#------------------------------------------------------------------------------
#$Date: 2017-06-01 04:31:03 +0300 (Thu, 01 Jun 2017) $
#$Revision: 197115 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/02/7120215.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_7120215
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 Cl4 S2'
_chemical_formula_sum            'C4 H12 B2 Cl4 S2'
_chemical_formula_weight         287.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9144(6)
_cell_length_b                   10.8859(7)
_cell_length_c                   11.2982(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      3.31
_cell_volume                     1219.38(13)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014) '
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15556
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.665
_diffrn_reflns_theta_min         3.313
_diffrn_source
'rotating-anode X-ray tube or sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0168
_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)+(0.0244P)²+0.3524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1239
_reflns_number_total             1290
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc03148c2.cif
_cod_data_source_block           done
_cod_database_code               7120215
_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   0.518
_shelx_estimated_absorpt_t_max   0.704
_exptl_absorpt_special_details
;The crystal was immersed in a film of perfluoropolyether oil, 
mounted on a a glass fiber and transferred to stream of cold nitrogen.
;
_shelx_res_file
;

    test_a.res created by SHELXL-2014/7


TITL test_a.res in Pbca
REM Old TITL test in Pbca
REM SHELXT solution in Pbca
REM R1 0.063,  Rweak 0.001,  Alpha 0.008,  Orientation as input
REM Formula found by SHELXT:  C2 B S Cl2
CELL  0.71073   9.9144  10.8859  11.2982   90.000   90.000   90.000
ZERR    4.000   0.0006   0.0007   0.0007    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H B S CL
UNIT 16 48 8 8 16
TEMP -173.000
SIZE 0.30 0.50 0.60
L.S. 10
BOND $H
LIST 6
ACTA 52
CONF
shel 999 0.78
FMAP 2
PLAN 20
WGHT    0.024400    0.352400
FVAR       0.51849
CL1   5    0.705809    0.575278    0.427995    11.00000    0.01225    0.01830 =
         0.01854    0.00009    0.00449   -0.00017
S1    4    0.508979    0.682741    0.617754    11.00000    0.01510    0.01463 =
         0.01439   -0.00238    0.00175   -0.00065
C1    1    0.647724    0.646942    0.714330    11.00000    0.02616    0.02073 =
         0.01608   -0.00145   -0.00569    0.00063
AFIX 137
H1A   2    0.730522    0.638836    0.667600    11.00000   -1.50000
H1B   2    0.629456    0.569496    0.755545    11.00000   -1.50000
H1C   2    0.658795    0.712986    0.772467    11.00000   -1.50000
AFIX   0
B1    3    0.527840    0.571930    0.480278    11.00000    0.01211    0.01487 =
         0.01021   -0.00024    0.00050    0.00106
CL2   5    0.417631    0.648286    0.368126    11.00000    0.01682    0.01836 =
         0.01527    0.00481   -0.00238    0.00171
C2    1    0.562686    0.830169    0.563645    11.00000    0.02133    0.01377 =
         0.02362   -0.00063   -0.00108   -0.00087
AFIX 137
H2A   2    0.648984    0.821332    0.522214    11.00000   -1.50000
H2B   2    0.573527    0.886879    0.630336    11.00000   -1.50000
H2C   2    0.494821    0.862650    0.508894    11.00000   -1.50000
AFIX   0
HKLF 4

REM  test_a.res in Pbca
REM R1 =  0.0168 for    1239 Fo > 4sig(Fo)  and  0.0176 for all    1290 data
REM     57 parameters refined using      0 restraints

