#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006257.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_2006257 loop_ _publ_author_name 'Zhu, Hong-Ping' 'Deng, Yu-Heng' 'Huang, Xiao-Ying' 'Chen, Chang-Neng' 'Liu, Qiu-Tian' _publ_section_title Tris(N,N-diethyldithiocarbamato-S,S')vanadium(III) _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 692 _journal_page_last 693 _journal_paper_doi 10.1107/S0108270196015065 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[V (C5 H10 N1 S2)3]' _chemical_formula_moiety 'C15 H30 N3 S6 V ' _chemical_formula_sum 'C15 H30 N3 S6 V' _chemical_formula_weight 495.75 _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' _atom_type_scat_source 'International Tables for X-ray Crystallography' _cell_angle_alpha 90. _cell_angle_beta 103.060(10) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 13.7310(10) _cell_length_b 10.2940(10) _cell_length_c 17.2300(10) _cell_measurement_reflns_used 23 _cell_measurement_temperature 293 _cell_measurement_theta_max 13 _cell_measurement_theta_min 12 _cell_volume 2372.4(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement MolEN _computing_structure_solution MolEN _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 4432 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0.6 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.92 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_type 'empirical via \y scans (Fair, 1990)' _exptl_crystal_colour yellow--brown _exptl_crystal_density_diffrn 1.39 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.35 _refine_diff_density_min -0.12 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.27 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 226 _refine_ls_number_reflns 2417 _refine_ls_R_factor_obs .0393 _refine_ls_shift/esd_max 0.0007 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs .0456 _reflns_number_observed 2417 _reflns_number_total 4267 _reflns_observed_criterion I>3sigma(I) _cod_data_source_file ta1121.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (30 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F)]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(F)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2372.350(10) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2006257 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_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 V .0392(3) .0329(4) .0430(3) -.0024(4) .0135(3) -.0020(4) S1 .0417(5) .0451(7) .0413(6) .0051(5) .0112(4) .0026(5) S2 .0585(6) .0528(7) .0444(6) .0145(6) .0138(5) .0092(6) S3 .0562(6) .0497(7) .0425(6) -.0188(6) .0164(5) -.0056(6) S4 .0512(6) .0517(7) .0412(6) -.0080(6) .0134(5) -.0061(6) S5 .0469(6) .0424(6) .0560(7) .0020(6) .0097(5) -.0002(6) S6 .0475(6) .0407(7) .0617(7) -.0047(6) .0070(5) -.0089(6) N1 .046(2) .041(2) .052(2) .007(2) .017(2) .001(2) N2 .049(2) .034(2) .054(2) -.003(2) .0240(10) .004(2) N3 .076(2) .030(2) .068(2) -.006(2) .023(2) -.004(2) C10 .043(2) .027(2) .051(2) .000(2) .013(2) .000(2) C11 .059(3) .063(3) .079(3) .020(3) .017(2) .014(3) C12 .115(5) .059(4) .149(6) .028(4) -.019(5) .001(4) C13 .058(2) .041(3) .064(3) .004(2) .030(2) -.003(2) C14 .106(4) .058(3) .064(3) -.007(3) .021(3) -.008(3) C20 .043(2) .028(2) .046(2) .004(2) .015(2) .004(2) C21 .061(3) .075(4) .059(3) -.003(3) .031(2) .013(3) C22 .079(3) .088(4) .078(4) .007(3) .011(3) .032(3) C23 .054(2) .046(3) .071(3) -.016(2) .028(2) -.002(2) C24 .055(3) .089(4) .097(4) .005(3) .010(3) .000(4) C30 .051(2) .039(2) .049(2) -.002(2) .024(2) -.004(2) C31 .110(4) .039(3) .091(4) -.024(3) .027(3) -.013(3) C32 .162(6) .084(5) .087(4) -.022(5) .028(4) -.020(4) C33 .101(4) .043(3) .101(4) .016(3) .021(3) .005(3) C34 .192(7) .085(5) .092(5) .008(5) .030(5) .025(4) 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_occupancy V .24208(5) .01783(7) .12547(4) .0377(2) Uani 1.0000 S1 .29648(8) -.03630(10) .00439(6) .0424(3) Uani 1.0000 S2 .38845(9) -.12120(10) .16367(7) .0515(3) Uani 1.0000 S3 .09679(8) -.12120(10) .08728(6) .0486(3) Uani 1.0000 S4 .18813(8) -.03580(10) .24693(6) .0476(3) Uani 1.0000 S5 .14682(8) .21140(10) .07229(7) .0488(3) Uani 1.0000 S6 .34206(8) .20610(10) .17896(7) .0508(4) Uani 1.0000 N1 .4673(2) -.1714(3) .0377(2) .0450(10) Uani 1.0000 N2 .0300(2) -.1965(3) .2143(2) .0440(10) Uani 1.0000 N3 .2481(3) .4285(3) .1249(2) .0570(10) Uani 1.0000 C10 .3940(3) -.1181(4) .0648(2) .0400(10) Uani 1.0000 C11 .5582(3) -.2242(5) .0926(3) .067(2) Uani 1.0000 C12 .5753(5) -.3620(6) .0846(5) .115(3) Uani 1.0000 C13 .4661(3) -.1725(4) -.0476(3) .0520(10) Uani 1.0000 C14 .4074(4) -.2838(6) -.0916(3) .076(2) Uani 1.0000 C20 .0961(3) -.1274(4) .1867(2) .0380(10) Uani 1.0000 C21 .0329(3) -.2053(5) .2997(3) .062(2) Uani 1.0000 C22 .0852(4) -.3226(6) .3388(3) .083(2) Uani 1.0000 C23 -.0497(3) -.2707(5) .1620(3) .0550(10) Uani 1.0000 C24 -.1483(4) -.2045(6) .1478(4) .081(2) Uani 1.0000 C30 .2461(3) .2996(4) .1256(3) .0440(10) Uani 1.0000 C31 .3366(4) .5006(5) .1679(3) .079(2) Uani 1.0000 C32 .3265(5) .5463(7) .2465(4) .111(3) Uani 1.0000 C33 .1642(4) .5060(5) .0813(4) .082(2) Uani 1.0000 C34 .1746(6) .5481(7) .0006(4) .123(3) Uani 1.0000 H111 .55242 -.20839 .14566 .08673 Uiso 1.0000 H112 .6145 -.17878 .08287 .08673 Uiso 1.0000 H121 .63455 -.38696 .12168 .14965 Uiso 1.0000 H122 .58224 -.37988 .03201 .14965 Uiso 1.0000 H123 .52016 -.40949 .0948 .14965 Uiso 1.0000 H131 .53304 -.17851 -.05357 .06706 Uiso 1.0000 H132 .43727 -.09349 -.07038 .06706 Uiso 1.0000 H141 .40923 -.27943 -.14633 .0985 Uiso 1.0000 H142 .33998 -.27857 -.08657 .0985 Uiso 1.0000 H143 .43574 -.36359 -.06975 .0985 Uiso 1.0000 H211 -.03388 -.20653 .30639 .08095 Uiso 1.0000 H212 .06633 -.13066 .32515 .08095 Uiso 1.0000 H221 .08428 -.3221 .39374 .10747 Uiso 1.0000 H222 .15243 -.32248 .33316 .10747 Uiso 1.0000 H223 .05222 -.39835 .3144 .10747 Uiso 1.0000 H231 -.05534 -.35273 .18579 .07172 Uiso 1.0000 H232 -.03225 -.283 .11217 .07172 Uiso 1.0000 H241 -.19712 -.25635 .11363 .1059 Uiso 1.0000 H242 -.14384 -.12248 .12347 .1059 Uiso 1.0000 H243 -.16693 -.19221 .1971 .1059 Uiso 1.0000 H311 .34622 .57372 .13682 .10304 Uiso 1.0000 H312 .39324 .44519 .17492 .10304 Uiso 1.0000 H321 .38526 .59207 .27169 .14396 Uiso 1.0000 H322 .31741 .47398 .27833 .14396 Uiso 1.0000 H323 .27039 .60251 .24023 .14396 Uiso 1.0000 H331 .15856 .58139 .11181 .10681 Uiso 1.0000 H332 .10496 .45561 .07518 .10681 Uiso 1.0000 H341 .11777 .59778 -.02421 .16031 Uiso 1.0000 H342 .17955 .47378 -.03095 .16031 Uiso 1.0000 H343 .23315 .59957 .00568 .16031 Uiso 1.0000 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 S1 V S2 72.69(4) yes S1 V S3 91.44(5) yes S1 V S4 153.65(5) yes S1 V S5 96.16(5) yes S1 V S6 104.54(5) yes S2 V S3 107.75(5) yes S2 V S4 91.55(5) yes S2 V S5 156.89(5) yes S2 V S6 90.30(4) yes S3 V S4 73.01(4) yes S3 V S5 92.39(4) yes S3 V S6 158.94(5) yes S4 V S5 105.43(5) yes S4 V S6 96.33(5) yes S5 V S6 72.61(4) yes V S1 C10 86.6(2) yes V S2 C10 86.50(10) yes V S3 C20 86.60(10) yes V S4 C20 86.0(2) yes V S5 C30 86.40(10) yes V S6 C30 86.80(10) yes S1 C10 S2 113.9(2) yes S1 C10 N1 122.8(3) yes S2 C10 N1 123.3(3) yes S3 C20 S4 114.4(2) yes S3 C20 N2 122.5(3) yes S4 C20 N2 123.1(3) yes S5 C30 S6 114.1(2) yes S5 C30 N3 122.6(3) yes S6 C30 N3 123.3(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V S1 . . 2.4340(10) yes V S2 . . 2.4340(10) yes V S3 . . 2.4230(10) yes V S4 . . 2.4360(10) yes V S5 . . 2.4450(10) yes V S6 . . 2.4330(10) yes S1 C10 . . 1.719(4) yes S2 C10 . . 1.722(4) yes S3 C20 . . 1.716(4) yes S4 C20 . . 1.723(4) yes S5 C30 . . 1.721(4) yes S6 C30 . . 1.721(4) yes N1 C10 . . 1.321(6) yes N2 C20 . . 1.324(6) yes N3 C30 . . 1.327(6) yes