#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/37/2003730.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_2003730 loop_ _publ_author_name 'Spek, A. L.' 'Markies, B. A.' 'Kruis, D.' 'Boersma, J.' 'van Koten, G.' _publ_section_title ;(2-Acetylbicyclo[2.2.1]heptyl-C^3^,O)(2,2'-bipyridyl)palladium(II) Trifluoromethanesulfonate 0.5-Diethyl Ether Solvate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1535 _journal_page_last 1537 _journal_paper_doi 10.1107/S0108270194004245 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C44 H52 F6 N4 O9 Pd2 S2' _chemical_formula_weight 585.94 _chemical_name_systematic ; [C,O-(2-acetylbicyclohept[2.2.1]-3-yl)palladium(II)(2,2'-bipyridyl)] trifluoromethanesulfonate 0.5 diethylether solvate ; _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' _cell_angle_alpha 90 _cell_angle_beta 128.707(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.3658(12) _cell_length_b 11.0537(6) _cell_length_c 19.3767(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150 _cell_measurement_theta_max 14 _cell_measurement_theta_min 11 _cell_volume 2401.1(3) _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_collection 'Locally modified CAD4 (Version 5) software' _computing_data_reduction 'HELENA (Spek, 1993)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'DIRDIF92 (Beurskens et al., 1992)' _diffrn_ambient_temperature 150 _diffrn_measurement_device 'Enraf-Nonius Turbo CAD4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enraf-Nonius Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 6075 _diffrn_reflns_reduction_process ; ? ; _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.80 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_type 'empirical (DIFABS; Walker & Stuart, 1983)' _exptl_crystal_colour yellowish _exptl_crystal_density_diffrn 1.621 _exptl_crystal_description block _exptl_crystal_F_000 1188 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.830 _refine_diff_density_min -0.590 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.40 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 328 _refine_ls_number_reflns 4095 _refine_ls_R_factor_obs 0.037 _refine_ls_shift/esd_max 0.500 _refine_ls_shift/esd_mean 0.050 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)+0.0004F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.043 _reflns_number_observed 4095 _reflns_number_total 