Crystal and molecular structure of 2-(<Emphasis Type="Italic">o</Emphasis>-hydroxyphenyl)-4,6-diphenylpyridine

Crystal and molecular structure of 2-(o-hydroxyphenyl)-4,6-diphenylpyridine C₂₃H₁₇NO (I) has been studied by single crystal XRD. The structure (monoclinic, space group P2₁/c, a = 8.757(2) Å, b = 20.682(4) Å, c = 9.743(2) Å, β = 108.14(2)°, Z = 4) was solved by the direct method and refined anisotropically in the full-matrix approximation to R = 0.076 using all 2660 measured independent reflections (automated diffractometer CAD-4, CuK_α). OH group of the molecule of I is disordered in the crystal over three positions with occupation factors 70%, 15% and 15%. The structure contains a very strong intramolecular hydrogen bond O-H?N disordered over three directions.     

Theoretical and experimental study of molecular structure and vibrational spectra of <Emphasis Type="Italic">N</Emphasis>-(2-pyridylmethyl)-2-pyrazinecarboxamide

N-(2-Pyridylmethyl)-2-pyrazinecarboxamide was prepared and its crystal structure was investigated by X-ray analysis. The compound crystallizes in the triclinic space group \(P{\bar 1}\) with a = 4.262(3), b = 12.117(9), c = 20.840(18) Å, α = 91.802(6), β = 89.834(7), γ = 91.845(6)°, V = 1075.2(16) ų, Z = 4, and D = 1.323?Mg/m³. The structure was solved by direct method and refined to R = 0.0699 and wR ₂ = 0.1268 by full matrix anisotropic least-squares method. Using the Hartree-Fock and density functional method (B3LYP) with 6-31G(d) basis set, the molecular geometry and vibrational frequencies of the title compound has been investigated and compared with experimental ones from experimental studies. The optimized bond lengths obtained by RHF method and bond angles obtained by B3LYP method show better agreement with the experimental values. The vibrations computed of the title compound by the RHF and DFT methods are in good agreement with the observed IR spectra data.     

Crystal structure of <Emphasis Type="Italic">tris</Emphasis>-(dipivaloylmethanato) (ethylendiamine)yttrium(III)

The structure of a mixed-ligand complex tris-(dipivaloylmethanato)(ethylendiamine)yttrium(III) [Y(en)(dpm)₃] is studied at 150(2) K by single crystal XRD. The crystallographic data for C₃₅H₆₅N₂O₆Y are as follows: space group P2₁/c, a = 10.3771(3) Å, b = 26.3566(8) Å, c = 14.8412(4) Å, β = 100.385(2)°, V = 3992.6(2) ų, Z = 4. The structure is molecular. The coordination environment of yttrium atoms is square antiprismatic; the Y–О distances are 2.2597(13)-2.3760(12) Å and Y–N distances are 2.5381(16) Å and 2.5499(17) Å.     

Synthesis and crystal structure of 1-ethyl-3-(phenyl)-1,2,3-triazolium percholorate

The isolation of stable carbenes of the Arduengo (1a) and Wanzlick (2a) type has prompted us to look for stable nitrenium ions of the related structural type 1-ethyl-3-(phenyl)-1,2,3-triazolium perchlorate (6⁺). The title compound C₁₀H₁₄Cl N₃O₄ was isolated and structure was investigated by X-ray crystallography. It crystallizes in the monoclinic space group P2₁/c with cell parameters a=6.697(4) Å, b=9.724(9) Å, c=19.844(2) Å and Z=4. The final residual factor is R1=0.0471 for 1545 reflections with I>2σ(I). The structure exhibits intermolecular hydrogen bonds.     

