Zinc iodide complexes of propaneamide, benzamide, dimethylurea, and thioacetamide: syntheses and structures

Article abstract of DOI:10.1002/zaac.200801337

Complexes of zinc iodide with propaneamide EtCONH₂, benzamide BzNH₂, dimethylurea MeNHCONHMe, and thioacetamide MeCSNH₂ have been synthesized and characterized by elemental analyses, vibrational spectra and X-ray diffracti

Full text of DOI:10.1002/zaac.200801337

ARTICLE
DOI: 10.1002/zaac.200801337
Zinc Iodide Complexes of Propaneamide, Benzamide, Dimethylurea, and
Thioacetamide: Syntheses and Structures
Elena V. Savinkina,*[a] Evgeny A. Buravlev,[a] Ilia A. Zamilatskov,[a] Dmitry V. Albov,[b]
Valery V. Kravchenko,[a] Maria G. Zaitseva,[a] and Boris N. Mavrin[c]
Keywords: Amides; Structure elucidation; Coordination modes; Dimethylurea; Zinc
Abstract. Complexes of zinc iodide with propaneamide EtCONH2,
benzamide BzNH2, dimethylurea MeNHCONHMe, and thio-
acetamide MeCSNH2 have been synthesized and characterized by
elemental analyses, vibrational spectra and X-ray diffraction. The
vibrational spectra indicate coordination of amides through oxygen
atoms. The elemental analyses have justified the complexes with the
ZnI2/L ratio of 1:3 for propaneamide and 1:2 for other amides. The
X-ray study has shown that the complexes have different coordi-
nation modes. The complexes of benzamide, dimethylurea, and
thioacetamide are molecular, [ZnL2I2], and the complex of pro-
paneamide is ionic, [ZnL6][ZnI4]. Structures of zinc and cadmium
complexes with various amides are compared.
of the work was to synthesize and study structures of zinc
iodide complexes with propaneamide, benzamide, 1,3-di-
methylurea, and thioacetamide.
Introduction
This work continues the systematic study of 12 group
metal iodide complexes with amides and thioamides [1Ϫ5].
These compounds can be used for the synthesis of the cor-
responding polyiodides [6, 7] and nano-size forms of metals
or metal oxides and sulfides [8, 9].
The zinc iodide complex with acetamide (AA) [Zn(AA)2I2]
and cadmium complexes with thioacetamide (TAA) and
benzamide (BA), [Cd(TAA)2I2] and [Cd(BA)4I2], are molecu-
lar [1, 2, 5], whereas the cadmium iodide complexes with
acetamide and propaneamide (PA) [CdL6][Cd2I6] (L ϭ AA,
PA) are ionic [3]. For the zinc iodide complex with pro-
paneamide, only vibrational spectra were reported [10]. Zinc
iodide forms a molecular complex with urea (Ur) [Zn(Ur)2I2]
[11], and cadmium iodide forms an ionic complex with urea
Experimental Section
Syntheses: Zinc iodide (1 g, 3.13 mmol) and the Ligand L (L ϭ
BA, PA, DMU, TAA) (6.26 mmol) were dissolved in EtOH (for
L ϭ BA) or MeCN (L ϭ PA, DMU, TAA) (10 mL). The solution
was layered on to a liquid perfluorinated hydrocarbon, 1-methyl-
decahydronaphthalene, allowing formation of colorless crystals
(yields were 50, 65, 56, and 40 % for L ϭ PA, BA, DMU, and
TAA, respectively). All complexes were stable in air excluding
[Zn(TAA)2I2], which decomposed within a few hours. M.p.:
[Zn(PA)6][ZnI4], 51.0Ϫ52.5 °C; [Zn(BA)2I2], 124.0Ϫ125.5 °C;
[Cd(Ur)6][CdI3]2 [12] and a molecular complex with 1,3-di- [Zn(DMU)2I2], 114.0Ϫ115.0 °C.
methylurea (DMU) [Cd(DMU)3I2] [4].
