data_k1163 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C16 H17 N3 O Pd' _chemical_formula_weight 373.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0923(12) _cell_length_b 10.9151(14) _cell_length_c 15.353(2) _cell_angle_alpha 84.402(2) _cell_angle_beta 88.593(2) _cell_angle_gamma 89.179(2) _cell_volume 1515.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4697 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5764 _exptl_absorpt_correction_T_max 0.9935 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (1271 frames at 6 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.30\% in omega and an exposure time of 25 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 4697 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be -1, and the space group was shown to be either P1 or P-1. The asymmetric unit consists of two independent molecules. ; _publ_section_figure_captions ; Fig. 1 -- View of one molecule showing the atom numbering scheme. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens as spheres of arbitrary diameter. To get atom numbers for the other molecule add 1 to Pd and O, 3 to N, and 16 to C numbers shown. Fig. 2 -- Isotropic view of the molecule. Fig. 3 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(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-Nonius APEX II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 6963 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5157 _reflns_number_gt 4156 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v6.12 (G.M. Sheldrick, 2001)' _computing_structure_refinement 'SHELXL v6.12 (G.M. Sheldrick, 2001)' _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^ > 4sigma(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^)+(0.0540P)^2^+6.7865P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 5157 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.008 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 0.23417(4) 0.76928(4) 0.92419(3) 0.03301(15) Uani 1 1 d . . . O1 O 0.0290(4) 0.6328(4) 1.1505(3) 0.0409(10) Uani 1 1 d . . . N1 N 0.0672(5) 0.8890(4) 0.8694(3) 0.0316(10) Uani 1 1 d . . . N2 N 0.0815(5) 0.7402(4) 1.0168(3) 0.0294(10) Uani 1 1 d . . . N3 N 0.4000(5) 0.7957(5) 0.8354(4) 0.0440(12) Uani 1 1 d . . . C1 C 0.0651(7) 0.9609(6) 0.7950(4) 0.0428(14) Uani 1 