# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Damir Safin' _publ_contact_author_email damir.safin@ksu.ru _publ_author_name 'M.Babashkina ' data_safin87 _database_code_depnum_ccdc_archive 'CCDC 852935' #TrackingRef '- [(PdLCl2)].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H46 Cl2 N4 O9 P2 Pd2 S4' _chemical_formula_sum 'C30 H46 Cl2 N4 O9 P2 Pd2 S4' _chemical_formula_weight 1080.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 8.6119(9) _cell_length_b 11.1471(14) _cell_length_c 13.3906(9) _cell_angle_alpha 106.140(9) _cell_angle_beta 99.678(7) _cell_angle_gamma 108.160(10) _cell_volume 1126.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3261 _cell_measurement_theta_min 2.0506 _cell_measurement_theta_max 21.7052 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 546 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_T_min 0.94644 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'RU200 rotating anode' _diffrn_radiation_monochromator 'Zr filter' _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '120 images, \D\F 2.0\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6570 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 21.75 _reflns_number_total 2535 _reflns_number_gt 1990 _reflns_threshold_expression >2sigma(I) _computing_data_collection MAR _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1124P)^2^+3.7458P] 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 2535 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1819 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _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 0.48603(9) -0.05073(8) 0.11121(6) 0.0433(4) Uani 1 1 d . . . Cl2 Cl 0.5375(3) -0.2257(2) 0.1601(2) 0.0490(7) Uani 1 1 d . . . S3 S 0.4515(4) 0.0304(3) 0.2826(2) 0.0586(8) Uani 1 1 d . . . P4 P 0.4280(3) 0.2061(3) 0.2919(2) 0.0479(8) Uani 1 1 d . . . O5 O 0.2472(9) 0.1952(7) 0.2362(6) 0.0545(19) Uani 1 1 d . . . C6 C 0.0899(14) 0.1082(12) 0.2511(10) 0.065(3) Uani 1 1 d . . . H6 H 0.1199 0.0707 0.3062 0.078 Uiso 1 1 calc R . . C7 C -0.005(2) 0.1970(17) 0.290(2) 0.151(10) Uani 1 1 d . . . H7A H 0.0646 0.2682 0.3566 0.227 Uiso 1 1 calc R . . H7B H -0.1083 0.1441 0.3004 0.227 Uiso 1 1 calc R . . H7C H -0.0325 0.2351 0.2362 0.227 Uiso 1 1 calc R . . C8 C -0.0094(19) -0.0043(17) 0.1453(14) 0.120(7) Uani 1 1 d . . . H8A H -0.0327 0.0327 0.0904 0.181 Uiso 1 1 calc R . . H8B H -0.1147 -0.0592 0.1524 0.181 Uiso 1 1 calc R . . H8C H 0.0556 -0.0585 0.1253 0.181 Uiso 1 1 calc R . . O9 O 0.4560(9) 0.2883(7) 0.4133(6) 0.056(2) Uani 1 1 d . . . C10 C 0.5938(17) 0.3122(14) 0.5057(9) 0.070(4) Uani 1 1 d . . . H10 H 0.6105 0.2283 0.5025 0.084 Uiso 1 1 calc R . . C11 C 0.548(3) 0.364(3) 0.6007(15) 0.194(12) Uani 1 1 d . . . H11A H 0.4846 0.4185 0.5887 