Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Martin Broring' _publ_contact_author_address ; Fachbereich Chemie Philipps-Universitat Marburg Hans-Meerwein-Strasse Marburg D-35032 GERMANY ; _publ_contact_author_email MARTIN.BROERING@CHEMIE.UNI-MARBURG.DE _publ_section_title ; Cyclometalation vs. Werner-type coordination of sterically enforced palladium(II)-1,3-bis(pyridyl-2-imino)isoindolines (Pd-BPIs) ; loop_ _publ_author_name M.Broring C.Kleeberg # Attachment 'structures.cif' data_ck7ck _database_code_depnum_ccdc_archive 'CCDC 626407' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H23 N5 O2 Pd, C H2 Cl2, O0.21 H0.42' _chemical_formula_sum 'C25 H25.42 Cl2 N5 O2.21 Pd' _chemical_formula_weight 608.62 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6799(16) _cell_length_b 14.5846(18) _cell_length_c 15.753(2) _cell_angle_alpha 115.166(14) _cell_angle_beta 100.800(14) _cell_angle_gamma 96.971(15) _cell_volume 2522.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1281 _exptl_absorpt_coefficient_mu 0.974 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.71822 _exptl_absorpt_correction_T_max 0.89016 _exptl_absorpt_process_details 'XPREP 6.13' _exptl_special_details ; The asymmetric unit contains two dichlormethane molecules (one of them is disordered (48:52)) and 0.42 molecules of water. One of two acetate groups in the asymmetrich unit is disordered (34:66) and a combined ADP is refined. The hydrogen atoms of the water molecule were refined employing restraints (DFIX, DANG) idealizing the geometry. ; _diffrn_ambient_temperature 193(2) _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 'IPDS-1 (Stoe)' _diffrn_measurement_method phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22917 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8379 _reflns_number_gt 6497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX v1.64.05' _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^)+(0.0658P)^2^+2.9188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8379 _refine_ls_number_parameters 677 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _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 0.3773(5) 0.2079(6) 0.0047(4) 0.062(2) Uani 1 1 d . . . H1A H 0.3458 0.1344 -0.0169 0.093 Uiso 1 1 calc R . . H1B H 0.3924 0.2464 0.0756 0.093 Uiso 1 1 calc R . . H1C H 0.4461 0.2145 -0.0142 0.093 Uiso 1 1 calc R . . C2 C 0.2971(4) 0.2516(4) -0.0416(3) 0.0381(13) Uani 1 1 d . . . C3 C 0.2814(4) 0.3501(4) 0.0116(4) 0.0428(14) Uani 1 1 d . . . H3 H 0.3291 0.3929 0.0749 0.051 Uiso 1 1 calc R . . C4 C 0.1991(4) 0.3885(4) -0.0238(4) 0.0386(13) Uani 1 1 d . . . C5 C 0.1835(5) 0.4953(4) 0.0348(4) 0.0562(16) Uani 1 1 d . . . H5A H 0.2165 0.5182 0.1040 0.084 Uiso 1 1 calc R . . H5B H 0.1046 0.4941 0.0238 0.084 Uiso 1 1 calc R . . H5C H 0.2193 0.5434 0.0149 0.084 Uiso 1 1 calc R . . C6 C 0.1284(4) 0.3207(4) -0.1139(3) 0.0323(11) Uani 1 1 d . . . H6 H 0.0675 0.3417 -0.1399 0.039 Uiso 1 1 calc R . . C7 C 0.1453(4) 0.2216(3) -0.1672(3) 0.0263(10) Uani 1 1 d . . . C8 C 0.0549(3) 0.0607(3) -0.3035(3) 0.0229(9) Uani 1 1 d . . . C9 C -0.0379(3) -0.0033(3) -0.3917(3) 0.0230(9) Uani 1 1 d . . . C10 C -0.1341(4) 0.0192(4) -0.4268(3) 0.0299(11) Uani 1 1 d . . . H10 H -0.1519 0.0842 -0.3928 0.036 Uiso 1 1 calc R . . C11 C -0.2041(4) -0.0584(4) -0.5147(3) 0.0315(11) Uani 1 1 d . . . H11 H -0.2704 -0.0453 -0.5422 0.038 Uiso 1 1 calc R . . C12 C -0.1790(4) -0.1538(4) -0.5628(3) 0.0326(11) Uani 1 1 d . . . H12 H -0.2284 -0.2049 -0.6225 0.039 Uiso 1 1 calc R . . C13 C -0.0831(4) -0.1764(4) -0.5255(3) 0.0296(10) Uani 1 1 d . . . H13 H -0.0663 -0.2424 -0.5578 0.036 Uiso 1 1 calc R . . C14 C -0.0128(3) -0.0984(3) -0.4389(3) 0.0234(9) Uani 1 1 d . . . C15 C 0.0962(3) -0.0940(3) -0.3817(3) 0.0243(10) Uani 1 1 d . . . C16 C 0.2509(4) -0.1686(4) -0.3652(3) 0.0286(10) Uani 1 1 d . . . C17 C 0.2798(4) -0.2639(4) -0.4070(4) 0.0350(11) Uani 1 1 d . . . H17 H 0.2324 -0.3181 -0.4661 0.042 Uiso 1 1 calc R . . C18 C 0.3757(4) -0.2816(4) -0.3649(4) 0.0382(12) Uani 1 1 d . . . C19 C 0.4062(5) -0.3852(5) -0.4080(5) 0.0569(16) Uani 1 1 d . . . H19A H 0.3394 -0.4400 -0.4478 0.085 Uiso 1 1 calc R . . H19B H 0.4434 -0.3988 -0.3555 0.085 Uiso 1 1 calc R . . H19C H 0.4557 -0.3844 -0.4486 0.085 Uiso 1 1 calc R . . C20 C 0.4393(4) -0.2009(4) -0.2768(4) 0.0377(12) Uani 1 1 d . . . H20 H 0.5044 -0.2106 -0.2437 0.045 Uiso 1 1 calc R . . C21 C 0.4094(4) -0.1070(4) -0.2367(4) 0.0345(11) Uani 1 1 d . . . C22 C 0.4772(5) -0.0277(5) -0.1362(4) 0.0509(15) Uani 1 1 d . . . H22A H 0.5256 -0.0608 -0.1079 0.076 Uiso 1 1 calc R . . H22B H 0.4280 -0.0001 -0.0950 0.076 Uiso 1 1 calc R . . H22C H 0.5218 0.0292 -0.1403 0.076 Uiso 1 1 calc R . . C23 C 0.4662(4) 0.1854(4) -0.2206(4) 0.0388(13) Uani 1 1 d . . . C24 C 0.5837(5) 0.2496(5) -0.1821(5) 0.0582(17) Uani 1 1 d . B . H24A H 0.6351 0.2038 -0.1861 0.087 Uiso 1 1 calc R . . H24B H 0.5960 0.3012 -0.1142 0.087 Uiso 1 1 calc R . . H24C H 0.5958 0.2852 -0.2212 0.087 Uiso 1 1 calc R . . C25 C 0.9892(4) 0.6502(4) 0.6154(4) 0.0386(12) Uani 1 1 d . . . H25A H 0.9270 0.6027 