# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Robertus J M Klein Gebbink' 'Alexsandro Berger' 'Harmen Dijkstra' 'Cornelis A. Kruithof' 'Martin Lutz' 'Fouad Soulimani' 'A Spek' 'G van Koten' 'Tom Visser' _publ_contact_author_name 'Robertus J M Klein Gebbink' _publ_contact_author_email R.J.M.KLEINGEBBINK@UU.NL _publ_section_title ; Sulfato-Bridged ECE-Pincer Palladium(II) Complexes: Structures in the Solid State and in Solution, and Catalytic Properties ; # Attachment 'deposit.cif' data_s3028a _database_code_depnum_ccdc_archive 'CCDC 704292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H50 O4 Pd2 S5, 2(H2 O)' _chemical_formula_sum 'C32 H54 O6 Pd2 S5' _chemical_formula_weight 907.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.5104(6) _cell_length_b 14.0482(6) _cell_length_c 17.2217(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.700(5) _cell_angle_gamma 90.00 _cell_volume 3674.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 273 _cell_measurement_theta_min 4.36 _cell_measurement_theta_max 22.38 _exptl_crystal_description plate _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35292 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4226 _reflns_number_gt 3797 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Dirax _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+5.1256P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4226 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.571161(8) 0.656627(8) 0.328571(7) 0.01470(4) Uani 1 1 d . . . S1 S 0.70578(3) 0.62123(3) 0.29694(2) 0.01704(8) Uani 1 1 d . . . S2 S 0.44422(3) 0.71404(3) 0.36207(2) 0.01769(9) Uani 1 1 d . . . S3 S 0.5000 0.45186(4) 0.2500 0.01801(12) Uani 1 2 d S . . O1 O 0.52466(8) 0.51354(8) 0.32174(7) 0.0239(3) Uani 1 1 d . . . O2 O 0.42515(9) 0.39357(9) 0.25954(8) 0.0305(3) Uani 1 1 d . . . C1 C 0.61116(10) 0.79008(11) 0.33475(9) 0.0155(3) Uani 1 1 d . . . C2 C 0.69183(11) 0.81530(12) 0.31550(10) 0.0172(3) Uani 1 1 d . . . C3 C 0.71876(11) 0.91004(12) 0.31721(10) 0.0211(3) Uani 1 1 d . . . H3 H 0.7744 0.9259 0.3057 0.025 Uiso 1 1 calc R . . C4 C 0.66427(12) 0.98109(12) 0.33572(11) 0.0232(4) Uani 1 1 d . . . H4 H 0.6823 1.0458 0.3365 0.028 Uiso 1 1 calc R . . C5 C 0.58368(11) 0.95784(12) 0.35303(10) 0.0208(3) Uani 1 1 d . . . H5 H 0.5461 1.0069 0.3646 0.025 Uiso 1 1 calc R . . C6 C 0.55705(11) 0.86318(11) 0.35368(10) 0.0166(3) Uani 1 1 d . . . C7 C 0.74831(11) 0.74060(12) 0.28847(11) 0.0216(4) Uani 1 1 d . . . H7A H 0.8087 0.7449 0.3208 0.026 Uiso 1 1 calc R . . H7B H 0.7515 0.7528 0.2325 0.026 Uiso 1 1 calc R . . C8 C 0.46964(12) 0.84009(12) 0.37301(12) 0.0237(4) Uani 1 1 d . . . H8A H 0.4232 0.8768 0.3375 0.028 Uiso 1 1 calc R . . H8B H 0.4697 0.8597 0.4283 0.028 Uiso 1 1 calc R . . C9 C 0.77661(11) 0.57496(12) 0.38915(10) 0.0218(4) Uani 1 1 d . . . C10 C 0.87160(11) 0.57210(13) 0.37745(12) 0.0266(4) Uani 1 1 d . . . H10A H 0.9090 0.5418 0.4235 0.040 Uiso 1 1 calc R . . H10B H 0.8923 0.6371 0.3718 0.040 Uiso 1 1 calc R . . H10C H 0.8744 0.5355 0.3296 0.040 Uiso 1 1 calc R . . C11 C 0.76882(13) 0.63696(15) 0.45978(11) 0.0307(4) Uani 1 1 d . . . H11A H 0.7080 0.6356 0.4676 0.046 Uiso 1 1 calc R . . H11B H 0.7852 0.7025 0.4498 0.046 Uiso 1 1 calc R . . H11C H 0.8083 0.6127 0.5074 0.046 Uiso 1 1 calc R . . C12 C 0.74306(13) 0.47463(14) 0.39775(12) 0.0306(4) Uani 1 1 d . . . H12A H 0.7524 0.4356 0.3530 0.046 Uiso 1 1 calc R . . H12B H 0.6801 0.4769 0.3984 0.046 Uiso 1 1 calc R . . H12C H 0.7751 0.4467 0.4474 0.046 Uiso 1 1 calc R . . C13 C 0.43443(12) 0.67380(13) 0.46254(11) 0.0240(4) Uani 1 1 d . . . C14 C 0.36130(15) 0.73144(16) 0.48735(14) 