#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060302.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_4060302 _journal_name_full 'Organometallics' _journal_year 2005 _publ_section_title ; Trapping Unstable Terminal Ta-O Multiple Bonds of Monocyclopentadienyl Tantalum Complexes with a Lewis Acid ; loop_ _publ_author_name 'Sanchez-Nieves, J.' 'Frutos, L. M.' 'Royo, P.' 'Castano, O.' 'Herdtweck, E.' _chemical_formula_moiety'C28 H15 B Cl2 F15 O Ta' _chemical_formula_sum'C28 H15 B Cl2 F15 O Ta' _chemical_formula_weight 915.06 _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.6113(1) _cell_length_b 11.2399(1) _cell_length_c 13.7102(2) _cell_angle_alpha 88.8081(5) _cell_angle_beta 69.2081(5) _cell_angle_gamma 74.7048(5) _cell_volume 1469.76(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _exptl_crystal_density_diffrn 2.068 _diffrn_ambient_temperature 173(1) _refine_diff_density_rms 0.092 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ta Ta Uani 0.14209(1) 0.17466(1) 0.36797(1) 1.000 0.0224(1) . . Cl1 Cl Uani 0.11568(11) -0.01278(8) 0.33217(9) 1.000 0.0420(3) . . Cl2 Cl Uani -0.05953(9) 0.26892(9) 0.50350(7) 1.000 0.0350(3) . . F32 F Uani -0.0818(3) 0.3398(2) 0.03584(18) 1.000 0.0463(8) . . F33 F Uani -0.0372(3) 0.1690(3) -0.1128(2) 1.000 0.0599(10) . . F34 F Uani 0.1739(4) -0.0436(3) -0.1490(2) 1.000 0.0669(10) . . F35 F Uani 0.3380(4) -0.0798(2) -0.0308(2) 1.000 0.0725(10) . . F36 F Uani 0.3038(3) 0.0945(3) 0.1110(2) 1.000 0.0583(9) . . F42 F Uani -0.1312(2) 0.20828(18) 0.29588(16) 1.000 0.0310(6) . . F43 F Uani -0.4055(2) 0.3075(2) 0.39629(18) 1.000 0.0396(7) . . F44 F Uani -0.5246(2) 0.5516(2) 0.3851(2) 1.000 0.0445(8) . . F45 F Uani -0.3621(2) 0.69422(19) 0.27406(18) 1.000 0.0386(7) . . F46 F Uani -0.0886(2) 0.60007(18) 0.17589(17) 1.000 0.0330(6) . . F52 F Uani 0.0911(2) 0.5171(2) 0.30746(16) 1.000 0.0376(7) . . F53 F Uani 0.2408(3) 0.6819(2) 0.2508(2) 1.000 0.0563(9) . . F54 F Uani 0.3973(3) 0.6900(2) 0.0463(2) 1.000 0.0546(9) . . F55 F Uani 0.4040(3) 0.5269(3) -0.10081(18) 1.000 0.0497(9) . . F56 F Uani 0.2661(2) 0.3574(2) -0.04673(16) 1.000 0.0427(8) . . O O Uani 0.1195(2) 0.2630(2) 0.26280(18) 1.000 0.0243(7) . . C11 C Uani 0.3145(4) 0.0504(4) 0.4420(3) 1.000 0.0339(11) . . C12 C Uani 0.3853(4) 0.0753(3) 0.3373(3) 1.000 0.0327(11) . . C13 C Uani 0.3661(4) 0.2055(3) 0.3338(3) 1.000 0.0275(10) . . C14 C Uani 0.2789(4) 0.2616(3) 0.4368(3) 1.000 0.0296(11) . . C15 C Uani 0.2503(4) 0.1640(4) 0.5026(3) 1.000 0.0335(11) . . C21 