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1.
Ligand π‐Radical Interaction with f‐Shell Unpaired Electrons in Phthalocyaninato–Lanthanoid Single‐Molecule Magnets: A Solution NMR Spectroscopic and DFT Study
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Marko Damjanović Takaumi Morita Prof. Keiichi Katoh Prof. Masahiro Yamashita Prof. Markus Enders 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(41):14421-14432
The phthalocyaninato double‐decker complexes [M(obPc)2]0 (M= YIII, TbIII, DyIII; obPc=2,3,9,10,16,17,23,24‐octabutoxyphthalocyaninato), along with their reduced ([M(obPc)2]?[P(Ph)4]+; M=TbIII, DyIII) and oxidized ([M(obPc)2]+[SbCl6]? (M=YIII, TbIII) counterparts were studied with 1H, 13C and 2D NMR. From the NMR data of the neutral (i.e., with one unpaired electron in the ligands) and anionic TbIII complexes, along with the use of dispersion corrected DFT methods, it was possible to separate the metal‐centered and ligand‐centered contributions to the hyperfine NMR shift. These contributions to the 1H and 13C hyperfine NMR shifts were further analyzed in terms of pseudocontact and Fermi contact shifts. Furthermore, from a combination of NMR data and DFT calculations, we have determined the spin multiplicity of the neutral complexes [M(obPc)2]0 (M=TbIII and DyIII) at room temperature. From the NMR data of the cationic TbIII complex, for which actually no experimental structure determination is available, we have analyzed the structural changes induced by oxidation from its neutral/anionic species and shown that the interligand distance decreases upon oxidation. The fast electron exchange process between the neutral and anionic TbIII double‐decker complexes was also studied. 相似文献
2.
《Magnetic resonance in chemistry : MRC》2002,40(3):175-181
A 1H, 13C and 31P NMR study of monoethyl (HL1) and monobutyl (HL2) esters of (α‐anilinobenzyl)phosphonic acid and their metallocyclic dipalladium complexes (Pd2L4,L = L1, L2) in DMSO‐d6 was performed, based on 1D and 2D homo‐ and heteronuclear experiments including 1H,13C,31P,APT,1H–1H COSY, 1H–13C COSY, gs‐HMQC and gs‐HMBC NMR techniques. The results obtained are discussed with respect to those for some palladium(II) complexes reported for various anilinobenzylphosphonate derivatives. Copyright © 2002 John Wiley & Sons, Ltd. 相似文献
3.
Two new non‐metallic filled β‐manganese phases M2Ga6Te10 (M: Li, Na) are obtained as black, homogeneous, microcristalline samples as well as single crystals by direct reaction of the elements. According to the single crystal structure determinations both compounds crystallize in space group R32 (No. 155, Z = 2) with the lattice constants: a = 1436.9(2), c = 1759.0(4) pm (T = 180 K, Li2Ga6Te10) and a = 1458(1) pm, c = 1776.1(4) pm (T = 290 K, Na2Ga6Te10). Their structures are characterized by tetrahedral close packings of Te2–, corresponding to the arrangement of Mn atoms in β‐Mn. While Ga3+ ions are distributed in an ordered way over 12% of the tetrahedral holes, the M+ ions occupy all distorted octahedral (“metaprismatic”) holes. As the Li+ ions are too small they occupy off‐center positions inside the metaprisms. Positions with the strongest off‐centering can only be refined on the basis of a split model. MAS‐NMR measurements, including multiple quantum NMR, allowed the two different crystallographic M+ sites to be distinguished unambigously by separate 7Li and 23Na signals, respectively. The assignment of the NMR signals was supported by measurements of samples in which Li+ was partly substituted by larger cations (Sn2+, Pb2+). 相似文献
4.
