# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Manda Curic' _publ_contact_author_email manda.curic@irb.hr _publ_section_title ; Unusual azobenzene/bipyridine palladacycles: structural, dynamical, photophysical and theoretical studies ; _publ_author_name 'Manda Curic' # Attachment '- 1a.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_mand26 _database_code_depnum_ccdc_archive 'CCDC 746371' #TrackingRef '- 1a.cif' _audit_creation_date 2009-09-02T13:00:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C22 H16 N4 Cl2 Pd2' _chemical_formula_sum 'C22 H16 Cl2 N4 Pd2' _chemical_formula_weight 619.32 #------------------ UNIT CELL INFORMATION -----------------------------------# _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 10.2884(5) _cell_length_b 10.6609(8) _cell_length_c 11.6302(5) _cell_angle_alpha 107.874(5) _cell_angle_beta 100.279(4) _cell_angle_gamma 114.137(5) _cell_volume 1037.86(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 8.3 _cell_measurement_theta_max 20.1 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 16.488 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.0239 _exptl_absorpt_correction_T_max 0.0971 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_ambient_temperature 293(2) _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 -2 0 -2 4 4 -3 -2 _diffrn_reflns_number 4587 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 76.2 _diffrn_reflns_theta_full 76.2 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 4336 _reflns_number_gt 3188 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0833P)^2^+1.7382P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4336 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1441 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0 _refine_diff_density_max 1.115 _refine_diff_density_min -2.43 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.031 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.122 3.934 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.364 0.702 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd1 Pd 0.03107(6) 0.12482(6) 0.17935(5) 0.01998(17) Uani 1 d . . . Pd2 Pd -0.10186(6) 0.11419(6) 0.40641(5) 0.01895(16) Uani 1 d . . . Cl1 Cl 0.0635(2) 0.0338(2) 0.34885(19) 0.0301(4) Uani 1 d . . . N2 N -0.2677(8) 0.0276(8) 0.0165(6) 0.0270(15) Uani 1 d . . . N4 N -0.2418(7) 0.1953(7) 0.4552(6) 0.0240(14) Uani 1 d . . . N1 N -0.1998(7) 0.0058(7) 0.1056(6) 0.0206(13) Uani 1 d . . . N3 N 0.0577(7) 0.3286(7) 0.5565(6) 0.0233(14) Uani 1 d . . . C18 C -0.1726(9) 0.3395(9) 0.5490(7) 0.0205(16) Uani 1 d . . . C17 C -0.0070(9) 0.4120(9) 0.6070(7) 0.0223(16) Uani 1 d . . . C2 C -0.0088(9) 0.1954(9) 0.0469(7) 0.0228(17) Uani 1 d . . . C13 C 0.2081(9) 0.3907(10) 0.6017(9) 0.037(2) Uani 1 d . . . H13 H 0.2514 0.3352 0.5643 0.044 Uiso 1 calc R . . C20 C -0.4092(10) 0.3354(11) 0.5235(9) 0.037(2) Uani 1 d . . . H20 H -0.4648 0.3838 0.5442 0.044 Uiso 1 calc R . . C1 C -0.1658(10) 0.1325(9) -0.0165(8) 0.0261(18) Uani 1 d . . . C22 C -0.3948(9) 0.1225(10) 0.3985(8) 0.031(2) Uani 1 d . . . H22 H -0.4441 0.0235 0.3352 0.037 Uiso 1 calc R . . C21 C -0.4793(10) 0.1893(12) 0.4309(10) 0.040(2) Uani 1 d . . . H21 H -0.5844 0.1358 0.3902 0.048 Uiso 1 calc R . . C19 C -0.2532(10) 0.4090(11) 0.5852(9) 0.035(2) Uani 1 d . . . H19 H -0.2036 0.5061 0.6517 0.042 Uiso 1 calc R . . C15 C 0.2403(10) 0.6155(10) 0.7531(8) 0.038(2) Uani 1 d . . . H15 H 0.3022 0.712 0.8199 0.046 Uiso 1 calc R . . C14 C 0.3028(10) 0.5321(11) 0.7008(9) 0.037(2) Uani 1 d . . . H14 H 0.4073 0.5701 0.7314 0.045 Uiso 1 calc R . . C16 C 0.0833(10) 0.5561(9) 0.7065(8) 0.0270(18) Uani 1 d . . . H16 H 0.0397 0.6125 0.7417 0.032 Uiso 1 calc R . . C3 C 0.0871(12) 0.2962(10) 0.0092(10) 0.039(2) Uani 1 d . . . H3 H 0.1916 0.3387 0.0471 0.047 Uiso 1 calc R . . C6 C -0.2217(12) 0.1748(12) -0.1071(9) 0.041(2) Uani 1 d . . . H6 H -0.3259 0.135 -0.1441 0.05 Uiso 1 calc R . . C4 C 0.0322(13) 0.3363(12) -0.0838(10) 0.051(3) Uani 1 d . . . H4 H 0.1001 0.4044 -0.1073 0.062 Uiso 1 calc R . . C5 C -0.1219(14) 0.2757(13) -0.1413(11) 0.053(3) Uani 1 d . . . H5 H -0.158 0.3033 -0.2032 0.064 Uiso 1 calc R . . C7 C -0.2972(8) -0.1064(8) 0.1393(7) 0.0217(16) Uani 1 d . . . C8 C -0.2679(9) -0.0795(8) 0.2678(7) 0.0222(16) Uani 1 d . . . C12 C -0.4218(10) -0.2392(10) 0.0395(9) 0.035(2) Uani 1 d . . . H12 H -0.4385 -0.2539 -0.0461 0.042 Uiso 1 calc R . . C9 C -0.3685(11) -0.1943(10) 0.2941(8) 0.034(2) Uani 1 d . . . H9 H -0.351 -0.1815 0.3792 0.041 Uiso 1 calc R . . C11 C -0.5183(10) -0.3468(10) 0.0704(9) 0.036(2) Uani 1 d . . . H11 H -0.602 -0.4351 0.0057 0.043 Uiso 1 calc R . . C10 C -0.4910(11) -0.3238(10) 0.1992(10) 0.040(2) Uani 1 d . . . H10 H -0.5562 -0.3969 0.2203 0.048 Uiso 1 calc R . . Cl2 Cl 0.2908(2) 0.2789(2) 0.2497(2) 0.0369(5) Uani 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 Pd1 0.0145(3) 0.0184(3) 0.0198(3) 0.0049(2) 0.0013(2) 0.0061(2) Pd2 0.0164(3) 0.0179(3) 0.0141(3) 0.0037(2) -0.0010(2) 0.0060(2) Cl1 0.0305(11) 0.0397(11) 0.0263(10) 0.0136(9) 0.0070(8) 0.0242(10) N2 0.024(4) 0.030(4) 0.019(3) 0.007(3) 0.001(3) 0.012(3) N4 0.018(3) 0.022(3) 0.024(4) 0.008(3) 0.000(3) 0.009(3) N1 0.018(3) 0.023(3) 0.017(3) 0.007(3) 0.003(3) 0.009(3) N3 0.018(3) 0.026(3) 0.012(3) 0.003(3) -0.006(3) 0.007(3) C18 0.022(4) 0.030(4) 0.017(4) 0.013(3) 0.006(3) 0.017(3) C17 0.025(4) 0.025(4) 0.018(4) 0.011(3) 0.003(3) 0.012(3) C2 0.022(4) 0.020(4) 0.017(4) 0.005(3) -0.001(3) 0.007(3) C13 0.014(4) 0.034(5) 0.034(5) 0.003(4) -0.005(4) 0.001(4) C20 0.028(5) 0.049(6) 0.042(6) 0.017(5) 0.012(4) 0.028(5) C1 0.029(4) 0.021(4) 0.020(4) 0.004(3) 0.004(3) 0.011(4) C22 0.012(4) 0.037(5) 0.030(5) 0.002(4) 0.003(3) 0.011(4) C21 0.021(5) 0.049(6) 0.046(6) 0.019(5) 0.013(4) 0.015(4) C19 0.032(5) 0.035(5) 0.029(5) 0.007(4) 0.004(4) 0.017(4) C15 0.031(5) 0.024(5) 0.023(4) -0.005(4) -0.008(4) -0.001(4) C14 0.020(4) 0.039(5) 0.029(5) 0.005(4) -0.003(4) 0.006(4) C16 0.028(4) 0.027(4) 0.020(4) 0.002(3) 0.003(3) 0.016(4) C3 0.038(5) 0.031(5) 0.047(6) 0.024(4) 0.013(5) 0.013(4) C6 0.042(6) 0.049(6) 0.030(5) 0.021(5) -0.001(4) 0.021(5) C4 0.055(7) 0.048(6) 0.045(6) 0.030(5) 0.015(5) 0.013(6) C5 0.062(7) 0.057(7) 0.043(6) 0.039(6) 0.009(5) 0.022(6) C7 0.013(4) 0.018(4) 0.021(4) 0.005(3) 0.000(3) 0.001(3) C8 0.022(4) 0.017(4) 0.020(4) 0.006(3) 0.001(3) 0.006(3) C12 0.026(5) 0.026(5) 0.023(4) 0.000(4) 0.001(4) -0.001(4) C9 0.045(6) 0.026(5) 0.024(4) 0.011(4) 0.008(4) 0.012(4) C11 0.019(4) 0.021(4) 0.039(5) 0.001(4) -0.002(4) -0.002(4) C10 0.032(5) 0.023(5) 0.052(6) 0.021(4) 0.008(5) 0.001(4) Cl2 0.0133(9) 0.0344(11) 0.0473(13) 0.0121(10) 0.0016(9) 0.0058(8) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.960(8) . ? Pd1 N1 2.032(6) . ? Pd1 Cl2 2.305(2) . ? Pd1 Cl1 2.478(2) . ? Pd1 Pd2 3.1942(8) . ? Pd2 C8 1.967(7) . ? Pd2 N4 2.037(7) . ? Pd2 N3 2.104(6) . ? Pd2 Cl1 2.307(2) . ? N2 N1 1.279(9) . ? N2 C1 1.395(11) . ? N4 C22 1.354(10) . ? N4 C18 1.363(10) . ? N1 C7 1.427(10) . ? N3 C13 1.329(10) . ? N3 C17 1.371(10) . ? C18 C19 1.360(11) . ? C18 C17 1.466(10) . ? C17 C16 1.386(11) . ? C2 C3 1.377(12) . ? C2 C1 1.411(11) . ? C13 C14 1.372(12) . ? C13 H13 0.93 . ? C20 C21 1.371(13) . ? C20 C19 1.386(12) . ? C20 H20 0.93 . ? C1 C6 1.389(11) . ? C22 C21 1.366(12) . ? C22 H22 0.93 . ? C21 H21 0.93 . ? C19 H19 0.93 . ? C15 C14 1.360(13) . ? C15 C16 1.395(12) . ? C15 H15 0.93 . ? C14 H14 0.93 . ? C16 H16 0.93 . ? C3 C4 1.391(14) . ? C3 H3 0.93 . ? C6 C5 1.370(14) . ? C6 H6 0.93 . ? C4 C5 1.377(15) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C7 C8 1.383(11) . ? C7 C12 1.403(10) . ? C8 C9 1.404(11) . ? C12 C11 1.372(13) . ? C12 H12 0.93 . ? C9 C10 1.363(12) . ? C9 H9 0.93 . ? C11 C10 1.397(14) . ? C11 H11 0.93 . ? C10 H10 0.93 . ? 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 Pd1 N1 79.3(3) . . ? C2 Pd1 Cl2 93.6(2) . . ? N1 Pd1 Cl2 172.63(19) . . ? C2 Pd1 Cl1 175.7(2) . . ? N1 Pd1 Cl1 97.11(19) . . ? Cl2 Pd1 Cl1 89.93(8) . . ? C2 Pd1 Pd2 130.1(2) . . ? N1 Pd1 Pd2 70.04(18) . . ? Cl2 Pd1 Pd2 114.05(7) . . ? Cl1 Pd1 Pd2 45.87(5) . . ? C8 Pd2 N4 94.4(3) . . ? C8 Pd2 N3 173.7(3) . . ? N4 Pd2 N3 79.4(3) . . ? C8 Pd2 Cl1 87.3(2) . . ? N4 Pd2 Cl1 176.8(2) . . ? N3 Pd2 Cl1 98.94(19) . . ? C8 Pd2 Pd1 81.8(2) . . ? N4 Pd2 Pd1 127.05(19) . . ? N3 Pd2 Pd1 101.32(19) . . ? Cl1 Pd2 Pd1 50.46(5) . . ? Pd2 Cl1 Pd1 83.67(7) . . ? N1 N2 C1 112.2(7) . . ? C22 N4 C18 117.6(7) . . ? C22 N4 Pd2 126.0(6) . . ? C18 N4 Pd2 116.3(5) . . ? N2 N1 C7 115.1(6) . . ? N2 N1 Pd1 118.2(5) . . ? C7 N1 Pd1 126.6(5) . . ? C13 N3 C17 118.7(7) . . ? C13 N3 Pd2 128.0(6) . . ? C17 N3 Pd2 113.2(5) . . ? C19 C18 N4 121.7(7) . . ? C19 C18 C17 123.2(7) . . ? N4 C18 C17 115.0(7) . . ? N3 C17 C16 120.2(7) . . ? N3 C17 C18 116.0(7) . . ? C16 C17 C18 123.8(7) . . ? C3 C2 C1 116.0(8) . . ? C3 C2 Pd1 131.9(7) . . ? C1 C2 Pd1 112.0(6) . . ? N3 C13 C14 123.6(9) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C21 C20 C19 118.1(9) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C6 C1 N2 119.3(8) . . ? C6 C1 C2 122.4(8) . . ? N2 C1 C2 118.3(7) . . ? N4 C22 C21 122.3(8) . . ? N4 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C22 C21 C20 120.0(8) . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C18 C19 C20 120.2(8) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C14 C15 C16 120.0(8) . . ? C14 C15 H15 120 . . ? C16 C15 H15 120 . . ? C15 C14 C13 118.4(8) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C17 C16 C15 119.1(8) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C2 C3 C4 121.9(9) . . ? C2 C3 H3 119 . . ? C4 C3 H3 119 . . ? C5 C6 C1 119.3(9) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C5 C4 C3 120.5(10) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.7(9) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C8 C7 C12 122.7(8) . . ? C8 C7 N1 119.3(6) . . ? C12 C7 N1 118.0(7) . . ? C7 C8 C9 116.3(7) . . ? C7 C8 Pd2 121.7(6) . . ? C9 C8 Pd2 121.9(6) . . ? C11 C12 C7 118.8(8) . . ? C11 C12 H12 120.6 . . ? C7 C12 H12 120.6 . . ? C10 C9 C8 122.3(8) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C12 C11 C10 120.0(8) . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C9 C10 C11 119.9(8) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? 