Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hor, T.S.A.' 'Neo, Yew Chin ' 'Vittal, Jagadese J.' _publ_contact_author_name 'Prof T S A Hor' _publ_contact_author_address ; Department of Chemistry, Faculty of Science National University of Singapore 3 Science Drive 3 Singapore 117543 SINGAPORE ; _publ_contact_author_email ANDYHOR@NUS.EDU.SG data_187 _database_code_CSD 165079 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 F10 Fe O4 P2 Pd' _chemical_formula_weight 986.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7763(10) _cell_length_b 20.9449(15) _cell_length_c 15.5108(12) _cell_angle_alpha 90.00 _cell_angle_beta 110.990(2) _cell_angle_gamma 90.00 _cell_volume 3875.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2648 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 22.45 _exptl_crystal_description 'rectangular plate, cut' _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32140 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.1681 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.05 _reflns_number_total 11255 _reflns_number_gt 5609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11255 _refine_ls_number_parameters 523 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.826 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.25938(3) 0.249756(15) 0.45980(2) 0.02387(8) Uani 1 1 d . . . Fe1 Fe 0.17110(5) 0.10553(3) 0.26377(4) 0.03425(17) Uani 1 1 d . . . C1 C 0.0768(4) 0.1801(2) 0.2722(3) 0.0336(11) Uani 1 1 d . . . C2 C 0.1541(4) 0.1985(2) 0.2279(3) 0.0360(11) Uani 1 1 d . . . H2 H 0.2131 0.2315 0.2506 0.043 Uiso 1 1 calc R . . C3 C 0.1320(4) 0.1621(2) 0.1482(3) 0.0436(12) Uani 1 1 d . . . H3 H 0.1741 0.1641 0.1057 0.052 Uiso 1 1 calc R . . C4 C 0.0422(4) 0.1211(2) 0.1397(3) 0.0528(14) Uani 1 1 d . . . H4 H 0.0112 0.0889 0.0904 0.063 Uiso 1 1 calc R . . C5 C 0.0069(4) 0.1306(2) 0.2148(3) 0.0401(12) Uani 1 1 d . . . H5 H -0.0548 0.1079 0.2262 0.048 Uiso 1 1 calc R . . C6 C 0.3347(4) 0.07951(19) 0.3113(3) 0.0370(11) Uani 1 1 d . . . H6 H 0.3957 0.1016 0.2980 0.044 Uiso 1 1 calc R . . C7 C 0.2698(4) 0.0291(2) 0.2602(4) 0.0482(13) Uani 1 1 d . . . H7 H 0.2763 0.0102 0.2037 0.058 Uiso 1 1 calc R . . C8 C 0.1910(4) 0.0112(2) 0.3001(3) 0.0449(13) Uani 1 1 d . . . H8 H 0.1335 -0.0226 0.2773 0.054 Uiso 1 1 calc R . . C9 C 0.2074(4) 0.05047(18) 0.3768(3) 0.0368(11) Uani 1 1 d . . . H9 H 0.1642 0.0486 0.4185 0.044 Uiso 1 1 calc R . . C10 C 0.2987(4) 0.09321(18) 0.3858(3) 0.0316(10) Uani 1 1 d . . . O1 O 0.1925(2) 0.34028(12) 0.4580(2) 0.0306(7) Uani 1 1 d . . . O2 O 0.1977(3) 0.35548(15) 0.3172(2) 0.0558(10) Uani 1 1 d . . . C11 C 0.1820(4) 0.3720(2) 0.3854(3) 0.0336(11) Uani 1 1 d . . . C12 C 0.1477(5) 0.4418(2) 0.3928(4) 0.0482(14) Uani 1 1 d . . . F1 F 0.1060(3) 0.46868(13) 0.3100(2) 0.1025(15) Uani 1 1 d D . . F2 F 0.0628(3) 0.44480(14) 0.4274(3) 0.0977(14) Uani 1 1 d D . . C13 C 0.2365(6) 0.4831(2) 0.4539(5) 0.0689(18) Uani 1 1 d . . . F3 F 0.2027(3) 0.54347(13) 0.4520(3) 0.0902(12) Uani 1 1 d D . . F4 F 0.2768(4) 0.46387(15) 0.5384(3) 0.1141(17) Uani 1 1 d D . . F5 F 0.3220(3) 0.48312(17) 0.4253(4) 0.1210(18) Uani 1 1 d D . . O3 O 0.4132(3) 0.29306(14) 0.5233(2) 0.0453(9) Uani 1 1 d . . . O4 O 0.3858(3) 0.31189(16) 0.6549(3) 0.0578(10) Uani 1 1 d . . . C14 C 0.4332(4) 0.3171(2) 0.5978(4) 0.0464(13) Uani 1 1 d . . . F6 F 0.5506(3) 0.38861(18) 0.7096(3) 0.1035(14) Uani 1 1 d D . . F7 F 0.5225(3) 0.41120(15) 0.5701(3) 0.1160(17) Uani 1 1 d D . . C15 C 0.5369(4) 0.3633(2) 0.6266(4) 0.0542(16) Uani 1 1 d . . . C16 C 0.6467(5) 0.3314(3) 0.6367(5) 0.0654(17) Uani 1 1 d . . . F8 F 0.7327(3) 0.36625(18) 0.6838(3) 0.1126(15) Uani 1 1 d D . . F9 F 0.6541(3) 0.3175(2) 0.5591(3) 0.1288(18) Uani 1 1 d D . . F10 F 0.6522(3) 0.27637(19) 0.6806(3) 0.1107(15) Uani 1 1 d D . . P1 P 0.08665(9) 0.21126(5) 0.38162(8) 0.0256(3) Uani 1 1 d . . . P2 P 0.35143(9) 0.15577(5) 0.47053(8) 0.0275(3) Uani 1 1 d . . . C1A C -0.0243(3) 0.27026(18) 0.3564(3) 0.0292(10) Uani 1 1 d . . . C2A C -0.0740(4) 0.2953(2) 0.2682(4) 0.0499(14) Uani 1 1 d . . . H2A H -0.0482 0.2832 0.2209 0.060 Uiso 1 1 calc R . . C3A C -0.1609(5) 0.3379(2) 0.2504(5) 0.0690(19) Uani 1 1 d . . . H3A H -0.1931 0.3553 0.1908 0.083 Uiso 1 1 calc R . . C4A C -0.2017(5) 0.3555(2) 0.3170(5) 0.069(2) Uani 1 1 d . . . H4A H -0.2625 0.3839 0.3028 0.082 Uiso 1 1 calc R . . C5A C -0.1529(4) 0.3313(2) 0.4061(5) 0.0603(16) Uani 1 1 d . . . H5A H -0.1793 0.3436 0.4529 0.072 Uiso 1 1 calc R . . C6A C -0.0634(4) 0.2881(2) 0.4244(4) 0.0445(13) Uani 1 1 d . . . H6A H -0.0298 0.2712 0.4842 0.053 Uiso 1 1 calc R . . C1B C 0.0441(3) 0.15320(18) 0.4491(3) 0.0283(10) Uani 1 1 d . . . C2B C -0.0536(4) 0.1162(2) 0.4113(3) 0.0362(11) Uani 1 1 d . . . H2B H -0.0981 0.1201 0.3485 0.043 Uiso 1 1 calc R . . C3B C -0.0841(4) 0.0742(2) 0.4669(4) 0.0438(13) Uani 1 1 d . . . H3B H -0.1475 0.0481 0.4413 0.053 Uiso 1 1 calc R . . C4B C -0.0218(4) 0.0706(2) 0.5594(4) 0.0480(13) Uani 1 1 d . . . H4B H -0.0429 0.0418 