# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Nathan Jones' _publ_contact_author_email NJONES26@UWO.CA _publ_section_title ; Modular Syntheses of Chiral and Achiral C,N-Chelated Pd(II)-Pyridinylidenes ; loop_ _publ_author_name 'Nathan Jones' 'Jacquelyn T. Price' 'Elizabeth T. J. Strong' # Attachment '732628.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 732628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H16 F6 N4 O7 Pd S2' _chemical_formula_sum 'C15 H16 F6 N4 O7 Pd S2' _chemical_formula_weight 648.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8534(16) _cell_length_b 8.9797(18) _cell_length_c 17.407(4) _cell_angle_alpha 80.77(3) _cell_angle_beta 77.31(3) _cell_angle_gamma 77.95(3) _cell_volume 1162.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50261 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6591 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5621 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4025 _reflns_number_gt 3505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SMART (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SMART (Bruker, 1997)' _computing_publication_material 'Bruker SMART (Bruker, 1997)' _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^)+(0.0535P)^2^+3.3902P] 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 4025 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 -0.43605(4) 0.92368(4) 0.75149(2) 0.02615(14) Uani 1 1 d . . . N1 N -0.1333(3) 1.0631(3) 0.74752(15) 0.0297(9) Uani 1 1 d G . . C2 C -0.2906(3) 1.0868(3) 0.71945(16) 0.0263(9) Uani 1 1 d G . . C3 C -0.3405(3) 1.2213(3) 0.67147(17) 0.0272(10) Uani 1 1 d G . . C4 C -0.2331(4) 1.3320(3) 0.65155(17) 0.0348(11) Uani 1 1 d G . . H4A H -0.2672 1.4239 0.6188 0.042 Uiso 1 1 calc R . . C5 C -0.0758(4) 1.3084(3) 0.67962(19) 0.0384(12) Uani 1 1 d G . . H5A H -0.0024 1.3841 0.6660 0.046 Uiso 1 1 calc R . . C6 C -0.0259(3) 1.1739(3) 0.72760(18) 0.0334(11) Uani 1 1 d G . . H6A H 0.0816 1.1577 0.7468 0.040 Uiso 1 1 calc R . . N2 N -0.3202(5) 0.8372(4) 0.6506(2) 0.0298(9) Uani 1 1 d . . . C9 C -0.2677(6) 0.7864(5) 0.5929(3) 0.0290(10) Uani 1 1 d . . . C10 C -0.1994(7) 0.7221(6) 0.5182(3) 0.0393(12) Uani 1 1 d . . . H10A H -0.2217 0.8016 0.4741 0.059 Uiso 1 1 calc R . . H10B H -0.2591 0.6371 0.5172 0.059 Uiso 1 1 calc R . . H10C H -0.0715 0.6844 0.5130 0.059 Uiso 1 1 calc R . . N4 N -0.5520(5) 1.0168(5) 0.8503(2) 0.0306(9) Uani 1 1 d . . . C7 C -0.6191(6) 1.0644(5) 0.9084(3) 0.0301(10) Uani 1 1 d . . . C8 C -0.7001(7) 1.1232(6) 0.9829(3) 0.0371(11) Uani 1 1 d . . . H8A H -0.7067 1.0376 1.0256 0.056 Uiso 1 1 calc R . . H8B H -0.8199 1.1798 0.9800 0.056 Uiso 1 1 calc R . . H8C H -0.6286 1.1919 0.9938 0.056 Uiso 1 1 calc R . . N3 N -0.5790(5) 0.7458(5) 0.7863(2) 0.0337(9) Uani 1 1 d . . . C13 C -0.6316(6) 0.6357(6) 0.8077(3) 0.0324(11) Uani 1 1 d . . . C14 C -0.6947(8) 0.4907(6) 0.8365(4) 0.0493(14) Uani 1 1 d . . . H14A H -0.5929 0.4064 0.8368 0.074 Uiso 1 1 calc R . . H14B H -0.7691 0.4733 0.8015 0.074 Uiso 1 1 calc R . . H14C H -0.7645 0.4952 0.8904 0.074 Uiso 1 1 calc R . . S1 S -0.74704(16) 0.64740(13) 0.60445(8) 0.0311(3) Uani 1 1 d . . . O1 O -0.8879(5) 0.6302(4) 0.6714(2) 0.0489(10) Uani 1 1 d . . . O2 O -0.7714(6) 0.6002(5) 0.5336(3) 0.0543(11) Uani 1 1 d . . . O3 O -0.5718(5) 0.6013(4) 0.6213(3) 0.0485(10) Uani 1 1 d . . . C1 C -0.7680(6) 0.8536(6) 0.5813(3) 0.0344(11) Uani 1 1 d . . . F1 F -0.9244(5) 0.9191(4) 0.5640(2) 0.0593(10) Uani 1 1 d . . . F2 F -0.7500(4) 0.9199(3) 0.64089(19) 0.0452(8) Uani 1 1 d . . . F3 F -0.6438(5) 0.8929(4) 0.5199(2) 0.0638(10) Uani 1 1 d . . . S2 S -0.17991(18) 0.28491(16) 0.92804(8) 0.0411(3) Uani 1 1 d . . . F4 F -0.3829(4) 0.5565(4) 0.9337(2) 0.0574(9) Uani 1 1 d . . . O5 O -0.0028(5) 0.2398(5) 0.8847(2) 0.0487(10) Uani 1 1 d . . . F6 F -0.1963(5) 0.5312(4) 0.8254(2) 0.0675(11) Uani 1 1 d . . . F5 F -0.1103(5) 0.5564(4) 0.9296(3) 0.0726(12) Uani 1 1 d . . . O4 O -0.3152(6) 0.2383(5) 0.8982(3) 0.0596(12) Uani 1 1 d . . . O7 O -0.6218(5) 1.1801(4) 0.6619(2) 0.0472(10) Uani 1 1 d . . . O6 O -0.1972(7) 0.2650(5) 1.0121(3) 0.0676(13) Uani 1 1 d . . . C12 C -0.5004(6) 1.2481(5) 0.6381(3) 0.0336(11) Uani 1 1 d . . . H12A H -0.5094 1.3252 0.5941 0.040 Uiso 1 1 calc R . . C11 C -0.0743(7) 0.9233(6) 0.7972(3) 0.0406(12) Uani 1 1 d . . . H11A H -0.1622 0.8560 0.8069 0.061 Uiso 1 1 calc R . . H11B H -0.0611 0.9494 0.8478 0.061 Uiso 1 1 calc R . . H11C H 0.0400 0.8705 0.7702 0.061 Uiso 1 1 calc R . . C20 C -0.2202(7) 0.4913(7) 0.9029(3) 0.0431(13) 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 0.0248(2) 0.0276(2) 0.0291(2) -0.00349(14) -0.00316(14) -0.01362(14) N1 0.024(2) 0.038(2) 0.029(2) -0.0082(17) -0.0028(16) -0.0088(17) C2 0.023(2) 0.032(2) 0.028(2) -0.0111(19) -0.0014(18) -0.0096(19) C3 0.025(2) 0.032(2) 0.027(2) -0.0066(19) -0.0011(18) -0.0112(19) C4 0.039(3) 0.030(3) 0.038(3) -0.004(2) -0.004(2) -0.015(2) C5 0.030(3) 0.046(3) 0.045(3) -0.014(2) 0.004(2) -0.025(2) C6 0.021(2) 0.046(3) 0.038(3) -0.017(2) -0.001(2) -0.014(2) N2 0.027(2) 0.028(2) 0.039(2) -0.0061(18) -0.0054(18) -0.0152(16) C9 0.024(2) 0.027(2) 0.038(3) -0.005(2) -0.003(2) -0.0135(19) C10 0.041(3) 0.038(3) 0.042(3) -0.015(2) -0.001(2) -0.012(2) N4 0.030(2) 0.034(2) 0.032(2) -0.0038(18) -0.0048(18) -0.0173(17) C7 0.027(2) 0.031(2) 0.036(3) 0.002(2) -0.011(2) -0.012(2) C8 0.037(3) 0.042(3) 0.034(3) -0.009(2) -0.005(2) -0.007(2) N3 0.031(2) 0.037(2) 0.036(2) -0.0033(19) -0.0080(18) -0.0133(19) C13 0.035(3) 0.033(3) 0.033(3) 0.002(2) -0.006(2) -0.019(2) C14 0.051(3) 0.041(3) 0.060(4) 0.005(3) -0.008(3) -0.030(3) S1 0.0285(6) 0.0271(6) 0.0422(7) -0.0059(5) -0.0085(5) -0.0120(5) O1 0.046(2) 0.039(2) 0.056(2) 0.0001(18) 0.0072(19) -0.0187(18) O2 