data_at111120_1_1 _audit_creation_date 2020-11-13 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelx_SHELXL_version_number '2018/3' loop_ _audit_author_name _audit_author_email _audit_author_address 'Zhang, K.' '' LAC-Togni _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_acknowledgements ; X-Ray services provided by SMoCC - The Small Molecule Crystallography Center of ETH Zurich. ; _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 'C18 H15 F2 N O2' _chemical_formula_sum 'C18 H15 F2 N O2' _chemical_formula_weight 315.31 _chemical_melting_point ? _chemical_oxdiff_formula C18H15F2NO2 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' 'N' 'N' 0.0311 0.0180 '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' _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 17.0365(3) _cell_length_b 5.52810(10) _cell_length_c 15.6934(3) _cell_angle_alpha 90 _cell_angle_beta 101.292(2) _cell_angle_gamma 90 _cell_volume 1449.39(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10322 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 79.6140 _cell_measurement_theta_min 2.6340 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.68a (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 colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plank _exptl_crystal_F_000 656 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0157 2 0 10 0.0130 2 3 5 0.0613 1 1 9 0.0345 0 -3 7 0.0518 -7 0 9 0.0210 6 -2 -8 0.0482 11 0 -4 0.0282 9 0 4 0.0265 0 -1 0 0.0673 2 2 -1 0.0727 -1 0 0 0.0203 1 0 0 0.0287 0 0 -1 0.0101 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_min 0.026 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 0.0017 -0.0007 0.9989 0.0110 -0.0993 0.0046 1.7624 0.0670 9.5481 -0.0248 -0.9909 0.1324 2.0919 2.9251 5.0914 -0.6066 -0.6390 -0.4731 1.3013 1.3479 8.9519 -0.2296 -0.9585 -0.1690 -0.1370 -2.5255 7.1245 0.5388 -0.6311 0.5581 -7.3766 -0.0693 8.7655 0.6003 -0.7006 -0.3856 5.8191 -1.9212 -7.6397 -0.1283 0.6824 0.7197 10.7368 0.0281 -4.3111 -0.7682 0.1826 0.6137 9.1778 0.0026 3.9265 -0.5693 -0.5996 0.5624 -0.0006 -0.9997 -0.0034 0.1787 0.0295 0.2117 2.0010 1.9997 -0.9931 -0.5018 -0.0053 -0.3090 -1.0007 0.0002 0.0005 0.0667 0.0228 -0.0596 1.0007 -0.0002 -0.0005 -0.0667 -0.0228 0.0596 -0.0017 0.0007 -0.9989 -0.0110 0.0993 -0.0046 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16452 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.950 _diffrn_reflns_theta_min 2.645 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 300K' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.981 _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 -63.00 -33.00 0.50 0.56 -- -48.62 57.00 60.00 60 2 \w -26.00 1.00 0.50 0.56 -- -48.62 57.00 60.00 54 3 \w -8.00 18.00 0.50 0.56 -- -48.62 19.00 30.00 52 4 \w -9.00 22.00 0.50 0.56 -- -48.62 19.00 -60.00 62 5 \w -8.00 18.00 0.50 0.56 -- -48.62 19.00 -90.00 52 6 \w -38.00 -13.00 0.50 1.96 -- -70.00 38.00 30.00 50 7 \w -36.00 5.00 0.50 1.96 -- -70.00 38.00 120.00 82 8 \w -61.00 -31.00 0.50 0.56 -- -48.62 -77.00 0.00 60 9 \w -91.00 -46.00 0.50 1.96 -- -70.00 -77.00 60.00 90 10 \w -89.00 -56.00 0.50 1.96 -- -70.00 -77.00 0.00 66 11 \w -114.00 -75.00 0.50 0.56 -- -48.62 -77.00 0.00 78 12 \w -142.00 -86.00 0.50 1.96 -- -70.00 -57.00 -30.00 112 13 \w -55.00 3.00 0.50 1.96 -- -70.00 54.00 -99.00 116 14 \w -23.00 5.00 0.50 0.56 -- 48.62 -19.00 120.00 56 15 \w -25.00 5.00 0.50 0.56 -- 48.62 -19.00 150.00 60 16 \w -27.00 -2.00 0.50 0.56 -- 48.62 -19.00 30.00 50 17 \w 40.00 104.00 0.50 1.96 -- 110.00 -99.00 150.00 128 18 \w 43.00 68.00 0.50 1.96 -- 110.00 -57.00 120.00 50 19 \w 44.00 92.00 0.50 1.96 -- 110.00 -99.00 90.00 96 20 \w 44.00 69.00 0.50 1.96 -- 110.00-125.00 150.00 50 21 \w 40.00 66.00 0.50 1.96 -- 110.00 -57.00 0.00 52 22 \w 38.00 63.00 0.50 1.96 -- 110.00 -57.00 -30.00 50 23 \w 38.00 68.00 0.50 1.96 -- 110.00 -57.00 -90.00 60 24 \w 68.00 98.00 0.50 1.96 -- 110.00 -99.00 -30.00 60 25 \w 48.00 104.00 0.50 1.96 -- 110.00 -99.00-120.00 112 26 \w 90.00 127.00 0.50 1.96 -- 110.00 -77.00-180.00 74 27 \w 45.00 76.00 0.50 1.96 -- 110.00 -77.00-180.00 62 28 \w 125.00 178.00 0.50 1.96 -- 110.00 54.00 -99.00 106 29 \w 144.00 175.00 0.50 1.96 -- 110.00 77.00 -60.00 62 30 \w 137.00 169.00 0.50 1.96 -- 110.00 77.00 0.00 64 31 \w 153.00 178.00 0.50 1.96 -- 110.00 57.00 60.00 50 32 \w 135.00 176.00 0.50 1.96 -- 110.00 77.00 30.00 82 33 \w 122.00 171.00 0.50 1.96 -- 110.00 77.00 -30.00 98 34 \w 106.00 134.00 0.50 1.96 -- 110.00 38.00 30.00 56 35 \w 105.00 132.00 0.50 1.96 -- 110.00 38.00 0.00 54 36 \w 98.00 142.00 0.50 1.96 -- 110.00 57.00 30.00 88 37 \w 98.00 149.00 0.50 1.96 -- 110.00 57.00 60.00 102 38 \w 149.00 178.00 0.50 1.96 -- 110.00 38.00 150.00 58 39 \w 104.00 130.00 0.50 1.96 -- 110.00 38.00 150.00 52 40 \w 87.00 113.00 0.50 1.96 -- 110.00 77.00 30.00 52 41 \w 86.00 119.00 0.50 1.96 -- 110.00 77.00 -30.00 66 42 \w 88.00 141.00 0.50 1.96 -- 110.00 77.00 -60.00 106 43 \w 86.00 127.00 0.50 1.96 -- 110.00 77.00 0.00 82 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0666732000 _diffrn_orient_matrix_UB_12 -0.1787744000 _diffrn_orient_matrix_UB_13 0.0109650000 _diffrn_orient_matrix_UB_21 -0.0228171000 _diffrn_orient_matrix_UB_22 -0.0291706000 _diffrn_orient_matrix_UB_23 -0.0993628000 _diffrn_orient_matrix_UB_31 0.0594685000 _diffrn_orient_matrix_UB_32 -0.2118643000 _diffrn_orient_matrix_UB_33 0.0043740000 _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 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2767 _reflns_number_total 3091 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 1.171.40.68a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.248 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.045 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 3091 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0365 _refine_ls_restrained_S_all 1.049 _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^)+(0.0459P)^2^+0.7219P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.0980 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C5(H5), C6(H6) 2.b Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C) ; _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 F1 F 0.09739(4) 0.13203(15) 0.09080(5) 0.02475(19) Uani 1 1 d . . . . . F2 F 0.14960(5) -0.22884(14) 0.10316(5) 0.02510(19) Uani 1 1 d . . . . . O1 O 0.22677(6) 0.03226(18) -0.01290(6) 0.0257(2) Uani 1 1 d . . . . . O2 O 0.32629(5) 0.65094(17) 0.12193(6) 0.0232(2) Uani 1 1 d . . . . . N1 N 0.26945(6) 0.28164(19) 0.10827(7) 0.0186(2) Uani 1 1 d . . . . . C1 C 0.32571(9) 0.4541(3) -0.01335(9) 0.0301(3) Uani 1 1 d . . . . . H1A H 0.345632 0.605515 -0.030266 0.045 Uiso 1 1 calc R U . . . H1B H 0.277470 0.412158 -0.053376 0.045 Uiso 1 1 calc R U . . . H1C H 0.365144 0.330327 -0.013849 0.045 Uiso 1 1 calc R U . . . C2 C 0.30849(7) 0.4762(2) 0.07566(9) 0.0204(3) Uani 1 1 d . . . . . C3 C 0.22508(7) 0.1002(2) 0.05964(8) 0.0198(3) Uani 1 1 d . . . . . C4 C 0.16776(7) 0.0086(2) 0.11685(9) 0.0202(3) Uani 1 1 d . . . . . C5 C 0.20762(7) 0.0661(2) 0.20947(8) 0.0185(3) Uani 1 1 d . . . . . H5 H 0.244999 -0.065872 0.229900 0.022 Uiso 1 1 calc R U . . . C6 C 0.25825(7) 0.2942(2) 0.19989(8) 0.0182(3) Uani 1 1 d . . . . . H6 H 0.227367 0.439340 0.207633 0.022 Uiso 1 1 calc R U . . . C7 C 0.15171(7) 0.0890(2) 0.27312(8) 0.0184(3) Uani 1 1 d . . . . . C8 C 0.10100(7) 0.2882(2) 0.27128(9) 0.0209(3) Uani 1 1 d . . . . . H8 H 0.102165 0.411599 0.231268 0.025 Uiso 1 1 calc R U . . . C9 C 0.04879(8) 0.3030(2) 0.32895(9) 0.0239(3) Uani 1 1 d . . . . . H9 H 0.015025 0.435861 0.327203 0.029 Uiso 1 1 calc R U . . . C10 C 0.04688(8) 0.1203(3) 0.38911(9) 0.0251(3) Uani 1 1 d . . . . . H10 H 0.012099 0.131171 0.427831 0.030 Uiso 1 1 calc R U . . . C11 C 0.09678(8) -0.0784(3) 0.39148(9) 0.0251(3) Uani 1 1 d . . . . . H11 H 0.095529 -0.201159 0.431718 0.030 Uiso 1 1 calc R U . . . C12 C 0.14886(8) -0.0940(2) 0.33343(9) 0.0215(3) Uani 1 1 d . . . . . H12 H 0.182082 -0.228032 0.334973 0.026 Uiso 1 1 calc R U . . . C13 C 0.33787(7) 0.3013(2) 0.26295(8) 0.0183(3) Uani 1 1 d . . . . . C14 C 0.39525(8) 0.1221(2) 0.26110(9) 0.0216(3) Uani 1 1 d . . . . . H14 H 0.383728 -0.006353 0.222398 0.026 Uiso 1 1 calc R U . . . C15 C 0.46938(8) 0.1342(2) 0.31661(9) 0.0231(3) Uani 1 