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 Pd1 Pd2 C8 84.8(4) . . . . ? N1 Pd1 Pd2 C8 29.2(3) . . . . ? Cl2 Pd1 Pd2 C8 -157.4(2) . . . . ? Cl1 Pd1 Pd2 C8 -93.2(2) . . . . ? C2 Pd1 Pd2 N4 -4.6(4) . . . . ? N1 Pd1 Pd2 N4 -60.1(3) . . . . ? Cl2 Pd1 Pd2 N4 113.2(2) . . . . ? Cl1 Pd1 Pd2 N4 177.5(2) . . . . ? C2 Pd1 Pd2 N3 -89.7(3) . . . . ? N1 Pd1 Pd2 N3 -145.3(3) . . . . ? Cl2 Pd1 Pd2 N3 28.08(19) . . . . ? Cl1 Pd1 Pd2 N3 92.31(19) . . . . ? C2 Pd1 Pd2 Cl1 178.0(3) . . . . ? N1 Pd1 Pd2 Cl1 122.4(2) . . . . ? Cl2 Pd1 Pd2 Cl1 -64.23(10) . . . . ? C8 Pd2 Cl1 Pd1 81.7(2) . . . . ? N4 Pd2 Cl1 Pd1 -39(3) . . . . ? N3 Pd2 Cl1 Pd1 -97.34(19) . . . . ? C2 Pd1 Cl1 Pd2 -21(3) . . . . ? N1 Pd1 Cl1 Pd2 -53.12(19) . . . . ? Cl2 Pd1 Cl1 Pd2 124.68(8) . . . . ? C8 Pd2 N4 C22 -0.3(8) . . . . ? N3 Pd2 N4 C22 179.0(7) . . . . ? Cl1 Pd2 N4 C22 121(3) . . . . ? Pd1 Pd2 N4 C22 82.8(7) . . . . ? C8 Pd2 N4 C18 -176.5(6) . . . . ? N3 Pd2 N4 C18 2.8(5) . . . . ? Cl1 Pd2 N4 C18 -56(4) . . . . ? Pd1 Pd2 N4 C18 -93.5(5) . . . . ? C1 N2 N1 C7 -176.8(7) . . . . ? C1 N2 N1 Pd1 0.8(9) . . . . ? C2 Pd1 N1 N2 -2.0(6) . . . . ? Cl2 Pd1 N1 N2 13.1(19) . . . . ? Cl1 Pd1 N1 N2 175.7(5) . . . . ? Pd2 Pd1 N1 N2 138.0(6) . . . . ? C2 Pd1 N1 C7 175.3(7) . . . . ? Cl2 Pd1 N1 C7 -169.5(11) . . . . ? Cl1 Pd1 N1 C7 -7.0(6) . . . . ? Pd2 Pd1 N1 C7 -44.6(6) . . . . ? C8 Pd2 N3 C13 -172(2) . . . . ? N4 Pd2 N3 C13 -178.6(8) . . . . ? Cl1 Pd2 N3 C13 -1.4(8) . . . . ? Pd1 Pd2 N3 C13 -52.7(8) . . . . ? C8 Pd2 N3 C17 5(3) . . . . ? N4 Pd2 N3 C17 -1.3(5) . . . . ? Cl1 Pd2 N3 C17 175.9(5) . . . . ? Pd1 Pd2 N3 C17 124.6(5) . . . . ? C22 N4 C18 C19 0.1(12) . . . . ? Pd2 N4 C18 C19 176.6(7) . . . . ? C22 N4 C18 C17 179.8(7) . . . . ? Pd2 N4 C18 C17 -3.7(8) . . . . ? C13 N3 C17 C16 -2.3(12) . . . . ? Pd2 N3 C17 C16 -179.8(6) . . . . ? C13 N3 C17 C18 177.4(8) . . . . ? Pd2 N3 C17 C18 -0.2(8) . . . . ? C19 C18 C17 N3 -177.8(8) . . . . ? N4 C18 C17 N3 2.5(10) . . . . ? C19 C18 C17 C16 1.9(13) . . . . ? N4 C18 C17 C16 -177.8(8) . . . . ? N1 Pd1 C2 C3 -179.7(9) . . . . ? Cl2 Pd1 C2 C3 2.2(9) . . . . ? Cl1 Pd1 C2 C3 148(3) . . . . ? Pd2 Pd1 C2 C3 128.1(8) . . . . ? N1 Pd1 C2 C1 2.6(6) . . . . ? Cl2 Pd1 C2 C1 -175.5(5) . . . . ? Cl1 Pd1 C2 C1 -30(3) . . . . ? Pd2 Pd1 C2 C1 -49.5(7) . . . . ? C17 N3 C13 C14 2.9(14) . . . . ? Pd2 N3 C13 C14 -179.9(7) . . . . ? N1 N2 C1 C6 -176.6(8) . . . . ? N1 N2 C1 C2 1.5(10) . . . . ? C3 C2 C1 C6 -3.2(13) . . . . ? Pd1 C2 C1 C6 174.9(7) . . . . ? C3 C2 C1 N2 178.8(8) . . . . ? Pd1 C2 C1 N2 -3.1(9) . . . . ? C18 N4 C22 C21 1.0(13) . . . . ? Pd2 N4 C22 C21 -175.2(7) . . . . ? N4 C22 C21 C20 0.3(15) . . . . ? C19 C20 C21 C22 -2.5(15) . . . . ? N4 C18 C19 C20 -2.3(14) . . . . ? C17 C18 C19 C20 178.0(8) . . . . ? C21 C20 C19 C18 3.5(15) . . . . ? C16 C15 C14 C13 0.5(15) . . . . ? N3 C13 C14 C15 -2.0(16) . . . . ? N3 C17 C16 C15 0.8(12) . . . . ? C18 C17 C16 C15 -178.9(8) . . . . ? C14 C15 C16 C17 0.1(14) . . . . ? C1 C2 C3 C4 1.4(14) . . . . ? Pd1 C2 C3 C4 -176.2(8) . . . . ? N2 C1 C6 C5 -178.8(9) . . . . ? C2 C1 C6 C5 3.2(15) . . . . ? C2 C3 C4 C5 0.3(17) . . . . ? C1 C6 C5 C4 -1.4(18) . . . . ? C3 C4 C5 C6 -0.3(19) . . . . ? N2 N1 C7 C8 -138.4(8) . . . . ? Pd1 N1 C7 C8 44.2(10) . . . . ? N2 N1 C7 C12 40.1(10) . . . . ? Pd1 N1 C7 C12 -137.3(7) . . . . ? C12 C7 C8 C9 1.2(13) . . . . ? N1 C7 C8 C9 179.7(8) . . . . ? C12 C7 C8 Pd2 -175.2(7) . . . . ? N1 C7 C8 Pd2 3.3(11) . . . . ? N4 Pd2 C8 C7 102.5(7) . . . . ? N3 Pd2 C8 C7 96(3) . . . . ? Cl1 Pd2 C8 C7 -74.7(7) . . . . ? Pd1 Pd2 C8 C7 -24.3(6) . . . . ? N4 Pd2 C8 C9 -73.7(8) . . . . ? N3 Pd2 C8 C9 -80(3) . . . . ? Cl1 Pd2 C8 C9 109.1(7) . . . . ? Pd1 Pd2 C8 C9 159.5(8) . . . . ? C8 C7 C12 C11 -0.2(14) . . . . ? N1 C7 C12 C11 -178.6(8) . . . . ? C7 C8 C9 C10 -1.7(14) . . . . ? Pd2 C8 C9 C10 174.7(7) . . . . ? C7 C12 C11 C10 -0.6(15) . . . . ? C8 C9 C10 C11 1.0(15) . . . . ? C12 C11 C10 C9 0.2(15) . . . . ? # Attachment '- 2a.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_manda-c2mabp-dmf _database_code_depnum_ccdc_archive 'CCDC 746372' #TrackingRef '- 2a.cif' _audit_creation_date 2009-05-06T13:16:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C23 H18 Cl2 N4 Pd2' _chemical_formula_sum 'C23 H18 Cl2 N4 Pd2' _chemical_formula_weight 634.11 #------------------ UNIT CELL INFORMATION -----------------------------------# _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 10.0962(4) _cell_length_b 10.9626(3) _cell_length_c 11.9130(5) _cell_angle_alpha 107.167(3) _cell_angle_beta 108.457(3) _cell_angle_gamma 105.761(3) _cell_volume 1093.75(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6565 _cell_measurement_theta_min 4.3025 _cell_measurement_theta_max 76.0688 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 15.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.434 _exptl_absorpt_correction_T_max 0.731 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 9446 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.31 _diffrn_reflns_theta_max 75.0 _diffrn_reflns_theta_full 76.28 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.97 _reflns_number_total 4437 _reflns_number_gt 3720 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.1754P)^2^+1.0105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4437 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2248 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0 _refine_diff_density_max 2.136 _refine_diff_density_min -1.599 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd1 Pd 0.65401(6) 0.06989(5) 0.68784(5) 0.0416(2) Uani 1 d . . . Pd2 Pd 0.98224(6) 0.28354(5) 0.91009(5) 0.0415(2) Uani 1 d . . . Cl1 Cl 0.7568(2) 0.3132(2) 0.85163(18) 0.0502(4) Uani 1 d . . . Cl2 Cl 0.4752(3) 0.0036(2) 0.7638(2) 0.0602(5) Uani 1 d . . . N1 N 0.8057(7) 0.1023(7) 0.6098(6) 0.0441(13) Uani 1 d . . . N2 N 0.7985(8) -0.0020(7) 0.5218(7) 0.0499(15) Uani 1 d . . . N3 N 0.9691(7) 0.2102(7) 1.0543(6) 0.0450(13) Uani 1 d . . . N4 N 1.1843(7) 0.2613(7) 0.9712(6) 0.0457(14) Uani 1 d . . . C1 C 0.6813(9) -0.1243(8) 0.4905(8) 0.0468(16) Uani 1 d . . . C2 C 0.5868(9) -0.1188(8) 0.5564(7) 0.0448(15) Uani 1 d . . . C3 C 0.4652(10) -0.2420(9) 0.5197(8) 0.0524(18) Uani 1 d . . . H3 H 0.3999 -0.2413 0.56 0.063 Uiso 1 calc R . . C4 C 0.4400(10) -0.3659(9) 0.4238(9) 0.057(2) Uani 1 d . . . C5 C 0.5354(12) -0.3682(10) 0.3625(9) 0.062(2) Uani 1 d . . . H5 H 0.5173 -0.4515 0.2978 0.075 Uiso 1 calc R . . C6 C 0.6571(12) -0.2482(9) 0.3963(8) 0.059(2) Uani 1 d . . . H6 H 0.7223 -0.2505 0.3561 0.07 Uiso 1 calc R . . C7 C 0.9177(9) 0.2345(8) 0.6398(8) 0.0465(16) Uani 1 d . . . C8 C 1.0039(10) 0.3302(9) 0.7679(9) 0.0504(17) Uani 1 d . . . C9 C 1.1094(12) 0.4584(9) 0.7896(9) 0.059(2) Uani 1 d . . . H9 H 1.1672 0.5276 0.874 0.07 Uiso 1 calc R . . C10 C 1.1290(12) 0.4840(10) 0.6860(11) 0.065(2) Uani 1 d . . . H10 H 1.2002 0.569 0.7023 0.078 Uiso 1 calc R . . C11 C 1.0429(11) 0.3832(11) 0.5603(10) 0.060(2) Uani 1 d . . . H11 H 1.0568 0.3999 0.4919 0.072 Uiso 1 calc R . . C12 C 0.9361(11) 0.2578(10) 0.5359(8) 0.0536(19) Uani 1 d . . . H12 H 0.8772 0.1896 0.4511 0.064 Uiso 1 calc R . . C13 C 0.8503(10) 0.1800(9) 1.0834(8) 0.0526(18) Uani 1 d . . . H13 H 0.7669 0.1978 1.0431 0.063 Uiso 1 calc R . . C14 C 0.8486(10) 0.1226(10) 1.1726(9) 0.056(2) Uani 1 d . . . H14 H 0.7653 0.1029 1.1923 0.068 Uiso 1 calc R . . C15 C 0.9698(12) 0.0952(9) 1.2310(9) 0.057(2) Uani 1 d . . . H15 H 0.9716 0.058 1.292 0.068 Uiso 1 calc R . . C16 C 1.0897(11) 0.1240(9) 1.1975(8) 0.0540(19) Uani 1 d . . . H16 H 1.1727 0.1045 1.2353 0.065 Uiso 1 calc R . . C17 C 1.0887(9) 0.1806(7) 1.1099(7) 0.0415(15) Uani 1 d . . . C18 C 1.2094(9) 0.2120(8) 1.0657(8) 0.0470(16) Uani 1 d . . . C19 C 1.3421(10) 0.1934(11) 1.1164(10) 0.062(2) Uani 1 d . . . H19 H 1.3592 0.1621 1.1821 0.074 Uiso 1 calc R . . C20 C 1.4502(13) 0.2225(12) 1.0676(12) 0.071(3) Uani 1 d . . . H20 H 1.5395 0.2094 1.0997 0.085 Uiso 1 calc R . . C21 C 1.4244(12) 0.2694(12) 0.9742(12) 0.070(3) Uani 1 d . . . H21 H 1.4956 0.2884 0.9409 0.084 Uiso 1 calc R . . C22 C 1.2910(10) 0.2895(10) 0.9272(9) 0.0560(19) Uani 1 d . . . H22 H 1.2753 0.3235 0.8634 0.067 Uiso 1 calc R . . C23 C 0.3016(15) -0.4957(11) 0.3794(14) 0.091(4) Uani 1 d . . . H23A H 0.3283 -0.5748 0.3641 0.137 Uiso 1 calc R . . H23B H 0.2231 -0.5089 0.3003 0.137 Uiso 1 calc R . . H23C H 0.2652 -0.4864 0.4454 0.137 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0441(4) 0.0404(4) 0.0419(4) 0.0135(3) 0.0233(3) 0.0178(3) Pd2 0.0456(4) 0.0395(3) 0.0379(3) 0.0119(2) 0.0214(2) 0.0158(2) Cl1 0.0545(10) 0.0493(9) 0.0476(9) 0.0140(8) 0.0241(8) 0.0264(8) Cl2 0.0610(12) 0.0611(12) 0.0707(13) 0.0257(10) 0.0448(10) 0.0243(10) N1 0.047(3) 0.048(3) 0.050(3) 0.026(3) 0.028(3) 0.023(3) N2 0.056(4) 0.043(3) 0.045(3) 0.011(3) 0.025(3) 0.017(3) N3 0.044(3) 0.042(3) 0.042(3) 0.008(3) 0.021(3) 0.015(3) N4 0.045(3) 0.045(3) 0.045(3) 0.014(3) 0.025(3) 0.015(3) C1 0.048(4) 0.048(4) 0.047(4) 0.017(3) 0.023(3) 0.023(3) C2 0.049(4) 0.039(4) 0.043(4) 0.015(3) 0.018(3) 0.017(3) C3 0.050(4) 0.059(5) 0.054(4) 0.025(4) 0.027(4) 0.024(4) C4 0.051(4) 0.043(4) 0.059(5) 0.014(4) 0.015(4) 0.012(4) C5 0.075(6) 0.049(5) 0.052(5) 0.008(4) 0.028(4) 0.023(4) C6 0.076(6) 0.052(5) 0.044(4) 0.009(4) 0.024(4) 0.033(4) C7 0.045(4) 0.047(4) 0.046(4) 0.014(3) 0.025(3) 0.016(3) C8 0.055(4) 0.052(4) 0.056(4) 0.028(4) 0.033(4) 0.022(4) C9 0.071(5) 0.044(4) 0.053(5) 0.018(4) 0.026(4) 0.015(4) C10 0.071(6) 0.048(5) 0.077(6) 0.028(5) 0.038(5) 0.014(4) C11 0.069(5) 0.069(5) 0.063(5) 0.038(5) 0.044(5) 0.029(5) C12 0.062(5) 0.061(5) 0.048(4) 0.024(4) 0.034(4) 0.025(4) C13 0.055(4) 0.050(4) 0.055(4) 0.016(4) 0.029(4) 0.025(4) C14 0.055(5) 0.056(5) 0.060(5) 0.022(4) 0.033(4) 0.019(4) C15 0.072(6) 0.051(4) 0.050(4) 0.021(4) 0.033(4) 0.020(4) C16 0.064(5) 0.054(5) 0.053(4) 0.026(4) 0.028(4) 0.029(4) C17 0.047(4) 0.035(3) 0.035(3) 0.006(3) 0.016(3) 0.017(3) C18 0.049(4) 0.040(4) 0.047(4) 0.010(3) 0.023(3) 0.018(3) C19 0.046(4) 0.077(6) 0.060(5) 0.025(5) 0.021(4) 0.028(4) C20 0.065(6) 0.081(7) 0.085(7) 0.035(6) 0.042(5) 0.043(5) C21 0.057(5) 0.076(6) 0.081(7) 0.024(5) 0.041(5) 0.025(5) C22 0.050(4) 0.061(5) 0.060(5) 0.021(4) 0.032(4) 0.023(4) C23 0.084(8) 0.042(5) 0.103(9) 0.020(6) 0.022(7) -0.005(5) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.960(8) . ? Pd1 N1 2.034(6) . ? Pd1 Cl2 2.306(2) . ? Pd1 Cl1 2.4777(19) . ? Pd1 Pd2 3.1694(7) . ? Pd2 C8 1.965(8) . ? Pd2 N4 2.046(7) . ? Pd2 N3 2.125(7) . ? Pd2 Cl1 2.303(2) . ? N1 N2 1.269(9) . ? N1 C7 1.434(10) . ? N2 C1 1.379(11) . ? N3 C13 1.337(11) . ? N3 C17 1.355(10) . ? N4 C22 1.343(11) . ? N4 C18 1.370(11) . ? C1 C6 1.383(11) . ? C1 C2 1.417(11) . ? C2 C3 1.390(12) . ? C3 C4 1.388(13) . ? C3 H3 0.93 . ? C4 C5 1.383(14) . ? C4 C23 1.505(13) . ? C5 C6 1.378(14) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.380(12) . ? C7 C12 1.393(11) . ? C8 C9 1.406(12) . ? C9 C10 1.403(13) . ? C9 H9 0.93 . ? C10 C11 1.377(15) . ? C10 H10 0.93 . ? C11 C12 1.377(13) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.387(13) . ? C13 H13 0.93 . ? C14 C15 1.362(14) . ? C14 H14 0.93 . ? C15 C16 1.378(13) . ? C15 H15 0.93 . ? C16 C17 1.361(12) . ? C16 H16 0.93 . ? C17 C18 1.472(11) . ? C18 C19 1.381(12) . ? C19 C20 1.398(14) . ? C19 H19 0.93 . ? C20 C21 1.340(16) . ? C20 H20 0.93 . ? C21 C22 1.390(14) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? 