#------------------------------------------------------------------------------ #$Date: 2022-10-29 14:06:44 +0200 (Sat, 29 Oct 2022) $ #$Revision: 278874 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022689.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_2022689 loop_ _publ_author_name 'Mandal, Koushik' 'Sarkar, Sounak' 'Ghosh, Peuli' 'Hathwar, Venkatesha R.' 'Chopra, Deepak' _publ_section_title ; Quantitative insights into noncovalent interactions involving halogen and tetrel bonds in 2,4,6-trimethylpyrylium tetrafluoroborate ; _journal_coeditor_code QZ3001 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229622009469 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C8 H11 O +, B F4 -' _chemical_formula_moiety 'C8 H11 O +, B F4 -' _chemical_formula_sum 'C8 H11 B F4 O' _chemical_formula_weight 209.98 _chemical_name_systematic ; 2,4,6-Trimethylpyrylium tetrafluoroborate ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7906(5) _cell_length_b 9.6859(5) _cell_length_c 9.8673(5) _cell_measurement_reflns_used 4437 _cell_measurement_temperature 100 _cell_measurement_theta_max 29.84 _cell_measurement_theta_min 2.93 _cell_volume 935.72(8) _computing_cell_refinement ; SAINT (Bruker, 2015) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2015) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009), PARST (Nardelli, 1995) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_unetI/netI 0.0173 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9024 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.880 _diffrn_reflns_theta_min 2.931 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_correction_T_min 0.6956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_description plate _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.189 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.065 _refine_diff_density_max 0.385 _refine_diff_density_min -0.246 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 93 _refine_ls_number_reflns 1424 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0354 _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^)+(0.0398P)^2^+0.3609P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.0896 _reflns_number_gt 1236 _reflns_number_total 1424 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qz3001sup1.cif _cod_data_source_block I _cod_database_code 2022689 _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 6.10 0.60 0 -3 0 -1.00 0.60 0 3 0 -0.90 0.60 0 3 0 0.90 0.80 0 4 0 1309.27 25.80 0 4 0 1370.16 26.20 0 4 0 1345.77 25.90 0 5 0 -0.20 0.90 0 5 0 -0.20 1.10 0 5 0 0.20 0.90 0 6 0 1172.48 24.40 0 6 0 1173.68 24.70 0 6 0 1196.88 24.50 0 7 0 -0.60 0.90 0 8 0 9527.35 170.58 0 8 0 9999.00 170.78 0 9 0 -0.70 1.40 0 9 0 2.30 1.70 0 -10 0 847.92 22.20 0 -10 0 867.51 22.10 0 10 0 885.41 22.20 0 -11 0 1.20 2.20 0 -11 0 3.50 2.20 0 11 0 1.60 2.30 0 12 0 5.60 2.70 0 -12 0 9.00 3.30 0 -12 0 6.30 3.00 0 13 0 0.40 2.80 0 -13 0 -1.20 2.70 0 -13 0 0.10 2.60 -1 0 0 -0.20 0.10 1 0 0 -0.30 0.10 1 0 0 0.10 0.20 1 -1 0 -5.30 0.40 -1 -1 0 -4.50 0.50 1 -1 0 -5.10 0.40 -1 1 0 -5.50 0.30 -1 1 0 -5.20 0.40 1 1 0 -5.20 0.50 1 2 0 0.70 0.60 1 -2 0 -0.40 0.40 1 -2 0 0.60 0.30 -1 -2 0 -0.50 0.40 -1 2 0 0.00 0.40 1 3 0 -1.00 0.50 1 -3 0 -0.20 0.50 -1 3 0 -0.30 0.60 -1 -3 0 -0.50 0.60 1 3 0 0.20 0.60 -1 3 0 0.00 0.60 -1 4 0 0.90 0.80 1 4 0 0.90 0.70 1 4 