#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/60/2006021.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_2006021 loop_ _publ_author_name 'Cox, O.' 'Cordero, M.' 'Pi\~neiro, S.' 'Huang, S. D.' _publ_contact_author ; Songping D. Huang Department of Chemistry University of Puerto Rico PO Box 23346 San Juan PR 00931 USA ; _publ_section_title ; Bis[(E)-2-(2,4-dichloro-5-nitrostyryl)-1,3-benzothiazole] Hydrate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 310 _journal_page_last 311 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '2C15 H8 Cl2 N2 O2 S,H2 O' _chemical_formula_moiety '2(C15 H8 Cl2 N2 O2 S),H2 O' _chemical_formula_sum 'C30 H18 Cl4 N4 O5 S2' _chemical_formula_weight 720.43 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 93.73(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.081(2) _cell_length_b 13.473(2) _cell_length_c 17.148(3) _cell_measurement_reflns_used 15 _cell_measurement_temperature 295.2 _cell_measurement_theta_max 22.0 _cell_measurement_theta_min 20.0 _cell_volume 3015.8(8) _computing_cell_refinement CAD-4-PC _computing_data_collection 'CAD-4-PC (Molecular Structure Corporation, 1995)' _computing_data_reduction TEXSAN _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 295.2 _diffrn_measurement_device CAD4 _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 6665 _diffrn_reflns_theta_max 26.29 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 3.11 _diffrn_standards_interval_count '120 min' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 1464.00 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.65 _refine_diff_density_min -0.70 _refine_ls_extinction_coef '2.676(2) \\times 10^-7^' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_goodness_of_fit_obs 2.161 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 407 _refine_ls_number_reflns 3476 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0706 _refine_ls_shift/esd_max 0.0004 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/\s^2^(F~o~) = [\s^2^(F~o~) + 0.0009/4F~o~^2^]^-1^' _refine_ls_wR_factor_obs 0.0936 _reflns_number_observed 3476 _reflns_number_total 6494 _reflns_observed_criterion '[I>3\s(I)]' _[local]_cod_data_source_file ta1116.cif _[local]_cod_data_source_block C30H18O5Cl4N4S2 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_chemical_formula_sum_orig 'C30 H18 Cl4 N4 O5 S2 ' _cod_original_cell_volume 3015.8(7) _cod_database_code 2006021 