Synthesis, Crystal Structure, and Physical Properties of the Type-I Clathrate Ba8-δNix( )ySi46-x-y
U. Aydemir; C. Candolfi; A. Ormeci; H. Borrmann; U. Burkhardt; Y. Oztan; N. Oeschler; M. Baitinger; F. Steglich; Yu. Grin; Inorganic Chemistry 51 (2012) 4730–4741; doi:10.1021/ic2027626

data_4328968
_publ_contact_author_address
;
Max-Planck-Institut f\"ur Chemische Physik fester Stoffe
N\"othnitzer Str. 40
D-01187 Dresden
Germany
;
_publ_contact_author_email       grin@cpfs.mpg.de
_publ_contact_author_fax         49(351)46464000
_publ_contact_author_name        'Yuri Grin'
_publ_contact_author_phone       49(351)46464249
_publ_section_title
;
 Synthesis, Crystal Structure, and Physical Properties of the Type-I
 Clathrate Ba8-\dNix( )ySi46-x-y
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4730
_journal_page_last               4741
_journal_paper_doi               10.1021/ic2027626
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'Prepared by annealing at 1000 # degree C'
_chemical_formula_analytical     'Ba8.00(2) Ni3.17(1) Si43.03(2)'
_chemical_formula_sum            'Ba8 Ni3.2 Si42.4'
_chemical_formula_weight         2477.25
_chemical_melting_point          1373
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      223
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.2922(1)
_cell_length_b                   10.2922(1)
_cell_length_c                   10.2922(1)
_cell_measurement_radiation      CuK\a1
_cell_measurement_reflns_used    66
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      1.5
_cell_measurement_wavelength     1.540598
_cell_volume                     1090.246(18)
_computing_cell_refinement       WinCSD
_computing_data_collection       'CrystalClear (Rigaku Inc. 2005)'
_computing_data_reduction        'CrystalClear (Rigaku Inc. 2005)'
_computing_publication_material
;
Akselrud, L.G., Zavalii, P.Y., Grin, Yu.N.,                                    
Pecharsky, V.K., Baumgartner, B., W\"olfel, E.
(1993) Materials Science Forum, v.133-136, 335-340  
;
_computing_structure_refinement  WinCSD
_computing_structure_solution    WinCSD
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'RIGAKU Spider'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7263
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    5.01
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8565
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            metallic-grey
_exptl_crystal_density_diffrn    3.7764
_exptl_crystal_description       plate
_exptl_crystal_F_000             1131
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method
;
gaussian isotropic
P.J. Becker, P. Coppens, Acta Crystallogr. A 30 (1974) 129-153
;
_refine_ls_goodness_of_fit_ref   1.70
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         503
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0233
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_all         0.1081
_refine_ls_wR_factor_ref         0.0387
_reflns_number_total             4417
_reflns_threshold_expression     'F~o~ > 4\s(F~o~)'
_cod_data_source_file            ic2027626_si_003.cif
_cod_data_source_block           global
_cod_original_cell_volume        1090.24(3)
_cod_original_formula_sum        'Ba8.0 Ni3.2 Si42.4'
_cod_database_code               4328968