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#$Date: 2020-02-14 02:38:05 +0200 (Fri, 14 Feb 2020) $
#$Revision: 248142 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557315.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_1557315
loop_
_publ_author_name
'Okamoto, Yukihiro'
'Tsuzuki, Seiji'
'Tatara, Ryoichi'
'Ueno, Kazuhide'
'Dokko, Kaoru'
'Watanabe, Masayoshi'
_publ_section_title
;
 High Transference Number of Na Ion in Liquid-State Sulfolane Solvates of
 Sodium Bis(fluorosulfonyl)amide
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.9b11458
_journal_year                    2020
_chemical_formula_sum            'C6 H12 F N0.5 Na0.5 O5 S2.5'
_chemical_formula_weight         281.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.179(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9451(5)
_cell_length_b                   11.9286(4)
_cell_length_c                   16.2807(7)
_cell_measurement_reflns_used    6037
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.3800
_cell_measurement_theta_min      3.2570
_cell_volume                     2275.79(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8455
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0392
_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)+(0.0589P)²+4.4099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2240
_reflns_number_total             2468
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp9b11458_si_002.cif
_cod_data_source_block           NaFSA_SL_1_3
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C6 H12 F N0.50 Na0.50 O5 S2.50'
_cod_database_code               1557315
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, 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
S14 S 0.750000 0.65938(6) 0.500000 0.02261(17) Uani 1 2 d S T P . .
S5 S 0.43212(5) 0.45953(5) 0.27652(3) 0.03127(17) Uani 1 1 d . . . . .
S9 S 0.33861(5) 0.76533(5) 0.45752(4) 0.03481(17) Uani 1 1 d . . . . .
Na13 Na 0.500000 0.500000 0.500000 0.0272(3) Uani 1 2 d S . P . .
O15 O 0.65345(14) 0.59641(14) 0.45608(10) 0.0361(4) Uani 1 1 d . . . . .
O6 O 0.41573(16) 0.47092(17) 0.36126(10) 0.0440(4) Uani 1 1 d . . . . .
F8 F 0.26378(16) 0.70830(18) 0.37978(11) 0.0653(5) Uani 1 1 d . . . . .
O10 O 0.39761(17) 0.67655(17) 0.50457(13) 0.0514(5) Uani 1 1 d . . . . .
N12 N 0.250000 0.8286(2) 0.500000 0.0341(6) Uani 1 2 d S T P . .
O7 O 0.3823(2) 0.3624(2) 0.23184(15) 0.0658(6) Uani 1 1 d . . . . .
O11 O 0.4020(2) 0.8466(2) 0.42294(17) 0.0705(7) Uani 1 1 d . . . . .
C16 C 0.7034(2) 0.75852(19) 0.56848(14) 0.0319(5) Uani 1 1 d . . . . .
H16A H 0.628136 0.739292 0.578153 0.038 Uiso 1 1 calc R U . . .
H16B H 0.756116 0.761330 0.621870 0.038 Uiso 1 1 calc R U . . .
C4 C 0.5792(2) 0.4703(2) 0.27086(16) 0.0380(5) Uani 1 1 d . . . . .
H4A H 0.626868 0.465362 0.326205 0.046 Uiso 1 1 calc R U . . .
H4B H 0.600824 0.411286 0.236047 0.046 Uiso 1 1 calc R U . . .
C17 C 0.7010(3) 0.8690(2) 0.5232(2) 0.0526(7) Uani 1 1 d . . . . .
H17A H 0.709176 0.930472 0.562926 0.063 Uiso 1 1 calc R U . . .
H17B H 0.629086 0.877761 0.484179 0.063 Uiso 1 1 calc R U . . .
C1 C 0.3856(3) 0.5830(3) 0.21870(19) 0.0538(7) Uani 1 1 d . . . . .
H1A H 0.316012 0.569047 0.178247 0.065 Uiso 1 1 calc R U . . .
H1B H 0.372086 0.643096 0.255703 0.065 Uiso 1 1 calc R U . . .
C3 C 0.5904(3) 0.5838(3) 0.2326(2) 0.0664(10) Uani 1 1 d . . . . .
H3A H 0.607181 0.639910 0.276389 0.080 Uiso 1 1 calc R U . . .
H3B H 0.652826 0.582809 0.202317 0.080 Uiso 1 1 calc R U . . .
C2 C 0.4832(3) 0.6123(3) 0.1750(2) 0.0623(9) Uani 1 1 d . . . . .
H2A H 0.476636 0.570068 0.123393 0.075 Uiso 1 1 calc R U . . .