1 d . . . . . H15 H 0.507318 0.014424 0.314694 0.028 Uiso 1 1 calc R U . . . C16 C 0.48709(8) 0.3241(3) 0.37487(9) 0.0227(3) Uani 1 1 d . . . . . H16 H 0.536881 0.332310 0.411799 0.027 Uiso 1 1 calc R U . . . C17 C 0.43020(8) 0.5020(2) 0.37785(9) 0.0235(3) Uani 1 1 d . . . . . H17 H 0.441705 0.629163 0.417091 0.028 Uiso 1 1 calc R U . . . C18 C 0.35596(8) 0.4900(2) 0.32215(8) 0.0214(3) Uani 1 1 d . . . . . H18 H 0.318010 0.609459 0.324535 0.026 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 F1 0.0168(4) 0.0284(4) 0.0282(4) 0.0023(3) 0.0022(3) 0.0018(3) F2 0.0269(4) 0.0181(4) 0.0307(4) -0.0036(3) 0.0067(3) -0.0071(3) O1 0.0297(5) 0.0240(5) 0.0242(5) -0.0036(4) 0.0074(4) -0.0030(4) O2 0.0221(5) 0.0185(4) 0.0292(5) 0.0003(4) 0.0060(4) -0.0033(4) N1 0.0186(5) 0.0165(5) 0.0212(5) -0.0004(4) 0.0051(4) -0.0015(4) C1 0.0318(7) 0.0325(8) 0.0282(7) -0.0008(6) 0.0116(6) -0.0090(6) C2 0.0145(5) 0.0199(6) 0.0268(6) 0.0031(5) 0.0037(5) 0.0002(5) C3 0.0175(6) 0.0172(6) 0.0245(6) 0.0004(5) 0.0036(5) 0.0005(5) C4 0.0179(6) 0.0158(6) 0.0269(6) -0.0004(5) 0.0045(5) -0.0003(5) C5 0.0160(6) 0.0146(6) 0.0252(6) 0.0014(5) 0.0050(5) 0.0013(4) C6 0.0182(6) 0.0154(6) 0.0220(6) 0.0000(4) 0.0065(5) 0.0004(4) C7 0.0156(6) 0.0170(6) 0.0222(6) -0.0005(5) 0.0028(5) -0.0013(4) C8 0.0181(6) 0.0175(6) 0.0273(6) 0.0018(5) 0.0048(5) 0.0004(5) C9 0.0190(6) 0.0207(6) 0.0327(7) -0.0024(5) 0.0064(5) 0.0022(5) C10 0.0202(6) 0.0300(7) 0.0263(7) -0.0029(5) 0.0072(5) -0.0020(5) C11 0.0244(7) 0.0252(7) 0.0266(7) 0.0041(5) 0.0075(5) -0.0012(5) C12 0.0203(6) 0.0180(6) 0.0262(6) 0.0014(5) 0.0044(5) 0.0012(5) C13 0.0173(6) 0.0166(6) 0.0221(6) 0.0018(5) 0.0064(5) -0.0011(5) C14 0.0200(6) 0.0176(6) 0.0283(7) -0.0026(5) 0.0072(5) -0.0004(5) C15 0.0183(6) 0.0213(6) 0.0307(7) 0.0010(5) 0.0072(5) 0.0034(5) C16 0.0182(6) 0.0260(7) 0.0232(6) 0.0011(5) 0.0027(5) -0.0007(5) C17 0.0246(6) 0.0219(6) 0.0241(6) -0.0041(5) 0.0050(5) -0.0006(5) C18 0.0206(6) 0.0185(6) 0.0258(6) -0.0011(5) 0.0062(5) 0.0030(5) _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 F1 C4 1.3703(14) . ? F2 C4 1.3562(15) . ? O1 C3 1.2044(16) . ? O2 C2 1.2106(16) . ? N1 C2 1.4123(16) . ? N1 C3 1.3907(16) . ? N1 C6 1.4887(16) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 C2 1.4876(19) . ? C3 C4 1.5359(17) . ? C4 C5 1.5128(18) . ? C5 H5 0.9800 . ? C5 C6 1.5516(17) . ? C5 C7 1.5145(17) . ? C6 H6 0.9800 . ? C6 C13 1.5151(17) . ? C7 C8 1.3966(18) . ? C7 C12 1.3925(18) . ? C8 H8 0.9300 . ? C8 C9 1.3900(19) . ? C9 H9 0.9300 . ? C9 C10 1.387(2) . ? C10 H10 0.9300 . ? C10 C11 1.385(2) . ? C11 H11 0.9300 . ? C11 C12 1.3932(18) . ? C12 H12 0.9300 . ? C13 C14 1.3961(17) . ? C13 C18 1.3906(18) . ? C14 H14 0.9300 . ? C14 C15 1.3884(19) . ? C15 H15 0.9300 . ? C15 C16 1.3859(19) . ? C16 H16 0.9300 . ? C16 C17 1.3879(19) . ? C17 H17 0.9300 . ? C17 C18 1.3911(19) . ? C18 H18 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 C2 N1 C6 118.23(10) . . ? C3 N1 C2 126.48(11) . . ? C3 N1 C6 113.88(10) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? O2 C2 N1 118.08(12) . . ? O2 C2 C1 123.82(12) . . ? N1 C2 C1 118.10(12) . . ? O1 C3 N1 129.23(12) . . ? O1 C3 C4 125.83(12) . . ? N1 C3 C4 104.86(10) . . ? F1 C4 C3 106.31(10) . . ? F1 C4 C5 112.59(10) . . ? F2 C4 F1 105.99(10) . . ? F2 C4 C3 112.20(10) . . ? F2 C4 C5 113.64(10) . . ? C5 C4 C3 105.98(10) . . ? C4 C5 H5 107.4 . . ? C4 C5 C6 103.35(10) . . ? C4 C5 C7 115.42(10) . . ? C6 C5 H5 107.4 . . ? C7 C5 H5 107.4 . . ? C7 C5 C6 115.42(10) . . ? N1 C6 C5 103.57(10) . . ? N1 C6 H6 109.4 . . ? N1 C6 C13 111.36(10) . . ? C5 C6 H6 109.4 . . ? C13 C6 C5 113.67(10) . . ? C13 C6 H6 109.4 . . ? C8 C7 C5 121.25(11) . . ? C12 C7 C5 119.85(11) . . ? C12 C7 C8 118.88(12) . . ? C7 C8 H8 119.8 . . ? C9 C8 C7 120.34(12) . . ? C9 C8 H8 119.8 . . ? C8 C9 H9 119.9 . . ? C10 C9 C8 120.23(12) . . ? C10 C9 H9 119.9 . . ? C9 C10 H10 120.0 . . ? C11 C10 C9 119.97(12) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.84(13) . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.74(12) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C6 120.59(11) . . ? C18 C13 C6 120.59(11) . . ? C18 C13 C14 118.80(12) . . ? C13 C14 H14 119.8 . . ? C15 C14 C13 120.48(12) . . ? C15 C14 H14 119.8 . . ? C14 C15 H15 119.9 . . ? C16 C15 C14 120.29(12) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 120.1 . . ? C15 C16 C17 119.70(12) . . ? C17 C16 H16 120.1 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.02(12) . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 120.71(12) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? 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 F1 C4 C5 C6 -86.70(12) . . . . ? F1 C4 C5 C7 40.27(14) . . . . ? F2 C4 C5 C6 152.79(10) . . . . ? F2 C4 C5 C7 -80.24(13) . . . . ? O1 C3 C4 F1 -81.90(15) . . . . ? O1 C3 C4 F2 33.53(18) . . . . ? O1 C3 C4 C5 158.09(12) . . . . ? N1 C3 C4 F1 95.10(11) . . . . ? N1 C3 C4 F2 -149.47(10) . . . . ? N1 C3 C4 C5 -24.90(13) . . . . ? N1 C6 C13 C14 -54.88(15) . . . . ? N1 C6 C13 C18 123.40(12) . . . . ? C2 N1 C3 O1 21.1(2) . . . . ? C2 N1 C3 C4 -155.76(11) . . . . ? C2 N1 C6 C5 175.08(10) . . . . ? C2 N1 C6 C13 -62.37(14) . . . . ? C3 N1 C2 O2 160.82(12) . . . . ? C3 N1 C2 C1 -19.49(18) . . . . ? C3 N1 C6 C5 7.76(13) . . . . ? C3 N1 C6 C13 130.30(11) . . . . ? C3 C4 C5 C6 29.12(12) . . . . ? C3 C4 C5 C7 156.09(10) . . . . ? C4 C5 C6 N1 -22.52(12) . . . . ? C4 C5 C6 C13 -143.51(10) . . . . ? C4 C5 C7 C8 -72.16(15) . . . . ? C4 C5 C7 C12 106.16(13) . . . . ? C5 C6 C13 C14 61.65(15) . . . . ? C5 C6 C13 C18 -120.07(13) . . . . ? C5 C7 C8 C9 178.49(12) . . . . ? C5 C7 C12 C11 -178.82(12) . . . . ? C6 N1 C2 O2 -4.74(17) . . . . ? C6 N1 C2 C1 174.96(11) . . . . ? C6 N1 C3 O1 -172.81(13) . . . . ? C6 N1 C3 C4 10.33(13) . . . . ? C6 C5 C7 C8 48.44(16) . . . . ? C6 C5 C7 C12 -133.23(12) . . . . ? C6 C13 C14 C15 177.43(12) . . . . ? C6 C13 C18 C17 -177.51(12) . . . . ? C7 C5 C6 N1 -149.49(10) . . . . ? C7 C5 C6 C13 89.52(13) . . . . ? C7 C8 C9 C10 0.3(2) . . . . ? C8 C7 C12 C11 -0.45(19) . . . . ? C8 C9 C10 C11 -0.4(2) . . . . ? C9 C10 C11 C12 0.1(2) . . . . ? C10 C11 C12 C7 0.3(2) . . . . ? C12 C7 C8 C9 0.14(19) . . . . ? C13 C14 C15 C16 0.3(2) . . . . ? C14 C13 C18 C17 0.80(19) . . . . ? C14 C15 C16 C17 0.3(2) . . . . ? C15 C16 C17 C18 -0.4(2) . . . . ? C16 C17 C18 C13 -0.2(2) . . . . ? C18 C13 C14 C15 -0.88(19) . . . . ? _shelx_res_file ; TITL at111120_1_1_a.res in P2(1)/c at111120_1_1.res created by SHELXL-2018/3 at 09:51:18 on 13-Nov-2020 REM Old TITL at111120_1_1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.095, Rweak 0.013, Alpha 0.015, Orientation as input REM Formula found by SHELXT: C18 N O2 F2 CELL 1.54184 17.0365 5.5281 15.6934 90 101.292 90 ZERR 4 0.0003 0.0001 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O UNIT 72 60 8 4 8 L.S. 9 PLAN 5 CONF BOND $H list 4 fmap 2 ACTA MORE -1 REM REM REM WGHT 0.045900 0.721900 FVAR 0.75562 F1 3 0.097390 0.132028 0.090797 11.00000 0.01676 0.02841 = 0.02817 0.00230 0.00221 0.00182 F2 3 0.149601 -0.228845 0.103159 11.00000 0.02690 0.01814 = 0.03069 -0.00358 0.00667 -0.00705 O1 5 0.226774 0.032260 -0.012898 11.00000 0.02970 0.02402 = 0.02419 -0.00355 0.00745 -0.00303 O2 5 0.326292 0.650938 0.121930 11.00000 0.02213 0.01854 = 0.02920 0.00028 0.00599 -0.00327 N1 4 0.269452 0.281640 0.108265 11.00000 0.01858 0.01649 = 0.02117 -0.00036 0.00509 -0.00148 C1 1 0.325711 0.454097 -0.013349 11.00000 0.03181 0.03253 = 0.02819 -0.00081 0.01164 -0.00901 AFIX 137 H1A 2 0.345632 0.605515 -0.030266 11.00000 -1.50000 H1B 2 0.277470 0.412158 -0.053376 11.00000 -1.50000 H1C 2 0.365144 0.330327 -0.013849 11.00000 -1.50000 AFIX 0 C2 1 0.308490 0.476242 0.075662 11.00000 0.01450 0.01992 = 0.02676 0.00306 0.00368 0.00016 C3 1 0.225077 0.100197 0.059640 11.00000 0.01755 0.01721 = 0.02453 0.00036 0.00361 0.00053 C4 1 0.167759 0.008632 0.116845 11.00000 0.01788 0.01579 = 0.02691 -0.00035 0.00450 -0.00030 C5 1 0.207623 0.066081 0.209473 11.00000 0.01596 0.01463 = 0.02521 0.00142 0.00502 0.00127 AFIX 13 H5 2 0.244999 -0.065872 0.229900 11.00000 -1.20000 AFIX 0 C6 1 0.258245 0.294188 0.199890 11.00000 0.01821 0.01540 = 0.02196 -0.00002 0.00646 0.00043 AFIX 13 H6 2 0.227367 0.439340 0.207633 11.00000 -1.20000 AFIX 0 C7 1 0.151713 0.088978 0.273121 