# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Daniela Pucci' _publ_contact_author_email D.PUCCI@UNICAL.IT _publ_section_title ; Unsuspected mesomorphism in "tail-free" cyclopalladated 3,5-disubstituted-2,2'-pyridylpyrroles ; loop_ _publ_author_name 'Daniela Pucci' 'Iolinda Aiello' 'Alessia Aprea' 'Anna Bellusci' 'Alessandra Crispini' 'Mauro Ghedini' # Attachment 'acrispinirevised.CIF' data_(3) _database_code_depnum_ccdc_archive 'CCDC 706172' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H18 N2 O2 Pd' _chemical_formula_sum 'C16 H18 N2 O2 Pd' _chemical_formula_weight 376.72 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 17.4226(13) _cell_length_b 12.8899(10) _cell_length_c 14.4266(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.117(3) _cell_angle_gamma 90.00 _cell_volume 3112.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5626 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31117 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7682 _reflns_number_gt 5626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+1.4078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7682 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.470659(16) 0.89455(2) 0.380235(19) 0.04437(9) Uani 1 1 d . . . Pd2 Pd 0.003451(15) 0.58791(2) 0.097017(18) 0.04352(9) Uani 1 1 d . . . O1 O 0.57231(14) 0.97374(19) 0.42652(17) 0.0570(6) Uani 1 1 d . . . O2 O 0.42866(14) 0.99106(18) 0.26883(16) 0.0548(6) Uani 1 1 d . . . O3 O 0.10906(14) 0.51530(18) 0.13195(17) 0.0565(6) Uani 1 1 d . . . O4 O -0.03935(15) 0.49863(18) 0.18421(17) 0.0563(6) Uani 1 1 d . . . N1 N 0.50664(16) 0.7945(2) 0.49095(19) 0.0452(6) Uani 1 1 d . . . N2 N 0.37774(16) 0.7979(2) 0.34784(19) 0.0453(6) Uani 1 1 d . . . N3 N 0.03957(16) 0.6864(2) 0.01026(18) 0.0458(6) Uani 1 1 d . . . N4 N -0.09488(16) 0.6742(2) 0.05422(19) 0.0458(6) Uani 1 1 d . . . C1 C 0.5758(2) 0.8028(3) 0.5607(3) 0.0557(9) Uani 1 1 d . . . H1A H 0.6094 0.8585 0.5594 0.067 Uiso 1 1 calc R . . C2 C 0.5983(2) 0.7317(3) 0.6335(3) 0.0661(11) Uani 1 1 d . . . H2A H 0.6469 0.7382 0.6805 0.079 Uiso 1 1 calc R . . C3 C 0.5478(3) 0.6505(4) 0.6363(3) 0.0702(12) Uani 1 1 d . . . H3A H 0.5620 0.6018 0.6857 0.084 Uiso 1 1 calc R . . C4 C 0.4766(2) 0.6412(3) 0.5662(3) 0.0618(10) Uani 1 1 d . . . H4A H 0.4422 0.5866 0.5682 0.074 Uiso 1 1 calc R . . C5 C 0.4558(2) 0.7146(3) 0.4915(2) 0.0465(8) Uani 1 1 d . . . C6 C 0.3853(2) 0.7149(2) 0.4116(2) 0.0438(7) Uani 1 1 d . . . C7 C 0.3195(2) 0.6494(3) 0.3808(2) 0.0482(8) Uani 1 1 d . . . C8 C 0.2717(2) 0.6935(3) 0.2956(2) 0.0491(8) Uani 1 1 d . . . H8A H 0.2238 0.6668 0.2574 0.059 Uiso 1 1 calc R . . C9 C 0.3088(2) 0.7849(3) 0.2782(2) 0.0486(8) Uani 1 1 d . . . C10 C 0.3014(3) 0.5511(3) 0.4272(3) 0.0660(11) Uani 1 1 d . . . H10A H 0.3462 0.5048 0.4380 0.099 Uiso 1 1 calc R . . H10B H 0.2550 0.5185 0.3854 0.099 Uiso 1 1 calc R . . H10C H 0.2913 0.5674 0.4877 0.099 Uiso 1 1 calc R . . C11 C 0.2798(2) 0.8586(3) 0.1958(3) 0.0700(11) Uani 1 1 d . . . H11A H 0.3166 0.9153 0.2026 0.105 Uiso 1 1 calc R . . H11B H 0.2281 0.8847 0.1957 0.105 Uiso 1 1 calc R . . H11C H 0.2759 0.8231 0.1362 0.105 Uiso 1 1 calc R . . C12 C 0.6731(2) 1.0951(3) 0.4302(3) 0.0716(12) Uani 1 1 d . . . H12A H 0.7047 1.0435 0.4717 0.107 Uiso 1 1 calc R . . H12B H 0.6681 1.1550 0.4676 0.107 Uiso 1 1 calc R . . H12C H 0.6987 1.1144 0.3818 0.107 Uiso 1 1 calc R . . C13 C 0.5919(2) 1.0520(3) 0.3827(3) 0.0528(9) Uani 1 1 d . . . C14 C 0.5448(2) 1.0959(3) 0.2990(3) 0.0571(10) Uani 1 1 d . . . H14A H 0.5671 1.1507 0.2735 0.068 Uiso 1 1 calc R . . C15 C 0.4684(2) 1.0674(3) 0.2493(2) 0.0524(9) Uani 1 1 d . . . C16 C 0.4240(3) 1.1287(3) 0.1619(3) 0.0725(12) Uani 1 1 d . . . H16A H 0.3684 1.1319 0.1593 0.109 Uiso 1 1 calc R . . H16B H 0.4299 1.0955 0.1047 0.109 Uiso 1 1 calc R . . H16C H 0.4455 1.1977 0.1661 0.109 Uiso 1 1 calc R . . C17 C 0.1106(2) 0.6825(3) -0.0078(3) 0.0590(10) Uani 1 1 d . . . H17A H 0.1456 0.6291 0.0193 0.071 Uiso 1 1 calc R . . C18 C 0.1340(3) 0.7544(4) -0.0650(3) 0.0733(12) Uani 1 1 d . . . H18A H 0.1843 0.7510 -0.0755 0.088 Uiso 1 1 calc R . . C19 C 0.0810(3) 0.8314(3) -0.1061(3) 0.0711(11) Uani 1 1 d . . . H19A H 0.0949 0.8806 -0.1456 0.085 Uiso 1 1 calc R . . C20 C 0.0078(3) 0.8357(3) -0.0891(3) 0.0624(10) Uani 1 1 d . . . H20A H -0.0280 0.8878 -0.1174 0.075 Uiso 1 1 calc R . . C21 C -0.0138(2) 0.7624(3) -0.0295(2) 0.0464(8) Uani 1 1 d . . . C22 C -0.0874(2) 0.7568(3) -0.0038(2) 0.0449(8) Uani 1 1 d . . . C23 C -0.1560(2) 0.8183(3) -0.0225(2) 0.0534(9) Uani 1 1 d . . . C24 C -0.2057(2) 0.7697(3) 0.0246(2) 0.0578(9) Uani 1 1 d . . . H24A H -0.2563 0.7923 0.0249 0.069 Uiso 1 1 calc R . . C25 C -0.1674(2) 0.6817(3) 0.0713(2) 0.0504(8) Uani 1 1 d . . . C26 C -0.1732(3) 0.9175(3) -0.0791(3) 0.0790(14) Uani 1 1 d . . . H26A H -0.1288 0.9344 -0.1036 0.118 Uiso 1 1 calc R . . H26B H -0.1813 0.9725 -0.0380 0.118 Uiso 1 1 calc R . . H26C H -0.2203 0.9091 -0.1320 0.118 Uiso 1 1 calc R . . C27 C -0.1970(3) 0.6062(3) 0.1317(3) 0.0750(12) Uani 1 1 d . . . H27A H -0.1578 0.5527 0.1538 0.113 Uiso 1 1 calc R . . H27B H -0.2460 0.5757 0.0940 0.113 Uiso 1 1 calc R . . H27C H -0.2062 0.6415 0.1862 0.113 Uiso 1 1 calc R . . C28 C 0.2083(3) 0.3937(3) 0.2008(3) 0.0763(13) Uani 1 1 d . . . H28A H 0.2472 0.4483 0.2176 0.114 Uiso 1 1 calc R . . H28B H 0.2103 0.3626 0.1410 0.114 Uiso 1 1 calc R . . H28C H 0.2198 0.3421 0.2507 0.114 Uiso 1 1 calc R . . C29 C 0.1263(2) 0.4377(3) 0.1899(3) 0.0568(10) Uani 1 1 d . . . C30 C 0.0767(3) 0.3945(3) 0.2394(3) 0.0625(11) Uani 1 1 d . . . H30A H 0.0971 0.3388 0.2796 0.075 Uiso 1 1 calc R . . C31 C -0.0006(3) 0.4256(3) 0.2354(3) 0.0591(10) Uani 1 1 d . . . C32 C -0.0466(3) 0.3704(3) 0.2955(3) 0.0811(14) Uani 1 1 d . . . H32A H -0.1023 0.3688 0.2610 0.122 Uiso 1 1 calc R . . H32B H -0.0397 0.4065 0.3555 0.122 Uiso 1 1 calc R . . H32C H -0.0271 0.3007 0.3082 0.122 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04881(16) 0.03812(15) 0.04986(15) 0.00354(11) 0.01981(12) -0.00161(11) Pd2 0.04289(15) 0.03942(16) 0.04413(15) 0.00264(10) 0.00521(11) 0.00280(11) O1 0.0565(15) 0.0525(15) 0.0637(15) 0.0039(12) 0.0196(12) -0.0075(12) O2 0.0646(15) 0.0451(14) 0.0541(13) 0.0092(11) 0.0154(12) -0.0100(12) O3 0.0521(14) 0.0475(14) 0.0632(15) 0.0051(12) 0.0047(12) 0.0085(11) O4 0.0598(14) 0.0495(14) 0.0588(14) 0.0182(12) 0.0148(12) 0.0050(12) N1 0.0480(15) 0.0404(15) 0.0514(15) 0.0040(12) 0.0208(13) 0.0039(12) N2 0.0488(15) 0.0407(16) 0.0484(15) 0.0024(12) 0.0170(13) -0.0014(12) N3 0.0469(15) 0.0454(16) 0.0440(14) -0.0001(12) 0.0108(12) -0.0001(13) N4 0.0433(15) 0.0440(16) 0.0468(15) 0.0049(12) 0.0069(12) 0.0025(12) C1 0.0449(19) 0.062(2) 0.061(2) 0.0038(18) 0.0149(17) 0.0024(17) C2 0.050(2) 0.082(3) 0.063(2) 0.016(2) 0.0088(18) 0.015(2) C3 0.071(3) 0.075(3) 0.066(2) 0.028(2) 0.021(2) 0.011(2) C4 0.064(2) 0.056(2) 0.066(2) 0.0199(19) 0.019(2) -0.0013(19) C5 0.0527(19) 0.0410(19) 0.0520(18) 0.0044(15) 0.0248(16) 0.0031(15) C6 0.0515(19) 0.0368(18) 0.0474(17) 0.0043(14) 0.0209(15) -0.0008(15) C7 0.057(2) 0.0408(19) 0.0547(19) 0.0004(15) 0.0280(17) -0.0009(16) C8 0.0497(19) 0.047(2) 0.0541(19) -0.0008(16) 0.0199(16) -0.0047(16) C9 0.0499(19) 0.050(2) 0.0489(18) 0.0008(16) 0.0191(16) 0.0021(16) C10 0.083(3) 0.050(2) 0.071(2) 0.0052(19) 0.032(2) -0.013(2) C11 0.068(3) 0.065(3) 0.065(2) 0.018(2) 0.000(2) -0.003(2) C12 0.057(2) 0.075(3) 0.086(3) -0.002(2) 0.027(2) -0.017(2) C13 0.056(2) 0.047(2) 0.065(2) -0.0069(18) 0.0335(19) -0.0090(17) C14 0.068(2) 0.046(2) 0.064(2) 0.0043(17) 0.031(2) -0.0107(18) C15 0.074(3) 0.0392(19) 0.0491(19) 0.0005(15) 0.0262(19) -0.0058(18) C16 0.099(3) 0.057(3) 0.060(2) 0.014(2) 0.020(2) -0.015(2) C17 0.049(2) 0.063(2) 0.066(2) 0.0056(19) 0.0168(18) 0.0056(18) C18 0.060(2) 0.090(3) 0.078(3) 0.009(2) 0.031(2) -0.006(2) C19 0.078(3) 0.069(3) 0.072(3) 0.015(2) 0.029(2) -0.008(2) C20 0.070(3) 0.059(3) 0.058(2) 0.0122(19) 0.018(2) 0.005(2) C21 0.0534(19) 0.0426(19) 0.0394(17) 0.0024(14) 0.0065(15) -0.0020(15) C22 0.0473(18) 0.0452(19) 0.0396(16) 0.0050(14) 0.0076(14) 0.0047(15) C23 0.060(2) 0.053(2) 0.0453(18) 0.0064(16) 0.0101(16) 0.0164(18) C24 0.052(2) 0.068(3) 0.054(2) 0.0017(18) 0.0154(17) 0.0185(19) C25 0.0448(18) 0.057(2) 0.0493(19) 0.0015(16) 0.0125(15) 0.0032(16) C26 0.091(3) 0.067(3) 0.083(3) 0.026(2) 0.031(3) 0.036(2) C27 0.057(2) 0.091(3) 0.082(3) 0.022(2) 0.028(2) 0.001(2) C28 0.067(3) 0.072(3) 0.078(3) -0.003(2) 0.000(2) 0.027(2) C29 0.059(2) 0.045(2) 0.053(2) -0.0060(17) -0.0069(18) 0.0121(17) C30 0.078(3) 0.047(2) 0.055(2) 0.0107(17) 0.005(2) 0.013(2) C31 0.078(3) 0.044(2) 0.050(2) 0.0034(16) 0.0102(19) 0.0066(19) C32 0.114(4) 0.067(3) 0.070(3) 0.026(2) 0.037(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1 1.992(2) . ? Pd1 N2 1.993(3) . ? Pd1 O2 2.003(2) . ? Pd1 N1 2.013(3) . ? Pd2 N4 1.992(3) . ? Pd2 O4 1.996(2) . ? Pd2 O3 2.000(2) . ? Pd2 N3 2.003(3) . ? O1 C13 1.286(4) . ? O2 C15 1.278(4) . ? O3 C29 1.284(4) . ? O4 C31 1.269(4) . ? N1 C1 