#------------------------------------------------------------------------------ #$Date: 2013-03-09 16:05:21 +0000 (Sat, 09 Mar 2013) $ #$Revision: 75301 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105309.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_2105309 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_volume 69 _journal_year 2013 _chemical_formula_moiety 'C13 H19 O2 Pd, F6 P' _chemical_formula_structural '(Pd (C8 H12) (O2 C5 H7)) (P F6)' _chemical_formula_sum 'C13 H19 F6 O2 P Pd' _chemical_formula_weight 458.65 _chemical_name_systematic ; (acetylacetonato)(\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 119.016(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.3166(6) _cell_length_b 15.4676(8) _cell_length_c 12.6132(6) _cell_measurement_reflns_used 4688 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.27 _cell_measurement_theta_min 3.22 _cell_volume 1589.49(16) _computing_cell_refinement 'Bruker SAINT-Plus (Bruker, 2004)' _computing_data_collection 'Bruker APEX2 (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT-Plus and XPREP (Bruker, 2004)' _computing_molecular_graphics 'DIAMOND 3.0c (Brandenburg & Putz, 2005)' _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 512 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker X8 Apex II 4K Kappa CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10747 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 3.31 _exptl_absorpt_coefficient_mu 1.335 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_correction_T_min 0.8456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Cuboid _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.696 _refine_diff_density_min -0.672 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 3952 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0332 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.1476P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.0806 _reflns_number_gt 3112 _reflns_number_total 3952 _reflns_threshold_expression >2\s(I) _journal_paper_doi 10.1107/S0108768112046733 _iucr_refine_instructions_details ; TITL 8fth3_0m in P2(1)/c CELL 0.71073 9.3166 15.4676 12.6132 90.000 119.016 90.000 ZERR 4.00 0.0006 0.0008 0.0006 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O F P PD UNIT 52 76 8 24 4 4 MERG 2 OMIT -4.00 180.00 OMIT 1 0 0 OMIT 0 2 1 OMIT -1 1 1 OMIT 1 1 0 OMIT 0 2 0 OMIT 0 1 1 EQIV $1 x+1, y, z EQIV $2 -x+1, -y, -z EQIV $3 -x+1, y+0.5, -z+0.5 EQIV $4 -x+2, y+0.5, -z+0.5 EQIV $5 -x+2, -y, -z+1 HTAB C10 F6 HTAB C7 F4_$1 HTAB C2 F6_$2 HTAB C2 F3_$2 HTAB C5 F3_$3 