Construction of Two 3D Main Group Coordination Polymers Based on 2‐(2‐Pyridyl)‐4,5‐imidazole‐dicarboxylic Acid: Structures and Luminescent Properties
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Ronghua Zeng Jinhui Liang Lujing Lin Xiaodian Chen Tingting Wang Sheng‐Run Zheng Daohang He 《无机化学与普通化学杂志》2015,641(15):2677-2682
Two main group coordination polymers based on 2‐(2‐pyridyl)‐4,5‐imidazole‐dicarboxylic acid (H3oPyIDC), namely [Ba(H2oPyIDC)2(H2O)]n ( 1 ) and [Pb2(HoPyIDC)2]n ( 2 ) are obtained under hydrothermal conditions. In compound 1 , the Ba2+ cations and HoPyIDC2– anions are connected to a 1D chain, and the 1D chains are further interconnected by Ba–O bonds, forming a 3D 3‐connected framework. In compound 2 , a 2D layer with (4,4) topology is formed by PbII ions and HoPyIDC2– anions. The 2D layer are pillared by HoPyIDC2–, yielding a 3D (3,4)‐connected framework. The thermogravimetric analyses and luminescence properties of compounds 1 and 2 are also investigated. 相似文献
5.
《Magnetic resonance in chemistry : MRC》2003,41(11):908-920
Structure elucidation of compounds in the benzisoxazole series ( 1 – 6 ) and naphtho[1,2‐d][1,3]‐ ( 7 – 10 ) and phenanthro[9,10‐d][1,3]oxazole ( 11 – 14 ) series was accomplished using extensive 2D NMR spectroscopic studies including 1H–1H COSY, long‐ range 1H–1H COSY, 1H–13C COSY, gHMQC, gHMBC and gHMQC‐TOCSY experiments. The distinction between oxazole and isoxazole rings was made on the basis of the magnitude of heteronuclear one‐bond 1JC2, H2 (or 1JC3, H3) coupling constants. Complete analysis of the 1H NMR spectra of 11 – 14 was achieved by iterative calculations. Gradient selected gHMQC‐TOCSY spectra of phenanthro[9,10‐d][1,3]oxazoles 11 – 14 were obtained at different mixing times (12, 24, 36, 48 and 80 ms) to identify the spin system where the protons of phenanthrene ring at H‐5, H‐6 and at H‐9 and H‐7 and H‐8 were highly overlapping. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
6.
Yun‐Chih Lin Dr. Hung‐Lung Chou Dr. Loka Subramanyam Sarma Dr. Bing‐Joe Hwang Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2009,15(40):10658-10665
Understanding the complex thermodynamic behavior of confined amphiphilic molecules in biological or mesoporous hosts requires detailed knowledge of the stacking structures. Here, we present detailed solid‐state NMR spectroscopic investigations on 1‐butanol molecules confined in the hydrophilic mesoporous SBA‐15 host. A range of NMR spectroscopic measurements comprising of 1H spin–lattice (T1), spin–spin (T2) relaxation, 13C cross‐polarization (CP), and 1H,1H two‐dimensional nuclear Overhauser enhancement spectroscopy (1H,1H 2D NOESY) with the magic angle spinning (MAS) technique as well as static wide‐line 2H NMR spectra have been used to investigate the dynamics and to observe the stacking structure of confined 1‐butanol in SBA‐15. The results suggest that not only the molecular reorientation but also the exchange motions of confined molecules of 1‐butanol are extremely restricted in the confined space of the SBA‐15 pores. The dynamics of the confined molecules of 1‐butanol imply that the 1H,1H 2D NOESY should be an appropriate technique to observe the stacking structure of confined amphiphilc molecules. This study is the first to observe that a significant part of confined 1‐butanol molecules are orientated as tilted bilayered structures on the surface of the host SBA‐15 pores in a time‐average state by solid‐state NMR spectroscopy with the 1H,1H 2D NOESY technique. 相似文献
7.
Roel Prins 《Angewandte Chemie (International ed. in English)》2019,58(43):15548-15552
A non‐spinel model for the structure of γ‐Al2O3, with 25 % of the Al3+ cations at tetrahedral positions, has been the subject of wide interest. However, 17O NMR measurements and, more recently, 27Al NMR measurements have shown that there are considerably more Al3+ cations at tetrahedral positions. This means that the Al3+ vacancies in γ‐Al2O3 are not at tetrahedral but at octahedral positions, as in isostructural γ‐Fe2O3 and in accordance with density functional theory predictions. This has consequences with regard to the surface structure of γ‐Al2O3, and thus, for catalysis. 相似文献
8.
