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Kristallstruktur des supramolekularen Silber(I)thiocyanate-Cyclam-Komplexes [Ag(SCN).(C10H24N4)1/2] 硫氰酸银-环糊精超分子配合物[Ag(SCN).(C10H24N4)1/2]的晶体结构
IF 0.8 4区 化学 Pub Date : 1994-01-01 DOI: 10.14279/DEPOSITONCE-7637
J. Pickardt, Jing Shen
Colourless crystals of the 1,4,8,11-tetraazacyclotetradecane (cyclam) silver(1) thiocyanate complex [Ag(SCN).(C 10 H 24 N 4 ) 1/2 ] were obtained by diffusion of a solution of cyclam in ethanol into an aqueous solution of K[Ag(SCN) 2 ]. The crystals are tetragonal, space group P4 2 /n, Z=8, a=b=1256.0(4), c=1185.5(9) pm. The SCN groups act as μ 3 ligands, the S atoms of two SCN groups bridge two neighbouring Ag ions, which are only 297.5 pm apart, forming butterfly-like Ag 2 S 2 moieties, the N atoms of the SCN groups form bonds to Ag atoms of adjacent Ag 2 S 2 moieties
1,4,8,11-四氮杂环十四烷(cyclam)银(1)硫氰酸盐配合物[Ag(SCN)]的无色晶体。(c10h24n4) 1/2]是通过将环环霉素在乙醇中的溶液扩散到K[Ag(SCN) 2]水溶液中得到的。晶体呈四边形,空间群P4 2 /n, Z=8, a=b=1256.0(4), c=1185.5(9) pm。SCN基团作为μ 3配体,两个SCN基团的S原子桥接两个相距仅297.5 pm的相邻Ag离子,形成蝴蝶状的Ag 2 S 2基团,SCN基团的N原子与相邻Ag 2 S 2基团的Ag原子形成键
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引用次数: 0
Silaheterocyclen. XXVII: Substituenteneffekte zur Steuerung des Cycloadditionsverhaltens von Silaethenen Silaheterocyclen .3vii:来控制锡拉因的合成活动的替代效应
IF 0.8 4区 化学 Pub Date : 1994-01-01 DOI: 10.1515/znb-1994-0618
N. Auner, C. Wagner, W. Ziche
The silence Cl 2 Si=C(Ph)CH 2 Bu t (2) is formed by the reaction of 1,1,1-trichloro-2-phenyl-1-silaprop-2-ene (1) with LiBu t in n-pentane in the temperature range from -15 to 0 o C. The reaction initially leads to the corresponding α-lithio adduct A (addition of LiBu t to the vinyl group of 1); subsequent LiCl elimination yields 2 as an intermediate. 2 can be trapped by Me 3 SiOMe (3) and dienes which add across the Si=C bond. In the absence of trapping agents but in the presence of the Lewis base NEt 3 the mixture 1/LiBu t reacts to give the disilacyclobutane 4
在正戊烷中,1,1,1-三氯-2-苯基-1-硅丙烯(1)在-15 ~ 0℃的温度范围内与LiBu -t反应形成沉默的Cl - Si=C(Ph) ch2 - Bu -t(2),反应初期生成相应的α-锂加合物A (LiBu -t加成到1的乙烯基上);随后的氯化锂消除产生2作为中间体。2可以被me3siome(3)和在Si=C键上添加的二烯所捕获。在没有捕集剂但有路易斯碱NEt 3的情况下,混合物1/LiBu t反应生成二环丁烷4
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引用次数: 0
Kristallstrukturen der [2.2.2]Cryptate [Cd(cryptand 222)][CdCl4] und [Hg(cryptand 222)][Hg2Cl6] mit achtfach koordinierten Metallionen [关于合成的][Cd(水晶要222)[cd4和[Hg(水晶要222]][Hg2Cl6
IF 0.8 4区 化学 Pub Date : 1994-01-01 DOI: 10.14279/DEPOSITONCE-7634
