# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jonas Peters' 'Daniel L. M. Suess' _publ_contact_author_name 'Jonas Peters' _publ_contact_author_email JONAS.PETERS@GMAIL.COM _publ_section_title ; Ligand design for site-selective installation of Pd and Pt centers to generate homo- and heteropolymetallic motifs ; # Attachment 'Pd_cifs.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 766171' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.33 H36 Cl1.33 N5.33 O2.67 Pd1.33' _chemical_formula_weight 743.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 5.1225(2) _cell_length_b 17.5023(7) _cell_length_c 24.8571(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.583(2) _cell_angle_gamma 90.00 _cell_volume 2228.46(15) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9813 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 68.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 8.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2373 _exptl_absorpt_correction_T_max 0.4440 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus 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_reflns_number 42087 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0100 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 68.91 _reflns_number_total 3997 _reflns_number_gt 3973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0285P)^2^+2.7202P] 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 3997 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Pd1 Pd 1.74965(3) 0.655982(7) 0.300726(5) 0.01101(6) Uani 1 1 d . . . Cl1 Cl 1.82301(10) 0.57626(3) 0.375487(18) 0.01756(11) Uani 1 1 d . . . N1 N 2.0391(3) 0.60324(9) 0.26056(7) 0.0129(3) Uani 1 1 d . . . N3 N 1.4451(3) 0.72868(9) 0.32207(7) 0.0131(3) Uani 1 1 d . . . C18 C 1.3205(4) 0.73898(11) 0.36861(8) 0.0144(4) Uani 1 1 d . . . N2 N 1.7004(3) 0.70695(10) 0.23067(7) 0.0149(3) Uani 1 1 d . . . C8 C 1.8455(4) 0.67698(12) 0.18926(8) 0.0150(4) Uani 1 1 d . . . C1 C 2.2200(4) 0.55564(11) 0.27932(8) 0.0161(4) Uani 1 1 d . . . H1 H 2.2242 0.5444 0.3167 0.019 Uiso 1 1 calc R . . C11 C 1.5094(4) 0.76227(11) 0.22868(8) 0.0147(4) Uani 1 1 d . . . C19 C 1.4083(4) 0.69422(12) 0.41758(8) 0.0171(4) Uani 1 1 d . . . H19A H 1.3508 0.6405 0.4135 0.021 Uiso 1 1 calc R . . H19B H 1.6015 0.6944 0.4193 0.021 Uiso 1 1 calc R . . C9 C 2.0363(4) 0.62190(11) 0.20648(8) 0.0142(4) Uani 1 1 d . . . C10 C 1.3687(4) 0.77225(11) 0.27758(8) 0.0136(4) Uani 1 1 d . . . C3 C 2.3994(4) 0.53617(12) 0.19174(9) 0.0193(4) Uani 1 1 d . . . H3 H 2.5206 0.5119 0.1686 0.023 Uiso 1 1 calc R . . C6 C 1.9994(5) 0.65572(12) 0.09816(9) 0.0218(5) Uani 1 1 d . . . H6 H 1.9821 0.6665 0.0608 0.026 Uiso 1 1 calc R . . C2 C 2.4056(4) 0.52136(12) 0.24574(9) 0.0192(4) Uani 1 1 d . . . H2 H 2.5344 0.4881 0.2605 0.023 Uiso 1 1 calc R . . C16 C 1.0291(4) 0.83223(12) 0.32969(9) 0.0194(4) Uani 1 1 d . . . H16 H 0.8851 0.8661 0.3327 0.023 Uiso 1 1 calc R . . C4 C 2.2127(4) 0.58753(12) 0.17029(9) 0.0176(4) Uani 1 1 d . . . C13 C 1.2420(4) 0.86362(13) 0.18919(9) 0.0207(5) Uani 1 1 d . . . H13 H 1.2030 0.8953 0.1591 0.025 Uiso 1 1 calc R . . C17 C 1.1072(4) 0.79013(12) 0.37287(9) 0.0190(4) Uani 1 1 d . . . H17 H 1.0185 0.7950 0.4061 0.023 Uiso 1 1 calc R . . C15 C 1.1619(4) 0.82563(12) 0.28032(9) 0.0166(4) Uani 1 1 d . . . C14 C 1.0969(4) 0.87055(12) 0.23476(9) 0.0197(4) Uani 1 1 d . . . H14 H 0.9541 0.9051 0.2359 0.024 Uiso 1 1 calc R . . C12 C 1.4477(4) 0.81066(12) 0.18572(8) 0.0190(4) Uani 1 1 d . . . H12 H 1.5464 0.8078 0.1536 0.023 Uiso 1 1 calc R . . C7 C 1.8281(4) 0.69123(12) 0.13416(8) 0.0194(4) Uani 1 1 d . . . H7 H 1.6987 0.7254 0.1208 0.023 Uiso 1 1 calc R . . O1 O 1.2695(3) 0.89295(9) 0.47693(6) 0.0233(3) Uani 1 1 d . . . O2 O 1.5602(3) 0.62910(9) 0.56104(6) 0.0225(3) Uani 1 1 d . . . N4 N 1.3075(4) 0.72424(10) 0.46828(7) 0.0166(4) Uani 1 1 d . . . C23 C 1.2002(4) 0.66417(12) 0.50274(9) 0.0184(4) Uani 1 1 d . . . H23A H 1.0523 0.6400 0.4832 0.022 Uiso 1 1 calc R . . H23B H 1.1283 0.6888 0.5352 0.022 Uiso 1 1 calc R . . C24 C 1.3862(4) 0.60106(12) 0.52099(8) 0.0185(4) Uani 1 1 d . . . H24A H 1.2849 0.5577 0.5356 0.022 Uiso 1 1 calc R . . H24B H 1.4867 0.5823 0.4898 0.022 Uiso 1 1 calc R . . C21 C 1.5091(5) 0.85315(12) 0.46918(9) 0.0213(5) Uani 1 1 d . . . H21A H 1.6552 0.8826 0.4853 0.026 Uiso 1 1 calc R . . H21B H 1.5421 0.8472 0.4302 0.026 Uiso 1 1 calc R . . C20 C 1.4926(4) 0.77535(12) 0.49547(8) 0.0193(4) Uani 1 1 d . . . H20A H 1.6678 0.7515 0.4955 0.023 Uiso 1 1 calc R . . H20B H 1.4394 0.7818 0.5334 0.023 Uiso 1 1 calc R . . C5 C 2.1913(4) 0.60585(13) 0.11489(9) 0.0213(5) Uani 1 1 d . . . H5 H 2.3078 0.5840 0.0897 0.026 Uiso 1 1 calc R . . C22 C 1.2532(6) 0.96062(13) 0.44584(10) 0.0316(6) Uani 1 1 d . . . H22A H 1.4009 0.9940 0.4548 0.047 Uiso 1 1 calc R . . H22B H 1.0894 0.9871 0.4537 0.047 Uiso 1 1 calc R . . H22C H 1.2581 0.9476 0.4075 0.047 Uiso 1 1 calc R . . C25 C 1.7178(5) 0.56882(14) 0.58196(10) 0.0265(5) Uani 1 1 d . . . H25A H 1.6058 0.5299 0.5982 0.040 Uiso 1 1 calc R . . H25B H 1.8380 0.5892 0.6093 0.040 Uiso 1 1 calc R . . H25C H 1.8180 0.5458 0.5528 0.040 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 0.01304(10) 0.00977(9) 0.01019(9) 0.00092(5) -0.00111(5) 0.00017(5) Cl1 0.0221(3) 0.0164(2) 0.0141(2) 0.00442(17) 0.00069(18) 0.00501(18) N1 0.0136(9) 0.0108(8) 0.0144(8) -0.0003(6) 0.0005(6) -0.0026(6) N3 0.0137(9) 0.0105(8) 0.0151(8) -0.0004(6) -0.0022(6) -0.0011(6) C18 0.0144(11) 0.0126(9) 0.0162(10) -0.0024(7) -0.0008(7) -0.0020(7) N2 0.0170(9) 0.0148(8) 0.0128(8) 0.0011(6) -0.0009(6) 0.0000(7) C8 0.0151(11) 0.0138(9) 0.0162(10) 0.0003(8) -0.0006(8) -0.0036(8) C1 0.0167(11) 0.0122(9) 0.0195(10) 0.0008(8) -0.0013(8) -0.0010(8) C11 0.0157(11) 0.0122(9) 0.0161(10) 0.0013(7) -0.0041(8) -0.0030(7) C19 0.0216(12) 0.0149(10) 0.0149(10) -0.0015(8) 0.0001(8) 0.0018(8) C9 0.0153(11) 0.0132(9) 0.0140(9) -0.0010(7) -0.0005(7) -0.0047(7) C10 0.0149(11) 0.0103(9) 0.0156(10) 0.0010(7) -0.0051(7) -0.0024(7) C3 0.0169(11) 0.0169(10) 0.0244(11) -0.0047(8) 0.0043(8) -0.0021(8) C6 0.0260(13) 0.0257(12) 0.0137(10) 0.0006(8) 0.0012(9) -0.0054(9) C2 0.0177(12) 0.0132(10) 0.0267(11) -0.0003(8) -0.0005(8) -0.0004(8) C16 0.0155(12) 0.0153(10) 0.0272(12) -0.0030(8) -0.0018(9) 0.0022(8) C4 0.0168(11) 0.0160(10) 0.0199(10) -0.0039(8) 0.0024(8) -0.0051(8) C13 0.0244(13) 0.0162(10) 0.0214(11) 0.0066(9) -0.0090(9) -0.0017(8) C17 0.0186(12) 0.0189(10) 0.0195(10) -0.0034(8) 0.0007(8) 0.0004(8) C15 0.0170(11) 0.0112(9) 0.0213(11) -0.0004(8) -0.0052(8) -0.0029(8) C14 0.0179(11) 0.0141(10) 0.0271(11) 0.0020(8) -0.0067(8) 0.0021(8) C12 0.0223(12) 0.0177(10) 0.0169(10) 0.0035(8) -0.0024(8) -0.0022(8) C7 0.0202(12) 0.0221(11) 0.0159(10) 0.0021(8) -0.0017(8) -0.0012(8) O1 0.0336(9) 0.0159(7) 0.0204(8) 0.0033(6) 0.0052(6) 0.0038(6) O2 0.0278(9) 0.0196(8) 0.0200(8) -0.0008(6) -0.0061(6) 0.0034(6) N4 0.0220(10) 0.0155(8) 0.0123(8) -0.0012(7) 0.0019(7) 0.0012(7) C23 0.0193(12) 0.0191(10) 0.0168(10) 0.0010(8) 0.0014(8) 0.0013(8) C24 0.0235(12) 0.0162(10) 0.0158(10) 0.0013(8) 0.0006(8) -0.0002(8) C21 0.0256(13) 0.0194(11) 0.0190(11) -0.0031(8) 0.0022(9) -0.0030(9) C20 0.0222(12) 0.0183(10) 0.0173(10) -0.0018(8) -0.0006(8) 0.0019(8) C5 0.0229(12) 0.0233(11) 0.0177(10) -0.0047(9) 0.0049(8) -0.0037(9) C22 0.0506(17) 0.0175(11) 0.0266(12) 0.0042(9) 0.0004(11) 0.0001(11) C25 0.0273(13) 0.0252(12) 0.0269(12) 0.0041(9) -0.0062(9) 0.0031(9) _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 1.9704(17) . ? Pd1 N1 2.0194(17) . ? Pd1 N3 2.0858(17) . ? Pd1 Cl1 2.3510(5) . ? N1 C1 1.327(3) . ? N1 C9 1.383(3) . ? N3 C18 1.339(3) . ? N3 C10 1.396(3) . ? C18 C17 1.417(3) . ? C18 C19 1.512(3) . ? N2 C11 1.377(3) . ? N2 C8 1.380(3) . ? C8 C7 1.394(3) . ? C8 C9 1.435(3) . ? C1 C2 1.406(3) . ? C1 H1 0.9500 . ? C11 C12 1.397(3) . ? C11 C10 1.430(3) . ? C19 N4 1.464(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C9 C4 1.416(3) . ? C10 C15 1.414(3) . ? C3 C2 1.367(3) . ? C3 C4 1.413(3) . ? C3 H3 0.9500 . ? C6 C5 1.376(3) . ? C6 C7 1.405(3) . ? C6 H6 0.9500 . ? C2 H2 0.9500 . ? C16 C17 1.359(3) . ? C16 C15 1.414(3) . ? C16 H16 0.9500 . ? C4 C5 1.417(3) . ? C13 C14 1.366(3) . ? C13 C12 1.407(3) . ? C13 H13 0.9500 . ? C17 H17 0.9500 . ? C15 C14 1.415(3) . ? C14 H14 0.9500 . ? C12 H12 0.9500 . ? C7 H7 0.9500 . ? O1 C22 1.416(3) . ? O1 C21 1.426(3) . ? O2 C24 1.417(3) . ? O2 C25 1.423(3) . ? N4 C20 1.464(3) . ? N4 C23 1.467(3) . ? C23 C24 1.525(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C21 C20 1.513(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C5 H5 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 N1 81.84(7) . . ? N2 Pd1 N3 81.90(7) . . ? N1 Pd1 N3 163.62(7) . . ? N2 Pd1 Cl1 170.13(5) . . ? N1 Pd1 Cl1 90.42(5) . . ? N3 Pd1 Cl1 105.96(5) . . ? C1 N1 C9 119.35(17) . . ? C1 N1 Pd1 128.81(14) . . ? C9 N1 Pd1 111.84(13) . . ? C18 N3 C10 118.59(17) . . ? C18 N3 Pd1 131.76(14) . . ? C10 N3 Pd1 109.65(13) . . ? N3 C18 C17 121.60(19) . . ? N3 C18 C19 119.03(18) . . ? C17 C18 C19 119.36(18) . . ? C11 N2 C8 128.94(17) . . ? C11 N2 Pd1 115.77(13) . . ? C8 N2 Pd1 114.97(14) . . ? N2 C8 C7 129.5(2) . . ? N2 C8 C9 113.78(18) . . ? C7 C8 C9 116.74(19) . . ? N1 C1 C2 122.23(19) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? N2 C11 C12 127.51(19) . . ? N2 C11 C10 114.79(17) . . ? C12 C11 C10 117.64(19) . . ? N4 C19 C18 113.72(17) . . ? N4 C19 H19A 108.8 . . ? C18 C19 H19A 108.8 . . ? N4 C19 H19B 108.8 . . ? C18 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N1 C9 C4 121.11(18) . . ? N1 C9 C8 116.68(18) . . ? C4 C9 C8 122.20(19) . . ? N3 C10 C15 121.79(19) . . ? N3 C10 C11 117.83(18) . . ? C15 C10 C11 120.37(18) . . ? C2 C3 C4 120.0(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C6 C7 122.5(2) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C3 C4 C9 117.67(19) . . ? C3 C4 C5 123.8(2) . . ? C9 C4 C5 118.6(2) . . ? C14 C13 C12 121.6(2) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C16 C17 C18 120.3(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C16 C15 C10 117.57(19) . . ? C16 C15 C14 122.5(2) . . ? C10 C15 C14 119.9(2) . . ? C13 C14 C15 119.2(2) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C11 C12 C13 121.1(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C7 C6 120.8(2) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C22 O1 C21 112.40(18) . . ? C24 O2 C25 110.49(16) . . ? C20 N4 C19 112.58(17) . . ? C20 N4 C23 114.40(17) . . ? C19 N4 C23 112.52(16) . . ? N4 C23 C24 117.16(18) . . ? N4 C23 H23A 108.0 . . ? C24 C23 H23A 108.0 . . ? N4 C23 H23B 108.0 . . ? C24 C23 H23B 108.0 . . ? H23A C23 H23B 107.3 . . ? O2 C24 C23 110.17(17) . . ? O2 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O2 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? O1 C21 C20 109.25(18) . . ? O1 C21 H21A 109.8 . . ? C20 C21 H21A 109.8 . . ? O1 C21 H21B 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? N4 C20 C21 112.90(18) . . ? N4 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N4 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C6 C5 C4 119.0(2) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? O1 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 N1 C1 173.48(18) . . . . ? N3 Pd1 N1 C1 166.4(2) . . . . ? Cl1 Pd1 N1 C1 -12.66(17) . . . . ? N2 Pd1 N1 C9 -6.53(13) . . . . ? N3 Pd1 N1 C9 -13.7(3) . . . . ? Cl1 Pd1 N1 C9 167.33(13) . . . . ? N2 Pd1 N3 C18 -179.51(19) . . . . ? N1 Pd1 N3 C18 -172.4(2) . . . . ? Cl1 Pd1 N3 C18 6.60(19) . . . . ? N2 Pd1 N3 C10 0.67(13) . . . . ? N1 Pd1 N3 C10 7.8(3) . . . . ? Cl1 Pd1 N3 C10 -173.23(11) . . . . ? C10 N3 C18 C17 2.9(3) . . . . ? Pd1 N3 C18 C17 -176.92(15) . . . . ? C10 N3 C18 C19 -177.74(17) . . . . ? Pd1 N3 C18 C19 2.4(3) . . . . ? N1 Pd1 N2 C11 -177.12(15) . . . . ? N3 Pd1 N2 C11 0.86(14) . . . . ? Cl1 Pd1 N2 C11 144.2(3) . . . . ? N1 Pd1 N2 C8 8.77(14) . . . . ? N3 Pd1 N2 C8 -173.25(15) . . . . ? Cl1 Pd1 N2 C8 -29.9(4) . . . . ? C11 N2 C8 C7 -4.1(4) . . . . ? Pd1 N2 C8 C7 169.08(18) . . . . ? C11 N2 C8 C9 177.60(19) . . . . ? Pd1 N2 C8 C9 -9.2(2) . . . . ? C9 N1 C1 C2 -2.0(3) . . . . ? Pd1 N1 C1 C2 177.99(15) . . . . ? C8 N2 C11 C12 -12.0(3) . . . . ? Pd1 N2 C11 C12 174.84(17) . . . . ? C8 N2 C11 C10 170.90(19) . . . . ? Pd1 N2 C11 C10 -2.2(2) . . . . ? N3 C18 C19 N4 164.65(18) . . . . ? C17 C18 C19 N4 -16.0(3) . . . . ? C1 N1 C9 C4 3.9(3) . . . . ? Pd1 N1 C9 C4 -176.07(15) . . . . ? C1 N1 C9 C8 -176.52(18) . . . . ? Pd1 N1 C9 C8 3.5(2) . . . . ? N2 C8 C9 N1 3.6(3) . . . . ? C7 C8 C9 N1 -174.94(18) . . . . ? N2 C8 C9 C4 -176.84(18) . . . . ? C7 C8 C9 C4 4.6(3) . . . . ? C18 N3 C10 C15 -1.0(3) . . . . ? Pd1 N3 C10 C15 178.85(15) . . . . ? C18 N3 C10 C11 178.05(18) . . . . ? Pd1 N3 C10 C11 -2.1(2) . . . . ? N2 C11 C10 N3 2.9(3) . . . . ? C12 C11 C10 N3 -174.47(18) . . . . ? N2 C11 C10 C15 -178.02(18) . . . . ? C12 C11 C10 C15 4.6(3) . . . . ? C4 C3 C2 C1 2.0(3) . . . . ? N1 C1 C2 C3 -1.0(3) . . . . ? C2 C3 C4 C9 -0.2(3) . . . . ? C2 C3 C4 C5 -179.6(2) . . . . ? N1 C9 C4 C3 -2.8(3) . . . . ? C8 C9 C4 C3 177.64(19) . . . . ? N1 C9 C4 C5 176.67(18) . . . . ? C8 C9 C4 C5 -2.9(3) . . . . ? C15 C16 C17 C18 -0.5(3) . . . . ? N3 C18 C17 C16 -2.2(3) . . . . ? C19 C18 C17 C16 178.45(19) . . . . ? C17 C16 C15 C10 2.3(3) . . . . ? C17 C16 C15 C14 -177.0(2) . . . . ? N3 C10 C15 C16 -1.6(3) . . . . ? C11 C10 C15 C16 179.41(19) . . . . ? N3 C10 C15 C14 177.78(18) . . . . ? C11 C10 C15 C14 -1.3(3) . . . . ? C12 C13 C14 C15 2.6(3) . . . . ? C16 C15 C14 C13 176.9(2) . . . . ? C10 C15 C14 C13 -2.4(3) . . . . ? N2 C11 C12 C13 178.6(2) . . . . ? C10 C11 C12 C13 -4.4(3) . . . . ? C14 C13 C12 C11 0.9(3) . . . . ? N2 C8 C7 C6 178.7(2) . . . . ? C9 C8 C7 C6 -3.1(3) . . . . ? C5 C6 C7 C8 -0.2(3) . . . . ? C18 C19 N4 C20 -95.9(2) . . . . ? C18 C19 N4 C23 133.06(19) . . . . ? C20 N4 C23 C24 -69.5(2) . . . . ? C19 N4 C23 C24 60.6(2) . . . . ? C25 O2 C24 C23 174.43(18) . . . . ? N4 C23 C24 O2 73.9(2) . . . . ? C22 O1 C21 C20 -169.94(18) . . . . ? C19 N4 C20 C21 75.0(2) . . . . ? C23 N4 C20 C21 -154.88(18) . . . . ? O1 C21 C20 N4 68.3(2) . . . . ? C7 C6 C5 C4 2.0(3) . . . . ? C3 C4 C5 C6 178.9(2) . . . . ? C9 C4 C5 C6 -0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 68.91 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.485 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.062 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 766172' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H16.50 Cl3.50 N4 O Pd0.50' _chemical_formula_weight 452.10 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3314(7) _cell_length_b 13.8105(13) _cell_length_c 18.3307(18) _cell_angle_alpha 84.743(2) _cell_angle_beta 88.483(2) _cell_angle_gamma 82.262(2) _cell_volume 1831.