CdI_2与TSC加成物的合成及结构

Synthesis and Structure of the Addition Product of Cadmium Iodide and Thiosemicarbazide

ＣｄＩ２与ＴＳＣ在丙酮溶剂及水中形成加成物ＣｄＩ２（Ｃ４Ｈ１０Ｎ３Ｓ）２·Ｈ２Ｏ，晶体属单斜晶系，空间群为Ｐ２１／ｍ．晶胞参数为ａ＝０．７５３３（３）ｎｍ，ｂ＝１．５３５（２）ｎｍ，ｃ＝０．８４３７（２）ｎｍ，β＝９０．９１（３）°，ｖ＝０．９７６（１）ｎｍ３，Ｍｒ＝６４８．６４，Ｚ＝２，Ｄｃ＝２．２０ｇ·ｃｍ－３，μ（ＣｕＫα）＝４４．５８ｃｍ－１，Ｆ（０００）＝６０８，Ｔ＝２９７Ｋ．用１６２２个Ｉ≥３σ（Ｉ）独立衍射精修结构，最终偏差因子Ｒ＝０．０５７，晶体中存在分离的单核络合物ＣｄＩ２（Ｃ４Ｈ１０Ｎ３Ｓ）２·Ｈ２Ｏ，Ｃｄ原子呈畸变四面体配位．两个Ｃｄ－Ｉ和Ｃｄ－Ｓ键长分别为０．２７３０ｎｍ，０．２７４３ｎｍ和０．２５７５ｎｍ．

An addition product Cd 2(C 4H 10 N 3S) 2·H 2O is synthesized from cadmium iodide and thiosemicarbazide (TSC) in the solvent of acetone and water. Its crystal belongs to monoclinic system, with a space group of P2 1/m. The cell parameters include: a =0.753 3(3) nm, b =1.535 0(2) nm, c =0.843 7(2) nm, β =90.91(3)°, v =0.976(1) nm 3, M r =648.64, Z =2, D c=2.20 g·cm -3 , μ (CuK α)=44.58 cm -1 , F (000)=608, T =297 K. To modify precisely the crystal structure by 1622 independent diffractions where I≥3(I ), a final deviation factor R =0.057 is ensured. There exists in crystal a separate mononuclear complex CdI 2(C 4H 10 N 3S) 2·H 2O, where Cd atoms assume a distorted tetrahedral coordination. There are two Cd-I bonds and a Cd-S bond with their repective length of 0.273 0 nm,0.274 3 nm and 0.257 5 nm.