# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Francesco Paolo Fanizzi' _publ_contact_author_email FP.FANIZZI@UNILE.IT _publ_section_title ; Hard/Soft Selectivity in Ligand Substitution Reactions of beta-diketonate Platinum(II) Complexes ; loop_ _publ_author_name 'Francesco Paolo Fanizzi' 'Serena Capoccia' 'Antonella Ciccarese' 'Sandra A De Pascali' 'Maurizio Lanfranchi' ; L.Marchio ; 'Paride Papadia' # Attachment 'cifdep_rev.cif' #BEGIN data_ptacs1 _database_code_depnum_ccdc_archive 'CCDC 713088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H13 Cl O3 Pt S' _chemical_formula_sum 'C7 H13 Cl O3 Pt S' _chemical_formula_weight 407.77 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 17.718(11) _cell_length_b 7.245(8) _cell_length_c 18.793(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.57(2) _cell_angle_gamma 90.00 _cell_volume 2243(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour 0.35 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 12.907 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9022 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Walker & Stuart' _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 'Philips PW 1100' _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5007 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.01 _reflns_number_total 4877 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local programs' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0990P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4877 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 C1 C 0.1591(5) 0.0632(13) 0.2809(5) 0.035(2) Uani 1 1 d . . . C2 C 0.1203(5) 0.0941(16) 0.2028(5) 0.045(2) Uani 1 1 d . . . H2 H 0.0645 0.1122 0.1854 0.055 Uiso 1 1 calc R . . C3 C 0.1550(5) 0.1010(16) 0.1483(5) 0.041(2) Uani 1 1 d . . . C4 C 0.1113(6) 0.0523(15) 0.3316(6) 0.050(3) Uani 1 1 d . . . H4A H 0.1472 0.0276 0.3831 0.075 Uiso 1 1 calc R . . H4B H 0.0721 -0.0451 0.3142 0.075 Uiso 1 1 calc R . . H4C H 0.0839 0.1675 0.3300 0.075 Uiso 1 1 calc R . . C5 C 0.1028(5) 0.137(2) 0.0658(5) 0.064(3) Uani 1 1 d . . . H5A H 0.1361 0.1380 0.0354 0.096 Uiso 1 1 calc R . . H5B H 0.0765 0.2547 0.0617 0.096 Uiso 1 1 calc R . . H5C H 0.0626 0.0419 0.0478 0.096 Uiso 1 1 calc R . . C6 C 0.4814(5) 0.1968(13) 0.3904(5) 0.0367(19) Uani 1 1 d . . . H6A H 0.4535 0.3111 0.3892 0.055 Uiso 1 1 calc R . . H6B H 0.5024 0.1958 0.3500 0.055 Uiso 1 1 calc R . . H6C H 0.5254 0.1846 0.4388 0.055 Uiso 1 1 calc R . . C7 C 0.4755(5) -0.1836(13) 0.3820(4) 0.0344(19) Uani 1 1 d . . . H7A H 0.4437 -0.2940 0.3753 0.052 Uiso 1 1 calc R . . H7B H 0.5194 -0.1871 0.4308 0.052 Uiso 1 1 calc R . . H7C H 0.4971 -0.1752 0.3421 0.052 Uiso 1 1 calc R . . C8 C 0.2797(6) 0.5486(12) 0.2202(5) 0.036(2) Uani 1 1 d . . . C9 C 0.2044(6) 0.5818(15) 0.1637(5) 0.046(2) Uani 1 1 d . . . H9 H 0.2042 0.5948 0.1145 0.055 Uiso 1 1 calc R . . C10 C 0.1301(5) 0.5982(16) 0.1703(5) 0.042(2) Uani 1 1 d . . . C11 C 0.3535(7) 0.5249(14) 0.2008(6) 0.045(2) Uani 1 1 d . . . H11A H 0.3996 0.5025 0.2467 0.068 Uiso 1 1 calc R . . H11B H 0.3624 0.6349 0.1765 0.068 Uiso 1 1 calc R . . H11C H 0.3459 0.4220 0.1666 0.068 Uiso 1 1 calc R . . C12 C 0.0550(6) 0.634(2) 0.1021(5) 0.064(3) Uani 1 1 d . . . H12A H 0.0090 0.6371 0.1175 0.096 Uiso 1 1 calc R . . H12B H 0.0478 0.5371 0.0653 0.096 Uiso 1 1 calc R . . H12C H 0.0598 0.7501 0.0797 0.096 Uiso 1 1 calc R . . C13 C 0.2903(6) 0.6902(14) 0.5128(5) 0.042(2) Uani 1 1 d . . . H27A H 0.3002 0.8081 0.4946 0.063 Uiso 1 1 calc R . . H27B H 0.3289 0.6698 0.5636 0.063 Uiso 1 1 calc R . . H27C H 0.2364 0.6879 0.5134 0.063 Uiso 1 1 calc R . . C14 C 0.2811(5) 0.3126(14) 0.4952(5) 0.041(2) Uani 1 1 d . . . H34A H 0.2845 0.2061 0.4661 0.062 Uiso 1 1 calc R . . H34B H 0.2278 0.3197 0.4971 0.062 Uiso 1 1 calc R . . H34C H 0.3207 0.3028 0.5462 0.062 Uiso 1 1 calc R . . O1 O 0.2355(4) 0.0378(8) 0.3162(4) 0.0315(14) Uani 1 1 d . . . O2 O 0.2301(3) 0.0762(10) 0.1582(3) 0.0362(15) Uani 1 1 d . . . O3 O 0.3882(4) 0.0021(9) 0.4449(3) 0.0341(13) Uani 1 1 d . . . O4 O 0.2937(4) 0.5358(8) 0.2915(3) 0.0303(13) Uani 1 1 d . . . O5 O 0.1181(4) 0.5911(11) 0.2326(4) 0.0449(17) Uani 1 1 d . . . O6 O 0.3853(4) 0.5074(10) 0.4572(4) 0.0432(16) Uani 1 1 d . . . S1 S 0.41345(11) 0.0118(3) 0.37791(11) 0.0242(4) Uani 1 1 d . . . S2 S 0.30017(12) 0.5140(3) 0.45109(11) 0.0284(4) Uani 1 1 d . . . Cl1 Cl 0.40863(12) 0.0307(3) 0.20487(12) 0.0326(5) Uani 1 1 d . . . Cl2 Cl 0.10653(14) 0.5611(4) 0.38602(14) 0.0473(7) Uani 1 1 d . . . Pt1 Pt 0.316189(16) 0.03802(4) 0.264564(16) 0.02369(13) Uani 1 1 d . . . Pt2 Pt 0.206692(18) 0.54996(5) 0.336166(17) 0.02892(13) 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 C1 0.021(4) 0.051(5) 0.032(5) -0.012(4) 0.010(3) -0.003(3) C2 0.020(4) 0.077(7) 0.038(5) -0.002(5) 0.009(4) -0.002(4) C3 0.028(4) 0.060(6) 0.025(4) -0.005(4) -0.001(3) 0.007(4) C4 0.038(5) 0.072(8) 0.051(6) -0.008(5) 0.028(5) -0.008(5) C5 0.028(5) 0.117(11) 0.034(5) 0.003(6) -0.004(4) 0.012(6) C6 0.029(4) 0.052(5) 0.028(4) -0.002(4) 0.008(3) -0.013(4) C7 0.035(4) 0.043(5) 0.026(4) 0.003(4) 0.012(3) 0.014(4) C8 0.049(5) 0.034(5) 0.033(5) -0.002(4) 0.026(4) -0.008(4) C9 0.050(6) 0.074(7) 0.016(4) 0.000(4) 0.015(4) 0.005(5) C10 0.031(4) 0.070(6) 0.020(4) 0.011(4) 0.005(3) -0.003(4) C11 0.059(6) 0.056(6) 0.034(5) 0.004(4) 0.033(5) 0.002(5) C12 0.052(6) 0.111(10) 0.022(4) 0.008(6) 0.007(4) 0.008(7) C13 0.052(5) 0.042(5) 0.032(5) -0.011(4) 0.016(4) -0.008(4) C14 0.042(5) 0.054(6) 0.029(4) 0.004(4) 0.014(4) 0.000(4) O1 0.022(3) 0.047(4) 0.023(3) -0.002(3) 0.006(2) -0.001(2) O2 0.017(3) 0.068(4) 0.020(3) 0.002(3) 0.003(2) 0.008(3) O3 0.033(3) 0.055(4) 0.022(3) 0.007(3) 0.019(2) 0.005(3) O4 0.031(3) 0.042(4) 0.017(3) 0.006(2) 0.008(2) 0.005(2) O5 0.023(3) 0.081(5) 0.027(3) 0.006(3) 0.004(2) 0.002(3) O6 0.026(3) 0.067(4) 0.038(4) 0.002(3) 0.013(3) 0.006(3) S1 0.0192(9) 0.0387(10) 0.0161(9) -0.0008(8) 0.0080(7) 0.0013(8) S2 0.0230(9) 0.0447(11) 0.0180(9) 0.0006(8) 0.0082(7) 0.0010(8) Cl1 0.0247(10) 0.0541(13) 0.0222(10) 0.0021(8) 0.0122(8) 0.0014(8) Cl2 0.0302(11) 0.0807(19) 0.0355(12) 0.0129(11) 0.0176(10) 0.0092(11) Pt1 0.01770(18) 0.0365(2) 0.01730(18) -0.00042(11) 0.00695(13) 0.00015(11) Pt2 0.0246(2) 0.0450(2) 0.01860(19) 0.00373(12) 0.00963(14) 0.00212(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 C1 O1 1.283(10) . ? C1 C2 1.392(13) . ? C1 C4 1.490(12) . ? C2 C3 1.376(13) . ? C2 H2 0.9300 . ? C3 O2 1.286(10) . ? C3 C5 1.508(12) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 S1 1.759(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 S1 1.777(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O4 1.272(11) . ? C8 C9 1.387(14) . ? C8 C11 1.492(13) . ? C9 C10 1.371(13) . ? C9 H9 0.9300 . ? C10 O5 1.265(11) . ? C10 C12 1.492(12) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 S2 1.775(9) . ? C13 H27A 0.9600 . ? C13 H27B 0.9600 . ? C13 H27C 0.9600 . ? C14 S2 1.770(10) . ? C14 H34A 0.9600 . ? C14 H34B 0.9600 . ? C14 H34C 0.9600 . ? O1 Pt1 2.002(6) . ? O2 Pt1 2.039(6) . ? O3 S1 1.485(6) . ? O4 Pt2 2.012(6) . ? O5 Pt2 2.024(6) . ? O6 S2 1.471(6) . ? S1 Pt1 2.201(2) . ? S2 Pt2 2.201(2) . ? Cl1 Pt1 2.301(2) . ? Cl2 Pt2 2.293(3) . ? 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 C1 C2 125.9(8) . . ? O1 C1 C4 113.7(8) . . ? C2 C1 C4 120.4(8) . . ? C3 C2 C1 127.6(8) . . ? C3 C2 H2 116.2 . . ? C1 C2 H2 116.2 . . ? O2 C3 C2 127.5(8) . . ? O2 C3 C5 112.6(8) . . ? C2 C3 C5 119.9(8) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S1 C6 H6A 109.5 . . ? S1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S1 C7 H7A 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 C9 125.4(9) . . ? O4 C8 C11 113.5(9) . . ? C9 C8 C11 121.1(8) . . ? C10 C9 C8 129.2(8) . . ? C10 C9 H9 115.4 . . ? C8 C9 H9 115.4 . . ? O5 C10 C9 124.9(8) . . ? O5 C10 C12 113.7(8) . . ? C9 C10 C12 121.4(8) . