Synthesis, characterization, crystal structure, thermal behavior, and biological activity of a new heterotrinuclear complex: [(NiL(NCS)(H2O))2Cd(DMF)2]

Article abstract of DOI:10.1080/15533174.2013.862679

A new trinuclear heterometallic nickel(II)-cadmium(II)-nickel(II) complex, [(NiL(NCS)(H₂O))₂Cd(DMF)₂] (DMF: dimethylformamide) (1), has been synthesized by using NiL as the so-called metallo ligand where H₂L = N,N′-bis(salicylidene)-1,3-diaminopropane, cadmium nitrate, and amonium thiocyanate. The title complex was characterized by various methods including elemental analyses, IR, ¹H-NMR, ¹³C-NMR, TG-DTA, and X-ray diffraction techniques. The complex crystallizes in monoclinic space group P2_1/c, with unit cell dimensions a = 10.6217(3), b = 13.3487(4), c = 16.0043(4) ?, β = 93.823(2)°. The complex was screened for antimicrobial activities by the disc diffusion using DMF as solvent. The minimum inhibitory concentration values were calculated.

Full text of DOI:10.1080/15533174.2013.862679

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Synthesis and Reactivity in Inorganic, Metal-Organic,
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Synthesis, Characterization, Crystal Structure,
Thermal Behavior, and Biological Activity of a New
Heterotrinuclear Complex: [(NiL(NCS)(H O)) Cd(DMF) ]
2
2
2
a
a
b
a
c
Alper Yardan , Ahmet Karahan , N. Burcu Arslan , Cigdem Hopa , Mukadderat Gokmen ,
b
d
Canan Kazak & Raif Kurtaran
a
Department of Chemistry, Balikesir University Art & Science Faculty, Balikesir, Turkey
b
Department of Physics, Faculty of Arts and Sciences, Ondokuz Mayis University, Samsun,
Turkey
c
Faculty of Veterinary, Balikesir University, Balikesir, Turkey
Click for updates
d
Materials Science and Engineering, Alanya Engineering Faculty, Akdeniz University, Alanya,
Antalya, Turkey
Accepted author version posted online: 13 Jan 2015.
To cite this article: Alper Yardan, Ahmet Karahan, N. Burcu Arslan, Cigdem Hopa, Mukadderat Gokmen, Canan Kazak &
Raif Kurtaran (2015) Synthesis, Characterization, Crystal Structure, Thermal Behavior, and Biological Activity of a New
Heterotrinuclear Complex: [(NiL(NCS)(H O)) Cd(DMF) ], Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal
2
2
2
Chemistry, 45:8, 1224-1233, DOI: 10.1080/15533174.2013.862679
To link to this article: http://dx.doi.org/10.1080/15533174.2013.862679
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Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry (2015) 45, 1224–1233
Copyright © Taylor & Francis Group, LLC
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533174.2013.862679
Synthesis, Characterization, Crystal Structure, Thermal
Behavior, and Biological Activity of a New Heterotrinuclear
Complex: [(NiL(NCS)(H O)) Cd(DMF) ]
2
2
2
1
1
2
1
3
ALPER YARDAN , AHMET KARAHAN , N. BURCU ARSLAN , CIGDEM HOPA , MUKADDERAT GOKMEN ,
2
4
CANAN KAZAK , and RAIF KURTARAN
1
Department of Chemistry, Balikesir University Art & Science Faculty, Balikesir, Turkey
Department of Physics, Faculty of Arts and Sciences, Ondokuz Mayis University, Samsun, Turkey
Faculty of Veterinary, Balikesir University, Balikesir, Turkey
2
3
4
Materials Science and Engineering, Alanya Engineering Faculty, Akdeniz University, Alanya, Antalya, Turkey
Received 26 August 2013; accepted 2 November 2013
A new trinuclear heterometallic nickel(II)-cadmium(II)-nickel(II) complex, [(NiL(NCS)(H O)) Cd(DMF) ] (DMF: dimethylformamide)
