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#$Date: 2023-05-05 03:12:29 +0300 (Fri, 05 May 2023) $
#$Revision: 283047 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/12/7131246.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7131246
loop_
_publ_author_name
'Köstler, Benedikt'
'Gilmer, Jannik'
'Bolte, Michael'
'Virovets, Alexander'
'Lerner, Hans-Wolfram'
'Albert, Philipp'
'Fantuzzi, Felipe'
'Wagner, Matthias'
_publ_section_title
;
 Group IV heteroadamantanes: synthesis of Si₆Sn₄ and
 site-selective derivatization of Si₆Ge₄.
;
_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       ω
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0115P)²+9.6398P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.699
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.63767(3) 0.86233(3) 0.250000 0.0190(2) Uani 0.171(2) 2 d S T P A 1
Cl1 Cl 0.6329(4) 0.7554(4) 0.3615(6) 0.0428(16) Uani 0.171(2) 1 d . . P A 1
Sn1 Sn 0.63767(3) 0.86233(3) 0.250000 0.0190(2) Uani 0.829(2) 2 d S T P A 2
C1 C 0.6329(4) 0.7554(4) 0.3615(6) 0.0428(16) Uani 0.829(2) 1 d . . P A 2
H1A H 0.683984 0.754419 0.415175 0.064 Uiso 0.829(2) 1 calc R U P A 2
H1B H 0.631944 0.702993 0.310445 0.064 Uiso 0.829(2) 1 calc R U P A 2
H1C H 0.580362 0.757610 0.412315 0.064 Uiso 0.829(2) 1 calc R U P A 2
Si2 Si 0.500000 1.000000 -0.01689(17) 0.0237(6) Uani 0.657(4) 4 d S T P A 1
Cl2 Cl 0.3904(3) 1.000000 -0.1127(4) 0.0336(10) Uani 0.657(4) 2 d S T P A 1
Sn2 Sn 0.500000 1.000000 -0.01689(17) 0.0237(6) Uani 0.343(4) 4 d S T P A 2
C2 C 0.3904(3) 1.000000 -0.1127(4) 0.0336(10) Uani 0.343(4) 2 d S T P A 2
H2A H 0.401059 0.976104 -0.195138 0.050 Uiso 0.171(2) 1 calc R U P A 2
H2B H 0.368838 1.059484 -0.120241 0.050 Uiso 0.171(2) 1 calc R U P A 2
H2C H 0.347202 0.964412 -0.069949 0.050 Uiso 0.171(2) 1 calc R U P A 2
Si3 Si 0.500000 0.87080(19) 0.1186(2) 0.0173(6) Uani 1 2 d S T P . .
Si4 Si 0.500000 0.75051(19) -0.0097(3) 0.0245(7) Uani 1 2 d S T P A .
Cl41 Cl 0.39361(16) 0.74671(16) -0.1222(2) 0.0431(6) Uani 1 1 d . . . . .
Cl45 Cl 0.500000 0.64095(19) 0.0958(3) 0.0378(7) Uani 1 2 d S T P . .
Si5 Si 0.500000 0.500000 0.500000 0.0375(17) Uani 1 8 d S T P . .
Cl51 Cl 0.500000 0.6063(3) 0.6076(4) 0.0606(10) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Si1 Cl1 114.0(4) . 16_665 ?
Cl1 Si1 Si3 109.8(2) . . ?
Cl1 Si1 Si3 109.85(18) 16_665 . ?
Cl1 Si1 Si3 109.85(18) . 12_655 ?
Cl1 Si1 Si3 109.8(2) 16_665 12_655 ?
Si3 Si1 Si3 102.94(13) . 12_655 ?
C1 Sn1 Si3 109.8(2) . . ?
Si3 Sn1 Si3 102.94(13) . 12_655 ?
Sn1 C1 H1A 109.5 . . ?
Sn1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sn1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Cl2 Si2 Cl2 117.0(2) 2_675 . ?
Cl2 Si2 Si3 108.05(7) 2_675 2_675 ?
Cl2 Si2 Si3 108.05(7) . 2_675 ?
Cl2 Si2 Si3 108.05(7) 2_675 . ?
Cl2 Si2 Si3 108.05(7) . . ?
Si3 Si2 Si3 107.31(14) 2_675 . ?
Si2 Cl2 H2A 109(10) . 5_575 ?
Si2 Cl2 H2B 109(10) . 5_575 ?
Si2 Cl2 H2C 109(6) . 5_575 ?
C2 Sn2 Si3 108.05(7) . 2_675 ?
C2 Sn2 Si3 108.05(7) . . ?
Si3 Sn2 Si3 107.31(14) 2_675 . ?
Sn2 C2 H2A 109.5 . . ?
Sn2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sn2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si4 Si3 Sn2 106.85(13) . . ?
Si4 Si3 Si2 106.85(13) . . ?
Si4 Si3 Si1 106.98(9) . 11_465 ?
Sn2 Si3 Si1 111.74(8) . 11_465 ?
Si2 Si3 Si1 111.74(8) . 11_465 ?
Si4 Si3 Sn1 106.98(9) . . ?
Sn2 Si3 Sn1 111.74(8) . . ?
Si4 Si3 Si1 106.98(9) . . ?
Si2 Si3 Si1 111.74(8) . . ?
Si1 Si3 Si1 112.17(10) 11_465 . ?
Cl45 Si4 Cl41 108.04(13) . 6_655 ?
Cl45 Si4 Cl41 108.04(13) . . ?