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S2 C13 H27A 109.5 . . ? S2 C13 H27B 109.5 . . ? H27A C13 H27B 109.5 . . ? S2 C13 H27C 109.5 . . ? H27A C13 H27C 109.5 . . ? H27B C13 H27C 109.5 . . ? S2 C14 H34A 109.5 . . ? S2 C14 H34B 109.5 . . ? H34A C14 H34B 109.5 . . ? S2 C14 H34C 109.5 . . ? H34A C14 H34C 109.5 . . ? H34B C14 H34C 109.5 . . ? C1 O1 Pt1 123.7(6) . . ? C3 O2 Pt1 121.4(6) . . ? C8 O4 Pt2 123.5(6) . . ? C10 O5 Pt2 124.1(6) . . ? O3 S1 C6 109.1(4) . . ? O3 S1 C7 107.5(4) . . ? C6 S1 C7 102.6(5) . . ? O3 S1 Pt1 116.9(3) . . ? C6 S1 Pt1 108.5(3) . . ? C7 S1 Pt1 111.3(3) . . ? O6 S2 C14 107.7(4) . . ? O6 S2 C13 108.5(4) . . ? C14 S2 C13 101.9(5) . . ? O6 S2 Pt2 117.4(3) . . ? C14 S2 Pt2 110.6(3) . . ? C13 S2 Pt2 109.6(3) . . ? O1 Pt1 O2 93.8(2) . . ? O1 Pt1 S1 88.58(18) . . ? O2 Pt1 S1 176.3(2) . . ? O1 Pt1 Cl1 178.63(18) . . ? O2 Pt1 Cl1 86.26(18) . . ? S1 Pt1 Cl1 91.46(9) . . ? O4 Pt2 O5 92.8(2) . . ? O4 Pt2 S2 89.30(18) . . ? O5 Pt2 S2 177.4(2) . . ? O4 Pt2 Cl2 178.96(19) . . ? O5 Pt2 Cl2 86.8(2) . . ? S2 Pt2 Cl2 91.12(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.653 _refine_diff_density_min -2.886 _refine_diff_density_rms 0.295 #END #BEGIN data_sa12s1 _database_code_depnum_ccdc_archive 'CCDC 713089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H13 Cl O2 Pt S' _chemical_formula_sum 'C7 H13 Cl O2 Pt S' _chemical_formula_weight 391.77 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 6.268(2) _cell_length_b 11.781(6) _cell_length_c 15.140(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.41(2) _cell_angle_gamma 90.00 _cell_volume 1102.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 9 _cell_measurement_theta_max 18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 13.115 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Walker & Stuart' _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 'Philips PW 1100' _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3314 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3213 _reflns_number_gt 2400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local programs' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0415P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3213 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.005 _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 C1 C 0.3500(11) 0.1676(5) 0.5242(4) 0.0380(14) Uani 1 1 d . . . C2 C 0.4737(12) 0.2614(5) 0.5051(4) 0.0440(16) Uani 1 1 d . . . H2 H 0.4144 0.3059 0.4565 0.053 Uiso 1 1 calc R . . C3 C 0.6748(11) 0.2953(5) 0.5506(4) 0.0401(14) Uani 1 1 d . . . C4 C 0.1424(12) 0.1385(6) 0.4674(5) 0.0532(19) Uani 1 1 d . . . H4A H 0.1581 0.0688 0.4363 0.080 Uiso 1 1 calc R . . H4B H 0.1017 0.1982 0.4248 0.080 Uiso 1 1 calc R . . H4C H 0.0326 0.1296 0.5042 0.080 Uiso 1 1 calc R . . C5 C 0.7833(14) 0.3988(6) 0.5198(5) 0.058(2) Uani 1 1 d . . . H5A H 0.7929 0.4566 0.5649 0.087 Uiso 1 1 calc R . . H5B H 0.7001 0.4265 0.4652 0.087 Uiso 1 1 calc R . . H5C H 0.9259 0.3791 0.5097 0.087 Uiso 1 1 calc R . . C6 C 0.3101(11) -0.0861(6) 0.6973(5) 0.0491(18) Uani 1 1 d . . . H6A H 0.3450 -0.1079 0.6402 0.074 Uiso 1 1 calc R . . H6B H 0.1948 -0.0316 0.6886 0.074 Uiso 1 1 calc R . . H6C H 0.2654 -0.1518 0.7270 0.074 Uiso 1 1 calc R . . C7 C 0.7313(11) -0.1420(6) 0.7706(6) 0.054(2) Uani 1 1 d . . . H7A H 0.6960 -0.1972 0.8126 0.082 Uiso 1 1 calc R . . H7B H 0.8756 -0.1147 0.7900 0.082 Uiso 1 1 calc R . . H7C H 0.7222 -0.1765 0.7127 0.082 Uiso 1 1 calc R . . O1 O 0.4017(7) 0.0988(3) 0.5903(3) 0.0399(10) Uani 1 1 d . . . O2 O 0.7793(7) 0.2468(3) 0.6190(3) 0.0407(10) Uani 1 1 d . . . S S 0.5431(2) -0.02474(12) 0.76431(10) 0.0328(3) Uani 1 1 d . . . Cl Cl 0.9721(3) 0.12440(13) 0.78934(12) 0.0484(4) Uani 1 1 d . . . Pt Pt 0.66781(4) 0.112567(17) 0.682480(14) 0.02850(8) 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 C1 0.055(4) 0.027(3) 0.031(3) -0.004(2) 0.002(3) 0.003(3) C2 0.065(4) 0.028(3) 0.035(3) 0.010(3) -0.003(3) -0.002(3) C3 0.058(4) 0.024(3) 0.039(3) 0.002(3) 0.012(3) -0.002(3) C4 0.059(5) 0.045(4) 0.048(4) 0.007(3) -0.011(3) 0.002(3) C5 0.079(6) 0.034(4) 0.060(5) 0.012(3) 0.011(4) -0.017(4) C6 0.045(4) 0.037(4) 0.062(5) 0.014(3) -0.002(3) -0.008(3) C7 0.044(4) 0.035(4) 0.083(6) 0.021(4) 0.007(4) 0.008(3) O1 0.049(3) 0.028(2) 0.040(2) 0.0090(18) -0.0050(19) -0.0065(19) O2 0.048(3) 0.025(2) 0.049(2) 0.0077(19) 0.008(2) -0.0082(19) S 0.0415(8) 0.0249(7) 0.0311(7) 0.0032(6) 0.0035(6) -0.0010(6) Cl 0.0535(10) 0.0328(8) 0.0519(9) 0.0019(7) -0.0117(7) -0.0080(7) Pt 0.03902(13) 0.01553(10) 0.02989(12) -0.00019(9) 0.00251(8) -0.00107(10) _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 C1 O1 1.288(7) . ? C1 C2 1.407(9) . ? C1 C4 1.478(9) . ? C2 C3 1.393(9) . ? C2 H2 0.9300 . ? C3 O2 1.267(7) . ? C3 C5 1.507(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 S 1.789(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 S 1.810(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O1 Pt 1.999(4) . ? O2 Pt 2.033(4) . ? S Pt 2.2538(18) . ? Cl Pt 2.295(2) . ? 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 C1 C2 125.3(6) . . ? O1 C1 C4 113.1(6) . . ? C2 C1 C4 121.7(6) . . ? C3 C2 C1 127.5(6) . . ? C3 C2 H2 116.3 . . ? C1 C2 H2 116.3 . . ? O2 C3 C2 125.5(6) . . ? O2 C3 C5 114.8(6) . . ? C2 C3 C5 119.8(6) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S C6 H6A 109.5 . . ? S C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S C7 H7A 109.5 . . ? S C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 O1 Pt 124.5(4) . . ? C3 O2 Pt 124.4(4) . . ? C6 S C7 100.7(3) . . ? C6 S Pt 107.6(2) . . ? C7 S Pt 107.2(2) . . ? O1 Pt O2 92.62(17) . . ? O1 Pt S 90.02(13) . . ? O2 Pt S 174.36(13) . . ? O1 Pt Cl 178.73(12) . . ? O2 Pt Cl 88.59(14) . . ? S Pt Cl 88.81(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.973 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.184 #END #BEGIN data_ptp1t _database_code_depnum_ccdc_archive 'CCDC 713090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H22 Cl O2 P Pt' _chemical_formula_sum 'C23 H22 Cl O2 P Pt' _chemical_formula_weight 591.92 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 9.948(1) _cell_length_b 12.738(2) _cell_length_c 18.411(2) _cell_angle_alpha 101.68(1) _cell_angle_beta 100.25(1) _cell_angle_gamma 106.83(2) _cell_volume 2116.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10944 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 6.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 1.000 _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 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23015 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8301 _reflns_number_gt 5795 _reflns_threshold_expression >2sigma(I) _computing_data_collection smart _computing_cell_refinement saint _computing_data_reduction saint _computing_structure_solution sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0010P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8301 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 0.41621(2) 0.705183(18) 0.402076(13) 0.03746(7) Uani 1 1 d . . . Pt2 Pt 0.57162(2) 0.315519(17) 0.087611(12) 0.03323(7) Uani 1 1 d . . . Cl1 Cl 0.32975(16) 0.73988(16) 0.28987(10) 0.0712(5) Uani 1 1 d . . . Cl2 Cl 0.63499(15) 0.29050(13) 0.20685(9) 0.0521(4) Uani 1 1 d . . . P1 P 0.63855(15) 0.83090(12) 0.42548(9) 0.0350(4) Uani 1 1 d . . . P2 P 0.34799(14) 0.19109(11) 0.06371(8) 0.0310(3) Uani 1 1 d . . . O11 O 0.4835(4) 0.6687(3) 0.5001(2) 0.0526(11) Uani 1 1 d . . . O21 O 0.2147(4) 0.5848(3) 0.3805(2) 0.0485(11) Uani 1 1 d . . . O25 O 0.7742(4) 0.4373(3) 0.1150(2) 0.0435(10) Uani 1 1 d . . . C11 C 0.4051(7) 0.5976(5) 0.5291(4) 0.0482(16) Uani 1 1 d . . . C22 C 0.7067(6) 0.6612(5) 0.3313(3) 0.0491(16) Uani 1 1 d . . . H22 H 0.6110 0.6159 0.3246 0.059 Uiso 1 1 calc R . . C25 C 0.7475(7) 0.4858(5) -0.0034(4) 0.0527(17) Uani 1 1 d . . . H25 H 0.7952 0.5349 -0.0289 0.063 Uiso 1 1 calc R . . C37 C 0.4226(6) -0.0879(5) 0.1098(3) 0.0453(15) Uani 1 1 d . . . H37 H 0.4945 -0.1206 0.1070 0.054 Uiso 1 1 calc R . . O15 O 0.5258(4) 0.3396(3) -0.0172(2) 0.0426(10) Uani 1 1 d . . . C26 C 0.2798(6) 0.3269(5) 0.1794(3) 0.0477(15) Uani 1 1 d . . . H26 H 0.3749 0.3425 0.2064 0.057 Uiso 1 1 calc R . . C41 C 0.4833(7) 0.5940(5) 0.6059(3) 0.067(2) Uani 1 1 d . . . H51A H 0.5799 0.6482 0.6205 0.100 Uiso 1 1 calc R . . H51B H 0.4878 0.5190 0.6027 0.100 Uiso 1 1 calc R . . H51C H 0.4321 0.6125 0.6434 0.100 Uiso 1 1 calc R . . C31 C 0.1775(6) 0.5222(5) 0.4256(4) 0.0502(16) Uani 1 1 d . . . C45 C 0.5441(7) 0.4118(5) -0.1224(3) 0.068(2) Uani 1 1 d . . . H55A H 0.4988 0.3346 -0.1535 0.102 Uiso 1 1 calc R . . H55B H 0.6181 0.4518 -0.1436 0.102 Uiso 1 1 calc R . . H55C H 0.4725 0.4486 -0.1211 0.102 Uiso 1 1 calc R . . C68 C 0.2367(5) 0.2105(5) -0.0808(3) 0.0429(14) Uani 1 1 d . . . H68 H 0.2546 0.2863 -0.0560 0.051 Uiso 1 1 calc R . . C21 C 0.2634(7) 0.5268(5) 0.4947(4) 0.0535(17) Uani 