Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Roberto Quesada' _publ_contact_author_email RQUESADA@UBU.ES _publ_section_title ; Hydrogen bonded networks in N-alkyl substituted thiourea platinum (II) oxocarbodianion and carboxylate salts ; loop_ _publ_author_name 'Roberto Quesada' 'Matthew G. Fisher' 'Philip Gale' 'Mark Light' # Attachment 'Gale-Quesada_combined_rev.cif' data_2005sot0811 _database_code_depnum_ccdc_archive 'CCDC 679247' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 5SOT0811 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H32 N8 S4 Pt, cl, 0.5(C4 O4), 0.125(C4 O4 H2), 0.5(H2 O)' _chemical_formula_sum 'C14.50 H33.25 Cl N8 O3 Pt S4' _chemical_formula_weight 726.52 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' Cl Cl 0.1484 0.1585 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 10.0310(2) _cell_length_b 10.0310(2) _cell_length_c 29.9790(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3016.52(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1735 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1437 _exptl_absorpt_coefficient_mu 5.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5282 _exptl_absorpt_correction_T_max 0.7517 _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 8845 reflections reduced R(int) from 0.0589 to 0.0323 Ratio of minimum to maximum apparent transmission: 0.738509 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _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 9764 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1759 _reflns_number_gt 1660 _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 squarates and water form disordered sheets and have partial occupancies The hydrogen's on the protonated squarate and the water have not been included in the refinement. Distance restraints were used to retain a plausible geometry for the squarate located on the 4/m site. It was also necessary to apply constraints to the thermal parameters (Shelx EADP, ISOR) ; _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^)+(0.0255P)^2^+6.9221P] 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 1759 _refine_ls_number_parameters 91 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.069 _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 C6 C 0.0982(7) 0.0049(18) 0.0000 0.077(4) Uani 0.25 2 d SPDU . . O3 O 0.2232(11) 0.002(2) 0.0000 0.077(4) Uani 0.25 2 d SPDU . . O4 O 0.361(2) 0.017(2) 0.0000 0.077(4) Uani 0.25 2 d SPU . . Pt1 Pt 0.5000 0.5000 0.182852(7) 0.01676(9) Uani 1 4 d S . . S1 S 0.45857(8) 0.27447(8) 0.18955(3) 0.02504(18) Uani 1 1 d . . . N1 N 0.3273(3) 0.2943(3) 0.11245(8) 0.0282(6) Uani 1 1 d . . . H1 H 0.3831 0.3601 0.1070 0.034 Uiso 1 1 calc R . . N2 N 0.2649(3) 0.1235(3) 0.15857(8) 0.0260(6) Uani 1 1 d . . . H2 H 0.2093 0.0974 0.1376 0.031 Uiso 1 1 calc R . . C1 C 0.3412(3) 0.2291(3) 0.15037(9) 0.0214(6) Uani 1 1 d . . . C2 C 0.2272(5) 0.2654(5) 0.07918(14) 0.0608(13) Uani 1 1 d U . . H2A H 0.2399 0.1746 0.0680 0.091 Uiso 1 1 calc R . . H2B H 0.2354 0.3288 0.0545 0.091 Uiso 1 1 calc R . . H2C H 0.1384 0.2733 0.0925 0.091 Uiso 1 1 calc R . . C3 C 0.2676(3) 0.0484(3) 0.20011(11) 0.0299(7) Uani 1 1 d . . . H3A H 0.3514 -0.0015 0.2021 0.045 Uiso 1 1 calc R . . H3B H 0.1924 -0.0139 0.2008 0.045 Uiso 1 1 calc R . . H3C H 0.2608 0.1100 0.2254 0.045 Uiso 1 1 calc R . . O1 O 0.4909(6) 0.2714(6) 0.0000 0.0269(13) Uani 0.50 2 d SP . . O2 O 0.5000 0.5000 0.07644(12) 0.0228(9) Uani 1 4 d S . . C4 C 0.4955(8) 0.3950(8) 0.0000 0.0193(17) Uani 0.50 2 d SP . . C5 C 0.5000 0.5000 0.0336(2) 0.0198(12) Uani 1 4 d S . . Cl1 Cl 0.0000 0.0000 0.11597(5) 0.0249(3) Uani 1 4 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 C6 0.089(6) 0.079(5) 0.065(5) 0.000 0.000 0.000(5) O3 0.089(6) 0.079(5) 0.065(5) 0.000 0.000 0.000(5) O4 0.089(6) 0.079(5) 0.065(5) 0.000 0.000 0.000(5) Pt1 0.01920(10) 0.01920(10) 0.01188(13) 0.000 0.000 0.000 S1 0.0268(4) 0.0206(4) 0.0277(4) 0.0066(3) -0.0107(3) -0.0028(3) N1 0.0295(14) 0.0372(15) 0.0179(13) 0.0069(12) -0.0046(11) -0.0136(11) N2 0.0279(13) 0.0295(14) 0.0207(13) 0.0032(11) -0.0037(11) -0.0090(11) C1 0.0214(14) 0.0246(15) 0.0182(15) -0.0014(12) 0.0003(12) 0.0006(11) C2 0.067(3) 0.083(3) 0.032(2) 0.024(2) -0.0250(19) -0.046(2) C3 0.0319(17) 0.0282(17) 0.0296(18) 0.0094(15) -0.0038(15) -0.0066(13) O1 0.039(4) 0.023(3) 0.019(3) 0.000 0.000 0.003(3) O2 0.0304(14) 0.0304(14) 0.0078(19) 0.000 0.000 0.000 C4 0.016(4) 0.031(5) 0.012(4) 0.000 0.000 0.001(3) C5 0.0200(17) 0.0200(17) 0.019(3) 0.000 0.000 0.000 Cl1 0.0204(4) 0.0204(4) 0.0341(8) 0.000 0.000 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 C6 O3 1.255(9) . ? C6 C6 1.394(10) 10 ? C6 C6 1.394(10) 2 ? Pt1 S1 2.3089(7) . ? Pt1 S1 2.3089(7) 3_665 ? Pt1 S1 2.3089(8) 2_655 ? Pt1 S1 2.3089(8) 4_565 ? S1 C1 1.724(3) . ? N1 C1 1.319(4) . ? N1 C2 1.445(4) . ? N2 C1 1.330(4) . ? N2 C3 1.455(4) . ? O1 C4 1.241(10) . ? O2 C5 1.284(7) . ? C4 C5 1.459(7) . ? C4 C5 1.459(7) 9_665 ? C4 C4 1.492(11) 2_655 ? C4 C4 1.491(11) 10_565 ? C5 C4 1.459(7) 10_565 ? C5 C4 1.459(7) 9_665 ? C5 C4 1.459(7) 2_655 ? 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 C6 C6 130.7(18) . 10 ? O3 C6 C6 139.3(18) . 2 ? C6 C6 C6 90.000(2) 10 2 ? O3 C6 C6 175.7(18) . 9 ? C6 C6 C6 45.0 10 9 ? C6 C6 C6 45.000(1) 2 9 ? S1 Pt1 S1 170.02(4) . 3_665 ? S1 Pt1 S1 89.567(4) . 2_655 ? S1 Pt1 S1 89.567(4) 3_665 2_655 ? S1 Pt1 S1 89.567(4) . 4_565 ? S1 Pt1 S1 89.567(4) 3_665 4_565 ? S1 Pt1 S1 170.02(4) 2_655 4_565 ? C1 S1 Pt1 108.81(10) . . ? C1 N1 C2 124.6(3) . . ? C1 N2 C3 124.0(3) . . ? N1 C1 N2 119.6(3) . . ? N1 C1 S1 121.9(2) . . ? N2 C1 S1 118.5(2) . . ? O1 C4 C5 136.3(3) . . ? O1 C4 C5 136.3(3) . 9_665 ? C5 C4 C5 87.4(6) . 9_665 ? O1 C4 C4 134.7(8) . 2_655 ? C5 C4 C4 59.26(16) . 2_655 ? C5 C4 C4 59.26(16) 9_665 2_655 ? O1 C4 C4 135.3(8) . 10_565 ? C5 C4 C4 59.26(16) . 10_565 ? C5 C4 C4 59.26(16) 9_665 10_565 ? C4 C4 C4 90.0 2_655 10_565 ? O2 C5 C4 133.7(3) . 10_565 ? O2 C5 C4 133.7(3) . . ? C4 C5 C4 61.5(3) 10_565 . ? O2 C5 C4 133.7(3) . 9_665 ? C4 C5 C4 61.5(3) 10_565 9_665 ? C4 C5 C4 92.6(6) . 9_665 ? O2 C5 C4 133.7(3) . 2_655 ? C4 C5 C4 92.6(6) 10_565 2_655 ? C4 C5 C4 61.5(3) . 2_655 ? C4 C5 C4 61.5(3) 9_665 2_655 ? O2 C5 C5 180.0 . 9_665 ? C4 C5 C5 46.3(3) 10_565 9_665 ? C4 C5 C5 46.3(3) . 9_665 ? C4 C5 C5 46.3(3) 9_665 9_665 ? C4 C5 C5 46.3(3) 2_655 9_665 ? 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 H1 O2 0.88 2.05 2.902(3) 164.0 . N2 H2 Cl1 0.88 2.40 3.197(3) 150.0 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.207 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.114 #===END data_2005sot1156 _database_code_depnum_ccdc_archive 'CCDC 679248' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 5SOT1156 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 N8 O6 Pt S4' _chemical_formula_weight 779.85 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.674(5) _cell_length_b 9.390(5) _cell_length_c 9.551(5) _cell_angle_alpha 90.064(5) _cell_angle_beta 112.979(5) _cell_angle_gamma 104.680(5) _cell_volume 688.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5432 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 5.448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4187 _exptl_absorpt_correction_T_max 0.9475 _exptl_absorpt_process_details ; TWINABS V1.0 (Sheldrick, G.M., 2005) ; _exptl_special_details ? _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 5430 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5432 _reflns_number_gt 5124 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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 structure was a non-merohedral twin, 180 degree rotation about 0 1 0 reciprocal lattice vector. The refinement was acheived using an unmerged hklf5 style input file. ; _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^)+(0.0847P)^2^+10.2338P] 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 5432 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.2574(12) 0.1414(10) 0.3615(10) 0.0149(17) Uani 1 1 d . . . C2 C 0.0851(14) 0.2071(13) 0.4927(11) 0.029(2) Uani 1 1 d . . . H2A H 0.1105 0.1458 0.5775 0.043 Uiso 1 1 calc R . . H2B H -0.0347 0.2137 0.4595 0.043 Uiso 1 1 calc R . . H2C H 0.1660 0.3066 0.5268 0.043 Uiso 1 1 calc R . . C3 C 0.5743(12) 0.1952(11) 0.4983(10) 0.023(2) Uani 1 1 d . . . H3A H 0.5708 0.1067 0.4415 0.034 Uiso 1 1 calc R . . H3B H 0.6542 0.2015 0.6057 0.034 Uiso 1 1 calc R . . H3C H 0.6147 0.2836 0.4539 0.034 Uiso 1 1 calc R . . C4 C 0.1419(12) 0.3593(11) -0.0143(10) 0.0171(19) Uani 1 1 d . . . C5 C 0.3069(14) 0.4754(12) -0.1623(10) 0.023(2) Uani 1 1 d . . . H5A H 0.3278 0.3802 -0.1783 0.034 Uiso 1 1 calc R . . H5B H 0.4148 0.5550 -0.1364 0.034 Uiso 1 1 calc R . . H5C H 0.2165 0.4928 -0.2562 0.034 Uiso 1 1 calc R . . C6 C 0.1810(13) 0.4915(11) 0.2261(10) 0.023(2) Uani 1 1 d . . . H6A H 0.3056 0.4988 0.2754 0.035 Uiso 1 1 calc R . . H6B H 0.1294 0.4717 0.3013 0.035 Uiso 1 1 calc R . . H6C H 0.1653 0.5850 0.1853 0.035 Uiso 1 1 calc R . . C7 C 0.3850(11) 0.0082(12) -0.1598(10) 0.0173(18) Uani 1 1 d . . . C8 C 0.5373(12) 0.1316(10) -0.0805(9) 0.0146(18) Uani 1 1 d . . . C9 C 0.6593(11) 0.1221(10) 0.0788(9) 0.0127(17) Uani 1 1 d . . . N1 N 0.1053(9) 0.1409(9) 0.3666(8) 0.0150(15) Uani 1 1 d . . . H1 H 0.0097 0.0966 0.2865 0.018 Uiso 1 1 calc R . . N2 N 0.4013(10) 0.1862(9) 0.4892(8) 0.0191(17) Uani 1 1 d . . . H2 H 0.3910 0.2119 0.5730 0.023 Uiso 1 1 calc R . . N3 N 0.2490(10) 0.4729(9) -0.0363(8) 0.0173(16) Uani 1 1 d . . . H3 H 0.2896 0.5536 0.0285 0.021 Uiso 1 1 calc R . . N4 N 0.0957(11) 0.3713(9) 0.1015(9) 0.0185(16) Uani 1 1 d . . . H4 H 0.0071 0.3015 0.1031 0.022 Uiso 1 1 calc R . . O1 O 0.2884(9) 0.0090(9) -0.2922(7) 