# 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 'Shi, Min' _publ_contact_author_email mshi@mail.sioc.ac.cn _publ_section_title ; PdCl2-promoted Reactions of Diaryl-substituted Methylenecyclopropanes ; loop_ _publ_author_name 'Min Shi' 'MingHui Qi' 'Li-Xiong Shao' # Attachment 'all.cif' data_cd26332 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 620092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Cl4 Pd2' _chemical_formula_weight 767.14 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' 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 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 9.1826(8) _cell_length_b 15.1250(13) _cell_length_c 11.1711(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.164(2) _cell_angle_gamma 90.00 _cell_volume 1539.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2298 _cell_measurement_theta_min 4.596 _cell_measurement_theta_max 45.669 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.193 _exptl_crystal_size_mid 0.122 _exptl_crystal_size_min 0.099 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79775 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs-Bruker _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8947 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3355 _reflns_number_gt 2467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3355 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.93872(3) 0.474848(19) 0.85138(3) 0.04403(12) Uani 1 1 d . . . Cl1 Cl 1.13044(11) 0.56320(7) 0.95320(9) 0.0562(3) Uani 1 1 d . . . Cl2 Cl 0.69245(16) 0.53220(11) 0.46856(12) 0.1028(5) Uani 1 1 d . . . C1 C 0.8032(4) 0.3868(3) 0.7331(3) 0.0472(10) Uani 1 1 d . . . C2 C 0.8354(5) 0.4656(3) 0.6725(3) 0.0518(10) Uani 1 1 d . . . C3 C 0.9853(5) 0.4880(3) 0.6740(4) 0.0581(11) Uani 1 1 d . . . H3A H 1.0063 0.5473 0.6478 0.070 Uiso 1 1 calc R . . H3B H 1.0481 0.4431 0.6454 0.070 Uiso 1 1 calc R . . C4 C 0.7221(5) 0.5327(3) 0.6285(4) 0.0713(13) Uani 1 1 d . . . H4A H 0.7544 0.5909 0.6570 0.086 Uiso 1 1 calc R . . H4B H 0.6309 0.5194 0.6602 0.086 Uiso 1 1 calc R . . C5 C 0.6511(4) 0.3685(3) 0.7618(3) 0.0500(10) Uani 1 1 d . . . C6 C 0.5816(5) 0.2901(3) 0.7216(4) 0.0675(13) Uani 1 1 d . . . H6 H 0.6313 0.2487 0.6804 0.081 Uiso 1 1 calc R . . C7 C 0.4396(5) 0.2737(3) 0.7427(5) 0.0797(15) Uani 1 1 d . . . H7 H 0.3936 0.2216 0.7146 0.096 Uiso 1 1 calc R . . C8 C 0.3656(5) 0.3328(4) 0.8043(4) 0.0731(14) Uani 1 1 d . . . H8 H 0.2698 0.3208 0.8184 0.088 Uiso 1 1 calc R . . C9 C 0.4316(4) 0.4100(3) 0.8456(4) 0.0597(11) Uani 1 1 d . . . H9 H 0.3807 0.4506 0.8873 0.072 Uiso 1 1 calc R . . C10 C 0.5739(4) 0.4275(3) 0.8253(3) 0.0496(10) Uani 1 1 d . . . H10 H 0.6188 0.4796 0.8545 0.060 Uiso 1 1 calc R . . C11 C 0.9012(4) 0.3067(3) 0.7322(4) 0.0549(11) Uani 1 1 d . . . C12 C 0.9410(5) 0.2594(3) 0.8363(4) 0.0635(12) Uani 1 1 d . . . H12 H 0.9061 0.2763 0.9076 0.076 Uiso 1 1 calc R . . C13 C 1.0331(5) 0.1865(3) 0.8358(5) 0.0797(15) Uani 1 1 d . . . H13 H 1.0596 0.1548 0.9065 0.096 Uiso 1 1 calc R . . C14 C 1.0843(6) 0.1615(3) 0.7326(6) 0.0897(19) Uani 1 1 d . . . H14 H 1.1472 0.1133 0.7330 0.108 Uiso 1 1 calc R . . C15 C 1.0441(6) 0.2067(4) 0.6276(6) 0.0899(18) Uani 1 1 d . . . H15 H 1.0783 0.1885 0.5567 0.108 Uiso 1 1 calc R . . C16 C 0.9527(5) 0.2797(3) 0.6267(5) 0.0763(14) Uani 1 1 d . . . H16 H 0.9259 0.3105 0.5553 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03924(19) 0.04548(19) 0.04799(19) -0.00345(14) 0.00791(13) -0.00408(14) Cl1 0.0535(6) 0.0622(6) 0.0539(6) -0.0017(5) 0.0108(5) -0.0221(5) Cl2 0.0759(9) 0.1701(16) 0.0626(8) 0.0248(9) 0.0093(7) 0.0080(10) C1 0.036(2) 0.054(2) 0.050(2) -0.0143(19) 0.0001(18) -0.0010(18) C2 0.049(3) 0.061(3) 0.044(2) -0.0060(19) 0.0040(19) 0.001(2) C3 0.056(3) 0.070(3) 0.051(3) -0.006(2) 0.016(2) -0.004(2) C4 0.073(3) 0.081(3) 0.059(3) 0.012(2) 0.006(2) 0.006(3) C5 0.035(2) 0.059(3) 0.053(2) -0.0049(19) -0.0027(18) 0.0006(19) C6 0.053(3) 0.067(3) 0.081(3) -0.021(2) 0.003(2) -0.003(2) C7 0.051(3) 0.074(3) 0.112(4) -0.018(3) 0.001(3) -0.017(3) C8 0.037(3) 0.085(4) 0.096(4) 0.011(3) 0.004(2) -0.010(3) C9 0.048(3) 0.070(3) 0.062(3) 0.006(2) 0.010(2) 0.010(2) C10 0.043(2) 0.053(2) 0.053(2) -0.0013(19) 0.0046(19) 0.001(2) C11 0.040(2) 0.057(3) 0.068(3) -0.020(2) 0.007(2) -0.007(2) C12 0.055(3) 0.048(3) 0.090(4) -0.012(2) 0.020(2) -0.006(2) C13 0.057(3) 0.049(3) 0.134(5) -0.001(3) 0.019(3) -0.002(2) C14 0.052(3) 0.059(3) 0.161(6) -0.038(4) 0.024(4) -0.002(3) C15 0.061(4) 0.099(4) 0.110(5) -0.058(4) 0.014(3) 0.001(3) C16 0.056(3) 0.090(4) 0.082(3) -0.037(3) 0.006(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 Pd C3 2.088(4) . ? Pd C2 2.107(4) . ? Pd C1 2.158(3) . ? Pd Cl1 2.3832(10) . ? Pd Cl1 2.4178(11) 3_767 ? Cl1 Pd 2.4178(11) 3_767 ? Cl2 C4 1.773(5) . ? C1 C2 1.420(5) . ? C1 C5 1.497(5) . ? C1 C11 1.510(5) . ? C2 C3 1.416(6) . ? C2 C4 1.492(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.389(5) . ? C5 C6 1.394(5) . ? C6 C7 1.376(6) . ? C6 H6 0.9300 . ? C7 C8 1.361(7) . ? C7 H7 0.9300 . ? C8 C9 1.369(6) . ? C8 H8 0.9300 . ? C9 C10 1.380(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.376(6) . ? C11 C16 1.385(6) . ? C12 C13 1.391(6) . ? C12 H12 0.9300 . ? C13 C14 1.351(7) . ? C13 H13 0.9300 . ? C14 C15 1.368(8) . ? C14 H14 0.9300 . ? C15 C16 1.386(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? 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 C3 Pd C2 39.44(15) . . ? C3 Pd C1 69.44(16) . . ? C2 Pd C1 38.88(14) . . ? C3 Pd Cl1 99.95(12) . . ? C2 Pd Cl1 135.09(12) . . ? C1 Pd Cl1 166.78(11) . . ? C3 Pd Cl1 170.90(12) . 3_767 ? C2 Pd Cl1 134.63(12) . 3_767 ? C1 Pd Cl1 102.09(11) . 3_767 ? Cl1 Pd Cl1 87.95(3) . 3_767 ? Pd Cl1 Pd 92.05(3) . 3_767 ? C2 C1 C5 120.8(3) . . ? C2 C1 C11 120.7(4) . . ? C5 C1 C11 115.2(3) . . ? C2 C1 Pd 68.6(2) . . ? C5 C1 Pd 117.8(3) . . ? C11 C1 Pd 101.6(2) . . ? C3 C2 C1 117.1(4) . . ? C3 C2 C4 118.6(4) . . ? C1 C2 C4 123.3(4) . . ? C3 C2 Pd 69.6(2) . . ? C1 C2 Pd 72.5(2) . . ? C4 C2 Pd 118.7(3) . . ? C2 C3 Pd 71.0(2) . . ? C2 C3 H3A 116.5 . . ? Pd C3 H3A 116.5 . . ? C2 C3 H3B 116.5 . . ? Pd C3 H3B 116.5 . . ? H3A C3 H3B 113.5 . . ? C2 C4 Cl2 110.0(3) . . ? C2 C4 H4A 109.7 . . ? Cl2 C4 H4A 109.7 . . ? C2 C4 H4B 109.7 . . ? Cl2 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C10 C5 C6 117.9(4) . . ? C10 C5 C1 122.6(4) . . ? C6 C5 C1 119.4(4) . . ? C7 C6 C5 120.3(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 120.8(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C5 121.0(4) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? C12 C11 C16 118.9(4) . . ? C12 C11 C1 120.5(4) . . ? C16 C11 C1 120.6(4) . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.1(5) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.5(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 119.9(5) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? 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 C3 Pd Cl1 Pd -175.45(13) . . . 3_767 ? C2 Pd Cl1 Pd 163.69(16) . . . 3_767 ? C1 Pd Cl1 Pd -139.8(5) . . . 3_767 ? Cl1 Pd Cl1 Pd 0.0 3_767 . . 3_767 ? C3 Pd C1 C2 -31.9(2) . . . . ? Cl1 Pd C1 C2 -69.8(5) . . . . ? Cl1 Pd C1 C2 151.5(2) 3_767 . . . ? C3 Pd C1 C5 -146.5(3) . . . . ? C2 Pd C1 C5 -114.6(4) . . . . ? Cl1 Pd C1 C5 175.6(3) . . . . ? Cl1 Pd C1 C5 36.9(3) 3_767 . . . ? C3 Pd C1 C11 86.7(3) . . . . ? C2 Pd C1 C11 118.6(4) . . . . ? Cl1 Pd C1 C11 48.9(6) . . . . ? Cl1 Pd C1 C11 -89.8(3) 3_767 . . . ? C5 C1 C2 C3 165.5(4) . . . . ? C11 C1 C2 C3 -36.0(5) . . . . ? Pd C1 C2 C3 55.1(3) . . . . ? C5 C1 C2 C4 -2.9(6) . . . . ? C11 C1 C2 C4 155.6(4) . . . . ? Pd C1 C2 C4 -113.3(4) . . . . ? C5 C1 C2 Pd 110.4(3) . . . . ? C11 C1 C2 Pd -91.1(3) . . . . ? C1 Pd C2 C3 -128.8(4) . . . . ? Cl1 Pd C2 C3 33.5(3) . . . . ? Cl1 Pd C2 C3 -169.7(2) 3_767 . . . ? C3 Pd C2 C1 128.8(4) . . . . ? Cl1 Pd C2 C1 162.30(17) . . . . ? Cl1 Pd C2 C1 -40.9(3) 3_767 . . . ? C3 Pd C2 C4 -112.2(4) . . . . ? C1 Pd C2 C4 119.0(4) . . . . ? Cl1 Pd C2 C4 -78.7(4) . . . . ? Cl1 Pd C2 C4 78.0(4) 3_767 . . . ? C1 C2 C3 Pd -56.6(3) . . . . ? C4 C2 C3 Pd 112.4(3) . . . . ? C1 Pd C3 C2 31.5(2) . . . . ? Cl1 Pd C3 C2 -156.7(2) . . . . ? Cl1 Pd C3 C2 53.4(9) 3_767 . . . ? C3 C2 C4 Cl2 81.3(4) . . . . ? C1 C2 C4 Cl2 -110.4(4) . . . . ? Pd C2 C4 Cl2 162.4(2) . . . . ? C2 C1 C5 C10 -54.2(5) . . . . ? C11 C1 C5 C10 146.1(4) . . . . ? Pd C1 C5 C10 26.2(5) . . . . ? C2 C1 C5 C6 124.4(4) . . . . ? C11 C1 C5 C6 -35.2(5) . . . . ? Pd C1 C5 C6 -155.1(3) . . . . ? C10 C5 C6 C7 1.4(6) . . . . ? C1 C5 C6 C7 -177.3(4) . . . . ? C5 C6 C7 C8 -0.9(8) . . . . ? C6 C7 C8 C9 0.4(8) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 C5 0.9(6) . . . . ? C6 C5 C10 C9 -1.4(6) . . . . ? C1 C5 C10 C9 177.2(4) . . . . ? C2 C1 C11 C12 135.8(4) . . . . ? C5 C1 C11 C12 -64.5(5) . . . . ? Pd C1 C11 C12 63.9(4) . . . . ? C2 C1 C11 C16 -44.0(5) . . . . ? C5 C1 C11 C16 115.7(4) . . . . ? Pd C1 C11 C16 -115.9(3) . . . . ? C16 C11 C12 C13 0.9(6) . . . . ? C1 C11 C12 C13 -179.0(4) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C12 C13 C14 C15 -1.1(8) . . . . ? C13 C14 C15 C16 1.3(8) . . . . ? C12 C11 C16 C15 -0.7(6) . . . . ? C1 C11 C16 C15 179.1(4) . . . . ? C14 C15 C16 C11 -0.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.790 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.096 data_cd26351 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 621667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.67 H30.67 Cl4 O2 Pd2' _chemical_formula_weight 809.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/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 14.9609(9) _cell_length_b 20.8396(13) _cell_length_c 15.0025(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.0760(10) _cell_angle_gamma 90.00 _cell_volume 4674.4(5) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5890 _cell_measurement_theta_min 4.376 _cell_measurement_theta_max 50.081 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.507 _exptl_crystal_size_mid 0.281 _exptl_crystal_size_min 0.224 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77689 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs-Bruker _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25386 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9165 _reflns_number_gt 6192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 6 distance restraints of solvent. 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. The high residual election density is because the ghost peak around Pd atom. ; _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^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9165 _refine_ls_number_parameters 533 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 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 0.35917(3) 0.26470(2) 0.69623(3) 0.04040(15) Uani 1 1 d . . . Pd2 Pd 0.15364(3) 0.25816(2) 0.57627(3) 0.03944(15) Uani 1 1 d . . . Pd3 Pd 0.11649(3) 0.50729(2) 0.00916(3) 0.03843(15) Uani 1 1 d . . . Cl1 Cl 0.20312(10) 0.26715(9) 0.73016(11) 0.0557(4) Uani 1 1 d . . . Cl2 Cl 0.30876(10) 0.26388(9) 0.54168(11) 0.0558(4) Uani 1 1 d . . . Cl3 Cl -0.00462(10) 0.49842(7) 0.11100(10) 0.0457(4) Uani 1 1 d . . . Cl4 Cl 0.3510(4) 0.4581(3) 0.5881(4) 0.223(2) Uiso 1 1 d D . . Cl5 Cl 0.1988(7) 0.4320(5) 0.5546(8) 0.271(6) Uiso 1 1 d D . . Cl6 Cl 0.1928(4) 0.4706(3) 0.6967(4) 0.217(2) Uiso 1 1 d D . . O1 O 0.4555(4) 0.3798(3) 0.8767(4) 0.0939(19) Uani 1 1 d . . . H1 H 0.4008 0.3790 0.8710 0.141 Uiso 1 1 calc RD . . O2 O 0.0876(3) 0.1394(2) 0.4094(3) 0.0634(13) Uani 1 1 d . . . H2 H 0.0649 0.1094 0.3813 0.095 Uiso 1 1 calc R . . O3 O 0.2780(3) 0.3925(3) -0.0782(4) 0.0721(14) Uani 1 1 d . . . H3 H 0.2334 0.3696 -0.0788 0.108 Uiso 1 1 calc R . . C1 C 0.5021(4) 0.2615(3) 0.6963(4) 0.0399(14) Uani 1 1 d . . . C2 C 0.4726(4) 0.2884(3) 0.7772(4) 0.0468(15) Uani 1 1 d . . . C3 C 0.4136(4) 0.2518(3) 0.8269(4) 0.0526(17) Uani 1 1 d . . . H3A H 0.3838 0.2740 0.8743 0.063 Uiso 1 1 calc RD . . H3B H 0.4329 0.2088 0.8428 0.063 Uiso 1 1 calc R . . C4 C 0.4921(4) 0.3583(3) 0.8001(5) 0.0590(18) Uani 1 1 d . . . H4A H 0.5564 0.3641 0.8053 0.071 Uiso 1 1 calc R . . H4B H 0.4700 0.3849 0.7509 0.071 Uiso 1 1 calc R . . C5 C 0.5554(4) 0.3021(3) 0.6356(4) 0.0420(14) Uani 1 1 d . . . C6 C 0.6458(4) 0.3091(3) 0.6530(5) 0.0626(19) Uani 1 1 d . . . H6 H 0.6724 0.2866 0.7004 0.075 Uiso 1 1 calc R . . C7 C 0.6980(5) 0.3482(4) 0.6027(6) 0.073(2) Uani 1 1 d . . . H7 H 0.7585 0.3531 0.6174 0.087 Uiso 1 1 calc R . . C8 C 0.6607(5) 0.3794(4) 0.5316(6) 0.073(2) Uani 1 1 d . . . H8 H 0.6963 0.4047 0.4962 0.088 Uiso 1 1 calc R . . C9 C 0.5720(6) 0.3742(4) 0.5116(6) 0.092(3) Uani 1 1 d . . . H9 H 0.5463 0.3972 0.4641 0.111 Uiso 1 1 calc R . . C10 C 0.5193(5) 0.3341(4) 0.5629(5) 0.074(2) Uani 1 1 d . . . H10 H 0.4590 0.3290 0.5475 0.089 Uiso 1 1 calc R . . C11 C 0.5247(4) 0.1911(3) 0.6904(5) 0.0494(16) Uani 1 1 d . . . C12 C 0.5051(4) 0.1562(3) 0.6122(5) 0.0553(17) Uani 1 1 d . . . H12 H 0.4765 0.1762 0.5637 0.066 Uiso 1 1 calc R . . C13 C 0.5282(5) 0.0920(4) 0.6071(6) 0.072(2) Uani 1 1 d . . . H13 H 0.5144 0.0693 0.5550 0.086 Uiso 1 1 calc R . . C14 C 0.5708(6) 0.0613(4) 0.6769(7) 0.085(3) Uani 1 1 d . . . H14 H 0.5850 0.0180 0.6733 0.102 Uiso 1 1 calc R . . C15 C 0.5923(6) 0.0958(4) 0.7526(7) 0.087(3) Uani 1 1 d . . . H15 H 0.6225 0.0755 0.7999 0.104 Uiso 1 1 calc R . . C16 C 0.5700(5) 0.1605(4) 0.7604(5) 0.065(2) Uani 1 1 d . . . H16 H 0.5854 0.1830 0.8123 0.078 Uiso 1 1 calc R . . C17 C 0.0094(4) 0.2570(3) 0.5744(4) 0.0414(14) Uani 1 1 d . . . C18 C 0.0435(4) 0.2294(3) 0.4959(4) 0.0369(13) Uani 1 1 d . . . C19 C 0.0997(4) 0.2669(3) 0.4456(4) 0.0428(14) Uani 1 1 d D . . H19A H 0.0776 0.3089 0.4281 0.051 Uiso 1 1 calc RD . . H19B H 0.1315 0.2450 0.3993 0.051 Uiso 1 1 calc RD . . C20 C 0.0303(4) 0.1588(3) 0.4760(4) 0.0478(15) Uani 1 1 d . . . H20A H 0.0427 0.1339 0.5297 0.057 Uiso 1 1 calc R . . H20B H -0.0312 0.1511 0.4565 0.057 Uiso 1 1 calc R . . C21 C -0.0183(4) 0.3264(3) 0.5772(4) 0.0447(15) Uani 1 1 d . . . C22 C -0.0056(5) 0.3623(3) 0.6551(5) 0.0594(19) Uani 1 1 d . . . H22 H 0.0224 0.3439 0.7052 0.071 Uiso 1 1 calc R . . C23 C -0.0345(5) 0.4251(4) 0.6576(6) 0.074(2) Uani 1 1 d . . . H23 H -0.0254 0.4493 0.7093 0.089 Uiso 1 1 calc R . . C24 C -0.0765(6) 0.4520(4) 0.5839(7) 0.084(3) Uani 1 1 d . . . H24 H -0.0963 0.4942 0.5862 0.100 Uiso 1 1 calc R . . C25 C -0.0896(5) 0.4180(4) 0.5083(6) 0.068(2) Uani 1 1 d . . . H25 H -0.1178 0.4369 0.4586 0.082 Uiso 1 1 calc R . . C26 C -0.0611(4) 0.3549(3) 0.5046(4) 0.0539(17) Uani 1 1 d . . . H26 H -0.0710 0.3315 0.4525 0.065 Uiso 1 1 calc R . . C27 C -0.0404(4) 0.2149(3) 0.6373(4) 0.0372(13) Uani 1 1 d . . . C28 C -0.1318(4) 0.2122(3) 0.6263(5) 0.0524(16) Uani 1 1 d . . . H28 H -0.1607 0.2367 0.5822 0.063 Uiso 1 1 calc R . . C29 C -0.1815(5) 0.1729(3) 0.6812(5) 0.0609(19) Uani 1 1 d . . . H29 H -0.2434 0.1714 0.6733 0.073 Uiso 1 1 calc R . . C30 C -0.1412(5) 0.1377(3) 0.7447(5) 0.061(2) Uani 1 1 d . . . H30 H -0.1752 0.1116 0.7807 0.073 Uiso 1 1 calc R . . C31 C -0.0498(5) 0.1393(3) 0.7575(5) 0.0618(19) Uani 1 1 d . . . H31 H -0.0217 0.1148 0.8020 0.074 Uiso 1 1 calc R . . C32 C -0.0003(4) 0.1781(3) 0.7031(4) 