# 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 _publ_contact_author # Name and address of author for correspondence ; Prof. Dr. Alfonso Casti\~A+-eiras Universidad de Santiago de Compostela Departamento de Quimica Inorganica Campus Vida E-15782 Santiago de Compostela (Spain) ; _publ_contact_author_phone +34-881814950 _publ_contact_author_fax +34-981547163 _publ_contact_author_email alfonso.castineiras@usc.es _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, For receiving a depository number, please find enclosed the data of X-ray structure analyses of the compounds: Compound 1a (Ref. 01lg15) [Ni(HAcb4DM)2].2H2O Compound 2a (Ref. 02lg15) [Pd(Acb4DM)(DMSO)].DMSO Compound 3a (Ref. 02lg01) [Pt(Acb4DM)(DMSO)].DMSO With thanks in advance, Yours sincerely, Alfonso Casti\~neiras ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Neutral Ni(II), Pd(II) and Pt(II) ONS-pincer complexes of 5-acetylbarbituric- 4N-dimethylthiosemicarbazone. Synthesis, characterization and properties ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address A.Castineiras ; University of Santiago de Compostela Department of Inorganic Chemistry Faculty of Pharmacy Santiago de Compostela Spain ; N.Fernandez-Hermida ; University of Santiago de Compostela Department of Inorganic Chemistry Faculty of Pharmacy Santiago de Compostela Spain ; I.Garcia-Santos ; University of Santiago de Compostela Department of Inorganic Chemistry Santiago de Compostela Town Spain ; ; L.GomeZ-Rodriguez ; ; University of Santiago de Compostela Department of Inorganic Chemistry Faculty of Pharmacy Santiago de Compostela Spain ; _publ_contact_author_name 'Prof. Dr. Alfonso CastiA+-eiras' #============================================================================== data_01lg15 _database_code_depnum_ccdc_archive 'CCDC 871179' #TrackingRef 'ni_pd_pt.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 N10 Ni O6 S2, 2(H2 O)' _chemical_formula_sum 'C18 H28 N10 Ni O8 S2' _chemical_formula_weight 635.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni -3.0029 0.5091 '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' O O 0.0492 0.0322 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2231(6) _cell_length_b 12.9966(13) _cell_length_c 13.1332(10) _cell_angle_alpha 63.518(6) _cell_angle_beta 81.209(6) _cell_angle_gamma 87.715(7) _cell_volume 1542.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.95 _cell_measurement_theta_max 42.21 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 2.657 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.4480 _exptl_absorpt_correction_T_max 0.6758 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MACH3 Enraf Nonius' _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 6436 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 72.94 _reflns_number_total 6150 _reflns_number_gt 4993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction 'GENHKL (Kretschmar, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Speck, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. There is a disordered region in the cell (volume ca. 263.6 A^3) which could not be described satisfatorily. Therefore a correction by SQUEEZE was used. ; _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^)+(0.0660P)^2^+0.8945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6150 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Ni1 Ni 0.42562(4) 0.25532(3) 0.25037(3) 0.03774(13) Uani 1 1 d . . . S1 S 0.36525(8) 0.14275(7) 0.45430(6) 0.0590(2) Uani 1 1 d . . . S2 S 0.34847(8) 0.12008(6) 0.19423(7) 0.0569(2) Uani 1 1 d . . . O11 O 0.52481(18) 0.34795(15) 0.08382(15) 0.0423(4) Uani 1 1 d . . . O13 O 0.6739(3) 0.2893(2) -0.22640(19) 0.0773(7) Uani 1 1 d . . . O15 O 0.8586(3) 0.0818(2) 0.0925(2) 0.0732(7) Uani 1 1 d . . . O21 O 0.46270(15) 0.39933(15) 0.27574(15) 0.0404(4) Uani 1 1 d . . . O23 O 0.34249(18) 0.5213(2) 0.54655(19) 0.0585(6) Uani 1 1 d . . . O25 O 0.01444(17) 0.4669(2) 0.37983(18) 0.0567(5) Uani 1 1 d . . . N11 N 0.6054(2) 0.3167(2) -0.06732(19) 0.0500(5) Uani 1 1 d . . . H11 H 0.5507 0.3665 -0.1040 0.060 Uiso 1 1 d R . . N12 N 0.6073(2) 0.19919(18) 0.28906(18) 0.0401(4) Uani 1 1 d . . . N13 N 0.6258(2) 0.1858(2) 0.39745(19) 0.0468(5) Uani 1 1 d . . . H13 H 0.7036 0.1928 0.4115 0.056 Uiso 1 1 d R . . N14 N 0.5410(3) 0.1563(2) 0.5793(2) 0.0606(7) Uani 1 1 d . . . N15 N 0.7700(3) 0.1913(2) -0.0648(2) 0.0572(6) Uani 1 1 d . . . H15 H 0.8233 0.1612 -0.1006 0.069 Uiso 1 1 d R . . N21 N 0.39676(19) 0.46076(19) 0.40918(18) 0.0404(5) Uani 1 1 d . . . H21 H 0.4784 0.4588 0.4185 0.049 Uiso 1 1 d R . . N22 N 0.25615(19) 0.33327(17) 0.19616(17) 0.0366(4) Uani 1 1 d . . . N23 N 0.2210(2) 0.31729(19) 0.10484(18) 0.0415(5) Uani 1 1 d . . . H23 H 0.1755 0.3670 0.0562 0.050 Uiso 1 1 d R . . N24 N 0.2257(3) 0.2062(2) 0.0101(2) 0.0569(6) Uani 1 1 d . . . N25 N 0.1811(2) 0.4929(2) 0.4599(2) 0.0462(5) Uani 1 1 d . . . H25 H 0.1223 0.5105 0.5033 0.055 Uiso 1 1 d R . . C11 C 0.6060(3) 0.2936(2) 0.0463(2) 0.0404(5) Uani 1 1 d . . . C13 C 0.6835(3) 0.2670(3) -0.1263(3) 0.0559(7) Uani 1 1 d . . . C15 C 0.7807(3) 0.1581(3) 0.0490(3) 0.0524(7) Uani 1 1 d . . . C16 C 0.6982(3) 0.2141(2) 0.1062(2) 0.0432(6) Uani 1 1 d . . . C17 C 0.7105(3) 0.1900(2) 0.2241(2) 0.0433(6) Uani 1 1 d . . . C18 C 0.5183(3) 0.1630(2) 0.4798(2) 0.0489(6) Uani 1 1 d . . . C19 C 0.4340(5) 0.1395(5) 0.6723(3) 0.0924(14) Uani 1 1 d . . . H19A