# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Kumar Biradha' _publ_contact_author_email kbiradha@yahoo.com _publ_section_title ; Separation of isomers of sulfophthalic acid by guest induced host framework formation with 4,4'-bipyridine. ; loop_ _publ_author_name K.Biradha G.Mahata S.Roy # Attachment '- kbcif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 817472' #TrackingRef '- kbcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N2 O7 S' _chemical_formula_weight 580.59 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.683(8) _cell_length_b 11.118(5) _cell_length_c 13.547(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.469(13) _cell_angle_gamma 90.00 _cell_volume 2651(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3764 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.00 _exptl_crystal_description Needles _exptl_crystal_colour 'pink color' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.973 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD APex-2' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13232 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3764 _reflns_number_gt 2364 _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^)+(0.0699P)^2^+9.1741P] 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 0.0031(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(2) _refine_ls_number_reflns 3764 _refine_ls_number_parameters 380 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1323 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.07149(13) 0.45139(19) 0.17015(17) 0.0577(6) Uani 1 1 d . . . O11 O 0.1530(4) 0.8892(5) 0.5011(4) 0.075(2) Uani 1 1 d . . . O12 O 0.1484(4) 1.0049(6) 0.3676(5) 0.079(2) Uani 1 1 d . . . O13 O 0.2495(3) 0.9060(5) 0.2166(5) 0.0637(17) Uani 1 1 d . . . O14 O 0.1394(4) 0.9449(6) 0.1280(5) 0.0701(19) Uani 1 1 d . . . O15 O 0.1025(6) 0.4672(7) 0.0780(6) 0.123(4) Uani 1 1 d . . . O16 O -0.0104(4) 0.4374(6) 0.1644(7) 0.095(3) Uani 1 1 d . . . O17 O 0.1065(4) 0.3510(5) 0.2311(6) 0.080(2) Uani 1 1 d . . . C11 C 0.1294(4) 0.7953(6) 0.3458(5) 0.0415(18) Uani 1 1 d . . . C12 C 0.1447(4) 0.7882(7) 0.2471(6) 0.0453(19) Uani 1 1 d . . . C13 C 0.1246(4) 0.6796(7) 0.1921(6) 0.0438(18) Uani 1 1 d . . . H13 H 0.1331 0.6746 0.1255 0.053 Uiso 1 1 calc R . . C14 C 0.0927(4) 0.5820(6) 0.2381(6) 0.0405(17) Uani 1 1 d . . . C15 C 0.0784(5) 0.5918(7) 0.3368(6) 0.052(2) Uani 1 1 d . . . H15 H 0.0560 0.5278 0.3672 0.062 Uiso 1 1 calc R . . C16 C 0.0975(5) 0.6980(7) 0.3919(6) 0.047(2) Uani 1 1 d . . . H16 H 0.0887 0.7027 0.4584 0.057 Uiso 1 1 calc R . . C17 C 0.1453(5) 0.9051(8) 0.4064(7) 0.057(2) Uani 1 1 d . . . C18 C 0.1805(5) 0.8891(8) 0.1935(6) 0.052(2) Uani 1 1 d . . . N11A N -0.0529(5) 0.2061(7) 0.2083(6) 0.063(2) Uani 1 1 d . . . C11A C -0.0049(5) 0.1127(8) 0.2104(7) 0.066(3) Uani 1 1 d . . . H11A H 0.0471 0.1260 0.2117 0.079 Uiso 1 1 calc R . . C12A C -0.0324(5) -0.0018(8) 0.2107(7) 0.057(2) Uani 1 1 d . . . H12A H 0.0014 -0.0661 0.2124 0.068 