data_hh-409 _audit_creation_date 2021-04-23 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C13 H12 F2 N2 O4' _chemical_formula_sum 'C13 H12 F2 N2 O4' _chemical_formula_weight 298.25 _chemical_melting_point ? _chemical_oxdiff_formula C13H12F2N2O4 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 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3647(2) _cell_length_b 6.29270(10) _cell_length_c 19.4215(2) _cell_angle_alpha 90 _cell_angle_beta 94.0540(10) _cell_angle_gamma 90 _cell_volume 2604.52(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 10624 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 75.7480 _cell_measurement_theta_min 4.1260 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0181 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 14008 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.315 _diffrn_reflns_theta_min 4.149 _diffrn_ambient_temperature 123(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _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 87.00 178.00 0.50 0.57 -- 108.75 45.00 120.00 182 2 \w 85.00 178.00 0.50 0.57 -- 108.75 61.00 -60.00 186 3 \w 82.00 178.00 0.50 0.57 -- 108.75 25.00-126.00 192 4 \w 85.00 178.00 0.50 0.57 -- 108.75 61.00-180.00 186 5 \w 16.00 122.00 0.50 0.14 -- 42.55 25.00-126.00 212 6 \w -175.00 -75.00 0.50 0.57 -- -102.00 -25.00 70.00 200 7 \w -122.00 -16.00 0.50 0.14 -- -42.55 -25.00 70.00 212 8 \w -72.00 -28.00 0.50 0.57 -- -102.00 61.00 60.00 88 9 \w -72.00 -28.00 0.50 0.57 -- -102.00 61.00 -60.00 88 10 \w -22.00 37.00 0.50 0.14 -- -42.55 25.00-126.00 118 11 \w -37.00 18.00 0.50 0.14 -- 42.55 -19.00 -90.00 110 12 \w 35.00 76.00 0.50 0.57 -- 108.75 -61.00-180.00 82 13 \w 35.00 76.00 0.50 0.57 -- 108.75 -61.00-150.00 82 14 \w 35.00 74.00 0.50 0.57 -- 108.75 -61.00 -60.00 78 15 \w -37.00 26.00 0.50 0.14 -- 42.55 -25.00 70.00 126 16 \w 35.00 76.00 0.50 0.57 -- 108.75 -61.00 150.00 82 17 \w 35.00 76.00 0.50 0.57 -- 108.75 -61.00 120.00 82 18 \w 35.00 138.00 0.50 0.57 -- 108.75 -77.00 60.00 206 19 \w 35.00 106.00 0.50 0.57 -- 108.75 -94.00 30.00 142 20 \w 42.00 83.00 0.50 0.57 -- 108.75-125.00 150.00 82 21 \w 35.00 112.00 0.50 0.57 -- 108.75-125.00 30.00 154 22 \w 35.00 106.00 0.50 0.57 -- 108.75 -94.00 0.00 142 23 \w 35.00 112.00 0.50 0.57 -- 108.75-125.00 -60.00 154 24 \w 35.00 112.00 0.50 0.57 -- 108.75-125.00-120.00 154 25 \w 18.00 96.00 0.50 0.14 -- 42.55-125.00 0.00 156 26 \w 35.00 106.00 0.50 0.57 -- 108.75 -94.00 120.00 142 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0091936000 _diffrn_orient_matrix_UB_12 -0.0721900000 _diffrn_orient_matrix_UB_13 0.0743991000 _diffrn_orient_matrix_UB_21 -0.0711221000 _diffrn_orient_matrix_UB_22 0.0381654000 _diffrn_orient_matrix_UB_23 -0.0121776000 _diffrn_orient_matrix_UB_31 -0.0088853000 _diffrn_orient_matrix_UB_32 -0.2308739000 _diffrn_orient_matrix_UB_33 -0.0253241000 _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' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2528 _reflns_number_total 2685 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _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 1.171.40.69a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _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 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.831 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 2685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0414 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+3.0153P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1193 _refine_ls_wR_factor_ref 0.1209 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C5(H5), C3(H3) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B) 