transition metal ether complex

File:VEHZAJ.svg | year = 1990 | volume = C46 | pages = 890–2 | doi = 10.1107/S010827018901382X | last1 = Duraj | first1 = S. A. | last2 = Towns | last3 = Baker | last4 = Schupp | first4 = J. | issue = 5| doi-access = }}]]

In chemistry, a transition metal ether complex is a coordination complex consisting of a transition metal bonded to one or more ether ligand. The inventory of complexes is extensive.{{Greenwood&Earnshaw2nd}} Common ether ligands are diethyl ether and tetrahydrofuran. Common chelating ether ligands include the glymes, dimethoxyethane (dme) and diglyme, and the crown ethers. Being lipophilic, metal-ether complexes often exhibit solubility in organic solvents, a property of interest in synthetic chemistry. In contrast, the di-ether 1,4-dioxane is generally a bridging ligand.

Bonding, structure, reactions

File:CoCl2(dioxane)XUBHEI).jpg of cobalt(II) chloride and 1,4-dioxane.{{cite journal |doi=10.1021/ja902101x|title=Crystal-to-Crystal Transformation from Antiferromagnetic Chains into a Ferromagnetic Diamondoid Framework |year=2009 |last1=Duan |first1=Zhiming |last2=Zhang |first2=Yan |last3=Zhang |first3=Bin |last4=Zhu |first4=Daoben |journal=Journal of the American Chemical Society |volume=131 |issue=20 |pages=6934–6935 |pmid=19402661 }}]]

Ethers are L-type ligands. They are σ-donors that exert weak field ligands. They resemble water ligands as seen in aquo complexes. They do not, however, readily participate in hydrogen bonding. The ether oxygen is nearly trigonal planar in its complexes.

Being weakly basic, ether ligands tend to be easily displaceable. Otherwise, ether ligands are relatively unreactive. Cyclic ethers such as thf can ring-open or even deoxygenated when bound to highly electrophilic metal halides. Thus treatment of tungsten hexachloride with one equivalent of thf gives 1,4-dichlorobutane:{{cite journal |doi=10.1016/j.poly.2016.07.024|year=2016 |volume=117 |last1=Bianchi |first1=Sabrina |last2=Bortoluzzi |first2=Marco |last3=Castelvetro |first3=Valter |last4=Marchetti |first4=Fabio |last5=Pampaloni |first5=Guido |last6=Pinzino |first6=Calogero |last7=Zacchini |first7=Stefano |title=The reactivity of tungsten hexachloride with tetrahydrofuran and 2-methoxyethanol |journal=Polyhedron |pages=769–776 |hdl=11568/803763 |hdl-access=free }}

:{{chem2|WCl6 + OC4H8 -> WOCl4 + ClCH2CH2CH2CH2Cl}}

At higher concentrations of thf, polytetrahydrofuran is produced.

Examples

=Homoleptic complexes=

Ethers are relatively bulky ligands, thus homoleptic (i.e., all ligands being the same) ether complexes are uncommon. Examples often feature weakly coordinating anions such as BArF4 and Al(ORF)4.