0.0505(16) Uani 1 1 d . . . H32 H 0.0616 0.1792 0.7114 0.061 Uiso 1 1 calc R . . C33 C 0.2376(4) 0.5226(3) 0.0913(4) 0.0450(15) Uani 1 1 d . . . C34 C 0.2556(4) 0.4906(3) 0.0084(4) 0.0449(15) Uani 1 1 d . . . C35 C 0.2265(4) 0.5208(3) -0.0703(4) 0.0526(17) Uani 1 1 d D . . H35A H 0.2279 0.4954 -0.1244 0.063 Uiso 1 1 calc RD . . H35B H 0.2460 0.5648 -0.0783 0.063 Uiso 1 1 calc RD . . C36 C 0.2903(5) 0.4215(3) 0.0079(5) 0.067(2) Uani 1 1 d . . . H36A H 0.3534 0.4212 0.0252 0.081 Uiso 1 1 calc R . . H36B H 0.2589 0.3964 0.0514 0.081 Uiso 1 1 calc R . . C37 C 0.2406(4) 0.5939(3) 0.0990(4) 0.0436(15) Uani 1 1 d . . . C38 C 0.3022(5) 0.6308(3) 0.0557(5) 0.0591(18) Uani 1 1 d . . . H38 H 0.3439 0.6107 0.0206 0.071 Uiso 1 1 calc R . . C39 C 0.3038(5) 0.6962(3) 0.0630(5) 0.065(2) Uani 1 1 d . . . H39 H 0.3448 0.7201 0.0318 0.078 Uiso 1 1 calc R . . C40 C 0.2441(5) 0.7266(4) 0.1171(5) 0.065(2) Uani 1 1 d . . . H40 H 0.2453 0.7710 0.1228 0.078 Uiso 1 1 calc R . . C41 C 0.1832(5) 0.6914(3) 0.1620(5) 0.0622(19) Uani 1 1 d . . . H41 H 0.1429 0.7117 0.1984 0.075 Uiso 1 1 calc R . . C42 C 0.1821(4) 0.6260(3) 0.1530(4) 0.0512(16) Uani 1 1 d . . . H42 H 0.1407 0.6023 0.1842 0.061 Uiso 1 1 calc R . . C43 C 0.2547(4) 0.4861(3) 0.1775(4) 0.0479(16) Uani 1 1 d . . . C44 C 0.1993(5) 0.4387(3) 0.2079(5) 0.068(2) Uani 1 1 d . . . H44 H 0.1468 0.4283 0.1761 0.082 Uiso 1 1 calc R . . C45 C 0.2225(6) 0.4065(4) 0.2869(6) 0.083(2) Uani 1 1 d . . . H45 H 0.1855 0.3743 0.3073 0.099 Uiso 1 1 calc R . . C46 C 0.2979(7) 0.4216(4) 0.3337(6) 0.085(3) Uani 1 1 d . . . H46 H 0.3138 0.3994 0.3857 0.102 Uiso 1 1 calc R . . C47 C 0.3495(7) 0.4688(5) 0.3050(7) 0.115(4) Uani 1 1 d . . . H47 H 0.3999 0.4803 0.3395 0.138 Uiso 1 1 calc R . . C48 C 0.3315(6) 0.5012(4) 0.2268(6) 0.093(3) Uani 1 1 d . . . H48 H 0.3703 0.5327 0.2074 0.111 Uiso 1 1 calc R . . C49 C 0.2759(10) 0.4262(9) 0.6608(11) 0.253(9) Uiso 1 1 d D . . H49 H 0.2879 0.3842 0.6880 0.304 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 0.0348(3) 0.0512(3) 0.0356(3) -0.0020(2) 0.0063(2) -0.0048(2) Pd2 0.0348(3) 0.0492(3) 0.0347(3) -0.0029(2) 0.0062(2) -0.0054(2) Pd3 0.0363(3) 0.0396(3) 0.0394(3) -0.0027(2) 0.0009(2) 0.00167(19) Cl1 0.0405(9) 0.0900(13) 0.0371(9) -0.0042(8) 0.0089(7) -0.0063(8) Cl2 0.0369(8) 0.0933(13) 0.0375(9) -0.0102(8) 0.0079(7) -0.0088(8) Cl3 0.0421(8) 0.0574(10) 0.0374(8) -0.0009(7) -0.0001(7) 0.0006(7) O1 0.090(4) 0.107(5) 0.087(4) -0.047(4) 0.026(3) -0.015(3) O2 0.078(3) 0.053(3) 0.061(3) -0.014(2) 0.022(3) -0.003(2) O3 0.066(3) 0.072(4) 0.079(4) -0.020(3) 0.017(3) 0.011(3) C1 0.033(3) 0.049(4) 0.037(3) -0.002(3) 0.003(3) 0.001(3) C2 0.038(3) 0.062(4) 0.040(4) 0.000(3) -0.005(3) -0.007(3) C3 0.046(4) 0.080(5) 0.032(4) 0.007(3) 0.001(3) 0.000(3) C4 0.047(4) 0.070(5) 0.060(5) -0.013(4) 0.004(3) -0.004(3) C5 0.045(4) 0.044(4) 0.038(4) -0.003(3) 0.007(3) -0.004(3) C6 0.044(4) 0.066(5) 0.078(5) 0.013(4) 0.006(4) 0.001(3) C7 0.040(4) 0.082(6) 0.098(7) 0.013(5) 0.017(4) -0.010(4) C8 0.060(5) 0.084(6) 0.078(6) 0.012(5) 0.017(4) -0.026(4) C9 0.084(6) 0.117(7) 0.074(6) 0.044(5) -0.004(5) -0.043(5) C10 0.056(5) 0.103(6) 0.062(5) 0.025(5) -0.008(4) -0.029(4) C11 0.041(4) 0.050(4) 0.059(4) 0.009(3) 0.014(3) -0.002(3) C12 0.048(4) 0.062(5) 0.056(4) -0.007(4) 0.007(3) 0.001(3) C13 0.056(5) 0.067(5) 0.093(7) -0.015(5) 0.019(4) 0.002(4) C14 0.081(6) 0.059(5) 0.117(8) -0.003(5) 0.032(6) 0.011(4) C15 0.078(6) 0.078(6) 0.106(8) 0.039(6) 0.012(5) 0.023(5) C16 0.059(5) 0.067(5) 0.069(5) 0.010(4) 0.006(4) 0.002(4) C17 0.032(3) 0.050(4) 0.042(4) -0.001(3) -0.001(3) -0.002(3) C18 0.033(3) 0.046(3) 0.032(3) 0.001(3) 0.002(2) -0.001(3) C19 0.045(4) 0.052(4) 0.032(3) 0.003(3) 0.003(3) 0.001(3) C20 0.045(4) 0.054(4) 0.045(4) -0.006(3) 0.002(3) -0.001(3) C21 0.045(4) 0.048(4) 0.042(4) -0.004(3) 0.013(3) -0.001(3) C22 0.062(5) 0.066(5) 0.051(4) -0.016(4) 0.007(3) -0.002(4) C23 0.092(6) 0.063(5) 0.069(6) -0.026(4) 0.028(5) -0.008(4) C24 0.105(7) 0.047(5) 0.100(7) -0.004(5) 0.027(6) 0.014(4) C25 0.078(5) 0.055(5) 0.073(6) 0.010(4) 0.009(4) 0.014(4) C26 0.060(4) 0.057(4) 0.046(4) -0.005(3) 0.008(3) 0.002(3) C27 0.039(3) 0.038(3) 0.035(3) -0.003(3) 0.009(3) -0.003(3) C28 0.037(3) 0.059(4) 0.061(4) -0.002(3) 0.000(3) -0.005(3) C29 0.044(4) 0.062(5) 0.078(6) -0.014(4) 0.015(4) -0.015(3) C30 0.074(5) 0.048(4) 0.064(5) -0.001(4) 0.030(4) -0.019(4) C31 0.077(5) 0.059(5) 0.050(4) 0.009(3) 0.010(4) -0.006(4) C32 0.042(4) 0.063(4) 0.047(4) 0.005(3) 0.005(3) -0.007(3) C33 0.030(3) 0.049(4) 0.056(4) -0.007(3) -0.001(3) -0.002(3) C34 0.032(3) 0.054(4) 0.049(4) -0.006(3) 0.003(3) 0.000(3) C35 0.048(4) 0.062(4) 0.049(4) -0.004(3) 0.010(3) -0.003(3) C36 0.054(4) 0.071(5) 0.078(6) -0.019(4) 0.000(4) 0.023(4) C37 0.038(3) 0.049(4) 0.044(4) 0.000(3) -0.006(3) -0.005(3) C38 0.053(4) 0.062(5) 0.063(5) -0.006(4) 0.009(4) -0.010(3) C39 0.067(5) 0.059(5) 0.068(5) 0.010(4) -0.009(4) -0.026(4) C40 0.080(6) 0.044(4) 0.070(6) -0.004(4) -0.025(5) -0.008(4) C41 0.069(5) 0.053(4) 0.063(5) -0.021(4) -0.008(4) 0.001(4) C42 0.048(4) 0.055(4) 0.050(4) -0.004(3) 0.002(3) -0.005(3) C43 0.050(4) 0.042(4) 0.051(4) -0.003(3) -0.004(3) 0.005(3) C44 0.066(5) 0.070(5) 0.067(5) 0.018(4) -0.021(4) -0.015(4) C45 0.094(7) 0.078(6) 0.076(6) 0.026(5) -0.007(5) -0.006(5) C46 0.113(8) 0.080(6) 0.060(6) 0.007(5) -0.029(5) 0.011(5) C47 0.112(8) 0.123(9) 0.104(8) 0.026(7) -0.069(7) -0.023(7) C48 0.093(7) 0.096(7) 0.086(7) 0.030(5) -0.047(5) -0.028(5) _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 2.110(6) . ? Pd1 C3 2.113(6) . ? Pd1 C1 2.139(6) . ? Pd1 Cl1 2.4080(16) . ? Pd1 Cl2 2.4121(17) . ? Pd2 C18 2.095(6) . ? Pd2 C19 2.100(6) . ? Pd2 C17 2.158(6) . ? Pd2 Cl2 2.3993(16) . ? Pd2 Cl1 2.4062(17) . ? Pd3 C35 2.086(6) . ? Pd3 C34 2.110(6) . ? Pd3 C33 2.177(6) . ? Pd3 Cl3 2.4180(16) 3_565 ? Pd3 Cl3 2.4192(15) . ? Cl3 Pd3 2.4180(16) 3_565 ? Cl4 C49 1.728(14) . ? Cl5 C49 1.938(15) . ? Cl6 C49 1.655(14) . ? O1 C4 1.367(7) . ? O1 H1 0.8200 . ? O2 C20 1.399(7) . ? O2 H2 0.8200 . ? O3 C36 1.433(8) . ? O3 H3 0.8200 . ? C1 C2 1.421(8) . ? C1 C5 1.494(8) . ? C1 C11 1.508(8) . ? C2 C3 1.401(8) . ? C2 C4 1.523(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.372(9) . ? C5 C6 1.376(8) . ? C6 C7 1.373(9) . ? C6 H6 0.9300 . ? C7 C8 1.352(10) . ? C7 H7 0.9300 . ? C8 C9 1.354(11) . ? C8 H8 0.9300 . ? C9 C10 1.399(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.384(9) . ? C11 C12 1.402(9) . ? C12 C13 1.385(10) . ? C12 H12 0.9300 . ? C13 C14 1.366(12) . ? C13 H13 0.9300 . ? C14 C15 1.371(12) . ? C14 H14 0.9300 . ? C15 C16 1.396(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.422(8) . ? C17 C21 1.505(8) . ? C17 C27 1.506(8) . ? C18 C19 1.390(8) . ? C18 C20 1.512(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.378(9) . ? C21 C22 1.394(9) . ? C22 C23 1.381(10) . ? C22 H22 0.9300 . ? C23 C24 1.371(11) . ? C23 H23 0.9300 . ? C24 C25 1.345(11) . ? C24 H24 0.9300 . ? C25 C26 1.383(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.372(8) . ? C27 C28 1.373(8) . ? C28 C29 1.395(9) . ? C28 H28 0.9300 . ? C29 C30 1.330(10) . ? C29 H29 0.9300 . ? C30 C31 1.375(10) . ? C30 H30 0.9300 . ? C31 C32 1.381(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.444(9) . ? C33 C37 1.491(8) . ? C33 C43 1.515(9) . ? C34 C35 1.395(9) . ? C34 C36 1.531(9) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.381(8) . ? C37 C42 1.387(8) . ? C38 C39 1.367(9) . ? C38 H38 0.9300 . ? C39 C40 1.381(9) . ? C39 H39 0.9300 . ? C40 C41 1.366(9) . ? C40 H40 0.9300 . ? C41 C42 1.369(9) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.377(9) . ? C43 C48 1.380(10) . ? C44 C45 1.394(10) . ? C44 H44 0.9300 . ? C45 C46 1.344(11) . ? C45 H45 0.9300 . ? C46 C47 1.331(12) . ? C46 H46 0.9300 . ? C47 C48 1.372(12) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 H49 0.9800 . ? 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 C3 38.8(2) . . ? C2 Pd1 C1 39.1(2) . . ? C3 Pd1 C1 69.1(2) . . ? C2 Pd1 Cl1 129.76(17) . . ? C3 Pd1 Cl1 98.68(18) . . ? C1 Pd1 Cl1 167.78(17) . . ? C2 Pd1 Cl2 140.53(17) . . ? C3 Pd1 Cl2 171.0(2) . . ? C1 Pd1 Cl2 106.13(16) . . ? Cl1 Pd1 Cl2 86.08(5) . . ? C18 Pd2 C19 38.7(2) . . ? C18 Pd2 C17 39.0(2) . . ? C19 Pd2 C17 68.8(2) . . ? C18 Pd2 Cl2 129.55(15) . . ? C19 Pd2 Cl2 97.80(16) . . ? C17 Pd2 Cl2 166.56(17) . . ? C18 Pd2 Cl1 141.55(16) . . ? C19 Pd2 Cl1 169.48(17) . . ? C17 Pd2 Cl1 106.65(17) . . ? Cl2 Pd2 Cl1 86.40(6) . . ? C35 Pd3 C34 38.8(2) . . ? C35 Pd3 C33 69.3(2) . . ? C34 Pd3 C33 39.3(2) . . ? C35 Pd3 Cl3 96.86(19) . 3_565 ? C34 Pd3 Cl3 130.08(18) . 3_565 ? C33 Pd3 Cl3 165.55(17) . 3_565 ? C35 Pd3 Cl3 174.71(19) . . ? C34 Pd3 Cl3 138.77(18) . . ? C33 Pd3 Cl3 106.32(17) . . ? Cl3 Pd3 Cl3 87.31(5) 3_565 . ? Pd2 Cl1 Pd1 93.58(5) . . ? Pd2 Cl2 Pd1 93.65(5) . . ? Pd3 Cl3 Pd3 92.69(5) 3_565 . ? C4 O1 H1 109.5 . . ? C20 O2 H2 109.5 . . ? C36 O3 H3 109.5 . . ? C2 C1 C5 119.0(5) . . ? C2 C1 C11 120.7(5) . . ? C5 C1 C11 112.9(5) . . ? C2 C1 Pd1 69.3(3) . . ? C5 C1 Pd1 122.5(4) . . ? C11 C1 Pd1 104.9(4) . . ? C3 C2 C1 117.5(6) . . ? C3 C2 C4 121.3(6) . . ? C1 C2 C4 120.5(5) . . ? C3 C2 Pd1 70.7(4) . . ? C1 C2 Pd1 71.6(3) . . ? C4 C2 Pd1 119.8(4) . . ? C2 C3 Pd1 70.5(4) . . ? C2 C3 H3A 116.6 . . ? Pd1 C3 H3A 116.6 . . ? C2 C3 H3B 116.6 . . ? Pd1 C3 H3B 116.6 . . ? H3A C3 H3B 113.6 . . ? O1 C4 C2 115.1(6) . . ? O1 C4 H4A 108.5 . . ? C2 C4 H4A 108.5 . . ? O1 C4 H4B 108.5 . . ? C2 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C10 C5 C6 117.0(6) . . ? C10 C5 C1 123.8(6) . . ? C6 C5 C1 119.2(6) . . ? C7 C6 C5 122.3(7) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.8 . . ? C8 C7 C6 119.4(7) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.7(7) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 119.5(8) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C5 C10 C9 121.0(7) . . ? C5 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C16 C11 C12 118.5(7) . . ? C16 C11 C1 120.5(6) . . ? C12 C11 C1 120.9(6) . . ? C13 C12 C11 120.2(7) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C14 C13 C12 121.3(8) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 118.6(8) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C16 121.8(9) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C11 C16 C15 119.5(8) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C21 121.4(5) . . ? C18 C17 C27 118.9(5) . . ? C21 C17 C27 113.6(5) . . ? C18 C17 Pd2 68.1(3) . . ? C21 C17 Pd2 105.4(4) . . ? C27 C17 Pd2 121.0(4) . . ? C19 C18 C17 117.6(5) . . ? C19 C18 C20 121.1(5) . . ? C17 C18 C20 120.6(5) . . ? C19 C18 Pd2 70.8(3) . . ? C17 C18 Pd2 72.9(3) . . ? C20 C18 Pd2 119.1(4) . . ? C18 C19 Pd2 70.4(3) . . ? C18 C19 H19A 116.6 . . ? Pd2 C19 H19A 116.6 . . ? C18 C19 H19B 116.6 . . ? Pd2 C19 H19B 116.6 . . ? H19A C19 H19B 113.6 . . ? O2 C20 C18 110.1(5) . . ? O2 C20 H20A 109.6 . . ? C18 C20 H20A 109.6 . . ? O2 C20 H20B 109.6 . . ? C18 C20 H20B 109.6 . . ? H20A C20 H20B 108.2 . . ? C26 C21 C22 118.5(6) . . ? C26 C21 C17 120.8(6) . . ? C22 C21 C17 120.6(6) . . ? C23 C22 C21 119.9(7) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.0(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.9(7) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.9(8) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.9(7) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C32 C27 C28 118.1(6) . . ? C32 C27 C17 124.4(5) . . ? C28 C27 C17 117.5(5) . . ? C27 C28 C29 120.2(6) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.6(7) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.6(6) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 118.9(7) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C27 C32 C31 121.5(6) . . ? C27 C32 H32 119.2 . . ? C31 C32 H32 119.3 . . ? C34 C33 C37 121.4(6) . . ? C34 C33 C43 118.2(5) . . ? C37 C33 C43 115.5(5) . . ? C34 C33 Pd3 67.8(3) . . ? C37 C33 Pd3 102.2(4) . . ? C43 C33 Pd3 121.4(4) . . ? C35 C34 C33 117.3(6) . . ? C35 C34 C36 121.1(6) . . ? C33 C34 C36 120.8(6) . . ? C35 C34 Pd3 69.7(3) . . ? C33 C34 Pd3 72.8(3) . . ? C36 C34 Pd3 119.3(4) . . ? C34 C35 Pd3 71.5(3) . . ? C34 C35 H35A 116.4 . . ? Pd3 C35 H35A 116.4 . . ? C34 C35 H35B 116.4 . . ? Pd3 C35 H35B 116.4 . . ? H35A C35 H35B 113.4 . . ? O3 C36 C34 111.6(6) . . ? O3 C36 H36A 109.3 . . ? C34 C36 H36A 109.3 . . ? O3 C36 H36B 109.3 . . ? C34 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C42 116.9(6) . . ? C38 C37 C33 122.5(6) . . ? C42 C37 C33 120.5(5) . . ? C39 C38 C37 121.8(7) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 119.6(7) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 120.0(7) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 119.5(7) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C41 C42 C37 122.1(6) . . ? C41 C42 H42 119.0 . . ? C37 C42 H42 119.0 . . ? C44 C43 C48 119.1(7) . . ? C44 C43 C33 123.9(6) . . ? C48 C43 C33 117.0(6) . . ? C43 C44 C45 119.5(7) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 120.7(8) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C47 C46 C45 119.3(8) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 122.8(9) . . ? C46 C47 H47 118.6 . . ? C48 C47 H47 118.6 . . ? C47 C48 C43 118.6(8) . . ? C47 C48 H48 120.7 . . ? C43 C48 H48 120.7 . . ? Cl6 C49 Cl4 120.3(11) . . ? Cl6 C49 Cl5 78.5(8) . . ? Cl4 C49 Cl5 80.7(8) . . ? Cl6 C49 H49 119.5 . . ? Cl4 C49 H49 119.5 . . ? Cl5 C49 H49 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Pd2 Cl1 Pd1 157.2(2) . . . . ? C19 Pd2 Cl1 Pd1 -118.0(9) . . . . ? C17 Pd2 Cl1 Pd1 179.19(16) . . . . ? Cl2 Pd2 Cl1 Pd1 -4.08(7) . . . . ? C2 Pd1 Cl1 Pd2 165.8(2) . . . . ? C3 Pd1 Cl1 Pd2 -168.3(2) . . . . ? C1 Pd1 Cl1 Pd2 -172.6(8) . . . . ? Cl2 Pd1 Cl1 Pd2 4.06(7) . . . . ? C18 Pd2 Cl2 Pd1 -160.9(2) . . . . ? C19 Pd2 Cl2 Pd1 174.37(17) . . . . ? C17 Pd2 Cl2 Pd1 170.5(7) . . . . ? Cl1 Pd2 Cl2 Pd1 4.07(7) . . . . ? C2 Pd1 Cl2 Pd2 -161.8(3) . . . . ? C3 Pd1 Cl2 Pd2 118.3(11) . . . . ? C1 Pd1 Cl2 Pd2 175.19(16) . . . . ? Cl1 Pd1 Cl2 Pd2 -4.07(7) . . . . ? C35 Pd3 Cl3 Pd3 142(2) . . . 3_565 ? C34 Pd3 Cl3 Pd3 -157.6(2) . . . 3_565 ? C33 Pd3 Cl3 Pd3 175.13(17) . . . 3_565 ? Cl3 Pd3 Cl3 Pd3 0.0 3_565 . . 