2
2
2
0
(
1), has been synthesized by using NiL as the so-called metallo ligand where H L D N,N -bis(salicylidene)-1,3-diaminopropane, cadmium
2
1
nitrate, and amonium thiocyanate. The title complex was characterized by various methods including elemental analyses, IR, H-NMR,
1
3
C-NMR, TG-DTA, and X-ray diffraction techniques. The complex crystallizes in monoclinic space group P21/c, with unit cell dimensions
ꢀ
ꢀ
a D 10.6217(3), b D 13.3487(4), c D 16.0043(4) A, b D 93.823(2) . The complex was screened for antimicrobial activities by the disc
diffusion using DMF as solvent. The minimum inhibitory concentration values were calculated.
Keywords: Schiff base ligands, hetero trinuclear complexes, thermal analysis, single crystal XRD, biological activity
Introduction
received enormous attention due to their extensive use in the
design and preparation of molecule based materials.
In this study, we report the synthesis and structural char-
[
14–17]
Research on coordination polynuclear complexes of transi-
tion metals containing Schiff base ligands, continue to attract acterization of the new linear hetero trinuclear complex of
intense interest because of their importance in catalysis, general formula [(Ni(L)(NCS)(H O)) Cd(DMF) ] has been
2
2
2
[1–3]
molecular electronics, photochemistry.
At the same time synthesized. Scheme 1 demonstrates the synthetic pathway
heteropolymetallic complexes are active fields of research for [(NiL(NCS)(H O)) Cd(DMF) ].
2
2
2
including chemistry, material science and nanostructure stud-
[
4–8]
ies.
Tetradentate ONNO type Schiff base ligands derived
Experimental
Materials and Measurements
from N,N’-bis(salicylidene)-1,3-diaminopropane (H L), salen
have been used for complexation in recent years. Salen-type
Schiff base complexes themselves can act as ligand-complexes
2
and can chelate a second metal substrate using phenolate All chemical reagents and solvents used were purchased from
oxygen atoms of Schiff base ligand to construct extended Merck, Aldrich, or Carlo Erba and used without further puri-
[9,10]
homo- or heteropolynuclear complexes.
Recently, phe- fication. The elemental analyses for complex were carried out
noxo bridged heterometallic complexes have been great inter- at the Eurovector 3018 CHNS analyzer. IR spectra were
[
11–13]
est to the chemists due to their magnetic interactions.
A
obtained by using IR grade KBr disks on a Perkin Elmer
survey of literature reveals that although heterotrinuclear 1600 Series FT-IR spectrophotometer in the range of 4000–
¡
1
1
13
complexes containing both nickel(II) and cadmium(II) cen- 400 cm . H-NMR and C-NMR analysis were performed
ters have not received adequate attention, mono-and poly- using a Bruker Ultrashield Superconducting 400 MHz liquid
nuclear Schiff base complexes of Ni(II) and Cd(II) have NMR spectrometer. Thermogravimetry/differential thermal
analysis (TG/DTA) measurements were run on a Perkin
Elmer Diamond.
Address correspondence to Alper Yardan, Department of Chem-
istry, Balikesir University Art & Science Faculty, Cagis 10145,
Balikesir, Turkey. E-mail: alpyardan@hotmail.com
Color versions of one or more of the figures in the article can be N,N -bis(salicylidene)-1,3-propanediamine (H L) and was pre-
Synthesis of the [(NiL(NCS)(H O)) Cd(DMF) ]
2
2
2
0
2
found online at www.tandfonline.com/lsrt.
pared by reacting basic ethanolic solution of salicylaldehyde and

