# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'McKinnon, Stephen' 'Gilroy, Joe' 'McDonald, Robert' 'Patrick, Brian' 'Hicks, Robin' _publ_contact_author_name 'Hicks, Robin' _publ_contact_author_email rhicks@uvic.ca _publ_section_title ; Magnetostructural studies of palladium(II) and platinum(II) complexes of verdazyl radicals ; # Attachment '- rh079_0m.cif' data_rh079_0m _database_code_depnum_ccdc_archive 'CCDC 787978' #TrackingRef '- rh079_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 Cl2 N6 O Pt' _chemical_formula_weight 529.32 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' Pt Pt -1.7033 8.3905 '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' 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 10.9511(3) _cell_length_b 10.1813(3) _cell_length_c 14.9822(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.8150(10) _cell_angle_gamma 90.00 _cell_volume 1658.66(8) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 8.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.119 _exptl_absorpt_correction_T_max 0.224 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16599 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.02 _reflns_number_total 4014 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0180P)^2^+2.1169P] 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 4014 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.013 _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 C1 C 0.0578(2) 0.0739(3) 0.67475(18) 0.0134(5) Uani 1 1 d . . . C2 C 0.2134(3) -0.1219(3) 0.7285(2) 0.0183(6) Uani 1 1 d . . . C3 C 0.3546(3) -0.0375(3) 0.6235(2) 0.0170(6) Uani 1 1 d . . . H3 H 0.3517 0.0318 0.5759 0.020 Uiso 1 1 calc R . . C4 C 0.4443(3) 0.0093(3) 0.7033(2) 0.0224(6) Uani 1 1 d . . . H4A H 0.4116 0.0886 0.7290 0.034 Uiso 1 1 calc R . . H4B H 0.5240 0.0292 0.6829 0.034 Uiso 1 1 calc R . . H4C H 0.4546 -0.0598 0.7491 0.034 Uiso 1 1 calc R . . C6 C 0.1102(3) -0.1396(3) 0.8654(2) 0.0206(6) Uani 1 1 d . . . H6 H 0.1449 -0.2306 0.8663 0.025 Uiso 1 1 calc R . . C7 C -0.0229(4) -0.1493(4) 0.8802(3) 0.0388(9) Uani 1 1 d . . . H7A H -0.0567 -0.0608 0.8854 0.058 Uiso 1 1 calc R . . H7B H -0.0300 -0.1984 0.9356 0.058 Uiso 1 1 calc R . . H7C H -0.0689 -0.1949 0.8293 0.058 Uiso 1 1 calc R . . C8 C 0.1870(4) -0.0598(4) 0.9359(2) 0.0344(9) Uani 1 1 d . . . H8A H 0.2720 -0.0562 0.9217 0.052 Uiso 1 1 calc R . . H8B H 0.1851 -0.1009 0.9949 0.052 Uiso 1 1 calc R . . H8C H 0.1537 0.0294 0.9370 0.052 Uiso 1 1 calc R . . C11 C -0.0195(3) 0.1830(3) 0.64121(19) 0.0152(5) Uani 1 1 d . . . C12 C -0.0787(3) 0.3384(3) 0.5466(2) 0.0219(6) Uani 1 1 d . . . H12 H -0.0855 0.3938 0.4952 0.026 Uiso 1 1 calc R . . C5 C 0.3947(3) -0.1645(3) 0.5826(2) 0.0246(7) Uani 1 1 d . . . H5A H 0.4070 -0.2322 0.6293 0.037 Uiso 1 1 calc R . . H5B H 0.4720 -0.1499 0.5571 0.037 Uiso 1 1 calc R . . H5C H 0.3312 -0.1932 0.5351 0.037 Uiso 1 1 calc R . . C13 C -0.1460(3) 0.3473(3) 0.6164(2) 0.0242(7) Uani 1 1 d . . . H13 H -0.2080 0.4107 0.6229 0.029 Uiso 1 1 calc R . . C14 C -0.1662(3) 0.2166(4) 0.7570(2) 0.0246(7) Uani 1 1 d . . . H14A H -0.2233 0.1431 0.7441 0.037 Uiso 1 1 calc R . . H14B H -0.2112 0.2932 0.7755 0.037 Uiso 1 1 calc R . . H14C H -0.1023 0.1919 0.8055 0.037 Uiso 1 1 calc R . . N1 N 0.2282(2) -0.0489(2) 0.65127(16) 0.0152(5) Uani 1 1 d . . . N2 N 0.1431(2) 0.0437(2) 0.61863(15) 0.0128(5) Uani 1 1 d . . . N3 N 0.1202(2) -0.0820(3) 0.77572(16) 0.0168(5) Uani 1 1 d . . . N4 N 0.0456(2) 0.0212(2) 0.75217(15) 0.0149(5) Uani 1 1 d . . . N11 N 0.0008(2) 0.2351(2) 0.56316(16) 0.0158(5) Uani 1 1 d . . . N12 N -0.1091(2) 0.2489(3) 0.67638(17) 0.0185(5) Uani 1 1 d . . . O1 O 0.2823(2) -0.2116(2) 0.75322(16) 0.0282(5) Uani 1 1 d . . . Cl1 Cl 0.07017(7) 0.26774(8) 0.37396(5) 0.02511(16) Uani 1 1 d . . . Cl2 Cl 0.25011(7) 0.02280(8) 0.41656(5) 0.02047(15) Uani 1 1 d . . . Pt1 Pt 0.120622(9) 0.139848(10) 0.497474(7) 0.01302(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 0.0110(12) 0.0144(13) 0.0146(12) -0.0032(11) -0.0001(9) -0.0013(11) C2 0.0185(14) 0.0180(15) 0.0183(14) 0.0031(11) 0.0014(11) 0.0015(11) C3 0.0126(13) 0.0181(15) 0.0204(14) -0.0021(11) 0.0029(10) 0.0028(11) C4 0.0193(15) 0.0202(16) 0.0258(16) -0.0029(13) -0.0057(12) 0.0012(12) C6 0.0288(16) 0.0178(15) 0.0155(14) 0.0057(11) 0.0041(12) 0.0017(13) C7 0.037(2) 0.048(3) 0.035(2) 0.0141(17) 0.0172(16) -0.0037(18) C8 0.052(2) 0.028(2) 0.0198(16) -0.0020(14) -0.0078(15) 0.0078(17) C11 0.0121(12) 0.0140(14) 0.0186(13) -0.0028(11) -0.0017(10) 0.0009(11) C12 0.0195(14) 0.0164(15) 0.0285(16) 0.0033(12) -0.0022(12) 0.0057(12) C5 0.0205(15) 0.0254(17) 0.0277(17) -0.0081(13) 0.0024(12) 0.0056(13) C13 0.0202(15) 0.0190(16) 0.0321(17) -0.0012(13) -0.0025(13) 0.0075(12) C14 0.0191(15) 0.0334(19) 0.0221(15) -0.0059(13) 0.0055(12) 0.0056(14) N1 0.0144(11) 0.0142(12) 0.0175(11) 0.0035(9) 0.0032(9) 0.0046(9) N2 0.0113(10) 0.0144(12) 0.0122(10) 0.0002(9) -0.0008(8) 0.0011(9) N3 0.0192(12) 0.0166(12) 0.0144(11) 0.0026(10) 0.0012(9) -0.0003(10) N4 0.0143(11) 0.0148(12) 0.0153(11) -0.0011(9) 0.0006(9) -0.0007(9) N11 0.0154(11) 0.0126(12) 0.0182(12) 0.0008(9) -0.0026(9) -0.0001(9) N12 0.0137(11) 0.0189(13) 0.0224(13) -0.0057(10) -0.0004(9) 0.0037(10) O1 0.0295(12) 0.0253(13) 0.0303(12) 0.0126(10) 0.0065(10) 0.0130(10) Cl1 0.0291(4) 0.0283(4) 0.0170(3) 0.0081(3) -0.0011(3) 