# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email leehm@cc.ncue.edu.tw _publ_contact_author_name 'Hon Man Lee' loop_ _publ_author_name J.-Y.Lee Y.-H.Huang S.-Y.Liu S.-C.Cheng Y.-M.Jhou 'Hon Man Lee' data_syl017 _database_code_depnum_ccdc_archive 'CCDC 850737' #TrackingRef '- 1.syl017.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C24 H22 Cl F N4 O Pd, C H2 Cl2' _chemical_formula_sum 'C25 H24 Cl3 F N4 O Pd' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 628.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5854(5) _cell_length_b 10.3690(6) _cell_length_c 14.3676(7) _cell_angle_alpha 83.969(2) _cell_angle_beta 71.762(2) _cell_angle_gamma 72.577(2) _cell_volume 1293.95(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2915 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 23.0 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7485 _exptl_absorpt_correction_T_max 0.8080 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17981 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.78 _reflns_number_total 6602 _reflns_number_gt 4868 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0413P)^2^+0.4860P] 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 6602 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C1 C -0.0597(5) 0.6806(5) 0.2714(3) 0.0353(10) Uani 1 1 d . . . H1 H -0.0021 0.7220 0.2955 0.042 Uiso 1 1 calc R . . C2 C -0.1800(5) 0.6425(5) 0.3368(3) 0.0478(13) Uani 1 1 d . . . H2 H -0.2035 0.6557 0.4051 0.057 Uiso 1 1 calc R . . C3 C -0.2669(5) 0.5844(5) 0.3017(3) 0.0474(12) Uani 1 1 d . . . H3 H -0.3511 0.5578 0.3455 0.057 Uiso 1 1 calc R . . C4 C -0.2285(5) 0.5665(4) 0.2033(3) 0.0338(9) Uani 1 1 d . . . H4 H -0.2867 0.5283 0.1772 0.041 Uiso 1 1 calc R . . C5 C 0.2549(5) 1.1670(4) 0.0151(3) 0.0335(10) Uani 1 1 d . . . H5 H 0.2718 1.2538 0.0047 0.040 Uiso 1 1 calc R . . C6 C 0.3496(5) 1.0527(4) -0.0305(3) 0.0314(9) Uani 1 1 d . . . H6 H 0.4455 1.0434 -0.0793 0.038 Uiso 1 1 calc R . . C7 C 0.0483(4) 0.9164(4) 0.1248(3) 0.0268(8) Uani 1 1 d . . . C8 C 0.3313(4) 0.8052(3) -0.0114(3) 0.0230(8) Uani 1 1 d . . . H8 H 0.4254 0.7644 0.0096 0.028 Uiso 1 1 calc R . . C9 C 0.3725(4) 0.7858(4) -0.1193(3) 0.0216(7) Uani 1 1 d . . . C10 C 0.5549(5) 0.6158(4) -0.4185(3) 0.0328(9) Uani 1 1 d . . . H10 H 0.5308 0.6634 -0.4742 0.039 Uiso 1 1 calc R . . C11 C 0.6504(5) 0.4854(4) -0.4289(3) 0.0340(10) Uani 1 1 d . . . H11 H 0.6926 0.4440 -0.4913 0.041 Uiso 1 1 calc R . . C12 C 0.6839(5) 0.4160(4) -0.3481(3) 0.0340(10) Uani 1 1 d . . . H12 H 0.7491 0.3260 -0.3547 0.041 Uiso 1 1 calc R . . C13 C 0.6231(4) 0.4764(4) -0.2569(3) 0.0294(9) Uani 1 1 d . . . H13 H 0.6461 0.4271 -0.2015 0.035 Uiso 1 1 calc R . . C14 C 0.5284(4) 0.6091(4) -0.2459(3) 0.0231(8) Uani 1 1 d . . . C15 C 0.4934(4) 0.6787(4) -0.3281(3) 0.0289(9) Uani 1 1 d . . . H15 H 0.4278 0.7685 -0.3221 0.035 Uiso 1 1 calc R . . C16 C 0.1468(4) 1.0025(4) 0.0733(3) 0.0253(8) Uani 1 1 d . . . C17 C -0.0043(5) 1.2305(4) 0.1445(3) 0.0347(10) Uani 1 1 d . . . H17A H -0.0978 1.2053 0.1485 0.042 Uiso 1 1 calc R . . H17B H -0.0149 1.3227 0.1157 0.042 Uiso 1 1 calc R . . C18 C 0.0077(4) 1.2321(4) 0.2465(3) 0.0288(9) Uani 1 1 d . . . C19 C 0.1010(5) 1.3003(4) 0.2644(3) 0.0367(10) Uani 1 1 d . . . H19 H 0.1563 1.3475 0.2128 0.044 Uiso 1 1 calc R . . C20 C -0.0738(5) 1.1654(4) 0.3227(3) 0.0342(10) Uani 1 1 d . . . H20 H -0.1394 1.1207 0.3103 0.041 Uiso 1 1 calc R . . C21 C -0.0618(5) 1.1626(5) 0.4159(3) 0.0422(11) Uani 1 1 d . . . H21 H -0.1168 1.1157 0.4679 0.051 Uiso 1 1 calc R . . C22 C 0.0331(5) 1.2302(5) 0.4314(3) 0.0427(11) Uani 1 1 d . . . C23 C 0.1128(5) 1.2991(5) 0.3587(3) 0.0433(11) Uani 1 1 d . . . H23 H 0.1757 1.3457 0.3722 0.052 Uiso 1 1 calc R . . C24 C -0.1046(4) 0.6044(4) 0.1421(3) 0.0240(8) Uani 1 1 d . . . H24 H -0.0774 0.5893 0.0739 0.029 Uiso 1 1 calc R . . C25 C 0.4653(10) 0.9443(10) 0.2953(5) 0.127(4) Uani 1 1 d . . . H25A H 0.4884 1.0304 0.2696 0.152 Uiso 1 1 calc R . . H25B H 0.5597 0.8704 0.2692 0.152 Uiso 1 1 calc R . . H7A H 0.0439 0.9213 0.1972 0.050 Uiso 1 1 d . . . H7B H -0.0577 0.9456 0.1038 0.050 Uiso 1 1 d . . . Cl1 Cl 0.28543(10) 0.49596(9) 0.02009(7) 0.0258(2) Uani 1 1 d . . . Cl2 Cl 0.33078(17) 0.92700(19) 0.25010(11) 0.0773(5) Uani 1 1 d . . . Cl3 Cl 0.4246(2) 0.9436(2) 0.41986(12) 0.0961(6) Uani 1 1 d . . . F1 F 0.0460(3) 1.2273(4) 0.52316(19) 0.0675(9) Uani 1 1 d . . . N1 N -0.0204(3) 0.6616(3) 0.1743(2) 0.0227(7) Uani 1 1 d . . . N2 N 0.2804(4) 0.9507(3) 0.0074(2) 0.0248(7) Uani 1 1 d . . . N3 N 0.1291(4) 1.1358(3) 0.0795(2) 0.0279(7) Uani 1 1 d . . . N4 N 0.4742(3) 0.6643(3) -0.1518(2) 0.0245(7) Uani 1 1 d . . . H4A H 0.5113 0.6131 -0.1073 0.029 Uiso 1 1 calc R . . O1 O 0.3186(3) 0.8709(3) -0.17416(18) 0.0292(6) Uani 1 1 d . . . Pd1 Pd 0.16074(3) 0.72504(3) 0.07541(2) 0.02014(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(2) 0.056(3) 0.021(2) -0.0023(18) -0.0060(17) -0.026(2) C2 0.047(3) 0.083(4) 0.021(2) -0.005(2) 0.0011(19) -0.039(3) C3 0.043(3) 0.072(4) 0.033(2) -0.003(2) 0.001(2) -0.037(3) C4 0.032(2) 0.044(3) 0.031(2) 0.0009(18) -0.0104(18) -0.0180(19) C5 0.047(3) 0.021(2) 0.043(2) 0.0067(17) -0.023(2) -0.0176(19) C6 0.036(2) 0.031(2) 0.033(2) 0.0046(17) -0.0112(18) -0.0190(19) C7 0.025(2) 0.0216(19) 0.031(2) -0.0038(16) -0.0034(16) -0.0073(16) C8 0.0249(19) 0.0188(18) 0.0259(19) -0.0022(14) -0.0085(15) -0.0054(15) C9 0.0207(18) 0.0247(19) 0.0227(19) 0.0014(15) -0.0056(15) -0.0128(15) C10 0.037(2) 0.044(3) 0.023(2) 0.0030(17) -0.0125(17) -0.017(2) C11 0.031(2) 0.048(3) 0.024(2) -0.0102(18) -0.0005(17) -0.016(2) C12 0.031(2) 0.032(2) 0.037(2) -0.0092(18) -0.0099(18) -0.0037(18) C13 0.030(2) 0.030(2) 0.026(2) -0.0029(16) -0.0100(17) -0.0046(17) C14 0.0207(18) 0.029(2) 0.0207(18) -0.0011(15) -0.0032(14) -0.0113(16) C15 0.027(2) 0.032(2) 0.028(2) 0.0003(16) -0.0075(16) -0.0082(17) C16 0.031(2) 0.0210(19) 0.027(2) -0.0004(15) -0.0137(17) -0.0054(16) C17 0.038(2) 0.023(2) 0.045(3) -0.0086(18) -0.023(2) 0.0025(18) C18 0.029(2) 0.0213(19) 0.039(2) -0.0103(17) -0.0150(18) -0.0025(16) C19 0.039(2) 0.039(2) 0.034(2) -0.0076(19) -0.0064(19) -0.016(2) C20 0.026(2) 0.032(2) 0.046(3) -0.0133(19) -0.0078(19) -0.0102(18) C21 0.032(2) 0.042(3) 0.045(3) -0.007(2) 0.000(2) -0.009(2) C22 0.033(2) 0.063(3) 0.031(2) -0.015(2) -0.0071(19) -0.010(2) C23 0.035(2) 0.064(3) 0.038(3) -0.014(2) -0.008(2) -0.025(2) C24 0.0266(19) 0.0220(19) 0.026(2) 0.0009(15) -0.0097(16) -0.0088(16) C25 0.146(7) 0.243(11) 0.047(4) 0.024(5) -0.029(4) -0.143(8) Cl1 0.0301(5) 0.0195(4) 0.0281(5) -0.0019(4) -0.0062(4) -0.0093(4) Cl2 0.0530(8) 0.1201(14) 0.0649(10) 0.0241(9) -0.0224(7) -0.0365(9) Cl3 0.1236(16) 0.1264(16) 0.0514(9) 0.0155(9) -0.0327(10) -0.0527(13) F1 0.0609(19) 0.111(3) 0.0333(16) -0.0137(16) -0.0114(14) -0.0266(19) N1 0.0200(15) 0.0246(16) 0.0230(16) 0.0023(12) -0.0041(13) -0.0088(13) N2 0.0310(18) 0.0195(16) 0.0260(17) 0.0015(12) -0.0074(14) -0.0119(14) N3 0.0368(19) 0.0183(16) 0.0322(18) -0.0003(13) -0.0163(15) -0.0066(14) N4 0.0267(17) 0.0241(16) 0.0206(16) -0.0006(12) -0.0054(13) -0.0057(13) O1 0.0328(15) 0.0261(14) 0.0274(14) 0.0016(11) -0.0098(12) -0.0063(12) Pd1 0.02230(15) 0.01877(14) 0.01963(14) -0.00059(10) -0.00448(10) -0.00791(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 C1 N1 1.345(5) . ? C1 C2 1.373(6) . ? C1 H1 0.9500 . ? C2 C3 1.392(6) . ? C2 H2 0.9500 . ? C3 C4 1.364(6) . ? C3 H3 0.9500 . ? C4 C24 1.375(5) . ? C4 H4 0.9500 . ? C5 C6 1.344(6) . ? C5 N3 1.374(5) . ? C5 H5 0.9500 . ? C6 N2 1.388(5) . ? C6 H6 0.9500 . ? C7 C16 1.471(5) . ? C7 Pd1 2.034(4) . ? C7 H7A 1.0344 . ? C7 H7B 1.0966 . ? C8 N2 1.467(4) . ? C8 C9 1.495(5) . ? C8 Pd1 2.059(4) . ? C8 H8 1.0000 . ? C9 O1 1.226(4) . ? C9 N4 1.363(4) . ? C10 C11 1.380(6) . ? C10 C15 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.374(6) . ? C11 H11 0.9500 . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 C14 1.396(5) . ? C13 H13 0.9500 . ? C14 C15 1.397(5) . ? C14 N4 1.405(4) . ? C15 H15 0.9500 . ? C16 N2 1.328(5) . ? C16 N3 1.350(5) . ? C17 N3 1.471(5) . ? C17 C18 1.509(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.384(6) . ? C18 C19 1.388(5) . ? C19 C23 1.393(6) . ? C19 H19 0.9500 . ? C20 C21 1.377(6) . ? C20 H20 0.9500 . ? C21 C22 1.382(6) . ? C21 H21 0.9500 . ? C22 F1 1.358(5) . ? C22 C23 1.362(6) . ? C23 H23 0.9500 . ? C24 N1 1.339(4) . ? C24 H24 0.9500 . ? C25 Cl2 1.675(7) . ? C25 Cl3 1.708(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Cl1 Pd1 2.4093(9) . ? N1 Pd1 2.101(3) . ? N4 H4A 0.8800 . ? 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 N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.0(4) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C24 119.2(4) . . ? C3 C4 H4 120.4 . . ? C24 C4 H4 120.4 . . ? C6 C5 N3 107.7(3) . . ? C6 C5 H5 126.2 . . ? N3 C5 H5 126.2 . . ? C5 C6 N2 106.8(4) . . ? C5 C6 H6 126.6 . . ? N2 C6 H6 126.6 . . ? C16 C7 Pd1 107.0(2) . . ? C16 C7 H7A 103.3 . . ? Pd1 C7 H7A 109.5 . . ? C16 C7 H7B 110.3 . . ? Pd1 C7 H7B 106.0 . . ? H7A C7 H7B 120.2 . . ? N2 C8 C9 108.3(3) . . ? N2 C8 Pd1 107.2(2) . . ? C9 C8 Pd1 116.2(2) . . ? N2 C8 H8 108.3 . . ? C9 C8 H8 108.3 . . ? Pd1 C8 H8 108.3 . . ? O1 C9 N4 122.6(3) . . ? O1 C9 C8 123.2(3) . . ? N4 C9 C8 114.3(3) . . ? C11 C10 C15 121.2(4) . . ? C11 C10 H10 119.4 . . ? C15 C10 H10 119.4 . . ? C12 C11 C10 119.4(4) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.4(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.6(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 N4 117.3(3) . . ? C15 C14 N4 124.0(3) . . ? C10 C15 C14 119.6(4) . . ? C10 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N2 C16 N3 107.6(3) . . ? N2 C16 C7 120.7(3) . . ? N3 C16 C7 131.7(4) . . ? N3 C17 C18 112.9(3) . . ? N3 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N3 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C20 C18 C19 119.7(4) . . ? C20 C18 C17 120.2(4) . . ? C19 C18 C17 120.1(4) . . ? C18 C19 C23 119.4(4) . . ? C18 C19 H19 120.3 . . ? C23 C19 H19 120.3 . . ? C21 C20 C18 121.3(4) . . ? C21 C20 H20 119.4 . . ? C18 C20 H20 119.4 . . ? C20 C21 C22 117.8(4) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? F1 C22 C23 119.4(4) . . ? F1 C22 C21 118.1(4) . . ? C23 C22 C21 122.5(4) . . ? C22 C23 C19 119.3(4) . . ? C22 C23 H23 120.4 . . ? C19 C23 H23 120.4 . . ? N1 C24 C4 123.1(3) . . ? N1 C24 H24 118.5 . . ? C4 C24 H24 118.5 . . ? Cl2 C25 Cl3 117.3(4) . . ? Cl2 C25 H25A 108.0 . . ? Cl3 C25 H25A 108.0 . . ? Cl2 C25 H25B 108.0 . . ? Cl3 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? C24 N1 C1 117.5(3) . . ? C24 N1 Pd1 120.7(2) . . ? C1 N1 Pd1 121.7(3) . . ? C16 N2 C6 109.2(3) . . ? C16 N2 C8 119.1(3) . . ? C6 N2 C8 131.6(3) . . ? C16 N3 C5 108.7(3) . . ? C16 N3 C17 125.0(4) . . ? C5 N3 C17 126.3(3) . . ? C9 N4 C14 129.4(3) . . ? C9 N4 H4A 115.3 . . ? C14 N4 H4A 115.3 . . ? C7 Pd1 C8 86.02(14) . . ? C7 Pd1 N1 88.16(13) . . ? C8 Pd1 N1 173.63(13) . . ? C7 Pd1 Cl1 177.88(11) . . ? C8 Pd1 Cl1 96.07(10) . . ? N1 Pd1 Cl1 89.76(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.3(7) . . . . ? C1 C2 C3 C4 0.4(8) . . . . ? C2 C3 C4 C24 0.9(7) . . . . ? N3 C5 C6 N2 -0.4(4) . . . . ? N2 C8 C9 O1 -25.1(5) . . . . ? Pd1 C8 C9 O1 95.4(4) . . . . ? N2 C8 C9 N4 155.6(3) . . . . ? Pd1 C8 C9 N4 -83.8(3) . . . . ? C15 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C13 -0.4(6) . . . . ? C11 C12 C13 C14 -0.7(6) . . . . ? C12 C13 C14 C15 1.4(6) . . . . ? C12 C13 C14 N4 -178.6(4) . . . . ? C11 C10 C15 C14 0.0(6) . . . . ? C13 C14 C15 C10 -1.0(6) . . . . ? N4 C14 C15 C10 178.9(4) . . . . ? Pd1 C7 C16 N2 1.1(4) . . . . ? Pd1 C7 C16 N3 -178.7(3) . . . . ? N3 C17 C18 C20 -102.6(4) . . . . ? N3 C17 C18 C19 77.2(5) . . . . ? C20 C18 C19 C23 0.9(6) . . . . ? C17 C18 C19 C23 -179.0(4) . . . . ? C19 C18 C20 C21 -1.5(6) . . . . ? C17 C18 C20 C21 178.4(4) . . . . ? C18 C20 C21 C22 0.8(6) . . . . ? C20 C21 C22 F1 -179.7(4) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? F1 C22 C23 C19 179.1(4) . . . . ? C21 C22 C23 C19 -1.0(7) . . . . ? C18 C19 C23 C22 0.3(7) . . . . ? C3 C4 C24 N1 -1.6(6) . . . . ? C4 C24 N1 C1 0.8(5) . . . . ? C4 C24 N1 Pd1 -177.1(3) . . . . ? C2 C1 N1 C24 0.7(6) . . . . ? C2 C1 N1 Pd1 178.5(4) . . . . ? N3 C16 N2 C6 -0.6(4) . . . . ? C7 C16 N2 C6 179.5(3) . . . . ? N3 C16 N2 C8 177.8(3) . . . . ? C7 C16 N2 C8 -2.0(5) . . . . ? C5 C6 N2 C16 0.6(4) . . . . ? C5 C6 N2 C8 -177.6(3) . . . . ? C9 C8 N2 C16 127.8(3) . . . . ? Pd1 C8 N2 C16 1.8(4) . . . . ? C9 C8 N2 C6 -54.2(5) . . . . ? Pd1 C8 N2 C6 179.8(3) . . . . ? N2 C16 N3 C5 0.4(4) . . . . ? C7 C16 N3 C5 -179.8(4) . . . . ? N2 C16 N3 C17 180.0(3) . . . . ? C7 C16 N3 C17 -0.2(6) . . . . ? C6 C5 N3 C16 0.0(4) . . . . ? C6 C5 N3 C17 -179.6(3) . . . . ? C18 C17 N3 C16 84.9(4) . . . . ? C18 C17 N3 C5 -95.6(5) . . . . ? O1 C9 N4 C14 -4.4(6) . . . . ? C8 C9 N4 C14 174.8(3) . . . . ? C13 C14 N4 C9 -174.6(4) . . . . ? C15 C14 N4 C9 5.5(6) . . . . ? C16 C7 Pd1 C8 0.0(3) . . . . ? C16 C7 Pd1 N1 177.4(3) . . . . ? C16 C7 Pd1 Cl1 -170(3) . . . . ? N2 C8 Pd1 C7 -0.9(2) . . . . ? C9 C8 Pd1 C7 -122.0(3) . . . . ? N2 C8 Pd1 N1 -25.0(13) . . . . ? C9 C8 Pd1 N1 -146.1(11) . . . . ? N2 C8 Pd1 Cl1 178.8(2) . . . . ? C9 C8 Pd1 Cl1 57.6(3) . . . . ? C24 N1 Pd1 C7 118.9(3) . . . . ? C1 N1 Pd1 C7 -58.8(3) . . . . ? C24 N1 Pd1 C8 142.9(11) . . . . ? C1 N1 Pd1 C8 -34.8(13) . . . . ? C24 N1 Pd1 Cl1 -60.7(3) . . . . ? C1 N1 Pd1 Cl1 121.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.745 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.120 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 2. ljy295_0t.cif' data_ljy295_0t _database_code_depnum_ccdc_archive 'CCDC 850738' #TrackingRef '- 2. ljy295_0t.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C37 H32 Cl F N3 O P Pd' _chemical_formula_sum 'C37 H32 Cl F N3 O P Pd' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 726.