#------------------------------------------------------------------------------
#$Date: 2017-06-01 04:31:03 +0300 (Thu, 01 Jun 2017) $
#$Revision: 197115 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/02/7120214.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_7120214
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 Br4 S2'
_chemical_formula_sum            'C4 H12 B2 Br4 S2'
_chemical_formula_weight         465.52
_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-2014/6
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.281(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4726(4)
_cell_length_b                   7.2585(4)
_cell_length_c                   12.3850(8)
_cell_measurement_reflns_used    6698
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.86
_cell_volume                     641.44(6)
_computing_cell_refinement       'Saint+ ver. V8.27B (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.27B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9027
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.863
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    12.825
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0176P)²+0.3202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1254
_reflns_number_total             1300
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc03148c2.cif
_cod_data_source_block           test_a
_cod_database_code               7120214
_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   0.114
_shelx_estimated_absorpt_t_max   0.360
_shelxl_version_number           2014/6
_shelx_res_file
;
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 0.058,  Rweak 0.003,  Alpha 0.011,  Orientation as input
REM Formula found by SHELXT:  C3 S Br2
CELL  0.71073   7.4726   7.2585  12.3850   90.000  107.281   90.000
ZERR    2.000   0.0004   0.0004   0.0008    0.000    0.002    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H B S BR
UNIT 8 24 4 4 8
TEMP -170.000
SIZE 0.10 0.16 0.30
L.S. 10
BOND $H
LIST 4
CONF
SHEL 999 0.8
ACTA 52
FMAP 2
PLAN 20
WGHT    0.017600    0.320200
FVAR       0.45273
BR1   5    0.359644    0.542227    0.657105    11.00000    0.01675    0.01579 =
         0.01189   -0.00141    0.00671    0.00138
C1    1    0.110633    0.261444    0.421253    11.00000    0.01312    0.02491 =
         0.02107   -0.00098    0.00118   -0.00340
AFIX 137
H1A   2    0.100158    0.345384    0.357694    11.00000   -1.50000
H1B   2    0.061634    0.321924    0.477339    11.00000   -1.50000
H1C   2    0.038213    0.149406    0.393822    11.00000   -1.50000
AFIX   0
S1    4    0.351996    0.202186    0.485127    11.00000    0.01444    0.01266 =
         0.01355   -0.00133    0.00651   -0.00192
B1    3    0.488220    0.425674    0.551288    11.00000    0.01125    0.01231 =
         0.01094   -0.00003    0.00378    0.00049
BR2   5    0.736258    0.308659    0.643812    11.00000    0.01245    0.01814 =
         0.01569    0.00389    0.00160    0.00290
C2    1    0.326507    0.072522    0.603444    11.00000    0.02414    0.01616 =
         0.01957    0.00253    0.01198   -0.00236
AFIX 137
H2A   2    0.257689   -0.041522    0.576210    11.00000   -1.50000
H2B   2    0.257240    0.146020    0.644069    11.00000   -1.50000
H2C   2    0.450705    0.042421    0.654517    11.00000   -1.50000
AFIX   0
HKLF 4

REM  test_a.res in P2(1)/n
REM R1 =  0.0148 for    1254 Fo > 4sig(Fo)  and  0.0157 for all    1300 data
REM     57 parameters refined using      0 restraints

