Crystal structure of the molecular adduct of antimony(III) fluoride with L-phenylalanine

The crystal structure of a newly synthesized molecular adduct of antimony(III) fluoride with L-phenylalanine of the composition SbF₃(C₉H₁₁NO₂) is determined for the first time (monoclinic crystal system: a = 5.8742(1) ?, b = 6.2079(1) ?, c = 15.5401(3) ?, β = 90.741(1)°, Z = 2, P2₁ space group). The structure consists of SbF₃ molecules and L-phenylalanine bound into polymer chains by bidentate bridging carboxyl groups of amino acid molecules. Weak Sb⋯F(3)^b bonds organize the adjacent chains into polymer ribbons that are bound into layers by N-H⋯F and N-H⋯O hydrogen bonds.     

Crystal structure of 1,9-dimethyl-4,5-dihydro-6H-pyrido[3’,2’:4,5]thieno[2,3-f] pyrrolo[1,2-a][1,4]diazepin-6-one

A new tetracyclic compound, 1,9-dimethyl-4,5-dihydro-6H-pyrido[3’,2’:4,5]thieno[2,3-f]pyrrolo[l,2-a][1,4]diazepin-6-one (2) was isolated and studied by X-ray crystallography. Compound 2 crystallizes in the orthorhombic system, space group Pna2₁, a = 11.1098(8) ?, b = 8.4815(6) ?, c = 28.367(2) ?, V= 2673.0(3) ?³, Z=8. The crystal structure comprises two crystallographically independent molecules of the compound. They relate as stereoisomers; in each the diazepine ring exhibits a boat conformation. The crystal packing reveals zigzag H-bonded chains with two distinct hydrogen bonds. The H…O distances and N-H…O angles for N3-H3…O1’ are 2.012? and 174°, and for N3’-H3’…O1 are 1.974? and 154°, respectively.     

Synthesis,characterization, and X-ray crystal structures of zinc(II) complexes with schiff bases 2-[(2-isopropylaminoethylimino)methyl]-5-methoxyphenol and N,N-dimethyl-N′-(1-pyridin-2-ylethylidene)ethane-1,2-diamine

Two new zinc(II) complexes, [ZnBr₂L¹] (I) and [ZnBr₂L²] (II), where L¹ is 2-[(2-isopropylaminoethylimino)methyl]-5-methoxyphenol and L² is N,N-dimethyl-N′-(1-pyridin-2-yl-ethylidene)ethane-1,2-diamine, were prepared and characterized using elemental analysis, FT-IR spectroscopy, and X-ray single-crystal diffraction. In complex I, the Zn(II) atom is coordinated by one phenolic O and one imino N atoms of L¹ and two Br atoms, forming a tetrahedral coordination geometry. In complex II, the Zn(II) atom is in a trigonal bipyramidal coordination geometry with the equatorial plane formed by the imino N atom of L² and two Br atoms and with the two axial positions occupied by one pyridine N and one amino N atoms of L². In the crystal structure of I, the mononuclear zinc complex molecules are linked through intermolecular N-H…O and N-H…Br hydrogen bonds, forming chains running along the y axis. The chains are further linked via intermolecular C-H…Br hydrogen bonds. In the crystal structure of II, the mononuclear zinc complex molecules are linked through intermolecular C-H…Br hydrogen bonds, forming a 3D network.     

