Crystal structure and triboluminescence of the [Eu(TTA)2(NO3)(TPPO)2] complex

The crystal structure of [Eu(TTA)₂(NO₃)(TPPO)₂] (I) (TTA = thenoyltrifluoroacetone, TPPO = triphenylphosphine oxide) possessing intense triboluminescence was established by X-ray crystallography. The crystals are triclinic, noncentrocymmetrical: a = 11.047(3) Å, b = 11.794(3) Å, c = 12.537(3) Å; α = 102.635 (4)°, β = 102.088(4)°,γ = 117.765(3)°; space group P1, Z = 1. The central Eu(III) atom coordinates two oxygen atoms of two TPPO molecules at distances of 2.271 Å and 2.282 Å, two oxygen atoms of the nitrate group at distances of 2.478 Å and 2.481 Å, four oxygen atoms of two TTA ions at distances of 2.365 Å, 2.381 Å, and 2.363 Å, 2.371 Å (coordination number is 8). The coordination polyhedron of the Eu(III) atom is a distorted dodecahedron. Possible reasons for spectral differences in the Stark structure of photo-and triboluminescence of I are discussed.     

Cu(I) cloride complexes with 4,5-(2-pyridylethylene)dithio-1,3-dithiol-2-thione and triphenylphosphine

Heteroligand binuclear complexes of CuCl with triphenylphosphine and 5-pyridine-2-yl-5,6-dihydro-[1,3]dithiolo[4,5-b][1,4]dithiine-2-thione (L¹) of the compositions [CuCl(PPh₃)(L¹)]₂ (I) and [CuCiL¹]₂ (II) are synthesized and studied by X-ray diffraction method. Crystals I are monoclinic; space group P2₁/n, a=8.9520(18) Å, b=18.926(4) Å, c=16.841(3) Å, β=94.96(3)°, Z=2. The Cu(I) atom has a quasi-tetrahedral surrounding involving the tetraphenylphosphine P atom, the pyridyl N atom of the molecule L¹, and two bridging Cl atoms. Crystals II are monoclinic; space group P2₁/c, a=9.3520(19) Å, b=8.1490(16) Å, c=18.660(4) A, β = 104.43(3)°, Z = 2. Both L¹ ligands in complex II act as bridges. The Cu(I) atom also has a quasi-tetrahedral surrounding formed by the Cl atoms, the pyridyl N atoms and thiol S atom of one L¹ ligand, and the thione S atom of the second L¹ ligand. Similar binuclear complexes with the bridging function of the L¹ ligand were also detected in a solution of II by the ESI method.     

Crystal and molecular structure of a new gadolinium nitrate complex with furancarboxylic acid and dipyridyl

The gadolinium nitrato complex with α-furancarboxylic acid (FA) and 2,2′-dipyridyl (Dipy) has been synthesized. According to X-ray diffraction results, the complex is composed of the [Gd(FA)₂(NO₃)(Dipy)]₂ dimers. The crystals are triclinic: a = 9.942(2) Å, b = 10.231(2) Å, c = 11.037(2) Å, α = 85.50(3)°, β = 75.71(3)°, γ = 69.82(3)°, Z = 1. Two gadolinium atoms are linked by four carboxylate groups of furancarboxylic acid molecules. Each gadolinium atom is coordinated to seven oxygen atoms (five belonging to the FA carboxyl groups and two belonging to the bidentate nitrate group) and to two nitrogen atoms (from Dipy).     

Luminescent and triboluminescent properties of europium(III) hexafluoroacetylacetonate and trifluoroacetate complexes with triphenylphosphine oxide

Crystalline and strongly luminescent complexes of europium hexafluoroacetylacetonate and trifluoroacetate with triphenylphosphine oxide of Eu(HFAA)₃ · 2TPPO and [Eu(TFA)₃ · 2TPPO(H₂O)]₂ composition are synthesized that demonstrating triboluminescent properties. It is established that the measured photoluminescence and triboluminescence spectra of these noncentrosymmetric complex compounds are identical, due to the characteristic f-f-luminescence of the europium(III) ion.     

