data_22dub_vj01_2 _audit_creation_date 2022-01-18 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email _audit_author_address 'Josef, V.' nena.josef@fau.de ; OC1-Dube DCP ; 'Hampel, F.' ? ? _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C17 H10 O2 S' _chemical_formula_sum 'C17 H10 O2 S' _chemical_formula_weight 278.31 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula 'C17 H10 O2 S' 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 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 29 _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 28.1928(11) _cell_length_b 3.8475(2) _cell_length_c 11.3330(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1229.31(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1718 _cell_measurement_temperature 153.00(10) _cell_measurement_theta_max 71.9420 _cell_measurement_theta_min 3.0920 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.314 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear orangish red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier orangish _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 576 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 14 0 5 0.0399 6 2 1 0.0817 -14 0 -5 0.0125 -16 0 -3 0.0084 -3 -2 1 0.1136 -3 0 -7 0.0318 3 0 7 0.0318 12 0 -6 0.0361 -12 0 6 0.0361 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of n-heptane and DCM by solvent layering' _exptl_crystal_size_max 0.207 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.054 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 13.8712 -0.1077 4.7810 -0.1224 -0.9395 0.3199 6.3145 2.3078 1.2084 -0.0811 -0.6098 -0.7884 -13.7086 0.2815 -4.7968 0.1191 0.9150 -0.3856 -16.1011 -0.1205 -3.4665 0.3264 0.9228 -0.2050 -3.0743 -2.4538 0.6426 0.1166 0.3351 0.9349 -2.8589 -0.1595 -7.2477 -0.5535 0.8047 -0.2149 2.8589 0.1595 7.2477 0.5535 -0.8047 0.2149 11.7523 -0.2382 -5.5951 -0.9915 0.1298 -0.0091 -11.7523 0.2382 5.5951 0.9915 -0.1298 0.0091 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_unetI/netI 0.0329 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3355 _diffrn_reflns_point_group_measured_fraction_full 0.765 _diffrn_reflns_point_group_measured_fraction_max 0.741 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.121 _diffrn_reflns_theta_min 3.135 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 153.