Lithium Diffusion Pathways in 3R-LixTiS2: A Combined Neutron Diffraction and Computational Study
Wiedemann, Dennis; Islam, Mazharul M.; Nakhal, Suliman; Senyshyn, Anatoliy; Bredow, Thomas; Lerch, Martin; The Journal of Physical Chemistry C 119 (2015) 11370–; doi:10.1021/acs.jpcc.5b01166

data_1519661
_publ_section_title
;
 Lithium Diffusion Pathways in 3R-LixTiS2: A Combined Neutron Diffraction
 and Computational Study
;
_journal_issue                   21
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              11370
_journal_paper_doi               10.1021/acs.jpcc.5b01166
_journal_volume                  119
_journal_year                    2015
_chemical_compound_source        synthetic
_chemical_formula_iupac          'Li0.90 Ti S2 (hR3.9)'
_chemical_formula_sum            'Li0.9 S2 Ti'
_chemical_formula_weight         118.2
_chemical_name_systematic
' lithium titanium disulfide (lithium deficient)'
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      166
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   notdet
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   3.53131(8)
_cell_length_b                   3.53131(8)
_cell_length_c                   18.6090(6)
_cell_measurement_temperature    973
_cell_volume                     200.967(9)
_computing_cell_refinement       'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_data_collection       'CARESS (HZB, 2013)'
_computing_data_reduction        'DATAPARSER (Senyshyn, 2011)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2013)'
_computing_publication_material  'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek, 2014)'
_computing_structure_solution    'ICSD (Bergerhoff, 1987)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      973
_diffrn_detector                 '^3^He counter'
_diffrn_detector_details
; curved position-sensitive detector-array of 80 counter tubes, height: 300 mm,
resolution: 3 mm (B. Krimmer, R. Gilles, K. Zeitelhack, R. Schneider,
G. Montermann, H. Boysen, H. Fuess, Appl. Phys. A: Mater. Sci. Process.
2002, 74, S154-S156)
;
_diffrn_measurement_device       'one-circle powder diffractometer'
_diffrn_measurement_device_details
; M. Hoelzel, A. Senyshyn, N. Juenke, H. Boysen, W. Schmahl, H. Fuess,
Nucl. Instrum. Methods Phys. Res., Sect. A 2012, 667, 32-37
;
_diffrn_measurement_device_type  SPODI
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_monochromator  'Ge 551'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.54829
_diffrn_source                   'nuclear reactor'
_diffrn_source_type              'FRM II beamline 8a'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
; correction for a cylindrical sample with \mR = 0.216 as
implemented in JANA2006
;
_exptl_crystal_density_diffrn    2.9311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1.84
_pd_char_atten_coef_mu_calc      0.058
_pd_char_colour                  black
_pd_instr_2theta_monochr_pre     155
_pd_instr_beam_size_ax           100
_pd_instr_beam_size_eq           25
_pd_instr_dist_mono/spec         5000
_pd_instr_dist_spec/detc         1120
_pd_instr_dist_src/mono          17500
_pd_instr_geometry               Debye-Scherrer
_pd_instr_location
; SPODI diffractometer, Heinz Maier-Leibnitz Zentrum,
Garching b. M\"unchen (Germany)
;
_pd_instr_monochr_pre_spec       'Ge 551'
_pd_instr_soller_eq_spec/detc    0.16667
_pd_meas_2theta_range_inc        0.05
_pd_meas_2theta_range_max        151.900
_pd_meas_2theta_range_min        0.950
_pd_meas_number_of_points        3020
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.05
_pd_proc_2theta_range_max        151.65
_pd_proc_2theta_range_min        10.05
_pd_proc_info_data_reduction
; efficiency/intensity correction and 2\q scattering-angle correction for each
detector-collimator pair, geometrical data correction with Lorentz factor,
variable integration height to obtain 1D data:
H~L~=(R^2^*sin(4\q))/(H~S~*cos^2^(2\q))*\D2\q+H~S~/2
with H~L~: limiting height, H~S~: sample height, R: detector radius
(M. Hoelzel, A. Senyshyn, N. Juenke, H. Boysen, W. Schmahl, H. Fuess,
Nucl. Instrum. Methods Phys. Res., Sect. A 2012, 667, 32-37)
;
_pd_proc_ls_background_function
; manual background (visual estimation, unrefined) interpolated by five
Legendre polynomials (1st: 11(2), 2nd: 9(4), 3rd: -2(5), 4th: 1(5),
5th: 10(6))
;
_pd_proc_ls_pref_orient_corr
' March-Dollase model for (001): r = 1.009(3)'
_pd_proc_ls_profile_function
; pseudo-Voigt profile with Thompson-Cox-Hastings approach:
G~U~ = 191(4), G~V~ = -235, G~W~ = 254(3), L~X~ = 3.5(2), L~Y~ = 0.31,
B\'erar-Baldinozzi asymmetry correction:
A~0~ = 0.337(6), A~1~ = -0.744
;
_pd_proc_ls_prof_R_factor        0.0211
_pd_proc_ls_prof_wR_expected     0.0214
_pd_proc_ls_prof_wR_factor       0.0260
_pd_spec_mounting                'compacted powder in niobium can'
_pd_spec_mount_mode              transmission
_pd_spec_orientation             vertical
_pd_spec_shape                   cylinder
_pd_spec_size_axial              40
_pd_spec_size_equat              7.5
_refine_diff_density_max         0.06
_refine_diff_density_min         -0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.22
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_constraints    0
_refine_ls_number_parameters     23
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0229
_refine_ls_R_I_factor            0.0296
_refine_ls_shift/su_max          0.0050
_refine_ls_shift/su_mean         0.0012
_refine_ls_weighting_details     w=1/[\s^2^(F~o~)+(0.01F~o~)^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0305
_refine_ls_wR_factor_gt          0.0298
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            jp5b01166_si_005.cif
_cod_data_source_block           0.9-700C
_cod_depositor_comments
'Adding full bibliography for 1519661--1519664.cif.'
_cod_original_cell_volume        200.967(13)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'Li0.90 S2 Ti1'
_cod_database_code               1519661