X-ray crystallographic characterization of hydrogen-bonding interactions in piperidinium chloride and piperidinium tetrachloroaluminate: relevance to the structure of room-temperature melts

A new bi-capped Keggin heteropoly molybdovanadated derivative, [Co (en)3]2[SiMo8V6O42]∙6H2O (1) (en = ethylendiamine) has been hydrothermally synthesized and structurally characterized by the elemental analysis, IR, XPS and single crystal X-ray diffraction. The crystal structure analysis reveals that compound 1 consists of [Co (en)3]2+transition metal coordination fragment and the [SiMo8V6O42]4-building blocks, which are linked together via hydrogen-bonding interactions to form a new 3-D supramolecular networks.

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Synthesis and Structural Characterization of a Tetranuclear Zinc(II) Complex with P,P'-Diphenylmethylenediphosphinate (pcp) and 2,2'-Bipyridine (2,2'-bipy) Ligands

Zeitschrift für Naturforschung B ◽

10.1515/znb-2007-1202 ◽

2007 ◽

Vol 62 (12) ◽

pp. 1476-1480 ◽

Cited By ~ 4

Author(s):

Andrea Ienco ◽

Stefano Midollini ◽

Annabella Orlandini ◽

Ferdinando Costantino

Keyword(s):

Hydrogen Bonding ◽

Zinc Ions ◽

Monodentate Ligand ◽

X Ray ◽

Hydrogen Bonding Interactions ◽

Metal Atoms ◽

Oxygen Donors ◽

Tetranuclear Complexes ◽

Water Hydrogen

A new tetranuclear complex of zinc(II) with P,P′-diphenylmethylenediphosphinate and 2,2′- bipyridine ligands was synthesized. [(pcp)(2,2′-bipy)Zn (μ3-pcp)Zn (2,2′-bipy)]2 · 6H2O was characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and X-ray diffractometry. The structure consists of tetranuclear complexes connected through water hydrogen-bonding interactions in corrugated 2D layers. Two crystallographically independent zinc ions are in a distorted five-coordinate environment, being surrounded by three oxygen atoms of phosphinate groups (from two pcp ligands) and by two bipy nitrogen donors. Of the two independent pcp anions the first one utilizes all of its oxygen donors to coordinate one metal as bidentate and two metal atoms as a monodentate ligand, whereas the second one is only bidentate for one metal atom.

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Energetic Materials: The Preparation and Structural Characterization of Three Biguanidinium Dinitramides

Acta Crystallographica Section B Structural Science ◽

10.1107/s0108768196013183 ◽

1997 ◽

Vol 53 (3) ◽

pp. 504-512 ◽

Cited By ~ 17

Author(s):

A. Martin ◽

A. A. Pinkerton ◽

R. D. Gilardi ◽

J. C. Bottaro

Keyword(s):

Hydrogen Bonding ◽

Structural Characterization ◽

Diffraction Data ◽

Energetic Materials ◽

Room Temperature ◽

Asymmetric Structure ◽

X Ray Diffraction ◽

X Ray ◽

Bond Lengths

Three biguanidinium salts of the energetic dinitramide anion have been prepared and structurally characterized from room-temperature X-ray diffraction data. Biguanidinium mono-dinitramide, (BIGH)(DN), triclinic, P\overline 1, a = 4.3686 (4), b = 9.404 (2), c = 10.742 (1) Å, \alpha = 83.54 (1), \beta = 80.386 (9), \gamma = 79.93 (1)°, V = 426.8 (1) Å3, Z = 2, D x = 1.62 g cm−3. Biguanidinium bis-dinitramide, (BIGH2)(DN)2, monoclinic, C2/c, a = 11.892 (2), b = 8.131 (1), c = 13.038 (2) Å, \beta = 115.79 (1)°, V = 1135.1 (3) Å3, Z = 4, D x = 1.84 g cm−3. Biguanidinium bis-dinitramide monohydrate, (BIGH2)(DN)2.H2O, orthorhombic, P212121, a = 6.4201 (6), b = 13.408 (1), c = 14.584 (2) Å, V = 1255.4 (4) Å3, Z = 4, D x = 1.76 g cm−3. All three structures are characterized by extensive hydrogen bonding. Both the mono- and diprotontated cations consist of two planar halves twisted with respect to each other. The dinitramide anion has a surprisingly variable and asymmetric structure. The two halves of the anion are twisted with respect to each other; however, the twist varies from 5.1 to 28.9°. In addition, the two ends of the anion have significantly different geometries, e.g. the `equivalent' N—N bond lengths differ by up to 0.045 Å.