P. Haranath M. F. Stephen Babu U. Anasuyamma C. Naga Raju C. Suresh Reddy 《Heteroatom Chemistry》2005,16(7):572-575
Novel 3 substituted 1,5‐dihydro‐2,4,3‐benzodioxaphosphepine 3‐oxides ( 5a–h ) were synthesized by reacting 1,2‐benzenedimethanol ( 1 ) with phosphorus tribromide in the presence of triethylamine at 0–30°C and subsequent reaction of the monobromide ( 2 ) with different Grignard reagents ( 3 ) at room temperature. The products ( 4 ) were converted to corresponding oxides 5a–i by oxidation with H2O2 at room temperature. The chemical structures of all the products were confirmed by analytical, IR and NMR (1H, 13C, and 31P) spectral data. Their antifungal and antibacterial activity is also evaluated. Most of these compounds exhibited moderate antimicrobial activity in the assay. © 2005 Wiley Periodicals, Inc. Heteroatom Chem 16:572–575, 2005; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20154 相似文献
9.
《Magnetic resonance in chemistry : MRC》2003,41(11):969-973
1H and 13C NMR spectral data for diethyl 2‐ and 8‐quinolylmethylphosphonates (L) and their palladium(II) dihalide complexes, trans‐[PdL2X2] (L = 2‐dqmp, 8‐dqmp; X = Cl, Br), are presented. The NMR analysis was performed on the basis of one‐ and two‐dimensional homo‐ and heteronuclear experiments including 1H, 13C, APT, 1H–1H COSY, 1H–13C COSY, HMQC and HMBC techniques. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
10.
Wei Zhang 《Magnetic resonance in chemistry : MRC》2013,51(7):431-434
A one‐step method was reported for the synthesis of 6‐acetamido‐3‐(N‐(2‐(dimethylamino) ethyl) sulfamoyl) naphthalene‐1‐yl 7‐acetamido‐4‐hydroxynaphthalene‐2‐sulfonate by treating 7‐acetamido‐4‐hydroxy‐2‐naphthalenesulfonyl chloride with equal moles of N, N‐dimethylethylenediamine in acetonitrile in the presence of K2CO3. The chemical structure of the obtained compounds was characterized by MS, FTIR, 1H NMR, 13C NMR, gCOSY, TOCSY, gHSQC, and gHMBC. The chemical shift differences of 1H and 13C being δ 0.04 and 0.2, respectively, were unambiguously differentiated. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
11.
《Magnetic resonance in chemistry : MRC》2003,41(12):1015-1020
Complex formation between N‐butylboronic acid and D ‐(+)‐glucose, D ‐(+)‐mannose, methyl‐α‐D ‐glucopyranoside, methyl‐β‐D ‐galactopyranoside and methyl α‐D ‐mannopyranoside under neutral conditions was investigated by 1H, 13C and 11B NMR spectroscopy and gas chromatography–mass spectrometry (GC–MS) D ‐(+)‐Glucose and D ‐(+)‐mannose formed complexes where the boronates are attached to the 1,2:4,6‐ and 2,3:5,6‐positions of the furanose forms, respectively. On the other hand, the boronic acid binds to the 4,6‐positions of the two methyl derivatives of glucose and galactose. Methyl α‐D ‐mannopyranoside binds two boronates at the 2,3:4,6‐positions. 11B NMR was used to show the ring size of the complexed sugars and the boronate. GC–MS confirmed the assignments. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
12.
