#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000698.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000698 loop_ _publ_author_name 'Keith Prout' 'Stephen J. Heyes' 'Christopher M. Dobson' 'Andrew McDaid' 'Thierry Maris' 'Matthias Muller' 'Matthew J. Seaman' _publ_section_title ; Variable-Temperature Studies of Order/Disorder Transitions in the Thiourea Pyridinium Halide Crystals by XRD and Solid-State 2H NMR ; _journal_name_full 'Chemistry of Material' _journal_page_first 3561 _journal_page_last 3569 _journal_paper_doi 10.1021/cm0001612 _journal_volume 12 _journal_year 2000 _chemical_formula_sum 'C7 H14 Br N5 S2' _chemical_formula_weight 312.25 _space_group_IT_number 36 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 36 _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_space_group_name_H-M 'C m c 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 44.128(6) _cell_length_b 10.7890(6) _cell_length_c 8.3510(10) _cell_measurement_temperature 150(2) _cell_volume 3975.9(8) _diffrn_ambient_temperature 150(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6034 _diffrn_reflns_theta_max 74.3 _diffrn_reflns_theta_min 2.0 _exptl_absorpt_coefficient_mu 3.34 _exptl_crystal_density_diffrn 1.461 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 1912 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.059 _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.057 _reflns_number_gt 1912 _reflns_number_total 2176 _reflns_threshold_expression >3sigma(I) _cod_data_source_file deposit.cif _cod_data_source_block Bromo_2 _cod_original_sg_symbol_H-M Cmc21 _cod_database_code 4000698 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z -x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,z 1/2+x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type C21 C 0.1627(2) 0.3904(8) -0.4910(10) 0.063(3) Uani C22 C 0.13930(10) 0.4639(7) -0.5500(10) 0.065(3) Uani C23 C 0.1451(2) 0.5857(7) -0.5903(9) 0.058(3) Uani C24 C 0.1739(2) 0.6327(7) -0.5710(9) 0.061(3) Uani C25 C 0.1965(2) 0.5610(9) -0.5090(10) 0.083(4) Uani C26 C 0.1909(2) 0.4395(9) -0.4709(9) 0.065(3) Uani C30 C 0.0000 -0.1319(9) -0.4610(10) 0.086(5) Uani C31 C 0.02680(10) -0.0728(8) -0.4833(8) 0.095(5) Uani C32 C 0.02690(10) 0.0477(9) -0.5291(8) 0.100(5) Uani C33 C 0.0000 0.1080(10) -0.5510(10) 0.080(5) Uani S3 S 0.25639(4) -0.2861(2) -0.2444(3) 0.0310(6) Uani N9 N 0.2159(2) -0.1373(7) -0.3871(9) 0.033(2) Uani N11 N 0.2165(2) -0.1342(8) -0.1133(8) 0.034(2) Uani C12 C 0.22740(10) -0.1785(6) -0.2440(10) 0.0207(17) Uani S4 S 0.07719(5) -0.2869(2) -0.2667(4) 0.0367(6) Uani N8 N 0.1160(2) -0.1398(7) -0.1330(9) 0.033(2) Uani N10 N 0.1184(2) -0.1398(7) -0.4047(9) 0.030(2) Uani C13 C 0.1052(2) -0.1813(6) -0.2640(10) 0.0283(19) Uani S5 S 0.08968(5) -0.2144(2) 0.2346(4) 0.0397(6) Uani N6 N 0.0480(2) -0.3541(6) 0.0913(7) 0.0253(17) Uani N7 N 0.0518(2) -0.3722(8) 0.3661(9) 0.0303(19) Uani C14 C 0.0616(2) -0.3217(6) 0.2350(10) 0.027(2) Uani Br1 