0.6148 0.058 Uiso 1 1 calc R . . H25B H 1.0361 0.6099 0.5787 0.058 Uiso 1 1 calc R . . H25C H 0.9614 0.6924 0.5855 0.058 Uiso 1 1 calc R . . C26 C 1.0551(4) 0.7201(4) 0.7185(4) 0.0321(11) Uani 1 1 d . . . C27 C 1.1499(4) 0.6972(4) 0.7542(4) 0.0362(12) Uani 1 1 d . . . H27 H 1.1683 0.6339 0.7156 0.043 Uiso 1 1 calc R . . C28 C 1.2200(4) 0.7647(4) 0.8460(4) 0.0385(12) Uani 1 1 d . . . C29 C 1.3208(5) 0.7375(5) 0.8885(5) 0.0522(15) Uani 1 1 d . . . H29A H 1.3656 0.7989 0.9476 0.078 Uiso 1 1 calc R . . H29B H 1.3642 0.7146 0.8410 0.078 Uiso 1 1 calc R . . H29C H 1.2983 0.6815 0.9046 0.078 Uiso 1 1 calc R . . C30 C 1.1929(4) 0.8574(4) 0.8950(4) 0.0328(11) Uani 1 1 d . . . H30 H 1.2412 0.9076 0.9557 0.039 Uiso 1 1 calc R . . C31 C 1.0972(4) 0.8802(4) 0.8587(3) 0.0269(10) Uani 1 1 d . . . C32 C 1.0083(3) 1.0207(4) 0.8884(3) 0.0250(10) Uani 1 1 d . . . C33 C 1.0023(3) 1.1283(3) 0.9507(3) 0.0248(10) Uani 1 1 d . . . C34 C 1.0692(4) 1.2036(4) 1.0400(3) 0.0313(11) Uani 1 1 d . . . H34 H 1.1342 1.1915 1.0707 0.038 Uiso 1 1 calc R . . C35 C 1.0382(4) 1.2969(4) 1.0831(3) 0.0348(11) Uani 1 1 d . . . H35 H 1.0828 1.3498 1.1443 0.042 Uiso 1 1 calc R . . C36 C 0.9431(4) 1.3147(4) 1.0385(4) 0.0363(12) Uani 1 1 d . . . H36 H 0.9242 1.3799 1.0694 0.044 Uiso 1 1 calc R . . C37 C 0.8752(4) 1.2389(4) 0.9495(3) 0.0326(11) Uani 1 1 d . . . H37 H 0.8101 1.2508 0.9186 0.039 Uiso 1 1 calc R . . C38 C 0.9062(4) 1.1452(4) 0.9075(3) 0.0272(10) Uani 1 1 d . . . C39 C 0.8505(4) 1.0467(4) 0.8183(3) 0.0272(10) Uani 1 1 d . . . C40 C 0.6931(4) 0.9418(4) 0.6874(3) 0.0297(10) Uani 1 1 d . . . C41 C 0.5950(4) 0.9523(4) 0.6395(4) 0.0339(11) Uani 1 1 d . . . H41 H 0.5719 1.0157 0.6680 0.041 Uiso 1 1 calc R . . C42 C 0.5307(4) 0.8739(4) 0.5522(4) 0.0368(12) Uani 1 1 d . . . C43 C 0.4262(4) 0.8858(5) 0.4986(4) 0.0502(15) Uani 1 1 d . . . H43A H 0.3647 0.8302 0.4865 0.075 Uiso 1 1 calc R . . H43B H 0.4343 0.8815 0.4364 0.075 Uiso 1 1 calc R . . H43C H 0.4115 0.9535 0.5379 0.075 Uiso 1 1 calc R . . C44 C 0.5700(4) 0.7848(4) 0.5148(4) 0.0384(12) Uani 1 1 d . . . H44 H 0.5302 0.7296 0.4529 0.046 Uiso 1 1 calc R . . C45 C 0.6652(4) 0.7730(4) 0.5641(3) 0.0326(11) Uani 1 1 d . . . C46 C 0.7042(5) 0.6759(4) 0.5147(4) 0.0448(14) Uani 1 1 d . . . H46A H 0.6725 0.6450 0.4443 0.067 Uiso 1 1 calc R . . H46B H 0.6809 0.6264 0.5382 0.067 Uiso 1 1 calc R . . H46C H 0.7848 0.6926 0.5294 0.067 Uiso 1 1 calc R . . C47 C 0.7241(4) 0.6558(4) 0.7254(3) 0.0333(11) Uani 1 1 d . . . C48 C 0.6889(5) 0.5423(4) 0.6993(4) 0.0496(15) Uani 1 1 d . . . H48A H 0.6107 0.5165 0.6638 0.074 Uiso 1 1 calc R . . H48B H 0.7003 0.5345 0.7589 0.074 Uiso 1 1 calc R . . H48C H 0.7328 0.5023 0.6584 0.074 Uiso 1 1 calc R . . C49 C -0.0876(4) 0.3047(4) -0.3361(4) 0.0394(12) Uani 1 1 d . . . H49A H -0.1181 0.2596 -0.4069 0.047 Uiso 1 1 calc R . . H49B H -0.0266 0.2776 -0.3127 0.047 Uiso 1 1 calc R . . C50 C 0.6433(7) 0.5854(8) 0.1966(8) 0.107(3) Uani 1 1 d . . . H50A H 0.6444 0.6606 0.2271 0.129 Uiso 1 1 calc R A 3 H50B H 0.6320 0.5596 0.1256 0.129 Uiso 1 1 calc R A 3 N1 N 0.2341(3) 0.1905(3) -0.1360(3) 0.0275(9) Uani 1 1 d . B . N2 N 0.0622(3) 0.1586(3) -0.2516(3) 0.0242(8) Uani 1 1 d . . . N3 N 0.1261(3) -0.0014(3) -0.2972(2) 0.0251(8) Uani 1 1 d . B . N4 N 0.1495(3) -0.1663(3) -0.4142(3) 0.0281(9) Uani 1 1 d . . . N5 N 0.3186(3) -0.0870(3) -0.2816(3) 0.0269(8) Uani 1 1 d . B . N6 N 1.0233(3) 0.8088(3) 0.7726(3) 0.0263(8) Uani 1 1 d . . . N7 N 1.0845(3) 0.9793(3) 0.9139(3) 0.0273(9) Uani 1 1 d . . . N8 N 0.9187(3) 0.9790(3) 0.8057(3) 0.0256(8) Uani 1 1 d . . . N9 N 0.7518(3) 1.0331(3) 0.7695(3) 0.0311(9) Uani 1 1 d . . . N10 N 0.7259(3) 0.8501(3) 0.6539(3) 0.0283(9) Uani 1 1 d . . . O1 O 0.4421(3) 0.1386(3) -0.1726(2) 0.0386(9) Uani 1 1 d . B . O2 O 0.393(3) 0.193(2) -0.285(3) 0.071(10) Uani 0.34(12) 1 d P B 1 O2' O 0.412(3) 0.174(3) -0.2943(16) 0.097(7) Uani 0.66(12) 1 d P B 2 O3 O 0.8034(3) 0.6741(2) 0.6903(2) 0.0323(8) Uani 1 1 d . . . O4 O 0.6795(3) 0.7196(3) 0.7755(3) 0.0482(10) Uani 1 1 d . . . Pd1 Pd 0.28023(3) 0.05801(3) -0.22057(2) 0.02488(11) Uani 1 1 d . . . Pd2 Pd 0.86687(3) 0.82797(3) 0.72765(2) 0.02519(11) Uani 1 1 d . . . Cl1 Cl -0.19027(15) 0.30028(14) -0.27700(13) 0.0689(5) Uani 1 1 d . . . Cl2 Cl -0.0362(2) 0.43214(15) -0.3145(2) 0.0956(7) Uani 1 1 d . . . Cl3 Cl 0.7657(2) 0.56203(19) 0.24798(19) 0.1004(7) Uani 1 1 d . C . Cl4 Cl 0.5427(4) 0.5182(5) 0.2202(4) 0.105(2) Uani 0.476(7) 1 d P C 3 Cl4' Cl 0.5523(5) 0.4967(5) 0.0939(8) 0.196(6) Uani 0.524(7) 1 d P C 4 O5 O 0.7284(8) 0.9314(8) 0.9125(8) 0.055(4) Uani 0.422(13) 1 d PD . . H51A H 0.710(11) 0.861(5) 0.861(8) 0.065 Uiso 0.422(13) 1 d PD . . H51B H 0.800(6) 0.940(10) 0.950(9) 0.065 Uiso 0.422(13) 1 d PD . . 