Synthesis, structure and electrochemistry of CO incorporated diruthenium metallacyclic compounds [Ru2(CO)6{μ-η:η:η:η-1,4-Fc2C5H2O}] and [Ru2(CO)6{μ-η:η:η:η-1,5-Fc2C5H2O}]

Ferrocenyl substituted ruthenium metallacyclic compounds, [Ru₂(CO)₆{μ-η¹:η¹:η²:η²-1,4-Fc₂C₅H₂O}] (1) and [Ru₂(CO)₆{μ-η¹:η¹:η²:η²-1,5-Fc₂C₅H₂O}] (2) have been synthesized and structurally characterized. Electrochemical studies for 1 and 2 and the respective quinone derivatives 3 and 4 show weak to no electrochemical coupling at the mixed-valent intermediate state which is dependent on the complex frameworks.     

Photochemical route to unusual tri-tungsten ferrocenylacetylene cluster [W3{μ-η,η- (H)CCFc}2(CO)12] and a dimetallacyclodecatetraene [W2{μ-η,η,η,η- (Fc)CC(H)C(H)C(Fc)C(Fc)C(H)C(H)C(Fc)}(CO)6]

Low temperature photoreaction between tungsten hexacarbonyl and ferrocenylacetylene yielded two unusual metal containing stable compounds, the tritungsten cluster, [W₃(μ-η²,η²- (H)CCFc)₂(CO)₁₂] (1), and ditungsten-1,4,5,8-ferrocenylcyclodecatetraene, [W₂{μ-η²,η²,η²,η²-(Fc)CC(H)C(H)C(Fc)C(Fc)C(H)C(H)C(Fc)}(CO)₆] (2). Both compounds were characterised by IR and ¹H and ¹³C NMR spectroscopy and their molecular structures established by single crystal X-ray diffraction methods.     

Synthesis of the cyclooctadiene and cyclooctenediyl cobalt complexes. Structures of [(η2,η2-cyclooctadiene)Co(η-1,2,4,5-C6H2Me4)]BF4 and [(η1,η3-cyclooctenediyl)Co(η-9-SMe2-7,8-C2B9H10)

Cobaltacarboranes (η¹, η³-cyclooctenediyl)Co(Carb) (Carb = η-9-SMe₂-7,8-C₂B₉H₁₀, η-1-tBuHN-1,7,9-C₃B₈H₁₀) were synthesized by the reaction of the carborane anions [Carb]⁻ with the acetonitrile complex [(η¹, η³-cyclooctenediyl)Co(MeCN)₃]⁺ generated in situ upon the dissolution of [(η¹, η³-cyclooctenediyl)Co(η-1,4-C₆H₄Me₂)]⁺ in MeCN. The structures of (η¹,η³-cyclooctenediyl)Co(η-9-SMe₂-7,8-C₂B₉H₁₀ and [(η²,η²-cyclooctadiene)Co((η-1,2,4,5-C₆H₂Me₄)]BF₄ were determined by X-ray diffraction analysis.     

Photochemical reactions of W(CO)6 with hydrosilanes: synthesis, spectroscopic characteristic, and crystal structure of W(CO)3(η-PhSiHPh2)

Photolysis of W(CO)₆ in the presence of Ph₃SiH in n-heptane leads to the formation of the first tricarbonyl(η⁶-triphenylhydrosilane)tungsten complex W(CO)₃(η⁶-PhSiHPh₂) (1) in good yield (ca. 70%). The molecular structure of the new tungsten-silane compound was established by single-crystal X-ray diffraction studies and characterized by IR, UV-Vis, ¹H, ¹³C{¹H}, and ²⁹Si{¹H} NMR spectroscopy.     

Synthesis, characterization and reactivity studies of the new compound [Os3(CO)9(μ3-η,η,η-{C5H5FeC5H3CCC(S)C(Fc)CHO}]

