Spectroscopic Investigations on New Organic NLO crystal – 2-amino-5-chloropyridinium-2,4-dinitrophenolate

2017 ◽  
Vol 232 (1) ◽  
Author(s):  
Pullithodi Mohamed Kutty ◽  
Joseph Chandrasekaran ◽  
Balraj Babu ◽  
Yoshitaka Matsushita
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Room Temperature ◽  
Methanol Solution ◽  
Powder Xrd ◽  
Single Crystal Xrd ◽  
Slow Evaporation ◽  
Crystalline Phases ◽  
Evaporation Method

AbstractNew organic single crystals of 2-amino-5-chloropyridinium-2,4-dinitrophenolate were successfully grown by the slow evaporation method at room temperature from methanol solution. Crystal structure and crystalline phases were confirmed from the single crystal XRD and powder XRD, respectively.

The crystal structure of a simple enol formed in a single-crystal-to-single-crystal enolene rearrangement

2004 ◽  
Vol 82 (2) ◽  
pp. 301-305 ◽  
Author(s):  
Kenneth CW Chong ◽  
Brian O Patrick ◽  
John R Scheffer
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Room Temperature ◽  
Thermal Reaction ◽  
Thermal Rearrangement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phenyl Ketone

When crystals of 9-tricyclo[4.4.1.0]undecalyl-4-(carbomethoxy)phenyl ketone (1) were allowed to stand in the dark for extended periods of time at room temperature, the compound underwent a thermal reaction — the enolene rearrangement — to afford enol 2. The crystals remained transparent and appeared unchanged in shape as the reaction proceeded. X-ray diffraction data were collected on single crystals containing 17%, 25%, 66%, and 100% of the enol. The crystal structure of a simple enol was obtained via this novel single-crystal-to-single-crystal enolene rearrangement.Key words: single crystal, thermal, rearrangement, enol, enolene.

Synthese, Kristallstruktur und Eigenschaften von 1,1,1,3,3, 3 - Hexaamino - 1λ5,3λ5-diphosphazeniumehlorid [(NH2)3PNP(NH2)3]Cl / Synthesis, Crystal Structure, and Properties of 1,1,1,3,3,3-Hexaamino- 1λ5 ,3λ5-diphosphazenium Chloride [(NH2)3 PNP(NH2)3 ]Cl

1996 ◽  
Vol 51 (12) ◽  
pp. 1732-1738 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
Temperature Gradient ◽  
Single Crystal ◽  
Single Crystals ◽  
Room Temperature ◽  
Acetonitrile Solution ◽  
Structure And Properties ◽  
X Ray ◽  
Ray Methods

[(NH2)3PNP(NH2)3]Cl has been prepared by a three step synthesis. The last step is the ammonolysis of [Cl3PNPCl3]Cl. Single crystals of 1,1,1,3,3,3-hexaamino-1λ5, 3λ5-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -100 °C [(NH2)3PNP(NH2)3]Cl is subject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P1̄, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, β = 76.36(3)°, γ = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles.

Piperazinediium Diselenatohexaaquacobaltate(II) Dihydrate (C4H12N2)[Co(SeO4)2(H2O)4]·2H2O

2012 ◽  
Vol 194 ◽  
pp. 171-174 ◽  
Author(s):  
Nouha Loulou Nkhili ◽  
Walid Rekik ◽  
Houcine Naili ◽  
Tahar Mhiri ◽  
Thierry Bataille
Keyword(s):  
Crystal Structure ◽  
Transition Metal ◽  
Hydrogen Bonds ◽  
Hybrid Material ◽  
Room Temperature ◽  
Water Molecules ◽  
Slow Evaporation ◽  
Monoclinic System ◽  
Space Group ◽  
Evaporation Method

