# 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 'Takumi Konno' _publ_contact_author_email konno@chem.sci.osaka-u.ac.jp loop_ _publ_author_name 'Yoshinari, Nobuto' 'Nagao, Yoshinori' 'Yokoi, Anzu' 'Igashira-Kamiyama, Asako' 'Takumi Konno' data_[1].H2O _database_code_depnum_ccdc_archive 'CCDC 891173' #TrackingRef '- konno.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H17 N3 O2 Pd S, H2 O' _chemical_formula_sum 'C7 H19 N3 O3 Pd S' _chemical_formula_weight 331.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.793(14) _cell_length_b 5.976(2) _cell_length_c 19.844(8) _cell_angle_alpha 90.00 _cell_angle_beta 123.240(16) _cell_angle_gamma 90.00 _cell_volume 2558(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10342 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 31.0 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12509 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5518 _reflns_number_gt 5068 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material ;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009) ; _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^)+(0.0274P)^2^+1.0796P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 2848 Friedel Pairs' _refine_ls_abs_structure_Flack -0.06(3) _refine_ls_number_reflns 5518 _refine_ls_number_parameters 288 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.398251(12) 0.33219(3) 0.689214(14) 0.02373(9) Uani 1 1 d . . . S1 S 0.45453(4) 0.45039(17) 0.64002(6) 0.0250(2) Uani 1 1 d . . . O1 O 0.23384(13) 0.4327(6) 0.42108(16) 0.0504(10) Uani 1 1 d . . . O2 O 0.28553(13) 0.3087(6) 0.36950(15) 0.0483(8) Uani 1 1 d . . . N1 N 0.32430(13) 0.3421(10) 0.57346(16) 0.0340(9) Uani 1 1 d . . . H1 H 0.2985 0.2243 0.5652 0.041 Uiso 1 1 calc R . . H2 H 0.3027 0.4721 0.5660 0.041 Uiso 1 1 calc R . . N2 N 0.47049(13) 0.3222(7) 0.80797(16) 0.0264(7) Uani 1 1 d . . . H3 H 0.4959 0.2023 0.8169 0.032 Uiso 1 1 calc R . . H4 H 0.4936 0.4512 0.8216 0.032 Uiso 1 1 calc R . . N3 N 0.34762(15) 0.2073(7) 0.73330(19) 0.0339(8) Uani 1 1 d . . . H5 H 0.3220 0.3168 0.7320 0.041 Uiso 1 1 calc R . . H6 H 0.3235 0.0894 0.7020 0.041 Uiso 1 1 calc R . . C1 C 0.39174(16) 0.4979(6) 0.5329(2) 0.0228(7) Uani 1 1 d . . . C2 C 0.33984(14) 0.3316(6) 0.51203(18) 0.0215(7) Uani 1 1 d . . . H7 H 0.3562 0.1781 0.5144 0.026 Uiso 1 1 calc R . . C3 C 0.28109(17) 0.3635(7) 0.42648(19) 0.0281(8) Uani 1 1 d . . . C4 C 0.41991(19) 0.4530(10) 0.4836(2) 0.0423(12) Uani 1 1 d . . . H8 H 0.3887 0.4807 0.4265 0.063 Uiso 1 1 calc R . . H9 H 0.4337 0.2969 0.4909 0.063 Uiso 1 1 calc R . . H10 H 0.4554 0.5525 0.5019 0.063 Uiso 1 1 calc R . . C5 C 0.36925(19) 0.7394(6) 0.5215(2) 0.0400(10) Uani 1 1 d . . . H11 H 0.4036 0.8411 0.5358 0.060 Uiso 1 1 calc R . . H12 H 0.3540 0.7691 0.5562 0.060 Uiso 1 1 calc R . . H13 H 0.3357 0.7633 0.4651 0.060 Uiso 1 1 calc R . . C6 C 0.44302(19) 0.2997(9) 0.8572(2) 0.0363(12) Uani 1 1 d . . . H14 H 0.4269 0.4462 0.8612 0.044 Uiso 1 1 calc R . . H15 H 0.4750 0.2489 0.9123 0.044 Uiso 1 1 calc R . . C7 C 0.3911(2) 