data_global _audit_creation_date 2017-09-19 _audit_creation_method 'by CrystalStructure 4.2.2' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'ENTER NAME' _publ_contact_author_email 'ENTER EMAIL ADDRESS' _publ_contact_author_fax 'ENTER FAX NUMBER' _publ_contact_author_phone 'ENTER PHONE NUMBER' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ENTER JOURNAL NAME HERE' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2016). CrystalStructure. Version 4.2.2. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C. and Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350. SIR92 Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_170915_HTA14-172-34 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C23 H23 N3 O4 S' _chemical_formula_moiety 'C23 H23 N3 O4 S' _chemical_formula_weight 437.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 6.40981(16) _cell_length_b 7.8759(2) _cell_length_c 21.6611(6) _cell_angle_alpha 93.1783(15) _cell_angle_beta 94.9086(15) _cell_angle_gamma 105.5473(15) _cell_volume 1046.13(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4560 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 67.81 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460.00 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.919 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 17440 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_theta_max 68.248 _diffrn_reflns_theta_min 4.111 _diffrn_reflns_theta_full 67.687 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 3784 _reflns_number_gt 1510 _reflns_threshold_expression F^2^>2.0\s(F^2^) _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1894 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2065 _refine_ls_wR_factor_gt 0.1432 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3784 _refine_ls_number_parameters 281 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.52 _refine_diff_density_min -0.57 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00084(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.0492 0.0322 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.3331 0.5567 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.0059(3) 0.1079(2) 0.16190(9) 0.0540(5) Uani 1 1 d . . . . . O1 O -0.2558(8) 0.5475(7) 0.2647(2) 0.0714(16) Uani 1 1 d . . . . . O2 O 0.2325(6) 0.1385(6) 0.1527(2) 0.0523(12) Uani 1 1 d . . . . . O3 O -0.1496(7) -0.0544(6) 0.1354(2) 0.0580(13) Uani 1 1 d . . . . . O4 O 0.0851(7) 0.2554(6) 0.4754(2) 0.0569(13) Uani 1 1 d . . . . . N1 N 0.0441(8) 0.5893(7) 0.2119(2) 0.0493(15) Uani 1 1 d . . . . . N2 N -0.0727(8) 0.2724(7) 0.1340(2) 0.0436(13) Uani 1 1 d . . . . . N3 N -0.1928(9) 0.1469(8) 0.5322(3) 0.0616(17) Uani 1 1 d . . . . . C1 C -0.1783(11) 0.5336(10) 0.2154(3) 0.0569(19) Uani 1 1 d . . . . . C2 C -0.3169(11) 0.4577(9) 0.1549(3) 0.0556(19) Uani 1 1 d . . . . . H1A H -0.2698 0.5375 0.1219 0.067 Uiso 1 1 calc R U . . . H2B H -0.4707 0.4522 0.1598 0.067 Uiso 1 1 calc R U . . . C3 