Crystal structure of trans*-[PtEnPyNO2(OH,NO2)*]Cl·2H2O

The structure of trans*-[PtEnPyNO₂(OH,NO₂)*]Cl·2H₂O was determined by X-ray crystallography. The crystals are monoclinic, a = 31.185(6)Å, b = 12.198(2)Å, c = 8.432(2)Å, b = 100.8(2)°, Z = 8, space group C2/c, R = 0.031 for 2059 reflections with I > 2σ(I). In the complex cation, the polyhedron of the Pt atom is an octahedron formed by five nitrogen atoms from ethylenediamine (Pt-N(aver.), 2.062(7) Å), pyridine (Pt-N, 2.053(7) Å), two NO₂ groups (Pt-N, 2.064(7) Å), and the oxygen atom of the OH group in trans position to the nitro group (Pt-O, 1.999(7) Å). Complex cations, anions Cl^?, and crystal water molecules are linked together through a branched system of hydrogen bonds.     

Synthesis and molecular and crystal structures of binuclear complexes of Sm(III), Eu(III), Gd(III), Tb(III), and Dy(III) nitrates with 4,4,10,10-tetramethyl-1,3,7,9-tetraazospiro[5.5]undecane-2,8-dione

Binuclear complexes of Sm(III), Eu(III), Gd(III), Tb(III), and Dy(III) nitrates with 4,4,10,10-tetramethyl-1,3,7,9-tetraazospiro[5.5]undecane-2,8-dione (C₁₁H₂₀N₄O₂, SC)—[Sm(NO₃)₃(SC)(H₂O)]₂(I), [Eu(NO₃)₃(SC)(H₂O)]₂ (II), [Gd(NO₃)₂(SC)(H₂O)₃)]₂(NO₃)₂ (III), [Tb(NO₃)₃(SC)(H₂O)]₂ (IV), [Dy(NO₃)₃(SC)(H₂O)]₂ (V), are synthesized, and their X-ray diffraction analyses are carried out. The crystals of complexes I–V are monoclinic: space group P2₁/n for III and P2₁/c for I, II, IV, and V. In centrosymmetric coordination complexes II, III, IV, and V, the Ln atoms are coordinated by two O(1) and O(2) atoms of two molecules of the SC ligands bound by a symmetry procedure (1 ? x, ?y, 1 ? z), three bidentate nitrate anions, and a water molecule. The coordination numbers of the metal atoms are equal to 9, and the coordination polyhedra are considerably distorted three-capped trigonal prisms, whose bases include the O(1), O(2), O(12) and O(3), O(7), O(9) atoms. The dihedral angle between the bases of the prism is 18°, and that between the mean planes of the side faces is 55°–71° for I, 17° and 55°–71° for II, 16° and 55°–70° for IV, and 16° and 55°–70° for V. The Sm...Sm distance in complex I is 9.44 Å, Eu...Eu in II is 9.42 Å, Tb...Tb in IV is 9.36Å, and Dy...Dy in V is 9.36Å. The gadolinium atom in complex III is coordinated by two oxygen atoms of two ligand molecules bound by a symmetry procedure (?x, ?y + 1, ?z + 1), two bidentate nitrate anions, and three water molecules. One of the nitro groups in compound III is localized in the external coordination sphere of the metal. The coordination number of gadolinium is 9, and the coordination polyhedron is a significantly distorted three-capped trigonal prism, whose base includes the O(1), O(2), O(7) and O(4), O(5), O(9) atoms. The dihedral angle between the bases of the prism is 22.8°, and that between the mean planes of the side faces is 53°–72°. The Gd...Gd distance in complex III is 9.17 Å.     

Coordination compounds of cobalt(II) and cadmium(II) with 2-amino-4-methylpyrimidine: Synthesis, crystal structure, and luminescent properties