Elemental Analysis for the Complexes: [Zn(PA)6][ZnI4] (1076.92):
The variability of coordination modes and structures of
metal iodide complexes with amides stimulated further syn-
thesis of new complexes with relative ligands. The purpose
calcd C 19.96, H 3.88, N 7.76, Zn 12.01; found C 18.97, H 2.98,
N 7.34, Zn 12.88. [Zn(BA)2I2] (561.44): calcd. C 28.52, H 2.38, N
4.75, Zn 11.65; found C 28.72, H 2.92, N 4.85, Zn 11.98.
[Zn(DMU)2I2] (495.40): calcd. Zn 13.13, C 14.55, N 11.31, H 3.23;
found C 14.87, H 3.27, N 12.08, Zn 12.95.
[Zn(PA)6][ZnI4] is soluble in H2O, EtOH, Me2CO, and MeCN;
[Zn(BA)2I2] is soluble in EtOH and Me2CO, poorly soluble in H2O,
and insoluble in CHCl3; [Zn(DMU)2I2] is soluble in H2O, EtOH,
and Me2CO, insoluble in CHCl3; [Zn(TAA)2I2] is soluble in H2O,
EtOH, Me2CO, and MeCN, insoluble in CHCl3. Specific conduc-
tivities (measured with a OK 102/1 conductometer) of 0.001 
aqueous solutions of [Zn(BA)2I2] and [Zn(DMU)2I2] (85 and 435
µS·cmϪ1) indicated that [Zn(BA)2I2] is stable, while [Zn(DMU)2I2]
decomposed under dissolution in water.
* Dr. E. V. Savinkina
Fax: ϩ7-495-4348711
E-Mail: e.savinkina@mail.ru
[a] Lomonosov Academy of Fine Chemical Technology,
Vernadskogo 86
117571, Moscow, Russian Federation
[b] Department of Chemistry
Moscow State University,
119992, Moscow, Russian Federation
[c] Institute of Spectroscopy
Russian Academy of Sciences,
Troitsk, Russian Federation
X-ray Diffraction: Details of the X-ray analysis are summarized in
Table 1.
Supporting information for this article is available on the
WWW under www.zaac.wiley-vch.de or from the author.
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Zinc IodideϪAmide Complexes: Syntheses and Structures
Table 1. Crystallographic characteristics, experimental details, and refinement parameters for the structures of [Zn(PA)6][ZnI4] (I),
[Zn(DMU)2I2] (II), [Zn(BA)2I2] (III), and [Zn(TAA)2I2] (IV).
Parameter
I
II
III
IV
Formula weight
Crystal system
Space group
2153.83
triclinic
P1
495.40
561.44
monoclinic
P21/c
0.1 ϫ 0.1 ϫ 0.1
8.458(4)
15.174(6)
14.294(5)
90
98.25(3)
90
1815.5
4
469.43
monoclinic
P21/c
0.4 ϫ 0.4 ϫ 0.4
7.551(4)
23.518(13)
7.814(5)
90
114.03(5)
90
1267.3
4
triclinic
¯
¯
P1
Crystal size /mm
0.1 ϫ 0.1 ϫ 0.1
10.8300(62)
18.3901(34)
19.0861(38)
93.498(15)
94.103(36)
92.090(36)
3799.7
0.1 ϫ 0.1 ϫ 0.1
7.122(3)
8.310(4)
12.868(6)
83.61(4)
79.18(4)
80.72(4)
735.7
˚
a /A
˚
b /A
˚
c /A
Ͱ /deg
β /deg
γ /deg
3
˚
V /A
Z
2
2
T /K
293(2)
1.883
0.71073
1.07Ϫ24.99
4.546
293(2)
2.236
0.71073
1.62Ϫ27.97
5.856
293(2)
2.054
1.54180
4.27Ϫ69.91
28.623
1056
293(2)
2.460
0.71073
1.73Ϫ26.00
7.094
dc /mg·mϪ3
˚
λ /A
θ Range
µ /mmϪ1
F (000)
2048
464
864
Reflns. collected
Reflns. unique
R, all data
10186
4952
0.1419
0.0686
0.1902
0.1555
0.935
Ϫ1.007
1.023
3532
3007
3246
2770
2484
1683
0.0415
0.0340
0.0887
0.0851
1.017
Ϫ0.748
0.868
0.0762
0.0704
0.1867
0.1792
1.057
Ϫ1.235
2.726
0.0861
0.0568
0.1519
0.1354
0.956
Ϫ1.144
1.603
R, I > 2σ (I)
wR, all data
wR, I > 2σ (I)
Goodness-of-fit on F2
Ϫ3
˚
˚
∆ρmin /e·A
Ϫ3
∆ρmax /e·A
Crystallographic data for the structure(s) have been deposited with
the Cambridge Crystallographic Data Centre under CCDC-695546
(I), -695546 (II), -695547 (III), -695544 (IV). Copies of the data can
be obtained free of charge on application to The Director, CCDC,
12 Union Road, Cambridge CB2 1EZ, UK [Fax: ϩ44-1223-336-
033; E-Mail for inquiry: fileserv@ccdc.cam.ac.uk; E-Mail for depo-
sition: deposit@ccdc.cam.ac.uk].