  • [V(thf)6](BArF4)2{{cite journal |doi=10.1002/(SICI)1521-3773(19981204)37:22<3169::AID-ANIE3169>3.0.CO;2-0|title=Cationic Homoleptic Vanadium(II), (IV), and (V) Complexes Arising from Protonolysis of [V(NEt2)4] |year=1998 |last1=Choukroun |first1=Robert |last2=Moumboko |first2=Pierre |last3=Chevalier |first3=Sandrine |last4=Etienne |first4=Michel |last5=Donnadieu |first5=Bruno |journal=Angewandte Chemie International Edition |volume=37 |issue=22 |pages=3169–3172 |pmid=29711321 }}
  • [Mn(thf)6](Mn(CO)5]2{{cite journal |doi=10.1021/ja00117a019|title=An Unusual Transition Metal Cluster Containing a Seven Metal Atom Plane. Syntheses and Crystal Structures of [Mn][Mn7(THF)6(CO)12]2, Mn3(THF)2(CO)10, and [Mn(THF)6][Mn(CO)5]2 |year=1995 |last1=Kong |first1=Gapgoung |last2=Harakas |first2=George N. |last3=Whittlesey |first3=Bruce R. |journal=Journal of the American Chemical Society |volume=117 |issue=12 |pages=3502–3509 }}
  • Fe(thf)6[BArF24]2{{cite journal |doi=10.1021/acs.organomet.5b00395|title=Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by an Amidinato-diolefin Ligand: Characterization and Catalytic Application |year=2015 |last1=Lichtenberg |first1=Crispin |last2=Adelhardt |first2=Mario |last3=Wörle |first3=Michael |last4=Büttner |first4=Torsten |last5=Meyer |first5=Karsten |last6=Grützmacher |first6=Hansjörg |journal=Organometallics |volume=34 |issue=12 |pages=3079–3089 }}
  • [Ni(thf)6][Al(ORF)4 ]2{{cite journal |doi=10.1002/zaac.201700367|title=Reactivity of [Ni(cod)2][Al(ORF)4] towards Small Molecules and Elements |year=2018 |last1=Schwab |first1=Miriam M. |last2=Himmel |first2=Daniel |last3=Kacprzak |first3=Sylwia |last4=Radtke |first4=Valentin |last5=Kratzert |first5=Daniel |last6=Yassine |first6=Zeinab |last7=Weis |first7=Philippe |last8=Weber |first8=Stefan |last9=Krossing |first9=Ingo |journal=Zeitschrift für Anorganische und Allgemeine Chemie |volume=644 |pages=50–57 }}

=Metal halide complexes=

File:NiI2(dme)2.png. The sum of the angles at O is 352°, indicating a nearly planar ether oxygen. Color code: O = red, I = purple, Ni = blue, C = black.{{cite journal |doi=10.1002/zaac.201000022|title=Polyether Adducts of d-Block Metal Compounds as Starting Materials for New Cluster Compounds |year=2010 |last1=Crochet |first1=Aurélien |last2=Fromm |first2=Katharina M. |journal=Zeitschrift für anorganische und allgemeine Chemie |volume=636 |issue=8 |pages=1484–1496 |url=http://doc.rero.ch/record/20544/files/fro_pad.pdf }}]]

File:UJIMUV.jpg

Metal chloride-tetrahydrofuran complexes are especially studied.{{cite book |doi=10.1002/9780470132524.ch31|title=Tetrahydrofuran Complexes of Selected Early Transition Metals|series=Inorganic Syntheses|year=1982|last1=Manzer|first1=L. E.|pages=135–140|volume=21}} These compounds are often reagents because they are soluble in organic solvents as well as being anhydrous.

class="wikitable"

