# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Samaresh Bhattacharya' _publ_contact_author_address ; Department of Chemistry Jadavpur University Inorganic Chemistry Section Kolkata 700032 INDIA ; _publ_contact_author_email 'SAMARESH B@YAHOO.COM' _publ_section_title ; Synthesis, structure, spectroscopic properties and cytotoxic effect of some thiosemicarbazone complexes of palladium ; loop_ _publ_author_name 'Samaresh Bhattacharya' 'Tanmay Chatterjee' 'Sushanta Dutta' 'Sarmistha Halder' 'Gene-Hsiang Lee' ; A.Mukherjee ; 'Shie-Ming Peng' 'Utpal Sanyal' # Attachment 'B707448D_skd251_gm-final.cif' data_skd251 _database_code_depnum_ccdc_archive 'CCDC 646551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H16 N4 O Pd S' _chemical_formula_sum 'C15 H16 N4 O Pd S' _chemical_formula_weight 406.78 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' 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.3942(12) _cell_length_b 15.149(2) _cell_length_c 25.099(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3191.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8070 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 25.95 _exptl_crystal_description Block _exptl_crystal_colour 'Orange Yellow' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5743 _exptl_absorpt_correction_T_max 0.8596 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30751 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.98 _reflns_number_total 3135 _reflns_number_gt 2843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0322P)^2^+1.2869P] 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 3135 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.378571(18) 0.584078(10) 0.402267(6) 0.03983(7) Uani 1 1 d . . . S1 S 0.33435(9) 0.72717(4) 0.42138(2) 0.05890(16) Uani 1 1 d . . . N1 N 0.3564(2) 0.85179(12) 0.34811(9) 0.0579(5) Uani 1 1 d . . . H1N H 0.3805 0.8736 0.3175 0.077(9) Uiso 1 1 calc R . . H2N H 0.3189 0.8854 0.3727 0.114(12) Uiso 1 1 calc R . . N2 N 0.4347(2) 0.71645(11) 0.31931(7) 0.0457(4) Uani 1 1 d . . . N3 N 0.46605(18) 0.62918(10) 0.33397(6) 0.0395(3) Uani 1 1 d . . . N4 N 0.2841(2) 0.53703(11) 0.47295(7) 0.0474(4) Uani 1 1 d . . . O1 O 0.41202(19) 0.45893(9) 0.37975(7) 0.0547(4) Uani 1 1 d . . . C1 C 0.5273(2) 0.43573(13) 0.34675(8) 0.0454(5) Uani 1 1 d . . . C2 C 0.5822(3) 0.34834(15) 0.35072(10) 0.0579(6) Uani 1 1 d . . . H2 H 0.5353 0.3106 0.3754 0.068(7) Uiso 1 1 calc R . . C3 C 0.7030(3) 0.31744(16) 0.31928(11) 0.0636(6) Uani 1 1 d . . . H3 H 0.7387 0.2597 0.3232 0.078(8) Uiso 1 1 calc R . . C4 C 0.7719(3) 0.37211(16) 0.28160(10) 0.0599(6) Uani 1 1 d . . . H4 H 0.8551 0.3516 0.2605 0.079(9) Uiso 1 1 calc R . . C5 C 0.7171(3) 0.45616(15) 0.27572(9) 0.0512(5) Uani 1 1 d . . . H5 H 0.7631 0.4917 0.2497 0.055(6) Uiso 1 1 