#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011917.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_2011917 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 366 _journal_page_last 367 _publ_section_title ; {N-[2-(\h^5^-cyclopentadienyl)ethyl]-4-toluenesulfonamido-N,O} (tetrahydrofuran-O)bis(trifluoromethanesulfonato-O)titanium(II) ; _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 'Lensink, Cornelis' 'Gainsford, Graeme J.' 'Baxter, Neville I.' _chemical_formula_moiety 'C20 H23 F6 N O9 S3 Ti' _chemical_formula_sum 'C20 H23 F6 N O9 S3 Ti' _chemical_formula_iupac '[Ti (C F3 O3 S)2 (C4 H8 O) (C14 H15 N O2 S)]' _chemical_formula_weight 679.47 _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 20.674(7) _cell_length_b 7.653(2) _cell_length_c 19.211(6) _cell_angle_alpha 90 _cell_angle_beta 116.939(4) _cell_angle_gamma 90 _cell_volume 2709.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _exptl_crystal_density_diffrn 1.666 _diffrn_ambient_temperature 168(2) loop_ _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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ti1 .19750(3) .91652(7) .26340(3) .02001(16) Uani d . 1 . . Ti S1 .27002(4) 1.12940(11) .20217(5) .0224(2) Uani d . 1 . . S S2 .04384(4) 1.17257(11) .16909(5) .0241(2) Uani d . 1 . . S S3 .32987(5) .81034(14) .44120(5) .0389(3) Uani d . 1 . . S O1 .23536(12) 1.2434(3) .13644(13) .0301(5) Uani d . 1 . . O O2 .26288(11) 1.1652(3) .27405(12) .0254(5) Uani d . 1 . . O O3 .11895(11) 1.1037(3) .20165(13) .0267(5) Uani d . 1 . . O O4 .03892(13) 1.3234(3) .21030(14) .0366(6) Uani d . 1 . . O O5 -.01109(12) 1.0415(3) .14941(14) .0361(6) Uani d . 1 . . O O6 .29812(12) .8581(3) .35731(13) .0292(5) Uani d . 1 . . O O7 .36277(18) .9541(4) .49175(16) .0708(10) Uani d . 1 . . O O8 .28477(17) .6958(5) .45916(18) .0731(10) Uani d . 1 . . O O9 .18276(12) 1.0355(3) .35697(12) .0265(5) Uani d . 1 . . O F1 .04941(12) 1.1340(3) .03568(12) .0435(6) Uani d . 1 . . F F2 .07159(12) 1.3933(3) .08131(12) .0414(5) Uani d . 1 . . F F3 -.03809(11) 1.2956(3) .03017(12) .0526(6) Uani d . 1 . . F F4 .45266(16) .7602(5) .43495(19) .0974(11) Uani d . 1 . . F F5 .38306(18) .5406(4) .40171(19) .1015(12) Uani d . 1 . . F F6 .44204(15) .6124(4) .52315(15) .0757(9) Uani d . 1 . . F N1 .23695(14) .9366(3) .18636(14) .0223(6) Uani d . 1 . . N C1 .36338(17) 1.1208(4) .22727(19) .0247(7) Uani d . 1 . . C C2 .38450(19) 1.1408(5) .1678(2) .0354(9) Uani d . 1 . . C H2 .3494 1.1587 .1152 .042 Uiso calc R 1 . . H C3 .4575(2) 1.1340(5) .1875(2) .0408(9) Uani d . 1 . . C H3 .4722 1.1455 .1475 .049 Uiso calc R 1 . . H C4 .50998(19) 1.1109(5) .2640(2) .0369(9) Uani d . 1 . . C C5 .4875(2) 1.0887(5) .3219(2) .0393(9) Uani d . 