Crystal structure of ethyl 3-amino-6-methyl-2-[(4-methylphenyl)carbamoyl]-4-[(<i>E</i>)-2-phenylethenyl]thieno[2,3-<i>b</i>]pyridine-5-carboxylate monohydrate
Mague, Joel T.; Akkurt, Mehmet; Mohamed, Shaaban K.; Bakhite, Etify A.; Albayati, Mustafa R.; Acta Crystallographica Section E 72 (2016) 297–299; doi:10.1107/S2056989016001341

data_2241538
_publ_section_title
;
 Crystal structure of ethyl
 3-amino-6-methyl-2-[(4-methylphenyl)carbamoyl]-4-[(<i>E</i>)-2-phenylethenyl]thieno[2,3-<i>b</i>]pyridine-5-carboxylate
 monohydrate
;
_journal_coeditor_code           RZ5183
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              297
_journal_page_last               299
_journal_paper_doi               10.1107/S2056989016001341
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C27 H25 N3 O3 S, H2 O'
_chemical_formula_moiety         'C27 H25 N3 O3 S, H2 O'
_chemical_formula_sum            'C27 H27 N3 O4 S'
_chemical_formula_weight         489.57
_chemical_name_systematic
;Ethyl
3-amino-6-methyl-2-[(4-methylphenyl)carbamoyl]-4-[(<i>E</i>)-2-phenylethenyl]thieno[2,3-<i>b</i>]pyridine-5-carboxylate monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.4460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.083(3)
_cell_length_b                   12.0766(10)
_cell_length_c                   14.7678(12)
_cell_measurement_reflns_used    7720
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6849
_cell_measurement_theta_min      2.1884
_cell_volume                     5227.3(8)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2015)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2015)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2015)
;
_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 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24570
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.012
_diffrn_reflns_theta_min         1.390
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0777P)^2^+0.6476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                4746
_reflns_number_total             6682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5183sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5227.2(7)
_cod_database_code               2241538
_cod_database_fobs_code          2241538
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              1628
_shelx_res_checksum              30658
_shelx_fab_checksum              48324