Silylative Coupling of Terminal Alkynes with Iodosilanes: New Catalytic Activation of sp-Hybridized Carbon−Hydrogen Bonds
Kownacki, Ireneusz; Marciniec, Bogdan; Dudziec, Beata; Kubicki, Maciej; Organometallics 30 (2011) 2539–; doi:10.1021/om200038r

data_4064315
_publ_contact_author
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Maciej Kubicki   
Faculty of Chemistry 
Adam Mickiewicz University
Grunwaldzka 6              
60-780 Pozna\'n   
Poland             
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_publ_section_title
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 Silylative Coupling of Terminal Alkynes with Iodosilanes: New Catalytic
 Activation of sp-Hybridized Carbon&#x2212;Hydrogen Bonds
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2539
_journal_paper_doi               10.1021/om200038r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C22 H32 Cl Ir N2 O Si'
_chemical_formula_sum            'C22 H32 Cl Ir N2 O Si'
_chemical_formula_weight         596.24
_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                82.076(10)
_cell_angle_beta                 85.871(10)
_cell_angle_gamma                62.673(12)
_cell_formula_units_Z            2
_cell_length_a                   7.9314(9)
_cell_length_b                   8.6025(10)
_cell_length_c                   21.520(3)
_cell_measurement_reflns_used    3163
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      26.8326
_cell_measurement_theta_min      2.6688
_cell_volume                     1291.9(3)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction (2009))'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction (2009))'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction (2009))'
_computing_molecular_graphics    'Stereochemical Workstation (Siemens, 1989)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.1929
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       \w-scan
_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  0.0598
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7355
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    5.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.113
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4547
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                3139
_reflns_number_total             4547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200038r_si_002.cif
_cod_data_source_block           IIIa
_cod_database_code               4064315