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#$Date: 2025-11-29 19:19:44 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303611 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/56/1575680.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_1575680
loop_
_publ_author_name
'Heller, Jan'
'Buch, Christoph D.'
'Virovets, Alexander V.'
'Peresypkina, Eugenia'
'Lerner, Hans-Wolfram'
'Fantuzzi, Felipe'
'Wagner, Matthias'
_publ_section_title
;
 Synthesis of perhalogenated silylboranes (X = Cl, I) and their
 application in regiodivergent alkene silaboration.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              20329
_journal_page_last               20343
_journal_paper_doi               10.1039/d5sc06234a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'B Cl6 Si, C8 H20 N'
_chemical_formula_sum            'C8 H20 B Cl6 N Si'
_chemical_formula_weight         381.85
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-07-08 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4943(4)
_cell_length_b                   12.1239(4)
_cell_length_c                   12.3124(5)
_cell_measurement_reflns_used    4475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.3020
_cell_measurement_theta_min      2.9630
_cell_volume                     1715.80(11)
_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_publication_material  'IUCr PublCIF online service'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0718
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20540
_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         27.077
_diffrn_reflns_theta_min         2.442
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79159
_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            colorless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0286
_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)+(0.0310P)²+0.3640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1598
_reflns_number_total             1898
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc06234a3.cif
_cod_data_source_block           Et4NCl3BSiCl3_wa3568_JH231
_cod_depositor_comments
'Adding full bibliography for 1575660--1575680.cif.'
_cod_original_cell_volume        1715.81(11)
_cod_database_code               1575680
_shelx_shelxl_version_number     2019/3
_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   0.921
_shelx_estimated_absorpt_t_max   0.959
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.5240(5) 0.6825(4) 0.3257(6) 0.0219(5) Uani 0.5 1 d . . P . .
B1 B 0.535(2) 0.694(2) 0.328(2) 0.0219(5) Uani 0.5 1 d . . P . .
Cl1 Cl 0.39441(4) 0.67894(4) 0.42673(4) 0.04161(14) Uani 1 1 d . . . . .
Cl2 Cl 0.61642(4) 0.81841(3) 0.36262(3) 0.03154(12) Uani 1 1 d . . . . .
Cl3 Cl 0.62925(4) 0.55947(4) 0.35776(4) 0.03939(14) Uani 1 1 d . . . . .
N1 N 1.000000 0.68527(13) 0.250000 0.0230(4) Uani 1 2 d S T P . .
C1 C 0.89084(13) 0.75675(12) 0.25298(14) 0.0285(3) Uani 1 1 d . . . . .
H1A H 0.822197 0.707775 0.258710 0.034 Uiso 1 1 calc R U . . .
H1B H 0.893233 0.802673 0.319425 0.034 Uiso 1 1 calc R U . . .
C2 C 0.87425(15) 0.83177(14) 0.15620(15) 0.0340(4) Uani 1 1 d . . . . .
H2A H 0.866606 0.787192 0.090191 0.051 Uiso 1 1 calc R U . . .
H2B H 0.941651 0.880769 0.149313 0.051 Uiso 1 1 calc R U . . .
H2C H 0.803715 0.876000 0.166347 0.051 Uiso 1 1 calc R U . . .
C3 C 1.00300(14) 0.61451(12) 0.14815(12) 0.0269(3) Uani 1 1 d . . . . .
H3A H 1.008197 0.663727 0.084173 0.032 Uiso 1 1 calc R U . . .
H3B H 1.074489 0.568995 0.149689 0.032 Uiso 1 1 calc R U . . .
C4 C 0.89945(15) 0.53894(14) 0.13351(14) 0.0324(4) Uani 1 1 d . . . . .
H4A H 0.908698 0.496477 0.066335 0.049 Uiso 1 1 calc R U . . .
H4B H 0.828162 0.583077 0.129340 0.049 Uiso 1 1 calc R U . . .
H4C H 0.894404 0.488303 0.195375 0.049 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Si1 Cl3 109.1(3) . . ?
Cl1 Si1 B1 110.3(6) . 3_655 ?
Cl3 Si1 B1 116.6(7) . 3_655 ?
Cl1 Si1 Cl2 106.2(3) . . ?
Cl3 Si1 Cl2 104.6(3) . . ?
B1 Si1 Cl2 109.5(10) 3_655 . ?
Cl2 B1 Cl3 110.6(14) . . ?
Cl2 B1 Si1 116.6(15) . 3_655 ?
Cl3 B1 Si1 107.6(13) . 3_655 ?
Cl2 B1 Cl1 109.9(14) . . ?
Cl3 B1 Cl1 104.5(12) . . ?
Si1 B1 Cl1 107.0(11) 3_655 . ?
Si1 Cl1 B1 4.7(8) . . ?
B1 Cl2 Si1 1.1(12) . . ?
Si1 Cl3 B1 5.3(8) . . ?
C3 N1 C3 111.27(16) . 3_755 ?
C3 N1 C1 106.39(9) . 3_755 ?
C3 N1 C1 111.05(9) 3_755 3_755 ?
C3 N1 C1 111.05(9) . . ?
C3 N1 C1 106.39(9) 3_755 . ?
C1 N1 C1 110.76(15) 3_755 . ?
C2 C1 N1 115.27(12) . . ?
C2 C1 H1A 108.5 . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
N1 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 114.98(12) . . ?
C4 C3 H3A 108.5 . . ?
N1 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
N1 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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 1.940(7) . ?
Si1 Cl3 1.961(7) . ?
Si1 B1 2.01(2) 3_655 ?
Si1 Cl2 2.012(4) . ?
B1 Cl2 1.83(2) . ?
B1 Cl3 1.99(3) . ?
B1 Cl1 2.03(3) . ?
N1 C3 1.5198(17) . ?
N1 C3 1.5198(17) 3_755 ?
N1 C1 1.5252(17) 3_755 ?
N1 C1 1.5253(17) . ?
C1 C2 1.511(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.513(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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
Cl3 B1 Cl2 Si1 -135(63) . . . . ?
Si1 B1 Cl2 Si1 102(62) 3_655 . . . ?
Cl1 B1 Cl2 Si1 -20(61) . . . . ?
C3 N1 C1 C2 -56.86(17) . . . . ?
C3 N1 C1 C2 -178.09(13) 3_755 . . . ?
C1 N1 C1 C2 61.12(12) 3_755 . . . ?
C3 N1 C3 C4 60.61(11) 3_755 . . . ?
C1 N1 C3 C4 -178.31(13) 3_755 . . . ?
C1 N1 C3 C4 -57.71(17) . . . . ?
