Carboxylative cyclization of substituted propenyl ketones using CO2: transition-metal-free synthesis of α-pyrones
Zhang, Wen-Zhen; Yang, Ming-Wang; Lu, Xiao-Bing; Green Chem. 18 (2016) 4181–; doi:10.1039/C6GC01346E

data_7225779
_publ_section_title
;
 Carboxylative cyclization of substituted propenyl ketones using CO2:
 transition-metal-free synthesis of \a-pyrones
;
_journal_issue                   15
_journal_name_full               'Green Chem.'
_journal_page_first              4181
_journal_paper_doi               10.1039/C6GC01346E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C17 H12 O2'
_chemical_formula_weight         248.27
_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_method           SHELXL-97
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.384(3)
_cell_angle_beta                 92.571(3)
_cell_angle_gamma                90.050(3)
_cell_formula_units_Z            4
_cell_length_a                   7.1649(11)
_cell_length_b                   7.1976(11)
_cell_length_c                   25.276(4)
_cell_measurement_reflns_used    3514
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.83
_cell_volume                     1301.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6307
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+1.0861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2510
_refine_ls_wR_factor_ref         0.2593
_reflns_number_gt                3035
_reflns_number_total             3610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6gc01346e2.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7225779.cif.
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7225779