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3340(4) _cell_length_b 10.4256(4) _cell_length_c 18.9156(8) _cell_angle_alpha 80.502(3) _cell_angle_beta 77.272(2) _cell_angle_gamma 68.741(2) _cell_volume 1665.96(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9942 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.0 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8991 _exptl_absorpt_correction_T_max 0.9443 _exptl_absorpt_process_details 'twinabs 2008/2' _exptl_special_details ; 'details of twinning from .abs file' 'BASF w/esd from .lst file' ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14418 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.73 _reflns_number_total 8601 _reflns_number_gt 6196 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0270P)^2^+1.0566P] 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 8601 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 C1 C 0.7927(7) 0.5655(5) 0.6896(2) 0.0523(13) Uani 1 1 d . . . H1A H 0.8943 0.4969 0.6988 0.063 Uiso 1 1 calc R . . H1B H 0.7093 0.5267 0.7126 0.063 Uiso 1 1 calc R . . C2 C 0.7932(6) 0.5986(5) 0.6108(2) 0.0454(11) Uani 1 1 d . . . C3 C 0.7976(7) 0.6022(7) 0.4931(3) 0.0655(17) Uani 1 1 d . . . H3 H 0.7937 0.5759 0.4480 0.079 Uiso 1 1 calc R . . C4 C 0.8164(6) 0.7178(6) 0.5028(2) 0.0581(14) Uani 1 1 d . . . H4 H 0.8304 0.7887 0.4663 0.070 Uiso 1 1 calc R . . C5 C 0.8188(6) 0.8155(5) 0.6209(2) 0.0428(11) Uani 1 1 d . . . H5 H 0.7392 0.9070 0.6093 0.051 Uiso 1 1 calc R . . C6 C 0.9749(5) 0.8299(5) 0.6016(2) 0.0416(10) Uani 1 1 d . . . N3 N 0.9849(4) 0.9377(4) 0.6304(2) 0.0501(10) Uani 1 1 d . . . H3A H 0.8961 0.9938 0.6519 0.060 Uiso 1 1 calc R . . C7 C 1.1174(5) 0.9706(5) 0.6302(2) 0.0470(12) Uani 1 1 d . . . C8 C 1.2608(6) 0.9145(6) 0.5868(3) 0.0675(16) Uani 1 1 d . . . H8 H 1.2737 0.8511 0.5532 0.081 Uiso 1 1 calc R . . C9 C 1.3859(7) 0.9520(7) 0.5929(4) 0.0820(19) Uani 1 1 d . . . H9 H 1.4849 0.9122 0.5637 0.098 Uiso 1 1 calc R . . C10 C 1.3695(8) 1.0447(8) 0.6398(4) 0.086(2) Uani 1 1 d . . . H10 H 1.4565 1.0680 0.6439 0.104 Uiso 1 1 calc R . . C11 C 1.2265(8) 1.1036(7) 0.6809(3) 0.0767(18) Uani 1 1 d . . . H11 H 1.2128 1.1708 0.7124 0.092 Uiso 1 1 calc R . . C12 C 1.1025(6) 1.0655(6) 0.6765(3) 0.0593(14) Uani 1 1 d . . . H12 H 1.0042 1.1055 0.7061 0.071 Uiso 1 1 calc R . . C13 C 0.7576(7) 0.3944(6) 0.5747(3) 0.0691(17) Uani 1 1 d . . . H13A H 0.8427 0.3257 0.5983 0.083 Uiso 1 1 calc R . . H13B H 0.7609 0.3610 0.5282 0.083 Uiso 1 1 calc R . . C14 C 0.6029(6) 0.4047(5) 0.6233(3) 0.0516(12) Uani 1 1 d . . . C15 C 0.4670(7) 0.5136(6) 0.6148(3) 0.0663(15) Uani 1 1 d . . . H15 H 0.4698 0.5860 0.5773 0.080 Uiso 1 1 calc R . . C16 C 0.3292(7) 0.5191(7) 0.6593(4) 0.0755(17) Uani 1 1 d . . . H16 H 0.2362 0.5937 0.6524 0.091 Uiso 1 1 calc R . . C17 C 0.3261(8) 0.4174(7) 0.7132(4) 0.0757(18) Uani 1 1 d . . . C18 C 0.4557(7) 0.3080(7) 0.7249(4) 0.0785(17) Uani 1 1 d . . . H18 H 0.4509 0.2372 0.7631 0.094 Uiso 1 1 calc R . . C19 C 0.5946(7) 0.3039(6) 0.6793(3) 0.0653(15) Uani 1 1 d . . . H19 H 0.6871 0.2291 0.6868 0.078 Uiso 1 1 calc R . . C20 C 0.7083(5) 0.4724(5) 0.8564(2) 0.0397(10) Uani 1 1 d . . . C21 C 0.8677(6) 0.3931(5) 0.8448(2) 0.0497(12) Uani 1 1 d . . . H21 H 0.9436 0.4376 0.8332 0.060 Uiso 1 1 calc R . . C22 C 0.9147(7) 0.2499(5) 0.8502(3) 0.0595(14) Uani 1 1 d . . . H22 H 1.0228 0.1966 0.8427 0.071 Uiso 1 1 calc R . . C23 C 0.8051(7) 0.1845(5) 0.8664(3) 0.0624(15) Uani 1 1 d . . . H23 H 0.8374 0.0866 0.8690 0.075 Uiso 1 1 calc R . . C24 C 0.6489(7) 0.2618(6) 0.8786(3) 0.0636(15) Uani 1 1 d . . . H24 H 0.5733 0.2168 0.8908 0.076 Uiso 1 1 calc R . . C25 C 0.6012(6) 0.4036(5) 0.8735(3) 0.0516(12) Uani 1 1 d . . . H25 H 0.4928 0.4555 0.8818 0.062 Uiso 1 1 calc R . . C26 C 0.4423(5) 0.7199(5) 0.8581(2) 0.0428(10) Uani 1 1 d . . . C27 C 0.3710(7) 0.7366(6) 0.7992(3) 0.0670(16) Uani 1 1 d . . . H27 H 0.4326 0.7253 0.7519 0.080 Uiso 1 1 calc R . . C28 C 0.2109(7) 0.7697(7) 0.8076(3) 0.0787(18) Uani 1 1 d . . . H28 H 0.1642 0.7773 0.7666 0.094 Uiso 1 1 calc R . . C29 C 0.1200(7) 0.7915(6) 0.8747(4) 0.0775(18) Uani 1 1 d . . . H29 H 0.0098 0.8167 0.8805 0.093 Uiso 1 1 calc R . . C30 C 0.1898(7) 0.7765(7) 0.9337(3) 0.0786(18) Uani 1 1 d . . . H30 H 0.1270 0.7910 0.9805 0.094 Uiso 1 1 calc R . . C31 C 0.3478(6) 0.7412(6) 0.9263(3) 0.0603(14) Uani 1 1 d . . . H31 H 0.3936 0.7310 0.9679 0.072 Uiso 1 1 calc R . . C32 C 0.6966(6) 0.6979(5) 0.9278(2) 0.0440(11) Uani 1 1 d . . . C33 C 0.7632(6) 0.5970(6) 0.9791(3) 0.0600(14) Uani 1 1 d . . . H33 H 0.7884 0.5025 0.9722 0.072 Uiso 1 1 calc R . . C34 C 0.7941(7) 0.6307(8) 1.0406(3) 0.083(2) Uani 1 1 d . . . H34 H 0.8382 0.5593 1.0759 0.100 Uiso 1 1 calc R . . C35 C 0.7618(7) 0.7649(9) 1.0511(3) 0.085(2) Uani 1 1 d . . . H35 H 0.7843 0.7877 1.0930 0.102 Uiso 1 1 calc R . . C36 C 0.6964(8) 0.8669(7) 1.0004(3) 0.0795(19) Uani 1 1 d . . . H36 H 0.6728 0.9609 1.0077 0.095 Uiso 1 1 calc R . . C37 C 0.6640(7) 0.8359(6) 0.9386(3) 0.0665(16) Uani 1 1 d . . . H37 H 0.6199 0.9079 0.9036 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.71526(19) 0.96566(13) 0.76742(7) 0.0687(4) Uani 1 1 d . . . F1 F 0.1897(4) 0.4251(5) 0.7584(2) 0.1241(16) Uani 1 1 d . . . N1 N 0.8118(4) 0.7149(4) 0.57709(19) 0.0452(9) Uani 1 1 d . . . N2 N 0.7846(5) 0.5270(5) 0.5596(2) 0.0588(12) Uani 1 1 d . . . O1 O 1.0866(4) 0.7503(4) 0.56593(18) 0.0604(10) Uani 1 1 d . . . P1 P 0.65459(14) 0.66028(12) 0.84485(6) 0.0387(3) Uani 1 1 d . . . Pd1 Pd 0.75382(4) 0.74577(4) 0.731096(18) 0.03824(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(4) 0.045(3) 0.041(2) -0.010(2) -0.002(2) -0.025(3) C2 0.050(3) 0.056(3) 0.036(2) -0.013(2) 0.003(2) -0.027(2) C3 0.076(4) 0.107(5) 0.032(2) -0.015(3) 0.000(2) -0.055(4) C4 0.064(3) 0.087(4) 0.033(2) -0.001(2) -0.004(2) -0.042(3) C5 0.045(3) 0.044(3) 0.041(2) -0.004(2) -0.001(2) -0.019(2) C6 0.041(3) 0.042(3) 0.041(2) 0.004(2) -0.007(2) -0.018(2) N3 0.042(2) 0.046(2) 0.062(2) -0.0156(19) 0.0100(18) -0.0198(19) C7 0.041(3) 0.054(3) 0.050(3) -0.001(2) -0.006(2) -0.024(2) C8 0.050(3) 0.070(4) 0.084(4) -0.015(3) 0.006(3) -0.030(3) C9 0.045(4) 0.092(5) 0.109(5) -0.020(4) 0.003(3) -0.028(3) C10 0.058(4) 0.112(6) 0.105(5) -0.009(5) -0.022(4) -0.043(4) C11 0.083(5) 0.104(5) 0.069(4) -0.018(4) -0.015(3) -0.056(4) C12 0.055(3) 0.071(4) 0.059(3) -0.009(3) -0.003(2) -0.033(3) C13 0.083(4) 0.074(4) 0.065(3) -0.037(3) 0.017(3) -0.048(3) C14 0.059(3) 0.051(3) 0.054(3) -0.015(2) -0.004(2) -0.029(3) C15 0.074(4) 0.070(4) 0.058(3) 0.004(3) -0.017(3) -0.029(4) C16 0.048(4) 0.077(4) 0.104(5) -0.016(4) -0.025(3) -0.014(3) C17 0.063(4) 0.086(5) 0.089(5) -0.015(4) 0.001(3) -0.044(4) C18 0.066(4) 0.086(4) 0.089(4) 0.013(4) -0.005(4) -0.045(4) C19 0.052(3) 0.054(3) 0.091(4) -0.005(3) -0.012(3) -0.021(3) C20 0.045(3) 0.044(3) 0.033(2) -0.0058(19) -0.0016(19) -0.021(2) C21 0.046(3) 0.056(3) 0.049(3) -0.011(2) -0.002(2) -0.021(3) C22 0.056(3) 0.052(3) 0.063(3) -0.017(3) -0.011(3) -0.004(3) C23 0.087(5) 0.039(3) 0.062(3) -0.006(2) -0.016(3) -0.020(3) C24 0.076(4) 0.054(3) 0.074(4) -0.004(3) -0.012(3) -0.038(3) C25 0.054(3) 0.047(3) 0.056(3) -0.006(2) -0.002(2) -0.024(2) C26 0.046(3) 0.041(2) 0.040(2) -0.0018(19) -0.007(2) -0.015(2) C27 0.055(4) 0.097(5) 0.043(3) 0.005(3) -0.007(2) -0.025(3) C28 0.062(4) 0.101(5) 0.074(4) 0.012(4) -0.027(3) -0.029(4) C29 0.038(3) 0.070(4) 0.102(5) 0.009(4) -0.005(3) -0.004(3) C30 0.052(4) 0.099(5) 0.067(4) -0.017(3) 0.012(3) -0.014(3) C31 0.045(3) 0.083(4) 0.047(3) -0.015(3) 0.002(2) -0.017(3) C32 0.040(3) 0.058(3) 0.037(2) -0.010(2) 0.003(2) -0.023(2) C33 0.060(3) 0.072(4) 0.050(3) -0.017(3) -0.013(2) -0.018(3) C34 0.071(4) 0.115(6) 0.060(4) -0.025(4) -0.026(3) -0.012(4) C35 0.065(4) 0.146(7) 0.066(4) -0.051(4) -0.008(3) -0.044(4) C36 0.101(5) 0.095(5) 0.062(4) -0.031(4) 0.003(4) -0.057(4) C37 0.093(4) 0.068(4) 0.047(3) -0.015(3) 0.003(3) -0.042(3) Cl1 0.0992(11) 0.0494(8) 0.0591(8) -0.0195(6) 0.0193(7) -0.0401(8) F1 0.057(2) 0.156(4) 0.157(4) -0.016(3) 0.015(2) -0.052(3) N1 0.051(2) 0.056(2) 0.0325(18) -0.0020(17) -0.0017(17) -0.027(2) N2 0.073(3) 0.075(3) 0.043(2) -0.021(2) 0.013(2) -0.048(3) O1 0.049(2) 0.076(3) 0.058(2) -0.0317(19) 0.0090(16) -0.0222(19) P1 0.0418(7) 0.0424(7) 0.0335(6) -0.0059(5) 0.0012(5) -0.0198(6) Pd1 0.04472(19) 0.03911(17) 0.03345(15) -0.00726(15) 0.00322(15) -0.02138(14) _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 C1 C2 1.474(6) . ? C1 Pd1 2.036(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.325(6) . ? C2 N2 1.347(5) . ? C3 C4 1.327(7) . ? C3 N2 1.375(6) . ? C3 H3 0.9500 . ? C4 N1 1.391(5) . ? C4 H4 0.9500 . ? C5 N1 1.467(6) . ? C5 C6 1.479(6) . ? C5 Pd1 2.122(4) . ? C5 H5 1.0000 . ? C6 O1 1.216(5) . ? C6 N3 1.367(5) . ? N3 C7 1.397(6) . ? N3 H3A 0.8800 . ? C7 C12 1.378(7) . ? C7 C8 1.383(7) . ? C8 C9 1.390(8) . ? C8 H8 0.9500 . ? C9 C10 1.365(8) . ? C9 H9 0.9500 . ? C10 C11 1.366(8) . ? C10 H10 0.9500 . ? C11 C12 1.376(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N2 1.465(6) . ? C13 C14 1.509(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.374(7) . ? C14 C15 1.382(7) . ? C15 C16 1.360(8) . ? C15 H15 0.9500 . ? C16 C17 1.348(9) . ? C16 H16 0.9500 . ? C17 F1 1.351(7) . ? C17 C18 1.359(8) . ? C18 C19 1.380(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.385(6) . ? C20 C21 1.403(6) . ? C20 P1 1.825(5) . ? C21 C22 1.388(7) . ? C21 H21 0.9500 . ? C22 C23 1.380(7) . ? C22 H22 0.9500 . ? C23 C24 1.375(8) . ? C23 H23 0.9500 . ? C24 C25 1.374(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.377(7) . ? C26 C31 1.394(6) . ? C26 P1 1.820(5) . ? C27 C28 1.384(8) . ? C27 H27 0.9500 . ? C28 C29 1.365(8) . ? C28 H28 0.9500 . ? C29 C30 1.372(8) . ? C29 H29 0.9500 . ? C30 C31 1.364(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.375(7) . ? C32 C37 1.398(7) . ? C32 P1 1.832(5) . ? C33 C34 1.384(7) . ? C33 H33 0.9500 . ? C34 C35 1.359(9) . ? C34 H34 0.9500 . ? C35 C36 1.369(9) . ? C35 H35 0.9500 . ? C36 C37 1.384(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? Cl1 Pd1 2.3810(12) . ? P1 Pd1 2.3173(11) . ? 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 C2 C1 Pd1 106.7(3) . . ? C2 C1 H1A 110.4 . . ? Pd1 C1 H1A 110.4 . . ? C2 C1 H1B 110.4 . . ? Pd1 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? N1 C2 N2 107.1(4) . . ? N1 C2 C1 120.8(4) . . ? N2 C2 C1 132.0(4) . . ? C4 C3 N2 108.1(4) . . ? C4 C3 H3 126.0 . . ? N2 C3 H3 126.0 . . ? C3 C4 N1 106.5(5) . . ? C3 C4 H4 126.7 . . ? N1 C4 H4 126.7 . . ? N1 C5 C6 109.6(4) . . ? N1 C5 Pd1 106.0(3) . . ? C6 C5 Pd1 115.7(3) . . ? N1 C5 H5 108.5 . . ? C6 C5 H5 108.5 . . ? Pd1 C5 H5 108.5 . . ? O1 C6 N3 122.6(4) . . ? O1 C6 C5 123.5(4) . . ? N3 C6 C5 113.9(4) . . ? C6 N3 C7 128.6(4) . . ? C6 N3 H3A 115.7 . . ? C7 N3 H3A 115.7 . . ? C12 C7 C8 118.5(5) . . ? C12 C7 N3 117.1(4) . . ? C8 C7 N3 124.4(5) . . ? C7 C8 C9 119.3(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 121.4(6) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.3(6) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 121.5(5) . . ? C11 C12 H12 119.2 . . ? C7 C12 H12 119.2 . . ? N2 C13 C14 112.5(4) . . ? N2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C19 C14 C15 117.6(5) . . ? C19 C14 C13 119.7(5) . . ? C15 C14 C13 122.7(5) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 119.3(6) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 F1 119.0(7) . . ? C16 C17 C18 122.6(6) . . ? F1 C17 C18 118.4(6) . . ? C17 C18 C19 117.5(6) . . ? C17 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C14 C19 C18 121.9(6) . . ? C14 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C25 C20 C21 118.1(4) . . ? C25 C20 P1 123.9(4) . . ? C21 C20 P1 117.9(3) . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.2(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.7(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 121.2(5) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C27 C26 C31 117.9(5) . . ? C27 C26 P1 119.0(4) . . ? C31 C26 P1 123.0(4) . . ? C26 C27 C28 121.1(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 120.2(6) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.1(6) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 121.2(5) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C26 120.4(5) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.8 . . ? C33 C32 C37 118.1(5) . . ? C33 C32 P1 123.3(4) . . ? C37 C32 P1 118.6(4) . . ? C32 C33 C34 121.1(6) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120.6(7) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.2(6) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C37 121.3(6) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C32 119.7(6) . . ? C36 C37 H37 120.2 . . ? C32 C37 H37 120.2 . . ? C2 N1 C4 109.5(4) . . ? C2 N1 C5 118.5(3) . . ? C4 N1 C5 131.9(4) . . ? C2 N2 C3 108.7(4) . . ? C2 N2 C13 124.5(4) . . ? C3 N2 C13 126.7(4) . . ? C26 P1 C20 103.3(2) . . ? C26 P1 C32 104.2(2) . . ? C20 P1 C32 102.7(2) . . ? C26 P1 Pd1 110.03(15) . . ? C20 P1 Pd1 113.92(13) . . ? C32 P1 Pd1 120.88(15) . . ? C1 Pd1 C5 83.99(18) . . ? C1 Pd1 P1 90.66(13) . . ? C5 Pd1 P1 171.01(13) . . ? C1 Pd1 Cl1 174.26(14) . . ? C5 Pd1 Cl1 90.27(13) . . ? P1 Pd1 Cl1 95.02(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 C1 C2 N1 17.7(6) . . . . ? Pd1 C1 C2 N2 -165.8(5) . . . . ? N2 C3 C4 N1 -1.2(6) . . . . ? N1 C5 C6 O1 -13.4(6) . . . . ? Pd1 C5 C6 O1 106.3(5) . . . . ? N1 C5 C6 N3 169.6(4) . . . . ? Pd1 C5 C6 N3 -70.7(5) . . . . ? O1 C6 N3 C7 -5.3(7) . . . . ? C5 C6 N3 C7 171.8(4) . . . . ? C6 N3 C7 C12 -165.8(5) . . . . ? C6 N3 C7 C8 14.2(8) . . . . ? C12 C7 C8 C9 2.0(8) . . . . ? N3 C7 C8 C9 -178.0(5) . . . . ? C7 C8 C9 C10 -1.1(10) . . . . ? C8 C9 C10 C11 -1.1(11) . . . . ? C9 C10 C11 C12 2.3(11) . . . . ? C10 C11 C12 C7 -1.4(10) . . . . ? C8 C7 C12 C11 -0.8(8) . . . . ? N3 C7 C12 C11 179.3(5) . . . . ? N2 C13 C14 C19 -136.6(5) . . . . ? N2 C13 C14 C15 42.4(7) . . . . ? C19 C14 C15 C16 -1.5(8) . . . . ? C13 C14 C15 C16 179.5(5) . . . . ? C14 C15 C16 C17 1.0(9) . . . . ? C15 C16 C17 F1 178.3(5) . . . . ? C15 C16 C17 C18 -0.4(10) . . . . ? C16 C17 C18 C19 0.3(10) . . . . ? F1 C17 C18 C19 -178.4(5) . . . . ? C15 C14 C19 C18 1.4(8) . . . . ? C13 C14 C19 C18 -179.5(5) . . . . ? C17 C18 C19 C14 -0.8(9) . . . . ? C25 C20 C21 C22 0.2(7) . . . . ? P1 C20 C21 C22 -177.5(4) . . . . ? C20 C21 C22 C23 0.6(8) . . . . ? C21 C22 C23 C24 -1.3(8) . . . . ? C22 C23 C24 C25 1.3(8) . . . . ? C23 C24 C25 C20 -0.5(8) . . . . ? C21 C20 C25 C24 -0.3(7) . . . . ? P1 C20 C25 C24 177.3(4) . . . . ? C31 C26 C27 C28 -1.8(8) . . . . ? P1 C26 C27 C28 174.1(5) . . . . ? C26 C27 C28 C29 2.5(10) . . . . ? C27 C28 C29 C30 -1.7(10) . . . . ? C28 C29 C30 C31 0.4(10) . . . . ? C29 C30 C31 C26 0.3(10) . . . . ? C27 C26 C31 C30 0.4(8) . . . . ? P1 C26 C31 C30 -175.3(5) . . . . ? C37 C32 C33 C34 1.4(8) . . . . ? P1 C32 C33 C34 179.4(4) . . . . ? C32 C33 C34 C35 -1.3(9) . . . . ? C33 C34 C35 C36 0.8(10) . . . . ? C34 C35 C36 C37 -0.6(10) . . . . ? C35 C36 C37 C32 0.8(9) . . . . ? C33 C32 C37 C36 -1.2(8) . . . . ? P1 C32 C37 C36 -179.2(4) . . . . ? N2 C2 N1 C4 -0.5(6) . . . . ? C1 C2 N1 C4 176.8(4) . . . . ? N2 C2 N1 C5 177.8(4) . . . . ? C1 C2 N1 C5 -5.0(7) . . . . ? C3 C4 N1 C2 1.1(6) . . . . ? C3 C4 N1 C5 -176.9(5) . . . . ? C6 C5 N1 C2 115.5(5) . . . . ? Pd1 C5 N1 C2 -10.0(5) . . . . ? C6 C5 N1 C4 -66.7(6) . . . . ? Pd1 C5 N1 C4 167.8(4) . . . . ? N1 C2 N2 C3 -0.3(6) . . . . ? C1 C2 N2 C3 -177.1(5) . . . . ? N1 C2 N2 C13 -177.4(5) . . . . ? C1 C2 N2 C13 5.8(9) . . . . ? C4 C3 N2 C2 0.9(6) . . . . ? C4 C3 N2 C13 178.0(5) . . . . ? C14 C13 N2 C2 61.3(7) . . . . ? C14 C13 N2 C3 -115.3(6) . . . . ? C27 C26 P1 C20 -88.0(4) . . . . ? C31 C26 P1 C20 87.7(4) . . . . ? C27 C26 P1 C32 165.0(4) . . . . ? C31 C26 P1 C32 -19.3(5) . . . . ? C27 C26 P1 Pd1 34.0(5) . . . . ? C31 C26 P1 Pd1 -150.3(4) . . . . ? C25 C20 P1 C26 -1.7(4) . . . . ? C21 C20 P1 C26 175.9(3) . . . . ? C25 C20 P1 C32 106.5(4) . . . . ? C21 C20 P1 C32 -75.9(4) . . . . ? C25 C20 P1 Pd1 -121.0(3) . . . . ? C21 C20 P1 Pd1 56.6(4) . . . . ? C33 C32 P1 C26 111.5(4) . . . . ? C37 C32 P1 C26 -70.6(4) . . . . ? C33 C32 P1 C20 4.0(5) . . . . ? C37 C32 P1 C20 -178.1(4) . . . . ? C33 C32 P1 Pd1 -124.3(4) . . . . ? C37 C32 P1 Pd1 53.7(4) . . . . ? C2 C1 Pd1 C5 -17.1(4) . . . . ? C2 C1 Pd1 P1 155.6(3) . . . . ? C2 C1 Pd1 Cl1 -17(2) . . . . ? N1 C5 Pd1 C1 15.2(3) . . . . ? C6 C5 Pd1 C1 -106.5(4) . . . . ? N1 C5 Pd1 P1 -38.6(11) . . . . ? C6 C5 Pd1 P1 -160.2(7) . . . . ? N1 C5 Pd1 Cl1 -164.8(3) . . . . ? C6 C5 Pd1 Cl1 73.6(3) . . . . ? C26 P1 Pd1 C1 -97.2(2) . . . . ? C20 P1 Pd1 C1 18.3(2) . . . . ? C32 P1 Pd1 C1 141.3(3) . . . . ? C26 P1 Pd1 C5 -43.8(9) . . . . ? C20 P1 Pd1 C5 71.6(9) . . . . ? C32 P1 Pd1 C5 -165.3(9) . . . . ? C26 P1 Pd1 Cl1 82.09(16) . . . . ? C20 P1 Pd1 Cl1 -162.50(17) . . . . ? C32 P1 Pd1 Cl1 -39.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.755 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.094 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 4.ljy309.cif' data_ljy309 _database_code_depnum_ccdc_archive 'CCDC 850739' #TrackingRef '- 4.ljy309.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C37 H32 Cl F N3 O P Pd, C3 H7 N O, 0.5(C4 H10 O)' _chemical_formula_sum 'C84 H88 Cl2 F2 N8 O5 P2 Pd2' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 836.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5982(11) _cell_length_b 16.6492(13) _cell_length_c 17.5208(15) _cell_angle_alpha 81.635(6) _cell_angle_beta 70.792(5) _cell_angle_gamma 82.732(4) _cell_volume 3964.