The crystal structures and Hirshfeld surface analyses of four 3,5-diacetyl-2-methyl-2,3-dihydro-1,3,4-thiadiazol-2-yl derivatives
NizamMohideen, M.; Syed Abuthahir, S.; Viswanathan, V.; Velmurugan, D.; Karthik Ananth, M.; Acta Crystallographica Section E 75 (2019) 1436–1444; doi:10.1107/S2056989019011915

data_2243082
_publ_section_title
;
 The crystal structures and Hirshfeld surface analyses of four
 3,5-diacetyl-2-methyl-2,3-dihydro-1,3,4-thiadiazol-2-yl derivatives
;
_journal_coeditor_code           SU5508
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1436
_journal_page_last               1444
_journal_paper_doi               10.1107/S2056989019011915
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C17 H21 N3 O4 S, 0.25H2 O'
_chemical_formula_moiety         'C17 H21 N3 O4 S, 0.25(H2 O)'
_chemical_formula_sum            'C17 H21.5 N3 O4.25 S'
_chemical_formula_weight         367.93
_chemical_name_common
;
4-(5-Acetamido-3-acetyl-2-methyl-2,3-dihydro-1,3,4-thiadiazol-2-yl)phenyl
isobutyrate 0.25-hydrate
;
_chemical_name_systematic
;
4-(5-Acetamido-3-acetyl-2-methyl-2,3-dihydro-1,3,4-thiadiazol-2-yl)phenyl
2-methylpropanoate 0.25-hydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                108.2240(10)
_cell_angle_beta                 99.0840(10)
_cell_angle_gamma                96.7200(10)
_cell_formula_units_Z            4
_cell_length_a                   6.78020(10)
_cell_length_b                   17.2671(4)
_cell_length_c                   17.3089(4)
_cell_measurement_reflns_used    7680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.41
_cell_volume                     1870.50(7)
_computing_cell_refinement
;
APEX2 (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and PLATON
(Spek, 2009)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-2018/3 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27060
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.484
_diffrn_reflns_theta_min         2.418
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7680
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0901P)^2^+0.7340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                5737
_reflns_number_total             7680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5508sup1.cif
_cod_data_source_block           II
_cod_original_formula_sum        'C17 H21.50 N3 O4.25 S'
_cod_database_code               2243082
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              99914
_shelx_res_checksum              30340