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_4330387
_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 C2 H10 C6 H5 C H2 O C O C H3        
;
_chemical_formula_sum            'C11 H20 B10 O2'
_chemical_formula_weight         292.37
_chemical_name_systematic
;
 1-acetoxymethyl-7-phenyl-1,2-dicarba-closo-dodecaborane(10) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.557(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2490(3)
_cell_length_b                   12.0008(3)
_cell_length_c                   13.2015(4)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.55
_cell_measurement_theta_min      4.29
_cell_volume                     1633.64(8)
_computing_cell_refinement       'Bruker SAINT 7.68A'
_computing_data_collection       'Bruker APEX 2010.9.1'
_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 0.982
_diffrn_measured_fraction_theta_max 0.983
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19681
_diffrn_reflns_theta_full        66.09
_diffrn_reflns_theta_max         66.09
_diffrn_reflns_theta_min         4.29
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_correction_T_min  0.9204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker SADABS 2008/1
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.6059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                2445
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014267_si_002_1.cif
_cod_data_source_block           '[B10C2H10](C6H5)(CH2OCOCH3)_(5b)'
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4330387