3_565 ? C3 Pd1 C1 C2 -31.3(4) . . . . ? Cl1 Pd1 C1 C2 -26.7(10) . . . . ? Cl2 Pd1 C1 C2 156.7(3) . . . . ? C2 Pd1 C1 C5 -112.0(6) . . . . ? C3 Pd1 C1 C5 -143.3(5) . . . . ? Cl1 Pd1 C1 C5 -138.7(6) . . . . ? Cl2 Pd1 C1 C5 44.7(5) . . . . ? C2 Pd1 C1 C11 117.7(6) . . . . ? C3 Pd1 C1 C11 86.4(4) . . . . ? Cl1 Pd1 C1 C11 90.9(8) . . . . ? Cl2 Pd1 C1 C11 -85.6(4) . . . . ? C5 C1 C2 C3 172.2(6) . . . . ? C11 C1 C2 C3 -39.9(8) . . . . ? Pd1 C1 C2 C3 55.6(5) . . . . ? C5 C1 C2 C4 2.3(9) . . . . ? C11 C1 C2 C4 150.2(6) . . . . ? Pd1 C1 C2 C4 -114.3(6) . . . . ? C5 C1 C2 Pd1 116.6(5) . . . . ? C11 C1 C2 Pd1 -95.5(5) . . . . ? C1 Pd1 C2 C3 -129.1(6) . . . . ? Cl1 Pd1 C2 C3 43.7(5) . . . . ? Cl2 Pd1 C2 C3 -165.8(3) . . . . ? C3 Pd1 C2 C1 129.1(6) . . . . ? Cl1 Pd1 C2 C1 172.9(3) . . . . ? Cl2 Pd1 C2 C1 -36.6(5) . . . . ? C3 Pd1 C2 C4 -115.7(7) . . . . ? C1 Pd1 C2 C4 115.2(6) . . . . ? Cl1 Pd1 C2 C4 -71.9(5) . . . . ? Cl2 Pd1 C2 C4 78.6(5) . . . . ? C1 C2 C3 Pd1 -56.0(5) . . . . ? C4 C2 C3 Pd1 113.8(6) . . . . ? C1 Pd1 C3 C2 31.5(4) . . . . ? Cl1 Pd1 C3 C2 -147.5(4) . . . . ? Cl2 Pd1 C3 C2 91.1(12) . . . . ? C3 C2 C4 O1 6.4(9) . . . . ? C1 C2 C4 O1 176.0(6) . . . . ? Pd1 C2 C4 O1 90.8(7) . . . . ? C2 C1 C5 C10 -97.3(8) . . . . ? C11 C1 C5 C10 112.4(7) . . . . ? Pd1 C1 C5 C10 -14.5(9) . . . . ? C2 C1 C5 C6 82.0(7) . . . . ? C11 C1 C5 C6 -68.3(7) . . . . ? Pd1 C1 C5 C6 164.8(5) . . . . ? C10 C5 C6 C7 2.6(10) . . . . ? C1 C5 C6 C7 -176.7(7) . . . . ? C5 C6 C7 C8 -2.3(12) . . . . ? C6 C7 C8 C9 2.3(13) . . . . ? C7 C8 C9 C10 -2.6(14) . . . . ? C6 C5 C10 C9 -2.9(12) . . . . ? C1 C5 C10 C9 176.4(7) . . . . ? C8 C9 C10 C5 2.9(14) . . . . ? C2 C1 C11 C16 -40.0(8) . . . . ? C5 C1 C11 C16 109.7(7) . . . . ? Pd1 C1 C11 C16 -114.5(6) . . . . ? C2 C1 C11 C12 143.7(6) . . . . ? C5 C1 C11 C12 -66.6(7) . . . . ? Pd1 C1 C11 C12 69.2(6) . . . . ? C16 C11 C12 C13 2.1(9) . . . . ? C1 C11 C12 C13 178.5(6) . . . . ? C11 C12 C13 C14 -0.5(11) . . . . ? C12 C13 C14 C15 -1.3(12) . . . . ? C13 C14 C15 C16 1.4(13) . . . . ? C12 C11 C16 C15 -2.0(10) . . . . ? C1 C11 C16 C15 -178.4(6) . . . . ? C14 C15 C16 C11 0.2(12) . . . . ? C19 Pd2 C17 C18 31.7(3) . . . . ? Cl2 Pd2 C17 C18 35.9(9) . . . . ? Cl1 Pd2 C17 C18 -158.3(3) . . . . ? C18 Pd2 C17 C21 -118.1(6) . . . . ? C19 Pd2 C17 C21 -86.4(4) . . . . ? Cl2 Pd2 C17 C21 -82.2(8) . . . . ? Cl1 Pd2 C17 C21 83.6(4) . . . . ? C18 Pd2 C17 C27 111.4(6) . . . . ? C19 Pd2 C17 C27 143.2(5) . . . . ? Cl2 Pd2 C17 C27 147.3(5) . . . . ? Cl1 Pd2 C17 C27 -46.9(5) . . . . ? C21 C17 C18 C19 38.5(8) . . . . ? C27 C17 C18 C19 -171.1(5) . . . . ? Pd2 C17 C18 C19 -56.7(5) . . . . ? C21 C17 C18 C20 -150.7(6) . . . . ? C27 C17 C18 C20 -0.2(8) . . . . ? Pd2 C17 C18 C20 114.1(5) . . . . ? C21 C17 C18 Pd2 95.2(5) . . . . ? C27 C17 C18 Pd2 -114.3(5) . . . . ? C17 Pd2 C18 C19 128.4(5) . . . . ? Cl2 Pd2 C18 C19 -41.5(4) . . . . ? Cl1 Pd2 C18 C19 163.1(3) . . . . ? C19 Pd2 C18 C17 -128.4(5) . . . . ? Cl2 Pd2 C18 C17 -169.8(3) . . . . ? Cl1 Pd2 C18 C17 34.7(5) . . . . ? C19 Pd2 C18 C20 115.6(6) . . . . ? C17 Pd2 C18 C20 -116.0(6) . . . . ? Cl2 Pd2 C18 C20 74.1(5) . . . . ? Cl1 Pd2 C18 C20 -81.3(5) . . . . ? C17 C18 C19 Pd2 57.8(5) . . . . ? C20 C18 C19 Pd2 -113.0(5) . . . . ? C17 Pd2 C19 C18 -32.0(3) . . . . ? Cl2 Pd2 C19 C18 149.0(3) . . . . ? Cl1 Pd2 C19 C18 -98.0(9) . . . . ? C19 C18 C20 O2 5.5(8) . . . . ? C17 C18 C20 O2 -165.0(5) . . . . ? Pd2 C18 C20 O2 -78.6(6) . . . . ? C18 C17 C21 C26 38.2(8) . . . . ? C27 C17 C21 C26 -113.7(6) . . . . ? Pd2 C17 C21 C26 111.7(6) . . . . ? C18 C17 C21 C22 -145.2(6) . . . . ? C27 C17 C21 C22 62.8(7) . . . . ? Pd2 C17 C21 C22 -71.8(6) . . . . ? C26 C21 C22 C23 -0.9(10) . . . . ? C17 C21 C22 C23 -177.5(6) . . . . ? C21 C22 C23 C24 0.7(11) . . . . ? C22 C23 C24 C25 -0.5(13) . . . . ? C23 C24 C25 C26 0.5(13) . . . . ? C22 C21 C26 C25 1.0(10) . . . . ? C17 C21 C26 C25 177.6(6) . . . . ? C24 C25 C26 C21 -0.8(11) . . . . ? C18 C17 C27 C32 85.0(8) . . . . ? C21 C17 C27 C32 -122.3(6) . . . . ? Pd2 C17 C27 C32 4.5(8) . . . . ? C18 C17 C27 C28 -93.5(7) . . . . ? C21 C17 C27 C28 59.2(7) . . . . ? Pd2 C17 C27 C28 -174.0(4) . . . . ? C32 C27 C28 C29 -0.1(9) . . . . ? C17 C27 C28 C29 178.6(6) . . . . ? C27 C28 C29 C30 0.1(10) . . . . ? C28 C29 C30 C31 0.1(11) . . . . ? C29 C30 C31 C32 -0.2(10) . . . . ? C28 C27 C32 C31 -0.1(9) . . . . ? C17 C27 C32 C31 -178.6(6) . . . . ? C30 C31 C32 C27 0.3(10) . . . . ? C35 Pd3 C33 C34 -31.5(4) . . . . ? Cl3 Pd3 C33 C34 -48.4(8) 3_565 . . . ? Cl3 Pd3 C33 C34 151.5(3) . . . . ? C35 Pd3 C33 C37 87.6(4) . . . . ? C34 Pd3 C33 C37 119.2(6) . . . . ? Cl3 Pd3 C33 C37 70.8(8) 3_565 . . . ? Cl3 Pd3 C33 C37 -89.3(4) . . . . ? C35 Pd3 C33 C43 -141.9(5) . . . . ? C34 Pd3 C33 C43 -110.4(6) . . . . ? Cl3 Pd3 C33 C43 -158.8(4) 3_565 . . . ? Cl3 Pd3 C33 C43 41.1(5) . . . . ? C37 C33 C34 C35 -35.7(8) . . . . ? C43 C33 C34 C35 170.2(6) . . . . ? Pd3 C33 C34 C35 55.4(5) . . . . ? C37 C33 C34 C36 154.5(6) . . . . ? C43 C33 C34 C36 0.4(8) . . . . ? Pd3 C33 C34 C36 -114.4(6) . . . . ? C37 C33 C34 Pd3 -91.1(5) . . . . ? C43 C33 C34 Pd3 114.8(5) . . . . ? C33 Pd3 C34 C35 -128.7(6) . . . . ? Cl3 Pd3 C34 C35 37.2(5) 3_565 . . . ? Cl3 Pd3 C34 C35 -172.7(3) . . . . ? C35 Pd3 C34 C33 128.7(6) . . . . ? Cl3 Pd3 C34 C33 165.9(3) 3_565 . . . ? Cl3 Pd3 C34 C33 -44.0(5) . . . . ? C35 Pd3 C34 C36 -115.1(7) . . . . ? C33 Pd3 C34 C36 116.2(7) . . . . ? Cl3 Pd3 C34 C36 -77.9(5) 3_565 . . . ? Cl3 Pd3 C34 C36 72.2(6) . . . . ? C33 C34 C35 Pd3 -57.0(5) . . . . ? C36 C34 C35 Pd3 112.7(6) . . . . ? C33 Pd3 C35 C34 31.9(4) . . . . ? Cl3 Pd3 C35 C34 -152.2(4) 3_565 . . . ? Cl3 Pd3 C35 C34 66(2) . . . . ? C35 C34 C36 O3 -7.0(9) . . . . ? C33 C34 C36 O3 162.3(6) . . . . ? Pd3 C34 C36 O3 75.7(7) . . . . ? C34 C33 C37 C38 -36.9(9) . . . . ? C43 C33 C37 C38 117.8(7) . . . . ? Pd3 C33 C37 C38 -108.2(6) . . . . ? C34 C33 C37 C42 145.0(6) . . . . ? C43 C33 C37 C42 -60.3(8) . . . . ? Pd3 C33 C37 C42 73.7(6) . . . . ? C42 C37 C38 C39 -2.2(10) . . . . ? C33 C37 C38 C39 179.6(6) . . . . ? C37 C38 C39 C40 1.9(11) . . . . ? C38 C39 C40 C41 -0.8(11) . . . . ? C39 C40 C41 C42 0.1(11) . . . . ? C40 C41 C42 C37 -0.5(10) . . . . ? C38 C37 C42 C41 1.5(10) . . . . ? C33 C37 C42 C41 179.7(6) . . . . ? C34 C33 C43 C44 -76.1(8) . . . . ? C37 C33 C43 C44 128.4(7) . . . . ? Pd3 C33 C43 C44 3.9(9) . . . . ? C34 C33 C43 C48 102.9(8) . . . . ? C37 C33 C43 C48 -52.7(8) . . . . ? Pd3 C33 C43 C48 -177.2(6) . . . . ? C48 C43 C44 C45 -1.0(12) . . . . ? C33 C43 C44 C45 178.0(7) . . . . ? C43 C44 C45 C46 0.6(13) . . . . ? C44 C45 C46 C47 1.4(15) . . . . ? C45 C46 C47 C48 -3.1(18) . . . . ? C46 C47 C48 C43 2.7(18) . . . . ? C44 C43 C48 C47 -0.6(14) . . . . ? C33 C43 C48 C47 -179.6(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 2.19 2.924(7) 149.1 4_565 O2 H2 Cl3 0.82 2.49 3.200(5) 146.0 2_545 O1 H1 O3 0.82 2.03 2.776(7) 150.4 1_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.035 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.131 data_cd27222 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 646598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H50 Cl2 N2 Pd' _chemical_formula_weight 772.15 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.1371(13) _cell_length_b 26.1371(13) _cell_length_c 23.7475(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16223.1(16) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4479 _cell_measurement_theta_min 4.408 _cell_measurement_theta_max 47.625 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.501 _exptl_crystal_size_mid 0.234 _exptl_crystal_size_min 0.196 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6432 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81271 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs-Bruker _exptl_special_details ; The Rint is higher than 0.1 because the refraction of crystal is rather weak. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45818 _diffrn_reflns_av_R_equivalents 0.1242 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 26.49 _reflns_number_total 8412 _reflns_number_gt 3618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8412 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _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 Pd Pd 0.775509(16) 0.805685(15) 1.016153(17) 0.06402(19) Uani 1 1 d . . . Cl1 Cl 0.76367(6) 0.86638(6) 1.08833(6) 0.0879(5) Uani 1 1 d . . . Cl2 Cl 0.83386(10) 0.63766(8) 1.02717(13) 0.1658(10) Uani 1 1 d . . . N1 N 0.69706(17) 0.87223(16) 0.95315(18) 0.0672(12) Uani 1 1 d . . . N2 N 0.66979(17) 0.79652(16) 0.96294(19) 0.0680(12) Uani 1 1 d . . . C1 C 0.8009(2) 0.7506(2) 0.9599(3) 0.0812(17) Uani 1 1 d . . . H1A H 0.7751 0.7279 0.9444 0.097 Uiso 1 1 calc R . . H1B H 0.8261 0.7616 0.9324 0.097 Uiso 1 1 calc R . . C2 C 0.8197(2) 0.7382(2) 1.0139(2) 0.0699(15) Uani 1 1 d . . . C3 C 0.7969(2) 0.6920(2) 1.0429(3) 0.0890(19) Uani 1 1 d . . . H3A H 0.7620 0.6868 1.0303 0.107 Uiso 1 1 calc R . . H3B H 0.7964 0.6975 1.0833 0.107 Uiso 1 1 calc R . . C4 C 0.8516(2) 0.7728(2) 1.0428(3) 0.0712(15) Uani 1 1 d . . . C5 C 0.7111(2) 0.82666(19) 0.9746(2) 0.0608(14) Uani 1 1 d . . . C6 C 0.6491(2) 0.8710(2) 0.9288(2) 0.0789(17) Uani 1 1 d . . . H6 H 0.6322 0.8981 0.9114 0.095 Uiso 1 1 calc R . . C7 C 0.6319(2) 0.8237(2) 0.9351(3) 0.0812(17) Uani 1 1 d . . . H7 H 0.6004 0.8111 0.9231 0.097 Uiso 1 1 calc R . . C8 C 0.7282(3) 0.9173(2) 0.9521(3) 0.0799(18) Uani 1 1 d . . . C9 C 0.7145(3) 0.9582(2) 0.9877(3) 0.093(2) Uani 1 1 d . . . C10 C 0.7445(4) 1.0015(3) 0.9832(4) 0.141(4) Uani 1 1 d . . . H10 H 0.7366 1.0301 1.0048 0.169 Uiso 1 1 calc R . . C11 C 0.7863(4) 1.0032(4) 0.9470(5) 0.147(5) Uani 1 1 d . . . H11 H 0.8063 1.0326 0.9458 0.177 Uiso 1 1 calc R . . C12 C 0.7988(3) 0.9624(4) 0.9128(4) 0.135(3) Uani 1 1 d . . . H12 H 0.8265 0.9647 0.8883 0.163 Uiso 1 1 calc R . . C13 C 0.7702(3) 0.9184(3) 0.9150(3) 0.097(2) Uani 1 1 d . . . C14 C 0.7810(3) 0.8758(3) 0.8740(3) 0.112(2) Uani 1 1 d . . . H14 H 0.7685 0.8443 0.8916 0.134 Uiso 1 1 calc R . . C15 C 0.7517(4) 0.8817(4) 0.8201(4) 0.179(4) Uani 1 1 d . . . H15A H 0.7617 0.9129 0.8018 0.268 Uiso 1 1 calc R . . H15B H 0.7157 0.8828 0.8282 0.268 Uiso 1 1 calc R . . H15C H 0.7588 0.8532 0.7958 0.268 Uiso 1 1 calc R . . C16 C 0.8369(4) 0.8666(4) 0.8606(4) 0.181(4) Uani 1 1 d . . . H16A H 0.8401 0.8367 0.8375 0.271 Uiso 1 1 calc R . . H16B H 0.8556 0.8618 0.8950 0.271 Uiso 1 1 calc R . . H16C H 0.8504 0.8957 0.8408 0.271 Uiso 1 1 calc R . . C17 C 0.6695(3) 0.9561(3) 1.0266(3) 0.107(2) Uani 1 1 d . . . H17 H 0.6595 0.9202 1.0309 0.129 Uiso 1 1 calc R . . C18 C 0.6824(3) 0.9771(3) 1.0848(3) 0.150(4) Uani 1 1 d . . . H18A H 0.7089 0.9567 1.1015 0.225 Uiso 1 1 calc R . . H18B H 0.6524 0.9759 1.1082 0.225 Uiso 1 1 calc R . . H18C H 0.6938 1.0119 1.0814 0.225 Uiso 1 1 calc R . . C19 C 0.6231(3) 0.9856(3) 1.0026(3) 0.141(3) Uani 1 1 d . . . H19A H 0.6325 1.0207 0.9964 0.211 Uiso 1 1 calc R . . H19B H 0.5953 0.9841 1.0290 0.211 Uiso 1 1 calc R . . H19C H 0.6127 0.9704 0.9677 0.211 Uiso 1 1 calc R . . C20 C 0.6651(2) 0.7429(2) 0.9792(3) 0.0804(18) Uani 1 1 d . . . C21 C 0.6705(2) 0.7065(2) 0.9355(3) 0.096(2) Uani 1 1 d . . . C22 C 0.6657(3) 0.6555(3) 0.9523(5) 0.128(3) Uani 1 1 d . . . H22 H 0.6689 0.6296 0.9256 0.154 Uiso 1 1 calc R . . C23 C 0.6562(3) 0.6428(3) 1.0075(5) 0.143(4) Uani 1 1 d . . . H23 H 0.6531 0.6086 1.0178 0.172 Uiso 1 1 calc R . . C24 C 0.6513(3) 0.6799(3) 1.0472(4) 0.124(3) Uani 1 1 d . . . H24 H 0.6453 0.6706 1.0844 0.148 Uiso 1 1 calc R . . C25 C 0.6549(2) 0.7309(2) 1.0338(3) 0.0847(19) Uani 1 1 d . . . C26 C 0.6475(3) 0.7711(3) 1.0783(3) 0.105(2) Uani 1 1 d . . . H26 H 0.6657 0.8018 1.0661 0.126 Uiso 1 1 calc R . . C27 C 0.5905(3) 0.7845(3) 1.0820(4) 0.168(4) Uani 1 1 d . . . H27A H 0.5811 0.8050 1.0501 0.252 Uiso 1 1 calc R . . H27B H 0.5842 0.8033 1.1160 0.252 Uiso 1 1 calc R . . H27C H 0.5706 0.7536 1.0821 0.252 Uiso 1 1 calc R . . C28 C 0.6678(3) 0.7565(3) 1.1365(3) 0.151(3) Uani 1 1 d . . . H28A H 0.6451 0.7322 1.1537 0.227 Uiso 1 1 calc R . . H28B H 0.6700 0.7865 1.1596 0.227 Uiso 1 1 calc R . . H28C H 0.7012 0.7415 1.1327 0.227 Uiso 1 1 calc R . . C29 C 0.6805(3) 0.7215(3) 0.8744(4) 0.123(3) Uani 1 1 d . . . H29 H 0.6923 0.7571 0.8737 0.148 Uiso 1 1 calc R . . C30 C 0.7207(3) 0.6882(4) 0.8451(4) 0.182(5) Uani 1 1 d . . . H30A H 0.7108 0.6529 0.8476 0.273 Uiso 1 1 calc R . . H30B H 0.7532 0.6930 0.8630 0.273 Uiso 1 1 calc R . . H30C H 0.7231 0.6980 0.8062 0.273 Uiso 1 1 calc R . . C31 C 0.6311(4) 0.7180(3) 0.8408(4) 0.155(3) Uani 1 1 d . . . H31A H 0.6175 0.6840 0.8437 0.233 Uiso 1 1 calc R . . H31B H 0.6379 0.7258 0.8020 0.233 Uiso 1 1 calc R . . H31C H 0.6067 0.7420 0.8555 0.233 Uiso 1 1 calc R . . C32 C 0.8882(2) 0.8051(2) 1.0099(3) 0.0779(16) Uani 1 1 d . . . C33 C 0.8913(3) 0.8579(3) 1.0188(3) 0.092(2) Uani 1 1 d . . . H33 H 0.8703 0.8732 1.0456 0.111 Uiso 1 1 calc R . . C34 C 0.9244(3) 0.8871(3) 0.9889(4) 0.132(3) Uani 1 1 d . . . H34 H 0.9255 0.9223 0.9948 0.158 Uiso 1 1 calc R . . C35 C 0.9563(3) 0.8648(4) 0.9498(4) 0.138(3) Uani 1 1 d . . . H35 H 0.9783 0.8852 0.9288 0.166 Uiso 1 1 calc R . . C36 C 0.9561(3) 0.8137(4) 0.9417(4) 0.136(3) Uani 1 1 d . . . H36 H 0.9789 0.7987 0.9166 0.164 Uiso 1 1 calc R . . C37 C 0.9214(3) 0.7837(3) 0.9712(3) 0.108(2) Uani 1 1 d . . . H37 H 0.9204 0.7486 0.9649 0.130 Uiso 1 1 calc R . . C38 C 0.8659(2) 0.7641(2) 1.1033(3) 0.0734(16) Uani 1 1 d . . . C39 C 0.8308(3) 0.7665(2) 1.1471(3) 0.0896(19) Uani 1 1 d . . . H39 H 0.7975 0.7771 1.1395 0.107 Uiso 1 1 calc R . . C40 C 0.8441(3) 0.7534(3) 1.2017(3) 0.108(2) Uani 1 1 d . . . H40 H 0.8197 0.7553 1.2302 0.130 Uiso 1 1 calc R . . C41 C 0.8926(4) 0.7377(3) 1.2139(4) 0.119(3) Uani 1 1 d . . . H41 H 0.9016 0.7289 1.2506 0.143 Uiso 1 1 calc R . . C42 C 0.9269(3) 0.7351(3) 1.1728(4) 0.111(3) Uani 1 1 d . . . H42 H 0.9598 0.7238 1.1810 0.133 Uiso 1 1 calc R . . C43 C 0.9151(2) 0.7488(2) 1.1174(3) 0.099(2) Uani 1 1 d . . . H43 H 0.9404 0.7477 1.0898 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0717(3) 0.0580(3) 0.0625(3) 0.0008(2) -0.0030(2) 0.0023(2) Cl1 0.1058(12) 0.0791(10) 0.0788(10) -0.0138(8) -0.0150(9) 0.0204(9) Cl2 0.168(2) 0.0735(13) 0.256(3) -0.0004(16) 0.022(2) 0.0319(13) N1 0.075(3) 0.056(3) 0.070(3) 0.004(2) -0.007(2) -0.007(2) N2 0.070(3) 0.056(3) 0.079(3) -0.002(2) -0.002(2) 0.000(2) C1 0.072(4) 0.087(4) 0.084(4) -0.011(4) 0.000(3) -0.004(3) C2 0.067(4) 0.067(4) 0.076(4) -0.005(3) -0.006(3) 0.006(3) C3 0.108(5) 0.057(4) 0.102(5) -0.001(3) -0.023(4) 0.004(3) C4 0.069(4) 0.062(4) 0.082(4) 0.002(3) 0.001(3) 0.001(3) C5 0.082(4) 0.043(3) 0.058(3) 0.000(2) -0.008(3) -0.004(3) C6 0.074(4) 0.076(4) 0.087(4) 0.005(3) -0.026(3) 0.003(3) C7 0.070(4) 0.065(4) 0.109(5) -0.007(4) -0.003(4) -0.001(3) C8 0.088(5) 0.070(4) 0.082(5) 0.028(4) -0.031(4) -0.018(4) C9 0.117(6) 0.057(4) 0.105(6) 0.006(4) -0.045(5) -0.006(4) C10 0.167(9) 0.072(5) 0.183(10) 0.016(6) -0.077(8) -0.016(6) C11 0.159(9) 0.101(7) 0.182(11) 0.050(7) -0.084(8) -0.075(7) C12 0.139(7) 0.121(7) 0.146(8) 0.060(6) -0.053(6) -0.051(7) C13 0.111(6) 0.085(5) 0.094(6) 0.035(4) -0.041(5) -0.024(5) C14 0.107(6) 0.134(7) 0.095(6) 0.043(5) 0.012(5) -0.015(5) C15 0.193(10) 0.236(12) 0.108(7) -0.013(7) -0.042(7) 0.025(8) C16 0.141(9) 0.253(13) 0.148(9) 0.029(8) 0.013(7) -0.002(8) C17 0.150(7) 0.068(4) 0.103(6) -0.014(4) -0.038(5) 0.011(5) C18 0.199(9) 0.129(7) 0.123(7) -0.055(5) -0.065(6) 0.062(6) C19 0.149(8) 0.108(6) 0.164(8) -0.014(5) -0.065(6) 0.025(5) C20 0.065(4) 0.051(3) 0.125(6) -0.005(4) 0.005(4) -0.004(3) C21 0.090(5) 0.068(4) 0.129(6) -0.020(4) 0.012(4) -0.018(4) C22 0.108(6) 0.062(5) 0.215(10) -0.035(6) 0.023(6) -0.021(4) C23 0.107(6) 0.080(6) 0.242(13) 0.034(7) 0.034(7) -0.016(5) C24 0.103(6) 0.080(5) 0.188(9) 0.024(6) 0.029(6) -0.002(5) C25 0.084(4) 0.071(4) 0.099(5) 0.014(4) 0.019(4) -0.007(3) C26 0.121(6) 0.094(5) 0.101(6) 0.009(4) 0.041(5) -0.005(4) C27 0.155(9) 0.174(9) 0.176(9) -0.001(7) 0.051(7) 0.054(7) C28 0.166(8) 0.186(9) 0.103(6) 0.025(6) 0.007(6) -0.013(7) C29 0.117(6) 0.104(6) 0.148(8) -0.063(6) 0.020(6) -0.024(5) C30 0.141(8) 0.228(11) 0.177(9) -0.126(8) 0.029(7) -0.013(7) C31 0.171(9) 0.146(8) 0.149(8) -0.031(6) -0.014(7) -0.016(7) C32 0.072(4) 0.082(4) 0.079(4) -0.002(4) 0.001(3) -0.006(3) C33 0.110(5) 