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6144 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -111.00 -18.00 1.00 1.60 -- -42.18 -38.00-120.00 93 2 \w 26.00 76.00 1.00 1.60 -- 42.18 -99.00 -90.00 50 3 \w 32.00 58.00 1.00 1.60 -- 42.18-125.00-150.00 26 4 \w 102.00 128.00 1.00 6.39 -- 104.13 125.00 -30.00 26 5 \w 41.00 127.00 1.00 6.39 -- 104.13 -45.00-120.00 86 6 \w 28.00 84.00 1.00 6.39 -- 104.13 -94.00 150.00 56 7 \w 124.00 168.00 1.00 6.39 -- 104.13 125.00-150.00 44 8 \w 31.00 127.00 1.00 6.39 -- 104.13 -45.00 150.00 96 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0401986000 _diffrn_orient_matrix_UB_12 0.0268563000 _diffrn_orient_matrix_UB_13 0.0916291000 _diffrn_orient_matrix_UB_21 -0.0361594000 _diffrn_orient_matrix_UB_22 -0.1159484000 _diffrn_orient_matrix_UB_23 -0.0942091000 _diffrn_orient_matrix_UB_31 0.0080802000 _diffrn_orient_matrix_UB_32 -0.3820119000 _diffrn_orient_matrix_UB_33 0.0348698000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.436 _reflns_Friedel_fraction_full 0.504 _reflns_Friedel_fraction_max 0.476 _reflns_number_gt 1703 _reflns_number_total 1794 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.260 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.047 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 1794 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0322 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0449P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.0856 _refine_special_details 'Chiral Space Group!' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C14(H14), C15(H15), C16(H16), C17(H17), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 S12 S 0.38889(2) 0.73776(17) 0.57898(8) 0.0214(2) Uani 1 1 d . . . . . O19 O 0.33638(8) 0.2361(6) 0.3130(2) 0.0306(6) Uani 1 1 d . . . . . O22 O 0.48630(7) 0.7649(5) 0.4983(2) 0.0231(5) Uani 1 1 d . . . . . C1 C 0.42922(10) 0.4982(8) 0.3697(3) 0.0230(6) Uani 1 1 d . . . . . H1 H 0.423898 0.387428 0.297980 0.028 Uiso 1 1 calc R U . . . C11 C 0.39112(10) 0.5351(8) 0.4396(3) 0.0225(6) Uani 1 1 d . . . . . C13 C 0.32717(9) 0.6583(7) 0.5906(3) 0.0218(6) Uani 1 1 d . . . . . C14 C 0.29892(11) 0.7591(7) 0.6855(3) 0.0249(7) Uani 1 1 d . . . . . H14 H 0.311921 0.872535 0.750336 0.030 Uiso 1 1 calc R U . . . C15 C 0.25064(12) 0.6850(8) 0.6802(3) 0.0271(6) Uani 1 1 d . . . . . H15 H 0.231006 0.752502 0.742063 0.033 Uiso 1 1 calc R U . . . C16 C 0.23133(9) 0.5114(7) 0.5839(3) 0.0267(6) Uani 1 1 d . . . . . H16 H 0.199022 0.462824 0.582157 0.032 Uiso 1 1 calc R U . . . C17 C 0.25971(10) 0.4107(8) 0.4908(3) 0.0255(6) Uani 1 1 d . . . . . H17 H 0.246723 0.293415 0.426725 0.031 Uiso 1 1 calc R U . . . C18 C 0.30806(10) 0.4864(8) 0.4938(3) 0.0215(6) Uani 1 1 d . . . . . C19 C 0.34347(10) 0.3994(7) 0.4040(3) 0.0225(6) Uani 1 1 d . . . . . C21 C 0.47681(10) 0.6068(7) 0.3912(3) 0.0220(6) Uani 1 1 d . . . . . C23 C 0.53403(9) 0.8437(8) 0.4969(3) 0.0220(6) Uani 1 1 d . . . . . C24 C 0.55824(10) 1.0038(8) 0.5870(3) 0.0245(6) Uani 1 1 d . . . . . H24 H 0.543256 1.072275 0.656294 0.029 Uiso 1 1 calc R U . . . C25 