0.5968 0.058 Uiso 1 1 calc R . . C5B C 0.0703(4) 0.1081(2) 0.5977(3) 0.0461(13) Uani 1 1 d . . . H5B H 0.1110 0.1062 0.6615 0.055 Uiso 1 1 calc R . . C6B C 0.1037(4) 0.1490(2) 0.5426(3) 0.0347(11) Uani 1 1 d . . . H6B H 0.1680 0.1744 0.5692 0.042 Uiso 1 1 calc R . . C1C C 0.3818(4) 0.11515(19) 0.5804(3) 0.0333(11) Uani 1 1 d . . . C2C C 0.3949(4) 0.0493(2) 0.5869(4) 0.0474(13) Uani 1 1 d . . . H2C H 0.3882 0.0251 0.5341 0.057 Uiso 1 1 calc R . . C3C C 0.4180(5) 0.0195(2) 0.6713(4) 0.0685(18) Uani 1 1 d . . . H3C H 0.4242 -0.0252 0.6752 0.082 Uiso 1 1 calc R . . C4C C 0.4319(5) 0.0544(3) 0.7485(4) 0.0609(16) Uani 1 1 d . . . H4C H 0.4491 0.0338 0.8058 0.073 Uiso 1 1 calc R . . C5C C 0.4209(4) 0.1198(2) 0.7432(4) 0.0535(14) Uani 1 1 d . . . H5C H 0.4300 0.1438 0.7966 0.064 Uiso 1 1 calc R . . C6C C 0.3965(4) 0.1499(2) 0.6589(3) 0.0431(12) Uani 1 1 d . . . H6C H 0.3899 0.1946 0.6554 0.052 Uiso 1 1 calc R . . C1D C 0.4845(4) 0.1718(2) 0.4587(3) 0.0336(11) Uani 1 1 d . . . C2D C 0.5792(4) 0.1368(2) 0.5068(4) 0.0480(13) Uani 1 1 d . . . H2D H 0.5768 0.1068 0.5511 0.058 Uiso 1 1 calc R . . C3D C 0.6773(5) 0.1460(3) 0.4899(4) 0.0658(17) Uani 1 1 d . . . H3D H 0.7413 0.1218 0.5225 0.079 Uiso 1 1 calc R . . C4D C 0.6820(4) 0.1892(3) 0.4272(4) 0.0650(17) Uani 1 1 d . . . H4D H 0.7493 0.1951 0.4165 0.078 Uiso 1 1 calc R . . C5D C 0.5881(4) 0.2254(2) 0.3779(4) 0.0532(14) Uani 1 1 d . . . H5D H 0.5919 0.2555 0.3343 0.064 Uiso 1 1 calc R . . C6D C 0.4896(4) 0.2166(2) 0.3935(3) 0.0419(12) Uani 1 1 d . . . H6D H 0.4258 0.2407 0.3604 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02408(15) 0.02189(13) 0.02590(15) 0.00037(15) 0.00929(12) -0.00235(15) Fe1 0.0374(4) 0.0374(3) 0.0327(4) -0.0097(3) 0.0185(3) -0.0095(3) C1 0.031(3) 0.044(3) 0.024(2) 0.000(2) 0.008(2) -0.005(2) C2 0.035(3) 0.045(3) 0.028(3) 0.005(2) 0.012(2) -0.011(2) C3 0.050(3) 0.060(3) 0.026(3) -0.003(2) 0.020(2) -0.006(3) C4 0.051(3) 0.070(4) 0.028(3) -0.016(3) 0.002(2) -0.003(3) C5 0.040(3) 0.052(3) 0.032(3) -0.012(2) 0.017(2) -0.019(2) C6 0.036(3) 0.034(2) 0.048(3) -0.012(2) 0.024(2) -0.002(2) C7 0.057(3) 0.040(3) 0.058(4) -0.018(2) 0.033(3) -0.003(3) C8 0.052(3) 0.033(3) 0.056(3) -0.013(2) 0.027(3) -0.014(2) C9 0.044(3) 0.025(2) 0.048(3) -0.002(2) 0.025(2) -0.004(2) C10 0.036(3) 0.020(2) 0.045(3) -0.0009(19) 0.023(2) -0.0024(19) O1 0.0355(18) 0.0256(14) 0.0318(18) 0.0023(13) 0.0133(14) 0.0022(13) O2 0.088(3) 0.046(2) 0.040(2) 0.0070(17) 0.030(2) 0.0056(19) C11 0.033(3) 0.032(2) 0.031(3) -0.003(2) 0.005(2) -0.002(2) C12 0.053(4) 0.035(3) 0.054(4) 0.011(3) 0.016(3) 0.006(3) F1 0.163(4) 0.0529(19) 0.061(2) 0.0176(17) 0.003(2) 0.037(2) F2 0.083(3) 0.0458(19) 0.192(5) 0.008(2) 0.083(3) 0.0140(18) C13 0.102(6) 0.033(3) 0.076(5) -0.005(3) 0.037(4) 0.002(3) F3 0.105(3) 0.0320(16) 0.131(3) -0.0131(18) 0.039(2) 0.0037(17) F4 0.168(4) 0.067(2) 0.073(3) -0.018(2) 0.001(3) 0.000(2) F5 0.093(3) 0.073(2) 0.230(6) -0.027(3) 0.098(4) -0.026(2) O3 0.036(2) 0.0473(19) 0.050(2) -0.0220(17) 0.0133(17) -0.0030(16) O4 0.058(2) 0.065(2) 0.053(2) -0.0093(19) 0.023(2) -0.008(2) C14 0.037(3) 0.044(3) 0.060(4) 0.009(3) 0.021(3) 0.013(2) F6 0.089(3) 0.115(3) 0.108(3) -0.069(3) 0.038(2) -0.022(2) F7 0.088(3) 0.060(2) 0.173(4) 0.055(2) 0.014(3) -0.013(2) C15 0.046(3) 0.038(3) 0.063(4) -0.016(3) 0.001(3) -0.007(3) C16 0.035(3) 0.083(5) 0.077(5) -0.012(4) 0.018(3) -0.007(3) F8 0.036(2) 0.144(3) 0.138(4) -0.046(3) 0.008(2) -0.035(2) F9 0.091(3) 0.205(5) 0.118(4) -0.079(4) 0.070(3) -0.046(3) F10 0.060(2) 0.112(3) 0.152(4) 0.035(3) 0.028(2) 0.037(2) P1 0.0247(6) 0.0271(5) 0.0256(6) -0.0002(5) 0.0096(5) -0.0034(5) P2 0.0278(6) 0.0262(6) 0.0294(6) 0.0008(5) 0.0111(5) 0.0004(5) C1A 0.027(2) 0.026(2) 0.032(3) -0.0001(18) 0.008(2) -0.0033(18) C2A 0.049(3) 0.041(3) 0.050(3) 0.009(2) 0.006(3) 0.004(3) C3A 0.072(4) 0.048(3) 0.066(5) 0.012(3) -0.001(4) 0.014(3) C4A 0.038(3) 0.034(3) 0.113(6) 0.008(3) 0.002(4) 0.003(3) C5A 0.049(4) 0.044(3) 0.097(5) -0.011(3) 0.038(3) 0.002(3) C6A 0.038(3) 0.036(3) 0.058(4) 0.003(2) 0.014(3) 0.004(2) C1B 0.028(2) 0.026(2) 0.034(3) -0.0001(19) 0.015(2) 0.0040(19) C2B 0.029(3) 0.038(3) 0.044(3) -0.006(2) 0.016(2) -0.006(2) C3B 0.039(3) 0.040(3) 0.060(4) -0.007(2) 0.027(3) -0.015(2) C4B 0.062(4) 0.037(3) 0.063(4) 0.005(3) 0.045(3) -0.003(3) C5B 0.056(3) 0.052(3) 0.035(3) 0.008(2) 0.023(3) -0.003(3) C6B 0.036(3) 0.036(2) 0.037(3) -0.003(2) 0.019(2) -0.004(2) C1C 0.033(3) 0.029(2) 0.034(3) 0.008(2) 0.007(2) 0.005(2) C2C 0.066(4) 0.034(3) 0.047(3) 0.013(2) 0.026(3) 0.014(2) C3C 0.086(5) 0.043(3) 0.075(5) 0.024(3) 0.027(4) 0.020(3) C4C 0.075(4) 0.063(4) 0.044(4) 0.026(3) 0.021(3) 0.017(3) C5C 0.066(4) 0.057(3) 0.039(3) 0.006(3) 0.020(3) 0.009(3) C6C 0.046(3) 0.039(3) 0.044(3) 0.006(2) 0.017(3) 0.003(2) C1D 0.030(3) 0.035(2) 0.036(3) -0.009(2) 0.012(2) 0.000(2) C2D 0.041(3) 0.059(3) 0.045(3) 0.002(3) 0.017(3) 0.008(3) C3D 0.035(3) 0.093(5) 0.069(4) 0.003(4) 0.019(3) 0.013(3) C4D 0.029(3) 0.096(5) 0.080(5) -0.026(4) 