Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_coden_cambridge 1145 _publ_contact_author_name 'Peter Horton' _publ_contact_author_email P.N.Horton@soton.ac.uk _publ_contact_author_address ; Department of Chemistry University of York Heslington York YO10 5DD UNITED KINGDOM ; loop_ _publ_author_name 'Viorel Circu' 'Timothy J. K. Gibbs' 'Laurent Omnes' 'Peter N. Horton' 'Michael B. Hursthouse' 'Duncan W. Bruce' _publ_section_title ; Orthometallated Palladium(II) Imine Complexes as Candidate Materials for the Biaxial Nematic Phase. Crystal and Molecular Structure of Three Palladium Imine Complexes ; _publ_requested_journal 'Journal of Materials Chemistry' data_1a _database_code_depnum_ccdc_archive 'CCDC 602441' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 F5 N O4 Pd' _chemical_formula_weight 704.05 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' _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 11.125(2) _cell_length_b 16.094(10) _cell_length_c 18.370(9) _cell_angle_alpha 77.92(5) _cell_angle_beta 87.20(2) _cell_angle_gamma 89.60(3) _cell_volume 3212(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11518 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Rod _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9810 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54621 _diffrn_reflns_av_R_equivalents 0.1313 _diffrn_reflns_av_sigmaI/netI 0.1687 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14625 _reflns_number_gt 6611 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _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^)+(0.2000P)^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 14625 _refine_ls_number_parameters 1100 _refine_ls_number_restraints 1914 _refine_ls_R_factor_all 0.2395 _refine_ls_R_factor_gt 0.1328 _refine_ls_wR_factor_ref 0.3870 _refine_ls_wR_factor_gt 0.3342 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.72065(6) 0.53048(5) 0.18677(4) 0.0534(3) Uani 1 1 d DU . . Pd2 Pd 0.70749(8) 0.54447(7) -0.25086(4) 0.0704(4) Uani 1 1 d DU . . C1 C 0.7079(8) 0.6065(7) 0.0877(5) 0.054(2) Uani 1 1 d U C . C2 C 0.7753(8) 0.5786(7) 0.0316(5) 0.051(2) Uani 1 1 d U . . C3 C 0.7720(8) 0.6245(7) -0.0436(5) 0.055(2) Uani 1 1 d U C . H3 H 0.8168 0.6055 -0.0824 0.066 Uiso 1 1 calc R . . C4 C 0.7019(8) 0.6977(7) -0.0593(5) 0.056(2) Uani 1 1 d U . . H4 H 0.6996 0.7292 -0.1091 0.067 Uiso 1 1 calc R C . C5 C 0.6361(8) 0.7247(7) -0.0034(6) 0.052(2) Uani 1 1 d U C . C6 C 0.6386(8) 0.6795(7) 0.0723(5) 0.054(2) Uani 1 1 d U . . H6 H 0.5940 0.6988 0.1109 0.065 Uiso 1 1 calc R C . C7 C 0.8446(8) 0.5037(7) 0.0561(5) 0.054(2) Uani 1 1 d U C . H7 H 0.8924 0.4789 0.0221 0.064 Uiso 1 1 calc R . . C8 C 0.9089(8) 0.3973(7) 0.1549(5) 0.052(2) Uani 1 1 d U . . C9 C 0.9210(8) 0.3318(7) 0.1156(6) 0.058(2) Uani 1 1 d U C . H9 H 0.8804 0.3349 0.0708 0.070 Uiso 1 1 calc R . . C10 C 0.9924(9) 0.2627(7) 0.1424(6) 0.061(2) Uani 1 1 d U . . H10 H 0.9988 0.2177 0.1162 0.073 Uiso 1 1 calc R C . C11 C 1.0548(9) 0.2574(7) 0.2066(6) 0.060(2) Uani 1 1 d U C . C12 C 1.0387(10) 0.3232(7) 0.2447(6) 0.065(2) Uani 1 1 d U . . H12 H 1.0800 0.3206 0.2892 0.078 Uiso 1 1 calc R C . C13 C 0.9669(9) 0.3905(7) 0.2213(5) 0.055(2) Uani 1 1 d U C . H13 H 0.9560 0.4329 0.2500 0.066 Uiso 1 1 calc R . . C14 C 0.5665(9) 0.8437(7) -0.0873(6) 0.069(3) Uani 1 1 d DU C . H14A H 0.5375 0.8082 -0.1209 0.082 Uiso 1 1 calc R . . H14B H 0.6479 0.8652 -0.1056 0.082 Uiso 1 1 calc R . . C15 C 0.4796(9) 0.9181(6) -0.0847(5) 0.068(3) Uani 1 1 d DU . . H15A H 0.3996 0.8955 -0.0643 0.082 Uiso 1 1 calc R . . H15B H 0.5101 0.9531 -0.0511 0.082 Uiso 1 1 calc R . . C16 C 0.4670(9) 0.9735(6) -0.1618(5) 0.071(3) Uani 1 1 d DU . . H16A H 0.4410 0.9379 -0.1961 0.086 Uiso 1 1 calc R . . H16B H 0.5462 0.9988 -0.1810 0.086 Uiso 1 1 calc R . . C17 C 0.3759(10) 1.0441(7) -0.1601(6) 0.080(3) Uani 1 1 d DU . . H17A H 0.2975 1.0188 -0.1393 0.096 Uiso 1 1 calc R . . H17B H 0.4033 1.0807 -0.1270 0.096 Uiso 1 1 calc R . . C18 C 0.3599(14) 1.0981(9) -0.2375(6) 0.114(5) Uani 1 1 d DU . . H18A H 0.3366 1.0616 -0.2717 0.137 Uiso 1 1 calc R . . H18B H 0.4366 1.1270 -0.2572 0.137 Uiso 1 1 calc R . . C19 C 0.2597(15) 1.1655(12) -0.2323(8) 0.134(7) Uani 1 1 d DU . . H19A H 0.1818 1.1368 -0.2197 0.201 Uiso 1 1 calc R . . H19B H 0.2564 1.2055 -0.2804 0.201 Uiso 1 1 calc R . . H19C H 0.2782 1.1965 -0.1936 0.201 Uiso 1 1 calc R . . C20 C 1.1895(10) 0.1830(8) 0.2932(6) 0.075(3) Uani 1 1 d DU B . H20A H 1.1318 0.1775 0.3367 0.090 Uiso 1 1 calc R . . H20B H 1.2409 0.2335 0.2910 0.090 Uiso 1 1 calc R . . C21 C 1.2658(11) 0.1035(8) 0.2989(6) 0.084(3) Uani 1 1 d DU B . H21A H 1.2144 0.0556 0.2929 0.101 Uiso 1 1 calc R . . H21B H 1.3287 0.1128 0.2580 0.101 Uiso 1 1 calc R . . C22 C 1.3251(15) 0.0802(8) 0.3727(6) 0.113(5) Uani 1 1 d DU . . H22A H 1.2637 0.0770 0.4141 0.135 Uiso 1 1 calc R A 1 H22B H 1.3847 0.1243 0.3764 0.135 Uiso 1 1 calc R A 1 C23A C 1.387(3) -0.0054(14) 0.3786(9) 0.115(8) Uani 0.53(3) 1 d PDU B 1 H23A H 1.3441 -0.0404 0.3499 0.138 Uiso 0.53(3) 1 calc PR B 1 H23B H 1.4707 0.0035 0.3569 0.138 Uiso 0.53(3) 1 calc PR B 1 C24A C 1.3903(10) -0.0518(10) 0.4592(11) 0.148(10) Uani 0.53(3) 1 d PDU B 1 H24A H 1.3107 -0.0774 0.4768 0.178 Uiso 0.53(3) 1 calc PR B 1 H24B H 1.4110 -0.0120 0.4912 0.178 Uiso 0.53(3) 1 calc PR B 1 C25A C 1.489(4) -0.123(2) 0.4627(15) 0.139(13) Uani 0.53(3) 1 d PDU B 1 H25A H 1.4833 -0.1498 0.4197 0.208 Uiso 0.53(3) 1 calc PR B 1 H25B H 1.4756 -0.1660 0.5088 0.208 Uiso 0.53(3) 1 calc PR B 1 H25C H 1.5688 -0.0977 0.4618 0.208 Uiso 0.53(3) 1 calc PR B 1 C23B C 1.4072(17) 0.0044(10) 0.3750(12) 0.118(8) Uani 0.47(3) 1 d PDU B 2 H23C H 1.4725 0.0070 0.4092 0.141 Uiso 0.47(3) 1 calc PR B 2 H23D H 1.4444 0.0059 0.3246 0.141 Uiso 0.47(3) 1 calc PR B 2 C24B C 1.337(3) -0.0777(9) 0.401(2) 0.125(9) Uani 0.47(3) 1 d PDU B 2 H24C H 1.2929 -0.0916 0.3597 0.150 Uiso 0.47(3) 1 calc PR B 2 H24D H 1.2779 -0.0722 0.4420 0.150 Uiso 0.47(3) 1 calc PR B 2 C25B C 1.431(4) -0.1493(14) 0.4296(18) 0.122(14) Uani 0.47(3) 1 d PDU B 2 H25D H 1.4006 -0.2039 0.4222 0.183 Uiso 0.47(3) 1 calc PR B 2 H25E H 1.4418 -0.1528 0.4827 0.183 Uiso 0.47(3) 1 calc PR B 2 H25F H 1.5076 -0.1358 0.4015 0.183 Uiso 0.47(3) 1 calc PR B 2 N1 N 0.8391(6) 0.4711(5) 0.1272(4) 0.0517(17) Uani 1 1 d U C . O1 O 0.5690(6) 0.7957(5) -0.0131(4) 0.0589(16) Uani 1 1 d U . . O2 O 1.1260(7) 0.1907(5) 0.2250(4) 0.0698(19) Uani 1 1 d U . . C31A C 0.8156(18) 0.3565(13) 0.4312(10) 0.129(6) Uani 0.560(11) 1 d PDU C 1 C32A C 0.6980(17) 0.3767(12) 0.4119(9) 0.098(5) Uani 0.560(11) 1 d PDU C 1 C33A C 0.675(2) 0.4433(13) 0.3483(11) 0.075(5) Uani 0.560(11) 1 d PDU C 1 C34A C 0.581(2) 0.4974(16) 0.3530(13) 0.070(5) Uani 0.560(11) 1 d PDU C 1 H34A H 0.5355 0.4874 0.3989 0.083 Uiso 0.560(11) 1 calc PR C 1 C35A C 0.544(2) 0.5667(13) 0.2977(13) 0.065(5) Uani 0.560(11) 1 d PDU C 1 C36A C 0.4409(19) 0.6285(13) 0.3136(11) 0.076(5) Uani 0.560(11) 1 d PDU C 1 H36A H 0.3724 0.5937 0.3396 0.091 Uiso 0.560(11) 1 calc PR C 1 H36B H 0.4705 0.6623 0.3483 0.091 Uiso 0.560(11) 1 calc PR C 1 C37A C 0.397(3) 0.686(2) 0.2497(14) 0.098(9) Uani 0.560(11) 1 d PDU C 1 H37A H 0.4647 0.7106 0.2162 0.147 Uiso 0.560(11) 1 calc PR C 1 H37B H 0.3517 0.7322 0.2662 0.147 Uiso 0.560(11) 1 calc PR C 1 H37C H 0.3437 0.6557 0.2232 0.147 Uiso 0.560(11) 1 calc PR C 1 O31A O 0.7384(19) 0.4448(11) 0.2884(9) 0.082(7) Uani 0.560(11) 1 d PDU C 1 O32A O 0.5881(15) 0.5923(13) 0.2306(12) 0.059(4) Uani 0.560(11) 1 d PDU C 1 F31A F 0.865(3) 0.3174(17) 0.3783(12) 0.262(13) Uani 0.560(11) 1 d PDU C 1 F32A F 0.8055(18) 0.2971(13) 0.4969(9) 0.183(9) Uani 0.560(11) 1 d PDU C 1 F33A F 0.862(2) 0.4322(14) 0.4381(12) 0.221(11) Uani 0.560(11) 1 d PDU C 1 F34A F 0.643(2) 0.2996(11) 0.4079(12) 0.187(8) Uani 0.560(11) 1 d PDU C 1 F35A F 0.648(2) 0.3979(15) 0.4768(8) 0.206(10) Uani 0.560(11) 1 d PDU C 1 C31B C 0.410(2) 0.7030(14) 0.2774(13) 0.095(6) Uani 0.440(11) 1 d PDU C 2 C32B C 0.4850(18) 0.6508(13) 0.3252(12) 0.091(5) Uani 0.440(11) 1 d PDU C 2 C33B C 0.559(2) 0.5870(15) 0.3004(14) 0.059(5) Uani 0.440(11) 1 d PDU C 2 C34B C 0.579(3) 0.5143(18) 0.3523(16) 0.074(7) Uani 0.440(11) 1 d PDU C 2 H34B H 0.5340 0.5073 0.3985 0.088 Uiso 0.440(11) 1 calc PR C 2 C35B C 0.660(3) 0.4489(17) 0.3436(15) 0.074(6) Uani 0.440(11) 1 d PDU C 2 C36B C 0.675(3) 0.3681(19) 0.4071(16) 0.094(7) Uani 0.440(11) 1 d PDU C 2 H36C H 0.6767 0.3867 0.4551 0.113 Uiso 0.440(11) 1 calc PR C 2 H36D H 0.6033 0.3317 0.4095 0.113 Uiso 0.440(11) 1 calc PR C 2 C37B C 0.781(3) 0.316(3) 0.401(2) 0.124(13) Uani 0.440(11) 1 d PDU C 2 H37D H 0.8218 0.3353 0.3515 0.187 Uiso 0.440(11) 1 calc PR C 2 H37E H 0.7570 0.2565 0.4068 0.187 Uiso 0.440(11) 1 calc PR C 2 H37F H 0.8365 0.3215 0.4394 0.187 Uiso 0.440(11) 1 calc PR C 2 O31B O 0.6034(15) 0.6036(15) 0.2340(14) 0.055(5) Uani 0.440(11) 1 d PDU C 2 O32B O 0.730(2) 0.4446(13) 0.2867(10) 0.060(5) Uani 0.440(11) 1 d PDU C 2 F31B F 0.352(2) 0.7486(14) 0.3241(13) 0.168(10) Uani 0.440(11) 1 d PDU C 2 F32B F 0.4915(17) 0.7583(9) 0.2342(13) 0.138(8) Uani 0.440(11) 1 d PDU C 2 F33B F 0.3476(17) 0.6466(13) 0.2498(11) 0.096(6) Uani 0.440(11) 1 d PDU C 2 F34B F 0.555(2) 0.7071(14) 0.3567(15) 0.174(10) Uani 0.440(11) 1 d PDU C 2 F35B F 0.393(2) 0.6140(14) 0.3774(13) 0.177(10) Uani 0.440(11) 1 d PDU C 2 C41 C 0.5738(9) 0.6138(8) -0.2218(5) 0.056(2) Uani 1 1 d U F . C42 C 0.5243(8) 0.5809(7) -0.1489(5) 0.055(2) Uani 1 1 d U . . C43 C 0.4263(8) 0.6230(8) -0.1226(6) 0.061(2) Uani 1 1 d U F . H43 H 0.3914 0.6007 -0.0743 0.073 Uiso 1 1 calc R . . C44 C 0.3805(8) 0.6929(8) -0.1629(6) 0.063(2) Uani 1 1 d U . . H44 H 0.3154 0.7210 -0.1430 0.075 Uiso 1 1 calc R F . C45 C 0.4292(9) 0.7250(8) -0.2353(6) 0.065(2) Uani 1 1 d U E . C46 C 0.5283(10) 0.6813(8) -0.2632(6) 0.068(3) Uani 1 1 d U . . H46 H 0.5612 0.7018 -0.3123 0.081 Uiso 1 1 calc R F . C47 C 0.5832(8) 0.5071(7) -0.1108(5) 0.058(2) Uani 1 1 d U F . H47 H 0.5548 0.4787 -0.0625 0.070 Uiso 1 1 calc R . . C48 C 0.7420(9) 0.4077(8) -0.1104(6) 0.059(2) Uani 1 1 d U . . C49 C 0.6931(8) 0.3336(7) -0.0704(5) 0.058(2) Uani 1 1 d U F . H49 H 0.6086 0.3301 -0.0596 0.069 Uiso 1 1 calc R . . C50 C 0.7623(8) 0.2648(7) -0.0458(5) 0.057(2) Uani 1 1 d U . . H50 H 0.7260 0.2124 -0.0217 0.068 Uiso 1 1 calc R F . C51 C 0.8903(8) 0.2715(8) -0.0560(6) 0.061(2) Uani 1 1 d U F . C52 C 0.9403(8) 0.3447(7) -0.0906(5) 0.053(2) Uani 1 1 d U . . H52 H 1.0255 0.3493 -0.0946 0.063 Uiso 1 1 calc R F . C53 C 0.8716(8) 0.4151(8) -0.1213(5) 0.066(3) Uani 1 1 d U F . H53 H 0.9085 0.4660 -0.1484 0.079 Uiso 1 1 calc R . . C54 C 0.2736(10) 0.8272(9) -0.2635(7) 0.087(4) Uani 1 1 d DU E . H54A H 0.2762 0.8490 -0.2170 0.104 Uiso 1 1 calc R . . H54B H 0.2107 0.7826 -0.2566 0.104 Uiso 1 1 calc R . . C55 C 0.2471(11) 0.8998(8) -0.3300(8) 0.097(4) Uani 1 1 d DU . . H55A H 0.3125 0.9426 -0.3372 0.117 Uiso 1 1 calc R D 1 H55B H 0.2449 0.8769 -0.3759 0.117 Uiso 1 1 calc R D 1 C56A C 