0.0023(3) Cl2 0.0214(3) 0.0247(4) 0.0160(3) -0.0030(3) 0.0050(3) -0.0010(3) Pt1 0.01239(6) 0.01464(6) 0.01158(6) 0.00071(4) -0.00048(4) -0.00142(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 C1 N4 1.299(4) . ? C1 N2 1.364(3) . ? C1 C11 1.450(4) . ? C2 O1 1.214(4) . ? C2 N3 1.370(4) . ? C2 N1 1.401(4) . ? C3 N1 1.497(4) . ? C3 C5 1.518(4) . ? C3 C4 1.530(4) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 N3 1.482(4) . ? C6 C7 1.504(5) . ? C6 C8 1.507(5) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 N11 1.326(4) . ? C11 N12 1.347(4) . ? C12 C13 1.352(5) . ? C12 N11 1.370(4) . ? C12 H12 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C13 N12 1.374(4) . ? C13 H13 0.9500 . ? C14 N12 1.462(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N1 N2 1.374(3) . ? N2 Pt1 2.051(2) . ? N3 N4 1.352(3) . ? N11 Pt1 1.984(2) . ? Cl1 Pt1 2.2765(7) . ? Cl2 Pt1 2.3040(7) . ? 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 N4 C1 N2 127.4(3) . . ? N4 C1 C11 120.6(3) . . ? N2 C1 C11 111.9(2) . . ? O1 C2 N3 122.7(3) . . ? O1 C2 N1 121.5(3) . . ? N3 C2 N1 115.8(2) . . ? N1 C3 C5 111.6(2) . . ? N1 C3 C4 109.6(2) . . ? C5 C3 C4 113.0(2) . . ? N1 C3 H3 107.5 . . ? C5 C3 H3 107.5 . . ? C4 C3 H3 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C6 C7 109.7(3) . . ? N3 C6 C8 109.1(3) . . ? C7 C6 C8 113.7(3) . . ? N3 C6 H6 108.1 . . ? C7 C6 H6 108.1 . . ? C8 C6 H6 108.1 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N11 C11 N12 110.6(3) . . ? N11 C11 C1 117.4(3) . . ? N12 C11 C1 132.0(3) . . ? C13 C12 N11 107.7(3) . . ? C13 C12 H12 126.1 . . ? N11 C12 H12 126.1 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C13 N12 108.2(3) . . ? C12 C13 H13 125.9 . . ? N12 C13 H13 125.9 . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 N1 C2 121.2(2) . . ? N2 N1 C3 117.3(2) . . ? C2 N1 C3 118.2(2) . . ? C1 N2 N1 114.9(2) . . ? C1 N2 Pt1 114.77(18) . . ? N1 N2 Pt1 130.33(18) . . ? N4 N3 C2 124.0(2) . . ? N4 N3 C6 115.9(2) . . ? C2 N3 C6 119.4(2) . . ? C1 N4 N3 115.5(2) . . ? C11 N11 C12 107.3(3) . . ? C11 N11 Pt1 115.59(19) . . ? C12 N11 Pt1 136.8(2) . . ? C11 N12 C13 106.2(3) . . ? C11 N12 C14 127.9(3) . . ? C13 N12 C14 125.7(3) . . ? N11 Pt1 N2 79.11(9) . . ? N11 Pt1 Cl1 90.73(7) . . ? N2 Pt1 Cl1 169.84(7) . . ? N11 Pt1 Cl2 176.61(7) . . ? N2 Pt1 Cl2 101.66(7) . . ? Cl1 Pt1 Cl2 88.47(3) . . ? 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 N4 C1 C11 N11 177.7(3) . . . . ? N2 C1 C11 N11 1.1(4) . . . . ? N4 C1 C11 N12 0.7(5) . . . . ? N2 C1 C11 N12 -175.8(3) . . . . ? N11 C12 C13 N12 -0.4(4) . . . . ? O1 C2 N1 N2 173.5(3) . . . . ? N3 C2 N1 N2 -9.2(4) . . . . ? O1 C2 N1 C3 -27.6(4) . . . . ? N3 C2 N1 C3 149.7(3) . . . . ? C5 C3 N1 N2 -126.3(3) . . . . ? C4 C3 N1 N2 107.8(3) . . . . ? C5 C3 N1 C2 74.0(3) . . . . ? C4 C3 N1 C2 -51.9(3) . . . . ? N4 C1 N2 N1 -3.3(4) . . . . ? C11 C1 N2 N1 173.0(2) . . . . ? N4 C1 N2 Pt1 175.0(2) . . . . ? C11 C1 N2 Pt1 -8.8(3) . . . . ? C2 N1 N2 C1 10.9(4) . . . . ? C3 N1 N2 C1 -148.2(2) . . . . ? C2 N1 N2 Pt1 -167.0(2) . . . . ? C3 N1 N2 Pt1 33.9(3) . . . . ? O1 C2 N3 N4 176.8(3) . . . . ? N1 C2 N3 N4 -0.5(4) . . . . ? O1 C2 N3 C6 6.9(5) . . . . ? N1 C2 N3 C6 -170.4(3) . . . . ? C7 C6 N3 N4 42.5(4) . . . . ? C8 C6 N3 N4 -82.6(3) . . . . ? C7 C6 N3 C2 -146.7(3) . . . . ? C8 C6 N3 C2 88.2(3) . . . . ? N2 C1 N4 N3 -5.7(4) . . . . ? C11 C1 N4 N3 178.4(2) . . . . ? C2 N3 N4 C1 7.5(4) . . . . ? C6 N3 N4 C1 177.8(2) . . . . ? N12 C11 N11 C12 -0.2(3) . . . . ? C1 C11 N11 C12 -177.8(2) . . . . ? N12 C11 N11 Pt1 -175.01(18) . . . . ? C1 C11 N11 Pt1 7.4(3) . . . . ? C13 C12 N11 C11 0.4(3) . . . . ? C13 C12 N11 Pt1 173.5(2) . . . . ? N11 C11 N12 C13 0.0(3) . . . . ? C1 C11 N12 C13 177.1(3) . . . . ? N11 C11 N12 C14 174.2(3) . . . . ? C1 C11 N12 C14 -8.6(5) . . . . ? C12 C13 N12 C11 0.3(3) . . . . ? C12 C13 N12 C14 -174.1(3) . . . . ? C11 N11 Pt1 N2 -9.2(2) . . . . ? C12 N11 Pt1 N2 178.1(3) . . . . ? C11 N11 Pt1 Cl1 170.6(2) . . . . ? C12 N11 Pt1 Cl1 -2.1(3) . . . . ? C11 N11 Pt1 Cl2 94.3(12) . . . . ? C12 N11 Pt1 Cl2 -78.4(13) . . . . ? C1 N2 Pt1 N11 9.93(19) . . . . ? N1 N2 Pt1 N11 -172.1(2) . . . . ? C1 N2 Pt1 Cl1 9.1(5) . . . . ? N1 N2 Pt1 Cl1 -172.9(3) . . . . ? C1 N2 Pt1 Cl2 -166.71(18) . . . . ? N1 N2 Pt1 Cl2 11.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.211 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.108 # Attachment '- vic0518.cif' data_vic0518 _database_code_depnum_ccdc_archive 'CCDC 787979' #TrackingRef '- vic0518.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H10 Cl2 N5 O Pd' _chemical_formula_sum 'C9 H10 Cl2 N5 O Pd' _chemical_formula_weight 381.52 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 Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.9439(8) _cell_length_b 11.4246(13) _cell_length_c 15.6571(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1242.