Merrill Crystal A, Cheetham Anthony K
Materials Research Laboratory, University of California, Santa Barbara, California 93106-5121, USA.
Inorg Chem. 2007 Jan 8;46(1):278-84. doi: 10.1021/ic0618302.
The reaction of nickel, cobalt, and manganese with 1,2-ethylenediphosphonic acid or 1,2-ethylenediphosphonic acid and 1,10-phenanthroline under hydrothermal conditions resulted in the pillared layered structures Co2(H2O)2(O3PC2H4PO3) (I) and Ni2(H2O)2(O3PC2H4PO3) (II), which are isostructural to a zinc phase that has previously been characterized by X-ray powder methods. In addition, a 1D chain structure, Mn(HO3P(CH2)2PO3H)(H2O)2(C12H8N2) (III), and a pillared layered structure, Mn(HO3P(CH2)2PO3H) (IV), were obtained. The structures of these phases were solved by single-crystal X-ray diffraction methods. The crystallographic data are as follows: compound I P21/n (No. 14), a = 5.6500(11) A, b = 4.7800(10) A, c = 15.330(3) A, beta = 98.50(3) degrees, V = 409.47(14) A3, Z = 2; compound II P21/n (No. 14), a = 5.5807(11) A, b = 4.7205(9) A, c = 15.250(3) A, beta = 98.55(3) degrees, V = 397.28(13) A3, Z = 2; compound III C2/c (No. 15), a = 12.109(2) A, b = 15.328(3) A, c = 9.848(2) A, beta = 108.88(3) degrees, V = 1729.5(6) A3, Z = 4; compound IV P (No. 2), a = 5.498(5) A, b = 7.715(6) A, c = 8.093(7) A, alpha = 82.986(12) degrees, beta = 75.565(12) degrees, gamma = 80.582(12)degrees, V = 326.7(5) A3, Z = 2. Magnetic measurements show antiferromagnetic behavior below TN = 7 K for I and 13 K for II.
镍、钴和锰与1,2 - 乙二膦酸或1,2 - 乙二膦酸和1,10 - 菲咯啉在水热条件下反应,生成了柱撑层状结构Co₂(H₂O)₂(O₃PC₂H₄PO₃)(I)和Ni₂(H₂O)₂(O₃PC₂H₄PO₃)(II),它们与先前通过X射线粉末法表征的一种锌相结构相同。此外,还得到了一维链状结构Mn(HO₃P(CH₂)₂PO₃H)(H₂O)₂(C₁₂H₈N₂)(III)和柱撑层状结构Mn(HO₃P(CH₂)₂PO₃H)(IV)。这些相的结构通过单晶X射线衍射法解析。晶体学数据如下:化合物I,P21/n(编号14),a = 5.6500(11) Å,b = 4.7800(10) Å,c = 15.330(3) Å,β = 98.50(3)°,V = 409.47(14) ų,Z = 2;化合物II,P21/n(编号14),a = 5.5807(11) Å,b = 4.7205(9) Å,c = 15.250(3) Å,β = 98.55(3)°,V = 397.28(13) ų,Z = 2;化合物III,C2/c(编号15),a = 12.109(2) Å,b = 15.328(3) Å,c = 9.848(2) Å,β = 108.88(3)°,V = 17,29.5(6) ų,Z = 4;化合物IV,P(编号2),a = 5.498(5) Å,b = 7.715(6) Å,c = 8.093(7) Å,α = 82.986(12)°,β = 75.565(12)°,γ = 80.582(12)°,V = 326.7(5) ų,Z = 2。磁性测量表明,对于I,在TN = 7 K以下表现出反铁磁行为;对于II,在TN = 13 K以下表现出反铁磁行为。