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_7115719
_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
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_journal_name_full               Chem.Commun.
_journal_page_first              12146
_journal_paper_doi               10.1039/C4cc05145A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C H7 B Cl N'
_chemical_formula_sum            'C H7 B Cl N'
_chemical_formula_weight         79.34
_chemical_name_systematic
;
 ? 
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-01
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7715(12)
_cell_length_b                   6.5471(6)
_cell_length_c                   5.2055(5)
_cell_measurement_reflns_used    5616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.69
_cell_measurement_theta_min      3.19
_cell_volume                     435.26(7)
_computing_cell_refinement       'Bruker Apex2 (Bruker, 2011)'
_computing_data_collection       'Bruker Apex2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT V7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker Apex II kappa with CCD area detector'
_diffrn_measurement_method       'phi and omega scans, 2deg width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10841
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.69
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         1044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0978P)^2^+0.7538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                939
_reflns_number_total             1044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05145a2.cif
_cod_data_source_block           OM25
_cod_database_code               7115719
_olex2_refinement_description
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1. Others
 Fixed Sof: H1(0.5) H2(0.5) H3(0.5)
 Fixed U12: C1(0) B1(0) N1(0) Cl1(0)
 Fixed U23: C1(0) B1(0) N1(0) Cl1(0)
 Fixed Uiso: H1(0.036) H2(0.036) H3(0.036)
 Fixed X: H1(0.4583) H2(0.4861) H3(0.4812)
 Fixed Y: C1(0.25) H1(0.2265) H2(0.1413) H3(0.3823) B1(0.25) N1(0.25) Cl1(0.25)
 Fixed Z: H1(-0.4417) H2(-0.1618) H3(-0.2116)
;