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Abstract

Using a hydrothermal reaction, a novel 4f–5d isonicotinic acid complex {[Tb₂(IA)₆(H₂O)₄](Hg₃Cl₇)}_n(nHgCl₄)·nCl·4nH₃O (1, HIA = isonicotinic acid) was synthesized and it was characterized by single crystal X-ray diffraction technique. Compound 1 is characterized by a two-dimensional layer-like structure. The photoluminescence measurement using solid-state samples uncovered that it shows four emission peaks at 489, 546, 587, and 622 nm, of which the peak at 546 nm is the strongest. These peaks could be assigned to the ⁵D₄ → ⁷F₆, ⁵D₄ → ⁷F₅, ⁵D₄ → ⁷F₄, and ⁵D₄ → ⁷F₃ transitions of the Tb³⁺ ions, respectively. The energy transfer mechanism of the photoluminescence emission was described by means of the energy level scheme of the Tb³⁺ ions and the isonicotinic acid ligand. Compound 1 shows remarkable CIE (Commission Internationale de I’Éclairage) chromaticity coordinates of (0.3633, 0.5038) in the yellowish green region. Compound 1 possesses a wide semiconductor band gap of 2.97 eV, as unveiled by the solid-state UV-Vis diffuse reflectance experiment.

Keywords

CIE mercury photoluminescence semiconductor terbium

A novel 4f–5d compound was reported. It shows yellowish green emission with CIE chromaticity coordinates of (0.3633, 0.5038). It possesses a wide optical band gap of 2.97 eV.

Introduction

It is well-known that most of lanthanide ions (except for La and Lu) are photoluminescent and, nowadays, lanthanide compounds with photoluminescence performance have received more and more attention.^1–5 Up to date, a lot of researchers have devoted themselves into the design, preparation, and characterization of novel lanthanide compounds, for the sake of investigating the useful applications of the lanthanide compounds in the areas of electrochemical displays, light-emitting diodes, luminescent probes, and so on.^6,7 In comparison with the large number of investigations on the photoluminescence performance of the lanthanide compounds, the exploration on the semiconductor performance of the lanthanide compounds is seldom yet and, therefore, it still needs to be investigated.⁸

Mercury is an interesting element and it has also drawn lots of attention in recent years due to the following reasons: different coordination geometries of mercury ions, photoelectric performance, semiconductor behaviors, photoluminescence properties, and so on.^9,10 These years we have kept focusing on the investigation of the compounds possessing photoluminescence and semiconductor properties, especially, the lanthanide mercury compounds, in order to obtain new findings on their crystal structures, photoluminescence, and semiconductor performance. In this work, we report the preparation, crystal structure, photoluminescence, energy transfer mechanism, and semiconductor property of a novel terbium–mercury complex {[Tb₂(IA)₆(H₂O)₄](Hg₃Cl₇)}_n(nHgCl₄)·nCl·4nH₃O (1, HIA = isonicotinic acid) with a two-dimensional (2D) layer-like structure.

Results and discussion

The molecular structure of complex 1 is presented in Figure 1. All crystallographically independent atoms are located on the general sites. The molecular structure of complex 1 consists of one {[Tb₂(IA)₆(H₂O)₄](Hg₃Cl₇)}_n^n– anionic 2D layer, one isolated (HgCl₄)^2– anion, one isolated Cl⁻ anion, and four lattice water molecules. There are four crystallographically independent mercury ions and they show different coordination geometries. Hg₁ is coordinated by two terminal chloride ions and two μ₂-bridging chloride ions to give a distorted tetrahedron. Hg₂ is bound by three μ₂-bridging chloride ions and two nitrogen atoms of two isonicotinic acid ligands to yield a distorted square pyramid. The bottom plane of the square pyramid is formed by Cl₃, N₆, Cl₅, and N₁(–0.5 + x, 4 – y, z), while the apex is Cl₄. Hg₃ is coordinated by two terminal chloride ions and one μ₂-bridging chloride ion to form a triangle. Hg₄ is surrounded by four terminal chloride ions to give an isolated and distorted (HgCl₄)^2– tetrahedron. Hg₁ tetrahedron edge shares with Hg₂ square pyramid and the latter corner shares with Hg₃ triangle and, in this way, they form a Hg₃Cl₇ moiety. The Hg–Cl bond lengths are in the range of 2.351(2)–2.886(4) Å, which is normal and comparable with those documented previously.^11–13 The Hg–N bond lengths are 2.110(8) and 2.20(1) Å, which is also normal and comparable with those reported previously.^14–16 The Cl–Hg–Cl bond angles are in the range of 89.29(9)°–165.8(1)°, while the N–Hg–Cl bond angles are in the range of 82.9(3)°–108.0(3)°. The N₁(–0.5 + x, 4 – y, z)–Hg₂–N₆ bond angle is 163.9(4)° which is close to linear.

