C. Desmarets, I. Azcarate, G. Gontard, H. Amouri
FULL PAPER
2.92, N 4.39. X-ray quality crystals were obtained by slow vapour
diffusion of diethyl ether into an acetonitrile solution of 1b.
[1]
[2]
W. L. Leong, J. J. Vittal, Chem. Rev. 2011, 111, 688.
S. R. Batten, S. M. Neville, D. R. Turner, Coordination Poly-
mers: Design, Analysis and Application, Cambridge, U. K.,
2009.
M. Oh, C. L. Stern, C. A. Mirkin, Inorg. Chem. 2005, 44, 2647.
Y. Y. Karabach, M. da Silva, M. N. Kopylovich, B. Gil-Her-
nandez, J. Sanchiz, A. M. Kirillov, A. J. L. Pombeiro, Inorg.
Chem. 2010, 49, 11096.
M. Mitsumi, K. Kitamura, A. Morinaga, Y. Ozawa, M. Kobay-
ashi, K. Toriumi, Y. Iso, H. Kitagawa, T. Mitani, Angew. Chem.
Int. Ed. 2002, 41, 2767.
H. Kitagawa, N. Onodera, T. Sonoyama, M. Yamamoto, T.
Fukawa, T. Mitani, M. Seto, Y. Maeda, J. Am. Chem. Soc.
1999, 121, 10068.
[AgL2NO3]n (1c): 1c was prepared in a similar way to 1a using L2
(50 mg, 0.16 mmol) in CH2Cl2 (5 mL) and AgNO3 (27 mg,
0.16 mmol) in CH3CN (5 mL); yield 79% (65 mg, 0.126 mmol). IR
[3]
[4]
1
(ATR): ν = 1302 [ν(N–O)]. H NMR (300 MHz, CD CN, 298 K):
˜
3
δ = 8.73 (d, J = 1.5 Hz, 2 H, py-H), 8.56 (dd, J = 5.1, 1.5 Hz, 2 H,
py-H), 7.89 (dt, J = 7.8, 2.1 Hz, 2 H, py-H), 7.41 (ddd, J = 8.1,
4.8, 0.9 Hz, 2 H, py-H), 7.35 (t, J = 1.2 Hz, 1 H, Ar-H), 7.17 (d, J
= 1.2 Hz, 1 H, Ar-H), 3.85 (s, 3 H, OMe) ppm. [AgL2NO3]·
0.6CH2Cl2 (531): calcd. C 48.84, H 2.88, N 7.91; found C 47.57, H
2.78, N 7.87.
[5]
[6]
[AgL2PF6]n (1d): 1d was prepared in a similar way to 1a using L2
(50 mg, 0.16 mmol) in CH2Cl2 (5 mL) and AgPF6 (40 mg,
[7]
[8]
C. Janiak, Dalton Trans. 2003, 2781.
S. Shimomura, M. Higuchi, R. Matsuda, K. Yoneda, Y. Hiji-
kata, Y. Kubota, Y. Mita, J. Kim, M. Takata, S. Kitagawa, Nat.
Chem. 2010, 2, 633.
C. Janiak, J. K. Vieth, New J. Chem. 2010, 34, 2366.
H. Amouri, M. N. Rager, F. Cagnol, J. Vaissermann, Angew.
Chem. Int. Ed. 2001, 40, 3636.
B. Therrien, J. Organomet. Chem. 2011, 696, 637.
J. Pospisil, I. Jess, C. Nather, M. Necas, P. Taborsky, New J.
Chem. 2011, 35, 861.
0.16 mmol) in CH3CN (5 mL); yield 90% (81 mg, 0.144 mmol). IR
1
(ATR): ν = 756 [ν(P–F)]. H NMR (300 MHz, CD CN, 298 K): δ
˜
3
= 8.73 (d, J = 1.5 Hz, 2 H, py-H), 8.58 (dd, J = 4.8, 1.5 Hz, 2 H,
py-H), 7.90 (dt, J = 7.8, 2.1 Hz, 2 H, py-H), 7.39 (ddd, J = 8.1,
4.8, 0.9 Hz, 2 H, py-H), 7.33 (t, J = 1.2 Hz, 1 H, Ar-H), 7.17 (d, J
= 1.2 Hz, 1 H, Ar-H), 3.85 (s, 3 H, OMe) ppm. [AgL2PF6]·
1.5CH2Cl2 (690): calcd. C 39.13, H 2.48, N 4.06; found C 38.64, H
2.12, N 4.16.
[9]
[10]
[11]
[12]
[13]
[14]
[15]
[16]
J. M. Yue, Y. Y. Niu, B. Zhang, S. W. Ng, H. W. Hou, Crys-
tEngComm 2011, 13, 2571.
F. L. Yang, J. Tao, R. B. Huang, L. S. Zheng, Inorg. Chem.
2011, 50, 911.
P. Phuengphai, S. Youngme, P. Gamez, J. Reedijk, Dalton
Trans. 2010, 39, 7936.
J.-M. Lehn, Supramolecular Chemsitry, Concepts and Perspec-
tives, VCH, Weinheim, Germany, 1995.
