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_7030893
_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     'Ge2.30 Li17 Si1.70'
_chemical_formula_moiety         'Ge2.30 Li17 Si1.70'
_chemical_formula_sum            'Ge2.3 Li17 Si1.7'
_chemical_formula_weight         332.69
_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                   18.7125(1)
_cell_length_b                   18.7125(1)
_cell_length_c                   18.7125(1)
_cell_measurement_reflns_used    17391
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.7863
_cell_measurement_theta_min      3.0711
_cell_volume                     6552.33(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0096
_diffrn_reflns_limit_h_max       14
_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            31663
_diffrn_reflns_theta_full        30.45
_diffrn_reflns_theta_max         30.45
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    5.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38559
_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    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(3)
_refine_ls_extinction_coef       0.00044(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   1.260
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+1.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0357
_reflns_number_gt                991
_reflns_number_total             1035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00743c5.cif
_cod_data_source_block           Li17Si3Ge1_123K
_cod_original_formula_sum        'Ge2.30 Li17 Si1.70'
_cod_database_code               7030893