1.342(4) . ? N1 C5 1.359(4) . ? N2 C9 1.346(4) . ? N2 C6 1.394(4) . ? N3 C17 1.335(4) . ? N3 C21 1.362(4) . ? N4 C25 1.355(4) . ? N4 C22 1.383(4) . ? C1 C2 1.368(5) . ? C2 C3 1.375(6) . ? C3 C4 1.371(6) . ? C4 C5 1.405(5) . ? C5 C6 1.431(5) . ? C6 C7 1.393(5) . ? C7 C8 1.399(5) . ? C7 C10 1.507(5) . ? C8 C9 1.399(5) . ? C9 C11 1.496(5) . ? C12 C13 1.498(5) . ? C13 C14 1.378(5) . ? C14 C15 1.375(5) . ? C15 C16 1.507(5) . ? C17 C18 1.375(5) . ? C18 C19 1.373(6) . ? C19 C20 1.365(6) . ? C20 C21 1.397(5) . ? C21 C22 1.433(5) . ? C22 C23 1.396(5) . ? C23 C24 1.391(5) . ? C23 C26 1.502(5) . ? C24 C25 1.391(5) . ? C25 C27 1.491(5) . ? C28 C29 1.505(5) . ? C29 C30 1.382(6) . ? C30 C31 1.391(6) . ? C31 C32 1.512(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd1 N2 171.03(10) . . ? O1 Pd1 O2 92.49(10) . . ? N2 Pd1 O2 96.21(10) . . ? O1 Pd1 N1 90.58(11) . . ? N2 Pd1 N1 80.75(11) . . ? O2 Pd1 N1 176.81(10) . . ? N4 Pd2 O4 94.46(11) . . ? N4 Pd2 O3 172.51(11) . . ? O4 Pd2 O3 92.86(10) . . ? N4 Pd2 N3 81.06(11) . . ? O4 Pd2 N3 175.19(11) . . ? O3 Pd2 N3 91.58(11) . . ? C13 O1 Pd1 124.7(2) . . ? C15 O2 Pd1 123.7(2) . . ? C29 O3 Pd2 124.1(3) . . ? C31 O4 Pd2 124.3(3) . . ? C1 N1 C5 120.5(3) . . ? C1 N1 Pd1 124.1(2) . . ? C5 N1 Pd1 115.4(2) . . ? C9 N2 C6 107.4(3) . . ? C9 N2 Pd1 138.7(2) . . ? C6 N2 Pd1 113.8(2) . . ? C17 N3 C21 120.4(3) . . ? C17 N3 Pd2 124.6(2) . . ? C21 N3 Pd2 115.0(2) . . ? C25 N4 C22 107.7(3) . . ? C25 N4 Pd2 138.4(2) . . ? C22 N4 Pd2 113.6(2) . . ? N1 C1 C2 121.9(4) . . ? C1 C2 C3 118.9(4) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 119.6(4) . . ? N1 C5 C4 119.0(3) . . ? N1 C5 C6 114.1(3) . . ? C4 C5 C6 126.8(3) . . ? C7 C6 N2 109.6(3) . . ? C7 C6 C5 134.6(3) . . ? N2 C6 C5 115.8(3) . . ? C6 C7 C8 105.7(3) . . ? C6 C7 C10 128.5(3) . . ? C8 C7 C10 125.8(3) . . ? C7 C8 C9 108.0(3) . . ? N2 C9 C8 109.3(3) . . ? N2 C9 C11 123.3(3) . . ? C8 C9 C11 127.4(3) . . ? O1 C13 C14 125.3(3) . . ? O1 C13 C12 114.3(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 127.0(3) . . ? O2 C15 C14 126.6(3) . . ? O2 C15 C16 113.9(3) . . ? C14 C15 C16 119.6(3) . . ? N3 C17 C18 122.5(4) . . ? C19 C18 C17 118.0(4) . . ? C20 C19 C18 120.1(4) . . ? C19 C20 C21 120.5(4) . . ? N3 C21 C20 118.5(3) . . ? N3 C21 C22 114.2(3) . . ? C20 C21 C22 127.3(3) . . ? N4 C22 C23 109.6(3) . . ? N4 C22 C21 115.9(3) . . ? C23 C22 C21 134.5(3) . . ? C24 C23 C22 105.4(3) . . ? C24 C23 C26 126.3(3) . . ? C22 C23 C26 128.3(4) . . ? C23 C24 C25 108.8(3) . . ? N4 C25 C24 108.5(3) . . ? N4 C25 C27 123.4(3) . . ? C24 C25 C27 128.1(3) . . ? O3 C29 C30 125.7(3) . . ? O3 C29 C28 113.9(4) . . ? C30 C29 C28 120.4(4) . . ? C29 C30 C31 126.9(3) . . ? O4 C31 C30 126.2(4) . . ? O4 C31 C32 113.7(4) . . ? C30 C31 C32 120.1(4) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 O1 C13 161.5(6) . . . . ? O2 Pd1 O1 C13 -4.3(3) . . . . ? N1 Pd1 O1 C13 176.6(3) . . . . ? O1 Pd1 O2 C15 2.9(3) . . . . ? N2 Pd1 O2 C15 -174.9(3) . . . . ? N1 Pd1 O2 C15 167.7(18) . . . . ? N4 Pd2 O3 C29 169.7(7) . . . . ? O4 Pd2 O3 C29 2.1(3) . . . . ? N3 Pd2 O3 C29 -179.8(3) . . . . ? N4 Pd2 O4 C31 -179.0(3) . . . . ? O3 Pd2 O4 C31 -0.6(3) . . . . ? N3 Pd2 O4 C31 -158.0(11) . . . . ? O1 Pd1 N1 C1 2.4(3) . . . . ? N2 Pd1 N1 C1 -179.9(3) . . . . ? O2 Pd1 N1 C1 -162.4(18) . . . . ? O1 Pd1 N1 C5 -177.2(2) . . . . ? N2 Pd1 N1 C5 0.5(2) . . . . ? O2 Pd1 N1 C5 18(2) . . . . ? O1 Pd1 N2 C9 -162.4(6) . . . . ? O2 Pd1 N2 C9 3.3(4) . . . . ? N1 Pd1 N2 C9 -177.6(4) . . . . ? O1 Pd1 N2 C6 13.5(8) . . . . ? O2 Pd1 N2 C6 179.3(2) . . . . ? N1 Pd1 N2 C6 -1.7(2) . . . . ? N4 Pd2 N3 C17 -178.4(3) . . . . ? O4 Pd2 N3 C17 160.4(11) . . . . ? O3 Pd2 N3 C17 3.0(3) . . . . ? N4 Pd2 N3 C21 3.0(2) . . . . ? O4 Pd2 N3 C21 -18.2(13) . . . . ? O3 Pd2 N3 C21 -175.6(2) . . . . ? O4 Pd2 N4 C25 1.1(4) . . . . ? O3 Pd2 N4 C25 -166.5(7) . . . . ? N3 Pd2 N4 C25 -177.2(4) . . . . ? O4 Pd2 N4 C22 174.2(2) . . . . ? O3 Pd2 N4 C22 6.6(9) . . . . ? N3 Pd2 N4 C22 -4.1(2) . . . . ? C5 N1 C1 C2 0.8(5) . . . . ? Pd1 N1 C1 C2 -178.8(3) . . . . ? N1 C1 C2 C3 -1.2(6) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C1 N1 C5 C4 0.3(5) . . . . ? Pd1 N1 C5 C4 179.9(3) . . . . ? C1 N1 C5 C6 -178.8(3) . . . . ? Pd1 N1 C5 C6 0.8(4) . . . . ? C3 C4 C5 N1 -0.9(6) . . . . ? C3 C4 C5 C6 178.1(4) . . . . ? C9 N2 C6 C7 -0.1(4) . . . . ? Pd1 N2 C6 C7 -177.3(2) . . . . ? C9 N2 C6 C5 179.8(3) . . . . ? Pd1 N2 C6 C5 2.7(4) . . . . ? N1 C5 C6 C7 177.7(4) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? N1 C5 C6 N2 -2.3(4) . . . . ? C4 C5 C6 N2 178.7(3) . . . . ? N2 C6 C7 C8 0.7(4) . . . . ? C5 C6 C7 C8 -179.2(4) . . . . ? N2 C6 C7 C10 -179.2(3) . . . . ? C5 C6 C7 C10 0.8(7) . . . . ? C6 C7 C8 C9 -1.1(4) . . . . ? C10 C7 C8 C9 178.9(3) . . . . ? C6 N2 C9 C8 -0.5(4) . . . . ? Pd1 N2 C9 C8 175.5(3) . . . . ? C6 N2 C9 C11 -179.8(3) . . . . ? Pd1 N2 C9 C11 -3.7(6) . . . . ? C7 C8 C9 N2 1.0(4) . . . . ? C7 C8 C9 C11 -179.8(4) . . . . ? Pd1 O1 C13 C14 2.5(5) . . . . ? Pd1 O1 C13 C12 -177.5(2) . . . . ? O1 C13 C14 C15 2.5(6) . . . . ? C12 C13 C14 C15 -177.6(4) . . . . ? Pd1 O2 C15 C14 0.4(5) . . . . ? Pd1 O2 C15 C16 180.0(2) . . . . ? C13 C14 C15 O2 -4.1(7) . . . . ? C13 C14 C15 C16 176.3(4) . . . . ? C21 N3 C17 C18 1.2(5) . . . . ? Pd2 N3 C17 C18 -177.4(3) . . . . ? N3 C17 C18 C19 -1.4(6) . . . . ? C17 C18 C19 C20 0.7(7) . . . . ? C18 C19 C20 C21 0.3(6) . . . . ? C17 N3 C21 C20 -0.2(5) . . . . ? Pd2 N3 C21 C20 178.5(3) . . . . ? C17 N3 C21 C22 180.0(3) . . . . ? Pd2 N3 C21 C22 -1.4(3) . . . . ? C19 C20 C21 N3 -0.6(5) . . . . ? C19 C20 C21 C22 179.3(4) . . . . ? C25 N4 C22 C23 0.8(4) . . . . ? Pd2 N4 C22 C23 -174.4(2) . . . . ? C25 N4 C22 C21 179.8(3) . . . . ? Pd2 N4 C22 C21 4.6(4) . . . . ? N3 C21 C22 N4 -2.1(4) . . . . ? C20 C21 C22 N4 178.0(3) . . . . ? N3 C21 C22 C23 176.5(3) . . . . ? C20 C21 C22 C23 -3.4(6) . . . . ? N4 C22 C23 C24 -0.8(4) . . . . ? C21 C22 C23 C24 -179.5(4) . . . . ? N4 C22 C23 C26 177.7(4) . . . . ? C21 C22 C23 C26 -1.0(7) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C26 C23 C24 C25 -178.0(4) . . . . ? C22 N4 C25 C24 -0.5(4) . . . . ? Pd2 N4 C25 C24 172.9(3) . . . . ? C22 N4 C25 C27 -179.8(3) . . . . ? Pd2 N4 C25 C27 -6.4(6) . . . . ? C23 C24 C25 N4 -0.1(4) . . . . ? C23 C24 C25 C27 179.2(4) . . . . ? Pd2 O3 C29 C30 -2.3(5) . . . . ? Pd2 O3 C29 C28 177.3(2) . . . . ? O3 C29 C30 C31 0.7(6) . . . . ? C28 C29 C30 C31 -178.9(4) . . . . ? Pd2 O4 C31 C30 -0.6(5) . . . . ? Pd2 O4 C31 C32 179.7(3) . . . . ? C29 C30 C31 O4 1.0(7) . . . . ? C29 C30 C31 C32 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.102 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.078 #===END data_(4) _database_code_depnum_ccdc_archive 'CCDC 706173' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H12 F6 N2 O2 Pd' _chemical_formula_sum 'C16 H12 F6 N2 O2 Pd' _chemical_formula_weight 484.68 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1129(13) _cell_length_b 11.095(2) _cell_length_c 11.9915(18) _cell_angle_alpha 67.327(4) _cell_angle_beta 87.256(5) _cell_angle_gamma 81.884(5) _cell_volume 864.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2695 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11528 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3463 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.1797P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3463 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.74507(4) 0.52339(3) 0.53041(2) 0.04136(11) Uani 1 1 d . . . F1 F 0.6818(5) 0.1420(3) 1.0253(2) 0.1069(10) Uani 1 1 d . . . F2 F 0.9803(4) 0.1482(3) 1.0139(2) 0.1010(9) Uani 1 1 d . . . F3 F 0.8080(5) 0.2487(3) 1.1104(2) 0.1188(12) Uani 1 1 d . . . F4 F 0.6844(5) 0.7370(2) 0.8352(2) 0.0954(9) Uani 1 1 d . . . F5 F 0.8344(4) 0.7625(2) 0.6699(2) 0.0831(8) Uani 1 1 d . . . F6 F 0.5352(4) 0.7532(2) 0.6784(2) 0.0836(8) Uani 1 1 d . . . O1 O 0.7435(4) 0.5275(3) 0.3648(2) 0.0549(6) Uani 1 1 d . . . O2 O 0.7023(4) 0.7174(2) 0.4748(2) 0.0530(6) Uani 1 1 d . . . N1 N 0.7890(4) 0.3267(3) 0.5967(3) 0.0430(7) Uani 1 1 d . . . N2 N 0.7508(4) 0.4877(3) 0.7076(2) 0.0409(7) Uani 1 1 d . . . C1 C 0.8027(5) 0.2547(4) 0.5284(4) 0.0605(11) Uani 1 1 d . . . H1A H 0.7919 0.2973 0.4449 0.073 Uiso 1 1 calc R . . C2 C 0.8325(6) 0.1194(4) 0.5787(5) 0.0719(13) Uani 1 1 d . . . H2A H 0.8415 0.0710 0.5299 0.086 Uiso 1 1 calc R . . C3 C 0.8487(6) 0.0571(4) 0.7011(5) 0.0691(12) Uani 1 1 d . . . H3A H 0.8690 -0.0345 0.7364 0.083 Uiso 1 1 calc R . . C4 C 0.8349(5) 0.1299(4) 0.7723(4) 0.0585(10) Uani 1 1 d . . . H4A H 0.8469 0.0880 0.8559 0.070 Uiso 1 1 calc R . . C5 C 0.8030(4) 0.2659(3) 0.7186(3) 0.0438(8) Uani 1 1 d . . . C6 C 0.7823(5) 0.3567(3) 0.7798(3) 0.0430(8) Uani 1 1 d . . . C7 C 0.7833(5) 0.3426(4) 0.9002(3) 0.0504(9) Uani 1 1 d . . . C8 C 0.7525(5) 0.4688(4) 0.9009(3) 0.0546(10) Uani 1 1 d . . . H8A H 0.7459 0.4904 0.9687 0.066 Uiso 1 1 calc R . . C9 C 0.7337(5) 0.5556(3) 0.7825(3) 0.0448(8) Uani 1 1 d . . . C10 C 0.8115(8) 0.2214(5) 1.0108(4) 