# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ganesan Mani' _publ_contact_author_email 'gmani@chem.iitkgp.ernet.in, gmani04@yahoo.com' loop_ _publ_author_name G.Mani D.Ghorai S.Kumar data_compound_2.2H2O _database_code_depnum_ccdc_archive 'CCDC 869470' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H25 N5 O2' _chemical_formula_weight 319.41 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 25.795(7) _cell_length_b 4.4057(12) _cell_length_c 16.118(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1831.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19760 _cell_measurement_theta_min 0.973 _cell_measurement_theta_max 0.997 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9728 _exptl_absorpt_correction_T_max 0.9968 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-APEX-II CCD area detector' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19760 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3221 _reflns_number_gt 1372 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0674P)^2^+0.0000P] 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(4) _refine_ls_number_reflns 3221 _refine_ls_number_parameters 215 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1565 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 N1 N 0.26598(18) 0.7634(11) 0.3589(3) 0.0971(13) Uani 1 1 d . . . N2 N 0.26401(14) 0.8839(8) 0.2826(3) 0.0820(12) Uani 1 1 d . . . N3 N 0.38286(14) 0.7207(7) 0.2505(3) 0.0727(11) Uani 1 1 d . . . H3B H 0.3841 0.7019 0.3035 0.087 Uiso 1 1 calc R . . N4 N 0.50342(14) 0.5644(8) 0.2538(3) 0.0782(11) Uani 1 1 d . . . N5 N 0.50321(18) 0.6638(11) 0.3345(3) 0.0955(13) Uani 1 1 d . . . C1 C 0.2119(3) 0.4239(16) 0.4443(5) 0.175(4) Uani 1 1 d . . . H1A H 0.1808 0.3063 0.4377 0.262 Uiso 1 1 calc R . . H1B H 0.2075 0.5642 0.4893 0.262 Uiso 1 1 calc R . . H1C H 0.2404 0.2910 0.4561 0.262 Uiso 1 1 calc R . . C2 C 0.2227(3) 0.5972(14) 0.3654(5) 0.113(2) Uani 1 1 d . . . C3 C 0.1946(2) 0.6145(16) 0.2932(6) 0.122(2) Uani 1 1 d . . . H3A H 0.1632 0.5185 0.2823 0.146 Uiso 1 1 calc R . . C4 C 0.2216(2) 0.8006(12) 0.2404(5) 0.0958(18) Uani 1 1 d . . . C5 C 0.20997(19) 0.9021(17) 0.1553(5) 0.136(2) Uani 1 1 d . . . H5A H 0.2377 1.0285 0.1356 0.204 Uiso 1 1 calc R . . H5B H 0.1782 1.0155 0.1552 0.204 Uiso 1 1 calc R . . H5C H 0.2065 0.7286 0.1197 0.204 Uiso 1 1 calc R . . C6 C 0.30643(17) 1.0757(10) 0.2511(4) 0.0916(14) Uani 1 1 d . . . H6A H 0.3215 1.1881 0.2969 0.110 Uiso 1 1 calc R . . H6B H 0.2925 1.2213 0.2118 0.110 Uiso 1 1 calc R . . C7 C 0.34758(17) 0.8928(9) 0.2098(4) 0.0719(12) Uani 1 1 d . . . C8 C 0.3589(2) 0.8628(11) 0.1278(4) 0.0889(15) Uani 1 1 d . . . H8A H 0.3414 0.9581 0.0846 0.107 Uiso 1 1 calc R . . C9 C 0.4015(2) 0.6631(12) 0.1190(4) 0.0937(16) Uani 1 1 d . . . H9A H 0.4165 0.6001 0.0695 0.112 Uiso 1 1 calc R . . C10 C 0.41615(17) 0.5809(10) 0.1969(4) 0.0720(12) Uani 1 1 d . . . C11 C 0.45880(17) 0.3876(10) 0.2250(4) 0.0962(17) Uani 1 1 d . . . H11A H 0.4696 0.2572 0.1797 0.115 Uiso 1 1 calc R . . H11B H 0.4467 0.2589 0.2698 0.115 Uiso 1 1 calc R . . C12 C 0.5524(2) 0.5953(17) 0.1231(4) 0.136(2) Uani 1 1 d . . . H12A H 0.5832 0.6951 0.1038 0.204 Uiso 1 1 calc R . . H12B H 0.5232 0.6627 0.0911 0.204 Uiso 1 1 calc R . . H12C H 0.5563 0.3797 0.1171 0.204 Uiso 1 1 calc R . . C13 C 0.5439(2) 0.6700(11) 0.2117(4) 0.0861(16) Uani 1 1 d . . . C14 C 0.5708(2) 0.8405(13) 0.2666(5) 0.106(2) Uani 1 1 d . . . H14A H 0.6015 0.9436 0.2556 0.127 Uiso 1 1 calc R . . C15 C 0.5454(3) 0.8360(13) 0.3407(5) 0.1001(17) Uani 1 1 d . . . C16 C 0.5596(3) 0.9875(18) 0.4206(5) 0.168(3) Uani 1 1 d . . . H16A H 0.5345 0.9365 0.4623 0.252 Uiso 1 1 calc R . . H16B H 0.5601 1.2036 0.4128 0.252 Uiso 1 1 calc R . . H16C H 0.5933 0.9198 0.4379 0.252 Uiso 1 1 calc R . . O1 O 0.4129(3) 0.505(2) 0.4204(4) 0.180(3) Uani 0.683(5) 1 d P A 1 O2 O 0.3525(3) 0.981(2) 0.4673(5) 0.179(2) Uani 0.683(5) 1 d P A 1 O1' O 0.4352(6) 0.919(5) 0.4580(8) 0.180(3) Uani 0.317(5) 1 d P A 2 O2' O 0.3490(7) 0.587(4) 0.4528(9) 0.179(2) Uani 0.317(5) 1 d P A 2 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 N1 0.098(4) 0.071(3) 0.122(4) -0.013(3) 0.021(3) 0.004(3) N2 0.060(3) 0.059(2) 0.127(4) -0.019(3) 0.012(3) -0.004(2) N3 0.067(2) 0.055(2) 0.096(3) 0.005(2) -0.002(3) -0.0098(19) N4 0.063(3) 0.063(2) 0.109(4) 0.004(3) -0.006(3) 0.005(2) N5 0.088(3) 0.088(3) 0.110(4) 0.008(3) -0.009(3) 0.019(3) C1 0.224(8) 0.102(5) 0.198(9) 0.000(6) 0.122(7) -0.003(5) C2 0.116(6) 0.063(4) 0.160(7) -0.022(5) 0.064(5) -0.002(4) C3 0.077(4) 0.090(4) 0.198(8) -0.054(5) 0.035(5) -0.019(4) C4 0.065(3) 0.075(4) 0.147(6) -0.030(4) 0.009(4) -0.001(3) C5 0.093(4) 0.154(6) 0.161(7) -0.034(5) -0.013(4) 0.015(4) C6 0.076(3) 0.061(3) 0.137(4) -0.006(4) 0.005(3) -0.008(3) C7 0.062(3) 0.051(3) 0.102(4) -0.002(3) -0.006(3) -0.007(2) C8 0.073(3) 0.080(4) 0.114(5) 0.013(3) -0.017(3) -0.004(3) C9 0.080(3) 0.092(4) 0.110(5) -0.009(4) 0.003(4) -0.014(3) C10 0.058(3) 0.050(3) 0.108(4) -0.002(3) 0.000(3) -0.005(2) C11 0.077(3) 0.061(3) 0.151(5) -0.006(3) -0.003(3) -0.009(3) C12 0.108(4) 0.166(7) 0.134(6) -0.017(5) 0.029(4) 0.006(4) C13 0.061(3) 0.067(3) 0.130(6) 0.007(3) 0.005(4) 0.004(3) C14 0.067(3) 0.082(4) 0.169(7) 0.023(5) -0.025(4) -0.004(3) C15 0.105(5) 0.081(4) 0.115(5) -0.004(4) -0.034(5) 0.019(4) C16 0.212(7) 0.136(6) 0.157(7) -0.023(5) -0.095(6) 0.035(5) O1 0.173(5) 0.246(7) 0.120(4) 0.021(5) 0.018(4) -0.007(5) O2 0.199(6) 0.186(6) 0.153(5) -0.009(5) -0.036(4) -0.011(6) O1' 0.173(5) 0.246(7) 0.120(4) 0.021(5) 0.018(4) -0.007(5) O2' 0.199(6) 0.186(6) 0.153(5) -0.009(5) -0.036(4) -0.011(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 C2 1.339(7) . ? N1 N2 1.339(5) . ? N2 C4 1.340(6) . ? N2 C6 1.473(6) . ? N3 C7 1.354(5) . ? N3 C10 1.365(6) . ? N3 H3B 0.8600 . ? N4 C13 1.330(6) . ? N4 N5 1.372(6) . ? N4 C11 1.466(5) . ? N5 C15 1.329(7) . ? C1 C2 1.510(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.373(8) . ? C3 C4 1.372(9) . ? C3 H3A 0.9300 . ? C4 C5 1.472(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.490(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.359(6) . ? C8 C9 1.415(7) . ? C8 H8A 0.9300 . ? C9 C10 1.360(6) . ? C9 H9A 0.9300 . ? C10 C11 1.463(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.481(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.352(8) . ? C14 C15 1.363(8) . ? C14 H14A 0.9300 . ? C15 C16 1.497(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 C2 N1 N2 104.9(6) . . ? C4 N2 N1 112.9(5) . . ? C4 N2 C6 126.0(6) . . ? N1 N2 C6 121.0(5) . . ? C7 N3 C10 111.7(4) . . ? C7 N3 H3B 124.2 . . ? C10 N3 H3B 124.2 . . ? C13 N4 N5 112.1(5) . . ? C13 N4 C11 129.8(6) . . ? N5 N4 C11 117.9(5) . . ? C15 N5 N4 104.4(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.1(6) . . ? N1 C2 C1 119.8(9) . . ? C3 C2 C1 130.1(9) . . ? C4 C3 C2 106.9(6) . . ? C4 C3 H3A 126.5 . . ? C2 C3 H3A 126.5 . . ? N2 C4 C3 105.2(7) . . ? N2 C4 C5 123.8(6) . . ? C3 C4 C5 131.0(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.9(3) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C8 105.8(4) . . ? N3 C7 C6 124.4(5) . . ? C8 C7 C6 129.8(5) . . ? C7 C8 C9 108.9(5) . . ? C7 C8 H8A 125.5 . . ? C9 C8 H8A 125.5 . . ? C10 C9 C8 106.8(5) . . ? C10 C9 H9A 126.6 . . ? C8 C9 H9A 126.6 . . ? C9 C10 N3 106.8(5) . . ? C9 C10 C11 130.6(6) . . ? N3 C10 C11 122.7(6) . . ? C10 C11 N4 112.3(3) . . ? C10 C11 H11A 109.1 . . ? N4 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? N4 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 105.2(6) . . ? N4 C13 C12 122.0(6) . . ? C14 C13 C12 132.7(6) . . ? C13 C14 C15 108.5(5) . . ? C13 C14 H14A 125.7 . . ? C15 C14 H14A 125.7 . . ? N5 C15 C14 109.7(6) . . ? N5 C15 C16 121.3(8) . . ? C14 C15 C16 129.0(8) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 C2 N1 N2 C4 -0.2(5) . . . . ? C2 N1 N2 C6 -177.9(4) . . . . ? C13 N4 N5 C15 0.0(5) . . . . ? C11 N4 N5 C15 -174.8(4) . . . . ? N2 N1 C2 C3 0.4(6) . . . . ? N2 N1 C2 C1 179.7(4) . . . . ? N1 C2 C3 C4 -0.3(7) . . . . ? C1 C2 C3 C4 -179.6(5) . . . . ? N1 N2 C4 C3 0.1(5) . . . . ? C6 N2 C4 C3 177.6(4) . . . . ? N1 N2 C4 C5 179.8(5) . . . . ? C6 N2 C4 C5 -2.7(7) . . . . ? C2 C3 C4 N2 0.2(6) . . . . ? C2 C3 C4 C5 -179.5(6) . . . . ? C4 N2 C6 C7 -89.0(6) . . . . ? N1 N2 C6 C7 88.3(6) . . . . ? C10 N3 C7 C8 -0.3(5) . . . . ? C10 N3 C7 C6 -179.4(4) . . . . ? N2 C6 C7 N3 -74.9(6) . . . . ? N2 C6 C7 C8 106.3(6) . . . . ? N3 C7 C8 C9 1.1(5) . . . . ? C6 C7 C8 C9 -179.9(4) . . . . ? C7 C8 C9 C10 -1.5(6) . . . . ? C8 C9 C10 N3 1.3(5) . . . . ? C8 C9 C10 C11 -177.8(4) . . . . ? C7 N3 C10 C9 -0.7(5) . . . . ? C7 N3 C10 C11 178.5(3) . . . . ? C9 C10 C11 N4 100.1(6) . . . . ? N3 C10 C11 N4 -78.8(6) . . . . ? C13 N4 C11 C10 -88.9(6) . . . . ? N5 N4 C11 C10 84.9(6) . . . . ? N5 N4 C13 C14 0.4(5) . . . . ? C11 N4 C13 C14 174.4(4) . . . . ? N5 N4 C13 C12 -179.6(4) . . . . ? C11 N4 C13 C12 -5.6(7) . . . . ? N4 C13 C14 C15 -0.7(6) . . . . ? C12 C13 C14 C15 179.3(5) . . . . ? N4 N5 C15 C14 -0.5(6) . . . . ? N4 N5 C15 C16 -179.5(5) . . . . ? C13 C14 C15 N5 0.7(6) . . . . ? C13 C14 C15 C16 179.