# 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 _publ_contact_author_name 'Pak-Hing Leung' _publ_contact_author_email PAKHING@NTU.EDU.SG _publ_section_title ; Steric effects on control of endo/exo-selectivity in asymmetric cycloaddition reaction of 3,4-dimethyl-1-phenylarsole ; loop_ _publ_author_name 'Pak-Hing Leung' 'Weiqiao Deng' 'Rui-Feng Lu' 'Mengtao Ma' 'Sumod A Pullarkat' # Attachment 'leung259.cif' data_leung259 _database_code_depnum_ccdc_archive 'CCDC 734386' #TrackingRef 'leung259.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 As I2 P Pd' _chemical_formula_sum 'C27 H28 As I2 P Pd' _chemical_formula_weight 818.58 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.3021(4) _cell_length_b 14.7810(7) _cell_length_c 18.3942(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2801.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6877 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.41 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 4.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4650 _exptl_absorpt_correction_T_max 0.7906 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 37334 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8543 _reflns_number_gt 7699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0463P)^2^+5.0778P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(14) _refine_ls_number_reflns 8543 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.28788(4) 0.64689(3) 1.00932(2) 0.02015(8) Uani 1 1 d . . . As1 As 0.26144(5) 0.72467(3) 0.89869(3) 0.02032(11) Uani 1 1 d . . . I1 I 0.22677(5) 0.79923(3) 1.07545(2) 0.03684(11) Uani 1 1 d . . . I2 I 0.32126(4) 0.55526(3) 1.131522(19) 0.02882(9) Uani 1 1 d . . . P1 P 0.31252(14) 0.52394(9) 0.93506(7) 0.0200(2) Uani 1 1 d . . . C1 C 0.2984(5) 0.8491(3) 0.8753(3) 0.0202(9) Uani 1 1 d . . . C2 C 0.4254(6) 0.8801(4) 0.8683(3) 0.0278(11) Uani 1 1 d . . . H2 H 0.4961 0.8404 0.8773 0.033 Uiso 1 1 calc R . . C3 C 0.4483(6) 0.9690(4) 0.8482(4) 0.0317(13) Uani 1 1 d . . . H3 H 0.5348 0.9903 0.8431 0.038 Uiso 1 1 calc R . . C4 C 0.3436(6) 1.0276(4) 0.8354(3) 0.0288(12) Uani 1 1 d . . . H4 H 0.3592 1.0884 0.8210 0.035 Uiso 1 1 calc R . . C5 C 0.2191(6) 0.9970(4) 0.8436(3) 0.0292(12) Uani 1 1 d . . . H5 H 0.1486 1.0373 0.8359 0.035 Uiso 1 1 calc R . . C6 C 0.1944(6) 0.9079(4) 0.8631(3) 0.0268(11) Uani 1 1 d . . . H6 H 0.1076 0.8871 0.8680 0.032 Uiso 1 1 calc R . . C7 C 0.0995(6) 0.6946(4) 0.8473(3) 0.0229(10) Uani 1 1 d . . . H7 H 0.0197 0.7260 0.8653 0.028 Uiso 1 1 calc R . . C8 C 0.1377(6) 0.7154(4) 0.7694(3) 0.0249(11) Uani 1 1 d . . . C9 C 0.0377(7) 0.7568(4) 0.7194(3) 0.0347(14) Uani 1 1 d . . . H9A H 0.0671 0.7515 0.6689 0.052 Uiso 1 1 calc R . . H9B H 0.0262 0.8208 0.7316 0.052 Uiso 1 1 calc R . . H9C H -0.0452 0.7250 0.7251 0.052 Uiso 1 1 calc R . . C10 C 0.2580(6) 0.6870(3) 0.7537(3) 0.0235(10) Uani 1 1 d . . . C11 C 0.3268(7) 0.6902(4) 0.6818(3) 0.0319(13) Uani 1 1 d . . . H11A H 0.3402 0.6285 0.6638 0.048 Uiso 1 1 calc R . . H11B H 0.4110 0.7202 0.6877 0.048 Uiso 1 1 calc R . . H11C H 0.2741 0.7241 0.6467 0.048 Uiso 1 1 calc R . . C12 C 0.3216(6) 0.6446(3) 0.8189(3) 0.0223(10) Uani 1 1 d . . . H12 H 0.4178 0.6372 0.8153 0.027 Uiso 1 1 calc R . . C13 C 0.2471(5) 0.5596(3) 0.8455(3) 0.0210(9) Uani 1 1 d . . . H13 H 0.2534 0.5094 0.8092 0.025 Uiso 1 1 calc R . . C14 C 0.1015(6) 0.5890(4) 0.8574(3) 0.0231(10) Uani 1 1 d . . . H14 H 0.0767 0.5748 0.9087 0.028 Uiso 1 1 calc R . . C15 C 0.0079(6) 0.5398(4) 0.8065(4) 0.0305(12) Uani 1 1 d . . . H15A H 0.0297 0.5541 0.7560 0.046 Uiso 1 1 calc R . . H15B H -0.0812 0.5593 0.8168 0.046 Uiso 1 1 calc R . . H15C H 0.0151 0.4744 0.8142 0.046 Uiso 1 1 calc R . . C16 C 0.2182(6) 0.4219(3) 0.9560(3) 0.0239(10) Uani 1 1 d . . . C17 C 0.1050(6) 0.4276(4) 0.9982(3) 0.0262(11) Uani 1 1 d . . . H17 H 0.0795 0.4839 1.0186 0.031 Uiso 1 1 calc R . . C18 C 0.0307(6) 0.3512(4) 1.0101(3) 0.0310(12) Uani 1 1 d . . . H18 H -0.0462 0.3550 1.0384 0.037 Uiso 1 1 calc R . . C19 C 0.0686(7) 0.2683(4) 0.9803(4) 0.0352(14) Uani 1 1 d . . . H19 H 0.0168 0.2159 0.9879 0.042 Uiso 1 1 calc R . . C20 C 0.1793(7) 0.2625(4) 0.9407(4) 0.0373(14) Uani 1 1 d . . . H20 H 0.2055 0.2055 0.9220 0.045 Uiso 1 1 calc R . . C21 C 0.2557(6) 0.3385(4) 0.9269(3) 0.0286(11) Uani 1 1 d . . . H21 H 0.3320 0.3337 0.8981 0.034 Uiso 1 1 calc R . . C22 C 0.4778(5) 0.4851(3) 0.9190(3) 0.0218(10) Uani 1 1 d . . . C23 C 0.5202(6) 0.4554(4) 0.8506(3) 0.0305(12) Uani 1 1 d . . . H23 H 0.4617 0.4563 0.8107 0.037 Uiso 1 1 calc R . . C24 