A convenient cyanide-free “one-pot” synthesis of nido-Me3N-7-CB10H12 and nido-7-CB10H13−
Batsanov, Andrei S.; Fox, Mark A.; Goeta, Andrés E.; Howard, Judith A. K.; Hughes, Andrew K.; Malget, John M.; Journal of the Chemical Society, Dalton Transactions  (2002) 2624–; doi:10.1039/b200930g

data_7011523
_publ_section_title
;
 A convenient cyanide-free &#x201C;one-pot&#x201D; synthesis of
 nido-Me3N-7-CB10H12 and nido-7-CB10H13&#x2212;
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2624
_journal_paper_doi               10.1039/b200930g
_journal_year                    2002
_chemical_formula_moiety         'C6 H25 B10 N'
_chemical_formula_sum            'C6 H25 B10 N'
_chemical_formula_weight         219.37
_chemical_name_common            nido-^t^BuMeHN-7-CB~10~H~12~
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.852(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3418(14)
_cell_length_b                   8.8099(11)
_cell_length_c                   13.7750(15)
_cell_measurement_reflns_used    869
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      10.22
_cell_volume                     1369.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART-1K CCD Diffractometer'
_diffrn_measurement_method       \w
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15282
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_T_max  0.9931
_exptl_absorpt_correction_T_min  0.9872
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0644P)^2^+0.4420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                2662
_reflns_number_total             3403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200930g.txt
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011523