1 d . . . H1 H 0.1462 0.9580 0.7561 0.051 Uiso 1 1 calc R . . C2 C -0.0508(8) 1.0402(6) 0.7715(4) 0.0502(17) Uani 1 1 d . . . H2 H -0.0477 1.0895 0.7177 0.060 Uiso 1 1 calc R . . C3 C -0.1690(7) 1.0461(6) 0.8271(4) 0.0461(16) Uani 1 1 d . . . H3 H -0.2473 1.1009 0.8124 0.055 Uiso 1 1 calc R . . C4 C -0.1741(6) 0.9694(5) 0.9073(4) 0.0363(13) Uani 1 1 d . . . C5 C -0.2923(6) 0.9665(6) 0.9687(4) 0.0432(15) Uani 1 1 d . . . H5 H -0.3751 1.0176 0.9575 0.052 Uiso 1 1 calc R . . C6 C -0.2872(7) 0.8908(6) 1.0432(4) 0.0442(15) Uani 1 1 d . . . H6 H -0.3679 0.8894 1.0827 0.053 Uiso 1 1 calc R . . C7 C -0.1657(6) 0.8139(5) 1.0641(4) 0.0353(13) Uani 1 1 d . . . H7 H -0.1656 0.7633 1.1172 0.042 Uiso 1 1 calc R . . C8 C -0.0461(6) 0.8122(5) 1.0068(3) 0.0278(11) Uani 1 1 d . . . C9 C -0.0517(6) 0.8918(5) 0.9266(3) 0.0281(11) Uani 1 1 d . . . C10 C 0.1093(6) 0.6553(5) 1.0851(3) 0.0302(11) Uani 1 1 d . . . C11 C 0.2517(6) 0.5827(5) 1.0711(4) 0.0347(12) Uani 1 1 d . . . C12 C 0.3544(7) 0.6547(7) 1.0057(5) 0.0536(18) Uani 1 1 d . . . H12A H 0.4115 0.5978 0.9722 0.064 Uiso 1 1 calc R . . H12B H 0.4233 0.7021 1.0369 0.064 Uiso 1 1 calc R . . C13 C 0.2045(8) 0.4643(7) 1.0317(5) 0.0533(17) Uani 1 1 d . . . H13A H 0.1342 0.4201 1.0711 0.080 Uiso 1 1 calc R . . H13B H 0.2903 0.4123 1.0237 0.080 Uiso 1 1 calc R . . H13C H 0.1597 0.4864 0.9755 0.080 Uiso 1 1 calc R . . C14 C 0.3240(8) 0.5453(8) 1.1576(5) 0.0592(19) Uani 1 1 d . . . H14A H 0.3536 0.6183 1.1836 0.089 Uiso 1 1 calc R . . H14B H 0.4100 0.4943 1.1479 0.089 Uiso 1 1 calc R . . H14C H 0.2549 0.4992 1.1968 0.089 Uiso 1 1 calc R . . C15 C 0.4997(7) 0.8090(6) 0.7897(4) 0.0391(14) Uani 1 1 d . . . C16 C 0.6275(7) 0.8236(7) 0.7311(5) 0.0507(17) Uani 1 1 d . . . H16A H 0.6377 0.9097 0.7097 0.071 Uiso 1 1 calc R . . H16B H 0.6152 0.7753 0.6821 0.071 Uiso 1 1 calc R . . H16C H 0.7150 0.7955 0.7625 0.071 Uiso 1 1 calc R . . Pd2 Pd 0.54981(4) 0.65066(4) 0.53622(3) 0.02979(14) Uani 1 1 d . . . O2 O 0.3344(5) 0.8910(5) 0.3639(3) 0.0581(13) Uani 1 1 d . . . N4 N 0.3819(5) 0.6161(4) 0.6338(3) 0.0338(10) Uani 1 1 d . . . N5 N 0.3957(5) 0.7634(4) 0.4856(3) 0.0308(10) Uani 1 1 d . . . N6 N 0.7130(6) 0.5365(5) 0.5836(3) 0.0393(11) Uani 1 1 d . . . C17 C 0.3805(8) 0.5396(6) 0.7063(4) 0.0445(15) Uani 1 1 d . . . H17 H 0.4652 0.4919 0.7199 0.053 Uiso 1 1 