#------------------------------------------------------------------------------ #$Date: 2024-07-20 04:58:36 +0300 (Sat, 20 Jul 2024) $ #$Revision: 293488 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023204.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023204 loop_ _publ_author_name 'Novikov, Egor M.' 'Guillen Campos, Jesus' 'Read de Alaniz, Javier' 'Fonari, Marina S.' 'Timofeeva, Tatiana V.' _publ_section_title ; Synthesis, molecular and crystal structures of 4-amino-3,5-difluorobenzonitrile, ethyl 4-amino-3,5-difluorobenzoate, and diethyl 4,4′-(diazene-1,2-diyl)bis(3,5-difluorobenzoate) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024006819 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C9 H9 F2 N O2' _chemical_formula_moiety 'C9 H9 F2 N O2' _chemical_formula_sum 'C9 H9 F2 N O2' _chemical_formula_weight 201.17 _chemical_name_systematic ; Ethyl 4-amino-3,5-difluorobenzoate ; _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.877(3) _cell_length_b 8.9995(18) _cell_length_c 13.635(3) _cell_measurement_reflns_used 3255 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 23.384 _cell_measurement_theta_min 2.645 _cell_volume 1825.5(7) _computing_cell_refinement ; SAINT-Plus V8.40b (Bruker, 2019) ; _computing_data_collection ; APEX2 Ver. 2019.11-0. (Bruker, 2019) ; _computing_data_reduction ; SAINT-Plus V8.40b (Bruker, 2019) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 100.15 _diffrn_detector 'charge-coupled device (CCD) area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1139 _diffrn_reflns_av_unetI/netI 0.0440 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 29363 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.253 _diffrn_reflns_theta_min 2.645 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_correction_T_min 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.198 _refine_diff_density_min -0.265 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1665 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.209 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0599 _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^)+3.0535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1176 _refine_ls_wR_factor_ref 0.1307 _reflns_number_gt 1265 _reflns_number_total 1665 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jq2034.cif _cod_data_source_block II _cod_original_cell_volume 1825.6(6) _cod_database_code 2023204 _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. ; _shelx_hkl_file ; 0 1 0 0.30 0.30 0 1 0 1.40 0.30 0 1 0 0.40 0.40 0 -1 0 0.30 0.20 0 -1 0 0.40 0.60 0 -1 0 0.60 0.40 0 -1 0 0.70 0.20 0 -2 0 1222.18 116.79 0 -2 0 1190.58 116.39 0 -2 0 1203.98 116.59 0 -2 0 1218.08 116.99 0 2 0 1193.58 116.59 0 2 0 1155.28 116.69 0 3 0 -1.00 0.80 0 -3 0 -0.20 0.80 0 -3 0 0.50 0.80 0 3 0 0.40 0.80 0 -3 0 -0.50 1.30 0 4 0 309.17 29.40 0 -4 0 326.17 30.40 0 4 0 272.17 30.00 0 4 0 289.37 29.90 0 -4 0 307.47 30.70 0 -4 0 297.67 29.80 0 -5 0 -1.20 1.80 0 5 0 -0.10 1.40 0 -5 0 -1.50 1.20 0 -5 0 -0.70 1.10 0 5 0 -0.60 0.60 0 5 0 0.10 1.20 0 6 0 396.36 39.00 0 6 0 385.16 39.20 0 -6 0 398.16 40.10 0 -6 0 387.16 39.50 0 -6 0 380.26 38.60 0 -7 0 3.30 1.90 0 7 0 0.40 2.00 0 -7 0 -0.30 2.00 0 -7 0 0.00 3.30 0 7 0 1.10 2.00 0 -8 0 0.00 3.30 0 8 0 -2.20 2.10 0 8 0 0.10 2.90 0 8 0 0.20 2.10 0 -8 0 2.00 2.50 0 9 0 2.40 3.20 0 -9 0 4.50 4.00 0 9 0 -2.10 2.40 0 -9 0 -2.20 2.20 0 9 0 -0.90 2.40 0 10 0 -1.60 2.70 0 -10 0 4.00 4.10 0 10 0 0.20 2.80 0 10 0 2.20 3.60 0 0 -1 0.30 0.20 0 0 -1 0.60 0.30 0 0 -1 -0.30 0.10 0 0 1 -0.10 0.30 0 0 1 0.10 0.20 0 0 -1 0.00 0.10 