data_publication_text _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Stephen J. Lippard' _publ_contact_author_address ;77 Massachusetts Ave, 18-498 Cambridge, MA 02139 ; _publ_contact_author_email lippard@mit.edu _publ_contact_author_phone (617)253-1892 _publ_contact_author_fax (617)258-8150 loop_ _publ_author_name _publ_author_address 'Johnstone, Timothy C.' ;77 Massachusetts Ave, 18-443 Cambridge, MA 02139 ; 'Wilson, Justin J.' ;77 Massachusetts Ave, 18-425 Cambridge, MA 02139 ; 'Lippard, Stephen J.' ;77 Massachusetts Ave, 18-498 Cambridge, MA 02139 ; data_1*DMA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H17 Cl2 N3 O5 Pt' _chemical_formula_weight 477.22 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6011(8) _cell_length_b 8.9779(10) _cell_length_c 10.4662(11) _cell_angle_alpha 94.369(2) _cell_angle_beta 96.246(2) _cell_angle_gamma 107.314(2) _cell_volume 673.37(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9040 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 29.12 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 10.828 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4106 _exptl_absorpt_correction_T_max 0.6135 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13251 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 29.19 _reflns_number_total 3591 _reflns_number_gt 3345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms of the ammonia ligand were located on the difference map. They were refined semi-freely by constraining the N-H distances to 0.88 angstroms and constraining the displacement parameters of the hydrogen atoms to be 1.5 times those of the nitrogen atoms to which they are attached. ; _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^)+(0.0143P)^2^+0.9047P] 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 3591 _refine_ls_number_parameters 175 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0363 _refine_ls_wR_factor_gt 0.0351 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _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 0.609268(14) 0.299150(12) 0.643096(10) 0.01016(3) Uani 1 1 d . . . Cl1 Cl 0.36253(9) 0.08759(8) 0.67673(7) 0.01619(13) Uani 1 1 d . . . Cl2 Cl 0.68811(10) 0.38503(8) 0.86183(6) 0.01743(14) Uani 1 1 d . . . O3 O 0.4422(3) 0.4349(2) 0.61975(19) 0.0140(4) Uani 1 1 d . . . O1 O 0.7687(3) 0.1571(2) 0.6618(2) 0.0179(4) Uani 1 1 d . . . N1 N 0.5450(3) 0.2278(3) 0.4490(2) 0.0130(5) Uani 1 1 d D . . H1A H 0.541(5) 0.128(2) 0.435(3) 0.020 Uiso 1 1 d D . . H1B H 0.623(4) 0.286(4) 0.405(3) 0.020 Uiso 1 1 d D . . H1C H 0.436(3) 0.233(4) 0.418(3) 0.020 Uiso 1 1 d D . . O4 O 0.2218(3) 0.5208(2) 0.6858(2) 0.0158(4) Uani 1 1 d . . . O2 O 0.9378(3) 0.2433(2) 0.5022(2) 0.0211(5) Uani 1 1 d . . . N2 N 0.8199(3) 0.4898(3) 0.6135(2) 0.0128(4) Uani 1 1 d D . . H2A H 0.803(5) 0.577(3) 0.646(3) 0.019 Uiso 1 1 d D . . H2B H 0.826(5) 0.502(4) 0.5310(19) 0.019 Uiso 1 1 d D . . H2C H 0.928(3) 0.483(4) 0.649(3) 0.019 Uiso 1 1 d D . . C1 C 0.8954(4) 0.1591(4) 0.5862(3) 0.0178(6) Uani 1 1 d . . . H1 H 0.9619 0.0857 0.5986 0.021 Uiso 1 1 calc R . . C2 C 0.3262(4) 0.4406(3) 0.7005(3) 0.0143(5) Uani 1 1 d . . . H2 H 0.3220 0.3815 0.7723 0.017 Uiso 1 1 calc R . . O5 O 0.7706(3) 