1 1 d . . . H21 H 0.2213 0.4766 0.5212 0.064 Uiso 1 1 calc R . . C18 C 0.2601(5) 0.1354(4) -0.0374(3) 0.0321(13) Uani 1 1 d . . . C17 C 0.3332(5) 0.0642(4) 0.0967(3) 0.0301(12) Uani 1 1 d . . . C27 C 0.4406(5) 0.0162(4) 0.0935(3) 0.0389(13) Uani 1 1 d . . . H27 H 0.5245 0.0533 0.0805 0.047 Uiso 1 1 calc R . . C35 C 0.8224(6) 0.4951(5) 0.0700(4) 0.0480(16) Uani 1 1 d . . . C36 C 0.1911(7) 0.3759(6) 0.2134(4) 0.0636(19) Uani 1 1 d . . . H36 H 0.2276 0.4266 0.2621 0.076 Uiso 1 1 calc R . . C51 C 0.0243(6) 0.4391(5) 0.3957(4) 0.071(2) Uani 1 1 d . . . H41A H -0.0415 0.4797 0.3857 0.106 Uiso 1 1 calc R . . H41B H -0.0001 0.3994 0.4332 0.106 Uiso 1 1 calc R . . H41C H 0.0171 0.3854 0.3491 0.106 Uiso 1 1 calc R . . C16 C 0.2293(6) 0.2557(4) 0.1064(3) 0.0360(13) Uani 1 1 d . . . C14 C 0.7259(6) 0.8617(4) 0.5269(3) 0.0398(14) Uani 1 1 d . . . C48 C 0.1570(6) 0.0601(6) -0.1968(4) 0.0557(17) Uani 1 1 d . . . H48 H 0.1244 0.0352 -0.2500 0.067 Uiso 1 1 calc R . . C55 C 0.9710(6) 0.5811(5) 0.1042(4) 0.0619(19) Uani 1 1 d . . . H45A H 0.9685 0.6380 0.1465 0.093 Uiso 1 1 calc R . . H45B H 1.0032 0.6166 0.0661 0.093 Uiso 1 1 calc R . . H45C H 1.0367 0.5441 0.1219 0.093 Uiso 1 1 calc R . . C28 C 0.2249(5) 0.0216(5) -0.0754(3) 0.0400(14) Uani 1 1 d . . . H28 H 0.2348 -0.0301 -0.0475 0.048 Uiso 1 1 calc R . . C67 C 0.2098(5) 0.0089(5) 0.1165(3) 0.0406(14) Uani 1 1 d . . . H67 H 0.1363 0.0402 0.1173 0.049 Uiso 1 1 calc R . . C38 C 0.1742(5) -0.0164(5) -0.1558(3) 0.0505(16) Uani 1 1 d . . . H38 H 0.1525 -0.0926 -0.1811 0.061 Uiso 1 1 calc R . . C24 C 0.8422(6) 0.8297(5) 0.5532(3) 0.0483(15) Uani 1 1 d . . . H24 H 0.8872 0.7988 0.5186 0.058 Uiso 1 1 calc R . . C58 C 0.1874(6) 0.1731(6) -0.1602(4) 0.0492(16) Uani 1 1 d . . . H58 H 0.1749 0.2240 -0.1884 0.059 Uiso 1 1 calc R . . C64 C 0.6609(6) 0.9081(5) 0.5806(3) 0.0480(15) Uani 1 1 d . . . H64 H 0.5817 0.9297 0.5637 0.058 Uiso 1 1 calc R . . C12 C 0.7547(5) 0.7744(4) 0.3744(3) 0.0344(13) Uani 1 1 d . . . C42 C 0.9385(7) 0.6818(6) 0.3086(4) 0.0571(18) Uani 1 1 d . . . H42 H 1.0017 0.6501 0.2885 0.069 Uiso 1 1 calc R . . C54 C 0.7115(6) 0.9226(6) 0.6572(4) 0.0583(18) Uani 1 1 d . . . H54 H 0.6686 0.9556 0.6921 0.070 Uiso 1 1 calc R . . C66 C 0.0845(6) 0.2294(5) 0.0675(3) 0.0446(14) Uani 1 1 d . . . H66 H 0.0472 0.1796 0.0185 0.054 Uiso 1 1 calc R . . C34 C 0.8932(7) 0.8432(6) 0.6312(4) 0.0608(18) Uani 1 1 d . . . H34 H 0.9725 0.8219 0.6484 0.073 Uiso 1 1 calc R . . C44 C 0.8264(7) 0.8880(6) 0.6827(4) 0.0612(19) Uani 1 1 d . . . H44 H 0.8587 0.8951 0.7346 0.073 Uiso 1 1 calc R . . C62 C 0.8962(6) 0.8414(5) 0.3808(3) 0.0486(15) Uani 1 1 d . . . H62 H 0.9293 0.9182 0.4071 0.058 Uiso 1 1 calc R . . C52 C 0.9881(6) 0.7952(6) 0.3484(3) 0.0543(17) Uani 1 1 d . . . H52 H 1.0830 0.8403 0.3534 0.065 Uiso 1 1 calc R . . C47 C 0.3006(6) -0.1437(5) 0.1301(3) 0.0479(16) Uani 1 1 d . . . H47 H 0.2892 -0.2140 0.1401 0.057 Uiso 1 1 calc R . . C46 C 0.0474(7) 0.3486(6) 0.1744(4) 0.0587(19) Uani 1 1 d . . . H46 H -0.0140 0.3786 0.1976 0.070 Uiso 1 1 calc R . . C56 C -0.0027(6) 0.2787(5) 0.1031(4) 0.0554(17) Uani 1 1 d . . . H56 H -0.0983 0.2629 0.0769 0.066 Uiso 1 1 calc R . . C32 C 0.7976(7) 0.6150(5) 0.2983(4) 0.0577(18) Uani 1 1 d . . . H32 H 0.7639 0.5393 0.2695 0.069 Uiso 1 1 calc R . . C15 C 0.6106(7) 0.4125(5) -0.0427(4) 0.0472(16) Uani 1 1 d . . . C57 C 0.1949(6) -0.0940(4) 0.1355(3) 0.0463(15) Uani 1 1 d . . . H57 H 0.1141 -0.1289 0.1517 0.056 Uiso 1 1 calc R . . C33 C 0.6454(6) 1.0793(5) 0.3155(3) 0.0494(15) Uani 1 1 d . . . H33 H 0.6169 1.0819 0.2651 0.059 Uiso 1 1 calc R . . C63 C 0.7328(6) 1.0709(5) 0.4640(3) 0.0458(15) Uani 1 1 d . . . H63 H 0.7629 1.0688 0.5143 0.055 Uiso 1 1 calc R . . C23 C 0.6206(6) 0.9754(5) 0.3320(3) 0.0456(14) Uani 1 1 d . . . H23 H 0.5737 0.9086 0.2928 0.055 Uiso 1 1 calc R . . C53 C 0.7566(6) 1.1748(5) 0.4475(4) 0.0514(16) Uani 1 1 d . . . H53 H 0.8025 1.2420 0.4865 0.062 Uiso 1 1 calc R . . C13 C 0.6648(5) 0.9694(4) 0.4067(3) 0.0366(13) Uani 1 1 d . . . C43 C 0.7116(6) 1.1783(5) 0.3727(4) 0.0506(16) Uani 1 1 d . . . H43 H 0.7263 1.2481 0.3614 0.061 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 0.03532(14) 0.03951(14) 0.03723(16) 0.01371(13) 0.01137(12) 0.00852(12) Pt2 0.03236(13) 0.03311(13) 0.03754(15) 0.01470(12) 0.01148(11) 0.01082(11) Cl1 0.0479(9) 0.1024(14) 0.0557(11) 0.0449(11) 0.0025(8) 0.0045(10) Cl2 0.0536(9) 0.0520(9) 0.0422(9) 0.0201(8) 0.0012(7) 0.0068(8) P1 0.0363(8) 0.0333(8) 0.0348(9) 0.0117(8) 0.0087(7) 0.0091(7) P2 0.0313(8) 0.0318(8) 0.0334(9) 0.0120(7) 0.0097(7) 0.0125(7) O11 0.045(2) 0.059(3) 0.053(3) 0.030(2) 0.012(2) 0.007(2) O21 0.041(2) 0.047(2) 0.054(3) 0.016(2) 0.017(2) 0.005(2) O25 0.037(2) 0.040(2) 0.059(3) 0.024(2) 0.017(2) 0.0117(19) C11 0.055(4) 0.043(4) 0.059(4) 0.023(4) 0.026(3) 0.022(3) C22 0.048(4) 0.042(4) 0.059(4) 0.023(4) 0.015(3) 0.010(3) C25 0.057(4) 0.043(4) 0.061(5) 0.023(4) 0.028(4) 0.008(3) C37 0.042(3) 0.040(3) 0.056(4) 0.015(3) 0.007(3) 0.019(3) O15 0.041(2) 0.046(2) 0.040(2) 0.018(2) 0.0140(19) 0.008(2) C26 0.047(4) 0.055(4) 0.041(4) 0.009(3) 0.011(3) 0.020(3) C41 0.085(5) 0.074(5) 0.056(5) 0.042(4) 0.020(4) 0.031(4) C31 0.054(4) 0.034(3) 0.064(5) 0.006(4) 0.032(4) 0.012(3) C45 0.100(5) 0.071(5) 0.052(5) 0.035(4) 0.034(4) 0.036(4) C68 0.040(3) 0.047(4) 0.046(4) 0.013(3) 0.008(3) 0.022(3) C21 0.068(4) 0.048(4) 0.054(5) 0.026(4) 0.031(4) 0.016(4) C18 0.027(3) 0.040(3) 0.032(3) 0.008(3) 0.010(2) 0.016(3) C17 0.036(3) 0.030(3) 0.025(3) 0.010(3) 0.008(2) 0.011(3) C27 0.035(3) 0.040(3) 0.047(4) 0.017(3) 0.018(3) 0.014(3) C35 0.051(4) 0.032(3) 0.073(5) 0.017(4) 0.036(4) 0.018(3) C36 0.080(5) 0.075(5) 0.048(4) 0.012(4) 0.025(4) 0.041(4) C51 0.049(4) 0.058(4) 0.094(6) 0.015(4) 0.029(4) -0.002(4) C16 0.042(3) 0.036(3) 0.040(4) 0.018(3) 0.020(3) 0.018(3) C14 0.043(3) 0.036(3) 0.037(4) 0.014(3) 0.007(3) 0.008(3) C48 0.044(4) 0.084(5) 0.030(4) 0.011(4) 0.007(3) 0.014(4) C55 0.045(4) 0.045(4) 0.088(6) 0.016(4) 0.025(4) 0.000(3) C28 0.034(3) 0.048(4) 0.037(4) 0.013(3) 0.007(3) 0.011(3) C67 0.033(3) 0.045(3) 0.048(4) 0.015(3) 0.009(3) 0.019(3) C38 0.037(3) 0.051(4) 0.045(4) -0.004(3) 0.006(3) 0.001(3) C24 0.049(4) 0.057(4) 0.043(4) 0.016(3) 0.011(3) 0.024(3) C58 0.041(3) 0.061(4) 0.051(4) 0.029(4) 0.010(3) 0.018(3) C64 0.033(3) 0.060(4) 0.044(4) 0.007(3) 0.010(3) 0.011(3) C12 0.037(3) 0.037(3) 0.032(3) 0.014(3) 0.006(3) 0.013(3) C42 0.057(4) 0.072(5) 0.064(5) 0.023(4) 0.031(4) 0.040(4) C54 0.046(4) 0.082(5) 0.040(4) 0.009(4) 0.015(3) 0.014(4) C66 0.043(3) 0.043(3) 0.049(4) 0.009(3) 0.014(3) 0.017(3) C34 0.059(4) 0.076(5) 0.047(4) 0.015(4) 0.000(3) 0.030(4) C44 0.055(4) 0.085(5) 0.033(4) 0.013(4) 0.003(3) 0.014(4) C62 0.047(4) 0.047(4) 0.048(4) 0.015(3) 0.013(3) 0.009(3) C52 0.035(3) 0.080(5) 0.052(4) 0.021(4) 0.017(3) 0.020(4) C47 0.061(4) 0.034(3) 0.050(4) 0.023(3) 0.006(3) 0.013(3) C46 0.069(5) 0.065(5) 0.068(5) 0.025(4) 0.038(4) 0.043(4) C56 0.044(4) 0.061(4) 0.075(5) 0.026(4) 0.023(4) 0.027(3) C32 0.073(5) 0.050(4) 0.057(5) 0.010(4) 0.024(4) 0.030(4) C15 0.071(4) 0.039(4) 0.053(4) 0.022(3) 0.034(4) 0.034(3) C57 0.046(3) 0.040(3) 0.059(4) 0.021(3) 0.022(3) 0.013(3) C33 0.062(4) 0.048(4) 0.040(4) 0.020(3) 0.011(3) 0.016(3) C63 0.054(4) 0.037(3) 0.039(4) 0.003(3) 0.005(3) 0.015(3) C23 0.047(3) 0.039(3) 0.038(4) 0.003(3) 0.008(3) 0.003(3) C53 0.052(4) 0.033(3) 0.065(5) 0.006(3) 0.019(3) 0.010(3) C13 0.039(3) 0.034(3) 0.040(4) 0.013(3) 0.012(3) 0.014(3) C43 0.050(4) 0.045(4) 0.064(5) 0.026(4) 0.019(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O11 2.003(4) . ? Pt1 O21 2.054(4) . ? Pt1 P1 2.2300(15) . ? Pt1 Cl1 2.2716(15) . ? Pt2 O15 2.008(3) . ? Pt2 O25 2.057(3) . ? Pt2 P2 2.2321(15) . ? Pt2 Cl2 2.2859(14) . ? P1 C13 1.820(5) . ? P1 C14 1.823(5) . ? P1 C12 1.825(5) . ? P2 C18 1.806(5) . ? P2 C17 1.814(5) . ? P2 C16 1.822(5) . ? O11 C11 1.284(6) . ? O21 C31 1.292(6) . ? O25 C35 1.282(6) . ? C11 C21 1.384(8) . ? C11 C41 1.503(7) . ? C22 C32 1.376(7) . ? C22 C12 1.394(7) . ? C22 H22 0.9300 . ? C25 C15 1.375(8) . ? C25 C35 1.385(8) . ? C25 H25 0.9300 . ? C37 C47 1.373(7) . ? C37 C27 1.387(6) . ? C37 H37 0.9300 . ? O15 C15 1.288(6) . ? C26 C16 1.374(7) . ? C26 C36 1.384(7) . ? C26 H26 0.9300 . ? C41 H51A 0.9600 . ? C41 H51B 0.9600 . ? C41 H51C 0.9600 . ? C31 C21 1.382(8) . ? C31 C51 1.509(7) . ? C45 C15 1.496(7) . ? C45 H55A 0.9600 . ? C45 H55B 0.9600 . ? C45 H55C 0.9600 . ? C68 