# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Song, Datong' _publ_contact_author_email dsong@chem.utoronto.ca _publ_section_title ; Unusual transmetallation-induced formation of a C2-symmetric tetrapallada-macrocycle ; loop_ _publ_author_name D.Song V.Annibale L.Lund data_complex2 _database_code_depnum_ccdc_archive 'CCDC 779764' #TrackingRef 'complex2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Cl N3 Pd' _chemical_formula_weight 470.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pc2(1)b loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, y, z+1/2' 'x, y+1/2, -z+1/2' _cell_length_a 6.4520(5) _cell_length_b 10.7360(10) _cell_length_c 29.278(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2028.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6717 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6717 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2883 _reflns_number_gt 2441 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+2.6489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 2883 _refine_ls_number_parameters 246 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.70727(6) -0.16004(6) -0.115972(13) 0.02242(13) Uani 1 1 d . . . Cl1 Cl -0.5522(2) -0.21808(15) -0.04749(5) 0.0306(4) Uani 1 1 d . . . N1 N -0.5552(7) -0.2920(5) -0.15127(16) 0.0239(12) Uani 1 1 d . . . N2 N -0.8253(7) -0.0883(5) -0.17435(17) 0.0247(12) Uani 1 1 d . . . N3 N -0.8567(7) -0.0338(5) -0.07532(16) 0.0249(12) Uani 1 1 d . . . C1 C -0.3728(12) -0.3859(6) -0.2160(2) 0.0392(18) Uani 1 1 d . . . H1A H -0.4207 -0.4696 -0.2079 0.059 Uiso 1 1 calc R . . H1B H -0.2324 -0.3732 -0.2041 0.059 Uiso 1 1 calc R . . H1C H -0.3717 -0.3769 -0.2493 0.059 Uiso 1 1 calc R . . C2 C -0.5173(9) -0.2900(6) -0.1955(2) 0.0290(15) Uani 1 1 d . . . C3 C -0.6049(11) -0.2031(6) -0.2256(2) 0.0345(17) Uani 1 1 d . . . H3A H -0.5540 -0.2046 -0.2560 0.041 Uiso 1 1 calc R . . C4 C -0.7579(10) -0.1146(6) -0.2163(2) 0.0292(16) Uani 1 1 d . . . C5 C -0.8497(11) -0.0472(6) -0.2564(2) 0.0370(17) Uani 1 1 d . . . H5A H -0.8325 0.0428 -0.2522 0.055 Uiso 1 1 calc R . . H5B H -0.9976 -0.0671 -0.2587 0.055 Uiso 1 1 calc R . . H5C H -0.7790 -0.0732 -0.2844 0.055 Uiso 1 1 calc R . . C6 C -0.4939(10) -0.3984(6) -0.1252(2) 0.0310(16) Uani 1 1 d . . . C7 C -0.6446(12) -0.4843(6) -0.1139(2) 0.0404(18) Uani 1 1 d . . . H7A H -0.7814 -0.4737 -0.1252 0.048 Uiso 1 1 calc R . . C8 C -0.6004(15) -0.5855(7) -0.0863(3) 0.057(2) Uani 1 1 d . . . H8A H -0.7064 -0.6431 -0.0784 0.069 Uiso 1 1 calc R . . C9 C -0.4013(18) -0.6023(8) -0.0703(2) 0.065(3) Uani 1 1 d . . . H9A H -0.3694 -0.6711 -0.0512 0.078 Uiso 1 1 calc R . . C10 C -0.2484(15) -0.5182(9) -0.0823(3) 0.056(2) Uani 1 1 d . . . H10A H -0.1109 -0.5305 -0.0716 0.067 Uiso 1 1 calc R . . C11 C -0.2929(11) -0.4153(7) -0.1099(2) 0.0401(18) Uani 1 1 d . . . H11A H -0.1870 -0.3580 -0.1180 0.048 Uiso 1 1 calc R . . C12 C -0.9828(10) 0.0061(6) -0.1693(2) 0.0261(15) Uani 1 1 d . . . C13 C -1.1889(9) -0.0288(7) -0.1650(2) 0.0296(15) Uani 1 1 d . . . H13A H -1.2272 -0.1142 -0.1662 0.035 Uiso 1 1 calc R . . C14 C -1.3384(10) 0.0625(7) -0.1587(2) 0.0375(18) Uani 1 1 d . . . H14A H -1.4800 0.0390 -0.1564 0.045 Uiso 1 1 calc R . . C15 C -1.2858(10) 0.1865(7) -0.1558(2) 0.0360(17) Uani 1 1 d . . . H15A H -1.3894 0.2483 -0.1514 0.043 Uiso 1 1 calc R . . C16 C -1.0805(10) 0.2194(7) -0.1594(2) 0.0398(18) Uani 1 1 d . . . H16A H -1.0425 0.3046 -0.1570 0.048 Uiso 1 1 calc R . . C17 C -0.9299(10) 0.1319(6) -0.1665(2) 0.0321(16) Uani 1 1 d . . . H17A H -0.7892 0.1567 -0.1694 0.039 Uiso 1 1 calc R . . C18 C -1.0504(9) -0.0537(6) -0.0603(2) 0.0278(15) Uani 1 1 d . . . H18A H -1.1249 -0.1227 -0.0722 0.033 Uiso 1 1 calc R . . C19 C -1.1466(11) 0.0205(7) -0.0285(2) 0.0358(17) Uani 1 1 d . . . H19A H -1.2846 0.0033 -0.0191 0.043 Uiso 1 1 calc R . . C20 C -1.0411(11) 0.1191(7) -0.0105(2) 0.0373(18) Uani 1 1 d . . . H20A H -1.1036 0.1713 0.0118 0.045 Uiso 1 1 calc R . . C21 C -0.8407(12) 0.1416(6) -0.0255(2) 0.0357(17) Uani 1 1 d . . . H21A H -0.7637 0.2098 -0.0137 0.043 Uiso 1 1 calc R . . C22 C -0.7551(10) 0.0646(6) -0.0576(2) 0.0304(16) Uani 1 1 d . . . H22A H -0.6180 0.0812 -0.0678 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0217(2) 0.0221(2) 0.0234(2) -0.0010(3) 0.00165(18) 0.0013(4) Cl1 0.0323(8) 0.0332(8) 0.0264(8) -0.0014(7) -0.0001(7) 0.0048(7) N1 0.031(3) 0.022(3) 0.019(3) 0.003(2) -0.002(2) 0.003(2) N2 0.021(3) 0.022(3) 0.031(3) 0.006(2) -0.004(2) 0.002(2) N3 0.026(3) 0.025(3) 0.024(3) -0.003(2) -0.003(2) 0.004(3) C1 0.059(5) 0.034(4) 0.025(4) 0.001(3) 0.002(4) 0.016(4) C2 0.027(3) 0.027(4) 0.033(4) -0.003(3) -0.002(3) -0.004(3) C3 0.045(4) 0.038(5) 0.020(3) -0.004(3) -0.001(3) 0.012(4) C4 0.040(4) 0.030(4) 0.017(3) 0.004(3) -0.004(3) -0.008(3) C5 0.045(4) 0.038(4) 0.028(4) 0.002(3) -0.003(3) 0.010(4) C6 0.036(4) 0.026(4) 0.031(4) -0.004(3) 0.004(3) 0.004(3) C7 0.053(5) 0.030(4) 0.039(4) -0.001(4) 0.006(4) 0.005(4) C8 0.089(7) 0.041(5) 0.042(5) 0.005(4) 0.018(5) 0.018(5) C9 0.127(9) 0.046(5) 0.021(4) 0.015(4) 0.013(5) 0.040(6) C10 0.081(6) 0.058(6) 0.028(4) -0.015(4) -0.008(4) 0.040(5) C11 0.046(4) 0.042(4) 0.032(4) -0.003(3) -0.003(4) 0.013(4) C12 0.029(4) 0.028(4) 0.021(3) -0.001(3) 0.002(3) 0.000(3) C13 0.024(4) 0.035(4) 0.030(4) 0.009(3) -0.005(3) -0.007(3) C14 0.026(4) 0.053(5) 0.033(4) 0.012(4) 0.000(3) 0.003(4) C15 0.030(4) 0.048(5) 0.031(4) 0.000(4) 0.001(3) 0.012(4) C16 0.034(4) 0.037(4) 0.049(5) 0.001(4) -0.009(3) 0.006(4) C17 0.025(4) 0.025(4) 0.046(4) 0.000(3) -0.001(3) -0.002(3) C18 0.023(3) 0.034(4) 0.026(4) 0.004(3) -0.003(3) -0.005(3) C19 0.031(4) 0.041(4) 0.035(4) -0.005(3) 0.008(3) 0.003(4) C20 0.039(5) 0.038(5) 0.035(5) -0.009(3) 0.001(3) 0.017(4) C21 0.053(5) 0.024(4) 0.031(4) -0.003(3) -0.009(3) 0.005(3) C22 0.034(4) 0.023(4) 0.034(4) 0.005(3) 