Two New Three-Dimensional Networks Constructed on Polyoxovanadates

2007 ◽  
Vol 60 (11) ◽  
pp. 871 ◽  
Author(s):  
Yan-fei Qi ◽  
Dongrong Xiao ◽  
Enbo Wang ◽  
Zhiming Zhang ◽  
Xinlong Wang
Keyword(s):  
Thermogravimetric Analysis ◽  
Rare Case ◽  
Three Dimensional ◽  
Network Connectivity ◽  
Two Dimensional ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray

To investigate the role of polyoxovanadates in network connectivity, two new organic–inorganic hybrid vanadates with three-dimensional entangled coordination frameworks, namely [Cu2(biim)3V4O12] 1 and [Co2(biim)3V4O12]·4H2O 2 have been synthesized and characterized by infrared (IR), thermogravimetric analysis (TGA), and single-crystal X-ray diffraction. Crystal data for compound 1: triclinic, P-1, a 9.504(2), b 10.650(2), c 11.993(2) Å; α 72.13(3), β 76.02(3), γ 65.40(3)°; V 1041.4(4) Å3, Z 2, R(final) 0.0492. Crystal data for compound 2: triclinic, P-1, a 9.037(3), b 10.577(2), c 11.9470(2) Å; α 87.80(3), β 81.71(3), γ 85.29(3)°; V 1125.8(4) Å3, Z 1, R(final) 0.0774. Compound 1 is a three-dimensional inclined hetero-catenated framework designed from two two-dimensional sub-layers, [Cu(biim)V4O12] and [Cu(biim)2]. Compound 2 is a rare case of a self-catenated ‘ilc’ network that displays an unusual 424·5·63 topology with the binuclear {Co2O4N6} units as eight-connected nodes.

Two Nickel-Bipyridinedicarboxylate Organic-Inorganic Hybrid Materials: Hydrothermal Synthesis, Crystal Structure and Thermal Properties

2010 ◽  
Vol 152-153 ◽  
pp. 144-148
Author(s):  
Yan Xia Song ◽  
Chong Chen Wang ◽  
Yuan Lan Wang
Keyword(s):  
Thermogravimetric Analysis ◽  
Dicarboxylic Acid ◽  
Hydrothermal Reaction ◽  
Three Dimensional ◽  
Tridentate Ligand ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Two two-dimensional and three-dimensional coordination-polymer, [Ni(2,2′,5,5′-bpdc) (H2O)]•H2O (1) and[Ni(2,2′,6,6′-bpdc)2]•4H2O (2) were obtained via hydrothermal reaction between NiCl2•6H2O and 2,2′-bipyridine-5,5′-dicarboxylic acid (2,2′,5,5′-bpdc), 2,2′-bipyridine-6,6′-dicarboxylic acid (2,2′,6,6′-bpdc) respectively, and were characterized by infrared spectra, thermogravimetric analysis and single crystal X-ray diffraction. The 2,2′,5,5′-bpdc and 2,2′,6,6′-bpdc ligands in compound 1 and 2 show different coordination modes respectively. The 2,2′,5,5′-bpdc ligand acts as pentadentate connector to coordinate with three different Ni(II) ions, and further extend to form square grid framework of compound 1; while 2,2′,6,6′-bpdc acts as tridentate ligand to chelate one Ni(II) ion to construct discrete monomeric unit, and those discrete units of [Ni(2,2′6,6′-bpdc)2]•4H2O are joined into 3-D framework via rich hydrogen bonding interactions. Thermogravimetric analysis revealed that both complex (1) and (2) display considerable thermal stability. CCDC 773845 & 773846.