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' 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 Cl(1a) 0.6152(1) 0.4125(1) 0.2542(1) 0.0627(6) Uij Cl(1b) 0.9534(1) 0.4130(1) 0.3097(1) 0.0613(6) Uij Cl(2a) 0.8645(1) 0.1183(1) 0.1869(1) 0.0573(5) Uij Cl(2b) 1.2133(1) 0.1255(1) 0.2529(1) 0.0621(6) Uij S(1a) 0.3004(1) 0.3670(1) 0.4077(1) 0.0460(5) Uij S(1b) 0.6778(1) 0.3825(1) 0.5042(1) 0.0490(5) Uij O(1a) 0.8156(4) -0.0318(4) 0.3035(3) 0.075(2) Uij O(1b) 1.1837(4) -0.0228(4) 0.3652(4) 0.092(2) Uij O(2a) 0.6584(4) -0.0718(3) 0.2761(3) 0.071(2) Uij O(2b) 1.0448(5) -0.0469(5) 0.4143(5) 0.129(3) Uij O(3) 0.6550(5) -0.0015(4) 0.4610(4) 0.095(2) Uij N(1a) 0.2886(3) 0.1898(3) 0.4640(3) 0.040(1) Uij N(1b) 0.6391(4) 0.1976(3) 0.5308(3) 0.042(1) Uij N(2a) 0.7273(4) -0.0113(4) 0.2864(3) 0.050(2) Uij N(2b) 1.1011(4) 0.0051(4) 0.3819(3) 0.051(2) Uij C(1a) 0.3427(4) 0.2437(4) 0.4196(3) 0.037(2) Uij C(1b) 0.7042(4) 0.2547(4) 0.4986(4) 0.040(2) Uij C(2a) 0.2058(4) 0.3430(4) 0.4706(3) 0.039(2) Uij C(2b) 0.5726(4) 0.3552(4) 0.5560(4) 0.040(2) Uij C(3a) 0.1319(5) 0.4080(5) 0.4978(4) 0.051(2) Uij C(3b) 0.5005(5) 0.4198(4) 0.5858(4) 0.052(2) Uij C(4a) 0.0649(5) 0.3696(5) 0.5483(4) 0.053(2) Uij C(4b) 0.4196(5) 0.3781(5) 0.6226(4) 0.050(2) Uij C(5a) 0.0689(5) 0.2717(5) 0.5721(3) 0.047(2) Uij C(5b) 0.4105(5) 0.2755(4) 0.6299(4) 0.047(2) Uij C(6a) 0.1413(4) 0.2082(4) 0.5456(3) 0.042(2) Uij C(6b) 0.4811(4) 0.2116(4) 0.6015(4) 0.043(2) Uij C(7a) 0.2108(4) 0.2437(4) 0.4947(3) 0.035(2) Uij C(7b) 0.5622(4) 0.2520(4) 0.5627(3) 0.036(2) Uij C(8a) 0.4303(4) 0.2065(4) 0.3828(4) 0.042(2) Uij C(8b) 0.7902(4) 0.2167(4) 0.4596(4) 0.042(2) Uij C(9a) 0.4901(4) 0.2608(4) 0.3386(3) 0.040(2) Uij C(9b) 0.8551(4) 0.2732(4) 0.4216(3) 0.040(2) Uij C(10a) 0.5819(4) 0.2246(4) 0.3033(3) 0.035(2) Uij C(10b) 0.9433(4) 0.2353(4) 0.3817(3) 0.034(2) Uij C(11a) 0.6444(4) 0.2878(4) 0.2626(4) 0.039(2) Uij C(11b) 0.9944(4) 0.2935(4) 0.3304(3) 0.034(2) Uij C(12a) 0.7309(4) 0.2556(4) 0.2263(3) 0.041(2) Uij C(12b) 1.0773(4) 0.2593(4) 0.2913(3) 0.039(2) Uij C(13a) 0.7598(4) 0.1576(4) 0.2336(3) 0.038(2) Uij C(13b) 1.1140(4) 0.1631(4) 0.3059(3) 0.040(2) Uij C(14a) 0.6997(4) 0.0930(4) 0.2759(3) 0.037(2) Uij C(14b) 1.0643(4) 0.1051(4) 0.3594(3) 0.037(2) Uij C(15a) 0.6132(4) 0.1251(4) 0.3083(3) 0.040(2) Uij C(15b) 0.9816(4) 0.1397(4) 0.3955(3) 0.038(2) Uij H(1a) 0.1153 0.4786 0.4638 0.0758 Uij H(1b) 0.5076 0.4913 0.5808 0.0627 Uij H(2a) 0.0092 0.4113 