Dimethylsulfide-dicarbaborane chemistry. Isolation and characterisation of isomers [9-(SMe2)-nido-7,8-C2B9H10-X-Me] (where X = 1, 2, 3 and 4) and some related compounds. An unusual skeletal rearrangement.
Grüner, Bohumír; Holub, Josef; Plesek, Jaromír; Stíbr, Bohumil; Thornton-Pett, Mark; Kennedy, John D.; Dalton transactions (Cambridge, England : 2003)  (2007) 4859–4865; doi:10.1039/b709526k

data_7006169
_publ_section_title
;
 Dimethylsulfide-dicarbaborane chemistry. Isolation and
 characterisation of isomers [9-(SMe2)-nido-7,8-C2B9H10-X-Me] (where X
 = 1, 2, 3 and 4) and some related compounds. An unusual skeletal
 rearrangement.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4859
_journal_page_last               4865
_journal_paper_doi               10.1039/b709526k
_journal_year                    2007
_chemical_formula_sum            'C5 H19 B9 S'
_chemical_formula_weight         208.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7170(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.65370(10)
_cell_length_b                   22.4790(3)
_cell_length_c                   8.86450(10)
_cell_measurement_reflns_used    19456
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     1248.12(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0097
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4664
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9220
_exptl_absorpt_correction_T_min  0.8746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.021(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.3865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                2312
_reflns_number_total             2367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709526k.txt
_cod_data_source_block           cz2
_cod_database_code               7006169