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9720 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 30.58 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7557 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 47572 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 29.13 _reflns_number_total 9810 _reflns_number_gt 8589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0356P)^2^+2.6333P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9810 _refine_ls_number_parameters 513 _refine_ls_number_restraints 394 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.042 _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 Pd1 Pd 0.71066(2) 0.209201(12) 0.206489(9) 0.01571(5) Uani 1 1 d U . . N2 N 0.6340(3) 0.34429(14) 0.16479(10) 0.0187(4) Uani 1 1 d U . . N61 N 0.8113(3) 0.33824(14) 0.41625(10) 0.0203(4) Uani 1 1 d U . . N4 N 0.8790(3) 0.12652(13) 0.36336(10) 0.0184(4) Uani 1 1 d U . . N52 N 0.7860(3) 0.05972(14) 0.22851(11) 0.0196(4) Uani 1 1 d U . . N1 N 0.4713(3) 0.18621(14) 0.16439(10) 0.0186(4) Uani 1 1 d U . . N3 N 0.9257(2) 0.27204(13) 0.24264(10) 0.0164(3) Uani 1 1 d U . . C17 C 1.2092(3) 0.28642(17) 0.29986(12) 0.0189(4) Uani 1 1 d U . . H17 H 1.3091 0.2563 0.3295 0.023 Uiso 1 1 calc R . . C212 C 0.9248(3) 0.25662(16) 0.44194(12) 0.0194(4) Uani 1 1 d U . . N51 N 0.8230(3) -0.09471(14) 0.27369(12) 0.0245(4) Uani 1 1 d U . . C202 C 0.8077(3) -0.00056(16) 0.28962(13) 0.0207(4) Uani 1 1 d U . . N62 N 1.0788(3) 0.27945(15) 0.46777(11) 0.0220(4) Uani 1 1 d U . . C16 C 1.2076(3) 0.38076(17) 0.26949(12) 0.0204(4) Uani 1 1 d U . . H16 H 1.3080 0.4155 0.2767 0.025 Uiso 1 1 calc R . . C18 C 1.0632(3) 0.23387(16) 0.28723(12) 0.0167(4) Uani 1 1 d U . . C211 C 0.8810(3) 0.15436(17) 0.43916(13) 0.0220(4) Uani 1 1 d U . . H21A H 0.9737 0.1081 0.4674 0.026 Uiso 1 1 calc R . . H21B H 0.7591 0.1489 0.4625 0.026 Uiso 1 1 calc R . . C3 C 0.1349(3) 0.18134(18) 0.09935(13) 0.0238(5) Uani 1 1 d U . . H3 H 0.0211 0.1784 0.0766 0.029 Uiso 1 1 calc R . . C4 C 0.2183(3) 0.26807(17) 0.08974(12) 0.0212(4) Uani 1 1 d U . . C14 C 1.0388(4) 0.52623(17) 0.19890(13) 0.0246(5) Uani 1 1 d U . . H14 H 1.1325 0.5654 0.2066 0.029 Uiso 1 1 calc R . . C9 C 0.3878(3) 0.26917(16) 0.12483(12) 0.0182(4) Uani 1 1 d U . . C214 C 0.8993(3) 0.41752(17) 0.42607(13) 0.0232(5) Uani 1 1 d U . . H214 H 0.8552 0.4847 0.4133 0.028 Uiso 1 1 calc R . . C213 C 0.6292(3) 0.34128(19) 0.38529(14) 0.0250(5) Uani 1 1 d U . . H21C H 0.5512 0.4011 0.3977 0.038 Uiso 1 1 calc R . . H21D H 0.5737 0.2837 0.4055 0.038 Uiso 1 1 calc R . . H21E H 0.6405 0.3411 0.3319 0.038 Uiso 1 1 calc R . . C1 C 0.3882(3) 0.10624(17) 0.17344(13) 0.0206(4) Uani 1 1 d U . . H1 H 0.4457 0.0505 0.2024 0.025 Uiso 1 1 calc R . . C15 C 1.0561(3) 0.42639(16) 0.22732(12) 0.0195(4) Uani 1 1 d U . . C11 C 0.7572(3) 0.40999(16) 0.17227(12) 0.0181(4) Uani 1 1 d U . . C10 C 0.9169(3) 0.36900(16) 0.21405(12) 0.0174(4) Uani 1 1 d U . . C2 C 0.2182(3) 0.10137(18) 0.14161(13) 0.0228(5) Uani 1 1 d U . . H2 H 0.1614 0.0433 0.1492 0.027 Uiso 1 1 calc R . . C7 C 0.3961(3) 0.43724(18) 0.07879(13) 0.0238(5) Uani 1 1 d U . . H7 H 0.4528 0.4955 0.0740 0.029 Uiso 1 1 calc R . . C6 C 0.2305(3) 0.43477(19) 0.04187(13) 0.0268(5) Uani 1 1 d U . . H6 H 0.1798 0.4915 0.0121 0.032 Uiso 1 1 calc R . . C215 C 1.0626(3) 0.38052(18) 0.45783(13) 0.0243(5) Uani 1 1 d U . . H215 H 1.1527 0.4188 0.4712 0.029 Uiso 1 1 calc R . . C5 C 0.1405(3) 0.35397(19) 0.04729(13) 0.0245(5) Uani 1 1 d U . . H5 H 0.0273 0.3553 0.0229 0.029 Uiso 1 1 calc R . . C204 C 0.8122(3) -0.09490(18) 0.19906(15) 0.0271(5) Uani 1 1 d U . . H204 H 0.8192 -0.1509 0.1721 0.032 Uiso 1 1 calc R . . C205 C 0.7898(3) -0.00021(17) 0.17136(14) 0.0236(5) Uani 1 1 d U . . H205 H 0.7784 0.0220 0.1209 0.028 Uiso 1 1 calc R . . C12 C 0.7449(3) 0.50906(17) 0.14722(13) 0.0232(5) Uani 1 1 d U . . H12 H 0.6394 0.5393 0.1208 0.028 Uiso 1 1 calc R . . C201 C 0.8259(3) 0.02812(17) 0.36556(13) 0.0231(5) Uani 1 1 d U . . H20A H 0.7072 0.0264 0.3923 0.028 Uiso 1 1 calc R . . H20B H 0.9200 -0.0194 0.3921 0.028 Uiso 1 1 calc R . . C13 C 0.8852(4) 0.56514(17) 0.16023(14) 0.0266(5) Uani 1 1 d U . . H13 H 0.8728 0.6321 0.1416 0.032 Uiso 1 1 calc R . . C8 C 0.4778(3) 0.35537(17) 0.12219(12) 0.0190(4) Uani 1 1 d U . . C203 C 0.8522(4) -0.18119(18) 0.32640(17) 0.0361(6) Uani 1 1 d U . . H20C H 0.9773 -0.1881 0.3455 0.054 Uiso 1 1 calc R . . H20D H 0.8360 -0.2397 0.3021 0.054 Uiso 1 1 calc R . . H20E H 0.7629 -0.1737 0.3669 0.054 Uiso 1 1 calc R . . Cl30 Cl 0.53962(10) 0.60067(5) 0.28603(4) 0.03549(15) Uani 1 1 d . . . Cl32 Cl 0.20989(10) 0.60164(5) 0.37646(4) 0.04016(16) Uani 1 1 d . . . Cl31 Cl 0.53231(12) 0.67014(6) 0.43018(4) 0.04612(19) Uani 1 1 d . . . Cl7A Cl 0.8062(10) 0.0937(3) -0.0323(3) 0.0525(15) Uani 0.473(10) 1 d PD A 1 Cl8A Cl 0.4483(4) 0.2040(5) -0.0595(2) 0.0775(17) Uani 0.473(10) 1 d PD A 1 Cl9A Cl 0.7729(6) 0.2884(3) -0.09992(17) 0.0558(11) Uani 0.473(10) 1 d PD A 1 Cl8B Cl 0.4844(9) 0.1241(13) -0.0400(4) 0.136(6) Uani 0.406(10) 1 d PD A 2 Cl7B Cl 0.8662(9) 0.1076(6) -0.0433(4) 0.058(2) Uani 0.406(10) 1 d PD A 2 Cl9B Cl 0.674(2) 0.2948(3) -0.0804(6) 0.129(4) Uani 0.406(10) 1 d PD A 2 Cl8C Cl 0.563(3) 0.0810(9) -0.0289(6) 0.130(10) Uani 0.131(5) 1 d PD A 3 Cl7C Cl 0.8719(18) 0.168(3) -0.0561(10) 0.215(19) Uani 0.131(5) 1 d PD A 3 Cl9C Cl 0.512(3) 0.2710(9) -0.0840(7) 0.098(7) Uani 0.131(5) 1 d PD A 3 C19 C 1.0579(3) 0.13295(16) 0.32549(12) 0.0181(4) Uani 1 1 d U . . H19A H 1.0779 0.0836 0.2892 0.022 Uiso 1 1 calc R . . H19B H 1.1582 0.1182 0.3615 0.022 Uiso 1 1 calc R . . C301 C 0.4018(3) 0.66257(18) 0.35215(13) 0.0250(5) Uani 1 1 d . . . H301 H 0.3570 0.7306 0.3307 0.030 Uiso 1 1 calc R . . C401 C 0.6706(4) 0.1737(2) -0.08907(16) 0.0384(7) Uani 1 1 d D . . H401 H 0.6692 0.1468 -0.1379 0.046 Uiso 1 1 calc R A 1 Cl1 Cl 0.30324(8) 0.88813(4) 0.26615(3) 0.01855(10) Uani 1 1 d . . . O1 O 0.4025(3) 0.14094(14) 0.46987(13) 0.0362(5) Uani 1 1 d D . . H101 H 0.308(3) 0.181(2) 0.4743(19) 0.043 Uiso 1 1 d D . . H102 H 0.366(5) 0.0930(19) 0.4560(19) 0.043 Uiso 1 1 d D . . O2 O 0.3782(4) -0.04051(18) 0.42057(13) 0.0452(5) Uani 1 1 d D . . H201 H 0.365(5) -0.064(3) 0.3806(14) 0.054 Uiso 1 1 d D . . H202 H 0.447(5) -0.083(2) 0.442(2) 0.054 Uiso 1 1 d 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 0.01582(8) 0.01577(8) 0.01522(8) -0.00093(6) -0.00293(6) -0.00075(6) N2 0.0182(9) 0.0182(8) 0.0185(9) 0.0027(7) -0.0036(7) -0.0004(7) N61 0.0211(9) 0.0225(9) 0.0169(9) -0.0021(7) -0.0015(7) -0.0011(7) N4 0.0204(9) 0.0170(8) 0.0178(9) -0.0006(7) -0.0014(7) -0.0036(7) N52 0.0184(9) 0.0185(9) 0.0219(9) -0.0026(7) -0.0052(7) -0.0013(7) N1 0.0161(8) 0.0226(9) 0.0171(9) -0.0037(7) -0.0017(7) -0.0011(7) N3 0.0167(8) 0.0167(8) 0.0156(8) -0.0019(7) -0.0008(7) -0.0013(7) C17 0.0174(10) 0.0232(10) 0.0164(10) -0.0030(8) -0.0018(8) -0.0026(8) C212 0.0226(10) 0.0209(10) 0.0138(10) -0.0011(8) -0.0003(8) -0.0004(8) N51 0.0229(10) 0.0169(9) 0.0337(11) -0.0016(8) -0.0052(8) -0.0024(7) C202 0.0180(10) 0.0166(10) 0.0277(12) -0.0016(8) -0.0034(9) -0.0025(8) N62 0.0235(9) 0.0237(9) 0.0189(9) -0.0047(7) -0.0012(7) -0.0013(8) C16 0.0209(10) 0.0235(10) 0.0182(10) -0.0038(8) 0.0000(8) -0.0064(8) C18 0.0172(9) 0.0186(9) 0.0146(9) -0.0031(8) -0.0002(8) -0.0017(8) C211 0.0253(11) 0.0223(10) 0.0180(10) 0.0006(8) -0.0012(9) -0.0031(9) C3 0.0186(10) 0.0313(12) 0.0224(11) -0.0090(9) -0.0028(9) -0.0013(9) C4 0.0198(10) 0.0270(11) 0.0162(10) -0.0049(9) -0.0021(8) 0.0018(9) C14 0.0300(12) 0.0211(11) 0.0237(12) -0.0011(9) 0.0009(9) -0.0084(9) C9 0.0180(10) 0.0218(10) 0.0143(9) -0.0027(8) -0.0008(8) 0.0002(8) C214 0.0282(12) 0.0202(10) 0.0212(11) -0.0048(9) 0.0003(9) -0.0010(9) C213 0.0206(11) 0.0299(12) 0.0241(12) -0.0028(10) -0.0031(9) -0.0009(9) C1 0.0192(10) 0.0209(10) 0.0217(11) -0.0042(8) -0.0010(8) -0.0009(8) C15 0.0226(11) 0.0201(10) 0.0159(10) -0.0023(8) 0.0013(8) -0.0030(8) C11 0.0193(10) 0.0193(10) 0.0150(10) -0.0007(8) 0.0011(8) -0.0004(8) C10 0.0201(10) 0.0174(9) 0.0142(9) -0.0019(8) 0.0007(8) -0.0004(8) C2 0.0193(10) 0.0257(11) 0.0250(11) -0.0083(9) -0.0001(9) -0.0040(9) C7 0.0222(11) 0.0261(11) 0.0213(11) 0.0033(9) -0.0011(9) -0.0006(9) C6 0.0247(11) 0.0326(13) 0.0198(11) 0.0051(10) -0.0043(9) 0.0032(10) C215 0.0271(12) 0.0242(11) 0.0225(11) -0.0065(9) -0.0013(9) -0.0040(9) C5 0.0194(10) 0.0342(13) 0.0182(11) -0.0021(9) -0.0049(8) 0.0035(9) C204 0.0245(12) 0.0214(11) 0.0364(14) -0.0092(10) -0.0041(10) -0.0020(9) C205 0.0226(11) 0.0243(11) 0.0252(12) -0.0088(9) -0.0035(9) -0.0022(9) C12 0.0273(12) 0.0192(10) 0.0218(11) 0.0006(9) -0.0028(9) 0.0007(9) C201 0.0275(12) 0.0187(10) 0.0236(11) 0.0014(9) -0.0040(9) -0.0059(9) C13 0.0364(13) 0.0168(10) 0.0260(12) -0.0001(9) -0.0006(10) -0.0027(9) C8 0.0180(10) 0.0232(10) 0.0143(9) 0.0002(8) 0.0000(8) 0.0015(8) C203 0.0429(16) 0.0169(11) 0.0477(17) 0.0045(11) -0.0041(13) -0.0052(11) Cl30 0.0423(4) 0.0333(3) 0.0303(3) -0.0077(3) 0.0091(3) -0.0015(3) Cl32 0.0340(3) 0.0378(4) 0.0490(4) 0.0006(3) 0.0070(3) -0.0106(3) Cl31 0.0579(5) 0.0575(5) 0.0272(3) -0.0070(3) -0.0080(3) -0.0191(4) Cl7A 0.102(4) 0.0252(9) 0.0278(12) 0.0010(8) -0.019(2) 0.0017(17) Cl8A 0.0304(10) 0.158(5) 0.0521(17) -0.052(2) 0.0101(9) -0.0137(17) Cl9A 0.092(2) 0.0325(14) 0.0488(13) 0.0036(9) -0.0120(13) -0.0331(15) Cl8B 0.056(3) 0.310(16) 0.074(4) -0.112(7) 0.036(3) -0.091(6) Cl7B 0.055(3) 0.075(4) 0.044(3) -0.036(3) -0.023(2) 0.021(3) Cl9B 0.214(11) 0.0355(18) 0.129(6) -0.017(3) -0.081(7) 0.035(4) Cl8C 0.31(3) 0.053(6) 0.028(4) 0.007(4) 0.022(9) -0.039(10) Cl7C 0.072(10) 0.51(5) 0.116(15) -0.18(3) 0.044(9) -0.14(2) Cl9C 0.146(15) 0.056(6) 0.072(7) -0.005(5) 0.017(8) 0.060(8) C19 0.0171(10) 0.0186(10) 0.0182(10) -0.0012(8) -0.0032(8) -0.0010(8) C301 0.0300(12) 0.0222(11) 0.0226(11) -0.0022(9) 0.0013(9) -0.0029(9) C401 0.0406(16) 0.0451(16) 0.0302(14) -0.0159(12) -0.0023(12) 0.0013(13) Cl1 0.0268(3) 0.0150(2) 0.0133(2) 0.00085(17) -0.00299(19) -0.00164(19) O1 0.0284(10) 0.0246(9) 0.0540(13) -0.0038(9) -0.0003(9) 0.0024(8) O2 0.0606(15) 0.0457(13) 0.0322(12) -0.0111(10) -0.0103(10) -0.0101(11) _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 1.9647(18) . ? Pd1 N1 2.0104(19) . ? Pd1 N3 2.0511(18) . ? Pd1 N52 2.0693(19) . ? N2 C11 1.381(3) . ? N2 C8 1.387(3) . ? N61 C212 1.362(3) . ? N61 C214 1.371(3) . ? N61 C213 1.458(3) . ? N4 C201 1.460(3) . ? N4 C211 1.476(3) . ? N4 C19 1.477(3) . ? N52 C202 1.333(3) . ? N52 C205 1.391(3) . ? N1 C1 1.327(3) . ? N1 C9 1.377(3) . ? N3 C18 1.335(3) . ? N3 C10 1.386(3) . ? C17 C16 1.368(3) . ? C17 C18 1.407(3) . ? C17 H17 0.9500 . ? C212 N62 1.323(3) . ? C212 C211 1.495(3) . ? N51 C202 1.348(3) . ? N51 C204 1.373(3) . ? N51 C203 1.462(3) . ? C202 C201 1.496(3) . ? N62 C215 1.380(3) . ? C16 C15 1.413(3) . ? C16 H16 0.9500 . ? C18 C19 1.507(3) . ? C211 H21A 0.9900 . ? C211 H21B 0.9900 . ? C3 C2 1.371(3) . ? C3 C4 1.412(3) . ? C3 H3 0.9500 . ? C4 C9 1.417(3) . ? C4 C5 1.418(3) . ? C14 C13 1.367(4) . ? C14 C15 1.419(3) . ? C14 H14 0.9500 . ? C9 C8 1.433(3) . ? C214 C215 1.361(3) . ? C214 H214 0.9500 . ? C213 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C1 C2 1.402(3) . ? C1 H1 0.9500 . ? C15 C10 1.413(3) . ? C11 C12 1.395(3) . ? C11 C10 1.437(3) . ? C2 H2 0.9500 . ? C7 C8 1.396(3) . ? C7 C6 1.411(3) . ? C7 H7 0.9500 . ? C6 C5 1.366(4) . ? C6 H6 0.9500 . ? C215 H215 0.9500 . ? C5 H5 0.9500 . ? C204 C205 1.349(3) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C12 C13 1.406(4) . ? C12 H12 0.9500 . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C13 H13 0.9500 . ? C203 H20C 0.9800 . ? C203 H20D 0.9800 . ? C203 H20E 0.9800 . ? Cl30 C301 1.765(2) . ? Cl32 C301 1.761(3) . ? Cl31 C301 1.760(3) . ? Cl7A C401 1.686(5) . ? Cl8A C401 1.714(4) . ? Cl9A C401 1.835(4) . ? Cl8B C401 1.792(7) . ? Cl7B C401 1.778(6) . ? Cl9B C401 1.699(6) . ? Cl8C C401 1.854(11) . ? Cl7C C401 1.600(12) . ? Cl9C C401 1.663(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C301 H301 1.0000 . ? C401 H401 1.0000 . ? O1 H101 0.834(18) . ? O1 H102 0.811(18) . ? O2 H201 0.838(18) . ? O2 H202 0.804(18) . ? 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 N1 82.67(8) . . ? N2 Pd1 N3 81.90(8) . . ? N1 Pd1 N3 164.28(7) . . ? N2 Pd1 N52 168.18(8) . . ? N1 Pd1 N52 90.79(8) . . ? N3 Pd1 N52 104.93(7) . . ? C11 N2 C8 129.17(19) . . ? C11 N2 Pd1 115.73(14) . . ? C8 N2 Pd1 114.21(15) . . ? C212 N61 C214 107.04(19) . . ? C212 N61 C213 126.7(2) . . ? C214 N61 C213 126.3(2) . . ? C201 N4 C211 108.41(18) . . ? C201 N4 C19 112.02(17) . . ? C211 N4 C19 111.78(18) . . ? C202 N52 C205 105.96(19) . . ? C202 N52 Pd1 134.35(16) . . ? C205 N52 Pd1 118.75(16) . . ? C1 N1 C9 120.06(19) . . ? C1 N1 Pd1 128.40(16) . . ? C9 N1 Pd1 111.45(15) . . ? C18 N3 C10 119.20(19) . . ? C18 N3 Pd1 130.08(15) . . ? C10 N3 Pd1 110.71(14) . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? N62 C212 N61 111.5(2) . . ? N62 C212 C211 124.8(2) . . ? N61 C212 C211 123.7(2) . . ? C202 N51 C204 107.9(2) . . ? C202 N51 C203 126.0(2) . . ? C204 N51 C203 126.1(2) . . ? N52 C202 N51 110.3(2) . . ? N52 C202 C201 126.6(2) . . ? N51 C202 C201 123.0(2) . . ? C212 N62 C215 105.1(2) . . ? C17 C16 C15 119.8(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? N3 C18 C17 121.5(2) . . ? N3 C18 C19 118.57(19) . . ? C17 C18 C19 119.96(19) . . ? N4 C211 C212 112.12(19) . . ? N4 C211 H21A 109.2 . . ? C212 C211 H21A 109.2 . . ? N4 C211 H21B 109.2 . . ? C212 C211 H21B 109.2 . . ? H21A C211 H21B 107.9 . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C9 118.1(2) . . ? C3 C4 C5 123.4(2) . . ? C9 C4 C5 118.6(2) . . ? C13 C14 C15 118.9(2) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N1 C9 C4 120.4(2) . . ? N1 C9 C8 117.21(19) . . ? C4 C9 C8 122.4(2) . . ? C215 C214 N61 106.0(2) . . ? C215 C214 H214 127.0 . . ? N61 C214 H214 127.0 . . ? N61 C213 H21C 109.5 . . ? N61 C213 H21D 109.5 . . ? H21C C213 H21D 109.5 . . ? N61 C213 H21E 109.5 . . ? H21C C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? N1 C1 C2 122.1(2) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C16 C15 C10 117.6(2) . . ? C16 C15 C14 122.8(2) . . ? C10 C15 C14 119.6(2) . . ? N2 C11 C12 129.3(2) . . ? N2 C11 C10 113.82(19) . . ? C12 C11 C10 116.9(2) . . ? N3 C10 C15 121.4(2) . . ? N3 C10 C11 117.4(2) . . ? C15 C10 C11 121.2(2) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C8 C7 C6 121.0(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C5 C6 C7 122.5(2) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C214 C215 N62 110.3(2) . . ? C214 C215 H215 124.8 . . ? N62 C215 H215 124.8 . . ? C6 C5 C4 119.1(2) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C205 C204 N51 106.7(2) . . ? C205 C204 H204 126.6 . . ? N51 C204 H204 126.6 . . ? C204 C205 N52 109.1(2) . . ? C204 C205 H205 125.4 . . ? N52 C205 H205 125.4 . . ? C11 C12 C13 121.4(2) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? N4 C201 C202 110.52(19) . . ? N4 C201 H20A 109.5 . . ? C202 C201 H20A 109.5 . . ? N4 C201 H20B 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 108.1 . . ? C14 C13 C12 122.0(2) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? N2 C8 C7 129.7(2) . . ? N2 C8 C9 113.85(19) . . ? C7 C8 C9 116.4(2) . . ? N51 C203 H20C 109.5 . . ? N51 C203 H20D 109.5 . . ? H20C C203 H20D 109.5 . . ? N51 C203 H20E 109.5 . . ? H20C C203 H20E 109.5 . . ? H20D C203 H20E 109.5 . . ? N4 C19 C18 110.75(17) . . ? N4 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? Cl31 C301 Cl32 110.25(14) . . ? Cl31 C301 Cl30 110.10(14) . . ? Cl32 C301 Cl30 110.32(13) . . ? Cl31 C301 H301 108.7 . . ? Cl32 C301 H301 108.7 . . ? Cl30 C301 H301 108.7 . . ? Cl7C C401 Cl9C 122.2(10) . . ? Cl7C C401 Cl7A 44.1(13) . . ? Cl9C C401 Cl7A 138.6(5) . . ? Cl7C C401 Cl9B 80.6(12) . . ? Cl9C C401 Cl9B 44.8(8) . . ? Cl7A C401 Cl9B 116.8(3) . . ? Cl7C C401 Cl8A 136.6(6) . . ? Cl9C C401 Cl8A 39.5(7) . . ? Cl7A C401 Cl8A 116.0(3) . . ? Cl9B C401 Cl8A 80.9(5) . . ? Cl7C C401 Cl7B 28.8(12) . . ? Cl9C C401 Cl7B 142.3(7) . . ? Cl7A C401 Cl7B 17.4(3) . . ? Cl9B C401 Cl7B 107.6(3) . . ? Cl8A C401 Cl7B 131.3(3) . . ? Cl7C C401 Cl8B 123.3(10) . . ? Cl9C C401 Cl8B 76.7(8) . . ? Cl7A C401 Cl8B 84.8(4) . . ? Cl9B C401 Cl8B 113.7(4) . . ? Cl8A C401 Cl8B 37.4(4) . . ? Cl7B C401 Cl8B 102.1(4) . . ? Cl7C C401 Cl9A 64.3(13) . . ? Cl9C C401 Cl9A 68.4(8) . . ? Cl7A C401 Cl9A 107.4(3) . . ? Cl9B C401 Cl9A 25.7(5) . . ? Cl8A C401 Cl9A 106.2(2) . . ? Cl7B C401 Cl9A 93.1(3) . . ? Cl8B C401 Cl9A 138.9(4) . . ? Cl7C C401 Cl8C 103.6(10) . . ? Cl9C C401 Cl8C 100.4(7) . . ? Cl7A C401 Cl8C 61.3(7) . . ? Cl9B C401 Cl8C 129.9(7) . . ? Cl8A C401 Cl8C 61.9(7) . . ? Cl7B C401 Cl8C 78.7(7) . . ? Cl8B C401 Cl8C 24.9(7) . . ? Cl9A C401 Cl8C 149.3(5) . . ? Cl7C C401 H401 114.1 . . ? Cl9C C401 H401 111.1 . . ? Cl7A C401 H401 109.0 . . ? Cl9B C401 H401 122.3 . . ? Cl8A C401 H401 109.0 . . ? Cl7B C401 H401 105.8 . . ? Cl8B C401 H401 103.2 . . ? Cl9A C401 H401 109.0 . . ? Cl8C C401 H401 101.7 . . ? H101 O1 H102 105(3) . . ? H201 O2 H202 103(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.382 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.087 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 766173' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 F6 N7 P Pd' _chemical_formula_weight 790.04 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 14.6795(13) _cell_length_b 13.2225(11) _cell_length_c 16.7504(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.096(2) _cell_angle_gamma 90.00 _cell_volume 3250.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 30.55 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8459 _exptl_absorpt_correction_T_max 0.8739 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus 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 8.3 _diffrn_reflns_number 74757 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9886 _reflns_number_gt 7656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0349P)^2^+3.2008P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9886 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Pd1 Pd 0.164278(10) 0.248033(10) 0.140843(9) 0.01795(5) Uani 1 1 d . . . N3 N -0.00027(11) 0.58804(11) 0.09302(9) 0.0168(3) Uani 1 1 d . . . N2 N -0.17005(11) 0.64068(12) 0.13030(11) 0.0205(3) Uani 1 1 d . . . C8 C -0.25832(13) 0.64368(14) 0.15870(11) 0.0185(4) Uani 1 1 d . . . N6 N 0.28394(12) 0.28692(12) 0.09140(10) 0.0203(3) Uani 1 1 d . . . N5 N 0.14547(11) 0.40774(12) 0.14578(9) 0.0171(3) Uani 1 1 d . . . C12 C -0.13976(14) 0.81681(14) 0.09131(12) 0.0211(4) Uani 1 1 d . . . H12 H -0.2012 0.8363 0.0991 0.025 Uiso 1 1 calc R . . C27 C 0.30106(13) 0.38769(14) 0.09849(11) 0.0195(4) Uani 1 1 d . . . C18 C 0.08103(13) 0.55813(14) 0.06894(11) 0.0183(3) Uani 1 1 d . . . C19 C 0.09929(13) 0.44531(13) 0.07115(11) 0.0174(3) Uani 1 1 d . . . H19A H 0.0405 0.4093 0.0643 0.021 Uiso 1 1 calc R . . H19B H 0.1375 0.4275 0.0251 0.021 Uiso 1 1 calc R . . C9 C -0.30644(13) 0.54907(14) 0.15789(11) 0.0181(3) Uani 1 1 d . . . C10 C -0.02205(13) 0.68817(13) 0.08636(11) 0.0171(3) Uani 1 1 d . . . C11 C -0.11381(13) 0.71742(14) 0.10473(11) 0.0183(4) Uani 1 1 d . . . C20 C 0.08726(13) 0.42052(14) 0.21664(11) 0.0189(4) Uani 1 1 d . . . H20A H 0.0583 0.4881 0.2153 0.023 Uiso 1 1 calc R . . H20B H 0.1252 0.4156 0.2660 0.023 Uiso 1 1 calc R . . C26 C 0.24063(13) 0.44544(14) 0.15494(12) 0.0189(4) Uani 1 1 d . . . H26A H 0.2625 0.4357 0.2107 0.023 Uiso 1 1 calc R . . H26B H 0.2428 0.5186 0.1426 0.023 Uiso 1 1 calc R . . C32 C 0.18596(17) 0.09701(15) 0.14217(14) 0.0313(5) Uani 1 1 d . . . H32A H 0.1508 0.0662 0.1849 0.047 Uiso 1 1 calc R . . H32B H 0.2510 0.0836 0.1515 0.047 Uiso 1 1 calc R . . H32C H 0.1667 0.0681 0.0907 0.047 Uiso 1 1 calc R . . N1 N -0.26205(12) 0.46679(12) 0.12763(10) 0.0217(3) Uani 1 1 d . . . C3 C -0.44026(14) 0.44821(15) 0.18385(12) 0.0240(4) Uani 1 1 d . . . H3 H -0.5004 0.4410 0.2030 0.029 Uiso 1 1 calc R . . C15 C 0.03996(14) 0.76131(14) 0.05694(12) 0.0195(4) Uani 1 1 d . . . C1 C -0.30594(15) 0.37965(15) 0.12572(12) 0.0236(4) Uani 1 1 d . . . H1 H -0.2753 0.3224 0.1049 0.028 Uiso 1 1 calc R . . C21 C 0.01437(14) 0.33929(15) 0.21684(12) 0.0211(4) Uani 1 1 d . . . C6 C -0.39081(15) 0.72039(16) 0.21902(13) 0.0250(4) Uani 1 1 d . . . H6 H -0.4188 0.7791 0.2401 0.030 Uiso 1 1 calc R . . C13 C -0.07594(15) 0.88949(14) 0.06621(12) 0.0240(4) Uani 1 1 d . . . H13 H -0.0946 0.9580 0.0607 0.029 Uiso 1 1 calc R . . C17 C 0.14665(14) 0.62550(15) 0.03871(12) 0.0228(4) Uani 1 1 d . . . H17 H 0.2040 0.6011 0.0218 0.027 Uiso 1 1 calc R . . C16 C 0.12639(15) 0.72659(15) 0.03414(13) 0.0239(4) Uani 1 1 d . . . H16 H 0.1706 0.7731 0.0156 0.029 Uiso 1 1 calc R . . C5 C -0.43835(14) 0.63181(15) 0.21788(13) 0.0248(4) Uani 1 1 d . . . H5 H -0.4987 0.6292 0.2372 0.030 Uiso 1 1 calc R . . C14 C 0.01214(15) 0.86409(15) 0.04965(12) 0.0241(4) Uani 1 1 d . . . H14 H 0.0541 0.9144 0.0335 0.029 Uiso 1 1 calc R . . C22 C -0.07241(15) 0.35710(17) 0.24452(13) 0.0268(4) Uani 1 1 d . . . H22 H -0.0886 0.4224 0.2632 0.032 Uiso 1 1 calc R . . C28 C 0.37134(14) 0.43285(16) 0.05813(13) 0.0246(4) Uani 1 1 d . . . H28 H 0.3816 0.5036 0.0626 0.029 Uiso 1 1 calc R . . C7 C -0.30160(14) 0.72772(14) 0.18990(12) 0.0217(4) Uani 1 1 d . . . H7 H -0.2708 0.7909 0.1917 0.026 Uiso 1 1 calc R . . N4 N 0.03866(12) 0.24673(12) 0.18907(10) 0.0209(3) Uani 1 1 d . . . C2 C -0.39558(15) 0.36656(15) 0.15271(13) 0.0255(4) Uani 1 1 d . . . H2 H -0.4245 0.3024 0.1494 0.031 Uiso 1 1 calc R . . C31 C 0.33767(15) 0.23002(16) 0.04544(13) 0.0266(4) Uani 1 1 d . . . H31 H 0.3255 0.1597 0.0407 0.032 Uiso 1 1 calc R . . C25 C -0.02405(15) 0.17183(16) 0.18813(14) 0.0277(4) Uani 1 1 d . . . H25 H -0.0075 0.1075 0.1677 0.033 Uiso 1 1 calc R . . C29 C 0.42727(15) 0.37330(18) 0.01057(14) 0.0297(5) Uani 1 1 d . . . H29 H 0.4763 0.4029 -0.0174 0.036 Uiso 1 1 calc R . . C4 C -0.39616(13) 0.54330(14) 0.18726(11) 0.0194(4) Uani 1 1 d . . . C23 C -0.13592(16) 0.27859(19) 0.24481(15) 0.0320(5) Uani 1 1 d . . . H23 H -0.1953 0.2892 0.2648 0.038 Uiso 1 1 calc R . . C30 C 0.41027(16) 0.27091(18) 0.00481(14) 0.0306(5) Uani 1 1 d . . . H30 H 0.4479 0.2289 -0.0267 0.037 Uiso 1 1 calc R . . C24 C -0.11085(16) 0.18529(18) 0.21557(15) 0.0320(5) Uani 1 1 d . . . H24 H -0.1532 0.1309 0.2144 0.038 Uiso 1 1 calc R . . P1 P 0.34231(4) 0.55181(4) 0.37408(3) 0.02037(10) Uani 1 1 d . . . F6 F 0.33144(9) 0.63220(10) 0.30305(8) 0.0313(3) Uani 1 1 d . . . F5 F 0.24617(9) 0.50207(9) 0.34698(8) 0.0294(3) Uani 1 1 d . . . F4 F 0.43711(10) 0.60071(11) 0.40060(9) 0.0405(3) Uani 1 1 d . . . F3 F 0.28957(10) 0.62647(10) 0.43234(8) 0.0368(3) Uani 1 1 d . . . F2 F 0.35181(11) 0.46998(10) 0.44405(8) 0.0375(3) Uani 1 1 d . . . F1 F 0.39301(10) 0.47594(11) 0.31464(9) 0.0375(3) Uani 1 1 d . . . N7 N 0.36416(16) 0.69499(18) 0.08771(16) 0.0459(6) Uani 1 1 d . . . C33 C 0.37603(16) 0.77916(19) 0.09767(15) 0.0330(5) Uani 1 1 d . . . C34 C 0.3935(2) 0.8863(2) 0.10986(16) 0.0458(7) Uani 1 1 d . . . H34A H 0.4519 0.8950 0.1383 0.069 Uiso 1 1 calc R . . H34B H 0.3446 0.9157 0.1414 0.069 Uiso 1 1 calc R . . H34C H 0.3957 0.9204 0.0580 0.069 Uiso 1 1 calc R . . H100 H -0.1484(19) 0.584(2) 0.1252(17) 0.040(8) Uiso 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 0.02067(8) 0.01393(7) 0.01918(8) -0.00044(5) -0.00116(5) 0.00025(5) N3 0.0175(8) 0.0165(7) 0.0162(7) 0.0007(6) -0.0008(6) 0.0004(5) N2 0.0175(8) 0.0155(7) 0.0286(9) -0.0006(6) 0.0045(7) 0.0019(6) C8 0.0183(9) 0.0188(8) 0.0185(9) -0.0002(7) -0.0002(7) 0.0012(7) N6 0.0218(8) 0.0201(7) 0.0191(8) -0.0009(6) -0.0008(6) 0.0020(6) N5 0.0178(8) 0.0169(7) 0.0166(7) -0.0004(6) -0.0014(6) -0.0004(6) C12 0.0247(10) 0.0195(8) 0.0191(9) 0.0000(7) 0.0009(7) 0.0035(7) C27 0.0190(9) 0.0217(9) 0.0178(9) -0.0003(7) -0.0031(7) 0.0021(7) C18 0.0202(9) 0.0195(8) 0.0150(8) 0.0020(7) -0.0004(7) 0.0010(7) C19 0.0184(9) 0.0182(8) 0.0156(8) -0.0005(6) -0.0023(7) 0.0021(6) C9 0.0196(9) 0.0177(8) 0.0171(8) 0.0005(7) -0.0016(7) 0.0015(7) C10 0.0204(9) 0.0161(8) 0.0148(8) -0.0002(6) -0.0010(7) -0.0005(6) C11 0.0222(10) 0.0165(8) 0.0161(9) -0.0018(7) -0.0005(7) 0.0000(7) C20 0.0230(10) 0.0186(8) 0.0152(8) -0.0010(7) 0.0006(7) -0.0012(7) C26 0.0178(9) 0.0178(8) 0.0210(9) -0.0010(7) -0.0033(7) -0.0006(6) C32 0.0426(13) 0.0170(9) 0.0341(12) -0.0001(8) -0.0020(10) 0.0018(8) N1 0.0229(9) 0.0184(7) 0.0240(8) 0.0005(6) 0.0015(7) 0.0026(6) C3 0.0202(10) 0.0268(10) 0.0248(10) 0.0036(8) 0.0004(8) -0.0037(7) C15 0.0214(9) 0.0193(8) 0.0179(9) 0.0023(7) 0.0011(7) -0.0022(7) C1 0.0276(11) 0.0187(9) 0.0245(10) 0.0001(7) 0.0005(8) 0.0013(7) C21 0.0229(10) 0.0225(9) 0.0180(9) 0.0030(7) -0.0016(7) -0.0003(7) C6 0.0250(11) 0.0229(9) 0.0272(11) -0.0027(8) 0.0044(8) 0.0053(8) C13 0.0341(12) 0.0155(8) 0.0224(10) 0.0023(7) 0.0010(8) 0.0022(7) C17 0.0198(10) 0.0262(9) 0.0224(10) 0.0032(8) 0.0031(8) 0.0002(7) C16 0.0226(10) 0.0247(9) 0.0245(10) 0.0056(8) 0.0043(8) -0.0031(7) C5 0.0199(10) 0.0258(10) 0.0287(11) 0.0003(8) 0.0047(8) 0.0026(7) C14 0.0322(11) 0.0176(8) 0.0225(10) 0.0030(7) 0.0025(8) -0.0037(7) C22 0.0251(11) 0.0284(10) 0.0268(11) 0.0033(8) 0.0008(8) 0.0024(8) C28 0.0197(10) 0.0274(10) 0.0266(10) 0.0025(8) -0.0006(8) -0.0015(7) C7 0.0226(10) 0.0189(8) 0.0238(10) -0.0025(7) 0.0015(8) 0.0002(7) N4 0.0213(8) 0.0203(7) 0.0210(8) 0.0023(6) -0.0029(6) -0.0013(6) C2 0.0270(11) 0.0215(9) 0.0280(11) 0.0017(8) -0.0017(8) -0.0037(8) C31 0.0256(11) 0.0280(10) 0.0261(10) -0.0036(8) -0.0005(8) 0.0066(8) C25 0.0282(11) 0.0228(9) 0.0319(11) 0.0039(8) -0.0042(9) -0.0053(8) C29 0.0211(11) 0.0400(12) 0.0283(11) 0.0027(9) 0.0025(8) 0.0007(9) C4 0.0183(9) 0.0210(8) 0.0190(9) 0.0015(7) 0.0001(7) 0.0004(7) C23 0.0199(11) 0.0396(12) 0.0363(12) 0.0101(10) 0.0001(9) 0.0009(9) C30 0.0253(11) 0.0411(12) 0.0253(11) -0.0043(9) 0.0010(9) 0.0064(9) C24 0.0243(11) 0.0325(11) 0.0390(13) 0.0116(10) -0.0058(9) -0.0067(9) P1 0.0220(3) 0.0159(2) 0.0231(2) 0.00020(18) -0.00054(19) -0.00104(17) F6 0.0338(7) 0.0275(6) 0.0324(7) 0.0115(5) -0.0015(6) -0.0051(5) F5 0.0260(7) 0.0278(6) 0.0342(7) 0.0009(5) -0.0018(5) -0.0082(5) F4 0.0292(7) 0.0396(8) 0.0521(9) 0.0023(7) -0.0139(6) -0.0104(6) F3 0.0472(9) 0.0313(7) 0.0320(7) -0.0095(6) 0.0036(6) 0.0076(6) F2 0.0516(9) 0.0290(7) 0.0318(7) 0.0112(6) -0.0076(6) -0.0009(6) F1 0.0364(8) 0.0369(7) 0.0396(8) -0.0084(6) 0.0069(6) 0.0109(6) N7 0.0357(12) 0.0399(12) 0.0618(16) 0.0028(11) -0.0083(11) -0.0004(9) C33 0.0263(12) 0.0385(12) 0.0341(12) 0.0006(10) -0.0020(9) 0.0034(9) C34 0.0656(19) 0.0379(14) 0.0335(14) -0.0047(11) -0.0094(13) 0.0040(13) _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 C32 2.022(2) . ? Pd1 N6 2.0228(17) . ? Pd1 N4 2.0274(18) . ? Pd1 N5 2.1315(16) . ? N3 C18 1.327(2) . ? N3 C10 1.366(2) . ? N2 C11 1.381(2) . ? N2 C8 1.389(3) . ? N2 H100 0.82(3) . ? C8 C7 1.387(3) . ? C8 C9 1.436(3) . ? N6 C31 1.343(3) . ? N6 C27 1.361(2) . ? N5 C20 1.485(2) . ? N5 C26 1.488(2) . ? N5 C19 1.496(2) . ? C12 C11 1.385(3) . ? C12 C13 1.412(3) . ? C12 H12 0.9500 . ? C27 C28 1.380(3) . ? C27 C26 1.515(3) . ? C18 C17 1.413(3) . ? C18 C19 1.516(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C9 N1 1.370(2) . ? C9 C4 1.417(3) . ? C10 C15 1.423(3) . ? C10 C11 1.440(3) . ? C20 C21 1.516(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 C1 1.320(3) . ? C3 C2 1.371(3) . ? C3 C4 1.415(3) . ? C3 H3 0.9500 . ? C15 C16 1.409(3) . ? C15 C14 1.424(3) . ? C1 C2 1.410(3) . ? C1 H1 0.9500 . ? C21 N4 1.359(2) . ? C21 C22 1.384(3) . ? C6 C5 1.363(3) . ? C6 C7 1.410(3) . ? C6 H6 0.9500 . ? C13 C14 1.369(3) . ? C13 H13 0.9500 . ? C17 C16 1.371(3) . ? C17 H17 0.9500 . ? C16 H16 0.9500 . ? C5 C4 1.424(3) . ? C5 H5 0.9500 . ? C14 H14 0.9500 . ? C22 C23 1.395(3) . ? C22 H22 0.9500 . ? C28 C29 1.398(3) . ? C28 H28 0.9500 . ? C7 H7 0.9500 . ? N4 C25 1.352(3) . ? C2 H2 0.9500 . ? C31 C30 1.385(3) . ? C31 H31 0.9500 . ? C25 C24 1.374(3) . ? C25 H25 0.9500 . ? C29 C30 1.380(3) . ? C29 H29 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C30 H30 0.9500 . ? C24 H24 0.9500 . ? P1 F4 1.5901(14) . ? P1 F3 1.5984(14) . ? P1 F2 1.5991(14) . ? P1 F6 1.6011(13) . ? P1 F1 1.6062(14) . ? P1 F5 1.6142(13) . ? N7 C33 1.138(3) . ? C33 C34 1.453(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 C32 Pd1 N6 96.77(9) . . ? C32 Pd1 N4 97.55(9) . . ? N6 Pd1 N4 165.68(6) . . ? C32 Pd1 N5 176.75(8) . . ? N6 Pd1 N5 83.00(6) . . ? N4 Pd1 N5 82.73(6) . . ? C18 N3 C10 118.32(16) . . ? C11 N2 C8 130.70(17) . . ? C11 N2 H100 114(2) . . ? C8 N2 H100 115(2) . . ? C7 C8 N2 126.06(18) . . ? C7 C8 C9 118.20(18) . . ? N2 C8 C9 115.69(16) . . ? C31 N6 C27 119.28(19) . . ? C31 N6 Pd1 128.05(15) . . ? C27 N6 Pd1 111.94(13) . . ? C20 N5 C26 115.64(15) . . ? C20 N5 C19 111.82(15) . . ? C26 N5 C19 112.61(15) . . ? C20 N5 Pd1 102.75(11) . . ? C26 N5 Pd1 102.34(11) . . ? C19 N5 Pd1 110.71(11) . . ? C11 C12 C13 120.80(19) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N6 C27 C28 121.30(18) . . ? N6 C27 C26 116.01(17) . . ? C28 C27 C26 122.67(18) . . ? N3 C18 C17 122.96(17) . . ? N3 C18 C19 116.45(16) . . ? C17 C18 C19 120.51(17) . . ? N5 C19 C18 115.11(15) . . ? N5 C19 H19A 108.5 . . ? C18 C19 H19A 108.5 . . ? N5 C19 H19B 108.5 . . ? C18 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? N1 C9 C4 122.51(17) . . ? N1 C9 C8 117.24(17) . . ? C4 C9 C8 120.25(17) . . ? N3 C10 C15 122.46(17) . . ? N3 C10 C11 117.46(17) . . ? C15 C10 C11 119.92(16) . . ? N2 C11 C12 125.65(18) . . ? N2 C11 C10 115.85(16) . . ? C12 C11 C10 118.39(18) . . ? N5 C20 C21 109.75(15) . . ? N5 