H 0.3551 0.1725 0.6408 0.139 Uiso 1 1 d R . . H19B H 0.4564 0.1745 0.7183 0.139 Uiso 1 1 d R . . H19C H 0.4191 0.0582 0.7192 0.139 Uiso 1 1 d R . . C20 C 0.6749(4) 0.1674(3) 0.6000(3) 0.0689(9) Uani 1 1 d . . . H20A H 0.7319 0.1168 0.5798 0.103 Uiso 1 1 d R . . H20B H 0.6732 0.1476 0.6799 0.103 Uiso 1 1 d R . . H20C H 0.7074 0.2454 0.5539 0.103 Uiso 1 1 d R . . C21 C 0.3666(2) 0.4286(2) 0.3277(2) 0.0347(5) Uani 1 1 d . . . C23 C 0.3086(2) 0.4938(2) 0.4756(2) 0.0428(6) Uani 1 1 d . . . C25 C 0.1372(2) 0.4647(2) 0.3801(2) 0.0406(5) Uani 1 1 d . . . C26 C 0.2332(2) 0.4345(2) 0.3095(2) 0.0356(5) Uani 1 1 d . . . C27 C 0.1957(2) 0.4120(2) 0.2176(2) 0.0362(5) Uani 1 1 d . . . C28 C 0.2614(3) 0.2197(2) 0.0968(2) 0.0448(6) Uani 1 1 d . . . C29 C 0.2782(5) 0.1129(4) -0.0164(4) 0.0861(12) Uani 1 1 d . . . H29A H 0.3726 0.1229 -0.0378 0.129 Uiso 1 1 d R . . H29B H 0.2391 0.1135 -0.0787 0.129 Uiso 1 1 d R . . H29C H 0.2571 0.0407 0.0505 0.129 Uiso 1 1 d R . . C30 C 0.1322(4) 0.2793(3) -0.0613(3) 0.0711(9) Uani 1 1 d . . . H30A H 0.0616 0.2967 -0.0147 0.107 Uiso 1 1 d R . . H30B H 0.0964 0.2401 -0.0984 0.107 Uiso 1 1 d R . . H30C H 0.1769 0.3494 -0.1184 0.107 Uiso 1 1 d R . . C170 C 0.8425(3) 0.1612(3) 0.2659(3) 0.0640(9) Uani 1 1 d . . . H17A H 0.8762 0.2253 0.2729 0.096 Uiso 1 1 d R . . H17B H 0.9036 0.1449 0.2122 0.096 Uiso 1 1 d R . . H17C H 0.8318 0.0950 0.3397 0.096 Uiso 1 1 d R . . C270 C 0.0955(3) 0.4859(3) 0.1462(2) 0.0477(6) Uani 1 1 d . . . H27A H 0.1380 0.5310 0.0687 0.071 Uiso 1 1 d R . . H27B H 0.0584 0.5360 0.1781 0.071 Uiso 1 1 d R . . H27C H 0.0263 0.4380 0.1462 0.071 Uiso 1 1 d R . . O1 O 0.80288(16) 0.38865(15) 0.32383(14) 0.0593(5) Uani 1 1 d . . . H1A H 0.7525 0.4250 0.3642 0.071 Uiso 1 1 d R . . H1B H 0.8836 0.4213 0.3235 0.071 Uiso 1 1 d R . . O2 O 0.71879(16) 0.48827(15) 0.10554(14) 0.0814(8) Uani 1 1 d R . . H2A H 0.7379 0.4603 0.1790 0.098 Uiso 1 1 d R . . H2B H 0.6560 0.5377 0.1071 0.098 Uiso 1 1 d 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 Ni1 0.0388(2) 0.0363(2) 0.0377(2) -0.01624(18) -0.00551(17) 0.00234(16) S1 0.0569(4) 0.0626(5) 0.0431(4) -0.0119(3) -0.0012(3) -0.0075(3) S2 0.0754(5) 0.0359(3) 0.0630(5) -0.0219(3) -0.0215(4) 0.0024(3) O11 0.0480(9) 0.0388(9) 0.0389(9) -0.0175(7) -0.0040(7) 0.0083(7) O13 0.118(2) 0.0759(16) 0.0459(12) -0.0350(12) -0.0116(13) 0.0162(15) O15 0.0828(16) 0.0747(15) 0.0787(16) -0.0484(13) -0.0234(13) 0.0402(13) O21 0.0296(8) 0.0516(10) 0.0490(10) -0.0319(8) -0.0017(7) 0.0034(7) O23 0.0335(9) 0.1020(17) 0.0727(14) -0.0668(14) -0.0141(9) 0.0106(10) O25 0.0259(8) 0.1036(17) 0.0654(13) -0.0600(13) -0.0070(8) 0.0067(9) N11 0.0626(14) 0.0484(13) 0.0395(12) -0.0202(10) -0.0087(10) 0.0094(11) N12 0.0466(11) 0.0374(10) 0.0373(11) -0.0173(9) -0.0086(9) 0.0062(9) N13 0.0511(12) 0.0518(13) 0.0401(12) -0.0211(10) -0.0139(9) 0.0097(10) N14 0.0750(17) 0.0654(16) 0.0391(13) -0.0211(12) -0.0104(12) 0.0076(13) N15 0.0682(16) 0.0568(14) 0.0540(14) -0.0349(12) -0.0001(12) 0.0115(12) N21 0.0267(9) 0.0561(13) 0.0484(12) -0.0320(11) -0.0062(8) 0.0042(8) N22 0.0366(10) 0.0416(11) 0.0346(10) -0.0193(9) -0.0055(8) -0.0020(8) N23 0.0423(11) 0.0456(11) 0.0427(11) -0.0238(10) -0.0110(9) 0.0018(9) N24 0.0689(16) 0.0537(14) 0.0639(16) -0.0379(13) -0.0173(13) 0.0004(12) N25 0.0277(9) 0.0751(15) 0.0538(13) -0.0450(12) -0.0062(9) 0.0068(9) C11 0.0457(13) 0.0362(12) 0.0385(13) -0.0168(10) -0.0025(10) -0.0013(10) C13 0.073(2) 0.0508(16) 0.0470(16) -0.0267(14) -0.0006(14) 0.0002(14) C15 0.0568(16) 0.0499(15) 0.0574(17) -0.0309(14) -0.0064(13) 0.0060(13) C16 0.0462(13) 0.0391(13) 0.0464(14) -0.0218(11) -0.0051(11) 0.0048(10) C17 0.0474(14) 0.0386(13) 0.0473(14) -0.0219(11) -0.0096(11) 0.0091(10) C18 0.0627(17) 0.0412(14) 0.0386(13) -0.0135(11) -0.0102(12) 0.0071(12) C19 0.098(3) 0.128(4) 0.0453(19) -0.036(2) -0.0041(19) 0.015(3) C20 0.094(3) 0.067(2) 0.0434(16) -0.0176(15) -0.0251(17) 0.0010(18) C21 0.0331(11) 0.0369(11) 0.0359(12) -0.0183(10) -0.0035(9) 0.0010(9) C23 0.0321(11) 0.0596(16) 0.0475(14) -0.0333(13) -0.0074(10) 0.0051(10) C25 0.0290(11) 0.0564(15) 0.0431(13) -0.0283(12) -0.0048(9) 0.0028(10) C26 0.0296(11) 0.0442(13) 0.0370(12) -0.0222(10) -0.0036(9) 0.0025(9) C27 0.0288(10) 0.0445(13) 0.0361(12) -0.0192(10) -0.0025(9) -0.0015(9) C28 0.0461(14) 0.0446(14) 0.0477(14) -0.0242(12) -0.0039(11) -0.0074(11) C29 0.121(3) 0.074(2) 0.096(3) -0.063(2) -0.029(3) 0.010(2) C30 0.079(2) 0.078(2) 0.077(2) -0.045(2) -0.0353(19) 0.0009(18) C170 0.0557(17) 0.082(2) 0.075(2) -0.0516(19) -0.0242(15) 0.0282(16) C270 0.0402(13) 0.0637(17) 0.0464(14) -0.0302(13) -0.0113(11) 0.0113(12) O1 0.0436(10) 0.0794(15) 0.0738(14) -0.0523(13) -0.0023(9) -0.0045(10) O2 0.0957(19) 0.0862(18) 0.0528(13) -0.0222(13) -0.0018(12) -0.0393(15) _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 Ni1 N12 2.022(2) . y Ni1 N22 2.032(2) . y Ni1 O11 2.0815(18) . y Ni1 O21 2.0998(17) . y Ni1 S2 2.3873(8) . y Ni1 S1 2.4015(9) . y S1 C18 1.704(3) . ? S2 C28 1.699(3) . ? O11 C11 1.252(3) . ? O11 O2 2.875(2) . ? O13 C13 1.233(4) . ? O15 C15 1.231(4) . ? O21 C21 1.254(3) . ? O21 O2 3.055(2) . ? O23 C23 1.234(3) . ? O25 C25 1.254(3) . ? N11 C13 1.368(4) . ? N11 C11 1.386(3) . ? N11 H11 0.8600 . ? N12 C17 1.289(3) . ? N12 N13 1.397(3) . ? N13 C18 1.357(4) . ? N13 H13 0.8600 . ? N14 C18 1.326(4) . ? N14 C19 1.452(4) . ? N14 C20 1.460(5) . ? N15 C13 1.357(4) . ? N15 C15 1.381(4) . ? N15 H15 0.8599 . ? N21 