0.128(4) 0.942(4) -0.317(3) 0.131(9) Uani 0.68(4) 1 d PDU E 1 H56A H 0.0626 0.8988 -0.3071 0.158 Uiso 0.68(4) 1 calc PR E 1 H56B H 0.1312 0.9680 -0.2728 0.158 Uiso 0.68(4) 1 calc PR E 1 C57A C 0.100(2) 1.0099(18) -0.3847(18) 0.156(10) Uani 0.68(4) 1 d PDU E 1 H57A H 0.1637 1.0541 -0.3926 0.187 Uiso 0.68(4) 1 calc PR E 1 H57B H 0.1027 0.9840 -0.4291 0.187 Uiso 0.68(4) 1 calc PR E 1 C58A C -0.021(2) 1.0516(19) -0.378(2) 0.174(11) Uani 0.68(4) 1 d PDU E 1 H58A H -0.0406 1.0562 -0.3259 0.209 Uiso 0.68(4) 1 calc PR E 1 H58B H -0.0853 1.0184 -0.3945 0.209 Uiso 0.68(4) 1 calc PR E 1 C59A C -0.009(3) 1.1426(18) -0.430(3) 0.214(17) Uani 0.68(4) 1 d PDU E 1 H59A H 0.0635 1.1446 -0.4634 0.321 Uiso 0.68(4) 1 calc PR E 1 H59B H -0.0024 1.1854 -0.3999 0.321 Uiso 0.68(4) 1 calc PR E 1 H59C H -0.0798 1.1542 -0.4604 0.321 Uiso 0.68(4) 1 calc PR E 1 C56B C 0.135(9) 0.952(7) -0.321(6) 0.128(11) Uani 0.32(4) 1 d PDU E 2 H56C H 0.0621 0.9173 -0.3213 0.154 Uiso 0.32(4) 1 calc PR E 2 H56D H 0.1341 0.9694 -0.2719 0.154 Uiso 0.32(4) 1 calc PR E 2 C57B C 0.131(5) 1.031(4) -0.383(4) 0.148(12) Uani 0.32(4) 1 d PDU E 2 H57C H 0.2024 1.0667 -0.3808 0.178 Uiso 0.32(4) 1 calc PR E 2 H57D H 0.1345 1.0139 -0.4312 0.178 Uiso 0.32(4) 1 calc PR E 2 C58B C 0.018(6) 1.084(4) -0.377(3) 0.159(13) Uani 0.32(4) 1 d PDU E 2 H58C H 0.0388 1.1374 -0.3620 0.190 Uiso 0.32(4) 1 calc PR E 2 H58D H -0.0401 1.0518 -0.3388 0.190 Uiso 0.32(4) 1 calc PR E 2 C59B C -0.037(6) 1.103(3) -0.456(4) 0.154(17) Uani 0.32(4) 1 d PDU E 2 H59D H 0.0281 1.1086 -0.4943 0.231 Uiso 0.32(4) 1 calc PR E 2 H59E H -0.0833 1.1553 -0.4618 0.231 Uiso 0.32(4) 1 calc PR E 2 H59F H -0.0898 1.0555 -0.4597 0.231 Uiso 0.32(4) 1 calc PR E 2 C60 C 1.0797(8) 0.2014(7) -0.0477(6) 0.067(3) Uani 1 1 d DU F . H60A H 1.1181 0.2406 -0.0208 0.081 Uiso 1 1 calc R . . H60B H 1.0965 0.2223 -0.1019 0.081 Uiso 1 1 calc R . . C61 C 1.1285(9) 0.1124(7) -0.0234(6) 0.075(3) Uani 1 1 d DU . . H61A H 1.0902 0.0749 -0.0520 0.090 Uiso 1 1 calc R . . H61B H 1.2160 0.1134 -0.0363 0.090 Uiso 1 1 calc R . . C62 C 1.1089(9) 0.0742(7) 0.0585(6) 0.076(3) Uani 1 1 d DU . . H62A H 1.1391 0.1147 0.0872 0.092 Uiso 1 1 calc R . . H62B H 1.0213 0.0672 0.0703 0.092 Uiso 1 1 calc R . . C63 C 1.1688(12) -0.0100(6) 0.0841(7) 0.092(4) Uani 1 1 d DU . . H63A H 1.2572 -0.0026 0.0777 0.111 Uiso 1 1 calc R . . H63B H 1.1445 -0.0498 0.0530 0.111 Uiso 1 1 calc R . . C64 C 1.1343(16) -0.0474(9) 0.1655(7) 0.124(5) Uani 1 1 d DU . . H64A H 1.0476 -0.0621 0.1707 0.149 Uiso 1 1 calc R . . H64B H 1.1483 -0.0045 0.1958 0.149 Uiso 1 1 calc R . . C65 C 1.2102(17) -0.1289(9) 0.1948(9) 0.121(5) Uani 1 1 d DU . . H65A H 1.1925 -0.1726 0.1669 0.181 Uiso 1 1 calc R . . H65B H 1.1896 -0.1504 0.2479 0.181 Uiso 1 1 calc R . . H65C H 1.2961 -0.1147 0.1881 0.181 Uiso 1 1 calc R . . N41 N 0.6779(7) 0.4786(6) -0.1436(4) 0.0573(18) Uani 1 1 d U F . O41 O 0.3886(7) 0.7937(5) -0.2814(4) 0.078(2) Uani 1 1 d U . . O42 O 0.9515(6) 0.1974(5) -0.0307(4) 0.0616(17) Uani 1 1 d U . . C71 C 0.755(3) 0.7215(17) -0.5000(14) 0.165(7) Uani 0.454(15) 1 d PDU F 1 C72 C 0.7243(19) 0.6368(15) -0.4856(10) 0.110(5) Uani 0.454(15) 1 d PDU F 1 C73 C 0.7514(17) 0.5867(14) -0.4131(10) 0.081(5) Uani 0.454(15) 1 d PDU F 1 C74 C 0.826(2) 0.5207(17) -0.4143(12) 0.087(6) Uani 0.454(15) 1 d PDU F 1 H74 H 0.8572 0.5143 -0.4618 0.104 Uiso 0.454(15) 1 calc PR F 1 C75 C 0.861(2) 0.4606(17) -0.3526(12) 0.093(7) Uani 0.454(15) 1 d PDU F 1 C76 C 0.954(3) 0.390(2) -0.3618(14) 0.106(8) Uani 0.454(15) 1 d PDU F 1 H76A H 0.9087 0.3430 -0.3754 0.127 Uiso 0.454(15) 1 calc PR F 1 H76B H 1.0089 0.4135 -0.4051 0.127 Uiso 0.454(15) 1 calc PR F 1 C77 C 1.028(4) 0.352(3) -0.3012(13) 0.119(12) Uani 0.454(15) 1 d PDU F 1 H77A H 1.0661 0.3972 -0.2817 0.179 Uiso 0.454(15) 1 calc PR F 1 H77B H 1.0907 0.3173 -0.3194 0.179 Uiso 0.454(15) 1 calc PR F 1 H77C H 0.9783 0.3165 -0.2615 0.179 Uiso 0.454(15) 1 calc PR F 1 O71 O 0.6958(16) 0.6067(12) -0.3571(8) 0.087(6) Uani 0.454(15) 1 d PDU F 1 O72 O 0.833(2) 0.4616(16) -0.2841(12) 0.073(6) Uani 0.454(15) 1 d PDU F 1 F71 F 0.730(4) 0.750(3) -0.5724(13) 0.207(13) Uani 0.454(15) 1 d PDU F 1 F72 F 0.875(3) 0.711(2) -0.485(2) 0.194(11) Uani 0.454(15) 1 d PDU F 1 F73 F 0.686(4) 0.750(2) -0.4464(16) 0.215(13) Uani 0.454(15) 1 d PDU F 1 F74 F 0.759(2) 0.6032(18) -0.5486(10) 0.147(9) Uani 0.454(15) 1 d PDU F 1 F75 F 0.6007(15) 0.644(2) -0.4956(9) 0.150(9) Uani 0.454(15) 1 d PDU F 1 C171 C 0.726(2) 0.7357(17) -0.4899(13) 0.164(7) Uani 0.546(15) 1 d PDU F 2 C172 C 0.787(2) 0.6586(14) -0.4792(11) 0.135(5) Uani 0.546(15) 1 d PDU F 2 C173 C 0.8016(19) 0.6082(14) -0.4052(10) 0.100(6) Uani 0.546(15) 1 d PDU F 2 C174 C 0.886(2) 0.5473(17) -0.4015(13) 0.117(7) Uani 0.546(15) 1 d PDU F 2 H174 H 0.9381 0.5501 -0.4448 0.140 Uiso 0.546(15) 1 calc PR F 2 C175 C 0.907(2) 0.4806(16) -0.3415(13) 0.103(7) Uani 0.546(15) 1 d PDU F 2 C176 C 1.008(3) 0.412(2) -0.3420(17) 0.142(11) Uani 0.546(15) 1 d PDU F 2 H17C H 0.9921 0.3799 -0.3810 0.170 Uiso 0.546(15) 1 calc PR F 2 H17D H 1.0864 0.4412 -0.3553 0.170 Uiso 0.546(15) 1 calc PR F 2 C177 C 1.016(5) 0.352(3) -0.2709(19) 0.175(15) Uani 0.546(15) 1 d PDU F 2 H17E H 0.9587 0.3055 -0.2682 0.263 Uiso 0.546(15) 1 calc PR F 2 H17F H 0.9974 0.3813 -0.2301 0.263 Uiso 0.546(15) 1 calc PR F 2 H17G H 1.0980 0.3291 -0.2667 0.263 Uiso 0.546(15) 1 calc PR F 2 O171 O 0.7263(17) 0.6179(11) -0.3541(7) 0.087(5) Uani 0.546(15) 1 d PDU F 2 O172 O 0.851(2) 0.4701(15) -0.2766(11) 0.085(5) Uani 0.546(15) 1 d PDU F 2 F171 F 0.738(4) 0.768(2) -0.5654(12) 0.218(12) Uani 0.546(15) 1 d PDU F 2 F172 F 0.8152(19) 0.7674(12) -0.4531(8) 0.133(7) Uani 0.546(15) 1 d PDU F 2 F173 F 0.6140(19) 0.708(2) -0.4656(16) 0.196(11) Uani 0.546(15) 1 d PDU F 2 F174 F 0.897(2) 0.6787(18) -0.5220(11) 0.198(10) Uani 0.546(15) 1 d PDU F 2 F175 F 0.712(3) 0.6198(18) -0.5225(14) 0.216(10) Uani 0.546(15) 1 d PDU F 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 0.0478(5) 0.0624(6) 0.0519(5) -0.0191(4) 0.0112(3) -0.0126(3) Pd2 0.0667(6) 0.0996(8) 0.0456(5) -0.0213(5) 0.0163(4) -0.0034(5) C1 0.041(5) 0.067(6) 0.052(4) -0.012(4) 0.018(4) -0.014(4) C2 0.047(5) 0.062(6) 0.047(4) -0.020(4) 0.004(4) -0.019(4) C3 0.051(5) 0.069(6) 0.052(4) -0.032(4) 0.011(4) -0.016(4) C4 0.051(5) 0.071(6) 0.045(5) -0.014(4) 0.007(4) -0.019(4) C5 0.041(5) 0.060(6) 0.058(5) -0.019(4) 0.000(4) -0.013(4) C6 0.052(5) 0.058(6) 0.053(5) -0.014(4) 0.008(4) -0.017(4) C7 0.043(5) 0.067(6) 0.056(5) -0.027(4) 0.006(4) -0.016(4) C8 0.048(5) 0.059(5) 0.052(5) -0.018(4) 0.012(4) -0.013(4) C9 0.041(5) 0.080(6) 0.059(6) -0.030(5) 0.009(4) -0.014(4) C10 0.054(6) 0.065(6) 0.066(6) -0.021(5) 0.016(4) -0.006(4) C11 0.052(5) 0.060(6) 0.067(6) -0.014(5) 0.016(4) -0.008(4) C12 0.065(6) 0.074(7) 0.051(6) -0.009(5) 0.019(4) -0.011(5) C13 0.057(6) 0.064(6) 0.044(5) -0.014(4) 0.011(4) -0.007(4) C14 0.059(6) 0.073(7) 0.071(6) -0.010(5) -0.001(5) -0.010(5) C15 0.065(6) 0.066(7) 0.072(6) -0.012(5) 0.010(5) -0.009(5) C16 0.058(6) 0.085(8) 0.068(6) -0.010(5) 0.001(5) 0.003(5) C17 0.076(7) 0.093(9) 0.071(7) -0.022(6) 0.009(6) 0.018(6) C18 0.139(12) 0.107(11) 0.086(8) -0.004(7) 0.006(9) 0.056(9) C19 0.115(12) 0.193(18) 0.085(10) -0.013(10) -0.001(9) 0.088(12) C20 0.071(7) 0.099(8) 0.052(6) -0.011(6) 0.016(4) 0.008(6) C21 0.081(8) 0.094(9) 0.082(7) -0.028(7) 0.000(6) 0.020(6) C22 0.144(12) 0.109(10) 0.080(8) -0.006(8) -0.014(8) 0.037(8) C23A 0.145(17) 0.118(15) 0.079(12) -0.015(12) 0.002(13) 0.047(13) C24A 0.21(2) 0.130(17) 0.093(14) 0.001(13) -0.001(16) 0.077(15) C25A 0.19(3) 0.15(3) 0.10(2) -0.055(17) -0.05(2) 0.08(2) C23B 0.158(18) 0.115(13) 0.074(15) -0.006(13) -0.014(13) 0.049(11) C24B 0.18(2) 0.116(12) 0.078(17) -0.014(15) 0.001(16) 0.041(13) C25B 0.18(3) 0.112(17) 0.06(2) 0.003(17) 0.046(19) 0.04(2) N1 0.038(4) 0.070(5) 0.048(4) -0.017(3) 0.007(3) -0.012(3) O1 0.052(4) 0.068(4) 0.054(4) -0.007(3) 0.000(3) -0.008(3) O2 0.071(5) 0.068(5) 0.064(4) -0.003(4) 0.011(3) 0.001(3) C31A 0.112(12) 0.164(16) 0.085(14) 0.033(11) -0.008(10) 0.010(10) C32A 0.100(10) 0.132(11) 0.055(8) 0.000(8) 0.000(8) -0.009(8) C33A 0.071(10) 0.098(10) 0.052(7) -0.009(8) 0.012(8) -0.003(8) C34A 0.075(11) 0.074(11) 0.060(10) -0.019(8) 0.025(9) -0.024(8) C35A 0.069(10) 0.067(11) 0.064(8) -0.032(7) 0.016(7) -0.015(7) C36A 0.086(12) 0.082(12) 0.074(10) -0.053(9) 0.015(8) -0.010(8) C37A 0.10(2) 0.11(2) 0.098(15) -0.046(14) 0.021(16) 0.030(14) O31A 0.074(13) 0.090(13) 0.071(8) -0.001(9) 0.026(9) 0.009(10) O32A 0.052(8) 0.081(10) 0.051(6) -0.028(6) 0.009(6) -0.009(6) F31A 0.30(3) 0.26(2) 0.167(16) 0.052(15) 0.083(19) 0.17(2) F32A 0.177(18) 0.209(18) 0.119(12) 0.071(13) -0.019(11) 0.012(14) F33A 0.195(19) 0.228(17) 0.20(2) 0.078(13) -0.131(16) -0.096(15) F34A 0.200(18) 0.125(11) 0.205(19) 0.050(10) -0.066(16) -0.041(12) F35A 0.27(2) 0.25(2) 0.062(8) 0.032(10) 0.063(12) 0.121(17) C31B 0.075(13) 0.107(14) 0.111(15) -0.046(9) 0.015(8) 0.006(7) C32B 0.082(13) 0.114(12) 0.090(12) -0.058(8) 0.009(7) 0.007(8) C33B 0.058(10) 0.064(10) 0.064(9) -0.036(7) 0.008(7) -0.023(8) C34B 0.083(13) 0.080(12) 0.059(11) -0.022(9) 0.020(11) -0.022(10) C35B 0.077(12) 0.089(11) 0.053(9) -0.007(9) 0.007(9) -0.005(9) C36B 0.089(14) 0.112(14) 0.070(12) 0.006(10) 0.010(12) -0.006(11) C37B 0.12(2) 0.12(2) 0.11(2) 0.038(19) 0.02(2) 0.023(16) O31B 0.058(11) 0.060(10) 0.056(8) -0.032(7) 0.007(8) -0.015(8) O32B 0.056(12) 0.074(12) 0.055(7) -0.023(7) -0.008(8) -0.010(9) F31B 0.20(2) 0.133(19) 0.18(2) -0.064(15) 0.041(15) 0.067(15) F32B 0.130(14) 0.046(9) 0.24(2) -0.040(9) 0.054(13) 0.008(7) F33B 0.084(12) 0.105(14) 0.095(12) -0.013(10) 0.000(9) -0.015(9) F34B 0.185(18) 0.160(18) 0.24(2) -0.171(18) -0.100(15) 0.078(12) F35B 0.182(17) 0.175(19) 0.143(17) 0.006(12) 0.102(14) 0.078(12) C41 0.050(5) 0.083(7) 0.039(4) -0.021(4) 0.004(3) -0.010(4) C42 0.044(5) 0.084(7) 0.044(4) -0.027(4) 0.005(4) -0.014(4) C43 0.038(5) 0.098(7) 0.050(5) -0.023(5) 0.010(4) -0.025(4) C44 0.038(5) 0.092(7) 0.059(5) -0.021(5) 0.009(4) -0.013(4) C45 0.056(6) 0.075(7) 0.065(6) -0.018(5) 0.004(5) -0.008(4) C46 0.063(6) 0.085(7) 0.055(6) -0.015(5) 0.014(5) -0.013(4) C47 0.043(5) 0.091(7) 0.043(5) -0.019(4) 0.008(4) -0.024(4) C48 0.051(4) 0.078(6) 0.054(5) -0.027(4) 0.008(4) -0.019(4) C49 0.037(4) 0.086(6) 0.055(6) -0.026(5) 0.004(4) -0.011(4) C50 0.047(4) 0.072(6) 0.051(5) -0.016(5) 0.014(4) -0.026(4) C51 0.040(4) 0.090(6) 0.059(6) -0.027(5) 0.003(4) -0.009(4) C52 0.033(4) 0.074(6) 0.057(6) -0.030(5) 0.013(4) -0.019(4) C53 0.042(4) 0.112(7) 0.042(5) -0.013(5) 0.000(4) -0.017(4) C54 0.053(6) 0.101(9) 0.099(9) -0.005(7) 0.002(6) 0.000(5) C55 0.086(7) 0.076(8) 0.117(10) 0.005(7) 0.007(7) -0.008(5) C56A 0.069(11) 0.088(15) 0.211(17) 0.029(12) -0.007(11) -0.008(11) C57A 0.090(13) 0.099(16) 0.241(18) 0.050(13) -0.008(14) -0.012(11) C58A 0.078(14) 0.126(19) 0.28(2) 0.056(17) -0.021(16) -0.010(12) C59A 0.18(3) 0.09(2) 0.33(4) 0.04(2) -0.05(3) 0.011(18) C56B 0.066(16) 0.092(19) 