Niobium(III) chloride

Niobium(III) chloride  Identifiers

CAS Number

* 13569-59-0

3D model (JSmol)

* Interactive image
* 1,2-dimethoxyethane complex: Interactive image

ChemSpider |

* 75410

EC Number |

* 236-985-0

PubChem CID

* 11542954
* 1,2-dimethoxyethane complex: 6096194

InChI

* InChI=1S/3ClH.Nb/h3*1H;/q;;;+3/p-3

Key: VPDYSPXEGTXWEU-UHFFFAOYSA-K

* 1,2-dimethoxyethane complex: InChI=1S/C4H10O2.3ClH.Nb/c1-5-3-4-6-2;;;;/h3-4H2,1-2H3;3*1H;/q;;;;+3/p-3

Key: SBSZUBUHOUKQMN-UHFFFAOYSA-K

SMILES

* [Cl-].[Cl-].[Cl-].[Nb+3]

* 1,2-dimethoxyethane complex: COCCOC.Cl[Nb](Cl)Cl

Properties

Chemical formula

| Cl3Nb
Molar mass | 199.26 g·mol−1
Appearance  | black solid
Density | 3.75
Structure[1]

Crystal structure

| hexagonal

Space group

| P3m1

Lattice constant

a = 6.744, c = 12.268

Formula units (Z)

| 2

Except where otherwise noted, data are given for materials in their standard state (at 25 °C [77 °F], 100 kPa).

Infobox references

Niobium(III) chloride also known as niobium trichloride is a compound of niobium and chlorine. The binary phase NbCl3 is not well characterized but many adducts are known.

## Contents

* 1 Synthesis
* 2 Structure
* 3 Reactions
* 3.1 Adducts
* 4 References

## Synthesis

thumb|left|184px|Structure of NbCl3(dimethoxyethane)(3-hexyne).[2] Nb3Cl8 is produced by reduction of niobium(V) chloride with hydrogen, or just by heating.

Salt-free reduction of dimethoxyethane solution of NbCl5 with 1,4-disilyl-cyclohexadiene in the presence of 3-hexyne produces the coordination complex NbCl3(dimethoxyethane)(3-hexyne):

NbCl5 \+ C6H6(SiMe3)2 \+ C2Et2 \+ dme → NbCl3(dme)(C2Et2) + C6H6 \+ 2 Me3SiCl

An impure dimethoxyethane (dme) adduct of niobium trichloride was produced by reduction of a dme solution of niobium pentachloride with tributyltin hydride:[3]

NbCl5 \+ 2 Bu3SnH + MeOCH2CH2OMe → NbCl3(MeOCH2CH2OMe) + 2 Bu3SnCl

## Structure

Nb3Cl8 has a hexagonal close packed array of chloride ions. Triangles of niobium occur in octahedral spaces in the chloride array. The compositions with higher chloride have some niobium atoms missing from the structure, creating vacancies and giving rise to nonstoichiometric compounds. NbCl4 has this pattern of vacancies stretched until the niobium atoms are in pairs rather than triangles. So NbCl3 can be considered as a solid solution of Nb3Cl8 and Nb2Cl8.[4]

The colour of niobium trichloride varies depending on the niobium:chloride ratio. NbCl2.67 is green, while NbCl3.13 is brown.[1]

## Reactions

Structure of Nb2Cl6(SMe2)3.[5]

When heated to over 600 °C niobium trichloride disproportionates to niobium metal and niobium pentachloride.

### Adducts

NbCl3(dimethoxyethane) has received significant attention as a reagent for reductive coupling of carbonyls and imines.[6] It is sold as a 1,2-dimethoxyethane complex. Nb(III) adducts are also known for 1,4-dioxane and diethyl ether.

Niobium(III) chloride forms a series of compounds with the formula Nb2Cl6Lx with Nb=Nb double bond. With tertiary phosphines and arsines, the complexes are edge-share bioctahedra, e.g., Nb2Cl6(PPhMe2)4.[7] Thioethers form adducts with one bridging thioether (R2S). These face-sharing bioctahedra have the formula Nb2X6(R2S)3 (X = Cl, Br).