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 Pd1 N1 79.0(3) . . ? C2 Pd1 Cl2 94.1(2) . . ? N1 Pd1 Cl2 172.76(19) . . ? C2 Pd1 Cl1 175.7(2) . . ? N1 Pd1 Cl1 96.84(19) . . ? Cl2 Pd1 Cl1 90.09(8) . . ? C2 Pd1 Pd2 130.5(2) . . ? N1 Pd1 Pd2 69.96(19) . . ? Cl2 Pd1 Pd2 114.07(6) . . ? Cl1 Pd1 Pd2 46.14(5) . . ? C8 Pd2 N4 95.2(3) . . ? C8 Pd2 N3 171.8(3) . . ? N4 Pd2 N3 79.0(3) . . ? C8 Pd2 Cl1 87.0(3) . . ? N4 Pd2 Cl1 177.24(19) . . ? N3 Pd2 Cl1 98.97(18) . . ? C8 Pd2 Pd1 82.7(3) . . ? N4 Pd2 Pd1 130.98(18) . . ? N3 Pd2 Pd1 96.68(18) . . ? Cl1 Pd2 Pd1 50.89(5) . . ? Pd2 Cl1 Pd1 82.97(6) . . ? N2 N1 C7 115.4(6) . . ? N2 N1 Pd1 118.3(5) . . ? C7 N1 Pd1 126.2(5) . . ? N1 N2 C1 112.6(7) . . ? C13 N3 C17 119.5(7) . . ? C13 N3 Pd2 125.9(6) . . ? C17 N3 Pd2 114.3(5) . . ? C22 N4 C18 118.4(7) . . ? C22 N4 Pd2 126.3(6) . . ? C18 N4 Pd2 115.3(5) . . ? N2 C1 C6 120.2(8) . . ? N2 C1 C2 118.3(7) . . ? C6 C1 C2 121.5(8) . . ? C3 C2 C1 117.5(7) . . ? C3 C2 Pd1 130.7(7) . . ? C1 C2 Pd1 111.7(6) . . ? C4 C3 C2 120.9(8) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.2(8) . . ? C5 C4 C23 119.8(10) . . ? C3 C4 C23 119.9(10) . . ? C6 C5 C4 120.6(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.3(9) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C8 C7 C12 123.2(8) . . ? C8 C7 N1 119.6(7) . . ? C12 C7 N1 117.1(7) . . ? C7 C8 C9 116.3(8) . . ? C7 C8 Pd2 120.7(6) . . ? C9 C8 Pd2 122.9(7) . . ? C10 C9 C8 121.1(9) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 120.0(9) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C12 C11 C10 120.1(8) . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C11 C12 C7 119.1(8) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? N3 C13 C14 121.4(8) . . ? N3 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C15 C14 C13 119.5(8) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 118.3(8) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C17 C16 C15 121.0(8) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? N3 C17 C16 120.3(8) . . ? N3 C17 C18 114.7(7) . . ? C16 C17 C18 125.0(7) . . ? N4 C18 C19 121.1(8) . . ? N4 C18 C17 116.7(7) . . ? C19 C18 C17 122.2(8) . . ? C18 C19 C20 119.0(10) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.7(10) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 119.8(10) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? N4 C22 C21 121.9(9) . . ? N4 C22 H22 119 . . ? C21 C22 H22 119 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? # Attachment '- 3a.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_juribasic _database_code_depnum_ccdc_archive 'CCDC 746373' #TrackingRef '- 3a.cif' _audit_creation_date 2009-07-07T16:13:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C22 H17 Cl2 N5 Pd2, 2(C2 H6 O S)' _chemical_formula_sum 'C26 H29 Cl2 N5 O2 Pd2 S2' _chemical_formula_weight 792.37 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9012(2) _cell_length_b 15.3882(17) _cell_length_c 26.0962(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5983.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 63498 _cell_measurement_theta_min 2.3366 _cell_measurement_theta_max 30.8486 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'area detector' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 0 _diffrn_reflns_number 53697 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_ambient_temperature 183(2) _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _reflns_number_total 6856 _reflns_number_gt 5353 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farugia, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0541P)^2^+20.4808P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6856 _refine_ls_number_parameters 362 _refine_ls_number_restraints 2 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1391 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.16 _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.716 _refine_diff_density_min -0.551 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd2 Pd 0.81712(3) 0.10825(3) 0.530311(17) 0.03268(13) Uani 1 d . . . Pd1 Pd 0.83243(3) 0.23195(3) 0.432582(17) 0.03114(13) Uani 1 d . . . Cl1 Cl 0.71212(11) 0.14114(10) 0.46929(6) 0.0418(4) Uani 1 d . . . Cl2 Cl 0.80780(12) 0.16783(12) 0.35372(7) 0.0521(4) Uani 1 d . . . N4 N 0.9075(3) 0.0694(3) 0.58463(18) 0.0334(11) Uani 1 d . . . N3 N 0.8549(3) -0.0136(3) 0.50020(18) 0.0343(11) Uani 1 d . . . N1 N 0.8597(3) 0.3019(3) 0.49453(19) 0.0295(10) Uani 1 d . . . N2 N 0.9175(4) 0.3655(3) 0.49183(19) 0.0385(12) Uani 1 d . . . N5 N 1.0782(4) 0.3706(4) 0.3020(2) 0.0454(13) Uani 1 d D . . C22 C 0.9325(5) 0.1134(4) 0.6259(3) 0.0447(15) Uani 1 d . . . H22 H 0.9091 0.1701 0.631 0.054 Uiso 1 calc R . . C21 C 0.9913(5) 0.0802(5) 0.6620(3) 0.0560(19) Uani 1 d . . . H21 H 1.0087 0.1138 0.6909 0.067 Uiso 1 calc R . . C20 C 1.0238(5) -0.0022(5) 0.6550(3) 0.0571(19) Uani 1 d . . . H20 H 1.0637 -0.027 0.6793 0.068 Uiso 1 calc R . . C19 C 0.9983(5) -0.0485(5) 0.6124(3) 0.0495(17) Uani 1 d . . . H19 H 1.0207 -0.1056 0.6073 0.059 Uiso 1 calc R . . C18 C 0.9405(4) -0.0127(4) 0.5772(2) 0.0358(14) Uani 1 d . . . C17 C 0.9137(4) -0.0576(4) 0.5302(2) 0.0358(13) Uani 1 d . . . C16 C 0.9432(4) -0.1391(4) 0.5167(3) 0.0417(15) Uani 1 d . . . H16 H 0.9838 -0.1695 0.5383 0.05 Uiso 1 calc R . . C15 C 0.9138(5) -0.1766(4) 0.4721(3) 0.0480(17) Uani 1 d . . . H15 H 0.9336 -0.233 0.4625 0.058 Uiso 1 calc R . . C14 C 0.8556(5) -0.1315(4) 0.4415(3) 0.0481(17) Uani 1 d . . . H14 H 0.8348 -0.1558 0.4102 0.058 Uiso 1 calc R . . C13 C 0.8280(5) -0.0511(4) 0.4566(2) 0.0417(15) Uani 1 d . . . H13 H 0.7877 -0.0201 0.4351 0.05 Uiso 1 calc R . . C7 C 0.8136(4) 0.3004(4) 0.5441(2) 0.0331(13) Uani 1 d . . . C8 C 0.7866(4) 0.2207(4) 0.5634(2) 0.0351(13) Uani 1 d . . . C9 C 0.7403(5) 0.2211(4) 0.6103(3) 0.0447(16) Uani 1 d . . . H9 H 0.7218 0.1674 0.6249 0.054 Uiso 1 calc R . . C10 C 0.7211(5) 0.2972(4) 0.6356(2) 0.0445(16) Uani 1 d . . . H10 H 0.6882 0.2956 0.6668 0.053 Uiso 1 calc R . . C11 C 0.7496(4) 0.3770(4) 0.6158(2) 0.0398(15) Uani 1 d . . . H11 H 0.738 0.4294 0.6338 0.048 Uiso 1 calc R . . C12 C 0.7944(4) 0.3785(4) 0.5701(2) 0.0355(13) Uani 1 d . . . H12 H 0.8126 0.4325 0.5558 0.043 Uiso 1 calc R . . C2 C 0.9293(4) 0.3071(3) 0.4063(2) 0.0297(12) Uani 1 d . . . C1 C 0.9564(4) 0.3682(4) 0.4443(2) 0.0353(13) Uani 1 d . . . C6 C 1.0227(5) 0.4299(4) 0.4327(3) 0.0428(15) Uani 1 d . . . H6 H 1.04 0.4713 0.4579 0.051 Uiso 1 calc R . . C5 C 1.0623(5) 0.4311(4) 0.3858(3) 0.0427(15) Uani 1 d . . . H5 H 1.1066 0.4737 0.3783 0.051 Uiso 1 calc R . . C4 C 1.0383(4) 0.3701(4) 0.3482(2) 0.0336(13) Uani 1 d . . . C3 C 0.9710(4) 0.3084(4) 0.3598(2) 0.0328(13) Uani 1 d . . . H3 H 0.9545 0.2668 0.3345 0.039 Uiso 1 calc R . . C23 C 1.3057(6) 0.3272(6) 0.2503(3) 0.076(3) Uani 1 d . . . H23A H 1.3207 0.3113 0.2856 0.114 Uiso 1 calc R . . H23B H 1.3499 0.3019 0.2268 0.114 Uiso 1 calc R . . H23C H 1.2458 0.3051 0.2418 0.114 Uiso 1 calc R . . C24 C 1.2674(9) 0.4438(7) 0.1806(4) 0.106(4) Uani 1 d . . . H24A H 1.207 0.4188 0.1792 0.159 Uiso 1 calc R . . H24B H 1.3078 0.41 0.1587 0.159 Uiso 1 calc R . . H24C H 1.2655 0.5041 0.1687 0.159 Uiso 1 calc R . . O1 O 1.2335(5) 0.4744(4) 0.2771(3) 0.101(3) Uani 1 d . . . S1 S 1.30675(15) 0.44095(15) 0.24409(8) 0.0629(5) Uani 1 d . . . C25 C 1.0572(7) 0.1424(7) 0.1440(4) 0.085(3) Uani 1 d . . . H25A H 1.0083 0.1739 0.127 0.128 Uiso 1 calc R . . H25B H 1.054 0.0807 0.1348 0.128 Uiso 1 calc R . . H25C H 1.1149 0.1662 0.1328 0.128 Uiso 1 calc R . . C26 C 0.9334(8) 0.1182(7) 0.2176(4) 0.095(3) Uani 1 d . . . H26A H 0.91 0.1343 0.2514 0.142 Uiso 1 calc R . . H26B H 0.9309 0.055 0.2136 0.142 Uiso 1 calc R . . H26C H 0.897 0.1458 0.1909 0.142 Uiso 1 calc R . . O2 O 1.0440(6) 0.2488(4) 0.2216(2) 0.093(2) Uani 1 d . . . S2 S 1.04673(19) 0.15391(14) 0.21206(10) 0.0781(7) Uani 1 d . . . H1N H 1.124(4) 0.405(5) 0.294(4) 0.094 Uiso 1 d D . . H2N H 1.060(6) 0.332(5) 0.279(3) 0.094 Uiso 1 d 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 Pd2 0.0406(3) 0.0254(2) 0.0321(2) 0.00514(18) 0.00080(19) -0.00170(19) Pd1 0.0376(3) 0.0256(2) 0.0303(2) 0.00026(17) -0.00601(19) -0.00228(19) Cl1 0.0434(8) 0.0351(7) 0.0470(9) 0.0077(7) -0.0088(7) -0.0059(7) Cl2 0.0585(11) 0.0560(10) 0.0418(9) -0.0097(8) -0.0074(8) -0.0172(9) N4 0.038(3) 0.032(2) 0.030(3) 0.005(2) 0.003(2) -0.004(2) N3 0.041(3) 0.033(2) 0.030(3) 0.007(2) 0.004(2) -0.004(2) N1 0.024(2) 0.022(2) 0.042(3) 0.016(2) -0.007(2) -0.0025(19) N2 0.053(3) 0.033(3) 0.029(3) -0.002(2) 0.002(2) 0.000(2) N5 0.054(4) 0.045(3) 0.037(3) 0.001(2) 0.003(3) -0.007(3) C22 0.049(4) 0.045(4) 0.039(4) -0.002(3) 0.005(3) 0.001(3) C21 0.060(5) 0.074(5) 0.033(4) -0.005(3) -0.008(3) -0.003(4) C20 0.061(5) 0.065(5) 0.046(4) 0.011(4) -0.011(4) 0.007(4) C19 0.054(4) 0.048(4) 0.046(4) 0.008(3) -0.006(3) 0.012(3) C18 0.035(3) 0.036(3) 0.036(3) 0.008(3) 0.004(3) -0.005(3) C17 0.036(3) 0.031(3) 0.041(3) 0.007(3) 0.004(3) -0.005(3) C16 0.043(4) 0.029(3) 0.053(4) 0.002(3) -0.002(3) 0.000(3) C15 0.046(4) 0.034(3) 0.063(5) -0.003(3) 0.007(3) -0.003(3) C14 0.048(4) 0.044(4) 0.052(4) -0.003(3) 0.002(3) -0.015(3) C13 0.056(4) 0.038(3) 0.031(3) 0.005(3) -0.005(3) -0.005(3) C7 0.039(3) 0.029(3) 0.031(3) -0.002(2) -0.006(3) -0.002(3) C8 0.039(3) 0.031(3) 0.035(3) -0.003(2) 0.006(3) 0.000(3) C9 0.051(4) 0.038(3) 0.046(4) 0.003(3) 0.006(3) -0.005(3) C10 0.049(4) 0.052(4) 0.032(3) 0.004(3) 0.008(3) 0.005(3) C11 0.047(4) 0.035(3) 0.037(3) -0.006(3) -0.002(3) 0.005(3) C12 0.040(3) 0.028(3) 0.038(3) -0.003(2) -0.005(3) 0.001(3) C2 0.035(3) 0.024(3) 0.031(3) 0.005(2) -0.006(2) 0.004(2) C1 0.046(4) 0.029(3) 0.030(3) 0.000(2) 0.001(3) -0.002(3) C6 0.051(4) 0.034(3) 0.043(4) -0.009(3) 0.004(3) -0.010(3) C5 0.056(4) 0.029(3) 0.044(4) -0.002(3) 0.007(3) -0.010(3) C4 0.035(3) 0.028(3) 0.038(3) 0.006(2) -0.003(3) 0.005(2) C3 0.037(3) 0.028(3) 0.033(3) -0.001(2) -0.005(2) 0.007(3) C23 0.087(7) 0.088(6) 0.053(5) 0.007(5) 0.011(4) 0.026(5) C24 0.138(10) 0.103(8) 0.077(7) -0.007(6) -0.015(7) 0.078(8) O1 0.119(6) 0.060(4) 0.125(6) -0.038(4) 0.074(5) -0.023(4) S1 0.0593(12) 0.0733(13) 0.0562(12) -0.0051(10) 0.0118(9) -0.0082(10) C25 0.093(7) 0.085(6) 0.078(7) -0.035(5) 0.025(5) -0.019(6) C26 0.127(9) 0.086(7) 0.072(7) -0.009(5) 0.025(6) -0.026(7) O2 0.158(7) 0.053(3) 0.069(4) -0.019(3) -0.001(4) -0.009(4) S2 0.110(2) 0.0509(11) 0.0739(15) -0.0102(11) -0.0232(14) 0.0090(12) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd2 C8 1.986(6) . ? Pd2 N4 2.045(5) . ? Pd2 N3 2.109(5) . ? Pd2 Cl1 2.2892(16) . ? Pd2 Pd1 3.1906(6) . ? Pd1 C2 1.972(6) . ? Pd1 N1 1.984(5) . ? Pd1 Cl2 2.3116(17) . ? Pd1 Cl1 2.4667(16) . ? N4 C22 1.326(8) . ? N4 C18 1.370(8) . ? N3 C13 1.337(8) . ? N3 C17 1.356(8) . ? N1 N2 1.305(7) . ? N1 C7 1.466(7) . ? N2 C1 1.369(7) . ? N5 C4 1.344(8) . ? N5 H1N 0.89(7) . ? N5 H2N 0.89(8) . ? C22 C21 1.383(10) . ? C22 H22 0.95 . ? C21 C20 1.369(11) . ? C21 H21 0.95 . ? C20 C19 1.373(10) . ? C20 H20 0.95 . ? C19 C18 1.373(9) . ? C19 H19 0.95 . ? C18 C17 1.464(9) . ? C17 C16 1.375(8) . ? C16 C15 1.372(9) . ? C16 H16 0.95 . ? C15 C14 1.367(10) . ? C15 H15 0.95 . ? C14 C13 1.362(9) . ? C14 H14 0.95 . ? C13 H13 0.95 . ? C7 C8 1.385(8) . ? C7 C12 1.409(8) . ? C8 C9 1.407(9) . ? C9 C10 1.375(9) . ? C9 H9 0.95 . ? C10 C11 1.399(9) . ? C10 H10 0.95 . ? C11 C12 1.365(9) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C2 C3 1.365(8) . ? C2 C1 1.426(8) . ? C1 C6 1.403(9) . ? C6 C5 1.359(9) . ? C6 H6 0.95 . ? C5 C4 1.403(8) . ? C5 H5 0.95 . ? C4 C3 1.414(8) . ? C3 H3 0.95 . ? C23 S1 1.757(9) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 S1 1.757(10) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? O1 S1 1.483(6) . ? C25 S2 1.793(9) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 S2 1.781(11) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? O2 S2 1.482(6) . ? 