scholarly journals Synthesis, structure, thermal decomposition and spectral properties of neutral [Fe(bpta)2(etOH)2(NCS)2]

2015 ◽  
Vol 8 (1) ◽  
pp. 78-85
Author(s):  
Zuzana Lukačovičová ◽  
Róbert Uhrecký ◽  
Ján Moncoľ ◽  
Darina Lackováa ◽  
Iveta Ondrejkovičová ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Infrared Spectroscopy ◽  
Structural Analysis ◽  
Spectral Properties ◽  
Ethanol Solution ◽  
Single Crystal Diffraction ◽  
Triclinic Space Group ◽  
X Ray

Abstract The new iron(II) complex [Fe(bpta)2(EtOH)2(NCS)2] (bpta = 3,3’-(1,2,4-thiadiazole-3,5-diyl) dipyridine; EtOH = ethanol) has been prepared by refluxing Fe(NCS)3 or Fe(NCS)2 with thionicotinamide in an ethanol solution and characterized by elemental analysis, infrared spectroscopy, thermal decomposition and X-ray structural analysis. The characterized compound is a mixture of three regioisomers resulting from differential coordination by the 3- and 5-position 2-pyridyl groups. The bpta ligand was generated in situ by the oxidation dimerization of thionicotinamide. X-ray single-crystal diffraction revealed that the crystal structure is centrosymmetric and the complex crystallizes in the triclinic space group P-1. The iron(II) atom lies in the centre of symmetry and it is octahedrally coordinated by two nitrogen atoms from two thiocyanate anions and two oxygen atoms from ethanol molecules in the equatorial plane and two nitrogen atoms of pyridine rings from two bpta ligands in the axial positions. This complex represents the second example of metal complex with bpta.

scholarly journals Raman Spectroscopy and Single-Crystal High-Temperature Investigations of Bentorite, Ca6Cr2(SO4)3(OH)12·26H2O

Minerals ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 38
Author(s):  
Rafał Juroszek ◽  
Biljana Krüger ◽  
Irina Galuskina ◽  
Hannes Krüger ◽  
Martina Tribus ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Single Crystal ◽  
Chemical Formula ◽  
Crystal Chemical Formula ◽  
Single Crystal Diffraction ◽  
Bending Vibrations ◽  
X Ray ◽  
First Time

The crystal structure of bentorite, ideally Ca6Cr2(SO4)3(OH)12·26H2O, a Cr3+ analogue of ettringite, is for the first time investigated using X-ray single crystal diffraction. Bentorite crystals of suitable quality were found in the Arad Stone Quarry within the pyrometamorphic rock of the Hatrurim Complex (Mottled Zone). The preliminary semi-quantitative data on the bentorite composition obtained by SEM-EDS show that the average Cr/(Cr + Al) ratio of this sample is >0.8. Bentorite crystallizes in space group P31c, with a = b = 11.1927(5) Å, c =21.7121(10) Å, V = 2355.60(18) Å3, and Z = 2. The crystal structure is refined, including the hydrogen atom positions, to an agreement index R1 = 3.88%. The bentorite crystal chemical formula is Ca6(Cr1.613Al0.387)Σ2[(SO4)2.750(CO3)0.499]Σ3.249(OH)11.502·~25.75H2O. The Raman spectra of bentorite from two different localities exhibit the presence of the main stretching and bending vibrations related to the sulfate group at 983 cm−1 (ν1), 1109 cm−1 (ν3), 442 cm−1 (ν2), and 601 cm−1 (ν4). Moreover, the presence of bands assigned to the symmetric Cr(OH)63− stretching mode and hydroxyl deformation vibrations of Cr–OH units at ~540 cm−1 and ~757 cm−1, respectively, may be used to distinguish between ettringite and bentorite. In situ high temperature single crystal XRD experiments show that the decomposition of bentorite starts at ca. 45 °C and that a dehydroxylation product similar to metaettringite is formed.

Crystal Structure of 3-Indolepropionic Acid

2013 ◽  
Vol 454 ◽  
pp. 272-275
Author(s):  
Li Hua Wang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Ethanol Solution ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
One Dimensional ◽  
X Ray

The crystals of 3-indolepropionic acid have been obtained by evaporation from ethanol solution. The crystal structure of the 3-indolepropionic acid was determined by X-ray single crystal diffraction analysis. The crystal data for 3-indolepropionic acid: monoclinic, space group P2(1)/c, a = 14.3592(8) Å, b = 5.2446(2) Å, c = 12.3518(6) Å, V = 926.96(8) Å3, Z = 4, Mr = 189.21, De = 1.356 g/cm3, T = 298(2) K, F (000) = 400, R = 0.0435 and wR = 0.1010. The compound forms one-dimensional chained structure through hydrogen bonds and π-π interaction.

scholarly journals Synthesis, Characterization, and Crystal Structure of a Diorganotin(IV) Complex with 2-Oxo-2-Phenylacetic Acid 4-Hydroxybenzohydrazone

