31355-55-2Relevant articles and documents
Improved preparations of molybdenum coordination compounds from tetrachlorobis(diethyl ether)molybdenum(IV)
Stoffelbach, Fran?ois,Saurenz, Dirk,Poli, Rinaldo
, p. 2699 - 2703 (2007/10/03)
The reduction of MoCl5 with metallic tin in diethyl ether provides a rapid and convenient entry to [MoCl4(OEt2)2] This compound can be transformed easily and in high yields into a variety of other useful synthon
Characterization and Properties of CH3C(CH2PPh2)3MoCl3
Walter, Olaf,Huttner, Gottfried,Zsolnai, Laszlo
, p. 636 - 640 (2007/10/02)
Starting from MoCl5 via the intermediates (MeCN)2MoCl4 (1) and (THF)2MoCl4 (2) the tripod complex CH3C(CH2PPh2)3MoCl3 (4) has been synthesized.The yellow cristalline compound 4 has been fully characterized by standard analytical techniques.X-ray-analysis proves the facial coordination of the tripod ligand.To our knowledge 4 is the first Mo(III)-trihalide coordination compound containing three P-donor-ligands in a facial coordination.Key Words: (Tripod)molybdenium Trichloride, Synthesis, Properties, Crystal Structure, Tripod Ligand
On the Reduction of Alkyne Complexes of Molybdenum and Tungsten in High Oxidation States. The Crystal Structure of MoCl3(THF)3
Hofacker, Peter,Friebel, Claus,Dehnicke, Kurt,Baeuml, Petra,Hiller, Wolfgang,Straehle, Joachim
, p. 1161 - 1166 (2007/10/02)
The reduction of the tungsten alkyne complexes CR)>2 (R = Ph, SiMe3) with cobaltocen in THF solutions leads to the complexes 2CR)>2 (R = Ph (1); R = SiMe3 (2)), as green, oxygen sensitive crystalline powders.Reduction of CSiMe3)>2 and of CPh)>2 with sodium naphthalide in THF solutions in the presence of 15-crown-5 gives 3, and MoCl3(THF)3, respectively.All compounds have been characterized by IR spectroscopy, and 1 and 2, in addition, by their EPR spectra.The crystal structure of MoCl3(THF)3 was determined by X-ray methods.Space group P21/c, Z = 4, 2642 observed unique reflexions, R = 0.050.Lattice dimensions at 20 deg C: a = 888.4(2), b = 1281.5(3), c = 1535.2(3) pm, β = 92.17(2) deg.The compound forms monomeric octahedral molecules with a meridional arrangement of the ligands. - Keywords: Alkyne Complexes of Molybdenum and Tungsten, Reduction, EPR Spectra, Crystal Structure, IR Spectra
The Use of (Me3Si)2NN(SiMe3)2 as a Reagent for the Synthesis of μ-Dinitrogen Complexes or as a Homogeneous One-electron Reducing Agent
Dilworth, Jonathan R.,Harrison, Stephen J.,Henderson, Richard A.,Walton, David R. M.
, p. 176 - 177 (2007/10/02)
The reaction of NbCl5 with (Me3Si)2NN(SiMe3)2, in the presence of tetrahydrofuran (thf) gives high yields (ca. 80percent) of 2N2> (A); (A), or its tantalum analogue, reacts with Me3SiS2CNEt2 to give a high yield of the dinitrogen complexes with exclusively sulphur co-ligands 2N2> (M = Nb or Ta), and reaction of (L = MeCN or thf) with (Me3Si)2NN(SiMe3)2 gives in high yield, together with N2.
Preparation and Crystal Structure of 3> and an Improved Route to
Dilworth, Jonathan R.,Zubieta, Jon A.
, p. 397 - 398 (2007/10/02)
The complex (thf = tetrahydrofuran) is prepared in high yield by the tin reduction of in thf.It reacts with in dry methanol to give 3> which crystallizes in the space group C2/c with a = 14.342(5), b = 11.239(5), c = 12.945(4) Angstroem, β = 97.12(1) deg, and Z = 4. 2 453 Reflections gave R = 0.039.The molybdenum is pseudo-octahedral and the complex has overall C2 symmetry.The Mo-S average distance is 2.507(2) Angstroem.
Tetranuclear dialkyl dithiophosphate complexes of molybdenum(V) with nitride ligands
Noble, Mark E.,Folting, Kirsten,Huffman,Wentworth
, p. 3772 - 3776 (2008/10/08)
The syntheses of the tetranuclear, ferromagnetic compounds [MoN(S2P(OR)2)2]4 (R = CH3 and C2H5) are described along with their unusual dissociative and chemical stabilities. The compound with R = CH3 crystallizes in the monoclinic space group A2/a with a = 18.632 (8) ?, b = 24.384 (12) ?, c = 12.600 (5) ?, β = 92.16 (1)°, and Z = 4 at -163°C. The structure was solved by direct methods (LSAM) using 3813 unique reflections with F > 2.33σ(F). Final residuals were R(F) = 0.082 and Rw(F) = 0.075. The chiral molecule contains a nearly square and planar [MoN]4 ring in which all bond distances are identical within experimental error. This portion of the structure contrasts markedly with the alternating triple and single bonds found in the [MoN]4 rings in the lattice of MoNCl3, and the differences in the structures are substantiated by the disparate values of ν(MoN). Explanations for the ferromagnetism are given in terms of a superexchange mechanism and molecular orbital theory.
