Three New Hydrogenosuccinate and Succinate Adducts Complexes:Synthesis and Spectroscopic Study

One new hydrogenosuccinate and two succinate adduct and complex have been synthesized and studied by infrared,UV-Visible and NMR(Nuclear Magnetic Resonance Spectroscopy)^(119)Sn spectroscopies.The suggested structure is discrete,the hydrogenosuccinate behaving as a monodentate ligand or only involved in hydrogen bonding,the environment around the magnesium centre being triangular(compound 3).The succiate anion is a monochelating ligand(compound 1 and 2).In all the suggested structures,when extra hydrogen bonds are considered,supramolecular architectures are obtained(compound 2 and 3).

Synthesis and Crystal Structure of Fe(aapo)_2Cl_3(aapo=2-Acetylamino Pyridine N-Oxide)

The complex Fe(aapo)2Cl3 with chemical formula C14H16Cl3FeN4O4 was obtained by the reaction of FeCl36H2O with apoHCl (apo = 2璦mino pyridine N璷xide) in acetonitrile. The result shows that CH3CN has been hydrolysised with the water from FeCl36H2O dissolving, and then the hydrolysised product condenses with apo to give aapo. A single-crystal X璻ay study of Fe(aapo)2Cl3 shows it belongs to the monoclinic system, space group C2/c with a = 15.873(3), b = 10.322(2), c = 11.987(2) ? b = 106.35(1), V = 1884.5(6) 3, Z = 4, Mr = 466.51, Dc = 1.644 g/cm3, m(MoKa) = 1.253 mm-1, F(000) = 948, R = 0.0377 and wR = 0.0749 for 1262 observed reflections with I > 2(I). Fe (Ⅲ) is coordinated by a trigonal bipyramidal geometry with three chlorine atoms lying on the equatorial plane and two oxygen atoms connected with the nitrogen atoms of pyridine rings occupying the axial positions, while the iron and Cl(1) atoms lie on the crystallographic 2-fold axis. The dihedral angle of two pyridine rings is 71.74(9). There exist N(2)H(2)…O(1)?hydrogen bonds in the crystal structure.

Crystal Structure of 2-Germatranylmethyl-N-(4'-methylphenyl) succinimide

The title crystal of 2-germatranylmethyl-N- (4'-methylphenyl)succinimide (C18H24GeN2O5) was determined by single crystal X-ray diffraction- The crystalbelongs to the orthorhombic system, space group P212121 with Mr = 420. 99, a= 6. 716(1), b=22- 860(8), c= 11. 891 (3) A, V= 1826(1) A3, Z=4,Dx= 1. 53 Mg. m-3,A= 0. 71073A, μ= 1. 684 mm-l, and F(000) =872. The structure was solved by direct methods. The final refinement is converged with unweighted and weighted agreement factors of 0. 047 and 0. 064 for 1610 observed reflections with I≥3δ(I). The results of structure analysis indicate that the framework of this five-coordinated germanium compound is a distorted trigonal bipyramid(TBP).

Synthesis and Uncommon Structural Characterization of Novel Zinc and Cadmium Complexes with Imino Nitroxide Radical

Two novel complexes {[Zn（IM4py）2（tp）（H2O）]2H2O}. 1 and {[Cd（IM4py）2（tp）- （H2O）]1.25H2O},, 2 （IM4py = 2-（4＇-pyridinyl）-4,4,5,5-tetramethylimidazoline-l-oxyl and tp = terephthalate dianion） have been synthesized and characterized by elemental analyses, IR spectrum and single-crystal X-ray diffraction. Crystal data for complex I： monoclinic, space group C2/c, a = 20.648（7）, b = 12.130（4）, c = 14.036（4） A, β = 106.351（5）°, C32H42N6O9Zn, Mr = 720.09, V = 3373.3（2） A3, Z= 4, Dc = 1.418 g/cm^3μt（MoKα） = 0.790 mm^-1, F（000） = 1512, the final R = 0.0407 and wR = 0.0894 for 3480 independent reflections with Rint = 0.0432. Crystal data for complex 2： monoclinic, space group C2/c, a = 21.332（6）, b = 12.063（3）, c = 14.246（4） A, β = 106.704（4）°, C32H40.50N6O8.25Cd, Mr = 753.60, V= 3511.2（2） A^3, Z = 4, Dc = 1.426 g/cm^3,μ（MoKα） = 0.679 mm^--1, F（000） = 1554, the final R = 0.0419 and wR = 0.0961 for 3627 independent reflections with Rint = 0.0440. The framework structures of complexes 1 and 2 are 3-D networks via the hydrogen bonds among 1-D chains. The notable characteristics of the two complexes are that the coordination polyhedron of Zn（Ⅱ） adopts a rare distorted five-coordinate square pyramidal geometry in 1, and the Cd（Ⅱ） complex exhibits an unusual distorted seven-coordinate pentagonal bipyramid in 2.