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Lewis-Base Adducts of Lead(II) Compounds. X. Synthetic and Structural Studies of Some 1:1 Adducts of 'tet-b' With Lead(II) (Pseudo-)Halides

Australian Journal of Chemistry ◽

10.1071/ch9961067 ◽

1996 ◽

Vol 49 (10) ◽

pp. 1067 ◽

Cited By ~ 10

Author(s):

JM Harrowfield ◽

H Miyamae ◽

BW Skelton ◽

AA Soudi ◽

AH White

Keyword(s):

Hydrogen Bonding ◽

Room Temperature ◽

Lewis Base ◽

Double Salt ◽

Rear Side ◽

Hydrogen Atoms ◽

X Ray ◽

Hydrogen Bonding Interactions ◽

Structure Determinations ◽

Pseudo Halides

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for 1 : 1 adducts of (7R*,14R*)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (' tet -b') with a variety of lead(II) salts. [( tet -b)PbCl2] is monoclinic, P 21/c, a 7.183(3), b 12.425(2), c 24.418(2) Ǻ, β 95.32(3)°, Z = 4; conventional R on |F| was 0.044 for 3188 independent, 'observed' (I > 3σ(I)) reflections. [( tet -b)PbI2] is monoclinic, P 21/c, a 19.920(5), b 7.772(5), c 15.605(6) Ǻ, β 108.39(2)°, Z = 4; R 0.051 for No 2507. [( tet -b) Pb (NCS)2] is orthorhombic, P 212121, a 36.99(1), b 8.996(5), c 6.964(3) Ǻ, Z = 4; R 0.043 for No 2100. All are discrete mononuclear [( tet -b)PbX2] entities in which the macrocyclic N4 ligand occupies one 'face' of the N4PbX2 coordination sphere, the thiocyanate ligands being N-bonded, with Pb -N-C angles of 116(2) and 118(1)°; interesting hydrogen-bonding interactions are found, columns of molecules being formed by way of hydrogen bonding between the coordinated (pseudo-)halides and the NH hydrogen atoms which project to the 'rear' face of the ligand of the next molecule, opposite the metal. In contrast to these, the bromide analogue, monoclinic, P21, a 9.342(3), b 12.720(5), c 18.845(5) Ǻ, β 103.17(2)°, Z = 4, R 0.035 for No 3593, is best formulated as [( tet -b) PbBr ] Br, one only of the bromide entities being bound to the lead, the other being fully dissociated by hydrogen bonding/ion pairing to the 'rear' side of adjacent ligands , forming hydrogen-bonded sheets rather than columns. This formulation has been extended to provide a description of an analogous mixed chloride- perchlorate 'double salt', [( tet -b) PbCl ] (ClO4).CH3OH, which is orthorhombic, P 212121, a 19.475(2), b 18.73(1), c 6.820(2) Ǻ, Z = 4, R 0.054 for No 3075. However, another double salt, modelled in refinement as Pb ( tet -b)Cl0.5(ClO4)1.5.H2O, orthorhombic Pnma , a 20.640(5), b 26.16(1), c 8.937(4) Ǻ, Z = 4 dimers , R 0.074 for No 1769, is in this case more appropriately described as [( tet -b) Pb (OClO2O)2Pb( tet -b)] (ClO4) Cl.H2O with perchlorate rather than halide coordinated, and an incipiently dimeric cation, as in the parent [( tet -b) Pb (OClO3)]2 (ClO4)2.2H2O.

