Construction of Sulfonyl Oxabenzo[3.3.1]bicyclic Core via Cyclocondensation of β-Ketosulfones and o-Formyl Allylbenzenes.
Hsueh, Nai-Chen; Chen, Hsing-Yin; Chang, Meng-Yang; The Journal of organic chemistry 82 (2017) 13324–13332; doi:10.1021/acs.joc.7b02425

data_4033250
_publ_section_title
;
 Construction of Sulfonyl Oxabenzo[3.3.1]bicyclic Core via
 Cyclocondensation of \b-Ketosulfones and o-Formyl Allylbenzenes.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              13324
_journal_page_last               13332
_journal_paper_doi               10.1021/acs.joc.7b02425
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C33 H30 O5 S'
_chemical_formula_weight         538.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
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_atom_sites_solution_hydrogens   geom
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_cell_formula_units_Z            8
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_cell_length_c                   22.0291(15)
_cell_measurement_reflns_used    7971
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.6526
_cell_volume                     5596.1(6)
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_computing_publication_material  'Bruker SHELXTL'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_number            22506
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
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_exptl_crystal_description       Lump
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_refine_ls_number_reflns         5720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+4.4305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4962
_reflns_number_total             5720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02425_si_001.cif
_cod_data_source_block           170638LT_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4033244--4033250.cif.
;
_cod_database_code               4033250
_shelxl_version_number           2014/6
_shelx_res_checksum              85716
_shelx_hkl_checksum              75352