0.033(3) -0.011(3) C5D 0.055(4) 0.051(3) 0.068(4) -0.001(3) 0.039(3) -0.013(3) C6D 0.037(3) 0.042(3) 0.051(3) -0.002(2) 0.020(2) -0.011(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 O3 2.065(3) . ? Pd1 O1 2.076(3) . ? Pd1 P1 2.2525(11) . ? Pd1 P2 2.2685(11) . ? Fe1 C1 2.004(4) . ? Fe1 C9 2.009(4) . ? Fe1 C2 2.016(4) . ? Fe1 C10 2.024(4) . ? Fe1 C6 2.026(4) . ? Fe1 C5 2.028(5) . ? Fe1 C8 2.045(4) . ? Fe1 C7 2.052(5) . ? Fe1 C3 2.056(5) . ? Fe1 C4 2.061(5) . ? C1 C2 1.442(6) . ? C1 C5 1.446(5) . ? C1 P1 1.781(5) . ? C2 C3 1.393(6) . ? C3 C4 1.401(6) . ? C4 C5 1.406(7) . ? C6 C7 1.401(6) . ? C6 C10 1.418(6) . ? C7 C8 1.408(6) . ? C8 C9 1.399(6) . ? C9 C10 1.437(5) . ? C10 P2 1.806(4) . ? O1 C11 1.272(5) . ? O2 C11 1.197(5) . ? C11 C12 1.543(6) . ? C12 F1 1.327(6) . ? C12 F2 1.373(6) . ? C12 C13 1.471(8) . ? C13 F4 1.290(7) . ? C13 F5 1.318(7) . ? C13 F3 1.332(6) . ? O3 C14 1.201(6) . ? O4 C14 1.245(6) . ? C14 C15 1.572(7) . ? F6 C15 1.345(6) . ? F7 C15 1.301(6) . ? C15 C16 1.510(8) . ? C16 F9 1.273(7) . ? C16 F8 1.303(6) . ? C16 F10 1.329(7) . ? P1 C1B 1.810(4) . ? P1 C1A 1.815(4) . ? P2 C1D 1.806(5) . ? P2 C1C 1.818(4) . ? C1A C6A 1.371(6) . ? C1A C2A 1.389(6) . ? C2A C3A 1.372(7) . ? C3A C4A 1.364(9) . ? C4A C5A 1.392(8) . ? C5A C6A 1.406(6) . ? C1B C6B 1.379(6) . ? C1B C2B 1.406(5) . ? C2B C3B 1.382(6) . ? C3B C4B 1.371(6) . ? C4B C5B 1.362(6) . ? C5B C6B 1.382(6) . ? C1C C6C 1.373(6) . ? C1C C2C 1.389(5) . ? C2C C3C 1.383(7) . ? C3C C4C 1.360(7) . ? C4C C5C 1.376(6) . ? C5C C6C 1.382(6) . ? C1D C2D 1.383(6) . ? C1D C6D 1.397(6) . ? C2D C3D 1.383(7) . ? C3D C4D 1.347(8) . ? C4D C5D 1.392(7) . ? C5D C6D 1.377(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Pd1 O1 85.53(11) . . ? O3 Pd1 P1 174.29(10) . . ? O1 Pd1 P1 90.03(8) . . ? O3 Pd1 P2 88.08(9) . . ? O1 Pd1 P2 173.59(8) . . ? P1 Pd1 P2 96.38(4) . . ? C1 Fe1 C9 110.27(18) . . ? C1 Fe1 C2 42.04(17) . . ? C9 Fe1 C2 139.79(18) . . ? C1 Fe1 C10 109.87(17) . . ? C9 Fe1 C10 41.76(16) . . ? C2 Fe1 C10 110.63(16) . . ? C1 Fe1 C6 138.71(17) . . ? C9 Fe1 C6 69.06(19) . . ? C2 Fe1 C6 110.83(18) . . ? C10 Fe1 C6 40.97(17) . . ? C1 Fe1 C5 42.03(16) . . ? C9 Fe1 C5 111.09(19) . . ? C2 Fe1 C5 69.58(18) . . ? C10 Fe1 C5 139.63(18) . . ? C6 Fe1 C5 179.22(18) . . ? C1 Fe1 C8 138.9(2) . . ? C9 Fe1 C8 40.37(17) . . ? C2 Fe1 C8 179.0(2) . . ? C10 Fe1 C8 68.91(17) . . ? C6 Fe1 C8 68.26(18) . . ? C5 Fe1 C8 111.33(19) . . ? C1 Fe1 C7 177.97(19) . . ? C9 Fe1 C7 67.9(2) . . ? C2 Fe1 C7 138.9(2) . . ? C10 Fe1 C7 68.22(18) . . ? C6 Fe1 C7 40.17(16) . . ? C5 Fe1 C7 139.10(18) . . ? C8 Fe1 C7 40.20(18) . . ? C1 Fe1 C3 69.12(18) . . ? C9 Fe1 C3 179.3(2) . . ? C2 Fe1 C3 39.98(16) . . ? C10 Fe1 C3 138.72(18) . . ? C6 Fe1 C3 111.7(2) . . ? C5 Fe1 C3 68.19(19) . . ? C8 Fe1 C3 139.87(19) . . ? C7 Fe1 C3 112.7(2) . . ? C1 Fe1 C4 68.88(18) . . ? C9 Fe1 C4 139.7(2) . . ? C2 Fe1 C4 67.56(19) . . ? C10 Fe1 C4 178.19(18) . . ? C6 Fe1 C4 139.2(2) . . ? C5 Fe1 C4 40.20(19) . . ? C8 Fe1 C4 112.9(2) . . ? C7 Fe1 C4 113.1(2) . . ? C3 Fe1 C4 39.79(18) . . ? C2 C1 C5 106.0(4) . . ? C2 C1 P1 121.9(3) . . ? C5 C1 P1 131.8(4) . . ? C2 C1 Fe1 69.4(3) . . ? C5 C1 Fe1 69.9(3) . . ? P1 C1 Fe1 120.6(2) . . ? C3 C2 C1 108.7(4) . . ? C3 C2 Fe1 71.6(3) . . ? C1 C2 Fe1 68.6(2) . . ? C2 C3 C4 108.5(4) . . ? C2 C3 Fe1 68.5(3) . . ? C4 C3 Fe1 70.3(3) . . ? C3 C4 C5 109.3(4) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 68.6(3) . . ? C4 C5 C1 107.5(4) . . ? C4 C5 Fe1 71.2(3) . . ? C1 C5 Fe1 68.1(2) . . ? C7 C6 C10 108.4(4) . . ? C7 C6 Fe1 70.9(3) . . ? C10 C6 Fe1 69.4(3) . . ? C6 C7 C8 108.8(5) . . ? C6 C7 Fe1 68.9(3) . . ? C8 C7 Fe1 69.6(3) . . ? C9 C8 C7 107.8(4) . . ? C9 C8 Fe1 68.4(2) . . ? C7 C8 Fe1 70.2(3) . . ? C8 C9 C10 108.5(4) . . ? C8 C9 Fe1 71.2(3) . . ? C10 C9 Fe1 69.7(2) . . ? C6 C10 C9 106.5(4) . . ? C6 C10 P2 126.5(3) . . ? C9 C10 P2 126.9(3) . . ? C6 C10 Fe1 69.6(3) . . ? C9 C10 Fe1 68.6(2) . . ? P2 C10 Fe1 123.6(2) . . ? C11 O1 Pd1 113.6(3) . . ? O2 C11 O1 129.4(4) . . ? O2 C11 C12 118.8(5) . . ? O1 C11 C12 111.8(4) . . ? F1 C12 F2 105.0(4) . . ? F1 C12 C13 108.9(5) . . ? F2 C12 C13 104.8(5) . . ? F1 C12 C11 110.9(4) . . ? F2 C12 C11 110.9(4) . . ? C13 C12 C11 115.6(4) . . ? F4 C13 F5 105.3(6) . . ? F4 C13 F3 109.1(5) . . ? F5 C13 F3 107.1(5) . . ? F4 C13 C12 113.9(5) . . ? F5 C13 C12 108.9(6) . . ? F3 C13 C12 112.0(5) . . ? C14 O3 Pd1 118.8(4) . . ? O3 C14 O4 131.2(5) . . ? O3 C14 C15 113.5(5) . . ? O4 C14 C15 115.3(5) . . ? F7 C15 F6 106.2(4) . . ? F7 C15 C16 108.2(6) . . ? F6 C15 C16 106.2(5) . . ? F7 C15 C14 112.4(4) . . ? F6 C15 C14 108.8(5) . . ? C16 C15 C14 114.5(4) . . ? F9 C16 F8 109.0(6) . . ? F9 C16 F10 106.2(6) . . ? F8 C16 F10 108.6(6) . . ? F9 C16 C15 112.6(6) . . ? F8 C16 C15 112.1(5) . . ? F10 C16 C15 108.2(5) . . ? C1 P1 C1B 111.79(19) . . ? C1 P1 C1A 105.2(2) . . ? C1B P1 C1A 102.05(19) . . ? C1 P1 Pd1 111.43(15) . . ? C1B P1 Pd1 111.64(14) . . ? C1A P1 Pd1 114.29(13) . . ? C1D P2 C10 100.4(2) . . ? C1D P2 C1C 