Tetramminenickel hydrogen hexamolybdometalates(III)

Tetramminenickel hydrogen hexamolybdoaluminate and hexamolybdogallate(III) of compositions [Ni(NH₃)₄] · H[AlMo₆O₁₈(OH)₆] · 10H₂O (I) and [Ni(NH₃)₄] · H[GaMo₆O₁₈(OH)₆] · 10H₂O (II) were synthesized and characterized by mass spectrometry, thermogravimetry, X-ray powder diffraction, and IR spectroscopy. Their crystals are triclinic. For compound I, a= 17.30 Å, b= 14.69 Å, c= 10.45 Å, α = 129.07, β = 65.91°, γ = 138.01°, V = 1338.7l ų, ρ_calcd = 2.75g/cm³, Z = 2; for compound II, a = 17.38 Å, b= 14.75 Å, c= 10.51 Å, α = 131.38°, β= 65.96°, γ = 138.09, V = 1338.15 ų, ρ_calcd = 2.68 g/cm³, Z = 2.     

Synthesis and structures of polyiodide acetamide complexes of transition metals

Polyiodides of acetamide complexes of transition elements have been synthesized and studied by X-ray diffraction analysis. Compounds [M(AA)₆][I₁₀] (M = Mn, Fe, Co, Ni, Zn) are isostructural with the earlier studied cadmium compound. The crystals of [Co(AA)₄(H₂O)₂][I₁₂] are monoclinic: a = 17.486(6) Å, b = 15.015(4) Å, c = 7.8309(15) Å, β = 99.87(2)°, V = 2025.6(10) ų, space group C2/m, Z = 4. The crystals of [Ni(AA)₆][I₃]₂ are monoclinic: a = 23.032(9) Å, b = 12.176(4) Å, c = 18.274(5) Å, β = 139.22(3)°, V = 3347.0(19) ų, space group Cc, Z = 4.     

Synthesis and crystal structure of a new Schiff base ligand and its cobalt(II) complex

The crystal structures of cobalt(II) Schiff base complex (Co^IIL₂ · H₂O) and Schiff base ligand 3,5-dichlorosalicylidene-2-chlorophenylmethylamine (HL) have been determined by single-crystal X-ray analysis. The geometry around cobalt in Co^IIL₂ · H₂O is distorted tetrahedral. Co^IIL₂ · H₂O crystallizes in the monoclinic system, in space group C2/c, with crystallographic parameters: a = 12.9143(16) Å, b = 8.8326(16) Å, c = 25.115(3) Å, β = 92.791(10)°, V = 2861.4(7) ų, Z = 4, F(000) = 1420, and the final R indices (I > 2σ(I)) are R ₁ = 0.0440, wR ₂ = 0.1272. HL crystallizes in the monoclinic system, in space group P2₁/c, with crystallographic parameters: a = 11.9764(15), b = 8.2331(10), c = 14.2211(17) Å, β = 98.723(6)°, V = 1386.0(3) ų, Z = 4, F(000) = 640, and the final R indices (I > 2σ(I)) are R ₁ = 0.0397, wR ₂ = 0.1018.     

Synthesis,characterization, and crystal structures of two Schiff base zinc(II) complexes with urease inhibitory activities

Two Schiff base zinc(II) complexes, [ZnBr₂L¹] · 2CH₃OH (I) (I) and [ZnBr₂L²] (II), where L¹ is 4-chloro-2-[(2-piperazin-1-ylethylimino)methyl]phenol and L² is 4-chloro-2-[(3-diethylaminopropylimino)methyl]phenol were synthesized and structurally characterized. The crystal of I is monoclinic: space group P2₁/c, a = 9.831(3), b = 18.680(6), c = 11.879(4) Å, β = 94.660(6)°, V = 2174.3(11) ų, Z = 4. The crystal of II is monoclinic: space group P2₁/n, a = 7.2310(14), b = 16.037(3), c = 15.856(3), β = 90.01(3)°, V = 1838.7(6) ų, Z = 4. The Zn atom in each complex is four-coordinated by one phenolate O and one imine N atoms of the Schiff base ligand and two bromide atoms, forming a tetrahedral coordination. The urease inhibitory activities of the complexes were evaluated.     

