Crystal structure of ethyl 2-methyl-5,10-dioxo-4-phenyl-5,10-dihydro-4<i>H</i>-11-thia-1,4a-diazabenzo[<i>b</i>]fluorene-3-carboxylate
Yartsev, Yegor; Lyubashov, Pavel; Povstyanoy, Vyacheslav; Povstyaniy, Mykhailo; Lebedyeva, Iryna; Acta Crystallographica Section E 74 (2018) 124–126; doi:10.1107/S2056989018000117

data_2242306
_publ_section_title
;
 Crystal structure of ethyl
 2-methyl-5,10-dioxo-4-phenyl-5,10-dihydro-4<i>H</i>-11-thia-1,4a-diazabenzo[<i>b</i>]fluorene-3-carboxylate
;
_journal_coeditor_code           ZQ2240
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              124
_journal_page_last               126
_journal_paper_doi               10.1107/S2056989018000117
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C24 H18 N2 O4 S'
_chemical_formula_moiety         'C24 H18 N2 O4 S'
_chemical_formula_sum            'C24 H18 N2 O4 S'
_chemical_formula_weight         430.46
_chemical_name_systematic
;
Ethyl 2-methyl-5,10-dioxo-4-phenyl-5,10-dihydro-4<i>H</i>-11-thia-1,4a-\
diazabenzo[<i>b</i>]fluorene-3-carboxylate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1038(3)
_cell_length_b                   13.3915(6)
_cell_length_c                   18.7377(9)
_cell_measurement_reflns_used    3614
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      3.0
_cell_volume                     2033.45(15)
_computing_cell_refinement
;
(CrysAlisPro; Oxford Diffraction, 2010
;
_computing_data_collection
;
(CrysAlisPro; Oxford Diffraction, 2010
;
_computing_data_reduction
;
(CrysAlisPro; Oxford Diffraction, 2010
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Sapphire3'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6202
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         3.042
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Oxford Diffraction, 2010
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.137
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1207 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0436P)^2^+0.1932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3160
_reflns_number_total             3574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2240sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2033.44(15)
_cod_database_code               2242306
_cod_database_fobs_code          2242306
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              17558
_shelx_res_checksum              86442