Synthesis of the Long-Sought Unsubstituted Aminodiboranate Na(H3B-NH2-BH3) and Its N-Alkyl Analogs
Scott R. Daly; Brian J. Bellott; Do Young Kim; Gregory S. Girolami; Journal of the American Chemical Society 132 (2010) 7254–7255; doi:10.1021/ja1016427

data_4102475
_publ_contact_author_address
;Department of Chemistry, Box 4-6
University of Illinois at Urbana-Champaign
600 South Mathews
Urbana, IL 61801
;
_publ_contact_author_email       girolami@scs.illinois.edu
_publ_contact_author_fax         '(217) 333-2685'
_publ_contact_author_name        'Gregory S. Girolami'
_publ_contact_author_phone       ' (217) 333-2729'
_publ_section_title
;
 Synthesis of the Long-Sought Unsubstituted Aminodiboranate
 Na(H3B-NH2-BH3) and Its N-Alkyl Analogs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7254
_journal_page_last               7255
_journal_paper_doi               10.1021/ja1016427
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C3 H14 B2 N Na O'
_chemical_formula_weight         124.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.984(2)
_cell_angle_beta                 97.495(2)
_cell_angle_gamma                114.189(2)
_cell_formula_units_Z            4
_cell_length_a                   8.2911(3)
_cell_length_b                   9.9884(4)
_cell_length_c                   10.8264(4)
_cell_measurement_reflns_used    975
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      1.91
_cell_volume                     807.02(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11540
_diffrn_reflns_theta_full        27.28
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.98864
_exptl_absorpt_correction_T_min  0.96783
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP/SHELXTL
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                2784
_reflns_number_total             3563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1016427_si_002_2.cif
_cod_data_source_block           fa51d_face
_cod_database_code               4102475