0 -1 1 0.10 0.60 0 1 -1 0.60 0.40 0 -1 1 -0.60 0.40 0 1 -1 0.10 0.30 0 1 -1 0.10 0.30 0 -1 -1 0.10 0.40 0 -1 -1 0.00 0.20 0 -1 -1 0.20 0.40 0 -1 -1 0.20 0.30 0 -1 1 0.40 0.30 0 -1 -1 0.30 0.40 0 -1 -1 0.00 0.40 0 -2 1 886.71 88.49 0 -2 1 921.21 88.99 0 -2 -1 881.41 88.39 0 -2 -1 885.11 88.79 0 2 -1 903.51 88.49 0 -2 1 936.01 88.69 0 2 -1 927.31 88.59 0 -2 -1 909.71 88.39 0 -2 -1 937.21 88.59 0 -2 -1 903.01 88.69 0 2 1 895.51 88.49 0 -3 -1 0.10 0.80 0 3 -1 0.70 0.80 0 3 1 0.10 0.80 0 -3 -1 -0.40 0.90 0 -3 -1 -1.10 1.00 0 -3 1 -0.60 0.90 0 -3 1 -0.40 0.80 0 -3 -1 0.10 0.90 0 3 -1 -0.50 0.80 0 -3 1 -0.40 1.20 0 4 1 2.70 1.00 0 4 1 1.00 1.40 0 -4 -1 3.20 2.10 0 4 1 5.00 1.60 0 -4 1 0.90 1.60 0 -4 1 1.40 2.10 0 -4 -1 4.50 1.80 0 -4 -1 2.90 1.30 0 -4 1 5.50 1.70 0 4 -1 4.10 1.60 0 4 -1 3.20 1.50 0 5 1 0.10 0.90 0 5 -1 -1.10 1.20 0 -5 -1 -0.80 1.10 0 5 -1 0.50 1.20 0 -5 -1 -1.60 1.80 0 -5 1 -0.60 1.20 0 -5 -1 -1.00 1.20 0 5 1 -0.50 1.40 0 -5 1 -2.10 2.10 0 -5 1 -0.50 1.30 0 5 1 -0.40 1.30 0 -6 1 6.20 2.10 0 6 -1 8.70 2.40 0 6 -1 3.50 2.50 0 -6 -1 6.20 2.00 0 -6 -1 4.60 3.00 0 -6 -1 5.40 2.40 0 6 -1 6.60 2.50 0 -6 1 8.90 3.60 0 -6 1 7.50 2.70 0 6 1 3.10 2.30 0 6 1 5.00 2.20 0 6 1 6.40 1.40 0 7 -1 -2.80 1.80 0 -7 1 1.90 2.60 0 7 -1 -1.60 1.70 0 -7 -1 0.60 1.70 0 -7 1 2.00 3.10 0 7 1 -0.90 1.20 0 -7 1 0.50 1.70 0 7 1 0.50 2.30 0 -7 -1 1.80 2.20 0 7 -1 2.60 3.00 0 7 1 1.00 2.00 0 -7 -1 2.20 3.10 0 -8 -1 27.10 6.80 0 8 -1 24.70 5.90 0 8 1 17.50 4.50 0 -8 1 31.10 7.40 0 8 -1 29.10 5.30 0 8 1 25.10 5.10 0 8 -1 25.00 4.90 0 -8 -1 29.60 6.10 0 9 -1 -1.10 2.20 0 9 -1 3.10 2.90 0 -9 -1 7.20 4.10 0 9 -1 -2.10 2.80 0 9 1 5.20 3.20 0 -9 -1 -3.00 2.10 0 9 1 -1.20 2.80 0 9 1 -1.40 2.80 0 -9 1 0.50 3.90 0 10 -1 -1.10 2.40 0 10 1 0.50 2.90 0 10 1 5.50 3.50 0 10 -1 3.10 3.30 0 -10 1 6.40 4.30 0 10 1 -3.90 2.70 0 -10 -1 -0.50 3.10 0 -10 -1 5.10 3.40 0 10 -1 -0.10 2.80 0 0 2 187.18 18.40 0 -1 2 1.40 1.10 0 1 -2 0.60 0.50 0 -1 -2 0.40 0.60 0 -1 -2 1.60 0.80 0 1 2 0.30 0.80 0 -1 -2 -0.20 0.60 0 1 -2 -0.10 0.50 0 -1 2 0.10 0.50 0 -1 -2 -0.70 0.40 0 -1 -2 -0.50 0.40 0 1 -2 0.20 0.50 0 -2 -2 2.90 1.20 0 -2 2 5.00 0.80 0 2 -2 3.20 1.00 0 2 -2 2.80 0.90 0 -2 -2 5.80 1.30 0 -2 2 -2.00 1.80 0 -2 -2 4.10 1.10 0 -2 -2 4.40 1.10 0 2 -2 4.70 1.20 0 -2 -2 2.40 1.00 0 -3 2 -0.60 1.10 0 3 -2 -1.00 0.70 0 3 -2 -0.70 1.00 0 -3 -2 0.50 0.80 0 -3 -2 0.10 0.90 0 -3 -2 -0.70 0.80 0 -3 2 0.80 1.60 0 -3 -2 0.50 0.90 0 -3 -2 -0.80 1.10 0 -3 -2 0.50 0.90 0 3 -2 -0.50 0.80 0 -4 2 104.19 10.80 0 4 -2 101.39 11.00 0 4 -2 110.29 10.80 0 -4 -2 104.89 11.10 0 4 2 99.29 10.90 0 4 -2 106.19 11.00 0 4 2 100.59 10.50 0 -4 2 91.19 11.50 0 -4 -2 104.69 10.60 0 -4 -2 108.49 11.00 0 -4 -2 96.09 11.30 0 5 -2 -2.20 1.70 0 -5 2 -0.20 1.40 0 -5 -2 -0.80 1.30 0 -5 -2 -1.30 1.20 0 5 -2 -1.30 1.30 0 5 2 0.40 1.40 0 -5 2 -3.20 1.70 0 5 2 -0.60 1.00 0 -5 -2 1.70 1.40 0 5 2 -1.30 1.50 0 5 -2 1.20 1.40 0 -5 -2 -1.40 1.50 0 -6 2 0.30 1.60 0 6 -2 0.00 2.10 0 6 2 -0.90 1.60 0 -6 2 0.30 2.40 0 -6 -2 -0.20 2.60 0 6 -2 0.70 1.50 0 6 2 -0.80 1.70 0 6 -2 -2.60 1.40 0 -6 -2 -2.40 1.20 0 6 2 -1.80 1.10 0 -6 -2 1.10 1.50 0 7 -2 -0.80 1.80 0 7 -2 0.20 2.60 0 -7 2 -0.40 3.00 0 -7 -2 4.30 3.80 0 7 2 -2.60 1.40 0 7 2 2.20 2.30 0 7 -2 1.40 1.90 0 -7 2 1.50 2.00 0 -7 -2 -0.40 2.00 0 7 2 -0.50 2.00 0 -7 -2 0.30 1.70 0 -8 -2 20.80 6.00 0 -8 -2 20.50 5.00 0 8 -2 15.50 3.90 0 8 2 13.20 3.90 0 -8 2 15.70 5.50 0 8 -2 10.60 4.20 0 8 -2 11.70 3.90 0 8 2 18.30 4.70 0 -9 -2 2.40 3.70 0 -9 -2 0.60 2.60 0 -9 2 0.20 3.50 0 9 2 -0.20 2.90 0 9 2 0.00 2.60 0 9 -2 -2.40 2.80 0 9 -2 -0.20 2.40 0 9 -2 0.60 2.40 0 