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? N5 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? N5 C26 C27 109.06(15) . . ? N5 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? N5 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? Pd1 C32 H32A 109.5 . . ? Pd1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Pd1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1 C9 117.81(18) . . ? C2 C3 C4 119.54(19) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C16 C15 C10 117.25(17) . . ? C16 C15 C14 123.11(18) . . ? C10 C15 C14 119.62(18) . . ? N1 C1 C2 123.87(19) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? N4 C21 C22 121.13(19) . . ? N4 C21 C20 116.57(17) . . ? C22 C21 C20 122.29(18) . . ? C5 C6 C7 122.20(19) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C14 C13 C12 121.87(18) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C16 C17 C18 119.08(19) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C16 C15 119.87(18) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C6 C5 C4 119.01(19) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C13 C14 C15 119.15(18) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C21 C22 C23 119.6(2) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C27 C28 C29 119.2(2) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C8 C7 C6 120.70(18) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C25 N4 C21 118.72(18) . . ? C25 N4 Pd1 128.74(15) . . ? C21 N4 Pd1 112.04(13) . . ? C3 C2 C1 118.77(19) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? N6 C31 C30 121.9(2) . . ? N6 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? N4 C25 C24 122.4(2) . . ? N4 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C30 C29 C28 119.0(2) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C3 C4 C9 117.49(18) . . ? C3 C4 C5 122.88(18) . . ? C9 C4 C5 119.62(18) . . ? C24 C23 C22 118.8(2) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C29 C30 C31 119.2(2) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C25 C24 C23 119.3(2) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? F4 P1 F3 90.56(8) . . ? F4 P1 F2 90.39(8) . . ? F3 P1 F2 90.39(8) . . ? F4 P1 F6 90.68(8) . . ? F3 P1 F6 90.06(8) . . ? F2 P1 F6 178.84(8) . . ? F4 P1 F1 90.79(8) . . ? F3 P1 F1 178.63(9) . . ? F2 P1 F1 89.82(8) . . ? F6 P1 F1 89.70(8) . . ? F4 P1 F5 179.87(10) . . ? F3 P1 F5 89.55(8) . . ? F2 P1 F5 89.65(7) . . ? F6 P1 F5 89.28(7) . . ? F1 P1 F5 89.10(8) . . ? N7 C33 C34 178.6(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 C11 N2 C8 C7 -20.3(3) . . . . ? C11 N2 C8 C9 162.26(19) . . . . ? C32 Pd1 N6 C31 24.16(19) . . . . ? N4 Pd1 N6 C31 -153.9(2) . . . . ? N5 Pd1 N6 C31 -159.11(18) . . . . ? C32 Pd1 N6 C27 -165.86(14) . . . . ? N4 Pd1 N6 C27 16.0(3) . . . . ? N5 Pd1 N6 C27 10.87(13) . . . . ? C32 Pd1 N5 C20 -64.4(15) . . . . ? N6 Pd1 N5 C20 -150.49(12) . . . . ? N4 Pd1 N5 C20 30.80(11) . . . . ? C32 Pd1 N5 C26 55.9(15) . . . . ? N6 Pd1 N5 C26 -30.25(11) . . . . ? N4 Pd1 N5 C26 151.04(12) . . . . ? C32 Pd1 N5 C19 176.1(15) . . . . ? N6 Pd1 N5 C19 89.98(12) . . . . ? N4 Pd1 N5 C19 -88.73(12) . . . . ? C31 N6 C27 C28 1.3(3) . . . . ? Pd1 N6 C27 C28 -169.62(15) . . . . ? C31 N6 C27 C26 -176.77(17) . . . . ? Pd1 N6 C27 C26 12.3(2) . . . . ? C10 N3 C18 C17 1.6(3) . . . . ? C10 N3 C18 C19 -175.17(16) . . . . ? C20 N5 C19 C18 65.1(2) . . . . ? C26 N5 C19 C18 -67.1(2) . . . . ? Pd1 N5 C19 C18 178.99(13) . . . . ? N3 C18 C19 N5 -93.7(2) . . . . ? C17 C18 C19 N5 89.4(2) . . . . ? C7 C8 C9 N1 -179.29(18) . . . . ? N2 C8 C9 N1 -1.7(3) . . . . ? C7 C8 C9 C4 1.0(3) . . . . ? N2 C8 C9 C4 178.57(17) . . . . ? C18 N3 C10 C15 -1.9(3) . . . . ? C18 N3 C10 C11 173.53(17) . . . . ? C8 N2 C11 C12 -9.8(3) . . . . ? C8 N2 C11 C10 174.05(19) . . . . ? C13 C12 C11 N2 179.09(19) . . . . ? C13 C12 C11 C10 -4.9(3) . . . . ? N3 C10 C11 N2 2.3(3) . . . . ? C15 C10 C11 N2 177.83(17) . . . . ? N3 C10 C11 C12 -174.12(17) . . . . ? C15 C10 C11 C12 1.4(3) . . . . ? C26 N5 C20 C21 -152.39(15) . . . . ? C19 N5 C20 C21 76.97(18) . . . . ? Pd1 N5 C20 C21 -41.79(16) . . . . ? C20 N5 C26 C27 154.22(15) . . . . ? C19 N5 C26 C27 -75.52(18) . . . . ? Pd1 N5 C26 C27 43.39(16) . . . . ? N6 C27 C26 N5 -39.9(2) . . . . ? C28 C27 C26 N5 142.01(19) . . . . ? C4 C9 N1 C1 0.5(3) . . . . ? C8 C9 N1 C1 -179.24(18) . . . . ? N3 C10 C15 C16 0.2(3) . . . . ? C11 C10 C15 C16 -175.14(18) . . . . ? N3 C10 C15 C14 178.45(18) . . . . ? C11 C10 C15 C14 3.1(3) . . . . ? C9 N1 C1 C2 0.2(3) . . . . ? N5 C20 C21 N4 35.4(2) . . . . ? N5 C20 C21 C22 -145.25(19) . . . . ? C11 C12 C13 C14 3.9(3) . . . . ? N3 C18 C17 C16 0.3(3) . . . . ? C19 C18 C17 C16 177.04(19) . . . . ? C18 C17 C16 C15 -2.1(3) . . . . ? C10 C15 C16 C17 1.8(3) . . . . ? C14 C15 C16 C17 -176.4(2) . . . . ? C7 C6 C5 C4 0.9(3) . . . . ? C12 C13 C14 C15 0.8(3) . . . . ? C16 C15 C14 C13 173.9(2) . . . . ? C10 C15 C14 C13 -4.2(3) . . . . ? N4 C21 C22 C23 0.7(3) . . . . ? C20 C21 C22 C23 -178.57(19) . . . . ? N6 C27 C28 C29 -1.5(3) . . . . ? C26 C27 C28 C29 176.44(19) . . . . ? N2 C8 C7 C6 -178.14(19) . . . . ? C9 C8 C7 C6 -0.8(3) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C22 C21 N4 C25 0.7(3) . . . . ? C20 C21 N4 C25 179.96(18) . . . . ? C22 C21 N4 Pd1 173.27(16) . . . . ? C20 C21 N4 Pd1 -7.4(2) . . . . ? C32 Pd1 N4 C25 -25.39(19) . . . . ? N6 Pd1 N4 C25 152.7(2) . . . . ? N5 Pd1 N4 C25 157.87(18) . . . . ? C32 Pd1 N4 C21 162.91(14) . . . . ? N6 Pd1 N4 C21 -19.0(3) . . . . ? N5 Pd1 N4 C21 -13.82(13) . . . . ? C4 C3 C2 C1 0.8(3) . . . . ? N1 C1 C2 C3 -0.8(3) . . . . ? C27 N6 C31 C30 0.0(3) . . . . ? Pd1 N6 C31 C30 169.29(16) . . . . ? C21 N4 C25 C24 -1.2(3) . . . . ? Pd1 N4 C25 C24 -172.46(17) . . . . ? C27 C28 C29 C30 0.5(3) . . . . ? C2 C3 C4 C9 -0.1(3) . . . . ? C2 C3 C4 C5 179.3(2) . . . . ? N1 C9 C4 C3 -0.5(3) . . . . ? C8 C9 C4 C3 179.20(18) . . . . ? N1 C9 C4 C5 -179.97(18) . . . . ? C8 C9 C4 C5 -0.2(3) . . . . ? C6 C5 C4 C3 179.9(2) . . . . ? C6 C5 C4 C9 -0.7(3) . . . . ? C21 C22 C23 C24 -1.5(3) . . . . ? C28 C29 C30 C31 0.8(3) . . . . ? N6 C31 C30 C29 -1.0(3) . . . . ? N4 C25 C24 C23 0.4(3) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.569 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.086 #===END data_14 _database_code_depnum_ccdc_archive 'CCDC 766174' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H28 Cl F6 N6 O1.50 P Pd2 S1.50' _chemical_formula_weight 997.94 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.542(3) _cell_length_b 32.618(5) _cell_length_c 14.722(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.131(2) _cell_angle_gamma 90.00 _cell_volume 7505(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.31 _exptl_crystal_description red _exptl_crystal_colour plate _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7916 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus 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 8.3 _diffrn_reflns_number 58464 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7673 _reflns_number_gt 6414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0458P)^2^+60.9976P] 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 consort _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7673 _refine_ls_number_parameters 527 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _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 -0.19614(2) 0.951711(10) 0.57328(2) 0.02540(10) Uani 1 1 d . . . Pd2 Pd -0.24187(2) 0.923859(11) 0.35442(2) 0.02668(10) Uani 1 1 d . . . Cl1 Cl -0.10259(7) 1.00509(3) 0.57228(7) 0.0278(2) Uani 1 1 d . . . P1 P -0.79238(11) 0.84272(6) 0.46374(13) 0.0568(4) Uani 1 1 d . . . N5 N -0.1105(2) 0.91948(11) 0.3659(2) 0.0256(7) Uani 1 1 d . . . N6 N -0.2233(2) 0.98417(11) 0.3361(2) 0.0272(8) Uani 1 1 d . . . C32 C -0.3717(3) 0.92699(14) 0.3378(3) 0.0274(9) Uani 1 1 d . . . H32A H -0.3954 0.9527 0.3056 0.041 Uiso 1 1 calc R . . H32B H -0.3792 0.9260 0.4011 0.041 Uiso 1 1 calc R . . H32C H -0.4015 0.9038 0.2988 0.041 Uiso 1 1 calc R . . N3 N -0.1241(2) 0.90093(11) 0.5689(2) 0.0265(7) Uani 1 1 d . . . N2 N -0.2709(2) 0.90990(13) 0.6003(3) 0.0322(8) Uani 1 1 d . . . N1 N -0.2866(2) 0.99024(13) 0.5871(3) 0.0312(8) Uani 1 1 d . . . C26 C -0.1020(3) 0.95354(14) 0.3018(3) 0.0293(9) Uani 1 1 d . . . H26A H -0.1270 0.9451 0.2338 0.035 Uiso 1 1 calc R . . H26B H -0.0407 0.9599 0.3146 0.035 Uiso 1 1 calc R . . C18 C -0.0587(3) 0.89545(13) 0.5348(3) 0.0275(9) Uani 1 1 d . . . C27 C -0.1474(3) 0.99098(14) 0.3198(3) 0.0287(9) Uani 1 1 d . . . N4 N -0.2325(3) 0.86187(12) 0.3675(3) 0.0356(9) Uani 1 1 d . . . C19 C -0.0453(3) 0.92556(14) 0.4640(3) 0.0276(9) Uani 1 1 d . . . H19A H 0.0129 0.9220 0.4601 0.033 Uiso 1 1 calc R . . H19B H -0.0499 0.9538 0.4864 0.033 Uiso 1 1 calc R . . C8 C -0.3450(3) 0.92536(17) 0.6119(3) 0.0362(11) Uani 1 1 d . . . C28 C -0.1167(3) 1.03028(14) 0.3172(3) 0.0323(10) Uani 1 1 d . . . H28 H -0.0642 1.0346 0.3056 0.039 Uiso 1 1 calc R . . C31 C -0.2676(3) 1.01680(15) 0.3498(3) 0.0306(9) Uani 1 1 d . . . H31 H -0.3201 1.0122 0.3615 0.037 Uiso 1 1 calc R . . F6 F -0.8314(3) 0.88646(13) 0.4321(3) 0.0824(13) Uani 1 1 d . . . C29 C -0.1643(3) 1.06351(15) 0.3318(3) 0.0364(11) Uani 1 1 d . . . H29 H -0.1442 1.0907 0.3306 0.044 Uiso 1 1 calc R . . C15 C -0.1018(3) 0.83204(14) 0.6382(3) 0.0355(11) Uani 1 1 d . . . C16 C -0.0287(3) 0.82892(15) 0.6100(4) 0.0394(11) Uani 1 1 d . . . H16 H 0.0069 0.8054 0.6272 0.047 Uiso 1 1 calc R . . C11 C -0.2290(3) 0.87374(15) 0.6342(3) 0.0330(10) Uani 1 1 d . . . F5 F -0.8143(3) 0.84793(18) 0.5604(3) 0.0947(15) Uani 1 1 d . . . C17 C -0.0084(3) 0.85960(15) 0.5579(3) 0.0350(10) Uani 1 1 d . . . H17 H 0.0400 0.8568 0.5371 0.042 Uiso 1 1 calc R . . C21 C -0.1592(3) 0.84738(15) 0.3562(3) 0.0360(11) Uani 1 1 d . . . C10 C -0.1500(3) 0.86895(14) 0.6143(3) 0.0307(10) Uani 1 1 d . . . C20 C -0.1043(3) 0.87789(15) 0.3261(3) 0.0351(10) Uani 1 1 d . . . H20A H -0.0440 0.8686 0.3494 0.042 Uiso 1 1 calc R . . H20B H -0.1229 0.8793 0.2551 0.042 Uiso 1 1 calc R . . C1 C -0.2894(3) 1.03064(16) 0.5799(3) 0.0359(11) Uani 1 1 d . . . H1 H -0.2444 1.0448 0.5666 0.043 Uiso 1 1 calc R . . C30 C -0.2406(3) 1.05651(16) 0.3479(3) 0.0364(11) Uani 1 1 d . . . H30 H -0.2739 1.0788 0.3575 0.044 Uiso 1 1 calc R . . C12 C -0.2527(4) 0.84263(16) 0.6847(4) 0.0420(12) Uani 1 1 d . . . H12 H -0.3033 0.8453 0.7013 0.050 Uiso 1 1 calc R . . C9 C -0.3528(3) 0.96911(17) 0.6045(3) 0.0369(11) Uani 1 1 d . . . C6 C -0.4834(3) 0.9252(2) 0.6371(4) 0.0531(16) Uani 1 1 d . . . H6 H -0.5286 0.9099 0.6474 0.064 Uiso 1 1 calc R . . F4 F -0.6984(3) 0.86114(18) 0.5206(4) 0.1003(16) Uani 1 1 d . . . C7 C -0.4134(3) 0.9035(2) 0.6249(3) 0.0462(13) Uani 1 1 d . . . H7 H -0.4127 0.8744 0.6256 0.055 Uiso 1 1 calc R . . F3 F -0.7609(4) 0.79957(16) 0.4941(4) 0.1051(16) Uani 1 1 d . . . C25 C -0.2847(4) 0.83550(17) 0.3928(4) 0.0450(13) Uani 1 1 d . . . H25 H -0.3358 0.8456 0.4009 0.054 Uiso 1 1 calc R . . F2 F -0.8854(3) 0.82640(16) 0.4084(4) 0.1083(18) Uani 1 1 d . . . C13 C -0.2023(4) 0.80716(17) 0.7114(4) 0.0489(14) Uani 1 1 d . . . H13 H -0.2190 0.7868 0.7478 0.059 Uiso 1 1 calc R . . C14 C -0.1297(4) 0.80054(16) 0.6872(4) 0.0462(13) Uani 1 1 d . . . H14 H -0.0991 0.7755 0.7029 0.055 Uiso 1 1 calc R . . C4 C -0.4234(3) 0.9900(2) 0.6166(3) 0.0447(13) Uani 1 1 d . . . C5 C -0.4888(3) 0.9665(3) 0.6348(4) 0.0571(17) Uani 1 1 d . . . H5 H -0.5361 0.9797 0.6452 0.068 Uiso 1 1 calc R . . C23 C -0.1914(5) 0.77948(17) 0.3967(4) 0.0587(17) Uani 1 1 d . . . H23 H -0.1773 0.7512 0.4069 0.070 Uiso 1 1 calc R . . C22 C -0.1374(4) 0.80623(17) 0.3712(4) 0.0490(14) Uani 1 1 d . . . H22 H -0.0857 0.7965 0.3641 0.059 Uiso 1 1 calc R . . F1 F -0.7672(4) 0.8399(2) 0.3696(3) 0.129(2) Uani 1 1 d . . . C2 C -0.3582(3) 1.05307(18) 0.5917(3) 0.0428(13) Uani 1 1 d . . . H2 H -0.3589 1.0821 0.5872 0.051 Uiso 1 1 calc R . . C3 C -0.4235(4) 1.0331(2) 0.6093(4) 0.0502(15) Uani 1 1 d . . . H3 H -0.4698 1.0484 0.6167 0.060 Uiso 1 1 calc R . . C24 C -0.2653(4) 0.79435(18) 0.4069(5) 0.0579(17) Uani 1 1 d . . . H24 H -0.3033 0.7763 0.4237 0.070 Uiso 1 1 calc R . . S1 S -0.5325(3) 0.81063(16) 0.4645(4) 0.0728(18) Uani 0.391(6) 1 d PU A 1 S2 S -0.5649(4) 0.79338(16) 0.3523(4) 0.0583(18) Uani 0.335(6) 1 d PU A 2 S3 S -0.4989(6) 0.7911(2) 0.4248(8) 0.088(4) Uani 0.274(8) 1 d PU A 3 C100 C -0.5960(6) 0.7671(3) 0.4191(9) 0.108(3) Uani 1 1 d U . . C101 C -0.5376(7) 0.8428(3) 0.3898(10) 0.115(3) Uani 1 1 d U . . O101 O -0.4915(8) 0.7801(4) 0.3280(10) 0.124(4) Uani 0.609(6) 1 d PU A 1 O100 O -0.4465(8) 0.7947(4) 0.5058(14) 0.103(6) Uani 0.391(6) 1 d PU A 2 S200 S -0.4722(4) 0.80360(17) 0.7401(4) 0.1037(16) Uani 0.50 1 d PU B -1 O200 O -0.4454(9) 0.7979(4) 0.6559(11) 0.112(4) Uani 0.50 1 d PU B -1 C200 C -0.4161(9) 0.7730(6) 0.8090(10) 0.176(6) Uani 1 1 d U B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02381(17) 0.03181(19) 0.02019(17) -0.00023(12) 0.00668(13) -0.00126(13) Pd2 0.02329(17) 0.03384(19) 0.02134(17) 0.00040(12) 0.00518(13) -0.00275(13) Cl1 0.0282(5) 0.0288(5) 0.0256(5) -0.0011(4) 0.0078(4) -0.0015(4) P1 0.0538(9) 0.0650(10) 0.0535(9) 0.0041(8) 0.0203(8) 0.0156(8) N5 0.0282(18) 0.0276(18) 0.0208(17) -0.0008(14) 0.0079(15) 0.0019(14) N6 0.0264(18) 0.033(2) 0.0178(16) -0.0007(14) 0.0014(14) 0.0031(15) C32 0.019(2) 0.041(2) 0.0190(19) 0.0044(17) 0.0032(16) -0.0036(17) N3 0.0252(18) 0.0295(19) 0.0226(17) -0.0004(14) 0.0049(14) -0.0037(14) N2 0.031(2) 0.041(2) 0.0258(19) -0.0007(16) 0.0117(16) -0.0093(17) N1 0.0279(19) 0.046(2) 0.0186(17) -0.0034(15) 0.0062(15) 0.0020(16) C26 0.030(2) 0.036(2) 0.022(2) 0.0008(17) 0.0091(18) -0.0018(18) C18 0.024(2) 0.030(2) 0.023(2) -0.0020(17) 0.0012(17) -0.0004(17) C27 0.026(2) 0.039(2) 0.0185(19) 0.0025(17) 0.0042(17) 0.0016(18) N4 0.039(2) 0.033(2) 0.028(2) 0.0004(16) 0.0021(17) -0.0078(17) C19 0.022(2) 0.035(2) 0.025(2) -0.0011(17) 0.0062(17) 0.0013(17) C8 0.029(2) 0.059(3) 0.020(2) -0.002(2) 0.0076(18) -0.007(2) C28 0.035(2) 0.037(3) 0.023(2) 0.0044(18) 0.0075(19) 0.0001(19) C31 0.025(2) 0.041(3) 0.023(2) 0.0018(18) 0.0036(17) 0.0069(19) F6 0.101(3) 0.067(3) 0.079(3) 0.018(2) 0.030(3) 0.036(2) C29 0.047(3) 0.031(2) 0.023(2) 0.0052(18) 0.001(2) -0.003(2) C15 0.043(3) 0.031(2) 0.025(2) 0.0000(18) 0.001(2) -0.004(2) C16 0.045(3) 0.031(2) 0.033(3) 0.0006(19) 0.001(2) 0.006(2) C11 0.038(2) 0.039(3) 0.020(2) -0.0065(18) 0.0056(19) -0.012(2) F5 0.083(3) 0.138(4) 0.071(3) 0.011(3) 0.037(2) 0.023(3) C17 0.032(2) 0.036(3) 0.033(2) -0.0006(19) 0.004(2) 0.0063(19) C21 0.043(3) 0.034(2) 0.025(2) -0.0067(19) 0.004(2) -0.004(2) C10 0.037(2) 0.032(2) 0.020(2) 0.0015(17) 0.0036(18) -0.0049(19) C20 0.038(3) 0.038(3) 0.029(2) -0.0067(19) 0.010(2) 0.001(2) C1 0.036(3) 0.046(3) 0.022(2) -0.0050(19) 0.0045(19) 0.005(2) C30 