! Formula of
metal-chloride-ether complexes

Coordination
sphere
color
TiCl4(thf)2TiO2Cl4yellow{{cite journal |doi=10.1021/ic060896u|title=Technetium Tetrachloride as a Precursor for Small Technetium(IV) Complexes|year=2006|last1=Hagenbach|first1=Adelheid|last2=Yegen|first2=Eda|last3=Abram|first3=Ulrich|journal=Inorganic Chemistry|volume=45|issue=18|pages=7331–7338|pmid=16933935}}
TiCl3(thf)3TiO3Cl3blue
[TiCl3(thf)2]2TiO2Cl4green{{cite journal |doi=10.1039/dt9930002353|title=New intermediates for the Synthesis of Olefin Polymerization Catalysts: The Complexes [M2(μ-Cl)2Cl4(THF)4] (M = Ti or V, THF = Tetrahydrofuran); Crystal Structures and Properties|year=1993| last1=Sobota|first1=Piotr|last2=Ejfler|first2=Jolanta|last3=Szafert|first3=Sławomir|last4=Szczegot|first4=Krzysztof|last5=Sawka-Dobrowolska|first5=Wanda|journal=Journal of the Chemical Society, Dalton Transactions |issue=15|pages=2353–2357}}
ZrCl4(thf)2ZrO2Cl4white
HfCl4(thf)2HfO2Cl4white
VCl3(thf)3VO3Cl3pink
VCl3(thf)2]2VO2Cl4red
NbCl4(thf)2NbO2Cl4yellow
Ta3Cl9(thf)4TaO2Cl4 and TaOCl5{{cite journal |doi=10.1021/ic00351a005|title=New Synthetic Routes for the Preparation of Niobium(III) and Tantalum(III) Triangular Cluster Compounds|year=1990|last1=Babaian-Kibala|first1=Elizabeth|last2=Cotton|first2=F. Albert|last3=Shang|first3=Maoyu|journal=Inorganic Chemistry|volume=29|issue=26|pages=5148–5156}}
CrCl3(thf)3CrO3Cl3pink
MoCl4(thf)2MoO2Cl4pink{{cite book| volume = 28 | chapter = The Synthesis of Molybdenum and Tungsten Dinitrogen Complexes | year = 1990 |doi=10.1002/9780470132593.ch7| last1 = Dilworth | first1 = Jonathan R. | last2 = Richards | first2 = Raymond L. | title = Inorganic Syntheses | series = Inorganic Syntheses | pages = 33–43| isbn = 9780470132593 }}
MoCl4(Et2O)2MoO2Cl4beige{{cite book |doi=10.1002/9781118744994.ch03|chapter=Ether Complexes of Molybdenum(III) and Molybdenum(IV) chlorides |series=Inorganic Syntheses |year=2014 |last1=Maria |first1=Sébastien |last2=Poli |first2=Rinaldo |title=Inorganic Syntheses: Volume 36 |pages=15–18 |isbn=9781118744994 |url=https://hal.archives-ouvertes.fr/hal-02042499/file/332-10.1002-9781118744994.ch03-Accepted.pdf }}
MoCl3(thf)3MoO3Cl3red
WCl4(Et2O)2WO2Cl4yellow{{cite journal |doi=10.1107/S2053229621002461|title=The Decades-Old Mystery of Bis(diethyl ether)tungsten(IV) Chloride Solved |year=2021 |last1=Schäfer |first1=André |journal=Acta Crystallographica Section C Structural Chemistry |volume=77 |issue=4 |pages=167–168 |pmid=33818437 |pmc=8020884 }}
MnCl3(thf)3MnO3Cl3brown-purple{{cite journal |doi=10.1002/zaac.201500106|title=Solvates of Manganese Trichloride Revisited - Synthesis, Isolation, and Crystal Structure of MnCl3(THF)3|year=2015|last1=Nachtigall|first1=Olaf|last2=Pataki|first2=Astrid|last3=Molski|first3=Matthias|last4=Lentz|first4=Dieter|last5=Spandl|first5=Johann|journal=Zeitschrift für Anorganische und Allgemeine Chemie|volume=641|issue=6|pages=1164–1168}}
TcCl4(thf)2TcO2Cl4yellow