0.1318(9) 0.8169(2) 0.0418(11) Uani 1 1 d . . . H16 H 0.4077 -0.0181 0.8174 0.050 Uiso 1 1 calc R . . H17 H 0.3697 0.1224 0.8457 0.050 Uiso 1 1 calc R . . Pd2 Pd 0.395796(12) 0.88226(4) 0.192929(14) 0.02278(9) Uani 1 1 d . . . S2 S 0.45341(4) 0.82425(18) 0.14032(5) 0.0246(2) Uani 1 1 d . . . O3 O 0.23398(14) 0.8925(7) -0.07398(18) 0.0689(12) Uani 1 1 d . . . O4 O 0.27304(13) 0.6660(7) -0.12138(16) 0.0556(10) Uani 1 1 d . . . N4 N 0.32082(14) 0.8166(9) 0.08016(17) 0.0347(11) Uani 1 1 d . . . H18 H 0.2971 0.7097 0.0844 0.042 Uiso 1 1 calc R . . H19 H 0.2973 0.9447 0.0606 0.042 Uiso 1 1 calc R . . N5 N 0.46884(15) 0.9386(6) 0.30840(17) 0.0260(8) Uani 1 1 d . . . H20 H 0.4992 0.8329 0.3229 0.031 Uiso 1 1 calc R . . H21 H 0.4855 1.0776 0.3121 0.031 Uiso 1 1 calc R . . N6 N 0.34308(15) 0.9415(7) 0.24148(18) 0.0323(8) Uani 1 1 d . . . H22 H 0.3108 1.0369 0.2088 0.039 Uiso 1 1 calc R . . H23 H 0.3269 0.8095 0.2461 0.039 Uiso 1 1 calc R . . C8 C 0.39080(14) 0.8581(7) 0.03195(18) 0.0213(7) Uani 1 1 d . . . C9 C 0.33402(15) 0.7387(6) 0.02014(19) 0.0215(7) Uani 1 1 d . . . H24 H 0.3436 0.5751 0.0292 0.026 Uiso 1 1 calc R . . C10 C 0.27503(18) 0.7686(7) -0.0663(2) 0.0297(9) Uani 1 1 d . . . C11 C 0.41414(18) 0.7494(8) -0.0159(2) 0.0319(10) Uani 1 1 d . . . H25 H 0.3835 0.7706 -0.0736 0.048 Uiso 1 1 calc R . . H26 H 0.4205 0.5890 -0.0037 0.048 Uiso 1 1 calc R . . H27 H 0.4535 0.8185 -0.0011 0.048 Uiso 1 1 calc R . . C12 C 0.37760(18) 1.1081(6) 0.0115(2) 0.0354(9) Uani 1 1 d . . . H28 H 0.4154 1.1828 0.0228 0.053 Uiso 1 1 calc R . . H29 H 0.3641 1.1756 0.0444 0.053 Uiso 1 1 calc R . . H30 H 0.3449 1.1254 -0.0457 0.053 Uiso 1 1 calc R . . C13 C 0.44664(19) 0.9260(9) 0.3623(2) 0.0360(12) Uani 1 1 d . . . H31 H 0.4768 0.9983 0.4144 0.043 Uiso 1 1 calc R . . H32 H 0.4419 0.7677 0.3727 0.043 Uiso 1 1 calc R . . C14 C 0.3850(2) 1.0443(9) 0.3224(2) 0.0416(12) Uani 1 1 d . . . H33 H 0.3671 1.0273 0.3554 0.050 Uiso 1 1 calc R . . H34 H 0.3903 1.2059 0.3169 0.050 Uiso 1 1 calc R . . O5 O 0.19055(15) 0.1110(8) 0.23068(18) 0.0602(11) Uani 1 1 d D . . H35 H 0.199(2) 0.101(9) 0.1940(19) 0.072 Uiso 1 1 d D . . H36 H 0.2212(17) 0.171(9) 0.2714(18) 0.072 Uiso 1 1 d D . . O6 O 0.2936(3) 0.5256(8) 0.2496(2) 0.0923(16) Uani 1 1 d D . . H37 H 0.286(3) 0.478(10) 0.281(3) 0.111 Uiso 1 1 d D . . H38 H 0.283(3) 0.444(9) 0.210(3) 0.111 Uiso 1 1 d 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 0.01987(16) 0.0300(2) 0.01756(14) 0.00257(13) 0.00788(13) -0.00169(13) S1 0.0189(4) 0.0294(5) 0.0234(4) 0.0030(4) 0.0095(4) -0.0010(4) O1 0.0291(15) 0.082(3) 0.0279(14) -0.0009(15) 0.0078(13) 0.0250(16) O2 0.0352(15) 0.086(3) 0.0217(12) -0.0151(16) 0.0143(12) -0.0128(16) N1 0.0205(15) 0.059(3) 0.0195(13) 0.0056(19) 0.0089(12) -0.0080(18) N2 0.0225(15) 0.0274(18) 0.0207(14) 0.0021(15) 0.0065(13) 0.0026(14) N3 0.0278(18) 0.047(2) 0.0266(16) 0.0001(15) 0.0147(15) -0.0090(15) C1 0.0241(18) 0.0204(17) 0.0236(17) 0.0014(15) 0.0129(15) -0.0009(14) C2 0.0203(16) 0.0223(17) 0.0227(15) 0.0000(15) 0.0124(14) 0.0013(14) C3 