# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2012 data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_cambridge 1326 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Qin-Yu Zhu' _publ_contact_author_email zhuqinyu@suda.edu.cn _publ_author_name 'Qin-Yu Zhu' data_Hpy_HL _database_code_depnum_ccdc_archive 'CCDC 881721' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 N O4 S6' _chemical_formula_weight 463.62 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6319(8) _cell_length_b 10.0114(9) _cell_length_c 22.265(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.953(2) _cell_angle_gamma 90.00 _cell_volume 1910.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8326 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13330 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4341 _reflns_number_gt 3839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.5108P] 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 0.0117(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4341 _refine_ls_number_parameters 247 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _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 S1 S 0.17538(6) 0.10773(5) 0.51623(2) 0.03294(14) Uani 1 1 d . . . S2 S 0.10948(6) -0.04721(5) 0.62350(2) 0.03452(15) Uani 1 1 d . . . S3 S -0.00712(6) 0.36221(5) 0.56317(2) 0.03485(15) Uani 1 1 d . . . S4 S -0.08317(7) 0.20488(5) 0.66822(2) 0.03649(15) Uani 1 1 d . . . S5 S -0.11200(7) 0.62162(5) 0.61078(3) 0.03946(15) Uani 1 1 d . . . S6 S -0.21918(7) 0.44403(6) 0.72605(3) 0.04219(16) Uani 1 1 d . . . C1 C 0.2498(2) -0.05407(19) 0.52358(8) 0.0290(4) Uani 1 1 d . . . C2 C 0.2205(2) -0.1257(2) 0.57277(8) 0.0289(4) Uani 1 1 d . . . C3 C 0.0878(2) 0.1037(2) 0.58337(8) 0.0296(4) Uani 1 1 d . . . C4 C 0.0102(2) 0.20918(19) 0.60220(8) 0.0299(4) Uani 1 1 d . . . C5 C -0.0826(2) 0.4494(2) 0.62151(9) 0.0317(4) Uani 1 1 d . . . C6 C -0.1193(2) 0.3776(2) 0.66920(9) 0.0307(4) Uani 1 1 d . . . C7 C -0.3112(3) 0.6246(3) 0.57808(16) 0.0672(8) Uani 1 1 d . . . H7A H -0.3231 0.5713 0.5414 0.101 Uiso 1 1 calc R . . H7B H -0.3423 0.7159 0.5684 0.101 Uiso 1 1 calc R . . H7C H -0.3764 0.5881 0.6066 0.101 Uiso 1 1 calc R . . C8 C -0.1627(4) 0.3359(3) 0.78951(11) 0.0596(8) Uani 1 1 d . . . H8A H -0.2105 0.2489 0.7819 0.089 Uiso 1 1 calc R . . H8B H -0.1971 0.3742 0.8257 0.089 Uiso 1 1 calc R . . H8C H -0.0500 0.3264 0.7952 0.089 Uiso 1 1 calc R . . C9 C 0.3379(2) -0.0921(2) 0.47166(9) 0.0336(4) Uani 1 1 d . . . C10 C 0.2712(2) -0.2621(2) 0.59380(9) 0.0336(4) Uani 1 1 d . . . C11 C 0.4701(3) 0.1649(2) 0.66861(11) 0.0452(5) Uani 1 1 d . . . H11 H 0.5229 0.0845 0.6634 0.054 Uiso 1 1 calc R . . C12 C 0.4010(3) 0.1860(3) 0.71982(11) 0.0490(6) Uani 1 1 d . . . H12 H 0.4063 0.1204 0.7502 0.059 Uiso 1 1 calc R . . C13 C 0.3237(3) 0.3037(3) 0.72651(10) 0.0450(6) Uani 1 1 d . . . H13 H 0.2750 0.3189 0.7614 0.054 Uiso 1 1 calc R . . C14 C 0.3176(3) 0.3990(2) 0.68213(11) 0.0445(5) Uani 1 1 d . . . H14 H 0.2654 0.4803 0.6864 0.053 Uiso 1 1 calc R . . C15 C 0.3887(3) 0.3743(2) 0.63147(10) 0.0395(5) Uani 1 1 d . . . H15 H 0.3856 0.4386 0.6006 0.047 Uiso 1 1 calc R . . O1 O 0.35849(19) -0.00455(16) 0.43476(7) 0.0432(4) Uani 1 1 d . . . O2 O 0.38500(19) -0.21349(16) 0.46922(7) 0.0430(4) Uani 1 1 d . . . O3 O 0.2537(2) -0.29431(16) 0.64539(7) 0.0481(4) Uani 1 1 d . . . O4 O 0.33085(19) -0.34254(16) 0.55719(7) 0.0419(4) Uani 1 1 d D . . N1 N 0.4621(2) 0.2590(2) 0.62626(8) 0.0366(4) Uani 1 1 d D . . H1 H 0.508(3) 0.247(3) 0.5937(10) 0.061(8) Uiso 1 1 d D . . H4 H 0.353(4) -0.300(3) 0.5263(11) 0.074(10) 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 S1 0.0432(3) 0.0297(3) 0.0277(3) 0.00194(19) 0.0113(2) 0.0019(2) S2 0.0491(3) 0.0295(3) 0.0273(3) 0.00259(19) 0.0138(2) 0.0050(2) S3 0.0450(3) 0.0312(3) 0.0299(3) 0.0027(2) 0.0108(2) 0.0048(2) S4 0.0502(3) 0.0287(3) 0.0336(3) 0.0007(2) 0.0174(2) 0.0020(2) S5 0.0448(3) 0.0275(3) 0.0475(3) 0.0020(2) 0.0117(2) 0.0020(2) S6 0.0502(3) 0.0404(3) 0.0387(3) -0.0068(2) 0.0170(2) 0.0040(2) C1 0.0302(9) 0.0304(10) 0.0267(9) -0.0021(8) 0.0049(7) 0.0007(8) C2 0.0282(9) 0.0326(10) 0.0260(9) -0.0017(8) 0.0038(7) 0.0024(8) C3 0.0350(10) 0.0280(10) 0.0265(9) 0.0001(8) 0.0065(7) -0.0002(8) C4 0.0357(10) 0.0283(10) 0.0265(9) 0.0008(8) 0.0063(7) 0.0003(8) C5 0.0325(10) 0.0282(10) 0.0347(10) -0.0015(8) 0.0055(8) 0.0018(8) C6 0.0336(10) 0.0290(10) 0.0300(10) -0.0027(8) 0.0061(7) 0.0006(8) C7 0.0485(15) 0.0535(17) 0.097(2) 0.0263(16) -0.0025(15) 0.0041(13) C8 0.101(2) 0.0418(14) 0.0414(13) 0.0009(11) 0.0317(14) -0.0021(14) C9 0.0329(10) 0.0412(12) 0.0274(9) -0.0012(9) 0.0073(8) 