C -0.3016(9) 0.2732(9) 0.1346(3) 0.0521(18) Uani 1 1 d . . . . . H3B H -0.3722 0.1882 0.1637 0.063 Uiso 1 1 calc R U . . . H4A H -0.3794 0.2353 0.0926 0.063 Uiso 1 1 calc R U . . . C4 C 0.0825(10) 0.4257(9) 0.1154(3) 0.0468(17) Uani 1 1 d . . . . . C5 C 0.1653(10) 0.4183(9) 0.0577(3) 0.0495(18) Uani 1 1 d . . . . . C6 C 0.3070(10) 0.5742(9) 0.0410(3) 0.0519(18) Uani 1 1 d . . . . . H5 H 0.3642 0.5747 0.0019 0.062 Uiso 1 1 calc R U . . . C7 C 0.3643(10) 0.7263(9) 0.0803(3) 0.0568(19) Uani 1 1 d . . . . . H6 H 0.4648 0.8287 0.0686 0.068 Uiso 1 1 calc R U . . . C8 C 0.2791(10) 0.7335(9) 0.1366(3) 0.0537(18) Uani 1 1 d . . . . . H7 H 0.3195 0.8399 0.1630 0.064 Uiso 1 1 calc R U . . . C9 C 0.1332(10) 0.5829(9) 0.1541(3) 0.0476(17) Uani 1 1 d . . . . . C10 C 0.1853(11) 0.6778(10) 0.2678(3) 0.065(2) Uani 1 1 d . . . . . H11A H 0.1033 0.7356 0.2942 0.078 Uiso 1 1 calc R U . . . H12B H 0.3108 0.7668 0.2557 0.078 Uiso 1 1 calc R U . . . H13C H 0.2361 0.5904 0.2908 0.078 Uiso 1 1 calc R U . . . C11 C 0.1122(11) 0.2486(9) 0.0161(3) 0.059(2) Uani 1 1 d . . . . . H8B H 0.2159 0.1814 0.0278 0.071 Uiso 1 1 calc R U . . . H9C H 0.1221 0.2764 -0.0272 0.071 Uiso 1 1 calc R U . . . H10A H -0.0358 0.1779 0.0209 0.071 Uiso 1 1 calc R U . . . C12 C -0.0184(10) 0.1197(9) 0.2420(3) 0.0479(17) Uani 1 1 d . . . . . C13 C -0.2069(10) 0.0272(9) 0.2647(3) 0.058(2) Uani 1 1 d . . . . . H14 H -0.3223 -0.0464 0.2368 0.070 Uiso 1 1 calc R U . . . C14 C -0.2296(11) 0.0404(10) 0.3274(3) 0.062(2) Uani 1 1 d . . . . . H15 H -0.3618 -0.0213 0.3423 0.074 Uiso 1 1 calc R U . . . C15 C -0.0594(11) 0.1438(9) 0.3687(3) 0.0538(18) Uani 1 1 d . . . . . C16 C 0.1316(10) 0.2338(9) 0.3465(3) 0.060(2) Uani 1 1 d . . . . . H16 H 0.2490 0.3035 0.3747 0.072 Uiso 1 1 calc R U . . . C17 C 0.1531(11) 0.2230(9) 0.2827(3) 0.0569(19) Uani 1 1 d . . . . . H17 H 0.2842 0.2858 0.2675 0.068 Uiso 1 1 calc R U . . . C18 C -0.0893(11) 0.1547(9) 0.4346(3) 0.0548(19) Uani 1 1 d . . . . . C19 C -0.2530(11) 0.0913(9) 0.4689(3) 0.059(2) Uani 1 1 d . . . . . H18 H -0.3922 0.0179 0.4525 0.070 Uiso 1 1 calc R U . . . C20 C 0.0088(12) 0.2431(9) 0.5334(3) 0.0564(19) Uani 1 1 d . . . . . C21 C 0.1565(11) 0.3326(10) 0.5869(3) 0.062(2) Uani 1 1 d . . . . . H19 H 0.0989 0.3107 0.6281 0.074 Uiso 1 1 calc R U . . . C22 C 0.3057(12) 0.5147(10) 0.5828(4) 0.071(2) Uani 1 1 d . . . . . H20A H 0.3021 0.5672 0.5424 0.085 Uiso 1 1 calc R U . . . H21B H 0.3318 0.6003 0.6198 0.085 Uiso 1 1 calc R U . . . C23 C 0.3991(11) 0.3604(9) 0.5872(3) 0.063(2) Uani 1 1 d . . . . . H22A H 0.4826 0.3509 0.6269 0.075 Uiso 1 1 calc R U . . . H23B H 0.4530 0.3178 0.5495 0.075 Uiso 1 1 calc R U . . . 