#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012329.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_2012329 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 1245 _journal_page_last 1247 _publ_section_title ; The nido osmaboranes [2,2,2-(CO)(PPh~3~)~2~-nido-2-OsB~5~H~9~] and [6,6,6-(CO)(PPh~3~)~2~-nido-6-OsB~9~H~13~]. ; _space_group_IT_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _[local]_cod_cif_authors_sg_H-M 'C c' loop_ _publ_author_name 'Bould, Jonathan' 'Kennedy, John D.' 'Thomas, Rhodri Ll.' 'Rath, Nigam P.' 'Barton, Lawrence' _chemical_formula_moiety 'C37 H39 B5 O Os P2' _chemical_formula_sum 'C37 H39 B5 O Os P2' _chemical_formula_iupac '[(B5 H9 Os) (C18 H15 P)2 (C O)]' _chemical_formula_weight 805.87 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.00540(10) _cell_length_b 13.02000(10) _cell_length_c 17.24450(10) _cell_angle_alpha 90 _cell_angle_beta 105.290(10) _cell_angle_gamma 90 _cell_volume 3466.39(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _exptl_crystal_density_diffrn 1.544 _diffrn_ambient_temperature 153(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 Os2 .501120(10) .801640(10) .270890(10) .01393(3) Uani d . 1 . . Os H23 .5044 .8033 .3700 .017 Uiso d R 1 . . H P1 .60724(6) .67533(9) .26835(7) .01696(19) Uani d . 1 . . P P2 .59124(5) .94852(7) .28822(5) .01514(15) Uani d . 1 . . P O .44307(19) .7775(3) .09035(17) .0304(6) Uani d . 1 . . O C1 .5621(2) .5612(3) .2099(2) .0224(7) Uani d . 1 . . C C2 .4959(3) .5072(3) .2305(3) .0314(9) Uani d . 1 . . C H2A .4726 .5324 .2721 .038 Uiso calc R 1 . . H C3 .4640(3) .4182(4) .1915(4) .0474(13) Uani d . 1 . . C H3A .4202 .3811 .2074 .057 Uiso calc R 1 . . H C4 .4951(3) .3820(4) .1290(4) .0539(16) Uani d . 1 . . C H4A .4718 .3212 .1012 .065 Uiso calc R 1 . . H C5 .5601(3) .4345(4) .1072(3) .0466(13) Uani d . 1 . . C H5A .5824 .4091 .0650 .056 Uiso calc R 1 . . H C6 .5927(3) .5240(4) .1465(3) .0325(9) Uani d . 1 . . C H6A .6366 .5607 .1302 .039 Uiso calc R 1 . . H C7 .6679(2) .6194(3) .3641(2) .0207(7) Uani d . 1 . . C C8 .7004(2) .6852(3) .4292(2) .0229(7) Uani d . 1 . . C H8A .6910 .7572 .4231 .028 Uiso calc R 1 . . H C9 .7467(2) .6448(3) .5033(2) .0252(8) Uani d . 1 . . C H9A .7685 .6895 .5475 .030 Uiso calc R 1 . . H C10 .7609(2) .5405(3) .5125(2) .0292(8) Uani d . 1 . . C H10A .7921 .5135 .5631 .035 Uiso calc R 1 . . H C11 .7299(3) .4753(3) .4482(3) .0345(9) Uani d . 1 . . C H11A .7398 .4035 .4545 .041 Uiso calc R 1 . . H C12 .6840(3) .5146(3) .3740(2) .0302(8) Uani d . 1 . . C H12A .6635 .4694 .3298 .036 Uiso calc R 1 . . H C13 .6914(2) .7085(3) .2180(2) .0217(7) Uani d . 