#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105311.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2105311 loop_ _publ_author_name 'Hill, Tania N.' 'Roodt, Andreas' 'Steyl, Gideon' _publ_section_title ; Electronic influence of \b-diketonato-type ligands on the coordination of 1,5-cyclooctadiene to palladium(II) as defined by `Venus fly trap' geometric parameters ; _journal_coeditor_code EB5019 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 36 _journal_page_last 42 _journal_paper_doi 10.1107/S0108768112046733 _journal_volume 69 _journal_year 2013 _chemical_formula_moiety 'C16 H16 F3 O2 Pd S, F6 P' _chemical_formula_structural '(Pd (C8 H12) (O2 S F3 C8 H7)) (P F6)' _chemical_formula_sum 'C16 H16 F9 O2 P Pd S' _chemical_formula_weight 580.72 _chemical_name_systematic ; (thenoyltrifluoroacetonato)(\h^4^-cyclo-octa-1,5-dienyl)palladium(II) hexafluorophosphate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 124.4390(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.9691(2) _cell_length_b 17.0294(3) _cell_length_c 13.6427(3) _cell_measurement_reflns_used 10209 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.0099 _cell_measurement_theta_min 2.1649 _cell_volume 1910.15(7) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_molecular_graphics 'DIAMOND 3.0c (Brandenburg & Putz, 2004)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1829 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 15058 _diffrn_reflns_theta_full 28 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_min 2.17 _exptl_absorpt_coefficient_mu 1.262 _exptl_absorpt_correction_T_max 0.8842 _exptl_absorpt_correction_T_min 0.6665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1144 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.146 _refine_diff_density_min -0.707 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4606 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.033 _refine_ls_R_factor_gt 0.0247 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.059 _refine_ls_wR_factor_ref 0.0611 _reflns_number_gt 3596 _reflns_number_total 4606 _reflns_threshold_expression >2\s(I) _iucr_refine_instructions_details ; TITL absx in P2(1)/c CELL 0.71073 9.9691 17.0294 13.6427 90.000 124.439 90.000 ZERR 4.00 0.0002 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O F P S PD UNIT 64 64 8 36 4 4 4 MERG 2 OMIT -4.00 56.00 OMIT -1 1 1 EQIV $1 -x+1, -y+2, -z+1 EQIV $2 -x+2, -y+2, -z+1 EQIV $3 x-1, y, z-1 EQIV $4 -x+1, y+0.5, -z+0.5 