## References

1. ↑ 1.0 1.1 Gutmann, Viktor (1967) (in en). Halogen Chemistry. Elsevier. p. 157. ISBN 978-0-323-14847-4. https://books.google.com/books?id=q0j8Imd8yQsC&pg=PA157.
2. ↑ Tsurugi, Hayato; Mashima, Kazushi (2019). "Salt-Free Reduction of Transition Metal Complexes by Bis(trimethylsilyl)cyclohexadiene, -dihydropyrazine, and -4,4′-bipyridinylidene Derivatives". Accounts of Chemical Research 52 (3): 769–779. doi:10.1021/acs.accounts.8b00638. PMID 30794373.
3. ↑ Pedersen, Steven F.; Hartung, Jack B.; Roskamp, Eric J.; Dragovich, Peter S. (1992). "Niobium(III) and (IV) Halide Complexes". Inorganic Syntheses. 28. pp. 119–123. doi:10.1002/9780470132609.ch28. ISBN 9780470132609.
4. ↑ Cotton, F. Albert; Wilkinson, Geoffrey (1966). Advanced Inorganic Chemistry: A Comprehensive Text. John Wiley. p. 927.
5. ↑ Kakeya, Masaki; Fujihara, Takashi; Nagasawa, Akira (2006). "Di-μ-chloro-μ-(dimethyl sulfide)-bis[dichloro(dimethyl sulfide)niobium(III)]". Acta Crystallographica Section E 62 (3): m553–m554. doi:10.1107/S1600536806005149. Bibcode: 2006AcCrE..62M.553K.
6. ↑ Roskamp, Carrie A.; Roskamp, Eric J. (2001). "Encyclopedia of Reagents for Organic Synthesis". Encyclopedia of Reagents for Organic Synthesis. doi:10.1002/047084289X.rt202s. ISBN 0471936235.
7. ↑ Sharma, Sangeeta; Vermani, O. P.; Narula, A. K. (January 1996). "Synthesis and Structural Studies of Complexes of Niobium(III) Chloride with Ditertiary Phosphines". Indian Journal of Chemistry, Section A 35A (1). ISSN 0975-0975. http://nopr.niscair.res.in/handle/123456789/41226.

* v
* t
* e

Niobium compounds

Niobium(II)|

* NbS
* NbO
* NbB2

Niobium(III)|

* NbN
* Nb2S3
* NbBr3
* NbF3

Niobium(IV)|

* NbCl4
* NbC
* NbF4
* NbS2
* NbSe2
* NbO2

Niobium(V)|

* NbBr5
* NbCl5
* NbF5
* NbI5
* NbOCl3
* Nb2O5
* LiNbO3
* KNbO3

| Organoniobium(V)|

* (C5H5)2NbCl2
* Nb2(OC2H5)10

|

* v
* t
* e

Salts and covalent derivatives of the chloride ion

HCl |  |  |  | He

|
|
|
|

LiCl | BeCl2 | BCl3
B2Cl4 | CCl4 | NCl3
ClN3 | Cl2O
ClO2
Cl2O7 | ClF
ClF3
ClF5 | Ne
NaCl | MgCl2 | AlCl
AlCl3 | SiCl4 | P2Cl4
PCl3
PCl5 | S2Cl2
SCl2
SCl4 | Cl2 | Ar
KCl | CaCl
CaCl2 | ScCl3 | TiCl2
TiCl3
TiCl4 | VCl2
VCl3
VCl4
VCl5 | CrCl2
CrCl3
CrCl4 | MnCl2 | FeCl2
FeCl3 | CoCl2
CoCl3 | NiCl2 | CuCl
CuCl2 | ZnCl2 | GaCl2
GaCl3 | GeCl2
GeCl4 | AsCl3
AsCl5 | Se2Cl2
SeCl4 | BrCl | KrCl
RbCl | SrCl2 | YCl3 | ZrCl3
ZrCl4 | NbCl4
NbCl5 | MoCl2
MoCl3
MoCl4
MoCl5
MoCl6 | TcCl4 | RuCl3 | RhCl3 | PdCl2 | AgCl | CdCl2 | InCl
InCl2
InCl3 | SnCl2
SnCl4 | SbCl3
SbCl5 | Te3Cl2
TeCl4 | ICl
ICl3 | XeCl
XeCl2
CsCl | BaCl2 |  | HfCl4 | TaCl5 | WCl2
WCl3
WCl4
WCl5
WCl6 | Re3Cl9
ReCl4
ReCl5
ReCl6 | OsCl4 | IrCl2
IrCl3
IrCl4 | PtCl2
PtCl4 | AuCl
AuCl3 | Hg2Cl2,
HgCl2 | TlCl | PbCl2,
PbCl4 | BiCl3 | PoCl2,
PoCl4 | AtCl  | RnCl2
FrCl | RaCl2 |  | Rf  | Db  | Sg  | Bh  | Hs  | Mt  | Ds  | Rg  | Cn  | Nh  | Fl  | Mc  | Lv  | Ts  | Og
| ↓  |  |
LaCl3 | CeCl3 | PrCl3 | NdCl2,
NdCl3 | PmCl3 | SmCl2,
SmCl3 | EuCl2,
EuCl3 | GdCl3 | TbCl3 | DyCl2,
DyCl3 | HoCl3 | ErCl3 | TmCl2
TmCl3 | YbCl2
YbCl3 | LuCl3
AcCl3 | ThCl4 | PaCl5 | UCl3
UCl4
UCl5
UCl6 | NpCl4 | PuCl3 | AmCl2
AmCl3 | CmCl3 | BkCl3 | CfCl3 | EsCl3 | Fm  | Md  | No  | LrCl3

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