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_7108356
_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_formula_sum            'C17 H17 Br N4 O4 S'
_chemical_formula_weight         453.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.425(2)
_cell_angle_beta                 95.329(2)
_cell_angle_gamma                106.406(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5819(7)
_cell_length_b                   9.2830(9)
_cell_length_c                   13.8365(14)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.407
_cell_measurement_theta_min      4.611
_cell_volume                     922.70(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6041
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1934
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisamatic
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0590
_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^)+(0.0669P)^2^+0.4855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                3208
_reflns_number_total             4011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35135h.txt
_cod_data_source_block           cd21283
_cod_original_cell_volume        922.70(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108356