The interplay of solvation, molecular conformation and supramolecular assembly in 1,1'-({[(ethane-1,2-diyl)dioxy](1,2-phenylene)}bis(methanylylidene))bis(thiosemicarbazide) and its <i>N</i>,<i>N</i>-dimethylformamide disolvate
Mohamed, Shaaban K.; Younes, Sabry H. H.; Abdel-Raheem, Eman M. M.; Mague, Joel T.; Akkurt, Mehmet; Glidewell, Christopher; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615018744

data_2020203
_publ_section_title
;
 The interplay of solvation, molecular conformation and supramolecular
 assembly in
 1,1'-({[(ethane-1,2-diyl)dioxy](1,2-phenylene)}bis(methanylylidene))bis(thiosemicarbazide)
 and its <i>N</i>,<i>N</i>-dimethylformamide disolvate
;
_journal_coeditor_code           FA3376
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615018744
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C18 H20 N6 O2 S2 , 2C3 H7 N O'
_chemical_formula_moiety         'C18 H20 N6 O2 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C24 H34 N8 O4 S2'
_chemical_formula_weight         562.71
_chemical_name_systematic
;
1,1'-({[(ethane-1,2-diyl)dioxy](1,2-
phenylene)}bis(methanylylidene))bis(thiosemicarbazide)
bis(N,N-dimethylformamide) solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_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
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 101.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6081(16)
_cell_length_b                   18.136(3)
_cell_length_c                   14.186(2)
_cell_measurement_reflns_used    7514
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.732
_cell_measurement_theta_min      1.792
_cell_volume                     2923.4(8)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.3660
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49268
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.792
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.266
_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     383
_refine_ls_number_reflns         6697
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0593P)^2^+0.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5575
_reflns_number_total             6697
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3376sup1.cif
_cod_data_source_block           II
_cod_database_code               2020203
_cod_database_fobs_code          2020203
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.982
_shelx_hkl_checksum              13651
_shelx_res_checksum              2605
_shelxl_version_number           2.014