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 0.0400(10) 0.0542(12) 0.0642(12) 0.0001(9) 0.0052(8) 0.0077(8) O1 0.059(3) 0.097(4) 0.058(3) -0.007(3) 0.015(3) 0.022(3) O2 0.022(2) 0.059(3) 0.076(3) 0.006(2) 0.014(2) 0.009(2) O3 0.045(3) 0.045(3) 0.073(3) -0.008(2) 0.000(2) -0.004(2) O4 0.051(3) 0.065(3) 0.052(3) 0.003(2) 0.007(2) 0.010(2) N1 0.032(3) 0.064(4) 0.049(3) -0.004(3) 0.006(3) 0.010(3) N2 0.034(3) 0.041(3) 0.060(4) 0.010(3) 0.001(2) 0.017(2) N3 0.051(4) 0.071(4) 0.061(4) 0.004(3) 0.007(3) 0.013(3) C1 0.047(4) 0.066(5) 0.057(5) 0.005(4) 0.004(4) 0.015(4) C2 0.049(4) 0.054(5) 0.062(5) -0.004(4) 0.003(4) 0.014(4) C3 0.023(3) 0.066(5) 0.070(5) 0.008(4) 0.009(3) 0.016(3) C4 0.032(3) 0.042(4) 0.062(5) 0.006(3) 0.003(3) 0.001(3) C5 0.038(4) 0.054(5) 0.052(4) -0.001(3) 0.005(3) 0.006(3) C6 0.037(4) 0.058(5) 0.059(5) 0.011(4) 0.010(3) 0.009(3) C7 0.037(4) 0.053(5) 0.075(5) 0.010(4) 0.004(4) 0.003(3) C8 0.043(4) 0.052(4) 0.067(5) -0.003(4) -0.001(4) 0.016(3) C9 0.039(4) 0.045(4) 0.057(4) 0.004(3) 0.009(3) 0.009(3) C10 0.058(5) 0.073(5) 0.058(5) -0.022(4) -0.008(4) 0.016(4) C11 0.053(4) 0.062(5) 0.058(5) -0.005(4) 0.008(4) 0.008(4) C12 0.037(4) 0.054(4) 0.049(4) -0.002(3) 0.015(3) 0.006(3) C13 0.036(4) 0.067(5) 0.060(5) 0.005(4) 0.002(3) -0.006(3) C14 0.038(4) 0.075(5) 0.063(5) 0.006(4) 0.010(4) -0.002(4) C15 0.042(4) 0.054(5) 0.061(5) 0.007(4) 0.008(3) 0.005(3) C16 0.036(4) 0.068(5) 0.066(5) 0.001(4) 0.004(3) 0.000(4) C17 0.043(4) 0.064(5) 0.059(5) 0.007(4) 0.004(3) 0.007(4) C18 0.045(4) 0.056(5) 0.057(5) 0.003(4) 0.004(3) 0.004(3) C19 0.044(4) 0.063(5) 0.066(5) 0.012(4) 0.010(4) 0.008(4) C20 0.051(4) 0.055(5) 0.064(5) 0.005(4) 0.009(4) 0.015(4) C21 0.052(4) 0.064(5) 0.061(5) -0.004(4) -0.001(4) 0.005(4) C22 0.066(5) 0.067(6) 0.080(6) -0.004(4) 0.001(4) 0.023(4) C23 0.051(4) 0.064(5) 0.071(5) 0.001(4) 0.004(4) 0.014(4) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.2.2 (Rigaku, 2016)' _computing_molecular_graphics 'CrystalStructure 4.2.2' #============================================================================== # MOLECULAR GEOMETRY _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 O2 1.440(4) . ? S1 O3 1.447(4) . ? S1 N2 1.638(5) . ? S1 C12 1.755(6) . ? O1 C1 1.228(7) . ? O4 C20 1.385(8) . ? O4 C18 1.392(7) . ? N1 C1 1.385(8) . ? N1 C9 1.424(7) . ? N1 C10 1.467(7) . ? N2 C4 1.445(7) . ? N2 C3 1.470(6) . ? N3 C20 1.308(8) . ? N3 C19 1.405(8) . ? C1 C2 1.515(9) . ? C2 C3 1.526(8) . ? C2 H1A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3B 0.9900 . ? C3 H4A 0.9900 . ? C4 C5 1.402(8) . ? C4 C9 1.402(8) . ? C5 C6 1.405(8) . ? C5 C11 1.511(8) . ? C6 C7 1.376(9) . ? C6 H5 0.9500 . ? C7 C8 1.382(9) . ? C7 H6 0.9500 . ? C8 C9 1.393(8) . ? C8 H7 0.9500 . ? C10 H11A 0.9800 . ? C10 H12B 0.9800 . ? C10 H13C 0.9800 . ? C11 H8B 0.9800 . ? C11 H9C 0.9800 . ? C11 H10A 0.9800 . ? C12 C13 1.379(8) . ? C12 C17 1.387(8) . ? C13 C14 1.379(9) . ? C13 H14 0.9500 . ? C14 C15 1.389(8) . ? C14 H15 0.9500 . ? C15 C16 1.380(8) . ? C15 C18 1.458(9) . ? C16 C17 1.401(9) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.341(8) . ? C19 H18 0.9500 . ? C20 C21 1.449(9) . ? C21 C22 1.507(9) . ? C21 C23 1.511(9) . ? C21 H19 1.0000 . ? C22 C23 1.496(9) . ? C22 H20A 0.9900 . ? C22 H21B 0.9900 . ? C23 H22A 0.9900 . ? C23 H23B 0.9900 . ? 