5168 _reflns_observed_criterion I>2.5\s(I) _cod_data_source_file ab1183.cif _cod_data_source_block S973A _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0004F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)+0.0004F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum ' C44 H52 F6 N4 O9 Pd2 S2' _cod_database_code 2003730 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Pd 0.0198(1) -0.0016(1) 0.0127(1) 0.0210(1) -0.0033(1) 0.0194(1) O 0.0245(14) 0.0003(11) 0.0140(13) 0.0304(15) -0.0064(12) 0.0344(16) N1 0.0240(16) -0.0011(11) 0.0147(14) 0.0217(15) -0.0014(12) 0.0198(16) N2 0.0243(16) 0.0017(12) 0.0177(15) 0.0254(16) -0.0007(12) 0.0246(17) C1 0.029(2) -0.0009(16) 0.0191(19) 0.0251(18) -0.0027(17) 0.031(2) C2 0.022(2) 0.0047(17) 0.013(2) 0.038(2) 0.0031(19) 0.040(3) C3 0.021(2) -0.0019(17) 0.010(2) 0.040(2) -0.0024(19) 0.038(3) C4 0.030(2) -0.0058(16) 0.0163(19) 0.031(2) -0.0046(17) 0.031(2) C5 0.0255(19) -0.0031(15) 0.0173(17) 0.0261(18) -0.0016(15) 0.0217(19) C6 0.0298(19) -0.0010(14) 0.0205(17) 0.0230(18) -0.0014(14) 0.0225(18) C7 0.040(2) -0.0058(17) 0.026(2) 0.0260(19) -0.0051(16) 0.030(2) C8 0.046(2) 0.0020(17) 0.032(2) 0.026(2) 0.0004(17) 0.035(2) C9 0.033(2) 0.0083(17) 0.023(2) 0.031(2) 0.0043(17) 0.035(2) C10 0.027(2) 0.0021(16) 0.0183(19) 0.0328(19) 0.0001(17) 0.029(2) C11 0.0231(18) -0.0014(14) 0.0147(16) 0.0231(17) -0.0031(14) 0.0215(19) C12 0.030(2) -0.0025(15) 0.0231(19) 0.0216(17) -0.0050(15) 0.031(2) C13 0.043(2) 0.0002(17) 0.029(2) 0.0252(18) -0.0052(17) 0.034(2) C14 0.046(3) -0.0024(17) 0.027(2) 0.0237(19) -0.0051(17) 0.034(2) C15 0.037(2) -0.0026(16) 0.0164(19) 0.026(2) -0.0058(15) 0.022(2) C16 0.0264(19) -0.0063(15) 0.0152(17) 0.0229(18) -0.0037(15) 0.024(2) C17 0.049(3) 0.0003(18) 0.033(2) 0.0283(19) -0.0005(17) 0.033(2) C18 0.026(2) -0.0023(17) 0.0165(19) 0.038(2) -0.0026(18) 0.030(2) C19 0.023(2) -0.004(2) 0.010(2) 0.054(3) -0.014(2) 0.053(3) O5 0.094(6) 0.009(5) 0.053(6) 0.105(6) 0.016(5) 0.120(7) C21 0.052(8) 0.009(6) 0.024(8) 0.068(9) -0.007(7) 0.073(10) C22 0.051(14) -0.04(2) -0.01(2) 0.32(5) 0.14(4) 0.24(5) C23 0.16(3) 0.010(13) -0.010(16) 0.049(10) 0.018(12) 0.096(17) C24 0.106(13) -0.010(8) 0.061(11) 0.055(9) -0.008(7) 0.084(11) S1 0.0295(6) 0.0029(4) 0.0073(5) 0.0250(5) -0.0023(4) 0.0373(6) F1 0.094(3) -0.011(2) 0.079(3) 0.094(3) -0.037(2) 0.113(3) F2 0.102(3) -0.019(3) 0.076(3) 0.104(3) 0.017(3) 