Solid state <sup>1</sup>H, <sup>7</sup>Li, and <sup>13</sup>C NMR studies on new ionic plastic crystals of crown ether-Li-TFSA complexes.
Kobayashi, Akira; Yamagami, Jun; Ranjan, Subham; Takamizawa, Satoshi; Honda, Hisashi; Physical chemistry chemical physics : PCCP 25 (2023) 27836–27847; doi:10.1039/d3cp02614k

data_7247488
_publ_section_title
;
 Solid state <sup>1</sup>H, <sup>7</sup>Li, and <sup>13</sup>C NMR studies
 on new ionic plastic crystals of crown ether-Li-TFSA complexes.
;
_journal_issue                   40
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              27836
_journal_page_last               27847
_journal_paper_doi               10.1039/d3cp02614k
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C12 H20 F6 N Na O9 S2'
_chemical_formula_weight         523.40
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2023-05-25 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.231(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.292(13)
_cell_length_b                   9.039(4)
_cell_length_c                   18.545(9)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.015
_cell_measurement_theta_min      1.51
_cell_volume                     4512(4)
_computing_cell_refinement       'APEX3 v2019.11 (Bruker AXS Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT (Bruker AXS Inc.)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16823
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9340
_exptl_absorpt_correction_T_min  0.7459
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     1932
_refine_ls_restrained_S_all      3.627
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.1478
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4292
_refine_ls_wR_factor_ref         0.4546
_reflns_number_gt                2607
_reflns_number_total             3907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3cp02614k2.cif
_cod_data_source_block           Na15C5_NTf2_296K
_cod_depositor_comments
'Adding full bibliography for 7247487--7247488.cif.'
_cod_database_code               7247488