0.040(4) 0.019(3) 0.006(3) -0.002(3) C40 0.028(3) 0.048(4) 0.056(4) 0.020(3) 0.004(3) -0.012(3) C41 0.024(3) 0.021(3) 0.062(4) 0.000(3) 0.009(3) -0.006(2) C42 0.016(2) 0.027(3) 0.046(4) 0.001(2) 0.005(2) 0.002(2) O13 0.040(3) 0.086(4) 0.037(3) 0.011(3) 0.011(2) -0.018(3) O14 0.026(2) 0.039(2) 0.047(3) -0.012(2) 0.0122(19) -0.0074(18) O15 0.024(2) 0.026(2) 0.027(2) 0.0004(16) 0.0067(16) -0.0018(16) C51 0.024(3) 0.037(3) 0.026(3) -0.012(2) 0.001(2) -0.003(2) C48 0.041(3) 0.030(3) 0.032(3) -0.007(2) 0.005(3) -0.003(3) C43 0.028(3) 0.030(3) 0.028(3) -0.010(2) 0.004(2) -0.006(2) C47 0.023(3) 0.034(3) 0.033(3) -0.009(2) 0.002(2) -0.009(2) C44 0.029(3) 0.045(4) 0.039(3) -0.011(3) -0.003(3) 0.002(3) C45 0.035(3) 0.039(4) 0.040(4) -0.008(3) 0.005(3) 0.001(3) C46 0.034(4) 0.058(5) 0.064(5) -0.014(4) 0.002(3) 0.007(3) C52 0.027(3) 0.038(3) 0.029(3) -0.014(2) 0.007(2) -0.003(2) C49 0.039(4) 0.032(3) 0.050(4) -0.002(3) 0.012(3) 0.002(3) C50 0.057(5) 0.041(4) 0.055(5) 0.008(3) 0.021(4) 0.011(3) C53 0.030(3) 0.059(5) 0.059(5) -0.034(4) 0.001(3) 0.003(3) C54 0.038(4) 0.069(6) 0.125(9) -0.042(6) 0.040(5) -0.018(4) C55 0.032(3) 0.034(3) 0.024(3) -0.009(2) 0.004(2) -0.004(2) C56 0.039(4) 0.042(4) 0.034(3) -0.009(3) 0.003(3) -0.009(3) C63 0.046(4) 0.050(5) 0.078(6) 0.038(4) 0.005(4) 0.008(4) C59 0.062(5) 0.088(6) 0.030(4) 0.020(4) 0.011(3) 0.021(5) C71 0.068(5) 0.097(7) 0.026(3) 0.025(4) 0.012(3) 0.035(5) C67 0.084(6) 0.053(5) 0.057(5) 0.027(4) 0.039(5) 0.026(4) C60 0.058(5) 0.102(7) 0.034(4) 0.014(4) 0.012(4) 0.021(5) C57 0.044(4) 0.044(4) 0.036(3) 0.000(3) 0.000(3) -0.006(3) C58 0.069(6) 0.063(5) 0.042(4) 0.008(4) 0.001(4) -0.021(4) C72 0.052(5) 0.089(7) 0.049(5) 0.022(4) 0.013(4) 0.020(5) C68 0.085(7) 0.046(5) 0.109(8) 0.013(5) 0.043(6) 0.015(5) C73 0.072(6) 0.118(9) 0.038(4) 0.013(5) -0.005(4) 0.027(6) C64 0.075(6) 0.053(5) 0.085(7) 0.031(5) 0.039(5) 0.012(4) C65 0.044(5) 0.054(5) 0.113(9) 0.016(5) -0.010(5) -0.009(4) C61 0.079(7) 0.091(7) 0.050(5) 0.011(5) 0.017(5) 0.033(6) C66 0.089(8) 0.040(5) 0.168(12) -0.011(6) 0.073(8) -0.016(5) C74 0.082(8) 0.130(11) 0.057(6) 0.022(6) -0.010(5) 0.002(7) C62 0.139(12) 0.086(9) 0.102(10) -0.008(7) 0.042(9) 0.007(8) N9 0.078(5) 0.037(3) 0.027(3) -0.007(2) 0.004(3) 0.011(3) C76 0.078(6) 0.053(5) 0.062(5) -0.017(4) -0.027(5) -0.003(4) C75 0.121(9) 0.056(5) 0.067(6) -0.026(5) -0.045(6) 0.027(6) C69 0.123(10) 0.099(9) 0.077(7) -0.035(7) 0.026(7) -0.062(8) C77 0.130(11) 0.102(10) 0.077(8) -0.011(7) -0.030(8) -0.032(9) C70 0.174(11) 0.186(11) 0.182(11) -0.015(9) 0.056(9) -0.004(9) C83 0.061(5) 0.056(5) 0.040(4) -0.008(3) 0.003(3) 0.007(4) C84 0.050(5) 0.076(6) 0.047(4) -0.008(4) 0.015(4) 0.004(4) C79 0.069(6) 0.066(6) 0.086(7) 0.003(5) 0.034(5) 0.019(5) C80 0.095(9) 0.127(11) 0.076(7) 0.017(7) 0.041(7) 0.051(8) C82 0.210(13) 0.230(14) 0.226(14) 0.008(9) 0.035(9) -0.017(9) C78 0.090(9) 0.170(16) 0.092(10) -0.011(10) -0.007(7) 0.024(10) N7 0.027(2) 0.031(3) 0.024(2) -0.0104(19) 0.0022(19) -0.0051(19) N8 0.055(4) 0.082(5) 0.037(3) 0.026(3) 0.015(3) 0.017(4) C86 0.036(4) 0.056(5) 0.056(4) 0.013(4) 0.021(3) 0.002(3) C85 0.049(4) 0.037(4) 0.057(5) 0.012(3) 0.004(3) 0.003(3) C89 0.120(9) 0.069(6) 0.037(4) 0.015(4) -0.005(5) -0.030(6) C87 0.256(18) 0.051(6) 0.037(5) 0.017(4) 0.040(7) 0.026(8) C88 0.42(3) 0.038(5) 0.037(5) 0.004(4) 