0.041(3) 0.039(3) 0.024(2) -0.0004(19) 0.004(2) 0.013(2) C12 0.051(3) 0.044(3) 0.031(2) -0.003(2) 0.012(2) -0.019(2) C9 0.025(2) 0.066(3) 0.018(2) -0.003(2) 0.0048(18) 0.002(2) C6 0.031(3) 0.101(5) 0.026(3) 0.004(3) 0.009(2) -0.014(3) F4 0.071(3) 0.125(4) 0.107(4) -0.002(3) 0.032(3) -0.009(3) C7 0.034(3) 0.079(4) 0.026(2) -0.001(2) 0.010(2) -0.014(3) F3 0.118(4) 0.082(3) 0.116(4) -0.006(3) 0.040(3) -0.003(3) C25 0.041(3) 0.047(3) 0.038(3) 0.007(2) 0.002(2) -0.013(2) F2 0.080(3) 0.091(4) 0.134(5) -0.031(3) 0.008(3) 0.003(3) C13 0.063(4) 0.045(3) 0.034(3) 0.005(2) 0.009(3) -0.021(3) C14 0.063(4) 0.033(3) 0.033(3) 0.004(2) 0.002(2) -0.010(2) C4 0.030(3) 0.081(4) 0.020(2) -0.002(2) 0.0049(19) 0.008(3) C5 0.029(3) 0.112(6) 0.032(3) 0.004(3) 0.012(2) 0.006(3) C23 0.072(4) 0.030(3) 0.055(4) 0.003(2) -0.004(3) -0.012(3) C22 0.056(3) 0.038(3) 0.041(3) -0.007(2) -0.001(3) -0.002(2) F1 0.119(4) 0.215(7) 0.060(3) 0.022(4) 0.038(3) 0.076(5) C2 0.039(3) 0.057(3) 0.028(2) -0.004(2) 0.004(2) 0.017(2) C3 0.039(3) 0.081(4) 0.027(2) -0.005(3) 0.005(2) 0.021(3) C24 0.058(4) 0.044(3) 0.057(4) 0.010(3) -0.002(3) -0.021(3) S1 0.065(3) 0.069(3) 0.076(3) -0.007(2) 0.012(2) -0.004(2) S2 0.065(4) 0.061(3) 0.050(3) -0.009(2) 0.022(3) 0.007(2) S3 0.073(6) 0.068(4) 0.142(9) -0.026(5) 0.063(6) -0.006(4) C100 0.100(6) 0.082(5) 0.169(9) -0.050(5) 0.081(7) -0.023(5) C101 0.104(7) 0.067(4) 0.181(10) -0.006(5) 0.058(7) 0.015(4) O101 0.111(8) 0.111(8) 0.176(11) -0.039(8) 0.080(8) 0.000(7) O100 0.047(7) 0.064(8) 0.148(13) 0.015(8) -0.036(8) 0.005(6) S200 0.126(5) 0.097(3) 0.103(4) -0.003(3) 0.058(3) -0.024(3) O200 0.105(9) 0.113(10) 0.140(9) -0.022(8) 0.073(8) -0.040(8) C200 0.137(11) 0.265(18) 0.122(9) -0.018(9) 0.038(9) 0.082(11) _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 1.967(4) . ? Pd1 N1 2.015(4) . ? Pd1 N3 2.054(4) . ? Pd1 Cl1 2.3329(11) . ? Pd1 Pd2 3.1909(7) . ? Pd2 N6 2.023(4) . ? Pd2 N4 2.032(4) . ? Pd2 C32 2.083(4) . ? Pd2 N5 2.129(4) . ? P1 F3 1.516(6) . ? P1 F6 1.573(4) . ? P1 F1 1.576(5) . ? P1 F2 1.578(5) . ? P1 F5 1.588(5) . ? P1 F4 1.620(5) . ? N5 C26 1.493(5) . ? N5 C20 1.494(6) . ? N5 C19 1.506(5) . ? N6 C31 1.345(6) . ? N6 C27 1.371(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N3 C18 1.344(6) . ? N3 C10 1.381(6) . ? N2 C11 1.377(6) . ? N2 C8 1.386(6) . ? N1 C1 1.322(6) . ? N1 C9 1.387(6) . ? C26 C27 1.502(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C18 C17 1.411(6) . ? C18 C19 1.501(6) . ? C27 C28 1.384(7) . ? N4 C25 1.355(6) . ? N4 C21 1.360(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C8 C7 1.402(7) . ? C8 C9 1.434(8) . ? C28 C29 1.397(7) . ? C28 H28 0.9500 . ? C31 C30 1.374(7) . ? C31 H31 0.9500 . ? C29 C30 1.376(7) . ? C29 H29 0.9500 . ? C15 C16 1.406(8) . ? C15 C14 1.417(7) . ? C15 C10 1.423(7) . ? C16 C17 1.368(7) . ? C16 H16 0.9500 . ? C11 C12 1.388(7) . ? C11 C10 1.439(7) . ? C17 H17 0.9500 . ? C21 C22 1.389(7) . ? C21 C20 1.509(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C1 C2 1.411(7) . ? C1 H1 0.9500 . ? C30 H30 0.9500 . ? C12 C13 1.405(8) . ? C12 H12 0.9500 . ? C9 C4 1.412(7) . ? C6 C5 1.349(10) . ? C6 C7 1.418(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C25 C24 1.380(8) . ? C25 H25 0.9500 . ? C13 C14 1.376(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C4 C3 1.412(9) . ? C4 C5 1.421(9) . ? C5 H5 0.9500 . ? C23 C24 1.369(10) . ? C23 C22 1.385(9) . ? C23 H23 0.9500 . ? C22 H22 0.9500 . ? C2 C3 1.355(9) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C24 H24 0.9500 . ? S1 C101 1.502(13) . ? S1 C100 1.762(10) . ? S2 C100 1.517(12) . ? S2 C101 1.715(11) . ? S3 C100 1.764(12) . ? S3 C101 1.818(13) . ? S200 O200 1.460(14) . ? S200 C200 1.507(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 Pd1 N1 82.80(17) . . ? N2 Pd1 N3 81.82(16) . . ? N1 Pd1 N3 164.59(15) . . ? N2 Pd1 Cl1 168.82(11) . . ? N1 Pd1 Cl1 92.95(12) . . ? N3 Pd1 Cl1 102.03(10) . . ? N2 Pd1 Pd2 92.87(11) . . ? N1 Pd1 Pd2 109.96(10) . . ? N3 Pd1 Pd2 71.73(10) . . ? Cl1 Pd1 Pd2 98.30(3) . . ? N6 Pd2 N4 165.95(16) . . ? N6 Pd2 C32 97.60(16) . . ? N4 Pd2 C32 95.96(17) . . ? N6 Pd2 N5 83.12(14) . . ? N4 Pd2 N5 83.18(15) . . ? C32 Pd2 N5 177.68(15) . . ? N6 Pd2 Pd1 82.06(10) . . ? N4 Pd2 Pd1 101.66(11) . . ? C32 Pd2 Pd1 89.93(12) . . ? N5 Pd2 Pd1 92.36(9) . . ? F3 P1 F6 176.0(3) . . ? F3 P1 F1 92.3(3) . . ? F6 P1 F1 89.6(3) . . ? F3 P1 F2 91.2(3) . . ? F6 P1 F2 85.2(3) . . ? F1 P1 F2 91.2(4) . . ? F3 P1 F5 89.6(3) . . ? F6 P1 F5 88.7(3) . . ? F1 P1 F5 176.6(4) . . ? F2 P1 F5 91.7(3) . . ? F3 P1 F4 90.7(3) . . ? F6 P1 F4 92.8(3) . . ? F1 P1 F4 89.5(3) . . ? F2 P1 F4 177.9(3) . . ? F5 P1 F4 87.6(3) . . ? C26 N5 C20 113.3(3) . . ? C26 N5 C19 108.8(3) . . ? C20 N5 C19 112.1(3) . . ? C26 N5 Pd2 101.8(3) . . ? C20 N5 Pd2 103.2(3) . . ? C19 N5 Pd2 117.3(3) . . ? C31 N6 C27 118.3(4) . . ? C31 N6 Pd2 129.5(3) . . ? C27 N6 Pd2 111.6(3) . . ? Pd2 C32 H32A 109.5 . . ? Pd2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Pd2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C18 N3 C10 119.7(4) . . ? C18 N3 Pd1 131.7(3) . . ? C10 N3 Pd1 108.6(3) . . ? C11 N2 C8 128.9(4) . . ? C11 N2 Pd1 113.1(3) . . ? C8 N2 Pd1 114.4(3) . . ? C1 N1 C9 120.1(4) . . ? C1 N1 Pd1 128.4(3) . . ? C9 N1 Pd1 111.5(3) . . ? N5 C26 C27 109.7(3) . . ? N5 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N5 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N3 C18 C17 120.3(4) . . ? N3 C18 C19 119.5(4) . . ? C17 C18 C19 120.0(4) . . ? N6 C27 C28 121.3(4) . . ? N6 C27 C26 116.0(4) . . ? C28 C27 C26 122.6(4) . . ? C25 N4 C21 119.1(5) . . ? C25 N4 Pd2 128.5(4) . . ? C21 N4 Pd2 112.2(3) . . ? C18 C19 N5 111.0(3) . . ? C18 C19 H19A 109.4 . . ? N5 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? N5 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N2 C8 C7 128.1(5) . . ? N2 C8 C9 114.5(4) . . ? C7 C8 C9 117.4(5) . . ? C27 C28 C29 119.0(4) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? N6 C31 C30 123.1(4) . . ? N6 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C30 C29 C28 119.5(5) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C16 C15 C14 123.6(5) . . ? C16 C15 C10 117.0(4) . . ? C14 C15 C10 119.4(5) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N2 C11 C12 128.6(5) . . ? N2 C11 C10 113.7(4) . . ? C12 C11 C10 117.7(5) . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N4 C21 C22 120.8(5) . . ? N4 C21 C20 116.9(4) . . ? C22 C21 C20 122.2(5) . . ? N3 C10 C15 121.4(4) . . ? N3 C10 C11 117.6(4) . . ? C15 C10 C11 120.9(4) . . ? N5 C20 C21 111.0(4) . . ? N5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N1 C1 C2 121.0(5) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C31 C30 C29 118.9(5) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N1 C9 C4 121.3(5) . . ? N1 C9 C8 116.8(4) . . ? C4 C9 C8 121.9(5) . . ? C5 C6 C7 123.0(5) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C8 C7 C6 119.5(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? N4 C25 C24 121.4(6) . . ? N4 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C14 C13 C12 123.0(5) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 118.4(5) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C3 C4 C9 116.8(5) . . ? C3 C4 C5 124.8(5) . . ? C9 C4 C5 118.4(6) . . ? C6 C5 C4 119.7(6) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C22 C21 119.6(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C23 C24 C25 120.0(6) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C101 S1 C100 113.6(7) . . ? C100 S2 C101 115.6(6) . . ? C100 S3 C101 99.6(7) . . ? S2 C100 S1 60.2(4) . . ? S2 C100 S3 44.1(5) . . ? S1 C100 S3 37.3(4) . . ? S1 C101 S2 61.7(5) . . ? S1 C101 S3 38.2(4) . . ? S2 C101 S3 41.5(4) . . ? O200 S200 C200 101.3(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _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 Pd2 N6 148.23(16) . . . . ? N1 Pd1 Pd2 N6 64.85(16) . . . . ? N3 Pd1 Pd2 N6 -131.36(15) . . . . ? Cl1 Pd1 Pd2 N6 -31.37(11) . . . . ? N2 Pd1 Pd2 N4 -45.53(17) . . . . ? N1 Pd1 Pd2 N4 -128.91(17) . . . . ? N3 Pd1 Pd2 N4 34.88(16) . . . . ? Cl1 Pd1 Pd2 N4 134.88(13) . . . . ? N2 Pd1 Pd2 C32 50.54(17) . . . . ? N1 Pd1 Pd2 C32 -32.83(18) . . . . ? N3 Pd1 Pd2 C32 130.95(16) . . . . ? Cl1 Pd1 Pd2 C32 -129.05(13) . . . . ? N2 Pd1 Pd2 N5 -129.05(15) . . . . ? N1 Pd1 Pd2 N5 147.57(16) . . . . ? N3 Pd1 Pd2 N5 -48.65(14) . . . . ? Cl1 Pd1 Pd2 N5 51.35(10) . . . . ? N6 Pd2 N5 C26 -31.0(2) . . . . ? N4 Pd2 N5 C26 145.9(3) . . . . ? C32 Pd2 N5 C26 77(4) . . . . ? Pd1 Pd2 N5 C26 -112.7(2) . . . . ? N6 Pd2 N5 C20 -148.7(3) . . . . ? N4 Pd2 N5 C20 28.2(3) . . . . ? C32 Pd2 N5 C20 -40(4) . . . . ? Pd1 Pd2 N5 C20 129.6(2) . . . . ? N6 Pd2 N5 C19 87.6(3) . . . . ? N4 Pd2 N5 C19 -95.6(3) . . . . ? C32 Pd2 N5 C19 -164(4) . . . . ? Pd1 Pd2 N5 C19 5.9(3) . . . . ? N4 Pd2 N6 C31 -170.9(5) . . . . ? C32 Pd2 N6 C31 24.4(4) . . . . ? N5 Pd2 N6 C31 -157.9(4) . . . . ? Pd1 Pd2 N6 C31 -64.5(3) . . . . ? N4 Pd2 N6 C27 -0.4(7) . . . . ? C32 Pd2 N6 C27 -165.2(3) . . . . ? N5 Pd2 N6 C27 12.6(3) . . . . ? Pd1 Pd2 N6 C27 106.0(3) . . . . ? N2 Pd1 N3 C18 164.9(4) . . . . ? N1 Pd1 N3 C18 168.0(5) . . . . ? Cl1 Pd1 N3 C18 -25.7(4) . . . . ? Pd2 Pd1 N3 C18 69.1(4) . . . . ? N2 Pd1 N3 C10 -18.1(3) . . . . ? N1 Pd1 N3 C10 -15.0(7) . . . . ? Cl1 Pd1 N3 C10 151.2(3) . . . . ? Pd2 Pd1 N3 C10 -113.9(3) . . . . ? N1 Pd1 N2 C11 -158.6(3) . . . . ? N3 Pd1 N2 C11 20.6(3) . . . . ? Cl1 Pd1 N2 C11 -90.4(7) . . . . ? Pd2 Pd1 N2 C11 91.7(3) . . . . ? N1 Pd1 N2 C8 1.8(3) . . . . ? N3 Pd1 N2 C8 -179.0(3) . . . . ? Cl1 Pd1 N2 C8 70.0(8) . . . . ? Pd2 Pd1 N2 C8 -107.9(3) . . . . ? N2 Pd1 N1 C1 179.5(4) . . . . ? N3 Pd1 N1 C1 176.4(4) . . . . ? Cl1 Pd1 N1 C1 9.9(4) . . . . ? Pd2 Pd1 N1 C1 -90.0(4) . . . . ? N2 Pd1 N1 C9 -1.8(3) . . . . ? N3 Pd1 N1 C9 -4.9(7) . . . . ? Cl1 Pd1 N1 C9 -171.4(3) . . . . ? Pd2 Pd1 N1 C9 88.7(3) . . . . ? C20 N5 C26 C27 153.9(4) . . . . ? C19 N5 C26 C27 -80.8(4) . . . . ? Pd2 N5 C26 C27 43.7(4) . . . . ? C10 N3 C18 C17 -9.7(6) . . . . ? Pd1 N3 C18 C17 166.9(3) . . . . ? C10 N3 C18 C19 164.0(4) . . . . ? Pd1 N3 C18 C19 -19.3(6) . . . . ? C31 N6 C27 C28 -0.2(6) . . . . ? Pd2 N6 C27 C28 -171.9(3) . . . . ? C31 N6 C27 C26 -178.1(4) . . . . ? Pd2 N6 C27 C26 10.2(4) . . . . ? N5 C26 C27 N6 -38.7(5) . . . . ? N5 C26 C27 C28 143.4(4) . . . . ? N6 Pd2 N4 C25 174.2(5) . . . . ? C32 Pd2 N4 C25 -21.0(4) . . . . ? N5 Pd2 N4 C25 161.1(4) . . . . ? Pd1 Pd2 N4 C25 70.1(4) . . . . ? N6 Pd2 N4 C21 0.0(8) . . . . ? C32 Pd2 N4 C21 164.8(3) . . . . ? N5 Pd2 N4 C21 -13.0(3) . . . . ? Pd1 Pd2 N4 C21 -104.1(3) . . . . ? N3 C18 C19 N5 -75.0(5) . . . . ? C17 C18 C19 N5 98.8(5) . . . . ? C26 N5 C19 C18 172.3(4) . . . . ? C20 N5 C19 C18 -61.6(5) . . . . ? Pd2 N5 C19 C18 57.6(4) . . . . ? C11 N2 C8 C7 -28.2(8) . . . . ? Pd1 N2 C8 C7 175.2(4) . . . . ? C11 N2 C8 C9 155.1(4) . . . . ? Pd1 N2 C8 C9 -1.5(5) . . . . ? N6 C27 C28 C29 0.2(6) . . . . ? C26 C27 C28 C29 178.0(4) . . . . ? C27 N6 C31 C30 0.3(6) . . . . ? Pd2 N6 C31 C30 170.3(3) . . . . ? C27 C28 C29 C30 -0.4(6) . . . . ? C14 C15 C16 C17 176.1(5) . . . . ? C10 C15 C16 C17 -3.0(7) . . . . ? C8 N2 C11 C12 3.4(8) . . . . ? Pd1 N2 C11 C12 160.3(4) . . . . ? C8 N2 C11 C10 -175.7(4) . . . . ? Pd1 N2 C11 C10 -18.8(5) . . . . ? C15 C16 C17 C18 2.4(7) . . . . ? N3 C18 C17 C16 4.1(7) . . . . ? C19 C18 C17 C16 -169.5(4) . . . . ? C25 N4 C21 C22 -0.7(7) . . . . ? Pd2 N4 C21 C22 174.1(4) . . . . ? C25 N4 C21 C20 178.8(4) . . . . ? Pd2 N4 C21 C20 -6.4(5) . . . . ? C18 N3 C10 C15 9.0(6) . . . . ? Pd1 N3 C10 C15 -168.3(3) . . . . ? C18 N3 C10 C11 -169.2(4) . . . . ? Pd1 N3 C10 C11 13.4(5) . . . . ? C16 C15 C10 N3 -2.6(6) . . . . ? C14 C15 C10 N3 178.2(4) . . . . ? C16 C15 C10 C11 175.6(4) . . . . ? C14 C15 C10 C11 -3.6(7) . . . . ? N2 C11 C10 N3 2.8(6) . . . . ? C12 C11 C10 N3 -176.4(4) . . . . ? N2 C11 C10 C15 -175.4(4) . . . . ? C12 C11 C10 C15 5.4(6) . . . . ? C26 N5 C20 C21 -147.7(4) . . . . ? C19 N5 C20 C21 88.8(4) . . . . ? Pd2 N5 C20 C21 -38.4(4) . . . . ? N4 C21 C20 N5 32.2(6) . . . . ? C22 C21 C20 N5 -148.3(4) . . . . ? C9 N1 C1 C2 1.3(6) . . . . ? Pd1 N1 C1 C2 179.9(3) . . . . ? N6 C31 C30 C29 -0.5(7) . . . . ? C28 C29 C30 C31 0.5(7) . . . . ? N2 C11 C12 C13 178.4(5) . . . . ? C10 C11 C12 C13 -2.6(7) . . . . ? C1 N1 C9 C4 -1.1(6) . . . . ? Pd1 N1 C9 C4 -180.0(3) . . . . ? C1 N1 C9 C8 -179.7(4) . . . . ? Pd1 N1 C9 C8 1.4(5) . . . . ? N2 C8 C9 N1 0.0(6) . . . . ? C7 C8 C9 N1 -177.1(4) . . . . ? N2 C8 C9 C4 -178.6(4) . . . . ? C7 C8 C9 C4 4.3(7) . . . . ? N2 C8 C7 C6 179.0(5) . . . . ? C9 C8 C7 C6 -4.4(7) . . . . ? C5 C6 C7 C8 1.4(8) . . . . ? C21 N4 C25 C24 -0.2(7) . . . . ? Pd2 N4 C25 C24 -174.1(4) . . . . ? C11 C12 C13 C14 -2.1(8) . . . . ? C12 C13 C14 C15 4.0(8) . . . . ? C16 C15 C14 C13 179.8(5) . . . . ? C10 C15 C14 C13 -1.1(7) . . . . ? N1 C9 C4 C3 0.5(7) . . . . ? C8 C9 C4 C3 179.0(4) . . . . ? N1 C9 C4 C5 -179.7(4) . . . . ? C8 C9 C4 C5 -1.2(7) . . . . ? C7 C6 C5 C4 1.9(8) . . . . ? C3 C4 C5 C6 177.8(5) . . . . ? C9 C4 C5 C6 -2.0(7) . . . . ? C24 C23 C22 C21 -0.3(8) . . . . ? N4 C21 C22 C23 0.9(8) . . . . ? C20 C21 C22 C23 -178.5(5) . . . . ? N1 C1 C2 C3 -0.9(7) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C9 C4 C3 C2 -0.1(7) . . . . ? C5 C4 C3 C2 -179.9(5) . . . . ? C22 C23 C24 C25 -0.6(9) . . . . ? N4 C25 C24 C23 0.9(9) . . . . ? C101 S2 C100 S1 -22.1(6) . . . . ? C101 S2 C100 S3 -65.4(7) . . . . ? C101 S1 C100 S2 25.0(6) . . . . ? C101 S1 C100 S3 77.1(9) . . . . ? C101 S3 C100 S2 51.7(6) . . . . ? C101 S3 C100 S1 -48.5(6) . . . . ? C100 S1 C101 S2 -21.6(5) . . . . ? C100 S1 C101 S3 -67.9(7) . . . . ? C100 S2 C101 S1 25.8(7) . . . . ? C100 S2 C101 S3 68.2(7) . . . . ? C100 S3 C101 S1 59.3(6) . . . . ? C100 S3 C101 S2 -46.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.689 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.121 #===END data_15 _database_code_depnum_ccdc_archive 'CCDC 766175' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H30 Cl3 F6 N6 P Pd Pt' _chemical_formula_weight 1063.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3949(4) _cell_length_b 15.6616(8) _cell_length_c 15.8870(9) _cell_angle_alpha 70.729(2) _cell_angle_beta 81.541(2) _cell_angle_gamma 86.647(2) _cell_volume 1717.88(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9426 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 68.39 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 14.