Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Olivier Siri' _publ_contact_author_address ; CNRS UMR 6114 CNRS, case 901 Universite de la Mediterranee Faculte des Sciences de Luminy MARSEILLE 13288 FRANCE ; _publ_contact_author_email SIRI@LUMINY.UNIV-MRS.FR _publ_section_title ; Di- and tetranuclear palladium complexes with benzoquinonediimine ligands: synthesis, molecular structure and electrochemistry ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Dowty, E. (1994). ATOMS for Mac. Version 3.0. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, E-U. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. Spek, A.L., PLATON 98, Utrecht University, The Netherland, 1998. ; loop_ _publ_author_name 'Olivier Siri' 'P. Braunstein' 'Jean-Paul Collin' 'Jean-Philippe Taquet' 'Richard Welter' # Attachment '9.cif' data_welt2 _database_code_depnum_ccdc_archive 'CCDC 279434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H104 N8 O8 Pd4' _chemical_formula_sum 'C60 H104 N8 O8 Pd4' _chemical_formula_weight 1491.11 _chemical_absolute_configuration . 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' 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' H H 0.0000 0.0000 '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 12.0830(10) _cell_length_b 14.324(2) _cell_length_c 20.217(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.02(5) _cell_angle_gamma 90.00 _cell_volume 3379.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 102848 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26964 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.1291 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9856 _reflns_number_gt 6314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0220P)^2^+13.9747P] 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 9856 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1854 _refine_ls_R_factor_gt 0.1154 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.02097(5) 0.20403(4) 0.35160(3) 0.02705(16) Uani 1 1 d . . . Pd2 Pd 0.23229(5) -0.20072(4) 0.60203(3) 0.02694(15) Uani 1 1 d . . . O1 O -0.1427(5) 0.2173(4) 0.2601(3) 0.0402(14) Uani 1 1 d . . . O2 O -0.3045(5) 0.2114(4) 0.2946(3) 0.0424(15) Uani 1 1 d . . . O3 O 0.0406(5) -0.3450(4) 0.6360(3) 0.0403(14) Uani 1 1 d . . . O4 O 0.2038(5) -0.3417(4) 0.6037(3) 0.0392(14) Uani 1 1 d . . . N1 N 0.0064(5) 0.0679(4) 0.3456(3) 0.0240(13) Uani 1 1 d . . . N2 N 0.1037(5) 0.1872(4) 0.4360(3) 0.0255(13) Uani 1 1 d . . . N3 N 0.1678(5) -0.1848(4) 0.5026(3) 0.0233(13) Uani 1 1 d . . . N4 N 0.2612(5) -0.0657(4) 0.5937(3) 0.0252(13) Uani 1 1 d . . . C1 C 0.0838(6) -0.0654(5) 0.4175(3) 0.0248(15) Uani 1 1 d . . . H1 H 0.0518 -0.1096 0.3827 0.030 Uiso 1 1 calc . . . C2 C 0.0669(6) 0.0305(5) 0.4042(3) 0.0213(15) Uani 1 1 d . . . C3 C 0.1239(6) 0.0986(5) 0.4572(3) 0.0225(15) Uani 1 1 d . . . C4 C 0.1914(6) 0.0678(5) 0.5196(3) 0.0254(16) Uani 1 1 d . . . H4 H 0.2311 0.1120 0.5523 0.030 Uiso 1 1 calc . . . C5 C 0.2019(6) -0.0271(5) 0.5352(3) 0.0240(15) Uani 1 1 d . . . C6 C 0.1476(6) -0.0963(5) 0.4819(3) 0.0224(15) Uani 1 1 d . . . C7 C -0.0454(6) 0.0125(5) 0.2850(4) 0.0281(17) Uani 1 1 d . . . H7A H -0.1219 0.0387 0.2630 0.034 Uiso 1 1 calc . . . H7B H -0.0568 -0.0520 0.2997 0.034 Uiso 1 1 calc . . . C8 C 0.0259(7) 0.0084(6) 0.2312(4) 0.0359(19) Uani 1 1 d . . . C9 C 0.0300(10) 0.1031(8) 0.1983(5) 0.070(3) Uani 1 1 d . . . H9A H 0.0641 0.1489 0.2338 0.105 Uiso 1 1 calc . . . H9B H -0.0479 0.1227 0.1747 0.105 Uiso 1 1 calc . . . H9C H 