Cascade Multiple Diels-Alder Reactions of Styrene Derivatives with Maleimide or Maleic Anhydride.
Yoshioka, Shohei; Aoyama, Hiroshi; Fujioka, Hiromichi; Arisawa, Mitsuhiro; The Journal of organic chemistry 83 (2018) 6599–6606; doi:10.1021/acs.joc.8b00890

data_4035855
_publ_section_title
;
 Cascade Multiple Diels-Alder Reactions of Styrene Derivatives with
 Maleimide or Maleic Anhydride.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6599
_journal_page_last               6606
_journal_paper_doi               10.1021/acs.joc.8b00890
_journal_volume                  83
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H40 Cl3 N3 O7 Si1'
_chemical_formula_sum            'C45 H40 Cl3 N3 O7 Si'
_chemical_formula_weight         869.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-31T18:15:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.626(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.513(4)
_cell_length_b                   13.967(4)
_cell_length_c                   20.430(6)
_cell_measurement_reflns_used    7776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.0843
_cell_measurement_wavelength     0.71073
_cell_volume                     4121(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_UB_11      -0.0084
_diffrn_orient_matrix_UB_12      -0.0475
_diffrn_orient_matrix_UB_13      -0.0497
_diffrn_orient_matrix_UB_21      0.071
_diffrn_orient_matrix_UB_22      -0.0074
_diffrn_orient_matrix_UB_23      -0.0049
_diffrn_orient_matrix_UB_31      -0.0019
_diffrn_orient_matrix_UB_32      -0.0386
_diffrn_orient_matrix_UB_33      0.0305
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36432
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         3.176
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.6
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1913P)^2^+2.8176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2916
_refine_ls_wR_factor_ref         0.3349
_reflns_number_gt                6294
_reflns_number_total             9411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00890_si_002.cif
_cod_data_source_block           hhh
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4035855