# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1833 data_zx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H19 Cl5 N2 O2 Pd' _chemical_formula_weight 777.17 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.359(2) _cell_length_b 13.218(3) _cell_length_c 14.597(3) _cell_angle_alpha 63.28(3) _cell_angle_beta 71.03(3) _cell_angle_gamma 75.74(3) _cell_volume 1676.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'OMEGA SCANS' _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description PRISM _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type SEMI-EMPIRICAL _exptl_absorpt_correction_T_min 0.8123 _exptl_absorpt_correction_T_max 0.8909 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SIMENS P4' _diffrn_measurement_method 'OMEGA SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.62 _diffrn_reflns_number 5104 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4846 _reflns_number_gt 4118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SIMENS XSCANS' _computing_cell_refinement 'SIMENS XSCANS' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4846 _refine_ls_number_parameters 409 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1997 _refine_ls_wR_factor_gt 0.1925 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 0.51979(3) -0.22129(2) -0.069622(19) 0.02937(7) Uani 1 1 d . . . Cl1 Cl -0.15779(11) 0.03156(12) -0.14153(10) 0.0735(5) Uani 1 1 d . . . Cl2 Cl 0.34984(13) -0.01667(12) -0.38405(8) 0.0707(5) Uani 1 1 d . . . Cl3 Cl 1.24535(12) -0.40746(12) -0.14936(10) 0.0765(5) Uani 1 1 d . . . Cl4 Cl 0.87713(12) -0.16309(11) -0.38313(8) 0.0630(4) Uani 1 1 d . . . C1 C 0.4176(3) -0.3924(3) 0.2059(2) 0.0270(9) Uani 1 1 d . . . C2 C 0.3666(3) -0.3844(3) 0.1266(3) 0.0349(10) Uani 1 1 d . . . C3 C 0.3333(4) -0.4832(3) 0.1263(3) 0.0412(11) Uani 1 1 d . . . H3A H 0.2973 -0.4769 0.0731 0.049 Uiso 1 1 calc R . . C4 C 0.3558(4) -0.5874(3) 0.2063(3) 0.0414(11) Uani 1 1 d . . . H4A H 0.3350 -0.6519 0.2062 0.050 Uiso 1 1 calc R . . C5 C 0.4087(4) -0.5993(3) 0.2873(3) 0.0412(12) Uani 1 1 d . . . C6 C 0.4368(5) -0.7064(4) 0.3690(3) 0.0618(16) Uani 1 1 d . . . H6A H 0.4156 -0.7712 0.3698 0.074 Uiso 1 1 calc R . . C7 C 0.4924(5) -0.7185(4) 0.4449(3) 0.0708(17) Uani 1 1 d . . . H7A H 0.5075 -0.7899 0.4981 0.085 Uiso 1 1 calc R . . C8 C 0.5268(5) -0.6221(4) 0.4422(3) 0.0592(15) Uani 1 1 d . . . H8A H 0.5679 -0.6309 0.4937 0.071 Uiso 1 1 calc R . . C9 C 0.5030(4) -0.5132(3) 0.3667(3) 0.0498(13) Uani 1 1 d . . . H9A H 0.5265 -0.4503 0.3678 0.060 Uiso 1 1 calc R . . C10 C 0.4423(3) -0.5007(3) 0.2881(2) 0.0333(10) Uani 1 1 d . . . C11 C 0.4467(3) -0.2865(2) 0.2055(2) 0.0265(9) Uani 1 1 d . . . C12 C 0.5507(3) -0.2267(3) 0.1261(2) 0.0305(10) Uani 1 1 d . . . C13 C 0.5854(4) -0.1285(3) 0.1246(3) 0.0415(12) Uani 1 1 d . . . H13A H 0.6577 -0.0909 0.0718 0.050 Uiso 1 1 calc R . . C14 C 0.5124(4) -0.0898(3) 0.2006(3) 0.0402(12) Uani 1 1 d . . . H14A H 0.5364 -0.0262 0.2002 0.048 Uiso 1 1 calc R . . C15 C 0.4004(4) -0.1444(3) 0.2807(2) 0.0346(10) Uani 1 1 d . . . C16 C 0.3164(4) -0.0993(3) 0.3572(2) 0.0401(11) Uani 1 1 d . . . H16A H 0.3379 -0.0348 0.3568 0.048 Uiso 1 1 calc R . . C17 C 0.2065(4) -0.1503(3) 0.4294(3) 0.0508(14) Uani 1 1 d . . . H17A