0.0401(5) Uani 1 1 d . . . H14A H 0.3073 0.7259 0.4466 0.060 Uiso 1 1 calc R . . H14B H 0.3789 0.7984 0.4935 0.060 Uiso 1 1 calc R . . H14C H 0.3506 0.7071 0.5379 0.060 Uiso 1 1 calc R . . C15 C 0.52113(14) 0.68370(17) 0.52124(12) 0.0360(5) Uani 1 1 d . . . H15A H 0.5400 0.7504 0.5237 0.054 Uiso 1 1 calc R . . H15B H 0.5658 0.6440 0.5042 0.054 Uiso 1 1 calc R . . H15C H 0.5136 0.6631 0.5738 0.054 Uiso 1 1 calc R . . C16 C 0.40614(15) 0.57007(14) 0.45005(14) 0.0356(5) Uani 1 1 d . . . H16A H 0.4044 0.5408 0.5014 0.053 Uiso 1 1 calc R . . H16B H 0.4483 0.5358 0.4250 0.053 Uiso 1 1 calc R . . H16C H 0.3475 0.5669 0.4157 0.053 Uiso 1 1 calc R . . O3 O 0.41158(17) 0.21260(15) 0.19375(15) 0.0833(7) Uani 1 1 d . . . H1O H 0.4083 0.2781 0.2100 0.050 Uiso 1 1 d . . . H2O H 0.4743 0.2004 0.2119 0.050 Uiso 0.50 1 d P . . H3O H 0.4558 0.2036 0.1604 0.050 Uiso 0.50 1 d P . . 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 0.01394(7) 0.01175(6) 0.01902(7) -0.00087(4) 0.00479(5) 0.00120(4) S1 0.01555(19) 0.01636(18) 0.01975(19) -0.00203(15) 0.00489(15) 0.00301(15) S2 0.01470(19) 0.01597(19) 0.0232(2) 0.00010(15) 0.00583(16) 0.00156(14) S3 0.0174(3) 0.0108(2) 0.0275(3) 0.000 0.0085(2) 0.000 O1 0.0314(7) 0.0140(6) 0.0277(7) -0.0007(5) 0.0091(5) -0.0026(5) O2 0.0277(7) 0.0242(7) 0.0419(8) 0.0006(6) 0.0126(6) -0.0099(5) C1 0.0159(8) 0.0145(7) 0.0153(7) 0.0005(6) 0.0011(6) 0.0018(6) C2 0.0160(8) 0.0172(8) 0.0179(8) 0.0013(6) 0.0022(6) 0.0011(6) C3 0.0174(8) 0.0206(8) 0.0251(9) 0.0022(7) 0.0042(7) -0.0028(6) C4 0.0251(9) 0.0144(8) 0.0296(9) 0.0012(7) 0.0046(7) -0.0022(7) C5 0.0217(8) 0.0149(8) 0.0256(9) 0.0002(6) 0.0041(7) 0.0043(6) C6 0.0170(8) 0.0157(8) 0.0167(8) 0.0005(6) 0.0022(6) 0.0019(6) C7 0.0175(8) 0.0182(8) 0.0303(9) 0.0002(7) 0.0078(7) -0.0006(6) C8 0.0236(9) 0.0131(8) 0.0371(10) -0.0006(7) 0.0127(8) 0.0030(6) C9 0.0181(8) 0.0240(9) 0.0225(9) 0.0007(7) 0.0028(7) 0.0070(7) C10 0.0180(8) 0.0262(9) 0.0351(10) -0.0037(8) 0.0039(8) 0.0081(7) C11 0.0275(10) 0.0418(11) 0.0217(9) -0.0066(8) 0.0023(8) 0.0122(8) C12 0.0279(10) 0.0279(10) 0.0351(11) 0.0098(8) 0.0047(8) 0.0056(8) C13 0.0254(9) 0.0232(9) 0.0276(9) 0.0045(7) 0.0158(8) 0.0040(7) C14 0.0433(12) 0.0371(11) 0.0495(13) 0.0080(10) 0.0325(11) 0.0127(10) C15 0.0401(12) 0.0447(12) 0.0231(10) 0.0024(9) 0.0063(9) 0.0027(10) C16 0.0389(11) 0.0255(10) 0.0486(13) 0.0078(9) 0.0236(10) -0.0019(8) O3 0.1091(19) 0.0540(13) 0.1018(17) -0.0322(12) 0.0570(15) -0.0380(12) _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 1.9708(16) . ? Pd1 O1 2.1308(12) . ? Pd1 S2 2.3067(4) . ? Pd1 S1 2.3163(4) . ? Pd1 Pd1 3.1263(3) 2_655 ? S1 C7 1.8186(17) . ? S1 C9 1.8557(17) . ? S2 C8 1.8156(17) . ? S2 C13 1.8555(18) . ? S3 O2 1.4569(13) 2_655 ? S3 O2 1.4570(13) . ? S3 O1 1.4940(13) . ? S3 O1 1.4940(13) 2_655 ? C1 C2 1.403(2) . ? C1 C6 1.406(2) . ? C2 C3 1.393(2) . ? C2 C7 1.500(2) . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 C6 1.393(2) . ? C5 H5 0.9500 . ? C6 C8 1.496(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C12 1.520(3) . ? C9 C11 1.521(2) . ? C9 C10 1.527(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.516(3) . ? C13 C14 1.524(3) . ? C13 C16 1.524(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O3 H1O 0.9659 . ? O3 H2O 0.9751 . ? O3 H3O 0.9880 . ? 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 O1 178.58(6) . . ? C1 Pd1 S2 85.94(5) . . ? O1 Pd1 S2 92.70(4) . . ? C1 Pd1 S1 85.87(5) . . ? O1 Pd1 S1 95.49(4) . . ? S2 Pd1 S1 171.801(15) . . ? C1 Pd1 Pd1 101.89(4) . 2_655 ? O1 Pd1 Pd1 77.32(3) . 2_655 ? S2 Pd1 Pd1 74.205(12) . 2_655 ? S1 Pd1 Pd1 107.959(12) . 