One-pot cascade Michael‒Michael‒Aldol condensation for diastereoselective synthesis of nitro-substituted cyclohexanes
Yunfeng Chen; Cheng Zhong; Xiaohua Sun; Novruz G. Akhmedov; Jeffrey L. Petersen; Xiaodong Shi; Chem. Commun. 34 (2009) 5150–5152; doi:10.1039/b909766j

data_7104691
_publ_section_title
;
 One-pot cascade Michael--Michael--Aldol condensation for
 diastereoselective synthesis of nitro-substituted cyclohexanes
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              5150
_journal_page_last               5152
_journal_paper_doi               10.1039/b909766j
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C25 H27 N O4'
_chemical_formula_weight         405.48
_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                84.2340(10)
_cell_angle_beta                 75.4250(10)
_cell_angle_gamma                72.6650(10)
_cell_formula_units_Z            4
_cell_length_a                   9.6784(6)
_cell_length_b                   14.8547(10)
_cell_length_c                   16.1677(11)
_cell_measurement_reflns_used    7308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.26
_cell_volume                     2146.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15150
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9495
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+0.2843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                6743
_reflns_number_total             9495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909766j.txt
_cod_data_source_block           ms93ccd
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104691