Br 0.0000 -0.58782(8) 0.2294(2) 0.0236(4) Uani Br2 Br 0.16665(2) 0.08771(5) -0.2508(2) 0.0239(3) Uani loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C21 0.092(6) 0.038(5) 0.058(7) 0.005(5) 0.000(5) 0.009(3) C22 0.046(4) 0.065(5) 0.084(8) -0.012(5) -0.012(5) -0.006(3) C23 0.070(4) 0.056(4) 0.048(6) -0.010(4) -0.017(7) 0.018(3) C24 0.092(7) 0.038(5) 0.052(7) 0.004(5) -0.010(5) -0.013(4) C25 0.078(7) 0.062(4) 0.110(10) -0.020(6) -0.013(7) 0.007(5) C26 0.075(5) 0.059(4) 0.061(7) -0.011(5) -0.020(5) 0.033(4) C30 0.210(10) 0.012(5) 0.037(8) 0.006(5) 0.000 0.000 C31 0.102(8) 0.083(6) 0.100(10) -0.048(7) -0.048(8) 0.055(5) C32 0.087(7) 0.074(6) 0.140(10) -0.058(8) 0.002(8) -0.001(5) C33 0.105(9) 0.046(7) 0.090(10) -0.017(9) 0.000 0.000 S3 0.037(1) 0.040(1) 0.016(1) -0.0022(9) -0.001(1) 0.0217(8) N9 0.043(4) 0.038(4) 0.019(4) 0.015(3) 0.000(3) 0.021(3) N11 0.053(5) 0.033(4) 0.016(3) 0.002(3) -0.006(3) 0.017(3) C12 0.018(3) 0.026(3) 0.018(3) -0.001(3) -0.009(3) 0.004(2) S4 0.043(1) 0.043(1) 0.024(1) 0.000(1) -0.001(1) -0.0253(9) N8 0.038(4) 0.038(4) 0.024(3) 0.014(3) -0.004(3) -0.013(3) N10 0.027(3) 0.036(4) 0.027(4) 0.005(3) 0.010(3) -0.013(3) C13 0.035(4) 0.025(3) 0.025(3) -0.002(3) 0.014(3) -0.011(2) S5 0.0430(10) 0.051(1) 0.025(1) 0.004(1) -0.002(1) -0.032(1) N6 0.027(3) 0.030(3) 0.019(3) -0.005(3) -0.006(3) -0.010(3) N7 0.037(4) 0.032(3) 0.022(3) -0.007(3) 0.001(3) -0.010(3) C14 0.032(4) 0.029(4) 0.020(2) 0.000(3) -0.011(3) -0.007(3) Br1 0.0205(5) 0.0154(4) 0.0350(10) -0.0007(5) 0.000 0.000 Br2 0.0219(4) 0.0173(3) 0.0324(8) 0.0017(4) 0.0023(2) 0.0002(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 C21 C26 120.0(8) . no C21 C22 C23 119.4(6) . no C22 C23 C24 119.5(7) . no C23 C24 C25 120.7(7) . no C24 C25 C26 119.9(8) . no C21 C26 C25 120.5(8) . no C31 C30 C31 121.4(8) 3_555 no C30 C31 C32 119.5(6) . no C31 C32 C33 119.5(6) . no C32 C33 C32 120.7(9) 3_555 no S3 C12 N9 119.3(6) . yes S3 C12 N11 121.9(6) . yes N9 C12 N11 118.7(6) . yes S4 C13 N8 121.6(7) . yes S4 C13 N10 121.1(6) . yes N8 C13 N10 117.2(8) . yes S5 C14 N6 119.1(6) . yes S5 C14 N7 122.1(7) . yes N6 C14 N7 118.7(8) . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S3 C12 1.728(6) . yes S4 C13 1.681(8) . yes S5 C14 1.696(8) . yes N9 C12 1.372(11) . yes N11 C12 1.285(11) . yes N8 C13 1.275(11) . yes N10 C13 1.386(11) . yes N6 C14 1.387(11) . yes N7 C14 1.297(11) . yes C21 C22 1.392(11) . no C21 C26 1.363(13) . no C22 C23 1.380(11) . no C23 C24 1.378(12) . no C24 C25 1.364(12) . no C25 C26 1.371(14) . no C30 C31 1.356(7) . no C30 C31 1.356(7) 3_555 no C31 C32 1.355(13) . no C32 C33 1.366(8) . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C26 C21 C22 C23 1.1(12) . . no C22 C21 C26 C25 -0.3(12) . . no C21 C22 C23 C24 -0.2(12) . . no C22 C23 C24 C25 -1.6(12) . . no C23 C24 C25 C26 2.5(12) . . no C24 C25 C26 C21 -1.5(12) . . no C31 C30 C31 C32 -0.1(12) 3_555 . no C30 C31 C32 C33 0.5(11) . . no C31 C32 C33 C32 -0.8(12) . 3_555 no