#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105312.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_2105312 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, B F4' _chemical_formula_structural '(Pd (C8 H12) (O2 S F3 C8 H7)) (B F4)' _chemical_formula_sum 'C16 H16 B F7 O2 Pd S' _chemical_formula_weight 522.56 _chemical_name_systematic ; (thenoyltrifluoroacetonato)(\h^4^-cyclo-octa-1,5-dienyl)palladium(II) tetrafluoroborate ; _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 125.684(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0528(3) _cell_length_b 16.6333(6) _cell_length_c 13.1600(3) _cell_measurement_reflns_used 8114 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.38 _cell_measurement_theta_min 2.78 _cell_volume 1787.35(10) _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 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker 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 0.0327 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 21884 _diffrn_reflns_theta_full 28.41 _diffrn_reflns_theta_max 28.41 _diffrn_reflns_theta_min 3.11 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_T_max 0.8761 _exptl_absorpt_correction_T_min 0.7237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cuboid _exptl_crystal_F_000 1032 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.611 _refine_diff_density_min -0.729 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 4464 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0269 _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^)+(0.0339P)^2^+1.0448P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.0707 _reflns_number_gt 3873 _reflns_number_total 4464 _reflns_threshold_expression >2\s(I) _iucr_refine_instructions_details ; TITL 10RTH7_0ma in P2(1)/c CELL 0.71073 10.0528 16.6333 13.1600 90.000 125.684 90.000 ZERR 4.00 0.0003 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B O F S PD UNIT 64 64 4 8 28 4 4 MERG 2 OMIT -4.00 180.00 OMIT 1 0 0 OMIT 0 2 0 OMIT -1 1 1 OMIT 1 1 0 OMIT 0 1 1 EQIV $1 -x+1, -y+1, -z+2 EQIV $2 x+1, y, z EQIV $3 -x, -y+1, -z+1 EQIV $4 x, -y+1.5, z-0.5 HTAB C10 F01 HTAB C10 F3 HTAB C14 F01 HTAB C14 F04 HTAB C2 F01_$1 HTAB C3 F03_$1 HTAB C5 F04_$2 HTAB C6 F04_$3 HTAB C16 F01_$4 HTAB C16 F02_$4 FMAP 2 PLAN 10 SIZE 0.11 0.16 0.28 ACTA BOND $H CONF LIST 4 L.S. 16 TEMP -173.20 WGHT 0.033900 1.044800 FVAR 