#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007356.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_2007356 _journal_name_full 'Acta Crystallographica' _journal_year 1998 _journal_volume C54 _journal_page_first 711 _journal_page_last 712 _publ_section_title ; Tris(tert-butylcyclopentadienyl)praseodymium-\m-bromo- tris(tetrahydrofuran)lithium ; loop_ _publ_author_name 'Luo, Yunjie' 'Yao, Yingming' 'Shen, Qi' 'Sun, Jie' 'Xue, Feng' _chemical_formula_moiety 'C39 H63 O3 Br1 Li1 Pr1' _chemical_formula_sum 'C39 H63 O3 Br1 Li1 Pr1' _chemical_formula_iupac '[Li Pr Br (C9 H13)3 (C4 H8 O)3]' _chemical_formula_weight 807.68 _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 11.905(4) _cell_length_b 12.337(3) _cell_length_c 14.218(4) _cell_angle_alpha 88.17(2) _cell_angle_beta 80.50(3) _cell_angle_gamma 84.52(2) _cell_volume 2049.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.308 _diffrn_ambient_temperature 293 _refine_ls_R_factor_obs .0388 _refine_ls_wR_factor_obs .0861 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 Pr1 .08598(4) .27611(4) .30082(3) .0633(2) Uani d ? 1 ? Pr Br1 .24531(9) .10434(8) .19163(7) .1021(3) Uani d ? 1 ? Br C1 .2140(7) .4270(6) .1646(5) .072(2) Uani d D 1 ? C C2 .1098(8) .4822(6) .2035(7) .096(3) Uani d D 1 ? C H2 .0509(8) .5061(6) .1702(7) .116 Uiso calc R 1 ? H C3 .1085(11) .4952(8) .2984(8) .181(7) Uani d DU 1 ? C H3 .0482(11) .5290(8) .3405(8) .217 Uiso calc R 1 ? H C4 .2068(13) .4523(11) .3212(8) .206(8) Uani d DU 1 ? C H4 .2274(13) .4519(11) .3815(8) .247 Uiso calc R 1 ? H C5 .2726(8) .4088(8) .2416(8) .120(4) Uani d D 1 ? C H5 .3453(8) .3727(8) .2389(8) .144 Uiso calc R 1 ? H C6 .2641(9) .4153(7) .0610(7) .117(4) Uani d D 1 ? C C7 .2132(17) .3425(15) .0052(13) .131(10) Uani d PDU .50 1 C H7A .2050(17) .2743(15) .0390(13) .197 Uiso calc PR .50 1 H H7B .2617(17) .3303(15) -.0552(13) .197 Uiso calc PR .50 1 H H7C .1394(17) .3746(15) -.0049(13) .197 Uiso calc PR .50 1 H C8 .3876(14) .3588(16) .0745(14) .146(10) Uani d PDU .50 1 C H8A .4236(14) .4052(16) .1111(14) .218 Uiso calc PR .50 1 H H8B .4341(14) .3472(16) .0131(14) .218 Uiso calc PR .50 1 H H8C .3791(14) .2900(16) .1073(14) .218 Uiso calc PR .50 1 H C9 .284(2) .5262(13) .0192(16) .128(11) Uani d PDU .50 1 C H9A .317(2) .5667(13) .0620(16) .192 Uiso calc PR .50 1 H H9B .212(2) .5636(13) .0095(16) .192 Uiso calc PR .50 1 H H9C .334(2) .5193(13) -.0408(16) .192 Uiso calc PR .50 1 H C7' .1514(15) .432(2) .0147(14) .189(14) Uani d PDU .50 2 C H7'1 .1710(15) .426(2) -.0533(14) .284 Uiso calc PR .50 2 H H7'2 .1128(15) .502(2) .0305(14) .284 Uiso calc PR .50 2 H H7'3 .1020(15) .376(2) .0389(14) .284 Uiso calc PR .50 2 H C8' .327(3) .3103(15) .020(2) .34(3) Uani d PDU .50 2 C H8'1 .352(3) .3203(15) -.047(2) .512 Uiso calc PR .50 2 H H8'2 .277(3) .2532(15) .030(2) .512 Uiso calc PR .50 2 H H8'3 .392(3) .2910(15) .051(2) .512 Uiso