data_m19080 _audit_creation_method 'SHELXL-2018/3' # CIF edited on-the-fly by script CIFFIX (S. Parkin, 2000-2017). # CIFFIX: http://xray.uky.edu/people/parkin/programs/ciffix _audit_update_record ? _shelx_SHELXL_version_number '2018/3' _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps, but subsequently included in the refinement using riding models, with constrained distances set to 0.95 \%A (C~sp2~H), 0.98 \%A (RCH~3~) and 0.99 \%A (R~2~CH~2~). U~iso~(H) parameters were set to values of either 1.2U~eq~ or 1.5U~eq~ (RCH~3~ only) of the attached atom. ; _publ_section_references ; Bruker-AXS (2016). APEX3 Bruker-AXS Inc., Madison, WI, USA. Hope, H. (1994). Prog. Inorg. Chem. 41, 1--19. Krause, L., Herbst-Irmer, R., Sheldrick, G.M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3--10. Parkin, S. & Hope, H. (1998). J. Appl. Cryst. 31, 945--953. Parkin, S. (2000). Acta Cryst. A56, 157--162. Parkin, S. (2013). CIFFIX, http://xray.uky.edu/people/parkin/programs/ciffix Sheldrick, G.M. (2008). Acta Cryst. A64, 112--122. Sheldrick, G.M. (2015a). Acta Cryst. A71, 3--8. Sheldrick, G.M. (2015b). Acta Cryst. C71, 3--8. Spek, A.L. (2009). Acta Cryst. D65, 148--155. ; _publ_section_acknowledgements ; The D8 Venture diffractometer was funded by the NSF (MRI CHE1625732), and by the University of Kentucky. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 N O2 S, B F4' _chemical_formula_sum 'C17 H19 B F4 N O2 S' _chemical_formula_weight 388.20 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2318(3) _cell_length_b 6.8098(2) _cell_length_c 24.3279(9) _cell_angle_alpha 90 _cell_angle_beta 93.294(1) _cell_angle_gamma 90 _cell_volume 1692.28(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.44 _exptl_crystal_description 'cut lath' _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_F_000 804 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.245 _shelx_estimated_absorpt_T_min 0.948 _shelx_estimated_absorpt_T_max 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details 'SADABS (Krause et al., 2015)' _exptl_absorpt_special_details ; In addition to absorption, multi-scan techniques also correct other slowly varying changes in scale factor over reciprocal space, such as those caused by X-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, crystal longer than the X-ray beam cross section, absorption by the crystal mount etc. These account, by and large, for much of the difference between estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. ; _exptl_special_details ; The crystal was mounted using polyisobutene oil on the tip of a fine glass fibre, which was fastened in a copper mounting pin with electrical solder. It was placed directly into the cold gas stream of a liquid-nitrogen based cryostat (Hope, 1994; Parkin & Hope, 1998). Diffraction data were collected with the crystal at 90K, which is standard practice in this laboratory for the majority of flash-cooled crystals. ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microsource' _diffrn_measurement_device_type 'Bruker D8 Venture dual source' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 7.41 _diffrn_reflns_number 37261 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.107 _diffrn_reflns_theta_max 27.450 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 3858 _reflns_number_gt 3150 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'APEX3 (Bruker-AXS, 2016)' _computing_cell_refinement 'APEX3 (Bruker-AXS, 2016)' _computing_data_reduction 'APEX3 (Bruker-AXS, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015b)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELX (Sheldrick, 2008) and CIFFIX (Parkin, 2013)' _refine_special_details ; Refinement progress was checked using Platon (Spek, 2009) and by an R-tensor (Parkin, 2000). The final model was further checked with the IUCr utility checkCIF. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+1.0881P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3858 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _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_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 0.63161(4) 0.28675(6) 0.54440(2) 0.01312(10) Uani 1 1 d . . . . . O1 O 0.44840(11) 0.45006(17) 0.32214(5) 0.0172(3) Uani 1 1 d . . . . . O2 O 0.56594(11) 0.81337(17) 0.29638(5) 0.0184(3) Uani 1 1 d . . . . . N1 N 0.49374(12) 0.22131(19) 0.42792(5) 0.0117(3) Uani 1 1 d . . . . . C1 C 0.62615(15) 0.2719(2) 0.43066(6) 0.0120(3) Uani 1 1 d . . . . . C2 C 0.69366(16) 0.2987(2) 0.38201(7) 0.0142(3) Uani 1 1 d . . . . . H2 H 0.647102 0.289650 0.347175 0.017 Uiso 1 1 calc R U . . . C3 C 0.82533(16) 0.3376(2) 0.38454(7) 0.0163(3) Uani 1 1 d . . . . . H3 H 0.868548 0.355178 0.351359 0.020 Uiso 1 1 calc R U . . . C4 C 0.89714(16) 0.3518(2) 0.43495(7) 0.0159(3) Uani 1 1 d . . . . . H4 H 0.988959 0.373496 0.435965 0.019 Uiso 1 1 calc R U . . . C5 C 0.83432(16) 0.3341(2) 0.48296(7) 0.0156(3) Uani 1 1 d . . . . . H5 H 0.882316 0.346562 0.517382 0.019 Uiso 1 1 calc R U . . . C6 C 0.69907(15) 0.2977(2) 0.48131(6) 0.0123(3) Uani 1 1 d . . . . . C7 C 0.46797(15) 0.2497(2) 0.52733(6) 0.0120(3) Uani 1 1 d . . . . . C8 C 0.38789(16) 0.2416(2) 0.57222(7) 0.0143(3) Uani 1 1 d . . . . . H8 H 0.424099 0.267851 0.608302 0.017 Uiso 1 1 calc R U . . . C9 C 0.25759(16) 0.1960(2) 0.56425(7) 0.0155(3) Uani 1 1 d . . . . . H9 H 0.203984 0.186432 0.594753 0.019 Uiso 1 1 calc R U . . . C10 C 0.20456(16) 0.1637(2) 0.51084(7) 0.0153(3) Uani 1 1 d . . . . . H10 H 0.114282 0.132303 0.505378 0.018 Uiso 1 1 calc R U . . . C11 C 0.28001(15) 0.1764(2) 0.46595(7) 0.0137(3) Uani 1 1 d . . . . . H11 H 0.240724 0.157484 0.430003 0.016 Uiso 1 1 calc R U . . . C12 C 0.41573(15) 0.2172(2) 0.47282(6) 0.0118(3) Uani 1 1 d . . . . . C13 C 0.43288(16) 0.1545(2) 0.37416(6) 0.0134(3) Uani 1 1 d . . . . . H13A H 0.372302 0.044870 0.380939 0.016 Uiso 1 1 calc R U . . . H13B H 0.502570 0.102662 0.351566 0.016 Uiso 1 1 calc R U . . . C14 C 0.35806(16) 0.3120(2) 0.34146(7) 0.0152(3) Uani 1 1 d . . . . . H14A H 0.307295 0.251924 0.309923 0.018 Uiso 1 1 calc R U . . . H14B H 0.296076 0.378639 0.365079 0.018 Uiso 1 1 calc R U . . . C15 C 0.38480(16) 0.5935(3) 0.28668(7) 0.0188(4) Uani 1 1 d . . . . . H15A H 0.334043 0.685595 0.308632 0.023 Uiso 1 1 calc R U . . . H15B H 0.323613 0.527822 0.259553 0.023 Uiso 1 1 calc R U . . . C16 C 0.48685(16) 0.7035(2) 0.25746(7) 