Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Longgen Zhu' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing university 22 hankou lu Nanjing 210093 CHINA ; _publ_contact_author_email ZHULG@PUBLIC1.PTT.JS.CN _publ_section_title ; Synergic Effect of Two Metal Centers in Catalytic Hydrolysis of Methionine-Containing Peptides Promoted by Dinuclear Palladium(II) Hexaazacyclooctadecane Complex ; loop_ _publ_author_name 'Longgen Zhu' 'Zijian Guo' 'Jing Hong' 'Yi-Zhi Li' 'Ren Miao' ; Gaosheng Yang ; 'Chuenmei Zhao' data_31109am _database_code_depnum_ccdc_archive 'CCDC 253854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (I-Hydroxo)-(I-1,4,7,10,13,16-hexa-azacyclo-octadecane)-di- palladinm triperchlorate ; _chemical_name_common ; (I-Hydroxo)-(I-1,4,7,10,13,16-hexa-azacyclo-octadecane)-di- palladinm triperchlorate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H31 N6 O Pd2, 3(Cl O4)' _chemical_formula_sum 'C12 H31 Cl3 N6 O13 Pd2' _chemical_formula_weight 786.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.5368(7) _cell_length_b 13.2019(10) _cell_length_c 19.8900(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2504.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5542 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.83 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13483 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2791 _reflns_number_gt 2361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _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^)+(0.08P)^2^+1.88P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _chemical_absolute_configuration UNK _refine_ls_number_reflns 2791 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.004 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 0.51519(9) -0.01965(5) 0.08872(4) 0.0458(2) Uani 1 1 d . . . Pd2 Pd 0.49863(8) 0.01009(5) 0.24268(4) 0.0440(2) Uani 1 1 d . . . C1 C 0.2732(10) 0.0622(10) 0.0173(6) 0.046(3) Uani 1 1 d . . . H1A H 0.2624 0.1338 0.0272 0.056 Uiso 1 1 calc R . . H1B H 0.1876 0.0381 -0.0036 0.056 Uiso 1 1 calc R . . C2 C 0.3978(11) 0.0456(10) -0.0295(6) 0.054(3) Uani 1 1 d . . . H2A H 0.3970 -0.0235 -0.0460 0.064 Uiso 1 1 calc R . . H2B H 0.3905 0.0907 -0.0678 0.064 Uiso 1 1 calc R . . C3 C 0.6575(12) 0.0420(9) -0.0292(7) 0.057(3) Uani 1 1 d . . . H3A H 0.6810 0.0954 -0.0607 0.068 Uiso 1 1 calc R . . H3B H 0.6499 -0.0215 -0.0535 0.068 Uiso 1 1 calc R . . C4 C 0.7690(11) 0.0343(10) 0.0268(6) 0.054(3) Uani 1 1 d . . . H4A H 0.8563 0.0099 0.0077 0.065 Uiso 1 1 calc R . . H4B H 0.7859 0.1012 0.0454 0.065 Uiso 1 1 calc R . . C5 C 0.8149(12) -0.0300(8) 0.1392(5) 0.048(2) Uani 1 1 d . . . H5A H 0.9117 -0.0309 0.1244 0.058 Uiso 1 1 calc R . . H5B H 0.7992 -0.0909 0.1655 0.058 Uiso 1 1 calc R . . C6 C 0.7939(12) 0.0608(8) 0.1843(5) 0.048(2) Uani 1 1 d . . . H6A H 0.8852 0.0870 0.1970 0.058 Uiso 1 1 calc R . . H6B H 0.7463 0.1131 0.1589 0.058 Uiso 1 1 calc R . . C7 C 0.7308(10) 0.1237(8) 0.2953(5) 0.039(2) Uani 1 1 d . . . H7A H 0.7340 0.1885 0.2723 0.047 Uiso 1 1 calc R . . H7B H 0.8183 0.1149 0.3194 0.047 Uiso 1 1 calc R . . C8 C 0.6094(12) 0.1229(9) 0.3447(6) 0.050(3) Uani 1 1 d . . . H8A H 0.6131 0.0621 0.3720 0.060 Uiso 1 1 calc R . . H8B H 0.6155 0.1812 0.3742 0.060 Uiso 1 1 calc R . . C9 C 0.3526(10) 0.1138(8) 0.3450(5) 0.040(2) Uani 1 1 d . . . H9A H 0.3267 0.1765 0.3671 0.048 Uiso 1 1 calc R . . H9B H 0.3635 0.0612 0.3786 0.048 Uiso 1 1 calc R . . C10 C 0.2447(11) 0.0840(8) 0.2932(6) 0.047(3) Uani 1 1 d . . . H10A H 0.1562 0.0705 0.3155 0.057 Uiso 1 1 calc R . . H10B H 0.2305 0.1400 0.2624 0.057 Uiso 1 1 calc R . . C11 C 0.2009(12) -0.0244(9) 0.1961(5) 0.050(3) Uani 1 1 d . . . H11A H 0.1032 -0.0179 0.2091 0.060 Uiso 1 1 calc R . . H11B H 0.2155 -0.0937 0.1815 0.060 Uiso 1 1 calc R . . C12 C 0.2284(11) 0.0463(8) 0.1363(5) 0.044(2) Uani 1 1 d . . . H12A H 0.1386 0.0722 0.1211 0.053 Uiso 1 1 calc R . . H12B H 0.2819 0.1037 0.1527 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.9586(3) 0.27491(18) 0.46074(12) 0.0430(6) Uani 1 1 d . . . Cl2 Cl 0.0402(3) 0.3200(2) 0.19096(14) 0.0531(6) Uani 1 1 d . . . Cl3 Cl 0.5246(3) 0.3029(2) 0.11709(14) 0.0589(7) Uani 1 1 d . . . N1 N 0.3005(9) 0.0061(7) 0.0788(5) 0.051(2) Uani 1 1 d . . . H1C H 0.2622 -0.0562 0.0719 0.061 Uiso 1 1 calc R . . N2 N 0.5279(10) 0.0648(6) 0.0057(4) 0.0446(19) Uani 1 1 d . . . H2C H 0.5296 0.1312 0.0181 0.054 Uiso 1 1 calc R . . N3 N 0.7248(9) -0.0336(7) 0.0803(4) 0.044(2) Uani 1 1 d . . . H3C H 0.7379 -0.0968 0.0631 0.053 Uiso 1 1 calc R . . N4 N 0.7139(9) 0.0409(6) 0.2453(4) 0.0434(19) Uani 1 1 d . . . H4C H 0.7543 -0.0146 0.2643 0.052 Uiso 1 1 calc R . . N5 N 0.4778(10) 0.1259(6) 0.3069(4) 0.0472(19) Uani 1 1 d . . . H5C H 0.4731 0.1849 0.2833 0.057 Uiso 1 1 calc R . . N6 N 0.2873(9) -0.0060(6) 0.2549(4) 0.045(2) Uani 1 1 d . . . H6C H 0.2748 -0.0601 0.2827 0.054 Uiso 1 1 calc R . . O1 O 0.5119(7) -0.1094(5) 0.1751(3) 0.0418(15) Uani 1 1 d . . . H1F H 0.5865 -0.1029 0.1521 0.050 Uiso 1 1 d R . . O11 O 0.8439(8) 0.2967(6) 0.4160(4) 0.0543(18) Uani 1 1 d . . . O12 O 1.0878(8) 0.2397(6) 0.4296(5) 0.063(2) Uani 1 1 d . . . O13 O 0.9342(8) 0.2159(6) 0.5209(4) 0.057(2) Uani 1 1 d . . . O14 O 0.9633(8) 0.3782(5) 0.4857(3) 0.0525(18) Uani 1 1 d . . . O21 O 0.0436(8) 0.4283(5) 0.1806(3) 0.0487(17) Uani 1 1 d . . . O22 O -0.0788(7) 0.2862(6) 0.2305(4) 0.0469(17) Uani 1 1 d . . . O23 O 0.1625(8) 0.3133(6) 0.2340(4) 0.058(2) Uani 1 1 d . . . O24 O 0.0464(8) 0.2615(6) 0.1298(4) 0.061(2) Uani 1 1 d . . . O31 O 0.6622(8) 0.3413(6) 0.1315(4) 0.0556(19) Uani 1 1 d . . . O32 O 0.4961(9) 0.2698(5) 0.0493(3) 0.0533(17) Uani 1 1 d . . . O33 O 0.5065(8) 0.2245(5) 0.1674(3) 0.0463(16) Uani 1 1 d . . . O34 O 0.4423(7) 0.3944(5) 0.1252(3) 0.0480(17) 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 0.0485(4) 0.0435(4) 0.0452(4) -0.0036(3) 0.0049(4) -0.0035(4) Pd2 0.0480(4) 0.0384(4) 0.0456(4) -0.0041(3) -0.0055(4) -0.0060(4) C1 0.033(5) 0.059(7) 0.047(6) 0.006(5) -0.006(4) -0.015(5) C2 0.048(6) 0.060(7) 0.053(7) -0.006(6) -0.010(5) -0.016(5) C3 0.048(6) 0.048(7) 0.073(8) 0.000(6) -0.002(6) -0.015(5) C4 0.041(6) 0.066(8) 0.055(7) -0.003(6) 0.012(5) -0.008(5) C5 0.060(6) 0.043(5) 0.042(5) -0.003(5) 0.007(5) 0.005(5) C6 0.058(6) 0.035(5) 0.052(6) -0.009(5) -0.010(5) -0.006(5) C7 0.036(5) 0.034(5) 0.047(5) -0.001(5) -0.011(4) -0.009(4) C8 0.050(6) 0.042(6) 0.058(7) -0.006(5) 0.004(5) -0.014(5) C9 0.036(5) 0.035(5) 0.048(6) 0.000(5) -0.010(4) -0.009(4) C10 0.041(6) 0.041(6) 0.061(7) -0.002(6) 0.006(5) -0.004(4) C11 0.052(6) 0.052(6) 0.047(6) -0.010(5) 0.008(5) -0.013(5) C12 0.046(6) 0.042(6) 0.045(5) -0.009(5) 0.001(4) -0.010(4) Cl1 0.0369(12) 0.0413(13) 0.0508(12) -0.0011(9) -0.0072(10) -0.0134(9) Cl2 0.0480(14) 0.0527(15) 0.0586(14) -0.0045(11) -0.0023(12) -0.0182(12) Cl3 0.0462(15) 0.0602(15) 0.0704(16) -0.0010(13) -0.0016(14) -0.0148(13) N1 0.044(4) 0.043(5) 0.066(6) -0.004(5) -0.001(4) -0.012(4) N2 0.052(5) 0.046(4) 0.036(4) -0.003(3) 0.012(4) -0.011(4) N3 0.046(4) 0.041(5) 0.044(5) -0.010(4) -0.012(4) -0.004(4) N4 0.052(5) 0.035(4) 0.043(5) -0.002(4) -0.011(4) -0.006(4) N5 0.054(5) 0.042(4) 0.045(4) -0.003(3) 0.007(4) 0.002(4) N6 0.051(5) 0.035(4) 0.050(5) -0.004(4) -0.008(4) -0.002(4) O1 0.032(3) 0.056(4) 0.036(3) -0.007(3) -0.008(3) -0.010(3) O11 0.049(4) 0.055(4) 0.059(4) -0.006(4) -0.003(4) -0.011(3) O12 0.044(4) 0.059(5) 0.086(6) -0.005(5) -0.004(4) -0.016(4) O13 0.049(4) 0.052(4) 0.071(5) -0.005(4) 0.011(4) -0.009(4) O14 0.058(5) 0.051(4) 0.048(4) 0.000(3) 0.003(4) -0.010(4) O21 0.054(4) 0.043(4) 0.049(4) -0.002(3) -0.007(3) -0.007(3) O22 0.038(4) 0.049(4) 0.054(4) -0.001(3) -0.006(3) -0.017(3) O23 0.056(5) 0.049(4) 0.068(5) -0.003(4) -0.012(4) -0.021(4) O24 0.046(4) 0.061(5) 0.075(5) -0.005(4) -0.001(4) -0.012(4) O31 