C58 1.390(8) . ? C68 C18 1.407(6) . ? C68 H68 0.9300 . ? C21 H21 0.9300 . ? C18 C28 1.386(7) . ? C17 C67 1.379(6) . ? C17 C27 1.381(6) . ? C27 H27 0.9300 . ? C35 C55 1.494(7) . ? C36 C46 1.388(8) . ? C36 H36 0.9300 . ? C51 H41A 0.9600 . ? C51 H41B 0.9600 . ? C51 H41C 0.9600 . ? C16 C66 1.399(6) . ? C14 C24 1.375(6) . ? C14 C64 1.399(7) . ? C48 C38 1.377(7) . ? C48 C58 1.379(8) . ? C48 H48 0.9300 . ? C55 H45A 0.9600 . ? C55 H45B 0.9600 . ? C55 H45C 0.9600 . ? C28 C38 1.409(7) . ? C28 H28 0.9300 . ? C67 C57 1.397(6) . ? C67 H67 0.9300 . ? C38 H38 0.9300 . ? C24 C34 1.392(7) . ? C24 H24 0.9300 . ? C58 H58 0.9300 . ? C64 C54 1.366(7) . ? C64 H64 0.9300 . ? C12 C62 1.389(7) . ? C42 C32 1.369(8) . ? C42 C52 1.378(8) . ? C42 H42 0.9300 . ? C54 C44 1.380(7) . ? C54 H54 0.9300 . ? C66 C56 1.388(7) . ? C66 H66 0.9300 . ? C34 C44 1.375(8) . ? C34 H34 0.9300 . ? C44 H44 0.9300 . ? C62 C52 1.379(7) . ? C62 H62 0.9300 . ? C52 H52 0.9300 . ? C47 C57 1.384(7) . ? C47 H47 0.9300 . ? C46 C56 1.342(8) . ? C46 H46 0.9300 . ? C56 H56 0.9300 . ? C32 H32 0.9300 . ? C57 H57 0.9300 . ? C33 C43 1.367(8) . ? C33 C23 1.381(7) . ? C33 H33 0.9300 . ? C63 C53 1.381(7) . ? C63 C13 1.389(7) . ? C63 H63 0.9300 . ? C23 C13 1.391(7) . ? C23 H23 0.9300 . ? C53 C43 1.385(7) . ? C53 H53 0.9300 . ? C43 H43 0.9300 . ? 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 O11 Pt1 O21 91.48(15) . . ? O11 Pt1 P1 87.49(11) . . ? O21 Pt1 P1 177.91(10) . . ? O11 Pt1 Cl1 177.30(11) . . ? O21 Pt1 Cl1 85.82(11) . . ? P1 Pt1 Cl1 95.19(6) . . ? O15 Pt2 O25 91.13(14) . . ? O15 Pt2 P2 90.34(11) . . ? O25 Pt2 P2 176.19(11) . . ? O15 Pt2 Cl2 177.31(10) . . ? O25 Pt2 Cl2 86.53(11) . . ? P2 Pt2 Cl2 92.08(5) . . ? C13 P1 C14 105.3(3) . . ? C13 P1 C12 103.5(2) . . ? C14 P1 C12 105.2(2) . . ? C13 P1 Pt1 120.79(17) . . ? C14 P1 Pt1 108.04(18) . . ? C12 P1 Pt1 112.73(18) . . ? C18 P2 C17 103.6(2) . . ? C18 P2 C16 105.7(2) . . ? C17 P2 C16 105.7(2) . . ? C18 P2 Pt2 112.85(17) . . ? C17 P2 Pt2 116.27(16) . . ? C16 P2 Pt2 111.79(18) . . ? C11 O11 Pt1 125.7(4) . . ? C31 O21 Pt1 123.7(4) . . ? C35 O25 Pt2 124.3(4) . . ? O11 C11 C21 125.5(6) . . ? O11 C11 C41 113.5(5) . . ? C21 C11 C41 121.0(5) . . ? C32 C22 C12 121.4(6) . . ? C32 C22 H22 119.3 . . ? C12 C22 H22 119.3 . . ? C15 C25 C35 127.5(5) . . ? C15 C25 H25 116.3 . . ? C35 C25 H25 116.3 . . ? C47 C37 C27 121.3(5) . . ? C47 C37 H37 119.3 . . ? C27 C37 H37 119.3 . . ? C15 O15 Pt2 125.4(4) . . ? C16 C26 C36 120.9(6) . . ? C16 C26 H26 119.6 . . ? C36 C26 H26 119.6 . . ? C11 C41 H51A 109.5 . . ? C11 C41 H51B 109.5 . . ? H51A C41 H51B 109.5 . . ? C11 C41 H51C 109.5 . . ? H51A C41 H51C 109.5 . . ? H51B C41 H51C 109.5 . . ? O21 C31 C21 126.1(6) . . ? O21 C31 C51 113.1(6) . . ? C21 C31 C51 120.8(6) . . ? C15 C45 H55A 109.5 . . ? C15 C45 H55B 109.5 . . ? H55A C45 H55B 109.5 . . ? C15 C45 H55C 109.5 . . ? H55A C45 H55C 109.5 . . ? H55B C45 H55C 109.5 . . ? C58 C68 C18 121.0(5) . . ? C58 C68 H68 119.5 . . ? C18 C68 H68 119.5 . . ? C31 C21 C11 127.4(5) . . ? C31 C21 H21 116.3 . . ? C11 C21 H21 116.3 . . ? C28 C18 C68 118.3(5) . . ? C28 C18 P2 122.0(4) . . ? C68 C18 P2 119.5(4) . . ? C67 C17 C27 119.8(4) . . ? C67 C17 P2 120.9(4) . . ? C27 C17 P2 118.9(4) . . ? C17 C27 C37 119.5(5) . . ? C17 C27 H27 120.2 . . ? C37 C27 H27 120.2 . . ? O25 C35 C25 125.7(6) . . ? O25 C35 C55 114.0(6) . . ? C25 C35 C55 120.2(5) . . ? C26 C36 C46 119.5(6) . . ? C26 C36 H36 120.3 . . ? C46 C36 H36 120.3 . . ? C31 C51 H41A 109.5 . . ? C31 C51 H41B 109.5 . . ? H41A C51 H41B 109.5 . . ? C31 C51 H41C 109.5 . . ? H41A C51 H41C 109.5 . . ? H41B C51 H41C 109.5 . . ? C26 C16 C66 119.0(5) . . ? C26 C16 P2 119.8(4) . . ? C66 C16 P2 121.1(5) . . ? C24 C14 C64 118.2(5) . . ? C24 C14 P1 123.3(5) . . ? C64 C14 P1 118.0(4) . . ? C38 C48 C58 120.9(6) . . ? C38 C48 H48 119.6 . . ? C58 C48 H48 119.6 . . ? C35 C55 H45A 109.5 . . ? C35 C55 H45B 109.5 . . ? H45A C55 H45B 109.5 . . ? C35 C55 H45C 109.5 . . ? H45A C55 H45C 109.5 . . ? H45B C55 H45C 109.5 . . ? C18 C28 C38 120.6(5) . . ? C18 C28 H28 119.7 . . ? C38 C28 H28 119.7 . . ? C17 C67 C57 120.3(5) . . ? C17 C67 H67 119.9 . . ? C57 C67 H67 119.9 . . ? C48 C38 C28 119.5(6) . . ? C48 C38 H38 120.2 . . ? C28 C38 H38 120.2 . . ? C14 C24 C34 120.7(6) . . ? C14 C24 H24 119.6 . . ? C34 C24 H24 119.6 . . ? C48 C58 C68 119.6(5) . . ? C48 C58 H58 120.2 . . ? C68 C58 H58 120.2 . . ? C54 C64 C14 121.3(5) . . ? C54 C64 H64 119.3 . . ? C14 C64 H64 119.3 . . ? C62 C12 C22 118.0(5) . . ? C62 C12 P1 120.9(4) . . ? C22 C12 P1 121.0(4) . . ? C32 C42 C52 121.0(6) . . ? C32 C42 H42 119.5 . . ? C52 C42 H42 119.5 . . ? C64 C54 C44 119.9(6) . . ? C64 C54 H54 120.0 . . ? C44 C54 H54 120.0 . . ? C56 C66 C16 119.0(6) . . ? C56 C66 H66 120.5 . . ? C16 C66 H66 120.5 . . ? C44 C34 C24 119.9(6) . . ? C44 C34 H34 120.0 . . ? C24 C34 H34 120.0 . . ? C34 C44 C54 119.9(6) . . ? C34 C44 H44 120.1 . . ? C54 C44 H44 120.1 . . ? C52 C62 C12 120.6(6) . . ? C52 C62 H62 119.7 . . ? C12 C62 H62 119.7 . . ? C42 C52 C62 119.7(6) . . ? C42 C52 H52 120.2 . . ? C62 C52 H52 120.2 . . ? C37 C47 C57 119.2(5) . . ? C37 C47 H47 120.4 . . ? C57 C47 H47 120.4 . . ? C56 C46 C36 119.9(6) . . ? C56 C46 H46 120.1 . . ? C36 C46 H46 120.1 . . ? C46 C56 C66 121.7(6) . . ? C46 C56 H56 119.1 . . ? C66 C56 H56 119.1 . . ? C42 C32 C22 119.1(6) . . ? C42 C32 H32 120.4 . . ? C22 C32 H32 120.4 . . ? O15 C15 C25 126.0(6) . . ? O15 C15 C45 112.7(6) . . ? C25 C15 C45 121.3(5) . . ? C47 C57 C67 119.8(5) . . ? C47 C57 H57 120.1 . . ? C67 C57 H57 120.1 . . ? C43 C33 C23 120.3(5) . . ? C43 C33 H33 119.8 . . ? C23 C33 H33 119.8 . . ? C53 C63 C13 121.1(5) . . ? C53 C63 H63 119.4 . . ? C13 C63 H63 119.4 . . ? C33 C23 C13 120.8(6) . . ? C33 C23 H23 119.6 . . ? C13 C23 H23 119.6 . . ? C63 C53 C43 119.6(6) . . ? C63 C53 H53 120.2 . . ? C43 C53 H53 120.2 . . ? C63 C13 C23 118.0(5) . . ? C63 C13 P1 122.4(4) . . ? C23 C13 P1 119.5(5) . . ? C33 C43 C53 120.0(5) . . ? C33 C43 H43 120.0 . . ? C53 C43 H43 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.109 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.104 #END #BEGIN data_ld342s1 _database_code_depnum_ccdc_archive 'CCDC 713091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 O5 Pt S' _chemical_formula_sum 'C12 H20 O5 Pt S' _chemical_formula_weight 471.43 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' O O 0.0106 0.0060 '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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.910(4) _cell_length_b 13.000(5) _cell_length_c 15.711(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.63(2) _cell_angle_gamma 90.00 _cell_volume 1582.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 9.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 1.173 _exptl_absorpt_process_details 'Walker & Stuart' _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 'Philips PW 1100' _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 2878 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2779 _reflns_number_gt 1795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local programs' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0125P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2779 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 C1 C 0.2355(13) -0.1825(8) 0.2095(6) 0.033(3) Uani 1 1 d . . . C2 C 0.3070(11) -0.1002(8) 0.2695(6) 0.030(3) Uani 1 1 d . . . H2 H 0.2981 -0.1233 0.3278 0.036 Uiso 1 1 calc R . . C3 C 0.4852(14) -0.0612(9) 0.2760(7) 0.045(3) Uani 1 1 d . . . C4 C 0.0867(14) -0.2453(8) 0.2321(8) 0.058(4) Uani 1 1 d . . . H4A H 0.0473 -0.2945 0.1869 0.087 Uiso 1 1 calc R . . H4B H -0.0065 -0.2000 0.2375 0.087 Uiso 1 1 calc R . . H4C H 0.1260 -0.2807 0.2861 0.087 Uiso 1 1 calc R . . C5 C 0.5674(13) -0.0599(9) 0.1996(7) 0.065(4) Uani 1 1 d . . . H5A H 0.6807 -0.0305 0.2156 0.097 Uiso 1 1 calc R . . H5B H 0.4989 -0.0193 0.1544 0.097 Uiso 1 1 calc R . . H5C H 0.5760 -0.1289 0.1792 0.097 Uiso 1 1 calc R . . C8 C -0.0975(13) 0.1652(7) 0.1225(6) 0.034(3) Uani 1 1 d . . . C7 C -0.0041(14) 0.1517(8) 0.0569(6) 0.045(3) Uani 1 1 d . . . H7 H -0.0414 0.1885 0.0058 0.054 Uiso 1 1 calc R . . C6 C 0.1377(14) 0.0895(8) 0.0602(6) 0.035(3) Uani 1 1 d . . . C10 C -0.2611(15) 0.2289(9) 0.1050(7) 0.065(4) Uani 1 1 d . . . H9A H -0.3101 0.2302 0.1561 0.098 Uiso 1 1 calc R . . H9B H -0.3423 0.1990 0.0578 0.098 Uiso 1 1 calc R . . H9C H -0.2345 0.2978 0.0901 0.098 