Crystal structures of <Emphasis Type="Italic">trans</Emphasis>-[Re<Subscript>6</Subscript>S<Subscript>8</Subscript>(CN)<Subscript>2</Subscript>L<Subscript>4</Subscript>] complexes,L = pyridine or 4-methylpyridine

The structures of three novel octahedral rhenium cluster compounds [Re₆S₈(CN)₂(py)₄]·H₂O (1), [Re₆S₈(CN)₂(4-Mepy)₄] (2), [Re₆S₈(CN)₂(4-Mepy)₄]·4-Mepy (3) (py = pyridine, 4-Mepy = 4-methylpyridine) are determined by X-ray crystallography. Crystal data are: C2/m space group, a = 14.813(1) Å, b = 14.772(1) Å, c = 9.2122(6) Å, β = 119.085(2)°, V = 1761.7(2) ų, d _x = 3.318 g/cm³, R = 0.0585 (1); I4₁/amd space group, a = 16.0018(3) Å, c = 14.7186(5) Å, V = 3768.81(16) ų, d _x = 3.169 g/cm³, R = 0.0489 (2); P2₁/c space group, a = 9.0452(4) Å, b = 15.8065(7) Å, c = 15.2951(6) Å, β = 103.700(2)°, V = 2124.57(16) ų, d _x = 2.957 g/cm³, R = 0.0245 (3). Molecular cluster complexes interact via π-π stacking affording 3D frameworks in 1 and 2 and chains in 3.     

The crystal and molecular structure of Ni(II) complex with 1-(2-carboxyphenyl)-3-isopropyl-5-(benzimidazole-2-yl)formazane

The binuclear Ni(II) 1-(2-carboxyphenyl)-3-isopropyl-5-(benzimidazole-2-yl)formazanate (Ni₂L₂ · 2H₂O) (I) was synthesized and its crystal and molecule structures were determined by X-ray diffraction. Crystals I are triclinic: space group P \(\bar 1\), a = 7.4811(11), b = 10.8821(15), c = 11.4168(13) Å, α = 105.690(11) Å, β = 90.537(11) Å, γ = 93.166(11) Å, V = 893.2(2) ų, ρ(calcd.) = 1.581 g/cm³, Z = 1.     

Crystal and molecular structure of <Emphasis Type="Italic">tris</Emphasis>(<Emphasis Type="Italic">m</Emphasis>-chlorophenyl)phosphine selenide

The crystal and molecular structure of tris(m-chlorophenyl)phosphine selenide, C₁₈H₁₂Cl₃PSe (I), was investigated by X-ray diffraction (XRD) analysis. The trigonal rhombohedral structure of I (space group \(R\overline 3 c\), a = 14.110(2) Å, c = 32.360(4) Å, Z = 12) was solved by direct methods and refined by least squares in an anisotropic approximation (R = 0.029) for 1319 averaged measured reflections (CAD-4 automatic diffractometer, λCuK_α).     

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.     

Crystal structure of WI<Subscript>4</Subscript>

Tungsten tetraiodide WI₄ (1) is produced by a high-temperature reaction of WTe₂ and I₂ in a vacuum sealed ampoule. The crystals of 1 belong to the triclinic crystal symmetry, space group P-1, Z = 4, a = = 7.9291(3) Å, b = 10.7695(4) Å, c = 10.8117(4) Å, α = 85.668(1)°, β = 71.772(1)°, γ = 71.559(1)°, V = = 831.60(5) ų, d_calc = 5.523 g/cm³. The structure of 1 consists of tetrameric W₄I₁₆ molecules in which W atoms are in a distorted octahedral environment formed by I atoms.     

Structure of A Coordination Polymer [Cu(En)<Subscript>2</Subscript>CrO<Subscript>4</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript>

The crystal structure of [Cu(En)₂CrO₄]_n (En is ethylenediamine) is determined: a = 14.7359(4) Å, b = 9.8083(3) Å, c = 14.2664(4) Å, V = 2061.98(10) ų, space group Cmce, Z = 8, d_x = 1.931 g/cm³. It is demonstrated that the studied phase is isostructural with [Сu(Еn)₂SO₄]_n. A pseudotetragonal copper atom coordination (Cu–N 2.0204 Å and 2.0244 Å, ∠N–Cu–N 84.73°) is completed to distorted octahedral by two oxygen atoms of chromate anions (Cu–O 2.433 Å and 2.380 Å).     