Uiso 1 1 calc R . . C13A C -0.1083(5) -0.0241(7) 0.2085(6) 0.0442(19) Uani 1 1 d . . . C14A C -0.1573(5) 0.0763(7) 0.2050(7) 0.052(2) Uani 1 1 d . . . H14A H -0.2096 0.0650 0.2015 0.063 Uiso 1 1 calc R . . C15A C -0.1276(6) 0.1917(9) 0.2068(7) 0.061(2) Uani 1 1 d . . . H15A H -0.1596 0.2581 0.2068 0.074 Uiso 1 1 calc R . . N21A N -0.1988(4) -0.3795(6) 0.2035(5) 0.0532(17) Uani 1 1 d . . . C21A C -0.2447(5) -0.2855(9) 0.2075(8) 0.071(3) Uani 1 1 d . . . H21A H -0.2965 -0.2985 0.2096 0.085 Uiso 1 1 calc R . . C22A C -0.2174(5) -0.1674(8) 0.2087(8) 0.066(3) Uani 1 1 d . . . H22A H -0.2509 -0.1032 0.2105 0.079 Uiso 1 1 calc R . . C23A C -0.1409(5) -0.1468(7) 0.2070(6) 0.0482(19) Uani 1 1 d . . . C24A C -0.0946(5) -0.2457(7) 0.2021(8) 0.061(2) Uani 1 1 d . . . H24A H -0.0425 -0.2355 0.2004 0.073 Uiso 1 1 calc R . . C25A C -0.1253(6) -0.3599(8) 0.1995(8) 0.065(3) Uani 1 1 d . . . H25A H -0.0932 -0.4255 0.1949 0.078 Uiso 1 1 calc R . . C101 C 0.2386(6) 0.6256(12) 0.9560(7) 0.081(3) Uani 1 1 d . . . H101 H 0.1906 0.5906 0.9517 0.097 Uiso 1 1 calc R . . C102 C 0.2450(7) 0.7469(11) 0.9628(8) 0.088(3) Uani 1 1 d . . . H102 H 0.2022 0.7948 0.9657 0.105 Uiso 1 1 calc R . . C103 C 0.3158(8) 0.7973(10) 0.9655(8) 0.080(3) Uani 1 1 d . . . H103 H 0.3191 0.8807 0.9689 0.096 Uiso 1 1 calc R . . C104 C 0.3799(7) 0.7361(9) 0.9635(8) 0.076(3) Uani 1 1 d . . . H104 H 0.4265 0.7752 0.9642 0.091 Uiso 1 1 calc R . . C105 C 0.3747(5) 0.6035(9) 0.9602(6) 0.060(2) Uani 1 1 d . . . C106 C 0.3024(5) 0.5527(9) 0.9553(6) 0.062(2) Uani 1 1 d . . . C107 C 0.2957(5) 0.4249(10) 0.9509(8) 0.074(3) Uani 1 1 d . . . H107 H 0.2478 0.3898 0.9482 0.089 Uiso 1 1 calc R . . C108 C 0.3593(6) 0.3521(10) 0.9506(6) 0.065(3) Uani 1 1 d . . . C109 C 0.4338(6) 0.4029(9) 0.9586(6) 0.060(2) Uani 1 1 d . . . C110 C 0.4387(5) 0.5313(9) 0.9608(7) 0.060(2) Uani 1 1 d . . . H110 H 0.4863 0.5675 0.9628 0.072 Uiso 1 1 calc R . . C111 C 0.3559(7) 0.2230(10) 0.9463(8) 0.080(3) Uani 1 1 d . . . H111 H 0.3089 0.1846 0.9414 0.096 Uiso 1 1 calc R . . C112 C 0.4201(9) 0.1567(10) 0.9492(9) 0.089(4) Uani 1 1 d . . . H112 H 0.4159 0.0734 0.9450 0.107 Uiso 1 1 calc R . . C113 C 0.4915(7) 0.2069(11) 0.9580(8) 0.082(3) Uani 1 1 d . . . H113 H 0.5346 0.1586 0.9616 0.098 Uiso 1 1 calc R . . C114 C 0.4977(6) 0.3295(10) 0.9615(7) 0.074(3) Uani 1 1 d . . . H114 H 0.5457 0.3646 0.9658 0.089 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 S1 0.0563(14) 0.0494(12) 0.0692(14) -0.0061(11) 0.0147(11) -0.0091(11) O11 0.118(6) 0.062(4) 0.046(4) -0.008(3) 0.007(4) 0.004(4) O12 0.118(6) 0.054(4) 0.063(4) -0.017(3) 0.009(4) -0.009(4) O13 0.045(4) 0.048(3) 0.099(5) 0.009(3) 0.011(3) -0.013(3) O14 0.076(5) 0.067(4) 0.067(4) 0.022(3) 0.002(3) -0.014(3) O15 0.211(10) 0.088(5) 0.081(5) -0.038(4) 0.064(6) -0.064(6) O16 0.045(4) 0.058(4) 0.178(8) -0.041(4) -0.006(4) -0.011(3) O17 0.071(4) 0.042(3) 0.121(6) 0.014(4) -0.015(4) 0.017(3) C11 0.045(5) 0.043(4) 0.038(4) 0.000(3) 0.013(3) -0.001(3) C12 