Spectroscopic studies and crystal structure of (E)-N′-(2-hydroxy-3-methoxybenzylidene)isonicotinohydrazide

The structure of compound has also been examined cyrstallographically. It crystallizes in the monoclinic space group P2₁/c with a = 7.673(1), b = 16.251(2), c = 10.874(1) Å, β = 110.42(1)°, V = 1270.7(3) ų, D _x = 1.418 g cm^?3, R ₁ = 0.0349 and wR ₂ = 0.0935 [I > 2σ(I)], respectively. The title compound has been synthesized from the reaction of isonicotinohydrazide with 2-hydroxy-3-methoxybenzaldehyde. It has been characterized by using elemental analysis, MS, IR, ¹H NMR, ¹³C NMR and UV-Visible spectroscopic techniques.     

Crystal structures of double vanadates, Ca9 R(VO4)7 ⋅ III. R = Nd, Sm, Gd, or Ce

The crystal structures of Ca₉ R(VO₄)₇ (R = Nd (I), Sm (II), or Gd (III)) were studied by the Rietveld method. The compounds are isostructural to Ca₃(VO₄)₂ and are crystallized in the trigonal system (sp. gr. R3c, Z = 6). The unit-cell parameters are as follows: for I, a = 10.8720(5) Å, c = 38.121(1) Å; for II, a = 10.8652(5) Å, c = 38.098(1) Å; and for III, a = 10.8631(5) Å, c = 38.072(1) Å. In the structures of I and II, the M(1), M(2), and M(3) positions are statistically occupied by the rare-earth cations and calcium anions. In the structure of III, the Gd³⁺ cations occupy the _M(1) and _M(2) positions. The distributions of the R ³⁺ cations over the positions are characteristic of each structure. The composition of the cerium-ontaining compound Ca_9.81Ce_0.42(VO₄)₇ (a = 10.8552(5) Å, c = 38.037(1) Å) was refined and its crystal structure was solved from the X-ray powder data. In this compound, cerium atoms are in the oxidation states +3 and +4.     

Crystal structures of two platinum-bipyrimidine complexes: Pt(bpm)Cl2·dmf and Pt(bpm)(dmso)(SO4)·H2O

Red Pt(bpm)Cl₂·dmf forms a stacked structure which has Pt…Pt separations of 3.423(2) A and 3.447(2) Å with Pt…Pt…Pt angles of 155.39(3)^o. The unit cell isP-1, witha=6.712(4) A,b=10.0765(6) Å,c=11.551(3) Å, α=106.732(12)^o, β=103.65(4)^o, γ=90.46(3)^o, andZ=2. The structure refined to anR(F) of 0.046 using 181 parameter and 2165 reflections withI>1σ(I). The yellow complex Pt(bpm)(dmso)(SO₄)·H₂O does not stack in the solid state: the shortest Pt…Pt separation is 4.638(2) Å. The unit cell is alsoP-1, witha=8.060(3) A,b=9.560(3) A,c=9.7534(18) Å, α=90.62(2)^o, β=99.43(3)^o, γ=90.66(3)^o, andZ=2. The structure refined to anR(F) of 0.039 using 208 parameters and 3689 reflections withI>1σ(l).     

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 and molecular structure of the membrane-active antibiotic enniatin C

The crystal structure of the cyclic hexadepsipeptide antibiotic enniatin C c[-(L-MeLeu-D-Hyi)₃-], C₃₄H₅₉N₃O₉, was established by X-ray structure analysis (sp. gr. P2₁, a = 20.205(5) Å, b = 8.702(2) Å, c = 25.587(6) Å, γ = 97.0(5)°, V = 4465.3(18) ų, Z = 4, R = 0.089 for 3601 reflections with I > 2σ(I)). The unit cell contains two independent molecules of enniatin C, one ethanol molecule disordered over two positions, and approximately two water molecules occupying four positions and forming hydrogen bonds with each other. The independent antibiotic molecules adopt virtually identical conformations similar to those observed in the structures of enniatin B and its Na,Ni-complex. These conformations are characterized by alternating upward and downward orientations of the carbonyl groups and pseudoequatorial orientations of side radicals. The Leu residues have stretched conformations. The N-methylamide groups of the independent antibiotic molecules face each other, whereas the molecules are displaced by approximately 8.4 Å with respect to each other along the mean planes of the rings.     