0.0266(15) Uani 1 1 d . . . O2 O 0.5670(9) 0.2426(7) -0.1455(7) 0.0223(15) Uani 1 1 d . . . O3 O 0.7956(9) 0.2225(8) 0.1436(7) 0.0233(15) Uani 1 1 d . . . S1 S 0.2762(3) 0.0942(3) 0.1954(2) 0.0173(5) Uani 1 1 d . . . S2 S 0.0545(3) 0.1974(2) -0.1372(2) 0.0194(5) Uani 1 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.01366(15) 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 C1 0.020(5) 0.003(4) 0.018(4) -0.002(3) 0.006(4) -0.001(4) C2 0.028(6) 0.033(6) 0.022(5) -0.001(4) 0.006(4) 0.009(5) C3 0.017(5) 0.024(5) 0.019(5) -0.002(4) 0.002(4) 0.000(4) C4 0.017(5) 0.017(5) 0.014(4) 0.005(4) 0.001(4) 0.008(4) C5 0.034(6) 0.020(5) 0.019(4) 0.003(4) 0.015(4) 0.008(5) C6 0.019(5) 0.015(5) 0.023(4) -0.002(4) 0.002(4) -0.006(4) C7 0.011(4) 0.016(5) 0.028(5) 0.005(4) 0.007(4) 0.010(4) C8 0.019(5) 0.015(5) 0.016(4) 0.008(3) 0.012(4) 0.008(4) C9 0.013(4) 0.011(4) 0.011(4) -0.001(3) 0.002(3) 0.003(4) N1 0.010(4) 0.017(4) 0.012(3) 0.002(3) 0.000(3) 0.001(3) N2 0.016(4) 0.024(5) 0.012(3) -0.001(3) 0.001(3) 0.004(4) N3 0.019(4) 0.014(4) 0.015(3) -0.003(3) 0.006(3) 0.000(3) N4 0.020(4) 0.010(4) 0.021(4) 0.003(3) 0.008(3) -0.003(3) O1 0.027(4) 0.023(4) 0.020(3) 0.008(3) 0.005(3) -0.003(4) O2 0.029(4) 0.017(4) 0.019(3) 0.005(3) 0.008(3) 0.004(3) O3 0.023(4) 0.019(4) 0.026(3) -0.001(3) 0.010(3) 0.002(3) S1 0.0176(11) 0.0170(12) 0.0107(9) -0.0032(8) -0.0002(9) 0.0035(10) S2 0.0284(13) 0.0111(11) 0.0121(9) -0.0003(8) 0.0045(9) 0.0004(10) Pt1 0.0182(3) 0.0082(2) 0.0097(2) -0.0004(2) 0.00197(17) 0.0013(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 C1 N2 1.329(11) . ? C1 N1 1.338(11) . ? C1 S1 1.726(9) . ? C2 N1 1.445(11) . ? C3 N2 1.448(11) . ? C4 N3 1.303(12) . ? C4 N4 1.329(10) . ? C4 S2 1.727(10) . ? C5 N3 1.472(11) . ? C6 N4 1.457(12) . ? C7 O1 1.215(10) . ? C7 C8 1.450(14) . ? C7 C9 1.497(13) 2_655 ? C8 O2 1.236(10) . ? C8 C9 1.495(11) . ? C9 O3 1.238(11) . ? C9 C7 1.497(13) 2_655 ? S1 Pt1 2.332(2) . ? S2 Pt1 2.328(2) . ? Pt1 S2 2.328(2) 2 ? Pt1 S1 2.332(2) 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 N2 C1 N1 118.3(8) . . ? N2 C1 S1 118.6(7) . . ? N1 C1 S1 123.0(7) . . ? N3 C4 N4 119.0(9) . . ? N3 C4 S2 120.8(7) . . ? N4 C4 S2 120.2(8) . . ? O1 C7 C8 121.1(9) . . ? O1 C7 C9 118.3(10) . 2_655 ? C8 C7 C9 120.5(7) . 2_655 ? O2 C8 C7 120.0(8) . . ? O2 C8 C9 120.5(9) . . ? C7 C8 C9 119.5(7) . . ? O3 C9 C8 119.9(8) . . ? O3 C9 C7 120.3(8) . 2_655 ? C8 C9 C7 119.8(8) . 2_655 ? C1 N1 C2 125.3(8) . . ? C1 N2 C3 123.8(7) . . ? C4 N3 C5 124.4(8) . . ? C4 N4 C6 124.8(9) . . ? C1 S1 Pt1 109.8(3) . . ? C4 S2 Pt1 108.4(3) . . ? S2 Pt1 S2 180.00(18) . 2 ? S2 Pt1 S1 90.29(9) . . ? S2 Pt1 S1 89.71(9) 2 . ? S2 Pt1 S1 89.71(9) . 2 ? S2 Pt1 S1 90.29(9) 2 2 ? S1 Pt1 S1 180.0 . 2 ? _diffrn_measured_fraction_theta_max 0.819 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.819 _refine_diff_density_max 2.856 _refine_diff_density_min -3.051 _refine_diff_density_rms 0.346 #===END data_2005sot1248 _database_code_depnum_ccdc_archive 'CCDC 679249' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 5SOT1248 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 N8 O6 Pt S4' _chemical_formula_weight 723.74 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 Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 10.5428(3) _cell_length_b 14.2305(3) _cell_length_c 17.6424(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2646.88(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3381 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 5.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6014 _exptl_absorpt_correction_T_max 0.8485 _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 14732 reflections reduced R(int) from 0.0893 to 0.0664 Ratio of minimum to maximum apparent transmission: 0.614055 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 28561 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3036 _reflns_number_gt 2127 _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. Disordered solvent was removed using squueze, however there are still a couple of peaks in the difference map, and a small solvent accessable void. ; _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^)+(0.0446P)^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 SHELXL _refine_ls_extinction_coef 0.00135(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3036 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 O2 O 0.0338(4) 0.1362(3) 0.1057(2) 0.0508(11) Uani 1 1 d . . . O3 O 0.0562(4) 0.1777(3) -0.0451(2) 0.0451(11) Uani 1 1 d . . . O1 O -0.0353(4) -0.0383(3) 0.1483(2) 0.0495(12) Uani 1 1 d . . . C6 C 0.0187(5) 0.0749(4) 0.0574(4) 0.0371(14) Uani 1 1 d . . . C7 C 0.0324(5) 0.0963(4) -0.0239(3) 0.0369(14) Uani 1 1 d . . . C5 C -0.0171(5) -0.0202(4) 0.0809(3) 0.0373(14) Uani 1 1 d . . . C2 C 0.9883(7) 0.2827(5) 0.2415(3) 0.0456(17) Uani 1 1 d . . . H2A H 1.0604 0.2435 0.2264 0.068 Uiso 1 1 calc R . . H2B H 1.0175 0.3470 0.2507 0.068 Uiso 1 1 calc R . . H2C H 0.9247 0.2829 0.2009 0.068 Uiso 1 1 calc R . . C4 C 0.3393(6) 0.3734(5) 0.5449(4) 0.0547(18) Uani 1 1 d . . . H4A H 0.3096 0.3709 0.5975 0.082 Uiso 1 1 calc R . . H4B H 0.2905 0.3288 0.5142 0.082 Uiso 1 1 calc R . . H4C H 0.3275 0.4370 0.5249 0.082 Uiso 1 1 calc R . . Pt1 Pt 0.7500 0.2500 0.480412(14) 0.02071(13) Uani 1 2 d S . . S2 S 0.72074(12) 0.36247(10) 0.57372(8) 0.0286(3) Uani 1 1 d . . . S1 S 0.78902(13) 0.12894(9) 0.39578(8) 0.0287(3) Uani 1 1 d . . . N2 N 0.9318(4) 0.2447(3) 0.3110(3) 0.0315(10) Uani 1 1 d . . . H2 H 0.9428 0.2765 0.3533 0.038 Uiso 1 1 calc R . . N1 N 0.8578(5) 0.1101(3) 0.2545(3) 0.0372(12) Uani 1 1 d . . . H1A H 0.8967 0.1244 0.2119 0.045 Uiso 1 1 calc R . . H1B H 0.8132 0.0580 0.2578 0.045 Uiso 1 1 calc R . . C3 C 0.5643(5) 0.3988(4) 0.5717(3) 0.0319(13) Uani 1 1 d . . . C1 C 0.8666(5) 0.1674(4) 0.3142(3) 0.0283(12) Uani 1 1 d . . . N4 N 0.4740(4) 0.3485(3) 0.5420(3) 0.0311(11) Uani 1 1 d . . . H4 H 0.4953 0.2961 0.5187 0.037 Uiso 1 1 calc R . . N3 N 0.5378(5) 0.4794(4) 0.6057(4) 0.076(2) Uani 1 1 d . . . H3A H 0.4589 0.4992 0.6082 0.091 Uiso 1 1 calc R . . H3B H 0.5992 0.5132 0.6256 0.091 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 O2 0.056(3) 0.056(3) 0.040(3) -0.026(2) 0.003(2) -0.009(2) O3 0.056(3) 0.035(2) 0.045(3) -0.009(2) -0.008(2) 0.008(2) O1 0.069(3) 0.049(3) 0.031(2) -0.005(2) -0.002(2) 0.017(2) C6 0.028(3) 0.044(4) 0.040(4) -0.016(3) -0.001(3) 0.008(3) C7 0.030(3) 0.041(4) 0.040(4) -0.012(3) -0.007(3) 0.014(3) C5 0.036(3) 0.042(3) 0.034(3) -0.012(3) -0.011(3) 0.016(3) C2 0.057(5) 0.049(4) 0.032(3) -0.002(3) 0.011(3) 0.001(4) C4 0.028(3) 0.060(4) 0.076(5) -0.021(4) -0.005(3) 0.010(3) Pt1 0.01997(17) 0.02264(18) 0.01953(17) 0.000 0.000 0.00480(11) S2 0.0269(8) 0.0323(7) 0.0266(7) -0.0081(6) -0.0032(5) 0.0062(5) S1 0.0359(8) 0.0243(7) 0.0257(7) -0.0028(6) 0.0000(6) 0.0097(5) N2 0.036(3) 0.037(3) 0.021(2) -0.005(2) -0.002(2) 0.009(2) N1 0.051(4) 0.039(3) 0.022(2) -0.005(2) -0.002(2) 0.003(2) C3 0.038(3) 0.028(3) 0.030(3) -0.011(2) -0.007(3) 0.011(2) C1 0.026(3) 0.036(3) 0.023(3) -0.003(2) -0.006(2) 0.011(2) N4 0.028(3) 0.023(2) 0.042(3) -0.008(2) 0.001(2) 0.0058(19) N3 0.045(4) 0.071(4) 0.111(5) -0.063(4) -0.040(4) 0.031(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 O2 C6 1.230(6) . ? O3 C7 1.243(7) . ? O1 C5 1.231(7) . ? C6 C5 1.465(8) . ? C6 C7 1.474(8) . ? C7 C5 1.486(8) 5 ? C5 C7 1.486(8) 5 ? C2 N2 1.466(8) . ? C4 N4 1.465(7) . ? Pt1 S1 2.3165(13) . ? Pt1 S1 2.3165(13) 2_655 ? Pt1 S2 2.3166(13) . ? Pt1 S2 2.3166(13) 2_655 ? S2 C3 1.729(5) . ? S1 C1 1.743(6) . ? N2 C1 1.299(6) . ? N1 C1 1.336(6) . ? C3 N4 1.301(7) . ? C3 N3 1.324(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 O2 C6 C5 119.5(6) . . ? O2 C6 C7 121.0(5) . . ? C5 C6 C7 119.4(5) . . ? O3 C7 C6 120.3(5) . . ? O3 C7 C5 119.9(5) . 5 ? C6 C7 C5 119.8(5) . 5 ? O1 C5 C6 120.4(5) . . ? O1 C5 C7 118.9(6) . 5 ? C6 C5 C7 120.7(5) . 5 ? S1 Pt1 S1 99.74(7) . 2_655 ? S1 Pt1 S2 174.53(4) . . ? S1 Pt1 S2 85.44(5) 2_655 . ? S1 Pt1 S2 85.44(5) . 2_655 ? S1 Pt1 S2 174.53(4) 2_655 2_655 ? S2 Pt1 S2 89.44(7) . 2_655 ? C3 S2 Pt1 108.60(18) . . ? C1 S1 Pt1 112.45(18) . . ? C1 N2 C2 124.3(5) . . ? N4 C3 N3 120.3(5) . . ? N4 C3 S2 122.8(4) . . ? N3 C3 S2 116.8(4) . . ? N2 C1 N1 121.3(5) . . ? N2 C1 S1 123.4(4) . . ? N1 C1 S1 115.3(4) . . ? C3 N4 C4 124.3(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 H2 O3 0.88 2.25 3.064(6) 153.4 7_666 N2 H2 S1 0.88 2.89 3.300(4) 110.4 2_655 N1 H1A O2 0.88 2.37 3.236(6) 167.1 1_655 N4 H4 O3 0.88 2.10 2.893(6) 149.9 8_656 N3 H3A S1 0.88 2.57 3.378(5) 152.4 6_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 2.703 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.160 #===END data_2005sot1324 _database_code_depnum_ccdc_archive 'CCDC 679250' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 5SOT1324 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 N8 O4 Pt S4' _chemical_formula_weight 723.83 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6900(1) _cell_length_b 9.1780(2) _cell_length_c 9.5430(2) _cell_angle_alpha 85.112(1) _cell_angle_beta 65.951(1) _cell_angle_gamma 65.564(1) _cell_volume 629.60(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2824 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Lath _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 5.