0.0299(18) 0.030(2) 0.0186(16) 0.0051(18) 0.0098(14) 0.0010(18) C4 0.029(2) 0.066(3) 0.037(2) -0.004(2) 0.022(2) -0.009(2) C5 0.039(2) 0.0217(18) 0.040(2) 0.0087(18) 0.0089(18) 0.0041(16) C6 0.037(2) 0.051(3) 0.0193(18) 0.001(2) 0.0142(18) 0.005(2) C7 0.042(3) 0.055(3) 0.030(2) 0.013(2) 0.021(2) 0.001(2) Pd2 0.01992(15) 0.0288(2) 0.01718(14) -0.00085(12) 0.00862(13) 0.00134(12) S2 0.0190(4) 0.0306(5) 0.0220(4) 0.0009(4) 0.0099(3) 0.0010(4) O3 0.0346(17) 0.094(3) 0.0423(18) -0.016(2) -0.0015(15) 0.0270(19) O4 0.0339(17) 0.104(3) 0.0273(14) -0.0233(17) 0.0158(13) -0.0114(17) N4 0.0201(15) 0.060(3) 0.0222(15) -0.0068(18) 0.0106(13) -0.0017(16) N5 0.0274(17) 0.0247(19) 0.0212(15) -0.0024(13) 0.0103(14) 0.0015(13) N6 0.0240(17) 0.049(2) 0.0225(15) -0.0033(15) 0.0121(14) 0.0016(15) C8 0.0206(16) 0.0228(17) 0.0180(15) 0.0035(16) 0.0089(13) 0.0005(15) C9 0.0237(18) 0.0238(17) 0.0198(16) -0.0023(15) 0.0138(14) -0.0005(14) C10 0.0232(19) 0.043(2) 0.0220(17) 0.0000(17) 0.0117(16) -0.0047(17) C11 0.028(2) 0.043(2) 0.032(2) -0.001(2) 0.0210(18) -0.0034(19) C12 0.037(2) 0.0253(18) 0.037(2) 0.0096(17) 0.0157(18) 0.0001(16) C13 0.033(2) 0.048(3) 0.0244(19) -0.005(2) 0.0139(19) 0.001(2) C14 0.039(3) 0.057(3) 0.027(2) -0.009(2) 0.017(2) 0.005(2) O5 0.052(2) 0.094(3) 0.0350(17) -0.014(2) 0.0245(16) -0.031(2) O6 0.158(4) 0.069(3) 0.051(2) -0.018(2) 0.058(3) -0.050(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 2.029(3) . ? Pd1 N2 2.053(3) . ? Pd1 N3 2.069(3) . ? Pd1 S1 2.2613(12) . ? S1 C1 1.857(4) . ? O1 C3 1.235(4) . ? O2 C3 1.241(4) . ? N1 C2 1.479(4) . ? N1 H1 0.9200 . ? N1 H2 0.9200 . ? N2 C6 1.495(5) . ? N2 H3 0.9200 . ? N2 H4 0.9200 . ? N3 C7 1.475(5) . ? N3 H5 0.9200 . ? N3 H6 0.9200 . ? C1 C5 1.525(5) . ? C1 C4 1.528(5) . ? C1 C2 1.531(5) . ? C2 C3 1.547(5) . ? C2 H7 1.0000 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? C4 H10 0.9800 . ? C5 H11 0.9800 . ? C5 H12 0.9800 . ? C5 H13 0.9800 . ? C6 C7 1.505(6) . ? C6 H14 0.9900 . ? C6 H15 0.9900 . ? C7 H16 0.9900 . ? C7 H17 0.9900 . ? Pd2 N4 2.039(3) . ? Pd2 N5 2.045(3) . ? Pd2 N6 2.083(3) . ? Pd2 S2 2.2625(12) . ? S2 C8 1.862(3) . ? O3 C10 1.232(5) . ? O4 C10 1.229(4) . ? N4 C9 1.482(4) . ? N4 H18 0.9200 . ? N4 H19 0.9200 . ? N5 C13 1.466(5) . ? N5 H20 0.9200 . ? N5 H21 0.9200 . ? N6 C14 1.490(5) . ? N6 H22 0.9200 . ? N6 H23 0.9200 . ? C8 C11 1.520(5) . ? C8 C9 1.527(5) . ? C8 C12 1.537(5) . ? C9 C10 1.559(5) . ? C9 H24 1.0000 . ? C11 H25 0.9800 . ? C11 H26 0.9800 . ? C11 H27 0.9800 . ? C12 H28 0.9800 . ? C12 H29 0.9800 . ? C12 H30 0.9800 . ? C13 C14 1.509(6) . ? C13 H31 0.9900 . ? C13 H32 0.9900 . ? C14 H33 0.9900 . ? C14 H34 0.9900 . ? O5 H35 0.87(5) . ? O5 H36 0.84(4) . ? O6 H37 0.80(7) . ? O6 H38 0.83(5) . ? 