The experimental intensities of the diffraction reflections were col-
lected at room temperature with
a CAD-4 automated dif-
fractometer (Cu-Kα or Mo-Kα, graphite monochromator, non-pro-
filed ω scans, γ scan absorption correction). The structures were
solved by the direct method and refined by the full-matrix least-
squares technique against F2 in the anisotropic approximation for
non-hydrogen atoms. The positions of hydrogen atoms were calcu-
lated and refined in an isotropic approximation in a riding model.
All calculations were performed using SHELXS-97 and SHELXL-
97 [13].
Spectra: IR spectra were recorded with Infralum FT-02
(500Ϫ4000 cmϪ1, nujol mulls) and Bruker EQUINOX 55/SB
(400Ϫ4000 cmϪ1, KBr pellets) spectrometers at room temperature.
˚
Figure 1. [Zn(PA)6][ZnI4]. Selected bond lengths /A and bond
angles /°: Zn(1)ϪI(4) 2.593(2), Zn(1)ϪI(3) 2.602(2), Zn(1)ϪI(2)
2.6142(19),
Zn(1)ϪI(1)
2.631(2),
Zn(3)ϪO(7)
2.066(9),
Zn(3)ϪO(13) 2.082(9), Zn(3)ϪO(16) 2.090(9), Zn(3)ϪO(4)
Raman spectra were excited by a 1064 nm Nd:YAG laser radiation
at room temperature and recorded using a Bruker Fourier-Raman
spectrometer RFS 100/S (80Ϫ3000 cmϪ1) with the resolution of
2.092(9),
I(4)ϪZn(1)ϪI(3)
I(3)ϪZn(1)ϪI(2)
I(3)ϪZn(1)ϪI(1)
O(7)ϪZn(3)ϪO(13)
O(13)ϪZn(3)ϪO(16)
O(13)ϪZn(3)ϪO(4)
Zn(3)ϪO(10)
2.095(9),
Zn(3)ϪO(1)
2.097(9);
110.92(8),
108.77(8),
105.94(7),
85.0(4),
91.7(4),
174.8(4),
111.03(7),
113.67(8),
106.15(7),
91.1(4),
90.9(4),
93.1(4),
I(4)ϪZn(1)ϪI(2)
I(4)ϪZn(1)ϪI(1)
I(2)ϪZn(1)ϪI(1)
O(7)ϪZn(3)ϪO(16)
O(7)ϪZn(3)ϪO(4)
O(16)ϪZn(3)ϪO(4)
2 cmϪ1
.
Results
O(7)ϪZn(3)ϪO(10) 175.9(3), O(13)ϪZn(3)ϪO(10) 86.5(4),
Crystal Structures
O(16)ϪZn(3)ϪO(10)
O(7)ϪZn(3)ϪO(1)
O(16)ϪZn(3)ϪO(1)
91.8(4),
90.0(4),
92.0(4),
O(4)ϪZn(3)ϪO(10)
O(13)ϪZn(3)ϪO(1)
O(4)ϪZn(3)ϪO(1)
91.7(4),
176.9(4),
84.0(4),
The crystal of [Zn(PA)6][ZnI4] is built from the
[Zn(PA)6]2ϩ and [ZnI4]2Ϫ ions. The zinc atom is octa- O(10)ϪZn(3)ϪO(1) 92.6(4).