0.7738(2) 0.7228(2) 0.0182(4) Uani 1 1 d . . . N3 N 0.9249(4) 0.7979(3) 0.9224(2) 0.0187(5) Uani 1 1 d . . . C3 C 0.7757(4) 0.7962(3) 0.8427(3) 0.0182(6) Uani 1 1 d . . . C6 C 1.0834(4) 0.7689(4) 0.8680(3) 0.0230(7) Uani 1 1 d . . . H6A H 1.0733 0.6574 0.8671 0.034 Uiso 1 1 calc R . . H6B H 1.1996 0.8325 0.9212 0.034 Uiso 1 1 calc R . . H6C H 1.0831 0.7974 0.7795 0.034 Uiso 1 1 calc R . . C5 C 0.9298(5) 0.7927(4) 1.0615(3) 0.0228(6) Uani 1 1 d . . . H5A H 0.8341 0.8341 1.0917 0.034 Uiso 1 1 calc R . . H5B H 1.0525 0.8567 1.1057 0.034 Uiso 1 1 calc R . . H5C H 0.9060 0.6839 1.0807 0.034 Uiso 1 1 calc R . . C4 C 0.6118(5) 0.8241(4) 0.8984(3) 0.0281(7) Uani 1 1 d . . . H4A H 0.5412 0.8663 0.8346 0.042 Uiso 1 1 calc R . . H4B H 0.6564 0.8993 0.9766 0.042 Uiso 1 1 calc R . . H4C H 0.5313 0.7246 0.9204 0.042 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 0.00945(5) 0.01007(5) 0.01223(5) 0.00218(3) 0.00250(3) 0.00435(4) Cl1 0.0152(3) 0.0111(3) 0.0230(3) 0.0034(2) 0.0068(3) 0.0035(2) Cl2 0.0199(3) 0.0207(3) 0.0125(3) 0.0018(3) 0.0023(3) 0.0074(3) O3 0.0117(9) 0.0144(10) 0.0179(10) 0.0033(8) 0.0043(8) 0.0060(8) O1 0.0203(11) 0.0192(11) 0.0197(10) 0.0056(8) 0.0037(8) 0.0131(9) N1 0.0133(12) 0.0117(11) 0.0153(11) 0.0030(9) 0.0025(9) 0.0053(9) O4 0.0121(10) 0.0164(10) 0.0200(10) 0.0012(8) 0.0037(8) 0.0060(8) O2 0.0194(11) 0.0180(11) 0.0261(11) 0.0018(9) 0.0077(9) 0.0049(9) N2 0.0114(11) 0.0134(11) 0.0141(11) 0.0025(9) 0.0021(9) 0.0046(9) C1 0.0144(14) 0.0187(14) 0.0197(14) -0.0027(11) -0.0021(11) 0.0072(12) C2 0.0129(13) 0.0134(13) 0.0173(13) 0.0032(10) 0.0054(11) 0.0036(11) O5 0.0202(11) 0.0184(11) 0.0181(10) -0.0008(8) -0.0001(8) 0.0106(9) N3 0.0194(13) 0.0204(13) 0.0156(12) 0.0019(10) -0.0001(10) 0.0062(10) C3 0.0187(15) 0.0150(14) 0.0220(15) 0.0032(11) 0.0035(12) 0.0063(12) C6 0.0140(15) 0.0281(17) 0.0264(16) -0.0013(13) 0.0011(12) 0.0076(13) C5 0.0280(17) 0.0259(17) 0.0151(14) 0.0036(12) 0.0022(12) 0.0091(14) C4 0.0201(16) 0.040(2) 0.0268(17) -0.0036(15) 0.0046(13) 0.0147(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 Pt1 O1 2.010(2) . ? Pt1 O3 2.0138(19) . ? Pt1 N2 2.037(2) . ? Pt1 N1 2.043(2) . ? Pt1 Cl2 2.3135(7) . ? Pt1 Cl1 2.3183(7) . ? O3 C2 1.294(3) . ? O1 C1 1.308(3) . ? N1 H1A 0.886(18) . ? N1 H1B 0.865(18) . ? N1 H1C 0.874(18) . ? O4 C2 1.226(3) . ? O2 C1 1.211(4) . ? N2 H2A 0.875(18) . ? N2 H2B 0.883(18) . ? N2 H2C 0.887(18) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? O5 C3 1.249(4) . ? N3 C3 1.329(4) . ? N3 C5 1.457(4) . ? N3 C6 1.469(4) . ? C3 C4 1.509(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 O3 177.80(8) . . ? O1 Pt1 N2 95.08(9) . . ? O3 Pt1 N2 86.43(9) . . ? O1 Pt1 N1 90.51(9) . . ? O3 Pt1 N1 87.85(9) . . ? N2 Pt1 N1 91.48(10) . . ? O1 Pt1 Cl2 89.55(6) . . ? O3 Pt1 Cl2 92.13(6) . . ? N2 Pt1 Cl2 87.11(7) . . ? N1 Pt1 Cl2 178.59(7) . . ? O1 Pt1 Cl1 86.95(6) . . ? O3 Pt1 Cl1 91.54(6) . . ? N2 Pt1 Cl1 177.96(7) . . ? N1 Pt1 Cl1 88.65(7) . . ? Cl2 Pt1 Cl1 92.76(3) . . ? C2 O3 Pt1 120.67(18) . . ? C1 O1 Pt1 121.02(19) . . ? Pt1 N1 H1A 109(2) . . ? Pt1 N1 H1B 112(2) . . ? H1A N1 H1B 111(3) . . ? Pt1 N1 H1C 112(2) . . ? H1A N1 H1C 107(3) . . ? H1B N1 H1C 106(3) . . ? Pt1 N2 H2A 111(2) . . ? Pt1 N2 H2B 114(2) . . ? H2A N2 H2B 104(3) . . ? Pt1 N2 H2C 110(2) . . ? H2A N2 H2C 110(3) . . ? H2B N2 H2C 108(3) . . ? O2 C1 O1 127.6(3) . . ? O2 C1 H1 116.2 . . ? O1 C1 H1 116.2 . . ? O4 C2 O3 121.1(3) . . ? O4 C2 H2 119.4 . . ? O3 C2 H2 119.4 . . ? C3 N3 C5 124.3(3) . . ? C3 N3 C6 119.1(3) . . ? C5 N3 C6 115.3(3) . . ? O5 C3 N3 120.9(3) . . ? O5 C3 C4 119.9(3) . . ? N3 C3 C4 119.1(3) . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.19 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.772 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.130 #===END data_2*CH3CH2OH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H12 Cl2 N2 O2 Pt, C2 H6 O' _chemical_formula_sum 'C4 H18 Cl2 N2 O3 Pt' _chemical_formula_weight 408.19 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 P2(1)/c 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 11.2499(9) _cell_length_b 12.7069(10) _cell_length_c 8.0645(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.8720(10) _cell_angle_gamma 90.00 _cell_volume 1146.78(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.69 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 12.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3637 _exptl_absorpt_correction_T_max 0.7856 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22392 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.72 _reflns_number_total 2968 _reflns_number_gt 2457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+3.8052P] 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 2968 _refine_ls_number_parameters 118 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _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 1.142447(16) 1.124720(15) 0.777830(19) 0.01634(7) Uani 1 1 d . . . Cl1 Cl 1.07622(13) 0.95137(10) 0.75904(14) 0.0248(3) Uani 1 1 d . . . Cl2 Cl 1.31289(12) 1.08888(12) 0.64822(15) 0.0277(3) Uani 1 1 d . . . O2 O 1.2258(4) 1.1076(3) 1.0077(4) 0.0247(8) Uani 1 1 d . . . O1 O 1.0556(4) 1.1598(3) 0.5540(4) 0.0241(8) Uani 1 1 d . . . H1 H 0.9982 1.1180 0.5330 0.036 Uiso 1 1 calc R . . N1 N 1.1995(4) 1.2761(3) 0.8006(5) 0.0202(8) Uani 1 1 d . . . H1A H 1.1515 1.3126 0.8644 0.030 Uiso 1 1 calc R . . H1B H 1.1965 1.3061 0.6978 0.030 Uiso 1 1 calc R . . H1C H 1.2759 1.2774 0.8498 0.030 Uiso 1 1 calc R . . N2 N 0.9899(4) 1.1578(4) 0.8826(5) 0.0220(9) Uani 1 1 d . . . H2A H 0.9783 1.1084 0.9610 0.033 Uiso 1 1 calc R . . H2B H 0.9268 1.1574 0.8024 0.033 Uiso 1 1 calc R . . H2C H 0.9963 1.2224 0.9314 0.033 Uiso 1 1 calc R . . O1S O 1.2070(4) 0.8776(4) 0.3947(6) 0.0414(11) Uani 1 1 d D . . H1S H 1.232(9) 0.932(5) 0.450(11) 0.09(4) Uiso 1 1 d D . . C1 C 1.2946(5) 1.0165(5) 1.0456(6) 0.0268(11) Uani 1 1 d . . . H1D H 1.3229 0.9879 0.9424 0.032 Uiso 1 1 calc R . . H1E H 1.2448 0.9622 1.0929 0.032 Uiso 1 1 calc R . . C2 C 1.3995(6) 1.0419(6) 1.1681(8) 0.0413(15) Uani 1 1 d . . . H2D H 1.4465 1.0982 1.1234 0.062 Uiso 1 1 calc R . . H2E H 1.4494 0.9791 1.1882 0.062 Uiso 1 1 calc R . . H2F H 1.3713 1.0651 1.2732 0.062 Uiso 1 1 calc R . . C1S C 1.2676(6) 0.7934(6) 0.4877(9) 0.0431(16) Uani 1 1 d . . . H1S1 H 1.2401 0.7256 0.4371 0.052 Uiso 1 1 calc R . . H1S2 H 1.2446 0.7949 0.6030 0.052 Uiso 1 1 calc R . . C2S C 1.3993(7) 0.7982(7) 0.4945(10) 0.056(2) Uani 