Wet-Environment-Induced Structural Alterations in Single- and Polycrystalline LLZTO Solid Electrolytes Studied by Diffraction Techniques
Redhammer, Günther J.; Badami, Pavan; Meven, Martin; Ganschow, Steffen; Berendts, Stefan; Tippelt, Gerold; Rettenwander, Daniel; ACS Applied Materials & Interfaces  (2020) –; doi:10.1021/acsami.0c16016

data_4518352
_publ_section_title
;
 Wet-Environment-Induced Structural Alterations in Single- and
 Polycrystalline LLZTO Solid Electrolytes Studied by Diffraction
 Techniques
;
_journal_name_full               'ACS Applied Materials &amp; Interfaces'
_journal_paper_doi               10.1021/acsami.0c16016
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'La2.93 Li3.59 H1.74 Ta0.95 Zr1.05 O12'
_chemical_formula_sum            'H1.74 La2.93 Li3.59 O12 Ta0.95 Zr1.05'
_chemical_formula_weight         893.34
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      220
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2020-05-29T12:04:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9536(2)
_cell_length_b                   12.9536(2)
_cell_length_c                   12.9536(2)
_cell_measurement_reflns_used    33607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.495
_cell_measurement_theta_min      3.853
_cell_measurement_wavelength     0.71073
_cell_volume                     2173.56(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2012)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2012)'
_computing_molecular_graphics    'Diamonds 3.2g (Brandenburg,2006)'
_computing_publication_material  'WinGX v1.70.01 (Farrugia 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method
'rotation, \w-scans at 4 different \f positions'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33607
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.495
_diffrn_reflns_theta_min         3.853
_exptl_absorpt_coefficient_mu    21.827
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'multiscan correction with APEX2 software (Bruker 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             3099.9
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_coef       0.00019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     49
_refine_ls_number_reflns         890
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.017
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+11.4938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0337
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.99
_reflns_number_gt                862
_reflns_number_total             890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c16016_si_004.cif
_cod_data_source_block           S-LLZTO_363K_2d
_cod_original_cell_volume        2173.56(10)
_cod_original_formula_sum        'La2.93 Li3.59 H1.74 Ta0.95 Zr1.05 O12'
_cod_database_code               4518352
_shelx_shelxl_version_number     2014/7