metal-organic papers
m1106
Houet al. [Ag(C2H3N)(C21H15N3)]PF6C2H3N DOI: 10.1107/S1600536804016472 Acta Cryst.(2004). E60, m1106±m1107 Acta Crystallographica Section EStructure Reports
Online
ISSN 1600-5368
(Acetonitrile-
j
N
)(4
000-phenyl-2,2
000:6
000,2
000000-ter-pyridine-
j
3N
)silver(I) hexafluorophosphate
acetonitrile solvate
Lei Hou,aDan Li,a* Ye-Gao Yin,a
Tao Wuaand Seik Weng Ngb
aDepartment of Chemistry, Shantou University,
Shantou, Guangdong 515063, People's Republic of China, andbDepartment of
Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: dli@stu.edu.cn
Key indicators Single-crystal X-ray study
T= 295 K
Mean(C±C) = 0.009 AÊ
Rfactor = 0.057
wRfactor = 0.178
Data-to-parameter ratio = 13.0
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
#2004 International Union of Crystallography Printed in Great Britain ± all rights reserved
In the title complex, [Ag(C2H3N)(C21H15N3)]PF6CH3CN, the
AgIatom is coordinated by a tridentate chelating 40
-phenyl-2,20:60,200-terpyridine ligand and an acetonitrile molecule, to
form a distorted square-planar geometry.
Comment
We have previously demonstrated that 40-phenyl-2,20:60,200
-terpyridine acts as a chelating tridentate ligand when coordi-nating to CuI, to form a ®ve-coordinate copper complex (Feng
et al., 2002). In this work, the ligand is used to coordinate to AgI, giving the title complex, (I).
In complex (I) (Fig. 1), the Ag centre is coordinated by three N atoms from the 40-phenyl-2,20:60,200-terpyridine ligand
and an N atom of the acetonitrile, showing an essentially square-planar geometry with constraints imposed by the
Received 29 June 2004 Accepted 6 July 2004 Online 17 July 2004
Figure 1
40-phenyl-2,20:60,200-terpyridyl ligand. The sum of the angles
about the Ag atom is 360.0.
It has been shown that 2,20:60,200-terpyridine-analogue
ligands and AgI form a series of dinuclear and polynuclear
moleculesviaAg Ag interactions. The anions and solvents, and the additional steric constraints of the substituents, are some of the factors which in¯uence the coordination and aggregation architecture of AgI±terpyridine systems (Baumet
al., 1998; Constableet al., 1998; Hannon et al., 2002). In the present study, a donor solvent, CH3CN, was used. It is not
surprising that only a mononuclear AgIcomplex was obtained.
Experimental
The 40-phenyl-2,20:60,200-terpyridine ligand was synthesized according
to the method of Constable et al. (1990). To an acetone solution (10 ml) of AgPF6(0.0253 g, 0.1 mmol) was added 40-phenyl-2,20:60,200 -terpyridine (0.0390 g, 0.1 mmol). A yellow precipitate was formed after stirring for 3 h and this was isolated by ®ltration. A solution of the resulting solid in acetonitrile was allowed to stand for 5 d and yellow prismatic crystals of (I) were obtained (yield 55%).
Crystal data
[Ag(C2H3N)(C21H15N3)]PF6C2H3N
Mr= 644.31
Monoclinic, P21=n a= 16.777 (1) AÊ
b= 7.8257 (6) AÊ
c= 19.447 (1) AÊ
= 90.356 (2)
V= 2553.2 (3) AÊ3
Z= 4
Dx= 1.676 Mg mÿ3
MoKradiation Cell parameters from 1971
re¯ections
= 2.4±20.3
= 0.92 mmÿ1
T= 295 (2) K Prism, yellow 0.200.180.12 mm Data collection
Bruker APEX CCD area-detector diffractometer
'and!scans
Absorption correction: multi-scan (SADABS; Bruker, 2002)
Tmin= 0.354,Tmax= 0.898 12 897 measured re¯ections
4488 independent re¯ections 3262 re¯ections withI> 2(I)
Rint= 0.038
max= 25.0
h=ÿ17!19
k=ÿ9!9
l=ÿ20!23 Re®nement
Re®nement onF2
R[F2> 2(F2)] = 0.057
wR(F2) = 0.178
S= 1.06 4488 re¯ections 345 parameters
H-atom parameters constrained
w= 1/[2(F
o2) + (0.0996P)2
+ 1.6223P]
whereP= (Fo2+ 2Fc2)/3
(/)max= 0.001
max= 1.06 e AÊÿ3
min=ÿ0.42 e AÊÿ3
Table 1
Selected geometric parameters (AÊ,).
