####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_s5974l _database_code_depnum_ccdc_archive 'CCDC 2129467' loop_ _audit_author_name _audit_author_address 'Soumitra Agasti' ;University of Manchester United Kingdom ; _audit_update_record ; 2021-12-17 deposited with the CCDC. 2022-10-03 downloaded from the CCDC. ; _audit_creation_date 2021-11-15 _audit_creation_method ; Olex2 1.5 (compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410) ; _shelx_SHELXL_version_number 2018/3 _audit_contact_author_address ? _audit_contact_author_email ? _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 'C15 H17 F O3 S' _chemical_formula_sum 'C15 H17 F O3 S' _chemical_formula_weight 296.34 _chemical_melting_point ? 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' F F 0.0727 0.0534 '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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4393(3) _cell_length_b 11.1812(3) _cell_length_c 10.9094(2) _cell_angle_alpha 90 _cell_angle_beta 98.768(2) _cell_angle_gamma 90 _cell_volume 1379.06(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3708 _cell_measurement_temperature 99.98(10) _cell_measurement_theta_max 75.8710 _cell_measurement_theta_min 5.5140 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.245 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 624 _exptl_crystal_size_max 0.071 _exptl_crystal_size_mid 0.012 _exptl_crystal_size_min 0.008 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_unetI/netI 0.0859 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7625 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.958 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.158 _diffrn_reflns_theta_min 5.565 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.98(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.958 _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 -46.00 133.00 1.00 1.00 -- 43.52 60.00 -30.00 179 2 \w 22.00 89.00 1.00 1.00 -- 43.52 60.00 30.00 67 3 \w 72.00 104.00 1.00 1.00 -- 43.52 10.00 60.00 32 4 \w 161.00 196.00 1.00 1.60 -- 108.20 50.00-180.00 35 5 \w 138.00 165.00 1.00 1.60 -- 108.20 50.00 -60.00 27 6 \w 42.00 124.00 1.00 1.60 -- 108.20 50.00 -60.00 82 7 \w 35.00 177.00 1.00 1.60 -- 108.20 50.00 -30.00 142 8 \w 20.00 197.00 1.00 1.60 -- 108.20 50.00 30.00 177 9 \w 20.00 162.00 1.00 1.60 -- 108.20 50.00 60.00 142 10 \w 79.00 106.00 1.00 1.60 -- 108.20 50.00-180.00 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0007254000 _diffrn_orient_matrix_UB_12 0.0350229000 _diffrn_orient_matrix_UB_13 0.1364493000 _diffrn_orient_matrix_UB_21 0.0180517000 _diffrn_orient_matrix_UB_22 0.1321728000 _diffrn_orient_matrix_UB_23 -0.0328083000 _diffrn_orient_matrix_UB_31 -0.1349765000 _diffrn_orient_matrix_UB_32 0.0173048000 _diffrn_orient_matrix_UB_33 -0.0270024000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Rotating-anode