0.054(10) 0.017(10) C81 0.075(9) 0.40(3) 0.096(11) 0.078(16) 0.009(8) -0.052(15) C90 0.211(18) 0.060(7) 0.138(13) 0.017(8) -0.062(12) -0.012(9) O16 0.044(3) 0.038(2) 0.031(2) 0.003(2) -0.002(2) -0.002(2) O17 0.061(3) 0.050(3) 0.030(2) 0.002(2) 0.005(2) 0.009(3) O18 0.046(3) 0.051(3) 0.032(2) -0.004(2) 0.005(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C5 1.985(6) . ? Pd1 N2 2.016(4) . ? Pd1 N1 2.039(5) . ? Pd1 O5 2.122(4) . ? N1 C1 1.358(7) . ? N1 C4 1.380(7) . ? C1 O1 1.226(7) . ? C1 C2 1.525(8) . ? C2 C3 1.516(10) . ? C3 C4 1.524(8) . ? C4 O2 1.224(7) . ? C5 C10 1.376(8) . ? C5 C6 1.389(8) . ? C6 F1 1.348(7) . ? C6 C7 1.383(9) . ? C7 F2 1.352(7) . ? C7 C8 1.382(10) . ? C8 F3 1.347(7) . ? C8 C9 1.370(10) . ? C9 F4 1.347(7) . ? C9 C10 1.384(8) . ? C10 F5 1.351(7) . ? N2 C11 1.362(7) . ? N2 C14 1.370(7) . ? C11 O3 1.221(7) . ? C11 C12 1.518(7) . ? C12 C13 1.523(9) . ? C13 C14 1.520(8) . ? C14 O4 1.212(7) . ? Pd2 C19 1.977(6) . ? Pd2 N4 2.008(5) . ? Pd2 N3 2.015(5) . ? Pd2 O10 2.109(4) . ? N3 C15 1.347(7) . ? N3 C18 1.389(7) . ? C15 O6 1.228(7) . ? C15 C16 1.526(8) . ? C16 C17 1.508(9) . ? C17 C18 1.523(8) . ? C18 O7 1.213(7) . ? C19 C20 1.367(9) . ? C19 C24 1.374(10) . ? C20 F6 1.342(8) . ? C20 C21 1.395(9) . ? C21 F7 1.343(9) . ? C21 C22 1.349(12) . ? C22 F8 1.345(8) . ? C22 C23 1.379(15) . ? C23 F9 1.350(11) . ? C23 C24 1.384(11) . ? C24 F10 1.357(10) . ? N4 C28 1.362(7) . ? N4 C25 1.368(8) . ? C25 O8 1.222(8) . ? C25 C26 1.522(9) . ? C26 C27 1.512(10) . ? C27 C28 1.522(9) . ? C28 O9 1.222(7) . ? Pd3 C33 1.988(6) . ? Pd3 N5 2.014(4) . ? Pd3 N6 2.018(4) . ? Pd3 O15 2.112(4) . ? N5 C29 1.366(7) . ? N5 C32 1.376(8) . ? C29 O11 1.211(8) . ? C29 C30 1.527(8) . ? C30 C31 1.520(12) . ? C31 C32 1.526(10) . ? C32 O12 1.212(9) . ? C33 C34 1.360(9) . ? C33 C38 1.384(9) . ? C34 F11 1.356(7) . ? C34 C35 1.397(9) . ? C35 F12 1.339(8) . ? C35 C36 1.384(11) . ? C36 F13 1.352(8) . ? C36 C37 1.367(12) . ? C37 F14 1.353(9) . ? C37 C38 1.382(10) . ? C38 F15 1.340(9) . ? N6 C42 1.362(8) . ? N6 C39 1.380(7) . ? C39 O13 1.206(8) . ? C39 C40 1.525(9) . ? C40 C41 1.530(10) . ? C41 C42 1.519(8) . ? C42 O14 1.223(7) . ? C51 C52 1.519(8) . ? C51 N7 1.524(7) . ? C48 C47 1.519(9) . ? C48 C49 1.528(9) . ? C43 C44 1.503(8) . ? C43 N7 1.532(7) . ? C47 N7 1.518(7) . ? C44 C45 1.529(9) . ? C45 C46 1.517(9) . ? C52 C53 1.519(8) . ? C49 C50 1.524(10) . ? C53 C54 1.541(13) . ? C55 N7 1.515(7) . ? C55 C56 1.516(9) . ? C56 C57 1.542(9) . ? C63 C64 1.505(13) . ? C63 N8 1.518(10) . ? C59 C60 1.483(12) . ? C59 N8 1.503(10) . ? C71 N8 1.531(11) . ? C71 C72 1.559(13) . ? C67 C68 1.475(14) . ? C67 N8 1.520(10) . ? C60 C61 1.547(12) . ? C57 C58 1.514(10) . ? C72 C73 1.484(12) . ? C68 C69 1.525(14) . ? C73 C74 1.480(15) . ? C64 C65 1.558(12) . ? C65 C66 1.513(15) . ? C61 C62 1.417(14) . ? N9 C87 1.465(11) . ? N9 C75 1.499(11) . ? N9 C79 1.513(12) . ? N9 C83 1.537(9) . ? C76 C75 1.500(13) . ? C76 C77 1.555(14) . ? C69 C70 1.317(15) . ? C77 C78 1.529(18) . ? C83 C84 1.450(11) . ? C84 C85 1.580(11) . ? C79 C80 1.460(14) . ? C80 C81 1.55(2) . ? C82 C81 1.693(17) . ? C86 C85 1.496(10) . ? C89 C88 1.485(15) . ? C89 C90 1.522(10) . ? C87 C88 1.340(16) . ? 