Evolving better solvate electrolytes for lithium secondary batteries.
Philippi, Frederik; Middendorf, Maleen; Shigenobu, Keisuke; Matsuyama, Yuna; Palumbo, Oriele; Pugh, David; Sudoh, Taku; Dokko, Kaoru; Watanabe, Masayoshi; Schönhoff, Monika; Shinoda, Wataru; Ueno, Kazuhide; Chemical science 15 (2024) 7342–7358; doi:10.1039/d4sc01492h

data_1571419
_publ_section_title
;
 Evolving better solvate electrolytes for lithium secondary batteries.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              7342
_journal_page_last               7358
_journal_paper_doi               10.1039/d4sc01492h
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C3 H3 F3 Li N O3 S'
_chemical_formula_sum            'C3 H3 F3 Li N O3 S'
_chemical_formula_weight         197.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-28 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            60
_cell_length_a                   63.7924(10)
_cell_length_b                   9.60050(10)
_cell_length_c                   17.2224(2)
_cell_measurement_reflns_used    27005
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      71.5850
_cell_measurement_theta_min      5.0530
_cell_volume                     10547.6(2)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.965
_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     12.00  38.22   0.38    4.48    --   45.70 -48.00  60.00   69
  2  \w     42.00  67.08   0.38    4.48    --   45.70  81.00  53.00   66
  3  \w     -1.00  24.08   0.38    4.48    --   45.70 -81.00 -69.00   66
  4  \w     41.00  66.08   0.38    4.48    --   45.70  48.00-151.00   66
  5  \w     94.00 119.08   0.38   17.92    --   98.30  48.00-151.00   66
  6  \w     76.00 101.08   0.38   17.92    --   98.30 -81.00 -69.00   66
  7  \w    102.00 128.22   0.38   17.92    --   98.30  81.00  53.00   69
  8  \w     77.00 102.08   0.38   17.92    --   98.30 -48.00  60.00   66
  9  \w      4.00  31.36   0.38    4.48    --   45.70  57.00 120.00   72
 10  \w     35.00 118.22   0.38    4.48    --   45.70  57.00 120.00  219
 11  \w    -35.00  87.36   0.38    4.48    --   45.70 -57.00 -60.00  322
 12  \w     62.00 101.14   0.38   17.92    --   98.30  61.00 150.00  103
 13  \w     27.00 107.18   0.38   17.92    --   98.30 -77.00 -30.00  211
 14  \w     65.00 187.74   0.38   17.92    --   98.30  45.00 -60.00  323
 15  \w    107.00 187.18   0.38   17.92    --   98.30  61.00 150.00  211
 16  \w     18.00 179.12   0.38   17.92    --   98.30  30.00  60.00  424
 17  \w    157.00 183.22   0.38   17.92    --   98.30  61.00 120.00   69
 18  \w     96.00 122.22   0.38   17.92    --   98.30  61.00-180.00   69
 19  \w     62.00 146.36   0.38   17.92    --   98.30  61.00 120.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -78
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35303
_diffrn_reflns_point_group_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.772
_diffrn_reflns_theta_min         5.136
_exptl_absorpt_coefficient_mu    4.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44421
_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    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1634
_refine_ls_number_reflns         17816
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      29.506
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0417P)^2^+41.0339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_full    0.784
_reflns_Friedel_fraction_max     0.750
_reflns_number_gt                16087
_reflns_number_total             17816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01492h3.cif
_cod_data_source_block           LiNTfAc
_cod_depositor_comments
'Adding full bibliography for 1571419--1571424.cif.'
_cod_database_code               1571419
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.983(19)
 0.017(19)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N13-F3 = N13-F3A
 1.34 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F1A) = Uanis(F2A) = Uanis(F3A)
Uanis(F28) = Uanis(F29) = Uanis(F30) = Uanis(F28A) = Uanis(F29A) = Uanis(F30A)
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F28A)=Sof(F29A)=Sof(F30A)=1-FVAR(2)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(2)
6.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              56913
_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
;