#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2010741.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_2010741 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first e78 _journal_page_last e78 _publ_section_title ; Me~4~C~2~(C~5~H~4~)~2~Zr(BH~4~)~2~, a bis-tetrahydroborate complex of a bridged zirconocene ; loop_ _publ_author_name 'Schaper, Frank' 'Brintzinger, Hans-Herbert' _chemical_name_common ; tetramethylethyliden- bis(cyclopentadienyl)zirconiumbis(tetrahydroborate)' ; _chemical_formula_moiety 'C16 H28 B2 Zr' _chemical_formula_sum 'C16 H28 B2 Zr' _chemical_formula_structural '(C H3)4 C2 (C5 H4)2 Zr (H4 B)2' _chemical_formula_iupac '[Zr (B1 H4)2 (C16 H20)]' _chemical_formula_weight 333.22 _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 7.699(2) _cell_length_b 9.341(2) _cell_length_c 12.934(3) _cell_angle_alpha 77.77(3) _cell_angle_beta 78.52(3) _cell_angle_gamma 69.09(3) _cell_volume 841.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153 _exptl_crystal_density_diffrn 1.315 _diffrn_ambient_temperature 153 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 Zr1 -.25624(2) -.04144(2) .251480(10) .01553(6) Uani d . 1 . . Zr B1 -.3376(3) .1093(3) .41112(17) .0287(4) Uani d . 1 . . B B2 -.1841(4) .1515(3) .08607(18) .0336(5) Uani d . 1 . . B C1 -.4236(2) -.20897(18) .21681(13) .0178(3) Uani d . 1 . . C C2 -.5218(2) -.14160(19) .30943(14) .0194(3) Uani d . 1 . . C C3 -.6051(2) .0197(2) .27883(16) .0252(4) Uani d . 1 . . C C4 -.5545(3) .0551(2) .16936(16) .0275(4) Uani d . 1 . . C C5 -.4410(3) -.0854(2) .13072(15) .0225(3) Uani d . 1 . . C C6 -.0768(2) -.32500(19) .28687(14) .0213(3) Uani d . 1 . . C C7 -.0728(3) -.2598(2) .37514(15) .0260(4) Uani d . 1 . . C C8 .0340(3) -.1581(2) .34076(17) .0310(4) Uani d . 1 . . C C9 .0927(3) -.1568(2) .23129(17) .0299(4) Uani d . 1 . . C C10 .0223(2) -.2569(2) .19692(15) .0241(4) Uani d . 1 . . C C11 -.3233(2) -.38148(19) .21138(14) .0208(3) Uani d . 1 . . C C12 -.1650(2) -.44810(19) .28787(15) .0238(4) Uani d . 1 . . C C13 -.2445(3) -.4029(2) .09454(16) .0290(4) Uani d . 1 . . C C14 -.4730(3) -.4629(2) .24496(18) .0297(4) Uani d . 1 . . C C15 -.2425(3) -.5001(2) .40367(17) .0331(4) Uani d . 1 . . C C16 -.0067(3) -.5913(2) .2514(2) .0377(5) Uani d . 1 . . C H2 -.536(3) -.192(3) .3778(19) .027(5) Uiso d . 1 . . H H5 -.383(3) -.093(2) .0589(18) .023(5) Uiso d . 1 . . H H1A -.361(3) -.009(3) .4068(19) .034(6) Uiso d . 1 . . H H15C -.342(3) -.423(3) .4339(19) .034(6) Uiso d . 1 . . H H2B -.154(3) .016(3) .0976(19) .036(6) Uiso d . 1 . . H H10 .045(3) -.277(2) .1262(19) .027(5) Uiso d . 1 . . H H3 -.673(3) .090(3) .324(2) .035(6) Uiso d . 1 . . H H13C -.349(4) -.352(3) .048(2) .038(6) Uiso d . 1 . . H H7 -.129(3) -.277(3) .442(2) .032(6) Uiso d . 1 . . H H13B -.150(3) -.356(3) .0637(19) .035(6) Uiso d . 1 . . H H14C -.546(3) -.443(3) .315(2) .032(6) Uiso d . 1 . . H H4 -.586(3) .155(3) .1277(19) .032(6) Uiso d . 1 . . H H15B -.141(4) -.533(3) .446(2) .040(6) Uiso d . 1 . . H H13A -.192(3) -.512(3) .0913(19) .031(6) Uiso d . 1 . . H H14B -.416(3) -.564(3) .250(2) .041(7) Uiso d . 1 . . H H8 .054(3) -.103(3) .384(2) .038(6) Uiso d . 