# 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 'Karuppannan Natarajan' _publ_contact_author_email k_natraj6@yahoo.com loop_ _publ_author_name 'Eswaran Ramachandran' 'Duraisamy Senthil Raja' 'Nattamai Bhuvanesh' 'Karuppannan Natarajan' data_pp60m _database_code_depnum_ccdc_archive 'CCDC 831519' #TrackingRef '- Complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 N4 O2 P Pd S' _chemical_formula_weight 657.00 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2896(12) _cell_length_b 11.4236(10) _cell_length_c 18.1864(15) _cell_angle_alpha 90.00 _cell_angle_beta 109.9050(10) _cell_angle_gamma 90.00 _cell_volume 2791.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9432 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.36 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8712 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31688 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6377 _reflns_number_gt 5379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.3868P] 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 6377 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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 0.582891(11) 0.781049(13) 0.012802(8) 0.02076(5) Uani 1 1 d . . . P1 P 0.66204(4) 0.65930(4) -0.04621(3) 0.02034(11) Uani 1 1 d . . . S1 S 0.43245(4) 0.71615(4) -0.06036(3) 0.02440(11) Uani 1 1 d . . . C1 C 0.54616(15) 0.96485(17) 0.11365(11) 0.0222(4) Uani 1 1 d . . . H1 H 0.5022 1.0105 0.1311 0.027 Uiso 1 1 calc R . . C2 C 0.65057(15) 0.98929(17) 0.14927(11) 0.0221(4) Uani 1 1 d . . . C3 C 0.73096(15) 0.93046(17) 0.13170(11) 0.0231(4) Uani 1 1 d . . . C4 C 0.84628(15) 1.05587(18) 0.21676(11) 0.0238(4) Uani 1 1 d . . . C5 C 0.77350(15) 1.11610(18) 0.23920(11) 0.0236(4) Uani 1 1 d . . . C6 C 0.67460(15) 1.07871(17) 0.20349(11) 0.0234(4) Uani 1 1 d . . . H6 H 0.6232 1.1158 0.2170 0.028 Uiso 1 1 calc R . . C7 C 0.94571(16) 1.09354(19) 0.24934(12) 0.0299(5) Uani 1 1 d . . . H7 H 0.9955 1.0553 0.2344 0.036 Uiso 1 1 calc R . . C8 C 0.97286(16) 1.1838(2) 0.30202(13) 0.0307(5) Uani 1 1 d . . . H8 H 1.0406 1.2073 0.3230 0.037 Uiso 1 1 calc R . . C9 C 0.90030(17) 1.24186(19) 0.32501(12) 0.0286(5) Uani 1 1 d . . . C10 C 0.80247(16) 1.20861(18) 0.29415(12) 0.0275(5) Uani 1 1 d . . . H10 H 0.7537 1.2480 0.3097 0.033 Uiso 1 1 calc R . . C11 C 1.02094(16) 1.3440(2) 0.42990(14) 0.0362(5) Uani 1 1 d . . . H11A H 1.0426 1.2681 0.4551 0.054 Uiso 1 1 calc R . . H11B H 1.0233 1.4027 0.4698 0.054 Uiso 1 1 calc R . . H11C H 1.0652 1.3677 0.4016 0.054 Uiso 1 1 calc R . . C12 C 0.36420(16) 0.80515(17) -0.01763(12) 0.0234(4) Uani 1 1 d . . . C13 C 0.19710(17) 0.8488(2) -0.01473(14) 0.0340(5) Uani 1 1 d . . . H13A H 0.2160 0.8331 0.0414 0.051 Uiso 1 1 calc R . . H13B H 0.1291 0.8208 -0.0415 0.051 Uiso 1 1 calc R . . H13C H 0.2003 0.9332 -0.0232 0.051 Uiso 1 1 calc R . . C14 C 0.75208(15) 0.56628(17) 0.02501(12) 0.0255(4) Uani 1 1 d . . . C15 C 0.83611(17) 0.5212(2) 0.01236(15) 0.0374(5) Uani 1 1 d . . . H15 H 0.8489 0.5400 -0.0342 0.045 Uiso 1 1 calc R . . C16 C 0.90093(18) 0.4488(2) 0.06789(18) 0.0492(7) Uani 1 1 d . . . H16 H 0.9582 0.4184 0.0593 0.059 Uiso 1 1 calc R . . C17 C 0.8827(2) 0.4204(2) 0.13571(16) 0.0490(7) Uani 1 1 d . . . H17 H 0.9274 0.3708 0.1735 0.059 Uiso 1 1 calc R . . C18 C 0.8002(2) 0.4640(2) 0.14825(13) 0.0429(6) Uani 1 1 d . . . H18 H 0.7874 0.4436 0.1946 0.051 Uiso 1 1 calc R . . C19 C 0.73502(18) 0.53779(19) 0.09378(12) 0.0329(5) Uani 1 1 d . . . H19 H 0.6787 0.5689 0.1035 0.039 Uiso 1 1 calc R . . C20 C 0.73017(15) 0.73731(17) -0.09884(11) 0.0227(4) Uani 1 1 d . . . C21 C 0.75919(17) 0.6826(2) -0.15641(13) 0.0317(5) Uani 1 1 d . . . H21 H 0.7418 0.6031 -0.1696 0.038 Uiso 1 1 calc R . . C22 C 0.81300(19) 0.7434(2) -0.19429(14) 0.0390(6) Uani 1 1 d . . . H22 H 0.8335 0.7056 -0.2328 0.047 Uiso 1 1 calc R . . C23 C 0.83688(18) 0.8592(2) -0.17597(13) 0.0369(5) Uani 1 1 d . . . H23 H 0.8738 0.9010 -0.2021 0.044 Uiso 1 1 calc R . . C24 C 0.80765(17) 0.91526(19) -0.11991(12) 0.0320(5) Uani 1 1 d . . . H24 H 0.8243 0.9952 -0.1078 0.038 Uiso 1 1 calc R . . C25 C 0.75390(16) 0.85455(17) -0.08120(12) 0.0259(4) Uani 1 1 d . . . H25 H 0.7335 0.8930 -0.0429 0.031 Uiso 1 1 calc R . . C26 C 0.58209(15) 0.56063(17) -0.11958(11) 0.0223(4) Uani 1 1 d . . . C27 C 0.51234(15) 0.60903(18) -0.18668(11) 0.0258(4) Uani 1 1 d . . . H27 H 0.5121 0.6910 -0.1954 0.031 Uiso 1 1 calc R . . C28 C 0.44413(16) 0.53882(19) -0.24007(12) 0.0282(5) Uani 1 1 d . . . H28 H 0.3969 0.5726 -0.2853 0.034 Uiso 1 1 calc R . . C29 C 0.44413(16) 0.4185(2) -0.22812(12) 0.0309(5) Uani 1 1 d . . . H29 H 0.3961 0.3702 -0.2644 0.037 Uiso 1 1 calc R . . C30 C 0.51469(17) 0.3699(2) -0.16304(12) 0.0325(5) Uani 1 1 d . . . H30 H 0.5160 0.2875 -0.1555 0.039 Uiso 1 1 calc R . . C31 C 0.58346(16) 0.43991(18) -0.10877(12) 0.0271(4) Uani 1 1 d . . . H31 H 0.6315 0.4056 -0.0642 0.032 Uiso 1 1 calc R . . N1 N 0.50569(12) 0.88759(14) 0.06057(9) 0.0217(3) Uani 1 1 d . . . N2 N 0.40178(12) 0.88218(14) 0.03743(9) 0.0236(4) Uani 1 1 d . . . N3 N 0.82490(13) 0.96443(15) 0.16525(10) 0.0259(4) Uani 1 1 d . . . N4 N 0.26456(13) 0.78884(15) -0.04546(11) 0.0285(4) Uani 1 1 d . . . H4N H 0.2485 0.7285 -0.0783 0.043 Uiso 1 1 d R . . O1 O 0.71685(11) 0.84226(13) 0.08366(8) 0.0281(3) Uani 1 1 d . . . O2 O 0.92152(12) 1.33432(15) 0.37632(10) 0.0399(4) 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 0.02564(9) 0.01951(8) 0.01778(8) -0.00127(6) 0.00824(6) 0.00062(6) P1 0.0247(3) 0.0176(2) 0.0189(2) -0.00105(19) 0.0076(2) -0.00042(19) S1 0.0276(3) 0.0227(3) 0.0241(3) -0.0042(2) 0.0103(2) -0.0014(2) C1 0.0282(11) 0.0218(10) 0.0197(9) 0.0003(8) 0.0122(8) 0.0018(8) C2 0.0274(10) 0.0223(10) 0.0178(9) 0.0021(8) 0.0093(8) 0.0010(8) C3 0.0284(11) 0.0230(10) 0.0178(9) 0.0016(8) 0.0078(8) 0.0036(8) C4 0.0277(11) 0.0250(10) 0.0179(9) 0.0004(8) 0.0066(8) 0.0034(8) C5 0.0263(10) 0.0251(10) 0.0191(9) 0.0005(8) 0.0073(8) 0.0021(8) C6 0.0288(11) 0.0234(10) 0.0201(10) 0.0008(8) 0.0110(8) 0.0034(8) C7 0.0262(11) 0.0351(12) 0.0275(11) -0.0032(9) 0.0079(9) 0.0059(9) C8 0.0244(11) 0.0345(12) 0.0305(11) -0.0032(9) 0.0061(9) 0.0015(9) C9 0.0327(12) 0.0265(11) 0.0254(11) -0.0046(9) 0.0084(9) -0.0003(9) C10 0.0281(11) 0.0280(11) 0.0263(11) -0.0044(9) 0.0094(9) 0.0040(9) C11 0.0301(12) 0.0396(13) 0.0365(13) -0.0101(11) 0.0080(10) -0.0065(10) C12 0.0303(11) 0.0190(9) 0.0239(10) 0.0018(8) 0.0130(9) -0.0006(8) C13 0.0316(12) 0.0307(12) 0.0444(13) -0.0065(10) 0.0190(10) -0.0038(10) C14 0.0276(11) 0.0174(9) 0.0263(10) -0.0020(8) 0.0023(8) -0.0033(8) C15 0.0321(12) 0.0287(12) 0.0489(14) 0.0064(11) 0.0106(11) 0.0011(10) C16 0.0274(13) 0.0306(13) 0.076(2) 0.0029(13) 0.0006(13) 0.0025(10) C17 0.0509(16) 0.0245(12) 0.0465(15) 0.0057(11) -0.0160(13) -0.0033(11) C18 0.0668(18) 0.0251(12) 0.0234(11) -0.0017(9) -0.0020(11) -0.0056(12) C19 0.0488(14) 0.0227(11) 0.0220(10) -0.0021(9) 0.0055(10) -0.0012(10) C20 0.0254(10) 0.0221(10) 0.0203(10) -0.0001(8) 0.0074(8) -0.0023(8) C21 0.0368(13) 0.0283(11) 0.0337(12) -0.0099(9) 0.0168(10) -0.0064(9) C22 0.0418(14) 0.0479(15) 0.0355(13) -0.0092(11) 0.0238(11) -0.0090(11) C23 0.0396(13) 0.0435(14) 0.0300(12) 0.0037(10) 0.0151(10) -0.0122(11) C24 0.0409(13) 0.0252(11) 0.0285(11) 0.0007(9) 0.0099(10) -0.0094(9) C25 0.0342(11) 0.0221(10) 0.0207(10) -0.0011(8) 0.0083(8) -0.0030(9) C26 0.0265(10) 0.0220(10) 0.0200(9) -0.0029(8) 0.0101(8) -0.0016(8) C27 0.0310(11) 0.0235(10) 0.0232(10) -0.0018(8) 0.0098(9) 0.0034(8) C28 0.0268(11) 0.0365(12) 0.0209(10) -0.0048(9) 0.0077(8) 0.0051(9) C29 0.0320(12) 0.0362(12) 0.0246(11) -0.0096(9) 0.0097(9) -0.0091(10) C30 0.0463(14) 0.0261(11) 0.0263(11) -0.0026(9) 0.0138(10) -0.0110(10) C31 0.0363(12) 0.0262(11) 0.0189(10) 0.0006(8) 0.0095(9) -0.0033(9) N1 0.0253(9) 0.0216(8) 0.0197(8) 0.0020(7) 0.0097(7) 0.0000(7) N2 0.0263(9) 0.0228(8) 0.0239(9) -0.0005(7) 0.0114(7) -0.0018(7) N3 0.0261(9) 0.0293(9) 0.0221(8) -0.0029(7) 0.0078(7) 0.0039(7) N4 0.0272(9) 0.0253(9) 0.0354(10) -0.0085(8) 0.0138(8) -0.0038(7) O1 0.0290(8) 0.0300(8) 0.0248(7) -0.0081(6) 0.0084(6) 0.0028(6) O2 0.0305(9) 0.0387(9) 0.0455(10) -0.0214(8) 0.0064(7) -0.0009(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 N1 2.0262(16) . ? Pd1 O1 2.0332(14) . ? Pd1 S1 2.2347(6) . ? Pd1 P1 2.2786(5) . ? P1 C20 1.815(2) . ? P1 C26 1.822(2) . ? P1 C14 1.824(2) . ? S1 C12 1.762(2) . ? C1 N1 1.290(2) . ? C1 C2 1.437(3) . ? C1 H1 0.9500 . ? C2 C6 1.380(3) . ? C2 C3 1.457(3) . ? C3 O1 1.304(2) . ? C3 N3 1.329(3) . ? C4 N3 1.366(3) . ? C4 C7 1.408(3) . ? C4 C5 1.418(3) . ? C5 C6 1.406(3) . ? C5 C10 1.416(3) . ? C6 H6 0.9500 . ? C7 C8 1.371(3) . ? C7 H7 0.9500 . ? C8 C9 1.409(3) . ? C8 H8 0.9500 . ? C9 C10 1.371(3) . ? C9 O2 1.373(3) . ? C10 H10 0.9500 . ? C11 O2 1.427(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.304(3) . ? C12 N4 1.352(3) . ? C13 N4 1.441(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.392(3) . ? C14 C15 1.396(3) . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 C18 1.369(4) . ? C17 H17 0.9500 . ? C18 C19 1.390(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.392(3) . ? C20 C21 1.398(3) . ? C21 C22 1.382(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C22 H22 0.9500 . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.392(3) . ? C26 C27 1.400(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.392(3) . ? C28 H28 0.9500 . ? C29 C30 1.383(3) . ? C29 H29 0.9500 . ? C30 C31 1.386(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? N1 N2 1.400(2) . ? N4 H4N 0.8895 . ? 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 N1 Pd1 O1 93.10(6) . . ? N1 Pd1 S1 84.31(5) . . ? O1 Pd1 S1 177.09(4) . . ? N1 Pd1 P1 176.97(5) . . ? O1 Pd1 P1 89.84(4) . . ? S1 Pd1 P1 92.765(19) . . ? C20 P1 C26 103.46(9) . . ? C20 P1 C14 106.58(10) . . ? C26 P1 C14 105.93(9) . . ? C20 P1 Pd1 112.96(7) . . ? C26 P1 Pd1 115.76(7) . . ? C14 P1 Pd1 111.37(7) . . ? C12 S1 Pd1 96.35(7) . . ? N1 C1 C2 127.02(18) . . ? N1 C1 H1 116.5 . . ? C2 C1 H1 116.5 . . ? C6 C2 C1 115.69(18) . . ? C6 C2 C3 118.38(19) . . ? C1 C2 C3 125.91(18) . . ? O1 C3 N3 115.78(18) . . ? O1 C3 C2 123.35(18) . . ? N3 C3 C2 120.86(18) . . ? N3 C4 C7 118.69(18) . . ? N3 C4 C5 123.61(19) . . ? C7 C4 C5 117.69(18) . . ? C6 C5 C10 123.99(19) . . ? C6 C5 C4 116.11(18) . . ? C10 C5 C4 119.89(19) . . ? C2 C6 C5 121.43(19) . . ? C2 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C4 121.9(2) . . ? C8 C7 H7 119.0 . . ? C4 C7 H7 119.0 . . ? C7 C8 C9 120.0(2) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 O2 116.73(19) . . ? C10 C9 C8 119.9(2) . . ? O2 C9 C8 123.3(2) . . ? C9 C10 C5 120.54(19) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 N4 119.12(18) . . ? N2 C12 S1 125.68(16) . . ? N4 C12 S1 115.21(15) . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.0(2) . . ? C19 C14 P1 118.51(17) . . ? C15 C14 P1 122.44(17) . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.2(2) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C25 C20 C21 119.45(19) . . ? C25 C20 P1 118.90(15) . . ? C21 C20 P1 121.65(16) . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.7(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 120.0(2) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C20 119.75(19) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? C31 C26 C27 119.07(18) . . ? C31 C26 P1 122.30(15) . . ? C27 C26 P1 118.49(15) . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.2(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.4(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.7(2) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C26 119.9(2) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C1 N1 N2 114.48(16) . . ? C1 N1 Pd1 124.12(14) . . ? N2 N1 Pd1 121.40(12) . . ? C12 N2 N1 112.22(16) . . ? C3 N3 C4 119.53(17) . . ? C12 N4 C13 123.21(18) . . ? C12 N4 H4N 110.9 . . ? C13 N4 H4N 125.1 . . ? C3 O1 Pd1 126.02(13) . . ? C9 O2 C11 117.48(18) . . ? 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 N1 Pd1 P1 C20 101.5(9) . . . . ? O1 Pd1 P1 C20 -64.81(8) . . . . ? S1 Pd1 P1 C20 116.48(7) . . . . ? N1 Pd1 P1 C26 -17.5(9) . . . . ? O1 Pd1 P1 C26 176.16(8) . . . . ? S1 Pd1 P1 C26 -2.54(7) . . . . ? N1 Pd1 P1 C14 -138.6(9) . . . . ? O1 Pd1 P1 C14 55.09(8) . . . . ? S1 Pd1 P1 C14 -123.61(7) . . . . ? N1 Pd1 S1 C12 -1.56(8) . . . . ? O1 Pd1 S1 C12 25.7(9) . . . . ? P1 Pd1 S1 C12 179.22(7) . . . . ? N1 C1 C2 C6 178.45(19) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? C6 C2 C3 O1 177.40(18) . . . . ? C1 C2 C3 O1 -4.2(3) . . . . ? C6 C2 C3 N3 -2.1(3) . . . . ? C1 C2 C3 N3 176.36(18) . . . . ? N3 C4 C5 C6 -1.7(3) . . . . ? C7 C4 C5 C6 177.90(18) . . . . ? N3 C4 C5 C10 178.81(18) . . . . ? C7 C4 C5 C10 -1.6(3) . . . . ? C1 C2 C6 C5 -176.18(18) . . . . ? C3 C2 C6 C5 2.4(3) . . . . ? C10 C5 C6 C2 178.85(19) . . . . ? C4 C5 C6 C2 -0.6(3) . . . . ? N3 C4 C7 C8 -179.3(2) . . . . ? C5 C4 C7 C8 1.1(3) . . . . ? C4 C7 C8 C9 0.0(3) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C7 C8 C9 O2 -178.8(2) . . . . ? O2 C9 C10 C5 178.35(19) . . . . ? C8 C9 C10 C5 0.0(3) . . . . ? C6 C5 C10 C9 -178.4(2) . . . . ? C4 C5 C10 C9 1.1(3) . . . . ? Pd1 S1 C12 N2 1.52(18) . . . . ? Pd1 S1 C12 N4 -177.90(14) . . . . ? C20 P1 C14 C19 151.80(16) . . . . ? C26 P1 C14 C19 -98.47(17) . . . . ? Pd1 P1 C14 C19 28.19(18) . . . . ? C20 P1 C14 C15 -29.4(2) . . . . ? C26 P1 C14 C15 80.33(19) . . . . ? Pd1 P1 C14 C15 -153.01(16) . . . . ? C19 C14 C15 C16 0.2(3) . . . . ? P1 C14 C15 C16 -178.59(18) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 -0.8(4) . . . . ? C17 C18 C19 C14 1.3(3) . . . . ? C15 C14 C19 C18 -1.0(3) . . . . ? P1 C14 C19 C18 177.86(16) . . . . ? C26 P1 C20 C25 144.66(17) . . . . ? C14 P1 C20 C25 -103.89(17) . . . . ? Pd1 P1 C20 C25 18.73(19) . . . . ? C26 P1 C20 C21 -35.3(2) . . . . ? C14 P1 C20 C21 76.12(19) . . . . ? Pd1 P1 C20 C21 -161.26(16) . . . . ? C25 C20 C21 C22 1.5(3) . . . . ? P1 C20 C21 C22 -178.50(18) . . . . ? C20 C21 C22 C23 -1.0(4) . . . . ? C21 C22 C23 C24 0.1(4) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C20 0.3(3) . . . . ? C21 C20 C25 C24 -1.2(3) . . . . ? P1 C20 C25 C24 178.84(16) . . . . ? C20 P1 C26 C31 123.38(18) . . . . ? C14 P1 C26 C31 11.5(2) . . . . ? Pd1 P1 C26 C31 -112.50(16) . . . . ? C20 P1 C26 C27 -61.02(17) . . . . ? C14 P1 C26 C27 -172.95(16) . . . . ? Pd1 P1 C26 C27 63.10(17) . . . . ? C31 C26 C27 C28 1.9(3) . . . . ? P1 C26 C27 C28 -173.82(15) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C27 C28 C29 C30 -1.4(3) . . . . ? C28 C29 C30 C31 1.7(3) . . . . ? C29 C30 C31 C26 -0.1(3) . . . . ? C27 C26 C31 C30 -1.7(3) . . . . ? P1 C26 C31 C30 173.91(16) . . . . ? C2 C1 N1 N2 179.20(17) . . . . ? C2 C1 N1 Pd1 -0.9(3) . . . . ? O1 Pd1 N1 C1 3.49(16) . . . . ? S1 Pd1 N1 C1 -177.85(16) . . . . ? P1 Pd1 N1 C1 -162.8(8) . . . . ? O1 Pd1 N1 N2 -176.57(13) . . . . ? S1 Pd1 N1 N2 2.09(13) . . . . ? P1 Pd1 N1 N2 17.1(10) . . . . ? N4 C12 N2 N1 179.20(17) . . . . ? S1 C12 N2 N1 -0.2(2) . . . . ? C1 N1 N2 C12 178.32(17) . . . . ? Pd1 N1 N2 C12 -1.6(2) . . . . ? O1 C3 N3 C4 -179.62(17) . . . . ? C2 C3 N3 C4 -0.1(3) . . . . ? C7 C4 N3 C3 -177.53(19) . . . . ? C5 C4 N3 C3 2.1(3) . . . . ? N2 C12 N4 C13 -3.0(3) . . . . ? S1 C12 N4 C13 176.44(16) . . . . ? N3 C3 O1 Pd1 -171.99(13) . . . . ? C2 C3 O1 Pd1 8.5(3) . . . . ? N1 Pd1 O1 C3 -7.38(16) . . . . ? S1 Pd1 O1 C3 -34.5(10) . . . . ? P1 Pd1 O1 C3 171.90(15) . . . . ? C10 C9 O2 C11 157.6(2) . . . . ? C8 C9 O2 C11 -24.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.586 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.065 # Attachment '- Complex4_revised.cif' data_pp6op _database_code_depnum_ccdc_archive 'CCDC 880537' #TrackingRef '- Complex4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H41 N4 O4 P Pd S' _chemical_formula_weight 835.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2382(5) _cell_length_b 12.4005(5) _cell_length_c 13.5466(5) _cell_angle_alpha 67.059(2) _cell_angle_beta 80.237(2) _cell_angle_gamma 81.519(2) _cell_volume 1858.29(13) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9934 _cell_measurement_theta_min 3.57 _cell_measurement_theta_max 62.73 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 5.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6165 _exptl_absorpt_correction_T_max 0.9004 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41891 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 59.99 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 5379 _reflns_number_gt 4722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two molecules of acetone, each disordered between two positions, were found solvated. Strong restraints (DFIX, EADP, and SAME) were used to keep their bond distances, angles, and the thermal ellipsoids of the disordered atoms meaningful. ; _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^)+(0.0597P)^2^+1.1555P] 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 5379 _refine_ls_number_parameters 471 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.157 _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 0.32732(2) 0.25586(2) 0.05696(2) 0.02028(12) Uani 1 1 d . . . S1 S 0.37232(8) 0.37006(10) -0.11402(8) 0.0309(3) Uani 1 1 d . . . P1 P 0.17328(8) 0.20335(8) 0.01827(8) 0.0208(2) Uani 1 1 d . . . C1 C 0.5047(3) 0.2735(3) 0.1728(3) 0.0241(9) Uani 1 1 d . . . H1A H 0.5745 0.2981 0.1731 0.029 Uiso 1 1 calc R . . C2 C 0.4461(3) 0.2083(3) 0.2769(3) 0.0232(9) Uani 1 1 d . . . C3 C 0.3462(3) 0.1514(3) 0.2916(3) 0.0240(9) Uani 1 1 d . . . C4 C 0.3424(3) 0.0865(3) 0.4841(3) 0.0258(9) Uani 1 1 d . . . C5 C 0.4389(3) 0.1403(3) 0.4728(3) 0.0251(9) Uani 1 1 d . . . C6 C 0.4899(3) 0.1990(3) 0.3676(3) 0.0256(9) Uani 1 1 d . . . H6A H 0.5571 0.2335 0.3585 0.031 Uiso 1 1 calc R . . C7 C 0.2882(3) 0.0264(4) 0.5874(3) 0.0295(10) Uani 1 1 d . . . H7A H 0.2220 -0.0092 