Abstract
C18H22O12Cd, monoclinic, P21/c (no. 14), a = 13.3069(9) Å, b = 9.9041(6) Å, c = 8.1580(5) Å, β = 96.244(10)°, V = 1031.57(12) Å3, Z = 2, R gt (F) = 0.0216, wR ref (F2) = 0.0522, T = 200 K.
The molecular 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.
Data collection and handling.
| Crystal: | Colorless block |
| Size: | 0.14 × 0.12 × 0.09 mm |
| Wavelength: | Mo Kα radiation (0.71073 Å) |
| μ: | 1.12 mm−1 |
| Diffractometer, scan mode: | SuperNova, ω |
| θmax, completeness: | 25.0°, 99% |
| N(hkl)measured, N(hkl)unique, Rint: | 3892, 1801, 0.022 |
| Criterion for Iobs, N(hkl)gt: | Iobs > 2 σ(Iobs), 1577 |
| N(param)refined: | 158 |
| Programs: | Bruker [1], Olex2 [2], Shelx [3], Diamond [4] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
| Atom | x | y | z | Uiso*/Ueq |
|---|---|---|---|---|
| Cd1 | 0.000000 | 0.500000 | 0.500000 | 0.01528 (10) |
| O1 | 0.07432 (11) | 0.44096 (15) | 0.28565 (19) | 0.0204 (4) |
| O2 | 0.15987 (13) | 0.63688 (15) | 0.29804 (19) | 0.0255 (4) |
| O3 | 0.21540 (11) | 0.58490 (15) | 0.01171 (19) | 0.0211 (4) |
| O4 | 0.70560 (13) | 0.68907 (17) | 0.1859 (2) | 0.0360 (4) |
| O6 | 0.08108 (15) | 0.32591 (17) | 0.6719 (2) | 0.0301 (5) |
| H6A | 0.058 (3) | 0.252 (2) | 0.702 (4) | 0.080 (12)* |
| H6B | 0.137 (2) | 0.325 (3) | 0.712 (3) | 0.021 (8)* |
| O7 | −0.14666 (13) | 0.37704 (18) | 0.3833 (2) | 0.0237 (4) |
| H7A | −0.162 (2) | 0.355 (3) | 0.472 (4) | 0.039 (9)* |
| H7B | −0.147 (3) | 0.316 (3) | 0.324 (4) | 0.055 (11)* |
| C1 | 0.12889 (17) | 0.5257 (2) | 0.2318 (3) | 0.0171 (5) |
| C2 | 0.1559 (2) | 0.4854 (2) | 0.0689 (3) | 0.0216 (6) |
| H2A | 0.195250 | 0.401643 | 0.089148 | 0.026* |
| H2B | 0.091495 | 0.469000 | −0.020538 | 0.026* |
| C3 | 0.32133 (16) | 0.5884 (2) | 0.0797 (3) | 0.0173 (5) |
| C4 | 0.37323 (17) | 0.6804 (2) | 0.0022 (3) | 0.0198 (5) |
| H4 | 0.335054 | 0.735801 | −0.085369 | 0.024* |
| C5 | 0.48019 (16) | 0.6888 (2) | 0.0549 (3) | 0.0200 (5) |
| H5 | 0.514450 | 0.749270 | 0.001815 | 0.024* |
| C6 | 0.53824 (17) | 0.6075 (2) | 0.1876 (3) | 0.0198 (5) |
| C7 | 0.4858 (2) | 0.5183 (2) | 0.2654 (3) | 0.0235 (6) |
| H7 | 0.524256 | 0.464421 | 0.354519 | 0.028* |
| C8 | 0.3773 (2) | 0.5071 (2) | 0.2139 (3) | 0.0219 (6) |
| H8 | 0.342965 | 0.447125 | 0.267520 | 0.026* |
| C9 | 0.65201 (19) | 0.6129 (2) | 0.2431 (3) | 0.0281 (6) |
| H9 | 0.686527 | 0.553633 | 0.328890 | 0.034* |
Source of material
An amount of 0.180 g 4-formylphenoxyacetic acid (1.0 mmol) and 0.040 g NaOH (1.0 mmol) were dissolved into 15 ml ethanol-water (v:v = 2:1) solution with stirring at room temperature. After the solution was stirred for 1.0 h, 5 ml water solution of 0.150 g cadmium nitrate tetrahydrate (0.5 mmol) was added. The mixture was stirred for 6 h at 70 °C. The colorless crystals of the title compound were obtained through slow evaporation in 25 days.
Experimental details
The hydrogen atoms were positioned geometrically. Their U iso values were set to 1.2U eq or 1.5U eq of the parent atoms.
Comment
Over the past decades, transition metal complexes show rich coordination pattern [5, 6] and properties in some fields [7], [8], [9], [10]. The Co(II), Mn(II) and Cu(II) complexes using 4-formylphenoxylate as ligand have been reported by Das [11]. Our group has been studying the synthesis, structure and properties of related metal complexes [12], [13], [14], [15].
In the title complex, the fundamental unit contains a Cd(II) ion, two 4-formylphenoxyacetic acid ligands and four coordinated water molecules. The asymmetric unit is one half of the complex (see the figure). The Cd(II) ion is six-coordinated with two O atoms from two 4-formylphenoxy-acetate ligands and four O atoms from four coordinated water molecules, forming a distorted octahedral coordination geometry. The Cd1–O bond distance are 2.3136(16) Å (O1, O1a), 2.2913(17) Å (O6, O6a) and 2.2695(17) Å (O7, O7a), respectively. The sum of bond angles around Cd1 (O7–Cd1–O6a 86.92(6)°, O6a–Cd1–O7a 93.08(6)°, O7a–Cd1–O6 86.92(6)°, O6–Cd1–O7 93.08(6)°) is 360. The complex molecules form 1D chained structure by hydrogen bonds.
Funding source: National Natural Science Foundation of China 10.13039/501100001809
Award Identifier / Grant number: 21171132
Funding source: Natural Science Foundation of Shandong 10.13039/501100007129
Award Identifier / Grant number: ZR2014BL003
Funding source: Project of Shandong Province Higher Educational Science and Technology Program 10.13039/501100015642
Award Identifier / Grant number: J14LC01
Funding source: Science Foundation of Weifang
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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Research funding: This project was supported by the National Natural Science Foundation of China (No. 21171132), the Natural Science Foundation of Shandong (ZR2014BL003), the Project of Shndong Province Higher Educational Science and Technology Program (J14LC01) and Science Foundation of Weifang.
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Conflict of interest statement: The authors declare no conflicts of interest regarding this article.
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© 2021 Xi-Shi Tai and Li-Hua Wang, published by De Gruyter, Berlin/Boston
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