Cl41 Si4 Cl41 106.79(19) 6_655 . ?
Cl45 Si4 Si3 109.16(17) . . ?
Cl41 Si4 Si3 112.32(12) 6_655 . ?
Cl41 Si4 Si3 112.32(12) . . ?
Cl51 Si5 Cl51 109.2(3) 4_656 3_566 ?
Cl51 Si5 Cl51 109.61(13) 4_656 2_665 ?
Cl51 Si5 Cl51 109.61(13) 3_566 2_665 ?
Cl51 Si5 Cl51 109.61(13) 4_656 . ?
Cl51 Si5 Cl51 109.61(13) 3_566 . ?
Cl51 Si5 Cl51 109.2(3) 2_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 Cl1 2.046(6) . ?
Si1 Cl1 2.046(6) 16_665 ?
Si1 Si3 2.5605(15) . ?
Si1 Si3 2.5605(15) 12_655 ?
Sn1 C1 2.046(6) . ?
Sn1 Si3 2.5605(15) . ?
Sn1 Si3 2.5605(15) 12_655 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Si2 Cl2 1.984(4) 2_675 ?
Si2 Cl2 1.984(4) . ?
Si2 Si3 2.476(3) 2_675 ?
Si2 Si3 2.476(3) . ?
Cl2 H2A 0.98(14) 5_575 ?
Cl2 H2B 0.98(5) 5_575 ?
Cl2 H2C 1.0(3) 5_575 ?
Sn2 C2 1.984(4) . ?
Sn2 Si3 2.476(3) 2_675 ?
Sn2 Si3 2.476(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 H2A 0.98(14) 5_575 ?
C2 H2B 0.98(5) 5_575 ?
C2 H2C 1.0(3) 5_575 ?
Si3 Si4 2.319(4) . ?
Si4 Cl45 2.040(4) . ?
Si4 Cl41 2.045(3) 6_655 ?
Si4 Cl41 2.045(3) . ?
Si5 Cl51 2.012(4) 4_656 ?
Si5 Cl51 2.012(4) 3_566 ?
Si5 Cl51 2.012(4) 2_665 ?
Si5 Cl51 2.012(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Sn2 Si3 Si4 63.72(12) . . . . ?
Si3 Sn2 Si3 Si4 180.000(0) 2_675 . . . ?
C2 Sn2 Si3 Sn1 -179.59(12) . . . . ?
Si3 Sn2 Si3 Sn1 -63.30(8) 2_675 . . . ?
Cl2 Si2 Si3 Si4 -63.72(12) 2_675 . . . ?
Cl2 Si2 Si3 Si4 63.72(12) . . . . ?
Si3 Si2 Si3 Si4 180.000(0) 2_675 . . . ?
Cl2 Si2 Si3 Si1 179.59(12) 2_675 . . 11_465 ?
Cl2 Si2 Si3 Si1 -52.98(16) . . . 11_465 ?
Si3 Si2 Si3 Si1 63.30(8) 2_675 . . 11_465 ?
Cl2 Si2 Si3 Si1 52.98(16) 2_675 . . . ?
Cl2 Si2 Si3 Si1 -179.59(12) . . . . ?
Si3 Si2 Si3 Si1 -63.30(8) 2_675 . . . ?
C1 Sn1 Si3 Si4 -64.2(2) . . . . ?
Si3 Sn1 Si3 Si4 178.83(14) 12_655 . . . ?
C1 Sn1 Si3 Sn2 179.2(2) . . . . ?
Si3 Sn1 Si3 Sn2 62.21(9) 12_655 . . . ?
Cl1 Si1 Si3 Si4 -64.2(2) . . . . ?
Cl1 Si1 Si3 Si4 61.9(2) 16_665 . . . ?
Si3 Si1 Si3 Si4 178.83(14) 12_655 . . . ?
Cl1 Si1 Si3 Si2 179.2(2) . . . . ?
Cl1 Si1 Si3 Si2 -54.7(2) 16_665 . . . ?
Si3 Si1 Si3 Si2 62.21(9) 12_655 . . . ?
Cl1 Si1 Si3 Si1 52.8(2) . . . 11_465 ?
Cl1 Si1 Si3 Si1 178.9(2) 16_665 . . 11_465 ?
Si3 Si1 Si3 Si1 -64.17(9) 12_655 . . 11_465 ?
Sn2 Si3 Si4 Cl45 180.000(1) . . . . ?
Si2 Si3 Si4 Cl45 180.000(1) . . . . ?
Si1 Si3 Si4 Cl45 -60.19(8) 11_465 . . . ?
Sn1 Si3 Si4 Cl45 60.19(8) . . . . ?
Si1 Si3 Si4 Cl45 60.19(8) . . . . ?
Sn2 Si3 Si4 Cl41 60.20(13) . . . 6_655 ?
Si2 Si3 Si4 Cl41 60.20(13) . . . 6_655 ?
Si1 Si3 Si4 Cl41 -179.99(12) 11_465 . . 6_655 ?
Sn1 Si3 Si4 Cl41 -59.61(18) . . . 6_655 ?
Si1 Si3 Si4 Cl41 -59.61(18) . . . 6_655 ?
Sn2 Si3 Si4 Cl41 -60.20(13) . . . . ?
Si2 Si3 Si4 Cl41 -60.20(13) . . . . ?
Si1 Si3 Si4 Cl41 59.61(18) 11_465 . . . ?
Sn1 Si3 Si4 Cl41 179.99(12) . . . . ?
Si1 Si3 Si4 Cl41 179.99(12) . . . . ?
