Formation and X-ray crystal structures of neutral 3D networks by charge-assisted hydrogen bonds between tetrakis(thiourea)platinum(II) complexes and dicarboxylates

Polyhedron ◽  
2006 ◽  
Vol 25 (4) ◽  
pp. 901-909 ◽  
Author(s):  
Philip A. Gale ◽  
Mark E. Light ◽  
Roberto Quesada
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
X Ray ◽  
3D Networks

Structure and properties of two new heteroleptic bismuth(III) dithiocabamates of the general composition Bi(S2CNH2)2X (X = Cl, SCN)

2022 ◽  
Vol 0 (0) ◽  
Author(s):  
Christoph Ludwig Teske ◽  
Huayna Terraschke ◽  
Sebastian Mangelsen ◽  
Wolfgang Bensch
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Electromagnetic Spectrum ◽  
Coordination Pattern ◽  
Structure And Properties ◽  
Acidic Solutions ◽  
Acetone Water ◽  
Asymmetric Coordination ◽  
3D Networks

Abstract The title compounds were prepared by precipitation from acidic solutions of the reactants in acetone/water. Bi(S2CNH2)2Cl (1) crystallizes in the non-centrosymmetric trigonal space group P32 with a = 8.6121(3) and c = 11.1554(4) Å, Z = 3; Bi(S2NH2)2SCN (2) in P21/c (monoclinic) with a = 5.5600(2), b = 14.3679(5), c = 12.8665(4) Å, and β = 90.37(3)°. In the crystal structure of 1 Bi3+ is in a sevenfold coordination of two bidentate and one monodentate S2CHNH2 − anions with an asymmetric coordination pattern of five Bi–S and two Bi–Cl− bonds. The linkage of these polyhedra via common Cl–S edges leads to a 1D polymeric structure with undulated chains propagating in the direction [001]. These chains are linked by strong and medium strong hydrogen bonds forming the 3D crystal structure. In the crystal structure of 2 the Bi3+ cation is in an eightfold coordination. The polyhedron can be described as a significantly distorted tetragonal anti-prism, capped by an additional S atom. Two of these prisms share a common quadrilateral face to form a “prism-double” (Bi2S10N2). These building units are linked by common edges, and the resulting 1D infinite angulated chains propagate along [100]. By contrast to organo-dithiocarbamate compounds, where C–H···X bridges are dominant, the interchain connections in the crystal structures of 1 and 2 are formed exclusively via N–H···S, N–H···Cl, and N–H···N interactions, generating the 3D networks. A significant eccentricity of the Bi3+ cation in the crystal structures of both complexes is observed. Both compounds emit light in the orange range of the electromagnetic spectrum.

Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate / Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates

1982 ◽  
Vol 37 (11) ◽  
pp. 1393-1401 ◽  
Author(s):  
Beatrix Milewski-Mahrla ◽  
Hubert Schmidbaur
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Molar Ratio ◽  
Ionic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Donor Acceptor ◽  
New Compounds

Reactions of pentamethylantimony (CH3)5Sb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramothylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed.The crystal structures of the hydrogen-dibenzoato (1), hydrogen-ortho-plithalato (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter­actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH3)4Sb-tetrahedron in 1 is distorted by two benzoate oxygon atoms (at 304(2) and 340(2) pin). The cation in 2 is largely undistorted and the anion has a hydrogenphthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate.

Hydrogen Bonds in "Carboxyoximes": the Case of Bomane Derivatives

2000 ◽  
Vol 55 (8) ◽  
pp. 677-684 ◽  
Author(s):  
Maciej Kubicki ◽  
Teresa Borowiak ◽  
Wiesław Z. Antkowiak
Keyword(s):  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Carboxylic Acids ◽  
Supramolecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylic Groups ◽  
Acid Function

Abstract The tendency of forming mixed carboxyl-to-oxime hydrogen bonds was tested on the series of bornane derivatives: one with the acid function only (bornane-2-endo-carboxylic acid), one with the oxime function (2,2′-diethylthiobomane-3-oxime), and one with both oxime and carboxylic functions (bornane-2-oxime-3-endo-carboxylic acid). The crystal structures of these compounds were determined by means of X-ray diffraction. In bornane-2-endo-carboxylic acid and 2,2′-diethylthiobornane-3-oxime 'homogenic' hydrogen bonds were found, and these hydrogen bonds close eight-and six-membered rings, respectively. By contrast, in bornane-2-oxime-3-endo-carboxylic acid 'heterogenic' hydrogen bonds between carboxylic and oxime bonds were found. This carboxylic-oxime, or 'carboxyoxime' system is almost always present in compounds which have both oxime and carboxylic groups; therefore it can be regarded as an element of supramolecular structures (synthon). The presence of such synthons can break the tendency of carboxylic acids and oximes towards crystallizing in centrosymmetric structures.