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 S1 O3 119.6(3) . . ? O2 S1 N2 106.8(3) . . ? O3 S1 N2 107.4(3) . . ? O2 S1 C12 108.8(3) . . ? O3 S1 C12 106.5(3) . . ? N2 S1 C12 107.0(3) . . ? C20 O4 C18 104.6(5) . . ? C1 N1 C9 121.4(5) . . ? C1 N1 C10 118.3(6) . . ? C9 N1 C10 119.8(5) . . ? C4 N2 C3 119.2(5) . . ? C4 N2 S1 121.3(4) . . ? C3 N2 S1 119.1(4) . . ? C20 N3 C19 103.4(6) . . ? O1 C1 N1 121.3(6) . . ? O1 C1 C2 122.9(6) . . ? N1 C1 C2 115.8(6) . . ? C1 C2 C3 112.5(6) . . ? C1 C2 H1A 109.1 . . ? C3 C2 H1A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H1A C2 H2B 107.8 . . ? N2 C3 C2 110.5(5) . . ? N2 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? N2 C3 H4A 109.6 . . ? C2 C3 H4A 109.6 . . ? H3B C3 H4A 108.1 . . ? C5 C4 C9 121.7(6) . . ? C5 C4 N2 119.9(6) . . ? C9 C4 N2 118.2(6) . . ? C4 C5 C6 117.2(6) . . ? C4 C5 C11 121.8(6) . . ? C6 C5 C11 121.0(6) . . ? C7 C6 C5 120.9(7) . . ? C7 C6 H5 119.5 . . ? C5 C6 H5 119.5 . . ? C6 C7 C8 121.5(7) . . ? C6 C7 H6 119.2 . . ? C8 C7 H6 119.2 . . ? C7 C8 C9 119.2(7) . . ? C7 C8 H7 120.4 . . ? C9 C8 H7 120.4 . . ? C8 C9 C4 119.3(6) . . ? C8 C9 N1 119.6(6) . . ? C4 C9 N1 121.1(6) . . ? N1 C10 H11A 109.5 . . ? N1 C10 H12B 109.5 . . ? H11A C10 H12B 109.5 . . ? N1 C10 H13C 109.5 . . ? H11A C10 H13C 109.5 . . ? H12B C10 H13C 109.5 . . ? C5 C11 H8B 109.5 . . ? C5 C11 H9C 109.5 . . ? H8B C11 H9C 109.5 . . ? C5 C11 H10A 109.5 . . ? H8B C11 H10A 109.5 . . ? H9C C11 H10A 109.5 . . ? C13 C12 C17 119.8(6) . . ? C13 C12 S1 120.4(5) . . ? C17 C12 S1 119.8(5) . . ? C12 C13 C14 120.7(6) . . ? C12 C13 H14 119.6 . . ? C14 C13 H14 119.6 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H15 120.0 . . ? C15 C14 H15 120.0 . . ? C16 C15 C14 119.6(7) . . ? C16 C15 C18 121.8(6) . . ? C14 C15 C18 118.6(6) . . ? C15 C16 C17 120.3(7) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 119.5(6) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 O4 106.8(6) . . ? C19 C18 C15 135.5(7) . . ? O4 C18 C15 117.7(6) . . ? C18 C19 N3 111.4(6) . . ? C18 C19 H18 124.3 . . ? N3 C19 H18 124.3 . . ? N3 C20 O4 113.8(6) . . ? N3 C20 C21 128.1(7) . . ? O4 C20 C21 118.1(6) . . ? C20 C21 C22 120.0(7) . . ? C20 C21 C23 120.6(7) . . ? C22 C21 C23 59.4(4) . . ? C20 C21 H19 115.1 . . ? C22 C21 H19 115.1 . . ? C23 C21 H19 115.1 . . ? C23 C22 C21 60.4(5) . . ? C23 C22 H20A 117.7 . . ? C21 C22 H20A 117.7 . . ? C23 C22 H21B 117.7 . . ? C21 C22 H21B 117.7 . . ? H20A C22 H21B 114.9 . . ? C22 C23 C21 60.2(5) . . ? C22 C23 H22A 117.8 . . ? C21 C23 H22A 117.8 . . ? C22 C23 H23B 117.8 . . ? C21 C23 H23B 117.8 . . ? H22A C23 H23B 114.9 . . ? 