0.115(3) F3 0.052(2) 0.004(2) 0.072(3) 0.118(3) -0.016(3) 0.175(5) O2 0.055(2) 0.0043(14) 0.0201(19) 0.0293(17) 0.0077(15) 0.058(2) O3 0.0286(16) 0.0072(13) 0.0080(15) 0.0430(17) -0.0069(14) 0.0383(18) O4 0.047(2) 0.0001(14) -0.0059(17) 0.0319(17) -0.0077(14) 0.046(2) C20 0.050(4) 0.001(3) 0.045(4) 0.068(4) -0.006(4) 0.099(5) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Pd 1.000 0.04125(2) 0.10808(2) 0.12473(2) 0.0198(1) Uani O 1.000 0.2177(2) 0.1285(2) 0.22633(18) 0.0328(9) Uani N1 1.000 -0.1303(3) 0.0789(3) 0.0193(2) 0.0211(9) Uani N2 1.000 0.0458(3) -0.0785(3) 0.1067(2) 0.0231(9) Uani C1 1.000 -0.2147(3) 0.1647(3) -0.0259(3) 0.0281(11) Uani C2 1.000 -0.3292(3) 0.1398(4) -0.1012(3) 0.0377(14) Uani C3 1.000 -0.3590(4) 0.0220(4) -0.1309(3) 0.0388(14) Uani C4 1.000 -0.2730(3) -0.0675(4) -0.0847(3) 0.0326(12) Uani C5 1.000 -0.1594(3) -0.0377(3) -0.0103(2) 0.0227(11) Uani C6 1.000 -0.0608(3) -0.1256(3) 0.0395(2) 0.0223(11) Uani C7 1.000 -0.0748(4) -0.2481(3) 0.0200(3) 0.0292(11) Uani C8 1.000 0.0236(4) -0.3232(4) 0.0706(3) 0.0311(12) Uani C9 1.000 0.1320(4) -0.2752(3) 0.1385(3) 0.0318(12) Uani C10 1.000 0.1406(3) -0.1528(3) 0.1556(3) 0.0291(11) Uani C11 1.000 0.0316(3) 0.2851(3) 0.1454(2) 0.0220(10) Uani C12 1.000 -0.0355(3) 0.3050(3) 0.1813(3) 0.0248(11) Uani C13 1.000 -0.0513(4) 0.4423(3) 0.1848(3) 0.0307(11) Uani C14 1.000 0.0768(4) 0.4863(3) 0.2617(3) 0.0332(14) Uani C15 1.000 0.1492(4) 0.3691(3) 0.2937(3) 0.0297(12) Uani C16 1.000 0.1602(3) 0.3309(3) 0.2222(2) 0.0248(11) Uani C17 1.000 0.0593(4) 0.2760(3) 0.2788(3) 0.0317(14) Uani C18 1.000 0.2500(3) 0.2320(4) 0.2564(3) 0.0320(12) Uani C19 1.000 0.3795(4) 0.2556(5) 0.3280(3) 0.0528(16) Uani O5 1.000 .5 .5 .5 0.116(4) Uani C21 0.500 0.4076(12) 0.5792(13) 0.4538(10) 0.075(5) Uani C22 0.500 0.382(3) 0.652(4) 0.391(3) 0.27(2) Uani C23 0.500 0.608(3) 0.336(2) 0.593(3) 0.163(12) Uani C24 0.500 0.5243(17) 0.4139(12) 0.5576(11) 0.081(6) Uani S1 1.000 0.32227(10) 0.48444(9) 0.11744(8) 0.0399(3) Uani F1 1.000 0.3195(4) 0.3775(3) -0.0037(3) 0.0906(17) Uani F2 1.000 0.3594(4) 0.5691(4) 0.0110(3) 0.1014(17) Uani F3 1.000 0.4919(3) 0.4434(4) 0.1082(3) 0.114(2) Uani O2 1.000 0.3415(3) 0.3673(3) 0.1569(2) 0.0579(11) Uani O3 1.000 0.1994(3) 0.5149(3) 0.0504(2) 0.0455(10) Uani O4 1.000 0.3945(3) 0.5796(3) 0.1782(2) 0.0656(11) Uani C20 1.000 0.3771(5) 0.4669(6) 0.0550(5) 0.073(3) Uani H1A 1.000 -0.1947(3) 