# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Armando J L Pombeiro' 'Maria de Fatima Guedes da Silva' 'Maximilian N Kopylovich' 'Jamal Lasri' _publ_contact_author_name 'Armando Pombeiro' _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_section_title ; Single-pot Template Transformations of Cyanopyridines on a PdII Centre: Syntheses of Ketoimine and 2,4-Dipyridyl-1,3, 5-Triazapentadiene Palladium(II) Complexes and their Catalytic Activity for Microwave-assisted Suzuki-Miyaura and Heck Cross-Coupling Reactions in Solid Phase ; # Attachment 'combinedcif.cif' data_jl247=compound3a _database_code_depnum_ccdc_archive 'CCDC 710109' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H15 Cl2 N3 O Pd), C H Cl3' _chemical_formula_sum 'C25 H31 Cl7 N6 O2 Pd2' _chemical_formula_weight 908.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.595(3) _cell_length_b 15.092(3) _cell_length_c 19.045(5) _cell_angle_alpha 66.858(12) _cell_angle_beta 89.921(10) _cell_angle_gamma 72.589(11) _cell_volume 3398.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6186 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6215 _exptl_absorpt_correction_T_max 0.7242 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _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 25641 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12399 _reflns_number_gt 7570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0475P)^2^+0.9258P] 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 SHELXL _refine_ls_extinction_coef 0.00044(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12399 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.0641(5) 0.1438(4) 0.3835(3) 0.0575(15) Uani 1 1 d . . . C2 C 0.3387(5) 0.8612(5) 0.3465(4) 0.0635(17) Uani 1 1 d . . . C3 C 0.0947(4) 0.6249(4) 0.3875(3) 0.0460(13) Uani 1 1 d . . . C4 C 0.3893(5) 0.2997(4) 0.3950(4) 0.0608(16) Uani 1 1 d . . . C10 C 0.3909(6) 0.3363(6) 0.7946(5) 0.105(3) Uani 1 1 d . . . H10 H 0.4546 0.3348 0.7681 0.126 Uiso 1 1 calc R . . C11 C 0.0058(4) 0.2602(4) 0.2557(3) 0.0509(14) Uani 1 1 d . . . C12 C -0.1064(4) 0.2665(5) 0.2568(4) 0.0679(18) Uani 1 1 d . . . H12A H -0.1395 0.2996 0.2905 0.081 Uiso 1 1 calc R . . H12B H -0.1137 0.1980 0.2749 0.081 Uiso 1 1 calc R . . C13 C -0.1543(5) 0.3316(5) 0.1724(4) 0.085(2) Uani 1 1 d . . . H13A H -0.1667 0.2881 0.1480 0.102 Uiso 1 1 calc R . . H13B H -0.2216 0.3830 0.1691 0.102 Uiso 1 1 calc R . . C14 C -0.0778(5) 0.3837(5) 0.1317(4) 0.0682(17) Uani 1 1 d . . . C15 C -0.0555(6) 0.3745(5) 0.0569(4) 0.099(2) Uani 1 1 d . . . H15A H -0.0081 0.4122 0.0331 0.148 Uiso 1 1 calc R . . H15B H -0.1207 0.4028 0.0221 0.148 Uiso 1 1 calc R . . H15C H -0.0232 0.3026 0.0669 0.148 Uiso 1 1 calc R . . C16 C -0.1104(5) 0.4952(4) 0.1198(4) 0.088(2) Uani 1 1 d . . . H16A H -0.0577 0.5250 0.0953 0.131 Uiso 1 1 calc R . . H16B H -0.1171 0.4993 0.1697 0.131 Uiso 1 1 calc R . . H16C H -0.1774 0.5327 0.0866 0.131 Uiso 1 1 calc R . . C20 C 0.7361(5) 0.0882(5) 0.1732(4) 0.0756(19) Uani 1 1 d . . . H20 H 0.8112 0.0698 0.1919 0.091 Uiso 1 1 calc R . . C21 C 0.3130(5) 0.9740(5) 0.2167(4) 0.0677(18) Uani 1 1 d . . . C22 C 0.4234(6) 0.9619(7) 0.2081(5) 0.116(3) Uani 1 1 d . . . H22A H 0.4619 0.8932 0.2111 0.139 Uiso 1 1 calc R . . H22B H 0.4576 0.9742 0.2476 0.139 Uiso 1 1 calc R . . C23 C 0.4149(7) 1.0481(9) 0.1238(5) 0.149(4) Uani 1 1 d . . . H23A H 0.4160 1.1119 0.1266 0.179 Uiso 1 1 calc R . . H23B H 0.4732 1.0256 0.0970 0.179 Uiso 1 1 calc R . . C24 C 0.3165(7) 1.0632(7) 0.0840(5) 0.097(3) Uani 1 1 d . . . C25 C 0.3157(8) 1.0015(8) 0.0389(5) 0.145(4) Uani 1 1 d . . . H25A H 0.3550 0.9298 0.0703 0.218 Uiso 1 1 calc R . . H25B H 0.3478 1.0263 -0.0079 0.218 Uiso 1 1 calc R . . H25C H 0.2438 1.0079 0.0248 0.218 Uiso 1 1 calc R . . C26 C 0.2584(8) 1.1757(8) 0.0284(5) 0.144(4) Uani 1 1 d . . . H26A H 0.1933 1.1801 0.0032 0.216 Uiso 1 1 calc R . . H26B H 0.3023 1.2001 -0.0107 0.216 Uiso 1 1 calc R . . H26C H 0.2430 1.2180 0.0577 0.216 Uiso 1 1 calc R . . C31 C 0.0651(4) 0.7155(4) 0.2534(3) 0.0457(13) Uani 1 1 d . . . C32 C -0.0473(4) 0.7272(4) 0.2413(3) 0.0509(14) Uani 1 1 d . . . H32A H -0.0905 0.7769 0.2600 0.061 Uiso 1 1 calc R . . H32B H -0.0594 0.6611 0.2683 0.061 Uiso 1 1 calc R . . C33 C -0.0718(4) 0.7654(4) 0.1551(3) 0.0556(15) Uani 1 1 d . . . H33A H -0.1426 0.8157 0.1367 0.067 Uiso 1 1 calc R . . H33B H -0.0677 0.7083 0.1406 0.067 Uiso 1 1 calc R . . C34 C 0.0095(5) 0.8148(4) 0.1205(3) 0.0558(15) Uani 1 1 d . . . C35 C 0.0504(5) 0.7914(5) 0.0539(3) 0.0767(19) Uani 1 1 d . . . H35A H 0.0740 0.7175 0.0694 0.115 Uiso 1 1 calc R . . H35B H 0.1088 0.8172 0.0389 0.115 Uiso 1 1 calc R . . H35C H -0.0050 0.8242 0.0102 0.115 Uiso 1 1 calc R . . C36 C -0.0251(5) 0.9282(4) 0.0992(4) 0.078(2) Uani 1 1 d . . . H36A H -0.0493 0.9414 0.1437 0.117 Uiso 1 1 calc R . . H36B H -0.0819 0.9631 0.0563 0.117 Uiso 1 1 calc R . . H36C H 0.0335 0.9536 0.0837 0.117 Uiso 1 1 calc R . . C41 C 0.3808(4) 0.3936(4) 0.2632(4) 0.0545(15) Uani 1 1 d . . . C42 C 0.4948(5) 0.3738(5) 0.2618(4) 0.084(2) Uani 1 1 d . . . H42A H 0.5319 0.3009 0.2749 0.100 Uiso 1 1 calc R . . H42B H 0.5240 0.3943 0.2983 0.100 Uiso 1 1 calc R . . C43 C 0.5025(6) 0.4390(7) 0.1797(5) 0.123(3) Uani 1 1 d . . . H43A H 0.5593 0.4004 0.1599 0.147 Uiso 1 1 calc R . . H43B H 0.5175 0.5005 0.1769 0.147 Uiso 1 1 calc R . . C44 C 0.3996(5) 0.4693(5) 0.1320(4) 0.076(2) Uani 1 1 d . . . C45 C 0.4033(8) 0.4059(7) 0.0876(5) 0.145(4) Uani 1 1 d . . . H45A H 0.3350 0.4275 0.0582 0.218 Uiso 1 1 calc R . . H45B H 0.4220 0.3340 0.1234 0.218 Uiso 1 1 calc R . . H45C H 0.4555 0.4146 0.0521 0.218 Uiso 1 1 calc R . . C46 C 0.3585(6) 0.5813(6) 0.0805(5) 0.120(3) Uani 1 1 d . . . H46A H 0.3549 0.6207 0.1115 0.180 Uiso 1 1 calc R . . H46B H 0.2888 0.5980 0.0549 0.180 Uiso 1 1 calc R . . H46C H 0.4050 0.5983 0.0416 0.180 Uiso 1 1 calc R . . C101 C 0.1575(5) 0.0673(4) 0.4410(4) 0.0555(15) Uani 1 1 d . . . C102 C 0.1453(6) 0.0030(5) 0.5127(4) 0.0742(19) Uani 1 1 d . . . H102 H 0.0779 0.0064 0.5274 0.089 Uiso 1 1 calc R . . C103 C 0.2330(7) -0.0667(5) 0.5630(5) 0.090(2) Uani 1 1 d . . . H103 H 0.2266 -0.1138 0.6121 0.108 Uiso 1 1 calc R . . C104 C 0.3273(7) -0.0674(5) 0.5421(5) 0.102(3) Uani 1 1 d . . . H104 H 0.3884 -0.1129 0.5768 0.122 Uiso 1 1 calc R . . C105 C 0.3341(6) -0.0008(5) 0.4693(5) 0.085(2) Uani 1 1 d . . . H105 H 0.4011 -0.0020 0.4546 0.102 Uiso 1 1 calc R . . C201 C 0.2854(4) 0.8076(4) 0.4103(3) 0.0539(15) Uani 1 1 d . . . C202 C 0.3405(5) 0.7293(5) 0.4787(4) 0.0724(19) Uani 1 1 d . . . H202 H 0.4143 0.7088 0.4857 0.087 Uiso 1 1 calc R . . C203 C 0.2902(5) 0.6812(5) 0.5360(4) 0.0707(18) Uani 1 1 d . . . H203 H 0.3278 0.6261 0.5824 0.085 Uiso 1 1 calc R . . C204 C 0.1844(5) 0.7147(4) 0.5246(4) 0.0648(17) Uani 1 1 d . . . H204 H 0.1468 0.6846 0.5640 0.078 Uiso 1 1 calc R . . C205 C 0.1320(5) 0.7925(4) 0.4556(4) 0.0626(16) Uani 1 1 d . . . H205 H 0.0582 0.8140 0.4482 0.075 Uiso 1 1 calc R . . C301 C 0.1747(4) 0.5436(4) 0.4522(3) 0.0439(12) Uani 1 1 d . . . C302 C 0.1487(5) 0.4893(4) 0.5226(3) 0.0552(15) Uani 1 1 d . . . H302 H 0.0782 0.5043 0.5319 0.066 Uiso 1 1 calc R . . C303 C 0.2254(5) 0.4138(4) 0.5788(3) 0.0627(17) Uani 1 1 d . . . H303 H 0.2081 0.3747 0.6270 0.075 Uiso 1 1 calc R . . C304 C 0.3265(5) 0.3946(4) 0.5660(3) 0.0652(17) Uani 1 1 d . . . H304 H 0.3804 0.3427 0.6050 0.078 Uiso 1 1 calc R . . C305 C 0.3494(5) 0.4523(4) 0.4948(4) 0.0604(16) Uani 1 1 d . . . H305 H 0.4199 0.4397 0.4857 0.073 Uiso 1 1 calc R . . C401 C 0.3282(5) 0.2572(4) 0.4575(4) 0.0561(15) Uani 1 1 d . . . C402 C 0.3764(5) 0.1839(5) 0.5297(4) 0.0760(19) Uani 1 1 d . . . H402 H 0.4501 0.1589 0.5407 0.091 Uiso 1 1 calc R . . C403 C 0.3161(7) 0.1471(5) 0.5859(4) 0.084(2) Uani 1 1 d . . . H403 H 0.3473 0.0959 0.6356 0.101 Uiso 1 1 calc R . . C404 C 0.2108(6) 0.1869(5) 0.5673(4) 0.080(2) Uani 1 1 d . . . H404 H 0.1678 0.1631 0.6048 0.096 Uiso 1 1 calc R . . C405 C 0.1650(5) 0.2614(5) 0.4947(4) 0.0688(18) Uani 1 1 d . . . H405 H 0.0914 0.2898 0.4837 0.083 Uiso 1 1 calc R . . N11 N 0.0870(3) 0.1967(3) 0.3123(3) 0.0493(11) Uani 1 1 d . . . N12 N 0.0161(4) 0.3251(4) 0.1897(3) 0.0640(13) Uani 1 1 d . . . H12 H 0.0765 0.3340 0.1796 0.077 Uiso 1 1 calc R . . N13 N 0.2498(4) 0.0662(3) 0.4178(3) 0.0591(13) Uani 1 1 d . . . N21 N 0.2709(4) 0.9335(4) 0.2802(3) 0.0560(12) Uani 1 1 d . . . N22 N 0.2584(5) 1.0338(4) 0.1495(3) 0.0825(17) Uani 1 1 d . . . H22 H 0.1899 1.0554 0.1437 0.099 Uiso 1 1 calc R . . N23 N 0.1813(4) 0.8390(3) 0.3985(3) 0.0513(11) Uani 1 1 d . . . N31 N 0.1343(3) 0.6637(3) 0.3192(2) 0.0442(10) Uani 1 1 d . . . N32 N 0.0917(3) 0.7630(3) 0.1872(3) 0.0542(12) Uani 1 1 d . . . H32 H 0.1557 0.7643 0.1822 0.065 Uiso 1 1 calc R . . N33 N 0.2743(3) 0.5258(3) 0.4381(2) 0.0458(11) Uani 1 1 d . . . N41 N 0.3301(3) 0.3639(3) 0.3245(3) 0.0497(11) Uani 1 1 d . . . N42 N 0.3350(4) 0.4450(4) 0.1930(3) 0.0722(15) Uani 1 1 d . . . H42 H 0.2669 0.4645 0.1825 0.087 Uiso 1 1 calc R . . N43 N 0.2238(4) 0.2937(3) 0.4399(3) 0.0543(12) Uani 1 1 d . . . O1 O -0.0217(3) 0.1548(3) 0.4046(3) 0.0803(13) Uani 1 1 d . . . O2 O 0.4317(4) 0.8373(4) 0.3566(3) 0.0992(17) Uani 1 1 d . . . O3 O 0.0048(3) 0.6526(3) 0.3982(2) 0.0619(11) Uani 1 1 d . . . O4 O 0.4825(4) 0.2738(4) 0.4110(3) 0.0879(14) Uani 1 1 d . . . Cl1 Cl 0.71191(18) -0.02365(16) 0.18698(15) 0.1176(8) Uani 1 1 d . . . Cl2 Cl 0.7150(2) 0.1688(2) 0.07810(14) 0.1434(10) Uani 1 1 d . . . Cl3 Cl 0.6643(2) 0.1435(2) 0.22771(16) 0.1494(11) Uani 1 1 d . . . Cl4 Cl 0.3436(2) 0.24596(19) 0.78625(16) 0.1370(9) Uani 1 1 d . . . Cl5 Cl 0.3008(2) 0.4564(2) 0.74753(17) 0.1434(10) Uani 1 1 d . . . Cl6 Cl 0.4273(3) 0.3077(3) 0.89067(16) 0.1824(15) Uani 1 1 d . . . Cl11 Cl 0.24392(14) 0.26675(13) 0.18107(11) 0.0834(5) Uani 1 1 d . . . Cl12 Cl 0.42363(14) 0.11811(15) 0.31844(15) 0.1041(7) Uani 1 1 d . . . Cl21 Cl 0.03558(13) 1.08713(11) 0.17618(9) 0.0722(5) Uani 1 1 d . . . Cl22 Cl -0.04879(12) 0.95995(14) 0.31997(11) 0.0883(6) Uani 1 1 d . . . Cl31 Cl 0.31996(12) 0.73289(13) 0.21558(10) 0.0734(5) Uani 1 1 d . . . Cl32 Cl 0.47164(12) 0.55600(14) 0.36138(11) 0.0829(5) Uani 1 1 d . . . Cl41 Cl 0.10902(12) 0.51756(11) 0.20436(9) 0.0648(4) Uani 1 1 d . . . Cl42 Cl 0.00034(12) 0.42712(12) 0.34859(10) 0.0709(4) Uani 1 1 d . . . Pd1 Pd 0.24579(3) 0.16395(3) 0.30771(3) 0.05703(15) Uani 1 1 d . . . Pd2 Pd 0.11583(3) 0.95340(3) 0.29345(2) 0.04891(13) Uani 1 1 d . . . Pd3 Pd 0.29439(3) 0.62009(3) 0.33252(2) 0.04548(13) Uani 1 1 d . . . Pd4 Pd 0.17083(3) 0.39781(3) 0.32908(3) 0.04698(13) 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 0.065(4) 0.060(4) 0.052(4) -0.022(3) 0.007(3) -0.028(3) C2 0.055(4) 0.071(4) 0.072(5) -0.035(4) 0.001(4) -0.024(3) C3 0.048(4) 0.055(3) 0.042(3) -0.023(3) 0.012(3) -0.023(3) C4 0.049(4) 0.063(4) 0.068(5) -0.030(3) 0.005(3) -0.009(3) C10 0.088(6) 0.142(7) 0.086(6) -0.027(5) 0.027(5) -0.067(6) C11 0.059(4) 0.053(3) 0.046(4) -0.021(3) 0.011(3) -0.023(3) C12 0.050(4) 0.077(4) 0.068(5) -0.021(3) 0.001(3) -0.022(3) C13 0.075(5) 0.092(5) 0.079(5) -0.018(4) -0.012(4) -0.039(4) C14 0.072(5) 0.072(4) 0.054(4) -0.020(3) -0.004(3) -0.021(4) C15 0.128(7) 0.100(6) 0.064(5) -0.039(4) 0.000(5) -0.024(5) C16 0.090(6) 0.066(4) 0.093(6) -0.025(4) -0.004(4) -0.018(4) C20 0.057(4) 0.076(4) 0.079(5) -0.023(4) 0.004(4) -0.013(3) C21 0.065(4) 0.097(5) 0.068(5) -0.051(4) 0.017(4) -0.041(4) C22 0.079(6) 0.218(10) 0.075(6) -0.065(6) 0.035(5) -0.075(6) C23 0.082(7) 0.291(14) 0.097(7) -0.088(9) 0.041(6) -0.081(8) C24 0.115(7) 0.137(7) 0.064(5) -0.047(5) 0.043(5) -0.067(6) C25 0.189(11) 0.197(10) 0.097(7) -0.090(8) 0.050(7) -0.088(9) C26 0.170(10) 0.183(10) 0.085(7) -0.038(7) 0.051(7) -0.087(9) C31 0.050(3) 0.046(3) 0.048(4) -0.023(3) 0.015(3) -0.020(3) C32 0.037(3) 0.056(3) 0.056(4) -0.019(3) 0.008(3) -0.014(3) C33 0.055(4) 0.060(3) 0.049(4) -0.021(3) -0.002(3) -0.015(3) C34 0.068(4) 0.055(3) 0.042(3) -0.019(3) 0.007(3) -0.019(3) C35 0.082(5) 0.088(5) 0.044(4) -0.017(3) 0.008(3) -0.019(4) C36 0.097(5) 0.052(4) 0.068(5) -0.012(3) 0.005(4) -0.017(4) C41 0.049(4) 0.051(3) 0.062(4) -0.022(3) 0.008(3) -0.016(3) C42 0.055(4) 0.101(5) 0.091(6) -0.034(4) 0.019(4) -0.025(4) C43 0.071(6) 0.140(7) 0.113(7) -0.002(6) 0.029(5) -0.043(5) C44 0.063(5) 0.093(5) 0.069(5) -0.024(4) 0.032(4) -0.035(4) C45 0.197(11) 0.196(10) 0.144(9) -0.119(8) 0.130(9) -0.138(9) C46 0.109(7) 0.099(6) 0.103(7) 0.001(5) 0.032(6) -0.024(5) C101 0.063(4) 0.053(3) 0.062(4) -0.030(3) 0.008(3) -0.024(3) C102 0.084(5) 0.069(4) 0.067(5) -0.019(4) 0.003(4) -0.034(4) C103 0.121(7) 0.071(5) 0.073(5) -0.021(4) -0.002(5) -0.035(5) C104 0.115(8) 0.066(5) 0.084(6) -0.013(4) -0.028(6) 0.004(5) C105 0.066(5) 0.073(5) 0.099(6) -0.035(5) -0.003(4) -0.002(4) C201 0.051(4) 0.055(3) 0.060(4) -0.028(3) 0.000(3) -0.017(3) C202 0.053(4) 0.068(4) 0.081(5) -0.022(4) -0.014(4) -0.012(3) C203 0.079(5) 0.059(4) 0.063(5) -0.016(3) -0.014(4) -0.019(4) C204 0.084(5) 0.050(3) 0.053(4) -0.014(3) 0.009(4) -0.022(3) C205 0.062(4) 0.066(4) 0.060(4) -0.026(3) 0.015(3) -0.023(3) C301 0.041(3) 0.055(3) 0.043(3) -0.025(3) 0.006(3) -0.020(3) C302 0.057(4) 0.070(4) 0.044(4) -0.021(3) 0.013(3) -0.031(3) C303 0.067(4) 0.073(4) 0.049(4) -0.016(3) 0.006(3) -0.037(4) C304 0.070(5) 0.064(4) 0.046(4) -0.009(3) -0.002(3) -0.019(3) C305 0.047(4) 0.071(4) 0.061(4) -0.026(3) 0.006(3) -0.018(3) C401 0.054(4) 0.056(3) 0.063(4) -0.032(3) 0.004(3) -0.014(3) C402 0.076(5) 0.069(4) 0.070(5) -0.020(4) 0.001(4) -0.017(4) C403 0.108(6) 0.067(4) 0.065(5) -0.010(4) 0.012(5) -0.034(5) C404 0.107(6) 0.067(4) 0.069(5) -0.023(4) 0.031(5) -0.042(4) C405 0.080(5) 0.065(4) 0.069(5) -0.028(4) 0.019(4) -0.033(4) N11 0.053(3) 0.051(3) 0.050(3) -0.024(2) 0.011(2) -0.021(2) N12 0.068(4) 0.071(3) 0.053(3) -0.022(3) 0.011(3) -0.029(3) N13 0.058(3) 0.052(3) 0.069(4) -0.032(3) 0.004(3) -0.012(3) N21 0.054(3) 0.074(3) 0.054(3) -0.033(3) 0.012(3) -0.032(3) N22 0.090(5) 0.109(5) 0.061(4) -0.039(4) 0.028(4) -0.043(4) N23 0.049(3) 0.050(3) 0.057(3) -0.026(2) 0.003(2) -0.014(2) N31 0.048(3) 0.053(3) 0.037(3) -0.020(2) 0.009(2) -0.021(2) N32 0.048(3) 0.064(3) 0.045(3) -0.014(2) 0.007(2) -0.021(2) N33 0.044(3) 0.052(3) 0.046(3) -0.022(2) 