#Copyright The Royal society of Chemistry, 1998 data_(1)0.5CH2Cl2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Pd(dmba)(Ph3PCHCONMe2)(OH2)]ClO4.0.5CH2Cl2' _chemical_formula_structural ? _chemical_formula_analytical 'C31 H33 Cl N2 O6 P Pd.0.5CH2Cl2' _chemical_formula_sum 'C31.50 H34 Cl2 N2 O6 P Pd' _chemical_formula_weight 744.88 _chemical_melting_point ? _chemical_compound_source ? 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' '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 'P21/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 10.2080(10) _cell_length_b 10.204(2) _cell_length_c 31.345(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.970(10) _cell_angle_gamma 90.00 _cell_volume 3225.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.5 _cell_measurement_theta_max 31.5 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.897 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Nonius CAD4' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 10800 _diffrn_standards_decay_% ? _diffrn_reflns_number 6029 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.1269 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.08 _reflns_number_total 5663 _reflns_number_observed 3362 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0619P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5663 _refine_ls_number_parameters 410 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_obs 0.0616 _refine_ls_wR_factor_all 0.1519 _refine_ls_wR_factor_obs 0.1327 _refine_ls_goodness_of_fit_all 0.967 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 0.967 _refine_ls_restrained_S_obs 1.122 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.02260(5) 0.05624(6) 0.16770(2) 0.0242(2) Uani 1 d . . P1 P -0.1622(2) -0.0650(2) 0.08742(6) 0.0236(4) Uani 1 d . . C1 C -0.1073(7) 0.0517(8) 0.2087(2) 0.026(2) Uani 1 d . . C2 C -0.2279(7) 0.1168(7) 0.2074(3) 0.031(2) Uani 1 d . . H2A H -0.2563(7) 0.1761(7) 0.1844(3) 0.037 Uiso 1 calc R . C3 C -0.3067(7) 0.0968(8) 0.2385(3) 0.034(2) Uani 1 d . . H3A H -0.3890(7) 0.1414(8) 0.2369(3) 0.041 Uiso 1 calc R . C4 C -0.2659(9) 0.0114(8) 0.2723(3) 0.042(2) Uani 1 d . . H4A H -0.3221(9) -0.0068(8) 0.2931(3) 0.051 Uiso 1 calc R . C5 C -0.1434(8) -0.0467(8) 0.2756(3) 0.037(2) Uani 1 d . . H5A H -0.1130(8) -0.1005(8) 0.2998(3) 0.045 Uiso 1 calc R . C6 C -0.0640(7) -0.0285(7) 0.2445(2) 