2_655 ? C7 S1 C9 103.31(8) . . ? C7 S1 Pd1 100.36(6) . . ? C9 S1 Pd1 106.22(6) . . ? C8 S2 C13 104.92(9) . . ? C8 S2 Pd1 100.87(6) . . ? C13 S2 Pd1 111.23(6) . . ? O2 S3 O2 111.61(11) 2_655 . ? O2 S3 O1 110.06(7) 2_655 . ? O2 S3 O1 107.99(7) . . ? O2 S3 O1 107.99(7) 2_655 2_655 ? O2 S3 O1 110.06(7) . 2_655 ? O1 S3 O1 109.10(10) . 2_655 ? S3 O1 Pd1 128.30(7) . . ? C2 C1 C6 118.24(15) . . ? C2 C1 Pd1 120.90(12) . . ? C6 C1 Pd1 120.74(12) . . ? C3 C2 C1 120.93(15) . . ? C3 C2 C7 118.90(15) . . ? C1 C2 C7 120.09(15) . . ? C4 C3 C2 119.90(16) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.99(16) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.66(16) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.23(16) . . ? C5 C6 C8 119.50(15) . . ? C1 C6 C8 120.26(15) . . ? C2 C7 S1 112.09(12) . . ? C2 C7 H7A 109.2 . . ? S1 C7 H7A 109.2 . . ? C2 C7 H7B 109.2 . . ? S1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C6 C8 S2 112.09(12) . . ? C6 C8 H8A 109.2 . . ? S2 C8 H8A 109.2 . . ? C6 C8 H8B 109.2 . . ? S2 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C12 C9 C11 111.64(16) . . ? C12 C9 C10 110.30(15) . . ? C11 C9 C10 110.84(15) . . ? C12 C9 S1 104.67(12) . . ? C11 C9 S1 110.77(12) . . ? C10 C9 S1 108.41(12) . . ? 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 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 111.99(17) . . ? C15 C13 C16 111.89(17) . . ? C14 C13 C16 109.77(17) . . ? C15 C13 S2 111.39(13) . . ? C14 C13 S2 107.82(13) . . ? C16 C13 S2 103.61(13) . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? H1O O3 H2O 100.5 . . ? H1O O3 H3O 111.9 . . ? H2O O3 H3O 53.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 S1 C7 -6.32(7) . . . . ? O1 Pd1 S1 C7 173.27(7) . . . . ? Pd1 Pd1 S1 C7 94.85(6) 2_655 . . . ? C1 Pd1 S1 C9 100.95(7) . . . . ? O1 Pd1 S1 C9 -79.45(7) . . . . ? Pd1 Pd1 S1 C9 -157.88(6) 2_655 . . . ? C1 Pd1 S2 C8 -1.24(8) . . . . ? O1 Pd1 S2 C8 179.17(7) . . . . ? Pd1 Pd1 S2 C8 -104.81(7) 2_655 . . . ? C1 Pd1 S2 C13 -112.08(8) . . . . ? O1 Pd1 S2 C13 68.33(7) . . . . ? Pd1 Pd1 S2 C13 144.35(7) 2_655 . . . ? O2 S3 O1 Pd1 94.30(10) 2_655 . . . ? O2 S3 O1 Pd1 -143.64(9) . . . . ? O1 S3 O1 Pd1 -24.03(5) 2_655 . . . ? S2 Pd1 O1 S3 111.88(9) . . . . ? S1 Pd1 O1 S3 -68.48(9) . . . . ? Pd1 Pd1 O1 S3 38.73(8) 2_655 . . . ? S2 Pd1 C1 C2 -176.45(13) . . . . ? S1 Pd1 C1 C2 3.96(12) . . . . ? Pd1 Pd1 C1 C2 -103.54(12) 2_655 . . . ? S2 Pd1 C1 C6 -0.53(13) . . . . ? S1 Pd1 C1 C6 179.88(13) . . . . ? Pd1 Pd1 C1 C6 72.38(13) 2_655 . . . ? C6 C1 C2 C3 1.7(2) . . . . ? Pd1 C1 C2 C3 177.77(12) . . . . ? C6 C1 C2 C7 -174.99(15) . . . . ? Pd1 C1 C2 C7 1.0(2) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? C7 C2 C3 C4 174.74(16) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C3 C4 C5 C6 1.3(3) . . . . ? C4 C5 C6 C1 -1.6(3) . . . . ? C4 C5 C6 C8 179.71(16) . . . . ? C2 C1 C6 C5 0.0(2) . . . . ? Pd1 C1 C6 C5 -175.99(13) . . . . ? C2 C1 C6 C8 178.77(15) . . . . ? Pd1 C1 C6 C8 2.7(2) . . . . ? C3 C2 C7 S1 176.09(13) . . . . ? C1 C2 C7 S1 -7.1(2) . . . . ? C9 S1 C7 C2 -101.16(13) . . . . ? Pd1 S1 C7 C2 8.42(13) . . . . ? C5 C6 C8 S2 175.01(13) . . . . ? C1 C6 C8 S2 -3.7(2) . . . . ? C13 S2 C8 C6 118.42(14) . . . . ? Pd1 S2 C8 C6 2.78(14) . . . . ? C7 S1 C9 C12 -179.66(12) . . . . ? Pd1 S1 C9 C12 75.19(12) . . . . ? C7 S1 C9 C11 59.87(15) . . . . ? Pd1 S1 C9 C11 -45.27(14) . . . . ? C7 S1 C9 C10 -61.95(13) . . . . ? Pd1 S1 C9 C10 -167.09(10) . . . . ? C8 S2 C13 C15 -63.81(15) . . . . ? Pd1 S2 C13 C15 44.42(15) . . . . ? C8 S2 C13 C14 59.44(16) . . . . ? Pd1 S2 C13 C14 167.67(13) . . . . ? C8 S2 C13 C16 175.75(13) . . . . ? Pd1 S2 C13 C16 -76.02(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.417 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.062 #===END data_s3461a _database_code_depnum_ccdc_archive 'CCDC 704293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 N4 O4 Pd2 S, 6(H2 O)' _chemical_formula_sum 'C24 H50 N4 O10 Pd2 S' _chemical_formula_weight 799.54 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.9056(3) _cell_length_b 24.7652(5) _cell_length_c 15.04568(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.169(1) _cell_angle_gamma 90.00 _cell_volume 3317.61(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22704 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36548 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.71 _reflns_number_total 12407 _reflns_number_gt 12212 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Mergehklf5' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+12.0199P] 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 -0.03(3) _refine_ls_number_reflns 12407 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.008 _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 0.47203(3) 0.391044(11) 0.391361(19) 0.01483(7) Uani 1 1 d . . . Pd2 Pd 0.50054(3) 0.143235(11) 0.499928(19) 0.01527(7) Uani 1 1 d . . . S1 S 0.42713(13) 0.26483(5) 0.43948(6) 0.01754(19) Uani 1 1 d . . . O1 O 0.5228(4) 0.31347(13) 0.4528(2) 0.0224(7) Uani 1 1 d . . . O2 O 0.5300(4) 0.21819(13) 0.4269(2) 0.0210(6) Uani 1 1 d . . . O3 O 0.3299(4) 0.27229(16) 0.3602(2) 0.0281(7) Uani 1 1 d . . . O4 O 0.3393(4) 0.25536(15) 0.5197(2) 0.0249(7) Uani 1 1 d . . . N11 N 0.6446(5) 0.38638(16) 0.2989(2) 0.0189(7) Uani 1 1 d . . . N12 N 0.2892(4) 0.41710(16) 0.4666(2) 0.0176(7) Uani 1 1 d . . . N21 N 0.6821(4) 0.15522(17) 0.5899(2) 0.0167(7) Uani 1 1 d . . . N22 N 0.3169(5) 0.11029(15) 0.4289(2) 0.0191(7) Uani 1 1 d . . . C11 C 0.4501(5) 0.4620(2) 0.3425(3) 0.0193(8) Uani 1 1 d . . . C12 C 0.5296(5) 0.47496(19) 0.2666(3) 0.0184(8) Uani 1 1 d . . . C13 C 0.5146(6) 0.5273(2) 0.2318(3) 0.0255(10) Uani 1 1 d . . . H13 H 0.5702 0.5378 0.1814 0.031 Uiso 1 1 calc R . . C14 C 0.4182(6) 0.56382(19) 0.2715(3) 0.0237(9) Uani 1 1 d . . . H14 H 0.4063 0.5989 0.2467 0.028 Uiso 1 1 calc R . . C15 C 0.3382(6) 0.5500(2) 0.3472(3) 0.0235(9) Uani 1 1 d . . . H15 H 0.2717 0.5752 0.3730 0.028 Uiso 1 1 calc R . . C16 C 0.3565(5) 0.49900(19) 0.3846(3) 0.0188(8) Uani 1 1 d . . . C17 C 0.6170(6) 0.4293(2) 0.2283(3) 0.0239(9) Uani 1 1 d . . . H17A H 0.7143 0.4429 0.2066 0.029 Uiso 1 1 calc R . . H17B H 0.5605 0.4135 0.1772 0.029 Uiso 1 1 calc R . . C18 C 0.6600(6) 0.3317(2) 0.2568(3) 0.0285(10) Uani 1 1 d . . . H18A H 0.5671 0.3227 0.2241 0.043 Uiso 1 1 calc R . . H18B H 0.6791 0.3046 0.3031 0.043 Uiso 1 1 calc R . . H18C H 0.7440 0.3322 0.2157 0.043 Uiso 1 1 calc R . . C19 C 0.7871(6) 0.3983(2) 0.3478(3) 0.0269(10) Uani 1 1 d . . . H19A H 0.8082 0.3695 0.3909 0.040 Uiso 1 1 calc R . . H19B H 0.7779 0.4328 0.3792 0.040 Uiso 1 1 calc R . . H19C H 0.8694 0.4005 0.3057 0.040 Uiso 1 1 calc R . . C110 C 0.2913(5) 0.47751(19) 0.4705(3) 0.0219(9) Uani 1 1 d . . . H11A H 0.3533 0.4897 0.5220 0.026 Uiso 1 1 calc R . . H11B H 0.1880 0.4914 0.4776 0.026 Uiso 1 1 calc R . . C111 C 0.1486(5) 0.4001(2) 0.4200(3) 0.0227(9) Uani 1 1 d . . . H11C H 0.1529 0.3613 0.4074 0.034 Uiso 1 1 calc R . . H11D H 0.1374 0.4201 0.3641 0.034 Uiso 1 1 calc R . . H11E H 0.0627 0.4077 0.4577 0.034 Uiso 1 1 calc R . . C112 C 0.2876(6) 0.3948(2) 0.5585(3) 0.0257(10) Uani 1 1 d . . . H11F H 0.1975 0.4074 0.5885 0.039 Uiso 1 1 calc R . . H11G H 0.3772 0.4071 0.5915 0.039 Uiso 1 1 calc R . . H11H H 0.2871 0.3553 0.5559 0.039 