The addition of 2,4-dinitrobenzenesulphenyl chloride to 2-methylenebicyclo[2.2.1]hept-5-ene: the crystal structure of 1-chloromethyl-3-endo-(2′,4′-dinitrophenylthio)tricyclo[2.2.1.02,6]heptane, C14H13ClN2O4S

1981 ◽  
Vol 59 (4) ◽  
pp. 658-662 ◽  
Author(s):  
Maria Przybylska ◽  
Dennis G. Garratt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Double Bond ◽  
Structural Data ◽  
Sulphur Atom ◽  
Hydrogen Bond System ◽  
Cell Dimensions ◽  
Bond System ◽  
Bifurcated Hydrogen Bond ◽  
Unit Cell Dimensions

1-Chloromethyl-3-endo-(2′,4′-dinitrophenylthio)tricyclo[2.2.1.02,6]heptane, C14H13ClN2O4S, crystallizes in space group P21/a with unit cell dimensions a = 12.785(2), b = 10.653(1), c = 11.061(1) Å, β = 101.54(l)° Z = 4.The structure was solved from Patterson and Fourier maps. The parameters were refined by block-diagonal least-squares to a final R = 0.038 for 2063 observed reflections. The structural data provide unequivocal proof for our earlier ascertainment of configurational-specific exo attack upon the endocyclic double bond of 2-methylenebicyclo[2.2.1]hept-5-ene with homoallylic participation.The molecule is characterized by the presence of an interaction between oxygen of the 2-nitro group and a sulphur atom, and of a weak bifurcated hydrogen bond system involving [Formula: see text] bonds.

Pyridine 1:1 adducts of urea (Z′ = 1) and thiourea (Z′ = 8)

2018 ◽  
Vol 74 (4) ◽  
pp. 406-410 ◽  
Author(s):  
Mark Strey ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Layer Structure ◽  
Urea Adduct ◽  
Standard Type ◽  
Space Group ◽  
Hydrogen Bond System ◽  
Bond System ◽  
Bifurcated Hydrogen Bond ◽  
Urea Adducts

During our studies of urea and thiourea adducts, we noticed that no adducts with unsubstituted pyridine had been structurally investigated. The 1:1 adduct of pyridine and urea, C5H5N·CH4N2O, crystallizes in the P21/c space group with Z = 4. The structure is of a standard type for urea adducts, whereby the urea molecules form a ribbon, parallel to the a axis, consisting of linked R 2 2(8) rings, and the pyridine molecules are attached to the periphery of the ribbon by bifurcated (N—H...)2N hydrogen bonds. The 1:1 adduct of pyridine and thiourea, C5H5N·CH4N2S, crystallizes in the P21/n space group, with Z = 32 (Z′ = 8). The structure displays similar ribbons to those of the urea adduct. There are two independent ribbons parallel to the b axis at z ≃ 0 and 1 \over 2, and three at z ≃ 1 \over 4 and 3 \over 4; the latter are crosslinked to form a layer structure by additional long N—H...S interactions, which each formally replace one branch of a bifurcated hydrogen-bond system.

scholarly journals Nickel alendronate

2012 ◽  
Vol 68 (6) ◽  
pp. m820-m821 ◽  
Author(s):  
Małgorzata Sikorska ◽  
Maria Gazda ◽  
Jaroslaw Chojnacki
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Title Compound ◽  
Intermolecular Hydrogen Bond ◽  
Hydrothermal Conditions ◽  
Complex Molecules ◽  
Hydrogen Bond System ◽  
Bond System

The title compound {systematic name: bis(μ2-dihydrogen 4-azaniumyl-1-hydroxybutane-1,1-diphosphonato)bis[aqua(dihydrogen 4-azaniumyl-1-hydroxybutane-1,1-diphosphonato)nickel(II)] dihydrate}, [Ni2(C4H12NO7P2)4(H2O)2]·2H2O, was synthesiized under hydrothermal conditions. Its structure is isotypic with the CoII analogue. The crystal structure is built up from centrosymmetric dinuclear complex molecules and the structure is reinforced by a net of intermolecular O—H...O and N—H...O hydrogen bonds. One water molecule is bound to the NiII atom in the octahedral coordination sphere, while the second is part of the intermolecular hydrogen-bond system.