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5879 _exptl_absorpt_correction_T_max 0.9430 _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 12669 reflections reduced R(int) from 0.0917 to 0.0378 Ratio of minimum to maximum apparent transmission: 0.741374 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 12713 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2879 _reflns_number_gt 2877 _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^)+(0.0061P)^2^+0.7797P] 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 2879 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0394 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 1.0000 0.0000 0.0000 0.00885(5) Uani 1 2 d S . . S1 S 0.93478(9) -0.13748(7) 0.21709(7) 0.01231(13) Uani 1 1 d . . . S2 S 0.69804(8) 0.19508(7) 0.10928(7) 0.01130(13) Uani 1 1 d . . . N1 N 0.7411(3) -0.0194(3) 0.5104(2) 0.0145(4) Uani 1 1 d . . . H1 H 0.7019 0.0504 0.5884 0.017 Uiso 1 1 calc R . . N2 N 0.9158(3) 0.1121(2) 0.3588(2) 0.0132(4) Uani 1 1 d . . . H2 H 1.0082 0.1092 0.2721 0.016 Uiso 1 1 calc R . . N3 N 0.8467(3) 0.3926(2) 0.1306(2) 0.0134(4) Uani 1 1 d . . . H3 H 0.9543 0.3091 0.0905 0.016 Uiso 1 1 calc R . . N4 N 0.5362(3) 0.5080(2) 0.1862(2) 0.0134(4) Uani 1 1 d . . . H4 H 0.5342 0.6009 0.2056 0.016 Uiso 1 1 calc R . . C1 C 0.6748(4) -0.1455(3) 0.5385(3) 0.0228(6) Uani 1 1 d . . . H1A H 0.6341 -0.1523 0.4584 0.038(10) Uiso 1 1 d R . . H1B H 0.5707 -0.1209 0.6399 0.049(11) Uiso 1 1 d R . . H1C H 0.7755 -0.2486 0.5355 0.030(9) Uiso 1 1 d R . . C2 C 0.8573(3) -0.0039(3) 0.3734(3) 0.0117(5) Uani 1 1 d . . . C3 C 0.8364(4) 0.2428(3) 0.4770(3) 0.0154(5) Uani 1 1 d . . . H3A H 0.7057 0.3064 0.4971 0.020(8) Uiso 1 1 d R . . H3B H 0.9035 0.3116 0.4424 0.024(8) Uiso 1 1 d R . . H3C H 0.8459 0.1985 0.5718 0.021(8) Uiso 1 1 d R . . C4 C 0.8426(4) 0.5404(3) 0.1798(3) 0.0178(6) Uani 1 1 d . . . H4A H 0.8051 0.6241 0.1146 0.023(8) Uiso 1 1 d R . . H4B H 0.9659 0.5217 0.1708 0.016(7) Uiso 1 1 d R . . H4C H 0.7533 0.5752 0.2875 0.023(8) Uiso 1 1 d R . . C5 C 0.6965(3) 0.3776(3) 0.1431(3) 0.0111(5) Uani 1 1 d . . . C6 C 0.3639(3) 0.5032(3) 0.2026(3) 0.0167(5) Uani 1 1 d . . . H6A H 0.3899 0.4313 0.1178 0.032(9) Uiso 1 1 d R . . H6B H 0.2755 0.6115 0.1997 0.024(8) Uiso 1 1 d R . . H6C H 0.3111 0.4630 0.3012 0.032(9) Uiso 1 1 d R . . O1 O 0.2004(2) 0.1875(2) 0.1243(2) 0.0150(4) Uani 1 1 d . . . O2 O 0.4466(2) -0.1570(2) 0.19932(19) 0.0128(4) Uani 1 1 d . . . C7 C 0.3642(3) 0.0853(3) 0.0560(3) 0.0098(5) Uani 1 1 d . . . C8 C 0.4772(3) -0.0718(3) 0.0894(3) 0.0103(5) 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 0.01043(7) 0.00629(7) 0.00728(7) -0.00039(5) -0.00172(5) -0.00283(5) S1 0.0172(3) 0.0081(3) 0.0083(3) 0.0007(2) -0.0025(2) -0.0049(2) S2 0.0103(3) 0.0079(3) 0.0127(3) -0.0012(2) -0.0022(2) -0.0030(2) N1 0.0157(11) 0.0166(11) 0.0092(10) 0.0002(9) -0.0011(9) -0.0085(9) N2 0.0134(10) 0.0129(11) 0.0098(10) 0.0000(8) -0.0004(9) -0.0063(9) N3 0.0107(10) 0.0091(10) 0.0169(11) -0.0005(8) -0.0038(9) -0.0025(8) N4 0.0128(10) 0.0072(10) 0.0157(11) -0.0015(8) -0.0038(9) -0.0016(8) C1 0.0275(16) 0.0235(15) 0.0172(14) 0.0034(12) -0.0023(12) -0.0175(13) C2 0.0116(12) 0.0101(12) 0.0103(12) 0.0026(9) -0.0042(10) -0.0024(10) C3 0.0194(13) 0.0142(13) 0.0121(13) -0.0001(10) -0.0054(11) -0.0072(11) C4 0.0189(14) 0.0137(13) 0.0223(14) -0.0009(11) -0.0074(12) -0.0089(11) C5 0.0133(12) 0.0090(12) 0.0075(11) 0.0009(9) -0.0018(10) -0.0041(10) C6 0.0114(12) 0.0159(13) 0.0180(14) -0.0006(11) -0.0043(11) -0.0027(11) O1 0.0095(9) 0.0121(9) 0.0152(9) 0.0003(7) -0.0009(7) -0.0009(7) O2 0.0157(9) 0.0099(9) 0.0091(8) 0.0032(7) -0.0027(7) -0.0048(7) C7 0.0119(12) 0.0087(12) 0.0095(12) -0.0007(9) -0.0040(10) -0.0050(10) C8 0.0122(12) 0.0087(12) 0.0119(12) 0.0001(9) -0.0057(10) -0.0053(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 Pt1 S2 2.3194(6) . ? Pt1 S2 2.3194(6) 2_755 ? Pt1 S1 2.3225(6) 2_755 ? Pt1 S1 2.3225(6) . ? S1 C2 1.730(3) . ? S2 C5 1.727(3) . ? N1 C2 1.327(3) . ? N1 C1 1.455(3) . ? N2 C2 1.333(3) . ? N2 C3 1.448(3) . ? N3 C5 1.325(3) . ? N3 C4 1.455(3) . ? N4 C5 1.334(3) . ? N4 C6 1.459(3) . ? O1 C7 1.255(3) . ? O2 C8 1.259(3) . ? C7 C8 1.467(3) . ? C7 C8 1.473(3) 2_655 ? C8 C7 1.473(3) 2_655 ? 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(3) . 2_755 ? S2 Pt1 S1 90.92(2) . 2_755 ? S2 Pt1 S1 89.08(2) 2_755 2_755 ? S2 Pt1 S1 89.08(2) . . ? S2 Pt1 S1 90.92(2) 2_755 . ? S1 Pt1 S1 180.00(3) 2_755 . ? C2 S1 Pt1 106.37(8) . . ? C5 S2 Pt1 110.30(9) . . ? C2 N1 C1 123.5(2) . . ? C2 N2 C3 123.9(2) . . ? C5 N3 C4 123.3(2) . . ? C5 N4 C6 122.9(2) . . ? N1 C2 N2 119.6(2) . . ? N1 C2 S1 119.5(2) . . ? N2 C2 S1 120.92(19) . . ? N3 C5 N4 119.0(2) . . ? N3 C5 S2 122.78(18) . . ? N4 C5 S2 118.23(19) . . ? O1 C7 C8 134.5(2) . . ? O1 C7 C8 135.7(2) . 2_655 ? C8 C7 C8 89.80(19) . 2_655 ? O2 C8 C7 133.8(2) . . ? O2 C8 C7 136.0(2) . 2_655 ? C7 C8 C7 90.20(19) . 2_655 ? 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 H1 O2 0.88 1.97 2.802(3) 156.7 2_656 N2 H2 O1 0.88 2.05 2.871(3) 155.2 1_655 N3 H3 O1 0.88 2.11 2.842(3) 140.2 1_655 N4 H4 O2 0.88 2.03 2.843(3) 152.5 1_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.596 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.111 #===END data_2006sot0111 _database_code_depnum_ccdc_archive 'CCDC 679251' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 6SOT0111 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 N8 O4 Pt S4' _chemical_formula_weight 667.72 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9248(2) _cell_length_b 11.2125(3) _cell_length_c 11.4504(3) _cell_angle_alpha 62.074(1) _cell_angle_beta 86.405(1) _cell_angle_gamma 87.683(1) _cell_volume 1123.54(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4540 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Slab _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 6.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2302 _exptl_absorpt_correction_T_max 0.8254 _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 14605 reflections reduced R(int) from 0.1160 to 0.0314 Ratio of minimum to maximum apparent transmission: 0.574611 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 15570 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5119 _reflns_number_gt 4943 _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^+1.2723P] 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 5119 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0425 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 0.8141(3) 0.5375(3) -0.3232(3) 0.0300(7) Uani 1 1 d . . . H1A H 0.7165 0.5514 -0.3330 0.045 Uiso 1 1 calc R . . H1B H 0.8592 0.5588 -0.4092 0.045 Uiso 1 1 calc R . . H1C H 0.8479 0.5967 -0.2903 0.045 Uiso 1 1 calc R . . C2 C 0.7923(2) 0.3385(3) -0.1060(3) 0.0141(5) Uani 1 1 d . . . C3 C 0.7553(3) 0.5830(3) 0.3338(3) 0.0288(7) Uani 1 1 d . . . H3A H 0.7372 0.6433 0.2410 0.043 Uiso 1 1 calc R . . H3B H 0.8179 0.6265 0.3646 0.043 Uiso 1 1 calc R . . H3C H 0.6705 0.5639 0.3877 0.043 Uiso 1 1 calc R . . C4 C 0.7605(3) 0.3842(3) 0.2984(2) 0.0149(5) Uani 1 1 d . . . C5 C 0.4715(3) -0.1821(3) 0.3581(3) 0.0300(7) Uani 1 1 d . . . H5A H 0.4580 -0.2443 0.4527 0.045 Uiso 1 1 calc R . . H5B H 0.5513 -0.2106 0.3222 0.045 Uiso 1 1 calc R . . H5C H 0.3920 -0.1830 0.3119 0.045 Uiso 1 1 calc R . . C6 C 0.3944(3) 0.0291(3) 0.3556(2) 0.0156(5) Uani 1 1 d . . . C7 C 0.1100(3) 0.2451(3) 0.0651(3) 0.0279(7) Uani 1 1 d . . . H7A H 0.0771 0.2881 -0.0247 0.042 Uiso 1 1 calc R . . H7B H 0.0747 0.2945 0.1121 0.042 Uiso 1 1 calc R . . H7C H 0.0791 0.1515 0.1125 0.042 Uiso 1 1 calc R . . C8 C 0.3357(2) 0.1658(3) 0.0293(2) 0.0135(5) Uani 1 1 d . . . C9 C -0.0069(3) 0.1989(3) 0.6300(2) 0.0161(5) Uani 1 1 d . . . C10 C 0.0555(2) 0.1160(2) 0.7542(2) 0.0135(5) Uani 1 1 d . . . C11 C 0.1377(2) 0.0472(2) 0.6924(2) 0.0131(5) Uani 1 1 d . . . C12 C 0.0703(2) 0.1294(2) 0.5669(2) 0.0136(5) Uani 1 1 d . . . N1 N 0.8419(2) 0.3973(2) -0.2295(2) 0.0211(5) Uani 1 1 d . . . H1 H 0.8946 0.3493 -0.2567 0.025 Uiso 1 1 calc R . . N2 N 0.8187(2) 0.2083(2) -0.0292(2) 0.0154(4) Uani 1 1 d . . . H2A H 0.8687 0.1624 -0.0609 0.018 Uiso 1 1 calc R . . H2B H 0.7862 0.1680 0.0533 0.018 Uiso 1 1 calc R . . N3 N 0.8150(2) 0.4579(2) 0.3459(2) 0.0198(5) Uani 1 1 d . . . H3 H 0.8910 0.4293 0.3867 0.024 Uiso 1 1 calc R . . N4 N 0.8199(2) 0.2687(2) 0.3180(2) 0.0176(5) Uani 1 1 d . . . H4A H 0.8943 0.2420 0.3618 0.021 Uiso 1 1 calc R . . H4B H 0.7850 0.2188 0.2871 0.021 Uiso 1 1 calc R . . N5 N 0.4910(2) -0.0467(2) 0.3395(2) 0.0216(5) Uani 1 1 d . . . H5 H 0.5727 -0.0130 0.3160 0.026 Uiso 1 1 calc R . . N6 N 0.2718(2) -0.0189(2) 0.4018(2) 0.0206(5) Uani 1 1 d . . . H6A H 0.2538 -0.1029 0.4223 0.025 Uiso 1 1 calc R . . H6B H 0.2084 0.0331 0.4119 0.025 Uiso 1 1 calc R . . N7 N 0.2566(2) 0.2467(2) 0.0581(2) 0.0175(5) Uani 1 1 d . . . H7 H 0.2955 0.3061 0.0744 0.021 Uiso 1 1 calc R . . N8 N 0.2847(2) 0.0800(2) -0.0052(2) 0.0216(5) Uani 1 1 d . . . H8A H 0.1968 0.0764 -0.0091 0.026 Uiso 1 1 calc R . . H8B H 0.3388 0.0266 -0.0241 0.026 Uiso 1 1 calc R . . O1 O -0.0917(2) 0.2949(2) 0.59245(19) 0.0310(5) Uani 1 1 d . . . O2 O 0.04378(17) 0.10849(19) 0.86733(17) 0.0179(4) Uani 1 1 d . . . O3 O 0.22762(17) -0.04244(18) 0.73280(18) 0.0181(4) Uani 1 1 d . . . O4 O 0.07399(18) 0.14061(18) 0.45254(17) 0.0164(4) Uani 1 1 d . . . Pt1 Pt 0.564193(8) 0.299092(9) 0.132016(8) 0.01038(4) Uani 1 1 d . . . S1 S 0.69821(7) 0.43632(6) -0.05046(6) 0.01673(13) Uani 1 1 d . . . S2 S 0.61272(6) 0.44235(6) 0.21720(6) 0.01433(13) Uani 1 1 d . . . S3 S 0.42550(7) 0.19369(7) 0.32242(6) 0.01762(14) Uani 1 1 d . . . S4 S 0.50973(6) 0.17261(6) 0.02811(6) 0.01415(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 0.0441(18) 0.0180(15) 0.0201(14) -0.0040(12) 0.0087(13) 0.0052(13) C2 0.0116(11) 0.0146(13) 0.0190(13) -0.0102(11) -0.0008(10) -0.0006(9) C3 0.0430(18) 0.0171(15) 0.0302(16) -0.0125(13) -0.0191(14) 0.0034(13) C4 0.0171(12) 0.0127(12) 0.0120(12) -0.0030(10) -0.0025(10) -0.0021(10) C5 0.0364(17) 0.0163(15) 0.0343(17) -0.0106(13) 0.0058(14) 0.0043(13) C6 0.0185(12) 0.0158(13) 