0.0015(9) C10 0.0340(10) 0.0345(11) 0.0324(10) 0.0020(9) 0.0043(8) 0.0051(8) C11 0.0529(14) 0.0388(13) 0.0451(13) 0.0057(10) 0.0112(10) 0.0091(11) C12 0.0576(14) 0.0536(15) 0.0371(12) 0.0168(11) 0.0107(10) 0.0035(12) C13 0.0470(12) 0.0603(16) 0.0295(11) -0.0089(10) 0.0128(9) -0.0041(11) C14 0.0456(13) 0.0400(13) 0.0491(13) -0.0059(10) 0.0108(10) 0.0066(10) C15 0.0413(12) 0.0398(12) 0.0377(11) 0.0094(9) 0.0061(9) 0.0013(9) O1 0.0550(9) 0.0420(9) 0.0358(8) 0.0021(7) 0.0190(7) 0.0005(7) O2 0.0498(9) 0.0418(9) 0.0411(8) 0.0003(7) 0.0204(7) 0.0093(7) O3 0.0690(11) 0.0427(9) 0.0341(8) 0.0088(7) 0.0118(7) 0.0142(8) O4 0.0520(9) 0.0371(9) 0.0388(8) 0.0061(7) 0.0145(7) 0.0155(7) N1 0.0379(9) 0.0446(11) 0.0286(9) -0.0011(8) 0.0100(7) 0.0009(8) _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 S1 C1 1.743(2) . ? S1 C3 1.7554(19) . ? S2 C3 1.753(2) . ? S2 C2 1.7532(19) . ? S3 C5 1.755(2) . ? S3 C4 1.759(2) . ? S4 C6 1.758(2) . ? S4 C4 1.7606(19) . ? S5 C5 1.755(2) . ? S5 C7 1.784(3) . ? S6 C6 1.747(2) . ? S6 C8 1.800(3) . ? C1 C2 1.358(3) . ? C1 C9 1.507(3) . ? C2 C10 1.492(3) . ? C3 C4 1.344(3) . ? C5 C6 1.351(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 O1 1.229(3) . ? C9 O2 1.285(3) . ? C10 O3 1.220(3) . ? C10 O4 1.297(3) . ? C11 N1 1.329(3) . ? C11 C12 1.366(3) . ? C11 H11 0.9400 . ? C12 C13 1.371(4) . ? C12 H12 0.9400 . ? C13 C14 1.370(4) . ? C13 H13 0.9400 . ? C14 C15 1.370(3) . ? C14 H14 0.9400 . ? C15 N1 1.328(3) . ? C15 H15 0.9400 . ? O4 H4 0.852(18) . ? N1 H1 0.873(17) . ? 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 C1 S1 C3 95.19(9) . . ? C3 S2 C2 95.21(9) . . ? C5 S3 C4 94.84(9) . . ? C6 S4 C4 94.94(9) . . ? C5 S5 C7 100.83(12) . . ? C6 S6 C8 103.26(11) . . ? C2 C1 C9 130.22(19) . . ? C2 C1 S1 117.63(15) . . ? C9 C1 S1 112.15(14) . . ? C1 C2 C10 131.33(18) . . ? C1 C2 S2 116.92(15) . . ? C10 C2 S2 111.72(14) . . ? C4 C3 S2 122.99(15) . . ? C4 C3 S1 121.96(15) . . ? S2 C3 S1 115.05(11) . . ? C3 C4 S3 123.11(15) . . ? C3 C4 S4 122.46(15) . . ? S3 C4 S4 114.43(11) . . ? C6 C5 S3 117.44(16) . . ? C6 C5 S5 125.86(16) . . ? S3 C5 S5 116.63(11) . . ? C5 C6 S6 123.38(16) . . ? C5 C6 S4 117.05(15) . . ? S6 C6 S4 119.15(11) . . ? S5 C7 H7A 109.5 . . ? S5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S6 C8 H8A 109.5 . . ? S6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 O2 125.03(19) . . ? O1 C9 C1 117.40(19) . . ? O2 C9 C1 117.56(18) . . ? O3 C10 O4 122.1(2) . . ? O3 C10 C2 118.23(18) . . ? O4 C10 C2 119.68(18) . . ? N1 C11 C12 119.5(2) . . ? N1 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 119.4(2) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.1(2) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N1 C15 C14 119.6(2) . . ? N1 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C10 O4 H4 110(2) . . ? C15 N1 C11 122.56(19) . . ? C15 N1 H1 117(2) . . ? C11 N1 H1 120(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 S1 C1 C2 0.26(17) . . . . ? C3 S1 C1 C9 179.70(14) . . . . ? C9 C1 C2 C10 3.4(4) . . . . ? S1 C1 C2 C10 -177.23(17) . . . . ? C9 C1 C2 S2 -178.96(16) . . . . ? S1 C1 C2 S2 0.4(2) . . . . ? C3 S2 C2 C1 -0.78(17) . . . . ? C3 S2 C2 C10 177.27(14) . . . . ? C2 S2 C3 C4 -178.98(18) . . . . ? C2 S2 C3 S1 0.94(13) . . . . ? C1 S1 C3 C4 179.13(18) . . . . ? C1 S1 C3 S2 -0.79(13) . . . . ? S2 C3 C4 S3 178.17(11) . . . . ? S1 C3 C4 S3 -1.7(3) . . . . ? S2 C3 C4 S4 -2.0(3) . . . . ? S1 C3 C4 S4 178.05(11) . . . . ? C5 S3 C4 C3 -168.90(18) . . . . ? C5 S3 C4 S4 11.29(13) . . . . ? C6 S4 C4 C3 169.42(18) . . . . ? C6 S4 C4 S3 -10.76(13) . . . . ? C4 S3 C5 C6 -7.64(18) . . . . ? C4 S3 C5 S5 175.18(12) . . . . ? C7 S5 C5 C6 -83.8(2) . . . . ? C7 S5 C5 S3 93.13(16) . . . . ? S3 C5 C6 S6 -171.17(11) . . . . ? S5 C5 C6 S6 5.7(3) . . . . ? S3 C5 C6 S4 1.3(2) . . . . ? S5 C5 C6 S4 178.21(11) . . . . ? C8 S6 C6 C5 -156.2(2) . . . . ? C8 S6 C6 S4 31.43(16) . . . . ? C4 S4 C6 C5 5.74(18) . . . . ? C4 S4 C6 S6 178.57(12) . . . . ? C2 C1 C9 O1 -174.4(2) . . . . ? S1 C1 C9 O1 6.3(2) . . . . ? C2 C1 C9 O2 6.0(3) . . . . ? S1 C1 C9 O2 -173.40(15) . . . . ? C1 C2 C10 O3 166.4(2) . . . . ? S2 C2 C10 O3 -11.3(3) . . . . ? C1 C2 C10 O4 -14.1(3) . . . . ? S2 C2 C10 O4 168.23(16) . . . . ? N1 C11 C12 C13 0.4(4) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C12 C13 C14 C15 0.4(4) . . . . ? C13 C14 C15 N1 -0.1(3) . . . . ? C14 C15 N1 C11 -0.1(3) . . . . ? C12 C11 N1 C15 -0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.427 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.115 ########End data_H(2,2_bpy)_HL _database_code_depnum_ccdc_archive 'CCDC 881722' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 O4 S6, C10 H9 N2' _chemical_formula_sum 'C20 H16 N2 O4 S6' _chemical_formula_weight 540.71 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_space_group_name_Hall '-P 2yab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.140(3) _cell_length_b 7.7891(12) _cell_length_c 17.338(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.363(4) _cell_angle_gamma 90.00 _cell_volume 2261.