C 0.6455(7) 0.4249(5) 0.8403(4) 0.0381(16) Uani 1 1 d . . . H24 H 0.6725 0.4038 0.7939 0.046 Uiso 1 1 calc R . . C25 C 0.7321(6) 0.4253(4) 0.8985(3) 0.0310(12) Uani 1 1 d . . . H25 H 0.8187 0.4050 0.8918 0.037 Uiso 1 1 calc R . . C26 C 0.6919(6) 0.4552(4) 0.9658(3) 0.0327(13) Uani 1 1 d . . . H26 H 0.7507 0.4552 1.0055 0.039 Uiso 1 1 calc R . . C27 C 0.5654(6) 0.4853(4) 0.9755(3) 0.0269(11) Uani 1 1 d . . . H27 H 0.5389 0.5064 1.0219 0.032 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 0.02501(19) 0.01753(16) 0.01792(15) -0.00045(13) -0.00129(14) 0.00003(14) As1 0.0253(3) 0.0163(2) 0.0193(2) 0.00029(17) -0.0008(2) 0.00018(19) I1 0.0506(3) 0.02411(17) 0.0358(2) -0.01007(14) 0.00060(18) 0.00328(17) I2 0.02672(18) 0.03647(19) 0.02328(15) 0.00873(14) -0.00237(13) -0.00295(15) P1 0.0255(7) 0.0154(5) 0.0191(5) 0.0008(4) 0.0009(5) 0.0001(5) C1 0.021(2) 0.018(2) 0.022(2) 0.0027(17) -0.0033(18) 0.0020(19) C2 0.023(3) 0.028(3) 0.032(3) 0.002(2) -0.002(2) 0.004(2) C3 0.023(3) 0.032(3) 0.040(3) 0.000(3) 0.002(2) -0.005(2) C4 0.038(3) 0.017(2) 0.031(3) 0.001(2) -0.002(2) -0.003(2) C5 0.036(3) 0.027(3) 0.025(2) -0.001(2) -0.004(2) 0.007(2) C6 0.023(3) 0.028(3) 0.030(3) -0.005(2) 0.000(2) 0.003(2) C7 0.026(3) 0.023(2) 0.020(2) -0.0011(19) 0.0011(19) 0.005(2) C8 0.032(3) 0.020(2) 0.022(2) 0.0013(19) -0.005(2) 0.002(2) C9 0.036(3) 0.036(3) 0.033(3) 0.007(3) -0.008(3) 0.005(3) C10 0.031(3) 0.018(2) 0.022(2) -0.0003(17) -0.001(2) 0.003(2) C11 0.047(4) 0.024(3) 0.024(2) 0.002(2) 0.009(3) 0.006(3) C12 0.024(2) 0.019(2) 0.024(2) -0.0031(19) 0.0011(19) -0.001(2) C13 0.026(3) 0.016(2) 0.021(2) 0.0012(17) 0.0039(18) 0.0024(19) C14 0.026(3) 0.025(3) 0.018(2) -0.0004(19) -0.0011(19) -0.001(2) C15 0.021(3) 0.026(3) 0.044(3) -0.004(3) -0.005(2) -0.006(2) C16 0.034(3) 0.021(2) 0.017(2) 0.0041(17) -0.001(2) 0.002(2) C17 0.033(3) 0.021(2) 0.025(2) 0.000(2) 0.000(2) 0.000(2) C18 0.029(3) 0.031(3) 0.033(3) 0.005(3) 0.002(2) -0.003(2) C19 0.036(3) 0.026(3) 0.043(3) 0.006(3) -0.001(3) -0.007(3) C20 0.042(4) 0.018(3) 0.053(4) -0.004(3) -0.004(3) -0.001(3) C21 0.031(3) 0.024(3) 0.031(3) 0.000(2) 0.001(2) -0.001(2) C22 0.024(3) 0.012(2) 0.030(3) 0.0022(19) 0.004(2) 0.0016(18) C23 0.033(3) 0.034(3) 0.025(3) 0.003(2) 0.002(2) 0.007(3) C24 0.043(4) 0.036(3) 0.036(3) 0.010(3) 0.018(3) 0.009(3) C25 0.028(3) 0.026(3) 0.039(3) 0.002(2) 0.005(3) 0.009(2) C26 0.026(3) 0.032(3) 0.040(3) -0.002(2) -0.004(2) 0.002(2) C27 0.020(3) 0.024(3) 0.036(3) 0.001(2) 0.000(2) 0.000(2) _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 P1 2.2875(13) . ? Pd1 As1 2.3532(6) . ? Pd1 I1 2.6357(5) . ? Pd1 I2 2.6466(5) . ? As1 C1 1.927(5) . ? As1 C7 1.968(6) . ? As1 C12 1.985(5) . ? P1 C22 1.821(6) . ? P1 C16 1.835(6) . ? P1 C13 1.857(5) . ? C1 C2 1.392(8) . ? C1 C6 1.398(7) . ? C2 C3 1.386(9) . ? C3 C4 1.403(9) . ? C4 C5 1.369(9) . ? C5 C6 1.388(8) . ? C7 C8 1.517(7) . ? C7 C14 1.572(8) . ? C8 C10 1.340(8) . ? C8 C9 1.512(8) . ? C10 C11 1.502(7) . ? C10 C12 1.504(7) . ? C12 C13 1.551(7) . ? C13 C14 1.578(8) . ? C14 C15 1.528(8) . ? C16 C21 1.398(7) . ? C16 C17 1.403(8) . ? C17 C18 1.382(8) . ? C18 C19 1.397(9) . ? C19 C20 1.357(10) . ? C20 C21 1.395(9) . ? C22 C27 1.375(8) . ? C22 C23 1.403(8) . ? C23 C24 1.380(9) . ? C24 C25 1.393(10) . ? C25 C26 1.378(9) . ? C26 C27 1.388(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 As1 83.37(4) . . ? P1 Pd1 I1 168.76(4) . . ? As1 Pd1 I1 87.36(2) . . ? P1 Pd1 I2 94.95(4) . . ? As1 Pd1 I2 178.21(2) . . ? I1 Pd1 I2 94.376(18) . . ? C1 As1 C7 106.0(2) . . ? C1 As1 C12 110.1(2) . . ? C7 As1 C12 77.0(2) . . ? C1 As1 Pd1 129.52(15) . . ? C7 As1 Pd1 113.77(16) . . ? C12 As1 Pd1 108.17(15) . . ? C22 P1 C16 105.7(2) . . ? C22 P1 C13 106.6(2) . . ? C16 P1 C13 103.2(2) . . ? C22 P1 Pd1 116.80(18) . . ? C16 P1 Pd1 117.95(17) . . ? C13 P1 Pd1 105.33(16) . . ? C2 C1 C6 120.1(5) . . ? C2 C1 As1 121.3(4) . . ? C6 C1 As1 118.6(4) . . ? C3 C2 C1 119.8(5) . . ? C2 C3 C4 120.0(6) . . ? C5 C4 C3 119.9(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C1 119.4(5) . . ? C8 C7 C14 108.0(4) . . ? C8 C7 As1 100.8(4) . . ? C14 C7 As1 99.0(4) . . ? C10 C8 C9 128.7(5) . . ? C10 C8 C7 112.4(5) . . ? C9 C8 C7 118.7(5) . . ? C8 C10 C11 128.1(5) . . ? C8 C10 C12 111.2(5) . . ? C11 C10 C12 120.7(5) . . ? C10 C12 C13 112.0(4) . . ? C10 C12 As1 101.8(3) . . ? C13 C12 As1 95.5(3) . . ? C12 C13 C14 106.9(4) . . ? C12 C13 P1 109.3(4) . . ? C14 C13 P1 107.5(3) . . ? C15 C14 C7 113.1(5) . . ? C15 C14 C13 112.6(4) . . ? C7 C14 C13 105.7(4) . . ? C21 C16 C17 119.6(5) . . ? C21 C16 P1 119.8(4) . . ? C17 C16 P1 120.4(4) . . ? C18 C17 C16 119.9(5) . . ? C17 C18 C19 120.0(6) . . ? C20 C19 C18 120.0(6) . . ? C19 C20 C21 121.5(6) . . ? C20 C21 C16 118.9(6) . . ? C27 C22 C23 118.2(5) . . ? C27 C22 P1 119.4(4) . . ? C23 C22 P1 122.3(4) . . ? C24 C23 C22 121.1(6) . . ? C23 C24 C25 119.5(6) . . ? C26 C25 C24 119.9(6) . . ? C25 C26 C27 120.0(6) . . ? C22 C27 C26 121.