Diffraction Structure — Direct Observation of Confined I−⋅⋅⋅I2⋅⋅⋅I− Interactions in a Metal–Organic Framework: Iodine Capture and Sensing

6 measurement groups · 57 results

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

Powder X-ray diffraction of crushed single crystals and calculated PXRD comparison.

X-ray diffraction and scattering

I2@1 iodine-loaded crystals · Single Crystal

PXRD at 293 K, Cu-Kalpha, scans 5 to 60 degrees at 5 degrees/min; patterns compared for G@1, 1, I2@1 and repeated iodine loading/release.

Temperature: 293
Atmosphere: ambient PXRD
Geometry: crushed single-crystal powder
Context: Pristine and guest-loaded/released framework states.
Measurement source: p003 / SI p.2 · General description · Figure 1b-c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
PXRD similarity after activation from G@1 to 1	PXRD data for 1 is similar to parent G@1	—	—	Text Qualitative	p002 / article p.8410 · Main text · Figure 1b
PXRD after repeated iodine loading/release cycles	after 3 and 5 times of iodine loading and release	—	—	Caption Exact Reported	p002 / article p.8410 · Figure caption · Figure 1c
Crystallinity retained after iodine uptake	PXRD indicated I2 uptake did not compromise crystallinity	—	—	Text Qualitative	p002 / article p.8410 · Main text · Figure 1b

Single-crystal X-ray diffraction on Bruker SMART APEX II CCD with Mo Kalpha radiation at 150 K.

X-ray diffraction and scattering

Activated compound 1 single crystals · Single Crystal

Crystal structure of activated 1; channel dimensions, void volume and iodide separations analysed.

Temperature: 150
Geometry: single crystal
Context: Pristine activated framework.
Measurement source: p006 / SI p.5 · X-ray Crystallography · Table S2; Figure S4-S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Compartmentalised channel A void size from coordinated DMF	4.066-4.538 A	—	—	Text Range	p004 / article p.8412 · Main text · Figure S13
Adjacent chain I...I separation in channel A of 1	9.232(2) A	—	0.002 A	Text Exact Reported	p004 / article p.8412 · Main text · Figure S12a
Channel A window dimensions in 1	ca. 7.2 x 10.0 A	—	—	Text Approximate	p002 / article p.8410 · Main text · Figure 1a; Figure S5
Long adjacent chain I...I separation in channel B of 1	11.803(2) A	—	0.002 A	Text Exact Reported	p004 / article p.8412 · Main text · Figure S12b
Short adjacent chain I...I separation in channel B of 1	7.769(2) A	—	0.002 A	Text Exact Reported	p004 / article p.8412 · Main text · Figure S12b
Channel B window dimensions in 1	ca. 7.2 x 7.6 A	—	—	Text Approximate	p002 / article p.8410 · Main text · Figure 1a; Figure S5
1 crystallographic formula	C21H19Cu4I4N4O7Tb	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 crystal system	Monoclinic	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 crystallographic measurement temperature	150(2) K	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 calculated density	2.514 g cm-3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 R1 and wR2 for I > 2sigma(I)	0.0230, 0.0481	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 space group	P21/n	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 unit-cell parameters a,b,c,beta	15.005(4), 8.341(2), 29.272(8); beta 101.167(4)	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
1 unit-cell volume	3594 A3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
Solvent-accessible volume of 1	ca. 530.3 A3, corresponding to 14.8% of the unit cell	14.8 % unit cell	—	Text Approximate	p002 / article p.8410 · Main text · Figure S5

Single-crystal X-ray diffraction on Bruker SMART APEX II CCD with Mo Kalpha radiation at 298 K.

X-ray diffraction and scattering

EtOH@1 crystals · Single Crystal

Structure of EtOH@1 solvent-loaded control.

Temperature: 298
Geometry: single crystal
Context: Ethanol guest-loaded control.
Measurement source: p006 / SI p.5 · X-ray Crystallography · Table S4; Figure S14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EtOH@1 crystallographic formula	C23H24Cu4TbI4N4O8	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 crystal system	Monoclinic	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 crystallographic measurement temperature	298(2) K	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 calculated density	2.668 g cm-3	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 elemental analysis carbon found	Found: C 19.58, H 1.87, N 4.01	—	—	Text Exact Reported	p006 / SI p.5 · Syntheses of the compounds
EtOH@1 R1 and wR2 for I > 2sigma(I)	0.0318, 0.0789	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 space group	P21/n	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 unit-cell parameters a,b,c,beta	15.3681(11), 8.1281(6), 28.608(2); beta 101.785(1)	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
EtOH@1 unit-cell volume	3498.2 A3	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4

Single-crystal X-ray diffraction on Bruker SMART APEX II CCD with Mo Kalpha radiation at 150 K.

