A variable-temperature X-ray diffraction and theoretical study of conformational polymorphism in a complex organic molecule (DTC)
Gionda, Andrea; Macetti, Giovanni; Loconte, Laura; Rizzato, Silvia; Orlando, Ahmed M.; Gatti, Carlo; Lo Presti, Leonardo; RSC Advances 8 (2018) 38445–; doi:10.1039/C8RA08063A

data_7231821
_publ_section_title
;
 A variable-temperature X-ray diffraction and theoretical study of
 conformational polymorphism in a complex organic molecule (DTC)
;
_journal_issue                   67
_journal_name_full               'RSC Advances'
_journal_page_first              38445
_journal_paper_doi               10.1039/C8RA08063A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C14 H17 N3 O3 S'
_chemical_formula_sum            'C14 H17 N3 O3 S'
_chemical_formula_weight         307.36
_chemical_name_systematic
;
'3-Diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1\l^6^
,2-thiazete-4-carbonitrile'
;
_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   direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2016-04-18
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-02-01 deposited with the CCDC.
2018-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7854(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.61220(10)
_cell_length_b                   13.3460(2)
_cell_length_c                   13.1742(2)
_cell_measurement_reflns_used    5720
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      27.249
_cell_measurement_theta_min      2.714
_cell_volume                     1508.94(4)
_computing_cell_refinement       'Saint+(Bruker, 2007/4)'
_computing_data_collection       'Saint+(Bruker, 2007/4)'
_computing_data_reduction        'Saint+(Bruker, 2007/4)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2016)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Smart APEX'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.176
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_correction_T_min  0.9179
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2007/4, Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.125
_exptl_transmission_factor_max   0.9391
_exptl_transmission_factor_min   0.9179
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0529P)^2^+0.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2779
_reflns_number_total             3489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra08063a2.cif
_cod_data_source_block           A_260
_cod_database_code               7231821
_shelx_res_checksum              28525
_shelx_hkl_checksum              57908