Uiso 1 1 calc R . . C9 C 0.2323(15) 0.0902(10) -0.0150(6) 0.065(4) Uani 1 1 d . . . H10A H 0.3290 0.0441 -0.0024 0.098 Uiso 1 1 calc R . . H10B H 0.2725 0.1585 -0.0229 0.098 Uiso 1 1 calc R . . H10C H 0.1553 0.0683 -0.0671 0.098 Uiso 1 1 calc R . . C11 C 0.2621(12) 0.0567(8) 0.4435(5) 0.043(3) Uani 1 1 d . . . H11A H 0.3552 0.0097 0.4423 0.065 Uiso 1 1 calc R . . H11B H 0.2377 0.0583 0.5009 0.065 Uiso 1 1 calc R . . H11C H 0.2942 0.1242 0.4279 0.065 Uiso 1 1 calc R . . C12 C -0.0731(13) 0.1113(8) 0.3833(6) 0.040(3) Uani 1 1 d . . . H12A H -0.1826 0.0969 0.3462 0.060 Uiso 1 1 calc R . . H12B H -0.0326 0.1773 0.3688 0.060 Uiso 1 1 calc R . . H12C H -0.0859 0.1117 0.4428 0.060 Uiso 1 1 calc R . . O1 O 0.2844(10) -0.2040(5) 0.1422(5) 0.048(2) Uani 1 1 d . . . O2 O 0.5639(9) -0.0295(7) 0.3457(5) 0.067(2) Uani 1 1 d . . . O4 O -0.0556(8) 0.1294(5) 0.2008(4) 0.0361(18) Uani 1 1 d . . . O3 O 0.2022(8) 0.0275(5) 0.1215(4) 0.0357(17) Uani 1 1 d . . . O5 O 0.0231(10) -0.0816(5) 0.4010(4) 0.053(2) Uani 1 1 d . . . S S 0.0769(3) 0.0158(2) 0.36902(14) 0.0283(6) Uani 1 1 d . . . Pt Pt 0.13120(5) 0.02070(3) 0.23716(2) 0.02424(11) 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 C1 0.027(6) 0.049(8) 0.024(6) 0.006(5) 0.005(5) 0.014(6) C2 0.025(6) 0.046(8) 0.019(6) 0.004(5) 0.006(5) 0.002(5) C3 0.037(8) 0.059(9) 0.043(7) 0.009(6) 0.019(6) 0.008(6) C4 0.064(10) 0.037(8) 0.082(9) -0.014(7) 0.038(8) 0.002(6) C5 0.038(7) 0.091(11) 0.075(9) 0.008(7) 0.036(7) 0.001(7) C8 0.046(7) 0.028(7) 0.029(6) 0.004(5) 0.013(5) 0.011(5) C7 0.065(9) 0.046(8) 0.021(6) 0.007(5) 0.003(6) 0.015(6) C6 0.044(7) 0.033(7) 0.031(6) -0.001(5) 0.018(6) 0.003(6) C10 0.068(10) 0.073(10) 0.061(9) 0.032(7) 0.027(7) 0.031(8) C9 0.081(10) 0.099(11) 0.025(7) 0.017(7) 0.031(7) 0.012(8) C11 0.056(8) 0.056(8) 0.016(5) -0.006(5) 0.002(5) -0.003(6) C12 0.048(7) 0.049(8) 0.031(6) -0.012(5) 0.028(6) 0.011(6) O1 0.068(6) 0.033(5) 0.048(5) -0.013(4) 0.021(4) 0.001(4) O2 0.036(5) 0.106(7) 0.055(5) -0.009(6) 0.001(4) 0.005(5) O4 0.042(5) 0.034(4) 0.033(4) 0.009(3) 0.010(4) 0.011(3) O3 0.050(4) 0.038(5) 0.024(4) 0.003(4) 0.019(3) 0.008(4) O5 0.078(6) 0.041(5) 0.047(5) 0.003(4) 0.033(5) -0.006(4) S 0.0423(15) 0.0270(15) 0.0193(12) 0.0013(13) 0.0146(11) -0.0046(14) Pt 0.0295(2) 0.0289(2) 0.01714(18) 0.0013(2) 0.01130(14) 0.0011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.229(10) . ? C1 C2 1.461(13) . ? C1 C4 1.532(13) . ? C2 C3 1.482(13) . ? C2 Pt 2.093(9) . ? C2 H2 0.9800 . ? C3 O2 1.217(12) . ? C3 C5 1.475(13) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 O4 1.294(10) . ? C8 C7 1.395(12) . ? C8 C10 1.513(13) . ? C7 C6 1.375(13) . ? C7 H7 0.9300 . ? C6 O3 1.279(11) . ? C6 C9 1.521(12) . ? C10 H9A 0.9600 . ? C10 H9B 0.9600 . ? C10 H9C 0.9600 . ? C9 H10A 0.9600 . ? C9 H10B 0.9600 . ? C9 H10C 0.9600 . ? C11 S 1.762(9) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 S 1.763(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O4 Pt 2.041(6) . ? O3 Pt 2.010(6) . ? O5 S 1.458(7) . ? S Pt 2.200(2) . ? 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 C1 C2 124.9(10) . . ? O1 C1 C4 117.9(10) . . ? C2 C1 C4 117.2(9) . . ? C1 C2 C3 122.3(9) . . ? C1 C2 Pt 104.0(6) . . ? C3 C2 Pt 109.6(7) . . ? C1 C2 H2 106.7 . . ? C3 C2 H2 106.7 . . ? Pt C2 H2 106.7 . . ? O2 C3 C5 119.9(10) . . ? O2 C3 C2 119.0(9) . . ? C5 C3 C2 121.1(10) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C8 C7 125.8(9) . . ? O4 C8 C10 114.5(9) . . ? C7 C8 C10 119.7(9) . . ? C6 C7 C8 126.5(10) . . ? C6 C7 H7 116.7 . . ? C8 C7 H7 116.7 . . ? O3 C6 C7 126.7(9) . . ? O3 C6 C9 113.8(9) . . ? C7 C6 C9 119.5(10) . . ? C8 C10 H9A 109.5 . . ? C8 C10 H9B 109.5 . . ? H9A C10 H9B 109.5 . . ? C8 C10 H9C 109.5 . . ? H9A C10 H9C 109.5 . . ? H9B C10 H9C 109.5 . . ? C6 C9 H10A 109.5 . . ? C6 C9 H10B 109.5 . . ? H10A C9 H10B 109.5 . . ? C6 C9 H10C 109.5 . . ? H10A C9 H10C 109.5 . . ? H10B C9 H10C 109.5 . . ? S C11 H11A 109.5 . . ? S C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S C12 H12A 109.5 . . ? S C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 O4 Pt 123.2(6) . . ? C6 O3 Pt 124.5(6) . . ? O5 S C11 107.1(5) . . ? O5 S C12 108.5(5) . . ? C11 S C12 101.2(5) . . ? O5 S Pt 118.4(3) . . ? C11 S Pt 108.8(3) . . ? C12 S Pt 111.3(3) . . ? O3 Pt O4 92.0(3) . . ? O3 Pt C2 87.7(3) . . ? O4 Pt C2 175.1(3) . . ? O3 Pt S 175.1(2) . . ? O4 Pt S 90.92(19) . . ? C2 Pt S 89.8(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.733 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.204 #END #BEGIN data_ds68 _database_code_depnum_ccdc_archive 'CCDC 713092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 O4 Pt S' _chemical_formula_sum 'C12 H20 O4 Pt S' _chemical_formula_weight 455.43 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' O O 0.0106 0.0060 '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' 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 8.766(1) _cell_length_b 14.185(2) _cell_length_c 25.006(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.561(2) _cell_angle_gamma 90.00 _cell_volume 3103.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3375 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 9.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details TWINABS _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 'Bruker Smart APEXII CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4838 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3256 _reflns_number_gt 2850 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The crystal was twinned and composed by a major and a minor components (0.87/0.13), which were sufficiently separeted so that two unit cells could be determined. The integration of the data was performed separately for each components. The data set obtained from the major component (Rint=0.0648) was used for the structure solution. The refinement of the structure was performed with the whole set of data using the instruction HKLF 5. ; _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^)+(0.0885P)^2^+54.2482P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3256 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Pt Pt 0.17746(5) 0.37648(4) 0.602509(17) 0.04261(17) Uani 1 1 d . . . S S 0.0047(4) 0.3769(3) 0.66537(13) 0.0542(8) Uani 1 1 d . . . O3 O 0.3352(10) 0.3820(7) 0.5475(3) 0.049(2) Uani 1 1 d . . . O4 O 0.0003(10) 0.3781(8) 0.5447(3) 0.050(2) Uani 1 1 d . . . C2 C 0.3670(16) 0.3690(11) 0.6570(5) 0.050(3) Uani 1 1 d . . . H2 H 0.4566 0.3857 0.6375 0.060 Uiso 1 1 calc R . . C6 C 0.3042(15) 0.3745(11) 0.4972(5) 0.049(3) Uani 1 1 d . . . C8 C 0.0222(18) 0.3686(11) 0.4936(5) 0.055(3) Uani 1 1 d . . . C7 C 0.1556(17) 0.3662(11) 0.4710(5) 0.052(3) Uani 1 1 d . . . H7 H 0.1515 0.3582 0.4340 0.062 Uiso 1 1 calc R . . O1 O 0.4864(15) 0.2227(8) 0.6556(5) 0.077(3) Uani 1 1 d . . . C9 C 0.4420(19) 0.3752(14) 0.4644(7) 0.073(5) Uani 1 1 d . . . H9A H 0.4791 0.4386 0.4616 0.109 Uiso 1 1 calc R . . H9B H 0.4146 0.3511 0.4293 0.109 Uiso 1 1 calc R . . H9C H 0.5206 0.3364 0.4815 0.109 Uiso 1 1 calc R . . C1 C 0.3885(18) 0.2688(11) 0.6755(5) 0.053(3) Uani 1 1 d . . . O2 O 0.3062(14) 0.4306(10) 0.7428(4) 0.076(3) Uani 1 1 d . . . C10 C -0.1257(18) 0.3683(15) 0.4595(6) 0.072(5) Uani 1 1 d . . . H10A H -0.2035 0.3994 0.4784 0.108 Uiso 1 1 calc R . . H10B H -0.1562 0.3045 0.4520 0.108 Uiso 1 1 calc R . . H10C H -0.1117 0.4009 0.4265 0.108 Uiso 1 1 calc R . . C3 C 0.3499(16) 0.4443(12) 0.6991(6) 0.057(4) Uani 1 1 d . . . C4 C 0.291(2) 0.2239(12) 0.7160(7) 0.074(5) Uani 1 1 d . . . H4A H 0.3259 0.2441 0.7513 0.111 Uiso 1 1 calc R . . H4B H 0.2994 0.1566 0.7136 0.111 Uiso 1 1 calc R . . H4C H 0.1867 0.2424 0.7088 0.111 Uiso 1 1 calc R . . C5 C 0.393(2) 0.5416(13) 0.6815(7) 0.075(5) Uani 1 1 d . . . H5A H 0.3079 0.5835 0.6847 0.112 Uiso 1 1 calc R . . H5B H 0.4197 0.5397 0.6449 0.112 Uiso 1 1 calc R . . H5C H 0.4787 0.5638 0.7038 0.112 Uiso 1 1 calc R . . C11 C -0.153(2) 0.313(2) 0.6392(10) 0.122(11) Uani 1 1 d . . . H11A H -0.2328 0.3149 0.6639 0.183 Uiso 1 1 calc R . . H11B H -0.1238 0.2486 0.6337 0.183 Uiso 1 1 calc R . . H11C H -0.1899 0.3399 0.6057 0.183 Uiso 1 1 calc R . . C12 C -0.077(3) 0.4898(16) 0.6623(12) 0.141(13) Uani 1 1 d . . . H12A H -0.0837 0.5114 0.6259 0.211 Uiso 1 1 calc R . . H12B H -0.0141 0.5324 0.6839 0.211 Uiso 1 1 calc R . . H12C H -0.1772 0.4875 0.6756 0.211 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 