Three-dimensional hydrogen-bonded assembly in 2,2'-disulfanylidene-5,5'-biimidazolidinylidene-4,4'-dione–dimethylformamide–water (3/2/4)
Wu, De-Hong; Acta Crystallographica Section C 69 (2013) 1545–1548; doi:10.1107/S0108270113031521

data_2019322
_publ_section_title
;
 Three-dimensional hydrogen-bonded assembly in
 2,2'-disulfanylidene-5,5'-biimidazolidinylidene-4,4'-dione--dimethylformamide--water
 (3/2/4)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1545
_journal_page_last               1548
_journal_paper_doi               10.1107/S0108270113031521
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '3C6 H4 N4 O2 S2, 2C3 H7 N O, 4H2 O'
_chemical_formula_moiety         '3(C6 H4 N4 O2 S2), 2(C3 H7 N O), 4(H2 O)'
_chemical_formula_sum            'C24 H34 N14 O12 S6'
_chemical_formula_weight         903.01
_chemical_name_systematic
'2,2'-Disulfanylidene-5,5'-biimidazolidinylidene-4,4'-dione--dimethylformamide--water (3/2/4)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.600(10)
_cell_angle_beta                 103.470(10)
_cell_angle_gamma                102.81(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0655(16)
_cell_length_b                   10.391(2)
_cell_length_c                   12.735(3)
_cell_measurement_reflns_used    8524
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.18
_cell_volume                     952.5(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9925
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.9179
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4359
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.4062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                3164
_reflns_number_total             4359
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wq3050.cif
_cod_data_source_block           I
_cod_original_cell_volume        952.5(3)
_cod_database_code               2019322