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Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)

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) cyano­tri­phenyl­borate complexes di­chlorido­(cyano­tri­phenyl­borato-κN)tetra­kis­(tetra­hydro­furan-κO)lanthanide(III), [Ln...

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Autores principales: Dumas, Megan T., White, Jessica R. K., Ziller, Joseph W., Evans, William J.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8340972/
https://www.ncbi.nlm.nih.gov/pubmed/34422304
http://dx.doi.org/10.1107/S2056989021006861
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author Dumas, Megan T.
White, Jessica R. K.
Ziller, Joseph W.
Evans, William J.
author_facet Dumas, Megan T.
White, Jessica R. K.
Ziller, Joseph W.
Evans, William J.
author_sort Dumas, Megan T.
collection PubMed
description 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) cyano­tri­phenyl­borate complexes di­chlorido­(cyano­tri­phenyl­borato-κN)tetra­kis­(tetra­hydro­furan-κO)lanthanide(III), [LnCl(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 tetra­ethyl­ammonium salt of (NCBPh(3))(−) from BPh(3) and [NEt(4)][CN] in THF yielded crystals of the phenyl-substituted cyclic borate, tetra­ethyl­aza­nium 2,2,4,6-tetra­phenyl-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 tetra­ethyl­aza­nium cyano­diphenyl-λ(4)-boranyl di­phenyl­borinate, 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-tetra­phenyl-1,3,5,2λ(4),4,6-trioxatriborinan-2-ide cyano­methyl­diphenyl­borate tetra­hydro­furan 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 mol­ecule was disordered and included using multiple components with partial site-occupancy factors.
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spelling pubmed-83409722021-08-19 Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−) Dumas, Megan T. White, Jessica R. K. Ziller, Joseph W. Evans, William J. Acta Crystallogr E Crystallogr Commun Research Communications 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) cyano­tri­phenyl­borate complexes di­chlorido­(cyano­tri­phenyl­borato-κN)tetra­kis­(tetra­hydro­furan-κO)lanthanide(III), [LnCl(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 tetra­ethyl­ammonium salt of (NCBPh(3))(−) from BPh(3) and [NEt(4)][CN] in THF yielded crystals of the phenyl-substituted cyclic borate, tetra­ethyl­aza­nium 2,2,4,6-tetra­phenyl-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 tetra­ethyl­aza­nium cyano­diphenyl-λ(4)-boranyl di­phenyl­borinate, 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-tetra­phenyl-1,3,5,2λ(4),4,6-trioxatriborinan-2-ide cyano­methyl­diphenyl­borate tetra­hydro­furan 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 mol­ecule was disordered and included using multiple components with partial site-occupancy factors. International Union of Crystallography 2021-07-13 /pmc/articles/PMC8340972/ /pubmed/34422304 http://dx.doi.org/10.1107/S2056989021006861 Text en © Dumas et al. 2021 https://creativecommons.org/licenses/by/4.0/This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
spellingShingle Research Communications
Dumas, Megan T.
White, Jessica R. K.
Ziller, Joseph W.
Evans, William J.
Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title_full Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title_fullStr Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title_full_unstemmed Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title_short Crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [NCBPh(3)](1−), [NCBPh(2)Me](1−), and [NCBPh(2)(μ-O)BPh(2)](1−)
title_sort crystallographic characterization of rare-earth cyano­tri­phenyl­borate complexes and the cyano­borates [ncbph(3)](1−), [ncbph(2)me](1−), and [ncbph(2)(μ-o)bph(2)](1−)
topic Research Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8340972/
https://www.ncbi.nlm.nih.gov/pubmed/34422304
http://dx.doi.org/10.1107/S2056989021006861
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