0.069(3) 0.049(2) 0.057(3) -0.021(2) -0.021(2) -0.017(2) O3 0.034(2) 0.036(2) 0.083(3) -0.016(2) -0.020(2) -0.0068(16) C1 0.031(3) 0.036(3) 0.039(3) -0.003(2) -0.007(2) -0.011(2) F1 0.054(2) 0.0415(18) 0.092(3) 0.0057(18) -0.043(2) -0.0106(16) F2 0.0487(19) 0.0360(16) 0.058(2) -0.0186(14) -0.0132(15) -0.0116(14) F3 0.080(3) 0.0459(19) 0.059(2) -0.0028(16) 0.0169(19) -0.0312(18) S2 0.0394(7) 0.0435(7) 0.0424(7) -0.0084(6) -0.0068(6) -0.0107(6) F4 0.0373(18) 0.059(2) 0.070(2) -0.0159(18) 0.0000(16) -0.0009(15) O5 0.038(2) 0.059(2) 0.051(2) -0.0171(19) -0.0122(18) 0.0007(18) F6 0.079(3) 0.057(2) 0.053(2) 0.0026(17) 0.0041(19) -0.0064(19) F5 0.053(2) 0.064(2) 0.116(3) -0.038(2) -0.017(2) -0.0245(18) O4 0.045(2) 0.059(3) 0.085(3) -0.018(2) -0.011(2) -0.027(2) O7 0.035(2) 0.045(2) 0.065(3) -0.0023(19) -0.0146(18) -0.0140(17) O6 0.084(4) 0.069(3) 0.041(2) -0.002(2) -0.003(2) -0.008(3) C12 0.035(3) 0.027(2) 0.042(3) -0.005(2) -0.010(2) -0.010(2) C11 0.028(3) 0.054(3) 0.041(3) -0.010(3) -0.011(2) 0.000(2) C20 0.030(3) 0.053(3) 0.049(3) -0.013(3) -0.003(2) -0.015(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 C2 1.979(2) . ? Pd1 N4 1.986(4) . ? Pd1 N2 1.989(4) . ? Pd1 N3 2.078(4) . ? N1 C2 1.3900 . ? N1 C6 1.3900 . ? N1 C11 1.457(6) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C12 1.457(5) . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N2 C9 1.129(6) . ? C9 C10 1.454(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N4 C7 1.137(6) . ? C7 C8 1.443(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 C13 1.128(6) . ? C13 C14 1.464(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? S1 O2 1.430(4) . ? S1 O3 1.432(4) . ? S1 O1 1.432(4) . ? S1 C1 1.811(5) . ? C1 F2 1.322(6) . ? C1 F1 1.323(6) . ? C1 F3 1.335(6) . ? S2 O6 1.425(5) . ? S2 O5 1.439(4) . ? S2 O4 1.440(4) . ? S2 C20 1.812(6) . ? F4 C20 1.323(6) . ? F6 C20 1.320(7) . ? F5 C20 1.333(6) . ? O7 C12 1.200(6) . ? C12 H12A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 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 N4 89.72(14) . . ? C2 Pd1 N2 88.86(14) . . ? N4 Pd1 N2 178.14(16) . . ? C2 Pd1 N3 177.50(14) . . ? N4 Pd1 N3 90.94(16) . . ? N2 Pd1 N3 90.53(16) . . ? C2 N1 C6 120.0 . . ? C2 N1 C11 122.0(3) . . ? C6 N1 C11 118.0(3) . . ? N1 C2 C3 120.0 . . ? N1 C2 Pd1 117.23(14) . . ? C3 C2 Pd1 122.77(14) . . ? C4 C3 C2 120.0 . . ? C4 C3 C12 118.1(3) . . ? C2 C3 C12 121.8(3) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 N1 120.0 . . ? C5 C6 H6A 120.0 . . ? N1 C6 H6A 120.0 . . ? C9 N2 Pd1 174.4(4) . . ? N2 C9 C10 179.5(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 N4 Pd1 177.2(4) . . ? N4 C7 C8 178.5(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 N3 Pd1 168.9(4) . . ? N3 C13 C14 178.1(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 S1 O3 115.4(3) . . ? O2 S1 O1 114.7(3) . . ? O3 S1 O1 115.1(3) . . ? O2 S1 C1 103.2(2) . . ? O3 S1 C1 103.0(2) . . ? O1 S1 C1 103.0(2) . . ? F2 C1 F1 106.3(4) . . ? F2 C1 F3 105.9(4) . . ? F1 C1 F3 107.6(4) . . ? F2 C1 S1 112.4(3) . . ? F1 C1 S1 112.3(3) . . ? F3 C1 S1 111.9(4) . . ? O6 S2 O5 114.9(3) . . ? O6 S2 O4 116.0(3) . . ? O5 S2 O4 114.1(3) . . ? O6 S2 C20 103.7(3) . . ? O5 S2 C20 102.7(3) . . ? O4 S2 C20 102.9(3) . . ? O7 C12 C3 124.9(5) . . ? O7 C12 H12A 117.5 . . ? C3 C12 H12A 117.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? F6 C20 F4 107.4(5) . . ? F6 C20 F5 106.6(5) . . ? F4 C20 F5 106.4(4) . . ? F6 C20 S2 111.9(4) . . ? F4 C20 S2 112.7(4) . . ? F5 C20 S2 111.5(4) . . ? _diffrn_measured_fraction_theta_max .978 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full .978 _refine_diff_density_max .830 _refine_diff_density_min -1.265 _refine_diff_density_rms .108 # Attachment '732629.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 732629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 F6 N6 O6 Pd S2' _chemical_formula_weight 843.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.968(3) _cell_length_b 13.049(3) _cell_length_c 22.681(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3838.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55219 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle/plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7024 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8748 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8748 _reflns_number_gt 7888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SMART (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SMART (Bruker, 1997)' _computing_publication_material 'Bruker SMART (Bruker, 1997)' _refine_special_details ; The acetonitrile was modeled in two parts. One part being 0.4 of one molecule and the other being 0.6. 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^)+(0.0805P)^2^+4.7287P] 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 -0.01(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 8748 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.042 _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 0.39316(2) 1.87253(2) 0.211825(14) 0.03137(10) Uani 1 1 d . . . C10 C 0.5728(7) 0.4788(7) -0.0076(3) 0.074(2) Uani 1 1 d . . . F3 F 0.4716(5) 0.4828(5) -0.0186(3) 0.122(2) Uani 1 1 d . . . F2 F 0.6150(6) 0.4371(4) -0.0519(2) 0.125(2) Uani 1 1 d . . . F1 F 0.5883(7) 0.4185(4) 0.0389(2) 0.134(3) Uani 1 1 d . . . S1 S 0.62157(11) 0.60661(10) 0.00873(6) 0.0445(3) Uani 1 1 d . . . O3 O 0.7262(3) 0.5896(4) 0.0235(2) 0.0643(12) Uani 1 1 d . . . O2 O 0.5605(4) 0.6372(4) 0.0573(2) 0.0743(14) Uani 1 1 d . . . O1 O 0.6104(5) 0.6600(5) -0.0454(2) 0.0933(18) Uani 1 1 d . . . S2 S 0.79579(9) 1.73432(10) 0.25010(6) 0.0403(3) Uani 1 1 d . . . O4 O 0.8852(3) 1.7843(3) 0.22688(18) 0.0537(9) Uani 1 1 d . . . O5 