ReCl4(thf)2ReO2Cl4green{{cite journal |doi=10.1021/ic060896u|first1=H.-W. |last1=Swidersky |first2=J. |last2=Pebler |first3=K. |last3=Dehnicke |first4=D. |last4=Fenske|title=Technetium Tetrachloride as a Precursor for Small Technetium(IV) Complexes|journal= Inorganic Chemistry|year=1990|volume=45|issue=18|pages=7331–8|pmid=16933935}}
Fe4Cl8(thf)6FeO2Cl3, FeO2Cl4brown{{cite journal |doi=10.1016/S0020-1693(00)85366-9|title=New polynuclear compounds of iron(II) chloride with oxygen donor ligands Part I. Fe4Cl8(THF)6: Synthesis and a single crystal X-ray structure determination|year=1991|last1=Cotton|first1=F. Albert|last2=Luck|first2=Rudy L.|last3=Son|first3=Kyung-Ae|journal=Inorganica Chimica Acta|volume=179|pages=11–15}}
FeCl3(thf)2FeO2Cl3{{cite journal|author=L. V. Ivakina, N. R. Strel'tsova, V. K. Bel'skii, P. A. Storozhenko, B. M. Bulychev, A. B. Tarasov|journal=Zh.Obshch.Khim. (Russ.J.Gen.Chem.)|year=1987|volume=57|page=1600}}the related diethyl ether complex is brown
FeCl3(OEt2)2FeO2Cl3brown
Co4Cl8(thf)6CoO2Cl3, CoO2Cl4blue{{cite journal |doi=10.1016/S0277-5387(00)84976-1|title=Synthesis, Magnetic Properties and Structure of the [Co43-Cl)22-Cl)4Cl2(THF)6] Complex|year=1993|last1=Sobota|first1=Piotr|last2=Olejnik|first2=Zofia|last3=Utko|first3=Józef|last4=Lis|first4=Tadeusz|journal=Polyhedron|volume=12|issue=6|pages=613–616}}
[CoCl2(dme)]2CoO2Cl3{{cite journal |doi=10.5562/cca1747|title=Octahedral and Tetrahedral Cobalt(II) Sites in Cobalt Chloride Complexes with Polyethers |year=2011 |last1=Petriček |first1=Saša |journal=Croatica Chemica Acta |pages=515–520 |doi-access=free }}
NiCl2(dimethoxyethane)2NiCl2O4yellow{{cite book|doi=10.1002/9780470132449.ch30|chapter=Anhydrous Nickel(II) Halides and their Tetrakis(ethanol) and 1,2-Dimethoxyethane Complexes|series=Inorganic Syntheses|year=1972|last1=Ward|first1=Laird G. L.|title=Inorganic Syntheses |volume=13|pages=154–164|isbn=9780470132449 }}
[Cu2Cl4(thf)3]nCuO2Cl4, CuOCl4orange{{cite journal |doi=10.1021/acs.inorgchem.5b02576|title=Copper Chloride Catalysis: Do μ4-Oxido Copper Clusters Play a Significant Role?|year=2016|last1=Becker|first1=Sabine|last2=Dürr|first2=Maximilian|last3=Miska|first3=Andreas|last4=Becker|first4=Jonathan|last5=Gawlig|first5=Christopher|last6=Behrens|first6=Ulrich|last7=Ivanović-Burmazović|first7=Ivana|last8=Schindler|first8=Siegfried|journal=Inorganic Chemistry|volume=55|issue=8|pages=3759–3766|pmid=27045752}}
ZnCl2(thf)2ZnO2Cl2white{{cite book |doi=10.1002/9780470132609.ch26|chapter=Solvated and Unsolvated Anhydrous Metal Chlorides from Metal Chloride Hydrates |series=Inorganic Syntheses |year=1992 |last1=Boudjouk |first1=Philip |last2=So |first2=Jeung-Ho |title=Inorganic Syntheses |pages=108–111 |volume=29 |isbn=9780470132609 }}

=Metal carbonyl complexes=

  • M(CO)5(thf) (M = Cr, Mo, W){{cite journal |doi=10.1016/S0022-328X(00)84160-1|title=Kristall- und molekülstruktur von pentacarbonyltetrahydrofuran-chrom(0) |year=1978 |last1=Schubert |first1=U. |last2=Friedrich |first2=P. |last3=Orama |first3=O. |journal=Journal of Organometallic Chemistry |volume=144 |issue=2 |pages=175–179 }}
  • Mo(CO)3(diglyme)

References