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.

Supramolecular architectures in two 1:1 cocrystals of 5-fluorouracil with 5-bromothiophene-2-carboxylic acid and thiophene-2-carboxylic acid

2017 ◽  
Vol 73 (6) ◽  
pp. 481-485 ◽  
Author(s):  
Marimuthu Mohana ◽  
Packianathan Thomas Muthiah ◽  
Colin D. McMillen
Keyword(s):  
Solid State ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Base Pairs ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Acid Acid ◽  
Carboxylic Acid Dimer

In solid-state engineering, cocrystallization is a strategy actively pursued for pharmaceuticals. Two 1:1 cocrystals of 5-fluorouracil (5FU; systematic name: 5-fluoro-1,3-dihydropyrimidine-2,4-dione), namely 5-fluorouracil–5-bromothiophene-2-carboxylic acid (1/1), C5H3BrO2S·C4H3FN2O2, (I), and 5-fluorouracil–thiophene-2-carboxylic acid (1/1), C4H3FN2O2·C5H4O2S, (II), have been synthesized and characterized by single-crystal X-ray diffraction studies. In both cocrystals, carboxylic acid molecules are linked through an acid–acid R 2 2(8) homosynthon (O—H...O) to form a carboxylic acid dimer and 5FU molecules are connected through two types of base pairs [homosynthon, R 2 2(8) motif] via a pair of N—H...O hydrogen bonds. The crystal structures are further stabilized by C—H...O interactions in (II) and C—Br...O interactions in (I). In both crystal structures, π–π stacking and C—F...π interactions are also observed.

Heterocyclic Tautomerism. II. 4-Acylpyrazolones. X-Ray Crystal Structures of 4-Benzoyl-5-methyl-2-phenylpyrazol-3(2H)-one and 4-Acetoacetyl-3-methyl-1-phenylpyrazol-5-ol

1985 ◽  
Vol 38 (3) ◽  
pp. 401 ◽  
Author(s):  
MJ O'Connell ◽  
CG Ramsay ◽  
PJ Steel
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Crystalline Form ◽  
Intermolecular Hydrogen Bonds ◽  
Intramolecular Hydrogen Bonds ◽  
X Ray ◽  
Intramolecular Hydrogen

The colourless crystalline form of the benzoylpyrazolone (2) has molecules with the NH structure (2c) stabilized by intermolecular hydrogen bonds. At room temperature crystals are monoclinic: P21/c, a 13.508(5), b 9.124(4), c 11.451(3)Ǻ, β 90.80(3)°, Z4; the structure was refined to R 0.059, Rw 0.048. The acetoacetylpyrazolone (3) has the OH structure (3c) with two intramolecular hydrogen bonds. At 193 K crystals are triclinic: Pī , a 7.142(2), b 13.704(8), c 14.699(7)Ǻ, α 117.36(3), β 96.87(3), γ 93.73(3)°, Z 4; the structure was refined to R 0.049, Rw 0.054.

Zur Kenntnis der Sulfite und Sulfithydrate des Zinks, Mangans, Magnesiums und Cobalts — Röntgenographische, spektroskopische und thermoanalytische Untersuchungen / Sulfites and Sulfite Hydrates of Zinc, Manganese, Magnesium and Cobalt-X-ray, Spectroscopic and Thermoanalytical Data

1977 ◽  
Vol 32 (11) ◽  
pp. 1230-1238 ◽  
Author(s):  
Heinz Dieter Lutz ◽  
Saleh M. El-Suradi ◽  
Bernward Engelen
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Ir Spectra ◽  
Single Crystal ◽  
Crystal Structures ◽  
Crystal Data ◽  
X Ray ◽  
Thermoanalytical Data ◽  
O 175 ◽  
Manganese Magnesium