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4348 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.34 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3429 _exptl_absorpt_correction_T_max 0.8463 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8853 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.38 _reflns_number_total 2553 _reflns_number_gt 2500 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0204P)^2^+0.2636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.32(2) _refine_ls_number_reflns 2553 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0159 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0399 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Pd Pd 0.32051(2) 0.314995(14) -0.018376(10) 0.02258(5) Uani 1 1 d . . . Cl1 Cl 0.28954(9) 0.51281(5) -0.02898(4) 0.03440(13) Uani 1 1 d . . . Cl2 Cl 0.28697(9) 0.30765(6) -0.16357(4) 0.03501(13) Uani 1 1 d . . . O O 0.2613(3) -0.15293(15) -0.05646(13) 0.0447(5) Uani 1 1 d . . . N1 N 0.3205(3) 0.04089(16) -0.03985(12) 0.0265(4) Uani 1 1 d . . . N2 N 0.3247(3) 0.13826(15) 0.01069(12) 0.0245(3) Uani 1 1 d . . . N3 N 0.2615(3) 0.01586(17) 0.13099(13) 0.0282(4) Uani 1 1 d . . . N4 N 0.2467(3) -0.07604(16) 0.07750(14) 0.0297(4) Uani 1 1 d . . . N10 N 0.3445(3) 0.32274(16) 0.11040(12) 0.0239(4) Uani 1 1 d . . . C1 C 0.2967(3) 0.1175(2) 0.09496(14) 0.0239(4) Uani 1 1 d . . . C2 C 0.2735(3) -0.06938(19) -0.00954(16) 0.0300(5) Uani 1 1 d . . . C3 C 0.3977(4) 0.0462(2) -0.12711(16) 0.0338(5) Uani 1 1 d . . . H3A H 0.4782 0.1161 -0.1333 0.041 Uiso 1 1 calc R . . H3B H 0.2910 0.0498 -0.1680 0.041 Uiso 1 1 calc R . . H3C H 0.4754 -0.0238 -0.1383 0.041 Uiso 1 1 calc R . . C4 C 0.1896(4) -0.1885(2) 0.11494(17) 0.0423(6) Uani 1 1 d . . . H4A H 0.2720 -0.2508 0.0922 0.051 Uiso 1 1 calc R . . H4B H 0.0550 -0.2050 0.1005 0.051 Uiso 1 1 calc R . . H4C H 0.2038 -0.1849 0.1772 0.051 Uiso 1 1 calc R . . C11 C 0.3129(3) 0.21989(18) 0.15118(14) 0.0242(4) Uani 1 1 d . . . C12 C 0.3022(4) 0.21313(19) 0.23884(15) 0.0295(5) Uani 1 1 d . . . H12 H 0.2770 0.1403 0.2659 0.035 Uiso 1 1 calc R . . C13 C 0.3283(3) 0.3129(2) 0.28725(15) 0.0332(5) Uani 1 1 d . . . H13 H 0.3198 0.3101 0.3478 0.040 Uiso 1 1 calc R . . C14 C 0.3672(3) 0.4173(2) 0.24560(16) 0.0324(6) Uani 1 1 d . . . H14 H 0.3884 0.4869 0.2774 0.039 Uiso 1 1 calc R . . C15 C 0.3748(3) 0.4192(2) 0.15776(16) 0.0288(5) Uani 1 1 d . . . H15 H 0.4024 0.4910 0.1297 0.035 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 Pd 0.02417(8) 0.02270(8) 0.02089(9) 0.00091(7) -0.00072(7) -0.00075(7) Cl1 0.0481(3) 0.0238(2) 0.0313(3) 0.0056(2) 0.0012(3) -0.0018(2) Cl2 0.0431(3) 0.0393(3) 0.0226(3) 0.0008(3) -0.0016(2) -0.0005(3) O 0.0674(13) 0.0270(9) 0.0396(11) -0.0105(8) -0.0003(10) -0.0038(8) N1 0.0306(9) 0.0252(9) 0.0238(9) -0.0049(7) -0.0026(9) -0.0005(9) N2 0.0249(8) 0.0230(8) 0.0256(9) -0.0027(7) -0.0040(9) 0.0007(7) N3 0.0343(10) 0.0232(9) 0.0271(10) -0.0015(8) -0.0035(8) 0.0000(8) N4 0.0398(10) 0.0197(9) 0.0297(10) -0.0005(8) -0.0043(8) -0.0024(8) N10 0.0258(9) 0.0229(8) 0.0231(9) -0.0012(7) -0.0026(7) 0.0007(9) C1 0.0216(11) 0.0261(11) 0.0241(10) 0.0006(9) -0.0038(9) 0.0006(9) C2 0.0320(11) 0.0272(11) 0.0308(12) -0.0045(10) -0.0041(10) 0.0019(9) C3 0.0380(12) 0.0353(12) 0.0281(12) -0.0065(11) 0.0036(11) -0.0003(11) C4 0.0623(16) 0.0238(10) 0.0407(14) 0.0044(11) -0.0083(14) -0.0069(16) C11 0.0229(9) 0.0246(10) 0.0250(10) -0.0018(8) -0.0012(10) 0.0005(9) C12 0.0362(12) 0.0268(11) 0.0255(11) 0.0011(9) 0.0021(10) -0.0016(10) C13 0.0399(12) 0.0356(11) 0.0240(11) -0.0033(10) 0.0021(10) -0.0009(14) C14 0.0374(14) 0.0300(11) 0.0297(12) -0.0088(10) -0.0038(10) -0.0015(10) C15 0.0334(12) 0.0237(10) 0.0293(11) -0.0010(10) -0.0032(10) -0.0013(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 Pd N10 2.0251(18) . ? Pd N2 2.0700(18) . ? Pd Cl1 2.2762(6) . ? Pd Cl2 2.2868(6) . ? O C2 1.207(3) . ? N1 N2 1.366(3) . ? N1 C2 1.385(3) . ? N1 C3 1.469(3) . ? N2 C1 1.355(3) . ? N3 C1 1.314(3) . ? N3 N4 1.347(3) . ? N4 C2 1.378(3) . ? N4 C4 1.467(3) . ? N10 C15 1.345(3) . ? N10 C11 1.355(3) . ? C1 C11 1.468(3) . ? C11 C12 1.377(3) . ? C12 C13 1.381(3) . ? C13 C14 1.386(3) . ? C14 C15 1.376(4) . ? 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 N10 Pd N2 79.78(7) . . ? N10 Pd Cl1 92.12(6) . . ? N2 Pd Cl1 170.34(5) . . ? N10 Pd Cl2 178.81(5) . . ? N2 Pd Cl2 100.62(5) . . ? Cl1 Pd Cl2 87.38(2) . . ? N2 N1 C2 123.18(19) . . ? N2 N1 C3 119.85(19) . . ? C2 N1 C3 116.24(19) . . ? C1 N2 N1 114.76(18) . . ? C1 N2 Pd 112.51(14) . . ? N1 N2 Pd 131.83(14) . . ? C1 N3 N4 115.9(2) . . ? N3 N4 C2 124.2(2) . . ? N3 N4 C4 117.1(2) . . ? C2 N4 C4 118.7(2) . . ? C15 N10 C11 118.44(19) . . ? C15 N10 Pd 126.69(16) . . ? C11 N10 Pd 114.70(14) . . ? N3 C1 N2 126.8(2) . . ? N3 C1 C11 117.4(2) . . ? N2 C1 C11 115.70(19) . . ? O C2 N4 123.3(2) . . ? O C2 N1 121.8(2) . . ? N4 C2 N1 114.9(2) . . ? N10 C11 C12 121.81(19) . . ? N10 C11 C1 114.88(19) . . ? C12 C11 C1 123.29(19) . . ? C11 C12 C13 119.6(2) . . ? C12 C13 C14 118.5(2) . . ? C15 C14 C13 119.4(2) . . ? N10 C15 C14 122.1(2) . . ? 