#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012425.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_2012425 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m41 _journal_page_last m42 _publ_section_title ; A dimeric constrained geometry titanium complex linked by double Ti-CH~2~-Al-CH~2~ heterocycles ; loop_ _publ_author_name 'Abboud, Khalil A.' 'Nickias, Peter N.' 'Chen, Eugene Y.-X.' _chemical_formula_moiety 'C84 H76 Al4 N2 Si2 Ti2, 2(C6 D6)' _chemical_formula_sum 'C96 H88 Al4 F30 N2 Si2 Ti2' _chemical_formula_weight 2099.58 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8651(7) _cell_length_b 13.7422(7) _cell_length_c 15.2642(9) _cell_angle_alpha 70.595(2) _cell_angle_beta 70.795(2) _cell_angle_gamma 71.944(2) _cell_volume 2341.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _exptl_crystal_density_diffrn 1.489 _diffrn_ambient_temperature 193(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 Ti .42688(4) .27710(4) .09256(4) .02225(14) Uani d . 1 . . Ti Si .29320(7) .14645(7) .25173(6) .0279(2) Uani d . 1 . . Si Al1 .74041(7) .27090(7) .13527(7) .0259(2) Uani d . 1 . . Al Al2 .58022(7) .41061(7) -.00737(7) .0248(2) Uani d . 1 . . Al N1 .33080(19) .26909(18) .21819(17) .0246(6) Uani d . 1 . . N C1 .3560(2) .1341(2) .1263(2) .0245(7) Uani d . 1 . . C C2 .3111(3) .2100(2) .0486(2) .0266(7) Uani d . 1 . . C C3 .3986(3) .2235(2) -.0360(2) .0288(7) Uani d . 1 . . C C4 .6109(3) .1200(3) -.0753(2) .0340(8) Uani d . 1 . . C C5 .6896(3) .0474(3) -.0310(3) .0398(9) Uani d . 1 . . C H5A .7639 .0281 -.0693 .048 Uiso calc R 1 . . H C6 .6672(3) -.0012(2) .0690(3) .0351(8) Uani d . 1 . . C C7 .5604(3) .0220(2) .1261(2) .0306(7) Uani d . 1 . . C H7A .5443 -.0117 .1928 .037 Uiso calc R 1 . . H C8 .4740(3) .0969(2) .0846(2) .0253(7) Uani d . 1 . . C C9 .5009(3) .1503(2) -.0158(2) .0252(7) Uani d . 1 . . C C10 .3662(3) .0417(3) .3398(2) .0412(9) Uani d . 1 . . C H10A .3262 .0495 .4048 .062 Uiso calc R 1 . . H H10B .4440 .0486 .3252 .062 Uiso calc R 1 . . H H10C .3667 -.0282 .3358 .062 Uiso calc R 1 . . H C11 .1416(3) .1458(3) .2997(3) .0466(10) Uani d . 1 . . C H11A .0982 .2047 .2594 .070 Uiso calc R 1 . . H H11B .1164 .1536 .3655 .070 Uiso calc R 1 . . H H11C .1297 .0787 .2997 .070 Uiso calc R 1 . . H C12 .1890(3) .2676(3) .0568(3) .0370(8) Uani d . 1 . . C H12A .1633 .3031 .1088 .056 Uiso calc R 1 . . H H12B .1428 .2168 .0708 .056 Uiso calc R 1 . . H H12C .1816 .3204 -.0038 .056 Uiso calc R 1 . . H C13 .3834(3) .2940(3) -.1326(2) .0403(9) Uani d . 1 . . C H13A .3739 .2525 -.1695 .060 Uiso calc R 1 . . H H13B .4501 .3239 -.1674 .060 Uiso calc R 1 . . H H13C .3163 .3516 -.1236 .060 Uiso calc R 1 . . H C14 .6385(3) .1581(3) -.1833(2) .0451(9) Uani d . 1 . . C H14A .7182 .1281 -.2100 .068 Uiso calc R 1 . . H H14B .6246 .2356 -.2025 .068 Uiso calc R 1 . . H H14C .5908 .1353 -.2077 .068 Uiso calc R 1 . . H C15 .7619(3) -.0795(3) .1094(3) .0488(10) Uani d . 