scholarly journals Redetermination of the structure of 2-amino-8-thia-1,5-diazaspiro[4,5]dec-1-en-5-ium chloride monohydrate

2022 ◽  
Vol 78 (2) ◽  
Author(s):  
Lyudmila A. Kayukova ◽  
Elmira M. Yergaliyeva ◽  
Anna V. Vologzhanina
Keyword(s):  
Room Temperature ◽  
Water Molecules ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tosyl Chloride ◽  
Hydrated Salt ◽  
Physicochemical Methods ◽  
Amine Groups ◽  
Chloride Monohydrate

The reaction of β-(thiomorpholin-1-yl)propioamidoxime with tosyl chloride in CHCl3 in the presence of DIPEA when heated at 343 K for 8 h afforded the title hydrated salt, C7H14N3S+·Cl−·H2O, in 84% yield. This course of the tosylation reaction differs from the result of tosylation obtained for this substrate at room temperature, when only 2-amino-8-thia-1,5-diazaspiro[4.5]dec-1-ene-5-ammonium tosylate was isolated in 56% yield. The structure of the reaction product was established by physicochemical methods, spectroscopy, and X-ray diffraction. The single-crystal data demonstrated that the previously reported crystal structure of this compound [Kayukova et al. (2021). Chem. J. Kaz, 74, 21–31] had been refined in a wrong space group. In the extended structure, the chloride anions, water molecules and amine groups of the cations form two-periodic hydrogen-bonded networks with the fes topology.

scholarly journals The Isomorphous Structures of Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)cobaltate(III) and Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)rhodate(III): Extended Metaloximate Chains with a Novel ···I–M–I···I–M–I··· Zigzagged Structure

1990 ◽  
Vol 45 (11) ◽  
pp. 1508-1512 ◽  
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Ammonium Salts ◽  
Monoclinic Space Group ◽  
Hydroxyl Groups ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anionic Complexes ◽  
Complex Anions

The ammonium salts of the complex anions trans-diiodobis(ethanedial-dioximato)-cobaltate(III), [Col2(GH)2]-, and trans-diiodobis(ethanedial-dioximato)rhodate(III), [RhI2(GH)2]- (GH- = ethanedial dioximate or glyoximate), have been synthesized and their structures determined from single crystal X-ray diffraction data at room temperature. The crystals of the two salts are monoclinic, space group C2/c. NH4[CoI2(GH)2] (I) crystallizes as dark-brown prisms with a greenish reflectance; its crystal data are: C4H10Col2N5O4, Mr = 504.90; a = 8.910(6), b = 11.700(9), c = 11.691(6) Å; β = 93.55(5)°; V = 1216.4 Å3; Z = 4; Dc = 2.78 Mg m-3. NH4[RhI2(GH)2] (II) crystallizes as yellow-brown blocks with crystal data: C4H10I2N5O4Rh, Mr = 548.88; a = 9.038(4), b = 11.949(5), c = 11.770(3) Å; β = 95.54(3)°; V = 1265.16 A3; Z = 4; Dc = 2.87 Mg m-3. The two structures were refined to a final RW = 0.045 for 1209 observed independent reflections and 95 parameters for I, and to a final RW = 0.040 for 1922 observed independent reflections and 87 parameters for II. The coordination geometry around Co or Rh in the anionic complexes is a distorted (4 + 2) octahedron of four equatorial chelating N atoms and two apical iodides. The H atoms of the hydroxyl groups are involved, as usual, in intramolecular O—H—O bridges with uniform Ο···Ο separations of 2.582 Å for I, and 2.713 Å for II. The rectilinear I—Co—I or I—Rh—I triads form “infinite” zigzag chains extending parallel to the ab plane, with a weak I—I contact of 3.988 Å for I, and 4.010 Å for II.

