Crystal structure determination of the silver carboxylate dimer [Ag(O2C22H43)]2, silver behenate, using powder X-ray diffraction methods

2011 ◽  
Vol 26 (4) ◽  
pp. 313-320 ◽  
Author(s):  
Thomas N. Blanton ◽  
Manju Rajeswaran ◽  
Peter W. Stephens ◽  
David R. Whitcomb ◽  
Scott T. Misture ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Density Functional ◽  
Structural Model ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Alkyl Side Chains ◽  
Silver Carboxylate

High-resolution powder X-ray diffraction has been used to determine the crystal structure of silver behenate, [Ag(O2C(CH2)20CH3]2. Using CASTEP density functional plane wave pseudopotential techniques to obtain an optimized structural model, Rietveld refinement of the structure gives Rwp = 8.66%. The unit cell is triclinic, space group P1, with cell dimensions of a = 4.1769(2) Å, b = 4.7218(2) Å, c = 58.3385(1) Å, α = 89.440(3)°, β = 89.634(3)°, γ = 75.854(1)°. The structure is characterized by an 8-membered ring dimer of Ag atoms and carboxyl groups with a fully extended all-trans configuration of the alkyl side chains. The dimers are joined by four-membered Ag-O rings creating a polymeric network, giving rise to one-dimensional chains along the b-axis. This structure is supported by EXAFS measurements of the local structure around the silver atoms and IR measurements.

Structure determination of the silver carboxylate dimer [Ag(O2C20H39)]2, silver arachidate, using powder X-ray diffraction methods

2012 ◽  
Vol 27 (2) ◽  
pp. 99-103 ◽  
Author(s):  
Peter W. Stephens ◽  
James A. Kaduk ◽  
Thomas N. Blanton ◽  
David R. Whitcomb ◽  
Scott T. Misture ◽  
...  
Keyword(s):  
Density Functional ◽  
Structural Model ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Cell Dimensions ◽  
Silver Carboxylate ◽  
Pseudo Potential

High-resolution powder X-ray diffraction and density functional plane wave pseudo-potential techniques have been used to obtain an optimized structural model of silver arachidate, [Ag(O2C(CH2)18CH3]2. The unit cell is triclinic, space group P-1 with cell dimensions of a = 4.1519(10) Å, b = 4.7055(10) Å, c = 53.555(4) Å, α = 89.473(15)°, β = 87.617(5)° and γ = 76.329(5)°. The structure is characterized by an 8-membered ring dimer of Ag atoms and carboxyl groups joined by four-member Ag–O rings with fully extended zigzag side chains, giving rise to one-dimensional chains along the b-axis.

Cluster Chemistry. XLVII. X-Ray Crystal Structure of OsPt2(μ-CO)3(CO)2(PPh3)3

1986 ◽  
Vol 39 (12) ◽  
pp. 2145 ◽  
Author(s):  
MI Bruce ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
Metal Metal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Triphenylphosphine Ligand

The crystal structure of OsPt2(μ-CO)3(CO)2(PPh3)3 has been determined by single-crystal X-ray diffraction techniques. Crystals are triclinic, space group Pī with unit cell dimensions a 13.593(4), b 15.839(4), c 12.633(8) Ǻ, α 102.97(3), β 108.18(2), γ 84.86(3)° with Z2. The structure was refined by a full-matrix least-squares procedure on 5896 reflections [I ≥ 2.5σ(I)] to final R 0.028 and Rw 0.034. A triphenylphosphine ligand binds each of the metal atoms disposed at the corners of a triangle. Each metal-metal bond is spanned by a bridging carbonyl group. The coordination about the osmium atom is completed by two terminal carbonyl groups.

scholarly journals Synthesis of FeN4at 180 GPa and its crystal structure from a submicron-sized grain

2018 ◽  
Vol 74 (10) ◽  
pp. 1392-1395 ◽  
Author(s):  
Maxim Bykov ◽  
Saiana Khandarkhaeva ◽  
Timofey Fedotenko ◽  
Pavel Sedmak ◽  
Natalia Dubrovinskaia ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diamond Anvil Cell ◽  
Structural Model ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Wyckoff Position ◽  
Diamond Anvil ◽  
Laser Heated

