Intramolecular [2 + 2] and [4 + 2] Cycloaddition Reactions of Cinnamylamides of Ethenetricarboxylate in Sequential Processes.
Yamazaki, Shoko; Sugiura, Hirotaka; Ohashi, Shinnosuke; Ishizuka, Keisuke; Saimu, Rina; Mikata, Yuji; Ogawa, Akiya; The Journal of organic chemistry 81 (2016) 10863–10886; doi:10.1021/acs.joc.6b01947

data_4037302
_publ_section_title
;
 Intramolecular [2 + 2] and [4 + 2] Cycloaddition Reactions of
 Cinnamylamides of Ethenetricarboxylate in Sequential Processes.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10863
_journal_page_last               10886
_journal_paper_doi               10.1021/acs.joc.6b01947
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C31 H37 N5 O8'
_chemical_formula_sum            'C31 H37 N5 O8'
_chemical_formula_weight         607.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                76.989(6)
_cell_angle_beta                 62.670(4)
_cell_angle_gamma                72.283(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5911(12)
_cell_length_b                   12.1293(15)
_cell_length_c                   12.5797(13)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.13
_cell_volume                     1489.0(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11656
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             644.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.2209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                5685
_reflns_number_total             6497
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo6b01947_si_004.cif
_cod_data_source_block           301X-1-160304
_cod_database_code               4037302