New route to 1-thia-closo-dodecaborane(11), closo-1-SB11H11, and its halogenation reactions. The effect of the halogen on the dipole moments and the NMR spectra and the importance of spin-orbit coupling for the 11B chemical shifts.
Machácek, Jan; Plesek, Jaromír; Holub, Josef; Hnyk, Drahomír; Vsetecka, Václav; Císarová, Ivana; Kaupp, Martin; Stíbr, Bohumil; Dalton transactions (Cambridge, England : 2003)  (2006) 1024–1029; doi:10.1039/b512345c

data_7006634
_publ_section_title
;
 New route to 1-thia-closo-dodecaborane(11), closo-1-SB11H11, and its
 halogenation reactions. The effect of the halogen on the dipole
 moments and the NMR spectra and the importance of spin-orbit coupling
 for the 11B chemical shifts.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1024
_journal_page_last               1029
_journal_paper_doi               10.1039/b512345c
_journal_year                    2006
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'B11 H10 I S'
_chemical_formula_sum            'B11 H10 I S'
_chemical_formula_weight         287.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.258(2)
_cell_length_b                   13.260(3)
_cell_length_c                   11.463(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      14
_cell_volume                     1103.2(4)
_computing_cell_refinement       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_collection       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_reduction        'Jana98 (Petricek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CAD4-MACHIII
_diffrn_measurement_method       'theta-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2088
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        1.7
_diffrn_standards_interval_time  1hour
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.024
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'JANA98,Petricek, 1998'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0157(6)
_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   1.092
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0273P)^2^+1.7095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                1808
_reflns_number_total             1934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b512345c.txt
_cod_data_source_block           sb11cry
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7006634