Processes such as S-C and C-H bond activations as well as C-C coupling reactions have taken place in the synthesis of the new compound [Os₃(CO)₉(μ₃-η²,η³,η³-{C₅H₅FeC₅H₃CCC(S)C(Fc)CHO}] (Fc = C₅H₄FeC₅H₅), which contains an aldehyde oxametallacycle. A reactivity study of it has been carried out. In addition, other new triosmium clusters such as [Os₃(CO)₉(μ₃,η²-CCFc)(μ,η¹-SCCFc)], [Os₃(CO)₁₀(μ,η²-CCFc)(μ,η¹-SCCFc)] and [Os₃(CO)₉(μ-CO)(μ₃,η²-FcCCSCCFc)] have been prepared from the reaction of [Os₃(CO)₁₀(NCMe)₂] and FcCCSCCFc. All the compounds have been characterized by analytical and spectroscopic techniques. The crystal structures of [Os₃(CO)₉(μ₃,η²-CCFc)(μ,η¹-SCCFc)] and [Os₃(CO)₉(μ₃-η²,η³,η³-{C₅H₅FeC₅H₃CCC(S)C(Fc)CHO}] have been determined by X-ray crystallography and some electrochemical studies have also carried out.     

Cyclopentadienyl chromium complexes with halide, methyl, isothiocyanate and isoselenocyanate ligands: Structures of [η-(C5H4-COOCH3)]Cr(NO)2(Br) and [η-(C5H4-COOCH3)]Cr(NO)2(NCS)

Bromination/nitrosylation of [η⁵-(carbomethoxy)cyclopentadienyl]dicarbonylnitrosylchromium (8) (hereafter called carbomethoxycynichrodene) with hydrogen bromide/isoamyl nitrite gives bromo [η⁵-(carboxymethoxy)cyclopentadienyl]dinitrosylchromium (10) in 84%. Compounds 15 in 74% and 16 in 90% were obtained from the corresponding cynichrodene derivatives via the same method. Compounds [η⁵-(carbomethoxy)cyclopentadienyl](isothiocyanato)dinitrosylchromium (13) and [η⁵-(carbomethoxy)cyclopentadienyl](isoselenocyanato)dinitrosylchromium (14) were prepared from [η⁵-(carbomethoxy)cyclopentadienyl]chlorodinitrosylchromium (9) with excess potassium thiocyanate and selenocyanate, respectively, after detaching the chloride by the action of silver nitrate. One of the nitrosyl groups in each compound is located at the site away from the exocyclic carbonyl carbon of the Cp(Cr) ring with twist angles of 168.5° and 172.3°, respectively. The chemical shifts of C(2)-C(5) carbon atoms of a series of substituted-cyclopentadienyldinitrosylchromium derivatives, [η⁵-(C₅H₄-sub)]Cr(NO)₂X, have been assigned using two-dimensional HetCOR NMR spectroscopy. The assigned chemical shifts were compared with the NMR data of their analogues of ferrocene, and the opposite correlation on the assignments was observed. The electron density distribution in the cyclopentadienyl ring is discussed on the basis of ¹³C NMR data and those of 10 and 13 are compared with the calculations via density functional B3LYP correlation-exchange method.     

Cyclopentadienyl chromium and tungsten complexes with halide, methyl and σ-phenylethynyl ligands: Structures of (η-C5H5)Cr(NO)2(-CC-C6H5), (η-C5H5)Cr(NO)2I and [(η-C5H4)-COOCH3]W(CO)3Cl

With copper(I) iodide as catalyst, σ-alkynyls, compounds (η⁵-C₅H₅)Cr(NO)₂(CC-C₆H₅) (5), [(η⁵-C₅H₄)-COOCH₃]Cr(NO)₂(CC-C₆H₅) (10), and [(η⁵-C₅H₄)-COOCH₃]W(CO)₃(CC-C₆H₅) (13), were prepared from their corresponding metal chloride 1, 6 and 12. Structures of compound 3, 5 and 12 have been solved by X-ray diffraction studies. In the case of 5, there is an internal mirror plane passing through the phenylethynyl ligand and bisecting the Cp ring. The phenyl group is oriented perpendicularly to the Cp with an eclipsed conformation. The twist angle is 0° and 118.4° for -CC-Ph and two NO ligands, respectively. The orientation is rationalized in terms of orbital overlap between ψ₃ of Cp, dπ of Cr atom, and π^∗ of alkynyl ligand, and complemented by molecular orbital calculation. The opposite correlation was observed on the chemical shift assignments of C(2)-C(5) on Cp ring in compounds 6 and 12, using HetCOR NMR spectroscopy. The electron density distribution in the cyclopentadienyl ring is discussed on the basis of ¹³C NMR data and compared with the calculations via density functional B3LYP correlation-exchange method.     