New binuclear complex of bis(2,4,6,8-tetramethyl-2,4,6,8- tetraazabicyclo(3.3.0)octane-3,7-dione-<Emphasis Type="Italic">O,O</Emphasis>')-diaquatetrakis(nitrato-<Emphasis Type="Italic">O,O</Emphasis>')-dimanganese(II) monohydrate: Synthesis and crystal structure

The centrosymmetric binuclear manganese(II) nitrate complex with a bicyclic bis-carbamide, namely, 2,4,6,8-tetramethyl-2,4,6,8-tetraazabicyclo(3.3.0)octane-3,7-dione, or mebicar (Mk) [Mn(C₈H₁₄N₄O₂)(H₂O)(NO₃)₂]₂ · H₂O (I), has been synthesized for the first time. The structure of complex I has been solved (CCDC no. 1435139). Crystals of complex I are monoclinic, space group P2₁/c, a = 12.8108(11) Å, _b = 10.0662(2) Å, c = 18.6367(17) Å, β = 136.512(16)°, V = 1654.0(4) ų, ρcalcd = 1.659 g/cm³, Z = 2. Each manganese atom is coordinated to the two oxygen atoms of two Mk molecules related by the symmetry codes (1–x, 2–y, 1–z) and to two bidentate nitrate anions and one water molecule. The coordination polyhedron of the manganese atom is a strongly distorted pentagonal bipyramid. The Mn···Mn distance in the complex is 8.7261(9) Å.     

Synthesis and structure of bis(1,2-diaminoethane) copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-hydroxybenzoate) monohydrate and <Emphasis Type="Italic">trans</Emphasis>-diaquabis(1,2-diaminoethane)copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-aminobenzoate)

X-ray structural analysis has been performed for two complex compounds: Cu(en)₂(o-HB)₂H₂O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) ų, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)₂(OH₂)₂]²⁺(o-AB^?)₂ (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) ų, P2₁/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment.     

Crystal structure of KPb<Subscript>2</Subscript>Cl<Subscript>5</Subscript> and KPb<Subscript>2</Subscript>Br<Subscript>5</Subscript>

The KPb₂Cl₅ and KPb₂Br₅ crystals are monoclinic (P2₁/c) with a microtwinned structure. X-ray analysis of chloride resulted in the parameters a = 8.854(2) Å, b = 7.927(2) Å, c = 12.485(3) Å; β = 90.05(3)°, d_calc = 4.78(1) g/cm³ (STOE STADI4, MoK_α, 2θ_max = 80°), R₁ = 0.0702 for 4094 F ≥ 4 σ(F) reflections. For bromide, a = 9.256(2) Å, b = 8.365(2) Å, c = 13.025(3) Å; β = 90.00(3)°, d_calc = 5.62(1) g/cm³ (Bruker P4, MoK_α, 2θ_max = 70°), R₁ = 0.0692 for 3076 F ≥ 4 (F) reflections.     

Crystal structure of EuLnAgS<Subscript>3</Subscript> (Ln = Gd and Ho) compounds

The crystal structures of the first prepared EuLnAgS₃ (Ln = Gd and Ho) compounds, which have two polymorphs, were determined by X-ray powder diffraction. α-EuLnAgS₃ phases are isostructural to BaErAgS₃ (monoclinic crystal system, space group C2/m): a = 17.3168(10) Å, b = 3.9683(2) Å, c = 8.3174(4) Å, β = 103.94° (EuGdCuS₃); a = 17.1729(12) Å, b = 3.9367(3) Å, c = 8.2905(6) Å, β = 103.9° (EuHoCuS₃). β-EuLnAgS₃ phases belong to the AgBiS₂ structure type (cubic crystal system, space group Fm-3m): a = 5.739(2) Å (EuGdCuS₃) and a = 5.678 Å (EuHoCuS₃). In the α-EuLnAgS₃ crystal structure, LnS₆ octahedra and AgS₅ trigonal bipyramids share edges to form a three-dimensional (3D) structure with channels accommodating Eu²⁺ ions. A decrease in Ln³⁺ ionic radius gives rise to the crystal-chemical contraction of the 3D structure.     