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 O2 S1 N2 C4 -9.6(6) . . . . ? O3 S1 N2 C4 -139.1(5) . . . . ? C12 S1 N2 C4 106.8(5) . . . . ? O2 S1 N2 C3 177.6(5) . . . . ? O3 S1 N2 C3 48.0(5) . . . . ? C12 S1 N2 C3 -66.0(5) . . . . ? C9 N1 C1 O1 -176.2(7) . . . . ? C10 N1 C1 O1 -4.4(11) . . . . ? C9 N1 C1 C2 3.1(10) . . . . ? C10 N1 C1 C2 174.9(6) . . . . ? O1 C1 C2 C3 -106.9(8) . . . . ? N1 C1 C2 C3 73.8(8) . . . . ? C4 N2 C3 C2 -35.7(8) . . . . ? S1 N2 C3 C2 137.3(5) . . . . ? C1 C2 C3 N2 -52.2(8) . . . . ? C3 N2 C4 C5 -107.8(7) . . . . ? S1 N2 C4 C5 79.4(7) . . . . ? C3 N2 C4 C9 67.4(8) . . . . ? S1 N2 C4 C9 -105.4(6) . . . . ? C9 C4 C5 C6 1.9(10) . . . . ? N2 C4 C5 C6 176.9(6) . . . . ? C9 C4 C5 C11 179.6(6) . . . . ? N2 C4 C5 C11 -5.5(10) . . . . ? C4 C5 C6 C7 1.1(10) . . . . ? C11 C5 C6 C7 -176.5(6) . . . . ? C5 C6 C7 C8 -2.4(10) . . . . ? C6 C7 C8 C9 0.6(10) . . . . ? C7 C8 C9 C4 2.4(10) . . . . ? C7 C8 C9 N1 -179.8(6) . . . . ? C5 C4 C9 C8 -3.7(10) . . . . ? N2 C4 C9 C8 -178.8(6) . . . . ? C5 C4 C9 N1 178.6(6) . . . . ? N2 C4 C9 N1 3.5(9) . . . . ? C1 N1 C9 C8 128.4(7) . . . . ? C10 N1 C9 C8 -43.3(9) . . . . ? C1 N1 C9 C4 -53.9(9) . . . . ? C10 N1 C9 C4 134.4(7) . . . . ? O2 S1 C12 C13 -152.5(6) . . . . ? O3 S1 C12 C13 -22.3(7) . . . . ? N2 S1 C12 C13 92.4(6) . . . . ? O2 S1 C12 C17 27.6(7) . . . . ? O3 S1 C12 C17 157.8(6) . . . . ? N2 S1 C12 C17 -87.5(6) . . . . ? C17 C12 C13 C14 2.0(11) . . . . ? S1 C12 C13 C14 -177.9(6) . . . . ? C12 C13 C14 C15 -1.8(12) . . . . ? C13 C14 C15 C16 0.3(12) . . . . ? C13 C14 C15 C18 180.0(7) . . . . ? C14 C15 C16 C17 0.8(11) . . . . ? C18 C15 C16 C17 -178.8(7) . . . . ? C13 C12 C17 C16 -0.8(11) . . . . ? S1 C12 C17 C16 179.1(5) . . . . ? C15 C16 C17 C12 -0.6(11) . . . . ? C20 O4 C18 C19 0.2(8) . . . . ? C20 O4 C18 C15 179.2(6) . . . . ? C16 C15 C18 C19 176.6(8) . . . . ? C14 C15 C18 C19 -3.0(14) . . . . ? C16 C15 C18 O4 -2.0(11) . . . . ? C14 C15 C18 O4 178.4(6) . . . . ? O4 C18 C19 N3 0.0(8) . . . . ? C15 C18 C19 N3 -178.8(8) . . . . ? C20 N3 C19 C18 -0.1(9) . . . . ? C19 N3 C20 O4 0.3(8) . . . . ? C19 N3 C20 C21 -178.7(7) . . . . ? C18 O4 C20 N3 -0.3(8) . . . . ? C18 O4 C20 C21 178.8(6) . . . . ? N3 C20 C21 C22 -140.0(8) . . . . ? O4 C20 C21 C22 41.0(10) . . . . ? N3 C20 C21 C23 149.9(8) . . . . ? O4 C20 C21 C23 -29.0(10) . . . . ? C20 C21 C22 C23 -110.0(8) . . . . ? C20 C21 C23 C22 109.0(8) . . . . ? #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelxl_version_number 2013-4 _shelx_res_file ; TITL 170915_HTA14-172-34 CELL 1.54187 6.40981 7.87587 21.66106 93.17830 94.90860 105.54730 ZERR 2 0.00016 0.00022 0.00059 0.00150 0.00150 0.00150 LATT 1 SFAC C H O N S UNIT 46 46 8 6 2 L.S. 10 FMAP 2 PLAN 38 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -100.0 ACTA SIZE 0.100 0.100 0.050 WGHT 0.000000 3.000000 EXTI 0.000837 FVAR 0.79792 S1 5 0.005894 0.107924 0.161896 11.00000 0.03996 0.05424 = 0.06417 0.00006 0.00520 0.00766 O1 3 -0.255804 0.547526 0.264727 11.00000 0.05901 0.09747 = 0.05803 -0.00680 0.01504 0.02168 O2 3 0.232528 0.138460 0.152744 11.00000 0.02153 0.05930 = 0.07649 0.00609 0.01372 0.00904 O3 3 -0.149604 -0.054385 0.135373 11.00000 0.04480 0.04459 = 0.07265 -0.00750 0.00025 -0.00400 O4 3 0.085064 0.255350 0.475430 11.00000 0.05085 0.06453 = 0.05204 0.00255 0.00688 