0 0.10 0.90 1 -4 0 0.80 0.60 1 4 0 -0.20 0.60 -1 4 0 2.20 0.90 1 5 0 0.60 1.10 1 5 0 -0.40 0.80 -1 5 0 -0.10 0.90 -1 5 0 -1.30 0.60 1 5 0 0.70 0.80 1 6 0 -0.10 0.90 -1 6 0 1.00 0.90 -1 6 0 -0.50 0.90 1 6 0 -0.30 0.90 1 6 0 -0.60 1.10 1 -7 0 0.70 1.30 1 7 0 -0.50 1.00 -1 7 0 -1.30 0.90 1 7 0 2.60 1.60 1 7 0 -0.50 0.90 -1 7 0 -0.30 1.10 1 8 0 0.10 1.50 1 -8 0 1.50 1.60 1 8 0 -0.80 1.40 -1 8 0 -0.70 1.20 1 8 0 -1.70 1.10 -1 8 0 -0.60 1.10 1 -9 0 -1.40 1.40 1 9 0 -1.30 1.40 -1 9 0 1.60 1.90 1 9 0 -2.00 1.30 1 10 0 0.60 1.70 1 -10 0 0.00 2.00 1 10 0 2.60 2.10 -1 10 0 1.20 2.00 1 -10 0 -0.40 1.70 -1 -11 0 3.00 2.10 1 11 0 3.10 2.10 1 -11 0 0.10 1.90 -1 11 0 0.90 2.30 1 -11 0 -0.70 2.10 -1 -12 0 0.50 2.30 -1 12 0 6.00 2.80 -1 -12 0 -0.20 2.30 1 -12 0 1.50 2.30 1 12 0 -1.00 2.10 1 -12 0 1.10 2.60 1 13 0 6.50 3.20 -1 -13 0 -1.60 2.80 -1 -13 0 1.40 2.50 -1 13 0 -0.70 2.60 1 -13 0 0.10 2.70 1 -13 0 -1.50 2.30 2 0 0 149.09 3.70 -2 0 0 155.68 3.80 2 0 0 157.98 3.70 2 -1 0 3800.42 65.39 -2 -2 0 4638.34 82.69 -2 2 0 4901.01 82.19 -2 3 0 3062.29 55.59 -2 3 0 3105.49 54.99 2 -3 0 3161.18 56.79 2 -3 0 3142.59 54.79 2 -3 0 3193.88 54.59 2 3 0 3184.48 56.09 -2 4 0 316.27 8.50 2 -4 0 319.17 7.20 2 4 0 330.87 8.40 -2 4 0 316.77 8.00 2 4 0 321.47 8.70 2 -4 0 327.47 7.80 2 -4 0 331.87 8.60 2 -5 0 2372.76 43.50 2 5 0 2427.66 43.90 2 5 0 1982.20 42.10 -2 5 0 2387.36 42.90 -2 5 0 2358.46 43.60 2 5 0 2372.46 43.40 2 -5 0 2376.36 41.20 -2 6 0 379.56 10.20 2 6 0 376.96 10.70 2 -6 0 373.76 10.60 2 6 0 389.16 10.20 2 6 0 386.86 10.90 -2 6 0 376.36 10.70 2 7 0 582.34 14.10 2 -7 0 548.05 14.50 -2 7 0 558.14 14.60 -2 7 0 553.34 14.10 2 7 0 546.15 14.70 2 7 0 551.04 14.60 2 -8 0 10.70 2.50 2 8 0 10.20 2.40 2 -8 0 17.60 3.00 -2 8 0 7.00 2.20 2 8 0 16.50 2.80 2 8 0 13.00 2.70 -2 8 0 14.90 2.60 -2 9 0 504.55 15.00 2 9 0 493.25 15.10 2 -9 0 501.25 15.00 2 9 0 489.35 15.00 2 9 0 504.95 14.30 2 -9 0 504.15 15.00 2 10 0 260.77 10.10 2 -10 0 253.57 10.50 2 10 0 277.77 11.10 -2 10 0 267.97 10.90 2 10 0 286.67 11.00 2 -10 0 270.77 10.80 2 -11 0 23.50 4.10 2 -11 0 39.30 5.20 -2 -11 0 26.20 4.10 -2 11 0 24.70 4.20 2 11 0 36.90 4.90 2 12 0 4.20 2.80 -2 12 0 6.30 3.20 2 -12 0 9.20 3.30 2 -12 0 11.10 3.70 -2 -12 0 7.00 2.90 2 -13 0 184.88 10.40 2 -13 0 164.38 10.00 -2 -13 0 176.08 10.30 -2 13 0 182.28 10.30 3 0 0 -9.20 0.60 3 0 0 -10.30 0.60 -3 0 0 -9.30 0.70 3 1 0 -0.70 0.40 -3 -1 0 -1.50 0.40 -3 1 0 -0.70 0.60 -3 -1 0 -1.40 0.40 3 1 0 -1.30 0.30 -3 -1 0 -2.10 0.50 -3 1 0 -1.20 0.50 3 -1 0 -1.60 0.50 -3 2 0 -0.30 0.40 -3 -2 0 0.10 0.40 3 -2 0 0.10 0.50 -3 2 0 0.60 0.60 3 -2 0 -0.40 0.50 3 -2 0 0.10 0.50 3 2 0 0.10 0.60 -3 2 0 -0.60 0.50 -3 -2 0 0.90 0.40 3 -3 0 -0.30 0.70 3 -3 0 -0.60 0.50 -3 -3 0 -0.90 0.30 3 -3 0 0.60 0.80 -3 3 0 1.00 0.80 3 3 0 0.00 0.70 -3 3 0 0.10 0.60 3 -3 0 0.30 0.60 -3 3 0 -0.10 0.50 3 3 0 0.50 0.80 3 4 0 -0.20 0.90 3 -4 0 -2.50 0.80 3 4 0 -0.80 0.90 3 4 0 -1.60 0.60 3 -4 0 -1.90 0.60 -3 4 0 -0.80 0.90 3 -4 0 -1.00 1.00 -3 4 0 -1.10 0.50 -3 4 0 -1.10 0.70 3 -5 0 0.50 1.00 3 5 0 0.20 0.90 -3 5 0 1.10 0.90 -3 5 0 -0.20 1.00 3 -5 0 -0.10 1.00 3 -5 0 0.60 0.80 3 5 0 1.00 0.90 3 5 0 1.20 1.10 -3 6 0 -0.40 0.80 3 -6 0 0.20 1.20 3 -6 0 0.00 1.00 3 6 0 -1.20 0.70 3 6 0 0.70 1.10 -3 6 0 0.50 1.10 3 6 0 0.20 1.20 -3 7 0 1.40 1.20 -3 7 0 1.30 1.40 3 -7 0 0.10 1.20 3 7 0 -0.80 1.10 3 7 0 0.10 0.60 3 -7 0 0.40 1.50 3 7 0 