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.697 _refine_diff_density_min -2.311 _refine_diff_density_rms 0.323 # Attachment 'leung256t.cif' data_leung256t _database_code_depnum_ccdc_archive 'CCDC 734387' #TrackingRef 'leung256t.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 As I2 P Pd' _chemical_formula_sum 'C27 H28 As I2 P Pd' _chemical_formula_weight 818.58 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.0804(5) _cell_length_b 9.1106(9) _cell_length_c 9.3713(5) _cell_angle_alpha 100.727(4) _cell_angle_beta 110.589(3) _cell_angle_gamma 98.244(4) _cell_volume 694.44(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9713 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 390 _exptl_absorpt_coefficient_mu 4.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4912 _exptl_absorpt_correction_T_max 0.6362 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 15286 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.77 _reflns_number_total 7491 _reflns_number_gt 6512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0458P)^2^+1.7631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(15) _refine_ls_number_reflns 7491 _refine_ls_number_parameters 290 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.092 _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 Pd1 Pd 0.40460(5) 0.97182(5) -0.13242(5) 0.02018(11) Uani 1 1 d . . . As1 As 0.20548(8) 0.77300(7) -0.13838(8) 0.02132(15) Uani 1 1 d . . . I1 I 0.66001(7) 1.16536(6) -0.11760(7) 0.04705(17) Uani 1 1 d . . . I2 I 0.30924(6) 0.85885(6) -0.43937(5) 0.03285(13) Uani 1 1 d . . . P1 P 0.4331(2) 1.0493(2) 0.1256(2) 0.0206(3) Uani 1 1 d . . . C1 C 0.1533(10) 0.5689(8) -0.2665(9) 0.0304(15) Uani 1 1 d . . . C2 C 0.2644(14) 0.4753(10) -0.2284(13) 0.048(2) Uani 1 1 d . . . H2 H 0.3624 0.5144 -0.1380 0.058 Uiso 1 1 calc R . . C3 C 0.2352(17) 0.3303(11) -0.3177(16) 0.061(3) Uani 1 1 d U . . H3 H 0.3114 0.2685 -0.2903 0.074 Uiso 1 1 calc R . . C4 C 0.0949(19) 0.2756(13) -0.4471(18) 0.074(3) Uani 1 1 d U . . H4 H 0.0724 0.1735 -0.5088 0.089 Uiso 1 1 calc R . . C5 C -0.0174(17) 0.3664(15) -0.4916(18) 0.081(4) Uani 1 1 d U . . H5 H -0.1112 0.3285 -0.5863 0.097 Uiso 1 1 calc R . . C6 C 0.0078(13) 0.5042(11) -0.4014(12) 0.049(2) Uani 1 1 d U . . H6 H -0.0730 0.5617 -0.4271 0.058 Uiso 1 1 calc R . . C7 C 0.0083(9) 0.8319(8) -0.1193(8) 0.0251(14) Uani 1 1 d . . . H7 H -0.0721 0.8457 -0.2181 0.030 Uiso 1 1 calc R . . C8 C -0.0488(9) 0.7031(8) -0.0607(9) 0.0272(14) Uani 1 1 d . . . C9 C -0.2275(10) 0.6276(11) -0.1227(12) 0.041(2) Uani 1 1 d . . . H9A H -0.2617 0.5627 -0.2298 0.062 Uiso 1 1 calc R . . H9B H -0.2900 0.7069 -0.1244 0.062 Uiso 1 1 calc R . . H9C H -0.2460 0.5646 -0.0539 0.062 Uiso 1 1 calc R . . C10 C 0.0739(9) 0.6731(8) 0.0546(9) 0.0265(14) Uani 1 1 d . . . C11 C 0.0654(10) 0.5551(9) 0.1455(10) 0.0354(17) Uani 1 1 d . . . H11A H -0.0465 0.5212 0.1343 0.053 Uiso 1 1 calc R . . H11B H 0.1343 0.5999 0.2572 0.053 Uiso 1 1 calc R . . H11C H 0.1027 0.4671 0.1045 0.053 Uiso 1 1 calc R . . C12 C 0.2336(8) 0.7708(7) 0.0823(8) 0.0224(13) Uani 1 1 d U . . H12 H 0.3300 0.7339 0.1418 0.027 Uiso 1 1 calc R . . C13 C 0.2462(7) 0.9449(7) 0.1370(7) 0.0176(11) Uani 1 1 d U . . H13 H 0.2512 0.9725 0.2472 0.021 Uiso 1 1 calc R . . C14 C 0.0872(8) 0.9784(8) 0.0180(9) 0.0241(13) Uani 1 1 d U . . H14 H 0.0121 0.9857 0.0742 0.029 Uiso 1 1 calc R . . C15 C 0.1008(9) 1.1239(9) -0.0396(10) 0.0316(17) Uani 1 1 d . . . H15A H 0.1787 1.1254 -0.0901 0.047 Uiso 1 1 calc R . . H15B H 0.1374 1.2140 0.0502 0.047 Uiso 1 1 calc R . . H15C H -0.0051 1.1257 -0.1158 0.047 Uiso 1 1 calc R . . C16 C 0.6003(7) 0.9856(7) 0.2564(8) 0.0224(13) Uani 1 1 d . . . C17 C 0.6305(9) 1.0113(10) 0.4156(9) 0.0300(15) Uani 1 1 d . . . H17 H 0.5632 1.0604 0.4567 0.036 Uiso 1 1 calc R . . C18 C 0.7602(10) 0.9649(10) 0.5160(10) 0.0373(19) Uani 1 1 d . . . H18 H 0.7801 0.9814 0.6249 0.045 Uiso 1 1 calc R . . C19 C 0.8585(10) 0.8957(10) 0.4567(11) 0.0384(19) Uani 1 1 d . . . H19 H 0.9452 0.8626 0.5245 0.046 Uiso 1 1 calc R . . C20 C 0.8319(9) 0.8736(9) 0.2973(9) 0.0315(16) Uani 1 1 d . . . H20 H 0.9013 0.8271 0.2571 