11.00000 0.01562 0.01695 = 0.02217 -0.00047 0.00280 -0.00129 C8 1 0.100999 0.288206 0.271281 11.00000 0.01810 0.01751 = 0.02732 0.00178 0.00475 0.00040 AFIX 43 H8 2 0.102165 0.411599 0.231268 11.00000 -1.20000 AFIX 0 C9 1 0.048791 0.303004 0.328950 11.00000 0.01901 0.02068 = 0.03269 -0.00236 0.00636 0.00218 AFIX 43 H9 2 0.015025 0.435861 0.327203 11.00000 -1.20000 AFIX 0 C10 1 0.046877 0.120255 0.389112 11.00000 0.02021 0.02997 = 0.02628 -0.00289 0.00720 -0.00198 AFIX 43 H10 2 0.012099 0.131171 0.427831 11.00000 -1.20000 AFIX 0 C11 1 0.096779 -0.078421 0.391477 11.00000 0.02441 0.02523 = 0.02659 0.00405 0.00750 -0.00118 AFIX 43 H11 2 0.095529 -0.201159 0.431718 11.00000 -1.20000 AFIX 0 C12 1 0.148855 -0.093968 0.333428 11.00000 0.02032 0.01804 = 0.02618 0.00135 0.00437 0.00122 AFIX 43 H12 2 0.182082 -0.228032 0.334973 11.00000 -1.20000 AFIX 0 C13 1 0.337875 0.301344 0.262947 11.00000 0.01735 0.01656 = 0.02213 0.00176 0.00643 -0.00108 C14 1 0.395249 0.122100 0.261096 11.00000 0.02004 0.01756 = 0.02828 -0.00264 0.00716 -0.00041 AFIX 43 H14 2 0.383728 -0.006353 0.222398 11.00000 -1.20000 AFIX 0 C15 1 0.469382 0.134235 0.316611 11.00000 0.01831 0.02131 = 0.03071 0.00101 0.00719 0.00344 AFIX 43 H15 2 0.507318 0.014424 0.314694 11.00000 -1.20000 AFIX 0 C16 1 0.487093 0.324107 0.374868 11.00000 0.01823 0.02599 = 0.02325 0.00108 0.00273 -0.00073 AFIX 43 H16 2 0.536881 0.332310 0.411799 11.00000 -1.20000 AFIX 0 C17 1 0.430196 0.501960 0.377848 11.00000 0.02459 0.02195 = 0.02411 -0.00410 0.00502 -0.00057 AFIX 43 H17 2 0.441705 0.629163 0.417091 11.00000 -1.20000 AFIX 0 C18 1 0.355957 0.490001 0.322151 11.00000 0.02061 0.01845 = 0.02576 -0.00111 0.00621 0.00302 AFIX 43 H18 2 0.318010 0.609459 0.324535 11.00000 -1.20000 AFIX 0 HKLF 4 REM at111120_1_1_a.res in P2(1)/c REM wR2 = 0.0980, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0365 for 2767 Fo > 4sig(Fo) and 0.0403 for all 3091 data REM 209 parameters refined using 0 restraints END WGHT 0.0458 0.7235 REM Highest difference peak 0.248, deepest hole -0.230, 1-sigma level 0.045 Q1 1 0.3011 0.2902 0.2340 11.00000 0.05 0.25 Q2 1 0.2024 0.0533 0.0917 11.00000 0.05 0.24 Q3 1 0.3545 0.4075 0.2765 11.00000 0.05 0.24 Q4 1 0.1790 0.0794 0.2428 11.00000 0.05 0.23 Q5 1 0.3698 0.2271 0.2599 11.00000 0.05 0.23 ; _shelx_res_checksum 28839 _shelx_hkl_file ; 1 0 0 466.00 19.71 1 0 0 506.89 19.51 2 0 0 4136.51 163.13 2 0 0 4155.25 162.68 2 0 0 4137.39 163.18 3 0 0 628.06 24.63 3 0 0 603.04 25.31 3 0 0 591.97 25.31 4 0 0 1181.17 46.23 4 0 0 1132.50 47.17 4 0 0 1165.03 46.05 4 0 0 1130.52 47.20 5 0 0 2499.32 102.59 5 0 0 2664.89 103.96 5 0 0 2654.11 102.42 6 0 0 276.32 11.87 6 0 0 284.47 13.63 7 0 0 382.93 19.30 7 0 0 420.01 17.27 -8 0 0 2.74 0.46 8 0 0 3.55 2.44 8 0 0 1.36 1.56 9 0 0 441.84 18.91 10 0 0 302.00 13.73 11 0 0 456.03 20.07 11 0 0 456.77 20.00 11 0 0 477.21 20.07 11 0 0 436.48 19.80 12 0 0 557.55 24.57 12 0 0 567.15 24.06 12 0 0 556.75 24.57 12 0 0 563.35 24.63 12 0 0 591.31 24.56 13 0 0 98.84 5.88 13 0 0 103.36 6.56 13 0 0 98.35 6.46 13 0 0 105.59 6.60 13 0 0 107.18 5.94 13 0 0 107.40 6.50 14 0 0 91.32 6.31 14 0 0 99.55 6.39 14 0 0 93.79 5.67 14 0 0 101.77 6.50 14 0 0 94.99 5.68 14 0 0 96.85 6.44 15 0 0 96.08 6.40 15 0 0 99.34 5.78 15 0 0 103.89 6.68 15 0 0 93.96 5.66 15 0 0 92.60 6.47 16 0 0 1082.52 43.58 16 0 0 1045.86 44.61 16 0 0 1096.86 43.56 16 0 0 1000.63 44.38 17 0 0 493.18 20.14 17 0 0 499.89 21.47 17 0 0 434.95 20.03 17 0 0 477.05 20.76 18 0 0 168.39 9.10 18 0 0 166.59 8.49 19 0 0 798.15 33.42 19 0 0 802.23 32.94 20 0 0 160.34 7.62 20 0 0 196.24 8.11 21 0 0 138.40 6.05 0 -1 0 -0.15 1.44 0 1 0 0.68 0.84 1 -1 0 4016.06 159.38 1 -1 0 4094.27 159.86 -1 -1 0 4103.47 159.99 1 1 0 4024.46 159.72 2 1 0 17.13 1.97 -2 -1 0 19.97 2.30 -3 -1 0 48.78 3.61 3 -1 0 52.98 3.31 3 1 0 49.26 2.52 3 1 0 57.56 3.39 3 1 0 52.76 4.04 4 1 0 1013.44 41.34 4 1 0 1029.16 42.21 -4 -1 0 1109.51 42.58 4 -1 0 961.03 41.95 4 1 0 1059.24 41.41 4 -1 0 1082.35 41.43 5 -1 0 5518.31 216.41 5 1 0 5474.09 216.40 5 1 0 5624.34 218.90 6 1 0 331.57 13.40 -6 -1 0 330.78 14.78 6 -1 0 320.84 13.88 6 1 0 329.08 16.46 6 1 0 