0.039(4) 0.039(4) 0.060(5) 0.009(3) 0.014(4) -0.001(3) C13 0.045(4) 0.047(4) 0.041(4) -0.009(3) 0.012(3) 0.004(4) C14 0.037(4) 0.039(4) 0.047(5) 0.002(3) 0.014(3) -0.003(3) C15 0.055(5) 0.043(4) 0.060(5) -0.007(4) 0.015(4) -0.003(4) C16 0.059(5) 0.041(4) 0.044(4) -0.010(3) 0.017(4) -0.003(4) C17 0.070(6) 0.044(5) 0.059(6) -0.012(4) 0.016(5) 0.000(4) C18 0.047(5) 0.060(5) 0.052(5) -0.001(4) 0.020(4) -0.008(4) N11A 0.073(6) 0.059(5) 0.059(5) 0.000(4) 0.019(4) 0.003(4) C11A 0.045(5) 0.059(6) 0.093(7) 0.005(5) 0.011(5) 0.000(5) C12A 0.041(5) 0.057(5) 0.075(6) 0.003(4) 0.010(4) -0.002(4) C13A 0.049(5) 0.045(4) 0.041(4) 0.006(3) 0.018(4) 0.006(4) C14A 0.039(5) 0.053(5) 0.066(5) -0.002(4) 0.014(4) -0.006(4) C15A 0.065(6) 0.064(6) 0.059(5) -0.007(5) 0.026(5) 0.002(5) N21A 0.046(4) 0.058(4) 0.056(4) -0.004(3) 0.012(3) -0.004(4) C21A 0.049(6) 0.073(7) 0.094(8) -0.007(6) 0.022(5) -0.007(5) C22A 0.046(5) 0.042(5) 0.113(8) -0.005(5) 0.020(5) -0.003(4) C23A 0.043(5) 0.049(5) 0.055(5) -0.004(4) 0.021(4) -0.005(4) C24A 0.037(4) 0.043(5) 0.108(7) 0.002(5) 0.031(5) -0.006(4) C25A 0.063(6) 0.052(5) 0.084(6) -0.006(5) 0.032(5) -0.015(5) C101 0.061(7) 0.118(10) 0.066(7) -0.007(6) 0.014(5) 0.015(7) C102 0.093(9) 0.088(8) 0.086(8) -0.006(6) 0.031(7) 0.019(7) C103 0.101(9) 0.068(7) 0.076(7) -0.001(5) 0.030(6) 0.005(7) C104 0.099(9) 0.065(6) 0.069(7) 0.001(5) 0.031(6) -0.012(6) C105 0.062(6) 0.083(7) 0.036(5) 0.015(4) 0.010(4) 0.007(5) C106 0.059(6) 0.077(7) 0.053(5) -0.001(5) 0.013(4) -0.001(5) C107 0.043(6) 0.105(9) 0.076(7) -0.007(6) 0.017(5) -0.011(6) C108 0.057(6) 0.094(8) 0.047(5) 0.009(5) 0.017(4) -0.019(6) C109 0.056(6) 0.072(6) 0.052(5) 0.004(5) 0.012(4) -0.006(5) C110 0.041(5) 0.079(6) 0.062(5) -0.006(5) 0.012(4) -0.010(5) C111 0.083(8) 0.075(7) 0.084(8) -0.012(6) 0.008(6) -0.036(6) C112 0.120(11) 0.064(7) 0.087(8) 0.004(6) 0.027(7) 0.009(8) C113 0.082(8) 0.083(8) 0.081(8) -0.012(6) 0.009(6) 0.022(7) C114 0.055(6) 0.094(8) 0.072(7) -0.010(6) -0.002(5) 0.002(6) _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 O15 1.421(8) . ? S1 O16 1.452(7) . ? S1 O17 1.488(6) . ? S1 C14 1.741(8) . ? O11 C17 1.288(11) . ? O12 C17 1.232(10) . ? O13 C18 1.245(10) . ? O14 C18 1.256(10) . ? C11 C12 1.392(10) . ? C11 C16 1.395(10) . ? C11 C17 1.482(10) . ? C12 C13 1.445(10) . ? C12 C18 1.507(11) . ? C13 C14 1.397(10) . ? C14 C15 1.389(11) . ? C15 C16 1.421(10) . ? N11A C15A 1.329(12) . ? N11A C11A 1.340(11) . ? C11A C12A 1.362(12) . ? C12A C13A 1.363(10) . ? C13A C14A 1.410(10) . ? C13A C23A 1.479(10) . ? C14A C15A 1.386(11) . ? N21A C21A 1.327(11) . ? N21A C25A 1.325(11) . ? C21A C22A 1.398(12) . ? C22A C23A 1.376(11) . ? C23A C24A 1.376(11) . ? C24A C25A 1.381(11) . ? C101 C102 1.355(15) . ? C101 C106 1.391(13) . ? C102 C103 1.369(15) . ? C103 C104 1.325(15) . ? C104 C105 1.478(13) . ? C105 C110 1.386(13) . ? C105 C106 1.394(13) . ? C106 C107 1.427(12) . ? C107 C108 1.386(14) . ? C108 C109 1.427(13) . ? C108 C111 1.438(14) . ? C109 C114 1.392(14) . ? C109 C110 1.431(12) . ? C111 C112 1.352(16) . ? C112 C113 1.375(17) . ? C113 C114 1.369(14) . ? 