Diffraction Structure — Novel Topology in Semiconducting Tetrathiafulvalene Lanthanide Metal-Organic Frameworks

4 measurement groups · 15 results

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

Powder X-ray diffraction, Bruker Advance II, Ni-filtered Cu Kalpha radiation

X-ray diffraction and scattering

phase-pure Lu6(TTFTB)5 bulk sample · Powder

Theta/2theta Bragg-Brentano geometry; 40 kV and 40 mA; thin layer on zero-background silicon crystal plate.

Context: pristine framework powder
Measurement source: p004 · main text · Figure 4a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
phase assignment by PXRD	phase-pure and isostructural to Tm6(TTFTB)5	—	—	Text Qualitative	p004 · main text · Figure 4a

Selected TTF-core bond lengths and intermolecular S...S distances from crystallographic model

diffraction-quality Tm6(TTFTB)5 red rhombic crystals · Single Crystal

Bond lengths from Table S2; S...S contacts discussed from Figures 3 and main text.

Temperature: 100
Context: pristine framework single crystal
Measurement source: S5 · Table S2 · Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
shortest intermolecular S...S contactMarked as a best value within this paper	as short as 3.72 A	—	—	Text Rounded Reported	p004 · main text · Figure 3
TTF1 C1-C2 bond length	1.331(5) A	—	0.005 A	SI Table Exact Reported	S5 · Table S2 · Table S2
TTF1/TTF3 close S...S distance 1	4.044(3) A	—	0.003 A	Text Exact Reported	p004 · main text · Figure 3
TTF1/TTF3 close S...S distance 2	4.411(3) A	—	0.003 A	Text Exact Reported	p004 · main text · Figure 3
TTF2 C1-C2 bond length	1.345(5) A	—	0.005 A	SI Table Exact Reported	S5 · Table S2 · Table S2
TTF3 C1-C1 bond length	1.337(8) A	—	0.008 A	SI Table Exact Reported	S5 · Table S2 · Table S2

Single-crystal X-ray diffraction with Mo Kalpha radiation on Bruker-AXS X8 Kappa Duo / Smart APEX II CCD

X-ray diffraction and scattering

diffraction-quality Tm6(TTFTB)5 red rhombic crystals · Single Crystal

Solvated single crystal mounted in Paratone oil on Kapton loop; low-temperature data at 100 K; solved with SHELXT and refined with SHELXL-2016; SQUEEZE/PLATON used for residual electron density.

Temperature: 100
Context: pristine framework single crystal
Measurement source: S2-S4 · Single crystal X-ray diffraction · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit cell a	a = 18.0429(12) A	—	0.0012 A	SI Table Exact Reported	S4 · Table S1 · Table S1
unit cell b	b = 19.3054(13) A	—	0.0013 A	SI Table Exact Reported	S4 · Table S1 · Table S1
unit cell c	c = 20.1294(13) A	—	0.0013 A	SI Table Exact Reported	S4 · Table S1 · Table S1
final R1 index, I > 2sigma(I)	R1 = 0.0412	—	—	SI Table Exact Reported	S4 · Table S1 · Table S1
space group	P-1	—	—	SI Table Exact Reported	S4 · Table S1 · Table S1
network topology	(3,3,3,6,6)-coordinated net, point symbol (4.6^2)2(4^2.6)4(4^6.6^4.8^5)(4^6.6^6.8^3)2, named lsx	—	—	Text Qualitative	p004 · main text · Figure 2
unit-cell volume	6353.2(7) A3	—	0.7 A3	SI Table Exact Reported	S4 · Table S1 · Table S1

Powder X-ray diffraction, Bruker Advance II, Ni-filtered Cu Kalpha radiation

X-ray diffraction and scattering

phase-pure Yb6(TTFTB)5 bulk sample · Powder

Theta/2theta Bragg-Brentano geometry; 40 kV and 40 mA; thin layer on zero-background silicon crystal plate.

Context: pristine framework powder
Measurement source: p004 · main text · Figure 4a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
phase assignment by PXRD	phase-pure and isostructural to Tm6(TTFTB)5	—	—	Text Qualitative	p004 · main text · Figure 4a