IR, Raman, and X-ray data of ZnSO3 · 2½ H2O, ZnSO3 · 2 H2O, ZnSO3 ·½ H2O, ZnSO3, MnSO3 · 3 H2O, MnSO3 · H2O, MnSO3, MgSO3 · 6 H2O, MgSO3 · 3 H2O, CoSO3 · 3 H2O, CoSO3 · 2½ H2O, and CoSO3·2 H2O are presented. Except of MgSO3·6 H2O and ZnSO3 · 2½ H2O the crystal structures of these compounds are yet unknown. The following crystal data could be determined by single crystal measurements: ZnSO3 · 2 H2O (monoclinic, P21/n) : a = 642.1, b = 852.4, c = 757.4 pm, β = 98.93°, Z = 4, MnSO3 · 3 Η2Ο (monoclinic, Ρ21/n) : a = 665.0, b = 890.6, c = 879.3 pm, ß = 96.11°, Z = 4, MnSO3 · Η2Ο (orthorhombic) : a = 2565.1, b = 483.9, c = 576.0 pm, Z = 8, CoSO3 · 3 Η2Ο (orthorhombic, Pna21, isotype with MgSO3 · 3 H2O): a = 952.7, b = 942.0, c = 552.1 pm, Z = 4, CoSO3• 2½ H2O (tetragonal) : a = b = 946.4, c = 1021.1 pm, Z = 8, CoSO3 · 2 H2O (isotype with ZnSO3 · 2 H2O) : a = 639.7, b = 855.3, c = 753.7 pm, β = 98.85°, Z = 4. The IR spectra show that with exception of MnSO3· H2O strong hydrogen bonds are present in the sulfite hydrates. The decomposition of the sulfites has been examined by thermal analysis. Dehydration of the sulfite hydrates starts at 90 (ZnSO3 · 2½ H2O), 120 (ZnSO3 · 2 H2O), 175 (ZnSO3 · 1/2 H2O), 85 (MnSO3 · 3 H2O), 205 (MnSO3 · H2O), 70 (MgSO3 · 6 H2O), 130 (MgSO3 · 3 H2O), 120 (CoSO3 · 3 H2O), 140 (CoSO3 · 2½ H2O), and 150 °C (CoSO3 · 2 H2O). Decomposition of the anhydrous sulfites occurs at 300-350 (ZnSO3), 390-460 (MnSO3), and 400-530 °C (MgSO3).

Synthesen, Kristallstrukturen und Eigenschaften von Trisilber-und Trikalium-tri-μ-imido-cyclotriphosphat, Ag3(PO2NH)3 und K3(PO2NH)3 / Syntheses, Crystal Structures, and Properties of Trisilver and Tripotassium Tri-μ-im ido Cyclotriphosphate, Ag3(PO2NH)3 and K3(PO2NH)3

1997 ◽  
Vol 52 (2) ◽  
pp. 251-255 ◽  
Author(s):  
N. Stock ◽  
W. Schnick
Keyword(s):  
Aqueous Solution ◽  
Thermal Decomposition ◽  
Nitrogen Atom ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Chair Conformation ◽  
X Ray ◽  
Diffusion Controlled ◽  
Structures And Properties ◽  
Ray Methods

Abstract Coarse crystalline Ag3(PO2NH)3 (1) and K3(PO2NH)3 (2) are obtained by addition of an aqueous solution of AgNO3 to an acidified solution of Na3(PO2NH)3 · 4H2O and by diffusion controlled addition of ethanol to a solution of K3(PO2NH)3 in water, respectively. The crystal structures of 1 and 2 have been determined by single crystal X-ray methods (Ag3(PO2NH)3: P21/c; a = 1166.6(1), b = 786.4(1), c = 997.8(1) pm, β = 106.91(1)°; Z = 4. K3(PO2NH)3: R3̄; a = 1271.4(2), c = 1017.9(2) pm, Z = 6). In Ag3(PO2NH)3 the cyclic anion is markedly distorted because of interactions between Ag+ and one nitrogen atom of the anion. In K3(PO2NH)3 the trimetaphosphimate ring shows a chair conformation and two cyclic anions are connected to each other by hydrogen bonds. DTA/TG investigations show thermal decomposition above 275 and 250 °C for 1 and 2, respectively.

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