Structure Prediction and Ultrasonic Assisted Synthesis of Coordination Compound Cadmium (II) Bromide with N,N’-diethylthiourea Ligand

Yuni Susanti, Fariati Fariati, Effendy Effendy, Yulyani Nur Azizah


Cadmium (II) halides with N,N'-diethylthiourea (detu) ligands at a stoichiometry of 1: 2 tend to form molecular complexes [Cd(detu)2X2] with a distorted tetrahedral geometry at the central atom. Generally, these complex compounds are prepared by the conventional method of reflux for 4 hour. The use of ultrasonic waves for complex synthesis can be an alternative to make the reaction time more efficient and environmentally friendly. The aim of this study was to synthesize and characterize complex compounds from CdBr2 and detu ligands using the ultrasonication method that have not previously reported. The synthesis of complex compounds was carried out by reacting CdBr2 and detu (1:2) in methanol solvent. In the synthesized compounds, a melting point test, electrical conductivity test, Fourier Transform Infrared (FTIR), Scanning Electron Microscope-Energy Dispersive Xray (SEM-EDX), qualitative test of bromide ion and calculation of free energy using Spartan'14 software were carried out for the complex structure prediction. The complex compound resulted has colorless needle crystals with a melting point of 93-94°C. The results of the EDX analysis provide the empirical formula C10H24CdBr2N4S2. The electrical conductivity test data and the bromide ion qualitative test proved that the synthesized complex compound was a molecular complex compound with the molecular formula [Cd(detu)2Br2]. The complex compound has two possible structures, namely a distorted tetrahedral and a square planar. Free energy calculations showed that complex compounds with a distorted tetrahedral structure and a square  planar have free energies of -527.5574 kJ/mol and -408.7424 kJ/mol, respectively.


CdBr2; characterization; coordination compound; detu; ultrasonication


Ahmad, S., Altaf, M., Evans, H. S., Isab, A. A., Malik, M. R., Ali, S., Shuja, S. (2011). Synthesis and Structural Characterization of Dibromodobis(N,N-dimethylthiourea-κS)cadmium(II) and Diidobis(N,N-dimethylthiourea-κS)cadmium(II). Journal of Chemistry Crystallography, 41, 1099-1104.

Ahmad, S., Amir, Q., Naz, G., Fazal, A., Fettouhi, M., Isab, A. A., . . . Lang, H. (2012). . Synthesis and Crystal Structures of Cadmium Iodide Complexes of N,N’-Diethylthiourea and 1,3-Diazinane-2-thione. Journal of Chemistry Crystallography, 42, 615-620.

Ajibade, P. A. (2013). Synthesis and Use of [Cd(detu)2(OOCCH3)2].H2O as Single Molecule Precursor for CdS Nanoparticles. The Scientific World Journal, 907562, 1-6.

Alfanaar, R., Notario, D. (2019). Sintesis Senyawa Koordinasi Astaxanthin dengan Bantuan Gelombang Ultrasonik. Jurnal Kimia dan Kemasan, 41(2), 88-94.

Alizadeh, R., Amani, V. (2016). Syntheses, crystal structure and photoluminescence of three cadmium (II) coordination complexes based on bipyridine ligands with different positions matheyl substituent. Inorganica Chimica Acta, 443, 151-159.

Althaf, M., Stoeckli-Evans, H., Murtaza, G., Isab, A. A., Ahmad, S., Shaheen, M. A. (2011). Structural Characterization of Cadmium(II)-Sulfato Complex, [Cd(N.N'-diethylthiourea)4(SO4)]. Journal of Structural Chemistry, 52(3), 625-630.

Andersen, O. (1984). Chelation of Cadmium. Environmental Health Perspectives, 54, 249-266.

Armaghan, M., Najafi, E., Knedel, Frank, W., Janiak, C. (2020). Synthesis and single crystal structure characterization of mixed-ligand coordination compound of zinc and cadmium with teh bridging ligand 1,2-bis(pyridin-4-ylmethylen)hydrazine. Zeitschrift fur anorganische und allgemeine chemie, 646(22), 1861-1868.

