3-Methoxalylchromones - versatile reagents for the regioselective synthesis of functionalized 2,4'-dihydroxybenzophenones, potential UV-filters.
Iaroshenko, Viktor O.; Bunescu, Alina; Spannenberg, Anke; Supe, Linda; Milyutina, Maria; Langer, Peter; Organic & biomolecular chemistry 9 (2011) 7554–7558; doi:10.1039/c1ob05931a

data_7152039
_publ_section_title
;
 3-Methoxalylchromones - versatile reagents for the regioselective
 synthesis of functionalized 2,4'-dihydroxybenzophenones, potential
 UV-filters.
;
_journal_issue                   21
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7554
_journal_page_last               7558
_journal_paper_doi               10.1039/c1ob05931a
_journal_volume                  9
_journal_year                    2011
_chemical_formula_sum            'C17 H16 Cl2 O6'
_chemical_formula_weight         387.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.241(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.4384(10)
_cell_length_b                   5.6289(2)
_cell_length_c                   22.7063(8)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      1.90
_cell_volume                     3246.0(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25744
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.9389
_exptl_absorpt_correction_T_min  0.7898
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                3228
_reflns_number_total             3889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ob05931a.txt
_cod_data_source_block           ks1140
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7152039