Structure determination of KScS~2~, RbScS~2~ and KLnS~2~ (Ln = Nd, Sm, Tb, Dy, Ho, Er, Tm and Yb) and crystal‒chemical discussion
Havlák, Lubomír; Fábry, Jan; Henriques, Margarida; Dušek, Michal; Acta Crystallographica Section C 71 (2015) 623–630; doi:10.1107/S2053229615011833

data_2020016
_publ_section_title
;
 Structure determination of KScS~2~, RbScS~2~ and KLnS~2~ (Ln = Nd, Sm,
 Tb, Dy, Ho, Er, Tm and Yb) and crystal--chemical discussion
;
_journal_coeditor_code           FA3364
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              623
_journal_page_last               630
_journal_paper_doi               10.1107/S2053229615011833
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'K1 Yb1 S2'
_chemical_formula_moiety         'K1 S2 Yb1'
_chemical_formula_sum            'K S2 Yb'
_chemical_formula_weight         276.3
_chemical_name_systematic
;
Potassium ytterbium sulfide
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   3.9615(8)
_cell_length_b                   3.9615(8)
_cell_length_c                   21.810(3)
_cell_measurement_reflns_used    582
_cell_measurement_temperature    301.00(15)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      5.56
_cell_volume                     296.42(9)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_publication_material
;
<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_refinement
;
<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      301
_diffrn_detector_area_resol_mean 5.1873
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Xcalibur Gemini Ultra diffractometer with Atlas detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            444
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         5.61
_exptl_absorpt_coefficient_mu    25.519
_exptl_absorpt_correction_T_max  0.1927
_exptl_absorpt_correction_T_min  0.0988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(<i>JANA2006</i>; Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.6428
_exptl_crystal_description       plate
_exptl_crystal_F_000             363
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.42
_refine_diff_density_min         -2.15
_refine_ls_abs_structure_details
;
Refinement of a model with
obverse--reverse twinning turned out to be insignificant
;
_refine_ls_extinction_coef       39E2(4)
_refine_ls_extinction_method
;
B-C type 1 Lorentzian isotropic
[Becker, P. J. & Coppens, P. (1974). <i>Acta Cryst.</i> A<b>30</b>, 129--147]
;
_refine_ls_goodness_of_fit_ref   1.65
_refine_ls_number_constraints    0
_refine_ls_number_parameters     9
_refine_ls_number_reflns         124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.0025
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(I) + 0.0004I^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                124
_reflns_number_total             124
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fa3364sup1.cif
_cod_data_source_block           X
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'K1 S2 Yb1'
_cod_database_code               2020016
_cod_database_fobs_code          2020016