X-ray tube (dual wavelength)' _diffrn_source_type 'Rigaku (Cu) X-ray DW Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2389 _reflns_number_total 2770 _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 1.171.41.120a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)' _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 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.507 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.129 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2770 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0689 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1413P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1802 _refine_ls_wR_factor_ref 0.1875 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C3(H3) 2.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C2(H2A,H2B), C9(H9A,H9B), C6(H6A,H6B), C4(H4A,H4B) 2.c Aromatic/amide H refined with riding coordinates: C15(H15), C11(H11), C14(H14), C13(H13), C12(H12) ; _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 S1 S 0.30577(5) 0.59570(5) 0.61158(5) 0.0167(2) Uani 1 1 d . . . . . F1 F 0.18939(13) 0.63310(14) 0.52842(13) 0.0243(4) Uani 1 1 d . . . . . O3 O 0.53078(15) 0.80878(16) 0.44944(14) 0.0198(4) Uani 1 1 d . . . . . O2 O 0.38535(16) 0.56203(16) 0.52857(16) 0.0231(4) Uani 1 1 d . . . . . O1 O 0.27589(16) 0.50979(16) 0.69745(16) 0.0250(4) Uani 1 1 d . . . . . C5 C 0.41433(19) 0.8203(2) 0.61085(18) 0.0133(5) Uani 1 1 d . . . . . C7 C 0.5229(2) 0.7859(2) 0.55722(19) 0.0144(5) Uani 1 1 d . . . . . C8 C 0.6240(2) 0.7287(2) 0.6427(2) 0.0168(5) Uani 1 1 d . . . . . H8A H 0.616693 0.640656 0.636522 0.020 Uiso 1 1 calc R U . . . H8B H 0.618988 0.751751 0.729413 0.020 Uiso 1 1 calc R U . . . C10 C 0.84400(19) 0.6996(2) 0.6893(2) 0.0154(5) Uani 1 1 d . . . . . C1 C 0.35478(19) 0.7298(2) 0.68928(18) 0.0140(5) Uani 1 1 d . . . . . H1 H 0.411291 0.709632 0.765727 0.017 Uiso 1 1 calc R U . . . C2 C 0.2536(2) 0.8103(2) 0.7260(2) 0.0186(5) Uani 1 1 d . . . . . H2A H 0.174197 0.781201 0.689487 0.022 Uiso 1 1 calc R U . . . H2B H 0.258327 0.817881 0.817049 0.022 Uiso 1 1 calc R U . . . C9 C 0.7448(2) 0.7665(2) 0.6112(2) 0.0181(5) Uani 1 1 d . . . . . H9A H 0.747302 0.750575 0.522372 0.022 Uiso 1 1 calc R U . . . H9B H 0.755717 0.853507 0.625477 0.022 Uiso 1 1 calc R U . . . C15 C 0.8801(2) 0.7300(2) 0.8131(2) 0.0178(5) Uani 1 1 d . . . . . H15 H 0.845010 0.796737 0.847263 0.021 Uiso 1 1 calc R U . . . C6 C 0.4228(2) 0.9299(2) 0.7019(2) 0.0196(5) Uani 1 1 d . . . . . H6A H 0.451848 0.910524 0.789789 0.024 Uiso 1 1 calc R U . . . H6B H 0.462305 1.001394 0.673805 0.024 Uiso 1 1 calc R U . . . C11 C 0.8986(2) 0.6031(2) 0.6406(2) 0.0185(5) Uani 1 1 d . . . . . H11 H 0.876119 0.582084 0.555943 0.022 Uiso 1 1 calc R U . . . C3 C 0.2864(2) 0.9280(2) 