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Syntheses, crystal structures, and characterizations of two new Zn(ii)/Ni(ii) coordination polymers constructed by N-donor ligands and sulfate-bridge

  • Huilin Wang , Sai Li , Hua Zhang , Beihao Su and Xiuyan Wang EMAIL logo
Published/Copyright: February 26, 2025
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Main Group Metal Chemistry
From the journal Main Group Metal Chemistry Volume 48 Issue 1

Abstract

Two new coordination polymers, {(NH2(CH3)2)2[Zn2(bipy)(SO4)3]} n (1) and [Ni(phen)(SO4)(H2O)2] n (2) (bipy = 4,4′-bipyridine, phen = 1,10-phenanthroline) have been synthesized by using metal sulfate, nitrogen-containing ligands, and different template agents under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction. 1 exhibits binuclear units and SO4 2− connect two Zn(ii) ions’ centers. It shows 2D layer structure and further extends into 3D supramolecular framework by N–H⋯S hydrogen bonds. Moreover, 2 possesses a 1D double-chain structure and form 2D layer by hydrogen-bonding interactions. And we further explored the infrared (IR) of 1 and 2 and luminescent properties of 1.

Graphical abstract

Keywords: coordination polymer; Zn(ii); Ni(ii); sulfate-bridge; luminescent properties

1 Introduction

Coordination polymers (CPs) are synthesized by metal ions or metal clusters connected by organic/inorganic linkers [1,2], which have attracted considerable interest during the past few decades [3], not only because they combine the advantages of inorganic and organic materials [4,5] but also their fascinating aesthetical architecture structures and their potential applications in the field of catalysis [6,7], batteries [8], gas storage and separation [9,10], chemical sensing [11], magnetism, and so on [12]. As a family special class of crystalline materials [13,14], CPs can be constructed through two types of interactions: coordinate covalent bonds and weak interactions, such as π–π stacking interaction and hydrogen bond [15,16,17]. CPs can extend into 1D, 2D, or 3D structures through several of the interactions described above [18]. However, it is still of difficulty to predict the architectures of final material of CPs [19]. Structural indeterminacy results from many subtle conditions related to the crystallization process, such as organic ligands, metal ions, pH, solvent system, temperature, and so on [20]. Therefore, through reasonable selection and modification of metal ions and organic ligands, it is expected to obtain CPs with target structures and properties [21,22]. In this situation, d10 metal ions have been frequently used because of their close-shell configuration, e.g., Zn and Cd [23]. Sulfate is also a very interesting anion for the architecture of hydrogen bond networks because it easily forms strong hydrogen bonds [24]. Owing to their prominent binding ability, containing nitrogen ligands are important linkers in the process of synthesizing CPs, such as 4,4′-bipy and 1,10-phen are privileged as they produce aromatic π–π stacking interaction that gives stability to supramolecular assembly [25].

Herein, we report two novel CPs based on 4,4′-bipy or 1,10-phen ligands under solvothermal conditions, which are named {(NH2(CH3)2)2[Zn2(bipy)(SO4)3]} n (1) and [Ni(phen)(SO4)(H2O)2] n (2), meanwhile 3-carboxy-1-carboxymethyl-2-oxidopyridinium or 3-(carboxymethoxy)-2-naphthoic acid serves as a formulating agent in the reaction but they do not coordinate with the metal ions. Their syntheses, structural characterizations, and characterizations are explored in details below.

2 Results and discussion

2.1 Structural analysis

1 crystallizes in the triclinic crystal system with P 1 ̅ space group. Single crystal X ray analysis indicates that the asymmetric unit contains two Zn(ii) ions, one 4,4′-bipy ligand, three SO4 2− anions, and two free dimethylamine cation from decomposed N,N-dimethylformamide (DMF). As shown in Figure 1, 1 exhibits binuclear units and two Zn(ii) atoms exhibit the same coordination geometries, each Zn ion is four-coordinated by N atoms from 4,4′-bipy ligand and three O atoms from three sulfate anions, exhibiting the [ZnNO3] distorted tetrahedral. The Zn–N bond lengths [N(1)-Zn(2) and N(2)-Zn(1)ⅰ] are 2.0290(18) Å and 2.0408(18) Å, while the distances of Zn–O fall in the range from 1.9307(19) Å to 1.9599(18) Å.

