Crystal structure and Hirshfeld surface analysis of 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic acid dimethyl sulfoxide-d 6 monosolvate
Mammadova, Gunay Z.; Yakovleva, Elizaveta D.; Erokhin, Pavel P.; Grigoriev, Mikhail S.; Atioğlu, Zeliha; Azizova, Asmet N.; Akkurt, Mehmet; Bhattarai, Ajaya; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 1127–1131; doi:10.1107/S2056989023009635

data_2022937
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic
 acid dimethyl sulfoxide-d 6 monosolvate
;
_journal_coeditor_code           TX2077
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1127
_journal_page_last               1131
_journal_paper_doi               10.1107/S2056989023009635
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C22 H19 N O5 S, C2 D6 O S'
_chemical_formula_moiety         'C22 H19 N O5 S, C2 D6 O S'
_chemical_formula_sum            'C24 H19 D6 N O6 S2'
_chemical_formula_weight         493.61
_chemical_name_systematic
;10-Hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1<i>H</i>-9-thia-2-azacyclopenta[<i>b</i>]fluorene-4-carboxylic acid dimethyl
sulfoxide-<i>d</i>~6~ 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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.7710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3178(4)
_cell_length_b                   9.2747(2)
_cell_length_c                   14.8720(4)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      2.59
_cell_volume                     2245.90(10)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX4 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker Kappa APEXII area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69078
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.211
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6531
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0518P)^2^+1.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                5693
_reflns_number_total             6531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2077sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022937.cif.'
_cod_original_cell_volume        2245.89(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022937
_cod_database_fobs_code          2022937
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.941
_shelx_hkl_checksum              98466
_shelx_res_checksum              34432