0.5952 0.035 Uiso 1 1 calc R . . C8 C 0.3315(4) 0.0194(4) 0.6767(3) 0.0337(10) Uani 1 1 d . . . H8A H 0.2952 -0.0218 0.7466 0.040 Uiso 1 1 calc R . . C9 C 0.4293(4) 0.0724(4) 0.6664(3) 0.0311(10) Uani 1 1 d . . . C10 C 0.4830(3) 0.1322(4) 0.5662(3) 0.0279(9) Uani 1 1 d . . . H10A H 0.5489 0.1679 0.5593 0.033 Uiso 1 1 calc R . . C11 C 0.5614(4) 0.1102(4) 0.7573(4) 0.0420(12) Uani 1 1 d . . . H11A H 0.5794 0.0902 0.8305 0.063 Uiso 1 1 calc R . . H11B H 0.5473 0.1957 0.7224 0.063 Uiso 1 1 calc R . . H11C H 0.6241 0.0821 0.7153 0.063 Uiso 1 1 calc R . . C12 C 0.5027(3) 0.4018(3) -0.0989(3) 0.0252(9) Uani 1 1 d . . . C13 C 0.6642(3) 0.5102(3) -0.2190(3) 0.0267(9) Uani 1 1 d . . . C14 C 0.7249(3) 0.5141(3) -0.1432(3) 0.0264(9) Uani 1 1 d . . . H14A H 0.6992 0.4805 -0.0683 0.032 Uiso 1 1 calc R . . C15 C 0.8238(3) 0.5678(4) -0.1779(4) 0.0319(10) Uani 1 1 d . . . H15A H 0.8663 0.5694 -0.1260 0.038 Uiso 1 1 calc R . . C16 C 0.8613(4) 0.6188(4) -0.2864(4) 0.0355(11) Uani 1 1 d . . . H16A H 0.9276 0.6578 -0.3092 0.043 Uiso 1 1 calc R . . C17 C 0.8017(4) 0.6125(4) -0.3613(4) 0.0394(11) Uani 1 1 d . . . H17A H 0.8279 0.6462 -0.4360 0.047 Uiso 1 1 calc R . . C18 C 0.7038(4) 0.5576(4) -0.3285(4) 0.0353(10) Uani 1 1 d . . . H18A H 0.6639 0.5523 -0.3806 0.042 Uiso 1 1 calc R . . C19 C 0.0438(3) 0.2223(3) 0.1011(3) 0.0231(9) Uani 1 1 d . . . C20 C -0.0473(3) 0.2961(4) 0.0583(4) 0.0330(10) Uani 1 1 d . . . H20A H -0.0453 0.3365 -0.0176 0.040 Uiso 1 1 calc R . . C21 C -0.1416(4) 0.3107(4) 0.1270(4) 0.0384(11) Uani 1 1 d . . . H21A H -0.2033 0.3624 0.0975 0.046 Uiso 1 1 calc R . . C22 C -0.1469(4) 0.2512(4) 0.2373(4) 0.0366(11) Uani 1 1 d . . . H22A H -0.2118 0.2614 0.2835 0.044 Uiso 1 1 calc R . . C23 C -0.0562(4) 0.1762(4) 0.2799(4) 0.0360(11) Uani 1 1 d . . . H23A H -0.0593 0.1340 0.3557 0.043 Uiso 1 1 calc R . . C24 C 0.0387(3) 0.1628(4) 0.2125(3) 0.0306(10) Uani 1 1 d . . . H24A H 0.1010 0.1126 0.2425 0.037 Uiso 1 1 calc R . . C25 C 0.1449(3) 0.2764(4) -0.1219(3) 0.0265(9) Uani 1 1 d . . . C26 C 0.1295(3) 0.3991(4) -0.1657(3) 0.0299(10) Uani 1 1 d . . . H26A H 0.1313 0.4428 -0.1221 0.036 Uiso 1 1 calc R . . C27 C 0.1116(4) 0.4569(4) -0.2729(4) 0.0394(11) Uani 1 1 d . . . H27A H 0.1010 0.5404 -0.3026 0.047 Uiso 1 1 calc R . . C28 C 0.1089(4) 0.3941(5) -0.3363(4) 0.0468(13) Uani 1 1 d . . . H28A H 0.0959 0.4342 -0.4095 0.056 Uiso 1 1 calc R . . C29 C 0.1252(4) 0.2722(5) -0.2940(4) 0.0448(12) Uani 1 1 d . . . H29A H 0.1242 0.2291 -0.3384 0.054 Uiso 1 1 calc R . . C30 C 0.1430(3) 0.2134(4) -0.1865(3) 0.0329(10) Uani 1 1 d . . . H30A H 0.1539 0.1299 -0.1573 0.039 Uiso 1 1 calc R . . C31 C 0.1978(3) 0.0486(3) 0.0398(3) 0.0235(9) Uani 1 1 d . . . C32 C 0.2992(3) 0.0119(4) -0.0070(3) 0.0272(9) Uani 1 1 d . . . H32A H 0.3526 0.0668 -0.0455 0.033 Uiso 1 1 calc R . . C33 C 0.3225(3) -0.1040(4) 0.0021(3) 0.0311(10) Uani 1 1 d . . . H33A H 0.3915 -0.1284 -0.0306 0.037 Uiso 1 1 calc R . . C34 C 0.2457(4) -0.1838(4) 0.0587(4) 0.0387(11) Uani 1 1 d . . . H34A H 0.2618 -0.2635 0.0655 0.046 Uiso 1 1 calc R . . C35 C 0.1450(4) -0.1483(4) 0.1057(5) 0.0506(14) Uani 1 1 d . . . H35A H 0.0925 -0.2042 0.1449 0.061 Uiso 1 1 calc R . . C36 C 0.1197(4) -0.0328(4) 0.0963(4) 0.0398(11) Uani 1 1 d . . . H36A H 0.0499 -0.0088 0.1280 0.048 Uiso 1 1 calc R . . N1 N 0.4717(2) 0.3017(3) 0.0799(2) 0.0206(7) Uani 1 1 d . . . N2 N 0.5442(3) 0.3678(3) -0.0081(3) 0.0245(7) Uani 1 1 d . . . N3 N 0.3006(3) 0.0925(3) 0.3934(3) 0.0249(7) Uani 1 1 d . . . N4 N 0.5589(3) 0.4659(3) -0.1951(3) 0.0293(8) Uani 1 1 d . . . H4N H 0.5157 0.4956 -0.2489 0.044 Uiso 1 1 d R . . O1 O 0.2968(2) 0.1485(2) 0.2166(2) 0.0265(6) Uani 1 1 d . . . O2 O 0.4647(3) 0.0558(3) 0.7625(2) 0.0414(8) Uani 1 1 d . . . C50 C 0.3783(9) 0.5246(6) 0.5967(7) 0.0268(5) Uani 0.572(9) 1 d PD A 1 C51 C 0.3897(7) 0.3986(6) 0.6040(8) 0.0268(5) Uani 0.572(9) 1 d PD A 1 H51A H 0.4674 0.3760 0.5822 0.040 Uiso 0.572(9) 1 calc PR A 1 H51B H 0.3421 0.3914 0.5559 0.040 Uiso 0.572(9) 1 calc PR A 1 H51C H 0.3670 0.3468 0.6785 0.040 Uiso 0.572(9) 1 calc PR A 1 C52 C 0.3029(15) 0.5893(14) 0.5140(13) 0.0268(5) Uani 0.572(9) 1 d PD A 1 H52A H 0.2796 0.6676 0.5159 0.040 Uiso 0.572(9) 1 calc PR A 1 H52B H 0.2373 0.5462 0.5288 0.040 Uiso 0.572(9) 1 calc PR A 1 H52C H 0.3419 0.5971 0.4424 0.040 Uiso 0.572(9) 1 calc PR A 1 O53 O 0.4205(6) 0.5761(8) 0.6314(6) 0.0268(5) Uani 0.572(9) 1 d PD A 1 C50A C 0.3664(11) 0.5331(8) 0.5775(9) 0.0268(5) Uani 0.428(9) 1 d PD A 2 C51A C 0.4154(9) 0.4063(8) 0.6102(10) 0.0268(5) Uani 0.428(9) 1 d PD A 2 H51D H 0.4223 0.3816 0.5487 0.040 Uiso 0.428(9) 1 calc PR A 2 H51E H 0.3665 0.3561 0.6705 0.040 Uiso 0.428(9) 1 calc PR A 2 H51F H 0.4891 0.3991 0.6325 0.040 Uiso 0.428(9) 1 calc PR A 2 C52A C 0.4079(13) 0.5789(15) 0.6467(11) 0.0268(5) Uani 0.428(9) 1 d PD A 2 H52D H 0.3560 0.6438 0.6550 0.040 Uiso 0.428(9) 1 calc PR A 2 H52E H 0.4811 0.6074 0.6139 0.040 Uiso 0.428(9) 1 calc PR A 2 H52F H 0.4145 0.5163 0.7177 0.040 Uiso 0.428(9) 1 calc PR A 2 O53A O 0.3007(13) 0.5862(12) 0.5237(11) 0.0268(5) Uani 0.428(9) 1 d PD A 2 C60 C 0.1598(7) 0.8586(6) 0.4409(7) 0.0268(5) Uani 0.506(8) 1 d PD B 3 C61 C 0.0685(7) 0.7808(7) 0.4540(8) 0.0268(5) Uani 0.506(8) 1 d PD B 3 H61A H 0.0611 0.7797 0.3835 0.040 Uiso 0.506(8) 1 calc PR B 3 H61B H -0.0022 0.8122 0.4831 0.040 Uiso 0.506(8) 1 calc PR B 3 H61C H 0.0881 0.7007 0.5036 0.040 Uiso 0.506(8) 1 calc PR B 3 C62 C 0.2545(11) 0.7929(12) 0.5012(11) 0.0268(5) Uani 0.506(8) 1 d PD B 3 H62A H 0.3198 0.8380 0.4721 0.040 Uiso 0.506(8) 1 calc PR B 3 H62B H 0.2716 0.7166 0.4935 0.040 Uiso 0.506(8) 1 calc PR B 3 H62C H 0.2346 0.7805 0.5777 0.040 Uiso 0.506(8) 1 calc PR B 3 O63 O 0.1407(8) 0.9582(7) 0.4201(7) 0.0268(5) Uani 0.506(8) 1 d PD B 3 C60A C 0.1687(8) 0.8374(7) 0.4613(8) 0.0268(5) Uani 0.494(8) 1 d PD B 4 C61A C 0.1004(7) 0.7709(8) 0.4228(8) 0.0268(5) Uani 0.494(8) 1 d PD B 4 H61D H 0.0797 0.6984 0.4828 0.040 Uiso 0.494(8) 1 calc PR B 4 H61E H 0.1449 0.7512 0.3638 0.040 Uiso 0.494(8) 1 calc PR B 4 H61F H 0.0330 0.8204 0.3972 0.040 Uiso 0.494(8) 1 calc PR B 4 C62A C 0.1296(12) 0.9621(9) 0.4319(12) 0.0268(5) Uani 0.494(8) 1 d PD B 4 H62D H 0.1897 1.0055 0.4330 0.040 Uiso 0.494(8) 1 calc PR B 4 H62E H 0.0659 0.9709 0.4836 0.040 Uiso 0.494(8) 1 calc PR B 4 H62F H 0.1069 0.9933 0.3592 0.040 Uiso 0.494(8) 1 calc PR B 4 O63A O 0.2545(8) 0.8012(8) 0.4856(7) 0.0268(5) Uani 0.494(8) 1 d PD B 4 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 0.02083(17) 0.02278(18) 0.01945(18) -0.00934(14) -0.00474(12) -0.00203(11) S1 0.0292(6) 0.0432(6) 0.0204(5) -0.0081(5) -0.0048(4) -0.0126(5) P1 0.0207(5) 0.0240(5) 0.0198(5) -0.0096(5) -0.0046(4) -0.0017(4) C1 0.022(2) 0.025(2) 0.028(2) -0.012(2) -0.0063(17) -0.0018(16) C2 0.027(2) 0.022(2) 0.022(2) -0.0104(19) -0.0053(17) 0.0013(16) C3 0.024(2) 0.023(2) 0.024(2) -0.0071(19) -0.0062(17) 0.0025(16) C4 0.026(2) 0.025(2) 0.024(2) -0.0075(19) -0.0058(17) 0.0017(17) C5 0.031(2) 0.021(2) 0.022(2) -0.0079(19) -0.0085(18) 0.0036(17) C6 0.027(2) 0.027(2) 0.026(2) -0.012(2) -0.0064(18) -0.0015(17) C7 0.027(2) 0.032(2) 0.028(2) -0.011(2) -0.0031(18) 0.0004(18) C8 0.037(2) 0.038(2) 0.024(2) -0.010(2) -0.0020(19) 0.001(2) C9 0.039(3) 0.032(2) 0.023(2) -0.012(2) -0.0113(19) 0.0082(19) C10 0.033(2) 0.027(2) 0.027(2) -0.012(2) -0.0107(19) 0.0014(18) C11 0.056(3) 0.046(3) 0.030(3) -0.016(2) -0.018(2) 0.001(2) C12 0.025(2) 0.026(2) 0.026(2) -0.011(2) -0.0024(18) -0.0028(17) C13 0.026(2) 0.023(2) 0.028(2) -0.0061(19) -0.0026(18) -0.0017(17) C14 0.027(2) 0.021(2) 0.028(2) -0.0062(19) -0.0041(18) 0.0001(17) C15 0.025(2) 0.028(2) 0.047(3) -0.018(2) -0.010(2) 0.0032(18) C16 0.026(2) 0.030(2) 0.047(3) -0.014(2) 0.003(2) -0.0014(18) C17 0.038(3) 0.040(3) 0.033(3) -0.010(2) 0.006(2) -0.006(2) C18 0.037(3) 0.037(3) 0.030(2) -0.010(2) -0.004(2) -0.005(2) C19 0.024(2) 0.026(2) 0.024(2) -0.0126(19) -0.0030(17) -0.0050(17) C20 0.030(2) 0.039(2) 0.028(2) -0.011(2) -0.0051(19) -0.0009(19) C21 0.024(2) 0.045(3) 0.045(3) -0.018(2) -0.005(2) 0.005(2) C22 0.031(2) 0.049(3) 0.035(3) -0.022(2) 0.005(2) -0.010(2) C23 0.032(2) 0.055(3) 0.024(2) -0.015(2) -0.0016(19) -0.015(2) C24 0.025(2) 0.042(3) 0.028(2) -0.014(2) -0.0047(18) -0.0075(19) C25 0.019(2) 0.037(2) 0.024(2) -0.011(2) -0.0042(17) -0.0009(17) C26 0.026(2) 0.034(2) 0.026(2) -0.009(2) -0.0039(18) 0.0021(18) C27 0.037(3) 0.040(3) 0.031(3) -0.006(2) -0.004(2) 0.005(2) C28 0.043(3) 0.062(3) 0.026(2) -0.006(3) -0.016(2) 0.006(2) C29 0.046(3) 0.064(3) 0.029(3) -0.020(3) -0.014(2) -0.002(2) C30 0.033(2) 0.041(3) 0.030(2) -0.017(2) -0.0088(19) -0.0025(19) C31 0.024(2) 0.025(2) 0.024(2) -0.0089(19) -0.0092(17) -0.0010(16) C32 0.030(2) 0.030(2) 0.024(2) -0.012(2) -0.0027(18) -0.0059(18) C33 0.031(2) 0.034(2) 0.033(2) -0.018(2) -0.0095(19) 0.0039(19) C34 0.039(3) 0.029(2) 0.054(3) -0.022(2) -0.009(2) -0.001(2) C35 0.038(3) 0.031(3) 0.083(4) -0.023(3) 0.006(3) -0.014(2) C36 0.028(2) 0.035(3) 0.058(3) -0.022(3) 