Stereoselective Synthesis of 1-Nitrobicyclo[3.1.0]hexanes and Fused Isoxazoline-N-oxides from Primary Nitro Compounds
Akio Kamimura; Ryota Takeuchi; Kosuke Ikeda; Takaaki Moriyama; Michinori Sumimoto; Journal of Organic Chemistry 77 (2012) 2236–2245; doi:10.1021/jo202489v

data_4027023
_publ_contact_author_email       uno@dpc.ehime-u.ac.jp
_publ_contact_author_fax         +81-89-927-9610
_publ_contact_author_name        'Prof Hidemitsu Uno'
_publ_contact_author_phone       +81-89-927-9610
_publ_section_title
;
 Stereoselective Synthesis of 1-Nitrobicyclo[3.1.0]hexanes and Fused
 Isoxazoline-N-oxides from Primary Nitro Compounds
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2236
_journal_page_last               2245
_journal_paper_doi               10.1021/jo202489v
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C13 H19 Ag N O6'
_chemical_formula_weight         393.16
_chemical_name_systematic
; 
 ? 
;
_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                78.30(3)
_cell_angle_beta                 79.01(3)
_cell_angle_gamma                61.71(3)
_cell_formula_units_Z            4
_cell_length_a                   10.888(2)
_cell_length_b                   11.294(2)
_cell_length_c                   15.876(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1673.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16172
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.228
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             796
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          2.995
_refine_ls_shift/su_mean         0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+1.3839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2130
_reflns_number_gt                4832
_reflns_number_total             7568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo202489v_si_006.cif
_cod_data_source_block           090129
_cod_original_cell_volume        1673.3(6)
_cod_database_code               4027023