Home Crystal structure of diaqua-bis(4-(hydroxymethyl)-benzoato-k1 O)zinc(II), C16H18O8Zn
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Crystal structure of diaqua-bis(4-(hydroxymethyl)-benzoato-k1 O)zinc(II), C16H18O8Zn

  • Yujiao Huang , Ben Li , Siyi Miao , Linhui Luo , Haixia Pang ORCID logo EMAIL logo and Qiang Tang EMAIL logo
Published/Copyright: November 1, 2022

Abstract

C16H18O8Zn, monoclinic, I2/a (no. 15), a = 12.152(2) Å, b = 5.0051(8) Å, c = 27.273(5) Å, β = 101.536(7)°, V = 1625.3(5) Å3, Z = 4, Rgt (F) = 0.052, wRref (F 2) = 0.143, T = 296 K.

CCDC No.: 2194575

The crystal structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Colorless block
Size: 0.12 × 0.1 × 0.08 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.55 mm−1
Diffractometer, scan mode: Bruker Apex-II, φ and ω-scans
θ max, completeness: 32.2°, >99%
N(hkl)measured, N(hkl)unique, R int: 8502, 2683, 0.059
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 1804
N(param)refined: 114
Programs: Bruker programs [1], SHELX [2, 3]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

x y z U iso*/U eq
Zn1 0.250000 0.07395 (9) 0.500000 0.03397 (17)
O1 0.23136 (17) 0.3320 (4) 0.44306 (7) 0.0356 (4)
O2 0.41157 (18) 0.2527 (4) 0.46461 (8) 0.0418 (5)
O3 0.36122 (17) −0.2058 (4) 0.52767 (8) 0.0422 (5)
H3A 0.335282 −0.306215 0.546251 0.063*
H3B 0.418732 −0.135805 0.543211 0.063*
O4 0.4828 (3) 1.1050 (5) 0.26783 (13) 0.0858 (12)
H4 0.467313 0.955961 0.255949 0.129*
C1 0.3498 (2) 0.5713 (5) 0.39939 (10) 0.0284 (5)
C2 0.4550 (3) 0.6760 (7) 0.40037 (11) 0.0393 (7)
H2 0.515386 0.620562 0.424821 0.047*
C3 0.4715 (3) 0.8643 (7) 0.36501 (12) 0.0423 (7)
H3 0.542939 0.933144 0.365899 0.051*
C4 0.3826 (3) 0.9498 (6) 0.32860 (11) 0.0396 (7)
C5 0.2783 (3) 0.8448 (8) 0.32810 (12) 0.0478 (8)
H5 0.217923 0.901357 0.303734 0.057*
C6 0.2604 (2) 0.6582 (7) 0.36264 (11) 0.0404 (7)
H6 0.188711 0.590100 0.361469 0.049*
C7 0.3326 (2) 0.3712 (5) 0.43759 (10) 0.0308 (6)
C8 0.3997 (4) 1.1633 (8) 0.29231 (15) 0.0607 (11)
H8A 0.330318 1.188505 0.268086 0.073*
H8B 0.417269 1.330152 0.310276 0.073*

Source of materials

The title compound was synthesized by mixing 0.760 g (0.5 mmol) 4-hydroxymethylbenzoic acid, 0.0845 g (0.5 mmol) ZnI2, 5 ml ethyl alcohol absolute and 3 ml H2O in a 50 ml beaker. After all the raw materials were dissolved, triethylamine was added dropwise until a large amount of white granular precipitate appears. After stirring the solution thoroughly, strain the supernatant through filter paper into another beaker. Then waiting for the solution to evaporate, yellow block crystals came out with a yield of 76% after a month. Elemental Analysis Data (%, measured/theoretical): C 47.51/47.56; H, 4.48/4.46; O, 31.63/31.71. IR spectrum (cm−1, KBr pellet): 3072(m), 1608(m), 1569(m), 1428(w), 408(w), 1278(s), 1202(w), 1178(w), 1048(s), 987(w), 761(s), 523(m).

Comment

Organic aromatic carboxylate ligands contain a ring facilitating electron transfer, and are preferred for the construction of metal complexes due to the diversity and flexibility of carboxylate coordination patterns and potential functionality [4], [5], [6]. The hydroxyl and carboxyl groups of 4-hydroxymethylbenzoic acid have attracted much attention because of their ability to react with various functional groups [7]. We have previously published some metal complexes of Co(II), Ni(II) with 4-hydroxymethylbenzoic acid ligand [8, 9]. Zinc is a very important biocompatible metal of the highest importance in the metabolism and proper performance of the immune system [10].

The title zinc complex was synthesized under solvent conditions. There is one half of the title molecules in one asymmetric unit. The zinc atom adopts a tetrahedral coordination derived from two carboxylate groups and oxygen atoms in the two water molecules. In the complex, the Zn1—O1 bond length is 1.997(2) Å, the Zn1—O3 bond length is 1.987(2) Å [11, 12]. The Zn—O2 is too long and weak for a coordination ability. The O3—Zn1—O3 bond angle is 90.40(13)°, the O3—Zn1—O1 bond angle is 135.52(8)°, the relative O3—Zn1—O1 bond angle is 101.39(9)°, the O1—Zn1—O1 bond angle is 99.45(12)°, and the remaining bond lengths and angles are all within the normal range. Due to the two coordinated water molecules acting as the hydrogen-bonding donors and acceptors, a three-dimensional hydrogen-bonded network is formed.


Corresponding authors: Haixia Pang and Qiang Tang, Hubei Provincial Key Laboratory of Green Materials for Light Industry, Collaborative Innovation Center of Green Lightweight Materials and Processing, School of Materials and Chemical Engineering, Hubei University of Technology, Wuhan 430068, China, E-mail:

Funding source: Hubei Provincial Key Laboratory of Green Materials for Light Industry and Collaborative Innovation Center of Green Light-Weight Materials and Processing

Award Identifier / Grant number: 202107A08

Funding source: Student’s Platform for Innovation and Entrepreneurship Training Program of Hubei University of Technology

Award Identifier / Grant number: X202110500107

Funding source: Hubei University of Technology School-Level Teaching and Research Project

Award Identifier / Grant number: 2013003

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This work is supported by the Hubei Provincial Key Laboratory of Green Materials for Light Industry and Collaborative Innovation Center of Green Light-Weight Materials and Processing (No. 202107A08), the Student’s Platform for Innovation and Entrepreneurship Training Program of Hubei University of Technology (No. X202110500107) and Hubei University of Technology School-Level Teaching and Research Project (No. 2013003).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2022-08-25
Accepted: 2022-10-10
Published Online: 2022-11-01
Published in Print: 2023-01-27

© 2022 the author(s), published by De Gruyter, Berlin/Boston

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

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