J. Pickardt, Britta Kühn
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引用次数: 0
Kristallstruktur des „supramolekularen“ Quecksilber(II)chlorid-thiocyanat- Hexamethylentetramin-Addukts Hg(SCN)2 · 2HgCl2 · 2C6H12N4 “超分子”氯化硫氰酸汞-六亚甲基四胺加合物Hg(SCN)2·2HgCl2·2C6H12N4的晶体结构
IF 0.8 4区 化学 Pub Date : 1994-01-01 DOI: 10.14279/DEPOSITONCE-7636
J. Pickardt, Gill-Taik Gong, D. Röleke
Crystals of the adduct Hg(SCN) 2 -2 HgCl 2 -2 C 6 H 12 N 4 were obtained from an aqueous solution containing 0.1 mol/l hexamethylenetetramine and 0.05 mol/l potassium thiocyanate and mercury(II) chloride. The compound crystallizes monoclinically; space group P 2 1 /n, a= 767.3(4), b=1854.7(7), c=872.5(7) pm, and β=101.48(5) o . The structure consists of a network of chains -Cl-Hg-Cl-Hg- and -(Cl-Hg-) 2 NCS-Hg-SCN-(Hg-Cl) 2 - which share common Hg atoms and form distorted hexagonal and trigonal channels. The hexamethylenetetramine molecules lie in the hexagonal channels
在含有0.1 mol/l六亚甲基四胺和0.05 mol/l硫氰酸钾和氯化汞的水溶液中,得到了Hg(SCN) 2 -2 HgCl 2 -2 c6h12n4的加合物晶体。该化合物单临床结晶;空间群P =1 /n, a= 767.3(4), b=1854.7(7), c=872.5(7) pm, β=101.48(5) o。该结构由链-Cl-Hg-Cl-Hg-和-(Cl-Hg-) 2 NCS-Hg-SCN-(Hg- cl) 2 -组成,它们共享共同的Hg原子,形成扭曲的六边形和三角形通道。六亚甲基四胺分子位于六边形通道中
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引用次数: 0
Flexible ein-und zweikernige Aralkyl-und Aralkoxyquecksilberverbindungen als Modelle zum Nachweis von Hg(II)-Hg(II)-W echselwirkungen / Flexible Mono-and Dinuclear Aralkyl and Aralkoxy Mercury Compounds for Detection of Hg (II)-Hg (II) Interactions Hg(II)-Hg(II)-W echselwirkungen /单核和双核芳烷基和芳烷氧基汞化合物检测Hg(II)-Hg(II)相互作用
IF 0.8 4区 化学 Pub Date : 1992-01-01 DOI: 10.1515/znb-1992-0306
Hans-Jürgen Öller, P. Kiprof, H. Schmidbaur
The aralkyl and aralkoxy mercury(II) compounds 1-(chloromercury(II)methyl)naphthalene (1), bis[1-naphthylmethyl]mercury(II) (2), 1-naphthyl(1-naphthylmethyl)mercury(II) (3), 1,8-bis[chloromercury(II)methyl]naphthalene (4), methylmercury(II)-benzylate (5), methylmercury( II)-1-naphthylmethylate (6) and bis[methylmercury(II)]μ-1,8-naphthalenediyl-bismethylate (7) have been prepared and characterized by means of NMRspectroscopy, mass spectrometry and elemental analysis. The molecular structure of compound 2 has been determined by single X-ray crystallography. The unit cell of 2 contains two crystallographically independent molecules, one of which is disordered. The interatomic distances and angles meet the expectations with Hg ⋯ Hg separations larger than 5.60 Å, indicating the absence of metal metal interactions.
