#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006387.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2006387 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1041 _journal_page_last 1043 _publ_section_title ; A Bioctahedral Nb(IV) Cluster with Bridging Sulfides: Nb~2~(\m-S)~2~Cl~4~(thf)~4~ ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Myungok Yoon' 'Victor Young Jr' 'Gordon J. Miller' . _chemical_formula_sum 'C16 H32 Cl4 Nb2 O4 S2' _chemical_formula_weight 680.16 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5400(10) _cell_length_b 15.605(2) _cell_length_c 10.4450(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.900(10) _cell_angle_gamma 90.00 _cell_volume 2605.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.734 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0416 _refine_ls_wR_factor_obs .0972 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_disorder_group _atom_site_type_symbol Nb1 .48190(3) .44236(3) .09594(5) .0392(2) Uani d . 1 . Nb S1 .59482(10) .43875(10) .0000(2) .0521(4) Uani d . 1 . S Cl1 .39665(10) .34110(10) -.0465(2) .0613(4) Uani d . 1 . Cl Cl2 .55480(10) .50786(10) .29788(14) .0583(4) Uani d . 1 . Cl O11 .5426(2) .3167(3) .2117(4) .0583(11) Uani d . 1 . O C11 .6301(5) .3127(5) .2839(8) .084(2) Uani d . 1 . C H11A .6362(5) .3217(5) .3768(8) .080 Uiso d R 1 . H H11B .6616(5) .3557(5) .2522(8) .080 Uiso d R 1 . H C12 .6589(6) .2309(6) .2606(15) .164(6) Uani d . 1 . C H12A .6793(6) .2012(6) .3431(15) .080 Uiso d R 1 . H H12B .7037(6) .2350(6) .2178(15) .080 Uiso d R 1 . H C13 .5914(6) .1826(5) .1805(10) .105(3) Uani d . 1 . C H13A .5908(6) .1239(5) .2079(10) .080 Uiso d R 1 . H H13B .5929(6) .1845(5) .0893(10) .080 Uiso d R 1 . H C14 .5180(5) .2290(4) .1941(9) .091(3) Uani d . 1 . C H14A .4703(5) .2223(4) .1197(9) .080 Uiso d R 1 . H H14B .5036(5) .2089(4) .2723(9) .080 Uiso d R 1 . H O21 .3848(2) .4213(3) .2144(4) .0533(10) Uani d . 1 . O C21 .2962(4) .4386(6) .1696(7) .087(3) Uani d . 1 . C H21A .2712(4) .4035(6) .0944(7) .080 Uiso d R 1 . H H21B .2872(4) .4977(6) .1442(7) .080 Uiso d R 1 . H C22 .2615(5) .4208(8) .2795(9) .153(6) Uani d . 1 . C H22A .2150(5) .3825(8) .2506(9) .080 Uiso d R 1 . H H22B .2417(5) .4726(8) .3106(9) .080 Uiso d R 1 . H C23 .3206(4) .3830(6) .3804(7) .087(3) Uani d . 1 . C H23A .3057(4) .3246(6) .3917(7) .080 Uiso d R 1 . H H23B .3241(4) .4130(6) .4619(7) .080 Uiso d R 1 . H C24 .3997(5) .3847(6) .3436(7) .098(3) Uani d . 1 . C H24A .4383(5) .4203(6) .4055(7) .080 Uiso d R 1 . H H24B .4230(5) .3283(6) .3453(7) .080 Uiso d R 1 . H Nb1' .98201(3) .54478(3) .10917(5) .0395(2) Uani d . 1 . Nb S1' 1.10604(9) .54553(10) .04253(15) .0483(4) Uani d . 1 . S Cl1' 1.02107(10) .43760(10) .27691(14) .0578(4) Uani d . 1 . Cl Cl2' .93014(10) .67582(10) .0034(2) .0589(4) Uani d . 1 . Cl O1' 1.0489(3) .6348(3) .2827(4) .0578(11) Uani d . 1 . O C11' 1.0631(6) .6222(6) .4235(7) .107(3) Uani d . 1 . C H11C 1.0690(6) .5621(6) .4439(7) .080 Uiso d R 1 . H H11D 1.0176(6) .6449(6) .4543(7) .080 Uiso d R 1 . H C12' 1.1401(6) .6696(6) .4819(8) .113(3) Uani d . 1 . C H12C 1.1878(6) .6334(6) .4868(8) .080 Uiso d R 1 . H H12D 1.1415(6) .6898(6) .5693(8) .080 Uiso d R 1 . H C13' 1.1417(6) .7392(6) .3934(9) .107(3) Uani d . 1 . C H13C 1.1979(6) .7538(6) .3920(9) .080 Uiso d R 1 . H H13D 1.1162(6) .7886(6) .4216(9) .080 Uiso d R 1 . H C14' 1.0913(6) .7126(5) .2639(8) .091(3) Uani d . 