0.10288 C1 1 0.569765 0.274864 0.828953 11.00000 0.01661 0.01135 = 0.01511 0.00497 0.00919 0.00385 AFIX 13 H1 2 0.528397 0.250029 0.874786 11.00000 -1.20000 AFIX 0 C2 1 0.699360 0.327193 0.900544 11.00000 0.01442 0.01603 = 0.01109 0.00447 0.00574 0.00425 AFIX 13 H2 2 0.733900 0.333597 0.988387 11.00000 -1.20000 AFIX 0 C3 1 0.835085 0.341967 0.884645 11.00000 0.01136 0.02201 = 0.01372 0.00196 0.00594 0.00174 AFIX 23 H3A 2 0.848435 0.293616 0.847512 11.00000 -1.20000 H3B 2 0.939285 0.350892 0.967845 11.00000 -1.20000 AFIX 0 C4 1 0.799792 0.414685 0.801051 11.00000 0.01261 0.02178 = 0.01566 -0.00054 0.00843 -0.00170 AFIX 23 H4A 2 0.832452 0.464099 0.852318 11.00000 -1.20000 H4B 2 0.868511 0.410776 0.769892 11.00000 -1.20000 AFIX 0 C5 1 0.623365 0.422586 0.690738 11.00000 0.01516 0.02216 = 0.01346 0.00584 0.01027 0.00302 AFIX 13 H5 2 0.595908 0.475061 0.645567 11.00000 -1.20000 AFIX 0 C6 1 0.516551 0.360484 0.619313 11.00000 0.01433 0.02289 = 0.00911 0.00318 0.00670 0.00263 AFIX 13 H6 2 0.425153 0.376852 0.532433 11.00000 -1.20000 AFIX 0 C7 1 0.562092 0.272241 0.631537 11.00000 0.02090 0.02125 = 0.01471 -0.00347 0.01027 0.00162 AFIX 23 H7A 2 0.678903 0.267715 0.664259 11.00000 -1.20000 H7B 2 0.496059 0.246983 0.547695 11.00000 -1.20000 AFIX 0 C8 1 0.533673 0.226481 0.719072 11.00000 0.01702 0.01671 = 0.01839 -0.00100 0.00837 0.00199 AFIX 23 H8A 2 0.418131 0.208551 0.670088 11.00000 -1.20000 H8B 2 0.603546 0.177840 0.750547 11.00000 -1.20000 AFIX 0 C9 1 0.295712 0.449794 0.854569 11.00000 0.01413 0.01303 = 0.01561 -0.00264 0.00963 -0.00335 C10 1 0.208260 0.506253 0.762567 11.00000 0.01363 0.01492 = 0.01663 0.00030 0.00927 0.00080 AFIX 43 H10 2 0.129101 0.537001 0.763190 11.00000 -1.20000 AFIX 0 C11 1 0.228854 0.521493 0.666632 11.00000 0.00993 0.01012 = 0.01353 -0.00065 0.00423 -0.00083 C12 1 0.261687 0.437971 0.952884 11.00000 0.01522 0.01429 = 0.01642 0.00012 0.01031 -0.00001 C13 1 0.129147 0.582178 0.571903 11.00000 0.01296 0.01343 = 0.01281 0.00028 0.00654 -0.00154 C14 1 -0.002125 0.627302 0.550919 11.00000 0.01378 0.01449 = 0.01707 0.00131 0.00614 -0.00126 AFIX 43 H14 2 -0.042648 0.624084 0.600408 11.00000 -1.20000 AFIX 0 C15 1 -0.066590 0.678462 0.445958 11.00000 0.01825 0.01477 = 0.02260 -0.00026 0.00793 0.00209 AFIX 43 H15 2 -0.157491 0.713131 0.415941 11.00000 -1.20000 AFIX 0 C16 1 0.015731 0.672744 0.392292 11.00000 0.02397 