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_4106463
_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         'C37 H76 B Ir N P2, C32 H12 B F24'
_chemical_formula_sum            'C69 H88 B2 F24 Ir N P2'
_chemical_formula_weight         1663.16
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.6288(5)
_cell_angle_beta                 84.1492(5)
_cell_angle_gamma                86.7710(5)
_cell_formula_units_Z            2
_cell_length_a                   12.68240(10)
_cell_length_b                   17.1470(2)
_cell_length_c                   17.4894(2)
_cell_measurement_reflns_used    19363
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      5.097
_cell_volume                     3748.65(7)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30029
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         5.08
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         17753
_refine_ls_number_restraints     800
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+3.2895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                14817
_reflns_number_total             17753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2040738_si_003.cif
_cod_data_source_block           184abc10
_cod_database_code               4106463