Crystal structure of acrylamide

The crystal structure of acrylamide is re-determined by single crystal X-ray diffraction (133(1) K, BRUKER SMART 1000 CCD, a = 8.228(1) Å, b = 5.759(1) Å, c = 9.760(1) Å, β = 120.04(1)°, V = 400.3(1) Å,³, space group P2₁/c, Z = 4, R = 0.0543 for 867 reflections). In the structure strong hydrogen bonds N-H...O join the molecules of C₃H₅NO into bi-molecular layers that make C...C molecular contacts. It is demonstrated that the process of solid phase polymerization of acrylamide should proceed through the cleavage of double bonds C(1)=C(2) in the monomers and formation of bonds C(1)-C(1) and C(2)-C(2) between the closest carbon atoms of different layers.     

Crystal structure of diacetato-bis(2-methyl-2-propylamine)zinc(II)

The diacetato-bis(2-methyl-2-propylamine)zinc(II) compound crystallizes in the triclinic system, space group P-1 with unit cell parameters a = 10.0144(10)Å, b = 10.2687(10)Å, c = 10.5149(10)Å. α = 115.184(2)°, β = 97.489(2)°, γ = 114.066(2)°, ν = 830.85(14)ų. The obtained solid state structure of (^tBuNH₂)₂Zn(OOCCH₃)₂ shows both inter- and intramolecular NH—O hydrogen bond interactions which are analyzed.     

π-Complexes of Cu(I) with Alkynes. Synthesis and Crystal Structure of Cs[CuCl<Subscript>2</Subscript>(HOCH<Subscript>2</Subscript>C≡CCH<Subscript>2</Subscript>OH)] ⋅ H<Subscript>2</Subscript>O

Crystals of anionic π-complex Cs[CuCl₂(HOCH₂C≡CCH₂OH)] ? H₂O were synthesized by reaction of 2-butyne-1,4-diol with CuCl in a saturated aqueous solution of CsCl at 90°C and studied by X-ray diffraction analysis. The crystals are triclinic (space group \(P\bar 1\) ; a = 10.155(4) Å, b = 7.828(4) Å, c = 7.115(3) Å, α = 102.62(4)°, β = 100.77(3)°, γ = 106.71(4)°, V = 509(1) ų, Z = 2) and consist of stacks of individual anions [CuCl₂(HOCH₂C≡CCH₂OH)]^? and hydrated [Cs ? H₂O]⁺ cations between the stacks. The Cu(I) atom has trigonal surrounding of two Cl atoms and the C≡C bond of 2-butyne-1,4-diol molecule. The Cu-(C≡C) distance in the π-core is 1.905(8) Å; the C≡C bond is elongated to 1.223(11) Å. In addition to hydrogen bonds O-H?Cl, crystals of the complex also contain O(w)?H-O and O(w)?Cl bonds stabilizing their structure.     

A study of the structure and properties of mixed-ligand Cu(II) complexes with hexafluoroacetylacetone and methyl-, phenyl-ketoimines

The synthesis and X-ray single crystal study of two mixed-ligand Cu(II) complexes are performed: (CH₃C(NCH₃)CHC(O)CH₃)(CF₃C(O)CHC(O)CF₃)Cu (1) (space group P2₁/c, a = 7.0848(12) Å, b = 17.854(3) Å, c = 11.837(2) Å, β = 100.495(6)°, V = 1472.4(4) ų, Z = 4), (CH₃C(NC₆H₅)CHC(O)CH₃)· (CF₃C(O)CHC(O)CF₃)Cu (2) (space group P-1, a = 9.1119(4) Å, b = 9.6954(4) Å, c = 11.1447(6) Å, α = 113.784(2)°, β = 92.383(2)°, γ = 95.402(2)°, V = 893.52(7) ų, Z = 2). The structures are molecular, formed from neutral mixed-ligand copper complexes. The central copper atom has the (3O+N) coordination environment with average Cu-O distances of 1.948 Å and Cu-N of 1.932 Å; the chelate O-Cu-N angle (average) is 94.0°. In the structures, the complexes are linked into dimeric associates with Cu…Cu distances of 3.197 Å (for 1) and 3.246 Å (for 2). The volatility of mixed-ligand complexes 1 and 2 is in between of that of the starting homo-ligand complexes.     

