A hydrogen-bonded dimer of a novel Co(II) complex of monoethanolamine with thiocyanate: Synthesis, spectra, thermal behaviour and crystal structure

Article abstract of DOI:10.1016/S0022-2860(02)00105-9

A strongly hydrogen-bonded dimer of the Co(II) complex of monoethanolamine, [Co(meaH)₃][Co(mea)(meaH)₂](SCN)₃, was synthesized and characterized by single crystal X-ray diffractometry, UV-Vis and IR spectroscopy. The complex consists of [Co(meaH)₃]²⁺ and [Co(mea)(meaH)₂]⁺, and three SCN^- anions. In each cation, the Co(II) ion is coordinated by a distorted octahedral arrangement of three monoethanolamine ligands in a bidentate manner. One of the monoethanolamine ligands in the [Co(mea)(meaH)₂]⁺ cation is in the deprotonated form by losing its hydroxyl hydrogen. The complex cation units are held together by three strong O-H...O bonds formed between three ethanolic oxygens forming a hydrogen-bonded dimer of [Co(meaH)₃]²⁺?[Co(mea) (meaH)₂]⁺. The hydrogen bonding O?O distances are significantly short at ca. 2.41(4) ?. The SCN^- anions are involved in hydrogen bonding connecting the dimeric units to give a three dimensional infinite network. During the thermal decomposition process, the complex loses the monoethanolamine ligands in the first stage, followed by the decomposition of the SCN^- anions at higher temperatures to give metallic cobalt as the end product.

Full text of DOI:10.1016/S0022-2860(02)00105-9

Journal of Molecular Structure 641 (2002) 119±124
www.elsevier.com/locate/molstruc
A hydrogen-bonded dimer of a novel Co(II) complex
of monoethanolamine with thiocyanate:
synthesis, spectra, thermal behaviour and crystal structure
a,
a
Veysel T. Yilmaz , Omer Andac , Ahmet Karadag , William T.A. Harrison
a
b
*
aDepartment of Chemistry, Faculty of Arts and Sciences, Ondokuz Mayis University, 55139 Kurupelit, Samsun, Turkey
bDepartment of Chemistry, University of Aberdeen, Meston Walk, Aberdeen AB24 3UE, Scotland, UK
Received 1 August 2001; revised 1 March 2002; accepted 1 March 2002
Abstract
A strongly hydrogen-bonded dimer of the Co(II) complex of monoethanolamine, [Co(meaH)3][Co(mea)(meaH)2](SCN)3,
was synthesized and characterized by single crystal X-ray diffractometry, UV±Vis and IR spectroscopy. The complex consists
of [Co(meaH)3]21 and [Co(mea)(meaH)2]1, and three SCN2 anions. In each cation, the Co(II) ion is coordinated by a distorted
octahedral arrangement of three monoethanolamine ligands in a bidentate manner. One of the monoethanolamine ligands in the
[Co(mea)(meaH)2]1 cation is in the deprotonated form by losing its hydroxyl hydrogen. The complex cation units are held
together by three strong O±H¼O bonds formed between three ethanolic oxygens forming a hydrogen-bonded dimer of
1
[Co(meaH)3]21´´´[Co(mea)(meaH)2] . The hydrogen bonding O´´´O distances are signi®cantly short at ca. 2.41(4) A. T he
Ê
SCN2 anions are involved in hydrogen bonding connecting the dimeric units to give a three dimensional in®nite network.
During the thermal decomposition process, the complex loses the monoethanolamine ligands in the ®rst stage, followed by the
decomposition of the SCN2 anions at higher temperatures to give metallic cobalt as the end product. q 2002 Elsevier Science
B.V. All rights reserved.