0.029(2) Uani 1 d . . C7 C 0.0737(7) -0.0847(8) 0.2469(2) 0.035(2) Uani 1 d . . H7A H 0.1151(7) -0.0946(8) 0.2775(2) 0.042 Uiso 1 calc R . H7B H 0.0691(7) -0.1723(8) 0.2331(2) 0.042 Uiso 1 calc R . N1 N 0.1545(6) 0.0055(6) 0.2241(2) 0.0287(14) Uani 1 d . . C8 C 0.1944(8) 0.1186(8) 0.2522(3) 0.039(2) Uani 1 d . . H8A H 0.2519(37) 0.0890(10) 0.2784(7) 0.047 Uiso 1 calc R . H8B H 0.1153(8) 0.1608(28) 0.2601(12) 0.047 Uiso 1 calc R . H8C H 0.2426(40) 0.1815(22) 0.2368(6) 0.047 Uiso 1 calc R . C9 C 0.2760(7) -0.0633(8) 0.2167(2) 0.034(2) Uani 1 d . . H9A H 0.3240(24) -0.0949(39) 0.2443(3) 0.040 Uiso 1 calc R . H9B H 0.3326(21) -0.0029(14) 0.2035(13) 0.040 Uiso 1 calc R . H9C H 0.2521(7) -0.1379(27) 0.1973(12) 0.040 Uiso 1 calc R . C10 C -0.1233(7) 0.0887(6) 0.1130(2) 0.022(2) Uani 1 d . . H10A H -0.2040(7) 0.1316(6) 0.1212(2) 0.027 Uiso 1 calc R . C11 C -0.0589(7) 0.1730(7) 0.0836(2) 0.028(2) Uani 1 d . . O1 O 0.0046(5) 0.1204(5) 0.0571(2) 0.0310(12) Uani 1 d . . N2 N -0.0634(6) 0.3048(6) 0.0868(2) 0.035(2) Uani 1 d . . C12 C 0.0101(9) 0.3864(8) 0.0608(3) 0.045(2) Uani 1 d . . H12A H 0.0137(43) 0.3432(24) 0.0330(7) 0.054 Uiso 1 calc R . H12B H 0.1005(17) 0.3997(41) 0.0760(8) 0.054 Uiso 1 calc R . H12C H -0.0342(29) 0.4714(19) 0.0556(14) 0.054 Uiso 1 calc R . C13 C -0.1214(8) 0.3692(8) 0.1205(3) 0.044(2) Uani 1 d . . H13A H -0.1022(42) 0.3182(26) 0.1472(5) 0.053 Uiso 1 calc R . H13B H -0.2176(10) 0.3757(44) 0.1118(7) 0.053 Uiso 1 calc R . H13C H -0.0837(37) 0.4572(19) 0.1253(11) 0.053 Uiso 1 calc R . C14 C -0.0216(7) -0.1701(7) 0.0872(2) 0.027(2) Uani 1 d . . C15 C 0.0411(7) -0.1821(7) 0.0515(2) 0.028(2) Uani 1 d . . H15A H 0.0101(7) -0.1334(7) 0.0261(2) 0.033 Uiso 1 calc R . C16 C 0.1493(7) -0.2648(8) 0.0526(3) 0.038(2) Uani 1 d . . H16A H 0.1902(7) -0.2759(8) 0.0276(3) 0.046 Uiso 1 calc R . C17 C 0.1969(8) -0.3308(8) 0.0900(3) 0.038(2) Uani 1 d . . H17A H 0.2730(8) -0.3848(8) 0.0908(3) 0.046 Uiso 1 calc R . C18 C 0.1386(8) -0.3213(8) 0.1262(3) 0.038(2) Uani 1 d . . H18A H 0.1725(8) -0.3682(8) 0.1517(3) 0.046 Uiso 1 calc R . C19 C 0.0272(7) -0.2402(7) 0.1246(2) 0.032(2) Uani 1 d . . H19A H -0.0157(7) -0.2328(7) 0.1493(2) 0.039 Uiso 1 calc R . C20 C -0.2469(6) -0.0497(8) 0.0327(2) 0.028(2) Uani 1 d . . C21 C -0.3088(7) 0.0657(9) 0.0183(2) 0.035(2) Uani 1 d . . H21A H -0.3032(7) 0.1405(9) 0.0365(2) 0.042 Uiso 1 calc R . C22 C -0.3795(7) 0.0706(10) -0.0234(3) 0.047(2) Uani 1 d . . H22A H -0.4229(7) 0.1495(10) -0.0336(3) 0.056 Uiso 1 calc R . C23 C -0.3874(8) -0.0387(12) -0.0501(3) 0.056(3) Uani 1 d . . H23A H -0.4332(8) -0.0333(12) -0.0789(3) 0.067 Uiso 1 calc R . C24 C -0.3303(9) -0.1523(11) -0.0353(3) 0.059(3) Uani 1 d . . H24A H -0.3388(9) -0.2273(11) -0.0535(3) 0.070 Uiso 1 calc R . C25 C -0.2591(9) -0.1617(10) 0.0063(3) 0.048(2) Uani 1 d . . H25A H -0.2195(9) -0.2422(10) 0.0166(3) 0.058 Uiso 1 calc R . C26 C -0.2780(7) -0.1530(7) 0.1148(2) 0.027(2) Uani 1 d . . C27 C -0.3647(7) -0.0926(8) 0.1365(3) 0.036(2) Uani 1 d . . H27A H -0.3609(7) -0.0001(8) 0.1398(3) 0.043 Uiso 1 calc R . C28 C -0.4582(8) -0.1622(10) 0.1540(3) 0.056(3) Uani 1 d . . H28A H -0.5184(8) -0.1175(10) 0.1691(3) 0.067 Uiso 1 calc R . C29 C -0.4653(8) -0.2957(9) 0.1497(3) 0.044(2) Uani 1 d . . H29A H -0.5291(8) -0.3435(9) 0.1624(3) 0.053 Uiso 1 calc R . C30 C -0.3815(9) -0.3598(9) 0.1273(3) 0.059(3) Uani 1 d . . H30A H -0.3881(9) -0.4519(9) 0.1232(3) 0.071 Uiso 1 calc R . C31 C -0.2861(9) -0.2884(8) 0.1107(3) 0.056(3) Uani 1 d . . H31A H -0.2246(9) -0.3330(8) 0.0961(3) 0.067 Uiso 1 calc R . O6 O 0.1813(5) 0.0540(5) 0.1276(2) 0.0329(12) Uani 1 d . . Cl1 Cl 0.4660(2) 0.3032(2) 0.14577(6) 0.0332(5) Uani 1 d . . O2 O 0.5541(6) 0.2711(7) 0.1163(2) 0.061(2) Uani 1 d . . O3 O 0.3608(6) 0.3814(6) 0.1239(2) 0.055(2) Uani 1 d . . O4 O 0.4124(6) 0.1834(6) 0.1596(2) 0.059(2) Uani 1 d . . O5 O 0.5369(6) 0.3719(6) 0.1821(2) 0.048(2) Uani 1 d . . C32 C 0.5165(21) 0.9834(46) 0.4719(10) 0.166(19) Uani 0.50 d PD . Cl2 Cl 0.3673(16) 0.9650(18) 0.4883(5) 0.113(7) Uani 0.50 d PD . Cl3 Cl 0.6403(11) 1.0399(15) 0.5120(5) 0.081(5) Uani 0.50 d PD . 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 0.0236(3) 0.0198(3) 0.0288(3) 0.0014(3) 0.0028(2) -0.0016(3) P1 0.0242(9) 0.0173(9) 0.0296(10) -0.0002(9) 0.0054(8) -0.0022(9) C1 0.027(4) 0.021(4) 0.030(4) 0.000(4) 0.005(3) -0.002(4) C2 0.032(4) 0.023(4) 0.039(5) -0.001(4) 0.009(4) -0.005(4) C3 0.027(4) 0.030(5) 0.047(5) -0.009(4) 0.014(4) -0.005(3) C4 0.047(5) 0.037(5) 0.046(5) -0.006(4) 0.016(4) -0.011(4) C5 0.042(4) 0.030(5) 0.040(5) -0.003(4) 0.007(4) -0.004(4) C6 0.033(4) 0.025(5) 0.031(4) 0.001(3) 0.006(3) -0.003(3) C7 0.037(4) 0.032(5) 0.035(4) 0.010(4) 0.006(4) 0.002(4) N1 0.030(3) 0.027(3) 0.029(3) -0.001(3) 0.005(3) 0.002(3) C8 0.041(5) 0.034(5) 