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 C8 Pd2 N4 96.0(2) . . ? C8 Pd2 N3 175.7(2) . . ? N4 Pd2 N3 79.77(19) . . ? C8 Pd2 Cl1 87.31(19) . . ? N4 Pd2 Cl1 175.67(14) . . ? N3 Pd2 Cl1 96.88(14) . . ? C8 Pd2 Pd1 81.01(17) . . ? N4 Pd2 Pd1 132.96(13) . . ? N3 Pd2 Pd1 102.33(13) . . ? Cl1 Pd2 Pd1 50.27(4) . . ? C2 Pd1 N1 79.3(2) . . ? C2 Pd1 Cl2 93.28(17) . . ? N1 Pd1 Cl2 171.66(13) . . ? C2 Pd1 Cl1 177.38(17) . . ? N1 Pd1 Cl1 98.04(14) . . ? Cl2 Pd1 Cl1 89.34(6) . . ? C2 Pd1 Pd2 132.83(15) . . ? N1 Pd1 Pd2 71.75(12) . . ? Cl2 Pd1 Pd2 116.46(5) . . ? Cl1 Pd1 Pd2 45.54(4) . . ? Pd2 Cl1 Pd1 84.18(5) . . ? C22 N4 C18 119.0(5) . . ? C22 N4 Pd2 126.8(4) . . ? C18 N4 Pd2 114.1(4) . . ? C13 N3 C17 118.0(5) . . ? C13 N3 Pd2 128.4(4) . . ? C17 N3 Pd2 113.6(4) . . ? N2 N1 C7 111.6(5) . . ? N2 N1 Pd1 119.9(4) . . ? C7 N1 Pd1 128.0(3) . . ? N1 N2 C1 110.6(5) . . ? C4 N5 H1N 124(6) . . ? C4 N5 H2N 118(6) . . ? H1N N5 H2N 118(8) . . ? N4 C22 C21 122.9(6) . . ? N4 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C20 C21 C22 118.3(7) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C21 C20 C19 119.4(7) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C18 C19 C20 120.4(7) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? N4 C18 C19 120.1(6) . . ? N4 C18 C17 117.0(5) . . ? C19 C18 C17 122.9(6) . . ? N3 C17 C16 120.9(6) . . ? N3 C17 C18 115.2(5) . . ? C16 C17 C18 123.9(6) . . ? C15 C16 C17 119.9(6) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C14 C15 C16 119.0(6) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C13 C14 C15 118.9(7) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C13 C14 123.2(6) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C8 C7 C12 121.4(6) . . ? C8 C7 N1 118.0(5) . . ? C12 C7 N1 120.5(5) . . ? C7 C8 C9 117.0(5) . . ? C7 C8 Pd2 123.2(4) . . ? C9 C8 Pd2 119.6(4) . . ? C10 C9 C8 121.6(6) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.5(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C7 120.3(6) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C3 C2 C1 118.7(5) . . ? C3 C2 Pd1 130.6(4) . . ? C1 C2 Pd1 110.7(4) . . ? N2 C1 C6 121.0(5) . . ? N2 C1 C2 119.3(5) . . ? C6 C1 C2 119.7(5) . . ? C5 C6 C1 120.6(6) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? N5 C4 C5 120.7(6) . . ? N5 C4 C3 120.5(6) . . ? C5 C4 C3 118.8(6) . . ? C2 C3 C4 121.5(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? S1 C23 H23A 109.5 . . ? S1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S1 C24 H24A 109.5 . . ? S1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 S1 C24 107.1(5) . . ? O1 S1 C23 106.6(4) . . ? C24 S1 C23 96.2(5) . . ? S2 C25 H25A 109.5 . . ? S2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S2 C26 H26A 109.5 . . ? S2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 S2 C26 105.3(5) . . ? O2 S2 C25 105.4(4) . . ? C26 S2 C25 97.6(5) . . ? # end Validation Reply Form # Attachment '- 4a.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_marina-19022008 _database_code_depnum_ccdc_archive 'CCDC 746374' #TrackingRef '- 4a.cif' _audit_creation_date 2009-05-06T13:20:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C24 H20 Cl2 N6 O2 Pd2' _chemical_formula_sum 'C24 H20 Cl2 N6 O2 Pd2' _chemical_formula_weight 708.16 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.04790(10) _cell_length_b 17.48810(10) _cell_length_c 13.34500(10) _cell_angle_alpha 90 _cell_angle_beta 104.9400(10) _cell_angle_gamma 90 _cell_volume 2491.19(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9614 _cell_measurement_theta_min 2.5229 _cell_measurement_theta_max 75.9435 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colour _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 13.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61412 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 13421 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 75.5 _diffrn_reflns_theta_full 76.11 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.979 _reflns_number_total 5094 _reflns_number_gt 4502 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0508P)^2^+2.8639P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5094 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0954 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.766 _refine_diff_density_min -0.566 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd1 Pd 0.73149(2) 0.075970(16) 0.17753(2) 0.04045(10) Uani 1 d . . . Pd2 Pd 0.98995(2) 0.131721(16) 0.27338(2) 0.04017(10) Uani 1 d . . . Cl1 Cl 0.81315(9) 0.20777(6) 0.23385(8) 0.0499(2) Uani 1 d . . . Cl2 Cl 0.61397(10) 0.07621(6) 0.29795(8) 0.0533(2) Uani 1 d . . . O1 O 1.2799(4) 0.2792(2) 0.0659(4) 0.0751(10) Uani 1 d . . . O2 O 1.2177(4) 0.2551(3) -0.0981(3) 0.0791(11) Uani 1 d . . . N1 N 0.8152(3) 0.0691(2) 0.0594(2) 0.0429(7) Uani 1 d . . . N2 N 0.7687(3) 0.0187(2) -0.0125(2) 0.0450(7) Uani 1 d . . . N6 N 1.2090(4) 0.2484(2) -0.0091(4) 0.0589(10) Uani 1 d . . . N5 N 0.4730(4) -0.1933(3) 0.1134(3) 0.0620(10) Uani 1 d . . . N3 N 1.0022(3) 0.1159(2) 0.4325(2) 0.0439(7) Uani 1 d . . . N4 N 1.1438(3) 0.0628(2) 0.3141(2) 0.0424(7) Uani 1 d . . . C1 C 0.6839(4) -0.0279(2) 0.0136(3) 0.0434(8) Uani 1 d . . . C2 C 0.6586(3) -0.0197(2) 0.1120(3) 0.0428(8) Uani 1 d . . . C3 C 0.5882(4) -0.0744(2) 0.1451(3) 0.0468(9) Uani 1 d . . . H3 H 0.5742 -0.0705 0.2107 0.056 Uiso 1 calc R . . C4 C 0.5368(4) -0.1367(2) 0.0799(3) 0.0476(9) Uani 1 d . . . C5 C 0.5517(4) -0.1385(2) -0.0222(3) 0.0499(9) Uani 1 d . . . H5 H 0.5105 -0.1757 -0.0683 0.06 Uiso 1 calc R . . C6 C 0.6248(4) -0.0867(3) -0.0537(3) 0.0497(9) Uani 1 d . . . H6 H 0.6364 -0.0899 -0.1202 0.06 Uiso 1 calc R . . C7 C 0.9117(4) 0.1148(2) 0.0415(3) 0.0426(8) Uani 1 d . . . C8 C 0.9988(4) 0.1465(2) 0.1272(3) 0.0430(8) Uani 1 d . . . C9 C 1.0971(4) 0.1902(2) 0.1096(3) 0.0475(9) Uani 1 d . . . H9 H 1.1555 0.2121 0.1651 0.057 Uiso 1 calc R . . C10 C 1.1071(4) 0.2008(2) 0.0094(3) 0.0475(9) Uani 1 d . . . C11 C 1.0206(4) 0.1709(3) -0.0759(3) 0.0544(10) Uani 1 d . . . H11 H 1.028 0.1798 -0.1427 0.065 Uiso 1 calc R . . C12 C 0.9238(5) 0.1278(3) -0.0593(3) 0.0552(10) Uani 1 d . . . H12 H 0.8654 0.1069 -0.1156 0.066 Uiso 1 calc R . . C23 C 0.4143(7) -0.2549(4) 0.0452(5) 0.092(2) Uani 1 d . . . H23A H 0.3555 -0.2339 -0.0143 0.138 Uiso 1 calc R . . H23B H 0.3714 -0.2883 0.0816 0.138 Uiso 1 calc R . . H23C H 0.4773 -0.2832 0.0231 0.138 Uiso 1 calc R . . C24 C 0.4744(7) -0.2016(4) 0.2223(5) 0.089(2) Uani 1 d . . . H24A H 0.557 -0.191 0.2647 0.134 Uiso 1 calc R . . H24B H 0.4511 -0.2529 0.2349 0.134 Uiso 1 calc R . . H24C H 0.416 -0.1663 0.239 0.134 Uiso 1 calc R . . C13 C 0.9248(4) 0.1427(3) 0.4860(4) 0.0542(10) Uani 1 d . . . H13 H 0.8526 0.1685 0.451 0.065 Uiso 1 calc R . . C14 C 0.9489(5) 0.1331(3) 0.5929(4) 0.0623(12) Uani 1 d . . . H14 H 0.8948 0.1535 0.6291 0.075 Uiso 1 calc R . . C15 C 1.0533(5) 0.0934(3) 0.6442(3) 0.0617(12) Uani 1 d . . . H15 H 1.0703 0.0861 0.7155 0.074 Uiso 1 calc R . . C16 C 1.1330(5) 0.0643(3) 0.5897(3) 0.0558(11) Uani 1 d . . . H16 H 1.2042 0.0372 0.6236 0.067 Uiso 1 calc R . . C17 C 1.1053(4) 0.0762(2) 0.4827(3) 0.0456(9) Uani 1 d . . . C18 C 1.1839(4) 0.0473(2) 0.4170(3) 0.0450(8) Uani 1 d . . . C19 C 1.2914(4) 0.0038(3) 0.4553(4) 0.0596(12) Uani 1 d . . . H19 H 1.32 -0.0057 0.526 0.071 Uiso 1 calc R . . C20 C 1.3553(4) -0.0250(3) 0.3871(4) 0.0645(13) Uani 1 d . . . H20 H 1.4275 -0.0539 0.4117 0.077 Uiso 1 calc R . . C21 C 1.3115(4) -0.0107(3) 0.2832(4) 0.0597(11) Uani 1 d . . . H21 H 1.3527 -0.0303 0.2363 0.072 Uiso 1 calc R . . C22 C 1.2052(4) 0.0332(3) 0.2493(3) 0.0502(9) Uani 1 d . . . H22 H 1.1752 0.0425 0.1786 0.06 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03964(15) 0.04524(17) 0.03712(15) -0.00013(10) 0.01109(11) 0.00103(10) Pd2 0.03965(15) 0.04463(16) 0.03627(15) -0.00043(10) 0.00987(11) -0.00036(10) Cl1 0.0481(5) 0.0470(5) 0.0549(5) -0.0037(4) 0.0137(4) 0.0041(4) Cl2 0.0552(5) 0.0649(6) 0.0439(5) -0.0009(4) 0.0203(4) 0.0021(4) O1 0.061(2) 0.066(2) 0.102(3) 0.004(2) 0.028(2) -0.0109(17) O2 0.068(2) 0.095(3) 0.085(3) 0.036(2) 0.038(2) 0.006(2) N1 0.0442(17) 0.0511(19) 0.0341(15) 0.0019(13) 0.0117(13) 0.0015(13) N2 0.0475(17) 0.0488(19) 0.0396(16) -0.0008(14) 0.0127(13) 0.0022(14) N6 0.049(2) 0.052(2) 0.080(3) 0.019(2) 0.0249(19) 0.0062(16) N5 0.059(2) 0.060(2) 0.063(2) 0.0114(19) 0.0075(18) -0.0130(18) N3 0.0468(17) 0.0477(18) 0.0374(15) -0.0025(13) 0.0110(13) -0.0064(14) N4 0.0397(16) 0.0488(18) 0.0388(15) 0.0019(13) 0.0102(12) 0.0021(13) C1 0.0421(19) 0.044(2) 0.0436(19) 0.0008(16) 0.0097(15) -0.0006(15) C2 0.0372(17) 0.046(2) 0.0442(19) 0.0032(16) 0.0092(14) 0.0045(15) C3 0.0410(19) 0.052(2) 0.047(2) 0.0033(17) 0.0109(16) -0.0008(16) C4 0.0367(18) 0.050(2) 0.054(2) 0.0061(18) 0.0073(16) 0.0023(16) C5 0.046(2) 0.046(2) 0.052(2) -0.0052(17) 0.0030(17) -0.0014(16) C6 0.050(2) 0.054(2) 0.044(2) -0.0011(17) 0.0106(17) 0.0019(18) C7 0.0435(19) 0.046(2) 0.0400(18) 0.0021(16) 0.0144(15) 0.0042(15) C8 0.0432(19) 0.048(2) 0.0367(18) 0.0052(15) 0.0093(15) 0.0029(16) C9 0.0413(19) 0.048(2) 0.054(2) 0.0051(17) 0.0123(16) 0.0022(16) C10 0.044(2) 0.042(2) 0.060(2) 0.0099(17) 0.0194(17) 0.0080(16) C11 0.061(2) 0.061(3) 0.047(2) 0.0084(19) 0.0248(19) 0.001(2) C12 0.061(3) 0.065(3) 0.040(2) 0.0055(19) 0.0146(18) -0.002(2) C23 0.103(5) 0.084(4) 0.073(4) 0.015(3) -0.005(3) -0.045(4) C24 0.111(5) 0.084(4) 0.082(4) 0.005(3) 0.043(4) -0.035(4) C13 0.057(2) 0.059(3) 0.052(2) -0.0076(19) 0.0221(19) -0.0042(19) C14 0.079(3) 0.061(3) 0.054(3) -0.009(2) 0.032(2) -0.009(2) C15 0.083(3) 0.066(3) 0.038(2) -0.004(2) 0.018(2) -0.007(3) C16 0.060(3) 0.068(3) 0.0345(19) -0.0019(18) 0.0036(17) -0.001(2) C17 0.049(2) 0.046(2) 0.043(2) -0.0006(16) 0.0139(16) -0.0078(16) C18 0.045(2) 0.050(2) 0.0397(18) 0.0030(16) 0.0100(15) -0.0069(16) C19 0.050(2) 0.081(3) 0.046(2) 0.013(2) 0.0101(18) 0.009(2) C20 0.048(2) 0.083(4) 0.063(3) 0.017(3) 0.015(2) 0.018(2) C21 0.051(2) 0.078(3) 0.054(2) 0.006(2) 0.0211(19) 0.010(2) C22 0.050(2) 0.062(3) 0.0402(19) 0.0021(18) 0.0149(16) 0.0046(19) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.962(4) . ? Pd1 N1 2.027(3) . ? Pd1 Cl2 2.3117(10) . ? Pd1 Cl1 2.5183(11) . ? Pd1 Pd2 2.9760(4) . ? Pd2 C8 1.995(4) . ? Pd2 N4 2.040(3) . ? Pd2 N3 2.111(3) . ? Pd2 Cl1 2.3089(10) . ? O1 N6 1.225(6) . ? O2 N6 1.222(6) . ? N1 N2 1.306(5) . ? N1 C7 1.401(5) . ? N2 C1 1.353(5) . ? N6 C10 1.471(5) . ? N5 C4 1.357(6) . ? N5 C23 1.450(7) . ? N5 C24 1.455(7) . ? N3 C13 1.332(5) . ? N3 C17 1.354(6) . ? N4 C22 1.335(5) . ? N4 C18 1.357(5) . ? C1 C6 1.411(6) . ? C1 C2 1.419(5) . ? C2 C3 1.375(6) . ? C3 C4 1.419(6) . ? C3 H3 0.93 . ? C4 C5 1.414(6) . ? C5 C6 1.350(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.404(6) . ? C7 C8 1.405(6) . ? C8 C9 1.396(6) . ? C9 C10 1.383(6) . ? C9 H9 0.93 . ? C10 C11 1.386(6) . ? C11 C12 1.372(7) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C13 C14 1.393(7) . ? C13 H13 0.93 . ? C14 C15 1.369(8) . ? C14 H14 0.93 . ? C15 C16 1.376(7) . ? C15 H15 0.93 . ? C16 C17 1.397(6) . ? C16 H16 0.93 . ? C17 C18 1.473(6) . ? C18 C19 1.392(6) . ? C19 C20 1.383(7) . ? C19 H19 0.93 . ? C20 C21 1.369(7) . ? C20 H20 0.93 . ? C21 C22 1.377(6) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? 