#------------------------------------------------------------------------------ #$Date$ #$Revision$ #$URL$ #------------------------------------------------------------------------------ # # 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_2104217 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_sum 'C7 H14 I N5 S2' _chemical_formula_weight 359.25 _chemical_melting_point '2[SC(NH2)2] [C5H6N]+ [I]-' _chemical_name_systematic ; bis-thiourea pyridinium iodide ; _space_group_IT_number 63 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2c 2' _symmetry_space_group_name_H-M 'C m 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 15.180(3) _cell_length_b 11.827(2) _cell_length_c 8.375(2) _cell_measurement_reflns_used 34 _cell_measurement_temperature 295.0(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 7.0 _cell_volume 1503.6(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 295.0(2) _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _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 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2244 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 2.18 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.587 _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 0.1 _refine_diff_density_max 0.669 _refine_diff_density_min -0.915 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.737 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 1158 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.737 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0286 _refine_ls_shift/su_max 0.135 _refine_ls_shift/su_mean 0.032 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.0904 _reflns_number_gt 965 _reflns_number_total 1158 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ws5061.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M Cmcm 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' '-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 0.0000 0.40856(3) 0.2500 0.03794(14) Uani d S 1 S S1 0.22815(11) 0.27706(18) 0.2500 0.0843(6) Uani d S 1 C C11 0.3118(3) 0.1785(4) 0.2500 0.0518(11) Uani d S 1 N N11 0.3458(2) 0.1386(3) 0.1146(3) 0.0668(10) Uani d . 1 H H11A 0.3221 0.1674 0.0068 0.080 Uiso d R 1 H H11B 0.3957 0.0796 0.1172 0.080 Uiso d R 1 C C2 0.435(2) 0.424(3) -0.054(4) 0.145(13) Uani d P 0.50 C C3 0.4206(19) 0.458(3) 0.032(4) 0.142(11) Uani d P 0.50 C C1 0.5000 0.3829(16) -0.027(3) 0.178(11) Uani d S 1 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 0.03287(18) 0.0397(2) 0.0413(2) 0.000 0.000 0.000 S1 0.0916(10) 0.1316(14) 0.0297(5) 0.0793(10) 0.000 0.000 C11 0.057(2) 0.068(3) 0.0309(16) 0.026(2) 0.000 0.000 N11 0.080(2) 0.091(2) 0.0296(11) 0.0498(19) 0.0027(13) -0.0013(13) C2 0.17(3) 0.15(3) 0.114(16) -0.07(2) -0.02(2) 0.030(18) C3 0.116(13) 0.18(3) 0.125(17) -0.041(16) -0.001(14) 0.021(16) C1 0.26(3) 0.100(8) 0.17(2) 0.000 0.000 -0.024(11) 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 . 1.724(4) y C11 N11 . 1.333(3) y C11 N11 10_556 1.333(3) y C2 C1 . 1.13(4) y C2 C3 4_565 1.42(4) y C3 C1 . 1.58(4) 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 . 10_556 116.7(4) y N11 C11 S1 . . 121.7(2) y N11 C11 S1 10_556 . 121.7(2) y C1 C2 C3 . 4_565 122(4) y C2 C3 C1 4_565 . 118(3) y C2 C1 C3 12_655 . 119(2) 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 S1 13 1.03 2.37 3.403(3) 176.1 N11 H11B I1 5_545 1.03 2.80 3.763(3) 156.1