H 0.1529 -0.1216 0.4793 0.061 Uiso 1 1 calc R . . C18 C 0.1730(4) -0.2474(3) 0.4291(3) 0.0483(14) Uani 1 1 d . . . H18A H 0.0961 -0.2810 0.4785 0.058 Uiso 1 1 calc R . . C19 C 0.2505(4) -0.2931(3) 0.3584(3) 0.0402(12) Uani 1 1 d . . . H19A H 0.2264 -0.3574 0.3603 0.048 Uiso 1 1 calc R . . C20 C 0.3675(3) -0.2430(3) 0.2820(2) 0.0327(10) Uani 1 1 d . . . N1 N 0.3503(3) -0.2783(2) 0.0375(2) 0.0340(9) Uani 1 1 d . . . C21 C 0.2270(3) -0.2380(3) 0.0234(3) 0.0389(11) Uani 1 1 d . . . H21A H 0.1540 -0.2688 0.0801 0.047 Uiso 1 1 calc R . . C22 C 0.1937(3) -0.1509(3) -0.0713(2) 0.0337(11) Uani 1 1 d . . . C23 C 0.0557(4) -0.1042(3) -0.0619(3) 0.0425(12) Uani 1 1 d . . . H23A H -0.0065 -0.1238 0.0041 0.051 Uiso 1 1 calc R . . C24 C 0.0134(4) -0.0285(3) -0.1525(3) 0.0443(13) Uani 1 1 d . . . C25 C 0.1017(4) -0.0043(3) -0.2518(3) 0.0506(13) Uani 1 1 d . . . H25A H 0.0701 0.0422 -0.3123 0.061 Uiso 1 1 calc R . . C26 C 0.2368(4) -0.0498(3) -0.2599(3) 0.0452(13) Uani 1 1 d . . . C27 C 0.2913(3) -0.1260(3) -0.1683(3) 0.0341(10) Uani 1 1 d . . . O1 O 0.4211(2) -0.1643(2) -0.18439(18) 0.0426(8) Uani 1 1 d . . . N2 N 0.6223(3) -0.2559(2) 0.0370(2) 0.0343(9) Uani 1 1 d . . . C28 C 0.7536(3) -0.2824(3) 0.0242(3) 0.0374(11) Uani 1 1 d . . . H28A H 0.7907 -0.2987 0.0801 0.045 Uiso 1 1 calc R . . C29 C 0.8473(3) -0.2882(3) -0.0732(3) 0.0387(11) Uani 1 1 d . . . C30 C 0.9817(4) -0.3433(3) -0.0663(3) 0.0455(12) Uani 1 1 d . . . H30A H 1.0036 -0.3804 -0.0011 0.055 Uiso 1 1 calc R . . C31 C 1.0798(4) -0.3417(4) -0.1574(3) 0.0506(14) Uani 1 1 d . . . C32 C 1.0479(4) -0.2834(3) -0.2552(3) 0.0504(14) Uani 1 1 d . . . H32A H 1.1159 -0.2788 -0.3167 0.060 Uiso 1 1 calc R . . C33 C 0.9161(4) -0.2323(3) -0.2618(3) 0.0425(12) Uani 1 1 d . . . C34 C 0.8102(4) -0.2308(3) -0.1712(3) 0.0358(11) Uani 1 1 d . . . O2 O 0.6898(2) -0.1780(2) -0.18467(18) 0.0378(8) Uani 1 1 d . . . C35 C -0.8637(11) 0.4004(10) -0.3938(8) 0.154(14) Uiso 0.25 1 d PD . . Cl5 Cl -1.0092(7) 0.4804(6) -0.3425(5) 0.102(2) Uiso 0.25 1 d PD A 1 Cl6 Cl -0.7862(6) 0.2894(5) -0.2973(5) 0.0951(19) Uiso 0.25 1 d PD A 1 Cl5' Cl -0.8680(9) 0.2575(8) -0.2671(7) 0.131(3) Uiso 0.25 1 d P A 2 Cl6' Cl -0.9566(13) 0.4620(11) -0.2837(10) 0.188(5) Uiso 0.25 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02488(10) 0.03412(10) 0.02995(9) -0.01473(7) -0.00621(7) -0.00207(9) Cl1 0.0416(5) 0.0844(8) 0.0733(6) -0.0181(6) -0.0263(4) 0.0176(5) Cl2 0.0680(7) 0.0831(8) 0.0379(4) -0.0118(5) -0.0124(4) 0.0043(6) Cl3 0.0368(5) 0.0987(8) 0.0840(7) -0.0447(6) -0.0096(5) 0.0175(6) Cl4 0.0518(6) 0.0760(7) 0.0419(4) -0.0222(4) 0.0007(4) 0.0054(5) C1 0.0222(13) 0.0252(13) 0.0282(12) -0.0103(10) -0.0019(11) -0.0003(12) C2 0.0239(14) 0.0436(16) 0.0427(14) -0.0239(11) -0.0068(11) -0.0024(13) C3 0.0494(17) 0.0387(15) 0.0515(14) -0.0242(11) -0.0223(12) -0.0069(14) C4 0.0431(17) 0.0370(16) 0.0535(16) -0.0234(12) -0.0179(13) -0.0025(14) C5 0.0421(17) 0.0294(16) 0.0510(17) -0.0144(13) -0.0174(14) 0.0019(15) C6 0.096(3) 0.0289(18) 0.058(2) -0.0139(15) -0.020(2) -0.008(2) C7 0.116(3) 0.040(2) 0.0574(19) -0.0075(17) -0.0516(18) 0.006(2) C8 0.084(2) 0.051(2) 0.0461(16) -0.0157(15) -0.0417(15) 0.012(2) C9 0.071(2) 0.0409(17) 0.0486(16) -0.0217(12) -0.0246(15) -0.0044(17) C10 