Synthesis · CO2-Sensitive Porous Magnet: Antiferromagnet Creation from a Paramagnetic Charge-Transfer Layered Metal-Organic Framework

Partial recipeSource: Main

Route 1: Other

p009 · Single Crystal X-ray Crystallography

Metal precursorsactivated compound 1

Linker precursorsactivated compound 1

Solventsnone; gas dosing

AdditivesCO2 gas

Atmosphere100 kPa CO2; cooled using N2 gas stream for SCXRD

Temperatureroom temperature dosing followed by cooling to -78.15 C (195 K)

Timenot specified for CO2 dosing/cooling

Substrate orientationsingle crystal mounted in silica glass capillary for SCXRD

Oxidant / reductantCO2 guest, not a redox reagent

Work-upin situ gas loading; no isolation workup reported

Activationstarting compound 1 obtained by vacuum heating at 400 K for 12 h

Scalability contextIn situ guest loading; not a bulk synthetic scale-up route.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1 single crystal	0.112 x 0.045 x 0.045 mm3 crystal	p009 · Single Crystal X-ray Crystallography
Other	CO2 gas	100 kPa	p009 · Single Crystal X-ray Crystallography

Complete recipeSource: Main

p008-p009 · Materials and Synthesis

Metal precursors[Ru2(2,4-F2PhCO2)4(THF)2], 3.90 mg, 0.04 mmol, in 2 mL benzene

Linker precursorsTCNQ(OEt)2, 5.9 mg, 0.02 mmol, dissolved in benzene and divided into 2 mL portions

Solventsbenzene (PhH), distilled under N2

Additivesnone reported

Atmosphereinert atmosphere; Schlenk-line techniques and glovebox; solvents distilled under N2

Temperaturenot specified for 1 week layering; activation at 126.85 C (400 K)

Time168 h crystallisation; 12 h activation

Substrate orientationnarrow glass tubes, inner diameter 8 mm; bottom/top liquid layers

Oxidant / reductantnone reported

Work-upblock-shaped dark brown crystals isolated as 1-PhH; detailed collection/washing not specified

Activationheat 1-PhH crystals at 400 K under vacuum for 12 h to obtain 1

Scalability contextSmall-batch layered crystallisation in narrow glass tubes; no scale-up described.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	[Ru2(2,4-F2PhCO2)4(THF)2]	3.90 mg; 0.04 mmol · in 2 mL benzene	p008-p009 · Materials and Synthesis
Linker	TCNQ(OEt)2	5.9 mg; 0.02 mmol · dissolved in 20 mL benzene; divided into 2 mL portions	p008-p009 · Materials and Synthesis
Solvent	benzene (PhH)	2 mL metal-source layer plus 20 mL linker stock	p008-p009 · Materials and Synthesis