calc R . . C18 C 0.2585(10) 0.5272(7) 0.7632(5) 0.059(2) Uani 1 1 d . . . H18 H 0.2622 0.4728 0.8145 0.071 Uiso 1 1 calc R . . C19 C 0.1357(9) 0.5931(7) 0.7442(5) 0.058(2) Uani 1 1 d . . . H19 H 0.0533 0.5847 0.7824 0.070 Uiso 1 1 calc R . . C20 C 0.1296(7) 0.6751(6) 0.6673(5) 0.0466(16) Uani 1 1 d . . . C21 C 0.0069(7) 0.7478(8) 0.6424(6) 0.061(2) Uani 1 1 d . . . H21 H -0.0787 0.7441 0.6781 0.073 Uiso 1 1 calc R . . C22 C 0.0110(7) 0.8230(7) 0.5675(6) 0.060(2) Uani 1 1 d . . . H22 H -0.0731 0.8704 0.5520 0.072 Uiso 1 1 calc R . . C23 C 0.1378(7) 0.8337(6) 0.5107(5) 0.0460(15) Uani 1 1 d . . . H23 H 0.1370 0.8879 0.4592 0.055 Uiso 1 1 calc R . . C24 C 0.2620(6) 0.7632(5) 0.5324(4) 0.0326(12) Uani 1 1 d . . . C25 C 0.2576(6) 0.6835(5) 0.6119(4) 0.0340(12) Uani 1 1 d . . . C26 C 0.4250(7) 0.8301(5) 0.4082(4) 0.0368(13) Uani 1 1 d . . . C27 C 0.5898(7) 0.8261(6) 0.3819(4) 0.0388(13) Uani 1 1 d . . . C28 C 0.6653(7) 0.7108(6) 0.4277(4) 0.0411(14) Uani 1 1 d . . . H28A H 0.7654 0.7308 0.4432 0.049 Uiso 1 1 calc R . . H28B H 0.6716 0.6460 0.3878 0.049 Uiso 1 1 calc R . . C29 C 0.6545(7) 0.9426(6) 0.4130(4) 0.0463(15) Uani 1 1 d . . . H29A H 0.6441 0.9395 0.4762 0.069 Uiso 1 1 calc R . . H29B H 0.6024 1.0144 0.3864 0.069 Uiso 1 1 calc R . . H29C H 0.7579 0.9477 0.3961 0.069 Uiso 1 1 calc R . . C30 C 0.6062(9) 0.8301(7) 0.2822(4) 0.0578(19) Uani 1 1 d . . . H30A H 0.7098 0.8275 0.2657 0.087 Uiso 1 1 calc R . . H30B H 0.5619 0.9055 0.2555 0.087 Uiso 1 1 calc R . . H30C H 0.5573 0.7599 0.2623 0.087 Uiso 1 1 calc R . . C31 C 0.7993(7) 0.4682(6) 0.6091(4) 0.0397(14) Uani 1 1 d . . . C32 C 0.9091(8) 0.3790(7) 0.6422(5) 0.059(2) Uani 1 1 d . . . H32A H 0.9299 0.3916 0.7023 0.082 Uiso 1 1 calc R . . H32B H 0.9985 0.3894 0.6066 0.082 Uiso 1 1 calc R . . H32C H 0.8722 0.2965 0.6398 0.059 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 0.0240(2) 0.0392(3) 0.0339(3) 0.00351(19) 0.00737(17) 0.00163(17) O1 0.035(2) 0.053(3) 0.031(2) 0.0084(18) 0.0050(17) 0.0035(19) N1 0.033(2) 0.031(2) 0.031(2) 0.0000(19) 0.0005(19) -0.0030(19) N2 0.019(2) 0.035(2) 0.033(2) 0.0030(19) 0.0022(18) 0.0026(18) N3 0.029(3) 0.050(3) 0.051(3) 0.000(2) 0.010(2) 0.001(2) C1 0.051(4) 0.045(4) 0.031(3) 0.007(3) 0.002(3) -0.004(3) C2 0.054(4) 0.055(4) 0.038(3) 0.015(3) -0.007(3) -0.006(3) C3 0.048(4) 0.038(3) 