22

d-Metal Organometallic Chemistry

Metal-Carbon Bonds, Ligands, and Reactions

Fe

Exploring the fascinating world of compounds containing metal-carbon bonds, from metal carbonyls to metallocenes and their transformative reactions

Introduction to Organometallic Chemistry

Organometallic chemistry is the chemistry of compounds containing metal–carbon bonds. The d-block organometallic chemistry has developed rapidly since the discovery of ferrocene in 1951, spanning new types of reactions, unusual structures, and practical applications in organic synthesis and industrial catalysis.

Key Distinction: Unlike coordination complexes that are normally charged, with variable d-electron counts, and are water-soluble, organometallic compounds are often neutral, with fixed d-electron counts, and are soluble in organic solvents like THF.

Historical Milestones

1827 - Zeise's Salt

First organometallic compound: [Pt(C₂H₄)Cl₃]⁻, an ethene complex of platinum(II).

[PtCl₃(C₂H₄)]⁻

1890 - Nickel Carbonyl

Mond, Langer, and Quinke synthesized tetracarbonylnickel, [Ni(CO)₄].

[Ni(CO)₄]

1951 - Ferrocene

Discovery of the remarkably stable "sandwich" compound [Fe(C₅H₅)₂] revolutionized the field.

[Fe(Cp)₂]

1973 - Nobel Prize

Ernst-Otto Fischer and Geoffrey Wilkinson awarded for contributions to organometallic chemistry.

22.1 Bonding and the 18-Electron Rule

Unlike coordination compounds, d-metal organometallic compounds normally have relatively few stable electron configurations and often have a total of 16 or 18 valence electrons around the metal atom. This restriction is due to the strength of the π (and δ) bonding interactions.

18-Electron Rule

18 e⁻

Maximum stability achieved when metal has 18 valence electrons (like noble gas configuration)

[Ni(CO)₄] [Fe(Cp)₂] [Cr(CO)₆]

16-Electron Complexes

16 e⁻

Common for d⁸ square planar complexes; reactive towards oxidative addition

[Ir(CO)Cl(PPh₃)₂] [RhCl(PPh₃)₃]

Origin of the 18-Electron Rule

In an octahedral complex with strong π-acceptor ligands like CO, six σ-bonding interactions utilize the a₁g, t₁u, and eg orbitals. Additionally, the three t₂g orbitals can form π bonds with ligand acceptor orbitals. This gives nine bonding molecular orbitals that can accommodate 18 electrons.

Molecular Orbital Scheme for Octahedral Carbonyl

t₁u*, a₁g*
σ antibonding
eg*
σ antibonding
t₂g (π*)
eg
t₁u
a₁g

22.2-22.3 Electron Counting Methods

Two methods are commonly used to count electrons in organometallic compounds. Both give the same total electron count but differ in how they assign oxidation states.

Neutral-Ligand Method

All ligands treated as neutral; uses L/X notation

  • L = 2-electron neutral donor (CO, PR₃)
  • X = 1-electron radical (H, Cl, CH₃)
  • Cp = L₂X (5 electrons)
Metal e⁻ = Group number

Donor-Pair Method

Some ligands treated as anions; uses formal charges

  • CO, PR₃ = 2 electrons (neutral)
  • H⁻, Cl⁻, CH₃⁻ = 2 electrons (anionic)
  • Cp⁻ = 6 electrons (anionic)
Metal e⁻ = Group - Oxidation state

Example: Electron Counting for [IrBr₂(CH₃)(CO)(PPh₃)₂]

Method Calculation Total
Neutral-Ligand Ir(9) + 2Br(2×1) + CH₃(1) + CO(2) + 2PPh₃(2×2) = 9 + 2 + 1 + 2 + 4 18 e⁻
Donor-Pair Ir(III)(6) + 2Br⁻(2×2) + CH₃⁻(2) + CO(2) + 2PPh₃(2×2) = 6 + 4 + 2 + 2 + 4 18 e⁻

Common Ligands and Their Electron Counts

Ligand Formula Designation (L/X) Electrons (neutral) Electrons (donor-pair)
Carbonyl CO L 2 2
Phosphine PR₃ L 2 2
Hydride H X 1 2 (as H⁻)
Alkyl R (CH₃, etc.) X 1 2 (as R⁻)
η²-Alkene CH₂=CH₂ L 2 2
η³-Allyl C₃H₅ LX 3 4 (as C₃H₅⁻)
Butadiene C₄H₆ L₂ 4 4
η⁵-Cyclopentadienyl C₅H₅ L₂X 5 6 (as Cp⁻)
η⁶-Benzene C₆H₆ L₃ 6 6

22.5-22.17 Ligands in Organometallic Chemistry

Hapticity (η) - Modes of Ligand Binding

Hapticity describes the number of contiguous atoms of a ligand that are coordinated to the metal. It is denoted as ηn, where n is the number of atoms bonded to the metal.