0.01000 N1 4 0.044061 0.589300 0.211870 11.00000 0.03221 0.06423 = 0.04867 -0.00426 0.00562 0.00992 N2 4 -0.072670 0.272392 0.133955 11.00000 0.03396 0.04056 = 0.06041 0.01025 0.00101 0.01719 N3 4 -0.192758 0.146930 0.532243 11.00000 0.05147 0.07059 = 0.06083 0.00418 0.00653 0.01342 C1 1 -0.178316 0.533639 0.215384 11.00000 0.04694 0.06638 = 0.05683 0.00463 0.00399 0.01523 C2 1 -0.316949 0.457693 0.154880 11.00000 0.04933 0.05372 = 0.06197 -0.00380 0.00321 0.01382 AFIX 23 H1A 2 -0.269815 0.537462 0.121934 11.00000 -1.20000 H2B 2 -0.470677 0.452208 0.159830 11.00000 -1.20000 AFIX 0 C3 1 -0.301576 0.273152 0.134644 11.00000 0.02341 0.06622 = 0.06970 0.00815 0.00864 0.01555 AFIX 23 H3B 2 -0.372200 0.188230 0.163653 11.00000 -1.20000 H4A 2 -0.379424 0.235278 0.092589 11.00000 -1.20000 AFIX 0 C4 1 0.082535 0.425675 0.115356 11.00000 0.03166 0.04190 = 0.06165 0.00645 0.00318 0.00139 C5 1 0.165276 0.418265 0.057730 11.00000 0.03820 0.05440 = 0.05169 -0.00058 0.00509 0.00638 C6 1 0.307049 0.574194 0.040972 11.00000 0.03696 0.05824 = 0.05938 0.01065 0.00964 0.00855 AFIX 43 H5 2 0.364181 0.574675 0.001915 11.00000 -1.20000 AFIX 0 C7 1 0.364345 0.726290 0.080349 11.00000 0.03727 0.05317 = 0.07485 0.00951 0.00422 0.00320 AFIX 43 H6 2 0.464850 0.828666 0.068584 11.00000 -1.20000 AFIX 0 C8 1 0.279065 0.733518 0.136592 11.00000 0.04275 0.05160 = 0.06678 -0.00272 -0.00142 0.01648 AFIX 43 H7 2 0.319452 0.839931 0.163031 11.00000 -1.20000 AFIX 0 C9 1 0.133178 0.582928 0.154062 11.00000 0.03925 0.04535 = 0.05712 0.00360 0.00852 0.00858 C10 1 0.185292 0.677847 0.267774 11.00000 0.05825 0.07311 = 0.05820 -0.02159 -0.00848 0.01648 AFIX 33 H11A 2 0.103324 0.735582 0.294171 11.00000 -1.20000 H12B 2 0.310796 0.766752 0.255688 11.00000 -1.20000 H13C 2 0.236093 0.590351 0.290806 11.00000 -1.20000 AFIX 0 C11 1 0.112183 0.248561 0.016134 11.00000 0.05253 0.06203 = 0.05817 -0.00542 0.00837 0.00759 AFIX 33 H8B 2 0.215902 0.181395 0.027813 11.00000 -1.20000 H9C 2 0.122056 0.276380 -0.027242 11.00000 -1.20000 H10A 2 -0.035836 0.177870 0.020861 11.00000 -1.20000 AFIX 0 C12 1 -0.018393 0.119674 0.241992 11.00000 0.03737 0.05410 = 0.04940 -0.00161 0.01503 0.00577 C13 1 -0.206867 0.027220 0.264662 11.00000 0.03553 0.06708 = 0.06023 0.00479 0.00243 -0.00634 AFIX 43 H14 2 -0.322333 -0.046352 0.236806 11.00000 -1.20000 AFIX 0 C14 1 -0.229589 0.040396 0.327359 11.00000 0.03810 0.07504 = 0.06289 0.00633 0.00989 -0.00170 AFIX 43 H15 2 -0.361752 -0.021337 0.342309 11.00000 -1.20000 AFIX 0 C15 1 -0.059447 0.143823 0.368658 11.00000 0.04189 0.05428 = 0.06107 0.00709 0.00762 0.00477 C16 1 0.131571 0.233822 0.346545 11.00000 0.03599 0.06823 = 0.06646 0.00101 0.00440 -0.00016 AFIX 43 H16 2 0.248979 0.303465 0.374712 11.00000 -1.20000 AFIX 0 C17 1 0.153143 0.222956 0.282744 11.00000 0.04251 0.06449 = 0.05914 0.00699 0.00446 0.00675 AFIX 43 H17 2 0.284206 0.285816 0.267501 11.00000 -1.20000 AFIX 0 C18 1 -0.089294 0.154746 0.434608 11.00000 0.04490 