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 Pd1 N1 79.62(15) . . ? C2 Pd1 Cl2 94.11(12) . . ? N1 Pd1 Cl2 172.58(10) . . ? C2 Pd1 Cl1 171.05(11) . . ? N1 Pd1 Cl1 94.96(10) . . ? Cl2 Pd1 Cl1 90.75(4) . . ? C2 Pd1 Pd2 135.16(11) . . ? N1 Pd1 Pd2 76.94(9) . . ? Cl2 Pd1 Pd2 110.44(3) . . ? Cl1 Pd1 Pd2 48.83(2) . . ? C8 Pd2 N4 95.16(14) . . ? C8 Pd2 N3 173.73(14) . . ? N4 Pd2 N3 79.70(13) . . ? C8 Pd2 Cl1 87.35(11) . . ? N4 Pd2 Cl1 177.36(10) . . ? N3 Pd2 Cl1 97.84(10) . . ? C8 Pd2 Pd1 84.57(11) . . ? N4 Pd2 Pd1 124.19(10) . . ? N3 Pd2 Pd1 101.26(9) . . ? Cl1 Pd2 Pd1 55.19(3) . . ? Pd2 Cl1 Pd1 75.99(3) . . ? N2 N1 C7 115.5(3) . . ? N2 N1 Pd1 116.1(3) . . ? C7 N1 Pd1 128.2(3) . . ? N1 N2 C1 112.6(3) . . ? O2 N6 O1 124.0(4) . . ? O2 N6 C10 118.2(4) . . ? O1 N6 C10 117.8(4) . . ? C4 N5 C23 121.4(5) . . ? C4 N5 C24 121.9(4) . . ? C23 N5 C24 116.2(4) . . ? C13 N3 C17 119.3(4) . . ? C13 N3 Pd2 127.5(3) . . ? C17 N3 Pd2 113.1(3) . . ? C22 N4 C18 119.4(4) . . ? C22 N4 Pd2 125.8(3) . . ? C18 N4 Pd2 114.9(3) . . ? N2 C1 C6 120.9(4) . . ? N2 C1 C2 119.5(4) . . ? C6 C1 C2 119.6(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 Pd1 130.6(3) . . ? C1 C2 Pd1 110.0(3) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? N5 C4 C5 120.1(4) . . ? N5 C4 C3 121.2(4) . . ? C5 C4 C3 118.7(4) . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N1 C7 C12 121.4(4) . . ? N1 C7 C8 118.5(3) . . ? C12 C7 C8 120.1(4) . . ? C9 C8 C7 118.6(4) . . ? C9 C8 Pd2 118.1(3) . . ? C7 C8 Pd2 123.3(3) . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 122.2(4) . . ? C9 C10 N6 119.6(4) . . ? C11 C10 N6 118.1(4) . . ? C12 C11 C10 118.4(4) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C7 120.9(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C13 C14 121.8(5) . . ? N3 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 119.0(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N3 C17 C16 121.1(4) . . ? N3 C17 C18 115.6(4) . . ? C16 C17 C18 123.4(4) . . ? N4 C18 C19 120.4(4) . . ? N4 C18 C17 116.4(4) . . ? C19 C18 C17 123.2(4) . . ? C20 C19 C18 119.3(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 119.5(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 118.9(4) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N4 C22 C21 122.4(4) . . ? N4 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? # Attachment '- 3b1.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_manda-c2aabbp _database_code_depnum_ccdc_archive 'CCDC 746375' #TrackingRef '- 3b1.cif' _audit_creation_date 2009-07-08T16:36:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C32 H25 Cl N7 Pd2, 2(C2 H6 O S), H2 O, Cl' _chemical_formula_sum 'C36 H39 Cl2 N7 O3 Pd2 S2' _chemical_formula_weight 965.58 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7652(2) _cell_length_b 14.9221(3) _cell_length_c 17.6810(4) _cell_angle_alpha 99.709(2) _cell_angle_beta 94.075(2) _cell_angle_gamma 96.168(2) _cell_volume 1999.39(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11888 _cell_measurement_theta_min 2.5381 _cell_measurement_theta_max 76.1339 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 9.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_T_max 0.456 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_reflns_number 17952 _diffrn_ambient_temperature 293(2) _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 76.0 _diffrn_reflns_theta_full 76.21 _diffrn_measured_fraction_theta_max 1.002 _diffrn_measured_fraction_theta_full 0.961 _reflns_number_total 8372 _reflns_number_gt 6919 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0773P)^2^+0.7014P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8044 _refine_ls_number_parameters 475 _refine_ls_number_restraints 11 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1126 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.008 _refine_diff_density_max 1.175 _refine_diff_density_min -0.42 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd1 Pd 0.10055(3) 0.569682(16) 0.236410(14) 0.04454(9) Uani 1 d . . . Pd2 Pd 0.43005(3) 0.484594(15) 0.287792(13) 0.04318(9) Uani 1 d . . . Cl1 Cl 0.31209(13) 0.41306(7) 0.38159(6) 0.0586(2) Uani 1 d . . . Cl2 Cl -0.09874(19) 0.93102(8) 0.27270(9) 0.0843(4) Uani 1 d . . . N1 N 0.1836(4) 0.4912(2) 0.14571(17) 0.0469(6) Uani 1 d . . . N2 N 0.2309(4) 0.5270(2) 0.08880(17) 0.0520(7) Uani 1 d . . . N3 N 0.5186(4) 0.6113(2) 0.36115(16) 0.0459(6) Uani 1 d . . . N4 N 0.5643(4) 0.5524(2) 0.21427(17) 0.0470(6) Uani 1 d . . . N5 N 0.0562(4) 0.6503(2) 0.33849(18) 0.0512(7) Uani 1 d . . . N6 N -0.0341(4) 0.4716(2) 0.2931(2) 0.0546(7) Uani 1 d . . . N7 N 0.1488(7) 0.8918(3) 0.1273(3) 0.0760(11) Uani 1 d D . . C1 C 0.2172(5) 0.6185(3) 0.0992(2) 0.0516(8) Uani 1 d . . . C2 C 0.1624(5) 0.6615(2) 0.1698(2) 0.0477(7) Uani 1 d . . . C3 C 0.1400(5) 0.7519(3) 0.1779(2) 0.0536(8) Uani 1 d . . . H3 H 0.0998 0.7808 0.2229 0.064 Uiso 1 calc R . . C4 C 0.1775(5) 0.8032(3) 0.1183(2) 0.0559(8) Uani 1 d . . . C5 C 0.2420(6) 0.7601(3) 0.0510(2) 0.0622(10) Uani 1 d . . . H5 H 0.2716 0.7935 0.0129 0.075 Uiso 1 calc R . . C6 C 0.2610(6) 0.6688(3) 0.0417(2) 0.0619(10) Uani 1 d . . . H6 H 0.3031 0.6401 -0.0029 0.074 Uiso 1 calc R . . C7 C 0.2212(5) 0.3984(2) 0.1441(2) 0.0506(8) Uani 1 d . . . C8 C 0.3280(5) 0.3803(2) 0.2056(2) 0.0487(7) Uani 1 d . . . C9 C 0.3603(6) 0.2896(3) 0.2025(3) 0.0648(10) Uani 1 d . . . H9 H 0.4301 0.2743 0.2421 0.078 Uiso 1 calc R . . C10 C 0.2897(8) 0.2218(3) 0.1410(3) 0.0801(14) Uani 1 d . . . H10 H 0.3146 0.162 0.1396 0.096 Uiso 1 calc R . . C11 C 0.1837(8) 0.2419(3) 0.0822(3) 0.0794(14) Uani 1 d . . . H11 H 0.1351 0.1955 0.0421 0.095 Uiso 1 calc R . . C12 C 0.1491(6) 0.3310(3) 0.0824(2) 0.0626(10) Uani 1 d . . . H12 H 0.0793 0.3455 0.0424 0.075 Uiso 1 calc R . . C13 C 0.4942(5) 0.6358(3) 0.4354(2) 0.0556(9) Uani 1 d . . . H13 H 0.4515 0.591 0.4622 0.067 Uiso 1 calc R . . C14 C 0.5299(6) 0.7247(3) 0.4736(2) 0.0638(10) Uani 1 d . . . H14 H 0.5094 0.7398 0.5251 0.077 Uiso 1 calc R . . C15 C 0.5961(6) 0.7908(3) 0.4346(3) 0.0645(10) Uani 1 d . . . H15 H 0.6209 0.8514 0.4594 0.077 Uiso 1 calc R . . C16 C 0.6258(6) 0.7664(3) 0.3582(2) 0.0574(9) Uani 1 d . . . H16 H 0.6724 0.8102 0.3311 0.069 Uiso 1 calc R . . C17 C 0.5848(5) 0.6757(2) 0.3224(2) 0.0456(7) Uani 1 d . . . C18 C 0.6139(4) 0.6432(2) 0.2416(2) 0.0448(7) Uani 1 d . . . C19 C 0.6925(6) 0.6991(3) 0.1954(2) 0.0580(9) Uani 1 d . . . H19 H 0.7243 0.7612 0.2141 0.07 Uiso 1 calc R . . C20 C 0.7229(6) 0.6618(3) 0.1211(2) 0.0642(10) Uani 1 d . . . H20 H 0.7724 0.6988 0.0891 0.077 Uiso 1 calc R . . C21 C 0.6793(6) 0.5693(3) 0.0951(2) 0.0641(10) Uani 1 d . . . H21 H 0.7025 0.5424 0.046 0.077 Uiso 1 calc R . . C22 C 0.6005(5) 0.5175(3) 0.1434(2) 0.0564(9) Uani 1 d . . . H22 H 0.571 0.455 0.1257 0.068 Uiso 1 calc R . . C23 C 0.1244(6) 0.7378(3) 0.3622(3) 0.0619(10) Uani 1 d . . . H23 H 0.185 0.768 0.3285 0.074 Uiso 1 calc R . . C24 C 0.1077(7) 0.7846(3) 0.4351(3) 0.0734(12) Uani 1 d . . . H24 H 0.1537 0.8458 0.4495 0.088 Uiso 1 calc R . . C25 C 0.0235(7) 0.7405(4) 0.4855(3) 0.0758(13) Uani 1 d . . . H25 H 0.0116 0.7709 0.5349 0.091 Uiso 1 calc R . . C26 C -0.0435(6) 0.6508(4) 0.4624(3) 0.0700(12) Uani 1 d . . . H26 H -0.1006 0.6196 0.4966 0.084 Uiso 1 calc R . . C27 C -0.0270(5) 0.6057(3) 0.3883(2) 0.0552(9) Uani 1 d . . . C28 C -0.0876(5) 0.5082(3) 0.3610(2) 0.0553(9) Uani 1 d . . . C29 C -0.1923(6) 0.4558(4) 0.4015(3) 0.0727(13) Uani 1 d . . . H29 H -0.2297 0.4821 0.448 0.087 Uiso 1 calc R . . C30 C -0.2406(7) 0.3639(4) 0.3718(4) 0.0818(15) Uani 1 d . . . H30 H -0.3094 0.3275 0.3987 0.098 Uiso 1 calc R . . C31 C -0.1862(7) 0.3270(4) 0.3029(4) 0.0766(13) Uani 1 d . . . H31 H -0.218 0.2655 0.282 0.092 Uiso 1 calc R . . C32 C -0.0828(6) 0.3828(3) 0.2645(3) 0.0648(10) Uani 1 d . . . H32 H -0.0461 0.3578 0.2174 0.078 Uiso 1 calc R . . HN1 H 0.169(7) 0.926(3) 0.094(3) 0.078 Uiso 1 d D . . HN2 H 0.106(7) 0.916(4) 0.170(2) 0.078 Uiso 1 d D . . S1 S 0.4185(3) 0.09436(10) 0.30825(11) 0.1090(6) Uani 1 d . . . O1 O 0.5650(8) 0.1484(3) 0.3601(5) 0.148(3) Uani 1 d . . . C33 C 0.2262(10) 0.1318(4) 0.3428(5) 0.110(2) Uani 1 d . . . H33A H 0.2199 0.1936 0.3353 0.165 Uiso 1 calc R . . H33B H 0.2267 0.1293 0.3967 0.165 Uiso 1 calc R . . H33C H 0.1273 0.0928 0.3151 0.165 Uiso 1 calc R . . C34 C 0.3912(14) -0.0160(5) 0.3324(7) 0.151(4) Uani 1 d . . . H34A H 0.4872 -0.0481 0.3169 0.226 Uiso 1 calc R . . H34B H 0.2848 -0.0493 0.3064 0.226 Uiso 1 calc R . . H34C H 0.3866 -0.0108 0.3871 0.226 Uiso 1 calc R . . S2 S 0.8004(2) 0.00479(15) 0.07653(12) 0.1097(6) Uani 1 d . . . O2 O 0.7571(9) 0.0251(5) -0.0010(4) 0.144(2) Uani 1 d . . . C35 C 0.758(2) 0.0958(7) 0.1430(9) 0.200(6) Uani 1 d . . . H35A H 0.8443 0.1471 0.1432 0.3 Uiso 1 calc R . . H35B H 0.7624 0.0792 0.1932 0.3 Uiso 1 calc R . . H35C H 0.6451 0.1118 0.1298 0.3 Uiso 1 calc R . . C36 C 0.6248(12) -0.0710(6) 0.0932(5) 0.128(3) Uani 1 d . . . H36A H 0.6234 -0.1288 0.0597 0.192 Uiso 1 calc R . . H36B H 0.5181 -0.0461 0.0833 0.192 Uiso 1 calc R . . H36C H 0.6364 -0.0795 0.1459 0.192 Uiso 1 calc R . . O3 O 0.1792(15) 0.9794(6) 0.5598(5) 0.332(8) Uani 1 d DU . . OH1 H 0.1626 1.0061 0.6029 0.498 Uiso 1 d D . . OH2 H 0.2162 0.9319 0.5624 0.498 Uiso 1 d 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 Pd1 0.04581(15) 0.04596(14) 0.04344(14) 