calc PR .50 2 H C9' .333(2) .5113(16) .024(2) .132(12) Uani d PDU .50 2 C H9'1 .363(2) .5016(16) -.042(2) .198 Uiso calc PR .50 2 H H9'2 .394(2) .5148(16) .060(2) .198 Uiso calc PR .50 2 H H9'3 .283(2) .5778(16) .032(2) .198 Uiso calc PR .50 2 H C10 .1893(7) .1718(7) .4611(5) .077(2) Uani d D 1 ? C C11 .1562(9) .2795(7) .4844(6) .100(3) Uani d D 1 ? C H11 .2057(9) .3316(7) .4911(6) .120 Uiso calc R 1 ? H C12 .0405(11) .2976(9) .4959(6) .133(5) Uani d DU 1 ? C H12 -.0017(11) .3635(9) .5125(6) .160 Uiso calc R 1 ? H C13 -.0035(8) .2041(10) .4795(6) .111(4) Uani d D 1 ? C H13 -.0807(8) .1948(10) .4829(6) .133 Uiso calc R 1 ? H C14 .0863(9) .1248(7) .4566(6) .094(3) Uani d D 1 ? C H14 .0802(9) .0532(7) .4411(6) .113 Uiso calc R 1 ? H C15 .3049(8) .1081(10) .4632(7) .130(4) Uani d D 1 ? C C16 .3274(9) .1008(11) .5644(7) .172(6) Uani d DU 1 ? C H16A .2657(9) .0687(11) .6042(7) .258 Uiso calc R 1 ? H H16B .3331(9) .1725(11) .5864(7) .258 Uiso calc R 1 ? H H16C .3977(9) .0566(11) .5670(7) .258 Uiso calc R 1 ? H C17 .3992(8) .1581(10) .3960(9) .156(5) Uani d DU 1 ? C H17A .3813(8) .1609(10) .3325(9) .234 Uiso calc R 1 ? H H17B .4703(8) .1145(10) .3968(9) .234 Uiso calc R 1 ? H H17C .4057(8) .2304(10) .4161(9) .234 Uiso calc R 1 ? H C18 .3037(11) -.0115(9) .4296(9) .179(6) Uani d DU 1 ? C H18A .2896(11) -.0103(9) .3650(9) .269 Uiso calc R 1 ? H H18B .2444(11) -.0463(9) .4701(9) .269 Uiso calc R 1 ? H H18C .3763(11) -.0512(9) .4331(9) .269 Uiso calc R 1 ? H C19 -.1586(7) .3087(7) .2834(6) .084(3) Uani d D 1 ? C C20 -.0940(8) .3253(7) .1934(6) .098(3) Uani d D 1 ? C H20 -.0914(8) .3916(7) .1604(6) .118 Uiso calc R 1 ? H C21 -.0348(8) .2287(10) .1612(7) .118(4) Uani d D 1 ? C H21 .0144(8) .2186(10) .1035(7) .142 Uiso calc R 1 ? H C22 -.0608(9) .1519(8) .2279(9) .122(4) Uani d D 1 ? C H22 -.0323(9) .0790(8) .2239(9) .146 Uiso calc R 1 ? H C23 -.1356(8) .1972(8) .3025(7) .104(3) Uani d D 1 ? C H23 -.1663(8) .1601(8) .3573(7) .124 Uiso calc R 1 ? H C24 -.2508(8) .3862(9) .3382(7) .118(4) Uani d D 1 ? C C25 -.248(2) .403(3) .4437(11) .218(19) Uani d PDU .50 1 C H25A -.311(2) .454(3) .4693(11) .327 Uiso calc PR .50 1 H H25B -.178(2) .431(3) .4506(11) .327 Uiso calc PR .50 1 H H25C -.254(2) .335(3) .4776(11) .327 Uiso calc PR .50 1 H C26 -.228(2) .5010(14) .2896(16) .183(15) Uani d PDU .50 1 C H26A -.284(2) .5558(14) .3203(16) .275 Uiso calc PR .50 1 H H26B -.235(2) .4987(14) .2232(16) .275 Uiso calc PR .50 1 H H26C -.153(2) .5179(14) .2957(16) .275 Uiso calc PR .50 1 H C27 -.3768(15) .373(3) .3300(19) .192(18) Uani d PDU .50 1 C H27A -.4262(15) .426(3) .3679(19) .287 Uiso calc PR .50 1 H H27B -.3951(15) .301(3) .3525(19) .287 Uiso calc PR .50 1 H H27C -.3870(15) .382(3) .2646(19) .287 Uiso calc PR .50 1 H C25' -.293(2) .324(2) .4316(13) .207(18) Uani d PDU .50 2 C H25D -.310(2) .253(2) .4168(13) .310 Uiso calc PR .50 2 H H25E -.360(2) .363(2) .4655(13) .310 