The correlation between O—H stretching frequencies and hydrogen bond distances in a crystalline sugar monohydrate

1979 ◽  
Vol 57 (19) ◽  
pp. 2640-2645 ◽  
Author(s):  
J. Umemura ◽  
G. I. Birnbaum ◽  
D. R. Bundle ◽  
W. F. Murphy ◽  
H. J. Bernstein ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Infrared Spectra ◽  
Room Temperature ◽  
Isotopic Dilution ◽  
X Ray

The Raman and infrared spectra of crystalline methyl 3,6-dideoxy-β-D-ribo-hexopyranoside monohydrate in the O—H stretching region have been studied at room temperature and lower temperatures. Four bands have been identified and correlated with the corresponding O … O distances of the four distinct hydrogen bonds obtained from X-ray data. The assignments were substantiated by a deuterium isotopic dilution study.

Synthesis and Structural Characterisation of New Bifunctional o-Hydroxyacetophenones – Potential Linker Molecules for Coordinative Framework Construction

2013 ◽  
Vol 68 (3) ◽  
pp. 214-222 ◽  
Author(s):  
Jörg Hübscher ◽  
Michael Günthel ◽  
Robert Rosin ◽  
Wilhelm Seichter ◽  
Florian Mertens ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
X Ray ◽  
Structural Characterisation ◽  
Crystallographic Study ◽  
Copper Coordination ◽  
Resonance Assisted Hydrogen Bond ◽  
Intramolecular Hydrogen ◽  
Fitting In ◽  
Linker Molecules

Two new linker-type molecules 1a and 1b composed of o-hydroxyacetophenone coordinative groups attached to linear ethynylene or 1,4-phenylenediethynylene spacer units have been synthesised and structurally characterised. An X-ray crystallographic study for both compounds has shown structures with strong intramolecular hydrogen bonds fitting in the model of ‘Intramolecular Resonance Assisted Hydrogen Bond (IRHAB)’. Initial coordination experiments with Cu(II) were performed and the resulting materials characterised by PXRD. The similarity of the copper coordination between these compounds and copper(II) acetylacetonate complexes was demonstrated by XPS measurements. Based on the evidence of these studies, and on elemental analysis, the formation of the corresponding coordination polymers comprising Cu(II) and the linkers has been proposed

Infrared spectra of the ammonium ion in crystals. Part VIII. Spectroscopic criteria of highly-bent hydrogen bonds

1980 ◽  
Vol 58 (9) ◽  
pp. 867-874 ◽  
Author(s):  
Osvald Knop ◽  
Wolfgang J. Westerhaus ◽  
Michael Falk
Keyword(s):  
Low Temperature ◽  
Hydrogen Bonds ◽  
Infrared Spectra ◽  
Room Temperature ◽  
Ammonium Ion ◽  
Temperature Transition ◽  
Increasing Temperature

Available evidence suggests that (1) the stretching frequencies of highly-bent hydrogen bonds decrease with increasing temperature, regardless of whether the bonds are static or dynamic in character, to a single acceptor or to several competing acceptors; and (2) departures from symmetric trifurcation (or bifurcation) toward asymmetric situations lower the stretching frequency. In further support of these criteria isotopic probe ion spectra between 10 K and room temperature have been obtained for taurine and for trigonal (NH4)2MF6 (M = Si, Ge, Sn, Ti). Evidence of a low-temperature transition at 100(10) K in trigonal (NH4)2SnF6 is presented, and existence of the previously reported transition at 38.6 K in trigonal (NH4)2SiF6 is confirmed. Symmetry changes associated with these transitions are discussed.

scholarly journals INFRARED SPECTRA OF THIOSACCHARINATES OF CADMIUM AND LEAD COMPARISON WITH THE ANALOGOUS METAL SACCHARINATES

2017 ◽  
Vol 27 (1-2) ◽  
Author(s):  
Gligor Jovanovski ◽  
Adnan Kahil ◽  
Orhideja Grupče
Keyword(s):  
Infrared Spectra ◽  
Room Temperature ◽  
Spectral Characteristics ◽  
Crystalline Hydrate ◽  
Water Molecules ◽  
X Ray ◽  
Weak Hydrogen Bonds ◽  
Deuterated Analogue ◽  
The Fourier Transform ◽  
Cadmium And Lead

