Syntheses, Characterization and X-ray Crystal Structure of Polymeric Heteronuclear Oxo-bridged Fe/Na Assembled with Salen-type Schiff Base and Dicyanamide
Science Journal of Chemistry
Volume 8, Issue 2, April 2020, Pages: 20-27
Received: Mar. 6, 2020; Accepted: Mar. 23, 2020; Published: Apr. 17, 2020
Views 293      Downloads 189
Popa Haba, Organic Coordination Chemistry Laboratory, Department of Chemistry, Faculty of Science and Technology, Cheikh Anta DIOP University, Dakar, Senegal
Mouhamadou Moustapha Sow, Coordination Chemistry Laboratory, Department of Chemistry, UFR SATIC, Alioune DIOP University, Bambey, Senegal
Mamour Sarr, Organic Coordination Chemistry Laboratory, Department of Chemistry, Faculty of Science and Technology, Cheikh Anta DIOP University, Dakar, Senegal
Ibrahima Elhadji Thiam, Organic Coordination Chemistry Laboratory, Department of Chemistry, Faculty of Science and Technology, Cheikh Anta DIOP University, Dakar, Senegal
Mahy Diaw, Coordination Chemistry Laboratory, Department of Chemistry, UFR SATIC, Alioune DIOP University, Bambey, Senegal
Mohamed Lamine Gaye, Organic Coordination Chemistry Laboratory, Department of Chemistry, Faculty of Science and Technology, Cheikh Anta DIOP University, Dakar, Senegal
Article Tools
Follow on us
Reaction of FeCl2.4H2O with 2-(-(2-(-2-hydroxy-3-methoxybenzylideneamino)phenylimino)methyl)-6-methoxyphenol (H2L) gives the metalloligand [Fe(L)].(H2O) (1). Reaction of metalloligand (1) with three fold of sodium dicyanamide Na[N(CN)2] gives the new tetranuclear compound [{FeIINaI(L)(EtOH)(HN(CN)2)}(μ-O){FeIIINaI(L)(NO3)]}]n (2) in which one of the two irons is oxidized to +3. Suitable crystals of (2) were grown by slow evaporation of ethanol solution during two weeks. The metalloligand (1) and the tetranuclear (2) complexes are characterized by IR and physical measurement. Spectroscopic evidence indicated that the Schiff base H2L behave an N2O2O’2 coordination tetradentate ligand. The structure of (2) was elucidated by X-ray diffraction analysis. The asymmetric unit of the compound contains two dideprotonated ligand molecules, two iron ions, one hexacoordinated sodium ion, one heptacoordinated sodium ion, one bidentate nitrate group, one monodentate dicyanamide unit, one coordinated ethanol molecule and an O2- ion which acts as a bridge between the FeII and the FeIII of two entities: [FeIINaI(L)(EtOH)(HN(CN)2)] and [FeIIINaI(L)(NO3)]. Bridge Fe—O(μ) bond lengths are 1.7813(14) and 1.7856(13) Å and bridging angle Fe—O—Fe is 144.78(8)°. The second terminal cyano group of the dicyanamide link another molecule complex through the heptacoordinated NaI leading a polymeric structure. Intermolecular hydrogen bond connect the polymeric chains to develop a three dimensional structure.
Iron, Metalloligand, O-vanillin, Sodium Dicyanamide
To cite this article
Popa Haba, Mouhamadou Moustapha Sow, Mamour Sarr, Ibrahima Elhadji Thiam, Mahy Diaw, Mohamed Lamine Gaye, Syntheses, Characterization and X-ray Crystal Structure of Polymeric Heteronuclear Oxo-bridged Fe/Na Assembled with Salen-type Schiff Base and Dicyanamide, Science Journal of Chemistry. Vol. 8, No. 2, 2020, pp. 20-27. doi: 10.11648/j.sjc.20200802.11
Copyright © 2020 Authors retain the copyright of this article.
