Construction of Bridged and Fused Ring Systems via Intramolecular Michael Reactions of Vinylnitroso Compounds
Ilia Korboukh; Praveen Kumar; Steven M. Weinreb; Journal of the American Chemical Society 129 (2007) 10342–10343; doi:10.1021/ja074108r

data_4109829
_publ_section_title
;
 Construction of Bridged and Fused Ring Systems via Intramolecular Michael
 Reactions of Vinylnitroso Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10342
_journal_page_last               10343
_journal_paper_doi               10.1021/ja074108r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C14 H22 N O5'
_chemical_formula_sum            'C14 H22 N O5'
_chemical_formula_weight         284.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.615(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.467(3)
_cell_length_b                   15.301(4)
_cell_length_c                   14.892(4)
_cell_measurement_reflns_used    7040
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.324
_cell_measurement_theta_min      2.501
_cell_volume                     2840.6(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21513
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       brick
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+4.3194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                4723
_reflns_number_total             6959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074108rsi20070530_013526.cif
_cod_data_source_block           ixk1s
_cod_original_cell_volume        2840.6(12)
_cod_database_code               4109829