END

WGHT      0.0244      0.3524

REM Highest difference peak  0.409,  deepest hole -0.158,  1-sigma level  0.049
Q1    1   0.5000  0.5000  0.5000  10.50000  0.05    0.41
Q2    1   0.5354  0.7622  0.5899  11.00000  0.05    0.35
Q3    1   0.5698  0.6594  0.6655  11.00000  0.05    0.29
Q4    1   0.5181  0.6216  0.5557  11.00000  0.05    0.29
Q5    1   0.6180  0.5688  0.4404  11.00000  0.05    0.26
Q6    1   0.4239  0.6847  0.6351  11.00000  0.05    0.23
Q7    1   0.3625  0.5870  0.3584  11.00000  0.05    0.22
Q8    1   0.7400  0.5192  0.4568  11.00000  0.05    0.21
Q9    1   0.7308  0.6419  0.4294  11.00000  0.05    0.20
Q10   1   0.4772  0.8719  0.5715  11.00000  0.05    0.19
Q11   1   0.4828  0.6078  0.3909  11.00000  0.05    0.18
Q12   1   0.4754  0.7217  0.3741  11.00000  0.05    0.17
Q13   1   0.3362  0.6748  0.3860  11.00000  0.05    0.17
Q14   1   0.6121  0.5969  0.7418  11.00000  0.05    0.15
Q15   1   0.3799  0.7257  0.3988  11.00000  0.05    0.12
Q16   1   0.5413  0.8373  0.5210  11.00000  0.05    0.12
Q17   1   0.6070  0.8288  0.5308  11.00000  0.05    0.12
Q18   1   0.7030  0.6199  0.6820  11.00000  0.05    0.10
Q19   1   0.5742  0.8591  0.6080  11.00000  0.05    0.10
Q20   1   0.4973  0.8144  0.4144  11.00000  0.05    0.08
;
_shelx_res_checksum              34392
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Cl1 Cl 0.70581(3) 0.57528(2) 0.42800(2) 0.01637(9) Uani 1 1 d . .
S1 S 0.50898(3) 0.68274(2) 0.61775(2) 0.01471(9) Uani 1 1 d . .
C1 C 0.64772(12) 0.64694(11) 0.71433(10) 0.0210(3) Uani 1 1 d . .
H1A H 0.7305 0.6388 0.6676 0.031 Uiso 1 1 calc R U
H1B H 0.6295 0.5695 0.7555 0.031 Uiso 1 1 calc R U
H1C H 0.6588 0.7130 0.7725 0.031 Uiso 1 1 calc R U
B1 B 0.52784(12) 0.57193(11) 0.48028(10) 0.0124(2) Uani 1 1 d . .
Cl2 Cl 0.41763(3) 0.64829(2) 0.36813(2) 0.01682(9) Uani 1 1 d . .
C2 C 0.56269(12) 0.83017(10) 0.56365(11) 0.0196(2) Uani 1 1 d . .
H2A H 0.6490 0.8213 0.5222 0.029 Uiso 1 1 calc R U
H2B H 0.5735 0.8869 0.6303 0.029 Uiso 1 1 calc R U
H2C H 0.4948 0.8627 0.5089 0.029 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
Cl1 0.01225(14) 0.01830(15) 0.01854(15) 0.00009(10) 0.00449(9) -0.00017(9)
S1 0.01510(15) 0.01463(15) 0.01439(15) -0.00238(10) 0.00175(9) -0.00065(10)
C1 0.0262(6) 0.0207(6) 0.0161(5) -0.0014(4) -0.0057(5) 0.0006(5)
B1 0.0121(6) 0.0149(6) 0.0102(5) -0.0002(5) 0.0005(4) 0.0011(4)
Cl2 0.01682(15) 0.01836(15) 0.01527(14) 0.00481(10) -0.00238(9) 0.00171(9)
C2 0.0213(6) 0.0138(5) 0.0236(6) -0.0006(5) -0.0011(5) -0.0009(4)
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'
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
C2 S1 C1 99.97(6) .
C2 S1 B1 104.46(5) .
C1 S1 B1 105.80(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 .
B1 B1 Cl1 113.86(10) 5_666
B1 B1 Cl2 113.16(10) 5_666
Cl1 B1 Cl2 109.30(6) .
B1 B1 S1 108.78(9) 5_666
Cl1 B1 S1 109.11(6) .
Cl2 B1 S1 101.90(6) .
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
Cl1 B1 1.8611(12) .
S1 C2 1.7980(12) .
S1 C1 1.7985(12) .
S1 B1 1.9755(12) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
B1 B1 1.719(2) 5_666
B1 Cl2 1.8683(12) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
