Diffraction Structure — Synthesis and structure of anhydrous Zn2EDTA metal-organic framework

4 measurement groups · 36 results

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

checkCIF/PLATON validation of supplied structure factors

single crystal of Zn2EDTA picked from powder sample · Single Crystal

checkCIF/PLATON report for datablock zn2edta; PLATON version 06/07/2023, check.def 30/06/2023; wavelength 0.71073 A; temperature 110 K.

Temperature: 110
Context: pristine anhydrous framework single-crystal structure
Measurement source: p001-p002 · checkCIF/PLATON report · Alert summary

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
checkCIF alert level A count	0 ALERT level A	—	—	SI Table Exact Reported	p002 · checkCIF/PLATON report · Alert summary
checkCIF alert level G count	7 ALERT level G	—	—	SI Table Exact Reported	p002 · checkCIF/PLATON report · Alert summary
checkCIF polymeric structure maximum dimension	maximum dimension 3	—	—	SI Table Exact Reported	p002 · checkCIF/PLATON report · Alert summary
checkCIF data completeness	1.000	1 fraction	—	SI Table Exact Reported	p001 · checkCIF/PLATON report · Datablock summary

Powder X-ray diffraction with Rietveld phase quantification

X-ray diffraction and scattering

pH-dependent Zn-EDTA hydrothermal powder series · Powder

Samples synthesised at pH 2.5-3.4 with Zn:EDTA 2:1; MiniFlex Benchtop Rigaku XRD with Cu source, lambda Kalpha1 = 1.54056 A and Kalpha2 = 1.54439 A; Rietveld with TOPAS.

Context: pH-dependent phase formation series
Measurement source: p002-p003 / journal pages 2-3 · Experimental; Results and discussions · Fig. 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Optimal Zn:EDTA stoichiometric ratioMarked as a best value within this paper	2:1	—	—	Text Exact Reported	p003 / journal page 3 · Results and discussions
Phase at pH 2.5	Zn2(EDTA)H2O phase observed; Zn2EDTA fraction not reported and effectively absent	—	—	Text Approximate	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 2.6	2.3%	0.023 fraction	—	Text Rounded Reported	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 2.7Marked as a best value within this paper	pure Zn2EDTA phase	1 fraction	—	Text Approximate	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 2.8	65% Zn2EDTA and 35% Zn2EDTA(H2O)	0.65 fraction	—	Text Rounded Reported	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 2.9	31%	0.31 fraction	—	Text Rounded Reported	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 3.0	1.71%	0.0171 fraction	—	Text Exact Reported	p003 / journal page 3 · Results and discussions · Fig. 1
Zn2EDTA fraction at pH 3.4	Zn2EDTA phase completely vanished	0 fraction	—	Text Approximate	p003 / journal page 3 · Results and discussions · Fig. 1

Powder X-ray diffraction Rietveld refinement using SCXRD structural model

X-ray diffraction and scattering

pure anhydrous Zn2EDTA powder synthesised at pH 2.7 · Powder

PXRD data collected with Cu X-ray tube; Fig. 3 gives observed, calculated and difference plot with Rwp, Rexp and GOF.

Context: pristine anhydrous framework powder
Measurement source: p004-p005 / journal pages 4-5 · Results and discussions · Fig. 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
PXRD-refined unit-cell a	12.9652(4) A	—	(4)	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
PXRD-refined unit-cell b	7.0637(3) A	—	(3)	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
PXRD-refined beta angle	94.760(2) deg	—	(2)	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
PXRD-refined unit-cell c	14.1652(7) A	—	(7)	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
PXRD-refined cell volume	1292.82(9) A3	—	(9)	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
Rietveld goodness of fit	GOF = 3.16	—	—	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
Rietveld expected R factor	Rexp = 2.77%	0.0277 fraction	—	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3
Rietveld Rwp	Rwp = 8.75%	0.0875 fraction	—	Visual Estimate Rounded Reported	p005 / journal page 5 · Results and discussions · Fig. 3

Single-crystal X-ray diffraction; Bruker D8 QUEST; Mo-target X-ray tube; Olex2/ShelXT/ShelXL refinement

X-ray diffraction and scattering

single crystal of Zn2EDTA picked from powder sample · Single Crystal

PHOTONII detector, Mo radiation; main text gives lambda = 0.73071 A but Table 1/CIF give MoKalpha lambda = 0.71073 A; crystal kept at 110.15 K; numerical absorption correction used for final solution.

Temperature: 110.15
Atmosphere: liquid nitrogen cryostream
Context: pristine anhydrous framework
Measurement source: p002-p003 / journal pages 2-3 · Experimental; Results and discussions · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ZnO6 bond-length range	1.981-2.311 A	—	—	Text Range	p004 / journal page 4 · Results and discussions · Table 4
CIF chemical formula sum	C5 H6 N O4 Zn	—	—	SI Table Exact Reported	text CIF · data_zn2edta · _chemical_formula_sum
CIF independent reflections used in refinement	1710	—	—	SI Table Exact Reported	text CIF · data_zn2edta · _refine_ls_number_reflns
CIF diffraction radiation wavelength	0.71073 A	—	—	SI Table Exact Reported	text CIF · data_zn2edta · _diffrn_radiation_wavelength
CIF reflections collected	6049	—	—	SI Table Exact Reported	text CIF · data_zn2edta · _diffrn_reflns_number
SCXRD unit-cell a	12.945(10) A	—	(10)	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
SCXRD unit-cell b	7.063(2) A	—	(2)	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
SCXRD beta angle	94.92(3) deg	—	(3)	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
SCXRD unit-cell c	14.142(10) A	—	(10)	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
Calculated density	2.160 g/cm3	—	—	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
Solvent-water inclusion	No vacancies or inclusion of solvent water found	—	—	Text Qualitative	p003-p004 / journal pages 3-4 · Results and discussions
Final R1 index for I >= 2 sigma(I)	R1 = 0.0351	—	—	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
Space group	C2/c	—	—	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
SCXRD unit-cell volume	1288.3(14) A3	—	(14)	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
Z	8	—	—	Table Exact Reported	p003 / journal page 3 · Results and discussions · Table 1
Framework connectivity and channels	Each EDTA molecule links four chains, forming a 3D network of channels suitable for interstitial ionic mobility	—	—	Text Qualitative	p004 / journal page 4 · Results and discussions · Fig. 2