10 -2 -0.20 2.50 0 -10 -2 1.60 3.10 0 -10 -2 7.00 4.40 0 10 2 4.60 3.40 0 10 -2 -0.70 2.80 0 10 2 -0.40 3.10 0 10 -2 -0.20 2.80 0 -10 2 4.20 4.00 0 10 2 4.20 3.20 0 0 -3 0.40 0.80 0 0 -3 0.30 0.50 0 0 3 0.00 1.20 0 0 3 0.80 0.90 0 0 -3 0.30 0.60 0 0 -3 -0.80 0.80 0 -1 -3 0.60 0.50 0 -1 -3 1.30 0.70 0 -1 -3 -1.40 0.70 0 1 -3 -0.20 0.20 0 -1 3 5.30 1.90 0 -1 3 2.20 1.60 0 1 -3 0.00 0.70 0 -1 3 0.40 0.80 0 1 3 0.40 1.10 0 1 -3 0.60 0.70 0 1 3 0.20 0.70 0 -1 -3 1.50 0.90 0 2 -3 198.18 19.40 0 2 3 187.88 19.40 0 -2 -3 176.28 19.50 0 -2 3 185.88 19.90 0 -2 -3 200.48 19.50 0 -2 3 202.18 19.30 0 -2 -3 203.18 19.50 0 2 -3 203.58 19.50 0 -2 -3 202.58 19.50 0 -2 -3 200.58 19.60 0 -2 3 198.98 19.60 0 2 -3 183.88 19.40 0 -3 3 0.90 0.70 0 -3 -3 -0.40 0.70 0 3 -3 0.70 0.90 0 -3 -3 0.80 0.50 0 -3 -3 -0.70 0.90 0 -3 3 1.40 0.70 0 -3 -3 -0.10 1.10 0 -3 -3 0.40 1.00 0 -3 -3 -1.20 0.70 0 3 3 -0.40 0.90 0 3 -3 2.00 1.10 0 3 -3 -0.60 0.90 0 -3 3 1.40 1.90 0 -4 -3 185.68 19.60 0 -4 -3 193.78 19.30 0 -4 3 190.78 20.10 0 -4 -3 193.08 19.10 0 -4 -3 190.58 19.10 0 4 -3 187.18 19.10 0 4 -3 197.18 19.30 0 -4 -3 181.38 19.40 0 4 3 190.58 19.00 0 4 -3 191.58 19.40 0 -4 3 176.08 19.10 0 -5 -3 -1.30 1.60 0 5 -3 -0.90 1.30 0 -5 3 -0.80 2.00 0 -5 -3 0.50 1.90 0 5 -3 -0.10 1.40 0 5 3 1.20 1.70 0 5 -3 -3.10 1.60 0 -5 -3 -1.10 1.60 0 -5 3 -0.20 1.60 0 -5 -3 -0.40 1.20 0 5 3 -1.10 1.00 0 6 3 0.80 2.00 0 -6 3 3.80 2.20 0 6 -3 2.30 2.20 0 6 -3 0.90 1.70 0 6 3 3.00 2.10 0 6 3 -0.30 1.40 0 -6 -3 0.60 1.80 0 6 -3 0.00 1.60 0 -6 -3 -0.90 2.30 0 -6 3 -0.30 2.40 0 -6 -3 0.70 2.00 0 -6 -3 0.30 1.50 0 -7 3 5.20 2.50 0 7 -3 2.30 2.40 0 7 3 4.50 2.70 0 7 3 1.20 2.70 0 7 -3 4.20 2.40 0 7 3 0.60 1.80 0 -7 3 5.40 4.00 0 7 -3 4.30 3.00 0 -7 -3 3.00 2.20 0 -7 -3 3.40 3.30 0 -7 -3 4.90 2.70 0 8 -3 2.70 2.60 0 -8 -3 0.30 3.30 0 8 -3 0.10 2.30 0 -8 -3 -1.40 2.30 0 8 3 -0.40 2.50 0 -8 3 1.80 3.70 0 8 3 4.00 3.00 0 8 -3 -2.00 2.10 0 9 -3 5.40 3.00 0 -9 3 4.40 4.20 0 9 -3 1.30 2.50 0 9 3 -0.60 2.80 0 9 -3 4.60 3.40 0 -9 -3 0.70 2.60 0 9 3 2.30 3.10 0 -9 -3 2.60 3.80 0 -10 -3 5.50 4.40 0 10 -3 -0.90 2.40 0 10 -3 3.10 3.40 0 -10 3 3.80 4.10 0 -10 -3 0.30 2.80 0 10 -3 2.20 3.00 0 10 3 3.60 3.80 0 10 3 5.30 3.50 0 0 4 9103.19 893.91 0 0 -4 9999.00 894.61 0 0 4 8588.94 894.11 0 0 -4 9575.14 894.31 0 0 -4 9054.89 894.01 0 0 4 8818.82 894.01 0 0 -4 9279.07 893.81 0 1 4 1.20 1.50 0 1 -4 1.70 1.10 0 -1 4 2.40 1.10 0 -1 -4 -1.10 1.00 0 -1 -4 1.30 1.20 0 1 4 0.80 1.00 0 -1 -4 -2.70 1.00 0 -1 4 0.40 1.70 0 -1 4 -1.40 1.60 0 -2 4 78.49 7.80 0 2 4 75.19 8.00 0 -2 4 62.69 8.20 0 -2 -4 78.09 7.90 0 2 -4 65.39 7.70 0 -2 -4 79.69 7.90 0 -2 4 75.39 8.10 0 2 4 62.69 7.90 0 -2 -4 79.29 8.00 0 2 -4 85.79 7.90 0 -2 -4 67.39 8.00 0 2 -4 79.99 7.90 0 -2 -4 79.49 7.90 0 3 -4 1.60 1.10 0 -3 -4 0.90 1.20 0 -3 -4 -0.20 1.00 0 -3 -4 1.00 1.20 0 -3 -4 0.40 1.10 0 -3 4 -1.50 1.80 0 -3 4 2.40 1.00 0 3 4 1.80 1.40 0 -3 -4 1.60 1.10 0 3 -4 -0.60 1.00 0 3 -4 -0.20 0.90 0 -3 4 2.20 1.80 0 3 4 -2.30 1.30 0 4 -4 110.09 11.60 0 -4 -4 118.19 11.80 0 4 -4 120.99 11.90 0 4 -4 115.19 11.80 0 -4 4 106.99 12.50 0 -4 -4 111.49 12.00 0 -4 4 106.19 11.00 0 -4 -4 110.69 11.70 0 -4 -4 102.89 11.60 0 4 4 108.09 11.60 0 5 -4 -4.30 1.70 0 -5 -4 -0.20 1.50 0 5 -4 -1.10 1.40 0 -5 4 0.80 2.20 0 -5 -4 -0.80 1.40 0 -5 -4 -0.50 1.50 0 -5 -4 0.70 1.50 0 5 -4 0.80 1.50 0 -5 4 0.20 1.80 0 5 4 -0.80 1.60 0 5 4 0.00 1.40 0 -5 -4 0.20 1.90 0 -6 4 13.10 3.20 0 -6 -4 9.60 3.30 0 -6 -4 12.10 2.90 0 -6 4 9.90 4.00 0 6 -4 10.10 3.20 0 6 4 5.70 2.60 0 6 -4 3.10 2.10 0 6 4 9.20 2.40 0 -6 -4 10.00 2.90 0 6 -4 8.70 2.70 0 -6 -4 10.90 2.90 