Synthesis and X‐ray Structure of [{(Cp′ ₂ Nb) ₂ WTe ₄ }⋅W(CO) ₄ ]·1.5C ₇ H ₈ , the First Organometallic Derivative of the WTe ₄ ²⁻ Anion, and of [Cp′ ₄ Nb ₂ Te <

Abstract

Reaction of [Cp′2NbTe2H] (1) (Cp′ = η5‐tBuC5H4) with [W(CO)6] in decane at 140 °C gives red [{(Cp′2Nb)2WTe4}⋅W(CO)4] (2), whereas in the reaction of 1 with [Cr(CO)6] green‐black [Cp′4Nb2Te2] (3) is formed. The crystal structures of 2 and 3 have been determined. The structure of 2 contains a slightly distorted WTe4 tetrahedron to which two niobocene fragments and one W(CO)4 group are coordinated. The crystal structure determination of 3 reveals the presence of two Cp′2Nb units bridged by two Te atoms. Complex 2 represents the first example of an organometallic derivative of the unknown WTe42− anion.

Synthesis and structural characterization of the neutral pentagonal-prismatic Co11Te7(CO)10 cluster in a matrix of [Cp′4Nb2(CH3Te)Te]I (Cp′ = tBuC5H4)

“…2). This arrangement is similar to that in Cp′ 4 Nb 2 Te 2 [10,14] and [Cp′ 4 Nb 2 (CH 3 Te) 2 ]I 2 [10] and similarities are also observed for the metric parameters (Table 1). Two methyl groups (C29) are fixed at the Te bridges in a trans position, but with an occupancy of 50% for each of the methyl groups.…”

Synthesis and structural characterization of the neutral pentagonal-prismatic Co11Te7(CO)10 cluster in a matrix of [Cp′4Nb2(CH3Te)Te]I (Cp′ = tBuC5H4)

“…2). This arrangement is similar to that in Cp′ 4 Nb 2 Te 2 [10,14] and [Cp′ 4 Nb 2 (CH 3 Te) 2 ]I 2 [10] and similarities are also observed for the metric parameters (Table 1). Two methyl groups (C29) are fixed at the Te bridges in a trans position, but with an occupancy of 50% for each of the methyl groups.…”

Bis(η-tert-butylcyclopentadienyl)hydridoniobium Ditelluride, a Convenient Reagent for the Synthesis of Polynuclear Metal Telluride Complexes

“…In complex 5 each Nb center is surrounded by two CpЈ anions and two Te 2Ϫ bridges. A bonding interaction between opposite atoms Te(1) and Te(1Ј) [d ϭ 4.262(1) Å ] was excluded [25] in agreement with literature values given for planar M 2 Te 2 rings: Whereas in the Ni 2 Te 2 cycle of [(iPr 4 C 5 H) 2 Ni 2 (µ-Te) 2 ] the observed Te···Te distance of 3.052(5) Å has been ascribed to a bond order of nearly one, [26] a clearly nonbonding situation has been found in [CpЈ 4 Zr 2 Te 2 ] [d(Te···Te) ϭ 4.006(1) Å ]. [21] Less evident is the interpretation of the Nb(1)···Nb(1Ј) distance in 5.…”

“…Complex 5 has been obtained in still better yield from the reaction of 1 with [Cr(CO) 6 ] in refluxing toluene. [25] The analytical and spectroscopic data of 5 are in agreement with the independently synthesized compound, the solid state structure of which has been described briefly. In this study direct bonding interactions between opposite atoms of the Nb 2 Te 2 core were excluded.…”

[{(C5Me5)2Nb}2PdTe4], a heterometallic palladium telluride cluster with a planar PdTe4 fragment

“…In contrast to the tetrahedral MTe 4 derivatives [{(tBuC 5 H 4 ) 2 NbTe 2 } 2 W AE W(CO) 4 ] (2) [8] and ½ðCp à 2 NbÞ 2 NiTe 4 (3) [6] the heavy atom core of 1 has a deck-chair like structure with angles of 160°between the planes Te1/Nb1/ Te2 and Te1/Te2/Pd (Fig. 2).…”

Synthesis and structural characterization of the neutral pentagonal-prismatic Co11Te7(CO)10 cluster in a matrix of [Cp′4Nb2(CH3Te)Te]I (Cp′ = tBuC5H4)

“…2). This arrangement is similar to that in Cp′ 4 Nb 2 Te 2 [10,14] and [Cp′ 4 Nb 2 (CH 3 Te) 2 ]I 2 [10] and similarities are also observed for the metric parameters (Table 1). Two methyl groups (C29) are fixed at the Te bridges in a trans position, but with an occupancy of 50% for each of the methyl groups.…”

