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#$Date: 2025-08-23 01:57:28 +0300 (Sat, 23 Aug 2025) $
#$Revision: 301878 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/15/7701501.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_7701501
loop_
_publ_author_name
'Nukazawa, Takumi'
'Kosai, Tomoyuki'
'Honda, Shunya'
'Ishida, Shintaro'
'Iwamoto, Takeaki'
_publ_section_title
;
 Reactions of a tetrasilabicyclo[1.1.0]but-1(3)-ene with carbon
 tetrachloride and methanol.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10874
_journal_page_last               10880
_journal_paper_doi               10.1039/c9dt01627a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H80 Cl40 Si12'
_chemical_formula_sum            'C32 H80 Cl4 Si12'
_chemical_formula_weight         943.84
_chemical_melting_point          443
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-04-08 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                69.0200(10)
_cell_angle_beta                 84.5210(10)
_cell_angle_gamma                65.6520(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6683(5)
_cell_length_b                   10.7582(5)
_cell_length_c                   12.9529(6)
_cell_measurement_reflns_used    8117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.22
_cell_volume                     1262.24(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18763
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.687
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0318
_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)+(0.0358P)²+1.0187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5055
_reflns_number_total             5793
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01627a2.cif
_cod_data_source_block           TK64a_a
_cod_database_code               7701501
_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   0.948
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Si1 Si 0.59936(5) 0.53473(5) 0.54138(4) 0.01165(10) Uani 1 1 d . .
Si2 Si 0.53627(4) 0.59628(5) 0.34864(3) 0.00929(10) Uani 1 1 d . .
Si3 Si 0.40652(5) 0.95797(5) 0.28809(4) 0.01729(11) Uani 1 1 d . .
Si4 Si 0.27252(5) 0.83235(5) 0.16831(4) 0.01678(11) Uani 1 1 d . .
Si5 Si 0.85945(5) 0.52501(6) 0.27273(4) 0.02058(12) Uani 1 1 d . .
Si6 Si 0.71426(5) 0.35426(5) 0.22181(4) 0.01837(11) Uani 1 1 d . .
Cl1 Cl 0.64729(5) 0.67282(5) 0.59173(4) 0.02279(11) Uani 1 1 d . .
Cl2 Cl 0.78221(4) 0.35309(5) 0.55133(4) 0.02193(10) Uani 1 1 d . .
C1 C 0.43784(17) 0.79457(17) 0.24593(13) 0.0126(3) Uani 1 1 d . .
C2 C 0.55064(18) 0.79724(18) 0.15804(14) 0.0155(3) Uani 1 1 d . .
H1 H 0.5084 0.8777 0.0874 0.019 Uiso 1 1 calc R U
H2 H 0.6240 0.8138 0.1852 0.019 Uiso 1 1 calc R U
C3 C 0.61198(18) 0.65300(19) 0.13937(14) 0.0160(3) Uani 1 1 d . .
H3 H 0.6821 0.6539 0.0836 0.019 Uiso 1 1 calc R U
H4 H 0.5389 0.6369 0.1113 0.019 Uiso 1 1 calc R U
C4 C 0.68044(17) 0.52669(18) 0.25261(13) 0.0133(3) Uani 1 1 d . .
C5 C 0.2995(3) 0.9650(2) 0.40871(18) 0.0338(5) Uani 1 1 d . .
H5 H 0.3451 0.8766 0.4728 0.051 Uiso 1 1 calc R U
H6 H 0.2091 0.9714 0.3913 0.051 Uiso 1 1 calc R U
H7 H 0.2875 1.0507 0.4259 0.051 Uiso 1 1 calc R U
C6 C 0.3281(2) 1.1327(2) 0.16673(17) 0.0259(4) Uani 1 1 d . .
H8 H 0.2384 1.1437 0.1432 0.039 Uiso 1 1 calc R U
H9 H 0.3892 1.1302 0.1053 0.039 Uiso 1 1 calc R U
H10 H 0.3160 1.2152 0.1884 0.039 Uiso 1 1 calc R U
C7 C 0.5690(2) 0.9639(2) 0.32427(17) 0.0277(4) Uani 1 1 d . .