0.20(2) 0.022(15) -0.011(16) -0.007(13) C57B 0.090(19) 0.091(19) 0.23(2) 0.032(16) -0.011(18) -0.013(16) C58B 0.09(2) 0.10(2) 0.25(2) 0.04(2) -0.03(2) -0.005(16) C59B 0.15(3) 0.04(3) 0.27(3) -0.01(3) -0.07(3) 0.00(3) C60 0.046(5) 0.078(6) 0.086(7) -0.038(5) 0.007(5) -0.010(5) C61 0.044(5) 0.078(7) 0.112(7) -0.042(6) 0.014(5) -0.017(4) C62 0.050(6) 0.085(7) 0.103(7) -0.041(5) -0.007(6) -0.003(5) C63 0.099(9) 0.070(7) 0.120(8) -0.042(6) -0.022(8) -0.019(6) C64 0.177(15) 0.101(10) 0.108(8) -0.040(7) -0.052(10) 0.014(9) C65 0.155(15) 0.077(10) 0.137(12) -0.036(8) -0.021(11) 0.009(9) N41 0.048(4) 0.083(5) 0.044(4) -0.020(3) 0.002(3) -0.017(3) O41 0.067(4) 0.088(6) 0.074(5) -0.009(4) 0.022(4) -0.005(4) O42 0.046(3) 0.068(4) 0.076(5) -0.026(4) 0.004(3) -0.021(3) C71 0.213(15) 0.186(13) 0.084(12) -0.007(11) 0.012(14) 0.009(15) C72 0.110(11) 0.194(12) 0.035(7) -0.044(9) -0.017(11) 0.021(11) C73 0.053(11) 0.155(13) 0.039(6) -0.032(8) 0.011(7) -0.001(9) C74 0.078(14) 0.149(15) 0.042(8) -0.043(9) 0.000(10) 0.003(11) C75 0.087(15) 0.151(15) 0.050(8) -0.042(9) 0.005(10) 0.021(11) C76 0.092(17) 0.181(19) 0.061(12) -0.065(12) 0.002(11) 0.038(14) C77 0.23(3) 0.10(2) 0.018(12) 0.004(15) 0.023(14) 0.09(2) O71 0.058(11) 0.158(15) 0.042(6) -0.017(8) 0.012(7) 0.023(10) O72 0.068(11) 0.111(13) 0.046(7) -0.035(8) 0.003(7) 0.009(9) F71 0.29(3) 0.24(3) 0.075(11) -0.001(15) -0.001(16) 0.03(3) F72 0.224(16) 0.17(2) 0.19(3) -0.04(2) -0.046(18) -0.040(16) F73 0.33(3) 0.21(2) 0.111(15) -0.069(17) 0.01(2) 0.04(3) F74 0.149(16) 0.27(2) 0.035(8) -0.059(12) 0.040(9) -0.020(16) F75 0.100(10) 0.30(3) 0.029(8) 0.003(13) -0.010(8) 0.039(12) C171 0.188(13) 0.198(14) 0.092(12) 0.001(11) -0.005(11) 0.018(12) C172 0.201(13) 0.136(12) 0.063(8) -0.017(9) 0.041(9) -0.018(11) C173 0.106(14) 0.143(14) 0.055(7) -0.039(8) 0.031(8) 0.007(10) C174 0.118(16) 0.155(16) 0.080(11) -0.040(10) 0.030(12) 0.008(11) C175 0.104(14) 0.148(14) 0.069(10) -0.054(9) 0.010(9) 0.023(11) C176 0.16(2) 0.16(2) 0.120(19) -0.070(14) 0.048(16) 0.045(16) C177 0.22(3) 0.20(3) 0.13(2) -0.088(19) -0.07(3) 0.12(3) O171 0.075(10) 0.135(12) 0.045(6) -0.013(6) 0.029(6) -0.020(8) O172 0.074(10) 0.130(12) 0.067(8) -0.063(8) 0.008(7) 0.007(8) F171 0.32(3) 0.24(3) 0.077(11) 0.006(14) -0.021(13) 0.03(2) F172 0.205(16) 0.137(13) 0.054(8) -0.031(8) 0.069(9) -0.050(13) F173 0.168(12) 0.25(3) 0.15(2) 0.032(19) -0.057(12) 0.002(13) F174 0.273(17) 0.22(2) 0.094(13) -0.041(12) 0.114(14) 0.006(15) F175 0.28(2) 0.28(2) 0.106(18) -0.077(17) -0.052(17) 0.04(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 C1 1.980(10) . ? Pd1 O32A 2.003(13) . ? Pd1 N1 2.031(8) . ? Pd1 O31B 2.034(15) . ? Pd1 O32B 2.061(15) . ? Pd1 O31A 2.093(13) . ? Pd2 C41 1.973(10) . ? Pd2 O71 2.008(15) . ? Pd2 O171 2.015(13) . ? Pd2 N41 2.044(8) . ? Pd2 O72 2.079(15) . ? Pd2 O172 2.088(14) . ? C1 C6 1.387(14) . ? C1 C2 1.393(13) . ? C2 C3 1.426(13) . ? C2 C7 1.429(14) . ? C3 C4 1.396(14) . ? C3 H3 0.9500 . ? C4 C5 1.374(13) . ? C4 H4 0.9500 . ? C5 O1 1.346(12) . ? C5 C6 1.430(14) . ? C6 H6 0.9500 . ? C7 N1 1.301(12) . ? C7 H7 0.9500 . ? C8 C13 1.393(13) . ? C8 C9 1.398(14) . ? C8 N1 1.431(13) . ? C9 C10 1.381(14) . ? C9 H9 0.9500 . ? C10 C11 1.384(14) . ? C10 H10 0.9500 . ? C11 O2 1.326(12) . ? C11 C12 1.393(15) . ? C12 C13 1.350(14) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O1 1.419(12) . ? C14 C15 1.541(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.520(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.521(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.521(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.564(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O2 1.451(13) . ? C20 C21 1.519(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.511(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23B 1.514(10) . ? C22 C23A 1.524(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23A C24A 1.514(9) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A C25A 1.575(13) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C23B C24B 1.517(10) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B C25B 1.571(14) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C31A F31A 1.356(15) . ? C31A F33A 1.357(16) . ? C31A F32A 1.375(15) . ? C31A C32A 1.391(19) . ? C32A F35A 1.396(15) . ? C32A F34A 1.404(15) . ? C32A C33A 1.442(17) . ? C33A O31A 1.272(17) . ? C33A C34A 1.37(2) . ? C34A C35A 1.42(2) . ? C34A H34A 0.9500 . ? C35A O32A 1.289(18) . ? C35A C36A 1.57(2) . ? C36A C37A 1.443(19) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? C31B F33B 1.34(2) . ? C31B F32B 1.37(2) . ? C31B F31B 1.379(19) . ? C31B C32B 1.39(2) . ? C32B F35B 1.412(19) . ? C32B F34B 1.427(18) . ? C32B C33B 1.45(2) . ? C33B O31B 1.268(18) . ? C33B C34B 1.37(2) . ? C34B C35B 1.41(2) . ? C34B H34B 0.9500 . ? C35B O32B 1.285(19) . ? C35B C36B 1.57(2) . ? C36B C37B 1.455(13) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C41 C46 1.302(15) . ? C41 C42 1.419(14) . ? C42 C43 1.399(14) . ? C42 C47 1.420(15) . ? C43 C44 1.323(15) . ? C43 H43 0.9500 . ? C44 C45 1.406(15) . ? C44 H44 0.9500 . ? C45 O41 1.335(13) . ? C45 C46 1.435(15) . ? C46 H46 0.9500 . ? C47 N41 1.315(12) . ? C47 H47 0.9500 . ? C48 C49 1.365(15) . ? C48 N41 1.386(14) . ? C48 C53 1.448(14) . ? C49 C50 1.355(14) . ? C49 H49 0.9500 . ? C50 C51 1.429(13) . ? C50 H50 0.9500 . ? C51 C52 1.327(15) . ? C51 O42 1.374(13) . ? C52 C53 1.396(15) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 O41 1.435(13) . ? C54 C55 1.542(12) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56A 1.521(12) . ? C55 C56B 1.528(19) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56A C57A 1.516(13) . ? C56A H56A 0.9900 . ? C56A H56B 0.9900 . ? C57A C58A 1.515(12) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C58A C59A 1.577(16) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C59A H59A 0.9800 . ? C59A H59B 0.9800 . ? C59A H59C 0.9800 . ? C56B C57B 1.517(13) . ? C56B H56C 0.9900 . ? C56B H56D 0.9900 . ? C57B C58B 1.516(13) . ? C57B H57C 0.9900 . ? C57B H57D 0.9900 . ? C58B C59B 1.572(16) . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? C59B H59D 0.9800 . ? C59B H59E 0.9800 . ? C59B H59F 0.9800 . ? C60 O42 1.444(11) . ? C60 C61 1.514(12) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.506(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.501(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.522(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.569(13) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C71 F71 1.357(19) . ? C71 F73 1.37(2) . ? C71 F72 1.38(2) . ? C71 C72 1.38(2) . ? C72 F75 1.398(19) . ? C72 F74 1.412(18) . ? C72 C73 1.449(19) . ? C73 O71 1.273(16) . ? C73 C74 1.34(2) . ? C74 C75 1.40(2) . ? C74 H74 0.9500 . ? C75 O72 1.287(17) . ? C75 C76 1.56(2) . ? C76 C77 1.44(2) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C171 F173 1.35(2) . ? C171 F171 1.376(19) . ? C171 F172 1.39(2) . ? C171 C172 1.39(2) . ? C172 F175 1.41(2) . ? C172 F174 1.419(19) . ? C172 C173 1.447(19) . ? C173 O171 1.261(16) . ? C173 C174 1.35(2) . ? C174 C175 1.39(2) . ? C174 H174 0.9500 . ? C175 O172 1.293(17) . ? C175 C176 1.57(2) . ? C176 C177 1.46(2) . ? C176 H17C 0.9900 . ? C176 H17D 0.9900 . ? C177 H17E 0.9800 . ? C177 H17F 0.9800 . ? C177 H17G 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 O32A 91.4(7) . . ? C1 Pd1 N1 81.1(4) . . ? O32A Pd1 N1 170.7(6) . . ? C1 Pd1 O31B 91.2(8) . . ? O32A Pd1 O31B 7.6(10) . . ? N1 Pd1 O31B 172.1(8) . . ? C1 Pd1 O32B 176.1(7) . . ? O32A Pd1 O32B 90.2(12) . . ? N1 Pd1 O32B 96.9(8) . . ? O31B Pd1 O32B 90.9(8) . . ? C1 Pd1 O31A 176.7(7) . . ? O32A Pd1 O31A 91.6(7) . . ? N1 Pd1 O31A 95.7(7) . . ? O31B Pd1 O31A 92.0(12) . . ? O32B Pd1 O31A 2.6(11) . . ? C41 Pd2 O71 89.2(6) . . ? C41 Pd2 O171 92.6(6) . . ? O71 Pd2 O171 11.3(7) . . ? C41 Pd2 N41 82.1(4) . . ? O71 Pd2 N41 166.9(5) . . ? O171 Pd2 N41 174.6(6) . . ? C41 Pd2 O72 173.1(9) . . ? O71 Pd2 O72 90.4(7) . . ? O171 Pd2 O72 88.3(9) . . ? N41 Pd2 O72 97.1(7) . . ? C41 Pd2 O172 177.4(7) . . ? O71 Pd2 O172 93.1(9) . . ? O171 Pd2 O172 89.5(7) . . ? N41 Pd2 O172 95.7(6) . . ? O72 Pd2 O172 8.4(15) . . ? C6 C1 C2 121.3(9) . . ? C6 C1 Pd1 125.8(7) . . ? C2 C1 Pd1 112.9(8) . . ? C1 C2 C3 119.9(9) . . ? C1 C2 C7 115.1(9) . . ? C3 C2 C7 125.0(9) . . ? C4 C3 C2 118.8(9) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 120.6(9) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? O1 C5 C4 124.5(9) . . ? O1 C5 C6 114.2(9) . . ? C4 C5 C6 121.2(10) . . ? C1 C6 C5 118.0(9) . . ? C1 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? N1 C7 C2 116.8(9) . . ? N1 C7 H7 121.6 . . ? C2 C7 H7 121.6 . . ? C13 C8 C9 119.2(9) . . ? C13 C8 N1 119.9(9) . . ? C9 C8 N1 120.9(9) . . ? C10 C9 C8 119.6(9) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.5(10) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? O2 C11 C10 116.6(10) . . ? O2 C11 C12 126.3(10) . . ? C10 C11 C12 117.1(10) . . ? C13 C12 C11 122.9(10) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C8 119.6(10) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? O1 C14 C15 106.3(8) . . ? O1 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? O1 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C16 C15 C14 111.2(8) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.3(8) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 111.7(8) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 108.9(9) . . ? C17 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 C21 105.8(9) . . ? O2 C20 H20A 110.6 . . ? C21 C20 H20A 110.6 . . ? O2 C20 H20B 110.6 . . ? C21 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? C22 C21 C20 112.1(8) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23B 111.0(9) . . ? C21 C22 C23A 109.4(8) . . ? C23B C22 C23A 10.2(18) . . ? C21 C22 H22A 109.8 . . ? C23B C22 H22A 117.2 . . ? C23A C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? C23B C22 H22B 100.2 . . ? C23A C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C24A C23A C22 110.7(9) . . ? C24A C23A H23A 109.5 . . ? C22 C23A H23A 109.5 . . ? C24A C23A H23B 109.5 . . ? C22 C23A H23B 109.5 . . ? H23A C23A H23B 108.1 . . ? C23A C24A C25A 106.9(9) . . ? C23A C24A H24A 110.3 . . ? C25A C24A H24A 110.3 . . ? C23A C24A H24B 110.3 . . ? C25A C24A H24B 110.3 . . ? H24A C24A H24B 108.6 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C22 C23B C24B 110.4(9) . . ? C22 C23B H23C 109.6 . . ? C24B C23B H23C 109.6 . . ? C22 C23B H23D 109.6 . . ? C24B C23B H23D 109.6 . . ? H23C C23B H23D 108.1 . . ? C23B C24B C25B 107.1(10) . . ? C23B C24B H24C 110.3 . . ? C25B C24B H24C 110.3 . . ? C23B C24B H24D 110.3 . . ? C25B C24B H24D 110.3 . . ? H24C C24B H24D 108.6 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C7 N1 C8 119.1(8) . . ? C7 N1 Pd1 113.8(7) . . ? C8 N1 Pd1 127.0(6) . . ? C5 O1 C14 116.1(8) . . ? C11 O2 C20 117.2(8) . . ? F31A C31A F33A 119.1(18) . . ? F31A