cMOF Evidence Base
Diffraction Structure — Electronic Conductivity, Ferrimagnetic Ordering, and Reductive Insertion Mediated by Organic Mixed-Valence in a Ferric Semiquinoid Metal-Organic Framework

Measurement evidence

Diffraction Structure

Electronic Conductivity, Ferrimagnetic Ordering, and Reductive Insertion Mediated by Organic Mixed-Valence in a Ferric Semiquinoid Metal-Organic Framework · Darago L.E., Aubrey M.L., Yu C.J. et al. · Journal of the American Chemical Society · 2015 · 15703-15711

2 measurement groups · 13 results

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

High-resolution powder X-ray diffraction

X-ray diffraction and scattering

Brown microcrystalline powder of 2 · Powder

Microcrystalline samples loaded in 1.0 mm boron-rich glass capillaries in Ar glovebox and flame-sealed; lambda = 0.72768 A.

Temperature
100
Atmosphere
Ar during loading; sealed capillaries
Geometry
Powder in capillary
Context
Reduced frameworks compared with simulated 1
Measurement source
S-4 · Powder X-Ray Diffraction · Figures S3-S4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD comparison of 2 with simulated 1almost perfectly overlays with simulated 1; little if any change in unit cell——Text
Qualitative		4 · Chemical Reduction of 1 · Figure S3
PXRD comparison of Na3.2 derivative with 1almost perfectly overlays with that of 1——Text
Qualitative		4 · Chemical Reduction of 1 · Figure S4
Electron count introduced in 20.7 e- per mole of 1——Text
Rounded Reported		4 · Chemical Reduction of 1
ICP Fe:Na ratio of 2Fe:Na, 2.23(1):1—(1)Text
Exact Reported		2 · Experimental Section
Na insertion in 2 from ICP0.9 mol equiv of Na+ ions per mole of 1——Text
Rounded Reported		2 · Experimental Section

Single-crystal X-ray diffraction

X-ray diffraction and scattering

Black cubic crystals of 1 · Single Crystal

Synchrotron radiation lambda = 0.8856 A; Bruker PHOTON100 CMOS; structure solved with SHELXS and refined with SHELXL/OLEX2.

Temperature
100
Atmosphere
N2 cryostream
Geometry
Single crystals in Paratone-N oil on MiTeGen loops
Context
Pristine framework 1
Measurement source
S-4 · Single Crystal X-Ray Diffraction · Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Unit-cell a parameter of 122.1401(5)—(5)SI Table
Exact Reported		S-7 · Table S1 · Table S1
Calculated density of 11.237——SI Table
Exact Reported		S-7 · Table S1 · Table S1
Fe-O1 bond distance in 12.005(7)—(7)Caption
Exact Reported		S-9 · Figure S2 · Figure S2
Fe-O2 bond distance in 12.030(7)—(7)Caption
Exact Reported		S-9 · Figure S2 · Figure S2
Final R1 for 1, I > 2sigma(I)R1 = 0.0733——SI Table
Exact Reported		S-7 · Table S1 · Table S1
Space group of 1I-43d——SI Table
Exact Reported		S-7 · Table S1 · Table S1
Unit-cell volume of 110852.7(7)—(7)SI Table
Exact Reported		S-7 · Table S1 · Table S1
Z of 18——SI Table
Exact Reported		S-7 · Table S1 · Table S1