Keywords: Monoethanolamine complex; Hydrogen-bonded dimer; Crystal structure; Thermal analysis
1. Introduction
monoethanolamine in aqueous solution. The IR and
EPR spectra of the solid metal complexes of mono-
ethanolamine were reported by Brannon et al. [5], and
Masoud et al. [6]. There are a few reports on the
synthesis and structural characterization of mixed-
ligand metal complexes of monoethanolamine
[7±9]. These studies indicated that the monoethano-
lamine ligand coordinates to metal ion as a neutral
ligand or ethanolaminate monoanion, which is formed
by losing the ethanolic hydroxyl hydrogen. Further-
more, the X-ray structural analysis showed two mono-
ethanolamine ligands coordinating to the Cu(II) ion
mono- and bidentately [8].
Ethanolamines are a class of alkoxides used to a
large extent in sol±gel processing [1,2]. Monoethano-
lamine is a versatile bifunctional ligand coordinating
metal ions through the amine nitrogen and ethanol
oxygen atoms behaving as a bidentate ligand.
Hancock [3] and Casassas et al. [4] studied the d±d
spectra and stability of transition metal complexes of
* Corresponding author. Tel.: 190-362-457-6020x5116; fax:
190-362-457-6081.
E-mail address: vtyilmaz@omu.edu.tr (V.T. Yilmaz).
0022-2860/02/$ - see front matter q 2002 Elsevier Science B.V. All rights reserved.
PII: S0022-2860(02)00105-9

120
V.T. Yilmaz et al. / Journal of Molecular Structure 641 (2002) 119±124
Table 1
Crystallographic data for the Co(II) complex of monoethanolamine
and KSCN were purchased from Merck and used
without further puri®cation.
The electronic spectrum was measured on a
Unicam UV2 spectrophotometer in a 1 £ 1023 M
aqueous solution of the monoethanolamine complex
in the 200±900 nm range. The IR spectrum was
recorded on a Mattson FTIR spectrophotometer in
the range 300±4000 cm21 as KBr pellets. The
elemental analyses (C, H and N contents) were
performed at TUBITAK Marmara Research Center
(Gebze). Thermal analysis curves (TG, DTA and
DTG) were obtained using a Rigaku TG8110 thermal
analyser in a dynamic nitrogen atmosphere with a
¯ow rate of 80 cm3 min21. A sample size of
5±10 mg and a heating rate of 10 8C min21 were used.
Formula
Molecular weight
Temperature
C15H41N9O6S3Co2
657.61
298(2) K
Ê
0.71073 A
Monoclinic
Wavelength
Crystal system
Space group
P21/n
ꢀ
Unit cell dimensions
a ˆ 15:4278ꢀ9† A
ꢀ
b ˆ 8:5463ꢀ5† A
ꢀ
c ˆ 22:4539ꢀ12† A
a ˆ 908
b ˆ 109:198ꢀ1†8
g ˆ 908
Ê 3
Volume
Z
2795.9(3)A
4
Calculated density
m
F(000)
1.562 Mg/m3
1.457 mm21
1376
2.2. Synthesis
Crystal size
u range
Index ranges
0:28 £ 0:24 £ 0:06 mm
1.41 to 26.118
A quantity of 20 mmol (1.94 g) solid KSCN were
dissolved in a 20 cm3 aqueous solution of CoCl2´6H2O
(10 mmol, 2.38 g), and 20 mmol (1.22 g) monoetha-
nolamine were added to this solution slowly with stir-
ring. The resulting solution was stirred for one hour at
room temperature. The polycrystalline precipitate
formed was removed by suction ®ltration and the
dark violet solution was left at room temperature
until evaporation resulted in the formation of violet
crystals suitable for X-ray diffraction analysis. The
crystals were ®ltered off, washed with ethanol and
dried in air. Yield, ca. 87%. Anal. Found: C, 26.31;
H, 6.01; N, 18.23%; C15H41N9O6S3Co2 Calcd: C,
26.40; H, 6.28; N, 18.57%.