0.01116(10) 0.00869(10) 0.00450(10) Pd2 0.04558(15) 0.04304(14) 0.04102(14) 0.00940(9) 0.00428(9) 0.00252(9) Cl1 0.0603(5) 0.0638(5) 0.0541(5) 0.0221(4) 0.0083(4) -0.0017(4) Cl2 0.0961(9) 0.0604(6) 0.0912(8) 0.0001(6) 0.0258(7) -0.0040(6) N1 0.0504(16) 0.0471(14) 0.0428(14) 0.0071(11) 0.0038(12) 0.0050(12) N2 0.0630(19) 0.0515(16) 0.0412(14) 0.0083(12) 0.0050(13) 0.0053(13) N3 0.0454(15) 0.0494(15) 0.0412(14) 0.0069(11) 0.0018(11) 0.0014(12) N4 0.0490(16) 0.0498(15) 0.0417(14) 0.0076(12) 0.0070(12) 0.0029(12) N5 0.0522(16) 0.0568(16) 0.0481(15) 0.0123(13) 0.0116(13) 0.0134(13) N6 0.0459(16) 0.0587(17) 0.0655(19) 0.0276(15) 0.0121(14) 0.0040(13) N7 0.099(3) 0.060(2) 0.080(3) 0.0284(19) 0.024(2) 0.022(2) C1 0.059(2) 0.0519(18) 0.0445(17) 0.0117(14) 0.0039(15) 0.0043(15) C2 0.0465(18) 0.0511(17) 0.0473(17) 0.0174(14) 0.0017(14) 0.0020(14) C3 0.056(2) 0.0561(19) 0.0515(19) 0.0131(16) 0.0100(16) 0.0110(16) C4 0.057(2) 0.0518(19) 0.062(2) 0.0181(17) 0.0048(17) 0.0076(16) C5 0.074(3) 0.064(2) 0.053(2) 0.0248(18) 0.0087(18) 0.0048(19) C6 0.076(3) 0.065(2) 0.0470(19) 0.0152(17) 0.0106(18) 0.009(2) C7 0.059(2) 0.0450(17) 0.0469(17) 0.0068(14) 0.0088(15) 0.0018(15) C8 0.0504(19) 0.0422(16) 0.0525(18) 0.0059(14) 0.0083(15) 0.0030(14) C9 0.072(3) 0.0480(19) 0.075(3) 0.0107(18) 0.004(2) 0.0112(18) C10 0.106(4) 0.044(2) 0.088(3) 0.004(2) 0.009(3) 0.010(2) C11 0.106(4) 0.052(2) 0.069(3) -0.008(2) 0.000(3) -0.002(2) C12 0.076(3) 0.054(2) 0.052(2) 0.0011(16) 0.0011(18) 0.0008(18) C13 0.057(2) 0.063(2) 0.0453(18) 0.0085(16) 0.0076(15) -0.0030(17) C14 0.072(3) 0.069(2) 0.0446(19) -0.0022(17) 0.0121(18) -0.004(2) C15 0.072(3) 0.056(2) 0.059(2) -0.0032(18) 0.0062(19) -0.0011(19) C16 0.066(2) 0.0504(19) 0.053(2) 0.0081(16) 0.0056(17) -0.0029(16) C17 0.0434(17) 0.0478(16) 0.0446(17) 0.0075(13) 0.0005(13) 0.0043(13) C18 0.0388(16) 0.0503(17) 0.0445(16) 0.0084(13) 0.0031(12) 0.0011(13) C19 0.065(2) 0.056(2) 0.0507(19) 0.0111(16) 0.0063(17) -0.0068(17) C20 0.068(3) 0.074(3) 0.050(2) 0.0160(18) 0.0130(18) -0.009(2) C21 0.068(3) 0.075(3) 0.0468(19) 0.0043(18) 0.0168(18) 0.001(2) C22 0.059(2) 0.057(2) 0.0509(19) 0.0044(16) 0.0136(16) 0.0025(17) C23 0.071(3) 0.059(2) 0.057(2) 0.0078(17) 0.0122(19) 0.0122(19) C24 0.088(3) 0.066(3) 0.065(3) 0.002(2) 0.011(2) 0.018(2) C25 0.087(3) 0.091(3) 0.052(2) 0.002(2) 0.016(2) 0.030(3) C26 0.068(3) 0.097(3) 0.054(2) 0.024(2) 0.024(2) 0.024(2) C27 0.0467(19) 0.069(2) 0.057(2) 0.0196(18) 0.0138(16) 0.0202(17) C28 0.0429(18) 0.073(2) 0.059(2) 0.0288(18) 0.0129(15) 0.0167(16) C29 0.062(3) 0.089(3) 0.081(3) 0.039(3) 0.030(2) 0.014(2) C30 0.063(3) 0.089(3) 0.105(4) 0.049(3) 0.025(3) 0.003(2) C31 0.062(3) 0.067(3) 0.104(4) 0.031(3) 0.009(3) -0.006(2) C32 0.057(2) 0.065(2) 0.073(3) 0.017(2) 0.0120(19) -0.0033(18) S1 0.1648(18) 0.0662(7) 0.0996(11) 0.0128(7) 0.0366(11) 0.0179(9) O1 0.111(4) 0.086(3) 0.226(8) -0.027(4) 0.039(4) -0.012(3) C33 0.112(5) 0.078(4) 0.132(6) 0.008(4) 0.012(4) -0.008(3) C34 0.164(8) 0.069(4) 0.214(11) 0.048(5) -0.047(8) -0.003(4) S2 0.1006(11) 0.1362(14) 0.1225(13) 0.0762(12) 0.0418(10) 0.0459(10) O2 0.158(5) 0.177(6) 0.130(5) 0.097(5) 0.046(4) 0.041(4) C35 0.281(17) 0.129(8) 0.230(14) 0.079(9) 0.121(13) 0.064(9) C36 0.140(7) 0.134(6) 0.113(6) 0.064(5) -0.003(5) -0.026(5) O3 0.264(11) 0.296(11) 0.334(13) -0.205(10) 0.111(10) -0.067(9) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.995(3) . ? Pd1 N1 2.009(3) . ? Pd1 N5 2.066(3) . ? Pd1 N6 2.134(3) . ? Pd1 Pd2 3.1210(3) . ? Pd2 C8 1.993(4) . ? Pd2 N4 2.052(3) . ? Pd2 N3 2.121(3) . ? Pd2 Cl1 2.3091(9) . ? N1 N2 1.274(4) . ? N1 C7 1.441(5) . ? N2 C1 1.363(5) . ? N3 C13 1.334(5) . ? N3 C17 1.350(5) . ? N4 C22 1.336(5) . ? N4 C18 1.362(5) . ? N5 C23 1.341(6) . ? N5 C27 1.351(5) . ? N6 C32 1.339(6) . ? N6 C28 1.346(6) . ? N7 C4 1.348(5) . ? N7 HN1 0.85(5) . ? N7 HN2 0.88(2) . ? C1 C6 1.403(5) . ? C1 C2 1.419(5) . ? C2 C3 1.364(5) . ? C3 C4 1.431(5) . ? C3 H3 0.93 . ? C4 C5 1.406(6) . ? C5 C6 1.370(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.391(5) . ? C7 C8 1.401(6) . ? C8 C9 1.395(5) . ? C9 C10 1.389(7) . ? C9 H9 0.93 . ? C10 C11 1.372(8) . ? C10 H10 0.93 . ? C11 C12 1.384(7) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.373(6) . ? C13 H13 0.93 . ? C14 C15 1.373(6) . ? C14 H14 0.93 . ? C15 C16 1.381(6) . ? C15 H15 0.93 . ? C16 C17 1.388(5) . ? C16 H16 0.93 . ? C17 C18 1.470(5) . ? C18 C19 1.389(5) . ? C19 C20 1.384(6) . ? C19 H19 0.93 . ? C20 C21 1.377(7) . ? C20 H20 0.93 . ? C21 C22 1.377(6) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? C23 C24 1.380(6) . ? C23 H23 0.93 . ? C24 C25 1.358(8) . ? C24 H24 0.93 . ? C25 C26 1.366(8) . ? C25 H25 0.93 . ? C26 C27 1.390(6) . ? C26 H26 0.93 . ? C27 C28 1.467(6) . ? C28 C29 1.385(6) . ? C29 C30 1.385(8) . ? C29 H29 0.93 . ? C30 C31 1.365(9) . ? C30 H30 0.93 . ? C31 C32 1.387(6) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? S1 O1 1.480(7) . ? S1 C33 1.763(8) . ? S1 C34 1.766(7) . ? C33 H33A 0.96 . ? C33 H33B 0.96 . ? C33 H33C 0.96 . ? C34 H34A 0.96 . ? C34 H34B 0.96 . ? C34 H34C 0.96 . ? S2 O2 1.476(6) . ? S2 C35 1.715(13) . ? S2 C36 1.750(8) . ? C35 H35A 0.96 . ? C35 H35B 0.96 . ? C35 H35C 0.96 . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? O3 OH1 0.82 . ? O3 OH2 0.8 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 N1 78.40(14) . . ? C2 Pd1 N5 102.94(14) . . ? N1 Pd1 N5 170.41(12) . . ? C2 Pd1 N6 164.50(14) . . ? N1 Pd1 N6 102.94(13) . . ? N5 Pd1 N6 78.36(13) . . ? C2 Pd1 Pd2 110.42(11) . . ? N1 Pd1 Pd2 69.69(9) . . ? N5 Pd1 Pd2 101.17(9) . . ? N6 Pd1 Pd2 84.18(9) . . ? C8 Pd2 N4 94.36(13) . . ? C8 Pd2 N3 169.06(14) . . ? N4 Pd2 N3 79.15(12) . . ? C8 Pd2 Cl1 91.18(11) . . ? N4 Pd2 Cl1 172.40(9) . . ? N3 Pd2 Cl1 96.15(8) . . ? C8 Pd2 Pd1 82.53(11) . . ? N4 Pd2 Pd1 88.21(9) . . ? N3 Pd2 Pd1 88.43(8) . . ? Cl1 Pd2 Pd1 97.68(3) . . ? N2 N1 C7 115.0(3) . . ? N2 N1 Pd1 119.7(2) . . ? C7 N1 Pd1 124.6(2) . . ? N1 N2 C1 112.3(3) . . ? C13 N3 C17 119.0(3) . . ? C13 N3 Pd2 127.7(3) . . ? C17 N3 Pd2 112.6(2) . . ? C22 N4 C18 118.6(3) . . ? C22 N4 Pd2 126.8(3) . . ? C18 N4 Pd2 114.6(2) . . ? C23 N5 C27 118.9(4) . . ? C23 N5 Pd1 124.9(3) . . ? C27 N5 Pd1 115.5(3) . . ? C32 N6 C28 119.2(3) . . ? C32 N6 Pd1 126.7(3) . . ? C28 N6 Pd1 113.7(3) . . ? C4 N7 HN1 124(4) . . ? C4 N7 HN2 118(4) . . ? HN1 N7 HN2 118(5) . . ? N2 C1 C6 120.1(4) . . ? N2 C1 C2 118.8(3) . . ? C6 C1 C2 121.2(3) . . ? C3 C2 C1 118.2(3) . . ? C3 C2 Pd1 130.6(3) . . ? C1 C2 Pd1 110.7(3) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? N7 C4 C5 121.1(4) . . ? N7 C4 C3 119.5(4) . . ? C5 C4 C3 119.4(4) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 123.0(4) . . ? C12 C7 N1 118.9(4) . . ? C8 C7 N1 118.1(3) . . ? C9 C8 C7 116.5(4) . . ? C9 C8 Pd2 124.9(3) . . ? C7 C8 Pd2 118.5(3) . . ? C10 C9 C8 121.0(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 118.4(4) . . ? C11 C12 H12 120.8 . . ? C7 C12 H12 120.8 . . ? N3 C13 C14 122.5(4) . . ? N3 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N3 C17 C16 121.1(3) . . ? N3 C17 C18 116.0(3) . . ? C16 C17 C18 122.8(3) . . ? N4 C18 C19 120.7(3) . . ? N4 C18 C17 115.9(3) . . ? C19 C18 C17 123.3(3) . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 118.4(4) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N4 C22 C21 123.3(4) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N5 C23 C24 122.1(4) . . ? N5 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 118.9(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C27 120.5(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? N5 C27 C26 120.2(4) . . ? N5 C27 C28 116.4(4) . . ? C26 C27 C28 123.4(4) . . ? N6 C28 C29 121.2(4) . . ? N6 C28 C27 115.6(3) . . ? C29 C28 C27 123.3(4) . . ? C30 C29 C28 119.2(5) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C30 C29 119.4(4) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 119.0(5) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? N6 C32 C31 122.1(5) . . ? N6 C32 H32 119 . . ? C31 C32 H32 119 . . ? O1 S1 C33 106.7(4) . . ? O1 S1 C34 107.4(4) . . ? C33 S1 C34 97.6(5) . . ? S1 C33 H33A 109.5 . . ? S1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? S1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? S1 C34 H34A 109.5 . . ? S1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? S1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O2 S2 C35 107.9(5) . . ? O2 S2 C36 105.4(4) . . ? C35 S2 C36 95.9(5) . . ? S2 C35 H35A 109.5 . . ? S2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? S2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? S2 C36 H36A 109.5 . . ? S2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? S2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? OH1 O3 OH2 111 . . ? # Attachment '- 3b2.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_new _database_code_depnum_ccdc_archive 'CCDC 746376' #TrackingRef '- 3b2.cif' _audit_creation_date 2009-09-02T13:43:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C74 H58 Cl4 N16 O5 Pd4' _chemical_formula_sum 'C74 H58 Cl4 N16 O5 Pd4' _chemical_formula_weight 1818.76 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.2858(9) _cell_length_b 26.7698(8) _cell_length_c 17.6814(6) _cell_angle_alpha 90 _cell_angle_beta 122.432(2) _cell_angle_gamma 90 _cell_volume 7704.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10937 _cell_measurement_theta_min 2.9567 _cell_measurement_theta_max 76.0233 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3313 _exptl_absorpt_coefficient_mu 9.