Metal-free dehydrogenation of amine-boranes by an N-heterocyclic carbene.
Sabourin, Kyle J.; Malcolm, Adam C.; McDonald, Robert; Ferguson, Michael J.; Rivard, Eric; Dalton transactions (Cambridge, England : 2003) 42 (2013) 4625–4632; doi:10.1039/c3dt32988g

data_7022758
_publ_section_title
;
 Metal-free dehydrogenation of amine-boranes by an N-heterocyclic carbene.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4625
_journal_page_last               4632
_journal_paper_doi               10.1039/c3dt32988g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C31 H51 B2 N3, 1.5(C4 H8 O)'
_chemical_formula_sum            'C37 H63 B2 N3 O1.5'
_chemical_formula_weight         595.52
_chemical_name_common            3
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.4379(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8935(5)
_cell_length_b                   13.6955(4)
_cell_length_c                   17.7459(5)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.90
_cell_measurement_theta_min      4.15
_cell_volume                     3917.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXD (Schneider & Sheldrick, 2002)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26141
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         69.88
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as
disordered or partial-occupancy solvent tetrahydrofuran oxygen or
carbon atoms were unsuccessful. The data were corrected for
disordered electron density through use of the SQUEEZE procedure
(Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201)
as implemented in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46,
C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 7-13. PLATON - a
multipurpose crystallographic tool. Utrecht University, Utrecht, The
Netherlands). A total solvent-accessible void volume of 1174.0 cubic
Angstroms with a total electron count of 244 (consistent with 6
molecules of solvent tetrahydrofuran, or 1.5 molecules per formula
unit of the molecule of interest) was found in the unit cell.
;
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.033
_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     349
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0757P)^2^+0.4605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                6132
_reflns_number_total             7069
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt32988g.txt
_cod_data_source_block           riv12b9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7022758
_diffrn_reflns_av_unetl/netl     0.0382