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_1571420
_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_formula_moiety         'C5 H9 F3 Li N O3 S'
_chemical_formula_sum            'C5 H9 F3 Li N O3 S'
_chemical_formula_weight         227.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                80.255(2)
_cell_angle_beta                 83.499(2)
_cell_angle_gamma                86.548(2)
_cell_formula_units_Z            2
_cell_length_a                   5.5440(2)
_cell_length_b                   9.2231(2)
_cell_length_c                   10.2431(2)
_cell_measurement_reflns_used    5443
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      71.2310
_cell_measurement_theta_min      4.4080
_cell_volume                     512.43(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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.981
_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    -41.00  49.00   0.50    0.50    --    0.00  64.00 -78.91  180
  2  \w     94.00 135.00   0.50    0.50    --   45.70  82.00  30.00   82
  3  \w      7.00  32.00   0.50    0.50    --   45.70  57.00  90.00   50
  4  \w     90.00 134.00   0.50    0.50    --   45.70  57.00  90.00   88
  5  \w      0.00  63.00   0.50    0.50    --   45.70  82.00  30.00  126
  6  \w    -35.00  82.00   0.50    0.50    --   45.70 -57.00  90.00  234
  7  \w      8.00  61.00   0.50    0.50    --   48.00  80.00-142.31  106
  8  \w     79.00 105.00   0.50    0.50    --   48.00  80.00-142.31   52
  9  \w     12.00  54.00   0.50    0.50    --   56.00  79.00 171.25   84
 10  \w     82.00 142.00   0.50    0.50    --   56.00  79.00 171.25  120
 11  \w     11.00  64.00   0.50    0.50    --   56.00  82.00 -33.52  106
 12  \w    100.00 139.00   0.50    0.50    --   56.00  82.00 -33.52   78
 13  \w     16.00  55.00   0.50    0.50    --   60.00  81.00-126.03   78
 14  \w     20.00  69.00   0.50    0.50    --   64.00  79.00 -83.87   98
 15  \w     81.00 107.00   0.50    0.50    --   64.00  79.00 -83.87   52
 16  \w     21.00  65.00   0.50    0.50    --   68.00  82.00  77.45   88
 17  \w     33.00  63.00   0.50    1.59    --   80.00  82.00  38.73   60
 18  \w    108.00 142.00   0.50    1.59    --   80.00  82.00  38.73   68
 19  \w    137.00 177.00   0.50    1.59    --   88.00  82.00 115.59   80
 20  \w     41.00  78.00   0.50    1.59    --   88.00  82.00 115.59   74
 21  \w     82.00 123.00   0.50    1.59    --   88.00  82.00 115.59   82
 22  \w     95.00 144.00   0.50    1.59    --   98.30  82.00-120.00   98
 23  \w     36.00 137.00   0.50    1.59    --   98.30 -15.00-150.00  202
 24  \w     51.00  92.00   0.50    1.59    --   98.30  82.00-120.00   82
 25  \w     51.00  91.00   0.50    1.59    --   98.30  82.00-180.00   80
 26  \w    141.00 188.00   0.50    1.59    --   98.30  82.00 -60.00   94
 27  \w     37.00 117.00   0.50    1.59    --   98.30 -82.00 120.00  160
 28  \w    157.00 188.00   0.50    1.59    --   98.30 -15.00-150.00   62
 29  \w     52.00 145.00   0.50    1.59    --   98.30 -82.00 -30.00  186
 30  \w     54.00 157.00   0.50    1.59    --   98.30  77.00  30.00  206
 31  \w     90.00 115.00   0.50    1.59    --   98.30  77.00  90.00   50
 32  \w      9.00 118.00   0.50    1.59    --   98.30 -77.00  30.00  218
 33  \w    159.00 188.00   0.50    1.59    --   98.30  77.00   0.00   58
 34  \w     54.00  84.00   0.50    1.59    --   98.30  77.00  90.00   60
 35  \w     51.00 110.00   0.50    1.59    --   98.30  82.00 -60.00  118
 36  \w     54.00 100.00   0.50    1.59    --   98.30  77.00   0.00   92
 37  \w    101.00 127.00   0.50    1.59    --   98.30  30.00 -60.00   52
 38  \w    140.00 166.00   0.50    1.59    --   98.30  82.00 -90.00   52
 39  \w     21.00  63.00   0.50    1.59    --   98.30  30.00 -60.00   84
 40  \w     51.00  79.00   0.50    1.59    --   98.30  82.00 -30.00   56
 41  \w     51.00 101.00   0.50    1.59    --   98.30  82.00 -90.00  100
 42  \w    113.00 138.00   0.50    1.59    --   98.30  30.00-180.00   50
 43  \w     26.00  94.00   0.50    1.59    --   98.30  30.00-180.00  136
 44  \w    148.00 174.00   0.50    1.59    --   98.30  82.00 150.00   52
 45  \w    106.00 138.00   0.50    1.59    --   98.30 -45.00  90.00   64
 46  \w     18.00  75.00   0.50    1.59    --   98.30 -45.00  90.00  114
 47  \w     51.00 134.00   0.50    1.59    --   98.30  82.00 150.00  166
 48  \w     51.00  95.00   0.50    1.59    --   98.30  82.00-150.00   88
 49  \w    160.00 186.00   0.50    1.59    --   98.30  77.00  60.00   52
 50  \w     17.00 184.00   0.50    1.59    --   98.30   0.00   0.00  334
 51  \w    109.00 134.00   0.50    1.59    --   98.30  77.00  60.00   50
 52  \w     54.00  80.00   0.50    1.59    --   98.30  77.00  60.00   52
 53  \w     60.00 139.00   0.50    1.59    --   98.30 -82.00-150.00  158
 54  \w    156.00 183.00   0.50    1.59    --   98.30  82.00-180.00   54
 55  \w    162.00 187.00   0.50    1.59    --   98.30  77.00  30.00   50
 56  \w     24.00  49.00   0.50    1.59    --   98.30 -82.00-150.00   50
;
_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      -0.0363040000
_diffrn_orient_matrix_UB_12      -0.1221848000
_diffrn_orient_matrix_UB_13      0.1223573000
_diffrn_orient_matrix_UB_21      -0.0314290000
_diffrn_orient_matrix_UB_22      0.1172427000
_diffrn_orient_matrix_UB_23      0.0920237000
_diffrn_orient_matrix_UB_31      -0.2757727000
_diffrn_orient_matrix_UB_32      0.0099398000
_diffrn_orient_matrix_UB_33      -0.0102831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9087
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.765
_diffrn_reflns_theta_min         4.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02289
_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    1.472
_exptl_crystal_description       needle
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1210P)^2^+0.0061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1768
_reflns_number_total             1966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01492h3.cif
_cod_data_source_block           LiNTfN3O1
_cod_depositor_comments
'Adding full bibliography for 1571419--1571424.cif.'
_cod_database_code               1571420
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.509
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              80950
_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 15.580
_oxdiff_exptl_absorpt_empirical_full_min 0.240