Jinhong Song Prof. Dr. Zhiming Zhou Dan Cao Haifeng Huang Lixuan Liang Kai Wang Jun Zhang 《无机化学与普通化学杂志》2012,638(5):811-820
Energetic salts that contain nitrogen‐rich cations and the 2‐(dinitromethyl)‐3‐nitro‐1, 3‐diazacyclopent‐1‐ene anion were synthesized in high yield by direct neutralization reactions. The resulting salts were fully characterized by multinuclear NMR spectroscopy (1H and 13C), vibrational spectroscopy (IR), elemental analysis, density and differential scanning calorimetry (DSC), and elemental analysis. Additionally, the structures of the ammonium ( 1 ) and isopropylideneaminoguanidinium ( 9 ) 2‐(dinitromethyl)‐3‐nitro‐1, 3‐diazacyclopent‐l‐ene salts were confirmed by single‐crystal X‐ray diffraction. Solid‐state 15N NMR spectroscopy was used as an effective technique to further determine the structure of some of the products. The densities of the energetic salts paired with organic cations fell between 1.50 and 1.79 g · cm–3 as measured by a gas pycnometer. Based on the measured densities and calculated heats of formation, detonation pressures and velocities were calculated using Explo 5.05 and found to to be 25.2–35.5 GPa and 7949–9004 m · s–1, respectively, which make them competitive energetic materials. 相似文献
13.
N‐acetyl‐4‐nitrotryptophan methyl ester (2), N‐acetyl‐5‐nitrotryptophan methyl ester (3), N‐acetyl‐6‐nitrotryptophan methyl ester (4) and N‐acetyl‐7‐nitrotryptophan methyl ester (5) were synthesized through a modified malonic ester reaction of the appropriate nitrogramine analogs followed by methylation with BF3‐methanol. Assignments of the 1H and 13C NMR chemical shifts were made using a combination of 1H–1H COSY, 1H–13C HETCOR and 1H–13C selective INEPT experiments. Copyright © 2008 Crown in the right of Canada. Published by John Wiley & Sons, Ltd 相似文献
14.
Tracking “Apolar” NMe4+ Ions within Two Polyoxothiomolybdates that Have the Same Pores: Smaller Clathrate and Larger Highly Porous Clusters in Action
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Dr. Vladimir S. Korenev Antoine G. Boulay Dr. Mohamed Haouas Dr. Fatma Bannani Prof. Dr. Vladimir P. Fedin Prof. Dr. Maxim N. Sokolov Emmanuel Terazzi Somenath Garai Prof. Dr. Achim Müller Dr. Francis Taulelle Dr. Jérôme Marrot Dr. Nathalie Leclerc Dr. Sébastien Floquet Prof. Dr. Emmanuel Cadot 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(11):3097-3105
15.
Annemarie A. M. L. Huijbrechts Junrong Huang Henk A. Schols Barend van Lagen Gerben M. Visser Carmen G. Boeriu Ernst J. R. Sudhölter 《Journal of polymer science. Part A, Polymer chemistry》2007,45(13):2734-2744
New reactive unsaturated starch derivatives, 1‐allyloxy‐2‐hydroxy‐propyl‐starches (AHP‐starches), were synthesized by the reaction of waxy maize starch (WMS) and amylose‐enriched maize starch (AEMS) with allyl glycidyl ether in a heterogeneous alkaline suspension containing NaOH and Na2SO4. The degree of substitution (DS) was determined by 1H NMR spectroscopy, and a DS of 0.20 ± 0.01 was found for both AHP‐WMS and AHP‐AEMS, respectively. The AHP derivatives of WMS and AEMS were further characterized with 1H and 13C NMR. It was shown that the AHP substitution was located on the C‐6 hydroxyl group of the glucose residues in the starch. The substitution pattern of the AHP groups along the polymer chain was randomly clustered, as determined by enzymatic digestion using pullulanase, α‐amylase, and amyloglucosidase, followed by matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry analysis of the digestion products. With X‐ray diffraction and scanning electron microscopy, no changes in the granular morphology and crystallinity between the unmodified starches and AHP‐starches were detected. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 2734–2744, 2007 相似文献
16.