0.0118(12) -0.0059(10) -0.0018(10) 0.0019(10) C7 0.0124(13) 0.0351(18) 0.0485(19) -0.0298(16) -0.0020(12) 0.0030(12) C8 0.0130(11) 0.0121(12) 0.0132(12) -0.0038(10) -0.0038(9) 0.0026(9) C9 0.0152(12) 0.0184(13) 0.0154(12) -0.0085(11) -0.0041(10) 0.0039(10) C10 0.0124(11) 0.0115(12) 0.0161(12) -0.0057(10) -0.0047(9) 0.0012(9) C11 0.0126(11) 0.0090(12) 0.0165(12) -0.0049(10) -0.0010(9) -0.0013(9) C12 0.0116(11) 0.0125(12) 0.0173(12) -0.0073(10) -0.0002(9) -0.0022(9) N1 0.0256(12) 0.0143(12) 0.0226(12) -0.0089(10) 0.0035(10) 0.0042(9) N2 0.0131(10) 0.0136(11) 0.0203(11) -0.0092(9) 0.0010(8) 0.0031(8) N3 0.0230(12) 0.0136(11) 0.0226(12) -0.0072(10) -0.0132(9) 0.0022(9) N4 0.0180(11) 0.0154(11) 0.0218(11) -0.0102(9) -0.0095(9) 0.0047(9) N5 0.0209(11) 0.0152(12) 0.0241(12) -0.0064(10) 0.0037(10) 0.0038(9) N6 0.0198(11) 0.0128(11) 0.0263(12) -0.0075(10) 0.0051(9) 0.0003(9) N7 0.0129(10) 0.0196(12) 0.0265(12) -0.0159(10) -0.0043(9) 0.0020(9) N8 0.0122(11) 0.0228(13) 0.0406(14) -0.0231(12) -0.0078(10) 0.0033(9) O1 0.0388(12) 0.0349(12) 0.0199(10) -0.0143(9) -0.0120(9) 0.0273(10) O2 0.0164(9) 0.0243(10) 0.0142(9) -0.0100(8) -0.0038(7) 0.0055(8) O3 0.0171(9) 0.0149(9) 0.0209(9) -0.0072(8) -0.0065(7) 0.0091(7) O4 0.0181(9) 0.0172(9) 0.0161(9) -0.0098(8) -0.0026(7) 0.0033(7) Pt1 0.00980(6) 0.01031(6) 0.01287(6) -0.00680(4) -0.00324(4) 0.00222(4) S1 0.0205(3) 0.0109(3) 0.0190(3) -0.0079(3) 0.0044(3) 0.0002(2) S2 0.0164(3) 0.0131(3) 0.0172(3) -0.0098(3) -0.0065(2) 0.0039(2) S3 0.0203(3) 0.0167(3) 0.0183(3) -0.0107(3) 0.0035(3) -0.0016(3) S4 0.0111(3) 0.0162(3) 0.0206(3) -0.0130(3) -0.0030(2) 0.0014(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 C1 N1 1.456(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.321(3) . ? C2 N2 1.331(3) . ? C2 S1 1.724(3) . ? C3 N3 1.449(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N4 1.326(3) . ? C4 N3 1.329(3) . ? C4 S2 1.722(3) . ? C5 N5 1.451(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N5 1.317(3) . ? C6 N6 1.325(3) . ? C6 S3 1.738(3) . ? C7 N7 1.453(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N7 1.318(3) . ? C8 N8 1.326(3) . ? C8 S4 1.731(2) . ? C9 O1 1.260(3) . ? C9 C10 1.448(3) . ? C9 C12 1.457(4) . ? C10 O2 1.257(3) . ? C10 C11 1.465(3) . ? C11 O3 1.251(3) . ? C11 C12 1.481(3) . ? C12 O4 1.254(3) . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 H3 0.8800 . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? N5 H5 0.8800 . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? N7 H7 0.8800 . ? N8 H8A 0.8800 . ? N8 H8B 0.8800 . ? Pt1 S1 2.3039(6) . ? Pt1 S2 2.3136(6) . ? Pt1 S3 2.3209(6) . ? Pt1 S4 2.3328(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 N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 119.2(2) . . ? N1 C2 S1 118.0(2) . . ? N2 C2 S1 122.88(19) . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 N3 119.0(2) . . ? N4 C4 S2 123.1(2) . . ? N3 C4 S2 117.9(2) . . ? N5 C5 H5A 109.5 . . ? N5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 N6 121.2(2) . . ? N5 C6 S3 120.9(2) . . ? N6 C6 S3 117.9(2) . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N7 C8 N8 121.0(2) . . ? N7 C8 S4 121.40(19) . . ? N8 C8 S4 117.51(19) . . ? O1 C9 C10 133.7(2) . . ? O1 C9 C12 135.2(2) . . ? C10 C9 C12 91.1(2) . . ? O2 C10 C9 134.3(2) . . ? O2 C10 C11 135.5(2) . . ? C9 C10 C11 90.2(2) . . ? O3 C11 C10 133.7(2) . . ? O3 C11 C12 136.8(2) . . ? C10 C11 C12 89.50(19) . . ? O4 C12 C9 133.1(2) . . ? O4 C12 C11 137.7(2) . . ? C9 C12 C11 89.19(19) . . ? C2 N1 C1 123.4(2) . . ? C2 N1 H1 118.3 . . ? C1 N1 H1 118.3 . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C4 N3 C3 123.2(2) . . ? C4 N3 H3 118.4 . . ? C3 N3 H3 118.4 . . ? C4 N4 H4A 120.0 . . ? C4 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C6 N5 C5 124.2(2) . . ? C6 N5 H5 117.9 . . ? C5 N5 H5 117.9 . . ? C6 N6 H6A 120.0 . . ? C6 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C8 N7 C7 124.9(2) . . ? C8 N7 H7 117.5 . . ? C7 N7 H7 117.5 . . ? C8 N8 H8A 120.0 . . ? C8 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? S1 Pt1 S2 86.34(2) . . ? S1 Pt1 S3 169.89(2) . . ? S2 Pt1 S3 84.28(2) . . ? S1 Pt1 S4 90.25(2) . . ? S2 Pt1 S4 174.63(2) . . ? S3 Pt1 S4 98.82(2) . . ? C2 S1 Pt1 109.43(9) . . ? C4 S2 Pt1 107.04(9) . . ? C6 S3 Pt1 110.04(9) . . ? C8 S4 Pt1 108.59(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 N1 H1 O1 0.88 2.08 2.806(3) 139.3 1_654 N2 H2A O2 0.88 2.06 2.890(3) 156.0 1_654 N2 H2B O3 0.88 2.18 3.025(3) 161.4 2_656 N3 H3 O1 0.88 2.13 2.744(3) 125.8 1_655 N4 H4A O4 0.88 2.12 2.986(3) 166.0 1_655 N4 H4B O3 0.88 2.10 2.917(3) 153.5 2_656 N5 H5 O3 0.88 2.06 2.940(3) 173.0 2_656 N6 H6B O4 0.88 1.94 2.818(3) 174.2 . N7 H7 S1 0.88 2.77 3.560(2) 149.6 2_665 N7 H7 S3 0.88 2.88 3.346(2) 114.8 . N8 H8A O2 0.88 2.05 2.809(3) 144.5 1_554 N8 H8B S4 0.88 2.66 3.524(2) 167.8 2_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.597 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.104 #===END data_2006sot0112 _database_code_depnum_ccdc_archive 'CCDC 679252' _chemical_compound_source 'Robeto Quesada' _database_code_CSD 6SOT0112 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 N8 O9 Pt S4' _chemical_formula_weight 863.88 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 9.0790(2) _cell_length_b 10.1629(2) _cell_length_c 18.0682(3) _cell_angle_alpha 86.435(1) _cell_angle_beta 75.880(1) _cell_angle_gamma 70.191(1) _cell_volume 1520.71(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6701 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Orange _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 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 4.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36345 _exptl_absorpt_correction_T_max 0.37196 _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 24068 reflections reduced R(int) from 0.0820 to 0.0346 Ratio of minimum to maximum apparent transmission: 0.794885 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _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 28297 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6942 _reflns_number_gt 6164 _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. Distance and angle restraints were used to model the hydrogen positions of the water molecules. ; _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^)+(0.0204P)^2^+0.9644P] 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 0.00232(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6942 _refine_ls_number_parameters 417 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.009 _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 0.5099(3) 0.1990(3) 0.28529(16) 0.0153(6) Uani 1 1 d . . . C2 C 0.4713(3) 0.0557(3) 0.38024(17) 0.0196(6) Uani 1 1 d . . . H2 H 0.4189 0.0113 0.4209 0.024 Uiso 1 1 calc R . . C3 C 0.6314(4) 0.0262(3) 0.35422(17) 0.0210(7) Uani 1 1 d . . . H3 H 0.7134 -0.0428 0.3731 0.025 Uiso 1 1 calc R . . C4 C 0.8103(3) 0.1206(4) 0.2513(2) 0.0312(8) Uani 1 1 d . . . H4A H 0.8062 0.1411 0.1980 0.047 Uiso 1 1 calc R . . H4B H 0.8940 0.0303 0.2537 0.047 Uiso 1 1 calc R . . H4C H 0.8355 0.1942 0.2729 0.047 Uiso 1 1 calc R . . C5 C 0.4640(3) 0.3984(3) 0.42493(15) 0.0134(6) Uani 1 1 d . . . C6 C 0.2350(3) 0.3793(3) 0.49629(16) 0.0186(6) Uani 1 1 d . . . H6 H 0.1240 0.3895 0.5135 0.022 Uiso 1 1 calc R . . C7 C 0.3537(3) 0.3065(3) 0.53015(16) 0.0180(6) Uani 1 1 d . . . H7 H 0.3422 0.2561 0.5761 0.022 Uiso 1 1 calc R . . C8 C 0.6558(3) 0.2531(3) 0.50046(17) 0.0205(7) Uani 1 1 d . . . H8A H 0.7102 0.1642 0.4718 0.031 Uiso 1 1 calc R . . H8B H 0.6452 0.2358 0.5552 0.031 Uiso 1 1 calc R . . H8C H 0.7193 0.3154 0.4844 0.031 Uiso 1 1 calc R . . C9 C 0.5191(3) 0.8404(3) 0.20818(15) 0.0139(6) Uani 1 1 d . . . C10 C 0.5863(4) 0.9350(3) 0.09660(17) 0.0222(7) Uani 1 1 d . . . H10 H 0.6481 0.9530 0.0490 0.027 Uiso 1 1 calc R . . C11 C 0.4273(4) 0.9999(3) 0.12623(17) 0.0208(7) Uani 1 1 d . . . H11 H 0.3561 1.0725 0.1034 0.025 Uiso 1 1 calc R . . C12 C 0.2251(3) 0.9740(3) 0.24428(18) 0.0258(7) Uani 1 1 d . . . H12A H 0.1717 0.9145 0.2291 0.039 Uiso 1 1 calc R . . H12B H 0.1635 1.0725 0.2387 0.039 Uiso 1 1 calc R . . H12C H 0.2310 0.9572 0.2977 0.039 Uiso 1 1 calc R . . C13 C 0.5235(3) 0.6148(3) 0.07809(15) 0.0145(6) Uani 1 1 d . . . C15 C 0.6474(3) 0.6429(3) -0.04144(16) 0.0205(7) Uani 1 1 d . . . H15 H 0.6646 0.6695 -0.0933 0.025 Uiso 1 1 calc R . . C16 C 0.3417(4) 0.7474(3) -0.00362(17) 0.0237(7) Uani 1 1 d . . . H16A H 0.2667 0.6962 0.0160 0.036 Uiso 1 1 calc R . . H16B H 0.3516 0.7604 -0.0586 0.036 Uiso 1 1 calc R . . H16C H 0.3011 0.8389 0.0224 0.036 Uiso 1 1 calc R . . C17 C 0.0178(3) 0.4175(3) 0.21888(17) 0.0199(7) Uani 1 1 d . . . C18 C 0.0513(3) 0.4268(3) 0.29319(17) 0.0188(7) Uani 1 1 d . . . C19 C 0.0411(3) 0.5710(3) 0.30544(16) 0.0157(6) Uani 1 1 d . . . C20 C -0.0173(3) 0.6562(3) 0.24393(15) 0.0147(6) Uani 1 1 d . . . C21 C -0.0343(3) 0.5612(3) 0.19070(16) 0.0162(6) Uani 1 1 d . . . C104 C 0.7618(4) 0.5740(4) -0.00438(17) 0.0245(7) Uani 1 1 d . . . H104 H 0.8750 0.5440 -0.0248 0.029 Uiso 1 1 calc R . . N1 N 0.3984(3) 0.1617(2) 0.33706(13) 0.0165(5) Uani 1 1 d . . . H1 H 0.2936 0.1999 0.3425 0.020 Uiso 1 1 calc R . . N2 N 0.6538(3) 0.1151(2) 0.29506(13) 0.0175(5) Uani 1 1 d . . . N3 N 0.3050(3) 0.4365(3) 0.43169(13) 0.0161(5) Uani 1 1 d . . . H3A H 0.2528 0.4901 0.3997 0.019 Uiso 1 1 calc R . . N4 N 0.4958(3) 0.3186(2) 0.48556(12) 0.0145(5) Uani 1 1 d . . . N5 N 0.6407(3) 0.8383(3) 0.14848(13) 0.0168(5) Uani 1 1 d . . . H5 H 0.7411 0.7827 0.1433 0.020 Uiso 1 1 calc R . . N6 N 0.3878(3) 0.9411(2) 0.19567(13) 0.0167(5) Uani 1 1 d . . . N7 N 0.6834(3) 0.5551(3) 0.06891(13) 0.0201(6) Uani 1 1 d . . . H7A H 0.7312 0.5105 0.1045 0.024 Uiso 