Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_year 2005 _publ_contact_author_name 'Philip Gale' _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email PHILIP.GALE@SOTON.AC.UK _publ_section_title ; Tetrakis(thiourea)platinum (II) oxocarbodianions salts as molecular building blocks for the synthesis of hydrogen bonded networks in the solid state ; loop_ _publ_author_name 'Philip Gale' 'Mark E. Light' 'Roberto Quesada' #===END data_2005sot0384 _database_code_depnum_ccdc_archive 'CCDC 284038' # Compound 6 _chemical_compound_source 'Roberto Quesada' _database_code_CSD 5SOT0384 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H21 N8 O7.50 Pt S4' _chemical_formula_weight 684.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 17.518(4) _cell_length_b 13.767(3) _cell_length_c 9.0857(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.32(3) _cell_angle_gamma 90.00 _cell_volume 2190.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2574 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Shard _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 6.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5480 _exptl_absorpt_correction_T_max 0.8754 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 8838 reflections reduced R(int) from 0.0695 to 0.0561 Ratio of minimum to maximum apparent transmission: 0.764139 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12592 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2506 _reflns_number_gt 1883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were located in geometrical positions and refined using a riding model, except those on the water which were refined with universal temperature factors and fixed distances. ; _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^)+(0.0226P)^2^+4.1169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00041(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2506 _refine_ls_number_parameters 152 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 C3 C 0.0000 0.8290(5) 0.2500 0.0161(15) Uani 1 2 d S . . C4 C -0.0535(3) 0.7652(3) 0.1694(5) 0.0170(11) Uani 1 1 d . . . C5 C -0.0330(2) 0.6641(4) 0.1987(5) 0.0164(10) Uani 1 1 d . . . O4 O -0.22794(18) 0.6090(3) 0.1614(4) 0.0213(8) Uani 1 1 d D . . O5 O 0.0000 1.1528(9) 0.2500 0.049(3) Uani 0.50 2 d SPD . . C1 C 0.1432(3) 0.9600(3) -0.0216(5) 0.0164(10) Uani 1 1 d . . . C2 C 0.3518(3) 0.8598(3) 0.2555(5) 0.0158(10) Uani 1 1 d . . . N1 N 0.0956(2) 1.0173(3) 0.0467(4) 0.0183(9) Uani 1 1 d . . . H1A H 0.0960 1.0803 0.0296 0.022 Uiso 1 1 calc R . . H1B H 0.0633 0.9928 0.1096 0.022 Uiso 1 1 calc R . . N2 N 0.1917(2) 0.9980(3) -0.1163(4) 0.0175(9) Uani 1 1 d . . . H2A H 0.1917 1.0610 -0.1328 0.021 Uiso 1 1 calc R . . H2B H 0.2237 0.9601 -0.1626 0.021 Uiso 1 1 calc RD . . N3 N 0.3212(2) 0.7896(3) 0.3326(5) 0.0210(9) Uani 1 1 d . . . H3A H 0.3340 0.7824 0.4262 0.025 Uiso 1 1 calc R . . H3B H 0.2880 0.7498 0.2906 0.025 Uiso 1 1 calc R . . N4 N 0.4020(2) 0.9200(3) 0.3190(4) 0.0196(9) Uani 1 1 d . . . H4A H 0.4147 0.9128 0.4126 0.024 Uiso 1 1 calc R . . H4B H 0.4224 0.9670 0.2674 0.024 Uiso 1 1 calc R . . O1 O 0.0000 0.9193(3) 0.2500 0.0161(10) Uani 1 2 d S . . O2 O -0.10733(18) 0.7937(2) 0.0863(4) 0.0206(8) Uani 1 1 d . . . O3 O -0.06605(17) 0.5916(2) 0.1468(3) 0.0175(7) Uani 1 1 d . . . S1 S 0.13695(7) 0.83619(9) 0.01444(15) 0.0208(3) Uani 1 1 d . . . S2 S 0.32763(7) 0.88007(9) 0.07166(13) 0.0171(3) Uani 1 1 d . . . Pt1 Pt 0.2500 0.7500 0.0000 0.01251(11) Uani 1 2 d S . . H96 H -0.025(10) 1.194(14) 0.20(2) 0.040 Uiso 0.25 1 d PD . . H97 H 0.046(4) 1.153(13) 0.23(3) 0.040 Uiso 0.25 1 d PD . . H98 H -0.1861(15) 0.609(3) 0.200(4) 0.040 Uiso 1 1 d D . . H99 H -0.232(3) 0.565(3) 0.098(5) 0.040 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C3 0.018(4) 0.016(4) 0.014(4) 0.000 0.009(3) 0.000 C4 0.021(3) 0.019(3) 0.011(2) 0.002(2) -0.0006(19) -0.003(2) C5 0.018(2) 0.015(3) 0.016(3) 0.004(2) 0.0046(19) 0.002(2) O4 0.0196(17) 0.018(2) 0.026(2) -0.0054(16) -0.0034(15) 0.0024(15) O5 0.031(7) 0.040(9) 0.075(10) 0.000 -0.022(7) 0.000 C1 0.016(2) 0.017(3) 0.016(3) 0.002(2) -0.0065(19) 0.000(2) C2 0.019(2) 0.013(3) 0.015(2) 0.000(2) -0.0031(19) 0.0020(19) N1 0.021(2) 0.010(2) 0.024(2) 0.0046(18) 0.0058(18) 0.0046(17) N2 0.020(2) 0.013(2) 0.020(2) 0.0042(18) 0.0049(17) 0.0048(17) N3 0.031(2) 0.016(2) 0.016(2) 0.0026(19) -0.0036(18) -0.0124(19) N4 0.028(2) 0.012(2) 0.019(2) 0.0012(18) -0.0068(17) -0.0049(18) O1 0.022(2) 0.009(3) 0.018(3) 0.000 0.0046(19) 0.000 O2 0.0265(19) 0.0139(18) 0.021(2) 0.0023(16) -0.0085(15) 0.0014(15) O3 0.0217(17) 0.0096(18) 0.0208(19) -0.0027(15) -0.0051(14) -0.0041(14) S1 0.0184(6) 0.0112(6) 0.0331(8) 0.0022(6) 0.0055(5) 0.0002(5) S2 0.0250(6) 0.0111(6) 0.0149(6) 0.0019(5) -0.0040(5) -0.0030(5) Pt1 0.01703(15) 0.00849(15) 0.01195(15) -0.00015(12) -0.00113(9) -0.00029(11) _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 C3 O1 1.244(8) . ? C3 C4 1.467(6) . ? C3 C4 1.467(6) 2 ? C4 O2 1.257(6) . ? C4 C5 1.461(6) . ? C5 O3 1.241(6) . ? C5 C5 1.469(9) 2 ? C1 N1 1.314(6) . ? C1 N2 1.330(6) . ? C1 S1 1.739(5) . ? C2 N3 1.314(6) . ? C2 N4 1.329(6) . ? C2 S2 1.737(5) . ? S1 Pt1 2.3150(12) . ? S2 Pt1 2.3321(12) . ? Pt1 S1 2.3150(12) 7_565 ? Pt1 S2 2.3321(12) 7_565 ? 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 C3 C4 126.7(3) . . ? O1 C3 C4 126.7(3) . 2 ? C4 C3 C4 106.6(6) . 2 ? O2 C4 C5 125.7(4) . . ? O2 C4 C3 125.1(4) . . ? C5 C4 C3 109.1(4) . . ? O3 C5 C4 125.9(4) . . ? O3 C5 C5 126.5(3) . 2 ? C4 C5 C5 107.6(3) . 2 ? N1 C1 N2 119.4(4) . . ? N1 C1 S1 117.2(3) . . ? N2 C1 S1 123.4(4) . . ? N3 C2 N4 120.0(4) . . ? N3 C2 S2 122.5(4) . . ? N4 C2 S2 117.5(4) . . ? C1 S1 Pt1 115.73(16) . . ? C2 S2 Pt1 105.83(16) . . ? S1 Pt1 S1 180.0 7_565 . ? S1 Pt1 S2 85.14(5) 7_565 . ? S1 Pt1 S2 94.86(5) . . ? S1 Pt1 S2 94.86(5) 7_565 7_565 ? S1 Pt1 S2 85.14(5) . 7_565 ? S2 Pt1 S2 180.0 . 7_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O1 0.88 1.99 2.860(4) 171.3 . O4 H99 N2 0.84(3) 2.51(3) 3.244(6) 146(5) 3_445 O4 H99 S2 0.84(3) 2.77(5) 3.404(4) 134(5) 3_445 N2 H2A O2 0.88 2.53 3.241(5) 138.5 5_575 N1 H1A O2 0.88 2.04 2.878(5) 158.3 5_575 N2 H2B O4 0.88 2.06 2.892(5) 157.3 8_565 N4 H4A O3 0.88 2.15 3.022(5) 172.5 8_566 N3 H3A O2 0.88 2.05 2.839(5) 148.8 8_566 N4 H4B O3 0.88 2.05 2.896(5) 161.3 3 N3 H3B O4 0.88 2.25 2.976(5) 139.4 2 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.116 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.204 #===END data_2005sot0383 _database_code_depnum_ccdc_archive 'CCDC 284039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pt S4 C4 N8 H16, 4(S O C2 H6), C5 O5 ' _chemical_formula_sum 'C17 H40 N8 O9 Pt S8' _chemical_formula_weight 952.