The presence of mixed-valent silver in the uranyl phenylenediphosphonate framework

Article abstract of DOI:10.1039/d0nj00573h

In this work, a new 2D layered silver uranyl phosphonate compound Ag⁰_1.51[Ag^I₄(UO₂)₃(O₃PC₆H₄PO₃)(O₃PC₆H₄PO₃

Full text of DOI:10.1039/d0nj00573h

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DOI: 10.1039/D0NJ00573H
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The Presence of Allovalent Silver in the Uranyl
Phenylenediphosphonate Framework
Ru Bai,a,b, § Lanhua Chen,b, § Yugang Zhang,b Long Chen,b Juan Diwu,b and Xiao-Feng Wang*a
Received 00th January 20xx,
Accepted 00th January 20xx
In this work, a new 2D layered silver uranyl phosphonate compound, Ag02.7[AgI8(UO2)6(O3PC6H4PO3)2(O3PC6H4PO3H)4]
(denoted as compound 1) was synthesized by reaction of 1,2-phenylenediphosphonic acid (H4PDPA) with UO2(NO3)2·6H2O
and AgNO3 under the mild hydrothermal condition. The uranyl layered framework consists of two types of UO8 and UO7
coordination units simultaneously connected by two kinds of phenylenediphosphonate linkers. To our surprise, the
presence of both silver ions and metallic silver atoms in the free space between the layers is identified by the single crystal
X-ray diffraction, EDS, and XPS techniques. The ratio of Ag+ and Ag0 was estimated to be 2.81:1, based on the primary peak
area of Ag 3d5/2 from the XPS results, which corroborates with the ratio of 2.96:1 obtained from the XRD results. More
importantly, the incorporation of the allovalent silver sites results in the quenching of the fluorescent emission of the
uranyl phosphonate compound as evidenced by its single crystal fluorescence spectrum.
DOI: 10.1039/x0xx00000x
plane, yielding UO6 tetragonal, UO7 pentagonal, and UO8
hexagonal bipyramidal geometries, respectively.6-10
Introduction
Actinide phosphonate framework materials have attracted
widespread attention in the past few decades, not only due to
their adjustable structures and superior properties, but also
because that phosphonates play the important role to
separate uranium and plutonium in the PUREX process for the
recycling of spent nuclear fuel.1-5 Uranium is the most
abundant and prior actinide element, which adopts diverse
oxidation states and coordination topologies and geometries.
The uranium ion is predominantly present in the hexavalent
state by strongly binding with two oxo donors to form the
linear triatomic uranyl unit, UO22+. As a result, with both
vertical coordination positions occupied by terminal -yl oxo
groups, the uranyl unit further will be coordinated with four to
six O-donor atoms from the organic ligands in the equatorial
The phosphoric ligands can be easily prepared and readily
complexed with actinides; therefore, actinide phosphonates
have gradually developed into an important class of inorganic-
organic hybrids. For instance, uranium phosphonates exhibit
high thermal stability that originates from the extremely high
binding affinity of the -CPO3 moieties, and high structural
flexibility by virtue of the various selection of the organic
compartments. In addition, superior properties of uranyl
phosphonate hybrid materials have been demonstrated in
fields of proton conducting materials,11 ion exchangers,12
magnetism materials,13 and chiral materials.14 Up to date,
various structure types have been reported in uranyl
phosphonates including 1D chain15 and tubular, 2D layer,16,17
3D framework,2,18 as a consequence of the uranyl hydrolysis
and the uranyl complexation with phosphonic ligands through
the -CPO3 in basis η2 and/or η3 coordination modes.17 Multiple-
topic phosphonate ligands containing more than one -CPO3
groups and various derivatives have been designed and their
uranyl coordination chemistry has been investigated to
remarkably enrich the structures and topologies of uranyl
phosphonates. For example, by modifying the organic
skeleton,19-21 phenylphosphonate ligands were utilized to
construct different low-dimensional functional architectures.
a. School of Chemistry and Chemical Engineering, and Hunan Key Laboratory for the
Design and Application of Actinide Complexes, University of South China,
Hengyang, 421001, China. E-mail:xfwang518@sina.cn
b. State Key Laboratory of Radiation Medicine and Protection, School for
Radiological and Interdisciplinary Sciences (RAD-X), Collaborative Innovation
Center of Radiation Medicine of Jiangsu Higher Education Institutions and School
of Radiation Medicine and Protection, Soochow University, Suzhou 215123, China.