0.008(2) -0.019(2) N41 0.045(3) 0.054(3) 0.057(3) -0.028(2) 0.011(2) -0.018(2) N42 0.051(3) 0.095(4) 0.064(4) -0.025(3) 0.019(3) -0.024(3) N43 0.068(4) 0.050(3) 0.055(3) -0.026(2) 0.015(3) -0.027(3) O1 0.062(3) 0.105(3) 0.064(3) -0.021(3) 0.025(2) -0.032(3) O2 0.050(3) 0.121(4) 0.098(4) -0.016(3) 0.000(3) -0.028(3) O3 0.047(3) 0.080(3) 0.050(3) -0.023(2) 0.016(2) -0.014(2) O4 0.055(3) 0.118(4) 0.074(3) -0.029(3) 0.003(3) -0.019(3) Cl1 0.1103(17) 0.0960(15) 0.148(2) -0.0442(15) 0.0160(16) -0.0443(13) Cl2 0.162(2) 0.134(2) 0.0841(17) -0.0016(14) 0.0159(16) -0.0379(18) Cl3 0.142(2) 0.156(2) 0.127(2) -0.0840(19) 0.0200(18) 0.0195(18) Cl4 0.137(2) 0.1310(19) 0.143(2) -0.0341(17) 0.0174(18) -0.0737(17) Cl5 0.132(2) 0.147(2) 0.143(2) -0.0690(19) 0.0493(19) -0.0208(18) Cl6 0.203(3) 0.284(4) 0.0903(19) -0.039(2) 0.026(2) -0.171(3) Cl11 0.0859(13) 0.0830(11) 0.0920(14) -0.0380(10) 0.0467(11) -0.0396(10) Cl12 0.0543(11) 0.1080(15) 0.157(2) -0.0629(15) 0.0327(12) -0.0250(10) Cl21 0.0804(12) 0.0642(9) 0.0554(10) -0.0131(8) -0.0013(8) -0.0162(8) Cl22 0.0483(10) 0.1025(13) 0.0751(12) -0.0040(10) 0.0059(9) -0.0151(9) Cl31 0.0614(10) 0.0905(11) 0.0640(11) -0.0163(9) 0.0225(8) -0.0401(9) Cl32 0.0437(9) 0.1114(13) 0.0783(12) -0.0221(10) 0.0121(8) -0.0275(9) Cl41 0.0562(9) 0.0611(9) 0.0642(10) -0.0210(8) 0.0065(8) -0.0081(7) Cl42 0.0491(9) 0.0874(11) 0.0781(12) -0.0388(9) 0.0202(8) -0.0185(8) Pd1 0.0513(3) 0.0582(3) 0.0763(4) -0.0385(3) 0.0205(2) -0.0232(2) Pd2 0.0489(3) 0.0504(3) 0.0476(3) -0.0211(2) 0.0041(2) -0.0151(2) Pd3 0.0414(3) 0.0568(3) 0.0459(3) -0.0242(2) 0.0130(2) -0.0223(2) Pd4 0.0453(3) 0.0478(2) 0.0538(3) -0.0269(2) 0.0111(2) -0.0152(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.218(7) . ? C1 N11 1.367(7) . ? C1 C101 1.509(8) . ? C2 O2 1.199(7) . ? C2 N21 1.397(8) . ? C2 C201 1.494(8) . ? C3 O3 1.213(6) . ? C3 N31 1.384(6) . ? C3 C301 1.492(7) . ? C4 O4 1.210(7) . ? C4 N41 1.379(7) . ? C4 C401 1.494(8) . ? C10 Cl5 1.728(9) . ? C10 Cl4 1.730(8) . ? C10 Cl6 1.742(8) . ? C10 H10 1.0000 . ? C11 N12 1.294(7) . ? C11 N11 1.363(7) . ? C11 C12 1.500(7) . ? C12 C13 1.534(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.520(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N12 1.480(7) . ? C14 C15 1.506(9) . ? C14 C16 1.527(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C20 Cl2 1.704(7) . ? C20 Cl3 1.708(7) . ? C20 Cl1 1.735(6) . ? C20 H20 1.0000 . ? C21 N22 1.302(8) . ? C21 N21 1.339(8) . ? C21 C22 1.473(9) . ? C22 C23 1.598(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.449(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N22 1.466(8) . ? C24 C25 1.498(10) . ? C24 C26 1.554(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 N32 1.296(6) . ? C31 N31 1.363(7) . ? C31 C32 1.493(7) . ? C32 C33 1.510(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.522(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N32 1.474(7) . ? C34 C35 1.508(8) . ? C34 C36 1.513(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C41 N42 1.294(7) . ? C41 N41 1.345(7) . ? C41 C42 1.491(8) . ? C42 C43 1.509(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.511(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N42 1.453(7) . ? C44 C45 1.497(10) . ? C44 C46 1.505(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C101 N13 1.327(7) . ? C101 C102 1.374(8) . ? C102 C103 1.381(9) . ? C102 H102 0.9500 . ? C103 C104 1.340(10) . ? C103 H103 0.9500 . ? C104 C105 1.379(10) . ? C104 H104 0.9500 . ? C105 N13 1.352(8) . ? C105 H105 0.9500 . ? C201 N23 1.339(7) . ? C201 C202 1.385(8) . ? C202 C203 1.363(8) . ? C202 H202 0.9500 . ? C203 C204 1.361(8) . ? C203 H203 0.9500 . ? C204 C205 1.379(8) . ? C204 H204 0.9500 . ? C205 N23 1.343(7) . ? C205 H205 0.9500 . ? C301 N33 1.347(6) . ? C301 C302 1.380(7) . ? C302 C303 1.366(8) . ? C302 H302 0.9500 . ? C303 C304 1.360(8) . ? C303 H303 0.9500 . ? C304 C305 1.389(8) . ? C304 H304 0.9500 . ? C305 N33 1.350(7) . ? C305 H305 0.9500 . ? C401 N43 1.349(7) . ? C401 C402 1.385(8) . ? C402 C403 1.389(9) . ? C402 H402 0.9500 . ? C403 C404 1.362(9) . ? C403 H403 0.9500 . ? C404 C405 1.388(9) . ? C404 H404 0.9500 . ? C405 N43 1.340(7) . ? C405 H405 0.9500 . ? N11 Pd1 2.075(4) . ? N12 H12 0.8800 . ? N13 Pd1 2.024(5) . ? N21 Pd2 2.068(4) . ? N22 H22 0.8800 . ? N23 Pd2 2.036(5) . ? N31 Pd3 2.062(4) . ? N32 H32 0.8800 . ? N33 Pd3 2.030(4) . ? N41 Pd4 2.080(4) . ? N42 H42 0.8800 . ? N43 Pd4 2.040(5) . ? Cl11 Pd1 2.2935(19) . ? Cl12 Pd1 2.2924(18) . ? Cl21 Pd2 2.3233(17) . ? Cl22 Pd2 2.2754(17) . ? Cl31 Pd3 2.3133(16) . ? Cl32 Pd3 2.2882(17) . ? Cl41 Pd4 2.3102(17) . ? Cl42 Pd4 2.2847(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N11 126.8(6) . . ? O1 C1 C101 118.6(6) . . ? N11 C1 C101 114.6(5) . . ? O2 C2 N21 127.9(6) . . ? O2 C2 C201 118.3(6) . . ? N21 C2 C201 113.7(5) . . ? O3 C3 N31 126.2(5) . . ? O3 C3 C301 120.0(5) . . ? N31 C3 C301 113.8(5) . . ? O4 C4 N41 128.0(6) . . ? O4 C4 C401 117.8(6) . . ? N41 C4 C401 114.2(5) . . ? Cl5 C10 Cl4 109.9(4) . . ? Cl5 C10 Cl6 112.5(5) . . ? Cl4 C10 Cl6 111.3(4) . . ? Cl5 C10 H10 107.6 . . ? Cl4 C10 H10 107.6 . . ? Cl6 C10 H10 107.6 . . ? N12 C11 N11 123.4(5) . . ? N12 C11 C12 108.8(5) . . ? N11 C11 C12 127.8(5) . . ? C11 C12 C13 103.6(5) . . ? C11 C12 H12A 111.1 . . ? C13 C12 H12A 111.1 . . ? C11 C12 H12B 111.1 . . ? C13 C12 H12B 111.1 . . ? H12A C12 H12B 109.0 . . ? C14 C13 C12 107.3(5) . . ? C14 C13 H13A 110.2 . . ? C12 C13 H13A 110.2 . . ? C14 C13 H13B 110.2 . . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? N12 C14 C15 110.0(6) . . ? N12 C14 C13 100.6(5) . . ? C15 C14 C13 114.2(6) . . ? N12 C14 C16 109.1(5) . . ? C15 C14 C16 110.4(6) . . ? C13 C14 C16 112.1(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl2 C20 Cl3 112.4(4) . . ? Cl2 C20 Cl1 111.4(4) . . ? Cl3 C20 Cl1 109.9(4) . . ? Cl2 C20 H20 107.6 . . ? Cl3 C20 H20 107.6 . . ? Cl1 C20 H20 107.6 . . ? N22 C21 N21 123.3(6) . . ? N22 C21 C22 108.1(6) . . ? N21 C21 C22 128.7(7) . . ? C21 C22 C23 101.5(7) . . ? C21 C22 H22A 111.5 . . ? C23 C22 H22A 111.5 . . ? C21 C22 H22B 111.5 . . ? C23 C22 H22B 111.5 . . ? H22A C22 H22B 109.3 . . ? C24 C23 C22 105.3(7) . . ? C24 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? C24 C23 H23B 110.7 . . ? C22 C23 H23B 110.7 . . ? H23A C23 H23B 108.8 . . ? C23 C24 N22 100.2(7) . . ? C23 C24 C25 118.2(9) . . ? N22 C24 C25 109.5(6) . . ? C23 C24 C26 114.0(8) . . ? N22 C24 C26 108.7(7) . . ? C25 C24 C26 105.8(8) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N32 C31 N31 122.3(5) . . ? N32 C31 C32 107.9(5) . . ? N31 C31 C32 129.8(5) . . ? C31 C32 C33 104.0(4) . . ? C31 C32 H32A 111.0 . . ? C33 C32 H32A 111.0 . . ? C31 C32 H32B 111.0 . . ? C33 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? C32 C33 C34 105.8(4) . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33B 110.6 . . ? C34 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? N32 C34 C35 109.7(5) . . ? N32 C34 C36 108.8(5) . . ? C35 C34 C36 110.9(5) . . ? N32 C34 C33 99.8(4) . . ? C35 C34 C33 113.4(5) . . ? C36 C34 C33 113.6(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N42 C41 N41 123.6(5) . . ? N42 C41 C42 108.0(5) . . ? N41 C41 C42 128.3(6) . . ? C41 C42 C43 103.6(6) . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42B 111.0 . . ? C43 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C42 C43 C44 107.8(5) . . ? C42 C43 H43A 110.2 . . ? C44 C43 H43A 110.2 . . ? C42 C43 H43B 110.2 . . ? C44 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? N42 C44 C45 110.0(5) . . ? N42 C44 C46 109.7(6) . . ? C45 C44 C46 111.4(7) . . ? N42 C44 C43 99.9(6) . . ? C45 C44 C43 112.3(7) . . ? C46 C44 C43 112.9(6) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N13 C101 C102 123.1(6) . . ? N13 C101 C1 116.2(5) . . ? C102 C101 C1 120.7(6) . . ? C101 C102 C103 118.6(7) . . ? C101 C102 H102 120.7 . . ? C103 C102 H102 120.7 . . ? C104 C103 C102 119.6(8) . . ? C104 C103 H103 120.2 . . ? C102 C103 H103 120.2 . . ? C103 C104 C105 118.8(8) . . ? C103 C104 H104 120.6 . . ? C105 C104 H104 120.6 . . ? N13 C105 C104 123.1(7) . . ? N13 C105 H105 118.5 . . ? C104 C105 H105 118.5 . . ? N23 C201 C202 121.2(6) . . ? N23 C201 C2 116.9(5) . . ? C202 C201 C2 121.9(6) . . ? C203 C202 C201 120.9(6) . . ? C203 C202 H202 119.6 . . ? C201 C202 H202 119.6 . . ? C202 C203 C204 117.8(6) . . ? C202 C203 H203 121.1 . . ? C204 C203 H203 121.1 . . ? C203 C204 C205 119.8(6) . . ? C203 C204 H204 120.1 . . ? C205 C204 H204 120.1 . . ? N23 C205 C204 122.6(6) . . ? N23 C205 H205 118.7 . . ? C204 C205 H205 118.7 . . ? N33 C301 C302 121.7(5) . . ? N33 C301 C3 116.2(5) . . ? C302 C301 C3 122.1(5) . . ? C303 C302 C301 119.3(5) . . ? C303 C302 H302 120.4 . . ? C301 C302 H302 120.4 . . ? C304 C303 C302 120.2(6) . . ? C304 C303 H303 119.9 . . ? C302 C303 H303 119.9 . . ? C303 C304 C305 118.7(6) . . ? C303 C304 H304 120.7 . . ? C305 C304 H304 120.7 . . ? N33 C305 C304 121.9(5) . . ? N33 C305 H305 119.0 . . ? C304 C305 H305 119.0 . . ? N43 C401 C402 121.7(6) . . ? N43 C401 C4 116.6(5) . . ? C402 C401 C4 121.7(6) . . ? C401 C402 C403 119.5(7) . . ? C401 C402 H402 120.3 . . ? C403 C402 H402 120.3 . . ? C404 C403 C402 117.7(7) . . ? C404 C403 H403 121.1 . . ? C402 C403 H403 121.1 . . ? C403 C404 C405 121.3(7) . . ? C403 C404 H404 119.3 . . ? C405 C404 H404 119.3 . . ? N43 C405 C404 120.5(7) . . ? N43 C405 H405 119.7 . . ? C404 C405 H405 119.7 . . ? C11 N11 C1 117.5(5) . . ? C11 N11 Pd1 129.7(4) . . ? C1 N11 Pd1 112.8(4) . . ? C11 N12 C14 117.3(5) . . ? C11 N12 H12 121.3 . . ? C14 N12 H12 121.3 . . ? C101 N13 C105 116.7(6) . . ? C101 N13 Pd1 115.1(4) . . ? C105 N13 Pd1 128.1(5) . . ? C21 N21 C2 117.5(5) . . ? C21 N21 Pd2 128.9(4) . . ? C2 N21 Pd2 113.3(4) . . ? C21 N22 C24 116.7(7) . . ? C21 N22 H22 121.7 . . ? C24 N22 H22 121.7 . . ? C205 N23 C201 117.7(5) . . ? C205 N23 Pd2 127.4(4) . . ? C201 N23 Pd2 114.9(4) . . ? C31 N31 C3 117.0(4) . . ? C31 N31 Pd3 129.5(3) . . ? C3 N31 Pd3 113.2(3) . . ? C31 N32 C34 116.7(5) . . ? C31 N32 H32 121.6 . . ? C34 N32 H32 121.6 . . ? C301 N33 C305 118.3(5) . . ? C301 N33 Pd3 114.7(3) . . ? C305 N33 Pd3 127.0(4) . . ? C41 N41 C4 117.5(5) . . ? C41 N41 Pd4 129.1(4) . . ? C4 N41 Pd4 113.3(4) . . ? C41 N42 C44 117.9(5) . . ? C41 N42 H42 121.1 . . ? C44 N42 H42 121.1 . . ? C405 N43 C401 119.2(5) . . ? C405 N43 Pd4 126.2(4) . . ? C401 N43 Pd4 114.7(4) . . ? N13 Pd1 N11 81.10(19) . . ? N13 Pd1 Cl12 92.23(16) . . ? N11 Pd1 Cl12 173.11(14) . . ? N13 Pd1 Cl11 176.67(13) . . ? N11 Pd1 Cl11 99.73(14) . . ? Cl12 Pd1 Cl11 87.03(8) . . ? N23 Pd2 N21 80.97(19) . . ? N23 Pd2 Cl22 92.96(14) . . ? N21 Pd2 Cl22 173.86(15) . . ? N23 Pd2 Cl21 177.50(14) . . ? N21 Pd2 Cl21 100.97(15) . . ? Cl22 Pd2 Cl21 85.13(6) . . ? N33 Pd3 N31 80.70(17) . . ? N33 Pd3 Cl32 92.34(13) . . ? N31 Pd3 Cl32 172.97(12) . . ? N33 Pd3 Cl31 176.70(12) . . ? N31 Pd3 Cl31 100.26(12) . . ? Cl32 Pd3 Cl31 86.74(6) . . ? N43 Pd4 N41 80.71(19) . . ? N43 Pd4 Cl42 93.24(14) . . ? N41 Pd4 Cl42 173.67(14) . . ? N43 Pd4 Cl41 179.04(14) . . ? N41 Pd4 Cl41 99.92(14) . . ? Cl42 Pd4 Cl41 86.11(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.746 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.088 #===END data_jl253=compound3a' _database_code_depnum_ccdc_archive 'CCDC 710110' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Cl2 N6 O2 Pd2' _chemical_formula_sum 'C24 H28 Cl2 N6 O2 Pd2' _chemical_formula_weight 716.22 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 MONOCLINIC _symmetry_space_group_name_H-M P21/C _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.032(4) _cell_length_b 13.255(4) _cell_length_c 16.918(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.612(12) _cell_angle_gamma 90.00 _cell_volume 2689.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6611 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.46 _exptl_crystal_description RHOMBOHEDRON _exptl_crystal_colour WHITE _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6677 _exptl_absorpt_correction_T_max 0.7340 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _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 52244 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.54 _reflns_number_total 8224 _reflns_number_gt 7016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0263P)^2^+1.3156P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8224 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.48071(19) 0.12026(18) 0.98442(14) 0.0359(5) Uani 1 1 d . . . H1 H 0.5438 0.1269 1.0216 0.043 Uiso 1 1 calc R . . C2 C 0.3764(2) 0.1090(2) 1.01204(16) 0.0439(5) Uani 1 1 d . . . H2 H 0.3682 0.1069 1.0674 0.053 Uiso 1 1 calc R . . C3 C 0.2844(2) 0.1011(2) 0.95827(17) 0.0458(6) Uani 1 1 d . . . H3 H 0.2120 0.0933 0.9760 0.055 Uiso 1 1 calc R . . C4 C 0.29911(17) 0.10445(18) 0.87858(16) 0.0388(5) Uani 1 1 d . . . H4 H 0.2367 0.1000 0.8406 0.047 Uiso 1 1 calc R . . C5 C 0.40560(16) 0.11438(15) 0.85431(13) 0.0286(4) Uani 1 1 d . . . C6 C 0.42834(16) 0.11022(15) 0.76893(12) 0.0283(4) Uani 1 1 d . . . C7 C 0.57894(16) 0.09101(15) 0.68803(11) 0.0267(4) Uani 1 1 d . . . C8 C 0.5241(2) 0.1184(2) 0.60821(13) 0.0430(5) Uani 1 1 d . . . H8A H 0.5016 0.1903 0.6061 0.052 Uiso 1 1 calc R . . H8B H 0.4579 0.0757 0.5942 0.052 Uiso 1 1 calc R . . C9 C 0.6161(2) 0.0976(2) 0.55440(14) 0.0454(6) Uani 1 1 d . . . H9A H 0.6545 0.1610 0.5418 0.054 Uiso 1 1 calc R . . H9B H 0.5854 0.0661 0.5042 0.054 Uiso 1 1 calc R . . C10 C 0.6972(2) 0.02494(19) 0.60100(12) 0.0375(5) Uani 1 1 d . . . C11 C 0.6739(3) -0.0851(2) 0.57724(16) 0.0555(7) Uani 1 1 d . . . H11A H 0.5952 -0.1005 0.5824 0.083 Uiso 1 1 calc R . . H11B H 0.7208 -0.1297 0.6120 0.083 Uiso 1 1 calc R . . H11C H 0.6910 -0.0953 0.5221 0.083 Uiso 1 1 calc R . . C12 C 0.8182(2) 0.0527(3) 0.59372(17) 0.0615(9) Uani 1 1 d . . . H12A H 0.8303 0.1233 0.6093 0.092 Uiso 1 1 calc R . . H12B H 0.8361 0.0435 0.5387 0.092 Uiso 1 1 calc R . . H12C H 0.8663 0.0091 0.6285 0.092 Uiso 1 1 calc R . . N21 N 0.82914(14) -0.13605(13) 0.85147(10) 0.0280(3) Uani 1 1 d . . . C22 C 0.80498(19) -0.23140(17) 0.86946(14) 0.0361(5) Uani 1 1 d . . . H22 H 0.7383 -0.2612 0.8463 0.043 Uiso 1 1 calc R . . C23 C 0.8755(2) -0.2875(2) 