C23 1.349(3) . ? N21 C21 1.387(3) . ? N21 H21 0.8600 . ? N22 C27 1.290(3) . ? N22 N23 1.404(3) . ? N23 C28 1.362(3) . ? N23 H23 0.8601 . ? N24 C28 1.331(3) . ? N24 C30 1.450(4) . ? N24 C29 1.465(4) . ? N25 C23 1.351(3) . ? N25 C25 1.391(3) . ? N25 H25 0.8599 . ? C11 C16 1.413(4) . ? C15 C16 1.431(4) . ? C16 C17 1.461(4) . ? C17 C170 1.506(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9599 . ? C20 H20B 0.9600 . ? C20 H20C 0.9601 . ? C21 C26 1.413(3) . ? C25 C26 1.411(3) . ? C26 C27 1.468(3) . ? C27 C270 1.504(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9599 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C170 H17A 0.9600 . ? C170 H17B 0.9599 . ? C170 H17C 0.9600 . ? C270 H27A 0.9600 . ? C270 H27B 0.9599 . ? C270 H27C 0.9601 . ? O1 O23 2.710(2) 2_666 ? O1 O25 2.754(2) 1_655 ? O1 O2 2.8263 . ? O1 H1A 0.9437 . ? O1 H1B 0.9414 . ? O2 H2A 0.9165 . ? O2 H2B 0.8948 . ? 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 N12 Ni1 N22 171.96(8) . . y N12 Ni1 O11 84.61(8) . . y N22 Ni1 O11 88.97(7) . . y N12 Ni1 O21 88.98(7) . . y N22 Ni1 O21 85.77(7) . . y O11 Ni1 O21 86.32(7) . . y N12 Ni1 S2 103.09(6) . . y N22 Ni1 S2 81.63(6) . . y O11 Ni1 S2 89.36(6) . . y O21 Ni1 S2 166.74(5) . . y N12 Ni1 S1 81.69(6) . . y N22 Ni1 S1 104.37(6) . . y O11 Ni1 S1 165.90(6) . . y O21 Ni1 S1 90.07(6) . . y S2 Ni1 S1 97.00(3) . . y C18 S1 Ni1 92.14(10) . . ? C28 S2 Ni1 93.17(9) . . ? C11 O11 Ni1 116.18(16) . . ? C11 O11 O2 96.08(15) . . ? Ni1 O11 O2 104.59(8) . . ? C21 O21 Ni1 115.06(15) . . ? C21 O21 O2 143.55(16) . . ? Ni1 O21 O2 98.37(6) . . ? C13 N11 C11 125.9(2) . . ? C13 N11 H11 117.0 . . ? C11 N11 H11 117.1 . . ? C17 N12 N13 116.6(2) . . ? C17 N12 Ni1 129.65(18) . . ? N13 N12 Ni1 112.92(15) . . ? C18 N13 N12 118.6(2) . . ? C18 N13 H13 120.6 . . ? N12 N13 H13 120.7 . . ? C18 N14 C19 121.8(3) . . ? C18 N14 C20 121.5(3) . . ? C19 N14 C20 116.7(3) . . ? C13 N15 C15 126.4(2) . . ? C13 N15 H15 116.6 . . ? C15 N15 H15 117.0 . . ? C23 N21 C21 125.4(2) . . ? C23 N21 H21 117.4 . . ? C21 N21 H21 117.2 . . ? C27 N22 N23 116.7(2) . . ? C27 N22 Ni1 127.80(16) . . ? N23 N22 Ni1 113.71(14) . . ? C28 N23 N22 117.2(2) . . ? C28 N23 H23 121.4 . . ? N22 N23 H23 121.3 . . ? C28 N24 C30 123.0(3) . . ? C28 N24 C29 120.7(3) . . ? C30 N24 C29 116.3(3) . . ? C23 N25 C25 125.3(2) . . ? C23 N25 H25 117.3 . . ? C25 N25 H25 117.4 . . ? O11 C11 N11 115.3(2) . . ? O11 C11 C16 127.3(2) . . ? N11 C11 C16 117.4(2) . . ? O13 C13 N15 123.7(3) . . ? O13 C13 N11 122.0(3) . . ? N15 C13 N11 114.3(3) . . ? O15 C15 N15 117.0(3) . . ? O15 C15 C16 126.1(3) . . ? N15 C15 C16 116.9(3) . . ? C11 C16 C15 119.0(2) . . ? C11 C16 C17 120.7(2) . . ? C15 C16 C17 120.3(2) . . ? N12 C17 C16 118.4(2) . . ? N12 C17 C170 121.1(2) . . ? C16 C17 C170 120.4(2) . . ? N14 C18 N13 116.1(3) . . ? N14 C18 S1 123.2(2) . . ? N13 C18 S1 120.7(2) . . ? N14 C19 H19A 109.5 . . ? N14 C19 H19B 110.9 . . ? H19A C19 H19B 109.5 . . ? N14 C19 H19C 108.0 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 H20A 109.6 . . ? N14 C20 H20B 109.4 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.4 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O21 C21 N21 115.7(2) . . ? O21 C21 C26 126.7(2) . . ? N21 C21 C26 117.6(2) . . ? O23 C23 N21 122.0(2) . . ? O23 C23 N25 122.7(2) . . ? N21 C23 N25 115.3(2) . . ? O25 C25 N25 115.9(2) . . ? O25 C25 C26 126.5(2) . . ? N25 C25 C26 117.5(2) . . ? C25 C26 C21 118.6(2) . . ? C25 C26 C27 120.7(2) . . ? C21 C26 C27 120.7(2) . . ? N22 C27 C26 118.4(2) . . ? N22 C27 C270 121.8(2) . . ? C26 C27 C270 119.6(2) . . ? N24 C28 N23 116.0(2) . . ? N24 C28 S2 122.4(2) . . ? N23 C28 S2 121.6(2) . . ? N24 C29 H29A 109.6 . . ? N24 C29 H29B 109.7 . . ? H29A C29 H29B 109.5 . . ? N24 C29 H29C 109.1 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N24 C30 H30A 110.0 . . ? N24 C30 H30B 109.2 . . ? H30A C30 H30B 109.5 . . ? N24 C30 H30C 109.3 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C17 C170 H17A 109.4 . . ? C17 C170 H17B 109.7 . . ? H17A C170 H17B 109.5 . . ? C17 C170 H17C 109.4 . . ? H17A C170 H17C 109.5 . . ? H17B C170 H17C 109.5 . . ? C27 C270 H27A 109.5 . . ? C27 C270 H27B 109.2 . . ? H27A C270 H27B 109.5 . . ? C27 C270 H27C 109.7 . . ? H27A C270 H27C 109.5 . . ? H27B C270 H27C 109.5 . . ? O23 O1 O25 83.68(7) 2_666 1_655 ? O23 O1 O2 107.40(6) 2_666 . ? O25 O1 O2 125.27(6) 1_655 . ? O23 O1 H1A 4.1 2_666 . ? O25 O1 H1A 83.6 1_655 . ? O2 O1 H1A 104.1 . . ? O23 O1 H1B 94.2 2_666 . ? O25 O1 H1B 14.3 1_655 . ? O2 O1 H1B 112.7 . . ? H1A O1 H1B 93.4 . . ? O1 O2 O11 113.15(5) . . ? O1 O2 O21 75.73(5) . . ? O11 O2 O21 57.58(5) . . ? O1 O2 H2A 6.8 . . ? O11 O2 H2A 112.9 . . ? O21 O2 H2A 70.9 . . ? O1 O2 H2B 107.0 . . ? O11 O2 H2B 89.7 . . ? O21 O2 H2B 60.4 . . ? H2A O2 H2B 100.2 . . ? 