Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _database_code_CSD 180738 # ---------------------------------------- # 1. SUBMISSION DETAILS # ---------------------------------------- _publ_contact_author_name 'Rudi van Eldik ' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Friedrich-Alexander-Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Germany ; _publ_contact_author_email vaneldik@chemie.uni-erlangen.de # _publ_contact_author_fax +49-9131-8527387 _publ_contact_author_phone +49-9131-8527350 _publ_requested_journal 'Dalton ' _publ_requested_category CM # ---------------------------------------- # 2. TITLE AND AUTHOR LIST # ---------------------------------------- _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Paper in Dalton. ; _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_section_title ; Kinetics and mechanism of the reations of [Pt(terpy)H2O]2+ with thiols in acidic aqueous solution. Synthesis and crystal structure of [Pt(terpy)(tu)](ClO4)2 (tu=thiourea) ; _publ_section_abstract ; The kinetics between [Pt(terpy)H2O]2+ and thiols were studied by using stopped-flow. The crystal structure of [Pt(terpy)(tu)](ClO4)2 was determined. ; loop_ _publ_author_name 'Zivadin Bugarcic ' _publ_author_address ; Institut f\"ur Anorganische Chemie Friedrich-Alexander-Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Germany ; 'Liehr, G\"unter' ; Institut f\"ur Anorganische Chemie Friedrich-Alexander-Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Germany ; 'Rudi van Eldik ' ; Institut f\"ur Anorganische Chemie Friedrich-Alexander-Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Germany ; # ---------------------------------------- # 3. CHEMICAL DATA # ---------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H15 Cl2 N5 O8 Pt S' _chemical_formula_weight 703.38 # ---------------------------------------- # 4. CRYSTAL DATA # ---------------------------------------- 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c' #(No. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.811(4) _cell_length_b 17.855(4) _cell_length_c 19.277(5) _cell_angle_alpha 90.00 _cell_angle_beta 150.888(10) _cell_angle_gamma 90.00 _cell_volume 2145.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 14.4 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max .38 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 6.944 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min .87 _exptl_absorpt_correction_T_max .91 _exptl_special_details ; Because of crystal decay it was necessary to stop data collection irregularly without adding another asymmetric unit to the data set. ; # ---------------------------------------- # 5. EXPERIMENTAL DATA # ---------------------------------------- _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device cad4 _diffrn_measurement_method w/2The _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3357 