Diffraction Structure — Efficient sequestration of radioactive 99TcO4- by a rare 3-fold interlocking cationic metal-organic framework: A combined batch experiments, pair distribution function, and crystallographic investigation

5 measurement groups · 78 results

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

PXRD after acid/base water stability exposure

X-ray diffraction and scattering

ZJU-X6 powder/material for batch sorption · Powder

ZJU-X6 exposed to HNO3/NaOH solutions from pH 3 to 11, stirred 12 h/overnight, washed with deionized water, filtered and dried; PXRD used to confirm stability.

Atmosphere: aqueous acid/base solutions
Context: pristine ZJU-X6 stability
Measurement source: 2 · 2.3. Hydrolytic stability measurements · Fig. S4a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
highest pH tested with retained PXRD	pH 11	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. S4a
lowest pH tested with retained PXRD	pH 3	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. S4a

X-ray pair distribution function (PDF)

X-ray diffraction and scattering

ZJU-X6-Re / ReO4-loaded ZJU-X6 · Single Crystal

Bruker D8 Discover diffractometer; 2D Eiger2R_500K detector at 280 mm; 1 mm borosilicate capillaries; Ag source lambda = 0.560871 A; Si powder calibration; processed with PDFgetX3.

Geometry: 1 mm borosilicate capillary
Context: ZJU-X6 compared before and after ReO4- sorption
Measurement source: 3,5-6 · 2.9. Pair distribution function (PDF) measurements; 3.7. Sorption mechanism · Fig. 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
PDF Ni-C distance before ReO4- sorption	3.04 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4b
PDF Ni-C distance before ReO4- sorption	4.27 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4b
PDF Ni-O distance before ReO4- sorption	2.09 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4b
PDF Ni-O distance after ReO4- sorption	1.97 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4c
PDF Re-Ni distance after ReO4- sorption	3.81 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4c
PDF Re-O distance after ReO4- sorption	1.67 A	—	—	Text Exact Reported	5 · 3.7. Sorption mechanism · Fig. 4c

Single-crystal X-ray diffraction

X-ray diffraction and scattering

ZJU-X6 yellow crystals · Single Crystal

Bruker D8-Venture diffractometer; Mo-Kalpha lambda = 0.71073 A and Ga-Kalpha lambda = 1.34139 A; CMOS detector; data collected at 100 K, 173 K and 296 K; SAINT/APEX3 and SHELXTL-2014 refinement.

Temperature: 100; 173; 296
Context: pristine ZJU-X6 structure
Measurement source: 2 · 2.2. Single crystal X-ray diffraction measurements · Fig. 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
one-dimensional channel size	11 A	—	—	Text Rounded Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. S2
average Ni-N bond distance	2.111 A	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. 1c
average Ni-O(water) bond distance	2.086 A	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. 1c
space group	R32	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Table S1
ZJU-X6 unit-cell a	16.1827 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 unit-cell b	16.1827 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 unit-cell c	59.037 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 CCDC number	2049644	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 data completeness	1.0	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 calculated density	0.9282	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 F(000)	3852.0	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 empirical formula	C54H36N4NiO2	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 formula weight	799.4	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 absorption coefficient Mu	0.36	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 Npar	231	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 Nref	5273	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 R(reflections)	0.1173(3757)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 goodness-of-fit S	1.411	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 crystallography temperature	100 K	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 theta(max)	25.095	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 unit-cell volume	13389.3 A3	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 wR2(reflections)	0.3528(5305)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6 Z	9	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
2D layer window long dimension	21.8 A	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. S2b
2D layer window short dimension	16.2 A	—	—	Text Exact Reported	3 · 3.1. Synthesis and structure of ZJU-X6 · Fig. S2b

Single-crystal X-ray diffraction of ReO4-loaded ZJU-X6

X-ray diffraction and scattering

ZJU-X6-Re / ReO4-loaded ZJU-X6 · Single Crystal

ZJU-X6-Re single crystals analysed by single-crystal X-ray diffraction; crystallographic data and refinement details are listed in SI Table S1.

Temperature: 173
Context: ReO4-loaded ZJU-X6 surrogate structure
Measurement source: S4 · 3. X-ray crystallography · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ZJU-X6-Re unit-cell a	16.326 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re unit-cell b	16.326 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re unit-cell c	58.546 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re CCDC number	2049649	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re data completeness	0.96	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re calculated density	1.4332	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re F(000)	5634	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re empirical formula	C54H32N4NiO8Re2	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re formula weight	1295.94	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re absorption coefficient Mu	7.007	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re Npar	314	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re Nref	5539	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re R(reflections)	0.0707(3249)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re goodness-of-fit S	0.933	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re crystallography temperature	173 K	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re theta(max)	55.03	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re unit-cell volume	13515 A3	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re wR2(reflections)	0.2045(5539)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Re Z	9	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1

Single-crystal X-ray diffraction of 99TcO4-incorporated ZJU-X6

X-ray diffraction and scattering

ZJU-X6-Tc / 99TcO4-loaded ZJU-X6 · Single Crystal

ZJU-X6-Tc single crystals obtained after immersion in 99TcO4- solution; single-crystal structure used to identify TcO4- binding mode and hydrogen bonding.

Context: 99TcO4-loaded ZJU-X6
Measurement source: 6-7 · 3.7. Sorption mechanism · Fig. 5c-d; Fig. S8-S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
crystal cavity size after 99TcO4- uptake	7.8 A	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. S8
crystal cavity size before 99TcO4- uptake	11 A	—	—	Text Rounded Reported	6 · 3.7. Sorption mechanism · Fig. S8
ZJU-X6-Tc unit-cell a	16.4582 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc unit-cell b	16.4582 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc unit-cell c	57.905 A	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc CCDC number	2050619	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc data completeness	1.0	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc calculated density	1.232	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc F(000)	5058	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc empirical formula	C54H32N4NiO8Tc2	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc formula weight	10075.9	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc absorption coefficient Mu	0.808	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc Npar	291	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc Nref	5180	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc R(reflections)	0.0666(2375)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc goodness-of-fit S	1.007	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc crystallography temperature	296 K	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc theta(max)	24.716	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc unit-cell volume	13583 A3	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc wR2(reflections)	0.1969(5180)	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
ZJU-X6-Tc Z	1	—	—	SI Table Exact Reported	S4 · 3. X-ray crystallography · Table S1
maximum C-H...O hydrogen-bond angle to 99TcO4-	163 degrees	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. 5d
minimum C-H...O hydrogen-bond angle to 99TcO4-	108 degrees	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. 5d
maximum C-H...O hydrogen-bond length to 99TcO4-	2.89 A	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. 5d
minimum C-H...O hydrogen-bond length to 99TcO4-	2.49 A	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. 5d
average Ni-O bond distance in ZJU-X6-Tc	2.06 A	—	—	Text Exact Reported	6 · 3.7. Sorption mechanism · Fig. 5c