Generation of 1,3-Dimethylene-Substituted Isobenzofurans via Pd(II)-Catalyzed Selective Oxo-cyclization/SO<sub>2</sub> Insertion Cascade of β-Alkynyl Ketones.
Liu, Shuai; Chen, Ke; Hao, Wen-Juan; Tu, Xing-Chao; Tu, Shu-Jiang; Jiang, Bo; The Journal of organic chemistry 84 (2019) 1964–1971; doi:10.1021/acs.joc.8b02934

data_4033789
_publ_section_title
;
 Generation of 1,3-Dimethylene-Substituted Isobenzofurans via
 Pd(II)-Catalyzed Selective Oxo-cyclization/SO<sub>2</sub> Insertion
 Cascade of \b-Alkynyl Ketones.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1964
_journal_page_last               1971
_journal_paper_doi               10.1021/acs.joc.8b02934
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C28 H17 Br3 O3 S'
_chemical_formula_weight         673.21
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.289(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.149(2)
_cell_length_b                   5.7598(5)
_cell_length_c                   23.403(2)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.084
_cell_measurement_theta_min      2.612
_cell_volume                     2762.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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
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_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
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_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11726
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  0.8069
_exptl_absorpt_correction_T_min  0.4003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.25
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_refine_diff_density_max         1.821
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_refine_ls_extinction_method     none
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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^)+(0.1397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2933
_refine_ls_wR_factor_ref         0.3371
_reflns_number_gt                2009
_reflns_number_total             4830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b02934_si_002.cif
_cod_data_source_block           170518a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/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      P2(1)/n
_cod_database_code               4033789