END

WGHT      0.0176      0.3202

REM Highest difference peak  0.645,  deepest hole -0.237,  1-sigma level  0.080
Q1    1   0.8255  0.3698  0.6236  11.00000  0.05    0.64
Q2    1   0.4614  0.5432  0.6434  11.00000  0.05    0.58
Q3    1   0.2565  0.5311  0.6728  11.00000  0.05    0.55
Q4    1   0.6172  0.3070  0.6498  11.00000  0.05    0.47
Q5    1   0.5000  0.5000  0.5000  10.50000  0.05    0.41
Q6    1   0.6991  0.2973  0.5635  11.00000  0.05    0.33
Q7    1   0.2238  0.2267  0.4486  11.00000  0.05    0.32
Q8    1   0.3118  0.5542  0.5880  11.00000  0.05    0.30
Q9    1   0.3957  0.5460  0.7248  11.00000  0.05    0.30
Q10   1   0.4329  0.3119  0.5212  11.00000  0.05    0.28
Q11   1   0.6099  0.3768  0.5761  11.00000  0.05    0.26
Q12   1   0.4352  0.1448  0.4616  11.00000  0.05    0.26
Q13   1  -0.0801  0.4663  0.4606  11.00000  0.05    0.24
Q14   1   0.7674  0.3088  0.7156  11.00000  0.05    0.22
Q15   1   0.1010  0.3873  0.4331  11.00000  0.05    0.19
Q16   1   0.1110  0.2850  0.3769  11.00000  0.05    0.17
Q17   1   0.2532  0.2003  0.5265  11.00000  0.05    0.16
Q18   1   0.1158 -0.1635  0.5665  11.00000  0.05    0.16
Q19   1   0.0903  0.2880  0.4595  11.00000  0.05    0.16
Q20   1   0.1911  0.4205  0.5431  11.00000  0.05    0.16
;
_shelx_res_checksum              85666
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
Br1 Br 0.35964(3) 0.54223(3) 0.65711(2) 0.01428(7) Uani 1 1 d . .
C1 C 0.1106(3) 0.2614(3) 0.42125(18) 0.0205(4) Uani 1 1 d . .
H1A H 0.1002 0.3454 0.3577 0.031 Uiso 1 1 calc R U
H1B H 0.0616 0.3219 0.4773 0.031 Uiso 1 1 calc R U
H1C H 0.0382 0.1494 0.3938 0.031 Uiso 1 1 calc R U
S1 S 0.35200(7) 0.20219(6) 0.48513(4) 0.01304(11) Uani 1 1 d . .
B1 B 0.4882(3) 0.4257(3) 0.55129(18) 0.0114(4) Uani 1 1 d . .
Br2 Br 0.73626(3) 0.30866(3) 0.64381(2) 0.01599(7) Uani 1 1 d . .
C2 C 0.3265(3) 0.0725(3) 0.60344(18) 0.0188(4) Uani 1 1 d . .
H2A H 0.2577 -0.0415 0.5762 0.028 Uiso 1 1 calc R U
H2B H 0.2572 0.1460 0.6441 0.028 Uiso 1 1 calc R U
H2C H 0.4507 0.0424 0.6545 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
Br1 0.01675(12) 0.01579(12) 0.01189(11) -0.00141(6) 0.00671(8) 0.00138(7)
C1 0.0131(10) 0.0249(12) 0.0211(11) -0.0010(9) 0.0012(8) -0.0034(9)
S1 0.0144(2) 0.0127(2) 0.0135(2) -0.00133(16) 0.00651(19) -0.00192(17)
B1 0.0112(10) 0.0123(10) 0.0109(10) 0.0000(8) 0.0038(8) 0.0005(8)
Br2 0.01245(12) 0.01814(12) 0.01569(12) 0.00389(7) 0.00160(8) 0.00290(7)
C2 0.0241(11) 0.0162(10) 0.0196(11) 0.0025(8) 0.0120(9) -0.0024(8)
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'
Br Br -0.2901 2.4595 '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 .
C1 S1 C2 98.56(10) .
C1 S1 B1 108.37(10) .
C2 S1 B1 105.07(9) .
B1 B1 S1 111.45(17) 3_666
B1 B1 Br1 112.90(18) 3_666
S1 B1 Br1 109.19(10) .
B1 B1 Br2 113.56(18) 3_666
S1 B1 Br2 99.30(9) .
Br1 B1 Br2 109.57(10) .
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
Br1 B1 2.026(2) .
C1 S1 1.793(2) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
S1 C2 1.799(2) .
S1 B1 1.961(2) .
B1 B1 1.715(4) 3_666
B1 Br2 2.051(2) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