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 0.057(4) 0.094(5) 0.015(2) 0.006(3) -0.004(2) 0.043(4) C2 0.024(2) 0.049(3) 0.024(2) 0.004(2) -0.0009(19) 0.010(2) C3 0.030(3) 0.049(3) 0.025(2) 0.001(2) -0.002(2) 0.001(2) C4 0.041(3) 0.032(3) 0.028(3) 0.006(2) 0.004(2) -0.003(2) C5 0.064(4) 0.036(3) 0.041(3) 0.002(3) -0.002(3) 0.001(3) C6 0.033(2) 0.031(3) 0.029(2) 0.012(2) 0.003(2) 0.005(2) C7 0.029(2) 0.025(2) 0.020(2) 0.0085(19) 0.0038(18) 0.0020(19) C8 0.020(2) 0.028(2) 0.018(2) 0.0095(19) 0.0026(16) 0.0022(18) C9 0.025(2) 0.025(2) 0.016(2) 0.0093(18) 0.0015(16) 0.0020(18) C10 0.030(2) 0.032(3) 0.027(2) 0.014(2) 0.0030(19) 0.006(2) C11 0.023(2) 0.043(3) 0.025(2) 0.017(2) -0.0039(18) 0.003(2) C12 0.028(2) 0.038(3) 0.018(2) 0.006(2) -0.0036(18) -0.003(2) C13 0.029(2) 0.031(3) 0.021(2) 0.007(2) 0.0045(18) 0.005(2) C14 0.020(2) 0.032(2) 0.017(2) 0.0117(19) 0.0014(16) 0.0039(18) C15 0.025(2) 0.028(2) 0.020(2) 0.0109(19) 0.0072(17) 0.0033(19) C16 0.031(2) 0.031(2) 0.024(2) 0.013(2) 0.0078(19) 0.008(2) C17 0.036(3) 0.040(3) 0.030(3) 0.016(2) 0.007(2) 0.014(2) C18 0.042(3) 0.039(3) 0.042(3) 0.022(3) 0.016(2) 0.018(2) C19 0.054(4) 0.046(3) 0.066(4) 0.020(3) 0.012(3) 0.026(3) C20 0.034(3) 0.047(3) 0.039(3) 0.026(3) 0.006(2) 0.015(2) C21 0.030(2) 0.041(3) 0.034(3) 0.020(2) 0.002(2) 0.012(2) C22 0.046(3) 0.053(4) 0.037(3) 0.015(3) -0.014(2) 0.018(3) C23 0.026(2) 0.039(3) 0.038(3) 0.010(3) -0.001(2) 0.003(2) C24 0.033(3) 0.055(4) 0.070(4) 0.024(3) -0.001(3) -0.006(3) C25 0.045(3) 0.035(3) 0.032(3) 0.010(2) 0.016(2) 0.011(2) C26 0.036(3) 0.032(3) 0.033(3) 0.016(2) 0.015(2) 0.010(2) C27 0.039(3) 0.036(3) 0.044(3) 0.021(3) 0.020(2) 0.017(2) C28 0.036(3) 0.047(3) 0.047(3) 0.030(3) 0.017(2) 0.019(2) C29 0.042(3) 0.054(4) 0.068(4) 0.032(3) 0.013(3) 0.027(3) C30 0.030(2) 0.038(3) 0.031(3) 0.018(2) 0.005(2) 0.007(2) C31 0.025(2) 0.032(2) 0.026(2) 0.015(2) 0.0087(18) 0.008(2) C32 0.023(2) 0.032(2) 0.025(2) 0.016(2) 0.0073(18) 0.008(2) C33 0.025(2) 0.029(2) 0.024(2) 0.015(2) 0.0059(18) 0.0058(19) C34 0.031(2) 0.034(3) 0.026(2) 0.014(2) 0.0021(19) 0.007(2) C35 0.041(3) 0.030(3) 0.023(2) 0.007(2) 0.000(2) 0.002(2) C36 0.044(3) 0.026(3) 0.031(3) 0.007(2) 0.005(2) 0.010(2) C37 0.036(3) 0.031(3) 0.030(2) 0.014(2) 0.005(2) 0.013(2) C38 0.028(2) 0.029(2) 0.024(2) 0.014(2) 0.0049(18) 0.005(2) C39 0.032(2) 0.030(2) 0.022(2) 0.014(2) 0.0048(19) 0.010(2) C40 0.030(2) 0.033(3) 0.023(2) 0.014(2) 0.0011(19) 0.004(2) C41 0.031(2) 0.041(3) 0.032(3) 0.020(2) 0.003(2) 0.009(2) C42 0.030(2) 0.048(3) 0.034(3) 0.026(3) -0.001(2) 0.005(2) C43 0.035(3) 0.060(4) 0.048(3) 0.030(3) -0.009(2) 0.000(3) C44 0.039(3) 0.039(3) 0.027(3) 0.015(2) -0.005(2) -0.005(2) C45 0.037(3) 0.030(3) 0.027(2) 0.014(2) 0.003(2) 0.000(2) C46 0.060(3) 0.032(3) 0.025(3) 0.003(2) -0.002(2) 0.004(3) C47 0.030(2) 0.040(3) 0.026(2) 0.017(2) -0.002(2) 0.003(2) C48 0.053(3) 0.045(3) 0.044(3) 0.020(3) 0.007(3) -0.003(3) C49 0.045(3) 0.039(3) 0.026(2) 0.008(2) 0.007(2) 0.010(2) C50 0.070(5) 0.105(7) 0.110(8) 0.027(6) 0.003(5) 0.010(5) N1 0.0235(19) 0.033(2) 0.0201(18) 0.0081(17) 0.0029(15) 0.0062(17) N2 0.0235(18) 0.025(2) 0.0194(18) 0.0083(16) 0.0004(14) 0.0053(16) N3 0.0243(18) 0.029(2) 0.0176(18) 0.0100(16) 0.0016(14) 0.0007(16) N4 0.0279(19) 0.031(2) 0.0205(18) 0.0081(17) 0.0050(15) 0.0075(17) N5 0.0265(19) 0.031(2) 0.0234(19) 0.0128(17) 0.0032(15) 0.0096(17) N6 0.0299(19) 0.029(2) 0.0229(19) 0.0128(17) 0.0080(16) 0.0104(17) N7 0.0258(19) 0.032(2) 0.0249(19) 0.0153(18) 0.0018(15) 0.0065(17) N8 0.0272(19) 0.032(2) 0.0216(18) 0.0151(17) 0.0065(15) 0.0081(17) N9 0.033(2) 0.031(2) 0.024(2) 0.0091(18) 0.0024(16) 0.0092(18) N10 0.032(2) 0.028(2) 0.0228(19) 0.0132(17) 0.0022(16) 0.0032(17) O1 0.0227(16) 0.052(2) 0.0314(18) 0.0161(17) -0.0032(14) 0.0014(16) O2 0.035(12) 0.069(17) 0.14(3) 0.089(16) -0.004(12) 0.005(13) O2' 0.041(8) 0.178(17) 0.056(9) 0.076(9) -0.031(6) -0.044(9) O3 0.0354(18) 0.0286(17) 0.0312(17) 0.0127(15) 0.0082(14) 0.0063(14) O4 0.048(2) 0.053(2) 0.044(2) 0.018(2) 0.0208(18) 0.0147(19) Pd1 0.01956(18) 0.0316(2) 0.01717(17) 0.00731(15) 0.00085(13) 0.00508(14) Pd2 0.02744(19) 0.0254(2) 0.02179(19) 0.01049(15) 0.00500(14) 0.00632(15) Cl1 0.0688(10) 0.0715(11) 0.0575(10) 0.0141(9) 0.0345(8) 0.0165(9) Cl2 0.1027(15) 0.0478(10) 0.137(2) 0.0359(12) 0.0527(15) 0.0107(10) Cl3 0.1057(17) 0.0824(15) 0.0952(16) 0.0326(13) 0.0116(13) 0.0137(13) Cl4 0.073(3) 0.134(5) 0.097(4) 0.050(3) 0.019(3) 0.000(3) Cl4' 0.086(4) 0.091(4) 0.301(13) 0.042(5) -0.052(5) -0.020(3) O5 0.048(6) 0.051(6) 0.065(7) 0.029(6) 0.005(5) 0.019(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 C1 C2 1.498(8) . ? C2 N1 1.378(6) . ? C2 C3 1.384(8) . ? C3 C4 1.380(8) . ? C4 C6 1.382(7) . ? C4 C5 1.495(8) . ? C6 C7 1.397(7) . ? C7 N1 1.349(6) . ? C7 N2 1.387(6) . ? C8 N2 1.289(6) . ? C8 N3 1.374(6) . ? C8 C9 1.484(6) . ? C9 C14 1.376(6) . ? C9 C10 1.378(7) . ? C10 C11 1.396(6) . ? C11 C12 1.383(7) . ? C12 C13 1.388(7) . ? C13 C14 1.389(6) . ? C14 C15 1.479(6) . ? C15 N4 1.294(6) . ? C15 N3 1.377(6) . ? C16 N5 1.372(6) . ? C16 N4 1.383(6) . ? C16 C17 1.391(7) . ? C17 C18 1.379(7) . ? C18 C20 1.386(7) . ? C18 C19 1.504(8) . ? C20 C21 1.378(7) . ? C21 N5 1.365(6) . ? C21 C22 1.508(7) . ? C23 O2' 1.167(19) . ? C23 O1 1.267(7) . ? C23 O2 1.28(3) . ? C23 C24 1.518(7) . ? C25 C26 1.500(7) . ? C26 C27 1.371(7) . ? C26 N6 1.372(6) . ? C27 C28 1.395(8) . ? C28 C30 1.367(7) . ? C28 C29 1.505(8) . ? C30 C31 1.382(7) . ? C31 N6 1.374(6) . ? C31 