#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105310.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_2105310 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, B F4' _chemical_formula_structural '(Pd (C8 H12) (O2 C5 H7)) (B F4)' _chemical_formula_sum 'C13 H19 B F4 O2 Pd' _chemical_formula_weight 400.49 _chemical_name_systematic ; (acetylacetonato)(\h^4^-cyclo-octa-1,5-dienyl)palladium(II) tetrafluoroborate ; _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 26.2908(11) _cell_length_b 7.1684(3) _cell_length_c 7.7782(3) _cell_measurement_reflns_used 8277 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.38 _cell_measurement_theta_min 2.84 _cell_volume 1465.90(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 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0254 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 15654 _diffrn_reflns_theta_full 28.38 _diffrn_reflns_theta_max 28.38 _diffrn_reflns_theta_min 3.04 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_correction_T_min 0.6644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.052 _refine_diff_density_min -0.61 _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881, 1143 Friedel pairs ; _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 3117 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.927 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0221 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.7363P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0618 _reflns_number_gt 2960 _reflns_number_total 3117 _reflns_threshold_expression >2\s(I) _journal_paper_doi 10.1107/S0108768112046733 _iucr_refine_instructions_details ; TITL 10RTH5_0ma in Pca2(1) CELL 0.71073 26.2908 7.1684 7.7782 90.000 90.000 90.000 ZERR 4.00 0.0011 0.0003 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, - Y, Z SYMM 1/2 - X, Y, 1/2 + Z SFAC C H B O F PD UNIT 52 76 4 8 16 4 MERG 2 OMIT -4.00 180.00 OMIT 0 1 0 OMIT 2 0 0 EQIV $1 -x+1, -y+1, z+0.5 EQIV $2 -x+1, -y+2, z-0.5 EQIV $3 x+0.5, -y+2, z HTAB C7 F01 HTAB C2 F02_$1 HTAB C6 F04_$2 HTAB C12 F04_$3 HTAB C10 F03_$3 HTAB C13 F03_$3 FMAP 2 PLAN 10 SIZE 0.07 0.10 0.34 ACTA BOND $H CONF LIST 4 L.S. 8 TEMP -173.20 WGHT 0.046000 0.736300 FVAR 0.12956 C1 1 0.608089 0.537277 0.103471 11.00000 0.01611 0.01673 = 0.02600 0.00661 -0.00133 -0.00215 AFIX 13 H1 2 0.633491 0.435041 0.086750 11.00000 -1.20000 AFIX 0 C2 1 0.608909 0.615965 0.266307 11.00000 0.01686 0.02120 = 0.02222 0.00903 0.00082 -0.00272 AFIX 13 H2 2 0.634455 0.559026 0.345802 11.00000 -1.20000 AFIX 0 C3 1 0.564985 0.709382 0.356196 11.00000 0.02339 0.03012 = 0.01726 0.00264 0.00609 -0.00307 AFIX 23 H3A 2 0.578483 0.788729 0.449848 11.00000 -1.20000 H3B 2 0.543314 0.612238 0.409294 11.00000 -1.20000 AFIX 0 C4 1 0.531915 0.830206 0.237237 11.00000 