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 N2 177.52(10) . . ? N1 Pd1 N3 94.00(13) . . ? N2 Pd1 N3 83.69(13) . . ? N1 Pd1 S1 85.97(10) . . ? N2 Pd1 S1 96.39(10) . . ? N3 Pd1 S1 177.06(12) . . ? C1 S1 Pd1 100.28(12) . . ? C2 N1 Pd1 114.9(2) . . ? C2 N1 H1 108.5 . . ? Pd1 N1 H1 108.5 . . ? C2 N1 H2 108.5 . . ? Pd1 N1 H2 108.5 . . ? H1 N1 H2 107.5 . . ? C6 N2 Pd1 107.2(2) . . ? C6 N2 H3 110.3 . . ? Pd1 N2 H3 110.3 . . ? C6 N2 H4 110.3 . . ? Pd1 N2 H4 110.3 . . ? H3 N2 H4 108.5 . . ? C7 N3 Pd1 108.6(2) . . ? C7 N3 H5 110.0 . . ? Pd1 N3 H5 110.0 . . ? C7 N3 H6 110.0 . . ? Pd1 N3 H6 110.0 . . ? H5 N3 H6 108.4 . . ? C5 C1 C4 110.3(3) . . ? C5 C1 C2 111.7(3) . . ? C4 C1 C2 111.4(3) . . ? C5 C1 S1 109.7(3) . . ? C4 C1 S1 106.5(3) . . ? C2 C1 S1 107.2(2) . . ? N1 C2 C1 110.0(3) . . ? N1 C2 C3 110.7(3) . . ? C1 C2 C3 113.7(3) . . ? N1 C2 H7 107.4 . . ? C1 C2 H7 107.4 . . ? C3 C2 H7 107.4 . . ? O1 C3 O2 126.1(3) . . ? O1 C3 C2 117.6(3) . . ? O2 C3 C2 116.3(3) . . ? C1 C4 H8 109.5 . . ? C1 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C1 C4 H10 109.5 . . ? H8 C4 H10 109.5 . . ? H9 C4 H10 109.5 . . ? C1 C5 H11 109.5 . . ? C1 C5 H12 109.5 . . ? H11 C5 H12 109.5 . . ? C1 C5 H13 109.5 . . ? H11 C5 H13 109.5 . . ? H12 C5 H13 109.5 . . ? N2 C6 C7 108.3(3) . . ? N2 C6 H14 110.0 . . ? C7 C6 H14 110.0 . . ? N2 C6 H15 110.0 . . ? C7 C6 H15 110.0 . . ? H14 C6 H15 108.4 . . ? N3 C7 C6 107.5(4) . . ? N3 C7 H16 110.2 . . ? C6 C7 H16 110.2 . . ? N3 C7 H17 110.2 . . ? C6 C7 H17 110.2 . . ? H16 C7 H17 108.5 . . ? N4 Pd2 N5 177.01(15) . . ? N4 Pd2 N6 94.22(13) . . ? N5 Pd2 N6 83.55(13) . . ? N4 Pd2 S2 86.09(10) . . ? N5 Pd2 S2 96.17(10) . . ? N6 Pd2 S2 179.01(11) . . ? C8 S2 Pd2 98.23(11) . . ? C9 N4 Pd2 116.4(2) . . ? C9 N4 H18 108.2 . . ? Pd2 N4 H18 108.2 . . ? C9 N4 H19 108.2 . . ? Pd2 N4 H19 108.2 . . ? H18 N4 H19 107.3 . . ? C13 N5 Pd2 108.7(2) . . ? C13 N5 H20 109.9 . . ? Pd2 N5 H20 109.9 . . ? C13 N5 H21 109.9 . . ? Pd2 N5 H21 109.9 . . ? H20 N5 H21 108.3 . . ? C14 N6 Pd2 107.3(2) . . ? C14 N6 H22 110.3 . . ? Pd2 N6 H22 110.3 . . ? C14 N6 H23 110.3 . . ? Pd2 N6 H23 110.3 . . ? H22 N6 H23 108.5 . . ? C11 C8 C9 112.3(3) . . ? C11 C8 C12 110.9(3) . . ? C9 C8 C12 111.0(3) . . ? C11 C8 S2 106.6(2) . . ? C9 C8 S2 106.1(2) . . ? C12 C8 S2 109.7(2) . . ? N4 C9 C8 110.7(3) . . ? N4 C9 C10 109.5(3) . . ? C8 C9 C10 113.0(3) . . ? N4 C9 H24 107.8 . . ? C8 C9 H24 107.8 . . ? C10 C9 H24 107.8 . . ? O4 C10 O3 125.2(4) . . ? O4 C10 C9 117.5(4) . . ? O3 C10 C9 117.3(3) . . ? C8 C11 H25 109.5 . . ? C8 C11 H26 109.5 . . ? H25 C11 H26 109.5 . . ? C8 C11 H27 109.5 . . ? H25 C11 H27 109.5 . . ? H26 C11 H27 109.5 . . ? C8 C12 H28 109.5 . . ? C8 C12 H29 109.5 . . ? H28 C12 H29 109.5 . . ? C8 C12 H30 109.5 . . ? H28 C12 H30 109.5 . . ? H29 C12 H30 109.5 . . ? N5 C13 C14 108.4(3) . . ? N5 C13 H31 110.0 . . ? C14 C13 H31 110.0 . . ? N5 C13 H32 110.0 . . ? C14 C13 H32 110.0 . . ? H31 C13 H32 108.4 . . ? N6 C14 C13 107.8(4) . . ? N6 C14 H33 110.2 . . ? C13 C14 H33 110.2 . . ? N6 C14 H34 110.2 . . ? C13 C14 H34 110.2 . . ? H33 C14 H34 108.5 . . ? H35 O5 H36 107(3) . . ? H37 O6 H38 115(3) . . ? 