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10050 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Platelet _exptl_crystal_colour Red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12347 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5117 _reflns_number_gt 4038 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.5549P] 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 5117 _refine_ls_number_parameters 298 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 S2 S 0.47881(6) 0.44802(15) 0.23699(6) 0.0382(3) Uani 1 1 d . . . S1 S 0.32105(6) 0.56438(15) 0.26005(6) 0.0386(3) Uani 1 1 d . . . S3 S 0.26939(7) 0.68385(16) 0.08375(6) 0.0439(3) Uani 1 1 d . . . S4 S 0.42333(6) 0.58050(15) 0.04850(6) 0.0404(3) Uani 1 1 d . . . S5 S 0.18315(7) 0.67567(16) -0.08675(7) 0.0487(3) Uani 1 1 d . . . S6 S 0.35677(7) 0.55018(16) -0.12654(6) 0.0470(3) Uani 1 1 d . . . O4 O 0.50946(17) 0.2741(4) 0.45243(17) 0.0497(8) Uani 1 1 d . . . O3 O 0.58453(16) 0.2902(4) 0.36218(17) 0.0465(8) Uani 1 1 d . . . O1 O 0.27798(18) 0.5140(5) 0.40080(18) 0.0582(9) Uani 1 1 d . . . O2 O 0.37953(19) 0.3690(5) 0.47151(18) 0.0515(8) Uani 1 1 d D . . N1 N 0.61389(19) 0.0950(5) 0.5673(2) 0.0356(8) Uani 1 1 d D . . N2 N 0.47661(19) 0.1373(5) 0.6144(2) 0.0411(9) Uani 1 1 d . . . C6 C 0.3397(3) 0.5894(5) -0.0317(2) 0.0377(9) Uani 1 1 d . . . C7 C 0.1054(3) 0.6033(7) -0.0386(3) 0.0599(13) Uani 1 1 d . . . H7A H 0.0537 0.6198 -0.0738 0.090 Uiso 1 1 calc R . . H7B H 0.1076 0.6690 0.0094 0.090 Uiso 1 1 calc R . . H7C H 0.1130 0.4825 -0.0256 0.090 Uiso 1 1 calc R . . C2 C 0.4554(2) 0.4063(5) 0.3288(2) 0.0322(8) Uani 1 1 d . . . C3 C 0.3864(2) 0.5432(5) 0.1955(2) 0.0311(8) Uani 1 1 d . . . C14 C 0.6809(2) -0.0288(6) 0.6853(2) 0.0425(10) Uani 1 1 d . . . H14A H 0.6828 -0.0635 0.7376 0.051 Uiso 1 1 calc R . . C12 C 0.7440(2) -0.0039(6) 0.5750(2) 0.0418(10) Uani 1 1 d . . . H12A H 0.7883 -0.0213 0.5520 0.050 Uiso 1 1 calc R . . C15 C 0.6133(2) 0.0482(5) 0.6419(2) 0.0337(9) Uani 1 1 d . . . C1 C 0.3833(2) 0.4591(5) 0.3391(2) 0.0332(9) Uani 1 1 d . . . C5 C 0.2694(2) 0.6355(5) -0.0150(2) 0.0370(9) Uani 1 1 d . . . C4 C 0.3647(2) 0.5960(5) 0.1205(2) 0.0357(9) Uani 1 1 d . . . C10 C 0.5226(2) 0.3181(6) 0.3851(2) 0.0386(9) Uani 1 1 d . . . C9 C 0.3436(3) 0.4487(6) 0.4083(2) 0.0427(10) Uani 1 1 d . . . C11 C 0.6767(2) 0.0720(6) 0.5333(2) 0.0402(10) Uani 1 1 d . . . H11A H 0.6740 0.1081 0.4811 0.048 Uiso 1 1 calc R . . C19 C 0.5363(3) 0.0697(6) 0.7491(2) 0.0410(10) Uani 1 1 d . . . H19A H 0.5815 0.0346 0.7867 0.049 Uiso 1 1 calc R . . C20 C 0.5390(2) 0.0852(5) 0.6702(2) 0.0362(9) Uani 1 1 d . . . C16 C 0.4089(2) 0.1702(6) 0.6376(3) 0.0465(11) Uani 1 1 d . . . H16A H 0.3643 0.2046 0.5991 0.056 Uiso 1 1 calc R . . C17 C 0.4002(3) 0.1569(6) 0.7146(3) 0.0481(11) Uani 1 1 d . . . H17A H 0.3510 0.1812 0.7280 0.058 Uiso 1 1 calc R . . C8 C 0.3652(3) 0.7655(7) -0.1600(3) 0.0573(13) Uani 1 1 d . . . H8A H 0.3752 0.7633 -0.2130 0.086 Uiso 1 1 calc R . . H8B H 0.4092 0.8229 -0.1249 0.086 Uiso 1 1 calc R . . H8C H 0.3160 0.8270 -0.1603 0.086 Uiso 1 1 calc R . . C13 C 0.7462(3) -0.0547(6) 0.6515(3) 0.0471(11) Uani 1 1 d . . . H13A H 0.7923 -0.1075 0.6811 0.056 Uiso 1 1 calc R . . C18 C 0.4652(3) 0.1074(6) 0.7712(3) 0.0478(11) Uani 1 1 d . . . H18A H 0.4614 0.0991 0.8243 0.057 Uiso 1 1 calc R . . H1A H 0.5701(15) 0.139(5) 0.540(2) 0.032(11) Uiso 1 1 d D . . H2A H 0.4254(14) 0.340(7) 0.468(3) 0.075(19) 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 S2 0.0340(5) 0.0505(6) 0.0315(5) 0.0067(5) 0.0098(4) 0.0038(5) S1 0.0348(5) 0.0502(6) 0.0305(5) 0.0023(5) 0.0060(4) 0.0058(5) S3 0.0469(6) 0.0530(7) 0.0301(5) 0.0005(5) 0.0048(4) 0.0133(5) S4 0.0404(6) 0.0510(7) 0.0296(5) 0.0041(5) 0.0068(4) 0.0021(5) S5 0.0479(6) 0.0559(7) 0.0371(6) 0.0035(5) -0.0024(5) 0.0098(6) S6 0.0619(7) 0.0505(7) 0.0293(6) 0.0020(5) 0.0116(5) 0.0046(6) O4 0.0442(17) 0.073(2) 0.0327(16) 0.0201(15) 0.0096(13) 0.0109(16) O3 0.0313(15) 0.062(2) 0.0464(18) 0.0116(15) 0.0095(13) 0.0039(15) O1 0.0419(18) 0.091(3) 0.0456(19) 0.0134(18) 0.0178(15) 0.0210(18) O2 0.0413(18) 0.081(2) 0.0353(17) 0.0129(16) 0.0142(14) 0.0122(18) N1 0.0286(17) 0.046(2) 0.0305(18) 0.0036(15) 0.0030(14) 