Topochemical conversion of a hydrogen-bonded three-dimensional network into a covalently bonded framework

Angewandte Chemie - International Edition

Volumn 37, Issue 8, 1998, Pages 1114-1116

  Ranford, John D ^a   Vittal, Jagadese J ^a   Wu, Daqing ^a  

^a NATIONAL UNIVERSITY OF SINGAPORE   (Singapore)

Author keywords

Coordination polymers; Crystal engineering; Supramolecular chemistry; Topochemistry; Zinc

Indexed keywords

EID: 0032482107     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/(SICI)1521-3773(19980504)37:8<1114::AID-ANIE1114>3.0.CO;2-E     Document Type: Article

References (29)

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20. 2 = 0.0662 for all 3385 data. The Flack parameter x was refined to 0.003(15).
21. Close intermolecular hydrogen-bonding distances [Å] and angles [°]: O2 ⋯ H1 2.050, O3 ⋯ H4B 1.857, O2 ⋯ N1 2.950, O3 ⋯ O4 2.645; O2-H1-N1 169.6, O3-H4B-O4 174.0.
22. The channels are oval with approximate dimensions 7 × 10 Å (non-hydrogen contacts). However, the alternating, stacked arrangement means that the effective pore size is bigger than this. The channels are occupied by (disordered) water molecules and held together by hydrogen bonds. Selected hydrogen-bonded distances [Å]: O3 ⋯ O5 2.771, O3 ⋯ O5 A 2.781, O3 ⋯ O5 B 2.556.
23. Thermogravimetric analysis of 1 indicated a weight loss of 11.2% in the temperature range 50-120°C, corresponding to the loss of two molecules of water (expected weight loss 12.2 %) and the formation of the anhydrous compound 2. The X-ray powder pattern of this anhydrous material was the same as that of 2. Both 1 and 2 show the same decomposition pattern, which starts at about 340°C.
24. The structures of the bulk materials for 1 and 2 were confirmed by matching their X-ray powder patterns with those generated from the corresponding single crystals. Compound 2 was also prepared independently. The crystal structure was carried out on the single crystal grown from aqueous solution.
25. 2 = 0.0425 for all 2571 data. The Flack parameter x was refined to -0.004(8).
26. The single crystal of 1 became opaque and brittle on heating at 90°C for two hours.
27. Distances [Å] and angles [°] of the hydrogen bonds: O2 ⋯ H1 2.161, O2 ⋯N1 2.944; N1-H1-O2 144.
28. L. L. Koh, J. D. Ranford, W. T. Robinson, J. O. Svensson, L. C. Tan, D. Wu, Inorg. Chem. 1996, 35, 6466-6472.
29. General crystallographic details: Data were collected on a Siemens SMART CCD system with graphite-monochromated MoKn radiation and a sealed tube (2.4 kW) at 23°C. Absorption corrections were made with the program SADABS (G. M. Sheldrick, Göttingen, 1996), and the crystallographic software package SHELXTL (SHELXTL Reference Manual, Version 5.03, Wisconsin, 1996) was used for all calculations. Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Center as supplementary publication no. CCDC-100837. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: (+44)1223-336-033; e-mail: deposit@ccdc.cam. ac.uk).