1 . . C H15A .7340 -.1063 .1789 .073 Uiso calc R 1 . . H H15B .8232 -.0446 .0966 .073 Uiso calc R 1 . . H H15C .7902 -.1386 .0792 .073 Uiso calc R 1 . . H C16 .3005(3) .3441(2) .2785(2) .0265(7) Uani d . 1 . . C H16A .342(2) .398(2) .248(2) .026(8) Uiso d . 1 . . H C17 .1769(3) .4012(3) .2910(2) .0353(8) Uani d . 1 . . C H17A .1295 .3483 .3200 .042 Uiso calc R 1 . . H H17B .1631 .4413 .2272 .042 Uiso calc R 1 . . H C18 .1424(3) .4774(3) .3547(3) .0429(9) Uani d . 1 . . C H18A .1827 .5356 .3219 .051 Uiso calc R 1 . . H H18B .0603 .5088 .3649 .051 Uiso calc R 1 . . H C19 .1697(3) .4211(3) .4510(3) .0505(10) Uani d . 1 . . C H19A .1223 .3688 .4873 .061 Uiso calc R 1 . . H H19B .1519 .4732 .4886 .061 Uiso calc R 1 . . H C20 .2934(3) .3649(3) .4382(3) .0498(10) Uani d . 1 . . C H20A .3078 .3253 .5019 .060 Uiso calc R 1 . . H H20B .3404 .4182 .4087 .060 Uiso calc R 1 . . H C21 .3277(3) .2884(3) .3751(2) .0407(9) Uani d . 1 . . C H21A .4098 .2569 .3650 .049 Uiso calc R 1 . . H H21B .2874 .2302 .4082 .049 Uiso calc R 1 . . H C22 .4071(3) .4421(2) .0064(3) .0259(7) Uani d . 1 . . C H22A .391(2) .447(2) -.046(2) .030(9) Uiso d . 1 . . H H22B .342(3) .445(2) .058(3) .045(10) Uiso d . 1 . . H C23 .5945(3) .2806(3) .1029(2) .0263(7) Uani d . 1 . . C H23A .554(3) .271(3) .168(3) .046(10) Uiso d . 1 . . H H23B .622(3) .212(3) .090(2) .043(10) Uiso d . 1 . . H C24 .8564(2) .3095(2) .0121(2) .0277(7) Uani d . 1 . . C C25 .9052(3) .2426(3) -.0477(3) .0353(8) Uani d . 1 . . C C26 .9856(3) .2634(3) -.1331(3) .0404(9) Uani d . 1 . . C C27 1.0228(3) .3547(3) -.1613(2) .0376(8) Uani d . 1 . . C C28 .9770(3) .4250(3) -.1054(2) .0348(8) Uani d . 1 . . C C29 .8954(3) .4011(2) -.0212(2) .0296(7) Uani d . 1 . . C C30 .7947(2) .1235(2) .2128(2) .0280(7) Uani d . 1 . . C C31 .7203(3) .0709(3) .2882(2) .0331(8) Uani d . 1 . . C C32 .7517(3) -.0254(3) .3506(2) .0392(9) Uani d . 1 . . C C33 .8636(3) -.0725(3) .3397(3) .0435(9) Uani d . 1 . . C C34 .9423(3) -.0245(3) .2673(3) .0388(9) Uani d . 1 . . C C35 .9067(3) .0700(2) .2054(2) .0341(8) Uani d . 1 . . C C36 .7193(2) .3602(2) .2226(2) .0266(7) Uani d . 1 . . C C37 .8110(3) .3566(2) .2529(2) .0302(7) Uani d . 1 . . C C38 .8089(3) .4103(3) .3149(2) .0335(8) Uani d . 1 . . C C39 .7079(3) .4748(3) .3500(2) .0391(9) Uani d . 1 . . C C40 .6129(3) .4808(3) .3239(2) .0369(8) Uani d . 1 . . C C41 .6207(3) .4244(2) .2622(2) .0294(7) Uani d . 1 . . C C42 .6697(3) .3775(2) -.1289(2) .0322(8) Uani d . 1 . . C H42A .7222 .4246 -.1623 .048 Uiso calc R 1 . . H H42B .6193 .3875 -.1689 .048 Uiso calc R 1 . . H H42C .7124 .3038 -.1165 .048 Uiso calc R 1 . . H C43 .1269(5) .8313(4) .4862(4) .0794(16) Uani d . 1 . . C H43A .0499 .8675 .4922 .095 Uiso calc R 1 . . H C44 .1737(4) .7564(4) .4342(3) .0729(14) Uani d . 