0.5691 0.0758 Uij H(2b) 0.3463 0.4284 0.6088 0.0758 Uij H(3a) 0.0264 0.2535 0.6152 0.0758 Uij H(3b) 0.3320 0.2502 0.6461 0.0758 Uij H(4a) 0.1572 0.1452 0.5772 0.0758 Uij H(4b) 0.4544 0.1329 0.5772 0.0758 Uij H(5a) 0.4697 0.1454 0.4171 0.0758 Uij H(5b) 0.8274 0.1550 0.4983 0.0758 Uij H(6a) 0.4508 0.3223 0.3097 0.0758 Uij H(6b) 0.8231 0.3271 0.3869 0.0758 Uij H(7a) 0.7483 0.3029 0.1714 0.0758 Uij H(7b) 1.1037 0.2987 0.2404 0.0758 Uij H(8a) 0.5798 0.0854 0.3521 0.0758 Uij H(8b) 0.9611 0.1031 0.4452 0.0758 Uij H(9) 0.5990 0.0113 0.4621 0.0758 Uij H(10) 0.7020 0.0087 0.4609 0.0758 Uij loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl(1a) ? C(11a) ? 1.727(6) no Cl(1b) ? C(11b) ? 1.727(6) no Cl(2a) ? C(13a) ? 1.715(5) no Cl(2b) ? C(13b) ? 1.710(5) no S(1a) ? C(1a) ? 1.759(6) no S(1a) ? C(2a) ? 1.725(6) no S(1b) ? C(1b) ? 1.760(5) no S(1b) ? C(2b) ? 1.726(5) no O(1a) ? N(2a) ? 1.205(6) no O(1b) ? N(2b) ? 1.197(6) no O(2a) ? N(2a) ? 1.220(6) no O(2b) ? N(2b) ? 1.181(7) no N(1a) ? C(1a) ? 1.296(7) no N(1a) ? C(7a) ? 1.383(7) no N(1b) ? C(1b) ? 1.299(7) no N(1b) ? C(7b) ? 1.385(7) no N(2a) ? C(14a) ? 1.460(7) no N(2b) ? C(14b) ? 1.474(7) no C(1a) ? C(8a) ? 1.434(7) no C(1b) ? C(8b) ? 1.439(7) no C(2a) ? C(3a) ? 1.406(8) no C(2a) ? C(7a) ? 1.399(8) no C(2b) ? C(3b) ? 1.404(7) no C(2b) ? C(7b) ? 1.403(7) no C(3a) ? C(4a) ? 1.372(9) no C(3b) ? C(4b) ? 1.386(8) no C(4a) ? C(5a) ? 1.382(9) no C(4b) ? C(5b) ? 1.394(8) no C(5a) ? C(6a) ? 1.375(8) no C(5b) ? C(6b) ? 1.375(8) no C(6a) ? C(7a) ? 1.387(7) no C(6b) ? C(7b) ? 1.399(7) no C(8a) ? C(9a) ? 1.342(8) no C(8b) ? C(9b) ? 1.340(8) no C(9a) ? C(10a) ? 1.463(7) no C(9b) ? C(10b) ? 1.471(7) no C(10a) ? C(11a) ? 1.398(7) no C(10a) ? C(15a) ? 1.403(8) no C(10b) ? C(11b) ? 1.383(7) no C(10b) ? C(15b) ? 1.398(7) no C(11a) ? C(12a) ? 1.396(7) no C(11b) ? C(12b) ? 1.389(8) no C(12a) ? C(13a) ? 1.377(8) no C(12b) ? C(13b) ? 1.399(8) no C(13a) ? C(14a) ? 1.406(8) no C(13b) ? C(14b) ? 1.398(8) no C(14a) ? C(15a) ? 1.363(7) no C(14b) ? C(15b) ? 1.363(7) no loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cl(1a) 0.058(1) 0.0012(7) 0.0279(10) 0.0328(8) 0.0047(9) 0.100(1) Cl(1b) 0.066(1) 0.0044(8) 0.0219(10) 0.0337(8) 0.0137(9) 0.086(1) Cl(2a) 0.0401(9) 0.0031(8) 0.0314(8) 0.066(1) -0.0079(9) 0.069(1) Cl(2b) 0.0483(10) 0.0044(8) 0.0368(9) 0.068(1) -0.0059(10) 0.075(1) S(1a) 0.0361(8) 0.0026(7) 0.0243(8) 0.0357(8) 0.0073(8) 0.069(1) S(1b) 0.0391(9) -0.0006(7) 