0.292 Uiso 1 1 calc R . . H11B H 0.6496 0.4190 0.6595 0.292 Uiso 1 1 calc R . . H11C H 0.4803 0.2912 0.6184 0.292 Uiso 1 1 calc R . . C12 C 0.754(3) 0.418(2) 0.5102(17) 0.172(11) Uani 1 1 d . . . H12A H 0.7350 0.4984 0.5120 0.259 Uiso 1 1 calc R . . H12B H 0.7905 0.3860 0.4474 0.259 Uiso 1 1 calc R . . H12C H 0.8409 0.4365 0.5742 0.259 Uiso 1 1 calc R . . N13 N 0.5592(11) 0.3014(8) 0.2455(7) 0.047(2) Uani 1 1 d . . . C14 C 0.5767(12) 0.2659(10) 0.1487(9) 0.046(3) Uani 1 1 d . . . N15 N 0.6946(11) 0.3416(8) 0.1167(7) 0.048(2) Uani 1 1 d . . . H15 H 0.6982 0.3064 0.0517 0.058 Uiso 1 1 calc R . . C16 C 0.8161(14) 0.4740(10) 0.1764(9) 0.049(3) Uani 1 1 d . . . C17 C 0.7735(15) 0.5658(11) 0.2496(11) 0.067(4) Uani 1 1 d . . . H17 H 0.6675 0.5385 0.2625 0.080 Uiso 1 1 calc R . . C18 C 0.8888(17) 0.6984(12) 0.3036(12) 0.080(4) Uani 1 1 d . . . H18 H 0.8598 0.7602 0.3516 0.096 Uiso 1 1 calc R . . C19 C 1.0460(16) 0.7366(12) 0.2850(10) 0.067(3) Uani 1 1 d . . . H19 H 1.1240 0.8248 0.3210 0.080 Uiso 1 1 calc R . . C20 C 1.0891(15) 0.6461(11) 0.2138(10) 0.059(3) Uani 1 1 d . . . H20 H 1.1948 0.6741 0.2006 0.071 Uiso 1 1 calc R . . C21 C 0.9756(13) 0.5125(11) 0.1610(9) 0.048(3) Uani 1 1 d . . . S21 S 0.4329(3) 0.1068(3) 0.0460(2) 0.0440(7) Uani 1 1 d . . . C22 C 1.0290(15) 0.4140(12) 0.0862(9) 0.050(3) Uani 1 1 d . . . O23 O 0.9345(10) 0.3046(9) 0.0228(7) 0.071(2) Uani 1 1 d . . . O24 O 1.1945(9) 0.4627(8) 0.0975(7) 0.068(2) Uani 1 1 d . . . C25 C 1.2609(16) 0.3755(13) 0.0334(11) 0.074(4) Uani 1 1 d . . . H25A H 1.2336 0.2932 0.0485 0.111 Uiso 1 1 calc R . . H25B H 1.3822 0.4195 0.0508 0.111 Uiso 1 1 calc R . . H25C H 1.2112 0.3555 -0.0419 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0331(5) 0.0499(6) 0.0516(6) 0.0183(4) 0.0128(4) 0.0210(4) Cl2 0.0491(16) 0.0502(15) 0.0693(18) 0.0323(13) 0.0264(14) 0.0320(13) S3 0.067(2) 0.0670(19) 0.0577(18) 0.0268(15) 0.0280(16) 0.0360(16) P4 0.0369(16) 0.0590(18) 0.0500(17) 0.0176(14) 0.0156(14) 0.0206(14) O5 0.034(4) 0.073(5) 0.062(5) 0.029(4) 0.018(4) 0.021(4) C6 0.040(7) 0.080(9) 0.065(8) 0.026(7) 0.020(6) 0.007(6) C7 0.079(12) 0.107(13) 0.28(3) 0.037(15) 0.107(16) 0.046(10) C8 0.064(11) 0.130(14) 0.116(14) 0.017(12) 0.012(10) 0.000(10) O9 0.051(5) 0.070(5) 0.048(4) 0.015(4) 0.008(4) 0.030(4) C10 0.070(9) 0.097(10) 0.049(7) 0.021(7) 0.013(7) 0.047(8) C11 0.17(2) 0.36(4) 0.079(13) 0.056(19) 0.023(14) 0.17(3) C12 0.103(16) 0.19(2) 0.149(19) 0.084(16) -0.048(14) -0.013(15) N13 0.043(5) 0.044(5) 0.051(6) 0.014(4) 0.014(4) 0.016(4) C14 0.022(6) 0.049(6) 0.058(8) 0.009(6) 0.005(5) 0.013(5) N15 0.041(5) 0.056(6) 0.049(5) 0.014(5) 0.024(5) 0.018(5) C16 0.046(7) 0.052(7) 0.055(7) 0.024(6) 0.019(6) 0.021(6) C17 0.045(7) 0.056(8) 0.101(10) 0.021(7) 0.034(7) 0.020(6) C18 0.072(10) 