2.c Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C13(H13A,H13B,H13C) ; _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 0.60702(5) 0.15327(16) 0.74605(5) 0.0322(3) Uani 1 1 d . . . . . F2 F 0.56270(5) -0.10831(16) 0.69079(5) 0.0343(3) Uani 1 1 d . . . . . O2 O 0.69320(5) 0.44723(18) 0.48417(6) 0.0249(3) Uani 1 1 d . . . . . O1 O 0.63851(5) 0.75397(18) 0.48368(6) 0.0279(3) Uani 1 1 d . . . . . O4 O 0.43823(5) 0.79402(18) 0.58997(6) 0.0272(3) Uani 1 1 d . . . . . O3 O 0.41430(5) 0.53621(19) 0.66404(6) 0.0279(3) Uani 1 1 d . . . . . N1 N 0.57360(6) 0.2075(2) 0.63316(6) 0.0219(3) Uani 1 1 d . . . . . N2 N 0.73148(6) 0.4967(2) 0.68060(7) 0.0277(3) Uani 1 1 d . . . . . C10 C 0.65006(7) 0.5525(2) 0.50301(7) 0.0195(3) Uani 1 1 d . . . . . C7 C 0.55230(7) 0.5811(2) 0.56317(7) 0.0201(3) Uani 1 1 d . . . . . H7 H 0.545530 0.713599 0.542801 0.024 Uiso 1 1 calc R U . . . C8 C 0.50667(7) 0.4997(2) 0.60783(7) 0.0210(3) Uani 1 1 d . . . . . C6 C 0.60429(7) 0.4719(2) 0.54998(7) 0.0188(3) Uani 1 1 d . . . . . C12 C 0.45049(7) 0.6266(2) 0.61866(7) 0.0219(3) Uani 1 1 d . . . . . C5 C 0.61393(7) 0.2467(2) 0.57558(7) 0.0195(3) Uani 1 1 d . . . . . H5 H 0.602032 0.148073 0.537847 0.023 Uiso 1 1 calc R U . . . C3 C 0.67956(7) 0.1828(2) 0.60878(8) 0.0209(3) Uani 1 1 d . . . . . H3 H 0.706876 0.134385 0.573472 0.025 Uiso 1 1 calc R U . . . C4 C 0.70878(7) 0.3601(2) 0.64888(8) 0.0213(3) Uani 1 1 d . . . . . C1 C 0.60064(7) 0.0609(2) 0.68207(8) 0.0222(3) Uani 1 1 d . . . . . C9 C 0.52056(7) 0.3191(2) 0.64365(8) 0.0217(3) Uani 1 1 d . . . . . H9 H 0.493551 0.270786 0.675756 0.026 Uiso 1 1 calc R U . . . C2 C 0.66341(7) -0.0019(2) 0.65628(8) 0.0238(3) Uani 1 1 d . . . . . H2A H 0.660085 -0.134638 0.630911 0.029 Uiso 1 1 calc R U . . . H2B H 0.695000 -0.016960 0.694360 0.029 Uiso 1 1 calc R U . . . C11 C 0.67649(8) 0.8401(3) 0.43139(9) 0.0278(3) Uani 1 1 d . . . . . H11A H 0.664344 0.775840 0.387631 0.042 Uiso 1 1 calc R U . . . H11B H 0.719930 0.810435 0.443622 0.042 Uiso 1 1 calc R U . . . H11C H 0.670339 0.990981 0.428261 0.042 Uiso 1 1 calc R U . . . C13 C 0.35843(7) 0.6529(3) 0.67843(8) 0.0285(4) Uani 1 1 d . . . . . H13A H 0.329080 0.649076 0.638673 0.043 Uiso 1 1 calc R U . . . H13B H 0.369334 0.797681 0.689196 0.043 Uiso 1 1 calc R U . . . H13C H 0.339776 0.589299 0.716981 0.043 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 0.0392(6) 0.0320(5) 0.0253(5) -0.0015(4) 0.0012(4) 0.0036(4) F2 0.0341(5) 0.0267(5) 0.0417(6) 0.0072(4) 0.0005(4) -0.0056(4) O2 0.0218(5) 0.0269(6) 0.0268(5) 0.0014(4) 0.0066(4) 0.0041(4) O1 0.0294(6) 0.0226(6) 0.0331(6) 0.0070(5) 0.0132(5) 0.0039(5) O4 0.0242(5) 0.0279(6) 0.0300(6) 0.0040(5) 0.0045(4) 0.0067(4) O3 0.0214(5) 0.0316(6) 0.0318(6) 0.0050(5) 0.0101(4) 0.0055(5) N1 0.0200(6) 0.0228(6) 0.0232(6) 0.0054(5) 0.0036(5) 0.0031(5) N2 0.0250(7) 0.0288(7) 0.0295(7) 0.0007(6) 0.0025(5) -0.0012(5) C10 0.0192(7) 0.0209(7) 0.0185(6) -0.0005(5) 0.0007(5) 0.0003(5) C7 0.0197(7) 0.0200(7) 0.0203(7) 0.0005(5) -0.0001(5) 0.0013(5) C8 0.0181(7) 0.0229(7) 0.0220(7) -0.0006(5) 0.0020(5) 0.0013(6) C6 0.0184(7) 0.0198(7) 0.0182(6) 0.0007(5) 0.0011(5) 0.0007(5) C12 0.0187(7) 0.0259(7) 0.0210(7) -0.0013(6) 0.0012(5) 0.0014(6) C5 0.0191(7) 0.0194(7) 0.0200(7) 0.0000(5) 0.0022(5) 0.0017(5) C3 0.0212(7) 0.0197(7) 0.0219(7) 0.0001(5) 0.0026(5) 0.0047(5) C4 0.0169(7) 0.0232(7) 0.0242(7) 0.0035(6) 0.0033(5) 0.0038(5) C1 0.0262(7) 0.0180(7) 0.0223(7) 0.0022(5) 0.0019(5) -0.0009(6) C9 0.0190(7) 0.0242(7) 0.0221(7) 0.0013(6) 0.0029(5) -0.0004(6) C2 0.0258(8) 0.0183(7) 0.0269(7) 0.0018(6) -0.0003(6) 0.0041(6) C11 0.0285(8) 0.0263(8) 0.0298(8) 0.0067(6) 0.0092(6) -0.0017(6) C13 0.0218(7) 0.0362(9) 0.0283(8) -0.0028(7) 