0.082(5) 0.084(5) -0.009(4) 0.018(4) -0.030(4) C34 0.150(8) 0.118(7) 0.127(7) -0.016(6) 0.042(6) -0.044(6) C35 0.132(7) 0.148(8) 0.134(8) -0.002(7) 0.033(6) -0.058(7) C36 0.106(6) 0.154(8) 0.149(8) -0.018(7) 0.057(6) -0.014(6) C37 0.092(5) 0.113(6) 0.120(6) -0.021(5) 0.026(5) -0.002(4) C38 0.078(4) 0.061(4) 0.081(4) 0.000(3) -0.012(4) 0.003(3) C39 0.098(5) 0.089(5) 0.082(5) 0.015(4) 0.002(4) 0.016(4) C40 0.119(6) 0.122(6) 0.083(5) 0.026(4) -0.010(5) 0.023(5) C41 0.143(8) 0.111(6) 0.104(7) 0.013(5) -0.015(6) 0.009(6) C42 0.108(6) 0.103(6) 0.121(7) 0.014(5) -0.052(5) 0.018(5) C43 0.078(5) 0.093(5) 0.125(6) -0.005(4) -0.007(4) 0.010(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 Pd C5 2.028(5) . ? Pd C1 2.074(5) . ? Pd C2 2.107(5) . ? Pd C4 2.257(6) . ? Pd Cl1 2.3560(15) . ? Cl2 C3 1.757(6) . ? N1 C5 1.346(6) . ? N1 C6 1.381(6) . ? N1 C8 1.432(7) . ? N2 C5 1.364(6) . ? N2 C7 1.388(6) . ? N2 C20 1.459(7) . ? C1 C2 1.410(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.407(7) . ? C2 C3 1.514(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C32 1.496(8) . ? C4 C38 1.503(8) . ? C6 C7 1.323(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.407(9) . ? C8 C9 1.409(9) . ? C9 C10 1.382(10) . ? C9 C17 1.495(10) . ? C10 C11 1.390(13) . ? C10 H10 0.9300 . ? C11 C12 1.380(13) . ? C11 H11 0.9300 . ? C12 C13 1.374(9) . ? C12 H12 0.9300 . ? C13 C14 1.506(10) . ? C14 C15 1.501(9) . ? C14 C16 1.513(10) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.525(8) . ? C17 C19 1.546(9) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C25 1.361(8) . ? C20 C21 1.415(8) . ? C21 C22 1.397(9) . ? C21 C29 1.526(10) . ? C22 C23 1.375(12) . ? C22 H22 0.9300 . ? C23 C24 1.359(11) . ? C23 H23 0.9300 . ? C24 C25 1.372(9) . ? C24 H24 0.9300 . ? C25 C26 1.503(8) . ? C26 C28 1.529(9) . ? C26 C27 1.531(9) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C31 1.521(10) . ? C29 C30 1.531(9) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C37 1.383(8) . ? C32 C33 1.398(8) . ? C33 C34 1.354(9) . ? C33 H33 0.9300 . ? C34 C35 1.377(10) . ? C34 H34 0.9300 . ? C35 C36 1.351(10) . ? C35 H35 0.9300 . ? C36 C37 1.389(10) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C43 1.388(7) . ? C38 C39 1.388(8) . ? C39 C40 1.386(8) . ? C39 H39 0.9300 . ? C40 C41 1.366(9) . ? C40 H40 0.9300 . ? C41 C42 1.328(10) . ? C41 H41 0.9300 . ? C42 C43 1.398(9) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? 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 C5 Pd C1 98.0(2) . . ? C5 Pd C2 131.9(2) . . ? C1 Pd C2 39.4(2) . . ? C5 Pd C4 166.2(2) . . ? C1 Pd C4 68.5(2) . . ? C2 Pd C4 37.43(19) . . ? C5 Pd Cl1 93.63(14) . . ? C1 Pd Cl1 168.08(17) . . ? C2 Pd Cl1 130.83(17) . . ? C4 Pd Cl1 99.71(15) . . ? C5 N1 C6 112.6(5) . . ? C5 N1 C8 125.5(5) . . ? C6 N1 C8 121.8(5) . . ? C5 N2 C7 111.4(5) . . ? C5 N2 C20 124.6(5) . . ? C7 N2 C20 123.9(5) . . ? C2 C1 Pd 71.6(3) . . ? C2 C1 H1A 116.4 . . ? Pd C1 H1A 116.4 . . ? C2 C1 H1B 116.4 . . ? Pd C1 H1B 116.4 . . ? H1A C1 H1B 113.4 . . ? C4 C2 C1 120.2(5) . . ? C4 C2 C3 121.5(5) . . ? C1 C2 C3 117.5(5) . . ? C4 C2 Pd 77.1(3) . . ? C1 C2 Pd 69.0(3) . . ? C3 C2 Pd 116.2(4) . . ? C2 C3 Cl2 109.5(4) . . ? C2 C3 H3A 109.8 . . ? Cl2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? Cl2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C2 C4 C32 119.2(5) . . ? C2 C4 C38 121.2(5) . . ? C32 C4 C38 115.1(5) . . ? C2 C4 Pd 65.5(3) . . ? C32 C4 Pd 101.6(4) . . ? C38 C4 Pd 123.0(4) . . ? N1 C5 N2 102.7(4) . . ? N1 C5 Pd 130.5(4) . . ? N2 C5 Pd 126.8(4) . . ? C7 C6 N1 106.4(5) . . ? C7 C6 H6 126.8 . . ? N1 C6 H6 126.8 . . ? C6 C7 N2 106.9(5) . . ? C6 C7 H7 126.6 . . ? N2 C7 H7 126.6 . . ? C13 C8 C9 124.1(7) . . ? C13 C8 N1 118.1(6) . . ? C9 C8 N1 117.9(7) . . ? C10 C9 C8 115.4(9) . . ? C10 C9 C17 121.6(8) . . ? C8 C9 C17 123.0(6) . . ? C9 C10 C11 121.4(10) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 121.7(9) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 119.7(10) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C8 117.7(8) . . ? C12 C13 C14 119.5(9) . . ? C8 C13 C14 122.5(6) . . ? C15 C14 C13 112.3(7) . . ? C15 C14 C16 109.3(7) . . ? C13 C14 C16 115.7(8) . . ? C15 C14 H14 106.3 . . ? C13 C14 H14 106.3 . . ? C16 C14 H14 106.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 C18 111.9(7) . . ? C9 C17 C19 111.9(7) . . ? C18 C17 C19 109.1(6) . . ? C9 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? C19 C17 H17 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 124.2(6) . . ? C25 C20 N2 119.3(6) . . ? C21 C20 N2 116.4(6) . . ? C22 C21 C20 115.1(8) . . ? C22 C21 C29 122.2(7) . . ? C20 C21 C29 122.7(6) . . ? C23 C22 C21 121.3(8) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C24 C23 C22 120.4(9) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.7(9) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C20 C25 C24 117.3(7) . . ? C20 C25 C26 122.3(6) . . ? C24 C25 C26 120.4(7) . . ? C25 C26 C28 114.6(6) . . ? C25 C26 C27 109.0(7) . . ? C28 C26 C27 110.2(6) . . ? C25 C26 H26 107.6 . . ? C28 C26 H26 107.6 . . ? C27 C26 H26 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C21 109.8(7) . . ? C31 C29 C30 108.0(7) . . ? C21 C29 C30 113.8(8) . . ? C31 C29 H29 108.4 . . ? C21 C29 H29 108.4 . . ? C30 C29 H29 108.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 117.7(6) . . ? C37 C32 C4 121.2(6) . . ? C33 C32 C4 121.1(6) . . ? C34 C33 C32 120.9(7) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 120.2(8) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.8(8) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 119.3(8) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C32 C37 C36 121.1(7) . . ? C32 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C43 C38 C39 116.5(6) . . ? C43 C38 C4 120.3(6) . . ? C39 C38 C4 123.0(6) . . ? C40 C39 C38 121.6(7) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C41 C40 C39 120.4(8) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 119.1(8) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C41 C42 C43 122.1(8) . . ? C41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C38 C43 C42 120.3(7) . . ? C38 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? 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 C5 Pd C1 C2 -153.0(3) . . . . ? C4 Pd C1 C2 30.1(3) . . . . ? Cl1 Pd C1 C2 38.8(10) . . . . ? Pd C1 C2 C4 -60.0(5) . . . . ? Pd C1 C2 C3 109.5(5) . . . . ? C5 Pd C2 C4 166.9(3) . . . . ? C1 Pd C2 C4 129.8(5) . . . . ? Cl1 Pd C2 C4 -40.3(4) . . . . ? C5 Pd C2 C1 37.1(5) . . . . ? C4 Pd C2 C1 -129.8(5) . . . . ? Cl1 Pd C2 C1 -170.1(3) . . . . ? C5 Pd C2 C3 -74.1(5) . . . . ? C1 Pd C2 C3 -111.2(6) . . . . ? C4 Pd C2 C3 119.0(6) . . . . ? Cl1 Pd C2 C3 78.6(5) . . . . ? C4 C2 C3 Cl2 -98.7(6) . . . . ? C1 C2 C3 Cl2 91.9(6) . . . . ? Pd C2 C3 Cl2 170.8(3) . . . . ? C1 C2 C4 C32 -33.9(8) . . . . ? C3 C2 C4 C32 157.1(5) . . . . ? Pd C2 C4 C32 -89.9(5) . . . . ? C1 C2 C4 C38 171.1(5) . . . . ? C3 C2 C4 C38 2.1(8) . . . . ? Pd C2 C4 C38 115.1(5) . . . . ? C1 C2 C4 Pd 56.1(5) . . . . ? C3 C2 C4 Pd -113.0(5) . . . . ? C5 Pd C4 C2 -44.8(10) . . . . ? C1 Pd C4 C2 -31.6(3) . . . . ? Cl1 Pd C4 C2 150.2(3) . . . . ? C5 Pd C4 C32 72.2(10) . . . . ? C1 Pd C4 C32 85.3(4) . . . . ? C2 Pd C4 C32 116.9(5) . . . . ? Cl1 Pd C4 C32 -92.8(4) . . . . ? C5 Pd C4 C38 -157.3(7) . . . . ? C1 Pd C4 C38 -144.2(5) . . . . ? C2 Pd C4 C38 -112.6(6) . . . . ? Cl1 Pd C4 C38 37.7(4) . . . . ? C6 N1 C5 N2 -0.3(6) . . . . ? C8 N1 C5 N2 -177.1(5) . . . . ? C6 N1 C5 Pd -178.6(4) . . . . ? C8 N1 C5 Pd 4.6(8) . . . . ? C7 N2 C5 N1 0.0(6) . . . . ? C20 N2 C5 N1 -178.1(5) . . . . ? C7 N2 C5 Pd 178.4(4) . . . . ? C20 N2 C5 Pd 0.2(8) . . . . ? C1 Pd C5 N1 -119.2(5) . . . . ? C2 Pd C5 N1 -142.0(4) . . . . ? C4 Pd C5 N1 -106.8(9) . . . . ? Cl1 Pd C5 N1 58.4(5) . . . . ? C1 Pd C5 N2 62.9(5) . . . . ? C2 Pd C5 N2 40.1(6) . . . . ? C4 Pd C5 N2 75.2(10) . . . . ? Cl1 Pd C5 N2 -119.6(4) . . . . ? C5 N1 C6 C7 0.4(7) . . . . ? C8 N1 C6 C7 177.3(6) . . . . ? N1 C6 C7 N2 -0.3(6) . . . . ? C5 N2 C7 C6 0.2(7) . . . . ? C20 N2 C7 C6 178.4(5) . . . . ? C5 N1 C8 C13 71.2(7) . . . . ? C6 N1 C8 C13 -105.3(7) . . . . ? C5 N1 C8 C9 -109.6(7) . . . . ? C6 N1 C8 C9 73.9(7) . . . . ? C13 C8 C9 C10 1.9(9) . . . . ? N1 C8 C9 C10 -177.3(6) . . . . ? C13 C8 C9 C17 179.7(6) . . . . ? N1 C8 C9 C17 0.5(9) . . . . ? C8 C9 C10 C11 -2.0(11) . . . . ? C17 C9 C10 C11 -179.9(8) . . . . ? C9 C10 C11 C12 1.9(15) . . . . ? C10 C11 C12 C13 -1.3(14) . . . . ? C11 C12 C13 C8 1.0(11) . . . . ? C11 C12 C13 C14 174.5(7) . . . . ? C9 C8 C13 C12 -1.4(9) . . . . ? N1 C8 C13 C12 177.8(5) . . . . ? C9 C8 C13 C14 -174.7(6) . . . . ? N1 C8 C13 C14 4.5(9) . . . . ? C12 C13 C14 C15 -88.1(9) . . . . ? C8 C13 C14 C15 85.1(8) . . . . ? C12 C13 C14 C16 38.3(9) . . . . ? C8 C13 C14 C16 -148.5(7) . . . . ? C10 C9 C17 C18 -46.4(9) . . . . ? C8 C9 C17 C18 135.9(6) . . . . ? C10 C9 C17 C19 76.3(8) . . . . ? C8 C9 C17 C19 -101.4(7) . . . . ? C5 N2 C20 C25 75.2(7) . . . . ? C7 N2 C20 C25 -102.8(7) . . . . ? C5 N2 C20 C21 -106.1(7) . . . . ? C7 N2 C20 C21 75.9(7) . . . . ? C25 C20 C21 C22 -1.2(10) . . . . ? N2 C20 C21 C22 -179.8(5) . . . . ? C25 C20 C21 C29 178.2(7) . . . . ? N2 C20 C21 C29 -0.4(9) . . . . ? C20 C21 C22 C23 0.1(11) . . . . ? C29 C21 C22 C23 -179.3(8) . . . . ? C21 C22 C23 C24 0.0(14) . . . . ? C22 C23 C24 C25 0.9(14) . . . . ? C21 C20 C25 C24 2.0(10) . . . . ? N2 C20 C25 C24 -179.4(6) . . . . ? C21 C20 C25 C26 -177.7(6) . . . . ? N2 C20 C25 C26 0.9(9) . . . . ? C23 C24 C25 C20 -1.9(11) . . . . ? C23 C24 C25 C26 177.8(8) . . . . ? C20 C25 C26 C28 -144.8(7) . . . . ? C24 C25 C26 C28 35.5(10) . . . . ? C20 C25 C26 C27 91.2(8) . . . . ? C24 C25 C26 C27 -88.5(8) . . . . ? C22 C21 C29 C31 77.9(9) . . . . ? C20 C21 C29 C31 -101.4(7) . . . . ? C22 C21 C29 C30 -43.2(10) . . . . ? C20 C21 C29 C30 137.5(7) . . . . ? C2 C4 C32 C37 -51.6(8) . . . . ? C38 C4 C32 C37 104.9(7) . . . . ? Pd C4 C32 C37 -119.9(6) . . . . ? C2 C4 C32 C33 130.8(6) . . . . ? C38 C4 C32 C33 -72.7(7) . . . . ? Pd C4 C32 C33 62.5(6) . . . . ? C37 C32 C33 C34 2.4(10) . . . . ? C4 C32 C33 C34 -179.9(7) . . . . ? C32 C33 C34 C35 -1.2(13) . . . . ? C33 C34 C35 C36 -1.6(15) . . . . ? C34 C35 C36 C37 3.1(15) . . . . ? C33 C32 C37 C36 -0.9(11) . . . . ? C4 C32 C37 C36 -178.6(7) . . . . ? C35 C36 C37 C32 -1.9(13) . . . . ? C2 C4 C38 C43 107.3(7) . . . . ? C32 C4 C38 C43 -48.6(7) . . . . ? Pd C4 C38 C43 -173.3(4) . . . . ? C2 C4 C38 C39 -66.9(8) . . . . ? C32 C4 C38 C39 137.2(6) . . . . ? Pd C4 C38 C39 12.5(8) . . . . ? C43 C38 C39 C40 -1.0(9) . . . . ? C4 C38 C39 C40 173.4(6) . . . . ? C38 C39 C40 C41 0.0(11) . . . . ? C39 C40 C41 C42 -0.1(12) . . . . ? C40 C41 C42 C43 1.2(13) . . . . ? C39 C38 C43 C42 2.0(9) . . . . ? C4 C38 C43 C42 -172.6(6) . . . . ? C41 C42 C43 C38 -2.2(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.826 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.100 data_cd27559 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 744566' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl2 N2 O2 Pd2' _chemical_formula_weight 812.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.8340(11) _cell_length_b 10.3767(8) _cell_length_c 12.6185(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.7140(10) _cell_angle_gamma 90.00 _cell_volume 1670.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2199 _cell_measurement_theta_min 5.060 _cell_measurement_theta_max 44.800 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.176 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.051 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8629 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs-Bruker _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9528 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3615 _reflns_number_gt 2456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 3 distance restraints of solvent. 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^)+(0.0233P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3615 _refine_ls_number_parameters 218 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.09251(2) 0.89806(3) 0.09504(3) 0.04400(12) Uani 1 1 d . . . Cl1 Cl 0.06140(8) 1.12793(10) 0.07895(9) 0.0535(3) Uani 1 1 d . . . O1 O 0.2877(4) 0.5585(5) 0.3660(4) 0.098(2) Uani 0.758(6) 1 d P A 1 O1' O 0.0770(10) 0.4642(14) 0.2042(13) 0.075(5) Uani 0.242(6) 1 d P A 2 N1 N 0.1172(3) 0.5721(4) 0.2954(4) 0.0380(12) Uani 0.758(6) 1 d PD A 1 H1 H 0.0571 0.5347 0.2681 0.046 Uiso 0.758(6) 1 calc PR A 1 N1' N 0.1802(12) 0.5940(14) 0.3440(12) 0.033(4) Uiso 0.242(6) 1 d PD A 2 H1' H 0.2343 0.5947 0.4075 0.040 Uiso 0.242(6) 1 calc PR A 2 C1 C 0.2354(3) 0.8775(4) 0.2464(3) 0.0423(10) Uani 1 1 d . . . C2 C 0.1758(3) 0.7610(4) 0.2209(3) 0.0456(10) Uani 1 1 d . A . C3 C 0.1485(3) 0.7091(4) 0.1114(3) 0.0552(11) Uani 1 1 d . . . H3A H 0.0962 0.6413 0.0899 0.066 Uiso 1 1 calc R . . H3B H 0.2055 0.6931 0.0865 0.066 Uiso 1 1 calc R . . C4 C 0.1276(4) 0.7066(4) 0.3010(4) 0.0670(13) Uani 1 1 d . . . H4A H 0.1708 0.7312 0.3792 0.080 Uiso 0.758(6) 1 calc PR A 1 H4B H 0.0590 0.7449 0.2820 0.080 Uiso 0.758(6) 1 calc PR A 1 H4C H 0.1359 0.7664 0.3674 0.080 Uiso 0.242(6) 1 d PR A 2 H4D H 0.0549 0.6884 0.2584 0.080 Uiso 0.242(6) 1 d PR A 2 C5 C 0.2070(7) 0.5061(8) 0.3353(6) 0.063(2) Uani 0.758(6) 1 d PD A 1 C5' C 0.1476(19) 0.4835(15) 0.2875(18) 0.048(6) Uiso 0.242(6) 1 d PD A 2 C6 C 0.1960(5) 0.3652(5) 0.3392(5) 0.103(2) Uani 1 1 d D . . H6A H 0.2515 0.3241 0.3240 0.170 Uiso 0.758(6) 1 calc PR A 1 H6B H 0.1296 0.3394 0.2821 0.170 Uiso 0.758(6) 1 calc PR A 1 H6C H 0.1995 0.3402 0.4138 0.170 Uiso 0.758(6) 1 calc PR A 1 H6D H 0.1633 0.2948 0.2867 0.170 Uiso 0.242(6) 1 d PR A 2 H6E H 0.2695 0.3687 0.3531 0.170 Uiso 0.242(6) 1 d PR A 2 H6F H 0.1881 0.3537 0.4109 0.170 Uiso 0.242(6) 1 d PR A 2 C7 C 0.2455(3) 0.9537(4) 0.3513(3) 0.0449(10) Uani 1 1 d . . . C8 C 0.3435(4) 0.9673(5) 0.4392(4) 0.0725(14) Uani 1 1 d . . . H8 H 0.4019 0.9326 0.4302 0.087 Uiso 1 1 calc R . . C9 C 0.3562(4) 1.0315(6) 0.5402(4) 0.0852(17) Uani 1 1 d . . . H9 H 0.4223 1.0381 0.5986 0.102 Uiso 1 1 calc R . . C10 C 0.2713(5) 1.0852(5) 0.5539(4) 0.0767(15) Uani 1 1 d . . . H10 H 0.2795 1.1294 0.6210 0.092 Uiso 1 1 calc R . . C11 C 0.1742(4) 1.0730(4) 0.4677(4) 0.0630(13) Uani 1 1 d . . . H11 H 0.1162 1.1092 0.4765 0.076 Uiso 1 1 calc R . . C12 C 0.1613(3) 1.0069(4) 0.3672(4) 0.0530(11) Uani 1 1 d . . . H12 H 0.0947 0.9987 0.3099 0.064 Uiso 1 1 calc R . . C13 C 0.3219(3) 0.8981(4) 0.2035(3) 0.0483(10) Uani 1 1 d . . . C14 C 0.3413(3) 1.0212(5) 0.1720(4) 0.0595(12) Uani 1 1 d . . . H14 H 0.2995 1.0902 0.1746 0.071 Uiso 1 1 calc R . . C15 C 0.4229(4) 1.0395(6) 0.1369(4) 0.0784(16) Uani 1 1 d . . . H15 H 0.4356 1.1214 0.1153 0.094 Uiso 1 1 calc R . . C16 C 0.4860(4) 0.9387(7) 0.1335(4) 0.0833(18) Uani 1 1 d . . . H16 H 0.5413 0.9526 0.1102 0.100 Uiso 1 1 calc R . . C17 C 0.4673(4) 0.8191(7) 0.1641(4) 0.0820(16) Uani 1 1 d . . . H17 H 0.5095 0.7507 0.1611 0.098 Uiso 1 1 calc R . . C18 C 0.3862(3) 0.7982(5) 0.1995(4) 0.0636(13) Uani 1 1 d . . . H18 H 0.3746 0.7157 0.2210 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.04443(19) 0.0427(2) 0.04228(19) 