Derivatisation of boryl substituted titanium half-sandwich complexes - Molecular structures of [Ti{(η-C5H4)B(NiPr2)N(H)tBu}Cl2(NMe2)] and [{TiCl2(μ-{OB(NHMe2)-η-C5H4})}2-μ-O]

The half-sandwich complex [Ti{(η⁵-C₅H₄)B(NiPr₂)N(H)iPr}(NMe₂)₃] (6) was prepared from (η¹-C₅H₅)B(NiPr₂)N(H)iPr (5) and [Ti(NMe₂)₄] with cleavage of one equivalent of HNMe₂ and further converted into the corresponding constrained geometry complex [Ti{(η⁵-C₅H₄)B(NiPr₂)NiPr}(NMe₂)₂] (7) by elimination of a second equivalent of HNMe₂. Reaction of the half-sandwich complexes [Ti{(η⁵-C₅H₄)B(NiPr₂)N(H)R}(NMe₂)₃] (R = iPr, tBu) with excess Me₃SiCl yielded the corresponding dichloro complexes [Ti{(η⁵-C₅H₄)B(NiPr₂)N(H)R}Cl₂(NMe₂)] (R = tBu (10), iPr (11)). The intermediate species [Ti{(η⁵-C₅H₄)B(NiPr₂)N(H)iPr}Cl(NMe₂)₂] (9) could also be spectroscopically characterised. Partial hydrolysis of 10 and 11, respectively, resulted in formation of [{TiCl₂(μ-{OB(NHMe₂)-η⁵-C₅H₄})}₂-μ-O] (12). The molecular structures of 10 and 12 have been determined by X-ray crystallographic analyses. Complex 10, when activated with MAO, was found to be a highly active styrene polymerisation catalyst while being inactive towards the polymerisation of ethylene.     

New ferrocenylmethylphosphines - Preparation, characterisation and coordination chemistry of PH(CH2Fc)2, P(CH2Fc)3 [Fc = Fe(η-C5H5)(η-C5H4)] and their derivatives

The new ferrocenylmethylphosphines PH(CH₂Fc)₂ (1) [Fc = Fe(η⁵-C₅H₅)(η⁵-C₅H₄)] and P(CH₂Fc)₃ (2) and the phosphonium salt [P(CH₂Fc)₃(CH₂OH)]I (3) were synthesised from P(CH₂OH)₃ and [FcCH₂NMe₃]I. [P(CH₂Fc)(CH₂OH)₃]Cl (4) was obtained from P(CH₂Fc)(CH₂OH)₂, CH₂O and HCl. The new phosphines and phosphonium salts were fully characterised by NMR and IR spectroscopy and MS. [Mo(CO)₆] reacts with 1 to give [Mo(CO)₅{PH(CH₂Fc)₂}] (5) in high yield, but attempts to employ 2 as a ligand failed. The reaction of [P(CH₂Fc)₃(CH₂OH)]I (3) and [PH(CH₂Fc)₃]I (obtained in situ from 3 and Na₂S₂O₅) with [WI₂(CO)₃(NCMe)₂] gave the complex salts [P(CH₂Fc)₃(CH₂OH)][WI₃(CO)₄] (6) and [PH(CH₂Fc)₃][WI₃(CO)₄] (7), respectively. [P(CH₂Fc)₄]I (8) was synthesized from PH₂CH₂Fc and [FcCH₂NMe₃]I. Crystal structures were obtained for 1, 3-8.     

Synthesis, properties and structures of methyldiphenylphosphonium 1-indenylide, 1-C9H6PMePh2, and its chiral tricarbonylchromium(0) complex Cr(η-1-C9H6PMePh2)(CO)3

The hitherto unknown indenyl-derived ylide, methyldiphenylphosphonium 1-indenylide, 1-C₉H₆PMePh₂ (1) and its chromium(0) complex, Cr(η⁵-1-C₉H₆PMePh₂)(CO)₃ (2) have been synthesized and characterized spectroscopically and crystallographically. The structures and properties of 1 and 2 are compared with those of the analogous C₅H₄PMePh₂ and its chromium complex, Cr(η⁵-C₅H₄PMePh₂)(CO)₃. Compound 2, obtained as a racemic mixture, exhibits planar chirality resulting from coordination of the prochiral aromatic ligand.     

