Synthesis evidence

High-κ Samarium-Based Metal-Organic Framework for Gate Dielectric Applications

Pathak A., Chiou G.R., Gade N.R. et al. · ACS Applied Materials and Interfaces · 2017 · 21872-21878

2 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

p002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)

Metal precursorsSm(NO3)3.6H2O (67.0 mg, 0.20 mmol)
Linker precursorsbenzenehexacarboxylic acid (H6bhc) (34.2 mg, 0.10 mmol)
SolventsEtOH and H2O, 1:3 v/v
Additives1 drop of 1.0 M KOH solution
Atmospherenot specified
Temperature170
Time72
Work-upColorless hexagonal crystals isolated on a filter, washed thoroughly with water, and dried at room temperature.
ActivationDried at room temperature; no high-temperature activation reported for as-synthesised crystals.
Scalability contextYield 55.1% (41.8 mg; 0.05 mmol) reported for the KOH-assisted route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSm(NO3)3.6H2O67.0 mg, 0.20 mmolp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
Linkerbenzenehexacarboxylic acid (H6bhc)34.2 mg, 0.10 mmolp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
SolventEtOH and H2O1:3 v/v mixture; total volume not statedp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
BaseKOH solution1 drop · 1.0 Mp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
Vague recipeSource: Main

Route 2: Hydrothermal

p002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)

Metal precursorsSm(NO3)3.6H2O
Linker precursorsbenzenehexacarboxylic acid (H6bhc)
SolventsEtOH and H2O, inferred same solvent system as KOH-assisted route
Additivesnone; absence of KOH
Atmospherenot specified
Temperature170
Time72
Work-upnot separately specified; stated to use similar reaction conditions
Scalability contextProduct yields are lower than the KOH-assisted 55.1% route; exact yield not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSm(NO3)3.6H2Onot separately specifiedp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
Linkerbenzenehexacarboxylic acid (H6bhc)not separately specifiedp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)
SolventEtOH and H2Onot separately specified; similar conditionsp002 / journal page 21873 · 2.2. Synthesis of [Sm2(bhc)(H2O)6]n (1)