O 0.7336(3) 1.7981(3) 0.2874(2) 0.0580(10) Uani 1 1 d . . . O6 O 0.7400(3) 1.6729(3) 0.2086(2) 0.0510(9) Uani 1 1 d . . . C50 C 0.8480(4) 1.6403(5) 0.3008(3) 0.0556(15) Uani 1 1 d . . . F4 F 0.9093(3) 1.5739(3) 0.2727(2) 0.0841(14) Uani 1 1 d . . . F5 F 0.7737(3) 1.5874(3) 0.3271(2) 0.0789(13) Uani 1 1 d . . . F6 F 0.9055(3) 1.6856(3) 0.34237(17) 0.0725(11) Uani 1 1 d . . . N4 N 0.4517(3) 1.9561(3) 0.27911(17) 0.0313(8) Uani 1 1 d . . . C31 C 0.2660(3) 1.8849(3) 0.2615(2) 0.0322(9) Uani 1 1 d . . . C18 C 0.4871(3) 2.1385(3) 0.2163(2) 0.0384(10) Uani 1 1 d . . . H18A H 0.4246 2.1331 0.2380 0.046 Uiso 1 1 calc R . . C35 C 0.0943(4) 1.8616(4) 0.2942(2) 0.0443(11) Uani 1 1 d . . . H35A H 0.0270 1.8364 0.2861 0.053 Uiso 1 1 calc R . . N1 N 0.5341(3) 1.8617(3) 0.16798(17) 0.0363(8) Uani 1 1 d . . . C11 C 0.7553(4) 2.0300(4) 0.2143(3) 0.0448(11) Uani 1 1 d . . . H11A H 0.7526 1.9813 0.2454 0.054 Uiso 1 1 calc R . . C23 C 0.3886(4) 1.9772(3) 0.3202(2) 0.0358(9) Uani 1 1 d . . . H23A H 0.4087 2.0171 0.3533 0.043 Uiso 1 1 calc R . . C201 C 0.5591(3) 1.9933(4) 0.2774(2) 0.0322(9) Uani 1 1 d . . . H20A H 0.6035 1.9342 0.2656 0.039 Uiso 1 1 calc R . . C15 C 0.6725(4) 2.1595(4) 0.1532(2) 0.0424(12) Uani 1 1 d . . . C20 C 0.6663(4) 2.0869(4) 0.2003(2) 0.0362(10) Uani 1 1 d . . . N3 N 0.1694(3) 1.8486(3) 0.2536(2) 0.0405(9) Uani 1 1 d . . . C41 C 0.6064(4) 1.8500(4) 0.1415(2) 0.0398(10) Uani 1 1 d . . . C17 C 0.4958(4) 2.2105(4) 0.1701(3) 0.0457(12) Uani 1 1 d . . . H17A H 0.4387 2.2530 0.1607 0.055 Uiso 1 1 calc R . . C43 C 0.3270(4) 1.7506(4) 0.0993(2) 0.0386(10) Uani 1 1 d . . . C34 C 0.1126(4) 1.9101(4) 0.3465(2) 0.0444(11) Uani 1 1 d . . . H34A H 0.0597 1.9157 0.3753 0.053 Uiso 1 1 calc R . . N2 N 0.3391(3) 1.7933(3) 0.14135(19) 0.0377(9) Uani 1 1 d . . . C16 C 0.5832(4) 2.2195(4) 0.1396(3) 0.0463(13) Uani 1 1 d . . . H16A H 0.5864 2.2671 0.1080 0.056 Uiso 1 1 calc R . . C33 C 0.2096(4) 1.9509(4) 0.3570(2) 0.0444(12) Uani 1 1 d . . . H33A H 0.2240 1.9870 0.3925 0.053 Uiso 1 1 calc R . . C19 C 0.5703(4) 2.0753(4) 0.2301(2) 0.0332(9) Uani 1 1 d . . . C12 C 0.8458(4) 2.0436(5) 0.1840(3) 0.0580(16) Uani 1 1 d . . . H12A H 0.9050 2.0047 0.1944 0.070 Uiso 1 1 calc R . . C14 C 0.7654(5) 2.1715(5) 0.1215(3) 0.0564(16) Uani 1 1 d . . . H14A H 0.7687 2.2182 0.0894 0.068 Uiso 1 1 calc R . . C44 C 0.3123(5) 1.6938(4) 0.0449(2) 0.0487(13) Uani 1 1 d . . . H44A H 0.3693 1.6454 0.0397 0.073 Uiso 1 1 calc R . . H44B H 0.3106 1.7416 0.0116 0.073 Uiso 1 1 calc R . . H44C H 0.2470 1.6561 0.0468 0.073 Uiso 1 1 calc R . . C13 C 0.8516(5) 2.1153(5) 0.1371(3) 0.0615(17) Uani 1 1 d . . . H13A H 0.9146 2.1248 0.1165 0.074 Uiso 1 1 calc R . . C42 C 0.7008(4) 1.8369(5) 0.1072(3) 0.0505(14) Uani 1 1 d . . . H42A H 0.6997 1.8834 0.0733 0.076 Uiso 1 1 calc R . . H42B H 0.7053 1.7660 0.0933 0.076 Uiso 1 1 calc R . . H42C H 0.7606 1.8525 0.1321 0.076 Uiso 1 1 calc R . . C22 C 0.5970(4) 2.0303(4) 0.3378(2) 0.0438(11) Uani 1 1 d . . . H22A H 0.5889 1.9751 0.3668 0.066 Uiso 1 1 calc R . . H22B H 0.5564 2.0899 0.3502 0.066 Uiso 1 1 calc R . . H22C H 0.6699 2.0495 0.3351 0.066 Uiso 1 1 calc R . . C36 C 0.1402(5) 1.7912(7) 0.2001(4) 0.086(3) Uani 1 1 d . . . H36A H 0.0674 1.7717 0.2025 0.129 Uiso 1 1 calc R . . H36B H 0.1828 1.7294 0.1969 0.129 Uiso 1 1 calc R . . H36C H 0.1511 1.8344 0.1653 0.129 Uiso 1 1 calc R . . C32 C 0.2850(3) 1.9377(4) 0.3143(2) 0.0331(9) Uani 1 1 d . . . N6 N 0.1175(6) 1.5699(6) 0.1340(4) 0.090(2) Uani 1 1 d . . . C400 C 0.0456(6) 1.6088(6) 0.1156(3) 0.0677(19) Uani 1 1 d . . . C401 C -0.0463(6) 1.6613(7) 0.0943(4) 0.076(2) Uani 1 1 d . . . H40A H -0.0943 1.6717 0.1272 0.113 Uiso 1 1 calc R . . H40B H -0.0797 1.6196 0.0639 0.113 Uiso 1 1 calc R . . H40C H -0.0268 1.7278 0.0777 0.113 Uiso 1 1 calc R . . N7 N 0.8497(12) -0.0155(11) 0.5051(5) 0.059(4) Uani 0.40 1 d P A 1 C601 C 0.8248(10) -0.0790(8) 0.4778(5) 0.032(2) Uani 0.40 1 d P A 1 C600 C 0.8055(13) -0.1579(10) 0.4431(6) 0.048(3) Uani 0.40 1 d P A 1 H60A H 0.7312 -0.1716 0.4427 0.072 Uiso 0.40 1 calc PR A 1 H60B H 0.8422 -0.2184 0.4578 0.072 Uiso 0.40 1 calc PR A 1 H60C H 0.8288 -0.1423 0.4029 0.072 Uiso 0.40 1 calc PR A 1 N5 N 1.0929(10) -0.1787(9) 0.4885(5) 0.079(3) Uani 0.60 1 d P B 2 C500 C 1.0966(8) -0.1134(8) 0.5208(4) 0.049(2) Uani 0.60 1 d P B 2 C501 C 1.0961(9) -0.0301(7) 0.5621(4) 0.056(3) Uani 0.60 1 d P B 2 H50A H 1.1625 0.0057 0.5605 0.085 Uiso 0.60 1 calc PR B 2 H50B H 1.0849 -0.0568 0.6020 0.085 Uiso 0.60 1 calc PR B 2 H50C H 1.0406 0.0177 0.5520 0.085 Uiso 0.60 1 calc PR B 2 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 0.02624(14) 0.03171(15) 0.03615(16) -0.00375(14) -0.00078(14) -0.00215(13) C10 0.094(6) 0.079(5) 0.050(4) -0.010(4) -0.002(4) -0.014(4) F3 0.095(4) 0.140(5) 0.132(5) -0.045(4) -0.023(4) -0.045(4) F2 0.197(7) 0.093(3) 0.084(3) -0.043(3) 0.014(4) 0.004(4) F1 0.255(9) 0.058(3) 0.091(4) 0.013(3) -0.022(5) -0.050(4) S1 0.0447(7) 0.0469(7) 0.0420(6) 0.0061(5) -0.0020(5) -0.0023(5) O3 0.048(2) 0.070(3) 0.075(3) 0.009(2) -0.008(2) 0.010(2) O2 0.063(3) 0.083(3) 0.077(3) -0.028(3) 0.015(2) -0.012(3) O1 0.105(4) 0.097(4) 0.078(3) 0.047(3) -0.020(3) -0.024(4) S2 0.0284(5) 0.0426(6) 0.0498(7) -0.0004(5) -0.0023(5) -0.0036(5) O4 0.0333(18) 0.065(2) 0.063(2) 0.0073(18) -0.0006(18) -0.0172(18) O5 0.045(2) 0.054(2) 0.075(3) -0.008(2) 0.007(2) 0.0031(17) O6 0.0377(18) 0.059(2) 0.057(2) -0.005(2) -0.0115(19) -0.0104(16) C50 0.042(3) 0.058(4) 0.067(4) 0.003(3) -0.013(3) -0.010(3) F4 0.067(3) 0.062(2) 0.124(4) -0.018(2) -0.026(3) 0.024(2) F5 0.075(3) 0.079(3) 0.083(3) 0.033(2) -0.011(2) -0.022(2) F6 0.067(3) 0.084(3) 0.066(2) 0.001(2) -0.028(2) -0.008(2) N4 0.0252(17) 0.0345(18) 0.034(2) -0.0038(15) -0.0019(15) -0.0025(14) C31 