#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006206.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_2006206 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 767 _journal_page_last 768 _publ_section_title ; 7,8-Bis(pyridinium-2-ylthio)-9:10-\mH-7,8-dicarba-nido-undecaborate Trifluoromethanesulfonate ; loop_ _publ_author_name 'Jones, Peter G.' 'Crespo, Olga' "Gimeno, M. Concepci\'on" 'Laguna, Antonio' _chemical_formula_moiety '(C12 H20 B9 N2 S2)^+^ (C F3 S O3)^-^' _chemical_formula_sum 'C13 H20 B9 F3 N2 O3 S3' _chemical_formula_iupac 'C12 H20 B9 N2 S2 1+, C F3 S O3 1-' _chemical_formula_weight 502.78 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4438(12) _cell_length_b 9.5077(10) _cell_length_c 21.497(3) _cell_angle_alpha 90 _cell_angle_beta 98.245(10) _cell_angle_gamma 90 _cell_volume 2314.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _exptl_crystal_density_diffrn 1.443 _diffrn_ambient_temperature 173(2) _refine_ls_R_factor_obs .0349 _refine_ls_wR_factor_obs .0737 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 S1 .32649(5) .06687(7) .57060(3) .0278(2) Uani d . 1 . S S2 .30971(5) .37183(7) .64500(3) .0276(2) Uani d . 1 . S B1 .5892(2) .0861(3) .73231(14) .0282(7) Uani d U 1 . B H1 .6142 .0200 .77528 .034 Uiso calc R 1 . H B2 .5175(2) .2509(3) .73621(13) .0251(6) Uani d U 1 . B H2 .4929 .2931 .78122 .030 Uiso calc R 1 . H B3 .4411(2) .1050(3) .69669(13) .0249(7) Uani d U 1 . B H3 .3644 .0536 .71466 .030 Uiso calc R 1 . H B4 .5432(2) .0098(3) .65861(13) .0265(7) Uani d U 1 . B H4 .5362 -.1072 .65307 .032 Uiso calc R 1 . H B5 .6801(3) .0965(3) .67031(14) .0297(7) Uani d U 1 . B H5 .7642 .0357 .67181 .036 Uiso calc R 1 . H B6 .6630(2) .2483(3) .71965(13) .0280(7) Uani d U 1 . B H6 .7362 .2900 .75502 .034 Uiso calc R 1 . H C7 .4405(2) .2686(3) .66137(11) .0220(5) Uani d . 1 . C C8 .4537(2) .1339(3) .61873(11) .0225(5) Uani d . 1 . C B9 .5846(3) .1236(3) .59789(14) .0279(7) Uani d U 1 . B H9 .5956(18) .076(2) .5539(10) .020(6) Uiso d . 1 . H B10 .6725(3) .2704(3) .63863(14) .0285(7) Uani d U 1 . B H10A .7509(19) .318(2) .6227(10) .021(6) Uiso d . 1 . H H10B .598(2) .269(3) .5986(12) .048(8) Uiso d . 1 . H B11 .5606(2) .3607(3) .67628(13) .0261(6) Uani d U 1 . B H11 .5553(18) .473(3) .6824(10) .021(6) Uiso d . 1 . H C11 .3172(2) .1749(3) .50422(11) .0247(6) Uani d . 1 . C C12 .3822(2) .2943(3) .49693(12) .0349(7) Uani d . 1 . C H12 .4419 .3237 .52967 .042 Uiso calc R 1 . H C13 .3604(3) .3708(3) .44223(12) .0409(7) Uani d . 1 . C H13 .4062 .4522 .43704 .049 Uiso calc R 1 . H C14 .2721(2) .3300(3) .39451(12) .0372(7) Uani d . 1 . C H14 .2559 .3829 .35679 .045 Uiso calc R 1 . H C15 .2094(2) .2122(3) .40331(11) .0316(6) Uani d . 1 . C H15 .1482 .1824 .37142 .038 Uiso calc R 1 . H N16 .2329(2) .1375(2) .45643(9) .0268(5) Uani d . 1 . N H16 .1917 .0607 .46041 .032 Uiso calc R 1 . H C21 .1988(2) .2873(3) .68046(11) .0252(6) Uani d . 1 . C C22 .2011(2) .2667(3) .74376(12) .0315(6) Uani d . 1 . C H22 .2691 .2919 .77230 .038 Uiso calc R 1 . H C23 .1040(2) .2093(3) .76582(12) .0354(7) Uani d . 1 . C H23 .1061 .1928 .80954 .042 Uiso calc R 1 . H C24 .0041(2) .1760(3) .72468(12) .0383(7) Uani d . 1 . C H24 -.0639 .1394 .73969 .046 Uiso calc R 1 . H C25 .0049(2) .1965(3) .66201(12) .0371(7) Uani d . 1 . C H25 -.0626 .1731 .63280 .045 Uiso calc R 1 . H N26 .1003(2) .2495(2) .64163(10) .0306(5) Uani d . 1 . N H26 .0992 .2603 .60089 .037 Uiso calc R 1 . H S3 -.06599(6) .18891(7) .48117(3) .0298(2) Uani d . 