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 17.315(4) _cell_length_b 9.4289(19) _cell_length_c 23.344(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.70(3) _cell_angle_gamma 90.00 _cell_volume 3630.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4374 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Translucent Pale Yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 4.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4178 _exptl_absorpt_correction_T_max 0.4178 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 18055 reflections reduced R(int) from 0.0991 to 0.0398 Ratio of minimum to maximum apparent transmission: 0.701321 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21798 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4155 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0217P)^2^+16.7700P] 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 SHELXL _refine_ls_extinction_coef 0.00031(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4155 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.2500 0.7500 0.0000 0.01386(7) Uani 1 2 d S . . S1 S 0.23980(5) 0.91209(9) 0.07232(4) 0.02067(18) Uani 1 1 d . . . S2 S 0.36096(5) 0.63272(9) 0.06332(4) 0.02537(19) Uani 1 1 d . . . S3 S 0.34559(5) 1.18023(10) -0.01668(4) 0.02603(19) Uani 1 1 d . . . S4 S 0.24064(6) 1.20137(11) -0.22339(5) 0.0346(2) Uani 1 1 d . . . O4 O 0.36815(17) 1.0261(3) -0.01509(11) 0.0329(6) Uani 1 1 d . . . N2 N 0.13133(17) 0.7240(3) 0.08761(13) 0.0200(6) Uani 1 1 d . . . H2A H 0.0932 0.6970 0.1030 0.024 Uiso 1 1 calc R . . H2B H 0.1485 0.6654 0.0648 0.024 Uiso 1 1 calc R . . N1 N 0.13666(16) 0.9400(3) 0.13317(12) 0.0201(6) Uani 1 1 d . . . H1A H 0.0985 0.9127 0.1485 0.024 Uiso 1 1 calc R . . H1B H 0.1575 1.0257 0.1407 0.024 Uiso 1 1 calc R . . C1 C 0.16273(18) 0.8523(3) 0.09874(13) 0.0159(6) Uani 1 1 d . . . N3 N 0.47384(18) 0.7004(3) 0.16338(13) 0.0250(6) Uani 1 1 d . . . H3A H 0.5088 0.7569 0.1883 0.030 Uiso 1 1 calc R . . H3B H 0.4702 0.6109 0.1730 0.030 Uiso 1 1 calc R . . C6 C 0.3682(2) 1.2339(4) 0.05998(17) 0.0274(8) Uani 1 1 d . . . H6A H 0.3345 1.1802 0.0792 0.041 Uiso 1 1 calc R . . H6B H 0.3571 1.3355 0.0618 0.041 Uiso 1 1 calc R . . H6C H 0.4256 1.2156 0.0811 0.041 Uiso 1 1 calc R . . N4 N 0.43227(16) 0.8839(3) 0.09729(13) 0.0217(6) Uani 1 1 d . . . H4A H 0.4673 0.9400 0.1223 0.026 Uiso 1 1 calc R . . H4B H 0.4010 0.9174 0.0628 0.026 Uiso 1 1 calc R . . C8 C 0.2118(3) 1.0529(5) -0.1880(2) 0.0443(10) Uani 1 1 d . . . H8A H 0.2603 1.0089 -0.1605 0.066 Uiso 1 1 calc R . . H8B H 0.1836 0.9838 -0.2186 0.066 Uiso 1 1 calc R . . H8C H 0.1756 1.0838 -0.1653 0.066 Uiso 1 1 calc R . . C7 C 0.4253(2) 1.2742(4) -0.03315(19) 0.0335(9) Uani 1 1 d . . . H7A H 0.4776 1.2431 -0.0058 0.050 Uiso 1 1 calc R . . H7B H 0.4186 1.3761 -0.0280 0.050 Uiso 1 1 calc R . . H7C H 0.4237 1.2552 -0.0748 0.050 Uiso 1 1 calc R . . C2 C 0.4266(2) 0.7501(3) 0.11136(15) 0.0185(7) Uani 1 1 d . . . O5 O 0.2861(2) 1.2956(3) -0.17374(15) 0.0570(9) Uani 1 1 d . . . C9 C 0.3139(2) 1.1152(5) -0.2501(2) 0.0432(10) Uani 1 1 d . . . H9A H 0.3369 1.1832 -0.2722 0.065 Uiso 1 1 calc R . . H9B H 0.2882 1.0373 -0.2769 0.065 Uiso 1 1 calc R . . H9C H 0.3572 1.0773 -0.2160 0.065 Uiso 1 1 calc R . . O1 O 0.0000 0.4290(3) 0.2500 0.0203(7) Uani 1 2 d S . . O2 O 0.03830(13) 0.6106(2) 0.16071(9) 0.0180(5) Uani 1 1 d . . . O3 O 0.01937(14) 0.9079(2) 0.19315(11) 0.0242(5) Uani 1 1 d . . . C5 C 0.01041(18) 0.8009(4) 0.22198(14) 0.0172(6) Uani 1 1 d . . . C4 C 0.01925(18) 0.6530(3) 0.20535(13) 0.0155(6) Uani 1 1 d . . . C3 C 0.0000 0.5603(5) 0.2500 0.0161(9) Uani 1 2 d S . . 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 0.01724(10) 0.01098(10) 0.01595(10) -0.00272(6) 0.00892(7) -0.00319(6) S1 0.0244(4) 0.0179(4) 0.0252(4) -0.0091(3) 0.0157(3) -0.0078(3) S2 0.0278(4) 0.0127(4) 0.0291(5) -0.0029(3) -0.0011(4) -0.0016(3) S3 0.0255(4) 0.0237(5) 0.0273(4) 0.0011(4) 0.0056(4) -0.0012(4) S4 0.0374(5) 0.0256(5) 0.0385(5) -0.0028(4) 0.0083(4) 0.0004(4) O4 0.0516(17) 0.0189(13) 0.0275(13) -0.0040(10) 0.0110(12) -0.0035(12) N2 0.0249(14) 0.0163(14) 0.0229(14) -0.0029(11) 0.0133(12) -0.0042(11) N1 0.0252(14) 0.0163(14) 0.0233(14) -0.0026(11) 0.0142(12) -0.0023(11) C1 0.0158(14) 0.0173(16) 0.0148(14) 0.0025(12) 0.0049(12) 0.0001(12) N3 0.0288(15) 0.0114(13) 0.0286(16) 0.0000(12) -0.0006(13) -0.0007(12) C6 0.035(2) 0.0173(18) 0.0300(19) -0.0018(14) 0.0107(16) 0.0010(15) N4 0.0205(14) 0.0147(14) 0.0277(15) -0.0007(11) 0.0036(12) -0.0009(11) C8 0.052(3) 0.038(2) 0.045(2) 0.003(2) 0.018(2) -0.008(2) C7 0.031(2) 0.031(2) 0.040(2) 0.0089(17) 0.0147(18) -0.0010(16) C2 0.0182(15) 0.0144(16) 0.0242(16) -0.0034(12) 0.0085(13) -0.0012(12) O5 0.083(3) 0.0298(16) 0.054(2) -0.0169(16) 0.0136(19) -0.0147(18) C9 0.0254(19) 0.054(3) 0.048(3) -0.003(2) 0.0070(18) 0.0047(19) O1 0.0279(17) 0.0125(16) 0.0237(16) 0.000 0.0125(14) 0.000 O2 0.0232(11) 0.0171(11) 0.0169(11) -0.0018(9) 0.0109(9) -0.0025(9) O3 0.0320(13) 0.0153(12) 0.0320(13) 0.0056(10) 0.0199(11) 0.0035(10) C5 0.0156(14) 0.0151(15) 0.0218(16) 0.0011(13) 0.0070(12) 0.0005(13) C4 0.0124(13) 0.0173(16) 0.0167(14) 0.0014(12) 0.0041(11) -0.0012(12) C3 0.0137(19) 0.018(2) 0.017(2) 0.000 0.0046(16) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S2 2.3177(11) 7_565 ? Pt1 S2 2.3177(11) . ? Pt1 S1 2.3235(8) 7_565 ? Pt1 S1 2.3235(8) . ? S1 C1 1.726(3) . ? S2 C2 1.732(3) . ? S3 O4 1.502(3) . ? S3 C7 1.778(4) . ? S3 C6 1.785(4) . ? S4 O5 1.482(3) . ? S4 C9 1.772(4) . ? S4 C8 1.772(4) . ? N2 C1 1.319(4) . ? N1 C1 1.325(4) . ? N3 C2 1.327(4) . ? N4 C2 1.315(4) . ? O1 C3 1.239(5) . ? O2 C4 1.250(4) . ? O3 C5 1.248(4) . ? C5 C5 1.459(6) 2 ? C5 C4 1.468(5) . ? C4 C3 1.474(4) . ? C3 C4 1.474(4) 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 S2 Pt1 S2 180.00(4) 7_565 . ? S2 Pt1 S1 94.69(4) 7_565 7_565 ? S2 Pt1 S1 85.31(4) . 7_565 ? S2 Pt1 S1 85.31(4) 7_565 . ? S2 Pt1 S1 94.69(4) . . ? S1 Pt1 S1 180.00(3) 7_565 . ? C1 S1 Pt1 106.41(11) . . ? C2 S2 Pt1 111.18(11) . . ? O4 S3 C7 105.91(18) . . ? O4 S3 C6 105.87(16) . . ? C7 S3 C6 97.3(2) . . ? O5 S4 C9 106.4(2) . . ? O5 S4 C8 105.5(2) . . ? C9 S4 C8 97.7(2) . . ? N2 C1 N1 119.8(3) . . ? N2 C1 S1 123.1(2) . . ? N1 C1 S1 117.1(2) . . ? N4 C2 N3 119.7(3) . . ? N4 C2 S2 122.4(3) . . ? N3 C2 S2 117.9(2) . . ? O3 C5 C5 126.05(18) . 2 ? O3 C5 C4 125.8(3) . . ? C5 C5 C4 108.13(17) 2 . ? O2 C4 C5 126.8(3) . . ? O2 C4 C3 125.0(3) . . ? C5 C4 C3 108.2(3) . . ? O1 C3 C4 126.35(19) . . ? O1 C3 C4 126.35(19) . 