制备了芳烷基和芳烷氧基汞(II)化合物1-(氯汞(II)甲基)萘(1)、二[1-萘甲基]汞(II)(2)、1-萘甲基(1-萘甲基)汞(II)(3)、1,8-二[氯汞(II)甲基]萘(4)、甲基汞(II)-苄基酸盐(5)、甲基汞(II)- 1-萘甲基化盐(6)和二[甲基汞(II)]μ-1,8-萘二基双甲基化盐(7),并用核磁共振光谱、质谱和元素分析对其进行了表征。化合物2的分子结构已用单x射线晶体学测定。2的单晶胞包含两个晶体学上独立的分子,其中一个是无序的。原子间距离和角度符合预期,汞⋯⋯汞分离大于5.60 Å,表明不存在金属间相互作用。
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引用次数: 0
Calcium-bis{[tris(trimethylsilyl)silyl]tellanid} · 4 THF : Synthese, spektroskopische Charakterisierung und Struktur Calcium-bis{[去吧(trimethylsilyl) silyl] tellanid·4 THF:合成、spektroskopische特性和结构
IF 0.8 4区 化学 Pub Date : 1992-01-01 DOI: 10.18419/OPUS-1299
G. Becker, K. Klinkhammer, W. Schwarz, M. Westerhausen, T. Hildenbrand
Calcium bis {[tris(trimethylsilyl)silyl]tellanide} · 4THF is obtained by metallation of tris(trimethylsilyl)silyl)tellane using dimeric calcium bis[bis(trimethylsilyl)amide] in toluene, followed by recrystallisation from tetrahydrofuran. The compound is characterized by a remarkable highfield shift of the 1 2.5 Te{1H}-NMR resonance (-2204 ppm vs. Me2Te). The X-ray structure determination (triclinie, pI; Z = 1; a = 1042.6(2), b = 995.7(2), c = 1379.6(3) pm; α= 90.06(2), β= 92.76(2),), γ= 94.03(2)° at -100 "C) shows a distorted octahedral coordination sphere of the calcium atom (Ca-Te 319; Ca-O 236 and 241 pm). The two [tris(trimetbylsilyl)silyl}-tellanide ligands are in a trans position; the angle Ca-Te-Si is widened to 129°.
用二聚体钙二[二(三甲基硅基)酰胺]在甲苯中金属化三(三甲基硅基)硅基碲化钙二{[三(三甲基硅基)硅基]碲化钙}·4THF,然后由四氢呋喃重结晶。该化合物具有显著的1.25 Te{1H}-NMR共振高场位移(-2204 ppm vs. Me2Te)。x射线结构测定(三线,pI;Z = 1;A = 1042.6(2), b = 995.7(2), c = 1379.6(3) pm;α= 90.06(2), β= 92.76(2),), γ= 94.03(2)°(-100”C),表明钙原子(Ca-Te 319;Ca-O 236和241 pm)。两个[三(三甲基硅基)硅基}-碲化物配体处于反位;Ca-Te-Si角加宽至129°。
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引用次数: 0
Neue Sesquisulfide der Lanthanoide im U2S3-typ: Tb2Si3 und Dy2S3 硫化物新型硫化物:t2si3与Dy2S3
IF 0.8 4区 化学 Pub Date : 1992-01-01 DOI: 10.15488/2449
T. Schleid
New sesquisulfides o f the lanthanides with the U 2 S3-type structure (M 2 S3, M = T b and Dy) were prepared through the oxidation o f T bC lH 0 67 and D yCl2, respectively, with appropriate am ounts o f sulfur in the presence o f N aCl fluxes in silica protected sealed tan talum containers at 850 C for at least seven days. The preparation from the elements (2M + 3S; M = Tb and Dy) under otherwise analogous reaction conditions and tem peratures was also successful when equim oiar fluxes o f NaCl were applied. The crystal structure was determ ined from single crystal da ta for Tb-,S3 and Dy2 S3, both crystallizing with the U-,S3-type structure (orthorhom bic, Pnm a, Z = 4; T b 2 S3: a = 1067.87(8), b = 388.06(4), c = 1049.07(7) pm; Dy 2 S3: a = 1062.45(7), b = 386.59(4), c = 1044.36(8) pm) when prepared under the above-m entioned conditions.
