| A new kind of analyzer crystal for X-ray spectroscopy synthesized by low-molecular-weight acid and long-chain aliphatic alcohol was found. It should be possible to tailor the 2d spacing to virtually any desired value, by varying the alcohol or acid chain length. Tetradecyl Hydrogen Maleate (THM) ,Hexadecyl Hydrogen Maleate,Eicosyl Hydrogen Maleate (EHM) belong to this new kind crystal. They are ideal as an ultrasoft X-ray dispersing crystal . In this paper , firstly, we have synthesized the THM ,HHM,EHM. Then we did the themel analysis of these crystal. IR and XRD properties of these cystal were also investagted. The single crystal of THM and EHM were grown from solution by the method of lowering solution temperature. We got THM singal crystal which size is 40×25×2.5mm~3 and EHM singal crystal which size is 30×25×0.5mm~3. In order to obtain large, good quality of singal crystals, nucleation in supersaturated solution of EHM has been investigated in this paper. The nucleation rate as indicated by induction period are measured. The effects of temperature,supersaturation on the nucleation rate in non-agitated system are reported. The interfacial tension,energy of formation and critical radius of muclei crystal are calculated based on classical nucleation theory. From singal crystal structure analysis. We found HHM belongs to triclinic crystal system,P1|-space group with a=5.4330(10),b=6.8510(7), c=29.5650(4)A|°, α=94.8210(12)°, β=93.835(9)°,γ=103.258(8)°, Z =2, V =1063.1(2)A|°3. |