Structural and Thermodynamic Similarities of Phases in the Li‒Tt (Tt = Si, Ge) Systems: Redetermination of the Lithium-Rich Side of the Li‒Ge Phase Diagram and Crystal Structures of Li17Si4.0−xGex for x = 2.3, 3.1, 3.5, and 4 as well as Li4.1Ge
Fässler, Thomas F; Zeilinger, Michael; Dalton Transactions  (2014) –; doi:10.1039/c4dt00743c

data_7030895
_publ_section_title
;
 Structural and Thermodynamic Similarities of Phases in the Li--Tt (Tt =
 Si, Ge) Systems: Redetermination of the Lithium-Rich Side of the Li--Ge
 Phase Diagram and Crystal Structures of Li17Si4.0&#x2212;xGex for x =
 2.3, 3.1, 3.5, and 4 as well as Li4.1Ge
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/c4dt00743c
_journal_year                    2014
_chemical_formula_analytical     'Ge3.08 Li17 Si0.92'
_chemical_formula_moiety         'Ge3.08 Li17 Si0.92'
_chemical_formula_sum            'Ge3.08 Li17 Si0.92'
_chemical_formula_weight         367.44
_chemical_name_common            'Lithium Tetrelide'
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      216
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 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            20
_cell_length_a                   18.7515(2)
_cell_length_b                   18.7515(2)
_cell_length_c                   18.7515(2)
_cell_measurement_reflns_used    15558
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.9248
_cell_measurement_theta_min      3.0655
_cell_volume                     6593.38(12)
_citation_year                   2014
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'Diamond 3.2i (Crystal Impact 2012)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate Sapphire3'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford-Diffraction Xcalibur3 '
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    6.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic silver'
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3249
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(5)
_refine_ls_extinction_coef       0.00024(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   1.000
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                880
_reflns_number_total             952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00743c4.cif
_cod_data_source_block           Li17Si2Ge2_123K
_cod_database_code               7030895
_cell_oxdiff_twin_number         2