219 # h # 18; 27 # k # 10;
227 # l # 24
14,861
Re¯ections collected
Independent re¯ections
Re¯ections observed ꢀ.2s†
Absorption correction
Max. and min. transmission
Re®nement method
5340 ‰Rint ˆ 0:0483Š
3296
Multi-scan
0.916 and 0.672
Full-matrix least-squares on F2
5340/51/372
Data/restraints/parameters
Goodness-of-®t on F2
Final R indices ‰I . 2sꢀI†Š
R indices (all data)
0.870
R1 ˆ 0:0368; wR2 ˆ 0:0696
R1 ˆ 0:0751; wR2 ˆ 0:0783
Ê 23
Largest diff. peak and hole
0.359 and 20.546 e A
As a part of our ongoing research on the synthesis
and spectral, thermal and structural characterization
of plain and mixed ligand complexes of monoethano-
lamine [10±14]; we report here the synthesis, IR
spectra, thermal analysis and single crystal structure
of a new monoethanolamine cobalt complex with
thiocyanate, [Co(meaH)3][Co(mea)(meaH)2](SCN)3,
where meaH and mea are the neutral monoethanola-
mine molecule and monoethanolaminate anions,
respectively.
2.3. Crystal structure analysis
A suitable single crystal was mounted on a glass
®bre with cyanoacrylate glue and data collection was
performed on a BRUKER SMART1000 CCD area
ꢀ
detector using Mo Ka radiation ꢀl ˆ 0:71073 A†:
Intensity data were collected in the u range 1.41±
26.118 at 298(2)K. Crystal data and details of data
collection and re®nement are given in Table 1,
while fractional atomic coordinates with isotropic
displacement parameters are listed in Table 2. An
absorption correction was made using the program
SADABS [15]. The structure was solved by direct-
methods using SHELXS-97 [16] and aniso-
tropic displacement parameters were applied to
non-hydrogen atoms in a full-matrix least-squares
2. Experimental
2.1. Materials and instrumentation
Monoethanolamine (NH2CH2CH2OH), CoCl2´6H2O

V.T. Yilmaz et al. / Journal of Molecular Structure 641 (2002) 119±124
121
re®nement based on F2 using SHELXL-97 [17]. All
the non-H atoms were re®ned anisotropically. The
coordinates of S3A, S3B, S3C, C15A, C15B, C15C,
N9A, N9B and N9C were ®xed and approximate
occupation factors were entered. The H atoms
attached to O1, O2 and O6 were located from differ-
ence map and the other OH hydrogen atoms were
placed in calculated positions. All the hydrogen
were re®ned with a riding model with Uiso 1.2 times
that of their attached atoms. Molecular drawings were
obtained using ORTEPIII [18].
Table 2
Atomic coordinates ( £ 104) and equivalent isotropic displacement
3
Ê 2
parameters (A £ 10 ) for the Co(II) complex of monoethanolamine
Atom
x
y
z
U(eq.)a
Co(1)
Co(2)
O(1)
2782(1)
2406(1)
1674(1)
3479(1)
2972(1)
1539(1)
3388(1)
2478(1)
2017(2)
2645(2)
3921(2)
2274(2)
3345(2)
1414(2)
1135(4)
862(4)
6393(1)
7560(1)
6162(2)
5460(3)
8441(3)
6343(2)
6386(2)
9088(2)
7292(3)
4275(3)
6771(3)
5984(3)
8666(3)
8831(3)
7777(9)
6524(10)
6895(16)
7109(15)
3225(4)
3802(4)
8447(5)
8945(4)
4996(4)
4823(4)
8432(4)
6757(4)
10357(4)
10045(4)
2335(2)
1288(5)
566(4)
1135(1)
2 914(1)
444(1)
35(1)
32(1)
38(1)
41(1)
41(1)
36(1)
34(1)
37(1)
46(1)