0.92125(16) 0.0447(6) Uani 1 1 d . . . H23 H 0.8578 -0.3555 0.9328 0.054 Uiso 1 1 calc R . . C24 C 0.9709(2) -0.2441(2) 0.95572(15) 0.0472(6) Uani 1 1 d . . . H24 H 1.0185 -0.2809 0.9928 0.057 Uiso 1 1 calc R . . C25 C 0.99706(19) -0.1460(2) 0.93577(14) 0.0411(5) Uani 1 1 d . . . H25 H 1.0633 -0.1148 0.9582 0.049 Uiso 1 1 calc R . . C26 C 0.92503(16) -0.09489(17) 0.88283(12) 0.0305(4) Uani 1 1 d . . . C27 C 0.94848(16) 0.01173(17) 0.85882(13) 0.0316(4) Uani 1 1 d . . . C28 C 0.86219(16) 0.15200(15) 0.79457(12) 0.0276(4) Uani 1 1 d . . . C29 C 0.95605(19) 0.2166(2) 0.76950(17) 0.0443(6) Uani 1 1 d . . . H29A H 0.9704 0.2041 0.7135 0.053 Uiso 1 1 calc R . . H29B H 1.0255 0.2054 0.8038 0.053 Uiso 1 1 calc R . . C30 C 0.9096(3) 0.3219(2) 0.7806(2) 0.0646(9) Uani 1 1 d . . . H30A H 0.9277 0.3666 0.7365 0.078 Uiso 1 1 calc R . . H30B H 0.9415 0.3515 0.8312 0.078 Uiso 1 1 calc R . . C31 C 0.7839(2) 0.30964(16) 0.78151(14) 0.0357(5) Uani 1 1 d . . . C32 C 0.7202(3) 0.3280(2) 0.70223(17) 0.0595(8) Uani 1 1 d . . . H32A H 0.7503 0.2849 0.6620 0.089 Uiso 1 1 calc R . . H32B H 0.7276 0.3989 0.6873 0.089 Uiso 1 1 calc R . . H32C H 0.6413 0.3120 0.7060 0.089 Uiso 1 1 calc R . . C33 C 0.7374(3) 0.3766(2) 0.84369(18) 0.0586(8) Uani 1 1 d . . . H33A H 0.7787 0.3648 0.8951 0.088 Uiso 1 1 calc R . . H33B H 0.6584 0.3607 0.8475 0.088 Uiso 1 1 calc R . . H33C H 0.7449 0.4475 0.8286 0.088 Uiso 1 1 calc R . . N1 N 0.49527(13) 0.12208(13) 0.90723(10) 0.0271(3) Uani 1 1 d . . . N2 N 0.53973(13) 0.11569(13) 0.75942(10) 0.0256(3) Uani 1 1 d . . . N23 N 0.77233(13) 0.20034(12) 0.80270(9) 0.0251(3) Uani 1 1 d . . . N22 N 0.86728(13) 0.04877(13) 0.80686(10) 0.0272(3) Uani 1 1 d . . . N3 N 0.66893(14) 0.04028(12) 0.68486(9) 0.0262(3) Uani 1 1 d . . . O6 O 0.35312(13) 0.09619(13) 0.71723(10) 0.0387(4) Uani 1 1 d . . . O27 O 1.03056(14) 0.05646(15) 0.88808(13) 0.0517(5) Uani 1 1 d . . . Cl1 Cl 0.74320(4) 0.17058(5) 0.97581(3) 0.03582(11) Uani 1 1 d . . . Cl2 Cl 0.58982(5) -0.15157(4) 0.75665(4) 0.04275(14) Uani 1 1 d . . . Pd1 Pd 0.639190(11) 0.148878(11) 0.857150(8) 0.02151(4) Uani 1 1 d . . . Pd2 Pd 0.739777(11) -0.044888(11) 0.774404(8) 0.02349(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 0.0303(10) 0.0439(12) 0.0343(11) 0.0011(9) 0.0081(8) 0.0009(9) C2 0.0375(12) 0.0514(14) 0.0454(13) -0.0002(11) 0.0179(10) 0.0019(11) C3 0.0270(10) 0.0514(15) 0.0617(16) -0.0056(12) 0.0199(10) -0.0030(10) C4 0.0214(9) 0.0400(12) 0.0552(14) -0.0068(10) 0.0032(9) -0.0022(8) C5 0.0236(9) 0.0238(9) 0.0382(11) -0.0026(8) 0.0011(8) 0.0011(7) C6 0.0244(9) 0.0234(9) 0.0360(10) -0.0023(7) -0.0046(7) 0.0016(7) C7 0.0301(9) 0.0270(9) 0.0219(8) -0.0009(7) -0.0052(7) -0.0011(7) C8 0.0486(13) 0.0522(14) 0.0262(10) 0.0026(9) -0.0087(9) 0.0101(11) C9 0.0559(15) 0.0555(15) 0.0243(10) 0.0046(10) 0.0000(10) 0.0016(12) C10 0.0425(12) 0.0479(13) 0.0221(9) -0.0059(9) 0.0033(8) -0.0003(10) C11 0.076(2) 0.0537(16) 0.0362(13) -0.0175(12) 0.0006(13) 0.0088(15) C12 0.0460(15) 0.105(3) 0.0356(13) -0.0030(14) 0.0145(11) -0.0052(15) N21 0.0236(7) 0.0312(9) 0.0292(8) -0.0006(6) 0.0018(6) 0.0050(6) C22 0.0333(10) 0.0344(11) 0.0405(12) 0.0025(9) 0.0024(9) 0.0041(9) C23 0.0470(13) 0.0410(13) 0.0466(14) 0.0122(10) 0.0060(11) 0.0117(11) C24 0.0424(13) 0.0585(16) 0.0404(13) 0.0105(11) 0.0005(10) 0.0192(12) C25 0.0283(10) 0.0554(15) 0.0383(12) 0.0000(10) -0.0049(9) 0.0099(10) C26 0.0229(9) 0.0382(11) 0.0304(10) -0.0036(8) 0.0017(7) 0.0072(8) C27 0.0207(8) 0.0406(11) 0.0336(10) -0.0048(8) 0.0018(7) 0.0017(8) C28 0.0247(9) 0.0309(10) 0.0277(9) -0.0021(7) 0.0054(7) -0.0060(7) C29 0.0301(11) 0.0486(14) 0.0559(15) 0.0011(11) 0.0153(10) -0.0121(10) C30 0.0486(16) 0.0456(16) 0.101(3) 0.0143(16) 0.0145(16) -0.0165(13) C31 0.0410(11) 0.0272(10) 0.0391(11) 0.0053(8) 0.0050(9) -0.0058(9) C32 0.090(2) 0.0411(14) 0.0452(15) 0.0130(12) -0.0071(15) -0.0059(15) C33 0.096(2) 0.0279(12) 0.0529(16) -0.0012(11) 0.0131(16) 0.0016(14) N1 0.0202(7) 0.0294(8) 0.0320(8) -0.0003(6) 0.0043(6) 0.0015(6) N2 0.0231(7) 0.0274(8) 0.0257(8) -0.0013(6) -0.0024(6) 0.0013(6) N23 0.0262(7) 0.0245(8) 0.0249(8) -0.0001(6) 0.0037(6) -0.0041(6) N22 0.0193(7) 0.0310(8) 0.0313(8) -0.0033(6) 0.0015(6) -0.0007(6) N3 0.0296(8) 0.0279(8) 0.0206(7) -0.0023(6) -0.0005(6) -0.0017(6) O6 0.0292(7) 0.0407(9) 0.0437(9) -0.0040(7) -0.0114(6) -0.0016(6) O27 0.0304(8) 0.0569(11) 0.0647(12) 0.0011(9) -0.0152(8) -0.0104(8) Cl1 0.0269(2) 0.0542(3) 0.0255(2) -0.0016(2) -0.00370(17) -0.0001(2) Cl2 0.0332(3) 0.0335(3) 0.0590(4) 0.0069(2) -0.0116(2) -0.0094(2) Pd1 0.01745(6) 0.02546(7) 0.02153(7) -0.00024(5) 0.00101(5) 0.00059(5) Pd2 0.01980(7) 0.02510(7) 0.02519(7) -0.00104(5) -0.00059(5) 0.00017(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 N1 1.332(3) . ? C1 C2 1.382(3) . ? C1 H1 0.9500 . ? C2 C3 1.379(4) . ? C2 H2 0.9500 . ? C3 C4 1.374(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 N1 1.349(3) . ? C5 C6 1.493(3) . ? C6 O6 1.221(2) . ? C6 N2 1.365(3) . ? C7 N3 1.279(3) . ? C7 N2 1.371(3) . ? C7 C8 1.499(3) . ? C8 C9 1.514(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.542(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N3 1.499(3) . ? C10 C12 1.516(4) . ? C10 C11 1.532(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N21 C22 1.337(3) . ? N21 C26 1.346(3) . ? N21 Pd2 2.0225(17) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.372(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.374(3) . ? C25 H25 0.9500 . ? C26 C27 1.503(3) . ? C27 O27 1.222(3) . ? C27 N22 1.353(3) . ? C28 N23 1.274(3) . ? C28 N22 1.385(3) . ? C28 C29 1.505(3) . ? C29 C30 1.521(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.523(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N23 1.502(3) . ? C31 C32 1.510(4) . ? C31 C33 1.517(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Pd1 2.0196(17) . ? N2 Pd1 2.0103(17) . ? N23 Pd1 2.0292(17) . ? N22 Pd2 2.0152(17) . ? N3 Pd2 2.0219(17) . ? Cl1 Pd1 2.2967(9) . ? Cl2 Pd2 2.2931(8) . ? Pd1 Pd2 3.2084(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.9(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.2(2) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.4(2) . . ? N1 C5 C6 116.48(17) . . ? C4 C5 C6 122.02(19) . . ? O6 C6 N2 127.0(2) . . ? O6 C6 C5 121.05(19) . . ? N2 C6 C5 111.74(16) . . ? N3 C7 N2 120.98(17) . . ? N3 C7 C8 113.74(18) . . ? N2 C7 C8 125.28(19) . . ? C7 C8 C9 101.94(19) . . ? C7 C8 H8A 111.4 . . ? C9 C8 H8A 111.4 . . ? C7 C8 H8B 111.4 . . ? C9 C8 H8B 111.4 . . ? H8A C8 H8B 109.2 . . ? C8 C9 C10 105.65(19) . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? N3 C10 C12 109.67(19) . . ? N3 C10 C11 109.1(2) . . ? C12 C10 C11 111.4(2) . . ? N3 C10 C9 102.51(18) . . ? C12 C10 C9 112.3(2) . . ? C11 C10 C9 111.4(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C22 N21 C26 119.23(18) . . ? C22 N21 Pd2 126.68(15) . . ? C26 N21 Pd2 113.98(14) . . ? N21 C22 C23 121.2(2) . . ? N21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 119.6(2) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.2(2) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 118.6(2) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? N21 C26 C25 122.2(2) . . ? N21 C26 C27 116.61(17) . . ? C25 C26 C27 121.2(2) . . ? O27 C27 N22 127.2(2) . . ? O27 C27 C26 120.6(2) . . ? N22 C27 C26 112.04(17) . . ? N23 C28 N22 120.57(17) . . ? N23 C28 C29 114.01(19) . . ? N22 C28 C29 125.41(19) . . ? C28 C29 C30 101.30(19) . . ? C28 C29 H29A 111.5 . . ? C30 C29 H29A 111.5 . . ? C28 C29 H29B 111.5 . . ? C30 C29 H29B 111.5 . . ? H29A C29 H29B 109.3 . . ? C29 C30 C31 106.2(2) . . ? C29 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? C29 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? N23 C31 C32 108.49(19) . . ? N23 C31 C33 110.62(19) . . ? C32 C31 C33 109.4(2) . . ? N23 C31 C30 102.52(19) . . ? C32 C31 C30 114.1(2) . . ? C33 C31 C30 111.5(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C1 N1 C5 119.21(18) . . ? C1 N1 Pd1 126.83(15) . . ? C5 N1 Pd1 113.69(14) . . ? C6 N2 C7 120.13(16) . . ? C6 N2 Pd1 116.10(13) . . ? C7 N2 Pd1 123.53(13) . . ? C28 N23 C31 111.32(17) . . ? C28 N23 Pd1 126.02(14) . . ? C31 N23 Pd1 121.63(13) . . ? C27 N22 C28 118.50(17) . . ? C27 N22 Pd2 116.60(14) . . ? C28 N22 Pd2 122.98(13) . . ? C7 N3 C10 111.60(17) . . ? C7 N3 Pd2 124.70(14) . . ? C10 N3 Pd2 121.28(14) . . ? N2 Pd1 N1 80.37(7) . . ? N2 Pd1 N23 98.03(7) . . ? N1 Pd1 N23 169.88(7) . . ? N2 Pd1 Cl1 173.13(5) . . ? N1 Pd1 Cl1 94.63(6) . . ? N23 Pd1 Cl1 87.71(5) . . ? N2 Pd1 Pd2 71.73(5) . . ? N1 Pd1 Pd2 114.11(5) . . ? N23 Pd1 Pd2 74.44(5) . . ? Cl1 Pd1 Pd2 106.47(2) . . ? N22 Pd2 N3 97.24(7) . . ? N22 Pd2 N21 80.72(7) . . ? N3 Pd2 N21 170.68(7) . . ? N22 Pd2 Cl2 171.64(5) . . ? N3 Pd2 Cl2 88.07(5) . . ? N21 Pd2 Cl2 95.05(6) . . ? N22 Pd2 Pd1 72.16(5) . . ? N3 Pd2 Pd1 74.27(5) . . ? N21 Pd2 Pd1 113.37(5) . . ? Cl2 Pd2 Pd1 103.32(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.702 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.111 #===END data_max930acet=compound5a _database_code_depnum_ccdc_archive 'CCDC 710111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 N10 Pd' _chemical_formula_sum 'C24 H20 N10 Pd' _chemical_formula_weight 554.90 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.1888(7) _cell_length_b 15.910(2) _cell_length_c 11.4138(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.660(8) _cell_angle_gamma 90.00 _cell_volume 1096.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4278 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.22 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9068 _exptl_absorpt_correction_T_max 0.9755 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 10220 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2709 _reflns_number_gt 2159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'WinGX v.1.70.01 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0290P)^2^+0.3130P] 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 2709 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 H2 H 0.108(4) 0.4209(16) -0.172(2) 0.025(6) Uiso 1 1 d . . . H1 H 0.245(5) 0.4824(15) 0.209(2) 0.030(7) Uiso 1 1 d . . . C10 C 0.4198(3) 0.42602(13) 0.13603(17) 0.0179(4) Uani 1 1 d . . . C11 C 0.5863(3) 0.41588(13) 0.25240(17) 0.0192(4) Uani 1 1 d . . . C12 C 0.8034(3) 0.39290(14) 0.25472(19) 0.0234(4) Uani 1 1 d . . . H12 H 0.8496 0.3814 0.1823 0.028 Uiso 1 1 calc R . . C13 C 0.9511(4) 0.38710(15) 0.36419(19) 0.0271(5) Uani 1 1 d . . . H13 H 1.1016 0.3729 0.3682 0.032 Uiso 1 1 calc R . . C14 C 0.8768(4) 0.40228(15) 0.46815(19) 0.0288(5) Uani 1 1 d . . . H14 H 0.9737 0.3974 0.5449 0.035 Uiso 1 1 calc R . . C15 C 0.6576(4) 0.42473(16) 0.45718(19) 0.0305(5) Uani 1 1 d . . . H15 H 0.6067 0.4349 0.5286 0.037 Uiso 1 1 calc R . . C20 C 0.3463(3) 0.39359(13) -0.06893(17) 0.0190(4) Uani 1 1 d . . . C21 C 0.4366(3) 0.34932(13) -0.16510(18) 0.0202(4) Uani 1 1 d . . . C22 C 0.6565(3) 0.32391(13) -0.14452(19) 0.0231(4) Uani 1 1 d . . . H22 H 0.7534 0.3330 -0.0687 0.028 Uiso 1 1 calc R . . C23 C 0.7321(4) 0.28494(15) -0.2368(2) 0.0279(5) Uani 1 1 d . . . H23 H 0.8824 0.2680 -0.2260 0.033 Uiso 1 1 calc R . . C24 C 0.5838(4) 0.27128(15) -0.3449(2) 0.0310(5) Uani 1 1 d . . . H24 H 0.6292 0.2437 -0.4093 0.037 Uiso 1 1 calc R . . C25 C 0.3684(4) 0.29872(16) -0.3569(2) 0.0325(5) Uani 1 1 d . . . H25 H 0.2674 0.2891 -0.4312 0.039 Uiso 1 1 calc R . . N1 N 0.2399(3) 0.46810(12) 0.13807(16) 0.0202(3) Uani 1 1 d . . . N2 N 0.1539(3) 0.43036(12) -0.10105(15) 0.0208(4) Uani 1 1 d . . . N3 N 0.4793(3) 0.39000(11) 0.04107(15) 0.0197(4) Uani 1 1 d . . . N10 N 0.5134(3) 0.43293(13) 0.35252(15) 0.0260(4) Uani 1 1 d . . . N20 N 0.2933(3) 0.33796(12) -0.27026(16) 0.0266(4) Uani 1 1 d . . . Pd1 Pd 0.0000 0.5000 0.0000 0.01700(7) Uani 1 2 d S . . 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 C10 0.0162(9) 0.0182(10) 0.0182(9) 0.0011(7) 0.0014(7) -0.0011(8) C11 0.0176(10) 0.0195(10) 0.0194(9) 0.0016(8) 0.0014(8) 0.0013(8) C12 0.0199(10) 0.0285(12) 0.0219(10) 0.0014(8) 0.0051(8) 0.0031(9) C13 0.0171(10) 0.0320(12) 0.0298(11) 0.0009(9) 0.0001(9) 0.0040(9) C14 0.0286(12) 0.0321(13) 0.0210(10) -0.0005(9) -0.0049(9) 0.0083(10) C15 0.0298(12) 0.0415(14) 0.0194(10) -0.0011(9) 0.0034(9) 0.0112(10) C20 0.0184(10) 0.0179(10) 0.0203(10) -0.0007(7) 0.0036(8) -0.0011(8) C21 0.0219(10) 0.0191(10) 0.0199(10) 0.0005(8) 0.0053(8) 0.0002(8) C22 0.0213(10) 0.0218(11) 0.0260(10) -0.0003(8) 0.0045(8) -0.0001(9) C23 0.0231(11) 0.0265(12) 0.0361(12) -0.0004(9) 0.0107(9) 0.0043(9) C24 0.0381(13) 0.0305(13) 0.0280(12) -0.0006(9) 0.0150(10) 0.0088(11) C25 0.0367(13) 0.0376(14) 0.0213(11) -0.0044(9) 0.0024(10) 0.0085(11) N1 0.0184(8) 0.0251(9) 0.0165(8) -0.0006(7) 0.0026(7) 0.0024(7) N2 0.0192(9) 0.0264(10) 0.0155(8) -0.0025(7) 0.0013(7) 0.0027(7) N3 0.0176(9) 0.0229(9) 0.0176(8) -0.0012(7) 0.0017(6) 0.0021(7) N10 0.0212(9) 0.0363(11) 0.0190(8) -0.0001(7) 0.0011(7) 0.0085(8) N20 0.0257(10) 0.0308(11) 0.0215(9) -0.0037(7) 0.0014(7) 0.0085(8) Pd1 0.01416(11) 0.01993(11) 0.01598(10) -0.00079(9) 0.00126(7) 0.00237(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 N1 1.304(3) . ? C10 N3 1.347(2) . ? C10 C11 1.500(3) . ? C11 N10 1.345(2) . ? C11 C12 1.387(3) . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 N10 1.332(3) . ? C15 H15 0.9500 . ? C20 N2 1.305(3) . ? C20 N3 1.343(3) . ? C20 C21 1.511(3) . ? C21 N20 1.339(3) . ? C21 C22 1.389(3) . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.381(3) . ? C24 H24 0.9500 . ? C25 N20 1.336(3) . ? C25 H25 0.9500 . ? N1 Pd1 1.9799(18) . ? N1 H1 0.84(3) . ? N2 Pd1 1.9864(17) . ? N2 H2 0.81(2) . ? Pd1 N1 1.9799(18) 3_565 ? Pd1 N2 1.9864(17) 3_565 ? 