0.0028(16) N2 0.0327(18) 0.056(2) 0.0348(19) 0.0038(17) 0.0072(15) 0.0024(17) C6 0.047(2) 0.038(2) 0.028(2) 0.0022(17) 0.0077(17) 0.003(2) C7 0.046(3) 0.065(3) 0.065(3) -0.002(3) 0.003(2) 0.000(3) C2 0.0322(19) 0.038(2) 0.0260(19) -0.0003(17) 0.0062(15) -0.0033(18) C3 0.0303(19) 0.034(2) 0.027(2) -0.0019(16) 0.0033(15) -0.0002(17) C14 0.040(2) 0.056(3) 0.031(2) 0.006(2) 0.0064(18) -0.001(2) C12 0.034(2) 0.055(3) 0.038(2) 0.002(2) 0.0119(18) 0.002(2) C15 0.033(2) 0.040(2) 0.028(2) 0.0025(17) 0.0068(16) -0.0036(18) C1 0.034(2) 0.040(2) 0.026(2) -0.0001(17) 0.0070(16) -0.0040(18) C5 0.044(2) 0.036(2) 0.029(2) 0.0038(17) 0.0045(17) 0.0019(19) C4 0.039(2) 0.041(2) 0.026(2) 0.0029(17) 0.0039(16) 0.0013(19) C10 0.036(2) 0.043(2) 0.035(2) 0.0037(19) 0.0033(17) -0.0013(19) C9 0.040(2) 0.057(3) 0.032(2) -0.002(2) 0.0097(18) -0.004(2) C11 0.039(2) 0.052(3) 0.030(2) 0.0032(19) 0.0071(17) -0.002(2) C19 0.041(2) 0.047(3) 0.034(2) 0.0041(19) 0.0067(18) -0.002(2) C20 0.035(2) 0.038(2) 0.035(2) -0.0012(18) 0.0062(17) -0.0053(18) C16 0.031(2) 0.058(3) 0.048(3) 0.007(2) 0.0055(19) 0.003(2) C17 0.040(2) 0.057(3) 0.052(3) 0.002(2) 0.019(2) 0.000(2) C8 0.067(3) 0.063(3) 0.047(3) 0.012(2) 0.021(2) 0.000(3) C13 0.038(2) 0.063(3) 0.038(2) 0.006(2) 0.0055(19) 0.008(2) C18 0.050(3) 0.058(3) 0.039(3) 0.002(2) 0.018(2) -0.002(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 S2 C2 1.753(4) . ? S2 C3 1.757(4) . ? S1 C1 1.750(4) . ? S1 C3 1.752(4) . ? S3 C5 1.754(4) . ? S3 C4 1.760(4) . ? S4 C4 1.766(4) . ? S4 C6 1.772(4) . ? S5 C5 1.744(4) . ? S5 C7 1.808(5) . ? S6 C6 1.758(4) . ? S6 C8 1.791(5) . ? O4 C10 1.281(5) . ? O3 C10 1.230(5) . ? O1 C9 1.215(5) . ? O2 C9 1.295(5) . ? O2 H2A 0.831(10) . ? N1 C15 1.346(5) . ? N1 C11 1.346(5) . ? N1 H1A 0.865(18) . ? N2 C16 1.332(5) . ? N2 C20 1.343(5) . ? C6 C5 1.346(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C2 C1 1.350(5) . ? C2 C10 1.508(5) . ? C3 C4 1.340(5) . ? C14 C15 1.376(5) . ? C14 C13 1.383(6) . ? C14 H14A 0.9400 . ? C12 C11 1.358(6) . ? C12 C13 1.378(6) . ? C12 H12A 0.9400 . ? C15 C20 1.488(5) . ? C1 C9 1.503(5) . ? C11 H11A 0.9400 . ? C19 C20 1.384(5) . ? C19 C18 1.385(6) . ? C19 H19A 0.9400 . ? C16 C17 1.378(6) . ? C16 H16A 0.9400 . ? C17 C18 1.373(6) . ? C17 H17A 0.9400 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C13 H13A 0.9400 . ? C18 H18A 0.9400 . ? 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 C2 S2 C3 95.04(18) . . ? C1 S1 C3 95.16(18) . . ? C5 S3 C4 94.34(19) . . ? C4 S4 C6 93.67(19) . . ? C5 S5 C7 102.2(2) . . ? C6 S6 C8 100.5(2) . . ? C9 O2 H2A 111(4) . . ? C15 N1 C11 123.8(3) . . ? C15 N1 H1A 116(3) . . ? C11 N1 H1A 120(3) . . ? C16 N2 C20 116.7(4) . . ? C5 C6 S6 125.6(3) . . ? C5 C6 S4 117.0(3) . . ? S6 C6 S4 117.3(2) . . ? S5 C7 H7A 109.5 . . ? S5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C2 C10 130.3(4) . . ? C1 C2 S2 117.2(3) . . ? C10 C2 S2 112.4(3) . . ? C4 C3 S1 120.6(3) . . ? C4 C3 S2 124.4(3) . . ? S1 C3 S2 115.0(2) . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C11 C12 C13 118.9(4) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? N1 C15 C14 117.7(4) . . ? N1 C15 C20 116.6(3) . . ? C14 C15 C20 125.8(4) . . ? C2 C1 C9 132.3(4) . . ? C2 C1 S1 117.4(3) . . ? C9 C1 S1 110.2(3) . . ? C6 C5 S5 123.8(3) . . ? C6 C5 S3 117.0(3) . . ? S5 C5 S3 118.7(2) . . ? C3 C4 S3 120.9(3) . . ? C3 C4 S4 125.7(3) . . ? S3 C4 S4 113.3(2) . . ? O3 C10 O4 125.4(4) . . ? O3 C10 C2 117.6(4) . . ? O4 C10 C2 116.9(3) . . ? O1 C9 O2 123.5(4) . . ? O1 C9 C1 117.3(4) . . ? O2 C9 C1 119.1(4) . . ? N1 C11 C12 119.5(4) . . ? N1 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C20 C19 C18 118.1(4) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? N2 C20 C19 123.4(4) . . ? N2 C20 C15 115.2(3) . . ? C19 C20 C15 121.4(4) . . ? N2 C16 C17 124.2(4) . . ? N2 C16 H16A 117.9 . . ? C17 C16 H16A 117.9 . . ? C18 C17 C16 118.2(4) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? S6 C8 H8A 109.5 . . ? S6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C17 C18 C19 119.4(4) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 S6 C6 C5 79.3(4) . . . . ? C8 S6 C6 S4 -96.5(3) . . . . ? C4 S4 C6 C5 12.1(4) . . . . ? C4 S4 C6 S6 -171.6(3) . . . . ? C3 S2 C2 C1 -2.0(4) . . . . ? C3 S2 C2 C10 179.4(3) . . . . ? C1 S1 C3 C4 175.7(4) . . . . ? C1 S1 C3 S2 -3.7(3) . . . . ? C2 S2 C3 C4 -175.8(4) . . . . ? C2 S2 C3 S1 3.6(3) . . . . ? C11 N1 C15 C14 -0.5(6) . . . . ? C11 N1 C15 C20 179.3(4) . . . . ? C13 C14 C15 N1 0.1(6) . . . . ? C13 C14 C15 C20 -179.7(4) . . . . ? C10 C2 C1 C9 -0.7(8) . . . . ? S2 C2 C1 C9 -179.0(4) . . . . ? C10 C2 C1 S1 178.0(3) . . . . ? S2 