Spectroscopic studies and structure of 3-methoxy-2-[(2,4,4,6,6-pentachloro-1,3,5,2λ5,4λ5,6λ5-triazatriphosphin-2-yl)oxy]benzaldehyde

The compound called 3-methoxy-2-[(2,4,4,6,6-pentachloro-1,3,5,2λ⁵,4λ⁵,6λ⁵-triazatriphosphin-2-yl)oxy]benzaldehyde has been synthesized from the reaction of 2-hydroxy-3-methoxybenzaldehyde with hexachlorocyclotriphosphazene. It has been characterized by elemental analysis, MS, IR, ¹H NMR, ¹³C NMR, ³¹P NMR and UV-visible spectroscopic techniques. The structure of the title compound has been determind by X-ray analysis. Crystals are orthorhombic, space group P2₁2₁2₁, Z = 4, a = 7.705(1), b = 12.624(1), c = 17.825(2) Å, R ₁ = 0.0390 and wR ₂ = 0.1074 [I > 2σ(I)], respectively.     

X-ray structure investigation of 1-acetoxy-1-cyano-2-naphthylethylene and 1,1-dicyano-2-naphthylethylene

The crystal structures of 1-acetoxy-1-cyano-2-naphthylethylene (I) and 1,1-dicyano-2-naphthylethylene (II) are determined by X-ray structure analysis. Crystals I are monoclinic; at 25° C, the unit cell parameters are as follows: a = 17.308(6) Å, b = 4.507(1) Å, c = 17.845(5) Å, β = 107.90(2)°, V = 1324.7(7) ų, d _calcd = 1.260 g/cm³, Z = 4, and space group P2₁/n. Crystals II are monoclinic; at 25°C, the unit cell parameters are a = 3.827(1) Å, b = 15.784(4) Å, c = 17.226(2) Å, β = 91.22(2)°, V = 1040.3(4) ų, d _calcd = 1.304 g/cm³, Z = 4, and space group P2₁/n. It is revealed that, in crystal structures of I and II, the molecular stacks characteristic of compounds of this series are formed through stacking contacts along the direction of the smallest lattice parameter.     

Crystal structure and spectral characteristics of 2,4,7-trinitro-9-fluorenone

The crystal structure of 2,4,7-trinitro-9-fluorenone C₁₃H₅N₃O₇ is determined by X-ray diffraction analysis. The crystals are monoclinic, a = 4.024(1) Å, b = 16.763(3) Å, c = 18.250(4) Å, β = 96.32(3)°, V = 1223.6(5) ų, Z = 4, space group P2₁/c, and R = 0.0640 for 605 reflections with I > 2σ(I). The crystal is built of planar isolated molecules. The compound is characterized using IR and electronic absorption spectroscopy.     

Ligand substitution in the halo-bridged diruthenium compound [Ru(CO)3Cl2]2 by 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd). Synthesis, spectral properties, and X-ray diffraction structures of cis(CO), trans(Cl)-RuCl2(CO)2 (bpcd) and cis(CO)-RuCl[C(O)Et](CO)2(bpcd)

