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1.
Use of amphiphilic triblock copolymers to direct the organization of polymerizing silica species has resulted in the preparation of well-ordered hexagonal mesoporous silica structures (SBA-15) with uniform pore sizes up to approximately 300 angstroms. The SBA-15 materials are synthesized in acidic media to produce highly ordered, two-dimensional hexagonal (space group p6mm) silica-block copolymer mesophases. Calcination at 500 degrees C gives porous structures with unusually large interlattice d spacings of 74.5 to 320 angstroms between the (100) planes, pore sizes from 46 to 300 angstroms, pore volume fractions up to 0.85, and silica wall thicknesses of 31 to 64 angstroms. SBA-15 can be readily prepared over a wide range of uniform pore sizes and pore wall thicknesses at low temperature (35 degrees to 80 degrees C), using a variety of poly(alkylene oxide) triblock copolymers and by the addition of cosolvent organic molecules. The block copolymer species can be recovered for reuse by solvent extraction with ethanol or removed by heating at 140 degrees C for 3 hours, in both cases, yielding a product that is thermally stable in boiling water.  相似文献   

2.
Hydrogen storage in microporous metal-organic frameworks   总被引：2，自引：0，他引：2  
Metal-organic framework-5 (MOF-5) of composition Zn4O(BDC)3 (BDC = 1,4-benzenedicarboxylate) with a cubic three-dimensional extended porous structure adsorbed hydrogen up to 4.5 weight percent (17.2 hydrogen molecules per formula unit) at 78 kelvin and 1.0 weight percent at room temperature and pressure of 20 bar. Inelastic neutron scattering spectroscopy of the rotational transitions of the adsorbed hydrogen molecules indicates the presence of two well-defined binding sites (termed I and II), which we associate with hydrogen binding to zinc and the BDC linker, respectively. Preliminary studies on topologically similar isoreticular metal-organic framework-6 and -8 (IRMOF-6 and -8) having cyclobutylbenzene and naphthalene linkers, respectively, gave approximately double and quadruple (2.0 weight percent) the uptake found for MOF-5 at room temperature and 10 bar.  相似文献   

3.
Interpenetration (catenation) has long been considered a major impediment in the achievement of stable and porous crystalline structures. A strategy for the design of highly porous and structurally stable networks makes use of metal-organic building blocks that can be assembled on a triply periodic P-minimal geometric surface to produce structures that are interpenetrating-more accurately considered as interwoven. We used 4,4',4"-benzene-1,3,5-triyl-tribenzoic acid (H(3)BTB), copper(II) nitrate, and N,N'-dimethylformamide (DMF) to prepare Cu(3)(BTB)(2)(H(2)O)(3).(DMF)(9)(H(2)O)(2) (MOF-14), whose structure reveals a pair of interwoven metal-organic frameworks that are mutually reinforced. The structure contains remarkably large pores, 16.4 angstroms in diameter, in which voluminous amounts of gases and organic solvents can be reversibly sorbed.  相似文献   

4.
The molecular sieve MCM-22 contains structural features previously unobserved in this class of materials. Its framework topology, derived from high-resolution electron micrographs and refined with synchrotron x-ray diffraction powder data, contains two independent pore systems, both of which are accessed through rings composed of ten tetrahedral (T) atoms (such as Si, Al, and B). One of these pore systems is defined by two-dimensional, sinusoidal channels. The other consists of large supercages whose inner free diameter, 7.1 angstroms, is defined by 12 T-O species (12-rings) and whose inner height is 18.2 angstroms. These coexisting pore systems may provide opportunities for a wide variety of catalytic applications in the petrochemical and refining industries. Another structural feature is an unusual -T-O-T- chain that passes through the center of a modified dodecasil-1H [4(3)5(6)6(3)] cage.  相似文献   

5.
ZSM-18 is the first known aluminosilicate zeolite to contain rings of three (Si,Al)-O species (3-rings). Its framework topology has been determined by hypothetical model building, subsequent constrained distance and angle least-squares refinements of atomic coordinates, and x-ray powder diffraction pattern simulations. Its channel structure is characterized by a linear unidimensional 12-ring channel, with an approximate pore opening of 7.0 angstroms. In addition, the channels are lined with pockets that are capped by 7-rings with dimensions of 2.8 angstroms by 3.5 angstroms. An intraframework packing model of the organic moiety used in the synthesis suggests that a strong templating effect may be responsible for the formation of this unusual zeolite structure.  相似文献   