N7 1.382(6) . ? C32 N7 1.289(6) . ? C32 N8 1.401(6) . ? C32 C33 1.475(6) . ? C33 C38 1.382(7) . ? C33 C34 1.386(6) . ? C34 C35 1.382(7) . ? C35 C36 1.389(7) . ? C36 C37 1.389(7) . ? C37 C38 1.386(7) . ? C38 C39 1.484(6) . ? C39 N9 1.283(6) . ? C39 N8 1.367(6) . ? C40 N10 1.363(6) . ? C40 C41 1.390(7) . ? C40 N9 1.390(6) . ? C41 C42 1.371(7) . ? C42 C44 1.379(8) . ? C42 C43 1.503(7) . ? C44 C45 1.380(7) . ? C45 N10 1.373(6) . ? C45 C46 1.494(7) . ? C47 O4 1.217(6) . ? C47 O3 1.286(6) . ? C47 C48 1.511(7) . ? C49 Cl1 1.747(5) . ? C49 Cl2 1.755(6) . ? C50 Cl4' 1.667(11) . ? C50 Cl4 1.707(11) . ? C50 Cl3 1.754(10) . ? N1 Pd1 2.056(4) . ? N3 Pd1 1.960(4) . ? N5 Pd1 2.081(4) . ? N6 Pd2 2.071(4) . ? N8 Pd2 1.959(4) . ? N10 Pd2 2.082(4) . ? O1 Pd1 2.059(3) . ? O3 Pd2 2.072(3) . ? 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 C2 C3 120.0(5) . . ? N1 C2 C1 119.5(5) . . ? C3 C2 C1 120.4(5) . . ? C4 C3 C2 122.5(5) . . ? C3 C4 C6 116.2(5) . . ? C3 C4 C5 121.7(5) . . ? C6 C4 C5 122.1(5) . . ? C4 C6 C7 120.8(5) . . ? N1 C7 N2 123.8(4) . . ? N1 C7 C6 121.7(4) . . ? N2 C7 C6 114.4(4) . . ? N2 C8 N3 130.9(4) . . ? N2 C8 C9 121.2(4) . . ? N3 C8 C9 107.7(4) . . ? C14 C9 C10 122.1(4) . . ? C14 C9 C8 106.9(4) . . ? C10 C9 C8 130.9(4) . . ? C9 C10 C11 116.6(5) . . ? C12 C11 C10 121.5(5) . . ? C11 C12 C13 121.3(4) . . ? C12 C13 C14 117.0(4) . . ? C9 C14 C13 121.4(4) . . ? C9 C14 C15 107.2(4) . . ? C13 C14 C15 131.4(4) . . ? N4 C15 N3 130.2(4) . . ? N4 C15 C14 122.0(4) . . ? N3 C15 C14 107.7(4) . . ? N5 C16 N4 124.9(4) . . ? N5 C16 C17 121.2(4) . . ? N4 C16 C17 114.0(4) . . ? C18 C17 C16 121.7(5) . . ? C17 C18 C20 116.5(5) . . ? C17 C18 C19 122.2(5) . . ? C20 C18 C19 121.2(5) . . ? C21 C20 C18 120.9(5) . . ? N5 C21 C20 122.6(5) . . ? N5 C21 C22 120.2(5) . . ? C20 C21 C22 117.1(5) . . ? O2' C23 O1 126.3(9) . . ? O2' C23 O2 17(3) . . ? O1 C23 O2 122.5(16) . . ? O2' C23 C24 119.3(11) . . ? O1 C23 C24 113.9(5) . . ? O2 C23 C24 122.5(14) . . ? C27 C26 N6 121.5(5) . . ? C27 C26 C25 118.9(5) . . ? N6 C26 C25 119.5(5) . . ? C26 C27 C28 121.4(5) . . ? C30 C28 C27 116.4(5) . . ? C30 C28 C29 121.7(5) . . ? C27 C28 C29 121.9(5) . . ? C28 C30 C31 121.9(5) . . ? N6 C31 N7 123.9(4) . . ? N6 C31 C30 121.1(4) . . ? N7 C31 C30 115.0(4) . . ? N7 C32 N8 130.6(4) . . ? N7 C32 C33 121.9(4) . . ? N8 C32 C33 107.5(4) . . ? C38 C33 C34 120.9(4) . . ? C38 C33 C32 107.5(4) . . ? C34 C33 C32 131.5(4) . . ? C35 C34 C33 117.8(5) . . ? C34 C35 C36 121.3(4) . . ? C35 C36 C37 121.1(5) . . ? C38 C37 C36 117.2(5) . . ? C33 C38 C37 121.8(4) . . ? C33 C38 C39 106.8(4) . . ? C37 C38 C39 131.4(4) . . ? N9 C39 N8 129.8(4) . . ? N9 C39 C38 121.6(4) . . ? N8 C39 C38 108.4(4) . . ? N10 C40 C41 121.6(4) . . ? N10 C40 N9 125.2(4) . . ? C41 C40 N9 113.2(4) . . ? C42 C41 C40 121.9(5) . . ? C41 C42 C44 115.8(5) . . ? C41 C42 C43 122.2(5) . . ? C44 C42 C43 122.0(5) . . ? C42 C44 C45 122.2(5) . . ? N10 C45 C44 121.3(5) . . ? N10 C45 C46 120.6(5) . . ? C44 C45 C46 118.0(4) . . ? O4 C47 O3 126.5(5) . . ? O4 C47 C48 120.5(5) . . ? O3 C47 C48 113.0(5) . . ? Cl1 C49 Cl2 111.2(3) . . ? Cl4' C50 Cl4 68.9(5) . . ? Cl4' C50 Cl3 123.3(7) . . ? Cl4 C50 Cl3 104.2(6) . . ? C7 N1 C2 117.6(4) . . ? C7 N1 Pd1 124.0(3) . . ? C2 N1 Pd1 118.4(3) . . ? C8 N2 C7 123.7(4) . . ? C8 N3 C15 109.4(4) . . ? C8 N3 Pd1 121.5(3) . . ? C15 N3 Pd1 121.3(3) . . ? C15 N4 C16 125.6(4) . . ? C21 N5 C16 116.8(4) . . ? C21 N5 Pd1 121.2(3) . . ? C16 N5 Pd1 121.9(3) . . ? C26 N6 C31 117.1(4) . . ? C26 N6 Pd2 120.3(3) . . ? C31 N6 Pd2 122.5(3) . . ? C32 N7 C31 125.3(4) . . ? C39 N8 C32 109.0(4) . . ? C39 N8 Pd2 123.4(3) . . ? C32 N8 Pd2 120.1(3) . . ? C39 N9 C40 124.8(4) . . ? C40 N10 C45 116.7(4) . . ? C40 N10 Pd2 123.0(3) . . ? C45 N10 Pd2 120.2(3) . . ? C23 O1 Pd1 113.7(3) . . ? C47 O3 Pd2 117.1(3) . . ? N3 Pd1 N1 88.64(15) . . ? N3 Pd1 O1 161.30(15) . . ? N1 Pd1 O1 90.49(14) . . ? N3 Pd1 N5 91.25(15) . . ? N1 Pd1 N5 166.22(15) . . ? O1 Pd1 N5 93.97(15) . . ? N8 Pd2 N6 90.14(16) . . ? N8 Pd2 O3 160.24(13) . . ? N6 Pd2 O3 89.22(14) . . ? N8 Pd2 N10 89.49(15) . . ? N6 Pd2 N10 165.01(14) . . ? O3 Pd2 N10 96.12(14) . . ? 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 C4 4.4(8) . . . . ? C1 C2 C3 C4 -171.6(5) . . . . ? C2 C3 C4 C6 3.6(8) . . . . ? C2 C3 C4 C5 -179.9(5) . . . . ? C3 C4 C6 C7 -3.9(7) . . . . ? C5 C4 C6 C7 179.6(5) . . . . ? C4 C6 C7 N1 -4.0(7) . . . . ? C4 C6 C7 N2 174.0(4) . . . . ? N2 C8 C9 C14 170.4(4) . . . . ? N3 C8 C9 C14 -5.4(4) . . . . ? N2 C8 C9 C10 -9.7(7) . . . . ? N3 C8 C9 C10 174.6(4) . . . . ? C14 C9 C10 C11 -1.9(6) . . . . ? C8 C9 C10 C11 178.2(4) . . . . ? C9 C10 C11 C12 1.5(7) . . . . ? C10 C11 C12 C13 0.0(7) . . . . ? C11 C12 C13 C14 -1.1(7) . . . . ? C10 C9 C14 C13 0.8(6) . . . . ? C8 C9 C14 C13 -179.2(4) . . . . ? C10 C9 C14 C15 179.2(4) . . . . ? C8 C9 C14 C15 -0.8(4) . . . . ? C12 C13 C14 C9 0.7(6) . . . . ? C12 C13 C14 C15 -177.2(4) . . . . ? C9 C14 C15 N4 -170.3(4) . . . . ? C13 C14 C15 N4 7.9(7) . . . . ? C9 C14 C15 N3 6.7(4) . . . . ? C13 C14 C15 N3 -175.1(4) . . . . ? N5 C16 C17 C18 2.1(7) . . . . ? N4 C16 C17 C18 -176.7(4) . . . . ? C16 C17 C18 C20 2.6(7) . . . . ? C16 C17 C18 C19 178.2(5) . . . . ? C17 C18 C20 C21 -2.7(7) . . . . ? C19 C18 C20 C21 -178.4(5) . . . . ? C18 C20 C21 N5 -1.8(8) . . . . ? C18 C20 C21 C22 174.1(5) . . . . ? N6 C26 C27 C28 -2.1(7) . . . . ? C25 C26 C27 C28 173.6(5) . . . . ? C26 C27 C28 C30 -4.3(7) . . . . ? C26 C27 C28 C29 176.3(5) . . . . ? C27 C28 C30 C31 4.4(7) . . . . ? C29 C28 C30 C31 -176.2(5) . . . . ? C28 C30 C31 N6 1.9(7) . . . . ? C28 C30 C31 N7 -176.4(4) . . . . ? N7 C32 C33 C38 -174.2(4) . . . . ? N8 C32 C33 C38 4.3(5) . . . . ? N7 C32 C33 C34 1.2(7) . . . . ? N8 C32 C33 C34 179.7(4) . . . . ? C38 C33 C34 C35 -1.7(6) . . . . ? C32 C33 C34 C35 -176.7(4) . . . . ? C33 C34 C35 C36 0.1(7) . . . . ? C34 C35 C36 C37 0.7(8) . . . . ? C35 C36 C37 C38 0.2(7) . . . . ? C34 C33 C38 C37 2.7(7) . . . . ? C32 C33 C38 C37 178.7(4) . . . . ? C34 C33 C38 C39 -175.0(4) . . . . ? C32 C33 C38 C39 1.0(5) . . . . ? C36 C37 C38 C33 -1.8(7) . . . . ? C36 C37 C38 C39 175.2(5) . . . . ? C33 C38 C39 N9 170.3(4) . . . . ? C37 C38 C39 N9 -7.1(7) . . . . ? C33 C38 C39 N8 -6.1(5) . . . . ? C37 C38 C39 N8 176.5(5) . . . . ? N10 C40 C41 C42 -5.3(7) . . . . ? N9 C40 C41 C42 173.9(4) . . . . ? C40 C41 C42 C44 -0.6(7) . . . . ? C40 C41 C42 C43 -178.2(5) . . . . ? C41 C42 C44 C45 3.1(7) . . . . ? C43 C42 C44 C45 -179.3(5) . . . . ? C42 C44 C45 N10 0.1(7) . . . . ? C42 C44 C45 C46 -176.6(5) . . . . ? N2 C7 N1 C2 -165.9(4) . . . . ? C6 C7 N1 C2 11.9(6) . . . . ? N2 C7 N1 Pd1 14.0(6) . . . . ? C6 C7 N1 Pd1 -168.2(3) . . . . ? C3 C2 N1 C7 -12.0(7) . . . . ? C1 C2 N1 C7 164.0(5) . . . . ? C3 C2 N1 Pd1 168.1(4) . . . . ? C1 C2 N1 Pd1 -15.9(6) . . . . ? N3 C8 N2 C7 -7.2(7) . . . . ? C9 C8 N2 C7 178.2(4) . . . . ? N1 C7 N2 C8 7.7(7) . . . . ? C6 C7 N2 C8 -170.2(4) . . . . ? N2 C8 N3 C15 -165.4(4) . . . . ? C9 C8 N3 C15 9.8(4) . . . . ? N2 C8 N3 Pd1 -15.8(6) . . . . ? C9 C8 N3 Pd1 159.4(3) . . . . ? N4 C15 N3 C8 166.4(4) . . . . ? C14 C15 N3 C8 -10.3(4) . . . . ? N4 C15 N3 Pd1 16.7(6) . . . . ? C14 C15 N3 Pd1 -160.0(3) . . . . ? N3 C15 N4 C16 4.4(7) . . . . ? C14 C15 N4 C16 -179.4(4) . . . . ? N5 C16 N4 C15 -11.1(7) . . . . ? C17 C16 N4 C15 167.7(4) . . . . ? C20 C21 N5 C16 6.4(7) . . . . ? C22 C21 N5 C16 -169.4(5) . . . . ? C20 C21 N5 Pd1 -177.6(4) . . . . ? C22 C21 N5 Pd1 6.6(6) . . . . ? N4 C16 N5 C21 172.2(4) . . . . ? C17 C16 N5 C21 -6.5(6) . . . . ? N4 C16 N5 Pd1 -3.8(6) . . . . ? C17 C16 N5 Pd1 177.5(3) . . . . ? C27 C26 N6 C31 8.3(6) . . . . ? C25 C26 N6 C31 -167.4(4) . . . . ? C27 C26 N6 Pd2 -168.6(3) . . . . ? C25 C26 N6 Pd2 15.7(6) . . . . ? N7 C31 N6 C26 169.9(4) . . . . ? C30 C31 N6 C26 -8.2(6) . . . . ? N7 C31 N6 Pd2 -13.3(6) . . . . ? C30 C31 N6 Pd2 168.6(3) . . . . ? N8 C32 N7 C31 3.4(7) . . . . ? C33 C32 N7 C31 -178.4(4) . . . . ? N6 C31 N7 C32 -6.3(7) . . . . ? C30 C31 N7 C32 171.9(4) . . . . ? N9 C39 N8 C32 -167.1(5) . . . . ? C38 C39 N8 C32 8.9(5) . . . . ? N9 C39 N8 Pd2 -17.5(6) . . . . ? C38 C39 N8 Pd2 158.5(3) . . . . ? N7 C32 N8 C39 170.1(4) . . . . ? C33 C32 N8 C39 -8.3(4) . . . . ? N7 C32 N8 Pd2 19.3(6) . . . . ? C33 C32 N8 Pd2 -159.1(3) . . . . ? N8 C39 N9 C40 -2.1(8) . . . . ? C38 C39 N9 C40 -177.6(4) . . . . ? N10 C40 N9 C39 8.5(7) . . . . ? C41 C40 N9 C39 -170.7(4) . . . . ? C41 C40 N10 C45 8.4(6) . . . . ? N9 C40 N10 C45 -170.7(4) . . . . ? C41 C40 N10 Pd2 -176.1(3) . . . . ? N9 C40 N10 Pd2 4.8(6) . . . . ? C44 C45 N10 C40 -5.9(6) . . . . ? C46 C45 N10 C40 170.8(4) . . . . ? C44 C45 N10 Pd2 178.4(3) . . . . ? C46 C45 N10 Pd2 -4.9(6) . . . . ? O2' C23 O1 Pd1 -12(4) . . . . ? O2 C23 O1 Pd1 9(2) . . . . ? C24 C23 O1 Pd1 176.9(4) . . . . ? O4 C47 O3 Pd2 3.0(7) . . . . ? C48 C47 O3 Pd2 -176.2(3) . . . . ? C8 N3 Pd1 N1 25.7(3) . . . . ? C15 N3 Pd1 N1 171.7(3) . . . . ? C8 N3 Pd1 O1 -61.8(6) . . . . ? C15 N3 Pd1 O1 84.2(6) . . . . ? C8 N3 Pd1 N5 -168.1(3) . . . . ? C15 N3 Pd1 N5 -22.0(3) . . . . ? C7 N1 Pd1 N3 -26.0(3) . . . . ? C2 N1 Pd1 N3 153.9(4) . . . . ? C7 N1 Pd1 O1 135.4(3) . . . . ? C2 N1 Pd1 O1 -44.8(4) . . . . ? C7 N1 Pd1 N5 -115.7(6) . . . . ? C2 N1 Pd1 N5 64.2(7) . . . . ? C23 O1 Pd1 N3 1.8(7) . . . . ? C23 O1 Pd1 N1 -85.4(4) . . . . ? C23 O1 Pd1 N5 107.7(4) . . . . ? C21 N5 Pd1 N3 -159.1(4) . . . . ? C16 N5 Pd1 N3 16.8(3) . . . . ? C21 N5 Pd1 N1 -69.7(7) . . . . ? C16 N5 Pd1 N1 106.2(6) . . . . ? C21 N5 Pd1 O1 38.9(4) . . . . ? C16 N5 Pd1 O1 -145.3(3) . . . . ? C39 N8 Pd2 N6 -173.4(3) . . . . ? C32 N8 Pd2 N6 -27.0(3) . . . . ? C39 N8 Pd2 O3 -85.3(5) . . . . ? C32 N8 Pd2 O3 61.1(6) . . . . ? C39 N8 Pd2 N10 21.6(3) . . . . ? C32 N8 Pd2 N10 168.0(3) . . . . ? C26 N6 Pd2 N8 -157.7(3) . . . . ? C31 N6 Pd2 N8 25.5(3) . . . . ? C26 N6 Pd2 O3 42.0(3) . . . . ? C31 N6 Pd2 O3 -134.7(3) . . . . ? C26 N6 Pd2 N10 -69.2(7) . . . . ? C31 N6 Pd2 N10 114.1(6) . . . . ? C47 O3 Pd2 N8 39.2(6) . . . . ? C47 O3 Pd2 N6 127.4(3) . . . . ? C47 O3 Pd2 N10 -66.6(3) . . . . ? C40 N10 Pd2 N8 -16.2(3) . . . . ? C45 N10 Pd2 N8 159.2(3) . . . . ? C40 N10 Pd2 N6 -104.9(6) . . . . ? C45 N10 Pd2 N6 70.6(7) . . . . ? C40 N10 Pd2 O3 144.8(3) . . . . ? C45 N10 Pd2 O3 -39.