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#$Date: 2023-11-18 01:58:18 +0200 (Sat, 18 Nov 2023) $
#$Revision: 287680 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/44/7714498.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_7714498
loop_
_publ_author_name
'Saal, Thomas'
'Haiges, Ralf'
'Christe, Karl O.'
_publ_section_title
;
 Synthesis and characterization of trifluoromethylcarboxonium salts.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02944a
_journal_year                    2023
_chemical_formula_moiety         'C2 H3 F3 N O, F6 Sb'
_chemical_formula_sum            'C2 H3 F9 N O Sb'
_chemical_formula_weight         349.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.205(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4747(12)
_cell_length_b                   10.4829(11)
_cell_length_c                   13.1367(13)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.0130
_cell_measurement_theta_min      4.1793
_cell_volume                     1575.9(3)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18920
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    3.635
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.316
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.783
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0133
_refine_ls_R_factor_gt           0.0127
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0130P)²+1.6814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0324
_reflns_number_gt                2356
_reflns_number_total             2403
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02944a2.cif
_cod_data_source_block           I
_cod_database_code               7714498
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb1 0.53971(2) 0.73531(2) 0.53965(2) 0.00743(3) Uani d . . . 1 . .
H H1 0.6293(19) 0.574(2) 0.3247(18) 0.024(6) Uiso d . . . 1 . .
N N1 0.75128(11) 0.52036(12) 0.14654(9) 0.0114(2) Uani d . . . 1 . .
O O1 0.63992(9) 0.58244(10) 0.26967(8) 0.01200(18) Uani d . . . 1 . .
C C1 0.78555(11) 0.41494(13) 0.31108(10) 0.0104(2) Uani d . . . 1 . .
F F1 0.80320(8) 0.46420(9) 0.40409(6) 0.01733(18) Uani d . . . 1 . .
C C2 0.72232(11) 0.51255(12) 0.23894(10) 0.0093(2) Uani d . . . 1 . .
H H2 0.8028(19) 0.475(2) 0.1292(17) 0.025(6) Uiso d . . . 1 . .
F F2 0.71922(8) 0.31153(8) 0.31680(7) 0.01550(17) Uani d . . . 1 . .
F F3 0.88644(8) 0.38185(10) 0.27667(7) 0.01838(18) Uani d . . . 1 . .
H H3 0.7161(18) 0.572(2) 0.1091(16) 0.020(5) Uiso d . . . 1 . .
F F5 0.57568(8) 0.85227(9) 0.43796(7) 0.01536(17) Uani d . . . 1 . .
F F4 0.50814(8) 0.61198(8) 0.63692(6) 0.01383(16) Uani d . . . 1 . .
F F6 0.68690(8) 0.76237(8) 0.60781(7) 0.01509(17) Uani d . . . 1 . .
F F9 0.47277(8) 0.86451(9) 0.61389(7) 0.01809(18) Uani d . . . 1 . .
F F8 0.39390(8) 0.70219(9) 0.46829(7) 0.01624(17) Uani d . . . 1 . .
F F7 0.60482(8) 0.60287(9) 0.46226(7) 0.01504(17) Uani d . . . 1 . .
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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F9 Sb1 F4 . . 92.11(4) ?
F9 Sb1 F6 . . 91.80(4) ?
F4 Sb1 F6 . . 89.49(4) ?
F9 Sb1 F5 . . 91.04(4) ?
F4 Sb1 F5 . . 176.85(4) ?
F6 Sb1 F5 . . 90.21(4) ?
F9 Sb1 F8 . . 90.53(4) ?
F4 Sb1 F8 . . 90.18(4) ?
F6 Sb1 F8 . . 177.66(4) ?
F5 Sb1 F8 . . 89.99(4) ?
F9 Sb1 F7 . . 178.75(4) ?
F4 Sb1 F7 . . 87.94(4) ?
F6 Sb1 F7 . . 89.45(4) ?
F5 Sb1 F7 . . 88.91(4) ?
F8 Sb1 F7 . . 88.22(4) ?
C2 N1 H2 . . 118.5(16) ?
C2 N1 H3 . . 117.5(15) ?
H2 N1 H3 . . 124.(2) ?
C2 O1 H1 . . 114.6(18) ?
F3 C1 F1 . . 109.80(11) ?
F3 C1 F2 . . 108.98(11) ?
F1 C1 F2 . . 108.31(11) ?
F3 C1 C2 . . 110.46(11) ?
F1 C1 C2 . . 109.94(11) ?
F2 C1 C2 . . 109.31(11) ?
O1 C2 N1 . . 120.54(13) ?
O1 C2 C1 . . 120.68(12) ?
N1 C2 C1 . . 118.76(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sb1 F9 . 1.8670(9) ?
Sb1 F4 . 1.8717(8) ?
Sb1 F6 . 1.8743(9) ?
Sb1 F5 . 1.8812(9) ?
Sb1 F8 . 1.8892(9) ?
Sb1 F7 . 1.9054(9) ?
N1 C2 . 1.2844(17) ?
N1 H2 . 0.80(2) ?
N1 H3 . 0.81(2) ?
O1 C2 . 1.2844(16) ?
O1 H1 . 0.75(2) ?
C1 F3 . 1.3197(15) ?
C1 F1 . 1.3283(15) ?
C1 F2 . 1.3298(16) ?
C1 C2 . 1.5397(18) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
F3 C1 C2 O1 . . . . -161.41(12) ?
F1 C1 C2 O1 . . . . -40.07(17) ?
F2 C1 C2 O1 . . . . 78.69(15) ?
F3 C1 C2 N1 . . . . 20.50(17) ?
F1 C1 C2 N1 . . . . 141.83(13) ?
F2 C1 C2 N1 . . . . -99.40(14) ?
