Crystal growth in aqueous hydrofluoric acid and (HF)x · pyridine solutions: syntheses and crystal structures of [Ni(H2O)6]2+[MF6]2- (M = Ti, Zr, Hf) and Ni3(py)12F6 · 7H2O

Paramasivan Halasyamani; Michael J. Willis; Charlotte L. Stern; Kenneth R. Poeppelmeier

doi:10.1016/0020-1693(95)04650-X

Crystal growth in aqueous hydrofluoric acid and (HF)_x · pyridine solutions: syntheses and crystal structures of [Ni(H₂O)₆]²⁺[MF₆]^2- (M = Ti, Zr, Hf) and Ni₃(py)₁₂F₆ · 7H₂O

Paramasivan Halasyamani, Michael J. Willis, Charlotte L. Stern, Kenneth R. Poeppelmeier^*

^*Corresponding author for this work

Chemistry

Research output: Contribution to journal › Article › peer-review

33 Scopus citations

Abstract

The syntheses and structures of [Ni(H₂O)₆]²⁺[MF₆]^2- (M = Ti,Zr,Hf) and Ni₃(py)₁₂F₆·7H₂O are reported. The former three compounds are isostructural, crystallizing in the trigonal space group R3 (No. 148) with Z = 3. The lattice parameters are a = 9.489(4), c = 9.764(7) A ̊, with V = 761(1) Å³ for Ti; a = 9.727(2), c = 10.051(3) Å, with V = 823.6(6) Å³ for Zr; and a = 9.724(3), c = 10.028(4)Å, with V = 821.2(8)Å³ for Hf. The structures consist of discrete [Ni(H₂O)₆]²⁺ and [MF₆]^2- octahedra joined by OH⋯F hydrogen bond Large single crystals were grown in an aqueous hydrofluoric acid solution. Ni₃(py)₁₂F₆·7H₂O crystallizes in the monoclinic space group I2/a (No. 15) with Z = 4. The lattice parameters are a = 16.117(4), b = 8.529(3), c = 46.220(7) A ̊, β = 92.46(2)°, and V = 6348(5) A ̊³. The structure consists of discrete Ni(py)₄F₂ octahedra linked through HOH⋯F and HOH⋯O hydrogen bonding interactions. Single c were grown from a (HF)_x·pyridine/pyridine/water solution.

Original language	English (US)
Pages (from-to)	109-115
Number of pages	7
Journal	Inorganica Chimica Acta
Volume	240
Issue number	1-2
DOIs	https://doi.org/10.1016/0020-1693(95)04650-X
State	Published - Dec 1995

Keywords

Crystal structure
Hexafluoro complexes
Hexahydrate complexes
Nickel complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0020-1693(95)04650-X

Cite this

@article{e72acbf2814d40aba7999b66a4011f49,

title = "Crystal growth in aqueous hydrofluoric acid and (HF)x · pyridine solutions: syntheses and crystal structures of [Ni(H2O)6]2+[MF6]2- (M = Ti, Zr, Hf) and Ni3(py)12F6 · 7H2O",

abstract = "The syntheses and structures of [Ni(H2O)6]2+[MF6]2- (M = Ti,Zr,Hf) and Ni3(py)12F6·7H2O are reported. The former three compounds are isostructural, crystallizing in the trigonal space group R3 (No. 148) with Z = 3. The lattice parameters are a = 9.489(4), c = 9.764(7) A ̊, with V = 761(1) {\AA}3 for Ti; a = 9.727(2), c = 10.051(3) {\AA}, with V = 823.6(6) {\AA}3 for Zr; and a = 9.724(3), c = 10.028(4){\AA}, with V = 821.2(8){\AA}3 for Hf. The structures consist of discrete [Ni(H2O)6]2+ and [MF6]2- octahedra joined by OH⋯F hydrogen bond Large single crystals were grown in an aqueous hydrofluoric acid solution. Ni3(py)12F6·7H2O crystallizes in the monoclinic space group I2/a (No. 15) with Z = 4. The lattice parameters are a = 16.117(4), b = 8.529(3), c = 46.220(7) A ̊, β = 92.46(2)°, and V = 6348(5) A ̊3. The structure consists of discrete Ni(py)4F2 octahedra linked through HOH⋯F and HOH⋯O hydrogen bonding interactions. Single c were grown from a (HF)x·pyridine/pyridine/water solution.",

keywords = "Crystal structure, Hexafluoro complexes, Hexahydrate complexes, Nickel complexes",

author = "Paramasivan Halasyamani and Willis, {Michael J.} and Stern, {Charlotte L.} and Poeppelmeier, {Kenneth R.}",

note = "Funding Information: The authors gratefully acknowledge support from the National Science Foundation, Solid State Chemistry, Contract DMR-9412971. The authors acknowledge Rachel Bain for help in collecting the IR spectra and Alan Allgeier for assistance in collecting the electronic spectra.",

year = "1995",

month = dec,

doi = "10.1016/0020-1693(95)04650-X",

language = "English (US)",

volume = "240",

pages = "109--115",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier B.V.",

number = "1-2",

}

Crystal growth in aqueous hydrofluoric acid and (HF)_x · pyridine solutions: syntheses and crystal structures of [Ni(H₂O)₆]²⁺[MF₆]^2- (M = Ti, Zr, Hf) and Ni₃(py)₁₂F₆ · 7H₂O. / Halasyamani, Paramasivan; Willis, Michael J.; Stern, Charlotte L. et al.
In: Inorganica Chimica Acta, Vol. 240, No. 1-2, 12.1995, p. 109-115.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Crystal growth in aqueous hydrofluoric acid and (HF)x · pyridine solutions

T2 - syntheses and crystal structures of [Ni(H2O)6]2+[MF6]2- (M = Ti, Zr, Hf) and Ni3(py)12F6 · 7H2O

AU - Halasyamani, Paramasivan

AU - Willis, Michael J.