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O1 0.86 2.20 3.000(8) 154.4 . N3 H3B O2' 0.86 2.62 3.427(16) 156.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.102 _refine_diff_density_min -0.104 _refine_diff_density_rms 0.027 #================================================================END data_compound_3.H2O _database_code_depnum_ccdc_archive 'CCDC 869471' #TrackingRef '- CIF.cif' # start Validation Reply Form _vrf_PLAT306_compound_3.H2O ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O5 RESPONSE: Hydrogen atoms could not be located and refined properly for this lattice water molecule. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H23 N5 O2 Pd), 2H2O' _chemical_formula_sum 'C36 H50 N10 O6 Pd2' _chemical_formula_weight 931.66 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 9.7596(9) _cell_length_b 12.8135(12) _cell_length_c 16.6319(15) _cell_angle_alpha 78.720(3) _cell_angle_beta 76.803(3) _cell_angle_gamma 84.894(3) _cell_volume 1983.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23913 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 25.00 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8931 _exptl_absorpt_correction_T_max 0.9183 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-APEX-II CCD area detector' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23913 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6961 _reflns_number_gt 4886 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0513P)^2^+2.4960P] 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 6961 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6418(6) 0.0651(5) 0.6314(4) 0.0456(15) Uani 1 1 d . . . C2 C 0.7236(6) -0.0270(6) 0.5983(5) 0.070(2) Uani 1 1 d . . . H2A H 0.6634 -0.0856 0.6086 0.104 Uiso 1 1 calc R . . H2B H 0.8007 -0.0479 0.6259 0.104 Uiso 1 1 calc R . . H2C H 0.7596 -0.0069 0.5389 0.104 Uiso 1 1 calc R . . C3 C 0.6898(6) 0.1654(5) 0.6289(4) 0.0474(15) Uani 1 1 d . . . H3A H 0.7809 0.1878 0.6063 0.057 Uiso 1 1 calc R . . C4 C 0.5780(5) 0.2247(5) 0.6657(3) 0.0407(13) Uani 1 1 d . . . C5 C 0.5690(6) 0.3352(5) 0.6796(4) 0.0530(16) Uani 1 1 d . . . H5A H 0.4747 0.3529 0.7074 0.080 Uiso 1 1 calc R . . H5B H 0.5933 0.3825 0.6266 0.080 Uiso 1 1 calc R . . H5C H 0.6332 0.3425 0.7140 0.080 Uiso 1 1 calc R . . C6 C 0.3214(5) 0.1870(5) 0.7282(4) 0.0447(14) Uani 1 1 d . . . H6A H 0.2608 0.1834 0.6901 0.054 Uiso 1 1 calc R . . H6B H 0.3137 0.2591 0.7391 0.054 Uiso 1 1 calc R . . C7 C 0.2740(5) 0.1121(4) 0.8081(4) 0.0400(13) Uani 1 1 d . . . C8 C 0.2107(6) 0.1266(5) 0.8878(4) 0.0474(15) Uani 1 1 d . . . H8A H 0.1865 0.1913 0.9059 0.057 Uiso 1 1 calc R . . C9 C 0.1896(6) 0.0242(5) 0.9371(4) 0.0481(15) Uani 1 1 d . . . H9A H 0.1491 0.0086 0.9942 0.058 Uiso 1 1 calc R . . C10 C 0.2397(6) -0.0478(5) 0.8855(3) 0.0408(14) Uani 1 1 d . . . C11 C 0.2444(6) -0.1670(5) 0.8969(4) 0.0494(15) Uani 1 1 d . . . H11A H 0.3415 -0.1943 0.8873 0.059 Uiso 1 1 calc R . . H11B H 0.1985 -0.1965 0.9540 0.059 Uiso 1 1 calc R . . C12 C 0.0572(7) -0.2548(5) 0.8543(4) 0.0539(17) Uani 1 1 d . . . C13 C -0.0220(8) -0.2940(6) 0.9422(4) 0.077(2) Uani 1 1 d . . . H13A H 0.0251 -0.2745 0.9814 0.115 Uiso 1 1 calc R . . H13B H -0.0258 -0.3702 0.9516 0.115 Uiso 1 1 calc R . . H13C H -0.1160 -0.2625 0.9499 0.115 Uiso 1 1 calc R . . C14 C 0.0296(7) -0.2643(5) 0.7793(4) 0.0557(17) Uani 1 1 d . . . H14A H -0.0441 -0.2996 0.7714 0.067 Uiso 1 1 calc R . . C15 C 0.1339(6) -0.2103(4) 0.7166(4) 0.0436(14) Uani 1 1 d . . . C16 C 0.1496(7) -0.1976(5) 0.6241(4) 0.0571(17) Uani 1 1 d . . . H16A H 0.2307 -0.1572 0.5961 0.086 Uiso 1 1 calc R . . H16B H 0.0670 -0.1609 0.6083 0.086 Uiso 1 1 calc R . . H16C H 0.1613 -0.2665 0.6082 0.086 Uiso 1 1 calc R . . C17 C 0.5098(6) -0.2076(5) 0.6003(4) 0.0502(15) Uani 1 1 d . . . C18 C 0.5561(7) -0.2409(6) 0.5171(4) 0.0635(19) Uani 1 1 d . . . H18A H 0.5273 -0.1867 0.4748 0.095 Uiso 1 1 calc R . . H18B H 0.5141 -0.3064 0.5187 0.095 Uiso 1 1 calc R . . H18C H 0.6569 -0.2511 0.5042 0.095 Uiso 1 1 calc R . . C19 C 0.1503(6) 0.4576(4) 0.7617(4) 0.0412(14) Uani 1 1 d . . . C20 C 0.1483(7) 0.4462(5) 0.8525(4) 0.0567(17) Uani 1 1 d . . . H20A H 0.0711 0.4040 0.8847 0.085 Uiso 1 1 calc R . . H20B H 0.1372 0.5153 0.8679 0.085 Uiso 1 1 calc R . . H20C H 0.2352 0.4119 0.8637 0.085 Uiso 1 1 calc R . . C21 C 0.2433(6) 0.5134(4) 0.6945(4) 0.0460(14) Uani 1 1 d . . . H21A H 0.3166 0.5532 0.6973 0.055 Uiso 1 1 calc R . . C22 C 0.2061(6) 0.4982(4) 0.6227(4) 0.0447(14) Uani 1 1 d . . . C23 C 0.2685(7) 0.5400(5) 0.5326(4) 0.0630(19) Uani 1 1 d . . . H23A H 0.2178 0.5148 0.4976 0.094 Uiso 1 1 calc R . . H23B H 0.3656 0.5156 0.5196 0.094 Uiso 1 1 calc R . . H23C H 0.2624 0.6165 0.5228 0.094 Uiso 1 1 calc R . . C24 C 0.0212(6) 0.3917(5) 0.5953(4) 0.0425(14) Uani 1 1 d . . . H24A H 0.0643 0.4150 0.5366 0.051 Uiso 1 1 calc R . . H24B H -0.0761 0.4187 0.6048 0.051 Uiso 1 1 calc R . . C25 C 0.0261(5) 0.2724(4) 0.6155(3) 0.0370(13) Uani 1 1 d . . . C26 C 0.0707(6) 0.1939(5) 0.5683(4) 0.0447(14) Uani 1 1 d . . . H26A H 0.1074 0.2040 0.5107 0.054 Uiso 1 1 calc R . . C27 C 0.0504(5) 0.0961(5) 0.6233(4) 0.0474(15) Uani 1 1 d . . . H27A H 0.0719 0.0290 0.6090 0.057 Uiso 1 1 calc R . . C28 C -0.0069(5) 0.1173(4) 0.7020(4) 0.0393(13) Uani 1 1 d . . . C29 C -0.0531(6) 0.0496(5) 0.7854(4) 0.0475(15) Uani 1 1 d . . . H29A H -0.0489 -0.0243 0.7789 0.057 Uiso 1 1 calc R . . H29B H 0.0109 0.0559 0.8208 0.057 Uiso 1 1 calc R . . C30 C -0.3108(6) 0.0196(5) 0.8546(4) 0.0516(16) Uani 1 1 d . . . C31 C -0.3088(7) -0.0944(5) 0.8462(5) 0.075(2) Uani 1 1 d . . . H31A H -0.2162 -0.1159 0.8182 0.112 Uiso 1 1 calc R . . H31B H -0.3758 -0.1028 0.8140 0.112 Uiso 1 1 calc R . . H31C H -0.3329 -0.1379 0.9009 0.112 Uiso 1 1 calc R . . C32 C -0.4180(6) 0.0821(5) 0.8893(4) 0.0561(17) Uani 1 1 d . . . H32A H -0.5095 0.0619 0.9139 0.067 Uiso 1 1 calc R . . C33 C -0.3670(6) 0.1818(5) 0.8815(4) 0.0498(16) Uani 1 1 d . . . C34 C -0.4466(6) 0.2778(6) 0.9099(4) 0.067(2) Uani 1 1 d . . . H34A H -0.3846 0.3358 0.8969 0.101 Uiso 1 1 calc R . . H34B H -0.4832 0.2621 0.9694 0.101 Uiso 1 1 calc R . . H34C H -0.5230 0.2973 0.8815 0.101 Uiso 1 1 calc R . . C35 C -0.2276(7) 0.4581(6) 0.8890(5) 0.0587(18) Uani 1 1 d . . . C36 C -0.2897(8) 0.4943(7) 0.9719(5) 0.079(2) Uani 1 1 d . . . H36A H -0.2614 0.4441 1.0167 0.118 Uiso 1 1 calc R . . H36B H -0.3907 0.4987 0.9810 0.118 Uiso 1 1 calc R . . H36C H -0.2565 0.5631 0.9704 0.118 Uiso 1 1 calc R . . N1 N 0.5050(4) 0.0622(4) 0.6683(3) 0.0417(11) Uani 1 1 d . . . N2 N 0.4667(4) 0.1613(4) 0.6890(3) 0.0383(11) Uani 1 1 d . . . N3 N 0.2901(4) 0.0063(4) 0.8067(3) 0.0389(11) Uani 1 1 d . . . N4 N 0.1727(5) -0.1995(4) 0.8377(3) 0.0440(12) Uani 1 1 d . . . N5 N 0.2216(5) -0.1705(4) 0.7525(3) 0.0420(11) Uani 1 1 d . . . N6 N 0.0591(5) 0.4092(3) 0.7333(3) 0.0392(11) Uani 1 1 d . . . N7 N 0.0958(5) 0.4345(3) 0.6477(3) 0.0387(11) Uani 1 1 d . . . N8 N -0.0216(4) 0.2254(3) 0.6967(3) 0.0362(10) Uani 1 1 d . . . N9 N -0.1965(5) 0.0793(4) 0.8264(3) 0.0459(12) Uani 1 1 d . . . N10 N -0.2292(4) 0.1801(4) 0.8429(3) 0.0423(11) Uani 1 1 d . . . O1 O 0.4449(4) -0.1177(3) 0.6003(2) 0.0459(10) Uani 1 1 d . . . O2 O 0.5351(6) -0.2668(4) 0.6631(3) 0.0912(18) Uani 1 1 d . . . O3 O -0.1600(4) 0.3691(4) 0.8952(2) 0.0515(10) Uani 1 1 d . . . O4 O -0.2506(6) 0.5120(5) 0.8236(4) 0.0944(18) Uani 1 1 d . . . O5 O 0.4992(9) -0.3476(7) 0.8336(4) 0.180(4) Uani 1 1 d . . . O6 O 0.7769(7) -0.4132(5) 0.6450(4) 0.119(2) Uani 1 1 d . . . Pd1 Pd 0.36865(4) -0.05787(3) 0.70691(3) 0.03647(14) Uani 1 1 d . . . Pd2 Pd -0.08992(4) 0.29910(3) 0.79213(3) 0.03660(14) 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 0.026(3) 0.055(4) 0.052(4) -0.012(3) 0.000(3) -0.002(3) C2 0.037(4) 0.077(5) 0.095(6) -0.042(4) 0.007(4) 0.002(3) C3 0.032(3) 0.064(4) 0.044(4) -0.007(3) -0.005(3) -0.007(3) C4 0.032(3) 0.053(4) 0.038(3) -0.007(3) -0.007(2) -0.009(3) C5 0.051(4) 0.051(4) 0.053(4) -0.002(3) -0.006(3) -0.011(3) C6 0.030(3) 0.045(3) 0.059(4) -0.016(3) -0.005(3) 0.004(2) C7 0.030(3) 0.045(3) 0.047(4) -0.018(3) -0.005(3) 0.000(2) C8 0.036(3) 0.060(4) 0.047(4) -0.024(3) 0.000(3) -0.005(3) C9 0.035(3) 0.076(5) 0.032(3) -0.012(3) 0.000(3) -0.009(3) C10 0.035(3) 0.054(4) 0.033(3) -0.009(3) -0.008(2) -0.002(3) C11 0.046(4) 0.060(4) 0.040(4) -0.002(3) -0.008(3) -0.004(3) C12 0.057(4) 0.036(3) 0.060(4) -0.010(3) 0.006(3) -0.003(3) C13 