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Formation and Structural Characterization of [RuCl2(CO)2(SPh2)2], [RuCl2(CO)3(OH2)], and [Ru(OH2)6][RuCl3(CO)3]2 · 2H2O

Zeitschrift für Naturforschung B ◽

10.1515/znb-2003-1005 ◽

2003 ◽

Vol 58 (10) ◽

pp. 959-964 ◽

Cited By ~ 5

Author(s):

Marjaana Taimisto ◽

Raija Oilunkaniemi ◽

Risto S. Laitinen ◽

Markku Ahlgrén

Keyword(s):

Hydrogen Bonding ◽

Hydrogen Bonds ◽

Room Temperature ◽

Three Dimensional ◽

Temperature Reaction ◽

X Ray ◽

X Ray Crystallography ◽

Dimensional Network ◽

Moderate Yield

While the room temperature reaction of [RuCl2(CO)3]2 and Ph2S in tetrahydrofuran in air affords [RuCl2(CO)2(SPh2)2] (1) in moderate yield, that in dichloromethane results in the formation of a mixture of [RuCl2(CO)3(H2O)] (2) and [Ru(H2O)6][RuCl3(CO)3]2·2H2O (3). Very small amounts of 1 are produced only upon prolonged reflux of the reagents. All compounds were characterized by X-ray crystallography. 1 crystallizes as discrete octahedral cis(CO), cis(Cl), trans(Ph2S) complexes, which are joined into stacks by weak H···Cl hydrogen bonds. 2 is also composed of discrete octahedral complexes. Four hydrogen bonds involving aqua and chlorido ligands link two complexes into a dimer. The structure of 3 consists of octahedral hexaaquaruthenium cations and two tricarbonyltrichloridoruthenate anions. The water of crystallization is involved in hydrogen bonding between the cations and anions resulting in the formation of a continuous three-dimensional network.

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Synthesis and X-Ray Crystal Structure of (1E)-1-(4-Chlorophenyl)-N-hydroxy-3-(1H-imidazol-1-yl)propan-1-imine

Journal of Chemistry ◽

10.1155/2013/418601 ◽

2013 ◽

Vol 2013 ◽

pp. 1-4 ◽

Cited By ~ 1

Author(s):

Mohamed I. Attia ◽

Hazem A. Ghabbour ◽

Maha S. Almutairi ◽

Soraya W. Ghoneim ◽

Hatem A. Abdel-Aziz ◽

...

Keyword(s):

Crystal Structure ◽

Hydrogen Bonding ◽

Antifungal Agents ◽

Synthesis And Characterization ◽

Monoclinic Space Group ◽

Space Group ◽

X Ray ◽

Hydrogen Bonding Interactions

Synthesis and characterization of (1E)-1-(4-chlorophenyl)-N-hydroxy-3-(1H-imidazol-1-yl)propan-1-imine (4) are reported. X-ray crystal structure of the title oxime4confirmed its assigned (E)-configuration. The compound crystallizes in the monoclinic space groupP21/cwitha=13.4292(3) Å,b=8.8343(2) Å,c=11.1797(3) Å,α=90°,β=108.873(2)°,γ=90°,V=1255.03(5) Å3, andZ=4. The molecules are packed in crystal structure by weak intermolecularO–H⋯Nhydrogen bonding interactions. Compound4is a useful intermediate for the synthesis of new imidazole-containing antifungal agents.

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{[(PhCH2Sn)12(μ3-O)14(μ-OH)6](F3CSO3)2}: A New Dodecanuclear Organostannoxane

Zeitschrift für Naturforschung B ◽

10.1515/znb-2011-0307 ◽

2011 ◽

Vol 66 (3) ◽

pp. 262-268

Author(s):

Laurent Plasseraud ◽

Hélène Cattey ◽

Philippe Richard

Keyword(s):

