# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1374 data_global _audit_creation_method 'shelxtl' _journal_date_recd_electronic '' _journal_date_accepted '' _journal_name_full 'Dalton Transactions' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _publ_contact_author_name 'Dr John D. Ranford' _publ_contact_author_address ; Department of Chemistry, National University of Singapore SINGAPORE 119 260 ; _publ_contact_author_email chmjdr@nus.edu.sg _publ_contact_author_fax '65 779 1691' _publ_contact_author_phone '65 874 2665' _publ_section_title ; Crystal structure of the anti-cancer analogue cis,trans,cis- [PtCl2(OCOCH3)2(NH3)2] and its reduction by cysteine and methionine ; loop_ _publ_author_name _publ_author_address 'Lee, Pen Foo' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Chen Lie' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Ranford, John D.' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; 'Vittal, Jagadese J.' ; Department National University of Singapore SINGAPORE 119 260 ; 'Wong, Siew Ying' ; Department of Chemistry National University of Singapore SINGAPORE 119 260 ; data_jdr19 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H14 Cl2 N2 O5 Pt' _chemical_formula_weight 436.16 _chemical_melting_point ? _chemical_compound_source 'see text' 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' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.9973(3) _cell_length_b 8.5722(1) _cell_length_c 11.1352(2) _cell_angle_alpha 90.00 _cell_angle_beta 126.769(1) _cell_angle_gamma 90.00 _cell_volume 1146.74(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3656 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 29.07 _exptl_crystal_description 'rectangular blocks' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.526 _exptl_crystal_density_method ? _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 12.701 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.0305 _exptl_absorpt_correction_T_max 0.1159 _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 'Siemens SMART CCD System' _diffrn_measurement_method 'frames \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3597 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 29.07 _reflns_number_total 1421 _reflns_number_observed 1385 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (Siemens, 1996)' _computing_molecular_graphics 'SHELXTL (Siemens, 1996)' _computing_publication_material 'SHELXTL (Siemens, 1996)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+4.0455P] 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 ; riding models; ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1421 _refine_ls_number_parameters 70 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_obs 0.0386 _refine_ls_wR_factor_all 0.0967 _refine_ls_wR_factor_obs 0.0965 _refine_ls_goodness_of_fit_all 1.114 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.113 _refine_ls_restrained_S_obs 1.126 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 2.226 _refine_diff_density_min -2.765 _refine_diff_density_rms 0.302 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.47715(4) 0.2500 0.0227(2) Uani 1 d S . Cl1 Cl -0.0810(2) 0.2880(2) 0.0643(2) 0.0368(4) Uani 1 d . . N1 N 0.0641(5) 0.6451(8) 0.4128(7) 0.0322(12) Uani 1 d . . H1A H 0.0526(38) 