0.082(5) 0.077(5) 0.052(4) 0.007(4) 0.019(4) -0.029(4) C14 0.055(4) 0.042(4) 0.072(5) -0.017(3) -0.007(4) -0.013(3) C15 0.047(4) 0.033(3) 0.049(4) -0.010(3) -0.006(3) 0.000(3) C16 0.067(4) 0.052(4) 0.056(4) -0.017(3) -0.014(3) -0.007(3) C17 0.045(4) 0.056(4) 0.045(4) -0.012(3) -0.001(3) 0.004(3) C18 0.047(4) 0.084(5) 0.065(5) -0.035(4) -0.005(3) 0.001(3) C19 0.046(3) 0.031(3) 0.048(4) -0.012(3) -0.008(3) -0.003(3) C20 0.069(4) 0.058(4) 0.053(4) -0.019(3) -0.021(3) -0.010(3) C21 0.045(3) 0.040(3) 0.054(4) -0.011(3) -0.009(3) -0.011(3) C22 0.044(3) 0.039(3) 0.048(4) -0.011(3) -0.003(3) -0.003(3) C23 0.071(5) 0.061(4) 0.054(4) -0.011(3) 0.004(4) -0.028(4) C24 0.038(3) 0.052(4) 0.038(3) -0.008(3) -0.011(3) 0.000(3) C25 0.029(3) 0.044(3) 0.037(3) -0.002(3) -0.008(2) -0.008(2) C26 0.033(3) 0.056(4) 0.047(4) -0.020(3) -0.002(3) -0.006(3) C27 0.030(3) 0.044(3) 0.072(4) -0.023(3) -0.007(3) -0.001(3) C28 0.026(3) 0.041(3) 0.051(4) -0.007(3) -0.009(3) -0.003(2) C29 0.037(3) 0.042(3) 0.064(4) -0.005(3) -0.014(3) -0.002(3) C30 0.033(3) 0.058(4) 0.059(4) 0.009(3) -0.012(3) -0.015(3) C31 0.055(4) 0.060(5) 0.104(6) 0.008(4) -0.018(4) -0.022(4) C32 0.031(3) 0.073(5) 0.055(4) 0.008(3) -0.004(3) -0.013(3) C33 0.033(3) 0.071(4) 0.042(4) -0.003(3) -0.006(3) -0.007(3) C34 0.038(4) 0.094(6) 0.067(5) -0.020(4) -0.002(3) 0.000(4) C35 0.052(4) 0.064(5) 0.061(5) -0.023(4) -0.003(4) -0.007(4) C36 0.065(5) 0.103(6) 0.076(5) -0.047(5) -0.006(4) -0.002(4) N1 0.031(3) 0.049(3) 0.044(3) -0.014(2) -0.001(2) -0.003(2) N2 0.027(2) 0.047(3) 0.042(3) -0.012(2) -0.005(2) 0.000(2) N3 0.030(2) 0.047(3) 0.037(3) -0.007(2) -0.002(2) -0.002(2) N4 0.043(3) 0.040(3) 0.042(3) 0.001(2) -0.002(2) -0.004(2) N5 0.046(3) 0.042(3) 0.035(3) -0.005(2) -0.004(2) -0.002(2) N6 0.044(3) 0.034(2) 0.040(3) -0.007(2) -0.008(2) -0.003(2) N7 0.040(3) 0.039(3) 0.036(3) -0.004(2) -0.007(2) -0.005(2) N8 0.024(2) 0.040(3) 0.043(3) -0.009(2) -0.004(2) -0.0036(19) N9 0.030(3) 0.052(3) 0.052(3) -0.002(2) -0.008(2) -0.004(2) N10 0.032(3) 0.049(3) 0.043(3) 0.001(2) -0.009(2) -0.004(2) O1 0.047(2) 0.050(3) 0.037(2) -0.0100(19) -0.0016(18) 0.002(2) O2 0.115(5) 0.087(4) 0.054(3) -0.004(3) -0.009(3) 0.047(3) O3 0.046(2) 0.065(3) 0.042(2) -0.014(2) -0.0054(19) 0.005(2) O4 0.106(4) 0.091(4) 0.072(4) -0.008(3) -0.010(3) 0.037(3) O5 0.179(7) 0.206(8) 0.090(5) 0.021(5) 0.020(5) 0.113(7) O6 0.132(5) 0.124(5) 0.090(4) -0.031(4) -0.014(4) 0.054(4) Pd1 0.0313(2) 0.0414(3) 0.0350(3) -0.00906(19) -0.00184(19) -0.00147(19) Pd2 0.0306(2) 0.0429(3) 0.0348(3) -0.00576(19) -0.00499(18) -0.00163(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(6) . ? C1 C3 1.397(8) . ? C1 C2 1.490(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.368(8) . ? C3 H3A 0.9300 . ? C4 N2 1.354(6) . ? C4 C5 1.470(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.457(6) . ? C6 C7 1.484(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.355(7) . ? C7 C8 1.370(7) . ? C8 C9 1.409(8) . ? C8 H8A 0.9300 . ? C9 C10 1.366(8) . ? C9 H9A 0.9300 . ? C10 N3 1.361(7) . ? C10 C11 1.499(8) . ? C11 N4 1.471(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.331(7) . ? C12 C14 1.364(9) . ? C12 C13 1.502(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.400(8) . ? C14 H14A 0.9300 . ? C15 N5 1.335(7) . ? C15 C16 1.488(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O2 1.225(7) . ? C17 O1 1.264(7) . ? C17 C18 1.486(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N6 1.343(7) . ? C19 C21 1.388(8) . ? C19 C20 1.484(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.378(8) . ? C21 H21A 0.9300 . ? C22 N7 1.349(7) . ? C22 C23 1.493(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N7 1.461(7) . ? C24 C25 1.499(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N8 1.360(7) . ? C25 C26 1.375(7) . ? C26 C27 1.400(8) . ? C26 H26A 0.9300 . ? C27 C28 1.370(8) . ? C27 H27A 0.9300 . ? C28 N8 1.367(7) . ? C28 C29 1.481(8) . ? C29 N9 1.463(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C32 1.351(8) . ? C30 N9 1.351(7) . ? C30 C31 1.493(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.384(8) . ? C32 H32A 0.9300 . ? C33 N10 1.352(7) . ? C33 C34 1.492(9) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 O4 1.224(8) . ? C35 O3 1.264(8) . ? C35 C36 1.518(9) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? N1 N2 1.378(6) . ? N1 Pd1 2.034(4) . ? N3 Pd1 1.964(4) . ? N4 N5 1.375(6) . ? N5 Pd1 2.040(5) . ? N6 N7 1.367(6) . ? N6 Pd2 2.058(4) . ? N8 Pd2 1.961(4) . ? N9 N10 1.368(6) . ? N10 Pd2 2.056(4) . ? O1 Pd1 2.029(4) . ? O3 Pd2 2.041(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 N1 C1 C3 109.4(5) . . ? N1 C1 C2 122.9(5) . . ? C3 C1 C2 127.8(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C1 107.4(5) . . ? C4 C3 H3A 126.3 . . ? C1 C3 H3A 126.3 . . ? N2 C4 C3 106.3(5) . . ? N2 C4 C5 123.2(5) . . ? C3 C4 C5 130.4(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.1(5) . . ? N2 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C8 109.0(5) . . ? N3 C7 C6 117.9(5) . . ? C8 C7 C6 133.0(5) . . ? C7 C8 C9 106.6(5) . . ? C7 C8 H8A 126.7 . . ? C9 C8 H8A 126.7 . . ? C10 C9 C8 107.2(5) . . ? C10 C9 H9A 126.4 . . ? C8 C9 H9A 126.4 . . ? N3 C10 C9 108.6(5) . . ? N3 C10 C11 116.9(5) . . ? C9 C10 C11 134.4(5) . . ? N4 C11 C10 109.9(5) . . ? N4 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N4 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N4 C12 C14 107.5(5) . . ? N4 C12 C13 122.6(6) . . ? C14 C12 C13 130.0(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C15 106.6(6) . . ? C12 C14 H14A 126.7 . . ? C15 C14 H14A 126.7 . . ? N5 C15 C14 109.1(5) . . ? N5 C15 C16 123.6(5) . . ? C14 C15 C16 127.3(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 O1 124.5(6) . . ? O2 C17 C18 119.6(6) . . ? O1 C17 C18 115.8(6) . . ? 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 . . ? N6 C19 C21 109.8(5) . . ? N6 C19 C20 122.4(5) . . ? C21 C19 C20 127.8(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C19 106.7(5) . . ? C22 C21 H21A 126.7 . . ? C19 C21 H21A 126.7 . . ? N7 C22 C21 106.7(5) . . ? N7 C22 C23 123.2(5) . . ? C21 C22 C23 130.1(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N7 C24 C25 110.5(4) . . ? N7 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? N7 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N8 C25 C26 108.6(5) . . ? N8 C25 C24 117.7(5) . . ? C26 C25 C24 133.7(5) . . ? C25 C26 C27 107.0(5) . . ? C25 C26 H26A 126.5 . . ? C27 C26 H26A 126.5 . . ? C28 C27 C26 107.5(5) . . ? C28 C27 H27A 126.2 . . ? C26 C27 H27A 126.2 . . ? N8 C28 C27 108.3(5) . . ? N8 C28 C29 117.9(5) . . ? C27 C28 C29 133.8(5) . . ? N9 C29 C28 112.1(5) . . ? N9 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? N9 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C32 C30 N9 107.3(6) . . ? C32 C30 C31 129.6(6) . . ? N9 C30 C31 123.0(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 C33 107.6(5) . . ? C30 C32 H32A 126.2 . . ? C33 C32 H32A 126.2 . . ? N10 C33 C32 108.8(6) . . ? N10 C33 C34 123.8(6) . . ? C32 C33 C34 127.4(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O4 C35 O3 125.4(6) . . ? O4 C35 C36 119.8(7) . . ? O3 C35 C36 114.8(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 N2 106.0(4) . . ? C1 N1 Pd1 132.7(4) . . ? N2 N1 Pd1 120.9(3) . . ? C4 N2 N1 110.9(4) . . ? C4 N2 C6 128.6(5) . . ? N1 N2 C6 120.4(4) . . ? C7 N3 C10 108.5(5) . . ? C7 N3 Pd1 125.6(4) . . ? C10 N3 Pd1 125.8(4) . . ? C12 N4 N5 110.8(5) . . ? C12 N4 C11 128.6(5) . . ? N5 N4 C11 120.6(4) . . ? C15 N5 N4 106.1(5) . . ? C15 N5 Pd1 132.2(4) . . ? N4 N5 Pd1 120.0(4) . . ? C19 N6 N7 105.8(4) . . ? C19 N6 Pd2 132.5(4) . . ? N7 N6 Pd2 121.0(3) . . ? C22 N7 N6 111.0(4) . . ? C22 N7 C24 128.0(5) . . ? N6 N7 C24 120.9(4) . . ? C25 N8 C28 108.6(4) . . ? C25 N8 Pd2 126.1(4) . . ? C28 N8 Pd2 125.2(4) . . ? C30 N9 N10 110.2(5) . . ? C30 N9 C29 129.5(5) . . ? N10 N9 C29 120.3(4) . . ? C33 N10 N9 106.0(5) . . ? C33 N10 Pd2 132.3(4) . . ? N9 N10 Pd2 120.6(3) . . ? C17 O1 Pd1 122.5(4) . . ? C35 O3 Pd2 120.2(4) . . ? N3 Pd1 O1 177.01(17) . . ? N3 Pd1 N1 87.34(18) . . ? O1 Pd1 N1 91.73(17) . . ? N3 Pd1 N5 87.97(18) . . ? O1 Pd1 N5 92.88(17) . . ? N1 Pd1 N5 175.07(17) . . ? N8 Pd2 O3 177.26(18) . . ? N8 Pd2 N10 87.80(18) . . ? O3 Pd2 N10 90.43(18) . . ? N8 Pd2 N6 86.90(17) . . ? O3 Pd2 N6 94.83(17) . . ? N10 Pd2 N6 174.57(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 N1 C1 C3 C4 0.1(7) . . . . ? C2 C1 C3 C4 179.3(6) . . . . ? C1 C3 C4 N2 -0.3(7) . . . . ? C1 C3 C4 C5 -179.8(6) . . . . ? N2 C6 C7 N3 -52.7(7) . . . . ? N2 C6 C7 C8 129.0(6) . . . . ? N3 C7 C8 C9 0.8(6) . . . . ? C6 C7 C8 C9 179.2(6) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 N3 -0.2(6) . . . . ? C8 C9 C10 C11 -177.3(6) . . . . ? N3 