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 C1 5.5(2) . . . . ? N2 Pd1 S1 C1 -173.70(17) . . . . ? N3 Pd1 N1 C2 -155.4(4) . . . . ? S1 Pd1 N1 C2 21.6(4) . . . . ? N3 Pd1 N2 C6 -16.2(3) . . . . ? S1 Pd1 N2 C6 166.7(3) . . . . ? N1 Pd1 N3 C7 167.8(3) . . . . ? N2 Pd1 N3 C7 -13.1(3) . . . . ? Pd1 S1 C1 C5 91.1(3) . . . . ? Pd1 S1 C1 C4 -149.6(3) . . . . ? Pd1 S1 C1 C2 -30.3(2) . . . . ? Pd1 N1 C2 C1 -48.0(4) . . . . ? Pd1 N1 C2 C3 -174.5(3) . . . . ? C5 C1 C2 N1 -70.1(4) . . . . ? C4 C1 C2 N1 166.1(3) . . . . ? S1 C1 C2 N1 50.0(3) . . . . ? C5 C1 C2 C3 54.7(4) . . . . ? C4 C1 C2 C3 -69.1(4) . . . . ? S1 C1 C2 C3 174.8(2) . . . . ? N1 C2 C3 O1 13.1(6) . . . . ? C1 C2 C3 O1 -111.3(4) . . . . ? N1 C2 C3 O2 -164.4(4) . . . . ? C1 C2 C3 O2 71.2(5) . . . . ? Pd1 N2 C6 C7 42.7(4) . . . . ? Pd1 N3 C7 C6 39.7(4) . . . . ? N2 C6 C7 N3 -55.2(5) . . . . ? N4 Pd2 S2 C8 18.30(17) . . . . ? N5 Pd2 S2 C8 -163.66(17) . . . . ? N6 Pd2 N4 C9 -174.1(4) . . . . ? S2 Pd2 N4 C9 6.9(3) . . . . ? N6 Pd2 N5 C13 15.3(3) . . . . ? S2 Pd2 N5 C13 -165.7(3) . . . . ? N4 Pd2 N6 C14 -168.0(3) . . . . ? N5 Pd2 N6 C14 14.0(3) . . . . ? Pd2 S2 C8 C11 -161.1(2) . . . . ? Pd2 S2 C8 C9 -41.3(2) . . . . ? Pd2 S2 C8 C12 78.7(2) . . . . ? Pd2 N4 C9 C8 -37.1(5) . . . . ? Pd2 N4 C9 C10 -162.3(3) . . . . ? C11 C8 C9 N4 167.8(3) . . . . ? C12 C8 C9 N4 -67.4(4) . . . . ? S2 C8 C9 N4 51.7(4) . . . . ? C11 C8 C9 C10 -69.1(4) . . . . ? C12 C8 C9 C10 55.8(4) . . . . ? S2 C8 C9 C10 174.9(3) . . . . ? N4 C9 C10 O4 -163.4(4) . . . . ? C8 C9 C10 O4 72.8(5) . . . . ? N4 C9 C10 O3 16.3(5) . . . . ? C8 C9 C10 O3 -107.5(4) . . . . ? Pd2 N5 C13 C14 -41.8(4) . . . . ? Pd2 N6 C14 C13 -40.1(4) . . . . ? N5 C13 C14 N6 55.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.92 2.01 2.903(6) 162.1 4_546 N3 H5 O5 0.92 2.00 2.841(5) 150.8 4_556 N3 H6 O1 0.92 2.25 3.072(5) 148.2 4_546 N2 H3 S2 0.92 2.51 3.399(4) 161.6 2_646 N2 H4 S2 0.92 2.51 3.421(4) 173.2 2_656 N4 H18 O3 0.92 2.02 2.872(6) 152.5 4_545 N6 H22 O4 0.92 2.04 2.937(5) 163.9 4 N6 H23 O6 0.92 1.92 2.839(6) 175.9 . N5 H20 S1 0.92 2.50 3.354(4) 155.3 2_656 N5 H21 S1 0.92 2.58 3.477(4) 165.8 2_666 O5 H35 O4 0.87(5) 1.97(5) 2.816(4) 163(5) 4_545 O5 H36 O2 0.84(4) 1.92(4) 2.755(4) 173(4) . O6 H37 O2 0.80(7) 2.02(3) 2.815(5) 165(7) . O6 H38 O4 0.83(5) 2.27(3) 3.042(5) 155(5) 4_545 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.732 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.076 _publ_section_references ;Wakita, K. (2001). Yadokari-XG. Software for Crystal Structure Analyses. \nRele ; _chemical_absolute_configuration rm #### END data_[2].H2O _database_code_depnum_ccdc_archive 'CCDC 891174' #TrackingRef '- konno.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H23 N3 O2 Pd S, H2 O' _chemical_formula_sum 'C11 H25 N3 O3 Pd S' _chemical_formula_weight 385.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 13.1888(11) _cell_length_b 19.5017(18) _cell_length_c 5.6250(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1446.