Uiso 1 1 calc R . . C21 C 0.4873(5) 0.07629(17) 0.5634(3) 0.0177(8) Uani 1 1 d . . . C22 C 0.5739(6) 0.0702(2) 0.6405(3) 0.0241(9) Uani 1 1 d . . . C23 C 0.5645(7) 0.0201(2) 0.6844(3) 0.0293(11) Uani 1 1 d . . . H23 H 0.6218 0.0140 0.7374 0.035 Uiso 1 1 calc R . . C24 C 0.4728(8) -0.0204(2) 0.6510(3) 0.0330(12) Uani 1 1 d . . . H24 H 0.4693 -0.0540 0.6814 0.040 Uiso 1 1 calc R . . C25 C 0.3842(6) -0.0133(2) 0.5733(3) 0.0267(10) Uani 1 1 d . . . H25 H 0.3187 -0.0411 0.5526 0.032 Uiso 1 1 calc R . . C26 C 0.3951(5) 0.0357(2) 0.5274(3) 0.0223(9) Uani 1 1 d . . . C27 C 0.6565(6) 0.1194(2) 0.6696(3) 0.0238(9) Uani 1 1 d . . . H27A H 0.7542 0.1092 0.6973 0.029 Uiso 1 1 calc R . . H27B H 0.5977 0.1392 0.7143 0.029 Uiso 1 1 calc R . . C28 C 0.7006(6) 0.2127(2) 0.6181(3) 0.0255(9) Uani 1 1 d . . . H28A H 0.7895 0.2160 0.6573 0.038 Uiso 1 1 calc R . . H28B H 0.6114 0.2243 0.6501 0.038 Uiso 1 1 calc R . . H28C H 0.7132 0.2355 0.5656 0.038 Uiso 1 1 calc R . . C29 C 0.8197(6) 0.1386(2) 0.5442(3) 0.0253(10) Uani 1 1 d . . . H29A H 0.8305 0.1600 0.4899 0.038 Uiso 1 1 calc R . . H29B H 0.8129 0.1002 0.5288 0.038 Uiso 1 1 calc R . . H29C H 0.9071 0.1445 0.5837 0.038 Uiso 1 1 calc R . . C210 C 0.3238(6) 0.0499(2) 0.4380(3) 0.0259(10) Uani 1 1 d . . . H21A H 0.3839 0.0344 0.3896 0.031 Uiso 1 1 calc R . . H21B H 0.2213 0.0346 0.4336 0.031 Uiso 1 1 calc R . . C211 C 0.1775(6) 0.1297(2) 0.4704(3) 0.0264(10) Uani 1 1 d . . . H21C H 0.1695 0.1689 0.4630 0.040 Uiso 1 1 calc R . . H21D H 0.1803 0.1209 0.5339 0.040 Uiso 1 1 calc R . . H21E H 0.0904 0.1122 0.4418 0.040 Uiso 1 1 calc R . . C212 C 0.3100(7) 0.1256(2) 0.3325(3) 0.0304(11) Uani 1 1 d . . . H21F H 0.2165 0.1119 0.3054 0.046 Uiso 1 1 calc R . . H21G H 0.3959 0.1098 0.3021 0.046 Uiso 1 1 calc R . . H21H H 0.3132 0.1650 0.3269 0.046 Uiso 1 1 calc R . . O31 O 0.6365(5) 0.35104(17) 0.6227(2) 0.0326(8) Uani 1 1 d . . . H31A H 0.5918 0.3377 0.5689 0.049 Uiso 1 1 d . . . H31B H 0.7433 0.3486 0.6208 0.049 Uiso 1 1 d . . . O32 O 0.6517(5) 0.17405(18) 0.2698(2) 0.0343(9) Uani 1 1 d . . . H32A H 0.6109 0.1919 0.3200 0.051 Uiso 1 1 d . . . H32B H 0.7397 0.1868 0.2419 0.051 Uiso 1 1 d . . . O33 O 0.0207(5) 0.2803(2) 0.3297(3) 0.0390(10) Uani 1 1 d . . . H33A H 0.1270 0.2801 0.3372 0.058 Uiso 1 1 d . . . H33B H -0.0308 0.2583 0.2869 0.058 Uiso 1 1 d . . . O34 O 0.0228(5) 0.26016(18) 0.5139(3) 0.0391(9) Uani 1 1 d . . . H34A H 0.1294 0.2586 0.5217 0.059 Uiso 1 1 d . . . H34B H 0.0184 0.2666 0.4515 0.059 Uiso 1 1 d . . . O35 O 0.4017(5) 0.28699(19) 0.6973(2) 0.0343(9) Uani 1 1 d . . . H35A H 0.3723 0.2711 0.6413 0.051 Uiso 1 1 d . . . H35B H 0.4834 0.3081 0.6767 0.051 Uiso 1 1 d . . . O36 O 0.9454(5) 0.34105(19) 0.6327(3) 0.0371(9) Uani 1 1 d . . . H36A H 0.9807 0.3154 0.5905 0.056 Uiso 1 1 d . . . H36B H 1.0116 0.3319 0.6810 0.056 Uiso 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 0.01421(14) 0.01142(14) 0.01889(13) 0.00043(10) 0.00110(9) 0.00043(11) Pd2 0.01508(14) 0.01161(13) 0.01914(13) 0.00030(10) 0.00101(9) 0.00009(11) S1 0.0176(5) 0.0137(5) 0.0214(4) 0.0004(3) 0.0010(3) 0.0005(4) O1 0.0237(18) 0.0147(16) 0.0284(15) 0.0033(11) -0.0046(12) 0.0006(13) O2 0.0241(17) 0.0106(14) 0.0285(15) 0.0038(11) 0.0057(12) 0.0002(13) O3 0.0215(17) 0.031(2) 0.0317(16) 0.0001(13) -0.0071(12) 0.0003(15) O4 0.0215(17) 0.0240(18) 0.0296(15) -0.0017(12) 0.0085(12) 0.0011(14) N11 0.0145(19) 0.020(2) 0.0225(17) -0.0020(13) 0.0006(12) -0.0003(15) N12 0.0147(17) 0.0184(19) 0.0197(15) -0.0016(12) 0.0024(12) 0.0005(14) N21 0.0075(16) 0.0197(19) 0.0228(16) -0.0038(13) -0.0036(11) 0.0025(14) N22 0.018(2) 0.0160(19) 0.0240(17) -0.0004(12) 