C31A F32A 107.5(16) . . ? F33A C31A F32A 114.1(16) . . ? F31A C31A C32A 106.6(16) . . ? F33A C31A C32A 103.1(15) . . ? F32A C31A C32A 105.3(14) . . ? C31A C32A F35A 101.9(13) . . ? C31A C32A F34A 106.0(14) . . ? F35A C32A F34A 105.3(16) . . ? C31A C32A C33A 119.9(14) . . ? F35A C32A C33A 110.0(13) . . ? F34A C32A C33A 112.4(13) . . ? O31A C33A C34A 122.9(17) . . ? O31A C33A C32A 117.9(15) . . ? C34A C33A C32A 118.9(16) . . ? C33A C34A C35A 128.1(15) . . ? C33A C34A H34A 116.0 . . ? C35A C34A H34A 116.0 . . ? O32A C35A C34A 128.4(17) . . ? O32A C35A C36A 109.4(15) . . ? C34A C35A C36A 122.2(16) . . ? C37A C36A C35A 116.4(16) . . ? C37A C36A H36A 108.2 . . ? C35A C36A H36A 108.2 . . ? C37A C36A H36B 108.2 . . ? C35A C36A H36B 108.2 . . ? H36A C36A H36B 107.3 . . ? C36A C37A H37A 109.5 . . ? C36A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C36A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C33A O31A Pd1 126.2(15) . . ? C35A O32A Pd1 122.5(14) . . ? F33B C31B F32B 122(2) . . ? F33B C31B F31B 119(2) . . ? F32B C31B F31B 105.7(19) . . ? F33B C31B C32B 102.3(18) . . ? F32B C31B C32B 101.7(18) . . ? F31B C31B C32B 102.2(18) . . ? C31B C32B F35B 96.1(16) . . ? C31B C32B F34B 105.2(17) . . ? F35B C32B F34B 109.5(19) . . ? C31B C32B C33B 121.5(17) . . ? F35B C32B C33B 111.8(16) . . ? F34B C32B C33B 111.5(15) . . ? O31B C33B C34B 125.5(19) . . ? O31B C33B C32B 118.0(17) . . ? C34B C33B C32B 116.4(19) . . ? C33B C34B C35B 126.1(17) . . ? C33B C34B H34B 116.9 . . ? C35B C34B H34B 116.9 . . ? O32B C35B C34B 128(2) . . ? O32B C35B C36B 110.4(17) . . ? C34B C35B C36B 121.7(19) . . ? C37B C36B C35B 116.9(19) . . ? C37B C36B H36C 108.1 . . ? C35B C36B H36C 108.1 . . ? C37B C36B H36D 108.1 . . ? C35B C36B H36D 108.1 . . ? H36C C36B H36D 107.3 . . ? C36B C37B H37D 109.5 . . ? C36B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C36B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C33B O31B Pd1 126.6(17) . . ? C35B O32B Pd1 122.1(17) . . ? C46 C41 C42 120.7(10) . . ? C46 C41 Pd2 126.5(8) . . ? C42 C41 Pd2 112.8(8) . . ? C43 C42 C41 118.3(10) . . ? C43 C42 C47 127.6(9) . . ? C41 C42 C47 114.1(9) . . ? C44 C43 C42 122.1(10) . . ? C44 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? C43 C44 C45 119.4(10) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? O41 C45 C44 124.5(10) . . ? O41 C45 C46 116.7(10) . . ? C44 C45 C46 118.8(11) . . ? C41 C46 C45 120.7(10) . . ? C41 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? N41 C47 C42 118.9(9) . . ? N41 C47 H47 120.6 . . ? C42 C47 H47 120.6 . . ? C49 C48 N41 125.6(9) . . ? C49 C48 C53 119.1(10) . . ? N41 C48 C53 115.3(10) . . ? C50 C49 C48 121.4(9) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C49 C50 C51 119.8(10) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 O42 125.4(9) . . ? C52 C51 C50 119.7(10) . . ? O42 C51 C50 114.9(10) . . ? C51 C52 C53 122.1(9) . . ? C51 C52 H52 118.9 . . ? C53 C52 H52 118.9 . . ? C52 C53 C48 117.6(10) . . ? C52 C53 H53 121.2 . . ? C48 C53 H53 121.2 . . ? O41 C54 C55 105.9(9) . . ? O41 C54 H54A 110.5 . . ? C55 C54 H54A 110.5 . . ? O41 C54 H54B 110.5 . . ? C55 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? C56A C55 C56B 7(7) . . ? C56A C55 C54 111.0(11) . . ? C56B C55 C54 116(2) . . ? C56A C55 H55A 109.4 . . ? C56B C55 H55A 102.8 . . ? C54 C55 H55A 109.4 . . ? C56A C55 H55B 109.4 . . ? C56B C55 H55B 110.6 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C57A C56A C55 110.1(13) . . ? C57A C56A H56A 109.6 . . ? C55 C56A H56A 109.6 . . ? C57A C56A H56B 109.6 . . ? C55 C56A H56B 109.6 . . ? H56A C56A H56B 108.2 . . ? C58A C57A C56A 113.4(15) . . ? C58A C57A H57A 108.9 . . ? C56A C57A H57A 108.9 . . ? C58A C57A H57B 108.9 . . ? C56A C57A H57B 108.9 . . ? H57A C57A H57B 107.7 . . ? C57A C58A C59A 105.4(14) . . ? C57A C58A H58A 110.7 . . ? C59A C58A H58A 110.7 . . ? C57A C58A H58B 110.7 . . ? C59A C58A H58B 110.7 . . ? H58A C58A H58B 108.8 . . ? C58A C59A H59A 109.5 . . ? C58A C59A H59B 109.5 . . ? H59A C59A H59B 109.5 . . ? C58A C59A H59C 109.5 . . ? H59A C59A H59C 109.5 . . ? H59B C59A H59C 109.5 . . ? C57B C56B C55 111(2) . . ? C57B C56B H56C 109.4 . . ? C55 C56B H56C 109.4 . . ? C57B C56B H56D 109.4 . . ? C55 C56B H56D 109.4 . . ? H56C C56B H56D 108.0 . . ? C58B C57B C56B 112.7(18) . . ? C58B C57B H57C 109.1 . . ? C56B C57B H57C 109.1 . . ? C58B C57B H57D 109.0 . . ? C56B C57B H57D 109.0 . . ? H57C C57B H57D 107.8 . . ? C57B C58B C59B 107.1(18) . . ? C57B C58B H58C 110.3 . . ? C59B C58B H58C 110.3 . . ? C57B C58B H58D 110.3 . . ? C59B C58B H58D 110.3 . . ? H58C C58B H58D 108.6 . . ? C58B C59B H59D 109.5 . . ? C58B C59B H59E 109.5 . . ? H59D C59B H59E 109.5 . . ? C58B C59B H59F 109.5 . . ? H59D C59B H59F 109.5 . . ? H59E C59B H59F 109.5 . . ? O42 C60 C61 107.3(8) . . ? O42 C60 H60A 110.3 . . ? C61 C60 H60A 110.3 . . ? O42 C60 H60B 110.3 . . ? C61 C60 H60B 110.3 . . ? H60A C60 H60B 108.5 . . ? C62 C61 C60 114.9(9) . . ? C62 C61 H61A 108.5 . . ? C60 C61 H61A 108.5 . . ? C62 C61 H61B 108.5 . . ? C60 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? C63 C62 C61 114.9(9) . . ? C63 C62 H62A 108.6 . . ? C61 C62 H62A 108.6 . . ? C63 C62 H62B 108.6 . . ? C61 C62 H62B 108.6 . . ? H62A C62 H62B 107.5 . . ? C62 C63 C64 111.0(10) . . ? C62 C63 H63A 109.4 . . ? C64 C63 H63A 109.4 . . ? C62 C63 H63B 109.4 . . ? C64 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C63 C64 C65 110.7(11) . . ? C63 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C47 N41 C48 123.0(9) . . ? C47 N41 Pd2 111.8(7) . . ? C48 N41 Pd2 125.0(7) . . ? C45 O41 C54 118.3(9) . . ? C51 O42 C60 115.1(8) . . ? F71 C71 F73 118(2) . . ? F71 C71 F72 116(2) . . ? F73 C71 F72 115(2) . . ? F71 C71 C72 104(2) . . ? F73 C71 C72 102(2) . . ? F72 C71 C72 97.5(19) . . ? C71 C72 F75 99.5(19) . . ? C71 C72 F74 108.7(19) . . ? F75 C72 F74 99.1(16) . . ? C71 C72 C73 117.0(16) . . ? F75 C72 C73 112.5(15) . . ? F74 C72 C73 117.3(17) . . ? O71 C73 C74 128.2(17) . . ? O71 C73 C72 116.4(16) . . ? C74 C73 C72 115.3(16) . . ? C73 C74 C75 126.5(16) . . ? C73 C74 H74 116.8 . . ? C75 C74 H74 116.8 . . ? O72 C75 C74 125.4(18) . . ? O72 C75 C76 113.2(16) . . ? C74 C75 C76 121.1(17) . . ? C77 C76 C75 120.6(18) . . ? C77 C76 H76A 107.2 . . ? C75 C76 H76A 107.2 . . ? C77 C76 H76B 107.2 . . ? C75 C76 H76B 107.2 . . ? H76A C76 H76B 106.8 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 O71 Pd2 125.2(14) . . ? C75 O72 Pd2 123.8(15) . . ? F173 C171 F171 114(2) . . ? F173 C171 F172 130(2) . . ? F171 C171 F172 110(2) . . ? F173 C171 C172 100(2) . . ? F171 C171 C172 105(2) . . ? F172 C171 C172 88.7(16) . . ? C171 C172 F175 96.1(18) . . ? C171 C172 F174 103.6(18) . . ? F175 C172 F174 106.3(18) . . ? C171 C172 C173 121.1(17) . . ? F175 C172 C173 113.4(17) . . ? F174 C172 C173 114.1(16) . . ? O171 C173 C174 127.0(18) . . ? O171 C173 C172 118.0(16) . . ? C174 C173 C172 114.4(16) . . ? C173 C174 C175 127.3(17) . . ? C173 C174 H174 116.3 . . ? C175 C174 H174 116.3 . . ? O172 C175 C174 125.0(17) . . ? O172 C175 C176 110.8(16) . . ? C174 C175 C176 124.1(17) . . ? C177 C176 C175 113.6(18) . . ? C177 C176 H17C 108.8 . . ? C175 C176 H17C 108.8 . . ? C177 C176 H17D 108.8 . . ? C175 C176 H17D 108.8 . . ? H17C C176 H17D 107.7 . . ? C176 C177 H17E 109.5 . . ? C176 C177 H17F 109.5 . . ? H17E C177 H17F 109.5 . . ? C176 C177 H17G 109.5 . . ? H17E C177 H17G 109.5 . . ? H17F C177 H17G 109.5 . . ? C173 O171 Pd2 126.7(14) . . ? C175 O172 Pd2 124.2(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.584 _refine_diff_density_min -1.400 _refine_diff_density_rms 0.188 # Attachment '04src0246c.cif' data_11b _database_code_depnum_ccdc_archive 'CCDC 602442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 F N O3 Pd' _chemical_formula_weight 712.16 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2597(3) _cell_length_b 16.848(2) _cell_length_c 27.261(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3334.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4337 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 0.8790 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28161 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7585 _reflns_number_gt 7226 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _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^)+(0.0219P)^2^+1.3629P] 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 -0.016(14) _refine_ls_number_reflns 7585 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.78487(2) 0.224855(8) 0.828578(5) 0.01549(4) Uani 1 1 d . . . C1 C 0.7356(3) 0.13248(11) 0.78664(7) 0.0183(4) Uani 1 1 d . . . C2 C 0.6930(3) 0.06355(11) 0.81293(7) 0.0199(4) Uani 1 1 d . . . C3 C 0.6525(3) -0.00726(12) 0.78863(8) 0.0265(5) Uani 1 1 d . . . H3 H 0.6214 -0.0536 0.8067 0.032 Uiso 1 1 calc R . . C4 C 0.6582(3) -0.00922(13) 0.73796(8) 0.0261(5) Uani 1 1 d . . . H4 H 0.6280 -0.0570 0.7213 0.031 Uiso 1 1 calc R . . C5 C 0.7075(3) 0.05780(12) 0.71102(7) 0.0214(4) Uani 1 1 d . . . C6 C 0.7426(3) 0.12913(11) 0.73582(7) 0.0196(4) Uani 1 1 d . . . H6 H 0.7715 0.1756 0.7176 0.023 Uiso 1 1 calc R . . C7 C 0.7054(3) 0.07227(11) 0.86531(7) 0.0218(4) Uani 1 1 d . . . H7 H 0.6796 0.0294 0.8868 0.026 Uiso 1 1 calc R . . C8 C 0.7840(3) 0.15114(11) 0.93335(7) 0.0183(4) Uani 1 1 d . . . C9 C 0.7156(3) 0.21687(11) 0.95772(6) 0.0181(4) Uani 1 1 d . . . H9 H 0.6537 0.2573 0.9399 0.022 Uiso 1 1 calc R . . C10 C 0.7371(3) 0.22397(12) 1.00826(6) 0.0182(4) Uani 1 1 d . . . H10 H 0.6892 0.2690 1.0250 0.022 Uiso 1 1 calc R . . C11 C 0.8285(3) 0.16521(12) 1.03412(7) 0.0183(4) Uani 1 1 d . . . C12 C 0.9042(3) 0.10052(12) 1.00932(8) 0.0207(4) Uani 1 1 d . . . H12 H 0.9705 0.0611 1.0269 0.025 Uiso 1 1 calc R . . C13 C 0.8827(3) 0.09387(12) 0.95928(7) 0.0200(4) Uani 1 1 d . . . H13 H 0.9352 0.0501 0.9424 0.024 Uiso 1 1 calc R . . C14 C 0.7291(4) 0.05061(12) 0.65595(7) 0.0261(5) Uani 1 1 d . . . H14A H 0.8497 0.0255 0.6492 0.031 Uiso 1 1 calc R . . H14B H 0.6326 0.0141 0.6437 0.031 Uiso 1 1 calc R . . C15 C 0.7179(4) 0.12653(12) 0.62672(7) 0.0273(5) Uani 1 1 d . . . H15A H 0.8142 0.1635 0.6385 0.033 Uiso 1 1 calc R . . H15B H 0.5968 0.1517 0.6327 0.033 Uiso 1 1 calc R . . C16 C 0.7421(3) 0.11421(13) 0.57165(7) 0.0292(5) Uani 1 1 d . . . H16A H 0.8640 0.0898 0.5655 0.035 Uiso 1 1 calc R . . H16B H 0.6468 0.0768 0.5598 0.035 Uiso 1 1 calc R . . C17 C 0.7280(4) 0.19097(14) 0.54269(9) 0.0404(6) Uani 1 1 d . . . H17A H 0.6019 0.2124 0.5466 0.048 Uiso 1 1 calc R . . H17B H 0.8143 0.2300 0.5571 0.048 Uiso 1 1 calc R . . C18 C 0.7692(5) 0.18396(18) 0.48827(9) 0.0541(8) Uani 1 1 d . . . H18A H 0.7579 0.2373 0.4733 0.065 Uiso 1 1 calc R . . H18B H 0.8988 0.1668 0.4844 0.065 Uiso 1 1 calc R . . C19 C 0.6544(8) 0.1304(2) 0.46150(12) 0.0961(19) Uani 1 1 d . . . H19A H 0.6616 0.0775 0.4763 0.144 Uiso 1 1 calc R . . H19B H 0.6961 0.1278 0.4274 0.144 Uiso 1 1 calc R . . H19C H 0.5267 0.1492 0.4625 0.144 Uiso 