Ammonia Triborane: A New Synthesis, Structural Determinations, and Hydrolytic Hydrogen-Release Properties
Chang Won Yoon; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 131 (2009) 855–864; doi:10.1021/ja808045p

data_4103783
_publ_section_title
;
 Ammonia Triborane: A New Synthesis, Structural Determinations, and
 Hydrolytic Hydrogen-Release Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              855
_journal_page_last               864
_journal_paper_doi               10.1021/ja808045p
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C12 H34 B3 N O6'
_chemical_formula_weight         320.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.555(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.961(3)
_cell_length_b                   8.5678(9)
_cell_length_c                   21.910(3)
_cell_measurement_temperature    143(1)
_cell_volume                     3779.0(8)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22010
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5869
_reflns_number_total             6590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808045p_si_002_1.cif
_cod_data_source_block           Penn3304
_cod_original_cell_volume        3779.1(8)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4103783