Selective synthesis of germasila-adamantanes through germanium-silicon shift processes.
Kühn, Steffen; Köstler, Benedikt; True, Celine; Albers, Lena; Wagner, Matthias; Müller, Thomas; Marschner, Christoph; Chemical science 14 (2023) 8956–8961; doi:10.1039/d3sc03301e

data_1569593
_publ_section_title
;
 Selective synthesis of germasila-adamantanes through germanium-silicon
 shift processes.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              8956
_journal_page_last               8961
_journal_paper_doi               10.1039/d3sc03301e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C24 H72 Ge4 Si10'
_chemical_formula_sum            'C24 H72 Ge4 Si10'
_chemical_formula_weight         932.145
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.6700(18)
_cell_length_b                   17.6700(18)
_cell_length_c                   29.511(6)
_cell_measurement_reflns_used    998
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      3.07
_cell_volume                     7980(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART V5.622 (?, 2016)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20863
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         1.50
_diffrn_source                   'sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.804725
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.0845 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.8047.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             2915.073
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.6909
_refine_diff_density_min         -0.7274
_refine_diff_density_rms         0.1286
_refine_ls_d_res_high            0.8041
_refine_ls_d_res_low             13.5849
_refine_ls_goodness_of_fit_ref   0.9974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9974
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+149.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              -36
_reflns_number_gt                3496
_reflns_number_total             3587
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc03301e3.cif
_cod_data_source_block           1384js
_cod_depositor_comments          'Adding full bibliography for 1569593.cif.'
_cod_original_cell_volume        7979.7(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1569593
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C008(H00d,H00e,H00f), C009(H00g,H00h,H00i), C00A(H00j,
 H00k,H00l), C00B(H00m,H00n,H00o), C00C(H00p,H00q,H00r), C00D(H00s,H00t,H00u),
 C00E(H00v,H00w,H00x)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id 1384j
_olex2_submission_special_instructions 'No special instructions were received'