C10 C11 N4 -54.4(7) . . . . ? C9 C10 C11 N4 122.5(7) . . . . ? N4 C12 C14 C15 -0.8(7) . . . . ? C13 C12 C14 C15 178.0(6) . . . . ? C12 C14 C15 N5 0.4(7) . . . . ? C12 C14 C15 C16 -179.9(6) . . . . ? N6 C19 C21 C22 0.2(6) . . . . ? C20 C19 C21 C22 178.2(6) . . . . ? C19 C21 C22 N7 -0.7(6) . . . . ? C19 C21 C22 C23 179.4(6) . . . . ? N7 C24 C25 N8 55.0(6) . . . . ? N7 C24 C25 C26 -124.7(6) . . . . ? N8 C25 C26 C27 -0.6(6) . . . . ? C24 C25 C26 C27 179.2(6) . . . . ? C25 C26 C27 C28 0.5(6) . . . . ? C26 C27 C28 N8 -0.3(6) . . . . ? C26 C27 C28 C29 179.3(6) . . . . ? N8 C28 C29 N9 51.1(7) . . . . ? C27 C28 C29 N9 -128.4(6) . . . . ? N9 C30 C32 C33 0.2(7) . . . . ? C31 C30 C32 C33 -179.8(7) . . . . ? C30 C32 C33 N10 -0.5(7) . . . . ? C30 C32 C33 C34 179.5(6) . . . . ? C3 C1 N1 N2 0.2(6) . . . . ? C2 C1 N1 N2 -179.1(6) . . . . ? C3 C1 N1 Pd1 -171.7(4) . . . . ? C2 C1 N1 Pd1 9.0(9) . . . . ? C3 C4 N2 N1 0.5(6) . . . . ? C5 C4 N2 N1 180.0(5) . . . . ? C3 C4 N2 C6 -177.6(5) . . . . ? C5 C4 N2 C6 1.9(9) . . . . ? C1 N1 N2 C4 -0.4(6) . . . . ? Pd1 N1 N2 C4 172.7(4) . . . . ? C1 N1 N2 C6 177.9(5) . . . . ? Pd1 N1 N2 C6 -9.1(7) . . . . ? C7 C6 N2 C4 -123.9(6) . . . . ? C7 C6 N2 N1 58.2(7) . . . . ? C8 C7 N3 C10 -1.0(6) . . . . ? C6 C7 N3 C10 -179.6(5) . . . . ? C8 C7 N3 Pd1 177.6(4) . . . . ? C6 C7 N3 Pd1 -1.1(7) . . . . ? C9 C10 N3 C7 0.7(6) . . . . ? C11 C10 N3 C7 178.4(5) . . . . ? C9 C10 N3 Pd1 -177.8(4) . . . . ? C11 C10 N3 Pd1 -0.2(7) . . . . ? C14 C12 N4 N5 0.9(7) . . . . ? C13 C12 N4 N5 -178.0(5) . . . . ? C14 C12 N4 C11 179.2(5) . . . . ? C13 C12 N4 C11 0.4(10) . . . . ? C10 C11 N4 C12 -116.6(6) . . . . ? C10 C11 N4 N5 61.6(6) . . . . ? C14 C15 N5 N4 0.1(6) . . . . ? C16 C15 N5 N4 -179.6(5) . . . . ? C14 C15 N5 Pd1 -164.4(4) . . . . ? C16 C15 N5 Pd1 15.9(8) . . . . ? C12 N4 N5 C15 -0.6(6) . . . . ? C11 N4 N5 C15 -179.1(5) . . . . ? C12 N4 N5 Pd1 166.2(4) . . . . ? C11 N4 N5 Pd1 -12.3(6) . . . . ? C21 C19 N6 N7 0.3(6) . . . . ? C20 C19 N6 N7 -177.8(5) . . . . ? C21 C19 N6 Pd2 171.0(4) . . . . ? C20 C19 N6 Pd2 -7.1(8) . . . . ? C21 C22 N7 N6 0.9(6) . . . . ? C23 C22 N7 N6 -179.2(5) . . . . ? C21 C22 N7 C24 -177.5(5) . . . . ? C23 C22 N7 C24 2.5(9) . . . . ? C19 N6 N7 C22 -0.7(6) . . . . ? Pd2 N6 N7 C22 -172.7(3) . . . . ? C19 N6 N7 C24 177.7(5) . . . . ? Pd2 N6 N7 C24 5.7(6) . . . . ? C25 C24 N7 C22 121.9(6) . . . . ? C25 C24 N7 N6 -56.3(6) . . . . ? C26 C25 N8 C28 0.4(6) . . . . ? C24 C25 N8 C28 -179.4(4) . . . . ? C26 C25 N8 Pd2 177.1(3) . . . . ? C24 C25 N8 Pd2 -2.7(7) . . . . ? C27 C28 N8 C25 -0.1(6) . . . . ? C29 C28 N8 C25 -179.8(5) . . . . ? C27 C28 N8 Pd2 -176.8(3) . . . . ? C29 C28 N8 Pd2 3.5(7) . . . . ? C32 C30 N9 N10 0.2(7) . . . . ? C31 C30 N9 N10 -179.8(6) . . . . ? C32 C30 N9 C29 178.8(6) . . . . ? C31 C30 N9 C29 -1.2(10) . . . . ? C28 C29 N9 C30 122.5(6) . . . . ? C28 C29 N9 N10 -59.1(7) . . . . ? C32 C33 N10 N9 0.6(6) . . . . ? C34 C33 N10 N9 -179.4(6) . . . . ? C32 C33 N10 Pd2 168.5(4) . . . . ? C34 C33 N10 Pd2 -11.6(9) . . . . ? C30 N9 N10 C33 -0.5(6) . . . . ? C29 N9 N10 C33 -179.2(5) . . . . ? C30 N9 N10 Pd2 -170.1(4) . . . . ? C29 N9 N10 Pd2 11.2(7) . . . . ? O2 C17 O1 Pd1 -1.0(9) . . . . ? C18 C17 O1 Pd1 178.7(4) . . . . ? O4 C35 O3 Pd2 -4.1(10) . . . . ? C36 C35 O3 Pd2 172.5(4) . . . . ? C7 N3 Pd1 O1 -35(3) . . . . ? C10 N3 Pd1 O1 143(3) . . . . ? C7 N3 Pd1 N1 36.8(4) . . . . ? C10 N3 Pd1 N1 -144.9(4) . . . . ? C7 N3 Pd1 N5 -141.7(4) . . . . ? C10 N3 Pd1 N5 36.6(4) . . . . ? C17 O1 Pd1 N3 -174(3) . . . . ? C17 O1 Pd1 N1 114.1(5) . . . . ? C17 O1 Pd1 N5 -67.6(5) . . . . ? C1 N1 Pd1 N3 139.9(6) . . . . ? N2 N1 Pd1 N3 -31.1(4) . . . . ? C1 N1 Pd1 O1 -43.0(6) . . . . ? N2 N1 Pd1 O1 146.1(4) . . . . ? C1 N1 Pd1 N5 158(2) . . . . ? N2 N1 Pd1 N5 -13(2) . . . . ? C15 N5 Pd1 N3 133.1(5) . . . . ? N4 N5 Pd1 N3 -29.6(4) . . . . ? C15 N5 Pd1 O1 -44.0(5) . . . . ? N4 N5 Pd1 O1 153.3(4) . . . . ? C15 N5 Pd1 N1 115(2) . . . . ? N4 N5 Pd1 N1 -47(2) . . . . ? C25 N8 Pd2 O3 -164(3) . . . . ? C28 N8 Pd2 O3 12(4) . . . . ? C25 N8 Pd2 N10 146.4(4) . . . . ? C28 N8 Pd2 N10 -37.5(4) . . . . ? C25 N8 Pd2 N6 -34.8(4) . . . . ? C28 N8 Pd2 N6 141.4(4) . . . . ? C35 O3 Pd2 N8 -162(3) . . . . ? C35 O3 Pd2 N10 -112.1(5) . . . . ? C35 O3 Pd2 N6 69.3(5) . . . . ? C33 N10 Pd2 N8 -136.9(5) . . . . ? N9 N10 Pd2 N8 29.6(4) . . . . ? C33 N10 Pd2 O3 45.2(5) . . . . ? N9 N10 Pd2 O3 -148.4(4) . . . . ? C33 N10 Pd2 N6 -149.5(17) . . . . ? N9 N10 Pd2 N6 17(2) . . . . ? C19 N6 Pd2 N8 -136.5(5) . . . . ? N7 N6 Pd2 N8 33.0(4) . . . . ? C19 N6 Pd2 O3 41.4(5) . . . . ? N7 N6 Pd2 O3 -149.1(4) . . . . ? C19 N6 Pd2 N10 -123.8(18) . . . . ? N7 N6 Pd2 N10 46(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.642 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.098 #================================================================END data_lithiumsalt_4 _database_code_depnum_ccdc_archive 'CCDC 869472' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Li2 N10, C3.5 H4' _chemical_formula_sum 'C35.50 H44 Li2 N10' _chemical_formula_weight 624.69 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.371(2) _cell_length_b 11.7200(14) _cell_length_c 17.301(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.893(4) _cell_angle_gamma 90.00 _cell_volume 3890.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 22442 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9870 _exptl_absorpt_correction_T_max 0.9935 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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-APEX-II CCD area detector' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22442 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3427 _reflns_number_gt 2333 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details SQUEEZE loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.250 0.000 212 54 ' ' 2 0.750 0.250 0.000 212 54 ' ' 3 0.750 -0.250 0.500 212 54 ' ' 4 0.250 0.250 0.500 212 54 ' ' _platon_squeeze_details ; The unit cell contains one toluene molecule which has been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.0554P)^2^+4.7080P] 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 3427 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 C1 C 0.30938(18) 0.3172(3) 0.08601(18) 0.0829(9) Uani 1 1 d . . . H1A H 0.3579 0.3341 0.0863 0.124 Uiso 1 1 calc R . . H1B H 0.2855 0.3846 0.0994 0.124 Uiso 1 1 calc R . . H1C H 0.2897 0.2917 0.0350 0.124 Uiso 1 1 calc R . . C2 C 0.30168(15) 0.2252(2) 0.14447(15) 0.0621(7) Uani 1 1 d . . . C3 C 0.24222(15) 0.1737(3) 0.16483(18) 0.0765(9) Uani 1 1 d . . . H3 H 0.1964 0.1887 0.1435 0.092 Uiso 1 1 calc R . . C4 C 0.26408(14) 0.0965(3) 0.22228(17) 0.0683(8) Uani 1 1 d . . . C5 C 0.22438(17) 0.0181(3) 0.2677(2) 0.0995(12) Uani 1 1 d . . . H5A H 0.2564 -0.0256 0.3034 0.149 Uiso 1 1 calc R . . H5B H 0.1965 -0.0325 0.2326 0.149 Uiso 1 1 calc R . . H5C H 0.1946 0.0620 0.2965 0.149 Uiso 1 1 calc R . . C6 C 0.38369(15) 0.0449(3) 0.29356(16) 0.0693(8) Uani 1 1 d . . . H6A H 0.3596 -0.0174 0.3153 0.083 Uiso 1 1 calc R . . H6B H 0.3972 0.0990 0.3353 0.083 Uiso 1 1 calc R . . C7 C 0.44783(15) -0.0009(2) 0.26709(14) 0.0603(7) Uani 1 1 d . . . C8 C 0.46671(16) -0.1129(3) 0.26050(18) 0.0816(10) Uani 1 1 d . . . H8 H 0.4400 -0.1767 0.2686 0.098 Uiso 1 1 calc R . . C9 C 0.42695(17) 0.1050(3) -0.00203(19) 0.0862(10) Uani 1 1 d . . . H9A H 0.4147 0.0785 0.0468 0.129 Uiso 1 1 calc R . . H9B H 0.4483 0.0441 -0.0273 0.129 Uiso 1 1 calc R . . H9C H 0.3857 0.1299 -0.0348 0.129 Uiso 1 1 calc R . . C10 C 0.47691(14) 0.2025(2) 0.01229(15) 0.0593(7) Uani 1 1 d . . . C11 C 0.50807(15) 0.2670(3) -0.03996(15) 0.0679(8) Uani 1 1 d . . . H11 H 0.5024 0.2580 -0.0939 0.082 Uiso 1 1 calc R . . C12 C 0.54870(14) 0.3466(2) 0.00220(15) 0.0578(7) Uani 1 1 d . . . C13 C 0.59402(17) 0.4390(3) -0.02275(18) 0.0802(9) Uani 1 1 d . . . H13A H 0.6153 0.4802 0.0223 0.120 Uiso 1 1 calc R . . H13B H 0.5663 0.4903 -0.0574 0.120 Uiso 1 1 calc R . . H13C H 0.6296 0.4059 -0.0492 0.120 Uiso 1 1 calc R . . C14 C 0.57938(13) 0.3779(2) 0.14865(14) 0.0620(7) Uani 1 1 d . . . H14A H 0.6084 0.4394 0.1338 0.074 Uiso 1 1 calc R . . H14B H 0.6100 0.3203 0.1749 0.074 Uiso 1 1 calc R . . C15 C 0.53424(13) 0.4236(2) 0.20492(13) 0.0526(6) Uani 1 1 d . . . C16 C 0.52181(15) 0.5352(2) 0.22082(15) 0.0675(8) Uani 1 1 d . . . H16 H 0.5389 0.5988 0.1975 0.081 Uiso 1 1 calc R . . Li1 Li 0.4606(2) 0.2099(4) 0.1866(2) 0.0555(10) Uani 1 1 d . . . N1 N 0.35822(11) 0.18146(19) 0.18658(12) 0.0601(6) Uani 1 1 d . . . N2 N 0.33428(11) 0.10179(19) 0.23314(12) 0.0600(6) Uani 1 1 d . . . N3 N 0.5000 0.0701(2) 0.2500 0.0554(8) Uani 1 2 d S . . N4 N 0.49747(11) 0.23843(19) 0.08508(12) 0.0593(6) Uani 1 1 d . . . N5 N 0.54128(11) 0.32773(18) 