#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200031.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_2200031 loop_ _publ_author_name 'Lynch, Daniel E.' 'McClenaghan, Ian' _publ_section_title ; 6-Amino-4-iminio-4H-1,3,5-dithiazole iodide ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o70 _journal_page_last o71 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C3 H6 N3 S2 1+, I 1-' _chemical_formula_moiety 'C3 H6 N3 S2 1+, I 1-' _chemical_formula_sum 'C3 H6 I N3 S2' _chemical_formula_weight 275.13 _chemical_melting_point '? K' _chemical_name_systematic ; 4-Amino-6-imidium-1,3,5-dithiazol-4-ene iodide ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 108.87(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 11.050(2) _cell_length_b 18.964(4) _cell_length_c 8.1307(16) _cell_measurement_reflns_used 5412 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.0 _cell_volume 1612.2(6) _computing_cell_refinement 'DENZO and COLLECT' _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction 'DENZO and COLLECT' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full .977 _diffrn_measured_fraction_theta_max .977 _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .074 _diffrn_reflns_av_sigmaI/netI .045 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7382 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.1 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.41 _exptl_absorpt_correction_T_max .719 _exptl_absorpt_correction_T_min .307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1040 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .08 _refine_diff_density_max 2.79 _refine_diff_density_min -2.70 _refine_ls_extinction_coef .0043(5) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1818 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.05 _refine_ls_R_factor_all .046 _refine_ls_R_factor_gt .044 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.3966P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .109 _reflns_number_gt 1726 _reflns_number_total 1818 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf6017.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2200031 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol I1 .5000 .127771(16) .2500 .01778(18) Uani d S 1 . . I I2 .0000 .10986(2) .2500 .01743(18) Uani d S 1 . . I S1 .17012(7) .19044(5) .82791(10) .0177(2) Uani d . 1 . . S C2 .3142(3) .22011(17) .7927(4) .0158(6) Uani d . 1 . . C H21 .3122 .2722 .7829 .020 Uiso calc R 1 . . H H22 .3885 .2072 .8946 .020 Uiso calc R 1 . . H S3 .33490(7) .18302(5) .60085(10) .0157(2) Uani d . 1 . . S C4 .3257(3) .09344(18) .6500(4) .0136(6) Uani d . 1 . . C N41 .3741(3) .05065(16) .5627(3) .0194(6) Uani d . 1 . . N H41 .371(3) .012(2) .576(5) .016(9) Uiso d . 1 . . H H42 .415(4) .066(3) .488(5) .041(12) Uiso d . 1 . . H N5 .2748(2) .06531(14) .7617(3) .0157(5) Uani d . 1 . . N C6 .2010(3) .09970(17) .8345(4) .0149(6) Uani d . 1 . . C N61 .1375(3) .06203(17) .9149(4) .0194(6) Uani d . 1 . . N H61 .131(4) .018(2) .897(6) .042(12) Uiso d . 1 . . H H62 .098(4) .080(3) .980(5) .036(12) Uiso d . 1 . . H 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 .0276(3) .0190(3) .0091(2) .000 .00924(17) .000 I2 .0201(2) .0194(3) .0158(2) .000 .00999(15) .000 S1 .0187(4) .0180(4) .0190(4) .0000(3) .0095(3) -.0039(3) C2 .0164(13) .0184(14) .0135(13) -.0035(11) .0062(10) -.0004(11) S3 .0234(4) .0159(4) .0092(4) -.0006(3) .0072(3) .0014(3) C4 .0129(13) .0168(15) .0098(13) .0021(11) .0017(10) .0008(11) N41 .0274(14) .0195(15) .0152(12) .0003(12) .0123(10) .0001(11) N5 .0194(10) .0170(12) .0127(11) -.0008(11) .0078(8) .0016(10) C6 .0151(13) .0174(16) .0123(13) -.0007(11) .0046(10) -.0011(12) N61 .0226(13) .0211(14) .0203(13) -.0055(12) .0150(11) -.0030(12) 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 C6 . 1.752(3) ? S1 C2 . 1.797(3) ? C2 S3 . 1.792(3) ? C2 H21 . .99 ? C2 H22 . .99 ? S3 C4 . 1.756(4) ? C4 N41 . 1.302(4) yes C4 N5 . 1.325(4) yes N41 H41 . .74(4) ? N41 H42 . .91(4) ? N5 C6 . 1.325(4) yes C6 N61 . 1.314(4) yes N61 H61 . .85(5) ? N61 H62 . .86(4) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C6 S1 C2 97.97(15) S3 C2 S1 112.62(15) S3 C2 H21 109.1 S1 C2 H21 109.1 S3 C2 H22 109.1 S1 C2 H22 109.1 H21 C2 H22 107.8 C4 S3 C2 98.54(15) N41 C4 N5 117.6(3) N41 C4 S3 114.5(2) N5 C4 S3 127.9(3) C4 N41 H41 119(3) C4 N41 H42 123(3) H41 N41 H42 117(4) C4 N5 C6 124.6(3) N61 C6 N5 117.4(3) N61 C6 S1 114.8(2) N5 C6 S1 127.7(2) C6 N61 H61 118(3) C6 N61 H62 123(3) H61 N61 H62 118(4) 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 _geom_hbond_publ_flag N41 H41 I1 5_656 .74(4) 3.13(4) 3.786(3) 150(3) yes N41 H42 I1 . .91(4) 2.68(4) 3.581(3) 169(4) yes N61 H61 I2 5_556 .85(5) 2.88(5) 3.663(3) 155(4) yes N61 H62 I2 1_556 .86(4) 2.80(4) 3.638(3) 165(4) yes 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 C6 S1 C2 S3 57.53(18) S1 C2 S3 C4 -55.58(18) C2 S3 C4 N41 -160.5(2) C2 S3 C4 N5 20.3(3) N41 C4 N5 C6 -166.4(3) S3 C4 N5 C6 12.7(4) C4 N5 C6 N61 166.9(3) C4 N5 C6 S1 -9.6(4) C2 S1 C6 N61 158.1(2) C2 S1 C6 N5 -25.3(3)