Figure 1.

Molecular structure of 1 with the lattice water molecules, hydrogen atoms, and isolated chloride ions being omitted for clarity. Symmetry codes: (1) –½ + x, 4 – y, z; (2) x, –1 + y, z; (3) x, 1 + y, z.

There are two crystallographically independent Tb³⁺ ions, and both of them have an eight-coordination environment, coordinated by two oxygen atoms of two coordination water molecules and six oxygen atoms of six isonicotinic acid molecules to form a slightly contorted square anti-prismatic geometry. The bond lengths of Tb–O_water are in the range of 2.442(6)–2.515(7) Å, while those of Tb–O_{isonicotinic acid} are in the range of 2.287(7)–2.427(6) Å. The bond lengths of Tb–O_water are obviously longer than those of Tb–O_{isonicotinic acid}, indicating that terbium ions show weaker affinity to water molecules than to isonicotinic acid ligands. These Tb–O bond lengths are in the normal range and comparable with those found in the literature.^17–20 The O–Tb–O bond angles locate in a very wide range of 69.0(2)°–145.6(2)°. The neighboring Tb³⁺ ions are interlinked by the isonicotinic acid molecules with the number of the isonicotinic acid molecules being of -2-4-2-4- to yield a one-dimensional (1D) infinite chain running along the b direction, as shown in Figure 2. The distances between the neighboring Tb³⁺ ions are 4.3638(1) and 5.1336(2) Å. The 1D infinite chains are interconnected by the Hg₂ atom of the Hg₃Cl₇ moiety to yield a 2D layer extending along the ab plane, as presented in Figure 3. The electro-static interaction and van der Waals interaction among the {[Tb₂(IA)₆(H₂O)₄](Hg₃Cl₇)}_n^n– anionic 2D layers, isolated (HgCl₄)^2– anions, isolated Cl⁻ anions, and lattice water molecules solidify the crystal packing structure of complex 1, as shown in Figure 4.

Figure 2.

The 1D chain running along the b axis. Pink: TbO₈ polyhedra.

Figure 3.

The 2D layer in 1. Pink: TbO₈ polyhedra.

Figure 4.

The packing diagram of 1. Pink: TbO₈ polyhedra.

The photoluminescence spectrum for compound 1 in this work was carried out in the solid state under room temperature. Figure 5 gives the result of the photoluminescence measurement. Upon excited by the wavelength of 375 nm, the photoluminescence spectrum of 1 displays four emission peaks at 489, 546, 587, and 622 nm, of which the peak at 546 nm is the strongest. The photoluminescence emission peaks of compound 1 reveal that it possesses remarkable CIE (Commission Internationale de I’Éclairage) chromaticity coordinates of (0.3633, 0.5038) in the yellowish green region, as given in Figure 6. Therefore, this compound is a potential candidate for yellowish green light emission materials. These emission peaks of compound 1 can be attributed to the characteristic emissions of the 4f electrons intrashell transitions of the Tb³⁺ ions. More concretely, the photoluminescence emission peaks at 489, 546, 587, and 622 nm could be originated from the ⁵D₄ → ⁷F₆, ⁵D₄ → ⁷F₅, ⁵D₄ → ⁷F₄, and ⁵D₄ → ⁷F₃ transitions of the Tb³⁺ ions.²¹

Figure 5.

The solid-state photoluminescence emission spectrum of 1.

Figure 6.

The CIE chromaticity diagram and chromaticity coordinate of the photoluminescence emission spectrum of 1.

For the sake of unveiling the nature of the photoluminescence spectrum of compound 1, the phosphorescence spectra of the isonicotinic acid were measured at 77 K, as shown in Figure 7. From the figure, the onset of the emission diagram of the isonicotinic acid can be determined as around 434 nm. So, the lowest triplet state energy of the isonicotinic acid could be about 23,041 cm⁻¹. The energy difference between the lowest triplet state of the isonicotinic acid and the resonant energy level of the Tb³⁺ ions (⁵D₄, 20,500 cm⁻¹) is 2541 cm⁻¹ in 1 (Figure 8). Based on the intramolecular energy transfer theory found by Dexter and Sato,^22,23 the intramolecular energy transfer efficiency mainly depends on two factors. One is the energy transfer from the lowest triplet state energy level of the ligand to the resonant state energy level of the lanthanide ion through Dexter’s resonant exchange process. The other is the reverse energy transfer process from the lanthanide ion to the ligand through a thermal deactivation process. The reverse energy transfer process maybe happen easier if the energy difference is too small. Both the energy transfer processes are obviously contrary, despite both of them depending on the energy gap between the ligand’s lowest triplet state energy level and the lanthanide ion’s resonant state energy level. An ideal energy gap maybe around 3000 ± 500 cm⁻¹, as pointed out by the intramolecular energy transfer theory.²⁴ The photoluminescence performance of a compound could probably be weakened by a smaller or a larger energy gap.