calc R . . C6 C 0.5932(2) 0.49208(14) 0.30739(8) 0.0428(4) Uani 1 1 d . . . C7 C 0.5437(2) 0.58299(12) 0.29834(8) 0.0409(4) Uani 1 1 d . . . C8 C 0.3779(2) 0.76424(13) 0.35757(9) 0.0450(5) Uani 1 1 d . . . C9 C 0.5865(3) 0.62602(16) 0.24618(9) 0.0543(5) Uani 1 1 d . . . H9A H 0.5088 0.6703 0.2377 0.072(8) Uiso 1 1 calc R . . H9B H 0.5884 0.5822 0.2185 0.096(11) Uiso 1 1 calc R . . H9C H 0.6897 0.6529 0.2491 0.077(8) Uiso 1 1 calc R . . C10 C 0.1922(3) 0.58498(15) 0.50567(10) 0.0581(6) Uani 1 1 d . . . H10 H 0.1714 0.6434 0.4967 0.057(6) Uiso 1 1 calc R . . C11 C 0.1274(3) 0.55215(18) 0.55180(10) 0.0610(6) Uani 1 1 d . . . H11 H 0.0653 0.5884 0.5733 0.081(9) Uiso 1 1 calc R . . C12 C 0.1541(3) 0.46578(17) 0.56632(9) 0.0555(6) Uani 1 1 d . . . C13 C 0.2502(3) 0.41682(15) 0.53306(10) 0.0611(6) Uani 1 1 d . . . H13 H 0.2733 0.3585 0.5416 0.064(7) Uiso 1 1 calc R . . C14 C 0.3122(3) 0.45345(15) 0.48735(9) 0.0568(5) Uani 1 1 d . . . H14 H 0.3763 0.4187 0.4656 0.068(9) Uiso 1 1 calc R . . C15 C 0.0810(4) 0.4269(2) 0.61537(12) 0.0727(8) Uani 1 1 d . . . H15A H 0.0002 0.3852 0.6054 0.101(11) Uiso 1 1 calc R . . H15B H 0.0341 0.4730 0.6364 0.19(2) Uiso 1 1 calc R . . H15C H 0.1617 0.3975 0.6358 0.127(14) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04169(11) 0.03560(10) 0.04222(11) -0.00580(6) 0.00393(6) -0.00100(6) S1 0.0864(4) 0.0396(3) 0.0507(3) -0.0060(2) 0.0117(3) 0.0075(3) N1 0.0716(13) 0.0381(10) 0.0639(12) 0.0025(9) 0.0051(10) 0.0057(9) N2 0.0485(9) 0.0390(8) 0.0497(9) -0.0012(7) 0.0003(8) -0.0023(7) N3 0.0371(8) 0.0376(8) 0.0436(8) -0.0040(7) -0.0012(7) -0.0039(7) N4 0.0493(10) 0.0456(9) 0.0472(9) -0.0043(7) 0.0044(8) 0.0001(8) O1 0.0634(9) 0.0362(7) 0.0646(10) -0.0095(7) 0.0230(8) -0.0068(7) C1 0.0439(11) 0.0422(10) 0.0500(11) -0.0123(9) 0.0030(9) -0.0031(8) C2 0.0650(13) 0.0451(12) 0.0636(14) -0.0038(11) 0.0082(12) 0.0027(11) C3 0.0652(15) 0.0523(13) 0.0734(16) -0.0103(12) 0.0018(13) 0.0149(11) C4 0.0513(12) 0.0624(14) 0.0661(14) -0.0177(12) 0.0070(11) 0.0093(11) C5 0.0447(11) 0.0579(13) 0.0511(12) -0.0132(10) 0.0057(9) -0.0033(10) C6 0.0388(10) 0.0453(11) 0.0443(10) -0.0137(9) -0.0021(8) -0.0044(8) C7 0.0346(10) 0.0457(11) 0.0424(10) -0.0082(8) -0.0005(8) -0.0078(8) C8 0.0423(11) 0.0390(11) 0.0538(12) -0.0039(9) -0.0034(8) -0.0018(8) C9 0.0622(13) 0.0554(13) 0.0454(11) -0.0046(10) 0.0069(10) -0.0034(11) C10 0.0711(16) 0.0476(13) 0.0555(13) -0.0054(10) 0.0140(12) 0.0022(11) C11 0.0690(16) 0.0631(15) 0.0510(13) -0.0091(12) 0.0139(11) -0.0027(12) C12 0.0543(12) 0.0693(15) 0.0429(12) -0.0012(10) -0.0063(10) -0.0125(11) C13 0.0693(15) 0.0554(14) 0.0588(14) 0.0087(11) -0.0012(12) 0.0016(11) C14 0.0633(14) 0.0511(13) 0.0560(13) -0.0007(10) 0.0070(11) 0.0082(11) C15 0.0795(18) 0.089(2) 0.0493(14) 