Bis(η-tert-butylcyclopentadienyl)hydridoniobium Ditelluride, a Convenient Reagent for the Synthesis of Polynuclear Metal Telluride Complexes

“…In complex 5 each Nb center is surrounded by two CpЈ anions and two Te 2Ϫ bridges. A bonding interaction between opposite atoms Te(1) and Te(1Ј) [d ϭ 4.262(1) Å ] was excluded [25] in agreement with literature values given for planar M 2 Te 2 rings: Whereas in the Ni 2 Te 2 cycle of [(iPr 4 C 5 H) 2 Ni 2 (µ-Te) 2 ] the observed Te···Te distance of 3.052(5) Å has been ascribed to a bond order of nearly one, [26] a clearly nonbonding situation has been found in [CpЈ 4 Zr 2 Te 2 ] [d(Te···Te) ϭ 4.006(1) Å ]. [21] Less evident is the interpretation of the Nb(1)···Nb(1Ј) distance in 5.…”

“…Complex 5 has been obtained in still better yield from the reaction of 1 with [Cr(CO) 6 ] in refluxing toluene. [25] The analytical and spectroscopic data of 5 are in agreement with the independently synthesized compound, the solid state structure of which has been described briefly. In this study direct bonding interactions between opposite atoms of the Nb 2 Te 2 core were excluded.…”

[{(C5Me5)2Nb}2PdTe4], a heterometallic palladium telluride cluster with a planar PdTe4 fragment

“…In contrast to the tetrahedral MTe 4 derivatives [{(tBuC 5 H 4 ) 2 NbTe 2 } 2 W AE W(CO) 4 ] (2) [8] and ½ðCp à 2 NbÞ 2 NiTe 4 (3) [6] the heavy atom core of 1 has a deck-chair like structure with angles of 160°between the planes Te1/Nb1/ Te2 and Te1/Te2/Pd (Fig. 2).…”

Synthesis and structural characterization of the neutral pentagonal-prismatic Co11Te7(CO)10 cluster in a matrix of [Cp′4Nb2(CH3Te)Te]I (Cp′ = tBuC5H4)

“…2). This arrangement is similar to that in Cp′ 4 Nb 2 Te 2 [10,14] and [Cp′ 4 Nb 2 (CH 3 Te) 2 ]I 2 [10] and similarities are also observed for the metric parameters (Table 1). Two methyl groups (C29) are fixed at the Te bridges in a trans position, but with an occupancy of 50% for each of the methyl groups.…”

Bis(η-tert-butylcyclopentadienyl)hydridoniobium Ditelluride, a Convenient Reagent for the Synthesis of Polynuclear Metal Telluride Complexes

“…In complex 5 each Nb center is surrounded by two CpЈ anions and two Te 2Ϫ bridges. A bonding interaction between opposite atoms Te(1) and Te(1Ј) [d ϭ 4.262(1) Å ] was excluded [25] in agreement with literature values given for planar M 2 Te 2 rings: Whereas in the Ni 2 Te 2 cycle of [(iPr 4 C 5 H) 2 Ni 2 (µ-Te) 2 ] the observed Te···Te distance of 3.052(5) Å has been ascribed to a bond order of nearly one, [26] a clearly nonbonding situation has been found in [CpЈ 4 Zr 2 Te 2 ] [d(Te···Te) ϭ 4.006(1) Å ]. [21] Less evident is the interpretation of the Nb(1)···Nb(1Ј) distance in 5.…”

“…Complex 5 has been obtained in still better yield from the reaction of 1 with [Cr(CO) 6 ] in refluxing toluene. [25] The analytical and spectroscopic data of 5 are in agreement with the independently synthesized compound, the solid state structure of which has been described briefly. In this study direct bonding interactions between opposite atoms of the Nb 2 Te 2 core were excluded.…”

[{(C5Me5)2Nb}2PdTe4], a heterometallic palladium telluride cluster with a planar PdTe4 fragment

“…In contrast to the tetrahedral MTe 4 derivatives [{(tBuC 5 H 4 ) 2 NbTe 2 } 2 W AE W(CO) 4 ] (2) [8] and ½ðCp à 2 NbÞ 2 NiTe 4 (3) [6] the heavy atom core of 1 has a deck-chair like structure with angles of 160°between the planes Te1/Nb1/ Te2 and Te1/Te2/Pd (Fig. 2).…”