0.05645 = 0.05677 0.00333 0.00373 0.00378 C19 1 -0.253042 0.091272 0.468950 11.00000 0.04415 0.06350 = 0.06609 0.01188 0.01015 0.00787 AFIX 43 H18 2 -0.392218 0.017935 0.452543 11.00000 -1.20000 AFIX 0 C20 1 0.008779 0.243085 0.533406 11.00000 0.05112 0.05546 = 0.06355 0.00484 0.00905 0.01515 C21 1 0.156508 0.332639 0.586913 11.00000 0.05199 0.06380 = 0.06120 -0.00434 -0.00137 0.00499 AFIX 13 H19 2 0.098902 0.310710 0.628066 11.00000 -1.20000 AFIX 0 C22 1 0.305689 0.514724 0.582844 11.00000 0.06638 0.06739 = 0.08014 -0.00377 0.00127 0.02264 AFIX 23 H20A 2 0.302111 0.567247 0.542422 11.00000 -1.20000 H21B 2 0.331781 0.600310 0.619804 11.00000 -1.20000 AFIX 0 C23 1 0.399120 0.360444 0.587202 11.00000 0.05094 0.06410 = 0.07099 0.00144 0.00397 0.01432 AFIX 23 H22A 2 0.482641 0.350886 0.626855 11.00000 -1.20000 H23B 2 0.452966 0.317818 0.549462 11.00000 -1.20000 AFIX 0 HKLF 4 REM 170915_HTA14-172-34 REM R1 = 0.0846 for 1510 Fo > 4sig(Fo) and 0.1894 for all 3784 data REM 281 parameters refined using 0 restraints END WGHT 0.1094 2.0594 REM Instructions for potential hydrogen bonds EQIV $1 x-1, y, z HTAB C3 O2_$1 EQIV $2 x, y+1, z HTAB C8 O2_$2 EQIV $3 -x-1, -y, -z+1 HTAB C19 N3_$3 EQIV $4 -x, -y+1, -z+1 HTAB C21 O1_$4 REM Highest difference peak 0.524, deepest hole -0.569, 1-sigma level 0.108 Q1 1 -0.2292 0.0963 0.1698 11.00000 0.05 0.52 Q2 1 0.2231 0.1022 0.1911 11.00000 0.05 0.50 Q3 1 -0.1227 0.0140 0.0558 11.00000 0.05 0.49 Q4 1 0.0413 0.2929 0.2011 11.00000 0.05 0.49 Q5 1 0.0460 0.0125 0.0577 11.00000 0.05 0.48 Q6 1 0.1466 -0.0448 0.1709 11.00000 0.05 0.46 Q7 1 -0.1237 0.2490 0.5904 11.00000 0.05 0.45 Q8 1 0.1976 0.8542 0.2767 11.00000 0.05 0.45 Q9 1 0.0212 0.1482 0.1728 11.00000 0.05 0.43 Q10 1 0.3963 0.6797 0.2543 11.00000 0.05 0.43 Q11 1 -0.0658 0.1379 0.2219 11.00000 0.05 0.42 Q12 1 0.0446 0.6192 0.3088 11.00000 0.05 0.42 Q13 1 -0.0992 0.0198 0.1520 11.00000 0.05 0.42 Q14 1 0.0757 0.1107 0.0970 11.00000 0.05 0.41 Q15 1 0.3037 0.2884 0.4684 11.00000 0.05 0.39 Q16 1 0.1719 0.3007 0.1609 11.00000 0.05 0.38 Q17 1 -0.5037 0.2618 0.1672 11.00000 0.05 0.37 Q18 1 -0.0562 0.3736 0.2302 11.00000 0.05 0.37 Q19 1 0.1154 0.4631 0.4593 11.00000 0.05 0.36 Q20 1 0.0105 0.1324 0.1448 11.00000 0.05 0.35 Q21 1 -0.3284 0.6783 0.1393 11.00000 0.05 0.35 Q22 1 0.4088 0.1249 0.1930 11.00000 0.05 0.35 Q23 1 -0.3452 0.3740 0.0735 11.00000 0.05 0.35 Q24 1 -0.2113 0.7130 0.3050 11.00000 0.05 0.34 Q25 1 0.1112 0.1575 0.2218 11.00000 0.05 0.34 Q26 1 0.0777 0.8865 0.3158 11.00000 0.05 0.34 Q27 1 -0.5466 0.1331 0.1384 11.00000 0.05 0.34 Q28 1 0.0811 -0.0192 0.1128 11.00000 0.05 0.34 Q29 1 0.1814 0.2776 0.1330 11.00000 0.05 0.33 Q30 1 -0.0975 0.0621 0.0915 11.00000 0.05 0.33 Q31 1 -0.2307 0.2031 0.2107 11.00000 0.05 0.33 Q32 1 0.0690 0.7061 0.1541 11.00000 0.05 0.33 Q33 1 -0.0312 -0.0842 0.1980 11.00000 0.05 0.33 Q34 1 0.3439 0.2253 0.1238 11.00000 0.05 0.32 Q35 1 0.0161 0.5719 0.0941 11.00000 0.05 0.32 Q36 1 0.0280 0.2475 0.1266 