[Rh(NH3)5Cl]WO4 crystal structure

At T 150 K the crystal structure of [Rh(NH₃)₅Cl]WO₄ is studied: a = 11.2374(4) Å, b = 8.4857(3) Å, c = 10.5326(3) Å, V = 1004.36(6) ų, space group Pnma, Z= 4, d _x = 3.117 g/cm³. In the structure, complex ions are bound by N—H…O hydrogen bonds, with the shortest ones of 2.85–2.94 Å. Ionic packing is shown to be considered as rhombohedral with a _t ≈ 5.26 Å, α_t ≈ 106°. Thermal properties of the salt are studied in the hydrogen atmosphere. The product of thermal decomposition at 750°C is a mixture of three solid solutions of Rh_x W _1- x based on fcc, bcc, and hcp structures. All the obtained phases are nanocrystalline. The sizes of coherent scattering regions are 10–12 nm.     

4,4′‐Tri­methyl­enedipyridinium bis­[carboxy­methyl­phos­pho­nate(1–)]: a three‐dimensional framework structure built from O—H⃛O,N—H⃛O and C—H⃛O hydrogen bonds

In the title compound, C₁₃H₁₆N₂²⁺·2C₂H₄O₅P⁻, the cation lies across a twofold rotation axis in space group Fdd2. The anions are linked into molecular ladders by two O—H⃛O hydrogen bonds [H⃛O = 1.73 and 1.77 Å, O⃛O = 2.538 (2) and 2.598 (3) Å, and O—H⃛O = 160 and 170°], these ladders are linked into sheets by a single type of N—H⃛O hydrogen bond [H⃛O = 1.75 Å, N⃛O = 2.624 (3) Å and N—H⃛O = 171°] and the sheets are linked into a three‐dimensional framework by a single type of C—H⃛O hydrogen bond [H⃛O = 2.48 Å, C⃛O = 3.419 (4) Å and C—H⃛O = 167°].     

Unique Isle Anion [Cu6Cl10]4- in π-Complex of Cu(I) Chloride with 1-(2-Pyridyl)-4-allyl-piperazinium. Synthesis and crystal structure of [(C5H4NH)NC4H8NH(C3H5]2+[Cu3Cl5]2-

Single crystals of [(C₅H₄NH)NC₄H₈NH(C₃H₅)]²⁺[Cu₃Cl₅]^2? are obtained by ac synthesis in ethanol from 1-(2-pyridyl)-4-allyl-piperazinium and Cu(II) dichlorides and their structure is studied by X-ray diffraction analysis (space group P-1, a = 7.246(7) Å, b = 8.54(1) Å, c = 16.41(1) Å, α = 70.76(8)°, β = 77.24(8)°, λ = 80.42(9)°, V = 30(4) ų, Z = 2, R(F) = 0.0686. In the structure of this π-complex, the Cu and Cl atoms form unusual centrosymmetrical Cu₆Cl₁₀ fragments, each fragment being bonded to two 1-(2-pyridyl)-4-allyl-piper-azinium cations via π-interaction Cu-(C=C). A three-dimensional structure is formed by means of N-H…Cl hydrogen bonds. The trigonal-pyramidal surrounding of the Cu(1) atom includes three Cl atoms and the C=C bond, while the tetrahedral surrounding of Cu(2) and the trigonal surrounding of Cu(3) involve the Cl atoms only.     