0.0080(6) 0.0051(6) _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 C1 1.3698(18) . ? F2 C1 1.3562(18) . ? O2 C10 1.2122(18) . ? O1 C10 1.3403(19) . ? O1 C11 1.4490(18) . ? O4 C12 1.212(2) . ? O3 C12 1.3397(19) . ? O3 C13 1.4451(18) . ? N1 C5 1.4798(18) . ? N1 C1 1.4176(19) . ? N1 C9 1.3605(19) . ? N2 C4 1.145(2) . ? C10 C6 1.474(2) . ? C7 H7 0.9300 . ? C7 C8 1.444(2) . ? C7 C6 1.346(2) . ? C8 C12 1.469(2) . ? C8 C9 1.354(2) . ? C6 C5 1.511(2) . ? C5 H5 0.9800 . ? C5 C3 1.5541(19) . ? C3 H3 0.9800 . ? C3 C4 1.473(2) . ? C3 C2 1.538(2) . ? C1 C2 1.517(2) . ? C9 H9 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 C10 O1 C11 116.68(12) . . ? C12 O3 C13 115.75(13) . . ? C1 N1 C5 112.53(12) . . ? C9 N1 C5 124.26(12) . . ? C9 N1 C1 122.66(13) . . ? O2 C10 O1 124.13(13) . . ? O2 C10 C6 123.42(14) . . ? O1 C10 C6 112.44(12) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C6 C7 C8 122.32(14) . . ? C7 C8 C12 119.09(13) . . ? C9 C8 C7 118.26(13) . . ? C9 C8 C12 122.30(14) . . ? C10 C6 C5 116.44(12) . . ? C7 C6 C10 122.34(13) . . ? C7 C6 C5 120.74(13) . . ? O4 C12 O3 123.76(14) . . ? O4 C12 C8 123.99(14) . . ? O3 C12 C8 112.24(13) . . ? N1 C5 C6 109.37(11) . . ? N1 C5 H5 109.0 . . ? N1 C5 C3 101.54(11) . . ? C6 C5 H5 109.0 . . ? C6 C5 C3 118.48(12) . . ? C3 C5 H5 109.0 . . ? C5 C3 H3 110.8 . . ? C4 C3 C5 111.08(12) . . ? C4 C3 H3 110.8 . . ? C4 C3 C2 111.07(12) . . ? C2 C3 C5 102.12(12) . . ? C2 C3 H3 110.8 . . ? N2 C4 C3 179.36(16) . . ? F1 C1 N1 109.97(12) . . ? F1 C1 C2 112.12(12) . . ? F2 C1 F1 104.00(12) . . ? F2 C1 N1 112.07(12) . . ? F2 C1 C2 112.75(12) . . ? N1 C1 C2 106.04(12) . . ? N1 C9 H9 119.6 . . ? C8 C9 N1 120.70(13) . . ? C8 C9 H9 119.6 . . ? C3 C2 H2A 111.0 . . ? C3 C2 H2B 111.0 . . ? C1 C2 C3 104.02(12) . . ? C1 C2 H2A 111.0 . . ? C1 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 C1 C2 C3 -97.68(14) . . . . ? F2 C1 C2 C3 145.34(12) . . . . ? O2 C10 C6 C7 -171.21(14) . . . . ? O2 C10 C6 C5 0.9(2) . . . . ? O1 C10 C6 C7 8.8(2) . . . . ? O1 C10 C6 C5 -179.11(12) . . . . ? N1 C5 C3 C4 -83.86(14) . . . . ? N1 C5 C3 C2 34.63(14) . . . . ? N1 C1 C2 C3 22.35(15) . . . . ? C10 C6 C5 N1 167.51(12) . . . . ? C10 C6 C5 C3 51.92(18) . . . . ? C7 C8 C12 O4 3.2(2) . . . . ? C7 C8 C12 O3 -176.68(13) . . . . ? C7 C8 C9 N1 -5.7(2) . . . . ? C7 C6 C5 N1 -20.22(18) . . . . ? C7 C6 C5 C3 -135.81(14) . . . . ? C8 C7 C6 C10 178.40(13) . . . . ? C8 C7 C6 C5 6.6(2) . . . . ? C6 C7 C8 C12 -178.86(13) . . . . ? C6 C7 C8 C9 7.8(2) . . . . ? C6 C5 C3 C4 35.86(17) . . . . ? C6 C5 C3 C2 154.35(12) . . . . ? C12 C8 C9 N1 -178.80(14) . . . . ? C5 N1 C1 F1 121.85(13) . . . . ? C5 N1 C1 F2 -123.00(13) . . . . ? C5 N1 C1 C2 0.42(16) . . . . ? C5 N1 C9 C8 -11.2(2) . . . . ? C5 C3 C2 C1 -35.31(14) . . . . ? C4 C3 C2 C1 83.18(14) . . . . ? C1 N1 C5 C6 -148.54(12) . . . . ? C1 N1 C5 C3 -22.54(15) . . . . ? C1 N1 C9 C8 159.67(14) . . . . ? C9 N1 C5 C6 23.16(19) . . . . ? C9 N1 C5 C3 149.15(14) . . . . ? C9 N1 C1 F1 -50.00(19) . . . . ? C9 N1 C1 F2 65.16(19) . . . . ? C9 N1 C1 C2 -171.42(14) . . . . ? C9 C8 C12 O4 176.31(15) . . . . ? C9 C8 C12 O3 -3.6(2) . . . . ? C11 O1 C10 O2 6.8(2) . . . . ? C11 O1 C10 C6 -173.18(12) . . . . ? C13 O3 C12 O4 -0.8(2) . . . . ? C13 O3 C12 C8 179.10(12) . . . . ? _shelx_res_file ; TITL hh-409_a.res in C2/c hh-409.res created by SHELXL-2018/3 at 13:49:38 on 23-Apr-2021 REM Old TITL hh-409_a.res in C2/c REM SHELXT solution in C2/c: R1 0.096, Rweak 0.002, Alpha 0.015 REM 1.032 for 256 systematic absences, Orientation as input REM Formula found by SHELXT: C13 F2 N2 O4 CELL 1.54184 21.3647 6.2927 19.4215 90 94.054 90 ZERR 8 0.0002 0.0001 0.0002 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O