Structures and properties of the mono- and diprotonated species of acetylenedicarbonyl fluoride
Hollenwäger, Dirk; Nitzer, Alexander; Leitz, Dominik; Kornath, Andreas J.; New Journal of Chemistry 48 (2024) 20140–20148; doi:10.1039/D4NJ04175E

data_7063548
_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)
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_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 \k-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w 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
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_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
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_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
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_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
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_refine_ls_matrix_type           full
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_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/[\s^2^(Fo^2^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
;
_shelx_res_checksum              73093