Coordination compounds of cobalt(II) and cadmium(II) with 2-amino-4-methylpyrimidine: Synthesis, crystal structure, and luminescent properties

The coordination compounds [CoL₂Cl₂] (I) and [CdL₂(H₂O)₂(NO₃)₂] (II) have been synthesized by the reaction of CoCl₂ · 6H₂O and Cd(NO₃)₂ · 4H₂O with L = 2-amino-4-methylpyrimidine (Ampym, C₅H₇N₃), and their structures have been solved. The crystals of complex I are triclinic, space group $P\bar 1$ , a = 5.627(1) Å, b = 11.191(1) Å, c = 12.445(1) Å, α = 81.00(1)°, β = 77.21(1)°, γ = 76.18(1)°, V = 737.7(2) ų, ρ_calcd = 1.567 g/cm³, Z = 2. The crystals of complex II are monoclinic, space group P2₁/c, a = 10.390(1) Å, b = 11.982(1) Å, c = 7.624(1) Å, β = 102.61(1)°, V = 926.1(2) ų, ρ_calcd = 1.760 g/cm³, Z = 2. Discrete [CoL₂Cl₂] moieties are realized in the structure of complex I. The cobalt atom is tetrahedrally coordinated to the two nitrogen atoms of crystallographically nonequivalent ligands L and two chlorine atoms (Co(1)-N_avg, 2.051(4)Å; Co(1)-Cl(1), 2.241(1) Å; Co(1)-Cl(2), 2.263 Å; bond angles at the cobalt atom lie within a range of 102.1°–118.6°). The complexes are linked into supramolecular zigzag chains by N-H...N(Cl) hydrogen bonds. In the structure of complex II, the Cd²⁺ ion (at the inversion center) is coordinated in pairs to the nitrogen atoms of ligand L and the O(NO₃) and O(H₂O) oxygen atoms. The coordination of the Cd²⁺ ion is distorted octahedral (Cd(1)-N(1), 2.341Å; Cd(1)-O(1), 2.340(4) Å; Cd(1)-O(4), 2.327(3) Å; bond angles at the cadmium atom lie within a range of 79.1°–100.9°). N-H...N hydrogen bonds link the complexes into supramolecular chains. These chains are linked into a supramolecular framework by the O-H...O hydrogen bonds between water molecules and NO₃ groups.     

Crystal structures of bis(AZIDO)bis(2-morpholin-4-ylethylamino)copper(II) and bis{2,4-dibromo-6-[(2-morpholin-4-ylethylimino)methyl] phenolato}copper(II)

Two new copper(II) complexes [Cu(MEA)₂(N₃)₂] (1) and [Cu(BMP)₂] (2), where MEA and BMP are 2-morpholin-4-ylethylamine and 2,4-dibromo-6-[(2-morpholin-4-ylethylimino)methyl]phenolate respectively, are prepared and characterized using elemental analysis, FT-IR spectroscopy, and X-ray single crystal diffraction. The crystal of 1 belongs to the triclinic system, space group P-1, with a = 6.661(2) Å, b = 8.440(3) Å, c = 8.913(3) Å, α = 102.032(3)°, β = 107.899(2)°, γ = 98.242(3)°, V = 454.6(3) ų, Z = 1, D _c = 1.490 g/cm³, R ₁ = 0.0226, and wR ₂ = 0.0564. The crystal of 2 belongs to the monoclinic system, space group P2₁/c, with α = 7.0707(7) Å, b = 15.438(1) Å, c = 14.227(1) Å, β = 96.659(2)°, V = 1542.5(3) ų, Z = 2, D _c = 1.821 g/cm³, R ₁ = 0.0437, and wR ₂ = 0.1041. In each complex, the Cu atom is in a square planar coordination. The molecules of 1 are linked through intermolecular N-H...N and N-H...O hydrogen bonds to form layers parallel to the ab plane. The molecules of 2 are linked through intermolecular C-H...Br hydrogen bonds to form a 3D network.     