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 C5 Pd1 N2 89.6(2) . . ? C5 Pd1 N1 89.9(2) . . ? N2 Pd1 N1 179.4(2) . . ? C5 Pd1 O5 177.26(19) . . ? N2 Pd1 O5 87.73(17) . . ? N1 Pd1 O5 92.72(18) . . ? C1 N1 C4 111.0(5) . . ? C1 N1 Pd1 123.7(4) . . ? C4 N1 Pd1 124.9(4) . . ? O1 C1 N1 125.0(5) . . ? O1 C1 C2 124.3(6) . . ? N1 C1 C2 110.6(5) . . ? C3 C2 C1 103.5(5) . . ? C2 C3 C4 104.0(5) . . ? O2 C4 N1 125.8(5) . . ? O2 C4 C3 124.5(5) . . ? N1 C4 C3 109.7(5) . . ? C10 C5 C6 114.8(5) . . ? C10 C5 Pd1 122.9(4) . . ? C6 C5 Pd1 122.3(4) . . ? F1 C6 C7 116.5(6) . . ? F1 C6 C5 120.1(5) . . ? C7 C6 C5 123.4(6) . . ? F2 C7 C8 119.8(6) . . ? F2 C7 C6 120.8(6) . . ? C8 C7 C6 119.4(6) . . ? F3 C8 C9 121.0(7) . . ? F3 C8 C7 120.0(6) . . ? C9 C8 C7 119.1(6) . . ? F4 C9 C8 119.3(6) . . ? F4 C9 C10 120.8(6) . . ? C8 C9 C10 119.8(6) . . ? F5 C10 C5 120.6(5) . . ? F5 C10 C9 115.9(5) . . ? C5 C10 C9 123.5(6) . . ? C11 N2 C14 111.6(4) . . ? C11 N2 Pd1 122.8(4) . . ? C14 N2 Pd1 125.6(4) . . ? O3 C11 N2 125.7(5) . . ? O3 C11 C12 124.0(5) . . ? N2 C11 C12 110.3(5) . . ? C11 C12 C13 103.9(5) . . ? C14 C13 C12 104.1(5) . . ? O4 C14 N2 125.8(5) . . ? O4 C14 C13 124.3(5) . . ? N2 C14 C13 109.9(5) . . ? C19 Pd2 N4 90.3(2) . . ? C19 Pd2 N3 89.1(2) . . ? N4 Pd2 N3 177.61(19) . . ? C19 Pd2 O10 176.7(2) . . ? N4 Pd2 O10 88.83(18) . . ? N3 Pd2 O10 91.92(18) . . ? C15 N3 C18 111.0(5) . . ? C15 N3 Pd2 124.5(4) . . ? C18 N3 Pd2 124.5(4) . . ? O6 C15 N3 125.1(5) . . ? O6 C15 C16 123.7(5) . . ? N3 C15 C16 111.1(5) . . ? C17 C16 C15 103.7(5) . . ? C16 C17 C18 104.7(5) . . ? O7 C18 N3 126.0(5) . . ? O7 C18 C17 124.6(5) . . ? N3 C18 C17 109.4(5) . . ? C20 C19 C24 114.3(6) . . ? C20 C19 Pd2 122.7(5) . . ? C24 C19 Pd2 123.0(5) . . ? F6 C20 C19 119.8(5) . . ? F6 C20 C21 115.8(6) . . ? C19 C20 C21 124.4(7) . . ? F7 C21 C22 120.2(7) . . ? F7 C21 C20 120.7(7) . . ? C22 C21 C20 119.1(7) . . ? F8 C22 C21 120.8(9) . . ? F8 C22 C23 120.2(9) . . ? C21 C22 C23 118.9(7) . . ? F9 C23 C22 119.3(8) . . ? F9 C23 C24 120.8(10) . . ? C22 C23 C24 119.9(8) . . ? F10 C24 C19 120.1(7) . . ? F10 C24 C23 116.7(8) . . ? C19 C24 C23 123.2(8) . . ? C28 N4 C25 110.8(5) . . ? C28 N4 Pd2 124.9(4) . . ? C25 N4 Pd2 124.3(4) . . ? O8 C25 N4 125.1(6) . . ? O8 C25 C26 123.9(6) . . ? N4 C25 C26 111.0(6) . . ? C27 C26 C25 103.3(5) . . ? C26 C27 C28 104.6(5) . . ? O9 C28 N4 125.1(5) . . ? O9 C28 C27 124.7(6) . . ? N4 C28 C27 110.2(5) . . ? C33 Pd3 N5 89.4(2) . . ? C33 Pd3 N6 89.5(2) . . ? N5 Pd3 N6 178.2(2) . . ? C33 Pd3 O15 177.9(2) . . ? N5 Pd3 O15 90.34(18) . . ? N6 Pd3 O15 90.75(18) . . ? C29 N5 C32 110.5(5) . . ? C29 N5 Pd3 125.0(4) . . ? C32 N5 Pd3 124.4(4) . . ? O11 C29 N5 125.5(5) . . ? O11 C29 C30 124.5(6) . . ? N5 C29 C30 110.0(5) . . ? C31 C30 C29 103.2(5) . . ? C30 C31 C32 103.3(6) . . ? O12 C32 N5 125.4(6) . . ? O12 C32 C31 124.3(7) . . ? N5 C32 C31 110.3(6) . . ? C34 C33 C38 115.9(6) . . ? C34 C33 Pd3 123.2(5) . . ? C38 C33 Pd3 120.9(5) . . ? F11 C34 C33 121.2(5) . . ? F11 C34 C35 115.5(6) . . ? C33 C34 C35 123.3(6) . . ? F12 C35 C36 120.2(6) . . ? F12 C35 C34 120.9(7) . . ? C36 C35 C34 118.9(7) . . ? F13 C36 C37 121.0(7) . . ? F13 C36 C35 119.8(8) . . ? C37 C36 C35 119.2(6) . . ? F14 C37 C36 118.7(7) . . ? F14 C37 C38 121.4(8) . . ? C36 C37 C38 119.9(7) . . ? F15 C38 C33 121.4(6) . . ? F15 C38 C37 115.9(7) . . ? C33 C38 C37 122.8(8) . . ? C42 N6 C39 110.8(5) . . ? C42 N6 Pd3 123.7(4) . . ? C39 N6 Pd3 125.5(4) . . ? O13 C39 