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Publications

Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

Cornell Affiliated Author(s)
Author
M. Heymann
A. Opthalage
J.L. Wierman
S. Akella
D.M.E. Szebenyi
Sol Gruner
S. Fraden
Abstract

An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop.

Journal
IUCrJ
Date Published
Research Area
Group (Lab)
Sol M. Gruner Group

Time-resolved x-ray diffraction techniques for bulk polycrystalline materials under dynamic loading

Cornell Affiliated Author(s)
Author
P.K. Lambert
C.J. Hustedt
K.S. Vecchio
E.L. Huskins
D.T. Casem
Sol Gruner
M.W. Tate
H.T. Philipp
A.R. Woll
P. Purohit
J.T. Weiss
V. Kannan
K.T. Ramesh
P. Kenesei
J.S. Okasinski
J. Almer
M. Zhao
A.G. Ananiadis
T.C. Hufnagel
Abstract

We have developed two techniques for time-resolved x-ray diffraction from bulk polycrystalline materials during dynamic loading. In the first technique, we synchronize a fast detector with loading of samples at strain rates of ∼103-104 s-1 in a compression Kolsky bar (split Hopkinson pressure bar) apparatus to obtain in situ diffraction patterns with exposures as short as 70 ns. This approach employs moderate x-ray energies (10-20 keV) and is well suited to weakly absorbing materials such as magnesium alloys.

Journal
Review of Scientific Instruments
Date Published
Funding Source
DMR-0936384
DE-FG02-10ER46693
Group (Lab)
Sol M. Gruner Group

Monolithic gyroidal mesoporous mixed titanium-niobium nitrides

Cornell Affiliated Author(s)
Author
S.W. Robbins
H. Sai
F.J. DiSalvo
Sol Gruner
U. Wiesner
Abstract

Mesoporous transition metal nitrides are interesting materials for energy conversion and storage applications due to their conductivity and durability. We present ordered mixed titanium-niobium (8:2, 1:1) nitrides with gyroidal network structures synthesized from triblock terpolymer structure-directed mixed oxides. The materials retain both macroscopic integrity and mesoscale ordering despite heat treatment up to 600 °C, without a rigid carbon framework as a support. Furthermore, the gyroidal lattice parameters were varied by changing polymer molar mass.

Journal
ACS Nano
Date Published
Research Area
Group (Lab)
Sol M. Gruner Group

Ordered nanostructured ceramic-metal composites through multifunctional block copolymer-metal nanoparticle self-assembly

Cornell Affiliated Author(s)
Author
Z. Li
H. Sai
K.W. Tan
T.N. Hoheisel
Sol Gruner
U. Wiesner
Abstract

A novel strategy for fabrication of ordered ceramic-metal nanocomposites was demonstrated by multifunctional block copolymer/metal nanoparticle self-assembly. Hybrid organic-inorganic block copolymer poly(3- methacryloxypropyl-T8-heptaisobutyl-polyhedral oligomeric silsesquioxane-block- N,N-dimethylaminoethyl methacrylate) was synthesized and used as a bi-functional structure directing agent for ligand-stabilized platinum nanoparticles to form ordered organic-inorganic nanocomposites with dense loading of inorganic species in both microphase separated domains.

Journal
Journal of Sol-Gel Science and Technology
Date Published
Funding Source
DMR-0225180
1104773
DMR-1104773
DMR-0936384
DMR-1120296
Group (Lab)
Sol M. Gruner Group

Linking experiment and theory for three-dimensional networked binary metal nanoparticle-triblock terpolymer superstructures

Cornell Affiliated Author(s)
Author
Z. Li
K. Hur
H. Sai
T. Higuchi
A. Takahara
H. Jinnai
Sol Gruner
U. Wiesner
Abstract

Controlling superstructure of binary nanoparticle mixtures in three dimensions from self-assembly opens enormous opportunities for the design of materials with unique properties. Here we report on how the intimate coupling of synthesis, in-depth electron tomographic characterization and theory enables exquisite control of superstructure in highly ordered porous three-dimensional continuous networks from single and binary mixtures of metal nanoparticles with a triblock terpolymer.

