A Brønsted Acid Mediated Cascade Enone Synthesis from Aldehydes Containing a Tethered Propargylsilane
Rui Ramalho; Peter J. Jervis; Benson M. Kariuki; Alexander C. Humphries; Liam R. Cox; Journal of Organic Chemistry 73 (2008) 1631–1634; doi:10.1021/jo702351s

data_4023294
_publ_section_title
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 A Br\/onsted Acid Mediated Cascade Enone Synthesis from Aldehydes
 Containing a Tethered Propargylsilane
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1631
_journal_page_last               1634
_journal_paper_doi               10.1021/jo702351s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C21 H29 N O5 Si'
_chemical_formula_sum            'C21 H29 N O5 Si'
_chemical_formula_weight         403.54
_chemical_name_systematic
;
 ?
;
_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                 90.322(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8890(5)
_cell_length_b                   8.0262(3)
_cell_length_c                   18.0566(6)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      70.6
_cell_measurement_theta_min      2.78
_cell_volume                     2302.69(14)
_computing_cell_refinement       SAINTPLUS
_computing_data_collection       SMART
_computing_data_reduction        SAINTPLUS
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker Smart 6000 CCD'
_diffrn_measurement_method       'CCD slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13619
_diffrn_reflns_theta_full        70.60
_diffrn_reflns_theta_max         70.60
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.8209
_exptl_absorpt_correction_T_min  0.8039
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4197
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0800P)^2^+1.0974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                2829
_reflns_number_total             4197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo702351s-File004.cif
_cod_data_source_block           rr5144
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4023294