1 . . H H1C -.472(4) .202(3) .418(2) .047(7) Uiso d . 1 . . H H2D -.053(4) .173(3) .079(2) .043(7) Uiso d . 1 . . H H16C .063(3) -.567(3) .185(2) .032(6) Uiso d . 1 . . H H2A -.278(4) .184(3) .165(2) .045(7) Uiso d . 1 . . H H15A -.280(3) -.592(3) .409(2) .040(7) Uiso d . 1 . . H H14A -.561(4) -.424(3) .194(2) .040(6) Uiso d . 1 . . H H16B .076(3) -.629(3) .304(2) .034(6) Uiso d . 1 . . H H2C -.267(4) .212(3) .022(2) .045(7) Uiso d . 1 . . H H9 .159(4) -.099(3) .187(2) .044(7) Uiso d . 1 . . H H1B -.247(3) .135(3) .330(2) .042(7) Uiso d . 1 . . H H1D -.248(4) .086(3) .473(2) .046(7) Uiso d . 1 . . H H16A -.051(4) -.669(4) .247(2) .060(9) Uiso d . 1 . . 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 Zr1 .01831(9) .01429(8) .01530(9) -.00710(6) -.00153(5) -.00270(5) B1 .0420(12) .0304(11) .0211(10) -.0204(10) .0018(9) -.0104(8) B2 .0502(14) .0258(10) .0233(11) -.0178(10) .0056(10) -.0011(8) C1 .0166(7) .0159(7) .0230(8) -.0049(6) -.0065(6) -.0042(6) C2 .0160(7) .0205(8) .0241(9) -.0082(6) -.0026(6) -.0049(7) C3 .0170(8) .0215(8) .0375(10) -.0021(7) -.0064(7) -.0107(8) C4 .0285(9) .0171(8) .0365(10) -.0016(7) -.0171(8) -.0020(7) C5 .0271(9) .0199(8) .0226(9) -.0069(7) -.0109(7) -.0019(7) C6 .0167(7) .0185(8) .0261(9) -.0010(6) -.0079(6) -.0016(6) C7 .0243(9) .0274(9) .0247(9) -.0050(7) -.0105(7) -.0001(7) C8 .0242(9) .0364(10) .0380(11) -.0092(8) -.0148(8) -.0090(9) C9 .0172(8) .0338(10) .0404(11) -.0102(7) -.0030(7) -.0070(8) C10 .0158(8) .0260(9) .0292(10) -.0042(7) -.0011(7) -.0078(7) C11 .0229(8) .0146(7) .0259(9) -.0049(6) -.0061(7) -.0047(6) C12 .0242(8) .0147(7) .0308(9) -.0032(7) -.0090(7) -.0005(7) C13 .0336(10) .0239(9) .0301(10) -.0066(8) -.0041(8) -.0108(7) C14 .0299(10) .0193(9) .0438(12) -.0117(8) -.0072(9) -.0050(8) C15 .0399(11) .0260(10) .0316(11) -.0117(9) -.0121(9) .0074(8) C16 .0322(11) .0193(9) .0571(15) .0021(8) -.0134(11) -.0080(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 Zr1 C10 . 2.463(2) ? Zr1 C2 . 2.4647(18) ? Zr1 C7 . 2.485(2) ? Zr1 C5 . 2.4911(18) ? Zr1 C9 . 2.494(2) ? Zr1 C6 . 2.5020(19) ? Zr1 C8 . 2.504(2) ? Zr1 C1 . 2.5051(17) ? Zr1 C3 . 2.5057(19) ? Zr1 C4 . 2.510(2) ? Zr1 B1 . 2.594(2) ? Zr1 B2 . 2.597(2) ? Zr1 H1A . 2.05(2) ? Zr1 H2B . 2.02(2) ? Zr1 H2A . 2.13(3) ? Zr1 H1B . 2.15(3) ? B1 H1A . 1.19(2) ? B1 H1C . 1.09(3) ? B1 H1B . 1.17(3) ? B1 H1D . 1.10(3) ? B2 H2B . 1.18(2) ? B2 H2D . 1.08(3) ? B2 H2A . 1.15(3) ? B2 H2C . 1.08(3) ? C1 C5 . 1.412(2) ? C1 C2 . 1.422(2) ? C1 C11 . 1.528(2) ? C2 C3 . 1.413(2) ? C2 H2 . .91(2) ? C3 C4 . 1.393(3) ? C3 H3 . .92(3) ? C4 C5 . 1.422(3) ? C4 H4 . .95(2) ? C5 H5 . .95(2) ? C6 C7 . 1.413(3) ? C6 C10 . 1.421(3) ? C6 C12 . 1.527(2) ? C7 C8 . 1.417(3) ? C7 H7 . .90(2) ? C8 C9 . 1.397(3) ? C8 H8 . .90(3) ? C9 C10 . 1.414(3) ? C9 H9 . .91(3) ? C10 H10 . .94(2) ? C11 C13 . 1.539(3) ? C11 C14 . 1.543(3) ? C11 C12 . 1.590(2) ? C12 C16 . 1.540(3) ? C12 C15 . 1.542(3) ? C13 H13C . 1.02(3) ? C13 H13B . .96(2) ? C13 H13A . .96(2) ? C14 H14C . .98(2) ? C14 H14B . .89(3) ? C14 H14A . .97(3) ? C15 H15C . .93(2) ? C15 H15B . .97(3) ? C15 H15A . .99(3) ? C16 H16C . .94(3) ? C16 H16B . .94(2) ? C16 H16A . .92(3) ? _cod_database_code 2010741