Generation of aminoborane monomers RR'N[double bond, length as m-dash]BH2 from amine-boronium cations [RR'NH-BH2L]^+^: metal catalyst-free formation of polyaminoboranes at ambient temperature
Owen J. Metters; Andy M. Chapman; Alasdair P. M. Robertson; Christopher H. Woodall; Paul J. Gates; Duncan F. Wass; Ian Manners; Chem.Commun. 50 (2014) 12146–; doi:10.1039/C4cc05145A

data_7115718
_publ_section_title
;
 Generation of aminoborane monomers RR'N[double bond, length as m-dash]BH2
 from amine-boronium cations [RR'NH-BH2L]^+^: metal catalyst-free
 formation of polyaminoboranes at ambient temperature
;
_journal_name_full               Chem.Commun.
_journal_page_first              12146
_journal_paper_doi               10.1039/C4cc05145A
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C24 B F20), 2(C5 H17 B N O), C H2 Cl2'
_chemical_formula_sum            'C29.5 H18 B2 Cl F20 N O'
_chemical_formula_weight         839.52
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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                 98.837(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8098(2)
_cell_length_b                   21.0038(6)
_cell_length_c                   17.4138(5)
_cell_measurement_reflns_used    5891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.92
_cell_measurement_theta_min      2.27
_cell_volume                     3183.99(15)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30403
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.4952
_exptl_absorpt_correction_T_min  0.4629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         14515
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                10973
_reflns_number_total             14515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05145a2.cif
_cod_data_source_block           amc365_0m
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7115718