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Biologia

九的原子Deltahedral Zintl离子锗和他们的官能合成有机基团

Published: February 11, 2012
doi:
10.3791/3532
,
1Department of Chemistry and Biochemistry,University of Notre Dame

Summary

我们提出的K高温金属间化合物的前体的合成<sub> 4</sub> GE<sub> 9</sub>，他们在解散乙二胺形成GE<sub> 9</sub<sup> 4 -</sup> deltahedral Zintl离子，炔集群的反应形成有机Zintl离子。后者的特点是通过电质谱解决方案，并通过单晶X-射线衍射固态。

Abstract

虽然1890年代末和1930年初的Zintl离子之间的日期最初的研究，他们并没有结构上的特点，直到多年以后。1,2它们的氧化还原化学是更年轻的，只是10岁，但尽管这短暂的历史这些离子deltahedral的集群北京时间9 N-（C =硅，锗，锡，铅，N = 2，3，4）。3-6已经显示出有趣的和多样化的反应，并已在迅速发展和令人振奋的新化学前沿的著名的里程碑9月 4锗的氧化耦合–低聚物和无限链，7-19金属化，14-16,20-25集群过渡金属有机碎片，26-34过渡金属原子插入在中心封顶有时被封盖和齐聚，除了主族有机金属碎片外保税取代35-47结合的产业集群，48-50和官能与各种有机残留物与有机卤化物和炔烃的反应。51-58

这后者的有机碎片直接连接集群的发展开辟了一个新的领域，即的有机Zintl化学，为进一步合成的探索，可能是肥沃的，它是一步一步由锗乙烯基合成过程此处描述的集群。最初的步骤概述合成革9 K的4间易制毒化学从戈9 4 –簇后在溶液中提取。这涉及到熔石英玻璃吹，铌容器弧焊，高度空气敏感材料的处理，在手套箱。空气敏感K戈9，然后在框中乙二胺溶解，然后跟我反应3 SiC≡CSiMe的alkenylated。反应，其次是电trospray质谱，而最终的解决方案是用获得单晶包含官能集群[H 2 C = CH戈9-CH = CH 2] 2 – 。用于此目的的解决方案是离心，过滤，并仔细分层与18 – 冠-6的甲苯溶液。离开几天原状，这样层次的解决方案产生的橙色[K（18 -冠-6）] 2 [葛9（HCCH 2）2]•EN由单晶X-射线衍射特征结晶块。

过程中突出反应技术标准，工作，和对官能deltahedral Zintl集群分析。它希望，这将有助于对这些化合物在大进一步发展和社会的理解。

Protocol

1。准备铌管切割铌（Nb）管前，准备NB清洗解决方案。在500毫升的塑料瓶，测出并添加通过测量缸以下的股票解决方案，收到100毫升：110毫升以H 2 SO 4，其次是硝 ​​酸 50毫升，40毫升高频。拌匀，并允许使用前达到室温。 测量铌管，长4.5厘米，切管刀。避免油管扭结。重复3次以上。 在通风良好的油烟罩，放置四个铌管，长度在100毫升的塑料烧杯。?…

Discussion

这是重要的清洁以及部分氧化铌管。然而，如果留在管铌清洗液的时间过长，将严重危及管的厚度。因此，10 – 15秒，是势在必行，管，应该是在结束（图3）非常有光泽。后密封石英外套管内，他们应与铌稀溶液清洗了一遍。这将导致轻度欢腾，清洁氧化铌管焊接或玻璃吹制过程中发生的任何地区。但是，要小心不要离开太久溶液蚀刻玻璃（图7B）。

重要的是要确保碱金属?…

Divulgazioni

The authors have nothing to disclose.