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2777 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 19.8 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_T_max 0.8962 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49723 _diffrn_reflns_av_R_equivalents 0.1182 _diffrn_reflns_av_sigmaI/netI 0.1576 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.00 _reflns_number_total 17316 _reflns_number_gt 8848 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0453P)^2^+0.0000P] 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 17316 _refine_ls_number_parameters 954 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 C1 C 0.9383(4) 0.6941(3) 0.0917(4) 0.0331(15) Uani 1 1 d . . . C2 C 0.9654(4) 0.6319(3) 0.1564(3) 0.0337(15) Uani 1 1 d . . . H2 H 1.0368 0.6151 0.1383 0.040 Uiso 1 1 calc R . . C3 C 0.9380(4) 0.4926(4) 0.1334(4) 0.0370(15) Uani 1 1 d . . . C4 C 0.8077(4) 0.5636(4) 0.2065(4) 0.0385(16) Uani 1 1 d . . . H4 H 0.7683 0.6051 0.2372 0.046 Uiso 1 1 calc R . . C5 C 0.7771(5) 0.4976(4) 0.1912(4) 0.0423(16) Uani 1 1 d . . . H5 H 0.7118 0.4834 0.2081 0.051 Uiso 1 1 calc R . . C6 C 1.0385(4) 0.4653(4) 0.0875(4) 0.0404(16) Uani 1 1 d . . . H6A H 1.0818 0.5071 0.0839 0.061 Uiso 1 1 calc R . . H6B H 1.0415 0.4563 0.0326 0.061 Uiso 1 1 calc R . . H6C H 1.0590 0.4144 0.1154 0.061 Uiso 1 1 calc R . . C7 C 0.8578(4) 0.3748(3) 0.1155(4) 0.0355(15) Uani 1 1 d . . . H7A H 0.9102 0.3704 0.0630 0.043 Uiso 1 1 calc R . . H7B H 0.7948 0.3748 0.1056 0.043 Uiso 1 1 calc R . . C8 C 0.8697(4) 0.3015(3) 0.1740(4) 0.0334(14) Uani 1 1 d . . . C9 C 0.8000(4) 0.2882(3) 0.2493(4) 0.0349(15) Uani 1 1 d . . . H9 H 0.7445 0.3261 0.2646 0.042 Uiso 1 1 calc R . . C10 C 0.8103(5) 0.2201(4) 0.3026(4) 0.0446(17) Uani 1 1 d . . . H10 H 0.7633 0.2113 0.3548 0.054 Uiso 1 1 calc R . . C11 C 0.8904(5) 0.1659(4) 0.2779(5) 0.0508(18) Uani 1 1 d . . . C12 C 0.9609(5) 0.1767(4) 0.2045(4) 0.0537(19) Uani 1 1 d . . . H12 H 1.0162 0.1386 0.1898 0.064 Uiso 1 1 calc R . . C13 C 0.9494(4) 0.2454(4) 0.1513(4) 0.0424(17) Uani 1 1 d . . . H13 H 0.9966 0.2537 0.0992 0.051 Uiso 1 1 calc R . . C14 C 0.9053(4) 0.8421(3) 0.0815(3) 0.0290(14) Uani 1 1 d . . . C15 C 0.8663(4) 0.8517(3) 0.0180(3) 0.0315(14) Uani 1 1 d . . . H15 H 0.8572 0.8048 -0.0029 0.038 Uiso 1 1 calc R . . C16 C 0.8404(4) 0.9285(4) -0.0153(4) 0.0440(17) Uani 1 1 d . . . H16 H 0.8133 0.9335 -0.0583 0.053 Uiso 1 1 calc R . . C17 C 0.8537(5) 0.9980(4) 0.0135(4) 0.0471(18) Uani 1 1 d . . . H17 H 0.8355 1.0506 -0.0090 0.057 Uiso 1 1 calc R . . C18 C 0.8933(5) 0.9892(4) 0.0745(4) 0.0478(18) Uani 1 1 d . . . H18 H 0.9038 1.0366 0.0937 0.057 Uiso 1 1 calc R . . C19 C 0.9194(4) 0.9124(3) 0.1102(4) 0.0365(15) Uani 1 1 d . . . H19 H 0.9462 0.9081 0.1534 0.044 Uiso 1 1 calc R . . C20 C 1.0493(4) 0.4875(4) 0.2861(3) 0.0371(15) Uani 1 1 d . . . H20 H 1.1033 0.5187 0.2592 0.045 Uiso 1 1 calc R . . C21 C 1.0565(5) 0.4065(4) 0.2757(4) 0.0406(16) Uani 1 1 d . . . H21 H 1.1158 0.3819 0.2427 0.049 Uiso 1 1 calc R . . C22 C 0.9779(5) 0.3607(4) 0.3132(4) 0.0433(17) Uani 1 1 d . . . H22 H 0.9828 0.3045 0.3065 0.052 Uiso 1 1 calc R . . C23 C 0.8915(5) 0.3978(4) 0.3609(4) 0.0459(17) Uani 1 1 d . . . H23 H 0.8368 0.3670 0.3866 0.055 Uiso 1 1 calc R . . C24 C 0.8849(4) 0.4789(3) 0.3712(4) 0.0383(15) Uani 1 1 d . . . H24 H 0.8253 0.5040 0.4032 0.046 Uiso 1 1 calc R . . C25 C 0.9645(4) 0.5242(3) 0.3351(3) 0.0291(13) Uani 1 1 d . . . C26 C 0.8564(4) 0.6454(3) 0.4370(3) 0.0298(14) Uani 1 1 d . . . C27 C 0.7641(4) 0.6712(3) 0.4343(4) 0.0339(14) Uani 1 1 d . . . H27 H 0.7540 0.6858 0.3830 0.041 Uiso 1 1 calc R . . C28 C 0.6851(4) 0.6766(3) 0.5049(4) 0.0348(14) Uani 1 1 d . . . H28 H 0.6220 0.6944 0.5013 0.042 Uiso 1 1 calc R . . C29 C 0.6979(5) 0.6564(4) 0.5786(4) 0.0489(18) Uani 1 1 d . . . H29 H 0.6437 0.6592 0.6267 0.059 Uiso 1 1 calc R . . C30 C 0.7886(5) 0.6322(4) 0.5837(4) 0.057(2) Uani 1 1 d . . . H30 H 0.7972 0.6189 0.6356 0.068 Uiso 1 1 calc R . . C31 C 0.8696(5) 0.6267(4) 0.5135(4) 0.0444(17) Uani 1 1 d . . . H31 H 0.9326 0.6104 0.5178 0.053 Uiso 1 1 calc R . . C32 C 1.0668(4) 0.6473(4) 0.3614(4) 0.0345(15) Uani 1 1 d . . . C33 C 1.1117(5) 0.5855(4) 0.4021(4) 0.0472(18) Uani 1 1 d . . . H33 H 1.0836 0.5349 0.4202 0.057 Uiso 1 1 calc R . . C34 C 1.1969(5) 0.5960(5) 0.4171(4) 0.062(2) Uani 1 1 d . . . H34 H 1.2274 0.5531 0.4447 0.075 Uiso 1 1 calc R . . C35 C 1.2371(5) 0.6717(5) 0.3903(5) 0.071(3) Uani 1 1 d . . . H35 H 1.2937 0.6812 0.4019 0.085 Uiso 1 1 calc R . . C36 C 1.1949(5) 0.7308(5) 0.3481(4) 0.061(2) Uani 1 1 d . . . H36 H 1.2242 0.7807 0.3282 0.073 Uiso 1 1 calc R . . C37 C 1.1101(5) 0.7202(4) 0.3332(4) 0.0493(18) Uani 1 1 d . . . H37 H 1.0814 0.7627 0.3038 0.059 Uiso 1 1 calc R . . C38 C 0.5452(4) 0.2092(3) 0.3863(4) 0.0328(14) Uani 1 1 d . . . C39 C 0.5225(4) 0.1610(3) 0.3274(3) 0.0317(14) Uani 1 1 d . . . H39 H 0.4517 0.1520 0.3461 0.038 Uiso 1 1 calc R . . C40 C 0.5562(4) 0.0114(3) 0.3620(4) 0.0342(15) Uani 1 1 d . . . C41 C 0.6802(4) 0.0743(4) 0.2757(4) 0.0399(16) Uani 1 1 d . . . H41 H 0.7167 0.1160 0.2401 0.048 Uiso 1 1 calc R . . C42 C 0.7151(5) -0.0024(3) 0.2916(4) 0.0393(16) Uani 1 1 d . . . H42 H 0.7799 -0.0256 0.2701 0.047 Uiso 1 1 calc R . . C43 C 0.4586(4) -0.0079(3) 0.4149(4) 0.0377(15) Uani 1 1 d . . . H43A H 0.4237 0.0405 0.4403 0.057 Uiso 1 1 calc R . . H43B H 0.4641 -0.0520 0.4571 0.057 Uiso 1 1 calc R . . H43C H 0.4228 -0.0252 0.3824 0.057 Uiso 1 1 calc R . . C44 C 0.6394(4) -0.1284(3) 0.3804(4) 0.0347(15) Uani 1 1 d . . . H44A H 0.5908 -0.1352 0.4352 0.042 Uiso 1 1 calc R . . H44B H 0.7046 -0.1454 0.3859 0.042 Uiso 1 1 calc R . . C45 C 0.6192(4) -0.1825(3) 0.3268(4) 0.0301(14) Uani 1 1 d . . . C46 C 0.5343(4) -0.2229(3) 0.3542(4) 0.0405(16) Uani 1 1 d . . . H46 H 0.4884 -0.2151 0.4061 0.049 Uiso 1 1 calc R . . C47 C 0.5169(5) -0.2747(4) 0.3058(4) 0.0481(18) Uani 1 1 d . . . H47 H 0.4590 -0.3021 0.3238 0.058 Uiso 1 1 calc R . . C48 C 0.5843(5) -0.2853(4) 0.2320(4) 0.0436(17) Uani 1 1 d . . . C49 C 0.6679(4) -0.2459(3) 0.2029(4) 0.0387(16) Uani 1 1 d . . . H49 H 0.7129 -0.2535 0.1506 0.046 Uiso 1 1 calc R . . C50 C 0.6856(4) -0.1951(3) 0.2507(4) 0.0343(15) Uani 1 1 d . . . H50 H 0.7439 -0.1683 0.2317 0.041 Uiso 1 1 calc R . . C51 C 0.5657(4) 0.3530(3) 0.3800(3) 0.0306(14) Uani 1 1 d . . . C52 C 0.6077(4) 0.3487(4) 0.4414(4) 0.0406(16) Uani 1 1 d . . . H52 H 0.6240 0.2972 0.4671 0.049 Uiso 1 1 calc R . . C53 C 0.6257(5) 0.4200(4) 0.4654(4) 0.0526(19) Uani 1 1 d . . . H53 H 0.6527 0.4164 0.5084 0.063 Uiso 1 1 calc R . . C54 C 0.6053(5) 0.4944(4) 0.4282(4) 0.054(2) Uani 1 1 d . . . H54 H 0.6198 0.5422 0.4441 0.064 Uiso 1 1 calc R . . C55 C 0.5638(5) 0.5002(4) 0.3676(4) 0.0480(18) Uani 1 1 d . . . H55 H 0.5487 0.5522 0.3420 0.058 Uiso 1 1 calc R . . C56 C 0.5437(4) 0.4301(3) 0.3432(4) 0.0373(16) Uani 1 1 d . . . H56 H 0.5147 0.4347 0.3014 0.045 Uiso 1 1 calc R . . C57 C 0.5219(4) 0.0893(3) 0.1518(3) 0.0279(13) Uani 1 1 d . . . C58 C 0.4339(4) 0.0648(3) 0.2050(4) 0.0393(16) Uani 1 1 d . . . H58 H 0.3857 0.1041 0.2322 0.047 Uiso 1 1 calc R . . C59 C 0.4154(5) -0.0172(4) 0.2190(4) 0.0453(17) Uani 1 1 d . . . H59 H 0.3546 -0.0338 0.2548 0.054 Uiso 1 1 calc R . . C60 C 0.4869(6) -0.0740(4) 0.1800(4) 0.0517(19) Uani 1 1 d . . . H60 H 0.4753 -0.1300 0.1891 0.062 Uiso 1 1 calc R . . C61 C 0.5740(5) -0.0498(4) 0.1286(4) 0.0523(19) Uani 1 1 d . . . H61 H 0.6227 -0.0893 0.1026 0.063 Uiso 1 1 calc R . . C62 C 0.5923(4) 0.0317(3) 0.1137(4) 0.0372(15) Uani 1 1 d . . . H62 H 0.6531 0.0478 0.0775 0.045 Uiso 1 1 calc R . . C63 C 0.4348(4) 0.2395(3) 0.1017(3) 0.0311(14) Uani 1 1 d . . . C64 C 0.3872(4) 0.3146(3) 0.1235(4) 0.0351(15) Uani 1 1 d . . . H64 H 0.4075 0.3433 0.1574 0.042 Uiso 1 1 calc R . . C65 C 0.3101(4) 0.3476(4) 0.0959(4) 0.0429(17) Uani 1 1 d . . . H65 H 0.2785 0.3991 0.1108 0.051 Uiso 1 1 calc R . . C66 C 0.2787(5) 0.3071(4) 0.0472(4) 0.0496(18) Uani 1 1 d . . . H66 H 0.2261 0.3302 0.0283 0.059 Uiso 1 1 calc R . . C67 C 0.3255(5) 0.2316(4) 0.0263(4) 0.0441(17) Uani 1 1 d . . . H67 H 0.3048 0.2028 -0.0072 0.053 Uiso 1 1 calc R . . C68 C 0.4012(4) 0.1987(4) 0.0536(4) 0.0372(15) Uani 1 1 d . . . H68 H 0.4315 0.1466 0.0394 0.045 Uiso 1 1 calc R . . C69 C 0.6461(4) 0.2074(3) 0.0440(3) 0.0289(13) Uani 1 1 d . . . C70 C 0.6428(5) 0.2058(4) -0.0340(4) 0.0425(16) Uani 1 1 d . . . H70 H 0.5830 0.1997 -0.0423 0.051 Uiso 1 1 calc R . . C71 C 0.7271(5) 0.2133(4) -0.1000(4) 0.0464(17) Uani 1 1 d . . . H71 H 0.7245 0.2123 -0.1533 0.056 Uiso 1 1 calc R . . C72 C 0.8142(5) 0.2221(3) -0.0891(4) 0.0426(17) Uani 1 1 d . . . H72 H 0.8716 0.2267 -0.1346 0.051 Uiso 1 1 calc R . . C73 C 0.8179(4) 0.2240(3) -0.0127(4) 0.0373(16) Uani 1 1 d . . . H73 H 0.8781 0.2299 -0.0051 0.045 Uiso 1 1 calc R . . C74 C 0.7342(4) 0.2174(3) 0.0544(4) 0.0339(15) Uani 1 1 d . . . H74 H 0.7373 0.2196 0.1073 0.041 Uiso 1 1 calc R . . C75 C 0.3526(6) 0.5443(5) 0.1984(4) 0.075(2) Uani 1 1 d . . . H75A H 0.3634 0.5900 0.2230 0.113 Uiso 1 1 calc R . . H75B H 0.3984 0.4976 0.2052 0.113 Uiso 1 1 calc R . . H75C H 0.2858 0.5293 0.2250 0.113 Uiso 1 1 calc R . . C76 C 0.4648(4) 0.5879(4) 0.0621(4) 0.0481(18) Uani 1 1 d . . . H76A H 0.4673 0.5960 0.0050 0.072 Uiso 1 1 calc R . . H76B H 0.5126 0.5433 0.0699 0.072 Uiso 1 1 calc R . . H76C H 0.4799 0.6380 0.0771 0.072 Uiso 1 1 calc R . . C77 C 0.2957(5) 0.5736(4) 0.0811(4) 0.0410(16) Uani 1 1 d . . . H77 H 0.3100 0.5911 0.0247 0.049 Uiso 1 1 calc R . . C78 C 0.8261(10) 0.8163(7) 0.6680(7) 0.180(6) Uani 1 1 d . . . H78A H 0.8294 0.8680 0.6872 0.270 Uiso 1 1 calc R . . H78B H 0.8689 0.7739 0.6873 0.270 Uiso 1 1 calc R . . H78C H 0.7590 0.8009 0.6892 0.270 Uiso 1 1 calc R . . C79 C 0.9624(7) 0.8060(7) 0.5340(7) 0.137(5) Uani 1 1 d . . . H79A H 0.9815 0.7493 0.5506 0.205 Uiso 1 1 calc R . . H79B H 1.0018 0.8422 0.5471 0.205 Uiso 1 1 calc R . . H79C H 0.9731 0.8135 0.4753 0.205 Uiso 1 1 calc R . . C80 C 0.7967(7) 0.8478(5) 0.5361(6) 0.076(3) Uani 1 1 d . . . H80 H 0.8204 0.8522 0.4783 0.091 Uiso 1 1 calc R . . C81 C 0.1710(13) 0.9405(8) 0.4344(8) 0.185(7) Uani 1 1 d . . . H81A H 0.1055 0.9269 0.4705 0.222 Uiso 1 1 calc R . . H81B H 0.1766 0.9983 0.4384 0.222 Uiso 1 1 calc R . . C82 C 0.2407(8) 0.8923(9) 0.4647(7) 0.187(8) Uani 1 1 d . . . H82A H 0.2167 0.8390 0.4885 0.280 Uiso 1 1 calc R . . H82B H 0.2521 0.9193 0.5064 0.280 Uiso 1 1 calc R . . H82C H 0.3018 0.8851 0.4202 0.280 Uiso 1 1 calc R . . C83 C 0.1036(9) 0.9673(7) 0.3228(8) 0.132(4) Uani 1 1 d . . . H83A H 0.0900 1.0255 0.3321 0.159 Uiso 1 1 calc R . . H83B H 0.0436 0.9400 0.3528 0.159 Uiso 1 1 calc R . . C84 C 0.1254(7) 0.9617(6) 0.2368(6) 0.101(3) Uani 1 1 d . . . H84A H 0.1766 0.9975 0.2055 0.152 Uiso 1 1 calc R . . H84B H 0.0667 0.9786 0.2212 0.152 Uiso 1 1 calc R . . H84C H 0.1477 0.9054 0.2255 0.152 Uiso 1 1 calc R . . Cl1 Cl 0.90140(11) 0.83228(9) 0.30922(10) 0.0394(4) Uani 1 1 d . . . Cl2 Cl 0.59156(10) 0.38060(8) 0.15148(8) 0.0324(3) Uani 1 1 d . . . F1 F 0.9011(3) 0.0992(2) 0.3309(3) 0.0742(13) Uani 1 1 d . . . F2 F 0.5672(3) -0.3368(2) 0.1852(3) 0.0670(12) Uani 1 1 d . . . N1 N 0.9086(3) 0.5607(3) 0.1690(3) 0.0346(12) Uani 1 1 d . . . N2 N 0.8608(4) 0.4525(3) 0.1448(3) 0.0372(13) Uani 1 1 d . . . N3 N 0.9328(3) 0.7661(3) 0.1200(3) 0.0287(11) Uani 1 1 d . . . N4 N 0.5820(3) 0.0828(3) 0.3197(3) 0.0307(12) Uani 1 1 d . . . N5 N 0.6355(4) -0.0414(3) 0.3469(3) 0.0374(13) Uani 1 1 d . . . N6 N 0.5460(3) 0.2858(3) 0.3502(3) 0.0279(11) Uani 1 1 d . . . N7 N 0.3676(4) 0.5678(3) 0.1133(3) 0.0409(13) Uani 1 1 d . . . N8 N 0.8581(6) 0.8257(5) 0.5779(5) 0.094(2) Uani 1 1 d . . . O1 O 0.9227(3) 0.6767(2) 0.0316(2) 0.0432(11) Uani 1 1 d . . . O2 O 0.5597(3) 0.1786(2) 0.4506(2) 0.0420(11) Uani 1 1 d . . . O3 O 0.2113(3) 0.5575(3) 0.1203(3) 0.0511(12) Uani 1 1 d . . . O4 O 0.7099(5) 0.8625(4) 0.5705(5) 0.123(3) Uani 1 1 d . . . O5 O 0.1765(5) 0.9334(4) 0.3549(4) 0.098(2) Uani 1 1 d . . . P1 P 0.95467(11) 0.63338(9) 0.34263(9) 0.0307(4) Uani 1 1 d . . . P2 P 0.53944(11) 0.19734(9) 0.13425(9) 0.0288(4) Uani 1 1 d . . . Pd1 Pd 0.93372(3) 0.71554(3) 0.23602(3) 0.02792(13) Uani 1 1 d . . . Pd2 Pd 0.55143(3) 0.25564(2) 0.23769(3) 0.02663(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(4) 0.029(3) 0.038(4) -0.003(3) 0.002(3) -0.002(3) C2 0.037(4) 0.029(3) 0.035(4) -0.001(3) -0.012(3) -0.007(3) C3 0.033(4) 0.043(4) 0.032(4) 0.003(3) -0.008(3) -0.008(3) C4 0.028(4) 0.034(4) 0.048(4) -0.003(3) -0.007(3) 0.003(3) C5 0.035(4) 0.045(4) 0.042(4) -0.003(3) -0.004(3) -0.004(3) C6 0.028(4) 0.049(4) 0.037(4) -0.001(3) -0.006(3) 0.006(3) C7 0.035(4) 0.033(3) 0.041(4) -0.002(3) -0.015(3) -0.004(3) C8 0.028(4) 0.033(3) 0.038(4) -0.008(3) -0.005(3) -0.007(3) C9 0.022(3) 0.032(3) 0.048(4) -0.009(3) -0.005(3) -0.004(3) C10 0.039(4) 0.038(4) 0.050(4) -0.002(3) -0.002(3) -0.012(3) C11 0.051(5) 0.042(4) 0.057(5) 0.006(4) -0.021(4) 0.000(4) C12 0.050(5) 0.039(4) 0.059(5) -0.007(4) -0.005(4) 0.015(3) C13 0.037(4) 0.037(4) 0.043(4) -0.011(3) 0.001(3) 0.004(3) C14 0.011(3) 0.028(3) 0.036(4) 0.003(3) 0.004(3) 0.000(2) C15 0.028(4) 0.031(3) 0.031(3) 0.000(3) -0.008(3) 0.003(3) C16 0.024(4) 0.050(4) 0.050(4) 0.005(3) -0.011(3) 0.009(3) C17 0.043(4) 0.024(3) 0.060(5) 0.008(3) -0.005(4) 0.002(3) C18 0.041(4) 0.035(4) 0.058(5) -0.006(3) 0.001(4) -0.012(3) C19 0.038(4) 0.029(3) 0.038(4) 0.003(3) -0.007(3) -0.011(3) C20 0.029(4) 0.039(4) 0.035(4) 0.002(3) -0.002(3) -0.002(3) C21 0.034(4) 0.047(4) 0.037(4) -0.007(3) -0.009(3) 0.007(3) C22 0.051(5) 0.034(4) 0.044(4) -0.008(3) -0.014(4) 0.000(3) C23 0.036(4) 0.045(4) 0.050(4) -0.006(3) -0.002(3) -0.011(3) C24 0.028(4) 0.037(4) 0.043(4) -0.003(3) -0.002(3) -0.008(3) C25 0.024(3) 0.036(3) 0.027(3) 0.001(3) -0.010(3) -0.001(3) C26 0.025(4) 0.029(3) 0.029(3) 0.002(3) -0.004(3) 0.000(3) C27 0.031(4) 0.037(3) 0.034(4) 0.004(3) -0.013(3) -0.005(3) C28 0.024(4) 0.039(4) 0.038(4) 0.001(3) -0.007(3) -0.003(3) C29 0.030(4) 0.060(5) 0.045(4) -0.009(3) 0.001(3) 0.009(3) C30 0.047(5) 0.081(5) 0.034(4) -0.005(4) -0.005(4) 0.005(4) C31 0.039(4) 0.049(4) 0.042(4) -0.004(3) -0.012(3) 0.005(3) C32 0.028(4) 0.040(4) 0.036(4) 0.001(3) -0.010(3) -0.007(3) C33 0.032(4) 0.064(5) 0.048(4) 0.011(4) -0.017(3) -0.020(3) C34 0.043(5) 0.088(6) 0.061(5) 0.025(4) -0.029(4) -0.028(4) C35 0.039(5) 0.117(7) 0.063(5) 0.030(5) -0.032(4) -0.036(5) C36 0.045(5) 0.081(6) 0.062(5) 0.024(4) -0.029(4) -0.033(4) C37 0.039(4) 0.061(5) 0.051(4) 0.013(4) -0.022(4) -0.018(4) C38 0.036(4) 0.028(3) 0.029(3) -0.004(3) -0.005(3) 0.005(3) C39 0.032(4) 0.022(3) 0.035(3) 0.000(3) -0.003(3) -0.006(3) C40 0.039(4) 0.029(3) 0.034(4) 0.000(3) -0.010(3) -0.006(3) C41 0.029(4) 0.034(4) 0.049(4) -0.002(3) -0.002(3) -0.007(3) C42 0.034(4) 0.033(4) 0.042(4) -0.008(3) 0.000(3) 0.001(3) C43 0.031(4) 0.035(3) 0.040(4) 0.005(3) -0.005(3) -0.002(3) C44 0.036(4) 0.025(3) 0.040(4) 0.004(3) -0.012(3) 0.003(3) C45 0.028(4) 0.019(3) 0.039(4) 0.007(3) -0.008(3) -0.003(2) C46 0.038(4) 0.029(3) 0.044(4) 0.003(3) -0.001(3) -0.005(3) C47 0.032(4) 0.041(4) 0.064(5) -0.004(3) -0.003(4) -0.011(3) C48 0.049(5) 0.031(4) 0.057(5) -0.007(3) -0.022(4) -0.005(3) C49 0.035(4) 0.033(4) 0.043(4) 0.000(3) -0.010(3) 0.007(3) C50 0.035(4) 0.029(3) 0.039(4) 0.001(3) -0.013(3) -0.001(3) C51 0.028(4) 0.028(3) 0.025(3) 0.003(3) 0.003(3) -0.001(3) C52 0.029(4) 0.045(4) 0.042(4) -0.005(3) -0.006(3) 0.002(3) C53 0.047(5) 0.057(5) 0.059(5) -0.017(4) -0.019(4) -0.006(4) C54 0.037(4) 0.052(5) 0.063(5) -0.019(4) 0.005(4) -0.017(4) C55 0.053(5) 0.039(4) 0.040(4) -0.001(3) 0.001(4) -0.009(3) C56 0.042(4) 0.030(3) 0.034(4) -0.006(3) -0.001(3) -0.006(3) C57 0.020(3) 0.023(3) 0.039(4) 0.003(3) -0.010(3) -0.001(2) C58 0.036(4) 0.027(3) 0.050(4) 0.001(3) -0.009(3) -0.007(3) C59 0.046(4) 0.035(4) 0.055(5) 0.008(3) -0.016(4) -0.019(3) C60 0.079(6) 0.026(4) 0.053(5) 0.001(3) -0.027(4) -0.007(4) C61 0.062(5) 0.028(4) 0.057(5) -0.008(3) -0.007(4) 0.004(3) C62 0.038(4) 0.028(3) 0.040(4) -0.003(3) -0.008(3) -0.001(3) C63 0.027(4) 0.028(3) 0.034(3) 0.002(3) -0.005(3) -0.010(3) C64 0.021(3) 0.033(3) 0.046(4) -0.002(3) -0.003(3) -0.004(3) C65 0.026(4) 0.037(4) 0.060(5) -0.007(3) -0.006(3) -0.004(3) C66 0.025(4) 0.061(5) 