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 23.92 _reflns_number_total 3357 _reflns_number_gt 2438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PWCH (Gomm, 1993)' _computing_cell_refinement 'PWCH (Gomm, 1993)' _computing_data_reduction 'Inread (Liehr,1992)' _computing_structure_solution 'SHELXS-86 (Sheldrick,1990)' _computing_structure_solution 'SHELXS-86(Sheldrick,1990)' _computing_structure_solution 'SHELXS-86(Sheldrick,1990)' _computing_structure_solution 'SHELXS-86(Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93(Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-93(Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTON (Spek, 1998)' _computing_molecular_graphics 'PLUTON (Spek, 1998)' _computing_molecular_graphics ? _computing_publication_material ? # ---------------------------------------- # 6. REFINEMENT DATA # ---------------------------------------- _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, andR-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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3357 _refine_ls_number_parameters 298 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.368 _refine_ls_restrained_S_all 1.368 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ---------------------------------------- # 7. ATOMIC COORDINATES and ADP # ---------------------------------------- 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.08779(10) 0.08994(4) 0.07775(7) 0.0359(3) Uani 1 d . . . N1 N -0.161(2) 0.0849(7) -0.0039(16) 0.037(3) Uani 1 d . . . N2 N 0.209(2) 0.0158(9) 0.2212(16) 0.046(4) Uani 1 d . . . N3 N -0.117(2) 0.1611(9) -0.0915(14) 0.045(4) Uani 1 d . . . S S 0.3741(8) 0.0936(3) 0.1687(5) 0.0496(12) Uani 1 d . . . C17 C 0.576(3) 0.1396(8) 0.3277(17) 0.030(4) Uani 1 d . . . N4 N 0.549(2) 0.1774(8) 0.3696(16) 0.045(4) Uani 1 d . . . H4A H 0.6566 0.1988 0.4518 0.054 Uiso 1 calc R . . H4B H 0.4233 0.1808 0.3149 0.054 Uiso 1 calc R . . N5 N 0.773(2) 0.1359(10) 0.4156(17) 0.051(4) Uani 1 d . . . H5A H 0.8777 0.1578 0.4972 0.061 Uiso 1 calc R . . H5B H 0.7956 0.1115 0.3910 0.061 Uiso 1 calc R . . C1 C -0.143(3) 0.0419(11) 0.064(2) 0.045(5) Uani 1 d . . . C2 C 0.065(3) 0.0032(10) 0.1879(18) 0.040(4) Uani 1 d . . . C3 C 0.120(4) -0.0490(11) 0.271(2) 0.052(5) Uani 1 d . . . H3 H 0.0250 -0.0585 0.2521 0.063 Uiso 1 calc R . . C4 C 0.310(4) -0.0858(11) 0.379(2) 0.060(6) Uani 1 d . . . H4 H 0.3437 -0.1223 0.4315 0.072 Uiso 1 calc R . . C5 C 0.452(3) -0.0682(10) 0.410(2) 0.048(5) Uani 1 d . . . H5 H 0.5861 -0.0907 0.4866 0.058 Uiso 1 calc R . . C6 C 0.395(3) -0.0174(10) 0.3273(19) 0.044(5) Uani 1 d . . . H6 H 0.4901 -0.0063 0.3469 0.052 Uiso 1 calc R . . C7 C -0.333(3) 0.1254(11) -0.1230(19) 0.045(5) Uani 1 d . . . C8 C -0.305(3) 0.1679(11) -0.171(2) 0.049(5) Uani 1 d . . . C9 C -0.469(3) 0.2092(12) -0.295(2) 0.061(6) Uani 1 d . . . H9 H -0.6040 0.2110 -0.3520 0.073 Uiso 1 calc R . . C10 C -0.427(4) 