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 O15 S1 O16 115.6(6) . . ? O15 S1 O17 113.9(6) . . ? O16 S1 O17 108.0(4) . . ? O15 S1 C14 106.2(4) . . ? O16 S1 C14 106.4(4) . . ? O17 S1 C14 106.0(4) . . ? C12 C11 C16 120.7(7) . . ? C12 C11 C17 122.4(7) . . ? C16 C11 C17 116.9(7) . . ? C11 C12 C13 118.8(7) . . ? C11 C12 C18 123.3(7) . . ? C13 C12 C18 117.9(7) . . ? C14 C13 C12 120.6(7) . . ? C15 C14 C13 119.2(7) . . ? C15 C14 S1 121.6(6) . . ? C13 C14 S1 119.2(6) . . ? C14 C15 C16 121.0(7) . . ? C11 C16 C15 119.7(7) . . ? O12 C17 O11 122.9(8) . . ? O12 C17 C11 121.2(8) . . ? O11 C17 C11 115.8(8) . . ? O13 C18 O14 126.2(8) . . ? O13 C18 C12 116.0(8) . . ? O14 C18 C12 117.8(8) . . ? C15A N11A C11A 122.2(8) . . ? N11A C11A C12A 120.0(8) . . ? C11A C12A C13A 121.4(8) . . ? C12A C13A C14A 117.2(7) . . ? C12A C13A C23A 123.3(7) . . ? C14A C13A C23A 119.5(7) . . ? C15A C14A C13A 120.1(8) . . ? N11A C15A C14A 119.1(9) . . ? C21A N21A C25A 118.6(8) . . ? N21A C21A C22A 121.9(9) . . ? C23A C22A C21A 119.7(8) . . ? C24A C23A C22A 117.3(8) . . ? C24A C23A C13A 120.3(7) . . ? C22A C23A C13A 122.4(7) . . ? C23A C24A C25A 120.2(9) . . ? N21A C25A C24A 122.4(9) . . ? C102 C101 C106 121.2(11) . . ? C101 C102 C103 118.6(11) . . ? C104 C103 C102 124.8(11) . . ? C103 C104 C105 117.6(10) . . ? C110 C105 C106 120.7(9) . . ? C110 C105 C104 121.9(10) . . ? C106 C105 C104 117.3(9) . . ? C101 C106 C105 120.4(10) . . ? C101 C106 C107 121.1(10) . . ? C105 C106 C107 118.5(9) . . ? C108 C107 C106 121.1(9) . . ? C107 C108 C109 120.8(10) . . ? C107 C108 C111 123.5(10) . . ? C109 C108 C111 115.7(10) . . ? C114 C109 C108 120.8(9) . . ? C114 C109 C110 122.4(10) . . ? C108 C109 C110 116.8(9) . . ? C105 C110 C109 121.9(9) . . ? C112 C111 C108 120.7(10) . . ? C111 C112 C113 122.9(11) . . ? C114 C113 C112 118.5(11) . . ? C113 C114 C109 121.4(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.343 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.075 data_2 _database_code_depnum_ccdc_archive 'CCDC 817473' #TrackingRef '- kbcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 N6 O22 S4' _chemical_formula_weight 1285.24 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.345(4) _cell_length_b 10.533(5) _cell_length_c 16.280(8) _cell_angle_alpha 102.425(13) _cell_angle_beta 93.061(15) _cell_angle_gamma 93.425(13) _cell_volume 1391.7(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4613 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.00 _exptl_crystal_description blocks _exptl_crystal_colour 'greenish yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruket CCD APEX-2' _diffrn_measurement_method Hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14322 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4613 _reflns_number_gt 2915 _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. Floating origin 