0.040(5) -0.008(4) -0.001(4) -0.005(4) C9 0.030(4) 0.029(4) 0.043(4) 0.012(4) 0.005(3) 0.002(4) C10 0.026(4) 0.014(4) 0.024(4) -0.006(3) -0.004(3) -0.002(3) C11 0.027(4) 0.022(4) 0.034(4) 0.007(3) 0.005(3) 0.000(3) O1 0.030(3) 0.030(3) 0.033(3) 0.005(2) 0.003(2) 0.001(2) N2 0.040(4) 0.021(4) 0.041(4) -0.002(3) -0.001(3) -0.004(3) C12 0.057(6) 0.015(4) 0.062(6) 0.010(4) 0.010(5) -0.014(4) C13 0.048(5) 0.025(5) 0.060(6) -0.003(4) 0.010(5) 0.000(4) C14 0.027(4) 0.016(4) 0.036(4) 0.001(3) 0.001(3) -0.003(3) C15 0.021(4) 0.025(4) 0.038(4) 0.000(4) 0.010(3) 0.004(3) C16 0.029(4) 0.038(5) 0.052(5) -0.003(4) 0.017(4) -0.007(4) C17 0.032(4) 0.032(5) 0.050(5) -0.002(4) 0.004(4) 0.000(4) C18 0.042(5) 0.027(5) 0.040(5) 0.007(4) -0.015(4) 0.003(4) C19 0.039(4) 0.019(4) 0.037(5) -0.006(3) 0.002(4) -0.001(4) C20 0.019(3) 0.026(4) 0.039(4) 0.008(4) 0.005(3) -0.001(4) C21 0.032(4) 0.033(5) 0.040(5) 0.005(4) 0.004(3) -0.011(4) C22 0.027(4) 0.064(7) 0.049(5) 0.016(5) 0.000(4) 0.002(5) C23 0.033(5) 0.098(9) 0.033(5) -0.012(6) -0.004(4) 0.000(6) C24 0.045(5) 0.082(8) 0.043(6) -0.022(6) -0.014(4) 0.022(6) C25 0.050(5) 0.048(6) 0.042(5) -0.016(5) -0.007(4) 0.007(5) C26 0.025(4) 0.021(4) 0.035(4) -0.003(3) 0.007(3) -0.005(3) C27 0.027(4) 0.025(5) 0.059(5) -0.003(4) 0.016(4) -0.006(3) C28 0.038(5) 0.052(6) 0.086(8) -0.015(6) 0.038(5) 0.001(5) C29 0.035(5) 0.043(6) 0.056(6) 0.020(5) 0.009(4) -0.016(4) C30 0.053(6) 0.026(5) 0.108(9) 0.000(5) 0.045(6) -0.002(4) C31 0.057(6) 0.026(5) 0.094(8) -0.009(5) 0.043(6) -0.003(4) O6 0.027(3) 0.036(3) 0.036(3) 0.004(3) 0.007(2) -0.002(3) Cl1 0.0319(10) 0.0254(10) 0.0405(11) 0.0028(9) 0.0003(9) -0.0040(8) O2 0.040(3) 0.084(5) 0.059(4) -0.020(4) 0.012(3) -0.001(4) O3 0.051(4) 0.047(4) 0.060(4) -0.007(3) -0.014(3) 0.020(3) O4 0.053(4) 0.057(4) 0.061(4) 0.025(3) -0.008(3) -0.033(3) O5 0.054(4) 0.039(4) 0.043(3) -0.011(3) -0.015(3) -0.006(3) C32 0.064(17) 0.321(55) 0.118(24) -0.063(31) 0.027(17) -0.090(26) Cl2 0.130(12) 0.101(12) 0.099(11) 0.062(9) -0.015(8) -0.040(9) Cl3 0.049(5) 0.066(8) 0.132(12) -0.008(7) 0.031(6) -0.014(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 1.987(7) . y Pd1 C10 2.113(6) . y Pd1 N1 2.114(6) . y Pd1 O6 2.200(5) . y P1 C10 1.778(7) . y P1 C14 1.793(7) . y P1 C20 1.803(7) . y P1 C26 1.805(7) . y C1 C2 1.393(10) . y C1 C6 1.403(10) . y C2 C3 1.374(10) . y C2 H2A 0.95 . ? C3 C4 