106.9(2) . . ? C10 P2 C1C 104.0(2) . . ? C1D P2 Pd1 108.24(14) . . ? C10 P2 Pd1 121.85(14) . . ? C1C P2 Pd1 113.94(15) . . ? C6A C1A C2A 119.4(4) . . ? C6A C1A P1 119.5(3) . . ? C2A C1A P1 121.0(4) . . ? C3A C2A C1A 119.7(5) . . ? C4A C3A C2A 121.7(6) . . ? C3A C4A C5A 119.8(5) . . ? C4A C5A C6A 118.5(6) . . ? C1A C6A C5A 120.9(5) . . ? C6B C1B C2B 118.5(4) . . ? C6B C1B P1 118.9(3) . . ? C2B C1B P1 122.4(3) . . ? C3B C2B C1B 119.8(4) . . ? C4B C3B C2B 120.1(4) . . ? C5B C4B C3B 120.7(5) . . ? C4B C5B C6B 119.9(5) . . ? C1B C6B C5B 120.9(4) . . ? C6C C1C C2C 119.2(4) . . ? C6C C1C P2 120.0(3) . . ? C2C C1C P2 120.8(4) . . ? C3C C2C C1C 119.7(5) . . ? C4C C3C C2C 120.5(5) . . ? C3C C4C C5C 120.3(5) . . ? C4C C5C C6C 119.6(5) . . ? C1C C6C C5C 120.7(4) . . ? C2D C1D C6D 119.2(5) . . ? C2D C1D P2 121.3(4) . . ? C6D C1D P2 119.2(3) . . ? C1D C2D C3D 120.1(5) . . ? C4D C3D C2D 120.5(5) . . ? C3D C4D C5D 120.6(5) . . ? C6D C5D C4D 119.6(5) . . ? C5D C6D C1D 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.902 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.136 #===END data_007 _database_code_CSD 165080 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H32 Ag F15 Fe O8 P2 Pd' _chemical_formula_weight 1293.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Ag' 'Ag' -0.8971 1.1015 '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 11.8087(1) _cell_length_b 13.7473(2) _cell_length_c 14.9548(1) _cell_angle_alpha 83.046(1) _cell_angle_beta 74.119(1) _cell_angle_gamma 82.730(1) _cell_volume 2306.77(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'mulfaced blocks' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.4700 _exptl_absorpt_correction_T_max 0.6474 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13307 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9075 _reflns_number_gt 8323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^)+(0.0860P)^2^+10.6966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9075 _refine_ls_number_parameters 607 _refine_ls_number_restraints 694 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1706 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.356 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63247(4) 0.19205(3) 0.27470(3) 0.02508(17) Uani 1 1 d . . . Ag1 Ag 0.83487(6) 0.27075(7) 0.11274(4) 0.0659(3) Uani 1 1 d . . . Fe1 Fe 0.37401(8) 0.23485(7) 0.11483(6) 0.0298(2) Uani 1 1 d . . . C1 C 0.5107(6) 0.1321(5) 0.1053(4) 0.0292(12) Uani 1 1 d . . . C2 C 0.4189(6) 0.0958(5) 0.0750(5) 0.0370(15) Uani 1 1 d . . . H2 H 0.3796 0.0404 0.1010 0.044 Uiso 1 1 calc R . . C3 C 0.4001(7) 0.1607(6) -0.0024(5) 0.0461(18) Uani 1 1 d . . . H3 H 0.3457 0.1551 -0.0358 0.055 Uiso 1 1 calc R . . C4 C 0.4777(7) 0.2350(6) -0.0201(5) 0.0460(18) Uani 1 1 d . . . H4 H 0.4828 0.2865 -0.0670 0.055 Uiso 1 1 calc R . . C5 C 0.5459(6) 0.2182(5) 0.0450(4) 0.0360(14) Uani 1 1 d . . . H5 H 0.6040 0.2565 0.0483 0.043 Uiso 1 1 calc R . . C6 C 0.3547(5) 0.3017(5) 0.2312(4) 0.0304(13) Uani 1 1 d . . . C7 C 0.2717(6) 0.2290(6) 0.2477(5) 0.0379(15) Uani 1 1 d . . . H7 H 0.2671 0.1738 0.2907 0.045 Uiso 1 1 calc R . . C8 C 0.1975(6) 0.2573(7) 0.1858(6) 0.0470(18) Uani 1 1 d . . . H8 H 0.1355 0.2239 0.1820 0.056 Uiso 1 1 calc R . . C9 C 0.2340(7) 0.3435(6) 0.1323(6) 0.0452(18) Uani 1 1 d . . . H9 H 0.2008 0.3764 0.0859 0.054 Uiso 1 1 calc R . . C10 C 0.3297(6) 0.3735(5) 0.1594(5) 0.0369(15) Uani 1 1 d . . . H10 H 0.3689 0.4293 0.1351 0.044 Uiso 1 1 calc R . . P1 P 0.57644(13) 0.08234(11) 0.19807(10) 0.0246(3) Uani 1 1 d . . . P2 P 0.46721(14) 0.30108(11) 0.29096(11) 0.0265(3) Uani 1 1 d . . . C1A C 0.7029(5) 0.0022(5) 0.1389(4) 0.0300(13) Uani 1 1 d . . . C2A C 0.7642(6) 0.0300(5) 0.0470(5) 0.0371(14) Uani 1 1 d . . . H2A H 0.7412 0.0892 0.0166 0.045 Uiso 1 1 calc R . . C3A C 0.8591(7) -0.0312(7) 0.0018(6) 0.0512(19) Uani 1 1 d . . . H3A H 0.8992 -0.0134 -0.0596 0.061 Uiso 1 1 calc R . . C4A C 0.8953(8) -0.1185(7) 0.0465(7) 0.058(2) Uani 1 1 d . . . H4A H 0.9596 -0.1590 0.0155 0.070 Uiso 1 1 calc R . . C5A C 0.8358(8) -0.1454(7) 0.1373(6) 0.055(2) Uani 1 1 d . . . H5A H 0.8599 -0.2044 0.1674 0.066 Uiso 1 1 calc R . . C6A C 0.7409(7) -0.0856(5) 0.1836(5) 0.0404(16) Uani 1 1 d . . . H6A H 0.7020 -0.1039 0.2452 0.048 Uiso 1 1 calc R . . C1B C 0.4789(5) 0.0010(4) 0.2791(4) 0.0298(12) Uani 1 1 d . . . C2B C 0.4395(6) 0.0188(5) 0.3732(5) 0.0354(14) Uani 1 1 d . . . H2B H 0.4631 0.0724 0.3934 0.043 Uiso 1 1 calc R . . C3B C 0.3650(7) -0.0434(6) 0.4368(6) 0.0491(19) Uani 1 1 d . . . H3B H 0.3381 -0.0307 0.4992 0.059 Uiso 1 1 calc R . . C4B C 0.3315(7) -0.1228(7) 0.4074(7) 0.055(2) Uani 1 1 d . . . H4B H 0.2818 -0.1643 0.4499 0.066 Uiso 1 1 calc R . . C5B C 0.3713(8) -0.1418(6) 0.3147(7) 0.054(2) Uani 1 1 d . . . H5B H 0.3482 -0.1963 0.2954 0.065 Uiso 1 1 calc R . . C6B C 0.4452(7) -0.0808(5) 0.2501(5) 0.0398(15) Uani 1 1 d . . . H6B H 0.4719 -0.0944 0.1879 0.048 Uiso 1 1 calc R . . C1C C 0.3838(6) 0.2896(5) 0.4135(4) 0.0301(12) Uani 