Organocatalytic (5+1) benzannulation of Morita–Baylis–Hillman carbonates: synthesis of multisubstituted 4-benzylidene pyrazolones
He, Shurong; Wang, Jie; Zheng, Jinfeng; Luo, Qing-Qing; Leng, Haijun; Zheng, Sixiang; Peng, Cheng; Han, Bo; Zhan, Gu; New Journal of Chemistry 46 (2022) 11617–11622; doi:10.1039/D2NJ01949C

data_7061509
_publ_section_title
;
 Organocatalytic (5+1) benzannulation of Morita--Baylis--Hillman
 carbonates: synthesis of multisubstituted 4-benzylidene pyrazolones
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11617
_journal_page_last               11622
_journal_paper_doi               10.1039/D2NJ01949C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C40 H25.2 N4 O6'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-02-20 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   16.0726(6)
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_cell_measurement_temperature    285(2)
_cell_measurement_theta_max      66.38
_cell_measurement_theta_min      4.32
_cell_volume                     3434.5(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      285(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.422
_diffrn_reflns_theta_min         3.754
_exptl_absorpt_coefficient_mu    0.714
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
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_refine_diff_density_max         0.399
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0059(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1077P)^2^+0.9218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4556
_reflns_number_total             6280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01949c2.cif
_cod_data_source_block           20211228HB_0m_a
_cod_depositor_comments
'Adding full bibliography for 7061508--7061509.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C40 H25.20 N4 O6'
_cod_database_code               7061509
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              57784