Synthesis and structure of the cadmium(II) complex [Cd2(Ph(NH2)2)5(DMFA)4](B10H10)2

A new binuclear cadmium(II) complex with neutral ligands, 1,2-diaminobenzene (DMB) and dimethylformamide (DMF), [Cd₂(Ph(NH₂)₂)₅(DMFA)₄](B₁₀H₁₀)₂, was synthesized and studied by IR spectroscopy and X-ray diffraction. The crystals are monoclinic, a = 26.198(3) ?, b = 12.742(3) ?, c = 21.658(3) ?, β = 119.985(10)°, Z = 8, space group C2/c. The distorted octahedral environment of Cd is formed by four nitrogen atoms of three DAB molecules and two oxygen atoms of DMF molecules. Three independent DAB molecules perform different functions: one chelates the Cd atom, another is linked to cadmium as a monodentate ligand, and the third one bridges two Cd atoms, thus forming the dimer. The amino groups of the DAB molecules are involved in the N-H⋯O and N-H⋯N hydrogen bonds and in N-H⋯B and N-H⋯H-B specific interactions with the cluster boron anion. Original Russian Text ? E.A. Malinina, V.V. Drozdova, L.V. Goeva, I.N. Polyakova, N.T. Kuznetsov, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 6, pp. 922–926.     

Hydrogen bonded complexes of cyanuric acid with pyridine and guanidinium carbonate

Hydrogen bonded complexes of cyanuric acid (CA) with pyridine, [C₃N₃H₃O₃:C₅H₅N], 1, and guanidinium carbonate [C₃H₂N₃][C(NH₂)₃],2, have been prepared at room temperature and characterized by single-crystal X-ray diffraction. Structure of 1 shows pyridine molecules substituting the inter-tape hydrogen bond in CA by N-H… N and C-H…O hydrogen bonds. The structure reveals CA-pyridine hydrogen-bonded single helices held together by dimeric N-H…O hydrogen bonding between CA molecules. In2, the CA tapes, resembling a sine wave interact with the guanidinium cations through N-H…O and N-H…N hydrogen bonds forming guanidinium cyanurate sheets.     

Influence of hydrogen bonds on the molecular structure and conformations of two (C30H48O2) pentacyclic triterpene isomers

The structural study of two (C₃₀H₄₈O₂) pentacyclic triterpene (PCTT) isomers is presented. These terpenes, known as 30-hydroxy-lup-20(29)-en-3-one (1) and (11α)-11-hydroxy-lup-20(29)-en-3-one (2), were isolated from Maytenus imbricata Mart. Ex Reissek (Celastraceae). The molecular structure of 1 and 2 differs in the position of the hydroxyl group. Both compounds crystallize in non-centrosymmetric space groups with two molecules in the asymmetric unit. The crystal structure of 1 shows a triclinic P1 space group (a = 9.5518(1) ?, b = 9.7083(1) ?, c = 14.4696(2) ?, α = 93.832(1)°, β = 102.833(1)°, and γ = 103.307(1)°), while compound 2 crystallizes in a monoclinic P2₁ one (a = 13.4439(16) ?, b = 14.4463(14) ?, c = 13.5224(9) ? and β = 99.703(8)°). The two molecules independent by symmetry of 1 differ slightly due to the presence of static disorder in oxygen atoms. In addition, the intermolecular geometries of 1 and 2 were analysed, and in each isomer the crystal packing is stabilized by O-H…O intermolecular hydrogen bonds and van der Waals forces.     

Synthesis of finely disperse nickel particles by thermolysis of complex (N<Subscript>2</Subscript>H<Subscript>5</Subscript>)[Ni(NH<Subscript>2</Subscript>NHCOO)<Subscript>3</Subscript>] · H<Subscript>2</Subscript>O in organic liquids and refinement of crystal structure of this complex

The crystal structure of the complex (N₂H₅)[Ni(NH₂NHCOO)₃] · H₂O (I) was refined using X-ray diffraction data (obtained on an Apex X8 diffractometer, MoK _α radiation, 1830 F _hkl , R = 0.0182). The structure is built of complex anions [Ni(NH₂NHCOO)₃]⁻, cations N₂H₅⁺, and water molecules and is characterized by strong hydrogen bonds N-H…O, O-H…O, and N-H…N. The N₃O₃ coordination polyhedron around a Ni atom is a slightly distorted octahedron. The thermal decomposition of complex I was studied in high-boiling organic liquids. The feasibility of preparing non-pyrophoric nickel powders having particle sizes of up to 20 nm is shown.     