Uiso calc PR .50 2 H H25F -.234(2) .317(2) .4706(13) .310 Uiso calc PR .50 2 H C26' -.223(3) .4964(17) .359(2) .27(2) Uani d PDU .50 2 C H26D -.289(3) .5360(17) .394(2) .409 Uiso calc PR .50 2 H H26E -.199(3) .5344(17) .300(2) .409 Uiso calc PR .50 2 H H26F -.162(3) .4902(17) .396(2) .409 Uiso calc PR .50 2 H C27' -.3510(15) .3917(19) .2830(15) .118(10) Uani d PDU .50 2 C H27D -.3672(15) .3192(19) .2707(15) .177 Uiso calc PR .50 2 H H27E -.3316(15) .4301(19) .2236(15) .177 Uiso calc PR .50 2 H H27F -.4172(15) .4292(19) .3200(15) .177 Uiso calc PR .50 2 H Li1 .2405(11) -.0888(12) .1468(9) .095(5) Uani d D 1 ? Li O1 .3421(6) -.1915(5) .2050(5) .109(2) Uani d DU 1 ? O C28 .4552(10) -.1732(9) .2083(11) .172(6) Uani d DU 1 ? C H28A .4577(10) -.1058(9) .2409(11) .206 Uiso calc R 1 ? H H28B .4974(10) -.1674(9) .1442(11) .206 Uiso calc R 1 ? H C29 .5049(10) -.2629(12) .2584(12) .201(6) Uani d DU 1 ? C H29A .5766(10) -.2921(12) .2213(12) .241 Uiso calc R 1 ? H H29B .5201(10) -.2391(12) .3191(12) .241 Uiso calc R 1 ? H C30 .4301(11) -.3402(10) .2728(13) .214(7) Uani d DU 1 ? C H30A .4238(11) -.3684(10) .3377(13) .256 Uiso calc R 1 ? H H30B .4557(11) -.4000(10) .2295(13) .256 Uiso calc R 1 ? H C31 .3228(9) -.2897(8) .2556(11) .165(5) Uani d DU 1 ? C H31A .2872(9) -.3373(8) .2186(11) .198 Uiso calc R 1 ? H H31B .2722(9) -.2753(8) .3155(11) .198 Uiso calc R 1 ? H O2 .0934(5) -.1443(5) .1751(4) .107(2) Uani d DU 1 ? O C32 .0247(11) -.1719(13) .1121(7) .183(6) Uani d DU 1 ? C H32A .0653(11) -.2268(13) .0686(7) .219 Uiso calc R 1 ? H H32B .0023(11) -.1084(13) .0751(7) .219 Uiso calc R 1 ? H C33 -.0750(10) -.2137(13) .1680(10) .181(6) Uani d DU 1 ? C H33A -.1442(10) -.1784(13) .1487(10) .218 Uiso calc R 1 ? H H33B -.0735(10) -.2915(13) .1593(10) .218 Uiso calc R 1 ? H C34 -.0720(11) -.1921(14) .2604(9) .189(6) Uani d DU 1 ? C H34A -.0925(11) -.2545(14) .3005(9) .227 Uiso calc R 1 ? H H34B -.1264(11) -.1305(14) .2811(9) .227 Uiso calc R 1 ? H C35 .0386(10) -.1685(11) .2686(7) .142(4) Uani d DU 1 ? C H35A .0796(10) -.2305(11) .2953(7) .170 Uiso calc R 1 ? H H35B .0358(10) -.1066(11) .3096(7) .170 Uiso calc R 1 ? H O3 .2891(7) -.0947(5) .0109(4) .128(3) Uani d DU 1 ? O C36 .306(3) -.1882(13) -.0450(15) .170(10) Uani d PDU .50 1 C H36A .347(3) -.2467(13) -.0135(15) .204 Uiso calc PR .50 1 H H36B .232(3) -.2116(13) -.0526(15) .204 Uiso calc PR .50 1 H C37 .368(3) -.1662(16) -.1339(14) .166(10) Uani d PDU .50 1 C H37A .444(3) -.2036(16) -.1399(14) .199 Uiso calc PR .50 1 H H37B .331(3) -.1908(16) -.1839(14) .199 Uiso calc PR .50 1 H C38 .374(3) -.0559(19) -.1416(13) .186(11) Uani d PDU .50 1 C H38A .322(3) -.0238(19) -.1823(13) .224 Uiso calc PR .50 1 H H38B .451(3) -.0400(19) -.1694(13) .224 Uiso calc PR .50 1 H C39 .345(3) -.0124(15) -.0483(14) .180(10) Uani d PDU .50 1 C H39A .294(3) .0537(15) -.0490(14) .216 Uiso calc PR .50 1 H H39B .413(3) .0046(15) -.0246(14) .216 Uiso calc PR .50 1 H C36' .362(2) -.1664(16) -.0505(14) .177(10) Uani d PDU .50 2 C H36C .328(2) -.2341(16) -.0536(14) .213 Uiso calc PR .50 2 H H36D .434(2) -.1826(16) -.0274(14) .213 Uiso calc PR .50 2 H C37' .380(3) -.116(2) -.1417(14) .168(10) Uani d PDU .50 2 C H37C .460(3) -.102(2) -.1586(14) .201 Uiso calc PR .50 2 H H37D .363(3) -.164(2) -.1890(14) .201 Uiso calc PR .50 2 H C38' .311(2) -.0200(19) -.1395(12) .150(9) Uani d PDU .50 2 C H38C .263(2) -.0192(19) -.1890(12) .179 Uiso calc PR .50 2 H H38D .357(2) .0414(19) -.1506(12) .179 Uiso calc PR .50 2 H C39' .242(2) -.0123(16) -.0500(12) .134(8) Uani d PDU .50 2 C H39C .164(2) -.0247(16) -.0549(12) .161 Uiso calc PR .50 2 H H39D .242(2) .0595(16) -.0242(12) .161 Uiso calc PR .50 2 H 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 _atom_site_aniso_type_symbol Pr1 .0841(3) .0520(2) .0544(2) -.0148(2) -.0070(2) -.0090(2) Pr Br1 .1255(8) .0760(6) .0974(7) -.0041(6) .0060(6) -.0307(5) Br C1 .089(6) .054(5) .073(5) -.007(5) -.016(5) .010(4) C C2 .114(8) .038(5) .126(8) -.002(5) .010(6) .006(5) C C3 .293(17) .069(7) .146(11) -.086(9) .116(11) -.072(7) C C4 .355(18) .205(14) .110(10) -.235(14) -.080(12) .038(9) C C5 .108(8) .117(8) .147(10) -.058(7) -.040(8) .053(8) C C6 .146(10) .102(8) .087(8) -.021(7) .033(7) .022(6) C C7 .23(3) .103(16) .056(12) -.032(18) .016(15) -.061(12) C C8 .14(2) .15(2) .119(18) -.029(18) .066(16) -.072(16) C C9 .16(2) .16(2) .051(13) -.044(18) .034(15) .028(14) C C7' .29(4) .23(3) .050(13) -.15(3) .037(18) -.029(18) C C8' .61(8) .12(2) .16(3) .15(4) .22(4) .03(2) C C9' .12(2) .13(2) .15(3) -.052(16) -.017(18) .046(19) C C10 .078(6) .089(6) .062(5) .002(5) -.014(4) .005(5) C C11 .155(10) .082(7) .072(6) -.015(7) -.037(6) -.013(5) C C12 .174(12) .150(11) .053(6) .085(10) -.003(7) -.016(7) C C13 .082(7) .177(12) .065(6) .006(8) -.005(5) .036(7) C C14 .138(9) .069(6) .080(6) -.024(6) -.027(6) .030(5) C C15 .078(7) .191(12) .113(9) .041(8) -.024(6) .013(8) C C16 .117(9) .253(16) .146(11) .059(10) -.067(8) -.009(11) C C17 .060(7) .192(13) .217(14) -.002(8) -.031(8) .000(11) C C18 .201(14) .124(10) .190(14) .064(10) -.012(11) -.004(10) C C19 .091(6) .090(7) .079(6) -.010(5) -.032(5) .003(5) C C20 .142(9) .093(7) .075(6) -.033(6) -.053(6) .020(5) C C21 .121(9) .146(10) .099(8) -.020(8) -.039(6) -.048(8) C C22 .117(9) .092(8) .170(12) -.023(7) -.052(9) -.034(8) C C23 .096(7) .102(8) .125(9) -.048(6) -.035(6) .027(7) C C24 .098(8) .138(10) .119(9) .011(7) -.034(7) -.020(8) C C25 .21(3) .32(5) .103(19) .13(3) -.04(2) -.12(2) C C26 .21(3) .102(19) .21(3) .03(2) .05(3) -.08(2) C C27 .10(2) .31(4) .17(3) -.06(2) .021(19) -.10(3) C C25' .15(3) .34(5) .11(2) .15(3) -.038(18) -.09(3) C C26' .21(4) .24(3) .38(5) .00(3) -.05(4) -.28(4) C C27' .073(15) .14(2) .13(2) .077(15) -.031(14) -.015(15) C Li1 .118(12) .081(10) .082(10) -.011(9) .003(9) -.012(8) Li