0.90 1.40 3 -8 0 0.50 1.50 -3 8 0 0.90 1.50 3 8 0 -0.30 1.20 3 8 0 -1.70 1.50 3 8 0 -1.70 1.20 3 -8 0 -0.90 1.20 3 9 0 -0.80 1.50 3 -9 0 1.00 1.70 -3 9 0 -2.70 1.40 3 -9 0 0.50 1.80 3 9 0 3.80 1.90 3 9 0 0.70 1.90 -3 10 0 -1.20 1.70 3 -10 0 -0.10 1.70 3 10 0 1.50 1.70 3 10 0 -0.60 2.10 3 -10 0 -0.70 1.70 3 -11 0 -0.50 1.80 3 -11 0 3.90 2.70 3 11 0 -1.90 1.90 -3 11 0 0.90 2.20 -3 12 0 -0.80 2.50 3 -12 0 2.00 2.70 3 -12 0 -0.70 2.20 3 -13 0 3.40 3.10 -3 13 0 0.80 3.00 4 0 0 69.09 2.90 4 0 0 66.19 2.70 -4 0 0 63.19 2.90 4 0 0 67.19 2.80 4 -1 0 2568.84 44.00 -4 1 0 2578.64 44.00 4 1 0 2390.46 44.10 -4 -1 0 2557.64 44.60 4 -1 0 2518.35 45.10 4 1 0 2539.05 44.90 4 -1 0 2480.65 45.10 -4 1 0 2495.15 45.20 4 1 0 2455.95 44.00 4 2 0 741.23 13.50 4 -2 0 763.92 15.60 4 2 0 746.93 15.20 -4 2 0 744.63 15.00 4 -2 0 757.72 15.60 -4 -2 0 726.13 14.50 -4 2 0 737.13 15.40 4 2 0 723.63 13.50 -4 2 0 741.93 15.00 4 -3 0 53.39 2.90 4 -3 0 56.89 2.90 -4 3 0 57.89 2.90 -4 -3 0 56.49 2.20 4 3 0 56.89 2.90 4 3 0 53.99 3.30 -4 3 0 54.99 2.70 -4 3 0 55.59 2.90 4 -3 0 54.69 3.10 4 -4 0 122.99 4.60 -4 4 0 125.69 4.50 4 4 0 122.19 3.90 4 -4 0 118.29 4.80 4 4 0 125.69 5.30 4 4 0 125.99 4.90 -4 -4 0 121.69 3.30 -4 4 0 122.89 4.90 4 -4 0 122.39 5.00 -4 4 0 123.29 4.10 4 -5 0 2.00 1.20 4 5 0 2.00 0.90 -4 5 0 0.60 1.10 -4 5 0 2.10 0.90 4 5 0 2.40 1.20 4 5 0 3.40 1.40 4 -5 0 1.40 1.20 -4 6 0 70.59 3.90 4 6 0 74.09 4.70 4 6 0 78.49 3.80 4 -6 0 82.29 4.60 4 6 0 70.89 4.30 -4 6 0 75.69 4.50 4 -6 0 66.59 4.30 4 7 0 144.99 5.70 4 7 0 152.58 7.10 4 -7 0 128.39 6.40 -4 7 0 140.09 6.60 4 -7 0 136.99 6.50 4 7 0 150.48 6.70 4 -8 0 0.70 1.60 4 8 0 -0.20 1.40 -4 8 0 2.70 1.70 4 -8 0 3.20 1.80 4 8 0 0.90 1.80 4 -9 0 519.75 15.50 4 -9 0 490.85 15.10 -4 9 0 482.25 15.10 4 9 0 487.55 15.20 4 9 0 512.15 20.30 4 -10 0 2.20 2.30 4 10 0 1.60 2.50 4 -10 0 2.30 2.20 -4 10 0 1.10 2.20 4 -11 0 0.00 2.40 4 11 0 5.40 2.90 4 -11 0 2.00 2.40 -4 11 0 0.80 2.30 4 -12 0 99.99 8.70 4 12 0 85.49 8.20 4 -12 0 93.79 8.40 -4 12 0 81.79 8.20 5 0 0 -0.10 0.70 5 0 0 -0.20 0.60 5 0 0 -0.70 0.50 5 1 0 -0.10 0.40 5 1 0 0.00 0.50 5 -1 0 0.00 0.60 -5 1 0 0.00 0.80 5 -1 0 -0.10 0.60 5 -1 0 0.80 0.70 5 -1 0 1.20 0.80 -5 1 0 0.70 0.60 5 1 0 0.80 0.70 5 2 0 -0.60 0.60 5 -2 0 0.10 0.70 5 -2 0 -0.10 0.70 -5 2 0 0.30 0.60 5 -2 0 1.10 0.70 -5 2 0 -0.40 0.70 5 2 0 0.10 0.40 -5 2 0 -0.60 0.60 5 2 0 -0.10 0.40 -5 -2 0 0.50 0.60 -5 -3 0 0.40 0.60 -5 3 0 0.10 0.70 5 -3 0 -0.20 0.70 -5 3 0 -0.30 0.70 5 -3 0 0.00 0.80 5 3 0 -0.20 0.70 -5 3 0 0.60 0.70 5 -3 0 0.40 0.70 5 4 0 1.70 1.20 5 -4 0 1.40 1.00 -5 4 0 -0.10 0.90 -5 4 0 0.40 0.70 5 4 0 1.50 1.10 5 -4 0 -0.10 0.80 5 -4 0 -0.20 1.00 5 -5 0 0.50 1.20 5 -5 0 0.50 1.00 5 5 0 1.80 1.30 5 5 0 -1.00 0.90 -5 5 0 0.50 1.00 -5 5 0 -0.60 0.80 5 -6 0 2.00 1.50 5 -6 0 -0.50 1.00 -5 6 0 -0.10 1.20 5 6 0 0.60 1.20 -5 6 0 0.30 0.90 5 6 0 2.50 1.60 5 -7 0 1.20 1.70 5 7 0 2.20 1.60 5 7 0 -0.40 1.30 -5 7 0 2.90 1.60 5 -7 0 -0.30 1.30 5 -8 0 -0.90 1.40 5 8 0 -0.60 1.70 -5 8 0 0.60 1.70 5 -8 0 0.20 1.60 5 8 0 -1.00 1.40 -5 9 0 2.50 2.10 5 -9 0 1.10 2.00 5 -9 0 1.00 1.90 5 9 0 1.80 2.30 5 -10 0 -2.80 1.60 5 -10 0 -0.60 2.00 -5 10 0 -2.80 1.90 5 10 0 -0.10 2.00 -5 11 0 5.80 3.10 5 -11 0 -1.20 2.10 5 -11 0 -1.30 2.10 5 11 0 3.10 3.00 -5 12 0 -1.00 2.60 5 -12 0 4.60 2.90 5 -12 0 1.60 2.90 6 0 0 8042.20 140.29 6 0 0 8205.08 140.69 6 -1 0 768.52 16.50 6 -1 