1 1 calc R . . N8 N 0.4996(3) 0.6679(3) 0.01024(13) 0.0156(5) Uani 1 1 d . . . O1 O 0.0311(3) 0.3098(2) 0.18521(13) 0.0308(5) Uani 1 1 d . . . O2 O 0.0867(2) 0.3291(2) 0.33827(12) 0.0257(5) Uani 1 1 d . . . O3 O 0.0771(2) 0.6143(2) 0.35991(11) 0.0210(5) Uani 1 1 d . . . O4 O -0.0445(2) 0.7836(2) 0.23523(11) 0.0212(5) Uani 1 1 d . . . O5 O -0.0847(2) 0.5976(2) 0.13162(11) 0.0224(5) Uani 1 1 d . . . O6 O 0.0797(3) 0.1047(3) 0.42997(14) 0.0326(6) Uani 1 1 d D . . O7 O 0.0735(3) 0.1417(3) 0.05315(15) 0.0389(7) Uani 1 1 d D . . O8 O 0.9616(3) 0.8932(3) 0.41456(15) 0.0327(6) Uani 1 1 d D . . O9 O 0.9653(3) 0.9158(3) 0.09116(15) 0.0349(6) Uani 1 1 d D . . Pt1 Pt 0.496187(12) 0.529941(11) 0.255208(5) 0.01251(5) Uani 1 1 d . . . S1 S 0.46722(9) 0.32672(8) 0.21855(4) 0.01875(16) Uani 1 1 d . . . S2 S 0.61063(8) 0.43862(8) 0.35677(4) 0.01525(15) Uani 1 1 d . . . S3 S 0.53442(9) 0.73275(8) 0.28627(4) 0.01686(15) Uani 1 1 d . . . S4 S 0.37122(8) 0.62926(8) 0.15781(4) 0.01507(15) Uani 1 1 d . . . H92 H 0.969(5) 0.869(4) 0.058(2) 0.050 Uiso 1 1 d D . . H93 H 0.964(5) 0.871(4) 0.128(2) 0.050 Uiso 1 1 d D . . H94 H 0.997(5) 0.820(5) 0.396(2) 0.050 Uiso 1 1 d D . . H95 H 0.944(5) 0.890(4) 0.458(2) 0.050 Uiso 1 1 d D . . H96 H 0.042(5) 0.081(4) 0.071(2) 0.050 Uiso 1 1 d D . . H97 H 0.043(5) 0.203(4) 0.087(2) 0.050 Uiso 1 1 d D . . H98 H 0.050(5) 0.172(4) 0.407(2) 0.050 Uiso 1 1 d D . . H99 H 0.045(5) 0.051(4) 0.418(2) 0.050 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 C1 0.0198(14) 0.0112(15) 0.0168(14) -0.0011(12) -0.0051(11) -0.0070(12) C2 0.0257(16) 0.0136(16) 0.0211(15) 0.0050(12) -0.0069(13) -0.0084(13) C3 0.0257(16) 0.0109(15) 0.0270(16) 0.0041(13) -0.0116(13) -0.0036(13) C4 0.0161(15) 0.028(2) 0.042(2) -0.0033(16) 0.0052(14) -0.0052(14) C5 0.0159(13) 0.0121(14) 0.0116(13) 0.0001(11) -0.0041(11) -0.0035(11) C6 0.0179(14) 0.0233(17) 0.0162(14) 0.0002(12) -0.0024(12) -0.0100(13) C7 0.0230(15) 0.0199(16) 0.0125(14) 0.0045(12) -0.0025(12) -0.0108(13) C8 0.0196(15) 0.0230(17) 0.0188(15) 0.0065(13) -0.0089(12) -0.0052(13) C9 0.0158(13) 0.0110(14) 0.0159(14) 0.0001(11) -0.0046(11) -0.0049(11) C10 0.0261(16) 0.0241(18) 0.0170(15) 0.0098(13) -0.0046(12) -0.0112(14) C11 0.0271(16) 0.0154(16) 0.0224(16) 0.0066(13) -0.0117(13) -0.0074(13) C12 0.0127(14) 0.0236(18) 0.0343(18) -0.0049(14) 0.0014(13) -0.0015(13) C13 0.0187(14) 0.0144(15) 0.0119(13) 0.0000(11) -0.0033(11) -0.0076(12) C15 0.0249(15) 0.0293(18) 0.0100(13) -0.0001(12) 0.0010(12) -0.0161(14) C16 0.0260(16) 0.0262(18) 0.0201(16) 0.0073(13) -0.0101(13) -0.0082(14) C17 0.0140(14) 0.0184(17) 0.0265(16) -0.0023(13) -0.0008(12) -0.0068(12) C18 0.0077(13) 0.0193(17) 0.0258(16) 0.0059(13) -0.0011(12) -0.0030(12) C19 0.0114(13) 0.0200(17) 0.0143(14) 0.0010(12) -0.0018(11) -0.0044(12) C20 0.0094(13) 0.0170(16) 0.0144(14) 0.0017(12) -0.0008(11) -0.0019(11) C21 0.0097(13) 0.0229(17) 0.0137(14) 0.0000(12) -0.0009(11) -0.0036(12) C104 0.0181(15) 0.038(2) 0.0177(15) -0.0067(14) 0.0005(12) -0.0116(14) N1 0.0141(11) 0.0147(13) 0.0204(13) 0.0027(10) -0.0049(10) -0.0043(10) N2 0.0151(12) 0.0122(13) 0.0232(13) -0.0006(10) -0.0021(10) -0.0037(10) N3 0.0148(12) 0.0200(14) 0.0137(12) 0.0029(10) -0.0059(10) -0.0048(10) N4 0.0180(12) 0.0153(13) 0.0109(11) 0.0032(10) -0.0043(9) -0.0063(10) N5 0.0138(11) 0.0172(14) 0.0184(12) 0.0034(10) -0.0036(10) -0.0045(10) N6 0.0155(12) 0.0134(13) 0.0196(13) 0.0014(10) -0.0042(10) -0.0032(10) N7 0.0168(12) 0.0283(15) 0.0146(12) -0.0011(11) -0.0051(10) -0.0055(11) N8 0.0193(12) 0.0176(13) 0.0117(11) 0.0021(10) -0.0036(9) -0.0087(10) O1 0.0356(13) 0.0233(13) 0.0363(13) -0.0043(11) -0.0063(11) -0.0141(11) O2 0.0192(11) 0.0219(12) 0.0338(13) 0.0129(10) -0.0061(9) -0.0064(9) O3 0.0208(11) 0.0222(12) 0.0192(11) 0.0012(9) -0.0074(9) -0.0045(9) O4 0.0235(11) 0.0156(12) 0.0230(11) 0.0037(9) -0.0070(9) -0.0042(9) O5 0.0164(10) 0.0292(13) 0.0193(11) -0.0024(9) -0.0073(8) -0.0020(9) O6 0.0373(14) 0.0289(15) 0.0330(14) 0.0104(11) -0.0058(11) -0.0164(12) O7 0.0486(16) 0.0433(18) 0.0307(14) -0.0048(12) -0.0026(12) -0.0269(14) O8 0.0375(14) 0.0243(14) 0.0349(14) -0.0050(12) -0.0148(12) -0.0030(11) O9 0.0407(14) 0.0407(17) 0.0256(13) 0.0129(11) -0.0076(12) -0.0189(13) Pt1 0.01447(6) 0.01306(7) 0.01005(6) 0.00226(4) -0.00234(4) -0.00542(4) S1 0.0296(4) 0.0159(4) 0.0153(3) 0.0028(3) -0.0087(3) -0.0115(3) S2 0.0156(3) 0.0178(4) 0.0131(3) 0.0044(3) -0.0042(3) -0.0067(3) S3 0.0256(4) 0.0155(4) 0.0130(3) 0.0034(3) -0.0070(3) -0.0103(3) S4 0.0150(3) 0.0188(4) 0.0119(3) 0.0033(3) -0.0033(3) -0.0067(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 N1 1.341(3) . ? C1 N2 1.343(3) . ? C1 S1 1.727(3) . ? C2 C3 1.347(4) . ? C2 N1 1.368(4) . ? C3 N2 1.377(4) . ? C4 N2 1.466(4) . ? C5 N3 1.338(3) . ? C5 N4 1.351(3) . ? C5 S2 1.721(3) . ? C6 C7 1.345(4) . ? C6 N3 1.382(4) . ? C7 N4 1.384(3) . ? C8 N4 1.463(3) . ? C9 N5 1.337(3) . ? C9 N6 1.340(3) . ? C9 S3 1.734(3) . ? C10 C11 1.351(4) . ? C10 N5 1.368(4) . ? C11 N6 1.376(4) . ? C12 N6 1.461(3) . ? C13 N7 1.342(3) . ? C13 N8 1.345(3) . ? C13 S4 1.710(3) . ? C15 C104 1.343(4) . ? C15 N8 1.387(3) . ? C16 N8 1.461(4) . ? C17 O1 1.241(4) . ? C17 C18 1.463(4) . ? C17 C21 1.473(4) . ? C18 O2 1.250(3) . ? C18 C19 1.464(4) . ? C19 O3 1.256(3) . ? C19 C20 1.457(4) . ? C20 O4 1.241(3) . ? C20 C21 1.473(4) . ? C21 O5 1.249(3) . ? C104 N7 1.378(4) . ? Pt1 S2 2.3181(7) . ? Pt1 S4 2.3195(7) . ? Pt1 S1 2.3231(7) . ? Pt1 S3 2.3254(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 N1 C1 N2 106.4(2) . . ? N1 C1 S1 124.4(2) . . ? N2 C1 S1 129.1(2) . . ? C3 C2 N1 107.0(3) . . ? C2 C3 N2 107.0(3) . . ? N3 C5 N4 106.7(2) . . ? N3 C5 S2 130.4(2) . . ? N4 C5 S2 122.9(2) . . ? C7 C6 N3 107.0(2) . . ? C6 C7 N4 107.2(2) . . ? N5 C9 N6 106.8(2) . . ? N5 C9 S3 125.3(2) . . ? N6 C9 S3 127.9(2) . . ? C11 C10 N5 106.6(3) . . ? C10 C11 N6 107.2(3) . . ? N7 C13 N8 106.5(2) . . ? N7 C13 S4 129.8(2) . . ? N8 C13 S4 123.7(2) . . ? C104 C15 N8 107.2(2) . . ? O1 C17 C18 127.0(3) . . ? O1 C17 C21 126.0(3) . . ? C18 C17 C21 106.9(3) . . ? O2 C18 C17 126.7(3) . . ? O2 C18 C19 125.2(3) . . ? C17 C18 C19 108.1(2) . . ? O3 C19 C20 125.5(3) . . ? O3 C19 C18 125.6(3) . . ? C20 C19 C18 108.8(2) . . ? O4 C20 C19 127.9(3) . . ? O4 C20 C21 125.2(3) . . ? C19 C20 C21 106.9(3) . . ? O5 C21 C20 125.2(3) . . ? O5 C21 C17 126.1(3) . . ? C20 C21 C17 108.7(2) . . ? C15 C104 N7 106.9(3) . . ? C1 N1 C2 110.1(2) . . ? C1 N2 C3 109.5(2) . . ? C1 N2 C4 125.2(3) . . ? C3 N2 C4 125.3(2) . . ? C5 N3 C6 109.9(2) . . ? C5 N4 C7 109.2(2) . . ? C5 N4 C8 125.1(2) . . ? C7 N4 C8 125.6(2) . . ? C9 N5 C10 110.1(2) . . ? C9 N6 C11 109.2(2) . . ? C9 N6 C12 125.5(2) . . ? C11 N6 C12 125.1(2) . . ? C13 N7 C104 110.1(2) . . ? C13 N8 C15 109.3(2) . . ? C13 N8 C16 124.2(2) . . ? C15 N8 C16 126.4(2) . . ? S2 Pt1 S4 177.14(2) . . ? S2 Pt1 S1 97.46(3) . . ? S4 Pt1 S1 83.99(3) . . ? S2 Pt1 S3 83.67(3) . . ? S4 Pt1 S3 94.99(3) . . ? S1 Pt1 S3 177.19(2) . . ? C1 S1 Pt1 110.17(10) . . ? C5 S2 Pt1 106.45(9) . . ? C9 S3 Pt1 106.80(10) . . ? C13 S4 Pt1 105.77(10) . . ? 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 H1 O2 0.88 1.91 2.759(3) 162.0 . N1 H1 O6 0.88 2.61 3.189(3) 124.6 . N3 H3A O3 0.88 1.93 2.777(3) 160.2 . O6 H98 O2 0.78(4) 2.03(4) 2.744(3) 152(4) . O7 H97 O1 0.82(4) 2.11(4) 2.893(3) 160(4) . N5 H5 O5 0.88 1.99 2.807(3) 154.1 1_655 N7 H7A O5 0.88 2.30 2.782(3) 114.8 1_655 O8 H94 O3 0.76(4) 2.06(4) 2.817(3) 172(4) 1_655 O9 H93 O4 0.78(4) 2.08(4) 2.850(3) 170(4) 1_655 O6 H99 O8 0.78(4) 2.00(4) 2.763(4) 164(4) 1_445 O7 H96 O9 0.79(4) 2.01(4) 2.778(4) 166(4) 1_445 O8 H95 O6 0.76(4) 1.99(4) 2.742(4) 172(5) 2_666 O9 H92 O7 0.78(4) 2.15(4) 2.836(4) 148(4) 2_665 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.767 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.142 #===END data_2006sot0113 _database_code_depnum_ccdc_archive 'CCDC 679253' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 6SOT0113 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 N8 O10 Pt S4' _chemical_formula_weight 891.89 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 8.9330(2) _cell_length_b 9.1168(2) _cell_length_c 10.3243(3) _cell_angle_alpha 73.117(1) _cell_angle_beta 89.962(1) _cell_angle_gamma 74.790(1) _cell_volume 773.79(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3272 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Orange' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 4.