Organozinc Siloxide-Hydrazide Aggregates [(RZn)4(NHNMe2)x(OSiMe3)(4 – x)]

2006 ◽  
Vol 61 (7) ◽  
pp. 838-845 ◽  
Author(s):  
Surajit Jana ◽  
Roland Fröhlich ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
General Formula ◽  
Elemental Analysis ◽  
Mirror Symmetry ◽  
The Novel ◽  
X Ray ◽  
X Ray Crystallography ◽  
The Core ◽  
Mixed Aggregates

The reaction of dialkylzinc compounds R2Zn (R = Me, Et) with N,N-dimethylhydrazine and trimethylsilanol in a 4 : 2 : 2 ratio leads to the formation of tetra(alkylzinc) tris-siloxide monohydrazide aggregates, [(RZn)4(NHNMe2)(OSiMe3)3] [R = Me (1) and Et (2)]. These compounds are aggregates of mirror symmetry, containing the novel Zn4N2O3 core. Both compounds have been characterised by 1H, 13C and 29Si NMR and IR spectroscopy, by mass spectrometry and by elemental analysis, and 2 also by X-ray crystallography. The structure can be derived from a heterocubane, in which one anionic vertex is replaced by an NHNMe2 group contributing two N atoms to the core constitution. By applying a ratio of hydrazine : silanol of 2 : 1 in a reaction with R2Zn (R = Me, Et, iPr), compounds of the general formula [(RZn)4(NHNMe2)2(OSiMe3)2] [R = Me (3), Et (4), iPr (5)] are obtained. These aggregates contain a Zn4N4O2 core. Upon employing a hydrazine : silanol ratio of 5 : 1 in a reaction with diisopropyl zinc, the compound [(iPrZn)4(NHNMe2)3(OSiMe3)] results, containing a Zn4N6O unit. Compounds 3 - 6 have been characterised by 1H, 13C and 29Si NMR and IR spectroscopy, by mass spectrometry and by elemental analysis. The topologic relationship between the pure hydrazides [(RZn)4(NHNMe2)4], the mixed aggregates [(RZn)4(NHNMe2)3(OR’)], [(RZn)4(NHNMe2)2(OR’)2] and [(RZn)4(NHNMe2)3(OR’)3] and the pure alkoxides [(RZn)4(OR’)4] is discussed.

Syntheses and Structures of Silver(I) and Palladium(II) Complexes with Ferrocenyl-phosphonodithiolate Ligands

2010 ◽  
Vol 65 (1) ◽  
pp. 32-36 ◽  
Author(s):  
Xi-Ying Wang ◽  
Hua-Tian Shi ◽  
Qing Ma ◽  
Qian-Feng Zhang
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar

Coordinative interaction of [Ag(PPh3)2NO3] or [Pd(MeCN)2Cl2] with in situ-prepared Na[FcP- (OR)S2] afforded 1 : 1 products [FcP(OR)S2Ag(PPh3)2] (R = Me 1, n-Pr 2) or the 1 : 2 product [{FcP(OMe)S2}2Pd] (3). Complexes 1 - 3 were characterized by elemental analysis, mass spectrometry, NMR (1H, 31P) and IR spectroscopy, as well as by X-ray crystallography. The distorted tetrahedral silver(I) coordination led to non-planar and distorted four-membered AgS2P rings in 1 and 2, whereas the square-planar palladium(II) coordination resulted in four-membered co-planar PdS2P rings in 3

scholarly journals 4-vinylpyridine derivatives: Protonation, methylation and silver(I) coordination chemistry

2021 ◽  
pp. 174751982198965
Author(s):  
Guoqi Zhang
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Coordination Chemistry ◽  
Elemental Analysis ◽  
Silver Complex ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Moiety ◽  
New Compounds

( E)-4-[2-(Pyridin-4-yl)vinyl]benzaldehyde, containing both a 4-vinylpyridine and an aldehyde functionality, is utilized to develop new, highly conjugated chalcone compounds and a bis-Schiff base azine compound. The chalcone-containing compounds are further explored for their protonation, methylation and silver(I) coordination chemistry using the pyridine moiety. In parallel, a cyano-containing analogue, ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile is also synthesized and studied for its silver(I) coordination chemistry. These new compounds are fully characterized by mass spectrometry, elemental analysis and spectroscopic techniques. The methylated product of ( E)-1-(9-anthryl)-3-{4-[2-(pyridin-4-yl)vinyl]phenyl}prop-2-en-1-one and a silver complex of ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile are structurally determined by X-ray crystallography.

