#------------------------------------------------------------------------------
#$Date: 2025-09-11 01:11:53 +0300 (Thu, 11 Sep 2025) $
#$Revision: 302090 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/56/1575666.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_1575666
loop_
_publ_author_name
'Heller, Jan'
'Buch, Christoph D.'
'Virovets, Alexander'
'Peresypkina, Eugenia V.'
'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_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC06234A
_journal_year                    2025
_chemical_formula_moiety         'C2 H6 B Cl5 S Si'
_chemical_formula_sum            'C2 H6 B Cl5 S Si'
_chemical_formula_weight         278.28
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 95.647(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1191(3)
_cell_length_b                   16.0988(7)
_cell_length_c                   9.7847(3)
_cell_measurement_reflns_used    4456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.6470
_cell_measurement_theta_min      3.3510
_cell_volume                     1115.97(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.755
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96027
_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    1.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0319
_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)+(0.0348P)²+0.7240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2053
_reflns_number_total             2361
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc06234a3.cif
_cod_data_source_block           3_SMe2_wa3576_JH227
_cod_original_cell_volume        1115.98(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1575666
_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   0.862
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_file
;
TITL JH227 in P2(1)/n at -100C CAP+erm set by Moritz
    fin.res
    created by SHELXL-2019/3 at 19:19:15 on 03-Jul-2024
CELL 0.71073   7.11910  16.09882   9.78473  90.0000  95.6467  90.0000
ZERR    4.00   0.00028   0.00065   0.00034   0.0000   0.0033   0.0000
LATT  1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H B SI S CL
UNIT 8 24 4 4 4 20

L.S. 10
PLAN  7
CONF
BOND $H
TEMP -100
SIZE 0.10 0.07 0.05
REM colourless plate
fmap 2
ACTA

WGHT    0.034800    0.724000
FVAR       0.25258
B1    3    0.576455    0.680553    0.216389    11.00000    0.02755    0.03384 =
         0.02339   -0.00217    0.00398    0.00115
CL1   6    0.775900    0.753159    0.209684    11.00000    0.04109    0.04344 =
         0.03674    0.00362    0.00880   -0.01095
CL2   6    0.416855    0.681494    0.058148    11.00000    0.04277    0.07224 =
         0.02628   -0.00337   -0.00397    0.00261
CL3   6    0.798974    0.561768    0.458510    11.00000    0.07393    0.06327 =
         0.05169    0.02247    0.00488    0.02361
CL4   6    0.882176    0.534837    0.137725    11.00000    0.05895    0.06084 =
         0.07700   -0.01359    0.03662    0.01491
CL5   6    0.481132    0.474535    0.239280    11.00000    0.07772    0.04044 =
         0.13345   -0.03010    0.04473   -0.02345
S1    5    0.449259    0.719767    0.372927    11.00000    0.03286    0.03188 =
         0.02786   -0.00396    0.00743    0.00362
SI1   4    0.677671    0.566384    0.260059    11.00000    0.03526    0.02869 =
         0.04485   -0.00296    0.01517    0.00359
C1    1    0.350595    0.817683    0.314675    11.00000    0.08257    0.03709 =
         0.06887    0.00711    0.03012    0.02756
AFIX 137
H1A   2    0.278461    0.810381    0.224899    11.00000   -1.50000
H1B   2    0.452590    0.857723    0.306557    11.00000   -1.50000
H1C   2    0.266885    0.838386    0.380776    11.00000   -1.50000
AFIX   0
C2    1    0.240330    0.657767    0.367701    11.00000    0.03355    0.05417 =
         0.05070   -0.00806    0.01548   -0.00432
AFIX 137
H2A   2    0.179362    0.656000    0.273480    11.00000   -1.50000
H2B   2    0.153362    0.682054    0.428329    11.00000   -1.50000
H2C   2    0.273740    0.601262    0.398429    11.00000   -1.50000

AFIX   0
HKLF 4




REM  JH227 in P2(1)/n at -100C CAP+erm set by Moritz
REM wR2 = 0.0819, GooF = S = 1.048, Restrained GooF = 1.048 for all data
REM R1 = 0.0319 for 2053 Fo > 4sig(Fo) and 0.0383 for all 2361 data
REM 93 parameters refined using 0 restraints

