Organocatalyzed enantioselective mannich reaction of pyrazoleamides with isatin-derived ketimines.
Li, Tian-Ze; Wang, Xi-Bo; Sha, Feng; Wu, Xin-Yan; The Journal of organic chemistry 79 (2014) 4332–4339; doi:10.1021/jo500145w

data_4029428
_publ_section_title
;
 Organocatalyzed enantioselective mannich reaction of pyrazoleamides with
 isatin-derived ketimines.
;
_journal_issue                   10
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4332
_journal_page_last               4339
_journal_paper_doi               10.1021/jo500145w
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C25 H25 Br N4 O4'
_chemical_formula_weight         525.40
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 123.323(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   41.527(6)
_cell_length_b                   11.0922(17)
_cell_length_c                   26.113(4)
_cell_measurement_reflns_used    3089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.411
_cell_measurement_theta_min      4.556
_cell_volume                     10051(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
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_diffrn_reflns_limit_h_max       50
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29608
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         18522
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                9374
_reflns_number_total             18522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo500145w_si_001.cif
_cod_data_source_block           cd213317
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4029428.cif.
;
_cod_original_cell_volume        10051(2)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4029428