1 . S O1 -.0464(2) .1061(2) .42815(9) .0438(5) Uani d . 1 . O O2 .03890(14) .2547(2) .51441(8) .0351(5) Uani d . 1 . O O3 -.14225(14) .1278(2) .52197(8) .0368(5) Uani d . 1 . O C99 -.1511(3) .3387(3) .4471(2) .0481(8) Uani d . 1 . C F1 -.2539(2) .2962(2) .41577(10) .0825(7) Uani d . 1 . F F2 -.1738(2) .4276(2) .49044(10) .0757(6) Uani d . 1 . F F3 -.0947(2) .4074(2) .40733(9) .0702(6) Uani d . 1 . F 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 S1 .0286(3) .0268(4) .0246(3) -.0058(3) -.0073(3) .0015(3) S2 .0241(3) .0249(3) .0333(4) .0028(3) .0023(3) .0060(3) B1 .0262(15) .030(2) .026(2) .0022(13) -.0050(12) .0002(14) B2 .0243(14) .029(2) .0197(14) -.0008(13) -.0038(12) -.0015(13) B3 .0289(15) .022(2) .0221(15) .0021(13) -.0014(12) .0033(12) B4 .028(2) .020(2) .030(2) .0042(13) -.0022(13) -.0003(13) B5 .0260(15) .030(2) .031(2) .0002(13) -.0013(13) -.0028(14) B6 .026(2) .030(2) .026(2) -.0027(14) -.0025(12) -.0052(14) C7 .0207(12) .0235(14) .0209(13) -.0001(11) -.0002(10) .0007(11) C8 .0238(12) .0216(13) .0200(12) -.0011(11) -.0039(10) -.0016(11) B9 .028(2) .029(2) .026(2) .0013(14) .0025(13) -.0050(14) B10 .0215(15) .033(2) .030(2) -.0015(13) -.0008(13) -.0037(14) B11 .0264(15) .028(2) .0233(15) -.0046(13) .0014(12) -.0049(14) C11 .0255(12) .0251(14) .0215(13) .0039(12) -.0040(10) -.0029(11) C12 .040(2) .032(2) .0282(15) -.0065(13) -.0086(12) -.0003(13) C13 .052(2) .035(2) .032(2) -.0101(15) -.0043(13) .0081(14) C14 .047(2) .039(2) .0240(14) .0046(15) -.0023(12) .0060(13) C15 .0328(15) .037(2) .0218(14) .0067(13) -.0060(11) .0000(12) N16 .0239(11) .0275(12) .0272(12) -.0001(9) -.0027(9) -.0035(10) C21 .0219(13) .0244(15) .0287(14) .0039(11) .0015(11) .0003(12) C22 .0252(14) .040(2) .0281(14) .0036(13) -.0011(11) -.0024(13) C23 .037(2) .041(2) .0288(15) .0086(13) .0066(12) .0070(13) C24 .0246(14) .051(2) .039(2) -.0013(14) .0046(12) .0097(15) C25 .0213(13) .050(2) .038(2) -.0037(14) -.0041(12) .0059(15) N26 .0247(11) .0395(14) .0263(12) .0019(10) -.0007(9) .0052(11) S3 .0278(3) .0274(4) .0319(4) .0023(3) -.0038(3) .0037(3) O1 .0482(12) .0432(13) .0394(11) -.0007(10) .0040(9) -.0113(10) O2 .0299(10) .0428(12) .0305(10) -.0034(9) -.0027(8) .0037(9) O3 .0306(10) .0368(11) .0421(11) -.0005(9) .0017(8) .0082(9) C99 .043(2) .041(2) .055(2) .007(2) -.009(2) .017(2) F1 .0552(12) .0698(14) .107(2) -.0011(11) -.0427(12) .0334(13) F2 .090(2) .0435(12) .094(2) .0297(11) .0167(13) -.0004(12) F3 .0763(13) .0602(14) .0725(13) .0055(11) .0054(11) .0394(11) 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 S1 C11 . 1.749(2) Y S1 C8 . 1.778(2) Y S2 C21 . 1.765(3) Y S2 C7 . 1.782(2) Y B1 B4 . 1.753(4) ? B1 B3 . 1.766(4) ? B1 B2 . 1.776(4) ? B1 B6 . 1.798(4) ? B1 B5 . 1.807(4) ? B2 C7 . 1.728(3) Y B2 B6 . 1.752(4) ? B2 B11 . 1.782(4) ? B2 B3 . 1.788(4) ? B3 C8 . 1.725(4) Y B3 C7 . 1.731(4) Y B3 B4 . 1.769(4) ? B4 C8 . 1.710(4) Y B4 B5 . 1.755(4) ? B4 B9 . 1.810(4) ? B5 B10 . 1.786(4) ? B5 B9 . 1.787(4) ? B5 B6 . 1.818(4) ? B6 B11 . 1.752(4) ? B6 B10 . 1.773(4) ? C8 C7 . 1.595(3) Y C8 B9 . 1.628(4) Y C7 B11 . 1.622(4) Y B9 B10 . 1.864(4) Y B10 B11 . 1.824(4) ? C11 N16 . 1.352(3) ? C11 C12 . 1.378(4) ? C12 C13 . 1.375(3) ? C13 C14 . 1.389(4) ? C14 C15 . 1.357(4) ? C15 N16 . 1.339(3) ? C21 N26 . 1.351(3) ? C21 C22 . 1.371(3) ? C22 C23 . 1.381(3) ? C23 C24 . 1.378(3) ? C24 C25 . 1.363(3) ? C25 N26 . 1.332(3) ? S3 O1 . 1.429(2) y S3 O3 . 1.445(2) y S3 O2 . 1.448(2) y S3 C99 . 1.819(3) ? C99 F2 . 1.311(4) ? C99 F3 . 1.317(3) ? C99 F1 . 1.331(3) ?