High-concentration LiPF<sub>6</sub>/sulfone electrolytes: structure, transport properties, and battery application.
Ugata, Yosuke; Chen, Yichuan; Miyazaki, Shuhei; Sasagawa, Shohei; Ueno, Kazuhide; Watanabe, Masayoshi; Dokko, Kaoru; Physical chemistry chemical physics : PCCP 25 (2023) 29566–29575; doi:10.1039/d3cp04561g

data_7247523
_publ_section_title
;
 High-concentration LiPF<sub>6</sub>/sulfone electrolytes: structure,
 transport properties, and battery application.
;
_journal_issue                   43
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              29566
_journal_page_last               29575
_journal_paper_doi               10.1039/d3cp04561g
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C16 H32 Li O8 S4, F6 P'
_chemical_formula_sum            'C16 H32 F6 Li O8 P S4'
_chemical_formula_weight         632.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.287(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7168(7)
_cell_length_b                   8.3892(3)
_cell_length_c                   19.5667(8)
_cell_measurement_reflns_used    10920
_cell_measurement_temperature    223
_cell_measurement_theta_max      29.9720
_cell_measurement_theta_min      3.2050
_cell_volume                     2699.94(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_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     -7.00  18.00   0.50   20.32    --    0.00   0.00  88.00   50
  2  \w    -24.00   1.00   0.50   20.32    --    0.00  -0.00-116.00   50
  3  \w    -43.00  31.00   0.50   20.32    --    0.00 -82.00-180.00  148
  4  \w    -28.00  75.00   0.50   20.32    --    0.00  77.00 -30.00  206
  5  \w     41.00  85.00   0.50   20.32    --    0.00  57.00 -90.00   88
  6  \w    -88.00 -31.00   0.50   20.32    --    0.00 -82.00 150.00  114
  7  \w      6.00  31.00   0.50   20.32    --    0.00 -82.00 150.00   50
  8  \w    -35.00  -4.00   0.50   20.32    --    0.00 -82.00 120.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407642000
_diffrn_orient_matrix_UB_12      0.0010386000
_diffrn_orient_matrix_UB_13      0.0056146000
_diffrn_orient_matrix_UB_21      -0.0140810000
_diffrn_orient_matrix_UB_22      -0.0004151000
_diffrn_orient_matrix_UB_23      -0.0363917000
_diffrn_orient_matrix_UB_31      -0.0004177000
_diffrn_orient_matrix_UB_32      -0.0845734000
_diffrn_orient_matrix_UB_33      0.0002475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.292
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
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    1.556
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0589P)^2^+1.1729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5515
_reflns_number_total             7333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04561g2.cif
_cod_data_source_block           220916_lipf6_5sl_take2
_cod_depositor_comments
'Adding full bibliography for 7247523--7247524.cif.'
_cod_database_code               7247523
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: S1(0.5) S2(0.5) S03(0.5) S04(0.5) O00A(0.5) O00D(0.5) O00H(0.5)
 O00S(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) O006(0.5) O007(0.5)
 O008(0.5) O8(0.5) O9(0.5) O10(0.5) C(0.5) HA(0.5) HB(0.5) H00A(0.5) H00B(0.5)
 H00C(0.5) H00D(0.5) H00G(0.5) H00H(0.5) H00I(0.5) H00J(0.5) C00K(0.5)
 H00K(0.5) H00L(0.5) H00O(0.5) H00P(0.5) H00M(0.5) H00N(0.5) C00O(0.5)
 H00Q(0.5) H00R(0.5) C00Q(0.5) H00S(0.5) H00T(0.5) C00R(0.5) H00U(0.5)
 H00V(0.5) C00T(0.5) H00W(0.5) H00X(0.5) C00U(0.5) H00Y(0.5) H(0.5) C00V(0.5)
 H00Z(0.5) HC(0.5) HD(0.5) HE(0.5) H00(0.5) HF(0.5) C00X(0.5) H1(0.5) HG(0.5)
 C00Z(0.5) H2(0.5) HH(0.5) C2(0.5) H2A(0.5) H2B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C010(0.5) H01A(0.5)
 H01B(0.5) F00C(0.5) F00E(0.33333) F00F(0.33333) F00L(0.33333) F00N(0.33333)
 F1(0.66666) F2(0.66666) F3(0.66666) F4(0.66666) F009(0.5) F10(0.5) F14(0.5)
 O6(0.5) C10(0.5) H10A(0.5) H10B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C(HA,HB), C00G(H00A,H00B), C00G(H00C,H00D), C00I(H00E,H00F), C00J(H00G,H00H),
 C00J(H00I,H00J), C00K(H00K,H00L), C00M(H00O,H00P), C00M(H00M,H00N), C00O(H00Q,
 H00R), C00Q(H00S,H00T), C00R(H00U,H00V), C00T(H00W,H00X), C00U(H00Y,H),
 C00V(H00Z,HC), C00W(HD,HE), C00W(H00,HF), C00X(H1,HG), C00Z(H2,HH), C2(H2A,
 H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C010(H01A,H01B), C10(H10A,H10B),
 C4(H4A,H4B), C1(H1A,H1B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B)
;
_shelx_res_checksum              74879
_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 1.040
_oxdiff_exptl_absorpt_empirical_full_min 0.970