Structures and Aggregation of the Methylamine-Borane Molecules, MenH3-nN.BH3 (n= 1-3), Studied by X-ray Diffraction, Gas-Phase Electron Diffraction, and Quantum Chemical Calculations
Simon Aldridge; Anthony J. Downs; Christina Y. Tang; Simon Parsons; Michael C. Clarke; Russell D. L. Johnstone; Heather E. Robertson; David W. H. Rankin; Derek A. Wann; Journal of the American Chemical Society 131 (2009) 2231–2243; doi:10.1021/ja807545p

data_4103909
_publ_contact_author_email       S.Parsons@ed.ac.uk
_publ_contact_author_name        S.Parsons
_publ_section_title
;
 Structures and Aggregation of the Methylamine-Borane Molecules,
 MenH3-nN.BH3 (n= 1-3), Studied by X-ray Diffraction, Gas-Phase Electron
 Diffraction, and Quantum Chemical Calculations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2231
_journal_page_last               2243
_journal_paper_doi               10.1021/ja807545p
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        'Christina Tang & Tony Downs'
_chemical_formula_moiety         MeNH2-BH3
_chemical_formula_sum            'C H8 B N'
_chemical_formula_weight         44.89
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             07-07-11
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1350(8)
_cell_length_b                   6.5575(4)
_cell_length_c                   4.9194(3)
_cell_measurement_reflns_used    889
_cell_measurement_temperature    150
_cell_measurement_theta_max      16
_cell_measurement_theta_min      1
_cell_volume                     359.20(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1813
_diffrn_reflns_theta_full        30.708
_diffrn_reflns_theta_max         31.987
_diffrn_reflns_theta_min         5.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.048
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.830
_exptl_crystal_description       plate
_exptl_crystal_F_000             104
_exptl_crystal_recrystallization_method
;
?
;
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.11
_refine_ls_extinction_coef       290(90)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0019
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         663
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000197
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.03P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1054
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1054
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                505
_reflns_number_total             663
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_scale          10.9(13)
_oxford_structure_analysis_title 'MeNH2-BH3 in Pnma'
_cod_data_source_file            ja807545p_si_001.cif
_cod_data_source_block           menh2bh3
_cod_original_formula_sum        'C1 H8 B1 N1'
_cod_database_code               4103909