Crystal structure of <Emphasis Type="Italic">p</Emphasis>-carboxyphenylhydrazone benzoylacetone

The crystal structure of p-carboxyphenylhydrazone benzoylacetone is determined. The crystals are monoclinic, a = 13.614(4) Å, b = 11.388(2) Å, c = 20.029(6) Å, β = 104.82(2)°, V = 2339(9) ų, Z = 8, space group C2/c, and R = 0.038 for 1622 reflections with I > 2σ(I). The crystal is built of C₁₇H₁₄N₂O₄ neutral molecules that are linked by O-H?O hydrogen bonds between the carboxyl groups into centrosymmetric pseudodimers. The effect of carboxylation of the phenylhydrazone fragment and the position of the carboxyl group on the molecular packing in the crystal is determined. The N(1)-H(1N)?O(1) intramolecular hydrogen bond (N-H, 0.94 Å; H?O, 1.87 Å; N?O, 2.59 Å; and the N-H?O angle, 133°) is formed in the molecule.     

X-ray mapping in heterocyclic design: V. Diffractometric study of the crystal structure of 2-hydroxy-3-trifluoracetylimidazo[1,2-a]pyridine hydrochloride at 180 K

The crystal structure of 2-hydroxy-3-trifluoracetylimidazo[1,2-a]pyridine hydrochloride C₉H₆F₃ClN₂O₂ is determined by X-ray diffraction at 180 K. The structure is solved by the direct method and refined by the least-squares procedure to R = 0.0296. The alternation of bond lengths in the six-membered fragment of the molecule is observed. One of the specific features of the crystal structure is the formation of a system of the N-H?Cl^? (N?Cl, 3.09 Å; N-H, 0.83 Å; H?Cl, 2.33 Å; and N-H?Cl, 153°) and O-H?Cl^? (O?Cl, 2.87 Å; O-H, 0.95 Å; H?Cl, 1.92 Å; and O-H?Cl, 178°) hydrogen bonds in which the chlorine atoms are related to the reference atom by different symmetry transformations.     

Crystal and molecular structures of 11,12-epoxydrim-8(9)-en-11β-ol-7-one

The crystal structure of 11,12-epoxydrim-8(9)-en-11β-ol-7-one is determined by X-ray diffraction. The crystal data for the C₁₅H₂₂O₃ composition are as follows: a = 6.646(1) Å, b = 7.242(1) Å, c = 7.635(2) Å, α = 84.34(3)°, β = 84.50(3)°, γ = 69.84(3)°, space group P1, and Z = 1. The structure is solved by the direct method and refined in the anisotropic approximation to R = 0.043 and R _w = 0.110. The stereochemical formula of the compound is determined. It is shown that the hydroxyl group at the C(11) atom is situated at the β position. In the crystal, the molecules related by the translation along the a-b direction of the unit cell are linked into infinite chains by intermolecular hydrogen bonds between the hydrohyl group and the carbonyl oxygen atom [O-H?O, 2.867(4) Å].     

Crystal structure of hydrazine 5-amino-1-benzyl-1,2,3-triazole-4-carboxylate hexafluorosilicate trihydrate

Hydrazine 5-amino-1-benzyl-1,2,3-triazole-4-carboxylate hexafluorosilicate trihydrate (I) is synthesized. The crystal structure of the compound synthesized is determined. Crystals I are monoclinic, a = 13.353(1) Å, b = 21.094(2) Å, c = 20.233(2) Å, β = 94.05(3)°, space group P2₁/c, and R = 0.0584 for 16 601 reflections with I > 2σ(I). In the asymmetric part of the unit cell, four organic cations protonated at the terminal hydrazine nitrogen atoms, two hexafluorosilicate anions, and six water molecules are linked into a three-dimensional framework through hydrogen bonds of the N-H?F, N-H?O, and O-H?F types.     

Crystal structure of lepidocrocite FeO(OH) from the electron-diffractometry data

The crystal structure of lepidocrocite γ-FeO(OH) with the lattice parameters a = 3.072(2), b = 12.516(3), c = 3.873(2) Å, sp. gr. Cmcm has been refined by the electron-diffractometry data for 135 crystallographically nonequivalent reflections up to R = 0.048. Using the difference syntheses of the Fourier potential, we established, for the first time, the anisotropy in the distribution of the electrostatic potential of hydrogen and the statistical occupancy (with the probability of 1/2) by hydrogen atoms of two positions in the m plane normal to the a-axis at a distance of 0.27 Å from the twofold axis. The O-H distance equals 0.97(3) Å, the O-H?O angle, 135°. The average Fe-O distance in octahedra is 2.022 Å.     

