#------------------------------------------------------------------------------ #$Date: 2008-04-03 13:11:48 +0300 (Thu, 03 Apr 2008) $ #$Revision: 326 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2217424.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_2217424 loop_ _publ_author_name 'Krupkov\'a, Radmila' 'F\'abry, Jan' 'C\'isa\O)tris(thiourea-\kS)zinc(II) ; _journal_coeditor_code BQ2062 _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m342 _journal_page_last m343 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac '[Zn (Se O4) (C H4 N2 S)3]' _chemical_formula_moiety 'C3 H12 N6 S3, Se1 O4, Zn1' _chemical_formula_sum 'C3 H12 N6 O4 S3 Se1 Zn1' _chemical_formula_weight 436.7 _chemical_name_systematic ; (Tetraoxidoselenato-\kO)tris(thiourea-\kS)zinc(II) ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.2045(2) _cell_length_b 7.88240(10) _cell_length_c 15.7960(2) _cell_measurement_reflns_used 14388 _cell_measurement_temperature 292 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 1395.08(4) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_data_reduction 'SCALEPACK and DENZO (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material '(JANA2000; Pet\et al., 2000)' _computing_structure_refinement '(JANA2000; Pet\et al., 2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _diffrn_ambient_temperature 292 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23449 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.16 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.833 _exptl_absorpt_correction_T_max 0.602 _exptl_absorpt_correction_T_min 0.223 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details ; (Coppens & Hamilton, 1970) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.07845 _exptl_crystal_description prism _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.36 _refine_diff_density_min -0.25 _refine_ls_abs_structure_details 'Flack (1983), 1492 Friedel pairs' _refine_ls_abs_structure_Flack -0.020(6) _refine_ls_extinction_coef 1.65(5) _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_ref 1.52 _refine_ls_hydrogen_treatment constr _refine_ls_number_constraints 48 _refine_ls_number_parameters 163 _refine_ls_number_reflns 3150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0216 _refine_ls_shift/su_max 0.0045 _refine_ls_shift/su_mean 0.0005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/[\s^2^(I)+0.0004I^2^] _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0501 _reflns_number_gt 3004 _reflns_number_total 3150 _reflns_threshold_expression I>3\s(I) _[local]_cod_data_source_file bq2062.cif loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,y,1/2+z 4 1/2+x,-y,z loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.050 -1 0 0 0.060 0 0 -1 0.175 0 1 3 0.172 0 -1 2 0.181 15 -14 0 0.125 -1 1 0 0.122 4 9 -1 0.125 1 -14 1 0.155 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 Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' Se -0.093 2.226 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' Zn 0.284 1.430 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' 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_occupancy Zn Zn1 0.43588(3) 0.34032(3) 0.42203(2) 0.02479(9) Uani d 1 Se Se1 0.37373(2) 0.15124(3) 0.247798 0.02293(7) Uani d 1 O O1 0.34191(19) 0.1846(2) 0.34926(13) 0.0363(6) Uani d 1 O O2 0.29853(18) -0.0173(2) 0.22066(12) 0.0317(6) Uani d 1 O O3 0.51627(17) 0.1169(2) 0.23987(16) 0.0372(6) Uani d 1 O O4 0.33169(19) 0.3147(2) 0.19315(15) 0.0392(6) Uani d 1 S S1 0.57849(6) 0.49589(8) 0.34906(5) 0.03060(19) Uani d 1 C C1 0.5054(2) 0.6544(2) 0.29483(16) 0.0290(8) Uani d 1 N N1 0.5667(2) 0.7339(3) 0.23498(16) 0.0401(8) Uani d 1 N N2 0.3957(2) 0.7021(3) 0.31154(18) 0.0447(9) Uani d 1 S S2 0.52313(7) 0.17226(9) 0.52667(5) 0.0327(2) Uani d 1 C C2 0.64030(18) 0.0636(3) 0.48127(17) 0.0314(8) Uani d 1 N N3 0.6501(2) 0.0405(4) 