This article is an open access article distributed under the Creative Commons Attribution License ( which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
N. Mahlooji, M. Behzad, H. A. Rudbari, G. Bruno and B. Ghanbari, Unique Examples of Copper(II)/Sodium(I) and Nickel(II)/Sodium(I) Schiff Base Complexes with Bridging Bis-Bidentate Salen Type Ligand: Synthesis, Crystal Structures and Antibacterial Studies. Inorganica Chimica Acta (2016), 445, 124–128.
M. Sarr, E. I. Thiam, M. Gaye, A. H. Barry, N. Alvarez and J. Ellena, Co-Crystal Structure of a Dinuclear (Zn-Y) and a Trinuclear (Zn-Y-Zn) Complexes Derived from a Schiff Base Ligand. European Journal of Chemistry (2018), 9, 67–73.
M. Sarr, M. Diop, E. I. Thiam, M. Gaye, A. H. Barry, J. B. Orton and S. J. Coles, A New Co-Crystal Dinuclear/Trinuclear ZnII–ZnII/ZnII–SmIII–ZnII Complex with a Salen-Type Schiff Base Ligand. Acta Crystallographica E (2018), 74, 1862–1866.
J.-P. Costes, F. Dahan, L. Vendier, S. Shova, G. Lorusso and M. Evangelisti, NiII–LnIII Complexes with o-Vanillin as the Main Ligand: Syntheses, Structures, Magnetic and Magnetocaloric Properties. Dalton Transactions (2018), 47, 1106–1116.
M. Mousavi, V. Béreau, J.-P. Costes, C. Duhayon and J.-P. Sutter, Oligomeric and Polymeric Organizations of Potassium Salts with Compartmental Schiff-Base Complexes as Ligands. CrystEngComm (2011), 13, 5908–5914.
T. Fatima, Imtiaz-ud-Din, A. Akbar, M. S. Anwar and M. N. Tahir, Six New Dinuclear Schiff Base Complexes of Cu(II)/Ln(III) System: Synthesis, Characterization and Magnetic Studies. Journal of Molecular Structure (2019), 1184, 462–467.
B. Cristóvão, D. Osypiuk, B. Miroslaw and Bartyzel, A. Syntheses, Crystal Structures, Thermal and Magnetic Properties of New Heterotrinuclear CuII–LnIII–CuII Complexes Incorporating N2O4-Donor Schiff Base Ligands. Polyhedron (2018), 144, 225–233.
L. Zhang, P.-P. Yang, L.-F. Li, Y.-Y. Hu and X.-L. Mei, A Tridecanuclear ZnGd12 Nanoscopic Cluster Exhibiting Large Magnetocaloric Effect. Inorganica Chimica Acta (2019), 499, 119170.
B. Monteiro, J. T. Coutinho and L. C. J. Pereira, Heterometallic 3d–4f SMMs. In Lanthanide-Based Multifunctional Materials; Elsevier, 2018; 1st Edition, pp 233–261.
S. Zhao, X. Lü, A. Hou, W.-Y. Wong, W.-K. Wong, X. Yang and R. A. Jones, Heteronuclear Trimetallic and 1D Polymeric 3d–4f Schiff Base Complexes with OCN and SCN Ligands. Dalton Transactions (2009), 43, 9595–9602.
W.-K. Dong, S.-S. Zheng, J.-T. Zhang, Y. Zhang and Y.-X. Sun, Luminescent Properties of Heterotrinuclear 3d–4f Complexes Constructed from a Naphthalenediol-Based Acyclic Bis(Salamo)-Type Ligand. Spectrochimica Acta, Part A: Molecular and Biomolecular Spectroscopy (2017), 184, 141–150.
J.-W. Zhang, W.-H. Liu, C.-R. Wang, B.-Q. Liu and Y.-P. Dong, A Series of Linear CoII2LnIII2 Clusters Derived from 3,4-Dichlorobenzoate and 2,2′-Bipyridine: Syntheses, Structures, and Properties. Inorganica Chimica Acta (2020), 502, 119343.