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 C10 N3 128.17(19) . . ? N1 C10 C11 117.56(17) . . ? N3 C10 C11 114.27(17) . . ? N10 C11 C12 122.74(19) . . ? N10 C11 C10 115.94(17) . . ? C12 C11 C10 121.29(17) . . ? C13 C12 C11 118.77(19) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 119.07(19) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 118.1(2) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N10 C15 C14 123.9(2) . . ? N10 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? N2 C20 N3 128.04(19) . . ? N2 C20 C21 117.72(18) . . ? N3 C20 C21 114.24(17) . . ? N20 C21 C22 122.96(19) . . ? N20 C21 C20 115.86(18) . . ? C22 C21 C20 121.17(19) . . ? C23 C22 C21 118.8(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 118.6(2) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 118.4(2) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? N20 C25 C24 124.0(2) . . ? N20 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? C10 N1 Pd1 127.72(14) . . ? C10 N1 H1 107.7(19) . . ? Pd1 N1 H1 124.5(18) . . ? C20 N2 Pd1 127.66(15) . . ? C20 N2 H2 107.3(17) . . ? Pd1 N2 H2 125.1(17) . . ? C20 N3 C10 120.96(17) . . ? C15 N10 C11 117.31(18) . . ? C25 N20 C21 117.18(19) . . ? N1 Pd1 N1 180.00(11) . 3_565 ? N1 Pd1 N2 87.01(7) . . ? N1 Pd1 N2 92.99(7) 3_565 . ? N1 Pd1 N2 92.99(7) . 3_565 ? N1 Pd1 N2 87.01(7) 3_565 3_565 ? N2 Pd1 N2 180.0 . 3_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.492 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.069 #===END data_max923=compound5b _database_code_depnum_ccdc_archive 'CCDC 710112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 N10 Pd, 2(H2 O)' _chemical_formula_sum 'C24 H24 N10 O2 Pd' _chemical_formula_weight 590.93 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.770(2) _cell_length_b 8.635(3) _cell_length_c 9.736(3) _cell_angle_alpha 73.758(15) _cell_angle_beta 72.058(14) _cell_angle_gamma 88.654(16) _cell_volume 595.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5022 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 29.55 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8862 _exptl_absorpt_correction_T_max 0.9522 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7835 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2429 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'WinGX v.1.70.01 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0191P)^2^+0.3863P] 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 2429 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C10 C 0.3088(3) 0.0201(2) 0.7774(2) 0.0164(4) Uani 1 1 d . . . C11 C 0.2892(3) 0.0923(2) 0.6255(2) 0.0169(4) Uani 1 1 d . . . C12 C 0.2327(3) -0.0040(3) 0.5524(2) 0.0210(4) Uani 1 1 d . . . H12 H 0.2049 -0.1168 0.5987 0.025 Uiso 1 1 calc R . . C13 C 0.2178(3) 0.0675(3) 0.4113(2) 0.0234(4) Uani 1 1 d . . . H13 H 0.1844 0.0041 0.3569 0.028 Uiso 1 1 calc R . . C14 C 0.2521(3) 0.2327(3) 0.3504(2) 0.0236(5) Uani 1 1 d . . . H14 H 0.2398 0.2809 0.2538 0.028 Uiso 1 1 calc R . . C15 C 0.3221(3) 0.2569(3) 0.5545(2) 0.0200(4) Uani 1 1 d . . . H15 H 0.3613 0.3225 0.6044 0.024 Uiso 1 1 calc R . . C20 C 0.1695(3) -0.1750(2) 1.0090(2) 0.0164(4) Uani 1 1 d . . . C21 C 0.0145(3) -0.3021(2) 1.0852(2) 0.0167(4) Uani 1 1 d . . . C22 C -0.1309(3) -0.2963(3) 1.0293(2) 0.0212(4) Uani 1 1 d . . . H22 H -0.1357 -0.2095 0.9456 0.025 Uiso 1 1 calc R . . C23 C -0.2685(3) -0.4182(3) 1.0969(2) 0.0248(5) Uani 1 1 d . . . H23 H -0.3691 -0.4157 1.0605 0.030 Uiso 1 1 calc R . . C24 C -0.2578(3) -0.5431(3) 1.2176(2) 0.0235(5) Uani 1 1 d . . . H24 H -0.3516 -0.6274 1.2618 0.028 Uiso 1 1 calc R . . C25 C 0.0107(3) -0.4317(3) 1.2090(2) 0.0215(4) Uani 1 1 d . . . H25 H 0.1082 -0.4362 1.2493 0.026 Uiso 1 1 calc R . . N1 N 0.4437(2) 0.0739(2) 0.80840(19) 0.0175(3) Uani 1 1 d . . . N2 N 0.7214(2) 0.1512(2) 0.91846(19) 0.0177(3) Uani 1 1 d . . . N3 N 0.1796(2) -0.0976(2) 0.86648(19) 0.0186(4) Uani 1 1 d . . . N10 N 0.3019(2) 0.3288(2) 0.4204(2) 0.0236(4) Uani 1 1 d . . . N20 N -0.1212(2) -0.5510(2) 1.2752(2) 0.0240(4) Uani 1 1 d . . . O1 O 0.7265(2) 0.3363(2) 0.60004(19) 0.0272(4) Uani 1 1 d . . . Pd1 Pd 0.5000 0.0000 1.0000 0.01435(8) Uani 1 2 d S . . H1 H 0.510(3) 0.139(3) 0.742(3) 0.017 Uiso 1 1 d . . . H1A H 0.786(3) 0.342(3) 0.521(3) 0.017 Uiso 1 1 d . . . H1B H 0.699(3) 0.420(3) 0.611(3) 0.017 Uiso 1 1 d . . . H2 H 0.750(3) 0.206(3) 0.831(3) 0.017 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 C10 0.0205(10) 0.0145(9) 0.0141(9) -0.0035(7) -0.0059(8) 0.0027(8) C11 0.0152(9) 0.0200(10) 0.0137(9) -0.0039(8) -0.0026(7) 0.0005(7) C12 0.0249(11) 0.0187(10) 0.0198(10) -0.0043(8) -0.0087(8) 0.0010(8) C13 0.0259(11) 0.0288(12) 0.0192(10) -0.0088(9) -0.0107(9) 0.0037(9) C14 0.0249(11) 0.0314(12) 0.0136(10) -0.0029(9) -0.0079(8) 0.0038(9) C15 0.0234(10) 0.0204(11) 0.0167(10) -0.0025(8) -0.0091(8) -0.0018(8) C20 0.0181(9) 0.0147(10) 0.0150(9) -0.0032(8) -0.0041(8) 0.0009(7) C21 0.0195(10) 0.0168(10) 0.0124(9) -0.0046(8) -0.0026(8) -0.0003(8) C22 0.0237(11) 0.0212(11) 0.0175(10) -0.0034(8) -0.0064(8) 0.0000(8) C23 0.0218(11) 0.0295(12) 0.0246(11) -0.0076(9) -0.0091(9) -0.0022(9) C24 0.0225(11) 0.0228(11) 0.0210(11) -0.0065(9) -0.0001(9) -0.0071(8) C25 0.0246(11) 0.0198(11) 0.0187(10) -0.0020(8) -0.0077(8) -0.0043(8) N1 0.0204(9) 0.0161(9) 0.0119(8) 0.0013(7) -0.0038(7) -0.0031(7) N2 0.0219(9) 0.0178(9) 0.0101(8) 0.0014(7) -0.0049(7) -0.0033(7) N3 0.0222(9) 0.0177(9) 0.0146(8) -0.0006(7) -0.0073(7) -0.0016(7) N10 0.0283(10) 0.0216(9) 0.0183(9) 0.0005(7) -0.0090(7) -0.0011(7) N20 0.0282(10) 0.0219(9) 0.0172(9) -0.0002(7) -0.0048(7) -0.0065(7) O1 0.0400(10) 0.0210(8) 0.0157(8) 0.0008(7) -0.0066(7) -0.0066(7) Pd1 0.01765(12) 0.01352(12) 0.01043(11) -0.00017(8) -0.00510(8) -0.00178(8) _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 C10 N1 1.305(3) . ? C10 N3 1.346(3) . ? C10 C11 1.490(3) . ? C11 C15 1.386(3) . ? C11 C12 1.389(3) . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 N10 1.340(3) . ? C14 H14 0.9500 . ? C15 N10 1.335(3) . ? C15 H15 0.9500 . ? C20 N2 1.311(3) 2_657 ? C20 N3 1.339(3) . ? C20 C21 1.503(3) . ? C21 C25 1.390(3) . ? C21 C22 1.391(3) . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 C24 1.378(3) . ? C23 H23 0.9500 . ? C24 N20 1.337(3) . ? C24 H24 0.9500 . ? C25 N20 1.341(3) . ? C25 H25 0.9500 . ? N1 Pd1 1.9755(18) . ? N1 H1 0.78(3) . ? N2 C20 1.311(3) 2_657 ? N2 Pd1 1.9947(18) . ? N2 H2 0.81(3) . ? O1 H1A 0.76(3) . ? O1 H1B 0.78(3) . ? Pd1 N1 1.9755(18) 2_657 ? Pd1 N2 1.9947(18) 2_657 ? 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 C10 N3 128.20(18) . . ? N1 C10 C11 118.72(18) . . ? N3 C10 C11 113.08(17) . . ? C15 C11 C12 118.12(19) . . ? C15 C11 C10 121.35(18) . . ? C12 C11 C10 120.52(18) . . ? C13 C12 C11 118.6(2) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 119.0(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? N10 C14 C13 123.5(2) . . ? N10 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? N10 C15 C11 123.95(19) . . ? N10 C15 H15 118.0 . . ? C11 C15 H15 118.0 . . ? N2 C20 N3 126.95(19) 2_657 . ? N2 C20 C21 120.21(18) 2_657 . ? N3 C20 C21 112.83(17) . . ? C25 C21 C22 116.95(19) . . ? C25 C21 C20 122.88(18) . . ? C22 C21 C20 120.13(18) . . ? C23 C22 C21 119.3(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 119.2(2) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? N20 C24 C23 122.9(2) . . ? N20 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N20 C25 C21 124.4(2) . . ? N20 C25 H25 117.8 . . ? C21 C25 H25 117.8 . . ? C10 N1 Pd1 126.83(15) . . ? C10 N1 H1 114.9(18) . . ? Pd1 N1 H1 118.2(18) . . ? C20 N2 Pd1 127.16(14) 2_657 . ? C20 N2 H2 114.2(17) 2_657 . ? Pd1 N2 H2 118.6(17) . . ? C20 N3 C10 122.63(17) . . ? C15 N10 C14 116.78(19) . . ? C24 N20 C25 117.24(19) . . ? H1A O1 H1B 113(3) . . ? N1 Pd1 N1 180.000(1) 2_657 . ? N1 Pd1 N2 88.10(8) 2_657 . ? N1 Pd1 N2 91.90(8) . . ? N1 Pd1 N2 91.90(8) 2_657 2_657 ? N1 Pd1 N2 88.10(8) . 