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#$Date: 2025-01-06 15:40:29 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297129 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/35/7063549.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_7063549
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         'F11 Sb2, 0.5 (C4 H2 F2 O2), F H'
_chemical_formula_sum            'C2 H2 F13 O Sb2'
_chemical_formula_weight         532.54
_chemical_name_common            '[C4(OH)2F2][Sb2F11]'
_chemical_name_systematic        'diprotonated 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             2021-01-13
_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                94.096(7)
_cell_angle_beta                 91.767(5)
_cell_angle_gamma                114.341(9)
_cell_formula_units_Z            2
_cell_length_a                   7.4703(6)
_cell_length_b                   8.0314(10)
_cell_length_c                   9.7471(5)
_cell_measurement_reflns_used    2292
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      32.2590
_cell_measurement_theta_min      2.8010
_cell_volume                     530.28(9)
_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      98(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.907
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5735
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.239
_diffrn_reflns_theta_min         2.796
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77134
_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    3.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             482
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HF'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.450
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0168P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2830
_reflns_number_total             3414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj04175e3.cif
_cod_data_source_block           xi002
_cod_depositor_comments
'Adding full bibliography for 7063547--7063549.cif.'
_cod_database_code               7063549
_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   0.481
_shelx_estimated_absorpt_t_max   0.716
_oxdiff_exptl_absorpt_empirical_full_min 0.829
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_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 0.34032(4) 0.43267(3) 0.74796(3) 0.01132(7) Uani 1 1 d . . . . .
Sb2 Sb 0.91279(4) 0.78499(3) 0.77140(3) 0.01275(7) Uani 1 1 d . . . . .
F7 F 0.4479(4) 0.3056(3) 0.6355(3) 0.0215(5) Uani 1 1 d . . . . .
F13 F 0.6200(3) 0.6215(3) 0.7822(3) 0.0257(6) Uani 1 1 d . . . . .
F10 F 0.8551(3) 0.9580(3) 0.8769(3) 0.0189(5) Uani 1 1 d . . . . .
F6 F 0.3957(4) 0.3245(3) 0.8965(3) 0.0206(5) Uani 1 1 d . . . . .
F1 F 0.2348(4) 0.7085(3) 0.1398(3) 0.0225(5) Uani 1 1 d . . . . .
F4 F 0.2817(4) 0.5952(3) 0.8611(3) 0.0229(6) Uani 1 1 d . . . . .
F12 F 0.9462(4) 0.6883(3) 0.9318(3) 0.0227(5) Uani 1 1 d . . . . .
F11 F 0.9219(4) 0.5861(3) 0.6675(3) 0.0250(6) Uani 1 1 d . . . . .
F2 F 0.2610(4) 0.7974(4) 0.4808(3) 0.0265(6) Uani 1 1 d D . . . .
F5 F 0.3308(4) 0.5635(4) 0.5969(3) 0.0254(6) Uani 1 1 d . . . . .
F8 F 1.1776(3) 0.9352(4) 0.7643(3) 0.0255(6) Uani 1 1 d . . . . .
F3 F 0.0823(3) 0.2638(3) 0.7128(3) 0.0231(6) Uani 1 1 d . . . . .
F9 F 0.8309(4) 0.8585(4) 0.6139(3) 0.0256(6) Uani 1 1 d . . . . .
O1 O 0.4124(5) 0.9476(4) 0.2823(3) 0.0208(6) Uani 1 1 d D . . . .
C2 C 0.4609(6) 0.9621(6) 0.0482(4) 0.0164(8) Uani 1 1 d . . . . .
C1 C 0.3672(6) 0.8727(6) 0.1646(4) 0.0170(8) Uani 1 1 d . . . . .
H2 H 0.287(8) 0.707(6) 0.523(6) 0.06(2) Uiso 1 1 d D . . . .
H1 H 0.376(14) 0.873(12) 0.359(7) 0.20(5) 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
F4 Sb1 F3 95.24(11) . . ?
F4 Sb1 F6 92.66(12) . . ?
F3 Sb1 F6 96.09(12) . . ?
F4 Sb1 F7 168.91(11) . . ?
F3 Sb1 F7 95.66(11) . . ?
F6 Sb1 F7 88.19(11) . . ?
F4 Sb1 F5 89.28(12) . . ?
F3 Sb1 F5 93.18(12) . . ?
F6 Sb1 F5 170.31(11) . . ?
F7 Sb1 F5 88.11(12) . . ?
F4 Sb1 F13 84.36(11) . . ?
F3 Sb1 F13 178.25(12) . . ?
F6 Sb1 F13 85.63(11) . . ?
F7 Sb1 F13 84.68(11) . . ?
F5 Sb1 F13 85.11(11) . . ?
F12 Sb2 F8 94.61(12) . . ?
F12 Sb2 F11 90.22(12) . . ?
F8 Sb2 F11 95.21(12) . . ?
F12 Sb2 F9 169.63(12) . . ?
F8 Sb2 F9 95.69(12) . . ?
F11 Sb2 F9 89.96(12) . . ?
F12 Sb2 F10 89.09(11) . . ?
F8 Sb2 F10 95.17(11) . . ?
F11 Sb2 F10 169.61(11) . . ?
F9 Sb2 F10 88.87(12) . . ?
F12 Sb2 F13 85.00(11) . . ?
F8 Sb2 F13 179.05(11) . . ?
F11 Sb2 F13 85.66(11) . . ?
F9 Sb2 F13 84.68(12) . . ?
F10 Sb2 F13 83.95(11) . . ?
Sb1 F13 Sb2 165.88(15) . . ?
C2 C2 C1 179.5(6) 2_675 . ?
O1 C1 F1 121.5(4) . . ?
O1 C1 C2 122.1(4) . . ?
F1 C1 C2 116.5(4) . . ?
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 F4 1.846(2) . ?
Sb1 F3 1.847(2) . ?
Sb1 F6 1.860(2) . ?
Sb1 F7 1.860(2) . ?
Sb1 F5 1.885(3) . ?
Sb1 F13 2.012(2) . ?
Sb2 F12 1.849(3) . ?
Sb2 F8 1.851(2) . ?
Sb2 F11 1.856(2) . ?
Sb2 F9 1.857(3) . ?
Sb2 F10 1.868(2) . ?
Sb2 F13 2.046(2) . ?
F1 C1 1.281(5) . ?
O1 C1 1.226(5) . ?
C2 C2 1.189(8) 2_675 ?
C2 C1 1.430(6) . ?
