Base-Promoted Ammonia Borane Hydrogen-Release
Daniel W. Himmelberger; Chang Won Yoon; Martin E. Bluhm; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 131 (2009) 14101–14110; doi:10.1021/ja905015x

data_4105085
_publ_section_title
;
 Base-Promoted Ammonia Borane Hydrogen-Release
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14101
_journal_page_last               14110
_journal_paper_doi               10.1021/ja905015x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C18 H44 B2 K N O6'
_chemical_formula_weight         431.26
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5950(7)
_cell_length_b                   14.7764(9)
_cell_length_c                   29.2387(18)
_cell_measurement_temperature    143(1)
_cell_volume                     5009.5(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20472
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
    Shape function based on spherical harmonics.
    Highest even and odd order for spherical harmonics:  4  and  3
    Laue group:  mmm
    Friedel opposites are equivalent.
;
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+1.3384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4944
_reflns_number_total             5721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905015x_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4105085