C2 C1 S1 -0.3(5) . . . . ? C3 S1 C1 C2 2.5(4) . . . . ? C3 S1 C1 C9 -178.6(3) . . . . ? S6 C6 C5 S5 -3.6(6) . . . . ? S4 C6 C5 S5 172.3(2) . . . . ? S6 C6 C5 S3 -175.1(2) . . . . ? S4 C6 C5 S3 0.8(5) . . . . ? C7 S5 C5 C6 146.9(4) . . . . ? C7 S5 C5 S3 -41.7(3) . . . . ? C4 S3 C5 C6 -13.4(4) . . . . ? C4 S3 C5 S5 174.7(3) . . . . ? S1 C3 C4 S3 -1.4(5) . . . . ? S2 C3 C4 S3 178.0(2) . . . . ? S1 C3 C4 S4 -179.1(2) . . . . ? S2 C3 C4 S4 0.3(6) . . . . ? C5 S3 C4 C3 -156.8(4) . . . . ? C5 S3 C4 S4 21.2(3) . . . . ? C6 S4 C4 C3 157.1(4) . . . . ? C6 S4 C4 S3 -20.7(3) . . . . ? C1 C2 C10 O3 -176.7(4) . . . . ? S2 C2 C10 O3 1.7(5) . . . . ? C1 C2 C10 O4 5.2(7) . . . . ? S2 C2 C10 O4 -176.4(3) . . . . ? C2 C1 C9 O1 177.5(5) . . . . ? S1 C1 C9 O1 -1.3(5) . . . . ? C2 C1 C9 O2 -3.8(7) . . . . ? S1 C1 C9 O2 177.5(3) . . . . ? C15 N1 C11 C12 0.6(7) . . . . ? C13 C12 C11 N1 -0.3(7) . . . . ? C16 N2 C20 C19 -1.9(6) . . . . ? C16 N2 C20 C15 179.5(4) . . . . ? C18 C19 C20 N2 1.1(7) . . . . ? C18 C19 C20 C15 179.6(4) . . . . ? N1 C15 C20 N2 9.7(6) . . . . ? C14 C15 C20 N2 -170.4(4) . . . . ? N1 C15 C20 C19 -168.9(4) . . . . ? C14 C15 C20 C19 10.9(7) . . . . ? C20 N2 C16 C17 1.2(7) . . . . ? N2 C16 C17 C18 0.2(8) . . . . ? C11 C12 C13 C14 -0.1(7) . . . . ? C15 C14 C13 C12 0.1(7) . . . . ? C16 C17 C18 C19 -1.1(7) . . . . ? C20 C19 C18 C17 0.5(7) . . . . ? 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 H1A O4 0.865(18) 1.96(2) 2.755(4) 153(4) . O2 H2A O4 0.831(10) 1.608(13) 2.435(4) 174(6) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.374 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.064 ########End data_H2(4,4_py)_2(HL) _database_code_depnum_ccdc_archive 'CCDC 881723' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C10 H7 O4 S6), C10 H10 N2' _chemical_formula_sum 'C30 H24 N2 O8 S12' _chemical_formula_weight 925.23 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6334(7) _cell_length_b 13.2801(9) _cell_length_c 13.5988(8) _cell_angle_alpha 77.855(8) _cell_angle_beta 78.677(8) _cell_angle_gamma 79.177(7) _cell_volume 1819.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7775 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16774 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8197 _reflns_number_gt 5738 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8197 _refine_ls_number_parameters 486 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2062 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 S9 S 0.01693(14) 0.87886(11) 0.96233(10) 0.0355(3) Uani 1 1 d . . . S7 S 0.10181(14) 0.90311(11) 0.70792(10) 0.0337(3) Uani 1 1 d . . . S8 S 0.09299(14) 0.67759(11) 0.73270(10) 0.0338(3) Uani 1 1 d . . . S2 S 0.39375(16) -0.35960(12) -0.15164(11) 0.0398(4) Uani 1 1 d . . . S1 S 0.39441(14) -0.13267(11) -0.18194(10) 0.0355(3) Uani 1 1 d . . . S10 S 0.02148(15) 0.65463(12) 0.97154(10) 0.0400(4) Uani 1 1 d . . . S3 S 0.47139(16) -0.12857(13) -0.43180(11) 0.0427(4) Uani 1 1 d . . . S6 S 0.58448(15) -0.38431(14) -0.60145(12) 0.0462(4) Uani 1 1 d . . . S11 S -0.12171(16) 0.87993(13) 1.17450(11) 0.0449(4) Uani 1 1 d . . . S4 S 0.44571(16) -0.35049(13) -0.39360(11) 0.0428(4) Uani 1 1 d . . . S12 S -0.10753(19) 0.61838(15) 1.19024(12) 0.0553(5) Uani 1 1 d . . . S5 S 0.61057(19) -0.12096(16) -0.64141(12) 0.0585(5) Uani 1 1 d . . . O3 O 0.3325(4) -0.4715(4) 0.0430(3) 0.0511(11) Uani 1 1 d . . . O4 O 0.2974(6) -0.3505(4) 0.1396(3) 0.0619(14) Uani 1 1 d D . . H4 H 0.317(8) -0.289(3) 0.125(6) 0.093 Uiso 1 1 d D . . O2 O 0.3109(5) -0.1638(4) 0.1140(3) 0.0574(13) Uani 1 1 d . . . O1 O 0.3524(4) -0.0352(3) -0.0171(3) 0.0482(11) Uani 1 1 d . . . O6 O 0.1756(4) 0.9012(3) 0.4142(3) 0.0466(11) Uani 1 1 d D . . H6 H 0.181(7) 0.8354(11) 0.422(5) 0.070 Uiso 1 1 d D . . O5 O 0.1466(4) 1.0202(3) 0.5114(3) 0.0449(10) Uani 1 1 d . . . O8 O 0.1514(4) 0.7162(3) 0.4372(3) 0.0466(11) Uani 1 1 d . . . O7 O 0.1207(4) 0.5860(3) 0.5673(3) 0.0396(10) Uani 1 1 d . . . N1 N 0.1680(5) 0.4513(4) 0.4429(4) 0.0375(11) Uani 1 1 d D . . H1 H 0.151(6) 0.498(4) 0.483(4) 0.056 Uiso 1 1 d D . . N2 N 0.2990(4) 0.0980(4) 0.1088(3) 0.0349(11) Uani 1 1 d D . . H2 H 0.316(6) 0.047(4) 0.074(4) 0.052 Uiso 1 1 d D . . C21 C 0.1757(6) 0.3504(5) 0.4812(4) 0.0383(13) Uani 1 1 d . . . H21 H 0.1640 0.3279 0.5522 0.046 Uiso 1 1 calc R . . C22 C 0.2009(5) 0.2777(5) 0.4176(4) 0.0370(13) Uani 1 1 d . . . H22 H 0.2045 0.2062 0.4449 0.044 Uiso 1 1 calc R . . C23 C 0.2208(5) 0.3121(4) 0.3120(4) 0.0307(12) Uani 1 1 d . . . C24 C 0.2128(6) 0.4184(5) 0.2758(4) 0.0417(14) Uani 1 1 d . . . H24 H 0.2259 0.4434 0.2051 0.050 Uiso 1 1 calc R . . C25 C 0.1858(6) 