Synthesis · Electrical semiconduction modulated by light in a cobalt and naphthalene diimide metal-organic framework

3 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Solvothermal

6 · Methods - Synthesis of MOF-CoNDI-py-2

Metal precursorsCo(NO3)2.6H2O

Linker precursorsNDI-py and TpA (terephthalic acid)

Solvents50 mL N,N-dimethylformamide

Atmospherenot specified

Temperature80

Time48

Work-upallowed to cool to room temperature; crystals collected by filtration and washed thoroughly with N,N-dimethylformamide

Activationno general activation reported; powder XRD samples dried at 300 deg C for 3 h and FTIR samples treated at 100 deg C for 3 h before analysis

Scalability contextYield based on NDI-py ligand was 50%.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.48 mmol	6 · Methods - Synthesis of MOF-CoNDI-py-2
Linker	NDI-py	0.24 mmol	6 · Methods - Synthesis of MOF-CoNDI-py-2
Linker	TpA	0.48 mmol	6 · Methods - Synthesis of MOF-CoNDI-py-2
Solvent	N,N-dimethylformamide	50 mL	6 · Methods - Synthesis of MOF-CoNDI-py-2

Complete recipeSource: Main

Route 2: Other

6 · Methods - Electronic device · Fig. 6; Supplementary Fig. 5

Metal precursorsAu electrodes; Ti adhesion layer; trimethyl(methylcyclopentadienyl)platinum(IV) Pt deposition precursor

Linker precursorspreformed MOF-CoNDI-py-2 crystals

Solventsacetone suspension; acetone ultrasonic cleaning bath

Atmospherenitrogen flow drying after acetone cleaning; FIB chamber atmosphere not specified

Temperature50 for Pt precursor crucible

Substrate orientation200 nm SiO2 on p-Si substrate; Au contact pads labelled t1, t2, b1, b2

Work-upsubstrates cleaned in acetone ultrasound bath for 5 min and dried over nitrogen; MOF crystals deposited from acetone suspension; Pt contacts deposited by vapour directed through needle in FIB system

Activationnot reported

Scalability contextDevice fabrication is single-crystal/contact fabrication, not bulk MOF synthesis.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	p-Si substrate with 200 nm SiO2	Not specified	6 · Methods - Electronic device · Fig. 6; Supplementary Fig. 5
Other	Au electrodes with Ti pre-layer	Not specified	6 · Methods - Electronic device · Fig. 6; Supplementary Fig. 5
Solvent	acetone	Not specified	6 · Methods - Electronic device · Fig. 6; Supplementary Fig. 5
Metal Source	trimethyl(methylcyclopentadienyl)platinum(IV) (Aldrich, 98%)	Not specified	6 · Methods - Electronic device · Fig. 6; Supplementary Fig. 5

Complete recipeSource: Both

Route 3: Other

6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11

Linker precursors1,4,5,8-naphthalic dianhydride; 4-aminopyridine

Solventsmolten imidazole; H2O:EtOH:HNO3 10:10:1 workup; H2O, EtOH and Et2O washes; DMF recrystallisation

Additivesimidazole; nitric acid in workup mixture

Atmospherenot specified

Temperature130

Time0.5

Work-upcooled to room temperature; treated with H2O:EtOH:HNO3 10:10:1; filtered; washed again with same solution, then H2O, EtOH and Et2O; recrystallised in DMF

Activationnot reported

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	1,4,5,8-naphthalic dianhydride (Aldrich)	503.7 mg (1.88 mmol)	6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11
Linker	4-aminopyridine (Acros)	543.4 mg (5.77 mmol)	6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11
Additive	molten imidazole (Vetec)	ca 2 g	6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11
Solvent	H2O:EtOH:HNO3 10:10:1 (v/v, Synth)	Not specified	6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11
Solvent	DMF	recrystallisation solvent	6 · Methods - Synthesis of NDI-py · Supplementary Fig. 11