UNIT 104 96 16 16 32 L.S. 4 PLAN 5 CONF BOND list 4 fmap 2 acta MORE -1 BOND $H REM REM REM WGHT 0.066800 3.015300 FVAR 0.27832 F1 3 0.607016 0.153273 0.746055 11.00000 0.03923 0.03196 = 0.02529 -0.00149 0.00120 0.00361 F2 3 0.562703 -0.108310 0.690786 11.00000 0.03408 0.02674 = 0.04167 0.00722 0.00050 -0.00562 O2 5 0.693195 0.447229 0.484169 11.00000 0.02176 0.02687 = 0.02680 0.00143 0.00661 0.00413 O1 5 0.638510 0.753968 0.483677 11.00000 0.02943 0.02259 = 0.03311 0.00699 0.01317 0.00392 O4 5 0.438230 0.794018 0.589970 11.00000 0.02421 0.02785 = 0.02997 0.00396 0.00447 0.00672 O3 5 0.414295 0.536215 0.664041 11.00000 0.02143 0.03165 = 0.03182 0.00501 0.01014 0.00550 N1 4 0.573596 0.207520 0.633157 11.00000 0.02003 0.02280 = 0.02319 0.00544 0.00359 0.00309 N2 4 0.731481 0.496680 0.680599 11.00000 0.02498 0.02879 = 0.02950 0.00066 0.00255 -0.00123 C10 1 0.650062 0.552471 0.503010 11.00000 0.01920 0.02091 = 0.01845 -0.00053 0.00072 0.00026 C7 1 0.552302 0.581064 0.563170 11.00000 0.01970 0.02000 = 0.02028 0.00050 -0.00009 0.00128 AFIX 43 H7 2 0.545530 0.713599 0.542801 11.00000 -1.20000 AFIX 0 C8 1 0.506666 0.499654 0.607835 11.00000 0.01810 0.02294 = 0.02205 -0.00060 0.00204 0.00129 C6 1 0.604291 0.471908 0.549979 11.00000 0.01843 0.01976 = 0.01821 0.00065 0.00113 0.00075 C12 1 0.450486 0.626631 0.618661 11.00000 0.01875 0.02590 = 0.02097 -0.00127 0.00123 0.00140 C5 1 0.613935 0.246667 0.575584 11.00000 0.01911 0.01943 = 0.02000 0.00003 0.00217 0.00169 AFIX 13 H5 2 0.602032 0.148073 0.537847 11.00000 -1.20000 AFIX 0 C3 1 0.679563 0.182848 0.608783 11.00000 0.02122 0.01968 = 0.02195 0.00010 0.00258 0.00466 AFIX 13 H3 2 0.706876 0.134385 0.573472 11.00000 -1.20000 AFIX 0 C4 1 0.708776 0.360076 0.648883 11.00000 0.01686 0.02319 = 0.02420 0.00347 0.00330 0.00376 C1 1 0.600641 0.060933 0.682073 11.00000 0.02625 0.01800 = 0.02233 0.00215 0.00189 -0.00092 C9 1 0.520557 0.319064 0.643648 11.00000 0.01902 0.02417 = 0.02206 0.00131 0.00289 -0.00043 AFIX 43 H9 2 0.493551 0.270786 0.675756 11.00000 -1.20000 AFIX 0 C2 1 0.663406 -0.001874 0.656284 11.00000 0.02582 0.01827 = 0.02694 0.00180 -0.00028 0.00408 AFIX 23 H2A 2 0.660085 -0.134638 0.630911 11.00000 -1.20000 H2B 2 0.695000 -0.016960 0.694360 11.00000 -1.20000 AFIX 0 C11 1 0.676485 0.840070 0.431386 11.00000 0.02845 0.02628 = 0.02980 0.00669 0.00922 -0.00167 AFIX 137 H11A 2 0.664344 0.775840 0.387631 11.00000 -1.50000 H11B 2 0.719930 0.810435 0.443622 11.00000 -1.50000 H11C 2 0.670339 0.990981 0.428261 11.00000 -1.50000 AFIX 0 C13 1 0.358433 0.652857 0.678430 11.00000 0.02180 0.03620 = 0.02827 -0.00277 0.00800 0.00511 AFIX 137 H13A 2 0.329080 0.649076 0.638673 11.00000 -1.50000 H13B 2 0.369334 0.797681 0.689196 11.00000 -1.50000 H13C 2 0.339776 0.589299 0.716981 11.00000 -1.50000 AFIX 0 HKLF 4 REM hh-409_a.res in C2/c REM wR2 = 0.1209, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0414 for 2528 Fo > 4sig(Fo) and 0.0431 for all 2685 data REM 192 parameters refined using 0 restraints END WGHT 0.0668 3.0148 REM Highest difference peak 0.831, deepest hole -0.339, 1-sigma level 0.055 Q1 1 0.5689 0.0071 0.7337 11.00000 0.05 0.83 Q2 1 0.6485 0.2208 0.5901 11.00000 0.05 0.27 Q3 1 0.6306 0.0284 0.6675 11.00000 0.05 0.26 Q4 1 0.6275 0.5117 0.5305 11.00000 0.05 0.26 Q5 1 0.4808 0.5455 0.6143 11.00000 0.05 0.25 ; _shelx_res_checksum 30221 _shelx_hkl_file ; 0 0 1 0.01 0.03 0 0 -1 1.61 0.14 0 0 2 291.62 7.90 0 0 -2 287.11 7.94 0 0 -3 0.24 0.26 0 0 3 0.28 0.18 0 0 4 1677.04 44.35 0 0 -4 1634.34 44.34 0 0 4 1669.40 44.25 0 0 5 0.08 0.33 0 0 5 0.48 0.29 0 0 -5 -0.08 0.38 0 0 6 1287.85 35.12 0 0 -6 1306.68 35.19 0 0 7 0.06 0.38 0 0 -7 0.06 0.42 0 0 8 4.08 0.69 0 0 -8 