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#$Date: 2024-10-06 03:22:45 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295080 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249437.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7249437
loop_
_publ_author_name
'Virmani, Alan'
'Jessen, Christoph'
'Nitzer, Alexander'
'Kornath, Andreas J.'
_publ_section_title
;
 Deoxyfluorination with superacids -- synthesis and characterization of
 protonated α-fluorohydroxyacetic acid
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              31517
_journal_page_last               31523
_journal_paper_doi               10.1039/D4RA05449K
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration RS
_chemical_formula_moiety         'As F6, C2 H4 F O3'
_chemical_formula_sum            'C2 H4 As F7 O3'
_chemical_formula_weight         283.97
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2019-10-23
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-05-19 deposited with the CCDC.	2024-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4858(3)
_cell_length_b                   8.0027(3)
_cell_length_c                   12.7743(5)
_cell_measurement_reflns_used    2404
_cell_measurement_temperature    121(2)
_cell_measurement_theta_max      31.5680
_cell_measurement_theta_min      2.9920
_cell_volume                     765.27(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      121(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8259
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.238
_diffrn_reflns_theta_min         3.004
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.497(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_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/[σ²(Fo²)+(0.0248P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2257
_reflns_number_total             2544
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra05449k2.cif
_cod_data_source_block           shelx
_cod_database_code               7249437
_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_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.549
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
As1 As 0.69693(5) 0.45388(5) 0.19175(3) 0.01405(9) Uani 1 1 d . . . . .
F3 F 0.5630(3) 0.6078(3) 0.1386(2) 0.0256(6) Uani 1 1 d . . . . .
F4 F 0.5753(3) 0.4579(3) 0.30439(18) 0.0250(5) Uani 1 1 d . . . . .
F7 F 0.8276(3) 0.4582(3) 0.08139(16) 0.0223(5) Uani 1 1 d . . . . .
F1 F 0.6530(4) 0.9920(3) 0.5570(2) 0.0385(9) Uani 1 1 d . . . . .
F6 F 0.8372(4) 0.3047(3) 0.2446(2) 0.0244(6) Uani 1 1 d . . . . .
F5 F 0.5634(4) 0.3029(3) 0.1407(2) 0.0262(6) Uani 1 1 d . . . . .
F2 F 0.8351(4) 0.6101(3) 0.2439(2) 0.0246(6) Uani 1 1 d . . . . .
O2 O 0.8062(5) 0.9920(3) 0.3150(2) 0.0168(5) Uani 1 1 d D . . . .
O1 O 0.8136(5) 0.7722(3) 0.4179(2) 0.0226(6) Uani 1 1 d D . . . .
O3 O 0.8037(6) 1.1961(4) 0.4720(2) 0.0338(7) Uani 1 1 d D . . . .
C2 C 0.8065(6) 1.0347(6) 0.5042(3) 0.0239(8) Uani 1 1 d . . . . .
C1 C 0.8093(6) 0.9282(5) 0.4062(3) 0.0170(7) Uani 1 1 d . . . . .
H2 H 0.804(8) 1.0947(17) 0.312(4) 0.028(12) Uiso 1 1 d D . . . .
H3 H 0.849(7) 1.255(5) 0.516(3) 0.034(16) Uiso 1 1 d D . . . .
H1 H 0.819(8) 0.721(5) 0.363(2) 0.034(14) Uiso 1 1 d D . . . .
H4 H 0.898(6) 1.015(5) 0.551(3) 0.015(12) Uiso 1 1 d . . . . .
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'
O O 0.0106 0.0060 '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'
As As 0.0499 2.0058 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F5 As1 F4 91.34(12) . . ?
F5 As1 F7 91.96(12) . . ?
F4 As1 F7 176.70(12) . . ?
F5 As1 F3 90.84(12) . . ?
F4 As1 F3 90.46(12) . . ?
F7 As1 F3 89.64(12) . . ?
F5 As1 F6 90.93(13) . . ?
F4 As1 F6 90.47(12) . . ?
F7 As1 F6 89.34(12) . . ?
F3 As1 F6 177.98(13) . . ?
F5 As1 F2 179.72(14) . . ?
F4 As1 F2 88.92(12) . . ?
F7 As1 F2 87.79(12) . . ?
F3 As1 F2 89.03(13) . . ?
F6 As1 F2 89.19(11) . . ?
O3 C2 F1 111.9(4) . . ?
O3 C2 C1 106.6(3) . . ?
F1 C2 C1 106.1(4) . . ?
O1 C1 O2 120.6(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 122.0(3) . . ?
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
As1 F5 1.698(3) . ?
As1 F4 1.703(2) . ?
As1 F7 1.716(2) . ?
As1 F3 1.727(2) . ?
As1 F6 1.727(2) . ?
As1 F2 1.754(2) . ?
F1 C2 1.376(5) . ?
O2 C1 1.272(4) . ?
O1 C1 1.258(4) . ?
O3 C2 1.355(5) . ?
C2 C1 1.515(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 F6 0.823(13) 1.91(3) 2.669(3) 154(5) 1_565 yes
O3 H3 F3 0.811(13) 2.020(16) 2.826(4) 172(5) 2_675 yes
O1 H1 F2 0.816(13) 1.763(14) 2.579(4) 179(6) . yes
C2 H4 F4 0.92(4) 2.28(4) 3.167(5) 160(3) 4_566 yes
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
O3 C2 C1 O1 179.5(4) . . . . ?
F1 C2 C1 O1 -61.2(5) . . . . ?
O3 C2 C1 O2 -1.0(6) . . . . ?
F1 C2 C1 O2 118.3(4) . . . . ?