0.052(8) 0.113(11) 0.016(8) 0.037(9) 0.025(7) C19 0.056(8) 0.048(7) 0.083(9) 0.015(6) 0.020(7) 0.010(6) C20 0.041(7) 0.058(8) 0.079(8) 0.028(7) 0.014(6) 0.018(6) C21 0.032(6) 0.060(7) 0.060(7) 0.028(6) 0.014(6) 0.022(6) S21 0.0357(15) 0.0479(16) 0.0508(16) 0.0173(13) 0.0095(13) 0.0206(12) C22 0.039(7) 0.065(8) 0.060(7) 0.036(6) 0.015(6) 0.026(6) O23 0.036(5) 0.073(6) 0.087(6) 0.006(5) 0.021(4) 0.015(4) O24 0.035(5) 0.066(5) 0.104(7) 0.023(5) 0.024(4) 0.025(4) C25 0.056(8) 0.097(10) 0.099(10) 0.049(8) 0.039(8) 0.046(7) _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 S21 2.298(3) . ? Pd1 S21 2.311(3) 2_655 ? Pd1 S3 2.328(3) . ? Pd1 Cl2 2.363(3) . ? S3 P4 2.004(4) . ? P4 O5 1.561(8) . ? P4 O9 1.563(7) . ? P4 N13 1.626(9) . ? O5 C6 1.481(12) . ? C6 C8 1.499(18) . ? C6 C7 1.510(19) . ? C6 H6 0.9800 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O9 C10 1.462(14) . ? C10 C11 1.42(2) . ? C10 C12 1.49(2) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N13 C14 1.295(13) . ? C14 N15 1.319(13) . ? C14 S21 1.809(10) . ? N15 C16 1.419(13) . ? N15 H15 0.8600 . ? C16 C21 1.376(14) . ? C16 C17 1.392(15) . ? C17 C18 1.394(16) . ? C17 H17 0.9300 . ? C18 C19 1.374(17) . ? C18 H18 0.9300 . ? C19 C20 1.372(16) . ? C19 H19 0.9300 . ? C20 C21 1.396(15) . ? C20 H20 0.9300 . ? C21 C22 1.509(16) . ? S21 Pd1 2.312(3) 2_655 ? C22 O23 1.201(13) . ? C22 O24 1.322(13) . ? O24 C25 1.433(13) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? 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 S21 Pd1 S21 81.72(10) . 2_655 ? S21 Pd1 S3 98.15(10) . . ? S21 Pd1 S3 170.43(11) 2_655 . ? S21 Pd1 Cl2 174.23(10) . . ? S21 Pd1 Cl2 92.99(9) 2_655 . ? S3 Pd1 Cl2 87.45(10) . . ? P4 S3 Pd1 104.37(15) . . ? O5 P4 O9 102.9(4) . . ? O5 P4 N13 105.7(4) . . ? O9 P4 N13 107.7(4) . . ? O5 P4 S3 115.5(3) . . ? O9 P4 S3 108.5(3) . . ? N13 P4 S3 115.6(3) . . ? C6 O5 P4 122.5(7) . . ? O5 C6 C8 108.3(10) . . ? O5 C6 C7 107.0(11) . . ? C8 C6 C7 112.8(14) . . ? O5 C6 H6 109.6 . . ? C8 C6 H6 109.6 . . ? C7 C6 H6 109.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 O9 P4 126.9(7) . . ? C11 C10 O9 107.3(12) . . ? C11 C10 C12 106.6(18) . . ? O9 C10 C12 110.8(12) . . ? C11 C10 H10 110.7 . . ? O9 C10 H10 110.7 . . ? C12 C10 H10 110.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 N13 P4 125.4(7) . . ? N13 C14 N15 123.8(9) . . ? N13 C14 S21 120.9(8) . . ? N15 C14 S21 115.3(8) . . ? C14 N15 C16 127.9(8) . . ? C14 N15 H15 116.0 . . ? C16 N15 H15 116.0 . . ? C21 C16 C17 119.9(10) . . ? C21 C16 N15 119.9(9) . . ? C17 C16 N15 120.2(9) . . ? C16 C17 C18 120.4(11) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 119.1(11) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 120.7(11) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.6(11) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 119.2(10) . . ? C16 C21 C22 121.4(10) . . ? C20 C21 C22 119.4(10) . . ? C14 S21 Pd1 103.4(4) . . ? C14 S21 Pd1 114.4(4) . 