Diffraction Structure — Interdigitated conducting tetrathiafulvalene-based coordination networks

Measurement evidence

Diffraction Structure

Interdigitated conducting tetrathiafulvalene-based coordination networks · Bechu D., Xie L.S., Le Breton N. et al. · Chemical Communications · 2020 · 2407-2410

7 measurement groups · 48 results

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

powder X-ray diffraction

Network 4 iodine-treated powder/crystals for EPR, PXRD, and EDX · Powder

PXRD patterns of 4 and 5 before and after treatment with 0.05 M I2 in CHCl3, compared with simulated single-crystal data.

Context
native versus oxidised frameworks
Measurement source
p003 / journal p2409 · Oxidation discussion · Fig. 5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
crystallinity after iodine solution oxidationsamples remained crystalline with retention of the original structureText
Qualitative
p003 / journal p2409 · Oxidation discussion · Fig. 5

single-crystal X-ray diffraction

Network 4 as-synthesised single crystal · Single Crystal

Network 4; Bruker SMART CCD, Mo-Kalpha, 173 K; SHELXS/SHELXL refinement.

Temperature
173
Context
native framework structure
Measurement source
p005 · X-ray crystallography · Table 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
a-axis36.6636SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
b-axis9.568SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
beta angle121.372SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
c-axis20.1665SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
crystal systemMonoclinicSI Table
Exact Reported
p005 · X-ray crystallography · Table 1
formulaC41H27Cl9CoN6S18SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
R1 I>2sigma(I)0.0604SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
space groupC2/cSI Table
Exact Reported
p005 · X-ray crystallography · Table 1
unit-cell volume6040.1SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
wR2 I>2sigma(I)0.1663SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
Z4SI Table
Exact Reported
p005 · X-ray crystallography · Table 1

single-crystal X-ray diffraction after iodine treatment

Network 4 iodine-treated single crystal · Single Crystal

Network 4 single crystals exposed to 0.05 M I2 for 3 h; oxidised sample structure determined.

Atmosphere
0.05 M I2 in CHCl3
Context
oxidised framework structure
Measurement source
p003 / journal p2409 · Oxidation discussion
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
guest/counterion observation in oxidised 4 channelsCHCl3 observed; iodide-based residues not clearly identifiedText
Qualitative
p003 / journal p2409 · Oxidation discussion

single-crystal X-ray diffraction

Network 5 as-synthesised single crystal · Single Crystal

Network 5; Bruker SMART CCD, Mo-Kalpha, 173 K; SHELXS/SHELXL refinement.

Temperature
173
Context
native framework structure
Measurement source
p005 · X-ray crystallography · Table 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
a-axis36.701SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
b-axis9.6026SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
beta angle121.187SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
c-axis20.217SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
crystal systemMonoclinicSI Table
Exact Reported
p005 · X-ray crystallography · Table 1
formulaC41H27Cl9FeN6S18SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
R1 I>2sigma(I)0.0605SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
space groupC2/cSI Table
Exact Reported
p005 · X-ray crystallography · Table 1
unit-cell volume6095.3SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
wR2 I>2sigma(I)0.1391SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
Z4SI Table
Exact Reported
p005 · X-ray crystallography · Table 1

single-crystal X-ray diffraction

Ligand 1 in CH2Cl2 solution for cyclic voltammetry · Model

Molecular crystal structure; Bruker SMART CCD, Mo-Kalpha, 173 K; SHELXS/SHELXL refinement.

Temperature
173
Context
model linker structure
Measurement source
p005 · X-ray crystallography · Table 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
a-axis13.6086(6)SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
b-axis12.8562(6)SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
beta angle97.382(2)SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
c-axis11.7791(6)SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
formulaC18H12N2S8SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
R1 I>2sigma(I)0.0309SI Table
Exact Reported
p005 · X-ray crystallography · Table 1
space groupP21/cSI Table
Exact Reported
p005 · X-ray crystallography · Table 1
unit-cell volume2043.73(17)SI Table
Exact Reported
p005 · X-ray crystallography · Table 1

single-crystal X-ray structure analysis

Network 5 as-synthesised single crystal · Single Crystal

Main-text structural values for Fe network 5.

Context
native framework structure
Measurement source
p002 / journal p2408 · Structure discussion · Fig. 3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
EDT moiety bend in 534.36 degText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
central TTF C=C distance in 51.333(4) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Fe apical M-N distance2.110(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Fe basal M-N distance 12.241(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Fe basal M-N distance 22.250(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
S...S stacking distance maximum in 53.600(1) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
S...S stacking distance minimum in 53.530(1) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3

single-crystal X-ray structure analysis

Network 4 as-synthesised single crystal · Single Crystal

Main-text structural description for isostructural networks 4 and 5.

Context
native framework structure
Measurement source
p002 / journal p2408 · Structure discussion · Fig. 3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
EDT moiety bend in 434.27 degText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
central TTF C=C distance in 41.337(4) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Co apical M-N distance2.078(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Co basal M-N distance 12.201(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
Co basal M-N distance 22.205(3) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
coordination-network dimensionalityone-dimensional coordination network along the c axisText
Qualitative
p002 / journal p2408 · Structure discussion · Fig. 3
metal-cation separation within chain10.10 AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
S...S stacking distance maximum in 43.598(1) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3
S...S stacking distance minimum in 43.513(1) AText
Exact Reported
p002 / journal p2408 · Structure discussion · Fig. 3