HTAB C10 F2 HTAB C14 F01_$1 HTAB C5 F01_$2 HTAB C6 F06_$3 HTAB C15 F03_$4 FMAP 2 PLAN 10 SIZE 0.10 0.20 0.35 ACTA BOND $H CONF LIST 4 L.S. 16 TEMP -173.20 WGHT 0.036600 FVAR 0.09619 C1 1 0.604384 0.776397 0.329097 11.00000 0.01639 0.01367 = 0.01763 0.00952 0.00957 0.00523 AFIX 13 H1 2 0.559137 0.746641 0.367405 11.00000 -1.20000 AFIX 0 C2 1 0.714244 0.834297 0.400578 11.00000 0.01310 0.01582 = 0.01086 0.00511 0.00436 0.00372 AFIX 13 H2 2 0.734596 0.838259 0.481085 11.00000 -1.20000 AFIX 0 C3 1 0.849381 0.866893 0.393657 11.00000 0.01204 0.01933 = 0.01207 0.00083 0.00464 0.00024 AFIX 23 H3A 2 0.944854 0.831705 0.438217 11.00000 -1.20000 H3B 2 0.881628 0.918833 0.433151 11.00000 -1.20000 AFIX 0 C4 1 0.804330 0.876100 0.266580 11.00000 0.01237 0.01854 = 0.01522 0.00089 0.00792 -0.00105 AFIX 23 H4A 2 0.878752 0.914568 0.266535 11.00000 -1.20000 H4B 2 0.819280 0.825106 0.239097 11.00000 -1.20000 AFIX 0 C5 1 0.630013 0.903396 0.180683 11.00000 0.01721 0.01766 = 0.01134 0.00335 0.00954 0.00234 AFIX 13 H5 2 0.619550 0.956052 0.144533 11.00000 -1.20000 AFIX 0 C6 1 0.499516 0.853900 0.110380 11.00000 0.01634 0.01937 = 0.01116 0.00121 0.00736 0.00197 AFIX 13 H6 2 0.412030 0.877202 0.032430 11.00000 -1.20000 AFIX 0 C7 1 0.503138 0.765611 0.111378 11.00000 0.01891 0.01678 = 0.01674 -0.00342 0.00813 0.00053 AFIX 23 H7A 2 0.544277 0.747546 0.064015 11.00000 -1.20000 H7B 2 0.390576 0.745816 0.072191 11.00000 -1.20000 AFIX 0 C8 1 0.609517 0.729475 0.236811 11.00000 0.01553 0.01375 = 0.02117 0.00162 0.00948 0.00040 AFIX 23 H8A 2 0.571799 0.675307 0.234544 11.00000 -1.20000 H8B 2 0.723400 0.726407 0.260614 11.00000 -1.20000 AFIX 0 C9 1 0.308053 0.943027 0.353699 11.00000 0.01189 0.01448 = 0.01431 -0.00207 0.00586 -0.00348 C10 1 0.221103 0.997499 0.265690 11.00000 0.01390 0.01502 = 0.01712 -0.00100 0.00887 -0.00010 AFIX 43 H10 2 0.141746 1.027257 0.267275 11.00000 -1.20000 AFIX 0 C11 1 0.241041 1.012794 0.171821 11.00000 0.01127 0.01129 = 0.01364 -0.00332 0.00519 -0.00363 C12 1 0.272409 0.932200 0.447072 11.00000 0.01444 0.01651 = 0.01690 0.00099 0.00847 0.00058 C13 1 0.142149 1.073538 0.085747 11.00000 0.01346 0.01320 = 0.01435 -0.00175 0.00710 -0.00080 C14 1 0.016712 1.117286 0.074909 11.00000 0.01498 0.01668 = 0.01903 0.00066 0.01036 -0.00020 AFIX 43 H14 2 -0.019355 1.111924 0.125819 11.00000 -1.20000 AFIX 0 C15 1 -0.050401 1.170481 -0.020590 11.00000 0.01479 0.01459 = 0.02497 0.00251 0.00912 0.00232 AFIX 43 H15 2 -0.137190 1.205279 -0.041404 11.00000 -1.20000 AFIX 0 C16 1 0.022701 1.166673 -0.080096 11.00000 0.01929 0.01446 = 0.01906 0.00579 0.00706 0.00232 AFIX 43 H16 2 -0.007716 1.198537 -0.146804 11.00000 -1.20000 AFIX 0 O1 3 0.421196 0.895727 0.371677 11.00000 0.01724 0.01817 = 0.01614 0.00375 0.01131 0.00372 O2 3 0.339807 0.977696 0.156166 11.00000 0.01405 0.01570 = 0.01331 0.00245 0.00705 0.00289 F01 4 1.196341 0.936496 0.829328 11.00000 0.03521 0.02109 = 0.02789 -0.00800 0.02475 -0.00455 F1 4 0.200695 0.862707 0.432881 11.00000 0.02146 0.02318 = 0.02497 0.00432 0.01534 -0.00264 F02 4 1.025606 0.857103 0.673748 11.00000 0.01777 0.03195 = 0.02374 -0.00210 0.00810 -0.00207 F2 4 0.173456 0.987185 0.442278 11.00000 0.03354 0.02666 = 0.02631 0.00687 0.02298 0.01268 F3 4 0.408799 0.933174 0.556879 11.00000 0.01907 0.03695 = 0.01420 0.00044 0.00750 -0.00234 F03 4 1.240509 0.808974 0.677023 11.00000 0.03034 0.03048 = 0.03222 -0.01733 0.01774 -0.00364 F04 4 1.409924 0.887948 0.833122 11.00000 0.01573 0.03347 = 0.03514 -0.01517 0.00853 -0.00370 F05 4 1.194813 0.939875 0.663355 11.00000 0.04308 0.02589 = 0.02413 0.00250 0.02272 -0.00323 F06 4 1.238625 0.805022 0.842231 11.00000 0.04655 0.02007 = 0.02018 0.00549 0.00953 -0.00429 P01 5 1.217852 0.872665 0.752631 11.00000 0.01571 0.01644 = 0.01293 -0.00240 0.00678 -0.00014 S1 6 0.174528 1.098534 -0.021744 11.00000 0.01977 0.01994 = 0.01611 0.00485 0.01086 0.00511 PD1 7 0.491474 0.891091 0.260022 11.00000 0.01125 0.01228 = 0.01165 0.00168 0.00606 0.00155 HKLF 4 REM absx in P2(1)/c REM R1 = 0.0247 for 3596 Fo > 4sig(Fo) and 0.0330 for all 4606 data REM 271 parameters refined using 0 restraints END WGHT 0.0366 0.0000 REM Highest difference peak 1.146, deepest hole -0.707, 1-sigma level 0.088 Q1 1 0.5044 0.8287 0.2361 11.00000 0.05 1.15 Q2 1 0.5236 0.8927 0.2143 11.00000 0.05 0.91 Q3 1 0.1021 1.0998 0.0929 11.00000 0.05 0.47 Q4 1 0.7217 0.8883 0.2376 11.00000 0.05 0.43 Q5 1 0.3901 0.8721 0.0608 11.00000 0.05 0.42 Q6 1 0.7730 0.8485 0.3896 11.00000 0.05 0.40 Q7 1 0.5857 0.9324 0.2971 11.00000 0.05 0.40 Q8 1 0.5088 0.8103 0.1097 11.00000 0.05 0.37 Q9 1 0.2892 0.9783 0.3130 11.00000 0.05 0.37 Q10 1 0.1547 0.8963 0.4984 11.00000 0.05 0.37 ; _cod_data_source_file eb5019.cif _cod_data_source_block 9Tth12_L _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2105311 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' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity C C1 0.6044(2) 0.77640(12) 0.32910(19) 0.0159(5) Uani d . 