2011 ◽  
Vol 2011 ◽  
pp. 1-5 ◽  
Author(s):  
Jing Li ◽  
Handong Yin ◽  
Min Hong
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Phenylacetic Acid ◽  
Pentagonal Bipyramid ◽  
Two Dimensional ◽  
Single Crystal Diffraction ◽  
Triclinic Space Group ◽  
Ethanol Molecule ◽  
X Ray ◽  
C Nmr

The complex dibutyltin 2-oxo-2-phenylacetic acid 4-hydroxybenzohydrazone has been synthesized and characterized by elemental analysis, IR, 1H and 13C NMR, and X-ray single-crystal diffraction studies. The crystal structure belongs to triclinic, space group P-1 with a=9.3220 (10) Å, b=9.8779 (11) Å, c=15.9401 (17) Å, β=97.0930 (10)∘, Z=2, V=1427.6(3) Å3, Dc=1.413 mg/cm3, μ=0.936 mm−1, F(000)=628, R=0.1158, and wR=0.2522. X-ray analysis indicates that O(2), N(2), O(4), and O(4)#1 from the ligand and O(5) from ethanol molecule are in the equatorial positions; the axial positions are occupied by two n-butyl groups. It shows a distorted pentagonal bipyramid configuration with seven-coordination for central tin atom. Fascinatingly, the supramolecular infrastructures are observed, which exist as two-dimensional sheets assembled from the organometallic subunits through intermolecular and intramolecular O–H⋯X or C–H⋯X (X = O or N) hydrogen bonds.

One-Dimensional Chained Polymer Constructed by 3-Indolepropionic Acid and 2,2'-Bipyridinium

2013 ◽  
Vol 454 ◽  
pp. 276-279
Author(s):  
Li Hua Wang ◽  
Zhi Xiang Ji
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Network Structure ◽  
Ethanol Solution ◽  
Monoclinic Space Group ◽  
Single Crystal Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
3D Network ◽  
The One

The crystals of one-dimensional chained polymer constructed by 3-indolepropionic acid and 2,2-bipyridinium have been synthesized by evaporation from ethanol solution. The crystal structure of one-dimensional chained polymer was determined by X-ray single crystal diffraction analysis. The results shows that the polymer belongs to monoclinic, space group P2(1)/c, a = 5.2557(11) Å, b = 12.249(2) Å, c = 21.467(4) Å, V = 1380.1(5) Å3, Z = 2, Mr = 531.58, De = 1.279 g/cm3, T = 293(2) K, F (000) = 558, R = 0.1136 and wR = 0.3376. The compound forms one-dimensional chained polymer through hydrogen bonds. 3D network structure was constructed by the interaction of the one-dimensional chained polymer.

Crystal Structure Characterization of 4,4-diaminodiphenyl Sulfoxide

2013 ◽  
Vol 848 ◽  
pp. 195-198
Author(s):  
Zhi Xiang Ji
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Ethanol Solution ◽  
Structure Characterization ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Dimensional Network

The crystals of 4,4-diaminodiphenyl sulfoxide have been obtained by evaporation from ethanol solution. The crystal structure of the 4,4-diaminodiphenyl sulfoxide was determined by X-ray single crystal diffraction analysis. The crystal data for 4,4-diaminodiphenyl sulfoxide: monoclinic, space groupP2(1)/c,a= 49.068(10) Å,b= 11.439(2) Å,c= 13.103(3) Å,V= 7347(3) Å3,Z= 24,Mr= 248.30,De= 1.347 g/cm3,T= 298(2) K,F(000) = 3120,R= 0.0786 andwR =0.2653. The compound forms three-dimensional network structure through hydrogen bonds and π-π interaction.

Structural investigation of co-evaporated methyl ammonium lead halide perovskite films during growth and thermal decomposition using different PbX2 (X = I, Cl) precursors

2015 ◽  
Vol 3 (39) ◽  
pp. 19842-19849 ◽  
Author(s):  
Juliane Borchert ◽  
Heidi Boht ◽  
Wolfgang Fränzel ◽  
René Csuk ◽  
Roland Scheer ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Structural Analysis ◽  
Structural Investigation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Detailed Structural Analysis ◽  
Halide Perovskite ◽  
Lead Halide

Here we present a detailed structural analysis of methylammonium lead halide (I, Cl) films by in situ X-ray diffraction during their growth and thermal recrystallization up to their decomposition.

Cystamindi-ium tetrachlorocuprate [NH3(CH2)2SS(CH2)2NH3][CuCl4]: synthesis, crystal structure, and thermal decomposition

2015 ◽  
Vol 30 (2) ◽  
pp. 163-169 ◽  
Author(s):  
D. Y. Leshok ◽  
N. N. Golovnev ◽  
S. D. Kirik
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Infrared Spectroscopy ◽  
Ionic Structure ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Organic Layers ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Inorganic Layers

The salt [NH3(CH2)2SS(CH2)2NH3][CuCl4] was obtained by crystallization after adding CuCl2 to cystamine (Cysta), solved in hydrochloric acid. The assumption of conserved disulfide connection (S–S) in the compound, made on the basis of infrared spectroscopy, is further supported by the crystal structure determined from X-ray powder diffraction data. The compound has an ionic structure. [CuCl4]2− and CystaH22+ ions package in the form of inorganic and organic layers in the cell, interconnected through the formation of hydrogen bonds via NH3-groups and chlorine atoms of the complex [CuCl4]2−. Inorganic layers are additionally stabilized in the parquet package of [CuCl4]2− ions which provides a Cu-distorted octahedral coordination. CystaH2[CuCl4] is stable in air up to 200 °C. Thermal decomposition occurs in several stages, accompanied by breaking of S–S bonds, releasing of the organic component and yielding CuO.