Acknowledgements

笔者想感谢的持续财政支持（译文-0742365）和国家科学基金会在Bruker APEX II衍射仪（译文-0443233），并在Bruker Microtof-II质谱仪（译文-0741793）购买。笔者也想感谢他们使用的微团的Quattro-LC质谱仪欧夏令时设施。

Materials

Name of the reagent Company Catalogue number Comments
D8-Xray diffractometer Bruker Bruker APEX II  
Electrospray mass spectrometer Bruker Microtof-II  
Electrospray mass spectrometer Micromass Quattro-LC triple -quadropole
Drybox Innovative Technology S-1-M-DL IT-Sys1 model
Inert Gas/Vacuum Shielded
Arc Welding Arrangement		 LDS Vacuum Products Special Order
Arc Welder Power Source Miller Maxstar-91  
Welding Rubber Gloves The Home Depot  KH643  
Electric Engraver Burgess Products 74 Vibro-Graver
Circular Glass Saw Pistorius Machine Co. Inc GC-12-B  
Tube Furnace Lindberg/Blue M TF55035 Minimite Laboratory Tube Furnace, Moldatherm (1100 °C)
Glass Drying Oven Fisher Scientific 13-247-650G  
High Vacuum Hg Schlenk-Line Special Order Univ Of Notre Dame Alternative: Edwards E050/60; VWR International; Cat. No. EVB302-07-110
Large Torch Victor JT100C Welding torch, tip: Victor 5-W-J
Small Torch Veriflo Co. 3A Blow-pipe
Tesla Coil VWR International KT691550-0000 Leak detector
Stirrer/Hot -Plate VWR International 12620-970 VWR HOT PLATE STR DY-DUAL120V
Balance Denver Instrument Co. 100A XE Series
Centrifuge LW Scientific E8C-08AV-1501 Variable speed
Graphite Reamer, (flaring) ABR Imagery, Inc. 850-523 B01 Open holes in Glass Blowing and flaring edges
Striker Fisher Scientific 12-007  
Vise-Grips The Home Depot 0902L3SM  
Pipe-Cutter The Home Depot 32820  
Cutting Pliers The Home Depot 437  
Plastic Beaker VWR International 13890-046  
Measuring Cylinder VWR International 65000-006 Careful, HF etches glass (if using a glass one)
Large Plastic Bottle VWR International 16128-542  
13 x 100 Test-Tubes VWR International 47729-572 CULTURE TUBE 13X100 CS1000
Laboratory (Rubber) Stoppers Sigma Chemical Co. Z164437-100EA Size 00
Test-Tube Rack VWR International 60196-702 10-13 mm tube OD
Stir-Bars StirBars.com/Big Science Inc. SBM-0803-MIC PTFE 8×3 mm Micro
Glass Pipettes VWR International 14673-043 VWR PIPET PASTEUR 9IN CS1000
Rubber Bulbs VWR International 56311-062 Latex, thin walled
Glass Wool Unifrax I LLC 6048 Fiberfrax Bulk Fiber Insulation, Ceramic fiber
Glass Slides VWR International 16004-422 75x25x1mm, Microscope Slides
Paratone-N oil Hampton Research Parabar 10312 Known as: Paratone-N, Paratone-8277, Infineum V8512
High Vacuum Silicone Grease VWR International 59344-055 Dow Corning
Liquid Nitrogen Univ. of Notre Dame    
Argon Gas Cylinder Praxair Distribution Inc. TARGHP  
Nitrogen Gas Cylinder Praxair Distribution Inc. QNITPP  
Oxygen Gas Cylinder Praxair Distribution Inc. OT 337 cf CYL
Hydrogen Gas Cylinder Praxair Distribution Inc. HK 195 cf CYL
Propane Gas Cylinder/source Univ. of Notre Dame UND  
Quartz tubing, Lg Quartz Scientific Inc. 100020B 20 mm id x 22mm od x 48″ clear fused quart tubing
Quartz tubing, Md Quartz Scientific Inc. 100007B Clear Fused Quartz Tubing,7mm id x 9mm od x 48″
Round Bottom Quartz Joint Quartz Scientific Inc. 6160189B Ball joint
Quartz Safety Glasses Wale Apparatus 11-1127 waleapparatus.com
Pyrex Safety Glasses Wale Apparatus 11-2125-B3 For clear and color borosilicate glass
Blow Hose Kit Glass House BH020 glasshousesupply.com
Niobium Tubes Shaanxi Tony Metals Co., Ltd Niobium Tube, 50 ft Seamless Niobium Tube Outside diameter: 0.375 (±0.005) inches.
Wall thickness: 0.02(±0.003) Inches Niobium should be annealed.
PEEK Starter Kit for Mass Spect Waters PSL613321 PEEK (PolyEtherEtherKetone) tubing, nuts, ferrule, fits
Mass Spect Needle Set VWR International 60373-992 Hamilton Manufacturer (81165)
H2SO4 VWR International BDH3072-2.5LG ACS Grade
HNO3 VWR International BDH3046-2.5LPC ACS Grade
HF VWR International BDH3040-500MLP ACS Grade
Distilled Water Univ. of Notre Dame UND  
Acetone VWR International BDH1101-4LP  
Ethylenediamine VWR International AAA12132-0F 99% 2.5 L
Toluene VWR International 200004-418 99.8 %, anhydrous
Mercury Strem Chemicals, Inc. 93-8046  
Potassium (K) metal Strem Chemicals, Inc. 19-1989 Sealed in glass ampoule under Ar
Germanium (Ge) powder VWR International AA10190-18 GERM PWR -100 MESH 99.999% 50G
Bistrimetylsilylacetylene,
(Me3SiC≡CCSiMe3)		 Fischer Scientific AC182010100  
18-crown-6
(1,4,7,10,13,16-Hexaoxacyclooctadecane)		 VWR International 200001-954 99%, 25 gm
2,2,2-crypt
(4,7,13,16,21,24-Hexaoxa-1,10 diazabicyclo[8.8.8]hexacosane)		 Sigma Aldrich 291110-1G 98%
DOWNLOAD MATERIALS LIST