η¹

Monohapto

1 atom bonded

CH₃, σ-alkyl

η²

Dihapto

2 atoms bonded

Ethene, alkyne

η³

Trihapto

3 atoms bonded

Allyl

η⁵

Pentahapto

5 atoms bonded

Cyclopentadienyl

η⁶

Hexahapto

6 atoms bonded

Benzene

22.5 Carbon Monoxide - The Archetypal Ligand

CO is particularly good at stabilizing very low oxidation states. The bonding involves σ-donation from the carbon lone pair (3σ orbital) and π-backbonding from filled metal d-orbitals to empty π* orbitals on CO.

σ Donation

CO M

3σ → Metal d orbital

Weak σ donor

σ bond

π backbond

π Backbonding

M π* CO

Metal d → CO π*

Strong π acceptor

Effect of Backbonding on ν(CO): As electron density on the metal increases (through better σ-donor co-ligands or negative charge), more electrons are donated into CO π*, weakening the C≡O bond and lowering the CO stretching frequency.

CO Stretching Frequencies and Metal Charge

Higher ν(CO) Lower ν(CO)
[Mn(CO)₆]⁺
2090 cm⁻¹
[Cr(CO)₆]
2000 cm⁻¹
[V(CO)₆]⁻
1860 cm⁻¹
[Ti(CO)₆]²⁻
1750 cm⁻¹
Less backbonding More backbonding

22.6 Phosphines

Phosphine ligands (PR₃) are excellent σ-donors and moderate π-acceptors. Their electronic and steric properties can be finely tuned by changing the R groups.

Tolman Cone Angle (θ)

Measures the steric bulk of phosphine ligands. Larger cone angles mean more steric hindrance.

  • PMe₃: 118°
  • PPh₃: 145°
  • P(tBu)₃: 182°

Electronic Parameter (ν)

Based on CO stretching frequency in [Ni(CO)₃L]. Lower values indicate better σ-donors.

  • P(tBu)₃: 2056 cm⁻¹
  • PPh₃: 2069 cm⁻¹
  • P(OPh)₃: 2085 cm⁻¹

22.15 Carbenes

Fischer Carbenes

Electron-poor at carbon, stabilized by π-donor substituents (OR, NR₂)

M=C(OR)R'

Electrophilic, attacked by nucleophiles

Schrock Carbenes

Electron-rich at carbon, with strong M=C backbonding

M=CR₂ (alkylidenes)

Nucleophilic, attacked by electrophiles

N-Heterocyclic Carbenes (NHCs)

Strong σ-donors, stabilized by adjacent N atoms

M-C(NR)₂

Excellent ancillary ligands in catalysis

22.18 Metal Carbonyls

Binary metal carbonyls contain only metal atoms and CO ligands. They represent the simplest class of organometallic compounds and follow the 18-electron rule.

Simple Binary Carbonyls

Tetrahedral

[Ni(CO)₄]

Ni(0): 10 + 8 = 18 e⁻

Colorless, toxic liquid

Trigonal Bipyramidal

[Fe(CO)₅]

Fe(0): 8 + 10 = 18 e⁻

Yellow liquid, fluxional

Octahedral

[Cr(CO)₆] [Mo(CO)₆] [W(CO)₆]

M(0): 6 + 12 = 18 e⁻

White solids, sublime

Polynuclear Metal Carbonyls

When mononuclear carbonyls cannot achieve 18 electrons, metal-metal bonds form. Each M-M bond contributes 1 electron to each metal.

[Mn₂(CO)₁₀]

Mn-Mn single bond

Each Mn: 7 + 10 + 1 = 18 e⁻

Mn Mn

[Co₂(CO)₈]

Co-Co bond + bridging COs

Each Co: 9 + 6-8 + 1 = 18 e⁻

Co Co

[Fe₂(CO)₉]

Three bridging COs

Fe-Fe bond debated

Fe Fe

Bridging vs Terminal CO

Bonding Mode Symbol ν(CO) Range Description
Terminal M-CO 2125-1850 cm⁻¹ CO bound to one metal
Edge-bridging μ₂-CO 1850-1750 cm⁻¹ CO bridges two metals
Face-bridging μ₃-CO 1730-1620 cm⁻¹ CO bridges three metals

22.19 Metallocenes

Metallocenes are "sandwich" compounds with two parallel cyclopentadienyl (Cp) rings bound to a central metal atom. Ferrocene [Fe(Cp)₂] is the archetypal metallocene.

