Catching the First Oligomerization Event in the Catalytic Formation of Polyaminoboranes: H3B.NMeHBH2.NMeH2 Bound to Iridium
Heather C. Johnson; Alasdair P. M. Robertson; Adrian B. Chaplin; Laura J. Sewell; Amber L. Thompson; Mairi F. Haddow; Ian Manners; Andrew S. Weller; Journal of the American Chemical Society 133 (2011) 11076–11079; doi:10.1021/ja2040738

data_4106462
_publ_section_title
;
 Catching the First Oligomerization Event in the Catalytic Formation of
 Polyaminoboranes: H3B.NMeHBH2.NMeH2 Bound to Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11076
_journal_page_last               11079
_journal_paper_doi               10.1021/ja2040738
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C2 H14 B2 N2'
_chemical_formula_sum            'C2 H14 B2 N2'
_chemical_formula_weight         87.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.081(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7173(4)
_cell_length_b                   8.5002(3)
_cell_length_c                   9.0429(3)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      3.30
_cell_volume                     666.30(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8590
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.875
_exptl_crystal_description       plate
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1682P)^2^+0.3377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2593
_refine_ls_wR_factor_ref         0.2667
_reflns_number_gt                1662
_reflns_number_total             1856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2040738_si_002.cif
_cod_data_source_block           ar4_0m
_cod_database_code               4106462