N6 124.8(6) . . ? O13 C39 C40 125.1(6) . . ? N6 C39 C40 110.1(6) . . ? C39 C40 C41 104.1(5) . . ? C42 C41 C40 103.4(5) . . ? O14 C42 N6 126.1(5) . . ? O14 C42 C41 122.5(6) . . ? N6 C42 C41 111.4(5) . . ? C52 C51 N7 115.1(4) . . ? C47 C48 C49 110.3(5) . . ? C44 C43 N7 116.8(5) . . ? N7 C47 C48 115.9(5) . . ? C43 C44 C45 108.6(5) . . ? C46 C45 C44 113.9(6) . . ? C53 C52 C51 110.2(5) . . ? C50 C49 C48 112.1(6) . . ? C52 C53 C54 112.7(7) . . ? N7 C55 C56 116.1(5) . . ? C55 C56 C57 108.8(5) . . ? C64 C63 N8 116.1(6) . . ? C60 C59 N8 115.6(6) . . ? N8 C71 C72 114.2(6) . . ? C68 C67 N8 115.4(7) . . ? C59 C60 C61 108.6(7) . . ? C58 C57 C56 113.3(6) . . ? C73 C72 C71 112.8(7) . . ? C67 C68 C69 109.3(9) . . ? C74 C73 C72 111.5(8) . . ? C63 C64 C65 111.7(8) . . ? C66 C65 C64 113.0(9) . . ? C62 C61 C60 113.2(9) . . ? C87 N9 C75 111.6(10) . . ? C87 N9 C79 105.9(8) . . ? C75 N9 C79 112.1(7) . . ? C87 N9 C83 108.4(6) . . ? C75 N9 C83 104.6(6) . . ? C79 N9 C83 114.4(7) . . ? C75 C76 C77 106.9(8) . . ? C76 C75 N9 116.3(7) . . ? C70 C69 C68 106.0(15) . . ? C78 C77 C76 111.3(10) . . ? C84 C83 N9 116.3(7) . . ? C83 C84 C85 109.9(7) . . ? C80 C79 N9 122.0(10) . . ? C79 C80 C81 110.2(11) . . ? C55 N7 C47 106.1(4) . . ? C55 N7 C51 111.1(4) . . ? C47 N7 C51 111.4(5) . . ? C55 N7 C43 111.1(5) . . ? C47 N7 C43 111.5(4) . . ? C51 N7 C43 105.7(4) . . ? C59 N8 C63 106.0(6) . . ? C59 N8 C67 111.1(7) . . ? C63 N8 C67 111.4(6) . . ? C59 N8 C71 110.9(6) . . ? C63 N8 C71 111.3(7) . . ? C67 N8 C71 106.3(6) . . ? C86 C85 C84 108.4(7) . . ? C88 C89 C90 113.0(10) . . ? C88 C87 N9 131.8(14) . . ? C87 C88 C89 121.0(15) . . ? C80 C81 C82 103.4(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O6 0.84(7) 1.91(7) 2.729(6) 166(6) 1_556 O5 H5B O9 0.79(7) 1.96(8) 2.750(6) 174(7) 1_556 O10 H10A O2 0.77(7) 1.96(8) 2.727(6) 176(7) 1_554 O10 H10B O3 0.72(8) 2.05(8) 2.760(6) 171(8) 1_554 O15 H15A O14 0.75(8) 1.98(8) 2.713(6) 168(7) 3_756 O15 H15B O11 0.78(9) 1.99(10) 2.759(6) 171(9) 3_756 O16 H161 O8 0.67 2.26 2.871(6) 153.4 . O16 H162 O7 0.90 1.92 2.819(5) 174.0 . O18 H18A O12 0.67 2.26 2.859(7) 149.4 . O18 H18B O13 0.86 1.98 2.806(6) 161.1 . _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 1.630 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.129 #===END data_complex_11 _database_code_depnum_ccdc_archive 'CCDC 265323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H57 F5 N4 O6 Pd' _chemical_formula_weight 831.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1604(5) _cell_length_b 10.3459(5) _cell_length_c 20.5010(10) _cell_angle_alpha 82.1130(10) _cell_angle_beta 80.4260(10) _cell_angle_gamma 69.3144(8) _cell_volume 1980.81(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8772 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23353 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.22 _reflns_number_total 8933 _reflns_number_gt 8109 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0609P)^2^+8.0273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8933 _refine_ls_number_parameters 476 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.260 _refine_ls_shift/su_mean 0.004 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 0.92365(3) 0.74241(2) 0.720581(12) 0.01334(8) Uani 1 1 d . . . N1 N 1.0905(3) 0.6711(3) 0.77468(14) 0.0163(5) Uani 1 1 d . . . C1 C 1.0583(4) 0.7347(4) 0.63642(16) 0.0179(7) Uani 1 1 d . . . C8 C 1.2864(4) 0.6606(4) 0.8270(2) 0.0280(8) Uani 1 1 d . . . H8A H 1.2790 0.7252 0.8599 0.034 Uiso 1 1 calc R . . H8B H 1.3866 0.6220 0.8073 0.034 Uiso 1 1 calc R . . C2 C 1.0669(4) 0.8527(4) 0.59699(17) 0.0197(7) Uani 1 1 d . . . C6 C 1.1538(4) 0.6114(4) 0.61359(18) 0.0207(7) Uani 1 1 d . . . C3 C 1.1605(4) 0.8499(4) 0.53957(17) 0.0237(7) Uani 1 1 d . . . C10 C 1.1048(4) 0.5648(3) 0.82259(17) 0.0194(7) Uani 1 1 d . . . C7 C 1.1919(4) 0.7326(3) 0.77394(17) 0.0178(7) Uani 1 1 d . . . C9 C 1.2295(4) 0.5444(4) 0.85915(19) 0.0247(8) Uani 1 1 d . . . H9A H 1.3026 0.4520 0.8531 0.030 Uiso 1 1 calc R . . H9B H 1.1987 0.5537 0.9072 0.030 Uiso 1 1 calc R . . C5 C 1.2477(4) 0.6032(4) 0.55653(19) 0.0235(7) Uani 1 1 d . . . F1 F 0.9796(2) 0.9794(2) 0.61465(10) 0.0269(5) Uani 1 1 d . . . F5 F 1.1569(2) 0.4900(2) 0.64931(12) 0.0289(5) Uani 1 1 d . . . F2 F 1.1655(3) 0.9677(2) 0.50398(11) 0.0318(5) Uani 1 1 d . . . O2 O 1.2022(3) 0.8313(2) 0.73625(12) 0.0221(5) Uani 1 1 d . . . F4 F 1.3364(3) 0.4801(3) 0.53665(13) 0.0391(6) Uani 1 1 d . . . O1 O 1.0283(3) 0.4933(3) 0.83531(12) 0.0228(5) Uani 1 1 d . . . O4 O 0.8731(3) 0.8698(3) 0.86800(12) 0.0225(5) Uani 1 1 d . . . O3 O 0.6628(3) 0.6207(2) 0.78195(12) 0.0212(5) Uani 1 1 d . . . N2 N 0.7855(3) 0.7520(3) 0.80856(14) 0.0174(6) Uani 1 1 d . . . C14 C 0.7980(4) 0.8008(3) 0.86482(16) 0.0172(6) Uani 1 1 d . . . C11 C 0.6925(4) 0.6794(3) 0.82223(17) 0.0182(7) Uani 1 1 d . . . C13 C 0.7064(4) 0.7590(4) 0.92435(17) 0.0214(7) Uani 1 1 d . . . H13A H 0.7652 0.6981 0.9579 0.026 Uiso 1 1 calc R . . H13B H 0.6375 0.8415 0.9452 0.026 Uiso 1 1 calc R . . C12 C 0.6313(4) 0.6821(4) 0.89503(19) 0.0279(8) Uani 1 1 d . . . H12A H 0.5275 0.7313 0.9001 0.033 Uiso 1 1 calc R . . H12B H 0.6506 0.5868 0.9167 0.033 Uiso 1 1 calc R . . F3 F 1.3408(2) 0.7186(3) 0.46250(11) 0.0358(6) Uani 1 1 d . . . N3 N 0.6747(3) 0.8069(3) 0.64038(15) 0.0216(6) Uani 1 1 d . . . C15 C 0.7678(4) 0.7897(4) 0.66878(17) 0.0202(7) Uani 1 1 d . . . C4 C 1.2502(4) 0.7238(4) 0.51875(18) 0.0249(8) Uani 1 1 d . . . C16 C 0.5483(4) 0.8129(4) 0.61195(17) 0.0203(7) Uani 1 1 d . . . C17 C 0.5130(4) 0.6832(4) 0.6406(2) 0.0295(8) Uani 1 1 d . . . H17A H 0.4899 0.6843 0.6889 0.044 Uiso 1 1 calc R . . H17B H 0.5950 0.6006 0.6299 0.044 Uiso 1 1 calc R . . H17C H 0.4316 0.6815 0.6215 0.044 Uiso 1 1 calc R . . C18 C 0.4296(4) 0.9444(4) 0.6329(2) 0.0286(8) Uani 1 1 d . . . H18A H 0.4086 0.9389 0.6815 0.043 Uiso 1 1 calc R . . H18B H 0.3446 0.9541 0.6134 0.043 Uiso 1 1 calc R . . H18C H 0.4595 1.0249 0.6174 0.043 Uiso 1 1 calc R . . C19 C 0.5858(4) 0.8156(4) 0.53708(18) 0.0287(8) Uani 1 1 d . . . H19A H 0.6084 0.8997 0.5202 0.043 Uiso 1 1 calc R . . H19B H 0.5051 0.8150 0.5169 0.043 Uiso 1 1 calc R . . H19C H 0.6682 0.7338 0.5257 0.043 Uiso 1 1 calc R . . N4 N 0.1108(3) 0.7786(3) 0.21643(14) 0.0178(6) Uani 1 1 d . . . C21 C 0.2261(4) 0.7979(4) 0.09638(17) 0.0214(7) Uani 1 1 d . . . H21A H 0.2686 0.8600 0.1109 0.026 Uiso 1 1 calc R . . H21B H 0.1375 0.8564 0.0782 0.026 Uiso 1 1 calc R . . C20 C 0.1916(4) 0.7050(3) 0.15547(16) 0.0177(6) Uani 1 1 d . . . H20A H 0.2814 0.6350 0.1677 0.021 Uiso 1 1 calc R . . H20B H 0.1351 0.6548 0.1419 0.021 Uiso 1 1 calc R . . C33 C -0.0059(4) 0.7246(4) 0.33347(18) 