2 ? C4 C3 C4 107.3(4) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.88 2.04 2.885(3) 160.7 . N1 H1A O3 0.88 1.96 2.812(3) 163.0 . N4 H4B O4 0.88 2.01 2.853(4) 159.1 . N2 H2B O4 0.88 2.12 2.904(4) 148.4 7_565 N1 H1B O5 0.88 1.98 2.851(4) 168.8 7_575 N3 H3A O1 0.88 2.21 2.895(4) 134.9 3 N4 H4A O2 0.88 2.06 2.911(4) 163.7 3 N3 H3B O3 0.88 2.09 2.895(4) 151.6 3_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.345 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.113 # Attachment 'Gale_Quesada_Light_Combined_Rev.cif' data_2005sot0432 _database_code_depnum_ccdc_archive 'CCDC 289742' # Compound 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H40 N8 O8 Pt S8' _chemical_formula_weight 924.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 16.3461(14) _cell_length_b 10.1444(6) _cell_length_c 11.1430(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1847.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2395 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Slab _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 4.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6733 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 13544 reflections reduced R(int) from 0.1076 to 0.0571 Ratio of minimum to maximum apparent transmission: 0.649599 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17029 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4206 _reflns_number_gt 3509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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 structrue us refined as a racemic twin 45/55. The solvent DMSO is loosley bound in channels and suffers from high thermal motion, and leaves large residual peaks. ; _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^)+(0.0813P)^2^+9.8254P] 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 SHELXL _refine_ls_extinction_coef 0.0032(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.458(19) _refine_ls_number_reflns 4206 _refine_ls_number_parameters 194 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.936 _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 0.5000 0.0000 1.06114(4) 0.03540(18) Uani 1 2 d S . . S1 S 0.39909(15) 0.0092(7) 0.9149(2) 0.0502(8) Uani 1 1 d . . . S2 S 0.39918(14) 0.0107(7) 1.2071(2) 0.0502(8) Uani 1 1 d . . . N2 N 0.4559(6) 0.2533(9) 0.8799(7) 0.044(2) Uani 1 1 d U . . H2A H 0.4577 0.3289 0.8413 0.053 Uiso 1 1 calc R . . H2B H 0.4858 0.2416 0.9448 0.053 Uiso 1 1 calc R . . N1 N 0.3630(6) 0.1750(11) 0.7425(8) 0.052(2) Uani 1 1 d U . . H1A H 0.3650 0.2507 0.7042 0.063 Uiso 1 1 calc R . . H1B H 0.3312 0.1113 0.7161 0.063 Uiso 1 1 calc R . . N3 N 0.4605(6) 0.2504(10) 1.2495(8) 0.052(2) Uani 1 1 d U . . H3A H 0.4605 0.3267 1.2869 0.063 Uiso 1 1 calc R . . H3B H 0.4936 0.2372 1.1884 0.063 Uiso 1 1 calc R . . C1 C 0.4080(6) 0.1568(11) 0.8404(8) 0.042(2) Uani 1 1 d U . . C2 C 0.4119(6) 0.1576(10) 1.2843(10) 0.044(2) Uani 1 1 d U . . O1 O 0.5000 0.5000 0.3603(7) 0.066(3) Uani 1 2 d SU . . O3 O 0.5000 0.5000 0.7700(7) 0.066(3) Uani 1 2 d SU . . C5 C 0.5000 0.5000 0.6577(12) 0.062(4) Uani 1 2 d SU . . O2 O 0.3882(6) 0.3632(9) 0.5644(8) 0.065(2) Uani 1 1 d U . . N4 N 0.3609(7) 0.1756(9) 1.3775(10) 0.061(3) Uani 1 1 d U . . H4A H 0.3602 0.2515 1.4157 0.073 Uiso 1 1 calc R . . H4B H 0.3281 0.1115 1.4002 0.073 Uiso 1 1 calc R . . C4 C 0.4502(10) 0.4390(11) 0.5625(11) 0.064(3) Uani 1 1 d U . . C3 C 0.5000 0.5000 0.4727(10) 0.051(3) Uani 1 2 d SU . . S3 S 0.3346(2) 0.6637(4) 0.0607(4) 0.0769(10) Uani 1 1 d D . . O4 O 0.4221(5) 0.7069(9) 0.0616(8) 0.074(3) Uani 1 1 d DU . . C6 C 0.3145(9) 0.6274(19) -0.0865(13) 0.099(5) Uani 1 1 d DU . . H6A H 0.3189 0.7078 -0.1349 0.149 Uiso 1 1 calc R . . H6B H 0.2590 0.5916 -0.0934 0.149 Uiso 1 1 calc R . . H6C H 0.3540 0.5620 -0.1154 0.149 Uiso 1 1 calc R . . C7 C 0.3375(7) 0.5027(14) 0.1159(14) 0.087(4) Uani 1 1 d DU . . H7A H 0.3795 0.4524 0.0729 0.131 Uiso 1 1 calc R . . H7B H 0.2841 0.4608 0.1042 0.131 Uiso 1 1 calc R . . H7C H 0.3507 0.5044 0.2017 0.131 Uiso 1 1 calc R . . S4 S 0.1695(5) 0.3444(6) 0.4130(6) 0.151(3) Uani 1 1 d D . . O5 O 0.1913(6) 0.4867(10) 0.4321(9) 0.105(4) Uani 1 1 d DU . . C8 C 0.0660(11) 0.346(2) 0.397(2) 0.164(10) Uani 1 1 d DU . . H8A H 0.0418 0.4018 0.4594 0.246 Uiso 1 1 calc R . . H8B H 0.0449 0.2557 0.4054 0.246 Uiso 1 1 calc R . . H8C H 0.0517 0.3802 0.3179 0.246 Uiso 1 1 calc R . . C9 C 0.1743(9) 0.2646(14) 0.5517(12) 0.082(4) Uani 1 1 d DU . . H9A H 0.2190 0.3021 0.5994 0.122 Uiso 1 1 calc R . . H9B H 0.1842 0.1704 0.5391 0.122 Uiso 1 1 calc R . . H9C H 0.1225 0.2767 0.5944 0.122 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 0.0382(2) 0.0305(2) 0.0375(2) 0.000 0.000 -0.0014(3) S1 0.0503(12) 0.0520(19) 0.0484(13) 0.008(2) -0.0116(9) -0.019(2) S2 0.0410(11) 0.057(2) 0.0522(14) -0.023(2) 0.0047(9) 0.0002(19) N2 0.057(5) 0.047(5) 0.030(4) 0.008(4) 0.002(4) -0.005(4) N1 0.052(5) 0.067(6) 0.037(4) -0.001(4) 0.000(4) -0.001(5) N3 0.065(6) 0.048(5) 0.044(5) -0.016(4) -0.002(4) 0.008(4) C1 0.046(5) 0.052(6) 0.029(5) -0.005(4) 0.006(4) 0.011(5) C2 0.040(5) 0.042(5) 0.049(6) -0.004(5) 0.000(4) 0.015(4) O1 0.131(9) 0.035(4) 0.033(4) 0.000 0.000 0.009(13) O3 0.124(8) 0.045(5) 0.029(4) 0.000 0.000 0.007(13) C5 0.106(10) 0.037(6) 0.044(7) 0.000 0.000 0.006(14) O2 0.094(6) 0.061(5) 0.041(4) 0.002(4) -0.004(5) 0.020(5) N4 0.074(7) 0.032(5) 0.075(7) -0.013(5) 0.017(6) 0.001(5) C4 0.120(10) 0.037(5) 0.035(5) -0.003(5) -0.017(7) 0.038(6) C3 0.089(9) 0.035(6) 0.030(5) 0.000 0.000 0.016(13) S3 0.071(2) 0.065(2) 0.095(3) 0.010(2) 0.012(2) -0.0066(17) O4 0.082(6) 0.086(6) 0.056(5) 0.003(5) 0.003(5) -0.043(5) C6 0.083(10) 0.132(13) 0.084(10) 0.011(9) -0.015(8) -0.037(9) C7 0.066(7) 0.069(7) 0.127(10) 0.030(10) -0.013(7) -0.030(9) S4 0.215(7) 0.114(4) 0.124(5) 0.045(4) 0.061(5) 0.094(5) O5 0.087(6) 0.112(8) 0.115(8) 0.071(9) -0.018(5) -0.004(7) C8 0.180(17) 0.156(16) 0.156(16) 0.065(13) -0.030(14) -0.090(14) C9 0.091(10) 0.077(9) 0.077(9) 0.015(8) 0.007(8) 0.010(7) _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 S2 2.318(2) 2_655 ? Pt1 S2 2.318(2) . ? Pt1 S1 2.320(2) 2_655 ? Pt1 S1 2.320(2) . ? S1 C1 1.718(13) . ? S2 C2 1.734(12) . ? N2 C1 1.329(14) . ? N1 C1 1.329(13) . ? N3 C2 1.291(15) . ? C2 N4 1.345(14) . ? O1 C3 1.252(15) . ? O3 C5 1.252(15) . ? C5 C4 1.472(16) 2_665 ? C5 C4 1.472(16) . ? O2 C4 1.273(17) . ? C4 C3 1.431(18) . ? C3 C4 1.431(18) 2_665 ? S3 O4 1.496(8) . ? S3 C6 1.712(14) . ? S3 C7 1.747(12) . ? S4 O5 1.502(10) . ? S4 C8 1.701(15) . ? S4 C9 1.746(12) . ? 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 S2 Pt1 S2 90.90(13) 2_655 . ? S2 Pt1 S1 89.15(9) 2_655 2_655 ? S2 Pt1 S1 179.6(3) . 2_655 ? S2 Pt1 S1 179.6(3) 2_655 . ? S2 Pt1 S1 89.15(9) . . ? S1 Pt1 S1 90.80(13) 2_655 . ? C1 S1 Pt1 108.3(4) . . ? C2 S2 Pt1 107.6(4) . . ? N1 C1 N2 119.7(10) . . ? N1 C1 S1 118.1(9) . . ? N2 C1 S1 122.2(8) . . ? N3 C2 N4 121.0(10) . . ? N3 C2 S2 123.5(8) . . ? N4 C2 S2 115.2(9) . . ? O3 C5 C4 136.0(7) . 