The coordination compounds [CoL₂Cl₂] (I) and [CdL₂(H₂O)₂(NO₃)₂] (II) have been synthesized by the reaction of CoCl₂ · 6H₂O and Cd(NO₃)₂ · 4H₂O with L = 2-amino-4-methylpyrimidine (Ampym, C₅H₇N₃), and their structures have been solved. The crystals of complex I are triclinic, space group $P\bar 1$ , a = 5.627(1) Å, b = 11.191(1) Å, c = 12.445(1) Å, α = 81.00(1)°, β = 77.21(1)°, γ = 76.18(1)°, V = 737.7(2) ų, ρ_calcd = 1.567 g/cm³, Z = 2. The crystals of complex II are monoclinic, space group P2₁/c, a = 10.390(1) Å, b = 11.982(1) Å, c = 7.624(1) Å, β = 102.61(1)°, V = 926.1(2) ų, ρ_calcd = 1.760 g/cm³, Z = 2. Discrete [CoL₂Cl₂] moieties are realized in the structure of complex I. The cobalt atom is tetrahedrally coordinated to the two nitrogen atoms of crystallographically nonequivalent ligands L and two chlorine atoms (Co(1)-N_avg, 2.051(4)Å; Co(1)-Cl(1), 2.241(1) Å; Co(1)-Cl(2), 2.263 Å; bond angles at the cobalt atom lie within a range of 102.1°–118.6°). The complexes are linked into supramolecular zigzag chains by N-H...N(Cl) hydrogen bonds. In the structure of complex II, the Cd²⁺ ion (at the inversion center) is coordinated in pairs to the nitrogen atoms of ligand L and the O(NO₃) and O(H₂O) oxygen atoms. The coordination of the Cd²⁺ ion is distorted octahedral (Cd(1)-N(1), 2.341Å; Cd(1)-O(1), 2.340(4) Å; Cd(1)-O(4), 2.327(3) Å; bond angles at the cadmium atom lie within a range of 79.1°–100.9°). N-H...N hydrogen bonds link the complexes into supramolecular chains. These chains are linked into a supramolecular framework by the O-H...O hydrogen bonds between water molecules and NO₃ groups.     

CRYSTAL STRUCTURE OF THE ISOMORPHOUS COMPLEXES TETRAAQUABIS(2,6-DIHYDROXY-BENZOATO-O)(2,6-DIHYDROXY-BENZOATO-O,O)TERBIUM(III) AND HOLMIUM(III) DIHYDRATE

Abstract

The structures of isomorphic Tb(III) and Ho(III) complexes with 2,6-dihydroxybenzoic acid of formula [Tb(C₇H₅O₄] 2H₂O and [Ho(C₇H₅O₄)₃ 4H₂O] 2H₂O has been determined by X-ray diffraction and refined to a residual R = 0.030 for 5376 observed reflections and R = 0.0284 for 5660 observed reflections, for Tb(III) and Ho(III) complexes, respectively. Crystals are triclinic, space group P1 with a= 10.748(2), b=11.309(2), c = 12.452(2)Å, α = 82.28(3), ? = 73.05(5), γ = 68.27(3)° for Tb(III) and a= 10.731(2), b=11.269(2), c = 12.436(2)Å, α = 82.25(3), β = 72.92(3), γ = 68.46(3)° for Ho(III).

In the structure of these monomelic complexes the metal ions are coordinated by oxygen atoms of one bidentate chelating and two monodentate carboxylate groups and four molecules of water. Tb-O distances are in the range 2.323(3)-2.506(3) Å and Ho-0 2.297(3)-2.486(3) Å. The crystal structure, consisting of discrete units of neutral complexes with two molecules of water of crystallization is stabilized by intra-and intermolecular hydrogen bonds.     

Crystal structure refinement for trans-[Pd(NO3)2(H2O)2]

Single crystals of trans-[Pd(NO₃)₂(H₂O)₂] were obtained, and the crystal structure of this complex, previously obtained for polycrystals, was refined. Crystal data (BRUKER X8APEX diffractometer): a = 4.9973(7) Å, b = 10.5982(14) Å, c = 11.7008(17) Å, V = 619.70(15) ų, space group Pbca, Z = 4, d _calc = 2.856 g/cm³. The structure is composed of neutral complexes with a trans configuration. The square plane environment of the Pd atom is formed by four oxygen atoms (Pd-O(NO₃) 1.999(5) Å, Pd-O(H₂O) 2.030(5) Å) and completed to a distorted bipyramid by two intramolecular contacts (Pd…O(NO₃) 2.926 Å). The shortest hydrogen bonds are O…H 2.72 Å.     