0.0290(15) 0.0319(15) 0.0413(14) -0.0199(11) -0.0142(11) 0.0101(13) C11 0.0255(13) 0.0229(13) 0.0334(12) -0.0125(10) -0.0093(10) -0.0020(11) C12 0.0264(14) 0.0369(15) 0.0308(12) -0.0175(10) -0.0106(10) 0.0045(13) C13 0.0336(17) 0.0412(16) 0.0488(17) -0.0210(13) 0.0000(14) -0.0109(14) C14 0.0472(19) 0.0309(15) 0.0436(15) -0.0169(12) -0.0105(14) -0.0035(15) C15 0.0382(16) 0.0342(15) 0.0328(13) -0.0158(11) -0.0112(12) 0.0009(14) C16 0.0557(19) 0.0365(15) 0.0364(13) -0.0217(11) -0.0188(13) 0.0042(15) C17 0.063(2) 0.0453(17) 0.0470(16) -0.0300(13) -0.0040(17) -0.0007(18) C18 0.044(2) 0.0517(19) 0.0416(16) -0.0221(14) 0.0020(15) -0.0037(17) C19 0.0346(17) 0.0420(17) 0.0408(16) -0.0160(13) -0.0039(13) -0.0080(15) C20 0.0377(16) 0.0284(14) 0.0338(13) -0.0147(10) -0.0127(11) 0.0026(13) N1 0.0267(12) 0.0368(14) 0.0364(12) -0.0131(10) -0.0095(10) -0.0015(11) C21 0.0260(15) 0.0511(18) 0.0406(15) -0.0208(13) -0.0028(12) -0.0091(14) C22 0.0387(16) 0.0322(16) 0.0267(13) -0.0071(11) -0.0100(11) -0.0051(14) C23 0.0345(16) 0.0413(18) 0.0471(17) -0.0094(14) -0.0169(13) -0.0038(15) C24 0.0340(16) 0.047(2) 0.0479(16) -0.0149(14) -0.0227(13) 0.0107(16) C25 0.059(2) 0.044(2) 0.0514(17) -0.0118(15) -0.0313(14) 0.0002(17) C26 0.051(2) 0.0412(19) 0.0323(15) -0.0073(14) -0.0085(14) -0.0027(17) C27 0.0323(14) 0.0321(14) 0.0498(14) -0.0217(11) -0.0192(11) -0.0015(12) O1 0.0368(12) 0.0525(13) 0.0365(10) -0.0181(9) -0.0075(9) -0.0039(11) N2 0.0248(12) 0.0445(14) 0.0347(11) -0.0203(10) -0.0015(10) -0.0052(11) C28 0.0297(15) 0.0452(17) 0.0444(14) -0.0213(12) -0.0124(12) -0.0055(13) C29 0.0298(16) 0.0459(16) 0.0507(15) -0.0310(11) -0.0068(12) -0.0038(14) C30 0.0379(18) 0.0527(18) 0.0506(16) -0.0299(13) -0.0109(14) 0.0046(16) C31 0.0284(17) 0.063(2) 0.0560(19) -0.0302(15) -0.0008(15) 0.0020(17) C32 0.041(2) 0.058(2) 0.0470(17) -0.0282(14) 0.0088(16) -0.0101(17) C33 0.0338(17) 0.0494(18) 0.0463(16) -0.0241(13) -0.0042(13) -0.0062(15) C34 0.0334(16) 0.0364(15) 0.0411(14) -0.0217(11) -0.0010(12) -0.0091(13) O2 0.0328(11) 0.0426(12) 0.0352(10) -0.0166(8) -0.0033(9) -0.0047(10) _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 N1 1.975(3) . ? Pd1 N2 1.989(3) . ? Pd1 O2 1.990(2) . ? Pd1 O1 2.004(3) . ? Cl1 C24 1.743(4) . ? Cl2 C26 1.734(4) . ? Cl3 C31 1.736(4) . ? Cl4 C33 1.721(4) . ? C1 C2 1.374(6) . ? C1 C10 1.424(4) . ? C1 C11 1.500(5) . ? C2 C3 1.433(6) . ? C2 N1 1.440(4) . ? C3 C4 1.373(4) . ? C4 C5 1.391(6) . ? C5 C6 1.419(5) . ? C5 C10 1.436(6) . ? C6 C7 1.339(8) . ? C7 C8 1.387(8) . ? C8 C9 1.387(5) . ? C9 C10 1.408(6) . ? C11 C12 1.384(4) . ? C11 C20 1.414(5) . ? C12 C13 1.420(6) . ? C12 N2 1.439(5) . ? C13 C14 1.357(6) . ? C14 C15 1.417(5) . ? C15 C20 1.417(6) . ? C15 C16 1.439(5) . ? C16 C17 1.350(5) . ? C17 C18 1.410(7) . ? C18 C19 1.364(6) . ? C19 C20 1.415(5) . ? N1 C21 1.302(4) . ? C21 C22 1.427(4) . ? C22 C27 1.396(4) . ? C22 C23 1.399(5) . ? C23 C24 1.384(5) . ? C24 C25 1.380(5) . ? C25 C26 1.370(6) . ? C26 C27 1.455(5) . ? C27 O1 1.299(4) . ? N2 C28 1.291(4) . ? C28 C29 1.460(5) . ? C29 C30 1.416(5) . ? C29 C34 1.417(5) . ? C30 C31 1.381(5) . ? C31 C32 1.392(6) . ? C32 C33 1.380(5) . ? C33 C34 1.421(5) . ? C34 O2 1.300(4) . ? C35 Cl6 1.754(11) . ? C35 Cl5 1.773(11) . ? C35 Cl5' 1.958(12) . ? C35 Cl6' 1.99(2) . ? 