Synthesis and Structural Characterization of a New Two-dimensional Organic-Inorganic Hybrid Molybdoarsenate: [Cu(en)2]2[(CuO6)Mo6O18(As3O3)2]

2010 ◽  
Vol 65 (2) ◽  
pp. 163-167 ◽  
Author(s):  
Qiang Wu ◽  
Qiuxia Han ◽  
Lijun Chen ◽  
Pengtao Ma ◽  
Jingyang Niu
Keyword(s):  
Thermogravimetric Analysis ◽  
Building Blocks ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
2D Network

A new organic-inorganic hybrid molybdoarsenate constructed from a unit with two (As3O3) rings capping Anderson-type moieties, [Cu(en)2]2[(CuO6)Mo6O18(As3O3)2] (1) (en = ethylenediamine), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction and thermogravimetric analysis. The compound crystallizes monoclinically, space group P21/c, with unit cell dimensions a = 9.1541(7), b = 19.6348(14), c = 14.5205(8) Å ,β = 129.082(3)◦,V = 364.20(4) Å3, Z = 2, T = 296(2) K. Complex 1 represents the first example of a 2D network of a POM polymer where [(CuO6)Mo6O18(As3O3)2]4− building blocks are connected by complex fragments {Cu(en)2}2+.

scholarly journals Intermetallic REPtZn Compounds with TiNiSi-type Structure

2011 ◽  
Vol 66 (7) ◽  
pp. 671-676 ◽  
Author(s):  
Trinath Mishra ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Coordination Number ◽  
High Frequency ◽  
Three Dimensional ◽  
Type Structure ◽  
Rare Earth Compounds ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray

The equiatomic rare earth compounds REPtZn (RE = Y, Pr, Nd, Gd-Tm) were synthesized from the elements in sealed tantalum tubes by high-frequency melting at 1500 K followed by annealing at 1120 K and quenching. The samples were characterized by powder X-ray diffraction. The structures of four crystals were refined from single-crystal diffractometer data: TiNiSi type, Pnma, a = 707.1(1), b = 430.0(1), c = 812.4(1) pm, wR2 = 0.066, 602 F2, 21 variables for PrPt1.056Zn0.944; a = 695.2(1), b = 419.9(1), c = 804.8(1) pm, wR2 = 0.041, 522 F2, 21 variables for GdPt0.941Zn1.059; a = 688.2(1), b = 408.1(1), c = 812.5(1) pm, wR2 = 0.041, 497 F2, 22 variables for HoPt1.055Zn0.945; a = 686.9(1), b = 407.8(1), c = 810.4(1) pm, wR2 = 0.061, 779 F2, 20 variables for ErPtZn. The single-crystal data indicate small homogeneity ranges REPt1±xZn1±x. The platinum and zinc atoms build up three-dimensional [PtZn] networks (265 - 269 pm Pt-Zn in ErPtZn) in which the erbium atoms fill cages with coordination number 16 (6 Pt + 6 Zn + 4 Er). Bonding of the erbium atoms to the [PtZn] network proceeds via shorter RE-Pt distances, i. e. 288 - 293 pm in ErPtZn.

scholarly journals Low-Zpolymer sample supports for fixed-target serial femtosecond X-ray crystallography

2015 ◽  
Vol 48 (4) ◽  
pp. 1072-1079 ◽  
Author(s):  
Geoffrey K. Feld ◽  
Michael Heymann ◽  
W. Henry Benner ◽  
Tommaso Pardini ◽  
Ching-Ju Tsai ◽  
...  
Keyword(s):  
Protective Antigen ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Fixed Target ◽  
X Ray ◽  
X Ray Crystallography ◽  
Transmission Electron ◽  
Linac Coherent Light Source ◽  
Efficient Alternative

X-ray free-electron lasers (XFELs) offer a new avenue to the structural probing of complex materials, including biomolecules. Delivery of precious sample to the XFEL beam is a key consideration, as the sample of interest must be serially replaced after each destructive pulse. The fixed-target approach to sample delivery involves depositing samples on a thin-film support and subsequent serial introductionviaa translating stage. Some classes of biological materials, including two-dimensional protein crystals, must be introduced on fixed-target supports, as they require a flat surface to prevent sample wrinkling. A series of wafer and transmission electron microscopy (TEM)-style grid supports constructed of low-Zplastic have been custom-designed and produced. Aluminium TEM grid holders were engineered, capable of delivering up to 20 different conventional or plastic TEM grids using fixed-target stages available at the Linac Coherent Light Source (LCLS). As proof-of-principle, X-ray diffraction has been demonstrated from two-dimensional crystals of bacteriorhodopsin and three-dimensional crystals of anthrax toxin protective antigen mounted on these supports at the LCLS. The benefits and limitations of these low-Zfixed-target supports are discussed; it is the authors' belief that they represent a viable and efficient alternative to previously reported fixed-target supports for conducting diffraction studies with XFELs.