A b s t r a c t: The Fourier transform (FT) infrared spectra of thiosaccharinates of cadmium and lead in the 4000–400 cm–1 region were studied. Although the observed resemblance between the spectra recorded in KBr pellets suggests a possible similarity between their structures as well, the powder X-ray diagrams show that these two compounds are not isomorphous. The presence of broad and intense bands in the region of the HOH stretchings shows that thiosaccharinate of cadmium is a crystalline hydrate and the spectral picture in the region of the O-D stretchings of the isotopically isolated HOD molecules in the partially deuterated analogue indicates that present in its structure are at least two types of crystallographically different water molecules involved in the formation of weak hydrogen bonds. The room temperature (RT) spectrum of lead thiosaccharinate in the region of the ν(HOH) modes differs significantly from the spectrum recorded at the boiling temperature of liquid nitrogen (LNT), which may perhaps be interpreted as an indication that a phase transition is taking place on lowering the temperature. The spectrum of lead thiosaccharinate was recorded in a Nujol mull as well. While the KBr and Nujol spectra are essentially identical in the region below 1600 cm–1, no bands are observed in the HOH stretching region of the mull spectra. In fact, it was shown that the appearance of the spectra of lead thiosaccharinates depends on the emulsion preparation rate. A comparison of the spectral characteristics of the thiosaccharinates of cadmium and lead with those of the corresponding saccharinates (their crystal structures are known) was made, special attention being paid to the analysis of the SO2 stretching region in the saccharinate and thiosaccharinate compounds.

Crystal Structures of Seven Terephthaldiamide Derivatives

2002 ◽  
Vol 57 (8) ◽  
pp. 914-921 ◽  
Author(s):  
P. G. Jones ◽  
J. Ossowski ◽  
P. Kus
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Layer Structure ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
X Ray ◽  
Layer Structures ◽  
Structure Determinations ◽  
Independent Molecules

N,N′-Dibutyl-terephthaldiamide (1), N,N′-dihexyl-terephthaldiamide (2), N,N′-di(tert-butyl)- terephthaldiamide (3), N,N,N′,N′-tetrabutyl-terephthaldiamide (4), 1,1′-terephthaloylbis- pyrrolidine (5), 1,1′-terephthaloyl-bis-piperidine (6), and 4,4′-terephthaloyl-bis-morpholine (7) have been synthesised and physicochemically characterised. The X-ray structure determinations reveal imposed inversion symmetry for compounds 1-6; compound 3 has two independent molecules with inversion symmetry in the asymmetric unit. Compounds 1-3 form classical hydrogen bonds of the type N-H···O=C, leading to a ribbon-like arrangement of molecules (1 and 2) or a layer structure (3). Compound 3 also displays a very short C-H···O interaction, a type of hydrogen bond that is also observed in compounds 4-7, which lack classical donors; thereby compounds 4-6 form layer structures and 7 a complex threedimensional network.

scholarly journals 1-[N-Methyl-N-(Phenyl)amino]-3- (4-Methylphenyl)Thiourea

Molbank ◽  
10.3390/m1052 ◽  
2019 ◽  
Vol 2019 (1) ◽  
pp. M1052 ◽  
Author(s):  
Chien Yeo ◽  
Edward Tiekink
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Title Compound ◽  
Molecular Conformation ◽  
Phenyl Hydrazine ◽  
X Ray ◽  
X Ray Crystallography

The title compound, 1-[N-methyl-N-(phenyl)amino]-3-(4-methylphenyl)thiourea (1), was synthesized by the reaction of 1-methyl-1-phenyl hydrazine and 4-tolyl isothiocyanate, and was characterized by spectroscopy (1H and 13C{1H} NMR, IR, and UV), elemental analysis as well as by single crystal X-ray crystallography. In the solid state, the molecule exists as the thioamide tautomer and features an anti-disposition of the thioamide–N–H atoms; an intramolecular N–H⋯N hydrogen bond is noted. The molecular conformation resembles that of the letter L. In the molecular packing, thioamide-N1–H⋯S1(thione) hydrogen bonds lead to centrosymmetric eight-membered {⋯HNCS}2 synthons. The dimers are assembled into a supramolecular layer in the bc-plane by phenyl- and methyl-C–H⋯π(phenyl) interactions.