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 N12 Ni1 S1 C18 28.02(11) . . . . ? N22 Ni1 S1 C18 -146.59(11) . . . . ? O11 Ni1 S1 C18 14.1(2) . . . . ? O21 Ni1 S1 C18 -60.94(11) . . . . ? S2 Ni1 S1 C18 130.30(10) . . . . ? N12 Ni1 S2 C28 -147.14(11) . . . . ? N22 Ni1 S2 C28 26.23(11) . . . . ? O11 Ni1 S2 C28 -62.83(11) . . . . ? O21 Ni1 S2 C28 8.0(3) . . . . ? S1 Ni1 S2 C28 129.80(10) . . . . ? N12 Ni1 O11 C11 46.76(18) . . . . ? N22 Ni1 O11 C11 -138.09(19) . . . . ? O21 Ni1 O11 C11 136.09(18) . . . . ? S2 Ni1 O11 C11 -56.45(18) . . . . ? S1 Ni1 O11 C11 60.6(3) . . . . ? N12 Ni1 O11 O2 -57.70(8) . . . . ? N22 Ni1 O11 O2 117.44(8) . . . . ? O21 Ni1 O11 O2 31.62(7) . . . . ? S2 Ni1 O11 O2 -160.92(6) . . . . ? S1 Ni1 O11 O2 -43.8(2) . . . . ? N12 Ni1 O21 C21 -139.08(18) . . . . ? N22 Ni1 O21 C21 47.01(17) . . . . ? O11 Ni1 O21 C21 136.25(17) . . . . ? S2 Ni1 O21 C21 65.1(3) . . . . ? S1 Ni1 O21 C21 -57.39(17) . . . . ? N12 Ni1 O21 O2 55.81(8) . . . . ? N22 Ni1 O21 O2 -118.09(8) . . . . ? O11 Ni1 O21 O2 -28.85(7) . . . . ? S2 Ni1 O21 O2 -100.0(2) . . . . ? S1 Ni1 O21 O2 137.51(6) . . . . ? N22 Ni1 N12 C17 -63.0(7) . . . . ? O11 Ni1 N12 C17 -25.8(2) . . . . ? O21 Ni1 N12 C17 -112.2(2) . . . . ? S2 Ni1 N12 C17 62.3(2) . . . . ? S1 Ni1 N12 C17 157.6(2) . . . . ? N22 Ni1 N12 N13 106.3(6) . . . . ? O11 Ni1 N12 N13 143.52(17) . . . . ? O21 Ni1 N12 N13 57.12(17) . . . . ? S2 Ni1 N12 N13 -128.40(16) . . . . ? S1 Ni1 N12 N13 -33.10(16) . . . . ? C17 N12 N13 C18 -162.0(2) . . . . ? Ni1 N12 N13 C18 27.1(3) . . . . ? N12 Ni1 N22 C27 -70.2(6) . . . . ? O11 Ni1 N22 C27 -107.2(2) . . . . ? O21 Ni1 N22 C27 -20.8(2) . . . . ? S2 Ni1 N22 C27 163.3(2) . . . . ? S1 Ni1 N22 C27 68.2(2) . . . . ? N12 Ni1 N22 N23 94.0(6) . . . . ? O11 Ni1 N22 N23 57.05(16) . . . . ? O21 Ni1 N22 N23 143.43(16) . . . . ? S2 Ni1 N22 N23 -32.45(15) . . . . ? S1 Ni1 N22 N23 -127.58(15) . . . . ? C27 N22 N23 C28 -166.1(2) . . . . ? Ni1 N22 N23 C28 27.8(3) . . . . ? Ni1 O11 C11 N11 138.92(19) . . . . ? O2 O11 C11 N11 -111.5(2) . . . . ? Ni1 O11 C11 C16 -42.3(3) . . . . ? O2 O11 C11 C16 67.3(3) . . . . ? C13 N11 C11 O11 -179.1(3) . . . . ? C13 N11 C11 C16 2.0(4) . . . . ? C15 N15 C13 O13 -176.3(3) . . . . ? C15 N15 C13 N11 3.0(5) . . . . ? C11 N11 C13 O13 177.4(3) . . . . ? C11 N11 C13 N15 -1.9(4) . . . . ? C13 N15 C15 O15 174.7(3) . . . . ? C13 N15 C15 C16 -4.1(5) . . . . ? O11 C11 C16 C15 178.3(3) . . . . ? N11 C11 C16 C15 -2.9(4) . . . . ? O11 C11 C16 C17 -2.4(4) . . . . ? N11 C11 C16 C17 176.4(2) . . . . ? O15 C15 C16 C11 -174.8(3) . . . . ? N15 C15 C16 C11 3.8(4) . . . . ? O15 C15 C16 C17 5.9(5) . . . . ? N15 C15 C16 C17 -175.5(3) . . . . ? N13 N12 C17 C16 -174.3(2) . . . . ? Ni1 N12 C17 C16 -5.4(4) . . . . ? N13 N12 C17 C170 2.6(4) . . . . ? Ni1 N12 C17 C170 171.6(2) . . . . ? C11 C16 C17 N12 29.7(4) . . . . ? C15 C16 C17 N12 -151.0(3) . . . . ? C11 C16 C17 C170 -147.3(3) . . . . ? C15 C16 C17 C170 32.0(4) . . . . ? C19 N14 C18 N13 176.1(3) . . . . ? C20 N14 C18 N13 -2.8(4) . . . . ? C19 N14 C18 S1 -4.8(5) . . . . ? C20 N14 C18 S1 176.3(2) . . . . ? N12 N13 C18 N14 -177.1(2) . . . . ? N12 N13 C18 S1 3.8(3) . . . . ? Ni1 S1 C18 N14 155.6(2) . . . . ? Ni1 S1 C18 N13 -25.3(2) . . . . ? Ni1 O21 C21 N21 138.57(18) . . . . ? O2 O21 C21 N21 -66.8(3) . . . . ? Ni1 O21 C21 C26 -43.1(3) . . . . ? O2 O21 C21 C26 111.6(3) . . . . ? C23 N21 C21 O21 -179.2(2) . . . . ? C23 N21 C21 C26 2.3(4) . . . . ? C21 N21 C23 O23 180.0(3) . . . . ? C21 N21 C23 N25 0.9(4) . . . . ? C25 N25 C23 O23 178.8(3) . . . . ? C25 N25 C23 N21 -2.2(4) . . . . ? C23 N25 C25 O25 178.8(3) . . . . ? C23 N25 C25 C26 0.1(4) . . . . ? O25 C25 C26 C21 -175.3(3) . . . . ? N25 C25 C26 C21 3.3(4) . . . . ? O25 C25 C26 C27 5.9(4) . . . . ? N25 C25 C26 C27 -175.5(2) . . . . ? O21 C21 C26 C25 177.3(2) . . . . ? N21 C21 C26 C25 -4.4(3) . . . . ? O21 C21 C26 C27 -3.9(4) . . . . ? N21 C21 C26 C27 174.4(2) . . . . ? N23 N22 C27 C26 -177.7(2) . . . . ? Ni1 N22 C27 C26 -13.9(3) . . . . ? N23 N22 C27 C270 -1.9(3) . . . . ? Ni1 N22 C27 C270 161.93(19) . . . . ? C25 C26 C27 N22 -144.5(2) . . . . ? C21 C26 C27 N22 36.8(3) . . . . ? C25 C26 C27 C270 39.6(3) . . . . ? C21 C26 C27 C270 -139.1(2) . . . . ? C30 N24 C28 N23 -9.7(4) . . . . ? C29 N24 C28 N23 171.7(3) . . . . ? C30 N24 C28 S2 168.7(3) . . . . ? C29 N24 C28 S2 -9.9(4) . . . . ? N22 N23 C28 N24 179.4(2) . . . . ? N22 N23 C28 S2 1.0(3) . . . . ? Ni1 S2 C28 N24 159.1(2) . . . . ? Ni1 S2 C28 N23 -22.6(2) . . . . ? O23 O1 O2 O11 -96.10(8) 2_666 . . . ? O25 O1 O2 O11 169.29(10) 1_655 . . . ? O23 O1 O2 O21 -51.37(7) 2_666 . . . ? O25 O1 O2 O21 -145.98(9) 1_655 . . . ? C11 O11 O2 O1 -90.40(15) . . . . ? Ni1 O11 O2 O1 28.69(7) . . . . ? C11 O11 O2 O21 -144.30(16) . . . . ? Ni1 O11 O2 O21 -25.21(6) . . . . ? C21 O21 O2 O1 97.5(3) . . . . ? Ni1 O21 O2 O1 -105.55(6) . . . . ? C21 O21 O2 O11 -132.5(3) . . . . ? Ni1 O21 O2 O11 24.40(6) . . . . ? 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 N13 H13 O1 0.86 2.46 2.955(3) 116.9 . N21 H21 O23 0.86 2.01 2.854(3) 167.7 2_666 N23 H23 O2 0.86 2.26 2.789(3) 119.6 2_665 N25 H25 O25 0.86 2.03 2.883(3) 173.3 2_566 O1 H1A O23 0.94 1.77 2.710(2) 173.7 2_666 O1 H1B O25 0.94 1.86 2.754(2) 158.5 1_655 O2 H2A O1 0.92 1.92 2.826 169.9 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 72.94 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.420 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 237 60 ' ' 2 0.402 0.351 0.765 11 1 ' ' 3 0.597 0.649 0.236 10 1 ' ' _platon_squeeze_details ; ; #============================================================================== data_02lg15 _database_code_depnum_ccdc_archive 'CCDC 871180' #TrackingRef 'ni_pd_pt.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H17 N5 O4 Pd S2, C2 H6 O S' _chemical_formula_sum 'C13 H23 N5 O5 Pd S3' _chemical_formula_weight 531.94 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' 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.547(2) _cell_length_b 13.218(4) _cell_length_c 13.463(4) _cell_angle_alpha 117.118(4) _cell_angle_beta 96.563(5) _cell_angle_gamma 92.827(5) _cell_volume 1023.