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1180 _exptl_absorpt_correction_T_max 0.5866 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus 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_reflns_number 33056 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 68.97 _reflns_number_total 6077 _reflns_number_gt 6030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0262P)^2^+3.6624P] 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 6077 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.002 _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 Pt1 Pt 0.713565(17) 0.732257(8) 0.250216(8) 0.01203(5) Uani 1 1 d . . . Pd1 Pd 0.28407(3) 0.709858(13) 0.297328(14) 0.01006(6) Uani 1 1 d . . . P1 P -0.04779(13) 1.28296(5) 0.28095(6) 0.01854(18) Uani 1 1 d . . . Cl1 Cl 0.27140(10) 0.62870(5) 0.45082(5) 0.01471(15) Uani 1 1 d . . . Cl3 Cl -0.46850(16) 1.09487(7) 0.18793(8) 0.0415(2) Uani 1 1 d . . . Cl2 Cl -0.4987(2) 1.03568(7) 0.38343(8) 0.0498(3) Uani 1 1 d . . . F6 F -0.0979(3) 1.36547(13) 0.19446(14) 0.0255(5) Uani 1 1 d . . . F5 F 0.0030(4) 1.20110(14) 0.36572(15) 0.0331(5) Uani 1 1 d . . . F4 F -0.0152(4) 1.35363(15) 0.32980(17) 0.0403(6) Uani 1 1 d . . . F3 F -0.0809(4) 1.21336(15) 0.23048(18) 0.0427(7) Uani 1 1 d . . . N3 N 0.3858(3) 0.61482(17) 0.23877(18) 0.0113(5) Uani 1 1 d . . . F2 F 0.1628(3) 1.29082(18) 0.23733(18) 0.0423(6) Uani 1 1 d . . . N4 N 0.7526(4) 0.70384(18) 0.13437(18) 0.0131(5) Uani 1 1 d . . . N5 N 0.7540(4) 0.59026(17) 0.31005(18) 0.0128(5) Uani 1 1 d . . . N1 N 0.1651(4) 0.82024(18) 0.32056(19) 0.0144(5) Uani 1 1 d . . . F1 F -0.2580(4) 1.27699(19) 0.32308(19) 0.0454(7) Uani 1 1 d . . . N6 N 0.6959(4) 0.73105(18) 0.37734(18) 0.0142(5) Uani 1 1 d . . . N2 N 0.2561(4) 0.77925(18) 0.17253(18) 0.0144(5) Uani 1 1 d . . . C18 C 0.4801(4) 0.5381(2) 0.2696(2) 0.0138(6) Uani 1 1 d . . . C10 C 0.3317(4) 0.6374(2) 0.1543(2) 0.0129(6) Uani 1 1 d . . . C32 C 0.6936(4) 0.87097(19) 0.1902(2) 0.0136(6) Uani 1 1 d . . . H32A H 0.5711 0.8868 0.1728 0.020 Uiso 1 1 calc R . . H32B H 0.7852 0.8905 0.1365 0.020 Uiso 1 1 calc R . . H32C H 0.7150 0.9013 0.2328 0.020 Uiso 1 1 calc R . . C26 C 0.8502(5) 0.5867(2) 0.3881(2) 0.0164(7) Uani 1 1 d . . . H26A H 0.9806 0.6020 0.3666 0.020 Uiso 1 1 calc R . . H26B H 0.8438 0.5247 0.4321 0.020 Uiso 1 1 calc R . . C25 C 0.7078(5) 0.7545(2) 0.0534(2) 0.0180(7) Uani 1 1 d . . . H25 H 0.6557 0.8129 0.0467 0.022 Uiso 1 1 calc R . . C7 C 0.1916(5) 0.9379(2) 0.0786(2) 0.0182(7) Uani 1 1 d . . . H7 H 0.2337 0.9278 0.0232 0.022 Uiso 1 1 calc R . . C15 C 0.3496(4) 0.5752(2) 0.1054(2) 0.0165(7) Uani 1 1 d . . . C4 C 0.0747(5) 0.9742(2) 0.2404(3) 0.0191(7) Uani 1 1 d . . . C31 C 0.6168(5) 0.7939(2) 0.4126(3) 0.0204(7) Uani 1 1 d . . . H31 H 0.5683 0.8477 0.3740 0.025 Uiso 1 1 calc R . . C28 C 0.7543(5) 0.6382(2) 0.5239(2) 0.0221(7) Uani 1 1 d . . . H28 H 0.8023 0.5838 0.5616 0.027 Uiso 1 1 calc R . . C27 C 0.7615(4) 0.6530(2) 0.4331(2) 0.0158(6) Uani 1 1 d . . . C17 C 0.4912(5) 0.4715(2) 0.2270(2) 0.0172(7) Uani 1 1 d . . . H17 H 0.5484 0.4149 0.2530 0.021 Uiso 1 1 calc R . . C12 C 0.2204(5) 0.7533(2) 0.0288(2) 0.0191(7) Uani 1 1 d . . . H12 H 0.1772 0.8129 0.0012 0.023 Uiso 1 1 calc R . . C14 C 0.2993(5) 0.6039(3) 0.0175(2) 0.0213(7) Uani 1 1 d . . . H14 H 0.3072 0.5630 -0.0158 0.026 Uiso 1 1 calc R . . C9 C 0.1446(4) 0.8887(2) 0.2404(2) 0.0151(6) Uani 1 1 d . . . C11 C 0.2646(4) 0.7285(2) 0.1162(2) 0.0143(6) Uani 1 1 d . . . C20 C 0.8766(4) 0.5667(2) 0.2367(2) 0.0155(6) Uani 1 1 d . . . H20A H 0.8694 0.5010 0.2471 0.019 Uiso 1 1 calc R . . H20B H 1.0047 0.5806 0.2383 0.019 Uiso 1 1 calc R . . C6 C 0.1230(5) 1.0239(2) 0.0784(2) 0.0209(7) Uani 1 1 d . . . H6 H 0.1192 1.0705 0.0223 0.025 Uiso 1 1 calc R . . C21 C 0.8224(4) 0.6192(2) 0.1447(2) 0.0146(6) Uani 1 1 d . . . C8 C 0.1978(4) 0.8682(2) 0.1588(2) 0.0153(6) Uani 1 1 d . . . C22 C 0.8484(5) 0.5849(2) 0.0745(2) 0.0197(7) Uani 1 1 d . . . H22 H 0.8941 0.5250 0.0835 0.024 Uiso 1 1 calc R . . C19 C 0.5899(4) 0.52881(19) 0.3444(2) 0.0129(6) Uani 1 1 d . . . H19A H 0.6314 0.4653 0.3690 0.015 Uiso 1 1 calc R . . H19B H 0.5127 0.5449 0.3935 0.015 Uiso 1 1 calc R . . C5 C 0.0619(5) 1.0425(2) 0.1561(3) 0.0211(7) Uani 1 1 d . . . H5 H 0.0116 1.1003 0.1538 0.025 Uiso 1 1 calc R . . C16 C 0.4199(5) 0.4883(2) 0.1488(2) 0.0188(7) Uani 1 1 d . . . H16 H 0.4174 0.4415 0.1232 0.023 Uiso 1 1 calc R . . C29 C 0.6761(5) 0.7037(3) 0.5596(3) 0.0270(8) Uani 1 1 d . . . H29 H 0.6718 0.6950 0.6220 0.032 Uiso 1 1 calc R . . C1 C 0.1131(5) 0.8346(2) 0.3981(2) 0.0187(7) Uani 1 1 d . . . H1 H 0.1274 0.7873 0.4526 0.022 Uiso 1 1 calc R . . C24 C 0.7350(5) 0.7245(2) -0.0202(2) 0.0209(7) Uani 1 1 d . . . H24 H 0.7047 0.7621 -0.0769 0.025 Uiso 1 1 calc R . . C30 C 0.6047(5) 0.7817(3) 0.5035(3) 0.0257(8) Uani 1 1 d . . . H30 H 0.5478 0.8265 0.5271 0.031 Uiso 1 1 calc R . . C13 C 0.2389(5) 0.6912(3) -0.0193(2) 0.0207(7) Uani 1 1 d . . . H13 H 0.2088 0.7103 -0.0789 0.025 Uiso 1 1 calc R . . C23 C 0.8073(5) 0.6383(2) -0.0097(3) 0.0218(7) Uani 1 1 d . . . H23 H 0.8284 0.6162 -0.0592 0.026 Uiso 1 1 calc R . . C3 C 0.0183(5) 0.9873(2) 0.3242(3) 0.0233(8) Uani 1 1 d . . . H3 H -0.0322 1.0438 0.3264 0.028 Uiso 1 1 calc R . . C2 C 0.0370(5) 0.9178(2) 0.4024(3) 0.0241(8) Uani 1 1 d . . . H2 H -0.0012 0.9259 0.4590 0.029 Uiso 1 1 calc R . . C33 C -0.5331(7) 1.1262(3) 0.2851(3) 0.0398(11) Uani 1 1 d . . . H33A H -0.6636 1.1445 0.2884 0.048 Uiso 1 1 calc R . . H33B H -0.4601 1.1787 0.2813 0.048 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 Pt1 0.01428(8) 0.00701(7) 0.01389(9) -0.00173(5) -0.00234(5) -0.00163(5) Pd1 0.01324(12) 0.00742(11) 0.00912(12) -0.00194(8) -0.00221(9) 0.00022(8) P1 0.0291(5) 0.0115(4) 0.0157(4) -0.0049(3) -0.0062(4) 0.0050(3) Cl1 0.0190(4) 0.0127(3) 0.0107(4) -0.0013(3) -0.0028(3) 0.0002(3) Cl3 0.0468(6) 0.0363(5) 0.0398(6) -0.0100(4) -0.0091(5) 0.0056(4) Cl2 0.0842(9) 0.0269(5) 0.0388(6) -0.0102(4) -0.0146(6) 0.0087(5) F6 0.0410(13) 0.0164(10) 0.0188(11) -0.0046(8) -0.0103(9) 0.0099(9) F5 0.0542(15) 0.0191(10) 0.0235(12) -0.0014(9) -0.0138(11) 0.0080(10) F4 0.0750(19) 0.0217(11) 0.0340(14) -0.0158(10) -0.0283(13) 0.0126(11) F3 0.080(2) 0.0172(11) 0.0414(15) -0.0159(10) -0.0323(14) 0.0126(11) N3 0.0114(12) 0.0102(12) 0.0126(14) -0.0040(10) 0.0002(10) -0.0037(10) F2 0.0321(13) 0.0462(15) 0.0381(15) -0.0023(12) -0.0020(11) 0.0095(11) N4 0.0156(13) 0.0120(12) 0.0103(14) -0.0028(10) 0.0015(10) -0.0031(10) N5 0.0140(13) 0.0083(12) 0.0134(14) 0.0005(10) -0.0027(11) -0.0006(10) N1 0.0168(13) 0.0110(12) 0.0151(14) -0.0033(10) -0.0025(11) -0.0016(10) F1 0.0349(14) 0.0473(15) 0.0417(16) -0.0023(12) 0.0025(12) 0.0039(12) N6 0.0188(14) 0.0132(12) 0.0127(14) -0.0062(11) -0.0029(11) -0.0034(10) N2 0.0182(14) 0.0102(12) 0.0129(14) -0.0009(10) -0.0037(11) 0.0016(10) C18 0.0133(15) 0.0123(14) 0.0134(17) -0.0026(12) 0.0027(12) -0.0020(12) C10 0.0119(15) 0.0162(15) 0.0120(17) -0.0070(13) 0.0007(12) -0.0031(12) C32 0.0176(16) 0.0044(13) 0.0179(17) -0.0017(12) -0.0034(13) -0.0015(11) C26 0.0178(16) 0.0140(15) 0.0160(17) -0.0008(12) -0.0075(13) -0.0006(12) C25 0.0184(17) 0.0155(15) 0.0167(18) -0.0011(13) -0.0005(13) -0.0038(12) C7 0.0182(17) 0.0173(16) 0.0187(18) -0.0037(13) -0.0054(14) -0.0013(13) C15 0.0137(15) 0.0208(16) 0.0175(18) -0.0107(14) 0.0010(13) -0.0033(13) C4 0.0173(16) 0.0126(15) 0.028(2) -0.0057(14) -0.0056(14) -0.0016(12) C31 0.0218(17) 0.0180(16) 0.025(2) -0.0113(14) -0.0015(14) -0.0034(13) C28 0.0207(17) 0.0241(18) 0.0202(19) -0.0038(14) -0.0036(14) -0.0071(14) C27 0.0144(15) 0.0169(15) 0.0140(17) -0.0012(13) -0.0024(13) -0.0073(12) C17 0.0166(16) 0.0111(14) 0.0238(19) -0.0068(13) 0.0018(13) -0.0031(12) C12 0.0187(17) 0.0202(16) 0.0161(18) -0.0023(13) -0.0041(14) -0.0002(13) C14 0.0202(17) 0.0289(18) 0.0198(19) -0.0150(15) -0.0003(14) -0.0045(14) C9 0.0130(15) 0.0116(14) 0.0205(18) -0.0046(13) -0.0032(13) -0.0009(12) C11 0.0119(15) 0.0162(15) 0.0154(17) -0.0064(13) 0.0001(12) -0.0020(12) C20 0.0150(15) 0.0127(15) 0.0170(18) -0.0029(13) -0.0012(13) 0.0007(12) C6 0.0216(17) 0.0130(15) 0.0233(19) 0.0030(13) -0.0082(14) -0.0024(13) C21 0.0127(15) 0.0127(15) 0.0171(18) -0.0039(13) 0.0000(12) -0.0012(12) C8 0.0131(15) 0.0121(15) 0.0196(18) -0.0029(13) -0.0034(13) -0.0024(12) C22 0.0190(17) 0.0159(16) 0.0229(19) -0.0062(14) 0.0025(14) -0.0045(13) C19 0.0140(15) 0.0061(13) 0.0148(17) 0.0012(11) 0.0000(12) -0.0033(11) C5 0.0215(17) 0.0095(15) 0.031(2) -0.0035(14) -0.0067(15) 0.0011(12) C16 0.0182(16) 0.0187(16) 0.0230(19) -0.0131(14) 0.0023(14) -0.0037(13) C29 0.029(2) 0.035(2) 0.018(2) -0.0102(16) -0.0021(15) -0.0116(16) C1 0.0264(18) 0.0158(16) 0.0138(17) -0.0056(13) -0.0007(14) 0.0001(13) C24 0.0204(17) 0.0219(17) 0.0175(19) -0.0012(14) -0.0034(14) -0.0061(14) C30 0.032(2) 0.0243(18) 0.025(2) -0.0147(16) -0.0010(16) -0.0060(15) C13 0.0189(17) 0.0314(19) 0.0127(18) -0.0078(14) -0.0020(13) -0.0054(14) C23 0.0226(18) 0.0239(18) 0.0207(19) -0.0107(14) 0.0020(14) -0.0061(14) C3 0.0255(18) 0.0148(16) 0.031(2) -0.0102(15) -0.0033(15) 0.0032(13) C2 0.031(2) 0.0197(17) 0.024(2) -0.0117(15) -0.0004(15) 0.0007(15) C33 0.051(3) 0.0197(19) 0.047(3) -0.0085(18) -0.010(2) 0.0088(18) _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 Pt1 N6 1.998(3) . ? Pt1 N4 2.009(3) . ? Pt1 C32 2.071(3) . ? Pt1 N5 2.133(3) . ? Pt1 Pd1 3.1668(3) . ? Pd1 N2 1.956(3) . ? Pd1 N1 2.012(3) . ? Pd1 N3 2.055(3) . ? Pd1 Cl1 2.3392(8) . ? P1 F4 1.593(2) . ? P1 F1 1.594(3) . ? P1 F5 1.597(2) . ? P1 F3 1.599(2) . ? P1 F2 1.603(3) . ? P1 F6 1.618(2) . ? Cl3 C33 1.763(5) . ? Cl2 C33 1.768(5) . ? N3 C18 1.336(4) . ? N3 C10 1.383(4) . ? N4 C25 1.347(4) . ? N4 C21 1.361(4) . ? N5 C20 1.500(4) . ? N5 C26 1.502(4) . ? N5 C19 1.514(4) . ? N1 C1 1.323(4) . ? N1 C9 1.390(4) . ? N6 C31 1.351(4) . ? N6 C27 1.362(4) . ? N2 C11 1.373(4) . ? N2 C8 1.389(4) . ? C18 C17 1.410(5) . ? C18 C19 1.500(4) . ? C10 C15 1.424(4) . ? C10 C11 1.444(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C26 C27 1.514(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C25 C24 1.383(5) . ? C25 H25 0.9500 . ? C7 C8 1.383(5) . ? C7 C6 1.411(5) . ? C7 H7 0.9500 . ? C15 C16 1.414(5) . ? C15 C14 1.417(5) . ? C4 C9 1.406(5) . ? C4 C3 1.413(5) . ? C4 C5 1.424(5) . ? C31 C30 1.382(5) . ? C31 H31 0.9500 . ? C28 C27 1.377(5) . ? C28 C29 1.388(6) . ? C28 H28 0.9500 . ? C17 C16 1.362(5) . ? C17 H17 0.9500 . ? C12 C11 1.396(5) . ? C12 C13 1.410(5) . ? C12 H12 0.9500 . ? C14 C13 1.375(5) . ? C14 H14 0.9500 . ? C9 C8 1.431(5) . ? C20 C21 1.522(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C6 C5 1.368(5) . ? C6 H6 0.9500 . ? C21 C22 1.374(5) . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C5 H5 0.9500 . ? C16 H16 0.9500 . ? C29 C30 1.383(6) . ? C29 H29 0.9500 . ? C1 C2 1.408(5) . ? C1 H1 0.9500 . ? C24 C23 1.389(5) . ? C24 H24 0.9500 . ? C30 H30 0.9500 . ? C13 H13 0.9500 . ? C23 H23 0.9500 . ? C3 C2 1.374(5) . ? C3 H3 0.9500 . ? C2 H2 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 N6 Pt1 N4 166.64(11) . . ? N6 Pt1 C32 97.45(12) . . ? N4 Pt1 C32 95.42(12) . . ? N6 Pt1 N5 82.97(11) . . ? N4 Pt1 N5 83.95(11) . . ? C32 Pt1 N5 176.07(11) . . ? N6 Pt1 Pd1 83.27(8) . . ? N4 Pt1 Pd1 99.66(8) . . ? C32 Pt1 Pd1 92.89(9) . . ? N5 Pt1 Pd1 91.03(7) . . ? N2 Pd1 N1 82.71(11) . . ? N2 Pd1 N3 81.62(11) . . ? N1 Pd1 N3 164.12(11) . . ? N2 Pd1 Cl1 171.68(9) . . ? N1 Pd1 Cl1 92.97(8) . . ? N3 Pd1 Cl1 102.25(8) . . ? N2 Pd1 Pt1 89.96(8) . . ? N1 Pd1 Pt1 110.94(8) . . ? N3 Pd1 Pt1 71.68(7) . . ? Cl1 Pd1 Pt1 98.23(2) . . ? F4 P1 F1 89.87(17) . . ? F4 P1 F5 90.51(13) . . ? F1 P1 F5 90.99(15) . . ? F4 P1 F3 179.08(14) . . ? F1 P1 F3 90.24(17) . . ? F5 P1 F3 90.40(12) . . ? F4 P1 F2 89.82(16) . . ? F1 P1 F2 178.92(16) . . ? F5 P1 F2 90.05(14) . . ? F3 P1 F2 90.05(17) . . ? F4 P1 F6 89.85(12) . . ? F1 P1 F6 89.44(14) . . ? F5 P1 F6 179.44(14) . . ? F3 P1 F6 89.24(12) . . ? F2 P1 F6 89.53(13) . . ? C18 N3 C10 119.0(3) . . ? C18 N3 Pd1 131.9(2) . . ? C10 N3 Pd1 109.0(2) . . ? C25 N4 C21 118.8(3) . . ? C25 N4 Pt1 128.4(2) . . ? C21 N4 Pt1 112.6(2) . . ? C20 N5 C26 113.1(3) . . ? C20 N5 C19 111.2(2) . . ? C26 N5 C19 108.9(2) . . ? C20 N5 Pt1 102.19(18) . . ? C26 N5 Pt1 101.68(18) . . ? C19 N5 Pt1 119.49(19) . . ? C1 N1 C9 119.7(3) . . ? C1 N1 Pd1 129.2(2) . . ? C9 N1 Pd1 111.1(2) . . ? C31 N6 C27 119.1(3) . . ? C31 N6 Pt1 127.7(2) . . ? C27 N6 Pt1 113.0(2) . . ? C11 N2 C8 129.5(3) . . ? C11 N2 Pd1 114.6(2) . . ? C8 N2 Pd1 114.6(2) . . ? N3 C18 C17 120.9(3) . . ? N3 C18 C19 118.1(3) . . ? C17 C18 C19 120.7(3) . . ? N3 C10 C15 121.6(3) . . ? N3 C10 C11 116.9(3) . . ? C15 C10 C11 121.4(3) . . ? Pt1 C32 H32A 109.5 . . ? Pt1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Pt1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C26 C27 109.9(3) . . ? N5 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N5 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N4 C25 C24 122.3(3) . . ? N4 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C16 C15 C14 124.6(3) . . ? C16 C15 C10 116.5(3) . . ? C14 C15 C10 118.8(3) . . ? C9 C4 C3 118.2(3) . . ? C9 C4 C5 118.4(3) . . ? C3 C4 C5 123.4(3) . . ? N6 C31 C30 121.5(3) . . ? N6 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C27 C28 C29 119.3(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? N6 C27 C28 121.4(3) . . ? N6 C27 C26 115.8(3) . . ? C28 C27 C26 122.7(3) . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C11 C12 C13 121.1(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N1 C9 C4 120.9(3) . . ? N1 C9 C8 117.1(3) . . ? C4 C9 C8 122.1(3) . . ? N2 C11 C12 129.2(3) . . ? N2 C11 C10 113.7(3) . . ? C12 C11 C10 117.1(3) . . ? N5 C20 C21 111.2(3) . . ? N5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C5 C6 C7 122.3(3) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? N4 C21 C22 121.5(3) . . ? N4 C21 C20 116.3(3) . . ? C22 C21 C20 122.2(3) . . ? C7 C8 N2 128.8(3) . . ? C7 C8 C9 117.4(3) . . ? N2 C8 C9 113.7(3) . . ? C21 C22 C23 119.6(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C18 C19 N5 110.1(3) . . ? C18 C19 H19A 109.6 . . ? N5 C19 H19A 109.6 . . ? C18 C19 H19B 109.6 . . ? N5 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C6 C5 C4 119.2(3) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C30 C29 C28 119.2(4) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? N1 C1 C2 121.9(3) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C25 C24 C23 118.8(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C14 C13 C12 122.0(3) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C24 C23 C22 119.0(3) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? Cl3 C33 Cl2 111.1(2) . . ? Cl3 C33 H33A 109.4 . . ? Cl2 C33 H33A 109.4 . . ? Cl3 C33 H33B 109.4 . . ? Cl2 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? 