0 -7 -4 3.30 2.70 0 7 4 2.70 2.20 0 -7 -4 5.10 2.40 0 -7 -4 6.40 2.70 0 7 4 6.60 3.00 0 7 -4 3.20 2.20 0 7 -4 1.30 2.10 0 -7 4 4.90 3.90 0 7 -4 8.40 3.30 0 -7 -4 5.20 3.40 0 -7 4 7.10 2.90 0 7 4 4.60 3.10 0 -8 -4 81.09 10.50 0 -8 4 79.09 11.50 0 8 -4 75.39 10.00 0 -8 -4 95.09 11.50 0 8 4 62.49 10.60 0 8 -4 83.29 10.30 0 8 -4 89.29 10.00 0 8 4 85.09 10.40 0 -9 -4 7.90 4.40 0 -9 -4 -0.50 2.40 0 9 -4 0.60 2.50 0 9 4 0.10 3.10 0 9 4 0.90 2.90 0 9 -4 -1.80 2.40 0 -9 4 3.80 3.90 0 9 -4 -1.00 3.10 0 10 -4 20.40 5.20 0 10 -4 17.30 5.00 0 10 4 10.40 4.30 0 -10 -4 17.90 5.50 0 -10 -4 25.20 6.30 0 -10 4 18.30 6.40 0 10 -4 19.10 5.00 0 10 4 10.30 4.30 0 0 5 2.00 1.40 0 0 -5 1.00 0.90 0 0 -5 1.60 1.10 0 0 5 2.30 1.90 0 0 5 2.00 1.40 0 0 -5 1.20 0.80 0 -1 -5 0.30 0.80 0 1 5 0.20 0.90 0 -1 5 0.30 1.10 0 -1 -5 0.00 1.10 0 1 5 3.60 1.90 0 -1 5 -0.40 1.60 0 -1 5 0.80 1.90 0 -1 -5 -1.10 0.80 0 1 -5 0.10 1.00 0 1 -5 -0.50 1.00 0 1 5 1.40 1.30 0 1 -5 -1.90 0.90 0 -1 -5 2.40 1.50 0 2 -5 525.85 50.19 0 -2 -5 521.05 50.09 0 -2 5 472.75 49.99 0 2 5 486.45 50.29 0 -2 5 491.45 50.49 0 -2 -5 548.65 50.19 0 2 5 525.85 49.99 0 2 5 489.55 50.29 0 2 -5 504.45 50.09 0 -2 5 512.65 50.39 0 -2 -5 523.75 50.39 0 -3 -5 -0.60 1.10 0 -3 -5 1.00 1.40 0 -3 5 -1.80 1.70 0 -3 5 -0.60 1.10 0 3 -5 0.20 1.20 0 -3 -5 -1.20 1.10 0 3 -5 1.30 1.20 0 3 5 -0.10 1.70 0 3 5 -0.10 1.40 0 3 -5 -0.40 0.90 0 -3 -5 0.40 1.00 0 -3 5 3.60 2.30 0 4 5 334.87 32.70 0 -4 -5 330.27 32.80 0 -4 -5 327.87 32.80 0 4 -5 320.77 32.60 0 -4 -5 322.17 32.70 0 -4 -5 328.97 33.00 0 -4 5 329.37 32.20 0 -4 5 289.07 32.70 0 4 -5 326.07 32.80 0 4 -5 344.97 32.80 0 4 5 337.37 32.70 0 -4 5 330.67 33.60 0 5 -5 0.90 1.60 0 5 5 -1.70 1.70 0 -5 -5 -0.30 1.50 0 -5 -5 -0.90 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6.10 5 2 -5 49.50 6.10 5 -2 -5 56.39 6.70 -5 2 -5 47.10 6.10 5 -2 -5 54.09 6.50 -5 2 -5 56.59 5.80 -5 2 -5 53.39 6.30 5 2 5 55.69 6.50 5 -2 -5 54.19 5.60 -5 -2 5 48.90 6.10 -5 -2 5 48.10 6.90 5 2 5 56.69 6.40 -5 -3 -5 3.10 1.50 -5 -3 -5 -0.90 1.60 5 -3 5 0.60 1.90 -5 3 5 3.00 2.90 5 3 -5 -1.20 1.30 -5 -3 -5 -0.80 1.70 5 -3 5 1.60 1.00 5 3 -5 0.30 1.00 5 -3 5 -0.80 2.50 -5 3 5 2.80 1.30 -5 -3 -5 0.00 1.40 5 3 -5 1.20 1.50 -5 -3 5 1.10 1.10 5 -3 -5 1.80 1.30 -5 3 -5 1.60 1.50 5 -3 -5 3.00 1.90 -5 -3 5 -0.50 1.90 -5 3 -5 1.40 1.80 5 3 5 3.90 2.10 5 -3 -5 0.90 1.30 -5 -3 5 0.70 2.80 -5 3 -5 1.10 1.50 5 3 5 3.00 2.00 5 -3 -5 2.30 2.20 -5 -4 -5 102.09 12.60 5 -4 5 135.39 13.70 -5 4 5 112.09 13.20 5 4 -5 105.39 12.60 -5 -4 -5 119.09 12.80 -5 -4 -5 103.19 12.80 5 4 -5 128.19 12.40 5 -4 5 115.29 13.40 5 4 -5 129.89 12.70 -5 -4 -5 116.19 12.80 -5 4 5 127.09 12.60 5 -4 5 120.69 12.40 -5 -4 5 110.09 12.40 5 -4 -5 109.29 12.80 -5 -4 5 110.89 13.60 5 4 5 116.49 12.90 -5 -4 5 121.39 12.60 5 -4 -5 129.79 12.50 5 -4 -5 113.19 13.40 5 -4 -5 117.49 12.20 -5 4 -5 109.49 12.60 -5 4 -5 105.09 12.70 5 4 5 126.89 12.40 5 4 5 132.99 12.90 5 -4 -5 129.69 13.40 -5 4 -5 119.59 12.20 5 -5 5 1.90 2.90 5 5 -5 4.60 2.20 -5 -5 -5 2.70 2.20 -5 5 5 2.30 2.10 5 5 -5 -0.30 1.40 5 -5 5 3.60 3.30 -5 -5 -5 10.10 2.90 5 -5 5 4.80 1.90 -5 -5 -5 -2.40 1.70 5 5 -5 2.00 2.30 -5 -5 5 0.40 3.00 -5 5 -5 1.40 1.70 -5 -5 5 -1.10 2.00 5 -5 -5 3.10 1.80 5 -5 -5 2.60 2.60 -5 5 -5 3.20 2.00 5 -5 -5 2.70 2.50 5 5 5 4.20 2.00 -5 5 -5 -0.40 2.30 5 -5 -5 -2.30 2.40 5 5 5 2.40 2.20 5 -5 -5 1.40 1.80 -5 -5 5 -0.10 1.60 5 5 5 0.70 2.10 5 6 -5 6.80 2.10 5 6 -5 8.90 3.20 -5 -6 -5 9.10 3.00 -5 6 5 10.10 3.30 -5 -6 -5 14.30 4.10 5 6 -5 7.10 3.00 5 -6 5 11.70 4.40 5 -6 5 14.20 2.60 5 -6 5 13.10 4.90 -5 -6 -5 7.30 3.20 -5 6 5 13.70 