0.0173(3) Uani 1 1 d . . . . . H16A H 0.542084 0.609976 0.237979 0.021 Uiso 1 1 calc R U . . . H16B H 0.444244 0.793113 0.229860 0.021 Uiso 1 1 calc R U . . . C17 C 0.66635(17) 0.9179(3) 0.27101(7) 0.0211(4) Uani 1 1 d . . . . . H17A H 0.718467 0.826247 0.250243 0.032 Uiso 1 1 calc R U . . . H17B H 0.722924 0.982892 0.299352 0.032 Uiso 1 1 calc R U . . . H17C H 0.626941 1.016827 0.245917 0.032 Uiso 1 1 calc R U . . . F1 F -0.03802(10) 0.08810(16) 0.58561(4) 0.0271(3) Uani 1 1 d . . . . . F2 F 0.04171(10) 0.18838(17) 0.67022(4) 0.0286(3) Uani 1 1 d . . . . . F3 F -0.16676(10) 0.07026(16) 0.65815(4) 0.0253(2) Uani 1 1 d . . . . . F4 F -0.11437(10) 0.36807(15) 0.62278(5) 0.0271(3) Uani 1 1 d . . . . . B1 B -0.06843(18) 0.1788(3) 0.63466(8) 0.0174(4) 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 S1 0.01380(19) 0.01508(19) 0.01036(19) 0.00083(15) -0.00034(14) -0.00034(15) O1 0.0156(6) 0.0191(6) 0.0165(6) 0.0064(5) -0.0019(5) -0.0018(5) O2 0.0234(6) 0.0208(6) 0.0111(6) -0.0020(5) 0.0018(5) -0.0034(5) N1 0.0126(6) 0.0116(6) 0.0109(6) -0.0008(5) 0.0002(5) 0.0003(5) C1 0.0122(7) 0.0093(7) 0.0145(8) -0.0004(6) 0.0006(6) 0.0019(6) C2 0.0170(8) 0.0143(8) 0.0115(8) -0.0006(6) 0.0007(6) 0.0018(6) C3 0.0174(8) 0.0165(8) 0.0155(8) 0.0015(6) 0.0049(6) 0.0010(6) C4 0.0128(8) 0.0151(8) 0.0197(9) 0.0026(6) 0.0002(6) -0.0009(6) C5 0.0158(8) 0.0142(8) 0.0166(8) 0.0018(6) -0.0015(6) -0.0007(6) C6 0.0157(8) 0.0094(7) 0.0116(7) 0.0008(6) -0.0002(6) 0.0011(6) C7 0.0136(7) 0.0093(7) 0.0129(8) 0.0008(6) -0.0004(6) 0.0013(6) C8 0.0183(8) 0.0125(8) 0.0121(8) 0.0007(6) 0.0021(6) 0.0038(6) C9 0.0190(8) 0.0131(8) 0.0151(8) 0.0025(6) 0.0068(6) 0.0039(6) C10 0.0142(8) 0.0122(8) 0.0196(9) 0.0011(6) 0.0031(7) 0.0007(6) C11 0.0153(8) 0.0116(7) 0.0140(8) -0.0004(6) 0.0005(6) 0.0005(6) C12 0.0143(7) 0.0071(7) 0.0143(8) 0.0008(6) 0.0025(6) 0.0017(6) C13 0.0154(8) 0.0141(7) 0.0104(8) -0.0028(6) -0.0010(6) -0.0014(6) C14 0.0149(8) 0.0181(8) 0.0124(8) 0.0009(6) -0.0018(6) -0.0022(6) C15 0.0177(8) 0.0223(9) 0.0160(8) 0.0048(7) -0.0029(7) 0.0031(7) C16 0.0218(8) 0.0193(8) 0.0104(8) 0.0002(6) -0.0017(6) -0.0013(7) C17 0.0227(9) 0.0231(9) 0.0176(9) -0.0017(7) 0.0029(7) -0.0032(7) F1 0.0256(6) 0.0358(6) 0.0204(6) -0.0042(5) 0.0046(4) -0.0002(5) F2 0.0201(5) 0.0404(7) 0.0243(6) 0.0058(5) -0.0077(4) -0.0055(5) F3 0.0200(5) 0.0327(6) 0.0234(6) 0.0053(5) 0.0032(4) -0.0089(4) F4 0.0245(6) 0.0231(6) 0.0339(6) 0.0054(5) 0.0031(5) 0.0026(4) B1 0.0131(9) 0.0232(10) 0.0158(9) 0.0015(7) -0.0001(7) -0.0015(7) _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 C6 1.7202(16) . ? S1 C7 1.7204(16) . ? O1 C14 1.4172(19) . ? O1 C15 1.4343(19) . ? O2 C17 1.420(2) . ? O2 C16 1.4224(19) . ? N1 C12 1.3898(19) . ? N1 C1 1.396(2) . ? N1 C13 1.4873(19) . ? C1 C6 1.414(2) . ? C1 C2 1.416(2) . ? C2 C3 1.371(2) . ? C2 H2 0.9500 . ? C3 C4 1.396(2) . ? C3 H3 0.9500 . ? C4 C5 1.370(2) . ? C4 H4 0.9500 . ? C5 C6 1.404(2) . ? C5 H5 0.9500 . ? C7 C8 1.404(2) . ? C7 C12 1.418(2) . ? C8 C9 1.372(2) . ? C8 H8 0.9500 . ? C9 C10 1.396(2) . ? C9 H9 0.9500 . ? C10 C11 1.376(2) . ? C10 H10 0.9500 . ? C11 C12 1.417(2) . ? C11 H11 0.9500 . ? C13 C14 1.517(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.497(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? F1 B1 1.395(2) . ? F2 B1 1.382(2) . ? F3 B1 1.397(2) . ? F4 B1 1.396(2) . ? 