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 Pd1 N2 94.14(12) . . ? N1 Pd1 O2 172.67(14) . . ? N2 Pd1 O2 89.96(11) . . ? N1 Pd1 O1 89.93(11) . . ? N2 Pd1 O1 172.16(12) . . ? O2 Pd1 O1 86.74(10) . . ? C2 C1 C10 120.2(4) . . ? C2 C1 C11 119.6(3) . . ? C10 C1 C11 120.2(3) . . ? C1 C2 C3 121.1(3) . . ? C1 C2 N1 122.1(4) . . ? C3 C2 N1 116.7(4) . . ? C4 C3 C2 118.6(4) . . ? C3 C4 C5 122.0(4) . . ? C4 C5 C6 123.1(4) . . ? C4 C5 C10 119.7(3) . . ? C6 C5 C10 117.2(4) . . ? C7 C6 C5 123.2(5) . . ? C6 C7 C8 118.4(4) . . ? C7 C8 C9 123.3(5) . . ? C8 C9 C10 118.1(4) . . ? C9 C10 C1 121.8(4) . . ? C9 C10 C5 119.9(3) . . ? C1 C10 C5 118.3(4) . . ? C12 C11 C20 118.5(3) . . ? C12 C11 C1 119.4(3) . . ? C20 C11 C1 122.0(3) . . ? C11 C12 C13 121.5(3) . . ? C11 C12 N2 121.8(4) . . ? C13 C12 N2 116.6(3) . . ? C14 C13 C12 119.6(3) . . ? C13 C14 C15 121.2(4) . . ? C14 C15 C20 118.7(3) . . ? C14 C15 C16 121.6(4) . . ? C20 C15 C16 119.6(3) . . ? C17 C16 C15 120.2(4) . . ? C16 C17 C18 119.9(4) . . ? C19 C18 C17 121.7(4) . . ? C18 C19 C20 120.3(4) . . ? C11 C20 C19 121.3(4) . . ? C11 C20 C15 120.3(3) . . ? C19 C20 C15 118.3(3) . . ? C21 N1 C2 117.9(3) . . ? C21 N1 Pd1 124.0(2) . . ? C2 N1 Pd1 116.9(2) . . ? N1 C21 C22 125.9(3) . . ? C27 C22 C23 123.1(3) . . ? C27 C22 C21 120.6(3) . . ? C23 C22 C21 115.9(3) . . ? C24 C23 C22 118.8(3) . . ? C25 C24 C23 121.5(3) . . ? C25 C24 Cl1 119.2(3) . . ? C23 C24 Cl1 119.2(3) . . ? C26 C25 C24 118.9(4) . . ? C25 C26 C27 123.0(3) . . ? C25 C26 Cl2 119.3(3) . . ? C27 C26 Cl2 117.7(3) . . ? O1 C27 C22 127.3(3) . . ? O1 C27 C26 118.2(3) . . ? C22 C27 C26 114.5(3) . . ? C27 O1 Pd1 120.9(2) . . ? C28 N2 C12 115.9(3) . . ? C28 N2 Pd1 125.3(3) . . ? C12 N2 Pd1 117.5(2) . . ? N2 C28 C29 123.7(4) . . ? C30 C29 C34 121.8(3) . . ? C30 C29 C28 116.2(3) . . ? C34 C29 C28 121.6(3) . . ? C31 C30 C29 119.4(4) . . ? C30 C31 C32 120.2(4) . . ? C30 C31 Cl3 119.5(3) . . ? C32 C31 Cl3 120.3(3) . . ? C33 C32 C31 120.4(3) . . ? C32 C33 C34 122.2(4) . . ? C32 C33 Cl4 119.9(3) . . ? C34 C33 Cl4 117.9(3) . . ? O2 C34 C29 125.8(3) . . ? O2 C34 C33 118.3(3) . . ? C29 C34 C33 115.9(3) . . ? C34 O2 Pd1 121.49(19) . . ? Cl6 C35 Cl5 114.2(7) . . ? Cl6 C35 Cl5' 28.2(4) . . ? Cl5 C35 Cl5' 98.8(5) . . ? Cl6 C35 Cl6' 86.1(7) . . ? Cl5 C35 Cl6' 32.4(5) . . ? Cl5' C35 Cl6' 80.8(6) . . ? _diffrn_measured_fraction_theta_max 0.737 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.737 _refine_diff_density_max 0.961 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.156 data_pdn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 Cl4 N2 O4 Pd' _chemical_formula_weight 830.87 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.317(2) _cell_length_b 13.332(3) _cell_length_c 13.668(3) _cell_angle_alpha 98.88(3) _cell_angle_beta 93.85(3) _cell_angle_gamma 102.00(3) _cell_volume 1807.