0.07773(11) 0.0547(5) Uani 1 1 d . . . N6 N 0.5000 0.3523(2) 0.2500 0.0499(7) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.093(2) 0.078(2) 0.078(2) 0.0143(17) 0.0138(17) 0.0147(18) C2 0.0648(17) 0.0642(17) 0.0564(16) -0.0001(13) 0.0047(14) 0.0037(14) C3 0.0574(18) 0.096(2) 0.074(2) 0.0022(18) 0.0019(15) -0.0045(17) C4 0.0565(17) 0.083(2) 0.0646(17) -0.0054(16) 0.0072(14) -0.0202(15) C5 0.075(2) 0.126(3) 0.098(3) 0.008(2) 0.0115(18) -0.043(2) C6 0.0687(18) 0.083(2) 0.0553(16) 0.0195(14) 0.0057(14) -0.0178(16) C7 0.0734(18) 0.0562(16) 0.0476(15) 0.0124(12) -0.0049(13) -0.0072(14) C8 0.102(2) 0.0556(17) 0.080(2) 0.0133(16) -0.014(2) -0.0121(15) C9 0.090(2) 0.086(2) 0.080(2) -0.0255(18) 0.0051(17) -0.0164(19) C10 0.0625(16) 0.0621(17) 0.0523(15) -0.0098(13) 0.0042(12) 0.0001(13) C11 0.0806(19) 0.081(2) 0.0426(14) -0.0035(14) 0.0116(14) 0.0024(16) C12 0.0639(16) 0.0639(17) 0.0481(14) 0.0095(13) 0.0172(12) 0.0068(13) C13 0.090(2) 0.085(2) 0.0686(19) 0.0207(16) 0.0226(16) -0.0053(17) C14 0.0577(16) 0.0743(18) 0.0532(15) 0.0010(14) 0.0051(12) -0.0216(14) C15 0.0561(15) 0.0551(16) 0.0438(13) -0.0001(12) -0.0032(11) -0.0111(12) C16 0.089(2) 0.0516(16) 0.0581(17) 0.0057(12) -0.0030(14) -0.0153(14) Li1 0.058(2) 0.064(3) 0.045(2) 0.0059(19) 0.0051(18) -0.012(2) N1 0.0621(14) 0.0650(14) 0.0529(12) 0.0087(11) 0.0064(11) -0.0106(11) N2 0.0590(14) 0.0681(14) 0.0525(12) 0.0083(11) 0.0065(10) -0.0160(11) N3 0.0642(19) 0.0519(18) 0.0496(17) 0.000 0.0060(14) 0.000 N4 0.0635(13) 0.0663(14) 0.0484(12) -0.0009(11) 0.0086(10) -0.0148(11) N5 0.0574(12) 0.0618(13) 0.0458(12) -0.0002(10) 0.0101(9) -0.0113(11) N6 0.0535(17) 0.0509(17) 0.0453(15) 0.000 0.0068(13) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.500(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.332(3) . ? C2 C3 1.388(4) . ? C3 C4 1.367(4) . ? C3 H3 0.9300 . ? C4 N2 1.348(3) . ? C4 C5 1.490(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.476(3) . ? C6 C7 1.483(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.372(4) . ? C7 N3 1.373(3) . ? C8 C8 1.387(6) 2_655 ? C8 H8 0.9300 . ? C9 C10 1.495(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N4 1.336(3) . ? C10 C11 1.380(4) . ? C11 C12 1.365(4) . ? C11 H11 0.9300 . ? C12 N5 1.352(3) . ? C12 C13 1.495(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N5 1.465(3) . ? C14 C15 1.495(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.364(4) . ? C15 N6 1.374(3) . ? C16 C16 1.403(6) 2_655 ? C16 H16 0.9300 . ? Li1 N1 2.012(5) . ? Li1 N4 2.012(4) . ? Li1 N3 2.059(5) . ? Li1 N6 2.083(5) . ? Li1 Li1 2.495(8) 2_655 ? N1 N2 1.356(3) . ? N3 C7 1.373(3) 2_655 ? N3 Li1 2.059(5) 2_655 ? N4 N5 1.364(3) . ? N6 C15 1.374(3) 2_655 ? N6 Li1 2.083(5) 2_655 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 110.0(2) . . ? N1 C2 C1 119.7(3) . . ? C3 C2 C1 130.3(3) . . ? C4 C3 C2 106.7(3) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? N2 C4 C3 106.1(2) . . ? N2 C4 C5 122.6(3) . . ? C3 C4 C5 131.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 115.7(2) . . ? N2 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? N2 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C8 C7 N3 110.5(3) . . ? C8 C7 C6 128.1(3) . . ? N3 C7 C6 121.3(2) . . ? C7 C8 C8 106.85(18) . 2_655 ? C7 C8 H8 126.6 . . ? C8 C8 H8 126.6 2_655 . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 110.1(2) . . ? N4 C10 C9 120.0(3) . . ? C11 C10 C9 129.9(3) . . ? C12 C11 C10 107.2(2) . . ? C12 C11 H11 126.4 . . ? C10 C11 H11 126.4 . . ? N5 C12 C11 105.9(2) . . ? N5 C12 C13 122.8(3) . . ? C11 C12 C13 131.2(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 C15 114.6(2) . . ? N5 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N5 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 N6 110.9(2) . . ? C16 C15 C14 127.6(2) . . ? N6 C15 C14 121.5(2) . . ? C15 C16 C16 106.58(16) . 2_655 ? C15 C16 H16 126.7 . . ? C16 C16 H16 126.7 2_655 . ? N1 Li1 N4 119.7(2) . . ? N1 Li1 N3 99.27(18) . . ? N4 Li1 N3 116.6(2) . . ? N1 Li1 N6 115.0(2) . . ? N4 Li1 N6 100.29(18) . . ? N3 Li1 N6 105.93(19) . . ? N1 Li1 Li1 118.9(3) . 2_655 ? N4 Li1 Li1 121.4(3) . 2_655 ? N3 Li1 Li1 52.71(12) . 2_655 ? N6 Li1 Li1 53.22(12) . 2_655 ? C2 N1 N2 105.5(2) . . ? C2 N1 Li1 132.3(2) . . ? N2 N1 Li1 122.1(2) . . ? C4 N2 N1 111.7(2) . . ? C4 N2 C6 128.4(2) . . ? N1 N2 C6 119.4(2) . . ? C7 N3 C7 105.3(3) 2_655 . ? C7 N3 Li1 111.59(16) 2_655 2_655 ? C7 N3 Li1 126.70(17) . 2_655 ? C7 N3 Li1 126.70(17) 2_655 . ? C7 N3 Li1 111.59(16) . . ? Li1 N3 Li1 74.6(2) 2_655 . ? C10 N4 N5 105.2(2) . . ? C10 N4 Li1 132.4(2) . . ? N5 N4 Li1 120.57(19) . . ? C12 N5 N4 111.4(2) . . ? C12 N5 C14 129.4(2) . . ? N4 N5 C14 118.56(19) . . ? C15 N6 C15 105.1(3) 2_655 . ? C15 N6 Li1 128.02(17) 2_655 . ? C15 N6 Li1 111.01(15) . . ? C15 N6 Li1 111.01(15) 2_655 2_655 ? C15 N6 Li1 128.02(17) . 2_655 ? Li1 N6 Li1 73.6(2) . 2_655 ? 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 N1 C2 C3 C4 0.7(3) . . . . ? C1 C2 C3 C4 -178.9(3) . . . . ? C2 C3 C4 N2 -1.4(3) . . . . ? C2 C3 C4 C5 178.7(3) . . . . ? N2 C6 C7 C8 -111.5(3) . . . . ? N2 C6 C7 N3 72.8(3) . . . . ? N3 C7 C8 C8 0.7(4) . . . 2_655 ? C6 C7 C8 C8 -175.3(3) . . . 2_655 ? N4 C10 C11 C12 -0.7(3) . . . . ? C9 C10 C11 C12 179.3(3) . . . . ? C10 C11 C12 N5 0.3(3) . . . . ? C10 C11 C12 C13 -179.8(3) . . . . ? N5 C14 C15 C16 -107.5(3) . . . . ? N5 C14 C15 N6 74.0(3) . . . . ? N6 C15 C16 C16 0.6(4) . . . 2_655 ? C14 C15 C16 C16 -178.1(3) . . . 2_655 ? C3 C2 N1 N2 0.4(3) . . . . ? C1 C2 N1 N2 180.0(2) . . . . ? C3 C2 N1 Li1 177.6(3) . . . . ? C1 C2 N1 Li1 -2.7(4) . . . . ? N4 Li1 N1 C2 -37.2(4) . . . . ? N3 Li1 N1 C2 -165.2(2) . . . . ? N6 Li1 N1 C2 82.3(3) . . . . ? Li1 Li1 N1 C2 142.4(2) 2_655 . . . ? N4 Li1 N1 N2 139.7(2) . . . . ? N3 Li1 N1 N2 11.7(3) . . . . ? N6 Li1 N1 N2 -100.8(3) . . . . ? Li1 Li1 N1 N2 -40.7(3) 2_655 . . . ? C3 C4 N2 N1 1.8(3) . . . . ? C5 C4 N2 N1 -178.3(3) . . . . ? C3 C4 N2 C6 173.3(3) . . . . ? C5 C4 N2 C6 -6.8(5) . . . . ? C2 N1 N2 C4 -1.3(3) . . . . ? Li1 N1 N2 C4 -179.0(2) . . . . ? C2 N1 N2 C6 -173.7(2) . . . . ? Li1 N1 N2 C6 8.7(3) . . . . ? C7 C6 N2 C4 140.2(3) . . . . ? C7 C6 N2 N1 -48.9(3) . . . . ? C8 C7 N3 C7 -0.29(15) . . . 2_655 ? C6 C7 N3 C7 176.1(3) . . . 2_655 ? C8 C7 N3 Li1 -133.1(3) . . . 2_655 ? C6 C7 N3 Li1 43.3(3) . . . 2_655 ? C8 C7 N3 Li1 140.5(2) . . . . ? C6 C7 N3 Li1 -43.2(3) . . . . ? N1 Li1 N3 C7 134.9(2) . . . 2_655 ? N4 Li1 N3 C7 4.8(3) . . . 2_655 ? N6 Li1 N3 C7 -105.7(2) . . . 2_655 ? Li1 Li1 N3 C7 -105.7(2) 2_655 . . 2_655 ? N1 Li1 N3 C7 4.5(2) . . . . ? N4 Li1 N3 C7 -125.6(2) . . . . ? N6 Li1 N3 C7 123.9(2) . . . . ? Li1 Li1 N3 C7 123.9(2) 2_655 . . . ? N1 Li1 N3 Li1 -119.4(3) . . . 2_655 ? N4 Li1 N3 Li1 110.5(3) . . . 2_655 ? N6 Li1 N3 Li1 0.0 . . . 2_655 ? C11 C10 N4 N5 0.9(3) . . . . ? C9 C10 N4 N5 -179.1(2) . . . . ? C11 C10 N4 Li1 165.3(3) . . . . ? C9 C10 N4 Li1 -14.7(4) . . . . ? N1 Li1 N4 C10 -30.4(4) . . . . ? N3 Li1 N4 C10 89.1(3) . . . . ? N6 Li1 N4 C10 -157.1(2) . . . . ? Li1 Li1 N4 C10 149.9(2) 2_655 . . . ? N1 Li1 N4 N5 132.1(2) . . . . ? N3 Li1 N4 N5 -108.4(3) . . . . ? N6 Li1 N4 N5 5.4(3) . . . . ? Li1 Li1 N4 N5 -47.6(3) 2_655 . . . ? C11 C12 N5 N4 0.3(3) . . . . ? C13 C12 N5 N4 -179.7(2) . . . . ? C11 C12 N5 C14 171.4(3) . . . . ? C13 C12 N5 C14 -8.6(4) . . . . ? C10 N4 N5 C12 -0.7(3) . . . . ? Li1 N4 N5 C12 -167.4(2) . . . . ? C10 N4 N5 C14 -172.9(2) . . . . ? Li1 N4 N5 C14 20.4(3) . . . . ? C15 C14 N5 C12 130.5(3) . . . . ? C15 C14 N5 N4 -58.9(3) . . . . ? C16 C15 N6 C15 -0.22(14) . . . 2_655 ? C14 C15 N6 C15 178.5(3) . . . 2_655 ? C16 C15 N6 Li1 141.7(2) . . . . ? C14 C15 N6 Li1 -39.6(3) . . . . ? C16 C15 N6 Li1 -133.2(2) . . . 2_655 ? C14 C15 N6 Li1 45.5(3) . . . 2_655 ? N1 Li1 N6 C15 4.4(3) . . . 2_655 ? N4 Li1 N6 C15 134.2(2) . . . 2_655 ? N3 Li1 N6 C15 -104.1(2) . . . 2_655 ? Li1 Li1 N6 C15 -104.1(2) 2_655 . . 2_655 ? N1 Li1 N6 C15 -126.4(2) . . . . ? N4 Li1 N6 C15 3.4(2) . . . . ? N3 Li1 N6 C15 125.07(19) . . . . ? Li1 Li1 N6 C15 125.07(19) 2_655 . . . ? N1 Li1 N6 Li1 108.5(3) . . . 2_655 ? N4 Li1 N6 Li1 -121.7(3) . . . 2_655 ? N3 Li1 N6 Li1 0.0 . . . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.280 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.036 #================================================================END data_chlorocomplex_5 _database_code_depnum_ccdc_archive 'CCDC 869473' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Cl N5 Pd' _chemical_formula_weight 424.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.811(4) _cell_length_b 14.946(4) _cell_length_c 8.938(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1711.