New Heterotrinuclear Complex
1225
Sch. 1. Synthetic pathway for [(NiL(NCS)(H O)) Cd(DMF) ].
2
2
2
1
,3-diamino propane as described previously in the literature (77%). C H CdN Ni O S (1088.84): Anal. Calcd. C 46.33; H
42 50 8 2 8 2
[18]
(Scheme 1). NiL was prepared by reacting basic ethanolic 4.63; N 10.29%; Found C 46.15; H 4.81; N 10.41%.
solution of H L with NiCl as described previously in the litera-
2
2
[18]
ture.
A solution of Cd(NO ) .4H O (1 mmol; 0.308 g) in
3 2 2
methanol (10 mL) was added slowly with constant stirring to a Crystal Structure Determination
DMF solution (10 mL) of the NiL (2 mmol; 0.678 g). NH SCN
4
The data collection was performed at 293 K on a STOE
(2 mmol; 0.194 g) dissolved in water (10 mL) was added drop-
IPDS II diffractometer equipped with a graphite monochro-
ꢀ
wise to the mixture. The mixture was stirred at boiling point
under air atmosphere. The resultant mixture filtered and left to
stand at room temperature for four days. Dark-green crystals
were collected by filtration and dried in open air. Yield: 0.84 g
mated Mo–Ka radiation (λ D 0.71073 A). The structure was
[19]
solved by direct methods using SHELXS-97
and refined
ꢀ
ꢀ
Table 2. Bond lengths (A) and angles ( ) in the metal coordina-
tion spheres of complex 1
Cd1-O1
Cd1-O2
Cd1-O3
Ni1-N2
Ni1-N1
Ni1-O2
Ni1-O1
O3-C19
N2-C11
N2-C10
N1-C7
2.2411(13)
2.3181(15)
2.3611(16)
2.0231(18)
2.025(2)
2.0358(14)
2.0376(15)
1.246(3)
N1-C8
N3-C18
N4-C19
N4-C20
N4-C21
Ni1-N3
Ni1-O4
S1-C18
O1-C17
O2-C1
1.466(3)
1.158(3)
1.301(3)
1.454(4)
1.455(3)
2.127(2)
2.1347(19)
1.630(3)
1.326(2)
1.325(3)
Table 1. Crystal and experimental data for the complex 1
Chemical formula
CCDC No.
Formula weight
C42 H50 Cd N Ni O S
8 2 8 2
769387
1088.84
Crystal system, space group
Monoclinic, P21/c
10.6217(3)
13.3487(4)
16.0043(4)
93.823(2)
2264.13(11)
2
1.597
1116
1.441
0.71073
293(2)
–13/13, –16/16, 20/20
1.92–26.63
3804 (I > 2s (I))
4735
294
0.0750
ꢀ
a (A)
ꢀ
b (A)
ꢀ
c (A)
1.271(3)
1.466(3)
1.273(3)
b
ꢀ
3
Volume (A )
Z
¡
3
Calculated Density (Mg.m
)
)
O1-Cd1-O1
O1-Cd1-O2
O1-Cd1-O2
O2-Cd1-O2
O1-Cd1-O3
O1-Cd1-O3
O2-Cd1-O3
O2-Cd1-O3
O1-Cd1-O3
O1-Cd1-O3
O2-Cd1-O3
O3-Cd1-O3
N2-Ni1-N1
N2-Ni1-O2
180.0
107.71(5)
72.29(5)
180.0
87.65(5)
92.35(5)
90.52(6)
89.48(6)
92.35(5)
87.65(5)
90.52(6)
180.0
N1-Ni1-O2
N2-Ni1-O1
N1-Ni1-O1
O2-Ni1-O1
N2-Ni1-N3
N1-Ni1-N3
O1-Ni1-N3
N2-Ni1-O4
N1-Ni1-O4
O2-Ni1-O4
O1-Ni1-O4
N3-Ni1-O4
O2-Ni1-N3
90.48(7)
90.02(7)
173.06(7)
82.65(6)
87.93(8)
88.74(8)
92.77(7)
89.30(8)
89.10(9)
88.53(7)
89.73(7)
176.27(9)
94.53(7)
(
F000
)
¡
1
Absoption coefficient (mm
Wavelength
Temperature (K)
ꢀ
h, k, l index ( )
umin-umax( )
ꢀ
Number of reflections used
Independent reflections
Number of parameters
Rint
R; R (I >2s (I))
S
Drmin.; Drmax.(e/A )
0.0265; 0.0603
0.950
–0.48, 0.33
w
96.80(8)
172.37(7)
ꢀ
3