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 C2 N1 N2 C1 5.9(3) . . . . ? C3 N1 N2 C1 -164.0(2) . . . . ? C2 N1 N2 Pd -162.28(16) . . . . ? C3 N1 N2 Pd 27.8(3) . . . . ? N10 Pd N2 C1 13.93(15) . . . . ? Cl1 Pd N2 C1 -19.4(4) . . . . ? Cl2 Pd N2 C1 -164.93(14) . . . . ? N10 Pd N2 N1 -177.7(2) . . . . ? Cl1 Pd N2 N1 148.9(3) . . . . ? Cl2 Pd N2 N1 3.4(2) . . . . ? C1 N3 N4 C2 2.6(3) . . . . ? C1 N3 N4 C4 -174.4(2) . . . . ? N2 Pd N10 C15 172.32(19) . . . . ? Cl1 Pd N10 C15 -12.98(18) . . . . ? Cl2 Pd N10 C15 -78(3) . . . . ? N2 Pd N10 C11 -12.51(15) . . . . ? Cl1 Pd N10 C11 162.19(15) . . . . ? Cl2 Pd N10 C11 97(3) . . . . ? N4 N3 C1 N2 -2.0(3) . . . . ? N4 N3 C1 C11 179.70(19) . . . . ? N1 N2 C1 N3 -2.1(3) . . . . ? Pd N2 C1 N3 168.40(19) . . . . ? N1 N2 C1 C11 176.27(19) . . . . ? Pd N2 C1 C11 -13.3(2) . . . . ? N3 N4 C2 O 179.3(2) . . . . ? C4 N4 C2 O -3.7(4) . . . . ? N3 N4 C2 N1 0.8(3) . . . . ? C4 N4 C2 N1 177.8(2) . . . . ? N2 N1 C2 O 176.2(2) . . . . ? C3 N1 C2 O -13.6(3) . . . . ? N2 N1 C2 N4 -5.3(3) . . . . ? C3 N1 C2 N4 164.9(2) . . . . ? C15 N10 C11 C12 3.1(3) . . . . ? Pd N10 C11 C12 -172.5(2) . . . . ? C15 N10 C11 C1 -175.3(2) . . . . ? Pd N10 C11 C1 9.1(3) . . . . ? N3 C1 C11 N10 -178.4(2) . . . . ? N2 C1 C11 N10 3.1(3) . . . . ? N3 C1 C11 C12 3.2(4) . . . . ? N2 C1 C11 C12 -175.3(2) . . . . ? N10 C11 C12 C13 -1.4(4) . . . . ? C1 C11 C12 C13 176.8(2) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? C12 C13 C14 C15 1.3(4) . . . . ? C11 N10 C15 C14 -2.6(3) . . . . ? Pd N10 C15 C14 172.45(18) . . . . ? C13 C14 C15 N10 0.4(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.338 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.081 # Attachment '- vic0528.cif' data_vic0528 _database_code_depnum_ccdc_archive 'CCDC 787980' #TrackingRef '- vic0528.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H18 Cl2 N5 O Pd' _chemical_formula_sum 'C13 H18 Cl2 N5 O Pd' _chemical_formula_weight 437.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.9445(9) _cell_length_b 17.0345(16) _cell_length_c 10.1105(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.8653(12) _cell_angle_gamma 90.00 _cell_volume 1647.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4731 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.35 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7896 _exptl_absorpt_correction_T_max 0.8001 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9900 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3374 _reflns_number_gt 2840 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0295P)^2^+0.6193P] 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 3374 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Pd Pd -0.03211(2) 0.434913(11) -0.13972(2) 0.02021(8) Uani 1 1 d . . . Cl1 Cl -0.15202(8) 0.51765(5) -0.30732(8) 0.0381(2) Uani 1 1 d . . . Cl2 Cl -0.23471(7) 0.41885(4) -0.07766(8) 0.03433(18) Uani 1 1 d . . . O O 0.1550(2) 0.24831(12) 0.3030(2) 0.0339(5) Uani 1 1 d . . . N1 N 0.0746(2) 0.31130(13) 0.0980(2) 0.0204(5) Uani 1 1 d . . . N2 N 0.0996(2) 0.36407(12) 0.0047(2) 0.0183(4) Uani 1 1 d . . . N3 N 0.3110(2) 0.31456(13) 0.2184(2) 0.0221(5) Uani 1 1 d . . . N4 N 0.3427(2) 0.35650(13) 0.1173(2) 0.0211(5) Uani 1 1 d . . . N10 N 0.1503(2) 0.45187(12) -0.1890(2) 0.0203(5) Uani 1 1 d . . . C1 C 0.2348(3) 0.38001(14) 0.0184(3) 0.0183(5) Uani 1 1 d . . . C2 C 0.1789(3) 0.28909(16) 0.2140(3) 0.0230(6) Uani 1 1 d . . . C3 C -0.0581(3) 0.26562(16) 0.0559(3) 0.0234(6) Uani 1 1 d . . . H3 H -0.1149 0.2877 -0.0336 0.028 Uiso 1 1 calc R . . C4 C -0.0264(3) 0.18066(17) 0.0309(3) 0.0349(7) Uani 1 1 d . . . H4A H 0.0287 0.1784 -0.0359 0.042 Uiso 1 1 calc R . . H4B H -0.1143 0.1520 -0.0052 0.042 Uiso 1 1 calc R . . H4C H 0.0267 0.1567 0.1176 0.042 Uiso 1 1 calc R . . C5 C -0.1434(3) 0.2744(2) 0.1589(3) 0.0395(8) Uani 1 1 d . . . H5A H -0.1602 0.3302 0.1718 0.047 Uiso 1 1 calc R . . H5B H -0.0920 0.2514 0.2471 0.047 Uiso 1 1 calc R . . H5C H -0.2331 0.2473 0.1244 0.047 Uiso 1 1 calc R . . C6 C 0.4293(3) 0.29459(17) 0.3400(3) 0.0270(6) Uani 1 1 d . . . H6 H 0.4033 0.2465 0.3841 0.032 Uiso 1 1 calc R . . C7 C 0.5594(3) 0.2764(2) 0.2945(3) 0.0436(9) Uani 1 1 d . . . H7A H 0.5392 0.2339 0.2267 0.052 Uiso 1 1 calc R . . H7B H 0.6350 0.2602 0.3744 0.052 Uiso 1 1 calc R . . H7C H 0.5881 0.3234 0.2533 0.052 Uiso 1 1 calc R . . C8 C 0.4506(3) 0.3611(2) 0.4425(3) 0.0398(8) Uani 1 1 d . . . H8A H 0.3629 0.3716 0.4657 0.048 Uiso 1 1 calc R . . H8B H 0.4798 0.4084 0.4023 0.048 Uiso 1 1 calc R . . H8C H 0.5231 0.3466 0.5260 0.048 Uiso 1 1 calc R . . C11 C 0.2645(3) 0.42401(14) -0.0960(3) 0.0207(6) Uani 1 1 d . . . C12 C 0.3972(3) 0.43247(15) -0.1115(3) 0.0238(6) Uani 1 1 d . . . H12 H 0.4760 0.4124 -0.0441 0.029 Uiso 1 1 calc R . . C13 C 0.4139(3) 0.47051(17) -0.2266(3) 0.0293(6) Uani 1 1 d . . . H13 H 0.5042 0.4771 -0.2397 0.035 Uiso 1 1 calc R . . C14 C 0.2967(3) 0.49874(17) -0.3225(3) 0.0313(7) Uani 1 1 d . . . H14 H 0.3055 0.5246 -0.4030 0.038 Uiso 1 1 calc R . . C15 C 0.1677(3) 0.48909(16) -0.3004(3) 0.0283(6) Uani 1 1 d . . . H15 H 0.0879 0.5094 -0.3660 0.034 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 Pd 0.01750(12) 0.01966(12) 0.02029(12) -0.00153(8) -0.00023(8) 0.00422(8) Cl1 0.0378(4) 0.0393(4) 0.0298(4) 0.0059(3) -0.0031(3) 0.0177(3) Cl2 0.0197(4) 0.0339(4) 0.0490(5) -0.0050(3) 0.0089(3) 0.0050(3) O 0.0281(11) 0.0461(13) 0.0273(11) 0.0163(10) 0.0074(9) -0.0015(9) N1 0.0174(11) 0.0241(11) 0.0194(11) 0.0023(9) 0.0042(9) -0.0012(9) N2 0.0184(11) 0.0185(11) 0.0178(11) 0.0004(9) 0.0048(8) 0.0021(9) N3 0.0183(11) 0.0268(12) 0.0197(11) 0.0067(9) 0.0031(9) 0.0023(9) N4 0.0199(12) 0.0247(12) 0.0185(11) 0.0053(9) 0.0050(9) 0.0015(9) N10 0.0205(12) 0.0192(11) 0.0184(11) 0.0002(9) 0.0006(9) 0.0010(9) C1 0.0202(13) 0.0153(12) 0.0188(12) 0.0001(10) 0.0045(10) 0.0018(10) C2 0.0225(14) 0.0248(14) 0.0221(13) 0.0033(11) 0.0071(11) -0.0006(11) C3 0.0187(14) 0.0304(14) 0.0198(13) -0.0018(11) 0.0033(11) -0.0058(11) C4 0.0457(19) 0.0272(16) 0.0298(16) 0.0038(13) 