Pt 0.0413(2) 0.0535(3) 0.0336(2) -0.0021(2) 0.00702(17) -0.0022(3) S 0.0522(17) 0.069(2) 0.0433(16) 0.0023(19) 0.0153(13) -0.0011(19) O3 0.050(5) 0.062(5) 0.034(4) -0.004(4) 0.006(4) -0.006(5) O4 0.043(4) 0.069(6) 0.039(4) 0.000(5) 0.008(3) -0.005(5) C2 0.051(7) 0.061(8) 0.037(6) -0.005(7) 0.010(5) -0.012(7) C6 0.052(7) 0.054(7) 0.041(6) -0.007(7) 0.008(5) 0.006(7) C8 0.072(9) 0.051(8) 0.042(7) 0.013(7) -0.002(6) 0.010(8) C7 0.060(8) 0.058(8) 0.036(6) 0.001(6) -0.009(5) -0.005(7) O1 0.091(9) 0.058(7) 0.085(8) -0.003(6) 0.016(7) 0.024(6) C9 0.069(9) 0.090(12) 0.063(9) -0.028(10) 0.029(8) -0.023(11) C1 0.058(8) 0.062(9) 0.039(7) -0.004(6) 0.002(6) 0.005(7) O2 0.078(8) 0.100(9) 0.051(6) -0.025(6) 0.019(6) -0.013(7) C10 0.061(9) 0.100(13) 0.053(8) -0.008(9) -0.013(7) 0.006(10) C3 0.044(7) 0.070(10) 0.057(8) -0.007(7) 0.002(6) -0.004(7) C4 0.086(12) 0.059(9) 0.076(11) 0.017(8) 0.003(10) 0.010(9) C5 0.095(13) 0.072(11) 0.058(10) -0.011(8) 0.003(9) -0.001(10) C11 0.064(12) 0.19(3) 0.119(19) -0.072(19) 0.044(13) -0.043(15) C12 0.14(2) 0.078(14) 0.22(3) 0.034(17) 0.14(2) 0.026(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt O3 2.011(8) . ? Pt O4 2.055(9) . ? Pt C2 2.085(14) . ? Pt S 2.250(3) . ? S C11 1.75(2) . ? S C12 1.75(2) . ? O3 C6 1.273(15) . ? O4 C8 1.310(16) . ? C2 C1 1.50(2) . ? C2 C3 1.51(2) . ? C2 H2 0.9800 . ? C6 C7 1.427(18) . ? C6 C9 1.502(18) . ? C8 C7 1.33(2) . ? C8 C10 1.51(2) . ? C7 H7 0.9300 . ? O1 C1 1.210(18) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C1 C4 1.50(2) . ? O2 C3 1.197(18) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C3 C5 1.50(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 O3 Pt O4 92.3(3) . . ? O3 Pt C2 84.0(4) . . ? O4 Pt C2 175.6(4) . . ? O3 Pt S 177.4(3) . . ? O4 Pt S 88.8(2) . . ? C2 Pt S 95.0(3) . . ? C11 S C12 98.5(15) . . ? C11 S Pt 106.8(7) . . ? C12 S Pt 105.2(6) . . ? C6 O3 Pt 123.9(8) . . ? C8 O4 Pt 122.3(9) . . ? C1 C2 C3 118.0(12) . . ? C1 C2 Pt 109.2(9) . . ? C3 C2 Pt 108.0(10) . . ? C1 C2 H2 107.0 . . ? C3 C2 H2 107.0 . . ? Pt C2 H2 107.0 . . ? O3 C6 C7 126.4(12) . . ? O3 C6 C9 114.1(12) . . ? C7 C6 C9 119.5(13) . . ? O4 C8 C7 127.0(14) . . ? O4 C8 C10 112.3(13) . . ? C7 C8 C10 120.5(13) . . ? C8 C7 C6 127.1(12) . . ? C8 C7 H7 116.4 . . ? C6 C7 H7 116.4 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C1 C2 117.7(14) . . ? O1 C1 C4 119.5(15) . . ? C2 C1 C4 122.8(13) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C3 C5 121.0(15) . . ? O2 C3 C2 124.9(15) . . ? C5 C3 C2 114.0(13) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S C11 H11A 109.5 . . ? S C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S C12 H12A 109.5 . . ? S C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.331 _refine_diff_density_min -1.407 _refine_diff_density_rms 0.196 #END #BEGIN data_ds64 _database_code_depnum_ccdc_archive 'CCDC 713093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H29 O4 P Pt, C H Cl3' _chemical_formula_sum 'C29 H30 Cl3 O4 P Pt' _chemical_formula_weight 774.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.067(6) _cell_length_b 12.310(4) _cell_length_c 27.577(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.55(1) _cell_angle_gamma 90.00 _cell_volume 5788(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14330 _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 5.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 1.000 _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 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 64056 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.1084 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12637 _reflns_number_gt 6681 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The crystallization solvent molecules (CHCl3) were treated with the Squeeze program since they were severely disordered. The residual density corresponds to 300 e/cell and the residual volume to 705 A3/cell. This corresponded roughly to 1 CHCl3 molecule per each platinum complex. ; _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^)+(0.0026P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12637 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.255098(15) 0.07112(2) 0.118980(10) 0.04486(8) Uani 1 1 d . . . Pt2 Pt 0.245655(16) 0.64854(2) 0.395278(10) 0.04686(8) Uani 1 1 d . . . P2 P 0.15426(10) 0.53258(14) 0.36848(6) 0.0444(5) Uani 1 1 d . . . P1 P 0.34754(10) 0.18416(14) 0.14716(6) 0.0411(5) Uani 1 1 d . . . O31 O 0.1689(3) -0.0309(3) 0.09208(16) 0.0603(14) Uani 1 1 d . . . O32 O 0.3311(3) 0.7553(3) 0.41955(17) 0.0639(15) Uani 1 1 d . . . O41 O 0.1789(2) 0.2015(4) 0.11385(17) 0.0656(15) Uani 1 1 d . . . C111 C 0.4497(3) 0.1414(5) 0.1427(2) 0.0380(16) Uani 1 1 d . . . C22 C 0.1724(4) 0.7796(5) 0.3857(3) 0.054(2) Uani 1 1 d . . . H22 H 0.1185 0.7536 0.3883 0.065 Uiso 1 1 calc R . . C51 C 0.2402(4) -0.1781(6) 0.1789(3) 0.097(3) Uani 1 1 d . . . H51A H 0.2501 -0.2549 0.1783 0.145 Uiso 1 1 calc R . . H51B H 0.2023 -0.1598 0.1534 0.145 Uiso 1 1 calc R . . H51C H 0.2202 -0.1583 0.2097 0.145 Uiso 1 1 calc R . . C141 C 0.6006(5) 0.0638(6) 0.1309(3) 0.074(2) Uani 1 1 d . . . H141 H 0.6510 0.0373 0.1272 0.088 Uiso 1 1 calc R . . C21 C 0.3275(4) -0.0630(5) 0.1244(2) 0.0473(18) Uani 1 1 d . . . H21 H 0.3817 -0.0365 0.1253 0.057 Uiso 1 1 calc R . . C171 C 0.3384(4) 0.2154(5) 0.2103(2) 0.0402(17) Uani 1 1 d . . . C251 C 0.3127(5) 0.4047(7) 0.0371(3) 0.078(3) Uani 1 1 d . . . H251 H 0.2981 0.4014 0.0043 0.094 Uiso 1 1 calc R . . C221 C 0.2729(4) 0.1819(5) 0.2338(2) 0.055(2) Uani 1 1 d . . . H221 H 0.2355 0.1393 0.2173 0.065 Uiso 1 1 calc R . . C62 C 0.4008(5) 0.7289(6) 0.4311(3) 0.060(2) Uani 1 1 d . . . C181 C 0.3935(4) 0.2799(5) 0.2370(2) 0.0492(19) Uani 1 1 d . . . H181 H 0.4384 0.3033 0.2222 0.059 Uiso 1 1 calc R . . C151 C 0.5625(4) 0.0412(6) 0.1726(3) 0.065(2) Uani 1 1 d . . . H151 H 0.5870 -0.0007 0.1968 0.077 Uiso 1 1 calc R . . C231 C 0.3400(4) 0.3121(5) 0.1136(2) 0.0452(18) Uani 1 1 d . . . C92 C 0.4527(4) 0.8233(6) 0.4467(3) 0.110(3) Uani 1 1 d . . . H92A H 0.4649 0.8654 0.4187 0.165 Uiso 1 1 calc R . . H92B H 0.5003 0.7963 0.4621 0.165 Uiso 1 1 calc R . . H92C H 0.4258 0.8681 0.4691 0.165 Uiso 1 1 calc R . . C281 C 0.3555(4) 0.4147(6) 0.1348(2) 0.056(2) Uani 1 1 d . . . H281 H 0.3702 0.4194 0.1676 0.067 Uiso 1 1 calc R . . C81 C 0.1082(4) 0.1964(6) 0.0979(3) 0.060(2) Uani 1 1 d . . . C161 C 0.4875(4) 0.0807(5) 0.1785(2) 0.0512(19) Uani 1 1 d . . . H161 H 0.4625 0.0660 0.2071 0.061 Uiso 1 1 calc R . . C121 C 0.4890(4) 0.1632(5) 0.1012(2) 0.056(2) Uani 1 1 d . . . H121 H 0.4643 0.2045 0.0768 0.068 Uiso 1 1 calc R . . C71 C 0.0694(4) 0.1016(7) 0.0834(2) 0.061(2) Uani 1 1 d . . . H71 H 0.0167 0.1091 0.0740 0.073 Uiso 1 1 calc R . . C241 C 0.3192(4) 0.3117(6) 0.0640(3) 0.060(2) Uani 1 1 d . . . H241 H 0.3093 0.2455 0.0487 0.072 Uiso 1 1 calc R . . C261 C 0.3278(4) 0.5021(7) 0.0588(3) 0.072(2) Uani 1 1 d . . . H261 H 0.3235 0.5654 0.0404 0.086 Uiso 1 1 calc R . . C271 C 0.3490(4) 0.5086(6) 0.1071(3) 0.071(2) Uani 1 1 d . . . H271 H 0.3591 0.5759 0.1213 0.086 Uiso 1 1 calc R . . C131 C 0.5650(4) 0.1250(6) 0.0948(3) 0.073(2) Uani 1 1 d . . . H131 H 0.5908 0.1407 0.0667 0.088 Uiso 1 1 calc R . . C12 C 0.1807(5) 0.8196(6) 0.3345(3) 0.078(3) Uani 1 1 d . . . C101 C 0.0663(4) 0.3072(6) 0.0944(3) 0.109(3) Uani 1 1 d . . . H10A H 0.0515 0.3293 0.1261 0.164 Uiso 1 1 calc R . . H10B H 0.0203 0.3011 0.0733 0.164 Uiso 1 1 calc R . . H10C H 0.1011 0.3603 0.0816 0.164 Uiso 1 1 calc R . . O21 O 0.3636(3) -0.1093(5) 0.2055(2) 0.124(3) Uani 1 1 d . . . O11 O 0.2918(3) -0.2248(4) 0.08083(19) 0.099(2) Uani 1 1 d . . . O22 O 0.2165(4) 0.9527(4) 0.4161(2) 0.111(2) Uani 1 1 d . . . C232 C 0.1619(4) 0.5026(5) 0.3052(2) 0.0428(18) Uani 1 1 d . . . C282 C 0.2285(4) 0.5363(5) 0.2817(3) 0.057(2) Uani 1 1 d . . . H282 H 0.2661 0.5785 0.2984 0.068 Uiso 1 1 calc R . . C112 C 0.0515(4) 0.5705(5) 0.3746(3) 0.0497(19) Uani 1 1 d . . . C162 C 0.0071(4) 0.6176(6) 0.3381(3) 0.065(2) Uani 1 1 d . . . H162 H 0.0280 0.6286 0.3079 0.078 Uiso 1 1 calc R . . C242 C 0.1065(4) 0.4420(6) 0.2773(3) 0.063(2) Uani 1 1 d . . . H242 H 0.0600 0.4218 0.2911 0.075 Uiso 1 1 calc R . . C272 C 0.2393(5) 0.5075(6) 0.2339(3) 0.070(2) Uani 1 1 d . . . H272 H 0.2838 0.5308 0.2186 0.084 Uiso 1 1 calc R . . O42 O 0.3234(3) 0.5211(4) 0.40445(17) 0.0651(15) Uani 1 1 d . . . C191 C 0.3825(4) 