Challenges in the synthetic routes to Mn(BH4)2: Insight into intermediate compounds

Nikolay A. Tumanov; Damir A. Safin; Bo Richter; Zbigniew Łodziana; Torben R. Jensen; Yann Garcia; Yaroslav Filinchuk

doi:10.1039/c4dt03807j

Challenges in the synthetic routes to Mn(BH₄)₂: Insight into intermediate compounds

Nikolay A. Tumanov, Damir A. Safin, Bo Richter, Zbigniew Łodziana, Torben R. Jensen, Yann Garcia, Yaroslav Filinchuk

Résultats de recherche: Contribution à un journal/une revue › Article › Revue par des pairs

Résumé

We have studied the reaction of MnCl₂ with MBH₄ (M = Li⁺, Na⁺, K⁺) in Et₂O. Crystal structures of two new intermediates, named [{M(Et₂O)₂}Mn₂(BH₄)₅] (M = Li⁺, Na⁺), were elucidated by X-ray diffraction. Mn(BH₄)₂ in a mixture with LiBH₄ or NaBH₄ forms upon the solvent removal in a vacuum. [{M(Et₂O)₂}Mn₂(BH₄)₅] contains 2D layers formed by Mn and BH₄ groups, linked through the alkali metal atoms coordinated to Et₂O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH₄/NaBH₄ and a creation of the 3D framework of the crystalline Mn(BH₄)₂. While using LiBH₄ led to Mn(BH₄)₂ contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH₄)₂-Et₂O] system, the reaction with NaBH₄ produced chlorine-free Mn(BH₄)₂ accompanied with NaBH₄. Using KBH₄ led to the formation of K₂Mn(BH₄)₄ as a second phase. Two pyridine-containing solvomorphs, [Mn(py)₃(BH₄)₂] and [Mn(py)₄(BH₄)₂]·2py, were isolated in pure form. However, Mn(BH₄)₂ partly decomposes upon removal of pyridine molecules. This journal is

langue originale	Anglais
Pages (de - à)	6571-6580
Nombre de pages	10
journal	Dalton Transactions
Volume	44
Numéro de publication	14
Les DOIs	https://doi.org/10.1039/c4dt03807j
Etat de la publication	Publié - 14 avr. 2015
Modification externe	Oui

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10.1039/c4dt03807j

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tumanov2015
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CCDC 985623: Experimental Crystal Structure Determination
Filinchuk, Y. (Contributeur), Garcia, Y. (Contributeur), Jensen, T. R. (Contributeur), Łodziana, Z. (Contributeur), Richter, B. (Contributeur), Safin, D. A. (Contributeur) & Tumanov, N. (Contributeur), Cambridge Crystallographic Data Centre, 1 janv. 2015
DOI: 10.5517/cc122m92, http://www.ccdc.cam.ac.uk/services/structure_request?id=doi:10.5517/cc122m92&sid=DataCite
Ensemble de données
CCDC 985622: Experimental Crystal Structure Determination
Filinchuk, Y. (Contributeur), Garcia, Y. (Contributeur), Jensen, T. R. (Contributeur), Łodziana, Z. (Contributeur), Richter, B. (Contributeur), Safin, D. A. (Contributeur) & Tumanov, N. (Contributeur), Cambridge Crystallographic Data Centre, 1 janv. 2015
DOI: 10.5517/cc122m81, http://www.ccdc.cam.ac.uk/services/structure_request?id=doi:10.5517/cc122m81&sid=DataCite
Ensemble de données
CCDC 985621: Experimental Crystal Structure Determination
Filinchuk, Y. (Contributeur), Garcia, Y. (Contributeur), Jensen, T. R. (Contributeur), Łodziana, Z. (Contributeur), Richter, B. (Contributeur), Safin, D. A. (Contributeur) & Tumanov, N. (Contributeur), Cambridge Crystallographic Data Centre, 1 janv. 2015
DOI: 10.5517/cc122m70, http://www.ccdc.cam.ac.uk/services/structure_request?id=doi:10.5517/cc122m70&sid=DataCite
Ensemble de données

