Novel [2 + 2 + 2] Annulation of 1,6-Diynes Mediated by Methallylchromate or Methallylmagnesium Chloride under CrCl3 Catalysis
Toshihiro Nishikawa; Hirotada Kakiya; Hiroshi Shinokubo; Koichiro Oshima; Journal of the American Chemical Society 123 (2001) 4629–4630; doi:10.1021/ja015746r

data_4115550
_publ_contact_author
; 
 Prof Koichiro Oshima 
 Department of Material Chemistry 
 Graduate School of Engineering 
 Kyoto University 
 Kyoto 606-8501 
 Japan 
;
_publ_contact_author_email       oshima@fm1.kuic.kyoto-u.ac.jp
_publ_section_title
;
 Novel [2 + 2 + 2] Annulation of 1,6-Diynes Mediated by Methallylchromate
 or Methallylmagnesium Chloride under CrCl3 Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4629
_journal_page_last               4630
_journal_paper_doi               10.1021/ja015746r
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         'C21 H31 N O4'
_chemical_formula_sum            'C21 H31 N O4'
_chemical_formula_weight         361.47
_chemical_melting_point          453
_chemical_name_systematic
; 
 8,8-Di(methoxymethyl)-2,5,10,10-tetramethyltricyclo[4.3.2.0]undeca-1(6)-ene
-3,4-dicarboximide 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.300(3)
_cell_angle_beta                 68.293(3)
_cell_angle_gamma                71.564(3)
_cell_formula_units_Z            2
_cell_length_a                   8.774(2)
_cell_length_b                   11.073(3)
_cell_length_c                   11.469(3)
_cell_measurement_temperature    293(2)
_cell_volume                     959.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5294
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.2532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                3010
_reflns_number_total             3474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja015746r_s3.cif
_cod_data_source_block           shino1
_cod_database_code               4115550