Ethyl 13-(4-chlorophenyl)-11-methyl-6-oxo-5-phenyl-8-thia-3,4,5,10-tetraazatricyclo[7.4.0.0^2,7^]trideca-1(9),2(7),3,10,12-pentaene-12-carboxylate
Al-Taifi, Elham A.; Mague, Joel T.; Mohamed, Shaaban K.; Akkurt, Mehmet; Bakhite, Etify A.; IUCrData 1 (2016) x160701–; doi:10.1107/S241431461600701X

data_1543256
_publ_section_title
;
 Ethyl
 13-(4-chlorophenyl)-11-methyl-6-oxo-5-phenyl-8-thia-3,4,5,10-tetraazatricyclo[7.4.0.0^2,7^]trideca-1(9),2(7),3,10,12-pentaene-12-carboxylate
;
_journal_coeditor_code           TK4011
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x160701
_journal_paper_doi               10.1107/S241431461600701X
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C24 H17 Cl N4 O3 S'
_chemical_formula_moiety         'C24 H17 Cl N4 O3 S'
_chemical_formula_sum            'C24 H17 Cl N4 O3 S'
_chemical_formula_weight         476.92
_chemical_name_systematic
'Ethyl 13-(4-chlorophenyl)-11-methyl-6-oxo-5-phenyl-8-thia-3,4,5,10-tetraazatricyclo[7.4.0.0^2,7^]trideca-1(9),2(7),3,10,12-pentaene-12-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.0450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8562(3)
_cell_length_b                   7.1984(2)
_cell_length_c                   25.4331(5)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.3070
_cell_measurement_theta_min      3.5413
_cell_volume                     2130.40(9)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i>  (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15584
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.352
_diffrn_reflns_theta_min         3.541
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.253
_refine_ls_extinction_coef       0.00183(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2014</i> (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4116
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+1.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                3824
_reflns_number_total             4116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk4011sup1.cif
_cod_data_source_block           I
_cod_database_code               1543256
_cod_database_fobs_code          1543256
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.849
_shelx_hkl_checksum              89469
_shelx_res_checksum              94280