0.005(2) -0.010(2) N1 0.0217(16) 0.0192(16) 0.0196(17) -0.0063(15) -0.0006(14) -0.0031(13) N2 0.0253(17) 0.0274(18) 0.0232(18) -0.0113(16) -0.0052(15) -0.0017(14) N3 0.0276(18) 0.0263(18) 0.0188(18) -0.0058(16) -0.0060(14) 0.0000(14) N4 0.0287(19) 0.035(2) 0.0233(18) -0.0057(17) -0.0062(15) -0.0099(15) O1 0.0262(15) 0.0298(15) 0.0246(15) -0.0080(13) -0.0085(12) -0.0063(12) O2 0.0494(19) 0.054(2) 0.0222(16) -0.0135(16) -0.0105(14) -0.0029(16) C50 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C51 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C52 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) O53 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C50A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C51A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C52A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) O53A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C60 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C61 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C62 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) O63 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C60A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C61A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) C62A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) O63A 0.0296(9) 0.0302(8) 0.0179(12) -0.0036(7) -0.0066(7) -0.0055(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.040(3) . ? Pd1 O1 2.053(3) . ? Pd1 S1 2.2167(10) . ? Pd1 P1 2.2838(10) . ? S1 C12 1.762(4) . ? P1 C31 1.812(4) . ? P1 C19 1.821(4) . ? P1 C25 1.826(4) . ? C1 N1 1.288(5) . ? C1 C2 1.448(6) . ? C1 H1A 0.9500 . ? C2 C6 1.379(5) . ? C2 C3 1.447(6) . ? C3 O1 1.282(5) . ? C3 N3 1.349(5) . ? C4 N3 1.381(5) . ? C4 C5 1.398(6) . ? C4 C7 1.404(6) . ? C5 C6 1.406(6) . ? C5 C10 1.420(6) . ? C6 H6A 0.9500 . ? C7 C8 1.369(6) . ? C7 H7A 0.9500 . ? C8 C9 1.409(6) . ? C8 H8A 0.9500 . ? C9 C10 1.372(6) . ? C9 O2 1.373(5) . ? C10 H10A 0.9500 . ? C11 O2 1.425(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.301(5) . ? C12 N4 1.361(5) . ? C13 C14 1.385(6) . ? C13 C18 1.394(6) . ? C13 N4 1.413(5) . ? C14 C15 1.389(6) . ? C14 H14A 0.9500 . ? C15 C16 1.380(7) . ? C15 H15A 0.9500 . ? C16 C17 1.377(7) . ? C16 H16A 0.9500 . ? C17 C18 1.386(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.386(6) . ? C19 C24 1.393(6) . ? C20 C21 1.391(6) . ? C20 H20A 0.9500 . ? C21 C22 1.380(7) . ? C21 H21A 0.9500 . ? C22 C23 1.386(6) . ? C22 H22A 0.9500 . ? C23 C24 1.383(6) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.386(6) . ? C25 C26 1.397(6) . ? C26 C27 1.386(6) . ? C26 H26A 0.9500 . ? C27 C28 1.373(7) . ? C27 H27A 0.9500 . ? C28 C29 1.388(7) . ? C28 H28A 0.9500 . ? C29 C30 1.391(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.393(6) . ? C31 C36 1.397(6) . ? C32 C33 1.384(6) . ? C32 H32A 0.9500 . ? C33 C34 1.374(6) . ? C33 H33A 0.9500 . ? C34 C35 1.382(7) . ? C34 H34A 0.9500 . ? C35 C36 1.381(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? N1 N2 1.405(4) . ? N4 H4N 0.9000 . ? C50 O53 1.144(4) . ? C50 C52 1.477(5) . ? C50 C51 1.514(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C50A O53A 1.132(6) . ? C50A C52A 1.456(7) . ? C50A C51A 1.516(6) . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C60 O63 1.150(4) . ? C60 C62 1.482(5) . ? C60 C61 1.525(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C60A O63A 1.129(6) . ? C60A C62A 1.465(6) . ? C60A C61A 1.529(6) . ? C61A H61D 0.9800 . ? C61A H61E 0.9800 . ? C61A H61F 0.9800 . ? C62A H62D 0.9800 . ? C62A H62E 0.9800 . ? C62A H62F 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 N1 Pd1 O1 92.43(11) . . ? N1 Pd1 S1 84.07(9) . . ? O1 Pd1 S1 176.16(7) . . ? N1 Pd1 P1 175.23(9) . . ? O1 Pd1 P1 91.11(7) . . ? S1 Pd1 P1 92.30(4) . . ? C12 S1 Pd1 97.02(14) . . ? C31 P1 C19 107.18(18) . . ? C31 P1 C25 104.86(19) . . ? C19 P1 C25 106.15(18) . . ? C31 P1 Pd1 107.34(12) . . ? C19 P1 Pd1 115.38(12) . . ? C25 P1 Pd1 115.19(14) . . ? N1 C1 C2 126.6(3) . . ? N1 C1 H1A 116.7 . . ? C2 C1 H1A 116.7 . . ? C6 C2 C3 118.4(4) . . ? C6 C2 C1 117.3(4) . . ? C3 C2 C1 124.3(4) . . ? O1 C3 N3 115.5(3) . . ? O1 C3 C2 126.4(4) . . ? N3 C3 C2 118.1(4) . . ? N3 C4 C5 119.8(4) . . ? N3 C4 C7 120.1(4) . . ? C5 C4 C7 120.1(4) . . ? C4 C5 C6 117.7(4) . . ? C4 C5 C10 119.8(4) . . ? C6 C5 C10 122.5(4) . . ? C2 C6 C5 122.5(4) . . ? C2 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C8 C7 C4 119.5(4) . . ? C8 C7 H7A 120.3 . . ? C4 C7 H7A 120.3 . . ? C7 C8 C9 120.9(4) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 O2 124.9(4) . . ? C10 C9 C8 120.5(4) . . ? O2 C9 C8 114.6(4) . . ? C9 C10 C5 119.2(4) . . ? C9 C10 H10A 120.4 . . ? C5 C10 H10A 120.4 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 N4 122.3(4) . . ? N2 C12 S1 125.5(3) . . ? N4 C12 S1 112.2(3) . . ? C14 C13 C18 119.9(4) . . ? C14 C13 N4 124.9(4) . . ? C18 C13 N4 115.2(4) . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C16 C17 C18 120.6(4) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C13 119.8(4) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? C20 C19 C24 119.2(4) . . ? C20 C19 P1 122.9(3) . . ? C24 C19 P1 117.9(3) . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C22 C21 C20 121.1(4) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C19 120.6(4) . . ? C23 C24 H24A 119.7 . . ? C19 C24 H24A 119.7 . . ? C30 C25 C26 119.6(4) . . ? C30 C25 P1 121.6(3) . . ? C26 C25 P1 118.8(3) . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.2(4) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 120.4(4) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C28 C29 C30 119.8(5) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C25 C30 C29 120.0(4) . . ? C25 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C36 119.4(4) . . ? C32 C31 P1 116.9(3) . . ? C36 C31 P1 123.6(3) . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C36 C35 C34 120.8(4) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C31 119.3(4) . . ? C35 C36 H36A 120.3 . . ? C31 C36 H36A 120.3 . . ? C1 N1 N2 114.6(3) . . ? C1 N1 Pd1 124.4(3) . . ? N2 N1 Pd1 121.0(2) . . ? C12 N2 N1 112.0(3) . . ? C3 N3 C4 123.5(3) . . ? C12 N4 C13 130.5(3) . . ? C12 N4 H4N 112.8 . . ? C13 N4 H4N 115.5 . . ? C3 O1 Pd1 123.8(2) . . ? C9 O2 C11 117.2(3) . . ? O53 C50 C52 119.0(5) . . ? O53 C50 C51 135.1(7) . . ? C52 C50 C51 105.4(8) . . ? O53A C50A C52A 120.9(7) . . ? O53A C50A C51A 133.0(9) . . ? C52A C50A C51A 105.4(9) . . ? C50A C51A H51D 109.5 . . ? C50A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C50A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C50A C52A H52D 109.5 . . ? C50A C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C50A C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? O63 C60 C62 120.9(6) . . ? O63 C60 C61 121.3(9) . . ? C62 C60 C61 112.8(8) . . ? O63A C60A C62A 122.4(6) . . ? O63A C60A C61A 121.6(9) . . ? C62A C60A C61A 113.3(8) . . ? 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 N1 Pd1 S1 C12 4.45(16) . . . . ? O1 Pd1 S1 C12 -20.2(12) . . . . ? P1 Pd1 S1 C12 -172.45(14) . . . . ? N1 Pd1 P1 C31 72.3(11) . . . . ? O1 Pd1 P1 C31 -65.64(16) . . . . ? S1 Pd1 P1 C31 112.57(14) . . . . ? N1 Pd1 P1 C19 -168.4(11) . . . . ? O1 Pd1 P1 C19 53.74(16) . . . . ? S1 Pd1 P1 C19 -128.05(14) . . . . ? N1 Pd1 P1 C25 -44.1(11) . . . . ? O1 Pd1 P1 C25 178.02(16) . . . . ? S1 Pd1 P1 C25 -3.77(15) . . . . ? N1 C1 C2 C6 -172.8(4) . . . . ? N1 C1 C2 C3 8.1(6) . . . . ? C6 C2 C3 O1 -177.8(4) . . . . ? C1 C2 C3 O1 1.3(6) . . . . ? C6 C2 C3 N3 0.3(5) . . . . ? C1 C2 C3 N3 179.4(3) . . . . ? N3 C4 C5 C6 -0.1(6) . . . . ? C7 C4 C5 C6 179.8(4) . . . . ? N3 C4 C5 C10 -178.8(3) . . . . ? C7 C4 C5 C10 1.1(6) . . . . ? C3 C2 C6 C5 -2.4(6) . . . . ? C1 C2 C6 C5 178.4(3) . . . . ? C4 C5 C6 C2 2.3(6) . . . . ? C10 C5 C6 C2 -179.0(4) . . . . ? N3 C4 C7 C8 178.9(4) . . . . ? C5 C4 C7 C8 -1.0(6) . . . . ? C4 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C7 C8 C9 O2 -178.4(4) . . . . ? O2 C9 C10 C5 178.3(4) . . . . ? C8 C9 C10 C5 0.1(6) . . . . ? C4 C5 C10 C9 -0.6(6) . . . . ? C6 C5 C10 C9 -179.3(4) . . . . ? Pd1 S1 C12 N2 -3.8(4) . . . . ? Pd1 S1 C12 N4 175.1(3) . . . . ? C18 C13 C14 C15 1.4(6) . . . . ? N4 C13 C14 C15 -175.3(4) . . . . ? C13 C14 C15 C16 1.1(6) . . . . ? C14 C15 C16 C17 -2.4(6) . . . . ? C15 C16 C17 C18 1.2(7) . . . . ? C16 C17 C18 C13 1.2(7) . . . . ? C14 C13 C18 C17 -2.5(6) . . . . ? N4 C13 C18 C17 174.5(4) . . . . ? C31 P1 C19 C20 -121.4(3) . . . . ? C25 P1 C19 C20 -9.7(4) . . . . ? Pd1 P1 C19 C20 119.2(3) . . . . ? C31 P1 C19 C24 61.1(4) . . . . ? C25 P1 C19 C24 172.7(3) . . . . ? Pd1 P1 C19 C24 -58.4(3) . . . . ? C24 C19 C20 C21 0.7(6) . . . . ? P1 C19 C20 C21 -176.8(3) . . . . ? C19 C20 C21 C22 -1.1(7) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C21 C22 C23 C24 0.9(7) . . . . ? C22 C23 C24 C19 -1.3(7) . . . . ? C20 C19 C24 C23 0.5(6) . . . . ? P1 C19 C24 C23 178.2(3) . . . . ? C31 P1 