Crystal structure of a synthetic aluminoan tantalian titanite: a reconnaissance study

2006 ◽  
Vol 70 (1) ◽  
pp. 115-121 ◽  
Author(s):  
R. P. Liferovich ◽  
R. H. Mitchell
Keyword(s):  
Crystal Structure ◽  
Structural Data ◽  
Rietveld Analysis ◽  
Synthetic Analogue ◽  
X Ray Diffraction ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Ceramic Synthesis ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

AbstractA synthetic analogue, Ca(Ti0.6Al0.2Ta0.16Nb0.04)OSiO4, of an aluminoan tantalian titanite previously described from Craveggia pegmatite (Piemonte, Italy) has been prepared by a ceramic synthesis technique and its crystal structure determined by Rietveld analysis of the powder X-ray diffraction pattern. The synthetic Al-Ta-Nb-rich titanite adopts space group A2/a implying that substitutions at the single octahedral site destroy the coherence of the off-centering of octahedral chains in the titanite structure resulting in a P21/a → A2/a phase transition. Unit-cell dimensions obtained for the Al-Ta-Nb-rich titanite are: a = 7.0649(1) Å; b = 8.7187(1) Å; c = 6.5701(1) Å; β = 113.755(1)°, V = 370.41(1) Å3. The extensive replacement of Ti by Al, Ta and Nb results in a considerable decrease in the distortion of all coordination polyhedra in the structure of this titanite. These structural data suggest that a solid solution CaTi1-x(Alx/2 [Ta,Nb]x/2)OSiO4 (0 ≤ x ≤ 0.4) adopting the titanite structure might exist.

Electrophilic cleavage of cyclopropanes. IV. The reaction of 2-nitrobenzenesulphenyl chloride with tetracyclo[3.2.0.02,7.04,6]heptane in methanol and acetic acid: the crystal structure of exo-3-(2′-nitrophenylthio)-exo-5-methoxytricyclo[2.2.1.02,6]heptane, C14H15NO3S

1983 ◽  
Vol 61 (6) ◽  
pp. 1176-1184 ◽  
Author(s):  
Dennis G. Garratt ◽  
Maria Przybylska ◽  
Miroslaw Cygler
Keyword(s):  
Crystal Structure ◽  
Acetic Acid ◽  
Ring Opening ◽  
Sulphur Atom ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Unambiguous Assignment ◽  
Made In ◽  
C Nmr

The electrophilic cleavage of a cyclopropane single bond in tetracyclo[3.2.0.02,7.04,6]heptane by 2-nitrobenzenesulphenyl chloride in methanol and acetic acid has been studied using both nmr and single crystal X-ray structural determination techniques. The orientation of ring opening has been shown to be inversion as a result of electrophilic corner attack. The crystal structure of one adduct allowed the unambiguous assignment of exo-3-(2′-nitrophenylthio)-exo-5-methoxytricyclo [2.2.1.02,6]-heptane, C14H15NO3S. This species crystallizes in space group P21/a with unit cell dimensions a = 10.633(1), b = 13.637(1), c = 9.938(1) Å, β = 115.36(1)°, Z = 4. The structure was solved by MULTAN 78. The parameters were refined by block-diagonal least squares to a final R = 0.039 for 2445 observed reflections. Of particular interest is an interaction between the sulphur atom and the oxygen atom of the nitro group with an [Formula: see text] distance of 2.694(2) Å and [Formula: see text]. The data presented in this paper show errors in previous assignments based on 13C nmr spectroscopy made in this laboratory and indicate the danger of basing assignments of configuration in nortricyclenes entirely upon this technique.

scholarly journals Isomorphous Crystals Formed by the Similar Supramolecular Motifs in Sorafenib Hydrochloride and Regorafenib Hydrochloride Salts