0.0248(8) Uani 1 1 d . . . H33A H -0.0069 0.8200 0.3357 0.030 Uiso 1 1 calc R . . H33B H -0.1051 0.7287 0.3346 0.030 Uiso 1 1 calc R . . C24 C 0.1984(3) 0.8488(3) 0.24266(16) 0.0166(6) Uani 1 1 d . . . H24A H 0.2075 0.9261 0.2101 0.020 Uiso 1 1 calc R . . H24B H 0.1460 0.8893 0.2844 0.020 Uiso 1 1 calc R . . C32 C 0.0808(4) 0.6690(3) 0.26805(17) 0.0208(7) Uani 1 1 d . . . H32A H 0.1723 0.5988 0.2781 0.025 Uiso 1 1 calc R . . H32B H 0.0289 0.6216 0.2487 0.025 Uiso 1 1 calc R . . C23 C 0.4770(4) 0.6402(4) 0.06162(18) 0.0235(7) Uani 1 1 d . . . H23A H 0.5386 0.5875 0.0252 0.035 Uiso 1 1 calc R . . H23B H 0.4723 0.5769 0.1014 0.035 Uiso 1 1 calc R . . H23C H 0.5156 0.7093 0.0709 0.035 Uiso 1 1 calc R . . C28 C -0.0261(4) 0.8926(3) 0.20006(18) 0.0194(7) Uani 1 1 d . . . H28A H -0.0763 0.9373 0.2411 0.023 Uiso 1 1 calc R . . H28B H -0.0014 0.9639 0.1681 0.023 Uiso 1 1 calc R . . C22 C 0.3295(4) 0.7128(4) 0.04197(17) 0.0223(7) Uani 1 1 d . . . H22A H 0.2921 0.6426 0.0317 0.027 Uiso 1 1 calc R . . H22B H 0.3354 0.7750 0.0012 0.027 Uiso 1 1 calc R . . C29 C -0.1264(4) 0.8438(4) 0.1711(2) 0.0240(7) Uani 1 1 d . . . H29A H -0.1590 0.7790 0.2044 0.029 Uiso 1 1 calc R . . H29B H -0.0753 0.7930 0.1318 0.029 Uiso 1 1 calc R . . C25 C 0.3454(4) 0.7546(4) 0.2560(2) 0.0259(8) Uani 1 1 d . . . H25A H 0.3382 0.6713 0.2844 0.031 Uiso 1 1 calc R . . H25B H 0.4030 0.7237 0.2134 0.031 Uiso 1 1 calc R . . C35 C -0.0427(5) 0.6777(5) 0.4572(2) 0.0397(10) Uani 1 1 d . . . H35A H -0.0015 0.6176 0.4953 0.059 Uiso 1 1 calc R . . H35B H -0.1351 0.6701 0.4547 0.059 Uiso 1 1 calc R . . H35C H -0.0549 0.7740 0.4627 0.059 Uiso 1 1 calc R . . C34 C 0.0562(4) 0.6330(5) 0.39339(19) 0.0334(9) Uani 1 1 d . . . H34A H 0.1499 0.6397 0.3961 0.040 Uiso 1 1 calc R . . H34B H 0.0699 0.5352 0.3882 0.040 Uiso 1 1 calc R . . C26 C 0.4190(4) 0.8255(4) 0.2896(2) 0.0331(9) Uani 1 1 d . . . H26A H 0.3593 0.8604 0.3311 0.040 Uiso 1 1 calc R . . H26B H 0.4309 0.9059 0.2602 0.040 Uiso 1 1 calc R . . C30 C -0.2540(4) 0.9646(4) 0.1510(2) 0.0321(9) Uani 1 1 d . . . H30A H -0.2212 1.0308 0.1188 0.039 Uiso 1 1 calc R . . H30B H -0.3067 1.0136 0.1906 0.039 Uiso 1 1 calc R . . C27 C 0.5642(4) 0.7266(5) 0.3059(3) 0.0410(11) Uani 1 1 d . . . H27A H 0.6093 0.7756 0.3276 0.061 Uiso 1 1 calc R . . H27B H 0.6240 0.6931 0.2648 0.061 Uiso 1 1 calc R . . H27C H 0.5525 0.6477 0.3356 0.061 Uiso 1 1 calc R . . C31 C -0.3531(5) 0.9160(5) 0.1198(3) 0.0440(12) Uani 1 1 d . . . H31A H -0.4343 0.9963 0.1075 0.066 Uiso 1 1 calc R . . H31B H -0.3869 0.8515 0.1518 0.066 Uiso 1 1 calc R . . H31C H -0.3017 0.8692 0.0800 0.066 Uiso 1 1 calc R . . O5 O 0.0340(4) 0.5917(3) 0.03201(14) 0.0350(7) Uani 1 1 d D . . O6 O 0.0148(5) 0.1267(4) 0.0164(2) 0.0556(11) Uani 1 1 d D . . H61 H 0.073(6) 0.081(11) -0.006(3) 0.21(6) Uiso 1 1 d D . . H62 H 0.045(5) 0.122(5) 0.0480(14) 0.028(12) Uiso 1 1 d D . . H51 H -0.004(11) 0.665(4) 0.021(3) 0.22(6) Uiso 1 1 d D . . H52 H 0.013(6) 0.577(5) 0.0677(11) 0.046(16) Uiso 1 1 d 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 0.01408(13) 0.01441(13) 0.01309(13) 0.00096(8) -0.00387(9) -0.00656(9) N1 0.0169(14) 0.0160(13) 0.0181(14) 0.0002(10) -0.0042(11) -0.0079(11) C1 0.0176(16) 0.0228(17) 0.0163(16) -0.0025(13) -0.0034(12) -0.0098(13) C8 0.0242(19) 0.037(2) 0.029(2) 0.0038(16) -0.0139(16) -0.0157(17) C2 