0.0072(14) -0.0054(14) C5 0.0245(16) 0.066(2) 0.0291(16) -0.0001(16) 0.0092(13) -0.0071(15) C6 0.0210(14) 0.0312(15) 0.0256(14) 0.0107(12) 0.0009(11) 0.0050(12) C7 0.0283(18) 0.064(2) 0.0347(18) 0.0055(16) 0.0029(14) 0.0199(16) C8 0.0359(18) 0.052(2) 0.0249(16) 0.0027(14) -0.0029(13) 0.0086(15) C11 0.0248(15) 0.0162(12) 0.0200(13) 0.0002(10) 0.0045(11) 0.0005(10) C12 0.0202(14) 0.0257(14) 0.0244(14) 0.0050(11) 0.0043(11) 0.0011(11) C13 0.0277(16) 0.0340(17) 0.0275(15) 0.0042(13) 0.0097(12) -0.0022(13) C14 0.0370(17) 0.0337(16) 0.0231(14) 0.0081(12) 0.0082(12) -0.0077(13) C15 0.0329(16) 0.0260(15) 0.0212(14) 0.0047(11) -0.0007(12) -0.0016(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 Pd N10 2.029(2) . ? Pd N2 2.063(2) . ? Pd Cl1 2.2748(7) . ? Pd Cl2 2.2846(8) . ? O C2 1.211(3) . ? N1 N2 1.374(3) . ? N1 C2 1.389(3) . ? N1 C3 1.490(3) . ? N2 C1 1.341(3) . ? N3 N4 1.353(3) . ? N3 C2 1.373(3) . ? N3 C6 1.489(3) . ? N4 C1 1.314(3) . ? N10 C15 1.344(3) . ? N10 C11 1.348(3) . ? C1 C11 1.474(4) . ? C3 C4 1.517(4) . ? C3 C5 1.521(4) . ? C6 C8 1.512(4) . ? C6 C7 1.519(4) . ? C11 C12 1.378(4) . ? C12 C13 1.381(4) . ? C13 C14 1.382(4) . ? C14 C15 1.371(4) . ? 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 N10 Pd N2 79.63(8) . . ? N10 Pd Cl1 92.90(6) . . ? N2 Pd Cl1 172.51(6) . . ? N10 Pd Cl2 177.93(6) . . ? N2 Pd Cl2 99.93(6) . . ? Cl1 Pd Cl2 87.52(3) . . ? N2 N1 C2 121.6(2) . . ? N2 N1 C3 117.2(2) . . ? C2 N1 C3 119.8(2) . . ? C1 N2 N1 115.2(2) . . ? C1 N2 Pd 112.28(16) . . ? N1 N2 Pd 132.03(16) . . ? N4 N3 C2 124.1(2) . . ? N4 N3 C6 116.7(2) . . ? C2 N3 C6 119.2(2) . . ? C1 N4 N3 115.2(2) . . ? C15 N10 C11 118.3(2) . . ? C15 N10 Pd 127.00(19) . . ? C11 N10 Pd 114.70(18) . . ? N4 C1 N2 127.2(2) . . ? N4 C1 C11 117.1(2) . . ? N2 C1 C11 115.6(2) . . ? O C2 N3 122.5(2) . . ? O C2 N1 122.1(2) . . ? N3 C2 N1 115.4(2) . . ? N1 C3 C4 109.8(2) . . ? N1 C3 C5 111.7(2) . . ? C4 C3 C5 112.8(3) . . ? N3 C6 C8 109.0(2) . . ? N3 C6 C7 110.1(2) . . ? C8 C6 C7 112.9(3) . . ? N10 C11 C12 122.3(2) . . ? N10 C11 C1 114.5(2) . . ? C12 C11 C1 123.1(2) . . ? C11 C12 C13 119.0(2) . . ? C12 C13 C14 118.8(3) . . ? C15 C14 C13 119.4(3) . . ? N10 C15 C14 122.3(3) . . ? 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 C2 N1 N2 C1 12.7(3) . . . . ? C3 N1 N2 C1 -154.3(2) . . . . ? C2 N1 N2 Pd -158.5(2) . . . . ? C3 N1 N2 Pd 34.5(3) . . . . ? N10 Pd N2 C1 16.33(17) . . . . ? Cl1 Pd N2 C1 12.4(6) . . . . ? Cl2 Pd N2 C1 -161.61(16) . . . . ? N10 Pd N2 N1 -172.2(2) . . . . ? Cl1 Pd N2 N1 -176.2(3) . . . . ? Cl2 Pd N2 N1 9.8(2) . . . . ? C2 N3 N4 C1 7.6(4) . . . . ? C6 N3 N4 C1 -173.3(2) . . . . ? N2 Pd N10 C15 170.4(2) . . . . ? Cl1 Pd N10 C15 -10.1(2) . . . . ? Cl2 Pd N10 C15 -111.7(17) . . . . ? N2 Pd N10 C11 -11.58(17) . . . . ? Cl1 Pd N10 C11 167.90(17) . . . . ? Cl2 Pd N10 C11 66.3(18) . . . . ? N3 N4 C1 N2 -3.1(4) . . . . ? N3 N4 C1 C11 -178.3(2) . . . . ? N1 N2 C1 N4 -6.7(4) . . . . ? Pd N2 C1 N4 166.3(2) . . . . ? N1 N2 C1 C11 168.6(2) . . . . ? Pd N2 C1 C11 -18.4(3) . . . . ? N4 N3 C2 O 176.2(3) . . . . ? C6 N3 C2 O -2.8(4) . . . . ? N4 N3 C2 N1 -1.9(4) . . . . ? C6 N3 C2 N1 179.1(2) . . . . ? N2 N1 C2 O 173.1(2) . . . . ? C3 N1 C2 O -20.3(4) . . . . ? N2 N1 C2 N3 -8.8(4) . . . . ? C3 N1 C2 N3 157.9(2) . . . . ? N2 N1 C3 C4 108.9(3) . . . . ? C2 N1 C3 C4 -58.4(3) . . . . ? N2 N1 C3 C5 -125.2(3) . . . . ? C2 N1 C3 C5 67.6(3) . . . . ? N4 N3 C6 C8 87.1(3) . . . . ? C2 N3 C6 C8 -93.8(3) . . . . ? N4 N3 C6 C7 -37.2(3) . . . . ? C2 N3 C6 C7 141.9(3) . . . . ? C15 N10 C11 C12 0.0(4) . . . . ? Pd N10 C11 C12 -178.2(2) . . . . ? C15 N10 C11 C1 -176.5(2) . . . . ? Pd N10 C11 C1 5.3(3) . . . . ? N4 C1 C11 N10 -175.1(2) . . . . ? N2 C1 C11 N10 9.1(3) . . . . ? N4 C1 C11 C12 8.4(4) . . . . ? N2 C1 C11 C12 -167.4(2) . . . . ? N10 C11 C12 C13 -0.3(4) . . . . ? C1 C11 C12 C13 176.0(2) . . . . ? C11 C12 C13 C14 -0.1(4) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C11 N10 C15 C14 0.7(4) . . . . ? Pd N10 C15 C14 178.6(2) . . . . ? C13 C14 C15 N10 -1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.331 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.087 # Attachment '- vic0532.cif' data_vic0532 _database_code_depnum_ccdc_archive 'CCDC 787981' #TrackingRef '- vic0532.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H18 Cl2 N5 O Pt' _chemical_formula_sum 'C13 H18 Cl2 N5 O Pt' _chemical_formula_weight 526.31 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' Pt Pt -1.7033 8.3905 '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/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.8844(13) _cell_length_b 17.179(2) _cell_length_c 10.0680(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.072(2) _cell_angle_gamma 90.00 _cell_volume 1642.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5735 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 26.23 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 8.