scholarly journals A Comprehensive Analysis of the Metal–Nitrile Bonding in an Organo-Diiron System

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7088
Author(s):  
Giulio Bresciani ◽  
Lorenzo Biancalana ◽  
Guido Pampaloni ◽  
Stefano Zacchini ◽  
Gianluca Ciancaleoni ◽  
...  
Keyword(s):  
Spectroscopic Data ◽  
Comprehensive Analysis ◽  
X Ray Diffraction ◽  
Bond Energies ◽  
Comprehensive Description ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Back Donation ◽  
Suitable System ◽  
Donor Power

Nitriles (N≡CR) are ubiquitous in coordination chemistry, yet literature studies on metal–nitrile bonding based on a multi-technique approach are rare. We selected an easily-available di-organoiron framework, containing both π-acceptor (CO, aminocarbyne) and donor (Cp = η5−C5H5) ligands, as a suitable system to provide a comprehensive description of the iron–nitrile bond. Thus, the new nitrile (2–12)CF3SO3 and the related imine/amine complexes (8–9)CF3SO3 were synthesized in 58–83% yields from the respective tris-carbonyl precursors (1a–d)CF3SO3, using the TMNO strategy (TMNO = trimethylamine-N-oxide). The products were fully characterized by elemental analysis, IR (solution and solid state) and multinuclear NMR spectroscopy. In addition, the structures of (2)CF3SO3, (3)CF3SO3, (5)CF3SO3 and (11)CF3SO3 were ascertained by single crystal X-ray diffraction. Salient spectroscopic data of the nitrile complexes are coherent with the scale of electron-donor power of the R substituents; otherwise, this scale does not match the degree of Fe → N π-back-donation and the Fe–N bond energies, which were elucidated in (2–7)CF3SO3 by DFT calculations.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

New iboga-type alkaloids from Ervatamia hainanensis

RSC Advances ◽  
2016 ◽  
Vol 6 (36) ◽  
pp. 30277-30284 ◽  
Author(s):  
Zhi-Wen Liu ◽  
Xiao-Jun Huang ◽  
Han-Lin Xiao ◽  
Guo Liu ◽  
Jian Zhang ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
X Ray Diffraction ◽  
X Ray

The structures and absolute configurations of seven new iboga-type alkaloids 1–7 were determined by spectroscopic data, Mosher's method, single crystal X-ray diffraction and ECD analyses.

The Effect of Different Methods to Pretreat Reed Pulp on the Crystallinity of Microcrystalline Cellulose

2014 ◽  
Vol 1056 ◽  
pp. 12-15 ◽  
Author(s):  
Wen Long Zhang ◽  
Wen Long Zhao ◽  
Ya Jie Dai
Keyword(s):  
Crystallite Size ◽  
Microcrystalline Cellulose ◽  
Average Crystallite Size ◽  
Comprehensive Analysis ◽  
Raw Material ◽  
Type I ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimethyl Acetamide ◽  
Crystal Type

Reed Pulp was Raw Material that Pretreated by Four Methods {ultrasonic, Microwave, N, N-Dimethyl Acetamide (DMAc) and Tetrahydrofuran (THF)}. Reed Microcrystalline Cellulose (MCC) was Prepared by the Dilute Hydrochloric Acid Hydrolysis from Pretreated Reed Pulp. the Influences of Pretreatment Methods on Crystalline Type, Crystallinity and Crystallite Size of MCC were Investigated by X-Ray Diffraction (XRD). the Results Showed that the Crystallinity of MCC with Four Pretreatment Methods was 68.45%, 62.28%, 63.21% and 69.56%, Respectively. the Average Crystallite Size of MCC Prepared by Hydrolysis after Pretreated by Dmac was the Largest. whereas, the Crystal Type of MCC was Not Changed, it was still the Cellulose Type I. Comprehensive Analysis Indicated that the Effects of MCC Prepared by Hydrolysis after Pretreated by Ultrasonic were the Best.

scholarly journals Aspergiloid I, an unprecedented spirolactone norditerpenoid from the plant-derived endophytic fungus Aspergillus sp. YXf3