H11 H 0.5462 1.0464 0.3489 0.042 Uiso 1 1 calc R U
H12 H 0.6236 0.9752 0.2590 0.042 Uiso 1 1 calc R U
H13 H 0.6224 0.8730 0.3839 0.042 Uiso 1 1 calc R U
C8 C 0.2767(2) 0.9339(2) 0.01618(16) 0.0277(4) Uani 1 1 d . .
H14 H 0.3530 0.8714 -0.0151 0.042 Uiso 1 1 calc R U
H15 H 0.2897 1.0222 0.0069 0.042 Uiso 1 1 calc R U
H16 H 0.1895 0.9608 -0.0222 0.042 Uiso 1 1 calc R U
C9 C 0.1058(2) 0.9485(2) 0.21152(19) 0.0295(5) Uani 1 1 d . .
H17 H 0.0290 0.9629 0.1663 0.044 Uiso 1 1 calc R U
H18 H 0.1061 1.0432 0.2010 0.044 Uiso 1 1 calc R U
H19 H 0.0952 0.9001 0.2898 0.044 Uiso 1 1 calc R U
C10 C 0.2489(2) 0.6690(2) 0.17012(17) 0.0255(4) Uani 1 1 d . .
H20 H 0.2341 0.6152 0.2458 0.038 Uiso 1 1 calc R U
H21 H 0.3315 0.6059 0.1445 0.038 Uiso 1 1 calc R U
H22 H 0.1688 0.7002 0.1211 0.038 Uiso 1 1 calc R U
C11 C 0.8693(2) 0.6325(2) 0.35572(18) 0.0291(4) Uani 1 1 d . .
H23 H 0.8345 0.5999 0.4289 0.044 Uiso 1 1 calc R U
H24 H 0.8131 0.7362 0.3173 0.044 Uiso 1 1 calc R U
H25 H 0.9653 0.6174 0.3644 0.044 Uiso 1 1 calc R U
C12 C 0.9180(2) 0.6100(3) 0.13363(18) 0.0319(5) Uani 1 1 d . .
H26 H 0.8608 0.7150 0.1049 0.048 Uiso 1 1 calc R U
H27 H 0.9092 0.5656 0.0821 0.048 Uiso 1 1 calc R U
H28 H 1.0146 0.5936 0.1416 0.048 Uiso 1 1 calc R U
C13 C 1.0020(2) 0.3397(2) 0.33404(18) 0.0307(5) Uani 1 1 d . .
H29 H 1.0884 0.3496 0.3388 0.046 Uiso 1 1 calc R U
H30 H 1.0123 0.2826 0.2870 0.046 Uiso 1 1 calc R U
H31 H 0.9799 0.2901 0.4084 0.046 Uiso 1 1 calc R U
C14 C 0.8304(2) 0.3460(2) 0.10350(16) 0.0264(4) Uani 1 1 d . .
H32 H 0.9194 0.3391 0.1247 0.040 Uiso 1 1 calc R U
H33 H 0.7878 0.4342 0.0386 0.040 Uiso 1 1 calc R U
H34 H 0.8446 0.2602 0.0855 0.040 Uiso 1 1 calc R U
C15 C 0.7950(3) 0.1785(2) 0.33931(17) 0.0351(5) Uani 1 1 d . .
H35 H 0.7341 0.1268 0.3565 0.053 Uiso 1 1 calc R U
H36 H 0.8093 0.1980 0.4046 0.053 Uiso 1 1 calc R U
H37 H 0.8839 0.1182 0.3186 0.053 Uiso 1 1 calc R U
C16 C 0.5568(2) 0.3558(2) 0.16797(18) 0.0290(4) Uani 1 1 d . .