§These authors contributed equally.
Electronic Supplementary Information (ESI) available: X-ray crystallography, PXRD
and TGA curve, EDS analysis, XPS and fitting parameters. CCDC 1978046. For ESI
and crystallographic data in CIF or other electronic format see
DOI: 10.1039/x0xx00000x
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Correspondingly, in contrast to the alkyl-phosphonic ligands, Shanghai Lingfeng chemical reagent Co. Ltd and Alfa Aesar,
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DOI: 10.1039/D0NJ00573H
the aryl-phosphonic ligands are capable of creating
a
respectively.
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hydrophobic surface of the uranyl phosphonate hybrid
materials.
Single crystal X-ray diffraction was carried out on a Bruker D8-
Venture diffractometer with a Turbo X-ray Source (Mo–Kα
radiation, λ = 0.71073 Å) at room temperature. PXRD patterns
were recorded on a Bruker D8 Advance diffractometer for Cu
Kα radiation (λ = 1.54056 Å) in the 2θ range of 5° to 50°. FT-IR
spectra were obtained between 4000 and 400 cm-1 on a
Thermo Nicolet iS50 spectrometer. The thermogravimetric
analysis (TGA) was performed on a NETZSCH STA 449F3
instrument under a nitrogen flow. The single crystal solid-state
photoluminescence and UV-vis-NIR absorption spectra were
collected from a Craic Technology microspectrophotometer. X-
ray photoelectron spectroscopy (XPS) was adopted on a
Thermo Scientific ESCALAB 250 Xi spectrometer equipped with
a monochromatic Al-Kα X-ray source. The photoluminescence
spectra of compound 1 were collected with 365 nm excitation
light at room temperature.
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Furthermore, the incorporation of alkali and/or alkali earth
ions also plays an important role as structural directing agents
and charge-balancing counterions. In order to increase the
complexity of the architecture of actinide phosphonates, the
introduction of heterometal ions as counterions and
connecting nodes has attracted considerable attention.
Amongst, the f-d hetero-systems supported by 3d or 4d
transition metal ions (such as Co2+, Zn2+, Mn2+, Ag+) have been
usually developed, with the emphasis on promoting the
crystallization of uranyl complexes and on generating electron
transitions.22-25 Generally, the overlap between the emission
and absorption region of the f-d hybrid compounds may lead
to partial quenching of its luminescent emission. But the
special photoluminescent properties of the corresponding
uranyl complexes by the introduction of transition metal ions
and the internal and intrinsic mechanism have not been well
studied.26
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Preparation of 1, 2-phenylenediphosphonic acid ligand
(H4PDPA):
A mixture of 1,2-bis (dimethoxyphosphoryl)
Herein,
a
new
bimetallic
silver
and
uranyl
benzene (2 g) and excess amount of concentrated hydrochloric
acid was added into a 500 mL round-bottomed flask, heated
phenylenediphosphonate layered coordination compound,
Ag02.7[AgI8(UO2)6(O3PC6H4PO3)2(O3PC6H4PO3H)4] (compound 1),
was successfully synthesized under mild hydrothermal
condition. Single crystal X-ray diffraction analysis indicated the
o
and refluxed at 120 C for 72 h. Then the mixture was heated
and evaporated to dry to yield the bright white powder, which
was subsequently dried in a vacuum oven as the final product
of H4PDPA.27
1
contains both metallic Ag0 atoms and Ag+ cations
simultaneously, which were confirmed by energy disperse
spectroscopy (EDS) and X-ray photoelectron spectroscopy
(XPS). Its spectroscopic properties also were studied using
UV−vis−NIR absorption and fluorescence spectroscopy, and
fourier transform infrared spectroscopy (FT-IR).
Synthesis of compound 1: The mixture of H4PDPA (142.8 mg,
0.6 mmol), UO2(NO3)2·6H2O (150.0 mg, 0.3 mmol), AgNO3
(138.0 mg, 0.8 mmol), and ultra-pure water (2.0 mL) were
mixed in a 20 mL teflon-lined stainless steel autoclave, heated
to 220 oC for 3 days, and then cooled down to 30 oC at a rate of
15 oC /h. The products were washed with deionized water and
ethanol, and then dried at 60 oC in a vacuum oven. The
resulting blue crystalline solids compound 1 was obtained as
the pure phase which was confirmed by the PXRD of bulk
products according with the simulated one.
Experimental section
Attention! Uranium is a radioactive and chemically toxic
element, and uranium-containing samples must be properly
treated and protected.