2_655 ? Pd1 S21 Pd1 98.28(10) . 2_655 ? O23 C22 O24 123.1(11) . . ? O23 C22 C21 125.0(10) . . ? O24 C22 C21 111.8(10) . . ? C22 O24 C25 116.7(9) . . ? O24 C25 H25A 109.5 . . ? O24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 S21 Pd1 S3 P4 -7.87(17) . . . . ? Cl2 Pd1 S3 P4 173.52(16) . . . . ? Pd1 S3 P4 O5 81.1(3) . . . . ? Pd1 S3 P4 O9 -164.1(3) . . . . ? Pd1 S3 P4 N13 -43.0(4) . . . . ? O9 P4 O5 C6 -71.7(8) . . . . ? N13 P4 O5 C6 175.4(8) . . . . ? S3 P4 O5 C6 46.3(8) . . . . ? P4 O5 C6 C8 -112.6(11) . . . . ? P4 O5 C6 C7 125.6(13) . . . . ? O5 P4 O9 C10 170.5(9) . . . . ? N13 P4 O9 C10 -78.1(10) . . . . ? S3 P4 O9 C10 47.7(10) . . . . ? P4 O9 C10 C11 -167.2(14) . . . . ? P4 O9 C10 C12 76.8(16) . . . . ? O5 P4 N13 C14 -72.9(10) . . . . ? O9 P4 N13 C14 177.6(9) . . . . ? S3 P4 N13 C14 56.2(10) . . . . ? P4 N13 C14 N15 -173.8(8) . . . . ? P4 N13 C14 S21 7.9(13) . . . . ? N13 C14 N15 C16 -3.2(17) . . . . ? S21 C14 N15 C16 175.2(8) . . . . ? C14 N15 C16 C21 145.8(11) . . . . ? C14 N15 C16 C17 -35.1(17) . . . . ? C21 C16 C17 C18 3.0(19) . . . . ? N15 C16 C17 C18 -176.1(12) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C17 C18 C19 C20 0(2) . . . . ? C18 C19 C20 C21 -2(2) . . . . ? C17 C16 C21 C20 -4.2(17) . . . . ? N15 C16 C21 C20 174.9(10) . . . . ? C17 C16 C21 C22 177.2(11) . . . . ? N15 C16 C21 C22 -3.7(16) . . . . ? C19 C20 C21 C16 3.6(17) . . . . ? C19 C20 C21 C22 -177.8(11) . . . . ? N13 C14 S21 Pd1 -65.1(9) . . . . ? N15 C14 S21 Pd1 116.4(8) . . . . ? N13 C14 S21 Pd1 -170.9(7) . . . 2_655 ? N15 C14 S21 Pd1 10.7(9) . . . 2_655 ? S21 Pd1 S21 C14 -117.7(4) 2_655 . . . ? S3 Pd1 S21 C14 52.6(4) . . . . ? S21 Pd1 S21 Pd1 0.000(1) 2_655 . . 2_655 ? S3 Pd1 S21 Pd1 170.34(11) . . . 2_655 ? C16 C21 C22 O23 12.2(18) . . . . ? C20 C21 C22 O23 -166.4(11) . . . . ? C16 C21 C22 O24 -168.4(10) . . . . ? C20 C21 C22 O24 13.1(15) . . . . ? O23 C22 O24 C25 -2.9(17) . . . . ? C21 C22 O24 C25 177.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 21.75 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.038 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.141 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.000 0.500 96 8 ' ' _platon_squeeze_details ; The unit cell contains 1 H2O molecule which has been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; # Attachment '- [PdL2].cif' data_safin95 _database_code_depnum_ccdc_archive 'CCDC 852936' #TrackingRef '- [PdL2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 N4 O8 P2 Pd S4, C4 H8 O2' _chemical_formula_sum 'C34 H52 N4 O10 P2 Pd S4' _chemical_formula_weight 973.