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 909 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 26.02 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4391 _exptl_absorpt_correction_T_max 0.9403 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SMART CCD-1000 Bruker' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% none _diffrn_reflns_number 11191 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4154 _reflns_number_gt 3034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-Software (Bruker, 1997)' _computing_cell_refinement 'SMART-Software (Bruker, 1997)' _computing_data_reduction 'SAINT-Software (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0496P)^2^+0.2366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4154 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.17769(5) 0.84282(3) 0.15232(3) 0.03703(13) Uani 1 1 d . . . S1 S 0.4250(2) 0.76646(12) 0.21590(11) 0.0548(3) Uani 1 1 d . . . S2 S 0.09173(19) 0.94098(10) 0.32791(9) 0.0434(3) Uani 1 1 d . . . O11 O -0.0354(5) 0.9116(3) 0.0906(2) 0.0458(8) Uani 1 1 d . . . O13 O -0.5324(6) 0.9410(3) -0.1483(3) 0.0605(10) Uani 1 1 d . . . O15 O -0.1149(6) 0.6705(3) -0.3060(3) 0.0676(11) Uani 1 1 d . . . O21 O 0.0417(7) 0.8737(3) 0.3844(3) 0.0680(11) Uani 1 1 d . . . N11 N -0.2735(6) 0.9215(3) -0.0328(3) 0.0409(9) Uani 1 1 d . . . H11A H -0.3229 0.9739 0.0368 0.049 Uiso 1 1 d R . . N12 N 0.2599(5) 0.7528(3) 0.0004(3) 0.0333(8) Uani 1 1 d . . . N13 N 0.4382(6) 0.6959(3) -0.0055(3) 0.0462(10) Uani 1 1 d . . . N14 N 0.6955(6) 0.6463(4) 0.0855(4) 0.0576(11) Uani 1 1 d . . . N15 N -0.3039(6) 0.8139(3) -0.2243(3) 0.0434(9) Uani 1 1 d . . . H15A H -0.3770 0.7929 -0.2930 0.052 Uiso 1 1 d R . . C11 C -0.1024(7) 0.8725(4) -0.0144(3) 0.0360(10) Uani 1 1 d . . . C13 C -0.3794(7) 0.8959(4) -0.1361(4) 0.0433(11) Uani 1 1 d . . . C15 C -0.1413(7) 0.7533(4) -0.2178(4) 0.0430(11) Uani 1 1 d . . . C16 C -0.0209(7) 0.7910(3) -0.1071(3) 0.0343(9) Uani 1 1 d . . . C17 C 0.1688(7) 0.7414(4) -0.0953(4) 0.0359(10) Uani 1 1 d . . . C18 C 0.5239(7) 0.6993(4) 0.0870(4) 0.0444(11) Uani 1 1 d . . . C19 C 0.7673(8) 0.5809(5) -0.0217(5) 0.0618(15) Uani 1 1 d . . . H19A H 0.6980 0.5044 -0.0578 0.093 Uiso 1 1 d R . . H19B H 0.9139 0.5787 -0.0089 0.093 Uiso 1 1 d R . . H19C H 0.7372 0.6163 -0.0693 0.093 Uiso 1 1 d R . . C20 C 0.7840(9) 0.6263(5) 0.1775(5) 0.0671(16) Uani 1 1 d . . . H20A H 0.7390 0.6793 0.2460 0.101 Uiso 1 1 d R . . H20B H 0.9323 0.6370 0.1860 0.101 Uiso 1 1 d R . . H20C H 0.7392 0.5495 0.1616 0.101 Uiso 1 1 d R . . C21 C 0.2920(9) 1.0495(5) 0.4160(5) 0.0769(18) Uani 1 1 d . . . H21A H 0.2582 1.0880 0.4910 0.115 Uiso 1 1 d R . . H21B H 0.3088 1.1033 0.3873 0.115 Uiso 1 1 d R . . H21C H 0.4185 1.0162 0.4178 0.115 Uiso 1 1 d R . . C22 C -0.1146(9) 1.0248(5) 0.3270(5) 0.0723(17) Uani 1 1 d . . . H22A H -0.2380 0.9749 0.2829 0.108 Uiso 1 1 d R . . H22B H -0.0775 1.0733 0.2947 0.108 Uiso 1 1 d R . . H22C H -0.1388 1.0712 0.4030 0.108 Uiso 1 1 d R . . C170 C 0.2675(8) 0.6761(4) -0.1989(4) 0.0513(13) Uani 1 1 d . . . H17A H 0.4140 0.6809 -0.1772 0.077 Uiso 1 1 d R . . H17B H 0.2424 0.7083 -0.2497 0.077 Uiso 1 1 d R . . H17C H 0.2092 0.5973 -0.2359 0.077 Uiso 1 1 d R . . S3 S 0.6744(2) 0.37927(13) 0.49911(12) 0.0618(4) Uani 1 1 d . . . O31 O 0.5786(7) 0.2594(3) 0.4269(3) 0.0804(12) Uani 1 1 d . . . C31 C 0.9289(9) 0.3695(6) 0.5500(6) 0.087(2) Uani 1 1 d . . . H31A H 0.9250 0.3245 0.5892 0.130 Uiso 1 1 d R . . H31B H 0.9967 0.4448 0.6007 0.130 Uiso 1 1 d R . . H31C H 1.0036 0.3338 0.4877 0.130 Uiso 1 1 d R . . C32 C 0.5753(12) 0.4269(6) 0.6265(6) 0.097(2) Uani 1 1 d . . . H32A H 0.4299 0.4323 0.6134 0.146 Uiso 1 1 d R . . H32B H 0.6454 0.5008 0.6799 0.146 Uiso 1 1 d R . . H32C H 0.5961 0.3738 0.6561 0.146 Uiso 1 1 d 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 0.0430(2) 0.0384(2) 0.02650(19) 0.01264(14) 0.00299(13) 0.00729(14) S1 0.0632(8) 0.0613(8) 0.0405(7) 0.0235(6) 0.0036(6) 0.0238(7) S2 0.0539(7) 0.0445(7) 0.0280(6) 0.0138(5) 0.0055(5) 0.0065(6) O11 0.055(2) 0.0496(19) 0.0259(16) 0.0104(14) 0.0044(14) 0.0216(16) O13 0.068(2) 0.063(2) 0.0370(19) 0.0136(17) -0.0070(17) 0.0284(19) O15 0.069(2) 0.072(2) 0.0318(19) -0.0016(18) 0.0017(17) 0.023(2) O21 0.107(3) 0.057(2) 0.045(2) 0.0257(19) 0.022(2) 0.008(2) N11 0.049(2) 0.039(2) 0.0281(19) 0.0100(16) 0.0017(16) 0.0133(17) N12 0.036(2) 0.0312(18) 0.032(2) 0.0138(16) 0.0074(16) 0.0033(15) N13 0.043(2) 0.048(2) 0.044(2) 0.0168(19) 0.0098(18) 0.0126(18) N14 0.049(3) 0.064(3) 0.062(3) 0.030(2) 0.008(2) 0.020(2) N15 0.050(2) 0.048(2) 0.0217(18) 0.0088(17) -0.0035(16) 0.0078(19) C11 0.042(3) 0.036(2) 0.026(2) 0.0117(18) 0.0018(18) 0.0031(19) C13 0.051(3) 0.041(3) 0.033(3) 0.015(2) -0.001(2) 0.005(2) C15 0.044(3) 0.043(3) 0.031(2) 0.009(2) 0.006(2) 0.000(2) C16 0.040(2) 0.032(2) 0.028(2) 0.0124(18) 0.0046(18) -0.0009(19) C17 0.039(2) 0.034(2) 0.033(2) 0.0142(19) 0.0096(19) 0.0020(19) C18 0.038(3) 0.043(3) 0.051(3) 0.021(2) 0.001(2) 0.002(2) C19 0.050(3) 0.065(4) 0.076(4) 0.034(3) 0.018(3) 0.025(3) C20 0.060(3) 0.067(4) 0.076(4) 0.037(3) -0.006(3) 0.017(3) C21 0.077(4) 0.080(4) 0.044(3) 0.010(3) -0.008(3) -0.023(3) C22 0.080(4) 0.087(4) 0.041(3) 0.020(3) 0.013(3) 0.031(3) C170 0.060(3) 0.058(3) 0.036(3) 0.018(2) 0.018(2) 0.017(3) S3 0.0776(10) 0.0613(9) 0.0442(8) 0.0243(7) 0.0014(7) 0.0063(7) O31 0.092(3) 0.073(3) 0.053(2) 