0.2470(12) -0.329(2) 0.066(6) Uani 1 d . . . H10 H -0.5349 0.2758 -0.4115 0.079 Uiso 1 calc R . . C11 C -0.233(4) 0.2445(11) -0.248(2) 0.065(7) Uani 1 d . . . H11 H -0.2081 0.2709 -0.2744 0.078 Uiso 1 calc R . . C12 C -0.070(4) 0.2005(11) -0.123(2) 0.055(5) Uani 1 d . . . H12 H 0.0661 0.1986 -0.0629 0.066 Uiso 1 calc R . . C13 C -0.310(3) 0.0395(14) 0.013(2) 0.064(6) Uani 1 d . . . H13 H -0.2982 0.0133 0.0610 0.077 Uiso 1 calc R . . C14 C -0.501(4) 0.0784(12) -0.116(3) 0.061(7) Uani 1 d . . . H14 H -0.6208 0.0758 -0.1571 0.074 Uiso 1 calc R . . C15 C -0.505(4) 0.1199(14) -0.179(3) 0.071(7) Uani 1 d . . . H15 H -0.6307 0.1454 -0.2626 0.085 Uiso 1 calc R . . Cl1 Cl 0.1162(7) 0.2524(3) 0.2475(5) 0.0519(13) Uani 1 d D . . O1 O -0.0982(19) 0.2333(11) 0.1374(14) 0.098(6) Uani 1 d D . . O2 O 0.129(2) 0.2755(10) 0.1838(16) 0.091(6) Uani 1 d D . . O3 O 0.247(2) 0.1876(9) 0.3307(17) 0.092(6) Uani 1 d D . . O4 O 0.187(4) 0.3098(10) 0.333(2) 0.143(10) Uani 1 d D . . Cl2 Cl -0.0067(9) 0.0599(4) 0.3752(6) 0.0656(15) Uani 1 d D . . O5 O 0.032(5) 0.1042(11) 0.339(3) 0.198(16) Uani 1 d D . . O6 O 0.051(4) -0.0112(10) 0.389(3) 0.145(9) Uani 1 d D . . O7 O 0.121(4) 0.0857(18) 0.501(2) 0.24(2) Uani 1 d D . . O8 O -0.219(3) 0.0695(12) 0.267(2) 0.174(14) Uani 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 Pt 0.0364(4) 0.0355(4) 0.0318(4) -0.0066(3) 0.0293(4) -0.0050(3) N1 0.041(8) 0.024(8) 0.048(9) -0.011(7) 0.039(8) -0.008(6) N2 0.053(10) 0.047(10) 0.050(10) 0.012(8) 0.046(9) 0.012(8) N3 0.037(9) 0.044(10) 0.031(8) -0.002(7) 0.027(8) 0.004(7) S 0.046(3) 0.066(3) 0.044(3) -0.017(2) 0.040(3) -0.014(3) C17 0.035(9) 0.014(8) 0.032(9) -0.005(7) 0.029(9) -0.006(7) N4 0.039(8) 0.048(10) 0.038(9) -0.008(7) 0.032(8) -0.006(7) N5 0.050(10) 0.057(11) 0.048(10) -0.003(8) 0.043(9) 0.000(8) C1 0.054(12) 0.054(12) 0.049(11) -0.007(10) 0.049(11) -0.005(10) C2 0.058(11) 0.031(10) 0.035(10) -0.013(8) 0.041(10) -0.015(9) C3 0.078(15) 0.033(11) 0.070(14) -0.010(10) 0.068(14) -0.012(11) C4 0.087(16) 0.040(12) 0.049(12) -0.008(10) 0.059(13) -0.014(12) C5 0.066(13) 0.031(11) 0.043(11) -0.004(8) 0.047(11) 0.002(9) C6 0.055(12) 0.035(11) 0.050(12) 0.004(9) 0.047(11) 0.011(9) C7 0.036(10) 0.043(11) 0.033(10) 0.007(9) 0.027(10) 0.008(9) C8 0.039(11) 0.047(12) 0.035(10) -0.023(9) 0.029(10) -0.013(9) C9 0.046(12) 0.060(15) 0.044(12) -0.025(11) 0.035(12) -0.017(11) C10 0.074(16) 0.040(13) 0.048(13) -0.005(10) 0.048(14) 0.003(11) C11 0.102(19) 0.025(11) 0.064(15) 0.009(10) 0.072(16) 0.008(11) C12 0.078(14) 0.050(13) 0.059(13) -0.018(11) 0.063(13) -0.023(11) C13 0.051(13) 0.080(17) 0.075(16) -0.029(13) 0.057(14) -0.021(12) C14 0.058(13) 0.052(14) 0.094(18) -0.040(12) 0.069(15) -0.025(11) C15 0.075(16) 0.058(15) 0.079(17) 0.016(13) 0.068(16) 0.022(13) Cl1 0.048(3) 0.056(3) 0.039(3) 0.006(2) 0.036(2) 0.008(2) O1 0.053(10) 0.168(19) 0.070(11) 0.026(12) 0.054(10) 0.012(11) O2 0.085(12) 0.119(15) 0.076(11) 0.033(11) 