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 18842 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 24.99 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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-APEX-II CCD area detector' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18842 _diffrn_reflns_av_R_equivalents 0.1735 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1514 _reflns_number_gt 827 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+7.1426P] 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 1514 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 C1 C -0.2214(7) 0.2609(6) 0.9225(10) 0.067(3) Uani 1 1 d . . . H1A H -0.1484 0.2753 0.9271 0.101 Uiso 1 1 calc R . . H1B H -0.2458 0.2450 1.0205 0.101 Uiso 1 1 calc R . . H1C H -0.2597 0.3118 0.8867 0.101 Uiso 1 1 calc R . . C2 C -0.2373(7) 0.1842(5) 0.8188(9) 0.045(2) Uani 1 1 d . . . C3 C -0.3306(6) 0.1454(5) 0.7816(8) 0.046(2) Uani 1 1 d . . . H3 H -0.3959 0.1624 0.8171 0.055 Uiso 1 1 calc R . . C4 C -0.3108(5) 0.0772(5) 0.6830(8) 0.0373(18) Uani 1 1 d . . . C5 C -0.3822(6) 0.0151(6) 0.6016(10) 0.061(3) Uani 1 1 d . . . H5A H -0.3418 -0.0249 0.5406 0.091 Uiso 1 1 calc R . . H5B H -0.4285 0.0491 0.5392 0.091 Uiso 1 1 calc R . . H5C H -0.4221 -0.0188 0.6725 0.091 Uiso 1 1 calc R . . C6 C -0.1435(5) 0.0134(4) 0.5737(8) 0.0361(18) Uani 1 1 d . . . H6A H -0.1071 0.0455 0.4952 0.043 Uiso 1 1 calc R . . H6B H -0.1889 -0.0304 0.5269 0.043 Uiso 1 1 calc R . . C7 C -0.0665(5) -0.0332(5) 0.6713(8) 0.0343(17) Uani 1 1 d . . . C8 C -0.0424(5) -0.1202(5) 0.6999(8) 0.042(2) Uani 1 1 d . . . H8 H -0.0757 -0.1703 0.6606 0.051 Uiso 1 1 calc R . . N1 N -0.1590(4) 0.1428(3) 0.7441(8) 0.0401(13) Uani 1 1 d . . . N2 N -0.2064(5) 0.0764(4) 0.6620(6) 0.0331(14) Uani 1 1 d . . . N3 N 0.0000 0.0204(4) 0.7500 0.0338(17) Uani 1 2 d S . . Cl1 Cl 0.0000 0.30618(18) 0.7500 0.1017(14) Uani 1 2 d S . . Pd1 Pd 0.0000 0.15143(4) 0.7500 0.0376(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.083(7) 0.061(6) 0.058(6) -0.026(5) -0.006(5) 0.019(5) C2 0.056(5) 0.039(4) 0.041(4) 0.000(4) -0.006(4) 0.017(4) C3 0.044(4) 0.051(5) 0.043(6) 0.007(4) 0.008(4) 0.014(4) C4 0.031(4) 0.042(4) 0.039(4) 0.006(4) 0.004(4) 0.000(4) C5 0.034(4) 0.069(6) 0.079(7) -0.012(5) 0.004(5) -0.010(4) C6 0.042(4) 0.034(4) 0.033(4) -0.016(3) 0.005(4) -0.006(3) C7 0.032(4) 0.038(4) 0.032(4) -0.002(4) -0.001(3) -0.002(3) C8 0.048(4) 0.030(4) 0.049(5) -0.006(3) 0.003(3) -0.006(3) N1 0.047(3) 0.035(3) 0.038(3) 0.002(4) -0.005(4) 0.002(3) N2 0.041(4) 0.030(3) 0.028(3) -0.004(3) -0.003(3) -0.002(3) N3 0.033(4) 0.033(4) 0.035(4) 0.000 0.005(6) 0.000 Cl1 0.079(2) 0.0281(14) 0.198(4) 0.000 -0.017(4) 0.000 Pd1 0.0403(4) 0.0256(4) 0.0469(4) 0.000 -0.0100(6) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.488(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.355(9) . ? C2 C3 1.369(10) . ? C3 C4 1.372(9) . ? C3 H3 0.9300 . ? C4 N2 1.351(8) . ? C4 C5 1.491(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.469(8) . ? C6 C7 1.490(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.362(9) . ? C7 N3 1.365(7) . ? C8 C8 1.408(14) 4_556 ? C8 H8 0.9300 . ? N1 N2 1.376(7) . ? N1 Pd1 2.041(5) . ? N3 C7 1.365(7) 4_556 ? N3 Pd1 1.958(7) . ? Cl1 Pd1 2.313(3) . ? Pd1 N1 2.041(5) 4_556 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.5(7) . . ? N1 C2 C1 123.9(8) . . ? C3 C2 C1 126.6(8) . . ? C2 C3 C4 108.0(7) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? N2 C4 C3 106.1(7) . . ? N2 C4 C5 122.2(7) . . ? C3 C4 C5 131.5(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 110.4(6) . . ? N2 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? N2 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 N3 108.8(6) . . ? C8 C7 C6 134.9(6) . . ? N3 C7 C6 116.2(6) . . ? C7 C8 C8 107.1(4) . 4_556 ? C7 C8 H8 126.4 . . ? C8 C8 H8 126.4 4_556 . ? C2 N1 N2 105.4(6) . . ? C2 N1 Pd1 134.2(6) . . ? N2 N1 Pd1 120.0(4) . . ? C4 N2 N1 110.9(6) . . ? C4 N2 C6 128.5(6) . . ? N1 N2 C6 120.5(6) . . ? C7 N3 C7 108.1(7) 4_556 . ? C7 N3 Pd1 126.0(4) 4_556 . ? C7 N3 Pd1 126.0(4) . . ? N3 Pd1 N1 86.37(14) . . ? N3 Pd1 N1 86.37(14) . 4_556 ? N1 Pd1 N1 172.7(3) . 4_556 ? N3 Pd1 Cl1 180.0 . . ? N1 Pd1 Cl1 93.63(14) . . ? N1 Pd1 Cl1 93.63(14) 4_556 . ? 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 N1 C2 C3 C4 0.9(9) . . . . ? C1 C2 C3 C4 179.9(7) . . . . ? C2 C3 C4 N2 -0.3(8) . . . . ? C2 C3 C4 C5 -177.2(8) . . . . ? N2 C6 C7 C8 126.0(9) . . . . ? N2 C6 C7 N3 -56.5(7) . . . . ? N3 C7 C8 C8 -0.1(10) . . . 4_556 ? C6 C7 C8 C8 177.6(8) . . . 4_556 ? C3 C2 N1 N2 -1.1(8) . . . . ? C1 C2 N1 N2 179.9(7) . . . . ? C3 C2 N1 Pd1 -173.4(5) . . . . ? C1 C2 N1 Pd1 7.5(12) . . . . ? C3 C4 N2 N1 -0.4(8) . . . . ? C5 C4 N2 N1 176.9(7) . . . . ? C3 C4 N2 C6 176.2(6) . . . . ? C5 C4 N2 C6 -6.6(12) . . . . ? C2 N1 N2 C4 0.9(8) . . . . ? Pd1 N1 N2 C4 174.6(5) . . . . ? C2 N1 N2 C6 -176.0(6) . . . . ? Pd1 N1 N2 C6 -2.3(8) . . . . ? C7 C6 N2 C4 -119.6(8) . . . . ? C7 C6 N2 N1 56.6(8) . . . . ? C8 C7 N3 C7 0.0(4) . . . 4_556 ? C6 C7 N3 C7 -178.1(7) . . . 4_556 ? C8 C7 N3 Pd1 -180.0(4) . . . . ? C6 C7 N3 Pd1 1.9(7) . . . . ? C7 N3 Pd1 N1 -141.9(4) 4_556 . . . ? C7 N3 Pd1 N1 38.1(4) . . . . ? C7 N3 Pd1 N1 38.1(4) 4_556 . . 4_556 ? C7 N3 Pd1 N1 -141.9(4) . . . 4_556 ? C7 N3 Pd1 Cl1 0(37) 4_556 . . . ? C7 N3 Pd1 Cl1 0(100) . . . . ? C2 N1 Pd1 N3 134.4(7) . . . . ? N2 N1 Pd1 N3 -37.0(5) . . . . ? C2 N1 Pd1 N1 134.4(7) . . . 4_556 ? N2 N1 Pd1 N1 -37.0(5) . . . 4_556 ? C2 N1 Pd1 Cl1 -45.6(7) . . . . ? N2 N1 Pd1 Cl1 143.0(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.554 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.112 #================================================================END data_compound_6.CH2Cl2.2H2O _database_code_depnum_ccdc_archive 'CCDC 869474' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H44 Cl6 N10 O2 Pd2' _chemical_formula_weight 1038.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7331(7) _cell_length_b 14.8663(9) _cell_length_c 15.3431(15) _cell_angle_alpha 107.086(2) _cell_angle_beta 106.270(2) _cell_angle_gamma 105.8830(10) _cell_volume 2263.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18664 _cell_measurement_theta_min 0.819 _cell_measurement_theta_max 0.877 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.877 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD APEX 2' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18664 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7909 _reflns_number_gt 6242 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution Sir-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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.The two water molecules are severely disordered and handled with EADP and SADI options and their hydrogen atoms are not located. ; _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^)+(0.0853P)^2^+2.7078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7909 _refine_ls_number_parameters 492 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 C1 C 0.1656(8) 0.5635(6) 0.1277(6) 0.082(2) Uani 1 1 d . . . H1A H 0.0992 0.5294 0.1454 0.122 Uiso 1 1 calc R . . H1B H 0.1377 0.5360 0.0569 0.122 Uiso 1 1 calc R . . H1C H 0.1831 0.6352 0.1519 0.122 Uiso 1 1 calc R . . C2 C 0.2854(6) 0.5477(4) 0.1727(5) 0.0598(15) Uani 1 1 d . . . C3 C 0.4048(7) 0.5816(5) 0.1675(6) 0.0733(19) Uani 1 1 d . . . H3 H 0.4284 0.6216 0.1339 0.088 Uiso 1 1 calc R . . C4 C 0.4807(6) 0.5461(5) 0.2202(5) 0.0662(17) Uani 1 1 d . . . C5 C 0.6175(7) 0.5574(8) 0.2419(7) 0.105(3) Uani 1 1 d . . . H5A H 0.6396 0.5211 0.2822 0.158 Uiso 1 1 calc R . . H5B H 0.6731 0.6283 0.2767 0.158 Uiso 1 1 calc R . . H5C H 0.6274 0.5298 0.1808 0.158 Uiso 1 1 calc R . . C6 C 0.4377(6) 0.4276(4) 0.3087(4) 0.0534(14) Uani 1 1 d . . . H6A H 0.3815 0.4183 0.3439 0.064 Uiso 1 1 calc R . . H6B H 0.5257 0.4626 0.3574 0.064 Uiso 1 1 calc R . . C7 C 0.4220(5) 0.3258(4) 0.2419(4) 0.0496(13) Uani 1 1 d . . . C8 C 0.5116(6) 0.2860(5) 0.2312(5) 0.0638(17) Uani 1 1 d . . . H8 H 0.6005 0.3193 0.2649 0.077 Uiso 1 1 calc R . . C9 C 0.4438(6) 0.1849(5) 0.1592(5) 0.0613(16) Uani 1 1 d . . . H9 H 0.4800 0.1386 0.1380 0.074 Uiso 1 1 calc R . . C10 C 0.3176(5) 0.1671(4) 0.1267(4) 0.0450(12) Uani 1 1 d . . . C11 C 0.2023(5) 0.0738(4) 0.0504(4) 0.0487(13) Uani 1 1 d . . . H11A H 0.1414 0.0539 0.0796 0.058 Uiso 1 1 calc R . . H11B H 0.1600 0.0893 -0.0041 0.058 Uiso 1 1 calc R . . C12 C 0.2605(6) -0.0387(5) -0.0717(4) 0.0556(14) Uani 1 1 d . . . C13 C 0.2559(7) 0.0203(6) -0.1354(5) 0.076(2) Uani 1 1 d . . . H13A H 0.2336 0.0767 -0.1078 0.115 Uiso 1 1 calc R . . H13B H 0.1923 -0.0234 -0.2010 0.115 Uiso 1 1 calc R . . H13C H 0.3387 0.0456 -0.1383 0.115 Uiso 1 1 calc R . . C14 C 0.2881(6) -0.1241(5) -0.0808(5) 0.0607(16) Uani 1 1 d . . . H14 H 0.3063 -0.1611 -0.1318 0.073 Uiso 1 1 calc R . . C15 C 0.2833(6) -0.1444(5) 0.0014(5) 0.0586(15) Uani 1 1 d . . . C16 C 0.3025(8) -0.2295(6) 0.0272(6) 0.084(2) Uani 1 1 d . . . H16A H 0.2925 -0.2233 0.0884 0.126 Uiso 1 1 calc R . . H16B H 0.3875 -0.2267 0.0343 0.126 Uiso 1 1 calc R . . H16C H 0.2398 -0.2935 -0.0246 0.126 Uiso 1 1 calc R . . C17 C 0.2813(6) -0.0755(5) 0.3875(5) 0.0582(15) Uani 1 1 d . . . C18 C 0.2055(8) -0.1862(5) 0.3255(6) 0.081(2) Uani 1 1 d . . . H18A H 0.1852 -0.1984 0.2569 0.121 Uiso 1 1 calc R . . H18B H 0.1272 -0.2072 0.3359 0.121 Uiso 1 1 calc R . . H18C H 0.2551 -0.2243 0.3437 0.121 Uiso 1 1 calc R . . C19 C 0.3316(7) -0.0228(5) 0.4892(5) 0.0633(16) Uani 1 1 d . . . H19 H 0.3251 -0.0504 0.5356 0.076 Uiso 1 1 calc R . . C20 C 0.3930(6) 0.0782(5) 0.5087(4) 0.0549(14) Uani 1 1 d . . . C21 C 0.4595(8) 0.1717(6) 0.6042(5) 0.076(2) Uani 1 1 d . . . H21A H 0.4921 0.2307 0.5910 0.114 Uiso 1 1 calc R . . H21B H 0.5296 0.1647 0.6483 0.114 Uiso 1 1 calc R . . H21C H 0.3993 0.1794 0.6343 0.114 Uiso 1 1 calc R . . C22 C 0.4202(5) 0.1756(4) 0.4020(4) 0.0474(12) Uani 1 1 d . . . H22A H 0.4206 0.1570 0.3360 0.057 Uiso 1 1 calc R . . H22B H 0.5071 0.2208 0.4491 0.057 Uiso 1 1 calc R . . C23 C 0.3322(5) 0.2312(4) 0.4100(4) 0.0436(12) Uani 1 1 d . . . C24 C 0.3547(6) 0.3236(4) 0.4761(4) 0.0550(14) Uani 1 1 d . . . H24 H 0.4322 0.3685 0.5287 0.066 Uiso 1 1 calc R . . C25 C 0.2380(6) 0.3397(4) 0.4504(4) 0.0524(14) Uani 1 1 d . . . H25 H 0.2253 0.3973 0.4830 0.063 Uiso 1 1 calc R . . C26 C 0.1488(5) 0.2560(4) 0.3701(4) 0.0433(12) Uani 1 1 d . . . C27 C 0.0110(5) 0.2297(4) 0.3087(4) 0.0468(12) Uani 1 1 d . . . H27A H -0.0001 0.2121 0.2399 0.056 Uiso 1 1 calc R . . H27B H -0.0430 0.1702 0.3130 0.056 Uiso 1 1 calc R . . C28 C -0.1199(5) 0.3143(4) 0.3788(4) 0.0468(12) Uani 1 1 d . . . C29 C -0.1850(7) 0.2301(5) 0.4044(5) 0.0712(18) Uani 1 1 d . . . H29A H -0.1507 0.1783 0.3909 0.107 Uiso 1 1 calc R . . H29B H -0.2759 0.2012 0.3652 0.107 Uiso 1 1 calc R . . H29C H -0.1701 0.2568 0.4734 0.107 Uiso 1 1 calc R . . C30 C -0.1364(5) 0.4046(4) 0.3864(4) 0.0510(13) Uani 1 1 d . . . H30 H -0.1914 0.4278 0.4114 0.061 Uiso 1 1 calc R . . C31 C -0.0555(5) 0.4540(4) 0.3496(4) 0.0460(12) Uani 1 1 d . . . C32 C -0.0413(6) 0.5514(5) 0.3378(5) 0.0645(16) Uani 1 1 d . . . H32A H 0.0228 0.5671 0.3110 0.097 Uiso 1 1 calc R . . H32B H -0.0152 0.6052 0.4012 0.097 Uiso 1 1 calc R . . H32C H -0.1221 0.5450 0.2936 0.097 Uiso 1 1 calc R . . C33 C 0.2020(11) 0.3145(8) -0.0456(7) 0.118(4) Uani 1 1 d . . . H33A H 0.2024 0.3431 0.0201 0.142 Uiso 1 1 calc R . . H33B H 0.1427 0.2436 -0.0770 0.142 Uiso 1 1 calc R . . N1 N 0.2886(4) 0.4918(3) 0.2263(3) 0.0479(11) Uani 1 1 d . . . N2 N 0.4085(4) 0.4917(3) 0.2566(4) 0.0500(11) Uani 1 1 d . . . N3 N 0.3051(4) 0.2532(4) 0.1775(3) 0.0439(10) Uani 1 1 d D . . H1 H 0.246(5) 0.258(5) 0.175(5) 0.053 Uiso 1 1 d D . . N4 N 0.2404(4) -0.0101(3) 0.0131(3) 0.0461(10) Uani 1 1 d . . . N5 N 0.2540(4) -0.0737(3) 0.0594(3) 0.0480(10) Uani 1 1 d . . . N6 N 0.3126(4) -0.0098(3) 0.3462(3) 0.0488(11) Uani 1 1 d . . . N7 N 0.3816(4) 0.0838(3) 0.4209(3) 0.0463(10) Uani 1 1 d . . . N8 N 0.2063(5) 0.1904(3) 0.3454(3) 0.0448(10) Uani 1 1 d D . . H2 H 0.176(6) 0.140(4) 0.309(4) 0.054 Uiso 1 1 d D . . N9 N -0.0310(4) 0.3122(3) 0.3393(3) 0.0434(10) Uani 1 1 d . . . N10 N 0.0089(4) 0.3977(3) 0.3208(3) 0.0453(10) Uani 1 1 d . . . O1 O 0.0951(7) 0.1872(5) 0.5812(6) 0.104(3) Uani 0.832(9) 1 d P A 1 O1' O 0.059(3) 0.106(2) 0.629(3) 0.104(3) Uani 0.168(9) 1 d P . 2 O2 O 0.1558(10) 0.0451(8) -0.3507(6) 0.132(4) Uani 0.854(12) 1 d P B 1 O2' O 0.031(6) -0.001(5) -0.403(4) 0.132(4) Uani 0.146(12) 1 d P . 2 Cl1 Cl 0.27613(14) 0.57921(11) 0.42397(11) 0.0584(4) Uani 1 1 d . . . Cl2 Cl 0.03949(14) 0.30399(12) 0.12288(11) 0.0599(4) Uani 1 1 d . . . Cl3 Cl 0.06851(13) -0.05876(12) 0.17233(11) 0.0587(4) Uani 1 1 d . . . Cl4 Cl 0.49413(14) -0.01361(13) 0.24173(12) 0.0612(4) Uani 1 1 d . . . Cl5 Cl 0.1467(3) 0.3793(3) -0.1138(2) 0.1457(12) Uani 1 1 d . . . Cl6 Cl 0.3532(4) 0.3202(3) -0.0345(3) 0.1612(13) Uani 1 1 d . . . Pd1 Pd 0.15251(4) 0.44013(3) 0.27454(3) 0.04328(14) Uani 1 1 d . . . Pd2 Pd 0.28081(4) -0.03951(3) 0.20307(3) 0.04439(14) 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 0.085(5) 0.075(5) 0.104(6) 0.047(5) 0.045(5) 0.039(4) C2 0.066(4) 0.045(3) 0.068(4) 0.022(3) 0.031(3) 0.017(3) C3 0.074(5) 0.060(4) 0.094(5) 0.040(4) 0.045(4) 0.017(4) C4 0.054(4) 0.060(4) 0.078(4) 0.022(3) 0.037(3) 0.007(3) C5 0.065(5) 0.134(8) 0.127(7) 0.064(6) 0.060(5) 0.019(5) C6 0.044(3) 0.047(3) 0.055(3) 0.009(3) 0.018(3) 0.011(3) C7 0.038(3) 0.049(3) 0.050(3) 0.013(3) 0.013(2) 0.011(2) C8 0.036(3) 0.059(4) 0.074(4) 0.010(3) 0.013(3) 0.014(3) C9 0.041(3) 0.053(3) 0.078(4) 0.013(3) 0.018(3) 0.022(3) C10 0.043(3) 0.043(3) 0.046(3) 0.015(2) 0.016(2) 0.017(2) C11 0.045(3) 0.048(3) 0.049(3) 0.016(2) 0.016(3) 0.019(3) C12 0.047(3) 0.057(3) 0.055(3) 0.014(3) 0.024(3) 0.014(3) C13 0.080(5) 0.087(5) 0.064(4) 0.031(4) 0.038(4) 0.024(4) C14 0.051(4) 0.061(4) 0.061(4) 0.009(3) 0.027(3) 0.021(3) C15 0.046(3) 0.052(3) 0.059(4) 0.003(3) 0.015(3) 0.020(3) C16 0.090(6) 0.067(4) 0.086(5) 0.019(4) 0.022(4) 0.044(4) C17 0.057(4) 0.057(4) 0.065(4) 0.029(3) 0.023(3) 0.026(3) C18 0.086(5) 0.060(4) 0.090(5) 0.035(4) 0.030(4) 0.018(4) C19 0.077(4) 0.070(4) 0.062(4) 0.037(3) 0.030(3) 0.040(4) C20 0.054(4) 0.064(4) 0.052(3) 0.025(3) 0.017(3) 0.032(3) C21 0.098(6) 0.079(5) 0.049(4) 0.026(3) 0.020(4) 0.039(4) C22 0.044(3) 0.047(3) 0.051(3) 0.019(3) 0.020(3) 0.019(2) C23 0.039(3) 0.046(3) 0.043(3) 0.019(2) 0.013(2) 0.016(2) C24 0.050(3) 0.047(3) 0.052(3) 0.010(3) 0.007(3) 0.019(3) C25 0.055(3) 0.041(3) 0.052(3) 0.010(2) 0.011(3) 0.024(3) C26 0.043(3) 0.040(3) 0.050(3) 0.019(2) 0.019(2) 0.018(2) C27 0.038(3) 0.032(3) 0.060(3) 0.012(2) 0.014(3) 0.011(2) C28 0.033(3) 0.053(3) 0.048(3) 0.018(2) 0.015(2) 0.010(2) C29 0.072(4) 0.060(4) 0.083(5) 0.026(4) 0.046(4) 0.014(3) C30 0.037(3) 0.054(3) 0.061(3) 0.019(3) 0.021(3) 0.019(3) C31 0.033(3) 0.046(3) 0.057(3) 0.017(2) 0.017(2) 0.018(2) C32 0.059(4) 0.061(4) 0.086(5) 0.035(3) 0.029(4) 0.034(3) C33 0.152(10) 0.096(7) 0.103(7) 0.049(6) 0.069(7) 0.014(6) N1 0.045(3) 0.038(2) 0.057(3) 0.015(2) 0.025(2) 0.011(2) N2 0.038(3) 0.043(2) 0.061(3) 0.013(2) 0.024(2) 0.008(2) N3 0.033(2) 0.047(2) 0.049(2) 0.015(2) 0.017(2) 0.016(2) N4 0.044(3) 0.045(2) 0.045(2) 0.012(2) 0.016(2) 0.017(2) N5 0.044(3) 0.044(2) 0.048(3) 0.012(2) 0.013(2) 0.018(2) N6 0.047(3) 0.048(3) 0.049(3) 0.018(2) 0.016(2) 0.019(2) N7 0.044(3) 0.049(3) 0.049(3) 0.021(2) 0.015(2) 0.025(2) N8 0.046(3) 0.037(2) 0.045(3) 0.0107(19) 0.015(2) 0.016(2) N9 0.033(2) 0.039(2) 0.053(3) 0.016(2) 0.015(2) 0.0113(18) N10 0.037(2) 0.046(2) 0.055(3) 0.020(2) 0.020(2) 0.017(2) O1 0.095(5) 0.075(4) 0.129(6) 0.060(4) 0.008(4) 0.029(4) O1' 0.095(5) 0.075(4) 0.129(6) 0.060(4) 0.008(4) 0.029(4) O2 0.187(10) 0.218(9) 0.136(7) 0.142(7) 0.110(7) 0.160(9) O2' 0.187(10) 0.218(9) 0.136(7) 0.142(7) 0.110(7) 0.160(9) Cl1 0.0481(8) 0.0458(7) 0.0641(9) 0.0045(6) 0.0255(7) 0.0088(6) Cl2 0.0438(8) 0.0590(9) 0.0552(8) 0.0089(7) 0.0156(6) 0.0082(6) Cl3 0.0388(7) 0.0666(9) 0.0637(9) 0.0216(7) 0.0172(7) 0.0185(7) Cl4 0.0435(8) 0.0774(10) 0.0652(9) 0.0283(8) 0.0190(7) 0.0297(7) Cl5 0.140(3) 0.203(3) 0.134(2) 0.095(3) 0.062(2) 0.085(3) Cl6 0.182(4) 0.177(3) 0.187(3) 0.113(3) 0.091(3) 0.097(3) Pd1 0.0344(2) 0.0390(2) 0.0525(3) 0.01361(18) 0.01981(19) 0.01113(17) Pd2 0.0378(2) 0.0457(3) 0.0471(2) 0.01584(19) 0.01406(19) 0.01817(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.497(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.330(7) . ? C2 C3 1.386(9) . ? C3 C4 1.353(10) . ? C3 H3 0.9300 . ? C4 N2 1.356(7) . ? C4 C5 1.495(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.462(8) . ? C6 C7 1.485(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.351(7) . ? C7 C8 1.365(8) . ? C8 C9 1.411(9) . ? C8 H8 0.9300 . ? C9 C10 1.344(8) . ? C9 H9 0.9300 . ? C10 N3 1.359(7) . ? C10 C11 1.501(7) . ? C11 N4 1.454(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.352(7) . ? C12 C14 1.372(9) . ? C12 C13 1.493(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.393(9) . ? C14 H14 0.9300 . ? C15 N5 1.354(7) . ? C15 C16 1.485(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.338(7) . ? C17 C19 1.383(9) . ? C17 C18 1.486(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.373(9) . ? C19 H19 0.9300 . ? C20 N7 1.346(7) . ? C20 C21 1.501(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N7 1.456(7) . ? C22 C23 1.497(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.348(8) . ? C23 N8 1.367(7) . ? C24 C25 1.421(8) . ? C24 H24 0.9300 . ? C25 C26 1.352(8) . ? C25 H25 0.9300 . ? C26 N8 1.355(7) . ? C26 C27 