Enantioselective aza-Micheal reaction of hydrazide to chalcones through the nonactivated amine moiety conjugated addition
Jun Jiang; Yunfei Cai; Weiliang Chen; Lili Lin; Xiaohua Liu; Xiaoming Feng; Chem.Commun. 47 (2011) 4016–; doi:10.1039/c0cc05804a

data_7106169
_publ_section_title
;
 Enantioselective aza-Micheal reaction of hydrazide to chalcones through
 the nonactivated amine moiety conjugated addition
;
_journal_name_full               Chem.Commun.
_journal_page_first              4016
_journal_paper_doi               10.1039/c0cc05804a
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H19 Cl N2 O2'
_chemical_formula_sum            'C22 H19 Cl N2 O2'
_chemical_formula_weight         378.84
_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                 105.291(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6570(9)
_cell_length_b                   5.2425(3)
_cell_length_c                   14.9418(10)
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.9651
_cell_measurement_theta_min      3.2564
_cell_volume                     956.35(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program.
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program.
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      294.0
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega -16.00 13.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -17.0486 -77.0000 -30.0000 29

2 omega 17.00 92.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 20.0174 38.0000 -150.0000 75

3 omega -53.00 52.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 20.0174 -27.0000 38.0000 105
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0134364
_diffrn_orient_matrix_UB_12      -0.0237866
_diffrn_orient_matrix_UB_13      -0.0484208
_diffrn_orient_matrix_UB_21      0.0544698
_diffrn_orient_matrix_UB_22      -0.0408583
_diffrn_orient_matrix_UB_23      0.0040331
_diffrn_orient_matrix_UB_31      -0.0150476
_diffrn_orient_matrix_UB_32      -0.1267862
_diffrn_orient_matrix_UB_33      0.0078078
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3884
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.98239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0511P)^2^+0.1425P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                2489
_reflns_number_total             3162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05804a.txt
_cod_data_source_block           101110_S1_JJ
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               7106169