The new hybrid material, (C4H12N2)[Co(H2O)4(SeO4)2]·2H2O, has been synthesized by the slow evaporation method at room temperature and crystallographically characterized. It crystallizes in the monoclinic system, space group P21 /n. The crystal structure of this compound consists of transition metal, Co(II), octahedrally coordinated by four water molecules and two selenate groups forming the [Co(H2O)4(SeO4)2]2-anions, water molecules and piperazinediium cations (C4H12N2)2+linked together by two types of hydrogen bonds, OW–H…O and N–H…O.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

scholarly journals Crystal Structure of Moganite and Its Anisotropic Atomic Displacement Parameters Determined by Synchrotron X-ray Diffraction and X-ray/Neutron Pair Distribution Function Analyses

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 272
Author(s):  
Seungyeol Lee ◽  
Huifang Xu ◽  
Hongwu Xu ◽  
Joerg Neuefeind
Keyword(s):  
Crystal Structure ◽  
Distribution Function ◽  
Single Crystal ◽  
Pair Distribution Function ◽  
Atomic Displacement ◽  
Single Crystal Xrd ◽  
X Ray Diffraction ◽  
X Ray ◽  
Neutron Pair ◽  
Atomic Displacement Parameters

The crystal structure of moganite from the Mogán formation on Gran Canaria has been re-investigated using high-resolution synchrotron X-ray diffraction (XRD) and X-ray/neutron pair distribution function (PDF) analyses. Our study for the first time reports the anisotropic atomic displacement parameters (ADPs) of a natural moganite. Rietveld analysis of synchrotron XRD data determined the crystal structure of moganite with the space group I2/a. The refined unit-cell parameters are a = 8.7363(8), b = 4.8688(5), c = 10.7203(9) Å, and β = 90.212(4)°. The ADPs of Si and O in moganite were obtained from X-ray and neutron PDF analyses. The shapes and orientations of the anisotropic ellipsoids determined from X-ray and neutron measurements are similar. The anisotropic ellipsoids for O extend along planes perpendicular to the Si-Si axis of corner-sharing SiO4 tetrahedra, suggesting precession-like movement. Neutron PDF result confirms the occurrence of OH over some of the tetrahedral sites. We postulate that moganite nanomineral is stable with respect to quartz in hypersaline water. The ADPs of moganite show a similar trend as those of quartz determined by single-crystal XRD. In short, the combined methods can provide high-quality structural parameters of moganite nanomineral, including its ADPs and extra OH position at the surface. This approach can be used as an alternative means for solving the structures of crystals that are not large enough for single-crystal XRD measurements, such as fine-grained and nanocrystalline minerals formed in various geological environments.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Calcium Carbodiimide Compounds Revisited – Syntheses, Single Crystal Structure Determination and Vibrational Spectra of Ca11N6[CN2]2, Ca4N2[CN2] and Ca[CN2]

2008 ◽  
Vol 63 (5) ◽  
pp. 530-536 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
X Ray ◽  
Characteristic Features ◽  
Reported Data ◽  
Correct Data

Single crystals of Ca11N6[CN2]2 (dark red needles, tetragonal, P42/mnm (no. 136), a = 1456.22(5), and c = 361.86(2) pm, Z = 2), Ca4N2[CN2] (transparent yellow needles, orthorhombic, Pnma (no. 62), a = 1146.51(11), b = 358.33(4), and c = 1385.77(13) pm, Z = 4) and Ca[CN2] (transparent, colorless, triangular plates, rhombohedral, R3̅m (no. 166), a = 369.00(3), and c = 1477.5(3) pm, Z = 3) were obtained by the reaction of Na2[CN2], CaCl2 and Ca3N2 (if demanded by stoichiometry) in arc-welded Ta ampoules at temperatures between 1200 - 1400 K. Their crystal structures were re-determined by means of single crystal X-ray structure analyses. Additionally, the Raman spectra were recorded on these same single crystals, whereas the IR spectra were obtained with the KBr pellet technique. The title compounds exhibit characteristic features for carbodiimide units with D∞h symmetry (d(C-N) = 121.7 - 123.8 pm and ∡ (N-C-N) = 180°). The vibrational frequencies of these units are in the expected range (Ca11N6[CN2]2: νs = 1230, νs = 2008; δ = 673/645/624 cm−1; Ca4N2[CN2]: νs = 1230, νs = 1986; δ = 672/647 cm−1; Ca[CN2]: νs = 1274, νs = 2031, δ = 668 cm−1). The structural results are more precise than the previously reported data, and with the newly attained Raman spectrum of Ca11N6[CN2]2 we correct data reported earlier.

