#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/02/7120213.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_7120213
loop_
_publ_author_name
'Arrowsmith, Merle'
'Böhnke, Julian'
'Braunschweig, Holger'
'Deißenberger, Andrea'
'Dewhurst, Rian David'
'Ewing, William'
'Hörl, Christian'
'Mies, Jan'
'Muessig, Jonas'
_publ_section_title
;
 Simple Solution-Phase Syntheses of Tetrahalodiboranes(4) and their Labile
 Dimethylsulfide Adducts
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03148C
_journal_year                    2017
_chemical_formula_moiety         'C4 H12 B2 I4 S2'
_chemical_formula_sum            'C4 H12 B2 I4 S2'
_chemical_formula_weight         653.48
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.556(4)
_cell_length_b                   7.455(5)
_cell_length_c                   13.174(8)
_cell_measurement_reflns_used    5011
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.91
_cell_measurement_theta_min      2.84
_cell_volume                     717.2(8)
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0242
_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       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7347
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         2.837
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    8.938
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.026
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0171
_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)+(0.0130P)²+0.6289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1485
_reflns_number_total             1532
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc03148c2.cif
_cod_data_source_block           test_a
_cod_original_cell_volume        717.2(7)
_cod_database_code               7120213
_shelx_shelxl_version_number     2014/7
_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   0.500
_shelx_estimated_absorpt_t_max   0.535
_shelx_res_file
;

    test_a.res created by SHELXL-2014/7


TITL test_a.res in P2(1)/n
REM Old TITL test in P2(1)/n

REM SHELXT solution in P2(1)/n
REM R1 0.052,  Rweak 0.003,  Alpha 0.011,  Orientation as input
REM Formula found by SHELXT:  C3 S I2
CELL  0.71073  7.55612    7.45513   13.17384   90.0000  104.8879   90.0000
ZERR    2.000  0.00378    0.00453    0.00824    0.0000    0.0260    0.0000
rem  above ESDs are from Monte-Carlo simulation
rem CELL  0.71073   7.5561   7.4551  13.1738   90.000  104.888   90.000
rem ZERR    2.000   0.0019   0.0023   0.0041    0.000    0.016    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H B S I
UNIT 8 24 4 4 8
TEMP -170.000
SIZE 0.08 0.08 0.09
L.S. 10
BOND $H
LIST 4
CONF
SHEL 999 0.79
ACTA 52
FMAP 2
PLAN 20
WGHT    0.013000    0.628900
FVAR       0.32031
I1    5    0.245531    0.697663    0.358404    11.00000    0.01228    0.01903 =
         0.01357    0.00322    0.00052    0.00296
C1    1    0.676695    0.919745    0.403638    11.00000    0.02158    0.01737 =
         0.01858    0.00349    0.00974   -0.00248
AFIX 137
H1A   2    0.730571    1.036540    0.428115    11.00000   -1.50000
H1B   2    0.560500    0.937687    0.350706    11.00000   -1.50000
H1C   2    0.761089    0.852289    0.372621    11.00000   -1.50000
AFIX   0
S1    4    0.636162    0.796202    0.512843    11.00000    0.01077    0.01297 =
         0.01132   -0.00041    0.00357   -0.00068
B1    3    0.513521    0.574920    0.453202    11.00000    0.00777    0.01325 =
         0.00731   -0.00144    0.00099    0.00067
I2    5    0.659817    0.453978    0.340968    11.00000    0.01379    0.01765 =
         0.00992   -0.00118    0.00339    0.00197
C2    1    0.870174    0.749599    0.579404    11.00000    0.01179    0.02277 =
         0.01991   -0.00245    0.00004   -0.00329
AFIX 137
H2A   2    0.874662    0.681783    0.643743    11.00000   -1.50000
H2B   2    0.936979    0.862693    0.597406    11.00000   -1.50000
H2C   2    0.926692    0.678868    0.533418    11.00000   -1.50000
AFIX   0
HKLF 4

REM  test_a.res in P2(1)/n
REM R1 =  0.0171 for    1485 Fo > 4sig(Fo)  and  0.0178 for all    1532 data
REM     57 parameters refined using      0 restraints