0.005(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.009(5) . ? Pd1 N2 2.023(5) . ? Pd1 N3 2.045(5) . ? Pd1 Cl1 2.3258(16) . ? N1 C2 1.317(7) . ? N1 C6 1.430(8) . ? N2 C4 1.334(8) . ? N2 C12 1.443(8) . ? N3 C18 1.342(7) . ? N3 C22 1.348(8) . ? C1 C2 1.513(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.403(9) . ? C3 C4 1.396(9) . ? C3 H3A 0.9500 . ? C4 C5 1.499(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.381(10) . ? C6 C11 1.384(9) . ? C7 C8 1.383(10) . ? C7 H7A 0.9500 . ? C8 C9 1.379(12) . ? C8 H8A 0.9500 . ? C9 C10 1.382(13) . ? C9 H9A 0.9500 . ? C10 C11 1.398(11) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.388(9) . ? C12 C17 1.395(9) . ? C13 C14 1.387(10) . ? C13 H13A 0.9500 . ? C14 C15 1.377(10) . ? C14 H14A 0.9500 . ? C15 C16 1.375(9) . ? C15 H15A 0.9500 . ? C16 C17 1.367(9) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.373(9) . ? C18 H18A 0.9500 . ? C19 C20 1.365(10) . ? C19 H19A 0.9500 . ? C20 C21 1.387(9) . ? C20 H20A 0.9500 . ? C21 C22 1.367(9) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 91.0(2) . . ? N1 Pd1 N3 175.3(2) . . ? N2 Pd1 N3 93.5(2) . . ? N1 Pd1 Cl1 92.56(14) . . ? N2 Pd1 Cl1 172.78(15) . . ? N3 Pd1 Cl1 83.03(14) . . ? C2 N1 C6 119.1(5) . . ? C2 N1 Pd1 125.8(4) . . ? C6 N1 Pd1 115.0(4) . . ? C4 N2 C12 118.2(5) . . ? C4 N2 Pd1 125.1(4) . . ? C12 N2 Pd1 116.5(4) . . ? C18 N3 C22 116.8(5) . . ? C18 N3 Pd1 121.6(4) . . ? C22 N3 Pd1 121.0(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 123.6(6) . . ? N1 C2 C1 119.6(6) . . ? C3 C2 C1 116.8(6) . . ? C4 C3 C2 128.0(6) . . ? C4 C3 H3A 116.0 . . ? C2 C3 H3A 116.0 . . ? N2 C4 C3 123.6(6) . . ? N2 C4 C5 119.3(6) . . ? C3 C4 C5 117.1(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.6(7) . . ? C7 C6 N1 117.9(6) . . ? C11 C6 N1 122.5(6) . . ? C6 C7 C8 121.3(8) . . ? C6 C7 H7A 119.3 . . ? C8 C7 H7A 119.3 . . ? C9 C8 C7 119.5(8) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 119.6(7) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 121.1(8) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C6 C11 C10 118.9(8) . . ? C6 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C13 C12 C17 119.4(6) . . ? C13 C12 N2 119.6(6) . . ? C17 C12 N2 120.9(6) . . ? C14 C13 C12 119.2(7) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C16 C15 C14 118.7(7) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C17 C16 C15 121.4(7) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C16 C17 C12 120.0(6) . . ? C16 C17 H17A 120.0 . . ? C12 C17 H17A 120.0 . . ? N3 C18 C19 123.5(6) . . ? N3 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? C20 C19 C18 119.1(7) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C21 118.5(6) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C22 C21 C20 119.3(6) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? N3 C22 C21 122.8(6) . . ? N3 C22 H22A 118.6 . . ? C21 C22 H22A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.170 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.090 # Attachment 'complex3.txt' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 779765' #TrackingRef 'complex3.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 N3 Pd' _chemical_formula_weight 449.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1137(6) _cell_length_b 23.4596(15) _cell_length_c 11.9041(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.157(2) _cell_angle_gamma 90.00 _cell_volume 3072.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12476 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.52 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6347 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker Apex 2 Software Package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12476 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3530 _reflns_number_gt 2354 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+4.3722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3530 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.07189(6) 0.35139(3) 0.28591(5) 0.02105(18) Uani 0.34 1 d P . 1 N1A N 0.0928(7) 0.3606(3) 0.1195(6) 0.0227(16) Uani 0.34 1 d P . 1 N2A N 0.2002(6) 0.4175(3) 0.3328(6) 0.0239(16) Uani 0.34 1 d P . 1 N3A N 0.0492(8) 0.3363(3) 0.4505(7) 0.0217(17) Uani 0.34 1 d P . 1 C1A C 0.1649(8) 0.4025(4) -0.0480(7) 0.030(2) Uani 0.34 1 d P . 1 H1AA H 0.1081 0.3760 -0.0874 0.046 Uiso 0.34 1 d PR . 1 H1AB H 0.1409 0.4407 -0.0700 0.046 Uiso 0.34 1 d PR . 1 H1AC H 0.2446 0.3952 -0.0670 0.046 Uiso 0.34 1 d PR . 1 C2A C 0.1663(7) 0.3973(4) 0.0792(7) 0.0238(19) Uani 0.34 1 d P . 1 C3A C 0.2473(7) 0.4335(4) 0.1453(7) 0.0246(19) Uani 0.34 1 d P . 1 H3AA H 0.2976 0.4556 0.1039 0.030 Uiso 0.34 1 calc PR . 1 C4A C 0.2667(9) 0.4425(4) 0.2656(8) 0.0229(19) Uani 0.34 1 d P . 1 C5A C 0.3648(8) 0.4846(4) 0.3081(8) 0.031(2) Uani 0.34 1 d P . 1 H5AA H 0.3319 0.5133 0.3552 0.047 Uiso 0.34 1 calc PR . 1 H5AB H 0.3939 0.5033 0.2434 0.047 Uiso 0.34 1 calc PR . 1 H5AC H 0.4324 0.4646 0.3534 0.047 Uiso 0.34 1 calc PR . 1 C6A C 0.0240(9) 0.3240(5) 0.0364(7) 0.024(2) Uani 0.34 1 d P . 1 C7A C 0.0675(8) 0.2714(4) 0.0127(7) 0.029(2) Uani 0.34 1 d P A 1 H7AA H 0.1450 0.2597 0.0495 0.034 Uiso 0.34 1 calc PR A 1 C8A C 0.0006(10) 0.2349(4) -0.0641(8) 0.032(2) Uani 0.34 1 d P . 1 H8AA H 0.0330 0.1988 -0.0801 0.039 Uiso 0.34 1 calc PR . 1 C9A C -0.1132(10) 0.2510(6) -0.1175(7) 0.027(2) Uani 0.34 1 d P . 1 H9AA H -0.1592 0.2259 -0.1711 0.033 Uiso 0.34 1 d PR . 1 C10A C -0.1586(10) 0.3042(5) -0.0921(9) 0.035(2) Uani 0.34 1 d P . 1 H10A H -0.2370 0.3163 -0.1288 0.042 Uiso 0.34 1 d PR . 1 C11A C -0.0895(10) 0.3407(5) -0.0143(10) 0.029(2) Uani 0.34 1 d P . 1 H11A H -0.1215 0.3768 0.0052 0.035 Uiso 0.34 1 d PR . 1 C12A C 0.2165(10) 0.4349(4) 0.4514(8) 0.030(2) Uani 0.34 1 d P . 1 C13A C 0.1513(8) 0.4805(4) 0.4835(7) 0.031(2) Uani 0.34 1 d P . 