Crystals ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 649 ◽  
Author(s):  
Chi Uyen Phan ◽  
Jie Shen ◽  
Jiyong Liu ◽  
Jianming Mao ◽  
Xiurong Hu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Crystal Structures ◽  
Pyridinium Cation ◽  
Supramolecular Motifs ◽  
Solubility Profile ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Similar Unit ◽  
Similar Crystal Structure

Sorafenib and regorafenib (or fluoro-sorafenib) are multikinase inhibitors active in the treatment of various human cancers, but their solubilities are very poor. To improve their solubilities, in this study, sorafenib hydrochloride (Sor·HCl, I) and regorafenib hydrochloride (Reg·HCl, II) have been prepared and their crystal structures were characterized. Their solubility properties in water were evaluated. Intriguingly, they are isomorphous crystal structures with the same space group and the similar unit cell dimensions, which were caused by the similar supramolecular patterns resulted by the formation of N–H···Cl− hydrogen bond instead of hydrogen bond between the protonated pyridinium cation and counterion. Moreover, the solubility properties displayed identical profiles. It may be concluded that a similar crystal structure leads to a comparable solubility profile.

Zur Kenntnis von Calciumtetrahydrogen-hexaoxo-diperiodattetrahydrat CaH4I2O10 · 4 H2O: Kristallstruktur, Schwingungsspektren und thermische Analyse / On Calciumtetrahydrogen-hexaoxo-diperiodatetetrahydrate CaH4I2O10 · 4 H2O: Crystal Structure, Vibrational Spectroscopy and Thermal Analysis

2002 ◽  
Vol 57 (12) ◽  
pp. 1337-1345 ◽  
Author(s):  
H. Haeuseler ◽  
M. Botova
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Aqueous Solution ◽  
Hydrogen Bond ◽  
Acidic Aqueous Solution ◽  
Oh Groups ◽  
Edge Sharing Octahedra ◽  
Hydrogen Bond System ◽  
Bond System ◽  
Ir And Raman

By crystallisation from a strongly acidic aqueous solution calciumtetrahydrogen-hexaoxo-diperiodatetetrahydrate CaH4I2O10 ∙ 4 H2O has been obtained. In the structure of this compound (S.G. C2/c, Nr. 15), Z = 4, a = 1986,6(4), b = 564,2(1), c = 1149,4(20) pm, β = 120,62(3)°) centrosymmetric H4I2O102− anions in the form of edge-sharing octahedra form layers via hydrogen bonds originating from the acidic, trans-configurated OH groups of the anions. IR and Raman spectra are analysed with respect to the hydrogen bond system and the internal vibrations of the periodate anion. The dehydration of the compound takes place via Ca(IO4)2 ∙ 5 H2O and Ca(IO4)2 ∙2H2O leading at 143°C to the anhydrous metaperiodate Ca(IO4)2 which decomposes above 248°C to Ca(IO3)2.

Structure refinement, hydrogen-bond system and vibrational spectroscopy of hohmannite, Fe3+2[O(SO4)2]·8H2O

2015 ◽  
Vol 79 (1) ◽  
pp. 11-24 ◽  
Author(s):  
G. Ventruti ◽  
G. Della Ventura ◽  
R. Orlando ◽  
F. Scordari
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Vibrational Spectroscopy ◽  
Structural Model ◽  
Structure Refinement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bond System ◽  
Bond System ◽  
First Time

AbstractThe crystal structure of hohmannite, Fe3+2[O(SO4)2]·8H2O, was studied by means of single-crystal X-ray diffraction (XRD) and vibrational spectroscopy. The previous structural model was confirmed, though new diffraction data allowed the hydrogen-bond system to be described in greater and more accurate detail.Ab initiocalculations were performed in order to determine accurate H positions and to support the experimental model obtained from XRD data. Infrared and Raman spectra are presented for the first time for this compound and comments are made on the basis of the crystal structure and the known literature for sulfate minerals.

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