cMOF Evidence Base
Diffraction Structure — Design and synthesis of hydroxide ion-conductive metal-organic frameworks based on salt inclusion

Measurement evidence

Diffraction Structure

Design and synthesis of hydroxide ion-conductive metal-organic frameworks based on salt inclusion · Sadakiyo M., Kasai H., Kato K. et al. · Journal of the American Chemical Society · 2014 · 1702-1705

4 measurement groups · 12 results

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

In-house X-ray powder diffraction (XRPD), Rigaku SmartLab, Cu K-alpha line

X-ray diffraction and scattering

NBu4-ZIF-8 powder · Powder

Patterns of calculated ZIF-8, ZIF-8, and NBu4-ZIF-8 compared.

Geometry
Powder diffraction
Context
Salt-loaded NBu4-ZIF-8 compared with pristine ZIF-8.
Measurement source
S2 · X-ray crystal structure analysis · Figure S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Framework retention after salt inclusionNBu4-ZIF-8 diffraction pattern fundamentally same as starting ZIF-8, with changed relative intensities——Text
Qualitative		1703 · XRPD · Figure S5

Maximum entropy method electron-density visualisation from synchrotron XRPD

X-ray diffraction and scattering

NBu4-ZIF-8 powder · Powder

MEM-Rietveld analysis comparing ZIF-8 and NBu4-ZIF-8 electron density.

Temperature
300
Atmosphere
Vacuum-packed capillary
Context
Salt-loaded sample compared with pristine ZIF-8.
Measurement source
1703 · Structure characterisation · Figure 2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Additional electron density in pore centreAdditional charge found around cage center in NBu4-ZIF-8; ZIF-8 showed no charge localisation in pore——Text
Qualitative		1703 · Electron density · Figure 2
MEM isodensity surface level0.15 e A-3——Caption
Exact Reported		1703 · Figure 2 caption · Figure 2

Synchrotron XRPD Rietveld refinement

X-ray diffraction and scattering

NBu4-ZIF-8 powder · Powder

BL44B2 at SPring-8; wavelength 0.499081(1) angstrom; vacuum-packed borosilicate capillary irradiated for 14 min at 300 K.

Temperature
300
Atmosphere
Vacuum-packed capillary
Geometry
Debye-Scherrer camera with imaging plate detector
Context
Salt-loaded NBu4-ZIF-8 refinement with disorder model for NBu4 sites.
Measurement source
S2 · X-ray crystal structure analysis · Table S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
NBu4 N2 site occupancyg of N2 in NBu4 fixed at 0.7——Text
Exact Reported		S2 · X-ray crystal structure analysis · Table S2
NBu4-ZIF-8 lattice constant aa = 16.9926(1) angstrom—(1)SI Table
Exact Reported		S9 · Table S2 · Table S2
NBu4-ZIF-8 RIRI = 6.4%——SI Table
Exact Reported		S9 · Table S2 · Table S2
NBu4-ZIF-8 RwpRwp = 2.5%——SI Table
Exact Reported		S9 · Table S2 · Table S2
NBu4-ZIF-8 space groupI-43m (No. 217)——SI Table
Exact Reported		S9 · Table S2 · Table S2

Synchrotron XRPD Rietveld refinement

X-ray diffraction and scattering

ZIF-8 powder · Powder

BL44B2 at SPring-8; wavelength 0.799139(1) angstrom; vacuum-packed borosilicate capillary irradiated for 2.5 min at 300 K.

Temperature
300
Atmosphere
Vacuum-packed capillary
Geometry
Debye-Scherrer camera with imaging plate detector
Context
Pristine ZIF-8 refinement.
Measurement source
S2 · X-ray crystal structure analysis · Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
ZIF-8 lattice constant aa = 17.04354(4) angstrom—(4)SI Table
Exact Reported		S8 · Table S1 · Table S1
ZIF-8 RIRI = 4.1%——SI Table
Exact Reported		S8 · Table S1 · Table S1
ZIF-8 RwpRwp = 1.9%——SI Table
Exact Reported		S8 · Table S1 · Table S1
ZIF-8 space groupI-43m (No. 217)——SI Table
Exact Reported		S8 · Table S1 · Table S1