Ag1ÐN1 2.348 (5)
Ag1ÐN2 2.378 (4) Ag1ÐN3Ag1ÐN4 2.470 (5)2.187 (6)
N1ÐAg1ÐN2 69.3 (1)
N1ÐAg1ÐN3 136.4 (2)
N1ÐAg1ÐN4 127.2 (2)
N2ÐAg1ÐN3 67.1 (2)
N2ÐAg1ÐN4 163.4 (2)
N3ÐAg1ÐN4 96.4 (2)
The reported transmission factors are those calculated by SADABS(Bruker, 2002), which treats other effects simultaneously with absorption as part of the interframe scaling process. H atoms were placed in calculated positions [CÐH = 0.93 AÊ andUiso(H) = 1.2Ueq(C) for phenyl H atoms, and CÐH = 0.96 AÊ andUiso(H) = 1.5Ueq(C) for methyl H atoms], and were included in the re®nement in the riding-model approximation. The methyl groups were allowed to rotate as rigid groups. The ®nal difference map had a signi®cant peak near atom F3, but was otherwise featureless.
Data collection:SMART(Bruker, 2002); cell re®nement:SAINT (Bruker, 2002); data reduction:SAINT; program(s) used to solve structure:SHELXS97 (Sheldrick, 1997); program(s) used to re®ne structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication:SHELXL97.
The authors thank the National Natural Science Foundation of China (grant Nos. 20271031 and 29901004), the Natural Science Foundation of Guangdong Province (grant No. 021240) and the University of Malaya for supporting this study.
References
Baum, G., Constable, E. C., Fenske, D., Housecrofe, C. E. & Kulke, T. (1998).
Chem. Commun.pp. 2659±2660.
Bruker (2002).SADABS,SMARTandSAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Constable, E. C., Edwards, A. J., Haire, G. R., Hannon, M. J. & Raithby, P. R. (1998).Polyhedron,17, 243±253.
Constable, E. C., Lewis, J., Liptrot, M. C. & Raithby, P. R. (1990).Inorg. Chim. Acta,178, 47±54.
Feng, Q., Li, D., Yin, Y.-G., Feng, X.-L. & Cai, J.-W. (2002).Acta Chim. Sin.60, 2167±2171.
Hannon, M. J., Painting, C. L., Plummer, E. A., Childs, L. J. & Alcock, N. W. (2002).Chem. Eur. J.8, 2225±2238.
Johnson, C. K. (1976).ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA.