1 1 H H1 0.5591 0.7466 0.3674 0.019 Uiso calc R 1 1 C C2 0.7142(2) 0.83430(13) 0.40058(18) 0.0146(4) Uani d . 1 1 H H2 0.7346 0.8383 0.4811 0.018 Uiso calc R 1 1 C C3 0.8494(3) 0.86689(13) 0.39366(19) 0.0157(5) Uani d . 1 1 H H3A 0.9449 0.8317 0.4382 0.019 Uiso calc R 1 1 H H3B 0.8816 0.9188 0.4332 0.019 Uiso calc R 1 1 C C4 0.8043(3) 0.87610(13) 0.26658(19) 0.0153(5) Uani d . 1 1 H H4A 0.8788 0.9146 0.2665 0.018 Uiso calc R 1 1 H H4B 0.8193 0.8251 0.2391 0.018 Uiso calc R 1 1 C C5 0.6300(3) 0.90340(12) 0.18068(18) 0.0146(4) Uani d . 1 1 H H5 0.6196 0.9561 0.1445 0.018 Uiso calc R 1 1 C C6 0.4995(3) 0.85390(13) 0.11038(19) 0.0159(5) Uani d . 1 1 H H6 0.412 0.8772 0.0324 0.019 Uiso calc R 1 1 C C7 0.5031(3) 0.76561(13) 0.11138(19) 0.0186(5) Uani d . 1 1 H H7A 0.5443 0.7475 0.064 0.022 Uiso calc R 1 1 H H7B 0.3906 0.7458 0.0722 0.022 Uiso calc R 1 1 C C8 0.6095(3) 0.72948(13) 0.23681(19) 0.0173(5) Uani d . 1 1 H H8A 0.5718 0.6753 0.2345 0.021 Uiso calc R 1 1 H H8B 0.7234 0.7264 0.2606 0.021 Uiso calc R 1 1 C C9 0.3081(2) 0.94303(12) 0.35370(18) 0.0144(4) Uani d . 1 1 C C10 0.2211(2) 0.99750(13) 0.26569(19) 0.0153(4) Uani d . 1 1 H H10 0.1417 1.0273 0.2673 0.018 Uiso calc R 1 1 C C11 0.2410(2) 1.01279(12) 0.17182(18) 0.0131(4) Uani d . 1 1 C C12 0.2724(3) 0.93220(13) 0.44707(19) 0.0162(5) Uani d . 1 1 C C13 0.1421(2) 1.07354(13) 0.08575(18) 0.0141(4) Uani d . 1 1 C C14 0.0167(3) 1.11729(13) 0.0749(2) 0.0165(5) Uani d . 1 1 H H14 -0.0194 1.1119 0.1258 0.02 Uiso calc R 1 1 C C15 -0.0504(3) 1.17048(13) -0.0206(2) 0.0193(5) Uani d . 1 1 H H15 -0.1372 1.2053 -0.0414 0.023 Uiso calc R 1 1 C C16 0.0227(3) 1.16667(13) -0.0801(2) 0.0197(5) Uani d . 1 1 H H16 -0.0077 1.1985 -0.1468 0.024 Uiso calc R 1 1 O O1 0.42120(18) 0.89573(9) 0.37168(13) 0.0161(3) Uani d . 1 1 O O2 0.33981(17) 0.97770(8) 0.15617(12) 0.0147(3) Uani d . 1 1 F F01 1.19634(16) 0.93650(8) 0.82933(12) 0.0242(3) Uani d . 1 1 F F1 0.20070(16) 0.86271(8) 0.43288(12) 0.0220(3) Uani d . 1 1 F F02 1.02561(16) 0.85710(8) 0.67375(12) 0.0265(3) Uani d . 1 1 F F2 0.17346(16) 0.98719(8) 0.44228(12) 0.0255(3) Uani d . 1 1 F F3 0.40880(15) 0.93317(8) 0.55688(11) 0.0245(3) Uani d . 1 1 F F03 1.24051(17) 0.80897(8) 0.67702(12) 0.0310(3) Uani d . 1 1 F F04 1.40992(16) 0.88795(8) 0.83312(13) 0.0314(4) Uani d . 1 1 F F05 1.19481(17) 0.93988(8) 0.66336(12) 0.0290(3) Uani d . 1 1 F F06 1.23862(18) 0.80502(8) 0.84223(12) 0.0341(4) Uani d . 1 1 P P01 1.21785(7) 0.87267(3) 0.75263(5) 0.01576(13) Uani d . 