0.020(2) -0.025(2) -0.010(2) C31 0.071(4) 0.088(5) 0.070(4) 0.014(4) -0.003(3) 0.002(4) C32 0.119(6) 0.102(6) 0.072(5) 0.033(4) 0.047(4) 0.027(5) _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 N12 1.997(3) . y Pd1 O11 2.003(3) . y Pd1 S1 2.2370(13) . y Pd1 S2 2.2734(13) . y S1 C18 1.769(5) . ? S2 O21 1.456(4) . ? S2 C21 1.758(5) . ? S2 C22 1.791(5) . ? O11 C11 1.276(5) . ? O13 C13 1.222(5) . ? O15 C15 1.232(5) . ? N11 C13 1.363(5) . ? N11 C11 1.375(5) . ? N11 H11A 0.9813 . ? N12 C17 1.294(5) . ? N12 N13 1.410(5) . ? N13 C18 1.287(6) . ? N14 C18 1.350(6) . ? N14 C20 1.445(6) . ? N14 C19 1.452(7) . ? N15 C13 1.358(6) . ? N15 C15 1.381(6) . ? N15 H15A 0.9020 . ? C11 C16 1.410(6) . ? C15 C16 1.452(6) . ? C16 C17 1.458(6) . ? C17 C170 1.508(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9599 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9599 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9599 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C170 H17A 0.9599 . ? C170 H17B 0.9600 . ? C170 H17C 0.9600 . ? S3 O31 1.486(4) . ? S3 C32 1.752(6) . ? S3 C31 1.761(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9599 . ? C32 H32B 0.9600 . ? C32 H32C 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 N12 Pd1 O11 91.68(13) . . y N12 Pd1 S1 86.26(10) . . y O11 Pd1 S1 177.40(10) . . y N12 Pd1 S2 177.65(10) . . y O11 Pd1 S2 90.62(9) . . y S1 Pd1 S2 91.46(5) . . ? C18 S1 Pd1 95.33(16) . . ? O21 S2 C21 108.4(3) . . ? O21 S2 C22 109.4(3) . . ? C21 S2 C22 100.6(3) . . ? O21 S2 Pd1 116.35(15) . . ? C21 S2 Pd1 109.9(2) . . ? C22 S2 Pd1 111.07(18) . . ? C11 O11 Pd1 123.8(3) . . ? C13 N11 C11 125.3(4) . . ? C13 N11 H11A 121.0 . . ? C11 N11 H11A 113.5 . . ? C17 N12 N13 115.1(3) . . ? C17 N12 Pd1 127.2(3) . . ? N13 N12 Pd1 117.7(3) . . ? C18 N13 N12 116.5(4) . . ? C18 N14 C20 123.6(5) . . ? C18 N14 C19 118.8(4) . . ? C20 N14 C19 115.8(4) . . ? C13 N15 C15 126.5(4) . . ? C13 N15 H15A 115.3 . . ? C15 N15 H15A 117.8 . . ? O11 C11 N11 112.1(4) . . ? O11 C11 C16 128.2(4) . . ? N11 C11 C16 119.7(4) . . ? O13 C13 N15 122.9(4) . . ? O13 C13 N11 122.9(4) . . ? N15 C13 N11 114.2(4) . . ? O15 C15 N15 117.0(4) . . ? O15 C15 C16 125.9(4) . . ? N15 C15 C16 117.0(4) . . ? C11 C16 C15 116.4(4) . . ? C11 C16 C17 123.2(4) . . ? C15 C16 C17 120.3(4) . . ? N12 C17 C16 123.3(4) . . ? N12 C17 C170 118.1(4) . . ? C16 C17 C170 118.6(4) . . ? N13 C18 N14 118.5(5) . . ? N13 C18 S1 123.5(4) . . ? N14 C18 S1 117.9(4) . . ? N14 C19 H19A 109.4 . . ? N14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 H20A 109.3 . . ? N14 C20 H20B 109.6 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.4 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.4 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C170 H17A 109.4 . . ? C17 C170 H17B 109.6 . . ? H17A C170 H17B 109.5 . . ? C17 C170 H17C 109.4 . . ? H17A C170 H17C 109.5 . . ? H17B C170 H17C 109.5 . . ? O31 S3 C32 106.1(3) . . ? O31 S3 C31 105.7(3) . . ? C32 S3 C31 97.7(3) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.4 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.4 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Pd1 S1 C18 6.72(18) . . . . ? O11 Pd1 S1 C18 -30(2) . . . . ? S2 Pd1 S1 C18 -173.82(16) . . . . ? N12 Pd1 S2 O21 -41(3) . . . . ? O11 Pd1 S2 O21 127.1(2) . . . . ? S1 Pd1 S2 O21 -54.4(2) . . . . ? N12 Pd1 S2 C21 82(3) . . . . ? O11 Pd1 S2 C21 -109.3(3) . . . . ? S1 Pd1 S2 C21 69.2(3) . . . . ? N12 Pd1 S2 C22 -167(3) . . . . ? O11 Pd1 S2 C22 1.1(3) . . . . ? S1 Pd1 S2 C22 179.6(2) . . . . ? N12 Pd1 O11 C11 15.7(4) . . . . ? S1 Pd1 O11 C11 53(2) . . . . ? S2 Pd1 O11 C11 -163.8(3) . . . . ? O11 Pd1 N12 C17 -8.5(4) . . . . ? S1 Pd1 N12 C17 173.1(4) . . . . ? S2 Pd1 N12 C17 160(2) . . . . ? O11 Pd1 N12 N13 170.6(3) . . . . ? S1 Pd1 N12 N13 -7.9(3) . . . . ? S2 Pd1 N12 N13 -21(3) . . . . ? C17 N12 N13 C18 -175.4(4) . . . . ? Pd1 N12 N13 C18 5.4(5) . . . . ? Pd1 O11 C11 N11 168.8(3) . . . . ? Pd1 O11 C11 C16 -12.6(7) . . . . ? C13 N11 C11 O11 -179.4(4) . . . . ? C13 N11 C11 C16 1.8(7) . . . . ? C15 N15 C13 O13 -175.3(5) . . . . ? C15 N15 C13 N11 2.9(7) . . . . ? C11 N11 C13 O13 179.1(4) . . . . ? C11 N11 C13 N15 0.9(7) . . . . ? C13 N15 C15 O15 169.4(5) . . . . ? C13 N15 C15 C16 -8.8(7) . . . . ? O11 C11 C16 C15 173.9(4) . . . . ? N11 C11 C16 C15 -7.6(6) . . . . ? O11 C11 C16 C17 -3.4(7) . . . . ? N11 C11 C16 C17 175.1(4) . . . . ? O15 C15 C16 C11 -167.4(5) . . . . ? N15 C15 C16 C11 10.6(6) . . . . ? O15 C15 C16 C17 10.0(7) . . . . ? N15 C15 C16 C17 -172.0(4) . . . . ? N13 N12 C17 C16 178.2(4) . . . . ? Pd1 N12 C17 C16 -2.8(6) . . . . ? N13 N12 C17 C170 -3.5(6) . . . . ? Pd1 N12 C17 C170 175.5(3) . . . . ? C11 C16 C17 N12 11.9(7) . . . . ? C15 C16 C17 N12 -165.3(4) . . . . ? C11 C16 C17 C170 -166.5(4) . . . . ? C15 C16 C17 C170 16.4(6) . . . . ? N12 N13 C18 N14 -179.7(4) . . . . ? N12 N13 C18 S1 2.1(6) . . . . ? C20 N14 C18 N13 -168.5(5) . . . . ? C19 N14 C18 N13 -4.5(7) . . . . ? C20 N14 C18 S1 9.8(7) . . . . ? C19 N14 C18 S1 173.9(4) . . . . ? Pd1 S1 C18 N13 -7.0(4) . . . . ? Pd1 S1 C18 N14 174.8(4) . . . . ? 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 N11 H11A O13 0.98 1.82 2.786(5) 168.0 2_475 N15 H15A O31 0.90 1.92 2.813(5) 168.3 2_565 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.732 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.102 #============================================================================== data_02lg01 _database_code_depnum_ccdc_archive 'CCDC 871181' #TrackingRef 'ni_pd_pt.