Riferimenti

  1. Corbett, J. D. Polyatomic Zintl Anions of the Post-Transition Elements. Chem. Rev. 85, 383-397 (1985).
  2. Fässler, T. F. The renaissance of homoatomic nine-atom polyhedral of the heavier carbon-group elements Si-Pb. Coord. Chem. Rev. 215, 347-377 (2001).
  3. Sevov, S. C., Goicoechea, J. M. Chemistry of Deltahedral Zintl Ions. Organometallics. 25, 5678-5692 (2006).
  4. Sevov, S. C., Davies, A. G. . Tin Chemistry: Fundamentals, Frontiers and Applications. , 138-151 (2008).
  5. Scharfe, S., Fässler, T. F. Polyhedral nine-atom clusters of tetrel elements and intermetalloid derivatives. Phil. Trans. R. Soc. A. , 368-1265 (2010).
  6. Scharfe, S., Kraus, F., Stegmaier, S., Schier, A., Fässler, T. F. Zintl Ions, Cage Compounds, and Intermetalloid Clusters of Group 14 and Group 15 Elements. Angew. Chem. Int. Ed. 50, 3630-3670 (2011).
  7. Xu, L., Sevov, S. C. Oxidative Coupling of Deltahedral [Ge9]4- Zintl Ions. J. Am. Chem. Soc. 121, 9245-9246 (1999).
  8. Hauptmann, R., Fässler, T. F. Low Dimensional Arrangements of the Zintl Ion [Ge9-Ge9]6- and Chemical Bonding in [Ge6]2-, [Ge9=Ge9]6- and 1∞{[Ge9]}2-. Z. Anorg. Allg. Chem. 629, 2266-2273 (2003).
  9. Suchentrunk, C., Daniels, J., Somer, M., Carrillo-Cabrera, W., Korber, N. Synthesis and Crystal Structures of the Polygermanide Ammoniates K4Ge9•9NH3, Rb4Ge9•5NH3 and Cs6Ge18•4NH3. Z. Naturforsch. 60b, 277-283 (2005).
  10. Ugrinov, A., Sevov, S. C. Ge9=Ge9=Ge9]6-: A Linear Trimer of 27 Germanium Atoms. J. Am. Chem. Soc. 124, 10990-10991 (2002).
  11. Yong, L., Hoffmann, S. D., Fässler, T. F. The Controlled Oxidative coupling of Ge94- Zintl Anions to a Linear Trimer [Ge9=Ge9=Ge9]6. Z. Anorg. Allg. Chem. 631, 1149-1153 (2005).
  12. Ugrinov, A., Sevov, S. C. Ge9=Ge9=Ge9=Ge9]8-: A Linear Tetramer of Nine-Atom Germanium Clusters, a Nanorod. Inorg. Chem. 42, 5789-5791 (2003).
  13. Yong, L., Hoffmann, S. D., Fässler, T. F. Oxidative Coupling of Ge94- Zintl Anions – Hexagonal Rod Packing of Linear [Ge9=Ge9=Ge9=Ge9]8-. Z. Anorg. Allg. Chem. 630, 1977-1981 (2004).
  14. Denning, M. S., Goicoechea, J. M. [Hg3(Ge9)4]10-: a nanometric molecular rod precursor to polymeric mercury-linked cluster chains. Dalton Trans. , 5882-5885 (2008).
  15. Boeddinghaus, M. B., Hoffmann, S. D., Fässler, T. F. Synthesis and Crystal Structure of [K([2,2,2]crypt)]2[HgGe9](dmf). Z. Annorg. Allg. Chem. 633, 2338-2341 (2007).
  16. Nienhaus, A., Hauptmann, R., Fässler, T. F. 1∞[HgGe9]2- –A Polymer with Zintl Ions as Building Blocks Covalently Linked by Heteroatoms. Angew. Chem., Int. Ed. 41, 3213-3215 (2002).
