Double carboxylation of o-alkynyl acetophenone with carbon dioxide
Zhang, Wen-Zhen; Yang, Ming-Wang; Yang, Xu-Tong; Shi, Ling-Long; Wang, Hui-Bo; Lu, Xiao-Bing; Organic Chemistry Frontiers 3 (2016) 217–; doi:10.1039/C5QO00374A

data_1553217
_publ_section_title
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 Double carboxylation of o-alkynyl acetophenone with carbon dioxide
;
_journal_issue                   2
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              217
_journal_paper_doi               10.1039/C5QO00374A
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C20 H16 O5'
_chemical_formula_weight         336.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
;
2015-06-15 deposited with the CCDC.
2015-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                107.811(3)
_cell_angle_beta                 95.510(3)
_cell_angle_gamma                91.238(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1154(3)
_cell_length_b                   11.1585(5)
_cell_length_c                   11.1645(5)
_cell_measurement_temperature    296(2)
_cell_volume                     838.83(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7163
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9811
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.253
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2955
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_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0621
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                2328
_reflns_number_total             2955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qo00374a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        838.83(6)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               1553217