1 H13A H 0.0999 0.5007 0.4252 0.037 Uiso 0.34 1 d PR . 1 C14A C 0.1597(10) 0.4959(5) 0.5969(9) 0.048(3) Uani 0.34 1 d P . 1 H14A H 0.1156 0.5284 0.6185 0.057 Uiso 0.34 1 d PR . 1 C15A C 0.2328(11) 0.4628(5) 0.6781(10) 0.043(3) Uiso 0.34 1 d P . 1 H15A H 0.2354 0.4711 0.7573 0.051 Uiso 0.34 1 d PR . 1 C16A C 0.3017(10) 0.4207(5) 0.6464(10) 0.047(3) Uiso 0.34 1 d P . 1 H16A H 0.3554 0.4001 0.7026 0.056 Uiso 0.34 1 d PR . 1 C17A C 0.2920(11) 0.4060(5) 0.5312(10) 0.042(3) Uani 0.34 1 d P . 1 H17A H 0.3412 0.3760 0.5068 0.050 Uiso 0.34 1 d PR . 1 C18A C -0.0206(8) 0.3694(5) 0.5076(8) 0.032(2) Uani 0.34 1 d P . 1 H18A H -0.0641 0.4002 0.4673 0.039 Uiso 0.34 1 d PR . 1 C19A C -0.0297(9) 0.3607(5) 0.6221(8) 0.039(3) Uani 0.34 1 d P . 1 H19A H -0.0827 0.3843 0.6590 0.046 Uiso 0.34 1 d PR . 1 C20A C 0.0366(8) 0.3169(5) 0.6786(8) 0.037(3) Uani 0.34 1 d P . 1 H20A H 0.0320 0.3105 0.7575 0.044 Uiso 0.34 1 d PR . 1 C21A C 0.1099(11) 0.2828(6) 0.6221(9) 0.030(3) Uiso 0.34 1 d P . 1 H21A H 0.1585 0.2529 0.6603 0.035 Uiso 0.34 1 d PR . 1 C22A C 0.1141(8) 0.2944(4) 0.5094(8) 0.026(2) Uani 0.34 1 d P . 1 H22A H 0.1631 0.2707 0.4683 0.031 Uiso 0.34 1 d PR . 1 C23A C -0.0522(14) 0.2863(8) 0.2495(13) 0.026(3) Uani 0.34 1 d P . 1 H23A H -0.0609 0.2776 0.1699 0.039 Uiso 0.34 1 d PR . 1 H23B H -0.0252 0.2530 0.2926 0.039 Uiso 0.34 1 d PR . 1 H23C H -0.1291 0.2984 0.2690 0.039 Uiso 0.34 1 d PR . 1 Pd2 Pd 0.23556(6) 0.49023(3) 0.54974(5) 0.02063(18) Uani 0.33 1 d P . 2 N1B N 0.2642(6) 0.5018(3) 0.3860(5) 0.0238(16) Uani 0.33 1 d P . 2 N2B N 0.3386(6) 0.5642(3) 0.6004(5) 0.0215(15) Uani 0.33 1 d P . 2 N3B N 0.2000(6) 0.4785(3) 0.7101(6) 0.0203(16) Uiso 0.33 1 d P . 2 C1B C 0.3070(8) 0.5554(4) 0.2181(8) 0.0256(19) Uiso 0.33 1 d P . 2 H1BA H 0.2774 0.5211 0.1796 0.038 Uiso 0.33 1 d PR . 2 H1BB H 0.2582 0.5871 0.1878 0.038 Uiso 0.33 1 d PR . 2 H1BC H 0.3899 0.5616 0.2072 0.038 Uiso 0.33 1 d PR . 2 C2B C 0.3032(9) 0.5508(5) 0.3458(10) 0.025(2) Uani 0.33 1 d P . 2 C3B C 0.3434(8) 0.5983(4) 0.4109(7) 0.029(2) Uani 0.33 1 d P . 2 H3BA H 0.3590 0.6320 0.3696 0.035 Uiso 0.33 1 d PR . 2 C4B C 0.3647(8) 0.6042(4) 0.5301(7) 0.0266(19) Uani 0.33 1 d P . 2 C5B C 0.4249(9) 0.6591(4) 0.5759(8) 0.039(2) Uani 0.33 1 d P . 2 H5BA H 0.4972 0.6501 0.6301 0.059 Uiso 0.33 1 calc PR . 2 H5BB H 0.3677 0.6812 0.6140 0.059 Uiso 0.33 1 calc PR . 2 H5BC H 0.4487 0.6814 0.5130 0.059 Uiso 0.33 1 calc PR . 2 C6B C 0.2392(9) 0.4562(5) 0.3064(8) 0.024(2) Uiso 0.33 1 d P . 2 C7B C 0.3393(12) 0.4215(5) 0.2870(9) 0.026(3) Uani 0.33 1 d P . 2 H7BA H 0.4202 0.4292 0.3239 0.031 Uiso 0.33 1 d PR . 2 C8B C 0.3194(12) 0.3758(5) 0.2148(9) 0.044(3) Uani 0.33 1 d P . 2 H8BA H 0.3871 0.3528 0.2008 0.053 Uiso 0.33 1 d PR . 2 C9B C 0.2047(15) 0.3620(5) 0.1621(9) 0.054(4) Uani 0.33 1 d P . 2 H9BA H 0.1926 0.3300 0.1117 0.065 Uiso 0.33 1 d PR . 2 C10B C 0.1081(11) 0.3952(5) 0.1825(8) 0.045(3) Uani 0.33 1 d P . 2 H10B H 0.0277 0.3848 0.1483 0.054 Uiso 0.33 1 d PR . 2 C11B C 0.1249(8) 0.4428(5) 0.2538(7) 0.034(2) Uani 0.33 1 d P . 2 H11B H 0.0567 0.4663 0.2642 0.041 Uiso 0.33 1 d PR . 2 C12B C 0.3800(6) 0.5699(3) 0.7197(4) 0.0234(19) Uani 0.33 1 d PG . 2 C13B C 0.3167(5) 0.6032(3) 0.7881(5) 0.031(4) Uani 0.33 1 d PG . 2 H13B H 0.2462 0.6242 0.7551 0.037 Uiso 0.33 1 d PR . 2 C14B C 0.3554(6) 0.6062(3) 0.9042(5) 0.033(2) Uani 0.33 1 d PG . 2 H14C H 0.3116 0.6293 0.9514 0.040 Uiso 0.33 1 d PR . 2 C15B C 0.4574(6) 0.5759(3) 0.9519(3) 0.035(2) Uani 0.33 1 d PG . 2 H15B H 0.4842 0.5780 1.0321 0.042 Uiso 0.33 1 d PR . 2 C16B C 0.5208(5) 0.5426(3) 0.8835(5) 0.035(2) Uani 0.33 1 d PG . 2 H16B H 0.5913 0.5217 0.9165 0.042 Uiso 0.33 1 d PR . 2 C17B C 0.4821(6) 0.5396(3) 0.7674(4) 0.035(3) Uani 0.33 1 d PG . 2 H17B H 0.5258 0.5166 0.7202 0.042 Uiso 0.33 1 d PR . 2 C18B C 0.2686(10) 0.4420(5) 0.7833(10) 0.033(2) Uani 0.33 1 d P . 2 H18B H 0.3294 0.4195 0.7542 0.040 Uiso 0.33 1 d PR . 2 C19B C 0.2500(11) 0.4353(5) 0.8944(9) 0.041(3) Uani 0.33 1 d P . 2 H19B H 0.3016 0.4104 0.9439 0.050 Uiso 0.33 1 d PR . 2 C20B C 0.1590(11) 0.4671(5) 0.9339(8) 0.044(3) Uani 0.33 1 d P . 2 H20B H 0.1430 0.4623 1.0105 0.053 Uiso 0.33 1 d PR . 2 C21B C 0.0877(9) 0.5021(4) 0.8602(8) 0.036(2) Uani 0.33 1 d P . 2 H21B H 0.0249 0.5240 0.8875 0.043 Uiso 0.33 1 d PR . 2 C22B C 0.1117(8) 0.5075(4) 0.7521(8) 0.029(2) Uani 0.33 1 d P . 2 H22B H 0.0617 0.5330 0.7025 0.035 Uiso 0.33 1 d PR . 2 C23B C 0.1283(7) 0.4171(4) 0.5132(6) 0.0167(17) Uani 0.33 1 d P . 2 H23D H 0.1678 0.3915 0.4646 0.025 Uiso 0.33 1 calc PR . 2 H23E H 0.0482 0.4281 0.4740 0.025 Uiso 0.33 1 calc PR . 2 H23F H 0.1188 0.3974 0.5841 0.025 Uiso 0.33 1 calc PR . 2 Pd3 Pd 0.07019(6) 0.26793(3) 0.44874(5) 0.01917(17) Uani 0.33 1 d P . 3 N1C N 0.0900(9) 0.2798(6) 0.2812(9) 0.016(2) Uani 0.33 1 d P . 3 N2C N 0.1869(6) 0.3376(3) 0.4969(5) 0.0198(15) Uani 0.33 1 d P . 3 N3C N 0.0382(10) 0.2558(4) 0.6122(8) 0.0196(17) Uiso 0.33 1 d P . 3 C1C C 0.1524(9) 0.3259(5) 0.1153(7) 0.027(2) Uani 0.33 1 d P . 3 H1CA H 0.0686 0.3276 0.0765 0.041 Uiso 0.33 1 calc PR . 3 H1CB H 0.1933 0.2925 0.0886 0.041 Uiso 0.33 1 calc PR . 3 H1CC H 0.1958 0.3606 0.0988 0.041 Uiso 0.33 1 calc PR . 3 C2C C 0.1516(8) 0.3211(4) 0.2438(7) 0.0236(19) Uani 0.33 1 d P . 3 C3C C 0.2161(9) 0.3644(4) 0.3069(7) 0.032(2) Uani 0.33 1 d P . 3 H3CA H 0.2541 0.3917 0.2632 0.038 Uiso 0.33 1 d PR . 3 C4C C 0.2330(8) 0.3729(4) 0.4249(7) 0.0232(19) Uani 0.33 1 d P . 3 C5C C 0.3056(11) 0.4243(5) 0.4687(9) 0.035(3) Uani 0.33 1 d P . 3 H5CA H 0.3701 0.4128 0.5293 0.053 Uiso 0.33 1 calc PR . 3 H5CB H 0.2521 0.4519 0.4987 0.053 Uiso 0.33 1 calc PR . 3 H5CC H 0.3420 0.4418 0.4067 0.053 Uiso 0.33 1 calc PR . 3 C6C C 0.0292(8) 0.2391(4) 0.2008(6) 0.026(2) Uani 0.33 1 d P . 3 C7C C -0.0917(7) 0.2440(4) 0.1607(7) 0.0228(19) Uani 0.33 1 d P . 3 H7CA H -0.1365 0.2763 0.1818 0.027 Uiso 0.33 1 d PR . 