METAL COMPLEXES OF POLYCYCLIC TERTIARY AMINES. PART VI. PREPARATION AND CRYSTAL STRUCTURE OF HEXAMETHYLENETETRAMINE-SILVER(I) BROMIDE (1/4)

<正> C6H12N4Br4Ag4,Mr = 891.31, orthorhombic, Pnma, a = 8.778(2),b = 9.80.5(2), c = 16.906(3) A, V = 1455.1(4) A3, Z = 4, Dx = 4.069, Dm (displacement of H2O) = 4.03 g cm-3 , A(Mo-Ka) = 161.3 cm-1 , F(OOO) = 1615.77,T = 295°, final R = 0.052 arid Rw = 0.062 for 1472 observed reflections.All four lone pairs of each (CH2)6N4 molecule serve as ligand sites in a polymeric framework comprising octahedral AgBr5N, tetrahedral AgBr3N, and tetragonal pyramidal AgBr4N coordination polyhedra. The Ag-N and Ag-Br bond lengths lie in the ranges 2.366(12)-2.454(12) and 2.640(2)-3.178(2) A, respectively.     

砷偶氮Ⅲ用作鈦的分析试剂——Ⅰ.鈦(Ⅳ)的检定

砷偶氮Ⅲ与釱(Ⅳ)在硫酸溶液中形成紫色絡合物。此反应可用于舦的检定,其灵敏度較常用的过氧化氫法为高。检出限为0.25微克Ti,稀度限1:200,000。在检定釱的反应条件下,有多种离子干扰,其界限比均分別求出。如应用适当的隐蔽剂和(或)分离可避免其影响。     

METAL COMPLEXES OF POLYCYCLIC TERTIARY. AMINES. PART VIII. SYNTHESIS AND CRYSTAL STRUCTURE OF 1,4-DIAZABICYCLO[2.2.2]OCTANEPENTACARBONYLMOLYBDENUM(0), (CH_2)_6N_2·Mo(CO)_5

<正> C11H12N2MoO5, Mr = 348.17, orthorhombic, space group p212121,a= 7.048(1), b = 11.060(4), c = 18.039(7) A, V = 1406.2(8) A3, Z = 4, D x=1.645, Dm = 1.61 (flotation in aqueous KI) g cm-3 , graphite-monochromatizedMo-Kα,λ = 0.71069 A, μ = 9.25 cm-1, F(OOO) = 695.73, T = 295°K, final RF =0.035 and RwF2 = 0.051 for 1335 observed reflections with |F0| > 3σ(|F0|). The measured molecular dimensions.reflect the trans influence and steric bulk of the organic cage ligand.     

含全碳和多炔阴离子配体的银簇化合物的超分子组装及其结构研究

总结了我们在新型炔银簇化合物研究方面的最新进展. 这些化合物分为以下几种类型: (a)1,3,5-己三炔基和1,3,5,7-辛四炔基; (b)1,5-己二炔基; (c)经膦酸配体组装的乙炔基和烷基乙炔基; (d)苯乙炔基、 环烷基乙炔基和含氮杂环基乙炔基结构单元的银簇化合物; (e)经不同类型的银-碳配位键连接, 并进一步通过分子内/分子间作用力稳固其配位网络的炔银化合物. 我们还进一步讨论了溶剂、 配体的位阻大小和辅助配体类型对于多维配位网络结构的影响.     

CRYSTAL STRUCTURES OF 1,2-BENZO[2.2]PARACYCLOPHANE AND 1,2-BENZO[2.2]PARACYCLOPHANE-1,7-DIENE

<正> C20H16 (1) Mr = 256.34 and C20H14 (2), Mr = 254.32 are isomorphous, orthorhombic, P212121, Z = 4. For (?), ?a= 7.116(1), b =7.874(2), c = 24.564(4) A, V = 1376.4(3) A3, Dx = 1.237 g cm-3, μ(Mo-K α) =0.65 cm-1 , final R = 0.047 for 1152 observed reflections; for 2, a=6.963(2), b = 7.985(4), c = 24.315(8) A, V = 1351.9(8) A3, Dx = 1.250 g cm-3,μ(Mo-Kα) = 0.66 cm-1 , final R = 0.076 for 886 observed data. Structuralfeatures are similar to those of the parent [2.2]paracyclophane and related derivatives.