0.01758 0.02987 = 0.02274 0.00378 0.00574 0.00299 AFIX 23 H4A 2 0.506736 0.749684 0.178500 11.00000 -1.20000 H4B 2 0.512987 0.922150 0.307428 11.00000 -1.20000 AFIX 0 C5 1 0.562895 0.932207 0.104189 11.00000 0.01275 0.02310 = 0.02443 0.00168 -0.00050 0.00612 AFIX 13 H5 2 0.561385 1.071147 0.114524 11.00000 -1.20000 AFIX 0 C6 1 0.572070 0.868858 -0.061957 11.00000 0.01171 0.03124 = 0.02220 0.00907 -0.00323 0.00363 AFIX 13 H6 2 0.575471 0.970570 -0.149192 11.00000 -1.20000 AFIX 0 C7 1 0.557284 0.683735 -0.136079 11.00000 0.01857 0.04241 = 0.01759 -0.00088 -0.00153 -0.00423 AFIX 23 H7A 2 0.579278 0.657449 -0.236512 11.00000 -1.20000 H7B 2 0.521776 0.691562 -0.177824 11.00000 -1.20000 AFIX 0 C8 1 0.561424 0.519895 -0.008852 11.00000 0.02136 0.03082 = 0.02646 -0.00402 -0.00272 -0.00696 AFIX 23 H8A 2 0.530684 0.516668 0.064598 11.00000 -1.20000 H8B 2 0.563020 0.401208 -0.073710 11.00000 -1.20000 AFIX 0 C9 1 0.750943 0.810540 0.109864 11.00000 0.01459 0.01554 = 0.01085 -0.00121 -0.00009 0.00007 C10 1 0.754617 0.983166 0.029439 11.00000 0.01414 0.01519 = 0.01779 0.00075 0.00123 -0.00284 AFIX 43 H10 2 0.787911 1.028625 0.007121 11.00000 -1.20000 AFIX 0 C11 1 0.714135 1.096145 -0.021685 11.00000 0.02029 0.01436 = 0.01305 0.00103 -0.00020 -0.00257 C12 1 0.798897 0.710090 0.160108 11.00000 0.01229 0.01810 = 0.02494 0.00455 0.00138 0.00122 AFIX 137 H12A 2 0.796860 0.673186 0.281228 11.00000 -1.50000 H12B 2 0.828140 0.792924 0.143475 11.00000 -1.50000 H12C 2 0.802946 0.598690 0.088368 11.00000 -1.50000 AFIX 0 C13 1 0.725421 1.284052 -0.101881 11.00000 0.02226 0.01245 = 0.02490 0.00477 0.00406 -0.00059 AFIX 137 H13A 2 0.702011 1.305967 -0.197825 11.00000 -1.50000 H13B 2 0.760521 1.285607 -0.144273 11.00000 -1.50000 H13C 2 0.721038 1.382230 -0.015463 11.00000 -1.50000 AFIX 0 B01 3 0.392216 0.779118 0.004739 11.00000 0.02100 0.01969 = 0.02461 -0.00323 -0.00069 -0.00006 O1 4 0.709863 0.720484 0.144547 11.00000 0.01196 0.01508 = 0.02264 0.00434 -0.00088 0.00010 O2 4 0.666749 1.060552 -0.006196 11.00000 0.01723 0.01562 = 0.02070 0.00443 0.00054 0.00086 F01 5 0.438046 0.757712 -0.080069 11.00000 0.02894 0.04415 = 0.06061 -0.00566 0.01401 -0.00201 F02 5 0.384059 0.631572 0.111205 11.00000 0.09789 0.03273 = 0.04876 0.01153 0.03341 0.00236 F03 5 0.354618 0.784787 -0.119746 11.00000 0.03407 0.08596 = 0.06852 -0.04399 -0.02256 0.03054 F04 5 0.391084 0.945531 0.094656 11.00000 0.05332 0.02626 = 0.03382 -0.01215 -0.00217 -0.00276 PD1 6 0.640693 0.819499 0.088001 11.00000 0.01080 0.01499 = 0.01429 0.00345 0.00009 -0.00024 HKLF 4 REM 10RTH5_0ma in Pca2(1) REM R1 = 0.0221 for 2960 Fo > 4sig(Fo) and 0.0238 for all 3117 data REM 192 parameters refined using 1 restraints END WGHT 0.0318 0.7405 REM Highest difference peak 1.052, deepest hole -0.610, 1-sigma level 0.086 Q1 