3.80 5 -6 -5 12.10 4.00 5 6 5 11.80 3.30 5 -6 -5 14.10 3.10 5 -6 -5 3.20 3.70 -5 -6 5 10.90 3.20 5 6 5 15.20 3.60 -5 -6 5 9.10 3.30 -5 -6 5 8.70 4.60 -5 6 -5 12.30 2.90 -5 6 -5 7.40 3.00 5 -6 -5 2.50 2.10 -5 6 -5 5.20 3.10 -5 7 5 8.40 4.50 -5 7 5 14.70 4.20 5 7 -5 21.70 4.40 5 -7 5 19.10 5.10 5 -7 5 18.00 6.10 -5 7 5 17.20 4.10 -5 -7 -5 20.10 5.10 -5 -7 -5 15.20 4.50 -5 -7 -5 11.60 3.70 5 7 -5 16.10 4.20 5 7 -5 16.70 4.40 -5 -7 5 11.90 5.50 5 -7 -5 23.20 5.20 -5 7 -5 14.90 3.50 5 7 5 29.40 4.60 5 -7 -5 18.00 5.30 5 7 5 7.40 3.70 -5 7 -5 15.40 4.50 -5 7 -5 9.10 3.60 5 -7 -5 17.10 4.20 5 -8 5 13.90 5.40 -5 8 5 15.40 4.30 -5 -8 -5 10.10 3.80 5 8 -5 14.90 4.30 -5 8 5 16.30 4.30 -5 -8 -5 19.10 5.50 5 -8 5 11.70 4.70 5 8 -5 6.90 3.70 5 8 -5 14.90 4.40 -5 -8 -5 12.00 4.00 -5 8 5 13.60 4.10 5 -8 -5 5.40 4.60 -5 8 -5 18.40 4.70 -5 8 -5 14.50 4.40 5 -8 -5 19.60 5.00 -5 8 -5 14.20 5.10 -5 -8 5 10.80 5.00 5 8 5 9.50 3.90 5 9 -5 -4.50 2.50 5 9 -5 1.40 3.40 5 -9 5 11.00 5.70 -5 9 5 1.30 3.20 -5 -9 -5 -2.80 1.90 5 -9 5 8.10 2.70 5 9 -5 4.80 3.80 -5 9 5 4.50 3.40 -5 -9 -5 0.10 2.70 -5 9 5 -2.80 3.50 5 -9 -5 -3.80 3.30 5 9 5 -3.90 2.40 5 -9 -5 -1.20 3.30 -5 9 -5 2.10 3.30 -5 -9 5 0.00 3.70 -5 9 -5 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2 6 8.50 2.90 5 -2 -6 6.50 1.90 -5 2 -6 1.70 2.10 5 -2 -6 4.50 2.70 -5 2 -6 0.20 1.70 5 -2 -6 4.00 2.50 5 -2 -6 3.00 1.40 5 3 -6 45.60 5.30 5 3 -6 46.50 6.00 5 -3 6 47.60 5.90 5 -3 6 54.79 7.50 -5 -3 -6 27.00 5.30 -5 -3 -6 41.30 4.90 -5 3 6 43.90 6.10 -5 3 6 43.90 5.00 5 3 -6 31.70 5.20 -5 -3 -6 38.50 5.90 -5 -3 -6 50.49 6.30 5 3 -6 37.30 4.80 -5 3 -6 34.40 5.50 5 -3 -6 46.30 5.00 -5 -3 6 46.90 7.70 -5 3 -6 43.60 5.10 -5 3 -6 36.30 5.70 5 -3 -6 42.70 6.60 5 3 6 54.09 6.70 5 3 6 46.40 5.60 5 -3 -6 64.49 7.40 5 4 -6 2.70 1.70 -5 -4 -6 1.70 2.10 5 4 -6 3.10 1.80 -5 -4 -6 2.80 1.70 -5 -4 -6 5.30 2.50 -5 -4 -6 1.40 1.90 5 4 -6 4.70 2.10 5 4 -6 4.10 2.10 -5 4 6 1.20 1.60 -5 4 6 0.60 2.50 5 -4 6 1.30 3.10 5 -4 6 2.40 2.40 5 -4 6 1.30 1.90 5 -4 -6 0.90 1.50 5 -4 -6 1.60 1.50 -5 4 -6 1.20 1.60 5 -4 -6 1.70 2.40 5 4 6 0.90 2.20 -5 4 -6 1.70 2.10 5 4 6 -0.90 2.00 -5 -4 6 1.20 2.50 -5 -4 6 -0.70 3.30 5 -4 -6 4.70 2.70 -5 4 -6 1.70 2.20 5 5 -6 3.80 2.30 -5 5 6 2.30 2.20 5 5 -6 6.60 2.40 5 5 -6 1.70 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-16 3 5 6.10 5.10 16 -3 5 8.80 4.40 16 -3 5 6.00 4.70 16 3 -5 4.00 4.30 -16 -3 5 -1.40 6.20 16 3 5 2.90 4.00 16 -3 -5 3.00 4.00 -16 3 -5 2.30 4.00 16 -3 -5 4.00 5.10 -16 3 -5 3.70 5.20 16 0 -6 -6.20 2.90 -16 0 -6 -2.70 3.70 -16 0 6 1.30 4.90 16 0 6 1.20 4.80 16 0 6 -1.10 3.50 16 0 -6 -0.20 6.30 16 -1 6 11.10 4.80 -16 -1 -6 6.20 4.30 16 1 -6 23.30 8.20 -16 1 6 13.40 6.20 16 -1 6 22.70 6.80 -16 1 -6 10.50 5.00 16 -1 -6 13.20 5.90 -16 -1 6 8.50 6.00 16 -1 -6 20.30 5.80 16 1 6 16.90 5.90 16 1 6 12.70 4.90 16 -2 6 6.00 4.40 16 2 -6 12.80 6.90 16 2 -6 13.70 5.30 16 -2 6 13.90 6.20 -16 2 6 8.90 6.00 -16 -2 -6 7.60 4.10 16 -2 -6 14.40 6.20 16 2 6 16.30 5.20 -16 2 -6 8.10 4.60 -16 -2 6 3.20 6.00 16 -2 -6 11.00 4.80 16 0 7 -1.10 3.00 16 0 -7 2.20 4.40 16 0 -7 5.30 7.10 -16 0 7 -3.80 4.40 -16 0 -7 0.80 4.10 16 0 7 2.40 4.50 16 1 -7 0.90 5.10 16 1 -7 8.20 4.80 -16 -1 -7 3.50 4.30 -16 1 7 2.10 6.00 16 -1 7 4.60 5.00 16 -1 7 10.30 4.30 16 1 7 13.20 6.00 -16 -1 7 1.40 6.10 16 -1 -7 7.70 5.50 16 -1 -7 6.60 4.60 16 1 7 2.80 4.00 -16 1 -7 5.90 4.30 17 0 0 -4.70 3.40 17 0 0 11.30 5.70 -17 0 0 -1.30 3.40 -17 0 0 -1.40 5.10 -17 1 0 0.00 5.10 17 1 0 5.70 4.70 17 1 0 3.50 4.60 -17 -1 0 -4.10 4.90 -17 -1 0 5.70 3.60 17 -1 0 2.70 5.10 -17 1 0 1.60 3.50 17 -1 0 4.00 