Catalytic Annulation of Diethyl Methylenecyclopropane-1,1-dicarboxylate with 1,1-Dicyanoalkenes.
Suzuki, Itaru; Tsunoi, Shinji; Shibata, Ikuya; Organic letters 19 (2017) 2690–2693; doi:10.1021/acs.orglett.7b01023

data_1545903
_publ_section_title
;
 Catalytic Annulation of Diethyl Methylenecyclopropane-1,1-dicarboxylate
 with 1,1-Dicyanoalkenes.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2690
_journal_page_last               2693
_journal_paper_doi               10.1021/acs.orglett.7b01023
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C20 H19 Br N2 O4'
_chemical_formula_sum            'C20 H19 Br N2 O4'
_chemical_formula_weight         431.29
_space_group_IT_number           14
_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                 91.5907(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   28.3676(5)
_cell_length_b                   12.0527(2)
_cell_length_c                   11.4928(2)
_cell_measurement_reflns_used    18751
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.12
_cell_volume                     3927.94(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37652
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.093
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
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_refine_diff_density_max         0.926
_refine_diff_density_min         -0.698
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         3309
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0008Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                1733
_reflns_number_total             5834
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol7b01023_si_002.cif
_cod_data_source_block           t449-4
_cod_depositor_comments          'Adding full bibliography for 1545903.cif.'
_cod_original_cell_volume        3927.92(12)
_cod_database_code               1545903