Synthesis, Structure and Spectroscopy of a New Polyiodide in the α,ω-Diazaniumalkane Iodide/Iodine System

2012 ◽  
Vol 67 (5) ◽  
pp. 447-451 ◽  
Author(s):  
Guido J. Reiss ◽  
Martin van Megen
Keyword(s):  
Raman Spectroscopy ◽  
Hydrogen Bonds ◽  
Excellent Agreement ◽  
Title Compound ◽  
Structural Parameters ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Spectroscopic Methods ◽  
Trans Conformation ◽  
X Ray

The reaction of 1,4-diaminobutane with hydroiodic acid in the presence of iodine yields the title compound 1,4-diazaniumbutane tetraiodide, C4H14N2I4 (1). The title compound has been structurally characterized by crystallographic and spectroscopic methods (Raman and IR). 1is built up by centrosymmetric 1,4-diazaniumbutane cations in all-trans conformation and linear I42- anions. Both, cations and anions are located on centers of inversion (2/m) in the monoclinic space group C2/m. The hydrogen bonds between the azanium groups and the terminal iodine atoms of the I42- anions lead to a three-dimensional framework. The structural parameters of the tetraiodide anion, derived from X-ray crystallographic data are in excellent agreement with the results from Raman spectroscopy. The Raman and IR data for the analogous a,w-diazaniumalkane tetraiodide salts (H3N-(CH2)6-NH3)I4 (2) and (H3N-(CH2)7-NH3)I4 (3) are reported, and the structures of 1, 2and 3are compared.

A new heteroleptic oxalate-based compound: poly[[2-(aminomethyl)pyridine]di-μ6-oxalato-chromium(III)potassium(I)]

2013 ◽  
Vol 70 (1) ◽  
pp. 12-15 ◽  
Author(s):  
Patrice Kenfack Tsobnang ◽  
Emmanuel Wenger ◽  
Siméon Ponou ◽  
Slimane Dahaoui ◽  
John Lambi Ngolui ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Hydrogen Bonding ◽  
Title Compound ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Ligands ◽  
Partial Overlap

The title compound, [KCr(C2O2)2(C6H8N2)]n, was obtained from aqueous solution and analyzed with single-crystal X-ray diffraction at 100 K. It crystallizes in the monoclinic space groupC2/cand displays a three-dimensional polymeric architecture built up by bimetallic oxalate-bridged CrIII–K helical chains linked through centrosymmetric K2O2units to yield a sheet-like alternatingP/Marrangement which looks like that of the previously described two-dimensional [NaCr(ox)2(pyim)(H2O)]·2H2O [pyim is 2-(pyridin-2-yl)imidazole; Leiet al.(2006).Inorg. Chem. Commun.9, 486–488]. The CrIIIions in each helix have the same chirality. The infinite neutral sheets are eclipsed with respect to each other and are held together by a hydrogen-bonding network involving 2-(aminomethyl)pyridine H atoms and oxalate O atoms. Each sheet gives rise to channels of Cr4K4octanuclear rings and each resultant hole is occupied by a pair of 2-(aminomethyl)pyridine ligands with partial overlap. The shortest Cr...Cr distance [5.593 (4) Å] is shorter than usually observed in the K–MIII–oxalate family.

scholarly journals 4-(4-Chlorophenyl)-4,5-dihydro-1H-1,2,4-triazole-5-thione

Molbank ◽  
10.3390/m1047 ◽  
2019 ◽  
Vol 2019 (1) ◽  
pp. M1047 ◽  
Author(s):  
Chien Yeo ◽  
Ainnul Azizan ◽  
Edward Tiekink
Keyword(s):  
Hydrogen Bonds ◽  
Structure Determination ◽  
Title Compound ◽  
Uv Spectroscopy ◽  
Three Dimensional ◽  
Membered Ring ◽  
X Ray ◽  
X Ray Crystallography ◽  
Orthogonal Relationship ◽  
Ir And Uv Spectroscopy