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6416 _exptl_absorpt_correction_T_max 0.9089 _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 15462 reflections reduced R(int) from 0.0992 to 0.0393 Ratio of minimum to maximum apparent transmission: 0.836924 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 15504 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3540 _reflns_number_gt 3533 _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^+0.8456P] 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 3540 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0414 _refine_ls_wR_factor_gt 0.0413 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.010 _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 0.0000 0.5000 0.5000 0.01129(5) Uani 1 2 d S . . S1 S -0.06640(7) 0.44896(7) 0.30267(6) 0.01573(13) Uani 1 1 d . . . S2 S 0.19747(7) 0.61425(7) 0.41723(6) 0.01480(13) Uani 1 1 d . . . N1 N 0.1811(2) 0.3690(2) 0.1575(2) 0.0160(4) Uani 1 1 d . . . H1 H 0.1987 0.2662 0.1980 0.019 Uiso 1 1 calc R . . N2 N 0.0796(2) 0.6224(2) 0.1011(2) 0.0160(4) Uani 1 1 d . . . N3 N 0.3672(2) 0.3040(2) 0.4410(2) 0.0145(4) Uani 1 1 d . . . H3 H 0.3043 0.2564 0.4918 0.017 Uiso 1 1 calc R . . N4 N 0.4694(2) 0.4863(2) 0.3249(2) 0.0138(4) Uani 1 1 d . . . C1 C 0.0684(3) 0.4835(3) 0.1855(2) 0.0138(5) Uani 1 1 d . . . C2 C 0.2647(3) 0.4360(3) 0.0566(3) 0.0198(5) Uani 1 1 d . . . H2 H 0.3506 0.3810 0.0189 0.024 Uiso 1 1 calc R . . C3 C 0.2015(3) 0.5950(3) 0.0213(3) 0.0206(6) Uani 1 1 d . . . H3A H 0.2347 0.6734 -0.0458 0.025 Uiso 1 1 calc R . . C4 C -0.0207(4) 0.7795(3) 0.0962(3) 0.0278(6) Uani 1 1 d . . . H4A H -0.1157 0.7673 0.1406 0.042 Uiso 1 1 calc R . . H4B H -0.0484 0.8450 0.0013 0.042 Uiso 1 1 calc R . . H4C H 0.0346 0.8312 0.1434 0.042 Uiso 1 1 calc R . . C5 C 0.3465(3) 0.4621(3) 0.3962(2) 0.0128(5) Uani 1 1 d . . . C6 C 0.5018(3) 0.2269(3) 0.3957(3) 0.0174(5) Uani 1 1 d . . . H6 H 0.5413 0.1152 0.4121 0.021 Uiso 1 1 calc R . . C7 C 0.5666(3) 0.3398(3) 0.3238(3) 0.0178(5) Uani 1 1 d . . . H7 H 0.6608 0.3228 0.2806 0.021 Uiso 1 1 calc R . . C8 C 0.4924(3) 0.6420(3) 0.2563(3) 0.0189(5) Uani 1 1 d . . . H8A H 0.4326 0.6865 0.1675 0.028 Uiso 1 1 calc R . . H8B H 0.6031 0.6306 0.2437 0.028 Uiso 1 1 calc R . . H8C H 0.4568 0.7137 0.3115 0.028 Uiso 1 1 calc R . . C9 C 0.0077(3) -0.0262(3) 0.6482(2) 0.0143(5) Uani 1 1 d . . . C10 C 0.1244(3) 0.0368(3) 0.5666(2) 0.0138(5) Uani 1 1 d . . . C11 C 0.1268(3) 0.0449(3) 0.4224(2) 0.0137(5) Uani 1 1 d . . . O1 O 0.0190(2) -0.0595(2) 0.77352(17) 0.0223(4) Uani 1 1 d . . . O2 O 0.2241(2) 0.0801(2) 0.62043(17) 0.0185(4) Uani 1 1 d . . . O3 O 0.2407(2) 0.0707(2) 0.35971(17) 0.0184(4) Uani 1 1 d . . . O4 O 0.3365(3) 0.9114(3) -0.0877(2) 0.0274(5) Uani 1 1 d . . . H98 H 0.282(5) 0.950(5) -0.150(4) 0.047(12) Uiso 1 1 d . . . H99 H 0.415(4) 0.929(4) -0.117(3) 0.030(10) Uiso 1 1 d . . . O5 O 0.3700(3) 0.0450(3) 0.1190(3) 0.0294(5) Uani 1 1 d . . . H96 H 0.322(5) 0.022(5) 0.181(4) 0.055(13) Uiso 1 1 d . . . H97 H 0.340(4) 0.009(4) 0.066(4) 0.037(11) Uiso 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 0.00992(7) 0.01253(7) 0.01129(7) -0.00443(5) 0.00255(5) -0.00191(5) S1 0.0142(3) 0.0226(3) 0.0138(3) -0.0089(3) 0.0038(2) -0.0072(3) S2 0.0141(3) 0.0144(3) 0.0172(3) -0.0062(2) 0.0051(2) -0.0046(2) N1 0.0178(11) 0.0142(10) 0.0156(11) -0.0050(8) 0.0031(8) -0.0032(9) N2 0.0195(11) 0.0167(11) 0.0116(10) -0.0056(8) 0.0015(8) -0.0032(9) N3 0.0121(10) 0.0155(10) 0.0154(10) -0.0039(8) 0.0023(8) -0.0038(8) N4 0.0112(10) 0.0162(10) 0.0144(10) -0.0048(8) 0.0028(8) -0.0044(8) C1 0.0147(12) 0.0176(12) 0.0096(11) -0.0051(9) -0.0011(9) -0.0039(10) C2 0.0190(13) 0.0245(14) 0.0173(13) -0.0084(11) 0.0072(10) -0.0061(11) C3 0.0269(14) 0.0256(14) 0.0114(12) -0.0054(11) 0.0064(11) -0.0109(12) C4 0.0344(17) 0.0171(13) 0.0248(15) -0.0043(12) 0.0020(13) 0.0026(12) C5 0.0119(11) 0.0171(12) 0.0103(11) -0.0046(10) -0.0004(9) -0.0048(10) C6 0.0130(12) 0.0145(12) 0.0233(14) -0.0069(10) 0.0005(10) -0.0003(10) C7 0.0111(12) 0.0216(13) 0.0220(14) -0.0095(11) 0.0046(10) -0.0031(10) C8 0.0169(13) 0.0194(13) 0.0200(13) -0.0025(11) 0.0041(10) -0.0079(11) C9 0.0169(12) 0.0107(11) 0.0144(12) -0.0038(9) 0.0041(10) -0.0024(10) C10 0.0128(12) 0.0095(11) 0.0159(12) -0.0023(9) 0.0011(10) 0.0005(9) C11 0.0156(12) 0.0078(11) 0.0144(12) -0.0006(9) 0.0028(10) -0.0010(9) O1 0.0318(11) 0.0270(10) 0.0110(9) -0.0061(8) 0.0036(8) -0.0122(9) O2 0.0176(9) 0.0206(9) 0.0183(9) -0.0060(8) 0.0011(7) -0.0068(8) O3 0.0181(9) 0.0193(9) 0.0184(9) -0.0051(7) 0.0063(7) -0.0069(8) O4 0.0304(13) 0.0312(12) 0.0195(11) -0.0065(9) -0.0024(10) -0.0081(10) O5 0.0326(12) 0.0356(12) 0.0251(12) -0.0157(10) 0.0117(10) -0.0108(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 Pt1 S2 2.3178(6) . ? Pt1 S2 2.3178(6) 2_566 ? Pt1 S1 2.3273(6) 2_566 ? Pt1 S1 2.3273(6) . ? S1 C1 1.729(2) . ? S2 C5 1.717(2) . ? N1 C1 1.345(3) . ? N1 C2 1.373(3) . ? N2 C1 1.341(3) . ? N2 C3 1.379(3) . ? N2 C4 1.463(3) . ? N3 C5 1.342(3) . ? N3 C6 1.380(3) . ? N4 C5 1.352(3) . ? N4 C7 1.392(3) . ? N4 C8 1.459(3) . ? C2 C3 1.347(4) . ? C6 C7 1.347(3) . ? C9 O1 1.238(3) . ? C9 C10 1.469(3) . ? C9 C11 1.478(3) 2_556 ? C10 O2 1.253(3) . ? C10 C11 1.470(3) . ? C11 O3 1.243(3) . ? C11 C9 1.478(3) 2_556 ? 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 180.000(1) . 2_566 ? S2 Pt1 S1 82.86(2) . 2_566 ? S2 Pt1 S1 97.14(2) 2_566 2_566 ? S2 Pt1 S1 97.14(2) . . ? S2 Pt1 S1 82.86(2) 2_566 . ? S1 Pt1 S1 180.0 2_566 . ? C1 S1 Pt1 110.13(8) . . ? C5 S2 Pt1 105.88(8) . . ? C1 N1 C2 110.2(2) . . ? C1 N2 C3 109.8(2) . . ? C1 N2 C4 125.1(2) . . ? C3 N2 C4 125.2(2) . . ? C5 N3 C6 110.0(2) . . ? C5 N4 C7 109.17(19) . . ? C5 N4 C8 125.0(2) . . ? C7 N4 C8 125.8(2) . . ? N2 C1 N1 106.2(2) . . ? N2 C1 S1 128.93(19) . . ? N1 C1 S1 124.77(18) . . ? C3 C2 N1 106.8(2) . . ? C2 C3 N2 107.1(2) . . ? N3 C5 N4 106.7(2) . . ? N3 C5 S2 129.98(18) . . ? N4 C5 S2 123.33(18) . . ? C7 C6 N3 107.2(2) . . ? C6 C7 N4 107.0(2) . . ? O1 C9 C10 120.9(2) . . ? O1 C9 C11 120.3(2) . 2_556 ? C10 C9 C11 118.7(2) . 2_556 ? O2 C10 C9 120.2(2) . . ? O2 C10 C11 119.9(2) . . ? C9 C10 C11 119.9(2) . . ? O3 C11 C10 119.8(2) . . ? O3 C11 C9 120.3(2) . 2_556 ? C10 C11 C9 119.9(2) . 2_556 ? 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 H1 O3 0.88 2.01 2.826(3) 154.4 . N1 H1 O5 0.88 2.53 3.130(3) 126.0 . N3 H3 O2 0.88 2.06 2.899(3) 160.2 . O4 H98 O2 0.75(4) 2.31(4) 2.993(3) 153(4) 1_564 O4 H98 O1 0.75(4) 2.50(4) 3.092(3) 137(4) 1_564 O4 H99 O5 0.80(4) 1.99(4) 2.758(3) 159(3) 2_665 O5 H96 O3 0.78(4) 2.11(4) 2.785(3) 146(4) . O5 H97 O4 0.79(4) 2.04(4) 2.798(3) 161(3) 1_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.525 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.102 #===END data_2006sot0114 _database_code_depnum_ccdc_archive 'CCDC 679254' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 6SOT0114 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 N8 Pt S4, C4 O4' _chemical_formula_sum 'C20 H24 N8 O4 Pt S4' _chemical_formula_weight 763.80 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.882(5) _cell_length_b 8.601(5) _cell_length_c 11.590(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1383.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1819 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 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 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4006 _exptl_absorpt_correction_T_max 0.4106 _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 10248 reflections reduced R(int) from 0.0735 to 0.0371 Ratio of minimum to maximum apparent transmission: 0.701724 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _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 12377 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1655 _reflns_number_gt 1452 _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. Due to the large percentage of disorder it was necessary to apply global thermal parameter restraints. ; _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^)+(0.0541P)^2^+36.6041P] 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 1655 _refine_ls_number_parameters 143 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.237 _refine_ls_shift/su_max 0.025 _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 Pt1 Pt 0.5000 0.5000 0.5000 0.0134(2) Uani 1 4 d S . . S2 S 0.3353(2) 0.5412(4) 0.5000 0.0184(7) Uani 1 2 d SU . . S1 S 0.4864(2) 0.2311(4) 0.5000 0.0191(7) Uani 1 2 d S . . N1 N 0.3216(11) 0.1025(18) 0.4041(13) 0.017(3) Uani 0.50 1 d PU A 1 N2 N 0.3974(11) 0.2554(18) 0.2864(12) 0.016(2) Uani 0.50 1 d PU A 1 H2 H 0.4392 0.3213 0.2569 0.019 Uiso 0.50 1 calc PR A 1 C1 C 0.2967(11) 0.0178(17) 0.5000 0.026(3) Uani 1 2 d SU A 1 H1A H 0.3353 0.0522 0.5660 0.039 Uiso 0.50 1 calc PR A 1 H1B H 0.3086 -0.0928 0.4855 0.039 Uiso 0.50 1 calc PR A 1 H1C H 0.2282 0.0336 0.5169 0.039 Uiso 0.50 1 calc PR A 1 C2 C 0.4014(13) 0.195(2) 0.3936(15) 0.015(3) Uani 0.50 1 d PU A 1 C3 C 0.3181(14) 0.198(2) 0.2306(16) 0.019(3) Uani 0.50 1 d PU A 1 H3 H 0.2998 0.2223 0.1537 0.023 Uiso 0.50 1 calc PR A 1 C4 C 0.2700(14) 0.101(2) 0.3011(15) 0.017(3) Uani 0.50 1 d PU A 1 H4 H 0.2132 0.0437 0.2843 0.021 Uiso 0.50 1 calc PR A 1 N3 N 0.1967(11) 0.3741(19) 0.3974(15) 0.019(3) Uani 0.50 1 d PU B 2 N4 N 0.3286(12) 0.3843(18) 0.3002(13) 0.018(2) Uani 0.50 1 d PU B 2 H4A H 0.3883 0.4066 0.2810 0.022 Uiso 0.50 1 calc PR B 2 C5 C 0.1266(10) 0.3973(19) 0.5000 0.029(3) Uani 1 2 d SU B 2 H5A H 0.1620 0.3864 0.5727 0.044 Uiso 0.50 1 calc PR B 2 H5B H 0.0755 0.3189 0.4964 0.044 Uiso 0.50 1 calc SR B 2 H5C H 0.0981 0.5014 0.4958 0.044 Uiso 0.50 1 calc SR B 2 C6 C 0.2875(13) 0.429(2) 0.3973(16) 0.016(3) Uani 0.50 1 d PU B 2 C7 C 0.2669(14) 0.298(2) 0.2326(17) 0.021(3) Uani 0.50 1 d PU B 2 H7 H 0.2792 0.2519 0.1596 0.025 Uiso 0.50 1 calc PR B 2 C8 C 0.1822(14) 0.296(2) 0.2970(16) 0.021(3) Uani 0.50 1 d PU B 2 H8 H 0.1237 0.2474 0.2744 0.025 Uiso 0.50 1 calc PR B 2 O1 O 0.4006(7) 0.2864(13) 0.0000 0.030(2) Uani 1 2 d SU C 2 O2 O 0.5000 0.5000 0.1979(11) 0.034(3) Uani 1 2 d SU D 2 C9 C 0.4544(11) 0.4013(19) 0.0000 0.030(3) Uani 1 2 d SU . 2 C10 C 0.5000 0.5000 0.0888(15) 0.028(3) Uani 1 2 d SU . 