0.038 Uiso 1 1 calc R . . C21 C 0.7033(9) 0.9201(9) 0.1974(9) 0.0284(15) Uani 1 1 d . . . H21 H 0.6859 0.9072 0.0893 0.034 Uiso 1 1 calc R . . C22 C 0.4610(8) 1.2501(8) 0.2261(9) 0.0242(13) Uani 1 1 d . . . C23 C 0.4108(12) 1.2876(10) 0.3498(11) 0.0401(19) Uani 1 1 d . . . H23 H 0.3564 1.2092 0.3795 0.048 Uiso 1 1 calc R . . C24 C 0.4410(12) 1.4415(11) 0.4302(12) 0.049(2) Uani 1 1 d U . . H24 H 0.4057 1.4665 0.5140 0.059 Uiso 1 1 calc R . . C25 C 0.5197(12) 1.5557(10) 0.3910(13) 0.046(2) Uani 1 1 d U . . H25 H 0.5436 1.6593 0.4494 0.055 Uiso 1 1 calc R . . C26 C 0.5654(15) 1.5179(11) 0.2619(14) 0.057(3) Uani 1 1 d U . . H26 H 0.6158 1.5958 0.2284 0.068 Uiso 1 1 calc R . . C27 C 0.5349(13) 1.3642(10) 0.1850(13) 0.050(3) Uani 1 1 d . . . H27 H 0.5676 1.3386 0.0996 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0210(3) 0.0201(2) 0.0209(2) 0.00549(19) 0.0099(2) 0.00430(19) As1 0.0232(3) 0.0189(3) 0.0205(3) 0.0041(3) 0.0081(3) 0.0030(3) I1 0.0428(3) 0.0405(3) 0.0555(4) -0.0032(3) 0.0320(3) -0.0108(2) I2 0.0353(3) 0.0386(3) 0.0247(2) 0.0039(2) 0.0151(2) 0.0051(2) P1 0.0196(8) 0.0212(8) 0.0225(8) 0.0074(7) 0.0088(7) 0.0057(6) C1 0.040(4) 0.019(3) 0.032(4) 0.002(3) 0.018(3) 0.002(3) C2 0.074(7) 0.033(4) 0.053(6) 0.016(4) 0.035(5) 0.024(5) C3 0.092(8) 0.030(5) 0.081(7) 0.011(5) 0.055(6) 0.018(5) C4 0.101(8) 0.030(5) 0.091(8) -0.007(5) 0.059(6) -0.010(5) C5 0.067(7) 0.057(6) 0.081(8) -0.028(6) 0.022(6) -0.020(6) C6 0.052(5) 0.034(4) 0.049(5) 0.003(4) 0.011(4) 0.006(4) C7 0.025(3) 0.027(3) 0.022(3) 0.005(3) 0.007(3) 0.008(3) C8 0.024(3) 0.026(3) 0.032(4) 0.006(3) 0.012(3) 0.002(3) C9 0.024(4) 0.041(5) 0.052(5) 0.011(4) 0.011(4) -0.002(3) C10 0.029(4) 0.020(3) 0.031(4) 0.006(3) 0.014(3) 0.001(3) C11 0.038(4) 0.027(4) 0.040(4) 0.012(3) 0.016(4) -0.002(3) C12 0.024(3) 0.016(3) 0.028(3) 0.006(3) 0.010(3) 0.006(2) C13 0.020(3) 0.015(3) 0.016(3) 0.002(2) 0.004(2) 0.005(2) C14 0.021(3) 0.022(3) 0.030(3) 0.007(3) 0.009(3) 0.005(2) C15 0.027(4) 0.023(3) 0.041(4) 0.010(3) 0.007(3) 0.010(3) C16 0.014(3) 0.020(3) 0.033(3) 0.008(3) 0.008(3) 0.002(2) C17 0.023(3) 0.047(4) 0.028(3) 0.021(3) 0.011(3) 0.014(3) C18 0.031(4) 0.047(5) 0.037(4) 0.020(4) 0.010(4) 0.011(4) C19 0.025(4) 0.039(4) 0.044(5) 0.014(4) 0.003(3) 0.010(3) C20 0.033(4) 0.034(4) 0.032(4) 0.011(3) 0.011(3) 0.021(3) C21 0.032(4) 0.030(4) 0.024(3) 0.008(3) 0.009(3) 0.016(3) C22 0.021(3) 0.017(3) 0.029(3) 0.003(3) 0.006(3) 0.003(2) C23 0.053(5) 0.036(4) 0.039(4) 0.008(4) 0.028(4) 0.007(4) C24 0.053(6) 0.044(5) 0.047(5) -0.004(4) 0.024(4) 0.009(4) C25 0.047(5) 0.021(4) 0.061(5) -0.005(4) 0.020(4) 0.004(3) C26 0.084(7) 0.030(4) 0.072(7) 0.018(5) 0.049(6) 0.004(5) C27 0.069(7) 0.023(4) 0.069(7) 0.003(4) 0.048(6) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2991(18) . ? Pd1 As1 2.3463(8) . ? Pd1 I2 2.6408(7) . ? Pd1 I1 2.6489(7) . ? As1 C1 1.907(7) . ? As1 C12 1.997(7) . ? As1 C7 1.997(7) . ? P1 C16 1.831(7) . ? P1 C22 1.831(7) . ? P1 C13 1.871(7) . ? C1 C2 1.407(12) . ? C1 C6 1.420(13) . ? C2 C3 1.359(14) . ? C3 C4 1.36(2) . ? C4 C5 1.40(2) . ? C5 C6 1.315(15) . ? C7 C8 1.488(10) . ? C7 C14 1.545(10) . ? C8 C10 1.355(10) . ? C8 C9 1.520(11) . ? C10 C12 1.497(10) . ? C10 C11 1.500(11) . ? C12 C13 1.548(8) . ? C13 C14 1.594(9) . ? C14 C15 1.526(10) . ? C16 C17 1.385(10) . ? C16 C21 1.392(10) . ? C17 C18 1.401(10) . ? C18 C19 1.372(13) . ? C19 C20 1.397(12) . ? C20 C21 1.393(9) . ? C22 C27 1.345(11) . ? C22 C23 1.392(11) . ? C23 C24 1.399(13) . ? C24 C25 1.358(14) . ? C25 C26 1.411(15) . ? C26 C27 1.389(13) . ? 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 P1 Pd1 As1 82.18(5) . . ? P1 Pd1 I2 168.14(5) . . ? As1 Pd1 I2 87.48(2) . . ? P1 Pd1 I1 98.65(5) . . ? As1 Pd1 I1 170.86(3) . . ? I2 Pd1 I1 92.48(2) . . ? C1 As1 C12 110.5(3) . . ? C1 As1 C7 110.7(3) . . ? C12 As1 C7 76.1(3) . . ? C1 As1 Pd1 123.8(2) . . ? C12 As1 Pd1 109.16(19) . . ? C7 As1 Pd1 116.2(2) . . ? C16 P1 C22 104.3(3) . . ? C16 P1 C13 105.6(3) . . ? C22 P1 C13 105.4(3) . . ? C16 P1 Pd1 111.1(2) . . ? C22 P1 Pd1 123.0(2) . . ? C13 P1 Pd1 106.2(2) . . ? C2 C1 C6 116.9(8) . . ? C2 C1 As1 119.2(7) . . ? C6 C1 As1 123.9(6) . . ? C3 C2 C1 121.7(11) . . ? C4 C3 C2 118.7(11) . . ? C3 C4 C5 121.5(11) . . ? C6 C5 C4 119.7(13) . . ? C5 C6 C1 121.3(11) . . ? C8 C7 C14 109.6(6) . . ? C8 C7 As1 99.7(5) . . ? C14 C7 As1 100.1(4) . . ? C10 C8 C7 111.8(6) . . ? C10 C8 C9 127.3(7) . . ? C7 C8 C9 120.8(7) . . ? C8 C10 C12 111.7(6) . . ? C8 C10 C11 128.0(7) . . ? C12 C10 C11 120.2(6) . . ? C10 C12 C13 113.7(5) . . ? C10 C12 