0.062(5) -0.002(4) -0.020(4) 0.007(3) C67 0.034(4) 0.054(4) 0.048(4) -0.005(3) -0.019(3) -0.004(3) C68 0.026(4) 0.037(4) 0.047(4) -0.007(3) -0.009(3) 0.000(3) C69 0.028(4) 0.024(3) 0.030(3) -0.002(2) -0.004(3) -0.002(3) C70 0.032(4) 0.054(4) 0.037(4) -0.001(3) -0.005(3) -0.011(3) C71 0.036(4) 0.059(4) 0.039(4) -0.008(3) -0.003(3) -0.003(3) C72 0.036(4) 0.035(4) 0.041(4) -0.002(3) 0.010(3) -0.009(3) C73 0.019(3) 0.032(3) 0.052(4) -0.009(3) 0.002(3) -0.003(3) C74 0.028(4) 0.028(3) 0.041(4) -0.003(3) -0.003(3) -0.008(3) C75 0.066(6) 0.109(7) 0.041(5) 0.014(5) -0.010(4) -0.020(5) C76 0.030(4) 0.060(4) 0.051(4) -0.001(3) -0.009(3) -0.008(3) C77 0.043(5) 0.040(4) 0.034(4) 0.003(3) -0.006(3) -0.009(3) C78 0.234(16) 0.176(13) 0.091(10) -0.046(9) -0.027(10) 0.095(11) C79 0.071(8) 0.176(12) 0.172(12) -0.080(10) -0.036(8) 0.018(7) C80 0.051(6) 0.074(6) 0.098(8) -0.026(5) -0.015(6) 0.007(5) C81 0.32(2) 0.138(12) 0.103(11) -0.009(9) -0.101(14) 0.028(12) C82 0.123(11) 0.35(2) 0.105(10) 0.106(12) -0.065(9) -0.140(13) C83 0.155(13) 0.094(8) 0.148(12) -0.012(8) -0.066(11) 0.034(8) C84 0.095(8) 0.093(7) 0.118(9) 0.023(7) -0.050(7) -0.011(6) Cl1 0.0407(10) 0.0330(8) 0.0456(10) -0.0064(7) -0.0145(8) -0.0021(7) Cl2 0.0352(9) 0.0277(8) 0.0323(8) 0.0049(6) -0.0094(7) -0.0080(6) F1 0.082(3) 0.047(2) 0.078(3) 0.019(2) -0.018(3) 0.004(2) F2 0.071(3) 0.062(3) 0.078(3) -0.022(2) -0.026(3) -0.020(2) N1 0.030(3) 0.037(3) 0.033(3) -0.001(2) -0.007(2) -0.001(2) N2 0.042(3) 0.033(3) 0.038(3) -0.004(2) -0.013(3) -0.008(2) N3 0.030(3) 0.029(3) 0.026(3) 0.003(2) -0.007(2) -0.010(2) N4 0.029(3) 0.027(3) 0.031(3) 0.000(2) -0.003(2) -0.005(2) N5 0.038(3) 0.032(3) 0.038(3) -0.001(2) -0.011(3) 0.003(2) N6 0.032(3) 0.021(2) 0.026(3) 0.003(2) -0.003(2) -0.006(2) N7 0.034(3) 0.046(3) 0.040(3) 0.004(3) -0.008(3) -0.008(3) N8 0.074(6) 0.108(6) 0.107(7) -0.035(5) -0.040(6) 0.020(5) O1 0.065(3) 0.033(2) 0.033(3) -0.0034(19) -0.016(2) -0.007(2) O2 0.061(3) 0.031(2) 0.030(2) 0.0037(19) -0.014(2) 0.001(2) O3 0.030(3) 0.053(3) 0.059(3) 0.003(2) 0.000(2) -0.010(2) O4 0.070(5) 0.073(4) 0.203(8) -0.034(5) -0.009(5) 0.009(4) O5 0.072(5) 0.123(6) 0.095(5) 0.016(4) -0.026(4) -0.025(4) P1 0.0224(9) 0.0352(9) 0.0329(9) 0.0004(7) -0.0077(7) -0.0038(7) P2 0.0229(9) 0.0267(8) 0.0338(9) -0.0009(7) -0.0057(7) -0.0024(7) Pd1 0.0234(3) 0.0270(3) 0.0316(3) -0.0006(2) -0.0067(2) -0.0043(2) Pd2 0.0244(3) 0.0223(2) 0.0287(3) 0.00051(19) -0.0031(2) -0.00394(19) _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 C1 O1 1.229(7) . ? C1 N3 1.345(7) . ? C1 C2 1.538(8) . ? C1 Pd1 2.583(6) . ? C2 N1 1.482(7) . ? C2 Pd1 2.018(5) . ? C2 H2 1.0000 . ? C3 N2 1.326(7) . ? C3 N1 1.329(7) . ? C3 C6 1.472(8) . ? C4 C5 1.330(8) . ? C4 N1 1.399(7) . ? C4 H4 0.9500 . ? C5 N2 1.417(7) . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N2 1.470(6) . ? C7 C8 1.506(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.383(8) . ? C8 C9 1.383(7) . ? C9 C10 1.386(8) . ? C9 H9 0.9500 . ? C10 C11 1.372(9) . ? C10 H10 0.9500 . ? C11 C12 1.362(9) . ? C11 F1 1.368(7) . ? C12 C13 1.396(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.389(8) . ? C14 C19 1.401(7) . ? C14 N3 1.421(7) . ? C15 C16 1.387(7) . ? C15 H15 0.9500 . ? C16 C17 1.387(8) . ? C16 H16 0.9500 . ? C17 C18 1.355(9) . ? C17 H17 0.9500 . ? C18 C19 1.404(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.373(8) . ? C20 C25 1.380(7) . ? C20 H20 0.9500 . ? C21 C22 1.383(8) . ? C21 H21 0.9500 . ? C22 C23 1.389(8) . ? C22 H22 0.9500 . ? C23 C24 1.375(8) . ? C23 H23 0.9500 . ? C24 C25 1.385(7) . ? C24 H24 0.9500 . ? C25 P1 1.825(6) . ? C26 C27 1.376(7) . ? C26 C31 1.402(8) . ? C26 P1 1.815(6) . ? C27 C28 1.391(8) . ? C27 H27 0.9500 . ? C28 C29 1.354(8) . ? C28 H28 0.9500 . ? C29 C30 1.363(8) . ? C29 H29 0.9500 . ? C30 C31 1.402(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.386(8) . ? C32 C37 1.390(8) . ? C32 P1 1.820(6) . ? C33 C34 1.389(8) . ? C33 H33 0.9500 . ? C34 C35 1.410(9) . ? C34 H34 0.9500 . ? C35 C36 1.352(9) . ? C35 H35 0.9500 . ? C36 C37 1.383(8) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 O2 1.239(6) . ? C38 N6 1.338(7) . ? C38 C39 1.534(7) . ? C38 Pd2 2.581(6) . ? C39 N4 1.467(7) . ? C39 Pd2 2.036(5) . ? C39 H39 1.0000 . ? C40 N4 1.334(7) . ? C40 N5 1.338(7) . ? C40 C43 1.467(8) . ? C41 C42 1.339(8) . ? C41 N4 1.388(7) . ? C41 H41 0.9500 . ? C42 N5 1.406(7) . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N5 1.484(7) . ? C44 C45 1.508(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.392(8) . ? C45 C46 1.394(7) . ? C46 C47 1.394(8) . ? C46 H46 0.9500 . ? C47 C48 1.362(9) . ? C47 H47 0.9500 . ? C48 F2 1.366(6) . ? C48 C49 1.370(8) . ? C49 C50 1.373(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.393(8) . ? C51 C56 1.398(7) . ? C51 N6 1.400(6) . ? C52 C53 1.396(8) . ? C52 H52 0.9500 . ? C53 C54 1.359(9) . ? C53 H53 0.9500 . ? C54 C55 1.373(9) . ? C54 H54 0.9500 . ? C55 C56 1.394(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.382(7) . ? C57 C58 1.386(7) . ? C57 P2 1.816(5) . ? C58 C59 1.396(7) . ? C58 H58 0.9500 . ? C59 C60 1.386(9) . ? C59 H59 0.9500 . ? C60 C61 1.364(9) . ? C60 H60 0.9500 . ? C61 C62 1.386(8) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.392(7) . ? C63 C68 1.392(7) . ? C63 P2 1.826(6) . ? C64 C65 1.388(8) . ? C64 H64 0.9500 . ? C65 C66 1.377(8) . ? C65 H65 0.9500 . ? C66 C67 1.390(8) . ? C66 H66 0.9500 . ? C67 C68 1.366(8) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.387(8) . ? C69 C74 1.390(7) . ? C69 P2 1.822(6) . ? C70 C71 1.388(8) . ? C70 H70 0.9500 . ? C71 C72 1.375(8) . ? C71 H71 0.9500 . ? C72 C73 1.363(8) . ? C72 H72 0.9500 . ? C73 C74 1.392(7) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 N7 1.435(8) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 N7 1.457(7) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 O3 1.239(7) . ? C77 N7 1.335(7) . ? C77 H77 0.9500 . ? C78 N8 1.483(12) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 N8 1.482(11) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 O4 1.222(9) . ? C80 N8 1.320(10) . ? C80 H80 0.9500 . ? C81 O5 1.391(12) . ? C81 C82 1.409(15) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 O5 1.385(11) . ? C83 C84 1.448(13) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? Cl1 Pd1 2.3960(15) . ? Cl2 Pd2 2.4010(14) . ? N3 Pd1 2.088(4) . ? N6 Pd2 2.078(4) . ? P1 Pd1 2.2317(16) . ? P2 Pd2 2.2408(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 O1 C1 N3 131.5(6) . . ? O1 C1 C2 124.9(5) . . ? N3 C1 C2 103.5(5) . . ? O1 C1 Pd1 166.7(4) . . ? N3 C1 Pd1 53.6(3) . . ? C2 C1 Pd1 51.3(3) . . ? N1 C2 C1 107.6(5) . . ? N1 C2 Pd1 123.4(4) . . ? C1 C2 Pd1 92.1(3) . . ? N1 C2 H2 110.6 . . ? C1 C2 H2 110.6 . . ? Pd1 C2 H2 110.6 . . ? N2 C3 N1 108.6(5) . . ? N2 C3 C6 124.7(6) . . ? N1 C3 C6 126.7(5) . . ? C5 C4 N1 107.5(5) . . ? C5 C4 H4 126.3 . . ? N1 C4 H4 126.3 . . ? C4 C5 N2 106.6(5) . . ? C4 C5 H5 126.7 . . ? N2 C5 H5 126.7 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 113.4(5) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C13 C8 C9 119.5(6) . . ? C13 C8 C7 119.8(6) . . ? C9 C8 C7 120.7(5) . . ? C8 C9 C10 120.6(6) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 118.1(6) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 F1 118.7(6) . . ? C12 C11 C10 123.2(7) . . ? F1 C11 C10 118.1(7) . . ? C11 C12 C13 118.0(6) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C8 C13 C12 120.5(6) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C19 118.1(5) . . ? C15 C14 N3 125.0(5) . . ? C19 C14 N3 116.8(5) . . ? C16 C15 C14 121.1(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 120.7(6) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 118.5(6) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C19 122.3(6) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C14 C19 C18 119.2(6) . . ? C14 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C21 C20 C25 120.9(6) . . ? C21 C20 H20 119.6 . . ? C25 C20 H20 119.6 . . ? C20 C21 C22 120.3(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.5(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 118.9(5) . . ? C20 C25 P1 119.7(4) . . ? C24 C25 P1 121.0(4) . . ? C27 C26 C31 118.0(5) . . ? C27 C26 P1 119.3(4) . . ? C31 C26 P1 122.7(5) . . ? C26 C27 C28 121.6(6) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C29 C28 C27 120.1(6) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.9(6) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 121.1(7) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C26 C31 C30 119.2(6) . . ? C26 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C33 C32 C37 118.8(6) . . ? C33 C32 P1 121.2(4) . . ? C37 C32 P1 120.0(5) . . ? C32 C33 C34 121.4(6) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 118.5(7) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 119.9(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.4(7) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C36 C37 C32 119.9(6) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? O2 C38 N6 132.0(5) . . ? O2 C38 C39 124.4(5) . . ? N6 C38 C39 103.6(5) . . ? O2 C38 Pd2 167.3(4) . . ? N6 C38 Pd2 53.2(3) . . ? C39 C38 Pd2 52.0(3) . . ? N4 C39 C38 110.7(5) . . ? N4 C39 Pd2 121.7(4) . . ? C38 C39 Pd2 91.5(3) . . ? N4 C39 H39 110.4 . . ? C38 C39 H39 110.4 . . ? Pd2 C39 H39 110.4 . . ? N4 C40 N5 107.8(5) . . ? N4 C40 C43 127.0(5) . . ? N5 C40 C43 125.2(5) . . ? C42 C41 N4 108.7(5) . . ? C42 C41 H41 125.7 . . ? N4 C41 H41 125.7 . . ? C41 C42 N5 105.5(5) . . ? C41 C42 H42 127.2 . . ? N5 C42 H42 127.2 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N5 C44 C45 111.8(5) . . ? N5 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? N5 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? C50 C45 C46 118.8(5) . . ? C50 C45 C44 121.2(5) . . ? C46 C45 C44 120.0(5) . . ? C47 C46 C45 120.1(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 118.8(6) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 F2 118.5(6) . . ? C47 C48 C49 122.6(6) . . ? F2 C48 C49 118.9(6) . . ? C48 C49 C50 118.7(6) . . ? C48 C49 H49 120.7 . . ? C50 C49 H49 120.7 . . ? C49 C50 C45 121.0(6) . . ? C49 C50 H50 119.5 . . ? C45 C50 H50 119.5 . . ? C52 C51 C56 118.1(6) . . ? C52 C51 N6 125.0(5) . . ? C56 C51 N6 116.9(5) . . ? C51 C52 C53 120.1(6) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 121.1(7) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C53 C54 C55 119.8(6) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 120.3(6) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C51 120.6(6) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? C62 C57 C58 119.4(5) . . ? C62 C57 P2 122.5(4) . . ? C58 C57 P2 118.1(4) . . ? C57 C58 C59 120.5(6) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C60 C59 C58 119.2(6) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C61 C60 C59 120.1(6) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C62 121.0(6) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C57 C62 C61 119.8(6) . . ? C57 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C68 118.0(6) . . ? C64 C63 P2 120.5(5) . . ? C68 C63 P2 121.5(4) . . ? C65 C64 C63 120.1(6) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C66 C65 C64 121.2(6) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C65 C66 C67 118.6(6) . . ? C65 C66 H66 120.7 . . ? C67 C66 H66 120.7 . . ? C68 C67 C66 120.5(6) . . ? C68 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C67 C68 C63 121.6(6) . . ? C67 C68 H68 119.2 . . ? C63 C68 H68 119.2 . . ? C70 C69 C74 119.0(5) . . ? C70 C69 P2 123.0(5) . . ? C74 C69 P2 118.1(4) . . ? C69 C70 C71 119.8(6) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C72 C71 C70 120.9(6) . . ? C72 C71 H71 119.6 . . ? C70 C71 H71 119.6 . . ? C73 C72 C71 119.6(6) . . ? C73 C72 H72 120.2 . . ? C71 C72 H72 120.2 . . ? C72 C73 C74 120.6(6) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C69 C74 C73 120.1(6) . . ? C69 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? N7 C75 H75A 109.5 . . ? N7 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N7 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N7 C76 H76A 109.5 . . ? N7 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N7 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O3 C77 N7 124.0(6) . . ? O3 C77 H77 118.0 . . ? N7 C77 H77 118.0 . . ? N8 C78 H78A 109.5 . . ? N8 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N8 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N8 C79 H79A 109.5 . . ? N8 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N8 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O4 C80 N8 121.0(10) . . ? O4 C80 H80 119.5 . . ? N8 C80 H80 119.5 . . ? O5 C81 C82 116.8(13) . . ? O5 C81 H81A 108.1 . . ? C82 C81 H81A 108.1 . . ? O5 C81 H81B 108.1 . . ? C82 C81 H81B 108.1 . . ? H81A C81 H81B 107.3 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O5 C83 C84 114.9(10) . . ? O5 C83 H83A 108.5 . . ? C84 C83 H83A 108.5 . . ? O5 C83 H83B 108.5 . . ? C84 C83 H83B 108.5 . . ? H83A C83 H83B 107.5 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C3 N1 C4 108.8(5) . . ? C3 N1 C2 126.8(5) . . ? C4 N1 C2 123.0(5) . . ? C3 N2 C5 108.5(5) . . ? C3 N2 C7 127.9(5) . . ? C5 N2 C7 123.6(5) . . ? C1 N3 C14 124.0(5) . . ? C1 N3 Pd1 95.1(4) . . ? C14 N3 Pd1 138.2(4) . . ? C40 N4 C41 108.5(5) . . ? C40 N4 C39 126.5(5) . . ? C41 N4 C39 124.3(4) . . ? C40 N5 C42 109.4(5) . . ? C40 N5 C44 125.9(5) . . ? C42 N5 C44 124.7(5) . . ? C38 N6 C51 125.4(5) . . ? C38 N6 Pd2 95.7(3) . . ? C51 N6 Pd2 136.4(3) . . ? C77 N7 C75 122.2(6) . . ? C77 N7 C76 120.0(5) . . ? C75 N7 C76 117.8(6) . . ? C80 N8 C79 119.4(9) . . ? C80 N8 C78 122.5(9) . . ? C79 N8 C78 118.0(9) . . ? C83 O5 C81 122.0(10) . . ? C26 P1 C32 106.9(3) . . ? C26 P1 C25 103.2(2) . . ? C32 P1 C25 103.0(3) . . ? C26 P1 Pd1 113.9(2) . . ? C32 P1 Pd1 112.6(2) . . ? C25 P1 Pd1 116.15(19) . . ? C57 P2 C69 104.6(2) . . ? C57 P2 C63 101.3(2) . . ? C69 P2 C63 106.1(3) . . ? C57 P2 Pd2 117.3(2) . . ? C69 P2 Pd2 112.75(19) . . ? C63 P2 Pd2 113.48(19) . . ? C2 Pd1 N3 67.0(2) . . ? C2 Pd1 P1 98.30(17) . . ? N3 Pd1 P1 164.86(13) . . ? C2 Pd1 Cl1 169.70(16) . . ? N3 Pd1 Cl1 103.02(13) . . ? P1 Pd1 Cl1 91.48(6) . . ? C2 Pd1 C1 36.51(19) . . ? N3 Pd1 C1 31.26(16) . . ? P1 Pd1 C1 134.60(13) . . ? Cl1 Pd1 C1 133.90(13) . . ? C39 Pd2 N6 66.63(19) . . ? C39 Pd2 P2 100.14(16) . . ? N6 Pd2 P2 166.29(12) . . ? C39 Pd2 Cl2 168.74(16) . . ? N6 Pd2 Cl2 102.24(12) . . ? P2 Pd2 Cl2 91.07(5) . . ? C39 Pd2 C38 36.44(19) . . ? N6 Pd2 C38 31.05(15) . . ? P2 Pd2 C38 136.33(13) . . ? Cl2 Pd2 C38 132.31(13) . . ? 