Ionic transport in highly concentrated lithium bis(fluorosulfonyl)amide electrolytes with keto ester solvents: structural implications for ion hopping conduction in liquid electrolytes.
Kondou, Shinji; Thomas, Morgan L.; Mandai, Toshihiko; Ueno, Kazuhide; Dokko, Kaoru; Watanabe, Masayoshi; Physical chemistry chemical physics : PCCP 21 (2019) 5097–5105; doi:10.1039/c9cp00425d

data_7234976
_publ_section_title
;
 Ionic transport in highly concentrated lithium bis(fluorosulfonyl)amide
 electrolytes with keto ester solvents: structural implications for ion
 hopping conduction in liquid electrolytes.
;
_journal_issue                   9
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              5097
_journal_page_last               5105
_journal_paper_doi               10.1039/c9cp00425d
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C9 H8 F12 Li2 N2 O11 S4'
_chemical_formula_sum            'C9 H8 F12 Li2 N2 O11 S4'
_chemical_formula_weight         690.30
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.679(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1850(5)
_cell_length_b                   10.4660(5)
_cell_length_c                   20.4745(9)
_cell_measurement_reflns_used    6359
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.3740
_cell_measurement_theta_min      3.2990
_cell_volume                     2396.62(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9609
_diffrn_measured_fraction_theta_max 0.8245
_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    -46.00 -19.00   0.50   29.20    --    5.10 -54.00  -0.00   54
  2  \w     10.00  35.00   0.50   29.20    --    5.10  54.00 143.00   50
  3  \w     52.00  84.00   0.50   29.20    --    5.10  57.00-150.00   64
  4  \w    -23.00  79.00   0.50   29.20    --    5.10  57.00   0.00  204
  5  \w     41.00  66.00   0.50   29.20    --    5.10  57.00 -60.00   50
  6  \w    -24.00  40.00   0.50   29.20    --    5.10  57.00-150.00  128
;
_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      -0.0528303000
_diffrn_orient_matrix_UB_12      -0.0147677000
_diffrn_orient_matrix_UB_13      -0.0179573000
_diffrn_orient_matrix_UB_21      -0.0180948000
_diffrn_orient_matrix_UB_22      -0.0417433000
_diffrn_orient_matrix_UB_23      0.0252978000
_diffrn_orient_matrix_UB_31      -0.0300421000
_diffrn_orient_matrix_UB_32      0.0513115000
_diffrn_orient_matrix_UB_33      0.0154295000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16128
_diffrn_reflns_theta_full        28.2584
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.9130
_exptl_crystal_description       needle
_exptl_crystal_F_000             1371.3974
_refine_diff_density_max         1.6341
_refine_diff_density_min         -0.6371
_refine_diff_density_rms         0.1228
_refine_ls_d_res_high            0.7506
_refine_ls_d_res_low             6.1476
_refine_ls_goodness_of_fit_ref   1.0606
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0606
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+5.8016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -14
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -11
_reflns_number_gt                3878
_reflns_number_total             4885
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cp00425d2.cif
_cod_data_source_block           exp_453
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7234976
_chemical_oxdiff_formula         'Li N S O F C'
_chemical_oxdiff_usercomment     LiTFSA_MA_1_0,5
_reflns_odcompleteness_completeness 96.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.20
_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. Restrained distances
3.a Secondary CH2 refined with riding coordinates:
 C33(H33a,H33b)
3.b Idealised Me refined as rotating group:
 C37(H37a,H37b,H37c), C36(H36a,H36b,H36c)
;
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.819