1 1 d . . . H2S1 H 1.4234 0.7910 0.3817 0.084 Uiso 1 1 calc R . . H2S2 H 1.4344 0.7410 0.5648 0.084 Uiso 1 1 calc R . . H2S3 H 1.4274 0.8660 0.5416 0.084 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 0.02026(11) 0.01881(10) 0.00975(9) -0.00009(6) 0.00055(6) -0.00060(7) Cl1 0.0359(7) 0.0210(6) 0.0170(5) -0.0014(4) 0.0002(5) -0.0048(5) Cl2 0.0277(7) 0.0356(7) 0.0207(6) -0.0003(5) 0.0067(5) 0.0047(6) O2 0.031(2) 0.028(2) 0.0134(16) -0.0050(13) -0.0043(14) 0.0057(16) O1 0.031(2) 0.0250(18) 0.0144(16) 0.0047(14) -0.0049(14) -0.0047(16) N1 0.023(2) 0.026(2) 0.0113(17) -0.0025(15) 0.0008(15) -0.0042(18) N2 0.024(2) 0.022(2) 0.020(2) 0.0016(16) 0.0011(16) -0.0017(18) O1S 0.035(3) 0.053(3) 0.034(2) 0.002(2) -0.0035(19) -0.007(2) C1 0.032(3) 0.029(3) 0.019(2) 0.003(2) 0.001(2) 0.002(2) C2 0.028(3) 0.048(4) 0.046(4) -0.005(3) -0.006(3) 0.010(3) C1S 0.046(4) 0.046(4) 0.038(3) 0.003(3) 0.006(3) -0.004(3) C2S 0.053(5) 0.057(5) 0.058(5) 0.001(4) 0.009(4) -0.001(4) _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 O2 2.002(3) . ? Pt1 O1 2.012(3) . ? Pt1 N1 2.030(4) . ? Pt1 N2 2.033(4) . ? Pt1 Cl2 2.3209(13) . ? Pt1 Cl1 2.3253(12) . ? O2 C1 1.408(6) . ? O1S C1S 1.438(8) . ? C1 C2 1.494(8) . ? C1S C2S 1.478(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 O2 Pt1 O1 173.22(15) . . ? O2 Pt1 N1 84.58(16) . . ? O1 Pt1 N1 89.48(16) . . ? O2 Pt1 N2 88.45(17) . . ? O1 Pt1 N2 88.52(17) . . ? N1 Pt1 N2 92.22(18) . . ? O2 Pt1 Cl2 93.75(12) . . ? O1 Pt1 Cl2 89.26(12) . . ? N1 Pt1 Cl2 87.63(13) . . ? N2 Pt1 Cl2 177.77(12) . . ? O2 Pt1 Cl1 94.24(11) . . ? O1 Pt1 Cl1 91.64(11) . . ? N1 Pt1 Cl1 178.50(11) . . ? N2 Pt1 Cl1 86.82(13) . . ? Cl2 Pt1 Cl1 93.37(5) . . ? C1 O2 Pt1 119.1(3) . . ? O2 C1 C2 110.2(5) . . ? O1S C1S C2S 114.1(6) . . ? 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 Pt1 O2 C1 -137.6(4) . . . . ? N2 Pt1 O2 C1 130.0(4) . . . . ? Cl2 Pt1 O2 C1 -50.4(4) . . . . ? Cl1 Pt1 O2 C1 43.3(4) . . . . ? Pt1 O2 C1 C2 146.5(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 O1 H1 O1S 0.84 2.44 3.062(7) 131.7 3_776 O1 H1 Cl1 0.84 2.57 3.131(4) 124.9 3_776 N1 H1A O1 0.91 1.99 2.852(6) 157.5 4_586 N1 H1B O2 0.91 1.94 2.828(5) 164.5 4_585 N1 H1C Cl2 0.91 2.94 3.420(4) 114.6 4_586 N2 H2A Cl1 0.91 2.52 3.357(4) 153.8 3_777 N2 H2B O1S 0.91 2.12 3.016(6) 167.3 3_776 N2 H2C O1 0.91 1.88 2.760(6) 162.6 4_586 O1S H1S Cl2 0.86(2) 2.66(2) 3.509(5) 175(9) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.421 _refine_diff_density_min -1.881 _refine_diff_density_rms 0.211 _iucr_refine_instructions_details ; TITL as in P2(1)/c CELL 0.71073 11.2499 12.7069 8.0645 90.000 95.872 90.000 ZERR 4.00 0.0009 0.0010 0.0006 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL PT UNIT 16 72 8 12 8 4 TEMP -173 L.S. 10 BOND CONF FMAP 2 PLAN 5 EQIV $1 -x+2, -y+2, -z+1 EQIV $2 x, -y+5/2, z+1/2 EQIV $3 x, -y+5/2, z-1/2 EQIV $4 -x+2, -y+2, -z+2 HTAB HTAB o1 o1s_$1 HTAB o1 cl1_$1 HTAB N1 o1_$2 HTAB N1 o2_$3 HTAB N1 Cl2_$2 HTAB N2 cl1_$4 HTAB N2 o1s_$1 HTAB N2 o1_$2 HTAB o1s Cl2 SIZE 0.020 0.040 0.100 ACTA DFIX 0.84 o1s H1s WGHT 0.035400 3.805200 FVAR 0.08298 PT1 6 1.142447 1.124720 0.777830 11.00000 0.02026 0.01881 = 0.00975 -0.00009 0.00055 -0.00060 CL1 5 1.076222 0.951369 0.759036 