Azizah, Y. N., Mulyani, I., Wahyuningrum, D., Bima, D. N. (2020). Synthesis, characterization and antioxidant activity of kobalt(II)-hydrazone complex. Educhemia (Jurnal Kimia dan Pendidikan), 5(2), 119-133.

Blumbergs, E., Serga, V., Platacis, E., Maiorov, M., Shishkin, A. (2021). Cadmium recovery from spent Ni-Cd batteries: a brief review. Metals, 11(1714), 1-14.

Borsari, M. (2014). Cadmium: Coordination Chemistry. In M. Borsari, Enclyclopedia of Inorganic and Bioinorganic Chemistry (pp. 2-16). New York City: John Wiley & Sons, Ltd.

Etaiw, S. E.-d., Shalaby, E. M., El-aziz, D. M., Elzeny, I. (2021). Ultrasound irradiation synthesis and crystal structure of Co(II) thiocyanate supramolecular complex: Photocatalytic and sonocatalytic degradation of methyl violet 2B dye. Applied Organometallic Chemistry, 3(e6159), 1-16.

Fariati, I., Dasna, W., Fadli, Y., Qurbayni, S. (2019). Study of structure prediction of complex compound of zinc(II) chloride and cadmium(II) chloride with potassium cyanida and N,N--diethylthiourea ligand. International conference on electromagnetism, rock magnetism and magnetic material (p. 2251). Malang, Indonesia: AIP Publishing.

Fariati, Istikfaroh, N., Effendy, Darojah, L. A. (2016). Synthesis and characterization of coordination compounds of silver(I) nitrite with ligand ethylenethiourea and N,N'-diethylthiourea. The Journal of Pure and Applied Chemistry Research, 5(3), 142-147.

Gao, M., Zhao, Q., Yu, H., Fu, M., Li, Q. (2022). Insight into spodium–π bonding characteristics of the MX2· · · π (M = Zn, Cd and Hg; X = Cl, Br and I) complexes—a theoretical study. Molecules, 27, 2885.

Gaur, R., Jeevanandam, P. (2015). Effect of anion on morphology of CdS nanoparticles prepared via thermal decomposition of different cadmium thiourea complexes in a solvent and solid state. New Journal of Chemistry, 1-13. doi:10.1039/C5NJ01605C

Genchi, G., Sinicropi, M. S., Lauria, G., Carocci, A., Catalano, A. (2020). The effect of cadmium toxicity. International Journal of Environmental Research and Public Health, 17(3782), 1-24.

Ghosh, D. C., Biswas, R. (2002). Theoretical calculation of absolute radii of atoms and ions part 1 the atomic radii. International Journal of Molecular Sciences, 3, 87-113.

Hui, K. S., Hui, K., Dinh, D., Tsang, C., Cho, Y., Zhou, W., . . . Chun, H.-H. (2014). Green synthesis of dimension-controlled silver nanoparticle–graphene oxide with in situ ultrasonication. Acta Materialia, 64, 326-332.

Ismiyarto, Saputri, N., Rahmatia , L., Sarjono, P., Ngadiwiyana, Prasetya, N., Bima, D. (2021). Synthesis of Mn(II) complexes-carboxymethyl chitosan schiff base salicylaldehyde and antibacterial activity. Jurnal Kimia Valensi, 7(1), 10-21.

Mahmood, R., Sadaf, S., Isab, A. A., Akkurt, M., Sharif, S., Khan, I. U., . . . Ahmad, S. (2012). Synthesis and structural characterization of cadmium(II) complexes of tetramethylthiourea (tmtu); x-ray structure of [Cd(Tmtu)2Cl2]. Russian Journal of Coordination Chemistry, 38(7), 456-460.

Marcos, C., Alia, J. M., Adovasio, V., Prieto, M., Granda, G. S. (1998). Bis(thiourea)cadmium Halides. Acta Crystallography, C(59), 1225-1229.