0.0757(13) Uani 1 1 d . . . C11 C 0.6971(7) 0.7013(4) 0.7395(4) 0.0612(11) Uani 1 1 d . . . C12 C 0.7224(6) 0.6064(5) 0.1548(3) 0.0762(14) Uani 1 1 d . . . H12A H 0.8427 0.5583 0.1480 0.114 Uiso 1 1 calc R . . H12B H 0.7038 0.6887 0.0865 0.114 Uiso 1 1 calc R . . H12C H 0.6226 0.5557 0.1567 0.114 Uiso 1 1 calc R . . C13 C 0.7192(5) 0.6322(5) 0.2694(3) 0.0531(10) Uani 1 1 d . . . C14 C 0.6875(5) 0.7594(4) 0.2663(3) 0.0563(10) Uani 1 1 d . . . H14A H 0.6682 0.8270 0.1905 0.068 Uiso 1 1 calc R . . C15 C 0.6816(5) 0.7966(4) 0.3649(3) 0.0492(9) Uani 1 1 d . . . C16 C 0.6484(6) 0.9385(4) 0.3469(4) 0.0674(12) Uani 1 1 d . . . H16A H 0.5598 0.9504 0.4059 0.101 Uiso 1 1 calc R . . H16B H 0.5976 0.9898 0.2673 0.101 Uiso 1 1 calc R . . H16C H 0.7663 0.9667 0.3558 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.04513(17) 0.03938(17) 0.04055(16) -0.01675(12) -0.00191(11) -0.00375(11) F1 0.140(3) 0.0718(19) 0.083(2) 0.0056(15) 0.0124(18) -0.0388(19) F2 0.116(2) 0.0680(18) 0.0843(19) 0.0007(14) -0.0330(16) 0.0220(16) F3 0.204(4) 0.089(2) 0.0448(15) -0.0085(15) -0.0136(17) -0.005(2) F4 0.175(3) 0.0606(16) 0.0623(16) -0.0384(13) 0.0088(16) -0.0117(16) F5 0.129(2) 0.0576(15) 0.0730(16) -0.0267(13) 0.0137(15) -0.0428(15) F6 0.105(2) 0.0580(15) 0.0778(17) -0.0264(13) -0.0091(15) 0.0263(14) O1 0.0654(17) 0.0561(17) 0.0465(15) -0.0242(13) -0.0016(12) -0.0049(13) O2 0.0706(17) 0.0431(15) 0.0400(14) -0.0110(12) -0.0011(12) -0.0051(12) N1 0.0409(16) 0.0440(18) 0.0514(18) -0.0261(15) -0.0009(13) -0.0054(13) N2 0.0448(16) 0.0381(16) 0.0414(16) -0.0168(14) -0.0009(13) -0.0054(13) C1 0.056(2) 0.064(3) 0.076(3) -0.044(2) 0.001(2) -0.006(2) C2 0.074(3) 0.054(3) 0.107(4) -0.053(3) -0.009(3) -0.001(2) C3 0.065(3) 0.041(2) 0.107(4) -0.035(3) -0.016(2) -0.001(2) C4 0.055(2) 0.041(2) 0.077(3) -0.019(2) -0.015(2) -0.0034(18) C5 0.0346(18) 0.036(2) 0.060(2) -0.0173(18) -0.0060(16) -0.0041(15) C6 0.0423(19) 0.0309(19) 0.054(2) -0.0144(17) -0.0039(16) -0.0033(15) C7 0.058(2) 0.045(2) 0.040(2) -0.0073(17) -0.0040(17) -0.0050(17) C8 0.069(3) 0.054(3) 0.043(2) -0.0203(19) -0.0018(18) -0.007(2) C9 0.052(2) 0.043(2) 0.043(2) -0.0204(18) -0.0010(16) -0.0043(16) C10 0.105(4) 0.055(3) 0.052(3) -0.006(2) -0.008(3) -0.006(3) C11 0.094(3) 0.049(2) 0.051(2) -0.029(2) 0.003(2) -0.011(2) C12 0.070(3) 0.120(4) 0.048(2) -0.042(3) 0.000(2) -0.013(3) C13 0.0378(19) 0.078(3) 0.044(2) -0.022(2) 0.0002(16) -0.0128(19) C14 0.057(2) 0.062(3) 0.038(2) -0.005(2) -0.0044(17) -0.010(2) C15 0.040(2) 0.051(2) 0.049(2) -0.0109(19) -0.0008(16) -0.0066(17) C16 0.074(3) 0.048(3) 0.065(3) -0.005(2) 0.000(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd O1 1.969(2) . ? Pd O2 1.975(2) . ? Pd N1 1.996(3) . ? Pd N2 2.007(3) . ? F1 C10 1.324(5) . ? F2 C10 1.345(5) . ? F3 C10 1.339(5) . ? F4 C11 1.345(4) . ? F5 C11 1.335(5) . ? F6 C11 1.328(5) . ? O1 C13 1.275(4) . ? O2 C15 1.272(4) . ? N1 C1 1.339(5) . ? N1 C5 1.355(4) . ? N2 C6 1.367(4) . ? N2 C9 1.369(4) . ? C1 C2 1.373(5) . ? C2 C3 1.363(6) . ? C3 C4 1.376(6) . ? C4 C5 1.383(5) . ? C5 C6 1.447(5) . ? C6 C7 1.391(5) . ? C7 C8 1.390(5) . ? C7 C10 1.476(5) . ? C8 C9 1.375(5) . ? C9 C11 1.483(5) . ? C12 C13 1.507(5) . ? C13 C14 1.384(5) . ? C14 C15 1.392(5) . ? C15 C16 1.490(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd O2 93.08(10) . . ? O1 Pd N1 90.32(11) . . ? O2 Pd N1 176.60(11) . . ? O1 Pd N2 170.81(11) . . ? O2 Pd N2 96.09(10) . . ? N1 Pd N2 80.52(11) . . ? C13 O1 Pd 124.7(3) . . ? C15 O2 Pd 124.9(2) . . ? C1 N1 C5 119.8(3) . . ? C1 N1 Pd 124.0(3) . . ? C5 N1 Pd 116.2(2) . . ? C6 N2 C9 106.8(3) . . ? C6 N2 Pd 113.8(2) . . ? C9 N2 Pd 139.4(2) . . ? N1 C1 C2 121.6(4) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 119.8(4) . . ? C3 C4 C5 119.4(4) . . ? N1 C5 C4 120.1(3) . . ? N1 C5 C6 113.3(3) . . ? C4 C5 C6 126.5(4) . . ? N2 C6 C7 109.3(3) . . ? N2 C6 C5 116.2(3) . . ? C7 C6 C5 134.5(3) . . ? C8 C7 C6 106.9(3) . . ? C8 C7 C10 123.6(4) . . ? C6 C7 C10 129.5(4) . . ? C9 C8 C7 107.1(3) . . ? N2 C9 C8 109.9(3) . . ? N2 C9 C11 123.9(3) . . ? C8 C9 C11 126.1(3) . . ? F1 C10 F3 106.8(4) . . ? F1 C10 F2 105.9(4) . . ? F3 C10 F2 105.4(4) . . ? F1 C10 C7 113.6(4) . . ? F3 C10 C7 111.7(4) . . ? F2 C10 C7 112.9(4) . . ? F6 C11 F5 107.0(3) . . ? F6 C11 F4 106.2(3) . . ? F5 C11 F4 106.2(3) . . ? F6 C11 C9 113.6(3) . . ? F5 C11 C9 113.9(3) . . ? F4 C11 C9 109.4(3) . . ? O1 C13 C14 125.4(3) . . ? O1 C13 C12 113.5(4) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C15 126.7(3) . . ? O2 C15 C14 125.1(4) . . ? O2 C15 C16 114.5(3) . . ? C14 C15 C16 120.4(3) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Pd O1 C13 -0.4(3) . . . . ? N1 Pd O1 C13 179.7(3) . . . . ? N2 Pd O1 C13 176.1(6) . . . . ? O1 Pd O2 C15 1.1(3) . . . . ? N1 Pd O2 C15 179(55) . . . . ? N2 Pd O2 C15 -178.3(3) . . . . ? O1 Pd N1 C1 -0.7(3) . . . . ? O2 Pd N1 C1 -179(55) . . . . ? N2 Pd N1 C1 178.7(3) . . . . ? O1 Pd N1 C5 180.0(2) . . . . ? O2 Pd N1 C5 1.8(19) . . . . ? N2 Pd N1 C5 -0.6(2) . . . . ? O1 Pd N2 C6 4.6(8) . . . . ? O2 Pd N2 C6 -179.0(2) . . . . ? N1 Pd N2 C6 0.9(2) . . . . ? O1 Pd N2 C9 -176.0(5) . . . . ? O2 Pd N2 C9 0.4(4) . . . . ? N1 Pd N2 C9 -179.7(4) . . . . ? C5 N1 C1 C2 -0.5(5) . . . . ? Pd N1 C1 C2 -179.8(3) . . . . ? N1 C1 C2 C3 -0.1(6) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C1 N1 C5 C4 1.1(5) . . . . ? Pd N1 C5 C4 -179.5(2) . . . . ? C1 N1 C5 C6 -179.1(3) . . . . ? Pd N1 C5 C6 0.3(4) . . . . ? C3 C4 C5 N1 -1.2(5) . . . . ? C3 C4 C5 C6 179.1(3) . . . . ? C9 N2 C6 C7 0.5(4) . . . . ? Pd N2 C6 C7 -179.9(2) . . . . ? C9 N2 C6 C5 179.4(3) . . . . ? Pd N2 C6 C5 -1.0(4) . . . . ? N1 C5 C6 N2 0.5(4) . . . . ? C4 C5 C6 N2 -179.8(3) . . . . ? N1 C5 C6 C7 179.0(4) . . . . ? C4 C5 C6 C7 -1.2(6) . . . . ? N2 C6 C7 C8 -0.3(4) . . . . ? C5 C6 C7 C8 -179.0(4) . . . . ? N2 C6 C7 C10 180.0(4) . . . . ? C5 C6 C7 C10 1.3(7) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C10 C7 C8 C9 179.8(4) . . . . ? C6 N2 C9 C8 -0.5(4) . . . . ? Pd N2 C9 C8 -179.9(3) . . . . ? C6 N2 C9 C11 -179.6(3) . . . . ? Pd N2 C9 C11 1.0(6) . . . . ? C7 C8 C9 N2 0.3(4) . . . . ? C7 C8 C9 C11 179.4(4) . . . . ? C8 C7 C10 F1 119.4(5) . . . . ? C6 C7 C10 F1 -61.0(6) . . . . ? C8 C7 C10 F3 -1.5(7) . . . . ? C6 C7 C10 F3 178.2(4) . . . . ? C8 C7 C10 F2 -120.1(5) . . . . ? C6 C7 C10 F2 59.6(6) . . . . ? N2 C9 C11 F6 60.4(5) . . . . ? C8 C9 C11 F6 -118.6(4) . . . . ? N2 C9 C11 F5 -62.5(5) . . . . ? C8 C9 C11 F5 118.5(4) . . . . ? N2 C9 C11 F4 178.8(3) . . . . ? C8 C9 C11 F4 -0.1(6) . . . . ? Pd O1 C13 C14 -1.0(5) . . . . ? Pd O1 C13 C12 -179.3(2) . . . . ? O1 C13 C14 C15 1.9(6) . . . . ? C12 C13 C14 C15 -179.8(4) . . . . ? Pd O2 C15 C14 -0.6(5) . . . . ? Pd O2 C15 C16 179.2(2) . . . . ? C13 C14 C15 O2 -1.0(6) . . . . ? C13 C14 C15 C16 179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.346 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.075 #===END data_(5) _database_code_depnum_ccdc_archive 'CCDC 706174' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H12 F6 N2 O2 Pd' _chemical_formula_sum 'C16 H12 F6 N2 O2 Pd' _chemical_formula_weight 484.68 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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' _cell_length_a 10.903(2) _cell_length_b 21.574(5) _cell_length_c 7.4042(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.426(7) _cell_angle_gamma 90.00 _cell_volume 1707.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4546 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 24.49 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14746 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3099 _reflns_number_gt 2249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+4.2238P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3099 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.24514(5) 0.18434(2) 0.10949(8) 0.0473(3) Uani 1 1 d . . . O1 O 0.1986(5) 0.0936(3) 0.0708(8) 0.0602(14) Uani 1 1 d . . . O2 O 0.4178(5) 0.1630(3) 0.2493(8) 0.0582(13) Uani 1 1 d . . . N1 N 0.0782(6) 0.2105(3) -0.0310(8) 0.0493(14) Uani 1 1 d . . . N2 N 0.2686(6) 0.2754(3) 0.1295(8) 0.0512(16) Uani 1 1 d . . . C1 C -0.0121(8) 0.1711(4) -0.1075(12) 0.061(2) Uani 1 1 d . . . H1B H 0.0022 0.1287 -0.0931 0.073 Uiso 1 1 calc R . . C2 C -0.1224(10) 0.1907(4) -0.2043(13) 0.073(3) Uani 1 1 d . . . H2B H -0.1831 0.1623 -0.2574 0.087 Uiso 1 1 calc R . . C3 C -0.1446(8) 0.2531(5) -0.2239(12) 0.071(2) Uani 1 1 d . . . H3A H -0.2213 0.2673 -0.2888 0.085 Uiso 1 1 calc R . . C4 C -0.0533(8) 0.2945(4) -0.1476(12) 0.064(2) Uani 1 1 d . . . H4A H -0.0676 0.3369 -0.1625 0.076 Uiso 1 1 calc R . . C5 C 0.0610(7) 0.2730(3) -0.0476(10) 0.0518(18) Uani 1 1 d . . . C6 C 0.1657(8) 0.3082(3) 0.0408(11) 0.056(2) Uani 1 1 d . . . C7 C 0.1889(9) 0.3714(4) 0.0682(13) 0.065(2) Uani 1 1 d . . . C8 C 0.3086(9) 0.3743(4) 0.1711(12) 0.064(2) Uani 1 1 d . . . H8A H 0.3511 0.4108 0.2094 0.077 Uiso 1 1 calc R . . C9 C 0.3573(9) 0.3151(4) 0.2100(12) 0.058(2) Uani 1 1 d . . . C10 C 0.1018(11) 0.4241(4) 0.0043(16) 0.087(3) Uani 1 1 d . . . H10A H 0.1459 0.4626 0.0300 0.131 Uiso 1 1 calc R . . H10B H 0.0332 0.4230 0.0679 0.131 Uiso 1 1 calc R . . H10C H 0.0705 0.4205 -0.1259 0.131 Uiso 1 1 calc R . . C11 C 0.4812(9) 0.2971(5) 0.3171(13) 0.072(2) Uani 1 1 d . . . H11A H 0.4707 0.2690 0.4132 0.108 Uiso 1 1 calc R . . H11B H 0.5248 0.3334 0.3704 0.108 Uiso 1 1 calc R . . H11C H 0.5286 0.2773 0.2372 0.108 Uiso 1 1 calc R . . C12 C 0.2180(10) -0.0136(4) 0.0637(15) 0.074(3) Uani 1 1 d . . . C13 C 0.2783(8) 0.0496(4) 0.1194(10) 0.057(2) Uani 1 1 d . . . C14 C 0.3981(8) 0.0519(4) 0.2100(12) 0.063(2) Uani 1 1 d . . . H14A H 0.4427 0.0150 0.2332 0.076 Uiso 1 1 calc R . . C15 C 0.4582(8) 0.1076(4) 0.2707(11) 0.058(2) Uani 1 1 d . A . C16 C 0.5934(10) 0.1066(6) 0.3739(14) 0.086(3) Uani 1 1 d . . . F1 F 0.3015(7) -0.0591(3) 0.0767(11) 0.119(2) Uani 1 1 d . . . F2 F 0.1471(8) -0.0306(3) 0.1799(12) 0.132(3) Uani 1 1 d . . . F3 F 0.1512(8) -0.0155(3) -0.0971(10) 0.135(3) Uani 1 1 d . . . F4 F 0.6400(10) 0.0455(6) 0.3862(16) 0.088(4) Uiso 0.545(15) 1 d P A 1 F5 F 0.6684(11) 0.1294(6) 0.2732(16) 0.088(4) Uiso 0.545(15) 1 d P A 1 F6 F 0.6012(13) 0.1165(8) 0.549(2) 0.118(5) Uiso 0.545(15) 1 d P A 1 F4A F 0.6266(12) 0.1564(8) 0.4734(19) 0.087(5) Uiso 0.455(15) 1 d P A 2 F5A F 0.6072(18) 0.0649(10) 0.509(3) 0.131(7) Uiso 0.455(15) 1 d P A 2 F6A F 0.668(2) 0.0896(14) 0.283(4) 0.173(10) Uiso 0.455(15) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0493(4) 0.0383(4) 0.0526(4) 0.0013(2) 0.0062(3) -0.0030(2) O1 0.056(3) 0.045(3) 0.074(3) 0.000(3) -0.001(3) -0.003(3) O2 0.056(3) 0.049(3) 0.066(3) 0.007(3) 0.003(3) -0.005(3) N1 0.050(3) 0.046(4) 0.050(3) -0.005(3) 0.006(3) -0.002(3) N2 0.064(4) 0.039(4) 0.052(4) -0.006(3) 0.016(3) -0.004(3) C1 0.058(5) 0.049(5) 0.070(5) -0.001(4) -0.002(4) -0.001(4) C2 0.071(6) 0.063(6) 0.078(6) 0.000(5) -0.001(5) -0.001(5) C3 0.057(5) 0.086(7) 0.067(5) 0.000(5) 0.004(4) 0.010(5) C4 0.064(5) 0.060(5) 0.067(5) 0.005(4) 0.012(4) 0.016(4) C5 0.060(5) 0.045(5) 0.052(4) 0.000(3) 0.014(4) 0.000(4) C6 0.073(6) 0.041(4) 0.056(5) 0.004(4) 0.016(4) 0.009(4) C7 0.083(6) 0.043(5) 0.072(5) -0.002(4) 0.022(5) 0.002(4) C8 0.084(6) 0.042(5) 0.069(5) -0.006(4) 0.021(5) -0.011(4) C9 0.065(5) 0.055(5) 0.054(5) -0.006(4) 0.014(4) -0.012(4) C10 0.116(9) 0.040(5) 0.109(8) 0.004(5) 0.030(7) 0.003(5) C11 0.069(6) 0.068(6) 0.077(6) -0.017(5) 0.010(5) -0.022(5) C12 0.083(7) 0.044(5) 0.091(7) -0.004(5) 0.005(6) -0.005(5) C13 0.074(5) 0.046(5) 0.053(4) 0.000(4) 0.013(4) -0.003(4) C14 0.062(5) 0.041(4) 0.082(6) 0.002(4) 0.004(4) 0.009(4) C15 0.056(5) 0.059(5) 0.058(5) 0.010(4) 0.009(4) 0.000(4) C16 0.087(7) 0.097(8) 0.071(6) 0.005(6) 0.011(5) 0.035(6) F1 0.121(5) 0.046(3) 0.181(7) -0.017(4) 0.005(5) 0.013(3) F2 0.169(7) 0.064(4) 0.182(7) -0.032(4) 0.080(6) -0.051(5) F3 0.186(8) 0.067(4) 0.119(5) -0.012(4) -0.052(5) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N2 1.983(6) . ? Pd N1 1.991(6) . ? Pd O2 2.013(5) . ? Pd O1 2.029(5) . ? O1 C13 1.290(10) . ? O2 C15 1.272(10) . ? N1 C1 1.339(10) . ? N1 C5 1.363(10) . ? N2 C9 1.340(10) . ? N2 C6 1.378(10) . ? C1 C2 1.341(13) . ? C2 C3 1.370(13) . ? C3 C4 1.373(13) . ? C4 C5 1.397(11) . ? C5 C6 1.418(11) . ? C6 C7 1.394(11) . ? C7 C8 1.376(14) . ? C7 C10 1.496(13) . ? C8 C9 1.391(12) . ? C9 C11 1.476(13) . ? C12 F3 1.267(11) . ? C12 F2 1.318(12) . ? C12 F1 1.329(11) . ? C12 C13 1.533(12) . ? C13 C14 1.346(12) . ? C14 C15 1.401(12) . ? C15 C16 1.520(13) . ? C16 F6A 1.21(3) . ? C16 F6 1.297(17) . ? C16 F5 1.307(16) . ? C16 F4A 1.313(18) . ? C16 F5A 1.33(2) . ? C16 F4 1.410(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd N1 81.3(3) . . ? N2 Pd O2 95.4(2) . . ? N1 Pd O2 176.6(2) . . ? N2 Pd O1 172.6(2) . . ? N1 Pd O1 91.3(2) . . ? O2 Pd O1 92.0(2) . . ? C13 O1 Pd 122.4(5) . . ? C15 O2 Pd 123.0(5) . . ? C1 N1 C5 121.0(7) . . ? C1 N1 Pd 124.0(6) . . ? C5 N1 Pd 115.0(5) . . ? C9 N2 C6 109.4(7) . . ? C9 N2 Pd 137.5(6) . . ? C6 N2 Pd 113.1(5) . . ? N1 C1 C2 122.1(8) . . ? C1 C2 C3 119.2(9) . . ? C2 C3 C4 119.8(9) . . ? C3 C4 C5 120.0(8) . . ? N1 C5 C4 117.9(7) . . ? N1 C5 C6 113.8(7) . . ? C4 C5 C6 128.3(8) . . ? N2 C6 C7 109.0(8) . . ? N2 C6 C5 116.8(7) . . ? C7 C6 C5 134.2(8) . . ? C8 C7 C6 104.5(8) . . ? C8 C7 C10 127.8(8) . . ? C6 C7 C10 127.7(9) . . ? C7 C8 C9 110.7(8) . . ? N2 C9 C8 106.4(8) . . ? N2 C9 C11 125.1(8) . . ? C8 C9 C11 128.6(8) . . ? F3 C12 F2 107.5(10) . . ? F3 C12 F1 107.6(9) . . ? F2 C12 F1 103.2(9) . . ? F3 C12 C13 114.7(8) . . ? F2 C12 C13 110.3(8) . . ? F1 C12 C13 112.7(8) . . ? O1 C13 C14 130.2(8) . . ? O1 C13 C12 110.5(8) . . ? C14 C13 C12 119.3(8) . . ? C13 C14 C15 122.5(8) . . ? O2 C15 C14 129.7(8) . . ? O2 C15 C16 110.7(8) . . ? C14 C15 C16 119.6(8) . . ? F6A C16 F6 133.3(17) . . ? F6A C16 F5 39.9(14) . . ? F6 C16 F5 125.6(13) . . ? F6A C16 F4A 114.9(18) . . ? F6 C16 F4A 49.5(9) . . ? F5 C16 F4A 82.9(12) . . ? F6A C16 F5A 102.9(17) . . ? F6 C16 F5A 52.1(10) . . ? F5 C16 F5A 133.8(13) . . ? F4A C16 F5A 98.9(13) . . ? F6A C16 F4 58.6(14) . . ? F6 C16 F4 97.9(11) . . ? F5 C16 F4 97.5(10) . . ? F4A C16 F4 132.3(11) . . ? F5A C16 F4 48.2(10) . . ? F6A C16 C15 114.5(15) . . ? F6 C16 C15 111.4(10) . . ? F5 C16 C15 111.2(9) . . ? F4A C16 C15 113.8(10) . . ? F5A C16 C15 110.0(12) . . ? F4 C16 C15 110.3(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.892 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.147 #===END data_(6) _database_code_depnum_ccdc_archive 'CCDC 706175' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H6 F12 N2 O2 Pd' _chemical_formula_sum 'C16 H6 F12 N2 O2 Pd' _chemical_formula_weight 592.63 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.289(6) _cell_length_b 16.499(10) _cell_length_c 19.408(8) _cell_angle_alpha 83.77(2) _cell_angle_beta 85.485(15) _cell_angle_gamma 66.752(18) _cell_volume 3884(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 10774 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68839 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15871 _reflns_number_gt 10774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+2.8521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15871 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.59805(3) 0.37386(2) 0.013858(18) 0.05121(11) Uani 1 1 d . . . Pd2 Pd 0.05730(3) 0.88241(2) 0.020830(19) 0.05433(11) Uani 1 1 d . . . Pd3 Pd 0.60074(3) 0.86992(2) 0.490251(19) 0.05834(11) Uani 1 1 d . . . Pd4 Pd 0.97107(3) 0.61735(2) 0.48746(2) 0.06185(12) Uani 1 1 d . . . F1 F 1.0015(3) 0.3648(3) 0.1190(2) 0.1147(13) Uani 1 1 d . . . F2 F 0.9289(3) 0.5006(3) 0.0816(2) 0.1209(14) Uani 1 1 d . . . F3 F 0.9244(4) 0.4640(3) 0.1898(2) 0.1432(17) Uani 1 1 d . . . F4 F 0.5242(3) 0.3671(2) 0.20306(17) 0.0888(10) Uani 1 1 d . . . F5 F 0.4483(2) 0.5041(2) 0.16690(17) 0.0879(9) Uani 1 1 d . . . F6 F 0.5437(3) 0.4663(3) 0.25741(17) 0.1181(13) Uani 1 1 d . . . F7 F 0.4844(5) 0.3350(4) -0.1911(2) 0.160(2) Uani 1 1 d . . . F8 F 0.4786(4) 0.2199(3) -0.1350(3) 0.157(2) Uani 1 1 d . . . F9 F 0.3375(4) 0.3318(3) -0.1552(2) 0.1409(17) Uani 1 1 d . . . F10 F 0.3020(4) 0.3254(3) 0.1382(4) 0.227(4) Uani 1 1 d . . . F11 F 0.1898(3) 0.4116(4) 0.0674(3) 0.176(2) Uani 1 1 d . . . F12 F 0.2600(3) 0.4593(3) 0.1313(3) 0.1388(17) Uani 1 1 d . . . F13 F 0.4063(3) 0.9380(3) -0.1456(2) 0.1059(12) Uani 1 1 d . . . F14 F 0.4982(3) 0.8058(3) -0.1091(2) 0.1299(16) Uani 1 1 d . . . F15 F 0.5165(3) 0.9136(4) -0.0656(3) 0.163(2) Uani 1 1 d . . . F16 F 0.1292(3) 1.0097(2) 0.14435(19) 0.0982(11) Uani 1 1 d . . . F17 F 0.2999(3) 0.9562(3) 0.1667(2) 0.1315(16) Uani 1 1 d . . . F18 F 0.2109(3) 0.8706(3) 0.17741(17) 0.1068(12) Uani 1 1 d . . . F19 F -0.2561(4) 0.8570(4) -0.0328(3) 0.1527(19) Uani 1 1 d . . . F20 F -0.2057(4) 0.7532(3) 0.0450(4) 0.180(3) Uani 1 1 d . . . F21 F -0.3345(3) 0.8774(3) 0.0645(3) 0.1551(19) Uani 1 1 d . . . F22 F -0.1767(4) 0.9406(5) 0.2546(3) 0.216(3) Uani 1 1 d . . . F23 F -0.0645(5) 0.9994(3) 0.2325(2) 0.157(2) Uani 1 1 d . . . F24 F -0.0111(5) 0.8667(3) 0.2587(2) 0.1496(19) Uani 1 1 d . . . F25 F 0.9000(4) 0.7646(3) 0.7187(2) 0.1344(16) Uani 1 1 d . . . F26 F 0.8405(4) 0.9040(3) 0.7166(2) 0.1327(15) Uani 1 1 d . . . F27 F 0.7776(5) 0.8346(3) 0.79458(19) 0.1526(18) Uani 1 1 d . . . F28 F 0.4337(3) 0.7953(3) 0.6216(2) 0.1167(13) Uani 1 1 d . . . F29 F 0.4071(4) 0.8513(4) 0.7192(2) 0.163(2) Uani 1 1 d . . . F30 F 0.3685(3) 0.9364(3) 0.6254(2) 0.1170(13) Uani 1 1 d . . . F31 F 0.6197(7) 0.8215(4) 0.2540(2) 0.226(4) Uani 1 1 d . . . F32 F 0.6172(5) 0.9437(5) 0.2589(2) 0.180(2) Uani 1 1 d . . . F33 F 0.4798(4) 0.9349(4) 0.2333(2) 0.163(2) Uani 1 1 d . . . F34 F 0.2762(3) 0.8194(3) 0.4756(4) 0.200(3) Uani 1 1 d . . . F35 F 0.2243(4) 0.9457(3) 0.5075(3) 0.162(2) Uani 1 1 d . . . F36 F 0.2075(4) 0.9320(5) 0.4088(4) 0.195(3) Uani 1 1 d . . . F37 F 0.5038(3) 0.6920(3) 0.4688(4) 0.175(3) Uani 1 1 d . . . F38 F 0.5260(5) 0.6276(5) 0.3756(5) 0.222(3) Uani 1 1 d . . . F39 F 0.5751(3) 0.5518(3) 