Synthesis of spiro[2,3-dihydrofuran-3,3′-oxindole] derivatives via a multi-component cascade reaction of α-diazo esters, water, isatins and malononitrile/ethyl cyanoacetate
Shi, Taoda; Teng, Shenghan; Wei, Yajie; Guo, Xin; Hu, Wenhao; Green Chemistry 21 (2019) 4936–; doi:10.1039/C9GC01751H

data_7233376
_publ_section_title
;
 Synthesis of spiro[2,3-dihydrofuran-3,3&#x2032;-oxindole] derivatives via
 a multi-component cascade reaction of \a-diazo esters, water, isatins and
 malononitrile/ethyl cyanoacetate
;
_journal_issue                   18
_journal_name_full               'Green Chemistry'
_journal_page_first              4936
_journal_paper_doi               10.1039/C9GC01751H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C15 H13 N3 O4'
_chemical_formula_weight         299.28
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-07-16 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.7660(14)
_cell_length_b                   19.7660(14)
_cell_length_c                   7.7429(6)
_cell_measurement_temperature    296(2)
_cell_volume                     3025.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            33852
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9657
_exptl_absorpt_correction_T_min  0.9546
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_platon_squeeze_details
;
;
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0467P)^2^+0.9894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                2412
_reflns_number_total             2673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9gc01751h2.cif
_cod_data_source_block           z_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7233375--7233376.cif.'
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7233376
_cod_duplicate_entry 7233375