0.00004(17) 0.01386(14) 0.00366(16) Cl1 0.0528(6) 0.0437(6) 0.0525(6) -0.0036(5) 0.0078(5) 0.0007(5) O1 0.069(4) 0.110(5) 0.101(4) 0.034(3) 0.019(3) 0.008(3) O1' 0.063(9) 0.075(10) 0.084(11) 0.004(9) 0.026(8) 0.006(7) N1 0.030(2) 0.028(3) 0.057(3) -0.002(2) 0.018(2) -0.012(2) C1 0.039(2) 0.048(3) 0.036(2) 0.0053(19) 0.0085(17) 0.0094(19) C2 0.052(2) 0.040(2) 0.045(2) 0.002(2) 0.019(2) 0.011(2) C3 0.058(3) 0.041(3) 0.064(3) 0.001(2) 0.021(2) 0.013(2) C4 0.080(3) 0.053(3) 0.079(4) 0.010(3) 0.042(3) 0.005(3) C5 0.060(5) 0.082(6) 0.049(4) 0.014(4) 0.022(4) 0.001(4) C6 0.136(6) 0.056(4) 0.144(6) 0.019(4) 0.088(5) 0.002(4) C7 0.048(2) 0.042(2) 0.044(2) 0.006(2) 0.018(2) 0.001(2) C8 0.059(3) 0.101(4) 0.055(3) -0.011(3) 0.019(3) 0.003(3) C9 0.074(4) 0.121(5) 0.050(3) -0.023(3) 0.012(3) -0.017(4) C10 0.112(5) 0.067(4) 0.055(3) -0.014(3) 0.037(3) -0.027(3) C11 0.094(4) 0.044(3) 0.066(3) 0.001(2) 0.047(3) 0.008(3) C12 0.062(3) 0.048(3) 0.051(3) 0.003(2) 0.024(2) 0.004(2) C13 0.044(2) 0.062(3) 0.037(2) 0.004(2) 0.0136(18) 0.005(2) C14 0.054(3) 0.068(3) 0.055(3) 0.002(3) 0.019(2) -0.006(2) C15 0.069(3) 0.102(5) 0.058(3) 0.013(3) 0.017(3) -0.023(3) C16 0.051(3) 0.141(6) 0.065(4) -0.001(4) 0.030(3) -0.007(4) C17 0.057(3) 0.116(5) 0.078(4) -0.003(4) 0.032(3) 0.013(3) C18 0.056(3) 0.075(4) 0.063(3) 0.008(3) 0.027(2) 0.012(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 Pd C3 2.089(4) . ? Pd C2 2.112(4) . ? Pd C1 2.165(3) . ? Pd Cl1 2.4117(10) 3_575 ? Pd Cl1 2.4184(11) . ? Cl1 Pd 2.4117(10) 3_575 ? O1 C5 1.166(9) . ? O1' C5' 1.14(2) . ? N1 C5 1.335(8) . ? N1 C4 1.402(6) . ? N1 H1 0.8600 . ? N1' C5' 1.334(19) . ? N1' C4 1.373(16) . ? N1' H1' 0.8600 . ? C1 C2 1.429(5) . ? C1 C7 1.502(5) . ? C1 C13 1.507(5) . ? C2 C3 1.393(5) . ? C2 C4 1.517(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 1.0122 . ? C4 H4D 0.9587 . ? C5 C6 1.473(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C6 H6D 0.9717 . ? C6 H6E 0.9645 . ? C6 H6F 0.9595 . ? C7 C12 1.371(5) . ? C7 C8 1.388(6) . ? C8 C9 1.389(6) . ? C8 H8 0.9300 . ? C9 C10 1.370(7) . ? C9 H9 0.9300 . ? C10 C11 1.369(6) . ? C10 H10 0.9300 . ? C11 C12 1.392(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.380(6) . ? C13 C14 1.394(5) . ? C14 C15 1.375(6) . ? C14 H14 0.9300 . ? C15 C16 1.373(7) . ? C15 H15 0.9300 . ? C16 C17 1.354(7) . ? C16 H16 0.9300 . ? C17 C18 1.376(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 C3 Pd C2 38.72(14) . . ? C3 Pd C1 69.07(15) . . ? C2 Pd C1 39.00(14) . . ? C3 Pd Cl1 98.53(12) . 3_575 ? C2 Pd Cl1 130.00(12) . 3_575 ? C1 Pd Cl1 167.60(11) . 3_575 ? C3 Pd Cl1 168.90(12) . . ? C2 Pd Cl1 139.03(12) . . ? C1 Pd Cl1 104.11(11) . . ? Cl1 Pd Cl1 88.16(4) 3_575 . ? Pd Cl1 Pd 91.84(3) 3_575 . ? C5 N1 C4 115.5(6) . . ? C5 N1 H1 122.3 . . ? C4 N1 H1 122.3 . . ? C5 N1 H4D 154.0 . . ? C4 N1 H4D 39.2 . . ? H1 N1 H4D 83.3 . . ? C5' N1' C4 120.2(16) . . ? C5' N1' H1' 119.9 . . ? C4 N1' H1' 119.9 . . ? C2 C1 C7 119.5(3) . . ? C2 C1 C13 120.6(4) . . ? C7 C1 C13 115.2(3) . . ? C2 C1 Pd 68.5(2) . . ? C7 C1 Pd 117.9(3) . . ? C13 C1 Pd 104.5(2) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 C4 119.8(4) . . ? C1 C2 C4 121.9(4) . . ? C3 C2 Pd 69.7(2) . . ? C1 C2 Pd 72.5(2) . . ? C4 C2 Pd 119.9(3) . . ? C2 C3 Pd 71.5(2) . . ? C2 C3 H3A 116.4 . . ? Pd C3 H3A 116.4 . . ? C2 C3 H3B 116.4 . . ? Pd C3 H3B 116.4 . . ? H3A C3 H3B 113.4 . . ? N1' C4 N1 36.9(6) . . ? N1' C4 C2 106.1(7) . . ? N1 C4 C2 113.5(4) . . ? N1' C4 H4A 78.3 . . ? N1 C4 H4A 108.9 . . ? C2 C4 H4A 108.9 . . ? N1' C4 H4B 139.9 . . ? N1 C4 H4B 108.9 . . ? C2 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N1' C4 H4C 108.7 . . ? N1 C4 H4C 128.9 . . ? C2 C4 H4C 112.6 . . ? H4A C4 H4C 33.8 . . ? H4B C4 H4C 75.0 . . ? N1' C4 H4D 109.5 . . ? N1 C4 H4D 73.1 . . ? C2 C4 H4D 109.6 . . ? H4A C4 H4D 136.4 . . ? H4B C4 H4D 39.4 . . ? H4C C4 H4D 110.2 . . ? O1 C5 N1 121.2(8) . . ? O1 C5 C6 123.4(7) . . ? N1 C5 C6 115.4(7) . . ? O1' C5' N1' 129(2) . . ? H6D C6 H6E 109.5 . . ? H6D C6 H6F 110.9 . . ? H6E C6 H6F 109.2 . . ? C12 C7 C8 117.7(4) . . ? C12 C7 C1 123.1(4) . . ? C8 C7 C1 119.1(4) . . ? C7 C8 C9 121.3(5) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 119.2(5) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 120.7(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 121.0(4) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C18 C13 C14 118.7(4) . . ? C18 C13 C1 121.3(4) . . ? C14 C13 C1 120.0(4) . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 121.0(5) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.7(5) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Pd Cl1 Pd 127.4(6) . . . 3_575 ? C2 Pd Cl1 Pd -160.73(16) . . . 3_575 ? C1 Pd Cl1 Pd 178.14(10) . . . 3_575 ? Cl1 Pd Cl1 Pd 0.0 3_575 . . 3_575 ? C3 Pd C1 C2 -31.2(2) . . . . ? Cl1 Pd C1 C2 -30.7(6) 3_575 . . . ? Cl1 Pd C1 C2 157.94(19) . . . . ? C3 Pd C1 C7 -144.2(3) . . . . ? C2 Pd C1 C7 -113.0(4) . . . . ? Cl1 Pd C1 C7 -143.7(4) 3_575 . . . ? Cl1 Pd C1 C7 45.0(3) . . . . ? C3 Pd C1 C13 86.4(3) . . . . ? C2 Pd C1 C13 117.6(4) . . . . ? Cl1 Pd C1 C13 86.9(5) 3_575 . . . ? Cl1 Pd C1 C13 -84.4(3) . . . . ? C7 C1 C2 C3 165.8(3) . . . . ? C13 C1 C2 C3 -39.5(5) . . . . ? Pd C1 C2 C3 55.0(3) . . . . ? C7 C1 C2 C4 -4.1(5) . . . . ? C13 C1 C2 C4 150.6(4) . . . . ? Pd C1 C2 C4 -114.8(4) . . . . ? C7 C1 C2 Pd 110.8(3) . . . . ? C13 C1 C2 Pd -94.5(3) . . . . ? C1 Pd C2 C3 -129.2(3) . . . . ? Cl1 Pd C2 C3 42.5(3) 3_575 . . . ? Cl1 Pd C2 C3 -163.0(2) . . . . ? C3 Pd C2 C1 129.2(3) . . . . ? Cl1 Pd C2 C1 171.76(16) 3_575 . . . ? Cl1 Pd C2 C1 -33.7(3) . . . . ? C3 Pd C2 C4 -113.5(4) . . . . ? C1 Pd C2 C4 117.3(4) . . . . ? Cl1 Pd C2 C4 -71.0(4) 3_575 . . . ? Cl1 Pd C2 C4 83.5(4) . . . . ? C1 C2 C3 Pd -56.4(3) . . . . ? C4 C2 C3 Pd 113.7(4) . . . . ? C1 Pd C3 C2 31.5(2) . . . . ? Cl1 Pd C3 C2 -148.4(2) 3_575 . . . ? Cl1 Pd C3 C2 85.0(6) . . . . ? C5' N1' C4 N1 20.1(12) . . . . ? C5' N1' C4 C2 -87.8(16) . . . . ? C5 N1 C4 N1' -17.9(10) . . . . ? C5 N1 C4 C2 67.8(6) . . . . ? C3 C2 C4 N1' 77.8(8) . . . . ? C1 C2 C4 N1' -112.6(7) . . . . ? Pd C2 C4 N1' 160.3(7) . . . . ? C3 C2 C4 N1 39.2(6) . . . . ? C1 C2 C4 N1 -151.1(4) . . . . ? Pd C2 C4 N1 121.7(4) . . . . ? C4 N1 C5 O1 -4.4(9) . . . . ? C4 N1 C5 C6 174.7(5) . . . . ? C4 N1' C5' O1' -2(3) . . . . ? C2 C1 C7 C12 -61.8(5) . . . . ? C13 C1 C7 C12 142.3(4) . . . . ? Pd C1 C7 C12 18.0(5) . . . . ? C2 C1 C7 C8 115.5(4) . . . . ? C13 C1 C7 C8 -40.5(5) . . . . ? Pd C1 C7 C8 -164.7(3) . . . . ? C12 C7 C8 C9 0.5(7) . . . . ? C1 C7 C8 C9 -176.9(5) . . . . ? C7 C8 C9 C10 -1.2(8) . . . . ? C8 C9 C10 C11 0.9(8) . . . . ? C9 C10 C11 C12 0.0(7) . . . . ? C8 C7 C12 C11 0.4(6) . . . . ? C1 C7 C12 C11 177.7(4) . . . . ? C10 C11 C12 C7 -0.7(7) . . . . ? C2 C1 C13 C18 -37.5(5) . . . . ? C7 C1 C13 C18 118.2(4) . . . . ? Pd C1 C13 C18 -110.8(4) . . . . ? C2 C1 C13 C14 145.5(4) . . . . ? C7 C1 C13 C14 -58.8(5) . . . . ? Pd C1 C13 C14 72.2(4) . . . . ? C18 C13 C14 C15 0.6(6) . . . . ? C1 C13 C14 C15 177.6(4) . . . . ? C13 C14 C15 C16 -0.5(7) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C15 C16 C17 C18 -0.6(8) . . . . ? C16 C17 C18 C13 0.6(8) . . . . ? C14 C13 C18 C17 -0.6(7) . . . . ? C1 C13 C18 C17 -177.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.577 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.093 data_cd28335 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 744567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Br4 Pd2' _chemical_formula_weight 942.97 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3228(16) _cell_length_b 12.311(2) _cell_length_c 14.328(2) _cell_angle_alpha 88.057(4) _cell_angle_beta 77.018(3) _cell_angle_gamma 82.383(3) _cell_volume 1588.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2013 _cell_measurement_theta_min 4.805 _cell_measurement_theta_max 45.485 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.256 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.094 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 6.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.60127 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs-Bruker _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8721 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6108 _reflns_number_gt 3766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6108 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2863 _refine_ls_wR_factor_gt 0.2723 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.75540(11) 0.80920(10) -0.12190(7) 0.0420(4) Uani 1 1 d . . . Pd2 Pd 0.65309(11) 0.63073(10) 0.08115(7) 0.0403(4) Uani 1 1 d . . . Br1 Br 0.53407(16) 0.80247(14) 0.01429(11) 0.0522(5) Uani 1 1 d . . . Br2 Br 0.86237(17) 0.62584(14) -0.06402(11) 0.0573(5) Uani 1 1 d . . . Br3 Br 0.7989(3) 1.0057(2) -0.42475(13) 0.0838(7) Uani 1 1 d . . . Br4 Br 0.4702(3) 0.3326(2) 0.27998(17) 0.1064(10) Uani 1 1 d . . . C1 C 0.7051(17) 0.9712(12) -0.1644(10) 0.049(4) Uani 1 1 d . . . H1 H 0.6557 1.0397 -0.1438 0.059 Uiso 1 1 calc R . . C2 C 0.7942(16) 0.9106(12) -0.2450(10) 0.044(3) Uani 1 1 d . . . C3 C 0.9357(15) 0.8551(13) -0.2340(9) 0.042(3) Uani 1 1 d . . . C4 C 0.7339(18) 0.8983(15) -0.3303(11) 0.056(4) Uani 1 1 d . . . H4A H 0.6263 0.9075 -0.3124 0.067 Uiso 1 1 calc R . . H4B H 0.7674 0.8254 -0.3566 0.067 Uiso 1 1 calc R . . C5 C 0.7362(16) 0.5035(13) 0.1623(9) 0.045(3) Uani 1 1 d . . . H5 H 0.8222 0.4645 0.1751 0.054 Uiso 1 1 calc R . . C6 C 0.5813(16) 0.5139(13) 0.1854(9) 0.044(3) Uani 1 1 d . . . C7 C 0.5016(14) 0.6200(13) 0.2211(9) 0.040(3) Uani 1 1 d . . . C8 C 0.5040(18) 0.4189(14) 0.1642(11) 0.055(4) Uani 1 1 d . . . H8A H 0.5662 0.3753 0.1116 0.066 Uiso 1 1 calc R . . H8B H 0.4107 0.4461 0.1472 0.066 Uiso 1 1 calc R . . C9 C 1.0180(16) 0.7711(14) -0.3055(9) 0.047(4) Uani 1 1 d . . . C10 C 0.967(2) 0.6753(15) -0.3151(10) 0.062(5) Uani 1 1 d . . . H10 H 0.8793 0.6584 -0.2750 0.075 Uiso 1 1 calc R . . C11 C 1.050(3) 0.5992(18) -0.3886(15) 0.095(7) Uani 1 1 d . . . H11 H 1.0135 0.5348 -0.3983 0.114 Uiso 1 1 calc R . . C12 C 1.180(3) 0.621(2) -0.4424(14) 0.102(8) Uani 1 1 d . . . H12 H 1.2352 0.5707 -0.4874 0.123 Uiso 1 1 calc R . . C13 C 1.232(2) 0.720(2) -0.4320(12) 0.084(6) Uani 1 1 d . . . H13 H 1.3217 0.7347 -0.4710 0.101 Uiso 1 1 calc R . . C14 C 1.1540(18) 0.7944(18) -0.3649(13) 0.073(5) Uani 1 1 d . . . H14 H 1.1898 0.8600 -0.3583 0.088 Uiso 1 1 calc R . . C15 C 1.0268(16) 0.9102(14) -0.1784(11) 0.052(4) Uani 1 1 d . . . C16 C 1.035(2) 1.0167(17) -0.1784(12) 0.072(5) Uani 1 1 d . . . H16 H 0.9751 1.0630 -0.2108 0.086 Uiso 1 1 calc R . . C17 C 1.127(3) 1.062(2) -0.1327(14) 0.093(7) Uani 1 1 d . . . H17 H 1.1299 1.1377 -0.1341 0.112 Uiso 1 1 calc R . . C18 C 1.215(3) 0.995(3) -0.0855(15) 0.102(9) Uani 1 1 d . . . H18 H 1.2794 1.0244 -0.0551 0.122 Uiso 1 1 calc R . . C19 C 1.209(2) 0.884(2) -0.0825(14) 0.085(7) Uani 1 1 d . . . H19 H 1.2704 0.8395 -0.0499 0.103 Uiso 1 1 calc R . . C20 C 1.1140(17) 0.8376(15) -0.1274(11) 0.058(4) Uani 1 1 d . . . H20 H 1.1078 0.7627 -0.1241 0.070 Uiso 1 1 calc R . . C21 C 0.5646(15) 0.6779(13) 0.2868(9) 0.043(3) Uani 1 1 d . . . C22 C 0.567(2) 0.7891(16) 0.2801(11) 0.065(5) Uani 1 1 d . . . H22 H 0.5337 0.8277 0.2304 0.077 Uiso 1 1 calc R . . C23 C 0.618(2) 0.8453(17) 0.3459(15) 0.077(6) Uani 1 1 d . . . H23 H 0.6173 0.9209 0.3404 0.092 Uiso 1 1 calc R . . C24 C 0.668(2) 0.792(2) 0.4157(13) 0.086(8) Uani 1 1 d . . . H24 H 0.7079 0.8301 0.4567 0.104 Uiso 1 1 calc R . . C25 C 0.661(2) 0.682(2) 0.4291(13) 0.078(6) Uani 1 1 d . . . H25 H 0.6884 0.6462 0.4817 0.094 Uiso 1 1 calc R . . C26 C 0.6098(18) 0.6228(18) 0.3611(10) 0.068(5) Uani 1 1 d . . . H26 H 0.6077 0.5475 0.3678 0.081 Uiso 1 1 calc R . . C27 C 0.3417(16) 0.6470(13) 0.2242(10) 0.047(4) Uani 1 1 d . . . C28 C 0.2491(18) 0.6864(16) 0.3077(12) 0.064(5) Uani 1 1 d . . . H28 H 0.2893 0.6973 0.3600 0.077 Uiso 1 1 calc R . . C29 C 0.0938(17) 0.7110(19) 0.3166(13) 0.076(6) Uani 1 1 d . . . H29 H 0.0342 0.7394 0.3738 0.092 Uiso 1 1 calc R . . C30 C 0.0315(19) 0.6935(17) 0.2428(15) 0.076(6) Uani 1 1 d . . . H30 H -0.0708 0.7071 0.2494 0.092 Uiso 1 1 calc R . . C31 C 0.1271(18) 0.6534(15) 0.1535(14) 0.064(5) Uani 1 1 d . . . H31 H 0.0854 0.6402 0.1024 0.077 Uiso 1 1 calc R . . C32 C 0.2797(15) 0.6341(12) 0.1427(12) 0.048(4) Uani 1 1 d . . . H32 H 0.3410 0.6133 0.0838 0.057 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 0.0408(6) 0.0469(8) 0.0377(6) -0.0027(5) -0.0072(5) -0.0047(5) Pd2 0.0375(6) 0.0452(8) 0.0373(6) -0.0040(5) -0.0050(4) -0.0061(5) Br1 0.0424(8) 0.0610(11) 0.0498(9) -0.0013(7) -0.0064(6) -0.0007(7) Br2 0.0506(9) 0.0562(11) 0.0538(9) 0.0025(8) 0.0054(7) 0.0038(7) Br3 0.1168(17) 0.0903(17) 0.0550(11) 0.0208(10) -0.0274(11) -0.0424(13) Br4 0.126(2) 0.106(2) 0.1053(17) 0.0477(15) -0.0425(15) -0.0644(17) C1 0.068(10) 0.031(9) 0.042(8) -0.001(6) -0.011(7) 0.011(7) C2 0.055(9) 0.036(9) 0.046(8) 0.004(6) -0.017(7) -0.011(7) C3 0.043(8) 0.050(10) 0.031(7) 0.000(6) -0.003(6) -0.009(7) C4 0.061(10) 0.057(11) 0.058(9) 0.008(8) -0.021(8) -0.022(8) C5 0.051(8) 0.044(10) 0.039(7) 0.006(6) -0.014(6) 0.002(7) C6 0.047(8) 0.052(10) 0.034(7) 0.000(6) -0.005(6) -0.015(7) C7 0.035(7) 0.050(10) 0.034(7) -0.005(6) 0.000(5) -0.013(6) C8 0.062(10) 0.049(11) 0.059(9) -0.003(8) -0.020(8) -0.010(8) C9 0.047(8) 0.059(11) 0.035(7) 0.006(7) -0.011(6) -0.006(7) C10 0.098(13) 0.052(12) 0.032(8) -0.002(7) -0.013(8) 0.003(10) C11 0.15(2) 0.052(14) 0.078(14) -0.012(11) -0.021(15) 0.011(13) C12 0.13(2) 0.10(2) 0.047(11) -0.008(12) 0.015(12) 0.026(16) C13 0.081(13) 0.11(2) 0.043(10) -0.005(11) 0.009(9) 0.010(13) C14 0.051(10) 0.095(16) 0.071(11) -0.012(11) -0.005(9) -0.010(10) C15 0.048(9) 0.056(11) 0.058(9) 0.022(8) -0.020(7) -0.022(8) C16 0.087(13) 0.074(15) 0.070(11) -0.004(10) -0.035(10) -0.035(11) C17 0.120(18) 0.092(19) 0.084(14) 0.017(13) -0.040(14) -0.050(15) C18 0.094(16) 0.15(3) 0.092(15) 0.015(16) -0.052(13) -0.075(17) C19 0.073(13) 0.11(2) 0.086(14) -0.033(13) -0.040(11) -0.015(12) C20 0.055(9) 0.056(11) 0.067(10) -0.022(8) -0.027(8) 0.012(8) C21 0.046(8) 0.044(10) 0.038(7) -0.012(6) -0.010(6) -0.001(6) C22 0.088(13) 0.065(13) 0.050(9) -0.017(8) -0.033(9) -0.009(10) C23 0.090(14) 0.055(13) 0.088(14) -0.033(11) -0.020(12) -0.008(10) C24 0.061(11) 0.14(2) 0.058(11) -0.063(14) -0.013(9) -0.006(13) C25 0.080(13) 0.096(18) 0.065(11) -0.037(11) -0.033(10) -0.001(12) C26 0.059(10) 0.105(17) 0.040(8) -0.002(9) -0.011(8) -0.014(10) C27 0.046(8) 0.058(11) 0.040(8) -0.002(7) -0.011(6) -0.013(7) C28 0.056(10) 0.080(14) 0.051(9) -0.007(9) 0.001(8) -0.010(9) C29 0.030(8) 0.123(19) 0.069(11) 0.012(11) -0.001(8) -0.004(9) C30 0.044(10) 0.079(15) 0.106(16) -0.007(12) -0.011(11) -0.016(9) C31 0.052(10) 0.059(12) 0.092(13) 0.016(10) -0.034(9) -0.014(8) C32 0.039(8) 0.032(9) 0.073(10) -0.006(7) -0.015(7) 0.000(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 C1 2.089(15) . ? Pd1 C2 2.117(14) . ? Pd1 C3 2.168(13) . ? Pd1 Br1 2.5095(17) . ? Pd1 Br2 2.535(2) . ? Pd2 C5 2.089(14) . ? Pd2 C6 2.100(14) . ? Pd2 C7 2.189(12) . ? Pd2 Br2 2.5082(17) . ? Pd2 Br1 2.518(2) . ? Br3 C4 1.916(15) . ? Br4 C8 1.927(15) . ? C1 C2 1.429(19) . ? C1 H1 0.9300 . ? C2 C3 1.44(2) . ? C2 C4 1.475(19) . ? C3 C9 1.49(2) . ? C3 C15 1.52(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.40(2) . ? C5 H5 0.9300 . ? C6 C7 1.46(2) . ? C6 C8 1.52(2) . ? C7 C21 1.465(18) . ? C7 C27 1.47(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.35(2) . ? C9 C14 1.42(2) . ? C10 C11 1.45(3) . ? C10 H10 0.9300 . ? C11 C12 1.34(3) . ? C11 H11 0.9300 . ? C12 C13 1.39(3) . ? C12 H12 0.9300 . ? C13 C14 1.37(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.32(2) . ? C15 C20 1.42(2) . ? C16 C17 1.38(2) . ? C16 H16 0.9300 . ? C17 C18 1.36(3) . ? C17 H17 0.9300 . ? C18 C19 1.37(3) . ? C18 H18 0.9300 . ? C19 C20 1.40(2) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.36(2) . ? C21 C22 1.37(2) . ? C22 C23 1.39(2) . ? C22 H22 0.9300 . ? C23 C24 1.31(3) . ? C23 H23 0.9300 . ? C24 C25 1.37(3) . ? C24 H24 0.9300 . ? C25 C26 1.43(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.37(2) . ? C27 C32 1.44(2) . ? C28 C29 1.42(2) . ? C28 H28 0.9300 . ? C29 C30 1.35(2) . ? C29 H29 0.9300 . ? C30 C31 1.45(2) . ? C30 H30 0.9300 . ? C31 C32 1.39(2) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? 