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_4064313
_publ_contact_author
;
Maciej Kubicki   
Faculty of Chemistry 
Adam Mickiewicz University
Grunwaldzka 6              
60-780 Pozna\'n   
Poland             
;
_publ_section_title
;
 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         'C17 H26 Si3'
_chemical_formula_sum            'C17 H26 Si3'
_chemical_formula_weight         314.65
_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                113.47(1)
_cell_angle_beta                 98.63(2)
_cell_angle_gamma                104.93(2)
_cell_formula_units_Z            4
_cell_length_a                   12.732(2)
_cell_length_b                   13.341(2)
_cell_length_c                   14.722(3)
_cell_measurement_reflns_used    11251
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      72.6515
_cell_measurement_theta_min      3.4098
_cell_volume                     2124.4(8)
_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      295(2)
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       /w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15792
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         72.76
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.43 (release 21-10-2010 CrysAlis171 .NET)
(compiled Oct 21 2010,17:48:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0300P)^2^+0.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                7120
_reflns_number_total             8197
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200038r_si_002.cif
_cod_data_source_block           17
_cod_original_cell_volume        2124.3(8)
_cod_database_code               4064313