1 . . C H44A .1287 .7399 .4051 .087 Uiso calc R 1 . . H C45 .2853(4) .7060(4) .4245(3) .0717(14) Uani d . 1 . . C H45A .3171 .6540 .3890 .086 Uiso calc R 1 . . H C46 .3522(4) .7297(4) .4657(3) .0699(14) Uani d . 1 . . C H46A .4300 .6954 .4575 .084 Uiso calc R 1 . . H C47 .3049(5) .8037(4) .5189(3) .0741(14) Uani d . 1 . . C H47A .3497 .8204 .5481 .089 Uiso calc R 1 . . H C48 .1925(5) .8532(4) .5293(4) .0822(17) Uani d . 1 . . C H48A .1596 .9032 .5669 .099 Uiso calc R 1 . . H F1 .87264(17) .14967(15) -.02248(15) .0490(5) Uani d . 1 . . F F2 1.02856(18) .19539(17) -.18922(16) .0576(6) Uani d . 1 . . F F3 1.10255(17) .37524(18) -.24308(15) .0619(7) Uani d . 1 . . F F4 1.00995(17) .51704(16) -.13341(15) .0506(6) Uani d . 1 . . F F5 .85175(15) .47535(14) .02991(13) .0389(5) Uani d . 1 . . F F6 .60791(15) .11783(15) .30520(14) .0444(5) Uani d . 1 . . F F7 .67309(18) -.07120(17) .42190(15) .0616(7) Uani d . 1 . . F F8 .89672(19) -.16596(16) .40026(16) .0645(7) Uani d . 1 . . F F9 1.05310(16) -.07091(16) .25674(17) .0564(6) Uani d . 1 . . F F10 .98908(14) .11159(15) .13412(15) .0456(5) Uani d . 1 . . F F11 .91194(14) .29469(15) .21849(14) .0410(5) Uani d . 1 . . F F12 .90134(16) .40156(17) .34182(15) .0506(6) Uani d . 1 . . F F13 .70205(19) .52930(17) .41032(15) .0577(6) Uani d . 1 . . F F14 .51417(17) .54291(17) .35970(16) .0576(6) Uani d . 1 . . F F15 .52404(14) .43539(15) .23844(14) .0420(5) 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 Ti .0245(3) .0214(3) .0233(3) -.0091(2) -.0049(2) -.0063(2) Si .0306(5) .0270(5) .0267(5) -.0124(4) -.0034(4) -.0061(4) Al1 .0247(5) .0242(5) .0295(5) -.0068(4) -.0073(4) -.0061(4) Al2 .0257(5) .0235(5) .0261(5) -.0085(4) -.0066(4) -.0047(4) N1 .0266(14) .0250(14) .0243(14) -.0085(11) -.0066(11) -.0063(11) C1 .0297(17) .0218(16) .0273(17) -.0133(13) -.0063(14) -.0070(13) C2 .0307(17) .0242(16) .0336(18) -.0108(13) -.0119(14) -.0105(13) C3 .0401(19) .0281(17) .0278(18) -.0139(15) -.0125(15) -.0098(14) C4 .040(2) .0320(19) .036(2) -.0173(16) -.0016(16) -.0150(15) C5 .0311(19) .038(2) .053(2) -.0087(16) .0019(17) -.0269(18) C6 .0319(19) .0250(18) .054(2) -.0062(15) -.0110(17) -.0174(16) C7 .0363(19) .0232(17) .039(2) -.0096(14) -.0131(16) -.0095(14) C8 .0317(17) .0218(16) .0269(17) -.0081(13) -.0069(14) -.0106(13) C9 .0324(17) .0233(16) .0265(17) -.0122(14) -.0067(14) -.0098(13) C10 .058(2) .034(2) .031(2) -.0162(18) -.0100(17) -.0028(15) C11 .039(2) .051(2) .050(2) -.0213(18) .0022(18) -.0152(18) C12 .0349(19) .0343(19) .046(2) -.0088(15) -.0174(17) -.0076(16) C13 .055(2) .042(2) .031(2) -.0202(18) -.0169(17) -.0050(16) C14 .047(2) .053(2) .037(2) -.0204(19) .0030(17) -.0202(18) C15 .041(2) .038(2) .077(3) .0026(17) -.025(2) -.027(2) C16 .0304(17) .0256(17) .0273(18) -.0104(14) -.0063(14) -.0088(14) C17 .0306(18) .036(2) .039(2) -.0059(15) -.0056(15) -.0143(16) C18 .039(2) .043(2) .046(2) -.0055(17) -.0022(17) -.0222(18) C19 .065(3) .048(2) .036(2) -.015(2) .0038(19) -.0216(18) C20 .073(3) .049(2) .035(2) -.012(2) -.019(2) -.0186(18) C21 .050(2) .042(2) .035(2) -.0046(17) -.0140(17) -.0175(16) C22 .0289(18) .0258(17) .0248(18) -.0077(14) -.0078(16) -.0062(14) C23 .0279(17) .0260(18) .0256(19) -.0073(14) -.0077(14) -.0054(14) C24 .0251(16) .0273(17) .0311(18) -.0047(14) -.0095(14) -.0065(14) C25 .0325(19) .0329(19) .042(2) -.0102(15) -.0103(16) -.0080(16) C26 .036(2) .044(2) .038(2) .0013(17) -.0051(17) -.0209(17) C27 .0288(18) .048(2) .0292(19) -.0108(16) .0006(15) -.0069(16) C28 .0309(18) .037(2) .036(2) -.0137(16) -.0103(15) -.0011(16) C29 .0304(17) .0305(18) .0289(18) -.0062(14) -.0089(15) -.0079(14) C30 .0278(17) .0269(17) .0317(18) -.0044(14) -.0112(14) -.0083(14) C31 .0302(18) .0356(19) .0335(19) -.0046(15) -.0086(15) -.0110(15) C32 .046(2) .040(2) .0285(19) -.0174(17) -.0081(16) .0008(16) C33 .054(2) .0284(19) .045(2) -.0043(17) -.0227(19) .0007(16) C34 .036(2) .0311(19) .050(2) -.0022(16) -.0174(17) -.0092(17) C35 .0354(19) .0275(18) .042(2) -.0127(15) -.0092(16) -.0082(15) C36 .0294(17) .0222(16) .0279(17) -.0087(13) -.0088(14) -.0019(13) C37 .0274(17) .0323(18) .0317(19) -.0097(14) -.0068(15) -.0072(15) C38 .0364(19) .039(2) .0305(19) -.0167(16) -.0119(16) -.0046(15) C39 .061(2) .039(2) .0260(19) -.0215(19) -.0107(17) -.0113(16) C40 .0359(19) .036(2) .035(2) -.0042(16) -.0048(16) -.0126(16) C41 .0298(18) .0326(18) .0268(18) -.0091(15) -.0083(14) -.0061(14) C42 .0346(18) .0279(18) .0339(19) -.0098(14) -.0066(15) -.0071(14) C43 .078(4) .071(3) .060(3) -.001(3) .003(3) -.015(3) C44 .076(3) .078(3) .050(3) -.001(3) -.011(2) -.017(3) C45 .088(4) .060(3) .045(3) .009(3) -.013(3) -.013(2) C46 .079(3) .056(3) .047(3) -.004(3) -.006(3) .001(2) C47 .106(4) .055(3) .051(3) -.029(3) -.009(3) -.002(2) C48 .112(5) .052(3) .058(3) -.018(3) .011(3) -.016(2) F1 .0571(13) .0386(12) .0563(14) -.0179(10) -.0069(11) -.0192(10) F2 .0571(14) .0587(14) .0548(15) -.0043(11) -.0025(11) -.0315(12) F3 .0481(13) .0773(16) .0467(14) -.0215(12) .0112(11) -.0148(12) F4 .0525(13) .0509(13) .0495(13) -.0309(11) -.0052(10) -.0040(10) F5 .0452(11) .0342(11) .0394(12) -.0152(9) -.0054(9) -.0115(9) F6 .0304(11) .0480(12) .0429(12) -.0074(9) -.0058(9) -.0013(10) F7 .0616(14) .0571(14) .0446(14) -.0183(12) -.0075(11) .0128(11) F8 .0708(15) .0410(13) .0633(16) -.0034(11) -.0292(13) .0136(11) F9 .0401(12) .0429(13) .0778(17) .0055(10) -.0253(11) -.0086(11) F10 .0301(11) .0405(12) .0582(14) -.0097(9) -.0077(10) -.0043(10) F11 .0282(10) .0454(12) .0537(13) -.0060(9) -.0130(9) -.0177(10) F12 .0496(13) .0658(14) .0529(14) -.0218(11) -.0266(11) -.0144(11) F13 .0730(15) .0681(15) .0489(14) -.0206(12) -.0136(11) -.0338(12) F14 .0482(13) .0633(15) .0629(15) .0022(11) -.0061(11) -.0398(12) F15 .0276(10) .0490(12) .0533(13) -.0015(9) -.0146(9) -.0203(10) 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 Ti N1 . 