  17. Downie, C., Tang, Z., Guloy, A. M. An Unprecedented 1∞[Ge9]2- Polymer: A Link between Molecular Zintl Clusters and Solid-State Phases. Angew. Chem., Int. Ed. 39, 337-340 (2000).
  18. Downie, C., Mao, J. -. G., Parmar, H., Guloy, A. M. The Role of Sequestering Agents in the Formation and Structure of Germanium Anion Cluster Polymers. Inorg. Chem. 43, 1992-1997 (2004).
  19. Ugrinov, A., Sevov, S. C. Synthesis of a chain of nine-atom germanium clusters accompanied with dimerization of the sequestering. 8, 1878-1882 (2005).
  20. Spiekermann, A., Hoffmann, S. D., Kraus, F., Fässler, T. F. Au3Ge18]5- – Gold-Germanium Cluster with Remarkable Au-Au Interactions. Angew. Chem., Int. Ed. 46, 1638-1640 (2007).
  21. Spiekermann, A., Hoffmann, S. D., Fässler, T. F., Krossing, I., Preiss, U. [Au3Ge45]9-–A Binary Anion Containing a {Ge45}. Cluster. Angew. Chem., Int. Ed. 46, 5310-5313 (2007).
  22. Wang, J. -. Q., Wahl, B., Fässler, T. F. [Ag(Sn9-Sn9)]5-: A Homoleptic Silver Complex of A Dimeric Sn9 Zintl Anion. Angew. Chem., Int. Ed. 49, 6592-6595 (2010).
  23. Scharfe, S., Fässler, T. F. VVarying Bonding Modes of the Zintl Ion [Ge9]4- in CuI Complexes: Syntheses and Structures of [Cu(η4-Ge9)(PR3)]3- (R = iPr, Cy) and [Cu(η4-Ge9)(η1-Ge9)]7-. Eur. J. Inorg. Chem. 8, 1207-1213 (2010).
  24. Yong, L., Boeddinghaus, M. B., Fässler, T. F. [Sn9HgSn9]6-: An Intermetalloid Zintl Ion with Two Sn9 Connected by Heteroatom. Z. Anorg. Allg. Chem. 636, 1293-1296 (2010).
  25. Rios, D., Gillett-Kunnath, M. M., Taylor, J. D., Oliver, A. G., Sevov, S. C. Addition of a Thallium Vertex to Empty and Centered Nine-Atom Deltahedral Zintl Ions of Germanium and Tin. Inorg. Chem. 50, 2373-2377 (2011).
  26. Eichhorn, B. W., Haushalter, R. C. Synthesis and Structure of closo-Sn9Cr(CO)34-: The First Member in a New Class of Polyhedral Clusters. J. Amer. Chem. Soc. 110, 8704-8706 (1988).
  27. Eichhorn, B. W., Haushalter, R. C. closo-[CrPb9(CO)3]4-: a 100 Year History of the Nonaplumbide Tetra-anion. J. Chem. Soc. Chem. Commun. , 937-938 (1990).
  28. Kesanli, B., Fettinger, J., Eichhorn, B. W. The closo-[Sn9M(CO)3]4- Zintl Ion Clusters where M = Cr, Mo, W: Two Structural Isomers and Their Dynamic Behavior. Chem. Eur. J. 7, 5277-5285 (2001).
  29. Kesanli, B., Fettinger, J., Gardner, D. R., Eichhorn, B. . The [Sn9Pt2(PPh3)]2- and [Sn9Ni2(CO)]3- Complexes: Two Markedly Different Sn9M2L Transition Metal Zintl Ion Clusters and Their Dynamic. 124, 4779-4788 (2002).
