A new dehydrogenative [4 + 1] annulation between para-quinone methides (p-QMs) and iodonium ylides for the synthesis of 2,3-dihydrobenzofurans
Xiong, Yan-Jie; Shi, Shao-Qing; Hao, Wen-Juan; Tu, Shu-Jiang; Jiang, Bo; Organic Chemistry Frontiers 5 (2018) 3483–; doi:10.1039/C8QO00950C

data_1554472
_publ_section_title
;
 A new dehydrogenative [4 + 1] annulation between para-quinone methides
 (p-QMs) and iodonium ylides for the synthesis of 2,3-dihydrobenzofurans
;
_journal_issue                   23
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              3483
_journal_paper_doi               10.1039/C8QO00950C
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C27 H28 Cl I N2 O5'
_chemical_formula_weight         622.86
_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
;
2018-08-31 deposited with the CCDC.
2018-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                106.048(2)
_cell_angle_beta                 95.0100(10)
_cell_angle_gamma                114.103(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8050(8)
_cell_length_b                   11.7571(9)
_cell_length_c                   12.8689(11)
_cell_measurement_reflns_used    2308
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.611
_cell_measurement_theta_min      2.392
_cell_volume                     1396.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7091
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.8312
_exptl_absorpt_correction_T_min  0.6557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.805
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     333
_refine_ls_number_reflns         4841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.2193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                2934
_reflns_number_total             4841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qo00950c2.cif
_cod_data_source_block           180809b
_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        1396.26(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1554472