scholarly journals The Reduction of Pyridine by K12Si17 to the 4,4′-Bipyridine Radical Anion [C10H8N2]-•: Crystal Structure and Spectroscopic Characterization of [K([2.2.2]crypt)][C10H8N2]

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1119-1123 ◽  
Author(s):  
Christian B. Benda ◽  
Thomas F. Fässler
Keyword(s):  
Crystal Structure ◽  
Radical Anion ◽  
Spectroscopic Characterization ◽  
X Ray Diffraction ◽  
Compound K ◽  
Zintl Phase ◽  
X Ray ◽  
Vis Spectroscopy ◽  
C Nmr

Abstract From an anhydrous pyridine extract of the binary Zintl phase K12Si17 in the presence of the cation sequestering agent [2.2.2]crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) crystals of the compound [K([2.2.2]crypt)][C10H8N2] have been isolated which contains the 4,4′- bipyridine radical monoanion. This compound was fully characterized by X-ray diffraction, 1H, 13C NMR, EPR, IR and UV=Vis spectroscopy

scholarly journals Synthesis, Crystal Structures, and Spectroscopic Characterization of Bis-aldehyde Monomers and Their Electrically Conductive Pristine Polyazomethines

Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  
Keyword(s):  
Electrical Conductivity ◽  
Spectroscopic Characterization ◽  
Spectroscopic Techniques ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
Electrically Conductive ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Ft Ir

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.

Structural and IR-spectroscopic characterization of magnesium acesulfamate

2016 ◽  
Vol 71 (1) ◽  
pp. 51-55 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Elemental Analysis ◽  
Spectroscopic Characterization ◽  
Magnesium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic

AbstractMagnesium acesulfamate, Mg(C4H4NO4S)2·6H2O, was prepared by the reaction of acesulfamic acid and magnesium carbonate in aqueous solution, and characterized by elemental analysis. Its crystal structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the triclinic space group P1̅ with one molecule per unit cell. The FTIR spectrum of the compound was also recorded and is briefly discussed. Some comparisons with other simple acesulfamate and saccharinate salts are also made.

Synthesis, Spectral, Thermal and Structural Characterization of the Copper(II) Saccharinato Complex of 2–Aminopyrimidine, [Cu(sac–O)2(ampym–N)2(H2O)2]·2ampym

2006 ◽  
Vol 61 (2) ◽  
pp. 153-158
Author(s):  
Okan Zafer Yeşilel ◽  
Halis Ölmez ◽  
Hümeyra Paşaoğlu ◽  
Gökhan Kaştaş ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Π Interactions ◽  
Hydrogen Bonding Interactions ◽  
Vis Spectroscopy ◽  
Phenyl Rings ◽  
In Trans

AbstractBis(2-aminopyrimidine-N)diaquabis(saccharinato-O)copper(II) di(2-aminopyrimidine), [Cu(sac-O)2(ampym-N)2(H2O)2] · 2ampym was synthesized and characterized by means of elemental analysis, IR and UV-vis spectroscopy, magnetic susceptibility, simultaneous TG, DTG, DTA techniques, and X-ray diffraction. The complex crystallizes in the monoclinic space group P21/c [a = 7.4697(5), b = 10.1679(5), c = 22.743(2)Å , β = 92.844(5), Z = 2, R = 0.0275, wR= 0.0757, V = 1725.26(19) Å3]. The copper atom is bonded to two ampym N atoms and two sac O atoms as well as to two water O atoms in trans positions in the geometry of a distorted octahedron. There are also two ampym moieties as solvate molecules in the unit cell. The crystal structure is stabilized by N-H· · ·O, O-H· · ·N and C-H· · ·O type hydrogen bonding interactions. Intermolecular π−π interactions between the phenyl rings of ampym groups and C-H· · ·π interactions also support the packing of the molecules. The thermal decomposition of the complex has been studied.

Darstellung und spektroskopische Charakterisierung von (η3-Hexahydro-closo-hexaborato)phenylquecksilber(1-) [Hg(η3-B6H6)Ph] sowie Kristallstruktur von [PPh4][Hg(η3-B6H6)Ph] / Preparation and Spectroscopic Characterization of (η3-Hexahydro-closo-hexaborato)phenylmercury(1 -) [Hg(η3-B6H6)Ph]- and Crystal Structure of [PPh4][Hg(η3-B6H6)Ph]

1997 ◽  
Vol 52 (1) ◽  
pp. 57-60 ◽  
Author(s):  
T. Schaper ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Lower Field ◽  
Nmr Spectrum ◽  
X Ray ◽  
Ir And Raman

By reaction of [B6H7]- with PhHg(CH3COO) in dichloromethane [Hg(η3-B6H6)Ph]- is formed. The crystal structure of [PPh4][Hg(η3-B6H6)Ph] has been determined by single crystal X-ray diffraction analysis; monoclinic space group P 21/c with a = 9.567(5) Å, b = 22.213(5) Å, c = 14.296(5) Å, β = 94.484(5)°. The 11B NMR spectrum exhibits a doublet at -9.9 ppm shifted to lower field as compared with [B6H7]- and the 199Hg NMR spectrum a singlet at -74.5 ppm. In the IR and Raman spectra characteristic B-H vibrations are observed

scholarly journals Crystal structure of 2-(2,6-diisopropylphenyl)-N,N-diethyl-3,3-dimethyl-2-azaspiro[4.5]decan-1-amine: a diethylamine adduct of a cyclic(alkyl)(amino)carbene (CAAC)

