Synthesis and characterization of mononuclear bis(aryldiazenido)-molybdenum complexes. Crystal structures of [Mo(NNC6HR-p)2-(acac)2] (R = Me and OMe)

Li-Kao, J.; Bustos, Carlos; Carrillo, David; Robert, Françis; Gouzerh, Pierre

doi:10.1007/bf00207943

Cited by 11 publications

(4 citation statements)

References 22 publications

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“…The synthesis of the title compound, (I), was undertaken as part of our current research (Carrillo, Gouzerh & Jeannin, 1985;Bustos et al 1991;Carrillo, Robert (C6H16N) , 1992;Debenjak, Bustos, Carrillo, Robert & Gouzerh, 1992a,b;Li-Kao, Bustos, Carrillo, Robert & Gouzerh, 1993). The purpose was to obtain a new precursor for the preparation of molybdenum complexes containing organo-dinitrogen ligands, for use as models of the postulated intermediates in the convertion of coordinated dinitrogen into ammonia (Henderson, Leigh & Picket, 1983;Leigh, 1992).…”

Section: Commentmentioning

confidence: 99%

Bis(triethylammonium) Bis(2-mercaptobenzoato-O,S)dioxomolybdate(VI)

Li-Kao¹,

González²,

Baggio³

et al. 1995

Acta Crystallogr C

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Anorg. Allg. Chem. 608, 100-114. CommentThe synthesis of the title compound, (I), was undertaken as part of our current research (Carrillo, Gouzerh & Jeannin, 1985;Bustos et al. 1991; Carrillo, Robert © 1995 , 1992; Debenjak, Bustos, Carrillo, Robert & Gouzerh, 1992a,b;Li-Kao, Bustos, Carrillo, Robert & Gouzerh, 1993). The purpose was to obtain a new precursor for the preparation of molybdenum complexes containing organo-dinitrogen ligands, for use as models of the postulated intermediates in the convertion of coordinated dinitrogen into ammonia (Henderson, Leigh & Picket, 1983;Leigh, 1992).The complex is dianionic in nature ( Fig. 1) and shows monomeric units composed of two mercaptobenzoate ligands coordinated to a cis-Mo02 core through atoms S1, $2, 03 and 05. The coordination sphere around the Mo vt ion is best described as a slightly distorted octahedron, where the basal plane is defined by Mo---O1 The apical sites are occupied by atoms S1 and $2 of the organic anion, 5 ° away from the vertical due to the strain imposed by the close chelate structure. The anion presents a non-crystallographic twofold axis which bisects the Ol~Mo---O2 and O3~Mo---05 angles. These structural characteristics are similar• cc,'~ c20 Fig. 1. View of the title molecule showing the atom-labelling scheme. Displacement ellipsoids are shown at the 40% probability level. H atoms are omitted for clarity, except for those involved in strong hydrogen bonds.to those found in closely related compounds, mainly in (NHn)2[MoO2{O2CC(S)Ph2}2].2H20 (Palanca et al., 1990). The structure is completed by two Et3NH ÷ cations, the geometry of which posed some problems in the early stages of refinement. A soft similarity restraint applied to the C---C and CmN bond lengths was enough to stabilize the convergence. The resulting geometry was fairly regular, showing a strong coupling to the anion through two rather short hydrogen-bonded contacts ( Fig. 1) (04...H1AmN1, estimated length/angle 1.86/~d175°; O6.--H2A~N2, estimated length/angle 1.80/~/171°), leading to somewhat independent neutral units connected to one another only through coulombian interactions (Fig. 2). ExperimentalThe title compound was prepared by reaction of 10 mmol 1.478 (9) CI0---CI 1 i.376 (9) N I---C!51.479(9) CI 1---C12 1.371 (10) N2--C211.477 (7) C12----C13 1.394 (9) N2---C231.481 (7) CI 3------CIA 1.403 (8) N2---C251.485 (8) C15---C16 1.505 (10) O3---CI 1.250 (7) C17---C18 1.514 (10) O4----CI 1.254 (7) Ci9---C20 1.502 (10) O5---C81.270 (7) C21----C22 1.506 (10) O6---C81.251 (7) C23----C24 1.505 (10) C 1----C21.499 (8) C25---C26 1.507 (10) The structure was solved through a combination of direct methods and difference Fourier synthesis using the