3 C8C C -0.1493(8) 0.2030(4) 0.0884(7) 0.028(2) Uani 0.33 1 d P . 3 H8CA H -0.2347 0.2063 0.0618 0.034 Uiso 0.33 1 d PR . 3 C9C C -0.0842(9) 0.1563(4) 0.0564(7) 0.031(2) Uani 0.33 1 d P . 3 H9CA H -0.1246 0.1274 0.0078 0.037 Uiso 0.33 1 d PR . 3 C10C C 0.0371(8) 0.1522(5) 0.0937(8) 0.031(2) Uani 0.33 1 d P . 3 H10C H 0.0833 0.1208 0.0707 0.038 Uiso 0.33 1 d PR . 3 C11C C 0.0946(8) 0.1931(4) 0.1652(7) 0.0255(19) Uani 0.33 1 d P . 3 H11C H 0.1800 0.1897 0.1921 0.031 Uiso 0.33 1 d PR . 3 C12C C 0.2152(8) 0.3510(4) 0.6157(6) 0.0214(18) Uani 0.33 1 d P . 3 C13C C 0.1305(8) 0.3774(4) 0.6731(8) 0.031(2) Uani 0.33 1 d P . 3 H13C H 0.0556 0.3906 0.6309 0.037 Uiso 0.33 1 d PR . 3 C14C C 0.1562(10) 0.3873(5) 0.7890(8) 0.043(3) Uani 0.33 1 d P . 3 H14D H 0.0969 0.4051 0.8288 0.052 Uiso 0.33 1 d PR . 3 C15C C 0.2644(10) 0.3705(5) 0.8470(8) 0.039(3) Uani 0.33 1 d P . 3 H15C H 0.2818 0.3759 0.9276 0.046 Uiso 0.33 1 d PR . 3 C16C C 0.3526(10) 0.3459(4) 0.7921(8) 0.036(2) Uani 0.33 1 d P . 3 H16C H 0.4309 0.3358 0.8320 0.043 Uiso 0.33 1 d PR . 3 C17C C 0.3261(8) 0.3349(4) 0.6759(7) 0.028(2) Uani 0.33 1 d P . 3 H17C H 0.3854 0.3169 0.6365 0.034 Uiso 0.33 1 d PR . 3 C18C C -0.0626(9) 0.2790(5) 0.6453(8) 0.034(2) Uani 0.33 1 d P . 3 H18C H -0.1203 0.2979 0.5900 0.041 Uiso 0.33 1 d PR . 3 C19C C -0.0874(9) 0.2756(5) 0.7548(8) 0.038(2) Uani 0.33 1 d P . 3 H19C H -0.1595 0.2931 0.7750 0.045 Uiso 0.33 1 d PR . 3 C20C C -0.0059(10) 0.2482(5) 0.8370(9) 0.037(3) Uani 0.33 1 d P . 3 H20C H -0.0202 0.2471 0.9147 0.044 Uiso 0.33 1 d PR . 3 C21C C 0.0963(9) 0.2227(5) 0.8016(8) 0.037(2) Uani 0.33 1 d P . 3 H21C H 0.1531 0.2016 0.8540 0.045 Uiso 0.33 1 d PR . 3 C22C C 0.1144(8) 0.2281(4) 0.6911(7) 0.027(2) Uani 0.33 1 d P . 3 H22C H 0.1870 0.2126 0.6679 0.032 Uiso 0.33 1 d PR . 3 C23C C -0.0518(8) 0.2007(4) 0.4130(7) 0.026(2) Uani 0.33 1 d P . 3 H23G H -0.0279 0.1778 0.3532 0.039 Uiso 0.33 1 d PR . 3 H23H H -0.0524 0.1777 0.4797 0.039 Uiso 0.33 1 d PR . 3 H23I H -0.1317 0.2158 0.3896 0.039 Uiso 0.33 1 d PR . 3 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 0.0227(3) 0.0233(4) 0.0176(3) 0.0003(3) 0.0044(2) -0.0008(3) N1A 0.023(4) 0.025(5) 0.020(4) 0.000(3) 0.001(3) 0.000(4) N2A 0.028(4) 0.024(5) 0.021(4) -0.004(3) 0.005(3) -0.007(3) N3A 0.025(5) 0.021(5) 0.018(4) -0.005(3) 0.001(4) -0.001(4) C1A 0.036(5) 0.036(6) 0.022(4) -0.004(4) 0.011(4) -0.011(4) C2A 0.020(4) 0.032(6) 0.020(4) 0.001(4) 0.004(3) 0.003(4) C3A 0.025(5) 0.025(5) 0.025(4) 0.000(4) 0.007(4) 0.001(4) C4A 0.020(5) 0.013(5) 0.038(5) -0.001(4) 0.013(4) 0.006(4) C5A 0.037(5) 0.027(6) 0.031(5) -0.002(4) 0.011(4) -0.003(4) C6A 0.021(5) 0.041(7) 0.012(4) -0.006(4) 0.005(4) 0.009(5) C7A 0.025(5) 0.037(6) 0.022(4) -0.003(4) -0.003(4) 0.002(4) C8A 0.047(6) 0.018(5) 0.030(5) -0.004(4) 0.000(5) -0.002(5) C9A 0.026(6) 0.038(7) 0.015(5) 0.011(5) -0.004(4) -0.010(5) C10A 0.033(6) 0.039(7) 0.031(6) 0.002(5) -0.002(5) -0.001(5) C11A 0.025(6) 0.030(7) 0.034(6) 0.002(5) 0.014(5) 0.006(5) C12A 0.036(6) 0.024(6) 0.027(5) 0.001(4) 0.000(4) -0.015(5) C13A 0.029(5) 0.039(7) 0.023(4) -0.006(4) -0.006(4) -0.001(4) C14A 0.037(6) 0.063(9) 0.046(6) -0.017(6) 0.015(5) -0.012(6) C17A 0.048(7) 0.024(6) 0.049(7) 0.000(5) -0.009(6) 0.001(5) C18A 0.032(5) 0.037(6) 0.029(5) 0.002(4) 0.008(4) 0.015(5) C19A 0.028(5) 0.054(8) 0.036(5) 0.001(5) 0.015(4) 0.006(5) C20A 0.031(5) 0.056(8) 0.025(5) 0.005(5) 0.008(4) -0.016(5) C22A 0.029(5) 0.023(6) 0.029(6) 0.001(4) 0.012(4) -0.006(4) C23A 0.013(7) 0.038(8) 0.024(8) 0.011(6) -0.006(5) -0.002(5) Pd2 0.0227(4) 0.0228(4) 0.0169(3) 0.0020(3) 0.0044(3) -0.0006(3) N1B 0.024(4) 0.032(5) 0.017(3) 0.005(3) 0.008(3) 0.005(3) N2B 0.023(4) 0.022(4) 0.019(3) 0.000(3) 0.001(3) -0.002(3) C2B 0.029(6) 0.028(6) 0.021(5) 0.003(5) 0.008(5) 0.006(4) C3B 0.035(5) 0.030(6) 0.025(4) 0.006(4) 0.010(4) 0.005(4) C4B 0.024(5) 0.021(5) 0.034(5) 0.000(4) 0.002(4) -0.003(4) C5B 0.049(6) 0.029(6) 0.041(6) -0.001(5) 0.011(5) -0.010(5) C7B 0.038(7) 0.022(7) 0.019(5) 0.006(5) 0.009(5) 0.010(6) C8B 0.081(9) 0.032(7) 0.023(5) 0.006(5) 0.019(6) 0.013(6) C9B 0.113(12) 0.031(7) 0.022(5) 0.002(5) 0.024(7) -0.016(7) C10B 0.064(8) 0.052(8) 0.020(5) -0.003(5) 0.007(5) -0.031(6) C11B 0.025(5) 0.057(8) 0.021(4) 0.004(5) 0.007(4) -0.006(5) C12B 0.026(5) 0.022(5) 0.022(4) -0.004(4) 0.005(4) -0.011(4) C13B 0.025(6) 0.030(8) 0.035(7) -0.020(7) -0.004(4) 0.005(5) C14B 0.034(5) 0.036(6) 0.033(5) -0.018(4) 0.014(4) -0.003(5) C15B 0.043(6) 0.041(6) 0.024(4) -0.004(4) 0.010(4) -0.010(5) C16B 0.034(5) 0.043(7) 0.026(5) 0.002(4) 0.000(4) 0.002(5) C17B 0.038(7) 0.039(6) 0.027(7) -0.007(5) -0.001(5) 0.008(5) C18B 0.043(7) 0.028(6) 0.029(6) 0.012(5) 0.005(5) 0.013(5) C19B 0.050(7) 0.038(7) 0.034(6) 0.023(5) -0.002(5) 0.014(5) C20B 0.076(8) 0.038(7) 0.023(5) 0.001(5) 0.018(5) -0.022(6) C21B 0.050(6) 0.029(6) 0.034(5) -0.006(4) 0.023(5) -0.001(5) C22B 0.028(5) 0.028(6) 0.030(5) -0.003(4) 0.004(4) -0.006(4) C23B 0.020(4) 0.023(5) 0.008(3) -0.004(3) 0.004(3) -0.005(3) Pd3 0.0225(3) 0.0221(4) 0.0134(3) 0.0009(3) 0.0041(2) -0.0001(3) N1C 0.013(7) 0.027(6) 0.010(6) 0.001(4) 0.006(4) -0.004(5) N2C 0.029(4) 0.018(4) 0.012(3) 0.000(3) 0.000(3) 0.002(3) C1C 0.034(5) 0.035(6) 0.013(4) 0.001(4) 0.006(4) -0.003(5) C2C 0.021(4) 0.031(6) 0.018(4) 0.006(4) 0.001(3) 0.003(4) C3C 0.042(6) 0.035(6) 0.019(4) 0.006(4) 0.007(4) -0.001(5) C4C 0.025(4) 0.025(5) 0.020(4) 0.008(4) 0.002(3) 0.004(4) C5C 0.046(7) 0.037(7) 0.021(5) 0.000(5) 0.002(5) -0.023(6) C6C 0.037(5) 0.027(6) 0.012(4) 0.007(4) 0.001(3) -0.008(4) C7C 0.023(5) 0.032(6) 0.015(4) 0.003(4) 0.009(3) 0.007(4) C8C 0.023(5) 0.046(7) 0.017(4) -0.004(4) 0.005(3) 0.001(4) C9C 0.045(6) 0.029(6) 0.019(4) -0.006(4) 0.010(4) -0.013(5) C10C 0.032(5) 0.031(6) 0.031(5) -0.005(4) 0.007(4) 0.005(4) C11C 0.023(5) 0.027(6) 0.027(5) -0.001(4) 0.002(4) 