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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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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2021
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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. |
format | Online Article Text |
id | pubmed-8340972 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2021 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
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−)
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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−)
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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−)
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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−)
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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−)
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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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