0.2482(3) -0.0041(3) 0.035(3) Uiso H2A 1.000 -0.3878(3) 0.2050(4) -0.1332(3) 0.035(3) Uiso H3A 1.000 -0.4400(4) 0.0018(4) -0.1837(3) 0.035(3) Uiso H4A 1.000 -0.2926(3) -0.1516(4) -0.1050(3) 0.035(3) Uiso H7A 1.000 -0.1528(4) -0.2817(3) -0.0285(3) 0.035(3) Uiso H8A 1.000 0.0162(4) -0.4100(4) 0.0580(3) 0.035(3) Uiso H9A 1.000 0.2029(4) -0.3268(3) 0.1746(3) 0.035(3) Uiso H10A 1.000 0.2180(3) -0.1185(3) 0.2046(3) 0.035(3) Uiso H11A 1.000 -0.0065(3) 0.3265(3) 0.0888(2) 0.035(3) Uiso H12A 1.000 -0.1110(3) 0.2605(3) 0.1478(3) 0.035(3) Uiso H13A 1.000 -0.0802(4) 0.4814(3) 0.1292(3) 0.035(3) Uiso H13B 1.000 -0.1068(4) 0.4588(3) 0.1970(3) 0.035(3) Uiso H14A 1.000 0.1060(4) 0.5447(3) 0.2411(3) 0.035(3) Uiso H14B 1.000 0.0790(4) 0.5229(3) 0.3088(3) 0.035(3) Uiso H15A 1.000 0.2266(4) 0.3755(3) 0.3528(3) 0.035(3) Uiso H16A 1.000 0.1858(3) 0.3964(3) 0.2033(2) 0.035(3) Uiso H17A 1.000 0.0882(4) 0.1925(3) 0.2893(3) 0.035(3) Uiso H17B 1.000 0.0337(4) 0.2932(3) 0.3143(3) 0.035(3) Uiso H19A 1.000 0.4002(4) 0.3334(5) 0.3166(3) 0.111(14) Uiso H19B 1.000 0.4269(4) 0.1912(5) 0.3286(3) 0.111(14) Uiso H19C 1.000 0.3964(4) 0.2585(5) 0.3855(3) 0.111(14) Uiso H21A 0.500 0.3330(12) 0.5358(13) 0.4282(10) 0.1534 Uiso H21B 0.500 0.4212(12) 0.6388(13) 0.4967(10) 0.1534 Uiso H22A 0.500 0.313(3) 0.705(4) 0.367(3) 0.1534 Uiso H22B 0.500 0.364(3) 0.597(4) 0.344(3) 0.1534 Uiso H22C 0.500 0.452(3) 0.701(4) 0.412(3) 0.1534 Uiso H23A 0.500 0.604(3) 0.280(2) 0.630(3) 0.1534 Uiso H23B 0.500 0.683(3) 0.382(2) 0.629(3) 0.1534 Uiso H23C 0.500 0.605(3) 0.289(2) 0.548(3) 0.1534 Uiso H24A 0.500 0.4528(17) 0.3629(12) 0.5242(11) 0.1534 Uiso H24B 0.500 0.5308(17) 0.4551(12) 0.6053(11) 0.1534 Uiso loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag S S 'Cromer \& Mann (1968)' 0.1246 0.1234 Pd Pd 'Cromer \& Mann (1968)' -0.9988 1.0072 O O 'Cromer \& Mann (1968)' 0.0106 0.0060 N N 'Cromer \& Mann (1968)' 0.0061 0.0033 F F 'Cromer \& Mann (1968)' 0.0171 0.0103 H H 'Cromer \& Mann (1968)' 0.0000 0.0000 C C 'Cromer \& Mann (1968)' 0.0033 0.0016 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -3 -4 1 -2 -4 -2 -3 -2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O Pd N1 . . 175.41(14) yes O Pd N2 . . 96.94(13) yes O Pd C11 . . 84.19(13) yes N1 Pd N2 . . 79.60(14) yes N1 Pd C11 . . 99.45(15) yes N2 Pd C11 . . 176.33(18) yes Pd O C18 . . 115.7(3) yes Pd N1 C1 . . 125.5(3) yes Pd N1 C5 . . 