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 C6 S1 C7 103.05(8) . . ? C14 O1 C15 111.66(12) . . ? C17 O2 C16 111.87(12) . . ? C12 N1 C1 124.55(13) . . ? C12 N1 C13 117.05(12) . . ? C1 N1 C13 118.28(12) . . ? N1 C1 C6 122.30(14) . . ? N1 C1 C2 120.70(14) . . ? C6 C1 C2 117.00(14) . . ? C3 C2 C1 120.84(15) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 121.26(15) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.58(15) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.06(15) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.10(14) . . ? C5 C6 S1 115.31(12) . . ? C1 C6 S1 123.59(12) . . ? C8 C7 C12 121.05(14) . . ? C8 C7 S1 114.93(12) . . ? C12 C7 S1 123.91(12) . . ? C9 C8 C7 120.33(15) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.32(15) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 121.53(15) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.63(15) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? N1 C12 C11 120.97(14) . . ? N1 C12 C7 121.95(14) . . ? C11 C12 C7 117.08(14) . . ? N1 C13 C14 114.71(13) . . ? N1 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? N1 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? O1 C14 C13 108.90(13) . . ? O1 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? O1 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O1 C15 C16 108.75(13) . . ? O1 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O1 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O2 C16 C15 109.43(13) . . ? O2 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O2 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F2 B1 F1 110.02(14) . . ? F2 B1 F4 109.80(15) . . ? F1 B1 F4 108.72(14) . . ? F2 B1 F3 110.44(14) . . ? F1 B1 F3 108.47(15) . . ? F4 B1 F3 109.35(14) . . ? 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 C12 N1 C1 C6 9.2(2) . . . . ? C13 N1 C1 C6 -166.65(14) . . . . ? C12 N1 C1 C2 -171.15(14) . . . . ? C13 N1 C1 C2 13.0(2) . . . . ? N1 C1 C2 C3 -176.32(14) . . . . ? C6 C1 C2 C3 3.4(2) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C2 C3 C4 C5 -2.5(2) . . . . ? C3 C4 C5 C6 1.4(2) . . . . ? C4 C5 C6 C1 2.2(2) . . . . ? C4 C5 C6 S1 -177.98(12) . . . . ? N1 C1 C6 C5 175.18(14) . . . . ? C2 C1 C6 C5 -4.5(2) . . . . ? N1 C1 C6 S1 -4.6(2) . . . . ? C2 C1 C6 S1 175.69(12) . . . . ? C7 S1 C6 C5 178.00(12) . . . . ? C7 S1 C6 C1 -2.16(15) . . . . ? C6 S1 C7 C8 -177.95(12) . . . . ? C6 S1 C7 C12 5.77(15) . . . . ? C12 C7 C8 C9 2.0(2) . . . . ? S1 C7 C8 C9 -174.40(12) . . . . ? C7 C8 C9 C10 -2.0(2) . . . . ? C8 C9 C10 C11 0.1(2) . . . . ? C9 C10 C11 C12 1.9(2) . . . . ? C1 N1 C12 C11 175.93(14) . . . . ? C13 N1 C12 C11 -8.2(2) . . . . ? C1 N1 C12 C7 -5.3(2) . . . . ? C13 N1 C12 C7 170.58(13) . . . . ? C10 C11 C12 N1 177.01(14) . . . . ? C10 C11 C12 C7 -1.8(2) . . . . ? C8 C7 C12 N1 -178.89(14) . . . . ? S1 C7 C12 N1 -2.8(2) . . . . ? C8 C7 C12 C11 -0.1(2) . . . . ? S1 C7 C12 C11 175.97(11) . . . . ? C12 N1 C13 C14 85.82(17) . . . . ? C1 N1 C13 C14 -98.02(16) . . . . ? C15 O1 C14 C13 174.76(13) . . . . ? N1 C13 C14 O1 69.93(17) . . . . ? C14 