0.0032(13) -0.0031(14) C11 0.014(2) 0.021(2) 0.0226(19) 0.0016(15) 0.0019(14) -0.0019(18) C12 0.017(2) 0.015(2) 0.0234(19) 0.0008(14) -0.0004(14) -0.0045(16) C13 0.031(3) 0.021(2) 0.024(2) 0.0068(17) -0.0009(17) -0.001(2) C14 0.030(3) 0.013(2) 0.028(2) 0.0031(16) -0.0079(17) -0.0031(19) C15 0.027(2) 0.021(2) 0.0230(19) -0.0035(16) -0.0050(16) 0.0024(19) C16 0.0137(19) 0.020(2) 0.0226(18) 0.0017(15) -0.0007(14) 0.0022(16) C17 0.025(2) 0.023(3) 0.0241(19) 0.0014(16) 0.0053(15) 0.002(2) C18 0.031(3) 0.023(3) 0.032(2) -0.0062(18) 0.0032(18) 0.004(2) C19 0.015(2) 0.034(3) 0.031(2) -0.0003(19) -0.0024(17) -0.001(2) C110 0.023(2) 0.020(2) 0.0228(19) -0.0018(15) 0.0025(15) 0.0015(18) C111 0.012(2) 0.028(3) 0.028(2) -0.0026(17) -0.0007(15) -0.0009(18) C112 0.031(3) 0.028(3) 0.0180(19) 0.0036(16) 0.0028(16) 0.002(2) C21 0.019(2) 0.0116(18) 0.0227(18) 0.0013(14) 0.0078(14) 0.0019(17) C22 0.023(2) 0.025(2) 0.0247(19) 0.0040(16) 0.0069(16) 0.0061(19) C23 0.040(3) 0.024(3) 0.024(2) 0.0053(17) 0.0037(18) 0.008(2) C24 0.054(4) 0.016(2) 0.030(2) 0.0054(17) 0.015(2) 0.003(2) C25 0.028(3) 0.016(2) 0.036(2) -0.0002(17) 0.0119(18) -0.003(2) C26 0.020(2) 0.017(2) 0.030(2) -0.0010(16) 0.0065(16) 0.0016(18) C27 0.024(2) 0.027(3) 0.0200(19) 0.0013(17) -0.0039(15) 0.002(2) C28 0.021(2) 0.024(2) 0.031(2) -0.0073(17) -0.0026(16) 0.0007(19) C29 0.017(2) 0.029(3) 0.030(2) -0.0008(17) 0.0004(17) 0.0073(19) C210 0.031(3) 0.018(2) 0.029(2) -0.0048(16) 0.0050(17) -0.003(2) C211 0.013(2) 0.033(3) 0.033(2) -0.0041(19) 0.0004(16) 0.001(2) C212 0.036(3) 0.033(3) 0.022(2) -0.0004(18) -0.0041(18) -0.009(2) O31 0.024(2) 0.040(2) 0.0339(18) -0.0091(15) -0.0042(14) 0.0035(17) O32 0.0230(19) 0.044(2) 0.0364(18) -0.0042(16) 0.0105(13) -0.0003(17) O33 0.026(2) 0.046(3) 0.044(2) -0.0168(18) -0.0042(15) -0.0057(19) O34 0.030(2) 0.041(2) 0.046(2) -0.0098(17) 0.0117(16) -0.0033(19) O35 0.028(2) 0.047(3) 0.0277(17) 0.0002(15) 0.0016(13) 0.0065(18) O36 0.032(2) 0.038(2) 0.041(2) -0.0119(16) 0.0004(15) -0.0013(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 C11 1.913(5) . ? Pd1 N11 2.097(4) . ? Pd1 N12 2.104(4) . ? Pd1 O1 2.176(3) . ? Pd2 C21 1.918(4) . ? Pd2 N22 2.100(4) . ? Pd2 N21 2.108(4) . ? Pd2 O2 2.176(3) . ? S1 O4 1.470(3) . ? S1 O3 1.471(3) . ? S1 O1 1.487(4) . ? S1 O2 1.489(3) . ? N11 C19 1.484(6) . ? N11 C18 1.502(6) . ? N11 C17 1.520(6) . ? N12 C111 1.484(6) . ? N12 C112 1.488(5) . ? N12 C110 1.497(6) . ? N21 C29 1.476(6) . ? N21 C28 1.494(6) . ? N21 C27 1.512(6) . ? N22 C211 1.482(6) . ? N22 C212 1.499(6) . ? N22 C210 1.503(6) . ? C11 C12 1.393(6) . ? C11 C16 1.399(6) . ? C12 C13 1.404(6) . ? C12 C17 1.495(7) . ? C13 C14 1.390(8) . ? C13 H13 0.9500 . ? C14 C15 1.398(7) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C110 1.524(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C21 C22 1.389(6) . ? C21 C26 1.400(7) . ? C22 C23 1.410(7) . ? C22 C27 1.485(7) . ? C23 C24 1.380(9) . ? C23 H23 0.9500 . ? C24 C25 1.408(9) . ? C24 H24 0.9500 . ? C25 C26 1.401(7) . ? C25 H25 0.9500 . ? C26 C210 1.517(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 H21C 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? C212 H21H 0.9800 . ? O31 H31A 0.9534 . ? O31 H31B 0.9541 . ? O32 H32A 0.9537 . ? O32 H32B 0.9508 . ? O33 H33A 0.9514 . ? O33 H33B 0.9531 . ? O34 H34A 0.9542 . ? O34 H34B 0.9522 . ? O35 H35A 0.9614 . ? O35 H35B 0.9533 . ? O36 H36A 0.9560 . ? O36 H36B 0.9535 . ? 