0.051(4) 0.005(3) -0.023(3) 0.003(3) C4 0.037(3) 0.033(3) 0.040(3) -0.007(2) -0.010(2) 0.003(2) C5 0.025(3) 0.053(4) 0.053(4) -0.015(3) -0.007(3) 0.017(3) C6 0.027(3) 0.055(4) 0.051(4) -0.009(3) 0.010(3) 0.008(3) C7 0.033(3) 0.039(3) 0.033(3) -0.002(2) 0.007(2) 0.004(2) C8 0.026(3) 0.027(3) 0.030(3) -0.002(2) -0.001(2) 0.000(2) C9 0.026(3) 0.029(3) 0.029(3) -0.005(2) -0.001(2) -0.003(2) C10 0.028(3) 0.033(3) 0.029(3) 0.000(2) 0.000(2) -0.001(2) C11 0.030(3) 0.035(3) 0.037(3) 0.005(2) -0.002(2) 0.003(2) C12 0.031(3) 0.065(5) 0.061(4) 0.011(4) 0.004(3) 0.012(3) C13 0.045(4) 0.056(4) 0.059(4) -0.009(3) 0.002(3) 0.006(3) C14 0.043(4) 0.079(5) 0.055(4) -0.003(4) -0.012(3) 0.018(4) C15 0.033(3) 0.040(3) 0.044(3) -0.005(3) 0.008(3) 0.001(2) C16 0.038(4) 0.059(4) 0.055(4) -0.011(3) 0.020(3) -0.013(3) Pd2 0.0260(2) 0.0344(3) 0.0283(2) -0.00037(17) 0.00164(16) 0.00189(17) O2 0.051(3) 0.067(3) 0.051(3) 0.026(2) -0.015(2) -0.004(2) N4 0.033(3) 0.037(3) 0.031(2) 0.000(2) -0.0028(19) -0.006(2) N5 0.033(2) 0.029(2) 0.030(2) -0.0037(19) -0.0005(19) -0.0016(19) N6 0.036(3) 0.044(3) 0.038(3) -0.004(2) -0.001(2) 0.001(2) C17 0.057(4) 0.042(3) 0.033(3) 0.001(3) 0.003(3) -0.009(3) C18 0.083(6) 0.057(4) 0.037(4) -0.001(3) 0.015(4) -0.027(4) C19 0.058(5) 0.069(5) 0.049(4) -0.015(4) 0.024(3) -0.025(4) C20 0.039(4) 0.046(4) 0.056(4) -0.016(3) 0.014(3) -0.012(3) C21 0.030(4) 0.080(6) 0.076(5) -0.033(5) 0.011(3) -0.004(3) C22 0.025(3) 0.060(5) 0.101(6) -0.037(5) -0.003(4) 0.011(3) C23 0.042(4) 0.040(3) 0.058(4) -0.011(3) -0.013(3) 0.003(3) C24 0.028(3) 0.033(3) 0.039(3) -0.010(2) -0.003(2) -0.002(2) C25 0.030(3) 0.037(3) 0.037(3) -0.011(2) 0.004(2) -0.006(2) C26 0.041(3) 0.038(3) 0.031(3) 0.000(2) -0.004(2) -0.008(3) C27 0.045(3) 0.045(3) 0.026(3) -0.004(2) 0.008(2) -0.010(3) C28 0.043(3) 0.043(3) 0.039(3) -0.010(3) 0.013(3) -0.004(3) C29 0.045(4) 0.048(4) 0.047(4) -0.010(3) 0.003(3) -0.014(3) C30 0.077(5) 0.064(5) 0.032(3) -0.005(3) 0.008(3) -0.016(4) C31 0.037(3) 0.045(4) 0.038(3) -0.008(3) -0.005(3) 0.007(3) C32 0.058(4) 0.064(5) 0.056(4) -0.019(4) -0.019(3) 0.027(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 1.969(4) . ? Pd1 C12 2.012(6) . ? Pd1 N3 2.013(5) . ? Pd1 N1 2.124(5) . ? O1 C10 1.234(7) . ? N1 C1 1.321(7) . ? N1 C9 1.377(7) . ? N2 C10 1.357(7) . ? N2 C8 1.395(7) . ? N3 C15 