supporting information
sup-1
Acta Cryst. (2004). E60, m1106–m1107
supporting information
Acta Cryst. (2004). E60, m1106–m1107 [https://doi.org/10.1107/S1600536804016472]
(Acetonitrile-
κ
N)(4
′
-phenyl-2,2
′
:6
′
,2
′′
-terpyridine-
κ
3N)silver(I)
hexafluoro-phosphate acetonitrile solvate
Lei Hou, Dan Li, Ye-Gao Yin, Tao Wu and Seik Weng Ng
(Acetonitrile-κN)(4′-phenyl-2,2′:6′,2′′-terpyridine-κ3N)silver(I) hexafluorophosphate acetonitrile solvate
Crystal data
[Ag(C2H3N)(C21H15N3)]PF6·C2H3N Mr = 644.31
Monoclinic, P21/n
Hall symbol: -P 2yn
a = 16.777 (1) Å
b = 7.8257 (6) Å
c = 19.447 (1) Å
β = 90.356 (2)°
V = 2553.2 (3) Å3 Z = 4
F(000) = 1288
Dx = 1.676 Mg m−3
Mo Kα radiation, λ = 0.71073 Å Cell parameters from 1971 reflections
θ = 2.4–20.3°
µ = 0.92 mm−1 T = 295 K Prism, yellow
0.20 × 0.18 × 0.12 mm
Data collection
Bruker APEX CCD area-detector diffractometer
Radiation source: fine-focus sealed tube Graphite monochromator
φ and ω scans
Absorption correction: multi-scan (SADABS; Bruker, 2002)
Tmin = 0.354, Tmax = 0.898
12897 measured reflections 4488 independent reflections 3262 reflections with I > 2σ(I)
Rint = 0.038
θmax = 25.0°, θmin = 1.6° h = −17→19
k = −9→9
l = −20→23
Refinement
Refinement on F2
Least-squares matrix: full
R[F2 > 2σ(F2)] = 0.057 wR(F2) = 0.178 S = 1.06 4488 reflections 345 parameters 0 restraints
Primary atom site location: structure-invariant direct methods
Secondary atom site location: difference Fourier map
Hydrogen site location: inferred from neighbouring sites
H-atom parameters constrained
w = 1/[σ2(F
o2) + (0.0996P)2 + 1.6223P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.001
Δρmax = 1.06 e Å−3
Δρmin = −0.42 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
x y z Uiso*/Ueq
P1 0.49678 (9) 0.8129 (2) 0.13043 (8) 0.0564 (4) F1 0.5325 (5) 0.709 (1) 0.1899 (4) 0.198 (4) F2 0.5194 (4) 0.6598 (9) 0.0861 (5) 0.198 (4) F3 0.4604 (6) 0.915 (2) 0.0740 (4) 0.229 (4) F4 0.4730 (5) 0.957 (1) 0.1773 (5) 0.208 (5) F5 0.4137 (3) 0.7281 (8) 0.1435 (3) 0.135 (2) F6 0.5801 (3) 0.8920 (8) 0.1226 (4) 0.166 (3) N1 0.5466 (3) 0.3825 (6) 0.3786 (2) 0.047 (1) N2 0.5507 (2) 0.3044 (5) 0.5131 (2) 0.040 (1) N3 0.6778 (3) 0.4362 (6) 0.5784 (2) 0.052 (1) N4 0.7557 (3) 0.6140 (8) 0.4294 (3) 0.073 (2) N5 0.2496 (5) 0.006 (1) 0.4065 (4) 0.100 (2) C1 0.5498 (4) 0.4129 (9) 0.3092 (3) 0.063 (2) C2 0.4950 (4) 0.3500 (9) 