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 N6 Pt1 Pd1 N2 147.99(11) . . . . ? N4 Pt1 Pd1 N2 -45.18(11) . . . . ? C32 Pt1 Pd1 N2 50.82(12) . . . . ? N5 Pt1 Pd1 N2 -129.22(11) . . . . ? N6 Pt1 Pd1 N1 65.81(12) . . . . ? N4 Pt1 Pd1 N1 -127.36(12) . . . . ? C32 Pt1 Pd1 N1 -31.36(12) . . . . ? N5 Pt1 Pd1 N1 148.60(11) . . . . ? N6 Pt1 Pd1 N3 -130.83(11) . . . . ? N4 Pt1 Pd1 N3 36.00(11) . . . . ? C32 Pt1 Pd1 N3 132.00(12) . . . . ? N5 Pt1 Pd1 N3 -48.04(11) . . . . ? N6 Pt1 Pd1 Cl1 -30.59(8) . . . . ? N4 Pt1 Pd1 Cl1 136.25(8) . . . . ? C32 Pt1 Pd1 Cl1 -127.76(9) . . . . ? N5 Pt1 Pd1 Cl1 52.21(8) . . . . ? N2 Pd1 N3 C18 166.5(3) . . . . ? N1 Pd1 N3 C18 176.0(3) . . . . ? Cl1 Pd1 N3 C18 -21.0(3) . . . . ? Pt1 Pd1 N3 C18 73.8(3) . . . . ? N2 Pd1 N3 C10 -17.5(2) . . . . ? N1 Pd1 N3 C10 -8.0(5) . . . . ? Cl1 Pd1 N3 C10 155.03(18) . . . . ? Pt1 Pd1 N3 C10 -110.2(2) . . . . ? N6 Pt1 N4 C25 173.5(4) . . . . ? C32 Pt1 N4 C25 -22.0(3) . . . . ? N5 Pt1 N4 C25 161.9(3) . . . . ? Pd1 Pt1 N4 C25 71.9(3) . . . . ? N6 Pt1 N4 C21 -1.7(6) . . . . ? C32 Pt1 N4 C21 162.8(2) . . . . ? N5 Pt1 N4 C21 -13.3(2) . . . . ? Pd1 Pt1 N4 C21 -103.3(2) . . . . ? N6 Pt1 N5 C20 -148.8(2) . . . . ? N4 Pt1 N5 C20 28.53(19) . . . . ? C32 Pt1 N5 C20 -52.4(17) . . . . ? Pd1 Pt1 N5 C20 128.13(18) . . . . ? N6 Pt1 N5 C26 -31.8(2) . . . . ? N4 Pt1 N5 C26 145.5(2) . . . . ? C32 Pt1 N5 C26 64.6(17) . . . . ? Pd1 Pt1 N5 C26 -114.85(18) . . . . ? N6 Pt1 N5 C19 88.0(2) . . . . ? N4 Pt1 N5 C19 -94.7(2) . . . . ? C32 Pt1 N5 C19 -175.6(16) . . . . ? Pd1 Pt1 N5 C19 4.9(2) . . . . ? N2 Pd1 N1 C1 175.6(3) . . . . ? N3 Pd1 N1 C1 166.2(3) . . . . ? Cl1 Pd1 N1 C1 2.8(3) . . . . ? Pt1 Pd1 N1 C1 -97.2(3) . . . . ? N2 Pd1 N1 C9 -6.5(2) . . . . ? N3 Pd1 N1 C9 -15.9(5) . . . . ? Cl1 Pd1 N1 C9 -179.3(2) . . . . ? Pt1 Pd1 N1 C9 80.7(2) . . . . ? N4 Pt1 N6 C31 -170.6(4) . . . . ? C32 Pt1 N6 C31 24.9(3) . . . . ? N5 Pt1 N6 C31 -159.0(3) . . . . ? Pd1 Pt1 N6 C31 -67.1(3) . . . . ? N4 Pt1 N6 C27 4.1(6) . . . . ? C32 Pt1 N6 C27 -160.4(2) . . . . ? N5 Pt1 N6 C27 15.7(2) . . . . ? Pd1 Pt1 N6 C27 107.6(2) . . . . ? N1 Pd1 N2 C11 -160.5(2) . . . . ? N3 Pd1 N2 C11 16.9(2) . . . . ? Cl1 Pd1 N2 C11 -101.4(6) . . . . ? Pt1 Pd1 N2 C11 88.4(2) . . . . ? N1 Pd1 N2 C8 8.2(2) . . . . ? N3 Pd1 N2 C8 -174.4(2) . . . . ? Cl1 Pd1 N2 C8 67.3(7) . . . . ? Pt1 Pd1 N2 C8 -102.9(2) . . . . ? C10 N3 C18 C17 -13.7(4) . . . . ? Pd1 N3 C18 C17 162.0(2) . . . . ? C10 N3 C18 C19 160.0(3) . . . . ? Pd1 N3 C18 C19 -24.3(4) . . . . ? C18 N3 C10 C15 9.6(4) . . . . ? Pd1 N3 C10 C15 -167.0(2) . . . . ? C18 N3 C10 C11 -167.5(3) . . . . ? Pd1 N3 C10 C11 15.9(3) . . . . ? C20 N5 C26 C27 151.0(3) . . . . ? C19 N5 C26 C27 -84.9(3) . . . . ? Pt1 N5 C26 C27 42.2(3) . . . . ? C21 N4 C25 C24 -1.8(5) . . . . ? Pt1 N4 C25 C24 -176.8(2) . . . . ? N3 C10 C15 C16 2.0(5) . . . . ? C11 C10 C15 C16 178.9(3) . . . . ? N3 C10 C15 C14 -177.2(3) . . . . ? C11 C10 C15 C14 -0.3(5) . . . . ? C27 N6 C31 C30 1.6(5) . . . . ? Pt1 N6 C31 C30 176.0(3) . . . . ? C31 N6 C27 C28 -2.2(5) . . . . ? Pt1 N6 C27 C28 -177.5(3) . . . . ? C31 N6 C27 C26 -179.3(3) . . . . ? Pt1 N6 C27 C26 5.5(3) . . . . ? C29 C28 C27 N6 1.0(5) . . . . ? C29 C28 C27 C26 177.8(3) . . . . ? N5 C26 C27 N6 -34.6(4) . . . . ? N5 C26 C27 C28 148.4(3) . . . . ? N3 C18 C17 C16 6.2(5) . . . . ? C19 C18 C17 C16 -167.4(3) . . . . ? C16 C15 C14 C13 -177.5(3) . . . . ? C10 C15 C14 C13 1.6(5) . . . . ? C1 N1 C9 C4 2.0(5) . . . . ? Pd1 N1 C9 C4 -176.1(2) . . . . ? C1 N1 C9 C8 -178.0(3) . . . . ? Pd1 N1 C9 C8 3.9(3) . . . . ? C3 C4 C9 N1 -2.7(5) . . . . ? C5 C4 C9 N1 178.1(3) . . . . ? C3 C4 C9 C8 177.3(3) . . . . ? C5 C4 C9 C8 -1.8(5) . . . . ? C8 N2 C11 C12 1.6(6) . . . . ? Pd1 N2 C11 C12 168.2(3) . . . . ? C8 N2 C11 C10 -179.5(3) . . . . ? Pd1 N2 C11 C10 -12.8(4) . . . . ? C13 C12 C11 N2 179.7(3) . . . . ? C13 C12 C11 C10 0.8(5) . . . . ? N3 C10 C11 N2 -2.9(4) . . . . ? C15 C10 C11 N2 180.0(3) . . . . ? N3 C10 C11 C12 176.2(3) . . . . ? C15 C10 C11 C12 -0.9(5) . . . . ? C26 N5 C20 C21 -147.2(3) . . . . ? C19 N5 C20 C21 89.9(3) . . . . ? Pt1 N5 C20 C21 -38.7(3) . . . . ? C8 C7 C6 C5 0.6(5) . . . . ? C25 N4 C21 C22 0.2(5) . . . . ? Pt1 N4 C21 C22 175.9(3) . . . . ? C25 N4 C21 C20 177.9(3) . . . . ? Pt1 N4 C21 C20 -6.4(3) . . . . ? N5 C20 C21 N4 32.8(4) . . . . ? N5 C20 C21 C22 -149.6(3) . . . . ? C6 C7 C8 N2 178.4(3) . . . . ? C6 C7 C8 C9 -4.3(5) . . . . ? C11 N2 C8 C7 -24.2(6) . . . . ? Pd1 N2 C8 C7 169.1(3) . . . . ? C11 N2 C8 C9 158.4(3) . . . . ? Pd1 N2 C8 C9 -8.3(4) . . . . ? N1 C9 C8 C7 -175.0(3) . . . . ? C4 C9 C8 C7 5.0(5) . . . . ? N1 C9 C8 N2 2.7(4) . . . . ? C4 C9 C8 N2 -177.3(3) . . . . ? N4 C21 C22 C23 1.7(5) . . . . ? C20 C21 C22 C23 -175.8(3) . . . . ? N3 C18 C19 N5 -70.9(4) . . . . ? C17 C18 C19 N5 102.8(3) . . . . ? C20 N5 C19 C18 -60.5(3) . . . . ? C26 N5 C19 C18 174.3(3) . . . . ? Pt1 N5 C19 C18 58.2(3) . . . . ? C7 C6 C5 C4 2.7(5) . . . . ? C9 C4 C5 C6 -2.0(5) . . . . ? C3 C4 C5 C6 178.9(3) . . . . ? C18 C17 C16 C15 5.8(5) . . . . ? C14 C15 C16 C17 169.6(3) . . . . ? C10 C15 C16 C17 -9.5(5) . . . . ? C27 C28 C29 C30 1.0(5) . . . . ? C9 N1 C1 C2 -0.1(5) . . . . ? Pd1 N1 C1 C2 177.6(3) . . . . ? N4 C25 C24 C23 1.4(5) . . . . ? N6 C31 C30 C29 0.4(6) . . . . ? C28 C29 C30 C31 -1.6(6) . . . . ? C15 C14 C13 C12 -1.8(5) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C25 C24 C23 C22 0.6(5) . . . . ? C21 C22 C23 C24 -2.1(5) . . . . ? C9 C4 C3 C2 1.5(5) . . . . ? C5 C4 C3 C2 -179.4(3) . . . . ? C4 C3 C2 C1 0.4(6) . . . . ? N1 C1 C2 C3 -1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 68.97 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.746 _refine_diff_density_min -1.572 _refine_diff_density_rms 0.119 #===END data_16 _database_code_depnum_ccdc_archive 'CCDC 766176' #TrackingRef 'Pd_cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H47 B2 Br3 F8 N13 Pd3' _chemical_formula_weight 1586.58 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.8582(13) _cell_length_b 19.3783(19) _cell_length_c 45.245(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11273.8(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.90 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6200 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3314 _exptl_absorpt_correction_T_max 0.5715 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 221928 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 29.13 _reflns_number_total 15158 _reflns_number_gt 12905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0130P)^2^+349.2203P] 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 15158 _refine_ls_number_parameters 780 _refine_ls_number_restraints 790 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1984 _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_restrained_S_all 1.230 _refine_ls_shift/su_max 0.003 _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 Pd3 Pd 0.62312(5) 0.11217(3) 0.290516(14) 0.01688(14) Uani 1 1 d U . . Pd2 Pd 0.64586(5) 0.12790(3) 0.365995(15) 0.01755(14) Uani 1 1 d U . . Pd1 Pd 0.61143(6) 0.16168(3) 0.435549(15) 0.01908(14) Uani 1 1 d U . . Br3 Br 0.77954(7) 0.04202(5) 0.29276(2) 0.0244(2) Uani 1 1 d U . . Br2 Br 0.48176(9) 0.06013(6) 0.36467(2) 0.0320(2) Uani 1 1 d U . . Br1 Br 0.61677(9) 0.28323(5) 0.42424(2) 0.0293(2) Uani 1 1 d U . . N6 N 0.6029(6) 0.2207(4) 0.34507(17) 0.0210(15) Uani 1 1 d U . . N9 N 0.5231(6) 0.0312(4) 0.29268(17) 0.0213(15) Uani 1 1 d U . . N5 N 0.7813(6) 0.1735(4) 0.36372(19) 0.0240(16) Uani 1 1 d U . . N7 N 0.6942(6) 0.2036(4) 0.28331(16) 0.0204(15) Uani 1 1 d U . . N3 N 0.4569(7) 0.1510(4) 0.43019(17) 0.0247(16) Uani 1 1 d U . . N2 N 0.6035(6) 0.0608(4) 0.44872(16) 0.0197(15) Uani 1 1 d U . . N8 N 0.4899(6) 0.1694(4) 0.28762(17) 0.0217(15) Uani 1 1 d U . . C23 C 0.6802(7) 0.2692(5) 0.35104(18) 0.0192(17) Uani 1 1 d U . . N4 N 0.7349(6) 0.0576(4) 0.38997(16) 0.0184(14) Uani 1 1 d U . . N1 N 0.7640(7) 0.1526(4) 0.44535(17) 0.0227(16) Uani 1 1 d U . . C16 C 0.8860(8) -0.0390(5) 0.4073(2) 0.027(2) Uani 1 1 d U . . H16 H 0.9344 -0.0745 0.4117 0.033 Uiso 1 1 calc R . . C14 C 0.7117(7) 0.0075(4) 0.4089(2) 0.0191(17) Uani 1 1 d U . . C21 C 0.8666(8) 0.1295(5) 0.3683(2) 0.0257(19) Uani 1 1 d U . . C28 C 0.6638(8) 0.3411(5) 0.34624(18) 0.0201(17) Uani 1 1 d U . . C34 C 0.6273(7) 0.2525(5) 0.27468(19) 0.0202(17) Uani 1 1 d U . . C15 C 0.7862(8) -0.0434(5) 0.4170(2) 0.0247(19) Uani 1 1 d U . . H15 H 0.7660 -0.0809 0.4293 0.030 Uiso 1 1 calc R . . C22 C 0.8394(7) 0.0672(4) 0.38253(19) 0.0180(16) Uani 1 1 d U . . C7 C 0.4983(8) 0.0563(5) 0.4629(2) 0.0261(19) Uani 1 1 d U . . H7A H 0.4780 0.0073 0.4653 0.031 Uiso 1 1 calc R . . H7B H 0.5002 0.0779 0.4827 0.031 Uiso 1 1 calc R . . C13 C 0.6081(8) 0.0067(4) 0.4246(2) 0.0218(18) Uani 1 1 d U . . H13A H 0.5966 -0.0395 0.4334 0.026 Uiso 1 1 calc R . . H13B H 0.5519 0.0153 0.4102 0.026 Uiso 1 1 calc R . . C37 C 0.6612(8) 0.3199(5) 0.2695(2) 0.0231(18) Uani 1 1 d U . . H37 H 0.6129 0.3538 0.2631 0.028 Uiso 1 1 calc R . . C27 C 0.7463(8) 0.3877(5) 0.3507(2) 0.0239(18) Uani 1 1 d U . . H27 H 0.7375 0.4357 0.3473 0.029 Uiso 1 1 calc R . . C24 C 0.7793(7) 0.2431(5) 0.35952(19) 0.0194(17) Uani 1 1 d U . . C41 C 0.3443(9) 0.0032(7) 0.2847(2) 0.035(2) Uani 1 1 d U . . H41 H 0.2770 0.0164 0.2782 0.042 Uiso 1 1 calc R . . C26 C 0.8414(9) 0.3613(5) 0.3602(2) 0.026(2) Uani 1 1 d U . . H26 H 0.8963 0.3929 0.3640 0.032 Uiso 1 1 calc R . . C35 C 0.8316(7) 0.2869(5) 0.2836(2) 0.0208(17) Uani 1 1 d U . . H35 H 0.9029 0.2975 0.2868 0.025 Uiso 1 1 calc R . . C18 C 1.0214(8) 0.0327(5) 0.3821(2) 0.028(2) Uani 1 1 d U . . H18 H 1.0746 0.0001 0.3862 0.034 Uiso 1 1 calc R . . C31 C 0.5150(8) 0.2424(5) 0.3322(2) 0.0228(18) Uani 1 1 d U . . C36 C 0.7635(8) 0.3375(5) 0.2736(2) 0.0260(19) Uani 1 1 d U . . H36 H 0.7872 0.3831 0.2698 0.031 Uiso 1 1 calc R . . C1 C 0.8444(8) 0.1924(5) 0.4366(2) 0.027(2) Uani 1 1 d U . . H1 H 0.8299 0.2334 0.4259 0.033 Uiso 1 1 calc R . . C8 C 0.4212(8) 0.0926(5) 0.4439(2) 0.026(2) Uani 1 1 d U . . C33 C 0.5189(7) 0.2295(5) 0.2682(2) 0.0224(18) Uani 1 1 d U . . H33A H 0.5133 0.2159 0.2472 0.027 Uiso 1 1 calc R . . H33B H 0.4700 0.2682 0.2718 0.027 Uiso 1 1 calc R . . C42 C 0.3608(9) -0.0634(6) 0.2949(2) 0.035(2) Uani 1 1 d U . . H42 H 0.3062 -0.0964 0.2952 0.041 Uiso 1 1 calc R . . C39 C 0.4152(9) 0.1223(6) 0.2720(2) 0.032(2) Uani 1 1 d U . . H39A H 0.3432 0.1391 0.2748 0.038 Uiso 1 1 calc R . . H39B H 0.4304 0.1221 0.2505 0.038 Uiso 1 1 calc R . . C25 C 0.8605(9) 0.2913(5) 0.3644(2) 0.030(2) Uani 1 1 d U . . H25 H 0.9273 0.2759 0.3706 0.036 Uiso 1 1 calc R . . C40 C 0.4252(8) 0.0510(6) 0.2841(2) 0.027(2) Uani 1 1 d U . . C17 C 0.9171(8) 0.0190(5) 0.3906(2) 0.0228(18) Uani 1 1 d U . . C29 C 0.5637(9) 0.3620(5) 0.3375(2) 0.028(2) Uani 1 1 d U . . H29 H 0.5461 0.4096 0.3369 0.034 Uiso 1 1 calc R . . C9 C 0.3198(9) 0.0726(6) 0.4404(2) 0.035(2) Uani 1 1 d U . . H9 H 0.2953 0.0324 0.4502 0.042 Uiso 1 1 calc R . . C12 C 0.3925(9) 0.1874(6) 0.4127(2) 0.031(2) Uani 1 1 d U . . H12 H 0.4188 0.2268 0.4027 0.038 Uiso 1 1 calc R . . C32 C 0.4455(7) 0.1909(5) 0.3166(2) 0.0259(19) Uani 1 1 d U . . H32A H 0.4363 0.1498 0.3292 0.031 Uiso 1 1 calc R . . H32B H 0.3762 0.2119 0.3133 0.031 Uiso 1 1 calc R . . C6 C 0.6910(8) 0.0530(5) 0.4702(2) 0.0229(18) Uani 1 1 d U . . H6A H 0.6686 0.0698 0.4899 0.028 Uiso 1 1 calc R . . H6B H 0.7092 0.0036 0.4721 0.028 Uiso 1 1 calc R . . C5 C 0.7844(8) 0.0925(5) 0.4605(2) 0.0227(18) Uani 1 1 d U . . C43 C 0.4612(8) -0.0802(5) 0.3045(2) 0.028(2) Uani 1 1 d U . . H43 H 0.4751 -0.1251 0.3120 0.034 Uiso 1 1 calc R . . C20 C 0.9683(7) 0.1430(5) 0.3604(2) 0.0219(18) Uani 1 1 d U . . H20 H 0.9868 0.1842 0.3503 0.026 Uiso 1 1 calc R . . C19 C 1.0445(9) 0.0925(5) 0.3680(2) 0.028(2) Uani 1 1 d U . . H19 H 1.1150 0.1012 0.3630 0.034 Uiso 1 1 calc R . . C44 C 0.5396(8) -0.0321(5) 0.3034(2) 0.0241(19) Uani 1 1 d U . . H44 H 0.6070 -0.0442 0.3103 0.029 Uiso 1 1 calc R . . C4 C 0.8864(9) 0.0730(6) 0.4664(2) 0.030(2) Uani 1 1 d U . . H4 H 0.9005 0.0312 0.4767 0.036 Uiso 1 1 calc R . . C30 C 0.4916(8) 0.3131(5) 0.3297(2) 0.028(2) Uani 1 1 d U . . H30 H 0.4255 0.3270 0.3225 0.034 Uiso 1 1 calc R . . C2 C 0.9462(8) 0.1762(5) 0.4426(3) 0.032(2) Uani 1 1 d U . . H2 H 1.0010 0.2062 0.4369 0.038 Uiso 1 1 calc R . . C11 C 0.2902(9) 0.1695(7) 0.4089(3) 0.039(3) Uani 1 1 d U . . H11 H 0.2457 0.1971 0.3970 0.046 Uiso 1 1 calc R . . C38 C 0.7948(9) 0.2206(5) 0.2889(2) 0.027(2) Uani 1 1 d U . . H38 H 0.8407 0.1866 0.2965 0.033 Uiso 1 1 calc R . . C10 C 0.2523(9) 0.1103(7) 0.4226(2) 0.037(2) Uani 1 1 d U . . H10 H 0.1822 0.0962 0.4200 0.045 Uiso 1 1 calc R . . C3 C 0.9671(9) 0.1150(6) 0.4573(3) 0.035(2) Uani 1 1 d U . . H3 H 1.0370 0.1018 0.4611 0.042 Uiso 1 1 calc R . . F4 F 0.6111(7) 0.0955(4) 0.53862(18) 0.053(2) Uani 1 1 d U . . F3 F 0.6252(8) 0.2046(4) 0.5547(2) 0.062(2) Uani 1 1 d U . . F7 F 0.2701(6) -0.2190(5) 0.2997(2) 0.075(3) Uani 1 1 d DU B . N100 N 0.9375(8) 0.4193(5) 0.2308(2) 0.038(2) Uani 1 1 d U . . F2 F 0.4716(9) 0.1538(5) 0.5553(3) 0.095(4) Uani 1 1 d U . . C100 C 0.9346(8) 0.4709(6) 0.2195(3) 0.031(2) Uani 1 1 d U . . F1 F 0.5438(10) 0.1859(5) 0.5118(2) 0.084(3) Uani 1 1 d U . . B2 B 0.3366(9) -0.2678(6) 0.3095(3) 0.027(2) Uani 1 1 d U . . C300 C 0.8810(11) 0.0845(9) 0.5437(3) 0.051(3) Uani 1 1 d U . . C200 C 0.2083(13) 0.1416(7) 0.5046(3) 0.049(3) Uani 1 1 d U . . N200 N 0.1707(13) 0.0895(6) 0.5087(3) 0.069(4) Uani 1 1 d U . . B1 B 0.5599(14) 0.1568(7) 0.5390(4) 0.047(3) Uani 1 1 d U . . C201 C 0.2571(14) 0.2078(8) 0.4995(3) 0.061(4) Uani 1 1 d U . . H20A H 0.2337 0.2408 0.5145 0.091 Uiso 1 1 calc R . . H20B H 0.2377 0.2248 0.4798 0.091 Uiso 1 1 calc R . . H20C H 0.3328 0.2028 0.5006 0.091 Uiso 1 1 calc R . . N300 N 0.8870(12) 0.0308(8) 0.5489(4) 0.072(4) Uani 1 1 d U . . C301 C 0.8714(13) 0.1581(9) 0.5353(4) 0.063(4) Uani 1 1 d U . . H30A H 0.7988 0.1685 0.5304 0.094 Uiso 1 1 calc R . . H30B H 0.9153 0.1674 0.5180 0.094 Uiso 1 1 calc R . . H30C H 0.8939 0.1872 0.5518 0.094 Uiso 1 1 calc R . . C101 C 0.9309(12) 0.5370(8) 0.2055(4) 0.062(4) Uani 1 1 d U . . H10A H 0.9997 0.5586 0.2065 0.093 Uiso 1 1 calc R . . H10B H 0.8801 0.5662 0.2157 0.093 Uiso 1 1 calc R . . H10C H 0.9104 0.5314 0.1848 0.093 Uiso 1 1 calc R . . C400 C 0.3510(15) -0.1179(11) 0.3818(5) 0.084(6) Uani 1 1 d U . . C501 C 0.263(2) -0.0909(13) 0.3655(5) 0.047(5) Uani 0.561(19) 1 d PU A 1 N500 N 0.1942(18) -0.0697(13) 0.3507(5) 0.058(6) Uani 0.561(19) 1 d PU A 1 C401 C 0.245(3) -0.132(2) 0.3845(9) 0.062(8) Uani 0.439(19) 1 d PU A 2 N400 N 0.161(3) -0.138(2) 0.3885(9) 0.081(12) Uani 0.439(19) 1 d PU A 2 F100 F 0.360(2) -0.2396(13) 0.3406(4) 0.070(10) Uani 0.324(19) 1 d PDU B 1 F101 F 0.3001(13) -0.3298(7) 0.3151(6) 0.048(8) Uani 0.324(19) 1 d PDU B 1 F102 F 0.4319(11) -0.2669(13) 0.2978(5) 0.060(10) Uani 0.324(19) 1 d PDU B 1 F8 F 0.4383(7) -0.2486(7) 0.3069(3) 0.039(3) Uani 0.676(19) 1 d PDU B 2 F6 F 0.3202(10) -0.3239(6) 0.2900(3) 0.064(4) Uani 0.676(19) 1 d PDU B 2 F5 F 0.3135(9) -0.2885(8) 0.3371(2) 