Synthese und Kristallstruktur von K2(HSO4)(H2PO4), K4(HSO4)3(H2PO4) und Na(HSO4)(H3PO4)

Synthesis and Crystal Structure of K₂(HSO₄)(H₂PO₄), K₄(HSO₄)₃(H₂PO₄), and Na(HSO₄)(H₃PO₄) Mixed hydrogen sulfate phosphates K₂(HSO₄)(H₂PO₄), K₄(HSO₄)₃(H₂PO₄) and Na(HSO₄)(H₃PO₄) were synthesized and characterized by X‐ray single crystal analysis. In case of K₂(HSO₄)(H₂PO₄) neutron powder diffraction was used additionally. For this compound an unknown supercell was found. According to X‐ray crystal structure analysis, the compounds have the following crystal data: K₂(HSO₄)(H₂PO₄) (T = 298 K), monoclinic, space group P 2₁/c, a = 11.150(4) Å, b = 7.371(2) Å, c = 9.436(3) Å, β = 92.29(3)°, V = 774.9(4) ų, Z = 4, R₁ = 0.039; K₄(HSO₄)₃(H₂PO₄) (T = 298 K), triclinic, space group P 1, a = 7.217(8) Å, b = 7.521(9) Å, c = 7.574(8) Å, α = 71.52(1)°, β = 88.28(1)°, γ = 86.20(1)°, V = 389.1(8)ų, Z = 1, R₁ = 0.031; Na(HSO₄)(H₃PO₄) (T = 298 K), monoclinic, space group P 2₁, a = 5.449(1) Å, b = 6.832(1) Å, c = 8.718(2) Å, β = 95.88(3)°, V = 322.8(1) ų, Z = 2, R₁ = 0,032. The metal atoms are coordinated by 8 or 9 oxygen atoms. The structure of K₂(HSO₄)(H₂PO₄) is characterized by hydrogen bonded chains of mixed H_nS/PO₄^– tetrahedra. In the structure of K₄(HSO₄)₃(H₂PO₄), there are dimers of H_nS/PO₄^– tetrahedra, which are further connected to chains. Additional HSO₄^– tetrahedra are linked to these chains. In the structure of Na(HSO₄)(H₃PO₄) the HSO₄^– tetrahedra and H₃PO₄ molecules form layers by hydrogen bonds.     

Sc(III), Eu(III), and Gd(III) Complexes with Macrocyclic Cavitand Cucurbit[6]uril: Synthesis and Crystal Structures

Slow evaporation of solutions of Sc and Eu nitrates with macrocyclic cavitand cucurbit[6]uril gives crystals of isostructural complexes [Sc(NO₃)(H₂O)₄(C₃₆H₃₆N₂₄O₁₂)](NO₃)₂ ? 8.5H₂O (space group Pna2₁, a = 32.0065(18) Å, b = 14.7904(8) Å, c = 11.5774(6) Å, V = 5480.6(5) ų, Z = 4) and [Eu(NO₃)(H₂O)₄(C₃₆H₃₆N₂₄O₁₂)](NO₃)₂ ? 6.75H₂O (space group Pna2₁, a = 31.9525(17) Å, b = 14.7203(8) Å, c = 11.8592(6) Å, V = 5578.0(5) ų, Z = 4). The metal to ligand ratio in these complexes is 1 : 1; the complexes are obtained at 0.025–0.1 mol/l concentrations of the metals in solutions. With higher lanthanide concentrations (0.7–1 mol/l), the 2 : 1 complex with cucurbit[6]uril is formed of the composition [{ Gd(NO₃)(H₂O)₅}₂(C₃₆H₃₆N₂₄O₁₂)](NO₃)₄ ? 6.5H₂O (space group \(P\bar 1\), a = 13.3972(6) Å, b = 14.4994(5) Å, c = 18.3290(8) Å, α = 73.5610(10)°, β = 87.2590(10)°, γ = 87.5540(10)°, V = 3409.4(2) ų, Z = 2) and isotypical complex [{Gd(NO₃)(H₂O)₅}₂{(C₅H₅N) ? (C₃₆H₃₆N₂₄O₁₂)}](NO₃)₄ ? 8H₂O with a pyridine molecule inside the cucurbit[6]uril cavity (space group P2₁/n, a = 14.8263(6) Å, b = 13.3688(7) Å, c = 18.5970(9) Å, β = 107.5860(10)°, V = 3513.8(3) ų, Z = 2). According to X-ray diffraction data, the metal atoms of the title complexes coordinate the O atoms in portals of cucurbit[6]uril molecules.     