0.01435 = 0.01548 0.00179 0.00608 -0.00009 AFIX 43 H16 2 -0.010826 0.703585 0.321977 11.00000 -1.20000 AFIX 0 B01 3 -0.171222 0.636331 0.740701 11.00000 0.02077 0.01656 = 0.01591 -0.00104 0.01007 0.00168 O1 4 0.406835 0.400205 0.874540 11.00000 0.01563 0.01611 = 0.01582 0.00335 0.01089 0.00392 O2 4 0.331652 0.486095 0.654010 11.00000 0.01430 0.01552 = 0.01478 0.00252 0.00822 0.00227 F01 5 -0.002332 0.648103 0.804069 11.00000 0.01730 0.02673 = 0.02193 -0.00578 0.00768 0.00206 F1 5 0.400330 0.440901 1.068045 11.00000 0.01599 0.02678 = 0.01258 0.00006 0.00661 -0.00180 F2 5 0.193361 0.366219 0.938051 11.00000 0.02278 0.01976 = 0.02199 -0.00144 0.01575 -0.00537 F02 5 -0.253595 0.705393 0.673357 11.00000 0.02549 0.02098 = 0.02552 0.00188 0.00690 0.00570 F03 5 -0.205848 0.620183 0.826217 11.00000 0.03811 0.03929 = 0.02632 -0.00454 0.02424 -0.00360 F3 5 0.160812 0.493482 0.946213 11.00000 0.02399 0.02322 = 0.02291 0.00221 0.01730 0.00729 F04 5 -0.219042 0.571983 0.658626 11.00000 0.02895 0.01798 = 0.01829 -0.00374 0.01309 -0.00350 S1 6 0.170449 0.604566 0.464990 11.00000 0.02184 0.01815 = 0.01687 0.00356 0.01125 0.00321 PD1 7 0.479840 0.396026 0.761842 11.00000 0.01058 0.01181 = 0.01148 0.00158 0.00650 0.00138 HKLF 4 REM 10RTH7_0ma in P2(1)/c REM R1 = 0.0269 for 3873 Fo > 4sig(Fo) and 0.0324 for all 4464 data REM 253 parameters refined using 0 restraints END WGHT 0.0339 1.0448 REM Highest difference peak 0.611, deepest hole -0.729, 1-sigma level 0.108 Q1 1 0.2936 0.4497 0.9124 11.00000 0.05 0.61 Q2 1 0.3377 0.4267 1.0105 11.00000 0.05 0.49 Q3 1 0.1787 0.5554 0.6229 11.00000 0.05 0.46 Q4 1 0.0650 0.6292 0.4038 11.00000 0.05 0.46 Q5 1 0.0987 0.5662 0.3935 11.00000 0.05 0.45 Q6 1 0.1395 0.5973 0.5127 11.00000 0.05 0.43 Q7 1 0.2243 0.4012 0.9360 11.00000 0.05 0.43 Q8 1 0.4964 0.3979 0.7154 11.00000 0.05 0.42 Q9 1 0.5679 0.2531 0.7728 11.00000 0.05 0.42 Q10 1 0.2757 0.6064 0.4656 11.00000 0.05 0.41 ; _cod_data_source_file eb5019.cif _cod_data_source_block 10Rth7 _cod_original_cell_volume 1787.35(9) _cod_original_sg_symbol_Hall '-P 2ybc ' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2105312 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 0.5698(3) 0.27486(13) 0.8290(2) 0.0144(4) Uani d . 1 1 H H1 0.5284 0.25 0.8748 0.017 Uiso calc R 1 1 C C2 0.6994(3) 0.32719(14) 0.9005(2) 0.0148(4) Uani d . 