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_7706538
_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         'C56 H142 Ge6 Li2 O4 Si12 Te8'
_chemical_formula_sum            'C56 H142 Ge6 Li2 O4 Si12 Te8'
_chemical_formula_weight         2686.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-21
_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                 99.818(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4374(12)
_cell_length_b                   21.327(3)
_cell_length_c                   25.337(3)
_cell_measurement_reflns_used    2363
_cell_measurement_temperature    150
_cell_measurement_theta_max      19.891
_cell_measurement_theta_min      2.389
_cell_volume                     5024.9(11)
_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      150.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0994
_diffrn_reflns_av_unetI/netI     0.1075
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.225
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1173 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.8177. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       plank
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         9865
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5967
_reflns_number_total             9865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04280c2.cif
_cod_data_source_block           78
_cod_depositor_comments
'Adding full bibliography for 7706536--7706539.cif.'
_cod_original_cell_volume        5024.8(11)
_cod_database_code               7706538
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C402 \\sim C406: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02
C405 \\sim C408: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C406) \\sim Ueq, Uanis(C402) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C404) \\sim Ueq, Uanis(C407) \\sim Ueq, Uanis(C408) \\sim Ueq,
Uanis(C405) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C402)=Sof(H40A)=Sof(H40B)=Sof(H40F)=Sof(H40G)=Sof(H40H)=Sof(C404)=
 Sof(H40I)=Sof(H40J)=Sof(C405)=Sof(H40K)=Sof(H40L)=Sof(H40M)=1-FVAR(1)
 Sof(H40C)=Sof(H40D)=Sof(H40E)=Sof(C406)=Sof(H40N)=Sof(H40O)=Sof(C407)=
 Sof(H40P)=Sof(H40Q)=Sof(C408)=Sof(H40R)=Sof(H40S)=Sof(H40T)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C402(H40A,H40B), C404(H40I,
 H40J), C406(H40N,H40O), C407(H40P,H40Q)
4.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C131(H13A,H13B,H13C),
 C132(H13D,H13E,H13F), C133(H13G,H13H,H13I), C211(H21A,H21B,H21C), C212(H21D,
 H21E,H21F), C213(H21G,H21H,H21I), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F),
 C223(H22G,H22H,H22I), C231(H23A,H23B,H23C), C232(H23D,H23E,H23F), C233(H23G,
 H23H,H23I), C403(H40C,H40D,H40E), C403(H40F,H40G,H40H), C405(H40K,H40L,H40M),
 C408(H40R,H40S,H40T)
;
_shelx_res_checksum              19764
_shelx_hkl_checksum              25627
_olex2_submission_special_instructions 'No special instructions were received'