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3138 _exptl_absorpt_correction_T_max 0.5022 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12633 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.31 _reflns_number_total 3329 _reflns_number_gt 2666 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0282P)^2^+0.6996P] 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 3329 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Pt Pt -0.03849(2) 0.432604(11) -0.13423(2) 0.02532(8) Uani 1 1 d . . . Cl1 Cl -0.16499(16) 0.51307(9) -0.30292(16) 0.0454(4) Uani 1 1 d . . . Cl2 Cl -0.24155(15) 0.41497(9) -0.07046(18) 0.0414(4) Uani 1 1 d . . . O O 0.1529(4) 0.2485(3) 0.3047(4) 0.0412(10) Uani 1 1 d . . . N1 N 0.0696(4) 0.3121(3) 0.1022(4) 0.0268(10) Uani 1 1 d . . . N2 N 0.0942(4) 0.3652(3) 0.0089(4) 0.0239(9) Uani 1 1 d . . . N3 N 0.3082(4) 0.3143(3) 0.2205(5) 0.0282(10) Uani 1 1 d . . . N4 N 0.3391(4) 0.3558(3) 0.1191(4) 0.0262(10) Uani 1 1 d . . . N10 N 0.1428(5) 0.4510(2) -0.1854(5) 0.0263(10) Uani 1 1 d . . . C1 C 0.2321(5) 0.3801(3) 0.0202(5) 0.0238(11) Uani 1 1 d . . . C2 C 0.1754(5) 0.2893(3) 0.2155(5) 0.0265(12) Uani 1 1 d . . . C3 C -0.0613(5) 0.2645(3) 0.0564(6) 0.0297(12) Uani 1 1 d . . . H3 H -0.1188 0.2866 -0.0334 0.036 Uiso 1 1 calc R . . C4 C -0.0247(7) 0.1805(3) 0.0291(7) 0.0449(16) Uani 1 1 d . . . H4A H 0.0307 0.1802 -0.0379 0.054 Uiso 1 1 calc R . . H4B H -0.1116 0.1508 -0.0079 0.054 Uiso 1 1 calc R . . H4C H 0.0303 0.1567 0.1158 0.054 Uiso 1 1 calc R . . C5 C -0.1484(6) 0.2702(4) 0.1579(7) 0.0471(17) Uani 1 1 d . . . H5A H -0.1668 0.3251 0.1731 0.056 Uiso 1 1 calc R . . H5B H -0.0969 0.2464 0.2459 0.056 Uiso 1 1 calc R . . H5C H -0.2379 0.2429 0.1207 0.056 Uiso 1 1 calc R . . C6 C 0.4285(6) 0.2949(4) 0.3422(6) 0.0338(13) Uani 1 1 d . . . H6 H 0.4017 0.2483 0.3890 0.041 Uiso 1 1 calc R . . C7 C 0.5552(7) 0.2739(5) 0.2946(7) 0.057(2) Uani 1 1 d . . . H7A H 0.5310 0.2314 0.2273 0.068 Uiso 1 1 calc R . . H7B H 0.6318 0.2573 0.3741 0.068 Uiso 1 1 calc R . . H7C H 0.5854 0.3194 0.2515 0.068 Uiso 1 1 calc R . . C8 C 0.4554(7) 0.3615(4) 0.4429(7) 0.0532(18) Uani 1 1 d . . . H8A H 0.3689 0.3735 0.4684 0.064 Uiso 1 1 calc R . . H8B H 0.4849 0.4073 0.4001 0.064 Uiso 1 1 calc R . . H8C H 0.5298 0.3470 0.5259 0.064 Uiso 1 1 calc R . . C11 C 0.2581(5) 0.4240(3) -0.0936(5) 0.0235(11) Uani 1 1 d . . . C12 C 0.3905(6) 0.4335(3) -0.1122(6) 0.0302(12) Uani 1 1 d . . . H12 H 0.4711 0.4136 -0.0458 0.036 Uiso 1 1 calc R . . C13 C 0.4047(6) 0.4715(4) -0.2259(6) 0.0384(14) Uani 1 1 d . . . H13 H 0.4948 0.4783 -0.2407 0.046 Uiso 1 1 calc R . . C14 C 0.2870(6) 0.4996(3) -0.3184(6) 0.0406(15) Uani 1 1 d . . . H14 H 0.2948 0.5263 -0.3986 0.049 Uiso 1 1 calc R . . C15 C 0.1568(6) 0.4896(3) -0.2964(6) 0.0333(13) Uani 1 1 d . . . H15 H 0.0757 0.5103 -0.3609 0.040 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 Pt 0.01970(11) 0.02506(12) 0.02609(12) -0.00246(9) -0.00219(8) 0.00450(9) Cl1 0.0415(9) 0.0483(9) 0.0362(9) 0.0050(7) -0.0064(7) 0.0205(7) Cl2 0.0212(7) 0.0425(9) 0.0587(10) -0.0105(7) 0.0081(7) 0.0034(6) O 0.033(2) 0.055(3) 0.035(2) 0.018(2) 0.0062(19) 0.000(2) N1 0.021(2) 0.032(3) 0.023(2) 0.001(2) -0.0010(18) -0.0003(19) N2 0.018(2) 0.028(2) 0.025(2) 0.0001(19) 0.0047(18) -0.0001(18) N3 0.014(2) 0.039(3) 0.027(2) 0.008(2) -0.0008(18) 0.0057(19) N4 0.022(2) 0.027(2) 0.028(2) 0.0108(19) 0.0047(19) 0.0018(18) N10 0.026(2) 0.024(2) 0.024(2) -0.0008(18) -0.0017(19) 0.0005(18) C1 0.019(2) 0.024(3) 0.027(3) 0.001(2) 0.004(2) 0.003(2) C2 0.022(3) 0.031(3) 0.025(3) 0.006(2) 0.003(2) 0.001(2) C3 0.021(3) 0.038(3) 0.028(3) -0.003(2) 0.002(2) -0.007(2) C4 0.050(4) 0.036(4) 0.043(4) 0.003(3) 0.004(3) -0.003(3) C5 0.027(3) 0.078(5) 0.037(4) -0.001(3) 0.010(3) -0.012(3) C6 0.028(3) 0.039(3) 0.030(3) 0.015(3) 0.002(2) 0.004(3) C7 0.038(4) 0.088(6) 0.040(4) 0.005(4) 0.002(3) 0.031(4) C8 0.046(4) 0.062(5) 0.039(4) 0.003(3) -0.010(3) 0.018(3) C11 0.022(3) 0.020(3) 0.025(3) -0.001(2) 0.000(2) 0.001(2) C12 0.025(3) 0.032(3) 0.033(3) -0.001(3) 0.007(2) -0.001(2) C13 0.030(3) 0.046(4) 0.040(4) 0.004(3) 0.010(3) -0.004(3) C14 0.047(4) 0.042(4) 0.033(3) 0.008(3) 0.010(3) -0.004(3) C15 0.037(3) 0.030(3) 0.027(3) 0.006(2) -0.002(2) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N10 2.022(5) . ? Pt N2 2.023(4) . ? Pt Cl1 2.2766(14) . ? Pt Cl2 2.2905(15) . ? O C2 1.209(6) . ? N1 C2 1.374(6) . ? N1 N2 1.378(6) . ? N1 C3 1.492(6) . ? N2 C1 1.360(6) . ? N3 N4 1.348(6) . ? N3 C2 1.368(6) . ? N3 C6 1.490(6) . ? N4 C1 1.304(6) . ? N10 C11 1.336(7) . ? N10 C15 1.339(7) . ? C1 C11 1.453(7) . ? C3 C5 1.511(8) . ? C3 C4 1.531(8) . ? C6 C8 1.503(9) . ? C6 C7 1.503(8) . ? C11 C12 1.382(7) . ? C12 C13 1.359(8) . ? C13 C14 1.362(8) . ? C14 C15 1.376(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 N10 Pt N2 79.94(17) . . ? N10 Pt Cl1 93.31(13) . . ? N2 Pt Cl1 173.22(12) . . ? N10 Pt Cl2 178.03(13) . . ? N2 Pt Cl2 99.80(12) . . ? Cl1 Pt Cl2 86.93(6) . . ? C2 N1 N2 121.1(4) . . ? C2 N1 C3 119.7(4) . . ? N2 N1 C3 117.0(4) . . ? C1 N2 N1 115.4(4) . . ? C1 N2 Pt 112.9(3) . . ? N1 N2 Pt 131.5(3) . . ? N4 N3 C2 123.6(4) . . ? N4 N3 C6 116.4(4) . . ? C2 N3 C6 119.9(4) . . ? C1 N4 N3 116.2(4) . . ? C11 N10 C15 118.9(5) . . ? C11 N10 Pt 114.6(4) . . ? C15 N10 Pt 126.4(4) . . ? N4 C1 N2 125.9(5) . . ? N4 C1 C11 119.0(4) . . ? N2 C1 C11 115.1(4) . . ? O C2 N3 121.8(5) . . ? O C2 N1 121.9(5) . . ? N3 C2 N1 116.4(5) . . ? N1 C3 C5 111.3(5) . . ? N1 C3 C4 110.2(5) . . ? C5 C3 C4 112.9(5) . . ? N3 C6 C8 109.7(5) . . ? N3 C6 C7 109.7(5) . . ? C8 C6 C7 112.9(5) . . ? N10 C11 C12 121.6(5) . . ? N10 C11 C1 114.9(4) . . ? C12 C11 C1 123.3(5) . . ? C13 C12 C11 119.6(5) . . ? C12 C13 C14 118.6(6) . . ? C13 C14 C15 120.4(6) . . ? N10 C15 C14 