The title compound, 4-(4-chlorophenyl)-4,5-dihydro-1H-1,2,4-triazole-5-thione (1), was synthesized by a hetero-cyclization reaction of 4-chlorophenyl isothiocyanate and formic hydrazide. Compound 1 was characterized by a single-crystal X-ray structure determination as well as 1H and 13C{1H} NMR, IR, and UV spectroscopy, and microelemental analysis. X-ray crystallography on 1 confirms the molecule exists as the thione tautomer and shows the five-membered ring to be planar and to form a dihedral angle of 82.70(5)° with the appended chlorophenyl ring, indicating an almost orthogonal relationship. In the molecular packing, supramolecular dimers are formed via thioamide-N–H⋯S(thione) hydrogen bonds and these are connected by C=S⋯π(triazolyl) and C-Cl⋯π(triazolyl) interactions, leading to a three-dimensional architecture.

scholarly journals A new polymorph ofN-(2-{N′-[(1E)-2-hydroxybenzylidene]hydrazinecarbonyl}phenyl)benzamide

2014 ◽  
Vol 70 (6) ◽  
pp. o645-o646
Author(s):  
Shaaban K. Mohamed ◽  
Joel T. Mague ◽  
Mehmet Akkurt ◽  
Herman Potgieter ◽  
Mustafa R. Albayati
Keyword(s):  
Hydrogen Bonds ◽  
Benzene Ring ◽  
Title Compound ◽  
Phenyl Ring ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Monoclinic Space Group ◽  
Acta Cryst ◽  
Space Group ◽  
Compound C

The title compound, C21H17N3O3, is a new polymorph of an already published structure [Shashidharet al.(2006).Acta Cryst.E62, o4473–o4475]. The previously reported structure crystallizes in the monoclinic space groupC2/c, whereas the structure reported here is in the tetragonal space groupI41/a. The bond lengths and angles are similar in both structures. The molecule adopts an extended conformationviaintramolecular N—H...O and O—H...N hydrogen bonds; the terminal phenyl ring and the hydroxylphenyl ring are twisted with respect to the central benzene ring by 44.43 (7) and 21.99 (8)°, respectively. In the crystal, molecules are linked by N—H...O hydrogen bonds, weak C—H...O hydrogen bonds and weak C—H...π interactions into a three-dimensional supramolecular network.

catena-Poly[[nickel(II)-μ2-[1,3-bis(imidazol-1-ylmethyl)benzene-κ2N3:N3′]-μ2-(5-carboxybenzene-1,3-dicarboxylato-κ4O1,O1′:O3,O3′)] 0.41-hydrate]

2012 ◽  
Vol 68 (12) ◽  
pp. m336-m339 ◽  
Author(s):  
Xiao-Dan Wang ◽  
Guang-Feng Hou ◽  
Ying-Hui Yu ◽  
Jin-Sheng Gao
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Three Dimensional ◽  
Water Molecules ◽  
Triangular Prism ◽  
Supramolecular Framework ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray

The title compound, {[Ni(C9H4O6)(C14H14N4)]·0.41H2O}n, exhibits a three-dimensional hydrogen-bonded supramolecular framework. The NiIIcation is six-coordinated in a distorted triangular prism defined by two N atoms from two 1,3-bis(imidazol-l-ylmethyl)benzene (bix) ligands and four O atoms from two 5-carboxybenzene-1,3-dicarboxylate (HBTC) dianions. The bix molecules and HBTC dianions both act as bidentate ligands, linking the NiIIcations to form a one-dimensional coordination polymer. A two-dimensional wave-like net is constructed by O—H...O hydrogen bonds linking adjacent chains. Partially occupied solvent water molecules fill the cavities and link these layers to form a three-dimensional supramolecular structureviaO—H...O hydrogen bonds. The title compound was also characterized by powder X-ray diffraction and thermogravimetric analysis.

scholarly journals Structure of (E)-N-((5-Nitrothiophen-2-YL)Methylene)-3-(Trifluoromethyl)Aniline

2014 ◽  
Vol 70 (a1) ◽  
pp. C997-C997
Author(s):  
Özlem Deveci ◽  
Sümeyye Gümüş ◽  
Erbil Agˇar
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Density Functional ◽  
Theoretical Calculations ◽  
Molecular Geometry ◽  
Basis Set ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray

The Schiff base compound, C12H7N2O2F3S, has been synthesized and characterized by IR, UV-Vis, 1H-NMR, 13C-NMR and single-crystal X-ray diffraction (XRD) and elemental analysis. The compound, an Ortep-3 [1] view of which is shown in Fig. 1, crystallizes in the monoclinic space group P-1 with a= 7.5700(11) Å, b= 12.8280(16) Å, c= 13.0170(16) Å, α= 89.295(10)o, β= 88.691(11)o, γ= 82.246(11)o and Z=4 in the unit cell. The molecular structure is stabilized by C-H...O and C-H...F intramolecular hydrogen bonds and molecules are linked through intermolecular C-H...O and C-H...F type hydrogen bonds and C-H...Cg (π-ring) interaction. The molecular geometry from X-ray determination of the title compound in the ground state has been compared using the Hartre-Fock (HF) and density functional theory (DFT/B3LYP) [2] with 6-31G(d) [3] basis set. The results of the optimized molecular structure are exhibited and compared with the experimental X-ray diffraction. To determine conformational flexibility, molecular energy profile of the title compound was obtained by B3LYP with the 6-31G(d) basis set calculations with respect to selected degree of torsional freedom, which was varied from –1800to +1800in steps of 100. In addition, molecular electrostatic potential (MEP) distribution and frontier molecular orbitals (FMOs) properties of the title molecule were investigated by theoretical calculations at the B3LYP/6-31G (d) level. Figure 1. Ortep 3 diagram of the title compound. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.

scholarly journals Preparation and Characterization of bis (4-methoxyanilinium) tetrachlorozincate

2014 ◽  
Vol 10 (3) ◽  
pp. 2355-2362
Author(s):  
H. Rahmouni ◽  
W. Smirani Sta ◽  
M. Rzaigui
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Van Der Waals Interactions ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Organic Layers ◽  
Dimensional Network ◽  
Uv Visible

A new zinc complex of formula [C7H10NO]2 ZnCl4 has been prepared and characterized by X-ray diffraction,  IR and UV-Visible spectroscopies. The complex crystallizes in the monoclinic space group P21/n with a minimal tetrahedral distortion of the ZnCl42- ion and with lattice parameters: a =12.054 (2) Å, b =7.129 (3) Å, c =23.480 (2) Å, β = 100.67 (2)°, V = 1983.03 (1) Å3 and Z = 4. The crystal structure was solved and refined to R = 0.080 and RW = 0.227 with 9611 independent reflections. It can be described by organic layers of p-anisidinium cations held together by C-H…O hydrogen bonds parallel to (010) plane, linked to the inorganic groups of ZnCl42- anions through N-H…Cl hydrogen bonds, electrostatic and Van Der Waals interactions, to form a three-dimensional network.

Polysulfonylamine, CXLIII [1], Rolle schwacher Wasserstoffbrücken (C - H···O) in den Kristallstrukturen von 2,6-Dimethylpyridinium-, 1-Hydroxypyridinium- und Imidazolium-dimesylamid / Polysulfonylamines, CXLIII [1], Role of Weak Hydrogen Bonds (C - H···O) in the Crystal Structures of 2,6-Dimethylpyridinium , 1-Hydroxypyridinium and Imidazolium Dimesylamide

2001 ◽  
Vol 56 (10) ◽  
pp. 1052-1062 ◽  
Author(s):  
Oliver Moers ◽  
Karna Wijaya ◽  
Thomas Hamann ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Strong Hydrogen Bond ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Onium Salts ◽  
Weak Hydrogen Bonds ◽  
Normalized Parameters ◽  
Imidazolium Ion