11.00000 0.03594 0.02102 = 0.01702 -0.00138 0.00023 -0.00476 CL2 5 1.312886 1.088876 0.648224 11.00000 0.02774 0.03560 = 0.02071 -0.00025 0.00667 0.00471 O2 4 1.225799 1.107588 1.007687 11.00000 0.03133 0.02812 = 0.01336 -0.00497 -0.00428 0.00574 O1 4 1.055637 1.159819 0.554019 11.00000 0.03129 0.02503 = 0.01438 0.00466 -0.00493 -0.00468 AFIX 147 H1 2 0.998206 1.118036 0.533029 11.00000 -1.50000 AFIX 0 N1 3 1.199465 1.276086 0.800598 11.00000 0.02326 0.02594 = 0.01131 -0.00253 0.00077 -0.00423 AFIX 137 H1A 2 1.151459 1.312554 0.864410 11.00000 -1.50000 H1B 2 1.196546 1.306117 0.697822 11.00000 -1.50000 H1C 2 1.275950 1.277444 0.849768 11.00000 -1.50000 AFIX 0 N2 3 0.989911 1.157815 0.882606 11.00000 0.02387 0.02154 = 0.02029 0.00157 0.00112 -0.00169 AFIX 137 H2A 2 0.978290 1.108385 0.960990 11.00000 -1.50000 H2B 2 0.926842 1.157444 0.802379 11.00000 -1.50000 H2C 2 0.996315 1.222431 0.931353 11.00000 -1.50000 AFIX 0 O1S 4 1.206964 0.877589 0.394693 11.00000 0.03549 0.05339 = 0.03389 0.00191 -0.00352 -0.00722 H1S 2 1.232435 0.931773 0.450436 11.00000 0.08834 C1 1 1.294649 1.016531 1.045630 11.00000 0.03174 0.02944 = 0.01892 0.00350 0.00108 0.00167 AFIX 23 H1D 2 1.322908 0.987930 0.942419 11.00000 -1.20000 H1E 2 1.244789 0.962221 1.092919 11.00000 -1.20000 AFIX 0 C2 1 1.399461 1.041917 1.168148 11.00000 0.02814 0.04809 = 0.04561 -0.00484 -0.00609 0.01003 AFIX 137 H2D 2 1.446475 1.098204 1.123427 11.00000 -1.50000 H2E 2 1.449392 0.979090 1.188166 11.00000 -1.50000 H2F 2 1.371264 1.065110 1.273214 11.00000 -1.50000 AFIX 0 C1S 1 1.267583 0.793433 0.487722 11.00000 0.04566 0.04565 = 0.03829 0.00342 0.00555 -0.00367 AFIX 23 H1S1 2 1.240091 0.725580 0.437064 11.00000 -1.20000 H1S2 2 1.244631 0.794860 0.602981 11.00000 -1.20000 AFIX 0 C2S 1 1.399295 0.798243 0.494547 11.00000 0.05309 0.05710 = 0.05838 0.00051 0.00869 -0.00059 AFIX 137 H2S1 2 1.423429 0.790957 0.381742 11.00000 -1.50000 H2S2 2 1.434351 0.740980 0.564818 11.00000 -1.50000 H2S3 2 1.427416 0.865981 0.541605 11.00000 -1.50000 HKLF 4 REM as in P2(1)/c REM R1 = 0.0266 for 2457 Fo > 4sig(Fo) and 0.0363 for all 2968 data REM 118 parameters refined using 1 restraints END WGHT 0.0354 3.8331 REM Highest difference peak 3.421, deepest hole -1.881, 1-sigma level 0.211 Q1 1 1.0809 1.1573 0.7806 11.00000 0.05 3.42 Q2 1 1.0852 1.0889 0.7759 11.00000 0.05 3.08 Q3 1 1.2005 1.0807 0.7975 11.00000 0.05 2.56 Q4 1 1.2018 1.1680 0.7945 11.00000 0.05 2.23 Q5 1 1.3624 1.1248 0.7074 11.00000 0.05 0.89 ; #===END data_3*DMSO _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Cl2 N2 O5 Pt, C2 H6 O S' _chemical_formula_sum 'C6 H18 Cl2 N2 O6 Pt S' _chemical_formula_weight 512.27 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.6918(10) _cell_length_b 13.2067(14) _cell_length_c 23.235(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2974.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 30.68 _exptl_crystal_description Shard _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 9.