Crystal Chemistry Study of Two Magnesium Complexes with Trifluoroacetylacetone

Single crystal X-ray diffraction at a temperature of 150(2) K is used to determine the structures of two magnesium complexes with trifluoroacetylacetone: [Mg(tfac)₂]₃I and [Mg(H₂O)₂(tfac)₂]·H₂O II. Crystallographic data for I: space group P2₁/n, a = 12.5226(10) Å, b = 13.0591(7) Å, c = 12.6034(13) Å, β = 95.243(2)°, V = 2052.5(3) ų, Z = 2; for II: space group P2₁/c, a = 10.826(2) Å, b = 7.0742(13) Å, c = 21.858(4) Å, β = 102.712(5)°, V = 1632.9(5) ų, Z = 4. The isle structure of I is formed by linear trimeric molecules; in the structure of II the molecules of the complex and crystallization water form a layered framework using hydrogen bondings; the coordinated water molecules are in a trans position. The magnesium atoms have a distorted octahedral coordination environment, the Mg–O distances are 1.991(4)- 2.146(4) Å and 2.040(5)-2.073(5) Å in molecules of I and II respectively.     

Investigation of pentaamminechloroplatinum(IV) perrhenate dihydrate

The crystal structure of the [Pt(NH₃)₅Cl](ReO₄)₃·2H₂O salt is determined. Crystallographic data: a = 10.3476(2) Å, b = 12.8955(2) Å, c = 14.3536(3) Å, β = 105.241(10)°, V = 1847.94(6) ų, space group P ₂1/n, Z = 4, d _x = 3.962 g/cm³. Thermal decomposition of the compound is studied in a helium and hydrogen atmosphere. A two-phase product arises in the former case, in the latter a substitution Re_0.75Pt_0.25 solid solution with unit cell parameters: a = 2.767(2) Å, c = 4.441(3) Å, space group P6₃/mmc.     

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.     

Hexafluorosilicates of cobalt(II) complexes with dimethylsulfoxide and dimethylformamide

New double complexes [Co(DMSO)₆][SiF₆] ? 2H₂O (I) and [Co(DMF)₃(H₂O)₃][SiF₆] ? DMF (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction. Crystals of complex I belong to the tetragonal symmetry system, space group R3?, Z = 3, a = 11.8232(3) Å, c = 18.4699(5) Å, V = 2235.97(10) ų, ρ_calc = 1.573 g/cm³. Crystals of complex II are triclinic, space group P1?, Z = 2, a = 8.6264(4) Å, b = 10.1419(4) Å, c = 13.9657(6) Å, α = 100.847(2)°, β = 98.549(2)°, γ = 93.479(2)°, V = 1181.71(9) ų, ρ_calc = 1.539 g/cm³.     

Supramolecular architecture of catechol and its 2:1 complex with dimethylsulfoxide

The crystal structures of catechol (o-dihydroxybenzene) and its 2:1 complex with dimethylsulfoxide are determined at T = 150 K. Crystal data: C₁₄H₁₈O₅S, M = 298.37, triclinic, space group P \(\bar 1\), unit cell parameters: a = 7.7285(13) Å, b = 9.9924(17) Å, c = 10.3188(18) Å, α = 89.963(4)°, β = 89.968(4)°, γ = 69.076(5)°, V = 744.3(2)ų, Z = 2, D _x = 1.331 g/cm³, R1 = 0.048; C₆H₆O₂, M = 110.11, monoclinic, space group P2₁/n, a = 9.8206(6)Å, b = 5.5903(3)Å, c = 10.4439(6)Å, β = 114.952(2)°; V = 519.85(5) ų, Z = 4, D _x = 1.407 g/cm³, R1 = 0.0289. In the 2:1 complex the molecules are joined in a supramolecular ensemble by D-H...A hydrogen bonds (D = O, C; A = O, π); in catechol they are bonded only by O-H...O. The state diagram of the catechol-dimethylsulfoxide system is examined by DTA.     

Structure of Potassium and Cesium Barbiturates

The structures of catena-[K(μ₆-Hba?O,O,O,O′,O′,O″)] (I) and catena-[Cs(μ₆-Hba–O,O,O′,O′,O″,O″)] (II), where Н₂ba is barbituric acid C₄H₄N₂O₃, were characterized by powder X-ray diffraction. Crystallographic data: a = 14.1603 (4) Å, b = 3.68977 (9) Å, c = 10.9508 (3) Å, β = 82.226 (1)°, V = 566.90 (3) ų, space group P2₁/n, Z = 4 for I; a = 14.652 (1) Å, b = 11.7275 (7) Å, c = 3.8098 (3) Å, β = 79.140 (6)°, V = 642.90 (8) ų, space group C2/m, Z = 4 for II. The structural topologies of alkali metal complexes with barbituric acid and some its derivatives were compared. The thermal stability of complexes I and II in an air atmosphere was studied.     