In order to study hydrogen bonding networks in ionic crystals, low-temperature X-ray structures were determined for three onium salts of general formula BH+(MeSO2)2N- , where BH+ is 2,6-dimethylpyridinium (1; monoclinic, space group P21/c, Z′ = 1), 1-hydroxypyridinium (2; triclinic, P1̅, Z′ = 1), or imidazolium (3; monoclinic, Cc, Z′ = 1). The asymmetric units consist of cation-anion pairs assembled in 1 and 3 by ordinary N+ - H···N hydrogen bonds, in 2 by a very short N+ - O - H···N- bond belonging to the class (+/-)CAHB [H···O 148(3), O···N 253.5(2) pm, O - H···N 175(3)°]. The second N -H donor of the imidazolium ion is involved in a nearly symmetric N - H (···O)2 three-centre bond to two different anions. In the pyridine derivatives, the (MeSO2 )2N- ions are associated via short C(sp3) - H···O contacts to form a three-dimensional framework of corrugated and cross-linked layers (1) or an assembly of discrete corrugated layers (2). As a common feature, these anion substructures are pervaded by hexagonal channels parallel to x, each one accommodating two stacks of cations that are linked to the channel walls by the unique strong hydrogen bond and a set of short Car - H···O contacts; moreover, cations drawn from adjacent stacks in structure 2 create inversion-symmetric dimers based upon a short Car - H···O(H) - N interaction. In contrast, the structure of 3 displays planar anion layers assembled by short C(sp3 ) - H···O contacts, intercalating the cations with their ring planes perpendicular to the layer planes and binding them by means of the strong hydrogen bonds and three Car -H···O interactions. All C - H···O taken into consideration have normalized parameters d( H···O) ≤ 267 pm and θ(C - H···O) ≥ 121°.

The protonation of the ethylenediphosphinetetraacetate anion and the crystal structure of the bis (hydrogen bromide) of ethylenediphosphinetetraacetic acid

1981 ◽  
Vol 46 (12) ◽  
pp. 3063-3073 ◽  
Author(s):  
Jana Podlahová ◽  
Bohumil Kratochvíl ◽  
Vratislav Langer ◽  
Josef Šilha ◽  
Jaroslav Podlaha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Free Acid ◽  
Hydrogen Bromide ◽  
Carboxyl Groups ◽  
Spectroscopic Methods ◽  
X Ray ◽  
Partial Formation

The equilibria and mechanism of addition of protons to the ethylenediphosphinetetraacetate anion (L4-) were studied in solution by the UV, IR, 1H and 31P NMR spectroscopic methods. A total of six protons can be bonded to the anion. They are added stepwise, first with partial formation of zwitterions containing P-H bonds, which then dissociate with formation of the free acid, H4L, where all four protons are bonded in carboxyl groups. The formation of zwitterions is strongly dependent on the concentration. In the final stage, the acid bonds two additional protons to form the bis-phosphonium cation, H6L2+. A number of isostructural salts containing this cation, H4L.2 HX (X = Cl, Br, I), have been prepared. The X-ray crystal structure determination of the bromide confirmed the expected arrangement. The bromide crystals are monoclinic, a = 578.2, b = 1 425.0, c = 1 046.7 pm, β = 103.07° with a space group of P21/c, Z = 2. The final R factor was 0.059 based on 1 109 observed reflections. The structure consists of H6L2+ cations containing protons bonded to phosphorus atoms (P-H distance 134 pm) and of bromide anions, located in gaps which are also sufficiently large for I- anions in the isostructural iodide. The interbonding of phosphonium cations proceeds through hydrogen bonds, C-OH...O=C, in which the O...O distance is 275.3 pm.

scholarly journals Powder study of 3-azabicyclo[3.3.1]nonane-2,4-dione form 2

2006 ◽  
Vol 62 (7) ◽  
pp. o3046-o3048 ◽  
Author(s):  
Ashley T Hulme ◽  
Philippe Fernandes ◽  
Alastair Florence ◽  
Andrea Johnston ◽  
Kenneth Shankland
Keyword(s):  
Crystal Structure ◽  
Simulated Annealing ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Title Compound ◽  
Variable Temperature ◽  
Polycrystalline Sample ◽  
Asymmetric Unit ◽  
X Ray ◽  
Compound C

A polycrystalline sample of a new polymorph of the title compound, C8H11NO2, was produced during a variable-temperature X-ray powder diffraction study. The crystal structure was solved at 1.67 Å resolution by simulated annealing from laboratory powder data collected at 250 K. Subsequent Rietveld refinement yielded an R wp of 0.070 to 1.54 Å resolution. The structure contains two molecules in the asymmetric unit, which form a C 2 2(8) chain motif via N—H...O hydrogen bonds.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

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