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3167 _exptl_absorpt_correction_T_max 0.7544 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57108 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.69 _reflns_number_total 3841 _reflns_number_gt 2862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+7.8080P] 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 3841 _refine_ls_number_parameters 173 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Pt1 Pt 0.246886(14) -0.807773(8) 0.329169(5) 0.01341(4) Uani 1 1 d . . . Cl2 Cl 0.41759(9) -0.68550(7) 0.33040(4) 0.02254(19) Uani 1 1 d . . . Cl5 Cl 0.31654(10) -0.87067(7) 0.41768(4) 0.0238(2) Uani 1 1 d . . . O1 O 0.3669(3) -0.9054(2) 0.28808(12) 0.0234(6) Uani 1 1 d D . . H1O H 0.436(3) -0.919(3) 0.3070(18) 0.035 Uiso 1 1 d D . . N2 N 0.0948(3) -0.9144(2) 0.32721(13) 0.0205(6) Uani 1 1 d . . . H2A H 0.0423 -0.9055 0.2951 0.031 Uiso 1 1 calc R . . H2B H 0.0409 -0.9080 0.3591 0.031 Uiso 1 1 calc R . . H2C H 0.1334 -0.9772 0.3265 0.031 Uiso 1 1 calc R . . N1 N 0.1945(3) -0.7597(2) 0.24914(13) 0.0172(6) Uani 1 1 d . . . H1A H 0.2667 -0.7256 0.2333 0.026 Uiso 1 1 calc R . . H1B H 0.1201 -0.7179 0.2515 0.026 Uiso 1 1 calc R . . H1C H 0.1732 -0.8141 0.2268 0.026 Uiso 1 1 calc R . . O2 O 0.1270(3) -0.70792(18) 0.37225(10) 0.0183(5) Uani 1 1 d . . . S1S S 0.88507(13) 0.16228(8) 0.46682(5) 0.0333(3) Uani 1 1 d . . . O3 O -0.0514(3) -0.7151(2) 0.31168(12) 0.0290(7) Uani 1 1 d . . . O1S O 0.9216(4) 0.0846(3) 0.42195(14) 0.0444(9) Uani 1 1 d . . . C1 C 0.0053(4) -0.6817(3) 0.35481(16) 0.0191(7) Uani 1 1 d . . . C2S C 0.7499(6) 0.1084(4) 0.5072(2) 0.0549(15) Uani 1 1 d . . . H2S1 H 0.6676 0.1021 0.4830 0.082 Uiso 1 1 calc R . . H2S2 H 0.7292 0.1519 0.5403 0.082 Uiso 1 1 calc R . . H2S3 H 0.7777 0.0412 0.5209 0.082 Uiso 1 1 calc R . . C1S C 1.0161(6) 0.1563(4) 0.5194(2) 0.0486(13) Uani 1 1 d . . . H1S1 H 1.0205 0.0876 0.5353 0.073 Uiso 1 1 calc R . . H1S2 H 0.9956 0.2045 0.5504 0.073 Uiso 1 1 calc R . . H1S3 H 1.1050 0.1735 0.5018 0.073 Uiso 1 1 calc R . . C2 C -0.0620(4) -0.6030(3) 0.39291(16) 0.0187(8) Uani 1 1 d . . . H2D H -0.0080 -0.5394 0.3911 0.022 Uiso 1 1 calc R . . H2E H -0.0612 -0.6271 0.4333 0.022 Uiso 1 1 calc R . . C4 C -0.2191(4) -0.5184(3) 0.32160(16) 0.0199(8) Uani 1 1 d . . . C3 C -0.2100(4) -0.5818(3) 0.37462(17) 0.0212(8) Uani 1 1 d . . . H3A H -0.2576 -0.6469 0.3677 0.025 Uiso 1 1 calc R . . H3B H -0.2585 -0.5468 0.4064 0.025 Uiso 1 1 calc R . . O4 O -0.3276(3) -0.5364(2) 0.28928(12) 0.0245(6) Uani 1 1 d D . . H4O H -0.340(5) -0.496(3) 0.2606(14) 0.037 Uiso 1 1 d D . . O5 O -0.1356(3) -0.4520(2) 0.30964(13) 0.0304(7) Uani 1 1 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 0.01152(6) 0.01303(6) 0.01567(6) -0.00171(5) 0.00005(6) 0.00048(6) Cl2 0.0168(4) 0.0248(4) 0.0260(4) -0.0033(4) 0.0018(4) -0.0074(4) Cl5 0.0279(5) 0.0219(4) 0.0215(4) 0.0026(4) -0.0040(4) 0.0043(4) O1 0.0200(14) 0.0248(14) 0.0255(15) -0.0084(12) -0.0048(12) 0.0087(12) N2 0.0203(16) 0.0204(15) 0.0206(16) -0.0031(13) 0.0037(13) -0.0038(13) N1 0.0154(14) 0.0188(15) 0.0175(15) -0.0024(13) 0.0011(12) 0.0003(12) O2 0.0160(12) 0.0215(13) 0.0175(12) -0.0053(10) -0.0032(10) 0.0030(10) S1S 0.0458(7) 0.0252(5) 0.0288(5) 0.0015(4) 0.0086(5) -0.0096(5) O3 0.0178(14) 0.0446(18) 0.0246(14) -0.0132(13) -0.0060(12) 0.0076(13) O1S 0.049(2) 0.049(2) 0.0346(18) -0.0152(16) 0.0222(16) -0.0242(17) C1 0.0163(17) 0.0221(19) 0.0188(17) 0.0033(15) 