Synthesis and crystal structures of cobalt(III) and zinc(II) complexes derived from 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol with urease inhibitory activity

A new mononuclear cobalt(III) complex, [CoL₂(N₃)]₂ · CH₃OH (I), and a new mononuclear zinc(II) complex, [ZnLCl(CH₃OH)] (II) (HL = 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol), were prepared and structurally characterized by elemental analyses, infrared spectroscopy, and single- crystal X-ray diffraction. The crystal of I is monoclinic: space group P2₁/c, a = 18.742(2) Å, b = 15.197(2) Å, c = 25.646(2) Å, β = 125.996(3)°, V = 5909.8(11) ų, Z = 4. The crystal of II is monoclinic: space group P2₁/c, a = 7.257(1) Å, b = 24.707(2) Å, c = 9.637(1) Å, β = 101.557(2)°, V = 1692.9(3) ų, Z = 4. The Co atom in I is in an octahedral coordination, and the Zn atom in II is in a trigonal-bipyramidal coordination. The urease inhibitory test shows that complex I has strong urease inhibitory activity, while complex II has no activity.     

Hexa(isothiocyanato)chromates(III) of Some Yttrium Group Lanthanide(III) and Europium Complexes with Nicotinic Acid: Synthesis and Crystal Structures

Double ionic complexes [M(C₅H₅NCOO)₃(H₂O)₂][Cr(NCS)₆] · nH₂O, where M = Eu (I), n = 1.15; Dy (II), Er (III), n = 1.5; M = Yb (IV), n = 2, have been synthesized by the reaction between M(NO₃)₃, M = Eu, Dy, Er, Yb, K₃[Cr(NCS)₆], and nicotinic acid (C₅H₅NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals of complexes I–IV are monoclinic, space group P2₁/n, Z = 4; a = 9.5358(2) Å, b = 25.4871(5) Å, c = 15.4303(4) Å, β = 105.513(1)°, V = 3613.6(1) ų, ρ_calcd = 1.799 g/cm³ for I, a = 9.5901(5) Å, b = 25.8599(15) Å, c = 15.6316(9) Å, β = 106.829(2)°, V = 3710.6(4) ų, ρ_calcd = 1.782 g/cm³ for II, a = 9.5640(3) Å, b = 25.8936(11) Å, c = 15.6498(7) Å, β = 106.895(2)°, V = 3708.3(3) ų, ρ_calcd = 1.791 g/cm³ for III, and a = 9.5049(2) Å, b = 25.6378(4) Å, c = 15.5120(3) Å, β = 106.934(1)°, V = 3616.1(1) ų, ρ_calcd = 1.864 g/cm³ for IV.     

Tetranuclear rhenium chalcochloride cluster complexes Cs<Subscript>3</Subscript>H[Re<Subscript>4</Subscript>Q<Subscript>4</Subscript>Cl<Subscript>12</Subscript>] · 3.33H<Subscript>2</Subscript>O (Q = Se and Te): Synthesis and structures

The tetranuclear cluster rhenium complexes Cs₃H[Re₄Q₄Cl₁₂] · 3.33H₂O (Q = Te (I) and Se (II)) with the Cl atoms as terminal ligands were obtained and structurally characterized. The structures of complexes I and II were determined by X-ray diffraction analysis. Their isostructural crystals are monoclinic; space group C2, Z = 6; a = 26.403(8) Å, b = 16.495(5) Å, c = 11.744(3) Å, β = 91.25(2)°, V = 5113(2) ų (I); a = 26.573(3) Å, b = 16.461(3) Å, c = 11.726(2) Å, β = 91.381(4)°, V = 5127.6(14) ų (II).     