1 . . C C14 .6701(3) .7659(4) .1479(2) .0286(8) Uani d . 1 . . C H14A .6154 .7991 .1321 .034 Uiso calc R 1 . . H C15 .7276(3) .7760(4) .1001(3) .0348(10) Uani d . 1 . . C H15A .7121 .8146 .0517 .042 Uiso calc R 1 . . H C16 .8081(3) .7284(4) .1246(3) .0423(12) Uani d . 1 . . C H16A .8472 .7329 .0918 .051 Uiso calc R 1 . . H C17 .8318(3) .6752(4) .1957(3) .0384(11) Uani d . 1 . . C H17A .8880 .6459 .2128 .046 Uiso calc R 1 . . H C18 .7740(2) .6637(4) .2429(3) .0292(8) Uani d . 1 . . C H18A .7903 .6258 .2917 .035 Uiso calc R 1 . . H C19 .7028(2) .9426(3) .3524(2) .0185(6) Uani d . 1 . . C C20 .7169(2) .9623(3) .4342(2) .0231(7) Uani d . 1 . . C H20A .6695 .9812 .4548 .028 Uiso calc R 1 . . H C21 .7997(3) .9548(3) .4863(3) .0292(8) Uani d . 1 . . C H21A .8085 .9677 .5421 .035 Uiso calc R 1 . . H C22 .8688(3) .9286(3) .4565(3) .0333(9) Uani d . 1 . . C H22A .9255 .9246 .4916 .040 Uiso calc R 1 . . H C23 .8555(2) .9082(4) .3756(3) .0309(9) Uani d . 1 . . C H23A .9033 .8903 .3553 .037 Uiso calc R 1 . . H C24 .7727(2) .9134(3) .3231(2) .0224(7) Uani d . 1 . . C H24A .7639 .8972 .2678 .027 Uiso calc R 1 . . H C25 .5962(2) 1.0180(3) .1969(2) .0181(6) Uani d . 1 . . C C26 .6693(2) 1.0726(3) .1903(2) .0235(7) Uani d . 1 . . C H26A .7220 1.0670 .2313 .028 Uiso calc R 1 . . H C27 .6651(3) 1.1347(3) .1242(2) .0289(8) Uani d . 1 . . C H27A .7152 1.1708 .1198 .035 Uiso calc R 1 . . H C28 .5889(3) 1.1444(3) .0650(2) .0277(8) Uani d . 1 . . C H28A .5864 1.1873 .0198 .033 Uiso calc R 1 . . H C29 .5152(3) 1.0913(3) .0712(2) .0248(7) Uani d . 1 . . C H29A .4623 1.0980 .0304 .030 Uiso calc R 1 . . H C30 .5194(3) 1.0288(4) .1370(3) .0215(9) Uani d . 1 . . C H30A .4692 .9928 .1412 .026 Uiso calc R 1 . . H C31 .5505(2) 1.0522(3) .3407(2) .0184(6) Uani d . 1 . . C C32 .4913(3) 1.0363(4) .3863(3) .0223(9) Uani d . 1 . . C H32A .4660 .9705 .3871 .027 Uiso calc R 1 . . H C33 .4691(3) 1.1159(4) .4304(3) .0301(9) Uani d . 1 . . C H33A .4285 1.1041 .4610 .036 Uiso calc R 1 . . H C34 .5054(3) 1.2125(3) .4305(3) .0317(9) Uani d . 1 . . C H34A .4906 1.2662 .4617 .038 Uiso calc R 1 . . H C35 .5632(3) 1.2305(3) .3848(3) .0342(9) Uani d . 1 . . C H35A .5874 1.2969 .3839 .041 Uiso calc R 1 . . H C36 .5858(3) 1.1510(3) .3401(3) .0298(8) Uani d . 1 . . C H36A .6255 1.1638 .3088 .036 Uiso calc R 1 . . H C37 .4674(2) .7903(3) .1589(2) .0192(7) Uani d . 1 . . C B1 .3802(3) .7122(4) .2865(3) .0242(10) Uani d . 1 . . B B3 .4699(3) .7120(3) .3741(3) .0223(8) Uani d . 1 . . B B4 .3650(3) .7230(4) .3865(3) .0288(10) Uani d . 1 . . B B5 .3015(3) .7933(4) .3151(3) .0282(10) Uani d . 