1 0.3475 0.6949 -0.0145 11.00000 0.05 1.05 Q2 1 0.4194 0.6530 0.1002 11.00000 0.05 0.87 Q3 1 0.3471 0.6921 0.1916 11.00000 0.05 0.80 Q4 1 0.4185 0.9380 0.0952 11.00000 0.05 0.48 Q5 1 0.6450 1.1973 -0.1989 11.00000 0.05 0.46 Q6 1 0.4121 0.7679 -0.1285 11.00000 0.05 0.41 Q7 1 0.5882 0.2222 -0.2086 11.00000 0.05 0.34 Q8 1 0.3799 0.9327 0.1309 11.00000 0.05 0.32 Q9 1 0.7534 0.9024 0.0861 11.00000 0.05 0.32 Q10 1 0.3809 0.9463 0.0482 11.00000 0.05 0.30 ; _[local]_cod_data_source_file eb5019.cif _[local]_cod_data_source_block 10rth5_0ma _cod_database_code 2105310 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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 0.60809(9) 0.5373(3) 0.1035(6) 0.0196(6) Uani d . 1 1 H H1 0.6335 0.435 0.0868 0.024 Uiso calc R 1 1 C C2 0.60891(10) 0.6160(4) 0.2663(4) 0.0201(6) Uani d . 1 1 H H2 0.6345 0.559 0.3458 0.024 Uiso calc R 1 1 C C3 0.56498(16) 0.7094(5) 0.3562(5) 0.0236(8) Uani d . 1 1 H H3A 0.5785 0.7887 0.4498 0.028 Uiso calc R 1 1 H H3B 0.5433 0.6122 0.4093 0.028 Uiso calc R 1 1 C C4 0.53191(12) 0.8302(4) 0.2372(4) 0.0234(7) Uani d . 1 1 H H4A 0.5067 0.7497 0.1785 0.028 Uiso calc R 1 1 H H4B 0.513 0.9221 0.3074 0.028 Uiso calc R 1 1 C C5 0.56289(9) 0.9322(4) 0.1042(5) 0.0201(6) Uani d . 1 1 H H5 0.5614 1.0711 0.1145 0.024 Uiso calc R 1 1 C C6 0.57207(10) 0.8689(5) -0.0620(4) 0.0217(6) Uani d . 1 1 H H6 0.5755 0.9706 -0.1492 0.026 Uiso calc R 1 1 C C7 0.55728(17) 0.6837(5) -0.1361(5) 0.0262(9) Uani d . 1 1 H H7A 0.5793 0.6574 -0.2365 0.031 Uiso calc R 1 1 H H7B 0.5218 0.6916 -0.1778 0.031 Uiso calc R 1 1 C C8 0.56142(12) 0.5199(5) -0.0089(4) 0.0262(7) Uani d . 1 1 H H8A 0.5307 0.5167 0.0646 0.031 Uiso calc R 1 1 H H8B 0.563 0.4012 -0.0737 0.031 Uiso calc R 1 1 C C9 0.75094(10) 0.8105(3) 0.1099(4) 0.0137(6) Uani d . 1 1 C C10 0.75462(11) 0.9832(4) 0.0294(4) 0.0157(5) Uani d . 1 1 H H10 0.7879 1.0286 0.0071 0.019 Uiso calc R 1 1 C C11 0.71414(10) 1.0961(4) -0.0217(4) 0.0159(5) Uani d . 1 1 C C12 0.79890(10) 0.7101(4) 0.1601(4) 0.0184(6) Uani d . 1 1 H H12A 0.7969 0.6732 0.2812 0.028 Uiso calc R 1 1 H H12B 0.8281 0.7929 0.1435 0.028 Uiso calc R 1 1 H H12C 0.8029 0.5987 0.0884 0.028 Uiso calc R 1 1 C C13 0.72542(12) 1.2841(4) -0.1019(4) 0.0199(6) Uani d . 1 1 H H13A 0.702 1.306 -0.1978 0.03 Uiso calc R 1 1 H H13B 0.7605 1.2856 -0.1443 0.03 Uiso calc R 1 1 H H13C 0.721 1.3822 -0.0155 0.03 Uiso calc R 1 1 B B01 0.39222(13) 0.7791(5) 0.0047(5) 0.0218(7) Uani d . 1 1 O O1 0.70986(7) 0.7205(3) 0.1445(3) 0.0166(4) Uani d . 1 1 O O2 0.66675(7) 1.0606(3) -0.0062(3) 0.0178(4) Uani d . 1 1 F F01 0.43805(8) 0.7577(3) -0.0801(4) 0.0446(5) Uani d . 1 1 F F02 0.38406(12) 0.6316(3) 0.1112(4) 0.0598(8) Uani d . 1 1 F F03 0.35462(9) 0.7848(5) -0.1197(5) 0.0629(10) Uani d . 1 1 F F04 0.39108(7) 0.9455(2) 0.0947(4) 0.0378(4) Uani d . 