1 . . C H5 .5227 1.0695 .3744 .047 Uiso calc R 1 . . H C6 .41441(18) 1.0944(5) .3039(2) .0347(9) Uani d . 1 . . C H6 .3997 1.0804 .3438 .042 Uiso calc R 1 . . H C7 .5899(2) 1.1106(6) .2851(3) .0541(12) Uani d . 1 . . C H7A .5990 1.0269 .2519 .081 Uiso calc R 1 . . H H7B .6181 1.0771 .3400 .081 Uiso calc R 1 . . H H7C .6045 1.2278 .2771 .081 Uiso calc R 1 . . H C8 .22006(18) .8411(4) .11286(19) .0277(8) Uani d . 1 . . C H8A .2612 .8471 .0999 .033 Uiso calc R 1 . . H H8B .1762 .8897 .0688 .033 Uiso calc R 1 . . H C9 .20710(19) .6542(4) .1306(2) .0320(8) Uani d . 1 . . C H9A .1755 .5924 .0816 .038 Uiso calc R 1 . . H H9B .2538 .5906 .1565 .038 Uiso calc R 1 . . H C10 .17103(18) .6613(4) .18390(19) .0265(8) Uani d . 1 . . C C11 .10399(17) .7457(4) .1670(2) .0262(7) Uani d . 1 . . C H11 .0718 .7972 .1186 .031 Uiso calc R 1 . . H C12 .09401(19) .7392(4) .2347(2) .0296(8) Uani d . 1 . . C H12 .0534 .7843 .2395 .036 Uiso calc R 1 . . H C13 .15406(19) .6552(4) .2943(2) .0318(8) Uani d . 1 . . C H13 .1618 .6352 .3463 .038 Uiso calc R 1 . . H C14 .20110(19) .6059(4) .2619(2) .0306(8) Uani d . 1 . . C H14 .2457 .5451 .2888 .037 Uiso calc R 1 . . H C15 .2136(2) 1.2082(5) .3870(2) .0373(9) Uani d . 1 . . C H15A .1922 1.2981 .3457 .045 Uiso calc R 1 . . H H15B .2669 1.2074 .4064 .045 Uiso calc R 1 . . H C16 .1946(3) 1.2434(6) .4522(3) .0688(16) Uani d . 1 . . C H16A .1904 1.3705 .4590 .083 Uiso calc R 1 . . H H16B .2315 1.1936 .5020 .083 Uiso calc R 1 . . H C17 .1229(2) 1.1542(6) .4263(3) .0529(12) Uani d . 1 . . C H17A .1141 1.1246 .4715 .064 Uiso calc R 1 . . H H17B .0827 1.2284 .3896 .064 Uiso calc R 1 . . H C18 .1305(2) .9940(6) .3871(2) .0486(11) Uani d . 1 . . C H18A .1486 .8958 .4246 .058 Uiso calc R 1 . . H H18B .0831 .9604 .3438 .058 Uiso calc R 1 . . H C19 .03139(18) 1.2536(4) .07416(19) .0275(8) Uani d . 1 . . C C20 .4062(3) .6738(7) .4509(3) .0552(12) Uani d . 1 . . C 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 Ti1 .0201(3) .0217(3) .0217(3) -.0002(2) .0125(2) .0000(2) S1 .0216(4) .0247(5) .0254(4) -.0008(3) .0147(3) .0003(3) S2 .0213(4) .0309(5) .0244(4) .0022(3) .0142(3) .0027(4) S3 .0332(5) .0559(7) .0276(5) .0131(5) .0136(4) .0090(4) O1 .0306(13) .0315(14) .0330(13) .0032(11) .0185(11) .0078(11) O2 .0279(12) .0286(13) .0261(12) -.0031(10) .0177(10) -.0026(10) O3 .0206(11) .0285(13) .0322(13) .0033(10) .0130(10) .0048(10) O4 .0392(15) .0411(16) .0390(14) .0080(12) .0260(12) -.0040(12) O5 .0236(13) .0388(15) .0476(16) -.0039(11) .0175(12) .0077(12) O6 .0245(12) .0336(14) .0308(13) .0025(10) .0137(10) .0052(11) O7 .066(2) .080(2) .0367(17) .0223(18) -.0021(15) -.0153(16) O8 .0523(19) .113(3) .061(2) .0055(19) .0321(16) .046(2) O9 .0322(13) .0288(13) .0280(12) -.0041(10) .0219(11) -.0035(10) F1 .0644(15) .0416(13) .0377(12) -.0106(11) .0347(11) -.0116(10) F2 .0586(14) .0325(12) .0411(12) -.0152(11) .0295(11) -.0010(10) F3 .0349(13) .0757(17) .0368(12) .0096(12) .0072(10) .0185(12) F4 .0544(18) .145(3) .109(2) .0409(19) .0513(18) .053(2) F5 .104(3) .087(2) .087(2) .055(2) .0190(19) -.0116(19) F6 .0688(18) .092(2) .0541(16) .0432(16) .0170(14) .0321(15) N1 .0225(14) .0266(16) .0222(14) -.0025(12) .0140(12) -.0017(11) C1 .0230(17) .0260(19) .0298(18) -.0029(14) .0160(14) -.0022(14) C2 .0309(19) .048(2) .032(2) -.0051(17) .0178(16) .0006(17) C3 .036(2) .051(3) .050(2) -.0035(19) .0326(19) -.0026(19) C4 .0268(19) .033(2) .057(3) -.0020(16) .0245(19) -.0034(18) C5 .028(2) .051(2) .037(2) -.0020(18) .0131(17) .0026(19) C6 .0293(19) .045(2) .0322(19) -.0041(17) .0161(16) .0001(17) C7 .031(2) .061(3) .077(3) -.002(2) .029(2) .002(2) C8 .0251(17) .033(2) .0293(18) -.0027(15) .0163(15) -.0054(15) C9 .0327(19) .030(2) .041(2) -.0067(16) .0235(17) -.0117(16) C10 .0293(18) .0189(18) .036(2) -.0062(14) .0184(16) -.0073(14) C11 .0245(18) .0260(19) .0309(18) -.0065(14) .0151(15) -.0059(15) C12 .0302(19) .0256(19) .042(2) -.0069(15) .0247(17) -.0045(16) C13 .040(2) .0255(19) .036(2) -.0083(16) .0225(17) .0010(16) C14 .0339(19) .0209(18) .039(2) -.0001(15) .0185(16) .0011(16) C15 .057(2) .030(2) .037(2) -.0094(18) .0325(19) -.0094(16) C16 .119(5) .056(3) .070(3) -.032(3) .076(3) -.029(3) C17 .066(3) .060(3) .054(3) .012(2) .045(2) -.001(2) C18 .053(3) .059(3) .061(3) -.020(2) .050(2) -.023(2) C19 .0290(19) .0276(19) .0242(17) -.0008(15) .0105(15) .0013(15) C20 .051(3) .065(3) .046(3) .022(2) .019(2) .013(2) 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 Ti1 N1 . 1.993(3) Y Ti1 O3 . 2.086(2) Y Ti1 O6 . 2.093(2) Y Ti1 O9 . 2.156(2) Y Ti1 O2 . 2.289(2) Y Ti1 C11 . 2.373(3) Y Ti1 C13 . 2.375(3) Y Ti1 C12 . 2.378(3) Y Ti1 C14 . 2.379(3) Y Ti1 C10 . 2.385(3) Y Ti1 S1 . 2.8078(11) N S1 O1 . 1.431(2) Y S1 O2 . 1.479(2) Y S1 N1 . 1.597(3) Y S1 C1 . 1.766(3) Y S2 O4 . 1.429(2) Y S2 O5 . 1.432(2) N S2 O3 . 1.483(2) Y S2 C19 . 1.831(3) Y S3 O7 . 1.420(3) N S3 O8 . 1.431(3) N S3 O6 . 1.484(2) N S3 C20 . 1.831(5) N O9 C15 . 1.467(4) Y O9 C18 . 1.472(4) N F1 C19 . 1.331(4) Y F2 C19 . 1.323(4) N F3 C19 . 1.335(4) N F4 C20 . 1.311(5) Y F5 C20 . 1.323(5) N F6 C20 . 1.329(5) N N1 C8 . 1.484(4) Y C1 C6 . 1.383(5) N C1 C2 . 1.404(5) N C2 C3 . 1.380(5) N C3 C4 . 1.387(5) N C4 C5 . 1.396(5) N C4 C7 . 1.513(5) N C5 C6 . 1.390(5) N C8 C9 . 1.522(5) Y C9 C10 . 1.516(4) Y C10 C14 . 1.403(5) Y C10 C11 . 1.427(5) Y C11 C12 . 1.408(5) N C12 C13 . 1.406(5) N C13 C14 . 1.422(5) N C15 C16 . 1.498(5) Y C16 C17 . 1.498(6) N C17 C18 . 1.485(5) N