Synthesis and crystallographic studies of two new 1,3,5-triazines

2020 ◽  
Vol 76 (4) ◽  
pp. 322-327
Author(s):  
Emmanuel Blas Patricio-Rangel ◽  
Margarita Tlahuextl ◽  
Hugo Tlahuext ◽  
Antonio Rafael Tapia-Benavides
Keyword(s):  
Noncovalent Interactions ◽  
Synthesis And Characterization ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Positional Disorder ◽  
Hydrated Salt ◽  
Symmetry Space ◽  
Symmetry Space Group

The synthesis and characterization of two new 1,3,5-triazines containing 2-(aminomethyl)-1H-benzimidazole hydrochloride as a substituent are reported, namely, 2-{[(4,6-dichloro-1,3,5-triazin-2-yl)amino]methyl}-1H-benzimidazol-3-ium chloride, C11H9Cl2N6 +·Cl− (1), and bis(2,2′-{[(6-chloro-1,3,5-triazine-2,4-diyl)bis(azanediyl)]bis(methylene)}bis(1H-benzimidazol-3-ium)) tetrachloride heptahydrate, 2C19H18ClN9 2+·4Cl−·7H2O (2). Both salts were characterized using single-crystal X-ray diffraction analysis and IR spectroscopy. Moreover, the NMR (1H and 13C) spectra of 1 were obtained. Salts 1 and 2 have triclinic symmetry (space group P-1) and their supramolecular structures are stabilized by hydrogen bonding and offset π–π interactions. In hydrated salt 2, the noncovalent interactions yield pseudo-nanotubes filled with chloride anions and water molecules, which were modelled in the refinement with substitutional and positional disorder.

Room temperature conversion of X0.3V2O5· nH2O phase into X2V6O16· nH2O phase Influence of the nature of the cation X+

2004 ◽  
Vol 848 ◽  
Author(s):  
Olivier Durupthy ◽  
Saïd Es-salhi ◽  
Nathalie Steunou ◽  
Thibaud Coradin ◽  
Jacques Livage
Keyword(s):  
Vanadium Oxide ◽  
Room Temperature ◽  
Interlayer Space ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxide Phases ◽  
New Phase ◽  
Supernatant Solution ◽  
Scanning Electron

ABSTRACTVarious cations (Li+, Na+, K+, NH4+, Cs+, Mg2+, Ca2+, Ba2+) were introduced during the formation of a V2O5. nH2O gel. Cation intercalated Xy V2O5. nH2O (y = 0.3 for X = Li+, Na+, K+, NH4+ or y = 0.15 for Mg2+, Ca2+, Ba2+) were first obtained at room temperature but some of them evolve upon ageing into a new phase: XV3O8. nH2O for X = Na+, K+, NH4+ and Cs+ or XV6O16. nH2O for X = Mg2+, Ca2+, Ba2+. All the vanadium oxide phases were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and infrared spectroscopy (IR); the supernatant solutions were analysed by 51V NMR spectroscopy. These vanadium oxide phases exhibit a layered structure with cations and water molecules intercalated within the interlayer space. The formation of the different phases depends mainly on the pH of the supernatant solution and on the nature of the cation.

Spaltung von S4N4 zu S2N2 bei Raumtemperatur: Darstellung und Struktur von S2N2 • 2AlBr3 / Cleavage of S4N4 to S2N2 at Room Tem perature: Preparation and Structure of S2N2 • 2AlBr3

1984 ◽  
Vol 39 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl
Keyword(s):  
Molecular Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

The compound S2N2 • 2AlBr3 has been prepared by reaction of S4N4 with AlBr3 in 1,2-dibromoethane at room temperature. Its crystal and molecular structure have been determined by X-ray diffraction; R = 0.068. Crystal data: monoclinic, P 21/n, a = 9.594(5), b = 9.975(4), c = 7.528(4) Å , β = 111.36(5)°. The S2N2 ring of the centrosymmetrical complex is bonded via its nitrogen atoms to two AlBr3 units thus completing coordination tetrahedra around the Al atoms. Bond distances and angles within the S2N2 ring are d(S-N) = 1.629(13) and 1.651(13) Å, ∢ (S-N-S) = 95.8, and ∢ (N-S-N) - 84.2°. Whereas the S-N bond lengths agree closely with those of free S2N2, the angle at N is enlarged by ca. 5° and the angle at S is decreased by ca. 5°. The sulfur atoms form two close S···Br contacts of length 3.149 (intramolecular) and 3.193 (intermolecular) Å , respectively. The intermolecular attractive nonbonded S···Br interactions tie the complexes together in a way that leads to infinite chains which run parallel to the crystallographic z axis

X-Ray Structure, Electrochemical and Electronic Spectroscopic Examination of Cobaloximatic Acid: Hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III). Extended Intermolecular O-H-O Bridging in the Solid