Crystal structure of trans*-[PtEnPyNO2(OH,NO2)*]Cl·2H2O

The structure of trans*-[PtEnPyNO₂(OH,NO₂)*]Cl·2H₂O was determined by X-ray crystallography. The crystals are monoclinic, a = 31.185(6)Å, b = 12.198(2)Å, c = 8.432(2)Å, b = 100.8(2)°, Z = 8, space group C2/c, R = 0.031 for 2059 reflections with I > 2σ(I). In the complex cation, the polyhedron of the Pt atom is an octahedron formed by five nitrogen atoms from ethylenediamine (Pt-N(aver.), 2.062(7) Å), pyridine (Pt-N, 2.053(7) Å), two NO₂ groups (Pt-N, 2.064(7) Å), and the oxygen atom of the OH group in trans position to the nitro group (Pt-O, 1.999(7) Å). Complex cations, anions Cl^?, and crystal water molecules are linked together through a branched system of hydrogen bonds.     

Two crystalline polymorphic forms of α-(<Emphasis Type="Italic">N</Emphasis>-benzoxazolin-2-one)acetic acid

Two crystalline polymorphic forms of α-(N-benzoxazolin-2-one)acetic acid (BAA) are prepared by changing the temperature of its crystallization from solution in ethanol. Crystallographic data of the α-form are determined: a = 12.7769(17) Å, b = 8.2574(9) Å, c = 16.7390(19) Å, β = 105.087(13)°, space group C2/c, V = 1705.2(4) ų, and Z = 8, while those of β form are a = 5.2854(4) Å, b = 5.9880(4) Å, c = 13.4509(5) Å, β = 94.666(4)°, space group P2₁, V = 424.30(4) ų, and Z = 2. It is found that BAA molecules of the α form combine into infinite one-dimensional chains arranged along axis b by means of O?H···O and C?H···O hydrogen bonds, and these chains are crosslinked via C?H···O hydrogen bonds to form a threedimensional structure. The β form has another system of hydrogen bonds, one of which is bifurcated (O4···O2, O4···O3), and the π–π-interactions between the benzoxazolinone fragments of BAA molecules combined into a chain also arranged along axis b are observed. Calorimetric analysis shows that the polymorphic transition from the α form to the β form occurs at 129°C.     

An X-ray and 13C CP/MAS NMR study of C,C-linked bipyrazoles and bispyrazolylmethanes

4,4′-Methylene-bispyrazole (1) crystallizes in the P2₁/n space group with Z = 4, a = 5.4199(8) Å, b = 16.194(6) Å, c = 8.381(5) Å, β = 98.18(5)°. 4,4′-Methylene-bis (3,5-dimethylpyrazole) (2) crystallizes in the Pbca space group with Z = 8, a = 8.350(3) Å, b = 16.078(3) Å and c = 17.154(5) Å. Finally, 3,3′-bipyrazole (4) crystallizes in the P2₁/n space group with Z = 2, a = 5.465(2) Å, b = 5.491(3) Å, c = 10.058(4) Å and sol; = 92.88(2)°. The packing adopted by molecules 1 and 2 is related to the disposition of the pyrazole rings. In compound 4, all the molecules are joined to their neighbors by two double hydrogen bond systems forming zigzag chains. Using solid state ¹³C NMR spectroscopy, no dynamic proton transfer was observed in these crystals, and not on those of 3,5,3′,5′-tetramethyl-4,4′-bipyrazole (3) either.     

Structure of two new compounds of fluoroquinolone antibiotics with mineral acids

New compounds of sparfloxacin (C₁₉H₂₂F₂N₄O₃, SfH) and levofloxacin (C₁₈H₂₀FN₃O₄, LevoH) with mineral acids, namely, sparfloxacinium bromide (SfH · HBr, I) and levofloxacindium diperchlorate (LevoH · 2HClO₄, II), have been synthesized and characterized by X-ray diffraction. Crystallographic data are a = 7.7151(7) Å, b = 26.109(3) Å, с = 10.008(1) Å, β = 103.556(1)°, V = 1959.7(3) ų, space group P2₁/n, Z = 4 for I and a = 9.727(6) Å, b = 20.440(12) Å, с = 12.286(7) Å, β = 104.327(8)°, V = 2367(2)ų, space group P2₁, Z = 4 for II. The structures of these compounds are stabilized by intra- and intermolecular hydrogen bonds and π–π interaction between SfH₂⁺ or LevoH₃²⁺ ions.     