2_665 ? O3 C5 C4 136.0(7) . . ? C4 C5 C4 87.9(15) 2_665 . ? O2 C4 C3 136.5(11) . . ? O2 C4 C5 133.0(12) . . ? C3 C4 C5 90.5(11) . . ? O1 C3 C4 134.4(7) . 2_665 ? O1 C3 C4 134.4(7) . . ? C4 C3 C4 91.2(13) 2_665 . ? O4 S3 C6 104.7(6) . . ? O4 S3 C7 104.2(6) . . ? C6 S3 C7 98.1(8) . . ? O5 S4 C8 104.1(9) . . ? O5 S4 C9 108.1(7) . . ? C8 S4 C9 98.0(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O3 0.88 2.03 2.878(9) 161.4 . N1 H1A O2 0.88 1.97 2.785(13) 153.9 . N2 H2B O4 0.88 2.06 2.870(12) 153.0 2_666 N3 H3B O4 0.88 2.05 2.873(13) 154.6 2_666 N3 H3A O1 0.88 2.04 2.891(10) 161.3 1_556 N4 H4A O2 0.88 2.06 2.857(13) 150.3 1_556 N1 H1B O5 0.88 2.11 2.867(13) 143.5 3_546 N4 H4B O5 0.88 2.28 2.984(16) 137.0 3_547 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.598 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.170 #===END data_2005sot0271 _database_code_depnum_ccdc_archive 'CCDC 289743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(Pt(S C N2 H4)4), 2Cl, 6((C H3)2S O), 2(C4 O4), 2((C H3)2C O)' _chemical_formula_sum 'C38 H96 Cl2 N24 O16 Pt3 S18' _chemical_formula_weight 2378.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.1828(16) _cell_length_b 14.1183(13) _cell_length_c 14.4599(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.579(6) _cell_angle_gamma 90.00 _cell_volume 4264.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Slab _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 5.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4070 _exptl_absorpt_correction_T_max 0.7713 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 31762 reflections reduced R(int) from 0.1038 to 0.0541 Ratio of minimum to maximum apparent transmission: 0.697838 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48953 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9760 _reflns_number_gt 7356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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 biggest peaks in the difference map are located near each Pt ; _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^)+(0.0270P)^2^+4.2275P] 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 9760 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.346033(9) 0.028778(13) 0.098598(13) 0.01373(6) Uani 1 1 d . . . S1 S 0.34291(6) 0.10232(9) -0.04503(9) 0.0176(3) Uani 1 1 d . . . S2 S 0.34366(6) -0.11465(9) 0.02126(9) 0.0192(3) Uani 1 1 d . . . S3 S 0.37595(6) -0.04851(9) 0.24127(9) 0.0195(3) Uani 1 1 d . . . S4 S 0.36489(6) 0.17213(9) 0.17721(9) 0.0201(3) Uani 1 1 d . . . N1 N 0.2901(2) 0.0471(3) -0.2132(3) 0.0297(12) Uani 1 1 d . . . H1A H 0.2585 0.0288 -0.2570 0.036 Uiso 1 1 calc R . . H1B H 0.3281 0.0587 -0.2277 0.036 Uiso 1 1 calc R . . N2 N 0.22323(19) 0.0394(3) -0.1048(3) 0.0224(10) Uani 1 1 d . . . H2A H 0.1918 0.0211 -0.1489 0.027 Uiso 1 1 calc R . . H2B H 0.2166 0.0459 -0.0467 0.027 Uiso 1 1 calc R . . N3 N 0.2370(2) -0.1578(3) 0.0886(3) 0.0249(11) Uani 1 1 d . . . H3A H 0.2092 -0.1979 0.1055 0.030 Uiso 1 1 calc R . . H3B H 0.2292 -0.0965 0.0883 0.030 Uiso 1 1 calc R . . N4 N 0.3023(2) -0.2802(3) 0.0637(3) 0.0255(11) Uani 1 1 d . . . H4A H 0.2749 -0.3211 0.0805 0.031 Uiso 1 1 calc R . . H4B H 0.3380 -0.3005 0.0468 0.031 Uiso 1 1 calc R . . N5 N 0.2641(2) 0.0106(3) 0.2825(3) 0.0231(10) Uani 1 1 d . . . H5A H 0.2363 0.0185 0.3209 0.028 Uiso 1 1 calc R . . H5B H 0.2542 0.0283 0.2235 0.028 Uiso 1 1 calc R . . N6 N 0.33427(19) -0.0537(3) 0.4021(3) 0.0205(10) Uani 1 1 d . . . H6A H 0.3062 -0.0455 0.4400 0.025 Uiso 1 1 calc R . . H6B H 0.3718 -0.0793 0.4233 0.025 Uiso 1 1 calc R . . N7 N 0.34139(19) 0.3453(3) 0.1145(3) 0.0212(10) Uani 1 1 d . . . H7A H 0.3177 0.3915 0.0863 0.025 Uiso 1 1 calc R . . H7B H 0.3810 0.3566 0.1418 0.025 Uiso 1 1 calc R . . N8 N 0.25848(19) 0.2426(3) 0.0751(3) 0.0190(10) Uani 1 1 d . . . H8A H 0.2349 0.2889 0.0470 0.023 Uiso 1 1 calc R . . H8B H 0.2424 0.1852 0.0760 0.023 Uiso 1 1 calc R . . C1 C 0.2806(2) 0.0570(4) -0.1261(3) 0.0188(11) Uani 1 1 d . . . C2 C 0.2898(2) -0.1892(4) 0.0637(4) 0.0201(12) Uani 1 1 d . . . C3 C 0.3200(2) -0.0274(3) 0.3131(4) 0.0178(11) Uani 1 1 d . . . C4 C 0.3175(2) 0.2593(4) 0.1159(3) 0.0178(12) Uani 1 1 d . . . Pt2 Pt 0.0000 0.0000 0.0000 0.01188(7) Uani 1 2 d S . . S5 S 0.06336(6) -0.13467(8) 0.03065(9) 0.0171(3) Uani 1 1 d . . . S6 S -0.05392(6) -0.02595(9) 0.12575(9) 0.0170(3) Uani 1 1 d . . . N9 N -0.04794(19) -0.2279(3) -0.0184(3) 0.0192(10) Uani 1 1 d . . . H9A H -0.0705 -0.2805 -0.0269 0.023 Uiso 1 1 calc R . . H9B H -0.0667 -0.1729 -0.0319 0.023 Uiso 1 1 calc R . . N10 N 0.0415(2) -0.3167(3) 0.0346(3) 0.0221(10) Uani 1 1 d . . . H10A H 0.0181 -0.3684 0.0256 0.026 Uiso 1 1 calc R . . H10B H 0.0827 -0.3207 0.0566 0.026 Uiso 1 1 calc R . . N11 N -0.0212(2) -0.0287(3) 0.3082(3) 0.0197(10) Uani 1 1 d . . . H11A H 0.0053 -0.0250 0.3619 0.024 Uiso 1 1 calc R . . H11B H -0.0622 -0.0384 0.3077 0.024 Uiso 1 1 calc R . . N12 N 0.0624(2) -0.0051(3) 0.2296(3) 0.0191(10) Uani 1 1 d . . . H12A H 0.0886 -0.0015 0.2836 0.023 Uiso 1 1 calc R . . H12B H 0.0774 0.0010 0.1767 0.023 Uiso 1 1 calc R . . C5 C 0.0144(2) -0.2317(3) 0.0147(3) 0.0173(11) Uani 1 1 d . . . C6 C 0.0010(2) -0.0196(3) 0.2281(3) 0.0160(11) Uani 1 1 d . . . O1 O 0.05534(16) 0.4560(2) -0.0128(2) 0.0208(8) Uani 1 1 d . . . O2 O 0.15896(16) 0.4544(2) 0.1817(2) 0.0225(8) Uani 1 1 d . . . O3 O 0.26994(16) 0.5158(2) 0.0630(3) 0.0203(8) Uani 1 1 d . . . O4 O 0.16412(17) 0.5288(3) -0.1250(3) 0.0276(9) Uani 1 1 d . . . C7 C 0.1136(2) 0.4757(3) 0.0108(4) 0.0159(11) Uani 1 1 d . . . C8 C 0.1606(2) 0.4744(3) 0.0979(4) 0.0170(11) Uani 1 1 d . . . C9 C 0.2101(2) 0.5040(3) 0.0446(4) 0.0163(11) Uani 1 1 d . . . C10 C 0.1628(2) 0.5082(3) -0.0408(4) 0.0171(11) Uani 1 1 d . . . S7 S 0.54357(7) 0.05539(11) 0.23294(11) 0.0356(4) Uani 1 1 d . . . O5 O 0.58016(19) -0.0340(3) 0.2587(3) 0.0395(11) Uani 1 1 d . . . C11 C 0.5162(3) 0.0474(4) 0.1107(4) 0.0306(14) Uani 1 1 d . . . H11C H 0.5519 0.0297 0.0790 0.046 Uiso 1 1 calc R . . H11D H 0.4990 0.1089 0.0870 0.046 Uiso 1 1 calc R . . H11E H 0.4825 -0.0007 0.0984 0.046 Uiso 1 1 calc R . . C12 C 0.6018(3) 0.1451(5) 0.2261(5) 0.062(2) Uani 1 1 d . . . H12C H 0.6281 0.1539 0.2880 0.093 Uiso 1 1 calc R . . H12D H 0.5801 0.2047 0.2056 0.093 Uiso 1 1 calc R . . H12E H 0.6292 0.1261 0.1810 0.093 Uiso 1 1 calc R . . S8 S 0.83009(8) 0.17269(11) 0.23990(11) 0.0374(4) Uani 1 1 d . . . O6 O 0.82904(17) 0.1903(2) 0.3428(2) 0.0242(9) Uani 1 1 d . . . C13 C 0.7773(3) 0.2575(5) 0.1785(5) 0.058(2) Uani 1 1 d . . . H13A H 0.7340 0.2470 0.1917 0.088 Uiso 1 1 calc R . . H13B H 0.7772 0.2510 0.1110 0.088 Uiso 1 1 calc R . . H13C H 0.7916 0.3213 0.1988 0.088 Uiso 1 1 calc R . . C14 C 0.9039(3) 