0.0020(14) -0.0021(15) C2S 0.071(4) 0.038(3) 0.055(3) -0.016(2) 0.038(3) -0.017(3) C1S 0.052(3) 0.055(3) 0.039(3) -0.016(2) 0.003(2) 0.011(3) C2 0.0192(18) 0.0186(18) 0.0183(18) -0.0023(14) -0.0013(15) 0.0046(15) C4 0.0146(17) 0.0197(17) 0.025(2) 0.0017(15) 0.0042(14) 0.0033(14) C3 0.0179(17) 0.0210(18) 0.0247(19) 0.0030(15) 0.0028(15) 0.0017(14) O4 0.0180(14) 0.0249(15) 0.0307(16) 0.0077(12) -0.0028(12) -0.0024(12) O5 0.0204(14) 0.0288(16) 0.0420(17) 0.0161(13) -0.0064(13) -0.0072(12) _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 1.982(3) . ? Pt1 O2 2.022(2) . ? Pt1 N1 2.029(3) . ? Pt1 N2 2.038(3) . ? Pt1 Cl2 2.3120(9) . ? Pt1 Cl5 2.3184(9) . ? O2 C1 1.294(4) . ? S1S O1S 1.505(3) . ? S1S C2S 1.762(5) . ? S1S C1S 1.764(5) . ? O3 C1 1.225(4) . ? C1 C2 1.513(5) . ? C2 C3 1.522(5) . ? C4 O5 1.224(4) . ? C4 O4 1.314(4) . ? C4 C3 1.492(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 O1 Pt1 O2 178.95(10) . . ? O1 Pt1 N1 84.78(12) . . ? O2 Pt1 N1 96.08(11) . . ? O1 Pt1 N2 87.96(12) . . ? O2 Pt1 N2 92.64(11) . . ? N1 Pt1 N2 90.84(12) . . ? O1 Pt1 Cl2 92.30(9) . . ? O2 Pt1 Cl2 87.10(7) . . ? N1 Pt1 Cl2 88.39(9) . . ? N2 Pt1 Cl2 179.16(10) . . ? O1 Pt1 Cl5 91.33(8) . . ? O2 Pt1 Cl5 87.82(7) . . ? N1 Pt1 Cl5 176.11(9) . . ? N2 Pt1 Cl5 89.02(9) . . ? Cl2 Pt1 Cl5 91.77(3) . . ? C1 O2 Pt1 122.9(2) . . ? O1S S1S C2S 105.6(2) . . ? O1S S1S C1S 106.3(2) . . ? C2S S1S C1S 98.5(3) . . ? O3 C1 O2 124.6(3) . . ? O3 C1 C2 122.2(3) . . ? O2 C1 C2 113.2(3) . . ? C1 C2 C3 111.7(3) . . ? O5 C4 O4 121.9(3) . . ? O5 C4 C3 123.4(3) . . ? O4 C4 C3 114.6(3) . . ? C4 C3 C2 112.9(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 Pt1 O2 C1 38.2(3) . . . . ? N2 Pt1 O2 C1 -52.9(3) . . . . ? Cl2 Pt1 O2 C1 126.3(3) . . . . ? Cl5 Pt1 O2 C1 -141.8(3) . . . . ? Pt1 O2 C1 O3 1.5(5) . . . . ? Pt1 O2 C1 C2 -177.7(2) . . . . ? O3 C1 C2 C3 6.5(5) . . . . ? O2 C1 C2 C3 -174.3(3) . . . . ? O5 C4 C3 C2 -33.4(5) . . . . ? O4 C4 C3 C2 149.0(3) . . . . ? C1 C2 C3 C4 -75.4(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 O1 H1O O5 0.820(19) 1.99(3) 2.722(4) 149(5) 8_655 N2 H2A O1 0.91 2.57 3.474(4) 169.8 6_556 N2 H2B O1S 0.91 1.87 2.769(4) 171.1 1_445 N2 H2C Cl2 0.91 2.80 3.584(3) 145.5 8_655 N1 H1A O3 0.91 2.05 2.900(4) 154.1 6_656 N1 H1B O3 0.91 2.17 2.853(4) 130.9 . N1 H1B Cl2 0.91 2.77 3.403(3) 127.9 6_556 N1 H1C O5 0.91 2.04 2.940(4) 168.9 3_545 O4 H4O O1 0.862(19) 1.67(2) 2.524(4) 172(5) 3 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.538 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.135 _iucr_refine_instructions_details ; TITL ag in Pbca CELL 0.71073 9.6918 13.2067 23.2351 90.000 90.000 90.000 ZERR 8.00 0.0010 0.0014 0.0024 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O CL PT S UNIT 48 144 16 48 16 8 8 TEMP -173 L.S. 10 BOND CONF SIZE 0.15 0.05 0.03 FMAP 2 PLAN 5 DFIX 0.84 o4 h4o o1 h1o SHEL 99999999 0.74 ACTA EQIV $1 -x+1/2, y-1/2, z EQIV $2 x-1/2, y, -z+1/2 EQIV $3 x-1, y-1, z EQIV $4 x+1/2, y, -z+1/2 EQIV $5 x+1/2, y, -z+1/2 EQIV $6 -x, y-1/2, -z+1/2 EQIV $7 -x, y+1/2, -z+1/2 HTAB HTAB o1 o5_$1 HTAB n2 o1_$2 HTAB n2 o1s_$3 HTAB n2 cl2_$1 HTAB n1 O3_$4 HTAB n1 o3 HTAB n1 o4_$5 HTAB n1 cl2_$2 HTAB n1 o5_$6 HTAB o4 o1_$7 WGHT 0.016000 7.808000 FVAR 