C25 C30 1.4(4) . . . . ? C19 P1 C25 C30 -111.9(3) . . . . ? Pd1 P1 C25 C30 119.1(3) . . . . ? C31 P1 C25 C26 -175.9(3) . . . . ? C19 P1 C25 C26 70.8(3) . . . . ? Pd1 P1 C25 C26 -58.2(3) . . . . ? C30 C25 C26 C27 0.5(6) . . . . ? P1 C25 C26 C27 177.9(3) . . . . ? C25 C26 C27 C28 0.0(7) . . . . ? C26 C27 C28 C29 -0.6(7) . . . . ? C27 C28 C29 C30 0.7(7) . . . . ? C26 C25 C30 C29 -0.4(6) . . . . ? P1 C25 C30 C29 -177.7(3) . . . . ? C28 C29 C30 C25 -0.2(7) . . . . ? C19 P1 C31 C32 -173.3(3) . . . . ? C25 P1 C31 C32 74.2(3) . . . . ? Pd1 P1 C31 C32 -48.8(3) . . . . ? C19 P1 C31 C36 9.3(4) . . . . ? C25 P1 C31 C36 -103.2(4) . . . . ? Pd1 P1 C31 C36 133.8(3) . . . . ? C36 C31 C32 C33 0.0(6) . . . . ? P1 C31 C32 C33 -177.5(3) . . . . ? C31 C32 C33 C34 -0.6(6) . . . . ? C32 C33 C34 C35 0.5(7) . . . . ? C33 C34 C35 C36 0.3(8) . . . . ? C34 C35 C36 C31 -0.9(8) . . . . ? C32 C31 C36 C35 0.7(7) . . . . ? P1 C31 C36 C35 178.1(4) . . . . ? C2 C1 N1 N2 178.6(3) . . . . ? C2 C1 N1 Pd1 -1.7(6) . . . . ? O1 Pd1 N1 C1 -7.7(3) . . . . ? S1 Pd1 N1 C1 173.9(3) . . . . ? P1 Pd1 N1 C1 -145.6(9) . . . . ? O1 Pd1 N1 N2 172.0(3) . . . . ? S1 Pd1 N1 N2 -6.4(2) . . . . ? P1 Pd1 N1 N2 34.1(12) . . . . ? N4 C12 N2 N1 -179.2(3) . . . . ? S1 C12 N2 N1 -0.5(5) . . . . ? C1 N1 N2 C12 -174.8(3) . . . . ? Pd1 N1 N2 C12 5.5(4) . . . . ? O1 C3 N3 C4 -179.8(3) . . . . ? C2 C3 N3 C4 1.9(5) . . . . ? C5 C4 N3 C3 -2.0(6) . . . . ? C7 C4 N3 C3 178.1(4) . . . . ? N2 C12 N4 C13 -1.6(7) . . . . ? S1 C12 N4 C13 179.5(3) . . . . ? C14 C13 N4 C12 -12.4(7) . . . . ? C18 C13 N4 C12 170.8(4) . . . . ? N3 C3 O1 Pd1 167.1(2) . . . . ? C2 C3 O1 Pd1 -14.7(5) . . . . ? N1 Pd1 O1 C3 15.6(3) . . . . ? S1 Pd1 O1 C3 40.1(14) . . . . ? P1 Pd1 O1 C3 -167.6(3) . . . . ? C10 C9 O2 C11 3.4(6) . . . . ? C8 C9 O2 C11 -178.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.830 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.088 # start Validation Reply Form _vrf_PLAT413_I ; PROBLEM: Short Inter XH3 .. XHn H10A .. H62A .. 1.59 Ang. RESPONSE: Two molecules of acetone were found solvated and both the molecules were disordered in two positions. This results in apparent short contact between the the two molecules. ; _vrf_PLAT415_I ; PROBLEM: Short Inter D-H..H-X H4N .. H52F .. 1.35 Ang. RESPONSE: Two molecules of acetone were found solvated and both the molecules were disordered in two positions. This results in apparent short contact between the the two molecules. ; # end Validation Reply Form # Attachment '- complex 3.cif' data_pp60e _database_code_depnum_ccdc_archive 'CCDC 834540' #TrackingRef '- complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H38.11 Cl N5 O3.56 P Pd S' _chemical_formula_weight 790.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.110(2) _cell_length_b 12.080(2) _cell_length_c 24.071(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.173(11) _cell_angle_gamma 90.00 _cell_volume 3504.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 861 _cell_measurement_theta_min 4.17 _cell_measurement_theta_max 60.16 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1622 _exptl_absorpt_coefficient_mu 6.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1441 _exptl_absorpt_correction_T_max 0.7860 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46209 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 59.99 _reflns_number_total 5163 _reflns_number_gt 4076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5163 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.45340(2) 0.10842(2) 0.084263(11) 0.01579(11) Uani 1 1 d . . . Cl1 Cl 0.02320(9) 0.31760(9) 0.06590(5) 0.0405(3) Uani 1 1 d . . . S1 S 0.62756(7) 0.04512(8) 0.11848(4) 0.0191(2) Uani 1 1 d . . . P1 P 0.51004(8) 0.27082(8) 0.13520(4) 0.0170(2) Uani 1 1 d . . . O1 O 0.2889(2) 0.1553(2) 0.05276(11) 0.0227(6) Uani 1 1 d . . . O2 O -0.2721(2) -0.0223(3) -0.18574(13) 0.0451(9) Uani 1 1 d . . . N1 N 0.4144(2) -0.0416(2) 0.04319(12) 0.0168(7) Uani 1 1 d . . . N2 N 0.4951(3) -0.1218(2) 0.05130(13) 0.0189(7) Uani 1 1 d . . . N3 N 0.1077(2) 0.1507(3) -0.00811(14) 0.0236(8) Uani 1 1 d . . . H3N H 0.1023 0.2139 0.0104 0.035 Uiso 1 1 d R . . N4 N 0.6819(3) -0.1574(3) 0.09783(14) 0.0222(8) Uani 1 1 d . . . H4N H 0.7437 -0.1303 0.1270 0.033 Uiso 1 1 d R . . C1 C 0.3160(3) -0.0710(3) 0.00731(16) 0.0199(9) Uani 1 1 d . . . H1 H 0.3085 -0.1437 -0.0088 0.024 Uiso 1 1 calc R . . C2 C 0.2152(3) -0.0053(3) -0.01125(16) 0.0198(9) Uani 1 1 d . . . C3 C 0.2093(3) 0.1027(3) 0.01308(16) 0.0202(9) Uani 1 1 d . . . C4 C 0.0131(3) 0.1071(3) -0.05284(17) 0.0258(10) Uani 1 1 d . . . C5 C 0.0183(3) 0.0046(3) -0.07611(17) 0.0236(10) Uani 1 1 d . . . C6 C 0.1214(3) -0.0502(3) -0.05382(17) 0.0244(9) Uani 1 1 d . . . H6 H 0.1258 -0.1217 -0.0691 0.029 Uiso 1 1 calc R . . C7 C -0.0883(4) 0.1674(4) -0.07394(19) 0.0366(11) Uani 1 1 d . . . H7 H -0.0930 0.2384 -0.0581 0.044 Uiso 1 1 calc R . . C8 C -0.1792(3) 0.1195(4) -0.11804(19) 0.0383(12) Uani 1 1 d . . . H8 H -0.2475 0.1588 -0.1330 0.046 Uiso 1 1 calc R . . C9 C -0.1743(3) 0.0143(4) -0.14168(18) 0.0339(11) Uani 1 1 d . . . C10 C -0.0777(3) -0.0423(4) -0.12130(17) 0.0309(11) Uani 1 1 d . . . H10 H -0.0741 -0.1135 -0.1372 0.037 Uiso 1 1 calc R . . C11 C -0.2653(4) -0.1269(4) -0.2117(2) 0.0578(16) Uani 1 1 d . . . H11A H -0.2083 -0.1236 -0.2284 0.087 Uiso 1 1 calc R . . H11B H -0.3371 -0.1445 -0.2440 0.087 Uiso 1 1 calc R . . H11C H -0.2459 -0.1843 -0.1805 0.087 Uiso 1 1 calc R . . C12 C 0.5948(3) -0.0882(3) 0.08591(16) 0.0174(9) Uani 1 1 d . . . C13 C 0.6680(3) -0.2703(3) 0.07592(19) 0.0315(11) Uani 1 1 d . . . H13A H 0.6374 -0.2702 0.0312 0.038 Uiso 1 1 calc R . . H13B H 0.6147 -0.3092 0.0890 0.038 Uiso 1 1 calc R . . C14 C 0.7772(4) -0.3304(4) 0.0998(2) 0.0552(14) Uani 1 1 d . . . H14A H 0.8285 -0.2943 0.0849 0.083 Uiso 1 1 calc R . . H14B H 0.7658 -0.4074 0.0859 0.083 Uiso 1 1 calc R . . H14C H 0.8085 -0.3286 0.1441 0.083 Uiso 1 1 calc R . . C15 C 0.4241(3) 0.3890(3) 0.09908(16) 0.0198(9) Uani 1 1 d . . . C16 C 0.4641(3) 0.4741(3) 0.07422(16) 0.0234(9) Uani 1 1 d . . . H16 H 0.5384 0.4717 0.0770 0.028 Uiso 1 1 calc R . . C17 C 0.3960(3) 0.5625(3) 0.04531(16) 0.0291(10) Uani 1 1 d . . . H17 H 0.4236 0.6200 0.0281 0.035 Uiso 1 1 calc R . . C18 C 0.2882(4) 0.5667(4) 0.04163(18) 0.0312(11) Uani 1 1 d . . . H18 H 0.2424 0.6281 0.0228 0.037 Uiso 1 1 calc R . . C19 C 0.2470(3) 0.4817(3) 0.06524(18) 0.0293(10) Uani 1 1 d . . . H19 H 0.1725 0.4843 0.0621 0.035 Uiso 1 1 calc R . . C20 C 0.3138(3) 0.3930(3) 0.09332(17) 0.0244(10) Uani 1 1 d . . . H20 H 0.2846 0.3343 0.1089 0.029 Uiso 1 1 calc R . . C21 C 0.5110(3) 0.2622(3) 0.21061(15) 0.0171(9) Uani 1 1 d . . . C22 C 0.5565(3) 0.1689(3) 0.24472(16) 0.0249(10) Uani 1 1 d . . . H22 H 0.5792 0.1087 0.2269 0.030 Uiso 1 1 calc R . . C23 C 0.5693(3) 0.1622(3) 0.30481(17) 0.0285(10) Uani 1 1 d . . . H23 H 0.6018 0.0983 0.3281 0.034 Uiso 1 1 calc R . . C24 C 0.5346(3) 0.2490(3) 0.33037(17) 0.0228(9) Uani 1 1 d . . . H24 H 0.5414 0.2442 0.3711 0.027 Uiso 1 1 calc R . . C25 C 0.4900(3) 0.3422(3) 0.29698(18) 0.0300(10) Uani 1 1 d . . . H25 H 0.4672 0.4023 0.3149 0.036 Uiso 1 1 calc R . . C26 C 0.4783(3) 0.3489(3) 0.23788(17) 0.0268(10) Uani 1 1 d . . . H26 H 0.4475 0.4139 0.2152 0.032 Uiso 1 1 calc R . . C27 C 0.6509(3) 0.3129(3) 0.14873(16) 0.0177(9) Uani 1 1 d . . . C28 C 0.6892(3) 0.3006(3) 0.10271(17) 0.0204(9) Uani 1 1 d . . . H28 H 0.6418 0.2700 0.0650 0.025 Uiso 1 1 calc R . . C29 C 0.7958(3) 0.3327(3) 0.11147(18) 0.0262(10) Uani 1 1 d . . . H29 H 0.8213 0.3249 0.0798 0.031 Uiso 1 1 calc R . . C30 C 0.8644(4) 0.3759(4) 0.1664(2) 0.0380(12) Uani 1 1 d . . . H30 H 0.9377 0.3978 0.1726 0.046 Uiso 1 1 calc R . . C31 C 0.8280(4) 0.3877(4) 0.2122(2) 0.0434(13) Uani 1 1 d . . . H31 H 0.8763 0.4170 0.2500 0.052 Uiso 1 1 calc R . . C32 C 0.7214(3) 0.3572(4) 0.20348(19) 0.0337(11) Uani 1 1 d . . . H32 H 0.6962 0.3667 0.2352 0.040 Uiso 1 1 calc R . . O75 O 0.8859(3) -0.0783(5) 0.1877(2) 0.121(2) Uani 1 1 d . . . N70 N 0.8765(3) 0.0264(4) 0.26312(19) 0.0558(12) Uani 1 1 d . . . C71 C 0.8953(7) 0.1206(7) 0.3026(4) 0.147(4) Uani 1 1 d . . . H71A H 0.9311 0.0963 0.3447 0.220 Uiso 1 1 calc R . . H71B H 0.8241 0.1557 0.2961 0.220 Uiso 1 1 calc R . . H71C H 0.9433 0.1738 0.2938 0.220 Uiso 1 1 calc R . . C72 C 0.8181(5) -0.0620(7) 0.2775(3) 0.118(3) Uani 1 1 d . . . H72A H 0.8152 -0.1263 0.2522 0.177 Uiso 1 1 calc R . . H72B H 0.7424 -0.0379 0.2700 0.177 Uiso 1 1 calc R . . H72C H 0.8566 -0.0820 0.3202 0.177 Uiso 1 1 calc R . . C73 C 0.9074(5) 0.0228(8) 0.2167(3) 0.098(3) Uani 1 1 d . . . H73A H 0.9417 0.0932 0.2205 0.147 Uiso 1 1 d R . . O90 O 0.9858(4) 0.5746(5) 0.0594(2) 0.0452(15) Uani 0.56 1 d P . . H90 H 0.9854 0.5059 0.0669 0.068 Uiso 0.56 1 d PR . . H91 H 0.9663 0.5896 0.0221 0.068 Uiso 0.56 1 d PR . . 