0.0228(17) 0.0212(17) 0.0159(16) -0.0039(13) -0.0022(13) -0.0075(14) C6 0.0204(17) 0.0183(16) 0.0264(18) -0.0033(13) -0.0036(14) -0.0095(14) C3 0.032(2) 0.0274(19) 0.0174(17) 0.0024(14) -0.0046(14) -0.0175(16) C10 0.0236(17) 0.0157(16) 0.0196(17) -0.0032(12) -0.0079(13) -0.0046(13) C7 0.0171(16) 0.0177(16) 0.0199(16) -0.0063(13) -0.0023(13) -0.0059(13) C9 0.0258(19) 0.0241(18) 0.0265(19) 0.0042(14) -0.0136(15) -0.0090(15) C5 0.0175(17) 0.0254(18) 0.0293(19) -0.0146(15) -0.0014(14) -0.0056(14) F1 0.0386(13) 0.0171(10) 0.0216(11) -0.0013(8) -0.0008(9) -0.0069(9) F5 0.0271(12) 0.0169(10) 0.0424(13) 0.0014(9) -0.0047(10) -0.0082(9) F2 0.0426(14) 0.0360(13) 0.0202(11) 0.0071(9) 0.0000(10) -0.0226(11) O2 0.0218(13) 0.0196(12) 0.0255(13) -0.0012(10) -0.0003(10) -0.0091(10) F4 0.0310(13) 0.0346(13) 0.0488(15) -0.0215(11) 0.0083(11) -0.0073(11) O1 0.0300(14) 0.0195(12) 0.0244(13) 0.0041(10) -0.0100(11) -0.0144(11) O4 0.0319(14) 0.0202(12) 0.0222(13) -0.0004(10) -0.0072(10) -0.0161(11) O3 0.0231(13) 0.0195(12) 0.0240(13) -0.0018(10) -0.0055(10) -0.0098(10) N2 0.0176(14) 0.0182(14) 0.0175(14) -0.0007(11) -0.0011(11) -0.0082(11) C14 0.0226(17) 0.0119(15) 0.0146(15) 0.0025(11) -0.0042(12) -0.0033(13) C11 0.0184(16) 0.0137(15) 0.0222(17) 0.0009(12) -0.0028(13) -0.0061(13) C13 0.0258(18) 0.0196(17) 0.0165(16) 0.0011(13) -0.0021(13) -0.0062(14) C12 0.033(2) 0.032(2) 0.0232(19) -0.0039(15) 0.0055(15) -0.0198(17) F3 0.0298(13) 0.0578(16) 0.0230(12) -0.0128(11) 0.0090(9) -0.0208(12) N3 0.0241(16) 0.0254(15) 0.0185(14) 0.0017(12) -0.0048(12) -0.0127(13) C15 0.0219(18) 0.0185(16) 0.0197(17) 0.0002(13) -0.0028(14) -0.0070(13) C4 0.0201(18) 0.042(2) 0.0198(17) -0.0110(15) 0.0004(14) -0.0168(16) C16 0.0149(16) 0.0262(18) 0.0215(17) 0.0013(13) -0.0067(13) -0.0085(14) C17 0.031(2) 0.030(2) 0.034(2) 0.0050(16) -0.0126(17) -0.0174(17) C18 0.0233(19) 0.034(2) 0.029(2) -0.0038(16) -0.0034(15) -0.0092(16) C19 0.028(2) 0.041(2) 0.0194(18) -0.0035(16) -0.0052(15) -0.0135(17) N4 0.0200(14) 0.0142(13) 0.0196(14) -0.0025(11) -0.0008(11) -0.0068(11) C21 0.0265(18) 0.0182(16) 0.0177(17) 0.0012(13) -0.0030(14) -0.0062(14) C20 0.0202(17) 0.0151(15) 0.0171(16) -0.0034(12) -0.0012(13) -0.0049(13) C33 0.031(2) 0.0247(18) 0.0227(18) -0.0055(14) 0.0050(15) -0.0164(16) C24 0.0184(16) 0.0164(15) 0.0164(15) -0.0019(12) -0.0001(12) -0.0084(13) C32 0.0271(19) 0.0147(15) 0.0216(17) -0.0006(13) 0.0014(14) -0.0106(14) C23 0.0214(18) 0.0303(19) 0.0191(17) -0.0031(14) 0.0007(14) -0.0101(15) C28 0.0167(16) 0.0149(15) 0.0246(18) -0.0020(13) -0.0010(13) -0.0037(13) C22 0.0256(18) 0.0258(18) 0.0153(16) -0.0018(13) -0.0011(13) -0.0092(15) C29 0.0225(18) 0.0193(17) 0.032(2) -0.0058(14) -0.0066(15) -0.0065(14) C25 0.0256(19) 0.0211(18) 0.033(2) -0.0011(15) -0.0086(16) -0.0089(15) C35 0.035(2) 0.062(3) 0.024(2) -0.006(2) -0.0011(17) -0.019(2) C34 0.0221(19) 0.060(3) 0.0205(19) -0.0058(18) -0.0020(15) -0.0162(19) C26 0.023(2) 0.036(2) 0.042(2) -0.0132(18) -0.0121(17) -0.0045(17) C30 0.027(2) 0.027(2) 0.042(2) -0.0090(17) -0.0121(17) -0.0025(16) C27 0.025(2) 0.043(3) 0.055(3) -0.015(2) -0.020(2) -0.0008(19) C31 0.038(3) 0.039(2) 0.060(3) -0.002(2) -0.030(2) -0.009(2) O5 0.055(2) 0.0370(17) 0.0190(15) 0.0058(12) -0.0066(14) -0.0257(15) O6 0.096(3) 0.0398(19) 0.044(2) 