Group IV heteroadamantanes: synthesis of Si<sub>6</sub>Sn<sub>4</sub> and site-selective derivatization of Si<sub>6</sub>Ge<sub>4</sub>.
Köstler, Benedikt; Gilmer, Jannik; Bolte, Michael; Virovets, Alexander; Lerner, Hans-Wolfram; Albert, Philipp; Fantuzzi, Felipe; Wagner, Matthias; Chemical communications (Cambridge, England) 59 (2023) 2295–2298; doi:10.1039/d2cc06697a

data_7131246
_publ_section_title
;
 Group IV heteroadamantanes: synthesis of Si<sub>6</sub>Sn<sub>4</sub> and
 site-selective derivatization of Si<sub>6</sub>Ge<sub>4</sub>.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2295
_journal_page_last               2298
_journal_paper_doi               10.1039/d2cc06697a
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C8 H24 Cl16 Si10 Sn4, Cl4 Si'
_chemical_formula_sum            'C8 H24 Cl20 Si11 Sn4'
_chemical_formula_weight         1613.02
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           119
_space_group_name_Hall           'I -4 -2'
_space_group_name_H-M_alt        'I -4 m 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-01-10 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4337(3)
_cell_length_b                   15.4337(3)
_cell_length_c                   10.8282(4)
_cell_measurement_reflns_used    3474
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.6470
_cell_measurement_theta_min      4.2500
_cell_volume                     2579.27(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'IUCr PublCIF online service'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6111
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         4.176
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_coef       0.00081(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1288
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0115P)^2^+9.6398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                1251
_reflns_number_total             1288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06697a3.cif
_cod_data_source_block           wa3101_AV
_cod_depositor_comments
'Adding full bibliography for 7131246--7131250.cif.'
_cod_original_cell_volume        2579.26(12)
_cod_database_code               7131246
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.699
_shelx_res_checksum              38550
_shelx_hkl_checksum              17576