The 1:1 crystal complex of salicylic acid and urea

The 1∶1 crystal complex of salicylic acid (C₇H₆O₃) and urea (CH₄N₂O), mp 121° C, is monoclinic, with space groupC2/c (C ₂ ⁶ h, No. 15) and unit cell dimensionsa=22.206(3),b=5.108(1),c=17.177(2) Å,β=106.18(1)°.d _calc=1.407 g cm^?3,d _meas=1.41 g cm^?3 forZ=8. The structure was determined by direct methods and refined by a full-matrix least-squares procedure to giveR=0.057 andR _w =0.050 for 1652 integrated intensities above 2σ(I). The structure contains a strong OH?O hydrogen bond with O?O distance 2.54 Å in which the carboxyl OH group is donor and urea oxygen atom is acceptor. There are two NH?O intermolecular hydrogen bonds with N?O distances of 2.90 and 2.96 Å. Additionally, the salicyclic acid contains an intramolecular OH?O hydrogen bond of 2.56 Å.     

X-ray structure analysis of 5N-ethyl-8-carboxy-9-oxo-11-methyl-pyrido[2,1-b]quinazoline

The crystal structure of 5N-ethyl-8-carboxy-9-oxo-11-methyl-pyrido[2,1-b]quinazoline (C₁₆H₁₆N₂O₃) has been determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system (space group P2₁/c) with the unit cell parameters a = 9.775(1) Å, b = 15.868(1) Å, c = 9.799(1) Å, β = 113.50(1)°, Z = 4. The benzene ring is planar, the pyrimidine ring exists in 11β-sofa conformation, and the pyridone ring deviates slightly from planarity. The crystal packing exhibits intra-and intermolecular interactions of the O-H?O, C-H?O, and C-H?N types.     

Crystal structures of molecular complexes of 18-crown-6 with 2-aminobenzoic and 5-amino-1-benzyl-1,2,3-triazole-4-carboxylic acid hydrazides

The crystal structures of two host-guest molecular complexes of 18-crown-6 with 2-aminobenzoic acid hydrazide monohydrate (the ratio host: guest: H₂O = 1: 2: 2) (complex I) and 5-amino-1-benzyl-1,2,3-triazole-4-carboxylic acid hydrazide (the host: guest ratio = 1: 2) (complex II) are determined by X-ray diffraction analysis. Crystals I are monoclinic, a = 8.468(2) Å, b = 17.378(3) Å, c = 10.517(2) Å, β = 96.88(3)°, space group P2₁/n, and R = 0.0393 for 6692 reflections. Crystals II are orthorhombic, a = 18.489(1) Å, b = 10.192(3) Å, c = 20.412(2) Å, space group Pbca, and R = 0.0540 for 3513 reflections. In both complexes, the centrosymmetric 18-crown-6 and guest molecules are joined together through the NH?O (crown) hydrogen bonds, which involve all the hydrogen atoms of the hydrazine group. The NH?O=C intramolecular hydrogen bond is observed in the guest molecule. In structure I, the water molecule serves as a bridge between the guest molecules related by the glide-reflection plane and combines the guest-host-guest complexes into layers. In structure II, the guest molecules are linked into chains through hydrogen bonds of the NH?O=C type; in turn, the chains composed of guest molecules and the crown ether molecules bonded to these chains form a layered structure.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

X-ray structure analysis of 3β-hydroxy-4-(1,4-oxazin-4-yl)-androstane (C31H54NO2)

The crystal structure of 3β-hydroxy-4-(1,4-oxazin-4-yl)-androstane (C₃₁H₅₄NO₂) has been determined by X-ray crystallographic techniques. The compound crystallizes in the orthorhombic space group P2₁2₁2 with the following unit-cell parameters: a = 7.124(1) Å, b = 10.127(1) Å, c = 40.660(1) Å, V = 2933.4(1) ų, and Z = 4. The structure has been solved by direct methods and refined to an R factor of 0.067. Three six-membered rings, A, C, and E, exist in the chair conformation, while the ring B adopts a distorted half-chair conformation. The five-membered ring, D, has a distorted envelope conformation. The crystal structure is stabilized by strong intermolecular O-H...O hydrogen bonds.     

Crystal structure of the supramolecular system of indole-2,3-dione 1-(2-oxopropyl)-3-ethylene ketal and its thiosemicarbazone

The crystal structure of a supramolecular system consisting of indole-2,3-dione 1-(2-oxopropyl)-3-ethylene ketal (I) and indole-2,3-dione 1-(2-oxopropyl)-3-ethylene ketal thiosemicarbazone (II) molecules that are linked together by hydrogen bonds is determined using X-ray diffraction. The crystal is monoclinic, and the unit cell parameters are as follows: a = 12.8360(3) Å, b = 10.7330(3) Å, c = 19.4610(3) Å, β = 99.566(1)°, space group P2₁/c, and Z = 4 (C₂₇H₂₉N₅O₇S). In molecules I and II, the indole-2,3-dione 3-ethylene ketal fragments have a virtually identical structure. The pyrrole and dioxolane fragments are spiro-linked through the carbon atom with a dihedral angle close to 90°. The adjacent pyrrole and benzene rings are coplanar to within 4.4°. In molecule II, the oxygen atom of the dioxolane fragment and the terminal nitrogen atom of the thiosemicarbazide fragment are involved in the N-HïO intramolecular hydrogen bond [3.294(2) Å]. The key role in the formation of the crystal structure is played by intermolecular hydrogen bonds of the N-H?dO, C-H?O, C-H?N, and N-H?S types.     

