Cascade reaction of o-enoyl arylisocyanide and o-hydroxy aromatic aldimine: a diastereoselective access to polycyclic spirobenzoxazine chromeno[4,3-b]pyrrole derivative
Li, Jian; Xiao, Yao; Peng, Xin; Shen, Jie; Cui, Lei; Lu, Shanya; Jia, Xueshun; Li, Chunju; Chemical Communications  (2022) –; doi:10.1039/D2CC02454C

data_7130602
_publ_section_title
;
 Cascade reaction of o-enoyl arylisocyanide and o-hydroxy aromatic
 aldimine: a diastereoselective access to polycyclic spirobenzoxazine
 chromeno[4,3-b]pyrrole derivative
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02454C
_journal_year                    2022
_chemical_formula_sum            'C30 H27 Cl N2 O6'
_chemical_formula_weight         546.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc29gkcq
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.333(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1210(7)
_cell_length_b                   16.5576(10)
_cell_length_c                   14.9717(9)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      4.03
_cell_volume                     2693.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker APEX-II CCD'
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios MX Multilayer Optic'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19566
_diffrn_reflns_theta_full        66.72
_diffrn_reflns_theta_max         66.72
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_type              'Incoatec Ius 3.0'
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      block
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       clear
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.714
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4761
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+1.5023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4401
_reflns_number_total             4761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02454c2.cif
_cod_data_source_block           20210118c
_cod_database_code               7130602
_shelx_res_checksum              50165
_shelx_hkl_checksum              14237