Synthesis and structure of diethylenetriammonium tetrachloroaurates(III)

The (DienH₃)[AuCl₄]₃ · H₂O (I) and (DienH₃)₂[AuCl₄]Cl₅ (II) compounds were obtained by the reaction of HAuCl₄ with diethylenetriamine trihydrochloride (DienH₃Cl₃) in hydrochloric acid. The compounds were characterized by elemental analysis, X-ray diffraction, thermogravimetry, and IR spectroscopy. Crystals of I and II are monoclinic with space group P2₁/n. For I, a = 12.2314(3) Å, b = 14.6077(5) Å, c = 13.2680(5) Å, β = 106.7350(10)°, V = 2270.22(13) ų, Z = 8. For II, a = 6.62990(10) Å, b = 17.9026(5) Å, c = 10.3661(3) Å, β = 101.9230(10)°, V = 1203.83(5) ų, Z = 2. Both structures are ionic. The gold atoms in I and II have a 4 + 2 coordination environment. The Au-Cl bond lengths are within 2.276–2.294 Å, and the axial Au…Cl contacts are within 3.315–3.405 Å. The diethylenetriammonium cation in I and II has different conformations.     

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.     

X-ray study of rhodium(III) sulfates

Compounds with compositions [Rh(H₂O)₆]₂(SO₄)₃·4H₂O (I), (H₃O)[Rh(H₂O)₆](SO₄)₂ (II), [Rh(H₂O)₅OH](SO₄)·0.5H₂O (III), and [Rh(H₂O)₆]₂(SO₄)·(H₂SO₄) _x ·5H₂O (IV) have been studied. The crystal structures of II, III, and IV were determined. All compounds crystallized in the monoclinic crystal system. Crystal data for II: a = 7.279(2) Å, b = 10.512(7) Å, c = 15.806(3) Å, β = 96.71(3)°, space group P2₁/n, Z = 2, d _calc = 2.334 g/cm³; III: a = 20.433(4) Å, b = 7.820(2) c = 11.215(2) Å, β = 114.14(1)°, space group C2/c, Z = 8, d _calc = 2.559 g/cm³; IV: a = 6.2250(4 Å), b = 27.0270(12) Å, c = 7.2674(5) Å, β = 97.04(3)°, space group P2₁/c, Z = 4, d _calc = 2.143 g/cm³. The compounds were studied by IR spectroscopy and powder X-ray diffraction. All of the isolated crystalline phases are sparingly soluble in ethanol and well soluble in water.     

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.     

Crystal structures of rhodium(III) aqua ion with tetrahedral anions

The crystal structures of compounds of the composition [Rh(H₂O)₆]₂(SO₄)₃·5H₂O (I) and [Rh(H₂O)₆]PO₄ (II) are determined. Crystallographic data for I: a = 7.272(9) Å, b = 27.047(1) Å, c = 12.464(9) Å, β = 97.038(10)°, P2₁ space group, Z = 4, d _x = 2.184 g/cm³; for II: a = 9.746(6)Å, b = 6.877(7) Å, c = 23.623(6) Å, β = 100.601(10)°, C2/c space group, Z = 8, d _x = 2.611 g/cm³. Compounds are analyzed by IR spectroscopy and powder XRD. Crystalline phase I is well soluble in water, whereas II is almost insoluble.     

Synthesis and physicochemical study of hexaamminechromium(III) hexamolybdogallate

Hexaamminechromium(III) hexamolybdogallate of composition [Cr(NH₃)₆][GaMo₆O₁₈(OH)₆] · 5H₂O (I) was synthesized and studied by mass spectrometry, IR spectroscopy, thermogravimetry, and X-ray diffraction. Crystals I are monoclinic: a = 11.77 Å, b = 10.97 Å, c = 15.49 Å, β = 115.11°, V = 1811.29 ų, ρ_calc = 1.17 g/cm³, Z = 1. The compound obtained was used as a catalyst for soft oxidation of natural gas at 633 K.     

