Facile synthesis of 2-pyrazolines and alpha,beta-diamino ketones via regioselective ring-opening of hydrazone-tethered aziridines
Zhen Zhang; De Wang; Yin Wei; Min Shi; Chem.Commun. 48 (2012) 9607–; doi:10.1039/c2cc35135h

data_7108357
_publ_section_title
;
 Facile synthesis of 2-pyrazolines and alpha,beta-diamino ketones via
 regioselective ring-opening of hydrazone-tethered aziridines
;
_journal_name_full               Chem.Commun.
_journal_page_first              9607
_journal_paper_doi               10.1039/c2cc35135h
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C17 H17 Br N4 O4 S'
_chemical_formula_weight         453.32
_chemical_name_systematic
;
?
;
_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'
_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                 102.327(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   53.632(4)
_cell_length_b                   9.3905(6)
_cell_length_c                   16.7335(10)
_cell_measurement_reflns_used    4195
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.415
_cell_measurement_theta_min      4.795
_cell_volume                     8233.2(9)
_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
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14905
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         0.78
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12906
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       4195
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.147
_platon_squeeze_details
;
;
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         14905
_refine_ls_number_restraints     795
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                8759
_reflns_number_total             14905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35135h.txt
_cod_data_source_block           cd212307
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7108357