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_1571423
_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         'C20 H36 F12 Li4 N4 O12 S4, C4 H8 O2 S'
_chemical_formula_sum            'C24 H44 F12 Li4 N4 O14 S5'
_chemical_formula_weight         1028.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 95.895(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3980(2)
_cell_length_b                   19.9938(3)
_cell_length_c                   22.1730(4)
_cell_measurement_reflns_used    6837
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      70.9920
_cell_measurement_theta_min      4.8050
_cell_volume                     4585.29(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.974
_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     57.00 111.00   0.50    5.61    --   45.70  77.00-120.00  108
  2  \w     21.00 132.00   0.50    5.61    --   45.70  38.00  30.00  222
  3  \w    -32.00  90.00   0.50    5.61    --   45.70 -57.00 120.00  244
  4  \w     16.00 115.00   0.50   22.43    --   98.30 -45.00 -90.00  198
  5  \w     10.00 140.00   0.50   22.43    --   98.30 -61.00 -90.00  260
  6  \w     92.00 122.00   0.50   22.43    --   98.30  77.00-150.00   60
  7  \w     17.00 143.00   0.50   22.43    --   98.30 -77.00  90.00  252
  8  \w     58.00 153.00   0.50   22.43    --   98.30  61.00-150.00  190
  9  \w     19.00  45.00   0.50   22.43    --   98.30 -77.00  60.00   52
 10  \w     30.00  90.00   0.50   22.43    --   98.30 -61.00  90.00  120
;
_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      -0.0037473000
_diffrn_orient_matrix_UB_12      -0.0643779000
_diffrn_orient_matrix_UB_13      0.0378968000
_diffrn_orient_matrix_UB_21      -0.0885606000
_diffrn_orient_matrix_UB_22      0.0348488000
_diffrn_orient_matrix_UB_23      0.0419396000
_diffrn_orient_matrix_UB_31      -0.1197020000
_diffrn_orient_matrix_UB_32      -0.0239194000
_diffrn_orient_matrix_UB_33      -0.0410834000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11939
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.860
_diffrn_reflns_theta_min         4.423
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22564
_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    1.490
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1063P)^2^+2.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3836
_reflns_number_total             4385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01492h3.cif
_cod_data_source_block           LiNTfN3O1-sulfolane
_cod_depositor_comments
'Adding full bibliography for 1571419--1571424.cif.'
_cod_database_code               1571423
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.557
_reflns_odcompleteness_completeness 99.93
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H11D(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) C12A(0.5) H12C(0.5) H12D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C11(H11C,H11D), C12(H12A,H12B), C12A(H12C,H12D)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              52644
_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 2.172
_oxdiff_exptl_absorpt_empirical_full_min 0.531