Stable radical adducts of diisopropylphosphoryl radicals with fullerene complexes (η2-C60)Os(CO)(PPh3)2(CNBut) and (η2-C70)Os(CO)(PPh3)2(CNBut)

It was determined by ESR spectroscopy that the UV irradiation of toluene solutions containing Hg[P(O)(OPrⁱ)₂ and the complex (²-C₆₀)Os(CO)(PPh₃)₂(CNBu^t) produces six stable regioisomeric adducts of phosphoryl radicals with complexes, which are not demetallated under UV irradiation and do not dimerize in the absence of UV irradiation. This is caused by the addition of the phosphoryl radicals to the carbon atoms of fullerene localized near the metal-containing moiety. The addition of the phosphoryl radicals to (²-C₇₀)Os(CO)(PPh₃)₂(CNBu^t) gives rise to the formation of nine stable regioisomeric radical adducts. A comparison of the composition of regioisomers of the radical adducts of C₇₀ with the phosphoryl radicals, which were formed directly from C₇₀ and from the radical adducts of ²-C₇₀)Os(CO)(PPh₃)₂(CNBu^t) by the demetallation of the latter, revealed an orienting effect of the osmium-containing moiety on the addition of the phosphoryl radicals to the fullerene complex.Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1968–1972, September, 2004.     

Synthesis and reactivity of [(η-[32](1,3)Cyclophane)Mn(CO)3][BF4]

The manganese cyclophane complex, [(η⁶-[3₂](1,3)cyclophane)Mn(CO)₃][BF₄] 2, was prepared by the reaction of [[3₂](1,3)cyclophane] 1 with Mn(CO)₅FBF₃. Reaction of 2 with NaBH₃CN yielded the cyclohexadienyl manganese complex [(η⁵-6H-[3₂](1,3)cyclophane)Mn(CO)₃] 3. Interestingly, treatment of 3 with Mn(CO)₅FBF₃ gave the bis-manganese complex (η⁶,η⁵-6H-[3₂](1,3)cyclophane)[Mn(CO)₃]₂[BF₄] 4. When NaBH₃CN was treated with 4, [(η⁵,η⁵-6H,6^′H-[3₂](1,3)cyclophane)Mn(CO)₃] 5 was isolated as yellow crystals. The structure of compounds 2 and 3 were determined by single-crystal X-ray crystallography.     

Synthesis of Mo(CO)2(η-PPh2(o-C6H4)C(O)H)2 and its reaction with C60

Reaction of Mo(CO)₃(NCMe)₃ and PPh₂(o-C₆H₄)C(O)H (abbreviated as PCHO) at room temperature affords Mo(CO)₂(η³-PCHO)₂ (1), while compound 1 and the phosphine-imine complex Mo(CO)₄(η²-PPh₂(o-C₆H₄)CHNMe) (2) are obtained by using Mo(CO)₃(η³-(MeNCH₂)₃) as the reactant. Thermal reaction of 1 with C₆₀ products Mo(CO)₂(η⁴-(PPh₂(o-C₆H₄)CH)₂)(η²-C₆₀) (3) in low yield, apparently through coupling of the formyl moieties. The structures of 1 and 3 have been determined by an X-ray diffraction study. The two aldehyde groups of 1 and C₆₀ ligand of 3 are coordinated to the molybdenum atom in a π-fashion.     

Effect of high external pressures on the vibrational spectra of Zeise’s complexes, K[Pt(η-C2H4)Cl3] and [Pt(η-C2H4)Cl2]2

The pressure dependences (dν/dP) of the main IR and Raman bands of Zeise’s complexes, K[Pt(η²-C₂H₄)Cl₃] and [Pt(η²-C₂H₄)Cl₂]₂, have been determined for the first time for selected pressures up to ∼33 kbar with the aid of diamond-anvil cells. Neither complex undergoes a pressure-induced structural change throughout the pressure range investigated. The dν/dP values range from −0.13 to 0.79 cm⁻¹ kbar⁻¹. The negative values have proved particularly informative in identifying the location of the CC stretching modes of the Pt-ethylene groups, a topic of considerable disagreement in the literature.     