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 0.01307(18) 0.01857(17) 0.01530(18) -0.00136(12) 0.00511(13) 0.00030(12) Cl1 0.0367(7) 0.0342(6) 0.0633(8) -0.0025(6) 0.0335(6) 0.0013(5) S1 0.0151(5) 0.0212(5) 0.0199(5) -0.0008(4) 0.0057(4) 0.0006(4) P1 0.0153(6) 0.0197(5) 0.0170(5) -0.0020(4) 0.0074(4) -0.0005(4) O1 0.0155(15) 0.0238(14) 0.0254(15) -0.0067(12) 0.0042(12) -0.0007(13) O2 0.0211(18) 0.066(2) 0.0362(18) 0.0172(17) -0.0018(15) -0.0116(16) N1 0.0144(18) 0.0211(18) 0.0164(18) 0.0030(14) 0.0076(14) 0.0023(15) N2 0.019(2) 0.0189(18) 0.0185(18) -0.0001(14) 0.0074(15) 0.0017(15) N3 0.0155(19) 0.0258(18) 0.0270(19) -0.0004(15) 0.0054(16) 0.0027(16) N4 0.0185(19) 0.0204(18) 0.0261(19) -0.0007(15) 0.0071(15) 0.0023(16) C1 0.018(2) 0.020(2) 0.020(2) -0.0011(17) 0.0053(18) -0.0035(19) C2 0.017(2) 0.026(2) 0.015(2) 0.0021(17) 0.0059(17) -0.0031(19) C3 0.018(2) 0.025(2) 0.019(2) 0.0046(18) 0.0093(19) -0.0001(19) C4 0.014(2) 0.041(3) 0.021(2) 0.014(2) 0.0047(18) -0.002(2) C5 0.020(2) 0.025(2) 0.023(2) 0.0094(19) 0.0055(19) -0.0033(19) C6 0.018(2) 0.027(2) 0.026(2) 0.0018(19) 0.0050(19) -0.005(2) C7 0.029(3) 0.045(3) 0.036(3) 0.011(2) 0.013(2) 0.011(2) C8 0.007(2) 0.068(4) 0.031(3) 0.021(2) -0.002(2) 0.004(2) C9 0.014(3) 0.052(3) 0.026(3) 0.013(2) -0.001(2) -0.013(2) C10 0.023(3) 0.037(3) 0.028(2) 0.006(2) 0.004(2) -0.009(2) C11 0.037(3) 0.060(4) 0.053(3) -0.006(3) -0.007(3) -0.027(3) C12 0.022(2) 0.018(2) 0.016(2) 0.0028(17) 0.0124(18) -0.0006(19) C13 0.031(3) 0.024(2) 0.041(3) 0.003(2) 0.016(2) 0.010(2) C14 0.052(3) 0.038(3) 0.082(4) 0.010(3) 0.033(3) 0.018(3) C15 0.022(2) 0.021(2) 0.014(2) -0.0047(17) 0.0043(17) -0.0011(18) C16 0.022(2) 0.026(2) 0.021(2) 0.0005(18) 0.0079(19) 0.0008(19) C17 0.033(3) 0.034(3) 0.017(2) 0.0056(19) 0.0064(19) 0.002(2) C18 0.032(3) 0.027(2) 0.026(2) 0.003(2) 0.002(2) 0.010(2) C19 0.019(2) 0.032(3) 0.035(3) -0.005(2) 0.009(2) 0.001(2) C20 0.026(2) 0.024(2) 0.023(2) 0.0014(18) 0.0087(19) 0.002(2) C21 0.012(2) 0.022(2) 0.016(2) -0.0003(17) 0.0039(16) -0.0055(18) C22 0.030(3) 0.026(2) 0.019(2) -0.0066(19) 0.0111(19) 0.005(2) C23 0.034(3) 0.022(2) 0.025(3) 0.0032(19) 0.007(2) 0.004(2) C24 0.027(2) 0.029(2) 0.014(2) -0.0014(18) 0.0103(18) -0.008(2) C25 0.043(3) 0.028(2) 0.024(3) -0.001(2) 0.019(2) 0.008(2) C26 0.034(3) 0.022(2) 0.028(3) 0.0009(19) 0.016(2) 0.004(2) C27 0.016(2) 0.016(2) 0.020(2) 0.0001(17) 0.0065(17) -0.0002(17) C28 0.018(2) 0.020(2) 0.021(2) -0.0004(17) 0.0056(17) -0.0010(18) C29 0.022(2) 0.030(2) 0.031(2) 0.000(2) 0.015(2) 0.001(2) C30 0.023(3) 0.044(3) 0.050(3) -0.005(2) 0.018(2) -0.012(2) C31 0.023(3) 0.068(4) 0.036(3) -0.019(2) 0.008(2) -0.020(2) C32 0.027(3) 0.047(3) 0.031(3) -0.013(2) 0.016(2) -0.008(2) O75 0.043(3) 0.191(6) 0.094(4) -0.066(4) -0.010(2) 0.028(3) N70 0.029(2) 0.078(3) 0.052(3) 0.009(3) 0.007(2) 0.007(2) C71 0.109(7) 0.143(8) 0.125(7) -0.071(6) -0.022(5) 0.058(6) C72 0.056(4) 0.154(7) 0.109(6) 0.066(6) -0.005(4) -0.020(5) C73 0.029(4) 0.199(10) 0.057(5) 0.044(5) 0.008(3) 0.030(5) O90 0.045(4) 0.041(3) 0.048(4) 0.001(3) 0.017(3) 0.008(3) _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 N1 2.031(3) . ? Pd1 O1 2.063(2) . ? Pd1 S1 2.2352(10) . ? Pd1 P1 2.2775(10) . ? S1 C12 1.768(4) . ? P1 C21 1.813(4) . ? P1 C27 1.816(4) . ? P1 C15 1.815(4) . ? O1 C3 1.273(4) . ? O2 C9 1.377(5) . ? O2 C11 1.427(6) . ? N1 C1 1.288(4) . ? N1 N2 1.391(4) . ? N2 C12 1.307(5) . ? N3 C3 1.356(5) . ? N3 C4 1.387(5) . ? N3 H3N 0.9000 . ? N4 C12 1.352(5) . ? N4 C13 1.448(5) . ? N4 H4N 0.8999 . ? C1 C2 1.452(5) . ? C1 H1 0.9500 . ? C2 C6 1.366(5) . ? C2 C3 1.445(5) . ? C4 C5 1.372(5) . ? C4 C7 1.423(6) . ? C5 C6 1.407(5) . ? C5 C10 1.419(5) . ? C6 H6 0.9500 . ? C7 C8 1.373(6) . ? C7 H7 0.9500 . ? C8 C9 1.404(6) . ? C8 H8 0.9500 . ? C9 C10 1.350(6) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.502(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.391(5) . ? C15 C20 1.398(6) . ? C16 C17 1.391(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(6) . ? C17 H17 0.9500 . ? C18 C19 1.383(6) . ? C18 H18 0.9500 . ? C19 C20 1.380(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 C26 1.390(5) . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.373(5) . ? C24 H24 0.9500 . ? C25 C26 1.372(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.385(5) . ? C27 C28 1.392(5) . ? C28 C29 1.384(5) . ? C28 H28 0.9500 . ? C29 C30 1.376(6) . ? C29 H29 0.9500 . ? C30 C31 1.371(6) . ? C30 H30 0.9500 . ? C31 C32 1.379(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? O75 C73 1.379(9) . ? N70 C73 1.330(7) . ? N70 C72 1.433(7) . ? N70 C71 1.440(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9500 . ? O90 H90 0.8500 . ? O90 H91 0.8502 . ? 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 N1 Pd1 O1 92.25(11) . . ? N1 Pd1 S1 84.22(9) . . ? O1 Pd1 S1 175.88(7) . . ? N1 Pd1 P1 175.52(9) . . ? O1 Pd1 P1 91.93(7) . . ? S1 Pd1 P1 91.54(4) . . ? C12 S1 Pd1 96.51(13) . . ? C21 P1 C27 103.32(16) . . ? C21 P1 C15 106.44(17) . . ? C27 P1 C15 105.15(17) . . ? C21 P1 Pd1 111.22(12) . . ? C27 P1 Pd1 115.51(12) . . ? C15 P1 Pd1 114.23(12) . . ? C3 O1 Pd1 124.6(2) . . ? C9 O2 C11 115.0(4) . . ? C1 N1 N2 114.1(3) . . ? C1 N1 Pd1 124.5(3) . . ? N2 N1 Pd1 121.4(2) . . ? C12 N2 N1 112.8(3) . . ? C3 N3 C4 125.1(3) . . ? C3 N3 H3N 115.6 . . ? C4 N3 H3N 119.1 . . ? C12 N4 C13 122.1(3) . . ? C12 N4 H4N 111.6 . . ? C13 N4 H4N 124.9 . . ? N1 C1 C2 127.3(4) . . ? N1 C1 H1 116.4 . . ? C2 C1 H1 116.4 . . ? C6 C2 C3 119.1(4) . . ? C6 C2 C1 117.1(4) . . ? C3 C2 C1 123.7(3) . . ? O1 C3 N3 117.6(3) . . ? O1 C3 C2 126.6(3) . . ? N3 C3 C2 115.8(3) . . ? C5 C4 N3 119.1(4) . . ? C5 C4 C7 120.4(4) . . ? N3 C4 C7 120.4(4) . . ? C4 C5 C6 117.6(4) . . ? C4 C5 C10 120.1(4) . . ? C6 C5 C10 122.2(4) . . ? C2 C6 C5 123.1(4) . . ? C2 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? C8 C7 C4 117.7(4) . . ? C8 C7 H7 121.2 . . ? C4 C7 H7 121.2 . . ? C7 C8 C9 122.0(4) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 O2 124.9(4) . . ? C10 C9 C8 119.9(4) . . ? O2 C9 C8 115.2(4) . . ? C9 C10 C5 119.9(4) . . ? C9 C10 H10 120.1 . . ? C5 C10 H10 120.1 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 N4 119.5(3) . . ? N2 C12 S1 124.9(3) . . ? N4 C12 S1 115.5(3) . . ? N4 C13 C14 110.6(4) . . ? N4 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? 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 . . ? C16 C15 C20 118.8(4) . . ? C16 C15 P1 121.3(3) . . ? C20 C15 P1 119.8(3) . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 120.5(4) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C22 C21 C26 118.3(3) . . ? C22 C21 P1 118.2(3) . . ? C26 C21 P1 123.2(3) . . ? C21 C22 C23 120.7(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.0(4) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 118.9(4) . . ? C32 C27 P1 122.0(3) . . ? C28 C27 P1 119.1(3) . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 119.5(4) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.6(4) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 120.2(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 120.3(4) . . ? C31 C32 H32 119.9 . . ? C27 C32 H32 119.9 . . ? C73 N70 C72 123.2(7) . . ? C73 N70 C71 123.4(7) . . ? C72 N70 C71 113.4(6) . . ? N70 C71 H71A 109.5 . . ? N70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N70 C72 H72A 109.5 . . ? N70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N70 C73 O75 112.6(7) . . ? N70 C73 H73A 100.3 . . ? O75 C73 H73A 146.8 . . ? H90 O90 H91 114.1 . . ? 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 N1 Pd1 S1 C12 -2.48(14) . . . . ? O1 Pd1 S1 C12 28.5(10) . . . . ? P1 Pd1 S1 C12 176.09(12) . . . . ? N1 Pd1 P1 C21 -71.2(11) . . . . ? O1 Pd1 P1 C21 87.90(14) . . . . ? S1 Pd1 P1 C21 -89.89(13) . . . . ? N1 Pd1 P1 C27 46.1(11) . . . . ? O1 Pd1 P1 C27 -154.76(15) . . . . ? S1 Pd1 P1 C27 27.45(13) . . . . ? N1 Pd1 P1 C15 168.3(11) . . . . ? O1 Pd1 P1 C15 -32.61(16) . . . . ? S1 Pd1 P1 C15 149.60(14) . . . . ? N1 Pd1 O1 C3 -10.7(3) . . . . ? S1 Pd1 O1 C3 -41.5(11) . . . . ? P1 Pd1 O1 C3 170.9(3) . . . . ? O1 Pd1 N1 C1 6.1(3) . . . . ? S1 Pd1 N1 C1 -176.0(3) . . . . ? P1 Pd1 N1 C1 165.2(9) . . . . ? O1 Pd1 N1 N2 -175.1(2) . . . . ? S1 Pd1 N1 N2 2.8(2) . . . . ? P1 Pd1 N1 N2 -16.0(12) . . . . ? C1 N1 N2 C12 177.4(3) . . . . ? Pd1 N1 N2 C12 -1.6(4) . . . . ? N2 N1 C1 C2 -178.5(3) . . . . ? Pd1 N1 C1 C2 0.4(5) . . . . ? N1 C1 C2 C6 174.6(4) . . . . ? N1 C1 C2 C3 -5.9(6) . . . . ? Pd1 O1 C3 N3 -172.4(2) . . . . ? Pd1 O1 C3 C2 9.0(5) . . . . ? C4 N3 C3 O1 177.4(3) . . . . ? C4 N3 C3 C2 -3.9(5) . . . . ? C6 C2 C3 O1 180.0(3) . . . . ? C1 C2 C3 O1 0.5(6) . . . . ? C6 C2 C3 N3 1.4(5) . . . . ? C1 C2 C3 N3 -178.1(3) . . . . ? C3 N3 C4 C5 3.9(6) . . . . ? C3 N3 C4 C7 -176.7(4) . . . . ? N3 C4 C5 C6 -1.3(5) . . . . ? C7 C4 C5 C6 179.3(4) . . . . ? N3 C4 C5 C10 179.1(3) . . . . ? C7 C4 C5 C10 -0.3(6) . . . . ? C3 C2 C6 C5 0.9(6) . . . . ? C1 C2 C6 C5 -179.6(3) . . . . ? C4 C5 C6 C2 -1.0(6) . . . . ? C10 C5 C6 C2 178.6(4) . . . . ? C5 C4 C7 C8 -0.2(6) . . . . ? N3 C4 C7 C8 -179.6(4) . . . . ? C4 C7 C8 C9 0.6(6) . . . . ? C11 O2 C9 C10 -2.2(6) . . . . ? C11 O2 C9 C8 177.1(4) . . . . ? C7 C8 C9 C10 -0.5(6) . . . . ? C7 C8 C9 O2 -179.8(4) . . . . ? O2 C9 C10 C5 179.2(4) . . . . ? C8 C9 C10 C5 0.0(6) . . . . ? C4 C5 C10 C9 0.4(6) . . . . ? C6 C5 C10 C9 -179.2(4) . . . . ? N1 N2 C12 N4 -179.9(3) . . . . ? N1 N2 C12 S1 -1.3(4) . . . . ? C13 N4 C12 N2 -3.1(5) . . . . ? C13 N4 C12 S1 178.1(3) . . . . ? Pd1 S1 C12 N2 3.0(3) . . . . ? Pd1 S1 C12 N4 -178.3(2) . . . . ? C12 N4 C13 C14 -175.7(4) . . . . ? C21 P1 C15 C16 125.0(3) . . . . ? C27 P1 C15 C16 15.8(3) . . . . ? Pd1 P1 C15 C16 -111.8(3) . . . . ? C21 P1 C15 C20 -58.1(3) . . . . ? C27 P1 C15 C20 -167.3(3) . . . . ? Pd1 P1 C15 C20 65.1(3) . . . . ? C20 C15 C16 C17 1.3(6) . . . . ? P1 C15 C16 C17 178.3(3) . . . . ? C15 C16 C17 C18 0.5(6) . . . . ? C16 C17 C18 C19 -1.7(6) . . . . ? C17 C18 C19 C20 0.9(6) . . . . ? C18 C19 C20 C15 1.1(6) . . . . ? C16 C15 C20 C19 -2.2(6) . . . . ? P1 C15 C20 C19 -179.1(3) . . . . ? C27 P1 C21 C22 -79.4(3) . . . . ? C15 P1 C21 C22 170.1(3) . . . . ? Pd1 P1 C21 C22 45.1(3) . . . . ? C27 P1 C21 C26 94.1(3) . . . . ? C15 P1 C21 C26 -16.4(4) . . . . ? Pd1 P1 C21 C26 -141.4(3) . . . . ? C26 C21 C22 C23 -0.1(6) . . . . ? P1 C21 C22 C23 173.8(3) . . . . ? C21 C22 C23 C24 1.1(6) . . . . ? C22 C23 C24 C25 -1.5(6) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C24 C25 C26 C21 0.0(6) . . . . ? C22 C21 C26 C25 -0.5(6) . . . . ? P1 C21 C26 C25 -174.0(3) . . . . ? C21 P1 C27 C32 -16.6(4) . . . . ? C15 P1 C27 C32 94.9(3) . . . . ? Pd1 P1 C27 C32 -138.3(3) . . . . ? C21 P1 C27 C28 163.6(3) . . . . ? C15 P1 C27 C28 -84.9(3) . . . . ? Pd1 P1 C27 C28 41.9(3) . . . . ? C32 C27 C28 C29 -0.3(6) . . . . ? P1 C27 C28 C29 179.5(3) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C28 C29 C30 C31 -0.2(6) . . . . ? C29 C30 C31 C32 -0.6(7) . . . . ? C30 C31 C32 C27 1.0(7) . . . . ? C28 C27 C32 C31 -0.5(6) . . . . ? P1 C27 C32 C31 179.7(3) . . . . ? C72 N70 C73 O75 -5.5(7) . . . . ? C71 N70 C73 O75 176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.043 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.086 # Attachment '- complex 5.cif' data_pp6od _database_code_depnum_ccdc_archive 'CCDC 841993' #TrackingRef '- complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H29 N4 O2 P Pd S' _chemical_formula_weight 671.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8863(3) _cell_length_b 11.3723(4) _cell_length_c 13.9140(5) _cell_angle_alpha 101.755(2) _cell_angle_beta 105.532(2) _cell_angle_gamma 103.784(2) _cell_volume 1402.71(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 62.82 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 6.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7248 _exptl_absorpt_correction_T_max 0.8202 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31583 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4078 _reflns_number_gt 3696 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-SEED (Barbour, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.6997P] 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 4078 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.39072(2) 0.419734(17) 0.258564(14) 0.01311(7) Uani 1 1 d . . . P1 P 0.39717(7) 0.24782(6) 0.14381(5) 0.01362(15) Uani 1 1 d . . . S1 S 0.58151(7) 0.54878(6) 0.23552(5) 0.01717(15) Uani 1 1 d . . . C1 C 0.3610(3) 0.5579(2) 0.44969(19) 0.0146(6) Uani 1 1 d . . . H1A H 0.3986 0.6265 0.5115 0.018 Uiso 1 1 calc R . . C2 C 0.2369(3) 0.4559(2) 0.44294(19) 0.0138(5) Uani 1 1 d . . . C3 C 0.1569(3) 0.3456(2) 0.35309(19) 0.0144(6) Uani 1 1 d . . . C4 C -0.0178(3) 0.2818(2) 0.43176(19) 0.0152(6) Uani 1 1 d . . . C5 C 0.0622(3) 0.3793(2) 0.52637(19) 0.0139(5) Uani 1 1 d . . . C6 C 0.1884(3) 0.4675(2) 0.52744(19) 0.0147(6) Uani 1 1 d . . . H6A H 0.2419 0.5371 0.5877 0.018 Uiso 1 1 calc R . . C7 C -0.1524(3) 0.1969(2) 0.4253(2) 0.0185(6) Uani 1 1 d . . . H7A H -0.2102 0.1330 0.3619 0.022 Uiso 1 1 calc R . . C8 C -0.2000(3) 0.2057(2) 0.5091(2) 0.0197(6) Uani 1 1 d . . . H8A H -0.2910 0.1481 0.5031 0.024 Uiso 1 1 calc R . . C9 C -0.1161(3) 0.2990(2) 0.6046(2) 0.0169(6) Uani 1 1 d . . . C10 C 0.0113(3) 0.3857(2) 0.61332(19) 0.0158(6) Uani 1 1 d . . . H10A H 0.0660 0.4501 0.6769 0.019 Uiso 1 1 calc R . . C11 C -0.1021(3) 0.3857(3) 0.7790(2) 0.0272(7) Uani 1 1 d . . . H11A H -0.1561 0.3715 0.8274 0.041 Uiso 1 1 calc R . . H11B H -0.0967 0.4692 0.7688 0.041 Uiso 1 1 calc R . . H11C H -0.0021 0.3814 0.8078 0.041 Uiso 1 1 calc R . . C12 C 0.6157(3) 0.6786(2) 0.3432(2) 0.0160(6) Uani 1 1 d . . . C13 C 0.8026(3) 0.8080(3) 0.2883(2) 0.0251(7) Uani 1 1 d . . . H13A H 0.7673 0.7334 0.2277 0.038 Uiso 1 1 calc R . . H13B H 0.9102 0.8309 0.3193 0.038 Uiso 1 1 calc R . . H13C H 0.7767 0.8786 0.2663 0.038 Uiso 1 1 calc R . . C14 C 0.7853(3) 0.8780(3) 0.4631(2) 0.0235(6) Uani 1 1 d . . . H14A H 0.7725 0.8397 0.5184 0.035 Uiso 1 1 calc R . . H14B H 0.7280 0.9373 0.4573 0.035 Uiso 1 1 calc R . . H14C H 0.8900 0.9234 0.4798 0.035 Uiso 1 1 calc R . . C15 C 0.4199(3) 0.1256(2) 0.20861(19) 0.0147(5) Uani 1 1 d . . . C16 C 0.4462(3) 0.0169(3) 0.1603(2) 0.0232(6) Uani 1 1 d . . . H16A H 0.4556 0.0070 0.0931 0.028 Uiso 1 1 calc R . . C17 C 0.4586(3) -0.0763(3) 0.2093(2) 0.0265(7) Uani 1 1 d . . . H17A H 0.4767 -0.1496 0.1755 0.032 Uiso 1 1 calc R . . C18 C 0.4451(3) -0.0637(3) 0.3070(2) 0.0242(6) Uani 1 1 d . . . H18A H 0.4518 -0.1285 0.3400 0.029 Uiso 1 1 calc R . . C19 C 0.4216(3) 0.0445(3) 0.3559(2) 0.0236(6) Uani 1 1 d . . . H19A H 0.4139 0.0546 0.4236 0.028 Uiso 1 1 calc R . . C20 C 0.4092(3) 0.1386(2) 0.3075(2) 0.0169(6) Uani 1 1 d . . . H20A H 0.3933 0.2125 0.3423 0.020 Uiso 1 1 calc R . . C21 C 0.5546(3) 0.2820(2) 0.09775(19) 0.0149(5) Uani 1 1 d . . . C22 C 0.5469(3) 0.3395(2) 0.01817(19) 0.0170(6) Uani 1 1 d . . . H22A H 0.4565 0.3509 -0.0172 0.020 Uiso 1 1 calc R . . C23 C 0.6711(3) 0.3805(3) -0.0096(2) 0.0203(6) Uani 1 1 d . . . H23A H 0.6659 0.4204 -0.0636 0.024 Uiso 1 1 calc R . . C24 C 0.8030(3) 0.3632(3) 0.0416(2) 0.0214(6) Uani 1 1 d . . . H24A H 0.8877 0.3908 0.0222 0.026 Uiso 1 1 calc R . . C25 C 0.8114(3) 0.3059(3) 0.1205(2) 0.0210(6) Uani 1 1 d . . . H25A H 0.9015 0.2935 0.1550 0.025 Uiso 1 1 calc R . . C26 C 0.6885(3) 0.2665(2) 0.1493(2) 0.0186(6) Uani 1 1 d . . . H26A H 0.6951 0.2286 0.2046 0.022 Uiso 1 1 calc R . . C27 C 0.2363(3) 0.1708(2) 0.02710(19) 0.0156(6) Uani 1 1 d . . . C28 C 0.1078(3) 0.2025(3) 0.0206(2) 0.0245(6) Uani 1 1 d . . . H28A H 0.1062 0.2682 0.0744 0.029 Uiso 1 1 calc R . . C29 C -0.0186(3) 0.1380(3) -0.0649(2) 0.0313(7) Uani 1 1 d . . . H29A H -0.1062 0.1606 -0.0699 0.038 Uiso 1 1 calc R . . C30 C -0.0179(3) 0.0414(3) -0.1423(2) 0.0281(7) Uani 1 1 d . . . H30A H -0.1053 -0.0030 -0.2000 0.034 Uiso 1 1 calc R . . C31 C 0.1091(3) 0.0088(3) -0.1365(2) 0.0249(7) Uani 1 1 d . . . H31A H 0.1091 -0.0583 -0.1899 0.030 Uiso 1 1 calc R . . C32 C 0.2358(3) 0.0737(3) -0.0530(2) 0.0220(6) Uani 1 1 d . . . H32A H 0.3238 0.0524 -0.0498 0.026 Uiso 1 1 calc R . . N1 N 0.4272(2) 0.56745(19) 0.38174(16) 0.0138(5) Uani 1 1 d . . . N2 N 0.5374(2) 0.67991(19) 0.40601(16) 0.0161(5) Uani 1 1 d . . . N3 N 0.0305(2) 0.26603(19) 0.34803(16) 0.0164(5) Uani 1 1 d . . . N4 N 0.7339(2) 0.7797(2) 0.36474(17) 0.0197(5) Uani 1 1 d . . . O1 O 0.20054(19) 0.31909(16) 0.27312(13) 0.0183(4) Uani 1 1 d . . . O2 O -0.1769(2) 0.29135(17) 0.68191(14) 0.0226(4) 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 0.01367(11) 0.01170(11) 0.01345(11) 0.00283(7) 0.00530(8) 0.00278(8) P1 0.0137(3) 0.0142(3) 0.0124(3) 0.0027(3) 0.0052(3) 0.0034(3) S1 0.0178(3) 0.0166(3) 0.0176(3) 0.0052(3) 0.0081(3) 0.0034(3) C1 0.0153(14) 0.0128(13) 0.0144(13) 0.0029(10) 0.0031(11) 0.0050(12) C2 0.0119(13) 0.0138(13) 0.0169(13) 0.0059(11) 0.0036(10) 0.0061(11) C3 0.0155(14) 0.0129(13) 0.0154(13) 0.0045(10) 0.0045(11) 0.0058(12) C4 0.0159(14) 0.0135(13) 0.0176(14) 0.0052(11) 0.0053(11) 0.0065(12) C5 0.0137(14) 0.0115(12) 0.0183(13) 0.0071(11) 0.0046(11) 0.0053(12) C6 0.0135(14) 0.0143(13) 0.0147(13) 0.0040(10) 0.0006(10) 0.0064(12) C7 0.0197(15) 0.0117(13) 0.0203(14) 0.0014(11) 0.0061(11) 0.0015(12) C8 0.0158(14) 0.0153(13) 0.0279(15) 0.0077(12) 0.0084(12) 0.0020(12) C9 0.0170(14) 0.0177(14) 0.0212(14) 0.0100(11) 0.0099(11) 0.0072(13) C10 0.0185(15) 0.0149(13) 0.0146(13) 0.0040(11) 0.0051(11) 0.0068(13) C11 0.0284(17) 0.0328(16) 0.0221(15) 0.0070(13) 0.0145(13) 0.0063(15) C12 0.0149(14) 0.0149(13) 0.0194(14) 0.0095(11) 0.0035(11) 0.0055(12) C13 0.0236(16) 0.0247(15) 0.0339(17) 0.0166(13) 0.0160(13) 0.0055(14) C14 0.0177(15) 0.0156(14) 0.0318(16) 0.0033(12) 0.0083(12) -0.0016(13) C15 0.0096(13) 0.0144(13) 0.0168(13) 0.0024(11) 0.0027(10) 0.0014(11) C16 0.0279(16) 0.0212(15) 0.0163(14) 0.0014(12) 0.0049(12) 0.0063(14) C17 0.0268(17) 0.0157(14) 0.0307(16) 0.0008(12) 0.0037(13) 0.0069(13) C18 0.0175(15) 0.0213(15) 0.0335(17) 0.0142(13) 0.0049(13) 0.0038(13) C19 