0.0765 0.0989 0.1653 0.105 Uiso 1 1 calc . . . C10 C 0.1486(8) -0.0226(9) 0.2626(5) 0.068(3) Uani 1 1 d . . . H10A H 0.1483 -0.0829 0.2855 0.102 Uiso 1 1 calc . . . H10B H 0.1878 0.0239 0.2961 0.102 Uiso 1 1 calc . . . H10C H 0.1888 -0.0290 0.2265 0.102 Uiso 1 1 calc . . . C11 C -0.0316(9) -0.0587(9) 0.1749(6) 0.080(4) Uani 1 1 d . . . H11A H -0.0370 -0.1205 0.1947 0.119 Uiso 1 1 calc . . . H11B H 0.0137 -0.0631 0.1412 0.119 Uiso 1 1 calc . . . H11C H -0.1086 -0.0359 0.1524 0.119 Uiso 1 1 calc . . . C12 C 0.1620(7) 0.2660(5) 0.4756(4) 0.0300(17) Uani 1 1 d . . . H12A H 0.1875 0.2474 0.5244 0.036 Uiso 1 1 calc . . . H12B H 0.1067 0.3179 0.4721 0.036 Uiso 1 1 calc . . . C13 C 0.2669(7) 0.3018(5) 0.4527(4) 0.0364(18) Uani 1 1 d . . . C14 C 0.3155(9) 0.3854(7) 0.4972(6) 0.063(3) Uani 1 1 d . . . H14A H 0.2558 0.4330 0.4928 0.095 Uiso 1 1 calc . . . H14B H 0.3800 0.4114 0.4822 0.095 Uiso 1 1 calc . . . H14C H 0.3419 0.3656 0.5451 0.095 Uiso 1 1 calc . . . C15 C 0.2328(8) 0.3316(7) 0.3779(5) 0.056(3) Uani 1 1 d . . . H15A H 0.1725 0.3791 0.3711 0.084 Uiso 1 1 calc . . . H15B H 0.2043 0.2774 0.3489 0.084 Uiso 1 1 calc . . . H15C H 0.2997 0.3576 0.3654 0.084 Uiso 1 1 calc . . . C16 C 0.3597(8) 0.2266(7) 0.4633(6) 0.065(3) Uani 1 1 d . . . H16A H 0.3816 0.2077 0.5115 0.098 Uiso 1 1 calc . . . H16B H 0.4269 0.2516 0.4506 0.098 Uiso 1 1 calc . . . H16C H 0.3302 0.1724 0.4346 0.098 Uiso 1 1 calc . . . C17 C 0.1322(6) -0.2645(5) 0.4571(4) 0.0303(18) Uani 1 1 d . . . H17A H 0.0659 -0.2456 0.4194 0.036 Uiso 1 1 calc . . . H17B H 0.1063 -0.3150 0.4830 0.036 Uiso 1 1 calc . . . C18 C 0.2262(7) -0.3032(5) 0.4260(4) 0.0375(19) Uani 1 1 d . . . C19 C 0.3281(8) -0.3385(7) 0.4820(5) 0.056(3) Uani 1 1 d . . . H19A H 0.3016 -0.3845 0.5103 0.084 Uiso 1 1 calc . . . H19B H 0.3640 -0.2859 0.5106 0.084 Uiso 1 1 calc . . . H19C H 0.3840 -0.3676 0.4609 0.084 Uiso 1 1 calc . . . C20 C 0.1740(9) -0.3861(7) 0.3810(5) 0.061(3) Uani 1 1 d . . . H20A H 0.1465 -0.4324 0.4087 0.091 Uiso 1 1 calc . . . H20B H 0.2324 -0.4146 0.3616 0.091 Uiso 1 1 calc . . . H20C H 0.1099 -0.3645 0.3438 0.091 Uiso 1 1 calc . . . C21 C 0.2657(11) -0.2306(7) 0.3819(7) 0.083(4) Uani 1 1 d . . . H21A H 0.3242 -0.2580 0.3621 0.125 Uiso 1 1 calc . . . H21B H 0.2980 -0.1767 0.4102 0.125 Uiso 1 1 calc . . . H21C H 0.2002 -0.2104 0.3450 0.125 Uiso 1 1 calc . . . C22 C 0.3297(6) -0.0090(5) 0.6509(4) 0.0269(16) Uani 1 1 d . . . H22A H 0.3186 -0.0337 0.6945 0.032 Uiso 1 1 calc . . . H22B H 0.3006 0.0559 0.6457 0.032 Uiso 1 1 calc . . . C23 C 0.4597(7) -0.0079(6) 0.6553(4) 0.0327(18) Uani 1 1 d . . . C24 C 0.5136(9) 0.0612(8) 0.7113(6) 0.069(3) Uani 1 1 d . . . H24A H 0.4787 0.1228 0.6997 0.104 Uiso 1 1 calc . . . H24B H 0.5961 0.0652 0.7154 0.104 Uiso 1 1 calc . . . H24C H 0.5010 0.0401 0.7549 0.104 Uiso 1 1 calc . . . C25 C 0.4824(8) 0.0223(9) 0.5881(5) 0.069(3) Uani 1 1 d . . . H25A H 0.4473 0.0835 0.5749 0.104 Uiso 1 1 calc . . . H25B H 0.4493 -0.0235 0.5525 0.104 Uiso 1 1 calc . . . H25C H 0.5652 0.0265 0.5936 0.104 Uiso 1 1 calc . . . C26 C 0.5129(7) -0.1038(7) 0.6739(5) 0.054(3) Uani 1 1 d . . . H26A H 0.4780 -0.1485 0.6379 0.081 Uiso 1 1 calc . . . H26B H 0.4993 -0.1242 0.7174 0.081 Uiso 1 1 calc . . . H26C H 0.5955 -0.1004 0.6785 0.081 Uiso 1 1 calc . . . C27 C -0.2492(8) 0.2203(5) 0.2506(4) 0.0316(18) Uani 1 1 d . . . C28 C -0.3179(8) 0.2387(6) 0.1781(4) 0.045(2) Uani 1 1 d . . . H28A H -0.3953 0.2133 0.1716 0.068 Uiso 1 1 calc R . . H28B H -0.2806 0.2086 0.1461 0.068 Uiso 1 1 calc R . . H28C H -0.3225 0.3061 0.1697 0.068 Uiso 1 1 calc R . . C29 C 0.1228(7) -0.3825(5) 0.6198(4) 0.0303(16) Uani 1 1 d . . . C30 C 0.1238(9) -0.4875(5) 0.6186(5) 0.052(2) Uani 1 1 d . . . H30A H 0.1471 -0.5112 0.6656 0.078 Uiso 1 1 calc R . . H30B H 0.1780 -0.5091 0.5933 0.078 Uiso 1 1 calc R . . H30C H 0.0469 -0.5105 0.5961 0.078 Uiso 1 1 calc R . . 