332.35 13.89 7 1 0 666.59 26.24 -7 -1 0 680.23 27.75 7 -1 0 649.31 26.84 7 1 0 671.27 29.94 7 1 0 622.80 26.80 8 1 0 652.64 25.40 -8 -1 0 586.58 25.15 8 1 0 577.68 24.53 8 -1 0 573.36 24.49 8 1 0 582.38 27.84 9 1 0 68.63 4.55 -9 -1 0 72.98 4.33 9 1 0 60.30 4.04 9 1 0 64.51 6.77 9 -1 0 57.82 4.00 10 1 0 226.10 15.25 10 1 0 256.65 11.92 10 -1 0 250.75 11.93 11 1 0 384.20 16.74 11 -1 0 370.45 16.72 11 -1 0 365.20 16.58 11 -1 0 384.29 16.88 11 1 0 365.08 16.51 11 1 0 378.92 16.81 11 -1 0 358.65 16.67 12 -1 0 193.24 9.56 12 -1 0 189.42 9.59 12 1 0 192.88 9.61 12 1 0 175.71 9.55 12 1 0 176.85 8.55 12 -1 0 190.45 9.75 12 -1 0 180.24 8.96 12 1 0 187.00 9.37 12 -1 0 177.15 9.53 13 1 0 169.78 8.90 13 1 0 146.90 8.61 13 -1 0 162.14 8.87 13 -1 0 161.07 8.78 13 -1 0 171.48 9.09 13 1 0 164.59 9.08 13 1 0 164.27 7.77 13 -1 0 160.02 8.23 13 -1 0 159.17 8.89 14 -1 0 308.30 14.75 14 1 0 304.55 14.83 14 1 0 336.36 15.15 14 1 0 323.74 13.51 14 -1 0 317.89 15.02 14 -1 0 283.52 14.83 14 -1 0 285.31 13.92 15 -1 0 3.66 2.06 15 -1 0 4.34 2.41 15 -1 0 7.91 2.34 15 1 0 8.03 2.81 15 -1 0 6.74 1.92 16 -1 0 129.19 7.00 16 1 0 126.92 7.47 16 -1 0 113.10 7.22 16 -1 0 104.79 6.07 16 -1 0 111.68 6.70 16 1 0 106.61 6.24 17 -1 0 222.45 10.24 17 1 0 199.36 10.67 17 -1 0 192.73 10.13 17 1 0 202.07 9.64 17 -1 0 201.26 9.89 18 -1 0 83.50 4.79 18 1 0 67.24 5.30 18 1 0 76.70 4.70 18 -1 0 80.46 4.97 19 1 0 0.64 1.91 19 -1 0 0.34 1.49 20 1 0 1.22 1.47 20 -1 0 -0.12 1.08 0 -2 0 200.79 10.36 0 2 0 195.64 9.28 -1 -2 0 277.66 13.36 -1 2 0 267.45 11.55 -2 -2 0 462.57 19.67 2 -2 0 411.70 18.06 2 2 0 406.77 17.18 2 2 0 454.52 19.13 2 -2 0 431.72 17.33 -3 -2 0 12.22 2.54 3 -2 0 6.42 2.22 3 -2 0 10.83 1.08 3 2 0 10.91 2.24 3 2 0 9.79 1.21 3 2 0 10.93 2.78 4 2 0 19.24 1.72 -4 -2 0 28.86 3.44 4 2 0 22.72 2.93 4 -2 0 21.71 2.93 4 -2 0 21.34 1.52 4 2 0 24.80 1.58 4 2 0 23.37 3.61 5 2 0 1668.60 66.04 5 -2 0 1521.30 65.73 5 2 0 1659.93 64.16 -5 -2 0 1666.55 66.68 5 -2 0 1573.06 63.99 5 2 0 1680.06 67.54 5 2 0 1614.91 64.01 6 2 0 15.72 2.70 6 2 0 18.41 1.63 6 -2 0 18.56 1.74 6 2 0 15.17 3.69 6 2 0 17.49 1.67 -7 -2 0 210.27 11.22 7 -2 0 207.09 9.10 7 2 0 205.25 12.67 7 2 0 194.10 9.02 -8 -2 0 403.19 20.28 8 2 0 451.14 17.97 8 -2 0 430.51 18.40 8 2 0 429.25 18.41 8 2 0 439.14 22.70 9 2 0 643.87 26.60 9 2 0 592.24 24.07 -9 -2 0 531.47 26.33 9 -2 0 581.45 24.69 9 2 0 615.88 29.80 9 2 0 595.38 24.74 10 -2 0 196.68 9.29 10 -2 0 176.21 8.95 10 -2 0 173.58 8.67 10 2 0 171.34 8.72 10 2 0 185.31 13.26 10 2 0 169.37 9.84 10 2 0 170.28 8.82 10 2 0 198.65 9.39 10 2 0 185.39 9.03 10 -2 0 168.38 8.69 10 -2 0 172.19 8.79 11 -2 0 108.26 6.08 11 -2 0 91.08 5.56 11 -2 0 82.64 5.47 11 2 0 94.85 5.55 11 2 0 89.36 6.38 11 2 0 92.02 5.70 11 2 0 84.41 5.52 11 2 0 88.53 5.39 11 -2 0 88.78 5.41 11 -2 0 98.94 5.70 12 -2 0 27.65 3.29 12 -2 0 23.71 2.81 12 2 0 17.08 2.62 12 2 0 26.87 3.02 12 2 0 25.27 2.28 12 2 0 24.29 3.06 12 -2 0 26.17 2.96 12 2 0 24.02 3.15 12 2 0 25.48 2.87 12 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640.48 27.42 1 3 0 643.04 27.12 2 3 0 311.51 12.99 2 -3 0 313.15 16.27 2 3 0 317.16 16.07 2 -3 0 331.22 13.19 2 -3 0 277.91 12.93 2 3 0 329.46 15.44 3 3 0 3.20 1.21 3 -3 0 2.58 2.57 3 -3 0 2.78 1.01 3 3 0 2.83 2.47 -3 -3 0 2.23 2.54 3 3 0 2.29 2.05 4 3 0 1048.56 43.40 -4 -3 0 1014.64 44.07 4 -3 0 990.87 39.93 4 3 0 966.27 43.59 5 -3 0 71.23 6.12 -5 -3 0 69.67 6.47 5 3 0 77.79 6.26 5 3 0 65.81 6.41 6 3 0 303.86 12.64 6 -3 0 278.65 15.20 6 3 0 254.62 14.89 7 3 0 154.48 7.38 7 3 0 153.07 8.06 7 3 0 168.81 8.37 7 -3 0 152.78 7.85 8 -3 0 10.08 2.19 8 3 0 6.83 3.41 8 -3 0 8.00 1.93 8 3 0 3.63 1.85 8 -3 0 9.39 1.90 8 -3 0 7.20 1.66 9 3 0 1.88 3.02 9 -3 0 1.34 1.83 9 3 0 3.07 1.27 9 3 0 3.22 2.09 9 3 0 7.26 2.03 9 3 0 4.21 2.01 9 -3 0 2.99 1.78 9 -3 0 3.49 1.48 9 -3 0 3.27 1.95 10 -3 0 129.09 7.10 10 -3 0 128.66 7.27 10 3 0 115.96 6.02 10 3 0 118.27 8.44 -10 -3 0 133.62 9.38 10 3 0 124.54 7.42 10 3 0 127.23 7.17 10 3 0 117.84 7.09 10 -3 0 118.99 6.65 10 -3 0 119.04 6.87 10 -3 0 129.75 6.73 11 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656.27 27.50 3 5 0 642.21 32.13 -3 -5 0 587.96 33.17 3 -5 0 