1 1 H H2 0.7339 0.3336 0.9884 0.018 Uiso calc R 1 1 C C3 0.8351(3) 0.34197(14) 0.8846(2) 0.0165(5) Uani d . 1 1 H H3A 0.8484 0.2936 0.8475 0.02 Uiso calc R 1 1 H H3B 0.9393 0.3509 0.9678 0.02 Uiso calc R 1 1 C C4 0.7998(3) 0.41469(15) 0.8011(2) 0.0166(5) Uani d . 1 1 H H4A 0.8325 0.4641 0.8523 0.02 Uiso calc R 1 1 H H4B 0.8685 0.4108 0.7699 0.02 Uiso calc R 1 1 C C5 0.6234(3) 0.42259(15) 0.6907(2) 0.0158(5) Uani d . 1 1 H H5 0.5959 0.4751 0.6456 0.019 Uiso calc R 1 1 C C6 0.5166(3) 0.36048(14) 0.6193(2) 0.0155(5) Uani d . 1 1 H H6 0.4252 0.3769 0.5324 0.019 Uiso calc R 1 1 C C7 0.5621(3) 0.27224(15) 0.6315(2) 0.0190(5) Uani d . 1 1 H H7A 0.6789 0.2677 0.6643 0.023 Uiso calc R 1 1 H H7B 0.4961 0.247 0.5477 0.023 Uiso calc R 1 1 C C8 0.5337(3) 0.22648(15) 0.7191(2) 0.0185(5) Uani d . 1 1 H H8A 0.4181 0.2086 0.6701 0.022 Uiso calc R 1 1 H H8B 0.6035 0.1778 0.7505 0.022 Uiso calc R 1 1 C C9 0.2957(3) 0.44979(13) 0.8546(2) 0.0137(4) Uani d . 1 1 C C10 0.2083(3) 0.50625(13) 0.7626(2) 0.0148(4) Uani d . 1 1 H H10 0.1291 0.537 0.7632 0.018 Uiso calc R 1 1 C C11 0.2289(3) 0.52149(13) 0.6666(2) 0.0127(4) Uani d . 1 1 C C12 0.2617(3) 0.43797(14) 0.9529(2) 0.0147(4) Uani d . 1 1 C C13 0.1291(3) 0.58218(14) 0.5719(2) 0.0136(4) Uani d . 1 1 C C14 -0.0021(3) 0.62730(14) 0.5509(2) 0.0168(5) Uani d . 1 1 H H14 -0.0426 0.6241 0.6004 0.02 Uiso calc R 1 1 C C15 -0.0666(3) 0.67846(14) 0.4460(2) 0.0209(5) Uani d . 1 1 H H15 -0.1575 0.7131 0.4159 0.025 Uiso calc R 1 1 C C16 0.0157(3) 0.67274(14) 0.3923(2) 0.0211(5) Uani d . 1 1 H H16 -0.0108 0.7036 0.322 0.025 Uiso calc R 1 1 B B01 -0.1712(3) 0.63633(17) 0.7407(3) 0.0181(5) Uani d . 1 1 O O1 0.4068(2) 0.40020(9) 0.87454(15) 0.0148(3) Uani d . 1 1 O O2 0.33165(19) 0.48609(9) 0.65401(15) 0.0150(3) Uani d . 1 1 F F01 -0.00233(17) 0.64810(9) 0.80407(14) 0.0242(3) Uani d . 1 1 F F1 0.40033(16) 0.44090(9) 1.06804(12) 0.0195(3) Uani d . 1 1 F F2 0.19336(17) 0.36622(8) 0.93805(13) 0.0199(3) Uani d . 1 1 F F02 -0.25359(18) 0.70539(9) 0.67336(14) 0.0287(3) Uani d . 1 1 F F03 -0.2058(2) 0.62018(10) 0.82622(15) 0.0314(4) Uani d . 1 1 F F3 0.16081(17) 0.49348(9) 0.94621(13) 0.0212(3) Uani d . 1 1 F F04 -0.21904(18) 0.57198(9) 0.65863(13) 0.0221(3) Uani d . 1 1 S S1 0.17045(8) 0.60457(4) 0.46499(6) 0.01898(13) Uani d . 