Synthesis and Crystal Structure Determination of a Nickel(II) Complex of an Acyclic Pentadentate (N5) Mono Schiff Base Ligand
Abstract
:Introduction
Results and Discussion
Description of the X-ray Structure
Parameter | Value | Parameter | Value | |||||
---|---|---|---|---|---|---|---|---|
Empirical formula | C15H29Cl2N5NiO9 | ρcalcd (g cm–3) | 1.564 | |||||
Formula weight | 553.04 | μ (mm–1) | 3.781 | |||||
Temperature (K) | 294(2) | V (Å 3) | 2349.3(8) | |||||
Wavelength (Å) | 1.54060 | F (000) | 1152 | |||||
Crystal system | Monoclinic | Crystal size (mm) | 0.35 X 0.30 X 0.05 | |||||
Space group | P2l/c | θ range (º) | 4.11 to 60.01 | |||||
a (Å) | 10.170(2) | Index ranges | –6 ≤ h ≤ 11 | |||||
–17 ≤ k ≤ 17 | ||||||||
–16 ≤ l ≤ 17 | ||||||||
b (Å) | 15.494(3) | Reflns. collected | 3717 | |||||
c (Å) | 15.145(3) | GOF on F2 | 1.063 | |||||
β (º) | 100.119(16) | Final R(Fο2) | 0.0601 | |||||
Z | 4 | Weighted R(F ο2) | 0.1643 |
Bond lengths | ||
M(1)-N(1) 2.093(4) | M(1)-N(4) 2.084(4) | N(2)-C(6) 1.280(7) |
M(1)-N(2) 2.035(4) | M(1)-N(5) 2.099(4) | N(2)-C(8) 1.483(7) |
M(1)-N(3) 2.116(6) | M(1)-O(1) 2.194(4) | |
Bond angles | ||
N(1)-M(1)-N(2) 77.66(16) | N(2)-M(1)-N(4) 92.82(17) | N(4)-M(1)-N(5) 171.83(17) |
N(1)-M(1)-N(3) 172.2(2) | N(2)-M(1)-N(5) 95.32(16) | N(4)-M(1)-O(1) 84.19(17) |
N(1)-M(1)-N(4) 91.59(17) | N(2)-M(1)-O(1) 170.26(17) | N(5)-M(1)-O(1) 87.68(16) |
N(1)-M(1)-N(5) 89.59(16) | N(3)-M(1)-N(4) 94.2(2) | N(2)-C(6)-C(5) 115.1(4) |
N(1)-M(1)-O(1) 93.12(16) | N(3)-M(1)-N(5) 85.5(2) | N(2)-C(6)-C(7) 125.0(5) |
N(2)-M(1)-N(3) 96.8(2) | N(3)-M(1)-O(1) 92.7(2) | C(6)-N(2)-C(8) 121.8(5) |
Conclusions
Experimental
General
X-ray Crystal Structure Analysis.