1 . C H14C 1.0521(6) .7561(5) .2229(8) .080 Uiso d R 1 . H H14D 1.1279(6) .7010(5) .2079(8) .080 Uiso d R 1 . H O21' .8761(3) .5690(3) .2111(4) .0570(11) Uani d . 1 . O C21' .8462(5) .6503(5) .2453(8) .083(2) Uani d . 1 . C H21C .8089(5) .6748(5) .1681(8) .080 Uiso d R 1 . H H21D .8917(5) .6893(5) .2786(8) .080 Uiso d R 1 . H C22' .7998(5) .6313(6) .3464(8) .091(3) Uani d . 1 . C H22C .7495(5) .6646(6) .3325(8) .080 Uiso d R 1 . H H22D .8347(5) .6436(6) .4331(8) .080 Uiso d R 1 . H C23' .7784(6) .5421(5) .3309(9) .099(3) Uani d . 1 . C H23C .7189(6) .5343(5) .3050(9) .080 Uiso d R 1 . H H23D .8001(6) .5139(5) .4143(9) .080 Uiso d R 1 . H C24' .8182(5) .5045(5) .2324(7) .076(2) Uani d . 1 . C H24C .8471(5) .4522(5) .2636(7) .080 Uiso d R 1 . H H24D .7762(5) .4931(5) .1518(7) .080 Uiso d R 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 Nb1 .0427(3) .0389(3) .0365(3) -.0014(2) .0111(2) -.0010(2) S1 .0524(9) .0531(9) .0559(9) .0095(7) .0231(7) .0103(7) Cl1 .0674(10) .0533(9) .0589(9) -.0139(8) .0084(8) -.0094(8) Cl2 .0617(9) .0639(10) .0451(8) -.0043(8) .0064(7) -.0116(7) O11 .053(2) .050(2) .070(3) .003(2) .012(2) .009(2) C11 .079(5) .081(5) .079(5) .005(4) -.002(4) .015(4) C12 .064(6) .079(7) .343(19) .014(5) .045(9) .028(9) C13 .149(9) .062(5) .122(8) .005(6) .070(7) -.007(5) C14 .085(6) .050(4) .126(7) -.008(4) .007(5) .014(5) O21 .046(2) .072(3) .045(2) .004(2) .017(2) .015(2) C21 .051(4) .136(8) .075(5) .006(4) .019(4) .037(5) C22 .063(5) .293(16) .115(8) .045(8) .046(5) .101(10) C23 .077(5) .127(7) .068(5) .014(5) .038(4) .030(5) C24 .077(5) .148(8) .081(5) .040(5) .044(4) .062(6) Nb1' .0437(3) .0391(3) .0376(3) .0023(2) .0139(2) .0038(2) S1' .0420(8) .0541(9) .0499(8) -.0009(7) .0140(6) -.0012(7) Cl1' .0733(11) .0539(9) .0468(8) .0046(8) .0167(8) .0143(7) Cl2' .0697(10) .0460(8) .0633(9) .0125(8) .0210(8) .0126(7) O1' .071(3) .059(3) .044(2) -.012(2) .017(2) -.005(2) C11' .160(9) .107(7) .050(4) -.037(7) .021(5) -.012(5) C12' .134(8) .110(8) .072(6) -.014(7) -.013(6) -.018(6) C13' .117(7) .105(7) .096(7) -.055(6) .026(6) -.041(6) C14' .125(7) .065(5) .083(5) -.032(5) .028(5) -.005(4) O21' .063(3) .053(2) .064(3) .001(2) .033(2) -.001(2) C21' .092(5) .070(5) .103(6) .002(4) .052(5) -.014(4) C22' .097(6) .104(7) .092(6) -.009(5) .060(5) -.024(5) C23' .105(6) .090(6) .130(8) .010(5) .082(6) .008(5) C24' .078(5) .081(5) .079(5) -.021(4) .038(4) -.005(4) 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 Nb1 O21 . 2.289(4) yes Nb1 S1 3_665 2.324(2) yes Nb1 S1 . 2.336(2) yes Nb1 Cl1 . 2.370(2) yes Nb1 Cl2 . 2.3747(15) yes Nb1 O11 . 2.385(4) yes Nb1 Nb1 3_665 2.8685(10) yes S1 Nb1 3_665 2.324(2) no O11 C14 . 1.426(7) no O11 C11 . 1.451(7) no C11 C12 . 1.405(11) no C12 C13 . 1.426(12) no C13 C14 . 1.452(10) no O21 C24 . 1.428(7) no O21 C21 . 1.446(7) no C21 C22 . 1.435(10) no C22 C23 . 1.372(10) no C23 C24 . 1.455(9) no Nb1' O21' . 2.303(4) yes Nb1' S1' . 2.330(2) yes Nb1' S1' 3_765 2.331(2) yes Nb1' O1' . 2.335(4) yes Nb1' Cl2' . 2.377(2) yes Nb1' Cl1' . 2.3879(15) yes Nb1' Nb1' 3_765 2.8647(10) yes S1' Nb1' 3_765 2.330(2) no O1' C14' . 1.440(8) no O1' C11' . 1.442(8) no C11' C12' . 1.464(11) no C12' C13' . 1.431(11) no C13' C14' . 1.456(10) no O21' C21' . 1.440(8) no O21' C24' . 1.445(7) no C21' C22' . 1.486(9) no C22' C23' . 1.434(11) no C23' C24' . 1.478(9) no _cod_database_code 2006387