#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012533.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_2012533 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m98 _journal_page_last m101 _publ_section_title ; An ion pair formed by protonated octamethyl-5,5'-di(2-pyridyl)ferrocene and the cluster U~8~Cl~24~O~4~(cp*py)~2~ [cp*py is tetramethyl-5-(2-pyridyl)cyclopentadiene] ; loop_ _publ_author_name 'Moisan, Lionel' 'Le Borgne, Thierry' "Thu\'ery, Pierre" 'Ephritikhine, Michel' _chemical_formula_moiety '2C28 H33 Fe N2 + , C28 H32 Cl24 N2 O4 U8 2- , 4C H2 Cl2' _chemical_formula_sum 'C88 H106 Cl32 Fe2 N6 O4 U8' _chemical_formula_iupac '[Fe (C14 H17 N) (C14 H16 N)]2 [U8 Cl24 O4 (C14 H16 N)2] , 4C H2 Cl2' _chemical_formula_weight 4462.13 _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 14.3894(8) _cell_length_b 15.9758(7) _cell_length_c 16.0646(9) _cell_angle_alpha 61.128(3) _cell_angle_beta 70.648(2) _cell_angle_gamma 83.316(3) _cell_volume 3047.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _exptl_crystal_density_diffrn 2.432 _diffrn_ambient_temperature 100(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 U1 -.16535(3) .40443(3) -.17498(3) .02944(11) Uani d . 1 . . U U2 -.20671(3) .14128(3) .00935(3) .03239(11) Uani d . 1 . . U U3 .04858(3) .24356(3) -.18078(3) .02978(11) Uani d . 1 . . U U4 -.02128(3) -.02242(3) -.09604(3) .03512(12) Uani d . 1 . . U Fe -.31218(14) .20283(13) -.51142(13) .0423(4) Uani d . 1 . . Fe Cl1 -.2875(2) .2620(2) -.1456(2) .0429(7) Uani d . 1 . . Cl Cl2 -.0367(2) .3754(2) -.32903(19) .0392(7) Uani d . 1 . . Cl Cl3 -.2718(2) .3095(2) .0260(2) .0462(8) Uani d . 1 . . Cl Cl4 .0329(2) .4209(2) -.1799(2) .0388(7) Uani d . 1 . . Cl Cl5 -.3840(2) .0799(2) .1254(3) .0576(10) Uani d . 1 . . Cl Cl6 -.1225(2) .1429(2) .1368(2) .0455(7) Uani d . 1 . . Cl Cl7 .1251(2) .2009(2) -.0324(2) .0392(7) Uani d . 1 . . Cl Cl8 .2185(2) .3137(2) -.3107(2) .0447(8) Uani d . 1 . . Cl Cl9 .0150(2) .1510(2) -.2727(2) .0419(7) Uani d . 1 . . Cl Cl10 -.2156(2) .0307(2) -.0753(2) .0405(7) Uani d . 1 . . Cl Cl11 -.0627(3) -.0569(3) -.2259(3) .0591(9) Uani d . 1 . . Cl Cl12 .1732(2) .0585(2) -.1494(2) .0391(7) Uani d . 1 . . Cl O1 -.1020(6) .2610(5) -.1066(5) .0311(17) Uani d . 1 . . O O2 -.0361(6) .0908(5) -.0433(5) .0330(18) Uani d . 1 . . O N1 -.1554(7) .5152(7) -.1047(7) .036(2) Uani d . 1 . . N N2 -.5789(8) .2039(7) -.4463(7) .042(2) Uani d . 