Crystal structure of tris[(2.2.2-cryptand)× (nitrato-O,O′)lead(II)] pentakis(nitrato-O,O′)lead(II)

A novel coordination compound tris[(2.2.2-cryptand)(nitrato-O,O′)lead(II)] pentakis(nitrato-O, O′)lead(II), 3[Pb(NO₃)(Crypt-222)]⁺·[Pb(NO₃)₅]^3? (I) has been prepared and studied by the single crystal X-ray diffraction technique. The crystals of I are monoclinic: space group Pc, a = 25.944 Å, b = 18.389 Å, c = 17.145 Å, β = 93.33°, Z = 4. The structure of I has been solved by the direct and heavy atom methods and refined in a full-matrix anisotropic-isotropic approximation to R = 0.122 for the total of 11145 measured reflections (automated diffractometer CAD-4, λMoK _α). The structure of I includes six independent host-guest complex cations [Pb(NO₃)(Crypt-222)]⁺ and two independent complex anions [Pb(NO₃)₅]^3?. Coordination number of the cation Pb²⁺ equals ten in all these complex ions, and its coordination polyhedron in the first of them is a strongly distorted “hexagonal bipyramid” with two forked vertices, while for the latter ones it is a strongly distorted “square pyramid” with all five vertices forked.     

Synthesis and structure of complex compound Rh(III) of (NH4)2[Rh(NO2)3(NH3)(µ-OH)]2 composition

The crystalline structure of a new compound Rh(III) of (NH₄)₂[Rh(NO₂)₃(NH₃)(μ-OH)]₂ composition has been determined. The crystallographic characteristics are H₁₆N₁₀O₁₄Rh₂: a = 6.3963(2) Å, b = 9.3701(4) Å, c = 13.6646(5) Å, β = 102.266(1)°, V = 800.28(5) ų, Z = 2, d _calc = 2.432 g/cm³. The distance Rh...Rh in the dimer is 3.200 Å. Original Russian Text Copyright ? 2006 by S. P. Khranenko, I. A. Baidina, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 2, pp. 380–384, March–April, 2006.     

Homo- und heterodinukleare α-Pyridonat-verbrückte Platin- und Palladium-komplexe mit Bis(N-methylimidazol-2-yl)keton (BMIK). Kristallstrukturen von [(BMIK)Pt(α-Pyridonat)2Pt(BMIK)](NO3)2 · 4H2O, [(BMIK)Pd(α-Pyridonat)2Pd(BMIK)](NO3)2 · 4H2O und [(BMIK)Pd(α-Pyridonat)2Pt/Pd(BMIK)](NO3)2 · 4H2O