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 0.0288(3) 0.0268(3) 0.0259(3) 0.0096(3) 0.0077(2) 0.0069(3) Pd2 0.0250(3) 0.0262(3) 0.0281(3) 0.0105(3) 0.0043(2) 0.0020(3) O1 0.039(3) 0.057(4) 0.024(3) 0.015(3) 0.007(2) 0.019(3) O2 0.033(3) 0.058(4) 0.031(3) 0.019(3) -0.001(2) -0.001(3) O3 0.036(3) 0.026(3) 0.062(4) 0.017(3) 0.017(3) 0.010(3) O4 0.043(3) 0.024(3) 0.057(4) 0.017(3) 0.023(3) 0.006(3) N1 0.023(3) 0.028(3) 0.022(3) 0.002(3) 0.007(3) 0.004(3) N2 0.030(3) 0.022(3) 0.025(3) 0.003(2) 0.008(3) 0.002(3) N3 0.022(3) 0.018(3) 0.028(3) -0.001(2) 0.004(2) -0.001(2) N4 0.026(3) 0.026(3) 0.022(3) 0.004(3) 0.002(3) 0.002(3) C1 0.025(4) 0.023(4) 0.023(4) -0.004(3) 0.001(3) -0.005(3) C2 0.020(3) 0.021(3) 0.024(4) 0.005(3) 0.007(3) 0.003(3) C3 0.027(4) 0.021(4) 0.021(3) -0.001(3) 0.009(3) 0.000(3) C4 0.034(4) 0.025(4) 0.018(3) -0.001(3) 0.007(3) -0.003(3) C5 0.022(4) 0.026(4) 0.021(4) 0.002(3) 0.002(3) 0.001(3) C6 0.018(3) 0.021(4) 0.027(4) -0.004(3) 0.005(3) 0.000(3) C7 0.021(4) 0.031(4) 0.028(4) 0.003(3) -0.001(3) 0.001(3) C8 0.031(4) 0.053(5) 0.023(4) -0.008(4) 0.005(3) -0.002(4) C9 0.094(9) 0.076(8) 0.054(6) 0.014(6) 0.047(6) 0.004(7) C10 0.042(6) 0.131(10) 0.032(5) 0.010(6) 0.013(4) 0.033(6) C11 0.057(7) 0.120(11) 0.060(7) -0.055(7) 0.012(6) -0.020(7) C12 0.041(5) 0.028(4) 0.020(4) -0.005(3) 0.007(3) -0.001(3) C13 0.037(4) 0.027(4) 0.045(5) 0.001(4) 0.010(4) -0.004(4) C14 0.066(7) 0.039(5) 0.077(7) -0.005(5) 0.004(6) -0.012(5) C15 0.043(5) 0.072(7) 0.052(6) 0.019(5) 0.012(4) -0.021(5) C16 0.034(5) 0.052(6) 0.112(10) 0.002(6) 0.022(6) 0.003(5) C17 0.023(4) 0.023(4) 0.037(5) -0.011(3) -0.007(3) -0.001(3) C18 0.047(5) 0.025(4) 0.043(5) -0.002(4) 0.018(4) 0.004(4) C19 0.038(5) 0.060(6) 0.070(7) -0.020(5) 0.015(5) 0.009(5) C20 0.067(7) 0.051(6) 0.058(6) -0.021(5) 0.004(5) 0.018(5) C21 0.119(11) 0.044(6) 0.124(11) 0.023(6) 0.098(9) 0.022(7) C22 0.030(4) 0.027(4) 0.023(4) 0.001(3) 0.005(3) 0.000(3) C23 0.030(4) 0.042(5) 0.024(4) -0.003(3) 0.003(3) -0.003(4) C24 0.046(6) 0.080(8) 0.070(7) -0.044(6) -0.006(5) -0.017(6) C25 0.037(6) 0.125(10) 0.047(6) 0.026(6) 0.014(5) -0.010(6) C26 0.028(5) 0.065(7) 0.066(6) 0.004(5) 0.009(4) 0.007(5) C27 0.049(5) 0.012(4) 0.025(4) 0.004(3) -0.005(4) 0.000(3) C28 0.056(6) 0.043(5) 0.024(4) 0.011(4) -0.011(4) 0.004(4) C29 0.036(4) 0.022(4) 0.030(4) 0.008(3) 0.002(3) 0.006(4) C30 0.059(6) 0.022(4) 0.078(7) 0.004(5) 0.023(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.976(6) . ? Pd1 N1 1.987(6) . ? Pd1 O1 2.051(5) . ? Pd1 O3 2.055(5) 3_556 ? Pd1 Pd2 2.9397(11) 3_556 ? Pd2 N3 1.971(6) . ? Pd2 N4 1.980(6) . ? Pd2 O2 2.051(5) 3_556 ? Pd2 O4 2.050(5) . ? Pd2 Pd1 2.9396(11) 3_556 ? O1 C27 1.252(10) . ? O2 C27 1.250(10) . ? O2 Pd2 2.051(5) 3_556 ? O3 C29 1.246(9) . ? O3 Pd1 2.055(5) 3_556 ? O4 C29 1.253(9) . ? N1 C2 1.331(8) . ? N1 C7 1.458(9) . ? N2 C3 1.341(8) . ? N2 C12 1.457(9) . ? N3 C6 1.338(8) . ? N3 C17 1.460(9) . ? N4 C5 1.335(8) . ? N4 C22 1.478(9) . ? C1 C6 1.401(9) . ? C1 C2 1.405(9) . ? C1 H1 0.9500 . ? C2 C3 1.480(9) . ? C3 C4 1.386(9) . ? C4 C5 1.393(10) . ? C4 H4 0.9500 . ? C5 C6 1.485(9) . ? C7 C8 