0.4879(5) 0.3422(5) 0.0418(14) Uani 1 1 d . . . H25 H 0.1799 0.5599 0.3172 0.050 Uiso 1 1 calc R . . C28 C 0.2488(5) 0.2382(4) 0.2397(4) 0.0290(11) Uani 1 1 d . . . C27 C 0.2327(5) 0.1341(4) 0.2750(4) 0.0327(12) Uani 1 1 d . . . H27 H 0.2047 0.1107 0.3447 0.039 Uiso 1 1 calc R . . C26 C 0.2578(6) 0.0659(5) 0.2078(4) 0.0387(13) Uani 1 1 d . . . H26 H 0.2458 -0.0040 0.2317 0.046 Uiso 1 1 calc R . . C30 C 0.3168(5) 0.1965(5) 0.0717(4) 0.0352(13) Uani 1 1 d . . . H30 H 0.3468 0.2168 0.0018 0.042 Uiso 1 1 calc R . . C29 C 0.2910(5) 0.2691(5) 0.1359(4) 0.0340(12) Uani 1 1 d . . . H29 H 0.3019 0.3388 0.1094 0.041 Uiso 1 1 calc R . . C2 C 0.3617(5) -0.3032(5) -0.0427(4) 0.0347(13) Uani 1 1 d . . . C1 C 0.3631(5) -0.1984(5) -0.0576(4) 0.0364(13) Uani 1 1 d . . . C10 C 0.3301(6) -0.3821(5) 0.0520(4) 0.0417(14) Uani 1 1 d . . . C9 C 0.3401(6) -0.1270(5) 0.0200(5) 0.0416(15) Uani 1 1 d . . . C4 C 0.4417(5) -0.2401(4) -0.3402(4) 0.0348(12) Uani 1 1 d . . . C6 C 0.5214(6) -0.2973(5) -0.5169(4) 0.0395(14) Uani 1 1 d . . . C5 C 0.5326(6) -0.1962(5) -0.5337(4) 0.0391(14) Uani 1 1 d . . . C7 C 0.5408(8) -0.1413(6) -0.7448(5) 0.063(2) Uani 1 1 d . . . H7A H 0.4470 -0.1298 -0.7276 0.094 Uiso 1 1 calc R . . H7B H 0.5702 -0.2122 -0.7563 0.094 Uiso 1 1 calc R . . H7C H 0.5678 -0.0929 -0.8062 0.094 Uiso 1 1 calc R . . C8 C 0.4416(6) -0.3880(6) -0.6517(5) 0.0577(19) Uani 1 1 d . . . H8A H 0.4088 -0.3184 -0.6844 0.086 Uiso 1 1 calc R . . H8B H 0.3759 -0.4135 -0.5966 0.086 Uiso 1 1 calc R . . H8C H 0.4631 -0.4341 -0.7012 0.086 Uiso 1 1 calc R . . C16 C -0.0560(6) 0.7066(5) 1.0813(4) 0.0381(13) Uani 1 1 d . . . C15 C -0.0554(5) 0.8094(5) 1.0763(4) 0.0341(13) Uani 1 1 d . . . C14 C 0.0406(5) 0.7768(4) 0.8933(4) 0.0306(12) Uani 1 1 d . . . C13 C 0.0717(5) 0.7873(4) 0.7904(4) 0.0293(11) Uani 1 1 d . . . C12 C 0.1153(5) 0.7487(4) 0.6086(4) 0.0285(11) Uani 1 1 d . . . C11 C 0.1201(5) 0.8509(5) 0.5966(4) 0.0326(12) Uani 1 1 d . . . C20 C 0.1301(5) 0.6786(5) 0.5306(4) 0.0360(13) Uani 1 1 d . . . C19 C 0.1467(6) 0.9318(5) 0.5032(4) 0.0351(13) Uani 1 1 d . . . C18 C -0.2395(7) 0.5778(6) 1.1528(5) 0.0535(17) Uani 1 1 d . . . H18A H -0.2088 0.5492 1.0908 0.080 Uiso 1 1 calc R . . H18B H -0.3068 0.6372 1.1406 0.080 Uiso 1 1 calc R . . H18C H -0.2746 0.5250 1.2066 0.080 Uiso 1 1 calc R . . C17 C -0.0104(7) 0.8268(6) 1.2644(5) 0.0544(18) Uani 1 1 d . . . H17A H 0.0763 0.8401 1.2326 0.082 Uiso 1 1 calc R . . H17B H -0.0103 0.7522 1.2847 0.082 Uiso 1 1 calc R . . H17C H -0.0377 0.8596 1.3241 0.082 Uiso 1 1 calc R . . C3 C 0.4147(5) -0.2437(4) -0.2387(4) 0.0334(12) 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 S9 0.0522(9) 0.0304(8) 0.0253(6) -0.0077(6) -0.0018(6) -0.0112(6) S7 0.0495(8) 0.0265(8) 0.0264(6) -0.0066(5) -0.0046(6) -0.0088(6) S8 0.0465(8) 0.0290(8) 0.0273(6) -0.0078(6) -0.0058(6) -0.0065(6) S2 0.0601(10) 0.0292(8) 0.0318(7) -0.0083(6) -0.0074(6) -0.0079(7) S1 0.0507(8) 0.0297(8) 0.0267(7) -0.0076(6) -0.0037(6) -0.0078(6) S10 0.0575(9) 0.0305(9) 0.0309(7) -0.0059(6) -0.0031(6) -0.0080(7) S3 0.0581(10) 0.0379(9) 0.0310(7) -0.0091(6) 0.0008(7) -0.0101(7) S6 0.0487(9) 0.0529(11) 0.0406(8) -0.0230(7) -0.0046(7) -0.0031(8) S11 0.0553(9) 0.0484(10) 0.0300(7) -0.0144(7) 0.0001(6) -0.0044(8) S4 0.0582(10) 0.0380(9) 0.0342(7) -0.0137(7) -0.0015(7) -0.0103(7) S12 0.0798(12) 0.0563(12) 0.0331(8) 0.0013(7) -0.0056(8) -0.0329(10) S5 0.0791(13) 0.0657(13) 0.0341(8) -0.0114(8) 0.0054(8) -0.0320(10) O3 0.072(3) 0.042(3) 0.039(2) -0.003(2) -0.007(2) -0.018(2) O4 0.105(4) 0.051(3) 0.030(2) -0.002(2) -0.004(2) -0.028(3) O2 0.092(4) 0.056(3) 0.028(2) -0.014(2) -0.008(2) -0.017(3) O1 0.072(3) 0.035(3) 0.043(2) -0.019(2) -0.004(2) -0.013(2) O6 0.065(3) 0.042(3) 0.031(2) -0.006(2) -0.0054(19) -0.008(2) O5 0.064(3) 0.033(3) 0.036(2) -0.0028(18) -0.0061(19) -0.008(2) O8 0.067(3) 0.045(3) 0.032(2) -0.0134(19) -0.012(2) -0.008(2) O7 0.053(2) 0.030(2) 0.038(2) -0.0156(18) -0.0093(18) -0.0013(19) N1 0.040(3) 0.036(3) 0.043(3) -0.016(2) -0.010(2) -0.010(2) N2 0.043(3) 0.031(3) 0.036(3) -0.015(2) -0.007(2) -0.007(2) C21 0.045(3) 0.039(4) 0.033(3) -0.007(3) -0.003(2) -0.013(3) C22 0.040(3) 0.039(4) 0.031(3) -0.001(2) -0.011(2) -0.006(3) C23 0.034(3) 0.027(3) 0.034(3) -0.007(2) -0.002(2) -0.011(2) C24 0.054(4) 0.045(4) 0.029(3) -0.014(3) 0.000(3) -0.014(3) C25 0.056(4) 0.027(3) 0.044(3) -0.010(3) -0.011(3) -0.004(3) C28 0.027(3) 0.032(3) 0.031(3) -0.010(2) -0.004(2) -0.008(2) C27 0.043(3) 0.029(3) 0.025(3) -0.006(2) -0.002(2) -0.008(2) C26 0.051(3) 0.031(3) 0.037(3) -0.011(3) -0.002(3) -0.012(3) C30 0.044(3) 0.032(3) 0.031(3) -0.009(2) -0.008(2) -0.006(3) C29 0.044(3) 