Iron tetranitride, FeN4, was synthesized from the elements in a laser-heated diamond anvil cell at 180 (5) GPa and 2700 (200) K. Its crystal structure was determined based on single-crystal X-ray diffraction data collected from a submicron-sized grain at the synchrotron beamline ID11 of ESRF. The compound crystallizes in the triclinic space groupP\overline{1}. In the asymmetric unit, the Fe atom occupies an inversion centre (Wyckoff position 1d), while two N atoms occupy general positions (2i). The structure is made up from edge-sharing [FeN6] octahedra forming chains along [100] and being interconnected through N—N bridges. N atoms formcatena-poly[tetraz-1-ene-1,4-diyl] anions [–N=N—N—N–]∞2−running along [001]. In comparison with the previously reported structure of FeN4at 135 GPa [Bykovet al.(2018).Nat. Commun.9, 2756], the crystal structure of FeN4at 180 GPa is similar but the structural model is significantly improved in terms of the precision of the bond lengths and angles.

scholarly journals Synthesis, Characterization, and Crystal Structure of N-(3-nitrophenyl)cinnamamide

Crystals ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 599
Author(s):  
Jung-Seop Lee ◽  
Matthias Zeller ◽  
Shrikant Dashrath Warkad ◽  
Satish Balasaheb Nimse
Keyword(s):  
Crystal Structure ◽  
Density Functional ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
Cell Dimensions ◽  
Atomic Scattering ◽  
Unit Cell Dimensions ◽  
Experimental Structure

N-(3-nitrophenyl)cinnamamide 1 with formula C15H12N2O3 was synthesized, and its crystal structure was determined by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P21/n with unit cell dimensions: a = 6.7810 (5) Å, b = 23.0913 (15) Å, c = 8.2079 (5) Å, V = 1282.76 (15) Å3, Z = 4, determined at 150 K with MoKα radiation. The experimental structure refined against atomic scattering factors is compared with the structure obtained using a Hirshfeld Atom Refinement (HAR) approach and Density Functional Theory (DFT) geometry optimizations.

X-Ray-Diffraction Study and Determination of Absolute Configuration of the Anticancer Drug S(–) Cyclophosphamide (Endoxan, Cytoxan, NSC-26271)

1977 ◽  
Vol 32 (9-10) ◽  
pp. 672-677 ◽  
Author(s):  
D. A. Adamiak ◽  
W. Saenger ◽  
R. Kinas ◽  
W. J. Stec
Keyword(s):  
Absolute Configuration ◽  
Direct Methods ◽  
Ratio Test ◽  
Equatorial Position ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Determination Of Absolute Configuration

Abstract (-) Cyclophosphamide (1) crystallized from tetrachlorom ethane in the triclinic space group P1 with cell dimensions a = 10.500 (4) Å, b = 10.490 (4) Å, c = 10.761 (4) A, α = 110.0 (2) ° , β = 11 0.0(2)°, γ = 1 0 8.9(2)°. Three molecules are contained in the unit cell. The X-ray analysis was based on diffractometer measurement of 2635 independent reflections and the structure was solved by Patterson and direct methods. The final R and R w factors after full-matrix least-squares refinement are 0.0717 and 0.0677, respectively. The absolute configuration is S based on Hamilton’s R-factor ratio test. The oxazaphosphorinane ring exists in a chair form with the bis-β-chloroethyl-amino group in equatorial position and about perpendicular to and bisecting .The structure is similar to that found in racemic 1 except a different conformation about one ethyl-amino N-C bond.

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

On tungstates of divalent cations (III) – Pb5O2[WO6]

2020 ◽  
Vol 235 (8-9) ◽  
pp. 311-317
Author(s):  
Stephan G. Jantz ◽  
Florian Pielnhofer ◽  
Henning A. Höppe
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Quantum Chemical ◽  
Density Functional ◽  
Divalent Cations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
First Results ◽  
Electrostatic Calculations