0.0185(15) 0.0322(16) 0.0242(15) 0.0152(13) 0.0095(12) 0.0064(14) C20 0.0149(14) 0.0159(13) 0.0201(14) 0.0052(11) 0.0063(11) 0.0042(12) C21 0.0162(14) 0.0127(13) 0.0134(13) -0.0005(10) 0.0064(11) 0.0022(12) C22 0.0145(14) 0.0178(13) 0.0159(13) 0.0026(11) 0.0037(11) 0.0037(12) C23 0.0234(15) 0.0216(14) 0.0157(14) 0.0056(11) 0.0087(12) 0.0039(13) C24 0.0174(15) 0.0225(14) 0.0215(14) 0.0011(12) 0.0104(12) 0.0012(13) C25 0.0147(14) 0.0252(15) 0.0223(15) 0.0044(12) 0.0060(11) 0.0068(13) C26 0.0226(15) 0.0185(14) 0.0165(14) 0.0052(11) 0.0079(11) 0.0078(13) C27 0.0159(14) 0.0169(13) 0.0144(13) 0.0059(11) 0.0065(11) 0.0031(12) C28 0.0204(15) 0.0308(16) 0.0205(15) 0.0042(13) 0.0068(12) 0.0077(14) C29 0.0155(15) 0.049(2) 0.0255(16) 0.0081(15) 0.0036(12) 0.0091(15) C30 0.0168(15) 0.0369(17) 0.0177(15) 0.0071(13) 0.0000(12) -0.0075(14) C31 0.0316(17) 0.0202(14) 0.0140(14) 0.0029(12) 0.0053(12) -0.0033(14) C32 0.0217(15) 0.0240(15) 0.0210(15) 0.0074(12) 0.0077(12) 0.0069(13) N1 0.0125(11) 0.0107(10) 0.0182(11) 0.0056(9) 0.0034(9) 0.0043(10) N2 0.0135(12) 0.0107(11) 0.0232(12) 0.0056(9) 0.0067(9) 0.0008(10) N3 0.0171(12) 0.0135(11) 0.0180(12) 0.0040(9) 0.0073(9) 0.0022(10) N4 0.0203(13) 0.0138(11) 0.0263(13) 0.0064(10) 0.0115(10) 0.0030(11) O1 0.0188(10) 0.0174(9) 0.0152(9) 0.0005(7) 0.0074(8) 0.0010(8) O2 0.0241(11) 0.0245(10) 0.0219(10) 0.0073(8) 0.0139(8) 0.0044(9) _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 N1 2.024(2) . ? Pd1 O1 2.0393(17) . ? Pd1 S1 2.2385(6) . ? Pd1 P1 2.2843(7) . ? P1 C27 1.818(3) . ? P1 C21 1.825(3) . ? P1 C15 1.830(3) . ? S1 C12 1.769(3) . ? C1 N1 1.294(3) . ? C1 C2 1.441(4) . ? C1 H1A 0.9500 . ? C2 C6 1.378(4) . ? C2 C3 1.456(4) . ? C3 O1 1.303(3) . ? C3 N3 1.332(3) . ? C4 N3 1.368(3) . ? C4 C7 1.414(4) . ? C4 C5 1.420(4) . ? C5 C6 1.397(4) . ? C5 C10 1.425(4) . ? C6 H6A 0.9500 . ? C7 C8 1.364(4) . ? C7 H7A 0.9500 . ? C8 C9 1.413(4) . ? C8 H8A 0.9500 . ? C9 C10 1.361(4) . ? C9 O2 1.373(3) . ? C10 H10A 0.9500 . ? C11 O2 1.421(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.314(3) . ? C12 N4 1.345(3) . ? C13 N4 1.456(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N4 1.454(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.389(4) . ? C15 C16 1.399(4) . ? C16 C17 1.384(4) . ? C16 H16A 0.9500 . ? C17 C18 1.384(4) . ? C17 H17A 0.9500 . ? C18 C19 1.383(4) . ? C18 H18A 0.9500 . ? C19 C20 1.388(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.391(4) . ? C21 C26 1.397(4) . ? C22 C23 1.390(4) . ? C22 H22A 0.9500 . ? C23 C24 1.389(4) . ? C23 H23A 0.9500 . ? C24 C25 1.381(4) . ? C24 H24A 0.9500 . ? C25 C26 1.383(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.387(4) . ? C27 C32 1.398(4) . ? C28 C29 1.387(4) . ? C28 H28A 0.9500 . ? C29 C30 1.376(4) . ? C29 H29A 0.9500 . ? C30 C31 1.378(4) . ? C30 H30A 0.9500 . ? C31 C32 1.377(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? N1 N2 1.378(3) . ? 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 N1 Pd1 O1 93.18(7) . . ? N1 Pd1 S1 83.95(6) . . ? O1 Pd1 S1 171.79(5) . . ? N1 Pd1 P1 166.81(6) . . ? O1 Pd1 P1 92.01(5) . . ? S1 Pd1 P1 92.45(2) . . ? C27 P1 C21 105.46(11) . . ? C27 P1 C15 105.71(11) . . ? C21 P1 C15 104.99(12) . . ? C27 P1 Pd1 117.11(9) . . ? C21 P1 Pd1 113.01(8) . . ? C15 P1 Pd1 109.65(8) . . ? C12 S1 Pd1 96.73(9) . . ? N1 C1 C2 127.8(2) . . ? N1 C1 H1A 116.1 . . ? C2 C1 H1A 116.1 . . ? C6 C2 C1 116.5(2) . . ? C6 C2 C3 118.3(2) . . ? C1 C2 C3 125.2(2) . . ? O1 C3 N3 115.9(2) . . ? O1 C3 C2 123.5(2) . . ? N3 C3 C2 120.5(2) . . ? N3 C4 C7 119.1(2) . . ? N3 C4 C5 123.0(2) . . ? C7 C4 C5 117.9(2) . . ? C6 C5 C4 116.5(2) . . ? C6 C5 C10 123.1(2) . . ? C4 C5 C10 120.4(2) . . ? C2 C6 C5 121.4(2) . . ? C2 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C8 C7 C4 120.7(2) . . ? C8 C7 H7A 119.7 . . ? C4 C7 H7A 119.7 . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 O2 126.2(2) . . ? C10 C9 C8 120.3(2) . . ? O2 C9 C8 113.5(2) . . ? C9 C10 C5 119.5(2) . . ? C9 C10 H10A 120.2 . . ? C5 C10 H10A 120.2 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 N4 118.2(2) . . ? N2 C12 S1 124.1(2) . . ? N4 C12 S1 117.57(19) . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.4(2) . . ? C20 C15 P1 120.1(2) . . ? C16 C15 P1 121.5(2) . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 119.0(3) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C18 C19 C20 120.8(3) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C15 120.5(3) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? C22 C21 C26 119.3(2) . . ? C22 C21 P1 119.0(2) . . ? C26 C21 P1 121.25(19) . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.5(2) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C28 C27 C32 119.1(2) . . ? C28 C27 P1 119.3(2) . . ? C32 C27 P1 121.4(2) . . ? C27 C28 C29 119.8(3) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.3(3) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C32 C31 C30 119.7(3) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C27 120.7(3) . . ? C31 C32 H32A 119.7 . . ? C27 C32 H32A 119.7 . . ? C1 N1 N2 115.2(2) . . ? C1 N1 Pd1 122.26(17) . . ? N2 N1 Pd1 122.03(15) . . ? C12 N2 N1 113.1(2) . . ? C3 N3 C4 119.6(2) . . ? C12 N4 C14 120.1(2) . . ? C12 N4 C13 123.4(2) . . ? C14 N4 C13 115.8(2) . . ? C3 O1 Pd1 125.40(15) . . ? C9 O2 C11 116.7(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 N1 Pd1 P1 C27 169.6(3) . . . . ? O1 Pd1 P1 C27 56.46(10) . . . . ? S1 Pd1 P1 C27 -116.64(9) . . . . ? N1 Pd1 P1 C21 -67.6(3) . . . . ? O1 Pd1 P1 C21 179.33(10) . . . . ? S1 Pd1 P1 C21 6.23(9) . . . . ? N1 Pd1 P1 C15 49.2(3) . . . . ? O1 Pd1 P1 C15 -63.92(10) . . . . ? S1 Pd1 P1 C15 122.98(9) . . . . ? N1 Pd1 S1 C12 0.27(10) . . . . ? O1 Pd1 S1 C12 70.2(4) . . . . ? P1 Pd1 S1 C12 -167.00(9) . . . . ? N1 C1 C2 C6 178.8(2) . . . . ? N1 C1 C2 C3 -3.8(4) . . . . ? C6 C2 C3 O1 -173.6(2) . . . . ? C1 C2 C3 O1 9.0(4) . . . . ? C6 C2 C3 N3 7.7(4) . . . . ? C1 C2 C3 N3 -169.7(2) . . . . ? N3 C4 C5 C6 5.8(4) . . . . ? C7 C4 C5 C6 -175.0(2) . . . . ? N3 C4 C5 C10 -175.7(2) . . . . ? C7 C4 C5 C10 3.4(4) . . . . ? C1 C2 C6 C5 175.0(2) . . . . ? C3 C2 C6 C5 -2.6(4) . . . . ? C4 C5 C6 C2 -3.7(4) . . . . ? C10 C5 C6 C2 177.9(2) . . . . ? N3 C4 C7 C8 176.5(2) . . . . ? C5 C4 C7 C8 -2.7(4) . . . . ? C4 C7 C8 C9 -0.4(4) . . . . ? C7 C8 C9 C10 2.9(4) . . . . ? C7 C8 C9 O2 -177.5(2) . . . . ? O2 C9 C10 C5 178.4(2) . . . . ? C8 C9 C10 C5 -2.1(4) . . . . ? C6 C5 C10 C9 177.3(2) . . . . ? C4 C5 C10 C9 -1.1(4) . . . . ? Pd1 S1 C12 N2 -1.3(2) . . . . ? Pd1 S1 C12 N4 175.20(19) . . . . ? C27 P1 C15 C20 -117.9(2) . . . . ? C21 P1 C15 C20 130.8(2) . . . . ? Pd1 P1 C15 C20 9.1(2) . . . . ? C27 P1 C15 C16 61.2(2) . . . . ? C21 P1 C15 C16 -50.0(2) . . . . ? Pd1 P1 C15 C16 -171.66(19) . . . . ? C20 C15 C16 C17 1.2(4) . . . . ? P1 C15 C16 C17 -178.0(2) . . . . ? C15 C16 C17 C18 0.1(4) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C17 C18 C19 C20 1.1(4) . . . . ? C18 C19 C20 C15 0.1(4) . . . . ? C16 C15 C20 C19 -1.3(4) . . . . ? P1 C15 C20 C19 178.0(2) . . . . ? C27 P1 C21 C22 48.3(2) . . . . ? C15 P1 C21 C22 159.7(2) . . . . ? Pd1 P1 C21 C22 -80.9(2) . . . . ? C27 P1 C21 C26 -140.0(2) . . . . ? C15 P1 C21 C26 -28.6(2) . . . . ? Pd1 P1 C21 C26 90.9(2) . . . . ? C26 C21 C22 C23 0.2(4) . . . . ? P1 C21 C22 C23 172.1(2) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C22 C23 C24 C25 -0.3(4) . . . . ? C23 C24 C25 C26 -0.5(4) . . . . ? C24 C25 C26 C21 1.2(4) . . . . ? C22 C21 C26 C25 -1.1(4) . . . . ? P1 C21 C26 C25 -172.8(2) . . . . ? C21 P1 C27 C28 -138.4(2) . . . . ? C15 P1 C27 C28 110.7(2) . . . . ? Pd1 P1 C27 C28 -11.8(2) . . . . ? C21 P1 C27 C32 46.3(2) . . . . ? C15 P1 C27 C32 -64.6(2) . . . . ? Pd1 P1 C27 C32 172.97(18) . . . . ? C32 C27 C28 C29 0.0(4) . . . . ? P1 C27 C28 C29 -175.4(2) . . . . ? C27 C28 C29 C30 1.0(4) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C30 C31 C32 C27 1.3(4) . . . . ? C28 C27 C32 C31 -1.1(4) . . . . ? P1 C27 C32 C31 174.1(2) . . . . ? C2 C1 N1 N2 176.0(2) . . . . ? C2 C1 N1 Pd1 -11.8(4) . . . . ? O1 Pd1 N1 C1 16.7(2) . . . . ? S1 Pd1 N1 C1 -171.0(2) . . . . ? P1 Pd1 N1 C1 -96.3(3) . . . . ? O1 Pd1 N1 N2 -171.65(18) . . . . ? S1 Pd1 N1 N2 0.63(17) . . . . ? P1 Pd1 N1 N2 75.4(3) . . . . ? N4 C12 N2 N1 -174.6(2) . . . . ? S1 C12 N2 N1 1.9(3) . . . . ? C1 N1 N2 C12 170.6(2) . . . . ? Pd1 N1 N2 C12 -1.6(3) . . . . ? O1 C3 N3 C4 175.3(2) . . . . ? C2 C3 N3 C4 -5.8(4) . . . . ? C7 C4 N3 C3 179.8(2) . . . . ? C5 C4 N3 C3 -1.0(4) . . . . ? N2 C12 N4 C14 9.1(4) . . . . ? S1 C12 N4 C14 -167.6(2) . . . . ? N2 C12 N4 C13 -161.0(2) . . . . ? S1 C12 N4 C13 22.3(3) . . . . ? N3 C3 O1 Pd1 -178.59(16) . . . . ? C2 C3 O1 Pd1 2.6(3) . . . . ? N1 Pd1 O1 C3 -12.7(2) . . . . ? S1 Pd1 O1 C3 -81.9(4) . . . . ? P1 Pd1 O1 C3 155.21(19) . . . . ? C10 C9 O2 C11 2.4(4) . . . . ? C8 C9 O2 C11 -177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.302 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.062