Data Collection and Structure Refinement: A single crystal of 1a or
1b was selected, mounted onto a glass fiber, and transferred in a
cold nitrogen gas stream. Intensity data were collected with a
Bruker-Nonius Kappa-CCD with graphite-monochromated Mo-
Kα radiation. Unit-cell parameter determination, data collection
strategy and integration were carried out with the Nonius EVAL-
14 suite of programs[54]). Multi-scan absorption correction was ap-
plied[55]. The structure was solved by direct methods using the
SIR92 program[56] and refined anisotropically by full-matrix least-
[17] V. W. W. Yam, C. H. Tao, L. J. Zhang, K. M. C. Wong, K. K.
Cheung, Organometallics 2001, 20, 453.
R. Ziessel, M. Hissler, A. El-Ghayoury, A. Harriman, Coord.
Chem. Rev. 1998, 178, 1251.
T. Yamada, S. Iwakiri, T. Hara, K. Kanaizuka, M. Kurmoo,
H. Kitagawa, Cryst. Growth Des. 2011.
Y. R. Zheng, Z. G. Zhao, M. Wang, K. Ghosh, J. B. Pollock,
T. R. Cook, P. J. Stang, J. Am. Chem. Soc. 2010, 132, 16873.
X. Zhang, T. Chen, H. J. Yan, D. Wang, Q. H. Fan, L. J. Wan,
K. Ghosh, H. B. Yang, P. J. Stang, Acs Nano 2010, 4, 5685.
Y. R. Zheng, H. B. Yang, B. H. Northrop, K. Ghosh, P. J.
Stang, Inorg. Chem. 2008, 47, 4706.
squares methods using the SHELXL-97 software package[57]
.
[18]
[19]
[20]
[21]
[22]
[23]
[24]
[25]
Crystal Data for 1a: Yellow crystal, C44H28Ag2N4F6O8S2, mono-
clinic, P21/c, a = 8.3889(16), b = 18.5773(16), c = 29.144(6) Å, α =
90, β = 98.787(11), γ = 90°, V = 4488.6(13) Å3, Z = 4, T = 200(1)
K, μ = 1.048 mm–1, 48054 reflections measured, 13079 independent
(Rint = 0.0756), 6132 observed [IՆ2σ(I)], 597 parameters, final R
indices R1 [IՆ2σ(I)] = 0.0474 and wR2 (all data) = 0.1250, GO-
F(on F2) = 0.957, max/min residual electron density 0.832/–
1.023 eÅ–3.
Y. Yamauchi, M. Yoshizawa, M. Fujita, J. Am. Chem. Soc.
2008, 130, 5832.
Crystal Data for 1b: Colourless crystal, C21H15AgN2F4BO1.5, mo-
noclinic, P21/c, a = 10.7344(9), b = 17.4781(16), c = 11.1875(9) Å,
α = 90, β = 103.965(6), γ = 90°, V = 2036.9(3) Å3, Z = 4, T =
200(1) K, μ = 1.043 mm–1, 16116 reflections measured, 5738 inde-
pendent (Rint = 0.0501), 3034 observed [IՆ2σ(I)], 272 parameters,
final R indices R1 [IՆ2σ(I)] = 0.0567 and wR2 (all data) = 0.1643,
GOF(on F2) = 1.043, max./min. residual electron density 0.860/
–0.836 eÅ–3. The BF4– anion and the water molecule are disordered
over two positions. Both were refined isotropically to avoid mean-
ingless anisotropic displacement parameters.
M. D. Zaman, K. Udachin, J. A. Ripmeester, M. D. Smith,
H. C. zur Loye, Inorg. Chem. 2005, 44, 5047.
T. M. Fasina, J. C. Collings, D. P. Lydon, D. Albesa-Jove, A. S.
Batsanov, J. A. K. Howard, P. Nguyen, M. Bruce, A. J. Scott,
W. Clegg, S. W. Watt, C. Viney, T. B. Marder, J. Mater. Chem.
2004, 14, 2395.
T. Rajendran, B. Manimaran, R. T. Liao, R. J. Lin, P. Thanase-
karan, G. H. Lee, S. M. Peng, Y. H. Liu, I. J. Chang, S. Rajago-
pal, K. L. Lu, Inorg. Chem. 2003, 42, 6388.
S. Shanmugaraju, A. K. Bar, S. A. Joshi, Y. P. Patil, P. S. Mu-
kherjee, Organometallics 2011, 30, 1951.
P. H. Liao, B. W. Langloss, A. M. Johnson, E. R. Knudsen,
F. S. Tham, R. R. Julian, R. J. Hooley, Chem. Commun. 2010,
46, 4932.
S. Ghosh, B. Gole, A. K. Bar, P. S. Mukherjee, Organometallics
2009, 28, 4288.
[26]
[27]
[28]
CCDC-826115 (for 1a) and -826116 (for 1b) contain the supple-
mentary crystallographic data for this paper. These data can be
obtained free of charge from The Cambridge Crystallographic
Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
[29]
[30]
[31]
[32]
N. Schultheiss, J. M. Ellsworth, E. Bosch, C. L. Barnes, Eur. J.
Inorg. Chem. 2005, 45.
H. J. Kim, J. H. Lee, M. Lee, Angew. Chem. Int. Ed. 2005, 44,
5810.
H. J. Kim, W. C. Zin, M. Lee, J. Am. Chem. Soc. 2004, 126,
7009.
Acknowledgments
We acknowledge the Université Pierre et Marie Curie Paris-6 and
the Centre National de la Recherche Scientifique (CNRS) for sup-
porting this work.
4562
www.eurjic.org
© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Eur. J. Inorg. Chem. 2011, 4558–4563