Abstract${\text{Pb}}_{5}{\text{O}}_{2}\left[{\text{WO}}_{6}\right]$ was discovered as a frequently observed side phase during our investigation on lead tungstates. Its crystal structure was solved by single-crystal X-ray diffraction ($P{2}_{1}/n$, $a=7.4379\left(2\right)$ Å, $b=12.1115\left(4\right)$ Å, $c=10.6171\left(3\right)$ Å, $\beta =90.6847\left(8\right)$°, $Z=4$, ${R}_{\text{int}}=0.038$, ${R}_{1}=0.020$, $\omega {R}_{2}=0.029$, 4188 data, 128 param.) and is isotypic with ${\text{Pb}}_{5}{\text{O}}_{2}\left[{\text{Te}}_{6}\right]$. ${\text{Pb}}_{5}{\text{O}}_{2}\left[{\text{WO}}_{6}\right]$ comprises a layered structure built up by non-condensed [WO6]${}^{6-}$ octahedra and ${\left[{\text{O}}_{4}{\text{Pb}}_{10}\right]}^{12+}$ oligomers. The compound was characterised by spectroscopic measurements (Infrared (IR), Raman and Ultraviolet–visible (UV/Vis) spectra) as well as quantum chemical and electrostatic calculations (density functional theory (DFT), MAPLE) yielding a band gap of 2.9 eV fitting well with the optical one of 2.8 eV. An estimation of the refractive index based on the Gladstone-Dale relationship yielded $n\approx 2.31$. Furthermore first results of the thermal analysis are presented.

Two-dimensional lanthanide(III) coordination polymers: solvothermal synthesis, crystal structure, and stability

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Runmei Ding ◽  
Zixin He ◽  
Meilin Wang ◽  
Danian Tian ◽  
Peipei Cen
Keyword(s):  
Crystal Structure ◽  
Coordination Polymers ◽  
Solvothermal Synthesis ◽  
Analysis Data ◽  
Water Stability ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Solvothermal Conditions

AbstractBased on 2-(4-pyridyl)-terephthalate (H2pta) and oxalate ligands, two new lanthanide-containing coordination polymers (CPs), [Tb(pta)(C2O4)0.5(H2O)2)]·2H2O (1) and [Sm(pta)(C2O4)0.5(H2O)2)]·2H2O (2), have been synthesized under solvothermal conditions. The structures of both 1 and 2 have been determined by single-crystal X-ray diffraction. Infrared, elemental analysis, powder X-ray diffraction and thermogravimetric analysis data are also presented. The crystals of 1 and 2 exhibit isostructural layer-like networks, crystallizing in the triclinic space group P$‾{1}$. The layers are further stabilized and associated into 3D architectures through hydrogen bonding. Remarkably, the CPs 1 and 2 exhibit excellent water stability and remarkable thermostability with thermal decomposition temperatures of more than 420 °C.

scholarly journals Investigation of Solvatomorphism and Its Photophysical Implications for Archetypal Trinuclear Au3(1-Methylimidazolate)3

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4404
Author(s):  
Shengyang Guan ◽  
David C. Mayer ◽  
Christian Jandl ◽  
Sebastian J. Weishäupl ◽  
Angela Casini ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Density Functional ◽  
Bulk Material ◽  
Variable Temperature ◽  
Active Phase ◽  
Solvent Free ◽  
X Ray Diffraction ◽  
X Ray ◽  
Aurophilic Interactions

A new solvatomorph of [Au3(1-Methylimidazolate)3] (Au3(MeIm)3)—the simplest congener of imidazolate-based Au(I) cyclic trinuclear complexes (CTCs)—has been identified and structurally characterized. Single-crystal X-ray diffraction revealed a dichloromethane solvate exhibiting remarkably short intermolecular Au⋯Au distances (3.2190(7) Å). This goes along with a dimer formation in the solid state, which is not observed in a previously reported solvent-free crystal structure. Hirshfeld analysis, in combination with density functional theory (DFT) calculations, indicates that the dimerization is generally driven by attractive aurophilic interactions, which are commonly associated with the luminescence properties of CTCs. Since Au3(MeIm)3 has previously been reported to be emissive in the solid-state, we conducted a thorough photophysical study combined with phase analysis by means of powder X-ray diffraction (PXRD), to correctly attribute the photophysically active phase of the bulk material. Interestingly, all investigated powder samples accessed via different preparation methods can be assigned to the pristine solvent-free crystal structure, showing no aurophilic interactions. Finally, the observed strong thermochromism of the solid-state material was investigated by means of variable-temperature PXRD, ruling out a significant phase transition being responsible for the drastic change of the emission properties (hypsochromic shift from 710 nm to 510 nm) when lowering the temperature down to 77 K.

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