0.0113(14) -0.0060(14) -0.0216(16) _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 N3 1.9862(16) . ? Pd1 O1 1.9981(14) . ? Pd1 N4 2.0700(17) . ? Pd1 S1 2.2510(6) . ? S1 C8 1.736(2) . ? N1 C8 1.359(3) . ? N1 H1N 0.8600 . ? N1 H2N 0.8600 . ? N2 C8 1.294(3) . ? N2 N3 1.397(2) . ? N3 C7 1.309(2) . ? N4 C14 1.338(3) . ? N4 C10 1.340(3) . ? O1 C1 1.322(2) . ? C1 C2 1.405(3) . ? C1 C6 1.418(3) . ? C2 C3 1.367(3) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.362(3) . ? C4 H4 0.9300 . ? C5 C6 1.417(3) . ? C5 H5 0.9300 . ? C6 C7 1.456(3) . ? C7 C9 1.506(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.372(3) . ? C10 H10 0.9300 . ? C11 C12 1.377(4) . ? C11 H11 0.9300 . ? C12 C13 1.377(3) . ? C12 C15 1.497(4) . ? C13 C14 1.377(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd1 O1 91.74(6) . . ? N3 Pd1 N4 179.16(7) . . ? O1 Pd1 N4 88.25(6) . . ? N3 Pd1 S1 85.04(5) . . ? O1 Pd1 S1 175.69(5) . . ? N4 Pd1 S1 94.92(5) . . ? C8 S1 Pd1 94.60(7) . . ? C8 N1 H1N 120.0 . . ? C8 N1 H2N 120.0 . . ? H1N N1 H2N 120.0 . . ? C8 N2 N3 113.81(17) . . ? C7 N3 N2 114.82(16) . . ? C7 N3 Pd1 126.14(13) . . ? N2 N3 Pd1 118.88(12) . . ? C14 N4 C10 116.68(19) . . ? C14 N4 Pd1 119.32(15) . . ? C10 N4 Pd1 123.98(15) . . ? C1 O1 Pd1 122.18(13) . . ? O1 C1 C2 116.5(2) . . ? O1 C1 C6 124.22(19) . . ? C2 C1 C6 119.25(19) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 120.0(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 123.1(2) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 116.5(2) . . ? C5 C6 C7 119.0(2) . . ? C1 C6 C7 124.52(18) . . ? N3 C7 C6 122.75(18) . . ? N3 C7 C9 118.76(18) . . ? C6 C7 C9 118.49(18) . . ? N2 C8 N1 117.7(2) . . ? N2 C8 S1 125.54(16) . . ? N1 C8 S1 116.68(17) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 123.3(2) . . ? N4 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 116.5(2) . . ? C11 C12 C15 121.7(3) . . ? C13 C12 C15 121.8(3) . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? N4 C14 C13 122.7(2) . . ? N4 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.322 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.061 data_ic9862 _database_code_depnum_ccdc_archive 'CCDC 646552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 N3 O P Pd S' _chemical_formula_weight 561.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5385(4) _cell_length_b 10.2179(5) _cell_length_c 16.9756(9) _cell_angle_alpha 77.025(1) _cell_angle_beta 80.819(1) _cell_angle_gamma 71.567(1) _cell_volume 1203.27(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8008 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.41 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7145 _exptl_absorpt_correction_T_max 0.8708 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15972 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5525 _reflns_number_gt 5158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0419P)^2^+0.2009P] 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 SHELXL _refine_ls_extinction_coef 0.0178(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5525 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Pd Pd 0.41073(2) 0.723581(15) 0.324760(9) 0.03008(8) Uani 1 1 d . . . S1 S 0.28094(9) 0.95509(6) 0.31867(4) 0.03841(13) Uani 1 1 d . . . P1 P 0.26451(8) 0.72699(6) 0.21693(3) 0.03077(12) Uani 1 1 d . . . O1 O 0.5349(3) 0.51528(17) 0.33485(11) 0.0499(4) Uani 1 1 d . . . N1 N 0.3639(3) 1.1005(2) 0.41011(13) 0.0473(5) Uani 1 1 d . . . H1A H 0.4206 1.1145 0.4462 0.057 Uiso 1 1 calc R . . H1B H 0.2841 1.1698 0.3836 0.057 Uiso 1 1 calc R . . N2 N 0.5202(3) 0.86724(19) 0.43566(11) 0.0360(4) Uani 1 1 d . . . N3 N 0.5487(3) 0.73804(18) 0.41332(11) 0.0316(4) Uani 1 1 d . . . C1 C 0.6548(3) 0.4390(2) 0.38694(14) 0.0394(5) Uani 1 1 d . . . C2 C 0.7266(4) 0.2942(3) 0.38499(17) 0.0498(6) Uani 1 1 d . . . H2A H 0.6876 0.2586 0.3471 0.060 Uiso 1 1 calc R . . C3 C 0.8518(4) 0.2048(3) 0.43724(17) 0.0530(6) Uani 1 1 d . . . H3A H 0.8962 0.1100 0.4342 0.064 Uiso 1 1 calc R . . C4 C 0.9132(4) 0.2532(3) 0.49447(16) 0.0491(6) Uani 1 1 d . . . H4A H 0.9988 0.1921 0.5297 0.059 Uiso 1 1 calc R . . C5 C 0.8458(3) 0.3925(3) 0.49832(15) 0.0428(5) Uani 1 1 d . . . H5A H 0.8854 0.4250 0.5375 0.051 Uiso 1 1 calc R . . C6 C 0.7185(3) 0.4889(2) 0.44519(14) 0.0364(5) Uani 1 1 d . . . C7 C 0.6617(3) 0.6325(2) 0.45525(13) 0.0370(5) Uani 1 1 d . . . H7A H 0.7118 0.6516 0.4965 0.044 Uiso 1 1 calc R . . C8 C 0.4001(3) 0.9695(2) 0.39512(13) 0.0345(4) Uani 1 1 d . . . C9 C 0.1799(3) 0.5785(2) 0.21681(13) 0.0364(5) Uani 1 1 d . . . C10 C 0.3019(4) 0.4444(3) 0.23007(16) 0.0478(6) Uani 1 1 d . . . H10A H 0.4246 0.4305 0.2405 0.057 Uiso 1 1 calc R . . C11 C 0.2417(4) 0.3306(3) 0.22788(16) 0.0525(6) Uani 1 1 d . . . H11A H 0.3250 0.2405 0.2359 0.063 Uiso 1 1 calc R . . C12 C 0.0620(4) 0.3494(3) 0.21404(19) 0.0605(7) Uani 1 1 d . . . H12A H 0.0224 0.2723 0.2132 0.073 Uiso 1 1 calc R . . C13 C -0.0599(5) 0.4806(4) 0.2015(3) 0.0833(11) Uani 1 1 d . . . H13A H -0.1826 0.4933 0.1916 0.100 Uiso 1 1 calc R . . C14 C -0.0016(4) 0.5962(3) 0.2032(2) 0.0648(8) Uani 1 1 d . . . H14A H -0.0860 0.6858 0.1952 0.078 Uiso 1 1 calc R . . C15 C 0.4283(3) 0.7367(2) 0.12593(13) 0.0349(4) Uani 1 1 d . . . C16 C 0.4338(4) 0.6690(3) 0.06330(16) 0.0529(6) Uani 1 1 d . . . H16A H 0.3533 0.6146 0.0671 0.063 Uiso 1 1 calc R . . C17 C 0.5589(5) 0.6821(3) -0.00498(17) 0.0672(8) Uani 1 1 d . . . H17A H 0.5632 0.6356 -0.0468 0.081 Uiso 1 1 calc R . . C18 C 0.6767(5) 0.7635(4) -0.01144(19) 0.0715(9) Uani 1 1 d . . . H18A H 0.7606 0.7718 -0.0575 0.086 Uiso 1 1 calc R . . C19 C 0.6709(5) 0.8317(4) 0.04936(18) 0.0666(8) Uani 