As1 100.8(5) . . ? C13 C12 As1 94.8(4) . . ? C12 C13 C14 105.9(5) . . ? C12 C13 P1 107.8(4) . . ? C14 C13 P1 111.7(4) . . ? C15 C14 C7 112.4(6) . . ? C15 C14 C13 119.0(6) . . ? C7 C14 C13 106.0(5) . . ? C17 C16 C21 120.0(6) . . ? C17 C16 P1 120.2(5) . . ? C21 C16 P1 119.7(5) . . ? C16 C17 C18 120.1(7) . . ? C19 C18 C17 119.8(8) . . ? C18 C19 C20 120.4(8) . . ? C21 C20 C19 119.8(7) . . ? C16 C21 C20 119.8(7) . . ? C27 C22 C23 118.6(7) . . ? C27 C22 P1 120.7(6) . . ? C23 C22 P1 120.7(6) . . ? C22 C23 C24 119.7(8) . . ? C25 C24 C23 121.4(9) . . ? C24 C25 C26 118.8(8) . . ? C27 C26 C25 118.5(9) . . ? C22 C27 C26 123.0(9) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 30.77 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.065 _refine_diff_density_min -1.775 _refine_diff_density_rms 0.194 # Attachment 'leung319.cif' data_leung319 _database_code_depnum_ccdc_archive 'CCDC 734388' #TrackingRef 'leung319.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H46 As N P Pd, 3(C H2 Cl2), Cl O4 ' _chemical_formula_sum 'C49 H52 As Cl7 N O4 P Pd' _chemical_formula_weight 1179.36 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' P P 0.1023 0.0942 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.6237(3) _cell_length_b 17.1807(4) _cell_length_c 23.4194(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5079.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9269 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 29.10 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7124 _exptl_absorpt_correction_T_max 0.7595 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 205225 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 31.28 _reflns_number_total 16459 _reflns_number_gt 14488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0440P)^2^+0.5257P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(5) _refine_ls_number_reflns 16459 _refine_ls_number_parameters 582 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.341703(11) 0.278597(9) 0.783297(6) 0.01855(4) Uani 1 1 d . . . As1 As 0.486957(16) 0.324492(12) 0.721005(9) 0.02128(5) Uani 1 1 d . . . C1 C 0.22178(16) 0.22723(13) 0.82806(9) 0.0215(4) Uani 1 1 d . . . C2 C 0.11946(18) 0.20408(13) 0.80855(10) 0.0248(5) Uani 1 1 d . . . H2 H 0.0976 0.2181 0.7711 0.030 Uiso 1 1 calc R . . C3 C 0.05220(18) 0.16225(14) 0.84235(10) 0.0282(5) Uani 1 1 d . . . H3 H -0.0159 0.1487 0.8283 0.034 Uiso 1 1 calc R . . C4 C 0.08211(18) 0.13877(13) 0.89785(10) 0.0262(5) Uani 1 1 d . . . C5 C 0.18318(18) 0.16106(13) 0.91894(9) 0.0253(4) Uani 1 1 d . . . C6 C 0.25124(17) 0.20608(13) 0.88287(9) 0.0221(4) Uani 1 1 d . . . C7 C 0.0141(2) 0.09302(14) 0.93302(11) 0.0317(5) Uani 1 1 d . . . H7 H -0.0535 0.0778 0.9191 0.038 Uiso 1 1 calc R . . C8 C 0.0448(2) 0.07076(16) 0.98658(12) 0.0369(6) Uani 1 1 d . . . H8 H -0.0013 0.0401 1.0094 0.044 Uiso 1 1 calc R . . C9 C 0.1431(2) 0.09272(17) 1.00773(11) 0.0395(6) Uani 1 1 d . . . H9 H 0.1635 0.0771 1.0451 0.047 Uiso 1 1 calc R . . C10 C 0.2113(2) 0.13682(16) 0.97526(10) 0.0349(6) Uani 1 1 d . . . H10 H 0.2782 0.1514 0.9905 0.042 Uiso 1 1 calc R . . C11 C 0.35512(18) 0.23681(14) 0.90456(9) 0.0264(5) Uani 1 1 d . . . H11 H 0.3843 0.2001 0.9337 0.032 Uiso 1 1 calc R . . C12 C 0.3366(2) 0.31648(17) 0.93224(12) 0.0422(6) Uani 1 1 d . . . H12A H 0.4013 0.3333 0.9518 0.063 Uiso 1 1 calc R . . H12B H 0.2786 0.3126 0.9599 0.063 Uiso 1 1 calc R . . H12C H 0.3180 0.3545 0.9027 0.063 Uiso 1 1 calc R . . C13 C 0.46557(19) 0.16145(14) 0.83987(11) 0.0297(5) Uani 1 1 d . . . H13A H 0.5067 0.1630 0.8044 0.045 Uiso 1 1 calc R . . H13B H 0.4035 0.1279 0.8346 0.045 Uiso 1 1 calc R . . H13C H 0.5097 0.1406 0.8707 0.045 Uiso 1 1 calc R . . C14 C 0.52571(18) 0.28786(15) 0.86998(10) 0.0305(5) Uani 1 1 d . . . H14A H 0.5520 0.2715 0.9075 0.046 Uiso 1 1 calc R . . H14B H 0.5072 0.3432 0.8712 0.046 Uiso 1 1 calc R . . H14C H 0.5809 0.2794 0.8412 0.046 Uiso 1 1 calc R . . C15 C 0.18077(16) 0.22843(13) 0.67106(9) 0.0217(4) Uani 1 1 d . . . C16 C 0.08851(18) 0.23382(14) 0.63797(10) 0.0271(5) Uani 1 1 d . . . H16 H 0.0516 0.2819 0.6354 0.032 Uiso 1 1 calc R . . C17 C 0.0511(2) 0.16917(17) 0.60899(11) 0.0346(6) Uani 1 1 d . . . H17 H -0.0116 0.1729 0.5867 0.042 Uiso 1 1 calc R . . C18 C 0.1049(2) 0.09898(16) 0.61249(12) 0.0372(6) Uani 1 1 d . . . H18 H 0.0788 0.0546 0.5927 0.045 Uiso 1 1 calc R . . C19 C 0.1955(2) 0.09339(15) 0.64432(12) 0.0375(6) Uani 1 1 d . . . H19 H 0.2325 0.0453 0.6463 0.045 Uiso 1 1 calc R . . C20 C 0.2337(2) 0.15772(14) 0.67380(11) 0.0309(5) Uani 