#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/00/2020016.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2020016
loop_
_publ_author_name
'Havlák, Lubomír'
'Fábry, Jan'
'Henriques, Margarida'
'Dušek, Michal'
_publ_section_title
;
 Structure determination of KScS₂, RbScS₂ and KLnS₂ (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
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_publication_material
;
JANA2006 (Petříček et al., 2014)
;
_computing_structure_refinement
;
JANA2006 (Petříček et al., 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       ω
_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
;
(JANA2006; Petříček et al., 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). Acta Cryst. A30, 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/[σ²(I) + 0.0004I²]'
_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>3σ(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
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 y,x,-z
5 x-y,-y,-z
6 -x,-x+y,-z
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 -y,-x,z
11 -x+y,y,z
12 x,x-y,z
13 x+2/3,y+1/3,z+1/3
14 -y+2/3,x-y+1/3,z+1/3
15 -x+y+2/3,-x+1/3,z+1/3
16 y+2/3,x+1/3,-z+1/3
17 x-y+2/3,-y+1/3,-z+1/3
18 -x+2/3,-x+y+1/3,-z+1/3
19 -x+2/3,-y+1/3,-z+1/3
20 y+2/3,-x+y+1/3,-z+1/3
21 x-y+2/3,x+1/3,-z+1/3
22 -y+2/3,-x+1/3,z+1/3
23 -x+y+2/3,y+1/3,z+1/3
24 x+2/3,x-y+1/3,z+1/3
25 x+1/3,y+2/3,z+2/3
26 -y+1/3,x-y+2/3,z+2/3
27 -x+y+1/3,-x+2/3,z+2/3
28 y+1/3,x+2/3,-z+2/3
29 x-y+1/3,-y+2/3,-z+2/3
30 -x+1/3,-x+y+2/3,-z+2/3
31 -x+1/3,-y+2/3,-z+2/3
32 y+1/3,-x+y+2/3,-z+2/3
33 x-y+1/3,x+2/3,-z+2/3
34 -y+1/3,-x+2/3,z+2/3
35 -x+y+1/3,y+2/3,z+2/3
36 x+1/3,x-y+2/3,z+2/3
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
K K 0 0 0 0.0133(13) Uani d 1
Yb Yb 0.333333 0.666667 0.166667 0.0063(5) Uani d 1
S S 0 0 0.23346(19) 0.0072(10) Uani d 1
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K 0.2009 0.2494 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Yb -0.3850 5.5486 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 30 0.0472
0 -1 -30 0.0472
6 -4 -2 0.0581
-6 4 2 0.0581
1 4 -5 0.0558
-1 -4 5 0.0558
-1 0 29 0.0446
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
S K S 25_444 25_544 77.67(6)
S K S 25_444 25_554 77.67(6)
S K S 25_444 16_445 102.33(6)
S K S 25_444 16_455 102.33(6)
S K S 25_444 16_555 180.0(5)
S K S 25_544 25_554 77.67(6)
S K S 25_544 16_445 102.33(6)
S K S 25_544 16_455 180.0(5)
S K S 25_544 16_555 102.33(6)
S K S 25_554 16_445 180.0(5)
S K S 25_554 16_455 102.33(6)
S K S 25_554 16_555 102.33(6)
S K S 16_445 16_455 77.67(6)
S K S 16_445 16_555 77.67(6)
S K S 16_455 16_555 77.67(6)
S Yb S . 1_565 93.85(7)
S Yb S . 1_665 93.85(7)
S Yb S . 16_455 86.15(7)
S Yb S . 16_555 86.15(7)
S Yb S . 16_565 180.0(5)
S Yb S 1_565 1_665 93.85(7)
S Yb S 1_565 16_455 86.15(7)
S Yb S 1_565 16_555 180.0(5)
S Yb S 1_565 16_565 86.15(7)
S Yb S 1_665 16_455 180.0(5)
S Yb S 1_665 16_555 86.15(7)
S Yb S 1_665 16_565 86.15(7)
S Yb S 16_455 16_555 93.85(7)
S Yb S 16_455 16_565 93.85(7)
S Yb S 16_555 16_565 93.85(7)
K S K 13_445 13_455 77.67(8)
K S K 13_445 13_555 77.67(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
K S 25_444 3.159(3)
K S 25_544 3.159(3)
K S 25_554 3.159(3)
K S 16_445 3.159(3)
K S 16_455 3.159(3)
K S 16_555 3.159(3)
Yb S . 2.712(2)
Yb S 1_565 2.712(2)
Yb S 1_665 2.712(2)
Yb S 16_455 2.712(2)
Yb S 16_555 2.712(2)
Yb S 16_565 2.712(2)
S S 1_445 3.961(2)
S S 1_455 3.9615(16)
S S 1_545 3.9615(16)
S S 1_565 3.9615(16)
S S 1_655 3.9615(16)
S S 1_665 3.961(2)
S S 16_445 3.704(5)
S S 16_455 3.704(5)
S S 16_555 3.704(5)