Structure and stereochemical assignment of spheropsidone, a phytotoxin from Diplodia cupressi

Sphaeropsidone is a phytotoxin produced in very large amount from Diplodia cupressi. It crystallizes in the monoclinic P2₁ space group with two molecules in the asymmetric unit. Cell parameters are: a = 4.1280(6) ?, b = 13.161(1) ?, c = 13.333(3) ?, β = 90.14(1)°, Z = 4, D _calc = 1.432 mg/m³ at 173 K. The final refinement converged to R ₁ = 0.0413, wR ₂ = 0.0730 for 1684 observed reflections. In sphaeropsidone, the hydroxyl group and oxirane oxygen atoms are mutually cis positioned. The absolute stereochemistry at the three chiral centres turns out to be 1S,5R,6S. The stereochemical assignment of spaeropsidone is a fundamental basis for the assignment of the absolute configuration of some of its derivatives used in structure-activity relationship studies. No intramolecular hydrogen bonds are found. In the crystal packing, the hydroxyl and carbonyl oxygen atoms are involved in head-to-tail intermolecular hydrogen bonds to form infinite linear chains of molecules running along c. The linear chains are arranged into layers of molecules stacked along a.     

Supramolecular pseudometallacycles in a nickel compound with 4,4-diaminodiphenylmethane: Synthesis and structure of {Ni[(CH2(C6H4NH2)2]2(NO3)2(H2O)2}

The [Ni(DDM)₂(NO₃)₂(H₂O)₂] complex (DDM is 4,4-diaminodiphenylmethane [CH₂(C₆H₄NH₂)₂]) is synthesized, and its structure is determined. The crystals are triclinic, space group P , a = 5.846(1) ?, b = 9.450(2) ?, c = 13.390(3) ?, α = 105.63(3)°, β = 98.13(3)°, γ = 105.84(3)°, V = 666.6(2) ?³, ρ_calcd = 1.553 g/cm³, Z = 2. The Ni(II) ion (in the inversion center) is bound to a distorted octahedral array formed by the nitrogen atoms of the primary amino groups of the DDM molecules and the oxygen atoms of the monodentate nitrato groups and water molecules (Ni(1)-N(3) 2.119(2) ?, Ni(1)-O(1) 2.122(2) ?, Ni(1)-O(w) 2.047(2) ?, angles at the Ni atoms vary in the 85.08(9)°–94.92(9)° interval). The structure contains supramolecular metallacycles formed by the O(w)-H…N(2) hydrogen bonds between the coordinated H₂O molecules and the terminal amino groups of DDM. The metallacycles are joined by the Ni²⁺ ions into infinite chains running in the [111] direction. Original Russian Text ? Yu.V. Kokunov, V.V. Kovalev, Yu.E. Gorbunova, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 11, pp. 1838–1843.     

π-complexes of copper(I) with but-2-yne-1,4-diol. Synthesis and crystal structure of the anionic π-complex (PipH2)[CuCl2(HOCH2C≡CCH2OH)]2 · H2O ((PipH2)2+ is the Piperazinium Cation)

A reaction of but-2-yne-1,4-diol with CuCl in a concentrated aqueous solution of piperazinium dichloride gave the π-complex (PipH₂)[CuCl₂(HOCH₂C≡CCH₂OH)]₂ · H₂O ((PipH₂)²⁺ is the piperazinium cation). The complex was examined by X-ray diffraction analysis (space group P , a = 7.355(1) ?, b = 10.3572(8) ?, c = 13.632(2) ?, α = 101.055(9)°, β = 95.350(1)°, γ = 101.875(9)°, Z = 2). The complex consists of two crystallographically independent anions [CuCl₂(HOCH₂C≡CCH₂OH)]⁻ and the biprotonated piperazinium cation. The trigonal environment of the Cu(I) atom in either complex anion includes is made up of two Cl atoms and the C≡C bond. Apart from the hydrogen bonds N-H⋯O that imparts a directed character to the ionic interaction Cat⁺⋯An⁻, the piperazinium cation with molecules of crystallization water with bridging function form the cross-linking hydrogen bonds N-H⋯OH₂ and OH-H⋯Cl. Original Russian Text ? Yu.I. Slyvka, V.V. Kinzhibalo, T. Lis, B.M. Mykhalichko, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya, 2009, Vol. 35, No. 4, pp. 311–315.     