Crystal structure of [N-(2-carbamoylethyl)iminodiacetato]-aqua(1,10-phenanthroline)cobalt(III) chloride 3.5 hydrate

The crystal structure of [N-(2-carbamoylethyl)iminodiacetato]-aqua(1,10-phenanthroline) cobalt(III) chloride 3.5 hydrate [Co(Ceida)(H₂O)(Phen)Cl · 3.5H₂O (I) has been determined by ¹H NMR technique and X-ray diffraction analysis. The crystals are triclinic, a = 10.352(2) Å, b = 12.534(3) Å, c = 20.665(4) Å, α = 107.02(3)°, β = 92.22(3)°, γ = 111.63(3)°, Z = 4, space group $P\bar 1$ , andR = 0.0438. The unit cell involves two crystallographically nonequivalent but virtually identical cationic complexes [Co(Ceida)(H₂O)(Phen)]⁺. The tridentate chelate ligand Ceida ^2? (N + 2O) occupies the face in the coordination octahedron of the Co atom, and the propionamide group remains free. The mean bond lengths are as follows: Co-O_Ceida, 1.876 Å; Co-N_Ceida, 1.981 Å; Co-N_Phen, 1.945 Å; and Co-O_w, 1.915 Å. In the structure, the arrangement of cationic complexes and certain water molecules exhibits a pseudosymmetry (the 2₁ axis). The cations and water molecules are located in the layers, and the anions are arranged between the layers. The structural elements are linked by hydrogen bonds and van der Waals interactions.     

Crystal Structure of 4-(8-chloro-[1,2,4]triazolo[4,3-α]pyridin-3-yl)phenol

The title compound 4-(8-chloro-[1,2,4]triazolo[4,3-α]pyridin-3-yl)phenol was structurally characterized by X-ray crystal structural analysis. The crystals are triclinic, space group P-1 with a = 7.307(3), b = 11.792(4), c = 12.474(5) Å, α = 83.850(10), β = 87.148(13), γ = 77.691(11)°, V = 1043.6(6) ų, Z = 2, F(000) = 504, D_c = 1.564 g/cm³, μ = 0.350 mm^?1, the final R = 0.0433 and wR = 0.1232. A total of 10,746 reflections were collected, of which 4920 were independent (R_int = 0.0357). In the crystal packing diagram, intermolecular O-H…Cl and C-H…O hydrogen bonds stabilize the solid state of the title compound.     

Synthesis and crystal structure of bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl)copper(II)

The title compound, bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl) copper(II), [Cu(C₁₇H₁₁NOCl)₂] (1) was synthesized and its crystal structure was determined. The Compound 1 is monoclinic, space group P2 ₁/c with a = 9.146(3) Å, b = 18.724(3) Å, c = 16.230(2) Å, β = 96.46(1)°, V = 2761.8(11) ų, Z = 4, D _c = 1.503 g cm^?3, μ(Mo Kα) = 1.020 mm^?1, R = 0.0606 for 2361 reflections [I > 2σ(I)]. In the title compound, the Cu atom is coordinated by an N₂O₂ donor set from the imine-phenol ligand in a slightly distorted square planar coordination geometry, with the two phenolate O atoms being deprotonated. The Cu–O bond lengths are 1.878(4) and 1.889(4) Å, the Cu–N bond lengths are 1.980(5) and 1.985(5) Å. The angles O1–Cu–N1 and O2–Cu–N2 are 90.96(19) and 90.72(19)°, respectively.     

Crystal and molecular structures of complex between ammonium iodide monohydrate and the cis-syn-cis isomer of dicyclohexano-18-crown-6

The structure of the [(DCH-6A ? NH₄)(H₂O)I]₂ complex obtained by the reaction between the cis-syn-cisisomer of dicyclohexano-18-crown-6 (DCH-6A) and NH₄I has been determined by X-ray diffraction analysis. The crystals are triclinic, a = 9.314(3) Å, b = 11.951(2) Å, c = 12.040(1) Å, α = 77.36(1)°, β = 81.59(1)°, γ = 80.41(2)°, space group $P\bar 1$ , Z = 2, and the final R factor is 0.044. The structure is built up of the (DCH-6A ? NH₄) + cationic complexes, iodide anions, and water molecules. The ammonium ion forms three hydrogen bonds of the NH?O type [N?O, 2.881(5)–2.890(5) Å] with the oxygen atoms of the crown ether molecule. The organic cations are joined together into centrosymmetric dimers through the system of hydrogen bonds of the NH?OH type. The I^??O distances (where the O atom belongs to the bridging water molecule) fall in the range 3.558(4)–3.610(4) Å.     