0.005(4) C12C 0.030(5) 0.019(5) 0.016(4) -0.005(3) 0.004(3) 0.000(4) C13C 0.030(5) 0.025(6) 0.038(5) -0.006(4) 0.009(4) 0.006(4) C14C 0.047(7) 0.049(7) 0.038(5) -0.017(5) 0.025(5) -0.010(5) C15C 0.055(7) 0.041(7) 0.021(4) -0.014(4) 0.012(4) -0.021(5) C16C 0.048(6) 0.030(6) 0.027(5) 0.005(4) -0.001(4) 0.002(5) C17C 0.030(5) 0.026(5) 0.028(5) 0.002(4) 0.004(4) 0.000(4) C18C 0.038(6) 0.041(7) 0.025(5) -0.001(4) 0.013(4) 0.010(5) C19C 0.042(6) 0.046(7) 0.030(5) -0.002(5) 0.019(4) 0.000(5) C20C 0.046(7) 0.042(7) 0.025(5) 0.001(5) 0.015(5) -0.010(6) C21C 0.034(6) 0.047(7) 0.028(5) 0.004(5) -0.004(4) -0.014(5) C22C 0.019(5) 0.039(6) 0.021(5) 0.002(4) 0.002(4) -0.004(4) C23C 0.041(6) 0.029(6) 0.008(4) -0.003(4) 0.001(4) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1A 2.039(7) . ? Pd1 N3A 2.042(8) . ? Pd1 C23A 2.061(14) . ? Pd1 N2A 2.127(7) . ? N1A C2A 1.323(11) . ? N1A C6A 1.443(12) . ? N2A C4A 1.303(11) . ? N2A C12A 1.455(11) . ? N3A C18A 1.347(12) . ? N3A C22A 1.353(12) . ? C1A C2A 1.518(11) . ? C2A C3A 1.396(12) . ? C3A C4A 1.434(12) . ? C4A C5A 1.504(13) . ? C6A C7A 1.370(14) . ? C6A C11A 1.375(14) . ? C7A C8A 1.389(12) . ? C8A C9A 1.384(15) . ? C9A C10A 1.397(16) . ? C10A C11A 1.406(15) . ? C12A C17A 1.356(15) . ? C12A C13A 1.376(14) . ? C13A C14A 1.388(13) . ? C14A C15A 1.405(16) . ? C15A C16A 1.337(16) . ? C16A C17A 1.404(15) . ? C18A C19A 1.395(12) . ? C19A C20A 1.383(14) . ? C20A C21A 1.383(15) . ? C21A C22A 1.377(14) . ? Pd2 N3B 2.023(7) . ? Pd2 N1B 2.037(6) . ? Pd2 C23B 2.099(8) . ? Pd2 N2B 2.118(7) . ? N1B C2B 1.340(12) . ? N1B C6B 1.430(12) . ? N2B C4B 1.318(11) . ? N2B C12B 1.436(7) . ? N3B C22B 1.347(11) . ? N3B C18B 1.373(12) . ? C1B C2B 1.532(12) . ? C2B C3B 1.394(15) . ? C3B C4B 1.411(12) . ? C4B C5B 1.517(13) . ? C6B C11B 1.371(13) . ? C6B C7B 1.423(15) . ? C7B C8B 1.372(15) . ? C8B C9B 1.377(17) . ? C9B C10B 1.375(18) . ? C10B C11B 1.399(15) . ? C12B C13B 1.3900 . ? C12B C17B 1.3900 . ? C13B C14B 1.3900 . ? C14B C15B 1.3900 . ? C15B C16B 1.3900 . ? C16B C17B 1.3900 . ? C18B C19B 1.376(13) . ? C19B C20B 1.391(16) . ? C20B C21B 1.371(15) . ? C21B C22B 1.357(12) . ? Pd3 N3C 2.047(10) . ? Pd3 N1C 2.057(10) . ? Pd3 C23C 2.084(9) . ? Pd3 N2C 2.115(7) . ? N1C C2C 1.300(15) . ? N1C C6C 1.450(14) . ? N2C C4C 1.344(10) . ? N2C C12C 1.439(9) . ? N3C C22C 1.340(13) . ? N3C C18C 1.354(14) . ? C1C C2C 1.535(11) . ? C2C C3C 1.399(13) . ? C3C C4C 1.405(11) . ? C4C C5C 1.504(13) . ? C6C C7C 1.365(12) . ? C6C C11C 1.400(13) . ? C7C C8C 1.385(13) . ? C8C C9C 1.396(13) . ? C9C C10C 1.361(13) . ? C10C C11C 1.380(13) . ? C12C C13C 1.386(11) . ? C12C C17C 1.387(12) . ? C13C C14C 1.389(13) . ? C14C C15C 1.357(15) . ? C15C C16C 1.379(14) . ? C16C C17C 1.396(12) . ? C18C C19C 1.372(12) . ? C19C C20C 1.394(15) . ? C20C C21C 1.401(15) . ? C21C C22C 1.364(12) . ? 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 N1A Pd1 N3A 176.0(3) . . ? N1A Pd1 C23A 92.2(5) . . ? N3A Pd1 C23A 84.4(6) . . ? N1A Pd1 N2A 90.8(3) . . ? N3A Pd1 N2A 92.5(3) . . ? C23A Pd1 N2A 176.9(5) . . ? C2A N1A C6A 115.6(7) . . ? C2A N1A Pd1 125.6(6) . . ? C6A N1A Pd1 118.7(6) . . ? C4A N2A C12A 117.7(8) . . ? C4A N2A Pd1 125.7(6) . . ? C12A N2A Pd1 116.5(5) . . ? C18A N3A C22A 117.3(8) . . ? C18A N3A Pd1 122.9(7) . . ? C22A N3A Pd1 119.6(6) . . ? N1A C2A C3A 125.0(8) . . ? N1A C2A C1A 119.6(8) . . ? C3A C2A C1A 115.3(8) . . ? C2A C3A C4A 130.2(8) . . ? N2A C4A C3A 122.0(8) . . ? N2A C4A C5A 122.4(9) . . ? C3A C4A C5A 115.6(8) . . ? C7A C6A C11A 119.6(9) . . ? C7A C6A N1A 120.5(8) . . ? C11A C6A N1A 119.7(10) . . ? C6A C7A C8A 121.3(9) . . ? C9A C8A C7A 120.2(10) . . ? C8A C9A C10A 118.6(10) . . ? C9A C10A C11A 120.4(10) . . ? C6A C11A C10A 119.8(10) . . ? C17A C12A C13A 119.4(9) . . ? C17A C12A N2A 121.2(10) . . ? C13A C12A N2A 119.3(9) . . ? C12A C13A C14A 120.6(10) . . ? C13A C14A C15A 118.4(11) . . ? C16A C15A C14A 120.9(11) . . ? C15A C16A C17A 119.3(11) . . ? C12A C17A C16A 121.1(11) . . ? N3A C18A C19A 122.4(9) . . ? C20A C19A C18A 118.4(9) . . ? C21A C20A C19A 120.2(9) . . ? C22A C21A C20A 117.6(11) . . ? N3A C22A C21A 124.0(10) . . ? N3B Pd2 N1B 177.7(3) . . ? N3B Pd2 C23B 84.4(3) . . ? N1B Pd2 C23B 94.1(3) . . ? N3B Pd2 N2B 90.7(3) . . ? N1B Pd2 N2B 90.7(3) . . ? C23B Pd2 N2B 175.1(3) . . ? C2B N1B C6B 116.5(8) . . ? C2B N1B Pd2 123.9(7) . . ? C6B N1B Pd2 119.5(6) . . ? C4B N2B C12B 119.5(7) . . ? C4B N2B Pd2 124.1(6) . . ? C12B N2B Pd2 116.3(5) . . ? C22B N3B C18B 116.6(8) . . ? C22B N3B Pd2 122.1(6) . . ? C18B N3B Pd2 121.3(7) . . ? N1B C2B C3B 125.6(10) . . ? N1B C2B C1B 118.1(9) . . ? C3B C2B C1B 116.3(9) . . ? C2B C3B C4B 129.2(9) . . ? N2B C4B C3B 123.3(9) . . ? N2B C4B C5B 120.2(8) . . ? C3B C4B C5B 116.5(8) . . ? C11B C6B C7B 119.3(10) . . ? C11B C6B N1B 123.7(10) . . ? C7B C6B N1B 116.9(9) . . ? C8B C7B C6B 119.2(12) . . ? C7B C8B C9B 121.7(12) . . ? C10B C9B C8B 118.9(11) . . ? C9B C10B C11B 121.2(11) . . ? C6B C11B C10B 119.7(10) . . ? C13B C12B C17B 120.0 . . ? C13B C12B N2B 120.9(5) . . ? C17B C12B N2B 119.0(5) . . ? C14B C13B C12B 120.0 . . ? C13B C14B C15B 120.0 . . ? C14B C15B C16B 120.0 . . ? C17B C16B C15B 120.0 . . ? C16B C17B C12B 120.0 . . ? N3B C18B C19B 122.4(10) . . ? C18B C19B C20B 118.6(9) . . ? C21B C20B C19B 119.1(9) . . ? C22B C21B C20B 119.3(9) . . ? N3B C22B C21B 123.8(9) . . ? N3C Pd3 N1C 176.2(4) . . ? N3C Pd3 C23C 83.8(4) . . ? N1C Pd3 C23C 93.5(4) . . ? N3C Pd3 N2C 91.9(3) . . ? N1C Pd3 N2C 90.7(4) . . ? C23C Pd3 N2C 175.2(3) . . ? C2C N1C C6C 118.9(9) . . ? C2C N1C Pd3 124.6(9) . . ? C6C N1C Pd3 116.5(7) . . ? C6C N1C Pd3 66.5(5) 2 . ? C4C N2C C12C 116.3(7) . . ? C4C N2C Pd3 125.3(5) . . ? C12C N2C Pd3 118.3(5) . . ? C22C N3C C18C 117.2(10) . . ? C22C N3C Pd3 123.8(8) . . ? C18C N3C Pd3 118.9(7) . . ? N1C C2C C3C 127.7(8) . . ? N1C C2C C1C 118.2(9) . . ? C3C