The reaction between 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) and the chlorobridged diruthenium complex [Ru(CO)₃Cl₂]₂ (1) proceeds readily at room temperature in CH₂Cl₂ to give the new ruthenium compounds cis(CO),trans(Cl)-RuCl₂(CO)₂(bpcd) (2) and cis(CO)-RuCl[C(O)Et](CO)₂(bpcd) (3) as the major and minor products, respectively. Compound 2 was isolated and fully characterized in solution, and the molecular structure was established by X-ray diffraction analysis. cis(CO),trans(Cl)-RuCl₂(CO)₂(bpcd) crystallizes in the triclinic space P-1, a = 9.931(5) Å, b = 12.093(7) Å, c = 13.529(7) Å, α = 72.886(9)°, β = 74.739(9)°, γ = 76.851(9)°, V = 1478.2(1) ų, Z = 2, and d _calc = 1.556 mg/m³; R = 0.0841, R _w = 0.1880 for 4137 reflections with I > 2σ(I). The chlorine atoms in 2 adopt a trans geometry at the octahedral ruthenium center, with the two CO groups exhibiting a cis orientation and trans to the bpcd ligand. cis(CO)–RuCl[C(O)Et](CO)₂(bpcd) crystallizes as two independent molecules in the unit cell in the triclinic space P-1, a = 9.941(2) Å, b = 14.867(2) Å, c = 22.414(3) Å, α = 80.257(3)°, β = 84.796(2)°, γ = 75.207(3)°, V = 3152.6(8) ų, Z = 4, and d _calc = 1.504 mg/m³; R = 0.0428, R _w = 0.0962 for 8242 reflections with I > 2σ(I). The two CO groups are situated cis to each and are opposite to chlorine and phosphine moieties. The production of the minor propionyl compound 3 is discussed with respect to the trace amount of EtOH that is present in the CHCl₃ solvent that is used in the preparation of [Ru(CO)₃Cl₂]₂.     

X-ray mapping in heterocyclic design: XI. X-ray diffraction study of 1-benzoyl-3-(pyridin-2-yl)-thiocarbamide and the product of its reaction with oxidants

The structures of 1-benzoyl-3-(pyridin-2-yl)-thiocarbamide C₁₃H₁₁N₃O₁S₁ (I) and 2-benzoylimino-1,2,4-thiadiazole[2,3-a]pyridine C₁₃H₉N₃O₁S₁ (II) are studied by X-ray diffraction. Structures I [a = 5.342(4) Å, b = 20.428(5) Å, c = 11.784(4) Å, β = 90.55(2)°, Z = 4, space group P2₁/n) and II [a = 6.258(6) Å, b = 18.068(14) Å, c = 10.185(10) tA, β = 95.45(8)°, Z = 4, space group P2₁/n) are determined by direct methods and refined to R ₁ = 0.0673 and 0.0802, respectively. In structure I, both intramolecular (involving the O atom) and intermolecular (involving the N and S atoms) hydrogen bonds are observed. The latter bonds are responsible for the formation of centrosymmetric molecular dimers. In structure II, a short intramolecular contact (2.168 Å) is observed between the S and O atoms.     

Yttrium barium heptaoxocobaltate YBaCo4O7+δ: Refinement of the structure and determination of the composition

Parameters of the crystal structure of compound YBaCo₄O₇ are refined. The experimental data [3917 reflections measured, 469 unique I _hkl , and 420 observed reflections with I > 2σ(I)] are obtained on a Bruker X8APEX automated diffractometer equipped with a CCD detector [MoK _α, graphite monochromator, θ_max = 33.09°, space group P6₃ mc, a = 6.3058(4) Å, c = 10.2442(7) Å, V = 352.77 ų, Z = 2, d _calcd = 5.404 g/cm³, R ₁ = 0.0183 for 420 observed reflections and 0.0216 for all unique reflections]. The refinement shows that the occupancy factors of all sites of the space group correspond within three standard deviations to the standard values, that is, to the Y: Ba: Co: O = 1: 1: 4: 7 whole-number ratio of elements in the formula of the compound and to the absence of an aluminum impurity in the crystal.     

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 structures and properties of isomers of 3,5-dinitro-(4-acetylphenyl)aminobenzoyl (p-bromophenyl)amide

The para and ortho isomers of 3,5-dinitro-(4-acetylphenyl)aminobenzoyl (p-bromophenyl)amide (I and II, respectively) are synthesized, and their physicochemical properties and structure are investigated. The para isomer I has a higher melting temperature and is less soluble in organic solvents as compared to the ortho isomer II. The electronic absorption spectra indicate that absorption for molecule I occurs at longer wavelengths than for molecule II. A correlation between the physicochemical properties and the crystal structures of compounds I and II is revealed. Crystals I · 0.5C₆H₆ are triclinic; the unit cell parameters are a = 11.760(2) Å, b = 13.958(3) Å, c = 15.012(3) Å, α = 108.01(2)°, β = 103.95(1)°, γ = 92.00(2)°, V = 2258.3(8) ų, space group $P\bar 1$ , and Z = 4. Crystals II are monoclinic; the unit cell parameters are a = 9.302(2) Å, b = 16.380(3) Å, c = 13.480(3) Å, β = 100.09(3)°, V = 2022.1(7) ų, space group P2₁/c, and Z = 4. Structures I · 0.5C₆H₆ and II are characterized by intramolecular and intermolecular hydrogen bonds.     