C 0.60662(10) 1.0577(8) 0.5685(3) 0.0268(6) Uani 1 1 d . . . . . H25 H 0.624746 1.162089 0.627153 0.032 Uiso 1 1 calc R U . . . C26 C 0.62824(10) 0.9567(8) 0.4626(3) 0.0266(6) Uani 1 1 d . . . . . H26 H 0.660453 0.998560 0.452125 0.032 Uiso 1 1 calc R U . . . C27 C 0.60302(11) 0.7965(8) 0.3731(3) 0.0235(6) Uani 1 1 d . . . . . H27 H 0.617888 0.729820 0.303426 0.028 Uiso 1 1 calc R U . . . C28 C 0.55429(11) 0.7371(7) 0.3904(3) 0.0210(6) Uani 1 1 d . . . . . C29 C 0.51666(10) 0.5823(8) 0.3235(3) 0.0221(6) Uani 1 1 d . . . . . H29 H 0.518967 0.484365 0.248733 0.027 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 S12 0.0187(3) 0.0269(3) 0.0185(3) -0.0018(3) -0.0005(3) -0.0019(2) O19 0.0247(12) 0.0430(14) 0.0243(12) -0.0113(10) -0.0031(9) -0.0005(9) O22 0.0190(10) 0.0306(11) 0.0197(11) -0.0012(9) 0.0015(8) -0.0009(7) C1 0.0215(13) 0.0272(14) 0.0204(14) 0.0011(12) -0.0010(11) 0.0004(10) C11 0.0220(13) 0.0242(14) 0.0214(16) 0.0000(13) -0.0025(10) -0.0002(11) C13 0.0191(11) 0.0222(12) 0.0240(15) 0.0029(14) -0.0015(12) -0.0018(10) C14 0.0254(15) 0.0293(16) 0.0200(16) -0.0011(12) -0.0004(13) 0.0024(10) C15 0.0273(14) 0.0277(15) 0.0263(17) 0.0015(13) 0.0061(12) 0.0025(12) C16 0.0197(11) 0.0288(13) 0.0317(16) 0.0029(16) -0.0006(14) -0.0002(10) C17 0.0230(13) 0.0284(15) 0.0251(17) -0.0007(14) -0.0032(12) -0.0021(11) C18 0.0214(13) 0.0240(13) 0.0190(15) 0.0028(12) -0.0003(11) 0.0019(10) C19 0.0201(12) 0.0241(14) 0.0234(15) 0.0007(13) -0.0011(11) 0.0012(10) C21 0.0233(13) 0.0238(14) 0.0188(14) 0.0018(12) -0.0001(11) 0.0006(10) C23 0.0198(12) 0.0246(13) 0.0217(15) 0.0044(13) 0.0004(11) 0.0021(11) C24 0.0278(13) 0.0279(13) 0.0176(13) -0.0002(14) -0.0004(13) 0.0021(11) C25 0.0266(13) 0.0299(15) 0.0238(17) 0.0010(14) -0.0047(12) -0.0026(11) C26 0.0187(11) 0.0304(15) 0.0307(16) 0.0057(14) 0.0000(12) 0.0008(11) C27 0.0198(13) 0.0296(14) 0.0212(16) 0.0036(13) 0.0040(12) 0.0036(11) C28 0.0218(14) 0.0227(14) 0.0185(15) 0.0031(12) 0.0007(11) 0.0034(9) C29 0.0205(12) 0.0263(14) 0.0195(14) 0.0020(12) 0.0006(11) 0.0036(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S12 C11 1.762(3) . ? S12 C13 1.772(3) . ? O19 C19 1.224(4) . ? O22 C21 1.384(4) . ? O22 C23 1.379(3) . ? C1 H1 0.9300 . ? C1 C11 1.343(4) . ? C1 C21 1.426(4) . ? C11 C19 1.497(4) . ? C13 C14 1.393(5) . ? C13 C18 1.390(5) . ? C14 H14 0.9300 . ? C14 C15 1.392(4) . ? C15 H15 0.9300 . ? C15 C16 1.391(5) . ? C16 H16 0.9300 . ? C16 C17 1.379(5) . ? C17 H17 0.9300 . ? C17 C18 1.394(4) . ? C18 C19 1.464(4) . ? C21 C29 1.363(4) . ? C23 C24 1.374(4) . ? C23 C28 1.397(5) . ? C24 H24 0.9300 . ? C24 C25 1.396(4) . ? C25 H25 0.9300 . ? C25 C26 1.401(5) . ? C26 H26 0.9300 . ? C26 C27 1.383(5) . ? C27 H27 0.9300 . ? C27 C28 1.406(4) . ? C28 C29 1.433(4) . ? C29 H29 0.9300 . ? 