Crystal and powder XRD data of Mg3(PO4)2-III: High-temperature and high-pressure form

1995 ◽  
Vol 10 (4) ◽  
pp. 293-295 ◽  
Author(s):  
F. Brunet ◽  
C. Chopin ◽  
A. Elfakir ◽  
M. Quarton
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Single Crystal ◽  
Diffraction Pattern ◽  
Structure Refinement ◽  
Powder Xrd ◽  
Single Crystal Structure ◽  
Crystal Structure Refinement ◽  
Pressure Form

A new diffraction pattern of the high-temperature and high-pressure polymorph Mg3(PO4)2-III (PDF 43-500) is given and indexed on the basis of a single-crystal structure refinement. It allows diffractogram indexing of the isostructural high-temperature and high-pressure form of Co3(PO4)2 (PDF 43-499).

The Characteristic of the La3Ga5SiO14 Single Crystal Grown by Vertical Bridgman Method in Ar Atmosphere

2006 ◽  
Vol 510-511 ◽  
pp. 842-845 ◽  
Author(s):  
Noriko Bamba ◽  
Kentaro Kato ◽  
Toshinori Taishi ◽  
Takayuki Hayashi ◽  
Keigo Hoshikawa ◽  
...  
Keyword(s):  
Melting Point ◽  
Single Crystal ◽  
Single Crystals ◽  
Room Temperature ◽  
Color Change ◽  
Piezoelectric Materials ◽  
Lead Free ◽  
Piezoelectric Constant ◽  
Interstitial Oxygen ◽  
Vertical Bridgman

Langasite (La3Ga5SiO14: denoted by LGS) single crystal is one of the lead free piezoelectric materials with high piezoelectricity that is maintained up to its melting point (1470°C). Although LGS single crystals have usually been grown by Czochralski (CZ) method in oxygen contained atmosphere to prevent evaporation of Ga, they were grown by the vertical Bridgman (VB) method in Ar atmosphere without oxygen, and their properties were evaluated in this work. Transparent and colorless LGS single crystals were successfully obtained without Ga evaporation by the VB method in Ar atmosphere, and their resistivity at room temperature was much higher than that grown by conventional CZ method. Piezoelectric constant d11 of the crystal grown by the VB method was 6 x 10-12 C/N, which was close to that of the crystal grown by CZ method. The colorless transparent LGS single crystal turned to orange and its resistivity decreased by annealing in air. Since an orange-colored transparent LGS single crystal has been grown by conventional CZ method, this indicates that color change and the resistivity decrease of LGS crystal is caused by extra interstitial oxygen atoms in the crystal.

scholarly journals Crystal structure of the new hybrid material bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate

2015 ◽  
Vol 71 (11) ◽  
pp. 1384-1387
Author(s):  
Marwen Chouri ◽  
Habib Boughzala
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Molar Ratio ◽  
Water Molecules ◽  
Site Symmetry ◽  
Two Dimensional ◽  
Slow Evaporation ◽  
Solution Ph

The title compound bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate, (C6H14N2)2[Bi2Cl10]·2H2O, was obtained by slow evaporation at room temperature of a hydrochloric aqueous solution (pH = 1) containing bismuth(III) nitrate and 1,4-diazabicyclo[2.2.2]octane (DABCO) in a 1:2 molar ratio. The structure displays a two-dimensional arrangement parallel to (100) of isolated [Bi2Cl10]4−bioctahedra (site symmetry -1) separated by layers of organic 1,4-diazoniabicyclo[2.2.2]octane dications [(DABCOH2)2+] and water molecules. O—H...Cl, N—H...O and N—H...Cl hydrogen bonds lead to additional cohesion of the structure.

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