Silylene-Mediated Polarity Reversal of Dienoates: Additions of Dienoates to Aldehydes at the δ-Position To Form trans-Dioxasilacyclononenes
Christian C. Ventocilla; K. A. Woerpel; Journal of the American Chemical Society 133 (2011) 406–408; doi:10.1021/ja109631z

data_4105529
_publ_section_title
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 Silylene-Mediated Polarity Reversal of Dienoates: Additions of Dienoates
 to Aldehydes at the \d-Position To Form trans-Dioxasilacyclononenes
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              406
_journal_page_last               408
_journal_paper_doi               10.1021/ja109631z
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C24 H38 O3 Si'
_chemical_formula_weight         402.63
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                76.7490(10)
_cell_angle_beta                 84.1220(10)
_cell_angle_gamma                88.0320(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5046(6)
_cell_length_b                   10.9462(6)
_cell_length_c                   11.6723(7)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.31
_cell_volume                     1175.76(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13579
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                4614
_reflns_number_total             5135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109631z_si_003.cif
_cod_data_source_block           kaw134
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4105529