All chemical reagents were purchased commercially and used
without further purification. AgNO3 and 1, 2-
bis(dimethoxyphosphoryl)benzene are purchased from
Results and discussion
Structure Description
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Figure 1. The representation of three uranyl coordinaton enviroments in compound 1.
1
Compound 1 crystalizes in the triclinic space group P (Table
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(Color mode: Ag, pink; C, black; P, sapphire; O, red. H atoms and part of the aromatic
DOI: 10.1039/D0NJ00573H
S1), and the asymmetric unit contains three independent
rings are omitted for clarity).
UO2 units, one full-deprotoned PDPA4- and two half-
2+
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deprotoned HPDPA3- ligands, 5.35 Ag0/AgI sites. As depicted in
Figure 1, both U1 and U2 are chelated by four oxygens from
two PDPA4-, and monodentated by one oxygen donor from the
monoprotonated -O3 moiety of the other HPDPA3-. The U1 is a
pentagonal bipyramidal coordination polyhedron with the
uranyl U=O bond distances of 1.758(4) and 1.775(4) Å,
respectively. The equatorial U-O bond distances range from
2.334(4) to 2.417(4) Å. The U2 adopts a similar pentagonal
bipyramidal coordination geometry as U1, where the U2=O
and U2−O bond lengths are in the range of 1.757(5) − 1.788(5)
Å and 2.196(14) − 2.418(4) Å, respectively. The BVS values of
U1 and U2 are calculated to be 6.08 and 6.08 v.u., respectively
(see Table S2).28,29
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The U3 is surrounded six O atoms to form tetragonal
bipyramid coordination environment which contains four
monodentate oxygens in equatorial plane from four -PO3
segments. Two U=O bond lengths are 1.770(5) and 1.800(5) Å,
while the four equatorial U-O bond distances are 2.251(5),
2.258(5), 2.260(4) and 2.27(5) Å, respectively. Additionally, the
results BVS value of U3 is 6.01 v.u. (Table S2). As shown in
Figure 2, U1 and U2 units are joined together by HPDPA3- and
PDPA4- ligands to form chains along the b-axis, which are
further linked by U3O6 units into a layers on [bc] plane. It is
interesting to note that the phenyl rings are all arranged on
one side of the uranyl phosphonate layer to form the
hydrophobic region, leaving the other side to be occupied by
hydrophilic terminal -yl oxo groups and phosphonate groups.
Figure 2. View of three-dimensional supramolecular structure with polyhedral uranyl of
compound 1 along a-axis (a) and the layered expansion diagram (b). Color code: yellow
polyhedron: U(1)O7 unit; green polyhedron: U(2)O7 unit; dark blue polyhedron: U(3)O6
unit ( light blue sphere: P; black sphere: C; red sphere: O. Ag+ and Ag0 are omitted for
clarity ).
The π-π interaction between the phenyl rings and the
hydrogen bonding interactions between the oxygen atoms
result in the ABAB type stacking of adjacent layers as shown in
Figure 2a.
X-ray Photoelectron Spectroscopy
X-ray Photoelectron Spectroscopy (XPS) is a widely adopted
technique to investigate the chemical compositions of the
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surface of materials, including the chemical valence of compound 1 under UV light excitation at 365 nm VaierweAsrhticolewOnnlinine
DOI: 10.1039/D0NJ00573H
different elements. In Figure S5, the peaks of C, O, P, Ag, and U Figure 4b.
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elements are all presented in the XPS survey spectra, where
the binding energies (BEs) of all peaks are adjusted according
to that of the C1s (284.8eV). As shown in Figure 3, the two
strong peaks in the Ag 3d narrow-scan XPS spectrum located at
368.97 and 375 eV could be observed, which correspond to Ag
3d5/2 and Ag 3d3/2 binding energies, respectively, strongly
support the presence of Ag element in compound 1. Then, this
spectrum was fitted with two Ag components of Ag+ and Ag0.
As the fitting parameters are given in Table S3, the BEs of Ag
3d5/2 peaks were at 368.59 and 369.15 eV, respectively; these
values are comparable with those reported in [Ag/Ag3PO4/GO
system] (368 eV), and [CN10UA] (369.5 eV), respectively.30,31
Meanwhile, the calculated molar ratio of Ag+ to Ag0 is 2.81:1,
Figure 3. Ag 3d XPS spectra of compound 1.