1 1 Pd Pd1 0.479840(19) 0.396026(10) 0.761842(15) 0.01125(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 0.0166(11) 0.0113(11) 0.0151(11) 0.0038(8) 0.0092(10) 0.0050(9) C2 0.0144(11) 0.0160(11) 0.0111(11) 0.0043(9) 0.0057(9) 0.0045(9) C3 0.0114(10) 0.0220(12) 0.0137(11) 0.0017(9) 0.0059(9) 0.0020(9) C4 0.0126(11) 0.0218(12) 0.0157(12) -0.0017(9) 0.0084(10) -0.0005(10) C5 0.0152(11) 0.0222(12) 0.0135(11) 0.0030(9) 0.0103(10) 0.0058(9) C6 0.0143(11) 0.0229(13) 0.0091(11) 0.0026(9) 0.0067(9) 0.0032(9) C7 0.0209(12) 0.0212(13) 0.0147(12) 0.0016(10) 0.0103(10) -0.0035(10) C8 0.0170(11) 0.0167(12) 0.0184(12) 0.0020(9) 0.0084(10) -0.0010(10) C9 0.0141(10) 0.0130(11) 0.0156(11) -0.0034(8) 0.0096(9) -0.0026(9) C10 0.0136(10) 0.0149(11) 0.0166(11) 0.0008(9) 0.0093(9) 0.0003(9) C11 0.0099(10) 0.0101(10) 0.0135(11) -0.0008(8) 0.0042(9) -0.0007(8) C12 0.0152(11) 0.0143(11) 0.0164(11) 0.0000(9) 0.0103(10) 0.0001(9) C13 0.0130(10) 0.0134(11) 0.0128(11) -0.0015(8) 0.0065(9) 0.0003(9) C14 0.0138(11) 0.0145(11) 0.0171(12) -0.0013(9) 0.0061(10) 0.0013(9) C15 0.0182(12) 0.0148(12) 0.0226(13) 0.0021(9) 0.0079(11) -0.0003(10) C16 0.0240(13) 0.0143(12) 0.0155(12) -0.0001(10) 0.0061(11) 0.0018(9) B01 0.0208(13) 0.0166(13) 0.0159(13) 0.0017(11) 0.0101(12) -0.0010(11) O1 0.0156(8) 0.0161(8) 0.0158(8) 0.0039(6) 0.0109(7) 0.0034(6) O2 0.0143(8) 0.0155(8) 0.0148(8) 0.0023(6) 0.0082(7) 0.0025(6) F01 0.0173(7) 0.0267(8) 0.0219(8) 0.0021(6) 0.0077(6) -0.0058(6) F1 0.0160(7) 0.0268(8) 0.0126(7) -0.0018(6) 0.0066(6) 0.0001(6) F2 0.0228(7) 0.0198(7) 0.0220(8) -0.0054(6) 0.0157(7) -0.0014(6) F02 0.0255(8) 0.0210(8) 0.0255(8) 0.0057(6) 0.0069(7) 0.0019(6) F03 0.0381(9) 0.0393(9) 0.0263(9) -0.0036(7) 0.0242(8) -0.0045(7) F3 0.0240(7) 0.0232(8) 0.0229(8) 0.0073(6) 0.0173(7) 0.0022(6) F04 0.0289(8) 0.0180(7) 0.0183(7) -0.0035(6) 0.0131(7) -0.0037(6) S1 0.0218(3) 0.0182(3) 0.0169(3) 0.0032(2) 0.0112(3) 0.0036(2) Pd1 0.01058(9) 0.01181(10) 0.01148(10) 0.00138(6) 0.00650(8) 0.00158(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' B B 0.0013 0.0007 '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' 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 126.6(2) C2 C1 Pd1 72.33(13) C8 C1 Pd1 107.20(15) C2 C1 H1 114 C8 C1 H1 114 Pd1 C1 H1 114 C1 C2 C3 125.0(2) C1 C2 Pd1 70.78(13) C3 C2 Pd1 110.49(15) C1 C2 H2 114.1 C3 C2 H2 114.1 Pd1 C2 H2 114.1 C2 C3 C4 112.16(18) C2 C3 H3A 109.2 C4 C3 H3A 109.2 C2 C3 H3B 109.2 C4 C3 H3B 109.2 H3A C3 H3B 107.9 C5 C4 C3 114.25(19) C5 C4 H4A 108.7 