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_4103911
_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_absolute_configuration unk
_chemical_compound_source        'Christina Tang, Oxford.'
_chemical_formula_moiety         Me3N-BH3
_chemical_formula_sum            'C3 H12 B N'
_chemical_formula_weight         72.95
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             07-07-27
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.0792(5)
_cell_length_b                   9.0792(5)
_cell_length_c                   5.8922(5)
_cell_measurement_reflns_used    303
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     420.63(5)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.985
_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  0.024
_diffrn_reflns_limit_h_max       10
_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            599
_diffrn_reflns_reduction_process
;
 Merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
;
_diffrn_reflns_theta_full        27.463
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         6.238
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.049
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.864
_exptl_crystal_description       block
_exptl_crystal_F_000             126
_exptl_crystal_recrystallization_method
;
?
;
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.10
_refine_diff_density_min         -0.10
_refine_ls_extinction_coef       190(90)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         130
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0738
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0738
_reflns_limit_h_max              0
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                128
_reflns_number_total             130
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          3.5(3)
_oxford_structure_analysis_title 'Me3N-BH3 in R3m'
_cod_data_source_file            ja807545p_si_003.cif
_cod_data_source_block           me3nbh3
_cod_original_sg_symbol_H-M      'R 3 m '
_cod_original_formula_sum        'C3 H12 B1 N1'
_cod_database_code               4103911