Direct asymmetric organocatalytic Michael reactions of alpha,alpha-disubstituted aldehydes with beta-nitrostyrenes for the synthesis of quaternary carbon-containing products.
Mase, Nobuyuki; Thayumanavan, Rajeswari; Tanaka, Fujie; Barbas, 3rd, Carlos F; Organic letters 6 (2004) 2527–2530; doi:10.1021/ol049196o

data_1507075
_publ_section_title
;
 Direct asymmetric organocatalytic Michael reactions of
 alpha,alpha-disubstituted aldehydes with beta-nitrostyrenes for the
 synthesis of quaternary carbon-containing products.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              2527
_journal_page_last               2530
_journal_paper_doi               10.1021/ol049196o
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C19 H21 N5 O6'
_chemical_formula_weight         415.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.65(3)
_cell_angle_beta                 88.22(3)
_cell_angle_gamma                74.29(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2921(17)
_cell_length_b                   11.639(2)
_cell_length_c                   12.066(2)
_cell_measurement_reflns_used    1689
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.6
_cell_volume                     1008.2(5)
_computing_cell_refinement       'Bruker SAINT+'
_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, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7293
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_correction_T_min  0.9714
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.28
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_exptl_crystal_size_min          0.17
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_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.2328
_reflns_number_gt                1578
_reflns_number_total             3525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol049196osi20040430_072712.cif
_cod_data_source_block           mn582
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1008.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507075