1
226
Yardan et al.
ꢀ
ꢀ
Table 3. Hydrogen bonding distances (A) and angles ( ) for com- Antimicrobial Screening
plex 1
Antimicrobial activities of complexes were determined by
d(D-H) d(H ¢ ¢ ¢ A) d(DvA) ff(D-H ¢ ¢ ¢ A) the disc diffusion method of CLSI (2006) on Mueller-
Hilton agar (Oxoid, CM337). All tests were performed in
D-HA
i
O(4)-HvO(3)
O(4)-H ¢ ¢ ¢ S(1)
0.809
0.886
1.920
2.417
2.690
3.294
158.54
170.03
duplicate to check the results. Suspension of the tested
microorganisms (10 CFU/mL) was spread on the solid
ii
6
i
ii
media plates. Test solution was prepared in DMF. Then
antimicrobial susceptibity blank discs (Oxoid Ltd., Basing-
stoke, England) were soaked with 10 mL of the stock solu-
tions and placed on the inoculated plates, they were
Symmetry codes: –x, –y, 2 – z; –x, –1/2 C y, 2.5 – z.
ꢀ
incubated at 35 C for 24 h for bacteria. The diameters of
by a full-matrix least-squares procedure using the program
All non-hydrogen atoms were easily found
from the difference Fourier map and refined anisotropically.
All carbon and hydrogen atoms were included using a riding
model. Molecular graphics were prepared using ORTEP 3.
[
20]
the inhibition zones were measured in millimeters. The
diameter of the zone of clearance (including the diameter
of the disk) was measured to the nearest whole milimeter
SHELXL-97.
[
22]
[
21] and interpreted on the basis of CLSI guideline.
Biological Activity of the Complex
Microorganisms Used
Determination of Minimum Inhibitory
Concentration
A total of 3 Gram-negative and 3 Gram-positive organisms
were used in the study. The isolates Escherichia coli ATCC
2
5292, Pseudomonas fluorencens ATCC 49642, Enterobacter The minimum inhibitory concentration (MIC) of the metal
sakazakii ATCC BAA-894, Staphylococcus aureus ATCC complex against the test microorganisms were employed to
538, Bacillus cereus ATCC 11778, Listeria monocytogenes the macrodilution broth susceptibility assay. Determination
6
ATCC 764.
of the results of MIC was done according to the method of
the turbidity of the inocula was adjusted to match that of 0.5
McFarland standards. The tubes were incubated in aerobi-
Antibiotic Gentamicin Used (Control)
ꢀ
cally at 35 C for 20 h and at the end of the incubation period,
The antibiotic standard used in this study was Gentamicin the bacterial growth in the test tubes was checked and the last
G10 susceptibility test discs (10 mg per disc) which were tube of growth observed concentration MIC was
[
22]
obtained from Oxoid Ltd., Basingstoke, England.
determined.
Fig. 1. FT-IR spectrum of (a) H L ligand and (b) complex 1.
2

New Heterotrinuclear Complex
1227
1
Fig. 2. H-NMR spectra of ligand (H L).
2
1
Fig. 3. H-NMR spectra of complex 1.