1 . . N N3 -.5154(7) .1506(7) -.2884(7) .037(2) Uani d . 1 . . N H3 -.5263 .1649 -.3474 .045 Uiso d R 1 . . H C1 -.1169(9) .5170(10) -.0396(10) .045(3) Uani d . 1 . . C H1 -.1053 .4588 .0100 .055 Uiso calc R 1 . . H C2 -.0946(10) .5966(11) -.0419(12) .056(4) Uani d . 1 . . C H2 -.0688 .5937 .0054 .067 Uiso calc R 1 . . H C3 -.1102(15) .6828(12) -.1151(12) .078(5) Uani d . 1 . . C H3A -.0987 .7393 -.1157 .094 Uiso calc R 1 . . H C4 -.1425(14) .6858(10) -.1869(12) .071(5) Uani d . 1 . . C H4 -.1463 .7438 -.2414 .085 Uiso calc R 1 . . H C5 -.1701(10) .5995(9) -.1767(9) .047(3) Uani d . 1 . . C C6 -.2161(10) .5806(9) -.2367(10) .042(3) Uani d . 1 . . C C7 -.3076(10) .5291(9) -.1966(8) .042(3) Uani d . 1 . . C C8 -.3103(9) .4978(8) -.2641(9) .037(3) Uani d . 1 . . C C9 -.2202(9) .5292(8) -.3460(9) .037(3) Uani d . 1 . . C C10 -.1609(9) .5808(8) -.3295(8) .033(3) Uani d . 1 . . C C11 -.3881(11) .5162(11) -.1062(10) .063(4) Uani d . 1 . . C H11A -.4394 .5582 -.1248 .094 Uiso calc R 1 . . H H11B -.3636 .5308 -.0656 .094 Uiso calc R 1 . . H H11C -.4141 .4510 -.0688 .094 Uiso calc R 1 . . H C12 -.3981(10) .4521(10) -.2588(11) .056(4) Uani d . 1 . . C H12A -.4325 .5001 -.3008 .083 Uiso calc R 1 . . H H12B -.4412 .4216 -.1909 .083 Uiso calc R 1 . . H H12C -.3771 .4052 -.2814 .083 Uiso calc R 1 . . H C13 -.1962(11) .5161(9) -.4366(9) .049(3) Uani d . 1 . . C H13A -.2322 .5597 -.4798 .074 Uiso calc R 1 . . H H13B -.2144 .4515 -.4165 .074 Uiso calc R 1 . . H H13C -.1268 .5285 -.4717 .074 Uiso calc R 1 . . H C14 -.0616(9) .6283(8) -.3988(9) .048(3) Uani d . 1 . . C H14A -.0694 .6910 -.4491 .072 Uiso calc R 1 . . H H14B -.0269 .5908 -.4303 .072 Uiso calc R 1 . . H H14C -.0247 .6337 -.3613 .072 Uiso calc R 1 . . H C15 -.6710(10) .1828(9) -.4226(11) .049(3) Uani d . 1 . . C H15 -.7058 .1474 -.3549 .059 Uiso calc R 1 . . H C16 -.7233(11) .2092(10) -.4915(11) .054(4) Uani d . 1 . . C H16 -.7909 .1964 -.4707 .065 Uiso calc R 1 . . H C17 -.6692(10) .2539(9) -.5893(10) .050(3) Uani d . 1 . . C H17 -.6979 .2690 -.6385 .060 Uiso calc R 1 . . H C18 -.5711(12) .2770(11) -.6152(11) .059(4) Uani d . 1 . . C H18 -.5352 .3103 -.6828 .071 Uiso calc R 1 . . H C19 -.5229(8) .2529(9) -.5452(10) .044(3) Uani d . 1 . . C C20 -.4118(8) .2774(7) -.5736(7) .032(3) Uani d . 1 . . C C21 -.3798(10) .3279(9) -.5394(10) .049(3) Uani d . 1 . . C C22 -.2793(10) .3484(8) -.5933(9) .043(3) Uani d . 1 . . C C23 -.2528(10) .3051(9) -.6567(9) .044(3) Uani d . 