X-ray Diffraction Studies of Solid Solutions of Pentaglycerine-Neopentylglycol

1988 ◽  
Vol 32 ◽  
pp. 609-616 ◽  
Author(s):  
D. Chandra ◽  
C. S. Barrett ◽  
D. K. Benson
Keyword(s):  
Crystal Structure ◽  
Energy Storage ◽  
Hydrogen Bonds ◽  
Solid Solutions ◽  
Room Temperature ◽  
Energy Storage Materials ◽  
Anisotropic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cubic Structure

AbstractAn array of molecules that is anisotropic in the extreme has been discovered in certain thermal-energy storage materials and is reported here: neopentylglycol (NPG) and NPG-rich solid solutions with pentaglycerine (PG) have a crystal structure, stable at room temperature, that consists of bimolecular chains of molecules that are all unidirectionally aligned throughout a crystal. There are hydrogen bonds between every molecule in one chain and its neighbors in that chain, but none between molecules of one chain and any molecules of the neighboring parallel chains. Thus there are strong intermolecular bonds along each chain and only weaker bonds between the chains. The structure has been determined by using modern single crystal techniques with 529 independent reflections from a crystal of NPG (C5H12O2). The structure is monoclinic with space group P21/c - C2h5. This anisotropic structure transforms to a cubic structure at higher temperatures.

M3+(H2AsO4)(H2As2O7) (M3+= Al, Ga) and In2(H2AsO4)2(H2As2O7)2: a new layer structure type and a new framework structure type containing the rare H2As2O72−group

2017 ◽  
Vol 73 (8) ◽  
pp. 600-608 ◽  
Author(s):  
Karolina Schwendtner ◽  
Uwe Kolitsch
Keyword(s):  
Hydrogen Bonds ◽  
Room Temperature ◽  
Layer Structure ◽  
Structure Type ◽  
Three Dimensions ◽  
Framework Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Third ◽  
New Framework

The crystal structures of hydrothermally synthesized aluminium dihydrogen arsenate(V) dihydrogen diarsenate(V), Al(H2AsO4)(H2As2O7), gallium dihydrogen arsenate(V) dihydrogen diarsenate(V), Ga(H2AsO4)(H2As2O7), and diindium bis[dihydrogen arsenate(V)] bis[dihydrogen diarsenate(V)], In2(H2AsO4)2(H2As2O7)2, were determined from single-crystal X-ray diffraction data collected at room temperature. The first two compounds are representatives of a novel sheet structure type, whereas the third compound crystallizes in a novel framework structure. In all three structures, the basic building units areM3+O6octahedra (M= Al, Ga, In) that are connectedviaone H2AsO4−and two H2As2O72−groups into chains, and furtherviaH2As2O72−groups into layers. In Al/Ga(H2AsO4)(H2As2O7), these layers are interconnected by weak-to-medium–strong hydrogen bonds. In In2(H2AsO4)2(H2As2O7)2, the H2As2O72−groups link the chains in three dimensions, thus creating a framework topology, which is reinforced by weak-to-medium–strong hydrogen bonds. The three title arsenates represent the first compounds containing both H2AsO4−and H2As2O72−groups.

Studies on the Nature and Strength of Pt . . .H(-N) Interactions. The Crystal Structures of Chloro[N-(2-aminoethyl)-N-(2-ammonioethyl)ethane-1,2-diamine]platinum(II) Chloride and Dichloro[4,7-diaza-1-azoniacyclononane]platinum(II) Tetrachlor

2000 ◽  
Vol 53 (6) ◽  
pp. 451 ◽  
Author(s):  
Murray S. Davies ◽  
Ronald R. Fenton ◽  
Fazlul Huq ◽  
Edwina C. H. Ling ◽  
Trevor W. Hambley
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Molecular Mechanics ◽  
Metal Ion ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Protonated Amine ◽  
Protonated Amines ◽  
Close Contacts