  30. Campbell, J., Mercier, H. P. A., Holger, F., Santry, D. P., Dixon, D. A., Schrobilgen, G. J. Syntheses, Crystal Structures, and Density Functional Theory Calculations of the closo-[1-M(CO)3(η4-E9)4- (E = Sn, Pb; M = Mo, W) Cluster Anions and Solution NMR Spectroscopic Characterization of [1-M(CO)3(η4-Sn9)4- (M = Cr, Mo, W). Inorg. Chem. 41, 86-107 (2002).
  31. Yong, L., Hoffmann, S. D., Fässler, T. F. Crystal Structures of [K(2.2.2-crypt)]4[Pb9Mo(CO)3]–Isolation of the Novel Isomers [(η5-Pb9)Mo(CO)3]4- beside [(η4-Pb9)Mo(CO)3]4. Eur. J. Inorg. Chem. , 3663-3669 (2005).
  32. Esenturk, E. N., Fettinger, J., Eichhorn, B. Synthesis and characterization of the [Ni6Ge13(CO)5]4- and [Ge9Ni2(PPh3)]2- Zintl ion clusters. Polyhedron. 25, 521-529 (2006).
  33. Rios, D., Sevov, S. C. The Elusive closo-Ge102- Zintl Ion: Finally “Captured” as a Ligand in the Complex [Ge10Mn(CO)4]3-. Inorg. Chem. 49, 6396-6398 (2010).
  34. Downing, D. O., Zavalij, P., Eichhorn, B. W. The closo-[Sn9Ir(cod)]3- and [Pb9Ir(cod)]3- Zintl Ions: Isostructural IrI Derivatives of the nido-E94- Anions (E = Sn, Pb). Eur. J. Inorg. Chem. , 890-894 (2010).
  35. Esenturk, E. N., Fettinger, J., Lam, Y. -. F., Eichhorn, B. Pt@Pb12]2-. Angew. Chem. Int. Ed. 43, 2132-2134 (2004).
  36. Goicoechea, J. M., Sevov, S. C. [(Ni-Ni-Ni)@(Ge9)2]4-: A Linear triatomic Nickel Filament Enclosed in a Dimer of Nine-Atom Germanium Clusters. Angew. Chem. Int. Ed. 44, 4026-4028 (2005).
  37. Goicoechea, J. M., Sevov, S. C. [(Pd-Pd)@Ge18]4-: A Palladium Dimer Inside the Largest Single-Cage Deltahedron. J. Am. Chem. Soc. 127, 7676-7677 (2005).
  38. Esenturk, E. N., Fettinger, J., Eichhorn, B. The closo-Pb102- Zintl ion in the [Ni@Pb10]2 cluster. Chem. Commun. , 247-249 (2005).
  39. Goicoechea, J. M., Sevov, S. C. Deltahedral Germanium Clusters: Insertion of Transition-Metal Atoms and Addition of Organometallic Fragments. J. Am. Chem. Soc. 128, 4155-4161 (2006).
  40. Esenturk, E. N., Fettinger, J., Eichhorn, B. W. Synthesis, Structure, and Dynamic Properties of [Ni2Sn17]4. J. Am. Chem. Soc. 128, 12-13 (2006).
  41. Esenturk, E. N., Fettinger, J., Eichhorn, B. W. The Pb122- and Pb102- Zintl Ions and the M@Pb122- and M@Pb102- Cluster Series Where M = Ni, Pd, Pt. J. Am. Chem. Soc. 128, 9178-9186 (2006).
  42. Kocak, F. S., Zavalij, P., Lam, Y. F., Eichhorn, B. W. Solution Dynamics and Gas-Phase Chemistry of Pd2@Sn184. Inorg. Chem. 47, 3515-3520 (2008).
  43. Scharfe, S., Fässler, T. F., Stegmaier, S., Hoffmann, S. D., Ruhland, K. [Cu@Sn9]3- and [Cu@Pb9]3-: Intermetalloid Clusters with Endohedral Cu Atoms in Spherical Environments. Chem. Eur. J. 14, 4479-4483 (2008).