1 . . C C24 -.3423(11) .2625(10) -.6451(9) .058(4) Uani d . 1 . . C C25 -.4365(11) .3684(10) -.4687(10) .052(4) Uani d . 1 . . C H25A -.5060 .3603 -.4545 .078 Uiso calc R 1 . . H H25B -.4183 .4353 -.5000 .078 Uiso calc R 1 . . H H25C -.4205 .3350 -.4074 .078 Uiso calc R 1 . . H C26 -.2083(11) .4065(10) -.5862(10) .056(4) Uani d . 1 . . C H26A -.2306 .4701 -.6041 .084 Uiso calc R 1 . . H H26B -.1436 .4095 -.6311 .084 Uiso calc R 1 . . H H26C -.2060 .3766 -.5188 .084 Uiso calc R 1 . . H C27 -.1509(10) .3103(10) -.7289(11) .058(4) Uani d . 1 . . C H27A -.1019 .3227 -.7072 .087 Uiso calc R 1 . . H H27B -.1469 .3608 -.7949 .087 Uiso calc R 1 . . H H27C -.1395 .2505 -.7304 .087 Uiso calc R 1 . . H C28 -.3485(13) .2077(12) -.6985(11) .070(5) Uani d . 1 . . C H28A -.3544 .2518 -.7632 .105 Uiso calc R 1 . . H H28B -.4051 .1635 -.6596 .105 Uiso calc R 1 . . H H28C -.2899 .1730 -.7064 .105 Uiso calc R 1 . . H C29 -.5893(10) .1588(9) -.2133(9) .047(3) Uani d . 1 . . C H29 -.6517 .1754 -.2197 .056 Uiso calc R 1 . . H C30 -.5710(11) .1427(10) -.1305(10) .052(4) Uani d . 1 . . C H30 -.6202 .1508 -.0805 .063 Uiso calc R 1 . . H C31 -.4814(13) .1147(10) -.1184(11) .066(5) Uani d . 1 . . C H31 -.4701 .1020 -.0597 .079 Uiso calc R 1 . . H C32 -.4089(11) .1053(9) -.1918(10) .048(3) Uani d . 1 . . C H32 -.3476 .0862 -.1835 .057 Uiso calc R 1 . . H C33 -.4249(10) .1239(8) -.2795(9) .043(3) Uani d . 1 . . C C34 -.3510(9) .1134(8) -.3609(9) .043(3) Uani d . 1 . . C C35 -.3624(10) .0652(8) -.4139(10) .051(4) Uani d . 1 . . C C36 -.2657(12) .0653(9) -.4823(10) .056(4) Uani d . 1 . . C C37 -.1968(11) .1176(10) -.4721(12) .061(4) Uani d . 1 . . C C38 -.2482(10) .1474(10) -.3986(11) .055(4) Uani d . 1 . . C C39 -.4517(11) .0107(9) -.3957(11) .055(4) Uani d . 1 . . C H39A -.4374 -.0552 -.3757 .083 Uiso calc R 1 . . H H39B -.4690 .0376 -.4561 .083 Uiso calc R 1 . . H H39C -.5059 .0149 -.3436 .083 Uiso calc R 1 . . H C40 -.2433(15) .0211(13) -.5453(13) .088(6) Uani d U 1 . . C H40A -.3001 .0206 -.5638 .132 Uiso calc R 1 . . H H40B -.2255 -.0435 -.5099 .132 Uiso calc R 1 . . H H40C -.1894 .0565 -.6046 .132 Uiso calc R 1 . . H C41 -.0891(13) .1301(14) -.5244(14) .088(6) Uani d U 1 . . C H41A -.0566 .0787 -.4832 .132 Uiso calc R 1 . . H H41B -.0649 .1900 -.5372 .132 Uiso calc R 1 . . H H41C -.0761 .1296 -.5868 .132 Uiso calc R 1 . . H C42 -.2000(11) .2005(12) -.3648(12) .063(4) Uani d . 