High-pressure high-temperature synthesis and crystal structure of the isotypic rare earth (RE)‒thioborate‒sulfides RE9[BS3]2[BS4]3S3, (RE=Dy‒Lu)
Borna, Marija; Hunger, Jens; Ormeci, Alim; Zahn, Dirk; Burkhardt, Ulrich; Carrillo-Cabrera, Wilder; Cardoso-Gil, Raul; Kniep, Rüdiger; Journal of Solid State Chemistry 184 (2011) 296–303; doi:10.1016/j.jssc.2010.11.004

data_1563312
_publ_section_title
;
 High-pressure high-temperature synthesis and crystal structure of the
 isotypic rare earth (RE)--thioborate--sulfides RE9[BS3]2[BS4]3S3,
 (RE=Dy--Lu)
;
_journal_issue                   2
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              296
_journal_page_last               303
_journal_paper_doi               10.1016/j.jssc.2010.11.004
_journal_volume                  184
_journal_year                    2011
_chemical_formula_moiety         'B3.33 S14 Tm6'
_chemical_formula_structural     'Tm9 (B S3)2 (B S4)3 S3 '
_chemical_formula_sum            'B3.33 S14 Tm6'
_chemical_formula_weight         1498.56
_chemical_name_systematic        'Thulium thioborate'
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            1
_cell_length_a                   9.2869(3)
_cell_length_b                   9.2869
_cell_length_c                   5.8781(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    298
_cell_measurement_theta_max      42.457
_cell_measurement_theta_min      1.500
_cell_volume                     439.05(3)
_computing_structure_refinement  GSAS
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'STOE StadiP-MP diffractometer'
_diffrn_radiation_monochromator  'curved germanium (111)'
_diffrn_radiation_polarisn_ratio 0.644
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.540594
_exptl_absorpt_coefficient_mu    69.57
_exptl_crystal_density_diffrn    5.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             654
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  'light orange'
_pd_char_particle_morphology     'size < 0.40mm'
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        109.98
_pd_meas_2theta_range_min        10.0
_pd_meas_number_of_points        5000
_pd_meas_scan_method             step
_pd_phase_name                   Tm9B5S21
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        109.98
_pd_proc_2theta_range_min        10.0
_pd_proc_ls_background_function
;  
 GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    7074.38     2:   -8604.41     3:    4374.30     4:   -1121.21    
      5:   -487.360     6:    949.032     7:   -551.105     8:   -28.2613    
      9:    309.253    10:   -395.666    11:    272.778    12:   -35.6928    
     13:   -143.514    14:    198.310    15:   -175.590    16:    69.6497    
     17:    13.5423    18:   -62.3871    19:    72.2612    20:   -69.4309    
;
_pd_proc_ls_peak_cutoff          0.00001
_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =   40.054 #2(GV)   =  -28.877 #3(GW)   =   11.114
 #4(GP)   =    7.034 #5(LX)   =    3.806 #6(LY)   =    6.107
 #7(S/L)  =   0.0077 #8(H/L)  =   0.0077
 #9(trns) =    -2.11 #10(shft)=   2.2634
 #11(stec)=     5.98 #12(ptec)=     0.18 #13(sfec)=     0.00
 #14(L11) =   -0.042 #15(L22) =   -0.020 #16(L33) =   -0.079
 #17(L12) =   -0.011 #18(L13) =   -0.074 #19(L23) =   -0.121
 Peak tails are ignored  where the intensity is below 0.0000 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0228
_pd_proc_ls_prof_wR_expected     0.0128
_pd_proc_ls_prof_wR_factor       0.0301
_pd_proc_number_of_points        5000
_pd_spec_mounting                capillary
_pd_spec_mount_mode              transmission
_refine_ls_goodness_of_fit_all   1.58
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     15
_refine_ls_number_restraints     3
_refine_ls_R_Fsqd_factor         0.02413
_refine_ls_shift/su_max          0.06
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_scheme      calc
_reflns_d_resolution_high        1.096
_reflns_d_resolution_low         4.746
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_total             136
_cod_data_source_file            JSSC-2011-184-296.cif
_cod_data_source_block           Tm9B5S21
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'N' was changed to 'n' in
accordance with the built-in table derived from the CIF Core
dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21 (48 times).

data item '_geom_bond_publ_flag' value 'N' was changed to 'n' in
accordance with the built-in table derived from the CIF Core
dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21 (26 times).

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        439.03(3)
_cod_database_code               1563312