115.9(3) yes C1 N1 C5 . . 118.5(4) yes Pd N2 C6 . . 113.9(3) yes Pd N2 C10 . . 127.2(3) yes C6 N2 C10 . . 118.8(3) yes N1 C1 C2 . . 122.7(3) yes C1 C2 C3 . . 118.9(4) no C2 C3 C4 . . 119.0(5) no C3 C4 C5 . . 119.9(4) no N1 C5 C4 . . 121.0(4) yes N1 C5 C6 . . 115.5(3) yes C4 C5 C6 . . 123.4(3) no N2 C6 C5 . . 115.1(3) yes N2 C6 C7 . . 121.6(4) yes C5 C6 C7 . . 123.3(4) no C6 C7 C8 . . 118.9(4) no C7 C8 C9 . . 119.5(4) no C8 C9 C10 . . 119.2(5) no N2 C10 C9 . . 122.0(4) yes Pd C11 C12 . . 111.9(3) yes Pd C11 C16 . . 108.4(3) yes C12 C11 C16 . . 103.2(3) no C11 C12 C13 . . 108.4(4) no C11 C12 C17 . . 102.0(4) no C13 C12 C17 . . 101.2(3) no C12 C13 C14 . . 103.4(4) no C13 C14 C15 . . 102.8(3) no C14 C15 C16 . . 107.0(4) no C14 C15 C17 . . 102.3(5) no C16 C15 C17 . . 101.2(3) no C11 C16 C15 . . 102.6(4) no C11 C16 C18 . . 111.3(3) no C15 C16 C18 . . 110.2(3) no C12 C17 C15 . . 95.0(4) no O C18 C16 . . 120.2(4) yes O C18 C19 . . 118.9(4) yes C16 C18 C19 . . 120.9(4) no N1 C1 H1A . . 118.8(5) no C2 C1 H1A . . 118.5(5) no C1 C2 H2A . . 120.4(5) no C3 C2 H2A . . 120.7(5) no C2 C3 H3A . . 120.4(6) no C4 C3 H3A . . 120.5(5) no C3 C4 H4A . . 120.1(6) no C5 C4 H4A . . 120.0(5) no C6 C7 H7A . . 121.0(5) no C8 C7 H7A . . 120.1(4) no C7 C8 H8A . . 120.5(6) no C9 C8 H8A . . 120.0(6) no C8 C9 H9A . . 120.7(4) no C10 C9 H9A . . 120.1(5) no N2 C10 H10A . . 118.8(4) no C9 C10 H10A . . 119.3(5) no Pd C11 H11A . . 106.9(3) no C12 C11 H11A . . 112.0(5) no C16 C11 H11A . . 114.5(4) no C11 C12 H12A . . 112.4(5) no C13 C12 H12A . . 113.0(5) no C17 C12 H12A . . 118.6(5) no C12 C13 H13A . . 111.0(5) no C12 C13 H13B . . 111.0(5) no C14 C13 H13A . . 110.5(6) no C14 C13 H13B . . 111.4(5) no H13A C13 H13B . . 109.5(7) no C13 C14 H14A . . 111.6(5) no C13 C14 H14B . . 110.6(7) no C15 C14 H14A . . 111.5(7) no C15 C14 H14B . . 110.7(5) no H14A C14 H14B . . 109.5(5) no C14 C15 H15A . . 113.6(4) no C16 C15 H15A . . 112.9(7) no C17 C15 H15A . . 118.4(5) no C11 C16 H16A . . 112.3(3) no C15 C16 H16A . . 113.9(4) no C18 C16 H16A . . 106.5(5) no C12 C17 H17A . . 113.0(5) no C12 C17 H17B . . 113.2(6) no C15 C17 H17A . . 113.3(7) no C15 C17 H17B . . 112.3(4) no H17A C17 H17B . . 109.5(6) no C18 C19 H19A . . 108.8(5) no C18 C19 H19B . . 109.7(5) no C18 C19 H19C . . 109.9(7) no H19A C19 H19B . . 109.5(8) no H19A C19 H19C . . 109.5(7) no H19B C19 H19C . . 109.5(7) no C21 O5 C24 . . 130.3(14) no C21 O5 C21 . 