0.6179(30) 0.4797(32) 0.039 Uiso 1 calc R . H1B H 0.0306(30) 0.7358(15) 0.3712(10) 0.039 Uiso 1 calc R . H1C H 0.1368(9) 0.6546(43) 0.4582(39) 0.039 Uiso 1 calc R . O1 O 0.1277(5) 0.4703(6) 0.2338(7) 0.0315(12) Uani 1 d . . O2 O 0.2581(5) 0.5866(12) 0.4510(8) 0.064(2) Uani 1 d . . C1 C 0.2269(8) 0.5264(9) 0.3332(11) 0.036(2) Uani 1 d . . C2 C 0.3038(9) 0.5031(12) 0.2903(14) 0.048(2) Uani 1 d . . H2A H 0.2639(9) 0.4540(12) 0.1937(14) 0.072 Uiso 0.50 calc PR . H2B H 0.3649(9) 0.4380(12) 0.3634(14) 0.072 Uiso 0.50 calc PR . H2C H 0.3315(9) 0.6023(12) 0.2863(14) 0.072 Uiso 0.50 calc PR . H2D H 0.3764(9) 0.5422(12) 0.3686(14) 0.072 Uiso 0.50 calc PR . H2E H 0.2753(9) 0.5582(12) 0.1989(14) 0.072 Uiso 0.50 calc PR . H2F H 0.3087(9) 0.3939(12) 0.2759(14) 0.072 Uiso 0.50 calc PR . O1S O 0.0000 0.9367(14) 0.2500 0.058(2) Uani 1 d SD . H1S H -0.0384(114) 0.9954(107) 0.1598(68) 0.050 Uiso 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 Pt1 0.0189(2) 0.0254(3) 0.0219(2) 0.000 0.0113(2) 0.000 Cl1 0.0365(9) 0.0360(10) 0.0323(8) -0.0085(7) 0.0175(7) -0.0076(7) N1 0.029(3) 0.032(3) 0.037(3) -0.006(2) 0.020(2) -0.007(2) O1 0.019(3) 0.043(4) 0.030(3) -0.004(2) 0.014(2) -0.002(2) O2 0.035(3) 0.092(6) 0.063(4) -0.036(4) 0.028(3) -0.019(4) C1 0.026(4) 0.041(5) 0.041(5) -0.001(3) 0.021(4) -0.002(3) C2 0.028(5) 0.068(6) 0.048(6) 0.006(4) 0.024(5) 0.007(4) O1S 0.076(7) 0.037(5) 0.083(7) 0.000 0.059(6) 0.000 _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 O1 2.030(6) 2 ? Pt1 O1 2.030(6) . ? Pt1 N1 2.049(6) . ? Pt1 N1 2.049(6) 2 ? Pt1 Cl1 2.318(2) . ? Pt1 Cl1 2.318(2) 2 ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? O1 C1 1.303(11) . ? O2 C1 1.213(11) . ? C1 C2 1.502(14) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C2 H2D 0.96 . ? C2 H2E 0.96 . ? C2 H2F 0.96 . ? O1S H1S 0.949(10) . ? 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 O1 Pt1 O1 176.7(3) 2 . ? O1 Pt1 N1 84.8(2) 2 . ? O1 Pt1 N1 97.6(2) . . ? O1 Pt1 N1 97.6(2) 2 2 ? O1 Pt1 N1 84.8(2) . 2 ? N1 Pt1 N1 90.7(4) . 2 ? O1 Pt1 Cl1 92.3(2) 2 . ? O1 Pt1 Cl1 85.3(2) . . ? N1 Pt1 Cl1 177.1(2) . . ? N1 Pt1 Cl1 89.1(2) 2 . ? O1 Pt1 Cl1 85.3(2) 2 2 ? O1 Pt1 Cl1 92.3(2) . 2 ? N1 Pt1 Cl1 89.1(2) . 2 ? N1 Pt1 Cl1 177.1(2) 2 2 ? Cl1 Pt1 Cl1 91.23(10) . 2 ? Pt1 N1 H1A 109.5(2) . . ? Pt1 N1 H1B 109.5(2) . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5(2) . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C1 O1 Pt1 124.8(5) . . ? O2 C1 O1 125.5(8) . . ? O2 C1 C2 121.9(9) . . ? O1 C1 C2 112.5(8) . . ? C1 C2 H2A 109.5(6) . . ? C1 C2 H2B 109.5(5) . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5(5) . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C2 H2D 109.5(6) . . ? H2A C2 H2D 141.1 . . ? H2B C2 H2D 56.3 . . ? H2C C2 H2D 56.3 . . ? C1 C2 H2E 109.5(5) . . ? H2A C2 H2E 56.3 . . ? H2B C2 H2E 141.1 . . ? H2C C2 H2E 56.3 . . ? H2D C2 H2E 109.5 . . ? C1 C2 H2F 109.5(5) . . ? H2A C2 H2F 56.3 . . ? H2B C2 H2F 56.3 . . ? H2C C2 H2F 141.1 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 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 O1 Pt1 O1 C1 -118.1(6) 2 . . . ? N1 Pt1 O1 C1 16.8(6) . . . . ? N1 Pt1 O1 C1 106.8(6) 2 . . . ? Cl1 Pt1 O1 C1 -163.7(6) . . . . ? Cl1 Pt1 O1 C1 -72.6(6) 2 . . . ? Pt1 O1 C1 O2 2.2(13) . . . . ? Pt1 O1 C1 C2 179.7(5) . . . . ?