O1 C15 C16 -166.69(13) . . . . ? C17 O2 C16 C15 178.85(13) . . . . ? O1 C15 C16 O2 -65.52(17) . . . . ? _refine_diff_density_max 0.308 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.057 _shelx_res_file ; TITL m19080 : space group P21/n m19080.res created by SHELXL-2018/3 at 19:05:27 on 19-Mar-2019 CELL 0.71073 10.2318 6.8098 24.3279 90.000 93.294 90.000 ZERR 4.000 0.0003 0.0002 0.0009 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H B F N O S UNIT 68 76 4 16 4 8 4 TEMP -183 SIZE 0.22 0.08 0.02 REM FORM cut lath REM COLR black REM One reflection obscured by the beamstop: OMIT 1 0 1 L.S. 10 BOND $H LIST 4 ACTA CONF HTAB FMAP 2 PLAN 5 REM EXTI 0.001006 not significant. WGHT 0.029700 1.088100 FVAR 0.43927 S1 7 0.631612 0.286754 0.544396 11.00000 0.01380 0.01508 = 0.01036 0.00083 -0.00034 -0.00034 O1 6 0.448401 0.450056 0.322141 11.00000 0.01562 0.01911 = 0.01654 0.00644 -0.00190 -0.00181 O2 6 0.565936 0.813367 0.296383 11.00000 0.02336 0.02084 = 0.01109 -0.00205 0.00181 -0.00340 N1 5 0.493743 0.221314 0.427921 11.00000 0.01257 0.01155 = 0.01092 -0.00080 0.00016 0.00029 C1 1 0.626152 0.271910 0.430665 11.00000 0.01218 0.00927 = 0.01449 -0.00043 0.00055 0.00193 C2 1 0.693655 0.298712 0.382010 11.00000 0.01697 0.01430 = 0.01146 -0.00057 0.00075 0.00177 AFIX 43 H2 2 0.647102 0.289650 0.347175 11.00000 -1.20000 AFIX 0 C3 1 0.825330 0.337569 0.384539 11.00000 0.01740 0.01647 = 0.01546 0.00145 0.00490 0.00096 AFIX 43 H3 2 0.868548 0.355178 0.351359 11.00000 -1.20000 AFIX 0 C4 1 0.897138 0.351757 0.434954 11.00000 0.01278 0.01513 = 0.01975 0.00256 0.00015 -0.00088 AFIX 43 H4 2 0.988959 0.373496 0.435965 11.00000 -1.20000 AFIX 0 C5 1 0.834321 0.334126 0.482956 11.00000 0.01576 0.01418 = 0.01657 0.00179 -0.00147 -0.00070 AFIX 43 H5 2 0.882316 0.346562 0.517382 11.00000 -1.20000 AFIX 0 C6 1 0.699073 0.297694 0.481312 11.00000 0.01570 0.00940 = 0.01156 0.00084 -0.00023 0.00110 C7 1 0.467970 0.249690 0.527326 11.00000 0.01360 0.00931 = 0.01294 0.00078 -0.00042 0.00130 C8 1 0.387886 0.241600 0.572217 11.00000 0.01830 0.01251 = 0.01207 0.00072 0.00209 0.00383 AFIX 43 H8 2 0.424099 0.267851 0.608302 11.00000 -1.20000 AFIX 0 C9 1 0.257589 0.195977 0.564250 11.00000 0.01903 0.01311 = 0.01512 0.00248 0.00679 0.00393 AFIX 43 H9 2 0.203984 0.186432 0.594753 11.00000 -1.20000 AFIX 0 C10 1 0.204558 0.163713 0.510844 11.00000 0.01425 0.01219 = 0.01963 0.00109 0.00313 0.00074 AFIX 43 H10 2 0.114282 0.132303 0.505378 11.00000 -1.20000 AFIX 0 C11 1 0.280010 0.176353 0.465951 11.00000 0.01535 0.01157 = 0.01402 -0.00041 0.00045 0.00052 AFIX 43 H11 2 0.240724 0.157484 0.430003 11.00000 -1.20000 AFIX 0 C12 1 0.415726 0.217240 0.472823 11.00000 0.01435 0.00709 = 0.01426 0.00083 0.00253 0.00172 C13 1 0.432879 0.154465 0.374160 11.00000 0.01538 0.01412 = 0.01036 -0.00284 -0.00104 -0.00144 AFIX 23 H13A 2 0.372302 0.044870 0.380939 11.00000 -1.20000 H13B 2 0.502570 0.102662 0.351566 11.00000 -1.20000 AFIX 0 C14 1 0.358061 0.312039 0.341456 11.00000 0.01486 0.01812 = 0.01244 0.00087 -0.00185 -0.00217 AFIX 23 H14A 2 0.307295 0.251924 0.309923 11.00000 -1.20000 H14B 2 0.296076 0.378639 0.365079 11.00000 -1.20000 AFIX 0 C15 1 0.384803 0.593494 0.286683 