Synthesis and phase width of new quaternary selenides PbxSn6−xBi2Se9 (x=0‒4.36)
Chen, Kuei-Bo; Lee, Chi-Shen; Journal of Solid State Chemistry 183 (2010) 2616–2622; doi:10.1016/j.jssc.2010.08.034

data_1563408
_publ_section_title
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 Synthesis and phase width of new quaternary selenides
 PbxSn6&#x2212;xBi2Se9 (x=0--4.36)
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_journal_issue                   11
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              2616
_journal_page_last               2622
_journal_paper_doi               10.1016/j.jssc.2010.08.034
_journal_volume                  183
_journal_year                    2010
_chemical_formula_moiety         'Bi2 Se9 Sn6'
_chemical_formula_sum            'Bi2 Se9 Sn6'
_chemical_formula_weight         1840.74
_chemical_name_systematic        'tin bismuth selenium (6/2/9)'
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.2058(18)
_cell_length_b                   13.903(6)
_cell_length_c                   32.120(13)
_cell_measurement_reflns_used    1272
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.54
_cell_volume                     1878.2(14)
_computing_cell_refinement       'Bruker Smart Apex'
_computing_data_collection       'Bruker Smart Apex'
_computing_data_reduction        'Bruker Smart Apex'
_computing_molecular_graphics    'Bruker Shelxtl'
_computing_publication_material  'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            4772
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    43.925
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.405856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 The absorption correction used the SADABS program. 
 Sheldric, G. M. (1996). SADABS. Bruker Area Detector 
 Absorption Correction Software. University of Gottingen, Germany. 
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_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    6.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.901
_refine_diff_density_min         -3.611
_refine_diff_density_rms         0.989
_refine_ls_extinction_coef       0.00038(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2685
_refine_ls_wR_factor_ref         0.2877
_reflns_number_gt                707
_reflns_number_total             1272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-2616.cif
_cod_data_source_block           Sn6Bi2Se9
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_geom_bond_publ_flag' value 'No' was changed to 'no' 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 (22 times).

data item '_geom_bond_publ_flag' value 'Yes' was changed to 'yes' 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 (25 times).

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
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_cod_database_code               1563408