Preparation and physicochemical study of sodium hexamolybdometallates(III)

Sodium hexamolybdocobaltate(III) Na₃[CoMo₆O₁₈(OH)₆] · 8H₂O (I) and sodium hexamolybdochromate Na₃[CrMo₆O₁₈(OH)₆] · 8H₂O (II) were synthesized and studied by mass spectrometry, thermogravimetry, powder X-ray diffraction, and IR spectroscopy. The crystals are monoclinic. For compound a = 10.31 Å, b = 10.31 Å, c = 17.55 Å, β = 100.93°, V = 1834.77 ų, ρ_calcd = 3.04 g/cm³, Z = 3; for compound II: a = 10.33 Å, b = 10.33 Å, c = 17.59 Å, β = 100.98°, V = 1835.09 Å3, ρ_calcd = 3.01 g/cm³, Z = 3.     

(18-Crown-6)sodium tribromide and (18-crown-6)potassium triiodide (with an admixture of bromodiiodide): Synthesis and crystal structure

Two crystalline host-guest complexes are synthesized and studied using X-ray diffraction analysis: (18-crown-6)sodium tribromide [Na(18-crown-6)]⁺ · Br ₃ ^? (I) and (18-crown-6)potassium tribromide (with an admixture of bromodiiodide) [K(18-crown-6)]⁺ · (Br_0.25I_2.75)^? (II). The structures of compound I (space group P2₁/_{n, a} = 8.957 Å, b = 8.288 Å, c = 14.054 Å, β = 104.80°, Z = 2) and compound II (space group Cc, a = 8.417 Å, b = 15.147 Å, c = 17.445 Å, β = 99.01°, Z = 4) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.098 (I) and 0.036 (II) for all 2311 (I) and 2678 (II) independent measured reflections on a CAD-4 automated diffractometer (λMoK _α). Similar crystalline complexes I and II exist as infinite chains of alternating complex cations and trihalide anions linked to each other through weak Na-Br or K-I coordination bonds. In [Na(18-crown-6)]⁺ and [K(18-crown-6)]⁺ complex cations, the Na⁺ or K⁺ cation (coordination number is eight) is located in the center of the cavity of the 18-crown-6 ligand and coordinated by the six O atoms and two terminal Br or I atoms of two trihalide anions lying on opposite sides of the rms plane of the crown ligand.     

Synthesis and crystal structures of binuclear complexes of cobalt(II) and cadmium(II) diisobutyldithiophosphinates with hexamethylenetetramine

Heteroligand complexes [Co₂(HMTA)(iso-Bu₂PS₂)₄] (I) (μ_eff = 4.67 μB) and [Cd₂(HMTA)(iso-Bu₂PS₂)₄] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)^o, V = 5464.3(6) Å,³, Z = 4, ρ_calcd = 1.331 g/cm³ for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)^o, V = 5893.5(2) Å, Z = 4, ρ_calcd = 1.355 g/cm³ for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS₄, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu₂PS ₂ ^? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.     

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.     

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.     

Deca(hydroxo)-23-aqua-hexa(lanthanum(III)) iodide octahydrate and deca(hydroxo)-23-aqua-hexa(neodymium(III)) iodide octahydrate: Syntheses and structures

New hexanuclear complexes of lanthanum and neodymium iodides, [La₆(H₂O)₂₃(OH)₁₀]I₈ · 8H₂O (I) and [Nd₆(H₂O)₂₃(OH)₁₀]I₈ · 8H₂O (II), are synthesized and studied by X-ray diffraction analysis. The isostructural crystals of complexes I and II are orthorhombic: a = 13.197(4) Å, b = 15.152(3) Å, c = 15.302(4) Å and a = 13.060(4) Å, b = 14.967(5) Å, c = 15.098(4) Å, respectively; Z = 2, space group Pnnm. The lanthanum (neodymium) atoms coordinate the aqua and hydroxo ligands and enter the composition of the Ln₆ -containing complex cations. The coordination polyhedron (ignoring the central oxygen atom) of each atom of the complexing agent is somewhat distorted square antiprism with the aqua and hydroxo ligands being in the vertices. Four bridging ligands link this atom of the complexing agent with the four adjacent atoms.     