0.029(3) 0.030(3) -0.004(2) -0.006(2) -0.010(2) C2 0.041(3) 0.038(4) 0.028(3) -0.012(2) -0.003(2) -0.009(3) C1 0.040(3) 0.043(4) 0.031(3) -0.014(3) -0.002(2) -0.014(3) C10 0.049(4) 0.042(4) 0.035(3) -0.003(3) -0.012(3) -0.009(3) C9 0.042(3) 0.049(4) 0.039(3) -0.019(3) -0.009(3) -0.004(3) C4 0.044(3) 0.027(3) 0.035(3) -0.006(2) -0.009(2) -0.005(2) C6 0.045(3) 0.043(4) 0.028(3) -0.007(3) -0.002(2) -0.006(3) C5 0.049(3) 0.040(4) 0.028(3) -0.010(2) 0.001(2) -0.010(3) C7 0.092(6) 0.054(5) 0.046(4) -0.002(3) -0.021(4) -0.019(4) C8 0.056(4) 0.061(5) 0.065(4) -0.026(4) -0.016(3) -0.009(4) C16 0.052(3) 0.040(4) 0.023(3) 0.001(2) -0.005(2) -0.015(3) C15 0.039(3) 0.039(4) 0.024(3) -0.010(2) -0.002(2) -0.006(3) C14 0.035(3) 0.032(3) 0.026(3) -0.007(2) -0.007(2) -0.003(2) C13 0.036(3) 0.028(3) 0.025(2) -0.008(2) 0.001(2) -0.007(2) C12 0.032(3) 0.030(3) 0.024(2) -0.006(2) -0.007(2) -0.001(2) C11 0.038(3) 0.031(3) 0.030(3) -0.008(2) -0.004(2) -0.009(2) C20 0.038(3) 0.037(4) 0.034(3) -0.011(3) -0.011(2) 0.002(3) C19 0.045(3) 0.033(4) 0.029(3) -0.005(2) -0.006(2) -0.011(3) C18 0.060(4) 0.048(4) 0.051(4) -0.010(3) 0.002(3) -0.017(3) C17 0.075(5) 0.054(5) 0.040(3) -0.014(3) -0.018(3) -0.010(4) C3 0.047(3) 0.031(3) 0.024(2) -0.007(2) -0.002(2) -0.010(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 S9 C15 1.744(6) . ? S9 C14 1.760(5) . ? S7 C13 1.745(6) . ? S7 C11 1.757(5) . ? S8 C12 1.747(5) . ? S8 C13 1.754(5) . ? S2 C2 1.745(5) . ? S2 C3 1.754(6) . ? S1 C1 1.732(6) . ? S1 C3 1.764(5) . ? S10 C16 1.766(5) . ? S10 C14 1.766(6) . ? S3 C4 1.758(6) . ? S3 C5 1.761(5) . ? S6 C6 1.753(6) . ? S6 C8 1.796(7) . ? S11 C15 1.751(5) . ? S11 C17 1.812(7) . ? S4 C4 1.757(6) . ? S4 C6 1.773(6) . ? S12 C16 1.749(6) . ? S12 C18 1.789(7) . ? S5 C5 1.746(6) . ? S5 C7 1.801(7) . ? O3 C10 1.215(7) . ? O4 C10 1.307(7) . ? O4 H4 0.851(10) . ? O2 C9 1.268(7) . ? O1 C9 1.238(8) . ? O6 C19 1.319(6) . ? O6 H6 0.849(10) . ? O5 C19 1.202(7) . ? O8 C20 1.255(7) . ? O7 C20 1.240(7) . ? N1 C21 1.325(8) . ? N1 C25 1.342(7) . ? N1 H1 0.871(10) . ? N2 C30 1.333(7) . ? N2 C26 1.336(7) . ? N2 H2 0.872(10) . ? C21 C22 1.384(8) . ? C21 H21 0.9400 . ? C22 C23 1.399(7) . ? C22 H22 0.9400 . ? C23 C24 1.386(8) . ? C23 C28 1.483(7) . ? C24 C25 1.378(7) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C28 C29 1.393(7) . ? C28 C27 1.395(8) . ? C27 C26 1.375(7) . ? C27 H27 0.9400 . ? C26 H26 0.9400 . ? C30 C29 1.390(7) . ? C30 H30 0.9400 . ? C29 H29 0.9400 . ? C2 C1 1.366(8) . ? C2 C10 1.506(8) . ? C1 C9 1.517(7) . ? C4 C3 1.347(7) . ? C6 C5 1.338(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C16 C15 1.354(8) . ? C14 C13 1.355(7) . ? C12 C11 1.342(8) . ? C12 C20 1.520(7) . ? C11 C19 1.498(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? 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 C15 S9 C14 95.4(3) . . ? C13 S7 C11 94.6(3) . . ? C12 S8 C13 94.3(2) . . ? C2 S2 C3 95.7(3) . . ? C1 S1 C3 95.5(3) . . ? C16 S10 C14 95.1(3) . . ? C4 S3 C5 95.3(3) . . ? C6 S6 C8 100.6(3) . . ? C15 S11 C17 101.3(3) . . ? C4 S4 C6 95.2(3) . . ? C16 S12 C18 101.3(3) . . ? C5 S5 C7 104.1(3) . . ? C10 O4 H4 103(6) . . ? C19 O6 H6 110(5) . . ? C21 N1 C25 122.3(5) . . ? C21 N1 H1 121(5) . . ? C25 N1 H1 117(5) . . ? C30 N2 C26 121.6(5) . . ? C30 N2 H2 126(4) . . ? C26 N2 H2 112(5) . . ? N1 C21 C22 120.7(5) . . ? N1 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 119.0(6) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 118.1(5) . . ? C24 C23 C28 120.2(5) . . ? C22 C23 C28 121.6(5) . . ? C25 C24 C23 120.7(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? N1 C25 C24 119.1(6) . . ? N1 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C29 C28 C27 118.0(5) . . ? C29 C28 C23 122.0(5) . . ? C27 C28 C23 120.0(5) . . ? C26 C27 C28 120.0(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? N2 C26 C27 120.5(5) . . ? N2 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? N2 C30 C29 120.3(5) . . ? N2 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C1 C2 C10 132.0(5) . . ? C1 C2 S2 116.7(4) . . ? C10 C2 S2 111.2(4) . . ? C2 C1 C9 129.7(5) . . ? C2 C1 S1 117.7(4) . . ? C9 C1 S1 112.7(5) . . ? O3 C10 O4 123.2(6) . . ? O3 C10 C2 118.3(5) . . ? O4 C10 C2 118.5(6) . . ? O1 C9 O2 125.9(5) . . ? O1 C9 C1 114.5(5) . . ? O2 C9 C1 119.6(6) . . ? C3 C4 S4 121.4(5) . . ? C3 C4 S3 125.2(4) . . ? S4 C4 S3 113.4(3) . . ? C5 C6 S6 126.4(4) . . ? C5 C6 S4 116.6(4) . . ? S6 C6 S4 116.8(4) . . ? C6 C5 S5 129.1(4) . . ? C6 C5 S3 117.2(4) . . ? S5 C5 S3 113.5(4) . . ? S5 C7 H7A 109.5 . . ? S5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? S5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S6 