Synthesis,structure, and physicochemical properties of the Cr(<Emphasis Type="Italic">iso</Emphasis>-Bu<Subscript>2</Subscript>PS<Subscript>2</Subscript>)<Subscript>3</Subscript> chelate compound

A paramagnetic (μ_ef = 3.86 BM) complex Cr(i-Bu₂PS₂)₃ (I) has been synthesized. Single crystals I were grown, and the crystal structure of the compound was determined from X-ray diffraction data (X8 APEX diffractometer, MoK _α radiation, 4516 F _hkl , R = 0.0604). Monoclinic crystals, space group P2₁/n, unit cell parameters a = 14.2665(5) Å, b = 11.4400(4) Å, c = 23.1299(8) Å, β = 90.245(1)°, V = 3775.0(2) ų, Z = 4, d _calc = 1.196 g/cm³. The structure is based on discrete mononuclear molecules. The coordination polyhedron of the Cr atom is a distorted S₆ octahedron formed from the S atoms of three cyclic bidentate ligands — i-Bu₂PS ₂ ⁻ ions. Electron spectroscopy data correspond to the octahedral structure of the CrS₆ chromophore. Original Russian Text Copyright ? 2007 by E. A. Sankova, L. A. Glinskaya, T. E. Kokina, R. F. Klevstova, and S. V. Larionov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 374–378, March–April, 2007.     

Crystal structures of [Zn(SALIMP)(CH<Subscript>3</Subscript>CO<Subscript>2</Subscript>)]<Subscript>2</Subscript> and [Cu(SALIMP)Cl] with 2-[[(2-pyridinylmethyl) imino]methyl]phenol (HSALIMP) as a ligand

Two complexes [Zn(SALIMP)(CH₃CO₂)]₂ (1) and [Cu(SALIMP)Cl] (2) are obtained by the reactions of zinc(II) and copper(II) salts with a tridentate Schiff base ligand 2-[[(2-pyridinylmethyl) imino]methyl]phenol (HSALIMP). Their structure is determined by single crystal X-ray diffraction. Data for complex 1: C₃₀H₂₈N₄O₆Zn₂, CCDC number: 668213, M _r = 671.3, monoclinic, C2/c, with a = 34.670(5) Å, b = 15.266(2) Å, c = 23.464(4) Å, β = 114.045(2)°, V = 11341(3) ų, Z = 16, F(000) = 5504, GOOF(F ²) = 0.894, the final R = 0.0520 and wR = 0.1272 for 10515 observed reflections with I > 2σ(I); complex 2: C₁₃H₁₂N₂OClCu, CCDC number: 668211, M _r = 311.24, triclinic, P-1, with a = 7.4050(8) Å, b = 10.2369(11) Å, c = 16.2873(17) Å, α = 87.728(2)°, β = 87.818(2)°, γ = 78.279(2)°, V = 1207.4(2) ų, Z = 4, F(000) = 632, GOOF(F ²) = 1.077, the final R = 0.0326 and wR = 0.0381 for 4209 observed reflections with I > 2σ(I).     

X-ray diffraction study of the monoclinic modification of [Cu(NH<Subscript>3</Subscript>)<Subscript>4</Subscript>](ReO<Subscript>4</Subscript>)<Subscript>2</Subscript> in the range 100-410 K

The monoclinic modification of [Cu(NH₃)₄](ReO₄)₂ complex salt in the range 100-410 K is studied by single crystal X-ray diffraction. The crystallographic data for 300 K are as follows: a = 10.6123(3) Å, b = 7.5443(2) Å, c = 15.2261(4) Å, β = 108.406(1)°, V = 1156.67(5) ų, space group Р2₁/n, Z = 4, d_x = 3.623 g/cm³. The coordination environment of the Cu atom, being a distorted square formed by four nitrogen atoms with Cu–N of 1.997-2.018 Å, is completed by the contacts with two oxygen atoms Cu…O of 2.472 Å and 2.598 Å. The comparative crystal chemical analysis with the triclinic modification of [Cu(NH₃)₄](ReO₄)₂ known in the literature is performed.     