0.2214(5) 0.2173(4) 0.0487(19) Uani 1 1 d . . . H14A H 0.9092 0.2856 0.2432 0.073 Uiso 1 1 calc R . . H14B H 0.9034 0.2237 0.1494 0.073 Uiso 1 1 calc R . . H14C H 0.9395 0.1816 0.2468 0.073 Uiso 1 1 calc R . . S9 S 0.48752(8) 0.70620(12) 0.02457(13) 0.0453(4) Uani 1 1 d . . . O7 O 0.42905(17) 0.6507(2) 0.0323(3) 0.0301(9) Uani 1 1 d . . . C15 C 0.5512(3) 0.6253(4) 0.0454(5) 0.0445(18) Uani 1 1 d . . . H15A H 0.5500 0.5916 0.1043 0.067 Uiso 1 1 calc R . . H15B H 0.5919 0.6595 0.0498 0.067 Uiso 1 1 calc R . . H15C H 0.5474 0.5797 -0.0064 0.067 Uiso 1 1 calc R . . C16 C 0.5057(3) 0.7729(4) 0.1300(4) 0.0335(15) Uani 1 1 d . . . H16A H 0.4697 0.8150 0.1357 0.050 Uiso 1 1 calc R . . H16B H 0.5443 0.8107 0.1287 0.050 Uiso 1 1 calc R . . H16C H 0.5129 0.7296 0.1838 0.050 Uiso 1 1 calc R . . O8 O 0.15788(17) 0.2981(3) -0.0714(3) 0.0271(9) Uani 1 1 d . . . C17 C 0.0819(3) 0.2744(4) -0.2095(4) 0.0431(17) Uani 1 1 d . . . H17A H 0.0678 0.2084 -0.2187 0.065 Uiso 1 1 calc R . . H17B H 0.0816 0.3045 -0.2707 0.065 Uiso 1 1 calc R . . H17C H 0.0528 0.3085 -0.1752 0.065 Uiso 1 1 calc R . . C18 C 0.1499(3) 0.2771(5) -0.1531(4) 0.0338(16) Uani 1 1 d . . . C19 C 0.2019(3) 0.2631(4) -0.2098(4) 0.0437(18) Uani 1 1 d . . . H19A H 0.2434 0.2610 -0.1680 0.065 Uiso 1 1 calc R . . H19B H 0.2016 0.3157 -0.2541 0.065 Uiso 1 1 calc R . . H19C H 0.1949 0.2033 -0.2445 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.16742(6) 0.05792(9) 0.08790(9) 0.0187(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01209(10) 0.01597(11) 0.01310(11) 0.00056(8) 0.00202(8) -0.00087(8) S1 0.0172(7) 0.0216(7) 0.0141(7) 0.0028(6) 0.0028(6) -0.0031(5) S2 0.0221(7) 0.0165(7) 0.0202(7) -0.0017(6) 0.0073(6) -0.0002(5) S3 0.0185(7) 0.0244(7) 0.0156(7) 0.0049(6) 0.0031(6) 0.0046(6) S4 0.0223(7) 0.0170(7) 0.0188(7) -0.0020(6) -0.0028(6) -0.0021(6) N1 0.018(2) 0.055(3) 0.016(3) -0.005(2) 0.002(2) -0.006(2) N2 0.016(2) 0.033(3) 0.018(2) -0.003(2) -0.0008(19) -0.002(2) N3 0.023(3) 0.020(2) 0.032(3) -0.002(2) 0.006(2) -0.007(2) N4 0.032(3) 0.015(2) 0.030(3) 0.001(2) 0.007(2) -0.005(2) N5 0.015(2) 0.038(3) 0.018(2) 0.007(2) 0.0049(19) 0.006(2) N6 0.015(2) 0.031(3) 0.016(2) 0.007(2) 0.0056(19) 0.0055(19) N7 0.014(2) 0.023(3) 0.026(3) 0.003(2) -0.002(2) -0.0008(19) N8 0.018(2) 0.012(2) 0.027(3) 0.0035(19) 0.001(2) 0.0034(18) C1 0.021(3) 0.022(3) 0.014(3) 0.003(2) 0.003(2) 0.007(2) C2 0.017(3) 0.024(3) 0.017(3) -0.002(2) -0.002(2) -0.003(2) C3 0.017(3) 0.016(3) 0.018(3) 0.001(2) -0.002(2) -0.002(2) C4 0.015(3) 0.028(3) 0.011(3) -0.001(2) 0.007(2) 0.000(2) Pt2 0.01167(14) 0.01358(15) 0.01048(14) 0.00027(11) 0.00206(11) -0.00012(11) S5 0.0145(6) 0.0136(7) 0.0230(7) 0.0021(6) 0.0031(6) 0.0000(5) S6 0.0132(6) 0.0264(7) 0.0120(6) 0.0012(6) 0.0036(5) 0.0002(5) N9 0.021(2) 0.010(2) 0.025(3) -0.0001(19) -0.001(2) -0.0041(18) N10 0.018(2) 0.016(2) 0.030(3) -0.003(2) -0.003(2) -0.0070(19) N11 0.016(2) 0.031(3) 0.013(2) -0.001(2) 0.0057(19) -0.0032(19) N12 0.019(2) 0.030(3) 0.009(2) -0.0018(19) 0.0028(19) -0.0051(19) C5 0.023(3) 0.019(3) 0.011(3) -0.002(2) 0.004(2) 0.003(2) C6 0.020(3) 0.013(3) 0.015(3) 0.001(2) 0.002(2) 0.001(2) O1 0.0140(18) 0.027(2) 0.020(2) -0.0006(17) 0.0004(16) -0.0035(15) O2 0.022(2) 0.030(2) 0.015(2) 0.0037(17) 0.0012(16) -0.0038(16) O3 0.0095(18) 0.024(2) 0.026(2) 0.0053(17) -0.0022(16) -0.0039(15) O4 0.018(2) 0.048(3) 0.017(2) 0.0076(18) 0.0032(17) -0.0024(18) C7 0.016(3) 0.012(3) 0.020(3) -0.001(2) 0.004(2) 0.005(2) C8 0.019(3) 0.010(3) 0.022(3) 0.001(2) 0.004(2) 0.002(2) C9 0.018(3) 0.011(3) 0.021(3) 0.001(2) 0.006(2) 0.002(2) C10 0.016(3) 0.016(3) 0.020(3) -0.002(2) 0.004(2) -0.001(2) S7 0.0332(9) 0.0420(9) 0.0326(9) -0.0019(8) 0.0084(7) 0.0002(7) O5 0.030(2) 0.053(3) 0.036(3) 0.009(2) 0.007(2) 0.017(2) C11 0.026(3) 0.042(4) 0.021(3) 0.003(3) -0.004(3) -0.001(3) C12 0.062(5) 0.084(6) 0.044(5) -0.027(4) 0.019(4) -0.036(4) S8 0.0545(11) 0.0283(9) 0.0265(9) -0.0002(7) -0.0021(8) -0.0042(8) O6 0.028(2) 0.025(2) 0.018(2) -0.0031(16) -0.0004(17) 0.0053(17) C13 0.060(5) 0.062(5) 0.041(5) 0.020(4) -0.024(4) -0.002(4) C14 0.057(5) 0.063(5) 0.031(4) -0.006(3) 0.021(4) -0.002(4) S9 0.0372(10) 0.0507(11) 0.0459(11) 0.0083(9) 0.0006(9) -0.0056(8) O7 0.022(2) 0.029(2) 0.038(3) -0.0032(19) 0.0009(19) -0.0025(17) C15 0.025(4) 0.056(4) 0.057(5) 0.000(4) 0.019(3) 0.004(3) C16 0.028(3) 0.029(3) 0.040(4) -0.008(3) -0.005(3) -0.007(3) O8 0.022(2) 0.030(2) 0.030(2) -0.0037(18) 0.0031(19) 0.0032(17) C17 0.049(4) 0.038(4) 0.040(4) 0.008(3) 0.001(3) -0.006(3) C18 0.022(3) 0.066(5) 0.014(3) -0.022(3) 0.006(3) -0.010(3) C19 0.063(5) 0.030(4) 0.045(4) 0.007(3) 0.027(4) 0.004(3) Cl1 0.0153(6) 0.0226(7) 0.0182(7) 0.0008(6) 0.0027(5) -0.0024(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 S2 2.3097(13) . ? Pt1 S1 2.3130(12) . ? Pt1 S4 2.3231(13) . ? Pt1 S3 2.3266(13) . ? S1 C1 1.735(5) . ? S2 C2 1.737(5) . ? S3 C3 1.727(5) . ? S4 C4 1.735(5) . ? N1 C1 1.317(6) . ? N2 C1 1.325(6) . ? N3 C2 1.310(6) . ? N4 C2 1.312(6) . ? N5 C3 1.309(6) . ? N6 C3 1.325(6) . ? N7 C4 1.317(6) . ? N8 C4 1.312(6) . ? Pt2 S5 2.3269(12) 3 ? Pt2 S5 2.3269(12) . ? Pt2 S6 2.3316(12) . ? Pt2 S6 2.3316(12) 3 ? S5 C5 1.711(5) . ? S6 C6 1.725(5) . ? N9 C5 1.328(6) . ? N10 C5 1.340(6) . ? N11 C6 1.327(6) . ? N12 C6 1.314(6) . ? O1 C7 1.255(6) . ? O2 C8 1.249(6) . ? O3 C9 1.261(6) . ? O4 C10 1.256(6) . ? C7 C10 1.455(6) . ? C7 C8 1.470(7) . ? C8 C9 1.464(7) . ? C9 C10 1.457(7) . ? S7 O5 1.496(4) . ? S7 C11 1.770(5) . ? S7 C12 1.782(6) . ? S8 O6 1.512(4) . ? S8 C13 1.772(6) . ? S8 C14 1.787(6) . ? S9 O7 1.485(4) . ? S9 C15 1.755(6) . ? S9 C16 1.779(6) . ? O8 C18 1.202(6) . ? C17 C18 1.532(8) . ? C18 C19 1.493(7) . ? 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 S2 Pt1 S1 87.92(5) . . ? S2 Pt1 S4 171.43(5) . . ? S1 Pt1 S4 91.44(5) . . ? S2 Pt1 S3 89.94(5) . . ? S1 Pt1 S3 165.83(4) . . ? S4 Pt1 S3 88.59(5) . . ? C1 S1 Pt1 110.22(17) . . ? C2 S2 Pt1 108.85(18) . . ? C3 S3 Pt1 109.85(18) . . ? C4 S4 Pt1 109.27(18) . . ? N1 C1 N2 119.6(5) . . ? N1 C1 S1 117.7(4) . . ? N2 C1 S1 122.5(4) . . ? N3 C2 N4 120.9(5) . . ? N3 C2 S2 122.2(4) . . ? N4 C2 S2 116.8(4) . . ? N5 C3 N6 119.4(5) . . ? N5 C3 S3 122.7(4) . . ? N6 C3 S3 117.9(4) . . ? N8 C4 N7 119.8(5) . . ? N8 C4 S4 122.0(4) . . ? N7 C4 S4 118.1(4) . . ? S5 Pt2 S5 180.00(5) 3 . ? S5 Pt2 S6 86.28(4) 3 . ? S5 Pt2 S6 93.72(4) . . ? S5 Pt2 S6 93.72(4) 3 3 ? S5 Pt2 S6 86.28(4) . 3 ? S6 Pt2 S6 180.00(8) . 