1 1 d . . . H20 H 0.2965 0.1533 0.6960 0.037 Uiso 1 1 calc R . . C21 C 0.13698(16) 0.38266(12) 0.72409(9) 0.0226(4) Uani 1 1 d . . . C22 C 0.1238(2) 0.40696(14) 0.78061(11) 0.0319(5) Uani 1 1 d . . . H22 H 0.1647 0.3839 0.8102 0.038 Uiso 1 1 calc R . . C23 C 0.0503(2) 0.46525(16) 0.79360(12) 0.0418(7) Uani 1 1 d . . . H23 H 0.0424 0.4825 0.8319 0.050 Uiso 1 1 calc R . . C24 C -0.0101(2) 0.49738(16) 0.75139(13) 0.0421(6) Uani 1 1 d . . . H24 H -0.0615 0.5358 0.7607 0.051 Uiso 1 1 calc R . . C25 C 0.0029(2) 0.47445(15) 0.69526(12) 0.0360(6) Uani 1 1 d . . . H25 H -0.0392 0.4973 0.6661 0.043 Uiso 1 1 calc R . . C26 C 0.07719(19) 0.41827(14) 0.68141(10) 0.0271(5) Uani 1 1 d . . . H26 H 0.0875 0.4039 0.6426 0.033 Uiso 1 1 calc R . . C27 C 0.32418(16) 0.35939(12) 0.65509(8) 0.0205(4) Uani 1 1 d . . . H27 H 0.2846 0.3683 0.6187 0.025 Uiso 1 1 calc R . . C28 C 0.36252(16) 0.43871(12) 0.68133(9) 0.0210(4) Uani 1 1 d . . . H28 H 0.3325 0.4422 0.7208 0.025 Uiso 1 1 calc R . . C29 C 0.32672(16) 0.51073(12) 0.64922(9) 0.0209(4) Uani 1 1 d . . . C30 C 0.28940(17) 0.57420(13) 0.68018(10) 0.0255(4) Uani 1 1 d . . . H30 H 0.2860 0.5711 0.7206 0.031 Uiso 1 1 calc R . . C31 C 0.25712(19) 0.64192(14) 0.65299(11) 0.0312(5) Uani 1 1 d . . . H31 H 0.2325 0.6849 0.6748 0.037 Uiso 1 1 calc R . . C32 C 0.26089(19) 0.64670(15) 0.59368(11) 0.0320(5) Uani 1 1 d . . . H32 H 0.2392 0.6930 0.5748 0.038 Uiso 1 1 calc R . . C33 C 0.2967(2) 0.58331(15) 0.56236(11) 0.0316(5) Uani 1 1 d . . . H33 H 0.2986 0.5861 0.5219 0.038 Uiso 1 1 calc R . . C34 C 0.32969(19) 0.51578(14) 0.58974(10) 0.0278(5) Uani 1 1 d . . . H34 H 0.3544 0.4729 0.5679 0.033 Uiso 1 1 calc R . . C35 C 0.48577(17) 0.43067(13) 0.68750(9) 0.0226(4) Uani 1 1 d . . . H35 H 0.5205 0.4717 0.7113 0.027 Uiso 1 1 calc R . . C36 C 0.53619(17) 0.41687(14) 0.62960(10) 0.0248(4) Uani 1 1 d . . . C37 C 0.6115(2) 0.47423(17) 0.60406(12) 0.0369(6) Uani 1 1 d . . . H37A H 0.6484 0.4502 0.5717 0.055 Uiso 1 1 calc R . . H37B H 0.6634 0.4901 0.6329 0.055 Uiso 1 1 calc R . . H37C H 0.5722 0.5200 0.5908 0.055 Uiso 1 1 calc R . . C38 C 0.50031(18) 0.35106(13) 0.60568(9) 0.0246(4) Uani 1 1 d . . . C39 C 0.5239(2) 0.32000(18) 0.54745(11) 0.0400(6) Uani 1 1 d . . . H39A H 0.4590 0.3198 0.5246 0.060 Uiso 1 1 calc R . . H39B H 0.5513 0.2668 0.5507 0.060 Uiso 1 1 calc R . . H39C H 0.5771 0.3531 0.5289 0.060 Uiso 1 1 calc R . . C40 C 0.42468(17) 0.30817(13) 0.64443(9) 0.0220(4) Uani 1 1 d . . . H40 H 0.4105 0.2527 0.6339 0.026 Uiso 1 1 calc R . . C41 C 0.63176(16) 0.28885(12) 0.71676(9) 0.0238(4) Uani 1 1 d . . . C42 C 0.7147(2) 0.33591(16) 0.73483(11) 0.0344(5) Uani 1 1 d . . . H42 H 0.7007 0.3868 0.7488 0.041 Uiso 1 1 calc R . . C43 C 0.8176(2) 0.30871(19) 0.73256(12) 0.0417(7) Uani 1 1 d . . . H43 H 0.8742 0.3409 0.7451 0.050 Uiso 1 1 calc R . . C44 C 0.8383(2) 0.23475(18) 0.71213(11) 0.0422(6) Uani 1 1 d . . . H44 H 0.9093 0.2164 0.7104 0.051 Uiso 1 1 calc R . . C45 C 0.7571(2) 0.18770(17) 0.69432(11) 0.0390(6) Uani 1 1 d . . . H45 H 0.7717 0.1369 0.6804 0.047 Uiso 1 1 calc R . . C46 C 0.6530(2) 0.21458(14) 0.69671(10) 0.0304(5) Uani 1 1 d . . . H46 H 0.5966 0.1820 0.6846 0.037 Uiso 1 1 calc R . . C47 C 0.2022(3) 0.3878(2) 0.44285(13) 0.0578(9) Uani 1 1 d . . . H47A H 0.1494 0.4049 0.4142 0.069 Uiso 1 1 calc R . . H47B H 0.2226 0.3336 0.4337 0.069 Uiso 1 1 calc R . . C48 C 0.5495(5) 0.6754(2) 0.4036(2) 0.111(2) Uani 1 1 d . . . H48A H 0.4985 0.6778 0.3715 0.133 Uiso 1 1 calc R . . H48B H 0.5617 0.7292 0.4173 0.133 Uiso 1 1 calc R . . C49 C 0.6501(3) 0.6306(2) 0.00360(14) 0.0593(9) Uani 1 1 d . . . H49A H 0.6911 0.5830 -0.0055 0.071 Uiso 1 1 calc R . . H49B H 0.5801 0.6263 -0.0152 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.51729(5) 0.52386(4) 0.83683(3) 0.03734(14) Uani 1 1 d . . . Cl2 Cl 0.14453(7) 0.39068(6) 0.51139(3) 0.0556(2) Uani 1 1 d . . . Cl3 Cl 0.31511(7) 0.44828(6) 0.43862(4) 0.0637(2) Uani 1 1 d . . . Cl4 Cl 0.49415(10) 0.61776(11) 0.46049(6) 0.1104(5) Uani 1 1 d . . . Cl5 Cl 0.66501(11) 0.63716(7) 0.38032(4) 0.0809(3) Uani 1 1 d . . . Cl6 Cl 0.63249(8) 0.63698(8) 0.07770(4) 0.0826(3) Uani 1 1 d . . . Cl7 Cl 0.71696(6) 0.71195(6) -0.02304(4) 0.0578(2) Uani 1 1 d . . . N1 N 0.43027(14) 0.24149(10) 0.85489(8) 0.0213(4) Uani 1 1 d . . . O1 O 0.5266(2) 0.5709(2) 0.88651(11) 0.0803(9) Uani 1 1 d . . . O2 O 0.5355(2) 0.57307(13) 0.78880(10) 0.0605(6) Uani 1 1 d . . . O3 O 0.4140(2) 0.49127(18) 0.83239(13) 0.0765(8) Uani 1 1 d . . . O4 O 0.5958(2) 0.46463(14) 0.83659(15) 0.0758(8) Uani 1 1 d . . . P1 P 0.23896(4) 0.31115(3) 0.70837(2) 0.01897(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01826(7) 0.02027(7) 0.01713(7) 0.00107(6) -0.00052(6) -0.00031(6) As1 0.01969(9) 0.02424(10) 0.01990(10) 0.00120(9) 0.00098(8) 0.00001(8) C1 0.0205(9) 0.0221(10) 0.0217(10) 0.0009(8) 0.0016(7) -0.0005(8) C2 0.0225(10) 0.0281(12) 0.0239(11) 0.0020(8) -0.0011(8) 0.0006(9) C3 0.0201(10) 0.0308(12) 0.0337(12) -0.0009(10) 0.0032(9) -0.0001(9) C4 0.0255(11) 0.0235(11) 0.0296(12) 0.0003(9) 0.0087(8) 0.0032(9) C5 0.0285(11) 0.0256(11) 0.0218(10) 0.0020(8) 0.0052(8) 0.0013(9) C6 0.0246(10) 0.0222(11) 0.0195(9) -0.0008(8) 0.0015(8) 0.0007(8) C7 0.0266(11) 0.0286(12) 0.0398(13) 0.0030(10) 0.0092(10) -0.0005(10) C8 0.0405(14) 0.0316(13) 0.0386(14) 0.0054(11) 0.0190(11) -0.0016(11) C9 0.0456(16) 0.0443(15) 0.0285(13) 0.0111(11) 0.0068(11) 0.0015(12) C10 0.0355(13) 0.0425(15) 0.0268(12) 0.0067(11) 0.0011(10) -0.0021(11) C11 0.0272(11) 0.0330(12) 0.0191(10) 0.0019(8) -0.0012(8) -0.0052(9) C12 0.0393(14) 0.0486(16) 0.0386(14) -0.0197(12) 0.0030(12) -0.0079(13) C13 0.0287(12) 0.0264(12) 0.0340(13) 0.0042(10) -0.0042(9) 0.0063(9) C14 0.0253(11) 0.0360(13) 0.0303(12) 0.0043(10) -0.0069(9) -0.0097(10) C15 0.0196(9) 0.0237(10) 0.0217(9) -0.0005(8) 0.0023(7) -0.0029(8) C16 0.0263(11) 0.0284(12) 0.0265(11) -0.0023(9) -0.0004(8) -0.0014(9) C17 0.0326(13) 0.0435(15) 0.0277(12) -0.0054(11) -0.0013(9) -0.0114(11) C18 0.0431(15) 0.0333(14) 0.0352(14) -0.0104(11) 0.0049(11) -0.0135(12) C19 0.0418(14) 0.0234(12) 0.0472(16) -0.0056(11) 0.0014(12) -0.0028(11) C20 0.0313(12) 0.0266(12) 0.0347(13) -0.0026(10) -0.0042(10) 0.0000(10) C21 0.0215(9) 0.0222(9) 0.0241(10) 0.0019(8) 0.0007(8) 0.0013(7) C22 0.0402(12) 0.0313(11) 0.0243(11) -0.0001(10) 0.0007(10) 0.0084(10) C23 0.0562(17) 0.0382(14) 0.0310(14) -0.0023(11) 0.0099(11) 0.0167(13) C24 0.0461(16) 0.0336(14) 0.0466(16) 0.0009(12) 0.0074(13) 0.0191(13) C25 0.0372(14) 0.0284(12) 0.0425(14) 0.0069(10) -0.0015(11) 0.0082(11) C26 0.0295(12) 0.0264(11) 0.0255(11) 0.0023(9) -0.0007(9) 0.0015(9) C27 0.0237(10) 0.0219(10) 0.0160(9) -0.0001(7) 0.0004(7) 0.0006(8) C28 0.0241(10) 0.0200(10) 0.0188(9) -0.0018(8) 0.0027(7) -0.0020(8) C29 0.0209(10) 0.0202(9) 0.0217(10) 0.0000(8) 0.0000(7) -0.0023(8) C30 0.0235(10) 0.0253(11) 0.0278(11) -0.0030(9) 0.0033(8) -0.0005(9) C31 0.0272(11) 0.0254(11) 0.0411(14) -0.0023(10) 0.0014(10) 0.0021(9) C32 0.0275(12) 0.0299(12) 0.0385(13) 0.0061(10) -0.0074(10) 0.0023(10) C33 0.0357(12) 0.0327(12) 0.0263(11) 0.0051(10) -0.0039(9) 0.0008(10) C34 0.0334(12) 0.0260(11) 0.0239(10) -0.0018(8) 0.0009(9) 0.0020(10) C35 0.0233(10) 0.0235(10) 0.0212(10) -0.0014(8) 0.0011(8) -0.0031(9) C36 0.0231(10) 0.0264(11) 0.0250(11) 0.0033(9) 0.0042(8) 0.0019(9) C37 0.0341(13) 0.0359(14) 0.0407(14) 0.0042(11) 0.0137(11) -0.0048(11) C38 0.0256(11) 0.0275(11) 0.0207(10) -0.0009(8) 0.0042(8) 0.0023(9) C39 0.0428(15) 0.0492(16) 0.0280(13) -0.0078(12) 0.0134(10) -0.0019(13) C40 0.0249(10) 0.0224(10) 0.0187(9) -0.0030(8) 0.0025(7) 0.0005(8) C41 0.0222(9) 0.0278(10) 0.0214(9) 0.0018(9) 0.0009(8) -0.0015(7) C42 0.0325(13) 0.0372(14) 0.0335(13) 0.0001(10) -0.0006(9) -0.0058(11) C43 0.0263(12) 0.0576(18) 0.0412(15) 0.0049(13) -0.0009(10) -0.0110(12) C44 0.0262(11) 0.0697(19) 0.0306(12) 0.0110(13) 0.0085(10) 0.0098(13) C45 0.0417(15) 0.0475(16) 0.0278(12) -0.0011(11) 0.0040(10) 0.0175(13) C46 0.0298(11) 0.0322(12) 0.0293(11) -0.0027(9) -0.0002(9) 0.0010(11) C47 0.0536(18) 0.083(3) 0.0372(16) -0.0098(16) -0.0035(14) -0.0099(18) C48 0.153(5) 0.037(2) 0.142(5) 0.008(3) -0.101(4) 0.003(2) C49 0.056(2) 0.071(2) 0.0507(19) -0.0093(17) -0.0021(16) -0.0118(18) Cl1 0.0424(3) 0.0366(3) 0.0330(3) 0.0002(2) 0.0009(3) -0.0009(3) Cl2 0.0487(4) 0.0753(6) 0.0429(4) -0.0079(4) 0.0015(3) 0.0015(4) Cl3 0.0571(5) 0.0798(6) 0.0542(5) -0.0186(4) 0.0123(4) -0.0098(4) Cl4 0.0673(7) 0.1703(15) 0.0935(9) -0.0210(9) 0.0157(7) -0.0315(9) Cl5 0.0958(8) 0.0988(8) 0.0483(5) -0.0010(5) 0.0006(5) -0.0297(7) Cl6 0.0699(6) 0.1277(10) 0.0501(5) 0.0154(6) 0.0212(4) 0.0259(6) Cl7 0.0464(4) 0.0738(6) 0.0532(5) 0.0100(4) -0.0010(3) 0.0013(4) N1 0.0219(9) 0.0225(9) 0.0195(8) 0.0037(7) -0.0011(6) -0.0020(7) O1 0.0746(18) 0.125(3) 0.0412(13) -0.0366(15) 0.0016(12) -0.0052(18) O2 0.0870(17) 0.0500(12) 0.0446(13) 0.0115(11) -0.0053(12) -0.0053(12) O3 0.0503(14) 0.093(2) 0.086(2) -0.0039(17) 0.0046(14) -0.0248(15) O4 0.0644(16) 0.0380(13) 0.125(3) 0.0152(15) 0.0086(17) 0.0089(12) P1 0.0191(2) 0.0201(2) 0.0178(2) -0.00026(19) -0.00035(18) 