2019
DOI: 10.1002/zaac.201800390
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Cyclic Tribismuthide as a Piano Stool Complex Ligand – Synthesis and Crystal Structure of (η3‐Bi3)M(CO)33– (M = Cr, Mo)

Abstract: The reactions between K 5 Bi 4 , [(C 6 H 6 )Cr(CO) 3 ] or [(C 7 H 8 )Mo(CO) 3 ], and [2.2.2]crypt in liquid ammonia yielded the compounds [K([2.2.2]crypt)] 3 (η 3 -Bi 3 )M(CO) 3 ·10NH 3 (M = Cr, Mo), which crystallize isostructurally in P2 1 /n. Both contain an 18 valence electron piano-stool complex with a η 3 -coordinated Bi 3 -ring ligand.

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Cited by 12 publications
(8 citation statements)
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“…However, the information gained by means of single-crystal data from isolated species in combination with mass spectrometric investigations at various steps of a reaction and different reaction conditions allows some insight that we are going to share herein. We additionally refer to the knowledge of solid state compounds comprising Bi 2 q – and Bi 4 q – motifs in nonstoichiometric phases K 3 Bi 2 and K 5 Bi 4 or in stoichiometric compounds [K­(crypt-222)] 2 Bi 4 and K 6 (Bi 4 )­(NH 3 ) 8 , and to cluster compounds comprising triangular or chain-like Bi 3 q – units: [{Ni 4 (CO) 6 }­Bi 3 ] 3– , [{Ni 6 (CO) 9 }­Bi 3 ] 3– , [Bi 12 Ni 7 (CO) 4 ] 4– , [{M 2 (CO) 6 }­Bi 3 ] 3– (M = Cr, Mo), [{M­(CO) 3 }­Bi 3 ] 2– (M = Cr, Mo), [Pd@Pd 2 ­Bi 10 ­@­(Bi 3 ) 2 ] 4– . These indicate the formation of small {Bi n } moieties to take place with a certain preference under the given, sometimes harsh, reaction conditions.…”
Section: Resultsmentioning
confidence: 99%
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“…However, the information gained by means of single-crystal data from isolated species in combination with mass spectrometric investigations at various steps of a reaction and different reaction conditions allows some insight that we are going to share herein. We additionally refer to the knowledge of solid state compounds comprising Bi 2 q – and Bi 4 q – motifs in nonstoichiometric phases K 3 Bi 2 and K 5 Bi 4 or in stoichiometric compounds [K­(crypt-222)] 2 Bi 4 and K 6 (Bi 4 )­(NH 3 ) 8 , and to cluster compounds comprising triangular or chain-like Bi 3 q – units: [{Ni 4 (CO) 6 }­Bi 3 ] 3– , [{Ni 6 (CO) 9 }­Bi 3 ] 3– , [Bi 12 Ni 7 (CO) 4 ] 4– , [{M 2 (CO) 6 }­Bi 3 ] 3– (M = Cr, Mo), [{M­(CO) 3 }­Bi 3 ] 2– (M = Cr, Mo), [Pd@Pd 2 ­Bi 10 ­@­(Bi 3 ) 2 ] 4– . These indicate the formation of small {Bi n } moieties to take place with a certain preference under the given, sometimes harsh, reaction conditions.…”
Section: Resultsmentioning
confidence: 99%
“…In contrast to the well-known tendency of bismuth to form polycations, it was shown only recently that Bi atoms are actually capable of forming polyanionic molecular assemblies: homoatomic, or heteroatomic in combination with other (semi)­metal(s). The synthetic access to Bi-rich polyanionic molecules was achieved through reactions of binary Zintl phases comprising homoatomic anions, K 3 Bi 2 or K 5 Bi 4 , or by employing [K­(crypt-222)] + salts of binary anions, (GaBi 3 ) 2– , (InBi 3 ) 2– , , or (TlBi 3 ) 2– , , in reactions with transition metal, lanthanide, or actinide complexes. In a significant amount of reactions with the binary anions (GaBi 3 ) 2– and (TlBi 3 ) 2– , the products turned out to comprise Bi atoms as the only main group component, as these anions tend to decompose under release of elemental group 13 metal. This is in contrast to the behavior of pseudo-tetrahedral binary anions of group 14/Bi combinations, in which the heteroatomic bonds usually seem to be strong enough, thus leading to ternary, yet usually less Bi-rich, intermetalloid clusters. …”
Section: Introductionmentioning
confidence: 99%
“…3.087 (2) Å) and (η 3 -Bi 3 )­M­(CO) 3 3– (M = Cr, Mo) ( av. 2.98 Å) . The six Bi 4 Rh-CO coordination patterns are divided into two groups; in three Bi 4 Rh-CO, each Rh makes a Bi 4 square use three Bi atoms of a Bi 6 crown and one Bi of a Bi 4 pyramid (Figure c).…”
Section: Resultsmentioning
confidence: 99%
“…2.98 Å). 25 The six Bi 4 Rh-CO coordination patterns are divided into two groups; in three Bi 4 Rh-CO, each Rh makes a Bi 4 square use three Bi atoms of a Bi 6 crown and one Bi of a Bi 4 pyramid (Figure 1c). In the remaining three Bi 4 Rh-CO, each Rh makes a Bi 4 square use three Bi atoms of a Bi 4 pyramid and one Bi of a Bi 6 crown (Figure 1d).…”
Section: ■ Results and Discussionmentioning
confidence: 99%
“…So, the average number of cluster electrons per atom can get close to 4 (per main group atom; 14 per transition metal atom) or below, and structures containing deltahedral architecturesindicative of electron deficiencyare obtained. [Bi 3 M 2 (CO) 6 ] 3– contains an ozone-like Bi 3 3– , [(η 3 -Bi 3 )­M­(CO) 3 ] 3– (M = Cr, Mo) is based on cyclic Bi 3 3– , and [Bi 6 Mo 3 (CO) 9 ] 4– has a distorted {Bi 6 } triangular prism (Figure f-h). The series of known Ni/Bi cluster anions demonstrate the variety in {Bi x } substructures, such as [Bi 3 Ni 4 (CO) 6 ] 3– , [Bi 4 Ni 4 (CO) 6 ] 2– , [Bi 3 Ni 6 (CO) 9 ] 3– , and [Ni x @{Bi 6 Ni 6 (CO) 8 }] 4– , whose heating and oxidation additionally yielded [Bi 12 Ni 7 (CO) 4 ] 4– (Figure i–m). , …”
Section: Bismuth-based Cluster Anionsmentioning
confidence: 99%