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^)+(0.1000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.016(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4613 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.1982 _refine_ls_goodness_of_fit_ref 1.379 _refine_ls_restrained_S_all 1.379 _refine_ls_shift/su_max 0.017 _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 N11A N -0.1923(5) 0.6207(3) 0.6244(2) 0.0580(10) Uani 1 1 d . . . H11N H -0.2572 0.6819 0.6329 0.070 Uiso 1 1 d R . . N21A N 0.3238(6) 0.1192(5) 0.5613(3) 0.0787(14) Uani 1 1 d . . . H21N H 0.3835 0.0546 0.5560 0.094 Uiso 1 1 d R . . C11A C -0.0338(6) 0.6509(5) 0.6395(3) 0.0652(14) Uani 1 1 d . . . H11A H 0.0048 0.7376 0.6581 0.078 Uiso 1 1 calc R . . C12A C 0.0715(6) 0.5551(4) 0.6277(3) 0.0615(13) Uani 1 1 d . . . H12A H 0.1815 0.5763 0.6386 0.074 Uiso 1 1 calc R . . C13A C 0.0130(5) 0.4256(4) 0.5993(3) 0.0496(11) Uani 1 1 d . . . C14A C -0.1509(5) 0.3988(4) 0.5837(3) 0.0557(12) Uani 1 1 d . . . H14A H -0.1930 0.3131 0.5643 0.067 Uiso 1 1 calc R . . C15A C -0.2515(6) 0.4977(4) 0.5966(3) 0.0595(12) Uani 1 1 d . . . H15A H -0.3620 0.4792 0.5859 0.071 Uiso 1 1 calc R . . C21A C 0.3720(6) 0.2287(6) 0.6157(4) 0.0804(17) Uani 1 1 d . . . H21A H 0.4711 0.2359 0.6460 0.096 Uiso 1 1 calc R . . C22A C 0.2767(6) 0.3316(5) 0.6278(3) 0.0660(14) Uani 1 1 d . . . H22A H 0.3118 0.4096 0.6650 0.079 Uiso 1 1 calc R . . C23A C 0.1248(5) 0.3183(4) 0.5833(3) 0.0552(12) Uani 1 1 d . . . C24A C 0.0846(6) 0.2032(4) 0.5254(3) 0.0613(13) Uani 1 1 d . . . H24A H -0.0130 0.1921 0.4934 0.074 Uiso 1 1 calc R . . C25A C 0.1866(7) 0.1057(5) 0.5145(3) 0.0736(15) Uani 1 1 d . . . H25A H 0.1597 0.0293 0.4742 0.088 Uiso 1 1 calc R . . N11B N 0.4276(5) 0.3047(4) 0.1167(3) 0.0731(12) Uani 1 1 d . . . H12N H 0.4090 0.3799 0.1459 0.088 Uiso 1 1 d R . . C11B C 0.4693(8) 0.2142(5) 0.1547(4) 0.0860(19) Uani 1 1 d . . . H11B H 0.4804 0.2322 0.2133 0.103 Uiso 1 1 calc R . . C12B C 0.4970(8) 0.0933(5) 0.1104(4) 0.0818(17) Uani 1 1 d . . . H12B H 0.5249 0.0294 0.1389 0.098 Uiso 1 1 calc R . . C13B C 0.4840(6) 0.0651(4) 0.0240(3) 0.0561(12) Uani 1 1 d . . . C14B C 0.4374(10) 0.1615(6) -0.0133(4) 0.110(3) Uani 1 1 d . . . H14B H 0.4215 0.1452 -0.0718 0.132 Uiso 1 1 calc R . . C15B C 0.4134(11) 0.2823(6) 0.0336(5) 0.113(3) Uani 1 1 d . . . H15B H 0.3870 0.3486 0.0069 0.135 Uiso 1 1 calc R . . S2 S 0.34279(15) 0.62903(12) 0.16938(9) 0.0643(4) Uani 1 1 d . . . O11 O -0.2506(4) 0.9760(3) 0.2504(2) 0.0717(10) Uani 1 1 d . . . H11O H -0.2640 1.0484 0.2731 0.108 Uiso 1 1 d R . . O12 O -0.0313(4) 1.0106(3) 0.3370(2) 0.0733(10) Uani 1 1 d . . . O13 O 0.2743(4) 0.8640(3) 0.3549(2) 0.0624(9) Uani 1 1 d . . . O14 O 0.2654(4) 0.9808(3) 0.25503(19) 0.0586(9) Uani 1 1 d . . . H14O H 0.3122 1.0382 0.2931 0.088 Uiso 1 1 d R . . O15 O 0.3484(4) 0.5685(3) 0.0796(2) 0.0735(10) Uani 1 1 d . . . O16 O 0.4389(4) 0.7507(3) 0.1943(3) 0.0834(12) Uani 1 1 d . . . O17 O 0.3756(5) 0.5372(4) 0.2216(2) 0.0835(12) Uani 