2.43 0.65 0 0 9 0.57 0.55 0 0 -9 0.50 0.55 0 0 10 0.37 0.47 0 0 -10 0.57 0.53 0 0 11 0.11 0.48 0 0 -11 0.11 0.58 0 0 12 859.69 24.81 0 0 -12 832.99 24.72 0 0 13 0.41 0.55 0 0 -14 55.74 2.32 0 0 14 52.69 3.33 0 0 -15 0.05 0.48 0 0 15 -0.17 0.57 0 0 -15 0.45 0.41 0 0 -15 0.52 0.42 0 0 -16 376.49 11.05 0 0 16 362.99 13.05 0 0 -16 363.65 10.74 0 0 -16 388.50 10.85 0 0 17 0.37 0.58 0 0 -17 0.18 0.56 0 0 -17 -0.10 0.41 0 0 -17 0.27 0.44 0 0 17 -0.18 0.64 0 0 -18 0.78 0.45 0 0 -18 0.96 0.48 0 0 -18 0.61 0.55 0 0 -19 -0.13 0.42 0 0 -19 0.28 0.38 0 0 -19 0.29 0.58 0 0 20 7.16 0.70 0 0 -20 6.10 0.82 0 0 -20 5.82 0.66 0 0 -20 5.37 0.71 0 0 -21 0.66 0.51 0 0 -21 0.16 0.38 0 0 21 0.04 0.37 0 0 -22 5.95 0.58 0 0 22 6.69 0.59 0 0 -22 6.05 0.69 0 0 -22 4.80 0.53 0 0 -23 0.18 0.25 0 0 23 0.02 0.25 0 0 -23 -0.06 0.35 0 0 24 21.50 0.84 0 -2 0 113.53 4.00 0 -2 1 571.70 16.06 0 -2 -1 598.18 16.05 0 -2 1 544.38 15.57 0 -2 2 165.68 4.97 0 2 2 155.35 4.28 0 -2 2 153.72 4.32 0 -2 2 158.33 4.33 0 2 2 152.69 4.30 0 -2 3 107.15 3.73 0 -2 3 106.56 3.93 0 2 3 105.30 3.17 0 -2 3 107.85 3.22 0 -2 4 154.43 5.12 0 -2 -4 163.85 5.21 0 -2 4 151.72 5.25 0 2 4 145.46 4.55 0 -2 4 154.94 4.62 0 -2 -5 492.02 13.86 0 -2 5 507.17 14.40 0 2 -5 488.70 13.88 0 -2 -5 525.75 14.43 0 -2 5 492.94 14.52 0 2 5 487.29 13.80 0 -2 5 497.02 13.87 0 -2 -6 1451.08 39.32 0 2 -6 1441.03 39.33 0 -2 -6 1548.09 39.81 0 2 6 1423.40 39.24 0 -2 6 1446.39 39.30 0 -2 7 122.90 4.22 0 2 7 111.90 4.09 0 2 -7 120.42 4.24 0 -2 -7 117.66 4.23 0 2 8 421.59 12.23 0 -2 8 415.82 12.25 0 -2 -8 406.97 12.29 0 2 -8 407.19 12.29 0 -2 9 157.30 5.57 0 2 9 154.42 5.51 0 -2 10 0.27 0.34 0 2 10 0.72 0.36 0 2 11 25.03 1.85 0 -2 11 23.96 1.80 0 2 12 7.99 1.13 0 -2 12 7.39 1.11 0 -2 -13 107.14 3.80 0 -2 -13 108.03 3.80 0 -2 -13 111.77 3.75 0 -2 13 109.54 4.94 0 2 13 109.21 4.93 0 -2 13 114.21 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1.31 1 -5 4 23.54 1.22 1 -5 4 22.57 1.31 -1 -5 -4 23.72 1.15 1 -5 4 23.06 1.25 -1 -5 -4 23.01 1.26 -1 -5 -4 22.04 1.26 -1 -5 -4 23.77 1.37 1 -5 4 17.35 2.12 1 -5 4 20.78 1.17 -1 -5 -4 20.91 1.14 1 -5 4 21.83 1.14 -1 -5 -5 23.05 1.35 1 -5 5 19.82 1.14 -1 -5 -5 20.96 1.08 -1 -5 -5 20.93 1.21 1 -5 5 20.41 1.20 -1 -5 -5 20.64 2.25 1 -5 5 17.14 2.12 -1 -5 -5 21.57 1.27 1 -5 5 21.59 1.19 -1 -5 -5 19.50 1.11 1 -5 5 20.91 1.13 -1 -5 -6 1.83 0.91 1 -5 6 1.14 0.91 -1 -5 -6 0.51 0.44 1 -5 6 0.83 0.40 -1 -5 -6 0.14 0.50 1 -5 6 0.95 0.32 -1 -5 -6 0.99 0.34 -1 -5 -6 0.80 0.43 1 -5 6 2.40 0.45 -1 -5 -6 1.38 0.41 -1 -5 -7 4.89 0.55 -1 -5 -7 4.54 0.66 -1 -5 -7 4.96 0.61 -1 -5 -7 4.99 0.61 -1 -5 -7 4.97 0.69 1 -5 7 4.56 0.56 -1 -5 -7 4.88 0.72 1 -5 7 4.54 1.14 -1 -5 -8 13.67 1.01 -1 -5 -8 14.04 0.86 -1 -5 -8 13.39 0.96 1 -5 8 13.05 0.94 -1 -5 -8 13.17 0.93 -1 -5 -8 14.90 1.05 1 -5 8 13.79 0.90 -1 -5 -8 13.71 1.08 -1 -5 -9 184.15 5.97 1 -5 9 187.66 5.72 -1 -5 -9 174.81 5.72 -1 -5 -9 183.65 5.70 -1 -5 -9 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13 79.81 4.15 -2 -2 13 92.43 3.06 2 -2 -13 87.05 3.14 2 -2 -13 89.67 3.29 2 -2 -13 90.34 3.35 2 -2 -12 11.92 1.43 2 2 -12 12.46 1.44 -2 2 12 9.58 1.23 -2 -2 12 10.83 1.31 2 2 -11 41.52 2.52 2 -2 -11 37.41 2.44 -2 2 11 37.12 2.34 -2 -2 11 42.61 2.48 -2 -2 10 24.36 1.72 2 2 -10 31.26 2.01 2 -2 -10 26.31 1.89 -2 -2 10 31.71 1.99 -2 2 10 28.93 1.89 -2 -2 9 0.38 0.41 2 2 -9 -0.33 0.50 2 -2 -9 -0.08 0.40 -2 2 9 1.01 0.41 -2 -2 9 0.48 0.47 -2 -2 8 -0.14 0.42 2 2 -8 0.92 0.41 2 -2 -8 0.65 0.43 -2 2 8 0.20 0.33 2 -2 -7 6.87 0.81 -2 -2 7 6.16 0.80 2 -2 -7 7.26 0.81 2 2 -7 7.07 0.79 -2 -2 7 8.65 0.82 -2 2 7 6.91 0.75 -2 -2 6 33.07 1.83 2 -2 -6 35.71 1.87 2 2 -6 33.33 1.66 2 -2 -6 36.87 1.74 -2 -2 6 31.42 1.62 -2 2 6 31.30 1.58 -2 -2 5 