Preparation of Ammonia Borane in High Yield and Purity, Methanolysis, and Regeneration
Ramachandran, P. Veeraraghavan; Gagare, Pravin D.; Inorganic Chemistry 46 (2007) 7810–7817; doi:10.1021/ic700772a

data_4333352
_publ_section_title
;
 Preparation of Ammonia Borane in High Yield and Purity, Methanolysis, and
 Regeneration
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7810
_journal_page_last               7817
_journal_paper_doi               10.1021/ic700772a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C H8 B4 N2 O12'
_chemical_formula_weight         283.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.537(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1997(8)
_cell_length_b                   10.6039(10)
_cell_length_c                   7.2604(8)
_cell_measurement_temperature    260(2)
_cell_volume                     548.15(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2192
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.9382
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(3)
_refine_ls_extinction_coef       0.20(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2186
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.161
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1285P)^2^+0.0057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                1846
_reflns_number_total             2186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700772asup1.cif
_cod_data_source_block           xl
_cod_database_code               4333352