1 1 d . . . C11 C -0.0627(5) 0.8164(4) 0.2286(3) 0.0537(11) Uani 1 1 d . . . C12 C 0.0990(5) 0.7873(4) 0.2318(3) 0.0515(11) Uani 1 1 d . . . C13 C 0.1394(5) 0.6690(4) 0.1830(3) 0.0548(11) Uani 1 1 d . . . C14 C 0.0217(6) 0.5818(5) 0.1350(4) 0.0728(15) Uani 1 1 d . . . H14 H 0.0499 0.5035 0.1025 0.087 Uiso 1 1 calc R . . C15 C -0.1373(6) 0.6108(5) 0.1353(4) 0.0790(17) Uani 1 1 d . . . H15 H -0.2166 0.5507 0.1049 0.095 Uiso 1 1 calc R . . C16 C -0.1779(6) 0.7280(5) 0.1805(4) 0.0687(14) Uani 1 1 d . . . H16 H -0.2847 0.7485 0.1788 0.082 Uiso 1 1 calc R . . C17 C -0.1117(5) 0.9438(5) 0.2780(3) 0.0568(12) Uani 1 1 d . . . C18 C 0.2221(5) 0.8799(4) 0.2883(3) 0.0496(11) Uani 1 1 d . . . C101 C 0.8785(7) 0.1190(6) -0.0384(4) 0.0862(18) Uani 1 1 d . . . H101 H 0.8221 0.1264 -0.0878 0.103 Uiso 1 1 calc R . . C102 C 0.8806(8) 0.2176(7) 0.0303(5) 0.095(2) Uani 1 1 d . . . H102 H 0.8290 0.2927 0.0277 0.114 Uiso 1 1 calc R . . C103 C 0.9627(8) 0.2051(7) 0.1067(4) 0.095(2) Uani 1 1 d . . . H103 H 0.9632 0.2714 0.1547 0.114 Uiso 1 1 calc R . . C104 C 1.0401(8) 0.0967(7) 0.1095(4) 0.0900(19) Uani 1 1 d . . . H104 H 1.0935 0.0895 0.1597 0.108 Uiso 1 1 calc R . . C105 C 0.9587(7) 0.0054(6) -0.0378(4) 0.0762(16) Uani 1 1 d . . . S1 S 0.55756(13) 0.21774(10) 0.39392(8) 0.0535(4) Uani 1 1 d . . . O101 O 0.5943(4) 0.1323(3) 0.4499(2) 0.0795(11) Uani 1 1 d . . . O102 O 0.6645(4) 0.1964(3) 0.3229(2) 0.0662(9) Uani 1 1 d . . . O103 O 0.5700(4) 0.3529(3) 0.4360(2) 0.0764(11) Uani 1 1 d . . . O104 O 0.3874(3) 0.1851(3) 0.3571(2) 0.0618(9) 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 N11A 0.055(2) 0.045(2) 0.074(3) 0.0091(18) 0.0002(19) 0.0261(19) N21A 0.073(3) 0.082(3) 0.096(3) 0.035(3) 0.021(3) 0.051(3) C11A 0.064(3) 0.049(3) 0.080(3) 0.012(2) -0.011(3) 0.008(2) C12A 0.047(3) 0.051(3) 0.089(4) 0.021(2) -0.006(2) 0.011(2) C13A 0.043(2) 0.040(2) 0.065(3) 0.013(2) -0.009(2) 0.0104(19) C14A 0.045(3) 0.041(2) 0.079(3) 0.008(2) -0.008(2) 0.011(2) C15A 0.042(3) 0.054(3) 0.082(3) 0.013(2) -0.004(2) 0.012(2) C21A 0.052(3) 0.097(5) 0.098(4) 0.028(4) 0.001(3) 0.037(3) C22A 0.058(3) 0.062(3) 0.079(3) 0.015(3) -0.004(3) 0.018(3) C23A 0.047(3) 0.055(3) 0.069(3) 0.023(2) -0.001(2) 0.019(2) C24A 0.064(3) 0.046(3) 0.076(3) 0.014(2) 0.000(2) 0.020(2) C25A 0.092(4) 0.065(3) 0.072(3) 0.021(3) 0.018(3) 0.035(3) N11B 0.083(3) 0.052(2) 0.081(3) 0.004(2) 0.006(2) 0.022(2) C11B 0.112(5) 0.066(4) 0.076(4) 0.004(3) -0.008(3) 0.034(3) C12B 0.111(5) 0.062(3) 0.076(4) 0.020(3) -0.007(3) 0.034(3) C13B 0.060(3) 0.049(3) 0.060(3) 0.015(2) -0.001(2) 0.013(2) C14B 0.197(8) 0.063(4) 0.072(4) 0.009(3) -0.006(4) 0.058(4) C15B 0.193(8) 0.060(4) 0.094(5) 0.023(3) 0.015(5) 0.057(4) S2 0.0499(8) 0.0512(7) 0.0861(10) 0.0000(6) -0.0031(6) 0.0198(6) O11 0.055(2) 0.063(2) 0.091(3) 0.0022(18) -0.0142(18) 0.0264(17) O12 0.054(2) 0.064(2) 0.090(2) -0.0093(19) -0.0148(18) 0.0209(17) O13 0.057(2) 0.0549(19) 0.075(2) 0.0168(16) -0.0170(16) 0.0149(15) O14 0.058(2) 0.0483(18) 