Table 8 Crystallographic data for compounds 1–6
1
2
3
4
5
6
Formula
M
Crystal system
Space group
C H F N O S Zn C H CoN O
C H Cl CoN O
1037.57
Monoclinic
P21/c
C120H120CoN O
C H CoN O
551.37
C H CoN O
51 46 6 11
977.87
5
6
46
6
6
17
2
22 18
6
10
46 40
4
6
10
14 18
24 20
4
8
1318.48
Triclinic
585.35
2105.23
Triclinic
¯
P1
Triclinic
Triclinic
Triclinic
¯
P1
¯
¯
¯
P1
P1
P1
a/Å
b/Å
c/Å
α/Њ
β/Њ
γ/Њ
9.323(2)
11.359(2)
11.765(2)
11.928(2)
112.50(1)
93.74(1)
112.77(1)
1314.7(4)
2
13.338(4)
15.531(5)
12.136(4)
90
113.02(1)
90
2313.8(13)
2
0.667
12.554(5)
18.420(5)
23.888(5)
89.02(1)
87.26(1)
87.11(1)
5510(3)
2
8.172(5)
8.482(5)
17.977(5)
81.23(1)
89.94(1)
75.46(1)
1191.2(11)
2
11.320(1)
13.261(1)
16.001(1)
92.38(1)
99.64(1)
98.53(1)
2336.4(3)
2
11.113(2)
14.306(2)
93.26(1)
93.42(1)
97.11(1)
1465.1(5)
1
3
U/Å
Z
µ(Mo-Kα)/mm
Refl. collected
Ϫ1
0.585
19777
0.718
10202
0.230
40207
0.779
10293
0.437
20146
25292
Indep. refl., R(int)
Refl. observed [F > 4σ(F)] 5058
7249, 0.0353
3368, 0.0442
2702
5068, 0.0669
3251
18283, 0.0635
8014
10293, 0.00
4019
8183, 0.0349
5503
R1 [F > 4σ(F)]
wR2 (all data)
0.0587
0.1396
0.1202
0.3533
0.0696
0.2196
0.0482
0.1183
0.1138
0.3586
0.0492
0.1342
3
See, for example: W. B. Lin, L. Ma and O. R. Evans, Chem.
Commun., 2000, 2263; O. R. Evans, R.-G. Xiong, Z. Wang,
G. K. Wong and W. Lin, Angew. Chem., Int. Ed., 1999, 38, 536;
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Ed., 2000, 39, 2081; M. Eddaoudi, H. L. Li and O. M. Yaghi, J. Am.
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L. R. MacGillivray, S. Subramanian and M. J. Zaworotko,
J. Chem. Soc., Chem Commun., 1994, 1325; L. Carlucci, G. Ciani,
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Crystallography
Single crystal X-ray experiments for compounds 1–6 were
performed on a Bruker SMART-CCD diffractometer, the data
collections were performed at 293 K by the ω-scan method
using Mo-Kα radiation (λ = 0.71073 Å). Other details of crystal
data, data collection and processing are given in Table 8.
24
Empirical absorption corrections (SADABS) were applied
in all cases. The structures were solved by direct methods
4
2
5
2
(
(
SIR97) and refined by full-matrix least-squares on F
26
SHELX-97). All hydrogen atoms were placed in geometric-
ally calculated positions and thereafter refined using a riding
model with U (H) = 1.2U (C). All non-hydrogen atoms were
iso
eq
refined with anisotropic displacement parameters. In com-
pound 1, the anion triflate was found to be disordered and was
refined using two models with occupancies of 52 and 48%. The
solvated water molecules were statistically disordered and were
refined isotropically with half occupancy. In compound 3, the
coordinated nitrate anion was found to be disordered and was
refined using two models with occupancies of 71 and 29%.
Structures 2 and 5 were found to be non-merohedrally twinned
and a suitable set of BASF parameters were used in the refine-
2
755; O. M. Yaghi and H. Li, J. Am. Chem. Soc., 1995, 117, 10401.
5 L. Carlucci, G. Ciani, D. W. v. Gudenberg and D. M. Proserpio,
Inorg. Chem., 1997, 36, 3812.
6
T. Hennigar, D. C. MacQuarrie, P. Losier, R. D. Rogers and
M. J. Zaworotko, Angew. Chem., Int. Ed. Engl., 1997, 36, 972;
L. Carlucci, G. Ciani, D. M. Proserpio and S. Rizzato, Chem.
Commun., 2000, 1319.
A. J. Blake, N. R. Champness, A. Khlobystov, D. A. Lemenovskii,
W.-S. Li and M. Schröder, Chem. Commun., 1997, 2027; M. Fujita,
O. Sasaki, K.-Y. Watanabe, K. Ogura and K. Yamaguchi, New
J. Chem., 1998, 22, 189; L. Carlucci, G. Ciani and D. M. Proserpio,
J. Chem. Soc., Dalton Trans., 1999, 1799.
(a) A. J. Blake, N. R. Champness, S. S. M. Chung, W.-S. Li and
M. Schröder, Chem. Commun., 1997, 1005; (b) M. A. Withersby,
A. J. Blake, N. R. Champness, P. A. Cooke, P. Hubberstey,
A. L. Realf, S. J. Teat and M. Schroder, J. Chem. Soc., Dalton Trans.,
7
27
ment, according to the procedure described in GEMINI. All
28
the diagrams were created using the SCHAKAL99 program.
8
9
CCDC reference numbers 173813–173818.
See http://www.rsc.org/suppdata/dt/b1/b110189g/ for crystal-
lographic data in CIF or other electronic format.
2
000, 3261; (c) C. He, B.-G. Zhang, C. Duan, J. Li and Q.-J. Meng,
Eur. J. Inorg. Chem., 2000, 2549; (d ) S. R. Batten, J. C. Jeffery and
M. D. Ward, Inorg. Chim. Acta, 1999, 292, 231.
Acknowledgements
L. Carlucci, G. Ciani, M. Moret, D. M. Proserpio and S. Rizzato,
Angew. Chem., Int. Ed., 2000, 39, 1506; L. Carlucci, G. Ciani and
D. M. Proserpio, Chem. Commun., 1999, 449; M. J. Plater, M. R. St
J. Foreman, T. Gelbrich and M. B. Hursthouse, Cryst. Eng., 2001, 4,
We thank MURST for financing the project “Solid Super-
molecules” 2000–2001.
3
19.
1
1
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