0.030(2) 0.027(2) 0.039(2) -0.0014(18) 0.0026(17) -0.0006(18) C18 0.031(2) 0.034(2) 0.050(3) -0.005(2) 0.003(2) -0.0041(18) C35 0.029(2) 0.045(3) 0.059(3) -0.001(2) 0.007(2) -0.003(2) N1 0.0280(17) 0.043(2) 0.0376(19) -0.0072(18) 0.0024(15) -0.0032(17) C11 0.034(2) 0.043(3) 0.058(3) -0.010(3) 0.009(3) -0.005(2) C23 0.032(2) 0.036(2) 0.040(2) -0.0022(18) -0.005(2) -0.001(2) C201 0.0241(19) 0.038(2) 0.035(2) -0.0065(18) -0.0020(17) -0.0116(17) C15 0.040(3) 0.039(3) 0.048(3) -0.008(2) 0.009(2) -0.012(2) C20 0.031(2) 0.036(2) 0.043(3) -0.0105(19) 0.0076(19) -0.0111(18) N3 0.0287(18) 0.043(2) 0.050(2) -0.0134(18) 0.0032(18) -0.0091(16) C41 0.035(2) 0.046(3) 0.038(2) -0.0074(18) 0.000(2) -0.002(2) C17 0.041(3) 0.039(3) 0.058(3) 0.005(2) -0.004(3) -0.002(2) C43 0.038(2) 0.041(3) 0.037(3) -0.001(2) -0.005(2) 0.000(2) C34 0.033(2) 0.049(3) 0.052(3) 0.001(2) 0.009(2) 0.000(2) N2 0.032(2) 0.041(2) 0.040(2) -0.0047(18) -0.0055(17) -0.0013(17) C16 0.055(3) 0.038(3) 0.046(3) 0.003(2) -0.001(2) -0.010(2) C33 0.038(3) 0.052(3) 0.043(3) -0.004(2) 0.005(2) -0.002(2) C19 0.028(2) 0.034(2) 0.038(2) -0.0052(18) 0.0018(17) -0.0022(17) C12 0.030(3) 0.059(4) 0.085(4) -0.019(3) 0.013(3) -0.005(2) C14 0.058(4) 0.058(3) 0.053(3) -0.013(3) 0.018(3) -0.026(3) C44 0.061(3) 0.052(3) 0.034(3) -0.011(2) -0.012(2) 0.008(3) C13 0.043(3) 0.065(4) 0.076(4) -0.023(3) 0.027(3) -0.021(3) C42 0.036(3) 0.071(4) 0.045(3) -0.008(3) 0.011(2) -0.002(2) C22 0.037(3) 0.054(3) 0.041(2) -0.008(2) -0.004(2) -0.009(2) C36 0.044(3) 0.126(7) 0.089(5) -0.066(5) 0.006(3) -0.025(4) C32 0.028(2) 0.032(2) 0.039(2) 0.0009(19) 0.0012(18) -0.0017(17) N6 0.065(4) 0.094(5) 0.111(6) -0.016(4) -0.007(4) 0.002(4) C400 0.052(4) 0.076(5) 0.074(4) -0.013(4) 0.001(3) -0.016(3) C401 0.055(4) 0.100(6) 0.072(5) 0.008(4) -0.009(3) -0.015(4) N7 0.084(10) 0.052(8) 0.042(6) 0.022(6) 0.011(6) 0.024(7) C601 0.052(7) 0.019(5) 0.026(5) 0.004(4) 0.020(5) 0.014(5) C600 0.068(9) 0.038(6) 0.037(6) -0.002(5) 0.006(6) -0.010(6) N5 0.087(8) 0.089(7) 0.062(6) 0.001(5) 0.023(6) 0.023(6) C500 0.060(6) 0.056(5) 0.032(4) 0.000(4) 0.017(4) 0.013(5) C501 0.078(7) 0.050(5) 0.041(4) -0.012(4) 0.025(5) -0.019(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 C31 2.004(4) . ? Pd1 N4 2.024(4) . ? Pd1 N2 2.028(4) . ? Pd1 N1 2.086(4) . ? C10 F2 1.267(9) . ? C10 F1 1.330(9) . ? C10 F3 1.338(10) . ? C10 S1 1.821(8) . ? S1 O2 1.415(5) . ? S1 O3 1.416(5) . ? S1 O1 1.419(5) . ? S2 O4 1.431(4) . ? S2 O6 1.433(4) . ? S2 O5 1.435(4) . ? S2 C50 1.812(6) . ? C50 F5 1.328(7) . ? C50 F4 1.338(8) . ? C50 F6 1.340(7) . ? N4 C23 1.271(6) . ? N4 C201 1.474(5) . ? C31 N3 1.351(6) . ? C31 C32 1.403(7) . ? C18 C19 1.393(7) . ? C18 C17 1.412(7) . ? C18 H18A 0.9500 . ? C35 N3 1.352(6) . ? C35 C34 1.366(8) . ? C35 H35A 0.9500 . ? N1 C41 1.123(6) . ? C11 C12 1.372(8) . ? C11 C20 1.409(7) . ? C11 H11A 0.9500 . ? C23 C32 1.446(6) . ? C23 H23A 0.9500 . ? C201 C19 1.522(7) . ? C201 C22 1.534(6) . ? C201 H20A 1.0000 . ? C15 C14 1.411(8) . ? C15 C20 1.430(7) . ? C15 C16 1.431(8) . ? C20 C19 1.426(6) . ? N3 C36 1.476(7) . ? C41 C42 1.460(7) . ? C17 C16 1.334(8) . ? C17 H17A 0.9500 . ? C43 N2 1.116(6) . ? C43 C44 1.452(7) . ? C34 C33 1.386(8) . ? C34 H34A 0.9500 . ? C16 H16A 0.9500 . ? C33 C32 1.386(7) . ? C33 H33A 0.9500 . ? C12 C13 1.418(10) . ? C12 H12A 0.9500 . ? C14 C13 1.383(10) . ? C14 H14A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C13 H13A 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N6 C400 1.142(10) . ? C400 C401 1.456(11) . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 0.9800 . ? N7 C601 1.084(19) . ? C601 C600 1.320(17) . ? C600 H60A 0.9800 . ? C600 H60B 0.9800 . ? C600 H60C 0.9800 . ? N5 C500 1.125(14) . ? C500 C501 1.435(12) . ? C501 H50A 0.9800 . ? C501 H50B 0.9800 . ? C501 H50C 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 C31 Pd1 N4 80.85(17) . . ? C31 Pd1 N2 101.56(17) . . ? N4 Pd1 N2 176.91(17) . . ? C31 Pd1 N1 174.15(17) . . ? N4 Pd1 N1 93.85(15) . . ? N2 Pd1 N1 83.83(16) . . ? F2 C10 F1 108.0(8) . . ? F2 C10 F3 107.0(7) . . ? F1 C10 F3 108.6(8) . . ? F2 C10 S1 113.8(6) . . ? F1 C10 S1 109.2(5) . . ? F3 C10 S1 110.1(6) . . ? O2 S1 O3 113.4(3) . . ? O2 S1 O1 118.6(4) . . ? O3 S1 O1 112.3(4) . . ? O2 S1 C10 102.8(3) . . ? O3 S1 C10 103.7(4) . . ? O1 S1 C10 103.8(4) . . ? O4 S2 O6 115.0(3) . . ? O4 S2 O5 114.1(3) . . ? O6 S2 O5 115.4(3) . . ? O4 S2 C50 103.9(3) . . ? O6 S2 C50 103.1(3) . . ? O5 S2 C50 103.2(3) . . ? F5 C50 F4 108.0(6) . . ? F5 C50 F6 108.5(5) . . ? F4 C50 F6 106.8(5) . . ? F5 C50 S2 111.5(4) . . ? F4 C50 S2 111.0(5) . . ? F6 C50 S2 110.8(4) . . ? C23 N4 C201 123.8(4) . . ? C23 N4 Pd1 115.4(3) . . ? C201 N4 Pd1 120.8(3) . . ? N3 C31 C32 116.7(4) . . ? N3 C31 Pd1 131.2(3) . . ? C32 C31 Pd1 112.1(3) . . ? C19 C18 C17 119.9(5) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? N3 C35 C34 121.6(4) . . ? N3 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C41 N1 Pd1 174.4(4) . . ? C12 C11 C20 121.3(6) . . ? C12 C11 H11A 119.4 . . ? C20 C11 H11A 119.4 . . ? N4 C23 C32 117.0(4) . . ? N4 C23 H23A 121.5 . . ? C32 C23 H23A 121.5 . . ? N4 C201 C19 109.9(4) . . ? N4 C201 C22 112.5(4) . . ? C19 C201 C22 112.2(4) . . ? N4 C201 H20A 107.3 . . ? C19 C201 H20A 107.3 . . ? C22 C201 H20A 107.3 . . ? C14 C15 C20 120.1(6) . . ? C14 C15 C16 121.4(5) . . ? C20 C15 C16 118.5(5) . . ? C11 C20 C19 123.5(5) . . ? C11 C20 C15 118.2(5) . . ? C19 C20 C15 118.3(5) . . ? C31 N3 C35 122.3(4) . . ? C31 N3 C36 121.7(4) . . ? C35 N3 C36 116.0(4) . . ? N1 C41 C42 178.9(6) . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? N2 C43 C44 179.1(6) . . ? C35 C34 C33 119.1(5) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? C43 N2 Pd1 167.6(4) . . ? C17 C16 C15 121.9(5) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C34 C33 C32 118.1(5) . . ? C34 C33 H33A 120.9 . . ? C32 C33 H33A 120.9 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 C201 120.0(4) . . ? C20 C19 C201 119.5(4) . . ? C11 C12 C13 120.4(6) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C14 C13 C12 120.0(5) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C201 C22 H22A 109.5 . . ? C201 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C201 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C32 C31 122.2(4) . . ? C33 C32 C23 123.1(5) . . ? C31 C32 C23 114.6(4) . . ? N6 C400 C401 177.5(9) . . ? C400 C401 H40A 109.5 . . ? C400 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C400 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? N7 C601 C600 173.6(16) . . ? C601 C600 H60A 109.5 . . ? C601 C600 H60B 109.5 . . ? H60A C600 H60B 109.5 . . ? C601 C600 H60C 109.5 . . ? H60A C600 H60C 109.5 . . ? H60B C600 H60C 109.5 . . ? N5 C500 C501 177.3(13) . . ? C500 C501 H50A 109.5 . . ? C500 C501 H50B 109.5 . . ? H50A C501 H50B 109.5 . . ? C500 C501 H50C 109.5 . . ? H50A C501 H50C 109.5 . . ? H50B C501 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .616 _refine_diff_density_min -.988 _refine_diff_density_rms .109 # Attachment '732630.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 732630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H17 Cl N3 O Pd), 2(C F3 O3 S), C2 H3 N' _chemical_formula_sum 'C36 H37 Cl2 F6 N7 O8 Pd2 S2' _chemical_formula_weight 1157.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.107(3) _cell_length_b 13.283(3) _cell_length_c 14.155(3) _cell_angle_alpha 98.15(3) _cell_angle_beta 115.18(3) _cell_angle_gamma 98.29(3) _cell_volume 2149.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15412 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 30.3 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_T_max 0.8472 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11969 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7561 _reflns_number_gt 6827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SMART (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SMART (Bruker, 1997)' _computing_publication_material 'Bruker SMART (Bruker, 1997)' _refine_special_details ; The triflate was solved in two parts and was attempted anisotropically, however it was found to be unstable and had to be left isotropic. Before merging there were 26707 reflections. 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^)+(0.0390P)^2^+9.6928P] 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 7561 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 S1 S 0.10860(10) -0.06842(9) -0.25047(9) 0.0303(2) Uani 1 1 d . . . O1 O 0.0303(4) -0.1200(4) -0.2182(4) 0.0626(12) Uani 1 1 d . . . O2 O 0.0574(3) -0.0370(3) -0.3467(3) 0.0432(9) Uani 1 1 d . . . O3 O 0.2034(4) -0.1177(3) -0.2376(3) 0.0483(10) Uani 1 1 d . . . C10 C 0.1781(5) 0.0545(5) -0.1569(4) 0.0468(13) Uani 1 1 d . . . F1 F 0.2544(4) 0.1109(3) -0.1761(3) 0.0826(13) Uani 1 1 d . . . F2 F 0.2328(3) 0.0403(4) -0.0615(3) 0.0754(12) Uani 1 1 d . . . F3 F 0.1006(4) 0.1093(3) -0.1584(3) 0.0853(14) Uani 1 1 d . . . S2 S 0.62617(12) 0.48293(11) 0.31180(11) 0.0265(2) Uiso 0.70 1 d PG A 1 O4 O 0.6959(2) 0.58089(15) 0.3829(2) 0.0443(4) Uiso 0.70 1 d PG A 1 O5 O 0.6846(2) 0.39907(18) 0.3210(2) 0.0443(4) Uiso 0.70 1 d PG A 1 O6 O 0.5545(2) 0.4888(2) 0.20421(13) 0.0443(4) Uiso 0.70 1 d PG A 1 C20 C 0.52354(17) 0.44646(18) 0.36116(17) 0.0390(3) Uiso 0.70 1 d PG A 1 F4 F 0.4502(2) 0.3575(2) 0.3065(3) 0.0674(6) Uiso 0.70 1 d PG A 1 F5 F 0.4599(2) 0.5137(3) 0.3597(3) 0.0674(6) Uiso 0.70 1 d PG A 1 F6 F 0.5716(3) 0.4366(3) 0.46006(19) 0.0674(6) Uiso 0.70 1 d PG A 1 S2' S 0.6630(3) 0.4868(3) 0.3362(3) 0.0311(6) Uiso 0.30 1 d PG B 2 O4' O 0.6800(5) 0.3863(4) 0.3034(6) 0.0519(10) Uiso 0.30 1 d PG B 2 O5' O 0.6291(6) 0.5453(5) 0.2549(5) 0.0519(10) Uiso 0.30 1 d PG B 2 O6' O 0.7496(4) 0.5455(5) 0.4395(4) 0.0519(10) Uiso 0.30 1 d PG B 2 C20' C 0.5360(4) 0.4562(5) 0.3557(5) 0.0457(8) Uiso 0.30 1 d PG B 2 F4' F 0.5046(6) 0.5385(6) 0.3864(7) 0.0790(15) Uiso 0.30 1 d PG B 2 F5' F 0.5483(7) 0.4018(7) 0.4280(6) 0.0790(15) Uiso 0.30 1 d PG B 2 F6' F 0.4448(3) 0.4017(7) 0.2695(6) 0.0790(15) Uiso 0.30 1 d PG B 2 Pd1 Pd 0.50240(2) 0.14562(2) -0.47633(2) 0.01696(9) Uani 1 1 d . . . Cl1 Cl 0.37480(9) 0.10860(8) -0.64925(8) 0.0259(2) Uani 1 1 d . . . C1 C 0.6479(3) 0.1316(3) -0.4842(3) 0.0188(8) Uani 1 1 d . . . N1 N 0.6788(3) 0.1271(3) -0.5620(3) 0.0208(7) Uani 1 1 d . . . Pd2 Pd -0.19237(3) -0.47968(2) -0.11215(2) 0.01910(9) Uani 1 1 d . . . Cl2 Cl -0.21257(10) -0.32641(8) -0.03683(9) 0.0315(2) Uani 1 1 d . . . N2 N 0.6088(3) 0.1635(3) -0.3228(3) 0.0194(7) Uani 1 1 d . . . C2 C 0.7808(4) 0.1046(3) -0.5513(4) 0.0263(9) Uani 1 1 d . . . H2 H 0.7964 0.1015 -0.6111 0.032 Uiso 1 1 calc R . . N3 N 0.3592(3) 0.1559(3) -0.4521(3) 0.0237(7) Uani 1 1 d . . . C3 C 0.8597(4) 0.0867(3) -0.4621(4) 0.0276(9) Uani 1 1 d . . . H3 H 0.9287 0.0686 -0.4581 0.033 Uiso 1 1 calc R . . N4 N -0.1336(3) -0.6049(3) -0.1530(3) 0.0209(7) Uani 1 1 d . . . C4 C 0.8365(4) 0.0957(3) -0.3773(4) 0.0262(9) Uani 1 1 d . . . H4 H 0.8907 0.0863 -0.3104 0.031 Uiso 1 1 calc R . . N5 N -0.2533(3) -0.5499(3) 0.0514(3) 0.0230(7) Uani 1 1 d . . . C5 C 0.7328(3) 0.1186(3) -0.3895(3) 0.0202(8) Uani 1 1 d . . . N6 N -0.1803(3) -0.4030(3) -0.2226(3) 0.0264(8) Uani 1 1 d . . . C6 C 0.7050(4) 0.1379(3) -0.3043(3) 0.0222(8) Uani 1 1 d . . . H6 H 0.7562 0.1321 -0.2346 0.027 Uiso 1 1 calc R . . O7 O 0.4977(3) 0.2663(3) 0.0002(3) 0.0413(8) Uani 1 1 d . . . C7 C 0.2805(4) 0.1666(3) -0.4407(3) 0.0238(9) Uani 1 1 d . . . O8 O 0.0048(3) -0.6531(3) -0.4640(2) 0.0370(8) Uani 1 1 d . . . C8 C 0.1804(4) 0.1816(4) -0.4267(4) 0.0368(11) Uani 1 1 d . . . H8A H 0.1851 0.2566 -0.4072 0.055 Uiso 1 1 calc R . . H8B H 0.1783 0.1488 -0.3695 0.055 Uiso 1 1 calc R . . H8C H 0.1099 0.1497 -0.4937 0.055 Uiso 1 1 calc R . . C9 C 0.6065(4) 0.1515(4) -0.6621(3) 0.0325(10) Uani 1 1 d . . . H9A H 0.5510 0.0877 -0.7120 0.049 Uiso 1 1 calc R . . H9B H 0.6551 0.1804 -0.6932 0.049 Uiso 1 1 calc R . . H9C H 0.5646 0.2029 -0.6492 0.049 Uiso 1 1 calc R . . C11 C 0.5789(3) 0.1857(3) -0.2396(3) 0.0213(8) Uani 1 1 d . . . C12 C 0.5292(4) 0.2700(3) -0.2316(3) 0.0249(9) Uani 1 1 d . . . H12 H 0.5139 0.3112 -0.2836 0.030 Uiso 1 1 calc R . . C13 C 0.5028(4) 0.2934(4) -0.1509(3) 0.0302(10) Uani 1 1 d . . . H13 H 0.4688 0.3510 -0.1451 0.036 Uiso 1 1 calc R . . C14 C 0.5254(4) 0.2334(4) -0.0775(3) 0.0307(10) Uani 1 1 d . . . C15 C 0.5735(4) 0.1482(4) -0.0853(3) 0.0311(10) Uani 1 1 d . . . H15 H 0.5880 0.1069 -0.0335 0.037 Uiso 1 1 calc R . . C16 C 0.5999(4) 0.1241(3) -0.1672(3) 0.0257(9) Uani 1 1 d . . . H16 H 0.6323 0.0656 -0.1740 0.031 Uiso 1 1 calc R . . C17 C 0.5110(5) 0.2051(5) 0.0748(4) 0.0504(15) Uani 1 1 d . . . H17A H 0.4638 0.1342 0.0379 0.076 Uiso 1 1 calc R . . H17B H 0.4861 0.2354 0.1264 0.076 Uiso 1 1 calc R . . H17C H 0.5926 0.2025 0.1127 0.076 Uiso 1 1 calc R . . C21 C -0.2014(3) -0.5596(3) -0.0109(3) 0.0213(8) Uani 1 1 d . . . C22 C -0.2355(4) -0.6063(4) 0.1256(3) 0.0307(10) Uani 1 1 d . . . H22 H -0.2708 -0.5959 0.1714 0.037 Uiso 1 1 calc R . . C23 C -0.1693(4) -0.6777(4) 0.1386(3) 0.0332(11) Uani 1 1 d . . . H23 H -0.1567 -0.7142 0.1943 0.040 Uiso 1 1 calc R . . C24 C -0.1208(4) -0.6972(3) 0.0717(3) 0.0282(9) Uani 1 1 d . . . H24 H -0.0769 -0.7489 0.0770 0.034 Uiso 1 1 calc R . . C25 C -0.1384(4) -0.6390(3) -0.0027(3) 0.0239(9) Uani 1 1 d . . . C26 C -0.1032(4) -0.6592(3) -0.0833(3) 0.0243(9) Uani 1 1 d . . . H26 H -0.0597 -0.7101 -0.0853 0.029 Uiso 1 1 calc R . . C27 C -0.1910(4) -0.3593(3) -0.2858(3) 0.0258(9) Uani 1 1 d . . . C28 C -0.2060(5) -0.3045(4) -0.3681(4) 0.0381(11) Uani 1 1 d . . . H28A H -0.2208 -0.3533 -0.4337 0.057 Uiso 1 1 calc R . . H28B H -0.1358 -0.2503 -0.3456 0.057 Uiso 1 1 calc R . . H28C H -0.2720 -0.2718 -0.3819 0.057 Uiso 1 1 calc R . . C29 C -0.3374(4) -0.4830(4) 0.0399(4) 0.0312(10) Uani 1 1 d . . . H29A H -0.2969 -0.4145 0.0889 0.047 Uiso 1 1 calc R . . H29B H -0.3971 -0.5160 0.0573 0.047 Uiso 1 1 calc R . . H29C H -0.3736 -0.4744 -0.0340 0.047 Uiso 1 1 calc R . . C31 C -0.1003(4) -0.6200(3) -0.2348(3) 0.0218(8) Uani 1 1 d . . . C32 C -0.1763(4) -0.6123(3) -0.3335(3) 0.0218(8) Uani 1 1 d . . . H32 H -0.2500 -0.5993 -0.3463 0.026 Uiso 1 1 calc R . . C33 C -0.1450(4) -0.6237(3) -0.4130(3) 0.0239(9) Uani 1 1 d . . . H33 H -0.1972 -0.6195 -0.4830 0.029 Uiso 1 1 calc R . . C34 C -0.0364(4) -0.6416(3) -0.3928(3) 0.0265(9) Uani 1 1 d . . . C35 C 0.0390(4) -0.6500(4) -0.2943(4) 0.0315(10) Uani 1 1 d . . . H35 H 0.1126 -0.6631 -0.2814 0.038 Uiso 1 1 calc R . . C36 C 0.0077(4) -0.6395(3) -0.2154(3) 0.0258(9) Uani 1 1 d . . . H36 H 0.0594 -0.6453 -0.1459 0.031 Uiso 1 1 calc R . . C37 C -0.0650(4) -0.6380(4) -0.5643(4) 0.0382(11) Uani 1 1 d . . . H37A H -0.1354 -0.6941 -0.6001 0.057 Uiso 1 1 calc R . . H37B H -0.0229 -0.6388 -0.6074 0.057 Uiso 1 1 calc R . . H37C H -0.0859 -0.5705 -0.5564 0.057 Uiso 1 1 calc R . . N7 N -0.1083(4) 0.0892(3) -0.0884(3) 0.0421(11) Uani 1 1 d . . . C41 C -0.1266(4) 0.0013(4) -0.1007(3) 0.0288(10) Uani 1 1 d . . . C42 C -0.1492(4) -0.1123(4) -0.1165(4) 0.0354(11) Uani 1 1 d . . . H42A H -0.1150 -0.1408 -0.1610 0.053 Uiso 1 1 calc R . . H42B H -0.2329 -0.1415 -0.1523 0.053 Uiso 1 1 calc R . . H42C H -0.1146 -0.1309 -0.0468 0.053 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 S1 0.0340(6) 0.0329(6) 0.0270(5) 0.0032(5) 0.0184(5) 0.0049(5) O1 0.055(3) 0.072(3) 0.067(3) 0.012(2) 0.042(2) -0.007(2) O2 0.044(2) 0.056(2) 0.0255(17) 0.0023(16) 0.0108(15) 0.0238(18) O3 0.073(3) 0.057(2) 0.044(2) 0.0276(19) 0.040(2) 0.039(2) C10 0.041(3) 0.053(3) 0.037(3) 0.002(2) 0.013(2) 0.005(3) F1 0.068(3) 0.074(3) 0.073(3) 0.012(2) 0.017(2) -0.030(2) F2 0.068(2) 0.110(3) 0.0249(17) -0.0026(18) 0.0086(16) 0.008(2) F3 0.084(3) 0.073(3) 0.072(3) -0.026(2) 0.018(2) 0.036(2) Pd1 0.01790(16) 0.01776(16) 0.01464(15) 0.00304(11) 0.00688(12) 0.00469(12) Cl1 0.0248(5) 0.0307(5) 0.0170(5) 0.0043(4) 0.0055(4) 0.0053(4) C1 0.024(2) 0.0138(18) 0.0193(19) 0.0025(15) 0.0112(16) 0.0023(15) N1 0.0238(17) 0.0197(17) 0.0195(17) 0.0044(14) 0.0114(14) 0.0021(14) Pd2 0.02418(17) 0.01675(16) 0.01648(16) 0.00429(12) 0.00927(13) 0.00442(12) Cl2 0.0500(7) 0.0204(5) 0.0282(5) 0.0054(4) 0.0205(5) 0.0117(5) N2 0.0235(17) 0.0177(16) 0.0157(16) 0.0020(13) 0.0083(14) 0.0046(14) C2 0.030(2) 0.024(2) 0.030(2) 0.0038(18) 0.0202(19) 0.0039(18) N3 0.0231(18) 0.0284(19) 0.0161(16) 0.0039(14) 0.0061(14) 0.0058(15) C3 0.027(2) 0.024(2) 0.038(2) 0.0076(19) 0.020(2) 0.0082(18) N4 0.0232(17) 0.0185(17) 0.0198(17) 0.0031(14) 0.0098(14) 0.0018(14) C4 0.024(2) 0.024(2) 0.030(2) 0.0074(18) 0.0114(18) 0.0063(17) N5 0.0267(18) 0.0235(18) 0.0173(16) 0.0029(14) 0.0109(14) -0.0001(14) C5 0.023(2) 0.0171(19) 0.0210(19) 0.0043(16) 0.0107(16) 0.0030(16) N6 0.034(2) 0.0225(18) 0.0253(19) 0.0049(16) 0.0157(16) 0.0090(16) C6 0.027(2) 0.020(2) 0.0156(19) 0.0030(16) 0.0068(16) 0.0031(17) O7 0.049(2) 0.053(2) 0.0239(17) -0.0011(15) 0.0231(16) 0.0069(17) C7 0.026(2) 0.026(2) 0.019(2) 0.0056(17) 0.0095(17) 0.0066(18) O8 0.0346(18) 0.058(2) 0.0246(16) 0.0052(15) 0.0183(14) 0.0177(16) C8 0.037(3) 0.042(3) 0.045(3) 0.013(2) 0.028(2) 0.017(2) C9 0.030(2) 0.050(3) 0.021(2) 0.014(2) 0.0131(19) 0.011(2) C11 0.025(2) 0.023(2) 0.0147(18) -0.0001(16) 0.0094(16) 0.0041(17) C12 0.029(2) 0.023(2) 0.017(2) 0.0007(16) 