0.0068(16) -0.050(2) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C15 1.935(4) . ? Pd1 C1 2.008(3) . ? Pd1 N1 2.041(3) . ? Pd1 N2 2.083(3) . ? N1 C10 1.354(4) . ? N1 C7 1.386(4) . ? C1 C6 1.388(5) . ? C1 C2 1.391(5) . ? C8 C7 1.509(5) . ? C8 C9 1.536(5) . ? C2 F1 1.355(4) . ? C2 C3 1.381(5) . ? C6 F5 1.357(4) . ? C6 C5 1.373(5) . ? C3 F2 1.345(4) . ? C3 C4 1.378(5) . ? C10 O1 1.226(4) . ? C10 C9 1.515(5) . ? C7 O2 1.218(4) . ? C5 F4 1.345(4) . ? C5 C4 1.382(6) . ? O4 C14 1.229(4) . ? O3 C11 1.222(4) . ? N2 C14 1.362(4) . ? N2 C11 1.375(4) . ? C14 C13 1.518(5) . ? C11 C12 1.518(5) . ? C13 C12 1.513(5) . ? F3 C4 1.345(4) . ? N3 C15 1.141(5) . ? N3 C16 1.475(4) . ? C16 C19 1.518(5) . ? C16 C18 1.523(5) . ? C16 C17 1.525(5) . ? N4 C20 1.515(4) . ? N4 C32 1.519(4) . ? N4 C28 1.525(4) . ? N4 C24 1.527(4) . ? C21 C20 1.514(5) . ? C21 C22 1.533(5) . ? C33 C34 1.524(6) . ? C33 C32 1.538(5) . ? C24 C25 1.513(5) . ? C23 C22 1.515(5) . ? C28 C29 1.514(5) . ? C29 C30 1.518(5) . ? C25 C26 1.507(5) . ? C35 C34 1.529(6) . ? C26 C27 1.529(5) . ? C30 C31 1.529(6) . ? 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 C15 Pd1 C1 89.75(14) . . ? C15 Pd1 N1 173.94(13) . . ? C1 Pd1 N1 90.16(12) . . ? C15 Pd1 N2 90.90(13) . . ? C1 Pd1 N2 179.14(12) . . ? N1 Pd1 N2 89.25(11) . . ? C10 N1 C7 111.1(3) . . ? C10 N1 Pd1 122.5(2) . . ? C7 N1 Pd1 125.9(2) . . ? C6 C1 C2 114.2(3) . . ? C6 C1 Pd1 123.0(3) . . ? C2 C1 Pd1 122.9(3) . . ? C7 C8 C9 103.9(3) . . ? F1 C2 C3 116.7(3) . . ? F1 C2 C1 119.5(3) . . ? C3 C2 C1 123.8(3) . . ? F5 C6 C5 116.8(3) . . ? F5 C6 C1 119.0(3) . . ? C5 C6 C1 124.2(3) . . ? F2 C3 C4 119.7(3) . . ? F2 C3 C2 121.2(3) . . ? C4 C3 C2 119.1(3) . . ? O1 C10 N1 125.4(3) . . ? O1 C10 C9 123.7(3) . . ? N1 C10 C9 110.9(3) . . ? O2 C7 N1 124.8(3) . . ? O2 C7 C8 125.0(3) . . ? N1 C7 C8 110.2(3) . . ? C10 C9 C8 103.8(3) . . ? F4 C5 C6 121.2(3) . . ? F4 C5 C4 119.6(3) . . ? C6 C5 C4 119.2(3) . . ? C14 N2 C11 110.4(3) . . ? C14 N2 Pd1 124.7(2) . . ? C11 N2 Pd1 123.1(2) . . ? O4 C14 N2 125.2(3) . . ? O4 C14 C13 123.5(3) . . ? N2 C14 C13 111.2(3) . . ? O3 C11 N2 125.3(3) . . ? O3 C11 C12 124.4(3) . . ? N2 C11 C12 110.3(3) . . ? C12 C13 C14 103.6(3) . . ? C13 C12 C11 104.4(3) . . ? C15 N3 C16 170.8(3) . . ? N3 C15 Pd1 174.1(3) . . ? F3 C4 C3 120.1(4) . . ? F3 C4 C5 120.4(3) . . ? C3 C4 C5 119.5(3) . . ? N3 C16 C19 107.6(3) . . ? N3 C16 C18 107.1(3) . . ? C19 C16 C18 111.9(3) . . ? N3 C16 C17 106.9(3) . . ? C19 C16 C17 111.4(3) . . ? C18 C16 C17 111.6(3) . . ? C20 N4 C32 106.8(2) . . ? C20 N4 C28 111.0(3) . . ? C32 N4 C28 111.3(3) . . ? C20 N4 C24 110.7(3) . . ? C32 N4 C24 110.4(3) . . ? C28 N4 C24 106.7(2) . . ? C20 C21 C22 111.3(3) . . ? C21 C20 N4 115.3(3) . . ? C34 C33 C32 111.3(3) . . ? C25 C24 N4 114.9(3) . . ? N4 C32 C33 114.7(3) . . ? C29 C28 N4 114.8(3) . . ? C23 C22 C21 112.8(3) . . ? C28 C29 C30 111.5(3) . . ? C26 C25 C24 112.1(3) . . ? C33 C34 C35 110.5(4) . . ? C25 C26 C27 111.4(3) . . ? C29 C30 C31 111.6(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H61 O6 0.75(2) 2.65(12) 2.919(7) 104(10) 2 O6 H62 O4 0.748(19) 2.06(2) 2.805(4) 174(5) 2_666 O5 H51 O6 0.74(2) 2.16(6) 2.840(5) 153(12) 2_565 O5 H52 O1 0.738(19) 2.05(2) 2.782(4) 172(6) 2_666 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.712 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.096 #===END