#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2005002.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_2005002 loop_ _publ_author_name 'Fern\'andez, V.' 'Doadrio, J. C.' 'Garc\'ia-Granda, S.' 'Pertierra, P.' _publ_section_title ; Bis(2-amino-4-chloromethylthiazolium) Tetrachlorocuprate at 200 and 100K and Bis(2-amino-4-methylthiazolium) Tetrachlorocuprate at 100K ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1412 _journal_page_last 1415 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(C4 H7 N2 S)2 [Cu Cl4]' _chemical_formula_moiety '2(C4 H6 Cl1 N2 S1 +),Cu Cl4 2-' _chemical_formula_sum 'C8 H12 Cl6 Cu N4 S2' _chemical_formula_weight 504.58 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 64.24(5) _cell_angle_beta 80.03(3) _cell_angle_gamma 84.72(3) _cell_formula_units_Z 2 _cell_length_a 8.168(2) _cell_length_b 10.919(4) _cell_length_c 11.437(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 15 _cell_volume 904.6(8) _computing_cell_refinement 'CRYSDA (Beurskens et al., 1992)' _computing_data_collection ' Enraf-Nonius CAD4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'DATAR (local program)' _computing_molecular_graphics 'EUCLID (Spek, 1982)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _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 0.015 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3417 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.00 _diffrn_standards_decay_% 12 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.319 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.875 _exptl_absorpt_correction_type 'refdelf (DIFABS; Walker & Stuart, 1983)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 502 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.764 _refine_diff_density_min -0.517 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_hydrogen_treatment 'see text' _refine_ls_matrix_type full _refine_ls_number_parameters 197 _refine_ls_number_reflns 3171 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.087 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_obs 0.0283 _refine_ls_shift/esd_max -0.861 _refine_ls_shift/esd_mean 0.385 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ' calc w = 1/[\s^2^(Fo^2^) + (0.0468P)^2^ + 1.5174P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0816 _refine_ls_wR_factor_obs 0.0797 _reflns_number_observed 2751 _reflns_number_total 3171 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file jz1065.cif _[local]_cod_data_source_block t9k100 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 904.7(8) _cod_database_code 2005002 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Cu 0.0171(2) 0.0093(2) 0.0139(2) 0.00125(13) -0.00583(14) -0.00321(14) Cl(1) 0.0190(4) 0.0129(3) 0.0198(4) -0.0010(3) -0.0057(3) -0.0021(3) Cl(2) 0.0217(4) 0.0106(3) 0.0258(4) 0.0008(3) -0.0093(3) -0.0059(3) Cl(3) 0.0217(4) 0.0184(4) 0.0141(3) 0.0013(3) -0.0061(3) -0.0021(3) Cl(4) 0.0233(4) 0.0118(3) 0.0266(4) 0.0045(3) -0.0124(3) -0.0053(3) Cl(5) 0.0307(4) 0.0177(4) 0.0217(4) 0.0003(3) -0.0135(3) -0.0045(3) S(1) 0.0304(4) 0.0138(4) 0.0159(4) -0.0002(3) -0.0085(3) -0.0003(3) N(11) 0.0220(13) 0.0120(12) 0.0148(13) 0.0013(10) -0.0070(10) -0.0036(10) N(12) 0.0252(14) 0.0232(14) 0.0250(14) -0.0029(11) -0.0091(12) -0.0101(12) C(14) 0.022(2) 0.031(2) 0.028(2) 0.0027(14) -0.0085(14) -0.0151(15) C(12) 0.0191(15) 0.0191(15) 0.022(2) 0.0010(12) -0.0036(12) -0.0108(13) C(13) 0.024(2) 0.0145(14) 0.0142(14) 0.0022(12) -0.0055(12) -0.0056(12) C(11) 0.026(2) 0.018(2) 0.020(2) -0.0027(13) -0.0046(13) -0.0066(13) Cl(6) 0.0428(5) 0.0348(5) 0.0260(4) 0.0105(4) -0.0166(4) -0.0168(4) S(2) 0.0249(4) 0.0146(4) 0.0241(4) 0.0098(3) -0.0096(3) -0.0091(3) N(21) 0.0185(13) 0.0152(12) 0.0194(13) 0.0041(10) -0.0070(10) -0.0089(11) N(22) 0.0216(14) 0.0215(14) 0.0267(14) 0.0022(11) -0.0074(11) -0.0150(12) C(24) 0.025(2) 0.033(2) 0.027(2) 0.0028(14) -0.0097(14) -0.018(2) C(22) 0.019(2) 0.021(2) 0.022(2) -0.0008(12) -0.0038(12) -0.0132(13) C(23) 0.0133(14) 0.0132(14) 0.0156(14) 0.0023(11) -0.0006(11) -0.0056(11) C(21) 0.025(2) 0.020(2) 0.029(2) 0.0009(13) -0.0055(13) -0.0151(14) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu 0.29680(4) 0.22133(3) 0.69792(3) 0.01370(10) Uani d . 