Ruthenium-Porphyrin-Catalyzed [4 + 2] Cycloaddition of α,β-Unsaturated Imines and Aldehydes.
Maeda, Kazuki; Terada, Takuma; Iwamoto, Takahiro; Kurahashi, Takuya; Matsubara, Seijiro; Organic letters 17 (2015) 5284–5287; doi:10.1021/acs.orglett.5b02654

data_1555362
_publ_section_title
;
 Ruthenium-Porphyrin-Catalyzed [4 + 2] Cycloaddition of \a,\b-Unsaturated
 Imines and Aldehydes.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5284
_journal_page_last               5287
_journal_paper_doi               10.1021/acs.orglett.5b02654
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C22 H24 N2 O4 S'
_chemical_formula_sum            'C22 H24 N2 O4 S'
_chemical_formula_weight         412.50
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.075(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.928(4)
_cell_length_b                   11.573(3)
_cell_length_c                   11.950(3)
_cell_measurement_reflns_used    15731
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.10
_cell_volume                     2105.7(9)
_computing_cell_refinement       'CrystalClear-SM Auto 2.0 r15'
_computing_data_collection       'CrystalClear-SM Auto 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Auto 2.0 r15'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19490
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4823
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                3640
_reflns_number_total             4823
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol5b02654_si_004.cif
_cod_data_source_block           2015_03_19_1_B
_cod_original_cell_volume        2105.7(10)
_cod_database_code               1555362