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Crystallographic characterization of rare-earth cyano-tri-phenyl-borate complexes and the cyano-borates [NCBPh3]1-, [NCBPh2Me]1-, and [NCBPh2(μ-O)BPh2]1.


ABSTRACT: The investigation of the coordination chemistry of rare-earth metal complexes with cyanide ligands led to the isolation and crystallographic characterization of the Ln III cyano-tri-phenyl-borate complexes di-chlorido-(cyano-tri-phenyl-borato-κN)tetra-kis-(tetra-hydro-furan-κO)lanthanide(III), [LnCl2(C19H15BN)(C4H8O)4] [lanthanide (Ln) = dysprosium (Dy) and yttrium Y)] from reactions of LnCl3, KCN, and NaBPh4. Attempts to independently synthesize the tetra-ethyl-ammonium salt of (NCBPh3)- from BPh3 and [NEt4][CN] in THF yielded crystals of the phenyl-substituted cyclic borate, tetra-ethyl-aza-nium 2,2,4,6-tetra-phenyl-1,3,5,2λ4,4,6-trioxatriborinan-2-ide, C8H20N+·C24H20B3O3 - or [NEt4][B3(μ-O)3(C6H5)4]. The mechanochemical reaction of BPh3 and [NEt4][CN] without solvent produced crystals of tetra-ethyl-aza-nium cyano-diphenyl-λ4-boranyl di-phenyl-borinate, C8H20N+·C25H20B2NO- or [NEt4][NCBPh2(μ-O)BPh2]. Reaction of BPh3 and KCN in THF in the presence of 2.2.2-cryptand (crypt) led to a crystal of bis-[(2.2.2-cryptand)potassium] 2,2,4,6-tetra-phenyl-1,3,5,2λ4,4,6-trioxatriborinan-2-ide cyano-methyl-diphenyl-borate tetra-hydro-furan disolvate, 2C18H36KN2O6 +·C24H20B3O3 -·C14H13BN-·2C4H8O or [K(crypt)]2[B3(μ-O)3(C6H5)4][NCBPh2Me]·2THF. The [NCBPh2(μ-O)BPh2]1- and (NCBPh2Me)1- anions have not been structurally characterized previously. The structure of 1-Y was refined as a two-component twin with occupancy factors 0.513 (1) and 0.487 (1). In 4, one solvent mol-ecule was disordered and included using multiple components with partial site-occupancy factors.

SUBMITTER: Dumas MT 

PROVIDER: S-EPMC8340972 | biostudies-literature | 2021 Aug

REPOSITORIES: biostudies-literature

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Crystallographic characterization of rare-earth cyano-tri-phenyl-borate complexes and the cyano-borates [NCBPh<sub>3</sub>]<sup>1-</sup>, [NCBPh<sub>2</sub>Me]<sup>1-</sup>, and [NCBPh<sub>2</sub>(μ-O)BPh<sub>2</sub>]<sup>1</sup>.

Dumas Megan T MT   White Jessica R K JRK   Ziller Joseph W JW   Evans William J WJ  

Acta crystallographica. Section E, Crystallographic communications 20210713 Pt 8


The investigation of the coordination chemistry of rare-earth metal complexes with cyanide ligands led to the isolation and crystallographic characterization of the <i>Ln</i> <sup>III</sup> cyano-tri-phenyl-borate complexes di-chlorido-(cyano-tri-phenyl-borato-κ<i>N</i>)tetra-kis-(tetra-hydro-furan-κ<i>O</i>)lanthanide(III), [<i>Ln</i>Cl<sub>2</sub>(C<sub>19</sub>H<sub>15</sub>BN)(C<sub>4</sub>H<sub>8</sub>O)<sub>4</sub>] [lanthanide (<i>Ln</i>) = dysprosium (Dy) and yttrium Y)] from reactions o  ...[more]

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