1 1 calc R . . C20 C 0.7881(3) 0.22922(12) 1.11262(6) 0.0207(4) Uani 1 1 d . . . H20A H 0.6572 0.2402 1.1050 0.025 Uiso 1 1 calc R . . H20B H 0.8610 0.2779 1.1064 0.025 Uiso 1 1 calc R . . C21 C 0.8097(3) 0.20266(11) 1.16506(7) 0.0207(4) Uani 1 1 d . . . H21A H 0.9371 0.1833 1.1699 0.025 Uiso 1 1 calc R . . H21B H 0.7253 0.1575 1.1711 0.025 Uiso 1 1 calc R . . C22 C 0.7702(3) 0.26750(12) 1.20281(7) 0.0219(4) Uani 1 1 d . . . H22A H 0.8612 0.3108 1.1991 0.026 Uiso 1 1 calc R . . H22B H 0.6461 0.2899 1.1968 0.026 Uiso 1 1 calc R . . C23 C 0.7796(3) 0.23487(12) 1.25471(7) 0.0237(4) Uani 1 1 d . . . H23A H 0.9052 0.2141 1.2606 0.028 Uiso 1 1 calc R . . H23B H 0.6928 0.1898 1.2575 0.028 Uiso 1 1 calc R . . C24 C 0.7340(3) 0.29535(13) 1.29438(7) 0.0284(5) Uani 1 1 d . . . H24A H 0.6153 0.3213 1.2864 0.034 Uiso 1 1 calc R . . H24B H 0.8305 0.3369 1.2949 0.034 Uiso 1 1 calc R . . C25 C 0.7208(4) 0.25721(15) 1.34497(8) 0.0382(6) Uani 1 1 d . . . H25A H 0.6287 0.2147 1.3443 0.057 Uiso 1 1 calc R . . H25B H 0.6844 0.2974 1.3691 0.057 Uiso 1 1 calc R . . H25C H 0.8409 0.2350 1.3540 0.057 Uiso 1 1 calc R . . N1 N 0.7534(2) 0.14139(9) 0.88175(6) 0.0181(4) Uani 1 1 d . . . O1 O 0.8554(2) 0.16437(8) 1.08350(5) 0.0220(3) Uani 1 1 d . . . C31 C 0.8229(3) 0.39240(11) 0.86229(7) 0.0170(4) Uani 1 1 d . . . C32 C 0.8133(3) 0.41995(11) 0.81381(7) 0.0195(4) Uani 1 1 d . . . H32 H 0.8099 0.4758 0.8092 0.023 Uiso 1 1 calc R . . C33 C 0.8084(3) 0.37292(11) 0.77161(7) 0.0172(4) Uani 1 1 d . . . C34 C 0.8239(3) 0.45007(12) 0.90418(7) 0.0174(4) Uani 1 1 d . . . C35 C 0.8887(3) 0.42320(12) 0.94930(7) 0.0198(4) Uani 1 1 d . A . H35 H 0.9364 0.3709 0.9524 0.024 Uiso 1 1 calc R . . C36 C 0.8830(3) 0.47301(13) 0.98931(8) 0.0249(5) Uani 1 1 d . . . H36 H 0.9302 0.4547 1.0198 0.030 Uiso 0.499(4) 1 calc PR A 1 C37 C 0.8113(3) 0.54835(12) 0.98657(8) 0.0260(5) Uani 1 1 d . A . H37 H 0.8077 0.5816 1.0147 0.031 Uiso 1 1 calc R . . C38 C 0.7442(3) 0.57495(12) 0.94168(8) 0.0278(5) Uani 1 1 d . . . H38 H 0.6920 0.6265 0.9392 0.033 Uiso 1 1 calc R A . C39 C 0.7532(3) 0.52650(12) 0.90045(7) 0.0243(5) Uani 1 1 d . A . H39 H 0.7110 0.5457 0.8697 0.029 Uiso 1 1 calc R . . C40 C 0.8039(3) 0.41106(12) 0.72211(7) 0.0182(4) Uani 1 1 d . . . C41 C 0.7394(3) 0.36635(12) 0.68278(6) 0.0222(4) Uani 1 1 d . A . H41 H 0.7045 0.3126 0.6875 0.027 Uiso 1 1 calc R . . C42 C 0.7263(4) 0.40033(13) 0.63694(7) 0.0293(5) Uani 1 1 d . . . H42 H 0.6814 0.3694 0.6104 0.035 Uiso 0.501(4) 1 calc PR A 1 C43 C 0.7768(4) 0.47819(13) 0.62870(7) 0.0272(5) Uani 1 1 d . A . H43 H 0.7657 0.5010 0.5970 0.033 Uiso 1 1 calc R . . C44 C 0.8435(3) 0.52221(12) 0.66739(8) 0.0251(4) Uani 1 1 d . . . H44 H 0.8806 0.5756 0.6622 0.030 Uiso 1 1 calc R A . C45 C 0.8570(3) 0.48935(12) 0.71377(8) 0.0221(4) Uani 1 1 d . A . H45 H 0.9029 0.5204 0.7401 0.027 Uiso 1 1 calc R . . O31 O 0.8308(2) 0.32016(8) 0.87502(5) 0.0186(3) Uani 1 1 d . . . O32 O 0.8027(2) 0.29718(7) 0.77024(5) 0.0195(3) Uani 1 1 d . . . F31 F 0.9377(4) 0.44859(17) 1.03218(9) 0.0356(9) Uani 0.501(4) 1 d P A 2 F32 F 0.6507(5) 0.36207(17) 0.60066(9) 0.0440(10) Uani 0.499(4) 1 d P A 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 0.01871(7) 0.01377(6) 0.01398(6) -0.00094(6) -0.00066(6) 0.00113(6) C1 0.0155(11) 0.0175(9) 0.0218(9) -0.0025(7) -0.0002(8) 0.0019(8) C2 0.0176(10) 0.0200(9) 0.0220(9) -0.0031(7) 0.0016(8) -0.0015(8) C3 0.0318(12) 0.0197(10) 0.0280(11) -0.0027(9) 0.0028(10) -0.0068(9) C4 0.0286(12) 0.0210(10) 0.0286(11) -0.0088(9) -0.0014(9) -0.0030(9) C5 0.0198(10) 0.0235(10) 0.0209(9) -0.0046(8) -0.0013(10) 0.0029(9) C6 0.0210(12) 0.0185(9) 0.0192(9) -0.0034(7) -0.0013(8) 0.0044(8) C7 0.0238(10) 0.0186(9) 0.0228(10) 0.0010(8) 0.0045(10) -0.0031(9) C8 0.0204(9) 0.0189(9) 0.0156(8) 0.0020(7) 0.0007(8) -0.0038(9) C9 0.0185(8) 0.0183(8) 0.0175(8) 0.0035(7) -0.0007(8) 0.0015(9) C10 0.0211(10) 0.0149(8) 0.0186(8) 0.0000(7) 0.0019(7) -0.0001(9) C11 0.0190(10) 0.0194(9) 0.0164(9) 0.0026(8) -0.0002(7) -0.0035(8) C12 0.0214(11) 0.0178(10) 0.0230(10) 0.0057(8) -0.0004(8) 0.0003(8) C13 0.0228(11) 0.0142(9) 0.0230(10) 0.0002(8) 0.0029(8) 0.0009(8) C14 0.0310(12) 0.0262(10) 0.0211(9) -0.0069(8) -0.0030(9) 0.0083(10) C15 0.0327(12) 0.0259(10) 0.0234(10) -0.0055(8) 0.0009(10) -0.0027(11) C16 0.0321(15) 0.0321(11) 0.0235(10) -0.0040(9) 0.0008(9) 0.0040(10) C17 0.0584(18) 0.0294(12) 0.0334(12) 0.0036(10) 0.0013(13) -0.0100(13) C18 0.074(2) 0.0525(16) 0.0360(13) 0.0121(13) 0.0084(16) 0.0020(17) C19 0.208(6) 0.0457(18) 0.0341(16) 0.0118(14) -0.027(2) -0.043(3) C20 0.0233(9) 0.0211(9) 0.0176(8) 0.0010(8) -0.0004(8) 0.0010(11) C21 0.0236(10) 0.0225(9) 0.0160(9) 0.0035(7) -0.0017(8) -0.0007(8) C22 0.0206(10) 0.0259(10) 0.0193(9) 0.0027(8) -0.0009(8) -0.0012(9) C23 0.0235(9) 0.0279(11) 0.0197(9) 0.0009(8) -0.0014(8) -0.0004(10) C24 0.0297(12) 0.0313(11) 0.0244(10) -0.0051(8) 0.0015(9) 0.0020(9) C25 0.0438(14) 0.0480(14) 0.0229(10) -0.0065(9) 0.0051(11) -0.0066(13) N1 0.0227(12) 0.0161(8) 0.0154(7) 0.0011(6) 0.0026(7) -0.0013(7) O1 0.0286(8) 0.0224(7) 0.0151(7) 0.0018(6) -0.0019(6) 0.0034(6) C31 0.0174(11) 0.0164(9) 0.0170(9) -0.0040(7) -0.0011(8) 0.0001(8) C32 0.0246(12) 0.0163(9) 0.0177(9) 0.0006(7) -0.0007(8) 0.0008(8) C33 0.0162(10) 0.0177(9) 0.0177(9) 0.0017(7) 0.0004(8) -0.0002(8) C34 0.0198(11) 0.0175(9) 0.0150(9) -0.0019(7) 0.0020(7) -0.0004(8) C35 0.0205(11) 0.0209(10) 0.0180(10) 0.0000(8) -0.0001(8) 0.0011(8) C36 0.0266(12) 0.0308(12) 0.0172(10) -0.0027(9) 0.0006(9) -0.0030(9) C37 0.0320(13) 0.0253(10) 0.0207(10) -0.0097(8) 0.0041(9) -0.0057(10) C38 0.0375(15) 0.0194(9) 0.0264(10) -0.0043(8) -0.0006(10) 0.0009(9) C39 0.0318(14) 0.0200(10) 0.0211(9) -0.0011(8) -0.0031(9) 0.0018(9) C40 0.0164(10) 0.0227(9) 0.0157(9) 0.0011(7) 0.0012(8) 0.0011(9) C41 0.0288(12) 0.0205(9) 0.0172(9) 0.0012(7) 0.0008(8) -0.0022(8) C42 0.0373(13) 0.0343(11) 0.0163(9) 0.0000(8) -0.0028(11) -0.0046(12) C43 0.0332(12) 0.0306(11) 0.0178(9) 0.0088(8) 0.0006(10) -0.0013(11) C44 0.0302(11) 0.0214(10) 0.0237(10) 0.0070(9) 0.0035(10) -0.0021(8) C45 0.0247(11) 0.0220(10) 0.0198(10) -0.0015(8) -0.0013(9) -0.0018(9) O31 0.0260(8) 0.0147(7) 0.0151(6) -0.0010(5) -0.0024(6) 0.0002(6) O32 0.0266(8) 0.0169(6) 0.0151(6) 0.0000(5) 0.0001(6) 0.0019(6) F31 0.0471(18) 0.0435(17) 0.0162(13) -0.0032(12) -0.0075(12) 0.0166(14) F32 0.085(3) 0.0335(16) 0.0139(13) -0.0001(11) -0.0109(14) -0.0195(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.9639(19) . ? Pd1 O32 2.0076(13) . ? Pd1 N1 2.0324(15) . ? Pd1 O31 2.0718(13) . ? C1 C6 1.388(3) . ? C1 C2 1.399(3) . ? C2 C3 1.396(3) . ? C2 C7 1.438(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? C5 C6 1.402(3) . ? C5 C14 1.514(3) . ? C6 H6 0.9500 . ? C7 N1 1.296(2) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 C13 1.394(3) . ? C8 N1 1.434(2) . ? C9 C10 1.392(2) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 O1 1.360(2) . ? C11 C12 1.395(3) . ? C12 C13 1.378(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.509(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.526(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.519(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.518(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.429(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O1 1.436(2) . ? C20 C21 1.506(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.528(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.519(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.522(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.524(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C31 O31 1.267(2) . ? C31 C32 1.402(3) . ? C31 C34 1.500(3) . ? C32 C33 1.397(3) . ? C32 H32 0.9500 . ? C33 O32 1.277(2) . ? C33 C40 1.495(3) . ? C34 C39 1.390(3) . ? C34 C35 1.393(3) . ? C35 C36 1.377(3) . ? C35 H35 0.9500 . ? C36 F31 1.301(3) . ? C36 C37 1.374(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 C39 1.391(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.391(3) . ? C40 C45 1.393(3) . ? C41 C42 1.378(3) . ? C41 H41 0.9500 . ? C42 F32 1.302(3) . ? C42 C43 1.381(3) . ? C42 H42 0.9500 . ? C43 C44 1.377(3) . ? C43 H43 0.9500 . ? C44 C45 1.384(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 O32 91.81(7) . . ? C1 Pd1 N1 81.17(7) . . ? O32 Pd1 N1 172.81(6) . . ? C1 Pd1 O31 177.72(7) . . ? O32 Pd1 O31 90.18(6) . . ? N1 Pd1 O31 96.80(6) . . ? C6 C1 C2 119.06(18) . . ? C6 C1 Pd1 127.37(15) . . ? C2 C1 Pd1 113.56(14) . . ? C3 C2 C1 120.85(18) . . ? C3 C2 C7 124.87(19) . . ? C1 C2 C7 114.20(17) . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.00(19) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.14(18) . . ? C4 C5 C14 118.96(18) . . ? C6 C5 C14 121.85(19) . . ? C1 C6 C5 120.64(19) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? N1 C7 C2 116.88(18) . . ? N1 C7 H7 121.6 . . ? C2 C7 H7 121.6 . . ? C9 C8 C13 119.66(17) . . ? C9 C8 N1 120.48(17) . . ? C13 C8 N1 119.86(17) . . ? C8 C9 C10 120.26(18) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.75(18) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? O1 C11 C10 125.47(18) . . ? O1 C11 C12 114.50(17) . . ? C10 C11 C12 120.03(18) . . ? C13 C12 C11 119.91(19) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.27(19) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C15 C14 C5 116.75(17) . . ? C15 C14 H14A 108.1 . . ? C5 C14 H14A 108.1 . . ? C15 C14 H14B 108.1 . . ? C5 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C14 C15 C16 113.45(17) . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 112.82(18) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C16 115.4(2) . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 115.7(3) . . ? C19 C18 H18A 108.4 . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18B 108.4 . . ? C17 C18 H18B 108.4 . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C20 C21 105.27(15) . . ? O1 C20 H20A 110.7 . . ? C21 C20 H20A 110.7 . . ? O1 C20 H20B 110.7 . . ? C21 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C20 C21 C22 114.05(16) . . ? C20 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 111.10(16) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 114.17(17) . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 C25 111.97(18) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C7 N1 C8 118.96(16) . . ? C7 N1 Pd1 113.92(13) . . ? C8 N1 Pd1 127.09(12) . . ? C11 O1 C20 119.34(15) . . ? O31 C31 C32 125.34(18) . . ? O31 C31 C34 114.43(17) . . ? C32 C31 C34 120.23(17) . . ? C33 C32 C31 126.12(18) . . ? C33 C32 H32 116.9 . . ? C31 C32 H32 116.9 . . ? O32 C33 C32 126.25(18) . . ? O32 C33 C40 113.73(17) . . ? C32 C33 C40 120.00(17) . . ? C39 C34 C35 119.38(18) . . ? C39 C34 C31 122.87(17) . . ? C35 C34 C31 117.63(17) . . ? C36 C35 C34 119.43(19) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? F31 C36 C37 117.2(2) . . ? F31 C36 C35 120.6(2) . . ? C37 C36 C35 122.1(2) . . ? F31 C36 H36 3.5 . