Reaction of Polyhaloalkyl-Substituted Chromones, Pyrones, and Furanones with Salicylaldehydes as a Direct Route to Fused 2H-Chromenes
Vyacheslav Ya. Sosnovskikh; Vladislav Yu. Korotaev; Dmitry L. Chizhov; Igor B. Kutyashev; Danil S. Yachevskii; Olga N. Kazheva; Oleg A. Dyachenko; Valery N. Charushin; Journal of Organic Chemistry 71 (2006) 4538–4543; doi:10.1021/jo060459x

data_4021745
_publ_contact_author             'Olga Kazheva'
_publ_contact_author_email       koh@ipc.ac.ru
_publ_section_title
;
 Reaction of Polyhaloalkyl-Substituted Chromones, Pyrones,
 and Furanones with Salicylaldehydes as a Direct Route
 to Fused 2H-Chromenes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4538
_journal_page_last               4543
_journal_paper_doi               10.1021/jo060459x
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C21 H10 F6 O4'
_chemical_formula_weight         440.29
_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_date             2005-11-07T17:13:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.37(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.053(2)
_cell_length_b                   12.222(2)
_cell_length_c                   13.902(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1862.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3392
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_refine_diff_density_max         0.13
_refine_diff_density_min         0.163
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0010(7)
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.1864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                2545
_reflns_number_total             3217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060459xsi20060303_121732.cif
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4021745