#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2104218.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2104218 loop_ _publ_author_name 'Ma\/luszy\'nska, H.' 'Czarnecki, P.' 'Fojud, Z.' 'Wasicki, J.' _publ_section_title ; Redetermination of the structure and dielectric properties of bis(thiourea) pyridinium iodide -- a new ferroelectric inclusion compound ; _journal_coeditor_code WS5061 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 567 _journal_page_last 572 _journal_volume 64 _journal_year 2008 _chemical_formula_moiety '2[SC(NH2)2] [C5H6N]+ [I]-' _chemical_formula_sum 'C7 H14 I N5 S2' _chemical_formula_weight 359.25 _chemical_name_systematic ; bis-thiourea pyridinium iodide ; _space_group_IT_number 40 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'C -2c 2' _symmetry_space_group_name_H-M 'C 2 c m' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.022(3) _cell_length_b 11.227(2) _cell_length_c 8.3410(17) _cell_measurement_reflns_used 23 _cell_measurement_temperature 155.0(2) _cell_measurement_theta_max 14.5 _cell_measurement_theta_min 7.5 _cell_volume 1406.7(5) _computing_cell_refinement 'KUMA KM-4' _computing_data_collection 'KUMA KM-4' _computing_data_reduction 'KUMA KM-4 Data reduction program' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 155.0(2) _diffrn_measured_fraction_theta_full 0.888 _diffrn_measured_fraction_theta_max 0.888 _diffrn_measurement_device_type 'KUMA KM-4 diffractometer' _diffrn_measurement_method 'omega - 2theta' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\alpha _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1960 _diffrn_reflns_theta_full 30.09 _diffrn_reflns_theta_max 30.09 _diffrn_reflns_theta_min 2.26 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.554 _exptl_absorpt_correction_T_max 0.62 _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.756 _refine_diff_density_min -0.692 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.35(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1010 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0220 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.030 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0576 _reflns_number_gt 920 _reflns_number_total 1010 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ws5061.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M C2cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y, -z+1/2' 'x, -y, z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy I I1 0.22848(7) 0.40864(2) 0.2500 0.01881(10) Uani d S 1 S S1 0.0145(2) 0.2562(3) 0.2500 0.0452(7) Uani d S 1 S S2 -0.0319(2) -0.2031(3) 0.2500 0.0471(8) Uani d S 1 C C11 -0.0788(7) 0.1692(11) 0.2500 0.032(2) Uani d S 1 C C21 0.0451(8) -0.3145(10) 0.2500 0.029(2) Uani d S 1 N N11 -0.1154(5) 0.1348(7) 0.1139(7) 0.0355(17) Uani d . 1 H H11A -0.0874 0.1592 0.0061 0.043 Uiso d R 1 H H11B -0.1721 0.0833 0.1157 0.043 Uiso d R 1 N N21 0.0771(6) -0.3569(7) 0.1119(7) 0.0367(16) Uani d . 1 H H21A 0.0554 -0.3210 0.0052 0.044 Uiso d R 1 H H21B 0.1234 -0.4246 0.1115 0.044 Uiso d R 1 C C4 0.268(4) -0.119(4) -0.038(7) 0.11(2) Uani d P 0.50 C C1 0.1546(18) -0.026(3) 0.051(3) 0.084(9) Uani d P 0.50 C C3 0.223(4) -0.109(3) -0.006(5) 0.085(14) Uani d P 0.50 C C2 0.172(4) -0.090(3) -0.058(5) 0.094(17) Uani d P 0.50 C C5 0.286(5) -0.068(4) -0.060(7) 0.11(2) Uani d P 0.50 C C6 0.320(3) -0.054(3) 0.028(4) 0.079(9) Uani d P 0.50 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.01728(15) 0.01789(15) 0.02127(13) -0.0010(3) 0.000 0.000 S1 0.0492(13) 0.0691(16) 0.0174(8) -0.0432(13) 0.000 0.000 S2 0.0621(17) 0.0637(15) 0.0154(7) 0.0471(14) 0.000 0.000 C11 0.027(4) 0.046(6) 0.023(4) -0.023(4) 0.000 0.000 C21 0.042(5) 0.035(4) 0.011(3) 0.014(4) 0.000 0.000 N11 0.043(3) 0.049(4) 0.015(2) -0.034(4) -0.003(2) 0.002(3) N21 0.048(4) 0.046(4) 0.017(3) 0.023(4) 0.001(3) -0.002(3) C4 0.15(5) 0.06(2) 0.12(3) 0.07(3) -0.04(3) 0.00(3) C1 0.071(13) 0.10(2) 0.077(13) -0.041(14) 0.015(9) -0.035(15) C3 0.11(3) 0.043(13) 0.102(18) -0.054(16) -0.01(2) -0.010(12) C2 0.13(4) 0.08(3) 0.068(18) -0.04(2) -0.05(2) 0.041(15) C5 0.16(5) 0.06(2) 0.10(3) 0.09(3) 0.05(3) 0.03(2) C6 0.079(18) 0.075(17) 0.08(2) 0.030(14) -0.005(14) 0.010(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C11 . 1.708(10) y S2 C21 . 1.705(11) y C11 N11 . 1.319(7) y C11 N11 2 1.319(7) y C21 N21 2 1.336(7) y C21 N21 . 1.336(7) y C4 C2 . 1.49(8) y C4 C6 . 1.20(7) y C1 C3 . 1.47(7) y C1 C2 4 1.33(4) y C3 C5 . 1.15(10) y C5 C6 4 1.49(7) y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N11 C11 N11 . 2 118.8(9) y N11 C11 S1 . . 120.6(4) y N11 C11 S1 2 . 120.6(4) y N21 C21 N21 2 . 119.2(10) y N21 C21 S2 2 . 120.4(5) y N21 C21 S2 . . 120.4(5) y C2 C4 C6 . . 124(5) y C3 C1 C2 . 4 120(3) y C1 C3 C5 . . 117(3) y C4 C2 C1 . 4 113(4) y C6 C5 C3 4 . 126(4) y C5 C6 C4 4 . 114(4) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N11 H11A S2 3_554 1.03 2.34 3.372(7) 175.1 N11 H11B I1 5_445 1.03 2.71 3.638(7) 150.3 N21 H21A S1 3_554 1.03 2.33 3.358(7) 173.9 N21 H21B I1 1_545 1.03 2.71 3.664(8) 154.5 _cod_database_code 2104218