Tetrahedral complexes of zinc(II) chloride with N- and O-containing organic ligands: Synthesis and crystal structures of [ZnCl2(C12H12N2O)] and [ZnCl2(H2O)2](Me4Pyz)2

New complex chlorides [ZnCl₂(ODA)] (I) (ODA=oxydianiline, C₁₂H₁₂N₂O) and [ZnCl₂(H₂O)₂](Me₄Pyz)₂ (II) (Me₄Pyz = 2,3,5,6-tetramethylpyrazine) were synthesized and crystallographically characterized. Crystals of I are monoclinic, space group C2/c, a = 22.682(2) ?, b = 12.646(1) ?, c = 9.951(1) ?, β = 93.23(2)°, V = 2849.7(5) ?³, ρ_calc = 1.569 g/cm³, Z = 8. Structure I contains cyclic fragments consisting of two tetrahedral complexes (ZnCl₂N₂) and two coordinated bridging oxydianiline ligands. Crystals of II are monoclinic, space group P2(1)/c, a = 8.972(2) ?, b = 13.862(3) ?, c = 17.528(4) ?, β = 101.72(3)°, V = 2134.5(7) ?³, ρ_calc = 1.384 g/cm³, Z = 4. In structure II, supramolecular pseudo-metallocycles are formed due to formation of hydrogen bonds O(w)-H…N between coordinated water molecules and noncoordinated nitrogen atoms of tetramethylpyrazine molecules.     

Synthesis and crystal structure of a new coordination polymer constructed from Dawson-type polyoxotungstate and transition metal complexes [Cu(H2Biim)2]2H2P2W18O62 · 2C2H5OH · 2H2O

A new coordination polymer constructed from Dawson-type polyoxotungstate and transition metal complexes [Cu(H₂Biim)₂]₂H₂P₂W₁₈O₂ · 2C₂H₅OH · 2H₂O (H₂Biim = 2,2′-diimidazole) (I) have been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, and TG analysis. The crystal structure of I contains a Dawson-type [α-P₂W₁₈O₆₂]⁶⁻ polyanion, two metal coordination cations [Cu(H₂Biim)₂]²⁺, two protons, two ethanol molecules, and two lattice water molecules. Interestingly, a three-dimensional supramolecular framework is formed via N-H⋯O hydrogen bonds. Complex I crystallizes in the monoclinic system, space group C2/c with a = 22.742(3), b = 14.780(2), c = 29.637(5) ?, β = 111.199(2)°, V = 9288(2) ?³, T = 296(2) K, Z = 4, μ = 22.774 mm⁻¹, GOOF = 1.017, R ₁ = 0.0590 and wR ₂ = 0.1394.     

Layered structure of the silver coordination polymer with nonrigid aromatic diamine {Ag[CH2(C6H4NH2)2]2(CH3C6H4NH2)}NO3

