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Universidade Federal de Juiz de fora

Chemistry Departament

43º SBQ anual Reunion

A new 3D Cu2+ coordination polymer with mixed O- and N- donors ligands and a 6-connected pcu topological network.

Authors: Carlos M. D. S. Junior (PG- UFJF)

Talita V. F. da Silva (IC-UFJF)

Júlia B. Alves (IC-UFJF)

Maria Clara. R. Freitas (PQ-UFRRJ)

Chris H. J. Franco (PQ-UFJF)

Charlane C. Corrêa (PQ-UFJF)

Introduction

Porous materials

Introduction

“Materials made up of cavities, channels or interstices that can have a high surface area”.

Applications in medicine, chemistry, environmental engineering, and others.

Synthesis of Inorganic Materials, 4 ed, p. 289, 2019

Zeolites

zeolites: alkali or alkaline earth metal aluminosilicates found abundantly in nature

Figure 1: Structure of Boggsite Zeolite

American Mineralogist; 75, 1200–1204, 1990

American Journal of Materials Science, 7, 5, 196–221, 2017.

MOF

Metal Organic Framework ( MOF)

Figure 2: Synthesis of metal-organic framework 5 (MOF-5) from a Zn metal cluster and terephthalic acid.

Applied in areas such as medicine, biology, chemistry and others.

  • Can be built in infinite ways
  • Cavity formation
  • High porosity
  • Flexibility

Biomaterials Science, 974–989, 2018

Journal of Alloys and Compounds, 176–186, 2017

Chemical Society Reviews, 6927–6945, 2017

Accounts of Chemical Research, 51, 12, 3052–3064, 2018

Objectives

Objectives

  • Synthesize 3D coordination polymer from Cu2+ and hexamethylenetetramine (hmt) and glutaric acid (H2glu) ligands.

  • Characterize the compound by spectroscopic and structural techniques.

Synthesis of compound 1

Experimental part

+

0.22 mmol H2glu + 5mL H2O

0.22 mmol hmt + 5mL H2O

Ligands added simultaneously into a solution of 0,22 mmol Cu(NO₃)₂.3H₂O

"After one day green colored crystals, in a needle shape, were present in the solution"

yield: ~ 40%

Fourier-transform infrared spectroscopy (FTIR)

FTIR

Figure 3. Infrared absorption spectra for H2glu, Na2glu, hmt and compound 1 ligands

Main bands in the spectrum (cm-1): 1700,1620,1417,1236,1017, 809,667

Na2glu [∆ =177 cm-1] ; ∆ = 190 cm-1

∆salt ~ ∆pol

bidentade bridging

Asymmetric unit

single-crystal X-ray diffraction

Figure 4: Asymmetric unit of compound 1.

Twinning

45/55%

Table 1: Crystallographic data for compound 1

Crystallographic data

Coordination sphere

Coordination sphere

Figure 5: (a) Coordination sphere (b) Secondary building unit (SBU) for compound 1.

(Symmetry codes: i: + x, -y, -½ + z; ii: 3/2-x, ½-y, 2-z; iii: 3/2-x, -½ + y, 3/2-z; iv: 1-x, + y, 3/2-z).

Polymeric expansion in 2D

polymeric expansion

Figure 6: Polymeric expansion of compound 1 in two dimensions seen along the ac plane

Polymeric expansion in 3D

Polymeric expansion in 3D

Figure 7: Polymeric expansion of compound 1 in three dimensions seen along the ab plane

Hydrogen bonds

Hydrogen bonds

Figure 9: Hydrogen bonds present in the compound 1.

Symmetry codes: i: 1-x, -1 + y, 3/2-z; ii: + x, -1 + y, + z; iii: 1-x, + y, 3/2-z.

Table 3- Parameters of hydrogen bonds present in the compound 1 network.

Symmetry codes: i:-x,1+y,1/2-z.

Topological analysis

Topological analysis

Figure 10: Topological study for compound 1 in two dimensions.

Topological study

Topological analysis

Figure 11: Topological study for compound 1 in three dimensions.

From the simplification in cluster mode, it was obtained that the fundamental network is of the pcu type, uninodal and with a Point symbol (4¹².6³).

Conclusion & perspectives

Conclusion

  • The synthesis of 3D coordination polymer (compound 1) was made using the H2glu and hmt ligands,

  • 1 was characterized by spectroscopic and structural techniques.

  • The compound is formed by the SBU paddle wheel containing Cu2+ ions, extended by the H2glu and HMT (mixed O- and N- donor ligands).

  • The crystal grows presents a twinned structure (45/55%) and is stabilized only by an unconventional hydrogen bond of type C-H···N.

  • Topological analysis revealed a fundamental pcu type network, uninodal with a dot symbol (4¹².6³)

Perspectives

Perspectives

  • Thermogravimetric analysis
  • N2 adsorption tests
  • Heterogeneous catalysis tests

Thank you for your attention!

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