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5701 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4323 _diffrn_radiation_probe x-ray _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 21812 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 75.5 _diffrn_reflns_theta_full 76.48 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.97 _reflns_number_total 8032 _reflns_number_gt 6351 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.11 (release 31-10-2007 CrysAlis171 .NET) (compiled Oct 31 2007,17:16:07) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.1115P)^2^+1.0894P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8032 _refine_ls_number_parameters 501 _refine_ls_number_restraints 25 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1555 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.208 _refine_diff_density_min -1.319 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.364 0.702 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.031 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.049 0.032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.122 3.934 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.333 0.557 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Cl1 Cl 0.48774(7) 0.77006(5) 0.31908(10) 0.0721(3) Uani 1 d . . . N1 N 0.4603(2) 0.72646(13) 0.1271(2) 0.0475(7) Uani 1 d . . . N2 N 0.3875(2) 0.74453(15) 0.0829(2) 0.0514(8) Uani 1 d . . . N3 N 0.6783(2) 0.79546(15) 0.3925(2) 0.0550(8) Uani 1 d . . . N5 N 0.65696(19) 0.80984(13) 0.1792(2) 0.0498(8) Uani 1 d . . . C17 C 0.7568(3) 0.78840(19) 0.4154(3) 0.0549(10) Uani 1 d . . . N6 N 0.6370(2) 0.71213(14) 0.1527(2) 0.0498(7) Uani 1 d . . . C18 C 0.7759(3) 0.73784(18) 0.4012(3) 0.0547(10) Uani 1 d . . . C28 C 0.7108(3) 0.73060(16) 0.1714(3) 0.0506(9) Uani 1 d . . . C27 C 0.7237(2) 0.78349(17) 0.1936(3) 0.0500(9) Uani 1 d . . . C22 C 0.7277(3) 0.65726(18) 0.3503(3) 0.0608(11) Uani 1 d . . . H22 H 0.6844 0.6346 0.325 0.073 Uiso 1 calc R . . C7 C 0.4704(2) 0.67972(15) 0.1707(3) 0.0479(8) Uani 1 d . . . C32 C 0.6206(3) 0.66377(18) 0.1302(3) 0.0621(11) Uani 1 d . . . H32 H 0.5701 0.6513 0.1165 0.075 Uiso 1 calc R . . C8 C 0.5300(2) 0.67565(16) 0.2611(3) 0.0505(9) Uani 1 d . . . C26 C 0.7986(3) 0.8065(2) 0.2298(3) 0.0643(12) Uani 1 d . . . H26 H 0.8436 0.7883 0.2392 0.077 Uiso 1 calc R . . C19 C 0.8547(3) 0.7235(2) 0.4260(4) 0.0714(14) Uani 1 d . . . H19 H 0.8977 0.7464 0.4522 0.086 Uiso 1 calc R . . C12 C 0.4186(3) 0.64035(18) 0.1226(3) 0.0582(10) Uani 1 d . . . H12 H 0.3793 0.6441 0.0619 0.07 Uiso 1 calc R . . C11 C 0.4256(3) 0.59565(18) 0.1648(4) 0.0697(13) Uani 1 d . . . H11 H 0.3916 0.5689 0.1325 0.084 Uiso 1 calc R . . C21 C 0.8041(3) 0.6408(2) 0.3733(4) 0.0719(13) Uani 1 d . . . H21 H 0.8122 0.6078 0.3635 0.086 Uiso 1 calc R . . C14 C 0.7066(3) 0.8817(2) 0.4292(4) 0.0768(14) Uani 1 d . . . H14 H 0.6886 0.9132 0.4331 0.092 Uiso 1 calc R . . C31 C 0.6732(4) 0.6320(2) 0.1262(4) 0.0722(13) Uani 1 d . . . H31 H 0.6592 0.5987 0.1103 0.087 Uiso 1 calc R . . C29 C 0.7669(3) 0.6996(2) 0.1686(3) 0.0665(12) Uani 1 d . . . H29 H 0.8172 0.7123 0.1819 0.08 Uiso 1 calc R . . C24 C 0.7414(3) 0.88186(19) 0.2388(3) 0.0668(12) Uani 1 d . . . H24 H 0.7459 0.9155 0.2538 0.08 Uiso 1 calc R . . C15 C 0.7861(4) 0.8742(2) 0.4528(4) 0.0777(15) Uani 1 d . . . H15 H 0.8225 0.901 0.4733 0.093 Uiso 1 calc R . . C16 C 0.8127(3) 0.8281(2) 0.4466(3) 0.0676(13) Uani 1 d . . . H16 H 0.8667 0.8232 0.4627 0.081 Uiso 1 calc R . . C23 C 0.6676(3) 0.85763(17) 0.2027(3) 0.0590(10) Uani 1 d . . . H23 H 0.6227 0.8756 0.1943 0.071 Uiso 1 calc R . . C25 C 0.8075(3) 0.8563(2) 0.2524(4) 0.0737(14) Uani 1 d . . . H25 H 0.8581 0.872 0.2766 0.088 Uiso 1 calc R . . C13 C 0.6542(3) 0.8413(2) 0.3998(3) 0.0674(12) Uani 1 d . . . H13 H 0.6004 0.8459 0.3845 0.081 Uiso 1 calc R . . C9 C 0.5344(3) 0.6298(2) 0.3017(3) 0.0655(12) Uani 1 d . . . H9 H 0.5734 0.6258 0.3624 0.079 Uiso 1 calc R . . C10 C 0.4833(3) 0.59080(19) 0.2551(4) 0.0733(14) Uani 1 d . . . H10 H 0.4875 0.561 0.2843 0.088 Uiso 1 calc R . . Cl2 Cl 0.21415(17) 1 -0.1617(2) 0.1079(8) Uani 1 d S . . Cl3 Cl 0.5576(4) 1 0.1360(4) 0.199(2) Uani 1 d S . . C30 C 0.7484(3) 0.6505(2) 0.1464(4) 0.0724(13) Uani 1 d . . . H30 H 0.7861 0.6295 0.1449 0.087 Uiso 1 calc R . . C20 C 0.8682(3) 0.6743(3) 0.4111(4) 0.0803(15) Uani 1 d . . . H20 H 0.9204 0.6642 0.4267 0.096 Uiso 1 calc R . . N8 N 0.7766(6) 0.5 0.3486(6) 0.139(4) Uani 1 d SD . . C37 C 0.7037(6) 0.5 0.2746(6) 0.095(3) Uani 1 d SD . . N9 N 0.6254(8) 0.5 0.1131(6) 0.142(5) Uani 1 d SD . . C38 C 0.7008(7) 0.5 0.1910(7) 0.100(3) Uani 1 d SD . . C35 C 0.6415(7) 0.5 0.3577(8) 0.128(5) Uani 1 d SD . . H35 H 0.5943 0.5 0.3597 0.154 Uiso 1 calc SR . . C33 C 0.7783(8) 0.5 0.4242(8) 0.143(5) Uani 1 d SD . . H33 H 0.8301 0.5 0.4767 0.171 Uiso 1 calc SR . . C36 C 0.6361(7) 0.5 0.2814(8) 0.149(6) Uani 1 d SD . . H36 H 0.5842 0.5 0.2291 0.178 Uiso 1 calc SR . . C39 C 0.7632(10) 0.5 0.1836(10) 0.143(5) Uani 1 d SD . . H39 H 0.8144 0.5 0.2369 0.171 Uiso 1 calc SR . . C40 C 0.7633(13) 0.5 0.1076(12) 0.174(7) Uani 1 d SD . . H40 H 0.8123 0.5 0.1092 0.209 Uiso 1 calc SR . . O1 O 0.1215(4) 1 -0.3545(5) 0.127(3) Uani 1 d S . . O3 O 1 0.9238(3) 0.5 0.161(4) Uani 1 d S . . C34 C 0.7164(7) 0.5 0.4343(8) 0.109(3) Uani 1 d SD . . H34 H 0.7232 0.5 0.4905 0.131 Uiso 1 calc SR . . O2 O 0.7192(13) 1 0.3475(11) 0.240(8) Uani 1 d S . . C41 C 0.6929(14) 0.5 0.0321(11) 0.164(9) Uani 1 d SD . . H41 H 0.6907 0.5 -0.0218 0.197 Uiso 1 calc SR . . O4 O 1.0100(5) 0.8180(4) 0.5407(6) 0.103(3) Uani 0.5 d P . . C42 C 0.6191(14) 0.5 0.0322(10) 0.161(8) Uani 1 d SD . . H42 H 0.5681 0.5 -0.0213 0.194 Uiso 1 calc SR . . O5A O 0.9827(16) 0.5 0.6580(18) 0.183(9) Uani 0.5 d SPU . . O5B O 0.997(4) 0.5 0.582(4) 0.41(2) Uani 0.5 d SPU . . Pd2 Pd 0.600937(17) 0.733682(11) 0.330510(19) 0.04816(12) Uani 1 d . . . Pd1 Pd 0.553633(16) 0.767789(10) 0.14200(2) 0.04569(12) Uani 1 d . . . N4 N 0.7124(2) 0.70466(15) 0.3626(2) 0.0523(8) Uani 1 d . . . C1 C 0.3862(2) 0.79245(17) 0.0572(3) 0.0494(9) Uani 1 d . . . C2 C 0.4620(2) 0.81706(16) 0.0876(3) 0.0513(9) Uani 1 d . . . N7 N 0.3814(3) 0.93955(19) -0.0105(5) 0.120(2) Uani 1 d . . . H7B H 0.3353 0.9549 -0.0424 0.144 Uiso 1 calc R . . H7A H 0.4267 0.955 0.0072 0.144 Uiso 1 calc R . . C5 C 0.3101(3) 0.86578(18) -0.0163(3) 0.0600(10) Uani 1 d . . . H5 H 0.2603 0.8824 -0.0501 0.072 Uiso 1 calc R . . C4 C 0.3827(3) 0.8908(2) 0.0120(4) 0.0705(13) Uani 1 d . . . C6 C 0.3112(2) 0.81737(19) 0.0049(3) 0.0567(10) Uani 1 d . . . H6 H 0.2621 0.8005 -0.0152 0.068 Uiso 1 calc R . . C3 C 0.4585(3) 0.86577(18) 0.0642(4) 0.0708(13) Uani 1 d . . . H3 H 0.5071 0.883 0.0829 0.085 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0428(6) 0.0863(8) 0.0827(8) -0.0199(6) 0.0307(5) -0.0074(5) N1 0.0348(16) 0.0555(18) 0.0466(16) 0.0000(14) 0.0182(13) -0.0043(13) N2 0.0313(16) 0.066(2) 0.0485(17) 0.0037(15) 0.0157(13) -0.0035(14) N3 0.0442(18) 0.066(2) 0.0485(17) -0.0066(16) 0.0208(14) -0.0108(16) N5 0.0349(15) 0.0569(19) 0.0549(18) 0.0094(15) 0.0224(13) 0.0005(13) C17 0.042(2) 0.074(3) 0.0407(18) -0.0006(19) 0.0175(15) -0.0133(19) N6 0.0425(17) 0.0564(19) 0.0518(17) 0.0037(15) 0.0261(14) 0.0018(14) C18 0.040(2) 0.076(3) 0.0414(19) 0.0035(18) 0.0179(16) -0.0035(18) C28 0.047(2) 0.062(2) 0.047(2) 0.0115(17) 0.0283(18) 0.0088(17) C27 0.0353(18) 0.066(2) 0.0458(18) 0.0107(18) 0.0195(15) -0.0007(17) C22 0.053(2) 0.064(3) 0.058(2) 0.008(2) 0.0246(19) 0.002(2) C7 0.0392(18) 0.0514(19) 0.0520(19) -0.0014(17) 0.0237(15) -0.0048(15) C32 0.062(3) 0.061(2) 0.068(3) -0.001(2) 0.038(2) 0.000(2) C8 0.0358(18) 0.055(2) 0.056(2) -0.0009(17) 0.0214(15) -0.0065(16) C26 0.040(2) 0.089(3) 0.068(3) 0.011(2) 0.0311(19) 0.001(2) C19 0.041(2) 0.099(4) 0.066(3) 0.009(3) 0.024(2) -0.005(2) C12 0.045(2) 0.065(3) 0.059(2) -0.010(2) 0.0242(18) -0.0116(19) C11 0.066(3) 0.053(2) 0.090(3) -0.011(2) 0.041(3) -0.018(2) C21 0.065(3) 0.076(3) 0.075(3) 0.014(3) 0.038(2) 0.018(3) C14 0.078(3) 0.070(3) 0.079(3) -0.023(3) 0.040(3) -0.018(3) C31 0.093(4) 0.059(3) 0.073(3) -0.003(2) 0.051(3) 0.008(3) C29 0.051(2) 0.086(3) 0.068(3) 0.012(3) 0.035(2) 0.015(2) C24 0.064(3) 0.061(3) 0.071(3) 0.002(2) 0.033(2) -0.014(2) C15 0.076(3) 0.079(3) 0.065(3) -0.015(3) 0.030(2) -0.031(3) C16 0.052(2) 0.086(3) 0.055(2) -0.009(2) 0.022(2) -0.020(2) C23 0.049(2) 0.054(2) 0.068(3) 0.005(2) 0.0277(19) -0.0046(18) C25 0.053(3) 0.086(4) 0.074(3) 0.002(3) 0.029(2) -0.025(3) C13 0.061(3) 0.073(3) 0.068(3) -0.018(2) 0.034(2) -0.013(2) C9 0.056(2) 0.069(3) 0.061(3) 0.014(2) 0.025(2) 0.002(2) C10 0.069(3) 0.054(2) 0.096(4) 0.013(2) 0.044(3) -0.006(2) Cl2 0.1017(17) 0.0689(12) 0.132(2) 0 0.0486(15) 0 Cl3 0.210(5) 0.184(5) 0.200(5) 0 0.107(5) 0 C30 0.073(3) 0.079(3) 0.077(3) 0.003(3) 0.047(3) 0.021(3) C20 0.053(3) 0.104(4) 0.082(3) 0.011(3) 0.034(2) 0.016(3) N8 0.117(8) 0.176(11) 0.091(6) 0 0.032(6) 0 C37 0.102(7) 0.058(4) 0.082(5) 0 0.021(5) 0 N9 0.196(11) 0.075(5) 0.078(5) 0 0.023(6) 0 C38 0.098(7) 0.065(5) 0.106(8) 0 0.033(6) 0 C35 0.082(7) 0.177(13) 0.099(8) 0 0.030(6) 0 C33 0.098(9) 0.197(16) 0.089(8) 0 0.021(6) 0 C36 0.062(6) 0.209(16) 0.113(9) 0 0.006(6) 0 C39 0.157(14) 0.134(12) 0.107(9) 0 0.051(9) 0 C40 0.24(2) 0.143(15) 0.168(17) 0 0.134(19) 0 O1 0.089(4) 0.104(5) 0.107(5) 0 -0.001(4) 0 O3 0.187(9) 0.068(4) 0.115(6) 0 0.007(5) 0 C34 0.116(9) 0.072(5) 0.111(8) 0 0.043(7) 0 O2 0.47(3) 0.110(8) 0.252(16) 0 0.265(18) 0 C41 0.28(3) 0.078(7) 0.095(9) 0 0.073(14) 0 O4 0.050(4) 0.147(8) 0.108(6) -0.012(6) 0.040(5) -0.003(5) C42 0.26(2) 0.075(7) 0.100(9) 0 0.060(13) 0 O5A 0.182(9) 0.183(9) 0.183(9) 0 0.098(5) 0 O5B 0.41(2) 0.41(2) 0.41(2) 0 0.222(11) 0 Pd2 0.03485(18) 0.0572(2) 0.04527(18) -0.00117(11) 0.01674(13) -0.00699(10) Pd1 0.03242(17) 0.04885(19) 0.05382(19) 0.00455(11) 0.02182(14) -0.00027(10) N4 0.0364(16) 0.067(2) 0.0443(16) 0.0075(15) 0.0158(13) -0.0023(14) C1 0.0322(17) 0.064(2) 0.0447(18) 0.0020(17) 0.0160(14) 0.0007(16) C2 0.0381(19) 0.058(2) 0.056(2) 0.0062(18) 0.0237(16) 0.0049(16) N7 0.060(3) 0.066(3) 0.185(6) 0.043(4) 0.034(3) 0.010(2) C5 0.043(2) 0.070(3) 0.058(2) 0.010(2) 0.0206(17) 0.0120(19) C4 0.053(3) 0.062(3) 0.083(3) 0.009(2) 0.028(2) 0.009(2) C6 0.0379(19) 0.074(3) 0.050(2) 0.0054(19) 0.0186(16) 0.0032(18) C3 0.044(2) 0.057(2) 0.095(3) 0.015(2) 0.026(2) 0.0042(19) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Pd2 2.2991(13) . ? N1 N2 1.281(5) . ? N1 C7 1.427(5) . ? N1 Pd1 2.005(3) . ? N2 C1 1.356(6) . ? N3 C13 1.342(6) . ? N3 C17 1.356(6) . ? N3 Pd2 2.099(4) . ? N5 C23 1.327(6) . ? N5 C27 1.367(5) . ? N5 Pd1 2.065(3) . ? C17 C16 1.398(6) . ? C17 C18 1.460(7) . ? N6 C32 1.341(6) . ? N6 C28 1.368(6) . ? N6 Pd1 2.126(4) . ? C18 N4 1.362(6) . ? C18 C19 1.390(7) . ? C28 C29 1.385(6) . ? C28 C27 1.455(6) . ? C27 C26 1.372(6) . ? C22 N4 1.347(6) . ? C22 C21 1.374(7) . ? C22 H22 0.93 . ? C7 C8 1.385(6) . ? C7 C12 1.385(6) . ? C32 C31 1.355(7) . ? C32 H32 0.93 . ? C8 C9 1.401(6) . ? C8 Pd2 1.997(4) . ? C26 C25 1.375(8) . ? C26 H26 0.93 . ? C19 C20 1.396(8) . ? C19 H19 0.93 . ? C12 C11 1.378(7) . ? C12 H12 0.93 . ? C11 C10 1.378(8) . ? C11 H11 0.93 . ? C21 C20 1.376(8) . ? C21 H21 0.93 . ? C14 C15 1.371(8) . ? C14 C13 1.378(7) . ? C14 H14 0.93 . ? C31 C30 1.385(8) . ? C31 H31 0.93 . ? C29 C30 1.365(8) . ? C29 H29 0.93 . ? C24 C25 1.351(8) . ? C24 C23 1.370(6) . ? C24 H24 0.93 . ? C15 C16 1.362(8) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C23 H23 0.93 . ? C25 H25 0.93 . ? C13 H13 0.93 . ? C9 C10 1.367(7) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? C30 H30 0.93 . ? C20 H20 0.93 . ? N8 C37 1.309(11) . ? N8 C33 1.321(12) . ? C37 C36 1.372(13) . ? C37 C38 1.449(13) . ? N9 C38 1.365(12) . ? N9 C42 1.371(14) . ? C38 C39 1.279(14) . ? C35 C36 1.296(13) . ? C35 C34 1.349(12) . ? C35 H35 0.93 . ? C33 C34 1.297(13) . ? C33 H33 0.93 . ? C36 H36 0.93 . ? C39 C40 1.344(15) . ? C39 H39 0.93 . ? C40 C41 1.297(15) . ? C40 H40 0.93 . ? C34 H34 0.93 . ? C41 C42 1.424(16) . ? C41 H41 0.93 . ? O4 O4 1.273(17) 2_756 ? C42 H42 0.93 . ? O5A O5B 1.51(5) . ? Pd2 N4 2.060(4) . ? Pd2 Pd1 3.0842(4) . ? Pd1 C2 1.992(4) . ? C1 C6 1.399(6) . ? C1 C2 1.420(6) . ? C2 C3 1.359(6) . ? N7 C4 1.361(7) . ? N7 H7B 0.86 . ? N7 H7A 0.86 . ? C5 C6 1.346(7) . ? C5 C4 1.379(7) . ? C5 H5 0.93 . ? C4 C3 1.412(6) . ? C6 H6 0.93 . ? C3 H3 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 N1 C7 116.6(3) . . ? N2 N1 Pd1 119.0(3) . . ? C7 N1 Pd1 124.1(3) . . ? N1 N2 C1 112.3(3) . . ? C13 N3 C17 119.2(4) . . ? C13 N3 Pd2 125.8(3) . . ? C17 N3 Pd2 114.4(3) . . ? C23 N5 C27 117.9(4) . . ? C23 N5 Pd1 125.8(3) . . ? C27 N5 Pd1 115.4(3) . . ? N3 C17 C16 120.8(5) . . ? N3 C17 C18 115.0(4) . . ? C16 C17 C18 124.1(4) . . ? C32 N6 C28 118.0(4) . . ? C32 N6 Pd1 127.1(3) . . ? C28 N6 Pd1 114.0(3) . . ? N4 C18 C19 120.9(5) . . ? N4 C18 C17 116.7(4) . . ? C19 C18 C17 122.4(4) . . ? N6 C28 C29 120.4(4) . . ? N6 C28 C27 114.9(4) . . ? C29 C28 C27 124.7(4) . . ? N5 C27 C26 120.4(4) . . ? N5 C27 C28 116.4(3) . . ? C26 C27 C28 123.2(4) . . ? N4 C22 C21 123.3(5) . . ? N4 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? C8 C7 C12 121.8(4) . . ? C8 C7 N1 118.7(4) . . ? C12 C7 N1 119.4(4) . . ? N6 C32 C31 123.9(5) . . ? N6 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? C7 C8 C9 116.4(4) . . ? C7 C8 Pd2 121.3(3) . . ? C9 C8 Pd2 122.2(3) . . ? C27 C26 C25 120.4(5) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C18 C19 C20 119.0(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C11 C12 C7 119.9(4) . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C22 C21 C20 118.4(5) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C15 C14 C13 118.3(5) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C32 C31 C30 118.2(5) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C30 C29 C28 119.9(5) . . ? C30 C29 H29 120 . . ? C28 C29 H29 120 . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.4(5) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? N5 C23 C24 123.3(5) . . ? N5 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C24 C25 C26 118.8(4) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N3 C13 C14 122.1(5) . . ? N3 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C10 C9 C8 122.3(4) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C29 C30 C31 119.6(5) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C21 C20 C19 119.8(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C37 N8 C33 116.2(12) . . ? N8 C37 C36 118.3(11) . . ? N8 C37 C38 116.9(11) . . ? C36 C37 C38 124.8(10) . . ? C38 N9 C42 120.1(15) . . ? C39 C38 N9 116.7(13) . . ? C39 C38 C37 125.5(11) . . ? N9 C38 C37 117.8(12) . . ? C36 C35 C34 119.3(13) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C34 C33 N8 127.9(12) . . ? C34 C33 H33 116.1 . . ? N8 C33 H33 116.1 . . ? C35 C36 C37 122.8(11) . . ? C35 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C38 C39 C40 127.4(17) . . ? C38 C39 H39 116.3 . . ? C40 C39 H39 116.3 . . ? C41 C40 C39 117.9(19) . . ? C41 C40 H40 121.1 . . ? C39 C40 H40 121.1 . . ? C33 C34 C35 115.5(13) . . ? C33 C34 H34 122.2 . . ? C35 C34 H34 122.2 . . ? C40 C41 C42 120(2) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? N9 C42 C41 118.3(18) . . ? N9 C42 H42 120.9 . . ? C41 C42 H42 120.9 . . ? C8 Pd2 N4 98.38(16) . . ? C8 Pd2 N3 173.81(16) . . ? N4 Pd2 N3 79.02(15) . . ? C8 Pd2 Cl1 88.29(12) . . ? N4 Pd2 Cl1 170.52(10) . . ? N3 Pd2 Cl1 94.98(11) . . ? C8 Pd2 Pd1 81.84(12) . . ? N4 Pd2 Pd1 94.00(9) . . ? N3 Pd2 Pd1 92.69(10) . . ? Cl1 Pd2 Pd1 93.61(4) . . ? C2 Pd1 N1 78.48(16) . . ? C2 Pd1 N5 104.35(15) . . ? N1 Pd1 N5 170.75(14) . . ? C2 Pd1 N6 160.19(15) . . ? N1 Pd1 N6 101.99(14) . . ? N5 Pd1 N6 78.39(14) . . ? C2 Pd1 Pd2 112.90(12) . . ? N1 Pd1 Pd2 72.75(10) . . ? N5 Pd1 Pd2 98.13(9) . . ? N6 Pd1 Pd2 85.71(9) . . ? C22 N4 C18 118.6(4) . . ? C22 N4 Pd2 126.7(3) . . ? C18 N4 Pd2 114.6(3) . . ? N2 C1 C6 120.0(4) . . ? N2 C1 C2 118.7(3) . . ? C6 C1 C2 121.2(4) . . ? C3 C2 C1 117.2(4) . . ? C3 C2 Pd1 132.0(3) . . ? C1 C2 Pd1 110.0(3) . . ? C4 N7 H7B 120 . . ? C4 N7 H7A 120 . . ? H7B N7 H7A 120 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N7 C4 C5 120.2(5) . . ? N7 C4 C3 119.7(5) . . ? C5 C4 C3 120.1(5) . . ? C5 C6 C1 120.0(4) . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C2 C3 C4 121.3(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? 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 C7 N1 N2 C1 169.2(3) . . . . ? Pd1 N1 N2 C1 -4.4(5) . . . . ? C13 N3 C17 C16 0.2(7) . . . . ? Pd2 N3 C17 C16 171.7(3) . . . . ? C13 N3 C17 C18 -177.3(4) . . . . ? Pd2 N3 C17 C18 -5.8(5) . . . . ? N3 C17 C18 N4 3.4(6) . . . . ? C16 C17 C18 N4 -174.1(4) . . . . ? N3 C17 C18 C19 -176.1(4) . . . . ? C16 C17 C18 C19 6.5(7) . . . . ? C32 N6 C28 C29 -1.3(6) . . . . ? Pd1 N6 C28 C29 -171.5(3) . . . . ? C32 N6 C28 C27 178.9(4) . . . . ? Pd1 N6 C28 C27 8.7(4) . . . . ? C23 N5 C27 C26 -1.2(6) . . . . ? Pd1 N5 C27 C26 -171.4(3) . . . . ? C23 N5 C27 C28 176.9(4) . . . . ? Pd1 N5 C27 C28 6.7(4) . . . . ? N6 C28 C27 N5 -10.3(5) . . . . ? C29 C28 C27 N5 169.9(4) . . . . ? N6 C28 C27 C26 167.7(4) . . . . ? C29 C28 C27 C26 -12.1(7) . . . . ? N2 N1 C7 C8 -127.6(4) . . . . ? Pd1 N1 C7 C8 45.6(5) . . . . ? N2 N1 C7 C12 50.1(5) . . . . ? Pd1 N1 C7 C12 -136.7(3) . . . . ? C28 N6 C32 C31 1.1(7) . . . . ? Pd1 N6 C32 C31 169.8(4) . . . . ? C12 C7 C8 C9 -0.9(6) . . . . ? N1 C7 C8 C9 176.8(4) . . . . ? C12 C7 C8 Pd2 -177.5(3) . . . . ? N1 C7 C8 Pd2 0.2(5) . . . . ? N5 C27 C26 C25 0.3(7) . . . . ? C28 C27 C26 C25 -177.6(4) . . . . ? N4 C18 C19 C20 -0.2(8) . . . . ? C17 C18 C19 C20 179.3(5) . . . . ? C8 C7 C12 C11 0.2(7) . . . . ? N1 C7 C12 C11 -177.5(4) . . . . ? C7 C12 C11 C10 1.0(8) . . . . ? N4 C22 C21 C20 0.3(8) . . . . ? N6 C32 C31 C30 -0.1(8) . . . . ? N6 C28 C29 C30 0.6(7) . . . . ? C27 C28 C29 C30 -179.6(4) . . . . ? C13 C14 C15 C16 0.6(9) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? N3 C17 C16 C15 -0.5(7) . . . . ? C18 C17 C16 C15 176.8(4) . . . . ? C27 N5 C23 C24 1.4(7) . . . . ? Pd1 N5 C23 C24 170.5(4) . . . . ? C25 C24 C23 N5 -0.7(8) . . . . ? C23 C24 C25 C26 -0.3(8) . . . . ? C27 C26 C25 C24 0.5(8) . . . . ? C17 N3 C13 C14 0.5(7) . . . . ? Pd2 N3 C13 C14 -170.0(4) . . . . ? C15 C14 C13 N3 -0.9(8) . . . . ? C7 C8 C9 C10 0.4(7) . . . . ? Pd2 C8 C9 C10 177.0(4) . . . . ? C8 C9 C10 C11 0.8(9) . . . . ? C12 C11 C10 C9 -1.5(9) . . . . ? C28 C29 C30 C31 0.4(8) . . . . ? C32 C31 C30 C29 -0.7(8) . . . . ? C22 C21 C20 C19 0.7(8) . . . . ? C18 C19 C20 C21 -0.7(9) . . . . ? C33 N8 C37 C36 0.000(2) . . . . ? C33 N8 C37 C38 180.000(2) . . . . ? C42 N9 C38 C39 0.000(2) . . . . ? C42 N9 C38 C37 180.000(2) . . . . ? N8 C37 C38 C39 0.000(3) . . . . ? C36 C37 C38 C39 180.000(2) . . . . ? N8 C37 C38 N9 180.000(2) . . . . ? C36 C37 C38 N9 0.000(2) . . . . ? C37 N8 C33 C34 0.000(3) . . . . ? C34 C35 C36 C37 0.000(4) . . . . ? N8 C37 C36 C35 0.000(3) . . . . ? C38 C37 C36 C35 180.000(3) . . . . ? N9 C38 C39 C40 0.000(3) . . . . ? C37 C38 C39 C40 180.000(2) . . . . ? C38 C39 C40 C41 0.000(3) . . . . ? N8 C33 C34 C35 0.000(4) . . . . ? C36 C35 C34 C33 0.000(4) . . . . ? C39 C40 C41 C42 0.0000(10) . . . . ? C38 N9 C42 C41 0.0000(10) . . . . ? C40 C41 C42 N9 0.0000(10) . . . . ? C7 C8 Pd2 N4 -115.9(3) . . . . ? C9 C8 Pd2 N4 67.7(4) . . . . ? C7 C8 Pd2 N3 -51.2(16) . . . . ? C9 C8 Pd2 N3 132.4(14) . . . . ? C7 C8 Pd2 Cl1 70.8(3) . . . . ? C9 C8 Pd2 Cl1 -105.6(4) . . . . ? C7 C8 Pd2 Pd1 -23.1(3) . . . . ? C9 C8 Pd2 Pd1 160.5(4) . . . . ? C13 N3 Pd2 C8 110.0(15) . . . . ? C17 N3 Pd2 C8 -60.9(16) . . . . ? C13 N3 Pd2 N4 175.7(4) . . . . ? C17 N3 Pd2 N4 4.8(3) . . . . ? C13 N3 Pd2 Cl1 -11.7(4) . . . . ? C17 N3 Pd2 Cl1 177.4(3) . . . . ? C13 N3 Pd2 Pd1 82.1(4) . . . . ? C17 N3 Pd2 Pd1 -88.7(3) . . . . ? N2 N1 Pd1 C2 8.8(3) . . . . ? C7 N1 Pd1 C2 -164.3(4) . . . . ? N2 N1 Pd1 N5 117.6(8) . . . . ? C7 N1 Pd1 N5 -55.5(10) . . . . ? N2 N1 Pd1 N6 -151.0(3) . . . . ? C7 N1 Pd1 N6 35.9(3) . . . . ? N2 N1 Pd1 Pd2 127.4(3) . . . . ? C7 N1 Pd1 Pd2 -45.7(3) . . . . ? C23 N5 Pd1 C2 29.3(4) . . . . ? C27 N5 Pd1 C2 -161.4(3) . . . . ? C23 N5 Pd1 N1 -77.4(9) . . . . ? C27 N5 Pd1 N1 91.8(9) . . . . ? C23 N5 Pd1 N6 -170.8(4) . . . . ? C27 N5 Pd1 N6 -1.5(3) . . . . ? C23 N5 Pd1 Pd2 -86.9(4) . . . . ? C27 N5 Pd1 Pd2 82.4(3) . . . . ? C32 N6 Pd1 C2 -73.0(6) . . . . ? C28 N6 Pd1 C2 96.1(5) . . . . ? C32 N6 Pd1 N1 16.2(4) . . . . ? C28 N6 Pd1 N1 -174.6(3) . . . . ? C32 N6 Pd1 N5 -173.2(4) . . . . ? C28 N6 Pd1 N5 -4.1(3) . . . . ? C32 N6 Pd1 Pd2 87.6(4) . . . . ? C28 N6 Pd1 Pd2 -103.3(3) . . . . ? C8 Pd2 Pd1 C2 98.55(18) . . . . ? N4 Pd2 Pd1 C2 -163.54(17) . . . . ? N3 Pd2 Pd1 C2 -84.37(17) . . . . ? Cl1 Pd2 Pd1 C2 10.79(14) . . . . ? C8 Pd2 Pd1 N1 29.54(16) . . . . ? N4 Pd2 Pd1 N1 127.45(15) . . . . ? N3 Pd2 Pd1 N1 -153.38(15) . . . . ? Cl1 Pd2 Pd1 N1 -58.22(11) . . . . ? C8 Pd2 Pd1 N5 -152.05(16) . . . . ? N4 Pd2 Pd1 N5 -54.14(15) . . . . ? N3 Pd2 Pd1 N5 25.03(14) . . . . ? Cl1 Pd2 Pd1 N5 120.20(10) . . . . ? C8 Pd2 Pd1 N6 -74.43(15) . . . . ? N4 Pd2 Pd1 N6 23.48(15) . . . . ? N3 Pd2 Pd1 N6 102.64(14) . . . . ? Cl1 Pd2 Pd1 N6 -162.19(10) . . . . ? C21 C22 N4 C18 -1.2(7) . . . . ? C21 C22 N4 Pd2 179.7(4) . . . . ? C19 C18 N4 C22 1.1(6) . . . . ? C17 C18 N4 C22 -178.4(4) . . . . ? C19 C18 N4 Pd2 -179.7(4) . . . . ? C17 C18 N4 Pd2 0.8(5) . . . . ? C8 Pd2 N4 C22 -9.5(4) . . . . ? N3 Pd2 N4 C22 176.2(4) . . . . ? Cl1 Pd2 N4 C22 124.9(6) . . . . ? Pd1 Pd2 N4 C22 -91.8(4) . . . . ? C8 Pd2 N4 C18 171.3(3) . . . . ? N3 Pd2 N4 C18 -3.0(3) . . . . ? Cl1 Pd2 N4 C18 -54.3(8) . . . . ? Pd1 Pd2 N4 C18 89.0(3) . . . . ? N1 N2 C1 C6 177.3(4) . . . . ? N1 N2 C1 C2 -5.4(6) . . . . ? N2 C1 C2 C3 -176.9(5) . . . . ? C6 C1 C2 C3 0.3(7) . . . . ? N2 C1 C2 Pd1 12.1(5) . . . . ? C6 C1 C2 Pd1 -170.6(3) . . . . ? N1 Pd1 C2 C3 -179.4(5) . . . . ? N5 Pd1 C2 C3 9.7(5) . . . . ? N6 Pd1 C2 C3 -85.9(7) . . . . ? Pd2 Pd1 C2 C3 115.1(5) . . . . ? N1 Pd1 C2 C1 -10.2(3) . . . . ? N5 Pd1 C2 C1 178.8(3) . . . . ? N6 Pd1 C2 C1 83.2(5) . . . . ? Pd2 Pd1 C2 C1 -75.7(3) . . . . ? C6 C5 C4 N7 179.2(6) . . . . ? C6 C5 C4 C3 -0.7(8) . . . . ? C4 C5 C6 C1 1.2(7) . . . . ? N2 C1 C6 C5 176.2(4) . . . . ? C2 C1 C6 C5 -1.0(7) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? Pd1 C2 C3 C4 168.7(4) . . . . ? N7 C4 C3 C2 -179.9(6) . . . . ? C5 C4 C3 C2 0.0(9) . . . . ? # start Validation Reply Form _vrf_PLAT306_new ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 Isolated Oxygen Atom (H-atoms Missing ?) ....... O2 Isolated Oxygen Atom (H-atoms Missing ?) ....... O3 Short Inter HL..A Contact Cl2 .. O1 .. 2.88 Ang. Structure Contains Solvent Accessible VOIDS of . 59.00 A**3 RESPONSE: The strucutre contains disordered water molecules. Due to the presence of heavy Pd atoms (and a large number of lighter ones, Cl, N, C, O), it could not be modelled correctly. Hydrogen atoms could not be attached to water molecules because of the disorder. ;