Contient cette citation

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title = "Challenges in the synthetic routes to Mn(BH4)2: Insight into intermediate compounds",

abstract = "We have studied the reaction of MnCl2 with MBH4 (M = Li+, Na+, K+) in Et2O. Crystal structures of two new intermediates, named [{M(Et2O)2}Mn2(BH4)5] (M = Li+, Na+), were elucidated by X-ray diffraction. Mn(BH4)2 in a mixture with LiBH4 or NaBH4 forms upon the solvent removal in a vacuum. [{M(Et2O)2}Mn2(BH4)5] contains 2D layers formed by Mn and BH4 groups, linked through the alkali metal atoms coordinated to Et2O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH4/NaBH4 and a creation of the 3D framework of the crystalline Mn(BH4)2. While using LiBH4 led to Mn(BH4)2 contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH4)2-Et2O] system, the reaction with NaBH4 produced chlorine-free Mn(BH4)2 accompanied with NaBH4. Using KBH4 led to the formation of K2Mn(BH4)4 as a second phase. Two pyridine-containing solvomorphs, [Mn(py)3(BH4)2] and [Mn(py)4(BH4)2]·2py, were isolated in pure form. However, Mn(BH4)2 partly decomposes upon removal of pyridine molecules. This journal is",

author = "Tumanov, {Nikolay A.} and Safin, {Damir A.} and Bo Richter and Zbigniew {\L}odziana and Jensen, {Torben R.} and Yann Garcia and Yaroslav Filinchuk",

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AU - Tumanov, Nikolay A.

AU - Safin, Damir A.

AU - Richter, Bo

AU - Łodziana, Zbigniew

AU - Jensen, Torben R.

AU - Garcia, Yann

AU - Filinchuk, Yaroslav

PY - 2015/4/14

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N2 - We have studied the reaction of MnCl2 with MBH4 (M = Li+, Na+, K+) in Et2O. Crystal structures of two new intermediates, named [{M(Et2O)2}Mn2(BH4)5] (M = Li+, Na+), were elucidated by X-ray diffraction. Mn(BH4)2 in a mixture with LiBH4 or NaBH4 forms upon the solvent removal in a vacuum. [{M(Et2O)2}Mn2(BH4)5] contains 2D layers formed by Mn and BH4 groups, linked through the alkali metal atoms coordinated to Et2O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH4/NaBH4 and a creation of the 3D framework of the crystalline Mn(BH4)2. While using LiBH4 led to Mn(BH4)2 contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH4)2-Et2O] system, the reaction with NaBH4 produced chlorine-free Mn(BH4)2 accompanied with NaBH4. Using KBH4 led to the formation of K2Mn(BH4)4 as a second phase. Two pyridine-containing solvomorphs, [Mn(py)3(BH4)2] and [Mn(py)4(BH4)2]·2py, were isolated in pure form. However, Mn(BH4)2 partly decomposes upon removal of pyridine molecules. This journal is

AB - We have studied the reaction of MnCl2 with MBH4 (M = Li+, Na+, K+) in Et2O. Crystal structures of two new intermediates, named [{M(Et2O)2}Mn2(BH4)5] (M = Li+, Na+), were elucidated by X-ray diffraction. Mn(BH4)2 in a mixture with LiBH4 or NaBH4 forms upon the solvent removal in a vacuum. [{M(Et2O)2}Mn2(BH4)5] contains 2D layers formed by Mn and BH4 groups, linked through the alkali metal atoms coordinated to Et2O. The loss of the solvent molecules leads to the segregation of the partially amorphous or nanocrystalline LiBH4/NaBH4 and a creation of the 3D framework of the crystalline Mn(BH4)2. While using LiBH4 led to Mn(BH4)2 contaminated with LiCl, presumably due to an efficient trapping of the latter salt by the [Mn(BH4)2-Et2O] system, the reaction with NaBH4 produced chlorine-free Mn(BH4)2 accompanied with NaBH4. Using KBH4 led to the formation of K2Mn(BH4)4 as a second phase. Two pyridine-containing solvomorphs, [Mn(py)3(BH4)2] and [Mn(py)4(BH4)2]·2py, were isolated in pure form. However, Mn(BH4)2 partly decomposes upon removal of pyridine molecules. This journal is

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ER -

Challenges in the synthetic routes to Mn(BH4)2: Insight into intermediate compounds

Résumé

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Autres fichiers et liens

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Ensembles de données

CCDC 985623: Experimental Crystal Structure Determination

CCDC 985622: Experimental Crystal Structure Determination

CCDC 985621: Experimental Crystal Structure Determination

Contient cette citation

Challenges in the synthetic routes to Mn(BH₄)₂: Insight into intermediate compounds