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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-κ N )tetra-kis-(tetra-hydro-furan-κ O )lanthanide(III), [ Ln Cl 2 (C 19 H 15 BN)(C 4 H 8 O) 4 ] [lanthanide ( Ln ) = dysprosium (Dy) and yttrium Y)] from reactions of LnCl 3 , KCN, and NaBPh 4 . Attempts to independently synthesize the tetra-ethyl-ammonium salt of (NCBPh 3 ) - from BPh 3 and [NEt 4 ][CN] in THF yielded crystals of the phenyl-substituted cyclic borate, tetra-ethyl-aza-nium 2,2,4,6-tetra-phenyl-1,3,5,2λ 4 ,4,6-trioxatriborinan-2-ide, C 8 H 20 N + ·C 24 H 20 B 3 O 3  - or [NEt 4 ][B 3 (μ-O) 3 (C 6 H 5 ) 4 ]. The mechanochemical reaction of BPh 3 and [NEt 4 ][CN] without solvent produced crystals of tetra-ethyl-aza-nium cyano-diphenyl-λ 4 -boranyl di-phenyl-borinate, C 8 H 20 N + ·C 25 H 20 B 2 NO - or [NEt 4 ][NCBPh 2 (μ-O)BPh 2 ]. Reaction of BPh 3 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-1,3,5,2λ 4 ,4,6-trioxatriborinan-2-ide cyano-methyl-diphenyl-borate tetra-hydro-furan disolvate, 2C 18 H 36 KN 2 O 6  + ·C 24 H 20 B 3 O 3  - ·C 14 H 13 BN - ·2C 4 H 8 O or [K(crypt)] 2 [B 3 (μ-O) 3 (C 6 H 5 ) 4 ][NCBPh 2 Me]·2THF. The [NCBPh 2 (μ-O)BPh 2 ] 1- and (NCBPh 2 Me) 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.

acta crystallographica. section e, crystallographic communications

Crystallographic characterization of rare-earth cyanotriphenylborate complexes and the cyanoborates [NCBPh3]1−, [NCBPh2Me]1−, and [NCBPh2(μ-O)BPh2]1−