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7040 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.383 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14229 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3325 _reflns_number_gt 3053 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material ;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009) ; _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^)+(0.0327P)^2^+0.9217P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_number_reflns 3325 _refine_ls_number_parameters 179 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.32954(2) 0.364114(14) 0.46631(5) 0.02094(9) Uani 1 1 d . . . S1 S 0.18933(8) 0.37772(5) 0.6929(2) 0.0256(2) Uani 1 1 d . . . O1 O 0.3556(3) 0.54300(16) 1.1929(6) 0.0378(9) Uani 1 1 d . . . O2 O 0.4152(2) 0.57449(14) 0.8390(6) 0.0271(7) Uani 1 1 d . . . N1 N 0.3843(3) 0.44773(16) 0.6431(6) 0.0231(8) Uani 1 1 d . . . H1 H 0.4515 0.4401 0.6778 0.028 Uiso 1 1 calc R . . H2 H 0.3812 0.4849 0.5428 0.028 Uiso 1 1 calc R . . N2 N 0.2726(3) 0.28464(17) 0.2652(7) 0.0256(8) Uani 1 1 d . . . H3 H 0.2341 0.2563 0.3597 0.031 Uiso 1 1 calc R . . H4 H 0.2315 0.3018 0.1472 0.031 Uiso 1 1 calc R . . N3 N 0.4618(3) 0.34283(17) 0.2672(6) 0.0225(8) Uani 1 1 d . . . H5 H 0.4869 0.3827 0.2031 0.027 Uiso 1 1 calc R . . H6 H 0.5106 0.3243 0.3647 0.027 Uiso 1 1 calc R . . C1 C 0.2147(3) 0.4632(2) 0.8226(8) 0.0219(9) Uani 1 1 d . . . C2 C 0.3306(3) 0.46551(19) 0.8678(7) 0.0220(8) Uani 1 1 d . . . H7 H 0.3463 0.4284 0.9849 0.026 Uiso 1 1 calc R . . C3 C 0.3700(3) 0.5337(2) 0.9761(9) 0.0241(9) Uani 1 1 d . . . C4 C 0.1536(3) 0.4679(2) 1.0504(8) 0.0308(10) Uani 1 1 d . . . H8 H 0.0864 0.4867 1.0152 0.046 Uiso 1 1 calc R . . H9 H 0.1886 0.4980 1.1632 0.046 Uiso 1 1 calc R . . H10 H 0.1464 0.4221 1.1198 0.046 Uiso 1 1 calc R . . C5 C 0.1825(3) 0.5199(2) 0.6509(8) 0.0271(9) Uani 1 1 d . . . H11 H 0.2397 0.5319 0.5475 0.041 Uiso 1 1 calc R . . H12 H 0.1616 0.5604 0.7414 0.041 Uiso 1 1 calc R . . H13 H 0.1257 0.5038 0.5536 0.041 Uiso 1 1 calc R . . C6 C 0.3560(3) 0.2454(2) 0.1586(9) 0.0289(10) Uani 1 1 d . . . H14 H 0.3865 0.2167 0.2873 0.035 Uiso 1 1 calc R . . C7 C 0.3226(3) 0.19707(19) -0.0392(8) 0.0260(9) Uani 1 1 d . . . H15 H 0.2731 0.1637 0.0251 0.031 Uiso 1 1 calc R . . H16 H 0.2884 0.2238 -0.1657 0.031 Uiso 1 1 calc R . . C8 C 0.4122(4) 0.1587(2) -0.1449(10) 0.0361(12) Uani 1 1 d . . . H17 H 0.4381 0.1255 -0.0265 0.043 Uiso 1 1 calc R . . H18 H 0.3891 0.1325 -0.2856 0.043 Uiso 1 1 calc R . . C9 C 0.4974(4) 0.2061(2) -0.2179(10) 0.0379(12) Uani 1 1 d . . . H19 H 0.4759 0.2329 -0.3586 0.045 Uiso 1 1 calc R . . H20 H 0.5570 0.1783 -0.2644 0.045 Uiso 1 1 calc R . . C10 C 0.5282(3) 0.2555(2) -0.0191(9) 0.0278(10) Uani 1 1 d . . . H21 H 0.5600 0.2294 0.1122 0.033 Uiso 1 1 calc R . . H22 H 0.5785 0.2887 -0.0804 0.033 Uiso 1 1 calc R . . C11 C 0.4365(3) 0.2936(2) 0.0735(9) 0.0271(10) Uani 1 1 d . . . H23 H 0.4075 0.3205 -0.0617 0.033 Uiso 1 1 calc R . . O3 O 0.3354(3) 0.66345(15) 0.5071(6) 0.0341(7) Uani 1 1 d D . . H24 H 0.332(4) 0.642(2) 0.379(5) 0.051 Uiso 1 1 d D . . H25 H 0.366(4) 0.637(2) 0.606(6) 0.051 Uiso 1 1 d 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 0.01923(15) 0.01597(14) 0.02762(16) -0.00265(11) -0.00036(13) -0.00143(12) S1 0.0225(5) 