Homo- and Heterodinuclear α-Pyridonate-bridged Platinum and Palladium Complexes with Bis(N-methylimidazol-2-yl)ketone (BMIK). Crystal Structures of [(BMIK)Pt(α-pyridonate)₂Pt(BMIK)](NO₃)₂ · 4H₂O, [(BMIK)Pd(α-pyridonate)₂Pd(BMIK)](NO₃)₂ · 4H₂O, and [(BMIK)Pd(α-pyridonate)₂Pt/Pd(BMIK)](NO₃)₂ · 4H₂O The isotypic dinuclear complexes [(BMIK)Pt(α-pyridonate)₂Pt(BMIK)](NO₃)₂ · 4H₂O ( 1 ) (P1 ; a = 12.197(5) Å, b = 12.505(5) Å, c = 12.866(5) Å, α = 88.17(3)°, β = 73.55(3)°, γ = 69.84(3)°; Z = 2) and [(BMIK)Pd(α-pyridonate)₂Pd(BMIK)](NO₃)₂ · 4H₂O ( 2 ) (a = 12.408(3) Å, b = 12.660(3) Å, c = 12.913(3) Å, α = 89.55(3)°, β = 74.59(2)°, γ = 68.68(2)°) were prepared by reaction of [Pt(BMIK)(H₂O)₂](NO₃)₂ or [Pd(BMIK)(H₂O)₂](NO₃)₂ with α-pyridone in aqueous solutions at 40°C and were isolated as red air-stable crystals (BMIK = bis(N-methylimidazol-2-yl)ketone). For the synthesis of mixed crystals of 2 with the heterometal complex [(BMIK)Pd(α-pyridonate)₂Pt(BMIK)](NO₃)₂ · 4H₂O ( 3 ) (a = 12.430(4) Å, b = 12.648(3) Å, c = 12.907(4) Å, α = 89.64(2)°, β = 74.57(2)°, γ = 68.65(2)°) α-pyridone was reacted with [Pd(BMIK)(H₂O)₂](NO₃)₂ in a molar ratio of 2 : 1 followed by addition of [Pt(BMIK)(H₂O)₂](NO₃)₂. The dinuclear cations consist of two M(BMIK) moieties (M = Pt, Pd) bridged by the N- and O-atoms of α-pyridonate, forcing the heterocyclic ring into head-head-orientation. Within the dinuclear cation, the two metal atoms are between 2.840 Å and 2.860 Å apart. The intermolecular distances are between 4.762 Å and 4.837 Å. The coordination geometry of both metal atoms is square-planar with the metal atoms being diplaced slightly from their respective coordination planes toward each other. ¹H and ¹⁹⁵Pt NMR spectra are reported for the complexes.     

Bis(triphenylphosphin)iminium-bis(methoxo)phthalocyaninato(2–)ferrat(III) – Synthese und Kristallstruktur

Bis(triphenylphosphine)iminium Bis(methoxo)phthalocyaninato(2–)ferrate(III) – Synthesis and Crystal Structure Chlorophthalocyaninato(2–)ferrate(III) reacts with bis(triphenylphosphine)iminium hydroxide in methanol/acetone solution to yield blue crystals of bis(triphenylphosphine)iminium bis(methoxo)phthalocyaninato(2–)ferrate(III). The complex salt crystallizes as an acetone/methanol solvate (^bPNP)[Fe(OCH₃)₂pc^2–] · (CH₃)₂CO · 1.5 CH₃OH in the triclinic space group P 1 (no. 2) with the cell parameters a = 13.160(5) Å, b = 15.480(5) Å, c = 17.140(5) Å, α = 97.54(5)°, β = 91.79(5)°, γ = 95.44(5)°. The Fe atom is located in the centre of the pc^2– ligand coordinating four isoindole N atoms (N_iso) of the pc^2– ligand and two O atoms of the methoxo ligands in a mutual trans arrangement. The average Fe–O and Fe–N_iso distances are 1.887 and 1.943 Å, respectively. The cation adopts the bent conformation (< P–N–P = 140.4(2)°) with P–N distances of 1.579(3) and 1.575(3) Å.     

Crystal and molecular structures of triaquabis(5-nitro-2-acetamidobenzoato)copper(II) dihydrate

A new copper(II) complex [Cu(5-NO₂-2-CH₃CONHC₆H₃COO)₂(H₂O)₃] · 2H₂O was synthesized by the reaction of sodium 5-nitro-5-acetamidobenzoate with CuSO₄ · 5H₂O (2: 1), and its structure was determined by X-ray diffraction. Crystals are monoclinic: a = 11.7146(7) Å, b = 16.8463(10) Å, c = 13.2408(9) Å, β = 113.896(5)°, Z = 4, ρ_calc = 1.668 g/cm³, space group P2₁/c, R = 0.0338. In the monomer complex, the copper atom has an elongated square-pyramidal coordination (4 + 1); the coordination sphere is formed by two oxygen atoms of the carboxylate groups of two monodentate organic ligands and the three oxygen atoms O(w) of the water molecules (the O(3w) atom is in the axial position). In the structure, the complex molecules are linked by hydrogen bonds involving two uncoordinated water molecules.     