3_666 180.00 no C21 O5 C24 . 3_666 49.7(14) no C21 O5 C24 3_666 . 49.7(14) no C24 O5 C24 . 3_666 180.00 no C21 O5 C24 3_666 3_666 130.3(14) no O5 C21 C22 . . 127(3) no O5 C24 C23 . . 127(3) no O5 C21 H21A . . 109.1(15) no O5 C21 H21B . . 106.3(16) no C22 C21 H21A . . 104(3) no C22 C21 H21B . . 100(2) no H21A C21 H21B . . 109(3) no C21 C22 H22A . . 115(6) no C21 C22 H22B . . 104(4) no C21 C22 H22C . . 110(5) no H22A C22 H22B . . 109(6) no H22A C22 H22C . . 110(6) no H22B C22 H22C . . 109(7) no C24 C23 H23A . . 111(6) no C24 C23 H23B . . 106(3) no C24 C23 H23C . . 112(5) no H23A C23 H23B . . 110(6) no H23A C23 H23C . . 109(4) no H23B C23 H23C . . 109(7) no O5 C24 H24A . . 103.9(17) no O5 C24 H24B . . 106.1(14) no C23 C24 H24A . . 102(2) no C23 C24 H24B . . 108(3) no H24A C24 H24B . . 109(3) no O2 S1 O3 . . 114.3(2) no O2 S1 O4 . . 115.2(2) no O2 S1 C20 . . 103.8(3) no O3 S1 O4 . . 115.0(2) no O3 S1 C20 . . 102.9(3) no O4 S1 C20 . . 103.5(3) no S1 C20 F1 . . 110.5(6) no S1 C20 F2 . . 110.1(5) no S1 C20 F3 . . 110.6(5) no F1 C20 F2 . . 108.2(6) no F1 C20 F3 . . 109.1(6) no F2 C20 F3 . . 108.2(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pd O 2.028(3) yes Pd N1 2.014(4) yes Pd N2 2.100(3) yes Pd C11 2.019(3) yes O C18 1.235(5) yes N1 C1 1.345(6) yes N1 C5 1.366(5) yes N2 C6 1.348(5) yes N2 C10 1.347(6) yes C1 C2 1.382(7) no C2 C3 1.379(6) no C3 C4 1.387(7) no C4 C5 1.381(6) no C5 C6 1.474(5) yes C6 C7 1.386(5) no C7 C8 1.384(7) no C8 C9 1.369(7) no C9 C10 1.380(5) no C11 C12 1.517(7) no C11 C16 1.564(5) yes C12 C13 1.542(5) no C12 C17 1.519(6) no C13 C14 1.554(8) no C14 C15 1.529(6) no C15 C16 1.548(7) no C15 C17 1.531(8) no C16 C18 1.493(6) yes C18 C19 1.492(8) yes C1 H1A 0.980(5) no C2 H2A 0.980(7) no C3 H3A 0.981(7) no C4 H4A 0.980(6) no C7 H7A 0.980(7) no C8 H8A 0.979(6) no C9 H9A 0.980(7) no C10 H10A 0.980(7) no C11 H11A 0.980(4) no C12 H12A 0.979(7) no C13 H13A 0.980(6) no C13 H13B 0.980(9) no C14 H14A 0.981(8) no C14 H14B 0.981(7) no C15 H15A 0.980(7) no C16 H16A 0.981(6) no C17 H17A 0.980(5) no C17 H17B 0.980(9) no C19 H19A 0.979(8) no C19 H19B 0.980(9) no C19 H19C 0.981(7) no O5 C21 1.358(17) yes O5 C24 1.336(16) yes C21 C22 1.31(5) no C23 C24 1.28(5) no C21 H21A 0.98(3) no C21 H21B 0.98(2) no C22 H22A 0.98(7) no C22 H22B 0.99(7) no C22 H22C 0.98(7) no C23 H23A 0.98(6) no C23 H23B 0.98(7) no C23 H23C 0.99(6) no C24 H24A 0.98(3) no C24 H24B 0.98(3) no S1 O2 1.440(3) yes S1 O3 1.431(4) yes S1 O4 1.429(3) yes S1 C20 1.820(9) yes F1 C20 1.333(8) yes F2 C20 1.340(8) yes F3 C20 1.313(10) yes 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag N2 Pd O C18 . -179.6(4) no C11 Pd O C18 . -3.1(4) no N2 Pd N1 C1 . -175.7(5) no N2 Pd N1 C5 . 