0.0202(5) 0.0341(6) -0.0047(4) 0.0034(4) -0.0044(4) O1 0.056(2) 0.0310(17) 0.0266(18) -0.0079(13) 0.0031(16) -0.0098(16) O2 0.0273(16) 0.0184(14) 0.0356(19) 0.0007(13) 0.0010(15) -0.0057(12) N1 0.0214(18) 0.0176(16) 0.030(2) -0.0004(14) 0.0038(16) -0.0035(14) N2 0.0199(18) 0.0221(17) 0.035(2) -0.0075(15) -0.0007(17) -0.0025(14) N3 0.0217(17) 0.0211(16) 0.0247(19) -0.0047(13) -0.0013(16) -0.0018(14) C1 0.021(2) 0.0186(19) 0.026(2) -0.0017(16) -0.0023(18) 0.0000(16) C2 0.023(2) 0.0192(17) 0.024(2) 0.0011(15) -0.003(2) -0.0020(18) C3 0.0224(19) 0.0209(18) 0.029(2) -0.0043(18) -0.006(2) 0.0009(15) C4 0.032(2) 0.027(2) 0.033(2) -0.0044(18) 0.004(2) -0.0018(19) C5 0.025(2) 0.025(2) 0.031(2) -0.0007(16) -0.004(2) 0.0029(19) C6 0.023(2) 0.028(2) 0.036(3) -0.0092(19) 0.0051(19) -0.0048(18) C7 0.028(2) 0.0213(18) 0.029(2) -0.0033(16) -0.005(3) -0.0027(17) C8 0.040(3) 0.026(2) 0.042(3) -0.011(2) 0.007(2) -0.007(2) C9 0.032(3) 0.035(3) 0.047(3) -0.012(2) 0.010(3) 0.003(2) C10 0.027(2) 0.0236(19) 0.033(3) -0.0015(18) 0.005(2) -0.0031(17) C11 0.027(2) 0.0215(19) 0.033(3) -0.0076(18) -0.002(2) -0.0004(17) O3 0.0372(17) 0.0299(15) 0.0351(19) 0.0022(13) 0.0033(19) 0.0063(14) _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 2.042(3) . ? Pd1 N2 2.061(3) . ? Pd1 N3 2.114(4) . ? Pd1 S1 2.2615(11) . ? S1 C1 1.851(4) . ? O1 C3 1.247(6) . ? O2 C3 1.257(5) . ? N1 C2 1.490(5) . ? N1 H1 0.9200 . ? N1 H2 0.9200 . ? N2 C6 1.468(5) . ? N2 H3 0.9200 . ? N2 H4 0.9200 . ? N3 C11 1.491(5) . ? N3 H5 0.9200 . ? N3 H6 0.9200 . ? C1 C4 1.516(6) . ? C1 C5 1.528(5) . ? C1 C2 1.550(6) . ? C2 C3 1.553(5) . ? C2 H7 1.0000 . ? C4 H8 0.9800 . ? C4 H9 0.9800 . ? C4 H10 0.9800 . ? C5 H11 0.9800 . ? C5 H12 0.9800 . ? C5 H13 0.9800 . ? C6 C11 1.496(6) . ? C6 C7 1.524(6) . ? C6 H14 1.0000 . ? C7 C8 1.521(6) . ? C7 H15 0.9900 . ? C7 H16 0.9900 . ? C8 C9 1.512(7) . ? C8 H17 0.9900 . ? C8 H18 0.9900 . ? C9 C10 1.531(6) . ? C9 H19 0.9900 . ? C9 H20 0.9900 . ? C10 C11 1.511(6) . ? C10 H21 0.9900 . ? C10 H22 0.9900 . ? C11 H23 1.0000 . ? O3 H24 0.838(18) . ? O3 H25 0.86(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 N1 Pd1 N2 175.51(16) . . ? N1 Pd1 N3 97.06(13) . . ? N2 Pd1 N3 82.09(13) . . ? N1 Pd1 S1 85.48(10) . . ? N2 Pd1 S1 95.70(10) . . ? N3 Pd1 S1 175.06(10) . . ? C1 S1 Pd1 100.37(14) . . ? C2 N1 Pd1 115.5(2) . . ? C2 N1 H1 108.4 . . ? Pd1 N1 H1 108.4 . . ? C2 N1 H2 108.4 . . ? Pd1 N1 H2 108.4 . . ? H1 N1 H2 107.5 . . ? C6 N2 Pd1 110.0(3) . . ? C6 N2 H3 109.7 . . ? Pd1 N2 H3 109.7 . . ? C6 N2 H4 109.7 . . ? Pd1 N2 H4 109.7 . . ? H3 N2 H4 108.2 . . ? C11 N3 Pd1 109.2(2) . . ? C11 N3 H5 109.8 . . ? Pd1 N3 H5 109.8 . . ? C11 N3 H6 109.8 . . ? Pd1 N3 H6 109.8 . . ? H5 N3 H6 108.3 . . ? C4 C1 C5 110.0(3) . . ? C4 C1 C2 112.5(4) . . ? C5 C1 C2 110.9(3) . . ? C4 C1 S1 107.0(3) . . ? C5 C1 S1 110.6(3) . . ? C2 C1 S1 105.6(3) . . ? N1 C2 C1 108.8(3) . . ? N1 C2 C3 111.9(3) . . ? C1 C2 C3 114.8(3) . . ? N1 C2 H7 107.0 . . ? C1 C2 H7 107.0 . . ? C3 C2 H7 107.0 . . ? O1 C3 O2 125.5(4) . . ? O1 C3 C2 117.2(4) . . ? O2 C3 