Sequential carboxylation/intramolecular cyclization reaction of o-alkynyl acetophenone with CO2
Zhang, Wen-Zhen; Shi, Ling-Long; Liu, Chuang; Yang, Xu-Tong; Wang, Yan-Bo; Luo, Yi; Lu, Xiao-Bing; Organic Chemistry Frontiers 1 (2014) 275–; doi:10.1039/c3qo00047h

data_1552964
_publ_section_title
;
 Sequential carboxylation/intramolecular cyclization reaction of o-alkynyl
 acetophenone with CO2
;
_journal_issue                   3
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              275
_journal_paper_doi               10.1039/c3qo00047h
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C21 H20 O3'
_chemical_formula_weight         320.37
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 96.853(8)
_cell_angle_gamma                99.139(9)
_cell_formula_units_Z            4
_cell_length_a                   11.2047(16)
_cell_length_b                   12.2098(18)
_cell_length_c                   13.3534(17)
_cell_measurement_temperature    296(2)
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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
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_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_theta_max         25.00
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_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9766
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.30
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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^)+(0.1298P)^2^+0.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2170
_reflns_number_gt                4601
_reflns_number_total             6234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qo00047h2.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_sg_symbol_H-M      'P-1   '
_cod_database_code               1552964