1 1 S S1 0.17453(7) 1.09853(3) -0.02174(5) 0.01822(12) Uani d . 1 1 Pd Pd1 0.491474(19) 0.891091(10) 0.260022(14) 0.01196(6) Uani d . 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0164(11) 0.0137(11) 0.0176(11) 0.0052(8) 0.0096(9) 0.0095(9) C2 0.0131(10) 0.0158(11) 0.0109(10) 0.0037(8) 0.0044(9) 0.0051(8) C3 0.0120(10) 0.0193(11) 0.0121(10) 0.0002(8) 0.0046(9) 0.0008(8) C4 0.0124(10) 0.0185(12) 0.0152(11) -0.0011(8) 0.0079(9) 0.0009(8) C5 0.0172(11) 0.0177(12) 0.0113(10) 0.0023(8) 0.0095(9) 0.0033(8) C6 0.0163(11) 0.0194(12) 0.0112(10) 0.0020(9) 0.0074(9) 0.0012(8) C7 0.0189(11) 0.0168(12) 0.0167(11) 0.0005(9) 0.0081(10) -0.0034(9) C8 0.0155(11) 0.0137(11) 0.0212(12) 0.0004(8) 0.0095(10) 0.0016(9) C9 0.0119(10) 0.0145(11) 0.0143(11) -0.0035(8) 0.0059(9) -0.0021(8) C10 0.0139(11) 0.0150(11) 0.0171(11) -0.0001(8) 0.0089(9) -0.0010(9) C11 0.0113(10) 0.0113(10) 0.0136(10) -0.0036(8) 0.0052(9) -0.0033(8) C12 0.0144(11) 0.0165(11) 0.0169(11) 0.0006(9) 0.0085(9) 0.0010(9) C13 0.0135(10) 0.0132(11) 0.0143(11) -0.0008(8) 0.0071(9) -0.0018(8) C14 0.0150(11) 0.0167(11) 0.0190(11) -0.0002(9) 0.0104(10) 0.0007(9) C15 0.0148(11) 0.0146(11) 0.0250(12) 0.0023(9) 0.0091(10) 0.0025(9) C16 0.0193(11) 0.0145(11) 0.0191(11) 0.0023(9) 0.0071(10) 0.0058(9) O1 0.0172(8) 0.0182(8) 0.0161(8) 0.0037(6) 0.0113(7) 0.0038(6) O2 0.0141(7) 0.0157(8) 0.0133(8) 0.0029(6) 0.0071(6) 0.0025(6) F01 0.0352(8) 0.0211(7) 0.0279(7) -0.0045(6) 0.0247(7) -0.0080(6) F1 0.0215(7) 0.0232(7) 0.0250(7) -0.0026(5) 0.0153(6) 0.0043(6) F02 0.0178(7) 0.0320(8) 0.0237(8) -0.0021(6) 0.0081(6) -0.0021(6) F2 0.0335(8) 0.0267(8) 0.0263(8) 0.0127(6) 0.0230(7) 0.0069(6) F3 0.0191(7) 0.0370(8) 0.0142(7) -0.0023(6) 0.0075(6) 0.0004(6) F03 0.0303(8) 0.0305(8) 0.0322(8) -0.0036(6) 0.0177(7) -0.0173(6) F04 0.0157(7) 0.0335(8) 0.0351(9) -0.0037(6) 0.0085(7) -0.0152(7) F05 0.0431(9) 0.0259(8) 0.0241(8) -0.0032(7) 0.0227(7) 0.0025(6) F06 0.0466(9) 0.0201(8) 0.0202(7) -0.0043(6) 0.0095(7) 0.0055(6) P01 0.0157(3) 0.0164(3) 0.0129(3) -0.0001(2) 0.0068(2) -0.0024(2) S1 0.0198(3) 0.0199(3) 0.0161(3) 0.0051(2) 0.0109(2) 0.0048(2) Pd1 0.01125(9) 0.01228(9) 0.01165(9) 0.00155(6) 0.00606(7) 0.00168(6) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' S S 0.1246 0.1234 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C8 125.2(2) C2 C1 Pd1 71.11(12) C8 C1 Pd1 111.36(14) C2 C1 H1 113.8 C8 C1 H1 113.8 Pd1 C1 H1 113.8 C1 C2 C3 126.7(2) C1 C2 Pd1 71.87(12) C3 C2 Pd1 106.50(13) C1 C2 H2 114.2 C3 C2 H2 