Figure 1 Coordination environment of the Zn(ii) ion of 1 (symmetry codes: ⅲ x, y, z + 1, ⅳ x − 1, y, z).
Figure 1

Coordination environment of the Zn(ii) ion of 1 (symmetry codes: ⅲ x, y, z + 1, ⅳ x − 1, y, z).

Two SO4 2− connect two Zn(ii) ions to generate [Zn2(SO4)2] bimetallic ring construction (Zn1⋯Zn2 = 4.425 Å). Adjacent [Zn2(SO4)2] bimetallic rings are further linked via the third SO4 2− generating a 1D chain with the Zn2⋯Zn1 distance of 5.618 Å (Figure 2). In Figure 2, the 4,4′-bipy ligands connect adjacent 1D chains to yield a 2D layer (Zn1⋯Zn2 = 11.080 Å) and dimethylamine cation located on both sides of the 1D chain. Moreover, the 2D layer are further extended into a 3D supramolecular structure by N–H⋯S (N(3)-H(3B)⋯S(2) and N(4)-H(4B)⋯S(3)) hydrogen bonds interactions (Figure 3). The 3D supramolecular structure is further stabilized by other hydrogen bonds (N(3)-H(3 A)⋯O(8)ⅷ; N(3)-H(3B)⋯O(6); N(4)-H(4 A)⋯O(10)ⅹ and N(4)-H(4B)⋯O(11), symmetric code: ⅷ −x + 1, −y, −z + 1; ⅹ −x + 1, −y + 1, −z) (Table 1).

Figure 2 View of the 2D layer structure of 1.
Figure 2

View of the 2D layer structure of 1.

Figure 3 View of the 3D supramolecular structure of 1.
Figure 3

View of the 3D supramolecular structure of 1.

Table 1

H-Bonding geometry parameters (Å, °) for complexes 1 and 2

Complex D–H⋯A D–H (Å) H⋯A (Å) D⋯A (Å) D–H⋯A (°)
1 N(3)–H(3A)⋯O(8)ⅷ 0.89 1.92 2.794(3) 168.4
N(3)–H(3B)⋯O(6) 0.89 1.83 2.712(3) 172.4
N(3)–H(3B)⋯S(2) 0.89 2.79 3.633(2) 159.3
N(4)–H(4A)⋯O(10)ⅹ 0.89 2.07 2.859(3) 147.6
N(4)–H(4B)⋯O(11) 0.89 1.97 2.817(3) 158.7
N(4)–H(4B)⋯S(3) 0.89 2.88 3.576(3) 139.2
2 O(1W)–H(1A)⋯O(1) 0.86 1.79 2.650(3) 174.1
O(1W)–H(1A)⋯O(2) 0.86 2.56 2.970(2) 110.3
O(1W)–H(1A)⋯S(1) 0.86 2.66 3.383(2) 142.5
O(1W)–H(1B)⋯O(1)ⅲ 0.81 1.93 2.7207(19) 165.6

Complex 1: Symmetry codes: ⅷ −x + 1, −y, −z + 1; ⅹ −x + 1, −y + 1, −z.

Complex 2: Symmetry codes: ⅲ x, −y, z − 1/2.