11.00000 0.05 0.32 Q37 1 0.0072 0.0874 0.1792 11.00000 0.05 0.32 Q38 1 -0.1834 -0.2441 0.1276 11.00000 0.05 0.31 ; _shelx_res_checksum 47284 _shelx_hkl_file ; 0 0 2 140.26 7.51 0 0 2 132.11 7.53 0 0 2 130.20 5.64 0 0 2 126.03 5.88 0 0 2 135.88 10.36 0 0 2 140.22 5.65 0 0 2 141.79 7.99 0 0 2 136.95 7.03 0 0 -2 128.56 7.22 0 0 -2 134.97 6.11 0 0 -2 136.92 5.66 0 0 -2 124.93 6.70 0 0 -2 135.61 6.86 0 0 -2 128.76 7.80 0 0 -2 135.38 6.84 0 0 -2 133.67 7.23 0 0 3 4954.04 256.98 0 0 3 5124.43 259.12 0 0 3 5207.32 244.36 0 0 3 4949.55 254.20 0 0 3 5827.35 281.19 0 0 3 5023.53 256.08 0 0 3 5252.89 265.29 0 0 -3 5272.32 269.42 0 0 -3 4953.09 251.12 0 0 -3 5442.58 268.19 0 0 -3 5165.52 257.32 0 0 -3 4992.87 249.59 0 0 -3 5374.29 265.27 0 0 4 522.13 32.14 0 0 4 434.06 19.99 0 0 4 420.92 25.17 0 0 4 422.50 27.12 0 0 4 433.84 26.19 0 0 4 401.29 24.94 0 0 -4 435.23 24.84 0 0 -4 416.12 25.40 0 0 -4 433.42 24.98 0 0 -4 434.44 25.04 0 0 -4 444.86 29.83 0 0 -4 415.10 36.15 0 0 5 68.92 13.27 0 0 5 57.48 12.93 0 0 5 63.32 12.95 0 0 5 74.18 16.62 0 0 5 65.83 12.76 0 0 5 69.39 14.88 0 0 -5 68.25 13.36 0 0 -5 57.44 22.86 0 0 -5 68.46 12.83 0 0 -5 65.75 10.18 0 0 -5 74.16 12.48 0 0 -5 68.78 12.81 0 0 6 272.29 25.20 0 0 6 291.56 21.97 0 0 6 270.63 23.88 0 0 6 250.37 22.14 0 0 6 263.93 25.04 0 0 6 262.61 26.12 0 0 6 264.56 28.25 0 0 -6 265.62 24.73 0 0 -6 265.50 20.10 0 0 -6 279.89 24.33 0 0 -6 265.21 38.58 0 0 -6 266.76 26.31 0 0 -6 283.32 25.39 0 0 7 3051.10 178.96 0 0 7 3138.86 179.04 0 0 7 3168.90 184.37 0 0 7 3159.54 190.98 0 0 7 3384.38 179.78 0 0 7 3056.24 155.72 0 0 7 3194.39 187.20 0 0 -7 3333.87 188.36 0 0 -7 3247.92 190.90 0 0 -7 3301.92 185.63 0 0 -7 3132.41 186.09 0 0 -7 3026.82 164.85 0 0 -7 3118.25 178.40 0 0 8 682.07 45.53 0 0 8 716.86 42.17 0 0 8 731.51 48.64 0 0 8 771.11 54.97 0 0 8 679.38 47.74 0 0 8 696.21 37.41 0 0 8 710.59 50.73 0 0 8 755.73 44.38 0 0 -8 783.20 50.88 0 0 -8 747.62 51.66 0 0 -8 729.44 42.11 0 0 -8 707.13 47.79 0 0 -8 688.58 41.12 0 0 -8 727.19 61.13 0 0 -8 736.67 50.96 0 0 9 386.68 26.75 0 0 9 395.89 33.86 0 0 9 381.99 35.00 0 0 9 377.01 31.13 0 0 9 368.37 23.81 0 0 9 411.81 29.79 0 0 9 380.54 33.45 0 0 -9 400.75 33.06 0 0 -9 389.98 36.31 0 0 -9 392.73 34.43 0 0 -9 378.79 26.99 0 0 -9 414.91 34.59 0 0 -9 349.02 34.42 0 0 -9 394.47 26.48 0 0 -9 401.84 43.72 0 0 10 2261.81 150.30 0 0 10 2533.18 165.67 0 0 10 2493.03 166.08 0 0 10 2416.65 144.62 0 0 10 2356.51 138.66 0 0 10 2071.03 127.89 0 0 10 2450.12 159.77 0 0 -10 2711.59 171.26 0 0 -10 2568.94 168.90 0 0 -10 2649.47 164.35 0 0 -10 2420.36 141.90 0 0 -10 2445.38 161.63 0 0 -10 2469.70 142.70 0 0 -10 2380.95 159.19 0 0 -10 2490.12 156.88 0 0 11 45.74 9.07 0 0 11 85.42 11.70 0 0 11 105.26 17.82 0 0 11 83.09 24.57 0 0 11 84.73 11.42 0 0 11 46.66 11.36 0 0 11 88.36 18.58 0 0 11 73.77 14.88 0 0 -11 91.77 17.14 0 0 -11 79.64 16.55 0 0 -11 85.47 15.29 0 0 -11 85.93 24.69 0 0 -11 87.48 12.03 0 0 -11 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