3 ? C5 S5 Pt2 108.13(18) . . ? C6 S6 Pt2 108.22(17) . . ? N9 C5 N10 118.6(5) . . ? N9 C5 S5 124.1(4) . . ? N10 C5 S5 117.3(4) . . ? N12 C6 N11 119.5(5) . . ? N12 C6 S6 123.2(4) . . ? N11 C6 S6 117.3(4) . . ? O1 C7 C10 133.4(5) . . ? O1 C7 C8 136.5(5) . . ? C10 C7 C8 90.1(4) . . ? O2 C8 C9 135.5(5) . . ? O2 C8 C7 135.2(5) . . ? C9 C8 C7 89.3(4) . . ? O3 C9 C10 134.3(5) . . ? O3 C9 C8 135.2(5) . . ? C10 C9 C8 90.3(4) . . ? O4 C10 C7 134.7(5) . . ? O4 C10 C9 135.1(5) . . ? C7 C10 C9 90.2(4) . . ? O5 S7 C11 105.4(3) . . ? O5 S7 C12 106.2(3) . . ? C11 S7 C12 96.0(3) . . ? O6 S8 C13 105.7(3) . . ? O6 S8 C14 105.9(3) . . ? C13 S8 C14 98.4(3) . . ? O7 S9 C15 105.7(3) . . ? O7 S9 C16 106.1(3) . . ? C15 S9 C16 98.5(3) . . ? O8 C18 C19 125.2(6) . . ? O8 C18 C17 119.7(5) . . ? C19 C18 C17 114.7(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B Cl1 0.88 2.36 3.214(4) 163.2 . N3 H3B Cl1 0.88 2.54 3.382(4) 159.8 . N5 H5B Cl1 0.88 2.49 3.262(5) 146.8 . N8 H8A O8 0.88 2.16 2.853(6) 134.9 . N8 H8B Cl1 0.88 2.42 3.267(4) 160.6 . N12 H12B Cl1 0.88 2.60 3.384(4) 149.4 . N7 H7A O3 0.88 2.03 2.875(5) 161.6 . N12 H12B S5 0.88 2.83 3.412(4) 125.0 . N2 H2A S6 0.88 3.00 3.554(4) 123.2 3 N9 H9A O8 0.88 2.53 3.016(5) 115.8 3 N9 H9A O1 0.88 2.55 3.258(5) 137.9 3 N9 H9B Cl1 0.88 2.70 3.511(4) 154.6 3 N10 H10A O1 0.88 1.97 2.822(5) 161.9 3 N4 H4A O3 0.88 2.32 2.959(5) 129.8 1_545 N4 H4B O7 0.88 2.09 2.962(6) 169.8 1_545 N1 H1A O2 0.88 2.16 2.936(6) 146.8 4_565 N2 H2A O2 0.88 2.46 3.161(6) 137.3 4_565 N3 H3A O6 0.88 1.98 2.829(5) 162.6 2_645 N4 H4A O6 0.88 2.63 3.316(6) 135.5 2_645 N10 H10B O6 0.88 2.17 3.009(6) 158.1 2_645 N1 H1B O5 0.88 2.10 2.936(6) 159.6 3_655 N11 H11B O2 0.88 2.08 2.957(5) 172.3 2_545 N5 H5A O4 0.88 1.95 2.743(5) 149.4 4_566 N6 H6A O3 0.88 2.09 2.934(5) 159.5 4_566 N6 H6B O7 0.88 2.08 2.863(6) 147.2 4_566 N7 H7B O5 0.88 2.18 2.830(6) 130.7 2_655 N11 H11A O1 0.88 2.17 2.997(6) 156.0 4_566 N12 H12A O4 0.88 1.94 2.768(6) 156.9 4_566 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.605 _refine_diff_density_min -1.324 _refine_diff_density_rms 0.186 #===END data_2005sot0334 _database_code_depnum_ccdc_archive 'CCDC 289744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 N10 O4 Pt S4' _chemical_formula_weight 693.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8659(9) _cell_length_b 12.7545(8) _cell_length_c 11.0019(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.910(7) _cell_angle_gamma 90.00 _cell_volume 1162.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2630 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Shard _exptl_crystal_colour 'Translucent Pale Yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 6.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 0.677 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 7487 reflections reduced R(int) from 0.0833 to 0.0508 Ratio of minimum to maximum apparent transmission: 0.737092 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11365 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2652 _reflns_number_gt 1924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0316P)^2^+0.3360P] 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 SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2652 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 C3 C 0.4571(6) 0.4916(3) 0.5758(5) 0.0136(9) Uani 1 1 d . . . C4 C 0.5161(5) 0.5796(4) 0.5184(4) 0.0159(11) Uani 1 1 d . . . N5 N 0.1554(6) 0.8165(4) 0.7413(5) 0.0322(11) Uani 1 1 d . . . C6 C 0.1250(6) 0.8609(4) 0.8178(5) 0.0264(12) Uani 1 1 d . . . C5 C 0.0804(7) 0.9208(5) 0.9150(6) 0.0355(14) Uani 1 1 d . . . H5A H 0.1174 0.9934 0.9173 0.053 Uiso 1 1 calc R . . H5B H 0.1314 0.8888 1.0010 0.053 Uiso 1 1 calc R . . H5C H -0.0372 0.9198 0.8911 0.053 Uiso 1 1 calc R . . Pt1 Pt 0.0000 0.0000 0.5000 0.01305(11) Uani 1 2 d S . . S1 S 0.19941(15) 0.01773(9) 0.40905(13) 0.0173(3) Uani 1 1 d . . . S2 S 0.12246(16) 0.11585(9) 0.66774(12) 0.0203(3) Uani 1 1 d . . . O2 O 0.5374(4) 0.6760(2) 0.5396(3) 0.0160(7) Uani 1 1 d . . . O1 O 0.4023(4) 0.4794(2) 0.6646(3) 0.0211(8) Uani 1 1 d . . . N3 N 0.1617(5) 0.2520(3) 0.4948(4) 0.0197(9) Uani 1 1 d . . . H3A H 0.2080 0.3066 0.4738 0.024 Uiso 1 1 calc R . . H3B H 0.0815 0.2199 0.4348 0.024 Uiso 1 1 calc R . . N4 N 0.3332(5) 0.2672(3) 0.7054(4) 0.0180(9) Uani 1 1 d . . . H4A H 0.3785 0.3217 0.6834 0.022 Uiso 1 1 calc R . . H4B H 0.3682 0.2454 0.7867 0.022 Uiso 1 1 calc R . . N2 N 0.4021(5) -0.1159(3) 0.3721(4) 0.0190(9) Uani 1 1 d . . . H2A H 0.4616 -0.1731 0.3871 0.023 Uiso 1 1 calc R . . H2B H 0.4051 -0.0713 0.3121 0.023 Uiso 1 1 calc R . . N1 N 0.3039(5) -0.1643(3) 0.5298(4) 0.0184(9) Uani 1 1 d . . . H1A H 0.3634 -0.2215 0.5448 0.022 Uiso 1 1 calc R . . H1B H 0.2414 -0.1518 0.5748 0.022 Uiso 1 1 calc R . . C2 C 0.2129(6) 0.2181(3) 0.6168(5) 0.0166(11) Uani 1 1 d . . . C1 C 0.3085(5) -0.0973(3) 0.4395(4) 0.0165(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 C3 0.014(2) 0.013(2) 0.015(2) -0.001(2) 0.0072(19) -0.001(2) C4 0.014(3) 0.016(3) 0.016(3) 0.0013(19) 0.004(2) -0.0002(19) N5 0.033(3) 0.037(3) 0.027(3) 0.011(2) 0.011(2) 0.003(2) C6 0.017(3) 0.031(3) 0.025(3) 0.009(3) 0.001(2) -0.006(2) C5 0.029(3) 0.047(4) 0.030(3) -0.004(3) 0.011(3) -0.010(3) Pt1 0.01209(15) 0.01078(16) 0.01798(17) 0.00100(11) 0.00745(11) 0.00024(11) S1 0.0165(6) 0.0143(6) 0.0258(7) 0.0031(5) 0.0131(5) 0.0017(5) S2 0.0245(7) 0.0188(7) 0.0201(7) -0.0013(5) 0.0111(6) -0.0076(5) O2 0.023(2) 0.0080(17) 0.0184(18) -0.0003(13) 0.0087(15) 0.0007(13) O1 0.034(2) 0.0185(19) 0.019(2) -0.0011(14) 0.0189(17) -0.0029(15) N3 0.026(2) 0.011(2) 0.022(2) -0.0012(17) 0.009(2) -0.0021(17) N4 0.021(2) 0.017(2) 0.016(2) 0.0008(17) 0.0065(19) -0.0063(18) N2 0.020(2) 0.017(2) 0.025(2) 0.0030(18) 0.0134(19) 0.0029(18) N1 0.019(2) 0.019(2) 0.019(2) 0.0073(17) 0.0094(19) 0.0089(18) C2 0.015(3) 0.014(2) 0.021(3) 0.002(2) 0.007(2) 0.001(2) C1 0.012(3) 0.017(3) 0.017(3) -0.004(2) 0.001(2) -0.001(2) _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 C3 O1 1.245(5) . ? C3 C4 1.460(6) 3_666 ? C3 C4 1.473(6) . ? C4 O2 1.253(6) . ? C4 C3 1.460(6) 3_666 ? N5 C6 1.125(6) . ? C6 C5 1.477(8) . ? Pt1 S2 2.3104(13) 3_556 ? Pt1 S2 2.3104(13) . ? Pt1 S1 2.3325(12) . ? Pt1 S1 2.3325(12) 3_556 ? S1 C1 1.723(5) . ? S2 C2 1.726(5) . ? N3 C2 1.327(6) . ? N4 C2 1.318(6) . ? N2 C1 1.317(6) . ? N1 C1 1.322(6) . ? 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 C3 C4 133.4(4) . 3_666 ? O1 C3 C4 136.8(4) . . ? C4 C3 C4 89.8(4) 3_666 . ? O2 C4 C3 133.6(4) . 3_666 ? O2 C4 C3 136.1(4) . . ? C3 C4 C3 90.2(4) 3_666 . ? N5 C6 C5 178.1(6) . . ? S2 Pt1 S2 180.0 3_556 . ? S2 Pt1 S1 86.06(4) 3_556 . ? S2 Pt1 S1 93.94(4) . . ? S2 Pt1 S1 93.94(4) 3_556 3_556 ? S2 Pt1 S1 86.06(4) . 3_556 ? S1 Pt1 S1 180.0 . 