0.3083(6) 0.2832(3) 0.062(2) Uani 1 1 d . . . H191 H 0.4202 0.3506 0.2997 0.075 Uiso 1 1 calc R . . C201 C 0.3176(5) 0.2768(7) 0.3064(3) 0.067(2) Uani 1 1 d . . . H201 H 0.3101 0.2988 0.3381 0.080 Uiso 1 1 calc R . . C91 C 0.0462(4) -0.0936(6) 0.0644(3) 0.097(3) Uani 1 1 d . . . H91A H 0.0697 -0.1321 0.0385 0.146 Uiso 1 1 calc R . . H91B H -0.0035 -0.0644 0.0529 0.146 Uiso 1 1 calc R . . H91C H 0.0383 -0.1424 0.0909 0.146 Uiso 1 1 calc R . . C182 C 0.1471(4) 0.3031(6) 0.3782(3) 0.060(2) Uani 1 1 d . . . H182 H 0.1299 0.3005 0.3457 0.072 Uiso 1 1 calc R . . C211 C 0.2621(5) 0.2109(6) 0.2817(3) 0.068(2) Uani 1 1 d . . . H211 H 0.2183 0.1865 0.2974 0.082 Uiso 1 1 calc R . . C41 C 0.3368(4) -0.0803(7) 0.0325(2) 0.094(3) Uani 1 1 d . . . H41A H 0.3471 -0.1360 0.0092 0.141 Uiso 1 1 calc R . . H41B H 0.3825 -0.0356 0.0375 0.141 Uiso 1 1 calc R . . H41C H 0.2936 -0.0364 0.0205 0.141 Uiso 1 1 calc R . . C172 C 0.1638(4) 0.4025(5) 0.4008(3) 0.0481(19) Uani 1 1 d . . . C222 C 0.1868(4) 0.4011(7) 0.4499(3) 0.067(2) Uani 1 1 d . . . H222 H 0.1985 0.4663 0.4657 0.081 Uiso 1 1 calc R . . C11 C 0.3164(4) -0.1324(7) 0.0801(3) 0.065(2) Uani 1 1 d . . . C31 C 0.3155(5) -0.1174(6) 0.1713(3) 0.070(2) Uani 1 1 d . . . C61 C 0.0995(5) -0.0019(7) 0.0814(2) 0.056(2) Uani 1 1 d . . . C192 C 0.1567(5) 0.2068(6) 0.4056(3) 0.079(3) Uani 1 1 d . . . H192 H 0.1488 0.1401 0.3902 0.094 Uiso 1 1 calc R . . O12 O 0.1255(4) 0.8103(5) 0.3045(2) 0.149(3) Uani 1 1 d . . . C82 C 0.3942(5) 0.5319(7) 0.4190(3) 0.061(2) Uani 1 1 d . . . C42 C 0.2564(5) 0.8690(7) 0.3193(3) 0.108(3) Uani 1 1 d . . . H42A H 0.2638 0.8527 0.2858 0.162 Uiso 1 1 calc R . . H42B H 0.2993 0.8397 0.3389 0.162 Uiso 1 1 calc R . . H42C H 0.2545 0.9464 0.3236 0.162 Uiso 1 1 calc R . . C202 C 0.1772(5) 0.2088(7) 0.4534(3) 0.079(3) Uani 1 1 d . . . H202 H 0.1807 0.1445 0.4711 0.095 Uiso 1 1 calc R . . C102 C 0.4372(4) 0.4236(6) 0.4236(3) 0.107(3) Uani 1 1 d . . . H10D H 0.4102 0.3769 0.4452 0.160 Uiso 1 1 calc R . . H10E H 0.4898 0.4358 0.4363 0.160 Uiso 1 1 calc R . . H10F H 0.4387 0.3900 0.3923 0.160 Uiso 1 1 calc R . . C212 C 0.1926(5) 0.3060(8) 0.4756(3) 0.083(3) Uani 1 1 d . . . H212 H 0.2072 0.3078 0.5084 0.100 Uiso 1 1 calc R . . C52 C 0.1715(4) 0.8298(7) 0.4756(3) 0.104(3) Uani 1 1 d . . . H52A H 0.2183 0.8015 0.4915 0.155 Uiso 1 1 calc R . . H52B H 0.1314 0.7750 0.4748 0.155 Uiso 1 1 calc R . . H52C H 0.1539 0.8920 0.4931 0.155 Uiso 1 1 calc R . . C262 C 0.1844(5) 0.4446(7) 0.2089(3) 0.077(3) Uani 1 1 d . . . H262 H 0.1924 0.4245 0.1769 0.093 Uiso 1 1 calc R . . C72 C 0.4327(4) 0.6272(7) 0.4314(3) 0.074(3) Uani 1 1 d . . . H72 H 0.4856 0.6216 0.4407 0.089 Uiso 1 1 calc R . . C142 C -0.1019(5) 0.6354(7) 0.3901(4) 0.091(3) Uani 1 1 d . . . H142 H -0.1536 0.6558 0.3946 0.109 Uiso 1 1 calc R . . C152 C -0.0692(5) 0.6493(6) 0.3462(3) 0.085(3) Uani 1 1 d . . . H152 H -0.0990 0.6809 0.3209 0.102 Uiso 1 1 calc R . . C252 C 0.1185(5) 0.4118(7) 0.2308(3) 0.076(3) Uani 1 1 d . . . H252 H 0.0817 0.3688 0.2140 0.091 Uiso 1 1 calc R . . C32 C 0.1881(4) 0.8619(7) 0.4256(3) 0.072(2) Uani 1 1 d . . . C122 C 0.0180(4) 0.5597(5) 0.4196(3) 0.071(2) Uani 1 1 d . . . H122 H 0.0475 0.5302 0.4455 0.085 Uiso 1 1 calc R . . C132 C -0.0585(5) 0.5924(7) 0.4262(3) 0.091(3) Uani 1 1 d . . . H132 H -0.0796 0.5840 0.4564 0.109 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 0.03702(16) 0.04054(17) 0.05653(19) -0.00306(15) -0.00352(13) -0.00168(16) Pt2 0.04029(17) 0.04109(18) 0.05887(19) -0.00367(15) -0.00146(13) 0.00033(16) P2 0.0381(12) 0.0389(12) 0.0563(13) -0.0034(9) 0.0032(9) 0.0035(9) P1 0.0384(11) 0.0382(12) 0.0465(12) -0.0014(9) 0.0014(9) 0.0017(9) O31 0.041(3) 0.049(3) 0.089(4) 0.001(3) -0.019(3) 0.000(2) O32 0.046(3) 0.046(3) 0.098(4) 0.001(3) -0.015(3) -0.001(3) O41 0.027(3) 0.062(4) 0.107(4) -0.014(3) -0.013(3) -0.001(3) C111 0.034(4) 0.036(4) 0.044(4) -0.015(4) 0.004(3) -0.009(3) C22 0.048(5) 0.052(5) 0.062(5) 0.000(4) 0.002(4) -0.009(4) C51 0.102(7) 0.088(7) 0.099(7) 0.047(5) -0.007(5) -0.036(6) C141 0.050(6) 0.068(6) 0.103(7) -0.019(6) 0.000(5) 0.013(5) C21 0.043(4) 0.048(5) 0.050(5) 0.002(4) -0.007(3) -0.007(4) C171 0.037(4) 0.035(4) 0.049(5) 0.010(3) 0.001(4) 0.011(3) C251 0.118(8) 0.057(6) 0.058(6) 0.011(5) -0.015(5) 0.005(6) C221 0.051(5) 0.056(5) 0.057(5) -0.004(4) 0.007(4) 0.001(4) C62 0.055(6) 0.054(6) 0.068(6) 0.001(5) -0.012(4) -0.012(5) C181 0.038(4) 0.067(5) 0.042(5) -0.007(4) 0.000(4) 0.003(4) C151 0.053(6) 0.058(6) 0.082(6) -0.013(5) -0.007(5) 0.022(4) C231 0.038(4) 0.044(5) 0.054(5) 0.006(4) 0.006(4) 0.008(4) C92 0.074(6) 0.081(7) 0.170(9) 0.007(6) -0.050(6) -0.030(5) C281 0.076(6) 0.049(5) 0.044(5) 0.000(4) 0.009(4) 0.006(5) C81 0.040(5) 0.066(6) 0.073(6) -0.009(4) -0.003(4) 0.006(5) C161 0.045(5) 0.055(5) 0.053(5) -0.006(4) -0.007(4) -0.001(4) C121 0.062(6) 0.045(5) 0.063(5) 0.002(4) 0.006(4) 0.002(4) C71 0.033(5) 0.076(7) 0.072(6) 0.001(5) -0.014(4) -0.008(4) C241 0.064(5) 0.059(6) 0.056(5) -0.005(4) -0.013(4) -0.001(4) C261 0.086(6) 0.067(7) 0.062(6) 0.022(5) -0.006(5) 0.005(5) C271 0.098(7) 0.025(5) 0.093(7) 0.008(5) 0.020(6) -0.002(4) C131 0.052(6) 0.081(7) 0.089(7) -0.007(5) 0.031(5) 0.007(5) C12 0.085(7) 0.060(6) 0.086(7) 0.015(5) -0.034(6) 0.000(5) C101 0.064(6) 0.064(6) 0.197(10) -0.017(6) -0.026(6) 0.033(5) O21 0.106(5) 0.160(7) 0.102(5) 0.060(4) -0.044(4) -0.060(4) O11 0.133(5) 0.058(4) 0.105(5) -0.022(4) -0.019(4) -0.007(4) O22 0.140(6) 0.045(4) 0.146(6) -0.014(4) -0.009(4) -0.002(4) C232 0.030(4) 0.039(4) 0.059(5) 0.006(4) 0.003(4) 0.014(3) C282 0.070(6) 0.039(5) 0.061(6) -0.008(4) 0.005(4) 0.011(4) C112 0.044(5) 0.029(4) 0.077(6) -0.009(4) 0.005(4) -0.006(4) C162 0.041(5) 0.072(6) 0.081(6) -0.014(5) -0.005(4) 0.013(4) C242 0.050(5) 0.076(6) 0.060(5) -0.012(5) -0.014(4) 0.019(4) C272 0.072(6) 0.064(6) 0.074(6) 0.012(5) 0.029(5) 0.019(5) O42 0.033(3) 0.057(4) 0.104(4) -0.018(3) -0.012(3) 0.004(3) C191 0.055(5) 0.075(6) 0.056(6) -0.010(4) -0.001(4) 0.010(4) C201 0.072(6) 0.088(7) 0.040(5) -0.011(5) -0.008(5) 0.026(5) C91 0.068(6) 0.078(7) 0.143(8) 0.005(6) -0.027(5) -0.030(5) C182 0.061(5) 0.062(6) 0.057(5) -0.014(5) 0.011(4) 0.003(5) C211 0.077(6) 0.074(6) 0.056(6) 0.005(5) 0.033(5) 0.018(5) C41 0.089(7) 0.137(9) 0.057(6) -0.014(6) 0.010(5) 0.011(6) C172 0.037(4) 0.044(5) 0.063(5) -0.003(4) 0.008(4) 0.001(4) C222 0.079(6) 0.066(6) 0.055(6) 0.003(5) -0.014(4) -0.010(5) C11 0.056(5) 0.046(6) 0.091(7) -0.029(5) -0.014(5) 0.013(4) C31 0.071(6) 0.058(6) 0.079(6) 0.014(5) -0.021(5) -0.009(5) C61 0.053(5) 0.060(6) 0.055(5) -0.001(4) -0.008(4) -0.018(5) C192 0.094(7) 0.026(5) 0.117(8) 0.002(5) 0.028(6) 0.002(5) O12 0.145(6) 0.173(7) 0.124(6) 0.073(5) -0.059(5) -0.065(5) C82 0.042(5) 0.065(6) 0.076(6) -0.012(5) -0.003(4) 0.023(5) C42 0.106(8) 0.111(8) 0.108(7) 0.041(6) 0.004(6) -0.040(6) C202 0.090(7) 0.068(7) 0.080(7) 0.017(6) 0.008(6) 0.015(6) C102 0.058(6) 0.087(7) 0.173(9) -0.037(7) -0.025(6) 0.018(5) C212 0.085(7) 0.085(7) 0.077(7) 0.008(6) -0.013(5) -0.010(6) C52 0.111(8) 0.143(10) 0.057(6) -0.015(6) 0.011(5) 0.041(6) C262 0.086(7) 0.081(7) 0.062(6) -0.010(5) -0.020(6) 0.031(6) C72 0.042(5) 0.082(7) 0.097(7) -0.009(6) -0.021(4) -0.001(5) C142 0.039(6) 0.069(7) 0.165(11) -0.014(7) 0.011(6) 0.005(5) C152 0.048(6) 0.068(6) 0.136(9) -0.038(6) -0.020(5) 0.027(5) C252 0.062(6) 0.097(7) 0.068(6) -0.018(5) -0.015(5) 0.014(5) C32 0.056(5) 0.046(6) 0.113(8) -0.006(6) -0.015(5) 0.015(5) C122 0.062(6) 0.044(5) 0.109(7) 0.004(5) 0.027(5) 0.009(4) C132 0.057(6) 0.068(7) 0.151(9) 0.012(6) 0.044(6) 0.010(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 Pt1 O31 2.048(4) . ? Pt1 C21 2.064(6) . ? Pt1 O41 2.067(4) . ? Pt1 P1 2.2182(18) . ? Pt2 C22 2.051(7) . ? Pt2 O32 2.053(4) . ? Pt2 O42 2.063(4) . ? Pt2 P2 2.2169(18) . ? P2 C232 1.793(7) . ? P2 C112 1.830(7) . ? P2 C172 1.836(7) . ? P1 C171 1.796(6) . ? P1 C231 1.829(6) . ? P1 C111 1.831(6) . ? O31 C61 1.259(7) . ? O32 C62 1.260(7) . ? O41 C81 1.267(7) . ? C111 C161 1.377(7) . ? C111 C121 1.378(8) . ? C22 C12 1.509(9) . ? C22 C32 1.510(9) . ? C22 H22 0.9800 . ? C51 C31 1.509(9) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C141 C131 1.369(9) . ? C141 C151 1.373(9) . ? C141 H141 0.9300 . ? C21 C31 1.480(8) . ? C21 C11 1.494(8) . ? C21 H21 0.9800 . ? C171 C221 1.381(7) . ? C171 C181 1.412(7) . ? C251 C261 1.358(9) . ? C251 C241 1.366(8) . ? C251 H251 0.9300 . ? C221 C211 1.389(8) . ? C221 