Proton Order–Disorder Phenomena in a Hydrogen‐Bonded Rhodium–η5‐Semiquinone Complex: A Possible Dielectric Response Mechanism
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Dr. Minoru Mitsumi Kazunari Ezaki Yuuki Komatsu Prof. Dr. Koshiro Toriumi Dr. Tatsuya Miyatou Prof. Dr. Motohiro Mizuno Nobuaki Azuma Prof. Dr. Yuji Miyazaki Prof. Dr. Motohiro Nakano Prof. Dr. Yasutaka Kitagawa Dr. Takayasu Hanashima Dr. Ryoji Kiyanagi Dr. Takashi Ohhara Prof. Dr. Kazuhiro Nakasuji 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(27):9682-9696
A newly synthesized one‐dimensional (1D) hydrogen‐bonded (H‐bonded) rhodium(II)–η5‐semiquinone complex, [Cp*Rh(η5‐p‐HSQ‐Me4)]PF6 ([ 1 ]PF6; Cp*=1,2,3,4,5‐pentamethylcyclopentadienyl; HSQ=semiquinone) exhibits a paraelectric–antiferroelectric second‐order phase transition at 237.1 K. Neutron and X‐ray crystal structure analyses reveal that the H‐bonded proton is disordered over two sites in the room‐temperature (RT) phase. The phase transition would arise from this proton disorder together with rotation or libration of the Cp* ring and PF6? ion. The relative permittivity εb′ along the H‐bonded chains reaches relatively high values (ca., 130) in the RT phase. The temperature dependence of 13C CP/MAS NMR spectra demonstrates that the proton is dynamically disordered in the RT phase and that the proton exchange has already occurred in the low‐temperature (LT) phase. Rate constants for the proton exchange are estimated to be 10?4–10?6 s in the temperature range of 240–270 K. DFT calculations predict that the protonation/deprotonation of [ 1 ]+ leads to interesting hapticity changes of the semiquinone ligand accompanied by reduction/oxidation by the π‐bonded rhodium fragment, producing the stable η6‐hydroquinone complex, [Cp*Rh3+(η6‐p‐H2Q‐Me4)]2+ ([ 2 ]2+), and η4‐benzoquinone complex, [Cp*Rh+(η4‐p‐BQ‐Me4)] ([ 3 ]), respectively. Possible mechanisms leading to the dielectric response are discussed on the basis of the migration of the protonic solitons comprising of [ 2 ]2+ and [ 3 ], which would be generated in the H‐bonded chain. 相似文献
17.
The reaction of tetra(alkyn‐1‐yl)silanes Si(C?C‐R1)4 1 [R1 = tBu ( a ), Ph ( b ), C6H4‐4‐Me ( c )] with 9‐borabicyclo[3.3.1]nonane (9‐BBN) in a 1:2 ratio affords the spirosilane derivatives 5a – c as a result of twofold intermolecular 1,2‐hydroboration, followed by twofold intramolecular 1,1‐organoboration. Intermediates 3a–c , in which two alkenyl‐ and two alkyn‐1‐yl groups are linked to silicon, were identified by NMR spectroscopy. The molecular structure of the spiro compound 5c was determined by X‐ray analysis, and the solution‐state structures of products and intermediates follow conclusively from the consistent NMR spectroscopic data sets (1H, 11B, 13C and 29Si NMR). Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
18.
Five cationic complexes of the general formula [Cp′2Ti(A)2]2+ [Cl?]2 [Cp′ = η5‐(CH3)C5H4 and A = glycine, 1 ; 2‐methylalanine, 2 ; N‐methylglycine, 3 ; L ‐alanine, 4 ; and D ‐alanine 5 ] were prepared by the reaction of Cp′2TiCl2 and the appropriate α‐amino acid in 1:2 molar ratio from methanol–water solution in high yield. Air‐stable crystalline solids, highly soluble in water, were characterized by means of elemental analysis, IR, Raman, 1H, 13C and 14N NMR spectroscopy. The structure of compound 3 was determined by single crystal X‐ray crystallography: orthorhombic Pbca No. 61, a = 9.5310(3), b = 18.2980(5), c = 26.6350(5) Å, V = 4654 Å3, Z = 8. Hydrolytic stability of all compounds in D2O was investigated using 1H NMR spectroscopy within the pD interval of 2.9–6.5. All compounds slowly decomposed during 24 h at pD = 2.94, forming a mixture of hydrolytic products [Cp′2Ti(A)(D2O)]2+, [Cp′2Ti(D2O)2]2+ and respective α‐amino acids. By elevating pD to 4.0 and up to 6.5, a yellowish precipitate was formed, which indicates decomposition of the complexes. These compounds were characterized using elemental analyses, IR and Raman spectroscopy and attributed to oligomeric and/or polymeric structures described empirically by the formula Ti(Cp′)xOy(OH)z (x = 0.65; y = 0.3, z = 1.9). Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
19.