60.35 2.58 2 -2 -5 61.50 2.61 2 -2 -5 58.41 2.30 2 2 -5 62.11 2.33 -2 -2 5 59.25 2.29 -2 2 5 56.86 2.22 -2 -2 4 -0.11 0.37 2 -2 -4 0.11 0.36 2 -2 -4 0.59 0.30 2 -2 -4 0.61 0.10 2 2 -4 0.26 0.27 -2 2 4 1.24 0.30 -2 -2 4 0.49 0.26 2 -2 -3 352.26 10.21 2 -2 -3 386.72 10.43 2 2 -3 379.25 10.43 -2 -2 3 396.17 10.46 -2 2 3 378.73 10.40 2 -2 -3 405.36 11.15 -2 -2 3 386.20 11.10 2 2 -2 63.96 2.02 2 -2 -2 65.58 2.03 2 -2 -2 61.99 2.09 2 -2 -2 71.33 2.73 -2 -2 2 68.33 2.72 -2 2 2 64.77 2.03 -2 -2 2 64.28 2.06 -2 2 1 35.78 1.13 -2 -2 1 38.75 1.84 2 -2 -1 34.51 1.39 2 -2 -1 34.02 1.10 2 2 -1 34.73 1.10 -2 2 0 185.64 5.03 -2 -2 0 180.50 5.03 2 -2 0 188.46 5.55 -2 -2 -1 100.41 2.91 -2 2 -1 100.62 2.92 2 -2 1 107.60 3.45 2 -2 1 101.67 2.87 2 2 1 94.79 2.85 -2 -2 -1 105.54 3.72 2 -2 1 112.55 3.86 2 -2 2 14.10 1.00 2 2 2 14.22 0.68 2 -2 2 14.79 0.70 -2 -2 -2 16.28 1.19 2 -2 2 16.28 1.23 2 -2 3 185.44 5.88 2 2 3 180.65 5.38 2 -2 3 177.92 5.38 -2 -2 -3 193.14 6.05 2 -2 3 186.58 6.18 2 -2 4 46.48 2.21 2 -2 4 50.00 1.94 2 2 4 46.52 1.90 2 -2 5 453.88 13.08 2 -2 5 429.27 12.46 2 2 5 433.94 12.44 2 -2 5 446.62 12.57 2 2 5 447.37 12.56 2 -2 6 1246.49 34.27 2 2 6 1291.92 34.28 2 2 6 1263.92 34.39 2 -2 6 1245.34 34.40 2 -2 7 136.93 4.79 2 2 7 144.02 4.83 2 2 7 134.99 4.89 2 -2 7 143.28 4.95 2 -2 8 53.67 2.82 2 2 8 48.07 2.42 2 -2 8 57.31 2.57 2 -2 8 56.97 2.68 2 2 8 51.25 2.57 2 -2 9 599.38 17.54 2 -2 9 579.51 17.19 2 2 9 572.84 17.17 2 -2 9 593.92 17.05 2 2 9 577.86 17.03 2 2 10 37.67 2.36 2 -2 10 40.47 2.42 2 2 10 35.70 2.22 2 -2 10 41.88 2.36 2 2 11 81.77 3.98 2 -2 11 79.77 3.93 2 2 11 85.77 3.91 2 -2 11 87.00 3.92 2 2 12 232.38 8.37 2 -2 12 240.58 8.41 2 -2 12 238.97 6.90 -2 -2 -12 240.32 7.12 2 -2 12 230.07 8.49 2 2 12 219.60 8.41 -2 -2 -13 2.40 0.54 -2 -2 -13 2.20 0.56 2 2 13 3.19 0.75 2 -2 13 2.61 0.70 -2 -2 -13 2.44 0.55 -2 2 -13 2.41 0.54 2 -2 13 1.36 0.40 -2 -2 -13 2.71 0.57 2 2 13 2.16 0.77 2 -2 13 1.54 0.69 2 -2 14 22.15 2.13 2 2 14 20.99 2.11 -2 -2 -14 26.16 1.44 -2 -2 -14 22.79 1.40 -2 -2 -14 23.51 1.32 2 -2 14 21.35 2.02 2 2 14 20.04 2.02 2 -2 14 23.05 1.18 -2 -2 -14 25.00 1.43 -2 -2 -14 23.68 1.41 -2 2 -14 22.24 1.36 2 -2 14 24.90 1.24 2 2 15 29.63 2.65 2 -2 15 32.36 2.74 -2 -2 -15 41.21 1.95 -2 -2 -15 39.71 1.94 -2 -2 -15 40.35 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-0.06 0.30 22 0 8 2.85 0.43 22 0 8 3.02 0.43 22 0 9 0.31 0.27 -22 0 -10 192.22 5.51 22 0 10 200.77 5.35 22 0 11 0.10 0.19 -22 0 -11 0.05 0.19 -22 0 -11 0.07 0.27 22 0 11 0.13 0.22 22 0 12 0.81 0.19 -22 -2 13 41.36 1.40 22 -2 -12 22.74 0.97 -22 2 12 22.53 0.86 -22 -2 12 20.91 0.93 -22 -2 11 2.66 0.39 -22 -2 11 2.77 0.31 22 -2 -11 3.16 0.45 -22 2 11 2.81 0.31 -22 -2 11 2.55 0.30 22 2 -11 3.31 0.32 22 -2 -10 44.26 1.68 22 -2 -10 39.07 1.44 22 2 -10 40.83 1.46 -22 2 10 38.42 1.46 -22 -2 10 39.84 1.48 -22 -2 10 40.21 1.56 22 -2 -9 0.69 0.44 -22 2 9 0.65 0.27 -22 -2 9 0.61 0.28 22 -2 -9 0.44 0.27 22 2 -9 0.42 0.27 -22 -2 9 0.77 0.35 -22 2 8 16.11 0.88 -22 -2 8 17.41 0.90 22 -2 -8 19.33 0.91 22 2 -8 19.20 0.91 -22 -2 8 17.33 0.98 -22 2 7 44.11 1.73 -22 -2 7 45.86 1.76 22 -2 -7 46.27 1.71 22 2 -7 47.36 1.72 -22 -2 7 48.29 1.86 -22 2 6 8.19 0.64 -22 -2 6 8.58 0.66 22 -2 -6 8.13 0.61 22 2 -6 9.23 0.65 -22 -2 6 9.10 0.73 -22 2 5 16.65 0.92 -22 -2 5 14.12 0.89 22 -2 -5 16.37 0.87 22 2 -5 17.19 0.89 -22 -2 5 14.08 0.93 -22 2 4 61.53 2.30 -22 -2 4 63.80 2.33 22 -2 -4 65.70 2.26 22 2 -4 67.01 2.28 -22 -2 4 66.13 2.41 22 -2 -3 30.52 1.30 22 2 -3 31.94 1.32 -22 2 3 28.14 1.33 -22 -2 3 28.67 1.35 22 -2 -2 35.54 1.42 22 2 -2 34.21 1.40 -22 -2 2 34.07 1.48 -22 2 2 31.01 1.44 -22 -2 2 31.80 1.47 22 -2 -1 68.77 2.35 22 2 -1 71.93 2.37 -22 -2 1 66.69 2.42 -22 2 