END

WGHT      0.0348      0.7224

REM Highest difference peak  0.549,  deepest hole -0.429,  1-sigma level  0.063
Q1    1   0.6912  0.5457  0.4620  11.00000  0.05    0.55
Q2    1   0.8218  0.5338  0.3948  11.00000  0.05    0.48
Q3    1   0.5093  0.4793  0.3159  11.00000  0.05    0.45
Q4    1   0.7954  0.5217  0.0864  11.00000  0.05    0.43
Q5    1   0.3592  0.6458  0.0784  11.00000  0.05    0.35
Q6    1   0.4136  0.4942  0.2160  11.00000  0.05    0.32
Q7    1   0.8476  0.5575  0.4906  11.00000  0.05    0.31
;
_shelx_res_checksum              76570
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-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
B1 B 0.5765(3) 0.68055(16) 0.2164(2) 0.0282(5) Uani 1 1 d . . . . .
Cl1 Cl 0.77590(8) 0.75316(4) 0.20968(6) 0.04009(16) Uani 1 1 d . . . . .
Cl2 Cl 0.41686(9) 0.68149(5) 0.05815(6) 0.04759(18) Uani 1 1 d . . . . .
Cl3 Cl 0.79897(12) 0.56177(5) 0.45851(8) 0.0631(2) Uani 1 1 d . . . . .
Cl4 Cl 0.88218(11) 0.53484(5) 0.13772(9) 0.0636(2) Uani 1 1 d . . . . .
Cl5 Cl 0.48113(14) 0.47454(5) 0.23928(12) 0.0816(3) Uani 1 1 d . . . . .
S1 S 0.44926(8) 0.71977(3) 0.37293(5) 0.03057(14) Uani 1 1 d . . . . .
Si1 Si 0.67767(9) 0.56638(4) 0.26006(7) 0.03552(16) Uani 1 1 d . . . . .
C1 C 0.3506(5) 0.81768(17) 0.3147(3) 0.0613(8) Uani 1 1 d . . . . .
H1A H 0.278461 0.810381 0.224899 0.092 Uiso 1 1 calc R U . . .
H1B H 0.452590 0.857723 0.306557 0.092 Uiso 1 1 calc R U . . .
H1C H 0.266885 0.838386 0.380776 0.092 Uiso 1 1 calc R U . . .
C2 C 0.2403(3) 0.65777(18) 0.3677(3) 0.0454(6) Uani 1 1 d . . . . .
H2A H 0.179362 0.656000 0.273480 0.068 Uiso 1 1 calc R U . . .
H2B H 0.153362 0.682054 0.428329 0.068 Uiso 1 1 calc R U . . .
H2C H 0.273740 0.601262 0.398429 0.068 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.0276(11) 0.0338(13) 0.0234(10) -0.0022(9) 0.0040(9) 0.0011(9)
Cl1 0.0411(3) 0.0434(3) 0.0367(3) 0.0036(2) 0.0088(2) -0.0110(2)
Cl2 0.0428(3) 0.0722(5) 0.0263(3) -0.0034(3) -0.0040(2) 0.0026(3)
Cl3 0.0739(5) 0.0633(5) 0.0517(4) 0.0225(4) 0.0049(3) 0.0236(4)
Cl4 0.0589(4) 0.0608(5) 0.0770(5) -0.0136(4) 0.0366(4) 0.0149(3)
Cl5 0.0777(6) 0.0404(4) 0.1334(9) -0.0301(5) 0.0447(6) -0.0234(4)
S1 0.0329(3) 0.0319(3) 0.0279(3) -0.0040(2) 0.0074(2) 0.0036(2)
Si1 0.0353(3) 0.0287(3) 0.0448(4) -0.0030(3) 0.0152(3) 0.0036(2)
C1 0.083(2) 0.0371(15) 0.0689(19) 0.0071(14) 0.0301(17) 0.0276(14)
C2 0.0335(12) 0.0542(16) 0.0507(14) -0.0081(12) 0.0155(11) -0.0043(11)
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
Cl2 B1 Cl1 112.39(13) . . ?
Cl2 B1 S1 111.28(12) . . ?
Cl1 B1 S1 103.90(12) . . ?
Cl2 B1 Si1 111.62(12) . . ?
Cl1 B1 Si1 109.06(12) . . ?
S1 B1 Si1 108.23(11) . . ?
C2 S1 C1 100.53(16) . . ?
C2 S1 B1 104.18(11) . . ?
C1 S1 B1 103.37(12) . . ?
B1 Si1 Cl5 114.60(8) . . ?
B1 Si1 Cl4 111.46(8) . . ?
Cl5 Si1 Cl4 106.53(4) . . ?
B1 Si1 Cl3 110.16(7) . . ?
Cl5 Si1 Cl3 106.89(5) . . ?
Cl4 Si1 Cl3 106.80(5) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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
B1 Cl2 1.828(2) . ?
B1 Cl1 1.845(3) . ?
B1 S1 1.959(2) . ?
B1 Si1 2.005(3) . ?
Cl3 Si1 2.0474(10) . ?
Cl4 Si1 2.0380(9) . ?
Cl5 Si1 2.0321(10) . ?
S1 C2 1.788(3) . ?
S1 C1 1.796(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
