Structure of bis(ethylenediamine)palladium(II) dichlorobis(ethylenediamine)palladium(IV) tetraperchlorate and remarks concerning the structures of analogous mixed-valence platinum compounds
Structure of bis(ethylenediamine)palladium(II) dichlorobis(ethylenediamine)palladium(IV) tetraperchlorate and remarks concerning the structures of analogous mixed-valence platinum compounds
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双(乙二胺)钯(II)二氯双(乙二胺)钯(IV)四高氯酸盐的结构及类似混合价铂化合物的结构备注
DOI：
10.1107/s0567740882005202
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发表时间：
1982
期刊：
影响因子：
--
通讯作者：
T. Theophanides
中科院分区：
文献类型：
--
作者：
A. Beauchamp;D. Layek;T. Theophanides
[Pd（C2 HsN 2）2] [Pd（C2 HsN 2）2Cl 2]（ClO 4）4，CsH 32 Cl 2 NsPd~+.4ClO ~ -，正交晶系，空间群Ibam，a = 9.665（2），B = 13.636（3），c = 10.715（7）A，Z = 2[Pd（en）2][PdCle（en）z]（ClO 4）4个晶胞单元（en =乙二胺，NHeCH 2CHeNH 2）。该结构在Ibam空间群中求解，并对573个非零反射进行了改进，得到了0.033的常规R因子。该晶体包含无限堆叠的大致平面的Pd（en）2单元垂直于链轴，并由卤素桥接。桥连明显是不对称的[Pd-Cl = 2.324（3）和3.033（3）A]，导致四配位Pd”物质与反式八面体Pd IV基团沿链沿着交替。链被平行于ac平面的CIO 4离子片在y ~ 1/4和~3/4处分开。每个C10-阴离子是 * 别名：链-N-氯-双（乙二胺）钯（II，IV）四高氯酸盐。0567-7408/82/041158-07501.00通过使用其两个氧原子桥接连续的Pd（en）2单元以与配位的乙二胺形成H键。阴离子被发现在两个无序的方向不同的相互作用与其余的结构。沿着c轴安装的晶体振荡图中奇数层线的正常布拉格衍射点下存在漫射背景表明，桥连卤素在沿沿着链轴的两个位置上是无序的，这通常见于类似的卤素桥连Ptn-Pt IV混合价络合物。
[Pd(C2HaNz)2] [Pd(C2HsN2)2CI2] (CIO4)4, CsH32C12 NsPd~+.4CIO~ -, is orthorhombic, space group Ibam, a = 9.665 (2), b = 13.636 (3), c = 10.715 (7) A, Z = 2[Pd(en)2][PdCle(en)z](CIO4) 4 units per cell (en = ethylenediamine, NHeCH2CHeNH2). The structure was solved in space group Ibam and refined to a conventional R factor of 0.033 for 573 nonzero reflections. The crystal contains infinite stacks of roughly planar Pd(en)2 units perpendicular to the chain axis and bridged by the halogens. Bridging is clearly unsymmetrical [Pd-CI = 2.324 (3) and 3.033 (3)A], leading to four-coordinate Pd" species alternating with trans octahedral Pd Iv groups along the chain. The chains are separated by sheets of CIO4 ions parallel to the ac plane at y ~ 1/4 and ~3/4. Each C10~ anion is * Alternative name: catena-/J-chloro-bis(ethylenediamine)palladium(II, IV) tetraperchlorate. 0567-7408/82/041158-07501.00 bridging successive Pd(en)2 units by using two of its oxygen atoms to form H bonds with coordinated ethylenediamine. The anion is found in two disordered orientations differing by their interactions with the rest of the structure. The presence of diffuse background under the normal Bragg diffraction spots for the odd layer lines in the oscillation diagram of the crystal mounted along the c axis indicates that the bridging halogens are disordered over two sites along the chain axis, as is usually found for similar halide-bridged Ptn-Pt Iv mixed-valence complexes.