Diffraction Structure — Million-fold electrical conductivity enhancement in Fe2(DEBDC) versus Mn2(DEBDC) (E = S, O)

Measurement evidence

Diffraction Structure

Million-fold electrical conductivity enhancement in Fe2(DEBDC) versus Mn2(DEBDC) (E = S, O) · Sun L., Hendon C.H., Minier M.A. et al. · Journal of the American Chemical Society · 2015 · 6164-6167

2 measurement groups · 14 results

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

PXRD and variable-temperature PXRD

X-ray diffraction and scattering

Fe2(DSBDC)(DMF)2 · Pellet

Room-temperature and variable-temperature PXRD under dynamic vacuum from 25 to 200 degC.

Temperature: 298-473
Atmosphere: dynamic vacuum for VT-PXRD; N2-filled glovebox sample preparation
Geometry: Bruker D8 Advance for PXRD; PANalytical X'pert Pro with Anton Parr HTK 1200 N for VT-PXRD
Context: pristine guest-free and guest-loaded Fe2(DSBDC)
Measurement source: S23 · Breathing behavior and PXRD pattern simulation · Figures S6-S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
hexagon area reduction on distortion	9.6%	—	—	Text Exact Reported	S29 · Breathing behavior and PXRD pattern simulation
distorted guest-free phase unit-cell a	51.41 A	—	—	Text Exact Reported	S29 · Breathing behavior and PXRD pattern simulation
distorted guest-free phase unit-cell b	37.27 A	—	—	Text Exact Reported	S29 · Breathing behavior and PXRD pattern simulation
distorted guest-free phase gamma angle	111.25 deg	—	—	Text Exact Reported	S29 · Breathing behavior and PXRD pattern simulation
distorted guest-free phase space group	P-1	—	—	Text Exact Reported	S29 · Breathing behavior and PXRD pattern simulation · Figures S13-S18
new PXRD peaks appearance temperature	7.9 deg and 11.6 deg peaks appeared at 35 degC	—	—	Text Exact Reported	S23 · Breathing behavior and PXRD pattern simulation · Figure S7
phase A peak disappearance temperature	6.4 deg peak completely disappeared at 65 degC	—	—	Text Exact Reported	S23 · Breathing behavior and PXRD pattern simulation · Figure S7

single-crystal X-ray diffraction

X-ray diffraction and scattering

Fe2(DSBDC)(DMF)2.x(DMF) · Pellet

Low-temperature 100 K diffraction with Mo Kalpha radiation; SHELXS/SHELXL refinement.

Temperature: 100
Atmosphere: Kapton loop with paratone-N oil
Geometry: Bruker-AXS X8 Kappa Duo with Smart APEX II CCD detector
Context: pristine guest-loaded framework
Measurement source: S3 · X-ray diffraction studies · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
unit-cell a	27.551(4) A	—	(4)	SI Table Exact Reported	S10 · Table S1 · Table S1
unit-cell c	7.1879(11) A	—	(11)	SI Table Exact Reported	S10 · Table S1 · Table S1
Fe-S bond length	2.444(2) A	—	(2)	Text Exact Reported	6164 · main text · Figure 1
Fe-S bond length	2.446(2) A	—	(2)	Text Exact Reported	6164 · main text · Figure 1
van der Waals pore diameter	ca. 16 A	—	—	Text Approximate	6164 · main text · Figure 1b
crystal system and space group	Trigonal, R-3	—	—	SI Table Exact Reported	S10 · Table S1 · Table S1
unit-cell volume	4725.0(13) A3	—	(13)	SI Table Exact Reported	S10 · Table S1 · Table S1