3.70 -17 2 0 -5.50 3.40 17 -2 0 1.70 3.50 -17 2 0 -4.50 4.00 17 2 0 1.30 4.20 -17 -2 0 -5.00 5.50 17 -2 0 -0.10 3.80 -17 -2 0 2.70 3.50 -17 3 0 -6.90 3.50 17 -3 0 -4.90 3.40 -17 3 0 -6.00 5.10 17 3 0 0.50 3.90 -17 -3 0 -8.60 6.00 -17 -3 0 2.80 3.40 17 0 1 0.90 4.60 -17 0 -1 -1.00 3.70 -17 0 1 -5.30 3.60 -17 0 -1 -1.70 5.20 17 0 -1 4.60 5.10 -17 0 1 -0.50 4.70 17 0 1 0.50 3.30 17 0 -1 -5.20 3.30 17 1 -1 8.10 4.70 -17 -1 -1 18.30 5.90 -17 -1 -1 1.90 3.60 -17 1 1 5.00 5.10 17 -1 1 5.10 4.20 17 1 -1 9.70 5.80 17 -1 1 7.60 5.50 -17 1 1 8.10 6.00 -17 1 -1 2.10 5.50 17 1 1 13.90 5.50 17 -1 -1 13.50 7.10 -17 -1 1 -1.20 5.30 -17 1 -1 7.60 4.50 17 -1 -1 8.00 4.50 17 1 1 12.80 4.90 -17 -1 1 10.70 6.50 17 -2 1 9.90 5.00 -17 2 1 0.70 4.50 17 -2 1 4.00 4.30 -17 -2 -1 -7.90 5.80 -17 -2 -1 0.70 3.60 -17 2 1 -5.00 4.20 17 2 -1 3.30 4.10 -17 2 -1 0.40 5.40 17 -2 -1 8.00 5.40 17 2 1 1.40 3.70 17 -2 -1 6.30 4.20 -17 -2 1 -3.30 5.40 -17 3 1 -7.40 5.00 17 3 -1 -1.90 3.90 -17 -3 -1 -9.80 5.90 -17 3 1 -0.50 4.50 17 -3 1 4.30 4.70 17 -3 1 -4.80 3.30 -17 -3 -1 8.50 4.20 -17 3 -1 -6.00 3.80 17 3 1 1.10 3.70 17 -3 -1 2.20 4.10 17 -3 -1 6.40 5.10 -17 -3 1 -8.90 6.10 -17 3 -1 -4.60 4.50 17 0 -2 11.00 6.20 17 0 -2 -4.90 3.40 -17 0 -2 -9.50 4.80 17 0 2 8.70 5.40 -17 0 2 -4.00 4.40 17 0 2 -4.30 3.30 -17 0 -2 -8.10 3.20 17 -1 2 1.50 4.50 -17 -1 -2 -3.30 5.20 -17 -1 -2 0.70 3.60 17 -1 2 6.50 4.10 17 1 -2 7.50 4.30 -17 1 2 0.60 4.60 17 1 -2 3.70 4.50 -17 -1 2 -5.90 4.40 17 1 2 5.90 4.60 -17 1 -2 -1.50 5.10 17 -1 -2 3.50 6.20 -17 1 -2 -0.40 3.80 17 1 2 2.80 3.80 17 -1 -2 4.60 4.10 -17 2 2 13.30 6.30 -17 -2 -2 8.70 4.30 17 2 -2 21.60 6.30 17 -2 2 14.80 5.10 -17 -2 -2 -1.30 6.30 17 -2 2 14.80 5.70 -17 2 -2 7.60 5.90 17 -2 -2 7.80 4.10 -17 2 -2 10.30 4.70 -17 -2 2 7.10 6.50 17 2 2 7.00 4.20 -17 -3 -2 -5.60 5.60 -17 -3 -2 0.90 3.60 -17 3 2 2.40 5.50 17 3 -2 3.10 4.20 17 -3 2 9.40 5.40 17 -3 2 1.10 4.10 17 3 2 8.10 4.20 17 -3 -2 8.80 5.60 17 -3 -2 1.50 4.10 -17 -3 2 -7.10 5.50 -17 3 -2 -4.40 4.00 -17 3 -2 3.60 5.20 -17 0 3 -7.70 4.70 17 0 3 7.80 4.20 -17 0 -3 -2.60 4.90 17 0 -3 2.50 3.90 17 0 3 6.40 5.00 17 0 -3 -1.60 5.80 -17 0 -3 3.40 4.10 -17 1 3 4.40 5.40 17 1 -3 0.70 5.50 17 -1 3 6.20 5.70 -17 -1 -3 0.10 3.90 17 1 -3 2.60 3.70 17 -1 3 -2.00 3.30 -17 -1 -3 -6.10 5.20 17 1 3 8.40 4.40 -17 1 -3 4.00 5.30 17 -1 -3 5.50 7.00 -17 1 -3 1.40 4.00 17 1 3 7.20 4.70 17 -1 -3 1.70 3.50 -17 -1 3 2.90 5.30 -17 -2 -3 2.30 4.10 17 -2 3 3.70 4.60 17 2 -3 5.10 4.40 -17 2 3 -0.30 4.70 -17 -2 -3 -10.40 3.80 17 2 -3 4.30 6.00 17 -2 3 -0.20 3.80 -17 2 -3 0.80 4.20 -17 2 -3 1.30 5.40 -17 -2 3 -7.60 4.70 17 -2 -3 11.90 5.70 17 2 3 -1.20 3.50 -17 0 -4 10.50 4.40 17 0 4 7.90 4.30 17 0 -4 2.40 6.30 -17 0 -4 -4.20 4.40 17 0 4 3.80 4.70 17 0 -4 2.30 3.90 -17 0 4 -0.50 4.70 17 -1 4 11.10 4.40 -17 -1 -4 2.40 10.80 17 1 -4 9.20 6.70 -17 1 4 4.00 5.10 -17 -1 -4 5.60 3.90 17 -1 4 22.70 6.10 17 1 -4 9.80 4.60 -17 1 -4 8.70 5.50 -17 -1 4 1.00 6.10 -17 1 -4 4.20 4.40 17 -1 -4 9.70 8.20 17 1 4 5.50 4.30 17 -1 -4 11.40 4.50 17 1 4 12.90 5.40 17 -2 4 7.60 4.40 17 -2 4 2.50 4.60 -17 2 4 -0.70 4.70 17 2 -4 6.20 6.30 -17 -2 -4 -0.80 3.90 17 2 -4 4.40 4.50 -17 -2 4 -7.20 5.70 -17 2 -4 7.10 5.60 17 2 4 -1.60 3.60 -17 2 -4 -3.40 4.00 17 -2 -4 -0.20 4.00 17 0 5 3.70 4.00 -17 0 5 1.20 5.70 -17 0 -5 -1.60 3.40 17 0 5 9.50 5.60 17 0 -5 0.60 6.90 17 0 -5 1.90 4.00 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 90008 _shelx_res_file ; TITL II_cut in Pbcn ii_revised.res created by SHELXL-2017/1 at 10:36:46 on 03-Apr-2024 rem list 6 CELL 0.71073 14.8774 8.9995 13.6349 90 90 90 ZERR 8 