在有N - aCl助熔剂存在的情况下,分别用tbc lh67和dycl2氧化法制备了具有u2s3型结构(m2s3, M = t_b和Dy)的镧系元素的新倍半硫化物,并在850℃的硅保护密封钽容器中放置了至少7天。从元素(2M + 3S;M = Tb和Dy)在其他类似的反应条件和温度下也成功地应用了等量的NaCl。通过单晶数据确定了Tb-、S3和Dy2 S3的晶体结构,两者均结晶为U-、S3型结构(正交立方,Pnm a, Z = 4;T b 2 S3: a = 1067.87(8), b = 388.06(4), c = 1049.07(7) pm;在上述条件下制备Dy 2 S3: a = 1062.45(7), b = 386.59(4), c = 1044.36(8) pm。
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引用次数: 0
Die Reaktionen von Wolframhexachlorid mit überschüssigem 2,2-Dimethylpropylidinphosphan : die Kristallstrukturen von WCl5P2(C5H9)3, WCl4P5(C5H9)5 und [C3(C4H9)3]+[WCl5(C4H9C≡CC4H9]- Wolframhexachlorid的反应应将2,2-Dimethylpropylidinphosphan: Kristallstrukturen WCl5P2 (C5H9) 3、WCl4P5 (C5H9) 5 [C3 (C4H9) 3] + [WCl5 (C4H9C≡CC4H9]——
IF 0.8 4区 化学 Pub Date : 1991-01-01 DOI: 10.18419/OPUS-7391
F. Weller, I. Pauls, K. Dehnicke, G. Becker
The reaction of tungsten hexachloride with excess 2,2-dimethylpropylidynephosphane, C 4 H 9 -C≡P, leads to the tungsten phosphaalkyne clusters WCl 5 P 2 (C 5 H 9 ) 3 and WCl 4 P 5 (C 5 H 9 ) 5 , as well as to the tris(t-butyl)cyclopropenium pentachloro tungsten alkyne complex [C 3 (C 4 H 9 ) 3 ] + [WCl 5 (C 4 H 9 C≡CC 4 H 9 )] − . All complexes were characterized by X-ray structure determinations
六氯化钨的反应2,过剩2-dimethylpropylidynephosphane, 4 H 9 C - C≡P,导致钨phosphaalkyne集群水控制法5 P 2 (C 5 H 9) 3和水控制法4 P (C 5 H 9) 5,以及三羟甲基氨基甲烷(叔丁基)cyclopropenium五氯液钨炔复杂[C 3 (C 4 H 9) 3] +[水控制法5 (4 H 9 C≡CC 4 H 9)]−。所有配合物均通过x射线结构测定进行了表征
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引用次数: 0
Synthese und Struktur aminosubstituierter Tetraphosphetane 合成和结构单元
IF 0.8 4区 化学 Pub Date : 1991-01-01 DOI: 10.18419/OPUS-7960
R. Appel, D. Gudat, E. Niecke, M. Nieger, C. Porz, H. Westermann
A number of aminotetraphosphetanes could be obtained by reductive dehalogenation of dichlorophosphines with magnesium as well as by elimination of chlorotrimethylsilane from vicinal chlorosily-functionalized biphosphines and from [2+2]-cyclodimerization of aminodiphosphenes, respectively. The molecular structures of several tetraphosphetanes are reported and discussed. The torsion-angle of the four-membered rings varies from 22,5 to 45,7 depending on the size und electronegativity of the exocyclic ligands.
用镁对二氯膦进行还原脱卤反应,用相邻氯硅官能化的二膦和氨基二膦的[2+2]环二聚化反应去除氯三甲基硅烷,可以得到大量的氨基四膦。报道并讨论了几种四磷酸烷的分子结构。根据外环配体的大小和电负性,四元环的扭转角在22,5 ~ 45,7之间变化。
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引用次数: 0
Alkoxigermanate(II), -stannate(II) und -plumbate(II) zweiwertiger Metallionen. - I 二价金属离子的烷氧基海纳酸盐(II)、-锡酸盐(Ⅱ)和-铅酸盐(II)-我
IF 0.8 4区 化学 Pub Date : 1991-01-01 DOI: 10.22028/D291-22554
M. Veith, Johannes Hans, Lothar Stahl, P. May, V. Huch, Angelika Sebald
Bis(tri-tert-butoxigernanates), -stannates and -plumbates of Mg, Sr, Ba, Cd, Eu and Pb have been synthesized by various procedures from starting materials such as sodium tri-tert-butoxigermanate and -plumbate and other analogous compounds
以三叔丁酸钠、铅酸钠及其它类似化合物为原料,通过各种方法合成了镁、锶、钡、镉、铕和铅的双(三叔丁酸盐)、-锡酸盐和-铅酸盐
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引用次数: 2
期刊
Zeitschrift Fur Naturforschung Section B-A Journal of Chemical Sciences
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