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3910(5) _cell_length_b 9.6617(10) _cell_length_c 13.2526(14) _cell_angle_alpha 111.262(10) _cell_angle_beta 104.326(7) _cell_angle_gamma 92.377(7) _cell_volume 1074.23(17) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5895 _cell_measurement_theta_min 2.2656 _cell_measurement_theta_max 25.2426 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_T_min 0.96394 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET) (compiled Nov 19 2010,18:13:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku Ultra 18 rotating anode' _diffrn_radiation_monochromator 'Zr filter' _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '110 images, \D\F 2.0\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8795 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.30 _reflns_number_total 3669 _reflns_number_gt 3371 _reflns_threshold_expression >2sigma(I) _computing_data_collection MAR _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET) (compiled Nov 19 2010,18:13:43) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.45 (release 19-11-2010 CrysAlis171 .NET) (compiled Nov 19 2010,18:13:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0413P)^2^+0.9112P] 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 3669 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 1.0000 0.0000 1.0000 0.02397(10) Uani 1 2 d S . . S2 S 0.81285(8) 0.09494(8) 1.08012(6) 0.02933(16) Uani 1 1 d . . . P3 P 0.76547(7) 0.25525(7) 1.01991(6) 0.02522(16) Uani 1 1 d . . . N4 N 0.7083(3) 0.2068(3) 0.88575(19) 0.0296(5) Uani 1 1 d . . . C5 C 0.7589(3) 0.1105(3) 0.8090(2) 0.0271(6) Uani 1 1 d . . . S6 S 0.89313(8) -0.00675(9) 0.82147(6) 0.03655(19) Uani 1 1 d . . . O7 O 0.6408(2) 0.3327(2) 1.07087(15) 0.0273(4) Uani 1 1 d . . . C8 C 0.4954(3) 0.2452(3) 1.0485(2) 0.0313(6) Uani 1 1 d . . . H8 H 0.4892 0.1421 0.9909 0.038 Uiso 1 1 calc R . . C9 C 0.3788(3) 0.3249(4) 1.0007(3) 0.0420(7) Uani 1 1 d . . . H9A H 0.3891 0.4284 1.0547 0.063 Uiso 1 1 calc R . . H9B H 0.2799 0.2726 0.9869 0.063 Uiso 1 1 calc R . . H9C H 0.3914 0.3253 0.9296 0.063 Uiso 1 1 calc R . . C10 C 0.4835(4) 0.2341(4) 1.1566(3) 0.0402(7) Uani 1 1 d . . . H10A H 0.5655 0.1861 1.1847 0.060 Uiso 1 1 calc R . . H10B H 0.3887 0.1740 1.1424 0.060 Uiso 1 1 calc R . . H10C H 0.4885 0.3349 1.2129 0.060 Uiso 1 1 calc R . . O11 O 0.8963(2) 0.3861(2) 1.06186(16) 0.0312(4) Uani 1 1 d . . . C12 C 0.9766(3) 0.4673(3) 1.1824(2) 0.0330(6) Uani 1 1 d . . . H12 H 0.9378 0.4220 1.2290 0.040 Uiso 1 1 calc R . . C13 C 0.9488(4) 0.6271(4) 1.2136(3) 0.0516(9) Uani 1 1 d . . . H13A H 0.9777 0.6676 1.1625 0.077 Uiso 1 1 calc R . . H13B H 1.0075 0.6867 1.2914 0.077 Uiso 1 1 calc R . . H13C H 0.8430 0.6313 1.2074 0.077 Uiso 1 1 calc R . . C14 