Synthesis of Polysubstituted Maleimides <i>via</i> Metal-Free Cascade Reaction of Isocyanides and α-Diazoketones.
Zhang, Xu; Cao, Wen-Bin; Li, Hai-Yan; Xu, Xiao-Ping; Ji, Shun-Jun; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02830

data_4037646
_publ_section_title
;
 Synthesis of Polysubstituted Maleimides <i>via</i> Metal-Free Cascade
 Reaction of Isocyanides and \a-Diazoketones.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02830
_journal_year                    2019
_chemical_formula_moiety         'C29 H26 N2 O3'
_chemical_formula_sum            'C29 H26 N2 O3'
_chemical_formula_weight         450.52
_space_group_crystal_system      monoclinic
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_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 97.0468(15)
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_cell_length_b                   7.93205(12)
_cell_length_c                   23.1683(4)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.9790
_cell_measurement_theta_min      3.8250
_cell_volume                     2350.18(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
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_diffrn_reflns_number            15766
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.385
_diffrn_reflns_theta_min         3.743
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93610
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
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_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1300P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4015
_reflns_number_total             4947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02830_si_002.cif
_cod_data_source_block           G190910A
_cod_original_cell_volume        2350.18(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4037646
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              75070
_shelx_hkl_checksum              63808