44(1)
51(1)
43(1)
42(1)
44(1)
53(2)
47(2)
53(2)
47(2)
53(1)
51(1)
60(1)
51(1)
50(1)
46(1)
50(1)
42(1)
52(1)
51(1)
102(1)
61(1)
72(1)
61(1)
64(1)
129(3)
129(4)
78(1)
60(2)
115(4)
78(1)
59(2)
116(4)
91(2)
60(2)
119(7)
O(2)
O(3)
669(1)
839(1)
O(4)
2 657(1)
2 361(1)
2 277(1)
1580(1)
1396(1)
1822(1)
2 1554(1)
2 1141(1)
2 1447(1)
1081(3)
581(4)
O(5)
O(6)
N(1)
N(2)
N(3)
N(4)
3. Results and discussion
N(5)
3.1. Spectral properties
N(6)
C(1A)
C(2A)
C(1B)
C(2B)
C(3)
The electronic spectrum exhibits intraligand transi-
tions with high intensity in the 200±300 nm range,
while the absorption bands occurred at 541, 737 and
1025(4)
996(8)
1239(5)
566(6)
899(2)
2734(3)
3528(2)
4162(3)
3897(2)
1468(2)
1440(2)
4225(2)
4257(2)
1422(2)
1674(2)
685(1)
851 nm with the
1
values of 566, 86 and
C(4)
714(2)
84 M21 cm21, respectively are attributed to the d±d
transitions, which are consistent with the octahedral
geometry around the Co(II) ion [18].
C(5)
1824(2)
1151(2)
2 1594(2)
2 936(2)
2 623(2)
2 426(2)
2 1139(2)
2 447(2)
1367(1)
1811(2)
2150(2)
2 3970(1)
2 3233(2)
2 2697(5)
C(6)
C(7)
C(8)
The FTIR spectrum of the Co(II) complex of mono-
ethanolamine shows a broad and weak absorption
band centred at 3460 cm21 for the OH stretching
vibration, due to the strong hydrogen bonding [5].
The very sharp bands at 3245 and 3110 cm21 corre-
spond to the n(NH) stretching vibration. This band
shifts by ca. 80 cm21 to the low frequency region
and splits into two bands compared to the free mono-
ethanolamine. These observations clearly indicate
coordination of the amine group of monoethanola-
mine to the Co(II) ion. Splitting of the CH stretching
absorption band observed in the 2800±3000 cm21
region is attributed to the presence of the ethanolate
functional group, which may be due to a partially
deprotonated monoethanolamine ligand. The spec-
trum of the complex presents a strong absorption
bands at 2075 cm21 for the n(CN) vibration and a
medium band at 900 cm21 for the n(CS) vibration
of the SCN anion [19]. The strong and medium
band observed in the 1000±1200 cm21 range are
assigned to the n(CN), n(CC) and n(CO) stretching
vibrations of monoethanolamine [5]. The weak bands
in the 300±600 cm21 region are due to the n(MN) and
n(MO) vibrations [20].
C(9)
C(10)
C(11)
C(12)
S(1)
C(13)
N(7)
1530(3)
2152(3)
1336(1)
1450(3)
1540(9)
S(2)
7615(1)
7718(5)
7782(17)
C(14)
N(8A)
N(8B)
S(3A)
C(15A)
N(9A)
S(3B)
C(15B)
N(9B)
S(3C)
C(15C)
N(9C)
1260(70)
4501
5455
6257
4576
5388
5981
5782
4921
4249
8400(120)
2609
2 2870(40)
2353
2746
3063
2220
2315
2923
2534
2953
2245
2704
3623
2018
2198
2832
2314
2607
2462
a
U(eq.) is de®ned as one third of the trace of the orthogonalized
Uij tensor.

122
V.T. Yilmaz et al. / Journal of Molecular Structure 641 (2002) 119±124
Fig. 1. A labelled drawing of the asymmetric unit of the Co(II) complex of monoethanolamine. Displacement ellipsoids are plotted at the 30%
probability level. The ethylene and amine hydrogen atoms have been omitted for clarity.