Mass Spectrometry ◽

Hydrogen Bonding ◽

Room Temperature ◽

Bond Cleavage ◽

Trifluoromethanesulfonic Acid ◽

Two Dimensional ◽

X Ray Diffraction ◽

Oh Groups ◽

X Ray ◽

Hydrogen Bonding Interactions

The new dodecanuclear organostannoxane {[(PhCH2Sn)12(μ3-O)14(μ-OH)6](F3CSO3)2} (2) has been isolated as single crystals from the reaction of trifluoromethanesulfonic acid (F3CSO3H) with the decanuclear dibenzyltin(IV)-oxo cluster, [(PhCH2)2SnO]6{[(PhCH2)2SnOH]2(CO3)}2 (1), in [D3]acetonitrile, at room temperature. Compound 2 was structurally characterized by X-ray diffraction analysis, multinuclear NMR and IR spectroscopy, mass spectrometry, and thermogravimetry. The structure of 2 can be described as a football cage framework containing twelve tin atoms, exhibiting two distinct coordination geometries, penta- and hexacoordinated respectively, and linked together through μ3-O and μ-OH ligands. Resulting from Sn-C bond cleavage, all tin atoms are only connected to one benzyl ligand. Furthermore, two of the three oxygen atoms of each trifluoromethanesulfonate counteranions are involved in hydrogen bonding interactions with bridging μ-OH groups of two distinct Sn12 cations leading to the propagation of a two-dimensional polymeric network.

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Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I / Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I

Zeitschrift für Naturforschung B ◽

10.1515/znb-1994-1012 ◽

1994 ◽

Vol 49 (10) ◽

pp. 1381-1386 ◽

Cited By ~ 5

Author(s):

Stefan Horstmann ◽

Wolfgang Schnick

Keyword(s):

Crystal Structure ◽

Hydrogen Bonding ◽

Room Temperature ◽

Bond Distance ◽

Acetonitrile Solution ◽

Structure And Properties ◽

X Ray ◽

Hydrogen Bonding Interactions ◽

Anions And Cations ◽

Ray Methods

Abstract The title compound has been prepared starting from phosphorothionic triamide SP(NH2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure of [P(NH2)4]I has been determined by single crystal X-ray methods (P4/nbm; a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+ - and I−-ions are found with significant N - H···I-hydrogen bonding interactions between anions and cations (H -I: 276.4 pm). The P - N - bond length in the cation (160.7(2) pm) represents the shortest P - NH2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(NH2)4]I in solution and in the solid has been investigated.

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Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaaminol- 1-thio-1 λ5,3λ5-diphosphaz-2-en (NH2)2P(S)N=P(NH2)3 / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam 1-thio-1 λ5,3λ5-diphosphaz-2-en (NH2)2P(S)N=P(NH2)3

Zeitschrift für Naturforschung B ◽

10.1515/znb-1997-0410 ◽

1997 ◽

Vol 52 (4) ◽

pp. 490-495 ◽

Cited By ~ 5

Author(s):

Stefan Horstmann ◽

Wolfgang Schnick

Keyword(s):

Crystal Structure ◽

Hydrogen Bond ◽

Hydrogen Bonding ◽

Hydrogen Atom ◽

Room Temperature ◽

Acetonitrile Solution ◽

Structure And Properties ◽

X Ray ◽

Hydrogen Bonding Interactions ◽

Ray Methods

Abstract (NH2)2P(S)N=P(NH2)3 has been prepared by a two step synthesis. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of (NH2)2P(S)N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c, a = 998.27(9) b = 762.78(8), c = 1007.70(15) pm, β = 107.340(7)°, Z = 4). In the crystal structure each hydrogen atom is subject to a hydrogen bond. Four N-H -N hydrogen bonding interactions per molecule build up a framework connecting two molecules in eight-membered rings. Each sulfur atom shows six distances N-H···S in the range of weak hydrogen bonding interactions.

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Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽

10.3390/chemistry3010013 ◽

2021 ◽

Vol 3 (1) ◽

pp. 149-163

Author(s):

Duncan Micallef ◽

Liana Vella-Zarb ◽

Ulrich Baisch

Keyword(s):

Crystal Structure ◽

Mass Spectrometry ◽

Nuclear Magnetic Resonance ◽

Hydrogen Bonding ◽

Nmr Spectroscopy ◽

Ir Spectroscopy ◽

Room Temperature ◽

Intermolecular Hydrogen Bonding ◽

X Ray Diffraction ◽

X Ray

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.

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