New Reaction Products of Acetylacetone with Semicarbazide Derivatives
Glukhacheva, Vera S.; Il’yasov, Sergey G.; Kazantsev, Igor V.; Shestakova, Elena O.; Il’yasov, Dmitri S.; Eltsov, Ilia V.; Nefedov, Andrey A.; Gatilov, Yuri V.; ACS Omega 6 (2021) 8637–8645; doi:10.1021/acsomega.1c00518

data_4518569
_publ_section_title
;
 New Reaction Products of Acetylacetone with Semicarbazide Derivatives
;
_journal_issue                   12
_journal_name_full               'ACS Omega'
_journal_page_first              8637
_journal_page_last               8645
_journal_paper_doi               10.1021/acsomega.1c00518
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C12 H16 N6 O2'
_chemical_formula_sum            'C12 H16 N6 O2'
_chemical_formula_weight         276.31
_chemical_melting_point          418
_chemical_name_systematic
;
Bis(3,5-dimethylpyrazole-1-carbonyl)hydrazine + ethanol-toluene solvents
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 106.521(2)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   32.0854(18)
_cell_length_b                   16.6338(7)
_cell_length_c                   18.7396(11)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.33
_cell_volume                     9588.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35665
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.333
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.8768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       prism
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2211
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5329
_reflns_number_total             8467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c00518_si_001.cif
_cod_data_source_block           bijskg4_sq
_cod_depositor_comments          'Adding full bibliography for 4518569.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4518569
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              41176
_shelx_hkl_checksum              2187
_shelx_fab_checksum              51110