The complex [Ag(DDM)₂(CH₃C₆H₄NH₂)]NO₃, where DDM is 4,4-diaminodiphenylmethane [CH₂(C₆H₄NH₂)₂], was synthesized and its structure was determined. The crystals are monoclinic, space group P2₁/n, a = 9.543(2) ?, b = 18.056(4) ?, c = 1.901(2) ?, β = 106.94(3)°, V = 1796.8(6) ?³, ρ_calcd = 1.443 g/cm³, Z = 4. The Ag atom (at the inversion center) is coordinated at the vertices of an almost undistorted octahedron by six nitrogen atoms of the primary amino groups from four bridging DDM molecules and two terminal p-toluidine molecules (Ag-N, 2.546(3) ?; NAgN, 89.7–90.3°). Wavelike layers composed of conjugate multiunit metal rings, each containing four Ag⁺ ions and four bridging DDM ligands, are formed in the structure in the [101] direction (a 2D polymer). Uncoordinated NO ₃ ⁻ anions are arranged in the cavities between the layers and link them by N-H⋯O hydrogen bonds. Original Russian Text ? Yu.V. Kokunov, V.V. Kovalev, Yu.E. Gorbunova, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 12, pp. 1992–1998.     

Molecular and crystal structures of [FeCl(HMPA)3(H2O)2]2+(FeCl4) 2? · 3HMPA

IR and single-crystal X-ray diffraction study are carried out for compound, C₃₆H₁₁₂Cl₉Fe₃N₁₈O₈P₆(I). It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 14.2992(3), b = 21.4351(4), c = 25.5407(5) ?, V = 7828.3(3) ?³, ρ_calcd = 1.553 g/cm³, Z = 4. The FeCl fragment is coordinated with chlorine atom of two water molecules and three HMPA molecules to form a cation, with a distorted octahedral coordinate geometry. In the crystal I, the cation is linked with HMPA by the O-H…O hydrogen bond. The chiral crystal is formed through self-assembly even from achiral molecules.     

Crystal Structure of Iridium(III) trans-Trifluoroacetylacetonate

Single crystal X-ray diffraction analysis is used to determine the structure of iridium(III) trans- trifluoroacetylacetonate at 150 K. The crystallographic data for trans- C₁₅H₁₂F₉O₆Ir are as follows: a =13.4334(5) ?, b = 14.9136(6) ?, c = 19.4229(8) ?, space group Pcab, V = 3891.2(3) ?³, Z=8, d_x = 2.224 g/cm³, R = 0.0236. The structure is molecular. The metal atom coordinates six oxygen atoms of three β-diketonate ligands of β-diketone. The Ir-O distances are within the range of 2.00 ? to 2.02 ?; the average value is 2.011(6) ?; the average value of the chelate angle∠O-Ir-O is 95.2(5)°. In the crystal, the molecules are bound only by van der Waals interactions; six shortest Ir…Ir distances in the structure are within the range of 7.469-9.712 ?.     

1-Allyl derivatives: Synthesis and crystal structures for [(NH2C5H4N(C3H5))2Cu3Cl3(NO3)2] and [C9H7N(C3H5)Cu(NO3)2]

1-Allyl-4-aminopyridinium chloride reacts with Cu(NO₃)₂ · 3H₂O in an ethanolic solution under the conditions of ac electrochemical synthesis at copper electrodes to form crystals of compound [(NH₂C₅H₄N(C₃H₅))₂Cu₃Cl₃(NO₃)₂] (I). The crystals of compound I are monoclinic: space group P2₁/c, Z = 4, a = 25.770(7), b = 7.230(4), c = 12.505(5) ?, β = 92.58(3)°, V = 2328(2) ?³. The direct interaction of 1-allylquinolinium nitrate with Cu(NO₃)₂ · 3H₂O in a methanolic solution in the presence of metallic copper yields crystals of compound [C₉H₇N(C₃H₅)Cu(NO₃)₂] (II). The crystals of compound II are triclinic: space group P , a = 6.756(3), b = 8.391(4), c = 12.489(5) ?, α = 77.18(3)°, β = 89.48(4)°, γ = 73.32(3)°, V = 662.0(5) ?³. The structure of compound I is built of infinite linear anions: polymeric fragments {(NH₂C₅H₄N(C₃H₅))₂Cu₃Cl₃(NO₃)₂} _n . Each of two copper atoms (Cu(1) and Cu(2)) π-coordinates the C=C bonds of the allyl groups of the 1-allyl-4-aminopyridinium cations, the oxygen atom of the nitrate ions, and two chlorine atoms. The third copper atom Cu(3) is linearly linked with two chlorine atoms. Particular polymeric fragments are additionally joined by the N-H…O, C-H…O, C-H…Cl hydrogen bonds. The crystal structure of compound II is built-up of the isolated L₂Cu₂(NO₃)₄ fragments (L is the 1-allylquinolinium cation). The metal atom is localized in the trigonal pyramidal coordination environment of three oxygen atoms of the nitrate ions and of the C=C bond of the allyl group of the cation. The particular L₂Cu₂(NO₃)₄ fragments are additionally joined by the C-H…O hydrogen bonds. Original Russian Text ? A.V. Pavlyuk, T. Lis, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya, 2009, Vol. 35, No. 6, pp. 458–462.     