6.
The hindrance effect on the aqueous diffusion rate of solutes within membrane pores of molecular size has been accurately determined. Mica membranes, 3 to 5 micrometers thick, were prepared with uniform, straight pores from 90 to 600 angstroms in diameter. With these membranes a direct estimation was possible of the interaction between pore size and molecular diffusion rates. There were no uncertainties due to wide pore size distributions or nonuniform tortuous channels as in previously used model microporous materials such as dialysis tubing or gels. Aqueous diffusion rates through these mica membranes were measured for a series of compounds with molecular diameters from 5.2 to 43 angstroms and were corrected for "liquid film resistances" adjacent to the membrane-solution interface to obtain estimates of molecular diffusivities within the micropores of the membrane. Definite evidence is presented showing that, even when molecular size is a small fraction of pore size, diffusion rates decrease markedly. The apparent reduction in solute diffusivity in the microporous membrane can be quantitatively estimated by means of the Renkin equation for hindered diffusion.  相似文献   

7.
TRAAK channels, members of the two-pore domain K(+) (potassium ion) channel family K2P, are expressed almost exclusively in the nervous system and control the resting membrane potential. Their gating is sensitive to polyunsaturated fatty acids, mechanical deformation of the membrane, and temperature changes. Physiologically, these channels appear to control the noxious input threshold for temperature and pressure sensitivity in dorsal root ganglia neurons. We present the crystal structure of human TRAAK at a resolution of 3.8 angstroms. The channel comprises two protomers, each containing two distinct pore domains, which create a two-fold symmetric K(+) channel. The extracellular surface features a helical cap, 35 angstroms tall, that creates a bifurcated pore entryway and accounts for the insensitivity of two-pore domain K(+) channels to inhibitory toxins. Two diagonally opposed gate-forming inner helices form membrane-interacting structures that may underlie this channel's sensitivity to chemical and mechanical properties of the cell membrane.  相似文献   

8.
In classical enzymology, intermediates and transition states in a catalytic mechanism are usually inferred from a series of biochemical experiments. Here, we derive an enzyme mechanism from true atomic-resolution x-ray structures of reaction intermediates. Two ultra-high resolution structures of wild-type and mutant d-2-deoxyribose-5-phosphate (DRP) aldolase complexes with DRP at 1.05 and 1.10 angstroms unambiguously identify the postulated covalent carbinolamine and Schiff base intermediates in the aldolase mechanism. In combination with site-directed mutagenesis and (1)H nuclear magnetic resonance, we can now propose how the heretofore elusive C-2 proton abstraction step and the overall stereochemical course are accomplished. A proton relay system appears to activate a conserved active-site water that functions as the critical mediator for proton transfer.  相似文献   

9.
X-ray diffraction shows that chondroitin 6-sulfate, and some further rulfated derivatives, can occur in two ordered structures in stretched films. Both structures contain single helices with similar projected disaccharide lengths (9.6 and 9.8 angstroms) but with very different turn angles between successive disaccharides (120 and 45 degrees). In contrast, coaxial double helices of hyaluronates and t-carrageenates have shorter projected disaccharide lengths (8.5 and 8.9 angstroms).  相似文献   

10.
We combined targeted chemistry and computational design to create a crystal structure for porous chromium terephthalate, MIL-101, with very large pore sizes and surface area. Its zeotype cubic structure has a giant cell volume (approximately 702,000 cubic angstroms), a hierarchy of extra-large pore sizes (approximately 30 to 34 angstroms), and a Langmuir surface area for N2 of approximately 5900 +/- 300 square meters per gram. Beside the usual properties of porous compounds, this solid has potential as a nanomold for monodisperse nanomaterials, as illustrated here by the incorporation of Keggin polyanions within the cages.  相似文献   

11.
An x-ray surface forces apparatus for simultaneously measuring forces and structures of confined complex fluids under static and flow conditions is described. This apparatus, combined with an intense synchrotron x-ray source, allows investigation of molecular orientations within a thin liquid crystal film confined between two shearing mica surfaces 3900 angstroms apart. The layer-forming smectic liquid crystal 8CB (4-cyano-4'-octylbiphenyl) adopted a series of distinct planar layer orientations, including the bulk flow-forbidden b orientation.  相似文献   

12.
Covalent organic frameworks (COFs) have been designed and successfully synthesized by condensation reactions of phenyl diboronic acid {C6H4[B(OH)2]2} and hexahydroxytriphenylene [C18H6(OH)6]. Powder x-ray diffraction studies of the highly crystalline products (C3H2BO)6.(C9H12)1 (COF-1) and C9H4BO2 (COF-5) revealed expanded porous graphitic layers that are either staggered (COF-1, P6(3)/mmc) or eclipsed (COF-5, P6/mmm). Their crystal structures are entirely held by strong bonds between B, C, and O atoms to form rigid porous architectures with pore sizes ranging from 7 to 27 angstroms. COF-1 and COF-5 exhibit high thermal stability (to temperatures up to 500 degrees to 600 degrees C), permanent porosity, and high surface areas (711 and 1590 square meters per gram, respectively).  相似文献   

