NMR Studies and Crystal Structure Determinations of CF3 Group-containing Bicyclic Phenolates

2009 ◽  
Vol 64 (4) ◽  
pp. 423-426 ◽  
Author(s):  
Constantin Mamat ◽  
Helmut Reinke ◽  
Peter Langer
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Hydrogen Bonding ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Nmr Studies ◽  
Enol Ethers ◽  
X Ray ◽  
Silyl Enol Ethers ◽  
Structure Determinations

Three new CF3-substituted bicyclic salicylate derivatives were synthesized by the TiCl4-mediated cyclization of trifluoromethyl-containing ketones with 1,3-bis(silyl enol ethers) and characterized by NMR and IR, spectroscopy, mass spectrometry and elemental analysis. The crystal structures of the bicyclic derivatives have been determined by single crystal X-ray analysis. All structures exhibit hydrogen bonding.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

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.

Structure, Stereochemistry and Novel 'Hydrogen Bonding' in Two Bipyridinium Salts of the B10H102- Anion

1987 ◽  
Vol 40 (12) ◽  
pp. 2097 ◽  
Author(s):  
DJ Fuller ◽  
DL Kepert ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Charge Transfer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Structure Determinations ◽  
Positively Charged

Crystal structure determinations of (LH)2(B10H10), (1), and (LH2)(B10H10), (2), L = 2,2'- bipyridine , have been carried out by single-crystal X-ray diffraction methods at 295 K, being refined by full-matrix least squares to residuals of 0.041, 0.047 for 1758, 1771 'observed' independent reflections respectively. Crystals of (1) are monoclinic, P21/n, a 12.040(7), b 17.71(1), c 11.142(4) �, β 101.78(4)�, Z 4. Crystals of (2) are monoclinic, P21/c, a 9.937(4), b 10.837(3), c 14.856(5) �, β 109 2l(3)�, Z 4. The colour of the compounds is accounted for by charge-transfer interactions of a novel type, namely between the positively charged cationic acid hydrogen atoms and the negatively charged non-apical hydrogen atoms of the anion. In yellow (1), these distances are 2.26(5) �, while in red (2), they are much shorter, being 1.89(4), 1.97(3) �.

A Three-Dimensional Silver(I) Framework Assembled from Nitrilotriacetate

2005 ◽  
Vol 58 (2) ◽  
pp. 115 ◽  
Author(s):  
Chun-Long Chen ◽  
Qian Zhang ◽  
Ji-Jun Jiang ◽  
Qin Wang ◽  
Cheng-Yong Su
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Three Dimensional ◽  
Single Crystal Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coordination Numbers

The reaction of AgCF3CO2 with nitrilotriacetate (NTA) yields the three-dimensional silver(i) coordination polymer {Ag3[N(CH2COO)3]}n 1 which was characterized by means of elemental analysis and IR spectroscopy as well as X-ray diffraction. The single crystal structure shows that the NTA3– anions act as unusual heptadentate 13-coordination agents and the silver(i) atoms exhibit various coordination numbers in the range 3–6.

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.

scholarly journals 4-(7-Bromobenzo[d][1,2,3]thiadiazol-4-yl)morpholine

Molbank ◽  
10.3390/m1202 ◽  
2021 ◽  
Vol 2021 (2) ◽  
pp. M1202
Author(s):  
Nikita Gudim ◽  
Ekaterina Knyazeva ◽  
Natalia Obruchnikova ◽  
Oleg Rakitin ◽  
Vadim Popov
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
13C Nmr ◽  
High Resolution Mass Spectrometry ◽  
Nitrogen Heterocycles ◽  
X Ray ◽  
Photovoltaic Materials ◽  
Resolution Mass

Dibromoderivatives of benzofused chalcogen-nitrogen heterocycles are important precursors in the synthesis of various photovoltaic materials. 4,7-Dibromobenzo[d][1,2,3]thiadiazole is a practically unexplored compound in this series. In this communication, it was shown that the nucleophilic substitution of 4,7-dibromobenzo[d][1,2,3]thiadiazole with morpholine gave selectively 4-substituted product—4-(7-bromobenzo[d][1,2,3]thiadiazol-4-yl)morpholine. The structure of the newly synthesized compound was established by means of elemental analysis, high resolution mass-spectrometry, 1H, 13C NMR, and IR spectroscopy, mass-spectrometry, and X-ray analysis.

Nitridomolybdenum Complexes of Tris(3,5-dimethylpyrazol-1-yl)Hydroborate and the X-Ray Crystal-Structure of {HB(3,5-Me2C3N2H)3)MoN(N3)2

1990 ◽  
Vol 43 (8) ◽  
pp. 1347 ◽  
Author(s):  
CG Young ◽  
F Janos ◽  
MA Bruck ◽  
PA Wexler ◽  
JH Enemark
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Least Squares ◽  
Elemental Analysis ◽  
Bond Distance ◽  
Octahedral Complex ◽  
Fourier Methods ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The reaction of (NEt4)2[MoNCl5] and K{HB(Me2pz)3}[HB(Me2pz)3- = tris (3,5- dimethylpyrazol-1-yl) hydroborate anion] produces both purple, diamagnetic {HB(Me2pz)3}MoNCl2 (1) and yellow, paramagnetic Net4 [{HB(Me2pz)3}MoNCl2] (2) (e.s.r.: {g} 1.961, {a}(95Mo) 57×10-4 cm-1), which have been separately isolated under different conditions. In contrast, the reaction of [ MoN (N3)4]- with Na{HB(Me2pz)3} results in the exclusive formation of red {HB(Me2pz)3} MoN (N3)2 (3). Crystals of (3) are monoclinic and belong to space group P21/n with a 16.440(2), b 8.787(2), c 16.754(2) Ǻ,β 112.47(1)°, V 2236.4 Ǻ3, and Z 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 3208 reflections, to a conventional R value of 0.032 ( Rw 0.047). In the distorted octahedral complex the molybdenum(VI) atom is coordinated by a facial HB(Me2pz)3- ligand , a terminal nitrido ligand with a Mo-N bond distance of 1.646(4)Ǻ, and two azide ligands. All complexes have been characterized by elemental analysis, infrared, 1H n.m.r. or e.s.r. spectroscopy, and mass spectrometry. Improved syntheses for the starting materials (NEt4)2 [MoNCl5] and (NEt4)2 [MoNCl4] are also reported.

scholarly journals Molecular design and synthesis of new dithiocarbazate complexes; crystal structure, bioactivities and nano studies

RSC Advances ◽  
2018 ◽  
Vol 8 (73) ◽  
pp. 41795-41809 ◽  
Author(s):  
Zahra Yekke-ghasemi ◽  
Reza Takjoo ◽  
Mohammad Ramezani ◽  
Joel T. Mague
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Metal Complexes ◽  
Elemental Analysis ◽  
Molecular Design ◽  
X Ray ◽  
Design And Synthesis

New metal complexes are synthesized and characterized by elemental analysis, mass spectrometry, spectroscopic, TGA and X-ray techniques. The compounds were evaluated in anin vitrocytotoxicity. Interaction of the samples with HSA was investigated.

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