The coordination polymer triaquabarium-μ-bis(citrato)germanate trihydrate: Synthesis, properties, and molecular and crystal structure of {[Ge(μ-HCit)2Ba(H2O)3] · 3H2O}n

The polymeric coordination compound {[Ge(μ-HCit)₂Ba(H₂O)₃] · 3H₂O} _n (H₄Cit = citric acid) was obtained for the first time for germanium(IV) citrates. The compound was characterized by elemental analysis, thermogravimetry, IR spectroscopy, and X-ray crystallography. Crystals of the compound are triclinic, a = 7.422(4) ?, b = 10.668(4) ?, c = 14.342(6) ?, α = 91.31(3)°, β = 95.81(4)°, γ = 104.08(4)°, V = 1094.5(8) ?³, Z = 2, space group P $ \bar 1 $ \bar 1 , R1 = 0.0479 for 2284 reflections with I > 2σ(I). Two crystallographically independent octahedral [Ge(HCit)₂]²⁻ anions are linked by Ba²⁺ ions to form a polymeric chain. The coordination number of Ba atoms is equal to 9. The chains are linked to each other and crystal water molecules by hydrogen bonds.     

Crystal structure of L-leucinium tetrafluoroantimonate(III)

The crystal structure of L-leucinium tetrafluoroantimonate(III) of the composition (C₆H₁₄NO₂)SbF₄ (orthorhombic symmetry: a = 6.1459(6) Å, b = 14.994(1) Å, c = 24.789(2) Å, Z = 8, P 2₁2₁2₁ space group) synthesized for the first time is determined. The (C₆H₁₄NO₂)SbF₄ structure represents a new structure type of tetrafluoroantimonate(III). It is formed by (C₆H₁₄NO₂)+ cations and chain complex [Sb₂F₈]_n ²ⁿ anions composed of Sb₂F₈ dimers linked into chains by bridging F atoms. The Sb₂F₈ dimers consist of SbF₃ and SbF₅ groups bound by bridging fluoride atoms of the SbF₅ group. Chains in the structure are linked by N-H…F, N-H…O, and O-H…F hydrogen bonds into a three-dimensional framework.     

Crystal structure of a new mononuclear complex of Mn(II) with a bbbi ligand (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene)

A new mononuclear complex Mn(bbbi)₂(H₂O)₄(ClO₄)₂·(bbbi)₂·(H₂O)₂ 1 (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene) is synthesized under hydrothermal conditions and characterized by IR spectroscopy, elemental analysis, and single crystal X-ray structural analysis. Crystal data for 1: triclinic, , a = 8.8478(7) ?, b = 15.0550(11) ?, c = 16.4310(12) ?, α = 108.657(7)°, β = 104.044(7)°, Γ = 99.317(7)°, V = 1942.2(3) ?³, Z = 1, final R = 0.0621. Each manganese atom is octahedrally coordinated by four aqua ligands and two nitrogen atoms of two distinct bbbi ligands. The molecule is stabilized by hydrogen bonding and π…π interactions.