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 C11 S12 C13 91.46(15) . . ? C23 O22 C21 106.0(2) . . ? C11 C1 H1 115.8 . . ? C11 C1 C21 128.4(3) . . ? C21 C1 H1 115.8 . . ? C1 C11 S12 127.2(2) . . ? C1 C11 C19 121.5(3) . . ? C19 C11 S12 111.4(2) . . ? C14 C13 S12 124.8(2) . . ? C18 C13 S12 113.8(2) . . ? C18 C13 C14 121.3(3) . . ? C13 C14 H14 121.0 . . ? C15 C14 C13 118.0(3) . . ? C15 C14 H14 121.0 . . ? C14 C15 H15 119.5 . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C15 C16 H16 119.7 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.7 . . ? C16 C17 H17 120.3 . . ? C16 C17 C18 119.3(3) . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 119.8(3) . . ? C13 C18 C19 113.1(3) . . ? C17 C18 C19 127.0(3) . . ? O19 C19 C11 123.6(3) . . ? O19 C19 C18 126.3(3) . . ? C18 C19 C11 110.2(3) . . ? O22 C21 C1 117.4(3) . . ? C29 C21 O22 111.4(2) . . ? C29 C21 C1 131.2(3) . . ? O22 C23 C28 110.2(3) . . ? C24 C23 O22 125.1(3) . . ? C24 C23 C28 124.8(3) . . ? C23 C24 H24 121.9 . . ? C23 C24 C25 116.1(3) . . ? C25 C24 H24 121.9 . . ? C24 C25 H25 119.6 . . ? C24 C25 C26 120.9(3) . . ? C26 C25 H25 119.6 . . ? C25 C26 H26 119.1 . . ? C27 C26 C25 121.9(3) . . ? C27 C26 H26 119.1 . . ? C26 C27 H27 120.9 . . ? C26 C27 C28 118.2(3) . . ? C28 C27 H27 120.9 . . ? C23 C28 C27 118.2(3) . . ? C23 C28 C29 106.0(3) . . ? C27 C28 C29 135.8(3) . . ? C21 C29 C28 106.5(3) . . ? C21 C29 H29 126.7 . . ? C28 C29 H29 126.7 . . ? 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 S12 C11 C19 O19 -177.0(2) . . . . ? S12 C11 C19 C18 2.2(3) . . . . ? S12 C13 C14 C15 178.4(2) . . . . ? S12 C13 C18 C17 -179.3(2) . . . . ? S12 C13 C18 C19 1.6(3) . . . . ? O22 C21 C29 C28 -0.6(3) . . . . ? O22 C23 C24 C25 179.5(3) . . . . ? O22 C23 C28 C27 -180.0(2) . . . . ? O22 C23 C28 C29 -0.4(3) . . . . ? C1 C11 C19 O19 3.1(5) . . . . ? C1 C11 C19 C18 -177.7(3) . . . . ? C1 C21 C29 C28 179.8(3) . . . . ? C11 S12 C13 C14 -179.2(3) . . . . ? C11 S12 C13 C18 -0.2(2) . . . . ? C11 C1 C21 O22 1.6(5) . . . . ? C11 C1 C21 C29 -178.8(3) . . . . ? C13 S12 C11 C1 178.8(3) . . . . ? C13 S12 C11 C19 -1.1(2) . . . . ? C13 C14 C15 C16 0.8(4) . . . . ? C13 C18 C19 O19 176.7(3) . . . . ? C13 C18 C19 C11 -2.4(3) . . . . ? C14 C13 C18 C17 -0.3(4) . . . . ? C14 C13 C18 C19 -179.4(3) . . . . ? C14 C15 C16 C17 -0.4(5) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C16 C17 C18 C13 0.7(5) . . . . ? C16 C17 C18 C19 179.7(3) . . . . ? C17 C18 C19 O19 -2.3(5) . . . . ? C17 C18 C19 C11 178.6(3) . . . . ? C18 C13 C14 C15 -0.5(4) . . . . ? C21 O22 C23 C24 -180.0(3) . . . . ? C21 O22 C23 C28 0.1(3) . . . . ? C21 C1 C11 S12 1.1(5) . . . . ? C21 C1 C11 C19 -179.0(3) . . . . ? C23 O22 C21 C1 -180.0(3) . . . . ? C23 O22 C21 C29 0.3(3) . . . . ? C23 C24 C25 C26 0.9(4) . . . . ? C23 C28 C29 C21 0.6(3) . . . . ? C24 C23 C28 C27 0.0(5) . . . . ? C24 C23 C28 C29 179.6(3) . . . . ? C24 C25 C26 C27 -0.9(5) . . . . ? C25 C26 C27 C28 0.3(5) . . . . ? C26 C27 C28 C23 0.1(4) . . . . ? C26 C27 C28 C29 -179.3(3) . . . . ? C27 C28 C29 C21 -179.9(3) . . . . ? C28 C23 C24 C25 -0.5(5) . . . . ? _shelx_res_file ; TITL 22dub_vj01_2_a.res in Pca2(1) 22dub_vj01_2.res created by SHELXL-2018/3 at 12:10:01 on 18-Jan-2022 REM Old TITL 22dub_vj01_2_a.res in Pca2(1) REM SHELXT solution in Pca2(1): R1 0.065, Rweak 0.031, Alpha 0.001 REM 0.359 for 220 systematic absences, Orientation as input REM Flack x = -0.046 ( 0.028 ) from 501 Parsons' quotients REM Formula found by SHELXT: C17 O2 S CELL 1.54184 28.1928 3.8475 11.333 90 90 90 ZERR 4 0.0011 0.0002 0.0005 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H O S UNIT 68 40 8 4 L.S. 8 PLAN 10 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.054200 0.044900 FVAR 0.71549 S12 4 0.388888 0.737761 0.578979 11.00000 0.01873 0.02692 = 0.01846 -0.00177 -0.00054 -0.00193 O19 3 0.336383 0.236113 0.312963 11.00000 0.02469 0.04296 = 0.02429 -0.01129 -0.00308 -0.00050 O22 3 0.486301 0.764908 0.498302 11.00000 0.01902 0.03063 = 0.01968 -0.00123 0.00148 -0.00086 C1 1 0.429224 0.498168 0.369709 11.00000 0.02148 0.02717 = 0.02042 0.00109 -0.00102 0.00035 AFIX 43 H1 2 0.423898 0.387428 0.297980 11.00000 -1.20000 AFIX 0 C11 1 0.391118 0.535072 0.439638 11.00000 0.02197 0.02421 = 0.02141 0.00001 -0.00248 -0.00023 C13 1 0.327171 0.658312 0.590632 11.00000 0.01914 0.02224 = 0.02405 0.00293 -0.00150 -0.00177 C14 1 0.298921 0.759137 0.685480 11.00000 0.02538 0.02932 = 0.01997 -0.00115 -0.00044 0.00244 AFIX 43 H14 2 0.311921 0.872535 0.750336 11.00000 -1.20000 AFIX 0 C15 1 0.250642 0.684994 0.680235 11.00000 0.02727 0.02772 = 0.02632 0.00151 0.00607 0.00246 AFIX 43 H15 2 0.231006 0.752502 0.742063 11.00000 -1.20000 AFIX 0 C16 1 0.231329 0.511372 0.583852 11.00000 0.01965 0.02881 = 0.03171 0.00287 -0.00058 -0.00021 AFIX 43 H16 2 0.199022 0.462824 0.582157 11.00000 -1.20000 AFIX 0 C17 1 0.259707 0.410675 0.490803 11.00000 0.02304 0.02837 = 0.02510 -0.00070 -0.00316 -0.00212 AFIX 43 H17 2 0.246723 0.293415 0.426725 11.00000 -1.20000 AFIX 0 C18 1 0.308056 0.486436 0.493764 11.00000 0.02140 0.02400 = 0.01905 0.00276 -0.00029 0.00187 C19 1 0.343472 0.399411 0.403991 11.00000 0.02011 0.02405 = 0.02342 0.00070 -0.00113 0.00120 C21 1 0.476807 0.606771 0.391167 11.00000 0.02331 0.02383 = 0.01876 0.00182 -0.00013 0.00060 C23 1 0.534026 0.843664 0.496896 11.00000 0.01977 0.02462 = 0.02175 0.00436 0.00045 0.00213 