catena-Poly[[silver(I)-μ-ethane-1,2-diamine-κ2 N:N′] 3-fluorobenzoate monohydrate]

Article abstract of DOI:10.1107/S0108270103028683

The title compound, {[Ag(C₂H₈N₂)] (C₇H₄FO₂)·H₂O}_n, has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Ag atom is bicoordinated in a linear configuration by two N atoms from two symmetry-related ethylenediamine ligands, giving linear polymeric chains with [-Ag-N-C-C-N-]_n backbones running parallel to the b axis. In the crystal packing, these linear chains are interconnected by N-H...O and O-H...O hydrogen bonds, and by weak Ag...OW interactions, forming layers parallel to the ab plane.

Full text of DOI:10.1107/S0108270103028683

metal-organic compounds
Acta Crystallographica Section C
Crystal Structure
Communications
ISSN 0108-2701
catena-Poly[[silver(I)-l-ethane-1,2-
diamine-j2N:N0] 3-fluorobenzoate
monohydrate]
Zhong-Lu You,a,b Li Yang,a Ying Zou,a Wei-Jie Zeng,a
Wei-Sheng Liub and Hai-Liang Zhua,b
*
aDepartment of Chemistry, Fuyang Normal College, Fuyang, Anhui 236041, People's
Republic of China, and bDepartment of Chemistry, Lanzhou University, Lanzhou
730000, People's Republic of China
Correspondence e-mail: hailiang_zhu@163.com
Figure 1
The structure of (I), showing the atom-numbering scheme. Displacement
ellipsoids are drawn at the 30% probability level and H atoms are shown
as small spheres of arbitrary radii.
Received 9 December 2003
Accepted 12 December 2003
Online 10 February 2004
The title compound, {[Ag(C2H8N2)](C7H4FO2)ÁH2O}n, has
been synthesized and characterized by elemental analysis and
single-crystal X-ray diffraction. The Ag atom is bicoordinated
in a linear con®guration by two N atoms from two symmetry-
related ethylenediamine ligands, giving linear polymeric
chains with [±AgÐNÐCÐCÐN±]n backbones running
parallel to the b axis. In the crystal packing, these linear
chains are interconnected by NÐHÁ Á ÁO and OÐHÁ Á ÁO
hydrogen bonds, and by weak AgÁ Á ÁOW interactions, forming
layers parallel to the ab plane.
these silver(I) carboxylates, the title novel complex, (I), is
reported here.
Complex (I) is a polymeric ethylenediamine±silver(I)
complex. The smallest repeat unit for the complex contains an
ethylenediamine±silver(I) cation, a 3-¯uorobenzoate anion
and a lattice water molecule (see scheme). In the cation, the
AgI atom is in a linear coordination environment and is
bicoordianted by two N atoms from different ethylenediamine
ligands. The N1ÐAg1ÐN2 angle is 170.50 (11)ꢀ, indicating a
signi®cantly distorted linear geometry for atom Ag1, which is
comparable with the value of 172.37 (8)ꢀ observed in a similar
silver complex (Zhu, Liu et al., 2003). The average AgÐN
Ê
bond length is 2.148 (3) A, which is a little longer than the
Comment
Ê
value of 2.138 (2) A observed in the related complex
Silver(I) complexes with carboxylate anions as counter-ions or
ligands are a group of metal compounds which, due to their
wide usage in many ®elds, have been structurally characterized
for 30 years (Graham et al., 1996; Kristiansson, 2001; Nomiya
et al., 2000; Pingrong et al., 1998). Recently, we have reported a
few dozen silver(I)±carboxylate complexes with various
described above. In the anion, the dihedral angle between the
benzene ring and the plane formed by the carboxylate group
amines and imines, all of which have been structurally char-
acterized (Usman et al., 2003; Zhu et al., 1999, 2000; Zhu,
Usman et al., 2003; Zhu, Zhang et al., 2003; Zheng, Tong, Zhu
& Chen, 2001; Zheng, Tong, Zhu, Fang & Chen, 2001). As an
extension of our work on the structural characterization of
Figure 2
The crystal packing of (I), viewed along the c axis. H atoms have been
omitted for clarity.
Acta Cryst. (2004). C60, m117±m118
DOI: 10.1107/S0108270103028683
# 2004 International Union of Crystallography m117