0.00002(19) _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 2.042(2) . ? Pd1 N1 2.1138(18) . ? Pd1 P1 2.2525(5) . ? Pd1 As1 2.4723(3) . ? As1 C41 1.930(2) . ? As1 C40 1.978(2) . ? As1 C35 1.986(2) . ? C1 C6 1.385(3) . ? C1 C2 1.427(3) . ? C2 C3 1.365(3) . ? C3 C4 1.412(3) . ? C4 C5 1.421(3) . ? C4 C7 1.426(3) . ? C5 C10 1.428(3) . ? C5 C6 1.432(3) . ? C6 C11 1.502(3) . ? C7 C8 1.368(4) . ? C8 C9 1.389(4) . ? C9 C10 1.376(4) . ? C11 N1 1.503(3) . ? C11 C12 1.532(4) . ? C13 N1 1.488(3) . ? C14 N1 1.487(3) . ? C15 C20 1.388(3) . ? C15 C16 1.402(3) . ? C15 P1 1.823(2) . ? C16 C17 1.385(4) . ? C17 C18 1.387(4) . ? C18 C19 1.369(4) . ? C19 C20 1.389(3) . ? C21 C26 1.394(3) . ? C21 C22 1.398(3) . ? C21 P1 1.817(2) . ? C22 C23 1.399(3) . ? C23 C24 1.365(4) . ? C24 C25 1.382(4) . ? C25 C26 1.384(3) . ? C27 C40 1.564(3) . ? C27 C28 1.571(3) . ? C27 P1 1.844(2) . ? C28 C29 1.517(3) . ? C28 C35 1.569(3) . ? C29 C30 1.392(3) . ? C29 C34 1.396(3) . ? C30 C31 1.388(3) . ? C31 C32 1.392(4) . ? C32 C33 1.389(4) . ? C33 C34 1.389(3) . ? C35 C36 1.517(3) . ? C36 C38 1.341(3) . ? C36 C37 1.495(3) . ? C38 C39 1.494(3) . ? C38 C40 1.509(3) . ? C41 C46 1.386(3) . ? C41 C42 1.389(3) . ? C42 C43 1.381(4) . ? C43 C44 1.383(4) . ? C44 C45 1.371(4) . ? C45 C46 1.393(4) . ? C47 Cl2 1.763(3) . ? C47 Cl3 1.767(4) . ? C48 Cl5 1.690(6) . ? C48 Cl4 1.801(6) . ? C49 Cl7 1.748(4) . ? C49 Cl6 1.753(4) . ? Cl1 O4 1.420(3) . ? Cl1 O1 1.421(3) . ? Cl1 O3 1.423(3) . ? Cl1 O2 1.426(2) . ? 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 N1 81.63(7) . . ? C1 Pd1 P1 94.61(6) . . ? N1 Pd1 P1 175.85(5) . . ? C1 Pd1 As1 172.16(6) . . ? N1 Pd1 As1 99.90(5) . . ? P1 Pd1 As1 83.582(15) . . ? C41 As1 C40 106.54(9) . . ? C41 As1 C35 106.15(9) . . ? C40 As1 C35 76.64(9) . . ? C41 As1 Pd1 129.16(6) . . ? C40 As1 Pd1 101.24(6) . . ? C35 As1 Pd1 121.37(6) . . ? C6 C1 C2 117.8(2) . . ? C6 C1 Pd1 112.97(15) . . ? C2 C1 Pd1 128.84(16) . . ? C3 C2 C1 121.6(2) . . ? C2 C3 C4 121.2(2) . . ? C3 C4 C5 118.9(2) . . ? C3 C4 C7 121.9(2) . . ? C5 C4 C7 119.3(2) . . ? C4 C5 C10 117.8(2) . . ? C4 C5 C6 118.6(2) . . ? C10 C5 C6 123.6(2) . . ? C1 C6 C5 121.8(2) . . ? C1 C6 C11 117.10(19) . . ? C5 C6 C11 120.95(19) . . ? C8 C7 C4 120.8(2) . . ? C7 C8 C9 120.3(2) . . ? C10 C9 C8 120.8(2) . . ? C9 C10 C5 121.0(2) . . ? C6 C11 N1 107.94(17) . . ? C6 C11 C12 108.9(2) . . ? N1 C11 C12 112.1(2) . . ? C20 C15 C16 118.9(2) . . ? C20 C15 P1 117.79(16) . . ? C16 C15 P1 123.25(17) . . ? C17 C16 C15 120.1(2) . . ? C16 C17 C18 120.1(2) . . ? C19 C18 C17 120.2(2) . . ? C18 C19 C20 120.3(3) . . ? C15 C20 C19 120.4(2) . . ? C26 C21 C22 118.9(2) . . ? C26 C21 P1 122.35(17) . . ? C22 C21 P1 118.57(16) . . ? C21 C22 C23 119.9(2) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C25 120.4(2) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 120.3(2) . . ? C40 C27 C28 107.49(17) . . ? C40 C27 P1 109.16(14) . . ? C28 C27 P1 107.75(13) . . ? C29 C28 C35 114.40(17) . . ? C29 C28 C27 114.95(17) . . ? C35 C28 C27 105.38(17) . . ? C30 C29 C34 118.7(2) . . ? C30 C29 C28 118.79(19) . . ? C34 C29 C28 122.50(19) . . ? C31 C30 C29 121.1(2) . . ? C30 C31 C32 119.8(2) . . ? C33 C32 C31 119.5(2) . . ? C32 C33 C34 120.6(2) . . ? C33 C34 C29 120.3(2) . . ? C36 C35 C28 110.34(17) . . ? C36 C35 As1 101.91(14) . . ? C28 C35 As1 97.17(13) . . ? C38 C36 C37 127.1(2) . . ? C38 C36 C35 111.34(19) . . ? C37 C36 C35 121.5(2) . . ? C36 C38 C39 128.0(2) . . ? C36 C38 C40 111.96(19) . . ? C39 C38 C40 120.0(2) . . ? C38 C40 C27 109.54(18) . . ? C38 C40 As1 102.98(14) . . ? C27 C40 As1 95.62(13) . . ? C46 C41 C42 119.5(2) . . ? C46 C41 As1 119.54(16) . . ? C42 C41 As1 120.91(18) . . ? C43 C42 C41 120.0(3) . . ? C42 C43 C44 120.1(3) . . ? C45 C44 C43 120.4(2) . . ? C44 C45 C46 119.8(3) . . ? C41 C46 C45 120.1(2) . . ? Cl2 C47 Cl3 111.56(18) . . ? Cl5 C48 Cl4 111.0(2) . . ? Cl7 C49 Cl6 111.4(2) . . ? O4 Cl1 O1 110.7(2) . . ? O4 Cl1 O3 110.92(18) . . ? O1 Cl1 O3 111.06(18) . . ? O4 Cl1 O2 108.03(17) . . ? O1 Cl1 O2 107.18(18) . . ? O3 Cl1 O2 108.85(17) . . ? C14 N1 C13 107.98(18) . . ? C14 N1 C11 110.86(17) . . ? C13 N1 C11 108.82(17) . . ? C14 N1 Pd1 117.09(14) . . ? C13 N1 Pd1 104.45(13) . . ? C11 N1 Pd1 107.23(13) . . ? C21 P1 C15 109.80(10) . . ? C21 P1 C27 104.26(10) . . ? C15 P1 C27 105.14(9) . . ? C21 P1 Pd1 114.71(7) . . ? C15 P1 Pd1 114.32(7) . . ? C27 P1 Pd1 107.63(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 31.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.973 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.211