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H17 N5 O4 Pt S2, C2 H6 O S' _chemical_formula_sum 'C13 H23 N5 O5 Pt S3' _chemical_formula_weight 620.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6141(15) _cell_length_b 13.122(3) _cell_length_c 13.394(3) _cell_angle_alpha 116.863(3) _cell_angle_beta 96.683(4) _cell_angle_gamma 92.316(4) _cell_volume 1024.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 965 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 26.1 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 7.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2470 _exptl_absorpt_correction_T_max 0.6330 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SMART CCD-1000 Bruker' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11334 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4180 _reflns_number_gt 3429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Software (Bruker, 1997)' _computing_cell_refinement 'SMART Software (Bruker, 1997)' _computing_data_reduction 'SAINT Software (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4180 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Pt1 Pt 0.67787(4) 0.34434(2) 0.153523(18) 0.03643(9) Uani 1 1 d . . . S1 S 0.9288(3) 0.26862(17) 0.21646(14) 0.0539(5) Uani 1 1 d . . . O11 O 0.4598(7) 0.4107(4) 0.0906(3) 0.0455(11) Uani 1 1 d . . . O13 O -0.0388(8) 0.4373(4) -0.1486(4) 0.0583(13) Uani 1 1 d . . . O15 O 0.3857(8) 0.1705(5) -0.3071(4) 0.0701(16) Uani 1 1 d . . . N11 N 0.2230(8) 0.4205(4) -0.0329(4) 0.0421(12) Uani 1 1 d . . . H11 H 0.1903 0.4853 0.0293 0.051 Uiso 1 1 d R . . N12 N 0.7553(7) 0.2548(4) 0.0002(4) 0.0323(10) Uani 1 1 d . . . N13 N 0.9347(8) 0.1952(5) -0.0072(4) 0.0445(13) Uani 1 1 d . . . N14 N 1.1899(9) 0.1425(5) 0.0830(5) 0.0560(15) Uani 1 1 d . . . N15 N 0.1930(8) 0.3121(5) -0.2249(4) 0.0445(13) Uani 1 1 d . . . H15 H 0.1040 0.3014 -0.2933 0.053 Uiso 1 1 d R . . C11 C 0.3929(9) 0.3722(5) -0.0149(5) 0.0367(13) Uani 1 1 d . . . C13 C 0.1154(10) 0.3934(6) -0.1372(5) 0.0448(15) Uani 1 1 d . . . C15 C 0.3560(10) 0.2524(6) -0.2186(5) 0.0421(15) Uani 1 1 d . . . C16 C 0.4770(9) 0.2906(5) -0.1067(5) 0.0357(13) Uani 1 1 d . . . C17 C 0.6650(9) 0.2410(5) -0.0968(5) 0.0391(14) Uani 1 1 d . . . C18 C 1.0213(10) 0.1992(6) 0.0866(5) 0.0448(15) Uani 1 1 d . . . C19 C 1.2842(11) 0.1275(7) 0.1771(7) 0.064(2) Uani 1 1 d . . . H19A H 1.4291 0.1483 0.1895 0.096 Uiso 1 1 calc R . . H19B H 1.2585 0.0486 0.1609 0.096 Uiso 1 1 calc R . . H19C H 1.2278 0.1755 0.2438 0.096 Uiso 1 1 calc R . . C20 C 1.2633(12) 0.0779(7) -0.0239(6) 0.064(2) Uani 1 1 d . . . H20A H 1.2033 -0.0003 -0.0583 0.095 Uiso 1 1 calc R . . H20B H 1.4096 0.0802 -0.0108 0.095 Uiso 1 1 calc R . . H20C H 1.2255 0.1112 -0.0733 0.095 Uiso 1 1 calc R . . C170 C 0.7618(10) 0.1747(6) -0.2013(5) 0.0526(17) Uani 1 1 d . . . H17A H 0.7415 0.2094 -0.2508 0.079 Uiso 1 1 calc R . . H17B H 0.6997 0.0967 -0.2398 0.079 Uiso 1 1 calc R . . H17C H 0.9058 0.1758 -0.1798 0.079 Uiso 1 1 calc R . . S2 S 0.5914(3) 0.44121(14) 0.32663(12) 0.0422(4) Uani 1 1 d . . . O21 O 0.5456(9) 0.3735(4) 0.3838(4) 0.0640(14) Uani 1 1 d . . . C21 C 0.3860(12) 0.5227(7) 0.3249(6) 0.066(2) Uani 1 1 d . . . H21A H 0.2650 0.4719 0.2814 0.099 Uiso 1 1 calc R . . H21B H 0.4195 0.5711 0.2914 0.099 Uiso 1 1 calc R . . H21C H 0.3618 0.5695 0.4010 0.099 Uiso 1 1 calc R . . C22 C 0.7885(13) 0.5506(8) 0.4143(6) 0.079(3) Uani 1 1 d . . . H22A H 0.7584 0.5868 0.4904 0.118 Uiso 1 1 calc R . . H22B H 0.7983 0.6067 0.3871 0.118 Uiso 1 1 calc R . . H22C H 0.9160 0.5180 0.4130 0.118 Uiso 1 1 calc R . . S3 S 0.8263(3) 0.12048(18) 0.50050(16) 0.0631(5) Uani 1 1 d . . . O31 O 0.9216(9) 0.2400(5) 0.5727(4) 0.0788(17) Uani 1 1 d . . . C31 C 0.5743(13) 0.1319(9) 0.4499(8) 0.091(3) Uani 1 1 d . . . H31A H 0.5031 0.1724 0.5128 0.136 Uiso 1 1 calc R . . H31B H 0.5044 0.0565 0.4031 0.136 Uiso 1 1 calc R . . H31C H 0.5782 0.1731 0.4063 0.136 Uiso 1 1 calc R . . C32 C 0.9262(16) 0.0705(9) 0.3724(8) 0.098(3) Uani 1 1 d . . . H32A H 0.9927 0.1342 0.3676 0.147 Uiso 1 1 calc R . . H32B H 0.8169 0.0327 0.3100 0.147 Uiso 1 1 calc R . . H32C H 1.0235 0.0173 0.3695 0.147 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 Pt1 0.04200(15) 0.04000(15) 0.02492(12) 0.01346(10) 0.00183(9) 0.00648(10) S1 0.0590(11) 0.0624(12) 0.0396(9) 0.0235(8) 0.0009(8) 0.0193(9) O11 0.058(3) 0.052(3) 0.022(2) 0.0129(19) 0.0016(18) 0.018(2) O13 0.066(3) 0.064(3) 0.032(2) 0.012(2) -0.005(2) 0.026(3) O15 0.067(3) 0.081(4) 0.029(2) -0.004(2) 0.000(2) 0.023(3) N11 0.051(3) 0.044(3) 0.025(2) 0.010(2) -0.001(2) 0.015(3) N12 0.034(3) 0.035(3) 0.029(2) 0.015(2) 0.009(2) -0.006(2) N13 0.042(3) 0.049(3) 0.044(3) 0.021(3) 0.009(2) 0.011(3) N14 0.049(3) 0.068(4) 0.056(4) 0.031(3) 0.005(3) 0.022(3) N15 0.050(3) 0.053(3) 0.026(2) 0.015(2) 0.000(2) 0.007(3) C11 0.044(3) 0.035(3) 0.030(3) 0.015(3) 0.002(2) 0.005(3) C13 0.055(4) 0.045(4) 0.029(3) 0.015(3) -0.005(3) 0.006(3) C15 0.043(4) 0.048(4) 0.028(3) 0.011(3) 0.005(3) 0.005(3) C16 0.037(3) 0.041(3) 0.028(3) 0.016(3) -0.001(2) 0.000(3) C17 0.043(3) 0.038(3) 0.034(3) 0.014(3) 0.008(3) 0.004(3) C18 0.046(4) 0.043(4) 0.044(4) 0.021(3) -0.002(3) 0.002(3) C19 0.053(4) 0.065(5) 0.072(5) 0.032(4) -0.004(4) 0.011(4) C20 0.058(5) 0.070(5) 0.066(5) 0.029(4) 0.020(4) 0.027(4) C170 0.053(4) 0.066(5) 0.038(3) 0.020(3) 