Synthesis of spiro[(6-phenyl-3,4-dihydro-2H-1,3-dioxine)-2<Emphasis Type="Italic">R</Emphasis>(<Emphasis Type="Italic">S</Emphasis>), 3′-(19′,28′-oxidooleanan)]-4-ones and X-ray diffraction analysis of their configuration

The structure of two stereoisomeric spiroadducts of allobetulone with 5-phenyl-2,3-dihydrofuran-2,3-dione was established by X-ray diffraction (XRD) analysis. The crystals of the 2R isomer are orthorhombic, P2₁2₁2₁, a = 10.825(5) Å, b = 12.849(6) Å, c = 23.358(9) Å; V = 3249(2) ų, Z = 4, d _calc = 1.200 g/cm³; the crystals of the 2S isomer hemihydrate are triclinic, P1, a = 11.505(7) Å, b = 12.192(8) Å, c = 13.123(8) Å; α = 103.35(5)°, β = 100.80(5)°, γ = 90.98(5)°; V = 1756(2) ų, Z = 2, d _calc = 1.127 g/cm³. The molecular structure of the spiroadducts is discussed.     

Synthesis and study of physicochemical properties of the magnesium heteropoly compound (NH<Subscript>4</Subscript>)<Subscript>4</Subscript>[MgMo<Subscript>6</Subscript>O<Subscript>18</Subscript>(OH)<Subscript>6</Subscript>] · 5H<Subscript>2</Subscript>O

The magnesium heteropoly compound (NH₄)₄[MgMo₆O₁₈(OH)₆] · 5H₂O (I) has been synthesized and studied by mass spectrometry, IR spectroscopy, X-ray powder diffraction, and thermogravimetry. Crystals of I are monoclinic, space group P2₁/n, a = 15.10 Å, b = 11.64 Å, c = 13.53 Å, β = 74.28°, V = 2289.31 ų, ρ_calc = 1.09 g/cm³, Z = 1.     

Spectral and thermal properties,and the crystal structure of 1,4,5,8-naphthalene-tetracarboxylate dinuclear Ni(II) complex

A novel dinuclear Ni^II complex, [Ni₂(ntc)(H₂O)₁₀]·7(H₂O) (1), with 1,4,5,8-naphthaenetetracarboxylate (ntc) has been synthesized and characterized by X-ray diffraction analysis, IR, UV-vis spectra and thermogravimetric analysis. Complex 1 crystallizes in triclinic system, space group P-1, a = 7.721(3) Å, b = 9.458(3) Å, c = 11.453(4) Å, α = 114.110(6)°, β = 92.184(6)°, γ = 107.472(6)°, V = 715.7(4) ų, Z = 1, final R = 0.048. Each nickel atom is octahedrally coordinated by five aqua ligands and one oxygen atom of the bridging ntc connecting two nickel atoms. The resulting dinuclear Ni^II complex forms a 3D H-bonded network.     

Crystal structures of a family of layered coordination polymers containing divalent metal ions (Mn<Superscript>2+</Superscript>, Co<Superscript>2+</Superscript>, Ni<Superscript>2+</Superscript> and Zn<Superscript>2+</Superscript>) and the 3-amino 4-methyl benzoate ion

The syntheses and crystal structures of the layered coordination polymers M(C₈H₈NO₂)₂ [M = Mn (1), Co (2), Ni (3) and Zn (4)] are described. These isostructural compounds contain centrosymmetric trans-MN₂O₄ octahedra as parts of infinite sheets; the ligand bonds to three adjacent metal ions in μ³-N,O,O′ mode from both its carboxylate O atoms and its amine N atom. In each case, weak intra-sheet N–H?O and C–H?O hydrogen bonds may help to consolidate the structure. Crystal data: 1, C₁₆H₁₆MnN₂O₄, M _r = 355.25, monoclinic, P2₁/c (No. 14), a = 10.6534(2) Å, b = 4.3990(1) Å, c = 15.5733(5) Å, β = 95.1827(10)°, V = 726.85(3) ų, Z = 2, R(F) = 0.026, wR(F ²) = 0.067. 2, C₁₆H₁₆CoN₂O₄, M _r = 359.24, monoclinic, P2₁/c (No. 14), a = 10.6131(10) Å, b = 4.3374(4) Å, c = 15.3556(17) Å, β = 95.473(4)°, V = 703.65(12) ų, Z = 2, R(F) = 0.041, wR(F ²) = 0.091. 3, C₁₆H₁₆N₂NiO₄, M _r = 359.02, monoclinic, P2₁/c (No. 14), a = 10.6374(4) Å, b = 4.2964(2) Å, c = 15.2827(8) Å, β = 95.9744(14)°, V = 694.66(6) ų, Z = 2, R(F) = 0.028, wR(F ²) = 0.070. 4, C₁₆H₁₆N₂O₄Zn, M _r = 365.68, monoclinic, P2₁/c (No. 14), a = 10.6385(5) Å, b = 4.2967(3) Å, c = 15.2844(8) Å, β = 95.941(3)°, V = 694.89(7) ų, Z = 2, R(F) = 0.038, wR(F ²) = 0.107.     