1 1 d . . . C2C C 0.4374(6) 0.2460(5) 0.4817(4) 0.0340(14) Uani 1 1 d . . . H2C H 0.5172 0.2231 0.4659 0.041 Uiso 1 1 calc R . . C3C C 0.3702(7) 0.2367(6) 0.5750(5) 0.0422(16) Uani 1 1 d . . . H3C H 0.4056 0.2068 0.6210 0.051 Uiso 1 1 calc R . . C4C C 0.2538(8) 0.2710(7) 0.5988(5) 0.0512(19) Uani 1 1 d . . . H4C H 0.2100 0.2638 0.6607 0.061 Uiso 1 1 calc R . . C5C C 0.2000(7) 0.3170(7) 0.5305(6) 0.054(2) Uani 1 1 d . . . H5C H 0.1210 0.3422 0.5472 0.064 Uiso 1 1 calc R . . C6C C 0.2640(7) 0.3254(6) 0.4382(5) 0.0437(17) Uani 1 1 d . . . H6C H 0.2277 0.3547 0.3924 0.052 Uiso 1 1 calc R . . C1D C 0.5134(6) 0.4251(5) 0.2667(5) 0.0324(13) Uani 1 1 d . . . C2D C 0.4827(8) 0.4908(6) 0.3339(6) 0.0488(18) Uani 1 1 d . . . H2D H 0.4343 0.4728 0.3926 0.059 Uiso 1 1 calc R . . C3D C 0.5229(10) 0.5830(6) 0.3150(8) 0.064(3) Uani 1 1 d . . . H3D H 0.5017 0.6270 0.3608 0.076 Uiso 1 1 calc R . . C4D C 0.5946(9) 0.6096(7) 0.2283(8) 0.063(3) Uani 1 1 d . . . H4D H 0.6233 0.6712 0.2161 0.075 Uiso 1 1 calc R . . C5D C 0.6242(8) 0.5457(6) 0.1597(7) 0.055(2) Uani 1 1 d . . . H5D H 0.6709 0.5650 0.1007 0.066 Uiso 1 1 calc R . . C6D C 0.5848(7) 0.4528(5) 0.1779(6) 0.0423(16) Uani 1 1 d . . . H6D H 0.6055 0.4093 0.1317 0.051 Uiso 1 1 calc R . . O1 O 0.6905(4) 0.2851(4) 0.3523(3) 0.0376(11) Uani 1 1 d . . . O2 O 0.8282(6) 0.3537(5) 0.2351(4) 0.0578(15) Uani 1 1 d . . . C11 C 0.7692(6) 0.3410(5) 0.3160(5) 0.0385(15) Uani 1 1 d D . . C12 C 0.7984(7) 0.4069(6) 0.3834(6) 0.057(2) Uani 1 1 d D A . F1 F 0.7040(5) 0.4204(7) 0.4568(5) 0.111(3) Uani 1 1 d D . . F2 F 0.8197(8) 0.4986(4) 0.3376(6) 0.105(3) Uani 1 1 d D . . C13 C 0.9014(8) 0.3692(6) 0.4180(6) 0.066(3) Uani 1 1 d D . . F3 F 0.9121(10) 0.4268(8) 0.4836(7) 0.079(4) Uiso 0.60 1 d PD A . F4 F 0.9994(8) 0.3770(9) 0.3438(7) 0.080(3) Uiso 0.60 1 d PD A . F5 F 0.8996(11) 0.2757(7) 0.4541(8) 0.086(4) Uiso 0.60 1 d PD A . F3A F 0.9944(10) 0.3329(11) 0.3531(9) 0.063(2) Uiso 0.40 1 d PD A 3 F4A F 0.8600(12) 0.2932(9) 0.4833(9) 0.063(2) Uiso 0.40 1 d PD A 3 F5A F 0.9378(13) 0.4383(9) 0.4573(11) 0.063(2) Uiso 0.40 1 d PD A 3 O3 O 0.7688(4) 0.0879(4) 0.2993(4) 0.0424(12) Uani 1 1 d . . . O4 O 0.9288(5) 0.1317(6) 0.1880(5) 0.0655(17) Uani 1 1 d . . . C14 C 0.8762(7) 0.0840(6) 0.2576(6) 0.052(2) Uani 1 1 d D B . C15 C 0.9421(10) -0.0091(8) 0.3008(8) 0.103(4) Uiso 1 1 d D . . F6 F 0.9820(18) -0.0901(13) 0.2519(12) 0.119(3) Uiso 0.50 1 d PD B . F7 F 0.8716(16) -0.0484(14) 0.3913(11) 0.119(3) Uiso 0.50 1 d PD B . F6A F 0.8821(14) -0.0887(12) 0.3407(12) 0.107(2) Uiso 0.50 1 d PD B 1 F7A F 1.0392(14) -0.0466(13) 0.2299(11) 0.107(2) Uiso 0.50 1 d PD B 1 C16 C 1.0428(17) 0.0101(13) 0.3315(13) 0.119(3) Uiso 0.50 1 d PD B . F8 F 0.9961(16) 0.0866(11) 0.3860(12) 0.119(3) Uiso 0.50 1 d PD . . F9 F 1.1231(13) 0.0340(12) 0.2515(11) 0.119(3) Uiso 0.50 1 d PD . . F10 F 1.0770(15) -0.0794(11) 0.3734(12) 0.119(3) Uiso 0.50 1 d PD . . C16A C 0.9897(17) 0.0203(14) 0.3688(15) 0.107(2) Uiso 0.50 1 d PD B 2 F8A F 0.9055(13) 0.0570(11) 0.4391(10) 0.107(2) Uiso 0.50 1 d PD B 2 F9A F 1.0651(14) 0.0935(10) 0.3326(11) 0.107(2) Uiso 0.50 1 d PD B 2 F10A F 1.0555(14) -0.0557(11) 0.4073(11) 0.107(2) Uiso 0.50 1 d PD B 2 O5 O 0.8322(5) 0.2604(4) -0.0299(4) 0.0516(14) Uani 1 1 d . . . O6 O 0.7445(8) 0.4117(5) -0.0381(5) 0.081(2) Uani 1 1 d . . . C17 C 0.7885(7) 0.3342(6) -0.0697(5) 0.0441(17) Uani 1 1 d D . . C18 C 0.7832(7) 0.3236(6) -0.1712(6) 0.062(2) Uani 1 1 d D C . F11 F 0.7815(8) 0.2250(5) -0.1805(5) 0.100(2) Uani 1 1 d D . . F12 F 0.6802(6) 0.3701(7) -0.1856(5) 0.102(2) Uani 1 1 d D . . C19 C 0.8803(10) 0.3613(8) -0.2460(6) 0.095(5) Uani 1 1 d D . . F13 F 0.8959(13) 0.4554(8) -0.2285(10) 0.095(3) Uiso 0.50 1 d PD C . F14 F 0.8666(13) 0.3655(11) -0.3308(7) 0.095(3) Uiso 0.50 1 d PD C . F15 F 0.9786(10) 0.2998(10) -0.2384(11) 0.095(3) Uiso 0.50 1 d PD C . F13A F 0.8584(12) 0.4584(7) -0.2588(10) 0.087(3) Uiso 0.50 1 d PD C 5 F14A F 0.8706(12) 0.3182(10) -0.3242(8) 0.087(3) Uiso 0.50 1 d PD C 5 F15A F 0.9864(9) 0.3348(10) -0.2307(10) 0.087(3) Uiso 0.50 1 d PD C 5 O1S O 1.0739(6) 0.3754(5) -0.0472(6) 0.073(2) Uani 1 1 d . . . O2S O 0.9560(13) 0.5175(11) 0.0596(11) 0.063(3) Uiso 0.50 1 d P . . O3S O 0.9709(14) 0.5652(14) 0.0237(11) 0.066(4) Uiso 0.50 1 d P . . 