Diffraction Structure — Continuous and reversible tuning of inter-layer spacings in two-dimensional conductive metal organic frameworks

Measurement evidence

Diffraction Structure

Continuous and reversible tuning of inter-layer spacings in two-dimensional conductive metal organic frameworks · Dontireddy G.M.R., Suman S.P., Merino-Gardea J.L. et al. · Journal of Materials Chemistry A · 2025 · 8734-8741

7 measurement groups · 12 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

PXRD before and after heating

Cu3HHTT2 multi-sample comparison series · Powder

Pristine Cu3HHTT2 compared with heat-treated Cu3HHTT2 at 90 deg C.

Temperature
363
Geometry
Powder PXRD
Context
water-free square-planar cMOF heat-control
Measurement source
p020 · Figure S14 · Fig. S14
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Cu3HHTT2 PXRD after heatingNo notable changes to diffraction patterns after 90 deg C heat treatment.Text
Qualitative
p005 · Solvent removal in Ni6HHTT3 · Fig. S14

PXRD peak full width at half maximum analysis

Ga9HHTP4 multi-sample comparison series · Powder

FWHM compared for in-plane 4.7 deg peak and inter-layer-stacking 25.8 deg peak.

Atmosphere
Ambient after post-treatment
Geometry
Powder PXRD
Context
pristine vs water/solvent-exchanged/dried Ga9HHTP4
Measurement source
p029 · Figure S23 · Fig. S23
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Ga9HHTP4 acetonitrile-soaked FWHM at 25.8 deg inter-layer peak~1.55 deg 2thetavisual estimateFigure Axis
Approximate
p029 · Figure S23 · Fig. S23b
Ga9HHTP4 pristine FWHM at 25.8 deg inter-layer peak~0.36 deg 2thetavisual estimateFigure Axis
Approximate
p029 · Figure S23 · Fig. S23b
Ga9HHTP4 water-soaked FWHM at 25.8 deg inter-layer peak~0.80 deg 2thetavisual estimateFigure Axis
Approximate
p006 · Discussion · Fig. S23b

Powder X-ray diffraction

Pristine Ga9HHTP4 powder · Powder

As-synthesised powder compared with simulated PXRD pattern.

Atmosphere
Ambient
Geometry
Cu Kalpha theta/2theta Bragg-Brentano geometry
Context
pristine
Measurement source
p002 · Results · Fig. S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Ga9HHTP4 phase purityExperimental PXRD matched simulated pattern; high crystallinity and phase purity.Text
Qualitative
p002 · Results · Fig. S1

PXRD after solvent exchange

Ga9HHTP4 multi-sample comparison series · Powder

Heat-treated Ga9HHTP4 soaked in water or organic solvents overnight, then compared by PXRD.

Atmosphere
Ambient measurement after post-treatment
Geometry
Powder PXRD
Context
solvent-exchanged samples compared with pristine and heated samples
Measurement source
p004 · Solvent removal/exchange in Ga9HHTP4 · Fig. 2 and Fig. S10
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Organic solvent-exchanged Ga9HHTP4 inter-layer spacing range3.29-3.35 AngstromrangeText
Range
p004 · Solvent removal/exchange in Ga9HHTP4 · Fig. 2b,c and Fig. S10
Water-soaked HT-Ga9HHTP4 inter-layer spacingfrom 3.27 to 3.42 AngstromText
Exact Reported
p003 · Solvent removal/exchange in Ga9HHTP4 · Fig. 2b,c and Fig. S8

In situ variable-temperature PXRD under reduced pressure

Heat-treated Ga9HHTP4 (HT-Ga9HHTP4) · Powder

Ga9HHTP4 under reduced pressure; 30 min vacuum at room temperature, then stepwise heating to 85 deg C.

Temperature
298-358
Atmosphere
Reduced pressure / vacuum
Geometry
Anton Paar XRK 900 furnace-type heater in PXRD; ceramic sample holder
Context
post-synthetic heat treatment compared with pristine
Measurement source
p003 · Solvent removal/exchange in Ga9HHTP4 · Fig. 1d,e and Fig. S6
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Heat-treated Ga9HHTP4 inter-layer spacing3.27 Angstrom after shift to 27.2 degText
Exact Reported
p003 · Solvent removal/exchange in Ga9HHTP4 · Fig. 1e
Pristine Ga9HHTP4 inter-layer spacing3.45 AngstromText
Exact Reported
p003 · Solvent removal/exchange in Ga9HHTP4 · Fig. 1e

Powder X-ray diffraction

Pristine Ni6HHTT3 powder · Powder

As-synthesised powder compared with simulated PXRD pattern.

Atmosphere
Ambient
Geometry
Cu Kalpha theta/2theta Bragg-Brentano geometry
Context
pristine
Measurement source
p007 · Figure S1 · Fig. S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Ni6HHTT3 phase purityExperimental PXRD matched simulated pattern; high crystallinity and phase purity.Caption
Qualitative
p007 · Figure S1 · Fig. S1

Variable-temperature PXRD under reduced pressure

Heat-treated Ni6HHTT3 · Powder

Ni6HHTT3 under reduced pressure at room temperature and upon heating to 90 deg C.

Temperature
298-363
Atmosphere
Reduced pressure / vacuum
Geometry
PXRD with temperature-control stage
Context
heated sample compared with pristine
Measurement source
p005 · Solvent removal in Ni6HHTT3 · Fig. 3 and Fig. S13
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Heat-treated Ni6HHTT3 inter-layer spacing3.28(6) Angstrom(6)Text
Exact Reported
p005 · Solvent removal in Ni6HHTT3 · Fig. 3c
Pristine Ni6HHTT3 inter-layer spacing3.30(2) Angstrom(2)Text
Exact Reported
p005 · Solvent removal in Ni6HHTT3 · Fig. 3c