1.555(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.517(13) . ? C8 C11 1.514(12) . ? C8 C10 1.520(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.546(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.521(12) . ? C13 C15 1.522(12) . ? C13 C16 1.529(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.537(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C21 1.526(13) . ? C18 C19 1.526(12) . ? C18 C20 1.529(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.550(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C25 1.517(12) . ? C23 C24 1.517(11) . ? C23 C26 1.522(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.507(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.504(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 N1 80.2(2) . . ? N2 Pd1 O1 175.8(2) . . ? N1 Pd1 O1 97.4(2) . . ? N2 Pd1 O3 95.8(2) . 3_556 ? N1 Pd1 O3 176.0(2) . 3_556 ? O1 Pd1 O3 86.6(2) . 3_556 ? N2 Pd1 Pd2 104.68(17) . 3_556 ? N1 Pd1 Pd2 100.12(17) . 3_556 ? O1 Pd1 Pd2 79.05(16) . 3_556 ? O3 Pd1 Pd2 80.78(16) 3_556 3_556 ? N3 Pd2 N4 80.4(2) . . ? N3 Pd2 O2 177.1(2) . 3_556 ? N4 Pd2 O2 97.0(2) . 3_556 ? N3 Pd2 O4 96.1(2) . . ? N4 Pd2 O4 175.9(2) . . ? O2 Pd2 O4 86.5(2) 3_556 . ? N3 Pd2 Pd1 100.40(17) . 3_556 ? N4 Pd2 Pd1 103.29(18) . 3_556 ? O2 Pd2 Pd1 81.31(17) 3_556 3_556 ? O4 Pd2 Pd1 79.35(16) . 3_556 ? C27 O1 Pd1 127.7(5) . . ? C27 O2 Pd2 124.6(5) . 3_556 ? C29 O3 Pd1 125.5(5) . 3_556 ? C29 O4 Pd2 127.6(5) . . ? C2 N1 C7 123.0(6) . . ? C2 N1 Pd1 113.8(5) . . ? C7 N1 Pd1 122.9(4) . . ? C3 N2 C12 122.4(6) . . ? C3 N2 Pd1 115.2(5) . . ? C12 N2 Pd1 122.1(5) . . ? C6 N3 C17 122.9(6) . . ? C6 N3 Pd2 114.9(4) . . ? C17 N3 Pd2 121.8(5) . . ? C5 N4 C22 122.0(6) . . ? C5 N4 Pd2 114.4(5) . . ? C22 N4 Pd2 123.0(4) . . ? C6 C1 C2 120.3(6) . . ? C6 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? N1 C2 C1 125.7(6) . . ? N1 C2 C3 115.0(6) . . ? C1 C2 C3 119.2(6) . . ? N2 C3 C4 127.4(6) . . ? N2 C3 C2 112.4(6) . . ? C4 C3 C2 120.2(6) . . ? C3 C4 C5 120.9(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N4 C5 C4 126.9(6) . . ? N4 C5 C6 113.7(6) . . ? C4 C5 C6 119.3(6) . . ? N3 C6 C1 127.0(6) . . ? N3 C6 C5 113.2(6) . . ? C1 C6 C5 119.8(6) . . ? N1 C7 C8 114.4(6) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C11 107.4(8) . . ? C9 C8 C10 107.8(8) . . ? C11 C8 C10 109.6(8) . . ? C9 C8 C7 111.1(7) . . ? C11 C8 C7 108.7(7) . . ? C10 C8 C7 112.1(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 114.2(6) . . ? N2 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? N2 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C15 109.3(8) . . ? C14 C13 C16 108.4(8) . . ? C15 C13 C16 109.7(8) . . ? C14 C13 C12 107.7(7) . . ? C15 C13 C12 111.1(7) . . ? C16 C13 C12 110.7(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 114.3(6) . . ? N3 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? N3 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C21 C18 C19 110.2(9) . . ? C21 C18 C20 108.9(9) . . ? C19 C18 C20 108.3(7) . . ? C21 C18 C17 111.7(7) . . ? C19 C18 C17 110.9(7) . . ? C20 C18 C17 106.9(7) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C23 113.8(6) . . ? N4 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N4 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C25 C23 C24 109.9(8) . . ? C25 C23 C26 108.4(8) . . ? C24 C23 C26 109.3(7) . . ? C25 C23 C22 111.6(7) . . ? C24 C23 C22 106.4(7) . . ? C26 C23 C22 111.2(7) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 O1 127.2(7) . . ? O2 C27 C28 116.6(8) . . ? O1 