0.0077(17) 0.0053(17) C13 0.033(2) 0.029(2) 0.024(2) -0.0040(18) 0.0117(19) 0.0075(19) C14 0.032(2) 0.038(3) 0.019(2) -0.0037(19) 0.0143(19) -0.001(2) C15 0.037(2) 0.038(3) 0.019(2) 0.0087(19) 0.0140(19) 0.004(2) C16 0.030(2) 0.025(2) 0.023(2) 0.0049(17) 0.0116(18) 0.0067(18) C17 0.056(3) 0.065(4) 0.029(3) 0.002(3) 0.027(3) -0.007(3) C21 0.023(2) 0.018(2) 0.0155(18) -0.0013(15) 0.0056(16) -0.0026(16) C22 0.037(2) 0.032(2) 0.020(2) 0.0039(18) 0.0134(19) -0.002(2) C23 0.042(3) 0.034(3) 0.018(2) 0.0100(19) 0.0104(19) 0.000(2) C24 0.033(2) 0.022(2) 0.024(2) 0.0064(17) 0.0077(19) 0.0030(18) C25 0.026(2) 0.022(2) 0.019(2) 0.0055(16) 0.0072(17) 0.0001(17) C26 0.027(2) 0.017(2) 0.027(2) 0.0046(17) 0.0116(18) 0.0050(17) C27 0.033(2) 0.022(2) 0.025(2) 0.0049(18) 0.0149(19) 0.0086(18) C28 0.052(3) 0.036(3) 0.032(3) 0.018(2) 0.021(2) 0.014(2) C29 0.033(2) 0.034(3) 0.032(2) 0.005(2) 0.021(2) 0.009(2) C31 0.028(2) 0.0171(19) 0.020(2) 0.0008(16) 0.0126(17) 0.0032(16) C32 0.023(2) 0.019(2) 0.024(2) 0.0037(16) 0.0116(17) 0.0059(16) C33 0.028(2) 0.021(2) 0.021(2) 0.0041(16) 0.0104(17) 0.0050(17) C34 0.032(2) 0.024(2) 0.024(2) -0.0009(17) 0.0159(19) 0.0057(18) C35 0.025(2) 0.041(3) 0.027(2) 0.002(2) 0.0103(19) 0.013(2) C36 0.026(2) 0.027(2) 0.020(2) -0.0001(17) 0.0078(17) 0.0071(18) C37 0.039(3) 0.051(3) 0.025(2) 0.005(2) 0.017(2) 0.008(2) N7 0.047(3) 0.030(2) 0.034(2) 0.0101(18) 0.0031(19) 0.0094(19) C41 0.026(2) 0.037(3) 0.018(2) 0.0092(19) 0.0044(18) 0.0099(19) C42 0.037(3) 0.030(2) 0.030(2) 0.009(2) 0.007(2) 0.007(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 S1 O2 1.394(4) . ? S1 O1 1.420(4) . ? S1 O3 1.443(4) . ? S1 C10 1.784(6) . ? C10 F2 1.289(7) . ? C10 F1 1.307(7) . ? C10 F3 1.328(7) . ? S2 O4 1.4298 . ? S2 O6 1.4302 . ? S2 O5 1.4303 . ? S2 C20 1.8001 . ? C20 F4 1.3032 . ? C20 F6 1.3034 . ? C20 F5 1.3037 . ? S2' O5' 1.4299 . ? S2' O4' 1.4301 . ? S2' O6' 1.4302 . ? S2' C20' 1.8002 . ? C20' F4' 1.3033 . ? C20' F5' 1.3033 . ? C20' F6' 1.3036 . ? Pd1 N2 1.975(3) . ? Pd1 C1 1.991(4) . ? Pd1 N3 2.066(4) . ? Pd1 Cl1 2.2289(14) . ? C1 N1 1.322(5) . ? C1 C5 1.385(6) . ? N1 C2 1.362(6) . ? N1 C9 1.444(5) . ? Pd2 C21 1.932(4) . ? Pd2 N6 2.030(4) . ? Pd2 N4 2.042(3) . ? Pd2 Cl2 2.2652(12) . ? N2 C6 1.281(5) . ? N2 C11 1.398(5) . ? C2 C3 1.328(6) . ? C2 H2 0.9500 . ? N3 C7 1.134(5) . ? C3 C4 1.351(6) . ? C3 H3 0.9500 . ? N4 C26 1.265(5) . ? N4 C31 1.399(5) . ? C4 C5 1.380(6) . ? C4 H4 0.9500 . ? N5 C21 1.327(5) . ? N5 C22 1.336(6) . ? N5 C29 1.484(6) . ? C5 C6 1.402(6) . ? N6 C27 1.106(5) . ? C6 H6 0.9500 . ? O7 C14 1.334(5) . ? O7 C17 1.391(7) . ? C7 C8 1.445(6) . ? O8 C34 1.332(5) . ? O8 C37 1.386(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C16 1.364(6) . ? C11 C12 1.389(6) . ? C12 C13 1.337(6) . ? C12 H12 0.9500 . ? C13 C14 1.359(7) . ? C13 H13 0.9500 . ? C14 C15 1.386(7) . ? C15 C16 1.353(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C25 1.418(6) . ? C22 C23 1.355(7) . ? C22 H22 0.9500 . ? C23 C24 1.363(7) . ? C23 H23 0.9500 . ? C24 C25 1.355(6) . ? C24 H24 0.9500 . ? C25 C26 1.408(6) . ? C26 H26 0.9500 . ? C27 C28 1.418(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.356(6) . ? C31 C36 1.393(6) . ? C32 C33 1.350(6) . ? C32 H32 0.9500 . ? C33 C34 1.391(6) . ? C33 H33 0.9500 . ? C34 C35 1.355(6) . ? C35 C36 1.341(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N7 C41 1.130(6) . ? C41 C42 1.461(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O2 S1 O1 115.4(3) . . ? O2 S1 O3 115.2(2) . . ? O1 S1 O3 113.6(3) . . ? O2 S1 C10 101.3(3) . . ? O1 S1 C10 105.9(3) . . ? O3 S1 C10 103.3(3) . . ? F2 C10 F1 106.7(5) . . ? F2 C10 F3 108.7(5) . . ? F1 C10 F3 108.1(6) . . ? F2 C10 S1 110.0(4) . . ? F1 C10 S1 112.8(4) . . ? F3 C10 S1 110.4(4) . . ? O4 S2 O6 114.8 . . ? O4 S2 O5 114.8 . . ? O6 S2 O5 114.8 . . ? O4 S2 C20 103.4 . . ? O6 S2 C20 103.3 . . ? O5 S2 C20 103.4 . . ? F4 C20 F6 105.2 . . ? F4 C20 F5 105.2 . . ? F6 C20 F5 105.1 . . ? F4 C20 S2 113.5 . . ? F6 C20 S2 113.5 . . ? F5 C20 S2 113.5 . . ? O5' S2' O4' 114.8 . . ? O5' S2' O6' 114.9 . . ? O4' S2' O6' 114.8 . . ? O5' S2' C20' 103.3 . . ? O4' S2' C20' 103.3 . . ? O6' S2' C20' 103.3 . . ? F4' C20' F5' 105.2 . . ? F4' C20' F6' 105.2 . . ? F5' C20' F6' 105.1 . . ? F4' C20' S2' 113.5 . . ? F5' C20' S2' 113.5 . . ? F6' C20' S2' 113.5 . . ? N2 Pd1 C1 79.60(15) . . ? N2 Pd1 N3 94.56(13) . . ? C1 Pd1 N3 173.73(14) . . ? N2 Pd1 Cl1 174.02(10) . . ? C1 Pd1 Cl1 101.71(12) . . ? N3 Pd1 Cl1 83.87(10) . . ? N1 C1 C5 113.2(4) . . ? N1 C1 Pd1 133.6(3) . . ? C5 C1 Pd1 113.1(3) . . ? C1 N1 C2 122.8(4) . . ? C1 N1 C9 120.6(4) . . ? C2 N1 C9 116.6(3) . . ? C21 Pd2 N6 176.53(16) . . ? C21 Pd2 N4 79.94(16) . . ? N6 Pd2 N4 96.61(14) . . ? C21 Pd2 Cl2 98.51(13) . . ? N6 Pd2 Cl2 84.93(11) . . ? N4 Pd2 Cl2 166.21(10) . . ? C6 N2 C11 120.2(3) . . ? C6 N2 Pd1 114.4(3) . . ? C11 N2 Pd1 124.6(3) . . ? C3 C2 N1 123.9(4) . . ? C3 C2 H2 118.0 . . ? N1 C2 H2 118.0 . . ? C7 N3 Pd1 176.1(4) . . ? C2 C3 C4 116.4(4) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C26 N4 C31 118.5(4) . . ? C26 N4 Pd2 114.2(3) . . ? C31 N4 Pd2 125.5(3) . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C21 N5 C22 119.9(4) . . ? C21 N5 C29 123.5(4) . . ? C22 N5 C29 116.5(4) . . ? C4 C5 C1 124.5(4) . . ? C4 C5 C6 123.1(4) . . ? C1 C5 C6 112.2(4) . . ? C27 N6 Pd2 168.7(4) . . ? N2 C6 C5 118.3(4) . . ? N2 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C14 O7 C17 116.6(4) . . ? N3 C7 C8 179.2(5) . . ? C34 O8 C37 115.8(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C11 C12 121.1(4) . . ? C16 C11 N2 119.1(4) . . ? C12 C11 N2 119.8(4) . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 118.8(4) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? O7 C14 C13 113.0(4) . . ? O7 C14 C15 125.5(4) . . ? C13 C14 C15 121.5(4) . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 118.5(4) . . ? C15 C16 H16 120.7 . . ? C11 C16 H16 120.7 . . ? O7 C17 H17A 109.5 . . ? O7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C21 C25 117.2(4) . . ? N5 C21 Pd2 130.7(3) . . ? C25 C21 Pd2 112.1(3) . . ? N5 C22 C23 123.0(4) . . ? N5 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C22 C23 C24 119.8(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 116.8(4) . . ? C25 C24 H24 121.6 . . ? C23 C24 H24 121.6 . . ? C24 C25 C26 121.9(4) . . ? C24 C25 C21 122.8(4) . . ? C26 C25 C21 115.0(4) . . ? N4 C26 C25 115.4(4) . . ? N4 C26 H26 122.3 . . ? C25 C26 H26 122.3 . . ? N6 C27 C28 179.1(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 121.1(4) . . ? C32 C31 N4 117.4(4) . . ? C36 C31 N4 121.6(4) . . ? C33 C32 C31 118.5(4) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? O8 C34 C35 113.1(4) . . ? O8 C34 C33 125.8(4) . . ? C35 C34 C33 121.1(4) . . ? C36 C35 C34 118.8(4) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C31 120.3(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? O8 C37 H37A 109.5 . . ? O8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N7 C41 C42 179.4(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? 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 O2 S1 C10 F2 -178.9(4) . . . . ? O1 S1 C10 F2 60.3(5) . . . . ? O3 S1 C10 F2 -59.3(4) . . . . ? O2 S1 C10 F1 -59.9(5) . . . . ? O1 S1 C10 F1 179.3(4) . . . . ? O3 S1 C10 F1 59.7(5) . . . . ? O2 S1 C10 F3 61.2(5) . . . . ? O1 S1 C10 F3 -59.6(5) . . . . ? O3 S1 C10 F3 -179.2(4) . . . . ? O4 S2 C20 F4 180.0 . . . . ? O6 S2 C20 F4 60.0 . . . . ? O5 S2 C20 F4 -60.0 . . . . ? O4 S2 C20 F6 -60.0 . . . . ? O6 S2 C20 F6 -180.0 . . . . ? O5 S2 C20 F6 60.0 . . . . ? O4 S2 C20 F5 60.0 . . . . ? O6 S2 C20 F5 -60.0 . . . . ? O5 S2 C20 F5 180.0 . . . . ? O5' S2' C20' F4' -60.0 . . . . ? O4' S2' C20' F4' 180.0 . . . . ? O6' S2' C20' F4' 60.0 . . . . ? O5' S2' C20' F5' 180.0 . . . . ? O4' S2' C20' F5' 60.0 . . . . ? O6' S2' C20' F5' -60.0 . . . . ? O5' S2' C20' F6' 60.0 . . . . ? O4' S2' C20' F6' -60.0 . . . . ? O6' S2' C20' F6' -180.0 . . . . ? N2 Pd1 C1 N1 -170.8(4) . . . . ? N3 Pd1 C1 N1 167.6(11) . . . . ? Cl1 Pd1 C1 N1 15.2(4) . . . . ? N2 Pd1 C1 C5 13.1(3) . . . . ? N3 Pd1 C1 C5 -8.5(15) . . . . ? Cl1 Pd1 C1 C5 -161.0(3) . . . . ? C5 C1 N1 C2 4.3(5) . . . . ? Pd1 C1 N1 C2 -171.8(3) . . . . ? C5 C1 N1 C9 -172.5(4) . . . . ? Pd1 C1 N1 C9 11.4(6) . . . . ? C1 Pd1 N2 C6 -13.1(3) . . . . ? N3 Pd1 N2 C6 164.6(3) . . . . ? Cl1 Pd1 N2 C6 90.1(10) . . . . ? C1 Pd1 N2 C11 176.8(3) . . . . ? N3 Pd1 N2 C11 -5.5(3) . . . . ? Cl1 Pd1 N2 C11 -80.0(11) . . . . ? C1 N1 C2 C3 -1.1(6) . . . . ? C9 N1 C2 C3 175.8(4) . . . . ? N2 Pd1 N3 C7 115(5) . . . . ? C1 Pd1 N3 C7 136(5) . . . . ? Cl1 Pd1 N3 C7 -71(5) . . . . ? N1 C2 C3 C4 -2.4(7) . . . . ? C21 Pd2 N4 C26 -16.4(3) . . . . ? N6 Pd2 N4 C26 164.0(3) . . . . ? Cl2 Pd2 N4 C26 68.3(5) . . . . ? C21 Pd2 N4 C31 179.2(3) . . . . ? N6 Pd2 N4 C31 -0.4(3) . . . . ? Cl2 Pd2 N4 C31 -96.1(5) . . . . ? C2 C3 C4 C5 2.2(6) . . . . ? C3 C4 C5 C1 1.3(6) . . . . ? C3 C4 C5 C6 -174.6(4) . . . . ? N1 C1 C5 C4 -4.5(6) . . . . ? Pd1 C1 C5 C4 172.5(3) . . . . ? N1 C1 C5 C6 171.8(3) . . . . ? Pd1 C1 C5 C6 -11.2(4) . . . . ? C21 Pd2 N6 C27 128(3) . . . . ? N4 Pd2 N6 C27 134.0(18) . . . . ? Cl2 Pd2 N6 C27 -59.8(18) . . . . ? C11 N2 C6 C5 -178.5(4) . . . . ? Pd1 N2 C6 C5 10.9(5) . . . . ? C4 C5 C6 N2 176.7(4) . . . . ? C1 C5 C6 N2 0.3(5) . . . . ? Pd1 N3 C7 C8 -6(40) . . . . ? C6 N2 C11 C16 -41.9(6) . . . . ? Pd1 N2 C11 C16 127.6(4) . . . . ? C6 N2 C11 C12 137.7(4) . . . . ? Pd1 N2 C11 C12 -52.7(5) . . . . ? C16 C11 C12 C13 1.2(6) . . . . ? N2 C11 C12 C13 -178.4(4) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C17 O7 C14 C13 175.9(4) . . . . ? C17 O7 C14 C15 -4.8(7) . . . . ? C12 C13 C14 O7 178.5(4) . . . . ? C12 C13 C14 C15 -0.9(7) . . . . ? O7 C14 C15 C16 -178.7(4) . . . . ? C13 C14 C15 C16 0.6(7) . . . . ? C14 C15 C16 C11 0.5(7) . . . . ? C12 C11 C16 C15 -1.4(6) . . . . ? N2 C11 C16 C15 178.2(4) . . . . ? C22 N5 C21 C25 6.7(6) . . . . ? C29 N5 C21 C25 -169.7(4) . . . . ? C22 N5 C21 Pd2 -171.4(3) . . . . ? C29 N5 C21 Pd2 12.2(6) . . . . ? N6 Pd2 C21 N5 -161(2) . . . . ? N4 Pd2 C21 N5 -167.0(4) . . . . ? Cl2 Pd2 C21 N5 26.9(4) . . . . ? N6 Pd2 C21 C25 21(3) . . . . ? N4 Pd2 C21 C25 14.9(3) . . . . ? Cl2 Pd2 C21 C25 -151.3(3) . . . . ? C21 N5 C22 C23 -2.7(6) . . . . ? C29 N5 C22 C23 173.9(4) . . . . ? N5 C22 C23 C24 -2.4(7) . . . . ? C22 C23 C24 C25 2.8(7) . . . . ? C23 C24 C25 C26 -173.2(4) . . . . ? C23 C24 C25 C21 1.5(6) . . . . ? N5 C21 C25 C24 -6.3(6) . . . . ? Pd2 C21 C25 C24 172.2(3) . . . . ? N5 C21 C25 C26 168.7(4) . . . . ? Pd2 C21 C25 C26 -12.8(4) . . . . ? C31 N4 C26 C25 179.2(3) . . . . ? Pd2 N4 C26 C25 13.6(5) . . . . ? C24 C25 C26 N4 174.2(4) . . . . ? C21 C25 C26 N4 -0.8(5) . . . . ? Pd2 N6 C27 C28 -67(36) . . . . ? C26 N4 C31 C32 144.0(4) . . . . ? Pd2 N4 C31 C32 -52.2(5) . . . . ? C26 N4 C31 C36 -37.6(6) . . . . ? Pd2 N4 C31 C36 126.3(4) . . . . ? C36 C31 C32 C33 -0.2(6) . . . . ? N4 C31 C32 C33 178.2(4) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C37 O8 C34 C35 -175.6(4) . . . . ? C37 O8 C34 C33 4.9(7) . . . . ? C32 C33 C34 O8 -179.3(4) . . . . ? C32 C33 C34 C35 1.3(7) . . . . ? O8 C34 C35 C36 179.7(4) . . . . ? C33 C34 C35 C36 -0.8(7) . . . . ? C34 C35 C36 C31 -0.2(7) . . . . ? C32 C31 C36 C35 0.7(7) . . . . ? N4 C31 C36 C35 -177.7(4) . . . . ? _diffrn_measured_fraction_theta_max .994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full .994 _refine_diff_density_max 1.756 _refine_diff_density_min -1.976 _refine_diff_density_rms .104