0.058(5) Uani 0.676(19) 1 d PDU B 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 Pd3 0.0155(3) 0.0197(3) 0.0155(3) 0.0011(2) -0.0008(2) -0.0002(2) Pd2 0.0195(3) 0.0168(3) 0.0163(3) 0.0010(2) -0.0001(2) 0.0005(2) Pd1 0.0243(3) 0.0149(3) 0.0181(3) -0.0006(2) 0.0013(3) -0.0015(2) Br3 0.0191(4) 0.0227(4) 0.0315(5) 0.0015(4) 0.0058(4) 0.0044(3) Br2 0.0356(6) 0.0332(5) 0.0271(5) 0.0016(4) -0.0010(4) -0.0036(4) Br1 0.0439(6) 0.0162(4) 0.0277(5) 0.0016(3) 0.0047(4) -0.0011(4) N6 0.019(4) 0.023(4) 0.021(4) 0.001(3) 0.003(3) 0.001(3) N9 0.024(4) 0.022(4) 0.018(4) -0.003(3) -0.001(3) -0.004(3) N5 0.021(4) 0.022(4) 0.029(4) 0.002(3) 0.001(3) -0.004(3) N7 0.026(4) 0.026(4) 0.009(3) -0.004(3) -0.012(3) 0.003(3) N3 0.036(4) 0.023(4) 0.016(4) -0.002(3) 0.007(3) 0.001(3) N2 0.020(4) 0.023(4) 0.016(3) 0.008(3) -0.003(3) -0.006(3) N8 0.016(4) 0.028(4) 0.021(4) 0.009(3) 0.001(3) 0.003(3) C23 0.024(4) 0.025(4) 0.009(3) -0.001(3) -0.001(3) 0.007(3) N4 0.023(4) 0.016(3) 0.016(3) 0.001(3) -0.004(3) 0.003(3) N1 0.031(4) 0.017(3) 0.020(4) -0.004(3) -0.001(3) -0.008(3) C16 0.033(5) 0.018(4) 0.031(5) 0.000(4) -0.011(4) 0.007(4) C14 0.027(4) 0.010(3) 0.021(4) 0.000(3) -0.004(3) 0.001(3) C21 0.026(5) 0.015(4) 0.036(5) -0.005(4) -0.002(4) -0.006(3) C28 0.030(5) 0.018(4) 0.012(4) 0.003(3) 0.005(3) 0.002(3) C34 0.015(4) 0.033(5) 0.013(4) -0.001(3) -0.002(3) 0.001(3) C15 0.034(5) 0.012(4) 0.028(5) 0.003(3) -0.007(4) 0.000(3) C22 0.020(4) 0.018(4) 0.016(4) -0.005(3) -0.005(3) 0.003(3) C7 0.030(5) 0.030(5) 0.019(4) 0.000(4) 0.002(4) -0.005(4) C13 0.031(5) 0.012(4) 0.022(4) 0.002(3) -0.006(4) -0.003(3) C37 0.023(4) 0.027(4) 0.019(4) 0.005(3) 0.001(3) 0.003(4) C27 0.038(5) 0.013(4) 0.020(4) -0.001(3) 0.006(4) -0.003(4) C24 0.016(4) 0.026(4) 0.016(4) 0.006(3) 0.005(3) 0.000(3) C41 0.026(5) 0.055(7) 0.024(5) 0.004(5) -0.002(4) -0.010(5) C26 0.036(5) 0.022(4) 0.020(4) 0.001(3) 0.005(4) -0.008(4) C35 0.015(4) 0.026(4) 0.021(4) -0.008(3) 0.000(3) -0.002(3) C18 0.023(5) 0.031(5) 0.031(5) -0.001(4) -0.006(4) 0.008(4) C31 0.025(5) 0.025(4) 0.019(4) 0.007(3) 0.007(3) 0.005(4) C36 0.033(5) 0.023(4) 0.022(4) -0.001(4) 0.006(4) -0.003(4) C1 0.031(5) 0.022(4) 0.029(5) -0.011(4) 0.002(4) -0.008(4) C8 0.029(5) 0.020(4) 0.029(5) -0.007(4) -0.004(4) -0.004(4) C33 0.018(4) 0.026(4) 0.023(4) 0.013(4) -0.005(3) -0.005(3) C42 0.034(6) 0.039(6) 0.031(5) -0.003(4) 0.008(4) -0.020(5) C39 0.030(5) 0.035(5) 0.030(5) 0.015(4) -0.010(4) -0.004(4) C25 0.033(5) 0.027(5) 0.030(5) 0.003(4) 0.004(4) -0.003(4) C40 0.026(5) 0.037(5) 0.018(4) 0.009(4) 0.002(4) -0.003(4) C17 0.024(4) 0.021(4) 0.024(4) 0.000(3) -0.005(4) 0.001(3) C29 0.038(5) 0.012(4) 0.035(5) 0.004(4) 0.010(4) 0.007(4) C9 0.034(6) 0.040(6) 0.030(5) -0.001(5) 0.005(4) -0.003(5) C12 0.031(5) 0.030(5) 0.032(5) -0.003(4) 0.002(4) 0.007(4) C32 0.017(4) 0.030(5) 0.031(5) 0.006(4) 0.001(4) 0.004(4) C6 0.028(5) 0.021(4) 0.020(4) -0.001(3) -0.005(4) -0.002(4) C5 0.029(5) 0.019(4) 0.021(4) -0.002(3) -0.003(3) -0.002(3) C43 0.031(5) 0.022(4) 0.031(5) -0.004(4) 0.008(4) -0.005(4) C20 0.017(4) 0.018(4) 0.031(5) 0.003(3) -0.003(4) -0.002(3) C19 0.029(5) 0.024(5) 0.031(5) 0.000(4) -0.003(4) 0.005(4) C44 0.023(5) 0.023(4) 0.026(5) -0.003(4) 0.005(4) -0.001(4) C4 0.035(5) 0.030(5) 0.025(5) -0.007(4) -0.006(4) -0.002(4) C30 0.027(5) 0.031(5) 0.026(5) 0.007(4) 0.005(4) 0.015(4) C2 0.024(5) 0.026(5) 0.045(6) -0.011(4) 0.006(4) -0.010(4) C11 0.030(5) 0.042(6) 0.044(6) -0.006(5) -0.001(5) 0.008(5) C38 0.035(5) 0.031(5) 0.016(4) -0.004(4) 0.007(4) -0.005(4) C10 0.022(5) 0.059(7) 0.031(5) 0.001(5) 0.001(4) -0.001(5) C3 0.027(5) 0.036(5) 0.042(6) -0.016(5) -0.004(4) -0.002(4) F4 0.074(6) 0.031(4) 0.054(5) -0.009(3) 0.014(4) 0.002(4) F3 0.073(6) 0.040(4) 0.071(6) -0.016(4) -0.007(5) 0.003(4) F7 0.032(4) 0.079(6) 0.112(8) 0.063(6) -0.006(5) -0.009(4) N100 0.035(5) 0.037(5) 0.042(6) -0.003(4) 0.006(4) 0.003(4) F2 0.079(7) 0.060(6) 0.147(11) 0.045(7) 0.055(7) 0.013(5) C100 0.019(5) 0.040(6) 0.034(6) -0.003(4) 0.002(4) 0.003(4) F1 0.148(11) 0.062(6) 0.042(5) 0.008(4) -0.012(6) -0.008(7) B2 0.026(5) 0.025(5) 0.030(5) -0.003(4) 0.004(4) -0.006(4) C300 0.037(7) 0.070(8) 0.045(7) 0.006(7) -0.009(6) 0.000(7) C200 0.076(10) 0.041(6) 0.030(6) 0.004(5) -0.007(6) 0.014(6) N200 0.097(11) 0.038(6) 0.073(9) 0.010(6) -0.027(8) 0.004(7) B1 0.067(10) 0.028(6) 0.046(8) 0.004(6) 0.008(7) -0.007(6) C201 0.080(11) 0.053(8) 0.049(8) -0.005(7) -0.012(8) 0.010(8) N300 0.058(9) 0.069(9) 0.089(11) 0.008(8) -0.011(8) 0.001(8) C301 0.062(10) 0.069(9) 0.057(9) -0.019(8) -0.013(8) 0.001(8) C101 0.040(8) 0.066(9) 0.080(11) 0.038(8) 0.013(7) 0.003(7) C400 0.063(9) 0.095(13) 0.093(13) 0.052(10) -0.017(9) -0.027(10) C501 0.050(12) 0.049(12) 0.041(11) 0.003(9) 0.006(9) -0.019(10) N500 0.050(13) 0.070(15) 0.055(13) -0.023(11) 0.005(9) -0.002(11) C401 0.049(12) 0.071(18) 0.066(17) 0.009(16) 0.014(15) -0.001(15) N400 0.044(14) 0.11(3) 0.09(2) 0.02(2) -0.009(16) -0.006(18) F100 0.07(2) 0.08(2) 0.054(14) -0.036(14) -0.015(13) 0.034(17) F101 0.008(9) 0.045(11) 0.09(2) 0.004(12) 0.003(10) -0.006(8) F102 0.011(9) 0.16(3) 0.010(12) 0.016(14) 0.002(8) -0.026(13) F8 0.025(5) 0.064(7) 0.028(7) 0.006(6) -0.011(4) -0.013(5) F6 0.057(8) 0.070(9) 0.066(9) -0.034(7) 0.015(7) -0.027(7) F5 0.040(6) 0.110(13) 0.023(5) 0.020(7) 0.002(5) 0.010(7) _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 Pd3 N7 2.020(8) . ? Pd3 N9 2.032(8) . ? Pd3 N8 2.044(8) . ? Pd3 Br3 2.4297(12) . ? Pd2 N5 1.955(8) . ? Pd2 N4 2.083(7) . ? Pd2 N6 2.106(8) . ? Pd2 Br2 2.4861(13) . ? Pd2 Pd1 3.2447(10) . ? Pd1 N3 2.013(9) . ? Pd1 N1 2.019(9) . ? Pd1 N2 2.047(7) . ? Pd1 Br1 2.4115(12) . ? N6 C31 1.339(12) . ? N6 C23 1.394(12) . ? N9 C44 1.336(12) . ? N9 C40 1.372(13) . ? N5 C24 1.363(12) . ? N5 C21 1.404(13) . ? N7 C34 1.338(12) . ? N7 C38 1.358(13) . ? N3 C12 1.344(14) . ? N3 C8 1.369(13) . ? N2 C6 1.496(12) . ? N2 C7 1.500(12) . ? N2 C13 1.513(12) . ? N8 C32 1.488(13) . ? N8 C39 1.502(13) . ? N8 C33 1.505(11) . ? C23 C24 1.424(12) . ? C23 C28 1.426(12) . ? N4 C14 1.330(11) . ? N4 C22 1.398(12) . ? N1 C1 1.348(13) . ? N1 C5 1.377(12) . ? C16 C15 1.358(15) . ? C16 C17 1.413(14) . ? C16 H16 0.9500 . ? C14 C15 1.423(12) . ? C14 C13 1.509(14) . ? C21 C20 1.380(13) . ? C21 C22 1.414(13) . ? C28 C29 1.406(14) . ? C28 C27 1.408(14) . ? C34 C37 1.396(13) . ? C34 C33 1.493(12) . ? C15 H15 0.9500 . ? C22 C17 1.414(12) . ? C7 C8 1.490(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C37 C36 1.372(14) . ? C37 H37 0.9500 . ? C27 C26 1.393(15) . ? C27 H27 0.9500 . ? C24 C25 1.419(14) . ? C41 C42 1.386(17) . ? C41 C40 1.393(15) . ? C41 H41 0.9500 . ? C26 C25 1.393(14) . ? C26 H26 0.9500 . ? C35 C38 1.390(14) . ? C35 C36 1.390(14) . ? C35 H35 0.9500 . ? C18 C19 1.355(15) . ? C18 C17 1.420(14) . ? C18 H18 0.9500 . ? C31 C30 1.406(13) . ? C31 C32 1.515(14) . ? C36 H36 0.9500 . ? C1 C2 1.374(15) . ? C1 H1 0.9500 . ? C8 C9 1.369(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C42 C43 1.401(16) . ? C42 H42 0.9500 . ? C39 C40 1.493(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C25 H25 0.9500 . ? C29 C30 1.371(15) . ? C29 H29 0.9500 . ? C9 C10 1.390(16) . ? C9 H9 0.9500 . ? C12 C11 1.372(16) . ? C12 H12 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C6 C5 1.490(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 C4 1.392(15) . ? C43 C44 1.373(13) . ? C43 H43 0.9500 . ? C20 C19 1.428(13) . ? C20 H20 0.9500 . ? C19 H19 0.9500 . ? C44 H44 0.9500 . ? C4 C3 1.381(16) . ? C4 H4 0.9500 . ? C30 H30 0.9500 . ? C2 C3 1.387(17) . ? C2 H2 0.9500 . ? C11 C10 1.391(18) . ? C11 H11 0.9500 . ? C38 H38 0.9500 . ? C10 H10 0.9500 . ? C3 H3 0.9500 . ? F4 B1 1.360(17) . ? F3 B1 1.438(18) . ? F7 B2 1.349(15) . ? N100 C100 1.123(15) . ? F2 B1 1.354(19) . ? C100 C101 1.429(18) . ? F1 B1 1.371(18) . ? B2 F101 1.315(18) . ? B2 F102 1.335(18) . ? B2 F5 1.344(15) . ? B2 F8 1.364(15) . ? B2 F6 1.417(15) . ? B2 F100 1.538(19) . ? C300 N300 1.07(2) . ? C300 C301 1.48(2) . ? C200 N200 1.134(19) . ? C200 C201 1.45(2) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C400 C401 1.39(4) . ? C400 C501 1.44(3) . ? C501 N500 1.19(3) . ? C401 N400 1.10(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 N7 Pd3 N9 166.4(3) . . ? N7 Pd3 N8 83.9(3) . . ? N9 Pd3 N8 83.8(3) . . ? N7 Pd3 Br3 97.1(2) . . ? N9 Pd3 Br3 95.2(2) . . ? N8 Pd3 Br3 178.3(2) . . ? N5 Pd2 N4 80.4(3) . . ? N5 Pd2 N6 79.9(3) . . ? N4 Pd2 N6 159.4(3) . . ? N5 Pd2 Br2 173.3(3) . . ? N4 Pd2 Br2 97.7(2) . . ? N6 Pd2 Br2 102.6(2) . . ? N5 Pd2 Pd1 94.7(3) . . ? N4 Pd2 Pd1 72.6(2) . . ? N6 Pd2 Pd1 103.2(2) . . ? Br2 Pd2 Pd1 90.82(3) . . ? N3 Pd1 N1 167.7(3) . . ? N3 Pd1 N2 83.5(3) . . ? N1 Pd1 N2 84.4(3) . . ? N3 Pd1 Br1 95.9(2) . . ? N1 Pd1 Br1 95.9(2) . . ? N2 Pd1 Br1 175.1(2) . . ? N3 Pd1 Pd2 89.8(2) . . ? N1 Pd1 Pd2 93.6(2) . . ? N2 Pd1 Pd2 95.5(2) . . ? Br1 Pd1 Pd2 89.28(3) . . ? C31 N6 C23 118.3(8) . . ? C31 N6 Pd2 133.2(7) . . ? C23 N6 Pd2 107.6(6) . . ? C44 N9 C40 120.4(9) . . ? C44 N9 Pd3 128.7(7) . . ? C40 N9 Pd3 110.5(6) . . ? C24 N5 C21 129.5(8) . . ? C24 N5 Pd2 115.9(6) . . ? C21 N5 Pd2 114.5(6) . . ? C34 N7 C38 119.6(9) . . ? C34 N7 Pd3 112.2(6) . . ? C38 N7 Pd3 127.8(7) . . ? C12 N3 C8 119.6(10) . . ? C12 N3 Pd1 128.6(7) . . ? C8 N3 Pd1 111.2(7) . . ? C6 N2 C7 113.2(7) . . ? C6 N2 C13 111.7(7) . . ? C7 N2 C13 107.7(7) . . ? C6 N2 Pd1 104.4(5) . . ? C7 N2 Pd1 103.0(6) . . ? C13 N2 Pd1 116.7(5) . . ? C32 N8 C39 109.8(8) . . ? C32 N8 C33 113.0(8) . . ? C39 N8 C33 110.7(7) . . ? C32 N8 Pd3 114.7(6) . . ? C39 N8 Pd3 103.7(6) . . ? C33 N8 Pd3 104.5(5) . . ? N6 C23 C24 116.8(8) . . ? N6 C23 C28 121.6(8) . . ? C24 C23 C28 121.4(9) . . ? C14 N4 C22 117.9(8) . . ? C14 N4 Pd2 133.6(7) . . ? C22 N4 Pd2 108.4(6) . . ? C1 N1 C5 119.0(9) . . ? C1 N1 Pd1 129.1(7) . . ? C5 N1 Pd1 111.6(6) . . ? C15 C16 C17 119.4(9) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N4 C14 C15 121.4(9) . . ? N4 C14 C13 120.6(8) . . ? C15 C14 C13 117.8(8) . . ? C20 C21 N5 126.0(9) . . ? C20 C21 C22 121.0(9) . . ? N5 C21 C22 113.1(8) . . ? C29 C28 C27 123.1(9) . . ? C29 C28 C23 117.4(9) . . ? C27 C28 C23 119.5(9) . . ? N7 C34 C37 120.7(8) . . ? N7 C34 C33 116.5(9) . . ? C37 C34 C33 122.5(8) . . ? C16 C15 C14 120.6(9) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N4 C22 C17 122.0(8) . . ? N4 C22 C21 117.4(8) . . ? C17 C22 C21 120.4(9) . . ? C8 C7 N2 109.0(8) . . ? C8 C7 H7A 109.9 . . ? N2 C7 H7A 109.9 . . ? C8 C7 H7B 109.9 . . ? N2 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C14 C13 N2 111.5(7) . . ? C14 C13 H13A 109.3 . . ? N2 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? N2 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C36 C37 C34 120.6(9) . . ? C36 C37 H37 119.7 . . ? C34 C37 H37 119.7 . . ? C26 C27 C28 118.1(8) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? N5 C24 C25 128.0(9) . . ? N5 C24 C23 114.0(8) . . ? C25 C24 C23 117.8(9) . . ? C42 C41 C40 120.8(11) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C27 C26 C25 123.7(10) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C38 C35 C36 119.5(9) . . ? C38 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C19 C18 C17 119.6(9) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? N6 C31 C30 121.4(10) . . ? N6 C31 C32 119.6(8) . . ? C30 C31 C32 118.5(9) . . ? C37 C36 C35 118.2(9) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? N1 C1 C2 122.8(10) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? N3 C8 C9 120.0(10) . . ? N3 C8 C7 115.4(9) . . ? C9 C8 C7 124.5(10) . . ? C34 C33 N8 110.4(7) . . ? C34 C33 H33A 109.6 . . ? N8 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? N8 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C41 C42 C43 117.4(10) . . ? C41 C42 H42 121.3 . . ? C43 C42 H42 121.3 . . ? C40 C39 N8 109.6(8) . . ? C40 C39 H39A 109.8 . . ? N8 C39 H39A 109.8 . . ? C40 C39 H39B 109.8 . . ? N8 C39 H39B 109.8 . . ? H39A C39 H39B 108.2 . . ? C26 C25 C24 119.3(10) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N9 C40 C41 119.5(10) . . ? N9 C40 C39 116.2(9) . . ? C41 C40 C39 124.0(10) . . ? C16 C17 C22 117.6(9) . . ? C16 C17 C18 124.1(9) . . ? C22 C17 C18 118.3(9) . . ? C30 C29 C28 119.4(8) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C8 C9 C10 120.9(11) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? N3 C12 C11 122.1(11) . . ? N3 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? N8 C32 C31 111.7(8) . . ? N8 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? N8 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C5 C6 N2 111.2(8) . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? N2 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N1 C5 C4 120.3(9) . . ? N1 C5 C6 115.4(9) . . ? C4 C5 C6 124.3(9) . . ? C44 C43 C42 120.5(10) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C21 C20 C19 117.2(9) . . ? C21 C20 H20 121.4 . . ? C19 C20 H20 121.4 . . ? C18 C19 C20 123.3(10) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? N9 C44 C43 121.3(10) . . ? N9 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C3 C4 C5 119.4(10) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C29 C30 C31 120.5(10) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C1 C2 C3 118.4(10) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C12 C11 C10 119.2(11) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N7 C38 C35 121.1(10) . . ? N7 C38 H38 119.4 . . ? C35 C38 H38 119.4 . . ? C9 C10 C11 118.1(11) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C4 C3 C2 120.1(11) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? N100 C100 C101 179.0(14) . . ? F101 B2 F102 114.5(14) . . ? F101 B2 F5 57.9(12) . . ? F102 B2 F5 125.1(15) . . ? F101 B2 F7 118.5(12) . . ? F102 B2 F7 116.3(13) . . ? F5 B2 F7 112.0(10) . . ? F101 B2 F8 127.3(13) . . ? F102 B2 F8 23.5(11) . . ? F5 B2 F8 111.8(11) . . ? F7 B2 F8 112.9(10) . . ? F101 B2 F6 50.5(12) . . ? F102 B2 F6 84.2(14) . . ? F5 B2 F6 108.4(11) . . ? F7 B2 F6 103.9(10) . . ? F8 B2 F6 107.3(10) . . ? F101 B2 F100 102.5(13) . . ? F102 B2 F100 100.6(12) . . ? F5 B2 F100 45.5(11) . . ? F7 B2 F100 100.0(11) . . ? F8 B2 F100 78.3(12) . . ? F6 B2 F100 150.6(14) . . ? N300 C300 C301 177.9(18) . . ? N200 C200 C201 179.6(19) . . ? F2 B1 F4 112.1(12) . . ? F2 B1 F1 112.4(15) . . ? F4 B1 F1 114.9(13) . . ? F2 B1 F3 104.4(13) . . ? F4 B1 F3 106.7(13) . . ? F1 B1 F3 105.5(11) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C300 C301 H30A 109.5 . . ? C300 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C300 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C401 C400 C501 49.5(19) . . ? N500 C501 C400 176(3) . . ? N400 C401 C400 173(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.658 _refine_diff_density_min -2.793 _refine_diff_density_rms 0.248 #===END