Crystal structures of 1,1,1-trifluoro-4-hydroxy-4-phenyl-but-3-en-2-one, 2,2,6,6-tetramethyl-3-hydroxy-hept-3-en-5-one, 2,2,6,6-tetramethyl-3-methylamino-hept-3-en-5-one and a study of the ability of these ligands to complex formation with metals

Crystal structures are determined (Bruker Nonius X8 Apex, 4K CCD-detector, λMoK _α, graphite monochromator, T 150 K and 293 K) for two β-diketones F₃CC(O)CH₂C(O)Ph (1) (space group P2₁/c, a = 7.0713(3)Å, b = 11.5190(6)Å, c = 11.3602(6) Å, β = 99.405(2)°, V = 912.90(8) ų, Z = 4), (CH₃)₃CC(O)CH₂C(O)C(CH₃)₃ (2) (space group Pbca, a = 11.5536(8) Å, b = 11.5796(10) Å, c = 17.2523(13) Å, V = 2308.1(3) ų, Z = 8) and a ketoimine (CH₃)₃CC(NCH₃)CH₂C(O)C(CH₃)₃ (3) (space group I4₁/a, a = 18.7687(6) Å, b = 18.7687(6) Å, c = 14.5182(6) Å, V = 5114.2(3) ų, Z = 16). All structures are molecular and comprise isolated molecules joined by van der Walls interactions. The substitution energy of a Na atom for a hydrogen atom in free ligands is calculated by the hybrid B3LYP quantum chemical method. A successful preparation of Na(I) chelates with ligands 1, 2 and failed attempts to prepare a complex with ligand 3 are in accordance with the calculations. Geometrical simulation of a copper(II) complex with ligand 3 reveals the overlap of CH₃ groups which hinders the complexation.     

Molecular structure of a zwitter-ionic 2-piperidinyl-4-dinitromethyl-1,3,5-triazin×(1H, 5H)-6-one salt

A zwitter-ionic salt 2-piperidinyl-4-dinitromethyl-1,3,5-triazin(1H,5H)-6-one is studied by the single crystal X-ray analysis. The crystals are monoclinic: a = 11.526(1) Å, b = 9.211(1) Å, c = 12.182(1) Å; β = 110.69(1)°, V = 1209.9(2) ų, space group P2₁/n; Z = 4, ρ_calc = 1.560 g/cm³. The transformation of the dinitromethyl fragment conformation, the conjugation of one of nitrogroups with the 1,3,5-triazine ring, and an intramolecular hydrogen bond are revealed. The 1,3,5-triazine cycle is strongly distorted due to lactam-lactim tautomerism.     

Synthesis and crystal structure of cadmium(II) complex with 2-pyrimidinecarboxamide

The complex [Cd(N₂H₃C₅ONH₂)₂(CH₃COO)₂] (I) was synthesized and its structure was determined. The crystals are monoclinic: space group C2/c, a = 14/416(1), b = 9.410(1), c = 13.708(1) Å, β = 113.82(1)°, V = 1701.0(1) ų, ρ(calcd.) = 1.862 g/cm³, Z = 4. The structure consists of individual complexes I united by the N-H…O hydrogen bonding system into supramolecular framework. The coordination sphere of the cadmium atom (on axis 2) involves two chelate pyrimidinecarboxamide ligands, which form five-membered chelate rings CdOCCN(Cd-N(2) 2.432(4), Cd-O(3) 2.388(4) Å), and two monodentate CH₃COO^? ions (Cd-O(1) 2.280(3) Å). The second O atom of the acetate group is involved in a weak contact with the Cd²⁺ ion (Cd-O 2.670(4) Å). With account for the latter two contacts, the coordination polyhedron of Cd is irregular octahedron.     