0.4711(4) 0.167(2) Uani 1 1 d . . . F40 F 0.9313(3) 0.7119(2) 0.30483(18) 0.0974(10) Uani 1 1 d . . . F41 F 0.8567(3) 0.6569(3) 0.2401(2) 0.1254(14) Uani 1 1 d . . . F42 F 0.9989(3) 0.5723(3) 0.2958(2) 0.1050(11) Uani 1 1 d . . . F43 F 1.1663(4) 0.7142(4) 0.6267(3) 0.171(2) Uani 1 1 d . . . F44 F 1.2245(7) 0.5789(4) 0.6531(3) 0.226(4) Uani 1 1 d . . . F45 F 1.3186(5) 0.6323(5) 0.5920(3) 0.198(3) Uani 1 1 d . . . F46 F 1.3298(4) 0.6076(6) 0.3527(3) 0.219(3) Uani 1 1 d . . . F47 F 1.1943(6) 0.7195(4) 0.3265(3) 0.221(4) Uani 1 1 d . . . F48 F 1.2090(4) 0.6010(4) 0.3002(2) 0.158(2) Uani 1 1 d . . . O1 O 0.5490(3) 0.3374(2) -0.06778(18) 0.0714(9) Uani 1 1 d . . . O2 O 0.4569(3) 0.3915(2) 0.06676(18) 0.0655(9) Uani 1 1 d . . . O3 O -0.0789(3) 0.8631(2) 0.00790(19) 0.0707(9) Uani 1 1 d . . . O4 O 0.0084(3) 0.9154(2) 0.11766(18) 0.0695(9) Uani 1 1 d . . . O5 O 0.6074(3) 0.8781(2) 0.38708(17) 0.0703(9) Uani 1 1 d . . . O6 O 0.4432(3) 0.8841(2) 0.4933(2) 0.0764(10) Uani 1 1 d . . . O7 O 1.0757(4) 0.6157(2) 0.55745(18) 0.0781(10) Uani 1 1 d . . . O8 O 1.0774(3) 0.6214(2) 0.40968(18) 0.0712(9) Uani 1 1 d . . . N1 N 0.7426(3) 0.3580(2) -0.03532(19) 0.0515(9) Uani 1 1 d . . . N2 N 0.6661(3) 0.4083(2) 0.08731(18) 0.0505(9) Uani 1 1 d . . . N3 N 0.1152(3) 0.8454(2) -0.0731(2) 0.0559(9) Uani 1 1 d . . . N4 N 0.1999(3) 0.8935(2) 0.02200(19) 0.0542(9) Uani 1 1 d . . . N5 N 0.7571(3) 0.8572(3) 0.4909(2) 0.0573(10) Uani 1 1 d . . . N6 N 0.6167(4) 0.8585(3) 0.5922(2) 0.0649(11) Uani 1 1 d . . . N7 N 0.8605(4) 0.6152(3) 0.5610(3) 0.0771(13) Uani 1 1 d . . . N8 N 0.8508(3) 0.6248(3) 0.4276(2) 0.0656(11) Uani 1 1 d . . . C1 C 0.7715(4) 0.3287(3) -0.0989(2) 0.0640(13) Uani 1 1 d . . . H1A H 0.7236 0.3133 -0.1218 0.077 Uiso 1 1 calc R . . C2 C 0.8710(5) 0.3210(4) -0.1307(3) 0.0750(15) Uani 1 1 d . . . H2A H 0.8899 0.3016 -0.1749 0.090 Uiso 1 1 calc R . . C3 C 0.9413(5) 0.3425(4) -0.0959(3) 0.0785(16) Uani 1 1 d . . . H3A H 1.0084 0.3385 -0.1166 0.094 Uiso 1 1 calc R . . C4 C 0.9129(4) 0.3699(3) -0.0307(3) 0.0681(14) Uani 1 1 d . . . H4A H 0.9615 0.3834 -0.0068 0.082 Uiso 1 1 calc R . . C5 C 0.8121(3) 0.3778(3) 0.0003(2) 0.0523(11) Uani 1 1 d . . . C6 C 0.7690(4) 0.4064(3) 0.0688(2) 0.0524(11) Uani 1 1 d . . . C7 C 0.8083(4) 0.4328(3) 0.1235(3) 0.0634(13) Uani 1 1 d . . . C8 C 0.7269(4) 0.4503(3) 0.1760(3) 0.0704(14) Uani 1 1 d . . . H8A H 0.7298 0.4692 0.2190 0.085 Uiso 1 1 calc R . . C9 C 0.6423(4) 0.4346(3) 0.1535(2) 0.0593(12) Uani 1 1 d . . . C10 C 0.9148(5) 0.4405(5) 0.1285(4) 0.0871(18) Uani 1 1 d . . . C11 C 0.5399(5) 0.4426(4) 0.1942(3) 0.0740(15) Uani 1 1 d . . . C12 C 0.4397(6) 0.3058(5) -0.1396(4) 0.0893(18) Uani 1 1 d . . . C13 C 0.4550(5) 0.3369(3) -0.0716(3) 0.0698(14) Uani 1 1 d . . . C14 C 0.3705(5) 0.3566(4) -0.0221(3) 0.0791(17) Uani 1 1 d . . . H14A H 0.3049 0.3542 -0.0330 0.095 Uiso 1 1 calc R . . C15 C 0.3786(4) 0.3798(3) 0.0429(3) 0.0671(14) Uani 1 1 d . . . C16 C 0.2848(5) 0.3888(5) 0.0980(4) 0.097(2) Uani 1 1 d . . . C17 C 0.0636(4) 0.8186(3) -0.1167(3) 0.0666(13) Uani 1 1 d . . . H17A H -0.0052 0.8185 -0.1037 0.080 Uiso 1 1 calc R . . C18 C 0.1106(5) 0.7909(4) -0.1808(3) 0.0782(16) Uani 1 1 d . . . H18A H 0.0732 0.7731 -0.2106 0.094 Uiso 1 1 calc R . . C19 C 0.2119(5) 0.7900(4) -0.1999(3) 0.0814(16) Uani 1 1 d . . . H19A H 0.2449 0.7706 -0.2424 0.098 Uiso 1 1 calc R . . C20 C 0.2648(5) 0.8184(4) -0.1554(3) 0.0735(15) Uani 1 1 d . . . H20A H 0.3338 0.8185 -0.1680 0.088 Uiso 1 1 calc R . . C21 C 0.2159(4) 0.8467(3) -0.0921(2) 0.0555(11) Uani 1 1 d . . . C22 C 0.2620(3) 0.8765(3) -0.0402(2) 0.0517(11) Uani 1 1 d . . . C23 C 0.3559(4) 0.8921(3) -0.0344(3) 0.0664(13) Uani 1 1 d . . . C24 C 0.3526(4) 0.9182(4) 0.0322(3) 0.0728(15) Uani 1 1 d . . . H24A H 0.4054 0.9327 0.0504 0.087 Uiso 1 1 calc R . . C25 C 0.2584(4) 0.9187(3) 0.0657(3) 0.0628(13) Uani 1 1 d . . . C26 C 0.4444(5) 0.8862(5) -0.0877(4) 0.0869(18) Uani 1 1 d . . . C27 C 0.2247(5) 0.9376(4) 0.1377(3) 0.0809(16) Uani 1 1 d . . . C28 C -0.2383(5) 0.8389(6) 0.0338(5) 0.105(2) Uani 1 1 d . . . C29 C -0.1516(4) 0.8679(4) 0.0564(4) 0.0771(17) Uani 1 1 d . . . C30 C -0.1558(5) 0.8909(4) 0.1219(4) 0.0831(17) Uani 1 1 d . . . H30A H -0.2157 0.8927 0.1508 0.100 Uiso 1 1 calc R . . C31 C -0.0766(4) 0.9119(3) 0.1479(3) 0.0703(14) Uani 1 1 d . . . C32 C -0.0860(6) 0.9316(5) 0.2233(3) 0.094(2) Uani 1 1 d . . . C33 C 0.8200(4) 0.8563(3) 0.4338(3) 0.0657(13) Uani 1 1 d . . . H33A H 0.7917 0.8605 0.3907 0.079 Uiso 1 1 calc R . . C34 C 0.9262(5) 0.8495(4) 0.4375(3) 0.0765(15) Uani 1 1 d . . . H34A H 0.9693 0.8492 0.3973 0.092 Uiso 1 1 calc R . . C35 C 0.9671(5) 0.8430(4) 0.5012(3) 0.0783(16) Uani 1 1 d . . . H35A H 1.0384 0.8388 0.5047 0.094 Uiso 1 1 calc R . . C36 C 0.9023(4) 0.8429(3) 0.5601(3) 0.0722(14) Uani 1 1 d . . . H36A H 0.9301 0.8380 0.6036 0.087 Uiso 1 1 calc R . . C37 C 0.7968(4) 0.8500(3) 0.5546(2) 0.0590(12) Uani 1 1 d . . . C38 C 0.7180(5) 0.8510(3) 0.6112(3) 0.0657(13) Uani 1 1 d . . . C39 C 0.7188(6) 0.8448(4) 0.6834(3) 0.0818(17) Uani 1 1 d . . . C40 C 0.6152(6) 0.8483(4) 0.7081(3) 0.0910(19) Uani 1 1 d . . . H40A H 0.5916 0.8454 0.7544 0.109 Uiso 1 1 calc R . . C41 C 0.5555(5) 0.8565(4) 0.6522(3) 0.0781(16) Uani 1 1 d . . . C42 C 0.8089(8) 0.8362(6) 0.7277(3) 0.108(2) Uani 1 1 d . . . C43 C 0.4418(7) 0.8604(6) 0.6535(3) 0.100(2) Uani 1 1 d . . . C44 C 0.5567(6) 0.8950(6) 0.2732(3) 0.099(2) Uani 1 1 d . . . C45 C 0.5278(5) 0.8916(4) 0.3498(3) 0.0715(14) Uani 1 1 d . . . C46 C 0.4227(5) 0.8988(4) 0.3717(3) 0.0831(17) Uani 1 1 d . . . H46A H 0.3720 0.9079 0.3383 0.100 Uiso 1 1 calc R . . C47 C 0.3903(5) 0.8932(4) 0.4402(4) 0.0752(15) Uani 1 1 d . . . C48 C 0.2760(5) 0.8936(5) 0.4580(5) 0.107(2) Uani 1 1 d . . . C49 C 0.8757(6) 0.6131(4) 0.6281(4) 0.099(2) Uani 1 1 d . . . H49A H 0.9418 0.6116 0.6421 0.118 Uiso 1 1 calc R . . C50 C 0.7948(9) 0.6131(5) 0.6775(4) 0.135(3) Uani 1 1 d . . . H50A H 0.8065 0.6108 0.7245 0.161 Uiso 1 1 calc R . . C51 C 0.6979(8) 0.6166(5) 0.6565(6) 0.130(4) Uani 1 1 d . . . H51A H 0.6421 0.6179 0.6890 0.157 Uiso 1 1 calc R . . C52 C 0.6821(6) 0.6184(4) 0.5865(5) 0.112(3) Uani 1 1 d . . . H52A H 0.6159 0.6205 0.5721 0.134 Uiso 1 1 calc R . . C53 C 0.7645(5) 0.6169(3) 0.5385(4) 0.0850(19) Uani 1 1 d . . . C54 C 0.7611(5) 0.6221(3) 0.4636(4) 0.0779(16) Uani 1 1 d . . . C55 C 0.6837(5) 0.6272(4) 0.4158(5) 0.091(2) Uani 1 1 d . . . C56 C 0.7299(5) 0.6331(4) 0.3505(4) 0.095(2) Uani 1 1 d . . . H56A H 0.6978 0.6368 0.3088 0.114 Uiso 1 1 calc R . . C57 C 0.8304(4) 0.6326(3) 0.3581(3) 0.0733(15) Uani 1 1 d . . . C58 C 0.5730(7) 0.6242(6) 0.4334(7) 0.138(4) Uani 1 1 d . . . C59 C 0.9052(5) 0.6437(4) 0.3013(3) 0.0823(16) Uani 1 1 d . . . C60 C 1.2171(7) 0.6355(6) 0.6065(4) 0.110(2) Uani 1 1 d . . . C61 C 1.1653(6) 0.6264(4) 0.5413(3) 0.0818(18) Uani 1 1 d . . . C62 C 1.2131(5) 0.6323(4) 0.4771(3) 0.0790(16) Uani 1 1 d . . . H62A H 1.2798 0.6388 0.4739 0.095 Uiso 1 1 calc R . . C63 C 1.1670(4) 0.6291(3) 0.4168(3) 0.0689(14) Uani 1 1 d . . . C64 C 1.2279(6) 0.6385(6) 0.3496(4) 0.105(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0513(2) 0.0624(2) 0.0470(2) 0.00104(16) -0.00504(15) -0.03056(18) Pd2 0.0471(2) 0.0602(2) 0.0575(2) 0.00131(17) -0.00214(16) -0.02436(17) Pd3 0.0660(2) 0.0622(2) 0.0512(2) -0.00624(18) 0.00596(17) -0.0309(2) Pd4 0.0676(2) 0.0568(2) 0.0612(2) -0.00554(19) -0.00575(19) -0.02361(19) F1 0.060(2) 0.129(3) 0.160(4) 0.001(3) -0.030(2) -0.040(2) F2 0.109(3) 0.127(3) 0.160(4) 0.016(3) -0.023(3) -0.085(3) F3 0.134(3) 0.220(5) 0.129(4) -0.051(3) -0.027(3) -0.112(4) F4 0.084(2) 0.099(2) 0.081(2) 0.0149(19) 0.0138(17) -0.0414(19) F5 0.0647(19) 0.093(2) 0.093(2) -0.0119(19) 0.0066(17) -0.0175(17) F6 0.114(3) 0.185(4) 0.058(2) -0.036(2) 0.0145(19) -0.059(3) F7 0.239(6) 0.238(6) 0.076(3) -0.038(3) -0.006(3) -0.166(5) F8 0.215(5) 0.080(3) 0.168(4) -0.023(3) -0.108(4) -0.029(3) F9 0.132(3) 0.147(4) 0.151(4) -0.020(3) -0.082(3) -0.046(3) F10 0.161(5) 0.104(3) 0.298(7) 0.089(4) 0.152(5) 0.016(3) F11 0.068(3) 0.250(6) 0.227(6) -0.032(5) 0.008(3) -0.079(3) F12 0.097(3) 0.128(4) 0.182(5) -0.025(3) 0.049(3) -0.041(3) F13 0.087(2) 0.119(3) 0.101(3) 0.027(2) 0.013(2) -0.042(2) F14 0.080(2) 0.111(3) 0.148(4) 0.011(3) 0.035(2) 0.003(2) F15 0.089(3) 0.298(7) 0.150(4) -0.023(4) 0.009(3) -0.126(4) F16 0.080(2) 0.100(2) 0.112(3) -0.043(2) -0.0013(19) -0.024(2) F17 0.090(2) 0.202(4) 0.118(3) -0.080(3) -0.019(2) -0.054(3) F18 0.109(3) 0.126(3) 0.061(2) 0.003(2) -0.0103(19) -0.021(2) F19 0.104(3) 0.217(6) 0.179(5) -0.011(4) -0.028(3) -0.104(4) F20 0.115(3) 0.107(3) 0.346(8) 0.013(4) -0.057(4) -0.074(3) F21 0.062(2) 0.200(5) 0.220(5) -0.031(4) 0.022(3) -0.070(3) F22 0.145(4) 0.409(10) 0.122(4) -0.102(5) 0.081(4) -0.132(5) F23 0.266(7) 0.123(4) 0.093(3) -0.032(3) 0.032(3) -0.088(4) F24 0.202(5) 0.127(4) 0.077(3) 0.017(3) -0.004(3) -0.025(4) F25 0.148(4) 0.124(3) 0.110(3) -0.009(3) -0.057(3) -0.022(3) F26 0.182(4) 0.139(4) 0.097(3) -0.023(3) -0.031(3) -0.075(3) F27 