2 crystallizes in monoclinic crystal system, C2/c space group. As seen in Figure 4, there are one crystallographically independent Ni(ii) ions, one SO4 2– ligands, two coordinated water molecules, and one phenanthroline. The Ni(ii) center is in a slightly distorted octahedral coordination geometry and six coordinated by two nitrogen atoms (N1 and N1i) of phen, two oxygen atoms (O1 and O1i) of two different coordinated water molecules, and two oxygen atoms (O2 and O2i) of two SO4 2– ligands. The Ni–O distances are in the range of 2.0539(12)–2.151(2) Å, and the Ni–N distance is 2.0573(15) Å.

Figure 4 Coordination environment of the Ni(ii) ion of 2 (symmetry codes: i −x + 1, y, −z + 3/2, ii −x + 1, y, −z + 5/2).
Figure 4

Coordination environment of the Ni(ii) ion of 2 (symmetry codes: i −x + 1, y, −z + 3/2, ii −x + 1, y, −z + 5/2).

As illustrated in Figure 5, these octahedrons are further connected by the SO4 2– ligands together, resulting in a 1D infinite chain structure extending along crystallographic b axis with the Ni–Ni separation of 6.547 Å. The 1D chain structure is also further consolidated through the face-to-face π–π stacking interactions between neighboring phenanthrolines with the centroid-to-centroid distance of 4.019(3). As shown in Figure 6, it is noteworthy that the intermolecular hydrogen bonds (O(1W)–H(1B)⋯O(1)iii, symmetric code: iii x, -y, z-1/2, as seen in Table 1) exist between oxygen atoms from the SO4 2– ligands and the coordinated water molecules, which connected the adjacent 1D chains into a 2D layered structure. Furthermore, the intramolecular hydrogen bonds further stabilized the two-dimensional structure of 2.

Figure 5 View of the 1D double-chain structure of 2 formed by one π–π interactions.
Figure 5

View of the 1D double-chain structure of 2 formed by one π–π interactions.

Figure 6 View of the 2D layer structure of 2 formed by hydrogen-bonding interactions (O–H⋯O).
Figure 6

View of the 2D layer structure of 2 formed by hydrogen-bonding interactions (O–H⋯O).

2.2 Luminescent properties

CPs constructed by the d10 metal centers and conjugated organic ligands are advantageous for constituting luminescent material. Thus, the solid phase luminescent spectra of 1 and 4,4′-bipy were measured at ambient temperature. In Figure 7, 4,4'-bipy exhibited a characteristic emission bands centered at 419 nm (λ ex = 343 nm), which can be attributed to the π*–π transition. 1 displayed a similar emission with 4,4′-bipy, the emission peak of 1 occurs at 421 nm (λ ex = 358 nm) [26,27]. Thus, the emission of 1 could be owing to the 4,4′-bipy.

Figure 7 Room-temperature solid-state luminescent spectra of 1 and 4,4′-bipy.
Figure 7

Room-temperature solid-state luminescent spectra of 1 and 4,4′-bipy.

3 Conclusion

In this study, we have successfully synthesized two novel CPs, and their structures and characters were studied. 1 displays binuclear units and each Zn ion is four-coordinated, which exhibit the [ZnNO3] distorted triangular cone geometry. 1 generated a 1D chain via the sulfate-bridge, and the 4,4′-bipy ligands connect adjacent 1D chains to yield a 2D layer which further extended into a 3D supramolecular network. 2 is six-coordinated and shows distorted octahedral coordination geometry. 2 possesses a 1D chain structure by sulfate-bridge and the adjacent 1D chains are connected by one π–π interactions into 1D double-chain structure which further extended into 2D layered structure through the hydrogen-bonding interactions. 1 shows a strong emission peak when excited, so it can be used as a potential fluorescent material.

4 Experimental method

All chemical reagents were derived from commercial origin and without further purification, and were obtained from Shanghai Hengfei Biological Technology Co., Ltd and Henan Pusai Chemical Products Co., Ltd, China. The C, H, and N contents were determined by a Perkin-Elmer 240 CHN elemental analyzer (Perkin-Elmer, North Waltham, USA). IR spectra were measured on a Perkin-Elmer Spectrum One FTIR spectrometer with a KBr background in the range of 4,000–400 cm−1. The luminescent properties were measured on a Renishaw inVia Raman Microscope.