3.2. Thermal analysis
The complex does not have a melting point and
Table 3
begins to decompose at 120 8C. The decomposition
Selected bond distances and hydrogen bonding geometry for the
stages between 90 and 388 8C correspond to elimina-
Co(II) complex of monoethanolamine
tion of the monoethanolamine ligands appeared as
Bond lengths
four endotherms at 142, 200, 242 and 265 8C in the
Co1±O1
Co1±O2
Co1±O3
Co1±N1
Co1±N2
Co1±N3
1.904(2)
1.904(2)
1.929(2)
1.939(3)
1.936(3)
1.948(3)
Co2±O4
Co2±O5
Co2±O6
Co2±N4
Co2±N5
Co2±N6
1.925(2)
1.900(2)
1.912(2)
1.930(3)
1.934(3)
1.936(2)
DTA curve. The calculated weight loss for the
removal of the monoethanolamine ligands is 55.2%
and is in good agreement with the experimental value
of 55.6%. The solid intermediate formed after the
removal of the monoethanolamine ligands is
Co(SCN)2, which decomposes in the temperature
range 390±960 8C with a mass loss of 26.4% (calcu-
lated 26.5%) to give metallic cobalt as the ®nal
decomposition product under nitrogen atmosphere.
Bond angles
O1±Co1±O2
O1±Co1±O3
O1±Co1±N1
O1±Co1±N2
O1±Co1±N3
O2±Co1±O3
O2±Co1±N1
O2±Co1±N2
O2±Co1±N3
O3±Co1±N1
O3±Co1±N2
O3±Co1±N3
N1±Co1±N3
N2±Co1±N1
N2±Co1±N3
91.57(9)
90.63(9)
O4±Co2±O5
O4±Co2±O6
O4±Co2±N4
O4±Co2±N6
O4±Co2±N5
O5±Co2±O6
O5±Co2±N6
O5±Co2±N4
O5±Co2±N5
O6±Co2±N5
O6±Co2±N4
O6±Co2±N6
N4±Co2±N5
N4±Co2±N6
N5±Co2±N6
90.14(8)
91.20(9)
85.70(10)
89.54(10)
176.17(11)
90.79(9)
86.12(10)
90.17(10)
175.69(10)
91.95(8)
3.3. Description of the crystal structure
177.09(10)
85.01(10)
88.82(11)
90.27(11)
175.80(11)
85.56(10)
93.97(12)
93.93(12)
94.29(12)
177.30(10)
89.06(10)
85.66(10)
89.91(10)
177.15(11)
85.36(10)
92.83(11)
93.63(11)
94.07(11)
The molecular structure of the complex is shown in
Fig. 1, while Table 3 lists the selected bond lengths
and angles.
The structure of the complex consists of two
complex cations, [Co(meaH)3]21 and [Co(mea)
(meaH)2]1, and three SCN2 anions. Two cations are
very similar and exhibit the same structural features.

V.T. Yilmaz et al. / Journal of Molecular Structure 641 (2002) 119±124
123
Fig. 2. A packing diagram of the unit cell of the Co(II) complex of monoethanolamine showing hydrogen bonding scheme.
