One of a series of compounds obtained by the reaction of chloropentacarbonylrhenium (1) with [3-diketones has been shown by single crystal X-ray diffraction to be bis(p-0-1,3-diphenylpropane-1,3-dionatotricarbonylrhenium(1)f. The crystals are monoclinic with lattice parameters a = 11.988(A) A, b = 14.441(9) A, c = 10.298(7) A, = 115.25(7)'. The space group is PZ,!c and there are two dimers per unit cell. A total of 1563 independent reflections were measured on a single crystal X-ray diffractometer and the structure was refined by least squares analysis to a weighted R, value of 0.0427. The dimer units are held together by two bridging oxygen atoms, one from each of the a-ketoenolate groups; the distance of the bridging oxygen from the rhenium atom to which it is chelated (2.162(9) A) is shorter than the distance to the other rhenium atom (2.204(7) A). The main part of the B-ketoenolate ring is 37" from the OReO plane.L'un des coinposCs obtenu par la reaction du chloropentacarbonylrheni~~n~(I) sur les a-dicetones a CtC identifie par diffraction aux rayons X sur un monocristal au bis (fi-0-diphenyl-I ,3-propanedionato-1,3 tricarbonylrhenium(1)). Ees cristaux sont monocliniques, les parametres du reseau sont: a = 11.988 A, b = 14.441(9) A, c = 10.298(7) A, [3 = 115.25(7)'. Le groupe spatial est P2,lc et il y a deux dimeres par maille. Un total de 1563 reflexions independantes a ete mesure au diffractometre aux rayons X sur un monocristal, la structure a Cte raffinee par la methode des moindres carrCs jusqu'a obtention d'une valeur ponderee sur R, de 0.0427. Les dimeres dans la maille sont relies entre eux par deux atomes d'oxygeile formant un pont, chacun d'eux provenant des groupes p-~Ctoenolates; la distance de I'oxygene pont B l'atome de rl~kniun~ auquel il est chelate (2.162(9) A) est plus courte que celle qui le separe de
The title compound, [Re(CO),CI(C6HS~COH~CH~CO~CH,)]2, is one of a series of compounds obtained by the reaction of chloropentacarbonylrhenium(I) with 0-diketones and has been characterized by n.m.r. and infrared spectroscopy and single crystal X-ray diffraction. The crystals are monoclinic with lattice parameters a = 14.77(2), b = 17.98(2), c = 13.48(2) A, 0 = 124.34(9)"; C2/c, Z = 4.A total of 1293 independent reflections were measured on a single crystal X-ray diffractometer and the structure was refined by full matrix least squares analysis to a weighted R2 value of 0.0444. The dimeric halves of the molecules are held together by two chlorine atoms symmetrically bridging the rhenium atoms (Re-CI = 2.511(5) A). The structure is thus very like that of [Re(C0)4C1]2, except that two neutral 0-ketoenol molecules replace two carbon monoxide molecules (one on each rhenium) and are bonded through the ketone group (Re-0 = 2.16(1) A). The arrangement of the keto and en01 groups is such that hydrogen bonding can occur between them.Le composC mentionnk dans le titre[Re(CO),CI(C6HS .COH .CH .CO .CH3)I2 appartient a une famille de produits obtenue par rCaction du chloropentacarbonylrhCnium(I) avec des 0-dicCtones. Ce produit a CtC caractkrist par r.m.n., par spectroscopie infrarouge et par diffraction de rayons-X (monocristal). Les cristaux sont du type monoclinique ave les parametres de mailles qui suivent: a = 14.77(2), b = 17.98(2), c = 13.48(2) A, 0 = 124.34(9)"; C2/c, Z = 4. Un total de 1293 reflections indkpendantes a ttC mesurt a partir d'un diffractometre a rayons-X sur un monocristal et la structure a CtC raffinCe par une matrice des moindres carrCs jusqu'i une valeur R2 pondCree de 0.0444. Les moitiCs dimCriques des molCcules sont retenues ensemble par deux atomes de chlore impliquCes symetriquement dans un pontage avec ceux de rhenium (Re-CI = 2.511(5) A). La structure, par suite, ressemble beaucoup a celle de [Re(C0)4C1]2 a I'exception des deux molCcules neutres 0-cCtoenol qui remplacent les deux molCcules de monoxyde de carbone (une sur chaque rhCnium) et qui sont relikes a I'aide du groupe cktonique (Re-0 = 2.16(1) A). L'arrangement spatial des groupes, cetone et Cnol, est tel que la formation de ponts hydrogenes peut se produire entre eux.[Traduit par le journal]Can.
The reaction of β-diketones with Re(CO)5Cl gave compounds of stoichiometries Re2(CO)6dik2 or Re2Cl2(CO)6(dikH)2. Reaction of the former compounds with carbon monoxide at high pressure gave Re(CO)4.dik, while with donor ligands such as pyridine or triphenylphosphine they gave compounds of stoichiometry Re(CO)3dikL. With triphenylphosphine further reaction gave Re(CO)2dik[P(C6H5)3]2. Compounds were investigated by infrared spectroscopy and mass spectroscopy, and a Cotton–Kraihânzel analysis was made of the carbonyl vibrational spectra in order to get an estimate of the π-acceptor ability of the β-ketoenolate ligands.
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