C 1.1376(4) 0.4506(4) 1.1947(3) 0.0517(9) Uani 1 1 d . . . H14A H 1.1481 0.3438 1.1689 0.077 Uiso 1 1 calc R . . H14B H 1.1945 0.5017 1.2741 0.077 Uiso 1 1 calc R . . H14C H 1.1751 0.4954 1.1490 0.077 Uiso 1 1 calc R . . N15 N 0.7080(3) 0.0932(3) 0.69859(19) 0.0305(5) Uani 1 1 d . . . H15 H 0.7375 0.0176 0.6512 0.037 Uiso 1 1 calc R . . C16 C 0.6171(3) 0.1748(3) 0.6477(2) 0.0274(6) Uani 1 1 d . . . C17 C 0.5231(3) 0.2663(3) 0.6986(2) 0.0317(6) Uani 1 1 d . . . H17 H 0.5200 0.2763 0.7720 0.038 Uiso 1 1 calc R . . C18 C 0.4341(3) 0.3428(3) 0.6435(3) 0.0363(7) Uani 1 1 d . . . H18 H 0.3701 0.4042 0.6791 0.044 Uiso 1 1 calc R . . C19 C 0.4381(3) 0.3301(4) 0.5363(3) 0.0395(7) Uani 1 1 d . . . H19 H 0.3784 0.3844 0.4994 0.047 Uiso 1 1 calc R . . C20 C 0.5286(3) 0.2387(3) 0.4838(3) 0.0355(6) Uani 1 1 d . . . H20 H 0.5291 0.2286 0.4098 0.043 Uiso 1 1 calc R . . C21 C 0.6201(3) 0.1606(3) 0.5378(2) 0.0292(6) Uani 1 1 d . . . C22 C 0.7173(3) 0.0630(3) 0.4784(2) 0.0315(6) Uani 1 1 d . . . O23 O 0.8037(2) -0.0070(3) 0.51749(18) 0.0424(5) Uani 1 1 d . . . O24 O 0.7015(3) 0.0602(2) 0.37473(18) 0.0420(5) Uani 1 1 d . . . C25 C 0.7931(4) -0.0334(4) 0.3137(3) 0.0500(9) Uani 1 1 d . . . H25A H 0.8980 0.0077 0.3521 0.075 Uiso 1 1 calc R . . H25B H 0.7687 -0.0358 0.2367 0.075 Uiso 1 1 calc R . . H25C H 0.7746 -0.1354 0.3110 0.075 Uiso 1 1 calc R . . O31 O 0.8813(3) 0.5259(3) 0.4234(2) 0.0529(6) Uani 1 1 d . . . C32 C 0.8824(4) 0.3867(4) 0.4356(3) 0.0568(9) Uani 1 1 d . . . H32A H 0.8280 0.3056 0.3628 0.068 Uiso 1 1 calc R . . H32B H 0.8304 0.3875 0.4922 0.068 Uiso 1 1 calc R . . C33 C 1.0359(4) 0.3558(4) 0.4715(3) 0.0575(10) Uani 1 1 d . . . H33A H 1.0330 0.2588 0.4809 0.069 Uiso 1 1 calc R . . H33B H 1.0860 0.3481 0.4125 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02598(17) 0.02580(16) 0.02501(16) 0.01217(12) 0.01102(11) 0.00995(11) S2 0.0315(4) 0.0336(4) 0.0318(4) 0.0172(3) 0.0161(3) 0.0134(3) P3 0.0272(4) 0.0254(3) 0.0245(4) 0.0092(3) 0.0098(3) 0.0070(3) N4 0.0339(13) 0.0310(12) 0.0255(12) 0.0111(10) 0.0099(9) 0.0104(10) C5 0.0264(14) 0.0294(13) 0.0276(14) 0.0119(11) 0.0092(10) 0.0063(11) S6 0.0424(4) 0.0476(4) 0.0277(4) 0.0180(3) 0.0156(3) 0.0256(3) O7 0.0268(10) 0.0256(9) 0.0294(10) 0.0081(8) 0.0111(8) 0.0070(8) C8 0.0299(15) 0.0310(14) 0.0305(15) 0.0077(12) 0.0103(11) 0.0064(12) C9 0.0325(16) 0.0536(19) 0.0425(18) 0.0198(15) 0.0119(13) 0.0141(14) C10 0.0405(17) 0.0454(18) 0.0389(17) 0.0176(14) 0.0163(13) 0.0077(14) O11 0.0321(11) 0.0321(10) 0.0298(10) 0.0114(8) 0.0107(8) 0.0017(8) C12 0.0275(15) 0.0336(15) 0.0316(15) 0.0071(12) 0.0064(11) 0.0006(12) C13 0.050(2) 0.0372(18) 0.052(2) 0.0059(16) 0.0049(16) 0.0089(15) C14 0.0314(17) 0.0483(19) 0.060(2) 0.0077(17) 0.0065(15) 0.0065(15) N15 0.0343(13) 0.0322(12) 