Crystal structure of 3,4-dimethyl 2-(<i>tert</i>-butylamino)-5-[2-oxo-4-(thiomorpholin-4-yl)-2<i>H</i>-chromen-3-yl]furan-3,4-dicarboxylate ethyl acetate hemisolvate
Moriguchi, Tetsuji; Jalli, Venkataprasad; Krishnamurthy, Suvratha; Tsuge, Akihiko; Yoza, Kenji; Acta Crystallographica Section E 71 (2015) o1003–o1004; doi:10.1107/S2056989015021970

data_2241360
_publ_section_title
;
 Crystal structure of 3,4-dimethyl
 2-(<i>tert</i>-butylamino)-5-[2-oxo-4-(thiomorpholin-4-yl)-2<i>H</i>-chromen-3-yl]furan-3,4-dicarboxylate
 ethyl acetate hemisolvate
;
_journal_coeditor_code           HB7531
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1003
_journal_page_last               o1004
_journal_paper_doi               10.1107/S2056989015021970
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          ' C25 H28 N2 O7 S, 0.5C4 H8 O2'
_chemical_formula_moiety         ' C25 H28 N2 O7 S, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C27 H32 N2 O8 S'
_chemical_formula_weight         544.61
_chemical_name_systematic
;3,4-Dimethyl
2-(<i>tert</i>-butylamino)-5-[2-oxo-4-(thiomorpholin-4-yl)-2<i>H</i>-chromen-3-yl]furan-3,4-dicarboxylate ethyl acetate hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.1-2'
_cell_angle_alpha                90
_cell_angle_beta                 95.0070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3733(17)
_cell_length_b                   16.1159(19)
_cell_length_c                   11.7019(14)
_cell_measurement_reflns_used    25410
_cell_measurement_temperature    90.(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.42
_cell_volume                     2700.3(6)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25410
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.229
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4757
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                4316
_reflns_number_total             4757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hb7531sup1.cif
_cod_data_source_block           I
_cod_database_code               2241360
_cod_database_fobs_code          2241360