A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4<i>H</i>-1λ^6^,2-thiazete-4-carbonitrile
Orlando, Ahmed M.; Lo Presti, Leonardo; Soave, Raffaella; Acta Crystallographica Section E 66 (2010) o2032–o2033; doi:10.1107/S1600536810027558

data_2227025
_publ_section_title
;
 A new monoclinic polymorph of
 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4<i>H</i>-1\l^6^,2-thiazete-4-carbonitrile
;
_journal_coeditor_code           NK2045
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2032
_journal_page_last               o2033
_journal_paper_doi               10.1107/S1600536810027558
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C14 H17 N3 O3 S'
_chemical_formula_moiety         'C14 H17 N3 O3 S'
_chemical_formula_sum            'C14 H17 N3 O3 S'
_chemical_formula_weight         307.37
_chemical_name_systematic
;
3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4<i>H</i>-1\l^6^,2-thiazete-
4-carbonitrile
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90.00
_cell_angle_beta                 95.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3853(17)
_cell_length_b                   17.554(4)
_cell_length_c                   10.458(2)
_cell_measurement_reflns_used    2885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.58
_cell_measurement_theta_min      2.28
_cell_volume                     1533.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16661
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0446P)^2^+0.4078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                1949
_reflns_number_total             2814
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nk2045.cif
_cod_data_source_block           I
_cod_original_cell_volume        1533.4(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2227025
_cod_database_fobs_code          2227025