O1 .114(5) .072(4) .146(6) -.016(4) -.034(4) .020(4) O C28 .142(11) .129(10) .243(15) -.031(9) -.021(11) .014(10) C C29 .157(12) .177(14) .292(17) -.009(11) -.112(12) .022(13) C C30 .142(11) .148(12) .369(19) -.020(10) -.108(13) .089(13) C C31 .148(10) .089(8) .269(15) -.025(8) -.065(10) .055(9) C O2 .132(5) .122(5) .072(4) -.047(4) -.015(4) -.003(4) O C32 .185(12) .276(16) .091(8) -.066(12) -.002(9) -.043(10) C C33 .152(11) .232(14) .175(13) -.075(11) -.036(11) -.006(12) C C34 .165(13) .238(15) .153(12) -.036(12) .010(11) .029(12) C C35 .145(10) .189(12) .087(8) -.040(9) .004(8) .015(8) C O3 .207(7) .079(4) .081(4) -.003(5) .020(5) -.011(4) O C36 .23(2) .082(13) .164(18) -.060(15) .098(17) -.032(13) C C37 .24(2) .131(18) .121(16) -.045(17) .006(16) -.047(15) C C38 .24(2) .18(2) .122(16) -.05(2) .042(17) -.030(17) C C39 .24(2) .163(17) .125(16) -.054(18) .019(18) -.039(15) C C36' .25(2) .099(15) .136(16) -.024(16) .103(17) -.007(14) C C37' .24(2) .12(2) .119(16) -.04(2) .045(16) -.021(16) C C38' .18(2) .160(18) .112(15) -.016(16) -.028(15) .011(15) C C39' .20(2) .107(14) .081(13) .037(15) -.005(15) .016(12) C 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 Pr1 Br1 . 2.9950(10) Yes Pr1 Cp1 . 2.602(7) Yes Pr1 Cp2 . 2.585(8) Yes Pr1 Cp3 . 2.589(7) Yes Pr1 C3 . 2.741(10) No Pr1 C13 . 2.742(9) No Pr1 C21 . 2.743(9) No Pr1 C12 . 2.754(9) No Pr1 C4 . 2.766(12) No Pr1 C22 . 2.773(10) No Pr1 C20 . 2.839(8) No Pr1 C14 . 2.851(7) No Pr1 C2 . 2.871(7) No Pr1 C11 . 2.872(8) No Pr1 C5 . 2.884(9) No Pr1 C23 . 2.894(9) No Pr1 C19 . 2.952(8) No Pr1 C10 . 2.966(7) No Pr1 C1 . 2.980(7) No Br1 Li1 . 2.495(15) Yes C1 C2 . 1.394(10) No C1 C5 . 1.394(11) No C1 C6 . 1.501(11) No C2 C3 . 1.361(12) No C3 C4 . 1.32(2) No C4 C5 . 1.359(13) No C6 C7 . 1.453(14) No C6 C9 . 1.497(15) No C6 C8' . 1.52(2) No C6 C9' . 1.53(2) No C6 C7' . 1.58(2) No C6 C8 . 1.60(2) No C10 C11 . 1.383(10) No C10 C14 . 1.417(10) No C10 C15 . 1.523(11) No C11 C12 . 1.357(12) No C12 C13 . 1.354(13) No C13 C14 . 1.383(11) No C15 C16 . 1.504(12) No C15 C17 . 1.514(12) No C15 C18 . 1.567(13) No C19 C20 . 1.399(10) No C19 C23 . 1.405(10) No C19 C24 . 1.513(12) No C20 C21 . 1.376(11) No C21 C22 . 1.340(12) No C22 C23 . 1.364(11) No C24 C26' . 1.48(2) No C24 C25 . 1.53(2) No C24 C27' . 1.527(15) No C24 C25' . 1.55(2) No C24 C27 . 1.55(2) No C24 C26 . 1.58(2) No Li1 O2 . 1.918(13) Yes Li1 O3 . 1.924(13) Yes Li1 O1 . 1.929(14) Yes O1 C28 . 1.395(11) No O1 C31 . 1.407(10) No C28 C29 . 1.430(13) No C29 C30 . 1.354(14) No C30 C31 . 1.422(12) No O2 C32 . 1.379(11) No O2 C35 . 1.416(9) No C32 C33 . 1.444(13) No C33 C34 . 1.356(14) No C34 C35 . 1.399(13) No O3 C36' . 1.40(2) No O3 C36 . 1.40(2) No O3 C39 . 1.44(2) No O3 C39' . 1.447(14) No C36 C37 . 1.39(2) No C37 C38 . 1.37(2) No C38 C39 . 1.42(2) No C36' C37' . 1.41(2) No C37' C38' . 1.38(2) No C38' C39' . 1.40(2) No