LiEC(SiMe<sub>3</sub>)<sub>3</sub> (E = Se, Te) as a new donor of chalcogen atoms for the generation of binary [(R<sub> <i>x</i> </sub>Ge<sub> <i>y</i> </sub>)E<sub> <i>z</i> </sub>] cage compounds with unique structural features.
Kunz, Tanja; Şahin, Orhan; Schrenk, Claudio; Schnepf, Andreas; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2663–2670; doi:10.1039/d0dt04280c

data_7706536
_publ_section_title
;
 LiEC(SiMe<sub>3</sub>)<sub>3</sub> (E = Se, Te) as a new donor of
 chalcogen atoms for the generation of binary [(R<sub> <i>x</i>
 </sub>Ge<sub> <i>y</i> </sub>)E<sub> <i>z</i> </sub>] cage compounds with
 unique structural features.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2663
_journal_page_last               2670
_journal_paper_doi               10.1039/d0dt04280c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C20 H56 Ge2 Si6 Te4'
_chemical_formula_sum            'C20 H56 Ge2 Si6 Te4'
_chemical_formula_weight         1120.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4299(11)
_cell_length_b                   11.7318(9)
_cell_length_c                   23.8209(19)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.727
_cell_measurement_theta_min      2.458
_cell_volume                     3753.1(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            118532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.459
_diffrn_reflns_theta_min         2.286
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.852
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1281 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8460. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0608P)^2^+33.6464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3226
_reflns_number_total             3873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04280c2.cif
_cod_data_source_block           53
_cod_depositor_comments
'Adding full bibliography for 7706536--7706539.cif.'
_cod_database_code               7706536
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All Te(H) groups
2. Uiso/Uaniso restraints and constraints
C121 \\sim C221: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C231) \\sim Ueq, Uanis(C131) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C221) \\sim Ueq, Uanis(C121) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C222) = Uanis(Te11)
Uanis(C132) = Uanis(Te12)
3. Others
 Fixed Sof: Te11(0.5) H11(0.5) Te12(0.5) H12(0.5) Ge1(0.5) Ge2(0.5) Si1(0.5)
 Si12(0.5) Si13(0.5) Si22(0.5) C121(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
 C122(0.5) H12D(0.5) H12E(0.5) H12F(0.5) H12J(0.5) H12K(0.5) H12L(0.5)
 H12G(0.5) H12H(0.5) H12I(0.5) C131(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C132(0.5) H13D(0.5) H13E(0.5) H13F(0.5) H13J(0.5) H13K(0.5) H13L(0.5)
 H13G(0.5) H13H(0.5) H13I(0.5) C221(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
 C222(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C231(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C232(0.5) H23D(0.5) H23E(0.5) H23F(0.5)
4.a Me refined with riding coordinates:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C123(H12J,H12K,H12L), C123(H12G,H12H,H12I),
 C131(H13A,H13B,H13C), C132(H13D,H13E,H13F), C133(H13J,H13K,H13L), C133(H13G,
 H13H,H13I), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F), C231(H23A,H23B,H23C),
 C232(H23D,H23E,H23F)
4.b Idealised tetrahedral OH refined as rotating group:
 Te11(H11), Te12(H12)
;
_shelx_res_checksum              83916
_shelx_hkl_checksum              33957
_olex2_submission_special_instructions 'No special instructions were received'