Full Paper
SC-SC transformations
Acknowledgements
Before carrying out metal-exchange reactions of 1 and linker-ex-
change and transmetalation reactions of 2, the individual as-syn-
thesized single crystals were immersed in DMF for 2 d to dissolve
any remaining reactants and side products adhering to the crystals.
During this process, the solvent was refreshed four times. After
washing with DMF, the crystals were allowed to dip in the appro-
priate solution at room temperature (RT). Detailed procedures for
each transformation are described below.
This work was supported by DST, India (J.C. Bose National Fel-
lowship to PKB.) and TKP. is grateful for SRF from the CSIR.
Keywords: carboxylate ligands
·
layered compounds
·
metalation · metal–organic frameworks · zinc
[1] a) O. K. Farha, I. Eryazici, N. C. Jeong, B. G. Hauser, C. E. Wilmer, A. A. Sar-
jeant, R. Q. Snurr, S. T. Nguyen, A. O. Yazaydın, J. T. Hupp, J. Am. Chem.
Lim, Chem. Rev. 2011, 111, 782–835; c) L. J. Murray, M. Dinca, J. R. Long,
Synthesis of {Zn(L)(L2)0.5]·3DMF·4H2O}n (3): Keeping single crystals
of 2 in a DMF solution of L2 (0.05m) for 5 d afforded compound 3
without any loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3433br,
2933w, 1657s, 1615s, 1585s, 1380s, 1260m, 1190m, 850s, 772s, 700
s; elemental analysis (%) calcd for C26H38N6O11Zn: C 46.19, H 5.67, N
12.43; found: C 46.00, H 5.35, N 12.20.
Sumida, D. L. Rogow, J. A. Mason, T. M. McDonald, E. D. Bloch, Z. R.
wa, N. Ko, Y. B. Go, N. Aratani, S. B. Choi, E. Choi, A. O. Yazaydin, R. Q.
Vaidhyanathan, S. S. Iremonger, G. K. H. Shimizu, P. G. Boyd, S. Alavi, T. K.
[3] a) J.-R. Li, Y. Ma, M. C. McCarthy, J. Sculley, J. Yu, H.-K. Jeong, P. B. Balbue-
A. M. Spokoyny, O. K. Farha, R. Q. Snurr, J. T. Hupp, C. A. Mirkin, Chem.
1256; c) R. K. Das, A. Aijaz, M. K. Sharma, P. Lama, P. K. Bharadwaj, Chem.
Synthesis of {Zn(L)(L3)0.5]·5DMF·2H2O}n (4): Keeping single crystals
of 2 in a DMF solution of L3 (0.05m) for 2 d afforded compound 4
without any loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3447br,
2924w, 1663s, 1619s, 1355s, 1101s, 804s, 767s; elemental analysis
(%) calcd for C34H50N6O11Zn: C 52.08, H 6.43, N 10.72; found: C
51.90, H 6.30, N 10.57.
Synthesis of {Zn(L)(L4)0.5]·4DMF·3H2O}n (5): Keeping single crystals
of 2 in a DMF solution of L4 (0.05m) for 3 d afforded compound 5
without loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3458br, 2929w,
1663s, 1609s, 1405m, 1101s, 777s, 673s; elemental analysis (%)
calcd for C28H43N5O11Zn: C 48.66, H 6.27, N 10.13; found: C 48.50, H
6.15, N 10.00.
Synthesis of {[Cu2(L)(DMF)2]·3DMF·2 MeCN·2H2O} (1Cu): Keeping
single crystals of 1 in a 0.05m solution of Cu(NO3)2 in acetonitrile
for 20 h afforded 1Cu without any loss of crystallinity. FTIR (KBr
pellet, cmÀ1): 3414br, 1621s, 1580s, 1369s, 1254s, 1038s; elemental
analysis (%) calcd for C41H55N7O15Cu2: C 48.61, H 5.47, N 9.68;
found: C 48.39, H 5.33, N 9.47.
[5] a) H.-J. Son, S. Jin, S. Patwardhan, S. J. Wezenberg, N. C. Jeong, M. So,
C. E. Wilmer, A. A. Sarjeant, G. C. Schatz, R. Q. Snurr, O. K. Farha, G. P.
Wiederrecht, J. T. Hupp, J. Am. Chem. Soc. 2012, 134, 862–869; b) J.-L.
47, 5122–5128; c) J. Lipkowski In Inclusion Compounds. J. L. Atwood,
J. E. D. Davies, D. D. MacNicol, Eds.; Academic Press: New York, 1984,
Zhang, Y.-B. Zhang, J.-B. Lin, X.-M. Chen, Chem. Rev. 2011, 111, 1001–
1033; h) L. E. Kreno, K. Leong, O. K. Farha, M. Allendorf, R. P. VanDuyne,
[7] a) L. Pan, H. Liu, S. P. Kelly, X. Huang, D. H. Olson, J. Li, Chem. Commun.
Synthesis of {[Cu(L)(L1)0.5]·4DMF·2H2O}n (2Cu): Keeping single crys-
tals of 2 in a 0.05m solution of Cu(NO3)2 in DMF for 2 d afforded
2Cu without any loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3440br,
2926w, 1657s, 1615s, 1375s, 1249s, 1001m, 839m, 700s, 752s; ele-
mental analysis (%) calcd for C29H43N7O10Cu: C 48.84, H 6.08, N
13.74; found: C 48.69, H 5.90, N 13.60.
Synthesis of {[Cu(L)(L3)0.5]·4DMF·H2O}n (4Cu): Keeping single crys-
tals of 4 in a 0.05m solution of Cu(NO3)2 in DMF for 2 d afforded
4Cu without any loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3433br,
2926w, 1652s, 1628s, 1098s, 785s, 700s, 752 s; elemental analysis
(%) calcd for C31H41N5O9Cu: C 53.87, H 5.98, N 10.13; found: C
53.63, H 5.77, N 10.01.
Synthesis of {Cu(L)(L4)0.5]·2DMF·4H2O}n (5Cu): Keeping single crys-
tals of 5 in a 0.05m solution of Cu(NO3)2 in DMF for 3 d afforded
5Cu without any loss of crystallinity. FTIR (KBr pellet, cmÀ1): 3425br,
3083w, 2918s, 1663s, 1603s, 1393s, 1229s, 1091s, 816s, 628 s; ele-
mental analysis (%) calcd for C22H31N3O10Cu: C 47.10, H 5.57, N
7.49; found: C 46.96, H 5.34, N 7.30.
[8] a) R. Kitaura, F. Iwahori, R. Matsuda, S. Kitagawa, Y. Kubota, M. Takata,
[9] a) O. Karagiaridi, W. Bury, A. A. Sarjeant, C. L. Stern, O. K. Farha, J. T.
131, 3866–3868; e) O. Karagiaridi, W. Bury, E. Tylianakis, A. A. Sarjeant,
Synthesis of {Cu(L)(L4)0.5]·3DMF·2H2O}n (5CuMeCN): Keeping single
crystals of 5 in a 0.05m solution of Cu(NO3)2 in MeCN afforded
MeCN
5Cu
without any loss of crystallinity. FTIR (KBr pellet, cmÀ1):
3439br, 2918s, 2850s, 1604s, 1393s, 1229s, 1003s, 816s, 687 s; ele-
mental analysis (%) calcd for C25H34N4O9Cu: C 50.21, H 5.73, N 7.37;
found: C 50.05, H 5.20, N 7.30.
Chem. Eur. J. 2015, 21, 16083 – 16090
16089
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