11.00000 0.01768 0.02235 = 0.01605 0.00477 -0.00291 0.00313 AFIX 23 H15A 2 0.334043 0.685595 0.308632 11.00000 -1.20000 H15B 2 0.323613 0.527822 0.259553 11.00000 -1.20000 AFIX 0 C16 1 0.486854 0.703462 0.257463 11.00000 0.02183 0.01927 = 0.01042 0.00019 -0.00174 -0.00134 AFIX 23 H16A 2 0.542084 0.609976 0.237979 11.00000 -1.20000 H16B 2 0.444244 0.793113 0.229860 11.00000 -1.20000 AFIX 0 C17 1 0.666346 0.917934 0.271008 11.00000 0.02271 0.02308 = 0.01763 -0.00170 0.00293 -0.00319 AFIX 137 H17A 2 0.718467 0.826247 0.250243 11.00000 -1.50000 H17B 2 0.722924 0.982892 0.299352 11.00000 -1.50000 H17C 2 0.626941 1.016827 0.245917 11.00000 -1.50000 AFIX 0 F1 4 -0.038021 0.088098 0.585606 11.00000 0.02561 0.03582 = 0.02039 -0.00417 0.00461 -0.00024 F2 4 0.041709 0.188378 0.670220 11.00000 0.02012 0.04038 = 0.02430 0.00578 -0.00766 -0.00549 F3 4 -0.166763 0.070264 0.658149 11.00000 0.01997 0.03267 = 0.02339 0.00526 0.00315 -0.00890 F4 4 -0.114366 0.368074 0.622784 11.00000 0.02446 0.02312 = 0.03389 0.00544 0.00312 0.00260 B1 3 -0.068430 0.178846 0.634658 11.00000 0.01313 0.02321 = 0.01578 0.00153 -0.00005 -0.00147 HKLF 4 REM m19080 : space group P21/n REM wR2 = 0.0845, GooF = S = 1.088, Restrained GooF = 1.088 for all data REM R1 = 0.0353 for 3150 Fo > 4sig(Fo) and 0.0491 for all 3858 data REM 236 parameters refined using 0 restraints END WGHT 0.0297 1.0882 REM Instructions for potential hydrogen bonds HTAB C2 O1 EQIV $1 x+1, y, z HTAB C5 F1_$1 HTAB C5 F4_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C8 O2_$2 EQIV $3 -x+1, -y, -z+1 HTAB C13 S1_$3 EQIV $4 -x, -y, -z+1 HTAB C13 F3_$4 EQIV $5 x, y-1, z HTAB C13 O2_$5 EQIV $6 -x, -y+1, -z+1 HTAB C14 F4_$6 HTAB C15 F3_$6 EQIV $7 x+1/2, -y+1/2, z-1/2 HTAB C15 F3_$7 HTAB C16 F2_$7 REM Highest difference peak 0.308, deepest hole -0.335, 1-sigma level 0.057 Q1 1 0.3542 0.1523 0.4698 11.00000 0.05 0.31 Q2 1 0.3440 0.2397 0.4686 11.00000 0.05 0.29 Q3 1 0.4426 0.2371 0.4994 11.00000 0.05 0.29 Q4 1 0.4538 0.2173 0.4506 11.00000 0.05 0.28 Q5 1 0.6605 0.2712 0.4563 11.00000 0.05 0.28 ; _shelx_res_checksum 99275 _shelx_hkl_file ; 2 0 0 719.372 16.4736 6 2 0 0 675.918 15.7867 2 2 0 0 722.908 16.5447 4 2 0 0 666.320 16.7205 5 2 0 0 685.523 16.1531 6 -2 0 0 629.748 15.7640 6 -2 0 0 693.056 16.4748 4 -2 0 0 701.111 15.9869 6 -2 0 0 663.658 15.5291 2 3 0 0 1.26470 2.04851 5 -3 0 0 -0.7906 1.17285 2 -3 0 0 0.21614 1.76088 6 3 0 0 0.09435 1.49502 6 3 0 0 0.35719 1.46994 2 3 0 0 0.77172 1.75733 4 -3 0 0 -0.1811 1.51270 4 -4 0 0 839.552 24.1752 4 -4 0 0 870.406 22.8738 2 4 0 0 870.906 24.1165 6 -4 0 0 844.787 23.5202 6 4 0 0 874.279 23.4967 2 4 0 0 884.993 24.2383 4 4 0 0 860.795 25.1094 5 4 0 0 877.125 24.1171 6 -4 0 0 882.967 23.1904 6 5 0 0 -0.2244 2.30288 5 5 0 0 -0.5164 1.91534 6 -5 0 0 0.31105 1.93017 6 -5 0 0 1.66335 1.92644 6 -5 0 0 -2.6202 1.54250 2 5 0 0 2.20581 2.07811 4 5 0 0 -0.1996 1.81845 6 5 0 0 0.46754 1.73091 2 -5 0 0 1.29202 2.23054 4 6 0 0 110.787 9.60904 6 -6 0 0 99.7304 8.21499 6 -6 0 0 99.4563 8.88443 6 6 0 0 95.0417 9.54906 5 6 0 0 93.8689 9.18966 6 -6 0 0 93.8398 9.22932 4 6 0 0 104.144 9.04266 4 6 0 0 99.0555 8.91562 2 -6 0 0 102.841 8.43778 2 7 0 0 1.73983 0.99182 7 7 0 0 -0.3338 3.06080 6 -7 0 0 0.03745 1.80650 2 7 0 0 -1.9371 2.23845 4 7 0 0 -1.6286 2.25132 5 -7 0 0 0.38430 3.35368 4 -7 0 0 -1.7159 2.43629 6 7 0 0 -1.3389 2.26760 2 7 0 0 1.76135 2.81519 6 8 0 0 7.04929 4.48759 6 -8 0 0 3.80888 3.50500 4 -8 0 0 -2.1040 3.12933 6 -8 0 0 5.73574 4.01990 6 8 0 0 2.02937 3.18100 2 8 0 0 7.72905 4.35846 5 -8 0 0 0.95082 3.15106 2 9 0 0 -2.9238 2.94061 5 -9 0 0 -1.5125 2.96030 4 -9 0 0 0.78270 3.31119 6 9 0 0 2.65392 3.14628 2 9 0 0 0.61456 3.70012 6 -10 0 0 39.5932 9.31564 4 10 0 0 60.6521 10.2100 5 10 0 0 58.2257 8.80967 2 -10 0 0 32.0192 7.99752 6 10 0 0 42.2520 8.63287 6 11 0 0 6.86129 3.90546 2 -11 0 0 -0.4677 4.14199 4 -11 0 0 -1.8544 4.19443 6 11 0 0 3.12637 4.62689 5 -12 0 0 107.656 15.0060 4 12 0 0 104.726 13.6113 2 13 0 0 4.17017 5.65657 2 -13 0 0 -5.5989 5.73039 4 0 -1 0 -0.0924 0.66651 2 0 -1 0 0.49550 1.13153 7 0 1 0 0.54407 0.53409 4 0 1 0 0.16769 0.66948 2 0 1 0 -0.3585 0.78588 7 -1 -1 0 385.515 7.43660 3 1 -1 0 398.067 8.95644 5 -1 -1 0 361.460 11.3179 4 1 -1 0 383.644 7.85720 4 1 -1 0 401.747 9.98573 6 1 -1 0 381.653 9.92740 6 -1 -1 0 377.293 10.5364 7 1 -1 0 389.136 10.7475 7 1 -1 0 392.449 11.1395 2 1 1 0 384.421 7.28439 3 1 1 0 383.621 10.6299 7 -1 1 0 405.880 10.5147 7 -1 1 0 401.889 10.1402 6 1 1 0 432.451 10.5959 4 -1 1 0 408.565 11.2446 2 -1 1 0 375.706 7.91901 4 -1 1 0 379.331 10.1343 6 2 -1 0 1100.17 24.4345 6 2 -1 0 1127.22 21.9426 4 -2 -1 0 1136.16 19.4921 3 -2 -1 0 1103.31 24.7255 4 -2 -1 0 1149.78 19.5596 6 2 -1 0 1078.03 24.2756 6 2 -1 0 1124.67 23.5758 5 2 -1 0 1097.22 25.4448 2 -2 -1 0 1101.84 22.4161 7 2 -1 0 1104.86 22.3223 7 -2 -1 0 1105.30 19.6483 6 2 1 0 1102.17 20.8255 6 -2 1 0 1091.09 24.6741 6 2 1 0 1103.86 24.0828 5 2 1 0 1103.59 22.8227 7 2 1 0 1144.44 21.2253 6 -2 1 0 1093.78 22.0375 4 -2 1 0 1165.31 25.6602 2 2 1 0 1117.36 24.6313 4 -2 1 0 1117.57 24.4570 6 2 1 0 1097.55 20.0910 2 -3 -1 0 67.3407 4.15903 6 3 -1 0 64.5420 5.56007 6 -3 -1 0 59.9529 3.84849 6 -3 -1 0 60.5051 3.74751 2 3 -1 0 62.1346 4.81033 4 3 -1 0 60.0452 6.12419 2 3 -1 0 61.7653 5.83705 6 3 -1 0 58.4607 3.89065 7 -3 -1 0 61.1597 5.73654 4 3 -1 0 57.3747 5.39283 5 3 1 0 70.0485 5.85845 4 -3 1 0 62.8904 4.82318 4 3 1 0 64.4065 5.97022 5 3 1 0 63.1622 4.63125 6 3 1 0 66.3394 4.37045 7 -3 1 0 59.4030 5.88433 6 -3 1 0 60.5284 5.63490 2 3 1 0 67.8408 4.35024 2 -3 1 0 68.6618 5.68012 6 3 1 0 57.8689 4.58056 6 4 -1 0 726.155 16.3697 7 4 -1 0 708.281 20.1079 4 4 -1 0 710.130 22.3322 6 -4 -1 0 700.668 22.5213 4 -4 -1 0 702.458 18.5989 6 4 -1 0 732.351 22.9294 2 4 -1 0 686.487 21.6909 5 -4 -1 0 716.834 17.7545 2 4 -1 0 703.324 22.2085 6 -4 1 0 698.873 22.2325 6 4 1 0 713.044 22.5105 5 -4 1 0 730.390 22.2801 2 4 1 0 710.074 18.5744 2 -4 1 0 732.365 20.8106 4 -4 1 0 728.144 22.0419 6 4 1 0 700.707 17.1056 7 4 1 0 725.285 20.1458 6 4 1 0 744.991 20.3315 6 4 1 0 707.194 22.1992 4 5 -1 0 118.853 9.62653 6 5 -1 0 128.439 8.54148 4 -5 -1 0 121.450 7.81695 6 5 -1 0 120.679 5.66406 7 -5 -1 0 128.013 10.1695 4 5 -1 0 129.937 9.65065 6 -5 -1 0 125.777 7.66552 6 5 -1 0 126.500 9.54392 5 -5 -1 0 115.668 7.08459 2 5 -1 0 110.084 9.16784 2 5 1 0 131.296 8.88865 6 5 1 0 119.978 7.81333 2 -5 1 0 118.443 9.31775 2 -5 1 0 