1 1 Pd Pd1 0.640693(6) 0.81950(2) 0.08800(5) 0.01336(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 0.0161(11) 0.0167(10) 0.0260(18) -0.0022(8) -0.0013(14) 0.0066(15) C2 0.0169(13) 0.0212(13) 0.0222(15) -0.0027(11) 0.0008(11) 0.0090(12) C3 0.0234(19) 0.0301(17) 0.0173(17) -0.0031(14) 0.0061(14) 0.0026(13) C4 0.0176(14) 0.0299(16) 0.0227(16) 0.0030(11) 0.0057(12) 0.0038(12) C5 0.0128(10) 0.0231(12) 0.0244(16) 0.0061(9) -0.0005(14) 0.0017(15) C6 0.0117(12) 0.0312(15) 0.0222(15) 0.0036(11) -0.0032(11) 0.0091(13) C7 0.0186(17) 0.042(2) 0.0176(18) -0.0042(13) -0.0015(14) -0.0009(13) C8 0.0214(14) 0.0308(16) 0.0265(16) -0.0070(12) -0.0027(13) -0.0040(13) C9 0.0146(11) 0.0155(10) 0.0109(19) 0.0001(8) -0.0001(11) -0.0012(10) C10 0.0141(12) 0.0152(11) 0.0178(11) -0.0028(10) 0.0012(9) 0.0007(10) C11 0.0203(12) 0.0144(12) 0.0130(12) -0.0026(10) -0.0002(11) 0.0010(10) C12 0.0123(12) 0.0181(12) 0.0249(15) 0.0012(10) 0.0014(11) 0.0045(11) C13 0.0223(15) 0.0124(11) 0.0249(15) -0.0006(10) 0.0041(12) 0.0048(11) B01 0.0210(16) 0.0197(15) 0.0246(18) -0.0001(12) -0.0007(13) -0.0032(14) O1 0.0120(8) 0.0151(8) 0.0226(10) 0.0001(7) -0.0009(7) 0.0043(7) O2 0.0172(9) 0.0156(9) 0.0207(10) 0.0009(7) 0.0005(8) 0.0044(8) F01 0.0289(11) 0.0441(12) 0.0606(16) -0.0020(10) 0.0140(11) -0.0057(12) F02 0.0979(19) 0.0327(10) 0.0488(19) 0.0024(12) 0.0334(17) 0.0115(14) F03 0.0341(14) 0.086(2) 0.069(2) 0.0305(12) -0.0226(12) -0.0440(18) F04 0.0533(11) 0.0263(8) 0.0338(10) -0.0028(7) -0.0022(15) -0.0121(14) Pd1 0.01080(9) 0.01499(9) 0.01429(10) -0.00024(5) 0.00009(12) 0.00345(11) 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' 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 125.0(3) C2 C1 Pd1 70.73(15) C8 C1 Pd1 111.1(2) C2 C1 H1 114 C8 C1 H1 114 Pd1 C1 H1 114 C1 C2 C3 126.3(3) C1 C2 Pd1 72.36(17) C3 C2 Pd1 107.0(2) C1 C2 H2 114.2 C3 C2 H2 114.2 Pd1 C2 H2 114.2 C2 C3 C4 113.9(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 112.4(3) 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 125.0(3) C6 C5 Pd1 70.49(15) C4 C5 Pd1 111.30(19) C6 C5 H5 114 C4 C5 H5 114 Pd1 C5 H5 114 C5 C6 C7 127.0(3) C5 C6 Pd1 72.48(16) C7 C6 Pd1 106.1(2) 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 111.5(3) C1 C8 H8A 109.3 C7 C8 H8A 109.3 C1 C8 H8B 109.3 C7 C8 H8B 109.3 H8A C8 H8B 108 O1 C9 C10 126.8(2) O1 C9 C12 114.1(2) C10 C9 C12 119.0(2) C9 C10 C11 126.3(3) C9 C10 H10 116.8 C11 C10 H10 116.8 O2 C11 C10 127.0(2) O2 C11 C13 114.1(2) C10 C11 C13 119.0(2) 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 F02 B01 F01 110.0(3) F02 B01 F04 111.1(3) F01 B01 F04 110.8(3) F02 B01 F03 109.6(3) F01 B01 F03 107.0(3) F04 B01 F03 108.2(3) C9 O1 Pd1 122.60(16) C11 O2 Pd1 122.80(17) O2 Pd1 O1 94.35(8) O2 Pd1 C6 86.97(10) O1 Pd1 C6 158.19(11) O2 Pd1 C2 160.69(10) O1 