Synthesis and X-ray Crystal Structure of the Novel Organotin Dication [n-Bu2Sn(H2O)4]2+:  A Lamellar Layered Structure Assisted by Intermolecular Hydrogen Bonding

2002 ◽  
Vol 21 (22) ◽  
pp. 4575-4577 ◽  
Author(s):  
Vadapalli Chandrasekhar ◽  
Ramamoorthy Boomishankar ◽  
Sanjay Singh ◽  
Alexander Steiner ◽  
Stefano Zacchini
Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.


1989 ◽  
Vol 44 (8) ◽  
pp. 942-945 ◽  
Author(s):  
Wolfgang Schnick

Phosphorothionic triamide SP(NH2)3 is obtained by slow addition of SPCl3 dissolved in dry CH2Cl2 to a satured solution of NH3 in CH2Cl2 at —50°C. Ammonium chloride is removed from the resulting precipitate by treatment with HNEt2 followed by extraction with CH2Cl2. Coarse crystalline SP(NH2)3 is obtained after recrystallization from dry methanol. The crystal structure of SP(NH2)3 has been determined by single crystal X-ray methods (Pbca; a = 922.3(1), b = 953.8(1), c = 1058.4(2) pm, Z = 8). In the crystals the molecules show non-crystallographic point symmetry C8. The P—S bond (195.4(1) pm) is slightly longer than in SPCl3. From P—N bond lengths of about 166 pm a significant electrostatic strengthening of the P—N single bonds is assumed. Weak intermolecular hydrogen bonding interactions (N —H · · · N ≥ 329.5 pm; N — H · · · S ≥ 348.3 pm) are observed.Investigation of thermal properties shows a melting temperature of 115°C for SP(NH2)3. According to combined DTA/TG and MS investigations above this temperature the compound decomposes by evolution of H2S and NH3 to yield amorphous phosphorus(V)nitride.


1978 ◽  
Vol 56 (7) ◽  
pp. 1020-1025 ◽  
Author(s):  
Farid R. Ahmed ◽  
Angs Ng ◽  
Alex G. Fallis

Methanol extraction of the ground seeds of Uncaria Gambier Roxb. followed by chromatography afforded a crystalline C30H38O10 terpene. This has been shown by X-ray analysis to be 7α-acetoxydihydronomilin. The crystals are orthorhombic, P212121, a = 13.158(2), b = 17.092(2), c = 12.689(2) Å, Z = 4, dx = 1.300, do = 1.300 g cm−3. The structure has been determined by the direct method and Fourier syntheses, and refined by block-diagonal least-squares to R = 0.042 for 2621 observed reflexions. The molecule contains a seven-membered lactone ring A, three six-membered rings B, C, D, a three-membered ring E, a furan ring F, and two acetate groups. A and B are chair, C is twist-boat, D is 1,3-diplanar, while E and F are planar. The A/B, A/C, C/D junctions are trans, D/E is cis, and F is linked to D by an equatorial C—C bond. The two acetate groups are in axial positions on A and B and are cis to each other. The O atom forming the apex of the three-membered ring is wedged between two H atoms and their parent C atoms at short intramolecular distances O … H = 2.28(2) and 2.28(3), and O … C = 2.623(3) and 2.668(4) Å. No intermolecular hydrogen bonding is indicated.


2018 ◽  
Vol 73 (5) ◽  
pp. 281-288
Author(s):  
Qing Zhao ◽  
Ying-Qi Pan ◽  
Xiao-Yan Li ◽  
Han Zhang ◽  
Wen-Kui Dong

AbstractA discrete heterotrinuclear complex [{Ni2LDy(OAc)3(CH3OH)}2] · 2CH3OH · 3CH2Cl2, with a naphthalenediol-based acyclic bis(salamo) ligand H4L, has been synthesized and structurally characterized using elemental analyses, IR, UV/Vis and fluorescence spectra and single crystal X-ray diffraction. The crystal structure shows two crystallographically independent but chemically identical molecules (molecules I and II). All the Ni(II) atoms are hexa-coordinated with slightly distorted octahedral geometries. The central Dy atoms are nona-coordinated with slightly distorted tricapped trigonal prism geometries. An infinite 3D supramolecular structure is formed via intermolecular hydrogen bonding and C–H…π interactions.