0.2642 (3) 0.067 (2) C3 0.4342 (4) 0.2517 (9) 0.2884 (3) 0.064 (2) C4 0.4296 (3) 0.2179 (8) 0.3581 (3) 0.052 (1) C5 0.4876 (3) 0.2857 (7) 0.4021 (3) 0.043 (1) C6 0.4871 (3) 0.2517 (6) 0.4782 (3) 0.039 (1) C7 0.4242 (3) 0.1685 (6) 0.5100 (3) 0.040 (1) C8 0.4289 (3) 0.1299 (6) 0.5798 (3) 0.040 (1) C9 0.4968 (3) 0.1842 (7) 0.6145 (3) 0.043 (1) C10 0.5558 (3) 0.2730 (6) 0.5803 (3) 0.040 (1) C11 0.6279 (3) 0.3443 (7) 0.6170 (3) 0.043 (1) C12 0.6407 (4) 0.3224 (8) 0.6864 (3) 0.057 (2) C13 0.7067 (4) 0.3943 (9) 0.7168 (3) 0.062 (2) C14 0.7579 (4) 0.4885 (8) 0.6782 (4) 0.063 (2) C15 0.7415 (4) 0.5046 (8) 0.6094 (4) 0.066 (2) C16 0.3645 (3) 0.0342 (7) 0.6145 (3) 0.042 (1) C17 0.3106 (3) −0.0636 (7) 0.5786 (3) 0.048 (1) C18 0.2506 (3) −0.1518 (8) 0.6107 (3) 0.060 (2) C19 0.2430 (4) −0.1433 (9) 0.6815 (3) 0.068 (2) C20 0.2968 (5) −0.049 (1) 0.7182 (4) 0.077 (2) C22 0.3562 (4) 0.0411 (8) 0.6863 (3) 0.062 (2) C23 0.8130 (4) 0.6851 (8) 0.4243 (3) 0.063 (2) C24 0.8867 (4) 0.779 (1) 0.4170 (5) 0.098 (3) C25 0.1925 (5) −0.066 (1) 0.4147 (4) 0.071 (2) C26 0.1195 (5) −0.157 (1) 0.4270 (5) 0.097 (3)
H1 0.5912 0.4793 0.2922 0.076*
H2 0.4988 0.3736 0.2175 0.081*
H3 0.3961 0.2078 0.2583 0.077*
H4 0.3885 0.1510 0.3754 0.062*
H7 0.3791 0.1385 0.4847 0.048*
H9 0.5028 0.1605 0.6611 0.051*
supporting information
sup-3
Acta Cryst. (2004). E60, m1106–m1107
H18 0.2151 −0.2173 0.5849 0.072* H19 0.2020 −0.2010 0.7037 0.082* H20 0.2930 −0.0446 0.7659 0.092* H22 0.3913 0.1069 0.7124 0.074* H24a 0.9161 0.7335 0.3789 0.147* H24b 0.9178 0.7674 0.4583 0.147* H24c 0.8752 0.8971 0.4089 0.147* H26a 0.0823 −0.0835 0.4497 0.145* H26b 0.1303 −0.2549 0.4554 0.145* H26c 0.0972 −0.1944 0.3839 0.145*
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
C23 0.053 (4) 0.053 (4) 0.082 (4) 0.004 (3) 0.017 (3) 0.000 (3) C24 0.054 (4) 0.074 (5) 0.165 (8) −0.017 (4) 0.022 (5) 0.006 (5) C25 0.074 (5) 0.071 (5) 0.068 (4) 0.003 (4) −0.009 (4) 0.003 (4) C26 0.072 (5) 0.097 (6) 0.122 (7) −0.006 (5) 0.003 (5) 0.002 (5)
Geometric parameters (Å, º)
Ag1—N1 2.348 (5) C13—C14 1.361 (9)
Ag1—N2 2.378 (4) C14—C15 1.37 (1)
Ag1—N3 2.470 (5) C16—C17 1.373 (8)
Ag1—N4 2.187 (6) C16—C22 1.406 (8)
P1—F3 1.485 (6) C17—C18 1.374 (8)
P1—F4 1.508 (6) C18—C19 1.385 (9)
P1—F2 1.525 (6) C19—C20 1.37 (1)
P1—F1 1.533 (6) C20—C22 1.370 (9)
P1—F6 1.537 (5) C23—C24 1.444 (9)
P1—F5 1.565 (5) C25—C26 1.44 (1)