Two complexes, namely, chloro[N-(2-aminoethyl)-N-(2-ammonioethyl)ethane-1,2-diamine]platinum(II) chloride {[PtCl(tren+H)]Cl2} and dichloro[4,7-diaza-1-azoniacyclononane]platinum(II) tetrachloroplatinate(II)–water (1/2) {[PtCl2(tacn+H)]2[PtCl4]·2H2O}, have been prepared and structurally characterized by single-crystal X-ray diffractometry as part of a study of the nature and strength of Pt···H(–N) interactions. Crystals of [PtCl(tren+H)]Cl2 are monoclinic, space group P21/c, a 8.293(2), b 14.396(6), c 11.305(3) Å, β 107.34(2)º, Z 4, and the structure has been refined to a residual of 0.042 based on 1631 reflections. Crystals of [PtCl2(tacn+H)]2[PtCl4]·2H2O are monoclinic, space group P21/a, a 12.834(4), b 8.206(4), c 13.116(8) Å, β 93.01(4)˚, Z 2, and the structure has been refined to a residual of 0.035 based on 1974 reflections. In [PtCl(tren+H)]2+, the protonated amine forms hydrogen bonds with chloride anions and no close contacts with the metal ion. In [PtCl2(tacn+H)]+, a short intramolecular contact is observed between the metal and the protonated amine and the results of molecular mechanics modelling are consistent with there being a Pt···H hydrogen bond. Molecular mechanics modelling of [PtCl(tren+H)]2+ and [PtCl2(dien+H)]+ shows that the protonated amines could readily form close contacts with the metal. It is concluded that there is evidence for the formation of Pt···H(–N) hydrogen bonds but these bonds are very weak, being similar or lower in energy than Cl···H(–NPt) hydrogen bonds.

scholarly journals The caesium phosphates Cs3(H1.5PO4)2(H2O)2, Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3

2020 ◽  
Vol 151 (9) ◽  
pp. 1317-1328
Author(s):  
Matthias Weil ◽  
Berthold Stöger
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Diffraction Data ◽  
Room Temperature ◽  
Structure Type ◽  
Solid State Reactions ◽  
X Ray Diffraction ◽  
Hydrogen Phosphate ◽  
X Ray

Abstract The caesium phosphates Cs3(H1.5PO4)2(H2O)2 and Cs3(H1.5PO4)2 were obtained from aqueous solutions, and Cs4P2O7(H2O)4 and CsPO3 from solid state reactions, respectively. Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3 were fully structurally characterized for the first time on basis of single-crystal X-ray diffraction data recorded at − 173 °C. Monoclinic Cs3(H1.5PO4)2 (Z = 2, C2/m) represents a new structure type and comprises hydrogen phosphate groups involved in the formation of a strong non-symmetrical hydrogen bond (accompanied by a disordered H atom over a twofold rotation axis) and a very strong symmetric hydrogen bond (with the H atom situated on an inversion centre) with symmetry-related neighbouring anions. Triclinic Cs4P2O7(H2O)4 (Z = 2, P$$\bar{1}$$ 1 ¯ ) crystallizes also in a new structure type and is represented by a diphosphate group with a P–O–P bridging angle of 128.5°. Although H atoms of the water molecules were not modelled, O···O distances point to hydrogen bonds of medium strengths in the crystal structure. CsPO3 is monoclinic (Z = 4, P21/n) and belongs to the family of catena-polyphosphates (MPO3)n with a repetition period of 2. It is isotypic with the room-temperature modification of RbPO3. The crystal structure of Cs3(H1.5PO4)2(H2O)2 was re-evaluated on the basis of single-crystal X-ray diffraction data at − 173 °C, revealing that two adjacent hydrogen phosphate anions are connected by a very strong and non-symmetrical hydrogen bond, in contrast to the previously described symmetrical bonding situation derived from room temperature X-ray diffraction data. In the four title crystal structures, coordination numbers of the caesium cations range from 7 to 12. Graphic abstract

scholarly journals Engineering short, strong hydrogen bonds in urea di-carboxylic acid complexes

CrystEngComm ◽  
2014 ◽  
Vol 16 (35) ◽  
pp. 8177-8184 ◽  
Author(s):  
Andrew O. F. Jones ◽  
Charlotte K. Leech ◽  
Garry J. McIntyre ◽  
Chick C. Wilson ◽  
Lynne H. Thomas
Keyword(s):  
Hydrogen Bond ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Neutron Diffraction ◽  
Structural Changes ◽  
Acid Amide ◽  
Molecular Complexes ◽  
Temperature Dependent ◽  
X Ray ◽  
Methyl Substitution

The persistence of the acid⋯amide heterodimer and the effect of methyl substitution on the short strong O–H⋯O hydrogen bond is investigated in urea and methylurea di-carboxylic acid molecular complexes. Temperature dependent structural changes are also reported utilising X-ray and neutron diffraction in tandem.

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