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 C11 Pd1 N11 82.30(17) . . ? C11 Pd1 N12 81.44(17) . . ? N11 Pd1 N12 163.69(15) . . ? C11 Pd1 O1 173.25(17) . . ? N11 Pd1 O1 94.85(15) . . ? N12 Pd1 O1 101.45(14) . . ? C21 Pd2 N22 82.09(18) . . ? C21 Pd2 N21 81.74(18) . . ? N22 Pd2 N21 163.83(15) . . ? C21 Pd2 O2 176.51(17) . . ? N22 Pd2 O2 100.09(14) . . ? N21 Pd2 O2 96.03(14) . . ? O4 S1 O3 111.8(2) . . ? O4 S1 O1 109.4(2) . . ? O3 S1 O1 109.5(2) . . ? O4 S1 O2 108.6(2) . . ? O3 S1 O2 110.4(2) . . ? O1 S1 O2 107.05(19) . . ? S1 O1 Pd1 122.99(19) . . ? S1 O2 Pd2 121.13(18) . . ? C19 N11 C18 107.7(4) . . ? C19 N11 C17 109.4(4) . . ? C18 N11 C17 110.5(3) . . ? C19 N11 Pd1 106.9(3) . . ? C18 N11 Pd1 113.8(3) . . ? C17 N11 Pd1 108.4(3) . . ? C111 N12 C112 108.1(4) . . ? C111 N12 C110 108.1(4) . . ? C112 N12 C110 109.5(3) . . ? C111 N12 Pd1 108.3(3) . . ? C112 N12 Pd1 114.1(3) . . ? C110 N12 Pd1 108.6(3) . . ? C29 N21 C28 108.1(4) . . ? C29 N21 C27 110.2(4) . . ? C28 N21 C27 110.5(3) . . ? C29 N21 Pd2 107.2(3) . . ? C28 N21 Pd2 113.3(3) . . ? C27 N21 Pd2 107.5(3) . . ? C211 N22 C212 107.9(4) . . ? C211 N22 C210 108.5(4) . . ? C212 N22 C210 109.9(4) . . ? C211 N22 Pd2 108.0(3) . . ? C212 N22 Pd2 114.2(3) . . ? C210 N22 Pd2 108.1(3) . . ? C12 C11 C16 122.5(4) . . ? C12 C11 Pd1 118.5(3) . . ? C16 C11 Pd1 119.0(3) . . ? C11 C12 C13 118.2(4) . . ? C11 C12 C17 114.8(4) . . ? C13 C12 C17 126.9(4) . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.3(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 118.5(4) . . ? C15 C16 C110 128.1(4) . . ? C11 C16 C110 113.3(4) . . ? C12 C17 N11 109.7(3) . . ? C12 C17 H17A 109.7 . . ? N11 C17 H17A 109.7 . . ? C12 C17 H17B 109.7 . . ? N11 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N11 C18 H18A 109.5 . . ? N11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N11 C19 H19A 109.5 . . ? N11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N12 C110 C16 108.7(3) . . ? N12 C110 H11A 109.9 . . ? C16 C110 H11A 109.9 . . ? N12 C110 H11B 109.9 . . ? C16 C110 H11B 109.9 . . ? H11A C110 H11B 108.3 . . ? N12 C111 H11C 109.5 . . ? N12 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? N12 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? N12 C112 H11F 109.5 . . ? N12 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? N12 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C22 C21 C26 123.8(4) . . ? C22 C21 Pd2 118.1(4) . . ? C26 C21 Pd2 118.0(3) . . ? C21 C22 C23 116.7(5) . . ? C21 C22 C27 114.9(4) . . ? C23 C22 C27 128.3(4) . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 122.0(5) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 118.3(5) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? C25 C26 C21 118.5(5) . . ? C25 C26 C210 127.3(5) . . ? C21 C26 C210 114.0(4) . . ? C22 C27 N21 109.2(3) . . ? C22 C27 H27A 109.8 . . ? N21 C27 H27A 109.8 . . ? C22 C27 H27B 109.8 . . ? N21 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? N21 C28 H28A 109.5 . . ? N21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N21 C29 H29A 109.5 . . ? N21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N22 C210 C26 109.1(4) . . ? N22 C210 H21A 109.9 . . ? C26 C210 H21A 109.9 . . ? N22 C210 H21B 109.9 . . ? C26 C210 H21B 109.9 . . ? H21A C210 H21B 108.3 . . ? N22 C211 H21C 109.5 . . ? N22 C211 H21D 109.5 . . ? H21C C211 H21D 109.5 . . ? N22 C211 H21E 109.5 . . ? H21C C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? N22 C212 H21F 109.5 . . ? N22 C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? N22 C212 H21H 109.5 . . ? H21F C212 H21H 109.5 . . ? H21G C212 H21H 109.5 . . ? H31A O31 H31B 110.7 . . ? H32A O32 H32B 121.8 . . ? H33A O33 H33B 122.9 . . ? H34A O34 H34B 98.6 . . ? H35A O35 H35B 97.6 . . ? H36A O36 H36B 98.