The crystal structure of chlorido-bis(1,10-phenantroline-κ 2 N,N′)-(2-formylphenoxyacetato-κ 2 O,O) lead(II), C33H23N4O4ClPb
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Hou Zhan-Feng
und
Tai Xi-Shi
Abstract
C33H23N4O4ClPb, monoclinic, P21/n (no. 14), a = 11.0932(8) Å, b = 16.7331(10) Å, c = 16.1349(10) Å, β = 107.018(2)°, V = 2863.9(3) Å3, Z = 4, R gt(F) = 0.0364, wR ref(F 2) = 0.0870, T = 293(2) K.
The molecular structure is shown in the figure. Table 1 contains the crystallographic data. The list of the atoms including atomic coordinates and displacement parameters can be found in the cif-file attached to this article.
Data collection and handling.
| Crystal: | Block, colourless |
| Wavelength: | Mo Kα radiation (0.71073 Å) |
| μ: | 6.03 mm−1 |
| Diffractometer, scan mode: | Bruker D8, φ and ω-scans |
| θ max, completeness: | 27.5°, >99 % |
| N(hkl)measured, N(hkl)unique, R int: | 78022, 6505, 0.093 |
| Criterion for I obs, N(hkl)gt: | I obs > 2 σ(I obs), 5367 |
| N(param)refined: | 388 |
| Programs: | Bruker programs 1 , OLEX2 2 , SHELX 3 , DIAMOND 4 |
1 Source of materials
Adding 0.2781 g PbCl2 (1.0 mmol) to 30 ml ethanol-water (v:v = 1:1) solution containing 0.1802 g 2-formylphenoxyacetic acid (1.0 mmol), 0.1982 g 1,10-phenantroline (1.0 mmol) and 0.040 g sodium hydroxide (1.0 mmol) at room temperature. Then the aforementioned mixture was heated at 81 °C for 3 h with stirring. After cooling to room temperature the mixture was filtered. The colorless block crystals were received from the filtrate after 25 days.
2 Experimental details
Coordinates of hydrogen atoms were refined without any constraints or restraints. The hydrogen atoms were positioned geometrically. Their U iso values were set to 1.2 U eq of the parent atoms.
3 Comment
The synthesis and characterization of lead(II) complexes has been one of the interests of coordination chemistry, as they exhibited novel structure 5 , 6 , 7 and properties such as luminescent property, 8 selective potentiometric microsensor, 9 iodine capture and dye removel, 10 and so on. In this work, a new Pb(II) complex has been synthesized by the assembly of PbCl2, 2-formylphenoxyacetic acid, 1,10-phenantroline and sodium hydroxide. The molecular structure of the title complex is shown in Figure 1. The single crystal X-ray diffraction shows that the Pb(II) complex is made up of one Pb(II) cation, two 1,10-phenantroline molecules, one 2-formylphenoxyacetate ligand, and one chloride ion. The Pb(II) ion is coordinated with four N atoms (N1, N2, N3, and N4) of two 1,10-phenantroline ligands, two O atoms (O1 and O2) of one coordinated H2O molecules, and two N atoms (N1, N2) of one 2-formylphenoxyacetate ligand, and one chloride ion, which forms a seven-coordinated distorted pentagonal bipyramid coordination geometry (Figure 1). Both 1,10-phenantroline and 2-formylphenoxyacetate ligands are in a bidentate coordination mode. The bond angles of N–Pb1–N, N–Pb–O, O–Pb–O, O–Pb–Cl, and N–Pb–Cl are in the range of 59.30(12)–129.61(12)°, 73.68(13)–151.33(13)°, 49.80(10)°, 94.53(10)–117.41(10)°, and 83.98(9)–148.55(9)°. The lengths of Pb–O bonds, Pb–N bonds, and Pb–Cl bond are in the range of 2.501(4)–2.710(4) Å, 2.531(4)–2.774(4) Å, and 2.9471(17) Å, respectively which are agreement with those in refs. 11 and 12. The dihedral angle of two phenantroline rings is 86.53°. The Pb(II) complex molecules form 1D chained structure by π–π interactions.
Acknowledgments
This project was supported by the Henan Academy of Sciences (20253808001) and the National Natural Science Foundation of China (No. 21171132, https://doi.org/10.13039/501100001809).
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