The structures, solvent-free synthesis and interconversions of the complexes [MCl2(CEAP)2] and their hydrogen-bonded salts [CEAPH]2[MCl4] {M=Zn, Co and Hg, CEAP=4-[N,N-bis(2-cyanoethyl)amino]pyridine}

Ni, Jun; Pan, Yuzhen; Wei, Zhi-Rui; Cong, Qian; Zhang, Dong; Wang, You-Gui; Liu, Xiaoyu

doi:10.1016/j.inoche.2013.01.008

Cited by 6 publications

(4 citation statements)

References 27 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Two mechanochemical methods were developed to prepare [CoCl 2 (CEAP) 2 ] 381 (CEAP = 4-[ N , N -bis(2-cyanoethyl)amino]pyridine, 378 ) . CEAP and CoCl 2 ·6H 2 O (2:1 ratio) or [CEAPH] 2 [CoCl 4 ] 380 and KOH were ground in an agate mortar and pestle for 15 min to produce the same complex 381 .…”

Section: Groupmentioning

confidence: 99%

“…As for ferrocene, nickelocene 475 could be synthesized by grinding NiCl 2 and TlCp in a 1:1.8 ratio for 60 min using an original homemade vibratory ball mill (90% yield, Scheme ). Similarly, grinding together NiCl 2 ·6H 2 O with paratoluidine in a 1:2 stoichiometric ratio for 15 min provided dichlorobis(paratoluidine) nickel(II) in 95% yield . Using an analogous strategy, and as reported for cobalt complexes, [NiCl 2 (4-PhPy) 4 ] could be mechanosynthesized directly and easily from 4-PhPy and NiCl 2 and confirmed by PXRD analysis …”

Section: Group 10mentioning

confidence: 99%

“…As already described with a copper source (Figure ), manual grinding of anhydrous gabapentin 584 with ZnCl 2 for 5 min with an agate mortar and pestle gave access to [ZnCl 2 (gabapentin) 2 ] 585 in quantitative yield (Scheme , reaction A) . Similarly, [MCl 2 (CEAP) 2 ] 586 and the corresponding hydrogen-bonded salts [CEAPH] 2 [MCl 4 ] (M = zinc or mercury) were synthesized mechanochemically using CEAP 378 or CEAP·HCl as ligand source and MCl 2 as metal source, respectively (Scheme , reaction B) . Interconversion of [MCl 2 (CEAP) 2 ] and [CEAPH] 2 [MCl 4 ] was possible either through grinding in the presence of a base or through absorption of HCl vapors.…”

Section: Group 12mentioning

confidence: 99%

“…146 Similarly, grinding together NiCl 2 •6H 2 O with para-toluidine in a 1:2 stoichiometric ratio for 15 min provided dichlorobis(paratoluidine) nickel(II) in 95% yield. 228 Using an analogous strategy, and as reported for cobalt complexes, [NiCl 2 (4-PhPy) 4 ] could be mechanosynthesized directly and easily from 4-PhPy and NiCl 2 and confirmed by PXRD analysis. 226…”