HTAB C8 F1_$4 HTAB C6 F1_$5 FMAP 2 PLAN 10 SIZE 0.03 0.07 0.13 ACTA BOND $H CONF LIST 4 L.S. 16 TEMP -173.20 WGHT 0.034500 0.147600 FVAR 0.09582 C1 1 1.138943 0.082176 0.134774 11.00000 0.02454 0.01946 = 0.01719 -0.00430 0.01610 -0.00052 AFIX 13 H1 2 1.135311 0.023652 0.099865 11.00000 -1.20000 AFIX 0 C2 1 1.002705 0.131995 0.065769 11.00000 0.02466 0.02260 = 0.01283 -0.00194 0.01334 -0.00293 AFIX 13 H2 2 0.919244 0.103234 -0.010344 11.00000 -1.20000 AFIX 0 C3 1 0.993028 0.229430 0.062063 11.00000 0.02497 0.02153 = 0.01440 0.00204 0.01079 -0.00198 AFIX 23 H3A 2 0.877045 0.246910 0.029920 11.00000 -1.20000 H3B 2 1.029786 0.250989 0.005247 11.00000 -1.20000 AFIX 0 C4 1 1.096570 0.272349 0.185582 11.00000 0.02148 0.01420 = 0.02320 -0.00089 0.01369 -0.00213 AFIX 23 H4A 2 1.211426 0.277137 0.201792 11.00000 -1.20000 H4B 2 1.054871 0.331574 0.183304 11.00000 -1.20000 AFIX 0 C5 1 1.093464 0.222374 0.287870 11.00000 0.02019 0.01095 = 0.01304 -0.00441 0.00820 -0.00491 AFIX 13 H5 2 1.043074 0.254682 0.330286 11.00000 -1.20000 AFIX 0 C6 1 1.209418 0.162166 0.359562 11.00000 0.01613 0.01714 = 0.01221 -0.00459 0.00678 -0.00349 AFIX 13 H6 2 1.228007 0.159036 0.444496 11.00000 -1.20000 AFIX 0 C7 1 1.351948 0.131703 0.345538 11.00000 0.01285 0.02299 = 0.02053 -0.00120 0.00607 -0.00035 AFIX 23 H7A 2 1.393596 0.077002 0.391074 11.00000 -1.20000 H7B 2 1.441038 0.175041 0.382415 11.00000 -1.20000 AFIX 0 C8 1 1.311450 0.116676 0.213435 11.00000 0.01664 0.02068 = 0.02747 -0.00430 0.01401 -0.00038 AFIX 23 H8A 2 1.323562 0.171906 0.178888 11.00000 -1.20000 H8B 2 1.391276 0.075086 0.212025 11.00000 -1.20000 AFIX 0 C9 1 0.732346 -0.035201 0.149567 11.00000 0.01473 0.01097 = 0.02163 0.00246 0.00525 0.00434 C10 1 0.709721 -0.016536 0.248804 11.00000 0.01318 0.01447 = 0.02277 0.00374 0.00955 -0.00161 AFIX 43 H10 2 0.622818 -0.045955 0.252602 11.00000 -1.20000 AFIX 0 C11 1 0.801736 0.040913 0.342941 11.00000 0.01234 0.01026 = 0.01630 0.00464 0.00704 0.00476 C12 1 0.624649 -0.101342 0.058027 11.00000 0.02452 0.01887 = 0.02402 -0.00306 0.01196 -0.00162 AFIX 137 H12A 2 0.557942 -0.073166 -0.020519 11.00000 -1.50000 H12B 2 0.552519 -0.127977 0.085092 11.00000 -1.50000 H12C 2 0.693322 -0.145976 0.049870 11.00000 -1.50000 AFIX 0 C13 1 0.762602 0.051451 0.444647 11.00000 0.01422 0.02194 = 0.02302 0.00125 0.01068 0.00108 AFIX 137 H13A 2 0.861126 0.039695 0.522124 11.00000 -1.50000 H13B 2 0.675676 0.010798 0.433473 11.00000 -1.50000 H13C 2 0.725487 0.110732 0.444662 11.00000 -1.50000 AFIX 0 O1 3 0.840053 -0.001496 0.126108 11.00000 0.01540 0.01728 = 0.01857 -0.00515 