C27 C28 116.3(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 O4 126.6(7) . . ? O3 C29 C30 116.5(8) . . ? O4 C29 C30 116.9(8) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 O1 C27 154(3) . . . . ? N1 Pd1 O1 C27 99.3(6) . . . . ? O3 Pd1 O1 C27 -81.0(6) 3_556 . . . ? Pd2 Pd1 O1 C27 0.3(6) 3_556 . . . ? N3 Pd2 O4 C29 -99.1(7) . . . . ? N4 Pd2 O4 C29 -130(3) . . . . ? O2 Pd2 O4 C29 82.2(7) 3_556 . . . ? Pd1 Pd2 O4 C29 0.4(6) 3_556 . . . ? N2 Pd1 N1 C2 15.8(5) . . . . ? O1 Pd1 N1 C2 -167.7(5) . . . . ? O3 Pd1 N1 C2 15(4) 3_556 . . . ? Pd2 Pd1 N1 C2 -87.5(5) 3_556 . . . ? N2 Pd1 N1 C7 -170.5(6) . . . . ? O1 Pd1 N1 C7 6.0(6) . . . . ? O3 Pd1 N1 C7 -171(3) 3_556 . . . ? Pd2 Pd1 N1 C7 86.1(5) 3_556 . . . ? N1 Pd1 N2 C3 -16.2(5) . . . . ? O1 Pd1 N2 C3 -72(3) . . . . ? O3 Pd1 N2 C3 163.8(5) 3_556 . . . ? Pd2 Pd1 N2 C3 81.9(5) 3_556 . . . ? N1 Pd1 N2 C12 169.3(6) . . . . ? O1 Pd1 N2 C12 114(3) . . . . ? O3 Pd1 N2 C12 -10.8(6) 3_556 . . . ? Pd2 Pd1 N2 C12 -92.7(5) 3_556 . . . ? N4 Pd2 N3 C6 -16.0(5) . . . . ? O2 Pd2 N3 C6 -40(5) 3_556 . . . ? O4 Pd2 N3 C6 166.2(5) . . . . ? Pd1 Pd2 N3 C6 85.9(5) 3_556 . . . ? N4 Pd2 N3 C17 171.2(6) . . . . ? O2 Pd2 N3 C17 147(5) 3_556 . . . ? O4 Pd2 N3 C17 -6.6(6) . . . . ? Pd1 Pd2 N3 C17 -86.9(5) 3_556 . . . ? N3 Pd2 N4 C5 16.1(5) . . . . ? O2 Pd2 N4 C5 -165.1(5) 3_556 . . . ? O4 Pd2 N4 C5 47(3) . . . . ? Pd1 Pd2 N4 C5 -82.4(5) 3_556 . . . ? N3 Pd2 N4 C22 -172.2(6) . . . . ? O2 Pd2 N4 C22 6.6(6) 3_556 . . . ? O4 Pd2 N4 C22 -141(3) . . . . ? Pd1 Pd2 N4 C22 89.3(5) 3_556 . . . ? C7 N1 C2 C1 -4.0(11) . . . . ? Pd1 N1 C2 C1 169.7(6) . . . . ? C7 N1 C2 C3 173.2(6) . . . . ? Pd1 N1 C2 C3 -13.1(7) . . . . ? C6 C1 C2 N1 -178.8(7) . . . . ? C6 C1 C2 C3 4.2(10) . . . . ? C12 N2 C3 C4 6.3(11) . . . . ? Pd1 N2 C3 C4 -168.3(6) . . . . ? C12 N2 C3 C2 -172.0(6) . . . . ? Pd1 N2 C3 C2 13.4(7) . . . . ? N1 C2 C3 N2 0.0(9) . . . . ? C1 C2 C3 N2 177.3(6) . . . . ? N1 C2 C3 C4 -178.5(6) . . . . ? C1 C2 C3 C4 -1.1(10) . . . . ? N2 C3 C4 C5 178.2(7) . . . . ? C2 C3 C4 C5 -3.6(11) . . . . ? C22 N4 C5 C4 -2.4(11) . . . . ? Pd2 N4 C5 C4 169.4(6) . . . . ? C22 N4 C5 C6 174.7(6) . . . . ? Pd2 N4 C5 C6 -13.5(8) . . . . ? C3 C4 C5 N4 -178.0(7) . . . . ? C3 C4 C5 C6 5.1(11) . . . . ? C17 N3 C6 C1 5.3(11) . . . . ? Pd2 N3 C6 C1 -167.4(6) . . . . ? C17 N3 C6 C5 -174.2(6) . . . . ? Pd2 N3 C6 C5 13.1(7) . . . . ? C2 C1 C6 N3 177.8(7) . . . . ? C2 C1 C6 C5 -2.7(10) . . . . ? N4 C5 C6 N3 0.3(9) . . . . ? C4 C5 C6 N3 177.6(6) . . . . ? N4 C5 C6 C1 -179.3(6) . . . . ? C4 C5 C6 C1 -1.9(10) . . . . ? C2 N1 C7 C8 -98.0(8) . . . . ? Pd1 N1 C7 C8 88.9(7) . . . . ? N1 C7 C8 C9 -67.6(9) . . . . ? N1 C7 C8 C11 174.4(8) . . . . ? N1 C7 C8 C10 53.1(10) . . . . ? C3 N2 C12 C13 97.1(8) . . . . ? Pd1 N2 C12 C13 -88.8(7) . . . . ? N2 C12 C13 C14 178.2(7) . . . . ? N2 C12 C13 C15 58.6(9) . . . . ? N2 C12 C13 C16 -63.5(9) . . . . ? C6 N3 C17 C18 96.4(8) . . . . ? Pd2 N3 C17 C18 -91.4(7) . . . . ? N3 C17 C18 C21 -61.7(10) . . . . ? N3 C17 C18 C19 61.6(9) . . . . ? N3 C17 C18 C20 179.4(7) . . . . ? C5 N4 C22 C23 -100.1(8) . . . . ? Pd2 N4 C22 C23 88.8(7) . . . . ? N4 C22 C23 C25 54.1(10) . . . . ? N4 C22 C23 C24 174.0(7) . . . . ? N4 C22 C23 C26 -67.0(8) . . . . ? Pd2 O2 C27 O1 5.8(11) 3_556 . . . ? Pd2 O2 C27 C28 -172.8(5) 3_556 . . . ? Pd1 O1 C27 O2 -3.6(12) . . . . ? Pd1 O1 C27 C28 175.0(5) . . . . ? Pd1 O3 C29 O4 -5.2(12) 3_556 . . . ? Pd1 O3 C29 C30 175.7(6) 3_556 . . . ? Pd2 O4 C29 O3 2.6(12) . . . . ? Pd2 O4 C29 C30 -178.