1,4,8,11-Tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes — Synthesis, characterization, and X-ray crystallography of the first tetrakistriazenes to be reported

2006 ◽  
Vol 84 (10) ◽  
pp. 1280-1289 ◽  
Author(s):  
Jeffery D Clarke ◽  
Keith Vaughan ◽  
Valerio Bertolasi
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Electrospray Mass Spectrometry ◽  
Diazonium Salt ◽  
Diazonium Salts ◽  
The Novel ◽  
Analogous Reaction ◽  
X Ray ◽  
X Ray Crystallography ◽  
The Mean

The reactions of a series of arene diazonium salts with 1,4,8,11-tetraazacyclotetradecane (cyclam) afford the novel compounds, the 1,4,8,11-tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes (1a–1f), which are the first examples of tetrakistriazenes to be reported. The tetrakistriazenes were characterized by IR spectroscopy, proton and carbon NMR, elemental analysis, high resolution electrospray mass spectrometry, and X-ray crystallography. The analogous reaction of a diazonium salt with 1,4,7-triazacyclononane or 1,5,9-triazacyclododecane yields the tristriazenes 2, 3a, and 3b. The structures of compounds 1c and 1e were solved by X-ray crystallography at low temperature (150 K). Both molecules display a conformation where the four phenyltriazenyl groups point alternately upwards and downwards with respect to the mean macrocyclic plane.Key words: triazene, tetrakistriazene, cyclam, tetraazacyclotetradecane, X-ray, NMR, cyclic polyamines.

1,3,5-Tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane

2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.

scholarly journals Synthesis and Characterisation of Zinc(II) Complex With 2-Amino-5-bromopyridine Ligand

2017 ◽  
Author(s):  
Fitriani
Keyword(s):  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Visible Absorption ◽  
X Ray ◽  
X Ray Crystallography ◽  
Uv Visible ◽  
Cl Atoms ◽  
Distorted Tetrahedral Coordination

The synthesis and characterisation of zinc(II) complex with 2-amino-5-bromopyridine (C5H5BrN2) ligand have been described. The complex was structurally characterised via X-ray crystallography, in the title compound, (2-amino-5-bromopyridinium) [ZnCl¬3(2-amino-5-bromopyridine)] or which is also called (C5H6BrN2) [ZnCl3(C5H5BrN2)]¬. The Zn(II) atom is four-coordinated by three Cl atoms and one imine N-atom of 2-amino-5-bromopyridine ligand, forming a distorted tetrahedral coordination geometry. The complex was also investigated by elemental analysis, 1H NMR, IR spectroscopy and UV-Visible absorption. The protonation behaviour upon coordination is discussed.

A new modification of [Ag4Br4(PPh3)4]: synthesis, structure and properties

2018 ◽  
Vol 73 (10) ◽  
pp. 733-738 ◽  
Author(s):  
Xintong Han ◽  
Shanshan Mao ◽  
Chuang Li ◽  
Kesheng Shen ◽  
Xinkui Shi ◽  
...  
Keyword(s):  
Solid State ◽  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
Elemental Analysis ◽  
Supramolecular Structure ◽  
Chair Conformation ◽  
Cyclic Voltammograms ◽  
Structure And Properties ◽  
X Ray ◽  
X Ray Crystallography

AbstractA new modification of the homometallic silver(I) cluster [Ag4Br4(PPh3)4] has been prepared and characterized by elemental analysis, UV/Vis and IR spectroscopy, and X-ray crystallography. The tetramer shows a polycyclic structure with a chair conformation. The bromine atoms adopt μ2- and μ3-bridging modes. The shortest Ag–Ag distance in the cluster is 3.159(2) Å, which indicates significant Ag–Ag interactions. A supramolecular structure is arranged by hydrogen bonds (C–H···Br). Cyclic voltammograms of the cluster indicate a quasi-reversible Ag+/Ag couple. The fluorescence properties of the ligand and the Ag(I) cluster were studied in the solid state. The emission peaks of the Ag(I) cluster are attributed to ligand-centered luminescence.