metal-organic compounds
(O1/C7/O2) is 9.4 (5)ꢀ. The C6ÐC5ÐC7ÐO2 and C4ÐC5Ð
Table 1
Hydrogen-bonding geometry (A, ).
ꢀ
Ê
C7ÐO1 torsion angles are
171.1 (4) and
170.2 (4)ꢀ,
respectively. Atom F1 lies in the plane of the phenyl ring.
The AgÐN bonds link the amine molecules and the AgI
atoms to form a chain along the b axis. Coordinatoin is
increased to three by the water atom O1W at a distance of
DÐHÁ Á ÁA
DÐH
HÁ Á ÁA
DÁ Á ÁA
DÐHÁ Á ÁA
O1WÐH1WAÁ Á ÁO2i
O1WÐH1WBÁ Á ÁO1ii
N1ÐN1BÁ Á ÁO1i
0.85
0.85
0.90
0.90
0.90
0.90
1.95
1.96
2.25
2.15
2.13
2.08
2.739 (4)
2.731 (4)
3.126 (4)
2.958 (4)
2.964 (4)
2.941 (4)
154
150
165
149
154
160
N2ÐH2AÁ Á ÁO2iii
N1ÐH1AÁ Á ÁO2
Ê
2.611 (4) A, leading to a T-shaped con®guration at Ag1. If the
longer Ag1Á Á ÁO1W(12 x; 21 y; 1 z) contact of 2.993 (4) A
Ê
N2ÐH2CÁ Á ÁO1
Symmetry codes: (i)
is also considered, coordination is further increased to four,
giving Ag2O2 tetragons, as shown in Fig. 2. The tetragons link
the chains to form layers along the ab direction.
x; 32 y; 1 z; (ii) 12 x; 12 y; 1 z; (iii) x; y 1; z.
1
2
The 3-¯uorobenzoate anions in (I) are located among the
chains, their carboxylate-group ends linking to the chains
through N1ÐH1AÁ Á ÁO1i and N1ÐH1BÁ Á ÁO2ii hydrogen
bonds. In addition, there are O1WÐH1WAÁ Á ÁO1i and O1WÐ
H1WBÁ Á ÁO2i hydrogen bonds between the water molecules
and the carboxylate groups.
All H atoms were placed in geometrically idealized positions and
Ê
constrained to ride on their parent atoms, with NÐH = 0.90 A,
Ê
CÐH = 0.96 A and OÐH = 0.85 A, and with Uiso(H) values ®xed at
Ê
2
0.08 A . The Ueq value for the F atom is large, but no attempt was
Ê
made to split it.
Data collection: SMART (Siemens, 1996); cell re®nement:
SMART; data reduction: SAINT (Siemens, 1996); program(s) used to
solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to
re®ne structure: SHELXL97 (Sheldrick, 1997a); molecular graphics:
SHELXTL (Sheldrick, 1997b); software used to prepare material for
publication: SHELXTL.
Experimental
All reagents and solvents were used as obtained without further
puri®cation. Silver 3-¯uorobenzoate (0.5 mmol, 124 mg) and 1,2-di-
aminoethane (0.5 mmol, 30 mg) were dissolved in an ammonia
solution (10 ml, 30%). The mixture was stirred for about 10 min at
room temperature to give a clear colourless solution. The resulting
solution was kept in air and, after slow evaporation of the solvent
over a period of 2 d, large colourless crystals of (I) formed at the
bottom of the vessel. The crystals were isolated, washed three times
with water and dried in a vacuum desiccator using CaCl2 (yield
85.2%). Analysis found: C 33.21, H 4.39, N 8.55%; calculated for
C9H14AgFN2O3: C 33.25, H 4.34, N 8.62%.
The authors thank the Education Of®ce of Hubei Province,
People's Republic of China, for research grant No.
2002B29002, and the Natural Science Foundation of Hubei
Province, People's Republic of China, for research grant No.
2003ABB010.
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: NA1632). Services for accessing these data are
described at the back of the journal.
Crystal data
References
[Ag(C2H8N2)](C7H4FO2)ÁH2O
Mo Kꢁ radiation
Cell parameters from 4521
re¯ections
Mr = 325.09
Monoclinic, C2=c
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Ê
a = 23.721 (5) A
1
Ê
b = 7.1800 (10) A
ꢃ = 1.73 mm
T = 293 (2) K
Ê
c = 13.961 (3) A
ꢀ = 100.45 (3)ꢀ
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Ê
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Re®nement
Re®nement on F2
R[F2 > 2ꢄ(F2)] = 0.040
wR(F2) = 0.091
S = 1.07
2372 re¯ections
w = 1/[ꢄ2(Fo2) + (0.0446P)2]
where P = (Fo2 + 2Fc2)/3
(Á/ꢄ)max = 0.001
3
Ê
Áꢅmax = 0.54 e A
3
Ê
0.56 e A
Áꢅmin
=
145 parameters
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ꢁ
m118 Zhong-Lu You et al.
[Ag(C2H8N2)](C7H4FO2)ÁH2O
Acta Cryst. (2004). C60, m117±m118