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Section: Commentmentioning

confidence: 99%

Bis(triethylammonium) Bis(2-mercaptobenzoato-O,S)dioxomolybdate(VI)

Li-Kao¹,

González²,

Baggio³

et al. 1995

Acta Crystallogr C

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“…We have previously used Pt 21 and Au 17-19 complexes with basic hydroxo or oxo ligands in the formation of hydrazido complexes. Others have used basic alkyl, 33 oxo, [34][35][36][37][38][39][40] (29) and amido 41 ligand complexes to produce mostly terminal hydrazido complexes. One of the notable features of the reactions in the current study is the product variation with the substituents on the hydrazine.…”

Section: Discussionmentioning

confidence: 99%

“…We have previously used Pt 21 and Au 17-19 complexes with basic hydroxo or oxo ligands in the formation of hydrazido complexes. Others have used basic alkyl, oxo, − and amido ligand complexes to produce mostly terminal hydrazido complexes.…”

Section: Discussionmentioning

confidence: 99%

Platinum(II) Hydrazido Complexes

Xia

Sharp

2001

Inorg. Chem.

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Reaction of 1,2-dimethylhydrazine with the platinum hydroxo complex [(dppp)Pt(mu-OH)](2)(BF(4))(2) gives the bridging 1,2-dimethylhydrazido(-2) product [(dppp)(2)Pt(2)(mu-eta(2):eta(2)-MeNNMe)](BF(4))(2) 1. Crystals of 1.CH(2)Cl(2) from CH(2)Cl(2)/Et(2)O are monoclinic (C/2) with a = 19.690(1), b = 18.886(1), c = 17.170 (1) A, and beta = 92.111(1) degrees. Treatment of [(dppp)Pt(mu-OH)](2)(OTf)(2) with 1,1-dimethylhydrazine gives [(dppp)(2)Pt(2)(mu-OH)(mu-NHNMe(2))](OTf)(2) 2. Crystals of 2.CH(2)Cl(2) from CH(2)Cl(2)/Et(2)O are triclinic (P-1) with a = 12.910 (3), b = 13.927(3), c = 17.5872 (3) A, alpha = 87.121(3), beta = 89.997(4), and gamma = 84.728(3) degrees. Reaction of [(dppp)Pt(mu-OH)](2)(OTf)(2) with 1 equiv of phenylhydrazine in CH(2)Cl(2) gives [(dppp)(2)Pt(2)(mu-OH)(mu-NHNHPh)](OTf)(2) 3. Two equivalents of phenylhydrazine with [(dppp)Pt(mu-OH)](2)(X)(2) gives [(dppp)Pt(mu-NHNHPh)](2)(X)(2) 4 (X = BF(4), OTf). Crystals of 3.ClCH(2)CH(2)Cl from ClCH(2)CH(2)Cl/(i)()Pr(2)O are monoclinic (P2(1)/n) with a = 20.990(2), b = 13.098(1), c = 25.773 (2) A, and beta = 112.944(2) degrees. Crystals of 4(X = BF(4)).ClCH(2)CH(2)Cl(.)()2((t)()BuOMe) from ClCH(2)CH(2)Cl/(t)()BuOMe are monoclinic (C2/m) with a = 30.508(1), b = 15.203(1), c = 19.049 (1) A, and beta = 118.505(2) degrees.