C8 H8A 109.5 . . ? S6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C16 S12 126.0(4) . . ? C15 C16 S10 116.2(4) . . ? S12 C16 S10 117.2(4) . . ? C16 C15 S9 117.7(4) . . ? C16 C15 S11 125.7(4) . . ? S9 C15 S11 116.5(3) . . ? C13 C14 S9 125.1(5) . . ? C13 C14 S10 121.6(4) . . ? S9 C14 S10 113.3(3) . . ? C14 C13 S7 124.7(4) . . ? C14 C13 S8 119.7(4) . . ? S7 C13 S8 115.5(3) . . ? C11 C12 C20 131.0(5) . . ? C11 C12 S8 118.0(4) . . ? C20 C12 S8 111.0(4) . . ? C12 C11 C19 131.8(5) . . ? C12 C11 S7 117.0(4) . . ? C19 C11 S7 111.0(4) . . ? O7 C20 O8 125.5(5) . . ? O7 C20 C12 114.9(5) . . ? O8 C20 C12 119.6(5) . . ? O5 C19 O6 122.3(5) . . ? O5 C19 C11 120.0(5) . . ? O6 C19 C11 117.7(5) . . ? S12 C18 H18A 109.5 . . ? S12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? S11 C17 H17A 109.5 . . ? S11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C3 S2 122.6(4) . . ? C4 C3 S1 123.1(5) . . ? S2 C3 S1 114.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 N1 C21 C22 -1.0(8) . . . . ? N1 C21 C22 C23 1.3(8) . . . . ? C21 C22 C23 C24 -0.7(8) . . . . ? C21 C22 C23 C28 179.7(5) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C28 C23 C24 C25 179.5(5) . . . . ? C21 N1 C25 C24 0.1(9) . . . . ? C23 C24 C25 N1 0.4(9) . . . . ? C24 C23 C28 C29 11.9(8) . . . . ? C22 C23 C28 C29 -168.5(5) . . . . ? C24 C23 C28 C27 -167.8(5) . . . . ? C22 C23 C28 C27 11.8(8) . . . . ? C29 C28 C27 C26 -0.2(8) . . . . ? C23 C28 C27 C26 179.5(5) . . . . ? C30 N2 C26 C27 -0.3(9) . . . . ? C28 C27 C26 N2 0.8(8) . . . . ? C26 N2 C30 C29 -0.7(8) . . . . ? N2 C30 C29 C28 1.2(8) . . . . ? C27 C28 C29 C30 -0.7(8) . . . . ? C23 C28 C29 C30 179.6(5) . . . . ? C3 S2 C2 C1 -0.2(5) . . . . ? C3 S2 C2 C10 176.8(4) . . . . ? C10 C2 C1 C9 4.1(10) . . . . ? S2 C2 C1 C9 -179.7(5) . . . . ? C10 C2 C1 S1 -175.5(5) . . . . ? S2 C2 C1 S1 0.8(6) . . . . ? C3 S1 C1 C2 -0.9(5) . . . . ? C3 S1 C1 C9 179.4(4) . . . . ? C1 C2 C10 O3 177.6(6) . . . . ? S2 C2 C10 O3 1.2(7) . . . . ? C1 C2 C10 O4 -0.3(10) . . . . ? S2 C2 C10 O4 -176.6(5) . . . . ? C2 C1 C9 O1 177.6(6) . . . . ? S1 C1 C9 O1 -2.8(7) . . . . ? C2 C1 C9 O2 -2.4(9) . . . . ? S1 C1 C9 O2 177.2(5) . . . . ? C6 S4 C4 C3 -167.0(5) . . . . ? C6 S4 C4 S3 14.6(4) . . . . ? C5 S3 C4 C3 167.1(5) . . . . ? C5 S3 C4 S4 -14.5(4) . . . . ? C8 S6 C6 C5 -100.6(6) . . . . ? C8 S6 C6 S4 84.3(4) . . . . ? C4 S4 C6 C5 -9.0(5) . . . . ? C4 S4 C6 S6 166.6(3) . . . . ? S6 C6 C5 S5 0.1(9) . . . . ? S4 C6 C5 S5 175.2(4) . . . . ? S6 C6 C5 S3 -175.0(3) . . . . ? S4 C6 C5 S3 0.1(7) . . . . ? C7 S5 C5 C6 53.6(7) . . . . ? C7 S5 C5 S3 -131.2(4) . . . . ? C4 S3 C5 C6 8.8(5) . . . . ? C4 S3 C5 S5 -167.0(3) . . . . ? C18 S12 C16 C15 118.3(6) . . . . ? C18 S12 C16 S10 -70.3(4) . . . . ? C14 S10 C16 C15 -10.2(5) . . . . ? C14 S10 C16 S12 177.6(3) . . . . ? S12 C16 C15 S9 173.1(3) . . . . ? S10 C16 C15 S9 1.7(6) . . . . ? S12 C16 C15 S11 -7.1(8) . . . . ? S10 C16 C15 S11 -178.5(3) . . . . ? C14 S9 C15 C16 7.8(5) . . . . ? C14 S9 C15 S11 -172.1(3) . . . . ? C17 S11 C15 C16 69.9(6) . . . . ? C17 S11 C15 S9 -110.3(4) . . . . ? C15 S9 C14 C13 166.2(5) . . . . ? C15 S9 C14 S10 -14.3(3) . . . . ? C16 S10 C14 C13 -165.6(5) . . . . ? C16 S10 C14 S9 15.0(3) . . . . ? S9 C14 C13 S7 3.4(7) . . . . ? S10 C14 C13 S7 -176.0(3) . . . . ? S9 C14 C13 S8 179.6(3) . . . . ? S10 C14 C13 S8 0.3(6) . . . . ? C11 S7 C13 C14 -175.8(5) . . . . ? C11 S7 C13 S8 7.7(3) . . . . ? C12 S8 C13 C14 175.4(4) . . . . ? C12 S8 C13 S7 -7.9(3) . . . . ? C13 S8 C12 C11 5.1(5) . . . . ? C13 S8 C12 C20 -176.6(4) . . . . ? C20 C12 C11 C19 -2.8(10) . . . . ? S8 C12 C11 C19 175.1(5) . . . . ? C20 C12 C11 S7 -178.5(4) . . . . ? S8 C12 C11 S7 -0.6(6) . . . . ? C13 S7 C11 C12 -4.3(5) . . . . ? C13 S7 C11 C19 179.1(4) . . . . ? C11 C12 C20 O7 179.8(5) . . . . ? S8 C12 C20 O7 1.8(6) . . . . ? C11 C12 C20 O8 0.4(9) . . . . ? S8 C12 C20 O8 -177.6(4) . . . . ? C12 C11 C19 O5 -179.5(6) . . . . ? S7 C11 C19 O5 -3.6(7) . . . . ? C12 C11 C19 O6 -2.6(9) . . . . ? S7 C11 C19 O6 173.3(4) . . . . ? S4 C4 C3 S2 4.9(7) . . . . ? S3 C4 C3 S2 -176.9(3) . . . . ? S4 C4 C3 S1 -173.8(3) . . . . ? S3 C4 C3 S1 4.4(8) . . . . ? C2 S2 C3 C4 -179.3(5) . . . . ? C2 S2 C3 S1 -0.5(4) . . . . ? C1 S1 C3 C4 179.6(5) . . . . ? C1 S1 C3 S2 0.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O7 0.871(10) 1.759(12) 2.630(5) 177(7) . N2 H2 O1 0.872(10) 1.767(18) 2.627(6) 168(7) . O4 H4 O2 0.851(10) 1.63(3) 2.457(7) 164(9) . O6 H6 O8 0.849(10) 1.63(2) 2.465(6) 165(8) . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.391 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.089 ########End