Preparation of {(NH2(CH3)2)2[Zn2(bipy)(SO4)3]} n (1)

ZnSO4·6H2O (0.0288 g, 0.1 mmol), 4,4′-bipy (0.0159 g, 0.10 mmol), and 3-carboxy-1-carboxymethyl-2-oxidopyridinium (0.06 mmol, 0.0118 g) dissolved in DMF/H2O (3 mL, v/v: 1.5/1.5) were mixed in a 15 mL vial. The solution mixture was stirred at room temperature and heated to 97°C for 4 days under autogenous pressure. After cooling to room temperature at a rate of 5°C/h, light yellow rectangular crystals were obtained. Yield: 41% based on Zn. Anal. (%) calculated for C14H24N4O12S3Zn2: C, 25.27; H, 3.33; N, 8.42; Found %: C, 25.03; H, 3.29; N, 8.31.

Preparation of [Ni(phen)(SO4)(H2O)2] n (2)

A mixture of NiSO4·6H2O (0.0263 g, 0.1 mmol), phen (0.0126 g, 0.1 mmol), and 3-(carboxymethoxy)-2-naphthoic acid (0.06 mmol, 0.0948 g) were dissolved in DMF/H2O (5 mL, v/v: 3/2). The solution mixture was stirred at room temperature, then placed in a closed capped 15 mL vial, which was heated to 95°C for 4 days. After cooling to room temperature at a rate of 5°C/h, blue rhombic crystals were obtained. Yield: 54% based on Ni. Anal. (%) calculated for C12H12N2NiO6S: C 38.85; H 3.26; N 7.55; found: C 38.80; H 3.22; N 7.46.

4.1 X-ray crystallography

The right size of 1 and 2 single crystals was chosen and single crystal X-Ray diffraction study was conducted, the data were collected by a Bruker-AXS Smart CCD diffractometer with graphite-monochromatized Mo-Kα radiation (λ = 0.71073 Å) at 293(2) K, using the ω scan technique. The programs named SIR2014 [28] and SHELXL2018/3 [29] were solved for the crystal structure by direct method and refined using the full-matrix least square procedure on F 2 . Crystallographic details of 1 and 2 are listed in Table 2, the selected bond lengths and bond angles are given in Table 3. Respectively, CCDC numbers of 1 and 2 are 2356993 and 1885911.

Table 2

Crystalline data and refinement parameters for complexes 1 and 2

Complex 1 2
Empirical formula C14H24N4O12S3Zn2 C12H12N2NiO6S
Formula weight 667.29 370.99
Crystal system Triclinic Monoclinic
Space group P 1 ̅ C2/c
a (Å) 9.5109 (19) 15.182 (5)
b (Å) 10.1798 (19) 14.187 (5)
c (Å) 13.391 (3) 6.547 (5)
α (°) 88.666 (3) 90
β (°) 70.690 (3) 102.209 (5)
γ (°) 81.183 (3) 90
Volume (Å3) 1,208.6 (4) 1,378.2 (12)
Z 2 4
D c (g·cm−3) 1.834 1.934
µ (mm−1) 2.310 4.498
F (000) 680 792
θ range (°) 1.612–27.153 1.986–25.994
Crystal size (mm) 0.688 × 0.398 × 0.130 0.240 × 0.220 × 0.141
Tot. reflections 8,311 4,181
Uniq. reflections, R int 5,329, 0.0173 1,351, 0.0132
GOF on F 2 1.045 1.078
R 1 indices [I > 2σ(I)] 0.0283 0.0199
wR 2 indices (all data) 0.0736 0.0519
∆ρ min, ∆ρ max (e·Å–3) −0.438, 0.540 −0.331, 0.248
CCDC No. 2356993 1885911
Table 3

