Crystal Structure and Thermoelectric Properties of the (7,7)L Lillianite Homologue Pb6Bi2Se9.
Casamento, Joseph; Lopez, Juan S.; Moroz, Nicholas A.; Olvera, Alan; Djieutedjeu, Honore; Page, Alexander; Uher, Ctirad; Poudeu, Pierre F. P.; Inorganic chemistry 56 (2017) 261–268; doi:10.1021/acs.inorgchem.6b02118

data_4345134
_publ_section_title
;
 Crystal Structure and Thermoelectric Properties of the (7,7)L Lillianite
 Homologue Pb6Bi2Se9.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              261
_journal_page_last               268
_journal_paper_doi               10.1021/acs.inorgchem.6b02118
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'Bi2 Pb6 Se9'
_chemical_formula_sum            'Bi2 Pb6 Se9'
_chemical_formula_weight         2371.74
_chemical_name_systematic
; 
Lead Bismuth Selenide (6/2/9)
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.2567(9)
_cell_length_b                   14.105(3)
_cell_length_c                   32.412(7)
_cell_measurement_reflns_used    725
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.49
_cell_volume                     1946.0(7)
_computing_cell_refinement       'CELL (STOE & Cie GmbH, Darmstadt, 2000)'
_computing_data_collection       'EXPOSE (STOE & Cie GmbH, Darmstadt, 2000)'
_computing_data_reduction
'INTEGRATE (STOE & Cie GmbH, Darmstadt, 2000)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'IPDS-2T Stoe'
_diffrn_measurement_method
'fixed phi and incremental omega oscillation 0.5 degree, 5 min exposure time'
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            3511
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    86.536
_exptl_absorpt_correction_T_max  0.167
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
crystal description from video camera using FACEIT 
(STOE & Cie GmbH, Darmstadt, 2003) and optimized with X-SHAPE 
(STOE & Cie GmbH, Darmstadt, 2003) 
using set of equivalent reflections 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    8.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.435
_refine_diff_density_min         -2.861
_refine_diff_density_rms         0.452
_refine_ls_extinction_coef       0.00010(2)
_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   1.210
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+96.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                1191
_reflns_number_total             1256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02118_si_001.cif
_cod_data_source_block           Pb6Bi2Se9-300K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               4345134