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 C1 Pd1 C2 39.7(5) . . ? C1 Pd1 C3 70.1(6) . . ? C2 Pd1 C3 39.3(5) . . ? C1 Pd1 Br1 97.9(4) . . ? C2 Pd1 Br1 132.3(4) . . ? C3 Pd1 Br1 166.9(4) . . ? C1 Pd1 Br2 168.6(4) . . ? C2 Pd1 Br2 138.5(4) . . ? C3 Pd1 Br2 103.3(4) . . ? Br1 Pd1 Br2 87.70(6) . . ? C5 Pd2 C6 38.9(6) . . ? C5 Pd2 C7 69.6(5) . . ? C6 Pd2 C7 39.8(6) . . ? C5 Pd2 Br2 100.7(4) . . ? C6 Pd2 Br2 133.5(4) . . ? C7 Pd2 Br2 169.4(4) . . ? C5 Pd2 Br1 168.8(4) . . ? C6 Pd2 Br1 135.7(4) . . ? C7 Pd2 Br1 101.1(4) . . ? Br2 Pd2 Br1 88.12(6) . . ? Pd1 Br1 Pd2 92.00(6) . . ? Pd2 Br2 Pd1 91.62(6) . . ? C2 C1 Pd1 71.2(8) . . ? C2 C1 H1 144.4 . . ? Pd1 C1 H1 144.4 . . ? C1 C2 C3 116.8(12) . . ? C1 C2 C4 119.9(14) . . ? C3 C2 C4 123.1(14) . . ? C1 C2 Pd1 69.1(8) . . ? C3 C2 Pd1 72.3(8) . . ? C4 C2 Pd1 124.0(10) . . ? C2 C3 C9 119.3(12) . . ? C2 C3 C15 119.4(14) . . ? C9 C3 C15 116.9(12) . . ? C2 C3 Pd1 68.4(7) . . ? C9 C3 Pd1 118.8(10) . . ? C15 C3 Pd1 102.6(8) . . ? C2 C4 Br3 109.9(10) . . ? C2 C4 H4A 109.7 . . ? Br3 C4 H4A 109.7 . . ? C2 C4 H4B 109.7 . . ? Br3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 Pd2 70.9(8) . . ? C6 C5 H5 144.5 . . ? Pd2 C5 H5 144.5 . . ? C5 C6 C7 117.5(13) . . ? C5 C6 C8 119.0(14) . . ? C7 C6 C8 123.2(13) . . ? C5 C6 Pd2 70.1(8) . . ? C7 C6 Pd2 73.4(8) . . ? C8 C6 Pd2 122.3(9) . . ? C6 C7 C21 116.9(12) . . ? C6 C7 C27 120.8(12) . . ? C21 C7 C27 117.9(12) . . ? C6 C7 Pd2 66.8(7) . . ? C21 C7 Pd2 105.0(8) . . ? C27 C7 Pd2 116.8(9) . . ? C6 C8 Br4 106.1(10) . . ? C6 C8 H8A 110.5 . . ? Br4 C8 H8A 110.5 . . ? C6 C8 H8B 110.5 . . ? Br4 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C10 C9 C14 119.9(16) . . ? C10 C9 C3 122.2(13) . . ? C14 C9 C3 117.9(15) . . ? C9 C10 C11 119.1(18) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 121(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 120(2) . . ? C13 C14 H14 120.2 . . ? C9 C14 H14 120.2 . . ? C16 C15 C20 119.8(15) . . ? C16 C15 C3 125.1(14) . . ? C20 C15 C3 115.0(14) . . ? C15 C16 C17 123(2) . . ? C15 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 119(2) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 120.4(19) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 121(2) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C15 116.6(19) . . ? C19 C20 H20 121.7 . . ? C15 C20 H20 121.7 . . ? C26 C21 C22 118.9(14) . . ? C26 C21 C7 119.7(15) . . ? C22 C21 C7 121.2(13) . . ? C21 C22 C23 121.3(17) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 120(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.8(18) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C26 119.2(19) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C21 C26 C25 119(2) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C32 118.9(14) . . ? C28 C27 C7 118.8(13) . . ? C32 C27 C7 122.3(13) . . ? C27 C28 C29 121.8(16) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 120.6(18) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 118.7(16) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 121.1(16) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C27 118.8(15) . . ? C31 C32 H32 120.6 . . ? C27 C32 H32 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 Br1 Pd2 -164.4(4) . . . . ? C2 Pd1 Br1 Pd2 173.1(5) . . . . ? C3 Pd1 Br1 Pd2 -142.0(16) . . . . ? Br2 Pd1 Br1 Pd2 5.62(6) . . . . ? C5 Pd2 Br1 Pd1 136(2) . . . . ? C6 Pd2 Br1 Pd1 -167.9(5) . . . . ? C7 Pd2 Br1 Pd1 169.0(4) . . . . ? Br2 Pd2 Br1 Pd1 -5.67(6) . . . . ? C5 Pd2 Br2 Pd1 -167.4(4) . . . . ? C6 Pd2 Br2 Pd1 168.5(5) . . . . ? C7 Pd2 Br2 Pd1 -145(2) . . . . ? Br1 Pd2 Br2 Pd1 5.62(6) . . . . ? C1 Pd1 Br2 Pd2 113.9(19) . . . . ? C2 Pd1 Br2 Pd2 -171.6(6) . . . . ? C3 Pd1 Br2 Pd2 167.2(4) . . . . ? Br1 Pd1 Br2 Pd2 -5.64(6) . . . . ? C3 Pd1 C1 C2 31.6(8) . . . . ? Br1 Pd1 C1 C2 -153.7(8) . . . . ? Br2 Pd1 C1 C2 88(2) . . . . ? Pd1 C1 C2 C3 -56.1(11) . . . . ? Pd1 C1 C2 C4 118.1(13) . . . . ? C3 Pd1 C2 C1 -128.9(12) . . . . ? Br1 Pd1 C2 C1 36.4(10) . . . . ? Br2 Pd1 C2 C1 -162.6(7) . . . . ? C1 Pd1 C2 C3 128.9(12) . . . . ? Br1 Pd1 C2 C3 165.4(6) . . . . ? Br2 Pd1 C2 C3 -33.7(10) . . . . ? C1 Pd1 C2 C4 -112.7(17) . . . . ? C3 Pd1 C2 C4 118.4(17) . . . . ? Br1 Pd1 C2 C4 -76.3(15) . . . . ? Br2 Pd1 C2 C4 84.7(14) . . . . ? C1 C2 C3 C9 166.3(13) . . . . ? C4 C2 C3 C9 -8(2) . . . . ? Pd1 C2 C3 C9 111.8(13) . . . . ? C1 C2 C3 C15 -38.2(18) . . . . ? C4 C2 C3 C15 147.9(13) . . . . ? Pd1 C2 C3 C15 -92.7(11) . . . . ? C1 C2 C3 Pd1 54.5(11) . . . . ? C4 C2 C3 Pd1 -119.5(14) . . . . ? C1 Pd1 C3 C2 -31.9(8) . . . . ? Br1 Pd1 C3 C2 -55.6(19) . . . . ? Br2 Pd1 C3 C2 157.8(7) . . . . ? C1 Pd1 C3 C9 -144.4(12) . . . . ? C2 Pd1 C3 C9 -112.5(13) . . . . ? Br1 Pd1 C3 C9 -168.1(10) . . . . ? Br2 Pd1 C3 C9 45.3(11) . . . . ? C1 Pd1 C3 C15 85.0(10) . . . . ? C2 Pd1 C3 C15 116.9(14) . . . . ? Br1 Pd1 C3 C15 61(2) . . . . ? Br2 Pd1 C3 C15 -85.3(10) . . . . ? C1 C2 C4 Br3 97.0(14) . . . . ? C3 C2 C4 Br3 -89.2(16) . . . . ? Pd1 C2 C4 Br3 -179.2(8) . . . . ? C7 Pd2 C5 C6 32.4(8) . . . . ? Br2 Pd2 C5 C6 -151.9(8) . . . . ? Br1 Pd2 C5 C6 67(2) . . . . ? Pd2 C5 C6 C7 -57.9(11) . . . . ? Pd2 C5 C6 C8 116.7(12) . . . . ? C7 Pd2 C6 C5 -128.3(12) . . . . ? Br2 Pd2 C6 C5 39.6(10) . . . . ? Br1 Pd2 C6 C5 -165.2(7) . . . . ? C5 Pd2 C6 C7 128.3(12) . . . . ? Br2 Pd2 C6 C7 168.0(6) . . . . ? Br1 Pd2 C6 C7 -36.9(10) . . . . ? C5 Pd2 C6 C8 -112.4(16) . . . . ? C7 Pd2 C6 C8 119.2(15) . . . . ? Br2 Pd2 C6 C8 -72.8(13) . . . . ? Br1 Pd2 C6 C8 82.4(13) . . . . ? C5 C6 C7 C21 -39.4(17) . . . . ? C8 C6 C7 C21 146.3(13) . . . . ? Pd2 C6 C7 C21 -95.6(11) . . . . ? C5 C6 C7 C27 164.6(12) . . . . ? C8 C6 C7 C27 -10(2) . . . . ? Pd2 C6 C7 C27 108.3(12) . . . . ? C5 C6 C7 Pd2 56.3(10) . . . . ? C8 C6 C7 Pd2 -118.1(13) . . . . ? C5 Pd2 C7 C6 -31.7(8) . . . . ? Br2 Pd2 C7 C6 -55(2) . . . . ? Br1 Pd2 C7 C6 154.7(7) . . . . ? C5 Pd2 C7 C21 81.6(11) . . . . ? C6 Pd2 C7 C21 113.3(13) . . . . ? Br2 Pd2 C7 C21 58(3) . . . . ? Br1 Pd2 C7 C21 -92.0(10) . . . . ? C5 Pd2 C7 C27 -145.8(13) . . . . ? C6 Pd2 C7 C27 -114.1(14) . . . . ? Br2 Pd2 C7 C27 -169.5(14) . . . . ? Br1 Pd2 C7 C27 40.6(11) . . . . ? C5 C6 C8 Br4 93.5(13) . . . . ? C7 C6 C8 Br4 -92.2(14) . . . . ? Pd2 C6 C8 Br4 177.2(8) . . . . ? C2 C3 C9 C10 -66(2) . . . . ? C15 C3 C9 C10 137.4(15) . . . . ? Pd1 C3 C9 C10 13.6(19) . . . . ? C2 C3 C9 C14 113.4(16) . . . . ? C15 C3 C9 C14 -42.7(19) . . . . ? Pd1 C3 C9 C14 -166.6(11) . . . . ? C14 C9 C10 C11 -2(2) . . . . ? C3 C9 C10 C11 177.8(15) . . . . ? C9 C10 C11 C12 4(3) . . . . ? C10 C11 C12 C13 -3(3) . . . . ? C11 C12 C13 C14 1(3) . . . . ? C12 C13 C14 C9 0(3) . . . . ? C10 C9 C14 C13 0(3) . . . . ? C3 C9 C14 C13 -179.5(16) . . . . ? C2 C3 C15 C16 -36(2) . . . . ? C9 C3 C15 C16 120.3(19) . . . . ? Pd1 C3 C15 C16 -107.9(16) . . . . ? C2 C3 C15 C20 147.5(14) . . . . ? C9 C3 C15 C20 -56.4(17) . . . . ? Pd1 C3 C15 C20 75.3(14) . . . . ? C20 C15 C16 C17 2(3) . . . . ? C3 C15 C16 C17 -175.0(17) . . . . ? C15 C16 C17 C18 0(3) . . . . ? C16 C17 C18 C19 -1(4) . . . . ? C17 C18 C19 C20 0(4) . . . . ? C18 C19 C20 C15 2(3) . . . . ? C16 C15 C20 C19 -3(2) . . . . ? C3 C15 C20 C19 174.4(15) . . . . ? C6 C7 C21 C26 -46.7(18) . . . . ? C27 C7 C21 C26 110.1(17) . . . . ? Pd2 C7 C21 C26 -117.9(13) . . . . ? C6 C7 C21 C22 139.3(15) . . . . ? C27 C7 C21 C22 -64.0(18) . . . . ? Pd2 C7 C21 C22 68.0(16) . . . . ? C26 C21 C22 C23 2(3) . . . . ? C7 C21 C22 C23 175.9(15) . . . . ? C21 C22 C23 C24 1(3) . . . . ? C22 C23 C24 C25 -4(3) . . . . ? C23 C24 C25 C26 5(3) . . . . ? C22 C21 C26 C25 -1(2) . . . . ? C7 C21 C26 C25 -175.2(14) . . . . ? C24 C25 C26 C21 -2(3) . . . . ? C6 C7 C27 C28 129.4(16) . . . . ? C21 C7 C27 C28 -26(2) . . . . ? Pd2 C7 C27 C28 -152.8(13) . . . . ? C6 C7 C27 C32 -51(2) . . . . ? C21 C7 C27 C32 153.2(14) . . . . ? Pd2 C7 C27 C32 26.8(19) . . . . ? C32 C27 C28 C29 2(3) . . . . ? C7 C27 C28 C29 -178.1(17) . . . . ? C27 C28 C29 C30 2(3) . . . . ? C28 C29 C30 C31 -2(3) . . . . ? C29 C30 C31 C32 -1(3) . . . . ? C30 C31 C32 C27 5(2) . . . . ? C28 C27 C32 C31 -5(2) . . . . ? C7 C27 C32 C31 175.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.780 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.241 data_cd29636 #TrackingRef '- all.cif' _database_code_depnum_ccdc_archive 'CCDC 758823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Br4 Cl4 Pd2' _chemical_formula_weight 1082.75 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' Cl Cl 0.1484 0.1585 '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' 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 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 10.7816(6) _cell_length_b 27.7470(16) _cell_length_c 25.1259(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.5670(10) _cell_angle_gamma 90.00 _cell_volume 7432.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5774 _cell_measurement_theta_min 4.376 _cell_measurement_theta_max 44.275 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.265 _exptl_crystal_size_mid 0.113 _exptl_crystal_size_min 0.101 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4296 _exptl_absorpt_coefficient_mu 5.651 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7696 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40804 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14600 _reflns_number_gt 7695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 2 distance restraints of solvent. PLATON SQUEEZE was used for removing the solvent contribution. 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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 411 81 ' ' 2 0.500 1.000 1.000 411 81 ' ' _platon_squeeze_details ; ; _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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14600 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.022 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 1.07890(6) 0.11375(3) 0.69777(3) 0.0374(2) Uani 1 1 d . . . Pd2 Pd 0.84294(7) 0.09874(3) 0.75364(3) 0.0425(2) Uani 1 1 d . . . Pd3 Pd 1.03402(7) 0.25424(3) 0.30610(3) 0.0432(2) Uani 1 1 d . . . Pd4 Pd 0.81390(7) 0.29391(3) 0.35584(3) 0.0414(2) Uani 1 1 d . . . Br1 Br 0.91582(9) 0.17595(4) 0.71505(4) 0.0448(3) Uani 1 1 d . . . Br2 Br 1.06936(9) 0.07757(4) 0.78824(5) 0.0516(3) Uani 1 1 d . . . Br3 Br 1.40820(11) 0.08335(5) 0.59031(6) 0.0704(4) Uani 1 1 d . . . Br4 Br 0.44856(15) 0.05601(6) 0.81050(9) 0.1175(7) Uani 1 1 d . . . Br5 Br 0.86795(10) 0.31358(4) 0.26415(4) 0.0510(3) Uani 1 1 d . . . Br6 Br 1.04574(10) 0.30023(4) 0.39236(5) 0.0534(3) Uani 1 1 d . . . Br7 Br 1.38311(11) 0.15568(5) 0.28084(6) 0.0759(4) Uani 1 1 d . . . Br8 Br 0.40217(13) 0.31939(6) 0.40334(8) 0.1124(6) Uani 1 1 d . . . Cl1 Cl 1.2015(3) 0.32090(11) 0.53245(16) 0.0847(11) Uani 1 1 d . . . Cl2 Cl 0.6212(3) 0.03470(12) 0.50155(13) 0.0710(9) Uani 1 1 d . . . Cl3 Cl 0.7345(4) -0.08735(13) 0.56728(15) 0.0974(12) Uani 1 1 d . . . Cl4 Cl 0.9342(4) -0.08430(15) 0.96468(17) 0.1187(15) Uani 1 1 d . . . Cl5 Cl 1.0045(3) 0.28792(14) 0.02194(14) 0.0885(11) Uani 1 1 d . . . Cl6 Cl 0.6187(3) 0.06265(12) 0.25121(18) 0.0964(13) Uani 1 1 d . . . Cl7 Cl 0.7957(3) 0.05029(10) 0.39055(14) 0.0778(10) Uani 1 1 d . . . Cl8 Cl 0.9314(4) 0.33844(16) 0.64387(16) 0.1206(17) Uani 1 1 d . . . C1 C 1.1683(10) 0.0544(4) 0.6691(4) 0.056(3) Uani 1 1 d . . . H1A H 1.2354 0.0399 0.6940 0.068 Uiso 1 1 calc R . . H1B H 1.1144 0.0309 0.6486 0.068 Uiso 1 1 calc R . . C2 C 1.2023(9) 0.0965(3) 0.6394(4) 0.041(2) Uani 1 1 d . . . C3 C 1.3297(8) 0.1129(4) 0.6484(4) 0.048(3) Uani 1 1 d . . . H3A H 1.3716 0.1025 0.6833 0.057 Uiso 1 1 calc R . . H3B H 1.3335 0.1478 0.6465 0.057 Uiso 1 1 calc R . . C4 C 1.0961(8) 0.1251(3) 0.6131(4) 0.038(2) Uani 1 1 d . . . C5 C 1.1257(8) 0.1745(3) 0.5938(4) 0.039(2) Uani 1 1 d . . . C6 C 1.1514(8) 0.2127(4) 0.6287(4) 0.048(3) Uani 1 1 d . . . H6 H 1.1512 0.2086 0.6654 0.057 Uiso 1 1 calc R . . C7 C 1.1770(9) 0.2566(4) 0.6087(5) 0.050(3) Uani 1 1 d . . . H7 H 1.1989 0.2820 0.6325 0.060 Uiso 1 1 calc R . . C8 C 1.1717(9) 0.2642(4) 0.5568(5) 0.051(3) Uani 1 1 d . . . C9 C 1.1446(11) 0.2270(4) 0.5228(5) 0.071(4) Uani 1 1 d . . . H9 H 1.1423 0.2316 0.4860 0.085 Uiso 1 1 calc R . . C10 C 1.1207(9) 0.1829(4) 0.5418(4) 0.050(3) Uani 1 1 d . . . H10 H 1.1001 0.1578 0.5175 0.060 Uiso 1 1 calc R . . C11 C 0.9800(8) 0.1006(3) 0.5852(4) 0.039(2) Uani 1 1 d . . . C12 C 0.9825(9) 0.0554(4) 0.5601(4) 0.050(3) Uani 1 1 d . . . H12 H 1.0584 0.0393 0.5607 0.060 Uiso 1 1 calc R . . C13 C 0.8745(9) 0.0350(4) 0.5349(4) 0.049(3) Uani 1 1 d . . . H13 H 0.8756 0.0044 0.5198 0.059 Uiso 1 1 calc R . . C14 C 0.7641(10) 0.0600(4) 0.5321(4) 0.053(3) Uani 1 1 d . . . C15 C 0.7553(9) 0.1051(4) 0.5547(5) 0.056(3) Uani 1 1 d . . . H15 H 0.6790 0.1211 0.5531 0.067 Uiso 1 1 calc R . . C16 C 0.8672(8) 0.1253(3) 0.5799(4) 0.042(3) Uani 1 1 d . . . H16 H 0.8661 0.1565 0.5936 0.051 Uiso 1 1 calc R . . C17 C 0.6508(9) 0.1019(4) 0.7229(5) 0.057(3) Uani 1 1 d . . . H17A H 0.6101 0.1328 0.7255 0.068 Uiso 1 1 calc R . . H17B H 0.6248 0.0857 0.6889 0.068 Uiso 1 1 calc R . . C18 C 0.6642(9) 0.0721(4) 0.7704(5) 0.057(3) Uani 1 1 d . . . C19 C 0.6146(10) 0.0877(4) 0.8169(5) 0.065(4) Uani 1 1 d . . . H19A H 0.6060 0.1225 0.8173 0.078 Uiso 1 1 calc R . . H19B H 0.6680 0.0776 0.8495 0.078 Uiso 1 1 calc R . . C20 C 0.7479(8) 0.0309(4) 0.7662(4) 0.045(3) Uani 1 1 d . . . C21 C 0.7458(10) 0.0038(3) 0.7148(4) 0.047(3) Uani 1 1 d . . . C22 C 0.8588(10) -0.0136(4) 0.6981(4) 0.049(3) Uani 1 1 d . . . H22 H 0.9363 -0.0053 0.7174 0.059 Uiso 1 1 calc R . . C23 C 0.8525(11) -0.0410(4) 0.6557(5) 0.057(3) Uani 1 1 d . . . H23 H 0.9262 -0.0540 0.6467 0.069 Uiso 1 1 calc R . . C24 C 0.7439(12) -0.0510(4) 0.6246(5) 0.057(3) Uani 1 1 d . . . C25 C 0.6329(13) -0.0331(4) 0.6377(5) 0.074(4) Uani 1 1 d . . . H25 H 0.5576 -0.0395 0.6156 0.088 Uiso 1 1 calc R . . C26 C 0.6328(9) -0.0061(4) 0.6827(5) 0.051(3) Uani 1 1 d . . . H26 H 0.5580 0.0055 0.6920 0.061 Uiso 1 1 calc R . . C27 C 0.7933(9) 0.0038(4) 0.8169(5) 0.047(3) Uani 1 1 d . . . C28 C 0.7756(10) -0.0457(4) 0.8202(5) 0.068(4) Uani 1 1 d . . . H28 H 0.7365 -0.0619 0.7899 0.082 Uiso 1 1 calc R . . C29 C 0.8144(12) -0.0724(4) 0.8675(6) 0.072(4) Uani 1 1 d . . . H29 H 0.7983 -0.1052 0.8684 0.087 Uiso 1 1 calc R . . C30 C 0.8738(12) -0.0504(5) 0.9103(5) 0.075(4) Uani 1 1 d . . . C31 C 0.8907(11) -0.0012(5) 0.9104(5) 0.079(4) Uani 1 1 d . . . H31 H 0.9282 0.0143 0.9416 0.095 Uiso 1 1 calc R . . C32 C 0.8527(11) 0.0247(4) 0.8652(5) 0.068(3) Uani 1 1 d . . . H32 H 0.8665 0.0578 0.8661 0.082 Uiso 1 1 calc R . . C33 C 1.1393(9) 0.1936(4) 0.3343(5) 0.050(3) Uani 1 1 d . . . H33A H 1.2135 0.1994 0.3604 0.060 Uiso 1 1 calc R . . H33B H 1.0923 0.1653 0.3422 0.060 Uiso 1 1 calc R . . C34 C 1.1507(9) 0.2006(3) 0.2831(5) 0.044(3) Uani 1 1 d . . . C35 C 1.2822(9) 0.2139(4) 0.2701(5) 0.055(3) Uani 1 1 d . . . H35A H 1.3192 0.2393 0.2938 0.066 Uiso 1 1 calc R . . H35B H 1.2766 0.2249 0.2332 0.066 Uiso 1 1 calc R . . C36 C 1.0408(8) 0.2022(3) 0.2430(4) 0.036(2) Uani 1 1 d . . . C37 C 1.0430(8) 0.2217(4) 0.1874(4) 0.040(2) Uani 1 1 d . . . C38 C 1.0817(9) 0.2679(4) 0.1803(4) 0.050(3) Uani 1 1 d . . . H38 H 1.1141 0.2862 0.2101 0.060 Uiso 1 1 calc R . . C39 C 1.0732(10) 0.2876(4) 0.1296(5) 0.054(3) Uani 1 1 d . . . H39 H 1.1007 0.3190 0.1252 0.065 Uiso 1 1 calc R . . C40 C 1.0248(10) 0.2613(4) 0.0861(5) 0.055(3) Uani 1 1 d . . . C41 C 0.9899(10) 0.2147(5) 0.0925(5) 0.065(3) Uani 1 1 d . . . H41 H 0.9591 0.1961 0.0627 0.078 Uiso 1 1 calc R . . C42 C 1.0004(9) 0.1956(4) 0.1426(5) 0.050(3) Uani 1 1 d . . . H42 H 0.9777 0.1636 0.1465 0.060 Uiso 1 1 calc R . . C43 C 0.9388(9) 0.1670(4) 0.2456(4) 0.045(3) Uani 1 1 d . . . C44 C 0.9623(10) 0.1190(4) 0.2529(5) 0.059(3) Uani 1 1 d . . . H44 H 1.0444 0.1079 0.2562 0.070 Uiso 1 1 calc R . . C45 C 0.8650(11) 0.0865(4) 0.2554(6) 0.086(5) Uani 1 1 d . . . H45 H 0.8827 0.0539 0.2605 0.103 Uiso 1 1 calc R . . C46 C 0.7411(10) 0.1025(4) 0.2504(5) 0.052(3) Uani 1 1 d . . . C47 C 0.7174(9) 0.1503(4) 0.2443(5) 0.053(3) Uani 1 1 d . . . H47 H 0.6354 0.1615 0.2420 0.064 Uiso 1 1 calc R . . C48 C 0.8140(9) 0.1829(4) 0.2416(4) 0.048(3) Uani 1 1 d . . . H48 H 0.7960 0.2156 0.2371 0.057 Uiso 1 1 calc R . . C49 C 0.6281(9) 0.2744(4) 0.3335(4) 0.046(3) Uani 1 1 d . . . H49A H 0.5775 0.2957 0.3085 0.056 Uiso 1 1 calc R . . H49B H 0.6121 0.2405 0.3259 0.056 Uiso 1 1 calc R . . C50 C 0.6442(9) 0.2880(4) 0.3885(4) 0.047(3) Uani 1 1 d . . . C51 C 0.5766(9) 0.3317(4) 0.4052(5) 0.059(3) Uani 1 1 d . . . H51A H 0.5874 0.3583 0.3813 0.070 Uiso 1 1 calc R . . H51B H 0.6129 0.3411 0.4414 0.070 Uiso 1 1 calc R . . C52 C 0.7407(8) 0.2621(3) 0.4223(4) 0.040(2) Uani 1 1 d . . . C53 C 0.7560(8) 0.2100(4) 0.4145(4) 0.039(2) Uani 1 1 d . . . C54 C 0.8689(9) 0.1894(4) 0.4234(4) 0.044(3) Uani 1 1 d . . . H54 H 0.9397 0.2081 0.4341 0.053 Uiso 1 1 calc R . . C55 C 0.8806(10) 0.1405(4) 0.4167(5) 0.057(3) Uani 1 1 d . . . H55 H 0.9600 0.1267 0.4237 0.068 Uiso 1 1 calc R . . C56 C 0.7801(11) 0.1117(4) 0.4003(4) 0.050(3) Uani 1 1 d . . . C57 C 0.6671(11) 0.1315(4) 0.3940(5) 0.063(3) Uani 1 1 d . . . H57 H 0.5965 0.1125 0.3838 0.075 Uiso 1 1 calc R . . C58 C 0.6531(10) 0.1812(4) 0.4026(4) 0.054(3) Uani 1 1 d . . . H58 H 0.5733 0.1945 0.4002 0.064 Uiso 1 1 calc R . . C59 C 0.7912(9) 0.2810(3) 0.4776(4) 0.042(2) Uani 1 1 d . . . C60 C 0.8008(8) 0.2524(4) 0.5212(4) 0.047(3) Uani 1 1 d . . . H60 H 0.7772 0.2202 0.5171 0.056 Uiso 1 1 calc R . . C61 C 0.8451(10) 0.2698(5) 0.5719(5) 0.066(3) Uani 1 1 d . . . H61 H 0.8508 0.2494 0.6016 0.079 Uiso 1 1 calc R . . C62 C 0.8804(11) 0.3170(5) 0.5787(5) 0.064(3) Uani 1 1 d . . . C63 C 0.8770(11) 0.3463(4) 0.5377(6) 0.071(4) Uani 1 1 d . . . H63 H 0.9011 0.3784 0.5427 0.085 Uiso 1 1 calc R . . C64 C 0.8356(11) 0.3279(4) 0.4855(5) 0.063(3) Uani 1 1 d . . . H64 H 0.8381 0.3477 0.4558 0.076 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 0.0344(4) 0.0395(4) 0.0377(5) -0.0034(3) 0.0036(3) 0.0033(3) Pd2 0.0367(4) 0.0394(5) 0.0511(6) -0.0023(4) 0.0052(4) -0.0013(3) Pd3 0.0400(4) 0.0481(5) 0.0422(5) 0.0093(4) 0.0080(4) 0.0006(4) Pd4 0.0423(4) 0.0443(5) 0.0373(5) 0.0072(4) 0.0048(4) 0.0022(4) Br1 0.0419(6) 0.0410(6) 0.0522(7) -0.0043(5) 0.0092(5) 0.0022(5) Br2 0.0450(6) 0.0639(7) 0.0448(7) 0.0050(5) 0.0031(5) 0.0026(5) Br3 0.0552(7) 0.0907(10) 0.0696(9) -0.0238(7) 0.0240(7) 0.0014(7) Br4 0.0910(11) 0.0998(12) 0.177(2) -0.0126(12) 0.0686(12) -0.0316(9) Br5 0.0586(7) 0.0513(7) 0.0429(7) 0.0141(5) 0.0069(5) 0.0039(5) Br6 0.0504(6) 0.0639(7) 0.0444(7) 0.0052(5) 0.0024(5) -0.0093(5) Br7 0.0529(7) 0.0916(10) 0.0852(11) 0.0108(8) 0.0168(7) 0.0191(7) Br8 0.0657(9) 0.1213(14) 0.1595(19) 0.0204(12) 0.0473(11) 0.0267(9) Cl1 0.077(2) 0.064(2) 0.106(3) 0.0315(19) -0.012(2) -0.0162(17) Cl2 0.0546(17) 0.088(2) 0.067(2) -0.0165(18) -0.0040(15) -0.0316(16) Cl3 0.143(3) 0.079(2) 0.065(2) -0.0264(19) -0.002(2) 0.006(2) Cl4 0.160(4) 0.111(3) 0.081(3) 0.040(2) 0.003(3) -0.025(3) Cl5 0.074(2) 0.141(3) 0.051(2) 0.026(2) 0.0102(17) 0.003(2) Cl6 0.065(2) 0.076(2) 0.144(4) 0.020(2) 0.004(2) -0.0325(18) Cl7 0.119(3) 0.0446(17) 0.075(2) -0.0047(15) 0.033(2) 0.0070(18) Cl8 0.124(3) 0.152(4) 0.071(3) -0.052(3) -0.032(2) 0.047(3) C1 0.066(7) 0.040(6) 0.057(8) -0.019(6) -0.011(6) 0.022(6) C2 0.046(6) 0.044(6) 0.032(6) -0.011(5) 0.005(5) 0.007(5) C3 0.031(5) 0.074(8) 0.041(7) -0.014(6) 0.017(5) -0.003(5) C4 0.039(5) 0.043(6) 0.030(6) -0.005(4) -0.003(5) 0.001(5) C5 0.026(5) 0.050(7) 0.042(7) 0.001(5) 0.004(5) -0.002(5) C6 0.039(6) 0.051(7) 0.050(7) -0.002(6) -0.004(5) -0.008(5) C7 0.052(7) 0.044(7) 0.056(8) -0.010(6) 0.016(6) -0.014(5) C8 0.043(6) 0.052(7) 0.056(8) 0.014(6) 0.002(6) -0.015(5) C9 0.087(9) 0.067(9) 0.049(8) 0.011(7) -0.020(7) -0.020(7) C10 0.048(6) 0.061(8) 0.041(7) -0.006(6) 0.007(5) -0.006(6) C11 0.036(5) 0.044(6) 0.036(6) -0.006(5) -0.001(5) 0.001(5) C12 0.042(6) 0.044(6) 0.059(8) -0.012(5) -0.010(5) 0.008(5) C13 0.051(7) 0.039(6) 0.055(8) -0.019(5) 0.005(6) -0.003(5) C14 0.048(7) 0.071(8) 0.037(7) -0.006(6) -0.004(5) -0.026(6) C15 0.042(6) 0.056(7) 0.064(8) -0.015(6) -0.010(6) 0.000(5) C16 0.041(6) 0.042(6) 0.042(7) -0.014(5) -0.001(5) 0.002(5) C17 0.036(6) 0.036(6) 0.096(10) -0.010(6) 0.000(6) -0.008(5) C18 0.032(6) 0.045(7) 0.088(10) 0.010(6) -0.015(6) -0.013(5) C19 0.054(7) 0.063(8) 0.091(10) -0.020(7) 0.055(7) -0.002(6) C20 0.030(5) 0.047(6) 0.059(8) 0.002(5) 0.009(5) -0.009(5) C21 0.057(7) 0.030(6) 0.052(7) -0.003(5) -0.003(6) -0.005(5) C22 0.050(7) 0.047(7) 0.051(8) -0.005(5) 0.010(6) 0.005(5) C23 0.055(7) 0.062(8) 0.054(8) -0.010(6) 0.008(6) 0.007(6) C24 0.072(8) 0.048(7) 0.060(8) -0.005(6) 0.034(7) 0.006(6) C25 0.090(10) 0.046(7) 0.071(10) -0.002(7) -0.033(8) -0.020(7) C26 0.044(6) 0.045(7) 0.063(8) -0.008(6) 0.006(6) -0.006(5) C27 0.046(6) 0.036(6) 0.059(8) 0.006(5) 0.008(5) -0.003(5) C28 0.072(8) 0.049(8) 0.080(10) -0.009(7) 0.000(7) -0.010(6) C29 0.089(9) 0.049(8) 0.075(10) 0.015(7) -0.001(8) -0.007(7) C30 0.086(9) 0.077(10) 0.063(10) 0.013(8) 0.012(8) -0.020(8) C31 0.081(9) 0.096(11) 0.054(9) 0.020(8) -0.007(7) -0.026(8) C32 0.088(9) 0.054(8) 0.061(9) -0.006(6) 0.006(7) -0.016(7) C33 0.037(6) 0.046(7) 0.067(9) 0.016(6) 0.012(6) 0.013(5) C34 0.036(6) 0.036(6) 0.060(8) 0.005(5) 0.012(5) 0.004(5) C35 0.046(6) 0.053(7) 0.064(8) 0.005(6) 0.002(6) 0.005(5) C36 0.031(5) 0.034(5) 0.046(6) -0.001(5) 0.020(5) 0.001(4) C37 0.034(5) 0.042(6) 0.044(7) 0.005(5) 0.007(5) 0.001(5) C38 0.051(7) 0.052(7) 0.049(8) 0.005(6) 0.016(6) 0.002(5) C39 0.059(7) 0.045(7) 0.062(9) 0.010(6) 0.020(6) 0.003(6) C40 0.046(6) 0.073(9) 0.043(7) 0.011(6) 0.000(5) 0.004(6) C41 0.052(7) 0.086(10) 0.057(9) -0.013(7) 0.008(6) -0.017(7) C42 0.050(6) 0.052(7) 0.054(8) 0.008(6) 0.024(6) -0.009(5) C43 0.033(6) 0.051(7) 0.052(7) 0.012(5) 0.010(5) -0.003(5) C44 0.042(6) 0.042(7) 0.098(10) 0.009(6) 0.029(6) -0.002(5) C45 0.067(9) 0.042(7) 0.143(15) 0.017(8) -0.006(9) 0.000(6) C46 0.050(7) 0.050(7) 0.056(8) 0.010(6) 0.013(6) -0.013(6) C47 0.030(6) 0.070(8) 0.063(8) 0.002(6) 0.015(5) -0.001(5) C48 0.038(6) 0.044(6) 0.060(8) 0.003(5) 0.002(5) -0.001(5) C49 0.046(6) 0.057(7) 0.037(7) 0.013(5) 0.008(5) -0.010(5) C50 0.042(6) 0.045(6) 0.055(8) 0.021(5) 0.004(5) 0.000(5) C51 0.058(7) 0.065(8) 0.054(8) 0.015(6) 0.012(6) 0.016(6) C52 0.034(5) 0.046(6) 0.040(6) 0.010(5) 0.003(5) 0.003(5) C53 0.033(5) 0.047(6) 0.036(6) 0.005(5) 0.001(5) -0.002(5) C54 0.031(5) 0.045(7) 0.061(8) 0.005(5) 0.019(5) 0.000(5) C55 0.050(7) 0.068(8) 0.057(8) 0.011(6) 0.026(6) 0.008(6) C56 0.058(7) 0.052(7) 0.045(7) 0.013(5) 0.026(6) 0.012(6) C57 0.076(8) 0.047(7) 0.059(8) -0.001(6) -0.010(7) -0.015(6) C58 0.052(7) 0.049(7) 0.057(8) 0.005(6) -0.003(6) 0.004(6) C59 0.042(6) 0.040(6) 0.043(7) 0.001(5) 0.006(5) 0.009(5) C60 0.036(6) 0.063(7) 0.042(7) 0.006(6) 0.008(5) -0.001(5) C61 0.063(8) 0.081(10) 0.052(9) 0.009(7) 0.009(6) 0.022(7) C62 0.055(7) 0.098(11) 0.036(7) -0.013(7) 0.001(6) 0.026(7) C63 0.080(9) 0.054(8) 0.072(10) -0.018(7) -0.007(8) 0.001(7) C64 0.079(8) 0.054(8) 0.054(8) 0.011(6) 0.000(7) -0.001(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 C1 2.090(9) . ? Pd1 C2 2.175(10) . ? Pd1 C4 2.186(10) . ? Pd1 Br2 2.5010(14) . ? Pd1 Br1 2.5468(12) . ? Pd2 C17 2.102(9) . ? Pd2 C18 2.162(10) . ? Pd2 C20 2.187(9) . ? Pd2 Br1 2.5248(13) . ? Pd2 Br2 2.5353(12) . ? Pd3 C34 2.085(10) . ? Pd3 C33 2.093(9) . ? Pd3 C36 2.155(9) . ? Pd3 Br6 2.5020(14) . ? Pd3 Br5 2.5428(13) . ? Pd4 C49 2.070(9) . ? Pd4 C50 2.121(10) . ? Pd4 C52 2.141(10) . ? Pd4 Br5 2.5190(14) . ? Pd4 Br6 2.5372(13) . ? Br3 C3 1.971(9) . ? Br4 C19 1.979(10) . ? Br7 C35 1.944(9) . ? Br8 C51 1.905(10) . ? Cl1 C8 1.736(10) . ? Cl2 C14 1.763(9) . ? Cl3 C24 1.748(12) . ? Cl4 C30 1.706(13) . ? Cl5 C40 1.758(11) . ? Cl6 C46 1.724(10) . ? Cl7 C56 1.733(11) . ? Cl8 C62 1.752(12) . ? C1 C2 1.462(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.433(12) . ? C2 C4 1.466(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.504(13) . ? C4 C11 1.503(12) . ? C5 C10 1.320(14) . ? C5 C6 1.379(13) . ? C6 C7 1.361(13) . ? C6 H6 0.9300 . ? C7 C8 1.314(14) . ? C7 H7 0.9300 . ? C8 C9 1.343(15) . ? C9 C10 1.352(14) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.386(12) . ? C11 C12 1.406(12) . ? C12 C13 1.363(12) . ? C12 H12 0.9300 . ? C13 C14 1.371(13) . ? C13 H13 0.9300 . ? C14 C15 1.383(14) . ? C15 C16 1.394(12) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.441(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.424(16) . ? C18 C20 1.469(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.494(14) . ? C20 C27 1.499(14) . ? C21 C26 1.384(13) . ? C21 C22 1.429(14) . ? C22 C23 1.303(14) . ? C22 H22 0.9300 . ? C23 C24 1.337(15) . ? C23 H23 0.9300 . ? C24 C25 1.381(15) . ? C25 C26 1.356(15) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.392(13) . ? C27 C32 1.410(15) . ? C28 C29 1.408(16) . ? C28 H28 0.9300 . ? C29 C30 1.317(16) . ? C29 H29 0.9300 . ? C30 C31 1.378(16) . ? C31 C32 1.354(16) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.324(14) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C36 1.438(13) . ? C34 C35 1.547(13) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C43 1.479(12) . ? C36 C37 1.501(13) . ? C37 C42 1.359(14) . ? C37 C38 1.366(13) . ? C38 C39 1.378(14) . ? C38 H38 0.9300 . ? C39 C40 1.353(15) . ? C39 H39 0.9300 . ? C40 C41 1.361(15) . ? C41 C42 1.354(15) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.363(13) . ? C43 C48 1.406(12) . ? C44 C45 1.393(14) . ? C44 H44 0.9300 . ? C45 C46 1.395(15) . ? C45 H45 0.9300 . ? C46 C47 1.357(13) . ? C47 C48 1.388(13) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.418(14) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C52 1.434(12) . ? C50 C51 1.507(14) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.473(13) . ? C52 C59 1.508(13) . ? C53 C54 1.332(12) . ? C53 C58 1.364(13) . ? C54 C55 1.373(14) . ? C54 H54 0.9300 . ? C55 C56 1.362(14) . ? C55 H55 0.9300 . ? C56 C57 1.325(14) . ? C57 C58 1.406(14) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 C60 1.344(13) . ? C59 C64 1.392(13) . ? C60 C61 1.381(15) . ? C60 H60 0.9300 . ? C61 C62 1.366(16) . ? C61 H61 0.9300 . ? C62 C63 1.309(17) . ? C63 C64 1.417(16) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? 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 C1 Pd1 C2 40.0(4) . . ? C1 Pd1 C4 70.6(4) . . ? C2 Pd1 C4 39.3(3) . . ? C1 Pd1 Br2 94.6(3) . . ? C2 Pd1 Br2 129.6(3) . . ? C4 Pd1 Br2 164.5(2) . . ? C1 Pd1 Br1 163.4(3) . . ? C2 Pd1 Br1 140.4(3) . . ? C4 Pd1 Br1 103.3(2) . . ? Br2 Pd1 Br1 89.67(4) . . ? C17 Pd2 C18 39.5(4) . . ? C17 Pd2 C20 68.4(4) . . ? C18 Pd2 C20 39.5(4) . . ? C17 Pd2 Br1 99.7(3) . . ? C18 Pd2 Br1 134.6(3) . . ? C20 Pd2 Br1 164.7(3) . . ? C17 Pd2 Br2 169.0(3) . . ? C18 Pd2 Br2 134.0(3) . . ? C20 Pd2 Br2 101.5(3) . . ? Br1 Pd2 Br2 89.39(4) . . ? C34 Pd3 C33 36.9(4) . . ? C34 Pd3 C36 39.6(4) . . ? C33 Pd3 C36 68.5(4) . . ? C34 Pd3 Br6 130.5(3) . . ? C33 Pd3 Br6 99.3(3) . . ? C36 Pd3 Br6 167.6(3) . . ? C34 Pd3 Br5 139.8(3) . . ? C33 Pd3 Br5 166.8(3) . . ? C36 Pd3 Br5 103.2(3) . . ? Br6 Pd3 Br5 88.31(4) . . ? C49 Pd4 C50 39.5(4) . . ? C49 Pd4 C52 69.4(4) . . ? C50 Pd4 C52 39.3(3) . . ? C49 Pd4 Br5 98.9(3) . . ? C50 Pd4 Br5 134.5(3) . . ? C52 Pd4 Br5 164.8(3) . . ? C49 Pd4 Br6 167.8(3) . . ? C50 Pd4 Br6 136.5(3) . . ? C52 Pd4 Br6 101.8(2) . . ? Br5 Pd4 Br6 88.06(4) . . ? Pd2 Br1 Pd1 75.68(4) . . ? Pd1 Br2 Pd2 76.30(4) . . ? Pd4 Br5 Pd3 74.04(4) . . ? Pd3 Br6 Pd4 74.43(4) . . ? C2 C1 Pd1 73.1(5) . . ? C2 C1 H1A 116.2 . . ? Pd1 C1 H1A 116.2 . . ? C2 C1 H1B 116.2 . . ? Pd1 C1 H1B 116.2 . . ? H1A C1 H1B 113.2 . . ? C3 C2 C1 118.7(9) . . ? C3 C2 C4 124.4(9) . . ? C1 C2 C4 115.1(9) . . ? C3 C2 Pd1 119.5(7) . . ? C1 C2 Pd1 66.8(5) . . ? C4 C2 Pd1 70.7(5) . . ? C2 C3 Br3 105.0(7) . . ? C2 C3 H3A 110.8 . . ? Br3 C3 H3A 110.7 . . ? C2 C3 H3B 110.7 . . ? Br3 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C2 C4 C5 116.7(8) . . ? C2 C4 C11 120.4(8) . . ? C5 C4 C11 117.6(8) . . ? C2 C4 Pd1 70.0(5) . . ? C5 C4 Pd1 119.9(6) . . ? C11 C4 Pd1 101.7(6) . . ? C10 C5 C6 117.9(10) . . ? C10 C5 C4 120.1(9) . . ? C6 C5 C4 121.9(10) . . ? C7 C6 C5 119.1(11) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C8 C7 C6 121.8(10) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 118.8(11) . . ? C7 C8 Cl1 120.8(9) . . ? C9 C8 Cl1 120.4(10) . . ? C8 C9 C10 120.4(12) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C5 C10 C9 121.8(11) . . ? C5 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C16 C11 C12 118.3(8) . . ? C16 C11 C4 118.6(8) . . ? C12 C11 C4 122.8(8) . . ? C13 C12 C11 120.4(9) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.3(9) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 123.3(9) . . ? C13 C14 Cl2 121.1(8) . . ? C15 C14 Cl2 115.5(9) . . ? C14 C15 C16 116.3(9) . . ? C14 C15 H15 121.9 . . ? C16 C15 H15 121.9 . . ? C11 C16 C15 122.1(9) . . ? C11 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C18 C17 Pd2 72.5(6) . . ? C18 C17 H17A 116.3 . . ? Pd2 C17 H17A 116.3 . . ? C18 C17 H17B 116.4 . . ? Pd2 C17 H17B 116.3 . . ? H17A C17 H17B 113.3 . . ? C19 C18 C17 120.2(10) . . ? C19 C18 C20 127.2(11) . . ? C17 C18 C20 112.0(11) . . ? C19 C18 Pd2 120.7(7) . . ? C17 C18 Pd2 68.0(6) . . ? C20 C18 Pd2 71.2(6) . . ? C18 C19 Br4 104.1(8) . . ? C18 C19 H19A 110.9 . . ? Br4 