Synthesis of [Ni(ppe-py)(H2O)](ClO4)2
Acknowledgements
References
- Prince, R.H.; Stotter, D.A. Complexes of quadri- and quinqudentate, mono- and bis Schiff-base ligands derived from acteylpyridine. Inorg. Chim. Acta 1974, 10, 89–92. [Google Scholar]
- Sorrell, T.N. Synthetic models for binuclear copper proteins. Tetrahedron Reports 1989, 45, 3–68. [Google Scholar]
- Mclachlan, G.A.; Fallon, G.D; Martin, R.L.; Mobarki, B.; Murray, K.S.; Spiccia, L. Binuclear nickel complexes with single azide bridges, structure and properties of [Ni2(N,N-bis(2-aminoethyl)-N’-(2-pyridylmethyl)ethane-1,2-diamine)2(μ-N3)](ClO4)3 and [Ni2(1,4-bis(2-pyridyl-methyl)-1,4,7-(triazacyclononane)2(μ-N3)](ClO4)3. Inorg. Chem. 1994, 33, 4663–4668. [Google Scholar]
- McLachlan, G.A.; Fallon, G.D; Martin, R.L.; Spiccia, L. Synthesis, structure and properties of five-coordinate copper(II) complexes of pentadentate ligands with pyridyl pendant arms. Inorg. Chem. 1995, 34, 254–261. [Google Scholar]
- McLachlan, G.A.; Brudenell, S.J.; Fallon, G.D. Synthesis, structure and properties of cobalt(III) complexes of pentadentate ligands with pyridyl pendant arms. J. Chem. Soc. Dalton 1995, 3, 439–447. [Google Scholar]
- Keypour, H.; Salehzadeh, S.; Pritchard, R.G.; Parish, R.V. Nickel(II) complexes of fully and partially condensed Schiff-base ligands derived from tris(3-aminopropyl)amine and acetylpyridine. Transition Met. Chem. Transition Met. Chem. 1998, 23, 605–607. [Google Scholar]
- Keypour, H.; Salehzadeh, S. Nickel(II) and copper(II) complexes of macrocyclic and acyclic Schiff-base ligands derived from new asymmetrical tripodal tetraamines and 2,6-diacetylpyridine. Transition Met. Chem. 2000, 25, 205–208. [Google Scholar]
- Keypour, H.; Salehzadeh, S.; Pritchard, R.G.; Parish, R.V. Synthesis and crystal structure determination of some asymmetrical and symmetrical CR-type macrocyclic Schiff-base complexes, with a single pendant coordinating 2-aminoethyl arm. Inorg. Chem. 2000, 39, 5787–5790. [Google Scholar]
- Keypour, H.; Pritchard, R.G.; Parish, R.V. Isolation of ternary complex precursors and partially condensed intermediates to macrocyclic complexes of nickel(II) and copper(II). Transition Met. Chem. 1998, 23, 609–613. [Google Scholar]
- Keypour, H.; Stotter, D.A. Macrocycle synthesis. CR-type complexes displaying pendant ligation and N3S co-ordination. Inorg. Chim. Acta 1979, 33, 149. [Google Scholar]
- Sheldrick, G. M. SHELX-97, Computer Program for Crystal Structure Refinement; University of Göttingen: Göttingen, Germany, 1997. [Google Scholar]
- International Tables for X-ray Crystallography; Kynoch Press: Birmingham, 1994; Vol. 4.
- Williams, D.H.; Fleming, I. Spectroscopic Methods in Organic Chemistry; McGraw-Hill: New York, 1966. [Google Scholar]
- Keypour, H.; Salehzadeh, S.; Pritchard, R.G.; Parish, R.V. Cadmium(II) complexes of fully condensed Schiff-base ligands derived from two different symmetrical and asymmetrical tripodal tetraamines and 2-acetylpyridine; the novel observations for heptadentate mono-capped trigonal antiprismatic Schiff-base complexes. Polyhedron 2000, 19, 1633–1637. [Google Scholar]
- Sample Availability: Available from the authors.
© 2001 by MDPI (http://www.mdpi.org). Reproduction is permitted for noncommercial purposes.
Share and Cite
Keypour, H.; Salehzadeh, S.; Pritchard, R.G.; Parish, R.V. Synthesis and Crystal Structure Determination of a Nickel(II) Complex of an Acyclic Pentadentate (N5) Mono Schiff Base Ligand. Molecules 2001, 6, 909-914. https://doi.org/10.3390/61100909
Keypour H, Salehzadeh S, Pritchard RG, Parish RV. Synthesis and Crystal Structure Determination of a Nickel(II) Complex of an Acyclic Pentadentate (N5) Mono Schiff Base Ligand. Molecules. 2001; 6(11):909-914. https://doi.org/10.3390/61100909
Chicago/Turabian StyleKeypour, Hassan, Sadegh Salehzadeh, R. G. Pritchard, and R. V. Parish. 2001. "Synthesis and Crystal Structure Determination of a Nickel(II) Complex of an Acyclic Pentadentate (N5) Mono Schiff Base Ligand" Molecules 6, no. 11: 909-914. https://doi.org/10.3390/61100909