2_657 ? N2 Pd1 N2 180.0 . 2_657 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.378 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.071 #===END data_max935mon=compound5d _database_code_depnum_ccdc_archive 'CCDC 710113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H14 Cl4 N10 Pd' _chemical_formula_sum 'C24 H14 Cl4 N10 Pd' _chemical_formula_weight 690.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.286(2) _cell_length_b 8.924(2) _cell_length_c 13.858(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.20(5) _cell_angle_gamma 90.00 _cell_volume 1325.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5188 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 26.64 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8944 _exptl_absorpt_correction_T_max 0.9552 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 are detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31010 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.31 _reflns_number_total 3273 _reflns_number_gt 2568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'WinGX v.1.70.01 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0357P)^2^+0.5656P] 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 3273 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 C10 C 0.3964(2) 0.2988(3) 0.42664(19) 0.0189(5) Uani 1 1 d . . . C11 C 0.3846(2) 0.4302(3) 0.3567(2) 0.0202(5) Uani 1 1 d . . . C12 C 0.3582(2) 0.5730(3) 0.3858(2) 0.0225(5) Uani 1 1 d . . . H12 H 0.3433 0.5876 0.4490 0.027 Uiso 1 1 calc R . . C13 C 0.3539(3) 0.6925(3) 0.3220(2) 0.0280(6) Uani 1 1 d . . . H13 H 0.3364 0.7889 0.3433 0.034 Uiso 1 1 calc R . . C14 C 0.3960(3) 0.5442(3) 0.2054(2) 0.0259(6) Uani 1 1 d . . . C15 C 0.4026(2) 0.4159(3) 0.2627(2) 0.0231(6) Uani 1 1 d . . . H15 H 0.4190 0.3210 0.2385 0.028 Uiso 1 1 calc R . . C20 C 0.3445(2) 0.2147(3) 0.56833(19) 0.0194(5) Uani 1 1 d . . . C21 C 0.2738(2) 0.2575(3) 0.6397(2) 0.0201(5) Uani 1 1 d . . . C22 C 0.3222(3) 0.2325(3) 0.7439(2) 0.0244(6) Uani 1 1 d . A . H22 H 0.4018 0.1875 0.7720 0.029 Uiso 1 1 calc R . . C23 C 0.2521(3) 0.2743(3) 0.8059(2) 0.0290(6) Uani 1 1 d . . . C24 C 0.0951(2) 0.3579(3) 0.6706(2) 0.0239(6) Uani 1 1 d . . . C25 C 0.1570(3) 0.3233(3) 0.6022(2) 0.0227(6) Uani 1 1 d . A . H25 H 0.1209 0.3437 0.5318 0.027 Uiso 1 1 calc R . . N1 N 0.4629(2) 0.1842(2) 0.41632(17) 0.0210(5) Uani 1 1 d . . . N2 N 0.5984(2) -0.0861(2) 0.41806(18) 0.0217(5) Uani 1 1 d . . . N3 N 0.3376(2) 0.3184(2) 0.49693(16) 0.0202(5) Uani 1 1 d . . . N10 N 0.3731(2) 0.6807(3) 0.23125(19) 0.0301(6) Uani 1 1 d . . . N20 N 0.1383(2) 0.3363(3) 0.76983(18) 0.0270(5) Uani 1 1 d . A . Cl10 Cl 0.42168(9) 0.52674(9) 0.08784(6) 0.0421(2) Uani 1 1 d . . . Cl20 Cl -0.05206(7) 0.43756(9) 0.62803(6) 0.0316(2) Uani 0.905(2) 1 d P A 1 Pd1 Pd 0.5000 0.0000 0.5000 0.01741(9) Uani 1 2 d S . . Cl2B Cl 0.2881(9) 0.2417(11) 0.9166(7) 0.045(3) Uiso 0.095(2) 1 d P A 2 H1 H 0.493(3) 0.194(3) 0.370(2) 0.028(8) Uiso 1 1 d . . . H2 H 0.610(3) -0.041(3) 0.374(2) 0.022(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C10 0.0211(13) 0.0205(12) 0.0179(12) -0.0008(10) 0.0103(10) -0.0014(10) C11 0.0167(12) 0.0241(13) 0.0223(13) 0.0018(10) 0.0096(10) 0.0002(10) C12 0.0199(13) 0.0232(14) 0.0265(14) -0.0022(11) 0.0103(11) 0.0010(11) C13 0.0226(14) 0.0225(13) 0.0377(17) 0.0000(12) 0.0077(12) 0.0004(11) C14 0.0244(14) 0.0336(14) 0.0226(14) 0.0065(11) 0.0114(11) 0.0016(11) C15 0.0252(14) 0.0227(14) 0.0240(14) 0.0036(11) 0.0114(11) 0.0016(11) C20 0.0195(13) 0.0228(13) 0.0208(13) -0.0031(10) 0.0133(11) -0.0015(10) C21 0.0249(14) 0.0177(12) 0.0235(13) -0.0021(10) 0.0158(11) -0.0021(10) C22 0.0237(14) 0.0274(14) 0.0254(14) 0.0000(11) 0.0128(12) 0.0054(11) C23 0.0332(16) 0.0349(16) 0.0253(14) -0.0012(12) 0.0185(13) 0.0031(12) C24 0.0224(13) 0.0217(13) 0.0324(15) 0.0007(11) 0.0155(12) 0.0014(11) C25 0.0262(14) 0.0229(13) 0.0228(13) 0.0008(10) 0.0130(11) 0.0015(11) N1 0.0269(12) 0.0217(11) 0.0219(12) 0.0011(9) 0.0184(10) 0.0012(9) N2 0.0306(13) 0.0205(11) 0.0214(12) 0.0024(9) 0.0190(10) 0.0022(9) N3 0.0225(11) 0.0214(11) 0.0210(11) 0.0005(8) 0.0130(9) 0.0016(9) N10 0.0272(13) 0.0272(12) 0.0362(14) 0.0104(10) 0.0105(11) 0.0002(10) N20 0.0307(13) 0.0284(12) 0.0298(13) -0.0026(10) 0.0208(11) 0.0029(10) Cl10 0.0554(5) 0.0492(5) 0.0297(4) 0.0154(3) 0.0250(4) 0.0094(4) Cl20 0.0235(4) 0.0372(4) 0.0402(5) 0.0080(3) 0.0187(3) 0.0104(3) Pd1 0.02240(15) 0.01695(13) 0.01887(14) 0.00054(11) 0.01509(10) 0.00162(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 N1 1.303(3) . ? C10 N3 1.350(3) . ? C10 C11 1.500(3) . ? C11 C15 1.386(4) . ? C11 C12 1.397(4) . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 N10 1.346(4) . ? C13 H13 0.9500 . ? C14 N10 1.318(4) . ? C14 C15 1.382(4) . ? C14 Cl10 1.748(3) . ? C15 H15 0.9500 . ? C20 N2 1.301(3) 3_656 ? C20 N3 1.339(3) . ? C20 C21 1.500(3) . ? C21 C25 1.387(4) . ? C21 C22 1.393(4) . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 N20 1.343(4) . ? C23 Cl2B 1.488(10) . ? C24 N20 1.322(4) . ? C24 C25 1.376(4) . ? C24 Cl20 1.732(3) . ? C25 H25 0.9500 . ? N1 Pd1 1.980(2) . ? N1 H1 0.81(3) . ? N2 C20 1.301(3) 3_656 ? N2 Pd1 1.975(2) . ? N2 H2 0.77(3) . ? Pd1 N2 1.975(2) 3_656 ? Pd1 N1 1.980(2) 3_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 C10 N3 127.6(2) . . ? N1 C10 C11 118.7(2) . . ? N3 C10 C11 113.6(2) . . ? C15 C11 C12 117.5(2) . . ? C15 C11 C10 121.7(2) . . ? C12 C11 C10 120.7(2) . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N10 C13 C12 123.8(3) . . ? N10 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? N10 C14 C15 126.1(3) . . ? N10 C14 Cl10 116.1(2) . . ? C15 C14 Cl10 117.8(2) . . ? C14 C15 C11 117.8(2) . . ? C14 C15 H15 121.1 . . ? C11 C15 H15 121.1 . . ? N2 C20 N3 128.9(2) 3_656 . ? N2 C20 C21 118.1(2) 3_656 . ? N3 C20 C21 113.0(2) . . ? C25 C21 C22 118.3(2) . . ? C25 C21 C20 120.0(2) . . ? C22 C21 C20 121.7(2) . . ? C23 C22 C21 118.9(3) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? N20 C23 C22 123.0(3) . . ? N20 C23 Cl2B 112.7(4) . . ? C22 C23 Cl2B 124.1(4) . . ? N20 C24 C25 125.6(3) . . ? N20 C24 Cl20 114.7(2) . . ? C25 C24 Cl20 119.8(2) . . ? C24 C25 C21 117.7(3) . . ? C24 C25 H25 121.1 . . ? C21 C25 H25 121.1 . . ? C10 N1 Pd1 127.69(18) . . ? C10 N1 H1 113(2) . . ? Pd1 N1 H1 119(2) . . ? C20 N2 Pd1 127.02(18) 3_656 . ? C20 N2 H2 112(2) 3_656 . ? Pd1 N2 H2 121(2) . . ? C20 N3 C10 121.0(2) . . ? C14 N10 C13 115.4(2) . . ? C24 N20 C23 116.5(2) . . ? N2 Pd1 N2 180.0 . 3_656 ? N2 Pd1 N1 92.32(9) . . ? N2 Pd1 N1 87.68(9) 3_656 . ? N2 Pd1 N1 87.68(9) . 3_656 ? N2 Pd1 N1 92.32(9) 3_656 3_656 ? N1 Pd1 N1 180.0 . 3_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.592 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.089