C Uani 0.3192(6) -0.0755(5) 0.4810(5) 1.000 0.0505(17) . . C22 C Uani 0.4767(5) -0.0219(4) 0.2486(4) 1.000 0.0442(14) . . C23 C Uani 0.4346(4) 0.2690(4) 0.2402(3) 1.000 0.0333(12) . . C24 C Uani 0.2348(5) 0.3957(4) 0.4721(4) 1.000 0.0372(12) . . C25 C Uani 0.1702(5) 0.1816(5) 0.6194(3) 1.000 0.0447(16) . . C31 C Uani 0.1033(4) 0.2237(3) 0.0853(3) 1.000 0.0256(10) . . C32 C Uani 0.0227(4) 0.2362(3) 0.0234(3) 1.000 0.0296(10) . . C33 C Uani 0.0450(4) 0.1498(4) -0.0551(3) 1.000 0.0378(11) . . C34 C Uani 0.1509(5) 0.0421(4) -0.0733(3) 1.000 0.0441(14) . . C35 C Uani 0.2329(5) 0.0244(4) -0.0143(3) 1.000 0.0440(14) . . C36 C Uani 0.2095(4) 0.1156(4) 0.0613(3) 1.000 0.0353(11) . . C41 C Uani -0.0925(3) 0.3989(3) 0.2334(2) 1.000 0.0228(9) . . C42 C Uani -0.1831(4) 0.3311(3) 0.2903(3) 1.000 0.0241(9) . . C43 C Uani -0.3251(4) 0.3796(3) 0.3414(3) 1.000 0.0282(10) . . C44 C Uani -0.3862(4) 0.5022(4) 0.3364(3) 1.000 0.0311(11) . . C45 C Uani -0.3029(4) 0.5738(3) 0.2795(3) 1.000 0.0284(10) . . C46 C Uani -0.1610(3) 0.5225(3) 0.2304(2) 1.000 0.0241(10) . . C51 C Uani 0.1719(3) 0.4272(3) 0.1345(3) 1.000 0.0250(10) . . C52 C Uani 0.1720(4) 0.5138(3) 0.2043(3) 1.000 0.0283(10) . . C53 C Uani 0.2461(4) 0.6011(3) 0.1778(3) 1.000 0.0357(11) . . C54 C Uani 0.3249(4) 0.6047(4) 0.0743(3) 1.000 0.0387(11) . . C55 C Uani 0.3290(4) 0.5221(4) 0.0012(3) 1.000 0.0334(11) . . C56 C Uani 0.2548(4) 0.4347(3) 0.0312(3) 1.000 0.0297(11) . . B B Uani 0.0763(4) 0.3307(3) 0.1755(3) 1.000 0.0229(10) . . H211 H Uiso 0.242(7) -0.070(6) 0.542(5) 1.000 0.079(19) . . H212 H Uiso 0.397(8) -0.108(6) 0.490(5) 1.000 0.09(2) . . H213 H Uiso 0.324(7) -0.118(6) 0.432(5) 1.000 0.08(2) . . H221 H Uiso 0.480(6) 0.010(5) 0.175(5) 1.000 0.067(16) . . H222 H Uiso 0.442(6) -0.088(6) 0.250(5) 1.000 0.074(18) . . H223 H Uiso 0.573(5) -0.059(4) 0.249(4) 1.000 0.051(13) . . H231 H Uiso 0.408(5) 0.355(5) 0.255(4) 1.000 0.052(13) . . H232 H Uiso 0.417(5) 0.251(4) 0.179(4) 1.000 0.047(13) . . H233 H Uiso 0.523(5) 0.247(4) 0.230(3) 1.000 0.039(12) . . H241 H Uiso 0.236(5) 0.445(4) 0.419(4) 1.000 0.042(12) . . H242 H Uiso 0.287(6) 0.411(5) 0.508(5) 1.000 0.073(18) . . H243 H Uiso 0.142(6) 0.424(5) 0.516(4) 1.000 0.054(14) . . H251 H Uiso 0.125(7) 0.117(7) 0.640(5) 1.000 0.10(2) . . H252 H Uiso 0.089(9) 0.268(8) 0.646(6) 1.000 0.12(3) . . H253 H Uiso 0.225(7) 0.188(6) 0.653(5) 1.000 0.077(19) . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta 0.0242(1) 0.0206(1) 0.0225(1) 0.0080(1) -0.0090(1) -0.0063(1) Cl1 0.0499(6) 0.0233(4) 0.0586(6) 0.0063(4) -0.0260(5) -0.0108(4) Cl2 0.0299(4) 0.0429(5) 0.0264(4) 0.0027(4) -0.0047(4) -0.0081(4) F32 0.0455(14) 0.0495(14) 0.0392(13) -0.0043(10) -0.0262(11) 0.0103(11) F33 0.0605(17) 0.083(2) 0.0448(15) -0.0113(14) -0.0270(13) -0.0217(15) F34 0.092(2) 0.0493(16) 0.0473(15) -0.0196(13) -0.0057(15) -0.0247(15) F35 0.088(2) 0.0380(14) 0.0472(16) -0.0033(12) -0.0025(15) 0.0253(14) F36 0.0443(14) 0.0664(17) 0.0417(14) -0.0045(12) -0.0188(12) 0.0267(13) F42 0.0327(11) 0.0238(10) 0.0385(11) 0.0105(8) -0.0144(9) -0.0094(8) F43 0.0294(11) 0.0464(13) 0.0460(13) 0.0197(10) -0.0115(10) -0.0195(10) F44 0.0207(11) 0.0474(14) 0.0547(15) 0.0050(11) -0.0058(10) -0.0027(10) F45 0.0310(11) 0.0256(11) 0.0519(14) 0.0039(9) -0.0143(10) 0.0033(9) F46 0.0291(11) 0.0268(10) 0.0416(12) 0.0164(9) -0.0115(9) -0.0079(9) F52 0.0425(12) 0.0366(12) 0.0278(11) -0.0011(9) -0.0032(9) -0.0143(10) F53 0.0609(17) 0.0398(14) 0.0624(17) -0.0075(12) -0.0066(13) -0.0251(12) F54 0.0472(14) 0.0407(14) 0.0744(18) 0.0222(13) -0.0122(13) -0.0246(12) F55 0.0401(13) 0.0761(18) 0.0354(13) 0.0300(12) -0.0098(10) -0.0276(13) F56 0.0446(13) 0.0665(16) 0.0210(10) 0.0090(10) -0.0088(9) -0.0266(12) O 0.0227(11) 0.0255(12) 0.0247(12) 0.0081(9) -0.0095(9) -0.0058(9) C11 0.0289(18) 0.035(2) 0.042(2) 0.0179(17) -0.0185(17) -0.0091(16) C12 0.0256(18) 0.0333(19) 0.042(2) 0.0131(16) -0.0175(16) -0.0059(15) C13 0.0229(17) 0.0312(18) 0.0304(18) 0.0093(14) -0.0124(14) -0.0075(14) C14 0.0284(18) 0.0362(19) 0.0316(18) 0.0100(15) -0.0161(15) -0.0141(15) C15 0.0319(19) 0.045(2) 0.0303(19) 0.0128(16) -0.0174(16) -0.0136(17) C21 0.054(3) 0.041(3) 0.062(3) 0.030(3) -0.029(3) -0.013(2) C22 0.034(2) 0.030(2) 0.056(3) 0.0043(19) -0.011(2) 0.0045(18) C23 0.029(2) 0.034(2) 0.035(2) 0.0116(17) -0.0095(17) -0.0091(17) C24 0.041(2) 0.037(2) 0.037(2) 0.0028(18) -0.015(2) -0.0152(18) C25 0.051(3) 0.067(3) 0.028(2) 0.017(2) -0.020(2) -0.029(2) C31 0.0262(17) 0.0248(17) 0.0218(16) 0.0073(13) -0.0056(14) -0.0050(14) C32 0.0295(18) 0.0306(18) 0.0256(17) 0.0050(14) -0.0078(15) -0.0065(15) C33 0.041(2) 0.045(2) 0.0283(19) 0.0016(16) -0.0089(17) -0.0183(18) C34 0.056(3) 0.038(2) 0.031(2) -0.0038(17) -0.0015(19) -0.020(2) C35 0.053(3) 0.0263(19) 0.033(2) 0.0043(16) -0.0014(19) 0.0016(18) C36 0.036(2) 0.034(2) 0.0261(18) 0.0056(15) -0.0079(16) 0.0018(16) C41 0.0261(17) 0.0242(16) 0.0183(15) 0.0044(12) -0.0096(13) -0.0052(13) C42 0.0283(17) 0.0240(16) 0.0232(16) 0.0064(13) -0.0140(14) -0.0064(14) C43 0.0270(17) 0.0368(19) 