0.0238(12) 0.0078(10) 0.0091(9) 0.0135(10) C16 0.0272(14) 0.0264(13) 0.0258(14) 0.0088(11) 0.0047(10) 0.0024(11) C17 0.0307(15) 0.0335(14) 0.0285(15) 0.0087(12) 0.0088(11) 0.0073(12) C18 0.0323(16) 0.0366(16) 0.0420(17) 0.0150(14) 0.0131(13) 0.0103(13) C19 0.0372(17) 0.0409(17) 0.0467(18) 0.0246(15) 0.0099(13) 0.0119(14) C20 0.0362(16) 0.0397(16) 0.0345(16) 0.0203(13) 0.0079(12) 0.0046(13) C21 0.0296(14) 0.0268(13) 0.0295(14) 0.0097(11) 0.0075(11) 0.0011(11) C22 0.0369(16) 0.0301(14) 0.0272(14) 0.0092(12) 0.0120(12) 0.0014(12) O23 0.0464(13) 0.0501(13) 0.0351(12) 0.0160(10) 0.0172(10) 0.0229(11) O24 0.0603(14) 0.0424(12) 0.0339(12) 0.0188(10) 0.0240(10) 0.0160(11) C25 0.072(2) 0.0472(19) 0.0420(19) 0.0167(16) 0.0340(17) 0.0172(18) O31 0.0493(14) 0.0527(14) 0.0524(15) 0.0211(12) 0.0046(11) 0.0123(11) C32 0.058(2) 0.051(2) 0.055(2) 0.0191(18) 0.0084(17) -0.0027(17) C33 0.064(2) 0.0421(19) 0.059(2) 0.0170(17) 0.0084(18) 0.0143(17) _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 S6 2.3058(7) 2_757 ? Pd1 S6 2.3059(7) . ? Pd1 S2 2.3256(7) 2_757 ? Pd1 S2 2.3256(7) . ? S2 P3 2.0029(9) . ? P3 O11 1.562(2) . ? P3 O7 1.5759(18) . ? P3 N4 1.604(2) . ? N4 C5 1.310(3) . ? C5 N15 1.366(3) . ? C5 S6 1.747(3) . ? O7 C8 1.480(3) . ? C8 C10 1.506(4) . ? C8 C9 1.507(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O11 C12 1.477(3) . ? C12 C13 1.499(4) . ? C12 C14 1.501(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N15 C16 1.401(3) . ? N15 H15 0.8800 . ? C16 C17 1.394(4) . ? C16 C21 1.420(4) . ? C17 C18 1.385(4) . ? C17 H17 0.9500 . ? C18 C19 1.391(4) . ? C18 H18 0.9500 . ? C19 C20 1.377(4) . ? C19 H19 0.9500 . ? C20 C21 1.401(4) . ? C20 H20 0.9500 . ? C21 C22 1.494(4) . ? C22 O23 1.216(3) . ? C22 O24 1.334(3) . ? O24 C25 1.445(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O31 C32 1.412(4) . ? O31 C33 1.445(4) 2_766 ? C32 C33 1.481(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O31 1.445(4) 2_766 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 S6 Pd1 S6 179.999(1) 2_757 . ? S6 Pd1 S2 97.80(3) 2_757 2_757 ? S6 Pd1 S2 82.20(3) . 2_757 ? S6 Pd1 S2 82.20(3) 2_757 . ? S6 Pd1 S2 97.80(3) . . ? S2 Pd1 S2 180.00(4) 2_757 . ? P3 S2 Pd1 101.44(3) . . ? O11 P3 O7 104.06(10) . . ? O11 P3 N4 105.36(11) . . ? O7 P3 N4 107.44(11) . . ? O11 P3 S2 113.96(8) . . ? O7 P3 S2 106.76(8) . . ? N4 P3 S2 118.24(9) . . ? C5 N4 P3 127.5(2) . . ? N4 C5 N15 120.1(2) . . ? N4 C5 S6 130.7(2) . . ? N15 C5 S6 109.17(19) . . ? C5 S6 Pd1 116.79(9) . . ? C8 O7 P3 120.89(16) . . ? O7 C8 C10 108.6(2) . . ? O7 C8 C9 106.5(2) . . ? C10 C8 C9 114.0(2) . . ? O7 C8 H8 109.2 . . ? C10 C8 H8 109.2 . . ? C9 C8 H8 109.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 O11 P3 122.70(17) . . ? O11 C12 C13 107.0(2) . . ? O11 C12 C14 107.0(2) . . ? C13 C12 C14 113.2(3) . . ? O11 C12 H12 109.8 . . ? C13 C12 H12 109.8 . . ? C14 C12 H12 109.