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_7108355
_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            'C24 H25 Br N4 O7 S2'
_chemical_formula_weight         625.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.0457(9)
_cell_length_b                   14.7223(15)
_cell_length_c                   36.520(4)
_cell_measurement_reflns_used    2281
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.289
_cell_measurement_theta_min      4.609
_cell_volume                     5938.8(10)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    0.1414
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            9942
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39276
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.101
_platon_squeeze_details
;
;
_refine_diff_density_max         2.652
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9942
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.1004
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2521
_reflns_number_gt                5209
_reflns_number_total             9942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35135h.txt
_cod_data_source_block           cd21255
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7108355