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.     

Crystal structure of the pyridine salt of gambogic acid

Pyridinium gambogate, (C₅H₆N)⁺(C₃₈H₄₃O₈)^?, crystallizes in space group P2 ₁2₁2₁ with cell parameters a = 9.536(3) Å, b = 18.502(4) Å, c = 22.223(4) Å, Z = 4. The X-ray structural analysis [R(F) = 0.098 for 1714 data with I ≥ σ(I); wR(F ²) = 0.157 for all 3874 independent data] confirms the structure assigned to gambogic acid on the basis of NMR analysis and of the X-ray structure of isomorellin p-bromobenzenesulfonate. A hydrogen bond links the pyridinium nitrogen atom to a carboxylate oxygen atom. The gambogate ion has two distinct faces that differ in polarity. The hydrophobic face is dominated by the alkenyl chains attached to C(2) and C(17) and a segment of the polycyclic ring system. The hydrophilic face includes the carboxylate ion and several oxygen atoms.     

Crystal structures of strontium and barium ethylenediaminetetraacetato cobaltates(III), Sr[CoEdta]2·9H2O and Ba[CoEdta]2·8H2O: Comparison of the structures of complexes in the series M’[CoEdta]2·nH2O (M’ = Mg, Ca, Sr, Ba; n = 7–10)

Cobalt(III) complexes, namely, Sr[CoEdta]₂·9H₂O (I) and Ba[CoEdta]₂·8H₂O (II) (where Edta ^4- is the ethylenediaminetetraacetate ion), are synthesized. The crystal structures of these compounds are determined using X-ray diffraction. Crystals of compound I are triclinic, a = 6.514(1) Å, b = 11.410(2) Å, c = 12.317(2) Å, α = 67.87(1)°, β = 88.73(2)°, γ = 84.22(2)°, V = 843.63(3) ų, Z = 1, space group P1, and R = 0.0295 for 4130 reflections with I > 2σ(I). Crystals of compound II are monoclinic, a = 6.543(2) Å, b = 12.895(3) Å, c = 19.489(4) Å, β = 95.24(3)°, V = 1637.5(5) ų, Z = 2, space group P2₁, and R = 0.050 for 3016 reflections with |F| > 3σ(|F|). The structures of compounds I and II are compared with those of the previously studied complexes Mg[CoEdta]₂·10H₂O (III) and Ca[CoEdta]₂·7H₂O (IV). The crystal structure of the cobalt(III) complex with the strontium cation (I) is topologically similar to the crystal structure of cobalt(III) complex with the calcium cation (IV). The former structure is built up of the two symmetrically independent homochiral anionic complexes [CoEdta]^? (A _I and B _I), the aqua cations [Sr(H₂O)₈]²⁺, and the molecules of crystalization water w _cr. The structure of compound II involves two independent anions [CoEdta]^? (A _II and B _II) with different chiralities (i.e., they are kryptoracemates). The A _II anions are linked via the barium cations into {Ba(H₂O)₇[CoEdta]} _1∞ ⁺ chain agglomerates due to the incorporation of two terminal oxygen atoms O_u of the anions neighboring in the chain into the coordination sphere of the barium atom. All four structures (I–IV) contain stacks composed of the [CoEdta]^? homochiral anions forming layers aligned parallel to the (001) plane. The aqua cations [Sr(H₂O)₈]²⁺, [Mg(H₂O)₆]²⁺, and [Ca(H₂O)₇]²⁺ or the partially hydrated barium cations [Ba(H₂O)₇(O_u)₂]²⁺ (in structure II), as well as water molecules w _cr, are located between the anion layers. The octahedral environment of the cobalt(III) atoms consists of donor atoms (2N and 4O) of the Edta ^4? ligand. The Co-N bonds in the A _I, B _I, A _II, and B _II anions [the mean bond lengths are 1.927(4), 1.921(4), 1.910(6), and 1.921(6) Å, respectively] are considerably longer than the Co-O bonds [the mean bond lengths are 1.908(5), 1.902(5), 1.904(6), and 1.908(6) Å, respectively]. The mean distances Sr-O_w and Ba-O_w in the strontium and barium polyhedra are 2.609(4) and 2.834(8) Å, respectively. The mean distance Ba-O_u is 2.814(7) Å.     