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.966 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.100 _exptl_crystal_recrystallization_method 'evap. of a sol. in CH2Cl2 ' data_ck10ck _database_code_depnum_ccdc_archive 'CCDC 626408' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H44 Cl2 N10 O4 Pd4' _chemical_formula_sum 'C48 H44 Cl2 N10 O4 Pd4' _chemical_formula_weight 1321.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5886(16) _cell_length_b 11.834(3) _cell_length_c 12.123(3) _cell_angle_alpha 90.44(3) _cell_angle_beta 97.63(2) _cell_angle_gamma 104.77(2) _cell_volume 1179.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4557 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.246 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.022 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6901 _exptl_absorpt_correction_T_max 0.9285 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS1 (Stoe)' _diffrn_measurement_method phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11593 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.1538 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.07 _reflns_number_total 4296 _reflns_number_gt 1747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX v1.64.05' _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^)+(0.1406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 4296 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2055 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _refine_ls_shift/su_max 0.000 _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 0.1815(19) 0.3401(16) 0.1521(17) 0.092(6) Uani 1 1 d . . . H1A H 0.1859 0.2758 0.1023 0.138 Uiso 1 1 calc R . . H1B H 0.1311 0.3948 0.1096 0.138 Uiso 1 1 calc R . . H1C H 0.1169 0.3088 0.2111 0.138 Uiso 1 1 calc R . . C2 C 0.3565(19) 0.4051(16) 0.205(2) 0.094(7) Uani 1 1 d . . . C3 C 0.417(2) 0.5135(16) 0.1493(19) 0.093(6) Uani 1 1 d . . . H3 H 0.3557 0.5343 0.0851 0.112 Uiso 1 1 calc R . . C4 C 0.568(2) 0.5851(17) 0.194(2) 0.093(6) Uani 1 1 d . . . C5 C 0.640(2) 0.6962(16) 0.140(2) 0.109(7) Uani 1 1 d . . . H5A H 0.6321 0.6806 0.0599 0.163 Uiso 1 1 calc R . . H5B H 0.7544 0.7263 0.1719 0.163 Uiso 1 1 calc R . . H5C H 0.5803 0.7543 0.1534 0.163 Uiso 1 1 calc R . . C6 C 0.641(2) 0.5515(17) 0.293(2) 0.099(6) Uani 1 1 d . . . H6 H 0.7406 0.6012 0.3279 0.119 Uiso 1 1 calc R . . C7 C 0.575(2) 0.4482(12) 0.343(2) 0.090(7) Uani 1 1 d . . . C8 C 0.6156(17) 0.3479(14) 0.5094(16) 0.071(4) Uani 1 1 d . . . C9 C 0.7137(17) 0.3432(13) 0.6120(16) 0.073(5) Uani 1 1 d . . . C10 C 0.8550(18) 0.4189(16) 0.6658(18) 0.082(5) Uani 1 1 d . . . H10 H 0.9031 0.4888 0.6315 0.099 Uiso 1 1 calc R . . C11 C 0.924(2) 0.3952(16) 0.764(2) 0.090(6) Uani 1 1 d . . . H11 H 1.0240 0.4458 0.7965 0.108 Uiso 1 1 calc R . . C12 C 0.851(2) 0.2964(18) 0.821(2) 0.101(6) Uani 1 1 d . . . H12 H 0.8957 0.2827 0.8940 0.122 Uiso 1 1 calc R . . C13 C 0.7077(18) 0.2182(15) 0.765(2) 0.083(6) Uani 1 1 d . . . H13 H 0.6571 0.1494 0.7995 0.100 Uiso 1 1 calc R . . C14 C 0.6453(18) 0.2407(16) 0.6654(16) 0.071(4) Uani 1 1 d . . . C15 C 0.5030(15) 0.1790(15) 0.5817(15) 0.070(5) Uani 1 1 d . . . C17 C 0.2408(16) 0.0430(12) 0.4116(17) 0.069(5) Uani 1 1 d . . . C18 C 0.0902(17) -0.0283(13) 0.3523(15) 0.068(4) Uani 1 1 d . . . C19 C -0.0020(17) -0.0034(15) 0.2440(16) 0.079(5) Uani 1 1 d . . . H19A H 0.0383 0.0790 0.2277 0.118 Uiso 1 1 calc R . . H19B H -0.1181 -0.0203 0.2506 0.118 Uiso 1 1 calc R . . H19C H 0.0141 -0.0530 0.1836 0.118 Uiso 1 1 calc R . . C20 C 0.0176(17) -0.1305(14) 0.4044(16) 0.073(5) Uani 1 1 d . . . H20 H -0.0813 -0.1800 0.3679 0.088 Uiso 1 1 calc R . . C21 C 0.0826(15) -0.1614(13) 0.5046(15) 0.065(4) Uani 1 1 d . . . C22 C 0.0097(19) -0.2759(15) 0.5597(16) 0.085(5) Uani 1 1 d . . . H22A H -0.0474 -0.3361 0.5019 0.128 Uiso 1 1 calc R . . H22B H -0.0671 -0.2626 0.6082 0.128 Uiso 1 1 calc R . . H22C H 0.0970 -0.3021 0.6039 0.128 Uiso 1 1 calc R . . C23 C 0.3490(19) 0.0708(15) 0.1284(17) 0.079(5) Uani 1 1 d . . . C24 C 0.272(2) 0.0330(19) 0.0128(18) 0.091(6) Uani 1 1 d . . . H24A H 0.2034 -0.0473 0.0117 0.137 Uiso 1 1 calc R . . H24B H 0.3562 0.0361 -0.0350 0.137 Uiso 1 1 calc R . . H24C H 0.2044 0.0851 -0.0149 0.137 Uiso 1 1 calc R . . N1 N 0.4318(15) 0.3707(12) 0.2888(14) 0.078(4) Uani 1 1 d . . . N2 N 0.6569(18) 0.4292(13) 0.4447(17) 0.090(5) Uani 1 1 d . . . N3 N 0.4781(13) 0.2433(11) 0.4936(13) 0.070(4) Uani 1 1 d . . . O1 O 0.2950(12) 0.1385(10) 0.1871(10) 0.079(3) Uani 1 1 d . . . O2 O 0.4701(13) 0.0276(10) 0.1646(11) 0.082(3) Uani 1 1 d . . . Pd1 Pd 0.35748(12) 0.19529(10) 0.34642(12) 0.0719(5) Uani 1 1 d . . . Pd2 Pd 0.62564(13) 0.07183(11) 0.30313(12) 0.0730(5) Uani 1 1 d . . . Cl1 Cl 0.7278(8) 0.2351(7) 0.2125(8) 0.160(3) Uani 1 1 d . . . C16 C 0.2904(15) 0.0096(13) 0.5106(15) 0.062(4) Uani 1 1 d . . . N4 N 0.4142(13) 0.0681(11) 0.5930(12) 0.068(3) Uani 1 1 d . . . N5 N 0.2210(15) -0.0890(11) 0.5589(13) 0.075(4) 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 0.068(9) 0.084(12) 0.121(18) 0.018(11) 0.033(10) 0.004(8) C2 0.064(9) 0.078(12) 0.15(2) 0.024(12) 