H221 0.9300 . ? C62 C72 1.365(9) . ? C62 C92 1.512(8) . ? C181 C191 1.341(7) . ? C181 H181 0.9300 . ? C151 C161 1.385(8) . ? C151 H151 0.9300 . ? C231 C241 1.397(8) . ? C231 C281 1.412(8) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C281 C271 1.388(8) . ? C281 H281 0.9300 . ? C81 C71 1.392(9) . ? C81 C101 1.541(9) . ? C161 H161 0.9300 . ? C121 C131 1.399(8) . ? C121 H121 0.9300 . ? C71 C61 1.376(9) . ? C71 H71 0.9300 . ? C241 H241 0.9300 . ? C261 C271 1.367(8) . ? C261 H261 0.9300 . ? C271 H271 0.9300 . ? C131 H131 0.9300 . ? C12 O12 1.231(8) . ? C12 C42 1.504(10) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? O21 C31 1.226(7) . ? O11 C11 1.213(8) . ? O22 C32 1.250(8) . ? C232 C282 1.397(8) . ? C232 C242 1.406(8) . ? C282 C272 1.387(8) . ? C282 H282 0.9300 . ? C112 C162 1.362(8) . ? C112 C122 1.394(8) . ? C162 C152 1.387(8) . ? C162 H162 0.9300 . ? C242 C252 1.358(8) . ? C242 H242 0.9300 . ? C272 C262 1.376(9) . ? C272 H272 0.9300 . ? O42 C82 1.263(7) . ? C191 C201 1.361(8) . ? C191 H191 0.9300 . ? C201 C211 1.400(9) . ? C201 H201 0.9300 . ? C91 C61 1.511(8) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C182 C172 1.397(8) . ? C182 C192 1.411(9) . ? C182 H182 0.9300 . ? C211 H211 0.9300 . ? C41 C11 1.517(9) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C172 C222 1.393(8) . ? C222 C212 1.369(9) . ? C222 H222 0.9300 . ? C192 C202 1.350(9) . ? C192 H192 0.9300 . ? C82 C72 1.381(9) . ? C82 C102 1.524(9) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C202 C212 1.365(9) . ? C202 H202 0.9300 . ? C102 H10D 0.9600 . ? C102 H10E 0.9600 . ? C102 H10F 0.9600 . ? C212 H212 0.9300 . ? C52 C32 1.476(9) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C262 C252 1.362(9) . ? C262 H262 0.9300 . ? C72 H72 0.9300 . ? C142 C132 1.324(10) . ? C142 C152 1.368(10) . ? C142 H142 0.9300 . ? C152 H152 0.9300 . ? C252 H252 0.9300 . ? C122 C132 1.386(9) . ? C122 H122 0.9300 . ? C132 H132 0.9300 . ? 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 O31 Pt1 C21 87.3(2) . . ? O31 Pt1 O41 90.68(17) . . ? C21 Pt1 O41 177.8(2) . . ? O31 Pt1 P1 178.88(13) . . ? C21 Pt1 P1 93.57(18) . . ? O41 Pt1 P1 88.41(13) . . ? C22 Pt2 O32 87.6(2) . . ? C22 Pt2 O42 177.5(2) . . ? O32 Pt2 O42 90.19(18) . . ? C22 Pt2 P2 92.7(2) . . ? O32 Pt2 P2 179.38(15) . . ? O42 Pt2 P2 89.45(13) . . ? C232 P2 C112 104.7(3) . . ? C232 P2 C172 106.5(3) . . ? C112 P2 C172 104.0(3) . . ? C232 P2 Pt2 112.1(2) . . ? C112 P2 Pt2 117.9(2) . . ? C172 P2 Pt2 110.7(2) . . ? C171 P1 C231 107.4(3) . . ? C171 P1 C111 104.5(3) . . ? C231 P1 C111 105.0(3) . . ? C171 P1 Pt1 112.5(2) . . ? C231 P1 Pt1 109.3(2) . . ? C111 P1 Pt1 117.4(2) . . ? C61 O31 Pt1 124.3(5) . . ? C62 O32 Pt2 124.4(5) . . ? C81 O41 Pt1 124.9(5) . . ? C161 C111 C121 118.2(6) . . ? C161 C111 P1 121.7(5) . . ? C121 C111 P1 120.0(5) . . ? C12 C22 C32 116.2(7) . . ? C12 C22 Pt2 107.1(5) . . ? C32 C22 Pt2 110.3(5) . . ? C12 C22 H22 107.6 . . ? C32 C22 H22 107.6 . . ? Pt2 C22 H22 107.6 . . ? C31 C51 H51A 109.5 . . ? C31 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C31 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C131 C141 C151 120.6(8) . . ? C131 C141 H141 119.7 . . ? C151 C141 H141 119.7 . . ? C31 C21 C11 116.0(7) . . ? C31 C21 Pt1 108.6(5) . . ? C11 C21 Pt1 110.1(4) . . ? C31 C21 H21 107.2 . . ? C11 C21 H21 107.2 . . ? Pt1 C21 H21 107.2 . . ? C221 C171 C181 117.1(6) . . ? C221 C171 P1 119.9(5) . . ? C181 C171 P1 122.8(5) . . ? C261 C251 C241 119.5(7) . . ? C261 C251 H251 120.3 . . ? C241 C251 H251 120.3 . . ? C171 C221 C211 121.0(7) . . ? C171 C221 H221 119.5 . . ? C211 C221 H221 119.5 . . ? O32 C62 C72 127.6(7) . . ? O32 C62 C92 114.0(7) . . ? C72 C62 C92 118.3(7) . . ? C191 C181 C171 121.6(7) . . ? C191 C181 H181 119.2 . . ? C171 C181 H181 119.2 . . ? C141 C151 C161 120.2(7) . . ? C141 C151 H151 119.9 . . ? C161 C151 H151 119.9 . . ? C241 C231 C281 116.3(6) . . ? C241 C231 P1 120.1(5) . . ? C281 C231 P1 123.6(5) . . ? C62 C92 H92A 109.5 . . ? C62 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C62 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C271 C281 C231 120.5(6) . . ? C271 C281 H281 119.7 . . ? C231 C281 H281 119.7 . . ? O41 C81 C71 125.1(7) . . ? O41 C81 C101 114.2(7) . . ? C71 C81 C101 120.7(7) . . ? C111 C161 C151 120.7(7) . . ? C111 C161 H161 119.6 . . ? C151 C161 H161 119.6 . . ? C111 C121 C131 121.8(7) . . ? C111 C121 H121 119.1 . . ? C131 C121 H121 119.1 . . ? C61 C71 C81 127.9(7) . . ? C61 C71 H71 116.1 . . ? C81 C71 H71 116.1 . . ? C251 C241 C231 122.6(7) . . ? C251 C241 H241 118.7 . . ? C231 C241 H241 118.7 . . ? C251 C261 C271 121.1(8) . . ? C251 C261 H261 119.4 . . ? C271 C261 H261 119.4 . . ? C261 C271 C281 119.9(7) . . ? C261 C271 H271 120.0 . . ? C281 C271 H271 120.0 . . ? C141 C131 C121 118.6(7) . . ? C141 C131 H131 120.7 . . ? C121 C131 H131 120.7 . . ? O12 C12 C42 119.5(8) . . ? O12 C12 C22 119.8(8) . . ? C42 C12 C22 120.7(7) . . ? C81 C101 H10A 109.5 . . ? C81 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C81 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C282 C232 C242 116.4(7) . . ? C282 C232 P2 119.0(6) . . ? C242 C232 P2 124.5(6) . . ? C272 C282 C232 120.7(7) . . ? C272 C282 H282 119.7 . . ? C232 C282 H282 119.7 . . ? C162 C112 C122 117.5(7) . . ? C162 C112 P2 122.9(6) . . ? C122 C112 P2 119.3(6) . . ? C112 C162 C152 119.8(8) . . ? C112 C162 H162 120.1 . . ? C152 C162 H162 120.1 . . ? C252 C242 C232 122.4(7) . . ? C252 C242 H242 118.8 . . ? C232 C242 H242 118.8 . . ? C262 C272 C282 120.3(8) . . ? C262 C272 H272 119.8 . . ? C282 C272 H272 119.8 . . ? C82 O42 Pt2 124.1(5) . . ? C181 C191 C201 121.6(7) . . ? C181 C191 H191 119.2 . . ? C201 C191 H191 119.2 . . ? C191 C201 C211 118.9(7) . . ? C191 C201 H201 120.5 . . ? C211 C201 H201 120.5 . . ? C61 C91 H91A 109.5 . . ? C61 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C61 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C172 C182 C192 118.7(7) . . ? C172 C182 H182 120.6 . . ? C192 C182 H182 120.6 . . ? C221 C211 C201 119.7(7) . . ? C221 C211 H211 120.1 . . ? C201 C211 H211 120.1 . . ? C11 C41 H41A 109.5 . . ? C11 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C11 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C222 C172 C182 117.8(7) . . ? C222 C172 P2 119.9(6) . . ? C182 C172 P2 122.3(6) . . ? C212 C222 C172 121.6(7) . . ? C212 C222 H222 119.2 . . ? C172 C222 H222 119.2 . . ? O11 C11 C21 123.7(8) . . ? O11 C11 C41 120.2(7) . . ? C21 C11 C41 116.1(7) . . ? O21 C31 C21 121.4(7) . . ? O21 C31 C51 118.7(7) . . ? C21 C31 C51 119.8(6) . . ? O31 C61 C71 127.0(7) . . ? O31 C61 C91 114.1(7) . . ? C71 C61 C91 118.8(7) . . ? C202 C192 C182 121.8(8) . . ? C202 C192 H192 119.1 . . ? C182 C192 H192 119.1 . . ? O42 C82 C72 127.3(7) . . ? O42 C82 C102 112.7(7) . . ? C72 C82 C102 120.0(7) . . ? C12 C42 H42A 109.5 . . ? C12 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C12 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C192 C202 C212 119.3(8) . . ? C192 C202 H202 120.3 . . ? C212 C202 H202 120.3 . . ? C82 C102 H10D 109.5 . . ? C82 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C82 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C202 C212 C222 120.8(8) . . ? C202 C212 H212 119.6 . . ? C222 C212 H212 119.6 . . ? C32 C52 H52A 109.5 . . ? C32 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C32 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C252 C262 C272 120.0(8) . . ? C252 C262 H262 120.0 . . ? C272 C262 H262 120.0 . . ? C62 C72 C82 126.3(7) . . ? C62 C72 H72 116.8 . . ? C82 C72 H72 116.8 . . ? C132 C142 C152 118.5(9) . . ? C132 C142 H142 120.7 . . ? C152 C142 H142 120.7 . . ? C142 C152 C162 122.0(9) . . ? C142 C152 H152 119.0 . . ? C162 C152 H152 119.0 . . ? C242 C252 C262 120.1(8) . . ? C242 C252 H252 120.0 . . ? C262 C252 H252 120.0 . . ? O22 C32 C52 121.8(8) . . ? O22 C32 C22 120.4(8) . . ? C52 C32 C22 117.8(7) . . ? C132 C122 C112 121.0(8) . . ? C132 C122 H122 119.5 . . ? C112 C122 H122 119.5 . . ? C142 C132 C122 121.2(9) . . ? C142 C132 H132 119.4 . . ? C122 C132 H132 119.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.255 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.101 # 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 0.500 -0.051 0.250 179 75 ' ' 2 0.500 0.051 0.750 179 75 ' ' 3 0.000 0.336 0.250 174 73 ' ' 4 0.000 0.664 0.750 173 77 ' ' _platon_squeeze_details ; ; #END