Retention of (4,4) Connectivity in the Absence of π…π Interactions in a Cadmium tris-Dicyanamide Compound

2006 ◽  
Vol 59 (2) ◽  
pp. 115 ◽  
Author(s):  
Moumita Biswas ◽  
Stuart R. Batten ◽  
Paul Jensen ◽  
Samiran Mitra
Keyword(s):  
Thermogravimetric Analysis ◽  
Ir Spectroscopy ◽  
Powder Diffraction ◽  
Elemental Analysis ◽  
Octahedral Geometry ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography ◽  
Extended Sheets

An anionic cadmium tris-dicyanamide compound (Et4N)[Cd(N(CN)2)3]·3/4H2O 1 has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, X-ray powder diffraction, and X-ray crystallography. The anions form extended sheets with retention of (4,4) connectivity in the absence of π···π interactions within the cation layers, and with octahedral geometry about individual CdII ions.

Preparation and Characterization of Macrocyclic Dinickel Complexes Coligated by Tetrazolate Ligands

2008 ◽  
Vol 63 (5) ◽  
pp. 496-502 ◽  
Author(s):  
Vasile Lozan ◽  
Sergei V. Voitekhovich ◽  
Pavel N. Gaponik ◽  
Oleg A. Ivashkevich ◽  
Berthold Kersting
Keyword(s):  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
X Ray ◽  
X Ray Crystallography

The dinuclear nickel(II) complex [Ni2LCl]+ (1), where (L)2− represents a 24-membered macrocyclic hexamine-dithiophenolate ligand, reacts readily with 5-R-tetrazolate ligands to give the complexes [Ni2L(RCN4)]+, where R = H (2), Me (3), Ph (4). The new complexes were either isolated as perchlorate or tetraphenylborate salts and fully characterized by elemental analysis, UV/Vis, and IR spectroscopy. The structures of 2[BPh4] · MeCN, 3[BPh4] · 2MeCN, and 4[BPh4] ·MeCN were determined by X-ray crystallography, showing that all tetrazolate units are in a 2,3-bridging mode to generate dioctahedral N3Ni(μ-S)2(μ-N4CR)NiN3 core structures. The RCN4− groups interact less strongly with the [Ni2L]2+ fragment than pyrazolate ligands (CH)3N2 − as reflected in the longer Ni-N distances.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

scholarly journals Crystal structure of an oxalate-bridged tetranuclear 8-hydroxyquinoline Zn(II) cluster: [Zn4Q6(Ox)]0.5n

2011 ◽  
Vol 76 (4) ◽  
pp. 529-537 ◽  
Author(s):  
Jiajun Wang ◽  
Qiang Wang ◽  
Yanjun Sun ◽  
Yuemei Wang ◽  
Guosheng Zhao ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Stacking Interactions ◽  
Monoclinic System ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polymeric Chains

The chain structure of a tetranuclear zinc(II) cluster [Zn4Q6(Ox)]0.5n ([Zn4 (C9H6NO)6(C2O4)]0.5n) (1) (Q = 8- hydroxyquinoline anion, Ox = oxalate dianion) was determined by X-ray crystallography and characterized by elemental analysis, IR spectroscopy and thermal analysis. It crystallizes in the monoclinic system, space group P21/n (No. 14), with the lattice parameters a = 13.2222(15) ?, b = 11.0566(12) ?, c = 16.2224(18) ?, ? = 92.1770(10)?, V = 2369.9(5) ?3, Z = 4, Mr = 607.23 g mol-1, Dc = 1.702 g cm-3. The tetranuclear zinc(II) clusters form 1D polymeric chains parallel to the b-axis. The ?-? stacking interactions involving aryl rings support the formation of the 1D polymeric structure. The neighboring polymeric chains are connected by C-H???? interactions.

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