In each cation, the Co(II) ion lies on the centre
of symmetry and are octahedrally coordinated by
three monoethanolamine moieties. The [Co(mea)
(meaH)2]1 cation contains two neutral and one depro-
tonated monoethanolamine ligands, while all the
monoethanolamine ligands are the neutral molecules
in the [Co(meaH)3]21 cation. Both the monoethanola-
mine molecule and monoethanolaminate anion act as
bidentate ligands through the amine nitrogen and
ethanol oxygen atoms and form ®ve-membered
chelate rings. The ethylene carbon atoms (C1±C2)
of one of the monoethanolamine ligands are notice-
ably disordered over two positions with the occupan-
cies of 41 and 59%, while all the atoms of the
thiocyanate anion S3±C15±N9 and the N8 atom of
the thiocyanate anion (S2±C14±N8) are extensively
disordered. Both the Co(meaH)3]21 and [Co(mea)
(meaH)2]1 cations show the same coordination and
bond geometry. The Co±N and Co±O bond distances
are in the range 1.928(3)±1.949(3) and 1.899(3)±
A packing diagram with hydrogen bonding scheme
is shown in Fig. 2. The structure exhibits extensive
intra- and intermolecular hydrogen bonds as listed in
Table 4. The two complex cation units form a
hydrogen-bonded dimer of Co(meaH)3]21´´´[Co(mea)
(meaH)2]1 and are held together by three strong O±
H´´´O bonds formed between three ethanolic oxygens
of each complex cation. The hydrogen bonding O´´´O
Ê
distances are signi®cantly short at ca. 2.41(2) A. This
Ê
type of strong hydrogen bonds (2.42 A) was reported
for 1,4,7-tris(hydroxyethyl)-1,4,7-triazacyclononane
containing ethanol groups with ionisable hydrogens
similar to mea [21]. The N and S atoms of the thio-
cyanate anions are involved in weaker hydrogen
bonding with the H atoms of the amine group of the
monoethanolamine ligands. The dimeric units are
connected to each other by the hydrogen bonds
through the SCN2 anions to form a three dimensional
in®nite network.
Ê
1.915(3) A, respectively. The cis angles of the coor-
dination octahedron range from 85.01(10) and
94.29(12)8, while the trans angles are in the range
175.80(10)±177.30(10)8. Therefore, the coordination
geometry around the Co(II) ion is best described as a
distorted octahedron. Bond distances and angles
within the monoethanolamine molecules and the thio-
cyanate anions have expected values.
4. Supplementary data
Crystallographic data (atomic coordinates, atomic
displacement parameters and bond geometries) for the
structure reported in the paper has been deposited with
the Cambridge Crystallographic Data Centre (CCDC)
as supplementary material with a deposition number

124
V.T. Yilmaz et al. / Journal of Molecular Structure 641 (2002) 119±124
Table 4
References
Hydrogen bonding for the Co(II) complex of monoethanolaminea
(Symmetry transformations used to generate equivalent atoms: [#1]
2x, 2y 1 1, 2z; [#2] 2x 1 1/2, y 1 1/2, 2z 1 1/2; [#3] x, y 1 1, z;
[#4] 2x 1 1/2, y 2 1/2, 2z 2 1/2; [#5] 2x 1 1, 2y 1 1, 2z; [#6]
2x 1 1/2, y 1 1/2, 2z 2 1/2; [#7] x 2 1/2, 2y 1 3/2, z 2 1/2; [#8]
2x, 2y 1 1, 2z)
[1] Y. Takahashi, H. Hayashi, Y. Ohya, Mater. Res. Soc. Proc.
271 (1992) 401.
[2] Y. Ohya, Y. Tanaka, H. Takahashi, Jpn. J. Appl. Phys. 32
(1993) 4163.
[3] R.D. Hancock, Inorg. Chim. Acta 49 (1981) 145.
[4] E. Casassas, L.L. Gustems, R. Tauler, J. Chem. Soc. Dalton
Trans. (1998) 569.
D±H´´´A
d(D±H) d(H´´´A) d(D´´´A) , (DHA)
[5] D.G. Brannon, R.H. Morrison, J.L. Hall, G.L. Humphrey,
D.N. Zimmerman, J. Inorg. Nucl. Chem. 33 (1971) 981.
[6] M.S. Masoud, A.M. Hafez, A.E. Ali, Spect. Lett. 31 (1998)
901.
O1±H1´´´O4
1.12
1.16
0.84
0.85
0.85
0.98
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
1.30
1.25
2.11
2.10
2.92
1.45
2.42
2.26
2.48
2.57
2.32
2.63
2.60
3.01
2.04
2.71
2.74
2.37
1.93
2.84
2.59
2.23
2.31
2.94
2.59
2.417(3) 178.2
2.404(3) 173.2
2.741(4) 131.3
2.734(3) 131.5
O2±H2´´´O5
O3±H3´´´N1
O4±H4´´´N6
[7] M.B. Hursthouse, K.J. Izod, M.A. Mazid, P. Thornton, Poly-
hedron 9 (1990) 535.