1.134(8) . ? C1 C2 1.386(9) . ? C2 C3 1.361(10) . ? C3 C4 1.420(9) . ? C4 C9 1.409(8) . ? C4 C5 1.410(9) . ? C5 C6 1.345(9) . ? C6 C7 1.402(8) . ? C7 C8 1.383(8) . ? C8 C9 1.437(8) . ? C10 C11 1.529(8) . ? C11 C14 1.514(8) . ? C11 C12 1.523(9) . ? C11 C13 1.550(9) . ? C15 C16 1.453(8) . ? Pd2 N5 1.975(5) . ? Pd2 C28 2.008(6) . ? Pd2 N6 2.026(5) . ? Pd2 N4 2.124(5) . ? O2 C26 1.227(7) . ? N4 C17 1.324(8) . ? N4 C25 1.370(8) . ? N5 C26 1.354(7) . ? N5 C24 1.396(7) . ? N6 C31 1.126(8) . ? C17 C18 1.396(10) . ? C18 C19 1.342(11) . ? C19 C20 1.412(10) . ? C20 C21 1.398(11) . ? C20 C25 1.423(8) . ? C21 C22 1.346(12) . ? C22 C23 1.428(10) . ? C23 C24 1.386(8) . ? C24 C25 1.430(8) . ? C26 C27 1.544(8) . ? C27 C29 1.531(8) . ? C27 C30 1.530(8) . ? C27 C28 1.541(9) . ? C31 C32 1.449(9) . ? 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 C12 83.3(2) . . ? N2 Pd1 N3 176.3(2) . . ? C12 Pd1 N3 93.3(2) . . ? N2 Pd1 N1 80.90(17) . . ? C12 Pd1 N1 163.9(2) . . ? N3 Pd1 N1 102.4(2) . . ? C1 N1 C9 118.8(5) . . ? C1 N1 Pd1 130.7(4) . . ? C9 N1 Pd1 110.4(3) . . ? C10 N2 C8 125.6(4) . . ? C10 N2 Pd1 118.2(3) . . ? C8 N2 Pd1 116.2(3) . . ? C15 N3 Pd1 175.5(5) . . ? N1 C1 C2 123.3(6) . . ? C3 C2 C1 119.3(6) . . ? C2 C3 C4 120.0(6) . . ? C9 C4 C5 118.2(5) . . ? C9 C4 C3 117.2(6) . . ? C5 C4 C3 124.5(6) . . ? C6 C5 C4 120.3(5) . . ? C5 C6 C7 122.4(6) . . ? C8 C7 C6 120.3(5) . . ? C7 C8 N2 127.5(5) . . ? C7 C8 C9 117.6(5) . . ? N2 C8 C9 114.8(5) . . ? N1 C9 C4 121.4(5) . . ? N1 C9 C8 117.4(5) . . ? C4 C9 C8 121.2(5) . . ? O1 C10 N2 125.7(5) . . ? O1 C10 C11 122.0(5) . . ? N2 C10 C11 112.3(4) . . ? C14 C11 C12 112.5(5) . . ? C14 C11 C10 110.7(5) . . ? C12 C11 C10 110.9(5) . . ? C14 C11 C13 108.2(5) . . ? C12 C11 C13 108.6(6) . . ? C10 C11 C13 105.6(5) . . ? C11 C12 Pd1 109.1(4) . . ? N3 C15 C16 179.0(7) . . ? N5 Pd2 C28 83.8(2) . . ? N5 Pd2 N6 177.63(19) . . ? C28 Pd2 N6 93.8(2) . . ? N5 Pd2 N4 80.68(18) . . ? C28 Pd2 N4 164.5(2) . . ? N6 Pd2 N4 101.67(19) . . ? C17 N4 C25 119.1(5) . . ? C17 N4 Pd2 130.1(4) . . ? C25 N4 Pd2 110.7(4) . . ? C26 N5 C24 125.6(5) . . ? C26 N5 Pd2 118.4(4) . . ? C24 N5 Pd2 116.0(4) . . ? C31 N6 Pd2 176.4(5) . . ? N4 C17 C18 122.6(7) . . ? C19 C18 C17 119.6(7) . . ? C18 C19 C20 120.4(6) . . ? C21 C20 C19 124.4(7) . . ? C21 C20 C25 118.4(7) . . ? C19 C20 C25 