0.00873 -0.00517 O2 3 0.922343 0.087195 0.354323 11.00000 0.01220 0.01855 = 0.01448 -0.00113 0.00695 -0.00118 F1 4 0.546633 -0.194095 0.353758 11.00000 0.02066 0.04482 = 0.03982 -0.00684 0.00956 0.00272 F2 4 0.306262 -0.256540 0.217128 11.00000 0.04465 0.03651 = 0.03980 -0.02345 0.01276 -0.01385 F3 4 0.166566 -0.141298 0.228560 11.00000 0.02001 0.04313 = 0.04841 0.01397 0.01489 -0.00053 F4 4 0.406174 -0.080442 0.366221 11.00000 0.04709 0.02320 = 0.03901 -0.00977 0.01951 -0.00864 F5 4 0.340636 -0.214431 0.398661 11.00000 0.04344 0.03918 = 0.02613 0.00727 0.01803 -0.01073 F6 4 0.368675 -0.121245 0.183417 11.00000 0.02892 0.06972 = 0.02289 0.00642 0.01137 -0.01873 P1 5 0.356166 -0.168839 0.291557 11.00000 0.01766 0.02157 = 0.01807 -0.00345 0.00792 -0.00642 PD1 6 0.991942 0.092702 0.227456 11.00000 0.01225 0.01267 = 0.01238 -0.00065 0.00634 -0.00086 HKLF 4 REM 8fth3_0m in P2(1)/c REM R1 = 0.0332 for 3112 Fo > 4sig(Fo) and 0.0467 for all 3952 data REM 210 parameters refined using 0 restraints END WGHT 0.0345 0.1476 REM Highest difference peak 0.696, deepest hole -0.672, 1-sigma level 0.121 Q1 1 1.0380 0.0901 0.3175 11.00000 0.05 0.70 Q2 1 1.2047 0.1229 0.4376 11.00000 0.05 0.55 Q3 1 0.9909 0.1775 0.0842 11.00000 0.05 0.54 Q4 1 0.7353 0.0346 0.2779 11.00000 0.05 0.54 Q5 1 0.9039 0.0947 0.1350 11.00000 0.05 0.53 Q6 1 1.3265 0.3370 0.2359 11.00000 0.05 0.53 Q7 1 1.0148 0.2275 0.2803 11.00000 0.05 0.50 Q8 1 1.0986 0.2417 0.2403 11.00000 0.05 0.50 Q9 1 1.0578 0.2410 0.1223 11.00000 0.05 0.50 Q10 1 0.9164 0.0889 0.3008 11.00000 0.05 0.48 ; _[local]_cod_data_source_file eb5019.cif _[local]_cod_data_source_block 8Fth3 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 1589.49(15) _cod_database_code 2105309 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 1.1389(4) 0.08218(19) 0.1348(3) 0.0179(7) Uani d . 1 1 H H1 1.1353 0.0237 0.0999 0.021 Uiso calc R 1 1 C C2 1.0027(4) 0.1320(2) 0.0658(3) 0.0182(7) Uani d . 1 1 H H2 0.9192 0.1032 -0.0103 0.022 Uiso calc R 1 1 C C3 0.9930(4) 0.22943(19) 0.0621(3) 0.0198(7) Uani d . 1 1 H H3A 0.877 0.2469 0.0299 0.024 Uiso calc R 1 1 H H3B 1.0298 0.251 0.0052 0.024 Uiso calc R 1 1 C C4 1.0966(4) 0.27235(19) 0.1856(3) 0.0184(7) Uani d . 1 1 H H4A 1.2114 0.2771 0.2018 0.022 Uiso calc R 1 1 H H4B 1.0549 0.3316 0.1833 0.022 Uiso calc R 1 1 C C5 1.0935(4) 0.22237(17) 0.2879(3) 0.0147(6) Uani d . 1 1 H H5 1.0431 0.2547 0.3303 0.018 Uiso calc R 1 1 C C6 1.2094(4) 0.16217(18) 0.3596(3) 0.0152(6) Uani d . 1 1 H H6 1.228 0.159 0.4445 0.018 Uiso calc R 1 1 C C7 1.3519(4) 0.1317(2) 0.3455(3) 0.0197(7) Uani d . 