Journal
Nature Communications
Date Published
Group (Lab)
Sol M. Gruner Group

Real-Space x-ray tomographic reconstruction of randomly oriented objects with sparse data frames

Cornell Affiliated Author(s)
Author
K. Ayyer
H.T. Philipp
M.W. Tate
V. Elser
Sol Gruner
Abstract

Schemes for X-ray imaging single protein molecules using new x-ray sources, like x-ray free electron lasers (XFELs), require processing many frames of data that are obtained by taking temporally short snapshots of identical molecules, each with a random and unknown orientation. Due to the small size of the molecules and short exposure times, average signal levels of much less than 1 photon/pixel/frame are expected, much too low to be processed using standard methods. One approach to process the data is to use statistical methods developed in the EMC algorithm (Loh & Elser, Phys. Rev.

Journal
Optics Express
Date Published
Group (Lab)
Sol M. Gruner Group
Veit Elser Group

Graphene as a protein crystal mounting material to reduce background scatter

Cornell Affiliated Author(s)
Author
J.L. Wierman
J.S. Alden
C.U. Kim
P.L. McEuen
Sol Gruner
Abstract

The overall signal-to-noise ratio per unit dose for X-ray diffraction data from protein crystals can be improved by reducing the mass and density of all material surrounding the crystals. This article demonstrates a path towards the practical ultimate in background reduction by use of atomically thin graphene sheets as a crystal mounting platform for protein crystals.

Journal
Journal of Applied Crystallography
Date Published
Group (Lab)
Paul McEuen Group
Sol M. Gruner Group

Structure of a pseudokinase-domain switch that controls oncogenic activation of Jak kinases

Cornell Affiliated Author(s)
Author
A.V. Toms
A. Deshpande
R. McNally
Y. Jeong
J.M. Rogers
C.U. Kim
Sol Gruner
S.B. Ficarro
J.A. Marto
M. Sattler
J.D. Griffin
M.J. Eck
Abstract

The V617F mutation in the Jak2 pseudokinase domain causes myeloproliferative neoplasms, and the equivalent mutation in Jak1 (V658F) is found in T-cell leukemias. Crystal structures of wild-type and V658F-mutant human Jak1 pseudokinase reveal a conformational switch that remodels a linker segment encoded by exon 12, which is also a site of mutations in Jak2. This switch is required for V617F-mediated Jak2 activation and possibly for physiologic Jak activation. © 2013 Nature America, Inc. All rights reserved.

Journal
Nature Structural and Molecular Biology
Date Published
Funding Source
CA936132
GM008313
R01CA134660
Group (Lab)
Sol M. Gruner Group

Hierarchical porous polymer scaffolds from block copolymers

Cornell Affiliated Author(s)
Author
H. Sai
K.W. Tan
K. Hur
E. Asenath-Smith
R. Hovden
Y. Jiang
M. Riccio
D.A. Muller
V. Elser
L.A. Estroff
Sol Gruner
U. Wiesner
Abstract

Hierarchical porous polymer materials are of increasing importance because of their potential application in catalysis, separation technology, or bioengineering. Examples for their synthesis exist, but there is a need for a facile yet versatile conceptual approach to such hierarchical scaffolds and quantitative characterization of their nonperiodic pore systems.

Journal
Science
Date Published
Research Area
Group (Lab)
Sol M. Gruner Group
Veit Elser Group

A prototype direct-detection CCD for protein crystallography

Cornell Affiliated Author(s)
Author
K.S. Green
D.M.E. Szebenyi
K. Boggs
R. Bredthauer
M.W. Tate
Sol Gruner
Abstract

The fabrication and testing of a prototype deep-depletion direct-conversion X-ray CCD detector are described. The device is fabricated on 600 μm-thick high-resistivity silicon, with 24 × 24 μm pixels in a 4k × 4k pixel format. Calibration measurements and the results of initial protein crystallography experiments at the Cornell High Energy Synchrotron Source (CHESS) F1 beamline are described, as well as suggested improvements for future versions of the detector. © 2013 International Union of Crystallography Printed in Singapore - all rights reserved.

Journal
Journal of Applied Crystallography
Date Published
Research Area
Group (Lab)
Sol M. Gruner Group