A co-crystal of heterobicyclic isomers as a product of the cyclocondensation reaction of 3,4-diaminofurazan with diethyl-2-oxosuccinate
Romanenko, Galina V.; Fokin, Sergey V.; Tolstikov, Svyatoslav E.; Letyagin, Gleb A.; Ovcharenko, Victor I.; Strizhenko, Kirill V.; Sheremetev, Aleksei B.; CrystEngComm 25 (2023) 5413–5419; doi:10.1039/D3CE00769C

data_7247374
_publ_section_title
;
 A co-crystal of heterobicyclic isomers as a product of the
 cyclocondensation reaction of 3,4-diaminofurazan with
 diethyl-2-oxosuccinate
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5413
_journal_page_last               5419
_journal_paper_doi               10.1039/D3CE00769C
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C8 H8 N4 O4'
_chemical_formula_weight         224.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-02 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                96.563(6)
_cell_angle_beta                 102.071(6)
_cell_angle_gamma                108.791(5)
_cell_formula_units_Z            2
_cell_length_a                   7.0461(7)
_cell_length_b                   7.5519(6)
_cell_length_c                   9.8725(9)
_cell_measurement_reflns_used    3105
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.64
_cell_measurement_theta_min      4.67
_cell_volume                     476.88(8)
_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 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5681
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.751
_diffrn_reflns_theta_min         4.671
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow_lemon
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0051(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.1164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1520
_reflns_number_total             1696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00769c2.cif
_cod_data_source_block           777a
_cod_depositor_comments
'Adding full bibliography for 7247374--7247376.cif.'
_cod_database_code               7247374
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              60368