Structure of the 1:1 complex of dimethyl sulfoxide with hydroquinone: Supramolecular architecture based on D-H⋯A hydrogen bonds (D = O,C; A = O, π)

The hydroquinone-dimethyl sulfoxide-toluene system was investigated by thermal and X-ray diffraction analyses. The crystal structure of the 1:1 complex of hydroquinone with dimethyl sulfoxide was determined. Crystal data: C₈H₁₂O₃S, M = 188.24, triclinic system, space group P1¯, unit cell parameters: a = 7.4202(2) Å, b = 8.4046(3) Å, c = 8.7340(3) Å; α = 100.830(1)°, β = 99.794(1)°, γ = 114.129(1)°; V = 469.35(4) ų, Z = 2, d _calc = 1.332 g/cm³, R1 = 0.028, T = 100 K. The molecules are linked in a supramolecular assembly via D-H...A hydrogen bonds (D = O, C; A = O, π).     

Synthesis,structure, and properties of the thermolysis products of [Os(NH<Subscript>3</Subscript>)<Subscript>5</Subscript>Cl][ReCl<Subscript>6</Subscript>]

The crystal structure of [Os(NH₃)₅Cl][ReCl₆] has been refined by X-ray powder analysis: a = 11.645(3) Å, b = 8.3788(2) Å, c = 15.277(4) Å, β = 91.029(6)°, V = 1490(1) ų, d _x = 3.163 g/cm³, space group P2₁/m, Z = 4. The thermolysis product of the salt in a hydrogen atmosphere is a solid substitution solution Os_0.5Re_0.5: a = 2.753(2) Å, c = 4.366(3) Å, space group P6₃/mmc; coherent scattering region (CSR) is ～230 Å.     

Copper(I) π-complexes with 2-butyne-1,4-diol. Synthesis and crystal structure of (2-AmpH)[CuCl<Subscript>2</Subscript>(HOCH<Subscript>2</Subscript>C≡CCH<Subscript>2</Subscript>OH)] (2-AmpH<Superscript>+</Superscript> is 2-aminopyridinium cation)

Crystals of the π-complex (2-AmpH)[CuCl₂(HOCH₂C≡CCH₂OH)] (2-AmpH⁺ is the 2-aminopyridinium cation) were obtained by the reaction of 2-butyne-1,4-diol with CuCl in aqueous 2-aminopyridinium chloride solution and studied by X-ray diffraction: space group P \(\overline 1 \), a= 7.172(4), b= 7.796(3), c = 11.60(9) Å, α = 99.75(6)°, β = 96.53(7)°, γ = 101.03(3)°, Z = 2. The crystals consist of individual anions [CuCl₂(HOCH₂C≡CCH₂OH)]^? and cations [2-AmpH]⁺. The π-coordinated Cu(I) atoms of the complex anion have trigonal-planar surrounding of two chlorine atoms and C≡C bond of the 2-butyne-1,4-diol molecule. The alcohol groups form stable hydrogen bonds N-H?O (1.89 Å) and O-H?Cl (2.20 Å).     

Crystalline and molecular structure of 2,4-diamino-6-dinitromethyl-1,3,5-triazine potassium salt

An X-ray diffraction study of 2,4-diamino-6-dinitromethyl-1,3,5-triazine potassium salt is reported. Crystals are monoclinic: a = 7.697(2) Å, b = 11.147(2) Å, c = 12.612(4) Å, β = 117.95(2)°, V = 955.9(4) ų, space group P2₁/c; Z = 4, ρ_calc = 1.885 g/cm³. The compound crystallizes as a crystalline hydrate with one molecule of water. Anion consists of two planar fragments: dinitromethyl and diamino-1,3,5-triazine, the geometrical parameters of which were analyzed. The coordination of potassium cations and multiple hydrogen bonds leading to the formation of a complex three-dimensional skeleton has been detected.