Z. Anorg. Allg. Chem. 2009, 1458Ϫ1462
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E. V. Savinkina, E. A. Buravlev, I. A. Zamilatskov, D. V. Albov, V. V. Kravchenko, M. G. Zaitseva, B. N. Mavrin
ARTICLE
hedrally coordinated by oxygen atoms of the ligand in the
cation and tetrahedrally coordinated by iodine atoms in the
anion (Figure 1).
In both independent cations, five propaneamide ligands
are planar with respect to the metal (the MϪOϪCϪN tor-
sion angles < 17°); while the sixth ligand is essentially non-
planar (the MϪOϪCϪN torsion angles are 44.90 and
46.51°). This is not typical for transition metal complexes
of amides [14]. In contrast to the zincϪacetamide complex
[1], where three of four independent ligands have nitrogen
atoms in trans-positions to the metal atom, in
[Zn(PA)6][ZnI4], the metal lying in the amide plane is always
cis to N. The cation is stabilized by six intermolecular
NϪH···O hydrogen bonds. Every iodine atom in the anion
is involved in short NϪH···I contacts with adjacent cations.
The crystals of [ZnL2I2] (L ϭ BA, DMU) are built of the
corresponding molecular complexes (Figure 2, Figure 3).
The zinc atom is tetrahedrally coordinated by two oxygen
atoms of two amide ligands and two iodine atoms. The
ZnϪO and ZnϪI bonds in the benzamide and 1,3-dimeth-
ylurea complexes are slightly shorter than in the propane-
amide complex. In the planar ZnϪOϪCϪN groups (the tor-
sion angle < 9°) of [Zn(BA)2I2], the metal is always cis to N.
The structure of each complex is stabilized by a single
intramolecular NϪH···O hydrogen bond. All iodine atoms
are involved in short NϪH···I contacts with adjacent mol-
ecules. Both structures are layered.
˚
Figure 3. [Zn(DMU)2I2]. Selected bond lengths /A and bond
angles /°: Zn(1)ϪO(1) 1.958(3), Zn(1)ϪO(2) 1.986(3), Zn(1)ϪI(1)
2.5572(15), Zn(1)ϪI(2) 2.5668(12), O(1)ϪZn(1)ϪO(2) 101.23(13),
O(1)ϪZn(1)ϪI(1) 108.76(12), O(2)ϪZn(1)ϪI(1) 109.91(11),
O(1)ϪZn(1)ϪI(2) 111.24(11), O(2)ϪZn(1)ϪI(1) 110.84(10),
I(1)ϪZn(1)ϪI(2) 114.08(4).
contact, forming infinite layer. The layers are combined in
a 3D-structure by the CϪH···S short contacts. The struc-
ture is similar to [Zn(TAA)2Cl2] [16].
˚
Figure 4. [Zn(TAA)2 I2]. Selected bond lengths /A and bond
angles /°: I(1)ϪZn(1) 2.5780(19), I(2)ϪZn(1) 2.5782(19),
Zn(1)ϪS(1) 2.339(2), Zn(1)ϪS(2) 2.352(3); S(1)ϪZn(1)ϪS(2)
97.35(10), S(1)ϪZn(1)ϪI(1) 113.87(9), S(2)ϪZn(1)ϪI(1) 112.16(9),
S(1)ϪZn(1)ϪI(2)
112.23(9),
S(2)ϪZn(1)ϪI(2)
111.92(9),
I(1)ϪZn(1)ϪI(2) 109.00(7).
˚
Figure 2. [Zn(BA)2I2]. Selected bond lengths /A and bond angles /°:
Zn(1)ϪO(1) 1.954(5), Zn(1)ϪO(2) 2.026(5), Zn(1)ϪI(1) 2.5316(10),
IR and Raman Spectra
Zn(1)ϪI(2)
O(1)ϪZn(1)ϪI(2) 110.31(19), O(2)ϪZn(1)ϪI(2) 111.51(18),
O(1)ϪZn(1)ϪI(1) 109.6(2), O(2)ϪZn(1)ϪI(1) 105.51(18),
I(1)ϪZn(1)ϪI(2) 119.84(4).