1 1 d . . . H19A H 0.7500 0.8873 0.0448 0.080 Uiso 1 1 calc R . . C20 C 0.5466(4) 0.8184(3) 0.11839(15) 0.0496(6) Uani 1 1 d . . . H20A H 0.5433 0.8652 0.1600 0.059 Uiso 1 1 calc R . . C21 C 0.0632(3) 0.8805(2) 0.19498(13) 0.0339(4) Uani 1 1 d . . . C22 C 0.0541(4) 0.9714(3) 0.12092(16) 0.0463(6) Uani 1 1 d . . . H22A H 0.1513 0.9534 0.0799 0.056 Uiso 1 1 calc R . . C23 C -0.0996(4) 1.0895(3) 0.10748(19) 0.0606(7) Uani 1 1 d . . . H23A H -0.1058 1.1497 0.0573 0.073 Uiso 1 1 calc R . . C24 C -0.2422(4) 1.1174(3) 0.1680(2) 0.0612(8) Uani 1 1 d . . . H24A H -0.3445 1.1971 0.1592 0.073 Uiso 1 1 calc R . . C25 C -0.2340(4) 1.0278(3) 0.24170(19) 0.0566(7) Uani 1 1 d . . . H25A H -0.3317 1.0464 0.2824 0.068 Uiso 1 1 calc R . . C26 C -0.0823(3) 0.9104(3) 0.25579(15) 0.0453(5) Uani 1 1 d . . . H26A H -0.0771 0.8509 0.3062 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03478(11) 0.02781(10) 0.02961(10) -0.00798(6) -0.00638(6) -0.00842(7) S1 0.0491(3) 0.0290(3) 0.0394(3) -0.0077(2) -0.0162(2) -0.0078(2) P1 0.0342(3) 0.0295(3) 0.0307(3) -0.0073(2) -0.0057(2) -0.0097(2) O1 0.0625(11) 0.0317(8) 0.0588(11) -0.0180(8) -0.0261(9) -0.0017(8) N1 0.0632(13) 0.0314(10) 0.0507(12) -0.0139(9) -0.0229(10) -0.0058(9) N2 0.0435(10) 0.0306(9) 0.0371(10) -0.0120(7) -0.0090(8) -0.0090(8) N3 0.0355(9) 0.0300(9) 0.0317(9) -0.0085(7) -0.0060(7) -0.0097(7) C1 0.0406(12) 0.0324(11) 0.0441(13) -0.0101(9) -0.0055(10) -0.0065(9) C2 0.0576(15) 0.0343(12) 0.0569(16) -0.0145(11) -0.0070(12) -0.0075(11) C3 0.0560(15) 0.0307(12) 0.0626(17) -0.0062(11) 0.0008(13) -0.0040(11) C4 0.0427(13) 0.0395(13) 0.0534(15) 0.0019(11) -0.0045(11) -0.0029(10) C5 0.0391(12) 0.0405(12) 0.0454(13) -0.0038(10) -0.0065(10) -0.0087(10) C6 0.0346(11) 0.0325(11) 0.0401(12) -0.0055(9) -0.0032(9) -0.0082(9) C7 0.0396(12) 0.0377(11) 0.0368(11) -0.0093(9) -0.0091(9) -0.0113(9) C8 0.0428(12) 0.0319(10) 0.0324(10) -0.0097(8) -0.0046(9) -0.0126(9) C9 0.0432(12) 0.0358(11) 0.0354(11) -0.0079(9) -0.0054(9) -0.0167(9) C10 0.0525(14) 0.0394(13) 0.0566(15) -0.0092(11) -0.0189(12) -0.0135(11) C11 0.0733(18) 0.0364(13) 0.0514(15) -0.0054(11) -0.0114(13) -0.0202(12) C12 0.0694(19) 0.0506(16) 0.0741(19) -0.0191(14) 0.0049(15) -0.0354(15) C13 0.0500(17) 0.069(2) 0.150(4) -0.037(2) -0.014(2) -0.0285(16) C14 0.0474(15) 0.0442(15) 0.110(3) -0.0200(16) -0.0234(16) -0.0113(12) C15 0.0357(11) 0.0351(11) 0.0316(10) -0.0075(8) -0.0044(8) -0.0056(9) C16 0.0724(18) 0.0498(14) 0.0420(13) -0.0163(11) -0.0003(12) -0.0226(13) C17 0.094(2) 0.0646(19) 0.0416(15) -0.0231(14) 0.0090(15) -0.0197(17) C18 0.067(2) 0.090(2) 0.0507(17) -0.0157(16) 0.0188(15) -0.0237(18) C19 0.0639(18) 0.096(2) 0.0510(16) -0.0142(16) 0.0049(14) -0.0432(18) C20 0.0486(14) 0.0683(17) 0.0403(13) -0.0142(12) -0.0013(11) -0.0273(13) C21 0.0342(10) 