1 1 H H7A 1.3936 0.077 0.3911 0.024 Uiso calc R 1 1 H H7B 1.441 0.175 0.3824 0.024 Uiso calc R 1 1 C C8 1.3114(4) 0.1167(2) 0.2134(3) 0.0202(7) Uani d . 1 1 H H8A 1.3236 0.1719 0.1789 0.024 Uiso calc R 1 1 H H8B 1.3913 0.0751 0.212 0.024 Uiso calc R 1 1 C C9 0.7323(4) -0.03520(18) 0.1496(3) 0.0173(7) Uani d . 1 1 C C10 0.7097(4) -0.01654(18) 0.2488(3) 0.0165(6) Uani d . 1 1 H H10 0.6228 -0.046 0.2526 0.02 Uiso calc R 1 1 C C11 0.8017(4) 0.04091(17) 0.3429(3) 0.0129(6) Uani d . 1 1 C C12 0.6246(4) -0.10134(19) 0.0580(3) 0.0224(7) Uani d . 1 1 H H12A 0.5579 -0.0732 -0.0205 0.034 Uiso calc R 1 1 H H12B 0.5525 -0.128 0.0851 0.034 Uiso calc R 1 1 H H12C 0.6933 -0.146 0.0499 0.034 Uiso calc R 1 1 C C13 0.7626(4) 0.0515(2) 0.4446(3) 0.0190(7) Uani d . 1 1 H H13A 0.8611 0.0397 0.5221 0.029 Uiso calc R 1 1 H H13B 0.6757 0.0108 0.4335 0.029 Uiso calc R 1 1 H H13C 0.7255 0.1107 0.4447 0.029 Uiso calc R 1 1 O O1 0.8401(3) -0.00150(12) 0.12611(18) 0.0169(5) Uani d . 1 1 O O2 0.9223(3) 0.08719(12) 0.35432(18) 0.0149(4) Uani d . 1 1 F F1 0.5466(3) -0.19410(13) 0.35376(18) 0.0373(5) Uani d . 1 1 F F2 0.3063(3) -0.25654(13) 0.2171(2) 0.0436(6) Uani d . 1 1 F F3 0.1666(3) -0.14130(13) 0.22856(19) 0.0379(5) Uani d . 1 1 F F4 0.4062(3) -0.08044(11) 0.3662(2) 0.0370(6) Uani d . 1 1 F F5 0.3406(3) -0.21443(13) 0.39866(17) 0.0358(5) Uani d . 1 1 F F6 0.3687(3) -0.12125(15) 0.18342(18) 0.0410(6) Uani d . 1 1 P P1 0.35617(11) -0.16884(5) 0.29156(7) 0.01942(19) Uani d . 1 1 Pd Pd1 0.99194(3) 0.092702(13) 0.22746(2) 0.01228(8) 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 0.0245(19) 0.0195(15) 0.0172(16) -0.0005(13) 0.0161(14) -0.0043(12) C2 0.0247(19) 0.0226(16) 0.0128(15) -0.0029(14) 0.0133(14) -0.0019(12) C3 0.0250(19) 0.0215(16) 0.0144(15) -0.0020(14) 0.0108(14) 0.0020(12) C4 0.0215(18) 0.0142(14) 0.0232(16) -0.0021(13) 0.0137(15) -0.0009(12) C5 0.0202(18) 0.0109(13) 0.0130(14) -0.0049(12) 0.0082(13) -0.0044(11) C6 0.0161(17) 0.0171(15) 0.0122(14) -0.0035(12) 0.0068(13) -0.0046(11) C7 0.0128(17) 0.0230(16) 0.0205(16) -0.0004(13) 0.0061(14) -0.0012(13) C8 0.0166(17) 0.0207(15) 0.0275(18) -0.0004(13) 0.0140(15) -0.0043(13) C9 0.0147(17) 0.0110(14) 0.0216(16) 0.0043(12) 0.0053(14) 0.0025(12) C10 0.0132(16) 0.0145(14) 0.0228(16) -0.0016(12) 0.0095(13) 0.0037(12) C11 0.0123(16) 0.0103(13) 0.0163(15) 0.0048(11) 0.0070(13) 0.0046(11) C12 0.0245(19) 0.0189(16) 0.0240(18) -0.0016(14) 0.0120(15) -0.0031(12) C13 0.0142(17) 0.0219(16) 0.0230(17) 0.0011(13) 0.0107(14) 0.0012(13) O1 0.0154(12) 0.0173(10) 0.0186(11) -0.0052(9) 0.0087(9) -0.0051(8) O2 0.0122(11) 