H2B H 0.481530 0.691615 0.161627 0.075 Uiso 1 1 calc R U . . .
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'
F F 0.0171 0.0103 '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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 '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
O15 S14 O15 117.32(15) 2_656 . ?
O15 S14 C16 110.53(10) 2_656 . ?
O15 S14 C16 109.74(10) . . ?
O15 S14 C16 109.74(10) 2_656 2_656 ?
O15 S14 C16 110.54(10) . 2_656 ?
C16 S14 C16 97.10(15) . 2_656 ?
O7 S5 O6 116.28(13) . . ?
O7 S5 C1 110.15(16) . . ?
O6 S5 C1 110.08(14) . . ?
O7 S5 C4 110.39(14) . . ?
O6 S5 C4 111.23(11) . . ?
C1 S5 C4 97.05(13) . . ?
O11 S9 O10 118.73(14) . . ?
O11 S9 F8 104.10(15) . . ?
O10 S9 F8 105.11(12) . . ?
O11 S9 N12 107.83(14) . . ?
O10 S9 N12 115.50(11) . . ?
F8 S9 N12 103.82(8) . . ?
O6 Na13 O6 180.00(4) . 5_666 ?
O6 Na13 O15 89.64(6) . . ?
O6 Na13 O15 90.36(6) 5_666 . ?
O6 Na13 O15 90.36(6) . 5_666 ?
O6 Na13 O15 89.64(6) 5_666 5_666 ?
O15 Na13 O15 180.0 . 5_666 ?
O6 Na13 O10 88.09(7) . 5_666 ?
O6 Na13 O10 91.91(7) 5_666 5_666 ?
O15 Na13 O10 89.32(7) . 5_666 ?
O15 Na13 O10 90.68(7) 5_666 5_666 ?
O6 Na13 O10 91.91(7) . . ?
O6 Na13 O10 88.09(7) 5_666 . ?
O15 Na13 O10 90.68(7) . . ?
O15 Na13 O10 89.32(7) 5_666 . ?
O10 Na13 O10 180.0 5_666 . ?
S14 O15 Na13 133.46(9) . . ?
S5 O6 Na13 146.82(11) . . ?
S9 O10 Na13 146.05(13) . . ?
S9 N12 S9 122.37(18) 2_556 . ?
C17 C16 S14 104.62(16) . . ?
C17 C16 H16A 110.8 . . ?
S14 C16 H16A 110.8 . . ?
C17 C16 H16B 110.8 . . ?
S14 C16 H16B 110.8 . . ?
H16A C16 H16B 108.9 . . ?
C3 C4 S5 104.73(18) . . ?
C3 C4 H4A 110.8 . . ?
S5 C4 H4A 110.8 . . ?
C3 C4 H4B 110.8 . . ?
S5 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C16 C17 C17 107.52(19) . 2_656 ?
C16 C17 H17A 110.2 . . ?
C17 C17 H17A 110.2 2_656 . ?
C16 C17 H17B 110.2 . . ?
C17 C17 H17B 110.2 2_656 . ?
H17A C17 H17B 108.5 . . ?
C2 C1 S5 104.4(2) . . ?
C2 C1 H1A 110.9 . . ?
S5 C1 H1A 110.9 . . ?
C2 C1 H1B 110.9 . . ?
S5 C1 H1B 110.9 . . ?
H1A C1 H1B 108.9 . . ?
C2 C3 C4 109.5(3) . . ?
C2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
C3 C2 C1 107.5(3) . . ?
C3 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
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
S14 O15 1.4443(16) 2_656 ?
S14 O15 1.4443(16) . ?
S14 C16 1.787(2) . ?
S14 C16 1.787(2) 2_656 ?
S5 O7 1.435(2) . ?
S5 O6 1.4370(17) . ?
S5 C1 1.778(3) . ?
S5 C4 1.781(2) . ?
S9 O11 1.413(2) . ?
S9 O10 1.4127(19) . ?
S9 F8 1.5572(18) . ?
S9 N12 1.5660(14) . ?
Na13 O6 2.3140(17) . ?
Na13 O6 2.3140(17) 5_666 ?
Na13 O15 2.3879(16) . ?
Na13 O15 2.3879(16) 5_666 ?
Na13 O10 2.4438(18) 5_666 ?
Na13 O10 2.4438(18) . ?
C16 C17 1.507(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C4 C3 1.507(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C17 C17 1.512(6) 2_656 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C1 C2 1.519(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C2 1.473(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