120.9(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 C2 N1 N2 C1 13.2(7) . . . . ? C3 N1 N2 C1 -150.1(5) . . . . ? C2 N1 N2 Pt -161.1(4) . . . . ? C3 N1 N2 Pt 35.7(6) . . . . ? N10 Pt N2 C1 14.5(3) . . . . ? Cl1 Pt N2 C1 9.4(13) . . . . ? Cl2 Pt N2 C1 -163.5(3) . . . . ? N10 Pt N2 N1 -171.1(5) . . . . ? Cl1 Pt N2 N1 -176.2(8) . . . . ? Cl2 Pt N2 N1 10.8(4) . . . . ? C2 N3 N4 C1 8.1(7) . . . . ? C6 N3 N4 C1 -172.6(5) . . . . ? N2 Pt N10 C11 -10.8(3) . . . . ? Cl1 Pt N10 C11 168.6(3) . . . . ? Cl2 Pt N10 C11 72(4) . . . . ? N2 Pt N10 C15 172.3(5) . . . . ? Cl1 Pt N10 C15 -8.3(4) . . . . ? Cl2 Pt N10 C15 -105(4) . . . . ? N3 N4 C1 N2 -2.1(8) . . . . ? N3 N4 C1 C11 -178.8(4) . . . . ? N1 N2 C1 N4 -8.2(8) . . . . ? Pt N2 C1 N4 167.2(4) . . . . ? N1 N2 C1 C11 168.7(4) . . . . ? Pt N2 C1 C11 -16.0(6) . . . . ? N4 N3 C2 O 175.8(5) . . . . ? C6 N3 C2 O -3.5(8) . . . . ? N4 N3 C2 N1 -3.1(8) . . . . ? C6 N3 C2 N1 177.6(5) . . . . ? N2 N1 C2 O 173.1(5) . . . . ? C3 N1 C2 O -24.1(8) . . . . ? N2 N1 C2 N3 -8.0(7) . . . . ? C3 N1 C2 N3 154.8(5) . . . . ? C2 N1 C3 C5 69.9(7) . . . . ? N2 N1 C3 C5 -126.6(5) . . . . ? C2 N1 C3 C4 -56.1(6) . . . . ? N2 N1 C3 C4 107.4(5) . . . . ? N4 N3 C6 C8 84.8(6) . . . . ? C2 N3 C6 C8 -95.9(6) . . . . ? N4 N3 C6 C7 -39.8(7) . . . . ? C2 N3 C6 C7 139.5(6) . . . . ? C15 N10 C11 C12 -1.4(8) . . . . ? Pt N10 C11 C12 -178.6(4) . . . . ? C15 N10 C11 C1 -177.5(5) . . . . ? Pt N10 C11 C1 5.3(6) . . . . ? N4 C1 C11 N10 -175.7(5) . . . . ? N2 C1 C11 N10 7.2(7) . . . . ? N4 C1 C11 C12 8.3(8) . . . . ? N2 C1 C11 C12 -168.8(5) . . . . ? N10 C11 C12 C13 0.3(8) . . . . ? C1 C11 C12 C13 176.1(5) . . . . ? C11 C12 C13 C14 0.4(9) . . . . ? C12 C13 C14 C15 0.0(10) . . . . ? C11 N10 C15 C14 1.8(8) . . . . ? Pt N10 C15 C14 178.6(4) . . . . ? C13 C14 C15 N10 -1.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.866 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.156 # Attachment '- vic0543.cif' data_vic0543 _database_code_depnum_ccdc_archive 'CCDC 787982' #TrackingRef '- vic0543.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H19 Cl2 N6 O Pd' _chemical_formula_sum 'C12 H19 Cl2 N6 O Pd' _chemical_formula_weight 440.63 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 '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 11.0168(6) _cell_length_b 10.3045(6) _cell_length_c 14.9488(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.9769(8) _cell_angle_gamma 90.00 _cell_volume 1684.46(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6731 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.7730 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13143 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3453 _reflns_number_gt 3234 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0222P)^2^+1.1961P] 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 3453 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0498 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Pd Pd 0.117499(12) 0.144206(13) -0.003185(9) 0.02477(6) Uani 1 1 d . . . Cl1 Cl 0.06179(6) 0.27243(6) -0.12417(4) 0.04697(14) Uani 1 1 d . . . Cl2 Cl 0.24566(5) 0.03317(5) -0.08610(3) 0.03793(12) Uani 1 1 d . . . O O 0.28347(15) -0.20973(16) 0.25291(12) 0.0481(4) Uani 1 1 d . . . N1 N 0.22895(14) -0.04685(15) 0.15262(11) 0.0268(3) Uani 1 1 d . . . N2 N 0.14472(13) 0.04498(14) 0.12027(10) 0.0224(3) Uani 1 1 d . . . N3 N 0.12237(14) -0.08243(15) 0.27650(10) 0.0280(3) Uani 1 1 d . . . N4 N 0.04716(14) 0.01905(15) 0.25328(10) 0.0262(3) Uani 1 1 d . . . N11 N -0.00108(14) 0.23488(15) 0.06550(11) 0.0291(3) Uani 1 1 d . . . N12 N -0.10885(14) 0.24123(16) 0.17979(12) 0.0324(4) Uani 1 1 d . . . C1 C 0.05962(15) 0.07281(17) 0.17562(12) 0.0227(3) Uani 1 1 d . . . C2 C 0.21512(18) -0.12088(19) 0.22876(14) 0.0309(4) Uani 1 1 d . . . C3 C 0.35279(16) -0.03866(19) 0.12185(13) 0.0287(4) Uani 1 1 d . . . H3 H 0.3488 0.0298 0.0742 0.034 Uiso 1 1 calc R . . C4 C 0.44573(19) 0.0060(2) 0.19938(15) 0.0390(5) Uani 1 1 d . . . H4A H 0.4177 0.0870 0.2243 0.047 Uiso 1 1 calc R . . H4B H 0.5249 0.0203 0.1773 0.047 Uiso 1 1 calc R . . H4C H 0.4545 -0.0608 0.2464 0.047 Uiso 1 1 calc R . . C5 C 0.3883(2) -0.1648(2) 0.07931(17) 0.0435(5) Uani 1 1 d . . . H5A H 0.3261 -0.1876 0.0292 0.052 Uiso 1 1 calc R . . H5B H 0.3940 -0.2341 0.1245 0.052 Uiso 1 1 calc R . . H5C H 0.4676 -0.1541 0.0568 0.052 Uiso 1 1 calc R . . C6 C 0.1124(2) -0.1415(2) 0.36546(14) 0.0377(5) Uani 1 1 d . . . H6 H 0.1472 -0.2311 0.3655 0.045 Uiso 1 1 calc R . . C7 C -0.0206(3) -0.1523(3) 0.3797(2) 0.0640(8) Uani 1 1 d . . . H7A H -0.0644 -0.2037 0.3309 0.077 Uiso 1 1 calc R . . H7B H -0.0567 -0.0653 0.3798 0.077 Uiso 1 1 calc R . . H7C H -0.0272 -0.1948 0.4375 0.077 Uiso 1 1 calc R . . C8 C 0.1885(3) -0.0636(3) 0.43751(16) 0.0569(7) Uani 1 1 d . . . H8A H 0.2735 -0.0609 0.4245 0.068 Uiso 1 1 calc R . . H8B H 0.1850 -0.1043 0.4964 0.068 Uiso 1 1 calc R . . H8C H 0.1563 0.0250 0.4384 0.068 Uiso 1 1 calc R . . C11 C -0.01910(16) 0.18014(18) 0.14265(13) 0.0262(4) Uani 1 1 d . . . C12 C -0.0818(2) 0.3361(2) 0.05144(16) 0.0406(5) Uani 1 1 d . . . H12 H -0.0899 0.3932 0.0012 0.049 Uiso 1 1 calc R . . C13 C -0.1478(2) 0.3402(2) 0.12175(17) 0.0422(5) Uani 1 1 d . . . H13 H -0.2104 0.4010 0.1297 0.051 Uiso 1 1 calc R . . C14 C -0.1636(2) 0.2061(2) 0.26031(15) 0.0424(5) Uani 1 1 d . . . H14A