C3 C4 H4A 108.7 C5 C4 H4B 108.7 C3 C4 H4B 108.7 H4A C4 H4B 107.6 C6 C5 C4 126.8(2) C6 C5 Pd1 72.23(12) C4 C5 Pd1 105.75(14) C6 C5 H5 114.3 C4 C5 H5 114.3 Pd1 C5 H5 114.3 C5 C6 C7 125.6(2) C5 C6 Pd1 70.72(12) C7 C6 Pd1 111.15(14) C5 C6 H6 113.8 C7 C6 H6 113.8 Pd1 C6 H6 113.8 C6 C7 C8 112.40(18) C6 C7 H7A 109.1 C8 C7 H7A 109.1 C6 C7 H7B 109.1 C8 C7 H7B 109.1 H7A C7 H7B 107.9 C1 C8 C7 114.1(2) C1 C8 H8A 108.7 C7 C8 H8A 108.7 C1 C8 H8B 108.7 C7 C8 H8B 108.7 H8A C8 H8B 107.6 O1 C9 C10 130.8(2) O1 C9 C12 109.90(19) C10 C9 C12 119.33(19) C9 C10 C11 123.9(2) C9 C10 H10 118 C11 C10 H10 118 O2 C11 C10 125.6(2) O2 C11 C13 114.33(19) C10 C11 C13 120.11(19) F1 C12 F2 107.87(18) F1 C12 F3 107.43(18) F2 C12 F3 107.61(17) F1 C12 C9 110.80(17) F2 C12 C9 109.94(18) F3 C12 C9 113.00(18) C14 C13 C11 129.8(2) C14 C13 S1 111.82(17) C11 C13 S1 118.38(16) C13 C14 C15 110.9(2) C13 C14 H14 124.5 C15 C14 H14 124.5 C16 C15 C14 113.0(2) C16 C15 H15 123.5 C14 C15 H15 123.5 C15 C16 S1 112.72(19) C15 C16 H16 123.6 S1 C16 H16 123.6 F03 B01 F02 109.9(2) F03 B01 F04 110.2(2) F02 B01 F04 109.4(2) F03 B01 F01 109.6(2) F02 B01 F01 109.2(2) F04 B01 F01 108.62(19) C9 O1 Pd1 121.37(14) C11 O2 Pd1 125.07(14) C16 S1 C13 91.52(12) O2 Pd1 O1 93.23(6) O2 Pd1 C1 160.45(8) O1 Pd1 C1 88.65(7) O2 Pd1 C5 87.08(8) O1 Pd1 C5 158.94(8) C1 Pd1 C5 98.05(9) O2 Pd1 C6 91.28(7) O1 Pd1 C6 163.63(8) C1 Pd1 C6 81.96(8) C5 Pd1 C6 37.05(9) O2 Pd1 C2 162.05(8) O1 Pd1 C2 91.56(7) C1 Pd1 C2 36.89(8) C5 Pd1 C2 82.31(8) C6 Pd1 C2 88.94(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.382(3) C1 C8 1.503(3) C1 Pd1 2.174(2) C1 H1 1 C2 C3 1.516(3) C2 Pd1 2.194(2) C2 H2 1 C3 C4 1.531(3) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.506(3) C4 H4A 0.99 C4 H4B 0.99 C5 C6 1.388(3) C5 Pd1 2.174(2) C5 H5 1 C6 C7 1.518(3) C6 Pd1 2.194(2) C6 H6 1 C7 C8 1.540(3) C7 H7A 0.99 C7 H7B 0.99 C8 H8A 0.99 C8 H8B 0.99 C9 O1 1.286(3) C9 C10 1.371(3) C9 C12 1.532(3) C10 C11 1.416(3) C10 H10 0.95 C11 O2 1.282(3) C11 C13 1.456(3) C12 F1 1.333(3) C12 F2 1.333(3) C12 F3 1.336(2) C13 C14 1.399(3) C13 S1 1.724(2) C14 C15 1.417(3) C14 H14 0.95 C15 C16 1.369(3) C15 H15 0.95 C16 S1 1.698(3) C16 H16 0.95 B01 F03 1.384(3) B01 F02 1.391(3) B01 F04 1.392(3) B01 F01 1.402(3) O1 Pd1 2.0032(15) O2 Pd1 2.0028(15) 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 F01 . 0.95 2.51 3.420(3) 161.5 C10 H10 F3 . 