1 . . C H42A -.1504 .2463 -.4215 .095 Uiso calc R 1 . . H H42B -.1701 .1555 -.3160 .095 Uiso calc R 1 . . H H42C -.2491 .2331 -.3355 .095 Uiso calc R 1 . . H Cl13 -.3451(4) .4818(4) .1392(3) .0876(14) Uani d U 1 . . Cl Cl14 -.3505(7) .6464(6) .1554(6) .078(3) Uiso d PDU .516(10) . . Cl Cl15 -.3854(8) .5867(8) .2651(8) .098(4) Uiso d PDU .484(10) . . Cl C43 -.3039(14) .5321(10) .1968(12) .095(6) Uani d DU 1 . . C Cl16 -.4235(6) -1.2419(5) -.1840(6) .070(2) Uani d DU 1 . . Cl Cl17 -.3383(6) -1.1448(5) -.1189(6) .070(2) Uani d DU 1 . . Cl C44 -.3260(14) -1.1591(16) -.2271(11) .073(9) Uani d PDU .50 . . C C45 -.4151(16) -1.2467(12) -.0718(9) .068(8) Uani d PDU .50 . . 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 U1 .0305(2) .0279(2) .0293(2) .00313(17) -.00959(18) -.01338(18) U2 .0298(2) .0296(2) .0311(2) .00045(17) -.00676(18) -.01097(18) U3 .0281(2) .0291(2) .0288(2) .00150(17) -.00668(17) -.01267(18) U4 .0413(3) .0302(2) .0384(2) .00493(19) -.0179(2) -.0170(2) Fe .0419(11) .0406(9) .0460(10) -.0033(8) -.0087(8) -.0238(9) Cl1 .0406(18) .0370(15) .0511(17) -.0013(13) -.0244(14) -.0138(14) Cl2 .0450(18) .0411(15) .0269(13) .0118(13) -.0116(12) -.0145(12) Cl3 .053(2) .0398(16) .0358(15) .0091(14) -.0031(14) -.0192(14) Cl4 .0366(17) .0341(14) .0482(17) -.0003(12) -.0133(13) -.0210(13) Cl5 .0348(18) .0418(16) .059(2) .0001(14) .0067(15) -.0092(16) Cl6 .053(2) .0522(18) .0445(17) .0120(15) -.0204(15) -.0319(15) Cl7 .0434(18) .0376(15) .0439(16) .0007(13) -.0219(14) -.0193(13) Cl8 .0346(17) .0387(15) .0416(16) .0023(13) -.0023(13) -.0110(13) Cl9 .0504(19) .0447(16) .0353(15) .0063(14) -.0201(14) -.0192(14) Cl10 .0419(18) .0404(15) .0437(16) .0014(13) -.0204(14) -.0187(14) Cl11 .082(3) .055(2) .054(2) .0082(19) -.0399(19) -.0254(17) Cl12 .0359(17) .0363(14) .0346(15) .0022(12) -.0098(12) -.0098(12) O1 .035(5) .026(4) .027(4) -.001(3) -.010(3) -.008(3) O2 .030(4) .031(4) .036(4) .002(3) -.009(3) -.016(4) N1 .033(6) .041(5) .042(6) .004(4) -.017(5) -.024(5) N2 .036(6) .050(6) .044(6) .007(5) -.014(5) -.026(5) N3 .033(6) .038(5) .041(6) -.002(4) -.016(5) -.014(5) C1 .041(8) .060(8) .049(8) .016(6) -.021(6) -.034(7) C2 .039(8) .075(10) .073(10) .002(7) -.018(7) -.049(9) C3 .119(16) .062(10) .076(11) -.012(10) -.030(11) -.046(10) C4 .123(16) .041(8) .066(10) -.009(9) -.026(10) -.038(8) C5 .056(9) .046(7) .046(7) .017(6) -.016(6) -.031(7) C6 .042(8) .039(6) .059(8) .014(6) -.023(6) -.031(6) C7 .055(9) .039(6) .028(6) .009(6) -.013(6) -.015(5) C8 .036(7) .028(6) .045(7) .003(5) -.017(6) -.013(5) C9 .038(7) .027(5) .041(7) .007(5) -.021(6) -.008(5) C10 .038(7) .027(5) .036(6) .010(5) -.021(5) -.013(5) C11 .048(9) .076(10) .054(9) .033(8) -.018(7) -.029(8) C12 .045(9) .051(8) .062(9) .002(7) -.025(7) -.014(7) C13 .064(10) .048(7) .047(7) .011(7) -.031(7) -.023(6) C14 .044(8) .030(6) .050(8) .000(6) -.013(6) -.007(6) C15 .046(9) .047(7) .062(9) .014(6) -.026(7) -.029(7) C16 .042(8) .053(8) .081(11) .012(7) -.022(8) -.042(8) C17 .046(9) .046(7) .055(8) .000(6) -.027(7) -.015(7) C18 .071(11) .060(9) .055(9) .004(8) -.025(8) -.031(8) C19 .039(8) .053(8) .050(8) -.001(6) -.020(6) -.027(7) C20 .063(7) .016(4) .020(4) .001(4) -.012(4) -.012(4) C21 .043(8) .048(7) .050(8) .004(6) -.014(6) -.019(7) C22 .051(8) .034(6) .038(7) -.008(6) -.011(6) -.013(6) C23 .041(8) .054(8) .043(7) -.009(6) -.006(6) -.030(6) C24 .064(10) .049(8) .032(7) -.026(7) .001(7) -.003(6) C25 .053(9) .051(8) .050(8) .004(7) -.009(7) -.028(7) C26 .055(9) .053(8) .046(8) -.011(7) .001(7) -.023(7) C27 .043(9) .058(9) .072(10) -.011(7) -.005(7) -.035(8) C28 .081(12) .083(11) .053(9) -.005(9) -.005(8) -.046(9) C29 .042(8) .048(7) .051(8) -.008(6) -.009(6) -.027(7) C30 .046(9) .075(10) .045(8) -.019(7) -.007(7) -.035(7) C31 .090(13) .053(9) .045(8) -.029(9) -.019(9) -.012(7) C32 .046(8) .050(8) .049(8) -.008(6) -.021(7) -.018(7) C33 .049(8) .032(6) .037(7) -.010(6) -.010(6) -.007(5) C34 .038(8) .036(6) .046(7) -.003(5) -.010(6) -.013(6) C35 .053(9) .028(6) .056(8) -.005(6) -.008(7) -.013(6) C36 .071(11) .040(7) .053(8) .007(7) -.004(7) -.029(7) C37 .038(8) .055(8) .072(10) .001(7) -.006(7) -.023(8) C38 .042(8) .058(8) .057(9) .001(7) -.019(7) -.019(7) C39 .061(10) .044(7) .060(9) -.011(7) -.021(7) -.021(7) C40 .096(10) .078(8) .088(9) -.002(7) -.008(7) -.051(7) C41 .075(9) .083(8) .096(9) .006(7) -.014(7) -.043(7) C42 .047(9) .084(11) .072(10) -.005(8) -.024(8) -.042(9) Cl13 .066(3) .111(3) .073(3) .000(2) -.013(2) -.039(3) C43 .098(10) .108(10) .090(9) .019(8) -.026(7) -.061(8) Cl16 .099(6) .068(4) .079(5) .039(4) -.051(4) -.056(4) Cl17 .090(5) .060(4) .080(5) .015(4) -.029(4) -.049(4) C44 .049(11) .071(11) .064(11) .037(9) -.022(8) -.010(8) C45 .067(12) .041(9) .086(11) -.002(8) .022(8) -.051(9) 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 U1 O1 . 2.244(7) yes U1 N1 . 2.553(9) yes U1 C6 . 2.596(12) yes U1 C7 . 2.671(13) yes U1 C8 . 