Me3SiI-promoted reaction of salicylic aldehydes with ketones: a facile way to construct benzopyranic [2,3-b]ketals and spiroketals
Feijun Wang; Mingliang Qu; Xi Lu; Feng Chen; Min Shi; Chem.Commun. 48 (2012) 6259–; doi:10.1039/c2cc32545d

data_7107866
_publ_section_title
;
 Me3SiI-promoted reaction of salicylic aldehydes with ketones: a facile
 way to construct benzopyranic [2,3-b]ketals and spiroketals
;
_journal_name_full               Chem.Commun.
_journal_page_first              6259
_journal_paper_doi               10.1039/c2cc32545d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C19 H20 O2'
_chemical_formula_weight         280.35
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   31.4581(18)
_cell_length_b                   31.4581(18)
_cell_length_c                   8.0818(6)
_cell_measurement_reflns_used    1754
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.516
_cell_measurement_theta_min      4.486
_cell_volume                     6926.3(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12654
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38194
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.105
_refine_diff_density_rms         0.024
_refine_ls_extinction_coef       0.00040(13)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0463P)^2^+1.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                1937
_reflns_number_total             3009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32545d.txt
_cod_data_source_block           cd211326
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7107866