END

WGHT      0.0130      0.6288

REM Highest difference peak  0.794,  deepest hole -0.889,  1-sigma level  0.121
Q1    1   0.6842  0.3324  0.3574  11.00000  0.05    0.79
Q2    1   0.6267  0.5564  0.3169  11.00000  0.05    0.68
Q3    1   0.2073  0.5836  0.3382  11.00000  0.05    0.67
Q4    1   0.2804  0.5816  0.3782  11.00000  0.05    0.66
Q5    1   0.2204  0.8141  0.3425  11.00000  0.05    0.66
Q6    1   0.5746  0.4523  0.3613  11.00000  0.05    0.64
Q7    1   0.6927  0.5690  0.3656  11.00000  0.05    0.60
Q8    1   0.1563  0.6654  0.3783  11.00000  0.05    0.54
Q9    1   0.2158  0.7817  0.2999  11.00000  0.05    0.50
Q10   1   0.3424  0.6970  0.3426  11.00000  0.05    0.46
Q11   1   0.7670  0.3949  0.3183  11.00000  0.05    0.44
Q12   1   0.7579  0.4962  0.3228  11.00000  0.05    0.43
Q13   1   0.6619  0.8642  0.4591  11.00000  0.05    0.41
Q14   1   0.7328  0.3587  0.2877  11.00000  0.05    0.41
Q15   1   0.5660  0.6964  0.4773  11.00000  0.05    0.38
Q16   1   0.5923  0.7278  0.4650  11.00000  0.05    0.36
Q17   1   0.2767  0.9335  0.2972  11.00000  0.05    0.35
Q18   1   0.6567  1.0207  0.4543  11.00000  0.05    0.33
Q19   1   0.5000  0.5000  0.5000  10.50000  0.05    0.32
Q20   1   0.4845  0.6704  0.3821  11.00000  0.05    0.32
;
_shelx_res_checksum              48610
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
I1 I 0.24553(2) 0.69766(3) 0.35840(2) 0.01547(7) Uani 1 1 d . .
C1 C 0.6767(4) 0.9197(5) 0.4036(3) 0.0183(6) Uani 1 1 d . .
H1A H 0.7306 1.0365 0.4281 0.028 Uiso 1 1 calc R U
H1B H 0.5605 0.9377 0.3507 0.028 Uiso 1 1 calc R U
H1C H 0.7611 0.8523 0.3726 0.028 Uiso 1 1 calc R U
S1 S 0.63616(9) 0.79620(10) 0.51284(6) 0.01155(15) Uani 1 1 d . .
B1 B 0.5135(4) 0.5749(5) 0.4532(2) 0.0096(6) Uani 1 1 d . .
I2 I 0.65982(2) 0.45398(3) 0.34097(2) 0.01373(7) Uani 1 1 d . .
C2 C 0.8702(4) 0.7496(5) 0.5794(3) 0.0189(7) Uani 1 1 d . .
H2A H 0.8747 0.6818 0.6437 0.028 Uiso 1 1 calc R U
H2B H 0.9370 0.8627 0.5974 0.028 Uiso 1 1 calc R U
H2C H 0.9267 0.6789 0.5334 0.028 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
I1 0.01228(11) 0.01903(12) 0.01357(11) 0.00322(7) 0.00052(8) 0.00296(7)
C1 0.0216(15) 0.0174(16) 0.0186(16) 0.0035(13) 0.0097(13) -0.0025(13)
S1 0.0108(3) 0.0130(4) 0.0113(3) -0.0004(3) 0.0036(3) -0.0007(3)
B1 0.0078(14) 0.0132(16) 0.0073(14) -0.0014(12) 0.0010(11) 0.0007(12)
I2 0.01379(11) 0.01765(12) 0.00992(11) -0.00118(7) 0.00339(8) 0.00197(7)
C2 0.0118(14) 0.0228(17) 0.0199(16) -0.0024(13) 0.0000(12) -0.0033(12)
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
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 .
C2 S1 C1 98.11(16) .
C2 S1 B1 109.80(15) .
C1 S1 B1 105.72(15) .
B1 B1 S1 113.1(3) 3_666
B1 B1 I2 112.4(3) 3_666
S1 B1 I2 109.88(14) .
B1 B1 I1 113.7(2) 3_666
S1 B1 I1 98.28(15) .
I2 B1 I1 108.55(13) .
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
I1 B1 2.280(3) .
C1 S1 1.800(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
S1 C2 1.794(3) .
S1 B1 1.955(4) .
B1 B1 1.714(7) 3_666
B1 I2 2.250(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139187772