1.496(7) . ? C27 N9 1.445(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N9 1.349(6) . ? C28 C30 1.384(8) . ? C28 C29 1.495(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.386(8) . ? C30 H30 0.9300 . ? C31 N10 1.336(6) . ? C31 C32 1.482(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 Cl6 1.711(11) . ? C33 Cl5 1.731(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? N1 N2 1.353(6) . ? N1 Pd1 2.004(4) . ? N3 H1 0.71(4) . ? N4 N5 1.355(6) . ? N5 Pd2 2.021(4) . ? N6 N7 1.355(6) . ? N6 Pd2 2.009(4) . ? N8 H2 0.70(4) . ? N9 N10 1.371(6) . ? N10 Pd1 2.022(4) . ? O1' O2' 1.42(6) 1_556 ? O2' O1' 1.42(6) 1_554 ? Cl1 Pd1 2.3119(14) . ? Cl2 Pd1 2.3031(15) . ? Cl3 Pd2 2.3197(14) . ? Cl4 Pd2 2.2960(15) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.4(6) . . ? N1 C2 C1 121.2(6) . . ? C3 C2 C1 130.3(6) . . ? C4 C3 C2 107.6(6) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? C3 C4 N2 106.8(6) . . ? C3 C4 C5 132.5(6) . . ? N2 C4 C5 120.7(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 113.4(5) . . ? N2 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N2 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N3 C7 C8 107.3(5) . . ? N3 C7 C6 122.1(5) . . ? C8 C7 C6 130.5(5) . . ? C7 C8 C9 106.9(5) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? C10 C9 C8 108.0(5) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? C9 C10 N3 107.5(5) . . ? C9 C10 C11 131.0(5) . . ? N3 C10 C11 121.5(5) . . ? N4 C11 C10 110.7(4) . . ? N4 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N4 C12 C14 107.0(5) . . ? N4 C12 C13 122.3(6) . . ? C14 C12 C13 130.6(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C15 106.3(5) . . ? C12 C14 H14 126.8 . . ? C15 C14 H14 126.8 . . ? N5 C15 C14 109.7(6) . . ? N5 C15 C16 121.5(6) . . ? C14 C15 C16 128.8(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C19 109.0(6) . . ? N6 C17 C18 120.9(6) . . ? C19 C17 C18 130.1(6) . . ? 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 . . ? C20 C19 C17 106.8(5) . . ? C20 C19 H19 126.6 . . ? C17 C19 H19 126.6 . . ? N7 C20 C19 106.8(5) . . ? N7 C20 C21 121.8(6) . . ? C19 C20 C21 131.3(6) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C22 C23 112.3(4) . . ? N7 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N7 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C24 C23 N8 107.5(5) . . ? C24 C23 C22 130.3(5) . . ? N8 C23 C22 122.2(5) . . ? C23 C24 C25 107.4(5) . . ? C23 C24 H24 126.3 . . ? C25 C24 H24 126.3 . . ? C26 C25 C24 107.5(5) . . ? C26 C25 H25 126.2 . . ? C24 C25 H25 126.2 . . ? C25 C26 N8 107.6(5) . . ? C25 C26 C27 132.1(5) . . ? N8 C26 C27 120.2(5) . . ? N9 C27 C26 112.9(4) . . ? N9 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? N9 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? N9 C28 C30 106.4(5) . . ? N9 C28 C29 123.3(5) . . ? C30 C28 C29 130.3(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 C31 107.1(5) . . ? C28 C30 H30 126.5 . . ? C31 C30 H30 126.5 . . ? N10 C31 C30 109.3(5) . . ? N10 C31 C32 122.5(5) . . ? C30 C31 C32 128.1(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl6 C33 Cl5 113.3(5) . . ? Cl6 C33 H33A 108.9 . . ? Cl5 C33 H33A 108.9 . . ? Cl6 C33 H33B 108.9 . . ? Cl5 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C2 N1 N2 107.5(5) . . ? C2 N1 Pd1 125.8(4) . . ? N2 N1 Pd1 125.8(4) . . ? N1 N2 C4 109.7(5) . . ? N1 N2 C6 120.1(4) . . ? C4 N2 C6 129.6(5) . . ? C7 N3 C10 110.3(4) . . ? C7 N3 H1 124(5) . . ? C10 N3 H1 125(5) . . ? C12 N4 N5 111.3(4) . . ? C12 N4 C11 126.3(5) . . ? N5 N4 C11 122.3(4) . . ? C15 N5 N4 105.7(5) . . ? C15 N5 Pd2 127.4(4) . . ? N4 N5 Pd2 124.2(3) . . ? C17 N6 N7 107.0(5) . . ? C17 N6 Pd2 128.6(4) . . ? N7 N6 Pd2 124.2(3) . . ? C20 N7 N6 110.4(5) . . ? C20 N7 C22 127.5(5) . . ? N6 N7 C22 121.7(4) . . ? C26 N8 C23 110.0(4) . . ? C26 N8 H2 126(6) . . ? C23 N8 H2 124(6) . . ? C28 N9 N10 110.5(4) . . ? C28 N9 C27 127.7(4) . . ? N10 N9 C27 121.5(4) . . ? C31 N10 N9 106.7(4) . . ? C31 N10 Pd1 125.9(4) . . ? N9 N10 Pd1 127.1(3) . . ? N1 Pd1 N10 174.71(18) . . ? N1 Pd1 Cl2 89.18(13) . . ? N10 Pd1 Cl2 91.80(13) . . ? N1 Pd1 Cl1 87.47(13) . . ? N10 Pd1 Cl1 91.59(13) . . ? Cl2 Pd1 Cl1 176.60(5) . . ? N6 Pd2 N5 177.17(18) . . ? N6 Pd2 Cl4 88.27(14) . . ? N5 Pd2 Cl4 89.68(13) . . ? N6 Pd2 Cl3 89.20(14) . . ? N5 Pd2 Cl3 92.90(13) . . ? Cl4 Pd2 Cl3 176.90(6) . . ? 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 N1 C2 C3 C4 -0.8(8) . . . . ? C1 C2 C3 C4 -179.4(7) . . . . ? C2 C3 C4 N2 0.0(8) . . . . ? C2 C3 C4 C5 -179.8(8) . . . . ? N2 C6 C7 N3 -70.0(7) . . . . ? N2 C6 C7 C8 110.2(7) . . . . ? N3 C7 C8 C9 -1.5(7) . . . . ? C6 C7 C8 C9 178.3(6) . . . . ? C7 C8 C9 C10 1.7(8) . . . . ? C8 C9 C10 N3 -1.1(7) . . . . ? C8 C9 C10 C11 179.4(6) . . . . ? C9 C10 C11 N4 4.2(9) . . . . ? N3 C10 C11 N4 -175.2(5) . . . . ? N4 C12 C14 C15 0.0(7) . . . . ? C13 C12 C14 C15 177.7(6) . . . . ? C12 C14 C15 N5 -0.1(7) . . . . ? C12 C14 C15 C16 178.4(6) . . . . ? N6 C17 C19 C20 1.1(7) . . . . ? C18 C17 C19 C20 -179.8(7) . . . . ? C17 C19 C20 N7 -1.4(7) . . . . ? C17 C19 C20 C21 176.6(6) . . . . ? N7 C22 C23 C24 113.5(7) . . . . ? N7 C22 C23 N8 -66.1(7) . . . . ? N8 C23 C24 C25 -0.1(6) . . . . ? C22 C23 C24 C25 -179.8(5) . . . . ? C23 C24 C25 C26 0.4(7) . . . . ? C24 C25 C26 N8 -0.6(6) . . . . ? C24 C25 C26 C27 -178.2(6) . . . . ? C25 C26 C27 N9 3.3(9) . . . . ? N8 C26 C27 N9 -174.0(5) . . . . ? N9 C28 C30 C31 0.4(6) . . . . ? C29 C28 C30 C31 -178.0(6) . . . . ? C28 C30 C31 N10 -0.2(6) . . . . ? C28 C30 C31 C32 177.3(6) . . . . ? C3 C2 N1 N2 1.3(7) . . . . ? C1 C2 N1 N2 -179.9(6) . . . . ? C3 C2 N1 Pd1 170.6(4) . . . . ? C1 C2 N1 Pd1 -10.6(8) . . . . ? C2 N1 N2 C4 -1.3(6) . . . . ? Pd1 N1 N2 C4 -170.7(4) . . . . ? C2 N1 N2 C6 -173.7(5) . . . . ? Pd1 N1 N2 C6 17.0(6) . . . . ? C3 C4 N2 N1 0.8(7) . . . . ? C5 C4 N2 N1 -179.4(6) . . . . ? C3 C4 N2 C6 172.2(6) . . . . ? C5 C4 N2 C6 -8.0(10) . . . . ? C7 C6 N2 N1 92.9(6) . . . . ? C7 C6 N2 C4 -77.7(7) . . . . ? C8 C7 N3 C10 0.9(7) . . . . ? C6 C7 N3 C10 -178.9(5) . . . . ? C9 C10 N3 C7 0.2(7) . . . . ? C11 C10 N3 C7 179.7(5) . . . . ? C14 C12 N4 N5 0.0(6) . . . . ? C13 C12 N4 N5 -177.9(5) . . . . ? C14 C12 N4 C11 -176.8(5) . . . . ? C13 C12 N4 C11 5.2(9) . . . . ? C10 C11 N4 C12 -97.9(6) . . . . ? C10 C11 N4 N5 85.6(6) . . . . ? C14 C15 N5 N4 0.1(6) . . . . ? C16 C15 N5 N4 -178.5(6) . . . . ? C14 C15 N5 Pd2 -161.8(4) . . . . ? C16 C15 N5 Pd2 19.7(8) . . . . ? C12 N4 N5 C15 -0.1(6) . . . . ? C11 N4 N5 C15 176.9(5) . . . . ? C12 N4 N5 Pd2 162.5(4) . . . . ? C11 N4 N5 Pd2 -20.5(6) . . . . ? C19 C17 N6 N7 -0.3(7) . . . . ? C18 C17 N6 N7 -179.5(6) . . . . ? C19 C17 N6 Pd2 174.8(4) . . . . ? C18 C17 N6 Pd2 -4.4(9) . . . . ? C19 C20 N7 N6 1.3(6) . . . . ? C21 C20 N7 N6 -177.0(5) . . . . ? C19 C20 N7 C22 173.6(5) . . . . ? C21 C20 N7 C22 -4.7(9) . . . . ? C17 N6 N7 C20 -0.6(6) . . . . ? Pd2 N6 N7 C20 -176.0(4) . . . . ? C17 N6 N7 C22 -173.5(5) . . . . ? Pd2 N6 N7 C22 11.2(6) . . . . ? C23 C22 N7 C20 -73.0(7) . . . . ? C23 C22 N7 N6 98.5(6) . . . . ? C25 C26 N8 C23 0.5(6) . . . . ? C27 C26 N8 C23 178.5(5) . . . . ? C24 C23 N8 C26 -0.3(6) . . . . ? C22 C23 N8 C26 179.4(5) . . . . ? C30 C28 N9 N10 -0.5(6) . . . . ? C29 C28 N9 N10 178.1(5) . . . . ? C30 C28 N9 C27 -174.0(5) . . . . ? C29 C28 N9 C27 4.5(9) . . . . ? C26 C27 N9 C28 -114.2(6) . . . . ? C26 C27 N9 N10 72.9(6) . . . . ? C30 C31 N10 N9 0.0(6) . . . . ? C32 C31 N10 N9 -177.8(5) . . . . ? C30 C31 N10 Pd1 -173.4(4) . . . . ? C32 C31 N10 Pd1 8.9(8) . . . . ? C28 N9 N10 C31 0.3(6) . . . . ? C27 N9 N10 C31 174.4(5) . . . . ? C28 N9 N10 Pd1 173.6(4) . . . . ? C27 N9 N10 Pd1 -12.4(7) . . . . ? C2 N1 Pd1 N10 -17(2) . . . . ? N2 N1 Pd1 N10 150.1(18) . . . . ? C2 N1 Pd1 Cl2 83.4(5) . . . . ? N2 N1 Pd1 Cl2 -109.1(4) . . . . ? C2 N1 Pd1 Cl1 -97.1(5) . . . . ? N2 N1 Pd1 Cl1 70.3(4) . . . . ? C31 N10 Pd1 N1 -20(2) . . . . ? N9 N10 Pd1 N1 167.9(18) . . . . ? C31 N10 Pd1 Cl2 -120.7(4) . . . . ? N9 N10 Pd1 Cl2 67.3(4) . . . . ? C31 N10 Pd1 Cl1 59.6(4) . . . . ? N9 N10 Pd1 Cl1 -112.4(4) . . . . ? C17 N6 Pd2 N5 -60(4) . . . . ? N7 N6 Pd2 N5 115(4) . . . . ? C17 N6 Pd2 Cl4 -103.4(5) . . . . ? N7 N6 Pd2 Cl4 71.0(4) . . . . ? C17 N6 Pd2 Cl3 78.4(5) . . . . ? N7 N6 Pd2 Cl3 -107.3(4) . . . . ? C15 N5 Pd2 N6 10(4) . . . . ? N4 N5 Pd2 N6 -149(4) . . . . ? C15 N5 Pd2 Cl4 53.9(5) . . . . ? N4 N5 Pd2 Cl4 -104.8(4) . . . . ? C15 N5 Pd2 Cl3 -127.8(5) . . . . ? N4 N5 Pd2 Cl3 73.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H1 Cl2 0.71(4) 2.67(5) 3.344(5) 160(6) . N8 H2 Cl3 0.70(4) 2.75(5) 3.453(5) 176(7) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.954 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.116 #================================================================END