X-ray diffraction and scattering

G@1 yellow crystals · Single Crystal

Theta-omega scan; direct-methods solution and full-matrix least-squares refinement in SHELXTL.

Temperature: 150
Geometry: single crystal
Context: Solvated precursor structure.
Measurement source: p006 / SI p.5 · X-ray Crystallography · Table S2; Figure S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
G@1 crystallographic formula	C69H71Cu12I12N14O23Tb3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 crystal system	Monoclinic	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 crystallographic measurement temperature	150(2) K	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 calculated density	2.644 g cm-3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 R1 and wR2 for I > 2sigma(I)	0.0216, 0.0436	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 space group	P21/c	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 unit-cell parameters a,b,c,beta	15.0740(7), 24.982(1), 29.613(1); beta 107.801(2)	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
G@1 unit-cell volume	10617.5 A3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2

Single-crystal X-ray diffraction on Bruker SMART APEX II CCD with Mo Kalpha radiation at 150 K.

X-ray diffraction and scattering

I2@1 iodine-loaded crystals · Single Crystal

Determined iodine positions, I2-framework contacts, I-...I2...I- geometry and conductive {Cu4I5}n layer motif.

Temperature: 150
Geometry: single crystal
Context: Guest-loaded iodine state.
Measurement source: p006-p007 / SI p.5-6 · X-ray Crystallography · Table S2; Figure S10-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
I...C contacts around I2 in channel B	3.97(1)-4.21(1) A	—	—	Text Range	p004 / article p.8412 · Main text · Figure S11b
I2@1 crystallographic formula	C42H38Cu8I14N8O14Tb2	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 crystal system	Monoclinic	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 crystallographic measurement temperature	150(2) K	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 calculated density	3.231 g cm-3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 R1 and wR2 for I > 2sigma(I)	0.0486, 0.1264	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 space group	P21/n	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 unit-cell parameters a,b,c,beta	15.318(2), 8.0546(13), 29.444(5); beta 99.920(2)	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2@1 unit-cell volume	3579 A3	—	—	SI Table Exact Reported	p009 / SI p.8 · Table S2/S4 · Table S2
I2 guest to framework iodide contact in channel AMarked as a best value within this paper	3.3417(3) A	—	0.0003 A	Text Exact Reported	p003 / article p.8411 · Main text · Figure 4; Figure S11
Short I5...O4 contact in I2@1 refinement alert	2.92 A	—	—	Text Rounded Reported	p006-p007 / SI p.5-6 · X-ray Crystallography
I7-I7 iodine molecule bond length in I2@1 refinement alert	2.75 A	—	—	Text Rounded Reported	p006-p007 / SI p.5-6 · X-ray Crystallography
Terminal iodide separation in linear I4(2-) arrangement	9.411(1) A	—	0.001 A	Text Exact Reported	p004 / article p.8412 · Main text · Figure 4

Single-crystal X-ray diffraction on Bruker SMART APEX II CCD with Mo Kalpha radiation at 298 K.

X-ray diffraction and scattering

MeCN@1 crystals · Single Crystal

Structure of MeCN@1 solvent-loaded control.

Temperature: 298
Geometry: single crystal
Context: Acetonitrile guest-loaded control.
Measurement source: p006 / SI p.5 · X-ray Crystallography · Table S4; Figure S14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
MeCN@1 crystallographic formula	C23H10Cu4TbI4N5O7	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 crystal system	Monoclinic	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 crystallographic measurement temperature	298(2) K	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 calculated density	2.672 g cm-3	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 elemental analysis carbon found	Found: C 19.65, H 1.71, N 4.94	—	—	Text Exact Reported	p006 / SI p.5 · Syntheses of the compounds
MeCN@1 R1 and wR2 for I > 2sigma(I)	0.0202, 0.0416	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 space group	P21/n	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 unit-cell parameters a,b,c,beta	15.4107(9), 8.0701(5), 28.593(2); beta 102.046(1)	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4
MeCN@1 unit-cell volume	3477.7 A3	—	—	SI Table Exact Reported	p011 / SI p.10 · Table S2/S4 · Table S4