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_4035854
_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_absolute_configuration unk
_chemical_formula_sum            'C41.25 H37.5 N2.5 O5 Si1.25'
_chemical_formula_weight         683.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2015-12-10T19:37:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.896(2)
_cell_length_b                   12.3718(16)
_cell_length_c                   26.501(3)
_cell_measurement_reflns_used    7305
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.0517
_cell_volume                     3244.6(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
        ????
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
        Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.1007
_diffrn_orient_matrix_UB_12      -0.0021
_diffrn_orient_matrix_UB_13      -0.0087
_diffrn_orient_matrix_UB_21      0.0036
_diffrn_orient_matrix_UB_22      -0.0772
_diffrn_orient_matrix_UB_23      -0.0237
_diffrn_orient_matrix_UB_31      -0.0029
_diffrn_orient_matrix_UB_32      -0.0112
_diffrn_orient_matrix_UB_33      0.0359
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29352
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         3.052
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5864
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1421 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.07(12)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0765
_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^)+(0.1404P)^2^+1.6401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2297
_reflns_number_gt                5004
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00890_si_003.cif
_cod_data_source_block           151209
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C41.25 H37.50 N2.50 O5 Si1.25'
_cod_database_code               4035854