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C38 118.57(19) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? C39 C38 C37 120.35(19) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C34 C39 C38 120.14(19) . . ? C34 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C45 118.69(18) . . ? C41 C40 C33 118.05(18) . . ? C45 C40 C33 123.25(18) . . ? C42 C41 C40 119.81(19) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? F32 C42 C41 120.8(2) . . ? F32 C42 C43 117.3(2) . . ? C41 C42 C43 121.6(2) . . ? F32 C42 H42 5.4 . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C44 C43 C42 118.71(19) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C43 C44 C45 120.61(19) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C40 120.6(2) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C31 O31 Pd1 124.74(12) . . ? C33 O32 Pd1 125.83(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.583 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.080 # Attachment '04src0247c.cif' data_4d _database_code_depnum_ccdc_archive 'CCDC 602443' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H45 N O2 Pd' _chemical_formula_weight 678.17 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' 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 P2(1)/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 17.801(4) _cell_length_b 16.966(3) _cell_length_c 22.192(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.646(13) _cell_angle_gamma 90.00 _cell_volume 6626(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15464 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour 'light orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8323 _exptl_absorpt_correction_T_max 0.9651 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98522 _diffrn_reflns_av_R_equivalents 0.0996 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15049 _reflns_number_gt 9096 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _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^)+(0.0549P)^2^+0.4571P] 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 15049 _refine_ls_number_parameters 880 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.014 _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 0.592691(14) 0.037157(15) 0.715898(11) 0.02238(8) Uani 1 1 d . . . Pd51 Pd 0.454569(15) 0.041412(16) 0.806339(12) 0.02897(9) Uani 1 1 d . B . C1 C 0.63907(19) 0.13745(19) 0.74655(15) 0.0246(7) Uani 1 1 d . . . C2 C 0.6143(2) 0.2030(2) 0.70984(17) 0.0332(9) Uani 1 1 d . . . C3 C 0.6404(2) 0.2789(2) 0.72564(19) 0.0441(11) Uani 1 1 d . . . H3 H 0.6225 0.3228 0.7010 0.053 Uiso 1 1 calc R . . C4 C 0.6925(2) 0.2894(2) 0.77737(19) 0.0423(10) Uani 1 1 d . . . H4 H 0.7104 0.3409 0.7884 0.051 Uiso 1 1 calc R . . C5 C 0.71959(19) 0.2255(2) 0.81394(16) 0.0295(8) Uani 1 1 d . . . C6 C 0.69210(19) 0.1500(2) 0.79823(15) 0.0256(8) Uani 1 1 d . . . H6 H 0.7100 0.1065 0.8233 0.031 Uiso 1 1 calc R . . C7 C 0.5592(2) 0.1839(2) 0.65743(16) 0.0333(9) Uani 1 1 d . . . H7 H 0.5379 0.2233 0.6296 0.040 Uiso 1 1 calc R . . C8 C 0.48918(19) 0.0885(2) 0.59616(15) 0.0249(8) Uani 1 1 d . . . C9 C 0.43107(18) 0.03558(19) 0.60147(15) 0.0247(7) Uani 1 1 d . . . H9 H 0.4259 0.0141 0.6402 0.030 Uiso 1 1 calc R . . C10 C 0.38087(19) 0.0141(2) 0.55070(15) 0.0251(8) Uani 1 1 d . . . H10 H 0.3407 -0.0213 0.5550 0.030 Uiso 1 1 calc R . . C11 C 0.38806(19) 0.04368(19) 0.49283(15) 0.0242(7) Uani 1 1 d . . . C12 C 0.4472(2) 0.0961(2) 0.48847(15) 0.0283(8) Uani 1 1 d . . . H12 H 0.4532 0.1171 0.4498 0.034 Uiso 1 1 calc R . . C13 C 0.49731(19) 0.1181(2) 0.53915(15) 0.0285(8) Uani 1 1 d . . . H13 H 0.5375 0.1536 0.5351 0.034 Uiso 1 1 calc R . . C14 C 0.7779(2) 0.2412(2) 0.87006(17) 0.0327(9) Uani 1 1 d . . . H14A H 0.8184 0.2748 0.8577 0.039 Uiso 1 1 calc R . . H14B H 0.7529 0.2720 0.8993 0.039 Uiso 1 1 calc R . . C15 C 0.8151(2) 0.1702(2) 0.90312(18) 0.0428(10) Uani 1 1 d . . . H15A H 0.8393 0.1380 0.8742 0.051 Uiso 1 1 calc R . . H15B H 0.7756 0.1375 0.9179 0.051 Uiso 1 1 calc R . . C16 C 0.8749(2) 0.1926(2) 0.95699(16) 0.0348(9) Uani 1 1 d . . . H16A H 0.9180 0.2187 0.9417 0.042 Uiso 1 1 calc R . . H16B H 0.8527 0.2307 0.9831 0.042 Uiso 1 1 calc R . . C17 C 0.9042(2) 0.1215(2) 0.99500(18) 0.0465(11) Uani 1 1 d . . . H17A H 0.8610 0.0960 1.0107 0.056 Uiso 1 1 calc R . . H17B H 0.9252 0.0829 0.9685 0.056 Uiso 1 1 calc R . . C18 C 0.9649(2) 0.1413(3) 1.04831(18) 0.0456(10) Uani 1 1 d . . . H18A H 0.9452 0.1829 1.0731 0.055 Uiso 1 1 calc R . . H18B H 1.0096 0.1631 1.0324 0.055 Uiso 1 1 calc R . . C19 C 0.9901(3) 0.0716(3) 1.0891(2) 0.0747(16) Uani 1 1 d . . . H19A H 0.9455 0.0465 1.1020 0.112 Uiso 1 1 calc R . . H19B H 1.0245 0.0897 1.1251 0.112 Uiso 1 1 calc R . . H19C H 1.0165 0.0334 1.0666 0.112 Uiso 1 1 calc R . . C20 C 0.3357(2) 0.0197(2) 0.43573(15) 0.0290(8) Uani 1 1 d . . . H20A H 0.3675 0.0026 0.4051 0.035 Uiso 1 1 calc R . . H20B H 0.3072 0.0669 0.4192 0.035 Uiso 1 1 calc R . . C21 C 0.2789(2) -0.0453(2) 0.44214(16) 0.0388(9) Uani 1 1 d . . . H21A H 0.2390 -0.0243 0.4644 0.047 Uiso 1 1 calc R . . H21B H 0.3052 -0.0885 0.4669 0.047 Uiso 1 1 calc R . . C22 C 0.2412(2) -0.0790(2) 0.38128(16) 0.0385(9) Uani 1 1 d . . . H22A H 0.2803 -0.1062 0.3616 0.046 Uiso 1 1 calc R . . H22B H 0.2034 -0.1190 0.3892 0.046 Uiso 1 1 calc R . . C23 C 0.2020(2) -0.0189(2) 0.33747(16) 0.0333(9) Uani 1 1 d . . . H23A H 0.2406 0.0172 0.3249 0.040 Uiso 1 1 calc R . . H23B H 0.1672 0.0129 0.3585 0.040 Uiso 1 1 calc R . . C24 C 0.1568(2) -0.0567(2) 0.28049(17) 0.0374(9) Uani 1 1 d . . . H24A H 0.1906 -0.0930 0.2622 0.045 Uiso 1 1 calc R . . H24B H 0.1150 -0.0884 0.2928 0.045 Uiso 1 1 calc R . . C25 C 0.1239(3) 0.0022(3) 0.2331(2) 0.0650(14) Uani 1 1 d . . . H25A H 0.0877 0.0362 0.2500 0.098 Uiso 1 1 calc R . . H25B H 0.0977 -0.0256 0.1973 0.098 Uiso 1 1 calc R . . H25C H 0.1648 0.0345 0.2212 0.098 Uiso 1 1 calc R . . N1 N 0.54019(16) 0.11037(16) 0.65005(12) 0.0269(7) Uani 1 1 d . . . C31 C 0.55867(19) -0.1363(2) 0.70494(14) 0.0245(8) Uani 1 1 d . . . C32 C 0.61163(18) -0.1518(2) 0.75666(14) 0.0239(7) Uani 1 1 d . A . H32 H 0.6182 -0.2054 0.7687 0.029 Uiso 1 1 calc R . . C33 C 0.65567(18) -0.0963(2) 0.79222(14) 0.0234(7) Uani 1 1 d . . . C34 C 0.51182(18) -0.20293(19) 0.67362(14) 0.0229(7) Uani 1 1 d . . . C35 C 0.44956(19) -0.1844(2) 0.63077(15) 0.0265(8) Uani 1 1 d . . . H35 H 0.4380 -0.1307 0.6215 0.032 Uiso 1 1 calc R . . C36 C 0.4039(2) -0.2428(2) 0.60113(16) 0.0321(8) Uani 1 1 d . . . H36 H 0.3612 -0.2289 0.5720 0.039 Uiso 1 1 calc R . . C37 C 0.4204(2) -0.3213(2) 0.61384(16) 0.0337(9) Uani 1 1 d . . . H37 H 0.3892 -0.3615 0.5935 0.040 Uiso 1 1 calc R . . C38 C 0.4823(2) -0.3407(2) 0.65618(17) 0.0360(9) Uani 1 1 d . . . H38 H 0.4938 -0.3945 0.6650 0.043 Uiso 1 1 calc R . . C39 C 0.5279(2) -0.2822(2) 0.68599(16) 0.0308(8) Uani 1 1 d . . . H39 H 0.5705 -0.2963 0.7151 0.037 Uiso 1 1 calc R . . C40 C 0.70922(18) -0.1219(2) 0.84738(14) 0.0239(7) Uani 0.501(13) 1 d PD A 1 C41 C 0.7368(6) -0.1969(5) 0.8560(5) 0.030(2) Uani 0.501(13) 1 d PD A 1 H41 H 0.7204 -0.2368 0.8270 0.036 Uiso 0.501(13) 1 calc PR A 1 C42 C 0.7884(7) -0.2142(7) 0.9069(5) 0.035(3) Uani 0.501(13) 1 d PD A 1 H42 H 0.8094 -0.2656 0.9121 0.042 Uiso 0.501(13) 1 calc PR A 1 C43 C 0.8095(19) -0.1571(8) 0.9504(13) 0.032(7) Uani 0.501(13) 1 d PD A 1 H43 H 0.8447 -0.1699 0.9856 0.039 Uiso 0.501(13) 1 calc PR A 1 C44 C 0.7802(7) -0.0811(5) 0.9434(4) 0.035(3) Uani 0.501(13) 1 d PD A 1 H44 H 0.7951 -0.0421 0.9735 0.042 Uiso 0.501(13) 1 calc PR A 1 C45 C 0.7293(6) -0.0634(4) 0.8922(3) 0.029(2) Uani 0.501(13) 1 d PD A 1 H45 H 0.7078 -0.0121 0.8870 0.034 Uiso 0.501(13) 1 calc PR A 1 O31 O 0.54358(13) -0.06859(13) 0.68131(10) 0.0255(5) Uani 1 1 d . . . O32 O 0.65613(13) -0.02165(13) 0.78322(10) 0.0260(5) Uani 1 1 d . A . C140 C 0.70922(18) -0.1219(2) 0.84738(14) 0.0239(7) Uani 0.499(13) 1 d PD A 2 C141 C 0.7075(6) -0.1961(5) 0.8741(5) 0.033(3) Uani 0.499(13) 1 d PD A 2 H141 H 0.6694 -0.2326 0.8576 0.040 Uiso 0.499(13) 1 calc PR A 2 C142 C 0.7599(7) -0.2184(6) 0.9241(5) 0.036(3) Uani 0.499(13) 1 d PD A 2 H142 H 0.7567 -0.2694 0.9412 0.043 Uiso 0.499(13) 1 calc PR A 2 C143 C 0.816(2) -0.1675(9) 0.9493(12) 0.035(6) Uani 0.499(13) 1 d PD A 2 H143 H 0.8517 -0.1824 0.9838 0.042 Uiso 0.499(13) 1 calc PR A 2 C144 C 0.8195(5) -0.0938(5) 0.9227(4) 0.032(2) Uani 0.499(13) 1 d PD A 2 H144 H 0.8582 -0.0578 0.9390 0.038 Uiso 0.499(13) 1 calc PR A 2 C145 C 0.7681(5) -0.0720(4) 0.8735(4) 0.025(2) Uani 0.499(13) 1 d PD A 2 H145 H 0.7723 -0.0212 0.8563 0.030 Uiso 0.499(13) 1 calc PR A 2 C51 C 0.4244(2) 0.1410(2) 0.76433(16) 0.0312(8) Uani 1 1 d . . . C52 C 0.4664(2) 0.2071(2) 0.78946(17) 0.0371(9) Uani 1 1 d . . . C53 C 0.4551(2) 0.2807(2) 0.76271(19) 0.0439(10) Uani 1 1 d . . . H53 H 0.4828 0.3248 0.7806 0.053 Uiso 1 1 calc R . . C54 C 0.4038(3) 0.2900(2) 0.71008(18) 0.0483(12) Uani 1 1 d . . . H54 H 0.3970 0.3405 0.6914 0.058 Uiso 1 1 calc R . . C55 C 0.3617(3) 0.2258(2) 0.68404(17) 0.0500(12) Uani 1 1 d . . . C56 C 0.3720(2) 0.1523(2) 0.71195(16) 0.0380(10) Uani 1 1 d . . . H56 H 0.3426 0.1089 0.6948 0.046 Uiso 1 1 calc R . . C57 C 0.5162(2) 0.1900(2) 0.84468(18) 0.0381(10) Uani 1 1 d . B . H57 H 0.5453 0.2302 0.8670 0.046 Uiso 1 1 calc R . . C58 C 0.5658(2) 0.0972(2) 0.91954(17) 0.0371(9) Uani 0.504(4) 1 d PD B 1 C59 C 0.5398(4) 0.0325(4) 0.9610(3) 0.0271(16) Uani 0.504(4) 1 d PD B 1 H59 H 0.4936 0.0055 0.9475 0.033 Uiso 0.504(4) 1 calc PR B 1 C60 C 0.5807(4) 0.0121(4) 1.0167(3) 0.0284(17) Uani 0.504(4) 1 d PD B 1 H60 H 0.5645 -0.0268 1.0427 0.034 Uiso 0.504(4) 1 calc PR B 1 C61 C 0.6518(2) 0.0569(3) 1.03159(19) 0.0418(11) Uani 0.504(4) 1 d PD B 1 C62 C 0.6785(4) 0.1049(4) 1.0000(3) 0.0281(17) Uani 0.504(4) 1 d PD B 1 H62 H 0.7269 0.1278 1.0131 0.034 Uiso 0.504(4) 1 calc PR B 1 C63 C 0.6365(4) 0.1250(4) 0.9445(3) 0.0265(16) Uani 0.504(4) 1 d PD B 1 H63 H 0.6590 0.1624 0.9208 0.032 Uiso 0.504(4) 1 calc PR B 1 C64 C 0.3085(4) 0.2365(3) 0.6253(2) 0.105(3) Uani 1 1 d . . . H64A H 0.2836 0.2884 0.6274 0.126 Uiso 1 1 calc R . . H64B H 0.3400 0.2398 0.5923 0.126 Uiso 1 1 calc R . . C65 C 0.2480(2) 0.1785(3) 0.60624(17) 0.0428(10) Uani 1 1 d . . . H65A H 0.2116 0.1805 0.6358 0.051 Uiso 1 1 calc R . . H65B H 0.2713 0.1254 0.6092 0.051 Uiso 1 1 calc R . . C66 C 0.2043(4) 0.1874(3) 0.54406(19) 0.0745(18) Uani 1 1 d . . . H66A H 0.1807 0.2404 0.5416 0.089 Uiso 1 1 calc R . . H66B H 0.2412 0.1866 0.5148 0.089 Uiso 1 1 calc R . . C67 C 0.1441(2) 0.1297(3) 0.52285(18) 0.0492(11) Uani 1 1 d . . . H67A H 0.1054 0.1329 0.5505 0.059 Uiso 1 1 calc R . . H67B H 0.1669 0.0764 0.5276 0.059 Uiso 1 1 calc R . . C68 C 0.1042(4) 0.1368(3) 0.4595(2) 0.0731(17) Uani 1 1 d . . . H68A H 0.0826 0.1906 0.4544 0.088 Uiso 1 1 calc R . . H68B H 0.1427 0.1323 0.4318 0.088 Uiso 1 1 calc R . . C69 C 0.0427(3) 0.0806(4) 0.4384(2) 0.0750(16) Uani 1 1 d . . . H69A H 0.0636 0.0271 0.4390 0.112 Uiso 1 1 calc R . . H69B