0.0251(17) 0.0094(14) -0.0111(14) -0.0140(15) C44 0.0232(17) 0.039(2) 0.0284(18) 0.0027(15) -0.0085(15) -0.0051(15) C45 0.0304(18) 0.0258(17) 0.0289(18) 0.0030(14) -0.0144(15) -0.0026(14) C46 0.0263(17) 0.0266(17) 0.0208(16) 0.0062(13) -0.0101(13) -0.0076(14) C51 0.0204(16) 0.0273(17) 0.0259(17) 0.0116(13) -0.0098(13) -0.0031(13) C52 0.0258(17) 0.0258(17) 0.0289(18) 0.0073(14) -0.0074(14) -0.0037(14) C53 0.0320(19) 0.0242(18) 0.049(2) 0.0049(16) -0.0138(18) -0.0058(15) C54 0.0287(19) 0.0292(19) 0.055(2) 0.0213(18) -0.0106(18) -0.0105(15) C55 0.0236(17) 0.044(2) 0.0306(19) 0.0195(17) -0.0086(15) -0.0090(16) C56 0.0244(17) 0.038(2) 0.0265(18) 0.0129(15) -0.0113(14) -0.0063(15) B 0.0235(18) 0.0230(18) 0.0219(18) 0.0087(14) -0.0098(15) -0.0042(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta Cl1 2.2826(10) . . yes Ta Cl2 2.2839(10) . . yes Ta O 1.784(2) . . yes Ta C11 2.498(4) . . yes Ta C12 2.411(4) . . yes Ta C13 2.372(5) . . yes Ta C14 2.390(4) . . yes Ta C15 2.482(4) . . yes F32 C32 1.344(5) . . yes F33 C33 1.348(5) . . yes F34 C34 1.343(5) . . yes F35 C35 1.345(6) . . yes F36 C36 1.369(6) . . yes F42 C42 1.356(4) . . yes F43 C43 1.354(5) . . yes F44 C44 1.342(5) . . yes F45 C45 1.346(4) . . yes F46 C46 1.352(4) . . yes F52 C52 1.365(4) . . yes F53 C53 1.342(5) . . yes F54 C54 1.349(5) . . yes F55 C55 1.350(5) . . yes F56 C56 1.343(4) . . yes O B 1.546(4) . . yes C11 C12 1.425(5) . . no C11 C15 1.403(6) . . no C11 C21 1.497(7) . . no C12 C13 1.426(5) . . no C12 C22 1.507(6) . . no C13 C14 1.432(5) . . no C13 C23 1.503(6) . . no C14 C15 1.432(5) . . no C14 C24 1.491(6) . . no C15 C25 1.511(5) . . no C31 C32 1.385(6) . . no C31 C36 1.373(6) . . no C31 B 1.639(5) . . yes C32 C33 1.378(6) . . no C33 C34 1.373(6) . . no C34 C35 1.361(7) . . no C35 C36 1.383(6) . . no C41 C42 1.394(5) . . no C41 C46 1.395(5) . . no C41 B 1.649(5) . . yes C42 C43 1.375(6) . . no C43 C44 1.371(5) . . no C44 C45 1.377(6) . . no C45 C46 1.375(5) . . no C51 C52 1.380(5) . . no C51 C56 1.392(5) . . no C51 B 1.635(5) . . yes C52 C53 1.379(6) . . no C53 C54 1.374(5) . . no C54 C55 1.362(6) . . no C55 C56 1.384(6) . . no C21 H211 0.93(7) . . no C21 H212 0.86(9) . . no C21 H213 0.81(6) . . no C22 H221 1.06(6) . . no C22 H222 0.91(7) . . no C22 H223 1.00(6) . . no C23 H231 0.94(5) . . no C23 H232 0.96(5) . . no C23 H233 0.86(6) . . no C24 H241 0.90(5) . . no C24 H242 0.91(7) . . no C24 H243 0.92(6) . . no C25 H251 0.96(8) . . no C25 H252 1.08(9) . . no C25 H253 0.88(8) . . no