C2C C1C 114.0(8) . . ? C2C C3C C4C 128.7(8) . . ? N2C C4C C3C 122.8(8) . . ? N2C C4C C5C 120.5(7) . . ? C3C C4C C5C 116.7(8) . . ? C7C C6C C11C 119.1(9) . . ? C7C C6C N1C 121.3(9) . . ? C11C C6C N1C 119.6(8) . . ? C6C C7C C8C 120.3(9) . . ? C7C C8C C9C 120.2(8) . . ? C10C C9C C8C 119.6(9) . . ? C9C C10C C11C 120.2(9) . . ? C10C C11C C6C 120.5(9) . . ? C13C C12C C17C 118.9(8) . . ? C13C C12C N2C 120.8(8) . . ? C17C C12C N2C 120.2(7) . . ? C12C C13C C14C 120.4(9) . . ? C15C C14C C13C 120.0(9) . . ? C14C C15C C16C 121.3(9) . . ? C15C C16C C17C 118.8(9) . . ? C12C C17C C16C 120.6(8) . . ? N3C C18C C19C 122.7(10) . . ? C18C C19C C20C 119.7(10) . . ? C19C C20C C21C 117.4(10) . . ? C22C C21C C20C 119.2(10) . . ? N3C C22C C21C 123.8(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.424 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.076 _vrf_PLAT088_complex3 ; RESPONSE: This alert is caused by whole molecule disordering, i.e., too many parameters were used to refine all atoms over three sets of coordinates. ; # Attachment 'complex4.txt' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 779766' #TrackingRef 'complex4.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H44 Cl4 N4 Pd4' _chemical_formula_weight 1220.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5383(8) _cell_length_b 13.6270(3) _cell_length_c 18.8184(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.5226(11) _cell_angle_gamma 90.00 _cell_volume 4550.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17143 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.51 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17143 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5211 _reflns_number_gt 4348 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.9774P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5211 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.128634(13) 0.070147(16) 0.150755(15) 0.02034(8) Uani 1 1 d . . . Pd2 Pd 0.009109(14) 0.001421(16) 0.135028(16) 0.02272(9) Uani 1 1 d . . . Cl1 Cl -0.05338(4) 0.16206(5) 0.12259(5) 0.02532(17) Uani 1 1 d . . . Cl2 Cl -0.11416(4) -0.05936(5) 0.07988(5) 0.02492(17) Uani 1 1 d . . . N1 N -0.19437(16) -0.00764(17) 0.17429(18) 0.0238(6) Uani 1 1 d . . . N2 N -0.13447(15) 0.17734(17) 0.22028(17) 0.0230(6) Uani 1 1 d . . . C1 C -0.1177(2) 0.2307(2) 0.3548(2) 0.0328(8) Uani 1 1 d . . . H1A H -0.1164 0.2965 0.3347 0.049 Uiso 1 1 calc R . . H1B H -0.0718 0.2199 0.4125 0.049 Uiso 1 1 calc R . . H1C H -0.1618 0.2248 0.3572 0.049 Uiso 1 1 calc R . . C2 C -0.12242(18) 0.1556(2) 0.2938(2) 0.0238(7) Uani 1 1 d . . . C3 C -0.11739(19) 0.0523(2) 0.3203(2) 0.0254(7) Uani 1 1 d . . . H3A H -0.1222 0.0514 0.3701 0.030 Uiso 1 1 calc R . . C4 C -0.1774(2) -0.0109(2) 0.2522(2) 0.0251(7) Uani 1 1 d . . . C5 C -0.2211(2) -0.0740(2) 0.2747(2) 0.0349(8) Uani 1 1 d . . . H5A H -0.2307 -0.1380 0.2466 0.052 Uiso 1 1 calc R . . H5B H -0.2691 -0.0421 0.2548 0.052 Uiso 1 1 calc R . . H5C H -0.1918 -0.0829 0.3374 0.052 Uiso 1 1 calc R . . C6 C -0.2177(2) 0.2968(2) 0.1121(2) 0.0298(8) Uani 1 1 d . . . H6A H -0.2547 0.2468 0.0838 0.036 Uiso 1 1 calc R . . C7 C -0.14826(19) 0.2761(2) 0.1869(2) 0.0250(7) Uani 1 1 d . . . C8 C -0.0937(2) 0.3476(2) 0.2270(2) 0.0357(8) Uani 1 1 d . . . H8A H -0.0457 0.3329 0.2778 0.043 Uiso 1 1 calc R . . C9 C -0.1099(2) 0.4415(3) 0.1920(3) 0.0447(10) Uani 1 1 d . . . H9A H -0.0725 0.4914 0.2188 0.054 Uiso 1 1 calc R . . C10 C -0.1798(2) 0.4628(3) 0.1187(3) 0.0405(9) Uani 1 1 d . . . H10A H -0.1910 0.5275 0.0960 0.049 Uiso 1 1 calc R . . C11 C -0.2327(2) 0.3908(3) 0.0789(2) 0.0386(9) Uani 1 1 d . . . H11A H -0.2805 0.4054 0.0278 0.046 Uiso 1 1 calc R . . C12 C -0.26033(19) -0.0568(2) 0.1045(2) 0.0272(7) Uani 1 1 d . . . C13 C -0.3283(2) -0.0073(3) 0.0597(3) 0.0363(9) Uani 1 1 d . . . H13A H -0.3310 0.0586 0.0743 0.044 Uiso 1 1 calc R . . C14 C -0.3925(2) -0.0540(3) -0.0066(3) 0.0457(10) Uani 1 1 d . . . H14A H -0.4395 -0.0205 -0.0371 0.055 Uiso 1 1 calc R . . C15 C -0.3881(2) -0.1496(3) -0.0284(3) 0.0441(10) Uani 1 1 d . . . H15A H -0.4321 -0.1819 -0.0737 0.053 Uiso 1 1 calc R . . C16 C -0.3204(2) -0.1977(3) 0.0155(2) 0.0380(9) Uani 1 1 d . . . H16A H -0.3175 -0.2628 -0.0004 0.046 Uiso 1 1 calc R . . C17 C -0.2561(2) -0.1521(2) 0.0827(2) 0.0308(8) Uani 1 1 d . . . H17A H -0.2093 -0.1862 0.1135 0.037 Uiso 1 1 calc R . . C18 C 0.04714(18) -0.1335(2) 0.1413(2) 0.0268(7) Uani 1 1 d . . . C19 C 0.06538(19) -0.1929(2) 0.2111(2) 0.0290(7) Uani 1 1 d . . . H19A H 0.0611 -0.1678 0.2552 0.035 Uiso 1 1 calc R . . C20 C 0.0898(2) -0.2890(2) 0.2163(2) 0.0369(9) Uani 1 1 d . . . H20A H 0.1024 -0.3290 0.2641 0.044 Uiso 1 1 calc R . . C21 C 0.0959(2) -0.3263(3) 0.1518(3) 0.0400(9) Uani 1 1 d . . . H21A H 0.1128 -0.3917 0.1556 0.048 Uiso 1 1 calc R . . C22 C 0.0771(2) -0.2683(3) 0.0818(2) 0.0364(9) Uani 1 1 d . . . H22A H 0.0810 -0.2935 0.0373 0.044 Uiso 1 1 calc R . . C23 C 0.05236(19) -0.1716(2) 0.0772(2) 0.0312(8) Uani 1 1 d . . . H23A H 0.0390 -0.1319 0.0290 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01879(14) 0.01960(14) 0.02112(14) -0.00165(8) 0.01041(11) -0.00063(9) Pd2 0.02165(15) 0.02284(15) 0.02335(15) -0.00053(8) 0.01255(12) -0.00064(9) Cl1 0.0246(4) 0.0231(4) 0.0302(4) -0.0015(3) 0.0167(4) -0.0024(3) Cl2 0.0228(4) 0.0230(4) 0.0292(4) -0.0052(3) 0.0149(4) -0.0022(3) N1 0.0219(15) 0.0247(14) 0.0259(15) -0.0012(10) 0.0141(13) 0.0003(10) N2 0.0219(14) 0.0202(12) 0.0237(14) -0.0018(10) 0.0109(12) 0.0008(10) C1 0.037(2) 0.0302(18) 0.0286(19) -0.0050(14) 0.0167(17) 0.0053(15) C2 0.0164(16) 0.0268(16) 0.0231(16) -0.0023(12) 0.0082(13) 0.0030(12) C3 0.0263(18) 0.0266(16) 0.0243(17) 0.0018(12) 0.0149(15) 0.0040(13) C4 0.0236(17) 0.0268(16) 0.0264(18) 0.0023(12) 0.0151(15) 0.0042(13) C5 0.031(2) 0.044(2) 0.035(2) -0.0008(15) 0.0216(18) -0.0056(16) C6 