Diffraction Structure — Paramagnetic Conducting Metal–Organic Frameworks with Three-Dimensional Structure

4 measurement groups · 14 results

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

Three-dimensional electron diffraction / selected-area electron diffraction

Electron diffraction

Co-THBQ well-crystallised powder · Powder

Themis 300 TEM, 300 kV, lambda 0.01971 A; sample cooled to 94 K; -45 to 50 deg range with 1 deg step; 2 s exposure; 96 frames; solved/refined with Olex2.

Temperature: 94
Geometry: nanocrystal on copper grid
Context: pristine Co-THBQ
Measurement source: 3,7 · Structure determination · Figure S6; Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
3D electron diffraction unit cell a	10.6776(12) A	—	0.0012 A	SI Table Exact Reported	7 · Table S2 · Table S2
3D electron diffraction R1 for I >= 2 sigma(I)	0.235	—	—	SI Table Exact Reported	7 · Table S2 · Table S2

Synchrotron powder X-ray diffraction with Rietveld refinement

X-ray diffraction and scattering

Co-THBQ well-crystallised powder · Powder

Beamline BL14B1 at SSRF; powder in flame-sealed 0.5 mm boron-rich glass capillary; room temperature; wavelength 0.690026 A.

Temperature: room temperature
Atmosphere: sealed capillary
Geometry: powder in capillary
Context: pristine framework powder
Measurement source: 7 · Table S1 · Table S1; Figure S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
distance between neighbouring parallel C6 rings	2.747 A	—	—	Text Exact Reported	2 · Crystal structure discussion · Figure 2
unit cell a	10.677 A	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
Rietveld refinement statistics	Rwp 3.10%; Rp 2.29%; GOF 1.31	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
space group	Pm-3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
unit cell volume	1217.2 A3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1

Synchrotron powder X-ray diffraction with Rietveld refinement

X-ray diffraction and scattering

Fe-THBQ black powder · Powder

Beamline BL14B1 at SSRF; microcrystalline sample in flame-sealed 0.5 mm boron-rich glass capillary; room temperature; 2-52 deg, 0.003 deg step, wavelength 0.690026 A.

Temperature: room temperature
Atmosphere: sealed capillary
Geometry: powder in capillary
Context: pristine framework powder
Measurement source: 2,7 · Structure determination · Table S1; Figure S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit cell a	10.580 A	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
Rietveld refinement statistics	Rwp 1.98%; Rp 1.32%; GOF 1.52	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
space group	Pm-3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
unit cell volume	1184.3 A3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1

Synchrotron powder X-ray diffraction indexing

X-ray diffraction and scattering

Mn-THBQ powder · Powder

Beamline BL14B1 at SSRF; powder in flame-sealed capillary; room temperature; wavelength 0.690026 A.

Temperature: room temperature
Atmosphere: sealed capillary
Geometry: powder in capillary
Context: pristine framework powder
Measurement source: 7 · Table S1 · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit cell a	10.699 A	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
space group	Pm-3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1
unit cell volume	1224.7 A3	—	—	SI Table Exact Reported	7 · Table S1 · Table S1