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 0.0238(3) 0.0296(3) 0.0238(3) -0.00196(17) -0.00978(18) -0.00221(17) Ag1 0.0499(4) 0.1151(7) 0.0341(3) -0.0047(3) -0.0143(3) -0.0078(4) Fe1 0.0284(5) 0.0370(5) 0.0267(5) -0.0027(4) -0.0126(4) -0.0009(4) C1 0.030(3) 0.034(3) 0.027(3) -0.004(2) -0.013(2) 0.000(2) C2 0.042(4) 0.036(3) 0.040(4) -0.011(3) -0.022(3) 0.001(3) C3 0.054(5) 0.060(5) 0.033(4) -0.011(3) -0.028(3) 0.005(4) C4 0.051(4) 0.060(5) 0.023(3) 0.002(3) -0.011(3) 0.009(4) C5 0.031(3) 0.046(4) 0.026(3) 0.002(3) -0.004(3) 0.001(3) C6 0.027(3) 0.037(3) 0.027(3) -0.006(2) -0.009(2) 0.001(2) C7 0.029(3) 0.054(4) 0.030(3) -0.005(3) -0.008(3) -0.003(3) C8 0.026(3) 0.069(5) 0.050(4) -0.008(4) -0.017(3) 0.000(3) C9 0.035(4) 0.058(5) 0.047(4) -0.011(3) -0.023(3) 0.013(3) C10 0.040(4) 0.035(3) 0.039(4) -0.007(3) -0.019(3) 0.006(3) P1 0.0252(7) 0.0276(7) 0.0216(7) -0.0019(5) -0.0076(6) -0.0016(6) P2 0.0279(8) 0.0293(7) 0.0237(7) -0.0038(6) -0.0095(6) -0.0007(6) C1A 0.028(3) 0.033(3) 0.030(3) -0.004(2) -0.011(2) -0.001(2) C2A 0.038(4) 0.038(3) 0.032(3) -0.001(3) -0.004(3) -0.005(3) C3A 0.042(4) 0.060(5) 0.041(4) -0.006(4) 0.006(3) -0.002(4) C4A 0.040(4) 0.067(5) 0.059(5) -0.016(4) -0.004(4) 0.015(4) C5A 0.052(5) 0.058(5) 0.052(5) -0.003(4) -0.017(4) 0.019(4) C6A 0.041(4) 0.045(4) 0.029(3) 0.003(3) -0.008(3) 0.007(3) C1B 0.028(3) 0.028(3) 0.032(3) 0.002(2) -0.009(2) -0.001(2) C2B 0.036(3) 0.037(3) 0.032(3) -0.001(3) -0.006(3) -0.004(3) C3B 0.040(4) 0.056(5) 0.041(4) 0.009(3) 0.001(3) -0.001(3) C4B 0.039(4) 0.057(5) 0.064(6) 0.023(4) -0.011(4) -0.017(4) C5B 0.058(5) 0.043(4) 0.074(6) 0.008(4) -0.035(5) -0.022(4) C6B 0.044(4) 0.038(4) 0.041(4) 0.001(3) -0.016(3) -0.011(3) C1C 0.032(3) 0.032(3) 0.027(3) -0.006(2) -0.007(2) -0.002(2) C2C 0.031(3) 0.043(4) 0.027(3) -0.002(3) -0.007(3) -0.004(3) C3C 0.048(4) 0.050(4) 0.026(3) 0.000(3) -0.008(3) -0.005(3) C4C 0.049(5) 0.070(5) 0.029(4) -0.002(3) -0.001(3) -0.008(4) C5C 0.034(4) 0.082(6) 0.040(4) -0.013(4) -0.004(3) 0.005(4) C6C 0.038(4) 0.059(5) 0.032(4) -0.007(3) -0.010(3) 0.008(3) C1D 0.033(3) 0.027(3) 0.040(4) 0.002(3) -0.016(3) -0.003(2) C2D 0.068(5) 0.042(4) 0.043(4) -0.010(3) -0.020(4) -0.009(4) C3D 0.093(7) 0.038(4) 0.071(6) -0.010(4) -0.034(6) -0.013(4) C4D 0.073(6) 0.040(4) 0.089(7) 0.007(4) -0.044(6) -0.018(4) C5D 0.050(5) 0.051(5) 0.064(5) 0.021(4) -0.024(4) -0.015(4) C6D 0.042(4) 0.038(4) 0.047(4) 0.000(3) -0.014(3) 0.000(3) O1 0.036(3) 0.047(3) 0.036(2) -0.010(2) -0.014(2) -0.011(2) O2 0.057(4) 0.072(4) 0.046(3) -0.009(3) -0.006(3) -0.027(3) C11 0.032(3) 0.046(4) 0.043(4) -0.012(3) -0.016(3) -0.003(3) C12 0.052(5) 0.062(5) 0.066(6) -0.026(4) -0.022(4) -0.012(4) F1 0.057(4) 0.187(8) 0.102(5) -0.108(6) -0.001(3) -0.019(4) F2 0.167(8) 0.049(3) 0.137(7) -0.012(4) -0.100(6) -0.013(4) C13 0.069(6) 0.080(7) 0.064(6) -0.013(5) -0.032(5) -0.024(5) O3 0.037(3) 0.047(3) 0.047(3) -0.002(2) -0.023(2) 0.007(2) O4 0.040(3) 0.084(5) 0.064(4) 0.003(3) -0.008(3) 0.005(3) C14 0.043(4) 0.059(5) 0.056(5) -0.008(4) -0.023(4) 0.011(4) O5 0.061(4) 0.056(3) 0.044(3) 0.004(2) -0.025(3) -0.008(3) O6 0.113(6) 0.062(4) 0.066(5) -0.017(3) -0.027(4) 0.015(4) C17 0.049(4) 0.046(4) 0.035(4) 0.001(3) -0.009(3) -0.007(3) C18 0.067(6) 0.073(6) 0.052(5) -0.008(4) -0.025(5) -0.002(5) F11 0.159(8) 0.083(4) 0.082(5) -0.022(4) -0.060(5) -0.029(5) F12 0.066(4) 0.154(7) 0.092(5) -0.007(5) -0.045(4) 0.014(4) C19 0.106(10) 0.124(11) 0.033(5) -0.006(6) -0.007(5) 0.040(8) O1S 0.061(4) 0.050(4) 0.133(7) 0.016(4) -0.071(5) -0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O3 2.095(5) . ? Pd1 O1 2.114(4) . ? Pd1 P1 2.2609(15) . ? Pd1 P2 2.2808(16) . ? Pd1 Ag1 3.0987(8) . ? Ag1 O5 2.164(6) . ? Ag1 O2 2.249(6) . ? Ag1 O4 2.403(7) . ? Fe1 C1 1.992(6) . ? Fe1 C5 2.011(7) . ? Fe1 C6 2.011(6) . ? Fe1 C7 2.022(7) . ? Fe1 C2 2.034(7) . ? Fe1 C10 2.054(7) . ? Fe1 C4 2.054(7) . ? Fe1 C3 2.065(7) . ? Fe1 C9 2.066(7) . ? Fe1 C8 2.067(7) . ? C1 C5 1.431(9) . ? C1 C2 1.447(9) . ? C1 P1 1.794(6) . ? C2 C3 1.423(10) . ? C3 C4 1.411(12) . ? C4 C5 1.406(10) . ? C6 C10 1.435(9) . ? C6 C7 1.442(10) . ? C6 P2 1.791(6) . ? C7 C8 1.430(10) . ? C8 C9 1.394(12) . ? C9 C10 1.422(10) . ? P1 C1B 1.811(6) . ? P1 C1A 1.823(6) . ? P2 C1D 1.820(6) . ? P2 C1C 1.826(6) . ? C1A C6A 1.391(9) . ? C1A C2A 1.399(9) . ? C2A C3A 1.380(10) . ? C3A C4A 1.379(13) . ? C4A C5A 1.376(13) . ? C5A C6A 1.376(11) . ? C1B C6B 1.392(10) . ? C1B C2B 1.396(9) . ? C2B C3B 1.395(10) . ? C3B C4B 1.365(13) . ? C4B C5B 1.383(14) . ? C5B C6B 1.388(11) . ? C1C C2C 1.381(9) . ? C1C C6C 1.401(10) . ? C2C C3C 1.403(9) . ? C3C C4C 1.358(12) . ? C4C C5C 1.394(12) . ? C5C C6C 1.379(11) . ? C1D C2D 1.377(10) . ? C1D C6D 1.402(10) . ? C2D C3D 1.381(12) . ? C3D C4D 1.377(15) . ? C4D C5D 1.376(14) . ? C5D C6D 1.385(11) . ? O1 C11 1.246(9) . ? O2 C11 1.224(9) . ? C11 C12 1.564(9) . ? C12 F1 1.344(9) . ? C12 F2 1.378(9) . ? C12 C13 1.462(12) . ? C13 F5 1.332(11) . ? C13 F3A 1.339(11) . ? C13 F5A 1.345(11) . ? C13 F4 1.372(11) . ? C13 F3 1.372(10) . ? C13 F4A 1.380(11) . ? F4 F3A 0.612(15) . ? F5 F4A 0.593(16) . ? F5 F3A 1.778(16) . ? O3 C14 1.248(10) . ? O4 C14 1.219(11) . ? C14 C15 1.576(12) . ? C15 F6A 1.365(13) . ? C15 F6 1.368(14) . ? C15 C16A 1.41(3) . ? C15 F7A 1.422(13) . ? C15 C16 1.45(2) . ? C15 F7 1.462(14) . ? F6 F7A 0.92(2) . ? F6 F6A 1.52(2) . ? F7 F6A 0.96(2) . ? F7 C16A 1.72(3) . ? F7A F9 1.69(2) . ? F7A C16 1.80(3) . ? C16 C16A 0.73(2) . ? C16 F9A 1.21(2) . ? C16 F9 1.343(15) . ? C16 F8 1.374(15) . ? C16 F10 1.376(15) . ? C16 F10A 1.39(2) . ? F8 F9A 0.977(19) . ? F8 C16A 0.99(2) . ? F8 F8A 1.23(2) . ? F9 F9A 1.50(2) . ? F10 F10A 0.61(2) . ? F10 C16A 1.61(2) . ? C16A F8A 1.333(16) . ? C16A F10A 1.386(16) . ? C16A F9A 1.389(16) . ? O5 C17 1.240(10) . ? O6 C17 1.214(10) . ? C17 C18 1.561(10) . ? C18 F12 1.360(9) . ? C18 F11 1.383(10) . ? C18 C19 1.464(13) . ? C19 F14 1.316(11) . ? C19 F13A 1.328(12) . ? C19 F15A 1.332(12) . ? C19 F15 1.368(12) . ? C19 F13 1.395(12) . ? C19 F14A 1.411(12) . ? F13 F13A 0.709(18) . ? F14 F14A 0.644(17) . ? F14 F13A 1.745(17) . ? F15 F15A 0.533(19) . ? O1S O3S 0.963(16) 2_765 ? O1S O2S 1.471(16) 2_765 ? O2S O3S 0.801(17) . ? O2S O1S 1.471(16) 2_765 ? O2S O3S 1.760(19) 2_765 ? O3S O1S 0.963(16) 2_765 ? O3S O2S 1.760(19) 2_765 ? 