0.0312(19) 0.0283(17) 0.0244(18) -0.0028(13) 0.0123(15) 0.0025(14) C7 0.0284(18) 0.0220(15) 0.0266(17) 0.0007(12) 0.0168(15) 0.0070(13) C8 0.0277(19) 0.0252(17) 0.045(2) 0.0032(15) 0.0151(18) 0.0042(14) C9 0.043(2) 0.0248(19) 0.069(3) 0.0014(17) 0.034(2) 0.0009(16) C10 0.053(3) 0.0271(18) 0.055(3) 0.0117(17) 0.039(2) 0.0164(18) C11 0.048(2) 0.0363(19) 0.030(2) 0.0082(15) 0.0212(19) 0.0168(18) C12 0.0231(18) 0.0328(18) 0.0257(18) -0.0024(13) 0.0138(15) -0.0065(13) C13 0.030(2) 0.041(2) 0.039(2) -0.0015(15) 0.0201(19) -0.0008(15) C14 0.022(2) 0.068(3) 0.041(2) 0.000(2) 0.0144(18) -0.0052(18) C15 0.036(2) 0.064(3) 0.034(2) -0.0126(18) 0.0208(19) -0.028(2) C16 0.043(2) 0.041(2) 0.039(2) -0.0142(16) 0.029(2) -0.0197(17) C17 0.0275(19) 0.0321(18) 0.036(2) -0.0048(14) 0.0202(17) -0.0061(14) C18 0.0183(16) 0.0252(16) 0.0315(18) -0.0006(13) 0.0108(15) -0.0015(13) C19 0.0264(18) 0.0285(17) 0.0311(19) -0.0023(13) 0.0156(16) -0.0019(14) C20 0.035(2) 0.0305(18) 0.036(2) 0.0046(15) 0.0139(17) 0.0003(15) C21 0.041(2) 0.0303(18) 0.046(2) -0.0037(16) 0.023(2) 0.0054(16) C22 0.033(2) 0.038(2) 0.037(2) -0.0086(16) 0.0189(17) 0.0042(16) C23 0.0277(19) 0.0329(18) 0.0290(19) -0.0013(14) 0.0137(16) 0.0012(14) _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 N1 2.009(3) . ? Pd1 N2 2.012(2) . ? Pd1 Cl1 2.3347(8) . ? Pd1 Cl2 2.3371(8) . ? Pd2 C18 1.988(3) . ? Pd2 C3 2.099(3) 2 ? Pd2 Cl2 2.3851(8) . ? Pd2 Cl1 2.5101(8) . ? N1 C4 1.295(4) . ? N1 C12 1.441(4) . ? N2 C2 1.288(4) . ? N2 C7 1.444(4) . ? C1 C2 1.499(4) . ? C2 C3 1.477(4) . ? C3 C4 1.475(5) . ? C3 Pd2 2.099(3) 2 ? C4 C5 1.501(5) . ? C6 C11 1.381(5) . ? C6 C7 1.383(5) . ? C7 C8 1.376(5) . ? C8 C9 1.390(5) . ? C9 C10 1.378(6) . ? C10 C11 1.362(6) . ? C12 C17 1.381(4) . ? C12 C13 1.383(5) . ? C13 C14 1.385(5) . ? C14 C15 1.386(6) . ? C15 C16 1.368(6) . ? C16 C17 1.386(5) . ? C18 C23 1.375(5) . ? C18 C19 1.396(5) . ? C19 C20 1.393(5) . ? C20 C21 1.389(5) . ? C21 C22 1.387(5) . ? C22 C23 1.406(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 85.87(10) . . ? N1 Pd1 Cl1 179.29(8) . . ? N2 Pd1 Cl1 93.75(8) . . ? N1 Pd1 Cl2 93.79(7) . . ? N2 Pd1 Cl2 175.63(8) . . ? Cl1 Pd1 Cl2 86.63(3) . . ? C18 Pd2 C3 87.41(13) . 2 ? C18 Pd2 Cl2 91.39(9) . . ? C3 Pd2 Cl2 177.85(9) 2 . ? C18 Pd2 Cl1 173.09(9) . . ? C3 Pd2 Cl1 99.47(9) 2 . ? Cl2 Pd2 Cl1 81.75(3) . . ? Pd1 Cl1 Pd2 85.15(2) . . ? Pd1 Cl2 Pd2 88.00(3) . . ? C4 N1 C12 121.0(3) . . ? C4 N1 Pd1 119.0(2) . . ? C12 N1 Pd1 119.9(2) . . ? C2 N2 C7 123.3(3) . . ? C2 N2 Pd1 118.8(2) . . ? C7 N2 Pd1 117.8(2) . . ? N2 C2 C3 120.9(3) . . ? N2 C2 C1 123.4(3) . . ? C3 C2 C1 115.5(3) . . ? C4 C3 C2 113.7(3) . . ? C4 C3 Pd2 112.5(2) . 2 ? C2 C3 Pd2 107.6(2) . 2 ? N1 C4 C3 120.6(3) . . ? N1 C4 C5 121.2(3) . . ? C3 C4 C5 118.0(3) . . ? C11 C6 C7 119.4(3) . . ? C8 C7 C6 120.6(3) . . ? C8 C7 N2 121.3(3) . . ? C6 C7 N2 118.0(3) . . ? C7 C8 C9 119.0(3) . . ? C10 C9 C8 120.4(4) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C6 120.7(4) . . ? C17 C12 C13 120.2(3) . . ? C17 C12 N1 120.7(3) . . ? C13 C12 N1 119.0(3) . . ? C12 C13 C14 119.8(3) . . ? C13 C14 C15 119.8(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 120.6(4) . . ? C12 C17 C16 119.5(3) . . ? C23 C18 C19 119.1(3) . . ? C23 C18 Pd2 122.2(3) . . ? C19 C18 Pd2 118.7(2) . . ? C20 C19 C18 120.4(3) . . ? C21 C20 C19 120.1(3) . . ? C22 C21 C20 120.1(3) . . ? C21 C22 C23 119.2(3) . . ? C18 C23 C22 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.195 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.122 # Attachment 'complex5.txt' data_complex5 _database_code_depnum_ccdc_archive 'CCDC 779767' #TrackingRef 'complex5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 Br2 Cl8 N4 Pd2' _chemical_formula_weight 1210.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8468(2) _cell_length_b 23.2955(7) _cell_length_c 11.6038(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.5891(13) _cell_angle_gamma 90.00 _cell_volume 2238.68(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21574 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 3.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.828 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21574 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5089 _reflns_number_gt 4217 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+6.0414P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5089 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.62416(3) 0.068815(12) 2.08741(2) 0.01706(10) Uani 1 1 d . . . Br1 Br 1.92055(5) 0.06004(2) 2.21302(4) 0.03208(13) Uani 1 1 d . . . N1 N 1.6684(4) 0.02976(14) 1.9457(3) 0.0191(6) Uani 1 1 d . . . N2 N 1.5611(4) 0.11229(14) 2.2174(3) 0.0193(6) Uani 1 1 d . . . C1 C 1.6211(5) -0.06437(17) 2.0101(4) 0.0203(8) Uani 1 1 d . . . H1A H 1.6464 -0.0476 2.0932 0.024 Uiso 1 1 calc R . . H1B H 1.6759 -0.1018 2.0155 0.024 Uiso 1 1 calc R . . C2 C 1.6537(4) -0.02520(17) 1.9245(3) 0.0197(8) Uani 1 1 d . . . C3 C 1.6734(5) -0.05097(18) 1.8104(4) 0.0254(9) Uani 1 1 d . . . H3A H 1.6563 -0.0202 1.7483 0.030 Uiso 1 1 calc R . . H3B H 1.7862 -0.0644 1.8325 0.030 Uiso 1 1 calc R . . C4 C 1.4377(5) 0.10027(17) 2.2482(3) 0.0212(8) Uani 1 1 d . . . C5 C 1.3967(5) 0.1317(2) 2.3458(4) 0.0336(10) Uani 1 1 d . . . H5C H 1.4865 0.1570 2.3912 0.050 Uiso 1 1 calc R . . H5B H 1.3776 0.1040 2.4028 0.050 Uiso 1 1 calc R . . H5A H 1.2992 0.1548 2.3075 0.050 Uiso 1 1 calc R . . C6 C 1.7104(5) 0.06845(17) 1.8657(3) 0.0212(8) Uani 1 1 d . . . C7 C 1.8634(5) 0.06591(19) 1.8574(4) 0.0275(9) Uani 1 1 d . . . H7A H 1.9394 0.0381 1.9032 0.033 Uiso 1 1 calc R . . C8 C 1.9041(6) 0.1046(2) 1.7812(4) 0.0365(11) Uani 1 1 d . . . H8A H 2.0083 0.1030 1.7750 0.044 Uiso 1 1 calc R . . C9 C 1.7946(6) 0.1451(2) 1.7150(4) 0.0397(11) Uani 1 1 d . . . H9A H 1.8231 0.1712 1.6630 0.048 Uiso 