Ferrocene [Fe(η⁵-Cp)₂]: 18-electron compound, Fe(II), remarkably stable (sublimes without decomposition), aromatic character preserved in Cp rings, undergoes electrophilic aromatic substitution.

Electron Configurations of Metallocenes

Complex Valence e⁻ Configuration M-C Bond (pm) Properties
[V(Cp)₂] 15 e₂'² a₁'¹ 228 Paramagnetic
[Cr(Cp)₂] 16 e₂'³ a₁'¹ 217 Paramagnetic
[Fe(Cp)₂] 18 e₂'⁴ a₁'² 206 Diamagnetic, stable
[Co(Cp)₂] 19 e₂'⁴ a₁'² e₁''¹ 212 Easily oxidized
[Ni(Cp)₂] 20 e₂'⁴ a₁'² e₁''² 220 Paramagnetic

Bent Metallocenes and Piano-Stool Complexes

Bent Sandwich

[Ti(Cp)₂Cl₂] [Zr(Cp)₂Cl₂]

Two Cp rings bent away from linear

Important in Ziegler-Natta catalysis

Half-Sandwich (Piano-Stool)

[Mn(Cp)(CO)₃] [Cr(C₆H₆)(CO)₃]

One Cp/arene ring + other ligands

Three "legs" like a piano stool

Triple-Decker

[Ni₂(Cp)₃]⁺

Three Cp rings, two metals

Rare but known

Ring Slipping (Hapticity Change)

Cyclopentadienyl ligands can "slip" from η⁵ to η³ or η¹ coordination, changing the electron count and creating a coordination site for incoming ligands.

η⁵-Cp (6 e⁻) ⟷ η³-Cp (4 e⁻) ⟷ η¹-Cp (2 e⁻)

22.20 Metal Clusters

Metal clusters are compounds with metal-metal bonds forming triangular or larger cyclic structures. Their electron counts correlate with structure via the Wade-Mingos-Lauher rules.

Cluster Valence Electron (CVE) Counts

For smaller clusters: CVE = 18n - 2m, where n = number of metals, m = number of M-M bonds

Triangle

3 metals, 3 M-M bonds

48 CVE
[Os₃(CO)₁₂]

Tetrahedron

4 metals, 6 M-M bonds

60 CVE
[Co₄(CO)₁₂]

Trigonal Bipyramid

5 metals, 9 M-M bonds

72 CVE
[Os₅(CO)₁₆]

Octahedron

6 metals, 12 M-M bonds

86 CVE
[Ru₆C(CO)₁₇]

Isolobal Analogy

Fragments that have frontier orbitals of the same symmetry, similar energies, and same electron occupancy are called isolobal (symbol: ↔).

Fragment Isolobal With Electrons in Frontier Orbital
CH₃ [Mn(CO)₅], [Co(CO)₄] 1
CH₂ [Fe(CO)₄], [Mn(CO)₄]⁻ 2
CH [Co(CO)₃], [Fe(CO)₃]⁻ 3

This allows prediction of structures: if CH₃-CH₃ (ethane) exists, then [(CO)₅Mn-Mn(CO)₅] should also be stable.

22.21 Ligand Substitution Reactions

Substitution in organometallic complexes follows similar principles to coordination chemistry, with the additional constraint that the electron count should not exceed 18.

18-Electron Complexes: Generally undergo dissociatively activated substitution because associative pathways would require a 20-electron intermediate.

16-Electron Complexes: Often undergo associatively activated substitution via an 18-electron intermediate.

Thermal and Photochemical Substitution

Thermal Substitution

[Cr(CO)₆] + L → [Cr(CO)₅L] + CO

Requires heating; goes through solvated intermediate [Cr(CO)₅(solv)]

Photochemical Substitution

[M(CO)₆] + hν → [M(CO)₅] + CO

UV light promotes CO loss; faster and milder conditions

Effect of Ligand Properties

Better σ-donor ligands (like phosphines) increase electron density on the metal, strengthening M-CO bonds through enhanced π-backbonding. This decreases the rate of further CO substitution.

