Structural complexities and sodium-ion diffusion in the intercalates NaxTiS2: move it, change it, re-diffract it
Wiedemann, Dennis; Suard, Emmanuelle; Lerch, Martin; RSC Advances 9 (2019) 27780–; doi:10.1039/C9RA05690D

data_7233626
_publ_section_title
;
 Structural complexities and sodium-ion diffusion in the intercalates
 NaxTiS2: move it, change it, re-diffract it
;
_journal_issue                   48
_journal_name_full               'RSC Advances'
_journal_page_first              27780
_journal_paper_doi               10.1039/C9RA05690D
_journal_volume                  9
_journal_year                    2019
_chemical_compound_source        synthetic
_chemical_formula_iupac          'Na0.5 Ti S2'
_chemical_formula_sum            'Na0.5 S2 Ti'
_chemical_formula_weight         123.5
_chemical_name_systematic
;
sodium titanium disulfide, sodium deficient
;
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_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'
_audit_update_record
;
2019-07-22 deposited with the CCDC.    2019-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   3.45878(5)
_cell_length_b                   3.45878(5)
_cell_length_c                   21.2010(5)
_cell_measurement_temperature    573.15
_cell_volume                     219.651(7)
_computing_cell_refinement       'JANA2006 (Pet\<r\'i\<cek et al., 2014)'
_computing_data_collection       'NOMAD 3.0.16 (Institut Laue-Langevin, 2016)'
_computing_data_reduction        'Lamp 8.5 (Richard et al., 1996)'
_computing_molecular_graphics    'Diamond 4.5 (Brandenbrug, 2019)'
_computing_publication_material  'JANA2006 (Pet\<r\'i\<cek et al., 2014)'
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek et al., 2014)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      573.15
_diffrn_detector                 '^3^He counter'
_diffrn_detector_details
;
array of 128 counting tubes (Suard & Hewat, 2001)
;
_diffrn_measurement_device       'two-axis diffractometer'
_diffrn_measurement_device_details 'Hewat (1986)'
_diffrn_measurement_device_type  D2B
_diffrn_measurement_method       'profile data from 2\q scans'
_diffrn_radiation_monochromator  'Ge 335'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.594
_diffrn_source                   'nuclear reactor'
_diffrn_source_type              'ILL, beam tube H11'
_exptl_absorpt_coefficient_mu    0.014
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
correction for a cylindrical sample with \mR = 0.042 as implemented in
 JANA2006 (Pet\<r\'i\<cek et al., 2014)
;
_exptl_crystal_density_diffrn    2.8008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             37.799
_pd_calc_method                  'Rietveld refinement'
_pd_char_atten_coef_mu_calc      0.008
_pd_char_colour                  grey-black
_pd_instr_2theta_monochr_pre     135
_pd_instr_beam_size_ax           50
_pd_instr_beam_size_eq           20
_pd_instr_dist_src/mono          3000
_pd_instr_geometry               Debye-Scherrer
_pd_instr_location
;
D2B, high-resolution two-axis diffractometer, Institut Laue-Langevin
 (Grenoble, France)
;
_pd_instr_monochr_pre_spec       'Ge 335'
_pd_instr_slit_ax_mono/spec      2985
_pd_instr_slit_eq_mono/spec      500
_pd_instr_soller_eq_spec/detc    0.083333
_pd_instr_soller_eq_src/mono     0.166667
_pd_meas_2theta_range_inc        0.05
_pd_meas_2theta_range_max        159.950
_pd_meas_2theta_range_min        0.050
_pd_meas_number_of_points        3199
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.05
_pd_proc_2theta_range_max        159.45
_pd_proc_2theta_range_min        7.55
_pd_proc_ls_background_function
;
manual background (visual estimation, unrefined) interpolated by 10 Legendre
 polynomials [1st: 0.1(2), 2nd: -0.9(4), 3rd: -1.0(5), 4th: -0.7(6),
 5th: -2.0(7), 6th: 2.3(7), 7th: 2.5(8), 8th: 2.8(8), 9th: 4.1(8),
 10th: 4.5(8)]
;
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
;
pseudo-Voigt profile according to Thompson, Cox & Hastings (1987):
 G~U~ = 46.3(16), G~V~ = -277.8544, G~W~ = 325(4), L~X~ = 12.5(2), L~Y~ = 0;
asymmetry correction according to Howard (1982): P = 16.3(3)
;
_pd_proc_ls_prof_R_factor        0.0195
_pd_proc_ls_prof_wR_expected     0.0176
_pd_proc_ls_prof_wR_factor       0.0257
_pd_proc_wavelength              1.594
_pd_spec_mounting                'compacted powder in vanadium can'
_pd_spec_mount_mode              transmission
_pd_spec_orientation             horizontal
_pd_spec_preparation             'grinding in an agate mortar'
_pd_spec_shape                   cylinder
_pd_spec_size_axial              49.8
_pd_spec_size_equat              13.9
_refine_diff_density_max         0.13
_refine_diff_density_min         -0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.46
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     26
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0297
_refine_ls_R_I_factor            0.0462
_refine_ls_shift/su_max          0.0085
_refine_ls_shift/su_mean         0.0025
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_details     w=1/[\s^2^(I)+(0.01*I)^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0351
_refine_ls_wR_factor_gt          0.0349
_reflns_number_gt                74
_reflns_number_total             79
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c9ra05690d2.cif
_cod_data_source_block           nd-300C
_cod_original_cell_volume        219.651(9)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7233626