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Two New 1,3-Diammonium-Propane Zinc Hydrogen Phosphates: H3N(CH2)3NH3·Zn2(HPO4)2(H2PO4)2, with 12-Ring Layers, and H3N(CH2)3NH3·Zn(HPO4)2, with 4-Ring Ladders

✍ Scribed by William T.A. Harrison; Zsolt Bircsak; Lakshitha Hannooman; Zhenghua Zhang

Publisher
Elsevier Science
Year
1998
Tongue
English
Weight
312 KB
Volume
136
Category
Article
ISSN
0022-4596

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✦ Synopsis

The solution-mediated syntheses, single-crystal structures, and some physical properties of the first 1,3-diammonium-propane zinc phosphates, H 3 N(CH 2 ) 3 NH 3 • Zn 2 (HPO 4 ) 2 (H 2 PO 4 ) 2 and H 3 N(CH 2 ) 3 NH 3 • Zn(HPO 4 ) 2 , are described. Both phases contain vertex-sharing ZnO 4 and (H 2 /H)PO 4 tetrahedra, accompanied by doubly protonated organic cations. H 3 N(CH 2 ) 3 NH 3 • Zn 2 (HPO 4 ) 2 (H 2 PO 4 ) 2 consists of a layered motif of infinite sheets of tetrahedral 12-rings, whereas H 3 N(CH 2 ) 3 NH 3 • Zn(HPO 4 ) 2 is strongly one-dimensional and consists of tetrahedral 4-ring ''ladders.'' Crystal data:

14), a ‫؍‬ 15.056(2) A s , b ‫؍‬ 7.8454(8) A s , c ‫؍‬ 16.344(2) A s , ‫؍‬ 115.469(8)°, V ‫؍‬ 1742.9(3) A > , Z ‫؍‬ 4, R(F) ‫؍‬ 5.17%, R (F) ‫؍‬ 5.68% [2859 observed reflections with I ‫؍‬ 3 (I )]; H 3 N(CH 2 ) 3 NH 3 • Zn(HPO 4 ) 2 , M r ‫؍‬ 333.48, orthorhombic, space group P2 1 2 1 2 1 (No. 19), a ‫؍‬ 5.2206(7) A s , b ‫؍‬ 12.717(2) A s , c ‫؍‬ 15.570(2) A s , V ‫؍‬ 1033.7(3) A > , Z ‫؍‬ 4, R(F) ‫؍‬ 4.16%, R (F) ‫؍‬ 3.75% [1491 observed reflections with I > 3 (I)].

1998 Academic Press

Physical Characterization

Powder X-ray data for well-ground, white powder samples of the title compounds were collected on a Siemens D5000 automated powder diffractometer [CuK radiation, "1.54178 A s , ¹"25(2)°C]. A software ''stripping'' and peak-fitting routine established peak positions relative to CuK ( "1.54056 A s ), and hkl indices were assigned by comparison with LAZY-PULVERIX ( 14) simulations of the single-crystal structures (vide infra). The least-squares refinements were performed by using the program UNITCELL 93

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