Synthesis and crystal structures of cobalt(III) and zinc(II) complexes with Schiff bases

Two new cobalt(III) and zinc(II) complexes, [Co(L¹)₂ (H₂O)] · ClO₄ (I) and [Ni(L²)₂ (H₂O)₂] · 2ClO₄ (II), where L¹ is the deprotonated form of 5-methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenol, and L² is the zwitterionic form of 2-[(2-isopropylaminoethylimino)methyl]-5-methoxyphenol, were synthesized and structurally characterized by elemental analyses, IR spectra, and single-crystal X-ray diffraction. The crystal of I is monoclinic: space group P2₁/c, a = 11.1512(4), b = 28.2424(11), c = 10.9655(4) Å, β = 95.746(2)°, V = 3436.1(2) ų, Z = 4. The crystal of II is triclinic: space group P2₁/c, a = 8.1441(2), b = 10.4531(3), c = 10.8849(3) Å, α = 84.0240(10)°, β = 76.9800(10)°, γ = 74.2280(10)°, V = 867.92(4) ų, Z = 1. Complex I consists of a mononuclear cobalt(III) complex cation and a perchlorate anion. Complex II consists of a crystallographic centrosymmetric mononuclear nickel(II) complex cation and two perchlorate anions. Each metal atom in the complexes is in an octahedral coordination.     

Synthesis and crystal structures of (2.2.2-cryptand)rubidium chloride and bromide hydrates

Two complexes, (2.2.2-cryptand)rubidium chloride and bromide hydrates [Rb(Crypt-222]Hal · 3.5H₂O (Hal = Cl (I) and Br (II)), are synthesized. The structures of isomorphic crystals of compounds I and II are studied by X-ray diffraction analysis. The crystals are trigonal: space group P \(\overline 3 \), Z = 2; I: a = 11.810 Å, c = 11.302 Å; II: a = 11.890 Å, c = 11.402 Å. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.060 (I) and 0.077 (II) for 2650 (I) and 2700 (II) independent reflections (CAD-4 automated diffractometer, λMoK _α radiation). In crystals of complexes I and II, the [Rb(Crypt-222)]⁺ cation of the host-guest type lies on the crystallographic axis 3 and has the approximate symmetry D ₃. In complexes I and II, the coordination polyhedron of the Rb⁺ cation is a two-base-centered trigonal prism somewhat distorted to an antiprism. The crystals of compounds I and II contain H-bonded disordered cubes of the water molecules and Cl^? or Br^? anions.     

Synthesis and X-ray investigation of Rb<Subscript>2</Subscript>[Pd(NO<Subscript>3</Subscript>)<Subscript>4</Subscript>] and Cs<Subscript>2</Subscript>[Pd(NO<Subscript>3</Subscript>)<Subscript>4</Subscript>]

Powder and single crystal X-ray diffraction studies have been performed for anhydrous nitrate complexes Rb₂[Pd(NO₃)₄] (I) and Cs₂[Pd(NO₃)₄] (II). Crystal data for I: a = 7.843(1) Å, b = 7.970(1) Å, c = 9.725(1) Å; β = 100.39(1)°, V = 597.9(1) Å ³, space group P2₁/c, Z = 2, d _calc = 2.918 g/cm³; for II: a = 10.309(2) Å, b = 10.426(2) Å, c = 11.839(2) Å; β = 108.17(3)°, V = 1209.0(4) ų, space group P2₁/c, Z = 4, d ^calc = 3.408 g/cm³. The structures are formed by isolated [Pd(NO₃)₄]^2? complex anions and alkali metal cations. The plane-square environment of the Pd atom is formed from the oxygen atoms of the monodentate nitrate groups. The geometrical characteristics of the complex anions are analyzed. Compound II has a short contact Pd...Cs 3.252 Å.     

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.     

Syntheses and crystal structures of (2.2.2-cryptand)potassium chloride and (2.2.2-cryptand)ammonium bromide<Subscript>(0.75)</Subscript>chloride<Subscript>(0.25)</Subscript> hydrates

Two new complexes were synthesized, namely, 7: 2 (2.2.2-cryptand)potassium chloride and (2.2.2-cryptand)ammonium bromide_(0.75)chloride_(0.25) hydrates: [M(Crypt-222)]⁺ · Hal^? · 3.5H₂O, where M = K, Hal = Cl (I) and M = NH₄, Hal = Br_0.75Cl_0.25 (II). The structures of two isomorphous crystals were studied by X-ray diffraction analysis. Trigonal (space group P \(\bar 3\), Z = 2) structures I (a = 11.763 Å, c = 11.262 Å) and II (a = 11.945 Å, c = 11.337 Å) were solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.057 (I) and 0.065 (II) for all 2626 (I) and 1654 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK _α). In structures I and II, the host-guest [M(Crypt-222)]⁺ complex cation lies on the threefold crystallographic axis and has the approximate D ₃ symmetry. In complex I, the coordination polyhedron of the K⁺ cation (CN = 8) is a bicapped trigonal prism somewhat distorted toward an antiprism. Complexes I and II contain H-bonded disordered cubes of the water molecules and the Cl^? or Br^? anions.     