1 . . B B6 .3559(3) .8382(4) .2475(3) .0239(8) Uani d . 1 . . B H1 .354(3) .649(4) .251(3) .028(12) Uiso d . 1 . . H H3 .516(3) .649(4) .406(3) .024(11) Uiso d . 1 . . H H4 .352(4) .660(5) .425(3) .045(15) Uiso d . 1 . . H H5 .232(4) .791(4) .289(4) .042(16) Uiso d . 1 . . H H6 .327(3) .883(3) .192(2) .017(10) Uiso d . 1 . . H H34 .434(4) .765(5) .426(3) .043(14) Uiso d . 1 . . H H56 .319(3) .880(4) .301(3) .027(12) 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 Os2 .01132(4) .01635(5) .01419(5) -.00172(8) .00348(3) -.00039(8) P1 .0150(4) .0181(5) .0178(5) -.0003(4) .0044(3) -.0024(4) P2 .0123(3) .0178(4) .0153(4) -.0014(3) .0035(3) .0009(3) O .0271(14) .0445(19) .0183(13) -.0012(12) .0039(11) -.0027(12) C1 .0187(15) .0193(18) .0291(19) -.0027(13) .0061(14) -.0061(14) C2 .035(2) .023(2) .042(2) -.0080(16) .0205(18) -.0140(17) C3 .044(3) .037(3) .071(4) -.021(2) .031(2) -.024(2) C4 .044(3) .047(3) .081(4) -.023(2) .033(3) -.043(3) C5 .040(2) .050(3) .058(3) -.014(2) .027(2) -.031(2) C6 .0274(18) .038(2) .035(2) -.0095(17) .0139(17) -.0175(18) C7 .0194(15) .0197(17) .0233(17) .0026(13) .0059(13) -.0006(13) C8 .0225(16) .0220(19) .0237(18) .0031(13) .0049(14) .0005(14) C9 .0198(16) .033(2) .0202(17) .0023(15) .0003(13) -.0030(14) C10 .0245(18) .039(2) .0209(18) .0078(16) .0012(15) .0064(16) C11 .041(2) .024(2) .035(2) .0097(18) .0034(19) .0029(17) C12 .036(2) .023(2) .028(2) .0046(16) .0026(16) -.0025(15) C13 .0152(14) .026(2) .0250(18) -.0055(13) .0079(14) -.0098(14) C14 .0218(17) .039(2) .027(2) -.0070(17) .0087(15) -.0032(17) C15 .031(2) .046(3) .031(2) -.0153(19) .0138(18) -.0057(19) C16 .030(2) .054(3) .051(3) -.018(2) .026(2) -.022(2) C17 .0198(18) .042(3) .057(3) -.0033(17) .0164(19) -.013(2) C18 .0182(16) .030(2) .040(2) .0004(15) .0090(16) -.0068(18) C19 .0151(14) .0187(17) .0205(16) -.0042(12) .0026(12) .0021(13) C20 .0225(16) .0245(19) .0199(17) -.0008(14) .0014(14) .0004(14) C21 .0272(18) .028(2) .027(2) .0000(15) -.0025(16) -.0016(16) C22 .0205(17) .034(2) .037(2) .0029(16) -.0076(16) .0014(17) C23 .0160(15) .033(2) .041(2) .0020(15) .0031(15) -.0020(18) C24 .0170(14) .0235(18) .0258(18) .0003(13) .0043(13) -.0008(14) C25 .0180(14) .0199(17) .0170(15) -.0011(12) .0058(12) .0001(12) C26 .0181(15) .029(2) .0236(18) -.0046(14) .0063(13) .0017(14) C27 .0276(18) .029(2) .032(2) -.0061(15) .0117(16) .0076(16) C28 .037(2) .026(2) .0214(18) .0004(16) .0105(16) .0063(15) C29 .0261(17) .024(2) .0204(18) .0016(15) -.0002(15) .0035(15) C30 .0203(18) .022(2) .022(2) .0002(14) .0051(15) .0022(16) C31 .0157(14) .0229(18) .0160(15) .0009(12) .0031(12) -.0004(12) C32 .0228(18) .023(2) .023(2) -.0003(15) .0105(16) -.0032(16) C33 .0285(19) .036(2) .028(2) .0034(17) .0124(17) -.0027(18) C34 .044(2) .025(2) .028(2) .0122(17) .0128(19) -.0016(16) C35 .049(3) .0166(18) .041(2) -.0042(18) .019(2) -.0027(17) C36 .036(2) .022(2) .036(2) -.0036(16) .0181(18) -.0026(16) C37 .0118(13) .0217(18) .0233(18) -.0015(12) .0033(13) .0018(13) B1 .022(2) .024(2) .027(2) -.0070(18) .0063(18) -.0030(19) B3 .0239(18) .021(2) .024(2) -.0028(15) .0106(16) .0045(15) B4 .026(2) .030(2) .036(3) -.0044(18) .018(2) .0029(19) B5 .0177(18) .030(2) .041(3) -.0028(16) .0149(18) -.0043(19) B6 .0171(17) .030(2) .025(2) -.0003(16) .0052(15) -.0029(17) 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 Os2 C37 . 1.869(4) yes Os2 B3 . 2.291(4) yes Os2 B6 . 2.301(4) yes Os2 B1 . 2.335(5) yes Os2 P2 . 2.3664(9) yes Os2 P1 . 2.3729(11) yes Os2 H23 . 1.6961 ? P1 C7 . 1.831(4) ? P1 C1 . 1.833(4) ? P1 C13 . 1.836(4) ? P2 C25 . 1.835(3) ? P2 C19 . 1.838(3) ? P2 C31 . 1.838(4) ? O C37 . 1.155(5) yes C1 C2 . 1.393(5) ? C1 C6 . 1.399(5) ? C2 C3 . 1.369(6) ? C2 H2A . .9500 ? C3 C4 . 1.384(7) ? C3 H3A . .9500 ? C4 C5 . 1.376(7) ? C4 H4A . .9500 ? C5 C6 . 1.379(6) ? C5 H5A . .9500 ? C6 H6A . .9500 ? C7 C12 . 1.391(6) ? C7 C8 . 1.399(5) ? C8 C9 . 1.400(6) ? C8 H8A . .9500 ? C9 C10 . 1.379(6) ? C9 H9A . .9500 ? C10 C11 . 1.381(6) ? C10 H10A . .9500 ? C11 C12 . 1.394(6) ? C11 H11A . .9500 ? C12 H12A . .9500 ? C13 C14 . 1.386(6) ? C13 C18 . 1.404(5) ? C14 C15 . 1.394(6) ? C14 H14A . .9500 ? C15 C16 . 1.391(7) ? C15 H15A . .9500 ? C16 C17 . 1.371(8) ? C16 H16A . .9500 ? C17 C18 . 1.392(6) ? C17 H17A . .9500 ? C18 H18A . .9500 ? C19 C20 . 1.392(5) ? C19 C24 . 1.396(5) ? C20 C21 . 1.394(5) ? C20 H20A . .9500 ? C21 C22 . 1.381(6) ? C21 H21A . .9500 ? C22 C23 . 1.381(6) ? C22 H22A . .9500 ? C23 C24 . 1.395(5) ? C23 H23A . .9500 ? C24 H24A . .9500 ? C25 C30 . 1.388(6) ? C25 C26 . 1.399(5) ? C26 C27 . 1.384(5) ? C26 H26A . .9500 ? C27 C28 . 1.375(6) ? C27 H27A . .9500 ? C28 C29 . 1.396(6) ? C28 H28A . .9500 ? C29 C30 . 1.383(6) ? C29 H29A . .9500 ? C30 H30A . .9500 ? C31 C32 . 1.398(5) ? C31 C36 . 1.406(5) ? C32 C33 . 1.386(6) ? C32 H32A . .9500 ? C33 C34 . 1.385(6) ? C33 H33A . .9500 ? C34 C35 . 1.384(6) ? C34 H34A . .9500 ? C35 C36 . 1.393(6) ? C35 H35A . .9500 ? C36 H36A . .9500 ? B1 B6 . 1.777(7) yes B1 B3 . 1.788(7) yes B1 B5 . 1.808(7) yes B1 B4 . 1.809(8) yes B1 H1 . 1.04(5) ? B3 B4 . 1.753(6) yes B3 H23 . 1.3202 ? B3 H3 . 1.15(5) ? B3 H34 . 1.37(6) ? B4 B5 . 1.652(8) yes B4 H4 . 1.10(6) ? B4 H34 . 1.25(6) ? B5 B6 . 1.730(6) yes B5 H5 . 1.09(6) ? B5 H56 . 1.20(5) ? B6 H6 . 1.11(4) ? B6 H56 . 1.33(4) ?