Regioselective and Stereospecific Dehydrogenative Annulation Utilizing Silylium Ion-Activated Alkenes.
Arii, Hidekazu; Yano, Yuto; Nakabayashi, Kenichi; Yamaguchi, Syuhei; Yamamura, Masaki; Mochida, Kunio; Kawashima, Takayuki; The Journal of organic chemistry 81 (2016) 6314–6319; doi:10.1021/acs.joc.6b00793

data_4036889
_publ_section_title
;
 Regioselective and Stereospecific Dehydrogenative Annulation Utilizing
 Silylium Ion-Activated Alkenes.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6314
_journal_page_last               6319
_journal_paper_doi               10.1021/acs.joc.6b00793
_journal_volume                  81
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_sum            'C24 H36 Si'
_chemical_formula_weight         352.61
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-02T10:07:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.437(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.106(3)
_cell_length_b                   15.762(6)
_cell_length_c                   16.823(7)
_cell_measurement_reflns_used    8673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2869
_cell_measurement_theta_min      2.4419
_cell_volume                     2131.3(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rgaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32037
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.98
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.778
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 2981 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.44(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9599
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                7941
_reflns_number_total             9599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00793_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2131.5(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C48 H72 Si2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     705.23
_cod_database_code               4036889
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.994