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 5 _cell_measurement_theta_max 14 _exptl_crystal_description PRISM _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type SEMI-EMPERICAL _exptl_absorpt_correction_T_min 0.7722 _exptl_absorpt_correction_T_max 0.8757 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type P4 _diffrn_measurement_method 'OMEGA SCAN ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.82 _diffrn_reflns_number 4142 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.54 _reflns_number_total 3825 _reflns_number_gt 3825 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3825 _refine_ls_number_parameters 456 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2344 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.374 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.003 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 0.004405(14) 0.256555(9) 0.557677(8) 0.04780(4) Uani 1 1 d D . . Cl1 Cl -0.21715(8) 0.23307(6) 0.85114(4) 0.0894(2) Uani 1 1 d . . . Cl2 Cl -0.68006(8) 0.05778(6) 0.62622(5) 0.0878(2) Uani 1 1 d . . . Cl3 Cl 0.31827(15) 0.36854(10) 0.85177(7) 0.0773(4) Uani 0.50 1 d P A 1 Cl3' Cl 0.30420(15) 0.38853(11) 0.85139(8) 0.0746(4) Uani 0.50 1 d P A 2 Cl4 Cl 0.70563(7) 0.48708(6) 0.62513(5) 0.0794(2) Uani 1 1 d . A . N1 N -0.14781(19) 0.25360(12) 0.45708(10) 0.0558(5) Uani 1 1 d D . . N2 N 0.12670(18) 0.22502(12) 0.45613(10) 0.0530(5) Uani 1 1 d D . . O1 O -0.11517(16) 0.27093(10) 0.66585(9) 0.0579(4) Uani 1 1 d D . . O2 O 0.15392(16) 0.28130(11) 0.66546(9) 0.0570(4) Uani 1 1 d D . . C1 C -0.0150(2) 0.16278(14) 0.29939(12) 0.0507(5) Uani 1 1 d . . . C2 C 0.0685(2) 0.14377(13) 0.37270(12) 0.0537(6) Uani 1 1 d . . . C3 C 0.0961(2) 0.04640(15) 0.37223(16) 0.0599(6) Uani 1 1 d . . . H3A H 0.1561 0.0360 0.4215 0.072 Uiso 1 1 calc R . . C4 C 0.0326(3) -0.03648(15) 0.29681(17) 0.0730(8) Uani 1 1 d . . . H4A H 0.0478 -0.1027 0.2978 0.088 Uiso 1 1 calc R . . C5 C -0.0515(2) -0.02048(15) 0.22171(15) 0.0611(6) Uani 1 1 d D . . C6 C -0.1155(3) -0.11108(16) 0.14295(17) 0.0788(9) Uani 1 1 d D . . H6A H -0.0456 -0.1379 0.1108 0.095 Uiso 1 1 calc R . . H6B H -0.1636 -0.1654 0.1750 0.095 Uiso 1 1 calc R . . C7 C -0.2089(4) -0.0908(2) 0.0645(3) 0.1563(14) Uani 1 1 d D . . H7A H -0.1655 -0.0927 0.0036 0.188 Uiso 1 1 calc R . . H7B H -0.2859 -0.1486 0.0527 0.188 Uiso 1 1 calc R . . C8 C -0.2582(4) 0.0048(3) 0.0792(3) 0.1343(14) Uani 1 1 d D . . H8A H -0.2673 0.0259 0.0148 0.161 Uiso 1 1 calc R . . H8B H -0.3472 -0.0127 0.0997 0.161 Uiso 1 1 calc R . . C9 C -0.1844(3) 0.09556(19) 0.14921(15) 0.0767(8) Uani 1 1 d D . . H9A H -0.2481 0.1270 0.1849 0.092 Uiso 1 1 calc R . . H9B H -0.1399 0.1458 0.1111 0.092 Uiso 1 1 calc R . . C10 C -0.0825(2) 0.07835(14) 0.22420(13) 0.0562(6) Uani 1 1 d D . . C11 C -0.0414(2) 0.26872(12) 0.30126(12) 0.0503(5) Uani 1 1 d . . . C12 C 0.0095(2) 0.32673(15) 0.22975(12) 0.0546(6) Uani 1 1 d D . . C13 C 0.0971(3) 0.2878(2) 0.15680(14) 0.0762(8) Uani 1 1 d D . . H13A H 0.1832 0.2902 0.1915 0.091 Uiso 1 1 calc R . . H13B H 0.0578 0.2158 0.1281 0.091 Uiso 1 1 calc R . . C14 C 0.1164(4) 0.3500(2) 0.0757(2) 0.1471(12) Uani 1 1 d D . . H14A H 0.0411 0.3229 0.0255 0.176 Uiso 1 1 calc R . . H14B H 0.1949 0.3369 0.0453 0.176 Uiso 1 1 calc R . . C15 C 0.1319(4) 0.4668(2) 0.0996(2) 0.1038(11) Uani 1 1 d D . . H15A H 0.2184 0.4979 0.1363 0.125 Uiso 1 1 calc R . . H15B H 0.1284 0.4943 0.0381 0.125 Uiso 1 1 calc R . . C16 C 0.0273(3) 0.49542(16) 0.15880(15) 0.0870(10) Uani 1 1 d D . . H16A H -0.0489 0.4958 0.1133 0.104 Uiso 1 1 calc R . . H16B H 0.0600 