Synthesis and crystal structure of zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3

Zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3 (HL) were synthesized. Crystals of [M(DMSO)₂L₂] · CHCl₃, where M= Zn^(II) (I) and Mn^(II) (II), obtained from chloroform plus dimethyl sulfoxide (DMSO) mixture were found to be isostructural based on the similarity of their unit cell parameters and unit cell volumes. The crystals are triclinic, Z = 2, space group P \(\bar 1\); a = 10.422(1) Å, b = 11.929(1) Å, c = 20.429(1) Å, α = 73.616(1)°, β = 85.095(1)°, γ = 77.586(1)° for complex I; a = 10.436(1) Å, b = 12.297(1) Å, c = 19.924(2) Å, α = 78.138(2)°, β = 87.625(2)°, γ = 82.048(2)° for complex II. X-ray structural analysis of complex I was carried out. For complex II, the structure was not refined because all of its atoms are each disordered over three to five positions. The two DMSO molecules in complex I coordinate the central metal atoms in the monodentate mode via their donor oxygen atoms to occupy an axial position and an equatorial position in an octahedral polyhedron. The other four positions are occupied by the four oxygen atoms of the two deprotonated ligands L^? coordinated in the bidentate-cyclic mode. The outer sphere of complex I contains the solvating chloroform molecule.     

Syntheses and crystal structures of hydrated complexes of strontium and barium bromides with 18-crown-6

Two complexes, namely, triaqua(18-crown-6)strontium dibromide monohydrate (I) and diaquabromo(18-crown-6)barium bromide (II), are synthesized. Their crystal structures are determined by X-ray diffraction analyses. For complex I, space group C2/c, a = 17.547 Å, b = 10.246 Å, c = 14.786 Å, β = 123.08°, Z = 4. For complex II, space group Pnma, a = 17.753 Å, b = 17.465 Å, c = 6.629 Å, Z = 4. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.056 (I) and 0.042 (II) for 2696 (I) and 2440 (II) independent reflections (CAD-4 automated diffractometer, λMoK _α radiation). Both complex cations—randomly disordered [Sr(18C6)(H₂O)₃]²⁺ in complex I and [BaBr(18C6)(H₂O)₂]⁺ in complex II—are of the host-guest type. The Sr²⁺ (Ba²⁺) cation resides in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In the structures complexes I and II, the coordination polyhedra of the Sr²⁺ and Ba²⁺ cations (coordination number 9) can be described as distorted hexagonal bipyramids with one apex at the O atom of the water molecule in complex I or at the Br^? ligand in complex II and the other split apex at the O atoms of two water molecules.     

Synthesis and crystal structure of Fe(III) and Al(III) complexes with 2-diphenylacetyl-1,3-indandione

Iron(III) and aluminum(III) complexes with 2-diphenylacetyl-1,3-indandione (HL) have been synthesized. The structures of the obtained compounds FeL₃(I) and AlL₃(II) were studied. The isostructural crystals are monoclinic, I: Z = 8, space group P2_1/c, a = 16.061(3) Å, b = 16.658(3) Å, c = 22.015(4) Å, β = 111.41(3)°; II: Z = 8, space group P2_1/c, a = 16.115(14) Å, b = 16.476(8) Å, c = 21.949(20) Å, β = 111.04(11)°. The structural units of crystals I and II are neutral molecules in which each ligand is bidentately coordinated to a central metal atom through the oxygen atom of the acyl keto group and an oxygen atom of the indandione fragment to form a six-membered chelate ring. In the crystals, neutral molecules I and II form pseudodimers due to stacking of indandione moieties of two adjacent coordination spheres and additional C-H…O contacts. Each pseudodimer is in contact with six neighboring dimers also through hydrogen bonds C-H…O to form an infinite framework.