Synthesis and structure determination from an extremely small single crystal of a new layered gallium phosphate

Three one-dimensional zinc phosphates, [C5N2H14][Zn(HPO4)2], I, [C10N4H26][Zn (HPO4)2].2H2O II, and [C4N2H6]2[Zn(HPO4)], III, have been prepared employing hydro/solvothermal methods in the presence of organic amines. While I and II consist of linear chains of corner-shared four-membered rings, III is a polymeric wire where the amine molecule is directly bonded to the metal center. The wire, as well as the chain in these structures, are held together by hydrogen bond interactions involving the amine and the framework oxygens. The polymeric zinc phosphate with wire-like architecture, III, is only the second example of such architecture. Crystal data: I, monoclinic, P21/c (no. 14), a=8.603(2), b=13.529(2), c=10.880(1) ?, (beta)=94.9(1)°, V=1261.6(1) ?3, Z= 4, (rho)calc.=1.893gcm-3, µ(MoK(alpha))=2.234mm-1, R1=0.032, wR2=0.086, [1532 observed reflections with I>2(sigma)(I)], II, orthorhombic, Pbca (no. 61), a=8.393(1), b=15.286(1), c=22.659(1) ?, V=2906.9(2) ?3, Z=8, (rho)calc.=1.794gcm-3, µ(MoK (alpha))=1.957mm-1, R1=0.055, wR2=0.11, [1565 observed reflections with I>2(sigma) (I) and III, monoclinic, P21/c (no. 14), a=8.241(1), b=13.750(2), c=10.572(1) ?, (beta) =90.9(1)°, V=1197.7(2) ?3, Z=4, (rho)calc.=1.805gcm-3, µ(MoK(alpha))=2.197mm-1, R1 =0.036, wR2=0.10, [1423 observed reflections with I>2(sigma)(I)].