Synthesis and structures of the silyl bridged bis(indenyl) diruthenium complexes and a novel indenyl nonanuclear ruthenium cluster Ru9(μ6-C)(CO)14(μ3-η:η:η-C9H7)2

Thermal treatment of C₉H₇SiMe₂C₉H₇ and C₉H₇Me₂SiOSiMe₂C₉H₇ with Ru₃(CO)₁₂ in refluxing xylene gave the corresponding diruthenium complexes (E)[(η⁵-C₉H₆)Ru(CO)]₂(μ-CO)₂ [E = Me₂Si (1), Me₂SiOSiMe₂ (2)]. A desilylation product [(η⁵-C₉H₇)Ru(CO)]₂(μ-CO)₂ (3) was also obtained in the latter case. Similar treatment of C₉H₇Me₂SiSiMe₂C₉H₇ with Ru₃(CO)₁₂ gave a novel indenyl nonanuclear ruthenium cluster Ru₉(μ₆-C)(CO)₁₄(μ₃-η⁵:η²:η²-C₉H₇)₂ (5) with carbon-centered tricapped trigonal prism geometry, in addition to the diruthenium complex (Me₂SiSiMe₂)[(η⁵-C₉H₆)Ru(CO)]₂(μ-CO)₂ (4) and the desilylation product 3. Complex 4 can undergo a thermal rearrangement to form the product [(Me₂Si)(η⁵-C₉H₆)Ru(CO)₂]₂ (6). The molecular structures of 1, 2, 4, 5, and 6 were determined by X-ray diffraction.     

Hexadecahydrotetrabenzo[a,c,d,f]fluorene - Ligand, available by Friedel-Crafts fluorene cycloalkylation. Synthesis, crystal and molecular structure of (η-C29H34)(η-C5H5)ZrCl2

Friedel-Crafts cycloalkylation of fluorene with 1,4-dichlorobutane has been studied in different conditions. This reaction allows to obtain the product of exhausting fluorene alkylation, hexadecahydrotetrabenzo[a,c,d,f]fluorene - perspective η⁵ ligand. The simplest zirconocene has been synthesized and its structure has been confirmed by X-ray diffraction analysis. The molecule of this compound possesses skewed conformation of metallocene fragment with the phenylene moiety of fluorenyl ligand oriented towards the front side of metallocene wedge.     

Nonsymmetrical iron bis(carborane) complexes (η-1-ButNH-1,7,9-C3B8H10)Fe(η-9-L-7,8-C2B9H10) (L = SMe2, NMe3)

Visible light irradiation of the benzene complex [(η-1-Bu^tNH-1,7,9-C₃B₈H₁₀)Fe(η-C₆H₆)]⁺ in the presence of the charge-compensated carborane anions [9-L-7,8-C₂B₉H₁₀]⁻ (L = SMe₂, NMe₃) affords ferracarboranes (η-1-Bu^tNH-1,7,9-C₃B₈H₁₀)Fe(η-9-L-7,8-C₂B₉H₁₀). Their structures were established by X-ray diffraction analysis.     

A synthetic, structural and reactivity study of [(η-C4R4)Co(η-C5H4X)] complexes, R = Me or Et; X = CHO, CHCHFc, CHCH(η-C5H4)Co(η-C4Ph4), CHC(CN)2: Unexpected formation of [(η-cyclopentadienyl)(η-3,4,5,6-tetraethyl-α-pyrone)cobalt]

The tetraethyl- and tetramethyl-cyclobutadiene complexes [(η⁴-C₄R₄)Co(η⁵-C₅H₄CHO)] R = Et, 5, R = Me, 7, and [(η⁴-C₄R₄)Co(η⁵-C₅H₄CO₂Me)] R = Et, 6, R = Me, 8, are conveniently prepared by photolysis of the corresponding isocobaltocenium cations [(η⁴-C₄R₄)Co(η⁶-C₆H₅Me)]⁺ in acetonitrile, and subsequent treatment with Na[C₅H₄CHO] or Na[C₅H₄CO₂Me]. The aldehydes 5 and 7 undergo Wittig and Knoevenagel reactions with [FcCH₂PPh₃]I and CH₂(CN)₂, to form [(η⁴-C₄R₄)Co(η⁵-C₅H₄CH=CHFc)] and [(η⁴-C₄R₄)Co(η⁵-C₅H₄CH=C(CN)₂], 11 and 15, respectively. The Horner-Wittig reaction of [(η⁴-C₄R₄)Co(η⁵-C₅H₄CH₂P(O)(OEt)₂] with [(η⁴-C₄Ph₄)Co(η⁵-C₅H₄CHO)] yields [(η⁴-C₄R₄)Co(η⁵:η⁵-C₅H₄CHCH-C₅H₄)Co(η⁴-C₄Ph₄)], 12 and 13. [(η⁴-C₄Me₄)Co(η⁵-C₅H₄CHO)] also reacts with t-BuLi and FcLi to furnish the corresponding secondary alcohols, 16 and 17, respectively. Surprisingly, the attempted direct synthesis of 5 by reaction of Na[C₅H₅] and ethyl formate with [(η⁴-C₄Et₄)Co(CO)₂I], 1, instead yielded [(η⁵-C₅H₅)Co(η⁴-3,4,5,6-tetraethyl-α-pyrone)], 18, and a mechanistic proposal is advanced. The X-ray crystal structures of 1, 7, 8, 11(Z), 15 and 18, and also the isocobaltocenium salts [(η⁴-C₄Et₄)Co(η⁶-C₆H₅Me)][PF₆], 2, and [(η⁴-C₄Et₄)Co(η⁶-1,3,5-C₆H₃Me₃)][PF₆], 4, are reported.     