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Roxanne A. Naumann ◽  
Joseph W. Ziller ◽  
Allegra L. Liberman-Martin
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Title Compound ◽  
Lithium Diisopropylamide ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compound C ◽  
Lithium Diethylamide ◽  
C Nmr

The structure of the title compound, C27H46N2, at 93 K has monoclinic (P21/n) symmetry. The title compound was prepared by treatment of 2-(2,6-diisopropylbenzene)-3,3-dimethyl-2-azaspiro[4.5]dec-1-en-2-ium hydrogen dichloride with two equivalents of lithium diethylamide. Characterization of the title compound by single-crystal X-ray diffraction and 1H and 13C NMR spectroscopy is presented. Formation of the diethylamine adduct of the cyclic(alkyl)(amino)carbene (CAAC) was unexpected, as deprotonation using lithium diisopropylamide results in free CAAC formation.

Structural and IR-spectroscopic characterization of pyridinium acesulfamate, a monoclinic twin

2018 ◽  
Vol 73 (11) ◽  
pp. 753-758
Author(s):  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridinium Cation ◽  
Ft Ir ◽  
The Fourier Transform ◽  
Ir Spectroscopic

AbstractThe crystal structure of pyridinium 6-methyl-1,2,3,-oxathiazine-4(3H)-one-2,2-dioxide [(C5NH6)(C4H4NO4S)], for short, pyH(ace), was determined by X-ray diffraction methods. It crystallizes as a twin in the monoclinic space group P21/c with a=6.9878(9), b=7.2211(7), c=21.740(2) Å, β=91.67(1)° and Z=4 molecules per unit cell. The structure was determined employing 1599 reflections with I>2σ(I) from one of the twin domains and refined employing 2092 reflections from both crystal domains to an agreement R1 factor of 0.0466. Besides electrostatic attractions, intermolecular pyH···O=C(ace) hydrogen bonds stabilize the acesulfamate anion and the pyridinium cation into planar discrete units parallel to the (100) crystal plane. The units form stacks of alternating ace− and pyH+ ions along the a axis that favors inter-ring π–π interactions. The Fourier transform-infrared (FT-IR) spectrum of the compound was recorded and is briefly discussed. Some comparisons with related pyridinium saccharinate salts are also made.

Synthese, Kristallstruktur und Spektroskopische Charakterisierung des Phosphaniminato-Komplexes [Cl2AlNPCl3]2 und des Phosphanimin-Komplexes [Me3SiNPCl3 · AlCl3]/Synthesis, Crystal Structure, and Spectroscopic Characterization of the Phosphorane Iminato Complex [Cl2AlNPCl3]2, and of the Phosphane Imine Complex [Me3SiNPCl3 · AlCl3]

2002 ◽  
Vol 57 (11) ◽  
pp. 1237-1243 ◽  
Author(s):  
Britta Jächke ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Point Group ◽  
Spectroscopic Characterization ◽  
Membered Ring ◽  
Site Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Donor Acceptor ◽  
New Compounds

Reaction of Me3SiNPCl3 with AlCl3 yields the donor-acceptor complex [Me3SiNPCl3 · AlCl3] (1). Thermal treatment of 1 and simultaneously removing the by-product Me3SiCl results in the formation of [Cl2AlNPCl3]2 (2). Crystallization of 2 from CH2Cl2 yields colorless crystals which have been characterized by single crystal X-ray diffraction analysis (P1̄, a = 719.1(2), b = 843.5(2), c = 857.4(2) pm, α = 64.23(1), β = 76.62(1), γ = 68.21(1)°, Z = 1, R1 = 0.0498). The molecule exhibits site symmetry Ci (point group approximately C2h) and shows as a characteristic feature a planar, almost square Al2N2 four-membered ring with Al-N distances of 187.5(3) and 187.9(3) pm. The phosphorus atoms of the PCl3-groups attached to the nitrogen atoms are almost located in the same plane as defined by the Al2N2-ring. Both new compounds have been characterized by IR, NMR, and MS spectroscopy.

Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.

Crystal structure characterization and electronic structure of a rare-earth-containing Zintl phase in the Yb–Al–Sb family: Yb3AlSb3

2021 ◽  
Vol 77 (6) ◽  
Author(s):  
Rongqing Shang ◽  
An T. Nguyen ◽  
Allan He ◽  
Susan M. Kauzlarich
Keyword(s):  
Crystal Structure ◽  
Electronic Structure ◽  
Rare Earth ◽  
Electronic Structure Calculations ◽  
Structure Characterization ◽  
Charge Balance ◽  
X Ray Diffraction ◽  
Zintl Phase ◽  
X Ray ◽  
Structure Calculations

A rare-earth-containing compound, ytterbium aluminium antimonide, Yb3AlSb3 (Ca3AlAs3-type structure), has been successfully synthesized within the Yb–Al–Sb system through flux methods. According to the Zintl formalism, this structure is nominally made up of (Yb2+)3[(Al1−)(1b – Sb2−)2(2b – Sb1−)], where 1b and 2b indicate 1-bonded and 2-bonded, respectively, and Al is treated as part of the covalent anionic network. The crystal structure features infinite corner-sharing AlSb4 tetrahedra, [AlSb2Sb2/2]6−, with Yb2+ cations residing between the tetrahedra to provide charge balance. Herein, the synthetic conditions, the crystal structure determined from single-crystal X-ray diffraction data, and electronic structure calculations are reported.

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