C24 1 0.558240 1.003797 0.586983 11.00000 0.02781 0.02793 = 0.01762 -0.00021 -0.00038 0.00207 AFIX 43 H24 2 0.543256 1.072275 0.656294 11.00000 -1.20000 AFIX 0 C25 1 0.606621 1.057732 0.568451 11.00000 0.02660 0.02988 = 0.02377 0.00100 -0.00469 -0.00257 AFIX 43 H25 2 0.624746 1.162089 0.627153 11.00000 -1.20000 AFIX 0 C26 1 0.628236 0.956706 0.462566 11.00000 0.01873 0.03037 = 0.03074 0.00568 -0.00004 0.00078 AFIX 43 H26 2 0.660453 0.998560 0.452125 11.00000 -1.20000 AFIX 0 C27 1 0.603023 0.796467 0.373101 11.00000 0.01982 0.02956 = 0.02117 0.00359 0.00403 0.00357 AFIX 43 H27 2 0.617888 0.729820 0.303426 11.00000 -1.20000 AFIX 0 C28 1 0.554294 0.737089 0.390385 11.00000 0.02181 0.02272 = 0.01849 0.00309 0.00072 0.00345 C29 1 0.516656 0.582278 0.323539 11.00000 0.02048 0.02627 = 0.01953 0.00195 0.00059 0.00357 AFIX 43 H29 2 0.518967 0.484365 0.248733 11.00000 -1.20000 AFIX 0 HKLF 4 REM 22dub_vj01_2_a.res in Pca2(1) REM wR2 = 0.0856, GooF = S = 1.068, Restrained GooF = 1.068 for all data REM R1 = 0.0322 for 1703 Fo > 4sig(Fo) and 0.0346 for all 1794 data REM 181 parameters refined using 1 restraints END WGHT 0.0542 0.0449 REM Highest difference peak 0.260, deepest hole -0.219, 1-sigma level 0.047 Q1 1 0.3531 0.7285 0.5823 11.00000 0.05 0.26 Q2 1 0.3894 0.6025 0.4997 11.00000 0.05 0.19 Q3 1 0.3905 0.5565 0.6455 11.00000 0.05 0.18 Q4 1 0.2828 0.4570 0.4873 11.00000 0.05 0.17 Q5 1 0.5495 0.7644 0.7021 11.00000 0.05 0.16 Q6 1 0.3950 0.9211 0.5055 11.00000 0.05 0.15 Q7 1 0.2562 0.2102 0.5864 11.00000 0.05 0.14 Q8 1 0.5823 0.6983 0.5839 11.00000 0.05 0.14 Q9 1 0.2717 0.6855 0.6823 11.00000 0.05 0.14 Q10 1 0.3239 0.3330 0.4564 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1.44 28 -1 -1 28.01 3.37 28 -1 -1 29.94 3.63 28 -1 0 4.92 1.83 28 -1 0 6.61 2.11 28 -1 1 31.15 3.57 28 -1 1 27.08 3.15 28 -1 2 2.06 1.34 28 -1 3 3.15 1.35 28 -1 4 47.82 4.20 28 -1 5 8.08 1.85 28 -1 6 13.54 2.16 28 -1 7 9.23 1.82 28 -2 -5 86.35 4.18 28 -2 -4 103.23 4.97 28 -2 -3 40.02 3.35 28 -2 -2 278.64 8.85 28 -2 -1 24.55 2.87 28 -2 0 66.28 4.49 28 -2 1 24.09 2.81 28 -2 2 268.14 8.66 28 -2 3 38.93 3.36 28 -2 4 90.77 4.66 28 -2 5 82.15 4.13 29 0 -7 -0.54 0.76 29 0 -6 3.05 1.42 29 0 -1 0.46 1.44 29 0 0 -1.54 1.19 29 0 1 1.55 0.95 29 0 1 -1.31 1.13 29 0 2 0.29 0.94 29 0 3 3.79 1.61 29 0 4 -2.91 1.40 29 0 5 0.03 1.08 29 0 6 -0.42 1.10 29 -1 -6 37.88 2.59 29 -1 -6 39.85 3.07 29 -1 -5 28.34 2.66 29 -1 -5 26.35 2.88 29 -1 -4 186.83 7.20 29 -1 -4 211.35 8.28 29 -1 -3 13.31 2.15 29 -1 -3 18.04 2.71 29 -1 -2 144.40 6.82 29 -1 -2 151.77 7.36 29 -1 -1 18.49 2.61 29 -1 -1 19.04 2.75 29 -1 0 445.98 12.23 29 -1 0 437.91 12.24 29 -1 1 18.96 2.80 29 -1 1 15.90 2.39 29 -1 2 132.67 6.71 29 -1 3 17.80 2.62 