0 783.62 15.10 -6 1 0 768.32 16.70 6 -1 0 767.72 16.80 6 -1 0 748.73 16.80 6 1 0 749.03 15.70 6 1 0 738.23 15.80 6 1 0 766.22 16.60 -6 1 0 762.42 15.00 -6 2 0 1195.28 24.50 6 -2 0 1251.77 24.60 -6 2 0 1183.58 23.80 6 -2 0 1213.68 22.90 6 2 0 1139.99 21.90 -6 2 0 1174.58 22.70 6 2 0 1153.38 22.10 6 2 0 1134.99 23.80 -6 -2 0 1200.58 23.60 6 -2 0 1141.69 24.20 6 -3 0 0.00 0.40 6 3 0 1.40 1.10 6 -3 0 5.20 1.50 -6 3 0 2.60 1.10 6 -3 0 2.80 1.20 -6 3 0 3.30 1.10 6 -4 0 27.20 2.70 -6 4 0 30.70 2.90 6 4 0 27.60 3.00 6 -4 0 20.10 2.60 6 -4 0 22.30 2.90 -6 4 0 28.80 2.90 6 5 0 157.68 7.00 6 -5 0 159.18 6.40 -6 5 0 150.08 5.90 6 5 0 148.59 6.30 -6 5 0 149.59 6.30 6 -5 0 153.78 6.70 -6 6 0 288.17 9.70 6 6 0 299.87 9.90 6 6 0 274.77 10.20 6 -6 0 278.17 9.60 6 -6 0 286.67 9.90 6 -7 0 127.49 6.60 6 7 0 127.99 7.10 -6 7 0 131.99 6.80 6 -7 0 137.29 6.90 6 7 0 130.39 6.70 6 8 0 1175.88 27.30 -6 8 0 1141.09 26.90 6 -8 0 1131.69 27.00 6 -8 0 1152.48 27.00 -6 9 0 82.99 6.40 6 9 0 99.59 6.70 6 -9 0 85.49 6.30 6 -9 0 92.59 6.40 -6 10 0 163.38 9.10 6 -10 0 161.88 8.90 6 10 0 163.78 9.20 6 -10 0 158.48 8.90 6 -11 0 30.50 4.90 6 -11 0 32.00 5.00 -6 11 0 35.10 5.50 -6 12 0 -1.80 2.60 6 -12 0 2.30 3.00 6 -12 0 -0.40 2.70 7 0 0 -0.70 0.70 7 0 0 -0.50 0.80 7 1 0 0.00 0.90 7 1 0 0.30 0.70 7 -1 0 -1.30 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2.30 1.20 0 7 -4 -0.50 1.30 0 7 -4 1.30 1.70 0 7 4 -0.80 1.10 0 -7 -4 0.50 1.20 0 7 -4 -1.90 1.10 0 8 -4 188.68 9.10 0 8 -4 186.58 8.80 0 8 -4 180.68 8.20 0 -8 -4 173.08 7.40 0 8 4 178.28 7.40 0 9 4 -2.30 1.40 0 9 -4 0.70 2.20 0 9 -4 -0.70 1.50 0 -9 -4 -0.90 1.30 0 -10 -4 -0.90 1.60 0 10 -4 1.90 2.20 0 10 4 -0.70 1.60 0 11 -4 -0.10 2.20 0 11 4 -0.50 2.10 0 -11 -4 -1.40 1.70 0 12 -4 225.88 11.60 0 -12 -4 207.28 10.20 0 12 4 209.98 10.00 -1 0 -4 169.88 4.80 -1 0 4 166.28 4.80 1 0 -4 166.08 4.90 -1 0 -4 161.98 4.90 -1 0 -4 176.98 5.30 1 0 4 172.08 4.90 -1 0 4 170.88 5.00 1 0 -4 179.28 5.40 1 0 -4 167.08 5.00 1 -1 -4 1885.01 33.90 -1 1 -4 1900.61 34.80 1 -1 -4 1887.21 34.70 1 -1 -4 1915.31 35.00 -1 1 -4 1920.81 34.60 -1 1 -4 1880.21 35.50 -1 -1 4 1885.41 34.70 1 1 4 1921.61 34.00 -1 -1 -4 1890.71 34.30 1 -1 4 1881.81 34.60 1 1 -4 1941.61 35.10 1 1 -4 1908.91 34.80 1 1 -4 1869.21 34.50 -1 1 4 1955.10 33.80 -1 1 4 1889.21 34.30 1 1 -4 1858.01 35.30 -1 -1 -4 1943.11 34.70 -1 -2 4 7.20 1.20 1 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9.20 1.70 -1 5 -4 8.10 1.00 -1 5 -4 7.30 1.90 1 -5 -4 12.50 1.80 -1 5 -4 9.80 2.10 -1 5 -4 7.10 1.70 1 5 -4 10.90 2.30 1 5 -4 12.70 2.10 -1 5 4 8.00 1.80 1 5 -4 7.50 2.00 -1 -5 -4 6.60 1.40 1 -6 -4 188.98 6.30 1 6 4 191.48 6.50 -1 6 -4 194.88 8.10 -1 6 -4 190.98 7.70 -1 6 -4 185.58 7.50 1 -6 -4 181.98 6.80 1 6 -4 180.78 7.20 -1 6 4 189.08 6.90 -1 -6 -4 178.78 6.40 1 6 -4 180.68 7.60 1 6 -4 189.28 8.10 1 7 4 240.98 8.00 1 -7 -4 249.78 7.90 1 -7 -4 244.38 8.60 -1 7 -4 256.47 9.30 -1 7 -4 235.78 9.30 -1 7 -4 230.98 9.60 1 7 -4 255.97 10.10 -1 -7 -4 239.18 8.10 1 7 -4 239.18 9.00 1 7 -4 250.07 9.60 -1 7 4 250.07 8.50 -1 8 -4 29.20 4.10 1 8 4 31.30 3.50 1 -8 -4 28.20 3.60 1 -8 -4 29.20 3.30 -1 8 -4 23.30 3.90 -1 -8 -4 25.20 3.30 1 8 -4 25.90 3.70 -1 8 4 34.90 3.90 1 8 -4 31.40 4.50 1 8 -4 29.10 4.20 1 -9 -4 288.97 10.60 1 9 4 295.67 10.20 -1 9 -4 313.07 11.80 1 9 -4 293.27 11.90 -1 -9 -4 308.27 10.40 1 9 -4 311.57 11.60 -1 9 4 293.27 10.50 -1 10 -4 6.60 3.00 1 10 4 8.20 2.40 1 -10 -4 3.40 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81.69 6.00 6 -2 -10 95.79 6.50 6 2 -10 90.79 6.50 6 2 -10 99.09 6.80 6 -3 -10 2.00 2.30 6 3 -10 0.90 2.30 6 3 -10 3.40 2.20 6 -4 -10 87.89 6.70 6 4 -10 73.49 6.80 6 4 -10 100.19 7.40 6 -5 -10 10.50 3.10 6 5 -10 7.10 3.40 6 5 -10 7.30 2.90 6 -6 -10 28.40 4.70 6 6 -10 28.00 4.70 6 6 -10 38.70 6.00 6 -7 -10 48.50 6.00 6 7 -10 59.89 7.70 6 7 -10 47.00 6.40 7 0 -10 261.77 10.80 7 0 -10 251.17 10.60 7 -1 -10 10.90 3.00 7 1 -10 13.40 3.30 7 1 -10 7.30 2.80 7 -2 -10 4.30 2.50 7 2 -10 4.10 2.30 7 2 -10 1.50 2.40 7 -3 -10 12.90 3.20 7 3 -10 19.90 4.40 7 3 -10 19.70 3.70 7 -4 -10 0.20 2.30 7 4 -10 2.40 2.70 7 4 -10 3.60 2.50 7 -5 -10 22.30 4.40 7 5 -10 25.80 5.20 7 5 -10 19.80 4.20 7 -6 -10 -0.40 2.50 7 6 -10 5.00 3.00 7 6 -10 -1.50 2.70 8 0 -10 184.78 9.10 8 0 -10 154.38 8.70 8 -1 -10 37.70 5.20 8 -1 -10 32.00 4.90 8 1 -10 22.50 4.30 8 1 -10 45.50 5.50 8 -2 -10 2.40 2.40 8 2 -10 6.80 3.30 8 2 -10 9.60 2.90 8 -3 -10 13.10 3.50 8 3 -10 20.30 4.10 8 3 -10 21.60 4.50 8 -4 -10 16.10 3.90 8 4 -10 8.20 3.50 8 4 -10 21.30 4.40 8 5 -10 9.60 3.80 9 0 -10 220.38 10.90 9 0 -10 214.78 10.10 9 -1 -10 82.59 7.70 9 -1 -10 83.59 7.40 9 1 -10 85.89 8.10 9 1 -10 83.79 6.50 9 -2 -10 -1.90 2.30 9 -2 -10 1.70 2.70 9 2 -10 3.20 2.50 9 2 -10 4.70 3.10 0 0 -11 -0.50 1.60 0 1 -11 4.80 2.20 0 -1 -11 6.50 2.40 0 -2 -11 1.40 1.90 0 2 -11 -0.70 1.70 0 -3 -11 18.30 3.30 0 3 -11 18.30 3.70 0 -4 -11 4.20 2.20 0 4 -11 2.50 2.40 0 5 -11 15.30 3.70 0 -5 -11 13.00 3.20 0 6 -11 -0.30 2.50 0 -6 -11 1.00 2.00 0 -7 -11 1.90 2.40 0 7 -11 6.00 3.30 0 8 -11 1.70 3.00 1 0 -11 36.70 4.50 -1 0 -11 46.90 5.00 1 -1 -11 139.69 7.30 -1 1 -11 132.29 7.20 -1 -1 -11 135.19 7.00 1 1 -11 138.89 7.50 1 -2 -11 2.90 2.00 -1 2 -11 1.90 2.10 1 2 -11 5.30 2.20 -1 -2 -11 3.50 1.90 -1 3 -11 114.69 7.30 1 -3 -11 109.09 6.70 -1 -3 -11 108.29 6.30 1 3 -11 124.39 7.40 -1 4 -11 690.13 20.00 1 -4 -11 685.33 19.00 -1 -4 -11 739.73 19.00 1 4 -11 690.53 20.10 1 -5 -11 119.09 7.30 -1 5 -11 117.79 7.80 1 5 -11 121.79 7.90 -1 -5 -11 113.79 6.80 1 -6 -11 2.30 2.40 -1 6 -11 2.70 2.60 1 6 -11 -1.90 2.30 1 -7 -11 38.60 5.10 -1 7 -11 42.10 5.90 1 7 -11 50.69 6.70 -1 8 -11 20.40 5.10 1 -8 -11 19.20 4.00 1 8 -11 27.90 5.30 -2 0 -11 -1.40 1.60 2 0 -11 -0.30 1.80 2 -1 -11 29.90 4.20 -2 1 -11 32.30 4.30 2 1 -11 24.80 3.90 -2 -1 -11 25.70 3.80 2 -2 -11 4.60 2.20 -2 2 -11 7.20 2.60 2 2 -11 3.20 2.20 -2 -2 -11 6.60 2.30 -2 3 -11 11.50 3.10 2 -3 -11 5.10 2.30 -2 -3 -11 7.80 3.80 2 3 -11 11.30 2.90 -2 4 -11 8.50 3.10 2 -4 -11 11.40 3.00 2 4 -11 10.30 3.10 2 -5 -11 -1.10 1.80 -2 5 -11 5.00 2.70 2 5 -11 -0.30 2.20 -2 6 -11 -0.80 2.40 2 -6 -11 -0.40 1.90 2 6 -11 0.20 2.50 2 -7 -11 12.10 3.20 -2 7 -11 7.10 3.60 2 7 -11 20.10 4.70 3 0 -11 312.77 11.70 -3 0 -11 309.87 11.10 3 -1 -11 189.08 8.90 -3 1 -11 183.08 8.50 3 1 -11 199.78 9.10 3 -2 -11 1.40 2.10 -3 2 -11 4.70 2.30 3 2 -11 3.60 2.20 3 -3 -11 12.60 3.00 -3 3 -11 15.70 3.50 3 3 -11 13.00 3.30 -3 4 -11 3.50 2.50 3 -4 -11 4.40 2.20 3 4 -11 1.20 2.30 -3 5 -11 11.30 3.30 3 -5 -11 13.20 3.40 3 5 -11 6.50 3.00 3 -6 -11 -0.20 2.40 -3 6 -11 0.40 2.50 3 6 -11 4.70 3.00 3 -7 -11 73.89 7.10 -3 7 -11 69.29 8.10 3 7 -11 78.99 8.50 3 7 -11 65.19 7.60 4 0 -11 62.09 6.00 4 -1 -11 18.20 3.60 4 1 -11 18.60 3.60 4 -2 -11 0.10 2.00 4 2 -11 0.70 2.20 4 -3 -11 0.60 1.90 -4 3 -11 -1.80 2.00 4 3 -11 2.20 2.20 4 -4 -11 5.80 2.70 -4 4 -11 5.60 2.60 4 4 -11 8.40 3.00 4 -5 -11 6.30 2.90 -4 5 -11 2.20 2.60 4 5 -11 -2.20 3.10 4 5 -11 3.90 2.70 4 -6 -11 15.40 4.00 -4 6 -11 10.40 3.70 4 6 -11 15.50 4.10 4 6 -11 14.10 4.30 4 -7 -11 3.90 2.90 -4 7 -11 2.60 3.10 4 7 -11 4.40 3.60 4 7 -11 6.40 3.50 5 0 -11 3.50 2.30 5 -1 -11 42.20 5.20 5 1 -11 52.99 5.70 5 -2 -11 3.90 2.50 5 2 -11 5.00 2.40 5 -3 -11 2.90 2.30 5 3 -11 5.20 2.40 5 -4 -11 178.68 9.40 5 4 -11 174.28 11.70 5 4 -11 177.88 9.50 5 -5 -11 -2.60 1.90 5 5 -11 4.00 2.70 5 5 -11 0.20 2.30 5 -6 -11 13.60 3.70 -5 6 -11 13.20 4.20 5 6 -11 10.80 4.20 5 6 -11 8.60 3.40 6 0 -11 39.90 5.00 6 -1 -11 21.70 4.10 6 1 -11 23.30 4.00 6 -2 -11 97.89 7.00 6 2 -11 94.89 6.90 6 -3 -11 30.20 4.60 6 3 -11 40.10 6.40 6 3 -11 23.90 4.30 6 -4 -11 3.40 2.70 6 4 -11 8.60 3.50 6 4 -11 7.30 3.20 6 -5 -11 24.00 4.40 6 5 -11 36.90 5.50 6 5 -11 26.90 5.40 7 0 -11 31.40 4.70 7 -1 -11 67.89 6.90 7 1 -11 58.59 6.30 7 -2 -11 3.60 2.90 7 2 -11 -0.80 2.60 7 2 -11 1.30 2.40 7 -3 -11 111.99 7.60 7 3 -11 106.39 7.50 7 3 -11 120.09 8.20 7 -4 -11 37.80 5.50 7 4 -11 27.50 4.90 7 4 -11 37.60 6.20 8 0 -11 85.19 7.80 8 -1 -11 0.20 2.50 8 1 -11 4.70 4.00 8 1 -11 2.50 2.50 8 -2 -11 -0.60 2.20 8 2 -11 0.40 3.00 8 2 -11 -1.70 2.20 0 0 -12 46.40 5.50 0 1 -12 -0.40 1.90 0 -1 -12 0.80 1.90 0 -2 -12 247.38 10.30 0 2 -12 242.28 10.80 0 -3 -12 0.40 2.00 0 3 -12 1.10 2.30 0 -4 -12 167.88 8.60 0 4 -12 176.28 9.70 0 5 -12 1.10 2.70 0 -5 -12 0.00 2.10 0 -6 -12 181.28 9.20 0 6 -12 188.78 10.70 1 0 -12 119.29 7.30 -1 0 -12 120.09 7.20 -1 1 -12 1.60 2.20 1 -1 -12 0.70 2.10 -1 -1 -12 0.60 2.00 1 1 -12 3.20 2.30 1 -2 -12 2.70 2.20 -1 2 -12 0.30 2.30 -1 -2 -12 3.70 2.20 1 2 -12 0.90 2.10 -1 3 -12 158.88 8.90 1 -3 -12 169.18 8.60 -1 -3 -12 161.08 8.10 1 3 -12 150.28 8.70 1 -4 -12 85.69 7.30 -1 4 -12 76.99 7.50 1 4 -12 82.69 7.70 -1 -4 -12 73.29 6.50 -1 5 -12 236.38 11.50 1 -5 -12 215.18 10.10 1 5 -12 213.28 11.00 -1 6 -12 10.50 3.70 1 -6 -12 5.60 2.90 1 6 -12 12.10 4.20 -2 0 -12 115.29 7.00 2 0 -12 104.59 7.00 -2 1 -12 26.20 4.20 2 1 -12 35.50 4.70 -2 -1 -12 35.20 4.60 2 -2 -12 3.10 2.40 -2 2 -12 -0.80 2.20 2 2 -12 -1.40 1.80 -2 3 -12 1.60 2.20 2 -3 -12 1.30 2.10 2 3 -12 -2.40 1.90 2 -4 -12 -3.20 1.70 -2 4 -12 1.50 2.30 2 4 -12 1.10 2.30 -2 5 -12 -1.10 2.20 2 -5 -12 3.40 2.60 2 5 -12 0.50 2.40 -2 6 -12 -0.10 3.00 2 -6 -12 -1.20 2.20 2 6 -12 3.50 3.00 3 0 -12 23.10 4.10 -3 1 -12 7.50 3.20 3 -1 -12 11.70 3.20 3 1 -12 6.30 2.70 3 -2 -12 40.80 5.10 -3 2 -12 51.09 5.80 3 2 -12 34.70 4.80 -3 3 -12 6.10 3.20 3 -3 -12 9.30 3.20 3 3 -12 5.00 2.70 -3 4 -12 5.20 3.00 3 -4 -12 11.20 3.30 3 4 -12 10.40 3.40 3 -5 -12 2.90 2.40 -3 5 -12 1.80 2.70 3 5 -12 6.70 3.20 3 -6 -12 27.60 4.70 -3 6 -12 27.50 5.00 3 6 -12 26.90 5.10 4 0 -12 4.50 2.60 4 -1 -12 10.90 3.20 4 1 -12 16.10 3.60 4 -2 -12 -2.50 1.90 4 2 -12 5.10 2.50 4 -3 -12 1.00 2.50 4 3 -12 2.60 2.50 4 -4 -12 13.10 3.30 -4 4 -12 9.90 4.60 4 4 -12 16.70 3.90 -4 5 -12 10.40 3.60 4 -5 -12 15.50 3.80 4 5 -12 12.60 4.10 5 0 -12 148.69 8.60 5 -1 -12 -1.10 2.00 5 1 -12 2.60 2.30 5 -2 -12 11.30 3.50 5 2 -12 7.60 2.90 5 -3 -12 52.89 6.20 5 3 -12 43.50 5.60 5 -4 -12 115.29 7.90 5 4 -12 104.09 7.80 6 0 -12 29.50 4.70 6 -1 -12 9.60 3.30 6 1 -12 22.70 4.30 6 -2 -12 36.20 5.30 6 2 -12 20.10 4.30 6 -3 -12 3.40 2.60 6 3 -12 1.30 2.30 0 0 -13 -3.70 1.80 0 1 -13 13.80 3.50 0 -1 -13 11.50 3.30 0 -2 -13 -3.80 1.80 0 2 -13 -1.30 2.20 0 3 -13 58.99 6.90 0 -3 -13 59.99 6.40 0 -4 -13 -0.80 2.10 0 4 -13 -1.10 2.40 -1 0 -13 8.70 2.80 -1 1 -13 9.40 3.10 1 -1 -13 2.80 2.50 1 1 -13 6.20 2.90 -1 -1 -13 7.80 3.10 1 -2 -13 19.50 4.00 -1 2 -13 15.10 3.80 -1 -2 -13 24.40 4.10 1 2 -13 20.50 4.30 1 -3 -13 45.00 5.70 -1 3 -13 42.30 5.90 -1 -3 -13 46.60 5.50 1 3 -13 36.10 5.60 1 -4 -13 42.90 5.70 -1 4 -13 41.50 5.90 1 4 -13 46.20 6.20 2 0 -13 4.20 2.40 -2 0 -13 3.80 2.60 -2 1 -13 24.60 4.40 2 -1 -13 26.50 4.60 2 1 -13 23.30 4.20 2 -2 -13 4.80 3.00 -2 2 -13 3.20 2.80 2 2 -13 1.20 2.50 2 -3 -13 32.20 5.00 -2 3 -13 21.40 4.30 2 3 -13 32.70 5.50 2 -4 -13 65.29 6.90 -2 4 -13 46.30 6.10 2 4 -13 45.00 6.30 3 0 -13 28.70 4.70 3 -1 -13 3.30 2.40 3 1 -13 3.30 2.40 3 -2 -13 13.80 3.70 3 2 -13 15.20 3.80 3 -3 -13 11.30 3.60 -3 3 -13 11.80 3.70 3 3 -13 8.40 3.20 4 0 -13 103.49 7.60 4 -1 -13 113.59 8.00 4 1 -13 106.59 7.80 4 -2 -13 72.99 7.10 4 2 -13 81.99 7.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 80984 _shelx_res_file ; TITL orthF_a.res in Pnma 1.res created by SHELXL-2018/3 at 10:20:20 on 14-Sep-2022 REM Old TITL orthF in Pnma REM SHELXT solution in Pnma REM R1 0.121, Rweak 0.002, Alpha 0.012, Orientation as input REM Formula found by SHELXT: C8 B F4 O CELL 0.71073 9.7906 9.6859 9.8673 90 90 90 ZERR 4 0.0005 0.0005 0.0005 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H B F O UNIT 32 44 4 16 4 L.S. 10 PLAN 5 TEMP -173.15 CONF BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.039800 0.360900 FVAR 1.02614 F1 4 0.360369 0.250000 0.454292 10.50000 0.01538 0.04766 = 0.03035 0.00000 0.00161 0.00000 F2 4 0.152096 0.250000 0.356557 10.50000 0.02819 0.03012 = 0.02436 0.00000 -0.00896 0.00000 F3 4 0.185154 0.367599 0.552501 11.00000 0.04066 0.01944 = 0.03185 -0.00958 0.01217 -0.00392 O1 5 0.485508 0.250000 0.722544 10.50000 0.01655 0.01451 = 0.01579 0.00000 0.00016 0.00000 C1 1 0.818971 0.250000 0.449891 10.50000 0.02007 0.03514 = 0.02296 0.00000 0.00564 0.00000 C2 1 0.702016 0.250000 0.546824 10.50000 0.01457 0.02464 = 0.01369 0.00000 -0.00193 0.00000 C3 1 0.644819 0.373718 0.592782 11.00000 0.01839 0.01862 = 0.01651 0.00141 -0.00179 -0.00348 AFIX 43 H3 2 0.681194 0.459536 0.563280 11.00000 0.02239 0.02389 = 0.01983 -0.00233 0.00149 0.00309 AFIX 0 C4 1 0.536714 0.371103 0.680040 11.00000 0.01866 0.01458 = 0.01478 0.00037 -0.00377 -0.00126 C5 1 0.463531 0.491828 0.736353 11.00000 0.02433 0.01595 = 0.02177 -0.00172 -0.00050 0.00206 AFIX 137 H5A 2 0.367463 0.488407 0.708666 11.00000 -1.50000 H5B 2 0.505327 0.576926 0.702199 11.00000 -1.50000 H5C 2 0.469335 0.490109 0.835489 11.00000 0.05952 0.01753 = 0.02301 -0.00521 -0.01001 0.01126 AFIX 0 B1 3 0.220130 0.250000 0.478689 10.50000 0.01569 0.01511 = 0.01695 0.00000 0.00142 0.00000 H1A 2 0.786295 0.250000 0.360106 10.50000 0.04956 H1B 2 0.871739 0.169864 0.460379 11.00000 0.06236 HKLF 4 REM orthF_a.res in Pnma REM wR2 = 0.0896, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0354 for 1236 Fo > 4sig(Fo) and 0.0417 for all 1424 data REM 93 parameters refined using 0 restraints END WGHT 0.0398 0.3608 REM Highest difference peak 0.385, deepest hole -0.246, 1-sigma level 0.044 Q1 1 0.5068 0.4329 0.7099 11.00000 0.05 0.39 Q2 1 0.5824 0.3658 0.6240 11.00000 0.05 0.35 Q3 1 0.6667 0.1877 0.5573 