Enantioselective Michael reactions of beta, beta-disubstituted nitroalkenes: a new approach to beta(2,2)-amino acids with hetero-quaternary stereocenters.
Lu, Hai-Hua; Zhang, Fu-Gen; Meng, Xiang-Gao; Duan, Shu-Wen; Xiao, Wen-Jing; Organic letters 11 (2009) 3946–3949; doi:10.1021/ol901572x

data_1504120
_publ_section_title
;
 Enantioselective Michael reactions of beta, beta-disubstituted
 nitroalkenes: a new approach to beta(2,2)-amino acids with
 hetero-quaternary stereocenters.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              3946
_journal_page_last               3949
_journal_paper_doi               10.1021/ol901572x
_journal_volume                  11
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H23 N O4 S'
_chemical_formula_sum            'C27 H23 N O4 S'
_chemical_formula_weight         457.52
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.412(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7746(9)
_cell_length_b                   5.8697(4)
_cell_length_c                   16.0370(11)
_cell_measurement_reflns_used    4081
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.30
_cell_volume                     1174.40(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'SMART, Bruker Version 5.628, 2001'
_computing_data_reduction        'SAINT+, Bruker Version 6.45, 2001'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART Apex CCD area-detector'
_diffrn_measurement_method       '0.3\% wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12746
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9681
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4769
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                4037
_reflns_number_total             4769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901572x_si_001.cif
_cod_data_source_block           090216dm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1504120