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 N15 C16 131.2(2) . . ? C5 N15 H15 114.4 . . ? C16 N15 H15 114.4 . . ? C17 C16 N15 123.3(2) . . ? C17 C16 C21 119.0(2) . . ? N15 C16 C21 117.7(2) . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 121.0(3) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 119.1(3) . . ? C20 C21 C22 119.5(3) . . ? C16 C21 C22 121.4(2) . . ? O23 C22 O24 121.8(3) . . ? O23 C22 C21 125.4(3) . . ? O24 C22 C21 112.8(2) . . ? C22 O24 C25 114.8(2) . . ? O24 C25 H25A 109.5 . . ? O24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C32 O31 C33 109.6(3) . 2_766 ? O31 C32 C33 111.5(3) . . ? O31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? O31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? O31 C33 C32 110.5(3) 2_766 . ? O31 C33 H33A 109.6 2_766 . ? C32 C33 H33A 109.6 . . ? O31 C33 H33B 109.6 2_766 . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? 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 S6 Pd1 S2 P3 136.86(4) 2_757 . . . ? S6 Pd1 S2 P3 -43.14(4) . . . . ? Pd1 S2 P3 O11 -64.35(9) . . . . ? Pd1 S2 P3 O7 -178.64(8) . . . . ? Pd1 S2 P3 N4 60.23(11) . . . . ? O11 P3 N4 C5 86.6(3) . . . . ? O7 P3 N4 C5 -162.9(2) . . . . ? S2 P3 N4 C5 -42.1(3) . . . . ? P3 N4 C5 N15 -173.2(2) . . . . ? P3 N4 C5 S6 4.9(4) . . . . ? N4 C5 S6 Pd1 1.4(3) . . . . ? N15 C5 S6 Pd1 179.73(15) . . . . ? S2 Pd1 S6 C5 -158.20(11) 2_757 . . . ? S2 Pd1 S6 C5 21.80(11) . . . . ? O11 P3 O7 C8 178.98(18) . . . . ? N4 P3 O7 C8 67.6(2) . . . . ? S2 P3 O7 C8 -60.18(19) . . . . ? P3 O7 C8 C10 111.2(2) . . . . ? P3 O7 C8 C9 -125.6(2) . . . . ? O7 P3 O11 C12 64.7(2) . . . . ? N4 P3 O11 C12 177.56(19) . . . . ? S2 P3 O11 C12 -51.2(2) . . . . ? P3 O11 C12 C13 -116.3(2) . . . . ? P3 O11 C12 C14 122.1(2) . . . . ? N4 C5 N15 C16 8.5(4) . . . . ? S6 C5 N15 C16 -170.0(2) . . . . ? C5 N15 C16 C17 -20.3(5) . . . . ? C5 N15 C16 C21 160.8(3) . . . . ? N15 C16 C17 C18 -179.1(3) . . . . ? C21 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C20 1.3(5) . . . . ? C18 C19 C20 C21 -1.5(5) . . . . ? C19 C20 C21 C16 0.9(4) . . . . ? C19 C20 C21 C22 -179.8(3) . . . . ? C17 C16 C21 C20 0.0(4) . . . . ? N15 C16 C21 C20 178.9(2) . . . . ? C17 C16 C21 C22 -179.3(3) . . . . ? N15 C16 C21 C22 -0.4(4) . . . . ? C20 C21 C22 O23 178.1(3) . . . . ? C16 C21 C22 O23 -2.6(5) . . . . ? C20 C21 C22 O24 -1.4(4) . . . . ? C16 C21 C22 O24 178.0(2) . . . . ? O23 C22 O24 C25 0.7(4) . . . . ? C21 C22 O24 C25 -179.8(3) . . . . ? C33 O31 C32 C33 -57.4(5) 2_766 . . . ? O31 C32 C33 O31 58.0(5) . . . 2_766 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.535 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.098