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#$Revision: 297129 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/35/7063548.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.
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data_7063548
loop_
_publ_author_name
'Hollenwäger, Dirk'
'Nitzer, Alexander'
'Leitz, Dominik'
'Kornath, Andreas J.'
_publ_section_title
;
 Structures and properties of the mono- and diprotonated species of
 acetylenedicarbonyl fluoride
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20140
_journal_page_last               20148
_journal_paper_doi               10.1039/D4NJ04175E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C4 H F2 O2, F6 Sb'
_chemical_formula_sum            'C4 H F8 O2 Sb'
_chemical_formula_weight         354.80
_chemical_name_common            '[C4(OH)OF2][SbF6]'
_chemical_name_systematic        'protonated Acetylenedicarbonyl Fluoride'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-17
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                102.824(7)
_cell_angle_beta                 104.736(8)
_cell_angle_gamma                110.992(9)
_cell_formula_units_Z            2
_cell_length_a                   7.6800(8)
_cell_length_b                   7.9588(7)
_cell_length_c                   8.2202(7)
_cell_measurement_reflns_used    2526
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      30.7470
_cell_measurement_theta_min      2.7030
_cell_volume                     425.53(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics
'ORTEP-3, Version ORTEP-III (1.0.3), L. J. Farrugia, J. Appl. Cryst. (2012),45, 849-854'
_computing_publication_material
'PLATON (A.L.Spek, Acta Cryst. 2009, D65, 148-155.) '
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7104
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.871
_diffrn_reflns_theta_min         2.732
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HF'
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.837
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2029
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0335
_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)+(0.0436P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1794
_reflns_number_total             2029
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj04175e3.cif
_cod_data_source_block           xh068
_cod_depositor_comments
'Adding full bibliography for 7063547--7063549.cif.'
_cod_original_cell_volume        425.53(7)
_cod_database_code               7063548
_shelx_shelxl_version_number     2018/3
_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   0.473
_shelx_estimated_absorpt_t_max   0.687
_oxdiff_exptl_absorpt_empirical_full_min 0.814
_oxdiff_exptl_absorpt_empirical_full_max 1.345
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Sb1 Sb 0.42995(4) 0.67493(4) 0.26612(4) 0.01905(12) Uani 1 1 d . . . . .
F3 F 0.3595(4) 0.4001(4) 0.1992(4) 0.0228(6) Uani 1 1 d D . . . .
F6 F 0.6147(4) 0.6913(4) 0.1517(4) 0.0256(6) Uani 1 1 d . . . . .
F1 F 0.8300(4) 0.4862(4) 0.3363(4) 0.0268(6) Uani 1 1 d . . . . .
F7 F 0.2327(4) 0.6149(4) 0.0466(4) 0.0274(6) Uani 1 1 d . . . . .
F8 F 0.5051(4) 0.9360(4) 0.3269(4) 0.0274(6) Uani 1 1 d . . . . .
F4 F 0.2415(4) 0.6313(4) 0.3761(4) 0.0294(6) Uani 1 1 d . . . . .
F5 F 0.6235(4) 0.7084(4) 0.4783(4) 0.0291(6) Uani 1 1 d . . . . .
F2 F 1.0438(5) -0.0994(4) 0.3617(4) 0.0350(7) Uani 1 1 d . . . . .
O1 O 0.5536(5) 0.2261(5) 0.1759(5) 0.0246(7) Uani 1 1 d D . . . .
O2 O 1.1340(6) -0.0271(6) 0.1439(5) 0.0354(9) Uani 1 1 d . . . . .
C1 C 0.7352(7) 0.3037(7) 0.2508(6) 0.0220(10) Uani 1 1 d . . . . .
C4 C 1.0513(7) -0.0102(7) 0.2441(7) 0.0261(11) Uani 1 1 d . . . . .
C3 C 0.9439(7) 0.1077(7) 0.2541(6) 0.0227(10) Uani 1 1 d . . . . .
C2 C 0.8537(7) 0.2011(7) 0.2527(6) 0.0228(10) Uani 1 1 d . . . . .
H1 H 0.504(8) 0.304(7) 0.197(8) 0.05(2) Uiso 1 1 d 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'
Sb Sb -0.5866 1.5461 '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
F8 Sb1 F4 94.69(13) . . ?
F8 Sb1 F7 93.31(13) . . ?
F4 Sb1 F7 91.11(13) . . ?
F8 Sb1 F5 92.60(13) . . ?
F4 Sb1 F5 89.39(14) . . ?
F7 Sb1 F5 174.00(12) . . ?
F8 Sb1 F6 91.44(13) . . ?
F4 Sb1 F6 173.81(12) . . ?
F7 Sb1 F6 89.37(13) . . ?
F5 Sb1 F6 89.50(13) . . ?
F8 Sb1 F3 177.78(12) . . ?
F4 Sb1 F3 87.47(12) . . ?
F7 Sb1 F3 87.13(12) . . ?
F5 Sb1 F3 86.92(12) . . ?
F6 Sb1 F3 86.39(12) . . ?
O1 C1 F1 120.6(4) . . ?
O1 C1 C2 122.9(4) . . ?
F1 C1 C2 116.4(4) . . ?
O2 C4 F2 123.1(5) . . ?
O2 C4 C3 125.1(5) . . ?
F2 C4 C3 111.7(4) . . ?
C2 C3 C4 176.5(5) . . ?
C3 C2 C1 176.5(5) . . ?
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
Sb1 F8 1.853(3) . ?
Sb1 F4 1.865(3) . ?
Sb1 F7 1.867(3) . ?
Sb1 F5 1.874(3) . ?
Sb1 F6 1.875(3) . ?
Sb1 F3 1.961(3) . ?
F1 C1 1.290(5) . ?
F2 C4 1.322(6) . ?
O1 C1 1.218(6) . ?
O2 C4 1.173(6) . ?
C1 C2 1.423(7) . ?
C4 C3 1.457(7) . ?
C3 C2 1.184(7) . ?