0.0185(10) 0.0145(11) -0.0012(9) 0.0070(9) -0.0011(8) F1 0.0207(12) 0.0448(13) 0.0398(13) 0.0027(10) 0.0096(10) -0.0068(10) F2 0.0447(16) 0.0365(12) 0.0398(13) -0.0138(11) 0.0128(12) -0.0234(10) F3 0.0200(12) 0.0431(12) 0.0484(14) -0.0005(10) 0.0149(11) 0.0140(10) F4 0.0471(16) 0.0232(10) 0.0390(13) -0.0086(10) 0.0195(12) -0.0098(9) F5 0.0434(15) 0.0392(12) 0.0261(11) -0.0107(10) 0.0180(10) 0.0073(9) F6 0.0289(13) 0.0697(15) 0.0229(11) -0.0187(12) 0.0114(10) 0.0064(10) P1 0.0177(5) 0.0216(4) 0.0181(4) -0.0064(3) 0.0079(4) -0.0034(3) Pd1 0.01225(13) 0.01267(12) 0.01238(13) -0.00086(9) 0.00634(10) -0.00065(8) 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' 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(3) C2 C1 Pd1 70.90(18) C8 C1 Pd1 111.2(2) C2 C1 H1 113.9 C8 C1 H1 113.9 Pd1 C1 H1 113.9 C1 C2 C3 127.0(3) C1 C2 Pd1 72.44(18) C3 C2 Pd1 106.18(19) C1 C2 H2 114.1 C3 C2 H2 114.1 Pd1 C2 H2 114.1 C2 C3 C4 113.8(3) C2 C3 H3A 108.8 C4 C3 H3A 108.8 C2 C3 H3B 108.8 C4 C3 H3B 108.8 H3A C3 H3B 107.7 C5 C4 C3 112.5(2) C5 C4 H4A 109.1 C3 C4 H4A 109.1 C5 C4 H4B 109.1 C3 C4 H4B 109.1 H4A C4 H4B 107.8 C6 C5 C4 124.7(3) C6 C5 Pd1 71.26(16) C4 C5 Pd1 110.73(18) C6 C5 H5 114.1 C4 C5 H5 114.1 Pd1 C5 H5 114.1 C5 C6 C7 126.3(3) C5 C6 Pd1 71.95(17) C7 C6 Pd1 107.63(19) C5 C6 H6 114.1 C7 C6 H6 114.1 Pd1 C6 H6 114.1 C6 C7 C8 114.2(3) C6 C7 H7A 108.7 C8 C7 H7A 108.7 C6 C7 H7B 108.7 C8 C7 H7B 108.7 H7A C7 H7B 107.6 C1 C8 C7 112.8(3) C1 C8 H8A 109 C7 C8 H8A 109 C1 C8 H8B 109 C7 C8 H8B 109 H8A C8 H8B 107.8 O1 C9 C10 126.6(3) O1 C9 C12 113.8(3) C10 C9 C12 119.6(3) C11 C10 C9 126.6(3) C11 C10 H10 116.7 C9 C10 H10 116.7 O2 C11 C10 126.5(3) O2 C11 C13 114.0(3) C10 C11 C13 119.5(3) C9 C12 H12A 109.5 C9 C12 H12B 109.5 H12A C12 H12B 109.5 C9 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C11 C13 H13A 109.5 C11 C13 H13B 109.5 H13A C13 H13B 109.5 C11 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C9 O1 Pd1 122.48(19) C11 O2 Pd1 122.82(18) F2 P1 F5 90.13(12) F2 P1 F4 179.88(17) F5 P1 F4 89.97(12) F2 P1 F1 91.05(12) F5 P1 F1 90.65(12) F4 P1 F1 89.02(12) F2 P1 F6 90.61(13) F5 P1 F6 178.64(14) F4 P1 F6 89.30(12) F1 P1 F6 90.47(13) F2 P1 F3 89.87(13) F5 P1 F3 90.37(12) F4 P1 F3 90.05(12) F1 P1 F3 178.62(12) F6 P1 F3 88.49(12) O2 Pd1 O1 94.41(8) O2 Pd1 C2 160.46(10) O1 Pd1 C2 86.82(10) O2 Pd1 C6 87.21(10) O1 Pd1 C6 162.43(10) C2 Pd1 C6 97.49(12) O2 Pd1 C5 90.78(10) O1 Pd1 C5 160.23(10) C2 Pd1 C5 82.06(11) C6 Pd1 C5 36.79(11) O2 Pd1 C1 162.06(10) O1 Pd1 C1 92.08(10) C2 Pd1 C1 36.66(12) C6 Pd1 C1 81.67(12) C5 Pd1 C1 88.71(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.375(5) C1 