Figure 7.

Phosphorescence spectrum of isonicotinic acid measured at 77 K.

Figure 8.

A schematic and partial energy level diagram of the main energy absorption transfer and phosphorescence processes in compound 1 and the isonicotinic acid ligand.

As mentioned previously, the energy gap between the isonicotinic acid’s lowest triplet state energy level and the Tb³⁺ ion’s resonant state energy level is 2541 cm⁻¹ in the title compound. The 2541 cm⁻¹ locates in the range of 3000 ± 500 cm⁻¹. Therefore, this compound is expected to exhibit good photoluminescence performance. This conclusion is in good line with the photoluminescence emission curve of compound 1, as presented in Figure 5. As shown in Figure 5, the four photoluminescence emission peaks are well separated. As a result, the isonicotinic acid is a suitable ligand for exciting the Tb³⁺ ions in compound 1, that is, it is a fine “antenna.”

Compound 1 is a mercury-containing compound and, to our knowledge, several mercury-containing compounds have been used as famous semiconductor materials, for example, the Hg_xCd_1−xTe (MCT) is a very important infrared (IR) detector in military domain. Therefore, we deem that the title compound could show semiconductor behavior. The solid-state UV-Vis diffuse reflectance spectrum of compound 1 was carried out with powder sample at room temperature. The data of the diffuse reflectance spectrum were treated using Kubelka–Munk function, namely, α/S = (1 − R)²/2R. With regard to this function, α means the absorption coefficient, S is the scattering coefficient, and R refers to the reflectance. The semiconductor band gap of compound 1 can be determined by extrapolating from the linear part of the absorption edges from the α/S versus energy curve, as given in Figure 9. As for compound 1, its solid-state UV-Vis diffuse reflectance spectrum reveals that it possesses a wide semiconductor band gap of 2.97 eV. So, this compound could probably be a candidate for the wide semiconductor band gap materials. Moreover, the solid-state UV-Vis diffuse reflectance spectrum of 1 displays a slow slope of the optical absorption edge, which suggests an indirect transition process.²⁵

Figure 9.

Solid-state diffuse reflectance spectrum of 1.

The thermal stability measurement of compound 1 was measured under nitrogen atmosphere and the result is presented in Figure 10. With regard to compound 1, the onset temperature of the decomposition is about 50°C. The thermogravimetric (TG) curve shows a three-stage decomposition process. The first decomposition stage locates in the temperature range of 40°C–146.6°C. The mass loss at this stage is 4.06%, which is close to the calculated value of 3.13% for the loss of four H₃O moieties. The second decomposition stage starts from 146.6°C and ends at 294.9°C. The mass loss at the second stage is 53.60%, which is very close to the calculated value of 53.59% for the loss of one isolated (HgCl₄)^2– anion, one isolated Cl⁻ anion, one Hg₃Cl₇ moiety, and four coordinating water molecules. The third decomposition stage happens in the temperature range of 294.9°C–600°C. The mass loss at the third stage is 30.86%, which is close to the calculated value of 30.17% for the loss of six isonicotinic acid ligands.

Figure 10.

TG curve of 1.

Conclusion

In summary, a novel terbium–mercury isonicotinic acid complex {[Tb₂(IA)₆(H₂O)₄](Hg₃Cl₇)}_n(nHgCl₄)·nCl·4nH₃O was synthesized and characterized. It is characterized by a 2D layer-like structure. The solid-state photoluminescence measurement revealed that it shows four emission peaks at 489, 546, 587, and 622 nm, which could be assigned to the ⁵D₄ → ⁷F₆, ⁵D₄ → ⁷F₅, ⁵D₄ → ⁷F₄, and ⁵D₄ → ⁷F₃ transitions of the Tb³⁺ ions, respectively. The energy transfer mechanism was described by virtue of the energy level scheme of the Tb³⁺ ions and the isonicotinic acid ligand. This compound possesses remarkable CIE chromaticity coordinates of (0.3633, 0.5038) in the yellowish green region. So, it is a potential yellowish green photoluminescence material. It possesses a wide optical band gap of 2.97 eV, suggesting that it is probably a wide gap semiconductor compound.