3_556 ? C1 S1 Pt1 107.03(16) . . ? C2 S2 Pt1 111.37(17) . . ? N4 C2 N3 119.2(4) . . ? N4 C2 S2 117.8(4) . . ? N3 C2 S2 122.9(4) . . ? N2 C1 N1 120.0(4) . . ? N2 C1 S1 117.8(3) . . ? N1 C1 S1 122.1(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O1 0.88 2.04 2.847(5) 151.8 . N2 H2A O2 0.88 2.48 3.209(5) 140.2 1_545 N1 H1A O2 0.88 2.04 2.878(5) 159.2 1_545 N1 H1B N5 0.88 2.26 3.066(6) 152.6 1_545 N3 H3A O2 0.88 2.32 2.970(5) 130.3 3_666 N3 H3B N5 0.88 2.34 3.194(6) 163.7 3_566 N4 H4B O2 0.88 2.00 2.870(5) 170.6 2_646 N2 H2A N4 0.88 2.67 3.375(5) 138.3 3_656 N2 H2B O1 0.88 1.99 2.872(5) 175.0 4_565 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.088 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.177 #===END data_2005sot0339 _database_code_depnum_ccdc_archive 'CCDC 289745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 N8 O6 Pt S4' _chemical_formula_weight 647.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9202(5) _cell_length_b 13.8259(6) _cell_length_c 9.1159(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.182(5) _cell_angle_gamma 90.00 _cell_volume 1008.91(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2391 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Shard _exptl_crystal_colour 'Translucent Pale Yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 7.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5034 _exptl_absorpt_correction_T_max 0.6382 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 11804 reflections reduced R(int) from 0.0623 to 0.0312 Ratio of minimum to maximum apparent transmission: 0.643156 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13651 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2308 _reflns_number_gt 2081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0000P)^2^+1.3330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2308 _refine_ls_number_parameters 133 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0357 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.004 _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 N4 N 0.8727(3) 0.24841(15) 0.5475(2) 0.0143(4) Uani 1 1 d . . . H4A H 0.8720 0.3117 0.5573 0.017 Uiso 1 1 calc R . . H4B H 0.9458 0.2133 0.6276 0.017 Uiso 1 1 calc R . . N3 N 0.6543(3) 0.26025(14) 0.2921(2) 0.0138(4) Uani 1 1 d . . . H3A H 0.6551 0.3235 0.3038 0.017 Uiso 1 1 calc R . . H3B H 0.5812 0.2331 0.2014 0.017 Uiso 1 1 calc R . . C2 C 0.7634(3) 0.20584(17) 0.4114(3) 0.0125(5) Uani 1 1 d . . . O1 O 0.4069(2) 0.15365(11) 0.0115(2) 0.0118(3) Uani 1 1 d . . . O2 O 0.7172(2) 0.05975(12) -0.0427(2) 0.0145(4) Uani 1 1 d . . . C3 C 0.4595(3) 0.06954(18) 0.0047(3) 0.0107(5) Uani 1 1 d . . . C4 C 0.5981(3) 0.02773(18) -0.0188(3) 0.0112(5) Uani 1 1 d . . . H98 H 0.1577(16) 0.137(2) -0.123(4) 0.041(10) Uiso 1 1 d D . . H99 H 0.027(3) 0.1862(19) -0.094(3) 0.040(10) Uiso 1 1 d D . . Pt1 Pt 1.0000 0.0000 0.5000 0.00838(6) Uani 1 2 d S . . S1 S 1.16122(8) 0.13009(4) 0.48924(7) 0.01291(13) Uani 1 1 d . . . S2 S 0.74785(8) 0.08174(4) 0.38229(8) 0.01482(13) Uani 1 1 d . . . N2 N 1.3104(3) 0.16868(15) 0.3030(3) 0.0150(4) Uani 1 1 d . . . H2A H 1.3349 0.1602 0.2204 0.018 Uiso 1 1 calc R . . H2B H 1.3535 0.2177 0.3702 0.018 Uiso 1 1 calc R . . N1 N 1.1432(3) 0.03384(15) 0.2260(2) 0.0146(4) Uani 1 1 d . . . H1A H 1.1678 0.0255 0.1434 0.018 Uiso 1 1 calc R . . H1B H 1.0754 -0.0068 0.2413 0.018 Uiso 1 1 calc R . . C1 C 1.2075(3) 0.10705(17) 0.3265(3) 0.0115(5) Uani 1 1 d . . . O4 O 0.0545(2) 0.14555(13) -0.1486(2) 0.0157(4) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N4 0.0174(11) 0.0090(10) 0.0152(11) -0.0034(8) 0.0059(9) 0.0007(8) N3 0.0143(11) 0.0096(10) 0.0135(10) -0.0009(8) 0.0025(9) -0.0007(8) C2 0.0111(12) 0.0132(12) 0.0151(12) -0.0010(9) 0.0076(10) -0.0009(10) O1 0.0133(9) 0.0065(8) 0.0151(9) -0.0010(6) 0.0059(7) 0.0015(7) O2 0.0163(9) 0.0112(8) 0.0214(9) -0.0008(7) 0.0133(8) -0.0025(7) C3 0.0112(11) 0.0118(13) 0.0070(11) -0.0008(9) 0.0019(9) -0.0009(10) C4 0.0144(12) 0.0094(11) 0.0086(11) -0.0010(9) 0.0039(10) -0.0005(10) Pt1 0.01267(9) 0.00563(9) 0.00875(8) 0.00000(4) 0.00647(6) 0.00015(4) S1 0.0200(3) 0.0085(3) 0.0151(3) -0.0017(2) 0.0122(3) -0.0020(2) S2 0.0143(3) 0.0080(3) 0.0174(3) -0.0009(2) 0.0026(2) 0.0008(2) N2 0.0200(11) 0.0135(10) 0.0173(11) -0.0046(8) 0.0134(9) -0.0055(9) N1 0.0213(12) 0.0126(10) 0.0159(10) -0.0044(9) 0.0136(9) -0.0061(9) C1 0.0110(11) 0.0114(11) 0.0126(11) 0.0021(9) 0.0056(10) 0.0027(9) O4 0.0145(10) 0.0134(9) 0.0186(9) -0.0020(7) 0.0068(8) 0.0015(7) _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 N4 C2 1.330(3) . ? N3 C2 1.327(3) . ? C2 S2 1.732(2) . ? O1 C3 1.266(3) . ? O2 C4 1.256(3) . ? C3 C4 1.464(3) . ? C3 C4 1.465(3) 3_655 ? C4 C3 1.465(3) 3_655 ? Pt1 S2 2.3146(6) 3_756 ? Pt1 S2 2.3146(6) . ? Pt1 S1 2.3317(6) 3_756 ? Pt1 S1 2.3317(6) . ? S1 C1 1.736(2) . ? N2 C1 1.337(3) . ? N1 C1 1.315(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 N3 C2 N4 119.0(2) . . ? N3 C2 S2 117.12(18) . . ? N4 C2 S2 123.87(19) . . ? O1 C3 C4 136.5(2) . . ? O1 C3 C4 133.4(2) . 3_655 ? C4 C3 C4 90.10(19) . 3_655 ? O2 C4 C3 136.1(2) . . ? O2 C4 C3 134.0(2) . 3_655 ? C3 C4 C3 89.90(19) . 3_655 ? S2 Pt1 S2 180.0 3_756 . ? S2 Pt1 S1 95.46(2) 3_756 3_756 ? S2 Pt1 S1 84.54(2) . 3_756 ? S2 Pt1 S1 84.54(2) 3_756 . ? S2 Pt1 S1 95.46(2) . . ? S1 Pt1 S1 180.000(18) 3_756 . ? C1 S1 Pt1 106.15(8) . . ? C2 S2 Pt1 114.64(9) . . ? N1 C1 N2 119.9(2) . . ? N1 C1 S1 122.78(18) . . ? N2 C1 S1 117.30(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O1 0.88 2.06 2.933(3) 171.3 . O4 H98 O1 0.853(9) 2.023(16) 2.824(2) 156(3) . O4 H99 N4 0.855(10) 2.437(14) 3.245(3) 158(3) 4_465 O4 H99 S1 0.855(10) 2.77(3) 3.3245(18) 124(2) 4_465 N4 H4A O2 0.88 2.19 2.937(3) 142.9 4_566 N3 H3A O2 0.88 2.05 2.834(3) 148.4 4_566 N4 H4B O4 0.88 2.06 2.892(3) 157.9 1_656 N2 H2A O1 0.88 2.26 3.141(2) 174.4 1_655 N2 H2B O1 0.88 2.12 2.991(3) 168.3 4_666 N1 H1A O2 0.88 2.03 2.802(3) 146.2 3_755 N1 H1B O4 0.88 2.21 2.943(3) 140.9 3_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.493 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.103 #===END data_2005sot0273 _database_code_depnum_ccdc_archive 'CCDC 289746' _database_code_CSD 5SOT0273 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H44 N8 O12 Pt S8' _chemical_formula_weight 1016.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21.409(4) _cell_length_b 14.734(3) _cell_length_c 14.767(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.24(3) _cell_angle_gamma 90.00 _cell_volume 3708.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4381 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Blade _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 4.