C19 H19A 110.9 . . ? C18 C19 H19B 110.9 . . ? Br4 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C18 C20 C21 121.6(9) . . ? C18 C20 C27 117.1(10) . . ? C21 C20 C27 116.3(9) . . ? C18 C20 Pd2 69.3(5) . . ? C21 C20 Pd2 104.8(7) . . ? C27 C20 Pd2 117.0(7) . . ? C26 C21 C22 118.6(10) . . ? C26 C21 C20 120.1(10) . . ? C22 C21 C20 121.3(9) . . ? C23 C22 C21 119.6(10) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 122.3(11) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C23 C24 C25 120.0(11) . . ? C23 C24 Cl3 122.6(9) . . ? C25 C24 Cl3 117.3(10) . . ? C26 C25 C24 120.4(11) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 119.0(11) . . ? C25 C26 H26 120.5 . . ? C21 C26 H26 120.5 . . ? C28 C27 C32 113.9(10) . . ? C28 C27 C20 121.0(10) . . ? C32 C27 C20 125.0(10) . . ? C27 C28 C29 122.8(11) . . ? C27 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C30 C29 C28 119.6(12) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.6(13) . . ? C29 C30 Cl4 118.7(11) . . ? C31 C30 Cl4 120.7(11) . . ? C32 C31 C30 120.0(13) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 123.0(11) . . ? C31 C32 H32 118.5 . . ? C27 C32 H32 118.5 . . ? C34 C33 Pd3 71.2(6) . . ? C34 C33 H33A 116.5 . . ? Pd3 C33 H33A 116.5 . . ? C34 C33 H33B 116.5 . . ? Pd3 C33 H33B 116.5 . . ? H33A C33 H33B 113.5 . . ? C33 C34 C36 120.0(9) . . ? C33 C34 C35 117.5(10) . . ? C36 C34 C35 122.0(10) . . ? C33 C34 Pd3 71.9(6) . . ? C36 C34 Pd3 72.8(5) . . ? C35 C34 Pd3 119.9(7) . . ? C34 C35 Br7 106.5(6) . . ? C34 C35 H35A 110.4 . . ? Br7 C35 H35A 110.4 . . ? C34 C35 H35B 110.5 . . ? Br7 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? C34 C36 C43 119.3(9) . . ? C34 C36 C37 122.5(8) . . ? C43 C36 C37 113.3(8) . . ? C34 C36 Pd3 67.6(5) . . ? C43 C36 Pd3 107.6(6) . . ? C37 C36 Pd3 116.7(6) . . ? C42 C37 C38 117.6(10) . . ? C42 C37 C36 121.8(9) . . ? C38 C37 C36 120.5(9) . . ? C37 C38 C39 120.9(11) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C40 C39 C38 119.7(11) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 119.9(11) . . ? C39 C40 Cl5 119.5(10) . . ? C41 C40 Cl5 120.6(10) . . ? C40 C41 C42 119.6(11) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C37 C42 C41 122.1(11) . . ? C37 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C44 C43 C48 118.2(9) . . ? C44 C43 C36 121.8(9) . . ? C48 C43 C36 120.0(9) . . ? C43 C44 C45 120.9(10) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C46 120.5(10) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 118.9(10) . . ? C47 C46 Cl6 119.8(9) . . ? C45 C46 Cl6 121.3(9) . . ? C46 C47 C48 120.8(10) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C47 C48 C43 120.6(9) . . ? C47 C48 H48 119.7 . . ? C43 C48 H48 119.7 . . ? C50 C49 Pd4 72.1(6) . . ? C50 C49 H49A 116.4 . . ? Pd4 C49 H49A 116.4 . . ? C50 C49 H49B 116.4 . . ? Pd4 C49 H49B 116.4 . . ? H49A C49 H49B 113.4 . . ? C49 C50 C52 114.6(10) . . ? C49 C50 C51 119.5(9) . . ? C52 C50 C51 125.2(10) . . ? C49 C50 Pd4 68.3(6) . . ? C52 C50 Pd4 71.1(6) . . ? C51 C50 Pd4 121.8(7) . . ? C50 C51 Br8 111.4(7) . . ? C50 C51 H51A 109.3 . . ? Br8 C51 H51A 109.3 . . ? C50 C51 H51B 109.4 . . ? Br8 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C50 C52 C53 120.0(9) . . ? C50 C52 C59 120.1(9) . . ? C53 C52 C59 115.6(8) . . ? C50 C52 Pd4 69.6(6) . . ? C53 C52 Pd4 103.8(7) . . ? C59 C52 Pd4 116.8(7) . . ? C54 C53 C58 118.6(9) . . ? C54 C53 C52 121.1(9) . . ? C58 C53 C52 120.0(9) . . ? C53 C54 C55 120.1(10) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 122.2(10) . . ? C56 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C57 C56 C55 117.9(10) . . ? C57 C56 Cl7 119.9(9) . . ? C55 C56 Cl7 122.1(9) . . ? C56 C57 C58 120.4(11) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C53 C58 C57 120.3(10) . . ? C53 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C60 C59 C64 116.9(10) . . ? C60 C59 C52 121.3(9) . . ? C64 C59 C52 121.7(9) . . ? C59 C60 C61 121.4(11) . . ? C59 C60 H60 119.3 . . ? C61 C60 H60 119.3 . . ? C62 C61 C60 120.1(11) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C63 C62 C61 121.5(12) . . ? C63 C62 Cl8 119.5(12) . . ? C61 C62 Cl8 119.0(11) . . ? C62 C63 C64 118.2(12) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? C59 C64 C63 121.6(11) . . ? C59 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Pd2 Br1 Pd1 -135.0(3) . . . . ? C18 Pd2 Br1 Pd1 -156.5(5) . . . . ? C20 Pd2 Br1 Pd1 -96.8(10) . . . . ? Br2 Pd2 Br1 Pd1 38.80(4) . . . . ? C1 Pd1 Br1 Pd2 65.9(11) . . . . ? C2 Pd1 Br1 Pd2 147.4(4) . . . . ? C4 Pd1 Br1 Pd2 131.8(2) . . . . ? Br2 Pd1 Br1 Pd2 -39.43(4) . . . . ? C1 Pd1 Br2 Pd2 -124.9(3) . . . . ? C2 Pd1 Br2 Pd2 -146.5(3) . . . . ? C4 Pd1 Br2 Pd2 -107.5(9) . . . . ? Br1 Pd1 Br2 Pd2 39.11(4) . . . . ? C17 Pd2 Br2 Pd1 106.7(18) . . . . ? C18 Pd2 Br2 Pd1 155.6(5) . . . . ? C20 Pd2 Br2 Pd1 129.6(3) . . . . ? Br1 Pd2 Br2 Pd1 -39.52(4) . . . . ? C49 Pd4 Br5 Pd3 -127.5(3) . . . . ? C50 Pd4 Br5 Pd3 -147.4(4) . . . . ? C52 Pd4 Br5 Pd3 -88.6(9) . . . . ? Br6 Pd4 Br5 Pd3 42.42(4) . . . . ? C34 Pd3 Br5 Pd4 150.5(4) . . . . ? C33 Pd3 Br5 Pd4 82.6(14) . . . . ? C36 Pd3 Br5 Pd4 132.2(2) . . . . ? Br6 Pd3 Br5 Pd4 -43.15(4) . . . . ? C34 Pd3 Br6 Pd4 -148.9(4) . . . . ? C33 Pd3 Br6 Pd4 -126.5(3) . . . . ? C36 Pd3 Br6 Pd4 -115.6(11) . . . . ? Br5 Pd3 Br6 Pd4 42.67(4) . . . . ? C49 Pd4 Br6 Pd3 82.2(14) . . . . ? C50 Pd4 Br6 Pd3 147.0(4) . . . . ? C52 Pd4 Br6 Pd3 125.2(3) . . . . ? Br5 Pd4 Br6 Pd3 -43.18(4) . . . . ? C4 Pd1 C1 C2 31.1(5) . . . . ? Br2 Pd1 C1 C2 -153.8(5) . . . . ? Br1 Pd1 C1 C2 101.6(12) . . . . ? Pd1 C1 C2 C3 112.1(8) . . . . ? Pd1 C1 C2 C4 -53.4(7) . . . . ? C1 Pd1 C2 C3 -111.0(10) . . . . ? C4 Pd1 C2 C3 119.4(10) . . . . ? Br2 Pd1 C2 C3 -76.1(9) . . . . ? Br1 Pd1 C2 C3 95.1(8) . . . . ? C4 Pd1 C2 C1 -129.7(8) . . . . ? Br2 Pd1 C2 C1 34.9(7) . . . . ? Br1 Pd1 C2 C1 -154.0(5) . . . . ? C1 Pd1 C2 C4 129.7(8) . . . . ? Br2 Pd1 C2 C4 164.5(4) . . . . ? Br1 Pd1 C2 C4 -24.3(7) . . . . ? C1 C2 C3 Br3 96.0(9) . . . . ? C4 C2 C3 Br3 -99.9(10) . . . . ? Pd1 C2 C3 Br3 174.2(5) . . . . ? C3 C2 C4 C5 1.1(14) . . . . ? C1 C2 C4 C5 165.7(9) . . . . ? Pd1 C2 C4 C5 114.3(8) . . . . ? C3 C2 C4 C11 154.8(9) . . . . ? C1 C2 C4 C11 -40.7(13) . . . . ? Pd1 C2 C4 C11 -92.1(9) . . . . ? C3 C2 C4 Pd1 -113.1(9) . . . . ? C1 C2 C4 Pd1 51.4(7) . . . . ? C1 Pd1 C4 C2 -31.7(5) . . . . ? Br2 Pd1 C4 C2 -50.1(11) . . . . ? Br1 Pd1 C4 C2 164.4(5) . . . . ? C1 Pd1 C4 C5 -141.7(8) . . . . ? C2 Pd1 C4 C5 -110.0(9) . . . . ? Br2 Pd1 C4 C5 -160.1(6) . . . . ? Br1 Pd1 C4 C5 54.4(7) . . . . ? C1 Pd1 C4 C11 86.6(6) . . . . ? C2 Pd1 C4 C11 118.3(8) . . . . ? Br2 Pd1 C4 C11 68.2(11) . . . . ? Br1 Pd1 C4 C11 -77.4(6) . . . . ? C2 C4 C5 C10 107.4(11) . . . . ? C11 C4 C5 C10 -47.0(13) . . . . ? Pd1 C4 C5 C10 -171.4(7) . . . . ? C2 C4 C5 C6 -76.6(12) . . . . ? C11 C4 C5 C6 129.1(10) . . . . ? Pd1 C4 C5 C6 4.6(12) . . . . ? C10 C5 C6 C7 -3.6(14) . . . . ? C4 C5 C6 C7 -179.7(9) . . . . ? C5 C6 C7 C8 3.6(16) . . . . ? C6 C7 C8 C9 -2.4(17) . . . . ? C6 C7 C8 Cl1 178.5(8) . . . . ? C7 C8 C9 C10 1.4(18) . . . . ? Cl1 C8 C9 C10 -179.6(9) . . . . ? C6 C5 C10 C9 2.6(16) . . . . ? C4 C5 C10 C9 178.9(10) . . . . ? C8 C9 C10 C5 -1.6(18) . . . . ? C2 C4 C11 C16 154.7(9) . . . . ? C5 C4 C11 C16 -51.9(13) . . . . ? Pd1 C4 C11 C16 81.2(9) . . . . ? C2 C4 C11 C12 -31.2(15) . . . . ? C5 C4 C11 C12 122.2(11) . . . . ? Pd1 C4 C11 C12 -104.7(10) . . . . ? C16 C11 C12 C13 -5.2(16) . . . . ? C4 C11 C12 C13 -179.4(10) . . . . ? C11 C12 C13 C14 3.1(17) . . . . ? C12 C13 C14 C15 -1.4(18) . . . . ? C12 C13 C14 Cl2 -178.4(9) . . . . ? C13 C14 C15 C16 1.8(17) . . . . ? Cl2 C14 C15 C16 178.9(8) . . . . ? C12 C11 C16 C15 5.7(16) . . . . ? C4 C11 C16 C15 -179.9(10) . . . . ? C14 C15 C16 C11 -4.0(17) . . . . ? C20 Pd2 C17 C18 34.4(7) . . . . ? Br1 Pd2 C17 C18 -155.7(6) . . . . ? Br2 Pd2 C17 C18 59(2) . . . . ? Pd2 C17 C18 C19 113.8(9) . . . . ? Pd2 C17 C18 C20 -57.4(7) . . . . ? C17 Pd2 C18 C19 -113.0(12) . . . . ? C20 Pd2 C18 C19 122.7(12) . . . . ? Br1 Pd2 C18 C19 -78.3(11) . . . . ? Br2 Pd2 C18 C19 80.1(10) . . . . ? C20 Pd2 C18 C17 -124.3(10) . . . . ? Br1 Pd2 C18 C17 34.6(9) . . . . ? Br2 Pd2 C18 C17 -166.9(5) . . . . ? C17 Pd2 C18 C20 124.3(10) . . . . ? Br1 Pd2 C18 C20 159.0(5) . . . . ? Br2 Pd2 C18 C20 -42.6(8) . . . . ? C17 C18 C19 Br4 95.9(10) . . . . ? C20 C18 C19 Br4 -94.3(11) . . . . ? Pd2 C18 C19 Br4 176.8(5) . . . . ? C19 C18 C20 C21 150.1(10) . . . . ? C17 C18 C20 C21 -39.5(12) . . . . ? Pd2 C18 C20 C21 -95.1(9) . . . . ? C19 C18 C20 C27 -4.2(14) . . . . ? C17 C18 C20 C27 166.3(8) . . . . ? Pd2 C18 C20 C27 110.6(8) . . . . ? C19 C18 C20 Pd2 -114.8(10) . . . . ? C17 C18 C20 Pd2 55.7(7) . . . . ? C17 Pd2 C20 C18 -34.4(7) . . . . ? Br1 Pd2 C20 C18 -75.3(13) . . . . ? Br2 Pd2 C20 C18 150.2(6) . . . . ? C17 Pd2 C20 C21 84.3(7) . . . . ? C18 Pd2 C20 C21 118.7(10) . . . . ? Br1 Pd2 C20 C21 43.4(14) . . . . ? Br2 Pd2 C20 C21 -91.1(6) . . . . ? C17 Pd2 C20 C27 -145.1(9) . . . . ? C18 Pd2 C20 C27 -110.8(11) . . . . ? Br1 Pd2 C20 C27 173.9(6) . . . . ? Br2 Pd2 C20 C27 39.4(8) . . . . ? C18 C20 C21 C26 -40.1(14) . . . . ? C27 C20 C21 C26 114.3(11) . . . . ? Pd2 C20 C21 C26 -114.7(9) . . . . ? C18 C20 C21 C22 141.5(10) . . . . ? C27 C20 C21 C22 -64.0(13) . . . . ? Pd2 C20 C21 C22 66.9(10) . . . . ? C26 C21 C22 C23 -4.9(16) . . . . ? C20 C21 C22 C23 173.5(10) . . . . ? C21 C22 C23 C24 4.7(18) . . . . ? C22 C23 C24 C25 -1.6(19) . . . . ? C22 C23 C24 Cl3 179.5(9) . . . . ? C23 C24 C25 C26 -1.4(18) . . . . ? Cl3 C24 C25 C26 177.5(9) . . . . ? C24 C25 C26 C21 1.1(17) . . . . ? C22 C21 C26 C25 2.0(16) . . . . ? C20 C21 C26 C25 -176.5(10) . . . . ? C18 C20 C27 C28 125.1(11) . . . . ? C21 C20 C27 C28 -30.6(14) . . . . ? Pd2 C20 C27 C28 -155.5(8) . . . . ? C18 C20 C27 C32 -53.0(14) . . . . ? C21 C20 C27 C32 151.4(11) . . . . ? Pd2 C20 C27 C32 26.4(14) . . . . ? C32 C27 C28 C29 -0.3(17) . . . . ? C20 C27 C28 C29 -178.6(11) . . . . ? C27 C28 C29 C30 -2(2) . . . . ? C28 C29 C30 C31 4(2) . . . . ? C28 C29 C30 Cl4 -173.3(10) . . . . ? C29 C30 C31 C32 -4(2) . . . . ? Cl4 C30 C31 C32 173.7(11) . . . . ? C30 C31 C32 C27 1(2) . . . . ? C28 C27 C32 C31 0.8(18) . . . . ? C20 C27 C32 C31 179.1(11) . . . . ? C36 Pd3 C33 C34 31.3(6) . . . . ? Br6 Pd3 C33 C34 -151.2(6) . . . . ? Br5 Pd3 C33 C34 84.1(15) . . . . ? Pd3 C33 C34 C36 -56.8(8) . . . . ? Pd3 C33 C34 C35 114.9(8) . . . . ? C36 Pd3 C34 C33 -130.7(9) . . . . ? Br6 Pd3 C34 C33 38.7(8) . . . . ? Br5 Pd3 C34 C33 -159.4(5) . . . . ? C33 Pd3 C34 C36 130.7(9) . . . . ? Br6 Pd3 C34 C36 169.4(4) . . . . ? Br5 Pd3 C34 C36 -28.7(7) . . . . ? C33 Pd3 C34 C35 -111.8(11) . . . . ? C36 Pd3 C34 C35 117.5(11) . . . . ? Br6 Pd3 C34 C35 -73.1(9) . . . . ? Br5 Pd3 C34 C35 88.8(9) . . . . ? C33 C34 C35 Br7 72.4(10) . . . . ? C36 C34 C35 Br7 -116.2(9) . . . . ? Pd3 C34 C35 Br7 156.3(5) . . . . ? C33 C34 C36 C43 -42.0(14) . . . . ? C35 C34 C36 C43 146.8(9) . . . . ? Pd3 C34 C36 C43 -98.3(8) . . . . ? C33 C34 C36 C37 164.6(9) . . . . ? C35 C34 C36 C37 -6.6(14) . . . . ? Pd3 C34 C36 C37 108.3(9) . . . . ? C33 C34 C36 Pd3 56.3(9) . . . . ? C35 C34 C36 Pd3 -114.9(9) . . . . ? C33 Pd3 C36 C34 -29.3(6) . . . . ? Br6 Pd3 C36 C34 -40.9(14) . . . . ? Br5 Pd3 C36 C34 161.4(5) . . . . ? C34 Pd3 C36 C43 115.1(9) . . . . ? C33 Pd3 C36 C43 85.7(7) . . . . ? Br6 Pd3 C36 C43 74.2(13) . . . . ? Br5 Pd3 C36 C43 -83.5(6) . . . . ? C34 Pd3 C36 C37 -116.3(9) . . . . ? C33 Pd3 C36 C37 -145.7(8) . . . . ? Br6 Pd3 C36 C37 -157.2(8) . . . . ? Br5 Pd3 C36 C37 45.1(7) . . . . ? C34 C36 C37 C42 126.1(11) . . . . ? C43 C36 C37 C42 -28.7(13) . . . . ? Pd3 C36 C37 C42 -154.5(8) . . . . ? C34 C36 C37 C38 -57.7(13) . . . . ? C43 C36 C37 C38 147.4(9) . . . . ? Pd3 C36 C37 C38 21.6(11) . . . . ? C42 C37 C38 C39 2.3(15) . . . . ? C36 C37 C38 C39 -174.0(9) . . . . ? C37 C38 C39 C40 0.7(16) . . . . ? C38 C39 C40 C41 -3.0(17) . . . . ? C38 C39 C40 Cl5 175.8(8) . . . . ? C39 C40 C41 C42 2.1(17) . . . . ? Cl5 C40 C41 C42 -176.7(8) . . . . ? C38 C37 C42 C41 -3.2(16) . . . . ? C36 C37 C42 C41 173.0(9) . . . . ? C40 C41 C42 C37 1.1(17) . . . . ? C34 C36 C43 C44 -47.7(15) . . . . ? C37 C36 C43 C44 108.1(12) . . . . ? Pd3 C36 C43 C44 -121.4(10) . . . . ? C34 C36 C43 C48 131.0(11) . . . . ? C37 C36 C43 C48 -73.3(12) . . . . ? Pd3 C36 C43 C48 57.3(11) . . . . ? C48 C43 C44 C45 1.1(18) . . . . ? C36 C43 C44 C45 179.8(12) . . . . ? C43 C44 C45 C46 0(2) . . . . ? C44 C45 C46 C47 -2(2) . . . . ? C44 C45 C46 Cl6 177.9(10) . . . . ? C45 C46 C47 C48 1.9(18) . . . . ? Cl6 C46 C47 C48 -177.6(9) . . . . ? C46 C47 C48 C43 -0.7(17) . . . . ? C44 C43 C48 C47 -0.9(17) . . . . ? C36 C43 C48 C47 -179.6(10) . . . . ? C52 Pd4 C49 C50 32.5(6) . . . . ? Br5 Pd4 C49 C50 -157.7(5) . . . . ? Br6 Pd4 C49 C50 78.0(16) . . . . ? Pd4 C49 C50 C52 -55.6(8) . . . . ? Pd4 C49 C50 C51 115.2(9) . . . . ? C52 Pd4 C50 C49 -127.5(9) . . . . ? Br5 Pd4 C50 C49 31.8(7) . . . . ? Br6 Pd4 C50 C49 -162.5(5) . . . . ? C49 Pd4 C50 C52 127.5(9) . . . . ? Br5 Pd4 C50 C52 159.3(5) . . . . ? Br6 Pd4 C50 C52 -35.0(8) . . . . ? C49 Pd4 C50 C51 -112.1(10) . . . . ? C52 Pd4 C50 C51 120.4(12) . . . . ? Br5 Pd4 C50 C51 -80.3(9) . . . . ? Br6 Pd4 C50 C51 85.3(8) . . . . ? C49 C50 C51 Br8 73.6(11) . . . . ? C52 C50 C51 Br8 -116.6(10) . . . . ? Pd4 C50 C51 Br8 155.0(5) . . . . ? C49 C50 C52 C53 -40.4(13) . . . . ? C51 C50 C52 C53 149.3(10) . . . . ? Pd4 C50 C52 C53 -94.6(9) . . . . ? C49 C50 C52 C59 164.0(9) . . . . ? C51 C50 C52 C59 -6.2(15) . . . . ? Pd4 C50 C52 C59 109.9(9) . . . . ? C49 C50 C52 Pd4 54.1(7) . . . . ? C51 C50 C52 Pd4 -116.1(10) . . . . ? C49 Pd4 C52 C50 -32.6(6) . . . . ? Br5 Pd4 C52 C50 -74.2(12) . . . . ? Br6 Pd4 C52 C50 156.2(6) . . . . ? C49 Pd4 C52 C53 84.6(6) . . . . ? C50 Pd4 C52 C53 117.2(9) . . . . ? Br5 Pd4 C52 C53 43.0(13) . . . . ? Br6 Pd4 C52 C53 -86.6(6) . . . . ? C49 Pd4 C52 C59 -147.0(8) . . . . ? C50 Pd4 C52 C59 -114.3(10) . . . . ? Br5 Pd4 C52 C59 171.5(6) . . . . ? Br6 Pd4 C52 C59 41.9(7) . . . . ? C50 C52 C53 C54 146.7(10) . . . . ? C59 C52 C53 C54 -56.7(13) . . . . ? Pd4 C52 C53 C54 72.5(10) . . . . ? C50 C52 C53 C58 -39.2(14) . . . . ? C59 C52 C53 C58 117.4(10) . . . . ? Pd4 C52 C53 C58 -113.4(9) . . . . ? C58 C53 C54 C55 4.7(16) . . . . ? C52 C53 C54 C55 178.8(10) . . . . ? C53 C54 C55 C56 1.1(17) . . . . ? C54 C55 C56 C57 -4.4(17) . . . . ? C54 C55 C56 Cl7 178.6(8) . . . . ? C55 C56 C57 C58 1.9(17) . . . . ? Cl7 C56 C57 C58 179.0(9) . . . . ? C54 C53 C58 C57 -7.1(16) . . . . ? C52 C53 C58 C57 178.7(10) . . . . ? C56 C57 C58 C53 3.8(17) . . . . ? C50 C52 C59 C60 130.4(10) . . . . ? C53 C52 C59 C60 -26.3(13) . . . . ? Pd4 C52 C59 C60 -148.8(8) . . . . ? C50 C52 C59 C64 -52.8(14) . . . . ? C53 C52 C59 C64 150.6(10) . . . . ? Pd4 C52 C59 C64 28.1(12) . . . . ? C64 C59 C60 C61 4.1(15) . . . . ? C52 C59 C60 C61 -178.9(9) . . . . ? C59 C60 C61 C62 -0.1(17) . . . . ? C60 C61 C62 C63 -2.0(18) . . . . ? C60 C61 C62 Cl8 178.0(8) . . . . ? C61 C62 C63 C64 -0.1(19) . . . . ? Cl8 C62 C63 C64 179.9(9) . . . . ? C60 C59 C64 C63 -6.3(16) . . . . ? C52 C59 C64 C63 176.7(10) . . . . ? C62 C63 C64 C59 4.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.159 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.162