Further Studies of Intramolecular Michael Reactions of Nitrosoalkenes for Construction of Functionalized Bridged Ring Systems
Praveen Kumar; Puhui Li; Ilia Korboukh; Tony L. Wang; Hemant Yennawar; Steven M. Weinreb; Journal of Organic Chemistry 76 (2011) 2094–2101; doi:10.1021/jo1024392

data_4026160
_publ_section_title
;
 Further Studies of Intramolecular Michael Reactions of Nitrosoalkenes for
 Construction of Functionalized Bridged Ring Systems
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2094
_journal_page_last               2101
_journal_paper_doi               10.1021/jo1024392
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C22 H23 N O7 S2'
_chemical_formula_sum            'C22 H23 N O7 S2'
_chemical_formula_weight         477.53
_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                 111.923(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1596(17)
_cell_length_b                   25.648(5)
_cell_length_c                   10.427(2)
_cell_measurement_reflns_used    6605
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.504
_cell_measurement_theta_min      2.250
_cell_volume                     2272.4(8)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17699
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.3641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                4340
_reflns_number_total             5617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1024392_si_001.cif
_cod_data_source_block           pxk1s
_cod_original_cell_volume        2272.5(7)
_cod_database_code               4026160