1
228
Yardan et al.
1
3
Fig. 4. C-NMR spectra of ligand (H L).
2
¡
1
Results and Discussion
broad absorptions in the 3366 cm region due to the presence
of water (Figure 1). This very broad band can also indicate
the presence of strong hydrogen bonds, which is substantiated
by crystal structure. The n(CHN) stretching vibration for N-
IR and NMR Spectra
¡
1
The H L ligand and the complex 1 FT-IR studies are shown in bonded thiocyanate usually appears below 2100 cm and our
2
¡
1
Figure 1. The interest of the IR spectrum of the title complex complex 1 shows a strong band at 2071 cm (Figure 1) sup-
lies mainly in the bands due to the thiocyanate ion, water mol- porting the presence of terminally N-bonded thiocyanate
ecule and carbonyl group from the DMF ligand. The spectrum groups to the Ni atom.[
16,25]
Also, the n(CHN) stretching
was compared with the free ligand’s one (H L) which shows vibrations of azomethine groups of the heterotrinuclear Schiff
2
¡
1
¡1
significant bands at 1611 cm for CHN stretching vibration, base complexes are observed a strong band at 1639 cm (Fig-
¡
1
¡1
2
752–2748 cm for phenolic O ÀÀ H stretching and 1294 cm
for phenolic C ÀÀ O (Figure 1). The mononuclear complex methine groups are coordinated to the metal ion. These data
ure 1). This situation indicates the nitrogen atoms of the azo-
[26,27]
(
NiL) does not show bands from the aromatic O–H stretching are consistent with the literature values.
The n(CHO)
and the C D N stretching frequency is shifted to upper wave- stretching vibration of the DMF molecules can be assigned to
¡
1
¡1
length from 1611 to 1639 cm . Also, medium intense bands the band at 1554 cm in the IR spectrum, which is lower
¡
1
¡1
¡1
assignable to Ni ÀÀ N (542 cm ) and Ni ÀÀ O (470 cm ) than that in free DMF molecules (1655 cm ) due to the coor-
[23,24]
[28]
stretching vibrations can be observed.
The FT-IR spectra dination of the DMF oxygen atoms to the Ni(II) ion, which
of the complex 1 clearly show the characteristic medium and is consistent with the results of X-ray analysis.

New Heterotrinuclear Complex
1229
1
3
Fig. 5. C-NMR spectra of complex 1.
Fig. 6. TG/DTA curves of the [(NiL(NCS)(H O) Cd(DMF) ].
2
2
2

1
230
Yardan et al.
Fig. 7. The ORTEP drawing of the complex 1 with the atomic numbering scheme. Displacement ellipsoids are drawn at the 50%
probability level and H atoms have been omitted for clarity.
H-NMR spectra of complex were recorded in DMF solu- curves (Figure 6) indicate that complex 1 is not decomposite
ꢀ
tion at 400 MHz and chemical shifts are in units of ppm rela- up to 83 C and then gradual decomposition occurs in three
ꢀ
tive to TMS. Peak of ligand azomethine proton was observed successive steps within the temperature range 83–1200 C
.58 ppm in H-NMR spectra (Figure 2). Otherwise, com- with endothermic effects at 113, 370, and 529 C. The first
1
ꢀ
8
ꢀ
plex azomethine proton signals shifted 7.91 ppm (Figure 3). weight loss between 83 and 145 C is associated with the
This situation has shown that azomethine nitrogen joined release of water and DMF molecules (observed 17.3%; calcd.
[
32,33]
coordination. Intramolecular hydrogen bonding accounts for 16.7%).
3.5 ppm frequency of the phenolic hydrogen signals in the ligand L and thiocyanate groups (observed 51.4%; calcd.
H L ligand. The absence of peak 13.5 ppm in the complex 56.6%) and probably the formation of Ni CdO as the final
Second and third steps involve the loss of the
1
2
2
4
ꢀ
spectra indicates loss of phenolic hydroxy proton on residue at 1200 C (observed 31.7%; calcd. 27%).
[
29]
complexation.
1
3
In C-NMR spectrum, ligand imine signals (166.1 ppm)
are shifted to upfield (163.7) after complexation which means
that the shifts are due to coordination of the ligand to metal
Crystal Structure
[30,31]
atom by the azomethine nitrogen (Figures 4 and 5).
The molecular structure of complex 1 obtained by X-ray dif-
fraction studies is shown in Figures 7 and 8. Also data collec-
tion and crystal data are given in Table 1, and important
bond lengths and bonding angles around the coordination
sphere are given in Table 2. The X-ray structural study
TG-DTA Curves
To examine thermal stability of 1, thermogravimetric and dif- reveals that complex 1 consists of heterometallic assembly of
ferential thermal analyses (TG-DTA) were made between 20 Ni(II) and Cd(II). The central cadmium atom, which is
ꢀ
and 1200 C in the static atmosphere of nitrogen. TG-DTA located on the inversion centre, has a distorted octahedral