0.042(4) 0.062(5) 0.062(5) 0.001(4) 0.006(4) -0.007(4) O32 0.059(5) 0.048(4) 0.053(4) -0.004(3) -0.004(4) -0.008(4) O33 0.046(4) 0.039(3) 0.053(4) -0.005(3) -0.005(4) -0.010(4) O34 0.049(4) 0.047(4) 0.048(4) -0.004(3) -0.007(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.996(7) . ? Pd1 N3 2.014(8) . ? Pd1 N1 2.084(9) . ? Pd1 O1 2.088(6) . ? Pd1 Pd2 3.0913(11) . ? Pd2 N5 2.002(8) . ? Pd2 N6 2.041(8) . ? Pd2 O1 2.076(6) . ? Pd2 N4 2.094(8) . ? C1 N1 1.453(14) . ? C1 C2 1.526(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.447(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.450(14) . ? C3 C4 1.543(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.454(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.454(13) . ? C5 C6 1.510(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N4 1.456(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.486(13) . ? C7 C8 1.518(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N5 1.464(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N5 1.422(13) . ? C9 C10 1.508(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N6 1.469(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N6 1.451(13) . ? C11 C12 1.535(16) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N1 1.437(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? Cl1 O11 1.439(8) . ? Cl1 O13 1.447(8) . ? Cl1 O14 1.452(7) . ? Cl1 O12 1.456(9) . ? Cl2 O24 1.441(9) . ? Cl2 O21 1.445(7) . ? Cl2 O23 1.450(8) . ? Cl2 O22 1.451(7) . ? Cl3 O31 1.436(8) . ? Cl3 O32 1.443(7) . ? Cl3 O33 1.450(6) . ? Cl3 O34 1.450(8) . ? N1 H1C 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N4 H4C 0.9100 . ? N5 H5C 0.9100 . ? N6 H6C 0.9100 . ? O1 H1F 0.8500 . ? 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 N3 85.5(4) . . ? N2 Pd1 N1 83.7(4) . . ? N3 Pd1 N1 169.0(4) . . ? N2 Pd1 O1 177.3(3) . . ? N3 Pd1 O1 91.8(3) . . ? N1 Pd1 O1 99.0(3) . . ? N2 Pd1 Pd2 138.7(2) . . ? N3 Pd1 Pd2 98.3(2) . . ? N1 Pd1 Pd2 91.3(3) . . ? O1 Pd1 Pd2 41.93(16) . . ? N2 Pd1 H1F 153.5 . . ? N3 Pd1 H1F 68.2 . . ? N1 Pd1 H1F 122.4 . . ? O1 Pd1 H1F 23.8 . . ? Pd2 Pd1 H1F 53.5 . . ? N5 Pd2 N6 84.6(4) . . ? N5 Pd2 O1 177.7(3) . . ? N6 Pd2 O1 93.3(3) . . ? N5 Pd2 N4 86.2(4) . . ? N6 Pd2 N4 170.2(3) . . ? O1 Pd2 N4 96.0(3) . . ? N5 Pd2 Pd1 137.2(2) . . ? N6 Pd2 Pd1 98.9(2) . . ? O1 Pd2 Pd1 42.21(16) . . ? N4 Pd2 Pd1 90.0(2) . . ? N1 C1 C2 107.5(9) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 110.3(9) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C4 104.8(10) . . ? N2 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? N2 