Synthesis and molecular structure of catena((μ<Subscript>2</Subscript>-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione-<Emphasis Type="Italic">O,O'</Emphasis>)- aquadinitratocadmium(II))

A coordination polymer, catena((μ₂-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane- 2,8-dione-O,O')-aquadinitratocadmium(II) {[Cd(C₁₁H₂₀N₄O₂)(H₂O)(NO₃)₂]} _n } (I), has been prepared for the first time from cadmium(II) nitrate and the bicyclic bisurea 4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione (TTSU). Its molecular structure has been determined (CIF file CCDC no. 903387). Triclinic crystals: space group P1?, a = 8.9967(4) Å, b = 9.6011(4) Å, c = 12.5131(7) Å, α = 76.307(4)°, β = 73.465(5)°, γ = 63.310(5)°, V = 918.26(8) ų, ρ_calc = 1.789 g/cm³, Z = 2. The Rietveld refinement was carried out at 293 K to confirm the single-phase constitution of the obtained powder sample of I: a = 8.9972(4) Å, b = 9.6104(4) Å, c = 12.5203(4) Å, α = 76.373(3)°, β = 73.485(3)°, γ = 73.485(3)°, V = 919.80(6) ų. A number of lines not corresponding to the main phase and not identified from PDF-2 database are observed on the powder X-ray diffraction pattern. The Rietveld refinement showed that the sample contains 91.4 wt % of the main compound I and 8.6 wt % of the TTSU nitrate admixture. The cadmium atom is coordinated by the O(1) and O(1)ⁱ atoms of two molecules of the organic ligand (L) generated by the symmetry operation (ⁱ1–x,–y,–z), the O(2)ⁱⁱ atom of the third ligand L molecule bound with the supporting one with the symmetry operation (ⁱⁱ–x,–y,–z), a water molecule, and a bidentate and a monodentate nitrate anions. The coordination number of the cadmium atom is 7, the coordination polyhedron is a distorted pentagonal bipyramid. The Cd···Cd distance is 4.0208 (3) Å.     

Co(II) and Ni(II) complexes incorporating <Emphasis Type="Italic">N</Emphasis>-acetimidoylacetamidine ligand: Synthesis and structures

Two new square planar complexes with the formula Co(L)₂ · CH₃OH (1) and Ni(L)₂ · CH₃OH (2) (HL = HN{C(Me)=NH}₂ = N-acetimidoylacetamidine) have been synthesized by solvothermal reactions in methanol/acetonitrile. N-acetimidoylacetamidine ligand was derived from the self-condensation reaction of acetonitrile, and the reaction was promoted by the cooperation of M(II) (M = Co in 1 and M = Ni in 2) with diphenylcarbazide. 1 and 2 are characterized by single crystal X-ray diffraction, elemental analysis and infrared spectrum. Both complexes crystallize in the monoclinic space group P2₁/c with a = 9.329(6) Å, b = 11.494(7) Å, c = 13.040(8) Å, β = 92.945(11)°, V = 1396.3(16) ų and Z = 4 for 1, and a = 9.323(4)Å, b = 11.512(5) Å, c = 13.020(6)Å, β = 92.819(7)°, V = 1395.7(10)ų and Z = 4 for 2.     

Synthesis and study of ammonium hexamolybdobismuthate(III)

Ammonium hexamolybdobismuthate(III) of composition (NH₄)₃[BiMo₆O₁₈(OH)₆] · 7H₂O (I) was synthesized and studied by mass spectrometry, X-ray diffraction, IR spectroscopy, and thermogravimetry. The compound is monoclinic: a = 10.438 Å, b = 7.909 Å, c = 18.127 Å, β = 96.59°, V = 1486.76 ų, ρ_calc = 3.32 g/cm³, Z = 2.