0.065(2) 0.0069(15) -0.0125(15) 0.0026(15) O15 0.083(3) 0.064(2) 0.069(2) -0.0022(17) 0.0112(18) 0.0265(19) O16 0.044(2) 0.065(2) 0.125(3) -0.015(2) 0.005(2) 0.0048(17) O17 0.084(3) 0.080(3) 0.088(3) 0.013(2) -0.004(2) 0.047(2) C11 0.043(3) 0.044(2) 0.073(3) 0.012(2) -0.008(2) 0.006(2) C12 0.044(2) 0.037(2) 0.073(3) 0.011(2) -0.010(2) 0.0102(19) C13 0.048(3) 0.041(2) 0.073(3) 0.008(2) 0.000(2) 0.007(2) C14 0.068(3) 0.044(3) 0.097(4) -0.007(3) -0.006(3) 0.014(2) C15 0.051(3) 0.050(3) 0.123(5) -0.001(3) -0.019(3) -0.003(2) C16 0.043(3) 0.063(3) 0.097(4) 0.014(3) -0.007(3) 0.010(2) C17 0.045(3) 0.054(3) 0.073(3) 0.014(2) 0.002(2) 0.014(2) C18 0.037(2) 0.040(2) 0.075(3) 0.018(2) -0.003(2) 0.0165(19) C101 0.082(4) 0.090(4) 0.093(4) 0.036(4) -0.010(3) 0.007(3) C102 0.092(5) 0.082(4) 0.117(5) 0.036(4) -0.010(4) 0.012(4) C103 0.099(5) 0.098(5) 0.084(4) 0.018(4) -0.012(4) 0.005(4) C104 0.091(5) 0.096(5) 0.085(4) 0.031(4) -0.015(3) 0.007(4) C105 0.068(4) 0.083(4) 0.082(4) 0.035(3) -0.014(3) -0.003(3) S1 0.0432(7) 0.0387(6) 0.0741(8) 0.0028(5) -0.0105(5) 0.0158(5) O101 0.081(3) 0.080(2) 0.088(3) 0.029(2) 0.007(2) 0.045(2) O102 0.058(2) 0.059(2) 0.084(2) 0.0107(17) 0.0257(17) 0.0238(16) O103 0.061(2) 0.0449(18) 0.107(3) -0.0163(17) -0.0196(19) 0.0165(16) O104 0.0421(18) 0.0390(16) 0.095(2) -0.0028(15) -0.0088(16) 0.0077(13) _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 N11A C15A 1.332(6) . ? N11A C11A 1.338(6) . ? N11A H11N 0.8598 . ? N21A C21A 1.320(7) . ? N21A C25A 1.324(7) . ? N21A H21N 0.8593 . ? C11A C12A 1.367(7) . ? C11A H11A 0.9300 . ? C12A C13A 1.392(6) . ? C12A H12A 0.9300 . ? C13A C14A 1.379(6) . ? C13A C23A 1.497(6) . ? C14A C15A 1.366(6) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? C21A C22A 1.369(7) . ? C21A H21A 0.9300 . ? C22A C23A 1.410(6) . ? C22A H22A 0.9300 . ? C23A C24A 1.377(6) . ? C24A C25A 1.362(7) . ? C24A H24A 0.9300 . ? C25A H25A 0.9300 . ? N11B C11B 1.297(6) . ? N11B C15B 1.320(8) . ? N11B H12N 0.8591 . ? C11B C12B 1.361(7) . ? C11B H11B 0.9300 . ? C12B C13B 1.370(7) . ? C12B H12B 0.9300 . ? C13B C14B 1.356(7) . ? C13B C13B 1.473(9) 2_655 ? C14B C15B 1.368(8) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? S2 O16 1.438(4) . ? S2 O17 1.447(4) . ? S2 O15 1.468(4) . ? S2 C13 1.787(5) . ? O11 C17 1.311(5) . ? O11 H11O 0.7899 . ? O12 C17 1.205(5) . ? O13 C18 1.196(5) . ? O14 C18 1.332(5) . ? O14 H14O 0.8291 . ? C11 C16 1.380(6) . ? C11 C12 1.402(6) . ? C11 C17 1.500(6) . ? C12 C13 1.397(6) . ? C12 C18 1.498(6) . ? C13 C14 1.386(6) . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C101 C102 1.351(9) . ? C101 C105 1.407(8) . ? C101 H101 0.9300 . ? C102 C103 1.423(8) . ? C102 H102 0.9300 . ? C103 C104 1.353(8) . ? C103 H103 0.9300 . ? C104 C105 1.406(8) 2_755 ? C104 H104 0.9300 . ? C105 C104 1.406(8) 2_755 ? C105 C105 1.409(10) 2_755 ? S1 O103 1.436(3) . ? S1 O101 1.446(4) . ? S1 O102 1.485(3) . ? S1 O104 1.502(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15A N11A C11A 