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based on the primary peak area of Ag 3d5/2
Taking the result of XPS into consideration, the formula of
compound is determined to be
.
The spectrum of the pristine H4PDPA ligand displays one
strong and broad emission peak between 410 and 600 nm,
which corresponds to the π-π* transition of the phenyl groups.
The spectrum of uranyl nitrate hexahydrate exhibits the classic
1
Ag02.7[AgI8(UO2)6(O3PC6H4PO3)2(O3PC6H4PO3H)4], where Ag+
cations compensate the negative charge of the uranyl layer. In
this formula, the ratio of Ag to U also corroborates with the
ratio obtained from the EDS (Figure S2) and the single crystal
XRD results. It is noteworthy that coordination compounds
containing Ag0 is exceeding rare. For example, to date, only
two MOF materials containing Ag0 have been reported, where
the Ag0 was proposed to originate from the reduction of the
Ag+ ion with the aid of the DMF solvent.32,33 In our previous
work, we have also noticed the thermal reduction of U(VI) to
U(IV) in solvothermal reactions without the presence of silver
ions.34 Therefore, we also speculate that the reduction of Ag+
occurred under the hydrothermal condition, affording the
allovalent silver uranyl phosphonate compound.
2+
fluorescence pattern of the UO2 unit that consists of several
strong emissions located at 486, 510, 530, 558, and 590 nm,
respectively. The typical uranyl emission arises from the
electronic and vibronic transitions S10 – S0v (v = 0−4) and S11-
S00 of the symmetrical and antisymmetric modes of the uranyl
centre.20,22,37 The emission spectra of uranyl phosphonate
compounds that contain Ag+ have been reported to exhibit the
typical uranyl emission patterns.38,39 In sharp contrast, the
emission of the U(VI) units in compound 1 was completely
quenched as shown in Figure 3b, probably owing to the
presence of the Ag0.
Spectroscopic Properties.
The FT-IR spectrum of compound 1 was further collected to
characterize its structural features as shown in Figure S3.
Peaks at 900-920 cm-1 are attributed to the asymmetric
stretching frequency νas(O=U=O), while those at the 820-840
cm-1 are ascribed to the symmetric stretching frequency
modes.19,40 The bands in the range of 1400~1565 cm-1 for
compound 1 are assigned to the stretch of the aromatic
rings.17 The characteristic antisymmetric and symmetric
stretch peaks of the P=O and P-O moieties are presented
The UV–vis-NIR spectrum of the compound 1 was collected at
room temperature, as shown in Figure 4a. The peak at ca. 278
nm is assigned to the axial U=O charge transfer, which is the
characteristic absorption peak of the uranyl unit. The peaks
ranging from 420 to 640 nm are ascribed to the ligand to metal
charge transfer (LMCT) between the O atoms from ligand and
empty orbitals from the uranyl units.35,36 The fluorescence
spectra of H4PDPA ligand, uranyl nitrate hexahydrate, and
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between 990-1257 cm-1, while the peaks from 750 to 775 cm-1
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Conflicts of interest
There are no conflicts to declare.
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DOI: 10.1039/D0NJ00573H
can be assigned to the P-C bonds.19,39 The peak located at 593
cm−1 is attributed to the Ag-O stretching vibrations according
to the literature report.41
Acknowledgements
9
This work is supported by the National Natural Science
Foundation of China (No.11375082, 51802147, 21906113 and
21806117) and a project funded by Jiangsu Provincial Key
Laboratory of Radiation Medicine and Protection.
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Figure 4. (a) UV-vis-NIR absorption spectrum and (b) luminescence spectra of
compound 1, H4PDPA ligand, and UO2(NO3)2·6H2O.
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Conclusion
In this work, a stable silver uranyl phenylenediphosphonate
coordination compound is synthesized, and structurally and
spectroscopically characterized. It is worth noting that our
results demonstrate the unique presence of the allovalent
silver in the uranyl phosphonate layered framework.
Specifically, it is the existence of Ag0 rather uranyl emission
that was observed in the luminescence spectrum. It is believed
that this result could shed some light on the design and
synthesis of novel allovalent silver uranyl coordination
compound.
18 W.-T. Yang, H.-Y. Wu, R. -X. Wang, Q. -J. Pan, Z. -M.
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DOI: 10.1039/D0NJ00573H
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A 2-D silver uranyl phosphonate present both Ag+ and Ag0 atoms in the free space between the adjacent layers and the
incorporation of the allovalent silver sites results in the quenching of the fluorescent emission.