0.6656(2) 0.0203(5) Uani 1 1 d . . . . . H3 H 0.239644 1.002187 0.674529 0.024 Uiso 1 1 calc R U . . . C4 C 0.3085(2) 0.8875(2) 0.5351(2) 0.0170(5) Uani 1 1 d . . . . . H4A H 0.330720 0.952497 0.481480 0.020 Uiso 1 1 calc R U . . . H4B H 0.246323 0.835154 0.490346 0.020 Uiso 1 1 calc R U . . . C14 C 0.9663(2) 0.6645(2) 0.8874(2) 0.0232(5) Uani 1 1 d . . . . . H14 H 0.989528 0.686148 0.971806 0.028 Uiso 1 1 calc R U . . . C13 C 1.0187(2) 0.5670(2) 0.8381(2) 0.0255(6) Uani 1 1 d . . . . . H13 H 1.076977 0.521188 0.889041 0.031 Uiso 1 1 calc R U . . . C12 C 0.9857(2) 0.5367(2) 0.7141(2) 0.0245(6) Uani 1 1 d . . . . . H12 H 1.022309 0.471110 0.679591 0.029 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 0.0183(4) 0.0127(4) 0.0169(4) -0.00003(17) -0.0043(2) -0.00274(18) F1 0.0208(8) 0.0240(8) 0.0237(7) -0.0021(6) -0.0108(6) -0.0016(6) O3 0.0185(9) 0.0275(10) 0.0115(8) 0.0033(6) -0.0034(6) -0.0007(6) O2 0.0232(9) 0.0165(9) 0.0305(9) -0.0076(7) 0.0072(7) -0.0021(7) O1 0.0258(10) 0.0182(9) 0.0299(9) 0.0067(7) 0.0001(7) -0.0053(7) C5 0.0164(11) 0.0117(11) 0.0094(9) 0.0017(7) -0.0057(8) 0.0008(8) C7 0.0169(11) 0.0122(10) 0.0114(10) 0.0005(7) -0.0064(8) -0.0029(8) C8 0.0146(11) 0.0181(12) 0.0153(10) 0.0044(8) -0.0053(8) -0.0009(8) C10 0.0120(11) 0.0145(11) 0.0182(11) 0.0021(8) -0.0029(8) -0.0012(8) C1 0.0157(11) 0.0126(11) 0.0111(9) 0.0011(7) -0.0060(7) -0.0015(8) C2 0.0177(11) 0.0200(12) 0.0172(10) -0.0032(8) -0.0001(8) 0.0014(9) C9 0.0163(11) 0.0180(12) 0.0185(10) 0.0052(8) -0.0017(8) 0.0008(8) C15 0.0203(11) 0.0123(11) 0.0191(11) -0.0007(8) -0.0024(8) -0.0015(8) C6 0.0234(13) 0.0139(11) 0.0186(11) -0.0045(8) -0.0064(9) -0.0022(9) C11 0.0163(12) 0.0168(12) 0.0218(12) -0.0020(8) 0.0004(9) -0.0033(8) C3 0.0241(13) 0.0143(11) 0.0207(11) -0.0037(9) -0.0025(9) 0.0049(9) C4 0.0179(11) 0.0138(11) 0.0161(11) 0.0029(8) -0.0075(8) 0.0027(8) C14 0.0199(12) 0.0232(13) 0.0227(12) 0.0016(9) -0.0090(9) -0.0051(9) C13 0.0151(12) 0.0247(13) 0.0332(13) 0.0082(10) -0.0074(10) 0.0007(9) C12 0.0168(12) 0.0183(12) 0.0381(14) -0.0001(10) 0.0031(10) 0.0047(9) _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 F1 1.5499(14) . ? S1 O2 1.4290(18) . ? S1 O1 1.4194(18) . ? S1 C1 1.771(2) . ? O3 C7 1.220(3) . ? C5 C7 1.502(3) . ? C5 C1 1.549(3) . ? C5 C6 1.571(3) . ? C5 C4 1.552(3) . ? C7 C8 1.513(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.533(3) . ? C10 C9 1.510(3) . ? C10 C15 1.393(3) . ? C10 C11 1.393(3) . ? C1 H1 1.0000 . ? C1 C2 1.566(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.543(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C15 H15 0.9500 . ? C15 C14 1.386(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C3 1.550(3) . ? C11 H11 0.9500 . ? C11 C12 1.394(3) . ? C3 H3 1.0000 . ? C3 C4 1.551(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C14 H14 0.9500 . ? C14 C13 1.392(4) . ? C13 H13 0.9500 . ? C13 C12 1.389(4) . ? C12 H12 0.9500 . ? 