650.89 33.03 -3 -5 0 657.58 31.75 3 5 0 628.52 27.68 3 5 0 675.37 27.35 -3 -5 0 613.54 27.53 3 -5 0 645.49 27.85 -3 -5 0 671.54 27.15 -4 -5 0 62.13 4.23 4 -5 0 57.10 3.72 4 -5 0 53.22 3.41 4 5 0 44.00 6.08 4 -5 0 59.39 6.96 -4 -5 0 59.10 6.70 4 5 0 47.23 3.76 -4 5 0 58.68 6.65 -4 -5 0 53.05 7.19 4 5 0 55.15 3.89 4 5 0 46.87 4.05 4 -5 0 57.88 4.46 -5 -5 0 10.93 2.25 5 -5 0 13.22 1.80 5 5 0 10.20 2.02 -5 5 0 10.69 3.43 -5 -5 0 13.27 3.97 -5 -5 0 10.00 3.54 -5 -5 0 12.42 2.30 5 5 0 10.53 2.07 5 5 0 8.75 2.14 5 -5 0 9.96 2.52 -6 -5 0 41.06 3.37 6 5 0 31.04 2.95 6 5 0 37.50 3.32 6 5 0 36.62 3.46 -6 -5 0 38.14 3.55 -7 -5 0 58.78 4.03 7 5 0 57.84 3.73 7 5 0 53.77 4.18 7 5 0 52.71 4.03 -7 -5 0 56.66 4.26 7 -5 0 52.39 4.28 8 5 0 48.36 3.32 8 5 0 52.16 3.83 -8 -5 0 50.13 4.02 8 5 0 40.00 3.66 8 5 0 49.46 4.20 8 -5 0 49.84 3.98 8 -5 0 47.68 3.92 -9 -5 0 64.32 4.02 9 5 0 71.79 3.96 9 5 0 67.29 4.83 9 5 0 66.26 4.44 -9 -5 0 66.58 4.60 9 -5 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337.85 15.30 5 -2 10 331.08 15.29 -5 -2 -10 316.10 20.41 5 -2 10 336.02 19.36 -5 -2 -10 325.24 15.38 5 2 10 366.74 21.15 5 2 10 311.66 14.70 5 2 10 332.82 14.90 5 2 10 340.38 14.88 5 -2 10 336.80 15.41 5 -2 10 340.34 14.61 5 -2 10 311.95 15.09 6 2 10 8.92 2.09 6 -2 10 8.80 2.36 -6 -2 -10 14.05 4.40 6 -2 10 6.63 3.16 6 2 10 3.16 3.82 6 2 10 6.90 1.87 6 2 10 7.19 1.84 6 2 10 10.73 2.25 6 -2 10 8.20 2.50 6 -2 10 8.30 1.88 6 -2 10 12.61 2.40 -7 -2 -10 212.39 15.05 7 2 10 184.29 9.31 7 -2 10 184.12 9.32 7 2 10 158.27 13.66 7 2 10 170.64 8.56 7 2 10 182.96 8.91 7 2 10 170.70 8.79 7 -2 10 178.67 9.42 7 -2 10 169.69 8.58 7 -2 10 171.14 9.08 7 -2 10 164.10 9.03 -8 -2 -10 6.52 4.42 8 2 10 4.42 1.95 8 -2 10 7.88 2.08 8 2 10 4.37 3.39 8 2 10 3.90 1.88 8 2 10 5.95 2.03 8 -2 10 3.73 2.31 8 -2 10 2.34 1.65 8 -2 10 3.25 1.68 8 -2 10 4.89 2.13 9 2 10 44.13 3.84 9 -2 10 51.35 4.05 9 2 10 55.33 3.86 9 -2 10 51.81 4.37 9 -2 10 45.97 3.52 9 -2 10 50.89 3.71 9 2 10 46.41 3.71 9 -2 10 42.53 3.84 10 2 10 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8.83 0.92 3 4 -16 9.80 1.33 2 4 -16 88.69 4.40 1 4 -16 5.60 1.06 0 -4 16 1.68 0.56 0 4 -16 0.87 0.77 14 0 -17 -0.37 0.87 -14 0 17 -0.07 0.66 13 0 -17 -0.26 1.23 -13 0 17 0.10 0.88 13 0 -17 0.94 1.12 12 0 -17 -0.33 1.42 11 0 -17 0.39 0.92 11 0 -17 0.76 1.49 10 0 -17 1.72 1.25 10 0 -17 1.48 1.80 9 0 -17 0.32 1.35 9 0 -17 -0.92 1.83 8 0 -17 0.23 1.31 8 0 -17 0.24 2.01 7 0 -17 1.47 1.51 7 0 -17 -2.28 2.21 6 0 -17 -1.51 1.58 -6 0 17 1.46 1.01 6 0 -17 -1.04 2.14 5 0 -17 2.05 1.56 5 0 -17 -1.59 2.18 -5 0 17 -0.14 1.21 4 0 -17 -0.26 1.39 4 0 -17 0.27 2.24 3 0 -17 -0.26 2.16 2 0 -17 3.18 1.71 2 0 -17 0.26 2.06 1 0 -17 -1.62 1.62 -1 0 17 1.26 1.58 1 0 -17 3.33 2.39 0 0 17 -1.63 1.56 0 0 -17 -0.75 1.91 1 0 17 -1.24 1.59 2 0 17 0.51 1.39 2 0 17 0.98 1.02 3 0 17 -1.26 1.44 3 0 17 -0.56 1.13 4 0 17 -1.19 1.06 5 0 17 -0.39 0.94 6 0 17 0.99 0.85 6 0 17 -0.20 0.95 14 -1 -17 1.71 0.84 14 -1 -17 2.29 0.71 -14 -1 17 3.85 0.69 13 -1 -17 -0.24 1.07 13 1 -17 -0.18 0.90 -13 -1 17 0.27 0.81 12 -1 -17 68.87 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1.70 1 1 17 22.63 2.45 -1 1 -17 26.67 2.85 1 -1 17 29.21 2.80 -1 -1 -17 30.49 2.94 2 1 17 18.01 1.98 -2 1 -17 17.97 2.34 -2 -1 -17 20.81 2.50 2 -1 17 12.79 1.51 2 1 17 12.91 1.42 2 -1 17 21.63 2.33 3 1 17 2.43 1.46 3 -1 17 3.77 1.12 3 1 17 2.17 1.02 3 -1 17 3.67 1.51 4 1 17 1.02 1.24 4 -1 17 1.17 1.03 4 1 17 0.82 0.90 4 -1 17 1.54 1.32 5 1 17 12.17 1.53 5 -1 17 13.63 1.37 5 1 17 10.92 1.28 5 -1 17 13.40 1.56 -6 -1 -17 1.57 1.00 -6 1 -17 0.21 0.99 6 1 17 0.95 0.68 6 -1 17 1.63 0.87 -12 -2 17 12.54 1.14 11 -2 -17 99.53 4.86 -11 -2 17 102.18 4.73 10 -2 -17 42.22 2.72 10 2 -17 39.90 2.52 -10 -2 17 41.44 2.43 9 -2 -17 1.59 1.30 9 -2 -17 0.29 1.29 9 2 -17 0.38 1.13 9 2 -17 -0.58 1.08 8 -2 -17 16.87 2.00 8 2 -17 19.19 1.88 -8 -2 17 20.30 1.66 8 2 -17 19.20 1.89 7 -2 -17 -0.17 1.55 7 2 -17 -1.20 1.42 7 2 -17 0.88 1.36 7 -2 -17 -0.60 1.31 6 -2 -17 3.54 1.67 6 2 -17 2.82 1.44 6 2 -17 2.66 1.38 6 -2 -17 1.43 1.42 5 -2 -17 0.18 1.55 -5 -2 17 0.89 0.77 5 2 -17 0.16 1.34 5 2 -17 1.30 1.30 5 -2 -17 