M. T. Kaczmarek, M. Zabiszak, M. Nowak and R. Jastrzab, Lanthanides: Schiff Base Complexes, Applications in Cancer Diagnosis, Therapy, and Antibacterial Activity. Coordination Chemistry Reviews (2018), 370, 42–54.
B. Cristóvão, B. Miroslaw, J. Kłak and M. Rams, Carbonato-Bridged Heteronuclear NiII2LnIII2 (Ln=Tb, Dy, Ho, Er, Tm, Yb, Lu) Complexes Synthesized by Fixation of Atmospheric CO2 – Structural and Magnetic Studies. Polyhedron (2015), 85, 697–704.
A. Bilyachenko, M. Levitsky, A. Yalymov, A. Korlyukov, A. Vologzhanina, Y. Kozlov, L. Shulpina, D. Nesterov, A. Pombeiro, F. Lamaty, X. Bantreil, A. Fetre, D. Liu, J. Martinez, J. Long, J. Larionova, Y. Guari, A. L. Trigub, Y. V. Zubavichus, I. E. Golub, O. A. Filippov, E. S. Shubina, and G. B. Shul’pin, A Heterometallic (Fe6Na8) Cage-like Silsesquioxane: Synthesis, Structure, Spin Glass Behavior and High Catalytic Activity. RSC Advances (2016), 6, 48165–48180.
S. Hou, X.-Y. Tang, Y. Li, R.-X. Wang, F.-F. Chen, Y. Wang, Y.-X. Chi and J. Jin, Syntheses, Crystal Structures and Photophysical Properties of a Series of Zn-Ln Coordination Polymers. Journal of Molecular Structure (2018), 1167, 239–247.
P.-P. Liu, C.-Y. Wang, M. Zhang and X.-Q. Song, Pentanuclear Sandwich-Type ZnII-LnIII Clusters Based on a New Salen-like Salicylamide Ligand: Structure, near-Infrared Emission and Magnetic Properties. Polyhedron (2017), 129, 133–140.
M. Maity, M. C. Majee, S. Kundu, S. K. Samanta, E. C. Sañudo, S. Ghosh and M. Chaudhury, Pentanuclear 3d–4f Heterometal Complexes of MII3LnIII2 (M = Ni, Cu, Zn and Ln = Nd, Gd, Tb) Combinations: Syntheses, Structures, Magnetism, and Photoluminescence Properties. Inorganic Chemistry (2015), 54 (20), 9715–9726.
W.-X. Feng, Y.-N. Hui, G.-X. Shi, D. Zou, X.-Q. Lü, J.-R. Song, D.-D. Fan, W.-K. Wong and R. A. Jones, Synthesis, Structure and near-Infrared (NIR) Luminescence of Series of Zn2Ln (Ln=Nd, Yb or Er) Complexes Based on the Salen-Type Schiff-Base Ligand with the Flexible Linker. Inorganic Chemistry Communications (2012), 20, 33–36.
Y. Chen, S. She, L. Zheng, B. Hu, W. Chen, B. Xu, Z. Chen, F. Zhou and Y. Li, Heteronuclear M(II)–Ln(III) (M=Co, Mn; Ln=La, Pr, Sm, Gd, Dy and Er) Coordination Polymers: Synthesis, Structures and Magnetic Properties. Polyhedron (2011), 30, 3010–3016.
D. Pinkert, S. Demeshko, F. Schax, B. Braun, F. Meyer and C. A Limberg, Dinuclear Molecular Iron(II) Silicate with Two High-Spin Square-Planar FeO4 Units. Angewandte Chemie International Edition (2013), 52, 5155–5158.
K. Mason, I. A. Gass, S. Parsons, A. Collins, F. J. White, A. M. Z. Slawin, E. K. Brechin and P. A. Tasker, Building Fe(Iii) Clusters with Derivatised Salicylaldoximes. Dalton Transactions (2010), 39, 2727–2734.