1993 ◽  
Vol 48 (10) ◽  
pp. 1360-1364
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Irene Jokwi ◽  
Emmanuel Ngameni ◽  
Robert Roux ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Strong Acid ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Acidic Proton ◽  
Spectroscopic Examination

The structure of the cobaloximatic acid, hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III), has been determined by X-ray diffraction. Crystal data: C4H7CoI2N4O4, Mr = 487.87; monoclinic space group P21/a (C2h5 ); a = 10.795(7), b = 9.003(7), c = 11.881(6) Å; β = 97.29(6)°; V = 1145.35 Å3; Z = 4; dc = 2.83 Mg m-3. Rw (R) = 3.6 (3.9)% for 3064 observed independent reflections and 148 parameters. The coordination geometry around CoIII is a distorted (4 + 2) octahedron of four chelating equatorial N atoms and two apical iodides. The compound is most adequately formulated as a monovalent strong acid: H(Co(GH)2I2) (GH- = ethanedioximate or glyoximate). The H atoms of the oxime groups are involved in the usual intramolecular, as well as in much stronger intermolecular O-H-O bridgings (O ••• Ointramol = 2.613-2.631, O ••• Ointramol = 2.454 A). The “acidic” H atom of each molecule participates in the intermolecular bridging which extends throughout the structure, and propagates nearly parallel to the [101] crystallographic direction. The redox properties of the present compound were examined by cyclic voltammetry in acetonitrile solution at room temperature. Redox waves attributed to the reduction of CoIII and to the oxidation of I- were observed, along with a wave which may be linked to the reduction of the “acidic” proton

A tentative interpretation of the results of recent X-ray and infra-red studies of liquid water and H 2 O + D 2 O mixtures

1958 ◽  
Vol 247 (1251) ◽  
pp. 472-481 ◽  
Keyword(s):  
Liquid Water ◽  
Room Temperature ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Infra Red ◽  
Stretching Vibration ◽  
Density Of Water ◽  
Absorption Measurements ◽  
Melting Entropy

An idealized model is proposed for the arrangement of the molecules in liquid water which involves essentially a sixfold co-ordination of water molecules with four short OH...O hydrogen bonds of ~2.9 Å length and two long O...O contacts of ~3.6 Å length. An ice-like structure may contribute to a small extent also. This octahedral model has been based on evidence obtained from X-ray and infra-red absorption measurements. The model has been found to be in agreement with the density of water and the melting entropy of ice. The reliability of the radial distribution curves W(r) of liquid water obtained from recent X-ray diffraction measurements is discussed. Infra-red absorption measurements have been made of liquid HDO in excess D 2 O and H 2 O, respectively. The respective O—H and O—D stretching vibration frequencies of liquid HDO have been determined. The position (at 3400 cm -1 ) and shape of the relatively sharp single O—H stretching absorption band of liquid HDO is closely comparable to the corresponding band in liquid interbonding alcohols. The results of the infra-red studies indicate an OH...O distance of 2.86 Å in liquid water at room temperature.

Pentafluoro[(4-methyl-1,4-bisazoniacy clohex-1 -yl)methy 1] germanate Hydrate: Synthesis and Crystal Structure of a Zwitterionic λ6Ge-Germanate with a GeF5C Framework

1998 ◽  
Vol 53 (5-6) ◽  
pp. 535-539 ◽  
Author(s):  
Reinhold Tacke ◽  
Joachim Heermann ◽  
Melanie Pülm
Keyword(s):  
Molar Ratio ◽  
Water Molecules ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Coordination Polyhedra ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Distorted Octahedra ◽  
Positively Charged

Abstract The zwitterionic (molecular) λ6Ge-germanate pentafluoro[(4-methyl-1,4-bisazoniacyclohexl-yl)methyl]germanate (5) was synthesized by reaction of 1-methyl-4-[(trimethoxygermyl) methyl]piperazine (8) with HF (molar ratio 1:5) in a mixture of water and ethanol at 0 °C and isolated as the hydrate 5 · H2O. The zwitterion 5 is characterized by the presence of a hexacoordinate (formally twofold negatively charged) germanium atom and two tetracoordinate (formally positively charged) nitrogen atoms. Compound 5 · H2O was structurally characterized by single-crystal X-ray diffraction. Crystal data are as follows: C6H17F5GeN2O , triclinic space group P1̄ (no. 2), a = 7.5228(11) Å, b = 12.174(2) Å, c = 12.3041(14) Å, α = 73.74(2)°, β = 82.44(2)°, γ = 74.762(10)°, V = 1041.7(2) Å3, T = 173(2) K, Z = 4, R1 = 0.0227. There are one pair each of crystallographically independent zwitterions 5 and water molecules in the asymmetric unit, the structures of the zwitterions being very similar. Their coordination polyhedra around the germanium atoms are slightly distorted octahedra.