Pd1 C2 88.35(9) C6 Pd1 C2 97.58(11) O2 Pd1 C1 161.58(14) O1 Pd1 C1 90.91(9) C6 Pd1 C1 81.72(12) C2 Pd1 C1 36.91(15) O2 Pd1 C5 91.27(9) O1 Pd1 C5 164.02(13) C6 Pd1 C5 37.02(13) C2 Pd1 C5 81.56(11) C1 Pd1 C5 88.42(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.387(6) C1 C8 1.511(4) C1 Pd1 2.200(2) C1 H1 1 C2 C3 1.507(5) C2 Pd1 2.180(3) C2 H2 1 C3 C4 1.537(5) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.506(5) C4 H4A 0.99 C4 H4B 0.99 C5 C6 1.391(5) C5 Pd1 2.203(2) C5 H5 1 C6 C7 1.498(5) C6 Pd1 2.177(3) C6 H6 1 C7 C8 1.540(5) C7 H7A 0.99 C7 H7B 0.99 C8 H8A 0.99 C8 H8B 0.99 C9 O1 1.287(3) C9 C10 1.390(3) C9 C12 1.504(4) C10 C11 1.395(4) C10 H10 0.95 C11 O2 1.277(3) C11 C13 1.514(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 B01 F02 1.360(5) B01 F01 1.382(4) B01 F04 1.383(4) B01 F03 1.384(4) O1 Pd1 2.0011(19) O2 Pd1 1.9980(18) 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 C7 H7B F01 . 0.99 2.38 3.209(5) 141.2 C2 H2 F02 2_665 1 2.52 3.222(4) 126.7 C6 H6 F04 2_674 1 2.26 3.137(4) 145.8 C12 H12B F04 3_575 0.98 2.53 3.497(3) 169.2 C10 H10 F03 3_575 0.95 2.42 3.320(4) 158.9 C13 H13B F03 3_575 0.98 2.53 3.435(4) 153.2 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 -4.4(5) Pd1 C1 C2 C3 98.4(3) C8 C1 C2 Pd1 -102.8(3) C1 C2 C3 C4 -39.4(4) Pd1 C2 C3 C4 40.9(3) C2 C3 C4 C5 -37.4(4) C3 C4 C5 C6 94.4(4) C3 C4 C5 Pd1 13.9(4) C4 C5 C6 C7 -5.6(5) Pd1 C5 C6 C7 97.2(3) C4 C5 C6 Pd1 -102.9(3) C5 C6 C7 C8 -36.9(5) Pd1 C6 C7 C8 43.0(3) C2 C1 C8 C7 95.1(4) Pd1 C1 C8 C7 14.4(3) C6 C7 C8 C1 -39.4(4) O1 C9 C10 C11 3.3(5) C12 C9 C10 C11 -178.4(3) C9 C10 C11 O2 -1.1(5) C9 C10 C11 C13 177.7(3) C10 C9 O1 Pd1 -0.7(4) C12 C9 O1 Pd1 -178.97(19) C10 C11 O2 Pd1 -3.3(4) C13 C11 O2 Pd1 177.89(19) C11 O2 Pd1 O1 4.3(2) C11 O2 Pd1 C6 -153.9(2) C11 O2 Pd1 C2 101.7(3) C11 O2 Pd1 C1 -101.9(3) C11 O2 Pd1 C5 169.3(2) C9 O1 Pd1 O2 -2.4(2) C9 O1 Pd1 C6 90.3(3) C9 O1 Pd1 C2 -163.3(2) C9 O1 Pd1 C1 159.9(3) C9 O1 Pd1 C5 -112.7(3) C5 C6 Pd1 O2 -96.14(17) C7 C6 Pd1 O2 139.4(2) C5 C6 Pd1 O1 169.7(2) C7 C6 Pd1 O1 45.3(4) C5 C6 Pd1 C2 65.00(19) C7 C6 Pd1 C2 -59.4(2) C5 C6 Pd1 C1 98.4(2) C7 C6 Pd1 C1 -26.0(2) C7 C6 Pd1 C5 -124.5(3) C1 C2 Pd1 O2 167.8(2) C3 C2 Pd1 O2 44.2(4) C1 C2 Pd1 O1 -93.72(16) C3 C2 Pd1 O1 142.7(2) C1 C2 Pd1 C6 65.21(17) C3 C2 Pd1 C6 -58.4(2) C3 C2 Pd1 C1 -123.6(3) C1 C2 Pd1 C5 98.69(18) C3 C2 Pd1 C5 -24.9(2) C2 C1 Pd1 O2 -167.3(2) C8 C1 Pd1 O2 -46.1(4) C2 C1 Pd1 O1 86.03(16) C8 C1 Pd1 O1 -152.8(2) C2 C1 Pd1 C6 -114.58(17) C8 C1 Pd1 C6 6.6(2) C8 C1 Pd1 C2 121.1(3) C2 C1 Pd1 C5 -78.01(19) C8 C1 Pd1 C5 43.1(3) C6 C5 Pd1 O2 83.27(18) C4 C5 Pd1 O2 -155.7(2) C6 C5 Pd1 O1 -166.1(3) C4 C5 Pd1 O1 -45.1(4) C4 C5 Pd1 C6 121.0(3) C6 C5 Pd1 C2 -114.74(19) C4 C5 Pd1 C2 6.3(2) C6 C5 Pd1 C1 -78.3(2) C4 C5 Pd1 C1 42.7(3) _cod_database_fobs_code 2105310