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 F1 S1 C1 103.46(9) . . ? O2 S1 F1 105.87(10) . . ? O2 S1 C1 109.92(11) . . ? O1 S1 F1 107.29(10) . . ? O1 S1 O2 118.73(11) . . ? O1 S1 C1 110.34(10) . . ? C7 C5 C1 120.48(19) . . ? C7 C5 C6 118.15(19) . . ? C7 C5 C4 122.76(18) . . ? C1 C5 C6 98.63(17) . . ? C1 C5 C4 103.73(18) . . ? C4 C5 C6 85.83(16) . . ? O3 C7 C5 120.58(19) . . ? O3 C7 C8 121.4(2) . . ? C5 C7 C8 117.93(18) . . ? C7 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C7 C8 C9 112.08(19) . . ? H8A C8 H8B 107.9 . . ? C9 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C15 C10 C9 120.9(2) . . ? C15 C10 C11 118.4(2) . . ? C11 C10 C9 120.7(2) . . ? S1 C1 H1 109.0 . . ? C5 C1 S1 115.01(14) . . ? C5 C1 H1 109.0 . . ? C5 C1 C2 99.79(17) . . ? C2 C1 S1 114.65(15) . . ? C2 C1 H1 109.0 . . ? C1 C2 H2A 112.1 . . ? C1 C2 H2B 112.1 . . ? H2A C2 H2B 109.8 . . ? C3 C2 C1 98.25(18) . . ? C3 C2 H2A 112.1 . . ? C3 C2 H2B 112.1 . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 C8 111.24(18) . . ? C10 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C10 C15 H15 119.4 . . ? C14 C15 C10 121.2(2) . . ? C14 C15 H15 119.4 . . ? C5 C6 H6A 114.9 . . ? C5 C6 H6B 114.9 . . ? H6A C6 H6B 112.0 . . ? C3 C6 C5 82.26(16) . . ? C3 C6 H6A 114.9 . . ? C3 C6 H6B 114.9 . . ? C10 C11 H11 119.4 . . ? C12 C11 C10 121.1(2) . . ? C12 C11 H11 119.4 . . ? C2 C3 C6 101.71(18) . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 103.15(19) . . ? C6 C3 H3 119.8 . . ? C6 C3 C4 86.59(18) . . ? C4 C3 H3 119.8 . . ? C5 C4 H4A 114.8 . . ? C5 C4 H4B 114.8 . . ? C3 C4 C5 82.83(16) . . ? C3 C4 H4A 114.8 . . ? C3 C4 H4B 114.8 . . ? H4A C4 H4B 111.9 . . ? C15 C14 H14 120.1 . . ? C15 C14 C13 119.9(2) . . ? C13 C14 H14 120.1 . . ? C14 C13 H13 120.1 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.1 . . ? C11 C12 H12 120.2 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 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 S1 C1 C2 C3 -126.67(16) . . . . ? F1 S1 C1 C5 -77.74(17) . . . . ? F1 S1 C1 C2 37.13(17) . . . . ? O3 C7 C8 C9 31.9(3) . . . . ? O2 S1 C1 C5 34.95(19) . . . . ? O2 S1 C1 C2 149.82(16) . . . . ? O1 S1 C1 C5 167.77(15) . . . . ? O1 S1 C1 C2 -77.37(18) . . . . ? C5 C7 C8 C9 -144.7(2) . . . . ? C5 C1 C2 C3 -3.23(19) . . . . ? C5 C6 C3 C2 68.05(17) . . . . ? C5 C6 C3 C4 -34.68(16) . . . . ? C7 C5 C1 S1 -59.4(2) . . . . ? C7 C5 C1 C2 177.43(18) . . . . ? C7 C5 C6 C3 159.88(19) . . . . ? C7 C5 C4 C3 -155.6(2) . . . . ? C7 C8 C9 C10 -174.54(18) . . . . ? C10 C15 C14 C13 0.4(4) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C1 C5 C7 O3 134.0(2) . . . . ? C1 C5 C7 C8 -49.5(3) . . . . ? C1 C5 C6 C3 -68.59(17) . . . . ? C1 C5 C4 C3 63.27(18) . . . . ? C1 C2 C3 C6 -42.88(19) . . . . ? C1 C2 C3 C4 