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_4021744
_publ_contact_author             'Olga Kazheva'
_publ_contact_author_email       koh@icp.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           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-11-07T17:13:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.24(1)
_cell_angle_beta                 99.95(2)
_cell_angle_gamma                96.12(2)
_cell_formula_units_Z            2
_cell_length_a                   7.912(2)
_cell_length_b                   9.4920(10)
_cell_length_c                   12.597(2)
_cell_measurement_temperature    293(2)
_cell_volume                     900.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3339
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_refine_diff_density_max         0.226
_refine_diff_density_min         0.174
_refine_diff_density_rms         0.027
_refine_ls_extinction_coef       0.013(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   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.1598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2706
_reflns_number_total             3094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060459xsi20060303_121703.cif
_cod_database_code               4021744