Lithium metal atoms fill vacancies in the germanium network of a type-I clathrate: Synthesis and structural characterization of Ba8Li5Ge41
Ghosh, Kowsik; Ovchinnikov, Alexander; Baitinger, Michael; Krnel, Mitja; Burkhardt, Ulrich; Grin, Yuri; Bobev, Svilen; Dalton Transactions  (2023) –; doi:10.1039/D3DT01168B

data_7713082
_publ_section_title
;
 Lithium metal atoms fill vacancies in the germanium network of a type-I
 clathrate: Synthesis and structural characterization of Ba8Li5Ge41
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01168B
_journal_year                    2023
_chemical_formula_moiety         '2(C33 H37 Al N4 O2), 3(C7 H8)'
_chemical_formula_sum            'C87 H98 Al2 N8 O4'
_chemical_formula_weight         1373.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                110.884(3)
_cell_angle_beta                 110.057(3)
_cell_angle_gamma                104.529(4)
_cell_formula_units_Z            1
_cell_length_a                   12.4063(12)
_cell_length_b                   13.7450(12)
_cell_length_c                   14.0446(13)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.55
_cell_volume                     1902.5(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            90466
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.606
_diffrn_reflns_theta_min         2.554
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.9397.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             734
_exptl_crystal_recrystallization_method
'The material was recrystallised from toluene by slow evaporation'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.332
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.3851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             8806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01168b2.cif
_cod_data_source_block           compound_3b
_cod_database_code               7713082
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C1'B)=Sof(C6'B)=Sof(H6'B)=Sof(C5'B)=Sof(H5'B)=Sof(C4'B)=Sof(H4'B)=
 Sof(C3'B)=Sof(H3'B)=Sof(C2'B)=Sof(C7'B)=Sof(H7'G)=Sof(H7'H)=Sof(H7'I)=1-FVAR(1)
 Sof(C1'A)=Sof(C2'A)=Sof(C3'A)=Sof(H3'A)=Sof(C4'A)=Sof(H4'A)=Sof(C5'A)=
 Sof(H5'A)=Sof(C6'A)=Sof(H6'A)=Sof(C7'A)=Sof(H7'D)=Sof(H7'E)=Sof(H7'F)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C19A)=Sof(H19A)=Sof(C18A)=
 Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=Sof(C20A)=
 Sof(H20A)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(H23)=Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(2)
 Fixed Sof: C14(0.5) H14(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5)
 C16(0.5) H16(0.5) C15(0.5) H15(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3'A(H3'A), C4'A(H4'A), C5'A(H5'A), C6'A(H6'A), C6'B(H6'B), C5'B(H5'B),
 C4'B(H4'B), C3'B(H3'B), C3(H3), C3'(H3'), C3A(H3A), C4(H4), C4'(H4'), C4A(H4A),
  C5(H5), C5'(H5'), C5A(H5A), C6(H6), C6'(H6'), C6A(H6A), C14(H14), C13(H13),
 C12(H12), C16(H16), C15(H15), C21(H21), C22(H22), C23(H23), C19(H19), C20(H20),
  C19A(H19A), C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A)
3.b Fitted hexagon refined as free rotating group:
 C1'A(C2'A,C3'A,C4'A,C5'A,C6'A), C1'B(C6'B,C5'B,C4'B,C3'B,C2'B), C14(C13,C12,
 C11,C16,C15), C21(C22,C23,C18,C19,C20), C19A(C18A,C23A,C22A,C21A,C20A)
3.c Idealised Me refined as rotating group:
 C7'(H7'A,H7'B,H7'C), C7'A(H7'D,H7'E,H7'F), C7'B(H7'G,H7'H,H7'I), C8(H8A,H8B,
 H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,
 H10C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              25779
_shelx_hkl_checksum              79039
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'