119.360 9.68359 6 -5 1 0 118.204 9.23737 6 5 1 0 126.831 6.36839 7 5 1 0 119.598 9.86905 5 5 1 0 114.088 9.33832 4 -5 1 0 120.015 8.90894 4 5 1 0 118.602 8.58495 6 6 -1 0 98.4364 9.68612 2 6 -1 0 103.485 8.60063 4 6 -1 0 102.970 9.71261 6 -6 -1 0 100.975 7.47595 6 -6 -1 0 95.2443 7.25406 2 6 -1 0 102.671 5.21247 7 -6 -1 0 116.391 8.40603 6 6 -1 0 108.637 10.0934 5 6 -1 0 104.245 9.60755 6 6 1 0 97.7013 10.1249 5 -6 1 0 86.6562 8.85019 2 6 1 0 101.505 8.88944 6 -6 1 0 95.3071 9.44073 6 6 1 0 104.751 7.97718 2 6 1 0 97.7285 8.79278 6 6 1 0 91.9997 5.69546 7 -6 1 0 94.8272 8.81780 4 7 -1 0 -1.6570 2.89194 6 -7 -1 0 -2.3257 1.87145 6 7 -1 0 -1.5856 1.94733 2 -7 -1 0 -1.9149 1.75411 2 -7 -1 0 2.17131 2.49796 6 -7 -1 0 -3.8502 2.62717 4 7 -1 0 2.58709 3.29783 5 7 -1 0 -0.4456 1.08339 7 7 -1 0 -2.0434 2.87009 4 -7 1 0 -0.7079 1.92395 4 7 1 0 -2.4491 2.59716 5 -7 1 0 6.82022 3.77990 6 7 1 0 -1.1303 2.57921 6 -7 1 0 -0.1742 2.57520 6 7 1 0 -1.5411 2.68740 2 -7 1 0 -2.6476 2.59533 2 7 1 0 0.35155 1.41236 7 7 1 0 12.1227 3.91224 6 8 -1 0 7.97127 4.49425 2 -8 -1 0 14.6226 5.05431 6 8 -1 0 4.00344 3.72231 5 -8 -1 0 10.1150 4.67745 4 8 -1 0 8.55378 4.26390 6 -8 -1 0 9.87201 3.65064 2 -8 -1 0 11.9818 4.42960 6 -8 1 0 8.99266 4.68765 4 8 1 0 14.6267 5.34709 6 -8 1 0 12.1788 5.18139 6 8 1 0 10.3873 2.54934 7 8 1 0 9.98212 4.09572 2 8 1 0 18.3170 6.08901 5 9 -1 0 47.3140 8.83514 2 9 -1 0 53.8178 9.28284 6 9 -1 0 38.4856 8.90247 5 -9 -1 0 58.4513 9.27503 4 -9 -1 0 40.6863 6.88671 2 -9 -1 0 62.4350 7.82535 6 -9 -1 0 37.0268 7.00800 6 9 1 0 42.7767 8.37543 6 -9 1 0 47.9907 9.02087 6 -9 1 0 36.4851 7.57618 4 9 1 0 49.8531 7.88159 2 9 1 0 43.7941 3.59793 7 9 1 0 50.5154 9.60307 5 10 -1 0 268.068 20.4021 6 10 -1 0 246.357 18.9917 2 -10 -1 0 218.446 18.5212 4 -10 -1 0 234.149 15.6989 6 10 -1 0 216.424 18.9192 5 10 1 0 248.395 19.7298 5 -10 1 0 238.142 18.3856 4 10 1 0 220.760 15.9542 2 -10 1 0 242.953 18.9415 6 10 1 0 241.637 18.4366 6 -11 -1 0 72.1936 11.7927 4 11 -1 0 64.2078 11.4814 6 11 -1 0 71.3785 12.0742 2 11 -1 0 75.7376 12.4982 5 11 1 0 55.9241 9.69462 2 11 1 0 68.6570 11.7210 5 -11 1 0 44.3646 9.32961 4 11 1 0 58.0606 11.3651 6 12 -1 0 11.4021 6.17783 2 -12 -1 0 1.31945 4.87192 4 -12 1 0 -4.7064 5.49973 4 12 1 0 8.06459 5.30557 2 -13 -1 0 20.8715 9.20150 4 13 -1 0 26.1751 10.0861 2 -13 1 0 45.2405 10.4991 4 0 -2 0 9999.99 165.758 1 0 2 0 9640.96 165.340 1 1 -2 0 3931.83 61.6863 5 -1 -2 0 3760.98 65.1371 2 1 -2 0 3886.21 69.3935 2 -1 -2 0 3925.61 66.3825 4 1 -2 0 3856.07 70.3262 7 -1 -2 0 3752.68 70.2654 7 1 -2 0 3925.65 63.9279 6 1 2 0 3984.95 64.1183 2 -1 2 0 3872.23 69.1172 2 -1 2 0 3983.31 65.7186 6 -1 2 0 3848.34 61.0595 4 1 2 0 3858.44 63.3853 5 1 2 0 3985.25 71.2959 7 -1 2 0 3931.77 66.1644 6 1 2 0 3936.73 66.2823 4 1 2 0 3778.12 65.3797 3 2 -2 0 42.6337 5.11170 2 2 -2 0 46.5673 4.32164 6 2 -2 0 44.9399 2.73953 4 -2 -2 0 42.7418 4.65516 4 -2 -2 0 45.0900 2.50045 3 2 -2 0 41.0004 4.19728 6 2 -2 0 41.3850 4.94095 7 2 -2 0 44.4725 3.61135 5 -2 -2 0 48.2085 5.13306 7 -2 2 0 45.7871 4.84107 6 -2 2 0 43.0421 4.55097 6 2 2 0 40.0149 4.08424 5 -2 2 0 41.8227 5.18038 2 2 2 0 48.5337 2.31672 3 2 2 0 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