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 O1 C1 C2 N1 -37.9(8) . . . . ? N3 C1 C2 N1 139.6(5) . . . . ? Pd1 C1 C2 N1 126.1(5) . . . . ? O1 C1 C2 Pd1 -164.0(5) . . . . ? N3 C1 C2 Pd1 13.4(4) . . . . ? N1 C4 C5 N2 1.1(7) . . . . ? N2 C7 C8 C13 -116.7(6) . . . . ? N2 C7 C8 C9 65.4(7) . . . . ? C13 C8 C9 C10 1.2(9) . . . . ? C7 C8 C9 C10 179.1(5) . . . . ? C8 C9 C10 C11 -1.2(9) . . . . ? C9 C10 C11 C12 1.5(11) . . . . ? C9 C10 C11 F1 179.3(5) . . . . ? F1 C11 C12 C13 -179.4(6) . . . . ? C10 C11 C12 C13 -1.6(11) . . . . ? C9 C8 C13 C12 -1.4(9) . . . . ? C7 C8 C13 C12 -179.3(6) . . . . ? C11 C12 C13 C8 1.5(10) . . . . ? C19 C14 C15 C16 -1.1(8) . . . . ? N3 C14 C15 C16 179.2(5) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C15 C16 C17 C18 0.5(9) . . . . ? C16 C17 C18 C19 -1.3(10) . . . . ? C15 C14 C19 C18 0.4(8) . . . . ? N3 C14 C19 C18 -179.9(5) . . . . ? C17 C18 C19 C14 0.8(9) . . . . ? C25 C20 C21 C22 1.2(9) . . . . ? C20 C21 C22 C23 0.4(10) . . . . ? C21 C22 C23 C24 -0.6(10) . . . . ? C22 C23 C24 C25 -0.9(10) . . . . ? C21 C20 C25 C24 -2.7(9) . . . . ? C21 C20 C25 P1 -176.2(5) . . . . ? C23 C24 C25 C20 2.6(9) . . . . ? C23 C24 C25 P1 176.0(5) . . . . ? C31 C26 C27 C28 -1.9(8) . . . . ? P1 C26 C27 C28 175.9(4) . . . . ? C26 C27 C28 C29 0.2(9) . . . . ? C27 C28 C29 C30 1.2(10) . . . . ? C28 C29 C30 C31 -0.9(11) . . . . ? C27 C26 C31 C30 2.1(9) . . . . ? P1 C26 C31 C30 -175.6(5) . . . . ? C29 C30 C31 C26 -0.8(10) . . . . ? C37 C32 C33 C34 1.8(10) . . . . ? P1 C32 C33 C34 -179.6(5) . . . . ? C32 C33 C34 C35 0.4(11) . . . . ? C33 C34 C35 C36 -2.8(12) . . . . ? C34 C35 C36 C37 2.8(13) . . . . ? C35 C36 C37 C32 -0.5(11) . . . . ? C33 C32 C37 C36 -1.8(10) . . . . ? P1 C32 C37 C36 179.6(5) . . . . ? O2 C38 C39 N4 -40.0(8) . . . . ? N6 C38 C39 N4 139.1(5) . . . . ? Pd2 C38 C39 N4 124.9(5) . . . . ? O2 C38 C39 Pd2 -164.9(5) . . . . ? N6 C38 C39 Pd2 14.2(4) . . . . ? N4 C41 C42 N5 0.0(7) . . . . ? N5 C44 C45 C50 69.6(7) . . . . ? N5 C44 C45 C46 -112.5(6) . . . . ? C50 C45 C46 C47 -0.2(9) . . . . ? C44 C45 C46 C47 -178.2(5) . . . . ? C45 C46 C47 C48 0.5(9) . . . . ? C46 C47 C48 F2 179.3(5) . . . . ? C46 C47 C48 C49 -1.2(10) . . . . ? C47 C48 C49 C50 1.6(10) . . . . ? F2 C48 C49 C50 -179.0(5) . . . . ? C48 C49 C50 C45 -1.2(9) . . . . ? C46 C45 C50 C49 0.6(8) . . . . ? C44 C45 C50 C49 178.5(5) . . . . ? C56 C51 C52 C53 0.6(9) . . . . ? N6 C51 C52 C53 178.8(5) . . . . ? C51 C52 C53 C54 -1.7(10) . . . . ? C52 C53 C54 C55 1.8(10) . . . . ? C53 C54 C55 C56 -0.9(10) . . . . ? C54 C55 C56 C51 -0.2(9) . . . . ? C52 C51 C56 C55 0.4(8) . . . . ? N6 C51 C56 C55 -178.0(5) . . . . ? C62 C57 C58 C59 -1.2(9) . . . . ? P2 C57 C58 C59 178.2(5) . . . . ? C57 C58 C59 C60 1.1(10) . . . . ? C58 C59 C60 C61 -0.1(10) . . . . ? C59 C60 C61 C62 -0.6(11) . . . . ? C58 C57 C62 C61 0.5(9) . . . . ? P2 C57 C62 C61 -178.9(5) . . . . ? C60 C61 C62 C57 0.4(10) . . . . ? C68 C63 C64 C65 -1.5(8) . . . . ? P2 C63 C64 C65 177.5(4) . . . . ? C63 C64 C65 C66 0.5(9) . . . . ? C64 C65 C66 C67 0.3(10) . . . . ? C65 C66 C67 C68 0.0(10) . . . . ? C66 C67 C68 C63 -1.0(9) . . . . ? C64 C63 C68 C67 1.8(9) . . . . ? P2 C63 C68 C67 -177.2(5) . . . . ? C74 C69 C70 C71 0.7(9) . . . . ? P2 C69 C70 C71 -179.5(5) . . . . ? C69 C70 C71 C72 0.1(9) . . . . ? C70 C71 C72 C73 -0.4(9) . . . . ? C71 C72 C73 C74 -0.2(9) . . . . ? C70 C69 C74 C73 -1.3(8) . . . . ? P2 C69 C74 C73 179.0(4) . . . . ? C72 C73 C74 C69 1.0(8) . . . . ? N2 C3 N1 C4 1.2(7) . . . . ? C6 C3 N1 C4 -179.7(6) . . . . ? N2 C3 N1 C2 -165.2(5) . . . . ? C6 C3 N1 C2 13.9(10) . . . . ? C5 C4 N1 C3 -1.5(7) . . . . ? C5 C4 N1 C2 165.6(5) . . . . ? C1 C2 N1 C3 95.1(7) . . . . ? Pd1 C2 N1 C3 -160.0(5) . . . . ? C1 C2 N1 C4 -69.5(7) . . . . ? Pd1 C2 N1 C4 35.3(7) . . . . ? N1 C3 N2 C5 -0.6(7) . . . . ? C6 C3 N2 C5 -179.6(6) . . . . ? N1 C3 N2 C7 179.1(5) . . . . ? C6 C3 N2 C7 0.0(10) . . . . ? C4 C5 N2 C3 -0.4(7) . . . . ? C4 C5 N2 C7 180.0(5) . . . . ? C8 C7 N2 C3 89.7(7) . . . . ? C8 C7 N2 C5 -90.7(7) . . . . ? O1 C1 N3 C14 0.0(10) . . . . ? C2 C1 N3 C14 -177.2(5) . . . . ? Pd1 C1 N3 C14 -164.2(6) . . . . ? O1 C1 N3 Pd1 164.2(6) . . . . ? C2 C1 N3 Pd1 -13.0(4) . . . . ? C15 C14 N3 C1 10.5(8) . . . . ? C19 C14 N3 C1 -169.2(5) . . . . ? C15 C14 N3 Pd1 -145.5(5) . . . . ? C19 C14 N3 Pd1 34.8(8) . . . . ? N5 C40 N4 C41 0.9(7) . . . . ? C43 C40 N4 C41 -178.0(6) . . . . ? N5 C40 N4 C39 -169.8(5) . . . . ? C43 C40 N4 C39 11.2(10) . . . . ? C42 C41 N4 C40 -0.6(7) . . . . ? C42 C41 N4 C39 170.5(5) . . . . ? C38 C39 N4 C40 94.2(6) . . . . ? Pd2 C39 N4 C40 -160.4(5) . . . . ? C38 C39 N4 C41 -75.2(7) . . . . ? Pd2 C39 N4 C41 30.2(8) . . . . ? N4 C40 N5 C42 -0.9(7) . . . . ? C43 C40 N5 C42 178.0(6) . . . . ? N4 C40 N5 C44 -178.8(5) . . . . ? C43 C40 N5 C44 0.1(10) . . . . ? C41 C42 N5 C40 0.6(7) . . . . ? C41 C42 N5 C44 178.5(5) . . . . ? C45 C44 N5 C40 89.3(7) . . . . ? C45 C44 N5 C42 -88.3(7) . . . . ? O2 C38 N6 C51 0.5(10) . . . . ? C39 C38 N6 C51 -178.5(5) . . . . ? Pd2 C38 N6 C51 -164.6(6) . . . . ? O2 C38 N6 Pd2 165.1(6) . . . . ? C39 C38 N6 Pd2 -14.0(4) . . . . ? C52 C51 N6 C38 14.6(9) . . . . ? C56 C51 N6 C38 -167.1(5) . . . . ? C52 C51 N6 Pd2 -142.8(5) . . . . ? C56 C51 N6 Pd2 35.5(8) . . . . ? O3 C77 N7 C75 -1.9(10) . . . . ? O3 C77 N7 C76 179.8(6) . . . . ? O4 C80 N8 C79 178.2(8) . . . . ? O4 C80 N8 C78 0.9(14) . . . . ? C84 C83 O5 C81 173.7(10) . . . . ? C82 C81 O5 C83 169.5(11) . . . . ? C27 C26 P1 C32 153.4(4) . . . . ? C31 C26 P1 C32 -28.9(6) . . . . ? C27 C26 P1 C25 -98.4(5) . . . . ? C31 C26 P1 C25 79.3(5) . . . . ? C27 C26 P1 Pd1 28.4(5) . . . . ? C31 C26 P1 Pd1 -153.9(4) . . . . ? C33 C32 P1 C26 78.6(5) . . . . ? C37 C32 P1 C26 -102.8(5) . . . . ? C33 C32 P1 C25 -29.7(6) . . . . ? C37 C32 P1 C25 148.9(5) . . . . ? C33 C32 P1 Pd1 -155.6(5) . . . . ? C37 C32 P1 Pd1 23.0(6) . . . . ? C20 C25 P1 C26 -159.7(5) . . . . ? C24 C25 P1 C26 27.0(5) . . . . ? C20 C25 P1 C32 -48.6(5) . . . . ? C24 C25 P1 C32 138.0(5) . . . . ? C20 C25 P1 Pd1 75.0(5) . . . . ? C24 C25 P1 Pd1 -98.4(5) . . . . ? C62 C57 P2 C69 13.9(6) . . . . ? C58 C57 P2 C69 -165.5(5) . . . . ? C62 C57 P2 C63 124.0(5) . . . . ? C58 C57 P2 C63 -55.4(5) . . . . ? C62 C57 P2 Pd2 -111.9(5) . . . . ? C58 C57 P2 Pd2 68.7(5) . . . . ? C70 C69 P2 C57 77.0(5) . . . . ? C74 C69 P2 C57 -103.3(4) . . . . ? C70 C69 P2 C63 -29.6(5) . . . . ? C74 C69 P2 C63 150.1(4) . . . . ? C70 C69 P2 Pd2 -154.4(4) . . . . ? C74 C69 P2 Pd2 25.3(5) . . . . ? C64 C63 P2 C57 144.2(5) . . . . ? C68 C63 P2 C57 -36.9(5) . . . . ? C64 C63 P2 C69 -106.8(5) . . . . ? C68 C63 P2 C69 72.1(5) . . . . ? C64 C63 P2 Pd2 17.5(5) . . . . ? C68 C63 P2 Pd2 -163.5(4) . . . . ? N1 C2 Pd1 N3 -121.9(5) . . . . ? C1 C2 Pd1 N3 -9.1(3) . . . . ? N1 C2 Pd1 P1 61.9(5) . . . . ? C1 C2 Pd1 P1 174.7(3) . . . . ? N1 C2 Pd1 Cl1 -136.5(8) . . . . ? C1 C2 Pd1 Cl1 -23.8(12) . . . . ? N1 C2 Pd1 C1 -112.8(6) . . . . ? C1 N3 Pd1 C2 10.4(3) . . . . ? C14 N3 Pd1 C2 170.7(6) . . . . ? C1 N3 Pd1 P1 24.8(7) . . . . ? C14 N3 Pd1 P1 -175.0(4) . . . . ? C1 N3 Pd1 Cl1 -172.2(3) . . . . ? C14 N3 Pd1 Cl1 -12.0(5) . . . . ? C14 N3 Pd1 C1 160.2(7) . . . . ? C26 P1 Pd1 C2 -132.4(3) . . . . ? C32 P1 Pd1 C2 105.7(3) . . . . ? C25 P1 Pd1 C2 -12.7(3) . . . . ? C26 P1 Pd1 N3 -145.7(5) . . . . ? C32 P1 Pd1 N3 92.4(5) . . . . ? C25 P1 Pd1 N3 -26.1(5) . . . . ? C26 P1 Pd1 Cl1 50.8(2) . . . . ? C32 P1 Pd1 Cl1 -71.0(2) . . . . ? C25 P1 Pd1 Cl1 170.5(2) . . . . ? C26 P1 Pd1 C1 -127.9(3) . . . . ? C32 P1 Pd1 C1 110.2(3) . . . . ? C25 P1 Pd1 C1 -8.3(3) . . . . ? O1 C1 Pd1 C2 79(2) . . . . ? N3 C1 Pd1 C2 -163.7(5) . . . . ? O1 C1 Pd1 N3 -118(2) . . . . ? C2 C1 Pd1 N3 163.7(5) . . . . ? O1 C1 Pd1 P1 71(2) . . . . ? N3 C1 Pd1 P1 -171.1(3) . . . . ? C2 C1 Pd1 P1 -7.4(4) . . . . ? O1 C1 Pd1 Cl1 -107.2(19) . . . . ? N3 C1 Pd1 Cl1 10.5(4) . . . . ? C2 C1 Pd1 Cl1 174.3(3) . . . . ? N4 C39 Pd2 N6 -125.2(5) . . . . ? C38 C39 Pd2 N6 -9.6(3) . . . . ? N4 C39 Pd2 P2 58.6(4) . . . . ? C38 C39 Pd2 P2 174.2(3) . . . . ? N4 C39 Pd2 Cl2 -116.3(8) . . . . ? C38 C39 Pd2 Cl2 -0.7(11) . . . . ? N4 C39 Pd2 C38 -115.6(6) . . . . ? C38 N6 Pd2 C39 11.1(3) . . . . ? C51 N6 Pd2 C39 172.8(6) . . . . ? C38 N6 Pd2 P2 26.9(8) . . . . ? C51 N6 Pd2 P2 -171.4(4) . . . . ? C38 N6 Pd2 Cl2 -167.1(3) . . . . ? C51 N6 Pd2 Cl2 -5.4(5) . . . . ? C51 N6 Pd2 C38 161.7(7) . . . . ? C57 P2 Pd2 C39 -5.8(3) . . . . ? C69 P2 Pd2 C39 -127.5(3) . . . . ? C63 P2 Pd2 C39 111.9(3) . . . . ? C57 P2 Pd2 N6 -20.6(6) . . . . ? C69 P2 Pd2 N6 -142.2(6) . . . . ? C63 P2 Pd2 N6 97.1(6) . . . . ? C57 P2 Pd2 Cl2 173.2(2) . . . . ? C69 P2 Pd2 Cl2 51.5(2) . . . . ? C63 P2 Pd2 Cl2 -69.15(19) . . . . ? C57 P2 Pd2 C38 -0.8(3) . . . . ? C69 P2 Pd2 C38 -122.4(3) . . . . ? C63 P2 Pd2 C38 116.9(3) . . . . ? O2 C38 Pd2 C39 78(2) . . . . ? N6 C38 Pd2 C39 -162.7(5) . . . . ? O2 C38 Pd2 N6 -119(2) . . . . ? C39 C38 Pd2 N6 162.7(5) . . . . ? O2 C38 Pd2 P2 70(2) . . . . ? N6 C38 Pd2 P2 -171.1(3) . . . . ? C39 C38 Pd2 P2 -8.4(4) . . . . ? O2 C38 Pd2 Cl2 -102(2) . . . . ? N6 C38 Pd2 Cl2 17.1(4) . . . . ? C39 C38 Pd2 Cl2 179.8(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.639 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.112 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 5.grl034.cif' data_grl034 _database_code_depnum_ccdc_archive 'CCDC 850740' #TrackingRef '- 5.grl034.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C33 H27 Cl N4 O Pd, C H2 Cl2' _chemical_formula_sum 'C34 H29 Cl3 N4 O Pd' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 722.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8587(2) _cell_length_b 11.1511(3) _cell_length_c 15.0170(4) _cell_angle_alpha 80.665(2) _cell_angle_beta 89.264(2) _cell_angle_gamma 73.218(2) _cell_volume 1558.65(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2842 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 22.5 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.8425 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22102 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.75 _reflns_number_total 8024 _reflns_number_gt 5539 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0333P)^2^+8.9357P] 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 8024 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 C1 C 0.5233(8) 1.1462(8) 0.5647(6) 0.050(2) Uani 1 1 d . . . H1 H 0.4396 1.2004 0.5848 0.060 Uiso 1 1 calc R . . C2 C 0.5751(8) 1.1814(7) 0.4847(5) 0.0448(18) Uani 1 1 d . . . H2 H 0.5292 1.2616 0.4495 0.054 Uiso 1 1 calc R . . C3 C 0.6985(7) 1.0995(6) 0.4520(4) 0.0316(14) Uani 1 1 d . . . C4 C 0.7544(8) 1.1344(6) 0.3667(5) 0.0379(16) Uani 1 1 d . . . H4 H 0.7082 1.2133 0.3300 0.045 Uiso 1 1 calc R . . C5 C 0.8720(8) 1.0566(6) 0.3375(5) 0.0412(17) Uani 1 1 d . . . H5 H 0.9072 1.0807 0.2803 0.049 Uiso 1 1 calc R . . C6 C 0.9432(7) 0.9398(6) 0.3913(4) 0.0332(15) Uani 1 1 d . . . H6 H 1.0265 0.8866 0.3700 0.040 Uiso 1 1 calc R . . C7 C 0.8943(6) 0.9015(6) 0.4738(4) 0.0280(13) Uani 1 1 d . . . C8 C 0.7697(6) 0.9813(5) 0.5066(4) 0.0281(13) Uani 1 1 d . . . C9 C 0.7123(6) 0.9502(6) 0.5912(4) 0.0307(13) Uani 1 1 d . . . H9 H 0.7585 0.8726 0.6293 0.037 Uiso 1 1 calc R . . C10 C 0.5929(7) 1.0288(7) 0.6190(5) 0.0418(17) Uani 1 1 d . . . H10 H 0.5556 1.0047 0.6755 0.050 Uiso 1 1 calc R . . C11 C 0.9752(6) 0.7781(5) 0.5306(4) 0.0275(13) Uani 1 1 d . . . H11A H 1.0702 0.7480 0.5056 0.033 Uiso 1 1 calc R . . H11B H 0.9888 0.7930 0.5926 0.033 Uiso 1 1 calc R . . C12 C 0.8584(6) 0.6423(5) 0.4592(4) 0.0271(13) Uani 1 1 d . . . H12 H 0.8790 0.6694 0.3986 0.033 Uiso 1 1 calc R . . C13 C 0.7813(6) 0.5634(5) 0.4860(4) 0.0251(12) Uani 1 1 d . . . H13 H 0.7366 0.5245 0.4481 0.030 Uiso 1 1 calc R . . C14 C 0.8542(6) 0.6183(5) 0.6082(4) 0.0218(11) Uani 1 1 d . . . C15 C 0.8763(6) 0.6221(5) 0.7041(4) 0.0206(11) Uani 1 1 d . . . C16 C 1.0090(6) 0.6274(5) 0.7333(4) 0.0254(12) Uani 1 1 d . . . H16 H 1.0802 0.6314 0.6906 0.030 Uiso 1 1 calc R . . C17 C 1.0372(6) 0.6271(6) 0.8228(4) 0.0298(13) Uani 1 1 d . . . H17 H 1.1262 0.6326 0.8422 0.036 Uiso 1 1 calc R . . C18 C 0.9329(7) 0.6184(6) 0.8839(4) 0.0317(14) Uani 1 1 d . . . H18 H 0.9505 0.6182 0.9460 0.038 Uiso 1 1 calc R . . C19 C 0.8027(6) 0.6101(5) 0.8556(4) 0.0254(12) Uani 1 1 d . . . H19 H 0.7334 0.6038 0.8992 0.030 Uiso 1 1 calc R . . C20 C 0.7704(6) 0.6107(5) 0.7646(4) 0.0235(12) Uani 1 1 d . . . C21 C 0.4591(7) 0.7834(6) 0.8439(5) 0.0361(15) Uani 1 1 d . . . H21 H 0.5029 0.8320 0.8015 0.043 Uiso 1 1 calc R . . C22 C 0.3816(7) 0.8403(6) 0.9109(5) 0.0378(16) Uani 1 1 d . . . H22 H 0.3727 0.9266 0.9143 0.045 Uiso 1 1 calc R . . C23 C 0.3172(7) 0.7710(7) 0.9729(4) 0.0361(15) Uani 1 1 d . . . H23 H 0.2630 0.8084 1.0194 0.043 Uiso 1 1 calc R . . C24 C 0.3334(7) 0.6473(7) 0.9659(5) 0.0373(15) Uani 1 1 d . . . H24 H 0.2915 0.5968 1.0081 0.045 Uiso 1 1 calc R . . C25 C 0.4110(7) 0.5961(6) 0.8970(4) 0.0321(14) Uani 1 1 d . . . H25 H 0.4199 0.5103 0.8918 0.039 Uiso 1 1 calc R . . C26 C 0.6995(6) 0.4783(5) 0.6378(4) 0.0225(12) Uani 1 1 d . . . H26 H 0.6295 0.4585 0.5993 0.027 Uiso 1 1 calc R . . C27 C 0.7931(6) 0.3557(5) 0.6873(4) 0.0249(12) Uani 1 1 d . . . C28 C 0.9057(6) 0.1117(6) 0.8213(4) 0.0304(13) Uani 1 1 d . . . H28 H 0.9762 0.1498 0.7981 0.036 Uiso 1 1 calc R . . C29 C 0.7659(6) 0.1639(5) 0.7902(4) 0.0261(12) Uani 1 1 d . . . C30 C 0.6641(7) 0.1060(6) 0.8257(5) 0.0351(15) Uani 1 1 d . . . H30 H 0.5677 0.1423 0.8058 0.042 Uiso 1 1 calc R . . C31 C 0.7019(8) -0.0028(7) 0.8889(5) 0.0448(18) Uani 1 1 d . . . H31 H 0.6318 -0.0418 0.9116 0.054 Uiso 1 1 calc R . . C32 C 0.8417(9) -0.0560(6) 0.9198(5) 0.0431(17) Uani 1 1 d . . . H32 H 0.8684 -0.1317 0.9631 0.052 Uiso 1 1 calc R . . C33 C 0.9418(7) 0.0033(6) 0.8865(5) 0.0377(15) Uani 1 1 d . . . H33 H 1.0372 -0.0310 0.9087 0.045 Uiso 1 1 calc R . . C34 C 0.2093(7) 0.3013(7) 0.8167(5) 0.0427(17) Uani 1 1 d . . . H34A H 0.2288 0.3716 0.7742 0.051 Uiso 1 1 calc R . . H34B H 0.1057 0.3231 0.8249 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.39190(14) 0.49976(14) 0.69963(11) 0.0297(3) Uani 1 1 d . . . Cl2 Cl 0.2967(2) 0.2850(2) 0.92101(13) 0.0549(5) Uani 1 1 d . . . Cl3 Cl 0.26593(18) 0.15887(17) 0.77026(13) 0.0443(4) Uani 1 1 d . . . N1 N 0.9030(5) 0.6773(4) 0.5347(3) 0.0223(10) Uani 1 1 d . . . N2 N 0.7784(5) 0.5487(4) 0.5795(3) 0.0209(10) Uani 1 1 d . . . N3 N 0.4744(5) 0.6635(4) 0.8367(3) 0.0248(10) Uani 1 1 d . . . N4 N 0.7179(5) 0.2751(5) 0.7262(3) 0.0260(11) Uani 1 1 d . . . H4A H 0.6282 0.2960 0.7085 0.031 Uiso 1 1 calc R . . O1 O 0.9219(4) 0.3305(4) 0.6951(3) 0.0294(9) Uani 1 1 d . . . Pd1 Pd 0.59124(5) 0.57220(4) 0.73428(3) 0.02178(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(4) 0.052(5) 0.057(5) -0.016(4) 0.009(4) -0.004(4) C2 0.041(4) 0.035(4) 0.053(5) -0.010(3) -0.010(3) -0.001(3) C3 0.034(3) 0.026(3) 0.036(4) -0.007(3) -0.010(3) -0.009(3) C4 0.059(5) 0.023(3) 0.032(4) -0.004(3) -0.007(3) -0.011(3) C5 0.067(5) 0.034(4) 0.029(4) -0.008(3) 0.006(3) -0.024(4) C6 0.047(4) 0.025(3) 0.032(4) -0.011(3) 0.013(3) -0.015(3) C7 0.031(3) 0.029(3) 0.030(3) -0.010(3) 0.006(3) -0.015(3) C8 0.029(3) 0.026(3) 0.033(3) -0.010(3) -0.001(3) -0.011(2) C9 0.030(3) 0.032(3) 0.029(3) -0.006(3) 0.002(3) -0.007(3) C10 0.034(4) 0.042(4) 0.047(4) -0.014(3) 0.012(3) -0.004(3) C11 0.021(3) 0.027(3) 0.036(4) -0.008(3) 0.003(2) -0.009(2) C12 0.028(3) 0.027(3) 0.024(3) -0.007(2) 0.005(2) -0.004(2) C13 0.022(3) 0.030(3) 0.021(3) -0.008(2) -0.002(2) -0.002(2) C14 0.019(3) 0.019(3) 0.025(3) -0.005(2) 0.003(2) -0.002(2) C15 0.022(3) 0.022(3) 0.019(3) -0.002(2) -0.003(2) -0.009(2) C16 0.020(3) 0.028(3) 0.030(3) -0.005(2) 0.003(2) -0.010(2) C17 0.022(3) 0.036(3) 0.034(4) -0.010(3) -0.007(3) -0.009(3) C18 0.035(3) 0.036(3) 0.027(3) -0.009(3) -0.004(3) -0.013(3) C19 0.025(3) 0.032(3) 0.022(3) -0.005(2) -0.001(2) -0.012(2) C20 0.022(3) 0.023(3) 0.025(3) -0.009(2) -0.003(2) -0.004(2) C21 0.041(4) 0.038(4) 0.035(4) -0.016(3) 0.005(3) -0.016(3) C22 0.049(4) 0.032(3) 0.036(4) -0.011(3) 0.004(3) -0.013(3) C23 0.030(3) 0.046(4) 0.029(4) -0.012(3) 0.001(3) -0.004(3) C24 0.034(4) 0.048(4) 0.033(4) -0.009(3) 0.005(3) -0.016(3) C25 0.032(3) 0.034(3) 0.028(3) -0.003(3) 0.003(3) -0.008(3) C26 0.020(3) 0.030(3) 0.022(3) -0.008(2) 0.002(2) -0.011(2) C27 0.028(3) 0.028(3) 0.023(3) -0.014(2) 0.007(2) -0.010(2) C28 0.028(3) 0.030(3) 0.032(4) -0.004(3) 0.005(3) -0.008(3) C29 0.028(3) 0.025(3) 0.028(3) -0.007(2) 0.001(2) -0.011(2) C30 0.034(3) 0.042(4) 0.036(4) -0.010(3) 0.006(3) -0.020(3) C31 0.059(5) 0.043(4) 0.045(4) -0.008(3) 0.007(4) -0.033(4) C32 0.066(5) 0.027(3) 0.037(4) -0.001(3) -0.001(4) -0.016(3) C33 0.036(4) 0.035(4) 0.038(4) -0.007(3) 0.004(3) -0.002(3) C34 0.037(4) 0.041(4) 0.051(5) 0.000(3) -0.001(3) -0.016(3) Cl1 0.0206(7) 0.0368(8) 0.0361(9) -0.0110(7) 0.0008(6) -0.0122(6) Cl2 0.0727(14) 0.0632(12) 0.0366(10) -0.0075(9) 0.0034(9) -0.0324(11) Cl3 0.0329(9) 0.0457(10) 0.0551(12) -0.0126(8) -0.0036(8) -0.0103(7) N1 0.020(2) 0.024(2) 0.025(3) -0.008(2) 0.0034(19) -0.0065(19) N2 0.020(2) 0.025(2) 0.021(2) -0.0068(19) 0.0025(18) -0.0089(19) N3 0.020(2) 0.026(2) 0.031(3) -0.008(2) 0.001(2) -0.009(2) N4 0.019(2) 0.032(3) 0.030(3) -0.003(2) 0.001(2) -0.012(2) O1 0.019(2) 0.027(2) 0.041(3) -0.0039(19) 0.0049(18) -0.0062(17) Pd1 0.0187(2) 0.0247(2) 0.0239(2) -0.00736(17) 0.00153(16) -0.00755(16) _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 C1 C2 1.343(11) . ? C1 C10 1.414(10) . ? C1 H1 0.9500 . ? C2 C3 1.430(9) . ? C2 H2 0.9500 . ? C3 C8 1.425(8) . ? C3 C4 1.428(9) . ? C4 C5 1.348(10) . ? C4 H4 0.9500 . ? C5 C6 1.410(9) . ? C5 H5 0.9500 . ? C6 C7 1.372(8) . ? C6 H6 0.9500 . ? C7 C8 1.427(8) . ? C7 C11 1.503(8) . ? C8 C9 1.417(9) . ? C9 C10 1.356(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N1 1.488(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.333(8) . ? C12 N1 1.374(7) . ? C12 H12 0.9500 . ? C13 N2 1.388(7) . ? C13 H13 0.9500 . ? C14 N2 1.342(7) . ? C14 N1 1.347(7) . ? C14 C15 1.468(8) . ? C15 C20 1.395(8) . ? C15 C16 1.406(7) . ? C16 C17 1.375(8) . ? C16 H16 0.9500 . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? C18 C19 1.390(8) . ? C18 H18 0.9500 . ? C19 C20 1.406(8) . ? C19 H19 0.9500 . ? C20 Pd1 2.008(5) . ? C21 N3 1.323(7) . ? C21 C22 1.380(9) . ? C21 H21 0.9500 . ? C22 C23 1.380(9) . ? C22 H22 0.9500 . ? C23 C24 1.363(9) . ? C23 H23 0.9500 . ? C24 C25 1.379(9) . ? C24 H24 0.9500 . ? C25 N3 1.347(8) . ? C25 H25 0.9500 . ? C26 N2 1.450(7) . ? C26 C27 1.494(8) . ? C26 Pd1 2.035(5) . ? C26 H26 1.0000 . ? C27 O1 1.222(7) . ? C27 N4 1.379(7) . ? C28 C33 1.386(9) . ? C28 C29 1.386(8) . ? C28 H28 0.9500 . ? C29 C30 1.399(8) . ? C29 N4 1.404(7) . ? C30 C31 1.373(10) . ? C30 H30 0.9500 . ? C31 C32 1.386(10) . ? C31 H31 0.9500 . ? C32 C33 1.385(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 Cl2 1.756(8) . ? C34 Cl3 1.777(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? Cl1 Pd1 2.4217(14) . ? N3 Pd1 2.124(5) . ? N4 H4A 0.8800 . ? 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 C2 C1 C10 120.3(7) . . ? C2 C1 H1 119.9 . . ? C10 C1 H1 119.9 . . ? C1 C2 C3 120.7(7) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C8 C3 C4 119.0(6) . . ? C8 C3 C2 119.3(6) . . ? C4 C3 C2 121.6(6) . . ? C5 C4 C3 120.7(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.5(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 121.2(6) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 119.7(6) . . ? C6 C7 C11 119.8(5) . . ? C8 C7 C11 120.5(5) . . ? C9 C8 C3 117.6(6) . . ? C9 C8 C7 123.7(6) . . ? C3 C8 C7 118.8(6) . . ? C10 C9 C8 121.5(6) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C1 120.6(7) . . ? C9 C10 H10 119.7 . . ? C1 C10 H10 119.7 . . ? N1 C11 C7 113.1(5) . . ? N1 C11 H11A 109.0 . . ? C7 C11 H11A 109.0 . . ? N1 C11 H11B 109.0 . . ? C7 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 N1 107.9(5) . . ? C13 C12 H12 126.0 . . ? N1 C12 H12 126.0 . . ? C12 C13 N2 107.3(5) . . ? C12 C13 H13 126.4 . . ? N2 C13 H13 126.4 . . ? N2 C14 N1 107.4(5) . . ? N2 C14 C15 123.0(5) . . ? N1 C14 C15 129.5(5) . . ? C20 C15 C16 121.8(5) . . ? C20 C15 C14 119.7(5) . . ? C16 C15 C14 118.3(5) . . ? C17 C16 C15 120.9(5) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 118.5(5) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C19 120.8(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 122.2(6) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C15 C20 C19 115.9(5) . . ? C15 C20 Pd1 125.1(4) . . ? C19 C20 Pd1 118.5(4) . . ? N3 C21 C22 122.4(6) . . ? N3 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 118.3(6) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C23 C24 C25 119.6(6) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N3 C25 C24 122.2(6) . . ? N3 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N2 C26 C27 112.2(4) . . ? N2 C26 Pd1 114.5(4) . . ? C27 C26 Pd1 105.8(4) . . ? N2 C26 H26 108.1 . . ? C27 C26 H26 108.1 . . ? Pd1 C26 H26 108.1 . . ? O1 C27 N4 123.3(6) . . ? O1 C27 C26 124.0(5) . . ? N4 C27 C26 112.7(5) . . ? C33 C28 C29 119.5(6) . . ? C33 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 119.0(6) . . ? C28 C29 N4 123.9(5) . . ? C30 C29 N4 117.0(5) . . ? C31 C30 C29 120.8(7) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.4(7) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 118.8(7) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C28 121.4(7) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? Cl2 C34 Cl3 111.2(4) . . ? Cl2 C34 H34A 109.4 . . ? Cl3 C34 H34A 109.4 . . ? Cl2 C34 H34B 109.4 . . ? Cl3 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C14 N1 C12 108.8(5) . . ? C14 N1 C11 127.6(5) . . ? C12 N1 C11 123.1(5) . . ? C14 N2 C13 108.6(5) . . ? C14 N2 C26 124.4(5) . . ? C13 N2 C26 126.9(5) . . ? C21 N3 C25 118.1(5) . . ? C21 N3 Pd1 123.7(4) . . ? C25 N3 Pd1 118.1(4) . . ? C27 N4 C29 128.5(5) . . ? C27 N4 H4A 115.8 . . ? C29 N4 H4A 115.8 . . ? C20 Pd1 C26 87.6(2) . . ? C20 Pd1 N3 94.1(2) . . ? C26 Pd1 N3 177.5(2) . . ? C20 Pd1 Cl1 173.24(16) . . ? C26 Pd1 Cl1 88.19(16) . . ? N3 Pd1 Cl1 89.86(13) . . ? 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 C10 C1 C2 C3 1.9(11) . . . . ? C1 C2 C3 C8 -2.2(10) . . . . ? C1 C2 C3 C4 179.3(7) . . . . ? C8 C3 C4 C5 0.6(9) . . . . ? C2 C3 C4 C5 179.1(6) . . . . ? C3 C4 C5 C6 -0.8(10) . . . . ? C4 C5 C6 C7 0.7(10) . . . . ? C5 C6 C7 C8 -0.5(9) . . . . ? C5 C6 C7 C11 -178.2(6) . . . . ? C4 C3 C8 C9 179.4(5) . . . . ? C2 C3 C8 C9 0.8(8) . . . . ? C4 C3 C8 C7 -0.3(8) . . . . ? C2 C3 C8 C7 -178.9(6) . . . . ? C6 C7 C8 C9 -179.4(6) . . . . ? C11 C7 C8 C9 -1.7(9) . . . . ? C6 C7 C8 C3 0.3(8) . . . . ? C11 C7 C8 C3 178.0(5) . . . . ? C3 C8 C9 C10 0.9(9) . . . . ? C7 C8 C9 C10 -179.4(6) . . . . ? C8 C9 C10 C1 -1.3(11) . . . . ? C2 C1 C10 C9 -0.1(12) . . . . ? C6 C7 C11 N1 -108.0(6) . . . . ? C8 C7 C11 N1 74.3(7) . . . . ? N1 C12 C13 N2 -0.3(6) . . . . ? N2 C14 C15 C20 -32.8(8) . . . . ? N1 C14 C15 C20 148.3(6) . . . . ? N2 C14 C15 C16 142.4(5) . . . . ? N1 C14 C15 C16 -36.5(8) . . . . ? C20 C15 C16 C17 -2.8(9) . . . . ? C14 C15 C16 C17 -177.9(5) . . . . ? C15 C16 C17 C18 1.4(9) . . . . ? C16 C17 C18 C19 0.1(9) . . . . ? C17 C18 C19 C20 -0.3(9) . . . . ? C16 C15 C20 C19 2.4(8) . . . . ? C14 C15 C20 C19 177.5(5) . . . . ? C16 C15 C20 Pd1 -168.9(4) . . . . ? C14 C15 C20 Pd1 6.2(7) . . . . ? C18 C19 C20 C15 -0.9(8) . . . . ? C18 C19 C20 Pd1 171.0(5) . . . . ? N3 C21 C22 C23 -0.1(10) . . . . ? C21 C22 C23 C24 0.3(10) . . . . ? C22 C23 C24 C25 -1.0(10) . . . . ? C23 C24 C25 N3 1.3(10) . . . . ? N2 C26 C27 O1 16.2(8) . . . . ? Pd1 C26 C27 O1 -109.3(5) . . . . ? N2 C26 C27 N4 -165.9(4) . . . . ? Pd1 C26 C27 N4 68.6(5) . . . . ? C33 C28 C29 C30 0.2(9) . . . . ? C33 C28 C29 N4 178.3(6) . . . . ? C28 C29 C30 C31 -1.5(9) . . . . ? N4 C29 C30 C31 -179.8(6) . . . . ? C29 C30 C31 C32 1.1(10) . . . . ? C30 C31 C32 C33 0.7(10) . . . . ? C31 C32 C33 C28 -2.0(10) . . . . ? C29 C28 C33 C32 1.6(10) . . . . ? N2 C14 N1 C12 -0.9(6) . . . . ? C15 C14 N1 C12 178.2(5) . . . . ? N2 C14 N1 C11 170.9(5) . . . . ? C15 C14 N1 C11 -10.1(9) . . . . ? C13 C12 N1 C14 0.7(6) . . . . ? C13 C12 N1 C11 -171.5(5) . . . . ? C7 C11 N1 C14 -117.6(6) . . . . ? C7 C11 N1 C12 53.0(7) . . . . ? N1 C14 N2 C13 0.7(6) . . . . ? C15 C14 N2 C13 -178.4(5) . . . . ? N1 C14 N2 C26 -175.3(5) . . . . ? C15 C14 N2 C26 5.6(8) . . . . ? C12 C13 N2 C14 -0.3(6) . . . . ? C12 C13 N2 C26 175.6(5) . . . . ? C27 C26 N2 C14 -78.8(6) . . . . ? Pd1 C26 N2 C14 41.8(6) . . . . ? C27 C26 N2 C13 106.0(6) . . . . ? Pd1 C26 N2 C13 -133.4(5) . . . . ? C22 C21 N3 C25 0.4(9) . . . . ? C22 C21 N3 Pd1 179.5(5) . . . . ? C24 C25 N3 C21 -1.0(9) . . . . ? C24 C25 N3 Pd1 179.8(5) . . . . ? O1 C27 N4 C29 10.5(9) . . . . ? C26 C27 N4 C29 -167.4(5) . . . . ? C28 C29 N4 C27 -4.4(9) . . . . ? C30 C29 N4 C27 173.7(5) . . . . ? C15 C20 Pd1 C26 28.2(5) . . . . ? C19 C20 Pd1 C26 -142.9(5) . . . . ? C15 C20 Pd1 N3 -153.6(5) . . . . ? C19 C20 Pd1 N3 35.3(5) . . . . ? C15 C20 Pd1 Cl1 80.2(16) . . . . ? C19 C20 Pd1 Cl1 -90.8(15) . . . . ? N2 C26 Pd1 C20 -48.9(4) . . . . ? C27 C26 Pd1 C20 75.2(4) . . . . ? N2 C26 Pd1 N3 176(5) . . . . ? C27 C26 Pd1 N3 -60(5) . . . . ? N2 C26 Pd1 Cl1 136.5(4) . . . . ? C27 C26 Pd1 Cl1 -99.5(3) . . . . ? C21 N3 Pd1 C20 56.0(5) . . . . ? C25 N3 Pd1 C20 -124.9(5) . . . . ? C21 N3 Pd1 C26 -169(5) . . . . ? C25 N3 Pd1 C26 11(5) . . . . ? C21 N3 Pd1 Cl1 -129.5(5) . . . . ? C25 N3 Pd1 Cl1 49.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.555 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.139 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 7.ljy379b.cif' data_ljy379b _database_code_depnum_ccdc_archive 'CCDC 850741' #TrackingRef '- 7.ljy379b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C46 H37 Cl N3 O P Pd, (C3 H7 N1 O)' _chemical_formula_sum 'C49 H44 Cl N4 O2 P Pd' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 893.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.507(6) _cell_length_b 13.088(12) _cell_length_c 14.438(7) _cell_angle_alpha 103.747(9) _cell_angle_beta 115.434(6) _cell_angle_gamma 90.425(9) _cell_volume 2057(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4456 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.2 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8892 _exptl_absorpt_correction_T_max 0.8995 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20509 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0990 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.90 _reflns_number_total 10604 _reflns_number_gt 7304 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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. The DMF solvent is disordered with two orientations of 50:50 occupancy ratio. The disordered molecule was refined as a rigid group. The SIMU instruction is used for C47 to O2 and C47a to O2A. ; _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^)+(0.1044P)^2^+0.0000P] 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 10604 _refine_ls_number_parameters 550 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.014 _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 C1 C 0.6996(4) 0.5127(3) 0.3484(4) 0.0255(9) Uani 1 1 d . . . C2 C 0.8473(4) 0.5638(4) 0.3189(4) 0.0303(10) Uani 1 1 d . . . H2A H 0.8915 0.5785 0.2831 0.036 Uiso 1 1 calc R . . C3 C 0.8888(4) 0.5795(3) 0.4246(4) 0.0269(9) Uani 1 1 d . . . H3A H 0.9677 0.6068 0.4774 0.032 Uiso 1 1 calc R . . C4 C 0.5825(4) 0.4692(4) 0.3327(4) 0.0301(10) Uani 1 1 d . . . C5 C 0.5551(7) 0.3632(5) 0.3120(7) 0.078(3) Uani 1 1 d . . . H5A H 0.6125 0.3169 0.3093 0.094 Uiso 1 1 calc R . . C6 C 0.4438(8) 0.3220(6) 0.2947(9) 0.100(3) Uani 1 1 d . . . H6A H 0.4252 0.2476 0.2798 0.120 Uiso 1 1 calc R . . C7 C 0.3620(6) 0.3862(6) 0.2989(5) 0.0570(17) Uani 1 1 d . . . H7A H 0.2855 0.3574 0.2861 0.068 Uiso 1 1 calc R . . C8 C 0.3886(6) 0.4899(6) 0.3209(6) 0.065(2) Uani 1 1 d . . . H8A H 0.3309 0.5354 0.3245 0.078 Uiso 1 1 calc R . . C9 C 0.4994(6) 0.5330(5) 0.3386(6) 0.0591(18) Uani 1 1 d . . . H9A H 0.5173 0.6077 0.3550 0.071 Uiso 1 1 calc R . . C10 C 0.6558(5) 0.4857(4) 0.1563(4) 0.0319(10) Uani 1 1 d . . . H10A H 0.5730 0.4639 0.1420 0.038 Uiso 1 1 calc R . . H10B H 0.6862 0.4226 0.1273 0.038 Uiso 1 1 calc R . . C11 C 0.6547(5) 0.5681(4) 0.1001(4) 0.0374(11) Uani 1 1 d . . . C12 C 0.7348(6) 0.5666(5) 0.0585(5) 0.0494(14) Uani 1 1 d . . . H12A H 0.7908 0.5168 0.0705 0.059 Uiso 1 1 calc R . . C13 C 0.7368(7) 0.6362(6) -0.0011(6) 0.068(2) Uani 1 1 d . . . H13A H 0.7928 0.6322 -0.0296 0.082 Uiso 1 1 calc R . . C14 C 0.6617(8) 0.7068(6) -0.0178(6) 0.075(2) Uani 1 1 d . . . H14A H 0.6647 0.7536 -0.0580 0.090 Uiso 1 1 calc R . . C15 C 0.5755(7) 0.7152(5) 0.0230(5) 0.069(2) Uani 1 1 d . . . C16 C 0.5716(5) 0.6418(4) 0.0846(5) 0.0493(15) Uani 1 1 d . . . C17 C 0.4863(6) 0.6467(6) 0.1228(6) 0.070(2) Uani 1 1 d . . . H17A H 0.4839 0.6007 0.1641 0.084 Uiso 1 1 calc R . . C18 C 0.4047(8) 0.7193(8) 0.0999(8) 0.104(4) Uani 1 1 d . . . H18A H 0.3464 0.7231 0.1260 0.124 Uiso 1 1 calc R . . C19 C 0.4074(10) 0.7863(7) 0.0396(9) 0.108(5) Uani 1 1 d . . . H19A H 0.3501 0.8347 0.0235 0.130 Uiso 1 1 calc R . . C20 C 0.4895(10) 0.7834(6) 0.0038(8) 0.111(4) Uani 1 1 d . . . H20A H 0.4889 0.8308 -0.0370 0.133 Uiso 1 1 calc R . . C21 C 0.8002(4) 0.5413(3) 0.5417(3) 0.0248(9) Uani 1 1 d . . . H21A H 0.7204 0.5511 0.5403 0.030 Uiso 1 1 calc R . . C22 C 0.8348(4) 0.4370(3) 0.5655(4) 0.0281(10) Uani 1 1 d . . . C23 C 0.9118(4) 0.3879(4) 0.7326(4) 0.0313(10) Uani 1 1 d . . . C24 C 0.9350(6) 0.2862(4) 0.7000(5) 0.0540(17) Uani 1 1 d . . . H24A H 0.9358 0.2630 0.6328 0.065 Uiso 1 1 calc R . . C25 C 0.9569(8) 0.2178(5) 0.7637(7) 0.080(3) Uani 1 1 d . . . H25A H 0.9735 0.1482 0.7402 0.096 Uiso 1 1 calc R . . C26 C 0.9551(7) 0.2490(6) 0.8609(6) 0.069(2) Uani 1 1 d . . . H26A H 0.9670 0.2006 0.9031 0.083 Uiso 1 1 calc R . . C27 C 0.9361(6) 0.3502(5) 0.8961(5) 0.0532(16) Uani 1 1 d . . . H27A H 0.9373 0.3729 0.9641 0.064 Uiso 1 1 calc R . . C28 C 0.9151(5) 0.4202(4) 0.8336(4) 0.0406(12) Uani 1 1 d . . . H28A H 0.9028 0.4908 0.8594 0.049 Uiso 1 1 calc R . . C29 C 0.8651(4) 0.8144(3) 0.5538(4) 0.0298(10) Uani 1 1 d . . . C30 C 0.7436(5) 0.7840(4) 0.4937(4) 0.0356(11) Uani 1 1 d . . . H30A H 0.6997 0.7543 0.5228 0.043 Uiso 1 1 calc R . . C31 C 0.6852(6) 0.7964(4) 0.3917(4) 0.0452(14) Uani 1 1 d . . . H31A H 0.6015 0.7766 0.3513 0.054 Uiso 1 1 calc R . . C32 C 0.7505(6) 0.8379(4) 0.3495(5) 0.0485(15) Uani 1 1 d . . . H32A H 0.7118 0.8441 0.2786 0.058 Uiso 1 1 calc R . . C33 C 0.8698(6) 0.8701(4) 0.4085(5) 0.0498(15) Uani 1 1 d . . . H33A H 0.9129 0.9007 0.3793 0.060 Uiso 1 1 calc R . . C34 C 0.9286(5) 0.8585(4) 0.5106(4) 0.0380(12) Uani 1 1 d . . . H34A H 1.0119 0.8806 0.5511 0.046 Uiso 1 1 calc R . . C35 C 1.0865(5) 0.8585(3) 0.7415(4) 0.0302(10) Uani 1 1 d . . . C36 C 1.1758(5) 0.8100(4) 0.7223(5) 0.0476(14) Uani 1 1 d . . . H36A H 1.1605 0.7378 0.6830 0.057 Uiso 1 1 calc R . . C37 C 1.2864(6) 0.8657(5) 0.7600(6) 0.0584(17) Uani 1 1 d . . . H37A H 1.3460 0.8324 0.7441 0.070 Uiso 1 1 calc R . . C38 C 1.3111(6) 0.9685(5) 0.8199(5) 0.0493(14) Uani 1 1 d . . . H38A H 1.3885 1.0058 0.8481 0.059 Uiso 1 1 calc R . . C39 C 1.2234(6) 1.0171(4) 0.8390(5) 0.0483(15) Uani 1 1 d . . . H39A H 1.2399 1.0889 0.8797 0.058 Uiso 1 1 calc R . . C40 C 1.1121(5) 0.9631(4) 0.8000(4) 0.0383(12) Uani 1 1 d . . . H40A H 1.0519 0.9981 0.8135 0.046 Uiso 1 1 calc R . . C41 C 0.8688(5) 0.8630(4) 0.7609(4) 0.0342(11) Uani 1 1 d . . . C42 C 0.7983(7) 0.9405(5) 0.7294(5) 0.0576(18) Uani 1 1 d . . . H42A H 0.7805 0.9535 0.6626 0.069 Uiso 1 1 calc R . . C43 C 0.7531(8) 0.9996(6) 0.7949(7) 0.085(3) Uani 1 1 d . . . H43A H 0.7072 1.0548 0.7742 0.102 Uiso 1 1 calc R . . C44 C 0.7749(7) 0.9781(5) 0.8895(6) 0.067(2) Uani 1 1 d . . . H44A H 0.7428 1.0174 0.9338 0.081 Uiso 1 1 calc R . . C45 C 0.8425(6) 0.9006(5) 0.9193(5) 0.0554(17) Uani 1 1 d . . . H45A H 0.8576 0.8861 0.9849 0.067 Uiso 1 1 calc R . . C46 C 0.8894(5) 0.8428(4) 0.8564(4) 0.0413(13) Uani 1 1 d . . . H46A H 0.9364 0.7887 0.8786 0.050 Uiso 1 1 calc R . . Cl1 Cl 1.09076(11) 0.65900(9) 0.86128(9) 0.0349(3) Uani 1 1 d . . . N1 N 0.7303(3) 0.5231(3) 0.2726(3) 0.0274(8) Uani 1 1 d . . . N2 N 0.7949(3) 0.5483(3) 0.4412(3) 0.0253(8) Uani 1 1 d . . . N3 N 0.8797(4) 0.4611(3) 0.6711(3) 0.0265(8) Uani 1 1 d . . . O1 O 0.8254(4) 0.3539(2) 0.4982(3) 0.0397(9) Uani 1 1 d . . . P1 P 0.93844(11) 0.78684(8) 0.68307(9) 0.0256(2) Uani 1 1 d . . . Pd1 Pd 0.93026(3) 0.61811(2) 0.68908(3) 0.02396(11) Uani 1 1 d . . . C47 C 0.5240(18) 0.0475(12) 0.5014(16) 0.133(8) Uani 0.50 1 d PGU A -1 H47A H 0.4849 0.0708 0.5474 0.199 Uiso 0.50 1 calc PR A -1 H47B H 0.5544 -0.0200 0.5107 0.199 Uiso 0.50 1 calc PR A -1 H47C H 0.4663 0.0382 0.4270 0.199 Uiso 0.50 1 calc PR A -1 C48 C 0.6896(18) 0.1065(14) 0.4679(14) 0.120(8) Uani 0.50 1 d PGU A -1 H48A H 0.7529 0.1656 0.4949 0.179 Uiso 0.50 1 calc PR A -1 H48B H 0.6366 0.1002 0.3928 0.179 Uiso 0.50 1 calc PR A -1 H48C H 0.7252 0.0406 0.4747 0.179 Uiso 0.50 1 calc PR A -1 C49 C 0.6519(9) 