114.2 Pd1 C2 H2 114.2 C2 C3 C4 114.04(18) C2 C3 H3A 108.7 C4 C3 H3A 108.7 C2 C3 H3B 108.7 C4 C3 H3B 108.7 H3A C3 H3B 107.6 C5 C4 C3 112.30(18) C5 C4 H4A 109.1 C3 C4 H4A 109.1 C5 C4 H4B 109.1 C3 C4 H4B 109.1 H4A C4 H4B 107.9 C6 C5 C4 124.47(19) C6 C5 Pd1 71.10(13) C4 C5 Pd1 110.79(14) C6 C5 H5 114.2 C4 C5 H5 114.2 Pd1 C5 H5 114.2 C5 C6 C7 126.5(2) C5 C6 Pd1 72.06(13) C7 C6 Pd1 107.17(15) C5 C6 H6 114.1 C7 C6 H6 114.1 Pd1 C6 H6 114.1 C6 C7 C8 114.01(18) C6 C7 H7A 108.8 C8 C7 H7A 108.8 C6 C7 H7B 108.8 C8 C7 H7B 108.8 H7A C7 H7B 107.6 C1 C8 C7 112.71(18) C1 C8 H8A 109 C7 C8 H8A 109 C1 C8 H8B 109 C7 C8 H8B 109 H8A C8 H8B 107.8 O1 C9 C10 129.8(2) O1 C9 C12 111.06(18) C10 C9 C12 119.11(19) C9 C10 C11 124.8(2) C9 C10 H10 117.6 C11 C10 H10 117.6 O2 C11 C10 125.48(19) O2 C11 C13 115.83(19) C10 C11 C13 118.69(19) F2 C12 F3 107.53(18) F2 C12 F1 107.07(17) F3 C12 F1 107.12(17) F2 C12 C9 113.06(18) F3 C12 C9 111.53(17) F1 C12 C9 110.24(18) C14 C13 C11 128.8(2) C14 C13 S1 111.55(16) C11 C13 S1 119.70(16) C13 C14 C15 111.8(2) C13 C14 H14 124.1 C15 C14 H14 124.1 C16 C15 C14 112.7(2) C16 C15 H15 123.7 C14 C15 H15 123.7 C15 C16 S1 112.71(17) C15 C16 H16 123.6 S1 C16 H16 123.6 C9 O1 Pd1 121.52(14) C11 O2 Pd1 124.93(14) F05 P01 F03 90.35(8) F05 P01 F04 90.40(8) F03 P01 F04 90.13(8) F05 P01 F02 90.28(8) F03 P01 F02 90.36(8) F04 P01 F02 179.16(9) F05 P01 F01 89.84(8) F03 P01 F01 179.61(9) F04 P01 F01 89.52(8) F02 P01 F01 89.99(8) F05 P01 F06 179.22(9) F03 P01 F06 90.00(8) F04 P01 F06 90.30(8) F02 P01 F06 89.02(8) F01 P01 F06 89.82(8) C16 S1 C13 91.23(11) O1 Pd1 O2 93.43(6) O1 Pd1 C2 88.22(7) O2 Pd1 C2 158.96(7) O1 Pd1 C6 159.28(7) O2 Pd1 C6 87.96(7) C2 Pd1 C6 97.84(8) O1 Pd1 C1 91.35(7) O2 Pd1 C1 163.40(7) C2 Pd1 C1 37.02(8) C6 Pd1 C1 82.04(8) O1 Pd1 C5 163.42(7) O2 Pd1 C5 90.84(7) C2 Pd1 C5 82.16(8) C6 Pd1 C5 36.84(8) C1 Pd1 C5 89.06(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.384(3) C1 C8 1.516(3) C1 Pd1 2.184(2) C1 H1 1 C2 C3 1.509(3) C2 Pd1 2.174(2) C2 H2 1 C3 C4 1.533(3) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.519(3) C4 H4A 0.99 C4 H4B 0.99 C5 C6 1.383(3) C5 Pd1 2.194(2) C5 H5 1 C6 C7 1.504(3) C6 Pd1 2.182(2) C6 H6 1 C7 C8 1.542(3) C7 H7A 0.99 C7 H7B 0.99 C8 H8A 0.99 C8 H8B 0.99 C9 O1 1.292(2) C9 C10 1.370(3) C9 C12 1.515(3) C10 C11 1.427(3) C10 H10 0.95 C11 O2 1.269(2) C11 C13 1.453(3) C12 F2 1.335(2) C12 F3 1.338(2) C12 F1 1.339(2) C13 C14 1.390(3) C13 S1 1.724(2) C14 C15 1.407(3) C14 H14 0.95 C15 C16 1.365(3) C15 H15 0.95 C16 S1 1.705(2) C16 H16 0.95 O1 Pd1 2.0061(15) O2 Pd1 2.0114(14) F01 P01 1.6051(14) F02 P01 1.6027(14) F03 P01 1.5984(14) F04 P01 1.6006(14) F05 P01 1.5905(14) F06 P01 1.6055(14) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C10 H10 F2 . 