Engineering a high-barrier d-f single-molecule magnet centered with hexagonal bipyramidal Dy(Ⅲ)unit

In the pursuit of high-performance single-molecule magnets(SMMs),incorporating intramolecular magnetic coupling emerges as a pivotal strategy.Among these,d-f SMMs have garnered significant attention due to their remarkable versatility,which lies in their ability to tune coordination environments and facilely substitute metal centers.However,achieving performance-centric d-f SMMs through the synergistic interplay between highly anisotropic f ions and d-f magnetic interactions remains a formidable challenge.While mononuclear hexagonal bipyramidal(D_(6h))Dy^(Ⅲ)SMMs have been successfully isolated,the exploration of d-f SMMs featuring D_(6h)-lanthanide metal centers remains uncharted territory.In this study,we employed planar bipodal ligands in conjunction with“staple-like”axial phenoxide ligands to synthesize the first hexagonal bipyramidal d-f SMM.Remarkably,this compound exhibits alternating-current magnetic susceptibilities peaking up to 68 K with an energy barrier surpassing 1,200 K,thus establishing a new benchmark within the heterometallic d-f SMM landscape inclusive of complexes with diamagnetic d metals and paramagnetic f ions.Notably,the ferromagnetic interaction at the d-f sites engenders oscillating relaxation times contingent on the magnetic field—a characteristic distinct from mononuclear SMMs.These findings shed light on a deliberate design approach for d-f SMMs,emphasizing the cooperative utilization of high-barrier lanthanide modules alongside d ions through magnetic interactions.This synergy significantly enhances and diversifies the magnetic dynamics of these intriguing molecular systems.

Getting rid of NaBH4:Gold seeds reduced by air-stable agents for synthesizing quasi one-dimensional gold nanoparticles

Herein,we have presented a novel and easy to operate seed-mediated system for fabricating gold bipyramids(AuBPs)with 85%yields without any separation/purification processes.The used gold seeds are reduced by tannin and citrate,two kinds of air stable ligands,and conventio nally employed unstable NaBH4 are thoroughly cast off.In addition,the as-proposed gold seeds can also be employed for AuNRs fabrication with rather larger diameters(22.2-60.3 nm),which is difficult to be achieved by conve ntional seed mediated fabrication system.

Controllable synthesis of elongated hexagonal bipyramid shaped La(OH)3 nanorods and the distribution of electric property by off-axis electron holography

Rare earth oxides/hydroxides are important emerging materials owing to their unique properties. Shape-controlled synthesis of elongated hexagonal bipyramid shaped La(OH)3nanorods with different aspect ratios and trigram-shaped LaCO3OH nanosheets was systematically carried out by controlling the reaction conditions. Hydrazine and polyvinylpyrrolidone (PVP) surfactants used in synthesis are assumed to play a key “dual-template” role in determining the aspect ratio and shape of the resulting nanostructures. Elongated hexagonal bipyramid shaped La(OH)3nanorods were found to grow along the preferred orientation [0001]. Six equivalent crystallographic facets, (Formula presented.), and (Formula presented.) lattice planes, were found to be exposed on the side surfaces on each nanorod as confirmed by combined transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) analyses. A double-polarization phenomenon was found to occur at the nanorod surfaces by employing off-axis electron holography, implying that the material could be used as an effective dielectric microwave absorber. La(OH)3nanorods with larger aspect ratios exhibit better absorption properties with respect to the maximum reflection loss and effective absorbing bandwidth. Thus, a novel method towards the reasonable design of bipyramid shaped La(OH)3nanorods exhibiting tunable microwave absorption properties is proposed based on our synthesis strategy. [Figure not available: see fulltext.] © 2016, Tsinghua University Press and Springer-Verlag Berlin Heidelberg.