Construction of bis-, tris- and tetrahydrazones by addition of azoalkenes to amines and ammonia
Semakin, Artem N.; Kokuev, Aleksandr O.; Nelyubina, Yulia V.; Sukhorukov, Alexey Yu; Zhmurov, Petr A.; Ioffe, Sema L.; Tartakovsky, Vladimir A.; Beilstein Journal of Organic Chemistry 12 (2016) 2471–; doi:10.3762/bjoc.12.241

data_4032067
_publ_section_title
;
 Construction of bis-, tris- and tetrahydrazones by addition of azoalkenes
 to amines and ammonia
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              2471
_journal_paper_doi               10.3762/bjoc.12.241
_journal_volume                  12
_journal_year                    2016
_chemical_formula_sum            'C18.5 H37 N7 O7.5'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.398(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.325(2)
_cell_length_b                   12.234(2)
_cell_length_c                   29.447(5)
_cell_measurement_temperature    100(2)
_cell_volume                     5040.3(14)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2198
_diffrn_reflns_av_unetI/netI     0.1794
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            61716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.750
_exptl_absorpt_coefficient_mu    0.098
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_F_000             2056
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0040(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         13409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.2222
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5215
_reflns_number_total             13409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-12-241-S2.cif
_cod_data_source_block           a
_cod_original_cell_volume        5040.2(15)
_cod_original_formula_sum        'C18.50 H37 N7 O7.50'
_cod_database_code               4032067
_shelxl_version_number           2014/6
_shelx_res_checksum              9368
_shelx_hkl_checksum              49312