Synthesis and X-ray investigation of novel Fe and Mn phenyltellurenyl-halide complexes: (CO)3FeBr2(PhTeBr), (η-C5H5)Fe(CO)2(PhTeI2) and CpMn(CO)2(PhTeI)

New complexes of transition metals with organotellurium halide ligands are reported. Iodination of [CpMn(CO)₂]₂(μ-Ph₂Te₂) leads to the Te-Te bond cleavage and formation of CpMn(CO)₂(PhTeI). Oxidative addition of PhTeBr₃ to Fe(CO)₅ gives the monomeric complex (CO)₃FeBr₂(PhTeBr) which is isostructural with the recently reported (CO)₃FeI₂(PhTeI). Insertion of phenyltellurenyl iodide (PhTeI) into the Fe-I bond of CpFe(CO)₂I forms CpFe(CO)₂(TeI₂Ph). Molecular structures of the reported complexes were determined by single-crystal X-ray diffraction analysis (XRD). A considerable shortening of metal-tellurium distances is observed.     

X-ray and conformation analysis of the new trinuclear cluster of osmium Os3(μ,η2-OCC6H5)(η3-C3H5)(CO)9

The crystal structure of the Os₃(μ,η²-O=CC₆H₅)(η³-C₃H₅)(CO)₉ cluster synthesized by the reaction of the (μ-H)Os₃(μ-O=CC₆H₅)(CO)₁₀ complex with allylamine in chloroform was determined by X-ray analysis. Prolonged storage of the reaction mixture led to N-C bond cleavage in allylamine and η³-addition of the allyl fragment at one of the Os atoms (Os-C 2.246 ?, 2.248 ?, and 2.273 ?). The unit cell parameters of the complex are a = 9.494(1) ?, b = 10.479(1) ?, c = 12.474(2) ?, α = 84.55(1)°, β = 70.08(1)°, γ = 70.72(1)°, V = 1255.8(4), ?³, space group P , Z = 2; C₁₉H₁₀O₁₀Os₃; d _calc = 2.922 g/cm³, 3085 I _hkl > 2σ _I of 3611 collected reflections; R = 0.0252. The structure of Os₃(μ,η²-O=CC₆H₅)(η³-C₃H₅)(CO)₉ is molecular. The plane of the Os₃ triangle and the OsCOOs plane are connected according to the “butterfly” principle with an angle of 103.4° between them. The Os-Os distances in the cluster core vary from 2.836(1) ? to 2.844(1) ?; the Os-C_carb distances are 1.88(1)–1.97(1) ?; the distances to the atoms of the bridging ligands are Os-C 2.11(1) ?, Os-O 2.14(1) ?; the O-C bridging bond is 1.24(1) ?. of the Os₃(μ,η²-O=CC₆H₅)(η³-C₃H₅)(CO)₉ triosmium cluster were studied theoretically. The potential curve of the internal rotation of the allyl ligand relative to the Os(1)-C(9) bond was determined. The rotation barrier of the allyl ligand in crystal relative to the Os(1)-C(9) bond is 8.38 kJ/mol, and the rotation of the ligand is not hindered. The effects of the intra-and intermolecular interactions on the conformation state of the cluster complex are considered. Original Russian Text Copyright ? 2008 by V. A. Maksakov, N. V. Pervukhina, N. V. Podberezskaya, M. Yu. Afonin, V. A. Potemkin, and V. P. Kirin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 5, pp. 926–932, September–October, 2008.