Nutalapati Venkatramaiah Ricardo F. Mendes Artur M. S. Silva Joo P. C. Tom Filipe A. Almeida Paz 《Acta Crystallographica. Section C, Structural Chemistry》2016,72(9):685-691
The preparation of coordination polymers (CPs) based on either transition metal centres or rare‐earth cations has grown considerably in recent decades. The different coordination chemistry of these metals allied to the use of a large variety of organic linkers has led to an amazing structural diversity. Most of these compounds are based on carboxylic acids or nitrogen‐containing ligands. More recently, a wide range of molecules containing phosphonic acid groups have been reported. For the particular case of Ca2+‐based CPs, some interesting functional materials have been reported. A novel one‐dimensional Ca2+‐based coordination polymer with a new organic linker, namely poly[[diaqua[μ4‐(4,5‐dicyano‐1,2‐phenylene)bis(phosphonato)][μ3‐(4,5‐dicyano‐1,2‐phenylene)bis(phosphonato)]dicalcium(II)] tetrahydrate], {[Ca2(C8H4N2O6P2)2(H2O)2]·4H2O}n, has been prepared at ambient temperature. The crystal structure features one‐dimensional ladder‐like ∞1[Ca2(H2cpp)2(H2O)2] polymers [H2cpp is (4,5‐dicyano‐1,2‐phenylene)bis(phosphonate)], which are created by two distinct coordination modes of the anionic H2cpp2− cyanophosphonate organic linkers: while one molecule is only bound to Ca2+ cations via the phosphonate groups, the other establishes an extra single connection via a cyano group. Ladders close pack with water molecules through an extensive network of strong and highly directional O—H…O and O—H…N hydrogen bonds; the observed donor–acceptor distances range from 2.499 (5) to 3.004 (6) Å and the interaction angles were found in the range 135–178°. One water molecule was found to be disordered over three distinct crystallographic positions. A detailed solution‐state NMR study of the organic linker is also provided. 相似文献
20.
The complex cis‐[RuIII(dmbpy)2Cl2](PF6) ( 2 ) (dmbpy = 4, 4′‐dimethyl‐2, 2′‐bipyridine) was obtained from the reaction of cis‐[RuII(dmbpy)2Cl2] ( 1 ) with ammonium cerium(IV) nitrate followed by precipitation with saturated ammonium hexafluoridophosphate. The 1H NMR spectrum of the RuIII complex confirms the presence of paramagnetic metal atoms, whereas that of the RuII complex displays diamagnetism. The 31P NMR spectrum of the RuIII complex shows one signal for the phosphorus atom of the PF6– ion. The perspective view of each [RuII/III(dmbpy)2Cl2]0/+ unit manifests that the ruthenium atom is in hexacoordinate arrangement with two dmbpy ligands and two chlorido ligands in cis position. As the oxidation state of the central ruthenium metal atom becomes higher, the average Ru–Cl bond length decreases whereas the Ru–N (dmbpy) bond length increases. The cis‐positioned dichloro angle in RuIII is 1.3° wider than that in the RuII. The dihedral angles between pair of planar six‐membered pyridyl ring in the dmbpy ligand for the RuII are 4.7(5)° and 5.7(4)°. The observed inter‐planar angle between two dmbpy ligands in the RuII is 89.08(15)°, whereas the value for the RuIII is 85.46(20)°. 相似文献