Hydrazone Radical Promoted Vicinal Difunctionalization of Alkenes and Trifunctionalization of Allyls: Synthesis of Pyrazolines and Tetrahydropyridazines
Xiao-Yong Duan; Xiu-Long Yang; Ran Fang; Xie-Xue Peng; Wei Yu; Bing Han; Journal of Organic Chemistry 78 (2013) 10692–10704; doi:10.1021/jo4016908

data_4028702
_publ_section_title
;
 Hydrazone Radical Promoted Vicinal Difunctionalization of Alkenes and
 Trifunctionalization of Allyls: Synthesis of Pyrazolines and
 Tetrahydropyridazines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              10692
_journal_page_last               10704
_journal_paper_doi               10.1021/jo4016908
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C41 H59 N2 O2'
_chemical_formula_weight         611.90
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.950(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1683(2)
_cell_length_b                   29.6471(7)
_cell_length_c                   15.3480(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3622.24(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22286
_diffrn_reflns_theta_full        72.72
_diffrn_reflns_theta_max         72.72
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.517
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_F_000             1340
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0905P)^2^+0.7772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                6059
_reflns_number_total             7160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo4016908_si_004.cif
_cod_data_source_block           yangxl1213
_cod_database_code               4028702