0.5660 0.1945 0.104 Uiso 1 1 calc R . . C17 C -0.0204(2) 0.42675(13) 0.23322(13) 0.0566(6) Uani 1 1 d D . . C18 C -0.0944(3) 0.46285(15) 0.30623(16) 0.0620(6) Uani 1 1 d . . . H18A H -0.1147 0.5277 0.3067 0.074 Uiso 1 1 calc R . . C19 C -0.1386(3) 0.40634(16) 0.37762(14) 0.0631(6) Uani 1 1 d . . . H19A H -0.1865 0.4330 0.4267 0.076 Uiso 1 1 calc R . . C20 C -0.1107(2) 0.30834(14) 0.37561(12) 0.0536(5) Uani 1 1 d . . . C21 C -0.2678(2) 0.22866(14) 0.47112(12) 0.0526(5) Uani 1 1 d . . . H21A H -0.3297 0.2322 0.4198 0.063 Uiso 1 1 calc R . . C22 C -0.3203(2) 0.19485(14) 0.55887(14) 0.0520(5) Uani 1 1 d . . . C23 C -0.2388(2) 0.22167(15) 0.65161(14) 0.0557(6) Uani 1 1 d . . . C24 C -0.3065(2) 0.20143(15) 0.73464(13) 0.0572(6) Uani 1 1 d . . . C25 C -0.4409(2) 0.15316(17) 0.72992(16) 0.0628(6) Uani 1 1 d . . . H25A H -0.4812 0.1433 0.7876 0.075 Uiso 1 1 calc R . . C26 C -0.5152(3) 0.11921(16) 0.63406(16) 0.0656(7) Uani 1 1 d . . . C27 C -0.4551(3) 0.14275(15) 0.55207(16) 0.0619(6) Uani 1 1 d . . . H27A H -0.5044 0.1239 0.4900 0.074 Uiso 1 1 calc R . . C28 C 0.2533(2) 0.25864(13) 0.46834(14) 0.0526(5) Uani 1 1 d . . . H28A H 0.3010 0.2400 0.4157 0.063 Uiso 1 1 calc R . . C29 C 0.3288(2) 0.32362(14) 0.55795(12) 0.0512(5) Uani 1 1 d . . . C30 C 0.2736(2) 0.32372(12) 0.65172(13) 0.0522(5) Uani 1 1 d . A . C31 C 0.3673(3) 0.37714(16) 0.73457(14) 0.0603(6) Uani 1 1 d . . . C32 C 0.4961(3) 0.42408(17) 0.72627(16) 0.0640(7) Uani 1 1 d . A . H32A H 0.5536 0.4551 0.7832 0.077 Uiso 1 1 calc R . . C33 C 0.5410(2) 0.42551(18) 0.63337(15) 0.0621(7) Uani 1 1 d . . . C34 C 0.4584(2) 0.37411(15) 0.54935(15) 0.0593(6) Uani 1 1 d . A . O3 O 0.4729(4) 0.2322(3) 0.30334(19) 0.1434(15) Uani 1 1 d . . . O4 O 0.4851(4) 0.2077(2) 0.14314(19) 0.1204(11) Uani 1 1 d . . . C35 C 0.3596(9) 0.0768(4) 0.2074(3) 0.174(3) Uani 1 1 d . . . H35A H 0.3323 0.0601 0.2698 0.260 Uiso 1 1 calc R . . H35B H 0.4073 0.0271 0.1784 0.260 Uiso 1 1 calc R . . H35C H 0.2824 0.0749 0.1632 0.260 Uiso 1 1 calc R . . C36 C 0.4511(4) 0.1875(3) 0.2250(2) 0.1092(13) Uani 1 1 d . . . C37 C 0.5739(6) 0.3106(4) 0.1496(4) 0.145(2) Uani 1 1 d D . . H37A H 0.5298 0.3638 0.1789 0.174 Uiso 1 1 calc R . . H37B H 0.6539 0.3146 0.1929 0.174 Uiso 1 1 calc R . . C38 C 0.6087(9) 0.3297(6) 0.0569(4) 0.201(3) Uani 1 1 d D . . H38A H 0.6666 0.3974 0.0640 0.301 Uiso 1 1 calc R . . H38B H 0.5298 0.3271 0.0143 0.301 Uiso 1 1 calc R . . H38C H 0.6538 0.2779 0.0282 0.301 Uiso 1 1 calc R . . H34A H 0.4757(18) 0.3615(12) 0.4831(11) 0.027(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.05062(8) 0.04356(6) 0.04994(5) 0.00961(4) 0.00612(5) 0.01058(5) Cl1 0.0928(5) 0.1109(5) 0.0576(2) 0.0168(3) 0.0129(2) 0.0040(4) Cl2 0.0645(4) 0.0990(4) 0.0953(3) 0.0273(3) 0.0161(3) -0.0023(3) Cl3 0.0868(8) 0.0796(6) 0.0516(4) 0.0036(4) 0.0024(4) -0.0060(6) Cl3' 0.0814(8) 0.0828(6) 0.0576(4) 0.0082(4) 0.0131(4) 0.0149(5) Cl4 0.0599(3) 0.0873(4) 0.0798(3) 0.0093(3) 0.0061(2) -0.0048(3) N1 0.0696(11) 0.0496(7) 0.0477(6) 0.0101(5) 0.0094(6) 0.0098(7) N2 0.0615(10) 0.0458(6) 0.0477(6) 0.0046(5) 0.0019(6) 0.0070(6) O1 0.0631(8) 0.0522(6) 0.0569(6) 0.0088(5) 0.0134(5) 0.0077(6) O2 0.0588(8) 0.0633(7) 0.0467(5) 0.0115(5) 0.0037(5) 0.0072(6) C1 0.0496(10) 0.0508(7) 