0.003 0.0018 0.0027 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H F N O UNIT 72 72 16 8 16 L.S. 20 PLAN 5 SIZE 0.21 0.11 0.13 TEMP -173 CONF MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.000000 3.053500 FVAR 0.28687 F1 3 0.549381 0.311687 0.350545 11.00000 0.04338 0.01988 = 0.05556 -0.00259 0.00500 0.00812 F2 3 0.268564 0.486122 0.453763 11.00000 0.03119 0.02949 = 0.06032 0.00131 0.00499 -0.00295 O2 5 0.586789 0.851638 0.348968 11.00000 0.03626 0.01764 = 0.04423 0.00273 0.00323 -0.00319 O1 5 0.454233 0.949984 0.394568 11.00000 0.03896 0.01952 = 0.05117 -0.00110 -0.00150 0.00443 N1 4 0.376696 0.250150 0.406379 11.00000 0.04054 0.01695 = 0.05472 0.00036 0.00477 -0.00220 C6 1 0.354257 0.515265 0.422828 11.00000 0.02501 0.02671 = 0.03347 0.00170 -0.00124 -0.00012 C1 1 0.407650 0.392508 0.401350 11.00000 0.03519 0.01904 = 0.02835 0.00009 -0.00530 -0.00123 C4 1 0.470659 0.687599 0.386598 11.00000 0.02849 0.01977 = 0.02756 0.00209 -0.00481 -0.00025 C2 1 0.494225 0.427615 0.372133 11.00000 0.02926 0.01943 = 0.03362 -0.00178 -0.00080 0.00836 C7 1 0.501203 0.842874 0.378070 11.00000 0.03292 0.02400 = 0.02638 -0.00173 -0.00493 0.00153 C3 1 0.527456 0.569315 0.364543 11.00000 0.03015 0.02365 = 0.02995 -0.00108 0.00019 0.00207 AFIX 43 H3 2 0.587797 0.586326 0.344706 11.00000 -1.20000 AFIX 0 C5 1 0.382932 0.658930 0.416041 11.00000 0.03264 0.01912 = 0.03206 -0.00144 -0.00544 0.00825 AFIX 43 H5 2 0.343351 0.738484 0.431279 11.00000 -1.20000 AFIX 0 C8 1 0.624140 1.000677 0.339181 11.00000 0.04371 0.01816 = 0.04321 0.00072 -0.00211 -0.00465 AFIX 23 H8A 2 0.625203 1.051356 0.403614 11.00000 -1.20000 H8B 2 0.587471 1.060564 0.293261 11.00000 -1.20000 AFIX 0 C9 1 0.717412 0.982484 0.300551 11.00000 0.04522 0.03480 = 0.06024 0.00142 0.00548 -0.01081 AFIX 137 H9A 2 0.715460 0.928930 0.238005 11.00000 -1.50000 H9B 2 0.753448 0.926045 0.347797 11.00000 -1.50000 H9C 2 0.744541 1.080539 0.290498 11.00000 -1.50000 AFIX 0 H1A 2 0.414412 0.178720 0.399035 11.00000 0.04288 H1B 2 0.325977 0.237018 0.435131 11.00000 0.04453 HKLF 4 REM II_cut in Pbcn REM R1 = 0.0599 for 1265 Fo > 4sig(Fo) and 0.0868 for all 1665 data REM 136 parameters refined using 0 restraints END WGHT 0.0000 3.0535 REM Highest difference peak 0.198, deepest hole -0.265, 1-sigma level 0.054 Q1 1 0.6566 0.8059 0.3995 11.00000 0.05 0.20 Q2 1 0.6266 0.2947 0.3429 11.00000 0.05 0.18 Q3 1 0.8197 1.0042 0.3037 11.00000 0.05 0.18 Q4 1 0.3759 0.2037 0.3530 11.00000 0.05 0.18 Q5 1 0.4233 0.6743 0.3801 11.00000 0.05 0.18 ; _shelx_res_checksum 61937 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F F1 0.54938(12) 0.31169(18) 0.35054(15) 0.0396(5) Uani d 1 . . F F2 0.26856(12) 0.4861(2) 0.45376(15) 0.0403(5) Uani d 1 . . O O2 0.58679(14) 0.8516(2) 0.34897(17) 0.0327(6) Uani d 1 . . O O1 0.45423(15) 0.9500(2) 0.39457(17) 0.0365(6) Uani d 1 . . N N1 0.3767(2) 0.2502(3) 0.4064(2) 0.0374(8) Uani d 1 . . C C6 0.35426(19) 0.5153(3) 0.4228(2) 0.0284(7) Uani d 1 . . C C1 0.4077(2) 0.3925(3) 0.4014(2) 0.0275(7) Uani d 1 . . C C4 0.4707(2) 0.6876(3) 0.3866(2) 0.0253(7) Uani d 1 . . C C2 0.4942(2) 0.4276(3) 0.3721(2) 0.0274(7) Uani d 1 . . C C7 0.5012(2) 0.8429(3) 0.3781(2) 0.0278(7) Uani d 1 . . C C3 0.5275(2) 0.5693(3) 0.3645(2) 0.0279(7) Uani d 1 . . H H3 0.587797 0.586326 0.344706 0.033 Uiso calc 1 . . C C5 0.3829(2) 0.6589(3) 0.4160(2) 0.0279(7) Uani d 1 . . H H5 0.343351 0.738484 0.431279 0.034 Uiso calc 1 . . C C8 0.6241(2) 1.0007(3) 0.3392(3) 0.0350(8) Uani d 1 . . H H8A 0.625203 1.051356 0.403614 0.042 Uiso calc 1 . . H H8B 0.587471 1.060564 0.293261 0.042 