121.4(4) . . ? C15A N11A H11N 119.3 . . ? C11A N11A H11N 119.3 . . ? C21A N21A C25A 122.2(4) . . ? C21A N21A H21N 119.0 . . ? C25A N21A H21N 118.9 . . ? N11A C11A C12A 120.4(4) . . ? N11A C11A H11A 119.8 . . ? C12A C11A H11A 119.8 . . ? C11A C12A C13A 119.5(4) . . ? C11A C12A H12A 120.2 . . ? C13A C12A H12A 120.2 . . ? C14A C13A C12A 118.3(4) . . ? C14A C13A C23A 120.6(4) . . ? C12A C13A C23A 121.1(4) . . ? C15A C14A C13A 120.1(4) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? N11A C15A C14A 120.3(4) . . ? N11A C15A H15A 119.8 . . ? C14A C15A H15A 119.8 . . ? N21A C21A C22A 120.3(5) . . ? N21A C21A H21A 119.9 . . ? C22A C21A H21A 119.9 . . ? C21A C22A C23A 119.4(5) . . ? C21A C22A H22A 120.3 . . ? C23A C22A H22A 120.3 . . ? C24A C23A C22A 117.3(4) . . ? C24A C23A C13A 122.0(4) . . ? C22A C23A C13A 120.7(4) . . ? C25A C24A C23A 120.5(5) . . ? C25A C24A H24A 119.7 . . ? C23A C24A H24A 119.7 . . ? N21A C25A C24A 120.2(5) . . ? N21A C25A H25A 119.9 . . ? C24A C25A H25A 119.9 . . ? C11B N11B C15B 120.6(5) . . ? C11B N11B H12N 119.7 . . ? C15B N11B H12N 119.7 . . ? N11B C11B C12B 121.2(5) . . ? N11B C11B H11B 119.4 . . ? C12B C11B H11B 119.4 . . ? C11B C12B C13B 120.5(5) . . ? C11B C12B H12B 119.8 . . ? C13B C12B H12B 119.8 . . ? C14B C13B C12B 116.6(5) . . ? C14B C13B C13B 122.9(5) . 2_655 ? C12B C13B C13B 120.5(5) . 2_655 ? C13B C14B C15B 121.0(6) . . ? C13B C14B H14B 119.5 . . ? C15B C14B H14B 119.5 . . ? N11B C15B C14B 120.1(5) . . ? N11B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? O16 S2 O17 113.8(2) . . ? O16 S2 O15 113.0(2) . . ? O17 S2 O15 111.2(2) . . ? O16 S2 C13 105.6(2) . . ? O17 S2 C13 106.8(2) . . ? O15 S2 C13 105.7(2) . . ? C17 O11 H11O 109.5 . . ? C18 O14 H14O 107.8 . . ? C16 C11 C12 120.4(4) . . ? C16 C11 C17 119.5(4) . . ? C12 C11 C17 120.1(4) . . ? C13 C12 C11 118.0(4) . . ? C13 C12 C18 121.8(4) . . ? C11 C12 C18 120.2(4) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 S2 116.2(4) . . ? C12 C13 S2 122.8(3) . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 120.9(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O12 C17 O11 123.1(4) . . ? O12 C17 C11 123.5(4) . . ? O11 C17 C11 113.4(4) . . ? O13 C18 O14 124.7(4) . . ? O13 C18 C12 123.5(4) . . ? O14 C18 C12 111.7(4) . . ? C102 C101 C105 122.3(6) . . ? C102 C101 H101 118.9 . . ? C105 C101 H101 118.9 . . ? C101 C102 C103 119.1(6) . . ? C101 C102 H102 120.5 . . ? C103 C102 H102 120.5 . . ? C104 C103 C102 120.1(7) . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C105 121.2(6) . 2_755 ? C103 C104 H104 119.4 . . ? C105 C104 H104 119.4 2_755 . ? C101 C105 C104 122.7(5) . 2_755 ? C101 C105 C105 118.2(8) . 2_755 ? C104 C105 C105 119.2(7) 2_755 2_755 ? O103 S1 O101 112.9(2) . . ? O103 S1 O102 110.1(2) . . ? O101 S1 O102 109.9(2) . . ? O103 S1 O104 107.14(17) . . ? O101 S1 O104 109.1(2) . . ? O102 S1 O104 107.5(2) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.351 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.077