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 O3 Pd1 O1 86.5(2) . . ? O3 Pd1 P1 89.46(15) . . ? O1 Pd1 P1 175.49(15) . . ? O3 Pd1 P2 164.43(16) . . ? O1 Pd1 P2 85.83(14) . . ? P1 Pd1 P2 97.64(6) . . ? O3 Pd1 Ag1 82.61(15) . . ? O1 Pd1 Ag1 83.22(14) . . ? P1 Pd1 Ag1 98.23(4) . . ? P2 Pd1 Ag1 109.86(5) . . ? O5 Ag1 O2 153.7(2) . . ? O5 Ag1 O4 117.0(2) . . ? O2 Ag1 O4 87.5(3) . . ? O5 Ag1 Pd1 119.26(16) . . ? O2 Ag1 Pd1 74.19(15) . . ? O4 Ag1 Pd1 75.54(15) . . ? C1 Fe1 C5 41.9(3) . . ? C1 Fe1 C6 107.7(2) . . ? C5 Fe1 C6 109.9(3) . . ? C1 Fe1 C7 109.3(3) . . ? C5 Fe1 C7 139.5(3) . . ? C6 Fe1 C7 41.9(3) . . ? C1 Fe1 C2 42.1(3) . . ? C5 Fe1 C2 69.9(3) . . ? C6 Fe1 C2 136.7(3) . . ? C7 Fe1 C2 109.2(3) . . ? C1 Fe1 C10 136.8(3) . . ? C5 Fe1 C10 110.2(3) . . ? C6 Fe1 C10 41.3(3) . . ? C7 Fe1 C10 69.4(3) . . ? C2 Fe1 C10 178.1(3) . . ? C1 Fe1 C4 69.3(3) . . ? C5 Fe1 C4 40.5(3) . . ? C6 Fe1 C4 140.0(3) . . ? C7 Fe1 C4 177.8(3) . . ? C2 Fe1 C4 68.6(3) . . ? C10 Fe1 C4 112.9(3) . . ? C1 Fe1 C3 69.3(3) . . ? C5 Fe1 C3 68.3(3) . . ? C6 Fe1 C3 177.0(3) . . ? C7 Fe1 C3 138.0(3) . . ? C2 Fe1 C3 40.6(3) . . ? C10 Fe1 C3 141.3(3) . . ? C4 Fe1 C3 40.1(3) . . ? C1 Fe1 C9 176.4(3) . . ? C5 Fe1 C9 138.6(3) . . ? C6 Fe1 C9 68.7(3) . . ? C7 Fe1 C9 68.1(3) . . ? C2 Fe1 C9 140.6(3) . . ? C10 Fe1 C9 40.4(3) . . ? C4 Fe1 C9 113.3(3) . . ? C3 Fe1 C9 114.2(3) . . ? C1 Fe1 C8 140.0(3) . . ? C5 Fe1 C8 178.0(3) . . ? C6 Fe1 C8 69.1(3) . . ? C7 Fe1 C8 40.9(3) . . ? C2 Fe1 C8 112.0(3) . . ? C10 Fe1 C8 67.9(3) . . ? C4 Fe1 C8 139.2(3) . . ? C3 Fe1 C8 112.7(3) . . ? C9 Fe1 C8 39.4(3) . . ? C5 C1 C2 107.3(6) . . ? C5 C1 P1 123.5(5) . . ? C2 C1 P1 129.2(5) . . ? C5 C1 Fe1 69.8(4) . . ? C2 C1 Fe1 70.5(4) . . ? P1 C1 Fe1 126.0(3) . . ? C3 C2 C1 107.0(6) . . ? C3 C2 Fe1 70.8(4) . . ? C1 C2 Fe1 67.4(4) . . ? C4 C3 C2 108.7(6) . . ? C4 C3 Fe1 69.5(4) . . ? C2 C3 Fe1 68.5(4) . . ? C5 C4 C3 108.7(6) . . ? C5 C4 Fe1 68.1(4) . . ? C3 C4 Fe1 70.4(4) . . ? C4 C5 C1 108.3(7) . . ? C4 C5 Fe1 71.4(4) . . ? C1 C5 Fe1 68.3(4) . . ? C10 C6 C7 107.4(6) . . ? C10 C6 P2 127.0(5) . . ? C7 C6 P2 125.5(5) . . ? C10 C6 Fe1 70.9(4) . . ? C7 C6 Fe1 69.5(4) . . ? P2 C6 Fe1 125.2(3) . . ? C8 C7 C6 107.4(7) . . ? C8 C7 Fe1 71.2(4) . . ? C6 C7 Fe1 68.7(4) . . ? C9 C8 C7 108.4(7) . . ? C9 C8 Fe1 70.3(4) . . ? C7 C8 Fe1 67.9(4) . . ? C8 C9 C10 109.5(6) . . ? C8 C9 Fe1 70.3(4) . . ? C10 C9 Fe1 69.3(4) . . ? C9 C10 C6 107.3(6) . . ? C9 C10 Fe1 70.3(4) . . ? C6 C10 Fe1 67.8(4) . . ? C1 P1 C1B 109.3(3) . . ? C1 P1 C1A 102.7(3) . . ? C1B P1 C1A 105.4(3) . . ? C1 P1 Pd1 116.6(2) . . ? C1B P1 Pd1 110.7(2) . . ? C1A P1 Pd1 111.4(2) . . ? C6 P2 C1D 105.3(3) . . ? C6 P2 C1C 102.6(3) . . ? C1D P2 C1C 106.4(3) . . ? C6 P2 Pd1 125.3(2) . . ? C1D P2 Pd1 108.2(2) . . ? C1C P2 Pd1 107.7(2) . . ? C6A C1A C2A 119.1(6) . . ? C6A C1A P1 121.5(5) . . ? C2A C1A P1 119.4(5) . . ? C3A C2A C1A 119.5(7) . . ? C4A C3A C2A 120.8(7) . . ? C5A C4A C3A 119.7(8) . . ? C6A C5A C4A 120.4(8) . . ? C5A C6A C1A 120.4(7) . . ? C6B C1B C2B 119.3(6) . . ? C6B C1B P1 121.3(5) . . ? C2B C1B P1 119.5(5) . . ? C3B C2B C1B 120.3(7) . . ? C4B C3B C2B 119.9(8) . . ? C3B C4B C5B 120.2(7) . . ? C4B C5B C6B 120.9(7) . . ? C5B C6B C1B 119.4(7) . . ? C2C C1C C6C 119.9(6) . . ? C2C C1C P2 120.8(5) . . ? C6C C1C P2 119.3(5) . . ? C1C C2C C3C 119.4(6) . . ? C4C C3C C2C 120.7(7) . . ? C3C C4C C5C 120.1(7) . . ? C6C C5C C4C 120.0(7) . . ? C5C C6C C1C 119.9(7) . . ? C2D C1D C6D 119.6(7) . . ? C2D C1D P2 121.6(6) . . ? C6D C1D P2 118.8(5) . . ? C1D C2D C3D 120.6(8) . . ? C4D C3D C2D 119.8(9) . . ? C5D C4D C3D 120.4(8) . . ? C4D C5D C6D 120.3(9) . . ? C5D C6D C1D 119.3(8) . . ? C11 O1 Pd1 122.7(4) . . ? C11 O2 Ag1 128.8(5) . . ? O2 C11 O1 130.5(7) . . ? O2 C11 C12 113.7(6) . . ? O1 C11 C12 115.8(6) . . ? F1 C12 F2 106.7(7) . . ? F1 C12 C13 108.8(7) . . ? F2 C12 C13 107.2(7) . . ? F1 C12 C11 109.7(6) . . ? F2 C12 C11 109.1(7) . . ? C13 C12 C11 115.0(6) . . ? F5 C13 F3A 83.5(9) . . ? F5 C13 F5A 122.3(11) . . ? F3A C13 F5A 107.9(10) . . ? F5 C13 F4 108.9(9) . . ? F3A C13 F4 26.1(7) . . ? F5A C13 F4 89.2(9) . . ? F5 C13 F3 109.2(9) . . ? F3A C13 F3 122.9(10) . . ? F5A C13 F3 19.1(8) . . ? F4 C13 F3 107.3(8) . . ? F5 C13 F4A 25.2(7) . . ? F3A C13 F4A 108.6(10) . . ? F5A C13 F4A 111.2(10) . . ? F4 C13 F4A 133.8(10) . . ? F3 C13 F4A 93.8(9) . . ? F5 C13 C12 113.8(8) . . ? F3A C13 C12 114.3(8) . . ? F5A C13 C12 111.8(9) . . ? F4 C13 C12 