Marcotrigiano, G. (1976). Preparation, Infrared, Raman, and NMR spectra of N,N-diethylthiourea complexes with zinc(II), cadmium (II), and mercury (II) halides. Zeitschrift für anorganische und allgemeine Chemie , 422, 80-88.

Mazor, L. (1975). Methods for detection of halogens in organic compounds. In L. Mazor, Analytical Chemistry of Organic Halogen Compounds (pp. 53-82). Hungary: Pergamon Press.

Moloto, M. J., Malik, M. A., O'Brien, P., Motevalli, M., Kolawole, G. A. (2003). Synthesis and characterisation of some N-alkyl/aryl and N,N’-dialkyl/diaryl thiourea cadmium(II) complexes: the single crystal X-ray structures of [CdCl2(CS(NH2)NHCH3)2] and [CdCl2(CS(NH2)NHCH2CH3)2]. Polyhedron, 22, 595-603.

Moloto, M. J., Revaprasadu, N., Kolawole, G. A., O'Brien, P., Malik, M. A., Motevalli, M. (2009). Synthesis and X-Ray single crystal structures of cadmium(II) complexes: CdCl2[CS(NHCH3)2]2 and CdCl2[CS(NH2)NHC6H5)4 single source precursors to CdS nanoparticles. E-Journal of Chemistry, 7(4), 1148-1155.

Mukhopadhyay, S. M. (2018). Sampel preparation for microscopic and spectroscopic characterization of solid surfaces and films. In S. Mitra, Sample preparatoion techniques in analytical chemistry (pp. 377-411). Ohio: John Wiley & Sons, Inc.

Nawaz, S., Sadaf, S., Fettouhi, M., Fazal, A., Ahmad, S. (2010). Dibromodobis(N,N,N’,N’-tetramethylthiourea- κS)cadmium(II). Acta Crystallographica Section E, 66, m950.

Nichols, L. (2022). Organic Chemistry Lab Techniques. California: LibreTexts.

Palmer, J. H., Parkin, G. (2015). Influence of benzannulation on metal coordination geometries: Synthesis and structural characterization of tris(2-mercapto-1-methylbenzimidazolyl)hydroborato cadmium bromide, {[TmMeBenz]Cd(l-Br)}2. Journal of Molecular Structure, 1081, 530-535.

Setiawan, W., Fariati, Effendy. (2017). Sintesis dan karakterisasi senyawa kompleks dari kadmium nitrat dan 1,3-bis(difenilfosfino)propana dengan stoikiometri 1:1. Journal Cis-Trans, 1(2), 18-21.

Shakeel, A., Altaf, A. A., Qureshi, A. M., Badshah, A. (2016). Thiourea derivaters in drug design and medicinal chemistry: a short review. Journal of Drug Design and Medicinal Chemistry, 2(1), 10-20.

Tariq, S., Aslam, M., Hasni, K., Khan, A., Ahmed, S., Khan, M., . . . Afzal, F. (2021). Determination of Total chloride/ bromide ion and total hardness of drinking water of Uthal and LUAWMS, Lasbela, Baluchistan, Pakistan. Frontiers in Chemical Sciences (FCS), 2(2), 107-115.

Ushasree, P. M., Jayavel, R. (2002). Growth and micromorphology of as-grown and etached bis(thiourea) cadmium chloride (BTCC) single crystal. Optical Materials, 21, 599-604.

Wahyuni, R. M., Wijaya, H. W., Sari, M. E., Dasna, I. W., Farida, N. (2022). Synthesis and characterization of complex compound from cadmium (II) chloride and cobalt (II) chloride with N.N'-diethylthiourea. The Journal of Pure and Applied Chemistry Research, 11(1), 1-8.

Young, J. C. (2013). True Melting Point Determination. The Chemical Educator, 18, 203-208.

Full Text: PDF

DOI: 10.15408/jkv.v9i1.30868


  • There are currently no refbacks.

Copyright (c) 2023 Yuni Susanti, Yulyani Nur Azizah

Creative Commons License
This work is licensed under a Creative Commons Attribution-ShareAlike 4.0 International License.