13.
Electron microscopy of purified Waldenstr?m macroglobulins and normal human and rabbit gammaM immunoglobulins revealed spider-like structures with five legs varying in length and often joining a central ring. Usually only the central more rigid part of this structure (about 150 by 170 angstroms) was clearly visible, but occasionally particles were seen with longer very flexible legs having a total span of about 350 angstroms. Molecules of gammaM antibody retained antibody activity during preparation for electron microscopy. Human and rabbit alpha macroglobulins revealed more rigid symmetric structures (100 by 200 angstroms) which resembled the Russian letter .  相似文献   

14.
Material structures of reduced dimensions exhibit electrical and mechanical properties different from those in the bulk. Measurements of room-temperature electronic transport in pulled metallic nanowires are presented, demonstrating that the conductance characteristics depend on the length, lateral dimensions, state and degree of disorder, and elongation mechanism of the wire. Conductance during the elongation of short wires (length l approximately 50 angstroms) exhibits periodic quantization steps with characteristic dips, correlating with the order-disorder states of layers of atoms in the wire predicted by molecular dynamics simulations. The resistance R of wires as long as l approximately 400 angstroms exhibits localization characteristics with In R(l) approximately l(2).  相似文献   

15.
A high-resolution crystallographic analysis of the nitrogenase MoFe-protein reveals a previously unrecognized ligand coordinated to six iron atoms in the center of the catalytically essential FeMo-cofactor. The electron density for this ligand is masked in structures with resolutions lower than 1.55 angstroms, owing to Fourier series termination ripples from the surrounding iron and sulfur atoms in the cofactor. The central atom completes an approximate tetrahedral coordination for the six iron atoms, instead of the trigonal coordination proposed on the basis of lower resolution structures. The crystallographic refinement at 1.16 angstrom resolution is consistent with this newly detected component being a light element, most plausibly nitrogen. The presence of a nitrogen atom in the cofactor would have important implications for the mechanism of dinitrogen reduction by nitrogenase.  相似文献   

16.
Emissions of atomic oxygen (1304 angstroms), atomic carbon (1657 angstroms), and atomic hydrogen (1216 angstroms) from Comet Kohoutek were observed with ultraviolet cameras carried on a sounding rocket on 8 January 1974. Analysis of the Lyman alpha halo at 1216 angstroms gave an atomic hydrogen production rate of 4.5 x 10(29) atoms per second.  相似文献   

17.
Electron micrographs of immunoglobulins A from human and rabbit colostrum, which were purified on tall agarose columns, revealed Y-shaped molecules (125 by 140 angstroms). The linear dimensions of the arms were 55 to 75 by 25 to 30 angstroms. A molecular model is postulated in which two immunoglobulin A monomers are superimposed on each other in a close-packed state with the secretory piece inserted in the constant region of the alpha-chains. High-polymer (11 or 13S) immunoglobulin A molecules (total span 100 to 110 angstroms) from human serum were composed of four arms (50 to 55 by 20 angstroms) joined at a contrast-rich center.  相似文献   

18.
Thin sections (500 to 1000 angstroms thick) of individual micrometeorites (5 to 15 micrometers) have been prepared with an ultramicrotome equipped with a diamond knife. Electron microscopic examination of these sections has revealed the internal structures of chondritic micrometeorites, and a subset of highly porous, fragile particles has been identified. Delicate meteoritic materials such as these are characteristic of debris from cometary meteors.  相似文献   

19.
Molecular structure of DNA by scanning tunneling microscopy   总被引：5，自引：0，他引：5  
Uncoated DNA molecules marked with an activated tris(l-aziridinyl) phosphine oxide (TAPO) solution were deposited on gold substrates and imaged in air with the use of a high-resolution scanning tunneling microscope (STM). Constant-current and gap-modulated STM images show clear evidence of the helicity of the DNA structure: pitch periodicity ranges from 25 to 35 angstroms, whereas the average diameter is 20 angstroms. Molecular structure within a single helix turn was also observed.  相似文献   

20.
Calibrated membranes with coated pore walls   总被引：1，自引：0，他引：1  
Extremely uniform small-radius pores, formed in thin mica membranes, have been coated with monoand multimolecular layers of fatty acids. Stearate monolayers orient themselves on the pore walls in layers 25 to 28 angstroms thick. The resulting membranes, with radii of the order 100 angstroms or less, may have applications in simulating certain features of biological membranes and in fabricating highly selective membranes for differential dialysis or ultrafiltration.  相似文献   

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