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.542 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.241 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 619233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H58 N4 O5 Pd2' _chemical_formula_sum 'C36 H58 N4 O5 Pd2' _chemical_formula_weight 839.66 _chemical_absolute_configuration . 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' O O 0.0106 0.0060 '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 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 9.6830(3) _cell_length_b 10.4650(3) _cell_length_c 11.2100(4) _cell_angle_alpha 62.5600(15) _cell_angle_beta 88.2790(18) _cell_angle_gamma 77.124(2) _cell_volume 979.32(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4855 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4855 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3840 _reflns_number_gt 3357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0283P)^2^+0.5722P] 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 3840 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.14910(2) 0.67287(2) 0.41777(2) 0.02259(10) Uani 1 1 d . . . O1 O 0.1291(2) 0.6575(2) 0.2480(2) 0.0303(5) Uani 1 1 d . . . O2 O 0.1974(2) 0.4521(2) 0.5327(2) 0.0278(5) Uani 1 1 d . . . O3 O -0.0077(9) 1.0662(9) 0.1166(9) 0.039(2) Uiso 0.28 1 d P . . O4 O 0.1421(11) 0.5785(12) 0.7995(11) 0.037(3) Uiso 0.22 1 d P . . N1 N 0.0970(3) 0.8931(3) 0.3220(2) 0.0223(5) Uani 1 1 d . . . N2 N 0.1489(3) 0.7145(3) 0.5737(2) 0.0225(5) Uani 1 1 d . . . C1 C -0.0283(3) 1.1005(3) 0.3585(3) 0.0237(7) Uani 1 1 d . . . H1 H -0.0471 1.1671 0.2648 0.028 Uiso 1 1 calc . . . C2 C 0.0440(3) 0.9544(3) 0.4004(3) 0.0212(6) Uani 1 1 d . . . C3 C 0.0740(3) 0.8491(3) 0.5474(3) 0.0223(6) Uani 1 1 d . . . C4 C 0.0971(3) 0.9793(3) 0.1780(3) 0.0284(7) Uani 1 1 d . . . H4A H 0.0271 1.0752 0.1484 0.034 Uiso 0.84 1 calc P . . H4B H 0.0648 0.9266 0.1342 0.034 Uiso 0.84 1 calc P . . C5 C 0.2401(4) 1.0105(4) 0.1280(3) 0.0319(8) Uani 1 1 d . . . C6 C 0.2760(5) 1.1185(5) 0.1722(5) 0.0610(12) Uani 1 1 d . . . H6A H 0.2015 1.2105 0.1340 0.091 Uiso 1 1 calc . . . H6B H 0.3674 1.1402 0.1401 0.091 Uiso 1 1 calc . . . H6C H 0.2820 1.0738 0.2709 0.091 Uiso 1 1 calc . . . C7 C 0.2249(5) 1.0842(6) -0.0252(4) 0.0636(13) Uani 1 1 d . . . H7A H 0.2083 1.0138 -0.0548 0.095 Uiso 1 1 calc . . . H7B H 0.3122 1.1154 -0.0602 0.095 Uiso 1 1 calc . . . H7C H 0.1444 1.1709 -0.0594 0.095 Uiso 1 1 calc . . . C8 C 0.3599(4) 0.8705(5) 0.1851(5) 0.0528(11) Uani 1 1 d . . . H8A H 0.3667 0.8243 0.2838 0.079 Uiso 1 1 calc . . . H8B H 0.4499 0.8962 0.1525 0.079 Uiso 1 1 calc . . . H8C H 0.3400 0.8011 0.1556 0.079 Uiso 1 1 calc . . . C9 C 0.2063(3) 0.6022(3) 0.7089(3) 0.0270(7) Uani 1 1 d . . . H9A H 0.1891 0.5064 0.7237 0.032 Uiso 0.66 1 calc P . . H9B H 0.1544 0.6289 0.7747 0.032 Uiso 0.66 1 calc P . . C10 C 0.3661(3) 0.5821(3) 0.7368(3) 0.0296(7) Uani 1 1 d . . . C11 C 0.3931(4) 0.7213(4) 0.7357(5) 0.0539(11) Uani 1 1 d . . . H11A H 0.4952 0.7080 0.7530 0.081 Uiso 1 1 calc . . . H11B H 0.3421 0.7380 0.8060 0.081 Uiso 1 1 calc . . . H11C H 0.3593 0.8068 0.6474 0.081 Uiso 1 1 calc . . . C12 C 0.4522(3) 0.5508(4) 0.6327(3) 0.0370(8) Uani 1 1 d . . . H12A H 0.4334 0.4627 0.6323 0.055 Uiso 1 1 calc . . . H12B H 0.5538 0.5335 0.6559 0.055 Uiso 1 1 calc . . . H12C H 0.4247 0.6360 0.5430 0.055 Uiso 1 1 calc . . . C13 C 0.4125(4) 0.4488(4) 0.8764(4) 0.0450(9) Uani 1 1 d . . . H13A H 0.3947 0.3602 0.8765 0.067 Uiso 1 1 calc . . . H13B H 0.3582 