H -0.2161 0.1298 0.2476 0.051 Uiso 1 1 calc R . . H14B H -0.2128 0.2787 0.2782 0.051 Uiso 1 1 calc R . . H14C H -0.0989 0.1860 0.3093 0.051 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 Pd 0.02422(8) 0.02821(9) 0.02116(8) 0.00180(5) -0.00012(5) -0.00317(5) Cl1 0.0536(3) 0.0545(3) 0.0311(3) 0.0163(2) -0.0017(2) 0.0025(3) Cl2 0.0410(3) 0.0478(3) 0.0265(2) -0.0043(2) 0.0106(2) -0.0027(2) O 0.0489(9) 0.0444(9) 0.0523(10) 0.0194(8) 0.0112(8) 0.0212(8) N1 0.0230(7) 0.0288(8) 0.0289(8) 0.0029(6) 0.0045(6) 0.0057(6) N2 0.0215(7) 0.0228(7) 0.0225(7) -0.0006(6) 0.0008(6) 0.0017(6) N3 0.0300(8) 0.0285(8) 0.0256(8) 0.0044(6) 0.0032(6) 0.0004(6) N4 0.0249(7) 0.0284(8) 0.0253(7) -0.0014(6) 0.0032(6) 0.0002(6) N11 0.0255(8) 0.0290(8) 0.0315(8) 0.0029(6) -0.0022(6) 0.0034(6) N12 0.0234(8) 0.0339(8) 0.0392(9) -0.0098(7) 0.0013(7) 0.0049(6) C1 0.0203(8) 0.0234(8) 0.0240(8) -0.0040(7) 0.0009(6) -0.0011(7) C2 0.0307(10) 0.0298(9) 0.0321(10) 0.0039(8) 0.0030(8) 0.0038(8) C3 0.0224(9) 0.0331(10) 0.0311(9) -0.0041(8) 0.0053(7) 0.0034(7) C4 0.0321(11) 0.0401(11) 0.0424(12) -0.0041(9) -0.0053(9) 0.0027(9) C5 0.0395(12) 0.0446(12) 0.0473(13) -0.0152(10) 0.0085(10) 0.0086(10) C6 0.0511(13) 0.0354(11) 0.0270(10) 0.0080(8) 0.0063(9) -0.0002(9) C7 0.0627(17) 0.076(2) 0.0585(17) 0.0239(14) 0.0289(14) -0.0066(14) C8 0.0834(19) 0.0513(14) 0.0321(12) -0.0014(10) -0.0088(12) 0.0097(13) C11 0.0209(8) 0.0265(9) 0.0304(9) -0.0053(7) -0.0001(7) 0.0008(7) C12 0.0346(11) 0.0352(11) 0.0492(13) 0.0057(9) -0.0060(10) 0.0098(9) C13 0.0308(11) 0.0367(11) 0.0567(14) -0.0050(10) -0.0043(10) 0.0128(9) C14 0.0323(10) 0.0543(13) 0.0420(12) -0.0140(10) 0.0096(9) 0.0074(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N11 1.9899(16) . ? Pd N2 2.0993(14) . ? Pd Cl1 2.2636(5) . ? Pd Cl2 2.2944(5) . ? O C2 1.212(2) . ? N1 N2 1.372(2) . ? N1 C2 1.394(2) . ? N1 C3 1.494(2) . ? N2 C1 1.354(2) . ? N3 N4 1.353(2) . ? N3 C2 1.374(3) . ? N3 C6 1.479(2) . ? N4 C1 1.308(2) . ? N11 C11 1.320(2) . ? N11 C12 1.370(2) . ? N12 C11 1.347(2) . ? N12 C13 1.373(3) . ? N12 C14 1.456(3) . ? C1 C11 1.454(2) . ? C3 C5 1.519(3) . ? C3 C4 1.521(3) . ? C6 C7 1.510(4) . ? C6 C8 1.512(3) . ? C12 C13 1.349(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pd N2 78.91(6) . . ? N11 Pd Cl1 90.40(5) . . ? N2 Pd Cl1 169.31(4) . . ? N11 Pd Cl2 176.92(5) . . ? N2 Pd Cl2 101.56(4) . . ? Cl1 Pd Cl2 89.10(2) . . ? N2 N1 C2 121.95(15) . . ? N2 N1 C3 117.16(14) . . ? C2 N1 C3 118.48(15) . . ? C1 N2 N1 114.81(14) . . ? C1 N2 Pd 113.47(11) . . ? N1 N2 Pd 131.63(11) . . ? N4 N3 C2 124.09(15) . . ? N4 N3 C6 116.01(15) . . ? C2 N3 C6 119.33(16) . . ? C1 N4 N3 115.33(15) . . ? C11 N11 C12 107.18(17) . . ? C11 N11 Pd 115.33(12) . . ? C12 N11 Pd 137.13(15) . . ? C11 N12 C13 105.97(18) . . ? C11 N12 C14 128.53(18) . . ? C13 N12 C14 125.30(18) . . ? N4 C1 N2 127.40(16) . . ? N4 C1 C11 120.02(16) . . ? N2 C1 C11 112.49(15) . . ? O C2 N3 122.50(18) . . ? O C2 N1 122.08(18) . . ? N3 C2 N1 115.36(16) . . ? N1 C3 C5 111.82(16) . . ? N1 C3 C4 109.74(15) . . ? C5 C3 C4 113.20(17) . . ? N3 C6 C7 109.65(19) . . ? N3 C6 C8 109.08(18) . . ? C7 C6 C8 113.7(2) . . ? N11 C11 N12 110.86(17) . . ? N11 C11 C1 118.31(16) . . ? N12 C11 C1 130.76(18) . . ? C13 C12 N11 107.8(2) . . ? C12 C13 N12 108.21(18) . . ? 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 C2 N1 N2 C1 10.5(2) . . . . ? C3 N1 N2 C1 -151.59(15) . . . . ? C2 N1 N2 Pd -165.78(14) . . . . ? C3 N1 N2 Pd 32.2(2) . . . . ? N11 Pd N2 C1 10.65(12) . . . . ? Cl1 Pd N2 C1 10.0(3) . . . . ? Cl2 Pd N2 C1 -166.25(11) . . . . ? N11 Pd N2 N1 -173.06(16) . . . . ? Cl1 Pd N2 N1 -173.68(16) . . . . ? Cl2 Pd N2 N1 10.05(15) . . . . ? C2 N3 N4 C1 6.7(3) . . . . ? C6 N3 N4 C1 178.00(16) . . . . ? N2 Pd N11 C11 -10.14(13) . . . . ? Cl1 Pd N11 C11 169.75(13) . . . . ? Cl2 Pd N11 C11 89.1(9) . . . . ? N2 Pd N11 C12 177.8(2) . . . . ? Cl1 Pd N11 C12 -2.3(2) . . . . ? Cl2 Pd N11 C12 -83.0(9) . . . . ? N3 N4 C1 N2 -5.6(3) . . . . ? N3 N4 C1 C11 178.12(15) . . . . ? N1 N2 C1 N4 -2.7(3) . . . . ? Pd N2 C1 N4 174.29(14) . . . . ? N1 N2 C1 C11 173.83(14) . . . . ? Pd N2 C1 C11 -9.22(18) . . . . ? N4 N3 C2 O 177.59(19) . . . . ? C6 N3 C2 O 6.6(3) . . . . ? N4 N3 C2 N1 0.4(3) . . . . ? C6 N3 C2 N1 -170.62(17) . . . . ? N2 N1 C2 O 173.38(19) . . . . ? C3 N1 C2 O -24.8(3) . . . . ? N2 N1 C2 N3 -9.4(3) . . . . ? C3 N1 C2 N3 152.41(17) . . . . ? N2 N1 C3 C5 -124.73(18) . . . . ? C2 N1 C3 C5 72.6(2) . . . . ? N2 N1 C3 C4 108.80(18) . . . . ? C2 N1 C3 C4 -53.9(2) . . . . ? N4 N3 C6 C7 42.0(3) . . . . ? C2 N3 C6 C7 -146.3(2) . . . . ? N4 N3 C6 C8 -83.1(2) . . . . ? C2 N3 C6 C8 88.6(2) . . . . ? C12 N11 C11 N12 0.2(2) . . . . ? Pd N11 C11 N12 -174.17(12) . . . . ? C12 N11 C11 C1 -177.20(16) . . . . ? Pd N11 C11 C1 8.5(2) . . . . ? C13 N12 C11 N11 -0.3(2) . . . . ? C14 N12 C11 N11 174.63(19) . . . . ? C13 N12 C11 C1 176.62(19) . . . . ? C14 N12 C11 C1 -8.4(3) . . . . ? N4 C1 C11 N11 177.69(16) . . . . ? N2 C1 C11 N11 0.9(2) . . . . ? N4 C1 C11 N12 0.9(3) . . . . ? N2 C1 C11 N12 -175.84(18) . . . . ? C11 N11 C12 C13 0.1(2) . . . . ? Pd N11 C12 C13 172.52(16) . . . . ? N11 C12 C13 N12 -0.2(3) . . . . ? C11 N12 C13 C12 0.3(2) . . . . ? C14 N12 C13 C12 -174.8(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.450 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.069