0.014(3) 0.014(4) S2 0.0524(9) 0.0450(9) 0.0250(7) 0.0132(7) 0.0025(6) 0.0055(7) O21 0.102(4) 0.059(3) 0.038(3) 0.026(2) 0.020(3) 0.007(3) C21 0.083(6) 0.077(6) 0.039(4) 0.022(4) 0.018(4) 0.036(5) C22 0.086(6) 0.078(6) 0.034(4) -0.002(4) -0.006(4) -0.025(5) S3 0.0792(14) 0.0663(13) 0.0420(10) 0.0247(9) 0.0028(9) 0.0098(11) O31 0.092(4) 0.075(4) 0.042(3) 0.013(3) -0.025(3) -0.010(3) C31 0.072(6) 0.095(7) 0.073(6) 0.016(5) -0.010(5) 0.002(5) C32 0.114(8) 0.101(8) 0.074(6) 0.028(6) 0.044(6) 0.019(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 Pt1 N12 1.994(4) . y Pt1 O11 2.008(4) . y Pt1 S1 2.2398(17) . y Pt1 S2 2.2412(15) . y S1 C18 1.758(7) . ? O11 C11 1.280(7) . ? O13 C13 1.219(7) . ? O15 C15 1.232(7) . ? N11 C11 1.362(7) . ? N11 C13 1.372(7) . ? N11 H11 0.9385 . ? N12 C17 1.294(7) . ? N12 N13 1.435(7) . ? N13 C18 1.297(8) . ? N14 C18 1.358(8) . ? N14 C19 1.439(9) . ? N14 C20 1.449(9) . ? N15 C13 1.355(8) . ? N15 C15 1.374(8) . ? N15 H15 0.9781 . ? C11 C16 1.409(8) . ? C15 C16 1.466(8) . ? C16 C17 1.446(8) . ? C17 C170 1.510(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C170 H17A 0.9600 . ? C170 H17B 0.9600 . ? C170 H17C 0.9600 . ? S2 O21 1.454(5) . ? S2 C22 1.763(7) . ? S2 C21 1.767(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? S3 O31 1.484(6) . ? S3 C32 1.759(8) . ? S3 C31 1.763(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 N12 Pt1 O11 90.73(18) . . y N12 Pt1 S1 86.70(14) . . y O11 Pt1 S1 177.21(12) . . y N12 Pt1 S2 178.59(14) . . y O11 Pt1 S2 90.30(12) . . y S1 Pt1 S2 92.29(6) . . y C18 S1 Pt1 95.6(2) . . ? C11 O11 Pt1 124.6(4) . . ? C11 N11 C13 125.0(5) . . ? C11 N11 H11 117.1 . . ? C13 N11 H11 117.1 . . ? C17 N12 N13 113.6(5) . . ? C17 N12 Pt1 129.1(4) . . ? N13 N12 Pt1 117.3(3) . . ? C18 N13 N12 115.8(5) . . ? C18 N14 C19 123.1(6) . . ? C18 N14 C20 120.0(6) . . ? C19 N14 C20 116.2(6) . . ? C13 N15 C15 127.0(5) . . ? C13 N15 H15 105.7 . . ? C15 N15 H15 127.2 . . ? O11 C11 N11 112.2(5) . . ? O11 C11 C16 127.1(5) . . ? N11 C11 C16 120.7(5) . . ? O13 C13 N15 123.5(5) . . ? O13 C13 N11 122.5(6) . . ? N15 C13 N11 114.0(5) . . ? O15 C15 N15 117.2(6) . . ? O15 C15 C16 125.7(6) . . ? N15 C15 C16 117.0(5) . . ? C11 C16 C17 124.9(5) . . ? C11 C16 C15 115.5(5) . . ? C17 C16 C15 119.6(5) . . ? N12 C17 C16 121.5(5) . . ? N12 C17 C170 119.1(5) . . ? C16 C17 C170 119.4(5) . . ? N13 C18 N14 117.6(6) . . ? N13 C18 S1 124.1(5) . . ? N14 C18 S1 118.2(5) . . ? N14 C19 H19A 109.5 . . ? N14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N14 C20 H20A 109.5 . . ? N14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C170 H17A 109.5 . . ? C17 C170 H17B 109.5 . . ? H17A C170 H17B 109.5 . . ? C17 C170 H17C 109.5 . . ? H17A C170 H17C 109.5 . . ? H17B C170 H17C 109.5 . . ? O21 S2 C22 108.4(4) . . ? O21 S2 C21 109.4(4) . . ? C22 S2 C21 101.2(5) . . ? O21 S2 Pt1 116.2(2) . . ? C22 S2 Pt1 109.4(3) . . ? C21 S2 Pt1 111.3(2) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O31 S3 C32 106.5(4) . . ? O31 S3 C31 105.9(4) . . ? C32 S3 C31 98.4(5) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Pt1 S1 C18 5.6(3) . . . . ? O11 Pt1 S1 C18 -17(3) . . . . ? S2 Pt1 S1 C18 -175.4(2) . . . . ? N12 Pt1 O11 C11 14.3(5) . . . . ? S1 Pt1 O11 C11 37(3) . . . . ? S2 Pt1 O11 C11 -164.8(5) . . . . ? O11 Pt1 N12 C17 -8.2(5) . . . . ? S1 Pt1 N12 C17 172.9(5) . . . . ? S2 Pt1 N12 C17 129(5) . . . . ? O11 Pt1 N12 N13 172.4(4) . . . . ? S1 Pt1 N12 N13 -6.5(4) . . . . ? S2 Pt1 N12 N13 -51(6) . . . . ? C17 N12 N13 C18 -174.9(6) . . . . ? Pt1 N12 N13 C18 4.6(7) . . . . ? Pt1 O11 C11 N11 169.7(4) . . . . ? Pt1 O11 C11 C16 -10.8(9) . . . . ? C13 N11 C11 O11 -178.2(6) . . . . ? C13 N11 C11 C16 2.3(10) . . . . ? C15 N15 C13 O13 -174.6(7) . . . . ? C15 N15 C13 N11 3.8(10) . . . . ? C11 N11 C13 O13 178.3(6) . . . . ? C11 N11 C13 N15 -0.1(10) . . . . ? C13 N15 C15 O15 170.0(7) . . . . ? C13 N15 C15 C16 -9.0(10) . . . . ? O11 C11 C16 C17 -4.3(10) . . . . ? N11 C11 C16 C17 175.1(6) . . . . ? O11 C11 C16 C15 173.4(6) . . . . ? N11 C11 C16 C15 -7.2(9) . . . . ? O15 C15 C16 C11 -168.8(7) . . . . ? N15 C15 C16 C11 10.1(9) . . . . ? O15 C15 C16 C17 9.0(11) . . . . ? N15 C15 C16 C17 -172.1(6) . . . . ? N13 N12 C17 C16 177.3(5) . . . . ? Pt1 N12 C17 C16 -2.1(9) . . . . ? N13 N12 C17 C170 -4.5(8) . . . . ? Pt1 N12 C17 C170 176.1(4) . . . . ? C11 C16 C17 N12 11.3(10) . . . . ? C15 C16 C17 N12 -166.3(6) . . . . ? C11 C16 C17 C170 -166.9(6) . . . . ? C15 C16 C17 C170 15.5(9) . . . . ? N12 N13 C18 N14 179.1(5) . . . . ? N12 N13 C18 S1 1.5(9) . . . . ? C19 N14 C18 N13 -171.6(7) . . . . ? C20 N14 C18 N13 -1.7(10) . . . . ? C19 N14 C18 S1 6.1(10) . . . . ? C20 N14 C18 S1 176.0(6) . . . . ? Pt1 S1 C18 N13 -5.7(6) . . . . ? Pt1 S1 C18 N14 176.8(5) . . . . ? N12 Pt1 S2 O21 -10(6) . . . . ? O11 Pt1 S2 O21 126.5(3) . . . . ? S1 Pt1 S2 O21 -54.5(3) . . . . ? N12 Pt1 S2 C22 113(6) . . . . ? O11 Pt1 S2 C22 -110.4(4) . . . . ? S1 Pt1 S2 C22 68.6(4) . . . . ? N12 Pt1 S2 C21 -136(6) . . . . ? O11 Pt1 S2 C21 0.5(4) . . . . ? S1 Pt1 S2 C21 179.5(3) . . . . ? 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 N11 H11 O13 0.94 1.89 2.766(7) 154.0 2_565 N15 H15 O31 0.98 1.85 2.807(7) 164.0 1_454 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.704 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.143 #============================================================================== # End of Crystallographic Information File