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_1571421
_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         'C4 H4 N2 O2 S'
_chemical_formula_sum            'C4 H4 N2 O2 S'
_chemical_formula_weight         144.15
_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             2024-01-24
_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                95.165(3)
_cell_angle_beta                 96.669(3)
_cell_angle_gamma                104.049(3)
_cell_formula_units_Z            2
_cell_length_a                   5.4317(2)
_cell_length_b                   7.1254(3)
_cell_length_c                   8.5194(3)
_cell_measurement_reflns_used    4826
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      71.1740
_cell_measurement_theta_min      5.2600
_cell_volume                     315.30(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 0.991
_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      6.00  43.00   0.50    0.50    --   45.50  49.00 -33.00   74
  2  \w     56.00 145.00   0.50    0.50    --   98.30 -49.00 178.00  178
  3  \w    124.00 173.00   0.50    0.50    --   98.30  49.00 -33.00   98
  4  \w     52.00 106.00   0.50    0.50    --   98.30  49.00 -33.00  108
  5  \w     17.00  68.00   0.50    0.50    --   45.50  57.00  60.00  102
  6  \w     12.00  88.00   0.50    0.50    --   45.50 -49.00 178.00  152
  7  \w    -41.00  66.00   0.50    0.50    --   45.50 -57.00 -60.00  214
  8  \w     95.00 121.00   0.50    0.50    --   45.50  49.00 -33.00   52
  9  \w     78.00 128.00   0.50    0.50    --   45.50  82.00 150.00  100
 10  \w      0.00  32.00   0.50    0.50    --   45.50  82.00 150.00   64
 11  \w    -27.00   1.00   0.50    0.50    --   45.50 -49.00 178.00   56
 12  \w     97.00 122.00   0.50    0.50    --   45.50  57.00  60.00   50
 13  \w      7.00  65.00   0.50    0.50    --   52.00  81.00-105.08  116
 14  \w     78.00 138.00   0.50    0.50    --   52.00  81.00-105.08  120
 15  \w    108.00 135.00   0.50    0.50    --   60.00  75.00-132.97   54
 16  \w     21.00  47.00   0.50    0.50    --   60.00  75.00-132.97   52
 17  \w     18.00  47.00   0.50    0.50    --   64.00  80.00  24.43   58
 18  \w     19.00  55.00   0.50    0.50    --   64.00  79.00 -62.68   72
 19  \w     25.00  67.00   0.50    0.50    --   72.00  82.00 -57.78   84
 20  \w     27.00  63.00   0.50    0.50    --   72.00  82.00 146.29   72
 21  \w     97.00 160.00   0.50    0.50    --   72.00  82.00 -57.78  126
 22  \w     90.00 116.00   0.50    0.50    --   76.00  81.00 114.28   52
 23  \w     29.00  55.00   0.50    0.50    --   76.00  82.00  66.19   52
 24  \w     30.00  55.00   0.50    0.50    --   76.00  81.00 114.28   50
 25  \w    155.00 188.00   0.50    0.50    --   98.30  30.00 150.00   66
 26  \w     19.00 145.00   0.50    0.50    --   98.30  30.00 150.00  252
 27  \w    100.00 126.00   0.50    0.50    --   98.30  82.00-120.00   52
 28  \w     10.00  65.00   0.50    0.50    --   98.30 -77.00  90.00  110
 29  \w    121.00 188.00   0.50    0.50    --   98.30  82.00   0.00  134
 30  \w     12.00 143.00   0.50    0.50    --   98.30 -77.00-150.00  262
 31  \w     85.00 110.00   0.50    0.50    --   98.30 -77.00  90.00   50
 32  \w     57.00 131.00   0.50    0.50    --   98.30  82.00  60.00  148
 33  \w    137.00 162.00   0.50    0.50    --   98.30  82.00  60.00   50
 34  \w     51.00  94.00   0.50    0.50    --   98.30  82.00   0.00   86
 35  \w    142.00 167.00   0.50    0.50    --   98.30  82.00  30.00   50
 36  \w     56.00  94.00   0.50    0.50    --   98.30  82.00  30.00   76
 37  \w    112.00 163.00   0.50    0.50    --   98.30  82.00 120.00  102
 38  \w     53.00  91.00   0.50    0.50    --   98.30  82.00-120.00   76
 39  \w     51.00  99.00   0.50    0.50    --   98.30  82.00 120.00   96
 40  \w     54.00  92.00   0.50    0.50    --   98.30  77.00 -30.00   76
 41  \w    163.00 188.00   0.50    0.50    --   98.30  61.00-120.00   50
 42  \w     58.00 126.00   0.50    0.50    --   98.30  61.00-120.00  136
 43  \w      9.00 142.00   0.50    0.50    --   98.30 -82.00  30.00  266
 44  \w    156.00 186.00   0.50    0.50    --   98.30   0.00   0.00   60
 45  \w     95.00 150.00   0.50    0.50    --   98.30   0.00   0.00  110
 46  \w    118.00 144.00   0.50    0.50    --   98.30  82.00 -60.00   52
 47  \w     66.00  91.00   0.50    0.50    --   98.30   0.00   0.00   50
 48  \w     39.00  96.00   0.50    0.50    --   98.30 -82.00-180.00  114
 49  \w     10.00  51.00   0.50    0.50    --   98.30   0.00   0.00   82
 50  \w     88.00 142.00   0.50    0.50    --   98.30 -77.00 -60.00  108
 51  \w     51.00  76.00   0.50    0.50    --   98.30  82.00 -60.00   50
 52  \w    119.00 146.00   0.50    0.50    --   98.30  45.00  60.00   54
 53  \w     58.00 164.00   0.50    0.50    --   98.30  61.00-180.00  212
 54  \w     51.00 104.00   0.50    0.50    --   98.30  82.00-180.00  106
 55  \w     91.00 116.00   0.50    0.50    --   98.30 -82.00-120.00   50
 56  \w     48.00  81.00   0.50    0.50    --   98.30  45.00  60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): 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      -0.2908751000
_diffrn_orient_matrix_UB_12      -0.0203450000
_diffrn_orient_matrix_UB_13      -0.0320902000
_diffrn_orient_matrix_UB_21      0.0464114000
_diffrn_orient_matrix_UB_22      0.1667407000
_diffrn_orient_matrix_UB_23      -0.1049831000
_diffrn_orient_matrix_UB_31      -0.0223000000
_diffrn_orient_matrix_UB_32      -0.1490482000
_diffrn_orient_matrix_UB_33      -0.1469751000
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.991
_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       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5481
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.550
_diffrn_reflns_theta_min         5.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38698
_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    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             148
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.130(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0418P)^2^+0.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1182
_reflns_number_total             1207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01492h3.cif
_cod_data_source_block           537-HCMs(CN)2
_cod_depositor_comments
'Adding full bibliography for 1571419--1571424.cif.'
_cod_database_code               1571421
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.586
_shelx_estimated_absorpt_t_min   0.503
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              54543
_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 2.011
_oxdiff_exptl_absorpt_empirical_full_min 0.528