Section: Photochemical Synthesis Of Iridium Complexesmentioning

confidence: 99%

See 3 more Smart Citations

Alternative Technologies That Facilitate Access to Discrete Metal Complexes

et al. 2019

View full text Add to dashboard Cite

Organometallic complexes: these two words jump to the mind of the chemist and are directly associated with their utility in catalysis or as a pharmaceutical. Nevertheless, to be able to use them, it is necessary to synthesize them, and it is not always a small matter. Typically, synthesis is via solution chemistry, using a roundbottom flask and a magnetic or mechanical stirrer. This review takes stock of alternative technologies currently available in laboratories that facilitate the synthesis of such complexes. We highlight five such technologies: mechanochemistry, also known as solvent-free chemistry, uses a mortar and pestle or a ball mill; microwave activation can drastically reduce reaction times; ultrasonic activation promotes chemical reactions because of cavitation phenomena; photochemistry, which uses light radiation to initiate reactions; and continuous flow chemistry, which is increasingly used to simplify scaleup. While facilitating the synthesis of organometallic compounds, these enabling technologies also allow access to compounds that cannot be obtained in any other way. This shows how the paradigm is changing and evolving toward new technologies, without necessarily abandoning the round-bottom flask. A bright future is ahead of the organometallic chemist, thanks to these novel technologies. CONTENTS1. Introduction 7530 2. Technologies 7530 2.1. Grinding and Milling 7530 2.2. Microwave Irradiation 7531 2.3. Ultrasound Activation 7531 2.4. Photochemistry 7532 2.5. Continuous Flow 7532 3. Contribution of Each Technology Compared to Classical Syntheses 7533 4. Lithium and Magnesium 7534 4.1. Mechanochemical Access to Grignard Reagents 7534 4.2. Microwave Irradiation for the Synthesis of Magnesium Complexes 7534 4.3. Ultrasonic Procedures 7535 4.4. Continuous Flow Syntheses 7535 5. Groups 2, 3, 4, and 5 7537 5.1. Mechanochemical Procedures for Complexes of Groups 2, 3, and 4 7537 5.2. Microwave Irradiation for the Synthesis of Vanadium Complexes 7537 5.3. Synthesis of Vanadium Complexes Using Ultrasound 7538 6. Group 6 7538 6.1. Mechanosynthesis of Molybdenum and Chromium Complexes 7538 6.2. Microwave Irradiation for the Synthesis of Group 6 Metal Complexes 7539 6.3. Photochemistry for Synthesis of Group 6 Metal Complexes 7543 6.4. Continuous Flow Chemistry for Synthesis of Chromium Complexes 7545 7. Group 7 7545 7.1. Mechanosynthesis of Rhenium Complexes 7545 7.2. Microwave Irradiation for the Synthesis of Group 7 Metal Complexes 7546 7.3. Photochemical Synthesis of Manganese and Rhenium Complexes 7549 8. Group 8 7550 8.1. Synthesis of Iron and Ruthenium Complexes Using Ball Milling 7550 8.2. Microwave Procedures 7552 8.3. Ultrasonic Irradiation for Iron Complexes 7562 8.4. Syntheses of Iron and Ruthenium Complexes Using Photochemistry 7563 8.5. Continuous Flow Conditions to Prepare Iron and Ruthenium Complexes 7566 9. Group 9 7566 9.1. Synthesis of Cobalt and Rhodium Complexes by Mechanochemistry 7566 9.2. Procedures Using Microwave Irradiation 7569 9.3. Photochemical Synthesis of Iridium Complexes 7...

show abstract

Section: Groupmentioning

confidence: 99%

Section: Group 10mentioning

confidence: 99%

Section: Group 12mentioning

confidence: 99%

Section: Photochemical Synthesis Of Iridium Complexesmentioning

confidence: 99%

See 2 more Smart Citations

Alternative Technologies That Facilitate Access to Discrete Metal Complexes

et al. 2019

View full text Add to dashboard Cite

show abstract

Metal Complexes in Mechanochemistry

León¹,

Garcı́a²

2021

Comprehensive Coordination Chemistry III

View full text Add to dashboard Cite

Mechanochemical and thermal formation of 1H-benzotriazole coordination polymers and complexes of 3d-transition metals with intriguing dielectric properties

et al. 2016

View full text Add to dashboard Cite

Liquid-assisted grinding (LAG) reactions have been successfully applied to achieve a series of complexes and coordination polymers based on divalent 3d-transition metal chlorides (TM chlorides) and the aromatic ligand 1H-benzotriazole (BtzH). The obtained substances were investigated via single crystal X-ray, powder X-ray determination and simultaneous DTA/TG analysis as model compounds for structural and chemical influences on their dielectric properties. Depending on the synthesis method, different constitutions and structures are observed. Two polymorphous forms of the 1D polymer [MnCl2(BtzH)2] (1 and 2) as well as the complexes [ZnCl2(BtzH)2]·BtzH (3) and [CoCl2(BtzH)2]·BtzH (4) have been obtained as phase-pure bulk substances via the mechanochemical LAG route, and even single crystals are available. For comparison, thermal reactions were also carried out and have led to the formation of the neutral complexes: [CoCl2(BtzH)2] (5) and [CoCl2(BtzH)4]·4BtzH (6), [ZnCl2(BtzH)2] (7) and the anionic complex BtzH2[CoCl3BtzH] (8). In addition, thermal treatment of 3 yields the benzotriazolium salt {(BtzH)2H}Cl (9). The transition metal compounds were additionally analysed regarding their dielectric properties by frequency-dependent as well as temperature-dependent permittivity investigations. It is intriguing that compounds 1 and 3 show remarkably low dielectric constants and loss factors up to 50 °C highlighting them as potential "low-k materials".

show abstract

The structures, solvent-free synthesis and interconversions of the complexes [MCl2(CEAP)2] and their hydrogen-bonded salts [CEAPH]2[MCl4] {M=Zn, Co and Hg, CEAP=4-[N,N-bis(2-cyanoethyl)amino]pyridine}

Cited by 6 publications

References 27 publications

Alternative Technologies That Facilitate Access to Discrete Metal Complexes

Alternative Technologies That Facilitate Access to Discrete Metal Complexes

Metal Complexes in Mechanochemistry

Mechanochemical and thermal formation of 1H-benzotriazole coordination polymers and complexes of 3d-transition metals with intriguing dielectric properties

Contact Info

Product

Resources

About