Crystal structure and Hirshfeld surface analysis of 2,5-di-imino-8a-methyl-4,9-bis-(4-methyl-phen-yl)-7-oxo-6-phenyl-deca-hydro-2<i>H</i>-3,8-methano-pyrano[3,2-<i>c</i>]pyridine-3,4a-dicarbo-nitrile <i>N</i>,<i>N</i>-di-methyl-formamide monosolvate.
Naghiyev, Farid N.; Khrustalev, Victor N.; Novikov, Anton P.; Akkurt, Mehmet; Khalilov, Ali N.; Bhattarai, Ajaya; Mamedov, İbrahim G; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 254–258; doi:10.1107/S2056989023001718

data_2022699
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 2,5-di-imino-8a-methyl-4,9-bis-(4-methyl-phen-yl)-7-oxo-6-phenyl-deca-hydro-2<i>H</i>-3,8-methano-pyrano[3,2-<i>c</i>]pyridine-3,4a-dicarbo-nitrile
 <i>N</i>,<i>N</i>-di-methyl-formamide monosolvate.
;
_journal_coeditor_code           WM5672
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              254
_journal_page_last               258
_journal_paper_doi               10.1107/S2056989023001718
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C32 H27 N5 O2, C3 H7 N O'
_chemical_formula_moiety         'C32 H27 N5 O2, C3 H7 N O'
_chemical_formula_sum            'C35 H34 N6 O3'
_chemical_formula_weight         586.68
_chemical_name_common
;2,5-Diimino-8a-methyl-4,9-bis(4-methylphenyl)-7-oxo-6-phenyl-decahydro-2<i>H</i>-3,8-methanopyrano[3,2-<i>c</i>]pyridine-3,4a-dicarbonitrile
<i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_chemical_name_systematic
;4,10-Diimino-8-methyl-2,11-bis(4-methylphenyl)-6-oxo-5-phenyl-9-oxa-5-azatricyclo[5.3.1.0^3,8^]undecane-1,3-dicarbonitrile
<i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.666(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6747(3)
_cell_length_b                   15.7656(2)
_cell_length_c                   10.9086(2)
_cell_measurement_reflns_used    19771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.0
_cell_measurement_theta_min      3.8
_cell_volume                     2926.79(9)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31226
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.491
_diffrn_reflns_theta_min         3.822
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0745P)^2^+3.3477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                5275
_reflns_number_total             6140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5672sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022699.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022699
_cod_database_fobs_code          2022699
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              31524
_shelx_res_checksum              91053