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O1 Pd1 -104.6(2) . . . . ? O3 S1 O1 Pd1 18.2(3) . . . . ? O2 S1 O1 Pd1 137.9(2) . . . . ? N11 Pd1 O1 S1 -107.1(2) . . . . ? N12 Pd1 O1 S1 73.4(2) . . . . ? O4 S1 O2 Pd2 13.9(3) . . . . ? O3 S1 O2 Pd2 -109.0(2) . . . . ? O1 S1 O2 Pd2 131.9(2) . . . . ? N22 Pd2 O2 S1 76.3(2) . . . . ? N21 Pd2 O2 S1 -105.0(2) . . . . ? C11 Pd1 N11 C19 97.7(3) . . . . ? N12 Pd1 N11 C19 102.1(6) . . . . ? O1 Pd1 N11 C19 -76.2(3) . . . . ? C11 Pd1 N11 C18 -143.6(3) . . . . ? N12 Pd1 N11 C18 -139.1(5) . . . . ? O1 Pd1 N11 C18 42.6(3) . . . . ? C11 Pd1 N11 C17 -20.1(3) . . . . ? N12 Pd1 N11 C17 -15.7(7) . . . . ? O1 Pd1 N11 C17 166.1(3) . . . . ? C11 Pd1 N12 C111 92.8(3) . . . . ? N11 Pd1 N12 C111 88.4(6) . . . . ? O1 Pd1 N12 C111 -93.4(3) . . . . ? C11 Pd1 N12 C112 -146.8(3) . . . . ? N11 Pd1 N12 C112 -151.2(5) . . . . ? O1 Pd1 N12 C112 27.0(3) . . . . ? C11 Pd1 N12 C110 -24.3(3) . . . . ? N11 Pd1 N12 C110 -28.8(6) . . . . ? O1 Pd1 N12 C110 149.5(3) . . . . ? C21 Pd2 N21 C29 95.6(3) . . . . ? N22 Pd2 N21 C29 93.5(6) . . . . ? O2 Pd2 N21 C29 -81.7(3) . . . . ? C21 Pd2 N21 C28 -145.2(3) . . . . ? N22 Pd2 N21 C28 -147.3(5) . . . . ? O2 Pd2 N21 C28 37.5(3) . . . . ? C21 Pd2 N21 C27 -22.8(3) . . . . ? N22 Pd2 N21 C27 -25.0(7) . . . . ? O2 Pd2 N21 C27 159.9(3) . . . . ? C21 Pd2 N22 C211 93.2(3) . . . . ? N21 Pd2 N22 C211 95.3(6) . . . . ? O2 Pd2 N22 C211 -89.5(3) . . . . ? C21 Pd2 N22 C212 -146.7(4) . . . . ? N21 Pd2 N22 C212 -144.6(5) . . . . ? O2 Pd2 N22 C212 30.6(4) . . . . ? C21 Pd2 N22 C210 -24.0(3) . . . . ? N21 Pd2 N22 C210 -21.9(7) . . . . ? O2 Pd2 N22 C210 153.2(3) . . . . ? N11 Pd1 C11 C12 9.6(4) . . . . ? N12 Pd1 C11 C12 -169.1(4) . . . . ? N11 Pd1 C11 C16 -169.6(4) . . . . ? N12 Pd1 C11 C16 11.6(3) . . . . ? C16 C11 C12 C13 0.1(7) . . . . ? Pd1 C11 C12 C13 -179.1(4) . . . . ? C16 C11 C12 C17 -176.8(4) . . . . ? Pd1 C11 C12 C17 3.9(5) . . . . ? C11 C12 C13 C14 -2.2(7) . . . . ? C17 C12 C13 C14 174.3(5) . . . . ? C12 C13 C14 C15 1.8(8) . . . . ? C13 C14 C15 C16 0.9(7) . . . . ? C14 C15 C16 C11 -2.9(7) . . . . ? C14 C15 C16 C110 174.4(4) . . . . ? C12 C11 C16 C15 2.5(7) . . . . ? Pd1 C11 C16 C15 -178.3(3) . . . . ? C12 C11 C16 C110 -175.2(4) . . . . ? Pd1 C11 C16 C110 4.0(5) . . . . ? C11 C12 C17 N11 -20.9(6) . . . . ? C13 C12 C17 N11 162.4(5) . . . . ? C19 N11 C17 C12 -89.6(5) . . . . ? C18 N11 C17 C12 152.0(4) . . . . ? Pd1 N11 C17 C12 26.6(4) . . . . ? C111 N12 C110 C16 -85.6(4) . . . . ? C112 N12 C110 C16 156.8(4) . . . . ? Pd1 N12 C110 C16 31.6(4) . . . . ? C15 C16 C110 N12 158.2(4) . . . . ? C11 C16 C110 N12 -24.3(5) . . . . ? N22 Pd2 C21 C22 -170.4(4) . . . . ? N21 Pd2 C21 C22 10.2(3) . . . . ? N22 Pd2 C21 C26 11.9(3) . . . . ? N21 Pd2 C21 C26 -167.5(4) . . . . ? C26 C21 C22 C23 -0.9(7) . . . . ? Pd2 C21 C22 C23 -178.5(3) . . . . ? C26 C21 C22 C27 -176.6(4) . . . . ? Pd2 C21 C22 C27 5.8(6) . . . . ? C21 C22 C23 C24 -0.1(7) . . . . ? C27 C22 C23 C24 175.0(5) . . . . ? C22 C23 C24 C25 -0.8(9) . . . . ? C23 C24 C25 C26 2.5(8) . . . . ? C24 C25 C26 C21 -3.3(7) . . . . ? C24 C25 C26 C210 173.0(5) . . . . ? C22 C21 C26 C25 2.6(7) . . . . ? Pd2 C21 C26 C25 -179.8(3) . . . . ? C22 C21 C26 C210 -174.2(4) . . . . ? Pd2 C21 C26 C210 3.4(5) . . . . ? C21 C22 C27 N21 -25.2(6) . . . . ? C23 C22 C27 N21 159.6(5) . . . . ? C29 N21 C27 C22 -85.6(5) . . . . ? C28 N21 C27 C22 155.1(4) . . . . ? Pd2 N21 C27 C22 30.9(4) . . . . ? C211 N22 C210 C26 -86.0(5) . . . . ? C212 N22 C210 C26 156.2(4) . . . . ? Pd2 N22 C210 C26 31.0(4) . . . . ? C25 C26 C210 N22 159.9(5) . . . . ? C21 C26 C210 N22 -23.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.846 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.160 #===END