2.795(12) yes U1 C9 . 2.816(11) yes U1 C10 . 2.700(10) yes U1 Cl1 . 2.798(3) yes U1 Cl2 . 2.764(3) yes U1 Cl3 . 2.758(3) yes U1 Cl4 . 2.867(3) yes U2 O1 . 2.184(7) yes U2 O2 . 2.493(8) yes U2 Cl1 . 2.833(3) yes U2 Cl3 . 2.848(3) yes U2 Cl5 . 2.571(3) yes U2 Cl6 . 2.713(3) yes U2 Cl10 . 2.734(3) yes U2 Cl12 2 2.985(3) yes U3 O1 . 2.159(7) yes U3 O2 . 2.454(7) yes U3 Cl2 . 2.847(3) yes U3 Cl4 . 2.822(3) yes U3 Cl7 . 2.712(3) yes U3 Cl8 . 2.566(3) yes U3 Cl9 . 2.711(3) yes U3 Cl12 . 3.183(3) yes U4 O2 . 2.303(7) yes U4 O2 2 2.354(8) yes U4 Cl6 2 2.793(3) yes U4 Cl7 2 2.808(3) yes U4 Cl9 . 2.786(3) yes U4 Cl10 . 2.785(3) yes U4 Cl11 . 2.650(3) yes U4 Cl12 . 2.901(3) yes U1 U2 . 3.7668(6) yes U1 U3 . 3.7800(6) yes U2 U3 . 3.8256(6) yes U2 U4 2 3.9156(7) yes U2 U4 . 4.0600(6) yes U3 U4 . 3.9269(6) yes U3 U4 2 4.0503(6) yes U4 U4 2 3.7281(9) yes Fe C20 . 1.969(11) yes Fe C21 . 2.028(14) yes Fe C22 . 2.061(12) yes Fe C23 . 2.042(12) yes Fe C24 . 2.063(15) yes Fe C34 . 2.038(12) yes Fe C35 . 2.025(12) yes Fe C36 . 2.090(13) yes Fe C37 . 2.086(15) yes Fe C38 . 2.070(15) yes Cl6 U4 2 2.793(3) ? Cl7 U4 2 2.808(3) ? Cl12 U2 2 2.985(3) ? O2 U4 2 2.354(8) ? N1 C5 . 1.337(16) ? N1 C1 . 1.348(15) ? N2 C15 . 1.288(16) ? N2 C19 . 1.372(15) ? N2 H3 . 1.7954 ? N2 N3 . 2.696(14) ? N3 H3 . .9239 ? N3 C33 . 1.354(16) ? N3 C29 . 1.370(15) ? C1 C2 . 1.329(19) ? C2 C3 . 1.37(2) ? C3 C4 . 1.36(2) ? C4 C5 . 1.398(18) ? C5 C6 . 1.486(18) ? C6 C7 . 1.416(18) ? C6 C10 . 1.436(16) ? C7 C8 . 1.407(17) ? C7 C11 . 1.465(17) ? C8 C9 . 1.431(16) ? C8 C12 . 1.490(18) ? C9 C10 . 1.416(16) ? C9 C13 . 1.492(17) ? C10 C14 . 1.496(16) ? C15 C16 . 1.41(2) ? C16 C17 . 1.349(19) ? C17 C18 . 1.37(2) ? C18 C19 . 1.389(19) ? C19 C20 . 1.552(9) ? C20 C24 . 1.350(17) ? C20 C21 . 1.359(17) ? C21 C22 . 1.399(18) ? C21 C25 . 1.531(18) ? C22 C23 . 1.421(17) ? C22 C26 . 1.524(18) ? C23 C24 . 1.442(19) ? C23 C27 . 1.521(18) ? C24 C28 . 1.52(2) ? C29 C30 . 1.339(18) ? C30 C31 . 1.36(2) ? C31 C32 . 1.35(2) ? C32 C33 . 1.386(18) ? C33 C34 . 1.455(17) ? C34 C35 . 1.448(19) ? C34 C38 . 1.459(18) ? C35 C36 . 1.459(19) ? C35 C39 . 1.505(18) ? C36 C40 . 1.43(2) ? C36 C37 . 1.46(2) ? C37 C38 . 1.43(2) ? C37 C41 . 1.48(2) ? C38 C42 . 1.53(2) ? Cl13 C43 . 1.75(2) ? Cl14 Cl15 . 1.473(13) ? Cl14 C43 . 1.751(9) ? Cl15 C43 . 1.781(9) ? Cl16 C44 . 1.762(10) ? Cl16 C45 . 1.812(10) ? Cl17 C44 . 1.809(10) ? Cl17 C45 . 1.766(10) ? _cod_database_code 2012533