Synthesis and structure of zinc iodide complex with thiocarbamide, [Zn(CH4N2S)2I2]

A complex compound of zinc iodide with thiocarbamide [Zn(CH₄N₂S)₂I₂] is obtained and its structure is studied by X-ray diffraction. Crystals are monoclinic, a = 10.494(2) Å, b = 7.473(2) Å, c = 14.871(4) Å, β = 91.354(18)°, V = 1165.9(5) ų, space group P2₁/c, Z = 4. The structural unit of the crystal is molecular complex [Zn(CH₄N₂S)₂I₂], in which the zinc atom is coordinated by sulfur atoms of two thiocarbamide molecules and two iodine atoms.     

Structure and refinement of the composition of Bi-Sr-Ca-Cu oxide crystals

The composite structure of the red phase, which accompanies the 2212 and 2201 superconducting phases prepared upon cooling of a melt in the Bi-Sr-Ca-Cu-O system, is revealed by scanning electron microscopy and X-ray diffraction analysis. The matrix component in two crystals I and II under investigation has a monoclinic structure with space group C2/m and the unit cell parameters a = 21.832(2) and 21.8142(9) Å, b = 4.3809(4) and 4.3771(2) Å, c = 12.9430(12) and 12.9378(6) Å, β = 102.832(2)° and 102.839(1)°, and V = 1207.0(2) and 1204.45(9) ų, respectively. The composition is described by the general formula Bi₄(Ca_2?x Sr_1.5+x )O_9.5 with x = 0.13(2) for crystal I and x = 0.19(2) for crystal II. The matrix contains intergrowing clusters of the composition Cu₂O. It is demonstrated that the presence of the second component is structurally justified by the commensurability of the systems of body-centered subcells of cations in the host matrix and anion sublattices in the structure of the Cu₂O oxide.     

Crystal and molecular structure of indolizine derivative C22H12O2NBr

The crystal structure of indolizine derivative C₂₂H₁₂O₂NBr (1) is studied using X-ray diffraction. The crystals are monoclinic, a = 12.888(3), b = 8.6250(2), c = 15.479(3)Å, β = 101.6(3)°, V = 1685.5(6) ų, Z = 4, space group P2₁/c and R = 0.0722 for 1292 reflections with I > 2σ(I). Single-crystal X-ray diffraction analysis reveals that the molecule 1 is monomeric and contains four six-membered rings and one five-membered ring. The fused four rings are in the same plane, giving rise to conjugative effect. Hydrogen bonds link the monomers into double chain. Short ring interactions with intrañhain π-π stacking are observed (distance between ring centroids is 3.85 Å, and the dihedral angle between their planes is ?8.7°). The data of IR spectroscopy confirm the formation of the structure.     

Crystal and molecular structure of phenanthrolinium peroxodisulfate dihydrate (C<Subscript>12</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>S<Subscript>2</Subscript>O<Subscript>8</Subscript> · 2H<Subscript>2</Subscript>O

The crystal structure of (HPhen)₂S₂O₈ · 2H₂O is studied using X-ray diffraction. The crystals are monoclinic, a = 23.716(5) Å, b = 10.220(2) Å, c = 13.103(3) Å, β = 128.03(2)°, V = 2501.6(9) ų, Z = 4, space group C2/c, and R = 0.0745 for 1579 reflections with I > 2σ(I). The crystal is built of S₂O ₈ ^2? centrosymmetric anions, HPhen ⁺ cations, and molecules of crystallization water. Hydrogen bonds link the structural units into chains. Within a chain, stacking interactions are observed between the phenanthroline rings (the interplanar spacing between the rings is 3.8 Å, and the dihedral angle between their planes is 8°). The data of IR spectroscopy confirm the formation of the N(Phen)-H bond.