Structural Frustration and Occupational Disorder: The Rare Earth Metal Polysulfides Tb8S14.8, Dy8S14.9, Ho8S14.9, and Y8S14.8
Thomas Doert; Christian Graf; Inga G. Vasilyeva; Walter Schnelle; Inorganic Chemistry 51 (2012) 282–289; doi:10.1021/ic201639f

data_4327786
_publ_contact_author_address
;
Thomas Doert
Fachrichtung Chemie und Lebensmittelchemie
Technische Universit\"at Dresden
D-01062 Dresden
Germany
;
_publ_contact_author_email       Thomas.Doert@chemie.tu-dresden.de
_publ_contact_author_fax         49(351)463-37287
_publ_contact_author_phone       49(351)463-33864
_publ_section_title
;
 Structural Frustration and Occupational Disorder: The Rare Earth Metal
 Polysulfides Tb8S14.8, Dy8S14.9, Ho8S14.9, and Y8S14.8
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              282
_journal_page_last               289
_journal_paper_doi               10.1021/ic201639f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Y8 S14.73'
_chemical_formula_sum            'S11.048 Y6'
_chemical_formula_weight         887.6
_chemical_name_common            'Ytterbium polysulfide'
_chemical_name_systematic
;
Ytterbium polysulfide
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'A 2'
_symmetry_space_group_name_H-M   'A 1 1 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90.21(2)
_cell_formula_units_Z            8
_cell_length_a                   11.505(1)
_cell_length_b                   15.386(2)
_cell_length_c                   15.727(2)
_cell_measurement_reflns_used    19372
_cell_measurement_temperature    295
_cell_measurement_theta_max      32.32
_cell_measurement_theta_min      2.42
_cell_volume                     2783.9(6)
_computing_cell_refinement       'X-AREA, STOE, 2006'
_computing_data_collection       'X-AREA, STOE, 2006'
_computing_data_reduction        'X-AREA, STOE, 2006'
_computing_molecular_graphics
;
DIAMOND-Visuelles Informationssystem f\"ur Kristallstrukturen 
 (G. Bergerhoff, Bonn, 2010)
;
_computing_publication_material
'Jana2006 (Petricek, Dusek & Palatinus, 2010)'
_computing_structure_refinement
'Jana2006 (Petricek, Dusek & Palatinus, 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_details
; 
360 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33754
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         2.56
_diffrn_source
; 
sealed x-ray tube, 12 x 0.4 mm long-fine focus
;
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    26.35
_exptl_absorpt_correction_T_max  0.3213
_exptl_absorpt_correction_T_min  0.2026
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED, X-SHAPE, STOE 2006'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.23
_exptl_crystal_F_000             3281
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.06
_refine_diff_density_min         -1.53
_refine_ls_abs_structure_details
'  4615 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.374(15)
_refine_ls_extinction_coef       0.36(1)
_refine_ls_extinction_method
'B-C type 1 gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    2.43
_refine_ls_goodness_of_fit_ref   2.10
_refine_ls_number_constraints    16
_refine_ls_number_parameters     232
_refine_ls_number_reflns         9566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.0479
_refine_ls_shift/su_mean         0.0054
_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          0.1104
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                6529
_reflns_number_total             9566
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ic201639f_si_002_2.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'A 2z'
_cod_database_code               4327786