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5650 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 24554 reflections reduced R(int) from 0.0733 to 0.0515 Ratio of minimum to maximum apparent transmission: 0.765901 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36424 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4247 _reflns_number_gt 3304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0094P)^2^+12.5824P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4247 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.23450(13) 0.92649(16) 0.34728(19) 0.0225(5) Uani 1 1 d . . . O1 O 0.16913(14) 0.65245(16) -0.06266(19) 0.0237(6) Uani 1 1 d . . . C3 C 0.1460(2) 0.6232(3) 0.0919(3) 0.0284(9) Uani 1 1 d . . . H3A H 0.0889 0.6295 0.0373 0.043 Uiso 1 1 calc R . . H3B H 0.1633 0.6428 0.1673 0.043 Uiso 1 1 calc R . . H3C H 0.1605 0.5595 0.0954 0.043 Uiso 1 1 calc R . . C4 C 0.2909(2) 0.6586(3) 0.1545(3) 0.0291(9) Uani 1 1 d . . . H4A H 0.2953 0.5924 0.1537 0.044 Uiso 1 1 calc R . . H4B H 0.3068 0.6780 0.2292 0.044 Uiso 1 1 calc R . . H4C H 0.3250 0.6871 0.1394 0.044 Uiso 1 1 calc R . . C6 C 0.2750(2) 0.9280(3) 0.2110(3) 0.0321(9) Uani 1 1 d . . . H6A H 0.2540 0.9897 0.1884 0.048 Uiso 1 1 calc R . . H6B H 0.2670 0.8965 0.1462 0.048 Uiso 1 1 calc R . . H6C H 0.3313 0.9306 0.2739 0.048 Uiso 1 1 calc R . . C5 C 0.1275(2) 0.8868(3) 0.1340(3) 0.0329(10) Uani 1 1 d . . . H5A H 0.0919 0.8529 0.1424 0.049 Uiso 1 1 calc R . . H5B H 0.1210 0.8660 0.0657 0.049 Uiso 1 1 calc R . . H5C H 0.1153 0.9517 0.1269 0.049 Uiso 1 1 calc R . . O4 O 0.46891(14) 0.71409(17) 0.4029(2) 0.0269(6) Uani 1 1 d . . . C7 C 0.48878(18) 0.6287(2) 0.2880(3) 0.0190(8) Uani 1 1 d . . . C8 C 0.48210(18) 0.7144(2) 0.3319(3) 0.0182(7) Uani 1 1 d . . . O3 O 0.47620(13) 0.55449(16) 0.3164(2) 0.0249(6) Uani 1 1 d . . . O5 O 0.48002(14) 0.87338(16) 0.3232(2) 0.0263(6) Uani 1 1 d . . . C9 C 0.49019(18) 0.8022(2) 0.2908(3) 0.0183(7) Uani 1 1 d . . . O6 O 0.44237(18) 0.8582(2) 0.5039(3) 0.0369(7) Uani 1 1 d . . . H99 H 0.456(3) 0.829(3) 0.471(4) 0.058(17) Uiso 1 1 d . . . H98 H 0.417(3) 0.822(4) 0.517(4) 0.075(19) Uiso 1 1 d . . . Pt1 Pt 0.2500 0.7500 0.5000 0.01405(5) Uani 1 2 d S . . S1 S 0.12714(5) 0.71499(6) 0.33062(7) 0.01835(18) Uani 1 1 d . . . S2 S 0.30884(5) 0.67925(6) 0.42940(7) 0.01832(19) Uani 1 1 d . . . S3 S 0.22598(5) 0.86850(6) 0.25537(7) 0.01943(19) Uani 1 1 d . . . S4 S 0.19186(5) 0.69164(6) 0.04772(7) 0.02112(19) Uani 1 1 d . . . N1 N 0.06180(16) 0.56265(19) 0.2207(2) 0.0198(6) Uani 1 1 d . . . H1A H 0.0537 0.5037 0.2135 0.024 Uiso 1 1 calc R . . H1B H 0.0339 0.5981 0.1607 0.024 Uiso 1 1 calc R . . C2 C 0.38194(19) 0.6078(2) 0.5321(3) 0.0181(7) Uani 1 1 d . . . N3 N 0.43901(16) 0.5870(2) 0.5250(2) 0.0226(7) Uani 1 1 d . . . H3D H 0.4759 0.5485 0.5736 0.027 Uiso 1 1 calc R . . H3E H 0.4401 0.6116 0.4716 0.027 Uiso 1 1 calc R . . N2 N 0.15772(16) 0.54534(19) 0.4119(2) 0.0215(7) Uani 1 1 d . . . H2A H 0.1497 0.4863 0.4048 0.026 Uiso 1 1 calc R . . H2B H 0.1937 0.5690 0.4790 0.026 Uiso 1 1 calc R . . N4 N 0.38074(16) 0.57065(19) 0.6121(2) 0.0210(7) Uani 1 1 d . . . H4D H 0.4177 0.5322 0.6605 0.025 Uiso 1 1 calc R . . H4E H 0.3429 0.5843 0.6172 0.025 Uiso 1 1 calc R . . C1 C 0.11594(19) 0.5981(2) 0.3220(3) 0.0175(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0252(13) 0.0259(14) 0.0207(13) 0.0003(11) 0.0162(11) 0.0004(11) O1 0.0294(14) 0.0264(15) 0.0183(13) -0.0008(11) 0.0161(12) 0.0003(11) C3 0.024(2) 0.042(3) 0.023(2) 0.0036(17) 0.0161(17) 0.0001(17) C4 0.024(2) 0.038(2) 0.023(2) 0.0028(17) 0.0128(17) -0.0009(17) C6 0.046(2) 0.033(2) 0.034(2) -0.0087(18) 0.033(2) -0.0106(19) C5 0.027(2) 0.032(2) 0.026(2) -0.0019(18) 0.0092(18) 0.0025(18) O4 0.0348(15) 0.0300(15) 0.0241(14) 0.0019(11) 0.0221(13) 0.0014(12) C7 0.0136(17) 0.0163(19) 0.0188(18) 0.0023(14) 0.0055(15) 0.0005(14) C8 0.0131(16) 0.0207(18) 0.0162(17) 0.0030(14) 0.0064(15) 0.0008(14) O3 0.0235(13) 0.0169(14) 0.0300(14) 0.0064(11) 0.0139(12) -0.0007(11) O5 0.0321(15) 0.0172(14) 0.0233(14) -0.0020(11) 0.0134(12) 0.0065(11) C9 0.0123(16) 0.018(2) 0.0151(17) -0.0008(14) 0.0034(14) 0.0013(14) O6 0.0388(18) 0.043(2) 0.0407(18) -0.0152(15) 0.0304(16) -0.0107(15) Pt1 0.01591(9) 0.01178(9) 0.01568(9) 0.00006(9) 0.01021(7) 0.00042(9) S1 0.0183(4) 0.0140(4) 0.0189(4) -0.0004(3) 0.0093(4) -0.0002(3) S2 0.0203(4) 0.0202(5) 0.0172(4) 0.0018(4) 0.0128(4) 0.0039(4) S3 0.0223(4) 0.0182(5) 0.0202(4) 0.0016(4) 0.0141(4) 0.0012(4) S4 0.0236(5) 0.0211(5) 0.0188(4) 0.0006(4) 0.0129(4) 0.0022(4) N1 0.0250(16) 0.0136(15) 0.0189(15) -0.0020(12) 0.0124(13) -0.0014(12) C2 0.0213(18) 0.0142(18) 0.0201(18) -0.0040(14) 0.0132(16) -0.0013(14) N3 0.0240(16) 0.0247(18) 0.0266(17) 0.0089(13) 0.0192(14) 0.0092(13) N2 0.0271(17) 0.0172(16) 0.0206(16) -0.0018(13) 0.0147(14) -0.0038(13) N4 0.0246(16) 0.0184(16) 0.0255(17) 0.0055(13) 0.0180(14) 0.0074(13) C1 0.0216(18) 0.0187(19) 0.0226(19) 0.0015(15) 0.0188(16) 0.0033(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 O2 S3 1.518(2) . ? O1 S4 1.506(2) . ? C3 S4 1.785(3) . ? C4 S4 1.781(4) . ? C6 S3 1.770(3) . ? C5 S3 1.777(4) . ? O4 C8 1.240(4) . ? C7 O3 1.257(4) . ? C7 C8 1.465(5) . ? C7 C7 1.465(7) 2_655 ? C8 C9 1.483(5) . ? O5 C9 1.226(4) . ? C9 C9 1.496(7) 2_655 ? Pt1 S2 2.3130(9) . ? Pt1 S2 2.3130(9) 7_566 ? Pt1 S1 2.3405(15) . ? Pt1 S1 2.3405(15) 7_566 ? S1 C1 1.733(4) . ? S2 C2 1.727(3) . ? N1 C1 1.324(4) . ? C2 N4 1.317(4) . ? C2 N3 1.324(4) . ? N2 C1 1.315(4) . ? 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 C7 C8 120.3(3) . . ? O3 C7 C7 119.46(19) . 2_655 ? C8 C7 C7 120.26(19) . 2_655 ? O4 C8 C7 120.2(3) . . ? O4 C8 C9 119.5(3) . . ? C7 C8 C9 120.3(3) . . ? O5 C9 C8 119.6(3) . . ? O5 C9 C9 121.1(2) . 2_655 ? C8 C9 C9 119.26(18) . 2_655 ? S2 Pt1 S2 180.00(3) . 7_566 ? S2 Pt1 S1 89.16(3) . . ? S2 Pt1 S1 90.84(3) 7_566 . ? S2 Pt1 S1 90.84(3) . 7_566 ? S2 Pt1 S1 89.16(3) 7_566 7_566 ? S1 Pt1 S1 180.0 . 7_566 ? C1 S1 Pt1 108.29(12) . . ? C2 S2 Pt1 109.29(11) . . ? O2 S3 C6 105.96(16) . . ? O2 S3 C5 104.11(16) . . ? C6 S3 C5 99.15(19) . . ? O1 S4 C4 106.58(16) . . ? O1 S4 C3 106.88(16) . . ? C4 S4 C3 98.34(17) . . ? N4 C2 N3 119.7(3) . . ? N4 C2 S2 122.8(3) . . ? N3 C2 S2 117.5(3) . . ? N2 C1 N1 120.1(3) . . ? N2 C1 S1 122.3(3) . . ? N1 C1 S1 117.6(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H99 O4 0.81(5) 2.08(5) 2.843(4) 156(5) . N3 H3E O4 0.88 2.11 2.926(4) 154.1 . O6 H99 O5 0.81(5) 2.62(5) 3.229(4) 133(4) . O6 H98 S2 0.86(5) 2.80(5) 3.540(3) 145(4) . N2 H2A O1 0.88 2.08 2.930(4) 160.9 6_566 N4 H4D O3 0.88 2.24 3.036(4) 150.6 6_566 N3 H3D O3 0.88 1.99 2.825(4) 157.0 5_666 N4 H4D O3 0.88 2.44 3.160(4) 138.9 5_666 N2 H2B O2 0.88 2.04 2.866(4) 155.3 7_566 N4 H4E O2 0.88 2.03 2.870(3) 160.6 7_566 O6 H98 S1 0.86(5) 2.97(5) 3.708(4) 145(4) 7_566 N1 H1A O5 0.88 2.01 2.880(4) 171.8 4_545 N1 H1B O6 0.88 2.03 2.870(4) 159.2 8_465 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.088 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.127 #===END