0.0327(10) 0.0383(11) -0.0098(9) -0.0086(9) -0.0098(8) C22 0.0441(13) 0.0462(13) 0.0426(13) -0.0041(10) -0.0051(10) -0.0071(11) C23 0.0564(16) 0.0508(16) 0.0615(18) 0.0043(13) -0.0155(14) -0.0025(13) C24 0.0421(14) 0.0494(16) 0.085(2) -0.0145(15) -0.0142(14) 0.0026(12) C25 0.0373(13) 0.0617(17) 0.0717(19) -0.0257(15) 0.0034(12) -0.0107(12) C26 0.0429(13) 0.0472(13) 0.0451(13) -0.0106(11) 0.0011(10) -0.0133(11) _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 Pd N3 2.0147(17) . ? Pd O1 2.0157(16) . ? Pd S1 2.2411(6) . ? Pd P1 2.2711(5) . ? S1 C8 1.748(2) . ? P1 C21 1.820(2) . ? P1 C15 1.822(2) . ? P1 C9 1.823(2) . ? O1 C1 1.306(3) . ? N1 C8 1.354(3) . ? N2 C8 1.289(3) . ? N2 N3 1.397(2) . ? N3 C7 1.290(3) . ? C1 C2 1.412(3) . ? C1 C6 1.415(3) . ? C2 C3 1.368(4) . ? C3 C4 1.381(4) . ? C4 C5 1.365(4) . ? C5 C6 1.409(3) . ? C6 C7 1.434(3) . ? C9 C14 1.372(3) . ? C9 C10 1.380(3) . ? C10 C11 1.385(3) . ? C11 C12 1.358(4) . ? C12 C13 1.357(4) . ? C13 C14 1.392(4) . ? C15 C20 1.377(3) . ? C15 C16 1.382(3) . ? C16 C17 1.383(4) . ? C17 C18 1.374(5) . ? C18 C19 1.357(4) . ? C19 C20 1.388(4) . ? C21 C22 1.383(3) . ? C21 C26 1.389(3) . ? C22 C23 1.388(4) . ? C23 C24 1.371(4) . ? C24 C25 1.372(4) . ? C25 C26 1.377(4) . ? 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 N3 Pd O1 92.82(7) . . ? N3 Pd S1 84.26(5) . . ? O1 Pd S1 177.07(5) . . ? N3 Pd P1 173.95(5) . . ? O1 Pd P1 91.19(5) . . ? S1 Pd P1 91.74(2) . . ? C8 S1 Pd 96.29(7) . . ? C21 P1 C15 104.48(10) . . ? C21 P1 C9 104.57(10) . . ? C15 P1 C9 105.09(10) . . ? C21 P1 Pd 114.39(7) . . ? C15 P1 Pd 108.41(7) . . ? C9 P1 Pd 118.66(8) . . ? C1 O1 Pd 125.30(14) . . ? C8 N2 N3 113.46(17) . . ? C7 N3 N2 114.99(18) . . ? C7 N3 Pd 124.29(15) . . ? N2 N3 Pd 120.67(13) . . ? O1 C1 C2 117.1(2) . . ? O1 C1 C6 125.6(2) . . ? C2 C1 C6 117.2(2) . . ? C3 C2 C1 121.9(2) . . ? C2 C3 C4 120.9(2) . . ? C5 C4 C3 118.7(2) . . ? C4 C5 C6 122.4(2) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C7 116.5(2) . . ? C1 C6 C7 124.7(2) . . ? N3 C7 C6 127.1(2) . . ? N2 C8 N1 118.9(2) . . ? N2 C8 S1 125.32(16) . . ? N1 C8 S1 115.75(17) . . ? C14 C9 C10 118.9(2) . . ? C14 C9 P1 121.88(19) . . ? C10 C9 P1 119.22(18) . . ? C9 C10 C11 120.1(2) . . ? C12 C11 C10 120.5(3) . . ? C13 C12 C11 120.1(3) . . ? C12 C13 C14 120.2(3) . . ? C9 C14 C13 120.3(3) . . ? C20 C15 C16 119.0(2) . . ? C20 C15 P1 118.55(17) . . ? C16 C15 P1 122.47(19) . . ? C15 C16 C17 119.9(3) . . ? C18 C17 C16 120.4(3) . . ? C19 C18 C17 120.0(3) . . ? C18 C19 C20 120.0(3) . . ? C15 C20 C19 120.7(3) . . ? C22 C21 C26 118.9(2) . . ? C22 C21 P1 122.12(18) . . ? C26 C21 P1 118.88(18) . . ? C21 C22 C23 120.3(2) . . ? C24 C23 C22 120.1(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.487 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.103