0.071(11) 0.013(11) O3 0.090(12) 0.088(13) 0.098(13) 0.048(11) 0.082(12) 0.040(10) O4 0.18(2) 0.099(17) 0.107(16) -0.018(13) 0.122(18) 0.016(15) Cl2 0.066(4) 0.078(4) 0.065(4) 0.004(3) 0.059(3) 0.008(3) O5 0.31(4) 0.13(2) 0.36(5) 0.10(3) 0.32(4) 0.09(2) O6 0.22(3) 0.12(2) 0.21(3) 0.053(19) 0.20(2) 0.062(19) O7 0.13(2) 0.37(6) 0.13(3) -0.11(3) 0.10(2) -0.05(3) O8 0.098(17) 0.098(17) 0.20(3) -0.079(18) 0.11(2) -0.037(13) _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. ; # ---------------------------------------- # 8. MOLECULAR GEOMETRY # ---------------------------------------- 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 Pt N1 1.971(14) . ? Pt N3 2.045(15) . ? Pt N2 2.078(15) . ? Pt S 2.301(5) . ? N1 C1 1.35(2) . ? N1 C7 1.35(2) . ? N2 C6 1.30(2) . ? N2 C2 1.34(2) . ? N3 C8 1.31(2) . ? N3 C12 1.36(2) . ? S C17 1.705(16) . ? C17 N4 1.31(2) . ? C17 N5 1.33(2) . ? C1 C13 1.36(2) . ? C1 C2 1.47(3) . ? C2 C3 1.40(3) . ? C3 C4 1.36(3) . ? C4 C5 1.36(3) . ? C5 C6 1.37(3) . ? C7 C15 1.37(3) . ? C7 C8 1.47(3) . ? C8 C9 1.37(3) . ? C9 C10 1.35(3) . ? C10 C11 1.35(3) . ? C11 C12 1.41(3) . ? C13 C14 1.42(3) . ? C14 C15 1.38(3) . ? Cl1 O4 1.399(13) . ? Cl1 O1 1.407(12) . ? Cl1 O3 1.422(12) . ? Cl1 O2 1.431(12) . ? Cl2 O7 1.357(17) . ? Cl2 O8 1.362(15) . ? Cl2 O6 1.372(15) . ? Cl2 O5 1.396(16) . ? 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 Pt N3 80.0(6) . . ? N1 Pt N2 80.7(6) . . ? N3 Pt N2 160.7(6) . . ? N1 Pt S 178.5(4) . . ? N3 Pt S 99.7(5) . . ? N2 Pt S 99.6(4) . . ? C1 N1 C7 126.7(16) . . ? C1 N1 Pt 117.5(12) . . ? C7 N1 Pt 115.8(12) . . ? C6 N2 C2 122.8(17) . . ? C6 N2 Pt 126.3(14) . . ? C2 N2 Pt 110.9(12) . . ? C8 N3 C12 120.3(18) . . ? C8 N3 Pt 114.3(14) . . ? C12 N3 Pt 125.4(14) . . ? C17 S Pt 106.9(6) . . ? N4 C17 N5 118.0(15) . . ? N4 C17 S 123.4(13) . . ? N5 C17 S 118.6(13) . . ? N1 C1 C13 118.9(19) . . ? N1 C1 C2 112.3(15) . . ? C13 C1 C2 128.7(19) . . ? N2 C2 C3 117.2(18) . . ? N2 C2 C1 118.6(15) . . ? C3 C2 C1 124.1(18) . . ? C4 C3 C2 121(2) . . ? C3 C4 C5 118.5(19) . . ? C4 C5 C6 120(2) . . ? N2 C6 C5 121(2) . . ? N1 C7 C15 114.5(18) . . ? N1 C7 C8 114.4(17) . . ? C15 C7 C8 131.1(19) . . ? N3 C8 C9 123(2) . . ? N3 C8 C7 115.4(18) . . ? C9 C8 C7 121.5(19) . . ? C10 C9 C8 117(2) . . ? C9 C10 C11 123(2) . . ? C10 C11 C12 118(2) . . ? N3 C12 C11 119(2) . . ? C1 C13 C14 118(2) . . ? C15 C14 C13 118.9(19) . . ? C7 C15 C14 123(2) . . ? O4 Cl1 O1 111.1(12) . . ? O4 Cl1 O3 110.7(11) . . ? O1 Cl1 O3 109.1(9) . . ? O4 Cl1 O2 110.4(13) . . ? O1 Cl1 O2 108.1(8) . . ? O3 Cl1 O2 107.4(10) . . ? O7 Cl2 O8 111.6(15) . . ? O7 Cl2 O6 111.1(15) . . ? O8 Cl2 O6 115.4(14) . . ? O7 Cl2 O5 107.5(14) . . ? O8 Cl2 O5 105.5(15) . . ? O6 Cl2 O5 105.1(11) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 23.92 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 3.348 _refine_diff_density_min -2.952 _refine_diff_density_rms 0.366 #========END of CIF