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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/7/06/35/7063547.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_7063547
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 F2 o2'
_chemical_formula_sum            'C4 F2 O2'
_chemical_formula_weight         118.04
_chemical_name_common            C4O2F2
_chemical_name_systematic        'Acetylenedicarbonyl Fluoride'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-26
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.8699(2)
_cell_length_b                   5.8699(2)
_cell_length_c                   13.4589(9)
_cell_measurement_reflns_used    2136
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      29.4300
_cell_measurement_theta_min      3.7640
_cell_volume                     463.74(4)
_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      99(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.265
_diffrn_reflns_theta_min         3.787
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92759
_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    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HF'
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.8(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0352
_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)+(0.0302P)²+0.0594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.522
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                722
_reflns_number_total             805
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj04175e3.cif
_cod_data_source_block           xi006
_cod_depositor_comments
'Adding full bibliography for 7063547--7063549.cif.'
_cod_database_code               7063547
_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   0.952
_shelx_estimated_absorpt_t_max   0.978
_oxdiff_exptl_absorpt_empirical_full_min 0.922
_oxdiff_exptl_absorpt_empirical_full_max 1.119
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_file
;
TITL shelxt_a.res in P4(1)2(1)2
    shelx.res
    created by SHELXL-2018/3 at 12:24:56 on 26-Jan-2021
CELL  0.71073   5.8699   5.8699  13.4589   90.000   90.000   90.000
ZERR     4.00   0.0002   0.0002   0.0009    0.000    0.000    0.000
LATT  -1
SYMM  - X, - Y, 1/2 + Z
SYMM  1/2 - Y, 1/2 + X, 1/4 + Z
SYMM  1/2 + Y, 1/2 - X, 3/4 + Z
SYMM  1/2 - X, 1/2 + Y, 1/4 - Z
SYMM  1/2 + X, 1/2 - Y, 3/4 - Z
SYMM    Y,   X, - Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    O    F
UNIT  16 8 8
MERG   2
OMIT     0   1   2
TWIN
FMAP   2
PLAN   20
SIZE     0.120   0.185   0.269
ACTA
BOND
CONF
LIST   6
L.S.  10
TEMP  -173.95
WGHT    0.030200    0.059400
BASF   0.80051
FVAR       1.54078
F1    3   -0.832015   -0.817895   -0.240296    11.00000    0.02408    0.03360 =
         0.03522    0.00356    0.00349   -0.00592
O1    2   -0.617159   -0.962583   -0.357994    11.00000    0.03168    0.02550 =
         0.03491   -0.00884   -0.00626   -0.00286
C1    1   -0.641159   -0.828828   -0.293576    11.00000    0.02082    0.01869 =
         0.02402    0.00356   -0.00377   -0.00111
C2    1   -0.478385   -0.659286   -0.261743    11.00000    0.02176    0.02220 =
         0.01946   -0.00162   -0.00185    0.00164
HKLF    4




REM  shelxt_a.res in P4(1)2(1)2
REM wR2 = 0.0732, GooF = S = 1.088, Restrained GooF = 1.088 for all data
REM R1 = 0.0352 for 722 Fo > 4sig(Fo) and 0.0421 for all 805 data
REM 38 parameters refined using 0 restraints

END

WGHT      0.0302      0.0596

REM Highest difference peak  0.246,  deepest hole -0.133,  1-sigma level  0.038
Q1    1  -0.3434 -0.6566 -0.2500  10.50000  0.05    0.25
Q2    1  -0.5524 -0.7383 -0.2891  11.00000  0.05    0.21
Q3    1  -0.6626 -0.8452 -0.3487  11.00000  0.05    0.15
Q4    1  -0.4621 -0.5402 -0.2804  11.00000  0.05    0.14
Q5    1  -0.8596 -0.9918 -0.2337  11.00000  0.05    0.12
Q6    1  -0.5612 -0.8590 -0.3475  11.00000  0.05    0.12
Q7    1  -0.5613 -0.9290 -0.3017  11.00000  0.05    0.12
Q8    1  -0.3308 -0.7852 -0.2663  11.00000  0.05    0.12
Q9    1  -0.6655 -1.1206 -0.3463  11.00000  0.05    0.12
Q10   1  -0.6480 -0.9946 -0.3044  11.00000  0.05    0.12
Q11   1  -0.7309 -1.0233 -0.2314  11.00000  0.05    0.11
Q12   1  -0.7167 -0.8647 -0.2485  11.00000  0.05    0.11
Q13   1  -0.4916 -0.6032 -0.2392  11.00000  0.05    0.10
Q14   1  -1.1385 -0.7830 -0.2771  11.00000  0.05    0.10
Q15   1  -0.5278 -1.0189 -0.3714  11.00000  0.05    0.09
Q16   1  -0.4685 -0.9755 -0.2313  11.00000  0.05    0.09
Q17   1  -0.7061 -0.8463 -0.2249  11.00000  0.05    0.09
Q18   1  -1.0143 -0.8602 -0.2237  11.00000  0.05    0.09
Q19   1  -0.5484 -0.8816 -0.3825  11.00000  0.05    0.09
Q20   1  -0.5977 -1.0346 -0.4295  11.00000  0.05    0.09
;
_shelx_res_checksum              8403
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'
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
F1 F -0.83202(15) -0.81789(15) -0.24030(6) 0.0310(2) Uani 1 1 d . . . . .
O1 O -0.61716(19) -0.96258(19) -0.35799(8) 0.0307(3) Uani 1 1 d . . . . .
C1 C -0.6412(2) -0.8288(2) -0.29358(10) 0.0212(3) Uani 1 1 d . . . . .
C2 C -0.4784(2) -0.6593(2) -0.26174(9) 0.0211(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F1 0.0241(4) 0.0336(5) 0.0352(5) 0.0036(4) 0.0035(4) -0.0059(3)
O1 0.0317(6) 0.0255(6) 0.0349(6) -0.0088(5) -0.0063(5) -0.0029(5)
C1 0.0208(6) 0.0187(6) 0.0240(5) 0.0036(5) -0.0038(5) -0.0011(6)
C2 0.0218(6) 0.0222(6) 0.0195(5) -0.0016(5) -0.0019(5) 0.0016(5)
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'
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'
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
O1 C1 F1 121.94(13) . . ?
O1 C1 C2 126.75(14) . . ?
F1 C1 C2 111.32(12) . . ?
C2 C2 C1 177.89(16) 8_444 . ?
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
F1 C1 1.3317(16) . ?
O1 C1 1.1781(18) . ?
C1 C2 1.4446(19) . ?
C2 C2 1.186(3) 8_444 ?