An X-ray diffraction refinement of the crystal structure of natural apophyllite

The crystal structure of apophyllite (Andersberg — GDR), with a = 8.966(2), c = = 15.767(1) Å, P4/mnc, z = 2, Q = 2.35 gm · cm⁻³, has been refined (R = 0.035) by least squares with 976 reflections collected with a diffractometer. Apophyllite is a sheet structure with the bringing Si O bond lengths 1.6236 Å, while the non-bridging bond length Si O(3) is 1.5843 Å. The two independent Si O Si angles are 140.09, 140.76 degrees. The mean Si O bond length is 1.6138 Å. As it was not possible to locate unequivocally the H-atoms with the X-ray data, the interpretation of the of water in the structure was based on the charge balance approach of DONNAY and ALLMAN . Assuming that the fluorine ion is bonded to calcium ion (Ca-F = = 2.416 Å) and to H3 atom (F-H3 = 0.9145(1) Å) and water molecule hydrogen bonded to silicate framework. The average bond distances O-H are 0.962(2) Å and angle 105.24(1)°.     

Crystal structure of nacrite from the electron diffraction data

The crystal structure of the nacrite mineral of the kaolin group (space group Cc; R = 2.76%; 634 unique reflections) is refined from the digital oblique-texture electron diffraction patterns obtained with the use of imaging plates. The maxima characterizing the locations and potentials of the hydrogen atoms of the hydroxyl groups are revealed from the difference Fourier-potential syntheses. The O-H interatomic distances and the angles of inclination of the O-H bond with respect to the ab plane are equal to 0.97 Å and ?18.3° for the inner hydroxyl group and 0.92, 0.85, 0.93 Å and 60.8°, 67.8°, 58.4° for the outer hydroxyl groups, respectively. The O_donor-O_acceptor interatomic distances are 2.940, 2.949, and 3.121 Å. It is established that the electrostatic potential distributions of the hydrogen atoms of the inner hydroxyl group and one of the outer hydroxyl groups located in the vicinity of the symmetry pseudoplane m of the layer are characterized by anisotropy, which can indicate a statistical distribution of these hydrogen atoms.     

Synthesis and IR and NMR spectroscopic studies of amino derivatives of oxo-, thio-, and selenopyrazole. Crystal and molecular structure of 1-phenyl-3-methyl-4-methylene-(N-8-aminoquinoline)-5-oxopyrazole

Three compounds of the pyrazole series—o-oxo, thio, and seleno derivatives—have been synthesized and characterized by IR and NMR spectroscopy. The crystal structure of the oxo derivative is determined (Syntex P2₁ diffractometer, MoK _α radiation, graphite monochromator, θ/2θ scan mode, 2θ_max = 57°, direct method, anisotropic—isotropic (H) least-squares refinement for 2015 reflections, R = 0.043, wR2 = 0.1084). The crystals are monoclinic, a = 7.543(1) Å, b = 7.850(2) Å, c = 27.909(6) Å, β = 93.79(3)°, Z = 2, and space group P2₁/c. It is found that the o-hydroxyazomethine derivatives of the pyrazolone series exist in the crystal as 4-aminomethylene-5-oxo tautomers. The proton is localized at the exocyclic N atom. It lies in the plane of the main molecular fragment and participates in the intramolecular bifurcate N—H?O(N) hydrogen bond, which closes the six-membered and five-membered H-rings, respectively.     

Synthesis and crystal structure of 3-ammonium-4-hydroxyphenyl sulfonate hemihydrate

The crystal structure of 3-ammonium-4-hydroxyphenyl sulfonate hemihydrate C₆H₃(NH₃)(OH)SO₃ · 0.5H₂O is determined by single-crystal X-ray diffraction. The unit cell parameters are as follows: a = 11.2395(3), b = 10.3814(3), c = 13.7509(4) Å, β = 100.326(1)°, V = 1578.49(8) ų, space group P2₁/n, Z = 4. The crystal structure can be described us a succession of infinite corrugated layers parallel to ab plane. These layers consist of rings formed by four sulfonate molecules located around a center of symmetry. The rings are connected to each other and to water molecules via O-H...O hydrogen bonds. The structure is further stabilized by π-π interactions between phenyl rings of organic entities of successive layers.