Dissociation Constants for [Ni(PR₃)₄] Complexes

Phosphine (L) Cone Angle (θ) Kd
PMe₃ 118° <10⁻⁹
PEt₃ 137° 1.2 × 10⁻⁵
PMePh₂ 136° 5.0 × 10⁻²
PPh₃ 145° Large
P(tBu)₃ 182° Large

Larger cone angles lead to greater dissociation (steric crowding).

22.22 Oxidative Addition and Reductive Elimination

These reactions are fundamental to organometallic catalysis. They involve changes in both coordination number and oxidation state by 2.

Oxidative Addition

MnLx + X-Y → Mn+2Lx(X)(Y)
  • Coordination number: +2
  • Oxidation state: +2
  • Electron count: +2
  • X-Y bond broken

Common for 16e⁻ d⁸ complexes (Ir(I), Rh(I), Pt(0), Pd(0))

Reductive Elimination

Mn+2Lx(X)(Y) → MnLx + X-Y
  • Coordination number: -2
  • Oxidation state: -2
  • Electron count: -2
  • X-Y bond formed

Requires X and Y to be cis; reverse of oxidative addition

Examples of Oxidative Addition

H₂ Addition (Concerted)

[Ir(CO)Cl(PPh₃)₂] + H₂ → [Ir(H)₂(CO)Cl(PPh₃)₂]

16e⁻ Ir(I) → 18e⁻ Ir(III)

Products are cis-dihydrides

Alkyl Halide (SN2-like)

[Ir(CO)Cl(PPh₃)₂] + CH₃I → [Ir(CH₃)(I)(CO)Cl(PPh₃)₂]

Stereochemistry at C inverted

CH₃ and I may be trans

22.23 σ-Bond Metathesis

When oxidative addition cannot occur (e.g., early d-metals with d⁰ configuration), a concerted σ-bond metathesis can exchange ligands through a four-membered transition state.

σ-Bond Metathesis

[(Cp)₂Zr(H)(CH₃)] + H₂ → [(Cp)₂Zr(H)₂] + CH₄

No change in oxidation state; concerted 4-center transition state

Zr H H Me

22.24-22.26 Insertion and Elimination Reactions

1,1-Migratory Insertion

An X group migrates to an adjacent ligand (like CO), reducing the electron count by 2. Despite the name "insertion," the mechanism involves migration of X to the CO.

CO Insertion (Migratory Insertion)

[Mn(CH₃)(CO)₅] + PPh₃ → [Mn(COCH₃)(CO)₄(PPh₃)]
Mn Me CO Mn acyl Mn C(O)Me PR₃

The methyl group migrates to an adjacent CO; incoming ligand occupies the vacated site. Stereochemistry at carbon is preserved.

1,2-Insertion and β-Hydride Elimination

1,2-Insertion involves migration of X to an η²-ligand (like an alkene), creating an η¹-alkyl. The reverse, β-hydride elimination, is a common decomposition pathway.

1,2-Insertion

M-H + CH₂=CH₂ → M-CH₂CH₃

Hydride migrates to coordinated alkene

Key step in alkene hydrogenation and polymerization

β-Hydride Elimination

M-CH₂CH₃ → M-H + CH₂=CH₂

Reverse of 1,2-insertion (requires β-H and vacant site)

Common decomposition pathway for metal alkyls

Requirements for β-Hydride Elimination:
  • A β-hydrogen on the alkyl group
  • A vacant coordination site on the metal (or ability to create one)
  • Syn-coplanar arrangement of M-C-C-H

Alkene Isomerization via β-H Elimination

M-CH₂-CH=CH₂ ⟷ M-H + CH₂=CH-CH₃ ⟷ M-CH(CH₃)-CH=CH₂

Sequential 1,2-insertion and β-elimination allows metal-catalyzed alkene isomerization

Chapter Summary

Key Concepts

  • 18-electron rule dominates stability
  • π-backbonding crucial for CO, alkenes
  • Hapticity describes ligand binding modes
  • Oxidation state changes drive reactivity

Important Ligands

  • CO: σ-donor, strong π-acceptor
  • Phosphines: tunable σ-donors
  • Cp: versatile, stabilizing, aromatic
  • Carbenes: Fischer vs Schrock types

Key Reactions

  • Ligand substitution (D or A activated)
  • Oxidative addition / Reductive elimination
  • Migratory insertion (1,1 and 1,2)
  • β-Hydride elimination

Applications

  • Catalytic hydrogenation
  • Alkene polymerization
  • Cross-coupling reactions
  • Hydroformylation