0.224(5) 0.197(5) 0.054(2) -0.005(3) -0.022(3) -0.098(4) F28 0.127(3) 0.121(3) 0.118(3) 0.000(3) 0.026(2) -0.073(3) F29 0.156(4) 0.254(6) 0.089(3) -0.008(3) 0.054(3) -0.104(4) F30 0.092(3) 0.120(3) 0.123(3) -0.031(3) 0.029(2) -0.025(2) F31 0.360(9) 0.130(4) 0.072(3) -0.029(3) 0.004(4) 0.030(5) F32 0.199(5) 0.312(8) 0.073(3) -0.005(4) 0.006(3) -0.152(6) F33 0.122(3) 0.264(6) 0.085(3) 0.012(3) -0.035(3) -0.056(4) F34 0.085(3) 0.082(3) 0.434(10) -0.003(4) 0.048(4) -0.047(2) F35 0.085(3) 0.156(4) 0.243(7) -0.053(4) 0.047(4) -0.043(3) F36 0.087(3) 0.292(8) 0.206(6) 0.034(6) -0.031(4) -0.084(4) F37 0.071(3) 0.103(3) 0.329(8) -0.012(4) 0.030(4) -0.018(2) F38 0.104(4) 0.274(8) 0.323(10) -0.015(7) -0.054(5) -0.106(5) F39 0.096(3) 0.099(3) 0.316(8) -0.006(4) 0.021(4) -0.059(3) F40 0.118(3) 0.099(3) 0.085(2) 0.004(2) -0.007(2) -0.054(2) F41 0.114(3) 0.177(4) 0.083(3) -0.020(3) -0.033(2) -0.046(3) F42 0.085(2) 0.111(3) 0.107(3) -0.031(2) -0.011(2) -0.019(2) F43 0.178(5) 0.149(4) 0.172(5) -0.085(4) -0.084(4) -0.016(4) F44 0.419(11) 0.199(6) 0.121(4) 0.069(4) -0.167(6) -0.178(7) F45 0.152(5) 0.298(8) 0.159(5) -0.055(5) -0.076(4) -0.081(5) F46 0.084(3) 0.446(11) 0.131(4) -0.003(5) 0.011(3) -0.114(5) F47 0.306(9) 0.136(4) 0.183(6) 0.026(4) 0.110(6) -0.078(5) F48 0.173(5) 0.255(6) 0.091(3) -0.038(4) 0.031(3) -0.131(5) O1 0.078(2) 0.090(3) 0.063(2) -0.0075(19) -0.0150(18) -0.048(2) O2 0.0535(19) 0.083(2) 0.068(2) -0.0015(18) -0.0014(16) -0.0371(18) O3 0.054(2) 0.082(2) 0.082(2) 0.000(2) -0.0024(18) -0.0341(18) O4 0.066(2) 0.082(2) 0.063(2) -0.0042(18) 0.0074(17) -0.0333(19) O5 0.074(2) 0.095(3) 0.0515(19) -0.0052(18) -0.0035(17) -0.044(2) O6 0.068(2) 0.077(3) 0.088(3) -0.004(2) 0.011(2) -0.035(2) O7 0.096(3) 0.076(3) 0.059(2) -0.0022(18) -0.021(2) -0.028(2) O8 0.066(2) 0.092(3) 0.062(2) -0.0049(19) -0.0106(17) -0.036(2) N1 0.048(2) 0.057(2) 0.050(2) 0.0005(18) -0.0035(17) -0.0225(18) N2 0.045(2) 0.063(2) 0.046(2) -0.0006(18) -0.0036(16) -0.0243(18) N3 0.045(2) 0.056(2) 0.066(3) 0.0045(19) -0.0068(18) -0.0207(18) N4 0.046(2) 0.061(2) 0.053(2) 0.0015(19) -0.0042(17) -0.0198(18) N5 0.062(2) 0.064(2) 0.048(2) -0.0078(19) 0.0057(18) -0.027(2) N6 0.076(3) 0.063(3) 0.051(2) -0.006(2) 0.014(2) -0.026(2) N7 0.094(4) 0.054(3) 0.077(3) -0.012(2) 0.015(3) -0.023(2) N8 0.058(2) 0.056(2) 0.082(3) -0.011(2) 0.000(2) -0.021(2) C1 0.073(3) 0.065(3) 0.050(3) -0.002(2) -0.002(2) -0.024(3) C2 0.078(4) 0.073(4) 0.059(3) -0.002(3) 0.012(3) -0.017(3) C3 0.059(3) 0.080(4) 0.080(4) 0.003(3) 0.016(3) -0.015(3) C4 0.051(3) 0.070(3) 0.078(4) 0.007(3) 0.000(3) -0.023(3) C5 0.044(2) 0.052(3) 0.056(3) 0.009(2) -0.003(2) -0.017(2) C6 0.051(3) 0.055(3) 0.053(3) 0.004(2) -0.007(2) -0.023(2) C7 0.061(3) 0.069(3) 0.067(3) -0.005(3) -0.016(3) -0.031(3) C8 0.081(4) 0.076(4) 0.057(3) -0.010(3) -0.017(3) -0.029(3) C9 0.060(3) 0.067(3) 0.049(3) 0.001(2) -0.009(2) -0.023(2) C10 0.083(4) 0.107(5) 0.094(5) -0.009(4) -0.019(4) -0.058(4) C11 0.076(4) 0.098(4) 0.047(3) -0.009(3) 0.005(3) -0.032(4) C12 0.098(5) 0.091(5) 0.092(5) -0.006(4) -0.038(4) -0.045(4) C13 0.081(4) 0.063(3) 0.079(4) 0.005(3) -0.029(3) -0.040(3) C14 0.061(3) 0.083(4) 0.104(5) 0.010(3) -0.029(3) -0.040(3) C15 0.055(3) 0.064(3) 0.085(4) 0.013(3) -0.006(3) -0.031(3) C16 0.055(4) 0.088(5) 0.147(7) -0.006(5) 0.021(4) -0.034(3) C17 0.066(3) 0.065(3) 0.073(4) -0.007(3) -0.011(3) -0.028(3) C18 0.091(4) 0.079(4) 0.069(4) -0.013(3) -0.018(3) -0.033(3) C19 0.097(4) 0.087(4) 0.053(3) -0.009(3) -0.002(3) -0.027(4) C20 0.073(3) 0.081(4) 0.061(3) 0.005(3) 0.004(3) -0.028(3) C21 0.051(3) 0.054(3) 0.057(3) 0.005(2) -0.005(2) -0.017(2) C22 0.045(2) 0.052(3) 0.056(3) 0.007(2) -0.005(2) -0.018(2) C23 0.050(3) 0.072(3) 0.075(4) 0.014(3) -0.010(2) -0.025(3) C24 0.052(3) 0.085(4) 0.088(4) 0.001(3) -0.016(3) -0.033(3) C25 0.055(3) 0.068(3) 0.067(3) -0.003(3) -0.013(2) -0.024(2) C26 0.053(3) 0.107(5) 0.096(5) 0.010(4) -0.004(3) -0.030(4) C27 0.065(4) 0.097(5) 0.081(4) -0.025(4) -0.012(3) -0.026(3) C28 0.063(4) 0.117(6) 0.145(7) 0.009(5) -0.007(4) -0.051(4) C29 0.043(3) 0.061(3) 0.120(5) 0.007(3) 0.005(3) -0.018(2) C30 0.065(4) 0.086(4) 0.093(5) 0.002(4) 0.021(3) -0.031(3) C31 0.062(3) 0.061(3) 0.075(4) 0.009(3) 0.008(3) -0.016(3) C32 0.098(5) 0.090(5) 0.074(4) -0.001(4) 0.024(4) -0.022(4) C33 0.075(3) 0.077(4) 0.049(3) -0.007(3) 0.007(2) -0.036(3) C34 0.067(4) 0.091(4) 0.070(4) -0.010(3) 0.010(3) -0.032(3) C35 0.060(3) 0.078(4) 0.092(4) -0.007(3) -0.001(3) -0.022(3) C36 0.073(4) 0.073(4) 0.068(3) -0.009(3) -0.011(3) -0.024(3) C37 0.074(3) 0.051(3) 0.050(3) -0.007(2) -0.002(2) -0.022(2) C38 0.088(4) 0.055(3) 0.050(3) -0.004(2) 0.000(3) -0.024(3) C39 0.113(5) 0.071(4) 0.054(3) -0.007(3) -0.007(3) -0.028(3) C40 0.124(5) 0.091(4) 0.049(3) -0.010(3) 0.017(4) -0.035(4) C41 0.092(4) 0.076(4) 0.059(3) -0.008(3) 0.023(3) -0.029(3) C42 0.156(7) 0.115(6) 0.058(4) -0.020(4) -0.017(4) -0.053(6) C43 0.114(6) 0.118(6) 0.066(4) -0.010(4) 0.030(4) -0.049(5) C44 0.090(5) 0.140(7) 0.072(4) -0.026(4) -0.019(4) -0.043(5) C45 0.078(4) 0.071(4) 0.069(4) -0.013(3) -0.006(3) -0.030(3) C46 0.074(4) 0.088(4) 0.093(5) -0.014(4) -0.014(3) -0.035(3) C47 0.065(3) 0.064(3) 0.102(5) -0.009(3) 0.002(3) -0.031(3) C48 0.057(4) 0.099(6) 0.163(8) -0.019(5) 0.006(5) -0.028(4) C49 0.131(6) 0.076(4) 0.082(5) -0.009(4) 0.032(4) -0.039(4) C50 0.194(10) 0.093(6) 0.093(6) -0.009(4) 0.045(7) -0.041(7) C51 0.130(7) 0.093(5) 0.143(8) -0.006(5) 0.073(7) -0.032(5) C52 0.109(6) 0.078(5) 0.135(7) -0.002(5) 0.034(5) -0.031(4) C53 0.073(4) 0.051(3) 0.123(6) -0.002(3) 0.026(4) -0.022(3) C54 0.073(4) 0.055(3) 0.101(5) -0.003(3) -0.002(3) -0.022(3) C55 0.061(4) 0.058(3) 0.157(7) -0.005(4) -0.015(4) -0.023(3) C56 0.077(4) 0.089(5) 0.126(6) -0.013(4) -0.027(4) -0.035(4) C57 0.067(3) 0.066(3) 0.090(4) -0.010(3) -0.023(3) -0.024(3) C58 0.075(5) 0.109(7) 0.240(12) -0.017(7) -0.019(6) -0.042(5) C59 0.081(4) 0.091(5) 0.071(4) -0.007(3) -0.021(3) -0.026(4) C60 0.120(6) 0.131(7) 0.098(6) -0.015(5) -0.045(5) -0.060(5) C61 0.094(5) 0.059(3) 0.088(5) -0.003(3) -0.045(4) -0.019(3) C62 0.068(3) 0.084(4) 0.085(4) -0.006(3) -0.021(3) -0.026(3) C63 0.064(3) 0.067(3) 0.076(4) -0.002(3) -0.014(3) -0.025(3) C64 0.097(5) 0.161(8) 0.081(5) 0.009(5) -0.014(4) -0.081(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.989(4) . ? Pd1 O1 1.994(3) . ? Pd1 O2 1.997(3) . ? Pd1 N1 2.009(4) . ? Pd2 N4 1.977(4) . ? Pd2 N3 1.984(4) . ? Pd2 O3 1.997(3) . ? Pd2 O4 2.000(3) . ? Pd3 N6 1.988(4) . ? Pd3 O5 1.990(3) . ? Pd3 N5 2.005(4) . ? Pd3 O6 2.009(4) . ? Pd4 N7 1.975(5) . ? Pd4 O8 2.000(4) . ? Pd4 N8 2.005(4) . ? Pd4 O7 2.010(4) . ? F1 C10 1.342(7) . ? F2 C10 1.331(7) . ? F3 C10 1.320(7) . ? F4 C11 1.334(6) . ? F5 C11 1.342(6) . ? F6 C11 1.338(6) . ? F7 C12 1.269(8) . ? F8 C12 1.299(7) . ? F9 C12 1.302(7) . ? F10 C16 1.191(8) . ? F11 C16 1.334(8) . ? F12 C16 1.306(8) . ? F13 C26 1.337(7) . ? F14 C26 1.330(7) . ? F15 C26 1.323(7) . ? F16 C27 1.363(6) . ? F17 C27 1.333(6) . ? F18 C27 1.343(7) . ? F19 C28 1.314(9) . ? F20 C28 1.303(8) . ? F21 C28 1.310(8) . ? F22 C32 1.268(7) . ? F23 C32 1.292(8) . ? F24 C32 1.309(7) . ? F25 C42 1.333(8) . ? F26 C42 1.335(8) . ? F27 C42 1.332(8) . ? F28 C43 1.341(8) . ? F29 C43 1.333(7) . ? F30 C43 1.338(8) . ? F31 C44 1.249(8) . ? F32 C44 1.339(8) . ? F33 C44 1.249(7) . ? F34 C48 1.234(8) . ? F35 C48 1.319(9) . ? F36 C48 1.301(9) . ? F37 C58 1.351(10) . ? F38 C58 1.311(12) . ? F39 C58 1.323(10) . ? F40 C59 1.311(7) . ? F41 C59 1.352(6) . ? F42 C59 1.341(7) . ? F43 C60 1.294(9) . ? F44 C60 1.207(9) . ? F45 C60 1.337(10) . ? F46 C64 1.249(8) . ? F47 C64 1.273(9) . ? F48 C64 1.286(8) . ? O1 C13 1.260(6) . ? O2 C15 1.260(6) . ? O3 C29 1.279(6) . ? O4 C31 1.251(6) . ? O5 C45 1.262(6) . ? O6 C47 1.256(7) . ? O7 C61 1.281(7) . ? O8 C63 1.265(6) . ? N1 C1 1.347(6) . ? N1 C5 1.351(6) . ? N2 C9 1.373(6) . ? N2 C6 1.375(5) . ? N3 C17 1.341(6) . ? N3 C21 1.367(6) . ? N4 C25 1.389(6) . ? N4 C22 1.397(6) . ? N5 C33 1.332(6) . ? N5 C37 1.357(6) . ? N6 C41 1.372(6) . ? N6 C38 1.379(7) . ? N7 C49 1.328(8) . ? N7 C53 1.369(8) . ? N8 C54 1.347(7) . ? N8 C57 1.380(7) . ? C1 C2 1.378(7) . ? C2 C3 1.367(8) . ? C3 C4 1.365(8) . ? C4 C5 1.388(6) . ? C5 C6 1.455(6) . ? C6 C7 1.400(6) . ? C7 C8 1.392(7) . ? C7 C10 1.482(7) . ? C8 C9 1.362(7) . ? C9 C11 1.484(7) . ? C12 C13 1.522(8) . ? C13 C14 1.379(8) . ? C14 C15 1.381(8) . ? C15 C16 1.549(8) . ? C17 C18 1.385(7) . ? C18 C19 1.363(8) . ? C19 C20 1.380(8) . ? C20 C21 1.380(7) . ? C21 C22 1.442(6) . ? C22 C23 1.385(6) . ? C23 C24 1.397(8) . ? C23 C26 1.483(8) . ? C24 C25 1.362(7) . ? C25 C27 1.461(8) . ? C28 C29 1.519(9) . ? C29 C30 1.357(8) . ? C30 C31 1.375(8) . ? C31 C32 1.517(8) . ? C33 C34 1.377(7) . ? C34 C35 1.366(8) . ? C35 C36 1.377(8) . ? C36 C37 1.372(7) . ? C37 C38 1.454(7) . ? C38 C39 1.394(7) . ? C39 C40 1.403(9) . ? C39 C42 1.481(9) . ? C40 C41 1.357(8) . ? C41 C43 1.485(9) . ? C44 C45 1.507(8) . ? C45 C46 1.389(8) . ? C46 C47 1.369(8) . ? C47 C48 1.528(8) . ? C49 C50 