46.3(2) . . . . ? C2 C3 C4 C5 -66.13(19) . . . . ? C9 C10 C15 C14 176.1(2) . . . . ? C9 C10 C11 C12 -176.4(2) . . . . ? C15 C10 C9 C8 -76.1(3) . . . . ? C15 C10 C11 C12 1.2(3) . . . . ? C15 C14 C13 C12 0.9(4) . . . . ? C6 C5 C7 O3 -105.2(2) . . . . ? C6 C5 C7 C8 71.4(3) . . . . ? C6 C5 C1 S1 170.61(14) . . . . ? C6 C5 C1 C2 47.41(19) . . . . ? C6 C5 C4 C3 -34.61(17) . . . . ? C6 C3 C4 C5 35.11(16) . . . . ? C11 C10 C9 C8 101.4(2) . . . . ? C11 C10 C15 C14 -1.4(4) . . . . ? C4 C5 C7 O3 -1.0(3) . . . . ? C4 C5 C7 C8 175.60(19) . . . . ? C4 C5 C1 S1 82.82(19) . . . . ? C4 C5 C1 C2 -40.37(19) . . . . ? C4 C5 C6 C3 34.69(17) . . . . ? C14 C13 C12 C11 -1.2(4) . . . . ? _shelx_res_file ; TITL s5974l_a.res in P2(1)/c s5974l.res created by SHELXL-2018/3 at 14:43:28 on 15-Nov-2021 REM Old TITL s5974l in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.135, Rweak 0.050, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C12 O1 Cl CELL 1.54184 11.4393 11.1812 10.9094 90 98.768 90 ZERR 4 0.0003 0.0003 0.0002 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F O S UNIT 60 68 4 12 4 L.S. 8 PLAN 5 TEMP -173 CONF fmap 2 MORE -1 BOND $H ACTA REM REM REM WGHT 0.141300 FVAR 0.72867 S1 5 0.305772 0.595701 0.611582 11.00000 0.01832 0.01273 = 0.01687 -0.00003 -0.00426 -0.00274 F1 3 0.189394 0.633098 0.528417 11.00000 0.02077 0.02399 = 0.02367 -0.00215 -0.01084 -0.00163 O3 4 0.530776 0.808780 0.449443 11.00000 0.01854 0.02750 = 0.01151 0.00330 -0.00336 -0.00066 O2 4 0.385350 0.562033 0.528567 11.00000 0.02316 0.01655 = 0.03050 -0.00762 0.00716 -0.00209 O1 4 0.275893 0.509786 0.697450 11.00000 0.02575 0.01819 = 0.02986 0.00670 0.00015 -0.00530 C5 1 0.414327 0.820330 0.610846 11.00000 0.01640 0.01171 = 0.00943 0.00171 -0.00565 0.00075 C7 1 0.522892 0.785876 0.557217 11.00000 0.01688 0.01217 = 0.01138 0.00053 -0.00644 -0.00289 C8 1 0.624048 0.728747 0.642748 11.00000 0.01463 0.01811 = 0.01529 0.00438 -0.00533 -0.00088 AFIX 23 H8A 2 0.616693 0.640656 0.636522 11.00000 -1.20000 H8B 2 0.618988 0.751751 0.729413 11.00000 -1.20000 AFIX 0 C10 1 0.844001 0.699618 0.689324 11.00000 0.01196 0.01448 = 0.01817 0.00205 -0.00290 -0.00124 C1 1 0.354776 0.729811 0.689281 11.00000 0.01566 0.01256 = 0.01115 0.00114 -0.00600 -0.00154 AFIX 13 H1 2 0.411291 0.709632 0.765727 11.00000 -1.20000 AFIX 0 C2 1 0.253626 0.810336 0.726012 11.00000 0.01774 0.02002 = 0.01715 -0.00320 -0.00013 0.00144 AFIX 23 H2A 2 0.174197 0.781201 0.689487 11.00000 -1.20000 H2B 2 0.258327 0.817881 0.817049 11.00000 -1.20000 AFIX 0 C9 1 0.744784 0.766513 0.611196 11.00000 0.01628 0.01802 = 0.01851 0.00518 -0.00174 0.00080 AFIX 23 H9A 2 0.747302 0.750575 0.522372 11.00000 -1.20000 H9B 2 0.755717 0.853507 0.625477 11.00000 -1.20000 AFIX 0 C15 1 0.880090 0.729977 0.813125 11.00000 0.02029 0.01225 = 0.01911 -0.00071 -0.00238 -0.00153 AFIX 43 H15 2 