scholarly journals The three-dimensional structure of a class-Pi glutathione S-transferase complexed with glutathione: the active-site hydration provides insights into the reaction mechanism

1998 ◽  
Vol 333 (3) ◽  
pp. 811-816 ◽  
Author(s):  
Antonio PÁRRAGA ◽  
Isabel GARCÍA-SÁEZ ◽  
Sinead B. WALSH ◽  
Timothy J. MANTLE ◽  
Miquel COLL
Keyword(s):  
Conformational Changes ◽  
Active Site ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Glutathione S Transferase ◽  
X Ray ◽  
The Right

The structure of mouse liver glutathione S-transferase P1-1 complexed with its substrate glutathione (GSH) has been determined by X-ray diffraction analysis. No conformational changes in the glutathione moiety or in the protein, other than small adjustments of some side chains, are observed when compared with glutathione adduct complexes. Our structure confirms that the role of Tyr-7 is to stabilize the thiolate by hydrogen bonding and to position it in the right orientation. A comparison of the enzyme–GSH structure reported here with previously described structures reveals rearrangements in a well-defined network of water molecules in the active site. One of these water molecules (W0), identified in the unliganded enzyme (carboxymethylated at Cys-47), is displaced by the binding of GSH, and a further water molecule (W4) is displaced following the binding of the electrophilic substrate and the formation of the glutathione conjugate. The possibility that one of these water molecules participates in the proton abstraction from the glutathione thiol is discussed.

Two new CdII MOFs of 1,4-bis(1H-benzimidazol-1-yl)butane and flexible dicarboxylate ligands: luminescence sensing towards Fe3+

2020 ◽  
Vol 76 (11) ◽  
pp. 1024-1033
Author(s):  
Fang-Hua Zhao ◽  
Shi-Yao Li ◽  
Wen-Yu Guo ◽  
Zi-Hao Zhao ◽  
Xiao-Wen Guo ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Layer Structure ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy

Two new CdII MOFs, namely, two-dimensional (2D) poly[[[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ2-heptanedioato)cadmium(II)] tetrahydrate], {[Cd(C7H10O4)(C18H18N4)]·4H2O} n or {[Cd(Pim)(bbimb)]·4H2O} n (1), and 2D poly[diaqua[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ4-decanedioato)(μ2-decanedioato)dicadmium(II)], [Cd2(C10H16O4)2(C18H18N4)(H2O)2] n or [Cd(Seb)(bbimb)0.5(H2O)] n (2), have been synthesized hydrothermally based on the 1,4-bis(1H-benzimidazol-1-yl)butane (bbimb) and pimelate (Pim2−, heptanedioate) or sebacate (Seb2−, decanedioate) ligands. Both MOFs were structurally characterized by single-crystal X-ray diffraction. In 1, the CdII centres are connected by bbimb and Pim2− ligands to generate a 2D sql layer structure with an octameric (H2O)8 water cluster. The 2D layers are further connected by O—H...O hydrogen bonds, resulting in a three-dimensional (3D) supramolecular structure. In 2, the CdII centres are coordinated by Seb2− ligands to form binuclear Cd2 units which are linked by bbimb and Seb2− ligands into a 2D hxl layer. The 2D layers are further connected by O—H...O hydrogen bonds, leading to an 8-connected 3D hex supramolecular network. IR and UV–Vis spectroscopy, thermogravimetric analysis and solid-state photoluminescence analysis were carried out on both MOFs. Luminescence sensing experiments reveal that both MOFs have good selective sensing towards Fe3+ in aqueous solution.

