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_7247487
_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 H18.86 F6 N Na O9 S2'
_chemical_formula_weight         522.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        '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
;
2023-01-19 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.468(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.1334(15)
_cell_length_b                   8.9809(5)
_cell_length_c                   18.4512(10)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.28
_cell_volume                     4428.3(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_publication_material  'APEX3 v2019.11 (Bruker AXS Inc., 2019)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      253(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17022
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.352
_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    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2135
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     1447
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1493P)^2^+16.5132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2590
_reflns_number_gt                3103
_reflns_number_total             3908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3cp02614k2.cif
_cod_data_source_block           Na15C5_NTf2_253K
_cod_depositor_comments
'Adding full bibliography for 7247487--7247488.cif.'
_cod_database_code               7247487