0.0564(7) 0.0192(6) 0.0143(7) 0.0120(7) C2 0.0703(12) 0.0385(7) 0.0466(7) -0.0017(6) 0.0053(7) 0.0058(7) C3 0.0635(13) 0.0436(8) 0.0696(9) 0.0102(7) 0.0029(8) 0.0059(8) C4 0.1079(17) 0.0334(7) 0.0769(11) 0.0011(8) 0.0018(11) 0.0226(8) C5 0.0572(12) 0.0507(9) 0.0730(10) 0.0007(8) 0.0091(8) 0.0127(8) C6 0.099(2) 0.0412(9) 0.0830(12) -0.0050(9) -0.0016(12) 0.0006(10) C7 0.198(3) 0.0674(14) 0.176(2) -0.0308(16) -0.1123(18) 0.0477(16) C8 0.119(2) 0.100(2) 0.153(2) -0.0163(19) -0.0760(16) 0.0097(19) C9 0.0924(17) 0.0729(12) 0.0612(10) -0.0014(9) -0.0079(10) 0.0248(11) C10 0.0633(12) 0.0436(8) 0.0572(8) 0.0036(6) 0.0012(8) 0.0069(8) C11 0.0651(11) 0.0402(7) 0.0498(7) 0.0080(5) 0.0044(7) 0.0217(6) C12 0.0572(11) 0.0557(9) 0.0512(7) 0.0100(6) 0.0070(7) 0.0122(7) C13 0.0856(14) 0.0879(13) 0.0605(8) 0.0240(8) 0.0310(8) 0.0159(11) C14 0.263(3) 0.0593(12) 0.1525(15) 0.0445(11) 0.1408(13) 0.0552(15) C15 0.130(2) 0.1134(15) 0.0958(12) 0.0594(10) 0.0439(13) 0.0484(14) C16 0.127(2) 0.0574(10) 0.0778(10) 0.0369(7) 0.0096(12) 0.0050(12) C17 0.0675(12) 0.0401(7) 0.0614(7) 0.0192(6) 0.0025(8) 0.0040(7) C18 0.0669(13) 0.0517(8) 0.0718(9) 0.0170(7) 0.0077(9) 0.0179(8) C19 0.0770(13) 0.0654(9) 0.0563(8) 0.0189(7) 0.0105(8) 0.0294(8) C20 0.0620(11) 0.0486(8) 0.0527(7) 0.0170(6) 0.0095(7) 0.0110(7) C21 0.0580(10) 0.0540(8) 0.0515(7) 0.0138(6) 0.0124(6) 0.0194(7) C22 0.0472(11) 0.0472(8) 0.0633(8) 0.0168(6) 0.0075(7) 0.0087(7) C23 0.0572(11) 0.0502(8) 0.0624(8) 0.0156(6) 0.0094(7) 0.0130(7) C24 0.0623(12) 0.0554(8) 0.0580(7) 0.0164(7) 0.0142(7) 0.0149(8) C25 0.0597(12) 0.0583(9) 0.0737(9) 0.0166(8) 0.0219(8) 0.0120(8) C26 0.0674(14) 0.0574(9) 0.0766(10) 0.0243(8) 0.0146(9) 0.0124(9) C27 0.0675(13) 0.0487(8) 0.0708(9) 0.0172(7) 0.0057(9) 0.0110(8) C28 0.0578(11) 0.0368(7) 0.0613(8) 0.0036(6) 0.0071(7) 0.0096(7) C29 0.0534(10) 0.0516(8) 0.0516(7) 0.0098(6) 0.0067(7) 0.0170(7) C30 0.0687(11) 0.0326(6) 0.0544(7) 0.0026(6) -0.0001(7) 0.0153(6) C31 0.0666(13) 0.0576(9) 0.0566(8) 0.0100(7) 0.0045(8) 0.0142(8) C32 0.0622(13) 0.0583(10) 0.0647(9) 0.0039(8) -0.0076(9) 0.0074(9) C33 0.0420(12) 0.0708(12) 0.0662(9) 0.0032(9) -0.0014(8) 0.0043(9) C34 0.0628(13) 0.0466(8) 0.0639(9) 0.0036(7) 0.0066(8) 0.0062(8) O3 0.153(3) 0.178(3) 0.0822(12) -0.0115(15) -0.0041(15) 0.028(2) O4 0.156(2) 0.1081(16) 0.0929(12) 0.0135(11) 0.0155(14) 0.0218(16) C35 0.278(7) 0.136(3) 0.124(2) 0.0622(19) 0.066(3) 0.038(4) C36 0.138(3) 0.133(2) 0.0744(13) 0.0237(13) 0.0126(15) 0.0666(16) C37 0.115(4) 0.136(4) 0.153(4) 0.002(3) 0.008(3) -0.019(3) C38 0.242(7) 0.178(6) 0.183(4) 0.042(4) 0.097(4) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.9926(18) . ? Pd1 O2 1.9980(15) . ? Pd1 O1 2.0000(16) . ? Pd1 N1 2.0064(18) . ? Cl1 C24 1.731(2) . ? Cl2 C26 1.716(3) . ? Cl3 C31 1.725(2) . ? Cl3' C31 1.761(2) . ? Cl4 C33 1.745(2) . ? N1 C21 1.249(3) . ? N1 C20 1.453(2) . ? N2 C28 1.280(3) . ? N2 C2 1.446(2) . ? O1 C23 1.294(3) . ? O2 C30 1.285(3) . ? C1 C2 1.365(3) . ? C1 C10 1.424(2) . ? C1 C11 1.490(3) . ? C2 C3 1.385(3) . ? C3 C4 1.403(3) . ? C4 C5 1.370(4) . ? C5 C10 1.415(3) . ? C5 C6 1.492(3) . ? C6 C7 1.488(5) . ? C7 C8 1.457(5) . ? C8 C9 1.457(4) . ? C9 C10 1.496(3) . ? C11 C20 1.383(3) . ? C11 C12 1.401(3) . ? C12 