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_7061508
_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            'C29 H24 N4 O5'
_chemical_formula_weight         508.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                87.333(2)
_cell_angle_beta                 85.052(2)
_cell_angle_gamma                86.919(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1555(3)
_cell_length_b                   9.7802(3)
_cell_length_c                   15.0579(5)
_cell_measurement_reflns_used    5430
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      61.89
_cell_measurement_theta_min      2.95
_cell_volume                     1340.17(7)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.958
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24770
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.256
_diffrn_reflns_theta_min         2.948
_exptl_absorpt_coefficient_mu    0.722
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0095(6)
_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   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0457P)^2^+0.3818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2467
_reflns_number_total             4703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01949c2.cif
_cod_data_source_block           20210607HSR_0m_a
_cod_depositor_comments
'Adding full bibliography for 7061508--7061509.cif.'
_cod_original_cell_volume        1340.17(8)
_cod_database_code               7061508
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              69996