Hydroalumination-Triggered Cyclization of Silylated 1,3-Dien-5-ynes to Polysubstituted Benzenes.
Kinoshita, Hidenori; Tohjima, Takayuki; Miura, Katsukiyo; Organic letters 16 (2014) 4762–4765; doi:10.1021/ol5022096

data_1517563
_publ_section_title
;
 Hydroalumination-Triggered Cyclization of Silylated 1,3-Dien-5-ynes to
 Polysubstituted Benzenes.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4762
_journal_page_last               4765
_journal_paper_doi               10.1021/ol5022096
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C27 H32 Si'
_chemical_formula_sum            'C27 H32 Si'
_chemical_formula_weight         384.61
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_formula_units_Z            4
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_cell_length_c                   17.4966(13)
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_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    Ortep3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir 97'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex II Ultra CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1218
_diffrn_reflns_av_unetI/netI     0.0591
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_min         1.559
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9791
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
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_refine_diff_density_max         0.402
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4676
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5022096_si_002.cif
_cod_data_source_block           2e
_cod_depositor_comments
'Adding full bibliography for 1517562--1517563.cif.'
_cod_database_code               1517563
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.992
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_shelx_res_checksum              49801
_shelx_hkl_checksum              83401