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_7706537
_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         'C40 H108 Ge6 Se10 Si12'
_chemical_formula_sum            'C40 H108 Ge6 Se10 Si12'
_chemical_formula_weight         2151.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-25
_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                 100.402(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9129(14)
_cell_length_b                   20.5298(17)
_cell_length_c                   13.9220(11)
_cell_measurement_reflns_used    5510
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.346
_cell_measurement_theta_min      2.270
_cell_volume                     5035.6(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 0.996
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26377
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.455
_diffrn_reflns_theta_min         1.487
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    5.546
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0936 before and 0.0377 after correction. The Ratio of minimum to maximum transmission is 0.7686. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         10533
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7218
_reflns_number_total             10533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04280c2.cif
_cod_data_source_block           92_sq
_cod_depositor_comments
'Adding full bibliography for 7706536--7706539.cif.'
_cod_database_code               7706537
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(2)
 0.07(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 Si24-C211 = Si21-C211
 1.98 with sigma of 0.02
 Si26-C217
 1.98 with sigma of 0.02
 Si26-C2 \\sim Si22-C2 \\sim Si25-C2 \\sim Si21-C2 \\sim Si24-C2 \\sim Si23-C2
\\sim Si36-C3 \\sim Si31-C3
 \\sim Si33-C3 \\sim Si35-C3 \\sim Si32-C3 \\sim Si34-C3
 with sigma of 0.02
 Si23-Si22 \\sim Si22-Si21 \\sim Si21-Si23 \\sim Si26-Si24 \\sim Si24-Si25
\\sim Si25-Si26
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Si32 \\sim Si35: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si33 \\sim Si36: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si21 \\sim Si25: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Si23) \\sim Ueq, Uanis(Si24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Si21) \\sim Ueq, Uanis(Si25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C220) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C318) \\sim Ueq, Uanis(C316) \\sim Ueq, Uanis(C317) \\sim Ueq,
Uanis(C314) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C313) \\sim Ueq,
Uanis(C312) \\sim Ueq, Uanis(C319) \\sim Ueq, Uanis(C315) \\sim Ueq: with sigma
of 0.03 and sigma for terminal atoms of 0.06
Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq, Uanis(C212) \\sim Ueq,
Uanis(C213) \\sim Ueq, Uanis(C214) \\sim Ueq, Uanis(C219) \\sim Ueq,
Uanis(C218) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C218) \\sim Ueq, Uanis(C217) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.005
Uanis(C211) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C214) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Si24)=Sof(Si25)=Sof(Si26)=Sof(Si34)=Sof(Si35)=Sof(Si36)=Sof(H6BA)=
 Sof(H7BA)=Sof(H8BA)=Sof(H21P)=Sof(H21Q)=Sof(H21R)=Sof(H21V)=Sof(H21W)=
 Sof(H21X)=Sof(HB)=Sof(HC)=Sof(HD)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(H21J)=
 Sof(H21K)=Sof(H21L)=Sof(C217)=Sof(H3AA)=Sof(H9BA)=Sof(H0CA)=Sof(HE)=Sof(HF)=
 Sof(HG)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(H31J)=Sof(H31K)=Sof(H31L)=Sof(H31P)=
 Sof(H31Q)=Sof(H31R)=Sof(HX)=Sof(HY)=Sof(HZ)=Sof(HS)=Sof(HT)=Sof(HU)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=Sof(H1BA)=Sof(H2BA)=Sof(H3BA)=Sof(H6AA)=Sof(H7AA)=
 Sof(H8AA)=Sof(H31V)=Sof(H31W)=Sof(H31X)=Sof(HN)=Sof(HO)=Sof(HP)=1-FVAR(1)
 Sof(Si21)=Sof(Si22)=Sof(Si23)=Sof(Si31)=Sof(Si32)=Sof(Si33)=Sof(H2AA)=
 Sof(H4BA)=Sof(H5BA)=Sof(H21M)=Sof(H21N)=Sof(H21O)=Sof(H21S)=Sof(H21T)=
 Sof(H21U)=Sof(H21Y)=Sof(H)=Sof(HA)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(H21G)=
 Sof(H21H)=Sof(H21I)=Sof(C218)=Sof(H21)=Sof(HJ)=Sof(HK)=Sof(H21Z)=Sof(HH)=
 Sof(HI)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(H31G)=Sof(H31H)=Sof(H31I)=Sof(H31M)=
 Sof(H31N)=Sof(H31O)=Sof(H31)=Sof(HV)=Sof(HW)=Sof(H31Z)=Sof(HQ)=Sof(HR)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(H1AA)=Sof(H9AA)=Sof(H0BA)=Sof(H0AA)=
 Sof(H4AA)=Sof(H5AA)=Sof(H31S)=Sof(H31T)=Sof(H31U)=Sof(H31Y)=Sof(HL)=Sof(HM)=
 FVAR(1)
6.a Me refined with riding coordinates:
 C211(H2AA,H4BA,H5BA), C211(H6BA,H7BA,H8BA), C212(H21M,H21N,H21O), C212(H21P,
 H21Q,H21R), C213(H21S,H21T,H21U), C213(H21V,H21W,H21X), C214(H21Y,H,HA),
 C214(HB,HC,HD), C215(H21A,H21B,H21C), C215(H21D,H21E,H21F), C216(H21G,H21H,
 H21I), C216(H21J,H21K,H21L), C217(H3AA,H9BA,H0CA), C218(H21,HJ,HK), C219(HE,HF,
 HG), C219(H21Z,HH,HI), C220(H22A,H22B,H22C), C220(H22D,H22E,H22F), C311(H31G,
 H31H,H31I), C311(H31J,H31K,H31L), C312(H31M,H31N,H31O), C312(H31P,H31Q,H31R),
 C313(H31,HV,HW), C313(HX,HY,HZ), C314(H31Z,HQ,HR), C314(HS,HT,HU), C315(H31A,
 H31B,H31C), C315(H31D,H31E,H31F), C316(H1AA,H9AA,H0BA), C316(H1BA,H2BA,H3BA),
 C317(H0AA,H4AA,H5AA), C317(H6AA,H7AA,H8AA), C318(H31S,H31T,H31U), C318(H31V,
 H31W,H31X), C319(H31Y,HL,HM), C319(HN,HO,HP)
;
_shelx_res_checksum              49251
_shelx_hkl_checksum              9214
_shelx_fab_checksum              29136
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'