Synthesis of C-substituted t-BuNH-8,9-R,R'-nido-7,8,9-C3B8H9 (R,R' = H,H; MeH; Me,Me; Ph,H and Ph,Ph) tricarbollide compounds and their tautomeric conversions. Effect of substituents on tautomeric equilibria between neutral and zwitterionic forms.
Bakardjiev, Mario; Holub, Josef; Stíbr, Bohumil; Císarová, Ivana; Dalton transactions (Cambridge, England : 2003) 39 (2010) 4186–4190; doi:10.1039/b924754h

data_7025052
_publ_section_title
;
 Synthesis of C-substituted t-BuNH-8,9-R,R'-nido-7,8,9-C3B8H9 (R,R' = H,H;
 MeH; Me,Me; Ph,H and Ph,Ph) tricarbollide compounds and their tautomeric
 conversions. Effect of substituents on tautomeric equilibria between
 neutral and zwitterionic forms.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4186
_journal_page_last               4190
_journal_paper_doi               10.1039/b924754h
_journal_volume                  39
_journal_year                    2010
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C8 H23 B8 N'
_chemical_formula_sum            'C8 H23 B8 N'
_chemical_formula_weight         219.75
_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                 111.6510(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9813(2)
_cell_length_b                   11.5093(2)
_cell_length_c                   12.7934(2)
_cell_measurement_reflns_used    3266
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1365.99(4)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24777
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0630P)^2^+0.2489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                2746
_reflns_number_total             3120
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b924754h.txt
_cod_data_source_block           hol427-2-rez
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7025052