107.1(8) . . ? F3 C13 C12 110.3(8) . . ? F4A C13 C12 102.9(8) . . ? F3A F4 C13 73.9(12) . . ? F4A F5 C13 81.9(14) . . ? F4A F5 F3A 130.3(15) . . ? C13 F5 F3A 48.4(6) . . ? F4 F3A C13 80.0(13) . . ? F4 F3A F5 126.9(15) . . ? C13 F3A F5 48.1(6) . . ? F5 F4A C13 72.9(13) . . ? C14 O3 Pd1 127.9(5) . . ? C14 O4 Ag1 122.8(5) . . ? O4 C14 O3 130.8(7) . . ? O4 C14 C15 120.1(8) . . ? O3 C14 C15 108.6(8) . . ? F6A C15 F6 67.4(10) . . ? F6A C15 C16A 106.9(13) . . ? F6 C15 C16A 126.2(14) . . ? F6A C15 F7A 104.8(11) . . ? F6 C15 F7A 38.6(9) . . ? C16A C15 F7A 106.8(12) . . ? F6A C15 C16 119.8(13) . . ? F6 C15 C16 104.2(13) . . ? C16A C15 C16 29.4(10) . . ? F7A C15 C16 77.8(11) . . ? F6A C15 F7 39.6(9) . . ? F6 C15 F7 104.1(11) . . ? C16A C15 F7 73.5(12) . . ? F7A C15 F7 135.5(12) . . ? C16 C15 F7 97.4(12) . . ? F6A C15 C14 119.7(11) . . ? F6 C15 C14 120.3(12) . . ? C16A C15 C14 108.8(10) . . ? F7A C15 C14 109.1(11) . . ? C16 C15 C14 115.3(10) . . ? F7 C15 C14 112.7(11) . . ? F7A F6 C15 73.9(13) . . ? F7A F6 F6A 128.1(16) . . ? C15 F6 F6A 56.2(8) . . ? F6A F7 C15 64.8(10) . . ? F6A F7 C16A 109.1(15) . . ? C15 F7 C16A 51.8(10) . . ? F7 F6A C15 75.6(12) . . ? F7 F6A F6 127.1(16) . . ? C15 F6A F6 56.4(8) . . ? F6 F7A C15 67.5(11) . . ? F6 F7A F9 149.4(19) . . ? C15 F7A F9 89.3(11) . . ? F6 F7A C16 104.6(16) . . ? C15 F7A C16 51.8(8) . . ? F9 F7A C16 45.1(7) . . ? C16A C16 F9A 88(2) . . ? C16A C16 F9 153(3) . . ? F9A C16 F9 71.8(13) . . ? C16A C16 F8 44(2) . . ? F9A C16 F8 43.9(10) . . ? F9 C16 F8 114.9(15) . . ? C16A C16 F10 95(2) . . ? F9A C16 F10 133(2) . . ? F9 C16 F10 111.2(14) . . ? F8 C16 F10 118.8(15) . . ? C16A C16 F10A 74(2) . . ? F9A C16 F10A 116.4(17) . . ? F9 C16 F10A 129.7(17) . . ? F8 C16 F10A 93.3(14) . . ? F10 C16 F10A 25.6(10) . . ? C16A C16 C15 72(3) . . ? F9A C16 C15 121.1(16) . . ? F9 C16 C15 103.6(14) . . ? F8 C16 C15 102.0(13) . . ? F10 C16 C15 103.9(14) . . ? F10A C16 C15 110.4(15) . . ? C16A C16 F7A 122(3) . . ? F9A C16 F7A 126.0(16) . . ? F9 C16 F7A 63.0(11) . . ? F8 C16 F7A 145.3(16) . . ? F10 C16 F7A 91.2(13) . . ? F10A C16 F7A 114.7(14) . . ? C15 C16 F7A 50.5(8) . . ? F9A F8 C16A 89.6(15) . . ? F9A F8 F8A 161.8(16) . . ? C16A F8 F8A 72.9(14) . . ? F9A F8 C16 59.2(12) . . ? C16A F8 C16 30.8(13) . . ? F8A F8 C16 103.7(14) . . ? C16 F9 F9A 50.0(10) . . ? C16 F9 F7A 71.9(11) . . ? F9A F9 F7A 115.4(10) . . ? F10A F10 C16 79(2) . . ? F10A F10 C16A 57.7(17) . . ? C16 F10 C16A 26.7(10) . . ? C16 C16A F8 105(3) . . ? C16 C16A F8A 166(3) . . ? F8 C16A F8A 61.7(15) . . ? C16 C16A F10A 75(2) . . ? F8 C16A F10A 114(2) . . ? F8A C16A F10A 107.1(16) . . ? C16 C16A F9A 61(2) . . ? F8 C16A F9A 44.7(12) . . ? F8A C16A F9A 106.2(16) . . ? F10A C16A F9A 105.9(15) . . ? C16 C16A C15 78(3) . . ? F8 C16A C15 131(2) . . ? F8A C16A C15 111.8(15) . . ? F10A C16A C15 113.2(15) . . ? F9A C16A C15 112.1(15) . . ? C16 C16A F10 58.2(19) . . ? F8 C16A F10 129(2) . . ? F8A C16A F10 127.1(16) . . ? F10A C16A F10 22.0(9) . . ? F9A C16A F10 104.5(14) . . ? C15 C16A F10 94.6(13) . . ? C16 C16A F7 121(3) . . ? F8 C16A F7 131.6(19) . . ? F8A C16A F7 72.2(12) . . ? F10A C16A F7 91.6(13) . . ? F9A C16A F7 161.8(17) . . ? C15 C16A F7 54.7(10) . . ? F10 C16A F7 89.9(13) . . ? F8 F8A C16A 45.4(11) . . ? F8 F9A C16 77.0(12) . . ? F8 F9A C16A 45.7(12) . . ? C16 F9A C16A 31.6(12) . . ? F8 F9A F9 133.9(14) . . ? C16 F9A F9 58.2(10) . . ? C16A F9A F9 88.6(12) . . ? F10 F10A C16A 100(2) . . ? F10 F10A C16 75.8(19) . . ? C16A F10A C16 30.4(11) . . ? C17 O5 Ag1 116.5(5) . . ? O6 C17 O5 128.2(8) . . ? O6 C17 C18 116.1(7) . . ? O5 C17 C18 115.6(7) . . ? F12 C18 F11 106.4(8) . . ? F12 C18 C19 107.7(7) . . ? F11 C18 C19 108.1(8) . . ? F12 C18 C17 110.0(7) . . ? F11 C18 C17 108.5(7) . . ? C19 C18 C17 115.8(7) . . ? F14 C19 F13A 82.6(10) . . ? F14 C19 F15A 120.3(12) . . ? F13A C19 F15A 112.1(11) . . ? F14 C19 F15 110.5(10) . . ? F13A C19 F15 133.8(12) . . ? F15A C19 F15 22.7(8) . . ? F14 C19 F13 108.5(10) . . ? F13A C19 F13 30.1(8) . . ? F15A C19 F13 85.6(11) . . ? F15 C19 F13 108.3(11) . . ? F14 C19 F14A 27.0(8) . . ? F13A C19 F14A 109.4(9) . . ? F15A C19 F14A 110.5(9) . . ? F15 C19 F14A 93.1(10) . . ? F13 C19 F14A 135.1(11) . . ? F14 C19 C18 115.4(10) . . ? F13A C19 C18 108.3(9) . . ? F15A C19 C18 113.4(9) . . ? F15 C19 C18 105.1(9) . . ? F13 C19 C18 108.7(8) . . ? F14A C19 C18 102.6(9) . . ? F13A F13 C19 69.7(11) . . ? F14A F14 C19 84.7(14) . . ? F14A F14 F13A 133.3(15) . . ? C19 F14 F13A 49.0(6) . . ? F15A F15 C19 74.8(16) . . ? F13 F13A C19 80.2(12) . . ? F13 F13A F14 121.6(16) . . ? C19 F13A F14 48.4(6) . . ? F14 F14A C19 68.2(12) . . ? F15 F15A C19 82.5(17) . . ? O3S O1S O2S 30.2(11) 2_765 2_765 ? O3S O2S O1S 37.2(14) . 2_765 ? O3S O2S O3S 94(2) . 2_765 ? O1S O2S O3S 129.7(15) 2_765 2_765 ? O2S O3S O1S 113(2) . 2_765 ? O2S O3S O2S 86(2) . 2_765 ? O1S O3S O2S 157.4(19) 2_765 2_765 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.756 _refine_diff_density_min -1.699 _refine_diff_density_rms 0.147