0.845010 0.796737 0.847263 11.00000 -1.20000 AFIX 0 C6 1 0.422761 0.929875 0.701874 11.00000 0.02342 0.01392 = 0.01859 -0.00452 -0.00640 -0.00217 AFIX 23 H6A 2 0.451848 0.910524 0.789789 11.00000 -1.20000 H6B 2 0.462305 1.001394 0.673805 11.00000 -1.20000 AFIX 0 C11 1 0.898613 0.603061 0.640640 11.00000 0.01629 0.01680 = 0.02177 -0.00201 0.00041 -0.00333 AFIX 43 H11 2 0.876119 0.582084 0.555943 11.00000 -1.20000 AFIX 0 C3 1 0.286430 0.928004 0.665552 11.00000 0.02408 0.01434 = 0.02068 -0.00367 -0.00249 0.00494 AFIX 13 H3 2 0.239644 1.002187 0.674529 11.00000 -1.20000 AFIX 0 C4 1 0.308475 0.887488 0.535059 11.00000 0.01789 0.01380 = 0.01612 0.00289 -0.00752 0.00266 AFIX 23 H4A 2 0.330720 0.952497 0.481480 11.00000 -1.20000 H4B 2 0.246323 0.835154 0.490346 11.00000 -1.20000 AFIX 0 C14 1 0.966289 0.664501 0.887401 11.00000 0.01989 0.02322 = 0.02269 0.00165 -0.00896 -0.00511 AFIX 43 H14 2 0.989528 0.686148 0.971806 11.00000 -1.20000 AFIX 0 C13 1 1.018723 0.566970 0.838054 11.00000 0.01512 0.02471 = 0.03319 0.00822 -0.00736 0.00073 AFIX 43 H13 2 1.076977 0.521188 0.889041 11.00000 -1.20000 AFIX 0 C12 1 0.985713 0.536686 0.714086 11.00000 0.01681 0.01826 = 0.03814 -0.00014 0.00313 0.00468 AFIX 43 H12 2 1.022309 0.471110 0.679591 11.00000 -1.20000 AFIX 0 HKLF 4 REM s5974l_a.res in P2(1)/c REM wR2 = 0.1875, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0689 for 2389 Fo > 4sig(Fo) and 0.0744 for all 2770 data REM 181 parameters refined using 0 restraints END WGHT 0.1384 0.0000 REM Highest difference peak 0.507, deepest hole -1.054, 1-sigma level 0.129 Q1 1 0.2529 0.5749 0.7162 11.00000 0.05 0.51 Q2 1 0.4034 0.5455 0.5816 11.00000 0.05 0.42 Q3 1 0.3801 0.6779 0.6054 11.00000 0.05 0.40 Q4 1 0.2275 0.4136 0.6962 11.00000 0.05 0.40 Q5 1 0.5588 0.6836 0.7327 11.00000 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1 6.72 4.79 -11 -4 1 5.61 4.58 -11 -4 1 10.23 5.03 -11 -4 0 167.06 17.60 -11 -4 0 175.31 18.00 -11 -4 0 198.99 18.30 -11 -4 -1 29.19 5.65 -11 -4 -1 22.21 5.15 -11 4 -2 9.08 3.61 -11 -4 -2 14.54 4.81 -11 -4 -2 15.94 4.07 -11 -4 -2 17.29 4.40 -11 -4 -3 49.05 6.60 -11 -4 -3 44.45 6.23 -11 -4 -4 5.09 3.68 -11 -4 -4 3.24 3.19 -11 -4 -5 43.88 5.30 -11 -4 -5 35.67 5.09 -11 -4 -6 19.99 2.97 -11 -5 8 40.61 4.12 11 -5 -8 14.02 3.36 -11 -5 7 63.26 7.52 -11 -5 7 55.79 7.15 -11 -5 6 10.09 4.56 -11 -5 6 6.87 4.33 -11 -5 5 3.49 4.41 -11 -5 4 -2.81 4.50 -11 -5 4 1.99 4.63 -11 -5 3 754.89 69.76 -11 -5 3 744.71 69.72 -11 -5 2 4.02 4.60 -11 -5 2 1.25 4.50 -11 -5 2 6.88 4.79 -11 -5 1 3.36 4.56 -11 -5 1 -2.47 3.95 -11 -5 1 5.79 4.80 -11 -5 0 5.49 4.77 -11 -5 0 7.48 3.78 -11 -5 0 6.26 4.56 -11 -5 -1 102.93 11.87 -11 -5 -1 120.11 12.19 -11 -5 -2 64.84 8.06 -11 -5 -2 79.41 8.70 -11 5 -3 8.81 3.16 -11 -5 -3 9.77 4.20 -11 -5 -3 6.15 2.99 -11 -5 -4 214.16 13.12 -11 5 -4 94.50 11.97 -11 -5 -5 184.62 