117.2(6) . . ? C22 C21 C20 120.2(7) . . ? C21 C22 C23 122.8(6) . . ? C24 C23 C22 119.2(7) . . ? C23 C24 N5 126.9(6) . . ? C23 C24 C25 118.0(6) . . ? N5 C24 C25 115.0(5) . . ? N4 C25 C20 121.0(6) . . ? N4 C25 C24 117.6(5) . . ? C20 C25 C24 121.4(6) . . ? O2 C26 N5 125.3(6) . . ? O2 C26 C27 122.3(5) . . ? N5 C26 C27 112.3(5) . . ? C29 C27 C30 109.8(5) . . ? C29 C27 C28 110.1(5) . . ? C30 C27 C28 111.5(5) . . ? C29 C27 C26 105.2(5) . . ? C30 C27 C26 109.5(5) . . ? C28 C27 C26 110.6(5) . . ? C27 C28 Pd2 109.9(4) . . ? N6 C31 C32 179.3(8) . . ? 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 N1 C1 -179.4(6) . . . . ? C12 Pd1 N1 C1 169.3(9) . . . . ? N3 Pd1 N1 C1 2.2(6) . . . . ? N2 Pd1 N1 C9 4.2(4) . . . . ? C12 Pd1 N1 C9 -7.1(11) . . . . ? N3 Pd1 N1 C9 -174.1(4) . . . . ? C12 Pd1 N2 C10 -6.3(5) . . . . ? N3 Pd1 N2 C10 -28(3) . . . . ? N1 Pd1 N2 C10 176.8(4) . . . . ? C12 Pd1 N2 C8 172.3(5) . . . . ? N3 Pd1 N2 C8 150(3) . . . . ? N1 Pd1 N2 C8 -4.6(4) . . . . ? N2 Pd1 N3 C15 -5(9) . . . . ? C12 Pd1 N3 C15 -27(7) . . . . ? N1 Pd1 N3 C15 150(7) . . . . ? C9 N1 C1 C2 0.5(9) . . . . ? Pd1 N1 C1 C2 -175.6(5) . . . . ? N1 C1 C2 C3 0.3(11) . . . . ? C1 C2 C3 C4 -1.4(10) . . . . ? C2 C3 C4 C9 1.7(9) . . . . ? C2 C3 C4 C5 -178.7(6) . . . . ? C9 C4 C5 C6 -0.3(9) . . . . ? C3 C4 C5 C6 -179.9(6) . . . . ? C4 C5 C6 C7 1.0(10) . . . . ? C5 C6 C7 C8 -1.0(10) . . . . ? C6 C7 C8 N2 -178.9(6) . . . . ? C6 C7 C8 C9 0.3(8) . . . . ? C10 N2 C8 C7 1.8(9) . . . . ? Pd1 N2 C8 C7 -176.7(5) . . . . ? C10 N2 C8 C9 -177.4(5) . . . . ? Pd1 N2 C8 C9 4.1(6) . . . . ? C1 N1 C9 C4 -0.1(8) . . . . ? Pd1 N1 C9 C4 176.7(4) . . . . ? C1 N1 C9 C8 179.8(5) . . . . ? Pd1 N1 C9 C8 -3.3(6) . . . . ? C5 C4 C9 N1 179.5(5) . . . . ? C3 C4 C9 N1 -0.9(8) . . . . ? C5 C4 C9 C8 -0.5(8) . . . . ? C3 C4 C9 C8 179.1(5) . . . . ? C7 C8 C9 N1 -179.5(5) . . . . ? N2 C8 C9 N1 -0.2(7) . . . . ? C7 C8 C9 C4 0.5(8) . . . . ? N2 C8 C9 C4 179.7(5) . . . . ? C8 N2 C10 O1 -3.5(9) . . . . ? Pd1 N2 C10 O1 175.0(5) . . . . ? C8 N2 C10 C11 173.7(5) . . . . ? Pd1 N2 C10 C11 -7.8(6) . . . . ? O1 C10 C11 C14 -34.2(8) . . . . ? N2 C10 C11 C14 148.5(5) . . . . ? O1 C10 C11 C12 -159.8(6) . . . . ? N2 C10 C11 C12 22.9(7) . . . . ? O1 C10 C11 C13 82.7(7) . . . . ? N2 C10 C11 C13 -94.6(6) . . . . ? C14 C11 C12 Pd1 -151.5(5) . . . . ? C10 C11 C12 Pd1 -26.9(7) . . . . ? C13 C11 C12 Pd1 88.7(5) . . . . ? N2 Pd1 C12 C11 18.3(5) . . . . ? N3 Pd1 C12 C11 -163.1(5) . . . . ? N1 Pd1 C12 C11 29.6(13) . . . . ? Pd1 N3 C15 C16 83(42) . . . . ? N5 Pd2 N4 C17 178.9(5) . . . . ? C28 Pd2 N4 C17 173.1(8) . . . . ? N6 Pd2 N4 C17 -0.8(6) . . . . ? N5 Pd2 N4 C25 1.5(4) . . . . ? C28 Pd2 N4 C25 -4.3(10) . . . . ? N6 Pd2 N4 C25 -178.2(4) . . . . ? C28 Pd2 N5 C26 -0.9(4) . . . . ? N6 Pd2 N5 C26 -6(5) . . . . ? N4 Pd2 N5 C26 -179.3(4) . . . . ? C28 Pd2 N5 C24 176.6(4) . . . . ? N6 Pd2 N5 C24 171(4) . . . . ? N4 Pd2 N5 C24 -1.8(4) . . . . ? N5 Pd2 N6 C31 -105(9) . . . . ? C28 Pd2 N6 C31 -111(8) . . . . ? N4 Pd2 N6 C31 68(8) . . . . ? C25 N4 C17 C18 -1.9(9) . . . . ? Pd2 N4 C17 C18 -179.1(5) . . . . ? N4 C17 C18 C19 1.0(10) . . . . ? C17 C18 C19 C20 -0.2(11) . . . . ? C18 C19 C20 C21 -179.7(7) . . . . ? C18 C19 C20 C25 0.3(10) . . . . ? C19 C20 C21 C22 -179.7(7) . . . . ? C25 C20 C21 C22 0.3(10) . . . . ? C20 C21 C22 C23 -0.5(11) . . . . ? C21 C22 C23 C24 0.7(10) . . . . ? C22 C23 C24 N5 -178.8(6) . . . . ? C22 C23 C24 C25 -0.7(9) . . . . ? C26 N5 C24 C23 -2.7(9) . . . . ? Pd2 N5 C24 C23 179.9(5) . . . . ? C26 N5 C24 C25 179.1(5) . . . . ? Pd2 N5 C24 C25 1.7(6) . . . . ? C17 N4 C25 C20 2.0(8) . . . . ? Pd2 N4 C25 C20 179.7(4) . . . . ? C17 N4 C25 C24 -178.8(5) . . . . ? Pd2 N4 C25 C24 -1.1(6) . . . . ? C21 C20 C25 N4 178.8(6) . . . . ? C19 C20 C25 N4 -1.2(9) . . . . ? C21 C20 C25 C24 -0.4(9) . . . . ? C19 C20 C25 C24 179.6(6) . . . . ? C23 C24 C25 N4 -178.7(5) . . . . ? N5 C24 C25 N4 -0.3(7) . . . . ? C23 C24 C25 C20 0.6(8) . . . . ? N5 C24 C25 C20 178.9(5) . . . . ? C24 N5 C26 O2 -7.3(9) . . . . ? Pd2 N5 C26 O2 170.0(5) . . . . ? C24 N5 C26 C27 170.4(5) . . . . ? Pd2 N5 C26 C27 -12.3(6) . . . . ? O2 C26 C27 C29 81.9(7) . . . . ? N5 C26 C27 C29 -95.9(6) . . . . ? O2 C26 C27 C30 -36.1(8) . . . . ? N5 C26 C27 C30 146.1(5) . . . . ? O2 C26 C27 C28 -159.3(6) . . . . ? N5 C26 C27 C28 22.9(7) . . . . ? C29 C27 C28 Pd2 92.8(5) . . . . ? C30 C27 C28 Pd2 -145.1(5) . . . . ? C26 C27 C28 Pd2 -23.0(6) . . . . ? N5 Pd2 C28 C27 13.6(4) . . . . ? N6 Pd2 C28 C27 -166.6(4) . . . . ? N4 Pd2 C28 C27 19.4(11) . . . . ? Pd2 N6 C31 C32 -23(61) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.081 _refine_diff_density_min -1.609 _refine_diff_density_rms 0.119