C17 1.424(3) . ? C12 C13 1.496(3) . ? C13 C14 1.484(4) . ? C14 C15 1.512(4) . ? C15 C16 1.470(5) . ? C16 C17 1.511(3) . ? C17 C18 1.385(3) . ? C18 C19 1.368(3) . ? C19 C20 1.392(3) . ? C21 C22 1.445(3) . ? C22 C27 1.409(3) . ? C22 C23 1.426(3) . ? C23 C24 1.404(3) . ? C24 C25 1.394(3) . ? C25 C26 1.431(3) . ? C26 C27 1.364(3) . ? C28 C29 1.456(2) . ? C29 C34 1.388(3) . ? C29 C30 1.437(3) . ? C30 C31 1.429(3) . ? C31 C32 1.366(3) . ? C32 C33 1.382(3) . ? C33 C34 1.378(3) . ? O3 C36 1.126(4) . ? O4 C36 1.246(4) . ? O4 C37 1.468(6) . ? C35 C36 1.551(7) . ? C37 C38 1.387(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 O2 90.05(7) . . ? N2 Pd1 O1 172.40(7) . . ? O2 Pd1 O1 86.97(6) . . ? N2 Pd1 N1 94.46(7) . . ? O2 Pd1 N1 171.42(6) . . ? O1 Pd1 N1 89.41(7) . . ? C21 N1 C20 119.43(19) . . ? C21 N1 Pd1 124.27(13) . . ? C20 N1 Pd1 114.50(14) . . ? C28 N2 C2 118.97(18) . . ? C28 N2 Pd1 124.34(12) . . ? C2 N2 Pd1 115.64(14) . . ? C23 O1 Pd1 120.36(12) . . ? C30 O2 Pd1 121.09(12) . . ? C2 C1 C10 118.87(18) . . ? C2 C1 C11 120.60(15) . . ? C10 C1 C11 120.44(17) . . ? C1 C2 C3 121.83(16) . . ? C1 C2 N2 120.22(18) . . ? C3 C2 N2 117.90(18) . . ? C2 C3 C4 119.5(2) . . ? C5 C4 C3 120.4(2) . . ? C4 C5 C10 119.79(17) . . ? C4 C5 C6 118.3(2) . . ? C10 C5 C6 121.8(2) . . ? C7 C6 C5 116.4(2) . . ? C8 C7 C6 119.9(3) . . ? C9 C8 C7 120.3(3) . . ? C8 C9 C10 117.3(3) . . ? C5 C10 C1 119.27(19) . . ? C5 C10 C9 121.15(17) . . ? C1 C10 C9 119.58(19) . . ? C20 C11 C12 122.04(17) . . ? C20 C11 C1 119.12(16) . . ? C12 C11 C1 118.79(17) . . ? C11 C12 C17 116.84(18) . . ? C11 C12 C13 121.5(2) . . ? C17 C12 C13 121.59(19) . . ? C14 C13 C12 112.2(3) . . ? C13 C14 C15 119.4(2) . . ? C16 C15 C14 111.8(3) . . ? C15 C16 C17 116.5(2) . . ? C18 C17 C12 119.83(18) . . ? C18 C17 C16 118.7(2) . . ? C12 C17 C16 121.5(2) . . ? C19 C18 C17 122.2(2) . . ? C18 C19 C20 118.9(2) . . ? C11 C20 C19 120.04(18) . . ? C11 C20 N1 121.73(18) . . ? C19 C20 N1 118.08(18) . . ? N1 C21 C22 126.71(19) . . ? C27 C22 C23 121.37(19) . . ? C27 C22 C21 118.69(18) . . ? C23 C22 C21 119.75(18) . . ? O1 C23 C24 118.80(17) . . ? O1 C23 C22 126.04(19) . . ? C24 C23 C22 114.78(19) . . ? C25 C24 C23 124.54(18) . . ? C25 C24 Cl1 116.91(16) . . ? C23 C24 Cl1 118.49(17) . . ? C24 C25 C26 118.3(2) . . ? C27 C26 C25 118.9(2) . . ? C27 C26 Cl2 121.84(18) . . ? C25 C26 Cl2 119.16(18) . . ? C26 C27 C22 121.8(2) . . ? N2 C28 C29 125.36(19) . . ? C34 C29 C30 122.95(16) . . ? C34 C29 C28 116.94(18) . . ? C30 C29 C28 119.72(18) . . ? O2 C30 C31 120.32(17) . . ? O2 C30 C29 126.62(16) . . ? C31 C30 C29 113.05(19) . . ? C32 C31 C30 123.9(2) . . ? C32 C31 Cl3 118.70(16) . . ? C30 C31 Cl3 117.00(18) . . ? C32 C31 Cl3' 120.12(16) . . ? C30 C31 Cl3' 115.81(18) . . ? Cl3 C31 Cl3' 10.78(7) . . ? C31 C32 C33 120.07(19) . . ? C34 C33 C32 120.0(2) . . ? C34 C33 Cl4 120.94(18) . . ? C32 C33 Cl4 119.00(16) . . ? C33 C34 C29 119.9(2) . . ? C36 O4 C37 113.9(3) . . ? O3 C36 O4 133.4(4) . . ? O3 C36 C35 118.2(4) . . ? O4 C36 C35 108.4(3) . . ? C38 C37 O4 111.8(5) . . ? _diffrn_measured_fraction_theta_max 0.565 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 0.565 _refine_diff_density_max 0.993 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.110