Selected bond lengths (Å) and angles (°) for the complexes 1 and 2

Bond Dist. Bond Dist.
Complex 1
N(1)–Zn(2) 2.0290 (18) O(5)–Zn(1) 1.9368 (18)
N(2)–Zn(1)ⅰ 2.0408 (18) O(7)–Zn(2)ⅱ 1.9599 (18)
O(2)–Zn(2) 1.9449 (16) O(9)–Zn(1) 1.9395 (17)
O(3)–Zn(1) 1.9354 (17) O(12)–Zn(2)ⅱ 1.9307 (19)
Angle (°) Angle (°)
O(3)–Zn(1)–O(5) 99.67 (8) O(12)ⅳ–Zn(2)–O(2) 102.53 (8)
O(3)–Zn(1)–O(9) 113.51 (9) O(12)ⅳ–Zn(2)–O(7)ⅳ 115.46 (9)
O(5)–Zn(1)–O(9) 115.17 (8) O(2)–Zn(2)–O(7)ⅳ 105.05 (8)
O(3)–Zn(1)–N(2)ⅲ 118.37 (8) O(12)ⅳ–Zn(2)–N(1) 120.36 (9)
O(5)–Zn(1)–N(2)ⅲ 107.74 (8) O(2)–Zn(2)–N(1) 116.66 (8)
O(9)–Zn(1)–N(2)ⅲ 102.84 (7) O(7)ⅳ–Zn(2)–N(1) 96.38 (8)
Complex 2
N(1)–Ni(1) 2.0573 (15) O(1W)–Ni(1) 2.0539 (12)
O(2)–Ni(1) 2.151 (2)
Angle (°) Angle (°)
O(1W)–Ni(1)–O(1W)ⅰ 94.54 (7) N(1)ⅰ–Ni(1)–O(2) 87.74 (5)
O(1W)–Ni(1)–N(1)ⅰ 172.65 (5) N(1)–Ni(1)–O(2) 89.85 (5)
O(1W)ⅰ–Ni(1)–N(1)ⅰ 92.49 (6) O(1W)–Ni(1)–O(2)ⅰ 92.33 (5)
O(1W)–Ni(1)–N(1) 92.49 (6) O(1W)ⅰ–Ni(1)–O(2)ⅰ 89.82 (4)
O(1W)ⅰ–Ni(1)–N(1) 172.65 (5) N(1)ⅰ–Ni(1)–O(2)ⅰ 89.85 (5)
N(1)ⅰ–Ni(1)–N(1) 80.58 (8) N(1)–Ni(1)–O(2)ⅰ 87.74 (5)
O(1W)–Ni(1)–O(2) 89.82 (4) O(2)–Ni(1)–O(2)ⅰ 176.83 (6)
O(1W)ⅰ–Ni(1)–O(2) 92.33 (5)

Complex 1: Symmetry codes: i x, y, z – 1, ii x + 1, y, z, ⅲ x, y, z + 1, ⅳ x – 1, y, z.

Complex 2: Symmetry codes: i −x + 1, y, −z + 3/2.

4.2 IR spectrum

The IR spectra of 1 and 2 are measured to characterize the functional groups. As seen in Figure S1, the absorption band of 1 at 3,425 cm–1 can be attributed to the N–H bond stretching. The absorption band of 2 at 3,327 cm–1 can be attributed to the O–H bond stretching vibrations of the water molecules. 1 and 2 absorption peaks residing at around 3,059 cm–1 is weak and can be ascribed to the C–H bond stretching vibrations of the pyridyl and phen rings. The bands of 1 and 2 appearing at 1,625–1,567 cm–1 are attributed to the ring vibration [ν(C═C) and ν(C═N)]. The bands of 1 and 2 located, respectively, at 1,414 and 1,427 cm–1 are attributed to the stretching vibrations of ν(C–N). The absorption bands of 1 residing at 1,305 cm–1 can be attributed to the N–H bond bending vibrations on the pyridyl rings of 4,4′-bipy. The absorption bands of 2 residing at 918–617 cm–1 can be attributed to the C–H bond bending vibrations on the phen rings.