Crystal structure of (glycine) sodium nitrate Gly·NaNO3

The crystal structure of Gly·NaNO₃ was determined by single crystal diffraction methods (monoclinic crystal system, B11n, a = 14.339(3) Å, b = 9.136(3) Å, c = 5.263(3) Å, γ = 119.14(5)°). The structure is built from alternating layers of glycine organic molecules and inorganic layers consisting of Na⁺ ions and planar NO ₃ ^? ions stretching along the b axis. The surroundings of the Na atom include the oxygen atoms of the NO ₃ ^? groups and the oxygen atoms of glycine molecules. The structure has a system of hydrogen bonds.     

Hydrolysis of coordinated aminoacetonitrile in a platinum(IV) complex. Crystal structure of [PtPy(NH<Subscript>2</Subscript>CH<Subscript>2</Subscript>COO)Cl<Subscript>3</Subscript>]

Heating of a hydrochloric acid solution of trans-PtPy(NH₂CH₂CN)Cl₄ results in the hydrolysis of coordinated aminoacetonitrile to aminoacetic acid with the formation of a five-membered chelate ring attached to platinum through the nitrogen atom of the amino group and the oxygen atom of the carboxy group. X-ray diffraction analysis of [PtPy(NH₂CH₂COO)Cl₃] is carried out. The crystals are monoclinic: space group C2/c, a = 21.704(2), b = 8.7027(7), c = 15.576(1) Å, β = 126.606(1)^o, V = 2361.8(3) ų, Z = 8; R _hkl = 0.057, wR = 0.141. In the neutral complex, the Pt atom has a distorted octahedral coordination. The equatorial plane is formed by a Cl atom (Pt-Cl, 2.284(3) Å), the N atom of the Py molecule (Pt-N, 2.062(8) Å), and the N and O atoms of the bidentate-chelating ligand (Pt-N, 2.039(8); Pt-O, 2.026(7) Å); two Cl atoms are arranged in the apical positions (Pt-Cl, 2.301(3) and 2.312(3) Å). The five-membered chelate ring has a flattened gauche conformation with an NCCO torsion angle of 19(1)°.     

N(B(NMe2)2)(Si(NMe2)3)(Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3) — Synthese und Charakterisierung neuer molekularer Einkomponentenvorläufer für nitridische und carbonitridische Keramiken

N(B(NMe₂)₂)(Si(NMe₂)₃) (Ti(NMe₂)₃), [N(Si(NMe₂)₃)(Ti(NMe₂)₂)]₂ und N(SiMe₃)(Si(NMe₂)₃)(Ti(NMe₂)₃) — Synthesis and Characterization of New Molecular Single-source Precursors for Nitride and Carbonitride Ceramics Synthesis and spectroscopic data of the title compounds are reported. [N(Si(NMe₂)₃)(Ti(NMe₂)₂)]₂ crystallizes in the space group P1 , a = 8.406(7), b = 10.673(8), c = 10.872(6) Å, α = 68.45(4)°, β = 71.72(4)°, γ = 78.11(7)°, 2 877 diffractometer data (F_o ? 2σF_o), R = 0.051. The compound is characterized by a planar four-membered Ti₂N₂-ring with exocyclic tris(dimethylamino)silyl substituents attached to the nitrogen atoms of the ring.     

Crystal structure of [Pb<Subscript>3</Subscript>(OH)<Subscript>4</Subscript>Co(NO<Subscript>2</Subscript>)<Subscript>3</Subscript>](NO<Subscript>3</Subscript>)(NO<Subscript>2</Subscript>)·2H<Subscript>2</Subscript>O

The structure of [Pb₃(OH)₄Co(NO₂)₃](NO₃)(NO₂)·2H₂O is determined by single crystal X-ray diffraction. The crystallographic characteristics are as follows: a = 8.9414(4) Å, b = 14.5330(5) Å, c = 24.9383(9) Å, V = 3240.6(2) ų, space group Pbca, Z = 8. The Co(III) atoms have a slightly distorted octahedral coordination formed by three nitrogen atoms belonging to nitro groups (Co–N_av is 1.91 Å) and three oxygen atoms belonging to hydroxyl groups (Co–O_av is 1.93 Å). The hydroxyl groups act as μ₃-bridges between the metal atoms. The geometric characteristics are analyzed and the packing motif is determined.