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0.97 0.65 3 -3 17 0.78 0.50 13 0 -18 -0.29 0.63 -13 0 18 0.95 0.52 12 0 -18 -0.52 0.95 -12 0 18 0.54 0.71 12 0 -18 -0.84 0.99 11 0 -18 24.16 2.13 10 0 -18 127.98 5.95 10 0 -18 148.56 6.74 9 0 -18 192.33 8.98 9 0 -18 226.45 9.70 8 0 -18 54.58 3.79 7 0 -18 36.79 3.10 6 0 -18 5.75 1.94 -5 0 18 0.88 0.87 5 0 -18 1.05 1.90 -4 0 18 0.23 1.03 4 0 -18 -1.27 1.68 -3 0 18 218.35 9.67 3 0 -18 211.61 10.33 2 0 -18 4.32 1.92 -2 0 18 5.48 1.50 1 0 -18 40.18 3.35 0 0 -18 343.63 15.20 -1 0 -18 762.90 31.48 -2 0 -18 5.53 1.61 -3 0 -18 2.02 1.39 3 0 18 -0.23 1.10 4 0 18 73.41 3.84 -4 0 -18 80.23 4.16 5 0 18 21.74 1.52 -5 0 -18 22.87 1.72 -12 -1 18 43.52 1.85 -12 1 18 36.58 1.76 11 -1 -18 6.32 0.86 -11 -1 18 8.55 1.04 11 1 -18 7.87 1.22 11 -1 -18 8.98 1.26 -10 -1 18 17.94 1.52 10 1 -18 14.87 1.72 10 -1 -18 13.58 1.66 9 -1 -18 22.69 2.00 -9 -1 18 25.60 1.89 9 1 -18 23.97 2.19 9 -1 -18 25.32 2.27 8 -1 -18 10.72 1.67 8 1 -18 9.85 1.19 8 1 -18 15.35 1.91 8 -1 -18 14.07 1.86 7 -1 -18 35.84 2.80 -7 -1 18 36.57 2.37 7 1 -18 32.81 2.88 7 -1 -18 38.92 3.00 6 1 -18 27.49 2.66 6 -1 -18 27.23 2.60 -5 -1 18 0.18 0.84 5 1 -18 -0.18 1.59 5 -1 -18 -0.18 1.45 -4 -1 18 18.69 1.74 4 1 -18 18.77 2.36 4 -1 -18 19.45 2.35 -3 -1 18 7.42 1.50 3 1 -18 3.50 1.73 3 -1 -18 2.20 1.51 -2 1 18 0.11 1.10 2 1 -18 -0.36 1.41 2 -1 -18 0.36 1.55 -1 -1 18 31.03 2.50 1 1 -18 27.42 2.66 1 -1 -18 27.09 2.65 0 1 18 272.50 12.09 0 -1 18 306.02 12.41 0 1 -18 265.70 12.44 0 -1 -18 283.50 12.52 1 1 18 11.99 1.59 -1 1 -18 14.61 1.91 -1 -1 -18 15.32 1.94 1 -1 18 16.21 1.87 2 1 18 -1.74 1.08 -2 1 -18 0.27 1.18 -2 -1 -18 0.67 1.22 2 -1 18 -0.25 1.16 3 1 18 16.92 1.64 3 -1 18 20.53 1.78 -3 1 -18 21.57 1.83 -3 -1 -18 18.73 1.79 -4 1 -18 0.77 0.87 -4 -1 -18 1.50 0.90 4 -1 18 1.01 0.82 9 -2 -18 23.53 1.77 8 -2 -18 60.57 3.36 7 -2 -18 1.66 1.19 7 2 -18 1.81 0.77 6 -2 -18 61.66 3.39 6 2 -18 49.59 2.87 5 -2 -18 12.53 1.66 5 2 -18 10.49 1.31 4 -2 -18 6.96 1.46 4 2 -18 5.85 1.11 3 -2 -18 4.61 1.27 -3 -2 18 6.77 0.87 3 2 -18 7.40 1.18 2 -2 -18 26.54 2.16 -2 2 18 30.99 1.85 -2 -2 18 31.10 1.90 2 2 -18 27.09 1.96 -1 -2 18 1.17 0.85 -1 2 18 1.01 0.80 -1 -2 18 0.79 1.07 1 2 -18 0.32 0.78 0 -2 -18 2.64 0.77 0 -2 18 0.11 1.04 1 -2 18 1.46 0.81 1 2 18 1.55 0.81 1 -2 18 2.12 1.01 2 -2 18 44.91 2.33 2 2 18 40.60 2.29 2 -2 18 38.21 2.39 3 2 18 21.83 1.37 3 -2 18 21.06 1.36 11 0 -19 -0.20 0.58 -10 0 19 0.24 0.55 10 0 -19 -0.17 0.77 -9 0 19 0.42 0.64 9 0 -19 0.96 0.98 8 0 -19 0.37 0.71 8 0 -19 -0.85 1.06 7 0 -19 -0.54 1.32 6 0 -19 -0.14 1.25 5 0 -19 0.59 1.33 4 0 -19 -1.03 1.31 -3 0 19 0.07 0.70 3 0 -19 -0.15 1.24 -2 0 19 -1.37 0.81 2 0 -19 -0.14 1.28 1 0 -19 -0.81 1.31 0 0 -19 0.12 1.20 0 0 19 1.13 0.84 -1 0 -19 0.22 0.93 1 0 19 0.24 0.79 -2 0 -19 1.16 0.85 2 0 19 -0.48 0.66 9 -1 -19 0.69 0.74 9 -1 -19 16.73 1.19 8 -1 -19 23.46 1.63 8 1 -19 18.70 1.62 8 -1 -19 22.63 1.70 7 -1 -19 32.96 2.22 7 1 -19 31.59 2.24 7 -1 -19 38.16 2.36 6 -1 -19 1.06 1.02 6 1 -19 1.80 1.10 6 -1 -19 1.13 1.13 5 -1 -19 5.10 1.20 5 1 -19 3.78 1.28 5 -1 -19 6.64 1.29 4 1 -19 1.43 1.05 4 -1 -19 2.28 1.09 -3 -1 19 17.10 1.33 3 1 -19 22.81 1.90 3 -1 -19 21.32 1.89 -2 -1 19 0.53 0.76 2 1 -19 2.47 1.07 2 -1 -19 0.11 1.02 -1 1 19 4.23 0.81 1 1 -19 2.80 1.04 1 -1 -19 4.52 1.12 0 -1 19 1.03 0.76 0 1 -19 -0.45 0.84 0 -1 -19 0.46 0.90 1 -1 19 5.13 0.88 1 1 19 5.89 0.81 -1 1 -19 3.94 0.86 -1 -1 -19 4.72 0.86 7 -2 -19 14.05 1.07 6 -2 -19 16.09 1.21 5 -2 -19 5.73 0.83 4 -2 -19 73.95 3.50 3 -2 -19 5.24 0.74 5 0 -20 -0.28 0.60 4 0 -20 5.26 0.84 3 0 -20 35.99 2.00 3 0 -20 41.26 2.16 TITL at111120_1_1 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 17.036499 5.528105 15.693389 90.0000 101.2919 90.0000 ZERR 4.00 0.000322 0.000090 0.000307 0.0000 0.0018 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O F UNIT 72.00 60.00 4.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65727 _olex2_date_sample_data_collection 2020-11-11 _olex2_date_sample_submission 2020-11-11 _olex2_submission_original_sample_id at111120_1_1 _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 1.432 _oxdiff_exptl_absorpt_empirical_full_min 0.776