New Heterotrinuclear Complex
1231
coordination geometry with six oxygen donor sets, four from Ni atom to complete the sixth-coordination [Ni–N5 D 2.127
ꢀ
the ligands in the equatorial planes and two from the DMF (2) A]. Ni-Cd atoms are equatorially bridged by two phenolic
ꢀ
groups in the apical positions. The Cd-O bond distances oxygen atoms of ligand with angles of Ni1–O1–Cd1 D 102.62
ꢀ
ꢀ
range from 2.241 to 2.361A. The bond angles around Cd are (6) and Ni1–O2–Cd1 D 100.07 (6). The Ni¢ ¢ ¢ Cd distance is
ꢀ
ꢀ
in the range of 72.29–180.0 . The greatest deviation of bond 3.342 A. The possible hydrogen bonds indicate intermolecular
angles from the ideal octahedral angles is found for O1–Cd– hydrogen bonds. These hydrogen bonds are rather weak inter-
i
ꢀ
ꢀ
O2 and O1 –Cd–O2, 72.29 (5) and 107.71 (5), respectively. actions as can be seen from the details given in Table 3. O–H¢ ¢ ¢
The distortion from an ideal octahedral geometry is a conse- O intermolecular interactions interlink these chains along the
quence of the limited opening of the tetradentate ligands, bc-axis.
which reduces the bridging O1–Cd–O2 angle. All other bond
angles are close to the ideal values. The isothiocyanato moi-
ꢀ
Biological Activity
ety is almost linear N5—C8—S1 178.3 (2). The maximum
¡
ꢀ
deviation from linearity of SCN ion is 1.7 .
Screening for antimicrobial activities of the stock solutions of
the Schiff base and the metal complexes were performed
qualitatively using the disc diffusion method. The metal com-
The terminal Ni atoms are also six-coordinated by two imine
nitrogen atoms, two deprotonated phenoxo oxygen atoms from
the ligand, an oxygen atom of water molecule, and a nitrogen
atom from terminal thiocyanate anion. The axial positions are
occupied with the O atom of the water molecule [Ni–O4 D
plex 1, NiL and the H L yielded clear inhibition zones
2
[
34]
around the disc.
These showed activity against E. coli
ATCC 25292, P. fluorescens ATCC 49642, and S. aureus
ATCC 6538, while NiL was showed strong activity against
ꢀ
¡
2
.1347 (19) A] and N atom of the SCN ion coordinate to the
Fig. 8. Packing of the atoms in the unit cell.