0.042(12) 0.028(8) C3 0.071(10) 0.074(11) 0.130(18) 0.006(11) 0.022(11) 0.007(8) C4 0.083(11) 0.080(12) 0.119(19) 0.036(12) 0.039(12) 0.014(9) C5 0.104(13) 0.073(12) 0.14(2) 0.038(12) 0.040(14) 0.000(10) C6 0.079(11) 0.079(12) 0.13(2) 0.016(12) 0.023(12) -0.004(9) C7 0.083(10) 0.040(8) 0.15(2) 0.012(10) 0.068(13) -0.001(7) C8 0.060(8) 0.060(9) 0.082(13) -0.011(9) 0.009(9) -0.006(7) C9 0.054(7) 0.058(9) 0.099(15) -0.005(9) 0.018(9) -0.007(6) C10 0.063(9) 0.087(12) 0.090(16) -0.003(11) 0.005(9) 0.010(8) C11 0.061(8) 0.079(12) 0.121(19) 0.005(11) 0.006(10) 0.003(8) C12 0.088(12) 0.095(14) 0.118(19) -0.001(13) 0.006(12) 0.023(10) C13 0.061(8) 0.062(10) 0.124(19) -0.002(10) 0.018(10) 0.006(7) C14 0.060(8) 0.090(12) 0.058(12) -0.003(9) -0.001(8) 0.013(8) C15 0.044(6) 0.085(11) 0.084(13) -0.006(10) 0.019(7) 0.018(7) C17 0.054(7) 0.051(8) 0.109(15) -0.006(9) 0.037(9) 0.011(6) C18 0.060(7) 0.067(9) 0.078(13) 0.003(8) 0.020(8) 0.012(7) C19 0.057(8) 0.073(10) 0.095(15) -0.001(9) 0.005(9) -0.001(7) C20 0.054(7) 0.066(9) 0.093(14) 0.004(9) 0.014(8) 0.001(7) C21 0.046(6) 0.066(9) 0.082(13) 0.013(8) 0.017(7) 0.008(6) C22 0.066(9) 0.081(11) 0.102(15) 0.021(10) 0.020(9) 0.001(8) C23 0.059(8) 0.080(11) 0.096(16) 0.016(10) 0.033(9) 0.005(8) C24 0.073(10) 0.111(15) 0.093(16) -0.003(12) 0.012(10) 0.028(10) N1 0.057(6) 0.071(9) 0.107(13) 0.028(8) 0.018(7) 0.012(6) N2 0.081(9) 0.071(9) 0.118(15) 0.020(10) 0.026(10) 0.013(7) N3 0.056(6) 0.068(8) 0.088(11) 0.022(7) 0.017(7) 0.015(5) O1 0.064(5) 0.088(8) 0.087(9) 0.011(6) 0.028(6) 0.013(5) O2 0.077(7) 0.075(7) 0.097(10) 0.002(6) 0.029(6) 0.014(6) Pd1 0.0542(6) 0.0621(7) 0.0993(12) 0.0088(7) 0.0250(7) 0.0072(5) Pd2 0.0549(6) 0.0680(8) 0.0964(12) 0.0069(7) 0.0217(7) 0.0110(5) Cl1 0.109(4) 0.132(6) 0.218(9) 0.030(6) -0.004(5) 0.005(4) C16 0.046(6) 0.070(9) 0.067(12) 0.020(8) 0.011(7) 0.011(6) N4 0.050(6) 0.066(7) 0.086(10) 0.007(7) 0.012(6) 0.008(5) N5 0.070(7) 0.058(7) 0.109(12) 0.012(7) 0.040(8) 0.025(6) _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 1.55(3) . ? C2 N1 1.26(2) . ? C2 C3 1.46(3) . ? C3 C4 1.40(3) . ? C4 C6 1.38(3) . ? C4 C5 1.50(2) . ? C6 C7 1.39(2) . ? C7 N2 1.39(3) . ? C7 N1 1.41(2) . ? C8 N2 1.26(2) . ? C8 C9 1.42(2) . ? C8 N3 1.468(18) . ? C9 C10 1.39(2) . ? C9 C14 1.41(2) . ? C10 C11 1.32(3) . ? C11 C12 1.41(3) . ? C12 C13 1.42(3) . ? C13 C14 1.31(2) . ? C14 C15 1.50(2) . ? C15 N3 1.34(2) . ? C15 N4 1.36(2) . ? C17 C16 1.32(2) . ? C17 C18 1.45(2) . ? C17 Pd1 2.046(15) . ? C18 C20 1.41(2) . ? C18 C19 1.51(2) . ? C20 C21 1.36(2) . ? C21 N5 1.36(2) . ? C21 C22 1.54(2) . ? C23 O1 1.28(2) . ? C23 O2 1.30(2) . ? C23 C24 1.48(3) . ? N1 Pd1 2.161(13) . ? N3 Pd1 1.942(15) . ? O1 Pd1 1.998(13) . ? O2 Pd2 1.979(13) . ? Pd1 Pd2 3.1208(17) . ? Pd2 N5 1.962(16) 2_656 ? Pd2 N4 2.074(13) 2_656 ? Pd2 Cl1 2.266(8) . ? Pd2 C16 2.550(18) 2_656 ? C16 N5 1.345(18) . ? C16 N4 1.39(2) . ? C16 Pd2 2.550(18) 2_656 ? N4 Pd2 2.074(13) 2_656 ? N5 Pd2 1.962(16) 2_656 ? 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 C2 C3 125.0(18) . . ? N1 C2 C1 123.5(16) . . ? C3 C2 C1 111.4(19) . . ? C4 C3 C2 117(2) . . ? C6 C4 C3 116.7(17) . . ? C6 C4 C5 122.9(19) . . ? C3 C4 C5 120(2) . . ? C4 C6 C7 123.0(19) . . ? N2 C7 C6 116.6(18) . . ? N2 C7 N1 124.3(14) . . ? C6 C7 N1 119(2) . . ? N2 C8 C9 120.8(15) . . ? N2 C8 N3 129.7(18) . . ? C9 C8 N3 109.3(14) . . ? C10 C9 C14 118.0(19) . . ? C10 C9 C8 132.4(16) . . ? C14 C9 C8 109.5(14) . . ? C11 C10 C9 120.9(18) . . ? C10 C11 C12 121.4(18) . . ? C11 C12 C13 117(2) . . ? C14 C13 C12 120.3(18) . . ? C13 C14 C9 121.9(16) . . ? C13 C14 C15 135.1(16) . . ? C9 C14 C15 103.0(16) . . ? N3 C15 N4 124.1(15) . . ? N3 C15 C14 113.0(15) . . ? N4 C15 C14 122.9(16) . . ? C16 C17 C18 117.1(14) . . ? C16 C17 Pd1 122.8(11) . . ? C18 C17 Pd1 119.9(14) . . ? C20 C18 C17 115.8(17) . . ? C20 C18 C19 116.3(14) . . ? C17 C18 C19 127.8(14) . . ? C21 C20 C18 122.9(15) . . ? N5 C21 C20 118.9(14) . . ? N5 C21 C22 117.6(16) . . ? C20 C21 C22 123.5(14) . . ? O1 C23 O2 123.8(19) . . ? O1 C23 C24 121.1(16) . . ? O2 C23 C24 115.1(16) . . ? C2 N1 C7 118.1(16) . . ? C2 N1 Pd1 122.6(12) . . ? C7 N1 Pd1 119.2(13) . . ? C8 N2 C7 128.5(15) . . ? C15 N3 C8 104.8(14) . . ? C15 N3 Pd1 130.0(11) . . ? C8 N3 Pd1 120.5(11) . . ? C23 O1 Pd1 131.4(12) . . ? C23 O2 Pd2 128.2(12) . . ? N3 Pd1 O1 163.4(5) . . ? N3 Pd1 C17 88.3(7) . . ? O1 Pd1 C17 95.9(6) . . ? N3 Pd1 N1 91.7(6) . . ? O1 Pd1 N1 88.0(6) . . ? C17 Pd1 N1 166.0(5) . . ? N3 Pd1 Pd2 87.9(4) . . ? O1 Pd1 Pd2 76.2(3) . . ? C17 Pd1 Pd2 87.4(4) . . ? N1 Pd1 Pd2 106.5(3) . . ? N5 Pd2 O2 170.8(5) 2_656 . ? N5 Pd2 N4 64.2(5) 2_656 2_656 ? O2 Pd2 N4 108.0(5) . 2_656 ? N5 Pd2 Cl1 103.1(4) 2_656 . ? O2 Pd2 Cl1 84.1(4) . . ? N4 Pd2 Cl1 166.7(4) 2_656 . ? N5 Pd2 C16 31.4(5) 2_656 2_656 ? O2 Pd2 C16 141.1(5) . 2_656 ? N4 Pd2 C16 33.1(5) 2_656 2_656 ? Cl1 Pd2 C16 134.5(4) . 2_656 ? N5 Pd2 Pd1 107.4(3) 2_656 . ? O2 Pd2 Pd1 78.6(3) . . ? N4 Pd2 Pd1 102.6(3) 2_656 . ? Cl1 Pd2 Pd1 84.8(2) . . ? C16 Pd2 Pd1 105.3(3) 2_656 . ? C17 C16 N5 126.4(15) . . ? C17 C16 N4 130.1(14) . . ? N5 C16 N4 103.4(15) . . ? C17 C16 Pd2 175.4(12) . 