0.4677 0.9442 0.067 Uiso 1 1 calc . . . H13C H 0.5141 0.4334 0.8979 0.067 Uiso 1 1 calc . . . C14 C 0.1400(3) 0.5355(4) 0.2437(3) 0.0280(7) Uani 1 1 d . . . C15 C 0.1158(4) 0.5542(4) 0.1040(4) 0.0418(9) Uani 1 1 d . . . H15A H 0.0145 0.5955 0.0735 0.063 Uiso 1 1 calc . . . H15B H 0.1459 0.4576 0.1054 0.063 Uiso 1 1 calc . . . H15C H 0.1711 0.6216 0.0422 0.063 Uiso 1 1 calc . . . C16 C 0.1742(3) 0.3948(3) 0.3532(3) 0.0294(7) Uani 1 1 d . . . H16 H 0.1786 0.3141 0.3348 0.035 Uiso 1 1 calc . . . C17 C 0.2027(3) 0.3596(3) 0.4870(3) 0.0272(7) Uani 1 1 d . . . C18 C 0.2485(4) 0.1999(4) 0.5922(4) 0.0388(8) Uani 1 1 d . . . H18A H 0.3510 0.1746 0.6161 0.058 Uiso 1 1 calc . . . H18B H 0.2269 0.1364 0.5564 0.058 Uiso 1 1 calc . . . H18C H 0.1975 0.1848 0.6728 0.058 Uiso 1 1 calc . . . 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 0.02405(16) 0.02038(13) 0.02517(15) -0.01275(10) 0.00555(11) -0.00428(10) O1 0.0386(13) 0.0268(11) 0.0286(12) -0.0166(10) 0.0043(11) -0.0051(10) O2 0.0304(12) 0.0222(11) 0.0310(12) -0.0125(9) 0.0025(10) -0.0062(9) N1 0.0231(13) 0.0191(12) 0.0229(13) -0.0092(10) 0.0062(11) -0.0034(10) N2 0.0231(14) 0.0219(13) 0.0234(13) -0.0124(11) 0.0049(11) -0.0031(10) C1 0.0264(16) 0.0202(15) 0.0216(15) -0.0088(12) 0.0035(14) -0.0026(12) C2 0.0170(14) 0.0241(15) 0.0248(15) -0.0123(13) 0.0056(13) -0.0072(12) C3 0.0185(15) 0.0231(15) 0.0273(16) -0.0134(13) 0.0032(13) -0.0054(12) C4 0.0286(18) 0.0256(16) 0.0276(17) -0.0124(14) 0.0041(15) -0.0002(14) C5 0.0351(19) 0.0349(18) 0.0280(17) -0.0147(15) 0.0121(16) -0.0136(15) C6 0.064(3) 0.059(3) 0.079(3) -0.038(3) 0.017(3) -0.037(2) C7 0.056(3) 0.091(4) 0.038(2) -0.023(2) 0.022(2) -0.024(3) C8 0.030(2) 0.049(2) 0.076(3) -0.028(2) 0.023(2) -0.0082(18) C9 0.0300(18) 0.0246(16) 0.0215(16) -0.0095(13) 0.0063(15) -0.0005(13) C10 0.0306(18) 0.0287(17) 0.0300(17) -0.0147(14) 0.0009(15) -0.0053(14) C11 0.052(2) 0.046(2) 0.076(3) -0.035(2) -0.007(2) -0.016(2) C12 0.0216(17) 0.051(2) 0.0352(19) -0.0189(17) 0.0017(15) -0.0046(15) C13 0.045(2) 0.045(2) 0.035(2) -0.0164(18) -0.0026(18) 0.0038(18) C14 0.0227(16) 0.0345(18) 0.0360(18) -0.0243(15) 0.0048(15) -0.0069(14) C15 0.052(2) 0.040(2) 0.042(2) -0.0292(18) 0.0024(18) -0.0063(17) C16 0.0255(17) 0.0290(17) 0.0427(19) -0.0228(15) 0.0056(16) -0.0095(14) C17 0.0204(16) 0.0255(16) 0.0384(18) -0.0164(14) 0.0045(15) -0.0069(13) C18 0.042(2) 0.0246(17) 0.047(2) -0.0147(16) -0.0019(18) -0.0072(15) _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. ; # start Validation Reply Form _vrf_PLAT029_shelxl ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.85 RESPONSE: small single crystal of bad quality, probably due to the disorder on carbonyl groups which occupies 25% of each alpha position of the nitrogen atoms. ; # end Validation Reply Form 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 1.987(2) . ? Pd1 N1 1.988(2) . ? Pd1 O1 2.001(2) . ? Pd1 O2 2.007(2) . ? O1 C14 1.281(3) . ? O2 C17 1.278(3) . ? N1 C2 1.339(4) . ? N1 C4 1.442(4) . ? N2 C3 1.331(4) . ? N2 C9 1.451(4) . ? C1 C2 1.389(4) . ? C1 C3 1.403(4) 2_576 ? C1 H1 0.9500 . ? C2 C3 1.492(4) . ? C3 C1 1.403(4) 2_576 ? C4 C5 1.524(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C7 1.520(5) . ? C5 C8 1.524(5) . ? C5 C6 1.531(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.536(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.529(5) . ? C10 C11 1.530(5) . ? C10 C13 1.532(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.388(5) . ? C14 C15 1.505(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.390(4) . ? C16 H16 0.9500 . ? C17 C18 1.505(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 N1 79.90(10) . . ? N2 Pd1 O1 172.04(9) . . ? N1 Pd1 O1 93.12(9) . . ? N2 Pd1 O2 94.15(9) . . ? N1 Pd1 O2 173.89(9) . . ? O1 Pd1 O2 92.72(9) . . ? C14 O1 Pd1 124.3(2) . . ? C17 O2 Pd1 124.1(2) . . ? C2 N1 C4 122.2(2) . . ? C2 N1 Pd1 113.86(19) . . ? C4 N1 Pd1 123.36(19) . . ? C3 N2 C9 122.4(2) . . ? C3 N2 Pd1 113.79(19) . . ? C9 N2 Pd1 123.16(19) . . ? C2 C1 C3 120.9(3) . 