2 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 0.0121(3) 0.0146(4) 0.0136(4) 0.000 0.000 -0.0017(3) S2 0.0130(14) 0.0188(15) 0.0234(16) 0.000 0.000 0.0002(12) S1 0.0202(16) 0.0152(15) 0.0218(16) 0.000 0.000 -0.0029(12) N1 0.022(6) 0.019(5) 0.011(5) -0.001(5) 0.001(5) 0.000(5) N2 0.023(5) 0.020(5) 0.004(5) 0.004(4) -0.002(4) -0.003(5) C1 0.022(6) 0.023(7) 0.033(7) 0.000 0.000 0.000(5) C2 0.021(6) 0.016(6) 0.008(6) -0.002(5) 0.000(5) -0.001(5) C3 0.024(6) 0.023(5) 0.010(5) -0.004(5) -0.006(5) -0.005(5) C4 0.023(6) 0.021(6) 0.008(6) -0.006(5) -0.002(5) -0.002(6) N3 0.017(5) 0.022(6) 0.020(6) 0.003(5) 0.005(5) -0.003(5) N4 0.023(5) 0.022(5) 0.009(5) 0.000(4) 0.001(5) -0.002(5) C5 0.017(6) 0.025(7) 0.046(9) 0.000 0.000 -0.003(6) C6 0.017(5) 0.018(5) 0.014(5) 0.004(5) -0.002(5) -0.002(5) C7 0.024(6) 0.024(5) 0.014(5) 0.001(5) -0.004(5) -0.002(5) C8 0.022(6) 0.024(6) 0.015(6) 0.004(6) -0.001(6) -0.005(6) O1 0.019(5) 0.023(5) 0.050(7) 0.000 0.000 -0.002(4) O2 0.030(5) 0.033(6) 0.039(6) 0.000 0.000 -0.010(5) C9 0.017(6) 0.025(6) 0.047(7) 0.000 0.000 0.001(5) C10 0.018(5) 0.023(6) 0.043(7) 0.000 0.000 -0.003(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 2.314(3) 5_666 ? Pt1 S2 2.314(3) . ? Pt1 S1 2.320(4) 5_666 ? Pt1 S1 2.320(4) . ? S2 C6 1.668(19) . ? S2 C6 1.668(19) 6_556 ? S1 C2 1.734(18) . ? S1 C2 1.734(18) 6_556 ? N1 C2 1.37(2) . ? N1 C1 1.374(18) . ? N1 C4 1.39(2) . ? N2 C2 1.35(2) . ? N2 C3 1.37(2) . ? C3 C4 1.34(3) . ? N3 C6 1.35(2) . ? N3 C8 1.36(3) . ? N3 C5 1.549(18) . ? N4 C6 1.32(2) . ? N4 C7 1.38(2) . ? C7 C8 1.39(3) . ? O1 C9 1.239(19) . ? O2 C10 1.26(2) . ? C9 C10 1.477(16) . ? C9 C10 1.477(16) 5_665 ? C10 C9 1.477(16) 5_665 ? 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 180.0 5_666 . ? S2 Pt1 S1 94.13(12) 5_666 5_666 ? S2 Pt1 S1 85.87(12) . 5_666 ? S2 Pt1 S1 85.87(12) 5_666 . ? S2 Pt1 S1 94.13(12) . . ? S1 Pt1 S1 180.0 5_666 . ? C6 S2 C6 91.1(12) . 6_556 ? C6 S2 Pt1 107.8(6) . . ? C6 S2 Pt1 107.8(6) 6_556 . ? C2 S1 C2 90.6(12) . 6_556 ? C2 S1 Pt1 103.4(6) . . ? C2 S1 Pt1 103.4(6) 6_556 . ? C2 N1 C1 125.8(15) . . ? C2 N1 C4 110.3(15) . . ? C1 N1 C4 123.9(15) . . ? C2 N2 C3 109.3(15) . . ? N2 C2 N1 105.8(15) . . ? N2 C2 S1 128.0(14) . . ? N1 C2 S1 126.2(14) . . ? C4 C3 N2 109.6(16) . . ? C3 C4 N1 105.0(16) . . ? C6 N3 C8 108.2(16) . . ? C6 N3 C5 122.8(15) . . ? C8 N3 C5 128.9(15) . . ? C6 N4 C7 112.0(16) . . ? N4 C6 N3 107.5(17) . . ? N4 C6 S2 127.3(14) . . ? N3 C6 S2 125.1(15) . . ? N4 C7 C8 103.1(17) . . ? N3 C8 C7 109.1(17) . . ? O1 C9 C10 135.8(7) . . ? O1 C9 C10 135.8(7) . 5_665 ? C10 C9 C10 88.4(13) . 5_665 ? O2 C10 C9 134.2(7) . . ? O2 C10 C9 134.2(7) . 5_665 ? C9 C10 C9 91.6(13) . 5_665 ? 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 O2 0.88 1.99 2.838(17) 160.5 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.945 _refine_diff_density_min -2.243 _refine_diff_density_rms 0.235 #===END data_2006sot0115 _database_code_depnum_ccdc_archive 'CCDC 679255' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 6SOT0115 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H24 N8 Pt S4, 2(C8 H5 O4)' _chemical_formula_sum 'C32 H34 N8 O8 Pt S4' _chemical_formula_weight 982.00 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3659(2) _cell_length_b 9.7365(1) _cell_length_c 12.5373(3) _cell_angle_alpha 90.805(2) _cell_angle_beta 98.259(1) _cell_angle_gamma 113.852(2) _cell_volume 921.37(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3842 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 4.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4847 _exptl_absorpt_correction_T_max 0.6849 _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 14323 reflections reduced R(int) from 0.0546 to 0.0291 Ratio of minimum to maximum apparent transmission: 0.764599 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 14729 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4127 _reflns_number_gt 4111 _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^)+(0.0232P)^2^+1.2570P] 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 0.0093(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4127 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.3154(3) 0.5604(3) 0.20016(19) 0.0111(4) Uani 1 1 d . . . C2 C 0.2870(3) 0.4900(3) 0.3668(2) 0.0145(5) Uani 1 1 d . . . H2 H 0.2482 0.4754 0.4350 0.017 Uiso 1 1 calc R . . C3 C 0.4055(3) 0.4450(3) 0.3327(2) 0.0138(5) Uani 1 1 d . . . H3 H 0.4655 0.3924 0.3722 0.017 Uiso 1 1 calc R . . C4 C 0.5419(3) 0.4683(3) 0.1627(2) 0.0188(5) Uani 1 1 d . . . H4A H 0.4755 0.4226 0.0909 0.028 Uiso 1 1 calc R . . H4B H 0.5926 0.4018 0.1970 0.028 Uiso 1 1 calc R . . H4C H 0.6375 0.5659 0.1554 0.028 Uiso 1 1 calc R . . C5 C 0.1114(3) 0.8601(3) 0.0606(2) 0.0152(5) Uani 1 1 d . . . C6 C 0.3280(3) 1.0379(3) 0.1732(2) 0.0184(5) Uani 1 1 d . . . H6 H 0.3997 1.0935 0.2382 0.022 Uiso 1 1 calc R . . C7 C 0.3562(4) 1.0712(3) 0.0711(2) 0.0207(6) Uani 1 1 d . . . H7 H 0.4513 1.1551 0.0509 0.025 Uiso 1 1 calc R . . C8 C 0.1984(5) 0.9519(4) -0.1160(2) 0.0339(7) Uani 1 1 d . . . H8A H 0.1680 0.8483 -0.1439 0.051 Uiso 1 1 calc R . . H8B H 0.3092 1.0196 -0.1386 0.051 Uiso 1 1 calc R . . H8C H 0.1033 0.9822 -0.1445 0.051 Uiso 1 1 calc R . . C9 C 0.0870(3) 0.2854(3) 0.63796(18) 0.0112(5) Uani 1 1 d . . . C10 C 0.1299(3) 0.1499(3) 0.62837(19) 0.0112(5) Uani 1 1 d . . . C11 C 0.0009(3) 0.0056(3) 0.63387(19) 0.0120(5) Uani 1 1 d . . . H11 H -0.1150 -0.0074 0.6431 0.014 Uiso 1 1 calc R . . C12 C 0.0405(3) -0.1193(3) 0.62587(19) 0.0120(5) Uani 1 1 d . . . H12 H -0.0485 -0.2173 0.6294 0.014 Uiso 1 1 calc R . . C13 C 0.2100(3) -0.1014(3) 0.61278(19) 0.0120(5) Uani 1 1 d . . . C14 C 0.3389(3) 0.0424(3) 0.6048(2) 0.0154(5) Uani 1 1 d . . . H14 H 0.4541 0.0551 0.5943 0.018 Uiso 1 1 calc R . . C15 C 0.2985(3) 0.1672(3) 0.6124(2) 0.0140(5) Uani 1 1 d . . . H15 H 0.3863 0.2650 0.6066 0.017 Uiso 1 1 calc R . . C16 C 0.2559(3) -0.2348(3) 0.6079(2) 0.0136(5) Uani 1 1 d . . . N1 N 0.2331(3) 0.5610(2) 0.28411(17) 0.0130(4) Uani 1 1 d . . . H91 H 0.1560 0.6008 0.2861 0.016 Uiso 1 1 calc R . . N2 N 0.4227(3) 0.4899(2) 0.22949(17) 0.0124(4) Uani 1 1 d . . . N3 N 0.1754(3) 0.9081(2) 0.16448(17) 0.0145(4) Uani 1 1 d . . . H93A H 0.1270 0.8632 0.2194 0.017 Uiso 1 1 calc R . . N4 N 0.2206(3) 0.9600(3) 0.00211(18) 0.0185(5) Uani 1 1 d . . . O1 O 0.1901(2) 0.40622(19) 0.60657(14) 0.0142(4) Uani 1 1 d . . . O2 O -0.0497(2) 0.2688(2) 0.67802(15) 0.0167(4) Uani 1 1 d . . . O3 O 0.4048(2) -0.2226(2) 0.60088(17) 0.0217(4) Uani 1 1 d . . . O4 O 0.1215(2) -0.3631(2) 0.61431(17) 0.0216(4) Uani 1 1 d . . . H4 H 0.1545 -0.4338 0.6126 0.032 Uiso 1 1 calc R . . Pt1 Pt 0.0000 0.5000 0.0000 0.01197(6) Uani 1 2 d S . . S1 S 0.29613(8) 0.63750(7) 0.07771(5) 0.01354(13) Uani 1 1 d . . . S2 S -0.07973(8) 0.70237(8) 0.01109(6) 0.02067(15) 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 0.0090(10) 0.0102(12) 0.0125(11) -0.0007(9) 0.0008(9) 0.0029(9) C2 0.0153(12) 0.0125(13) 0.0139(12) 0.0018(9) 0.0025(9) 0.0038(9) C3 0.0128(11) 0.0123(13) 0.0157(12) 0.0020(9) 0.0006(9) 0.0049(9) C4 0.0181(12) 0.0238(15) 0.0199(13) -0.0001(10) 0.0060(10) 0.0133(11) C5 0.0160(12) 0.0153(13) 0.0175(13) 0.0010(9) 0.0025(10) 0.0097(10) C6 0.0180(12) 0.0139(13) 0.0201(13) -0.0012(10) 0.0026(10) 0.0034(10) C7 0.0200(13) 0.0143(14) 0.0261(15) 0.0058(10) 0.0077(11) 0.0040(10) C8 0.0441(19) 0.052(2) 0.0142(14) 0.0089(13) 0.0076(13) 0.0272(17) C9 0.0158(11) 0.0116(12) 0.0076(11) -0.0005(8) 0.0011(9) 0.0074(9) C10 0.0156(11) 0.0107(12) 0.0088(11) 0.0009(8) 0.0005(9) 0.0075(9) C11 0.0128(11) 0.0143(13) 0.0106(11) 0.0009(9) 0.0025(9) 0.0070(9) C12 0.0136(11) 0.0084(12) 0.0129(12) 0.0006(9) 0.0020(9) 0.0036(9) C13 0.0162(11) 0.0112(12) 0.0104(11) -0.0003(9) 0.0008(9) 0.0079(9) C14 0.0117(11) 0.0156(13) 0.0209(13) 0.0007(10) 0.0029(10) 0.0076(10) C15 0.0143(11) 0.0105(12) 0.0173(12) 0.0003(9) 0.0026(9) 0.0052(9) C16 0.0161(12) 0.0137(13) 0.0123(12) -0.0005(9) 0.0001(9) 0.0082(10) N1 0.0120(9) 0.0138(11) 0.0163(11) 0.0021(8) 0.0046(8) 0.0076(8) N2 0.0112(9) 0.0133(11) 0.0141(10) -0.0010(8) 0.0024(8) 0.0063(8) N3 0.0171(10) 0.0118(11) 0.0142(10) 0.0026(8) 0.0049(8) 0.0048(8) N4 0.0230(11) 0.0220(12) 0.0130(11) 0.0036(9) 0.0048(9) 0.0111(9) O1 0.0146(8) 0.0100(9) 0.0202(9) 0.0032(7) 0.0056(7) 0.0064(7) O2 0.0199(9) 0.0146(9) 0.0219(10) 0.0054(7) 0.0111(7) 0.0110(7) O3 0.0159(9) 0.0153(10) 0.0369(12) 0.0018(8) 0.0047(8) 0.0094(8) O4 0.0179(9) 0.0095(10) 0.0406(12) 0.0034(8) 0.0096(8) 0.0072(7) Pt1 0.01127(8) 0.01337(9) 0.01150(8) 0.00026(5) 0.00121(5) 0.00552(5) S1 0.0108(3) 0.0152(3) 0.0136(3) 0.0025(2) 0.0013(2) 0.0044(2) S2 0.0144(3) 0.0159(3) 0.0311(4) -0.0059(3) -0.0037(3) 0.0082(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 N1 1.339(3) . ? C1 N2 1.350(3) . ? C1 S1 1.734(2) . ? C2 C3 1.351(4) . ? C2 N1 1.376(3) . ? C2 H2 0.9500 . ? C3 N2 1.380(3) . ? C3 H3 0.9500 . ? C4 N2 1.465(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.335(3) . ? C5 N4 1.346(3) . ? C5 S2 1.733(3) . ? C6 C7 1.354(4) . ? C6 N3 1.375(3) . ? C6 H6 0.9500 . ? C7 N4 1.381(4) . ? C7 H7 0.9500 . ? C8 N4 1.463(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.254(3) . ? C9 O2 1.267(3) . ? C9 C10 1.509(3) . ? C10 C11 1.393(3) . ? C10 C15 1.395(3) . ? C11 C12 1.390(3) . ? C11 H11 0.9500 . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.395(4) . ? C13 C16 1.499(3) . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O3 1.219(3) . ? C16 O4 1.313(3) . ? N1 H91 0.8800 . ? N3 H93A 0.8800 . ? O4 H4 0.8400 . ? Pt1 S2 2.3300(6) . ? Pt1 S2 2.3300(6) 2_565 ? Pt1 S1 2.3381(6) . ? Pt1 S1 2.3381(6) 2_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 N1 C1 N2 106.6(2) . . ? N1 C1 S1 128.00(18) . . ? N2 C1 S1 125.36(18) . . ? C3 C2 N1 107.1(2) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 106.9(2) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 106.9(2) . . ? N3 C5 S2 126.3(2) . . ? N4 C5 S2 126.8(2) . . ? C7 C6 N3 106.8(2) . . ? C7 C6 H6 126.6 . . ? N3 C6 H6 126.6 . . ? C6 C7 N4 107.0(2) . . ? C6 C7 H7 126.5 . . ? N4 C7 H7 126.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 O2 125.0(2) . . ? O1 C9 C10 117.6(2) . . ? O2 C9 C10 117.5(2) . . ? C11 C10 C15 119.2(2) . . ? C11 C10 C9 120.3(2) . . ? C15 C10 C9 120.4(2) . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.7(2) . . ? C12 C13 C16 120.7(2) . . ? C14 C13 C16 119.6(2) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 120.5(2) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? O3 C16 O4 124.3(2) . . ? O3 C16 C13 122.5(2) . . ? O4 C16 C13 113.2(2) . . ? C1 N1 C2 109.9(2) . . ? C1 N1 H91 125.0 . . ? C2 N1 H91 125.0 . . ? C1 N2 C3 109.5(2) . . ? C1 N2 C4 125.0(2) . . ? C3 N2 C4 125.5(2) . . ? C5 N3 C6 110.1(2) . . ? C5 N3 H93A 125.0 . . ? C6 N3 H93A 125.0 . . ? C5 N4 C7 109.3(2) . . ? C5 N4 C8 125.2(3) . . ? C7 N4 C8 125.5(3) . . ? C16 O4 H4 109.5 . . ? S2 Pt1 S2 180.0 . 2_565 ? S2 Pt1 S1 95.03(2) . . ? S2 Pt1 S1 84.97(2) 2_565 . ? S2 Pt1 S1 84.97(2) . 2_565 ? S2 Pt1 S1 95.03(2) 2_565 2_565 ? S1 Pt1 S1 180.0 . 2_565 ? C1 S1 Pt1 103.81(8) . . ? C5 S2 Pt1 107.21(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 N1 H91 O2 0.88 1.90 2.751(3) 161.9 2_566 N3 H93A O2 0.88 1.83 2.683(3) 163.8 2_566 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.653 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.103 #===END data_2006sot0116 _database_code_depnum_ccdc_archive 'CCDC 679256' _chemical_compound_source 'Roberto Quesada' _database_code_CSD 6SOT0116 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 N8 O8 Pt S4' _chemical_formula_weight 1082.11 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 9.5580(2) _cell_length_b 9.9340(2) _cell_length_c 11.1590(2) _cell_angle_alpha 80.721(1) _cell_angle_beta 78.108(1) _cell_angle_gamma 86.762(1) _cell_volume 1022.93(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4454 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour 'Pale Orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 3.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.8662 _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 15000 reflections reduced R(int) from 0.2756 to 0.0579 Ratio of minimum to maximum apparent transmission: 0.716868 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _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 15800 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4675 _reflns_number_gt 4546 _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^+1.2089P] 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 4675 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.029 _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 1.0000 0.0000 0.01286(6) Uani 1 2 d S . . S1 S 0.56992(8) 0.86305(8) 0.16678(7) 0.01899(17) Uani 1 1 d . . . S2 S 0.27751(7) 1.05863(8) 0.11122(7) 0.01587(16) Uani 1 1 d . . . N1 N 0.4539(3) 1.0250(3) 0.3403(2) 0.0165(5) Uani 1 1 d . . . H1 H 0.5142 1.0915 0.3098 0.020 Uiso 1 1 calc R . . N2 N 0.3478(3) 0.8334(3) 0.3685(2) 0.0167(5) Uani 1 1 d . . . N3 N 0.1906(3) 0.8460(3) 0.0136(2) 0.0169(5) Uani 1 1 d . . . H3 H 0.2720 0.8346 -0.0378 0.020 Uiso 1 1 calc R . . N4 N 0.0288(2) 0.9239(3) 0.1526(2) 0.0161(5) Uani 1 1 d . . . C1 C 0.4537(3) 0.9087(3) 0.2947(3) 0.0160(6) Uani 1 1 d . . . C2 C 0.3447(3) 1.0243(3) 0.4424(3) 0.0204(7) Uani 1 1 d . . . H2 H 0.3205 1.0959 0.4906 0.025 Uiso 1 1 calc R . . C3 C 0.2786(3) 0.9050(3) 0.4618(3) 0.0203(7) Uani 1 1 d . . . H3A H 0.2002 0.8753 0.5265 0.024 Uiso 1 1 calc R . . C4 C 0.3018(4) 0.7023(3) 0.3489(3) 0.0227(7) Uani 1 1 d . . . H4A H 0.2157 0.7162 0.3132 0.034 Uiso 1 1 calc R . . H4B H 0.2808 0.6413 0.4283 0.034 Uiso 1 1 calc R . . H4C H 0.3782 0.6613 0.2919 0.034 Uiso 1 1 calc R . . C5 C 0.1654(3) 0.9392(3) 0.0908(3) 0.0145(6) Uani 1 1 d . . . C6 C 0.0699(3) 0.7705(3) 0.0270(3) 0.0212(7) Uani 1 1 d . . . H6 H 0.0602 0.6980 -0.0165 0.025 Uiso 1 1 calc R . . C7 C -0.0307(3) 0.8189(3) 0.1128(3) 0.0214(7) Uani 1 1 d . . . H7 H -0.1256 0.7873 0.1413 0.026 Uiso 1 1 calc R . . C8 C -0.0421(3) 1.0023(4) 0.2486(3) 0.0252(7) Uani 1 1 d . . . H8A H -0.0318 0.9534 0.3301 0.038 Uiso 1 1 calc R . . H8B H -0.1438 1.0145 0.2456 0.038 Uiso 1 1 calc R . . H8C H 0.0017 1.0918 0.2348 0.038 Uiso 1 1 calc R . . O1 O -0.0753(2) 0.4560(2) 0.16786(19) 0.0178(5) Uani 1 1 d . . . H1A H -0.1639 0.4471 0.1769 0.027 Uiso 1 1 calc R . . O2 O -0.1095(2) 0.3247(2) 0.3530(2) 0.0223(5) Uani 1 1 d . . . O3 O 0.6619(2) 0.4544(2) 0.1701(2) 0.0247(5) Uani 1 1 d . . . O4 O 0.6360(2) 0.2278(2) 0.2061(2) 0.0194(5) Uani 1 1 d . . . C9 C -0.0302(3) 0.3864(3) 0.2644(3) 0.0145(6) Uani 1 1 d . . . C10 C 0.1288(3) 0.3879(3) 0.2509(3) 0.0131(6) Uani 1 1 d . . . C11 C 0.1949(3) 0.3699(3) 0.3571(3) 0.0142(6) Uani 1 1 d . . . C12 C 0.1180(3) 0.3632(3) 0.4808(3) 0.0170(6) Uani 1 1 d . . . H12 H 0.0165 0.3619 0.4972 0.020 Uiso 1 1 calc R . . C13 C 0.1877(3) 0.3586(3) 0.5768(3) 0.0199(7) Uani 1 1 d . . . H13 H 0.1336 0.3559 0.6587 0.024 Uiso 1 1 calc R . . C14 C 0.3375(3) 0.3578(3) 0.5569(3) 0.0202(7) Uani 1 1 d . . . H14 H 0.3841 0.3565 0.6245 0.024 Uiso 1 1 calc R . . C15 C 0.4160(3) 0.3590(3) 0.4399(3) 0.0177(6) Uani 1 1 d . . . H15 H 0.5175 0.3556 0.4270 0.021 Uiso 1 1 calc R . . C16 C 0.3478(3) 0.3652(3) 0.3368(3) 0.0136(6) Uani 1 1 d . . . C17 C 0.4287(3) 0.3700(3) 0.2141(3) 0.0142(6) Uani 1 1 d . . . C18 C 0.3624(3) 0.3892(3) 0.1145(3) 0.0162(6) Uani 1 1 d . . . H18 H 0.4175 0.3945 0.0328 0.019 Uiso 1 1 calc R . . C19 C 0.2119(3) 0.4012(3) 0.1343(3) 0.0156(6) Uani 1 1 d . . . H19 H 0.1671 0.4191 0.0647 0.019 Uiso 1 1 calc R . . C20 C 0.5887(3) 0.3493(3) 0.1953(3) 0.0154(6) 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 0.00991(8) 0.01384(9) 0.01409(10) -0.00155(6) -0.00085(6) -0.00154(6) S1 0.0170(3) 0.0209(4) 0.0161(4) 0.0009(3) -0.0008(3) 0.0048(3) S2 0.0116(3) 0.0172(4) 0.0186(4) -0.0048(3) -0.0006(3) -0.0014(3) N1 0.0183(12) 0.0158(13) 0.0142(13) 0.0011(10) -0.0018(11) -0.0053(10) N2 0.0201(12) 0.0142(13) 0.0132(13) 0.0006(10) 0.0012(11) -0.0020(10) N3 0.0115(11) 0.0178(14) 0.0205(14) -0.0074(11) 0.0027(10) -0.0017(10) N4 0.0123(11) 0.0188(14) 0.0155(13) -0.0010(11) -0.0002(10) -0.0015(10) C1 0.0148(14) 0.0179(16) 0.0139(15) 0.0038(12) -0.0044(12) -0.0015(12) C2 0.0281(16) 0.0170(16) 0.0145(16) -0.0020(13) -0.0007(13) -0.0011(13) C3 0.0234(15) 0.0175(16) 0.0158(16) 0.0006(13) 0.0032(13) -0.0012(13) C4 0.0273(16) 0.0132(16) 0.0267(18) -0.0026(14) -0.0030(14) -0.0042(13) C5 0.0118(13) 0.0157(15) 0.0146(15) -0.0005(12) -0.0015(12) 0.0009(11) C6 0.0204(15) 0.0210(17) 0.0231(17) -0.0023(14) -0.0056(14) -0.0054(13) C7 0.0172(14) 0.0226(17) 0.0236(17) 0.0021(14) -0.0047(13) -0.0072(13) C8 0.0189(15) 0.031(2) 0.0219(18) -0.0077(15) 0.0079(14) -0.0004(14) O1 0.0096(9) 0.0217(12) 0.0217(12) 0.0000(9) -0.0041(9) -0.0040(9) O2 0.0163(10) 0.0246(13) 0.0227(12) 0.0014(10) 0.0013(9) -0.0070(9) O3 0.0136(10) 0.0187(12) 0.0400(14) 0.0069(10) -0.0090(10) -0.0050(9) O4 0.0134(10) 0.0166(12) 0.0275(12) -0.0038(9) -0.0020(9) -0.0001(8) C9 0.0130(13) 0.0121(15) 0.0181(16) -0.0028(12) -0.0017(12) -0.0016(11) C10 0.0113(13) 0.0117(14) 0.0157(15) -0.0020(12) -0.0013(12) -0.0014(11) C11 0.0132(13) 0.0103(14) 0.0177(15) -0.0010(12) -0.0002(12) -0.0016(11) C12 0.0182(14) 0.0125(15) 0.0185(16) -0.0021(12) 0.0003(13) 0.0000(12) C13 0.0277(16) 0.0158(16) 0.0142(16) -0.0010(13) -0.0014(13) 0.0016(13) C14 0.0299(17) 0.0140(16) 0.0193(17) -0.0028(13) -0.0116(14) 0.0025(13) C15 0.0193(14) 0.0123(15) 0.0219(17) 0.0009(13) -0.0077(13) -0.0011(12) C16 0.0147(13) 0.0100(14) 0.0166(15) -0.0017(12) -0.0038(12) -0.0019(11) C17 0.0126(13) 0.0095(14) 0.0207(16) -0.0012(12) -0.0043(12) -0.0024(11) C18 0.0142(13) 0.0167(16) 0.0162(16) -0.0002(12) -0.0006(12) -0.0041(12) C19 0.0141(13) 0.0161(16) 0.0176(16) -0.0010(12) -0.0058(12) -0.0030(11) C20 0.0131(13) 0.0214(17) 0.0121(15) -0.0013(12) -0.0042(12) -0.0022(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S1 2.3140(8) 2_675 ? Pt1 S1 2.3140(8) . ? Pt1 S2 2.3254(7) 2_675 ? Pt1 S2 2.3254(7) . ? S1 C1 1.725(3) . ? S2 C5 1.715(3) . ? N1 C1 1.335(4) . ? N1 C2 1.376(4) . ? N2 C1 1.343(4) . ? N2 C3 1.389(4) . ? N2 C4 1.461(4) . ? N3 C5 1.343(4) . ? N3 C6 1.380(4) . ? N4 C5 1.349(4) . ? N4 C7 1.389(4) . ? N4 C8 1.458(4) . ? C2 C3 1.341(4) . ? C6 C7 1.338(5) . ? O1 C9 1.319(4) . ? O2 C9 1.215(3) . ? O3 C20 1.251(4) . ? O4 C20 1.260(4) . ? C9 C10 1.497(4) . ? C10 C19 1.368(4) . ? C10 C11 1.437(4) . ? C11 C12 1.416(4) . ? C11 C16 1.432(4) . ? C12 C13 1.368(4) . ? C13 C14 1.403(4) . ? C14 C15 1.363(4) . ? C15 C16 1.427(4) . ? C16 C17 1.422(4) . ? C17 C18 1.370(4) . ? C17 C20 1.507(4) . ? C18 C19 1.411(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 S1 Pt1 S1 180.0 2_675 . ? S1 Pt1 S2 94.91(3) 2_675 2_675 ? S1 Pt1 S2 85.09(3) . 2_675 ? S1 Pt1 S2 85.09(3) 2_675 . ? S1 Pt1 S2 94.91(3) . . ? S2 Pt1 S2 180.0 2_675 . ? C1 S1 Pt1 104.42(10) . . ? C5 S2 Pt1 104.22(10) . . ? C1 N1 C2 109.2(2) . . ? C1 N2 C3 109.5(3) . . ? C1 N2 C4 126.1(3) . . ? C3 N2 C4 124.2(3) . . ? C5 N3 C6 109.9(2) . . ? C5 N4 C7 109.0(3) . . ? C5 N4 C8 125.1(3) . . ? C7 N4 C8 125.9(3) . . ? N1 C1 N2 107.1(3) . . ? N1 C1 S1 126.3(2) . . ? N2 C1 S1 126.6(2) . . ? C3 C2 N1 108.0(3) . . ? C2 C3 N2 106.2(3) . . ? N3 C5 N4 106.6(2) . . ? N3 C5 S2 129.2(2) . . ? N4 C5 S2 124.2(2) . . ? C7 C6 N3 107.0(3) . . ? C6 C7 N4 107.5(3) . . ? O2 C9 O1 123.3(3) . . ? O2 C9 C10 123.8(3) . . ? O1 C9 C10 112.8(2) . . ? C19 C10 C11 119.9(3) . . ? C19 C10 C9 118.6(3) . . ? C11 C10 C9 121.4(3) . . ? C12 C11 C16 117.8(3) . . ? C12 C11 C10 124.0(3) . . ? C16 C11 C10 118.1(3) . . ? C13 C12 C11 121.0(3) . . ? C12 C13 C14 121.4(3) . . ? C15 C14 C13 119.7(3) . . ? C14 C15 C16 120.9(3) . . ? C17 C16 C15 121.3(3) . . ? C17 C16 C11 119.4(3) . . ? C15 C16 C11 119.2(3) . . ? C18 C17 C16 120.8(3) . . ? C18 C17 C20 120.3(3) . . ? C16 C17 C20 118.8(3) . . ? C17 C18 C19 119.6(3) . . ? C10 C19 C18 121.8(3) . . ? O3 C20 O4 126.2(3) . . ? O3 C20 C17 116.9(3) . . ? O4 C20 C17 116.9(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 N1 H1 O4 0.88 1.91 2.771(3) 166.0 1_565 N3 H3 O4 0.88 2.08 2.840(3) 144.3 2_665 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.074 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.152 #===END