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Solid Rh crystals isomerize butene without dissolving

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A crystalline Rh σ-alkane complex swaps NBA for alkenes in the solid state and the porous ethene polymorph isomerizes 1-butene with high TOF.

Source

Solid-state molecular organometallic chemistry. Single-crystal to single-crystal reactivity and catalysis with light hydrocarbon substrates

Chadwick FM, McKay AI, Martinez-Martinez AJ, et al. · Chemical science · 2017

doi.org/10.1039/c7sc01491kRead the full paper ↗37 citationscc by

Study at a glance

Design
Other — Solid/gas SC-SC organometallic substitutions and polymorphic catalysis of 1-butene isomerization
N
Solid-state organometallic materials — no sample N
Population
Molecular organometallic crystals ([1-NBA]/[BArF4] ethene polymorphs)
Outcome
SC-SC reactivity and TOF differences between porous hexagonal and octahedral polymorphs

Structured fields used in claim comparison tables when every cited study has a complete layer.

What they did

Authors used solid/gas substitution, X-ray, SSNMR, periodic DFT/GIPAW shifts, and compared 1-butene isomerization TOFs of octahedral vs hexagonal ethene polymorphs.

What they found

NBA is a token ligand; SC-SC ethene substitution gives an octahedral anion cage. The hexagonal porous polymorph (25% void) reaches TOF(90%) = 1160 h–1 versus 20–29 h–1 for nonporous crystals.

The limits

What it doesn't show

Solution lifetimes are minutes; X-ray R-factors are high after SC-SC; industrial TON still far below silica-supported systems.

Key terms

SMOM-Cat
Solid-state molecular organometallic catalyst: a molecular crystal that catalyzes gas-phase reactions.
σ-alkane complex
Metal bound to C–H σ bonds of an alkane (here norbornane, NBA).
Single-crystal to single-crystal (SC-SC)
A reaction that preserves crystallinity so a new X-ray structure can be solved.
[BArF4]–
Bulky fluorinated borate anion that builds a cavity around the Rh cation.
γ-agostic
C–H···M interaction from a γ carbon, related to allyl-hydride isomerization TSs.

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Quiz yourself

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NBA in [1-NBA][BArF4] is best described as:

Common questions

What does NBA do?

Acts as a weakly bound token ligand that can be swapped for alkenes in the crystal.

Which polymorph is fastest?

Hexagonal porous [1-(ethene)2][BArF4]-Hex, TOF(90%) = 1160 h–1.

Can solution make the same species?

Often not as pure; many decompose within minutes when dissolved.

What is the pore volume of Hex?

About 25% solvent-accessible volume.

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