Organolanthanoids. XVII. The Synthesis of Bis(diphenylphosphinocyclopentadienyl)ytterbium(II) and Derived Heterobimetallic Complexes [Yb(thf)n(C5H4PPh2)2Z] [Z=Ni(CO)2, Mo(CO)4 or PtMe2; n = 1 or 2; thf = Tetrahydrofuran]. The X-Ray Crystal-Structure of [Yb(thf)2(C5H4PPh2)2Ni(CO)2]

1992 ◽  
Vol 45 (3) ◽  
pp. 567 ◽  
Author(s):  
GB Deacon ◽  
CM Forsyth ◽  
WC Patalinghug ◽  
AH White ◽  
A Dietrich ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Transition Metal ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Heterobimetallic Complexes

Reaction of diphenylphosphinocyclopentadiene with Yb (C6F5)2 or with ytterbium metal and Hg(C6F5)2 in tetrahydrofuran ( thf ) gives, after workup with toluene, the phosphinoytter-bocene , [Yb (C5H4PPh2)2( thf )]. Treatment with thf or with N,N,N′,N′- tetramethylethane-1,2-diamine ( tmen ) yields [ Yb (C5H4PPh2)2L2] (L = thf or L2 = tmen ). Redox trans- metallation between ytterbium metal and Tl (C5H4PPh2) in l,2-dimethoxyethane ( dme ) gives thallium metal and [ Yb (C5H4PPh2)2(dme )]. The ytterbium-transition metal hetero-bimetallics [ Yb ( thf ) (C2H4PPh2)2Z]. nPhMe [Z = Ni(CO)2, Mo(CO)4 or PtMe2, n = 2/3 or 1] have been prepared by reaction of [ Yb ( thf )(C5H4PPh2)2] with Ni(CO)2(PPh3)2, Mo(CO)4( nbd ) ( nbd = norbornadiene ) or PtMe2(cod) (cod = cycloocta-1,5-diene) in toluene. Treatment of the heterobimetallics with tetrahydrofuran [Z = PtMe2 or Mo(CO)4] or a preparation in thf /toluene [Z = Ni(CO)2] yields [ Yb ( thf )2(C5H4PPh2)2PtMe2]. thf, [ Yb ( thf )2(C2H4PPh2)2Mo(CO)4]. thf and [ Yb ( thf )2 (C5H4PPh2)2Ni(CO)2]. The X-ray crystal structure of the last compound (triclinic, space group Pi, a 14.514(5), b 13.565(1), c 10.866(5) 93.11(2), β 104.65(3), γ 97.25(2)�, U 2045 � 3 , Z 2, 5141 data refined to R 0.031) reveals eight-coordinate ytterbium with a pseudo-tetrahedral arrangement of two thf ligands and the cyclopentadienyl ring centroids of two ή5 -diphenylphosphinocyclopentadienide ligands . The latter are also bonded through phosphorus to the Ni(CO)2 group, resulting in tetrahedral stereochemistry for nickel. Infrared spectroscopy suggests the presence of ytterbium- isocarbonyl bonding in solid [ Yb ( thf )(C2H4PPh2)2Z] [Z = Ni(CO)2 or Mo(CO)4].

Synthesis, Crystal Structure and Thermal Decomposition Mechanism of a Dysprosium(III) p-Fluorobenzoate 1,10-Phenanthroline Complex

2007 ◽  
Vol 62 (1) ◽  
pp. 51-54 ◽  
Author(s):  
Su-Ling Xu ◽  
Jian-Jun Zhang ◽  
Hui-Fang Yang ◽  
Ning Ren ◽  
Hai-Yan Zhang
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Molar Conductance ◽  
Thermal Decomposition Mechanism ◽  
Carboxylate Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Carboxylate Groups ◽  
Phenanthroline Complex

A dinuclear dysprosium(III) p-fluorobenzoate 1,10-phenanthroline complex, [Dy(p-FBA)3phen]2 was synthesized and characterized by elemental analysis, UV and IR spectroscopy, single crystal X-ray diffraction, molar conductance, and TG-DTG techniques. It crystallizes in the triclinic space group P1̄ with a = 9.895(5), b = 11.754(6), c = 14.756(10)Å ; α = 106.660(9)°, β = 107.956(9)°, γ =101.472(7)°; Z =1. The Dy(III) ions are eight coordinate including one terminal bidentate chelating carboxylate group, four bridging carboxylate groups and one 1,10-phenanthroline molecule. The thermal decomposition of [Dy(p-FBA)3phen]2 has been followed by thermal analysis. The lifetime equation at weight-loss of 10% was deduced as lnτ = −27.0798 +19010.2434/T by isothermal thermogravimetric analysis.

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.

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