0.2129(8) 0.6099(10) 0.137(7) Uani 0.50 1 d PGU A -1 H49A H 0.7187 0.2605 0.6256 0.164 Uiso 0.50 1 calc PR A -1 N4 N 0.6213(11) 0.1259(9) 0.5292(9) 0.132(6) Uani 0.50 1 d PGU A -1 O2 O 0.5984(10) 0.2352(8) 0.6657(10) 0.097(4) Uani 0.50 1 d PGU A -1 C47A C 0.5355(15) 0.0304(14) 0.413(2) 0.193(11) Uani 0.50 1 d PGU B -2 H47D H 0.4622 0.0511 0.4175 0.290 Uiso 0.50 1 calc PR B -2 H47E H 0.5543 -0.0348 0.4361 0.290 Uiso 0.50 1 calc PR B -2 H47F H 0.5243 0.0182 0.3400 0.290 Uiso 0.50 1 calc PR B -2 C48A C 0.7500(13) 0.0963(17) 0.489(2) 0.137(9) Uani 0.50 1 d PGU B -2 H48D H 0.8073 0.1586 0.5383 0.205 Uiso 0.50 1 calc PR B -2 H48E H 0.7474 0.0848 0.4187 0.205 Uiso 0.50 1 calc PR B -2 H48F H 0.7748 0.0338 0.5157 0.205 Uiso 0.50 1 calc PR B -2 C49A C 0.6169(12) 0.2030(10) 0.5399(13) 0.130(6) Uani 0.50 1 d PGU B -2 H49B H 0.6849 0.2539 0.5853 0.156 Uiso 0.50 1 calc PR B -2 N4A N 0.6320(11) 0.1135(10) 0.4820(11) 0.122(6) Uani 0.50 1 d PGU B -2 O2A O 0.5197(15) 0.2237(13) 0.5381(17) 0.219(9) Uani 0.50 1 d PGU 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 C1 0.029(2) 0.0180(19) 0.029(2) 0.0044(17) 0.014(2) 0.0039(17) C2 0.029(2) 0.030(2) 0.031(2) 0.008(2) 0.012(2) 0.0000(19) C3 0.024(2) 0.023(2) 0.029(2) 0.0035(18) 0.0090(19) 0.0019(17) C4 0.031(3) 0.027(2) 0.031(2) 0.0033(19) 0.014(2) -0.0008(19) C5 0.065(5) 0.028(3) 0.153(8) 0.000(4) 0.072(6) -0.005(3) C6 0.085(6) 0.040(4) 0.177(10) -0.013(5) 0.082(7) -0.027(4) C7 0.037(3) 0.078(5) 0.054(4) -0.001(3) 0.028(3) -0.019(3) C8 0.040(4) 0.069(5) 0.099(6) 0.017(4) 0.045(4) 0.011(3) C9 0.045(4) 0.037(3) 0.106(6) 0.016(3) 0.045(4) 0.007(3) C10 0.034(3) 0.031(2) 0.021(2) 0.0008(19) 0.007(2) 0.001(2) C11 0.042(3) 0.027(2) 0.031(3) 0.003(2) 0.007(2) 0.001(2) C12 0.048(4) 0.055(4) 0.041(3) 0.018(3) 0.013(3) 0.000(3) C13 0.062(5) 0.080(5) 0.056(4) 0.034(4) 0.014(4) -0.009(4) C14 0.089(6) 0.052(4) 0.062(5) 0.022(4) 0.009(4) -0.017(4) C15 0.074(5) 0.026(3) 0.043(4) -0.001(3) -0.027(3) 0.003(3) C16 0.046(3) 0.027(3) 0.039(3) -0.004(2) -0.007(3) 0.000(2) C17 0.046(4) 0.063(4) 0.051(4) -0.022(3) -0.003(3) 0.011(3) C18 0.062(5) 0.088(7) 0.087(7) -0.038(6) -0.003(5) 0.029(5) C19 0.090(7) 0.042(4) 0.101(8) -0.022(4) -0.020(6) 0.040(5) C20 0.113(8) 0.031(4) 0.088(7) -0.003(4) -0.037(6) 0.013(5) C21 0.029(2) 0.024(2) 0.025(2) 0.0046(18) 0.017(2) 0.0025(18) C22 0.032(2) 0.019(2) 0.037(3) 0.0098(19) 0.017(2) 0.0016(18) C23 0.034(3) 0.025(2) 0.040(3) 0.015(2) 0.017(2) 0.0054(19) C24 0.091(5) 0.032(3) 0.062(4) 0.025(3) 0.048(4) 0.024(3) C25 0.124(7) 0.039(4) 0.104(6) 0.042(4) 0.062(6) 0.032(4) C26 0.088(5) 0.056(4) 0.081(5) 0.052(4) 0.035(5) 0.014(4) C27 0.061(4) 0.053(4) 0.045(3) 0.026(3) 0.016(3) -0.002(3) C28 0.048(3) 0.037(3) 0.037(3) 0.017(2) 0.015(3) 0.003(2) C29 0.039(3) 0.0164(19) 0.031(2) 0.0060(18) 0.013(2) 0.0055(18) C30 0.045(3) 0.021(2) 0.039(3) 0.011(2) 0.016(2) 0.005(2) C31 0.056(4) 0.025(2) 0.041(3) 0.010(2) 0.009(3) 0.005(2) C32 0.063(4) 0.033(3) 0.039(3) 0.019(2) 0.008(3) 0.004(3) C33 0.071(4) 0.035(3) 0.042(3) 0.015(3) 0.021(3) -0.002(3) C34 0.052(3) 0.024(2) 0.039(3) 0.011(2) 0.020(3) 0.003(2) C35 0.041(3) 0.020(2) 0.028(2) 0.0080(18) 0.013(2) 0.0027(19) C36 0.045(3) 0.024(2) 0.065(4) 0.003(3) 0.020(3) 0.004(2) C37 0.042(3) 0.039(3) 0.093(5) 0.013(3) 0.031(4) 0.005(3) C38 0.045(3) 0.037(3) 0.056(4) 0.008(3) 0.015(3) -0.010(3) C39 0.069(4) 0.025(3) 0.045(3) -0.004(2) 0.028(3) -0.015(3) C40 0.048(3) 0.021(2) 0.043(3) 0.000(2) 0.023(3) -0.005(2) C41 0.045(3) 0.019(2) 0.040(3) 0.004(2) 0.022(2) 0.006(2) C42 0.089(5) 0.044(3) 0.056(4) 0.022(3) 0.041(4) 0.038(3) C43 0.124(7) 0.067(5) 0.086(6) 0.029(4) 0.062(6) 0.067(5) C44 0.094(6) 0.058(4) 0.072(5) 0.013(4) 0.060(5) 0.035(4) C45 0.082(5) 0.050(4) 0.053(4) 0.013(3) 0.046(4) 0.022(3) C46 0.053(3) 0.033(3) 0.042(3) 0.010(2) 0.024(3) 0.017(2) Cl1 0.0395(7) 0.0296(6) 0.0293(6) 0.0094(5) 0.0086(5) 0.0039(5) N1 0.029(2) 0.0233(18) 0.0247(19) 0.0039(15) 0.0082(17) -0.0005(15) N2 0.030(2) 0.0173(16) 0.0271(19) 0.0056(15) 0.0116(17) 0.0051(15) N3 0.038(2) 0.0128(16) 0.031(2) 0.0074(15) 0.0171(18) 0.0030(15) O1 0.060(2) 0.0188(16) 0.041(2) 0.0003(15) 0.0271(19) 0.0005(16) P1 0.0344(6) 0.0141(5) 0.0268(6) 0.0051(4) 0.0124(5) 0.0035(4) Pd1 0.0310(2) 0.01412(16) 0.02641(19) 0.00607(12) 0.01211(15) 0.00381(12) C47 0.117(16) 0.120(16) 0.130(15) 0.017(15) 0.036(14) 0.002(13) C48 0.112(16) 0.082(13) 0.171(17) 0.041(12) 0.065(13) -0.029(12) C49 0.078(10) 0.120(12) 0.188(14) 0.002(11) 0.058(10) 0.000(9) N4 0.091(10) 0.130(11) 0.165(13) 0.014(10) 0.060(10) 0.015(9) O2 0.075(7) 0.084(8) 0.156(11) 0.031(8) 0.074(8) 0.016(6) C47A 0.105(15) 0.166(19) 0.25(2) 0.003(18) 0.058(17) -0.023(15) C48A 0.085(14) 0.103(15) 0.193(19) 0.005(14) 0.052(13) 0.002(12) C49A 0.082(10) 0.096(11) 0.210(15) 0.023(11) 0.071(11) -0.028(9) N4A 0.089(9) 0.113(10) 0.190(14) 0.054(10) 0.077(10) -0.027(9) O2A 0.114(13) 0.130(13) 0.301(19) 0.012(14) 0.015(15) -0.008(12) _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 C1 N2 1.326(6) . ? C1 N1 1.338(6) . ? C1 C4 1.470(6) . ? C2 C3 1.345(6) . ? C2 N1 1.361(6) . ? C2 H2A 0.9500 . ? C3 N2 1.372(6) . ? C3 H3A 0.9500 . ? C4 C9 1.357(7) . ? C4 C5 1.357(7) . ? C5 C6 1.385(9) . ? C5 H5A 0.9500 . ? C6 C7 1.340(10) . ? C6 H6A 0.9500 . ? C7 C8 1.323(10) . ? C7 H7A 0.9500 . ? C8 C9 1.386(8) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 N1 1.480(6) . ? C10 C11 1.492(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.370(8) . ? C11 C16 1.406(7) . ? C12 C13 1.400(8) . ? C12 H12A 0.9500 . ? C13 C14 1.310(11) . ? C13 H13A 0.9500 . ? C14 C15 1.426(12) . ? C14 H14A 0.9500 . ? C15 C20 1.382(11) . ? C15 C16 1.469(10) . ? C16 C17 1.392(10) . ? C17 C18 1.389(10) . ? C17 H17A 0.9500 . ? C18 C19 1.384(16) . ? C18 H18A 0.9500 . ? C19 C20 1.329(16) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 N2 1.449(5) . ? C21 C22 1.508(6) . ? C21 Pd1 2.043(5) . ? C21 H21A 1.0000 . ? C22 O1 1.240(5) . ? C22 N3 1.331(6) . ? C22 Pd1 2.520(5) . ? C23 C24 1.380(7) . ? C23 C28 1.401(7) . ? C23 N3 1.403(5) . ? C24 C25 1.380(8) . ? C24 H24A 0.9500 . ? C25 C26 1.375(11) . ? C25 H25A 0.9500 . ? C26 C27 1.362(9) . ? C26 H26A 0.9500 . ? C27 C28 1.385(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.384(7) . ? C29 C34 1.394(7) . ? C29 P1 1.820(5) . ? C30 C31 1.386(7) . ? C30 H30A 0.9500 . ? C31 C32 1.382(8) . ? C31 H31A 0.9500 . ? C32 C33 1.363(9) . ? C32 H32A 0.9500 . ? C33 C34 1.383(8) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C40 1.380(6) . ? C35 C36 1.384(7) . ? C35 P1 1.811(5) . ? C36 C37 1.375(8) . ? C36 H36A 0.9500 . ? C37 C38 1.365(8) . ? C37 H37A 0.9500 . ? C38 C39 1.367(9) . ? C38 H38A 0.9500 . ? C39 C40 1.370(8) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.379(7) . ? C41 C46 1.380(7) . ? C41 P1 1.826(5) . ? C42 C43 1.389(9) . ? C42 H42A 0.9500 . ? C43 C44 1.371(10) . ? C43 H43A 0.9500 . ? C44 C45 1.355(9) . ? C44 H44A 0.9500 . ? C45 C46 1.372(7) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? Cl1 Pd1 2.3585(15) . ? N3 Pd1 2.068(4) . ? P1 Pd1 2.234(2) . ? C47 N4 1.4351 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N4 1.4573 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 O2 1.2388 . ? C49 N4 1.3346 . ? C49 H49A 0.9500 . ? C47A N4A 1.4352 . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48A N4A 1.4575 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C49A O2A 1.2387 . ? C49A N4A 1.3346 . ? C49A H49B 0.9500 . ? 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 C1 N1 107.4(4) . . ? N2 C1 C4 125.8(4) . . ? N1 C1 C4 126.8(4) . . ? C3 C2 N1 107.5(4) . . ? C3 C2 H2A 126.3 . . ? N1 C2 H2A 126.3 . . ? C2 C3 N2 106.6(4) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? C9 C4 C5 118.2(5) . . ? C9 C4 C1 121.4(5) . . ? C5 C4 C1 120.3(5) . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 120.6(7) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C8 C7 C6 119.6(6) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 120.9(6) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C4 C9 C8 120.3(6) . . ? C4 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? N1 C10 C11 112.8(4) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C16 120.1(5) . . ? C12 C11 C10 117.4(5) . . ? C16 C11 C10 122.4(5) . . ? C11 C12 C13 122.1(6) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C14 C13 C12 120.4(8) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 121.7(7) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C20 C15 C14 125.0(9) . . ? C20 C15 C16 116.5(10) . . ? C14 C15 C16 118.4(6) . . ? C17 C16 C11 123.3(6) . . ? C17 C16 C15 119.5(6) . . ? C11 C16 C15 117.2(6) . . ? C18 C17 C16 119.3(9) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C19 C18 C17 120.7(10) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C20 C19 C18 120.6(8) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C15 123.4(10) . . ? C19 C20 H20A 118.3 . . ? C15 C20 H20A 118.3 . . ? N2 C21 C22 113.0(3) . . ? N2 C21 Pd1 125.7(3) . . ? C22 C21 Pd1 89.1(3) . . ? N2 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? Pd1 C21 H21A 109.0 . . ? O1 C22 N3 132.1(4) . . ? O1 C22 C21 125.0(4) . . ? N3 C22 C21 102.8(4) . . ? O1 C22 Pd1 155.5(4) . . ? N3 C22 Pd1 55.1(2) . . ? C21 C22 Pd1 54.2(2) . . ? C24 C23 C28 117.8(4) . . ? C24 C23 N3 125.5(5) . . ? C28 C23 N3 116.6(4) . . ? C23 C24 C25 120.8(6) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C26 C25 C24 120.8(6) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 119.3(5) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C28 120.6(6) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C27 C28 C23 120.5(5) . . ? C27 C28 H28A 119.7 . . ? C23 C28 H28A 119.7 . . ? C30 C29 C34 119.1(5) . . ? C30 C29 P1 118.7(4) . . ? C34 C29 P1 122.1(4) . . ? C29 C30 C31 120.8(5) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C32 C31 C30 119.0(6) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C33 C32 C31 120.7(5) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 120.6(6) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C33 C34 C29 119.7(6) . . ? C33 C34 H34A 120.2 . . ? C29 C34 H34A 120.2 . . ? C40 C35 C36 118.3(5) . . ? C40 C35 P1 121.8(4) . . ? C36 C35 P1 119.8(4) . . ? C37 C36 C35 120.5(5) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C38 C37 C36 120.5(6) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C37 C38 C39 119.4(6) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? C38 C39 C40 120.6(5) . . ? C38 C39 H39A 119.7 . . ? C40 C39 H39A 119.7 . . ? C39 C40 C35 120.7(5) . . ? C39 C40 H40A 119.7 . . ? C35 C40 H40A 119.7 . . ? C42 C41 C46 118.7(5) . . ? C42 C41 P1 123.1(4) . . ? C46 C41 P1 118.2(4) . . ? C41 C42 C43 120.3(6) . . ? C41 C42 H42A 119.9 . . ? C43 C42 H42A 119.9 . . ? C44 C43 C42 119.9(6) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C45 C44 C43 119.6(6) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C44 C45 C46 121.1(6) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? C45 C46 C41 120.3(5) . . ? C45 C46 H46A 119.8 . . ? C41 C46 H46A 119.8 . . ? C1 N1 C2 109.1(4) . . ? C1 N1 C10 126.6(4) . . ? C2 N1 C10 123.9(4) . . ? C1 N2 C3 109.4(4) . . ? C1 N2 C21 123.8(4) . . ? C3 N2 C21 126.3(4) . . ? C22 N3 C23 125.4(4) . . ? C22 N3 Pd1 93.1(2) . . ? C23 N3 Pd1 137.6(3) . . ? C35 P1 C29 103.5(2) . . ? C35 P1 C41 103.4(2) . . ? C29 P1 C41 104.6(2) . . ? C35 P1 Pd1 115.86(15) . . ? C29 P1 Pd1 118.12(15) . . ? C41 P1 Pd1 109.71(16) . . ? C21 Pd1 N3 65.41(16) . . ? C21 Pd1 P1 103.25(13) . . ? N3 Pd1 P1 166.22(12) . . ? C21 Pd1 Cl1 164.29(12) . . ? N3 Pd1 Cl1 99.87(11) . . ? P1 Pd1 Cl1 92.06(5) . . ? C21 Pd1 C22 36.76(15) . . ? N3 Pd1 C22 31.84(14) . . ? P1 Pd1 C22 139.20(11) . . ? Cl1 Pd1 C22 127.54(11) . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N4 C48 H48A 109.5 . . ? N4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O2 C49 N4 124.0 . . ? O2 C49 H49A 118.0 . . ? N4 C49 H49A 118.0 . . ? C49 N4 C47 122.2 . . ? C49 N4 C48 120.0 . . ? C47 N4 C48 117.8 . . ? N4A C47A H47D 109.5 . . ? N4A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? N4A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? N4A C48A H48D 109.5 . . ? N4A C48A H48E 109.5 . . ? H48D C48A H48E 109.5 . . ? N4A C48A H48F 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? O2A C49A N4A 124.0 . . ? O2A C49A H49B 118.0 . . ? N4A C49A H49B 118.0 . . ? C49A N4A C47A 122.2 . . ? C49A N4A C48A 120.0 . . ? C47A N4A C48A 117.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.4(5) . . . . ? N2 C1 C4 C9 85.9(7) . . . . ? N1 C1 C4 C9 -94.6(7) . . . . ? N2 C1 C4 C5 -94.0(7) . . . . ? N1 C1 C4 C5 85.5(7) . . . . ? C9 C4 C5 C6 1.7(12) . . . . ? C1 C4 C5 C6 -178.5(8) . . . . ? C4 C5 C6 C7 -0.4(15) . . . . ? C5 C6 C7 C8 -0.8(15) . . . . ? C6 C7 C8 C9 0.6(13) . . . . ? C5 C4 C9 C8 -1.8(11) . . . . ? C1 C4 C9 C8 178.4(6) . . . . ? C7 C8 C9 C4 0.7(12) . . . . ? N1 C10 C11 C12 94.6(6) . . . . ? N1 C10 C11 C16 -88.7(6) . . . . ? C16 C11 C12 C13 -0.7(9) . . . . ? C10 C11 C12 C13 176.1(6) . . . . ? C11 C12 C13 C14 0.9(11) . . . . ? C12 C13 C14 C15 -0.4(12) . . . . ? C13 C14 C15 C20 -176.3(7) . . . . ? C13 C14 C15 C16 -0.3(10) . . . . ? C12 C11 C16 C17 178.8(6) . . . . ? C10 C11 C16 C17 2.1(8) . . . . ? C12 C11 C16 C15 0.0(8) . . . . ? C10 C11 C16 C15 -176.7(5) . . . . ? C20 C15 C16 C17 -2.0(8) . . . . ? C14 C15 C16 C17 -178.3(6) . . . . ? C20 C15 C16 C11 176.8(6) . . . . ? C14 C15 C16 C11 0.5(8) . . . . ? C11 C16 C17 C18 -177.4(6) . . . . ? C15 C16 C17 C18 1.4(9) . . . . ? C16 C17 C18 C19 0.2(11) . . . . ? C17 C18 C19 C20 -1.1(13) . . . . ? C18 C19 C20 C15 0.3(14) . . . . ? C14 C15 C20 C19 177.2(8) . . . . ? C16 C15 C20 C19 1.2(11) . . . . ? N2 C21 C22 O1 -20.9(7) . . . . ? Pd1 C21 C22 O1 -149.8(5) . . . . ? N2 C21 C22 N3 156.2(4) . . . . ? Pd1 C21 C22 N3 27.3(3) . . . . ? N2 C21 C22 Pd1 128.9(4) . . . . ? C28 C23 C24 C25 2.0(10) . . . . ? N3 C23 C24 C25 -174.9(7) . . . . ? C23 C24 C25 C26 0.6(13) . . . . ? C24 C25 C26 C27 -2.6(13) . . . . ? C25 C26 C27 C28 2.0(12) . . . . ? C26 C27 C28 C23 0.6(10) . . . . ? C24 C23 C28 C27 -2.6(8) . . . . ? N3 C23 C28 C27 174.6(5) . . . . ? C34 C29 C30 C31 0.4(7) . . . . ? P1 C29 C30 C31 -175.3(4) . . . . ? C29 C30 C31 C32 1.2(7) . . . . ? C30 C31 C32 C33 -2.5(8) . . . . ? C31 C32 C33 C34 2.2(9) . . . . ? C32 C33 C34 C29 -0.6(8) . . . . ? C30 C29 C34 C33 -0.7(7) . . . . ? P1 C29 C34 C33 174.9(4) . . . . ? C40 C35 C36 C37 -0.8(9) . . . . ? P1 C35 C36 C37 175.5(5) . . . . ? C35 C36 C37 C38 2.3(10) . . . . ? C36 C37 C38 C39 -2.4(10) . . . . ? C37 C38 C39 C40 1.0(9) . . . . ? C38 C39 C40 C35 0.5(9) . . . . ? C36 C35 C40 C39 -0.6(8) . . . . ? P1 C35 C40 C39 -176.8(4) . . . . ? C46 C41 C42 C43 2.5(10) . . . . ? P1 C41 C42 C43 -176.5(6) . . . . ? C41 C42 C43 C44 -2.5(13) . . . . ? C42 C43 C44 C45 1.3(14) . . . . ? C43 C44 C45 C46 -0.2(13) . . . . ? C44 C45 C46 C41 0.2(11) . . . . ? C42 C41 C46 C45 -1.3(9) . . . . ? P1 C41 C46 C45 177.7(5) . . . . ? N2 C1 N1 C2 1.2(5) . . . . ? C4 C1 N1 C2 -178.3(4) . . . . ? N2 C1 N1 C10 174.6(4) . . . . ? C4 C1 N1 C10 -4.9(7) . . . . ? C3 C2 N1 C1 -0.5(5) . . . . ? C3 C2 N1 C10 -174.1(4) . . . . ? C11 C10 N1 C1 132.4(5) . . . . ? C11 C10 N1 C2 -55.2(6) . . . . ? N1 C1 N2 C3 -1.5(5) . . . . ? C4 C1 N2 C3 178.0(4) . . . . ? N1 C1 N2 C21 -174.2(4) . . . . ? C4 C1 N2 C21 5.4(6) . . . . ? C2 C3 N2 C1 1.2(5) . . . . ? C2 C3 N2 C21 173.6(4) . . . . ? C22 C21 N2 C1 85.8(5) . . . . ? Pd1 C21 N2 C1 -167.7(3) . . . . ? C22 C21 N2 C3 -85.6(5) . . . . ? Pd1 C21 N2 C3 20.9(6) . . . . ? O1 C22 N3 C23 -11.4(8) . . . . ? C21 C22 N3 C23 171.8(4) . . . . ? Pd1 C22 N3 C23 -161.2(5) . . . . ? O1 C22 N3 Pd1 149.9(5) . . . . ? C21 C22 N3 Pd1 -27.0(3) . . . . ? C24 C23 N3 C22 19.8(8) . . . . ? C28 C23 N3 C22 -157.2(5) . . . . ? C24 C23 N3 Pd1 -131.8(6) . . . . ? C28 C23 N3 Pd1 51.3(7) . . . . ? C40 C35 P1 C29 88.2(4) . . . . ? C36 C35 P1 C29 -87.9(4) . . . . ? C40 C35 P1 C41 -20.8(4) . . . . ? C36 C35 P1 C41 163.1(4) . . . . ? C40 C35 P1 Pd1 -140.9(4) . . . . ? C36 C35 P1 Pd1 43.0(5) . . . . ? C30 C29 P1 C35 -170.6(4) . . . . ? C34 C29 P1 C35 13.8(4) . . . . ? C30 C29 P1 C41 -62.6(4) . . . . ? C34 C29 P1 C41 121.8(4) . . . . ? C30 C29 P1 Pd1 59.8(4) . . . . ? C34 C29 P1 Pd1 -115.8(4) . . . . ? C42 C41 P1 C35 95.0(5) . . . . ? C46 C41 P1 C35 -83.9(5) . . . . ? C42 C41 P1 C29 -13.1(6) . . . . ? C46 C41 P1 C29 167.9(4) . . . . ? C42 C41 P1 Pd1 -140.8(5) . . . . ? C46 C41 P1 Pd1 40.3(5) . . . . ? N2 C21 Pd1 N3 -136.5(4) . . . . ? C22 C21 Pd1 N3 -18.5(2) . . . . ? N2 C21 Pd1 P1 51.8(4) . . . . ? C22 C21 Pd1 P1 169.8(2) . . . . ? N2 C21 Pd1 Cl1 -115.1(4) . . . . ? C22 C21 Pd1 Cl1 3.0(6) . . . . ? N2 C21 Pd1 C22 -118.0(5) . . . . ? C22 N3 Pd1 C21 21.1(3) . . . . ? C23 N3 Pd1 C21 178.1(5) . . . . ? C22 N3 Pd1 P1 57.2(6) . . . . ? C23 N3 Pd1 P1 -145.7(4) . . . . ? C22 N3 Pd1 Cl1 -153.2(3) . . . . ? C23 N3 Pd1 Cl1 3.9(5) . . . . ? C23 N3 Pd1 C22 157.1(6) . . . . ? C35 P1 Pd1 C21 -137.8(2) . . . . ? C29 P1 Pd1 C21 -14.1(2) . . . . ? C41 P1 Pd1 C21 105.6(2) . . . . ? C35 P1 Pd1 N3 -171.2(5) . . . . ? C29 P1 Pd1 N3 -47.5(5) . . . . ? C41 P1 Pd1 N3 72.2(5) . . . . ? C35 P1 Pd1 Cl1 38.72(17) . . . . ? C29 P1 Pd1 Cl1 162.37(19) . . . . ? C41 P1 Pd1 Cl1 -77.9(2) . . . . ? C35 P1 Pd1 C22 -128.4(2) . . . . ? C29 P1 Pd1 C22 -4.8(3) . . . . ? C41 P1 Pd1 C22 114.9(2) . . . . ? O1 C22 Pd1 C21 97.0(9) . . . . ? N3 C22 Pd1 C21 -146.9(4) . . . . ? O1 C22 Pd1 N3 -116.1(10) . . . . ? C21 C22 Pd1 N3 146.9(4) . . . . ? O1 C22 Pd1 P1 81.7(9) . . . . ? N3 C22 Pd1 P1 -162.2(2) . . . . ? C21 C22 Pd1 P1 -15.3(3) . . . . ? O1 C22 Pd1 Cl1 -82.0(9) . . . . ? N3 C22 Pd1 Cl1 34.1(3) . . . . ? C21 C22 Pd1 Cl1 -179.0(2) . . . . ? O2 C49 N4 C47 -1.9 . . . . ? O2 C49 N4 C48 179.8 . . . . ? O2A C49A N4A C47A -1.9 . . . . ? O2A C49A N4A C48A 179.8 . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.90 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.577 _refine_diff_density_min -2.052 _refine_diff_density_rms 0.134 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 9.ljy306.cif' data_ljy306 _database_code_depnum_ccdc_archive 'CCDC 850742' #TrackingRef '- 9.ljy306.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C40 H38 Cl2 F2 N6 O2 Pd2, 4(C3 H7 N O)' _chemical_formula_sum 'C52 H66 Cl2 F2 N10 O6 Pd2' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 1248.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4686(11) _cell_length_b 11.5276(14) _cell_length_c 13.1627(16) _cell_angle_alpha 90.963(7) _cell_angle_beta 106.242(6) _cell_angle_gamma 94.606(7) _cell_volume 1373.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3907 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.4 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8538 _exptl_absorpt_correction_T_max 0.8670 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13690 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5937 _reflns_number_gt 4654 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0657P)^2^+0.0000P] 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 5937 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.54272(3) -0.04033(3) 0.63883(2) 0.03480(13) Uani 1 1 d . . . Cl1 Cl 0.66797(11) -0.02325(11) 0.50121(8) 0.0478(3) Uani 1 1 d . . . O1 O 0.5055(4) 0.1000(3) 0.9016(3) 0.0560(9) Uani 1 1 d . . . N3 N 0.6845(4) -0.0206(3) 0.9012(3) 0.0430(8) Uani 1 1 d . . . C3 C 0.2617(5) 0.0986(4) 0.7007(3) 0.0406(10) Uani 1 1 d . . . C20 C 0.6993(4) -0.1217(4) 0.7377(3) 0.0392(9) Uani 1 1 d . . . N1 N 0.3001(4) -0.0067(3) 0.7298(3) 0.0392(8) Uani 1 1 d . . . N2 N 0.1122(4) 0.0916(3) 0.6665(3) 0.0433(8) Uani 1 1 d . . . C2 C 0.0590(5) -0.0200(4) 0.6756(4) 0.0499(11) Uani 1 1 d . . . H2 H -0.0421 -0.0487 0.6572 0.060 Uiso 1 1 calc R . . C6 C -0.0234(5) 0.2518(4) 0.7119(4) 0.0446(10) Uani 1 1 d . . . C1 C 0.1740(5) -0.0820(4) 0.7149(4) 0.0444(10) Uani 1 1 d . . . H1 H 0.1700 -0.1624 0.7297 0.053 Uiso 1 1 calc R . . C5 C 0.0191(5) 0.1868(4) 0.6254(4) 0.0504(11) Uani 1 1 d . . . H5A H -0.0717 0.1539 0.5718 0.061 Uiso 1 1 calc R . . H5B H 0.0732 0.2422 0.5899 0.061 Uiso 1 1 calc R . . C7 C -0.1288(6) 0.2003(5) 0.7556(4) 0.0548(12) Uani 1 1 d . . . H7 H -0.1729 0.1240 0.7321 0.066 Uiso 1 1 calc R . . C4 C 0.3598(5) 0.2059(4) 0.7001(4) 0.0524(12) Uani 1 1 d . . . H4A H 0.3699 0.2544 0.7641 0.079 Uiso 1 1 calc R . . H4B H 0.3170 0.2496 0.6374 0.079 Uiso 1 1 calc R . . H4C H 0.4573 0.1845 0.6986 0.079 Uiso 1 1 calc R . . C8 C 0.0396(5) 0.3640(4) 0.7461(4) 0.0560(12) Uani 1 1 d . . . H8 H 0.1102 0.4009 0.7154 0.067 Uiso 1 1 calc R . . C10 C -0.1055(6) 0.3695(5) 0.8657(4) 0.0548(12) Uani 1 1 d . . . C9 C -0.0019(6) 0.4219(5) 0.8261(4) 0.0613(14) Uani 1 1 d . . . H9 H 0.0427 0.4974 0.8520 0.074 Uiso 1 1 calc R . . C11 C -0.1702(6) 0.2601(5) 0.8336(4) 0.0628(14) Uani 1 1 d . . . H11 H -0.2423 0.2253 0.8640 0.075 Uiso 1 1 calc R . . F1 F -0.1486(4) 0.4274(3) 0.9419(3) 0.0845(11) Uani 1 1 d . . . C12 C 0.4507(4) -0.0480(4) 0.7612(3) 0.0376(9) Uani 1 1 d . . . H12 H 0.4403 -0.1316 0.7791 0.045 Uiso 1 1 calc R . . C13 C 0.5467(5) 0.0184(4) 0.8591(3) 0.0422(10) Uani 1 1 d . . . C14 C 0.7681(5) 0.0241(5) 1.0081(4) 0.0601(14) Uani 1 1 d . . . H14A H 0.7256 0.0937 1.0262 0.090 Uiso 1 1 calc R . . H14B H 0.8714 0.0442 1.0102 0.090 Uiso 1 1 calc R . . H14C H 0.7628 -0.0357 1.0593 0.090 Uiso 1 1 calc R . . C15 C 0.7451(4) -0.1049(4) 0.8488(3) 0.0406(10) Uani 1 1 d . . . C19 C 0.7632(5) -0.2078(4) 0.6939(4) 0.0426(10) Uani 1 1 d . . . H19 H 0.7287 -0.2252 0.6198 0.051 Uiso 1 1 calc R . . C16 C 0.8552(5) -0.1690(4) 0.9095(4) 0.0512(11) Uani 1 1 d . . . H16 H 0.8850 -0.1579 0.9844 0.061 Uiso 1 1 calc R . . C18 C 0.8745(5) -0.2684(4) 0.7546(4) 0.0521(12) Uani 1 1 d . . . H18 H 0.9184 -0.3239 0.7218 0.063 Uiso 1 1 calc R . . C17 C 0.9217(5) -0.2485(5) 0.8625(4) 0.0554(12) Uani 1 1 d . . . H17 H 0.9995 -0.2890 0.9044 0.066 Uiso 1 1 calc R . . N5 N 0.4948(6) 0.6304(5) 0.9024(4) 0.0750(14) Uani 1 1 d . . . O3 O 0.2644(7) 0.6543(5) 0.8024(6) 0.125(2) Uani 1 1 d . . . C25 C 0.3658(10) 0.6669(6) 0.8874(8) 0.096(2) Uani 1 1 d . . . H25 H 0.3461 0.7063 0.9453 0.115 Uiso 1 1 calc R . . C27 C 0.5361(8) 0.5707(8) 0.8191(6) 0.101(2) Uani 1 1 d . . . H27A H 0.5982 0.5087 0.8492 0.152 Uiso 1 1 calc R . . H27B H 0.5911 0.6262 0.7856 0.152 Uiso 1 1 calc R . . H27C H 0.4469 0.5368 0.7662 0.152 Uiso 1 1 calc R . . C26 C 0.6082(9) 0.6486(7) 1.0038(6) 0.113(3) Uani 1 1 d . . . H26A H 0.5771 0.7038 1.0490 0.169 Uiso 1 1 calc R . . H26B H 0.7012 0.6801 0.9918 0.169 Uiso 1 1 calc R . . H26C H 0.6223 0.5742 1.0386 0.169 Uiso 1 1 calc R . . N6 N 0.7042(5) 0.4170(4) 0.5068(4) 0.0678(13) Uani 1 1 d . . . C28 C 0.6554(11) 0.4565(11) 0.5968(7) 0.151(4) Uani 1 1 d . . . H28A H 0.6874 0.4048 0.6556 0.226 Uiso 1 1 calc R . . H28B H 0.5474 0.4550 0.5758 0.226 Uiso 1 1 calc R . . H28C H 0.6986 0.5362 0.6192 0.226 Uiso 1 1 calc R . . C29 C 0.6611(11) 0.2997(7) 0.4693(9) 0.162(5) Uani 1 1 d . . . H29A H 0.7010 0.2834 0.4099 0.243 Uiso 1 1 calc R . . H29B H 0.5531 0.2873 0.4456 0.243 Uiso 1 1 calc R . . H29C H 0.6995 0.2473 0.5265 0.243 Uiso 1 1 calc R . . C30 C 0.7761(11) 0.4918(10) 0.4738(10) 0.154(5) Uani 1 1 d . . . H30 H 0.8092 0.4601 0.4182 0.184 Uiso 1 1 calc R . . O5 O 0.8172(8) 0.5912(5) 0.4895(5) 0.131(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02644(18) 0.0445(2) 0.03172(18) -0.00124(12) 0.00469(12) 0.00587(13) Cl1 0.0312(5) 0.0781(8) 0.0347(5) 0.0053(5) 0.0066(4) 0.0169(5) O1 0.050(2) 0.063(2) 0.0528(19) -0.0178(16) 0.0087(15) 0.0150(16) N3 0.0354(19) 0.053(2) 0.0350(18) -0.0062(15) 0.0023(15) 0.0006(17) C3 0.039(2) 0.047(3) 0.036(2) -0.0038(18) 0.0127(18) 0.0011(19) C20 0.029(2) 0.041(2) 0.048(2) 0.0000(18) 0.0117(17) 0.0001(18) N1 0.0318(18) 0.046(2) 0.0396(18) -0.0019(15) 0.0102(15) 0.0055(16) N2 0.0308(18) 0.052(2) 0.047(2) -0.0016(16) 0.0085(15) 0.0079(16) C2 0.032(2) 0.055(3) 0.059(3) -0.005(2) 0.010(2) -0.003(2) C6 0.030(2) 0.049(3) 0.052(3) 0.000(2) 0.0051(18) 0.0113(19) C1 0.035(2) 0.047(3) 0.050(2) 0.0008(19) 0.0113(19) 0.000(2) C5 0.040(2) 0.059(3) 0.049(3) -0.004(2) 0.006(2) 0.009(2) C7 0.051(3) 0.049(3) 0.062(3) -0.006(2) 0.013(2) -0.001(2) C4 0.046(3) 0.051(3) 0.056(3) 0.001(2) 0.010(2) -0.003(2) C8 0.045(3) 0.050(3) 0.069(3) 0.000(2) 0.012(2) 0.004(2) C10 0.052(3) 0.063(3) 0.046(3) -0.005(2) 0.005(2) 0.018(3) C9 0.055(3) 0.046(3) 0.074(3) -0.014(2) 0.002(3) 0.011(2) C11 0.054(3) 0.074(4) 0.064(3) 0.001(3) 0.022(3) 0.005(3) F1 0.094(3) 0.093(3) 0.066(2) -0.0177(18) 0.0167(18) 0.035(2) C12 0.030(2) 0.045(2) 0.035(2) -0.0025(17) 0.0057(16) 0.0031(18) C13 0.038(2) 0.054(3) 0.034(2) -0.0010(18) 0.0098(18) 0.001(2) C14 0.043(3) 0.084(4) 0.042(3) -0.016(2) -0.003(2) 0.003(3) C15 0.032(2) 0.050(3) 0.035(2) -0.0004(18) 0.0019(17) -0.0007(19) C19 0.033(2) 0.045(3) 0.048(2) -0.0031(19) 0.0087(18) 0.0045(19) C16 0.041(3) 0.057(3) 0.046(3) -0.001(2) -0.003(2) 0.004(2) C18 0.042(3) 0.048(3) 0.064(3) -0.002(2) 0.010(2) 0.009(2) C17 0.040(3) 0.052(3) 0.065(3) 0.006(2) -0.001(2) 0.010(2) N5 0.080(4) 0.073(3) 0.075(3) -0.006(3) 0.026(3) 0.009(3) O3 0.093(4) 0.109(5) 0.166(6) 0.028(4) 0.017(4) 0.041(4) C25 0.104(6) 0.071(5) 0.127(7) 0.010(4) 0.055(6) 0.022(4) C27 0.100(6) 0.125(7) 0.084(5) -0.018(4) 0.033(4) 0.017(5) C26 0.135(7) 0.098(6) 0.088(5) -0.010(4) 0.016(5) -0.038(5) N6 0.068(3) 0.058(3) 0.064(3) -0.005(2) -0.003(2) 0.004(2) C28 0.130(8) 0.204(12) 0.093(6) -0.022(6) -0.025(6) 0.078(8) C29 0.151(8) 0.079(6) 0.179(10) -0.042(6) -0.078(7) 0.015(6) C30 0.118(8) 0.109(8) 0.183(11) 0.054(7) -0.032(7) -0.031(6) O5 0.177(6) 0.075(4) 0.141(5) 0.004(3) 0.055(5) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C20 1.989(4) . ? Pd1 C12 2.034(4) . ? Pd1 Cl1 2.4295(11) . ? Pd1 Cl1 2.4774(11) 2_656 ? Cl1 Pd1 2.4774(11) 2_656 ? O1 C13 1.230(5) . ? N3 C13 1.381(6) . ? N3 C15 1.427(5) . ? N3 C14 1.470(5) . ? C3 N1 1.328(6) . ? C3 N2 1.355(5) . ? C3 C4 1.487(6) . ? C20 C19 1.399(6) . ? C20 C15 1.410(6) . ? N1 C1 1.383(5) . ? N1 C12 1.489(5) . ? N2 C2 1.364(6) . ? N2 C5 1.477(6) . ? C2 C1 1.337(6) . ? C2 H2 0.9500 . ? C6 C7 1.384(7) . ? C6 C8 1.392(7) . ? C6 C5 1.516(6) . ? C1 H1 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C11 1.388(7) . ? C7 H7 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C8 C9 1.400(7) . ? C8 H8 0.9500 . ? C10 C9 1.342(8) . ? C10 C11 1.363(8) . ? C10 F1 1.367(5) . ? C9 H9 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.508(6) . ? C12 H12 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.396(6) . ? C19 C18 1.380(6) . ? C19 H19 0.9500 . ? C16 C17 1.382(7) . ? C16 H16 0.9500 . ? C18 C17 1.373(7) . ? C18 H18 0.9500 . ? C17 H17 0.9500 . ? N5 C25 1.289(9) . ? N5 C27 1.443(8) . ? N5 C26 1.459(9) . ? O3 C25 1.251(10) . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N6 C30 1.216(11) . ? N6 C29 1.420(9) . ? N6 C28 1.465(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O5 1.176(11) . ? C30 H30 0.9500 . ? 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 C20 Pd1 C12 82.79(17) . . ? C20 Pd1 Cl1 95.11(12) . . ? C12 Pd1 Cl1 175.89(11) . . ? C20 Pd1 Cl1 168.93(12) . 2_656 ? C12 Pd1 Cl1 99.49(12) . 2_656 ? Cl1 Pd1 Cl1 83.24(4) . 2_656 ? Pd1 Cl1 Pd1 96.76(4) . 2_656 ? C13 N3 C15 123.7(3) . . ? C13 N3 C14 117.1(4) . . ? C15 N3 C14 119.2(4) . . ? N1 C3 N2 107.3(4) . . ? N1 C3 C4 128.2(4) . . ? N2 C3 C4 124.5(4) . . ? C19 C20 C15 117.2(4) . . ? C19 C20 Pd1 117.2(3) . . ? C15 C20 Pd1 125.5(3) . . ? C3 N1 C1 109.2(4) . . ? C3 N1 C12 128.2(4) . . ? C1 N1 C12 122.2(4) . . ? C3 N2 C2 108.5(4) . . ? C3 N2 C5 127.0(4) . . ? C2 N2 C5 124.5(4) . . ? C1 C2 N2 108.1(4) . . ? C1 C2 H2 126.0 . . ? N2 C2 H2 126.0 . . ? C7 C6 C8 119.6(4) . . ? C7 C6 C5 119.7(4) . . ? C8 C6 C5 120.7(4) . . ? C2 C1 N1 106.9(4) . . ? C2 C1 H1 126.6 . . ? N1 C1 H1 126.6 . . ? N2 C5 C6 112.4(4) . . ? N2 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C6 C7 C11 120.0(5) . . ? C6 C7 H7 120.0 . . ? C11 C7 H7 120.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C8 C9 119.5(5) . . ? C6 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C9 C10 C11 122.9(5) . . ? C9 C10 F1 119.1(5) . . ? C11 C10 F1 118.0(5) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C10 C11 C7 118.9(5) . . ? C10 C11 H11 120.6 . . ? C7 C11 H11 120.6 . . ? N1 C12 C13 110.8(3) . . ? N1 C12 Pd1 111.0(3) . . ? C13 C12 Pd1 112.2(3) . . ? N1 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? Pd1 C12 H12 107.5 . . ? O1 C13 N3 121.3(4) . . ? O1 C13 C12 123.1(4) . . ? N3 C13 C12 115.6(4) . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 119.8(4) . . ? C16 C15 N3 118.8(4) . . ? C20 C15 N3 121.4(4) . . ? C18 C19 C20 122.2(4) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C17 C18 C19 120.0(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C25 N5 C27 121.7(7) . . ? C25 N5 C26 122.0(7) . . ? C27 N5 C26 116.3(6) . . ? O3 C25 N5 124.9(8) . . ? O3 C25 H25 117.5 . . ? N5 C25 H25 117.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 N6 C29 128.9(10) . . ? C30 N6 C28 114.1(9) . . ? C29 N6 C28 117.0(8) . . ? N6 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C30 N6 139.4(14) . . ? O5 C30 H30 110.3 . . ? N6 C30 H30 110.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 Pd1 Cl1 Pd1 168.99(12) . . . 2_656 ? C12 Pd1 Cl1 Pd1 -131.9(18) . . . 2_656 ? Cl1 Pd1 Cl1 Pd1 0.0 2_656 . . 2_656 ? C12 Pd1 C20 C19 142.2(3) . . . . ? Cl1 Pd1 C20 C19 -41.4(3) . . . . ? Cl1 Pd1 C20 C19 39.5(8) 2_656 . . . ? C12 Pd1 C20 C15 -33.7(4) . . . . ? Cl1 Pd1 C20 C15 142.8(4) . . . . ? Cl1 Pd1 C20 C15 -136.3(5) 2_656 . . . ? N2 C3 N1 C1 -0.4(4) . . . . ? C4 C3 N1 C1 -178.2(4) . . . . ? N2 C3 N1 C12 172.3(4) . . . . ? C4 C3 N1 C12 -5.6(7) . . . . ? N1 C3 N2 C2 0.3(5) . . . . ? C4 C3 N2 C2 178.2(4) . . . . ? N1 C3 N2 C5 -179.5(4) . . . . ? C4 C3 N2 C5 -1.5(6) . . . . ? C3 N2 C2 C1 -0.1(5) . . . . ? C5 N2 C2 C1 179.7(4) . . . . ? N2 C2 C1 N1 -0.2(5) . . . . ? C3 N1 C1 C2 0.3(5) . . . . ? C12 N1 C1 C2 -172.8(4) . . . . ? C3 N2 C5 C6 -90.5(5) . . . . ? C2 N2 C5 C6 89.7(5) . . . . ? C7 C6 C5 N2 -74.2(5) . . . . ? C8 C6 C5 N2 107.5(5) . . . . ? C8 C6 C7 C11 -0.6(8) . . . . ? C5 C6 C7 C11 -178.9(5) . . . . ? C7 C6 C8 C9 1.6(7) . . . . ? C5 C6 C8 C9 179.9(4) . . . . ? C11 C10 C9 C8 1.8(8) . . . . ? F1 C10 C9 C8 -178.4(5) . . . . ? C6 C8 C9 C10 -2.2(8) . . . . ? C9 C10 C11 C7 -0.8(9) . . . . ? F1 C10 C11 C7 179.4(5) . . . . ? C6 C7 C11 C10 0.1(8) . . . . ? C3 N1 C12 C13 62.2(5) . . . . ? C1 N1 C12 C13 -126.0(4) . . . . ? C3 N1 C12 Pd1 -63.3(5) . . . . ? C1 N1 C12 Pd1 108.5(4) . . . . ? C20 Pd1 C12 N1 -173.1(3) . . . . ? Cl1 Pd1 C12 N1 127.4(17) . . . . ? Cl1 Pd1 C12 N1 -4.0(3) 2_656 . . . ? C20 Pd1 C12 C13 62.3(3) . . . . ? Cl1 Pd1 C12 C13 3(2) . . . . ? Cl1 Pd1 C12 C13 -128.7(3) 2_656 . . . ? C15 N3 C13 O1 -172.1(4) . . . . ? C14 N3 C13 O1 11.1(7) . . . . ? C15 N3 C13 C12 9.9(6) . . . . ? C14 N3 C13 C12 -167.0(4) . . . . ? N1 C12 C13 O1 -4.1(6) . . . . ? Pd1 C12 C13 O1 120.7(4) . . . . ? N1 C12 C13 N3 173.9(4) . . . . ? Pd1 C12 C13 N3 -61.3(4) . . . . ? C19 C20 C15 C16 3.2(6) . . . . ? Pd1 C20 C15 C16 179.1(3) . . . . ? C19 C20 C15 N3 -178.9(4) . . . . ? Pd1 C20 C15 N3 -3.0(6) . . . . ? C13 N3 C15 C16 -157.0(4) . . . . ? C14 N3 C15 C16 19.8(6) . . . . ? C13 N3 C15 C20 25.1(7) . . . . ? C14 N3 C15 C20 -158.2(4) . . . . ? C15 C20 C19 C18 -5.0(6) . . . . ? Pd1 C20 C19 C18 178.8(4) . . . . ? C20 C15 C16 C17 0.6(7) . . . . ? N3 C15 C16 C17 -177.4(4) . . . . ? C20 C19 C18 C17 2.9(7) . . . . ? C19 C18 C17 C16 1.1(8) . . . . ? C15 C16 C17 C18 -2.8(8) . . . . ? C27 N5 C25 O3 0.7(12) . . . . ? C26 N5 C25 O3 179.7(7) . . . . ? C29 N6 C30 O5 175.9(12) . . . . ? C28 N6 C30 O5 -3.2(17) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.169 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.117 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0