AU - Stern, Charlotte L.

AU - Poeppelmeier, Kenneth R.

N1 - Funding Information: The authors gratefully acknowledge support from the National Science Foundation, Solid State Chemistry, Contract DMR-9412971. The authors acknowledge Rachel Bain for help in collecting the IR spectra and Alan Allgeier for assistance in collecting the electronic spectra.

PY - 1995/12

Y1 - 1995/12

N2 - The syntheses and structures of [Ni(H2O)6]2+[MF6]2- (M = Ti,Zr,Hf) and Ni3(py)12F6·7H2O are reported. The former three compounds are isostructural, crystallizing in the trigonal space group R3 (No. 148) with Z = 3. The lattice parameters are a = 9.489(4), c = 9.764(7) A ̊, with V = 761(1) Å3 for Ti; a = 9.727(2), c = 10.051(3) Å, with V = 823.6(6) Å3 for Zr; and a = 9.724(3), c = 10.028(4)Å, with V = 821.2(8)Å3 for Hf. The structures consist of discrete [Ni(H2O)6]2+ and [MF6]2- octahedra joined by OH⋯F hydrogen bond Large single crystals were grown in an aqueous hydrofluoric acid solution. Ni3(py)12F6·7H2O crystallizes in the monoclinic space group I2/a (No. 15) with Z = 4. The lattice parameters are a = 16.117(4), b = 8.529(3), c = 46.220(7) A ̊, β = 92.46(2)°, and V = 6348(5) A ̊3. The structure consists of discrete Ni(py)4F2 octahedra linked through HOH⋯F and HOH⋯O hydrogen bonding interactions. Single c were grown from a (HF)x·pyridine/pyridine/water solution.

AB - The syntheses and structures of [Ni(H2O)6]2+[MF6]2- (M = Ti,Zr,Hf) and Ni3(py)12F6·7H2O are reported. The former three compounds are isostructural, crystallizing in the trigonal space group R3 (No. 148) with Z = 3. The lattice parameters are a = 9.489(4), c = 9.764(7) A ̊, with V = 761(1) Å3 for Ti; a = 9.727(2), c = 10.051(3) Å, with V = 823.6(6) Å3 for Zr; and a = 9.724(3), c = 10.028(4)Å, with V = 821.2(8)Å3 for Hf. The structures consist of discrete [Ni(H2O)6]2+ and [MF6]2- octahedra joined by OH⋯F hydrogen bond Large single crystals were grown in an aqueous hydrofluoric acid solution. Ni3(py)12F6·7H2O crystallizes in the monoclinic space group I2/a (No. 15) with Z = 4. The lattice parameters are a = 16.117(4), b = 8.529(3), c = 46.220(7) A ̊, β = 92.46(2)°, and V = 6348(5) A ̊3. The structure consists of discrete Ni(py)4F2 octahedra linked through HOH⋯F and HOH⋯O hydrogen bonding interactions. Single c were grown from a (HF)x·pyridine/pyridine/water solution.

KW - Crystal structure

KW - Hexafluoro complexes

KW - Hexahydrate complexes

KW - Nickel complexes

UR - http://www.scopus.com/inward/record.url?scp=0000364845&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0000364845&partnerID=8YFLogxK

U2 - 10.1016/0020-1693(95)04650-X

DO - 10.1016/0020-1693(95)04650-X

M3 - Article

AN - SCOPUS:0000364845

SN - 0020-1693

VL - 240

SP - 109

EP - 115

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

IS - 1-2

ER -

Crystal growth in aqueous hydrofluoric acid and (HF)_x · pyridine solutions: syntheses and crystal structures of [Ni(H₂O)₆]²⁺[MF₆]^2- (M = Ti, Zr, Hf) and Ni₃(py)₁₂F₆ · 7H₂O

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Crystal growth in aqueous hydrofluoric acid and (HF)x · pyridine solutions: syntheses and crystal structures of [Ni(H2O)6]2+[MF6]2- (M = Ti, Zr, Hf) and Ni3(py)12F6 · 7H2O

Abstract

Keywords

ASJC Scopus subject areas

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CCDC 107153: Experimental Crystal Structure Determination

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Crystal growth in aqueous hydrofluoric acid and (HF)_x · pyridine solutions: syntheses and crystal structures of [Ni(H₂O)₆]²⁺[MF₆]^2- (M = Ti, Zr, Hf) and Ni₃(py)₁₂F₆ · 7H₂O