A. Dogaru, J.-L. Liu, C. Maxim, G. Marinescu, R. Clérac and M. Andruh, Assembling CuIILnIIIOsIII Heterotrimetallic Octanuclear Complexes and 1D Coordination Polymers from the Same Molecular Modules. Polyhedron (2020), 175, 114242.
S. Thakurta, J. Chakraborty, G. Rosair, R. J. Butcher and Mitra, S. The Interplay of O–H⋯O Hydrogen Bonding in the Generation of Three New Supramolecular Complexes of CuII, NiII and CoIII: Syntheses, Characterization and Structural Aspects. Inorganica Chimica Acta (2009), 362, 2828–2836.
G. M. Sheldrick, It SHELXT – Integrated Space-Group and Crystal-Structure Determination. Acta Crystallographica A (2015), 71, 3–8.
G. M. Sheldrick, Crystal Structure Refinement with It SHELXL. Acta Crystallographica C (2015), 71, 3–8.
L. J. Farrugia, It WinGX and It ORTEP for Windows: An Update. Journal of Applied Crystallography (2012), 45, 849–854.
W. J. Geary, The Use of Conductivity Measurements in Organic Solvents for the Characterisation of Coordination Compounds. Coordination Chemistry Reviews (1971), 7, 81–122.
R. D. Bereman, M. L. Good, B. J. Kalbacher and J. Buttone, Preparation, Characterization, Moessbauer Spectra, and Electron Spin Resonance Spectra of Iron(II) and Iron(III) Complexes of the Dithiolate Cyclopentadienedithiocarboxylate. Inorganic Chemistry (1976), 15, 618–621.
S.; Ross, T. Weyhermüller, E. Bill, E. Bothe, U. Flörke, K. Wieghardt and P. Chaudhuri, Asymmetric Heterodinuclear FeIIIMII (M = Zn, Cu, Ni, Fe, Mn), CoIIIFeII and FeIICoIII Species: Synthesis, Structure, Redox Behavior, and Magnetism. European Journal of Inorganic Chemistry (2004), 984–997.
A. W. Addison, T. N. Rao, J. Reedijk, J. van Rijn and G. C. Verschoor, Synthesis, Structure, and Spectroscopic Properties of Copper(II) Compounds Containing Nitrogen–Sulphur Donor Ligands; the Crystal and Molecular Structure of Aqua[1,7-Bis(N-Methylbenzimidazol-2′-yl)-2,6-Dithiaheptane] Copper(II) Perchlorate. Journal of Chemical Society Dalton Transactions (1984), 1349–1356.
S. Jana, S. Chatterjee and S. Chattopadhyay, Syntheses, Characterization and X-Ray Crystal Structures of Hexa-Coordinated Monomeric and Oxo-Bridged Dimeric Fe(III) Compounds with Salen-Type Schiff Bases. Polyhedron (2012), 48, 189–198.
S. H. Strauss, M. J. Pawlik, J. Skowyra, J. R. Kennedy, O. P. Anderson, K. Spartalian and J. L. Dye, Comparison of the Molecular and Electronic Structures of (µ-Oxo)bis[(5,10,15,20-Tetraphenylporphyrinato)Iron(III)] and (µ-Oxo)bis[(7,8-Dihydro-5,10,15,20-Tetraphenylporphyrinato)Iron(III)]. Inorganic Chemistry (1987), 26, 724–730.
Y. Li, Q. Wu, L. Lecren and R. Clérac, Synthesis, Structure and Magnetism of New Polynuclear Transition Metal Aggregates Assembled with Schiff-Base Ligand and Anionic N-Donor Ligands. Journal of Molecular Structure (2008), 890, 339–345.
Science Publishing Group
1 Rockefeller Plaza,
10th and 11th Floors,
New York, NY 10020
Tel: (001)347-983-5186