Experimental

Materials and instrumentation

The chemicals and reagents are A.R. grade, purchased and directly used for the preparation of the title complex. IR was carried out with a KBr pellet on a Thermo Scientific Nicolet iS10 spectrometer. Solid-state photoluminescence measurement was measured on a F97XP photoluminescence spectrometer. Solid-state diffuse reflectance UV-Vis spectrum was conducted at room temperature on a computer-controlled TU1901 UV-Vis spectrometer equipped with an integrating sphere in the wavelength span of 190–1100 nm. BaSO₄ powder was applied as a reference (100% reflectance), on which the finely ground powder sample was coated. TG measurement was carried out on a NETZSCH TG 209F3 analyzer in nitrogen atmosphere.

Synthesis of compound 1

TbCl₃·6H₂O (1 mmol, 374 mg), HgCl₂ (3 mmol, 813 mg), isonicotinic acid (3 mmol, 369 mg), and 10 mL distilled water were mixed into a 25-mL Teflon-lined stainless steel vessel. The vessel was heated to 433 K and held there for 7 days. Once the vessel was slowly cooled down to room temperature, colorless crystals were obtained. The yield was 37% based on TbCl₃·6H₂O. IR peaks (cm⁻¹): 3431(vs), 3068(w), 1594(vs), 1558(w), 1421(s), 1386(vs), 1248(w), 1058(w), 855(w), 759(m), 681(m), 547(w), and 413(w).

X-ray structure determination

A single crystal was adhered on the tip of a glass fiber and mounted to a SuperNova CCD diffractometer with X-ray source being graphite monochromated Mo–Kα radiation. The crystal dataset was obtained with ω scan mode. CrystalClear software²⁶ was used for data reduction and the empirical absorption correction. Crystal structure was solved with direct method and the final structure was refined on F² with full-matrix least-squares by virtue of Siemens SHELXTL^TM V5 crystallographic software.²⁷ All non-hydrogen atoms were found based on difference Fourier maps and refined anisotropically. Crystal data as well as the details of data collection and refinement are presented in Table 1, and selected bond lengths and bond angles are shown in Table 2. Crystallographic data for the structural analysis have been deposited with the Cambridge Crystallographic Data Centre, CCDC No. 1885107. Copies of this information may be obtained free of charge from the Director, CCDC, Cambridge, UK (email: deposit@ccdc.cam.ac.uk or https://www.ccdc.cam.ac.uk).

Table 1.

Crystallographic data and structural analysis.

Formula	C₃₆H₄₄Cl₁₂Hg₄N₆O₂₀Tb₂
Mr	2426.37
Color	Colorless
Crystal size (mm³)	0.13, 0.02, 0.02
Crystal system	Orthorhombic
Space group	Pca2₁
a (Å)	33.5623(7)
b (Å)	9.4708(3)
c (Å)	19.5130(6)
V (Å³)	6202.4(3)
Z	4
2θ_max (°)	50
Reflections collected	16,761
Independent, observed reflections (R_int)	7725, 5782 (0.0509)
d_calcd. (g/cm³)	2.598
μ (mm⁻¹)	12.701
F(000)	4464
T (K)	293(2)
R₁, wR₂	0.0689, 0.1472
S	1.038
Largest and mean Δ/σ	0.002, 0
Δρ (max, min) (e/Å³)	1.799, –2.243

Table 2.

Selected bond lengths (Å) and bond angles (°).