H 0.0196 0.0941 0.3968 0.112 Uiso 1 1 calc R . . H69C H 0.0040 0.0832 0.4655 0.112 Uiso 1 1 calc R . . C70 C 0.6948(2) 0.0340(2) 1.09338(18) 0.0429(10) Uani 1 1 d . . . H70A H 0.7359 0.0729 1.1049 0.051 Uiso 1 1 calc R B 1 H70B H 0.6596 0.0378 1.1238 0.051 Uiso 1 1 calc R B 1 C71 C 0.7293(2) -0.0473(2) 1.0971(2) 0.0469(11) Uani 1 1 d . B . H71A H 0.7724 -0.0478 1.0736 0.056 Uiso 1 1 calc R . . H71B H 0.6909 -0.0852 1.0776 0.056 Uiso 1 1 calc R . . C72 C 0.7576(2) -0.0750(2) 1.16213(18) 0.0426(10) Uani 1 1 d . . . H72A H 0.7139 -0.0767 1.1849 0.051 Uiso 1 1 calc R B . H72B H 0.7773 -0.1294 1.1604 0.051 Uiso 1 1 calc R . . C73 C 0.8195(2) -0.0239(2) 1.19731(17) 0.0373(9) Uani 1 1 d . B . H73A H 0.8618 -0.0186 1.1733 0.045 Uiso 1 1 calc R . . H73B H 0.7987 0.0294 1.2024 0.045 Uiso 1 1 calc R . . C74 C 0.8500(3) -0.0572(3) 1.25939(19) 0.0583(13) Uani 1 1 d . . . H74A H 0.8693 -0.1111 1.2542 0.070 Uiso 1 1 calc R B . H74B H 0.8078 -0.0613 1.2836 0.070 Uiso 1 1 calc R . . C75 C 0.9131(3) -0.0083(3) 1.2946(2) 0.0658(14) Uani 1 1 d . B . H75A H 0.9568 -0.0074 1.2726 0.099 Uiso 1 1 calc R . . H75B H 0.9282 -0.0315 1.3351 0.099 Uiso 1 1 calc R . . H75C H 0.8949 0.0456 1.2990 0.099 Uiso 1 1 calc R . . N51 N 0.52004(16) 0.1173(2) 0.86288(14) 0.0354(8) Uani 1 1 d . . . C158 C 0.5658(2) 0.0972(2) 0.91954(17) 0.0371(9) Uani 0.496(4) 1 d PD B 2 C159 C 0.6138(4) 0.0399(4) 0.9171(3) 0.0250(16) Uani 0.496(4) 1 d PD B 2 H159 H 0.6196 0.0137 0.8803 0.030 Uiso 0.496(4) 1 calc PR B 2 C160 C 0.6554(4) 0.0203(4) 0.9723(3) 0.0264(17) Uani 0.496(4) 1 d PD B 2 H160 H 0.6906 -0.0217 0.9719 0.032 Uiso 0.496(4) 1 calc PR B 2 C161 C 0.6518(2) 0.0569(3) 1.03159(19) 0.0418(11) Uani 0.496(4) 1 d PD B 2 C162 C 0.6057(4) 0.1292(4) 1.0208(3) 0.0256(17) Uani 0.496(4) 1 d PD B 2 H162 H 0.6063 0.1644 1.0541 0.031 Uiso 0.496(4) 1 calc PR B 2 C163 C 0.5612(4) 0.1505(4) 0.9659(3) 0.0252(16) Uani 0.496(4) 1 d PD B 2 H163 H 0.5309 0.1968 0.9610 0.030 Uiso 0.496(4) 1 calc PR B 2 C81 C 0.4667(2) -0.1310(2) 0.83703(16) 0.0338(9) Uani 1 1 d . B . C82 C 0.4057(2) -0.1477(2) 0.79126(15) 0.0306(8) Uani 1 1 d . . . H82 H 0.3900 -0.2012 0.7872 0.037 Uiso 1 1 calc R . . C83 C 0.3655(2) -0.0943(2) 0.75110(15) 0.0269(8) Uani 1 1 d . B . C84 C 0.5060(2) -0.1958(2) 0.87562(17) 0.0411(10) Uani 1 1 d . . . C85 C 0.5515(4) -0.1766(3) 0.9293(2) 0.083(2) Uani 1 1 d . . . H85 H 0.5581 -0.1228 0.9406 0.100 Uiso 1 1 calc R . . C86 C 0.5876(4) -0.2337(3) 0.9669(2) 0.112(3) Uani 1 1 d . . . H86 H 0.6175 -0.2191 1.0044 0.135 Uiso 1 1 calc R . . C87 C 0.5805(3) -0.3120(3) 0.9505(2) 0.0746(17) Uani 1 1 d . . . H87 H 0.6060 -0.3515 0.9763 0.089 Uiso 1 1 calc R . . C88 C 0.5362(2) -0.3326(3) 0.89676(19) 0.0496(11) Uani 1 1 d . . . H88 H 0.5311 -0.3864 0.8852 0.060 Uiso 1 1 calc R . . C89 C 0.4990(2) -0.2753(2) 0.85938(17) 0.0385(10) Uani 1 1 d . . . H89 H 0.4683 -0.2901 0.8223 0.046 Uiso 1 1 calc R . . C90 C 0.30000(19) -0.1217(2) 0.70577(15) 0.0280(8) Uani 1 1 d . . . C91 C 0.2712(2) -0.0731(2) 0.65814(16) 0.0367(9) Uani 1 1 d . . . H91 H 0.2933 -0.0225 0.6549 0.044 Uiso 1 1 calc R . . C92 C 0.2110(2) -0.0961(2) 0.61484(17) 0.0425(10) Uani 1 1 d . . . H92 H 0.1925 -0.0618 0.5821 0.051 Uiso 1 1 calc R . . C93 C 0.1778(2) -0.1688(2) 0.61943(17) 0.0374(9) Uani 1 1 d . . . H93 H 0.1368 -0.1850 0.5896 0.045 Uiso 1 1 calc R . . C94 C 0.2043(2) -0.2179(2) 0.66726(18) 0.0365(9) Uani 1 1 d . . . H94 H 0.1806 -0.2674 0.6711 0.044 Uiso 1 1 calc R . . C95 C 0.2655(2) -0.1953(2) 0.70992(18) 0.0356(9) Uani 1 1 d . . . H95 H 0.2843 -0.2300 0.7423 0.043 Uiso 1 1 calc R . . O81 O 0.49261(14) -0.06201(15) 0.85091(11) 0.0337(6) Uani 1 1 d . . . O82 O 0.37930(13) -0.01991(14) 0.74792(10) 0.0298(6) 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 0.02453(14) 0.01926(14) 0.02225(14) 0.00106(11) -0.00006(11) -0.00083(11) Pd51 0.02869(16) 0.03181(17) 0.02740(15) -0.00962(12) 0.00747(12) -0.00818(12) C1 0.0266(18) 0.0201(18) 0.0273(18) -0.0009(14) 0.0041(15) -0.0007(14) C2 0.0280(19) 0.029(2) 0.041(2) 0.0022(17) -0.0021(17) -0.0032(16) C3 0.047(2) 0.024(2) 0.053(3) 0.0058(18) -0.020(2) -0.0031(18) C4 0.043(2) 0.022(2) 0.056(3) -0.0014(18) -0.010(2) -0.0061(18) C5 0.0231(18) 0.027(2) 0.036(2) 0.0009(16) -0.0033(16) -0.0002(15) C6 0.0269(18) 0.0217(19) 0.0278(18) 0.0014(14) 0.0028(15) 0.0003(15) C7 0.034(2) 0.027(2) 0.035(2) 0.0064(16) -0.0066(17) 0.0014(16) C8 0.0249(18) 0.0235(19) 0.0252(18) 0.0021(14) -0.0002(15) 0.0032(15) C9 0.0293(18) 0.0224(18) 0.0226(17) 0.0025(14) 0.0037(14) 0.0036(15) C10 0.0254(18) 0.0223(18) 0.0276(18) 0.0005(14) 0.0040(15) -0.0020(14) C11 0.0261(17) 0.0218(18) 0.0239(17) -0.0029(14) 0.0016(14) 0.0070(15) C12 0.034(2) 0.027(2) 0.0242(18) 0.0048(15) 0.0053(16) 0.0035(16) C13 0.0293(19) 0.0226(19) 0.0323(19) 0.0033(15) 0.0007(16) -0.0023(15) C14 0.033(2) 0.027(2) 0.035(2) -0.0030(16) -0.0041(17) -0.0040(16) C15 0.045(2) 0.029(2) 0.048(2) -0.0038(18) -0.016(2) -0.0019(18) C16 0.033(2) 0.035(2) 0.033(2) -0.0075(17) -0.0067(17) 0.0031(17) C17 0.053(3) 0.037(2) 0.043(2) -0.0087(19) -0.014(2) 0.007(2) C18 0.034(2) 0.059(3) 0.042(2) -0.006(2) -0.0023(19) 0.006(2) C19 0.079(4) 0.083(4) 0.054(3) -0.004(3) -0.019(3) 0.035(3) C20 0.036(2) 0.026(2) 0.0247(18) 0.0011(14) 0.0034(16) 0.0039(16) C21 0.053(2) 0.036(2) 0.0249(19) 0.0020(16) -0.0021(18) -0.0083(19) C22 0.049(2) 0.033(2) 0.031(2) -0.0024(17) -0.0027(19) -0.0040(19) C23 0.035(2) 0.031(2) 0.032(2) -0.0023(16) -0.0001(17) -0.0023(16) C24 0.038(2) 0.039(2) 0.033(2) -0.0005(17) -0.0025(18) -0.0046(18) C25 0.069(3) 0.052(3) 0.061(3) 0.011(2) -0.033(3) -0.020(3) N1 0.0282(16) 0.0207(16) 0.0304(16) 0.0016(12) -0.0006(13) -0.0012(12) C31 0.0303(19) 0.0250(19) 0.0201(17) 0.0039(14) 0.0096(15) 0.0089(15) C32 0.0263(18) 0.0209(18) 0.0241(17) 0.0026(14) 0.0033(15) 0.0035(14) C33 0.0216(17) 0.027(2) 0.0222(17) 0.0010(14) 0.0058(14) 0.0048(15) C34 0.0226(17) 0.0243(19) 0.0215(17) -0.0020(14) 0.0021(14) -0.0021(14) C35 0.0281(19) 0.0251(19) 0.0266(18) 0.0000(15) 0.0053(15) -0.0006(15) C36 0.030(2) 0.034(2) 0.0296(19) -0.0015(16) -0.0028(16) -0.0040(16) C37 0.039(2) 0.028(2) 0.032(2) -0.0034(16) -0.0007(17) -0.0134(17) C38 0.046(2) 0.0214(19) 0.037(2) 0.0023(16) -0.0041(19) -0.0066(17) C39 0.033(2) 0.027(2) 0.0294(19) 0.0001(16) -0.0062(16) -0.0035(16) C40 0.0258(18) 0.0261(19) 0.0200(16) -0.0007(14) 0.0035(14) -0.0010(15) C41 0.033(6) 0.024(4) 0.032(5) -0.004(4) 0.001(4) 0.007(4) C42 0.035(6) 0.031(5) 0.036(6) 0.005(4) -0.004(5) 0.007(5) C43 0.027(8) 0.036(10) 0.027(10) -0.001(7) -0.021(8) -0.002(8) C44 0.050(7) 0.033(5) 0.019(4) -0.006(3) -0.006(4) -0.004(4) C45 0.033(6) 0.025(4) 0.026(4) 0.003(3) -0.001(4) 0.003(4) O31 0.0296(13) 0.0202(13) 0.0247(12) 0.0016(10) -0.0029(10) -0.0014(10) O32 0.0300(13) 0.0209(13) 0.0253(12) 0.0030(10) -0.0019(10) -0.0019(10) C140 0.0258(18) 0.0261(19) 0.0200(16) -0.0007(14) 0.0035(14) -0.0010(15) C141 0.030(6) 0.032(5) 0.033(6) -0.004(4) -0.010(4) 0.003(4) C142 0.037(7) 0.028(5) 0.039(6) 0.009(4) -0.009(5) -0.002(5) C143 0.042(11) 0.032(9) 0.032(11) 0.011(8) 0.007(7) 0.006(7) C144 0.031(5) 0.020(4) 0.041(5) -0.008(4) -0.005(4) 0.002(4) C145 0.024(5) 0.020(4) 0.028(4) -0.002(3) -0.002(4) 0.000(3) C51 0.039(2) 0.028(2) 0.0296(19) -0.0065(16) 0.0171(18) -0.0099(17) C52 0.040(2) 0.036(2) 0.040(2) -0.0141(18) 0.0216(19) -0.0147(18) C53 0.053(3) 0.035(2) 0.047(3) -0.014(2) 0.021(2) -0.019(2) C54 0.081(3) 0.029(2) 0.038(2) -0.0043(18) 0.023(2) -0.023(2) C55 0.087(3) 0.038(2) 0.027(2) -0.0004(18) 0.015(2) -0.021(2) C56 0.056(3) 0.032(2) 0.029(2) -0.0058(17) 0.0125(19) -0.0140(19) C57 0.029(2) 0.039(3) 0.047(2) -0.022(2) 0.0127(19) -0.0083(18) C58 0.0238(19) 0.047(2) 0.041(2) -0.0217(19) 0.0065(18) -0.0054(18) C59 0.024(4) 0.030(4) 0.028(4) -0.002(3) 0.003(3) -0.007(3) C60 0.025(4) 0.035(4) 0.028(4) -0.003(3) 0.010(3) -0.004(3) C61 0.0220(19) 0.051(3) 0.051(3) -0.031(2) -0.0002(18) 0.0036(18) C62 0.030(4) 0.031(4) 0.023(4) -0.002(3) 0.001(3) -0.003(3) C63 0.026(4) 0.024(4) 0.030(4) -0.004(3) 0.004(3) -0.005(3) C64 0.214(8) 0.054(3) 0.032(3) 0.017(2) -0.035(4) -0.063(4) C65 0.040(2) 0.053(3) 0.036(2) 0.0152(19) 0.0096(19) 0.015(2) C66 0.149(5) 0.034(3) 0.032(2) 0.006(2) -0.013(3) -0.021(3) C67 0.034(2) 0.071(3) 0.042(2) 0.012(2) 0.0046(19) 0.010(2) C68 0.138(5) 0.034(3) 0.039(3) 0.001(2) -0.013(3) -0.005(3) C69 0.052(3) 0.113(5) 0.058(3) -0.013(3) 0.002(3) 0.010(3) C70 0.029(2) 0.052(3) 0.047(2) -0.019(2) 0.0031(18) 0.0026(19) C71 0.042(2) 0.046(3) 0.053(3) -0.021(2) 0.007(2) -0.005(2) C72 0.045(2) 0.039(2) 0.047(2) -0.0061(19) 0.019(2) -0.0090(19) C73 0.043(2) 0.035(2) 0.035(2) 0.0004(17) 0.0104(18) -0.0050(18) C74 0.093(4) 0.043(3) 0.037(2) 0.000(2) 0.005(2) -0.006(3) C75 0.084(4) 0.066(3) 0.040(3) -0.003(2) -0.014(3) 0.010(3) N51 0.0257(16) 0.041(2) 0.0407(19) -0.0201(16) 0.0102(15) -0.0070(14) C158 0.0238(19) 0.047(2) 0.041(2) -0.0217(19) 0.0065(18) -0.0054(18) C159 0.027(4) 0.023(4) 0.024(3) -0.001(3) 0.002(3) -0.001(3) C160 0.018(3) 0.037(4) 0.024(4) 0.000(3) 0.003(3) 0.000(3) C161 0.0220(19) 0.051(3) 0.051(3) -0.031(2) -0.0002(18) 0.0036(18) C162 0.035(4) 0.026(4) 0.017(3) -0.004(3) 0.008(3) -0.005(3) C163 0.027(4) 0.019(4) 0.033(4) 0.000(3) 0.015(3) -0.004(3) C81 0.036(2) 0.039(2) 0.029(2) -0.0072(17) 0.0129(17) -0.0126(18) C82 0.037(2) 0.029(2) 0.0261(18) -0.0053(16) 0.0069(17) -0.0078(17) C83 0.0313(19) 0.028(2) 0.0240(18) -0.0104(15) 0.0133(16) -0.0064(16) C84 0.049(2) 0.044(3) 0.028(2) 0.0128(18) -0.0005(18) -0.019(2) C85 0.138(5) 0.053(3) 0.043(3) 0.028(2) -0.038(3) -0.051(3) C86 0.181(7) 0.067(4) 0.061(3) 0.038(3) -0.072(4) -0.069(4) C87 0.092(4) 0.068(4) 0.051(3) 0.036(3) -0.031(3) -0.034(3) C88 0.049(3) 0.049(3) 0.049(3) 0.009(2) 0.004(2) -0.009(2) C89 0.039(2) 0.044(3) 0.030(2) 0.0038(18) -0.0042(18) -0.0052(19) C90 0.0262(18) 0.031(2) 0.0291(19) -0.0068(16) 0.0125(15) 0.0002(16) C91 0.042(2) 0.040(2) 0.028(2) -0.0012(17) 0.0037(18) -0.0176(18) C92 0.046(2) 0.049(3) 0.031(2) 0.0012(18) -0.0015(19) -0.018(2) C93 0.034(2) 0.040(2) 0.037(2) -0.0141(18) 0.0034(18) -0.0058(18) C94 0.0258(19) 0.027(2) 0.056(3) -0.0051(19) 0.0054(18) -0.0038(16) C95 0.031(2) 0.028(2) 0.047(2) -0.0028(17) 0.0024(18) -0.0004(16) O81 0.0369(14) 0.0387(16) 0.0248(13) -0.0043(11) 0.0025(11) -0.0115(12) O82 0.0343(14) 0.0300(15) 0.0251(12) -0.0034(10) 0.0044(11) -0.0085(11) _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 1.967(3) . ? Pd1 O32 1.999(2) . ? Pd1 N1 2.035(3) . ? Pd1 O31 2.091(2) . ? Pd51 C51 1.965(4) . ? Pd51 O82 2.009(2) . ? Pd51 N51 2.037(3) . ? Pd51 O81 2.077(3) . ? C1 C6 1.388(5) . ? C1 C2 1.410(5) . ? C2 C3 1.396(5) . ? C2 C7 1.441(5) . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 H4 0.9500 . ? C5 C6 1.398(5) . ? C5 C14 1.520(5) . ? C6 H6 0.9500 . ? C7 N1 1.296(4) . ? C7 H7 0.9500 . ? C8 C9 1.388(5) . ? C8 C13 1.389(5) . ? C8 N1 1.437(4) . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 C11 1.402(5) . ? C10 H10 0.9500 . ? C11 C12 1.393(5) . ? C11 C20 1.511(5) . ? C12 C13 1.377(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.511(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.519(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.515(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.516(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.518(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.526(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.506(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.534(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.505(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C31 O31 1.274(4) . ? C31 C32 1.396(5) . ? C31 C34 1.511(5) . ? C32 C33 1.392(5) . ? C32 H32 0.9500 . ? C33 O32 1.283(4) . ? C33 C40 1.498(4) . ? C34 C35 1.384(5) . ? C34 C39 1.394(5) . ? C35 C36 1.383(5) . ? C35 H35 0.9500 . ? C36 C37 1.384(5) . ? C36 H36 0.9500 . ? C37 C38 1.376(5) . ? C37 H37 0.9500 . ? C38 C39 1.385(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.367(9) . ? C40 C45 1.413(8) . ? C41 C42 1.376(10) . ? C41 H41 0.9500 . ? C42 C43 1.378(17) . ? C42 H42 0.9500 . ? C43 C44 1.391(17) . ? C43 H43 0.9500 . ? C44 C45 1.375(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C141 C142 1.391(10) . ? C141 H141 0.9500 . ? C142 C143 1.376(18) . ? C142 H142 0.9500 . ? C143 C144 1.389(16) . ? C143 H143 0.9500 . ? C144 C145 1.367(9) . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? C51 C56 1.390(5) . ? C51 C52 1.415(5) . ? C52 C53 1.384(6) . ? C52 C57 1.431(6) . ? C53 C54 1.380(6) . ? C53 H53 0.9500 . ? C54 C55 1.398(6) . ? C54 H54 0.9500 . ? C55 C56 1.392(6) . ? C55 C64 1.502(7) . ? C56 H56 0.9500 . ? C57 N51 1.297(5) . ? C57 H57 0.9500 . ? C58 C63 1.381(7) . ? C58 N51 1.432(5) . ? C58 C59 1.547(7) . ? C59 C60 1.381(9) . ? C59 H59 0.9500 . ? C60 C61 1.470(7) . ? C60 H60 0.9500 . ? C61 C62 1.218(7) . ? C61 C70 1.517(6) . ? C62 C63 1.385(8) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.472(7) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.486(6) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.476(6) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.482(6) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.474(7) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.508(6) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.529(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.521(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.512(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.515(6) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C159 C160 1.372(8) . ? C159 H159 0.9500 . ? C160 H160 0.9500 . ? C162 C163 1.397(9) . ? C162 H162 0.9500 . ? C163 H163 0.9500 . ? C81 O81 1.279(4) . ? C81 C82 1.400(5) . ? C81 C84 1.501(6) . ? C82 C83 1.391(5) . ? C82 H82 0.9500 . ? C83 O82 1.290(4) . ? C83 C90 1.495(5) . ? C84 C85 1.375(6) . ? C84 C89 1.397(6) . ? C85 C86 1.373(7) . ? C85 H85 0.9500 . ? C86 C87 1.379(7) . ? C86 H86 0.9500 . ? C87 C88 1.373(6) . ? C87 H87 0.9500 . ? C88 C89 1.380(6) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C91 1.377(5) . ? C90 C95 1.401(5) . ? C91 C92 1.385(5) . ? C91 H91 0.9500 . ? C92 C93 1.378(5) . ? C92 H92 0.9500 . ? C93 C94 1.376(5) . ? C93 H93 0.9500 . ? C94 C95 1.386(5) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 O32 90.73(11) . . ? C1 Pd1 N1 81.02(12) . . ? O32 Pd1 N1 171.22(10) . . ? C1 Pd1 O31 178.70(11) . . ? O32 Pd1 O31 90.23(9) . . ? N1 Pd1 O31 97.97(10) . . ? C51 Pd51 O82 91.76(12) . . ? C51 Pd51 N51 80.75(14) . . ? O82 Pd51 N51 171.48(12) . . ? C51 Pd51 O81 176.89(12) . . ? O82 Pd51 O81 90.46(9) . . ? N51 Pd51 O81 97.19(12) . . ? C6 C1 C2 118.1(3) . . ? C6 C1 Pd1 128.0(3) . . ? C2 C1 Pd1 113.8(2) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 C7 124.8(3) . . ? C1 C2 C7 113.8(3) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 C14 118.3(3) . . ? C6 C5 C14 122.4(3) . . ? C1 C6 C5 121.0(3) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? N1 C7 C2 116.9(3) . . ? N1 C7 H7 121.6 . . ? C2 C7 H7 121.6 . . ? C9 C8 C13 119.5(3) . . ? C9 C8 N1 118.8(3) . . ? C13 C8 N1 121.7(3) . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C12 C11 C10 117.8(3) . . ? C12 C11 C20 119.4(3) . . ? C10 C11 C20 122.8(3) . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C8 120.2(3) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C15 C14 C5 117.0(3) . . ? C15 C14 H14A 108.1 . . ? C5 C14 H14A 108.1 . . ? C15 C14 H14B 108.1 . . ? C5 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C14 C15 C16 112.7(3) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 112.2(3) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 113.7(3) . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 113.9(4) . . ? C17 C18 H18A 108.8 . . ? C19 C18 H18A 108.8 . . ? C17 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C11 C20 C21 116.9(3) . . ? C11 C20 H20A 108.1 . . ? C21 C20 H20A 108.1 . . ? C11 C20 H20B 108.1 . . ? C21 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 C21 C22 113.6(3) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 114.7(3) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 112.5(3) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 113.5(3) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C7 N1 C8 118.3(3) . . ? C7 N1 Pd1 114.4(2) . . ? C8 N1 Pd1 127.2(2) . . ? O31 C31 C32 125.7(3) . . ? O31 C31 C34 114.7(3) . . ? C32 C31 C34 119.6(3) . . ? C33 C32 C31 126.3(3) . . ? C33 C32 H32 116.9 . . ? C31 C32 H32 116.9 . . ? O32 C33 C32 126.6(3) . . ? O32 C33 C40 113.3(3) . . ? C32 C33 C40 120.2(3) . . ? C35 C34 C39 118.3(3) . . ? C35 C34 C31 118.4(3) . . ? C39 C34 C31 123.3(3) . . ? C36 C35 C34 121.1(3) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 120.0(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.5(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 120.4(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.6(3) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C41 C40 C45 120.5(6) . . ? C41 C40 C33 123.7(5) . . ? C45 C40 C33 115.8(4) . . ? C40 C41 C42 119.7(8) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C43 120.2(10) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C44 121.0(10) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C45 C44 C43 119.0(8) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C40 119.5(6) . . ? C44 C45 H45 120.2 . . ? C40 C45 H45 120.2 . . ? C31 O31 Pd1 124.9(2) . . ? C33 O32 Pd1 126.4(2) . . ? C142 C141 H141 119.0 . . ? C143 C142 C141 121.0(10) . . ? C143 C142 H142 119.5 . . ? C141 C142 H142 119.5 . . ? C142 C143 C144 117.8(12) . . ? C142 C143 H143 121.1 . . ? C144 C143 H143 121.1 . . ? C145 C144 C143 121.2(10) . . ? C145 C144 H144 119.4 . . ? C143 C144 H144 119.4 . . ? C144 C145 H145 118.8 . . ? C56 C51 C52 117.9(3) . . ? C56 C51 Pd51 128.1(3) . . ? C52 C51 Pd51 113.8(3) . . ? C53 C52 C51 120.8(4) . . ? C53 C52 C57 125.5(4) . . ? C51 C52 C57 113.6(4) . . ? C54 C53 C52 120.1(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.4(4) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C56 C55 C54 119.2(4) . . ? C56 C55 C64 121.2(4) . . ? C54 C55 C64 119.6(4) . . ? C51 C56 C55 121.5(4) . . ? C51 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? N51 C57 C52 117.1(3) . . ? N51 C57 H57 121.4 . . ? C52 C57 H57 121.4 . . ? C63 C58 N51 129.4(4) . . ? C63 C58 C59 109.9(4) . . ? N51 C58 C59 120.7(4) . . ? C60 C59 C58 123.1(5) . . ? C60 C59 H59 118.4 . . ? C58 C59 H59 118.4 . . ? C59 C60 C61 113.1(6) . . ? C59 C60 H60 123.5 . . ? C61 C60 H60 123.5 . . ? C62 C61 C60 127.9(5) . . ? C62 C61 C70 120.2(4) . . ? C60 C61 C70 111.8(4) . . ? C61 C62 C63 118.2(6) . . ? C61 C62 H62 120.9 . . ? C63 C62 H62 120.9 . . ? C58 C63 C62 127.6(6) . . ? C58 C63 H63 116.2 . . ? C62 C63 H63 116.2 . . ? C65 C64 C55 120.5(4) . . ? C65 C64 H64A 107.2 . . ? C55 C64 H64A 107.2 . . ? C65 C64 H64B 107.2 . . ? C55 C64 H64B 107.2 . . ? H64A C64 H64B 106.8 . . ? C64 C65 C66 117.2(4) . . ? C64 C65 H65A 108.0 . . ? C66 C65 H65A 108.0 . . ? C64 C65 H65B 108.0 . . ? C66 C65 H65B 108.0 . . ? H65A C65 H65B 107.2 . . ? C67 C66 C65 118.8(4) . . ? C67 C66 H66A 107.6 . . ? C65 C66 H66A 107.6 . . ? C67 C66 H66B 107.6 . . ? C65 C66 H66B 107.6 . . ? H66A C66 H66B 107.0 . . ? C66 C67 C68 118.1(4) . . ? C66 C67 H67A 107.8 . . ? C68 C67 H67A 107.8 . . ? C66 C67 H67B 107.8 . . ? C68 C67 H67B 107.8 . . ? H67A C67 H67B 107.1 . . ? C69 C68 C67 118.4(4) . . ? C69 C68 H68A 107.7 . . ? C67 C68 H68A 107.7 . . ? C69 C68 H68B 107.7 . . ? C67 C68 H68B 107.7 . . ? H68A C68 H68B 107.1 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 C61 115.4(3) . . ? C71 C70 H70A 108.4 . . ? C61 C70 H70A 108.4 . . ? C71 C70 H70B 108.4 . . ? C61 C70 H70B 108.4 . . ? H70A C70 H70B 107.5 . . ? C70 C71 C72 114.0(3) . . ? C70 C71 H71A 108.8 . . ? C72 C71 H71A 108.8 . . ? C70 C71 H71B 108.8 . . ? C72 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? C73 C72 C71 114.8(3) . . ? C73 C72 H72A 108.6 . . ? C71 C72 H72A 108.6 . . ? C73 C72 H72B 108.6 . . ? C71 C72 H72B 108.6 . . ? H72A C72 H72B 107.5 . . ? C74 C73 C72 112.8(3) . . ? C74 C73 H73A 109.0 . . ? C72 C73 H73A 109.0 . . ? C74 C73 H73B 109.0 . . ? C72 C73 H73B 109.0 . . ? H73A C73 H73B 107.8 . . ? C73 C74 C75 113.7(4) . . ? C73 C74 H74A 108.8 . . ? C75 C74 H74A 108.8 . . ? C73 C74 H74B 108.8 . . ? C75 C74 H74B 108.8 . . ? H74A C74 H74B 107.7 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C57 N51 C58 119.7(3) . . ? C57 N51 Pd51 114.3(3) . . ? C58 N51 Pd51 126.0(3) . . ? C160 C159 H159 122.8 . . ? C159 C160 H160 116.3 . . ? C163 C162 H162 117.1 . . ? C162 C163 H163 123.5 . . ? O81 C81 C82 124.9(4) . . ? O81 C81 C84 114.4(3) . . ? C82 C81 C84 120.7(3) . . ? C83 C82 C81 127.0(3) . . ? C83 C82 H82 116.5 . . ? C81 C82 H82 116.5 . . ? O82 C83 C82 126.0(3) . . ? O82 C83 C90 113.8(3) . . ? C82 C83 C90 120.2(3) . . ? C85 C84 C89 118.1(4) . . ? C85 C84 C81 119.0(4) . . ? C89 C84 C81 123.0(3) . . ? C86 C85 C84 121.4(5) . . ? C86 C85 H85 119.3 . . ? C84 C85 H85 119.3 . . ? C85 C86 C87 120.2(5) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C88 C87 C86 119.5(4) . . ? C88 C87 H87 120.3 . . ? C86 C87 H87 120.3 . . ? C87 C88 C89 120.3(4) . . ? C87 C88 H88 119.8 . . ? C89 C88 H88 119.8 . . ? C88 C89 C84 120.5(4) . . ? C88 C89 H89 119.7 . . ? C84 C89 H89 119.7 . . ? C91 C90 C95 117.9(3) . . ? C91 C90 C83 119.5(3) . . ? C95 C90 C83 122.5(3) . . ? C90 C91 C92 121.6(4) . . ? C90 C91 H91 119.2 . . ? C92 C91 H91 119.2 . . ? C93 C92 C91 119.8(4) . . ? C93 C92 H92 120.1 . . ? C91 C92 H92 120.1 . . ? C94 C93 C92 119.9(3) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.1(4) . . ? C93 C94 H94 119.9 . . ? C95 C94 H94 119.9 . . ? C94 C95 C90 120.6(4) . . ? C94 C95 H95 119.7 . . ? C90 C95 H95 119.7 . . ? C81 O81 Pd51 125.3(2) . . ? C83 O82 Pd51 125.8(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.800 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.091