Manganese(II) complexes derived from acyclic ligands having flexible alcohol arms: structural chracterization and SOD and catalase mimetic studies

2021 ◽  
Vol 77 (2) ◽  
pp. 100-110
Author(s):  
Vickie McKee ◽  
Muhammet Kose
Keyword(s):  
Crystal Structure ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Sod Activity ◽  
Potential Donor ◽  
X Ray ◽  
Flexible Ligands ◽  
Chloride Monohydrate ◽  
Acyclic Ligands

In this work, a series of seven MnII complexes of noncyclic flexible ligands derived from 2,6-diformylpyridine and ethanolamine or alkyl-substituted ethanolamines were prepared and characterized, six structurally by single-crystal X-ray diffraction studies. The complexes are dichlorido{2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]diethanol}manganese(II), [MnCl2(C11H15N3O2)] or [MnCl2(L1)], (2), bis{μ-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]diethanol}bis[dithiocyanatomanganese(II)], [Mn2(NCS)4(C11H15N3O2)2] or [Mn2(NCS)4(L1)2], (3), chlorido{1,1′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-2-ol)}manganese(II) chloride monohydrate, [MnCl(C13H19N3O2)(H2O)]Cl·H2O or [MnCl(L2)(H2O)]Cl·H2O, (4), {1,1′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-2-ol)}dithiocyanatomanganese(II), [Mn(NCS)2(C13H19N3O2)] or [Mn(NCS)2(L2)], (5), aquadichlorido{2,2′-dimethyl-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-1-ol)}manganese(II) 0.3-hydrate, [MnCl2(C15H23N3O2)(H2O)]·0.3H2O or [MnCl2(L3)(H2O)]·0.3H2O, (6), (dimethylformamide){2,2′-dimethyl-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-1-ol)}dithiocyanatomanganese(II), [Mn(NCS)2(C15H23N3O2)(C3H7NO)] or [Mn(NCS)2(L3)(DMF)], (7), and (dimethylformamide){2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(butan-1-ol)}dithiocyanatomanganese(II) dimethylformamide monosolvate, [Mn(NCS)2(C15H23N3O2)(C3H7NO)]·C3H7NO or [Mn(NCS)2(L4)(DMF)]·DMF, (8). The crystal structure of ligand L1 is also reported, but that of (5) is not. All four ligands (L1–L4) have five potential donor atoms in an N3O2 donor set, i.e. three N (pyridine/diimine donors) and two alcohol O atoms, to coordinate the MnII centre. The N3O2 donor set coordinates to the metal centre in a pentagonal planar arrangement; seven-coordinated MnII complexes were obtained via coordination of two auxiliary ligands (anions or water molecules) at the axial positions. However, in some cases, the alcohol O-atom donors remain uncoordinated, resulting in five- or six-coordinated MnII complexes. The structurally characterized complexes were tested for their catalytic scavenging of superoxide and peroxide. The results indicated that the complexes with coordinated exogenous water or chloride ligands showed higher SOD activity than those with exogenous thiocyanate ligands.

Crystal and molecular structures of 3-acetyl-5-[2-(3-ethyl-2-benzothiazolidene)]ethylidenerhodanine and its lithium and sodium salts. Layered organic–inorganic structures

1996 ◽  
Vol 52 (2) ◽  
pp. 277-286 ◽  
Author(s):  
F. Nüesch ◽  
M. Grätzel ◽  
R. Nesper ◽  
V. Shklover
Keyword(s):  
Molecular Structures ◽  
Water Molecules ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Oriented Molecules ◽  
Internal Surfaces ◽  
Solvent Molecules ◽  
Inorganic Layers