29 -1 4 174.35 7.34 29 -1 5 27.31 2.94 29 -1 6 46.92 3.42 29 -1 7 17.25 1.97 29 -2 -4 1.92 0.94 29 -2 -3 14.61 1.94 29 -2 -2 16.68 2.22 29 -2 -1 27.97 2.82 29 -2 0 -2.03 1.35 29 -2 1 25.12 2.59 29 -2 2 18.98 2.23 29 -2 3 14.34 1.94 29 -2 4 3.54 1.10 30 0 -6 23.73 2.45 30 0 -5 80.58 4.85 30 0 -3 226.68 8.98 30 0 -2 10.16 2.43 30 0 -1 426.72 12.14 30 0 0 -1.24 1.07 30 0 3 190.70 6.96 30 0 4 3.20 1.16 30 0 5 81.82 4.29 30 -1 -6 23.56 2.10 30 -1 -5 12.53 1.56 30 -1 -5 14.05 1.95 30 -1 -4 11.49 1.78 30 -1 -4 13.21 2.13 30 -1 -3 18.48 2.32 30 -1 -3 19.87 2.67 30 -1 -2 26.96 2.90 30 -1 -2 22.70 2.89 30 -1 -1 2.89 1.20 30 -1 -1 0.83 1.12 30 -1 0 19.27 2.63 30 -1 0 16.37 2.42 30 -1 1 4.27 1.51 30 -1 2 20.50 2.62 30 -1 3 19.85 2.58 30 -1 4 11.11 1.91 30 -1 5 13.56 2.00 30 -1 6 21.68 2.13 30 -2 -3 109.22 4.48 30 -2 -2 161.96 5.75 30 -2 -1 101.56 4.72 30 -2 0 64.42 3.83 30 -2 1 110.99 4.98 30 -2 2 152.38 5.63 30 -2 3 105.13 4.45 31 0 -6 -1.80 0.80 31 0 -5 2.35 1.21 31 0 -4 -0.95 1.18 31 0 -3 2.35 1.61 31 0 -2 1.81 1.33 31 0 -1 -0.98 1.20 31 0 0 0.93 1.25 31 -1 -5 153.79 5.43 31 -1 -4 11.68 1.57 31 -1 -4 11.11 1.78 31 -1 -3 149.35 5.66 31 -1 -3 162.96 6.63 31 -1 -2 79.23 4.38 31 -1 -2 72.71 4.58 31 -1 -1 197.13 7.09 31 -1 -1 203.04 7.53 31 1 -1 194.08 6.83 31 -1 0 42.87 3.47 31 -1 0 42.10 3.43 31 -1 1 174.90 6.80 31 -1 2 78.72 4.55 31 -1 3 161.72 6.35 31 -1 4 9.02 1.58 31 -1 5 136.88 5.16 31 -2 -2 7.36 1.20 31 -2 -1 63.60 3.40 31 -2 0 5.88 1.22 31 -2 1 57.61 3.26 31 -2 2 7.63 1.33 32 0 -5 38.81 2.80 32 0 -4 389.83 9.59 32 0 -3 70.41 4.38 32 0 -2 209.06 7.57 32 0 -1 51.66 3.79 32 0 0 343.81 8.99 32 1 -4 9.84 1.56 32 -1 -4 14.41 1.74 32 1 -3 14.01 1.88 32 -1 -3 14.06 1.63 32 -1 -3 16.91 2.08 32 1 -2 13.46 1.82 32 -1 -2 11.83 1.64 32 -1 -2 10.71 1.75 32 -1 -1 16.10 1.86 32 -1 -1 12.88 2.02 32 -1 0 69.77 4.01 32 -1 1 14.29 1.86 32 -1 2 11.51 1.71 32 -1 3 16.98 2.03 32 -1 4 9.46 1.42 33 0 -4 -0.65 0.72 33 0 -3 -0.28 0.95 33 0 -2 1.62 1.13 33 0 -1 -0.47 0.82 33 -1 -1 97.82 4.03 33 -1 0 237.65 6.41 33 -1 1 91.76 4.04 33 -1 2 79.53 3.69 0 0 0 0.00 0.00 TITL 22Dub_VJ01_2 in Pca2(1) REM Pca2(1) (#29, found as Pc2(1)b in cab setting) CELL 1.54184 28.192799 3.847542 11.333021 90.0000 90.0000 90.0000 ZERR 3.00 0.001101 0.000149 0.000498 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y, z SYMM -x+1/2, y, z+1/2 SFAC C H O S UNIT 51.00 30.00 6.00 3.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 35293 _olex2_date_sample_data_collection 2022-01-14 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop in perfluoroether oil' _olex2_submission_original_sample_id VJ38 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.294 _oxdiff_exptl_absorpt_empirical_full_min 0.732