Crystal structure and Hirshfeld surface analysis of dimethyl 3-methyl-8-{[4-(trifluoromethyl)phenyl]sulfonyl}-7,8-dihydro-4H-4,6a-epoxybenzo[b]naphtho[1,8-de]azepine-5,6-dicarboxylate
Burkin, Gleb M.; Annadurdyyeva, Selbi; Kutasevich, Alexandra G.; Guliyeva, Narmina A.; Hasanov, Khudayar I.; Akkurt, Mehmet; Manahelohe, Gizachew Mulugeta; Acta Crystallographica Section E Crystallographic Communications 81 (2025) –; doi:10.1107/S2056989025004426

data_2023516
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of dimethyl
 3-methyl-8-{[4-(trifluoromethyl)phenyl]sulfonyl}-7,8-dihydro-4H-4,6a-epoxybenzo[b]naphtho[1,8-de]azepine-5,6-dicarboxylate
;
_journal_coeditor_code           NX2026
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989025004426
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C29 H22 F3 N O7 S'
_chemical_formula_moiety         'C29 H22 F3 N O7 S'
_chemical_formula_sum            'C29 H22 F3 N O7 S'
_chemical_formula_weight         585.53
_chemical_name_systematic
;Dimethyl
3-methyl-8-{[4-(trifluoromethyl)phenyl]sulfonyl}-7,8-dihydro-4<i>H</i>-4,6a-epoxybenzo[<i>b</i>]naphtho[1,8-<i>de</i>]azepine-5,6-dicarboxylate
;
_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   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 93.9830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6375(5)
_cell_length_b                   11.0324(6)
_cell_length_c                   30.2019(8)
_cell_measurement_reflns_used    20964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.92
_cell_measurement_theta_min      2.93
_cell_volume                     2538.7(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b
;
_computing_structure_solution
;
<i>SHELXT2016/6</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy-S, HyPix-6000HE area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            31570
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.131
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.430
_refine_ls_extinction_coef       0.00089(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.8141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                5187
_reflns_number_total             5526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2026.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023516
_shelx_estimated_absorpt_t_min   0.572
_shelx_estimated_absorpt_t_max   0.750
_shelx_hkl_checksum              40084
_shelx_res_checksum              59800