0.04561 PT1 6 0.246886 -0.807773 0.329169 11.00000 0.01152 0.01303 = 0.01567 -0.00171 0.00005 0.00048 CL2 5 0.417591 -0.685502 0.330397 11.00000 0.01683 0.02482 = 0.02596 -0.00332 0.00178 -0.00740 CL5 5 0.316536 -0.870674 0.417677 11.00000 0.02792 0.02189 = 0.02154 0.00261 -0.00404 0.00433 O1 4 0.366949 -0.905405 0.288080 11.00000 0.01997 0.02483 = 0.02546 -0.00839 -0.00475 0.00866 H1O 2 0.435811 -0.918996 0.307040 11.00000 -1.50000 N2 3 0.094839 -0.914368 0.327212 11.00000 0.02034 0.02043 = 0.02059 -0.00313 0.00368 -0.00384 AFIX 137 H2A 2 0.042326 -0.905464 0.295142 11.00000 -1.50000 H2B 2 0.040941 -0.908034 0.359079 11.00000 -1.50000 H2C 2 0.133375 -0.977191 0.326542 11.00000 -1.50000 AFIX 0 N1 3 0.194508 -0.759708 0.249136 11.00000 0.01538 0.01879 = 0.01754 -0.00241 0.00108 0.00030 AFIX 137 H1A 2 0.266723 -0.725639 0.233275 11.00000 -1.50000 H1B 2 0.120117 -0.717868 0.251477 11.00000 -1.50000 H1C 2 0.173197 -0.814065 0.226768 11.00000 -1.50000 AFIX 0 O2 4 0.127032 -0.707920 0.372246 11.00000 0.01603 0.02146 = 0.01747 -0.00529 -0.00324 0.00304 S1S 7 0.885073 0.162278 0.466820 11.00000 0.04578 0.02515 = 0.02883 0.00150 0.00857 -0.00960 O3 4 -0.051383 -0.715139 0.311676 11.00000 0.01782 0.04463 = 0.02463 -0.01318 -0.00601 0.00761 O1S 4 0.921572 0.084555 0.421952 11.00000 0.04935 0.04913 = 0.03464 -0.01517 0.02217 -0.02418 C1 1 0.005310 -0.681719 0.354807 11.00000 0.01634 0.02211 = 0.01881 0.00332 0.00195 -0.00207 C2S 1 0.749898 0.108382 0.507222 11.00000 0.07147 0.03773 = 0.05541 -0.01558 0.03822 -0.01740 AFIX 137 H2S1 2 0.667590 0.102089 0.482984 11.00000 -1.50000 H2S2 2 0.729171 0.151870 0.540286 11.00000 -1.50000 H2S3 2 0.777745 0.041208 0.520869 11.00000 -1.50000 AFIX 0 C1S 1 1.016117 0.156310 0.519418 11.00000 0.05207 0.05457 = 0.03927 -0.01613 0.00343 0.01096 AFIX 137 H1S1 2 1.020520 0.087634 0.535288 11.00000 -1.50000 H1S2 2 0.995644 0.204458 0.550354 11.00000 -1.50000 H1S3 2 1.104977 0.173521 0.501827 11.00000 -1.50000 AFIX 0 C2 1 -0.061969 -0.602995 0.392915 11.00000 0.01924 0.01859 = 0.01833 -0.00232 -0.00131 0.00459 AFIX 23 H2D 2 -0.007985 -0.539433 0.391133 11.00000 -1.20000 H2E 2 -0.061242 -0.627071 0.433264 11.00000 -1.20000 AFIX 0 C4 1 -0.219059 -0.518351 0.321604 11.00000 0.01465 0.01968 = 0.02548 0.00172 0.00415 0.00330 C3 1 -0.209956 -0.581792 0.374616 11.00000 0.01788 0.02102 = 0.02470 0.00300 0.00282 0.00168 AFIX 23 H3A 2 -0.257632 -0.646947 0.367656 11.00000 -1.20000 H3B 2 -0.258524 -0.546818 0.406395 11.00000 -1.20000 AFIX 0 O4 4 -0.327551 -0.536448 0.289284 11.00000 0.01796 0.02495 = 0.03067 0.00766 -0.00278 -0.00243 H4O 2 -0.339618 -0.496059 0.260593 11.00000 -1.50000 O5 4 -0.135600 -0.452028 0.309637 11.00000 0.02039 0.02885 = 0.04196 0.01611 -0.00642 -0.00723 HKLF 4 REM ag in Pbca REM R1 = 0.0205 for 2862 Fo > 4sig(Fo) and 0.0366 for all 3841 data REM 173 parameters refined using 2 restraints END WGHT 0.0160 7.8084 REM Highest difference peak 1.538, deepest hole -1.219, 1-sigma level 0.135 Q1 1 0.2138 -0.8403 0.3525 11.00000 0.05 1.54 Q2 1 0.2054 -0.8451 0.3096 11.00000 0.05 0.83 Q3 1 0.2465 -0.7580 0.3538 11.00000 0.05 0.75 Q4 1 0.2503 -1.0356 0.3360 11.00000 0.05 0.56 Q5 1 0.2121 -0.7407 0.3123 11.00000 0.05 0.55 ; #===END