Bond lengths (Å)		Bond angles (°)
Hg(1)–Cl(1)	2.351(2)	Cl(1)–Hg(1)–Cl(2)	153.85(9)
Hg(1)–Cl(2)	2.354(2)	Cl(1)–Hg(1)–Cl(4)	99.36(9)
Hg(1)–Cl(3)	2.831(3)	Cl(2)–Hg(1)–Cl(4)	101.50(9)
Hg(1)–Cl(4)	2.776(3)	Cl(1)–Hg(1)–Cl(3)	100.12(8)
Hg(2)–Cl(3)	2.588(3)	Cl(2)–Hg(1)–Cl(3)	95.75(9)
Hg(2)–Cl(4)	2.705(4)	Cl(4)–Hg(1)–Cl(3)	89.29(9)
Hg(2)–Cl(5)	2.886(4)	N(1)#1–Hg(2)–N(6)	163.9(4)
Hg(2)–N(1)#1	2.110(8)	N(1)#1–Hg(2)–Cl(3)	101.6(3)
Hg(2)–N(6)	2.20(1)	N(6)–Hg(2)–Cl(3)	85.5(3)
Hg(3)–Cl(5)	2.450(4)	N(1)#1–Hg(2)–Cl(4)	85.8(3)
Hg(3)–Cl(6)	2.491(2)	N(6)–Hg(2)–Cl(4)	108.0(3)
Hg(3)–Cl(7)	2.678(3)	Cl(3)–Hg(2)–Cl(4)	96.2(1)
Hg(4)–Cl(8)	2.618(2)	N(1)#1–Hg(2)–Cl(5)	87.8(3)
Hg(4)–Cl(9)	2.776(3)	N(6)–Hg(2)–Cl(5)	82.9(3)
Hg(4)–Cl(10)	2.493(3)	Cl(3)–Hg(2)–Cl(5)	165.8(1)
Hg(4)–Cl(11)	2.437(3)	Cl(4)–Hg(2)–Cl(5)	95.1(1)
Tb(1)–O(2)	2.309(5)	Cl(5)–Hg(3)–Cl(6)	113.6(1)
Tb(1)–O(3)	2.384(6)	Cl(5)–Hg(3)–Cl(7)	113.5(1)
Tb(1)–O(5)	2.407(5)	Cl(6)–Hg(3)–Cl(7)	132.3(1)
Tb(1)–O(7)	2.353(7)	Cl(11)–Hg(4)–Cl(10)	104.9(1)
Tb(1)–O(9)	2.325(6)	Cl(11)–Hg(4)–Cl(8)	120.49(8)
Tb(1)–O(12)	2.360(5)	Cl(10)–Hg(4)–Cl(8)	129.59(9)
Tb(1)–O(1W)	2.442(6)	Cl(11)–Hg(4)–Cl(9)	94.7(1)
Tb(1)–O(2W)	2.455(7)	Cl(10)–Hg(4)–Cl(9)	92.0(1)
Tb(2)–O(1)#2	2.360(5)	Cl(8)–Hg(4)–Cl(9)	104.14(6)
Tb(2)–O(4)	2.287(7)	O(2)–Tb(1)–O(9)	142.1(2)
Tb(2)–O(6)	2.350(6)	O(12)–Tb(1)–O(5)	145.6(2)
Tb(2)–O(8)	2.427(6)	O(3)–Tb(1)–O(5)	72.3(2)
Tb(2)–O(10)	2.390(6)	O(2)–Tb(1)–O(1W)	73.9(2)
Tb(2)–O(11)#3	2.304(6)	O(2)–Tb(1)–O(2W)	69.3(2)
Tb(2)–O(3W)	2.452(6)	O(5)–Tb(1)–O(2W)	135.0(2)
Tb(2)–O(4W)	2.515(7)	O(8)–Tb(2)–O(4W)	69.0(2)

Symmetry codes: (1) –½ + x, 4 – y, z; (2) x, –1 + y, z; (3) x, 1 + y, z.

Supplemental Material

checkcif – Supplemental material for A novel terbium–mercury compound: Preparation, structure, and properties

Supplemental material, checkcif for A novel terbium–mercury compound: Preparation, structure, and properties by Wen-Tong Chen in Journal of Chemical Research

Supplemental Material

compound_1 – Supplemental material for A novel terbium–mercury compound: Preparation, structure, and properties

Supplemental material, compound_1 for A novel terbium–mercury compound: Preparation, structure, and properties by Wen-Tong Chen in Journal of Chemical Research

Footnotes

Declaration of conflicting interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This work was supported by the NSF of China (no. 21361013), Jiangxi Provincial Department of Education’s Item of Science and Technology (no. GJJ170637), and the open foundation of the State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences (no. 20180008).

ORCID iD

Wen-Tong Chen

Supplemental material

Supplemental material for this article is available online.

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Supplementary Material

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A novel terbium–mercury compound: Preparation,structure,and properties

Abstract

Keywords

Introduction

Results and discussion

Conclusion

Experimental

Materials and instrumentation

Synthesis of compound 1

X-ray structure determination

Supplemental Material

checkcif – Supplemental material for A novel terbium–mercury compound: Preparation, structure, and properties

Supplemental Material

compound_1 – Supplemental material for A novel terbium–mercury compound: Preparation, structure, and properties

Footnotes

Declaration of conflicting interests

Funding

ORCID iD

Supplemental material

References

Supplementary Material