1.385(11) . y C3 H3A 0.95 . ? C4 C5 1.373(11) . y C4 H4A 0.95 . ? C5 C6 1.373(10) . y C5 H5A 0.95 . ? C6 C7 1.509(10) . y C7 N1 1.490(9) . y C7 H7A 0.99 . ? C7 H7B 0.99 . ? N1 C8 1.470(9) . y N1 C9 1.476(9) . y C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.487(9) . y C10 H10A 1.00 . ? C11 O1 1.252(8) . y C11 N2 1.349(10) . y N2 C13 1.447(10) . y N2 C12 1.454(9) . y C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.377(10) . ? C14 C19 1.397(10) . ? C15 C16 1.386(10) . ? C15 H15A 0.95 . ? C16 C17 1.375(11) . ? C16 H16A 0.95 . ? C17 C18 1.362(11) . ? C17 H17A 0.95 . ? C18 C19 1.401(10) . ? C18 H18A 0.95 . ? C19 H19A 0.95 . ? C20 C21 1.378(10) . ? C20 C25 1.405(11) . ? C21 C22 1.392(10) . ? C21 H21A 0.95 . ? C22 C23 1.390(13) . ? C22 H22A 0.95 . ? C23 C24 1.347(14) . ? C23 H23A 0.95 . ? C24 C25 1.394(11) . ? C24 H24A 0.95 . ? C25 H25A 0.95 . ? C26 C27 1.346(10) . ? C26 C31 1.389(11) . ? C27 C28 1.369(11) . ? C27 H27A 0.95 . ? C28 C29 1.370(12) . ? C28 H28A 0.95 . ? C29 C30 1.356(12) . ? C29 H29A 0.95 . ? C30 C31 1.381(11) . ? C30 H30A 0.95 . ? C31 H31A 0.95 . ? Cl1 O2 1.424(6) . ? Cl1 O3 1.425(6) . ? Cl1 O4 1.433(6) . ? Cl1 O5 1.434(5) . ? C32 Cl2 1.67(3) 3_676 ? C32 Cl2 1.69(2) . ? C32 Cl3 1.73(2) . ? C32 Cl3 1.77(3) 3_676 ? C32 C32 1.87(6) 3_676 ? Cl2 Cl3 0.09(3) 3_676 ? Cl2 C32 1.67(3) 3_676 ? Cl3 Cl2 0.09(3) 3_676 ? Cl3 C32 1.77(3) 3_676 ? 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 C10 94.1(3) . . y C1 Pd1 N1 81.6(3) . . y C10 Pd1 N1 173.3(3) . . y C1 Pd1 O6 174.3(2) . . y C10 Pd1 O6 91.6(2) . . y N1 Pd1 O6 92.6(2) . . y C10 P1 C14 114.0(3) . . y C10 P1 C20 113.2(3) . . y C14 P1 C20 108.2(3) . . y C10 P1 C26 109.9(3) . . y C14 P1 C26 106.8(3) . . y C20 P1 C26 104.1(3) . . y C2 C1 C6 118.0(7) . . ? C2 C1 Pd1 130.1(6) . . ? C6 C1 Pd1 111.8(5) . . ? C3 C2 C1 121.3(7) . . ? C3 C2 H2A 119.4(5) . . ? C1 C2 H2A 119.4(4) . . ? C2 C3 C4 119.9(8) . . ? C2 C3 H3A 120.1(5) . . ? C4 C3 H3A 120.1(5) . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4A 120.3(5) . . ? C3 C4 H4A 120.3(5) . . ? C4 C5 C6 121.4(8) . . ? C4 C5 H5A 119.3(5) . . ? C6 C5 H5A 119.3(5) . . ? C5 C6 C1 119.9(7) . . ? C5 C6 C7 124.2(7) . . ? C1 C6 C7 115.9(6) . . ? N1 C7 C6 108.8(6) . . ? N1 C7 H7A 109.9(4) . . ? C6 C7 H7A 109.9(4) . . ? N1 C7 H7B 109.9(4) . . ? C6 C7 H7B 109.9(4) . . ? H7A C7 H7B 108.3 . . ? C8 N1 C9 107.9(6) . . ? C8 N1 C7 108.7(6) . . ? C9 N1 C7 108.9(6) . . ? C8 N1 Pd1 112.9(5) . . ? C9 N1 Pd1 115.2(4) . . ? C7 N1 Pd1 103.0(4) . . ? N1 C8 H8A 109.5(4) . . ? N1 C8 H8B 109.5(4) . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5(4) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5(4) . . ? N1 C9 H9B 109.5(4) . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5(4) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 108.6(5) . . y C11 C10 Pd1 105.6(4) . . y P1 C10 Pd1 107.9(3) . . y C11 C10 H10A 111.5(4) . . ? P1 C10 H10A 111.5(2) . . ? Pd1 C10 H10A 111.5(2) . . ? O1 C11 N2 120.2(7) . . y O1 C11 C10 119.2(7) . . y N2 C11 C10 120.5(7) . . y C11 N2 C13 121.9(7) . . y C11 N2 C12 120.2(7) . . y C13 N2 C12 117.1(7) . . y N2 C12 H12A 109.5(4) . . ? N2 C12 H12B 109.5(4) . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5(4) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5(4) . . ? N2 C13 H13B 109.5(4) . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5(4) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 119.0(7) . . ? C15 C14 P1 122.0(6) . . ? C19 C14 P1 118.9(6) . . ? C14 C15 C16 120.2(7) . . ? C14 C15 H15A 119.9(4) . . ? C16 C15 H15A 119.9(5) . . ? C17 C16 C15 119.5(8) . . ? C17 C16 H16A 120.2(5) . . ? C15 C16 H16A 120.2(5) . . ? C18 C17 C16 122.2(8) . . ? C18 C17 H17A 118.9(5) . . ? C16 C17 H17A 118.9(5) . . ? C17 C18 C19 118.0(7) . . ? C17 C18 H18A 121.0(5) . . ? C19 C18 H18A 121.0(5) . . ? C14 C19 C18 120.9(7) . . ? C14 C19 H19A 119.6(4) . . ? C18 C19 H19A 119.6(5) . . ? C21 C20 C25 120.5(7) . . ? C21 C20 P1 120.8(6) . . ? C25 C20 P1 118.4(6) . . ? C20 C21 C22 118.8(8) . . ? C20 C21 H21A 120.6(5) . . ? C22 C21 H21A 120.6(6) . . ? C23 C22 C21 120.7(9) . . ? C23 C22 H22A 119.7(5) . . ? C21 C22 H22A 119.7(6) . . ? C24 C23 C22 120.1(8) . . ? C24 C23 H23A 119.9(5) . . ? C22 C23 H23A 119.9(5) . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24A 119.5(5) . . ? C25 C24 H24A 119.5(6) . . ? C24 C25 C20 118.7(9) . . ? C24 C25 H25A 120.6(6) . . ? C20 C25 H25A 120.6(5) . . ? C27 C26 C31 117.9(7) . . ? C27 C26 P1 122.9(6) . . ? C31 C26 P1 119.0(6) . . ? C26 C27 C28 121.2(8) . . ? C26 C27 H27A 119.4(4) . . ? C28 C27 H27A 119.4(5) . . ? C27 C28 C29 120.4(8) . . ? C27 C28 H28A 119.8(5) . . ? C29 C28 H28A 119.8(5) . . ? C30 C29 C28 120.1(8) . . ? C30 C29 H29A 119.9(5) . . ? C28 C29 H29A 119.9(5) . . ? C29 C30 C31 118.6(8) . . ? C29 C30 