0.39895(16) 0.0468(9) Uani d 1 N N4 0.7222(2) 0.0025(3) 0.53155(17) 0.0460(9) Uani d 1 S S3 0.29592(6) 0.50137(8) 0.49583(5) 0.03039(18) Uani d 1 C C3 0.3845(2) 0.5992(3) 0.57094(15) 0.0295(7) Uani d 1 N N5 0.3360(3) 0.6436(3) 0.64329(16) 0.0453(9) Uani d 1 N N6 0.4979(2) 0.6351(3) 0.55684(18) 0.0455(9) Uani d 1 H H1n1 0.63954 0.698311 0.22123 0.0482 Uiso d 1 H H2n1 0.534956 0.822806 0.208546 0.0482 Uiso d 1 H H1n2 0.359482 0.77757 0.278428 0.0536 Uiso d 1 H H2n2 0.35742 0.658874 0.355973 0.0536 Uiso d 1 H H1n3 0.59099 0.071809 0.364689 0.0562 Uiso d 1 H H2n3 0.71576 -0.006424 0.377612 0.0562 Uiso d 1 H H1n4 0.718708 0.022995 0.58691 0.0552 Uiso d 1 H H2n4 0.781526 -0.059533 0.510475 0.0552 Uiso d 1 H H1n5 0.373839 0.715311 0.677503 0.0543 Uiso d 1 H H2n5 0.265147 0.601891 0.658106 0.0543 Uiso d 1 H H1n6 0.535457 0.589501 0.512718 0.0546 Uiso d 1 H H2n6 0.536798 0.705007 0.591462 0.0546 Uiso d 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 _atom_site_aniso_type_symbol Zn1 0.02747(16) 0.02426(15) 0.02265(16) 0.00004(11) 0.00160(12) -0.00106(11) Zn Se1 0.02532(13) 0.02427(12) 0.01920(13) -0.00028(8) 0.00161(10) 0.00140(11) Se O1 0.0414(12) 0.0444(10) 0.0231(9) -0.0183(9) 0.0063(9) -0.0069(8) O O2 0.0396(10) 0.0290(9) 0.0264(10) -0.0047(7) -0.0031(8) -0.0027(6) O O3 0.0268(9) 0.0441(10) 0.0408(12) 0.0020(8) 0.0042(10) 0.0047(10) O O4 0.0401(11) 0.0336(9) 0.0441(12) 0.0049(8) 0.0048(10) 0.0138(9) O S1 0.0252(3) 0.0343(3) 0.0323(3) 0.0001(2) 0.0004(3) 0.0102(3) S C1 0.0314(15) 0.0266(12) 0.0291(14) -0.0051(10) -0.0037(11) 0.0013(10) C N1 0.0423(14) 0.0369(12) 0.0412(15) 0.0019(10) 0.0037(11) 0.0138(11) N N2 0.0364(14) 0.0400(13) 0.0575(18) 0.0084(12) 0.0078(13) 0.0189(12) N S2 0.0354(4) 0.0400(4) 0.0227(3) 0.0119(3) 0.0055(3) 0.0041(2) S C2 0.0356(14) 0.0326(13) 0.0260(14) 0.0060(11) 0.0011(11) 0.0012(10) C N3 0.0477(16) 0.0652(17) 0.0276(13) 0.0260(14) 0.0023(11) -0.0063(12) N N4 0.0435(15) 0.0629(17) 0.0315(13) 0.0267(12) -0.0011(11) 0.0021(12) N S3 0.0228(3) 0.0406(3) 0.0279(3) 0.0011(2) -0.0020(3) -0.0110(3) S C3 0.0324(13) 0.0296(12) 0.0266(14) 0.0035(10) -0.0047(11) -0.0045(11) C N5 0.0384(15) 0.0655(17) 0.0320(14) -0.0047(12) 0.0003(12) -0.0218(12) N N6 0.0328(14) 0.0620(17) 0.0418(16) -0.0102(11) 0.0010(12) -0.0253(12) N loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zn1 O1 1.984(2) no Zn1 S1 2.3207(8) no Zn1 S2 2.3330(8) no Zn1 S3 2.3302(7) no Se1 O1 1.663(2) no Se1 O2 1.6307(18) no Se1 O3 1.6246(19) no Se1 O4 1.621(2) no S1 C1 1.722(2) no C1 N1 1.326(3) no C1 N2 1.313(4) no S2 C2 1.724(2) no C2 N3 1.317(4) no C2 N4 1.306(3) no S3 C3 1.729(2) no C3 N5 1.313(4) no C3 N6 1.321(3) no N1 H1n1 0.89 no N1 H2n1 0.89 no N2 H1n2 0.89 no N2 H2n2 0.89 no N3 H1n3 0.89 no N3 H2n3 0.89 no N4 H1n4 0.89 no N4 H2n4 0.89 no N5 H1n5 0.89 no N5 H2n5 0.89 no N6 H1n6 0.89 no N6 H2n6 0.89 no 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 Se1 Zn1 S1 88.22(2) no Se1 Zn1 S2 115.80(2) no Se1 Zn1 S3 122.45(2) no S1 Zn1 S2 111.31(3) no S1 Zn1 S3 115.09(3) no S2 Zn1 S3 103.70(3) no O1 Se1 O2 105.75(10) no O1 Se1 O3 108.14(11) no O1 Se1 O4 108.98(11) no O2 Se1 O3 110.62(10) no O2 Se1 O4 110.95(10) no O3 Se1 O4 112.15(11) no S1 C1 N1 116.84(19) no S1 C1 N2 123.6(2) no N1 C1 N2 119.5(2) no S2 C2 N3 122.86(19) no S2 C2 N4 117.7(2) no N3 C2 N4 119.4(2) no S3 C3 N5 118.6(2) no S3 C3 N6 122.2(2) no N5 C3 N6 119.2(2) no C1 N1 H1n1 120.0 no C1 N1 H2n1 120.0 no H1n1 N1 H2n1 120.0 no C1 N2 H1n2 120.0 no C1 N2 H2n2 120.0 no H1n2 N2 H2n2 120.0 no C2 N3 H1n3 120.0 no C2 N3 H2n3 120.0 no H1n3 N3 H2n3 120.0 no C2 N4 H1n4 120.0 no C2 N4 H2n4 120.0 no H1n4 N4 H2n4 120.0 no C3 N5 H1n5 120.0 no C3 N5 H2n5 120.0 no H1n5 N5 H2n5 120.0 no C3 N6 H1n6 120.0 no C3 N6 H2n6 120.0 no H1n6 N6 H2n6 120.0 no H1n1 N1 H2n1 120.0 no H1n2 N2 H2n2 120.0 no H1n3 N3 H2n3 120.0 no H1n4 N4 H2n4 120.0 no H1n5 N5 H2n5 120.0 no H1n6 N6 H2n6 120.0 no