2.5273(11);
O(1)ϪZn(1)ϪO(2)
97.7(2),
Vibrational spectra of the zinc iodide complex with pro-
paneamide are discussed in [10]. Shifts of the main bands
indicate that propaneamide ligand is bounded to zinc
through the amide oxygen.
The structure of [Zn(DMU)2I2] differs drastically from
In the 50Ϫ300 cmϪ1 range, four modes of the tetrahedral
[Zn(DMU)6](ClO4)2, which is built of [Zn(DMU)6]2ϩ [ZnI4]2Ϫ ion are active in Raman spectra: ν1(A1), ν2(E),
Ϫ
cations and ClO4 counterions [15].
ν3(F2), ν4(F2) [17]. The Raman spectrum of [Zn(PA)6][ZnI4]
The crystal of [Zn(TAA)2I2] has the similar structure reveals strong bands at 120 cmϪ1 (ν1) and 172 cmϪ1 (ν3).
(Figure 4). The metal lies in the thioacetamide planes (the The intensity ratio agrees with literature data: ν3 > ν1 [17].
ZnϪSϪCϪN torsion angles are 1.54° and 3.59°) and is cis The bands below 100 cmϪ1 (ν2 and ν4) overlap with the
to nitrogen. No intramolecular hydrogen bonds are found laser band.
in the complex molecule. One iodine atom is involved in
The full vibrational analysis of crystalline DMU has been
two NϪH···I short contact, and another, in one CϪH···I published [18]. To elucidate the shifts of the ν(CϪO) and
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Zinc IodideϪAmide Complexes: Syntheses and Structures
δas(NϪH) bands, IR spectra of the deuterated complex was [Zn(DMA)2I2] [20]. In the zinc iodide complexes of dimeth-
recorded. Table 2 gives diagnostic IR and Raman bands of ylurea and benzamide [ZnL2I2], the coordination number
the free ligand and its complex with zinc iodide. Assign- (CN) for zinc is also 4, whereas CNs for cadmium in
ments in Table 2 have been given in comparison with the [Cd(DMU)3I4] [4] and [Cd(BA)4I2] [5] are 5 and 6, respec-
data obtained for the uncoordinated DMU [18] and its co- tively. Both zinc and cadmium complexes with propaneam-
balt complexes [19]. In the IR and Raman spectra of ide are ionic, differing by the complex anion ([ZnI4]2Ϫ and
[Zn(DMU)2I2], the frequency of the CϭO stretching mode [Cd2I6]2Ϫ [3], respectively). Summary of all reported data
decreases as compared to the spectra of the free ligand indi- on the structures of zinc and cadmium iodides with relative
cating coordination of the ligand through the oxygen atom. ligands allows discussing effects of various factors on com-
Upon coordination through oxygen, the positively charged plex formation.
metal ion stabilizes the negative charge on the oxygen atom;
Combination of inductive and mesomeric effects in-
the NϪCϭO group now occurs in its polar resonance form creases donating ability of the oxygen atom in the row
and the double bond character of the CϪN bond increases, BA ഠ DMU ഠ DMA < Ur ഠ AA < PA. According to
while the double bond character of the CϭO bond de- this row, high donating ability of propaneamide allows it to
creases, resulting in an increase of the CϪN stretching fre- substitute all iodine atoms in the inner sphere of both zinc
quency with a decrease in the CϭO stretching frequency and cadmium central atoms resulting in formation of ionic
[17]. Increase of the frequencies of the NϪH stretching complexes (Table 3). Acetamide and urea ligands substitute
mode is caused by rearrangement of electron density in the iodine atoms in the inner sphere of the softer cadmium
ligand molecules.
atom and form the inner sphere along with the iodine atoms
in the complexes of the harder zinc atom. Neither dimeth-
ylurea, nor benzamide substitute iodine atoms in the inner
spheres of both zinc and cadmium atoms. These ligands
Table 2. IR/Raman spectra of DMU and deuterated DMU and
their zinc iodide complexes.
Assignment DMU
νs(NϪH) 3360
νas(NϪH) 3348/3339
[Zn(DMU)2I2] [D2]DMU [Zn([D2]DMU)I2] form molecular complexes with both central atoms. Di-
methylacetamide forms similar molecular complex with
zinc iodide.