  44. Zhou, B., Denning, M. S., Kays, D. L., Goicoechea, J. M. Synthesis and Isolation of [Fe@Ge10]3-: A Pentagonal Prismatic Zintl Ion Cage Encapsulating an Interstitial Iron Atom. J. Am. Chem. Soc. 131, 2802-2803 (2009).
  45. Wang, J. -. Q., Stegmaier, S., Fässler, T. F. [Co@Ge10]3-: An Intermetalloid Cluster with Archimedean Pentagonal Prismatic Structure. Angew. Chem. Int. Ed. 48, 1998-2002 (2009).
  46. Wang, J. -. Q., Stegmaier, S., Wahl, B., Fässler, T. F. Step-by-Step Synthesis of the Endohedral Stannaspherene [Ir@Sn12]3- via the Capped Cluster Anion [Sn9Ir(cod)]3. Chem. Eur. J. 16, 1793-1798 (2010).
  47. Gillett-Kunnath, M. M. P. a. i. k., Jensen, J. I., Taylor, S. M., D, &. a. m. p. ;. J., Sevov, S. C. Metal-Centered Deltahedral Zintl Ions: Synthesis of [Ni@Sn9]4- by Direct Extraction from Intermetallic Precursors and of the Vertex-Fused Dimer [{Ni@Sn8(μ-Ge)1/2}2]4. Inorg. Chem. 50, 11695-11701 (2011).
  48. Ugrinov, A., Sevov, S. C. Ph2Bi-(Ge9)-BiPh2]2-: A Deltahedral Zintl Ion Functionalized by Exo-Bonded Ligands. J. Am. Chem. Soc. 124, 2442-2443 (2002).
  49. Ugrinov, A., Sevov, S. C. Derivatization of Deltahedral Zintl Ions by Nucleophilic Addition: [Ph-Ge9-SbPh2]2- and [Ph2Sb-Ge9-Ge9-SbPh2]4. J. Am. Chem. Soc. 125, 14059-14064 (2003).
  50. Ugrinov, A., Sevov, S. C. Rationally Functionalized Deltahedral Zintl Ions: Synthesis and Characterization of [Ge9-ER3]3-, [R3E-Ge9-ER3]2-, and [R3E-Ge9-Ge9-ER3]4- (E= Ge, Sn; R = Me, Ph). Chem. Eur. J. 10, 3727-3733 (2004).
  51. Hull, M., Ugrinov, A., Petrov, I., Sevov, S. C. Alkylation of Deltahedral Zintl Clusters: Synthesis of [R-Ge9-Ge9-R]4- (R = tBu, sBu, nBu, tAm) and Structure of [tBu-Ge9-Ge9-tBu]4. Inorg. Chem. 46, 2704-2708 (2007).
  52. Hull, M., Sevov, S. C. Addition of Alkenes to Deltahedral Zintl Clusters by Reaction with Alkynes: Synthesis and Structure of [Fc-CH=CH-Ge9-CH=CH-Fc]2-, an Organo-Zintl-Organometallic Anion. Angew. Chem. Int. Ed. 46, 6695-6698 (2007).
  53. Hull, M., Sevov, S. C. Organo-Zintl Clusters Soluble in Conventional Organic Solvents: Setting the Stage for Organo-Zintl Cluster Chemistry. Inorg. Chem. 46, 10953-10955 (2007).
  54. Chapman, D. J., Sevov, S. C. Tin-Based Organo-Zintl Ions: Alkylation and Alkenylation of Sn94. Inorg. Chem. 47, 6009-6013 (2008).
  55. Hull, M., Sevov, S. C. Functionalization of Nine-Atom Deltahedral Zintl Ions with Organic Substituents: Detailed Studies of the Reactions. J. Am. Chem. Soc. 131, 9026-9037 (2009).