0.95 2.35 2.731(2) 103.3 C14 H14 F01 . 0.95 2.5 3.351(3) 149.4 C14 H14 F04 . 0.95 2.46 3.349(3) 155.2 C2 H2 F01 3_667 1 2.5 3.278(3) 134.6 C3 H3B F03 3_667 0.99 2.51 3.496(3) 177 C5 H5 F04 1_655 1 2.39 3.106(3) 127.8 C6 H6 F04 3_566 1 2.29 3.290(3) 173.9 C16 H16 F01 4_575 0.95 2.48 3.165(3) 128.5 C16 H16 F02 4_575 0.95 2.55 3.262(3) 131.8 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 -3.4(4) Pd1 C1 C2 C3 -102.0(2) C8 C1 C2 Pd1 98.6(2) C1 C2 C3 C4 94.5(3) Pd1 C2 C3 C4 14.2(2) C2 C3 C4 C5 -39.0(3) C3 C4 C5 C6 -36.9(3) C3 C4 C5 Pd1 42.5(2) C4 C5 C6 C7 -6.0(3) Pd1 C5 C6 C7 -102.7(2) C4 C5 C6 Pd1 96.7(2) C5 C6 C7 C8 93.6(3) Pd1 C6 C7 C8 12.7(2) C2 C1 C8 C7 -40.5(3) Pd1 C1 C8 C7 39.9(2) C6 C7 C8 C1 -35.9(3) O1 C9 C10 C11 -0.9(4) C12 C9 C10 C11 -179.4(2) C9 C10 C11 O2 -1.0(4) C9 C10 C11 C13 179.4(2) O1 C9 C12 F1 52.3(2) C10 C9 C12 F1 -128.9(2) O1 C9 C12 F2 -66.8(2) C10 C9 C12 F2 112.0(2) O1 C9 C12 F3 172.96(18) C10 C9 C12 F3 -8.3(3) O2 C11 C13 C14 174.3(2) C10 C11 C13 C14 -6.1(4) O2 C11 C13 S1 -5.0(3) C10 C11 C13 S1 174.60(17) C11 C13 C14 C15 -178.6(2) S1 C13 C14 C15 0.8(3) C13 C14 C15 C16 -1.1(3) C14 C15 C16 S1 1.0(3) C10 C9 O1 Pd1 -0.1(3) C12 C9 O1 Pd1 178.45(13) C10 C11 O2 Pd1 3.6(3) C13 C11 O2 Pd1 -176.77(14) C15 C16 S1 C13 -0.5(2) C14 C13 S1 C16 -0.19(19) C11 C13 S1 C16 179.27(19) C11 O2 Pd1 O1 -3.53(18) C11 O2 Pd1 C1 91.5(3) C11 O2 Pd1 C5 -162.45(18) C11 O2 Pd1 C6 160.73(18) C11 O2 Pd1 C2 -108.8(3) C9 O1 Pd1 O2 1.83(17) C9 O1 Pd1 C1 -158.70(18) C9 O1 Pd1 C5 92.1(3) C9 O1 Pd1 C6 -103.9(3) C9 O1 Pd1 C2 164.52(17) C2 C1 Pd1 O2 169.74(18) C8 C1 Pd1 O2 46.0(3) C2 C1 Pd1 O1 -94.40(13) C8 C1 Pd1 O1 141.84(15) C2 C1 Pd1 C5 65.56(14) C8 C1 Pd1 C5 -58.20(16) C2 C1 Pd1 C6 99.04(14) C8 C1 Pd1 C6 -24.72(15) C8 C1 Pd1 C2 -123.8(2) C6 C5 Pd1 O2 -96.00(14) C4 C5 Pd1 O2 139.72(16) C6 C5 Pd1 O1 172.58(18) C4 C5 Pd1 O1 48.3(3) C6 C5 Pd1 C1 65.04(15) C4 C5 Pd1 C1 -59.24(17) C4 C5 Pd1 C6 -124.3(2) C6 C5 Pd1 C2 98.51(15) C4 C5 Pd1 C2 -25.77(16) C5 C6 Pd1 O2 83.45(14) C7 C6 Pd1 O2 -154.86(16) C5 C6 Pd1 O1 -170.5(2) C7 C6 Pd1 O1 -48.8(3) C5 C6 Pd1 C1 -114.96(15) C7 C6 Pd1 C1 6.73(16) C7 C6 Pd1 C5 121.7(2) C5 C6 Pd1 C2 -78.60(14) C7 C6 Pd1 C2 43.09(16) C1 C2 Pd1 O2 -168.8(2) C3 C2 Pd1 O2 -47.6(3) C1 C2 Pd1 O1 85.67(13) C3 C2 Pd1 O1 -153.07(16) C3 C2 Pd1 C1 121.3(2) C1 C2 Pd1 C5 -114.55(14) C3 C2 Pd1 C5 6.71(16) C1 C2 Pd1 C6 -77.97(14) C3 C2 Pd1 C6 43.30(17)