1.898(2) y Ti C22 . 2.195(3) y Ti C23 . 2.230(3) y Ti C1 . 2.256(3) y Ti C2 . 2.333(3) y Ti C8 . 2.395(3) y Ti C3 . 2.474(3) y Ti C9 . 2.556(3) y Ti Al2 . 2.826(2) ? Ti Si . 2.890(2) ? Ti H22B . 2.19(3) y Ti H23A . 2.26(3) y Si N1 . 1.762(2) ? Si C11 . 1.846(3) ? Si C1 . 1.861(3) ? Si C10 . 1.863(3) ? Al1 C36 . 2.000(3) ? Al1 C24 . 2.007(3) ? Al1 C30 . 2.016(3) ? Al1 C23 . 2.048(3) y Al2 C42 . 1.950(3) y Al2 C23 . 2.015(3) y Al2 C22 . 2.085(3) y Al2 C22 2_665 2.086(3) y Al2 Al2 2_665 2.695(2) y N1 C16 . 1.486(4) ? C1 C8 . 1.440(4) ? C1 C2 . 1.443(4) ? C2 C3 . 1.409(4) ? C2 C12 . 1.508(4) ? C3 C9 . 1.442(4) ? C3 C13 . 1.507(4) ? C4 C5 . 1.362(5) ? C4 C9 . 1.429(4) ? C4 C14 . 1.509(5) ? C5 C6 . 1.417(5) ? C5 H5A . .9500 ? C6 C7 . 1.369(4) ? C6 C15 . 1.505(5) ? C7 C8 . 1.420(4) ? C7 H7A . .9500 ? C8 C9 . 1.438(4) ? C10 H10A . .9800 ? C10 H10B . .9800 ? C10 H10C . .9800 ? C11 H11A . .9800 ? C11 H11B . .9800 ? C11 H11C . .9800 ? C12 H12A . .9800 ? C12 H12B . .9800 ? C12 H12C . .9800 ? C13 H13A . .9800 ? C13 H13B . .9800 ? C13 H13C . .9800 ? C14 H14A . .9800 ? C14 H14B . .9800 ? C14 H14C . .9800 ? C15 H15A . .9800 ? C15 H15B . .9800 ? C15 H15C . .9800 ? C16 C17 . 1.518(4) ? C16 C21 . 1.518(4) ? C16 H16A . .95(3) ? C17 C18 . 1.531(5) ? C17 H17A . .9900 ? C17 H17B . .9900 ? C18 C19 . 1.517(5) ? C18 H18A . .9900 ? C18 H18B . .9900 ? C19 C20 . 1.517(5) ? C19 H19A . .9900 ? C19 H19B . .9900 ? C20 C21 . 1.529(5) ? C20 H20A . .9900 ? C20 H20B . .9900 ? C21 H21A . .9900 ? C21 H21B . .9900 ? C22 Al2 2_665 2.086(3) ? C22 H22A . .87(3) ? C22 H22B . .94(3) ? C23 H23A . .94(4) ? C23 H23B . .95(3) ? C24 C29 . 1.376(4) ? C24 C25 . 1.376(5) ? C25 F1 . 1.361(4) ? C25 C26 . 1.379(5) ? C26 F2 . 1.347(4) ? C26 C27 . 1.366(5) ? C27 F3 . 1.339(4) ? C27 C28 . 1.368(5) ? C28 F4 . 1.347(4) ? C28 C29 . 1.380(4) ? C29 F5 . 1.360(4) ? C30 C31 . 1.384(4) ? C30 C35 . 1.387(4) ? C31 F6 . 1.364(3) ? C31 C32 . 1.380(4) ? C32 F7 . 1.349(4) ? C32 C33 . 1.362(5) ? C33 F8 . 1.348(4) ? C33 C34 . 1.370(5) ? C34 F9 . 1.348(4) ? C34 C35 . 1.374(4) ? C35 F10 . 1.356(3) ? C36 C41 . 1.381(4) ? C36 C37 . 1.384(4) ? C37 F11 . 1.360(3) ? C37 C38 . 1.370(5) ? C38 F12 . 1.341(4) ? C38 C39 . 1.380(5) ? C39 F13 . 1.338(4) ? C39 C40 . 1.377(5) ? C40 F14 . 1.350(4) ? C40 C41 . 1.368(5) ? C41 F15 . 1.358(3) ? C42 H42A . .9800 ? C42 H42B . .9800 ? C42 H42C . .9800 ? C43 C48 . 1.375(7) ? C43 C44 . 1.376(7) ? C43 H43A . .9500 ? C44 C45 . 1.369(6) ? C44 H44A . .9500 ? C45 C46 . 1.383(7) ? C45 H45A . .9500 ? C46 C47 . 1.379(6) ? C46 H46A . .9500 ? C47 C48 . 1.375(7) ? C47 H47A . .9500 ? C48 H48A . .9500 ? _cod_database_code 2012425