N1—C5 1.329 (7) C1—H1 0.93
N1—C1 1.373 (7) C2—H2 0.93
N2—C6 1.327 (6) C3—H3 0.93
N2—C10 1.334 (6) C4—H4 0.93
N3—C15 1.336 (8) C7—H7 0.93
N3—C11 1.339 (7) C9—H9 0.93
N4—C23 1.116 (8) C12—H12 0.93
N5—C25 1.12 (1) C13—H13 0.93
C1—C2 1.357 (9) C14—H14 0.93
C2—C3 1.363 (9) C15—H15 0.93
C3—C4 1.384 (8) C17—H17 0.93
C4—C5 1.397 (7) C18—H18 0.93
C5—C6 1.504 (7) C19—H19 0.93
C6—C7 1.388 (7) C20—H20 0.93
C7—C8 1.392 (7) C22—H22 0.93
C8—C9 1.388 (7) C24—H24a 0.96
C8—C16 1.481 (7) C24—H24b 0.96
C9—C10 1.382 (7) C24—H24c 0.96
C10—C11 1.508 (7) C26—H26a 0.96
C11—C12 1.376 (8) C26—H26b 0.96
C12—C13 1.372 (8) C26—H26c 0.96
supporting information
sup-5
Acta Cryst. (2004). E60, m1106–m1107
F3—P1—F1 178.5 (6) C20—C22—C16 120.5 (6) F4—P1—F1 92.7 (6) N4—C23—C24 179.2 (8) F2—P1—F1 84.9 (5) N5—C25—C26 178.7 (9)
F3—P1—F6 94.6 (5) C2—C1—H1 118.6
F4—P1—F6 90.1 (4) N1—C1—H1 118.6
F2—P1—F6 91.8 (4) C1—C2—H2 120.4
F1—P1—F6 86.4 (4) C3—C2—H2 120.4
F3—P1—F5 89.1 (5) C2—C3—H3 120.2
F4—P1—F5 88.9 (4) C4—C3—H3 120.2
F2—P1—F5 89.0 (3) C3—C4—H4 120.5
F1—P1—F5 89.8 (4) C5—C4—H4 120.5
F6—P1—F5 176.0 (4) C6—C7—H7 120.1
C5—N1—C1 118.1 (5) C8—C7—H7 120.1
C5—N1—Ag1 119.2 (3) C10—C9—H9 119.7 C1—N1—Ag1 122.4 (4) C8—C9—H9 119.7 C6—N2—C10 119.3 (4) C13—C12—H12 120.3 C6—N2—Ag1 118.5 (3) C11—C12—H12 120.3 C10—N2—Ag1 122.0 (3) C14—C13—H13 120.2 C15—N3—C11 117.6 (5) C12—C13—H13 120.2 C15—N3—Ag1 123.7 (4) C13—C14—H14 121.2 C11—N3—Ag1 118.7 (3) C15—C14—H14 121.2 C23—N4—Ag1 171.9 (6) N3—C15—H15 118.0 C2—C1—N1 122.7 (6) C14—C15—H15 118.0 C1—C2—C3 119.2 (6) C16—C17—H17 118.9 C2—C3—C4 119.5 (6) C18—C17—H17 118.9 C3—C4—C5 119.0 (6) C17—C18—H18 120.0 N1—C5—C4 121.6 (5) C19—C18—H18 120.0 N1—C5—C6 116.6 (5) C20—C19—H19 120.6 C4—C5—C6 121.8 (5) C18—C19—H19 120.6 N2—C6—C7 122.0 (5) C19—C20—H20 119.3 N2—C6—C5 116.0 (4) C22—C20—H20 119.3 C7—C6—C5 122.0 (5) C20—C22—H22 119.8 C6—C7—C8 119.8 (5) C16—C22—H22 119.8 C9—C8—C7 116.7 (5) C23—C24—H24a 109.5 C9—C8—C16 122.1 (5) C23—C24—H24b 109.5 C7—C8—C16 121.2 (5) H24a—C24—H24b 109.5 C10—C9—C8 120.6 (5) C23—C24—H24c 109.5 N2—C10—C9 121.5 (5) H24a—C24—H24c 109.5 N2—C10—C11 116.2 (4) H24b—C24—H24c 109.5 C9—C10—C11 122.2 (4) C25—C26—H26a 109.5 N3—C11—C12 121.5 (5) C25—C26—H26b 109.5 N3—C11—C10 115.9 (5) H26a—C26—H26b 109.5 C12—C11—C10 122.6 (5) C25—C26—H26c 109.5 C13—C12—C11 119.5 (6) H26a—C26—H26c 109.5 C14—C13—C12 119.7 (6) H26b—C26—H26c 109.5