Structural and Electrochemical Properties of Type VIII Ba<sub>8</sub>Ga<sub>16-δ</sub>Sn<sub>30+δ</sub> Clathrate (δ ≈ 1) during Lithiation.
Dopilka, Andrew; Childs, Amanda; Ovchinnikov, Alexander; Zhao, Ran; Bobev, Svilen; Peng, Xihong; Chan, Candace K.; ACS applied materials & interfaces 13 (2021) 42564–42578; doi:10.1021/acsami.1c07240

data_4519041
_publ_section_title
;
 Structural and Electrochemical Properties of Type VIII
 Ba<sub>8</sub>Ga<sub>16-\d</sub>Sn<sub>30+\d</sub> Clathrate (\d &#x2248;
 1) during Lithiation.
;
_journal_issue                   36
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              42564
_journal_page_last               42578
_journal_paper_doi               10.1021/acsami.1c07240
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'Ba8 Ga14.893 Sn31.107'
_chemical_formula_sum            'Ba8 Ga14.89 Sn31.11'
_chemical_formula_weight         5829.30
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.5887(9)
_cell_length_b                   11.5887(9)
_cell_length_c                   11.5887(9)
_cell_measurement_reflns_used    1012
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      3.52
_cell_volume                     1556.3(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.380
_diffrn_reflns_theta_min         2.485
_diffrn_source_current           30.0
_diffrn_source_power             1.38
_diffrn_source_voltage           46.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.488
_exptl_absorpt_correction_T_max  0.2655
_exptl_absorpt_correction_T_min  0.1542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1515 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.5808.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    6.220
_exptl_crystal_description       block
_exptl_crystal_F_000             2465
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(12)
_refine_ls_extinction_coef       0.00177(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+2.8307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0335
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                453
_reflns_number_total             475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c07240_si_002.cif
_cod_data_source_block           mo_svib1610_0m
_cod_original_cell_volume        1556.3(4)
_cod_database_code               4519041
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.298
_shelx_estimated_absorpt_t_min   0.171
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(12)
 0.07(12)
2. Shared sites
{Sn2, Ga2}
{Sn1, Ga1}
{Sn3, Ga3}
{Sn4, Ga4}
3. Uiso/Uaniso restraints and constraints
Uanis(Sn2) = Uanis(Ga2)
Uanis(Sn1) = Uanis(Ga1)
Uanis(Sn3) = Uanis(Ga3)
Uanis(Sn4) = Uanis(Ga4)
4. Others
 Sof(Ga3)=0.16667*(1-FVAR(2))
 Sof(Sn3)=0.16667*FVAR(2)
 Sof(Ga4)=0.04167*(1-FVAR(3))
 Sof(Sn4)=0.04167*FVAR(3)
 Sof(Ga1)=0.5*(1-FVAR(4))
 Sof(Sn1)=0.5*FVAR(4)
 Sof(Ga2)=0.25*(1-FVAR(5))
 Sof(Sn2)=0.25*FVAR(5)
;
_shelx_res_checksum              50733
_shelx_hkl_checksum              8657
_olex2_submission_special_instructions 'No special instructions were received'