cMOF Evidence Base
Diffraction Structure — CO2-Sensitive Porous Magnet: Antiferromagnet Creation from a Paramagnetic Charge-Transfer Layered Metal-Organic Framework

Measurement evidence

Diffraction Structure

CO2-Sensitive Porous Magnet: Antiferromagnet Creation from a Paramagnetic Charge-Transfer Layered Metal-Organic Framework · Zhang J., Kosaka W., Liu Q. et al. · Journal of the American Chemical Society · 2023 · 26179-26189

2 measurement groups · 14 results

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

In situ powder X-ray diffraction under CO2

X-ray diffraction and scattering

Activated crystals of compound 1 · Single Crystal

Ground sample sealed in silica capillary connected to BELSORP MAX; Cu Kalpha radiation; CO2 pressures 3.2, 10, 32, and 100 kPa; temperature varied under N2 stream.

Temperature
160-310
Atmosphere
CO2 at fixed pressures
Geometry
silica glass capillary PXRD
Context
pristine framework converting reversibly to CO2-loaded phase
Measurement source
p009 · Physical Property Measurements · Figure 2; Figures S6-S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD complete conversion temperature at 100 kPa CO2complete conversion to 1-CO2 at 250 K; mixed phases between 260 and 270 K; 1 remains above 280 K——Text
Rounded Reported		p004 · Structural Characterization of 1-CO2 · Figure 2a

In situ single-crystal X-ray diffraction

X-ray diffraction and scattering

CO2-dosed single crystal of 1 for SCXRD · Single Crystal

100 kPa CO2 introduced at room temperature and slowly cooled to 195 K; Mo Kalpha radiation; structure solved/refined with SHELXT/F2 refinement.

Temperature
195
Atmosphere
100 kPa CO2
Geometry
single crystal in silica capillary connected to gas handling system
Context
guest-loaded framework phase
Measurement source
p009 · Single Crystal X-ray Crystallography · Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Crystallographically accommodated CO2 contentMarked as a best value within this paperthree molar equivalents of CO2 inside pores3 CO2 per formula unit—Text
Exact Reported		p005 · Structural Characterization of 1-CO2 · Figure 2
TCNQ(OEt)2 dihedral angle in 1-CO28.03 degrees (SI Table S6); main text reports 7.86 degrees—minor source discrepancySI Table
Exact Reported		S31 · Table S6 · Table S6
Ru-N-C bonding angle in 1-CO2144.8 degrees for 1-CO2 vs 131.9 degrees for 1—Table S2 gives 144.8(12)/144.7(12)Text
Rounded Reported		p005 · Structural Characterization of 1-CO2 · Table S2
Average Ru-Oeq length for [Ru(1)2] in 1-CO22.027 A——SI Table
Exact Reported		S21 · Discussion on oxidation state · Table S2
Average Ru-Oeq length for [Ru(2)2] in 1-CO22.071 A——SI Table
Exact Reported		S21 · Discussion on oxidation state · Table S2
Unit cell a parameter10.2498(12) A—(12)SI Table
Exact Reported		S18 · Table S1 · Table S1
Unit cell b parameter13.6541(16) A—(16)SI Table
Exact Reported		S18 · Table S1 · Table S1
Unit cell c parameter16.1061(16) A—(16)SI Table
Exact Reported		S18 · Table S1 · Table S1
SCXRD formula for 1-CO2C75H36F16N4O24Ru4——SI Table
Exact Reported		S18 · Table S1 · Table S1
Space group of 1-CO2triclinic P-1——SI Table
Exact Reported		S18 · Table S1 · Table S1
Unit cell volume1959.4(4) A3—(4)SI Table
Exact Reported		S18 · Table S1 · Table S1
Void volume of 1-CO2227.1 A3 (11.6% of total volume)11.6 % of total volume—Text
Exact Reported		p005 · Structural Characterization of 1-CO2 · Figure 2
Void volume of parent 1121.6 A3 (6.6% of total volume)6.6 % of total volume—Text
Exact Reported		p005 · Structural Characterization of 1-CO2 · Figure 2