C2 117.4(4) . . ? C1 C4 H8 109.5 . . ? C1 C4 H9 109.5 . . ? H8 C4 H9 109.5 . . ? C1 C4 H10 109.5 . . ? H8 C4 H10 109.5 . . ? H9 C4 H10 109.5 . . ? C1 C5 H11 109.5 . . ? C1 C5 H12 109.5 . . ? H11 C5 H12 109.5 . . ? C1 C5 H13 109.5 . . ? H11 C5 H13 109.5 . . ? H12 C5 H13 109.5 . . ? N2 C6 C11 109.6(3) . . ? N2 C6 C7 113.8(3) . . ? C11 C6 C7 111.1(4) . . ? N2 C6 H14 107.3 . . ? C11 C6 H14 107.3 . . ? C7 C6 H14 107.3 . . ? C8 C7 C6 111.4(4) . . ? C8 C7 H15 109.3 . . ? C6 C7 H15 109.3 . . ? C8 C7 H16 109.3 . . ? C6 C7 H16 109.3 . . ? H15 C7 H16 108.0 . . ? C9 C8 C7 112.6(4) . . ? C9 C8 H17 109.1 . . ? C7 C8 H17 109.1 . . ? C9 C8 H18 109.1 . . ? C7 C8 H18 109.1 . . ? H17 C8 H18 107.8 . . ? C8 C9 C10 112.5(4) . . ? C8 C9 H19 109.1 . . ? C10 C9 H19 109.1 . . ? C8 C9 H20 109.1 . . ? C10 C9 H20 109.1 . . ? H19 C9 H20 107.8 . . ? C11 C10 C9 110.4(4) . . ? C11 C10 H21 109.6 . . ? C9 C10 H21 109.6 . . ? C11 C10 H22 109.6 . . ? C9 C10 H22 109.6 . . ? H21 C10 H22 108.1 . . ? N3 C11 C6 109.2(4) . . ? N3 C11 C10 112.9(4) . . ? C6 C11 C10 111.7(3) . . ? N3 C11 H23 107.6 . . ? C6 C11 H23 107.6 . . ? C10 C11 H23 107.6 . . ? H24 O3 H25 106(3) . . ? 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 C1 11.37(17) . . . . ? N2 Pd1 S1 C1 -164.28(17) . . . . ? N3 Pd1 N1 C2 -158.7(3) . . . . ? S1 Pd1 N1 C2 17.0(3) . . . . ? N3 Pd1 N2 C6 17.0(3) . . . . ? S1 Pd1 N2 C6 -158.6(3) . . . . ? N1 Pd1 N3 C11 -166.0(3) . . . . ? N2 Pd1 N3 C11 9.5(3) . . . . ? Pd1 S1 C1 C4 -156.9(3) . . . . ? Pd1 S1 C1 C5 83.3(3) . . . . ? Pd1 S1 C1 C2 -36.8(3) . . . . ? Pd1 N1 C2 C1 -46.2(4) . . . . ? Pd1 N1 C2 C3 -174.1(3) . . . . ? C4 C1 C2 N1 169.6(3) . . . . ? C5 C1 C2 N1 -66.6(4) . . . . ? S1 C1 C2 N1 53.3(3) . . . . ? C4 C1 C2 C3 -64.1(5) . . . . ? C5 C1 C2 C3 59.7(5) . . . . ? S1 C1 C2 C3 179.5(3) . . . . ? N1 C2 C3 O1 -158.0(4) . . . . ? C1 C2 C3 O1 77.3(5) . . . . ? N1 C2 C3 O2 20.9(5) . . . . ? C1 C2 C3 O2 -103.8(4) . . . . ? Pd1 N2 C6 C11 -40.8(5) . . . . ? Pd1 N2 C6 C7 -165.9(3) . . . . ? N2 C6 C7 C8 179.2(4) . . . . ? C11 C6 C7 C8 54.9(5) . . . . ? C6 C7 C8 C9 -51.5(6) . . . . ? C7 C8 C9 C10 51.0(6) . . . . ? C8 C9 C10 C11 -53.0(5) . . . . ? Pd1 N3 C11 C6 -33.9(4) . . . . ? Pd1 N3 C11 C10 -158.8(3) . . . . ? N2 C6 C11 N3 49.5(5) . . . . ? C7 C6 C11 N3 176.2(3) . . . . ? N2 C6 C11 C10 175.2(4) . . . . ? C7 C6 C11 C10 -58.2(5) . . . . ? C9 C10 C11 N3 -179.7(4) . . . . ? C9 C10 C11 C6 56.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.92 2.00 2.897(5) 165.2 2_665 N1 H2 O1 0.92 2.30 3.163(5) 157.1 1_554 N2 H3 O3 0.92 2.16 3.042(5) 159.6 4_546 N3 H5 O1 0.92 2.53 3.307(5) 142.0 2_664 N3 H5 O2 0.92 2.56 3.322(5) 140.5 2_664 N3 H6 O3 0.92 2.20 2.999(5) 145.3 2_665 O3 H24 O1 0.838(18) 2.21(3) 2.951(4) 147(4) 1_554 O3 H25 O2 0.86(4) 1.90(2) 2.758(4) 172(5) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.742 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.103 _publ_section_references ; Wakita, K. (2001). Yadokari-XG. Software for Crystal Structure Analyses. \nRele ; _chemical_absolute_configuration rm