2_576 ? C2 C1 H1 119.5 . . ? C3 C1 H1 119.5 2_576 . ? N1 C2 C1 127.1(3) . . ? N1 C2 C3 113.1(2) . . ? C1 C2 C3 119.8(3) . . ? N2 C3 C1 127.0(3) . 2_576 ? N2 C3 C2 113.7(3) . . ? C1 C3 C2 119.3(3) 2_576 . ? N1 C4 C5 115.2(3) . . ? N1 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? N1 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C7 C5 C8 111.0(3) . . ? C7 C5 C4 107.9(3) . . ? C8 C5 C4 112.3(3) . . ? C7 C5 C6 108.7(3) . . ? C8 C5 C6 108.3(3) . . ? C4 C5 C6 108.6(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 114.1(3) . . ? N2 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N2 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C12 C10 C11 109.6(3) . . ? C12 C10 C13 108.7(3) . . ? C11 C10 C13 109.9(3) . . ? C12 C10 C9 111.5(3) . . ? C11 C10 C9 109.8(3) . . ? C13 C10 C9 107.3(3) . . ? 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 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 C16 125.8(3) . . ? O1 C14 C15 114.0(3) . . ? C16 C14 C15 120.1(3) . . ? 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 C17 126.8(3) . . ? C14 C16 H16 116.6 . . ? C17 C16 H16 116.6 . . ? O2 C17 C16 126.0(3) . . ? O2 C17 C18 114.1(3) . . ? C16 C17 C18 119.9(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 O1 C14 -146.1(6) . . . . ? N1 Pd1 O1 C14 -174.7(2) . . . . ? O2 Pd1 O1 C14 3.5(2) . . . . ? N2 Pd1 O2 C17 174.7(2) . . . . ? N1 Pd1 O2 C17 161.6(8) . . . . ? O1 Pd1 O2 C17 -1.3(2) . . . . ? N2 Pd1 N1 C2 -20.4(2) . . . . ? O1 Pd1 N1 C2 155.7(2) . . . . ? O2 Pd1 N1 C2 -7.2(9) . . . . ? N2 Pd1 N1 C4 167.7(2) . . . . ? O1 Pd1 N1 C4 -16.1(2) . . . . ? O2 Pd1 N1 C4 -179(34) . . . . ? N1 Pd1 N2 C3 20.8(2) . . . . ? O1 Pd1 N2 C3 -8.2(8) . . . . ? O2 Pd1 N2 C3 -157.8(2) . . . . ? N1 Pd1 N2 C9 -168.0(2) . . . . ? O1 Pd1 N2 C9 163.0(6) . . . . ? O2 Pd1 N2 C9 13.4(2) . . . . ? C4 N1 C2 C1 6.4(5) . . . . ? Pd1 N1 C2 C1 -165.5(2) . . . . ? C4 N1 C2 C3 -171.5(3) . . . . ? Pd1 N1 C2 C3 16.6(3) . . . . ? C3 C1 C2 N1 -177.8(3) 2_576 . . . ? C3 C1 C2 C3 -0.1(5) 2_576 . . . ? C9 N2 C3 C1 -6.1(5) . . . 2_576 ? Pd1 N2 C3 C1 165.1(3) . . . 2_576 ? C9 N2 C3 C2 171.1(3) . . . . ? Pd1 N2 C3 C2 -17.6(3) . . . . ? N1 C2 C3 N2 0.7(4) . . . . ? C1 C2 C3 N2 -177.4(3) . . . . ? N1 C2 C3 C1 178.1(3) . . . 2_576 ? C1 C2 C3 C1 0.1(5) . . . 2_576 ? C2 N1 C4 C5 103.2(3) . . . . ? Pd1 N1 C4 C5 -85.6(3) . . . . ? N1 C4 C5 C7 172.8(3) . . . . ? N1 C4 C5 C8 50.2(4) . . . . ? N1 C4 C5 C6 -69.6(4) . . . . ? C3 N2 C9 C10 -102.2(3) . . . . ? Pd1 N2 C9 C10 87.4(3) . . . . ? N2 C9 C10 C12 -54.7(3) . . . . ? N2 C9 C10 C11 67.0(4) . . . . ? N2 C9 C10 C13 -173.6(3) . . . . ? Pd1 O1 C14 C16 -3.5(4) . . . . ? Pd1 O1 C14 C15 178.1(2) . . . . ? O1 C14 C16 C17 0.1(6) . . . . ? C15 C14 C16 C17 178.4(3) . . . . ? Pd1 O2 C17 C16 -1.2(4) . . . . ? Pd1 O2 C17 C18 177.1(2) . . . . ? C14 C16 C17 O2 2.6(6) . . . . ? C14 C16 C17 C18 -175.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 0.965 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.090