1 Cu Cl(1) 0.05996(9) 0.10175(7) 0.77786(7) 0.0185(2) Uani d . 1 Cl Cl(2) 0.43307(9) 0.38650(7) 0.70719(7) 0.0193(2) Uani d . 1 Cl Cl(3) 0.22812(9) 0.34353(7) 0.49761(7) 0.0194(2) Uani d . 1 Cl Cl(4) 0.46890(9) 0.05073(7) 0.80152(7) 0.0208(2) Uani d . 1 Cl Cl(5) 0.09662(10) 0.23833(7) 1.23378(7) 0.0236(2) Uani d . 1 Cl S(1) -0.14561(10) 0.42449(7) 0.81731(7) 0.0216(2) Uani d . 1 S N(11) -0.0938(3) 0.2063(3) 1.0144(2) 0.0166(5) Uani d . 1 N H11 -0.095(8) 0.139(7) 1.062(7) 0.092(6) Uiso d . 1 H N(12) -0.3323(3) 0.2004(3) 0.9295(3) 0.0237(6) Uani d . 1 N H12 -0.4551(3) 0.2176(3) 0.9691(3) 0.092(6) Uiso d R 1 H H13 -0.3385(3) 0.1512(3) 0.8680(3) 0.092(6) Uiso d R 1 H C(14) 0.1725(4) 0.2382(4) 1.0758(3) 0.0258(7) Uani d . 1 C H15 0.2097(4) 0.1363(4) 1.0895(3) 0.092(6) Uiso d R 1 H H16 0.2762(4) 0.3042(4) 1.0297(3) 0.092(6) Uiso d R 1 H C(12) 0.0402(4) 0.2884(3) 0.9907(3) 0.0192(6) Uani d . 1 C C(13) -0.2007(4) 0.2611(3) 0.9290(3) 0.0175(6) Uani d . 1 C C(11) 0.0316(4) 0.4089(3) 0.8886(3) 0.0215(7) Uani d . 1 C H14 0.1078(4) 0.4972(3) 0.8406(3) 0.092(6) Uiso d R 1 H Cl(6) 0.56993(12) 0.36699(9) 0.14419(8) 0.0325(2) Uani d . 1 Cl S(2) 0.84760(10) 0.09628(8) 0.54525(8) 0.0209(2) Uani d . 1 S N(21) 0.6575(3) 0.2942(3) 0.4327(2) 0.0169(5) Uani d . 1 N H21 0.605(8) 0.365(7) 0.413(6) 0.092(6) Uiso d . 1 H N(22) 0.8189(3) 0.3358(3) 0.5621(3) 0.0212(6) Uani d . 1 N H22 0.7771(3) 0.3241(3) 0.6590(3) 0.092(6) Uiso d R 1 H H23 0.9290(3) 0.3949(3) 0.5243(3) 0.092(6) Uiso d R 1 H C(24) 0.5086(4) 0.2239(4) 0.2997(3) 0.0259(7) Uani d . 1 C H25 0.4946(4) 0.1341(4) 0.2866(3) 0.092(6) Uiso d R 1 H H26 0.3923(4) 0.2513(4) 0.3407(3) 0.092(6) Uiso d R 1 H C(22) 0.6304(4) 0.1964(3) 0.3909(3) 0.0193(6) Uani d . 1 C C(23) 0.7709(3) 0.2591(3) 0.5128(3) 0.0146(6) Uani d . 1 C C(21) 0.7231(4) 0.0847(3) 0.4413(3) 0.0226(7) Uani d . 1 C H24 0.7375(4) -0.0091(3) 0.4313(3) 0.092(6) Uiso d R 1 H 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl(3) Cu Cl(4) 140.23(5) no Cl(3) Cu Cl(2) 96.88(6) no Cl(4) Cu Cl(2) 96.02(5) no Cl(3) Cu Cl(1) 94.70(6) no Cl(4) Cu Cl(1) 97.12(5) no Cl(2) Cu Cl(1) 143.09(4) no C(13) S(1) C(11) 90.1(2) no C(13) N(11) C(12) 114.3(3) no C(12) C(14) Cl(5) 110.1(2) no C(11) C(12) N(11) 112.8(3) no C(11) C(12) C(14) 127.1(3) no N(11) C(12) C(14) 120.2(3) no N(12) C(13) N(11) 124.8(3) no N(12) C(13) S(1) 124.0(2) no N(11) C(13) S(1) 111.2(2) no C(12) C(11) S(1) 111.5(2) no C(23) S(2) C(21) 90.2(2) no C(23) N(21) C(22) 114.7(3) no C(22) C(24) Cl(6) 111.2(2) no C(21) C(22) N(21) 112.6(3) no C(21) C(22) C(24) 127.4(3) no N(21) C(22) C(24) 120.0(3) no N(22) C(23) N(21) 125.3(3) no N(22) C(23) S(2) 123.9(2) no N(21) C(23) S(2) 110.8(2) no C(22) C(21) S(2) 111.7(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu Cl(3) 2.235(2) no Cu Cl(4) 2.242(2) no Cu Cl(2) 2.24(11) no Cu Cl(1) 2.2580(10) no Cl(5) C(14) 1.806(4) no S(1) C(13) 1.728(3) no S(1) C(11) 1.742(3) no N(11) C(13) 1.328(4) no N(11) C(12) 1.393(4) no N(12) C(13) 1.312(4) no C(14) C(12) 1.486(5) no C(12) C(11) 1.333(5) no Cl(6) C(24) 1.810(4) no S(2) C(23) 1.729(3) no S(2) C(21) 1.742(3) no N(21) C(23) 1.329(4) no N(21) C(22) 1.394(4) no N(22) C(23) 1.312(4) no C(24) C(22) 1.483(4) no C(22) C(21) 1.328(5) no