Cationic Clathrate of Type-III Ge172-xPxTey (y~ 21.5,x~ 2y): Synthesis, Crystal Structure and Thermoelectric Properties
Maria A. Kirsanova; Takao Mori; Satofumi Maruyama; Artem M. Abakumov; Gustaaf Van Tendeloo; Andrei Olenev; Andrei V. Shevelkov; Inorganic Chemistry 52 (2013) 8272–8279; doi:10.1021/ic401203r

data_4335512
_publ_contact_author_address
;
Moscow State University
Department of Chemistry
Leninskie Gory 1 build. 3 GSP-1
119991 Moscow
Russia
;
_publ_contact_author_email       kirsanova@inorg.chem.msu.ru
_publ_contact_author_name        'Maria A. Kirsanova'
_publ_contact_author_phone       '007 495 939-1200'
_publ_section_title
;
 Cationic Clathrate of Type-III Ge172-xPxTey (y~ 21.5,x~ 2y): Synthesis,
 Crystal Structure and Thermoelectric Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8272
_journal_page_last               8279
_journal_paper_doi               10.1021/ic401203r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Ge129.28 P42.72 Te21.53'
_chemical_formula_sum            'Ge129.28 P42.72 Te21.53'
_chemical_formula_weight         13454.70
_chemical_name_common            'germanium-phosphor telluride'
_chemical_name_systematic        'germanium-phosphor telluride'
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_atom_sites_solution_hydrogens   none
_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            1
_cell_length_a                   19.948(3)
_cell_length_b                   19.948(3)
_cell_length_c                   10.440(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.12
_cell_measurement_theta_min      15.83
_cell_volume                     4154.3(12)
_computing_cell_refinement       'CAD4 (Nonius)'
_computing_data_collection       'CAD4 (Nonius)'
_computing_data_reduction        'XCAD7 (P.McArdle, 1999)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6387
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    27.098
_exptl_absorpt_correction_T_max  0.4103
_exptl_absorpt_correction_T_min  0.2932
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             5897
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.788
_refine_diff_density_min         -2.612
_refine_diff_density_rms         0.485
_refine_ls_extinction_coef       0.00014(3)
_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   1.059
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                2155
_reflns_number_total             3294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401203r_si_002.cif
_cod_data_source_block           xl3
_cod_database_code               4335512