Electrospray Ionization Mass Spectrometry Studies on the Mechanism of Hydrosilylation of Terminal Alkynes Using an N-Heterocyclic Carbene Complex of Iridium, Allow Detection/Characterization of All Reaction Intermediates⊥
Vicent, Cristian; Viciano, Mónica; Mas-Marzá, Elena; Sanaú, Mercedes; Peris, Eduardo; Organometallics 25 (2006) 3713–; doi:10.1021/om0602308

data_4075338
_publ_section_title
;
 Electrospray Ionization Mass Spectrometry Studies on the Mechanism of
 Hydrosilylation of Terminal Alkynes Using an N-Heterocyclic Carbene
 Complex of Iridium, Allow Detection/Characterization of All Reaction
 Intermediates&#x22A5;
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3713
_journal_paper_doi               10.1021/om0602308
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C23 H28 Cl3 Ir N4 Si, C H3 O'
_chemical_formula_sum            'C24 H31 Cl3 Ir N4 O Si'
_chemical_formula_weight         718.17
_chemical_name_systematic
; 
 ? 
;
_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                117.98(13)
_cell_angle_beta                 97.60(14)
_cell_angle_gamma                105.83(14)
_cell_formula_units_Z            2
_cell_length_a                   11.221(7)
_cell_length_b                   12.706(8)
_cell_length_c                   13.236(8)
_cell_measurement_reflns_used    4106
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.56
_cell_volume                     1526(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      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  '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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7235
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.438
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+3.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                3677
_reflns_number_total             4303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0602308si20060313_115147.cif
_cod_data_source_block           str770m
_cod_original_cell_volume        1526.3(28)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075338