0.0301(8) 0.0294(8) -0.0006(8) 0.082(1) O(1a) 0.061(3) 0.024(3) 0.012(3) 0.059(3) 0.018(3) 0.106(5) O(1b) 0.075(4) 0.038(3) 0.049(4) 0.069(4) 0.018(3) 0.137(6) O(2a) 0.078(4) -0.011(3) 0.036(3) 0.036(3) -0.011(3) 0.103(4) O(2b) 0.118(5) 0.050(4) 0.105(5) 0.068(4) 0.075(5) 0.214(8) O(3) 0.143(5) 0.007(3) 0.010(4) 0.047(3) 0.003(3) 0.097(5) N(1a) 0.033(3) 0.003(2) 0.013(2) 0.034(3) 0.001(2) 0.054(3) N(1b) 0.037(3) 0.005(2) 0.018(2) 0.028(3) -0.001(2) 0.062(3) N(2a) 0.050(3) 0.011(3) 0.024(3) 0.040(3) -0.001(3) 0.062(4) N(2b) 0.049(3) 0.009(3) 0.020(3) 0.044(3) 0.003(3) 0.063(4) C(1a) 0.029(3) 0.003(2) 0.012(3) 0.036(3) -0.001(3) 0.048(4) C(1b) 0.030(3) 0.004(2) 0.015(3) 0.029(3) 0.000(3) 0.063(4) C(2a) 0.032(3) 0.000(2) 0.013(3) 0.035(3) -0.002(3) 0.051(4) C(2b) 0.029(3) 0.001(2) 0.023(3) 0.028(3) -0.002(3) 0.066(4) C(3a) 0.037(3) 0.007(3) 0.015(3) 0.042(4) -0.003(3) 0.074(5) C(3b) 0.049(4) -0.003(3) 0.028(3) 0.030(3) -0.008(3) 0.081(5) C(4a) 0.040(4) 0.010(3) 0.023(3) 0.057(4) -0.009(4) 0.064(4) C(4b) 0.036(3) 0.004(3) 0.022(3) 0.051(4) -0.005(4) 0.067(4) C(5a) 0.041(4) -0.002(3) 0.018(3) 0.062(4) -0.004(3) 0.039(4) C(5b) 0.040(3) -0.011(3) 0.021(3) 0.044(4) -0.008(3) 0.058(4) C(6a) 0.040(3) 0.000(3) 0.011(3) 0.045(3) 0.006(3) 0.044(4) C(6b) 0.038(3) -0.007(3) 0.015(3) 0.037(3) -0.002(3) 0.056(4) C(7a) 0.024(3) 0.000(2) 0.011(2) 0.039(3) -0.002(3) 0.042(3) C(7b) 0.030(3) 0.002(2) 0.010(3) 0.033(3) -0.005(3) 0.044(4) C(8a) 0.035(3) 0.009(3) 0.012(3) 0.043(3) 0.001(3) 0.049(4) C(8b) 0.031(3) 0.006(3) 0.012(3) 0.040(3) 0.001(3) 0.054(4) C(9a) 0.031(3) 0.003(3) 0.017(3) 0.043(3) -0.002(3) 0.050(4) C(9b) 0.032(3) 0.007(3) 0.009(3) 0.041(3) 0.005(3) 0.047(4) C(10a) 0.028(3) 0.002(2) 0.012(3) 0.035(3) 0.000(3) 0.044(3) C(10b) 0.027(3) 0.002(2) 0.005(3) 0.033(3) -0.002(3) 0.042(3) C(11a) 0.031(3) -0.002(2) 0.012(3) 0.030(3) 0.003(3) 0.056(4) C(11b) 0.032(3) -0.004(2) -0.002(3) 0.034(3) 0.002(3) 0.037(3) C(12a) 0.032(3) -0.003(3) 0.013(3) 0.044(4) -0.001(3) 0.047(4) C(12b) 0.032(3) -0.009(3) 0.008(3) 0.040(3) -0.002(3) 0.046(4) C(13a) 0.028(3) -0.001(2) 0.016(3) 0.041(3) -0.006(3) 0.047(4) C(13b) 0.028(3) -0.002(3) 0.014(3) 0.042(3) -0.004(3) 0.050(4) C(14a) 0.034(3) 0.001(2) 0.013(3) 0.033(3) 0.000(3) 0.046(4) C(14b) 0.032(3) 0.003(2) 0.009(3) 0.039(3) -0.001(3) 0.041(3) C(15a) 0.035(3) 0.001(3) 0.020(3) 0.037(3) 0.004(3) 0.050(4) C(15b) 0.034(3) 0.005(3) 0.012(3) 0.035(3) 0.004(3) 