Synthesis of spiro[isoquinolinone-4,2'-oxiranes] and isoindolinones via a multicomponent reaction of 2-acetyl-oxirane-2-carboxamides, arylaldehydes and malononitrile
Bing Liu; Enxiang Wei; Shaoxia Lin; Baozhong Zhao; Fushun Liang; Chem.Commun. 50 (2014) 6995–; doi:10.1039/C4CC02141J

data_7114583
_publ_section_title
;
 Synthesis of spiro[isoquinolinone-4,2'-oxiranes] and isoindolinones via a
 multicomponent reaction of 2-acetyl-oxirane-2-carboxamides, arylaldehydes
 and malononitrile
;
_journal_name_full               Chem.Commun.
_journal_page_first              6995
_journal_paper_doi               10.1039/C4CC02141J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C22.50 H23 Cl Fe2 N O5 P Se2'
_chemical_formula_sum            'C22.5 H23 Cl Fe2 N O5 P Se2'
_chemical_formula_weight         723.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                92.552(14)
_cell_angle_beta                 103.678(17)
_cell_angle_gamma                91.248(8)
_cell_formula_units_Z            2
_cell_length_a                   9.6040(16)
_cell_length_b                   10.4610(17)
_cell_length_c                   13.6300(19)
_cell_measurement_reflns_used    4938
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.90
_cell_volume                     1328.5(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    4.026
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.7942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.986
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5074
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                4258
_reflns_number_total             5074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02141j2.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C22.50 H23 Cl Fe2 N O5 P Se2'
_cod_database_code               7114583