Acid-Induced Opening of [closo-B10H10]2- as a New Route to 6-Substituted nido-B10H13 Decaboranes and Related Carboranes
Oleg Bondarev; Yulia V. Sevryugina; Satish S. Jalisatgi; M. Frederick Hawthorne; Inorganic Chemistry 51 (2012) 9935–9942; doi:10.1021/ic3014267

data_4330388
_publ_section_title
;
 Acid-Induced Opening of [closo-B10H10]2- as a New Route to 6-Substituted
 nido-B10H13 Decaboranes and Related Carboranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9935
_journal_page_last               9942
_journal_paper_doi               10.1021/ic3014267
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
;
 B10 H13 C6 H4 C H3
;
_chemical_formula_sum            'C7 H20 B10'
_chemical_formula_weight         212.33
_chemical_name_systematic
;
 nido-6-tolyldecaborane(13) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.1729(3)
_cell_length_b                   14.8504(4)
_cell_length_c                   20.0887(6)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.14
_cell_measurement_theta_min      4.40
_cell_volume                     2736.51(14)
_computing_cell_refinement       'Bruker SAINT 7.68A'
_computing_data_collection       'Bruker APEX 2010.7'
_computing_data_reduction        'Bruker SADABS 2008/1'
_computing_molecular_graphics    'Bruker XP 5.1'
_computing_publication_material  'Bruker XCIF 2008/2'
_computing_structure_refinement  'Bruker SHELXTL 2008/4'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5 deg wide \w exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'ImuS micro-focus source with Quazar optics'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1214
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36256
_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         4.40
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker SADABS 2008/1
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0710P)^2^+0.9814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                1744
_reflns_number_total             2413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014267_si_002_2.cif
_cod_data_source_block           '[B10H13](p-Me-C6H4)_(1b)'
_cod_original_sg_symbol_Hall     '-P 2ac 2ab  '
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4330388