Supramolecular structures of bis-thionooxalamic acid esters derived from (±)-cyclohexane-1,2-diamine and (±)-1,2-diphenylethylenediamine
Piotrkowska, Barbara; Połoński, Tadeusz; Gdaniec, Maria; Acta Crystallographica Section C 63 (2007) o693–o696; doi:10.1107/S0108270107049797

data_2016327
_publ_section_title
;
 Supramolecular structures of bis-thionooxalamic acid esters derived
 from (+-)-cyclohexane-1,2-diamine and (+-)-1,2-diphenylethylenediamine
;
_journal_coeditor_code           GD3156
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o693
_journal_page_last               o696
_journal_paper_doi               10.1107/S0108270107049797
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H24 N2 O4 S2'
_chemical_formula_moiety         'C22 H24 N2 O4 S2'
_chemical_formula_sum            'C22 H24 N2 O4 S2'
_chemical_formula_weight         444.55
_chemical_name_systematic
;
(+-)-<i>N,N'</i>-diethyl (1,2-diphenylethane-1,2-diyl)bis(2-thiooxamate)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.273(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2414(4)
_cell_length_b                   21.7781(10)
_cell_length_c                   11.4322(6)
_cell_measurement_reflns_used    4659
_cell_measurement_temperature    110.0(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     2263.96(19)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
Stereochemical Workstation (Siemens, 1989) and
Mercury (Version 1.4; Macrae <i>et al.</i>,  2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110.0(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kuma KM-4 CCD \k geometry'
_diffrn_measurement_method       '\w 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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16375
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;calc w=1/[\\s\^2\^(Fo\^2\^)+(0.0469P)\^2\^+0.1761P]
where
 P=(Fo\^2\^+2Fc\^2\^)/3'
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                3649
_reflns_number_total             4613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3156.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016327
_cod_database_fobs_code          2016327