2_656 ? N5 C16 Pd2 49.4(9) . 2_656 ? N4 C16 Pd2 54.3(8) . 2_656 ? C15 N4 C16 122.0(14) . . ? C15 N4 Pd2 145.4(12) . 2_656 ? C16 N4 Pd2 92.6(9) . 2_656 ? C16 N5 C21 118.7(16) . . ? C16 N5 Pd2 99.2(11) . 2_656 ? C21 N5 Pd2 142.0(11) . 2_656 ? 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 C4 -1(3) . . . . ? C1 C2 C3 C4 175.1(17) . . . . ? C2 C3 C4 C6 -5(3) . . . . ? C2 C3 C4 C5 178.5(18) . . . . ? C3 C4 C6 C7 4(3) . . . . ? C5 C4 C6 C7 -179.6(18) . . . . ? C4 C6 C7 N2 -176.3(18) . . . . ? C4 C6 C7 N1 3(3) . . . . ? N2 C8 C9 C10 5(3) . . . . ? N3 C8 C9 C10 -179.7(16) . . . . ? N2 C8 C9 C14 -176.7(15) . . . . ? N3 C8 C9 C14 -0.9(18) . . . . ? C14 C9 C10 C11 0(3) . . . . ? C8 C9 C10 C11 178.9(18) . . . . ? C9 C10 C11 C12 -4(3) . . . . ? C10 C11 C12 C13 5(3) . . . . ? C11 C12 C13 C14 -2(3) . . . . ? C12 C13 C14 C9 -2(3) . . . . ? C12 C13 C14 C15 177.9(17) . . . . ? C10 C9 C14 C13 3(2) . . . . ? C8 C9 C14 C13 -176.2(16) . . . . ? C10 C9 C14 C15 -177.0(14) . . . . ? C8 C9 C14 C15 4.0(17) . . . . ? C13 C14 C15 N3 174.0(18) . . . . ? C9 C14 C15 N3 -6.3(16) . . . . ? C13 C14 C15 N4 -9(3) . . . . ? C9 C14 C15 N4 171.2(13) . . . . ? C16 C17 C18 C20 -4(2) . . . . ? Pd1 C17 C18 C20 -179.1(10) . . . . ? C16 C17 C18 C19 173.2(15) . . . . ? Pd1 C17 C18 C19 -2(2) . . . . ? C17 C18 C20 C21 0(2) . . . . ? C19 C18 C20 C21 -176.9(14) . . . . ? C18 C20 C21 N5 2(2) . . . . ? C18 C20 C21 C22 -176.6(14) . . . . ? C3 C2 N1 C7 9(3) . . . . ? C1 C2 N1 C7 -167.4(16) . . . . ? C3 C2 N1 Pd1 -167.6(14) . . . . ? C1 C2 N1 Pd1 16(3) . . . . ? N2 C7 N1 C2 169.9(16) . . . . ? C6 C7 N1 C2 -10(2) . . . . ? N2 C7 N1 Pd1 -14(2) . . . . ? C6 C7 N1 Pd1 166.9(13) . . . . ? C9 C8 N2 C7 -179.0(16) . . . . ? N3 C8 N2 C7 6(3) . . . . ? C6 C7 N2 C8 174.2(18) . . . . ? N1 C7 N2 C8 -5(3) . . . . ? N4 C15 N3 C8 -171.7(13) . . . . ? C14 C15 N3 C8 5.8(16) . . . . ? N4 C15 N3 Pd1 -17(2) . . . . ? C14 C15 N3 Pd1 160.8(10) . . . . ? N2 C8 N3 C15 172.2(17) . . . . ? C9 C8 N3 C15 -3.0(17) . . . . ? N2 C8 N3 Pd1 14(2) . . . . ? C9 C8 N3 Pd1 -161.0(10) . . . . ? O2 C23 O1 Pd1 -4(2) . . . . ? C24 C23 O1 Pd1 174.5(11) . . . . ? O1 C23 O2 Pd2 -12(2) . . . . ? C24 C23 O2 Pd2 170.3(11) . . . . ? C15 N3 Pd1 O1 -86(2) . . . . ? C8 N3 Pd1 O1 66(2) . . . . ? C15 N3 Pd1 C17 18.9(12) . . . . ? C8 N3 Pd1 C17 170.7(11) . . . . ? C15 N3 Pd1 N1 -175.1(12) . . . . ? C8 N3 Pd1 N1 -23.3(11) . . . . ? C15 N3 Pd1 Pd2 -68.6(11) . . . . ? C8 N3 Pd1 Pd2 83.2(11) . . . . ? C23 O1 Pd1 N3 27(2) . . . . ? C23 O1 Pd1 C17 -76.5(13) . . . . ? C23 O1 Pd1 N1 116.9(12) . . . . ? C23 O1 Pd1 Pd2 9.4(11) . . . . ? C16 C17 Pd1 N3 -13.0(12) . . . . ? C18 C17 Pd1 N3 162.0(11) . . . . ? C16 C17 Pd1 O1 150.8(12) . . . . ? C18 C17 Pd1 O1 -34.1(11) . . . . ? C16 C17 Pd1 N1 -103(3) . . . . ? C18 C17 Pd1 N1 72(3) . . . . ? C16 C17 Pd1 Pd2 75.0(12) . . . . ? C18 C17 Pd1 Pd2 -110.0(10) . . . . ? C2 N1 Pd1 N3 -159.9(14) . . . . ? C7 N1 Pd1 N3 23.8(12) . . . . ? C2 N1 Pd1 O1 36.7(14) . . . . ? C7 N1 Pd1 O1 -139.6(12) . . . . ? C2 N1 Pd1 C17 -70(3) . . . . ? C7 N1 Pd1 C17 114(3) . . . . ? C2 N1 Pd1 Pd2 111.7(14) . . . . ? C7 N1 Pd1 Pd2 -64.6(12) . . . . ? C23 O2 Pd2 N5 144(2) . . . 2_656 ? C23 O2 Pd2 N4 112.7(12) . . . 2_656 ? C23 O2 Pd2 Cl1 -72.9(12) . . . . ? C23 O2 Pd2 C16 113.3(13) . . . 2_656 ? C23 O2 Pd2 Pd1 13.0(11) . . . . ? N3 Pd1 Pd2 N5 3.6(5) . . . 2_656 ? O1 Pd1 Pd2 N5 178.5(5) . . . 2_656 ? C17 Pd1 Pd2 N5 -84.8(7) . . . 2_656 ? N1 Pd1 Pd2 N5 94.8(6) . . . 2_656 ? N3 Pd1 Pd2 O2 176.4(5) . . . . ? O1 Pd1 Pd2 O2 -8.7(4) . . . . ? C17 Pd1 Pd2 O2 88.0(6) . . . . ? N1 Pd1 Pd2 O2 -92.4(6) . . . . ? N3 Pd1 Pd2 N4 70.2(5) . . . 2_656 ? O1 Pd1 Pd2 N4 -114.9(5) . . . 2_656 ? C17 Pd1 Pd2 N4 -18.2(7) . . . 2_656 ? N1 Pd1 Pd2 N4 161.4(6) . . . 2_656 ? N3 Pd1 Pd2 Cl1 -98.6(4) . . . . ? O1 Pd1 Pd2 Cl1 76.3(4) . . . . ? C17 Pd1 Pd2 Cl1 173.0(6) . . . . ? N1 Pd1 Pd2 Cl1 -7.4(5) . . . . ? N3 Pd1 Pd2 C16 36.2(5) . . . 2_656 ? O1 Pd1 Pd2 C16 -148.9(5) . . . 2_656 ? C17 Pd1 Pd2 C16 -52.2(7) . . . 2_656 ? N1 Pd1 Pd2 C16 127.4(6) . . . 2_656 ? C18 C17 C16 N5 5(2) . . . . ? Pd1 C17 C16 N5 -179.7(11) . . . . ? C18 C17 C16 N4 -169.2(14) . . . . ? Pd1 C17 C16 N4 6(2) . . . . ? C18 C17 C16 Pd2 28(13) . . . 2_656 ? Pd1 C17 C16 Pd2 -157(12) . . . 2_656 ? N3 C15 N4 C16 2(2) . . . . ? C14 C15 N4 C16 -175.2(13) . . . . ? N3 C15 N4 Pd2 -176.0(12) . . . 2_656 ? C14 C15 N4 Pd2 7(2) . . . 2_656 ? C17 C16 N4 C15 3(2) . . . . ? N5 C16 N4 C15 -172.5(12) . . . . ? Pd2 C16 N4 C15 -178.8(15) 2_656 . . . ? C17 C16 N4 Pd2 -178.4(15) . . . 2_656 ? N5 C16 N4 Pd2 6.3(10) . . . 2_656 ? C17 C16 N5 C21 -3(2) . . . . ? N4 C16 N5 C21 172.9(12) . . . . ? Pd2 C16 N5 C21 179.7(15) 2_656 . . . ? C17 C16 N5 Pd2 177.7(13) . . . 2_656 ? N4 C16 N5 Pd2 -6.8(11) . . . 2_656 ? C20 C21 N5 C16 -1(2) . . . . ? C22 C21 N5 C16 177.6(13) . . . . ? C20 C21 N5 Pd2 178.3(12) . . . 2_656 ? C22 C21 N5 Pd2 -3(2) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.476 _refine_diff_density_min -2.103 _refine_diff_density_rms 0.199 _exptl_crystal_recrystallization_method 'evap. of a sol. in CH2Cl2/n-Hexane '