0.047(4) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' O 0.011 0.006 'International Tables' N 0.006 0.003 'International Tables' S 0.125 0.123 'International Tables' Cl 0.148 0.159 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 2 -2 5 -5 0 -2 -6 -3 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 C(1a) S(1a) C(2a) 89.1(3) no C(1b) S(1b) C(2b) 89.2(3) no C(1a) N(1a) C(7a) 111.9(5) no C(1b) N(1b) C(7b) 111.6(5) no O(1a) N(2a) O(2a) 124.8(6) no O(1a) N(2a) C(14a) 118.4(5) no O(2a) N(2a) C(14a) 116.8(5) no O(1b) N(2b) O(2b) 121.8(6) no O(1b) N(2b) C(14b) 120.5(5) no O(2b) N(2b) C(14b) 117.6(5) no S(1a) C(1a) N(1a) 114.7(4) no S(1a) C(1a) C(8a) 122.3(4) no N(1a) C(1a) C(8a) 123.0(5) no S(1b) C(1b) N(1b) 114.8(4) no S(1b) C(1b) C(8b) 122.4(4) no N(1b) C(1b) C(8b) 122.7(5) no S(1a) C(2a) C(3a) 128.8(5) no S(1a) C(2a) C(7a) 110.0(4) no C(3a) C(2a) C(7a) 121.2(5) no S(1b) C(2b) C(3b) 129.2(4) no S(1b) C(2b) C(7b) 109.8(4) no C(3b) C(2b) C(7b) 121.0(5) no C(2a) C(3a) C(4a) 117.1(6) no C(2b) C(3b) C(4b) 117.8(5) no C(3a) C(4a) C(5a) 122.2(6) no C(3b) C(4b) C(5b) 121.0(5) no C(4a) C(5a) C(6a) 120.7(5) no C(4b) C(5b) C(6b) 121.7(5) no C(5a) C(6a) C(7a) 119.1(6) no C(5b) C(6b) C(7b) 118.3(5) no N(1a) C(7a) C(2a) 114.3(5) no N(1a) C(7a) C(6a) 126.0(5) no C(2a) C(7a) C(6a) 119.7(5) no N(1b) C(7b) C(2b) 114.6(5) no N(1b) C(7b) C(6b) 125.1(5) no C(2b) C(7b) C(6b) 120.3(5) no C(1a) C(8a) C(9a) 124.8(5) no C(1b) C(8b) C(9b) 124.2(5) no C(8a) C(9a) C(10a) 125.2(5) no C(8b) C(9b) C(10b) 124.8(5) no C(9a) C(10a) C(11a) 121.7(5) no C(9a) C(10a) C(15a) 122.5(5) no C(11a) C(10a) C(15a) 115.8(5) no C(9b) C(10b) C(11b) 121.8(5) no C(9b) C(10b) C(15b) 121.6(5) no C(11b) C(10b) C(15b) 116.6(5) no Cl(1a) C(11a) C(10a) 120.1(4) no Cl(1a) C(11a) C(12a) 116.5(4) no C(10a) C(11a) C(12a) 123.4(5) no Cl(1b) C(11b) C(10b) 120.2(4) no Cl(1b) C(11b) C(12b) 116.9(4) no C(10b) C(11b) C(12b) 122.9(5) no C(11a) C(12a) C(13a) 118.9(5) no C(11b) C(12b) C(13b) 119.4(5) no Cl(2a) C(13a) C(12a) 118.5(4) no Cl(2a) C(13a) C(14a) 122.7(4) no C(12a) C(13a) C(14a) 118.7(5) no Cl(2b) C(13b) C(12b) 116.3(4) no Cl(2b) C(13b) C(14b) 125.8(5) no C(12b) C(13b) C(14b) 117.8(5) no N(2a) C(14a) C(13a) 121.1(5) no N(2a) C(14a) C(15a) 117.4(5) no C(13a) C(14a) C(15a) 121.4(5) no N(2b) C(14b) C(13b) 121.7(5) no N(2b) C(14b) C(15b) 116.6(5) no C(13b) C(14b) C(15b) 121.6(5) no C(10a) C(15a) C(14a) 121.6(5) no C(10b) C(15b) C(14b) 121.6(5) no