1
232
Yardan et al.
Table 4. Antimicrobial screening of complex 1 (mm)
Table 5. Antimicrobial activity (MIC) of the complexes (mg/mL)
Stock solution
Control
Micro
organisms
(including
Complex NiL H L culture)
Diameter of inhibition zone (mm)
Sources
2
*
Microorganism
Complex 1 NiL H L Control
Escherichia coli
Pseudomonas
fluorescens
Enterobacter
sakazakii
Staphylococcus
aureus
Bacillus cereus
Listeria
ATCC 25292
ATCC 49642
16
16
32 64
32 64
**
**
2
Escherichia coli
ATCC 25292
Pseudomonas
fluorescens
ATCC 49642
Enterobacter
14
13
11
11
9
8
23
24
ATCC 11778
ATCC 6538
32
16
64 128
32 64
**
**
10
12
9
24
ATCC 7064
ATCC 764
32
32
64 128
64 128
**
**
sakazakii
ATCC 11778
Staphylococcus
aureus ATCC 6538
Bacillus cereus ATCC
monocytogenes
12
11
9
11
10
9
7
7
8
23
24
24
**Growth determination.
7
064
may be due to the effect of the metal ions on the normal cell
process.
Listeria monocytogenes
ATCC 764
*
Gentamicin.
Conclusion
E. sakazakii ATCC 11778 and these complexes and the free
ligand showed weak activity against L. monocytogenes The heterometallic trinuclear Ni(II)-Cd(II)-Ni(II) complex
ATCC 764 (Table 4). If the inhibition zone measures 2 and from N,N’-bis(salicylidene)-1,3-diaminopropane (H L) has
2
3
mm, then the complex has a good bactericidal action on been synthesized in dimethylformamide medium and investi-
the tested bacterium. If the inhibition zone more than 3 mm gated using elemental analyses, infrared and electronic spec-
1
13
across, then it is considered very effective, but if there is no tra, H- and C-NMR spectra, XRD, and thermal analysis.
inhibition zone then the complex has no activity on the bacte- The phenolate oxygen atoms of Schiff base ligand bridged
[35]
rium, and will not be retained for treatment.
nickel and cadmium atoms. The distorted octahedral coordi-
The antimicrobial activities of free ligand (H L) and the nation sphere of nickel is completed by aqua molecule and
2
complex 1 on the inoculated plates have been screened isothiocyanate ion. Although the pseudohalide ions are
against Escherichia coli ATCC 25292, Pseudomonas fluores- attractive as coligands due to their bridging metal ions to
cens ATCC, Enterobacter sakazakii ATCC 11778, Staphylo- each other, and neutralize the charges of the complexes, in
coccus aureus ATCC 6538, Bacillus cereus ATCC 7064 ve this complex isothiocyanate ions are bonded to the nickel
[
36]
Listeria monocytogenes ATCC 764 by the Agar Disc Diffu- atoms as a terminal ligand. The most recent by Pearson,
¡
sion Method and the control antibiotic disc (gentamicin). suggest that S in SCN is soft and will prefer to coordinate
The metal complex yielded clear inhibition zones around the with soft acids whereas N in SCN is hard and coordinates
¡
disc. The complex 1 showed strong activity against E. coli with hard acids. So nickel ions are coordinated with the hard-
¡
ATCC 25292 and showed weak activity against L. mononcto- est part of the NCS ion. The biological activities of the char-
genes ATCC 764 (Table 4).
acterized complex 1 were also studied and compared with
As shown Table 5, the MIC values of the compounds that H L and NiL. Studies along these lines are currently in prog-
2
show positive results in the screening process were determined ress in our laboratory.
as a quantitative measurement of antibacterial activity. The
activities of the complex have been compared with the activ-
ity of standard antibiotic gentamicin. The results revealed Funding
that the complex is most effective against E. coli ATCC
2
5292, P. fluorescens ATCC, S. aureus ATCC 6538 with The financial support of scientific research Council of Balike-
MIC value of 16 mg/mL while the complex has lower MIC sir University (Project No. 2007/10) is gratefully
value of 32 mg/mL against bacteria of E. sakazakii ATCC acknowledged.
1
7
1778, B. cereus ATCC 7064 ve L. monocytogenes ATCC
64. Though there is sufficient increase in the bacteriostatic
activity of the complex 1, it could not reach the effectiveness Supplementary Material
of the conventional antibacterial agent, Gentamicin. The
results of this study are with similar to the our previous CCDC 769387 contains the supplementary crystallographic
[34]
study. This study suggests that the antibacterial activity of data. These data can be obtained free of charge via http://
the ligand is enhanced when it is chelated with metal ions. www.ccdc.cam.ac.uk/conts/retrieving.html, or from the
The increase in the antimicrobial activity of metal chelates Cambridge Crystallographic Data Centre, 12 Union Road,

New Heterotrinuclear Complex
1233
Cambridge CB21EZ, UK; fax: (C44) 1223 336 033; or e-mail:
18. Atakol, O.; Nazir, H.; Arici, C.; Durmus, S.; Svoboda, I.;
Fuess, H. Inorg. Chim. Acta 2003, 342, 295–300.
deposit@ccdc.cam.ac.uk
1
9. Sheldrick, G. M. SHELXS-97, Programs for Crystal Structure
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0. Sheldrick, G. M. SHELXL-97, Programs for Crystal Structure
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1. Farrugia, L. J. J. App. Cryst. 1997, 30, 565.
2. Methods for dilution antimicrobial susceptibility tests for bacteria
that grow aerobically; Approved standard-seventh edition; CLSI doc-
ument M7-A7 (ISBN 1–56238-587-9) Clinical and Laboratory
Standard Institute, 2006.
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