2014 ◽  
Vol 10 ◽  
pp. 2677-2682 ◽  
Author(s):  
Zhi Kai Guo ◽  
Rong Wang ◽  
Wei Huang ◽  
Xiao Nian Li ◽  
Rong Jiang ◽  
...  
Keyword(s):  
Endophytic Fungus ◽  
Spectroscopic Data ◽  
Biosynthetic Pathway ◽  
Culture Broth ◽  
Ring System ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anti Oxidant ◽  
Inhibitory Activities ◽  
Aspergillus Sp

An unusual C18 norditerpenoid, aspergiloid I (1), was isolated from the culture broth of Aspergillus sp. YXf3, an endophytic fungus derived from Ginkgo biloba. Its structure was unambiguously established by analysis of HRMS–ESI and spectroscopic data, and the absolute configuration was determined by low-temperature (100 K) single crystal X-ray diffraction with Cu Kα radiation. This compound is structurally characterized by a new carbon skeleton with an unprecedented 6/5/6 tricyclic ring system bearing an α,β-unsaturated spirolactone moiety in ring B, and represents a new subclass of norditerpenoid, the skeleton of which is named aspergilane. The hypothetical biosynthetic pathway for 1 was also proposed. The cytotoxic, antimicrobial, anti-oxidant and enzyme inhibitory activities of 1 were evaluated.

Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate / Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates

1982 ◽  
Vol 37 (11) ◽  
pp. 1393-1401 ◽  
Author(s):  
Beatrix Milewski-Mahrla ◽  
Hubert Schmidbaur
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Molar Ratio ◽  
Ionic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Donor Acceptor ◽  
New Compounds

Reactions of pentamethylantimony (CH3)5Sb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramothylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed.The crystal structures of the hydrogen-dibenzoato (1), hydrogen-ortho-plithalato (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter­actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH3)4Sb-tetrahedron in 1 is distorted by two benzoate oxygon atoms (at 304(2) and 340(2) pin). The cation in 2 is largely undistorted and the anion has a hydrogenphthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate.

Synthesis, characterization, and structures of zircona- and boracyclosiloxanes with ferrocenyl substituents

2002 ◽  
Vol 80 (11) ◽  
pp. 1469-1480 ◽  
Author(s):  
Karena Thieme ◽  
Sara C Bourke ◽  
Juan Zheng ◽  
Mark J MacLachlan ◽  
Fojan Zamanian ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Differential Scanning Calorimetry ◽  
Thermogravimetric Analysis ◽  
Ring Opening ◽  
Ring Opening Polymerization ◽  
The Novel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy

The novel zirconatetraferrocenylcyclotrisiloxane Cp2Zr(OSiFc2)2O (6), dizirconatetraferrocenylcyclotetrasiloxane [Cp2Zr(OSiFc2)O]2 (7), boratetraferrocenylcyclotrisiloxane (C6H5)B(OSiFc2)2O (8), and diboratetraferrocenylcyclotetrasiloxane [(C6H5)B(OSiFc2)O]2 (9) with ferrocenyl (Fc = Fe(η-C5H4)(η-C5H5)) substituents at silicon have been prepared from the reactions of Cp2Zr(NMe2)2 and PhBCl2 with diferrocenylsilanediol Fc2Si(OH)2 (3) and tetraferrocenyldisiloxanediol [Fc2SiOH]2O (5). The compounds were characterized by mass spectrometry, elemental analysis, UV–vis, IR, Raman, and multinuclear NMR spectroscopy, as well as single crystal X-ray diffraction. Thermogravimetric analysis and differential scanning calorimetry investigation of 6–9 showed that the cycles decompose before they can undergo any thermal ring-opening polymerization. In addition, no polymerization was detected in the presence of either KOSiMe3 or HOTf. The bulky ferrocenyl substituents on the Si atoms are likely to be at least partially responsible for the inability of these heterocycles to undergo ring-opening polymerization. Key words: heterocyclosiloxanes, ferrocenyl.

scholarly journals Discovery of Stealthin Derivatives and Implication of the Amidotransferase FlsN3 in the Biosynthesis of Nitrogen-Containing Fluostatins