H30A 120.7(5) . . ? C31 C30 H30A 120.7(5) . . ? C30 C31 C26 121.7(8) . . ? C30 C31 H31A 119.2(5) . . ? C26 C31 H31A 119.2(5) . . ? O2 Cl1 O3 108.7(4) . . ? O2 Cl1 O4 108.0(4) . . ? O3 Cl1 O4 109.1(4) . . ? O2 Cl1 O5 109.7(4) . . ? O3 Cl1 O5 111.0(4) . . ? O4 Cl1 O5 110.3(4) . . ? Cl2 C32 Cl2 112.2(18) 3_676 . ? Cl2 C32 Cl3 2.0(9) 3_676 . ? Cl2 C32 Cl3 114.0(19) . . ? Cl2 C32 Cl3 113.6(19) 3_676 3_676 ? Cl2 C32 Cl3 1.7(12) . 3_676 ? Cl3 C32 Cl3 115.4(17) . 3_676 ? Cl2 C32 C32 56.8(12) 3_676 3_676 ? Cl2 C32 C32 55.4(13) . 3_676 ? Cl3 C32 C32 58.5(13) . 3_676 ? Cl3 C32 C32 56.8(11) 3_676 3_676 ? Cl3 Cl2 C32 137.8(100) 3_676 3_676 ? Cl3 Cl2 C32 144.9(100) 3_676 . ? C32 Cl2 C32 67.8(18) 3_676 . ? Cl2 Cl3 C32 40.3(100) 3_676 . ? Cl2 Cl3 C32 33.3(100) 3_676 3_676 ? C32 Cl3 C32 64.6(17) . 3_676 ? 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 C10 Pd1 C1 C2 -31.1(7) . . . . ? N1 Pd1 C1 C2 154.1(7) . . . . ? O6 Pd1 C1 C2 159.5(22) . . . . ? C10 Pd1 C1 C6 150.7(5) . . . . ? N1 Pd1 C1 C6 -24.1(5) . . . . ? O6 Pd1 C1 C6 -18.8(30) . . . . ? C6 C1 C2 C3 -4.2(11) . . . . ? Pd1 C1 C2 C3 177.6(6) . . . . ? C1 C2 C3 C4 0.6(12) . . . . ? C2 C3 C4 C5 3.7(12) . . . . ? C3 C4 C5 C6 -4.3(12) . . . . ? C4 C5 C6 C1 0.6(12) . . . . ? C4 C5 C6 C7 177.4(7) . . . . ? C2 C1 C6 C5 3.6(11) . . . . ? Pd1 C1 C6 C5 -177.9(6) . . . . ? C2 C1 C6 C7 -173.5(7) . . . . ? Pd1 C1 C6 C7 5.0(8) . . . . ? C5 C6 C7 N1 -149.4(7) . . . . ? C1 C6 C7 N1 27.6(9) . . . . ? C6 C7 N1 C8 76.9(7) . . . . ? C6 C7 N1 C9 -165.8(6) . . . . ? C6 C7 N1 Pd1 -43.1(6) . . . . ? C1 Pd1 N1 C8 -79.8(5) . . . . ? C10 Pd1 N1 C8 -130.4(20) . . . . ? O6 Pd1 N1 C8 100.8(5) . . . . ? C1 Pd1 N1 C9 155.7(6) . . . . ? C10 Pd1 N1 C9 105.0(21) . . . . ? O6 Pd1 N1 C9 -23.8(5) . . . . ? C1 Pd1 N1 C7 37.3(5) . . . . ? C10 Pd1 N1 C7 -13.4(23) . . . . ? O6 Pd1 N1 C7 -142.1(5) . . . . ? C14 P1 C10 C11 75.4(5) . . . . ? C20 P1 C10 C11 -48.8(6) . . . . ? C26 P1 C10 C11 -164.8(5) . . . . ? C14 P1 C10 Pd1 -38.7(4) . . . . ? C20 P1 C10 Pd1 -162.9(3) . . . . ? C26 P1 C10 Pd1 81.2(4) . . . . ? C1 Pd1 C10 C11 146.4(5) . . . . ? N1 Pd1 C10 C11 -163.5(19) . . . . ? O6 Pd1 C10 C11 -34.7(5) . . . . ? C1 Pd1 C10 P1 -97.6(4) . . . . ? N1 Pd1 C10 P1 -47.5(23) . . . . ? O6 Pd1 C10 P1 81.4(3) . . . . ? P1 C10 C11 O1 -27.8(8) . . . . ? Pd1 C10 C11 O1 87.7(7) . . . . ? P1 C10 C11 N2 155.3(6) . . . . ? Pd1 C10 C11 N2 -89.1(7) . . . . ? O1 C11 N2 C13 -172.2(7) . . . . ? C10 C11 N2 C13 4.6(11) . . . . ? O1 C11 N2 C12 -2.6(11) . . . . ? C10 C11 N2 C12 174.2(6) . . . . ? C10 P1 C14 C15 -99.6(7) . . . . ? C20 P1 C14 C15 27.2(7) . . . . ? C26 P1 C14 C15 138.8(6) . . . . ? C10 P1 C14 C19 79.2(7) . . . . ? C20 P1 C14 C19 -153.9(6) . . . . ? C26 P1 C14 C19 -42.3(7) . . . . ? C19 C14 C15 C16 1.4(11) . . . . ? P1 C14 C15 C16 -179.7(6) . . . . ? C14 C15 C16 C17 -2.7(12) . . . . ? C15 C16 C17 C18 2.3(12) . . . . ? C16 C17 C18 C19 -0.6(12) . . . . ? C15 C14 C19 C18 0.3(11) . . . . ? P1 C14 C19 C18 -178.6(6) . . . . ? C17 C18 C19 C14 -0.7(11) . . . . ? C10 P1 C20 C21 -18.6(7) . . . . ? C14 P1 C20 C21 -145.9(6) . . . . ? C26 P1 C20 C21 100.7(6) . . . . ? C10 P1 C20 C25 167.4(6) . . . . ? C14 P1 C20 C25 40.0(7) . . . . ? C26 P1 C20 C25 -73.3(7) . . . . ? C25 C20 C21 C22 -2.3(11) . . . . ? P1 C20 C21 C22 -176.2(5) . . . . ? C20 C21 C22 C23 -0.2(11) . . . . ? C21 C22 C23 C24 2.4(13) . . . . ? C22 C23 C24 C25 -2.1(15) . . . . ? C23 C24 C25 C20 -0.4(14) . . . . ? C21 C20 C25 C24 2.6(12) . . . . ? P1 C20 C25 C24 176.7(7) . . . . ? C10 P1 C26 C27 27.7(8) . . . . ? C14 P1 C26 C27 151.9(7) . . . . ? C20 P1 C26 C27 -93.8(7) . . . . ? C10 P1 C26 C31 -157.5(7) . . . . ? C14 P1 C26 C31 -33.4(8) . . . . ? C20 P1 C26 C31 80.9(8) . . . . ? C31 C26 C27 C28 -0.1(13) . . . . ? P1 C26 C27 C28 174.7(7) . . . . ? C26 C27 C28 C29 0.1(15) . . . . ? C27 C28 C29 C30 -1.4(15) . . . . ? C28 C29 C30 C31 2.7(16) . . . . ? C29 C30 C31 C26 -2.7(16) . . . . ? C27 C26 C31 C30 1.4(15) . . . . ? P1 C26 C31 C30 -173.6(8) . . . . ? Cl2 C32 Cl2 Cl3 -144.3(334) 3_676 . . 3_676 ? Cl3 C32 Cl2 Cl3 -145.4(326) . . . 3_676 ? Cl3 C32 Cl2 Cl3 0.00(2) 3_676 . . 3_676 ? C32 C32 Cl2 Cl3 -144.3(334) 3_676 . . 3_676 ? Cl2 C32 Cl2 C32 0.000(4) 3_676 . . 3_676 ? Cl3 C32 Cl2 C32 -1.1(12) . . . 3_676 ? Cl3 C32 Cl2 C32 144.3(334) 3_676 . . 3_676 ? C32 C32 Cl2 C32 0.000(4) 3_676 . . 3_676 ? Cl2 C32 Cl3 Cl2 0.000(10) 3_676 . . 3_676 ? Cl2 C32 Cl3 Cl2 30.4(306) . . . 3_676 ? Cl3 C32 Cl3 Cl2 29.3(296) 3_676 . . 3_676 ? C32 C32 Cl3 Cl2 29.3(296) 3_676 . . 3_676 ? Cl2 C32 Cl3 C32 -29.3(296) 3_676 . . 3_676 ? Cl2 C32 Cl3 C32 1.1(11) . . . 3_676 ? Cl3 C32 Cl3 C32 0.001(3) 3_676 . . 3_676 ? C32 C32 Cl3 C32 0.000(3) 3_676 . . 3_676 ? _refine_diff_density_max 0.765 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.130