  1. Funding information: This work was supported by the Natural Science Fund Program of Jilin Province (No. 20240101148JC).

  2. Author contributions: Huilin Wang: writing – original draft, experimental work, and editing. Sai Li: data curation and synthesizing. Hua Zhang: investigation and collecting data. Beihao Su: collecting data and validation. Xiuyan Wang: supervision and writing – review and editing.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

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Received: 2024-11-07
Accepted: 2024-12-11
Published Online: 2025-02-26

© 2025 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

Articles in the same Issue

  1. Research Articles
  2. Syntheses, crystal structures, and characterizations of two new Zn(ii)/Ni(ii) coordination polymers constructed by N-donor ligands and sulfate-bridge
  3. M-polynomial and NM-polynomial indices of camptothecin–polymer conjugate IT-101 structure
  4. Effects of alkyl size of AlR3 on its reaction with thiophene-2-carbonyl chloride
  5. Degree-based topological properties of borophene sheets
  6. A zinc(ii) polymer constructed with 3,5-pyrazoledicarboxylic acid and 1,4-bis(imidazol-1-ylmethyl)butane: Syntheses, crystal structures, and photoluminescence properties
  7. Study on (r, s)-generalised transformation graphs, a novel perspective based on transformation graphs
  8. New pyrazole-based Schiff base ligand and its Ni(ii) and Co(iii) complexes as antibacterial and anticancer agents: Synthesis, characterization, and molecular docking studies
  9. Sombor indices in main group metal chemistry: Computational evaluation of bismuth(iii) iodide, oxide/silicate frameworks, and dendrimers for QSAR applications
  10. Predictive modeling of physical properties in silane compounds using topological descriptors: A computational approach
  11. Review Article
  12. Critical review on the derivative of graphene with binary metal oxide-based nanocomposites for high-performance supercapacitor electrodes
  13. Retraction
  14. Retraction of “Synthesis, structure, and in vitro anti-lung cancer activity on an In-based nanoscale coordination polymer”
https://doi.org/10.1515/mgmc-2024-0029
Keywords for this article
coordination polymer; Zn(ii); Ni(ii); sulfate-bridge; luminescent properties
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Syntheses, crystal structures, and characterizations of two new Zn(ii)/Ni(ii) coordination polymers constructed by N-donor ligands and sulfate-bridge
  3. M-polynomial and NM-polynomial indices of camptothecin–polymer conjugate IT-101 structure
  4. Effects of alkyl size of AlR3 on its reaction with thiophene-2-carbonyl chloride
  5. Degree-based topological properties of borophene sheets
  6. A zinc(ii) polymer constructed with 3,5-pyrazoledicarboxylic acid and 1,4-bis(imidazol-1-ylmethyl)butane: Syntheses, crystal structures, and photoluminescence properties
  7. Study on (r, s)-generalised transformation graphs, a novel perspective based on transformation graphs
  8. New pyrazole-based Schiff base ligand and its Ni(ii) and Co(iii) complexes as antibacterial and anticancer agents: Synthesis, characterization, and molecular docking studies
  9. Sombor indices in main group metal chemistry: Computational evaluation of bismuth(iii) iodide, oxide/silicate frameworks, and dendrimers for QSAR applications
  10. Predictive modeling of physical properties in silane compounds using topological descriptors: A computational approach
  11. Review Article
  12. Critical review on the derivative of graphene with binary metal oxide-based nanocomposites for high-performance supercapacitor electrodes
  13. Retraction
  14. Retraction of “Synthesis, structure, and in vitro anti-lung cancer activity on an In-based nanoscale coordination polymer”
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