1 1 calc R . . C10 C 1.6438(6) 0.1478(2) 1.7240(4) 0.0409(11) Uani 1 1 d . . . H10A H 1.5682 0.1757 1.6781 0.049 Uiso 1 1 calc R . . C11 C 1.6015(5) 0.1098(2) 1.8000(4) 0.0325(10) Uani 1 1 d . . . H11A H 1.4979 0.1123 1.8070 0.039 Uiso 1 1 calc R . . C12 C 1.6576(5) 0.16205(17) 2.2711(3) 0.0218(8) Uani 1 1 d . . . C13 C 1.7959(5) 0.15681(19) 2.3741(4) 0.0282(9) Uani 1 1 d . . . H13A H 1.8257 0.1206 2.4133 0.034 Uiso 1 1 calc R . . C14 C 1.8904(5) 0.2048(2) 2.4196(4) 0.0326(10) Uani 1 1 d . . . H14A H 1.9859 0.2012 2.4900 0.039 Uiso 1 1 calc R . . C15 C 1.8479(6) 0.2578(2) 2.3638(4) 0.0353(10) Uani 1 1 d . . . H15A H 1.9145 0.2903 2.3952 0.042 Uiso 1 1 calc R . . C16 C 1.7076(6) 0.2632(2) 2.2620(4) 0.0359(10) Uani 1 1 d . . . H16A H 1.6763 0.2997 2.2245 0.043 Uiso 1 1 calc R . . C17 C 1.6126(5) 0.21507(19) 2.2149(4) 0.0306(9) Uani 1 1 d . . . H17A H 1.5172 0.2185 2.1444 0.037 Uiso 1 1 calc R . . C18 C 1.9368(7) 0.1960(2) 2.0670(6) 0.0491(13) Uani 1 1 d . . . H18A H 1.8960 0.1578 2.0330 0.059 Uiso 1 1 calc R . . H18B H 1.9462 0.1965 2.1546 0.059 Uiso 1 1 calc R . . C19A C 1.3109(12) 0.0255(4) 1.6084(9) 0.042(2) Uani 0.50 1 d P A 1 H19B H 1.4252 0.0375 1.6449 0.050 Uiso 0.50 1 calc PR A 1 H19A H 1.2866 0.0019 1.6707 0.050 Uiso 0.50 1 calc PR A 1 C19B C 1.1483(11) 0.0228(4) 1.5372(9) 0.037(2) Uani 0.50 1 d P A 2 H19D H 1.0457 0.0214 1.4659 0.045 Uiso 0.50 1 calc PR A 2 H19C H 1.1310 0.0012 1.6050 0.045 Uiso 0.50 1 calc PR A 2 Cl1 Cl 1.79860(16) 0.24818(7) 1.98726(13) 0.0527(3) Uani 1 1 d . . . Cl2 Cl 2.12707(18) 0.20658(9) 2.05773(19) 0.0741(5) Uani 1 1 d . . . Cl3 Cl 1.2940(2) -0.01339(8) 1.49642(19) 0.0799(6) Uani 1 1 d . . . Cl4 Cl 1.18387(16) 0.09105(7) 1.58116(13) 0.0502(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01605(15) 0.01963(17) 0.01557(15) -0.00148(11) 0.00564(11) -0.00083(11) Br1 0.0216(2) 0.0427(3) 0.0278(2) -0.00449(19) 0.00343(17) 0.00495(17) N1 0.0176(15) 0.0230(18) 0.0171(15) 0.0000(13) 0.0067(12) 0.0001(12) N2 0.0195(15) 0.0200(17) 0.0174(15) -0.0013(13) 0.0055(13) 0.0013(12) C1 0.0208(18) 0.021(2) 0.0197(18) -0.0035(15) 0.0077(15) -0.0009(14) C2 0.0128(16) 0.023(2) 0.0202(18) -0.0042(16) 0.0026(14) 0.0002(14) C3 0.0241(19) 0.028(2) 0.028(2) -0.0064(18) 0.0145(17) -0.0037(17) C4 0.0216(18) 0.023(2) 0.0190(18) -0.0033(15) 0.0068(15) 0.0009(15) C5 0.032(2) 0.041(3) 0.034(2) -0.015(2) 0.019(2) -0.0051(19) C6 0.0254(19) 0.025(2) 0.0137(17) -0.0033(15) 0.0071(15) -0.0035(16) C7 0.025(2) 0.031(2) 0.028(2) 0.0007(18) 0.0110(17) -0.0007(17) C8 0.040(2) 0.040(3) 0.040(3) -0.003(2) 0.027(2) -0.010(2) C9 0.055(3) 0.036(3) 0.035(3) 0.002(2) 0.026(2) -0.010(2) C10 0.047(3) 0.039(3) 0.035(3) 0.014(2) 0.013(2) 0.003(2) C11 0.029(2) 0.035(3) 0.035(2) 0.006(2) 0.0132(19) 0.0030(19) C12 0.0229(18) 0.026(2) 0.0186(18) -0.0056(16) 0.0092(15) -0.0015(16) C13 0.029(2) 0.027(2) 0.023(2) -0.0023(17) 0.0036(17) 0.0008(17) C14 0.029(2) 0.034(3) 0.029(2) -0.0064(19) 0.0035(18) -0.0055(18) C15 0.042(3) 0.030(3) 0.034(2) -0.011(2) 0.014(2) -0.015(2) C16 0.052(3) 0.022(2) 0.033(2) -0.0009(19) 0.013(2) -0.009(2) C17 0.036(2) 0.029(2) 0.024(2) 0.0019(18) 0.0057(18) 0.0008(18) C18 0.052(3) 0.038(3) 0.062(4) 0.011(3) 0.026(3) 0.005(2) C19A 0.043(5) 0.038(6) 0.032(5) 0.000(4) -0.002(4) 0.002(4) C19B 0.031(5) 0.043(6) 0.039(5) 0.007(4) 0.015(4) 0.000(4) Cl1 0.0482(7) 0.0602(9) 0.0514(8) 0.0136(7) 0.0196(6) 0.0091(6) Cl2 0.0406(8) 0.0851(13) 0.0991(13) -0.0297(10) 0.0274(8) -0.0022(8) Cl3 0.1042(13) 0.0666(11) 0.1016(13) 0.0445(10) 0.0772(12) 0.0437(10) Cl4 0.0436(7) 0.0550(9) 0.0493(7) -0.0001(6) 0.0131(6) 0.0030(6) _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 N1 2.034(3) . ? Pd1 N2 2.050(3) . ? Pd1 C1 2.067(4) 3_859 ? Pd1 Br1 2.5206(5) . ? Pd1 C2 2.618(4) 3_859 ? N1 C2 1.302(5) . ? N1 C6 1.434(5) . ? N2 C4 1.293(5) . ? N2 C12 1.445(5) . ? C1 C2 1.450(5) . ? C1 Pd1 2.067(4) 3_859 ? C2 C3 1.519(5) . ? C2 Pd1 2.618(4) 3_859 ? C3 C4 1.509(6) 3_859 ? C4 C5 1.498(5) . ? C4 C3 1.509(6) 3_859 ? C6 C11 1.387(6) . ? C6 C7 1.392(6) . ? C7 C8 1.396(6) . ? C8 C9 1.376(7) . ? C9 C10 1.377(7) . ? C10 C11 1.389(6) . ? C12 C13 1.382(6) . ? C12 C17 1.388(6) . ? C13 C14 1.384(6) . ? C14 C15 1.383(7) . ? C15 C16 1.386(7) . ? C16 C17 1.392(6) . ? C18 Cl1 1.741(5) . ? C18 Cl2 1.741(5) . ? C19A Cl3 1.548(10) . ? C19A Cl4 1.856(10) . ? C19B Cl4 1.666(10) . ? C19B Cl3 1.739(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 174.35(12) . . ? N1 Pd1 C1 89.93(14) . 3_859 ? N2 Pd1 C1 85.56(14) . 3_859 ? N1 Pd1 Br1 88.52(9) . . ? N2 Pd1 Br1 96.40(9) . . ? C1 Pd1 Br1 172.20(11) 3_859 . ? N1 Pd1 C2 103.16(12) . 3_859 ? N2 Pd1 C2 74.78(12) . 3_859 ? C1 Pd1 C2 33.50(14) 3_859 3_859 ? Br1 Pd1 C2 139.96(9) . 3_859 ? C2 N1 C6 121.8(3) . . ? C2 N1 Pd1 123.9(3) . . ? C6 N1 Pd1 114.2(2) . . ? C4 N2 C12 118.9(3) . . ? C4 N2 Pd1 124.8(3) . . ? C12 N2 Pd1 116.2(2) . . ? C2 C1 Pd1 94.6(2) . 3_859 ? N1 C2 C1 121.4(3) . . ? N1 C2 C3 121.3(3) . . ? C1 C2 C3 117.4(3) . . ? N1 C2 Pd1 114.9(2) . 3_859 ? C1 C2 Pd1 51.89(19) . 3_859 ? C3 C2 Pd1 101.2(2) . 3_859 ? C4 C3 C2 115.9(3) 3_859 . ? N2 C4 C5 123.8(4) . . ? N2 C4 C3 121.3(3) . 3_859 ? C5 C4 C3 114.9(3) . 3_859 ? C11 C6 C7 119.8(4) . . ? C11 C6 N1 120.3(4) . . ? C7 C6 N1 119.9(4) . . ? C6 C7 C8 119.3(4) . . ? C9 C8 C7 120.6(4) . . ? C8 C9 C10 119.9(4) . . ? C9 C10 C11 120.3(5) . . ? C6 C11 C10 120.0(4) . . ? C13 C12 C17 120.4(4) . . ? C13 C12 N2 120.7(4) . . ? C17 C12 N2 118.9(3) . . ? C12 C13 C14 119.4(4) . . ? C15 C14 C13 120.9(4) . . ? C14 C15 C16 119.7(4) . . ? C15 C16 C17 119.8(4) . . ? C12 C17 C16 119.9(4) . . ? Cl1 C18 Cl2 112.5(3) . . ? Cl3 C19A Cl4 117.7(5) . . ? Cl4 C19B Cl3 117.9(5) . . ? C19A Cl3 C19B 49.4(5) . . ? C19B Cl4 C19A 46.0(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.673 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.128