2014 ◽  
Vol 70 (11) ◽  
pp. 1007-1010 ◽  
Author(s):  
Cristian Paz Robles ◽  
Viviana Burgos ◽  
Sebastián Suarez ◽  
Ricardo Baggio

The natural compound dendocarbin A, C15H22O3, is a sesquiterpene lactone isolated for the first time fromDrimys winterifor var chilensis. The compound crystallizes in the orthorhombic space groupP212121and its X-ray crystal structure confirmed theS/Rcharacter of the chiral centres at C-5/C-10 and C-9/C-11, respectively. The α-OH group at C-11 was found to be involved in intermolecular hydrogen bonding, defining chains along the <100> 21screw axis.


1993 ◽  
Vol 46 (7) ◽  
pp. 1093 ◽  
Author(s):  
TW Jackson ◽  
M Kojima ◽  
RM Lambrecht

The complexes oxo (1,1,8,8-tetraethyl-3,6-diazaoctane-1,8-dithiolato)rhenium[ ReO ( tedadt )], oxo (1,1,8,8-tetraethyl-4,4-dimethyl-3,6-diazaoctane-1,8-dithiolato)rhenium [ ReO ( tedmdadt )] and (1,1,4,4,8,8-hexamethyl-3,6-diazaoctane-1,8-dithiolato) oxorhenium [ ReO ( hmdadt )] were prepared. The crystal structure of the complex ReO ( tedadt ) was determined by X-ray crystallography to be a hydrogen-bonded dimer . This is the first example of intermolecular hydrogen bonding in rhenium diamino dithiolate ( dadt ) complexes.


1978 ◽  
Vol 33 (6) ◽  
pp. 588-589 ◽  
Author(s):  
Y. Sudhakara Babu ◽  
H. Manohar ◽  
K. Ramachandran ◽  
S. S. Krishnamurthy

Abstract An X-ray crystal structure analysis of tetrakis(dimethylamino)(ethylenediamino)cyclotriphosphazene reveals a novel spirocyclic structure with the spiro ring having an envelope conformation. There is evidence for an intermolecular N-H ··· N bond in the crystal which persists in solution


1989 ◽  
Vol 44 (3) ◽  
pp. 370-372 ◽  
Author(s):  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Petra Klinzing ◽  
Kurt Dehnicke

Di-trichloroacetimide, HN(COCCl3)2. was prepared by the reaction of trichloroacetic acid with trithiazylchloride at 60 °C. The compound was characterized by its IR spectrum as well as by an X-ray structure determination: Space group P 1, Z = 2, 1662 observed independent reflexions, R = 0.034. Lattice dimensions at 17 °C: a = 640.9(2); b = 924.1(3); c = 943.0(2) pm; α = 92.11(2)°; β = 106.53(3)°; γ = 99.02(3)°. The compound forms the Z,Z(trans-trans)isomer. There is no intermolecular hydrogen-bonding.


2021 ◽  
Vol 252 ◽  
pp. 02071
Author(s):  
Ying Liu ◽  
Haixing Liu

The novel Mn complex C24H18CrMnN4O5 was investigated by hydrothermal and its crystal structure was characterized using X-ray diffraction technology. The Mn atom is six coordinated by four N atom from two 1, 10-phenanthroline and two O atoms from CrO4-. The hydrogen bonding O-H...O had central effect for crystal stability.


2012 ◽  
Vol 557-559 ◽  
pp. 401-404
Author(s):  
Hai Xing Liu ◽  
Li Mei Wan ◽  
Qing Zhi Pan ◽  
Hui Juan Yue ◽  
Guang Zeng ◽  
...  

A novel Gadolinium complex Gd (C3O9H6) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Gd atom is coordinated by sixteen O atoms. The two-dimensional layered structure is formed and exhibits extensive O-H…O hydrogen-bonding interactions.


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