0.95 2.33 2.712(3) 103.6 C14 H14 F01 3_676 0.95 2.32 3.193(3) 152.3 C5 H5 F01 3_776 1 2.47 3.274(3) 137 C6 H6 F06 1_454 1 2.48 3.175(3) 126 C15 H15 F03 2_655 0.95 2.33 3.022(3) 128.9 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C8 C1 C2 C3 5.9(3) Pd1 C1 C2 C3 -97.4(2) C8 C1 C2 Pd1 103.3(2) C1 C2 C3 C4 38.1(3) Pd1 C2 C3 C4 -41.3(2) C2 C3 C4 C5 37.9(3) C3 C4 C5 C6 -95.0(2) C3 C4 C5 Pd1 -14.2(2) C4 C5 C6 C7 4.3(4) Pd1 C5 C6 C7 -98.4(2) C4 C5 C6 Pd1 102.7(2) C5 C6 C7 C8 40.9(3) Pd1 C6 C7 C8 -39.2(2) C2 C1 C8 C7 -93.7(2) Pd1 C1 C8 C7 -12.3(2) C6 C7 C8 C1 35.2(3) O1 C9 C10 C11 0.0(4) C12 C9 C10 C11 -179.17(19) C9 C10 C11 O2 0.9(3) C9 C10 C11 C13 -178.8(2) O1 C9 C12 F2 170.96(17) C10 C9 C12 F2 -9.7(3) O1 C9 C12 F3 49.6(2) C10 C9 C12 F3 -131.0(2) O1 C9 C12 F1 -69.2(2) C10 C9 C12 F1 110.1(2) O2 C11 C13 C14 174.8(2) C10 C11 C13 C14 -5.5(3) O2 C11 C13 S1 -4.8(3) C10 C11 C13 S1 175.00(15) C11 C13 C14 C15 -179.7(2) S1 C13 C14 C15 -0.1(2) C13 C14 C15 C16 0.1(3) C14 C15 C16 S1 0.0(3) C10 C9 O1 Pd1 -2.1(3) C12 C9 O1 Pd1 177.19(12) C10 C11 O2 Pd1 0.5(3) C13 C11 O2 Pd1 -179.79(13) C15 C16 S1 C13 -0.07(18) C14 C13 S1 C16 0.12(17) C11 C13 S1 C16 179.72(17) C9 O1 Pd1 O2 2.45(16) C9 O1 Pd1 C2 161.45(16) C9 O1 Pd1 C6 -90.9(2) C9 O1 Pd1 C1 -161.65(16) C9 O1 Pd1 C5 107.1(3) C11 O2 Pd1 O1 -1.77(16) C11 O2 Pd1 C2 -95.7(2) C11 O2 Pd1 C6 157.53(17) C11 O2 Pd1 C1 104.7(3) C11 O2 Pd1 C5 -165.74(16) C1 C2 Pd1 O1 94.61(13) C3 C2 Pd1 O1 -141.46(15) C1 C2 Pd1 O2 -170.45(17) C3 C2 Pd1 O2 -46.5(3) C1 C2 Pd1 C6 -65.49(14) C3 C2 Pd1 C6 58.44(15) C3 C2 Pd1 C1 123.9(2) C1 C2 Pd1 C5 -98.93(14) C3 C2 Pd1 C5 25.00(15) C5 C6 Pd1 O1 -171.57(17) C7 C6 Pd1 O1 -47.9(3) C5 C6 Pd1 O2 94.12(13) C7 C6 Pd1 O2 -142.21(15) C5 C6 Pd1 C2 -65.58(13) C7 C6 Pd1 C2 58.09(15) C5 C6 Pd1 C1 -99.16(13) C7 C6 Pd1 C1 24.51(14) C7 C6 Pd1 C5 123.7(2) C2 C1 Pd1 O1 -85.24(13) C8 C1 Pd1 O1 153.45(15) C2 C1 Pd1 O2 168.0(2) C8 C1 Pd1 O2 46.7(3) C8 C1 Pd1 C2 -121.3(2) C2 C1 Pd1 C6 114.47(14) C8 C1 Pd1 C6 -6.83(15) C2 C1 Pd1 C5 78.18(13) C8 C1 Pd1 C5 -43.13(15) C6 C5 Pd1 O1 169.5(2) C4 C5 Pd1 O1 48.9(3) C6 C5 Pd1 O2 -85.48(13) C4 C5 Pd1 O2 153.86(14) C6 C5 Pd1 C2 114.42(14) C4 C5 Pd1 C2 -6.23(14) C4 C5 Pd1 C6 -120.7(2) C6 C5 Pd1 C1 77.92(13) C4 C5 Pd1 C1 -42.74(15)