  56. Kocak, F. S., Zavalij, P. Y., Lam, Y. -. F., Eichhorn, B. W. Substituent-dependent exchange mechanisms in highly fluxional RSn93- anions. Chem. Commun. , 4197-4199 (2009).
  57. Gillett-Kunnath, M. M., Petrov, I., Sevov, S. C. Heteroatomic Deltahedral Zintl Ions of Group 14 and their Alkenylation. Inorg. Chem. 48, 721-729 (2010).
  58. Gillett-Kunnath, M. M., Oliver, A. G., Sevov, S. C. “n-Doping” of Deltahedral Zintl Ions. J. Am. Chem. Soc. 133, 6560-6562 (2011).
  59. Gaumet, J. J., Strouse, G. F. Electrospray Mass Spectrometry of Semiconductor Nanoclusters: Comparative Analysis of Positive and Negative Ion Mode. J. Am. Soc. Mass. Spectrom. 11, 338-344 (2000).
  60. Fässler, T. F. Lone Pair Interactions in Zintl Phases: Band Structure and Real Space Analysis of the cP124 Clathrate Structure Type. Z. Anorg. Allg. Chem. 624, 569-577 (1998).
  61. Guloy, A. M., Ramlau, R., Tang, Z., Schnelle, W., Baitinger, M., Grin, Y. A guest-free germanium clathrate. Nature. 443, 320-323 (2006).
  62. Guloy, A. M., Tang, Z., Ramlau, R., Böhme, B., Baitinger, M., Grin, Y. Synthesis of the Clathrate-II K8.6(4)Ge136 by Oxidation of K4Ge9 in an Ionic Liquid. Eur. J. Inorg. Chem. 17, 2455-2458 (2009).
  63. Chandrasekharan, N., Sevov, S. C. Anodic Electrodeposition of Germanium Films from Ethylenediamine Solution of Deltahedral Ge94- Zintl Ions. J. Electrochem. Soc. 157, C140-C145 (2010).
  64. Zheng, W. J., Thomas, O. C., Lippa, T. P., Xu, S. J., Bowen, K. H. The Ionic KAl13 molecule: A stepping stone to cluster-assembled materials. J. Chem. Pys. 124, 144304-144304 (2006).
  65. Riley, A. E., Tolbert, S. H. Syntehsis and characterization of tin telluride inorganic/organic composite materials with nanoscale periodicity through solution-phase self-assembly: a new class of composite materials based on Zintl cluster self-oligomerization. Res. Chem. Intermed. 33, 111-124 (2007).
  66. Sun, D., Riley, A. E., Cadby, A. J., Richman, E. K., Korlann, S. D., Tolbert, S. H. Hexagonal nanoporous germanium through surfactant-driven self-assembly of Zintl Clusters. Nature. 441, 1126-1130 (2006).

Tags

Zintl IonsGermaniumFunctionalizationOrganic GroupsRedox ChemistryDeltahedral ClustersReactivityChimicaClusters SynthesisGermanium-divinyl Clusters
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Gillett-Kunnath, M. M., Sevov, S. C. Synthesis of Nine-atom Deltahedral Zintl Ions of Germanium and their Functionalization with Organic Groups. J. Vis. Exp. (60), e3532, doi:10.3791/3532 (2012).
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