1.383(10) . ? C50 C51 1.359(12) . ? C51 C52 1.386(12) . ? C52 C53 1.375(9) . ? C53 C54 1.451(9) . ? C54 C55 1.411(9) . ? C55 C56 1.374(9) . ? C55 C58 1.503(10) . ? C56 C57 1.352(8) . ? C57 C59 1.471(8) . ? C60 C61 1.534(8) . ? C61 C62 1.365(9) . ? C62 C63 1.378(7) . ? C63 C64 1.507(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 O1 171.94(14) . . ? N2 Pd1 O2 95.97(14) . . ? O1 Pd1 O2 92.08(15) . . ? N2 Pd1 N1 81.17(15) . . ? O1 Pd1 N1 90.78(15) . . ? O2 Pd1 N1 177.14(15) . . ? N4 Pd2 N3 81.24(15) . . ? N4 Pd2 O3 172.27(16) . . ? N3 Pd2 O3 91.14(15) . . ? N4 Pd2 O4 95.96(15) . . ? N3 Pd2 O4 176.38(15) . . ? O3 Pd2 O4 91.60(15) . . ? N6 Pd3 O5 171.82(16) . . ? N6 Pd3 N5 81.15(17) . . ? O5 Pd3 N5 90.69(15) . . ? N6 Pd3 O6 96.79(18) . . ? O5 Pd3 O6 91.37(16) . . ? N5 Pd3 O6 177.80(16) . . ? N7 Pd4 O8 177.26(19) . . ? N7 Pd4 N8 81.1(2) . . ? O8 Pd4 N8 96.28(16) . . ? N7 Pd4 O7 91.7(2) . . ? O8 Pd4 O7 90.93(16) . . ? N8 Pd4 O7 172.27(17) . . ? C13 O1 Pd1 123.9(4) . . ? C15 O2 Pd1 123.6(4) . . ? C29 O3 Pd2 123.3(4) . . ? C31 O4 Pd2 124.1(4) . . ? C45 O5 Pd3 124.9(3) . . ? C47 O6 Pd3 123.7(4) . . ? C61 O7 Pd4 123.7(4) . . ? C63 O8 Pd4 124.6(3) . . ? C1 N1 C5 120.8(4) . . ? C1 N1 Pd1 123.8(3) . . ? C5 N1 Pd1 115.4(3) . . ? C9 N2 C6 106.8(4) . . ? C9 N2 Pd1 139.5(3) . . ? C6 N2 Pd1 113.7(3) . . ? C17 N3 C21 119.6(4) . . ? C17 N3 Pd2 124.5(3) . . ? C21 N3 Pd2 115.8(3) . . ? C25 N4 C22 106.4(4) . . ? C25 N4 Pd2 139.3(3) . . ? C22 N4 Pd2 114.2(3) . . ? C33 N5 C37 120.6(4) . . ? C33 N5 Pd3 123.9(3) . . ? C37 N5 Pd3 115.5(3) . . ? C41 N6 C38 107.1(5) . . ? C41 N6 Pd3 139.0(4) . . ? C38 N6 Pd3 113.9(3) . . ? C49 N7 C53 121.1(6) . . ? C49 N7 Pd4 123.4(5) . . ? C53 N7 Pd4 115.5(4) . . ? C54 N8 C57 107.3(5) . . ? C54 N8 Pd4 113.9(4) . . ? C57 N8 Pd4 138.8(4) . . ? N1 C1 C2 121.2(5) . . ? C3 C2 C1 118.6(5) . . ? C4 C3 C2 120.0(5) . . ? C3 C4 C5 120.6(5) . . ? N1 C5 C4 118.8(4) . . ? N1 C5 C6 113.7(4) . . ? C4 C5 C6 127.6(5) . . ? N2 C6 C7 109.0(4) . . ? N2 C6 C5 116.0(4) . . ? C7 C6 C5 135.0(4) . . ? C8 C7 C6 106.4(4) . . ? C8 C7 C10 124.4(5) . . ? C6 C7 C10 129.2(5) . . ? C9 C8 C7 107.9(4) . . ? C8 C9 N2 109.9(4) . . ? C8 C9 C11 125.7(5) . . ? N2 C9 C11 124.4(4) . . ? F3 C10 F2 106.5(5) . . ? F3 C10 F1 106.7(6) . . ? F2 C10 F1 105.5(6) . . ? F3 C10 C7 111.7(6) . . ? F2 C10 C7 112.8(5) . . ? F1 C10 C7 113.3(5) . . ? F4 C11 F6 106.9(5) . . ? F4 C11 F5 106.3(5) . . ? F6 C11 F5 105.8(5) . . ? F4 C11 C9 113.2(5) . . ? F6 C11 C9 109.7(5) . . ? F5 C11 C9 114.5(5) . . ? F7 C12 F8 110.4(7) . . ? F7 C12 F9 104.9(6) . . ? F8 C12 F9 105.8(5) . . ? F7 C12 C13 112.3(5) . . ? F8 C12 C13 109.4(5) . . ? F9 C12 C13 113.8(6) . . ? O1 C13 C14 128.4(5) . . ? O1 C13 C12 113.0(6) . . ? C14 C13 C12 118.6(5) . . ? C13 C14 C15 123.2(5) . . ? O2 C15 C14 128.7(5) . . ? O2 C15 C16 112.1(5) . . ? C14 C15 C16 119.1(5) . . ? F10 C16 F12 109.9(8) . . ? F10 C16 F11 111.4(6) . . ? F12 C16 F11 98.4(6) . . ? F10 C16 C15 114.2(6) . . ? F12 C16 C15 111.4(5) . . ? F11 C16 C15 110.4(7) . . ? N3 C17 C18 121.4(5) . . ? C19 C18 C17 119.6(5) . . ? C18 C19 C20 119.1(5) . . ? C21 C20 C19 120.3(5) . . ? N3 C21 C20 119.9(5) . . ? N3 C21 C22 113.7(4) . . ? C20 C21 C22 126.3(5) . . ? C23 C22 N4 108.7(4) . . ? C23 C22 C21 136.5(5) . . ? N4 C22 C21 114.8(4) . . ? C22 C23 C24 107.3(5) . . ? C22 C23 C26 128.4(5) . . ? C24 C23 C26 124.3(5) . . ? C25 C24 C23 108.1(5) . . ? C24 C25 N4 109.6(5) . . ? C24 C25 C27 126.3(5) . . ? N4 C25 C27 124.0(5) . . ? F15 C26 F14 108.4(5) . . ? F15 C26 F13 105.3(5) . . ? F14 C26 F13 104.4(6) . . ? F15 C26 C23 111.5(6) . . ? F14 C26 C23 114.3(5) . . ? F13 C26 C23 112.3(5) . . ? F17 C27 F18 107.4(5) . . ? F17 C27 F16 105.5(5) . . ? F18 C27 F16 106.2(5) . . ? F17 C27 C25 109.8(5) . . ? F18 C27 C25 114.0(5) . . ? F16 C27 C25 113.5(5) . . ? F20 C28 F21 109.8(6) . . ? F20 C28 F19 105.8(8) . . ? F21 C28 F19 104.8(7) . . ? F20 C28 C29 109.6(6) . . ? F21 C28 C29 113.4(7) . . ? F19 C28 C29 113.1(6) . . ? O3 C29 C30 128.6(5) . . ? O3 C29 C28 111.2(6) . . ? C30 C29 C28 120.1(6) . . ? C29 C30 C31 123.8(5) . . ? O4 C31 C30 128.3(6) . . ? O4 C31 C32 112.1(5) . . ? C30 C31 C32 119.5(5) . . ? F22 C32 F23 108.2(7) . . ? F22 C32 F24 105.7(7) . . ? F23 C32 F24 103.0(7) . . ? F22 C32 C31 115.4(7) . . ? F23 C32 C31 113.7(6) . . ? F24 C32 C31 109.9(5) . . ? N5 C33 C34 121.3(5) . . ? C35 C34 C33 118.8(5) . . ? C34 C35 C36 119.8(5) . . ? C37 C36 C35 119.9(5) . . ? N5 C37 C36 119.6(5) . . ? N5 C37 C38 113.6(5) . . ? C36 C37 C38 126.8(5) . . ? N6 C38 C39 108.6(5) . . ? N6 C38 C37 115.9(4) . . ? C39 C38 C37 135.5(6) . . ? C38 C39 C40 106.6(6) . . ? C38 C39 C42 128.4(6) . . ? C40 C39 C42 124.9(6) . . ? C41 C40 C39 107.6(5) . . ? C40 C41 N6 110.0(6) . . ? C40 C41 C43 126.5(5) . . ? N6 C41 C43 123.5(6) . . ? F25 C42 F27 108.2(7) . . ? F25 C42 F26 104.9(7) . . ? F27 C42 F26 105.1(6) . . ? F25 C42 C39 113.9(6) . . ? F27 C42 C39 110.9(7) . . ? F26 C42 C39 113.2(6) . . ? F29 C43 F30 106.3(6) . . ? F29 C43 F28 106.4(6) . . ? F30 C43 F28 106.7(6) . . ? F29 C43 C41 109.3(6) . . ? F30 C43 C41 114.6(6) . . ? F28 C43 C41 113.1(6) . . ? F33 C44 F31 112.8(7) . . ? F33 C44 F32 100.6(7) . . ? F31 C44 F32 102.2(7) . . ? F33 C44 C45 117.1(6) . . ? F31 C44 C45 112.7(7) . . ? F32 C44 C45 109.5(5) . . ? O5 C45 C46 127.6(5) . . ? O5 C45 C44 113.3(5) . . ? C46 C45 C44 119.0(6) . . ? C47 C46 C45 123.1(6) . . ? O6 C47 C46 129.2(5) . . ? O6 C47 C48 112.3(6) . . ? C46 C47 C48 118.4(7) . . ? F34 C48 F36 109.5(8) . . ? F34 C48 F35 108.2(8) . . ? F36 C48 F35 98.9(6) . . ? F34 C48 C47 113.6(6) . . ? F36 C48 C47 113.3(7) . . ? F35 C48 C47 112.3(6) . . ? N7 C49 C50 121.1(8) . . ? C51 C50 C49 119.0(9) . . ? C50 C51 C52 120.0(8) . . ? C53 C52 C51 119.8(8) . . ? N7 C53 C52 119.0(7) . . ? N7 C53 C54 113.4(5) . . ? C52 C53 C54 127.5(7) . . ? N8 C54 C55 108.2(6) . . ? N8 C54 C53 116.0(5) . . ? C55 C54 C53 135.7(6) . . ? C56 C55 C54 107.1(6) . . ? C56 C55 C58 126.8(8) . . ? C54 C55 C58 126.1(8) . . ? C57 C56 C55 107.5(6) . . ? C56 C57 N8 109.9(6) . . ? C56 C57 C59 125.6(6) . . ? N8 C57 C59 124.4(5) . . ? F38 C58 F39 106.7(8) . . ? F38 C58 F37 106.8(8) . . ? F39 C58 F37 105.2(9) . . ? F38 C58 C55 108.7(9) . . ? F39 C58 C55 114.7(7) . . ? F37 C58 C55 114.3(7) . . ? F40 C59 F42 107.4(5) . . ? F40 C59 F41 106.2(5) . . ? F42 C59 F41 105.6(5) . . ? F40 C59 C57 114.0(5) . . ? F42 C59 C57 113.6(5) . . ? F41 C59 C57 109.4(5) . . ? F44 C60 F43 111.8(9) . . ? F44 C60 F45 106.3(8) . . ? F43 C60 F45 102.3(7) . . ? F44 C60 C61 114.6(7) . . ? F43 C60 C61 110.0(6) . . ? F45 C60 C61 111.1(7) . . ? O7 C61 C62 128.7(5) . . ? O7 C61 C60 110.5(7) . . ? C62 C61 C60 120.8(7) . . ? C61 C62 C63 123.0(6) . . ? O8 C63 C62 128.6(6) . . ? O8 C63 C64 114.4(5) . . ? C62 C63 C64 117.0(5) . . ? F46 C64 F47 109.3(7) . . ? F46 C64 F48 105.1(8) . . ? F47 C64 F48 103.2(7) . . ? F46 C64 C63 115.1(6) . . ? F47 C64 C63 109.9(7) . . ? F48 C64 C63 113.6(6) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 O1 C13 -174.4(9) . . . . ? O2 Pd1 O1 C13 3.3(4) . . . . ? N1 Pd1 O1 C13 -176.7(4) . . . . ? N2 Pd1 O2 C15 178.9(4) . . . . ? O1 Pd1 O2 C15 -0.8(4) . . . . ? N1 Pd1 O2 C15 178(100) . . . . ? N4 Pd2 O3 C29 162.8(10) . . . . ? N3 Pd2 O3 C29 172.8(4) . . . . ? O4 Pd2 O3 C29 -4.8(4) . . . . ? N4 Pd2 O4 C31 -173.5(4) . . . . ? N3 Pd2 O4 C31 -134(2) . . . . ? O3 Pd2 O4 C31 4.9(4) . . . . ? N6 Pd3 O5 C45 179(37) . . . . ? N5 Pd3 O5 C45 -176.6(4) . . . . ? O6 Pd3 O5 C45 2.6(4) . . . . ? N6 Pd3 O6 C47 -179.2(4) . . . . ? O5 Pd3 O6 C47 0.2(4) . . . . ? N5 Pd3 O6 C47 160(4) . . . . ? N7 Pd4 O7 C61 -171.8(4) . . . . ? O8 Pd4 O7 C61 7.4(4) . . . . ? N8 Pd4 O7 C61 -151.6(11) . . . . ? N7 Pd4 O8 C63 158(3) . . . . ? N8 Pd4 O8 C63 171.4(4) . . . . ? O7 Pd4 O8 C63 -5.8(4) . . . . ? N2 Pd1 N1 C1 178.0(4) . . . . ? O1 Pd1 N1 C1 -2.3(4) . . . . ? O2 Pd1 N1 C1 179(100) . . . . ? N2 Pd1 N1 C5 -1.1(3) . . . . ? O1 Pd1 N1 C5 178.5(3) . . . . ? O2 Pd1 N1 C5 -1(3) . . . . ? O1 Pd1 N2 C9 179(35) . . . . ? O2 Pd1 N2 C9 1.3(5) . . . . ? N1 Pd1 N2 C9 -178.7(5) . . . . ? O1 Pd1 N2 C6 -0.9(12) . . . . ? O2 Pd1 N2 C6 -178.6(3) . . . . ? N1 Pd1 N2 C6 1.4(3) . . . . ? N4 Pd2 N3 C17 177.3(4) . . . . ? O3 Pd2 N3 C17 -1.3(4) . . . . ? O4 Pd2 N3 C17 138(2) . . . . ? N4 Pd2 N3 C21 -1.4(3) . . . . ? O3 Pd2 N3 C21 180.0(3) . . . . ? O4 Pd2 N3 C21 -41(2) . . . . ? N3 Pd2 N4 C25 178.7(5) . . . . ? O3 Pd2 N4 C25 -171.2(9) . . . . ? O4 Pd2 N4 C25 -3.7(5) . . . . ? N3 Pd2 N4 C22 3.5(3) . . . . ? O3 Pd2 N4 C22 13.6(13) . . . . ? O4 Pd2 N4 C22 -178.8(3) . . . . ? N6 Pd3 N5 C33 178.9(4) . . . . ? O5 Pd3 N5 C33 -0.5(4) . . . . ? O6 Pd3 N5 C33 -161(4) . . . . ? N6 Pd3 N5 C37 -1.7(3) . . . . ? O5 Pd3 N5 C37 179.0(3) . . . . ? O6 Pd3 N5 C37 19(4) . . . . ? O5 Pd3 N6 C41 -174.3(9) . . . . ? N5 Pd3 N6 C41 -179.0(6) . . . . ? O6 Pd3 N6 C41 1.8(6) . . . . ? O5 Pd3 N6 C38 6.4(13) . . . . ? N5 Pd3 N6 C38 1.8(3) . . . . ? O6 Pd3 N6 C38 -177.4(3) . . . . ? O8 Pd4 N7 C49 -164(3) . . . . ? N8 Pd4 N7 C49 -177.6(5) . . . . ? O7 Pd4 N7 C49 -0.3(5) . . . . ? O8 Pd4 N7 C53 16(4) . . . . ? N8 Pd4 N7 C53 1.8(4) . . . . ? O7 Pd4 N7 C53 179.1(4) . . . . ? N7 Pd4 N8 C54 -1.9(4) . . . . ? O8 Pd4 N8 C54 178.7(4) . . . . ? O7 Pd4 N8 C54 -22.4(13) . . . . ? N7 Pd4 N8 C57 177.7(5) . . . . ? O8 Pd4 N8 C57 -1.6(5) . . . . ? O7 Pd4 N8 C57 157.3(10) . . . . ? C5 N1 C1 C2 -2.4(7) . . . . ? Pd1 N1 C1 C2 178.5(4) . . . . ? N1 C1 C2 C3 1.0(8) . . . . ? C1 C2 C3 C4 0.8(8) . . . . ? C2 C3 C4 C5 -1.2(8) . . . . ? C1 N1 C5 C4 1.9(6) . . . . ? Pd1 N1 C5 C4 -179.0(3) . . . . ? C1 N1 C5 C6 -178.5(4) . . . . ? Pd1 N1 C5 C6 0.7(5) . . . . ? C3 C4 C5 N1 -0.1(7) . . . . ? C3 C4 C5 C6 -179.7(5) . . . . ? C9 N2 C6 C7 -0.8(5) . . . . ? Pd1 N2 C6 C7 179.2(3) . . . . ? C9 N2 C6 C5 178.6(4) . . . . ? Pd1 N2 C6 C5 -1.5(5) . . . . ? N1 C5 C6 N2 0.5(6) . . . . ? C4 C5 C6 N2 -179.9(4) . . . . ? N1 C5 C6 C7 179.7(5) . . . . ? C4 C5 C6 C7 -0.7(9) . . . . ? N2 C6 C7 C8 0.4(5) . . . . ? C5 C6 C7 C8 -178.8(5) . . . . ? N2 C6 C7 C10 179.3(6) . . . . ? C5 C6 C7 C10 0.1(10) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? C10 C7 C8 C9 -178.9(5) . . . . ? C7 C8 C9 N2 -0.6(6) . . . . ? C7 C8 C9 C11 178.2(5) . . . . ? C6 N2 C9 C8 0.9(5) . . . . ? Pd1 N2 C9 C8 -179.0(4) . . . . ? C6 N2 C9 C11 -178.0(5) . . . . ? Pd1 N2 C9 C11 2.1(8) . . . . ? C8 C7 C10 F3 1.5(9) . . . . ? C6 C7 C10 F3 -177.3(5) . . . . ? C8 C7 C10 F2 -118.3(6) . . . . ? C6 C7 C10 F2 62.9(8) . . . . ? C8 C7 C10 F1 122.0(6) . . . . ? C6 C7 C10 F1 -56.8(8) . . . . ? C8 C9 C11 F4 -120.4(6) . . . . ? N2 C9 C11 F4 58.3(7) . . . . ? C8 C9 C11 F6 -1.1(8) . . . . ? N2 C9 C11 F6 177.6(5) . . . . ? C8 C9 C11 F5 117.7(6) . . . . ? N2 C9 C11 F5 -63.7(7) . . . . ? Pd1 O1 C13 C14 -2.8(8) . . . . ? Pd1 O1 C13 C12 -179.8(4) . . . . ? F7 C12 C13 O1 -39.2(8) . . . . ? F8 C12 C13 O1 83.7(7) . . . . ? F9 C12 C13 O1 -158.2(5) . . . . ? F7 C12 C13 C14 143.5(6) . . . . ? F8 C12 C13 C14 -93.6(7) . . . . ? F9 C12 C13 C14 24.5(8) . . . . ? O1 C13 C14 C15 -1.1(10) . . . . ? C12 C13 C14 C15 175.7(5) . . . . ? Pd1 O2 C15 C14 -2.5(8) . . . . ? Pd1 O2 C15 C16 174.0(4) . . . . ? C13 C14 C15 O2 4.2(9) . . . . ? C13 C14 C15 C16 -172.1(5) . . . . ? O2 C15 C16 F10 -78.5(9) . . . . ? C14 C15 C16 F10 98.4(9) . . . . ? O2 C15 C16 F12 46.7(8) . . . . ? C14 C15 C16 F12 -136.4(6) . . . . ? O2 C15 C16 F11 155.0(6) . . . . ? C14 C15 C16 F11 -28.1(8) . . . . ? C21 N3 C17 C18 0.8(7) . . . . ? Pd2 N3 C17 C18 -177.9(4) . . . . ? N3 C17 C18 C19 0.7(8) . . . . ? C17 C18 C19 C20 -1.2(9) . . . . ? C18 C19 C20 C21 0.4(8) . . . . ? C17 N3 C21 C20 -1.6(7) . . . . ? Pd2 N3 C21 C20 177.2(4) . . . . ? C17 N3 C21 C22 -179.7(4) . . . . ? Pd2 N3 C21 C22 -0.9(5) . . . . ? C19 C20 C21 N3 1.0(8) . . . . ? C19 C20 C21 C22 178.9(5) . . . . ? C25 N4 C22 C23 -0.7(5) . . . . ? Pd2 N4 C22 C23 176.1(3) . . . . ? C25 N4 C22 C21 178.3(4) . . . . ? Pd2 N4 C22 C21 -5.0(5) . . . . ? N3 C21 C22 C23 -177.6(5) . . . . ? C20 C21 C22 C23 4.4(9) . . . . ? N3 C21 C22 N4 3.8(6) . . . . ? C20 C21 C22 N4 -174.1(4) . . . . ? N4 C22 C23 C24 0.6(6) . . . . ? C21 C22 C23 C24 -178.1(5) . . . . ? N4 C22 C23 C26 -177.6(5) . . . . ? C21 C22 C23 C26 3.8(10) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C26 C23 C24 C25 178.0(5) . . . . ? C23 C24 C25 N4 -0.1(6) . . . . ? C23 C24 C25 C27 176.7(5) . . . . ? C22 N4 C25 C24 0.5(5) . . . . ? Pd2 N4 C25 C24 -174.9(4) . . . . ? C22 N4 C25 C27 -176.4(5) . . . . ? Pd2 N4 C25 C27 8.2(8) . . . . ? C22 C23 C26 F15 174.3(6) . . . . ? C24 C23 C26 F15 -3.6(9) . . . . ? C22 C23 C26 F14 -62.3(8) . . . . ? C24 C23 C26 F14 119.8(6) . . . . ? C22 C23 C26 F13 56.5(8) . . . . ? C24 C23 C26 F13 -121.4(6) . . . . ? C24 C25 C27 F17 0.9(9) . . . . ? N4 C25 C27 F17 177.3(5) . . . . ? C24 C25 C27 F18 -119.6(6) . . . . ? N4 C25 C27 F18 56.8(7) . . . . ? C24 C25 C27 F16 118.7(6) . . . . ? N4 C25 C27 F16 -64.9(7) . . . . ? Pd2 O3 C29 C30 4.2(8) . . . . ? Pd2 O3 C29 C28 -172.9(4) . . . . ? F20 C28 C29 O3 86.0(8) . . . . ? F21 C28 C29 O3 -151.0(6) . . . . ? F19 C28 C29 O3 -31.9(9) . . . . ? F20 C28 C29 C30 -91.4(8) . . . . ? F21 C28 C29 C30 31.7(10) . . . . ? F19 C28 C29 C30 150.8(7) . . . . ? O3 C29 C30 C31 -1.6(10) . . . . ? C28 C29 C30 C31 175.2(6) . . . . ? Pd2 O4 C31 C30 -4.2(8) . . . . ? Pd2 O4 C31 C32 174.0(4) . . . . ? C29 C30 C31 O4 1.6(10) . . . . ? C29 C30 C31 C32 -176.5(6) . . . . ? O4 C31 C32 F22 171.2(7) . . . . ? C30 C31 C32 F22 -10.4(10) . . . . ? O4 C31 C32 F23 45.3(8) . . . . ? C30 C31 C32 F23 -136.3(6) . . . . ? O4 C31 C32 F24 -69.5(7) . . . . ? C30 C31 C32 F24 108.9(7) . . . . ? C37 N5 C33 C34 -1.0(8) . . . . ? Pd3 N5 C33 C34 178.4(4) . . . . ? N5 C33 C34 C35 0.3(8) . . . . ? C33 C34 C35 C36 0.5(9) . . . . ? C34 C35 C36 C37 -0.6(8) . . . . ? C33 N5 C37 C36 0.8(7) . . . . ? Pd3 N5 C37 C36 -178.6(4) . . . . ? C33 N5 C37 C38 -179.3(4) . . . . ? Pd3 N5 C37 C38 1.3(5) . . . . ? C35 C36 C37 N5 -0.1(8) . . . . ? C35 C36 C37 C38 -179.9(5) . . . . ? C41 N6 C38 C39 -0.4(6) . . . . ? Pd3 N6 C38 C39 179.1(3) . . . . ? C41 N6 C38 C37 178.8(4) . . . . ? Pd3 N6 C38 C37 -1.7(5) . . . . ? N5 C37 C38 N6 0.3(6) . . . . ? C36 C37 C38 N6 -179.9(5) . . . . ? N5 C37 C38 C39 179.2(6) . . . . ? C36 C37 C38 C39 -0.9(10) . . . . ? N6 C38 C39 C40 0.4(6) . . . . ? C37 C38 C39 C40 -178.6(6) . . . . ? N6 C38 C39 C42 -179.7(6) . . . . ? C37 C38 C39 C42 1.3(11) . . . . ? C38 C39 C40 C41 -0.2(7) . . . . ? C42 C39 C40 C41 179.8(6) . . . . ? C39 C40 C41 N6 0.0(7) . . . . ? C39 C40 C41 C43 178.3(6) . . . . ? C38 N6 C41 C40 0.2(6) . . . . ? Pd3 N6 C41 C40 -179.0(4) . . . . ? C38 N6 C41 C43 -178.2(6) . . . . ? Pd3 N6 C41 C43 2.6(9) . . . . ? C38 C39 C42 F25 -59.3(10) . . . . ? C40 C39 C42 F25 120.6(7) . . . . ? C38 C39 C42 F27 178.3(6) . . . . ? C40 C39 C42 F27 -1.8(10) . . . . ? C38 C39 C42 F26 60.4(9) . . . . ? C40 C39 C42 F26 -119.6(7) . . . . ? C40 C41 C43 F29 -2.2(10) . . . . ? N6 C41 C43 F29 176.0(6) . . . . ? C40 C41 C43 F30 116.9(7) . . . . ? N6 C41 C43 F30 -64.9(8) . . . . ? C40 C41 C43 F28 -120.5(7) . . . . ? N6 C41 C43 F28 57.7(9) . . . . ? Pd3 O5 C45 C46 -3.6(8) . . . . ? Pd3 O5 C45 C44 179.7(4) . . . . ? F33 C44 C45 O5 -157.6(7) . . . . ? F31 C44 C45 O5 69.1(9) . . . . ? F32 C44 C45 O5 -44.0(8) . . . . ? F33 C44 C45 C46 25.4(10) . . . . ? F31 C44 C45 C46 -107.9(8) . . . . ? F32 C44 C45 C46 139.0(6) . . . . ? O5 C45 C46 C47 1.0(10) . . . . ? C44 C45 C46 C47 177.5(6) . . . . ? Pd3 O6 C47 C46 -2.6(9) . . . . ? Pd3 O6 C47 C48 174.5(4) . . . . ? C45 C46 C47 O6 2.5(10) . . . . ? C45 C46 C47 C48 -174.5(6) . . . . ? O6 C47 C48 F34 -76.4(9) . . . . ? C46 C47 C48 F34 101.0(9) . . . . ? O6 C47 C48 F36 157.8(7) . . . . ? C46 C47 C48 F36 -24.7(10) . . . . ? O6 C47 C48 F35 46.7(9) . . . . ? C46 C47 C48 F35 -135.8(7) . . . . ? C53 N7 C49 C50 -0.5(9) . . . . ? Pd4 N7 C49 C50 178.9(5) . . . . ? N7 C49 C50 C51 -0.9(11) . . . . ? C49 C50 C51 C52 1.3(13) . . . . ? C50 C51 C52 C53 -0.3(12) . . . . ? C49 N7 C53 C52 1.4(8) . . . . ? Pd4 N7 C53 C52 -178.0(4) . . . . ? C49 N7 C53 C54 178.1(5) . . . . ? Pd4 N7 C53 C54 -1.4(6) . . . . ? C51 C52 C53 N7 -1.1(10) . . . . ? C51 C52 C53 C54 -177.2(6) . . . . ? C57 N8 C54 C55 0.7(6) . . . . ? Pd4 N8 C54 C55 -179.6(3) . . . . ? C57 N8 C54 C53 -178.0(5) . . . . ? Pd4 N8 C54 C53 1.8(6) . . . . ? N7 C53 C54 N8 -0.3(7) . . . . ? C52 C53 C54 N8 176.0(6) . . . . ? N7 C53 C54 C55 -178.5(6) . . . . ? C52 C53 C54 C55 -2.2(11) . . . . ? N8 C54 C55 C56 0.0(7) . . . . ? C53 C54 C55 C56 178.3(6) . . . . ? N8 C54 C55 C58 178.5(6) . . . . ? C53 C54 C55 C58 -3.3(11) . . . . ? C54 C55 C56 C57 -0.6(7) . . . . ? C58 C55 C56 C57 -179.1(6) . . . . ? C55 C56 C57 N8 1.1(7) . . . . ? C55 C56 C57 C59 -175.7(6) . . . . ? C54 N8 C57 C56 -1.1(6) . . . . ? Pd4 N8 C57 C56 179.2(4) . . . . ? C54 N8 C57 C59 175.8(5) . . . . ? Pd4 N8 C57 C59 -3.9(9) . . . . ? C56 C55 C58 F38 0.4(12) . . . . ? C54 C55 C58 F38 -177.8(7) . . . . ? C56 C55 C58 F39 119.7(10) . . . . ? C54 C55 C58 F39 -58.5(12) . . . . ? C56 C55 C58 F37 -118.8(10) . . . . ? C54 C55 C58 F37 63.0(11) . . . . ? C56 C57 C59 F40 120.4(6) . . . . ? N8 C57 C59 F40 -55.9(8) . . . . ? C56 C57 C59 F42 -116.1(6) . . . . ? N8 C57 C59 F42 67.5(7) . . . . ? C56 C57 C59 F41 1.6(9) . . . . ? N8 C57 C59 F41 -174.7(5) . . . . ? Pd4 O7 C61 C62 -6.7(9) . . . . ? Pd4 O7 C61 C60 171.5(4) . . . . ? F44 C60 C61 O7 49.5(11) . . . . ? F43 C60 C61 O7 -77.5(8) . . . . ? F45 C60 C61 O7 170.0(7) . . . . ? F44 C60 C61 C62 -132.2(9) . . . . ? F43 C60 C61 C62 100.9(9) . . . . ? F45 C60 C61 C62 -11.7(10) . . . . ? O7 C61 C62 C63 1.4(10) . . . . ? C60 C61 C62 C63 -176.6(6) . . . . ? Pd4 O8 C63 C62 3.1(8) . . . . ? Pd4 O8 C63 C64 -174.9(5) . . . . ? C61 C62 C63 O8 0.7(10) . . . . ? C61 C62 C63 C64 178.7(6) . . . . ? O8 C63 C64 F46 -149.4(7) . . . . ? C62 C63 C64 F46 32.3(11) . . . . ? O8 C63 C64 F47 86.8(8) . . . . ? C62 C63 C64 F47 -91.5(8) . . . . ? O8 C63 C64 F48 -28.2(10) . . . . ? C62 C63 C64 F48 153.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.706 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.075