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_1554051
_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 B F4 Li O2 S'
_chemical_formula_sum            'C4 H8 B F4 Li O2 S'
_chemical_formula_weight         213.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1560(11)
_cell_length_b                   8.8536(17)
_cell_length_c                   18.337(3)
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    223
_cell_measurement_theta_max      29.5470
_cell_measurement_theta_min      4.0750
_cell_volume                     837.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (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 0.9971
_diffrn_measured_fraction_theta_max 0.8698
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      5.00  30.00   0.50    0.61    --   -0.10  81.00 -89.00   50
  2  \w    -80.00 -54.00   0.50    0.61    --   -0.10 -40.00 -37.00   52
  3  \w     -1.00  67.00   0.50    0.61    --   -0.10  77.00 -30.00  136
  4  \w    -17.00  65.00   0.50    0.61    --   -0.10  38.00 -90.00  164
  5  \w     19.00  44.00   0.50    0.61    --   -0.10  38.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0732053000
_diffrn_orient_matrix_UB_12      0.0601265000
_diffrn_orient_matrix_UB_13      -0.0152504000
_diffrn_orient_matrix_UB_21      -0.1163973000
_diffrn_orient_matrix_UB_22      0.0344667000
_diffrn_orient_matrix_UB_23      -0.0121817000
_diffrn_orient_matrix_UB_31      -0.0093633000
_diffrn_orient_matrix_UB_32      0.0400406000
_diffrn_orient_matrix_UB_33      0.0333358000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7196
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.180
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       needle
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0447
_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/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.823
_reflns_number_gt                1913
_reflns_number_total             2164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b09439_si_002.cif
_cod_data_source_block           watanabe_lab180314bf4_sl_1_1
_cod_database_code               1554051
_chemical_oxdiff_formula         C4H8O2S1B1F4Li
_diffrn_oxdiff_ac3_digest_frames
;
01ee2f307a1e36ac507d514787649e188100037ca69
;
_diffrn_oxdiff_ac3_digest_hkl
;
016f548c67c67a9023d2035ec356e33240c17b
;
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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              2172
_shelx_hkl_checksum              19402
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.336
_oxdiff_exptl_absorpt_empirical_full_min 0.432