LiBi3S5—A lithium bismuth sulfide with strong cation disorder
Nakhal, Suliman; Wiedemann, Dennis; Stanje, Bernhard; Dolotko, Oleksandr; Wilkening, Martin; Lerch, Martin; Journal of Solid State Chemistry 238 (2016) 60–67; doi:10.1016/j.jssc.2016.03.010

data_1561480
_publ_section_title
;
 LiBi3S5---A lithium bismuth sulfide with strong cation disorder
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              60
_journal_page_last               67
_journal_paper_doi               10.1016/j.jssc.2016.03.010
_journal_volume                  238
_journal_year                    2016
_chemical_formula_iupac          'Bi3 Li S5'
_chemical_formula_structural     'Li Bi3 S5'
_chemical_formula_sum            'Bi3 Li S5'
_chemical_formula_weight         794.2
_chemical_name_structure_type    AgBi~3~S~5~
_chemical_name_systematic        'lithium tribismuth pentasulfide'
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.0723(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1079(2)
_cell_length_b                   4.00070(7)
_cell_length_c                   16.5085(3)
_cell_measurement_temperature    298
_cell_volume                     863.53(3)
_computing_cell_refinement       'FullProf (Rodr\'iguez-Carvajal, 1993)'
_computing_data_collection       'CARESS (Busse et al., 2013)'
_computing_data_reduction        'DATAPARSER (Senyshyn, 2011)'
_computing_molecular_graphics    'Diamond 3.2 (Brandenburg & Putz, 2014)'
_computing_publication_material  'WinPLOTR (Roisnel, 2001)'
_computing_structure_refinement  'FullProf (Rodr\'iguez-Carvajal, 1993)'
_computing_structure_solution    'CSD (Bergerhoff & Brown, 1987)'
_diffrn_ambient_temperature      298
_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 area detector'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.54831
_diffrn_source                   'nuclear reactor'
_diffrn_source_type              'FRM II beamline 8a'
_exptl_absorpt_coefficient_mu    0.0297
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
; correction for a cylindrical sample with \mR = 0.0850 as
implemented in FullProf
;
_exptl_crystal_density_diffrn    6.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             151.724
_pd_calc_method                  'Rietveld refinement'
_pd_char_atten_coef_mu_calc      0.0178
_pd_char_colour                  grey-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 bei 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        152.90
_pd_meas_2theta_range_min        0.95
_pd_meas_number_of_points        3020
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.05
_pd_proc_2theta_range_max        151.815
_pd_proc_2theta_range_min        0.865
_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_info_excluded_regions   'from 0.00 to 4.00\%: inclined inset'
_pd_proc_ls_background_function
; interpolation by cubic splines between 20 manually defined background points
with previously refined heights
;
_pd_proc_ls_peak_cutoff          0.005
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
; pseudo-Voigt function with U = 0.064(3), V = -0.081(5), W = 0.140(2),
\h~0~ = 0.098(16), X = 0.0018(3); one-term asymmetry correction with
P~1~ = 0.083(8), P~2~ = 0.024(2) on reflections with 2\q < 160\%
;
_pd_proc_ls_prof_R_factor        0.0160
_pd_proc_ls_prof_wR_expected     0.0125
_pd_proc_ls_prof_wR_factor       0.0190
_pd_proc_number_of_points        2958
_pd_proc_wavelength              1.54381
_pd_spec_mounting                'compacted powder in vanadium can'
_pd_spec_mount_mode              transmission
_pd_spec_orientation             vertical
_pd_spec_shape                   cylinder
_pd_spec_size_axial              40
_pd_spec_size_equat              9
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.52
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    4
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1094
_refine_ls_number_restraints     1
_refine_ls_R_I_factor            0.0367
_refine_ls_shift/su_max          0.0114
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0216
_cod_data_source_file            JSSC-2016-238-60.cif
_cod_data_source_block           LiBi3S5
_cod_database_code               1561480
_pd_proc_ls_prof_cr_factor       0.0713
_pd_proc_ls_prof_cwr_factor      0.0618
_pd_proc_ls_prof_cwr_expected    0.0406
_pd_proc_ls_prof_chi2            2.3184
_pd_proc_ls_prof_echi2           2.3184