17.62 -11 -6 7 3.41 3.13 -11 -6 7 2.91 2.87 -11 -6 6 3.66 3.81 -11 -6 6 2.62 3.57 -11 -6 5 144.19 14.43 -11 -6 5 135.17 14.34 -11 -6 4 0.95 4.29 -11 -6 4 0.96 4.24 -11 -6 3 68.42 8.24 -11 -6 3 65.43 8.27 -11 -6 3 57.72 8.10 -11 -6 2 8.16 4.52 -11 -6 2 10.32 4.44 -11 -6 1 4.08 4.54 -11 -6 1 8.02 4.17 -11 -6 1 9.92 4.49 -11 -6 0 22.46 4.37 -11 -6 0 20.73 5.06 -11 -6 -1 53.41 6.96 -11 -6 -2 36.93 5.29 -11 6 -3 27.86 4.49 -11 -6 -3 38.86 4.47 -11 -7 6 162.09 14.24 -11 -7 6 129.15 13.99 -11 -7 5 72.16 7.78 -11 -7 5 60.58 7.61 -11 -7 4 2.02 3.60 -11 -7 3 2.10 3.86 -11 -7 3 -3.04 3.99 -11 -7 2 22.62 4.94 -11 -7 2 31.16 5.33 -11 -7 1 20.84 4.36 -11 -7 0 186.07 17.52 -11 -7 0 172.31 17.87 -11 -7 0 186.91 18.17 -11 -7 -1 149.62 15.12 -11 -7 -1 156.89 15.40 -11 -7 -2 38.95 5.13 -11 7 -2 24.64 4.36 -11 -7 -2 41.01 4.74 -11 -7 -3 17.87 3.33 -11 7 -3 9.50 2.46 -11 -7 -4 40.74 4.57 -11 -8 5 -0.76 2.48 -11 -8 5 -0.88 2.10 -11 -8 4 32.04 4.52 -11 -8 3 3.14 3.12 -11 -8 3 -2.85 3.12 -11 -8 2 0.12 3.14 -11 -8 2 2.89 3.38 -11 -8 1 76.15 7.60 -11 -8 1 77.97 7.95 -11 -8 1 57.84 7.86 -11 -8 0 40.61 5.53 -11 -8 -1 1.75 2.74 -11 -8 -1 2.38 2.70 -11 -8 -2 9.01 2.65 -11 -9 2 27.45 3.62 -11 -9 1 3.94 2.18 -12 0 8 0.77 3.24 -12 0 7 1.28 3.76 -12 0 6 120.72 13.71 -12 0 6 138.15 13.66 -12 0 5 0.20 4.16 -12 0 5 2.67 4.16 -12 0 4 33.73 6.13 -12 0 4 37.32 6.01 -12 0 3 -3.00 4.29 -12 0 3 1.83 3.98 -12 0 2 396.47 33.85 -12 0 2 322.51 33.66 -12 1 9 50.24 5.98 -12 -1 9 58.62 6.09 -12 -1 8 30.92 4.70 -12 1 8 21.52 4.42 -12 1 7 164.46 17.13 -12 -1 7 183.27 17.35 -12 1 6 0.18 4.23 -12 -1 6 0.75 4.24 -12 1 6 -1.18 3.67 -12 -1 6 -0.92 4.00 -12 1 5 55.51 7.04 -12 -1 5 53.02 6.98 -12 1 5 31.36 6.29 -12 -1 5 42.47 6.72 -12 1 4 231.32 21.73 -12 -1 4 255.86 21.97 -12 1 4 181.99 21.39 -12 -1 4 225.81 21.80 -12 1 3 31.45 5.63 -12 -1 3 39.52 6.11 -12 1 3 30.11 5.31 -12 -1 3 35.94 5.88 -12 -1 2 47.39 6.41 -12 -1 2 40.16 6.43 -12 -1 1 109.15 11.53 -12 -1 -4 73.54 7.47 -12 -2 8 27.59 4.33 -12 2 8 22.46 4.02 -12 -2 8 27.55 4.42 -12 -2 7 125.98 11.46 -12 2 7 91.01 10.94 -12 2 6 1.78 3.48 -12 -2 6 -6.33 4.41 -12 -2 5 138.80 13.54 -12 2 5 102.57 12.80 -12 -2 5 142.44 13.42 -12 -2 4 18.40 5.00 -12 2 4 7.90 3.75 -12 -2 4 10.20 4.74 -12 -2 3 456.06 42.90 -12 -2 3 452.89 42.86 -12 -2 2 144.02 13.85 -12 -2 2 125.82 13.93 -12 -2 2 129.90 13.59 -12 -2 1 3.98 3.61 -12 -2 1 3.82 3.71 -12 -2 0 9.40 3.88 -12 -2 0 8.68 3.56 -12 -2 -1 274.26 26.10 -12 -2 -2 94.60 9.88 -12 -2 -3 11.16 3.08 -12 -2 -4 2.31 2.12 -12 -3 8 14.03 3.35 -12 -3 8 16.86 3.32 -12 -3 7 32.28 4.74 -12 -3 7 26.87 4.53 -12 3 6 9.68 3.37 -12 -3 5 158.92 13.57 -12 -3 5 149.38 13.36 -12 -3 4 114.08 12.42 -12 -3 4 115.35 12.40 -12 -3 3 2.43 4.16 -12 -3 3 11.83 4.57 -12 -3 2 40.73 5.94 -12 -3 2 38.95 6.27 -12 -3 2 40.76 5.85 -12 -3 1 2.59 3.79 -12 -3 1 1.26 3.18 -12 -3 1 -0.18 3.95 -12 -3 0 296.59 30.72 -12 -3 0 359.14 30.94 -12 -3 -1 1.90 3.67 -12 -3 -2 278.48 26.41 -12 -3 -3 10.02 3.21 -12 -3 -4 6.73 2.40 -12 -4 8 12.57 2.60 -12 -4 8 9.57 2.49 -12 -4 7 6.45 3.26 -12 -4 7 2.90 3.19 -12 -4 6 61.59 7.41 -12 -4 5 6.42 4.25 -12 -4 4 41.25 6.42 -12 -4 4 45.30 6.48 -12 -4 3 220.41 20.64 -12 -4 3 198.87 20.70 -12 -4 2 316.41 31.28 -12 -4 2 350.23 31.52 -12 -4 2 327.06 31.33 -12 -4 1 297.85 29.30 -12 -4 1 302.14 29.63 -12 -4 1 337.89 29.68 -12 -4 0 8.89 4.03 -12 -4 0 11.34 3.96 -12 -4 -1 14.40 3.93 -12 -4 -1 7.37 3.32 -12 -4 -2 68.11 7.77 -12 -4 -3 351.98 32.85 -12 -4 -4 2.05 2.07 -12 -5 7 68.81 7.29 -12 -5 6 4.63 3.28 -12 -5 6 1.74 3.05 -12 -5 5 129.44 12.81 -12 -5 5 118.59 12.70 -12 -5 4 6.52 3.84 -12 -5 3 63.44 7.45 -12 -5 3 55.09 7.50 -12 -5 2 2.28 3.58 -12 -5 2 5.95 3.95 -12 -5 2 4.86 3.57 -12 -5 1 285.21 26.84 -12 -5 1 284.69 27.19 -12 -5 1 284.75 27.15 -12 -5 0 -2.18 3.52 -12 -5 0 8.09 3.68 -12 -5 -1 52.45 6.73 -12 -5 -1 72.09 7.30 -12 -5 -2 107.64 10.99 -12 -5 -3 18.38 3.29 -12 -6 6 40.84 4.76 -12 -6 6 36.49 4.71 -12 -6 5 11.48 3.36 -12 -6 4 -0.76 3.23 -12 -6 4 0.80 3.29 -12 -6 3 155.32 15.34 -12 -6 2 155.65 14.84 -12 -6 2 146.57 15.09 -12 -6 1 6.22 2.69 -12 -6 1 12.74 3.57 -12 -6 1 2.23 3.47 -12 -6 0 75.81 8.00 -12 -6 0 68.74 8.06 -12 -6 -1 67.67 7.62 -12 -6 -1 80.72 8.02 -12 -6 -2 188.33 17.93 -12 -7 4 109.40 10.35 -12 -7 4 98.08 10.31 -12 -7 3 46.07 5.39 -12 -7 3 47.12 5.64 -12 -7 2 47.04 5.34 -12 -7 1 42.69 5.25 -12 -7 0 110.72 10.94 -13 0 7 0.78 2.31 -13 0 6 20.27 3.77 -13 0 5 -0.26 3.18 -13 0 5 0.35 2.85 -13 0 4 14.86 3.55 -13 0 4 3.16 3.19 -13 0 3 2.85 2.81 -13 -1 7 18.76 3.38 -13 -1 6 39.13 4.88 -13 -1 6 37.66 4.65 -13 -1 5 108.86 9.15 -13 -1 5 93.87 8.86 -13 -1 4 28.66 4.52 -13 -1 4 21.65 4.46 -13 -1 3 45.45 5.40 -13 -1 3 33.94 5.40 -13 -2 7 45.58 5.32 -13 -2 6 5.78 3.15 -13 -2 6 4.16 3.07 -13 -2 5 11.26 3.70 -13 -2 5 10.88 3.61 -13 -2 4 9.87 3.43 -13 -2 4 5.90 3.55 -13 -2 3 5.25 3.09 -13 -2 3 2.22 3.05 -13 -2 2 1.63 2.88 -13 -3 6 25.82 3.82 -13 -3 6 21.65 3.82 -13 -3 5 9.80 3.29 -13 -3 5 10.34 3.43 -13 -3 4 90.46 9.54 -13 -3 4 90.91 9.70 -13 -3 3 248.63 22.99 -13 -3 3 234.63 23.14 -13 -3 2 7.24 3.12 -13 -3 1 8.22 2.84 -13 -4 6 16.65 2.95 -13 -4 5 10.78 2.99 -13 -4 5 7.91 3.04 -13 -4 4 22.69 3.79 -13 -4 4 18.73 3.93 -13 -4 3 26.93 3.94 -13 -4 3 24.54 4.29 -13 -4 2 -1.11 2.72 -13 -4 1 71.34 7.59 -13 -4 0 34.17 4.26 -13 -5 4 29.90 3.78 -13 -5 4 26.93 4.05 -13 -5 3 69.15 7.47 -13 -5 2 -1.49 2.49 -13 -5 1 48.85 5.46 TITL s5974l in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 11.439311 11.181217 10.909443 90.0000 98.7679 90.0000 ZERR 6.00 0.000308 0.000246 0.000228 0.0000 0.0021 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 19476 _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 1.904 _oxdiff_exptl_absorpt_empirical_full_min 0.704