Synthesis and Reactivity of Silyl Vinylketenes: A Formal Interrupted Dötz Benzannulation with Unexpected Silyl Migration
Moser, William H.; Sun, Liangdong; Huffman, John C.; Organic Letters 3 (2001) 3389–; doi:10.1021/ol016615y

data_1507535
_publ_section_title
;
 Synthesis and Reactivity of Silyl Vinylketenes:&#x2009; A Formal
 Interrupted D\"otz Benzannulation with Unexpected Silyl Migration
;
_journal_issue                   21
_journal_name_full               'Organic Letters'
_journal_page_first              3389
_journal_paper_doi               10.1021/ol016615y
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C26 H28 Cr O5 Si'
_chemical_formula_weight         500.587
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 99.7669(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5976(2)
_cell_length_b                   28.7405(9)
_cell_length_c                   13.2540(4)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.64
_cell_volume                     2476.78(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
'   0.30 degree frames measured for  10.13 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67757
_diffrn_reflns_theta_full        30.123
_diffrn_reflns_theta_max         30.123
_diffrn_reflns_theta_min         1.202
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  614
_diffrn_standards_number         7117
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          .06
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.00000022(5)
_refine_ls_extinction_expression
;                                                                               
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)                         
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   0.9148
_refine_ls_hydrogen_treatment    'isotropic refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         3533
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.0089
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0283
_reflns_number_gt                3533
_reflns_number_total             7240
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_data_source_file            ol016615y_s2.cif
_cod_data_source_block           MSC01044
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C26 H28 Cr1 O5 Si1'
_cod_database_code               1507535