3368/3373
2496
2482
1627
1517
1336
1165
2518
2491
1580
1559
1369
1162
ν(CϪO)
δas(NH)
1627/1621 1581/1591
1591
1612/1602
1270/1284
Table 3. Zinc and cadmium iodide complexes with amides.
νas(CϪN) 1270
νs(NϪR)
νas(NϪR) 1040
1175/1191 1174/1179
1042/1048
931/930 896/899
775
702
Ligand
Zinc complex
Cadmium complex
1027, 982 1044, 953
950, 917 882
765
679
473
νs(CϪN)
π(CϪO)
δ(CϪO)
δ(NCN)
ν(MϪO)
Propaneamide (PA)
Acetamide (AA)
Urea (Ur)
[Zn(PA)6][ZnI4]
[Zn(AA)2I2] [2]
[Zn(Ur)2I2] [11]
[Cd(PA)6][Cd2I6] [3]
[Cd(AA)6][Cd2I6] [3]
[Cd(Ur)6][CdI3] [12]
[Cd(DMU)3I2] [4]
763
762
641
496/508
1,3-Dimethylurea (DMU) [Zn(DMU)2I2]
552
Dimethylacetamide (DMA) [Zn(DMA)2I2] [20] no data
Benzamide (BA)
Thioacetamide (TAA)
Thiourea (TUr)
[Zn(BA)2I2]
[Zn(TAA)2I2]
no data
[Cd(BA)4I2] [1]
[Cd(TAA)2I2] [5]
[Cd(TUr)2I2] [21]
Similar shifts of principle bands were found in the IR
spectrum of the benzamide complex. The Raman spectrum
of benzamide does not change significantly on com-
plexation.
Differences in CN seem to be caused by steric factors.
Zinc shows CN 4, when its coordination sphere contains
large iodine atoms. If it is coordinated by oxygen atoms
only, its CN increases up to 6. Cadmium shows CN 4 only
in the [Cd2I6]2Ϫ anion. If cadmium is coordinated by oxy-
gen atoms, its CN increases up to 5 in the complex of di-
methylurea and 6 in complexes of BA, Ur, AA, and PA.
Although the dimethylurea molecule is not larger than the
benzamide or propaneamide molecule, it has a fork just
nearby the donating atom producing steric hindrances.
For thioamides, inductive and mesomeric effects are of
less importance. In the zinc iodide and cadmium iodide
complexes of thioacetamide [2] and cadmium iodide com-
plex of thiourea (TUr) [Cd(TUr)2I2] [21], soft sulfur and
iodine atoms are equal when forming the inner sphere.
Large size of the iodine and sulfur atoms results in CN 4
for the complexes of thioacetamide and thiourea.
From nine bands, which are active for molecular com-
plexes [ZnL2I2], several bands were found in the Raman
spectra of the complexes. The bands at 119, 150, 170, and
201 cmϪ1 in the spectrum of [Zn(DMU)2L2] are assigned
to the ZnϪI vibration modes, and the bands at 515, 570,
and 650 cmϪ1 are assigned to the ZnϪO vibration modes.
In the spectrum of [Zn(BA)2I2], these bands are found at
122, 145, 155, 189, and 428 cmϪ1
.
Vibrational spectra of [Zn(TAA)2I2] were not studied be-
cause the compound decomposed under sampling.
Discussion
The zinc iodide complex of thioacetamide is similar to
the cadmium iodide complex of the same ligand [2]. Both
complexes are molecular with the tetrahedral coordination
of the central atom. Similar structure was reported for the
Supporting Information (see footnote on the first page of this
dimethylacetamide (DMA) complex from zinc iodide article): Positional and thermal displacement parameters for IϪIV.
Z. Anorg. Allg. Chem. 2009, 1458Ϫ1462
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E. V. Savinkina, E. A. Buravlev, I. A. Zamilatskov, D. V. Albov, V. V. Kravchenko, M. G. Zaitseva, B. N. Mavrin
ARTICLE
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Acknowledgement
The authors are indebted to the Russian Foundation for Basic
Research for covering the license fee for use of the Cambridge Struc-
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