0.6(3) no C11 Pd N1 C1 . 7.9(4) no C11 Pd N1 C5 . -175.8(3) no O Pd N2 C6 . -178.3(3) no O Pd N2 C10 . 3.7(4) no N1 Pd N2 C6 . -1.3(3) no N1 Pd N2 C10 . -179.3(5) no O Pd C11 C12 . -111.9(3) no O Pd C11 C16 . 1.3(3) no N1 Pd C11 C12 . 71.0(3) no N1 Pd C11 C16 . -175.9(3) no Pd O C18 C16 . 4.1(6) no Pd O C18 C19 . -176.7(4) no Pd N1 C1 C2 . 175.8(4) no C5 N1 C1 C2 . -0.4(7) no Pd N1 C5 C4 . -176.9(4) no Pd N1 C5 C6 . 0.2(6) no C1 N1 C5 C4 . -0.3(7) no C1 N1 C5 C6 . 176.7(4) no Pd N2 C6 C5 . 1.8(5) no Pd N2 C6 C7 . -178.0(4) no C10 N2 C6 C5 . 179.9(7) no C10 N2 C6 C7 . 0.2(7) no Pd N2 C10 C9 . 178.4(4) no C6 N2 C10 C9 . 0.5(8) no N1 C1 C2 C3 . 0.8(8) no C1 C2 C3 C4 . -0.5(8) no C2 C3 C4 C5 . -0.2(9) no C3 C4 C5 N1 . 0.6(8) no C3 C4 C5 C6 . -176.1(5) no N1 C5 C6 N2 . -1.3(6) no N1 C5 C6 C7 . 178.5(5) no C4 C5 C6 N2 . 175.6(4) no C4 C5 C6 C7 . -4.6(7) no N2 C6 C7 C8 . -0.5(8) no C5 C6 C7 C8 . 179.8(6) no C6 C7 C8 C9 . 0.1(13) no C7 C8 C9 C10 . 0.6(9) no C8 C9 C10 N2 . -0.9(9) no Pd C11 C12 C13 . -173.5(3) no Pd C11 C12 C17 . 80.2(3) no C16 C11 C12 C13 . 70.1(4) no C16 C11 C12 C17 . -36.2(3) no Pd C11 C16 C15 . -117.7(3) no Pd C11 C16 C18 . 0.2(5) no C12 C11 C16 C15 . 1.1(3) no C12 C11 C16 C18 . 119.0(4) no C11 C12 C13 C14 . -71.1(5) no C17 C12 C13 C14 . 35.7(6) no C11 C12 C17 C15 . 56.5(4) no C13 C12 C17 C15 . -55.3(5) no C12 C13 C14 C15 . -1.1(5) no C13 C14 C15 C16 . 72.2(5) no C13 C14 C15 C17 . -33.8(5) no C14 C15 C16 C11 . -72.9(4) no C14 C15 C16 C18 . 168.4(4) no C17 C15 C16 C11 . 33.9(4) no C17 C15 C16 C18 . -84.8(4) no C14 C15 C17 C12 . 55.2(4) no C16 C15 C17 C12 . -55.2(4) no C11 C16 C18 O . -2.9(6) no C11 C16 C18 C19 . 178.0(4) no C15 C16 C18 O . 110.4(5) no C15 C16 C18 C19 . -68.7(6) no C24 O5 C21 C22 . -172(3) no C24 O5 C21 C22 3_666 8(3) no C21 O5 C24 C23 . 174(2) no C21 O5 C24 C23 3_666 -6(2) no O2 S1 C20 F1 . 57.7(5) no O3 S1 C20 F1 . -61.7(5) no O4 S1 C20 F1 . 178.3(4) no O2 S1 C20 F2 . 177.2(5) no O3 S1 C20 F2 . 57.8(6) no O4 S1 C20 F2 . -62.2(6) no O2 S1 C20 F3 . -63.3(5) no O3 S1 C20 F3 . 177.3(4) no O4 S1 C20 F3 . 57.3(5) no