Diisobutylaluminum Hydride Promoted Cyclization of o-(Trimethylsilylethynyl)styrenes to Indenes.
Kinoshita, Hidenori; Hirai, Nobuyoshi; Miura, Katsukiyo; The Journal of organic chemistry 79 (2014) 8171–8181; doi:10.1021/jo501383v

data_4029872
_publ_section_title
;
 Diisobutylaluminum Hydride Promoted Cyclization of
 o-(Trimethylsilylethynyl)styrenes to Indenes.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8171
_journal_page_last               8181
_journal_paper_doi               10.1021/jo501383v
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C16 H24 Si2'
_chemical_formula_weight         272.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5758(8)
_cell_length_b                   24.740(2)
_cell_length_c                   16.4424(16)
_cell_measurement_temperature    296(2)
_cell_volume                     3488.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.1625
_diffrn_reflns_av_sigmaI/netI    0.1072
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19403
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.9458
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0572
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                6096
_reflns_number_total             7841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo501383v_si_002.cif
_cod_data_source_block           hirai2
_cod_depositor_comments          'Adding full bibliography for 4029872.cif.'
_cod_original_cell_volume        3488.0(6)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4029872