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Hydrothermal Synthesis and Crystal Structure of Zn4(PO4)2(HPO4)2·0.5(C10H28N4)·2H2O, a New Layered Zinc Phosphate with 12-Ring Cavities

✍ Scribed by Ping Zhang; Yue Wang; Guangshan Zhu; Zhan Shi; Yunling Liu; Hongming Yuan; Wenqin Pang

Publisher
Elsevier Science
Year
2000
Tongue
English
Weight
232 KB
Volume
154
Category
Article
ISSN
0022-4596

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✦ Synopsis

Using 1, 4, 8, 11-tetraazacyclotetradecane (cyclam) as a template, a new layered zinc phosphate Zn 4 (PO 4 ) 2 (HPO 4 ) 2 ' 0.5(C 10 H 28 N 4 ) ' 2H 2 O (de5ned as ZnPO-cyclam) with 12-ring cavities was synthesized under hydrothermal conditions in a molar ratio ZnO:P 2 O 5 :cyclam:H 2 O ‫؍‬ 1:2.2:0.5:284.7 at 1403C for 3 days. The gel had a pH 4 at the starting period. The ZnPO-cyclam crystal structure is solved using single-crystal X-ray di4raction data at 293 K. It crystallizes in monoclinic space group P2 1 /c (no.14) with lattice parameters a ‫؍‬ 15.758(3) A s , b ‫؍‬ 9.0292(15) A s , c ‫؍‬ 15.543(3) A s , ‫؍‬ 111.070 (16). V ‫؍‬ 2063.7(7) A s 3 , Z ‫؍‬ 4, R ‫؍‬ 0.0392, wR ‫؍‬ 0.0472, 4166 collected re6ections, 2794 observed re6ections with I > 2 (I). The structure of ZnPO-cyclam consists of alternating inorganic and organic layers. The inorganic layers are built up from ZnO 4 , ZnO 3 (H 2 O) 2 , PO 4 , and HPO 4 with Zn+O+Zn and Zn+O+P bonds. The protonated cyclam molecules in which the four nitrogen atoms are all protonated form the organic layers. Strong hydrogen bonding exists between the inorganic+organic layers, and there are 12-ring cavities in the inorganic layers, in which the template cyclam molecules reside.

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