1 67.92 2.44 -22 -2 1 63.62 2.42 -22 -2 0 28.67 1.35 -22 -2 0 29.97 1.42 22 -2 0 30.80 1.32 22 2 0 34.22 1.36 -22 2 0 29.40 1.38 -22 -2 0 32.30 1.44 -22 -2 -1 82.42 2.81 -22 -2 -1 80.68 2.93 22 -2 1 88.67 2.80 22 2 1 87.43 2.79 -22 2 -1 82.54 2.87 -22 -2 -1 82.68 2.89 -22 -2 -2 155.35 4.69 -22 -2 -2 155.94 4.91 22 -2 2 160.55 4.67 22 2 2 158.88 4.67 -22 2 -2 152.35 4.77 -22 -2 -2 148.64 4.76 -22 -2 -3 66.46 2.38 -22 2 -3 71.54 2.51 -22 -2 -3 69.26 2.51 -22 -2 -3 71.71 2.67 22 -2 3 76.43 2.43 22 2 3 74.09 2.41 -22 -2 -4 45.18 1.96 22 -2 4 47.43 1.72 22 2 4 48.82 1.73 -22 -2 -5 45.54 1.94 22 -2 5 46.48 1.68 22 2 5 48.03 1.69 -22 -2 -6 15.45 0.99 22 -2 6 13.49 0.71 22 2 6 13.05 0.71 22 2 6 14.95 0.83 -22 -2 -7 0.25 0.41 -22 -2 -7 0.07 0.40 22 -2 7 0.39 0.23 22 2 7 0.22 0.20 22 2 7 0.33 0.30 -22 -2 -8 1.79 0.43 22 2 8 2.09 0.27 22 2 8 2.03 0.34 -22 -2 -9 22.90 1.06 22 2 9 21.86 0.93 -22 -2 -9 24.50 1.11 -22 -2 -10 1.77 0.32 22 2 10 1.55 0.24 22 -2 10 1.39 0.18 -22 -2 -10 1.62 0.34 -22 -2 -11 0.58 0.21 22 -4 -8 5.93 0.39 22 -4 -7 2.51 0.29 -22 -4 6 15.87 0.74 22 -4 -6 15.32 0.73 -22 -4 5 0.19 0.16 -22 -4 5 -0.04 0.22 22 -4 -5 0.13 0.22 22 -4 -4 5.17 0.41 -22 -4 4 5.34 0.44 22 -4 -3 0.90 0.25 -22 -4 3 0.74 0.28 22 -4 -2 1.61 0.26 -22 4 2 1.76 0.32 -22 -4 2 2.45 0.36 -22 4 1 0.81 0.28 -22 -4 1 0.55 0.28 -22 4 0 -0.06 0.23 -22 -4 0 0.30 0.25 -22 4 -1 0.32 0.24 -22 -4 -1 0.12 0.24 -22 4 -2 33.24 1.22 -22 -4 -2 33.96 1.25 -22 4 -3 41.55 1.45 -22 -4 -3 45.57 1.49 -22 -4 -4 9.43 0.50 -23 1 13 95.53 2.83 -23 -1 13 95.70 2.83 -23 1 12 13.50 0.66 -23 -1 12 13.46 0.66 23 1 -12 13.92 0.65 23 -1 -12 13.55 0.65 23 -1 -11 0.99 0.33 23 -1 -11 1.77 0.32 23 1 -11 2.08 0.33 -23 1 11 1.54 0.32 -23 -1 11 1.53 0.32 23 -1 -10 13.40 0.73 23 1 -10 13.11 0.73 -23 1 10 12.32 0.75 -23 -1 10 13.83 0.77 23 -1 -9 61.35 2.13 23 1 -9 64.58 2.16 -23 1 9 61.54 2.19 -23 -1 9 62.16 2.19 -23 -1 8 2.16 0.36 23 -1 -8 3.12 0.42 23 1 -8 3.10 0.42 -23 1 8 2.61 0.43 -23 -1 8 3.40 0.45 23 -1 -7 20.13 0.98 23 1 -7 18.00 0.94 -23 1 7 19.00 1.02 -23 -1 7 17.99 0.99 -23 -1 6 3.61 0.45 23 -1 -6 4.69 0.52 23 1 -6 4.35 0.50 -23 1 6 4.23 0.54 -23 -1 6 4.65 0.55 23 -1 -5 10.03 0.72 23 1 -5 10.32 0.71 -23 1 5 8.99 0.74 -23 -1 5 9.80 0.77 23 -1 -4 4.82 0.53 23 1 -4 4.65 0.53 -23 -1 4 4.52 0.58 -23 1 4 4.62 0.59 23 -1 -3 37.96 1.53 23 1 -3 33.08 1.47 -23 1 3 35.75 1.60 -23 -1 3 35.22 1.59 23 -1 -2 46.23 1.78 23 1 -2 44.49 1.76 -23 1 2 46.26 1.88 -23 -1 2 42.10 1.83 23 -1 -1 1.13 0.38 23 1 -1 2.21 0.43 -23 1 1 2.00 0.47 -23 -1 1 1.75 0.45 23 -1 0 1.08 0.38 23 1 0 1.23 0.37 -23 1 0 0.70 0.40 -23 -1 0 0.89 0.42 23 -1 1 24.11 1.15 23 1 1 24.10 1.15 -23 1 -1 22.45 1.23 -23 -1 -1 23.04 1.24 23 -1 2 165.56 4.93 23 1 2 168.03 4.94 -23 1 -2 159.97 5.06 -23 -1 -2 160.11 5.06 23 -1 3 0.66 0.29 23 -1 3 0.58 0.34 23 1 3 0.12 0.30 -23 1 -3 0.22 0.38 -23 -1 -3 0.26 0.37 23 1 4 109.38 3.36 23 -1 4 96.11 3.19 23 -1 4 105.71 3.29 23 1 4 109.18 3.31 -23 1 -4 100.80 3.42 -23 -1 -4 105.59 3.44 23 -1 5 0.03 0.27 23 1 5 0.21 0.28 23 1 5 0.12 0.30 23 -1 5 0.35 0.25 23 -1 6 10.11 0.62 23 -1 6 10.99 0.67 23 1 6 11.60 0.68 -23 -1 -6 12.16 0.87 23 -1 7 0.58 0.25 23 -1 7 0.33 0.25 23 1 7 0.04 0.23 -23 -1 -8 3.28 0.46 23 -1 8 3.13 0.34 23 1 8 3.41 0.38 -23 -1 -8 3.41 0.49 23 -1 8 4.09 0.37 23 1 8 3.33 0.35 -23 -1 -9 4.99 0.48 23 -1 9 5.39 0.39 23 1 9 6.20 0.44 -23 -1 -9 5.65 0.52 23 1 9 6.98 0.42 23 -1 9 5.82 0.39 -23 -1 -10 1.64 0.30 -23 1 -10 1.45 0.27 -23 -1 -10 1.53 0.26 23 -1 10 1.42 0.20 23 1 10 1.28 0.22 -23 -3 10 6.00 0.37 -23 -3 9 2.95 0.31 -23 -3 8 0.20 0.18 -23 -3 8 0.12 0.22 23 -3 -8 0.58 0.29 -23 -3 7 1.09 0.24 -23 -3 7 1.31 0.30 23 -3 -7 1.01 0.32 -23 -3 6 0.95 0.31 23 -3 -6 1.61 0.36 -23 -3 5 4.64 0.42 23 -3 -5 4.75 0.50 -23 -3 5 5.39 0.48 23 -3 -4 111.35 3.54 -23 -3 4 117.78 3.52 23 -3 -3 3.51 0.45 -23 -3 3 2.56 0.38 23 -3 -2 38.42 1.48 -23 -3 2 40.80 1.50 23 -3 -1 8.49 0.56 -23 -3 1 10.23 0.63 -23 -3 0 10.73 0.65 -23 -3 -1 5.71 0.46 -23 -3 -2 59.88 1.97 -23 -3 -3 0.31 0.22 -23 -3 -3 0.29 0.26 -23 -3 -4 5.39 0.44 -23 -3 -4 4.75 0.37 -23 -3 -4 7.22 0.52 23 3 4 6.40 0.45 23 3 5 1.19 0.24 -23 -3 -5 1.17 0.30 -23 -3 -5 1.12 0.27 23 3 6 1.23 0.22 -23 -3 -6 1.72 0.28 -23 -3 -6 1.70 0.28 -24 0 12 0.74 0.22 -24 0 11 -0.10 0.23 24 0 -11 -0.05 0.22 24 0 -11 0.13 0.22 -24 0 10 27.31 1.14 24 0 -10 27.66 1.11 -24 0 9 0.16 0.28 24 0 -9 -0.18 0.26 -24 0 8 0.06 0.30 24 0 -8 0.10 0.27 -24 0 7 0.15 0.31 24 0 -7 0.18 0.29 -24 0 6 0.06 0.33 24 0 -6 -0.06 0.31 -24 0 5 -0.14 0.33 24 0 -5 0.11 0.30 -24 0 4 48.95 1.96 24 0 -4 53.04 1.91 -24 0 3 0.43 0.38 24 0 -3 0.09 0.31 -24 0 2 55.10 2.15 24 0 -2 58.27 2.06 -24 0 1 0.22 0.39 24 0 -1 0.59 0.34 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-24 -2 3 0.14 0.26 24 -2 -2 9.13 0.65 24 -2 -2 9.02 0.54 24 2 -2 8.72 0.55 -24 -2 2 8.28 0.55 -24 2 2 9.22 0.59 -24 -2 2 8.74 0.59 24 -2 -1 0.33 0.30 24 -2 -1 0.04 0.22 24 2 -1 0.12 0.23 -24 -2 1 0.02 0.21 -24 2 1 0.05 0.24 -24 -2 1 0.31 0.26 -24 -2 0 3.36 0.40 -24 2 0 3.56 0.40 24 -2 0 3.62 0.35 24 2 0 3.62 0.37 24 -2 0 2.72 0.38 24 -2 1 0.50 0.23 24 2 1 0.56 0.23 -24 2 -1 0.87 0.26 -24 -2 -1 0.85 0.28 24 2 2 47.51 1.59 24 2 3 24.91 0.95 -24 -2 -3 24.47 1.07 -24 -2 -4 133.56 3.87 -24 -2 -4 118.92 3.76 24 2 5 0.51 0.25 -24 -2 -5 0.52 0.31 -24 -2 -5 0.23 0.29 24 2 6 17.44 0.75 -24 -2 -6 17.85 0.82 24 2 7 3.09 0.28 -24 -2 -7 3.59 0.35 -25 1 9 60.91 1.87 -25 -1 9 62.04 1.87 25 -1 -8 6.86 0.43 25 1 -8 7.08 0.44 -25 1 8 6.33 0.45 -25 -1 8 6.31 0.44 25 -1 -7 17.36 0.91 -25 1 7 20.02 0.87 -25 -1 7 18.49 0.85 25 -1 -7 18.99 0.81 25 1 -7 19.35 0.82 -25 1 6 1.04 0.28 -25 -1 6 0.70 0.27 25 -1 -6 0.65 0.24 25 1 -6 0.88 0.25 -25 1 5 9.60 0.62 -25 -1 5 8.40 0.59 25 -1 -5 9.32 0.56 25 1 -5 8.98 0.56 -25 1 4 19.02 0.94 -25 -1 4 19.22 0.95 25 -1 -4 19.49 0.89 25 1 -4 21.32 0.91 -25 1 3 6.75 0.56 -25 -1 3 7.15 0.57 25 -1 -3 7.07 0.51 25 1 -3 8.04 0.53 -25 1 2 3.87 0.45 -25 -1 2 2.90 0.40 25 1 -2 3.15 0.37 25 -1 -2 3.56 0.39 25 1 -1 11.99 0.66 -25 1 1 13.26 0.78 -25 -1 1 14.69 0.79 25 -1 -1 13.92 0.72 25 1 -1 14.22 0.73 25 1 0 19.91 0.89 -25 1 0 19.73 0.98 -25 -1 0 20.37 0.99 25 -1 0 22.47 0.94 25 1 0 21.71 0.93 25 1 1 7.86 0.52 -25 1 -1 8.85 0.61 -25 -1 -1 7.54 0.59 25 -1 1 8.14 0.53 25 1 1 8.36 0.54 -25 -1 -2 2.13 0.37 25 1 2 2.80 0.34 -25 1 -2 2.66 0.38 -25 -1 -2 3.02 0.39 25 -1 2 3.01 0.34 25 1 2 2.77 0.33 -25 -1 -3 6.56 0.52 25 1 3 6.79 0.47 25 -1 3 7.22 0.47 25 1 3 7.21 0.47 -25 -1 -4 10.68 0.67 25 1 4 12.01 0.60 25 -1 4 11.76 0.59 25 1 4 12.44 0.60 -25 -1 -5 1.25 0.33 25 1 5 1.11 0.22 -25 -1 -6 -0.15 0.22 25 1 6 -0.16 0.16 -25 -1 -6 -0.17 0.22 -26 0 7 0.25 0.18 -26 0 6 2.53 0.31 26 0 -5 -0.10 0.18 -26 0 5 0.16 0.21 26 0 -4 59.70 1.90 -26 0 4 58.04 1.97 26 0 -3 0.15 0.20 -26 0 3 -0.02 0.23 26 0 -2 0.09 0.20 -26 0 2 -0.02 0.23 26 0 -1 -0.02 0.19 -26 0 1 -0.02 0.24 26 0 0 14.33 0.67 -26 0 0 14.21 0.74 26 0 1 -0.03 0.17 -26 0 -1 0.11 0.22 26 0 2 13.91 0.61 -26 0 -2 10.42 0.58 -26 0 -3 -0.05 0.20 0 0 0 0.00 0.00 TITL HH-409 in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 21.364693 6.292655 19.421479 90.0000 94.0541 90.0000 ZERR 7.00 0.000207 0.000055 0.000189 0.0000 0.0009 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O F UNIT 91.00 84.00 14.00 28.00 14.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 31971 _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 1.298 _oxdiff_exptl_absorpt_empirical_full_min 0.784