Direct Evidence for Li Ion Hopping Conduction in Highly Concentrated Sulfolane-Based Liquid Electrolytes.
Dokko, Kaoru; Watanabe, Daiki; Ugata, Yosuke; Thomas, Morgan L.; Tsuzuki, Seiji; Shinoda, Wataru; Hashimoto, Kei; Ueno, Kazuhide; Umebayashi, Yasuhiro; Watanabe, Masayoshi; The journal of physical chemistry. B 122 (2018) 10736–10745; doi:10.1021/acs.jpcb.8b09439

data_1554050
_publ_section_title
;
 Direct Evidence for Li Ion Hopping Conduction in Highly Concentrated
 Sulfolane-Based Liquid Electrolytes.
;
_journal_issue                   47
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              10736
_journal_page_last               10745
_journal_paper_doi               10.1021/acs.jpcb.8b09439
_journal_volume                  122
_journal_year                    2018
_chemical_formula_moiety         'C4 H8 F2 Li N O6 S3'
_chemical_formula_sum            'C4 H8 F2 Li N O6 S3'
_chemical_formula_weight         307.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.266(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0746(4)
_cell_length_b                   22.6735(13)
_cell_length_c                   9.7382(6)
_cell_measurement_reflns_used    2374
_cell_measurement_temperature    223
_cell_measurement_theta_max      28.1120
_cell_measurement_theta_min      3.5600
_cell_volume                     1120.19(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9150
_diffrn_measured_fraction_theta_max 0.9153
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f    -80.00 100.00   0.50    8.00   0.00  20.00   0.00    --   360
  2  \w    -20.00  28.00   0.50    8.00    --   20.00 -90.00   0.00   96
  3  \w    -20.00  28.00   0.50    8.00    --   20.00 -90.00  90.00   96
  4  \w    -20.00  28.00   0.50    8.00    --   20.00 -90.00 180.00   96
  5  \w    -20.00  28.00   0.50    8.00    --   20.00 -90.00 270.00   96
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0818898000
_diffrn_orient_matrix_UB_12      0.0017237000
_diffrn_orient_matrix_UB_13      -0.0598721000
_diffrn_orient_matrix_UB_21      -0.0530253000
_diffrn_orient_matrix_UB_22      -0.0281750000
_diffrn_orient_matrix_UB_23      0.0148640000
_diffrn_orient_matrix_UB_31      -0.1001393000
_diffrn_orient_matrix_UB_32      0.0134752000
_diffrn_orient_matrix_UB_33      0.0387821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9415
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.190
_diffrn_reflns_theta_min         2.758
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0523
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2001
_reflns_number_total             3039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b09439_si_003.cif
_cod_data_source_block           watanabelab_160714_fsa_sl1_1'52
_cod_database_code               1554050
_chemical_oxdiff_formula         LiC4H8O6S3N1F2
_reflns_odcompleteness_completeness 91.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_shelx_res_checksum              74047
_shelx_hkl_checksum              4482
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.740