Uiso calc 1 . . C C9 0.7174(2) 0.9825(4) 0.3006(3) 0.0468(10) Uani d 1 . . H H9A 0.715460 0.928930 0.238005 0.070 Uiso calc 1 . . H H9B 0.753448 0.926045 0.347797 0.070 Uiso calc 1 . . H H9C 0.744541 1.080539 0.290498 0.070 Uiso calc 1 . . H H1A 0.414(2) 0.179(4) 0.399(3) 0.043(11) Uiso d 1 . . H H1B 0.326(3) 0.237(4) 0.435(3) 0.045(12) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F1 0.0434(11) 0.0199(9) 0.0556(13) 0.0081(8) 0.0050(10) -0.0026(9) F2 0.0312(10) 0.0295(10) 0.0603(13) -0.0029(8) 0.0050(9) 0.0013(9) O2 0.0363(13) 0.0176(10) 0.0442(14) -0.0032(9) 0.0032(10) 0.0027(10) O1 0.0390(13) 0.0195(11) 0.0512(16) 0.0044(10) -0.0015(11) -0.0011(10) N1 0.0405(19) 0.0169(14) 0.055(2) -0.0022(14) 0.0048(16) 0.0004(13) C6 0.0250(16) 0.0267(17) 0.0335(18) -0.0001(13) -0.0012(14) 0.0017(14) C1 0.0352(18) 0.0190(15) 0.0284(18) -0.0012(13) -0.0053(14) 0.0001(13) C4 0.0285(17) 0.0198(15) 0.0276(17) -0.0003(12) -0.0048(13) 0.0021(12) C2 0.0293(17) 0.0194(15) 0.0336(18) 0.0084(13) -0.0008(14) -0.0018(13) C7 0.0329(18) 0.0240(16) 0.0264(17) 0.0015(14) -0.0049(14) -0.0017(14) C3 0.0302(18) 0.0236(16) 0.0299(18) 0.0021(13) 0.0002(13) -0.0011(13) C5 0.0326(18) 0.0191(15) 0.0321(18) 0.0082(13) -0.0054(14) -0.0014(13) C8 0.044(2) 0.0182(15) 0.043(2) -0.0047(15) -0.0021(16) 0.0007(14) C9 0.045(2) 0.035(2) 0.060(3) -0.0108(17) 0.0055(19) 0.0014(18) 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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 O2 C8 . . 116.4(2) ? C1 N1 H1A . . 118(2) ? C1 N1 H1B . . 117(2) ? H1A N1 H1B . . 122(3) ? F2 C6 C1 . . 116.4(3) ? C5 C6 F2 . . 119.6(3) ? C5 C6 C1 . . 124.0(3) ? N1 C1 C6 . . 122.9(3) ? N1 C1 C2 . . 122.9(3) ? C2 C1 C6 . . 114.2(3) ? C3 C4 C7 . . 121.4(3) ? C5 C4 C7 . . 119.2(3) ? C5 C4 C3 . . 119.4(3) ? F1 C2 C1 . . 116.7(3) ? F1 C2 C3 . . 118.7(3) ? C3 C2 C1 . . 124.7(3) ? O2 C7 C4 . . 111.9(3) ? O1 C7 O2 . . 123.9(3) ? O1 C7 C4 . . 124.2(3) ? C4 C3 H3 . . 120.8 ? C2 C3 C4 . . 118.4(3) ? C2 C3 H3 . . 120.8 ? C6 C5 C4 . . 119.3(3) ? C6 C5 H5 . . 120.4 ? C4 C5 H5 . . 120.4 ? O2 C8 H8A . . 110.4 ? O2 C8 H8B . . 110.4 ? O2 C8 C9 . . 106.6(3) ? H8A C8 H8B . . 108.6 ? C9 C8 H8A . . 110.4 ? C9 C8 H8B . . 110.4 ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9B . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 C2 . 1.360(3) ? F2 C6 . 1.368(3) ? O2 C7 . 1.336(4) ? O2 C8 . 1.458(4) ? O1 C7 . 1.212(4) ? N1 C1 . 1.363(4) ? N1 H1A . 0.86(4) ? N1 H1B . 0.86(4) ? C6 C1 . 1.392(4) ? C6 C5 . 1.365(4) ? C1 C2 . 1.385(4) ? C4 C7 . 1.474(4) ? C4 C3 . 1.392(4) ? C4 C5 . 1.390(4) ? C2 C3 . 1.372(4) ? C3 H3 . 0.9500 ? C5 H5 . 0.9500 ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C8 C9 . 1.493(5) ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A O1 1_545 0.85(3) 2.15(4) 2.942(3) 155(3) C8 H8B F1 1_565 0.99 2.46 3.015(3) 115 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag F1 C2 C3 C4 . . . . 179.9(3) ? F2 C6 C1 N1 . . . . 2.6(5) ? F2 C6 C1 C2 . . . . -178.9(3) ? F2 C6 C5 C4 . . . . 178.6(3) ? N1 C1 C2 F1 . . . . -1.7(5) ? N1 C1 C2 C3 . . . . 178.9(3) ? C6 C1 C2 F1 . . . . 179.8(3) ? C6 C1 C2 C3 . . . . 0.4(5) ? C1 C6 C5 C4 . . . . -0.4(5) ? C1 C2 C3 C4 . . . . -0.7(5) ? C7 O2 C8 C9 . . . . -176.7(3) ? C7 C4 C3 C2 . . . . -178.7(3) ? C7 C4 C5 C6 . . . . 179.2(3) ? C3 C4 C7 O2 . . . . -0.8(4) ? C3 C4 C7 O1 . . . . 178.6(3) ? C3 C4 C5 C6 . . . . 0.1(5) ? C5 C6 C1 N1 . . . . -178.3(3) ? C5 C6 C1 C2 . . . . 0.2(5) ? C5 C4 C7 O2 . . . . -179.9(3) ? C5 C4 C7 O1 . . . . -0.5(5) ? C5 C4 C3 C2 . . . . 0.4(5) ? C8 O2 C7 O1 . . . . 1.3(4) ? C8 O2 C7 C4 . . . . -179.3(3) ?