O4±H4´´´S1 [#1]
O6±H6´´´O3
3.463
123.8
2.432(3) 178.5
3.091(4) 132.0
3.056(4) 147.5
3.285(3) 148.6
3.425(3) 158.4
3.160(3) 155.7
3.431(3) 148.9
3.413(5) 151.3
3.820(3) 151.3
2.886(16) 155.7
3.53(11) 150.6
3.551(3) 150.1
3.252(3) 167.4
2.771(3) 153.8
3.657(3) 152.0
3.408(3) 151.8
3.014(7) 145.0
[8] P. Bombicz, J. Madarasz, E. Forisz, I. Foch, Polyhedron 16
(1997) 3601.
N1±H1A´´´N7 [#2]
N1±H1B´´´N7 [#3]
N2±H2A´´´S3A
N2±H2A´´´S3B
N2±H2A´´´N9C
N2±H2B´´´S1
[9] M. Petric, F. Pohleven, I. Turel, P. Segedin, A.J.P. White, D.J.
Williams, Polyhedron 17 (1998) 255.
[10] V.T. Yilmaz, O. Andac, Y. Topcu, W.T.A. Harrison, Acta
Cryst C57 (2001) 271.
[11] A. Karadag, V.T. Yilmaz, C. Thoene, Polyhedron 20 (2001)
635.
N3±H3A´´´N7 [#2]
N3±H3B´´´S3C
N4±H4A´´´N8A
N4±H4A´´´N8B
N4±H4B´´´S2 [#4]
[12] O. Andac, Y. Topcu, V.T. Yilmaz, W.T.A. Harrison, J. Chem.
Cryst. 30 (2000) 767.
[13] V.T. Yilmaz, Y. Topcu, A. Karadag, Thermochim. Acta 383
(2002) 129.
N5±H5A´´´N9A [#5] 0.90
N5±H5A´´´N9B [#5] 0.90
N5±H5A´´´S3C [#5] 0.90
[14] V.T. Yilmaz, Y. Topcu, F. Yilmaz, C. Thoene, Polyhedron 20
(2001) 3209.
N5±H5B´´´S2 [#6]
N6±H6A´´´N8A
N6±H6A´´´N8B
0.90
0.90
0.90
[15] Bruker, SADABS, SMARTand SAINT, Bruker AXS Inc,
Madison, WI, USA, 1999.
3.15(7)
155.0
[16] G.M. Sheldrick, Acta Cryst. A46 (1990) 467.
[17] G.M. Sheldrick, SHELXL-97. Program for Re®nement of
N6±H6A´´´S3C [#7] 0.90
N6±H6NB´´´S1 [#8] 0.90
3.605(3) 131.8
3.449(3) 159.3
È
Crystal Structures, University of Gottingen, Germany, 1997.
[18] L.J. Farrugia, J. Appl. Cryst. 30 (1997) 565.
[19] A.B.P. Lever, Lever, Inorganic Electronic Spectroscopy,
Elsevier, Amsterdam, 1984.
CCDC 167247. Copies of the data can be obtained,
free of charge, on an application to CCDC, 12 Union
Road, Cambridge CB2 1EZ, UK.
[20] K. Nakamato, Infrared and Raman Spectra of Inorganic and
Coordination Compounds, 5th Ed., Wiley, New York, 1997.
[21] L.R. Luckay, R.D. Hancock, I. Cukrowski, J.H. Reibenspies,
Inorg. Chim. Acta 246 (1996) 159.
Acknowledgements
VTY, OA and AK wish to thank Ondokuz Mayis
University for ®nancial support given to the project.