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? N3 C4 C3 111.6(9) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 115.2(9) . . ? N3 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N3 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N4 C6 C5 114.9(9) . . ? N4 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N4 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N4 C7 C8 110.2(8) . . ? N4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N5 C8 C7 108.8(9) . . ? N5 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? N5 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N5 C9 C10 103.8(9) . . ? N5 C9 H9A 111.0 . . ? C10 C9 H9A 111.0 . . ? N5 C9 H9B 111.0 . . ? C10 C9 H9B 111.0 . . ? H9A C9 H9B 109.0 . . ? N6 C10 C9 112.1(9) . . ? N6 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N6 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N6 C11 C12 115.2(8) . . ? N6 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N1 C12 C11 118.3(9) . . ? N1 C12 H12A 107.7 . . ? C11 C12 H12A 107.7 . . ? N1 C12 H12B 107.7 . . ? C11 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? O11 Cl1 O13 119.8(5) . . ? O11 Cl1 O14 92.7(5) . . ? O13 Cl1 O14 103.2(4) . . ? O11 Cl1 O12 116.4(5) . . ? O13 Cl1 O12 108.5(5) . . ? O14 Cl1 O12 114.8(5) . . ? O24 Cl2 O21 114.1(5) . . ? O24 Cl2 O23 115.6(5) . . ? O21 Cl2 O23 97.3(4) . . ? O24 Cl2 O22 109.0(4) . . ? O21 Cl2 O22 113.5(5) . . ? O23 Cl2 O22 106.9(4) . . ? O31 Cl3 O32 117.8(5) . . ? O31 Cl3 O33 102.9(5) . . ? O32 Cl3 O33 113.9(4) . . ? O31 Cl3 O34 100.3(5) . . ? O32 Cl3 O34 104.7(4) . . ? O33 Cl3 O34 117.0(4) . . ? C12 N1 C1 113.3(9) . . ? C12 N1 Pd1 117.1(7) . . ? C1 N1 Pd1 109.8(6) . . ? C12 N1 H1C 105.2 . . ? C1 N1 H1C 105.2 . . ? Pd1 N1 H1C 105.2 . . ? C2 N2 C3 117.6(8) . . ? C2 N2 Pd1 104.5(6) . . ? C3 N2 Pd1 109.4(7) . . ? C2 N2 H2C 108.4 . . ? C3 N2 H2C 108.4 . . ? Pd1 N2 H2C 108.4 . . ? C4 N3 C5 113.5(8) . . ? C4 N3 Pd1 107.0(7) . . ? C5 N3 Pd1 121.1(7) . . ? C4 N3 H3C 104.5 . . ? C5 N3 H3C 104.5 . . ? Pd1 N3 H3C 104.5 . . ? C6 N4 C7 111.6(8) . . ? C6 N4 Pd2 121.8(6) . . ? C7 N4 Pd2 105.4(6) . . ? C6 N4 H4C 105.6 . . ? C7 N4 H4C 105.6 . . ? Pd2 N4 H4C 105.6 . . ? C9 N5 C8 116.3(7) . . ? C9 N5 Pd2 109.7(7) . . ? C8 N5 Pd2 102.8(6) . . ? C9 N5 H5C 109.3 . . ? C8 N5 H5C 109.2 . . ? Pd2 N5 H5C 109.2 . . ? C11 N6 C10 113.3(9) . . ? C11 N6 Pd2 118.8(7) . . ? C10 N6 Pd2 104.5(6) . . ? C11 N6 H6C 106.5 . . ? C10 N6 H6C 106.5 . . ? Pd2 N6 H6C 106.5 . . ? Pd2 O1 Pd1 95.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.542 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.104