Marine Drugs ◽  
2019 ◽  
Vol 17 (3) ◽  
pp. 150 ◽  
Author(s):  
Chunshuai Huang ◽  
Chunfang Yang ◽  
Zhuangjie Fang ◽  
Liping Zhang ◽  
Wenjun Zhang ◽  
...  
Keyword(s):  
Spectroscopic Data ◽  
Bioinformatics Analysis ◽  
Biological Activities ◽  
Side Chain ◽  
X Ray Diffraction ◽  
X Ray ◽  
Aromatic Polyketides ◽  
Plausible Mechanism ◽  
Encoding Gene

Diazobenzofluorene-containing atypical angucyclines exhibit promising biological activities. Here we report the inactivation of an amidotransferase-encoding gene flsN3 in Micromonospora rosaria SCSIO N160, a producer of fluostatins. Bioinformatics analysis indicated that FlsN3 was involved in the diazo formation. Chemical investigation of the flsN3-inactivation mutant resulted in the isolation of a variety of angucycline aromatic polyketides, including four racemic aminobenzo[b]fluorenes stealthins D–G (9–12) harboring a stealthin C-like core skeleton with an acetone or butanone-like side chain. Their structures were elucidated on the basis of nuclear magnetic resonance (NMR) spectroscopic data and X-ray diffraction analysis. A plausible mechanism for the formation of stealthins D–G (9–12) was proposed. These results suggested a functional role of FlsN3 in the formation/modification of N–N bond-containing fluostatins.

scholarly journals Two New Isocoumarin Derivatives from an Endophytic Fungi Pestalotiopsis coffeae Isolated from a Mangrove Fishtail Palm

2018 ◽  
Vol 13 (1) ◽  
pp. 1934578X1801300 ◽  
Author(s):  
Zhong Wang ◽  
Peng Fan ◽  
Tong-Dan Xue ◽  
Lin-Lin Meng ◽  
Wen-Bin Gao ◽  
...  
Keyword(s):  
Carboxylic Acid ◽  
Endophytic Fungi ◽  
Endophytic Fungus ◽  
Spectroscopic Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chinese Plant

Two new isocoumarin derivatives, 6,8-dihydroxy-7-methyl-1-oxo-1H-isochromene-3-carboxylic acid (1) and 6,8-dihydroxy-3-methoxy-3,7- dimethyl-isochroman-1-one (2), together with five known compounds (3-7), were isolated from the endophytic fungus Pestalotiopsis coffeae derived from the Chinese plant fishtail palm. The structures of these compounds were determined mainly by analysis of their NMR spectroscopic data. The structure of compound 2 was further confirmed by X-ray diffraction.

scholarly journals Reactions of Dihaloboranes with Electron-Rich 1,4-Bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadienes

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2875
Author(s):  
Li Ma ◽  
Xiaolin Zhang ◽  
Wenbo Ming ◽  
Shengxin Su ◽  
Xiaoyong Chang ◽  
...  
Keyword(s):  
Double Bond ◽  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
1H Nmr Spectroscopy ◽  
Variable Temperature ◽  
Organosilicon Compounds ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Bond Character

The reactions of electron-rich organosilicon compounds 1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (1), 2,3,5,6-tetramethyl-1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (2), and 1,1′-bis(trimethylsilyl)-1,1′-dihydro-4,4′-bipyridine (12) with B-amino and B-aryl dihaloboranes afforded a series of novel B=N-bond-containing compounds 3–11 and 13. The B=N rotational barriers of 7 (>71.56 kJ/mol), 10 (58.79 kJ/mol), and 13 (58.65 kJ/mol) were determined by variable-temperature 1H-NMR spectroscopy, thus reflecting different degrees of B=N double bond character in the corresponding compounds. In addition, ring external olefin isomers 11 were obtained by a reaction between 2 and DurBBr2. All obtained B=N-containing products were characterized by multinuclear NMR spectroscopy. Compounds 5, 9, 10a, 11, and 13a were also characterized by single-crystal X-ray diffraction analysis.

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