11.00000 0.05 0.32 Q4 1 0.7581 0.2500 0.5023 10.50000 0.05 0.29 Q5 1 0.9040 0.2320 0.4884 11.00000 0.05 0.22 ; _shelx_res_checksum 53310 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 0.36037(9) 0.250000 0.45429(10) 0.0311(2) Uani d 1 . . F F2 0.15210(10) 0.250000 0.35656(9) 0.0276(2) Uani d 1 . . F F3 0.18515(8) 0.36760(7) 0.55250(7) 0.03065(19) Uani d 1 . . O O1 0.48551(10) 0.250000 0.72254(9) 0.0156(2) Uani d 1 . . C C1 0.81897(17) 0.250000 0.44989(17) 0.0261(3) Uani d 1 . . C C2 0.70202(14) 0.250000 0.54682(13) 0.0176(3) Uani d 1 . . C C3 0.64482(10) 0.37372(10) 0.59278(10) 0.0178(2) Uani d 1 . . H H3 0.681194 0.459536 0.563280 0.022(3) Uani calc 1 . . C C4 0.53671(10) 0.37110(9) 0.68004(9) 0.0160(2) Uani d 1 . . C C5 0.46353(11) 0.49183(10) 0.73635(11) 0.0207(2) Uani d 1 . . H H5A 0.367463 0.488407 0.708666 0.031 Uiso calc 1 . . H H5B 0.505327 0.576926 0.702199 0.031 Uiso calc 1 . . H H5C 0.469335 0.490109 0.835489 0.033(4) Uani calc 1 . . B B1 0.22013(15) 0.250000 0.47869(16) 0.0159(3) Uani d 1 . . H H1A 0.786(2) 0.250000 0.360(3) 0.050(7) Uiso d 1 . . H H1B 0.872(2) 0.1699(19) 0.4604(19) 0.062(5) 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 0.0154(4) 0.0477(6) 0.0303(5) 0.000 0.0016(4) 0.000 F2 0.0282(5) 0.0301(5) 0.0244(5) 0.000 -0.0090(4) 0.000 F3 0.0407(4) 0.0194(3) 0.0318(4) -0.0039(3) 0.0122(3) -0.0096(3) O1 0.0165(5) 0.0145(4) 0.0158(5) 0.000 0.0002(4) 0.000 C1 0.0201(7) 0.0351(8) 0.0230(8) 0.000 0.0056(6) 0.000 C2 0.0146(6) 0.0246(7) 0.0137(6) 0.000 -0.0019(5) 0.000 C3 0.0184(5) 0.0186(4) 0.0165(4) -0.0035(4) -0.0018(4) 0.0014(4) H3 0.022(8) 0.024(8) 0.020(7) 0.003(6) 0.001(6) -0.002(7) C4 0.0187(5) 0.0146(4) 0.0148(4) -0.0013(3) -0.0038(3) 0.0004(3) C5 0.0243(5) 0.0159(4) 0.0218(5) 0.0021(4) -0.0005(4) -0.0017(4) H5C 0.060(11) 0.018(8) 0.023(8) 0.011(8) -0.010(8) -0.005(7) B1 0.0157(7) 0.0151(6) 0.0169(7) 0.000 0.0014(5) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C4 O1 C4 . 7_565 121.74(11) ? C2 C1 H1A . . 110.0(15) ? C2 C1 H1B . 7_565 110.6(12) ? C2 C1 H1B . . 110.6(12) ? H1A C1 H1B . 7_565 106.9(14) ? H1A C1 H1B . . 106.9(14) ? H1B C1 H1B . 7_565 112(2) ? C3 C2 C1 7_565 . 121.02(6) ? C3 C2 C1 . . 121.02(6) ? C3 C2 C3 7_565 . 117.96(13) ? C2 C3 H3 . . 120.0 ? C4 C3 C2 . . 119.96(10) ? C4 C3 H3 . . 120.0 ? O1 C4 C3 . . 120.19(9) ? O1 C4 C5 . . 113.09(8) ? C3 C4 C5 . . 126.71(9) ? C4 C5 H5A . . 109.5 ? C4 C5 H5B . . 109.5 ? C4 C5 H5C . . 109.5 ? H5A C5 H5B . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? F1 B1 F3 . . 109.39(8) ? F1 B1 F3 . 7_565 109.39(8) ? F2 B1 F1 . . 108.99(12) ? F2 B1 F3 . 7_565 109.77(8) ? F2 B1 F3 . . 109.77(8) ? F3 B1 F3 7_565 . 109.51(12) ? 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 B1 . 1.3940(17) ? F2 B1 . 1.3769(18) ? F3 B1 . 1.3947(11) ? O1 C4 7_565 1.3428(10) ? O1 C4 . 1.3428(10) ? C1 C2 . 1.492(2) ? C1 H1A . 0.94(2) ? C1 H1B . 0.938(19) ? C1 H1B 7_565 0.938(19) ? C2 C3 7_565 1.3983(12) ? C2 C3 . 1.3983(12) ? C3 H3 . 0.9500 ? C3 C4 . 1.3646(14) ? C4 C5 . 1.4797(14) ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? 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 C1 C2 C3 C4 . . . . 179.13(12) ? C2 C3 C4 O1 . . . . 0.37(15) ? C2 C3 C4 C5 . . . . -179.06(10) ? C3 C2 C3 C4 7_565 . . . 0.15(19) ? C4 O1 C4 C3 7_565 . . . -0.91(17) ? C4 O1 C4 C5 7_565 . . . 178.59(7) ? _cod_database_fobs_code 2022689