Two novel organic–inorganic hybrid materials from tetrachloridometallate(II) salts and 4-[(E)-2-(pyridin-1-ium-2-yl)ethenyl]pyridinium

2015 ◽  
Vol 71 (1) ◽  
pp. 48-52 ◽  
Author(s):  
José J. Campos-Gaxiola ◽  
Susana P. Arredondo Rea ◽  
Ramón Corral Higuera ◽  
Herbert Höpfl ◽  
Adriana Cruz Enríquez
Keyword(s):  
Three Dimensional ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Pyridinium Cation ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Two organic–inorganic hybrid compounds have been prepared by the combination of the 4-[(E)-2-(pyridin-1-ium-2-yl)ethenyl]pyridinium cation with perhalometallate anions to give 4-[(E)-2-(pyridin-1-ium-2-yl)ethenyl]pyridinium tetrachloridocobaltate(II), (C12H12N2)[CoCl4], (I), and 4-[(E)-2-(pyridin-1-ium-2-yl)ethenyl]pyridinium tetrachloridozincate(II), (C12H12N2)[ZnCl4], (II). The compounds have been structurally characterized by single-crystal X-ray diffraction analysis, showing the formation of a three-dimensional network throughX—H...ClnM−(X= C, N+;n= 1, 2;M= CoII, ZnII) hydrogen-bonding interactions and π–π stacking interactions. The title compounds were also characterized by FT–IR spectroscopy and thermogravimetric analysis (TGA).

Synthesis, Structure and Characterization of a Novel Two-Dimensional Supramolecular Mn(II) Coordination Polymer Constructed from a 1,10-Phenanthroline Derivative and a Flexible Dicarboxylate

2010 ◽  
Vol 65 (9) ◽  
pp. 1173-1176 ◽  
Author(s):  
Zhi-Guo Kong ◽  
Xiao-Yuan Ma ◽  
Zhan-Lin Xu
Keyword(s):  
Ir Spectroscopy ◽  
Glutaric Acid ◽  
Title Complex ◽  
Two Dimensional ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
1D Chains

The title complex, [Mn2(glu)(L)2(HL)2]・0.5H2O (H2glu = glutaric acid, HL = 2-(2-chloro-6-fluorophenyl)-1Himidazo[ 4,5-f][1,10]phenanthroline) has been synthesized using a hydrothermal method and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal data: C162H88Cl8F8Mn4N32O9, triclinic, space group P1¯, a = 14.932(5), b = 16.414(5), c = 17.891(5) Å , α = 115.851(5), β = 91.288(5), γ = 112.894(5)◦, V = 3536.4(19) Å3, Z = 1. Compound 1 exhibits 1D chains which are further stacked by C-H...π interactions to give two-dimensional supramolecular layers.

High Resolution Synchrotron X-Ray Diffraction Tomography Of Large-Grained Samples

1996 ◽  
Vol 437 ◽  
Author(s):  
D.P. Piotrowski ◽  
S.R. Stock ◽  
A. Guvenilir ◽  
J.D. Haase ◽  
Z.U. Rek
Keyword(s):  
Spatial Distribution ◽  
High Resolution ◽  
Three Dimensional ◽  
Polycrystalline Materials ◽  
Diffraction Tomography ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Image Storage ◽  
X Ray ◽  
Dimensional Distribution

AbstractIn order to understand the macroscopic response of polycrystalline structural materials to loading, it is frequently essential to know the spatial distribution of strain as well as the variation of micro-texture on the scale of 100 μm. The methods must be nondestructive, however, if the three-dimensional evolution of strain is to be studied. This paper describes an approach to high resolution synchrotron x-ray diffraction tomography of polycrystalline materials. Results from model samples of randomly-packed, millimeter-sized pieces of Si wafers and of similarly sized single-crystal Al blocks have been obtained which indicate that polychromatic beams collimated to 30 μm diameter can be used to determine the depth of diffracting volume elements within ± 70 μm. The variation in the two-dimensional distribution of diffracted intensity with changing sample to detector separation is recorded on image storage plates and used to infer the depth of diffracting volume elements.

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