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“…25, 177-181. Li-Kao, J., Bustos, C., Carrillo, D., Robert, F. & Gouzerh, P. (1993).Transition Met. Chem.…”

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[(η6-C6H3Me3)Ru(D-pen)]2Cl2.4H2O

Capper¹,

Davies²,

Fawcett³

et al. 1995

Acta Crystallogr C

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The authors would like to thank Fundaci6n Andes for the purchase of the single-crystal diffractometer currently operating at the Universidad de Chile. JLK and DC acknowledge financial support from FONDECYT, grants 2930010 and 91/0556, respectively. JLK is grateful to Universidad of Atacama for a graduate fellowship. H10NO2S)2(r/6-C9HI2)2]C12.4H20, contains tridentate anionic amino acid ligands, where the S atoms adopt bridging positions between the two Ru atoms resulting in a near planar Ru--SmRu--S ring. The coordination at each Ru atom is completed by an amino N atom of the chelating ligand and the r/6-bonded mesitylene ring.Lists of structure factors, anisotropic displacement parameters, Hatom coordinates, complete geometry, including torsion angles and contact distances, have been deposited with the IUCr (Reference: BK1032). Copies may be obtained through The Managing Editor, International Union of Crystallography, 5 Abbey Square, Chester CH 1 2HU, England. ReferencesBustos, C., Manzur, C., Gonz~ilez, H., Schreberg, R., Carrillo, D., Bois, C., Jeannin, Y. & Gouzerh, P. (1991). lnorg. Chim. Acta, 185, 25-31. Carrillo, D., Gouzerh, P. & Jeannin, Y. (1985). Nouv. J. Chim. 9, 749-755. Carrillo, D., Robert, F. & Gouzerh, P. (1992). lnorg. Chim. Acta, 197, 209-215. Debenjak, B., Bustos, C., Carrillo, D., Robert, F. & Gouzerh, P. (1992a). Bol. Soc. Chil. Quim. 37, 105-113. Debenjak, B., Bustos, C., Carrillo, D., Robert, F. & Gouzerh, P. (1992b). Polyhedron, 11, 2321-2326. Henderson, B. A., Leigh, G. J. & Picket, C. J. (1983. Adv. lnorg. Radiochem. 27, 197-203. Leigh, G. J. (1992). Acc. Chem. Res. 25, 177-181. Li-Kao, J., Bustos, C., Carrillo, D., Robert, F. & Gouzerh, P. (1993).Transition Met. Chem. 18, 265-270. Palanca, P., Picher, T., Sanz, V., G6mez-Romero, P., Llopis, E., Domenech, A. & Cervilla, A. (1990 CommentThe determination of the structure of the title compound (1) was undertaken as part of a study of organometallic complexes with biologically important ligands (Carter, Davies, Fawcett & Russell, 1993 Compound (1) is analogous to the r/6-benzeneruthenium(II)-l-penicillamine complex (2) reported by Sheldrick & Heeb (1989), the most significant difference being that compound (1) has four water molecules associated with each dimeric cation, where only one was found for (2). The central four-membered Ru--S--Ru--S ring, while essentially planar ( Fig. 1) with deviations from the best least-squares plane of -0.15 for Ru (1) excluded from the refinement. However, the arrangement of the O atoms of the water molecules is consistent with a continuous hydrogen-bonded chain with O...O distances in the range 2.768-2.979 A. The threedimensional hydrogen-bonded network is completed by contacts between the atoms 0(5) and 0(6) of the water molecules and the carbonyl atoms 0(2) (2.825 ~,) and 0(3) (2.798/~), respectively. 0(4) = .= CI(1) .~O (7) C (7) ExperimentalThe complex was prepared by refluxing a 2:2:1 mixture of Dpenicillamine, sodium methoxide and [(r/6-C6H3Me3)RuC12]2 in a 50:50 methanol/water solutio...

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Synthesis and characterization of mononuclear bis(aryldiazenido)-molybdenum complexes. Crystal structures of [Mo(NNC6HR-p)2-(acac)2] (R = Me and OMe)

Cited by 11 publications

References 22 publications

Bis(triethylammonium) Bis(2-mercaptobenzoato-O,S)dioxomolybdate(VI)

Bis(triethylammonium) Bis(2-mercaptobenzoato-O,S)dioxomolybdate(VI)

Platinum(II) Hydrazido Complexes

[(η6-C6H3Me3)Ru(D-pen)]2Cl2.4H2O

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