An X-ray diffraction study of the crystals of 5-[2-(3-ethyl-2-benzothiazolidene)]ethylidenerhodanine N-acetic acid (1, solvate with dimethylsulfoxide), lithium 5-[2-(3-ethyl-2-benzothiazolidene)]ethylidenerhodanine N-acetate (2, solvate with water and dimethylformamide) and sodium 5-[2-(3-ethyl-2-benzothiazolidene]ethylidenerhodanine N-acetate (3, octahydrate) have been carried out at 295 K. Crystal data for (1): C16H14N2O3S3.C2H6OS, Mr = 456.6, triclinic, a = 7.664 (6), b = 9.874 (8), c = 14.851 (8) Å, α = 101.71 (5), β = 90.45 (5), γ = 102.27 (5)°, V = 1074 (1) Å3, space group P{\bar 1}, Z = 2, F(000) = 476, Dx = 1.412 g cm−3, μ(MoKα) = 0.469 mm−1, R = 0.0698 for 1688 reflections with F > 6σ(F); for (2): Li+.C16H13N2O3S− 3.2H2O.1.5C3H7NO, Mr = 530.1, triclinic, a = 7.249 (5), b = 10.773 (6), c = 16.433 (13) Å, α = 87.66 (6), β = 85.22 (6), γ = 77.04 (6)°, V = 1246 (1) Å3, space group P1, Z = 2, F(000) = 556, Dx = 1.413 g cm−3, μ(Mo Kα) = 0.342 mm−1, R = 0.0551 for 2360 reflections with F > 6σ(F); for (3): Na+.C16H13N2O3S− 3.8H2O, Mr = 544.6, monoclinic, a = 46.209 (12), b = 7.005 (3), c = 16.583 (8) Å, β = 109.45 (4)°, V = 5061 (6) Å3, space group C2/c, Z = 8, F(000) = 2288, Dx = 1.429 Mg m−3, μ(Mo Kα) = 0.365 mm−1, R = 0.0440 for 2680 reflections with F > 6σ(F). Crystals (1) and (2) are built up of stacks of head-to-tail oriented molecules and anions, respectively, which have alternating interplanar separations of 3.41 (1) and 3.46 (1) Å for (1), and 3.38 (1) and 3.45 (1) Å, for (2) (so-called H aggregation of dye). The Li+ cations and solvent molecules form the cationic layers in crystal (2), alternating with the anionic layers along the c direction. The shifted head-to-head oriented anions in crystal (3) form uniform stacks along the b axis at the interplanar separation of 3.39 (1) Å (so called J aggregation of dye). The stacks are arranged in bilayers with the O atoms on the outer surfaces of the bilayers. The inorganic layers situated between the anionic organic bilayers consist of extended chains of distorted edge-shared polyhedra of Na+ cations and water molecules. The O atoms on the outer surfaces of the bilayers do not participate in the direct ionic interactions with the Na+ cations. The structure and stability of layered organic inorganic structures with internal surfaces are discussed by means of the crystal structures of (1)–(3) and literature data.

Structure refinement of Cu8GeS6 using X-ray diffraction data from a multiple-twinned crystal

1999 ◽  
Vol 55 (5) ◽  
pp. 721-725 ◽  
Author(s):  
Mitsuko Onoda ◽  
Xue-An Chen ◽  
Katsuo Kato ◽  
Akira Sato ◽  
Hiroaki Wada
Keyword(s):  
Diffraction Data ◽  
Room Temperature ◽  
Structure Refinement ◽  
Unit Cell ◽  
Temperature Phase ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Germanium Sulfide ◽  
Symmetry Operations

The structure of the orthorhombic room-temperature phase of Cu8GeS6 (copper germanium sulfide), Mr = 773.27, has been refined on the basis of X-ray diffraction data from a 12-fold twinned crystal applying a six-dimensional twin refinement technique. For 1804 unique reflections measured using Mo Kα radiation, RF was 0.083 with 77 structure parameters and 12 scale factors. The symmetry operations, the unit cell and other crystal data are (0, 0, 0; ½, ½, 0) + x, y, z; y, x, z; ¼ − x, ¾ − y, ½ + z; ¾ − y, ¼ − x, ½ + z; a = b = 9.9073 (3) Å, c = 9.8703 (4) Å, α = β = 90°, γ = 90.642 (4)°; V = 968.7 (1) Å3, Z = 4, Dx  = 5.358 Mg m−3, μ = 21.70 mm−1. The standard setting of the space group and the reduced unit cell are Pmn21; a = 7.0445 (3), b = 6.9661 (3), c = 9.8699 (5) Å; Z = 2.

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