Crystal structures of <Emphasis Type="Italic">trans</Emphasis>-dichlorobis(ethylendiamine) rhodium(III) with univalent anions

The crystal structures of the compounds trans-[Rh(en)₂Cl₂]Cl₂ · H₅O₂ (I), trans-[Rh(en)₂Cl₂]ClO₄ (II), and trans-[Rh(en)₂Cl₂]ReO₄ (III) are determined. The crystal data are: I, a = 10.860(3) Å, b = 7.795(2) Å, c = 9.023(3) Å; β = 111.56(10)°, P2₁/c space group, Z = 4, d _x = 1.875 g/cm³; II, a = 6.593(2) Å, b = 8.309(3) Å, c = 11.922(4) Å, α = 83.55(10)°, β = 79.80(10)°, γ = 75.38(10)°, P \(\bar 1\) space group, Z = 2, d _x = 2.106 g/cm³; III, a = 6.533(2) Å, b = 16.391(4) Å, c = 12.411(3) Å; β = 98.30(10)°, P2₁/c space group, Z = 4, d _x = 2.749 g/cm³. The compounds are examined by IR spectroscopy and powder XRD. The solubility of the isolated crystalline phases in water decreases in the following order: trans-[Rh(en)₂Cl₂]Cl₂·H₅O₂ > trans-[Rh(en)₂Cl₂]ClO₄ > trans-[Rh(en)₂Cl₂]ReO₄.     

Organometallic coordination polymers based on silver carboxylates: [AgCF<Subscript>3</Subscript>CO<Subscript>2</Subscript>(2,3-Et<Subscript>2</Subscript>Pyz)] and [AgCF<Subscript>3</Subscript>CO<Subscript>2</Subscript>(Bpeta)]

Coordination polymers [AgCF₃CO₂(2,3-Et₂Pyz)](I)(2,3-Et₂Pyz-C₈H₁₂N₂) and [AgCF₃CO₂(Bpeta)] (II) (Bpeta is 4′4-bipyridylethane, C₁₂H₁₂N₂) are synthesized. Their structures are determined. The crystals of compound I are monoclinic, space group P2(1)/n, a = 7.185(1), b = 14.754(1), c = 12.317(1)Å, β = 97.09(1)°, V = 1295.7(2) ų, ρ_calcd = 1.831 g/cm³, Z = 4. Structure I consists of infinite chains of doubled polymeric chains joined by silver carboxylate dimers [[Ag₂(CF₃CO₂)₂(Et₂Pyz)₂]_∞. The coordination polyhedron of Ag⁺ is a distorted tetrahedron. The crystals of compound II are orthorhombic, space group Pbca, a = 13.555(3), b = 13.991(3), c = 16.449(3) Å, V = 3119.5(11) ų, ρ_calcd = 1.725 g/cm³, Z = 8. Doubled polymeric chains with the Ag…Ag bond (3.16 Å) are also formed in structure II. Supramolecular layers are formed in the structure due to the weak π-π-stacking interaction between the aromatic groups of chains. The CF₃CO ₂ ^? anion is weakly bound to Ag⁺ (Ag-O_avg 2.790 Å).     

Single crystal X-ray structure of 2-[({[(4-methylphenyl)sulfonyl]methyl} amino)carbonyl]-1,3-dioxo-2,3-dihydro-1<Emphasis Type="Italic">H</Emphasis>-inden-2-yl 2-thiophenecarboxylate

The title compound 2-[({[(4-methylphenyl)sulfonyl]methyl}amino)carbonyl]-1,3-dioxo-2,3-dihydro-1H-inden-2-yl 2-thiophenecarboxylate is synthesized and studied by the single crystal X-ray diffraction method. The structure of the product is confirmed by IR, ¹H and ¹³C NMR spectroscopy, and mass spectrometry. The structure is solved in the C2/c monoclinic space group with a = 16.739(3) Å, b = 11.087(3) Å, c = 23.194(4) Å, β = 93.32(3)°, V = 4297.2(16) ų, Z = 8, R1 = 0.033 and wR2 = 0.088.