H38 H 0.5808 0.2651 0.1541 0.043 Uiso 1 1 calc R U
H39 H 0.5204 0.4389 0.0988 0.043 Uiso 1 1 calc R U
H40 H 0.4867 0.3641 0.2228 0.043 Uiso 1 1 calc R U
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'
Si Si 0.0817 0.0704 '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'
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_3
Cl1 Si1 Cl2 107.49(3) .
Cl1 Si1 Si2 121.17(3) .
Cl2 Si1 Si2 96.23(2) .
Cl1 Si1 Si2 122.06(3) 2_666
Cl2 Si1 Si2 97.51(2) 2_666
Si2 Si1 Si2 106.35(2) 2_666
C1 Si2 C4 98.20(7) .
C1 Si2 Si1 124.37(5) .
C4 Si2 Si1 118.83(5) .
C1 Si2 Si1 118.10(5) 2_666
C4 Si2 Si1 125.35(5) 2_666
Si1 Si2 Si1 73.65(2) 2_666
C5 Si3 C7 106.16(11) .
C5 Si3 C6 110.41(10) .
C7 Si3 C6 102.53(9) .
C5 Si3 C1 113.59(9) .
C7 Si3 C1 113.34(9) .
C6 Si3 C1 110.21(8) .
C10 Si4 C9 105.50(10) .
C10 Si4 C8 103.55(9) .
C9 Si4 C8 105.08(10) .
C10 Si4 C1 116.26(8) .
C9 Si4 C1 115.88(9) .
C8 Si4 C1 109.34(8) .
C11 Si5 C13 105.30(10) .
C11 Si5 C12 103.51(10) .
C13 Si5 C12 104.97(10) .
C11 Si5 C4 117.24(8) .
C13 Si5 C4 115.31(9) .
C12 Si5 C4 109.24(9) .
C15 Si6 C16 107.39(11) .
C15 Si6 C14 107.44(10) .
C16 Si6 C14 102.60(10) .
C15 Si6 C4 115.67(9) .
C16 Si6 C4 113.47(8) .
C14 Si6 C4 109.32(8) .
C2 C1 Si3 103.73(11) .
C2 C1 Si4 106.86(11) .
Si3 C1 Si4 108.78(8) .
C2 C1 Si2 98.14(10) .
Si3 C1 Si2 120.31(9) .
Si4 C1 Si2 116.64(8) .
C3 C2 C1 109.23(13) .
C2 C3 C4 108.92(14) .
C3 C4 Si6 103.00(11) .
C3 C4 Si5 106.59(11) .
Si6 C4 Si5 106.82(8) .
C3 C4 Si2 98.01(10) .
Si6 C4 Si2 121.92(9) .
Si5 C4 Si2 117.84(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Cl1 2.0682(6) .
Si1 Cl2 2.0892(6) .
Si1 Si2 2.4277(6) .
Si1 Si2 2.4413(6) 2_666
Si2 C1 1.9521(17) .
Si2 C4 1.9559(17) .
Si2 Si1 2.4413(6) 2_666
Si3 C5 1.850(2) .
Si3 C7 1.870(2) .
Si3 C6 1.882(2) .
Si3 C1 1.9153(17) .
Si4 C10 1.867(2) .
Si4 C9 1.875(2) .
Si4 C8 1.887(2) .
Si4 C1 1.9343(18) .
Si5 C11 1.875(2) .
Si5 C13 1.875(2) .
Si5 C12 1.884(2) .
Si5 C4 1.9439(18) .
Si6 C15 1.866(2) .
Si6 C16 1.871(2) .
Si6 C14 1.880(2) .
Si6 C4 1.9186(17) .
C1 C2 1.578(2) .
C2 C3 1.515(2) .
C3 C4 1.578(2) .
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
Si3 C1 C2 C3 165.53(12)
Si4 C1 C2 C3 -79.61(14)
Si2 C1 C2 C3 41.49(15)
C1 C2 C3 C4 -60.25(18)
C2 C3 C4 Si6 167.58(12)
C2 C3 C4 Si5 -80.17(14)
C2 C3 C4 Si2 42.10(15)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168342625
