Fe-Catalyzed Olefin Hydroamination with Diazo Compounds for Hydrazone Synthesis.
Zheng, Jing; Qi, Jifeng; Cui, Sunliang; Organic letters 18 (2016) 128–131; doi:10.1021/acs.orglett.5b03317

data_1542387
_publ_section_title
;
 Fe-Catalyzed Olefin Hydroamination with Diazo Compounds for Hydrazone
 Synthesis.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              128
_journal_page_last               131
_journal_paper_doi               10.1021/acs.orglett.5b03317
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C10 H16 N4 O5'
_chemical_formula_weight         272.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   14.614(3)
_cell_length_b                   12.706(3)
_cell_length_c                   13.842(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2570.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8450
_diffrn_reflns_theta_full        20.15
_diffrn_reflns_theta_max         20.15
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.114
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1602P)^2^+2.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                941
_reflns_number_total             1227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b03317_si_002.cif
_cod_data_source_block           d
_cod_original_cell_volume        2570.4(9)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               1542387