Metallaborane Reactivity. A Stoichiometric Mechanism for the Insertion of Two Alkynes into an Iridaborane Framework via a Disposable Molybdenum Chaperone
Frédéric de Montigny; Ramón Macias; Bruce C. Noll; Thomas P. Fehlner; Karine Costuas; Jean-Yves Saillard; Jean-François Halet; Journal of the American Chemical Society 129 (2007) 3392–3401; doi:10.1021/ja068999z

data_4109189
_publ_section_title
;
 Metallaborane Reactivity. A Stoichiometric Mechanism for the Insertion of
 Two Alkynes into an Iridaborane Framework via a Disposable Molybdenum
 Chaperone
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3392
_journal_page_last               3401
_journal_paper_doi               10.1021/ja068999z
_journal_volume                  129
_journal_year                    2007
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C38 H38 B3 Ir), C6 H14, 0.5(C14 H14)'
_chemical_formula_sum            'C89 H97 B6 Ir2'
_chemical_formula_weight         1615.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                84.8800(19)
_cell_angle_beta                 80.900(2)
_cell_angle_gamma                82.220(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4500(4)
_cell_length_b                   16.0200(5)
_cell_length_c                   20.6100(7)
_cell_measurement_reflns_used    7238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5669
_cell_measurement_theta_min      2.3537
_cell_volume                     3689.6(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART Apex CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            65043
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.3744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2004). SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         18074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                13037
_reflns_number_total             18074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068999zsi20061215_010253.cif
_cod_data_source_block           bcn215sx
_cod_database_code               4109189