C8 1.518(5) C1 Pd1 2.196(3) C1 H1 1 C2 C3 1.509(4) C2 Pd1 2.176(3) C2 H2 1 C3 C4 1.530(4) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.516(4) C4 H4A 0.99 C4 H4B 0.99 C5 C6 1.380(4) C5 Pd1 2.191(3) C5 H5 1 C6 C7 1.498(4) C6 Pd1 2.182(3) C6 H6 1 C7 C8 1.537(4) C7 H7A 0.99 C7 H7B 0.99 C8 H8A 0.99 C8 H8B 0.99 C9 O1 1.286(4) C9 C10 1.397(4) C9 C12 1.504(4) C10 C11 1.395(4) C10 H10 0.95 C11 O2 1.280(3) C11 C13 1.503(4) C12 H12A 0.98 C12 H12B 0.98 C12 H12C 0.98 C13 H13A 0.98 C13 H13B 0.98 C13 H13C 0.98 O1 Pd1 2.0012(19) O2 Pd1 1.999(2) F1 P1 1.602(2) F2 P1 1.586(2) F3 P1 1.604(2) F4 P1 1.5962(19) F5 P1 1.591(2) F6 P1 1.603(2) 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 F6 . 0.95 2.39 3.295(4) 158.7 C7 H7A F4 1_655 0.99 2.47 3.311(4) 143.1 C2 H2 F6 3_655 1 2.52 3.366(4) 141.9 C2 H2 F3 3_655 1 2.54 3.257(4) 128.9 C5 H5 F3 2_655 1 2.36 3.142(4) 134.9 C8 H8A F1 2_755 0.99 2.53 3.481(4) 160.6 C6 H6 F1 3_756 1 2.45 3.242(3) 135.9 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 -5.7(5) Pd1 C1 C2 C3 97.3(3) C8 C1 C2 Pd1 -103.0(3) C1 C2 C3 C4 -37.9(4) Pd1 C2 C3 C4 42.1(3) C2 C3 C4 C5 -38.2(4) C3 C4 C5 C6 94.8(4) C3 C4 C5 Pd1 13.7(3) C4 C5 C6 C7 -3.7(5) Pd1 C5 C6 C7 99.0(3) C4 C5 C6 Pd1 -102.7(3) C5 C6 C7 C8 -41.2(4) Pd1 C6 C7 C8 39.0(3) C2 C1 C8 C7 93.4(4) Pd1 C1 C8 C7 12.3(3) C6 C7 C8 C1 -35.0(4) O1 C9 C10 C11 -1.4(5) C12 C9 C10 C11 178.0(3) C9 C10 C11 O2 0.6(5) C9 C10 C11 C13 -178.5(3) C10 C9 O1 Pd1 -3.8(4) C12 C9 O1 Pd1 176.70(19) C10 C11 O2 Pd1 5.2(4) C13 C11 O2 Pd1 -175.62(18) C11 O2 Pd1 O1 -7.6(2) C11 O2 Pd1 C2 85.3(4) C11 O2 Pd1 C6 -170.0(2) C11 O2 Pd1 C5 153.3(2) C11 O2 Pd1 C1 -118.4(3) C9 O1 Pd1 O2 6.9(2) C9 O1 Pd1 C2 -153.6(2) C9 O1 Pd1 C6 101.6(4) C9 O1 Pd1 C5 -97.9(3) C9 O1 Pd1 C1 170.1(2) C1 C2 Pd1 O2 168.0(2) C3 C2 Pd1 O2 43.5(4) C1 C2 Pd1 O1 -97.80(19) C3 C2 Pd1 O1 137.7(2) C1 C2 Pd1 C6 65.08(19) C3 C2 Pd1 C6 -59.4(2) C1 C2 Pd1 C5 98.6(2) C3 C2 Pd1 C5 -25.9(2) C3 C2 Pd1 C1 -124.5(3) C5 C6 Pd1 O2 -95.04(18) C7 C6 Pd1 O2 141.6(2) C5 C6 Pd1 O1 169.2(3) C7 C6 Pd1 O1 45.8(4) C5 C6 Pd1 C2 65.90(19) C7 C6 Pd1 C2 -57.4(2) C7 C6 Pd1 C5 -123.3(3) C5 C6 Pd1 C1 99.08(19) C7 C6 Pd1 C1 -24.3(2) C6 C5 Pd1 O2 84.29(18) C4 C5 Pd1 O2 -154.7(2) C6 C5 Pd1 O1 -170.3(2) C4 C5 Pd1 O1 -49.4(4) C6 C5 Pd1 C2 -114.0(2) C4 C5 Pd1 C2 7.0(2) C4 C5 Pd1 C6 121.0(3) C6 C5 Pd1 C1 -77.77(19) C4 C5 Pd1 C1 43.2(2) C2 C1 Pd1 O2 -166.9(3) C8 C1 Pd1 O2 -45.6(4) C2 C1 Pd1 O1 81.84(19) C8 C1 Pd1 O1 -156.8(2) C8 C1 Pd1 C2 121.3(3) C2 C1 Pd1 C6 -114.66(19) C8 C1 Pd1 C6 6.6(2) C2 C1 Pd1 C5 -78.40(19) C8 C1 Pd1 C5 42.9(2)